# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2022 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_001m _database_code_depnum_ccdc_archive 'CCDC 2184009' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H82 Cl2 Ga2 N4 P2' _chemical_formula_weight 1107.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7010(18) _cell_length_b 13.8715(16) _cell_length_c 15.7041(18) _cell_angle_alpha 90 _cell_angle_beta 105.336(6) _cell_angle_gamma 90 _cell_volume 2878.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9679 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 40.14 _exptl_crystal_description block _exptl_crystal_colour 'greenish yellow' #blueish? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_F_000 1168 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.452 _exptl_crystal_size_mid 0.402 _exptl_crystal_size_min 0.368 _exptl_absorpt_coefficient_mu 1.124 _shelx_estimated_absorpt_T_min 0.631 _shelx_estimated_absorpt_T_max 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_measurement_device_type 'Bruker D8 KAPPA II (APEX II detector)' _diffrn_measurement_method 'Data collection strategy APEX 2/COSMO' _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 72672 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.991 _diffrn_reflns_theta_max 40.215 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 18029 _reflns_number_gt 14347 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'BRUKER APEX3(v2019.1-0)' _computing_cell_refinement 'BRUKER APEX3(v2019.1-0)' _computing_data_reduction 'BRUKER APEX3(v2019.1-0)' _computing_structure_solution 'BRUKER APEX3(v2019.1-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. Disorder: An isopropyl group is disordered over two positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.6679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 18029 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.05089(2) 0.13275(2) 0.62152(2) 0.01090(2) Uani 1 1 d . . . . . Cl1 Cl 0.17261(2) 0.06680(2) 0.72780(2) 0.02082(4) Uani 1 1 d . . . . . P1 P -0.05565(2) 0.02967(2) 0.52365(2) 0.02004(5) Uani 1 1 d . . . . . N1 N 0.12000(5) 0.23320(5) 0.57372(4) 0.01175(10) Uani 1 1 d . . . . . N2 N -0.02279(5) 0.21625(5) 0.68146(4) 0.01227(10) Uani 1 1 d . . . . . C1 C 0.14150(6) 0.31567(6) 0.61850(5) 0.01433(12) Uani 1 1 d . . . . . C2 C 0.10070(7) 0.34190(6) 0.68893(6) 0.01688(13) Uani 1 1 d . . . . . H2 H 0.132720 0.394500 0.724164 0.020 Uiso 1 1 calc R U . . . C3 C 0.01857(6) 0.30000(6) 0.71358(5) 0.01443(12) Uani 1 1 d . . . . . C4 C 0.21247(8) 0.38703(7) 0.59364(7) 0.02349(18) Uani 1 1 d . . . . . H4A H 0.200245 0.388396 0.529276 0.035 Uiso 1 1 calc R U . . . H4B H 0.282629 0.367704 0.620715 0.035 Uiso 1 1 calc R U . . . H4C H 0.200621 0.451321 0.614775 0.035 Uiso 1 1 calc R U . . . C5 C -0.02340(8) 0.35396(7) 0.77978(7) 0.02208(17) Uani 1 1 d . . . . . H5A H -0.025885 0.423042 0.766317 0.033 Uiso 1 1 calc R U . . . H5B H 0.020290 0.343141 0.839376 0.033 Uiso 1 1 calc R U . . . H5C H -0.091813 0.330647 0.776542 0.033 Uiso 1 1 calc R U . . . C6 C 0.15325(6) 0.21441(6) 0.49516(5) 0.01229(11) Uani 1 1 d . . . . . C7 C 0.24928(6) 0.17390(6) 0.50184(5) 0.01347(12) Uani 1 1 d . . . . . C8 C 0.27566(7) 0.15117(7) 0.42385(6) 0.01886(15) Uani 1 1 d . . . . . H8 H 0.339883 0.123161 0.427397 0.023 Uiso 1 1 calc R U . . . C9 C 0.21012(8) 0.16868(9) 0.34184(6) 0.02300(17) Uani 1 1 d . . . . . H9 H 0.229632 0.153755 0.289634 0.028 Uiso 1 1 calc R U . . . C10 C 0.11577(8) 0.20816(9) 0.33642(6) 0.02438(19) Uani 1 1 d . . . . . H10 H 0.071171 0.220366 0.279918 0.029 Uiso 1 1 calc R U . . . C11 C 0.08458(7) 0.23046(8) 0.41180(6) 0.01961(15) Uani 1 1 d . . . . . C12 C 0.32496(6) 0.15243(7) 0.58951(6) 0.01722(14) Uani 1 1 d . . . . . H12 H 0.295979 0.175573 0.637986 0.021 Uiso 1 1 calc R U . . . C13 C 0.42562(8) 0.20489(10) 0.59758(7) 0.0268(2) Uani 1 1 d . . . . . H13A H 0.455037 0.183329 0.550345 0.040 Uiso 1 1 calc R U . . . H13B H 0.472455 0.190291 0.655022 0.040 Uiso 1 1 calc R U . . . H13C H 0.413632 0.274566 0.592523 0.040 Uiso 1 1 calc R U . . . C14 C 0.34447(9) 0.04391(9) 0.60145(8) 0.0282(2) Uani 1 1 d . . . . . H14A H 0.279976 0.010089 0.594137 0.042 Uiso 1 1 calc R U . . . H14B H 0.388274 0.031405 0.660688 0.042 Uiso 1 1 calc R U . . . H14C H 0.377644 0.020798 0.557157 0.042 Uiso 1 1 calc R U . . . C15 C -0.0248(4) 0.2620(3) 0.4025(3) 0.0179(6) Uani 0.53(2) 1 d . . P A 1 H15 H -0.043684 0.241658 0.457103 0.021 Uiso 0.53(2) 1 calc R U P A 1 C16 C -0.0299(3) 0.3716(3) 0.3977(6) 0.0417(13) Uani 0.53(2) 1 d . . P A 1 H16A H -0.007643 0.393721 0.346616 0.063 Uiso 0.53(2) 1 calc R U P A 1 H16B H 0.014402 0.398860 0.451804 0.063 Uiso 0.53(2) 1 calc R U P A 1 H16C H -0.099656 0.392651 0.391644 0.063 Uiso 0.53(2) 1 calc R U P A 1 C17 C -0.1017(5) 0.2178(4) 0.3232(4) 0.0219(7) Uani 0.53(2) 1 d . . P A 1 H17A H -0.087696 0.240306 0.268492 0.033 Uiso 0.53(2) 1 calc R U P A 1 H17B H -0.170163 0.237445 0.324054 0.033 Uiso 0.53(2) 1 calc R U P A 1 H17C H -0.096507 0.147378 0.326393 0.033 Uiso 0.53(2) 1 calc R U P A 1 C15' C -0.0142(6) 0.2875(9) 0.4017(5) 0.0334(15) Uani 0.47(2) 1 d . . P A 2 H15' H -0.030757 0.286420 0.459963 0.040 Uiso 0.47(2) 1 calc R U P A 2 C16' C -0.0084(8) 0.3933(7) 0.3751(4) 0.0495(18) Uani 0.47(2) 1 d . . P A 2 H16D H 0.012831 0.396687 0.320340 0.074 Uiso 0.47(2) 1 calc R U P A 2 H16E H 0.040669 0.427524 0.422127 0.074 Uiso 0.47(2) 1 calc R U P A 2 H16F H -0.075202 0.423257 0.365964 0.074 Uiso 0.47(2) 1 calc R U P A 2 C17' C -0.0997(7) 0.2377(10) 0.3349(7) 0.047(2) Uani 0.47(2) 1 d . . P A 2 H17D H -0.082801 0.232987 0.278227 0.071 Uiso 0.47(2) 1 calc R U P A 2 H17E H -0.162133 0.275068 0.327359 0.071 Uiso 0.47(2) 1 calc R U P A 2 H17F H -0.109453 0.172902 0.356131 0.071 Uiso 0.47(2) 1 calc R U P A 2 C18 C -0.11896(6) 0.18318(6) 0.69224(5) 0.01309(11) Uani 1 1 d . . . . . C19 C -0.12251(7) 0.12164(6) 0.76262(6) 0.01630(13) Uani 1 1 d . . . . . C20 C -0.21665(8) 0.08497(8) 0.76608(7) 0.02270(17) Uani 1 1 d . . . . . H20 H -0.220297 0.043232 0.813096 0.027 Uiso 1 1 calc R U . . . C21 C -0.30452(8) 0.10832(9) 0.70236(8) 0.02628(19) Uani 1 1 d . . . . . H21 H -0.367620 0.082441 0.705629 0.032 Uiso 1 1 calc R U . . . C22 C -0.29998(7) 0.16969(9) 0.63373(7) 0.02486(18) Uani 1 1 d . . . . . H22 H -0.360585 0.186129 0.590620 0.030 Uiso 1 1 calc R U . . . C23 C -0.20788(7) 0.20778(7) 0.62682(6) 0.01764(14) Uani 1 1 d . . . . . C24 C -0.02918(7) 0.09401(8) 0.83494(6) 0.02001(15) Uani 1 1 d . . . . . H24 H 0.030097 0.129228 0.824133 0.024 Uiso 1 1 calc R U . . . C25 C -0.04075(10) 0.12448(11) 0.92566(7) 0.0323(2) Uani 1 1 d . . . . . H25A H -0.053634 0.193977 0.925618 0.048 Uiso 1 1 calc R U . . . H25B H 0.021582 0.109350 0.971114 0.048 Uiso 1 1 calc R U . . . H25C H -0.097572 0.089592 0.938205 0.048 Uiso 1 1 calc R U . . . C26 C -0.00791(9) -0.01443(9) 0.83358(8) 0.0288(2) Uani 1 1 d . . . . . H26A H 0.000531 -0.032495 0.775620 0.043 Uiso 1 1 calc R U . . . H26B H -0.064774 -0.050365 0.844910 0.043 Uiso 1 1 calc R U . . . H26C H 0.054099 -0.029729 0.879345 0.043 Uiso 1 1 calc R U . . . C27 C -0.20637(8) 0.27591(9) 0.55114(7) 0.02567(19) Uani 1 1 d . . . . . H27 H -0.136128 0.276451 0.543650 0.031 Uiso 1 1 calc R U . . . C28 C -0.23265(13) 0.37943(10) 0.57320(10) 0.0398(3) Uani 1 1 d . . . . . H28A H -0.232926 0.421995 0.523328 0.060 Uiso 1 1 calc R U . . . H28B H -0.182043 0.402108 0.625862 0.060 Uiso 1 1 calc R U . . . H28C H -0.299692 0.379984 0.584420 0.060 Uiso 1 1 calc R U . . . C29 C -0.27852(11) 0.24398(11) 0.46347(8) 0.0351(3) Uani 1 1 d . . . . . H29A H -0.271015 0.287019 0.416124 0.053 Uiso 1 1 calc R U . . . H29B H -0.348420 0.246692 0.468078 0.053 Uiso 1 1 calc R U . . . H29C H -0.262269 0.177811 0.450159 0.053 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.01100(4) 0.01157(4) 0.01093(4) -0.00181(2) 0.00432(3) -0.00039(3) Cl1 0.01766(9) 0.02577(10) 0.01970(9) 0.00879(7) 0.00612(7) 0.00613(7) P1 0.01401(9) 0.02216(10) 0.02494(11) -0.01222(8) 0.00692(8) -0.00412(8) N1 0.0118(2) 0.0129(2) 0.0114(2) -0.00030(18) 0.0046(2) -0.00029(19) N2 0.0114(2) 0.0135(2) 0.0129(2) -0.00301(19) 0.0049(2) -0.00066(19) C1 0.0132(3) 0.0139(3) 0.0169(3) -0.0020(2) 0.0058(2) -0.0018(2) C2 0.0164(3) 0.0165(3) 0.0195(3) -0.0074(3) 0.0080(3) -0.0046(3) C3 0.0137(3) 0.0162(3) 0.0143(3) -0.0051(2) 0.0053(2) -0.0011(2) C4 0.0253(4) 0.0180(3) 0.0320(5) -0.0047(3) 0.0160(4) -0.0079(3) C5 0.0215(4) 0.0236(4) 0.0245(4) -0.0124(3) 0.0120(3) -0.0036(3) C6 0.0119(3) 0.0146(3) 0.0112(2) 0.0007(2) 0.0044(2) 0.0007(2) C7 0.0109(3) 0.0176(3) 0.0123(3) -0.0006(2) 0.0038(2) 0.0002(2) C8 0.0142(3) 0.0285(4) 0.0151(3) -0.0027(3) 0.0059(3) 0.0025(3) C9 0.0178(4) 0.0392(5) 0.0131(3) -0.0028(3) 0.0061(3) 0.0028(4) C10 0.0185(4) 0.0431(6) 0.0118(3) 0.0026(3) 0.0045(3) 0.0069(4) C11 0.0155(3) 0.0310(4) 0.0127(3) 0.0042(3) 0.0044(3) 0.0070(3) C12 0.0111(3) 0.0268(4) 0.0136(3) 0.0010(3) 0.0031(2) 0.0030(3) C13 0.0133(4) 0.0473(6) 0.0192(4) -0.0023(4) 0.0031(3) -0.0044(4) C14 0.0283(5) 0.0304(5) 0.0273(5) 0.0071(4) 0.0096(4) 0.0131(4) C15 0.0152(10) 0.0238(13) 0.0141(10) 0.0025(9) 0.0029(7) 0.0068(9) C16 0.0284(14) 0.0260(13) 0.066(3) 0.0020(14) 0.0044(15) 0.0094(10) C17 0.0125(10) 0.0372(15) 0.0146(9) 0.0021(9) 0.0008(7) 0.0035(9) C15' 0.025(2) 0.057(4) 0.0210(13) 0.017(2) 0.0117(14) 0.021(2) C16' 0.052(3) 0.044(3) 0.049(2) 0.007(2) 0.009(2) 0.027(3) C17' 0.025(2) 0.078(6) 0.041(4) 0.025(3) 0.012(2) 0.016(3) C18 0.0113(3) 0.0153(3) 0.0139(3) -0.0023(2) 0.0054(2) -0.0003(2) C19 0.0146(3) 0.0195(3) 0.0161(3) 0.0007(2) 0.0065(3) -0.0001(3) C20 0.0176(4) 0.0257(4) 0.0273(4) 0.0049(3) 0.0104(3) -0.0022(3) C21 0.0146(4) 0.0328(5) 0.0331(5) 0.0032(4) 0.0094(4) -0.0043(3) C22 0.0118(3) 0.0367(5) 0.0259(4) 0.0033(4) 0.0048(3) -0.0003(3) C23 0.0120(3) 0.0239(4) 0.0179(3) 0.0012(3) 0.0056(3) 0.0019(3) C24 0.0170(4) 0.0276(4) 0.0165(3) 0.0051(3) 0.0063(3) 0.0008(3) C25 0.0298(5) 0.0518(7) 0.0163(4) 0.0013(4) 0.0081(4) -0.0007(5) C26 0.0248(5) 0.0290(5) 0.0354(5) 0.0118(4) 0.0128(4) 0.0062(4) C27 0.0138(4) 0.0403(5) 0.0235(4) 0.0118(4) 0.0059(3) 0.0068(4) C28 0.0446(8) 0.0302(6) 0.0377(7) 0.0077(5) -0.0016(6) -0.0027(5) C29 0.0383(6) 0.0466(7) 0.0192(4) 0.0026(4) 0.0056(4) 0.0163(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.9363(7) . ? Ga1 N1 1.9436(7) . ? Ga1 Cl1 2.2207(3) . ? Ga1 P1 2.3131(3) . ? P1 P1 2.0381(5) 3_556 ? N1 C1 1.3344(10) . ? N1 C6 1.4473(10) . ? N2 C3 1.3320(11) . ? N2 C18 1.4469(10) . ? C1 C2 1.4127(12) . ? C1 C4 1.5095(12) . ? C2 C3 1.4085(12) . ? C3 C5 1.5127(11) . ? C6 C7 1.4089(11) . ? C6 C11 1.4132(12) . ? C7 C8 1.4015(11) . ? C7 C12 1.5179(12) . ? C8 C9 1.3828(13) . ? C9 C10 1.3856(14) . ? C10 C11 1.3955(13) . ? C11 C15 1.531(5) . ? C11 C15' 1.539(7) . ? C12 C14 1.5317(15) . ? C12 C13 1.5347(14) . ? C15 C16 1.522(5) . ? C15 C17 1.530(7) . ? C15' C17' 1.517(11) . ? C15' C16' 1.533(7) . ? C18 C19 1.4076(12) . ? C18 C23 1.4121(12) . ? C19 C20 1.4007(13) . ? C19 C24 1.5178(13) . ? C20 C21 1.3850(16) . ? C21 C22 1.3876(16) . ? C22 C23 1.3985(13) . ? C23 C27 1.5227(14) . ? C24 C26 1.5334(16) . ? C24 C25 1.5339(15) . ? C27 C29 1.5327(18) . ? C27 C28 1.542(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 97.40(3) . . ? N2 Ga1 Cl1 105.39(2) . . ? N1 Ga1 Cl1 103.88(2) . . ? N2 Ga1 P1 111.98(2) . . ? N1 Ga1 P1 118.22(2) . . ? Cl1 Ga1 P1 117.464(13) . . ? P1 P1 Ga1 95.182(18) 3_556 . ? C1 N1 C6 121.88(7) . . ? C1 N1 Ga1 118.25(5) . . ? C6 N1 Ga1 119.70(5) . . ? C3 N2 C18 122.80(6) . . ? C3 N2 Ga1 118.79(5) . . ? C18 N2 Ga1 118.38(5) . . ? N1 C1 C2 123.75(7) . . ? N1 C1 C4 119.57(7) . . ? C2 C1 C4 116.68(7) . . ? C3 C2 C1 128.26(7) . . ? N2 C3 C2 123.14(7) . . ? N2 C3 C5 119.40(7) . . ? C2 C3 C5 117.47(7) . . ? C7 C6 C11 120.77(7) . . ? C7 C6 N1 120.44(7) . . ? C11 C6 N1 118.60(7) . . ? C8 C7 C6 118.44(7) . . ? C8 C7 C12 118.45(7) . . ? C6 C7 C12 123.10(7) . . ? C9 C8 C7 121.36(8) . . ? C8 C9 C10 119.48(8) . . ? C9 C10 C11 121.70(9) . . ? C10 C11 C6 118.21(8) . . ? C10 C11 C15 119.6(2) . . ? C6 C11 C15 121.9(2) . . ? C10 C11 C15' 119.0(3) . . ? C6 C11 C15' 121.9(3) . . ? C7 C12 C14 111.04(8) . . ? C7 C12 C13 111.42(8) . . ? C14 C12 C13 109.39(9) . . ? C16 C15 C17 110.3(4) . . ? C16 C15 C11 108.7(3) . . ? C17 C15 C11 114.1(4) . . ? C17' C15' C16' 109.5(6) . . ? C17' C15' C11 109.5(6) . . ? C16' C15' C11 114.5(5) . . ? C19 C18 C23 121.04(8) . . ? C19 C18 N2 120.39(7) . . ? C23 C18 N2 118.38(7) . . ? C20 C19 C18 118.30(8) . . ? C20 C19 C24 118.78(8) . . ? C18 C19 C24 122.92(8) . . ? C21 C20 C19 121.36(9) . . ? C20 C21 C22 119.71(9) . . ? C21 C22 C23 121.25(9) . . ? C22 C23 C18 118.34(8) . . ? C22 C23 C27 119.59(8) . . ? C18 C23 C27 122.05(8) . . ? C19 C24 C26 111.28(9) . . ? C19 C24 C25 110.60(8) . . ? C26 C24 C25 110.48(9) . . ? C23 C27 C29 112.52(10) . . ? C23 C27 C28 110.52(10) . . ? C29 C27 C28 109.72(10) . . ? _refine_diff_density_max 1.096 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.088 _shelx_res_file ; TITL mks_001m in P2(1)/n mks_001m.res created by SHELXL-2017/1 at 09:32:02 on 28-Jul-2020 CELL 0.71073 13.70100 13.87150 15.70410 90.0000 105.3364 90.0000 ZERR 2.00000 0.00180 0.00160 0.00180 0.0000 0.0057 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H Cl Ga N P UNIT 116 164 4 4 8 4 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.140 SIZE 0.368 0.402 0.452 L.S. 16 ACTA FMAP 2 PLAN 20 WGHT 0.045900 0.667900 FVAR 0.13340 0.53348 GA1 4 0.050887 0.132751 0.621515 11.00000 0.01100 0.01157 = 0.01093 -0.00181 0.00432 -0.00039 CL1 3 0.172611 0.066803 0.727801 11.00000 0.01766 0.02577 = 0.01970 0.00879 0.00612 0.00613 P1 6 -0.055648 0.029667 0.523655 11.00000 0.01401 0.02216 = 0.02494 -0.01222 0.00692 -0.00412 N1 5 0.120001 0.233196 0.573719 11.00000 0.01178 0.01287 = 0.01144 -0.00030 0.00456 -0.00029 N2 5 -0.022788 0.216249 0.681459 11.00000 0.01141 0.01349 = 0.01290 -0.00301 0.00491 -0.00066 C1 1 0.141503 0.315671 0.618499 11.00000 0.01322 0.01389 = 0.01692 -0.00199 0.00579 -0.00179 C2 1 0.100697 0.341903 0.688935 11.00000 0.01644 0.01650 = 0.01952 -0.00735 0.00795 -0.00458 AFIX 43 H2 2 0.132720 0.394500 0.724164 11.00000 -1.20000 AFIX 0 C3 1 0.018574 0.300002 0.713579 11.00000 0.01365 0.01621 = 0.01433 -0.00514 0.00527 -0.00109 C4 1 0.212473 0.387031 0.593636 11.00000 0.02531 0.01799 = 0.03197 -0.00470 0.01604 -0.00788 AFIX 137 H4A 2 0.200245 0.388396 0.529276 11.00000 -1.50000 H4B 2 0.282629 0.367704 0.620715 11.00000 -1.50000 H4C 2 0.200621 0.451321 0.614775 11.00000 -1.50000 AFIX 0 C5 1 -0.023404 0.353958 0.779782 11.00000 0.02151 0.02361 = 0.02449 -0.01237 0.01202 -0.00362 AFIX 137 H5A 2 -0.025885 0.423042 0.766317 11.00000 -1.50000 H5B 2 0.020290 0.343141 0.839376 11.00000 -1.50000 H5C 2 -0.091813 0.330647 0.776542 11.00000 -1.50000 AFIX 0 C6 1 0.153254 0.214413 0.495164 11.00000 0.01187 0.01457 = 0.01120 0.00067 0.00439 0.00068 C7 1 0.249284 0.173897 0.501843 11.00000 0.01091 0.01759 = 0.01231 -0.00059 0.00377 0.00022 C8 1 0.275656 0.151172 0.423850 11.00000 0.01416 0.02853 = 0.01507 -0.00271 0.00595 0.00248 AFIX 43 H8 2 0.339883 0.123161 0.427397 11.00000 -1.20000 AFIX 0 C9 1 0.210122 0.168679 0.341844 11.00000 0.01781 0.03921 = 0.01310 -0.00280 0.00607 0.00278 AFIX 43 H9 2 0.229632 0.153755 0.289634 11.00000 -1.20000 AFIX 0 C10 1 0.115773 0.208160 0.336416 11.00000 0.01854 0.04308 = 0.01179 0.00257 0.00449 0.00685 AFIX 43 H10 2 0.071171 0.220366 0.279918 11.00000 -1.20000 AFIX 0 C11 1 0.084579 0.230456 0.411799 11.00000 0.01549 0.03104 = 0.01269 0.00422 0.00441 0.00699 C12 1 0.324958 0.152428 0.589515 11.00000 0.01112 0.02679 = 0.01364 0.00095 0.00308 0.00297 AFIX 13 H12 2 0.295979 0.175573 0.637986 11.00000 -1.20000 AFIX 0 C13 1 0.425616 0.204894 0.597580 11.00000 0.01327 0.04727 = 0.01916 -0.00227 0.00309 -0.00442 AFIX 137 H13A 2 0.455037 0.183329 0.550345 11.00000 -1.50000 H13B 2 0.472455 0.190291 0.655022 11.00000 -1.50000 H13C 2 0.413632 0.274566 0.592523 11.00000 -1.50000 AFIX 0 C14 1 0.344470 0.043908 0.601449 11.00000 0.02828 0.03037 = 0.02729 0.00712 0.00963 0.01310 AFIX 137 H14A 2 0.279976 0.010089 0.594137 11.00000 -1.50000 H14B 2 0.388274 0.031405 0.660688 11.00000 -1.50000 H14C 2 0.377644 0.020798 0.557157 11.00000 -1.50000 AFIX 0 PART 1 21 C15 1 -0.024815 0.262043 0.402477 21.00000 0.01520 0.02384 = 0.01406 0.00247 0.00286 0.00679 AFIX 13 H15 2 -0.043684 0.241658 0.457103 21.00000 -1.20000 AFIX 0 C16 1 -0.029879 0.371567 0.397711 21.00000 0.02842 0.02599 = 0.06602 0.00199 0.00445 0.00937 AFIX 137 H16A 2 -0.007643 0.393721 0.346616 21.00000 -1.50000 H16B 2 0.014402 0.398860 0.451804 21.00000 -1.50000 H16C 2 -0.099656 0.392651 0.391644 21.00000 -1.50000 AFIX 0 C17 1 -0.101707 0.217818 0.323231 21.00000 0.01248 0.03718 = 0.01460 0.00214 0.00082 0.00352 AFIX 137 H17A 2 -0.087696 0.240306 0.268492 21.00000 -1.50000 H17B 2 -0.170163 0.237445 0.324054 21.00000 -1.50000 H17C 2 -0.096507 0.147378 0.326393 21.00000 -1.50000 AFIX 0 PART 2 -21 C15' 1 -0.014151 0.287536 0.401677 -21.00000 0.02517 0.05727 = 0.02097 0.01708 0.01171 0.02084 AFIX 13 H15' 2 -0.030757 0.286420 0.459963 -21.00000 -1.20000 AFIX 0 C16' 1 -0.008449 0.393283 0.375135 -21.00000 0.05238 0.04442 = 0.04949 0.00690 0.00946 0.02726 AFIX 137 H16D 2 0.012831 0.396687 0.320340 -21.00000 -1.50000 H16E 2 0.040669 0.427524 0.422127 -21.00000 -1.50000 H16F 2 -0.075202 0.423257 0.365964 -21.00000 -1.50000 AFIX 0 C17' 1 -0.099701 0.237717 0.334946 -21.00000 0.02481 0.07800 = 0.04119 0.02494 0.01233 0.01628 AFIX 137 H17D 2 -0.082801 0.232987 0.278227 -21.00000 -1.50000 H17E 2 -0.162133 0.275068 0.327359 -21.00000 -1.50000 H17F 2 -0.109453 0.172902 0.356131 -21.00000 -1.50000 AFIX 0 PART 0 C18 1 -0.118964 0.183180 0.692238 11.00000 0.01131 0.01529 = 0.01387 -0.00226 0.00542 -0.00032 C19 1 -0.122515 0.121639 0.762623 11.00000 0.01459 0.01954 = 0.01613 0.00066 0.00647 -0.00008 C20 1 -0.216648 0.084975 0.766078 11.00000 0.01758 0.02572 = 0.02733 0.00493 0.01037 -0.00221 AFIX 43 H20 2 -0.220297 0.043232 0.813096 11.00000 -1.20000 AFIX 0 C21 1 -0.304517 0.108323 0.702361 11.00000 0.01459 0.03284 = 0.03314 0.00319 0.00936 -0.00432 AFIX 43 H21 2 -0.367620 0.082441 0.705629 11.00000 -1.20000 AFIX 0 C22 1 -0.299978 0.169686 0.633730 11.00000 0.01184 0.03675 = 0.02585 0.00331 0.00476 -0.00028 AFIX 43 H22 2 -0.360585 0.186129 0.590620 11.00000 -1.20000 AFIX 0 C23 1 -0.207877 0.207784 0.626816 11.00000 0.01200 0.02393 = 0.01792 0.00122 0.00558 0.00195 C24 1 -0.029181 0.094009 0.834940 11.00000 0.01697 0.02762 = 0.01649 0.00512 0.00629 0.00079 AFIX 13 H24 2 0.030097 0.129228 0.824133 11.00000 -1.20000 AFIX 0 C25 1 -0.040745 0.124483 0.925659 11.00000 0.02980 0.05180 = 0.01632 0.00132 0.00813 -0.00066 AFIX 137 H25A 2 -0.053634 0.193977 0.925618 11.00000 -1.50000 H25B 2 0.021582 0.109350 0.971114 11.00000 -1.50000 H25C 2 -0.097572 0.089592 0.938205 11.00000 -1.50000 AFIX 0 C26 1 -0.007912 -0.014429 0.833581 11.00000 0.02480 0.02902 = 0.03545 0.01184 0.01277 0.00625 AFIX 137 H26A 2 0.000531 -0.032495 0.775620 11.00000 -1.50000 H26B 2 -0.064774 -0.050365 0.844910 11.00000 -1.50000 H26C 2 0.054099 -0.029729 0.879345 11.00000 -1.50000 AFIX 0 C27 1 -0.206370 0.275909 0.551144 11.00000 0.01382 0.04031 = 0.02347 0.01184 0.00595 0.00678 AFIX 13 H27 2 -0.136128 0.276451 0.543650 11.00000 -1.20000 AFIX 0 C28 1 -0.232652 0.379431 0.573198 11.00000 0.04458 0.03019 = 0.03769 0.00768 -0.00156 -0.00267 AFIX 137 H28A 2 -0.232926 0.421995 0.523328 11.00000 -1.50000 H28B 2 -0.182043 0.402108 0.625862 11.00000 -1.50000 H28C 2 -0.299692 0.379984 0.584420 11.00000 -1.50000 AFIX 0 C29 1 -0.278523 0.243979 0.463473 11.00000 0.03829 0.04661 = 0.01916 0.00258 0.00557 0.01628 AFIX 137 H29A 2 -0.271015 0.287019 0.416124 11.00000 -1.50000 H29B 2 -0.348420 0.246692 0.468078 11.00000 -1.50000 H29C 2 -0.262269 0.177811 0.450159 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM mks_001m in P2(1)/n REM R1 = 0.0330 for 14347 Fo > 4sig(Fo) and 0.0495 for all 18029 data REM 347 parameters refined using 0 restraints END WGHT 0.0459 0.6679 REM Highest difference peak 1.096, deepest hole -0.610, 1-sigma level 0.088 Q1 1 0.0552 0.1737 0.6216 11.00000 0.05 1.10 Q2 1 -0.2036 0.3602 0.5506 11.00000 0.05 1.06 Q3 1 0.1504 0.0271 0.7167 11.00000 0.05 0.99 Q4 1 0.0521 0.0923 0.6221 11.00000 0.05 0.98 Q5 1 0.0014 0.1360 0.6226 11.00000 0.05 0.85 Q6 1 0.2029 0.1994 0.4996 11.00000 0.05 0.84 Q7 1 0.0994 0.1351 0.6228 11.00000 0.05 0.81 Q8 1 -0.0682 0.0733 0.5174 11.00000 0.05 0.72 Q9 1 -0.1694 0.1005 0.7625 11.00000 0.05 0.70 Q10 1 0.1231 0.0703 0.7277 11.00000 0.05 0.68 Q11 1 -0.2043 0.2432 0.5302 11.00000 0.05 0.65 Q12 1 -0.2535 0.1927 0.6326 11.00000 0.05 0.64 Q13 1 -0.0049 0.2590 0.6930 11.00000 0.05 0.63 Q14 1 0.1016 0.2680 0.4216 11.00000 0.05 0.62 Q15 1 0.1323 0.2717 0.5989 11.00000 0.05 0.60 Q16 1 0.2609 0.1615 0.4587 11.00000 0.05 0.60 Q17 1 0.3397 0.1025 0.5946 11.00000 0.05 0.60 Q18 1 0.1785 0.3507 0.6145 11.00000 0.05 0.59 Q19 1 0.1176 0.3295 0.6506 11.00000 0.05 0.59 Q20 1 -0.1589 0.1869 0.6545 11.00000 0.05 0.59 ; _shelx_res_checksum 65565 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_057m _database_code_depnum_ccdc_archive 'CCDC 2184320' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-06 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H102 B Cl2 F20 Ga2 N6 P2' _chemical_formula_weight 2002.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6151(10) _cell_length_b 16.6393(13) _cell_length_c 23.1348(18) _cell_angle_alpha 77.844(3) _cell_angle_beta 77.731(3) _cell_angle_gamma 86.897(3) _cell_volume 4638.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9646 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 79.99 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_F_000 2062 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.326 _exptl_crystal_size_mid 0.149 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 2.344 _shelx_estimated_absorpt_T_min 0.515 _shelx_estimated_absorpt_T_max 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 Venture (Photon II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/Queen' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 283933 _diffrn_reflns_av_unetI/netI 0.0146 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.996 _diffrn_reflns_theta_max 80.659 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 20142 _reflns_number_gt 18999 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX3(v2017.3-0)' _computing_cell_refinement 'Bruker APEX3(v2017.3-0)' _computing_data_reduction 'Bruker APEX3(v2017.3-0)' _computing_structure_solution 'Bruker APEX3(v2017.3-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. Disorder: The central core of the cation is disordered over two positions. The corresponding bond lengths and angles were restrained to be equal (SADI) and RIGU restraints were applied to the displacement prarmeters. Due to their close proximity C60 and C60' as well as c61 and C61' were refined with additional SIMU restraints. The toluene molecule is disorderd over two positions. RIGU restraints were used for the refinement of its atoms' displacement parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+4.4979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 20142 _refine_ls_number_parameters 1392 _refine_ls_number_restraints 266 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.20991(9) 0.30882(6) 0.89196(5) 0.01828(14) Uani 0.7342(12) 1 d . . P A 1 Ga2 Ga 0.31913(7) 0.32498(4) 0.64161(4) 0.01736(13) Uani 0.7342(12) 1 d . . P A 1 Cl1 Cl 0.05884(6) 0.38076(5) 0.90868(4) 0.02472(15) Uani 0.7342(12) 1 d . . P A 1 Cl2 Cl 0.45143(7) 0.41011(5) 0.63504(4) 0.02566(16) Uani 0.7342(12) 1 d . . P A 1 P1 P 0.30414(5) 0.33125(4) 0.79096(3) 0.01823(14) Uani 0.7342(12) 1 d . . P A 1 P2 P 0.22735(5) 0.26755(4) 0.73980(3) 0.02098(15) Uani 0.7342(12) 1 d . . P A 1 N5 N 0.3707(3) 0.4954(3) 0.7568(2) 0.0261(9) Uani 0.7342(12) 1 d D . P A 1 N6 N 0.2015(3) 0.4882(2) 0.75504(19) 0.0222(7) Uani 0.7342(12) 1 d D . P A 1 C59 C 0.2892(3) 0.44204(17) 0.76647(13) 0.0204(5) Uani 0.7342(12) 1 d D . P A 1 C60 C 0.3362(6) 0.5749(4) 0.7386(6) 0.0314(19) Uani 0.7342(12) 1 d D U P A 1 C61 C 0.2290(7) 0.5704(4) 0.7393(9) 0.0333(18) Uani 0.7342(12) 1 d D U P A 1 C62 C 0.4840(3) 0.4735(3) 0.75923(19) 0.0365(9) Uani 0.7342(12) 1 d D . P A 1 H62A H 0.529720 0.490214 0.718878 0.055 Uiso 0.7342(12) 1 calc R U P A 1 H62B H 0.490493 0.413911 0.773032 0.055 Uiso 0.7342(12) 1 calc R U P A 1 H62C H 0.507649 0.501718 0.787393 0.055 Uiso 0.7342(12) 1 calc R U P A 1 C63 C 0.0927(2) 0.4591(2) 0.75852(15) 0.0269(6) Uani 0.7342(12) 1 d D . P A 1 H63A H 0.074446 0.473649 0.718466 0.040 Uiso 0.7342(12) 1 calc R U P A 1 H63B H 0.040164 0.484934 0.786996 0.040 Uiso 0.7342(12) 1 calc R U P A 1 H63C H 0.090438 0.399265 0.772443 0.040 Uiso 0.7342(12) 1 calc R U P A 1 C64 C 0.4095(7) 0.6469(4) 0.7257(3) 0.058(2) Uani 0.7342(12) 1 d D . P A 1 H64A H 0.472365 0.639936 0.693903 0.087 Uiso 0.7342(12) 1 calc R U P A 1 H64B H 0.434126 0.650574 0.762426 0.087 Uiso 0.7342(12) 1 calc R U P A 1 H64C H 0.370056 0.697332 0.712163 0.087 Uiso 0.7342(12) 1 calc R U P A 1 C65 C 0.1477(5) 0.6369(3) 0.7254(2) 0.0446(12) Uani 0.7342(12) 1 d D . P A 1 H65A H 0.184581 0.689893 0.710900 0.067 Uiso 0.7342(12) 1 calc R U P A 1 H65B H 0.092907 0.638939 0.762120 0.067 Uiso 0.7342(12) 1 calc R U P A 1 H65C H 0.112561 0.625264 0.694202 0.067 Uiso 0.7342(12) 1 calc R U P A 1 Ga1' Ga 0.2268(3) 0.28751(16) 0.88822(15) 0.0214(4) Uani 0.2658(12) 1 d . . P A 2 Ga2' Ga 0.3361(2) 0.34987(12) 0.63565(11) 0.0188(4) Uani 0.2658(12) 1 d . . P A 2 Cl1' Cl 0.08661(19) 0.37152(13) 0.88417(12) 0.0273(4) Uani 0.2658(12) 1 d . . P A 2 Cl2' Cl 0.48143(19) 0.42779(14) 0.61233(12) 0.0264(5) Uani 0.2658(12) 1 d . . P A 2 P1' P 0.31679(14) 0.25716(11) 0.79574(8) 0.0228(4) Uani 0.2658(12) 1 d . . P A 2 P2' P 0.23940(13) 0.34309(10) 0.73498(7) 0.0180(4) Uani 0.2658(12) 1 d . . P A 2 N5' N 0.3455(8) 0.4872(7) 0.7476(6) 0.022(2) Uani 0.2658(12) 1 d D . P A 2 N6' N 0.1776(7) 0.5049(6) 0.7429(5) 0.022(2) Uani 0.2658(12) 1 d D . P A 2 C59' C 0.2570(7) 0.4488(4) 0.7442(4) 0.0182(14) Uani 0.2658(12) 1 d D . P A 2 C60' C 0.3193(15) 0.5692(8) 0.7501(15) 0.025(3) Uani 0.2658(12) 1 d D U P A 2 C61' C 0.2158(17) 0.5817(8) 0.742(2) 0.027(3) Uani 0.2658(12) 1 d D U P A 2 C62' C 0.4528(8) 0.4525(6) 0.7526(5) 0.0299(19) Uani 0.2658(12) 1 d D . P A 2 H62D H 0.454064 0.394082 0.750816 0.045 Uiso 0.2658(12) 1 calc R U P A 2 H62E H 0.468945 0.458373 0.791044 0.045 Uiso 0.2658(12) 1 calc R U P A 2 H62F H 0.507336 0.481691 0.719102 0.045 Uiso 0.2658(12) 1 calc R U P A 2 C63' C 0.0639(6) 0.4894(6) 0.7444(4) 0.0285(18) Uani 0.2658(12) 1 d D . P A 2 H63D H 0.039069 0.528892 0.712075 0.043 Uiso 0.2658(12) 1 calc R U P A 2 H63E H 0.019646 0.495428 0.783578 0.043 Uiso 0.2658(12) 1 calc R U P A 2 H63F H 0.056835 0.433391 0.738596 0.043 Uiso 0.2658(12) 1 calc R U P A 2 C64' C 0.4036(15) 0.6307(10) 0.7462(8) 0.041(4) Uani 0.2658(12) 1 d D . P A 2 H64D H 0.369438 0.684854 0.746835 0.049 Uiso 0.2658(12) 1 calc R U P A 2 H64E H 0.457647 0.633130 0.708573 0.049 Uiso 0.2658(12) 1 calc R U P A 2 H64F H 0.439279 0.614359 0.780720 0.049 Uiso 0.2658(12) 1 calc R U P A 2 C65' C 0.1443(15) 0.6562(9) 0.7422(8) 0.050(4) Uani 0.2658(12) 1 d D . P A 2 H65D H 0.187114 0.703328 0.742910 0.074 Uiso 0.2658(12) 1 calc R U P A 2 H65E H 0.085720 0.646413 0.778190 0.074 Uiso 0.2658(12) 1 calc R U P A 2 H65F H 0.113304 0.667832 0.705887 0.074 Uiso 0.2658(12) 1 calc R U P A 2 N1 N 0.17381(12) 0.19447(10) 0.93544(7) 0.0252(3) Uani 1 1 d . . . . . N2 N 0.29745(12) 0.33265(10) 0.94500(7) 0.0255(3) Uani 1 1 d . . . . . N3 N 0.38407(12) 0.23942(10) 0.60524(7) 0.0232(3) Uani 1 1 d . . . . . N4 N 0.24676(13) 0.38309(11) 0.57714(7) 0.0279(3) Uani 1 1 d . . . . . C1 C 0.16218(16) 0.17882(12) 0.99556(9) 0.0277(4) Uani 1 1 d . . . . . C2 C 0.19825(16) 0.23198(13) 1.02684(8) 0.0288(4) Uani 1 1 d . . . . . H2 H 0.171797 0.220984 1.069325 0.035 Uiso 1 1 calc R U . . . C3 C 0.26773(15) 0.29885(13) 1.00400(8) 0.0276(4) Uani 1 1 d . . . . . C4 C 0.1110(2) 0.09971(14) 1.03239(10) 0.0397(5) Uani 1 1 d . . . . . H4A H 0.042619 0.092108 1.020613 0.060 Uiso 1 1 calc R U . . . H4B H 0.096672 0.101795 1.075375 0.060 Uiso 1 1 calc R U . . . H4C H 0.160339 0.053661 1.025174 0.060 Uiso 1 1 calc R U . . . C5 C 0.31230(18) 0.33303(14) 1.04946(9) 0.0358(5) Uani 1 1 d . . . . . H5A H 0.389670 0.344588 1.034028 0.054 Uiso 1 1 calc R U . . . H5B H 0.302765 0.292732 1.087705 0.054 Uiso 1 1 calc R U . . . H5C H 0.273369 0.383935 1.056146 0.054 Uiso 1 1 calc R U . . . C6 C 0.15508(15) 0.12922(12) 0.90612(8) 0.0273(4) Uani 1 1 d . . . . . C7 C 0.05454(16) 0.12360(12) 0.89050(9) 0.0284(4) Uani 1 1 d . . . . . C8 C 0.04090(17) 0.06071(14) 0.86130(10) 0.0344(4) Uani 1 1 d . . . . . H8 H -0.026113 0.056624 0.849656 0.041 Uiso 1 1 calc R U . . . C9 C 0.12234(19) 0.00440(14) 0.84897(10) 0.0390(5) Uani 1 1 d . . . . . H9 H 0.111228 -0.038249 0.829362 0.047 Uiso 1 1 calc R U . . . C10 C 0.22041(18) 0.01046(14) 0.86536(10) 0.0382(5) Uani 1 1 d . . . . . H10 H 0.276281 -0.028572 0.856884 0.046 Uiso 1 1 calc R U . . . C11 C 0.23914(17) 0.07250(14) 0.89401(9) 0.0327(4) Uani 1 1 d . . . . . C12 C -0.03831(15) 0.18283(13) 0.90392(9) 0.0300(4) Uani 1 1 d . . . . . H12 H -0.015551 0.220688 0.927275 0.036 Uiso 1 1 calc R U . . . C13 C -0.14018(17) 0.13801(14) 0.94254(10) 0.0374(5) Uani 1 1 d . . . . . H13A H -0.197394 0.178317 0.951942 0.056 Uiso 1 1 calc R U . . . H13B H -0.123399 0.105752 0.980184 0.056 Uiso 1 1 calc R U . . . H13C H -0.164984 0.101256 0.920241 0.056 Uiso 1 1 calc R U . . . C14 C -0.06346(18) 0.23517(15) 0.84533(11) 0.0406(5) Uani 1 1 d . . . . . H14A H 0.003606 0.259835 0.819526 0.061 Uiso 1 1 calc R U . . . H14B H -0.115408 0.278777 0.855000 0.061 Uiso 1 1 calc R U . . . H14C H -0.094654 0.200360 0.824038 0.061 Uiso 1 1 calc R U . . . C15 C 0.34938(17) 0.07718(15) 0.91026(11) 0.0397(5) Uani 1 1 d . . . . . H15 H 0.346531 0.124116 0.931381 0.048 Uiso 1 1 calc R U . . . C16 C 0.3747(3) -0.0008(2) 0.95345(17) 0.0704(9) Uani 1 1 d . . . . . H16A H 0.373884 -0.048384 0.934745 0.106 Uiso 1 1 calc R U . . . H16B H 0.319988 -0.007894 0.991125 0.106 Uiso 1 1 calc R U . . . H16C H 0.446602 0.003696 0.962193 0.106 Uiso 1 1 calc R U . . . C17 C 0.4385(2) 0.0955(2) 0.85268(14) 0.0701(10) Uani 1 1 d . . . . . H17A H 0.447491 0.048179 0.832921 0.105 Uiso 1 1 calc R U . . . H17B H 0.506931 0.105799 0.863302 0.105 Uiso 1 1 calc R U . . . H17C H 0.417755 0.144059 0.825076 0.105 Uiso 1 1 calc R U . . . C18 C 0.38030(16) 0.39520(13) 0.92621(8) 0.0283(4) Uani 1 1 d . . . . . C19 C 0.35206(18) 0.47704(14) 0.93020(9) 0.0344(4) Uani 1 1 d . . . . . C20 C 0.4354(2) 0.53465(16) 0.91400(11) 0.0454(6) Uani 1 1 d . . . . . H20 H 0.418431 0.590631 0.915365 0.054 Uiso 1 1 calc R U . . . C21 C 0.5420(2) 0.51142(18) 0.89610(12) 0.0503(6) Uani 1 1 d . . . . . H21 H 0.597693 0.551185 0.886118 0.060 Uiso 1 1 calc R U . . . C22 C 0.56798(18) 0.43090(17) 0.89260(11) 0.0429(5) Uani 1 1 d . . . . . H22 H 0.641854 0.415872 0.880522 0.051 Uiso 1 1 calc R U . . . C23 C 0.48836(16) 0.37089(14) 0.90638(9) 0.0319(4) Uani 1 1 d . . . . . C24 C 0.23611(18) 0.50493(14) 0.95136(10) 0.0359(5) Uani 1 1 d . . . . . H24 H 0.189657 0.454959 0.966392 0.043 Uiso 1 1 calc R U . . . C25 C 0.2260(2) 0.55117(17) 1.00350(11) 0.0475(6) Uani 1 1 d . . . . . H25A H 0.269181 0.601391 0.989362 0.071 Uiso 1 1 calc R U . . . H25B H 0.252627 0.515882 1.037128 0.071 Uiso 1 1 calc R U . . . H25C H 0.149757 0.565638 1.017129 0.071 Uiso 1 1 calc R U . . . C26 C 0.1944(2) 0.55883(14) 0.89849(10) 0.0400(5) Uani 1 1 d . . . . . H26A H 0.239975 0.607623 0.882376 0.060 Uiso 1 1 calc R U . . . H26B H 0.119382 0.575827 0.912489 0.060 Uiso 1 1 calc R U . . . H26C H 0.197193 0.527580 0.866700 0.060 Uiso 1 1 calc R U . . . C27 C 0.51836(16) 0.28247(14) 0.90098(10) 0.0344(5) Uani 1 1 d . . . . . H27 H 0.455989 0.259102 0.889767 0.041 Uiso 1 1 calc R U . . . C28 C 0.5349(2) 0.22904(19) 0.96109(12) 0.0553(7) Uani 1 1 d . . . . . H28A H 0.557811 0.173611 0.955188 0.083 Uiso 1 1 calc R U . . . H28B H 0.466616 0.225999 0.991022 0.083 Uiso 1 1 calc R U . . . H28C H 0.590833 0.253368 0.975496 0.083 Uiso 1 1 calc R U . . . C29 C 0.61837(18) 0.27555(17) 0.85173(11) 0.0451(6) Uani 1 1 d . . . . . H29A H 0.628183 0.218331 0.846889 0.068 Uiso 1 1 calc R U . . . H29B H 0.682530 0.293136 0.863177 0.068 Uiso 1 1 calc R U . . . H29C H 0.608574 0.310723 0.813505 0.068 Uiso 1 1 calc R U . . . C30 C 0.40615(14) 0.24778(12) 0.54512(8) 0.0244(4) Uani 1 1 d . . . . . C31 C 0.36392(15) 0.31182(12) 0.50679(8) 0.0269(4) Uani 1 1 d . . . . . H31 H 0.394185 0.316916 0.464936 0.032 Uiso 1 1 calc R U . . . C32 C 0.28330(16) 0.36956(14) 0.52134(8) 0.0306(4) Uani 1 1 d . . . . . C33 C 0.47873(17) 0.18565(12) 0.51706(9) 0.0310(4) Uani 1 1 d . . . . . H33A H 0.478477 0.195280 0.473811 0.046 Uiso 1 1 calc R U . . . H33B H 0.452283 0.130187 0.536536 0.046 Uiso 1 1 calc R U . . . H33C H 0.552799 0.190947 0.522512 0.046 Uiso 1 1 calc R U . . . C34 C 0.2365(2) 0.41717(18) 0.46917(10) 0.0489(7) Uani 1 1 d . . . . . H34A H 0.286051 0.461423 0.446064 0.073 Uiso 1 1 calc R U . . . H34B H 0.166056 0.440803 0.484740 0.073 Uiso 1 1 calc R U . . . H34C H 0.227118 0.380164 0.442849 0.073 Uiso 1 1 calc R U . . . C35 C 0.40262(15) 0.16094(12) 0.64338(8) 0.0257(4) Uani 1 1 d . . . . . C36 C 0.50165(15) 0.14408(12) 0.66235(8) 0.0256(4) Uani 1 1 d . . . . . C37 C 0.51315(17) 0.06789(13) 0.69980(9) 0.0305(4) Uani 1 1 d . . . . . H37 H 0.579616 0.054479 0.712834 0.037 Uiso 1 1 calc R U . . . C38 C 0.42994(18) 0.01156(13) 0.71833(9) 0.0335(4) Uani 1 1 d . . . . . H38 H 0.439514 -0.039715 0.744064 0.040 Uiso 1 1 calc R U . . . C39 C 0.33262(18) 0.02962(13) 0.69951(9) 0.0342(4) Uani 1 1 d . . . . . H39 H 0.275824 -0.009427 0.712658 0.041 Uiso 1 1 calc R U . . . C40 C 0.31693(16) 0.10421(13) 0.66158(9) 0.0301(4) Uani 1 1 d . . . . . C41 C 0.59363(15) 0.20524(12) 0.64472(9) 0.0269(4) Uani 1 1 d . . . . . H41 H 0.573728 0.252933 0.614543 0.032 Uiso 1 1 calc R U . . . C42 C 0.70054(16) 0.16868(13) 0.61565(10) 0.0325(4) Uani 1 1 d . . . . . H42A H 0.690925 0.149502 0.579853 0.049 Uiso 1 1 calc R U . . . H42B H 0.722372 0.122310 0.644710 0.049 Uiso 1 1 calc R U . . . H42C H 0.756809 0.210794 0.603751 0.049 Uiso 1 1 calc R U . . . C43 C 0.60767(17) 0.23733(14) 0.70012(10) 0.0361(5) Uani 1 1 d . . . . . H43A H 0.661601 0.281191 0.687505 0.054 Uiso 1 1 calc R U . . . H43B H 0.632238 0.192306 0.729177 0.054 Uiso 1 1 calc R U . . . H43C H 0.538133 0.258986 0.719072 0.054 Uiso 1 1 calc R U . . . C44 C 0.21048(17) 0.12223(14) 0.63964(10) 0.0367(5) Uani 1 1 d . . . . . H44 H 0.203553 0.183138 0.626357 0.044 Uiso 1 1 calc R U . . . C45 C 0.2109(2) 0.08297(16) 0.58500(12) 0.0472(6) Uani 1 1 d . . . . . H45A H 0.140268 0.092190 0.573338 0.071 Uiso 1 1 calc R U . . . H45B H 0.224886 0.023758 0.595803 0.071 Uiso 1 1 calc R U . . . H45C H 0.267850 0.107959 0.551063 0.071 Uiso 1 1 calc R U . . . C46 C 0.11147(19) 0.09263(19) 0.68892(13) 0.0549(7) Uani 1 1 d . . . . . H46A H 0.045459 0.106990 0.672894 0.082 Uiso 1 1 calc R U . . . H46B H 0.109391 0.119035 0.723221 0.082 Uiso 1 1 calc R U . . . H46C H 0.115971 0.032836 0.702291 0.082 Uiso 1 1 calc R U . . . C47 C 0.16124(15) 0.44331(14) 0.58768(8) 0.0300(4) Uani 1 1 d . . . . . C48 C 0.18499(17) 0.52738(14) 0.57161(9) 0.0346(5) Uani 1 1 d . . . . . C49 C 0.09938(18) 0.58300(15) 0.58217(10) 0.0396(5) Uani 1 1 d . . . . . H49 H 0.113552 0.640302 0.572194 0.048 Uiso 1 1 calc R U . . . C50 C -0.00518(18) 0.55617(16) 0.60680(11) 0.0420(5) Uani 1 1 d . . . . . H50 H -0.062301 0.595027 0.613014 0.050 Uiso 1 1 calc R U . . . C51 C -0.02724(17) 0.47343(16) 0.62243(10) 0.0389(5) Uani 1 1 d . . . . . H51 H -0.099626 0.455828 0.639479 0.047 Uiso 1 1 calc R U . . . C52 C 0.05501(16) 0.41481(14) 0.61366(9) 0.0321(4) Uani 1 1 d . . . . . C53 C 0.29729(19) 0.56225(15) 0.54188(11) 0.0458(6) Uani 1 1 d . . . . . H53 H 0.347338 0.515518 0.533426 0.055 Uiso 1 1 calc R U . . . C54 C 0.2949(3) 0.6218(2) 0.48158(14) 0.0861(14) Uani 1 1 d . . . . . H54A H 0.369338 0.635980 0.460063 0.129 Uiso 1 1 calc R U . . . H54B H 0.254921 0.671873 0.489370 0.129 Uiso 1 1 calc R U . . . H54C H 0.259038 0.595540 0.456842 0.129 Uiso 1 1 calc R U . . . C55 C 0.3421(2) 0.60600(15) 0.58341(15) 0.0562(8) Uani 1 1 d . . . . . H55A H 0.415281 0.625898 0.563622 0.084 Uiso 1 1 calc R U . . . H55B H 0.345064 0.567476 0.621445 0.084 Uiso 1 1 calc R U . . . H55C H 0.294761 0.652644 0.591738 0.084 Uiso 1 1 calc R U . . . C56 C 0.02862(16) 0.32387(15) 0.62983(10) 0.0369(5) Uani 1 1 d . . . . . H56 H 0.092272 0.293885 0.643959 0.044 Uiso 1 1 calc R U . . . C57 C 0.0141(2) 0.29221(18) 0.57423(12) 0.0506(6) Uani 1 1 d . . . . . H57A H -0.043336 0.324049 0.556827 0.076 Uiso 1 1 calc R U . . . H57B H -0.005872 0.234062 0.586321 0.076 Uiso 1 1 calc R U . . . H57C H 0.082249 0.298337 0.544096 0.076 Uiso 1 1 calc R U . . . C58 C -0.07050(19) 0.30220(18) 0.68096(13) 0.0510(6) Uani 1 1 d . . . . . H58A H -0.135694 0.326441 0.667275 0.077 Uiso 1 1 calc R U . . . H58B H -0.061555 0.323957 0.715831 0.077 Uiso 1 1 calc R U . . . H58C H -0.077830 0.242318 0.692594 0.077 Uiso 1 1 calc R U . . . F12_1 F 0.29387(9) 0.30467(7) 0.35319(5) 0.0326(2) Uani 1 1 d . . . . . F13_1 F 0.28429(10) 0.46429(7) 0.31134(6) 0.0399(3) Uani 1 1 d . . . . . F14_1 F 0.19291(11) 0.52626(7) 0.21416(7) 0.0480(3) Uani 1 1 d . . . . . F15_1 F 0.10762(12) 0.42027(8) 0.16051(6) 0.0475(3) Uani 1 1 d . . . . . F16_1 F 0.10915(10) 0.25979(7) 0.20401(6) 0.0350(3) Uani 1 1 d . . . . . F22_1 F 0.16694(9) 0.04273(7) 0.42578(5) 0.0331(3) Uani 1 1 d . . . . . F23_1 F 0.32457(10) -0.02384(7) 0.47959(5) 0.0357(3) Uani 1 1 d . . . . . F24_1 F 0.53329(10) 0.03026(8) 0.43694(6) 0.0367(3) Uani 1 1 d . . . . . F25_1 F 0.57767(9) 0.15290(8) 0.33743(6) 0.0358(3) Uani 1 1 d . . . . . F26_1 F 0.42392(8) 0.21435(7) 0.27807(5) 0.0285(2) Uani 1 1 d . . . . . F32_1 F 0.11575(9) 0.21212(8) 0.42581(5) 0.0365(3) Uani 1 1 d . . . . . F33_1 F -0.08796(11) 0.21102(9) 0.48691(6) 0.0451(3) Uani 1 1 d . . . . . F34_1 F -0.25314(9) 0.17222(8) 0.43874(6) 0.0433(3) Uani 1 1 d . . . . . F35_1 F -0.20605(9) 0.12724(8) 0.32927(6) 0.0395(3) Uani 1 1 d . . . . . F36_1 F -0.00441(9) 0.11913(8) 0.27044(5) 0.0332(3) Uani 1 1 d . . . . . F41_1 F 0.13119(9) 0.00017(7) 0.32229(5) 0.0326(2) Uani 1 1 d . . . . . F42_1 F 0.17665(11) -0.09661(8) 0.24194(7) 0.0426(3) Uani 1 1 d . . . . . F43_1 F 0.29786(11) -0.04008(9) 0.12969(6) 0.0463(3) Uani 1 1 d . . . . . F44_1 F 0.37415(11) 0.11664(9) 0.10038(5) 0.0431(3) Uani 1 1 d . . . . . F45_1 F 0.32808(9) 0.21535(7) 0.17881(5) 0.0326(3) Uani 1 1 d . . . . . C11_1 C 0.20478(14) 0.27126(11) 0.27992(8) 0.0230(4) Uani 1 1 d . . . . . C12_1 C 0.24655(15) 0.32853(12) 0.30489(9) 0.0265(4) Uani 1 1 d . . . . . C13_1 C 0.24349(15) 0.41289(12) 0.28369(10) 0.0306(4) Uani 1 1 d . . . . . C14_1 C 0.19758(17) 0.44450(12) 0.23496(10) 0.0345(5) Uani 1 1 d . . . . . C15_1 C 0.15404(17) 0.39129(13) 0.20832(9) 0.0339(5) Uani 1 1 d . . . . . C16_1 C 0.15717(15) 0.30758(12) 0.23151(9) 0.0280(4) Uani 1 1 d . . . . . C21_1 C 0.28546(14) 0.13443(11) 0.34912(8) 0.0214(3) Uani 1 1 d . . . . . C22_1 C 0.26727(15) 0.07250(11) 0.40095(8) 0.0246(4) Uani 1 1 d . . . . . C23_1 C 0.34826(16) 0.03700(11) 0.43064(8) 0.0266(4) Uani 1 1 d . . . . . C24_1 C 0.45300(16) 0.06374(12) 0.40965(9) 0.0272(4) Uani 1 1 d . . . . . C25_1 C 0.47558(15) 0.12546(12) 0.35900(9) 0.0263(4) Uani 1 1 d . . . . . C26_1 C 0.39347(14) 0.15715(11) 0.32966(8) 0.0227(3) Uani 1 1 d . . . . . C31_1 C 0.06867(14) 0.16319(11) 0.34538(8) 0.0234(4) Uani 1 1 d . . . . . C32_1 C 0.03919(15) 0.18730(12) 0.40055(9) 0.0275(4) Uani 1 1 d . . . . . C33_1 C -0.06631(16) 0.18850(13) 0.43311(9) 0.0318(4) Uani 1 1 d . . . . . C34_1 C -0.14974(15) 0.16807(12) 0.40929(10) 0.0313(4) Uani 1 1 d . . . . . C35_1 C -0.12578(15) 0.14565(12) 0.35429(10) 0.0292(4) Uani 1 1 d . . . . . C36_1 C -0.01852(15) 0.14285(11) 0.32394(9) 0.0257(4) Uani 1 1 d . . . . . C41_1 C 0.22312(14) 0.11444(11) 0.25486(8) 0.0232(4) Uani 1 1 d . . . . . C42_1 C 0.19042(15) 0.03297(12) 0.26736(9) 0.0266(4) Uani 1 1 d . . . . . C43_1 C 0.21363(16) -0.01917(13) 0.22669(10) 0.0315(4) Uani 1 1 d . . . . . C44_1 C 0.27508(16) 0.00898(14) 0.17018(10) 0.0336(5) Uani 1 1 d . . . . . C45_1 C 0.31309(16) 0.08834(14) 0.15547(9) 0.0314(4) Uani 1 1 d . . . . . C46_1 C 0.28710(15) 0.13849(12) 0.19741(9) 0.0262(4) Uani 1 1 d . . . . . B1_1 B 0.19593(15) 0.17062(12) 0.30738(9) 0.0206(4) Uani 1 1 d . . . . . C1_2 C 0.6953(2) 0.20903(16) 0.13131(12) 0.0298(7) Uani 0.775(5) 1 d . . P B 3 C2_2 C 0.7381(4) 0.1998(2) 0.18263(16) 0.0326(8) Uani 0.775(5) 1 d . . P B 3 H2_2 H 0.691753 0.185238 0.221307 0.039 Uiso 0.775(5) 1 calc R U P B 3 C3_2 C 0.8476(3) 0.21135(19) 0.17844(14) 0.0376(7) Uani 0.775(5) 1 d . . P B 3 H3_2 H 0.875472 0.205074 0.214190 0.045 Uiso 0.775(5) 1 calc R U P B 3 C4_2 C 0.9160(2) 0.23182(18) 0.12303(16) 0.0394(8) Uani 0.775(5) 1 d . . P B 3 H4_2 H 0.990918 0.240397 0.120323 0.047 Uiso 0.775(5) 1 calc R U P B 3 C5_2 C 0.8752(3) 0.2398(2) 0.07132(17) 0.0394(8) Uani 0.775(5) 1 d . . P B 3 H5_2 H 0.922357 0.253333 0.032809 0.047 Uiso 0.775(5) 1 calc R U P B 3 C6_2 C 0.7662(3) 0.2283(4) 0.0753(2) 0.0334(10) Uani 0.775(5) 1 d . . P B 3 H6_2 H 0.739030 0.233617 0.039403 0.040 Uiso 0.775(5) 1 calc R U P B 3 C7_2 C 0.5760(3) 0.1984(2) 0.1363(2) 0.0435(8) Uani 0.775(5) 1 d . . P B 3 H7A_2 H 0.558881 0.213280 0.095963 0.065 Uiso 0.775(5) 1 calc R U P B 3 H7B_2 H 0.534886 0.234088 0.162009 0.065 Uiso 0.775(5) 1 calc R U P B 3 H7C_2 H 0.556520 0.140981 0.154071 0.065 Uiso 0.775(5) 1 calc R U P B 3 C1_3 C 0.8178(10) 0.2278(6) 0.1039(6) 0.042(3) Uani 0.225(5) 1 d . . P B 4 C2_3 C 0.7948(12) 0.2010(7) 0.1685(6) 0.033(2) Uani 0.225(5) 1 d . . P B 4 H2_3 H 0.851317 0.195242 0.190472 0.039 Uiso 0.225(5) 1 calc R U P B 4 C3_3 C 0.6899(11) 0.1839(8) 0.1974(6) 0.034(3) Uani 0.225(5) 1 d . . P B 4 H3_3 H 0.674861 0.164266 0.239964 0.041 Uiso 0.225(5) 1 calc R U P B 4 C6_3 C 0.7301(14) 0.2384(14) 0.0751(9) 0.041(4) Uani 0.225(5) 1 d . . P B 4 H6_3 H 0.742908 0.258665 0.032687 0.049 Uiso 0.225(5) 1 calc R U P B 4 C7_3 C 0.9301(14) 0.2468(11) 0.0706(8) 0.068(5) Uani 0.225(5) 1 d . . P B 4 H7A_3 H 0.929979 0.296620 0.039194 0.102 Uiso 0.225(5) 1 calc R U P B 4 H7B_3 H 0.960232 0.200744 0.051750 0.102 Uiso 0.225(5) 1 calc R U P B 4 H7C_3 H 0.974458 0.255672 0.098619 0.102 Uiso 0.225(5) 1 calc R U P B 4 C5_3 C 0.6256(10) 0.2204(6) 0.1062(5) 0.036(2) Uani 0.225(5) 1 d . . P B 4 H5_3 H 0.567629 0.226242 0.085221 0.043 Uiso 0.225(5) 1 calc R U P B 4 C4_3 C 0.6061(9) 0.1939(6) 0.1681(5) 0.034(2) Uani 0.225(5) 1 d . . P B 4 H4_3 H 0.534120 0.182519 0.190206 0.040 Uiso 0.225(5) 1 calc R U P B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0160(3) 0.0219(4) 0.0177(2) -0.0058(3) -0.0036(2) 0.0008(2) Ga2 0.0166(3) 0.0179(3) 0.0175(2) -0.0052(3) -0.00243(18) 0.0030(2) Cl1 0.0196(3) 0.0250(3) 0.0304(4) -0.0097(3) -0.0047(3) 0.0060(2) Cl2 0.0232(4) 0.0239(4) 0.0291(4) -0.0091(3) 0.0011(3) -0.0049(3) P1 0.0165(3) 0.0200(3) 0.0187(3) -0.0058(2) -0.0031(2) 0.0012(2) P2 0.0220(3) 0.0224(3) 0.0186(3) -0.0062(2) -0.0013(2) -0.0043(2) N5 0.0252(17) 0.0271(15) 0.027(2) -0.0086(11) -0.0031(13) -0.0094(13) N6 0.0240(17) 0.0174(16) 0.0251(18) -0.0035(13) -0.0059(12) 0.0009(13) C59 0.0189(14) 0.0220(14) 0.0213(14) -0.0067(11) -0.0034(11) -0.0017(11) C60 0.039(2) 0.0240(18) 0.027(5) -0.0028(17) 0.001(3) -0.0088(15) C61 0.046(3) 0.019(2) 0.036(4) -0.003(3) -0.012(3) 0.0014(17) C62 0.0213(18) 0.049(2) 0.042(2) -0.0136(16) -0.0054(14) -0.0094(15) C63 0.0228(15) 0.0284(16) 0.0318(16) -0.0078(13) -0.0102(12) 0.0049(12) C64 0.071(3) 0.034(3) 0.067(5) -0.010(3) -0.002(3) -0.027(3) C65 0.062(3) 0.020(2) 0.049(3) -0.0018(17) -0.015(2) 0.0074(19) Ga1' 0.0200(10) 0.0268(12) 0.0177(6) -0.0045(8) -0.0047(6) -0.0004(7) Ga2' 0.0201(8) 0.0193(10) 0.0171(6) -0.0054(7) -0.0030(5) 0.0041(6) Cl1' 0.0263(11) 0.0266(9) 0.0305(12) -0.0091(9) -0.0078(9) 0.0069(8) Cl2' 0.0210(11) 0.0235(10) 0.0325(13) -0.0065(9) 0.0006(9) -0.0023(8) P1' 0.0261(9) 0.0213(9) 0.0207(8) -0.0057(6) -0.0044(6) 0.0075(6) P2' 0.0183(8) 0.0183(8) 0.0174(8) -0.0050(6) -0.0027(6) 0.0009(6) N5' 0.019(4) 0.025(4) 0.026(5) -0.013(3) -0.008(3) 0.003(3) N6' 0.023(4) 0.021(4) 0.022(5) -0.006(3) -0.005(3) 0.009(3) C59' 0.016(3) 0.014(3) 0.023(4) -0.001(3) -0.003(3) 0.000(3) C60' 0.041(6) 0.018(4) 0.014(9) -0.005(4) 0.000(7) -0.007(3) C61' 0.033(5) 0.017(5) 0.030(7) -0.009(7) -0.002(5) -0.001(4) C62' 0.024(5) 0.035(5) 0.032(4) -0.004(4) -0.010(4) -0.001(4) C63' 0.022(4) 0.036(5) 0.032(5) -0.014(4) -0.011(3) 0.005(3) C64' 0.039(6) 0.026(7) 0.061(11) -0.014(6) -0.010(7) -0.004(5) C65' 0.062(7) 0.028(6) 0.066(10) -0.015(5) -0.028(7) 0.023(5) N1 0.0209(7) 0.0317(8) 0.0245(8) -0.0107(6) -0.0034(6) 0.0016(6) N2 0.0220(7) 0.0364(9) 0.0202(7) -0.0084(6) -0.0064(6) -0.0002(6) N3 0.0187(7) 0.0286(8) 0.0207(7) -0.0026(6) -0.0031(6) 0.0004(6) N4 0.0218(7) 0.0413(9) 0.0195(7) -0.0062(7) -0.0047(6) 0.0106(7) C1 0.0263(9) 0.0309(10) 0.0251(9) -0.0073(8) -0.0032(7) 0.0053(8) C2 0.0306(10) 0.0373(11) 0.0185(8) -0.0072(8) -0.0046(7) 0.0030(8) C3 0.0261(9) 0.0374(11) 0.0210(9) -0.0096(8) -0.0070(7) 0.0068(8) C4 0.0558(14) 0.0325(11) 0.0293(11) -0.0040(9) -0.0078(10) -0.0009(10) C5 0.0412(12) 0.0466(13) 0.0239(10) -0.0103(9) -0.0124(9) -0.0021(10) C6 0.0261(9) 0.0323(10) 0.0238(9) -0.0105(8) -0.0013(7) 0.0001(8) C7 0.0255(9) 0.0324(10) 0.0267(9) -0.0088(8) -0.0005(7) -0.0027(8) C8 0.0313(10) 0.0395(12) 0.0341(11) -0.0130(9) -0.0037(8) -0.0065(9) C9 0.0424(12) 0.0400(12) 0.0371(12) -0.0196(10) -0.0010(9) -0.0049(10) C10 0.0367(11) 0.0398(12) 0.0392(12) -0.0191(10) -0.0009(9) 0.0062(9) C11 0.0281(10) 0.0404(11) 0.0311(10) -0.0153(9) -0.0026(8) 0.0042(8) C12 0.0237(9) 0.0321(10) 0.0369(11) -0.0122(8) -0.0064(8) -0.0021(8) C13 0.0265(10) 0.0442(12) 0.0425(12) -0.0182(10) 0.0009(9) -0.0040(9) C14 0.0314(11) 0.0440(13) 0.0467(13) -0.0050(10) -0.0122(10) -0.0028(9) C15 0.0290(10) 0.0520(14) 0.0446(13) -0.0262(11) -0.0086(9) 0.0115(10) C16 0.0619(19) 0.0630(19) 0.099(3) -0.0211(18) -0.0462(18) 0.0213(15) C17 0.0274(12) 0.128(3) 0.0656(19) -0.054(2) 0.0004(12) 0.0021(15) C18 0.0262(9) 0.0398(11) 0.0218(9) -0.0086(8) -0.0079(7) -0.0041(8) C19 0.0358(11) 0.0419(12) 0.0285(10) -0.0125(9) -0.0070(8) -0.0029(9) C20 0.0496(14) 0.0448(13) 0.0439(13) -0.0171(11) -0.0038(11) -0.0119(11) C21 0.0424(13) 0.0610(16) 0.0510(15) -0.0208(13) -0.0029(11) -0.0216(12) C22 0.0274(11) 0.0639(16) 0.0410(12) -0.0173(11) -0.0064(9) -0.0086(10) C23 0.0245(9) 0.0480(12) 0.0267(10) -0.0104(9) -0.0098(8) -0.0021(8) C24 0.0390(11) 0.0390(12) 0.0314(11) -0.0138(9) -0.0056(9) 0.0027(9) C25 0.0547(15) 0.0551(15) 0.0371(12) -0.0209(11) -0.0093(11) 0.0075(12) C26 0.0508(13) 0.0363(12) 0.0368(12) -0.0143(9) -0.0122(10) 0.0041(10) C27 0.0219(9) 0.0493(13) 0.0343(11) -0.0104(9) -0.0100(8) 0.0046(9) C28 0.0498(15) 0.0716(19) 0.0413(14) -0.0051(13) -0.0140(11) 0.0212(13) C29 0.0268(11) 0.0625(16) 0.0464(13) -0.0158(12) -0.0057(10) 0.0075(10) C30 0.0209(8) 0.0284(9) 0.0243(9) -0.0067(7) -0.0037(7) -0.0018(7) C31 0.0268(9) 0.0338(10) 0.0189(8) -0.0063(7) -0.0021(7) 0.0040(8) C32 0.0286(10) 0.0431(12) 0.0191(9) -0.0055(8) -0.0055(7) 0.0077(8) C33 0.0388(11) 0.0282(10) 0.0265(10) -0.0084(8) -0.0063(8) 0.0043(8) C34 0.0525(14) 0.0707(17) 0.0224(10) -0.0111(10) -0.0122(10) 0.0333(13) C35 0.0249(9) 0.0290(10) 0.0211(8) -0.0033(7) -0.0023(7) 0.0009(7) C36 0.0245(9) 0.0292(9) 0.0219(9) -0.0062(7) -0.0020(7) 0.0026(7) C37 0.0319(10) 0.0332(10) 0.0266(9) -0.0059(8) -0.0083(8) 0.0060(8) C38 0.0400(11) 0.0315(10) 0.0258(10) -0.0004(8) -0.0053(8) 0.0011(9) C39 0.0343(11) 0.0350(11) 0.0295(10) -0.0011(8) -0.0021(8) -0.0072(9) C40 0.0265(9) 0.0356(11) 0.0262(9) -0.0035(8) -0.0027(7) -0.0045(8) C41 0.0213(9) 0.0291(10) 0.0300(10) -0.0066(8) -0.0056(7) 0.0047(7) C42 0.0246(9) 0.0342(11) 0.0355(11) -0.0060(9) -0.0017(8) 0.0055(8) C43 0.0283(10) 0.0418(12) 0.0427(12) -0.0165(10) -0.0107(9) 0.0045(9) C44 0.0274(10) 0.0413(12) 0.0390(12) 0.0006(9) -0.0080(9) -0.0086(9) C45 0.0465(14) 0.0456(14) 0.0547(15) -0.0067(11) -0.0228(12) -0.0091(11) C46 0.0283(12) 0.0715(19) 0.0560(16) 0.0046(14) -0.0038(11) -0.0121(12) C47 0.0237(9) 0.0471(12) 0.0193(9) -0.0085(8) -0.0067(7) 0.0135(8) C48 0.0289(10) 0.0472(12) 0.0228(9) -0.0037(8) -0.0012(8) 0.0143(9) C49 0.0363(11) 0.0471(13) 0.0328(11) -0.0103(10) -0.0035(9) 0.0162(10) C50 0.0290(11) 0.0596(15) 0.0422(12) -0.0250(11) -0.0089(9) 0.0209(10) C51 0.0207(9) 0.0616(15) 0.0410(12) -0.0261(11) -0.0086(8) 0.0116(9) C52 0.0230(9) 0.0516(13) 0.0271(10) -0.0170(9) -0.0106(8) 0.0087(9) C53 0.0368(12) 0.0415(13) 0.0401(12) 0.0103(10) 0.0119(10) 0.0143(10) C54 0.077(2) 0.074(2) 0.0594(18) 0.0358(16) 0.0313(16) 0.0435(18) C55 0.0343(12) 0.0318(12) 0.089(2) -0.0055(13) 0.0107(13) -0.0019(10) C56 0.0221(9) 0.0542(14) 0.0399(12) -0.0174(10) -0.0120(8) 0.0050(9) C57 0.0475(14) 0.0628(17) 0.0540(15) -0.0282(13) -0.0233(12) 0.0050(12) C58 0.0289(11) 0.0674(17) 0.0578(16) -0.0188(13) -0.0038(11) -0.0055(11) F12_1 0.0349(6) 0.0299(6) 0.0359(6) -0.0116(5) -0.0098(5) 0.0029(5) F13_1 0.0336(6) 0.0281(6) 0.0560(8) -0.0164(6) 0.0033(6) -0.0028(5) F14_1 0.0500(8) 0.0228(6) 0.0565(8) 0.0053(6) 0.0070(6) 0.0034(5) F15_1 0.0561(8) 0.0397(7) 0.0395(7) 0.0073(6) -0.0128(6) 0.0137(6) F16_1 0.0348(6) 0.0336(6) 0.0386(7) -0.0034(5) -0.0175(5) 0.0058(5) F22_1 0.0257(6) 0.0347(6) 0.0334(6) 0.0049(5) -0.0042(5) -0.0054(5) F23_1 0.0431(7) 0.0319(6) 0.0292(6) 0.0041(5) -0.0118(5) 0.0027(5) F24_1 0.0327(6) 0.0410(7) 0.0395(7) -0.0047(5) -0.0210(5) 0.0115(5) F25_1 0.0180(5) 0.0384(7) 0.0503(7) -0.0037(6) -0.0105(5) 0.0008(5) F26_1 0.0191(5) 0.0305(6) 0.0310(6) 0.0025(5) -0.0030(4) 0.0000(4) F32_1 0.0277(6) 0.0497(7) 0.0352(6) -0.0194(6) -0.0021(5) -0.0014(5) F33_1 0.0372(7) 0.0555(8) 0.0375(7) -0.0162(6) 0.0093(5) 0.0033(6) F34_1 0.0197(6) 0.0413(7) 0.0559(8) -0.0002(6) 0.0105(5) 0.0038(5) F35_1 0.0169(5) 0.0418(7) 0.0583(8) -0.0050(6) -0.0101(5) 0.0004(5) F36_1 0.0221(5) 0.0417(7) 0.0386(6) -0.0113(5) -0.0100(5) 0.0024(5) F41_1 0.0337(6) 0.0254(6) 0.0360(6) -0.0038(5) -0.0044(5) 0.0009(5) F42_1 0.0457(7) 0.0298(6) 0.0593(8) -0.0187(6) -0.0176(6) 0.0032(5) F43_1 0.0431(7) 0.0594(9) 0.0501(8) -0.0370(7) -0.0185(6) 0.0160(6) F44_1 0.0399(7) 0.0606(9) 0.0280(6) -0.0158(6) -0.0005(5) 0.0089(6) F45_1 0.0304(6) 0.0355(6) 0.0275(6) -0.0051(5) 0.0020(5) 0.0001(5) C11_1 0.0152(8) 0.0235(9) 0.0267(9) -0.0037(7) 0.0016(7) 0.0031(6) C12_1 0.0199(8) 0.0270(9) 0.0293(9) -0.0059(7) 0.0016(7) 0.0030(7) C13_1 0.0225(9) 0.0248(9) 0.0401(11) -0.0102(8) 0.0066(8) -0.0003(7) C14_1 0.0301(10) 0.0207(9) 0.0405(11) 0.0028(8) 0.0096(9) 0.0037(8) C15_1 0.0309(10) 0.0310(10) 0.0318(10) 0.0039(8) -0.0015(8) 0.0087(8) C16_1 0.0231(9) 0.0272(10) 0.0304(10) -0.0024(8) -0.0026(7) 0.0035(7) C21_1 0.0203(8) 0.0209(8) 0.0235(8) -0.0062(7) -0.0047(7) 0.0027(6) C22_1 0.0220(9) 0.0256(9) 0.0259(9) -0.0053(7) -0.0038(7) -0.0008(7) C23_1 0.0345(10) 0.0225(9) 0.0231(9) -0.0034(7) -0.0087(8) 0.0033(7) C24_1 0.0277(9) 0.0285(10) 0.0300(10) -0.0094(8) -0.0147(8) 0.0093(8) C25_1 0.0185(8) 0.0272(9) 0.0351(10) -0.0092(8) -0.0073(7) 0.0029(7) C26_1 0.0218(8) 0.0207(8) 0.0246(9) -0.0033(7) -0.0042(7) 0.0021(7) C31_1 0.0175(8) 0.0207(8) 0.0296(9) -0.0025(7) -0.0025(7) 0.0028(6) C32_1 0.0217(9) 0.0267(9) 0.0324(10) -0.0064(8) -0.0017(7) 0.0012(7) C33_1 0.0274(10) 0.0301(10) 0.0322(10) -0.0054(8) 0.0047(8) 0.0039(8) C34_1 0.0187(9) 0.0232(9) 0.0425(11) 0.0024(8) 0.0050(8) 0.0035(7) C35_1 0.0167(8) 0.0231(9) 0.0442(11) 0.0014(8) -0.0064(8) 0.0011(7) C36_1 0.0203(9) 0.0225(9) 0.0322(10) -0.0032(7) -0.0041(7) 0.0037(7) C41_1 0.0163(8) 0.0282(9) 0.0262(9) -0.0063(7) -0.0080(7) 0.0066(7) C42_1 0.0208(8) 0.0282(9) 0.0325(10) -0.0072(8) -0.0099(7) 0.0064(7) C43_1 0.0264(9) 0.0294(10) 0.0440(12) -0.0124(9) -0.0164(9) 0.0076(8) C44_1 0.0285(10) 0.0427(12) 0.0394(11) -0.0238(9) -0.0174(9) 0.0144(9) C45_1 0.0236(9) 0.0456(12) 0.0262(9) -0.0109(9) -0.0066(7) 0.0089(8) C46_1 0.0204(8) 0.0303(10) 0.0287(9) -0.0063(8) -0.0077(7) 0.0056(7) B1_1 0.0157(8) 0.0218(9) 0.0239(9) -0.0043(7) -0.0041(7) 0.0029(7) C1_2 0.0278(13) 0.0258(13) 0.0372(14) -0.0118(10) -0.0056(11) 0.0029(10) C2_2 0.032(2) 0.0310(18) 0.0336(19) -0.0058(14) -0.0062(17) 0.004(2) C3_2 0.0376(19) 0.0367(16) 0.0435(16) -0.0115(13) -0.0192(14) 0.0106(13) C4_2 0.0244(13) 0.0387(16) 0.060(2) -0.0222(14) -0.0098(13) 0.0087(11) C5_2 0.0347(18) 0.0416(18) 0.0385(17) -0.0159(14) 0.0064(16) 0.0026(16) C6_2 0.038(2) 0.039(2) 0.0268(15) -0.0152(13) -0.0072(17) 0.006(2) C7_2 0.0310(17) 0.0452(19) 0.055(2) -0.0128(17) -0.0085(17) -0.0014(14) C1_3 0.037(5) 0.027(5) 0.059(6) -0.021(4) 0.008(5) -0.001(4) C2_3 0.023(6) 0.029(5) 0.053(5) -0.014(4) -0.016(5) -0.002(5) C3_3 0.038(6) 0.029(6) 0.037(6) -0.012(5) -0.010(4) 0.007(5) C6_3 0.051(7) 0.030(7) 0.042(6) -0.018(5) 0.000(5) 0.002(7) C7_3 0.050(7) 0.068(9) 0.080(11) -0.036(8) 0.022(8) -0.012(8) C5_3 0.041(5) 0.034(5) 0.036(5) -0.011(4) -0.010(4) -0.002(4) C4_3 0.035(5) 0.029(5) 0.040(5) -0.011(4) -0.011(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.9261(19) . ? Ga1 N1 1.983(2) . ? Ga1 Cl1 2.2021(10) . ? Ga1 P1 2.3479(13) . ? Ga2 N3 1.8686(18) . ? Ga2 N4 1.9669(18) . ? Ga2 Cl2 2.2074(10) . ? Ga2 P2 2.3456(10) . ? P1 C59 1.823(3) . ? P1 P2 2.1423(8) . ? N5 C59 1.346(4) . ? N5 C60 1.377(7) . ? N5 C62 1.466(5) . ? N6 C59 1.353(4) . ? N6 C61 1.383(7) . ? N6 C63 1.461(4) . ? C60 C61 1.355(7) . ? C60 C64 1.494(6) . ? C61 C65 1.498(7) . ? Ga1' N1 1.768(4) . ? Ga1' N2 2.017(4) . ? Ga1' Cl1' 2.200(3) . ? Ga1' P1' 2.341(3) . ? Ga2' N4 1.917(3) . ? Ga2' N3 2.117(3) . ? Ga2' Cl2' 2.208(3) . ? Ga2' P2' 2.345(3) . ? P1' P2' 2.135(2) . ? P2' C59' 1.846(7) . ? N5' C59' 1.341(9) . ? N5' C60' 1.397(12) . ? N5' C62' 1.460(10) . ? N6' C59' 1.332(9) . ? N6' C61' 1.384(13) . ? N6' C63' 1.462(10) . ? C60' C61' 1.359(15) . ? C60' C64' 1.491(13) . ? C61' C65' 1.494(12) . ? N1 C1 1.337(2) . ? N1 C6 1.449(2) . ? N2 C3 1.342(2) . ? N2 C18 1.449(2) . ? N3 C30 1.338(2) . ? N3 C35 1.452(2) . ? N4 C32 1.337(2) . ? N4 C47 1.450(2) . ? C1 C2 1.402(3) . ? C1 C4 1.504(3) . ? C2 C3 1.395(3) . ? C3 C5 1.511(3) . ? C6 C7 1.403(3) . ? C6 C11 1.404(3) . ? C7 C8 1.396(3) . ? C7 C12 1.513(3) . ? C8 C9 1.378(3) . ? C9 C10 1.383(3) . ? C10 C11 1.393(3) . ? C11 C15 1.526(3) . ? C12 C13 1.530(3) . ? C12 C14 1.534(3) . ? C15 C16 1.526(4) . ? C15 C17 1.536(4) . ? C18 C19 1.406(3) . ? C18 C23 1.409(3) . ? C19 C20 1.399(3) . ? C19 C24 1.521(3) . ? C20 C21 1.379(4) . ? C21 C22 1.377(4) . ? C22 C23 1.395(3) . ? C23 C27 1.523(3) . ? C24 C26 1.529(3) . ? C24 C25 1.542(3) . ? C27 C29 1.527(3) . ? C27 C28 1.533(3) . ? C30 C31 1.395(3) . ? C30 C33 1.502(3) . ? C31 C32 1.398(3) . ? C32 C34 1.511(3) . ? C35 C36 1.405(3) . ? C35 C40 1.409(3) . ? C36 C37 1.397(3) . ? C36 C41 1.517(3) . ? C37 C38 1.382(3) . ? C38 C39 1.385(3) . ? C39 C40 1.392(3) . ? C40 C44 1.527(3) . ? C41 C42 1.529(3) . ? C41 C43 1.534(3) . ? C44 C46 1.526(3) . ? C44 C45 1.539(3) . ? C47 C48 1.401(3) . ? C47 C52 1.410(3) . ? C48 C49 1.399(3) . ? C48 C53 1.524(3) . ? C49 C50 1.379(3) . ? C50 C51 1.376(4) . ? C51 C52 1.398(3) . ? C52 C56 1.518(3) . ? C53 C55 1.531(4) . ? C53 C54 1.537(3) . ? C56 C58 1.528(3) . ? C56 C57 1.537(3) . ? F12_1 C12_1 1.354(2) . ? F13_1 C13_1 1.350(2) . ? F14_1 C14_1 1.347(2) . ? F15_1 C15_1 1.349(2) . ? F16_1 C16_1 1.354(2) . ? F22_1 C22_1 1.348(2) . ? F23_1 C23_1 1.343(2) . ? F24_1 C24_1 1.341(2) . ? F25_1 C25_1 1.346(2) . ? F26_1 C26_1 1.358(2) . ? F32_1 C32_1 1.353(2) . ? F33_1 C33_1 1.344(2) . ? F34_1 C34_1 1.343(2) . ? F35_1 C35_1 1.346(2) . ? F36_1 C36_1 1.350(2) . ? F41_1 C42_1 1.349(2) . ? F42_1 C43_1 1.344(2) . ? F43_1 C44_1 1.345(2) . ? F44_1 C45_1 1.345(2) . ? F45_1 C46_1 1.354(2) . ? C11_1 C12_1 1.391(3) . ? C11_1 C16_1 1.394(3) . ? C11_1 B1_1 1.662(3) . ? C12_1 C13_1 1.387(3) . ? C13_1 C14_1 1.370(3) . ? C14_1 C15_1 1.375(3) . ? C15_1 C16_1 1.385(3) . ? C21_1 C26_1 1.388(2) . ? C21_1 C22_1 1.393(3) . ? C21_1 B1_1 1.648(3) . ? C22_1 C23_1 1.388(3) . ? C23_1 C24_1 1.371(3) . ? C24_1 C25_1 1.375(3) . ? C25_1 C26_1 1.379(2) . ? C31_1 C36_1 1.383(3) . ? C31_1 C32_1 1.388(3) . ? C31_1 B1_1 1.656(3) . ? C32_1 C33_1 1.384(3) . ? C33_1 C34_1 1.375(3) . ? C34_1 C35_1 1.369(3) . ? C35_1 C36_1 1.389(3) . ? C41_1 C46_1 1.390(3) . ? C41_1 C42_1 1.391(3) . ? C41_1 B1_1 1.654(3) . ? C42_1 C43_1 1.387(3) . ? C43_1 C44_1 1.371(3) . ? C44_1 C45_1 1.378(3) . ? C45_1 C46_1 1.386(3) . ? C1_2 C2_2 1.382(4) . ? C1_2 C6_2 1.394(5) . ? C1_2 C7_2 1.502(4) . ? C2_2 C3_2 1.385(5) . ? C3_2 C4_2 1.372(5) . ? C4_2 C5_2 1.379(5) . ? C5_2 C6_2 1.380(6) . ? C1_3 C6_3 1.39(2) . ? C1_3 C2_3 1.436(19) . ? C1_3 C7_3 1.477(17) . ? C2_3 C3_3 1.366(17) . ? C3_3 C4_3 1.358(18) . ? C6_3 C5_3 1.38(2) . ? C5_3 C4_3 1.380(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 96.57(8) . . ? N2 Ga1 Cl1 106.28(6) . . ? N1 Ga1 Cl1 105.95(7) . . ? N2 Ga1 P1 112.02(7) . . ? N1 Ga1 P1 118.73(6) . . ? Cl1 Ga1 P1 115.17(6) . . ? N3 Ga2 N4 99.03(8) . . ? N3 Ga2 Cl2 105.72(6) . . ? N4 Ga2 Cl2 101.77(6) . . ? N3 Ga2 P2 108.10(6) . . ? N4 Ga2 P2 124.00(6) . . ? Cl2 Ga2 P2 115.82(5) . . ? C59 P1 P2 110.32(11) . . ? C59 P1 Ga1 102.17(9) . . ? P2 P1 Ga1 110.25(4) . . ? P1 P2 Ga2 100.12(3) . . ? C59 N5 C60 110.9(4) . . ? C59 N5 C62 125.8(4) . . ? C60 N5 C62 123.1(4) . . ? C59 N6 C61 109.6(4) . . ? C59 N6 C63 127.3(3) . . ? C61 N6 C63 123.2(4) . . ? N5 C59 N6 105.9(3) . . ? N5 C59 P1 123.5(3) . . ? N6 C59 P1 130.6(3) . . ? C61 C60 N5 106.2(5) . . ? C61 C60 C64 131.4(7) . . ? N5 C60 C64 122.4(6) . . ? C60 C61 N6 107.4(4) . . ? C60 C61 C65 130.6(6) . . ? N6 C61 C65 122.0(6) . . ? N1 Ga1' N2 100.68(17) . . ? N1 Ga1' Cl1' 105.36(17) . . ? N2 Ga1' Cl1' 100.29(11) . . ? N1 Ga1' P1' 107.46(13) . . ? N2 Ga1' P1' 125.22(16) . . ? Cl1' Ga1' P1' 115.49(16) . . ? N4 Ga2' N3 92.52(12) . . ? N4 Ga2' Cl2' 110.39(12) . . ? N3 Ga2' Cl2' 106.93(13) . . ? N4 Ga2' P2' 112.60(13) . . ? N3 Ga2' P2' 119.24(10) . . ? Cl2' Ga2' P2' 113.26(13) . . ? P2' P1' Ga1' 100.40(10) . . ? C59' P2' P1' 110.1(3) . . ? C59' P2' Ga2' 100.7(3) . . ? P1' P2' Ga2' 109.56(10) . . ? C59' N5' C60' 109.2(9) . . ? C59' N5' C62' 128.5(10) . . ? C60' N5' C62' 122.1(11) . . ? C59' N6' C61' 110.8(8) . . ? C59' N6' C63' 126.0(9) . . ? C61' N6' C63' 123.1(11) . . ? N6' C59' N5' 106.8(7) . . ? N6' C59' P2' 122.3(7) . . ? N5' C59' P2' 130.7(7) . . ? C61' C60' N5' 106.8(10) . . ? C61' C60' C64' 129.3(15) . . ? N5' C60' C64' 122.0(15) . . ? C60' C61' N6' 105.7(9) . . ? C60' C61' C65' 130.5(16) . . ? N6' C61' C65' 122.9(14) . . ? C1 N1 C6 119.13(17) . . ? C1 N1 Ga1' 123.27(17) . . ? C6 N1 Ga1' 117.16(16) . . ? C1 N1 Ga1 117.01(13) . . ? C6 N1 Ga1 123.81(13) . . ? C3 N2 C18 118.73(16) . . ? C3 N2 Ga1 117.33(14) . . ? C18 N2 Ga1 123.04(12) . . ? C3 N2 Ga1' 116.51(16) . . ? C18 N2 Ga1' 124.69(15) . . ? C30 N3 C35 119.97(16) . . ? C30 N3 Ga2 120.95(13) . . ? C35 N3 Ga2 118.90(12) . . ? C30 N3 Ga2' 114.30(14) . . ? C35 N3 Ga2' 125.50(13) . . ? C32 N4 C47 119.81(16) . . ? C32 N4 Ga2' 118.45(15) . . ? C47 N4 Ga2' 118.86(14) . . ? C32 N4 Ga2 117.99(13) . . ? C47 N4 Ga2 122.06(12) . . ? N1 C1 C2 123.21(18) . . ? N1 C1 C4 119.56(18) . . ? C2 C1 C4 117.20(18) . . ? C3 C2 C1 128.77(18) . . ? N2 C3 C2 123.96(17) . . ? N2 C3 C5 119.36(18) . . ? C2 C3 C5 116.68(17) . . ? C7 C6 C11 121.34(18) . . ? C7 C6 N1 120.06(17) . . ? C11 C6 N1 118.60(17) . . ? C8 C7 C6 118.05(18) . . ? C8 C7 C12 119.32(18) . . ? C6 C7 C12 122.63(17) . . ? C9 C8 C7 121.5(2) . . ? C8 C9 C10 119.5(2) . . ? C9 C10 C11 121.5(2) . . ? C10 C11 C6 118.04(19) . . ? C10 C11 C15 119.43(19) . . ? C6 C11 C15 122.53(19) . . ? C7 C12 C13 111.70(17) . . ? C7 C12 C14 110.94(17) . . ? C13 C12 C14 110.30(17) . . ? C11 C15 C16 111.6(2) . . ? C11 C15 C17 110.2(2) . . ? C16 C15 C17 111.6(2) . . ? C19 C18 C23 121.96(19) . . ? C19 C18 N2 119.76(18) . . ? C23 C18 N2 118.24(18) . . ? C20 C19 C18 117.7(2) . . ? C20 C19 C24 119.2(2) . . ? C18 C19 C24 123.02(19) . . ? C21 C20 C19 121.0(2) . . ? C22 C21 C20 120.4(2) . . ? C21 C22 C23 121.5(2) . . ? C22 C23 C18 117.4(2) . . ? C22 C23 C27 120.81(19) . . ? C18 C23 C27 121.80(19) . . ? C19 C24 C26 110.15(18) . . ? C19 C24 C25 112.02(19) . . ? C26 C24 C25 110.31(19) . . ? C23 C27 C29 113.2(2) . . ? C23 C27 C28 112.07(19) . . ? C29 C27 C28 109.44(19) . . ? N3 C30 C31 122.83(17) . . ? N3 C30 C33 119.20(17) . . ? C31 C30 C33 117.97(16) . . ? C30 C31 C32 129.10(17) . . ? N4 C32 C31 124.10(17) . . ? N4 C32 C34 120.34(18) . . ? C31 C32 C34 115.55(17) . . ? C36 C35 C40 121.99(18) . . ? C36 C35 N3 120.55(17) . . ? C40 C35 N3 117.43(17) . . ? C37 C36 C35 117.44(18) . . ? C37 C36 C41 119.75(17) . . ? C35 C36 C41 122.80(17) . . ? C38 C37 C36 121.43(19) . . ? C37 C38 C39 120.23(19) . . ? C38 C39 C40 120.89(19) . . ? C39 C40 C35 118.00(18) . . ? C39 C40 C44 120.32(18) . . ? C35 C40 C44 121.66(18) . . ? C36 C41 C42 112.34(16) . . ? C36 C41 C43 110.08(16) . . ? C42 C41 C43 110.27(16) . . ? C46 C44 C40 112.73(19) . . ? C46 C44 C45 109.2(2) . . ? C40 C44 C45 110.84(19) . . ? C48 C47 C52 121.73(18) . . ? C48 C47 N4 120.02(18) . . ? C52 C47 N4 118.25(19) . . ? C49 C48 C47 117.8(2) . . ? C49 C48 C53 117.9(2) . . ? C47 C48 C53 124.34(18) . . ? C50 C49 C48 121.2(2) . . ? C51 C50 C49 120.3(2) . . ? C50 C51 C52 121.1(2) . . ? C51 C52 C47 117.8(2) . . ? C51 C52 C56 120.35(19) . . ? C47 C52 C56 121.83(18) . . ? C48 C53 C55 111.50(19) . . ? C48 C53 C54 111.0(2) . . ? C55 C53 C54 109.7(3) . . ? C52 C56 C58 113.51(19) . . ? C52 C56 C57 111.3(2) . . ? C58 C56 C57 110.0(2) . . ? C12_1 C11_1 C16_1 112.82(17) . . ? C12_1 C11_1 B1_1 126.03(16) . . ? C16_1 C11_1 B1_1 120.75(17) . . ? F12_1 C12_1 C13_1 114.61(18) . . ? F12_1 C12_1 C11_1 121.19(17) . . ? C13_1 C12_1 C11_1 124.20(19) . . ? F13_1 C13_1 C14_1 119.66(18) . . ? F13_1 C13_1 C12_1 120.33(19) . . ? C14_1 C13_1 C12_1 120.01(19) . . ? F14_1 C14_1 C13_1 120.8(2) . . ? F14_1 C14_1 C15_1 120.4(2) . . ? C13_1 C14_1 C15_1 118.82(18) . . ? F15_1 C15_1 C14_1 120.43(18) . . ? F15_1 C15_1 C16_1 120.2(2) . . ? C14_1 C15_1 C16_1 119.35(19) . . ? F16_1 C16_1 C15_1 115.55(18) . . ? F16_1 C16_1 C11_1 119.67(17) . . ? C15_1 C16_1 C11_1 124.8(2) . . ? C26_1 C21_1 C22_1 113.17(16) . . ? C26_1 C21_1 B1_1 120.50(16) . . ? C22_1 C21_1 B1_1 125.80(16) . . ? F22_1 C22_1 C23_1 115.18(16) . . ? F22_1 C22_1 C21_1 120.98(16) . . ? C23_1 C22_1 C21_1 123.84(17) . . ? F23_1 C23_1 C24_1 119.86(17) . . ? F23_1 C23_1 C22_1 120.25(17) . . ? C24_1 C23_1 C22_1 119.89(17) . . ? F24_1 C24_1 C23_1 121.38(18) . . ? F24_1 C24_1 C25_1 119.77(18) . . ? C23_1 C24_1 C25_1 118.84(17) . . ? F25_1 C25_1 C24_1 120.08(16) . . ? F25_1 C25_1 C26_1 120.45(17) . . ? C24_1 C25_1 C26_1 119.45(17) . . ? F26_1 C26_1 C25_1 115.65(16) . . ? F26_1 C26_1 C21_1 119.61(15) . . ? C25_1 C26_1 C21_1 124.75(17) . . ? C36_1 C31_1 C32_1 113.61(17) . . ? C36_1 C31_1 B1_1 125.27(17) . . ? C32_1 C31_1 B1_1 120.70(16) . . ? F32_1 C32_1 C33_1 115.57(18) . . ? F32_1 C32_1 C31_1 120.09(16) . . ? C33_1 C32_1 C31_1 124.34(19) . . ? F33_1 C33_1 C34_1 119.90(18) . . ? F33_1 C33_1 C32_1 120.73(19) . . ? C34_1 C33_1 C32_1 119.36(19) . . ? F34_1 C34_1 C35_1 120.58(19) . . ? F34_1 C34_1 C33_1 120.5(2) . . ? C35_1 C34_1 C33_1 118.87(17) . . ? F35_1 C35_1 C34_1 120.11(17) . . ? F35_1 C35_1 C36_1 119.96(19) . . ? C34_1 C35_1 C36_1 119.93(18) . . ? F36_1 C36_1 C31_1 121.35(16) . . ? F36_1 C36_1 C35_1 114.81(17) . . ? C31_1 C36_1 C35_1 123.83(19) . . ? C46_1 C41_1 C42_1 113.07(17) . . ? C46_1 C41_1 B1_1 125.59(17) . . ? C42_1 C41_1 B1_1 121.07(16) . . ? F41_1 C42_1 C43_1 115.66(18) . . ? F41_1 C42_1 C41_1 119.68(17) . . ? C43_1 C42_1 C41_1 124.66(19) . . ? F42_1 C43_1 C44_1 119.76(19) . . ? F42_1 C43_1 C42_1 120.90(19) . . ? C44_1 C43_1 C42_1 119.34(19) . . ? F43_1 C44_1 C43_1 120.5(2) . . ? F43_1 C44_1 C45_1 120.5(2) . . ? C43_1 C44_1 C45_1 119.00(18) . . ? F44_1 C45_1 C44_1 119.71(18) . . ? F44_1 C45_1 C46_1 120.6(2) . . ? C44_1 C45_1 C46_1 119.65(19) . . ? F45_1 C46_1 C45_1 115.34(17) . . ? F45_1 C46_1 C41_1 120.44(17) . . ? C45_1 C46_1 C41_1 124.22(19) . . ? C21_1 B1_1 C41_1 101.61(13) . . ? C21_1 B1_1 C31_1 113.78(15) . . ? C41_1 B1_1 C31_1 113.39(15) . . ? C21_1 B1_1 C11_1 113.80(15) . . ? C41_1 B1_1 C11_1 113.79(15) . . ? C31_1 B1_1 C11_1 101.04(13) . . ? C2_2 C1_2 C6_2 118.0(3) . . ? C2_2 C1_2 C7_2 120.6(3) . . ? C6_2 C1_2 C7_2 121.5(3) . . ? C1_2 C2_2 C3_2 120.9(4) . . ? C4_2 C3_2 C2_2 120.5(3) . . ? C3_2 C4_2 C5_2 119.5(3) . . ? C4_2 C5_2 C6_2 120.2(4) . . ? C5_2 C6_2 C1_2 121.0(4) . . ? C6_3 C1_3 C2_3 117.4(13) . . ? C6_3 C1_3 C7_3 122.1(15) . . ? C2_3 C1_3 C7_3 120.4(14) . . ? C3_3 C2_3 C1_3 118.4(13) . . ? C4_3 C3_3 C2_3 122.8(13) . . ? C5_3 C6_3 C1_3 122.1(17) . . ? C6_3 C5_3 C4_3 119.2(12) . . ? C3_3 C4_3 C5_3 120.0(11) . . ? _refine_diff_density_max 0.580 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.048 _shelx_res_file ; TITL mks_057m in P-1 mks_057m.res created by SHELXL-2017/1 at 12:13:18 on 11-Jun-2021 CELL 1.54178 12.61510 16.63930 23.13480 77.8438 77.7315 86.8968 ZERR 2.00 0.00100 0.00130 0.00180 0.0032 0.0030 0.0032 LATT 1 SFAC C H B CL F GA N P UNIT 192 204 2 4 40 4 12 4 TEMP -173.150 SIZE 0.080 0.149 0.326 L.S. 16 ACTA LIST 6 FMAP 2 PLAN 20 RIGU_SOLV SADI c59 n5 c59 n6 c59' n5' c59' n6' SADI n5 c60 n6 c61 n5' c60' n6' c61' SADI c60 c61 c60' c61' SADI c60 c64 c61 c65 c60' c64' c61' c65' SADI n5 c62 n6 c63 n5' c62' n6' c63' SADI c59 c60 c59 c61 c59' c60' c59' c61' SADI n5 n6 n5' n6' RIGU n5 n6 c59 c60 c61 c62 c63 c64 c65 = N5' N6' C59' C60' C61' C62' C63' C64' C65' SIMU c60 c60' SIMU c61 c61' WGHT 0.018300 4.497900 FVAR 0.10329 0.73424 0.77475 PART 1 21 GA1 6 0.209908 0.308821 0.891963 21.00000 0.01599 0.02188 = 0.01768 -0.00577 -0.00358 0.00083 GA2 6 0.319131 0.324983 0.641612 21.00000 0.01656 0.01790 = 0.01750 -0.00520 -0.00243 0.00300 CL1 4 0.058835 0.380760 0.908683 21.00000 0.01955 0.02504 = 0.03043 -0.00965 -0.00465 0.00601 CL2 4 0.451433 0.410113 0.635041 21.00000 0.02320 0.02392 = 0.02915 -0.00914 0.00107 -0.00490 P1 8 0.304139 0.331252 0.790962 21.00000 0.01647 0.01998 = 0.01866 -0.00581 -0.00307 0.00121 P2 8 0.227353 0.267549 0.739805 21.00000 0.02198 0.02242 = 0.01861 -0.00622 -0.00132 -0.00428 N5 7 0.370701 0.495372 0.756817 21.00000 0.02521 0.02710 = 0.02742 -0.00855 -0.00306 -0.00941 N6 7 0.201514 0.488179 0.755035 21.00000 0.02401 0.01737 = 0.02514 -0.00354 -0.00594 0.00094 C59 1 0.289228 0.442040 0.766467 21.00000 0.01890 0.02196 = 0.02128 -0.00666 -0.00339 -0.00168 C60 1 0.336193 0.574863 0.738600 21.00000 0.03937 0.02405 = 0.02716 -0.00284 0.00095 -0.00882 C61 1 0.229019 0.570409 0.739278 21.00000 0.04565 0.01868 = 0.03587 -0.00283 -0.01187 0.00144 C62 1 0.484031 0.473491 0.759230 21.00000 0.02127 0.04905 = 0.04183 -0.01364 -0.00541 -0.00945 AFIX 137 H62A 2 0.529720 0.490214 0.718878 21.00000 -1.50000 H62B 2 0.490493 0.413911 0.773032 21.00000 -1.50000 H62C 2 0.507649 0.501718 0.787393 21.00000 -1.50000 AFIX 0 C63 1 0.092688 0.459116 0.758522 21.00000 0.02280 0.02841 = 0.03177 -0.00782 -0.01023 0.00494 AFIX 137 H63A 2 0.074446 0.473649 0.718466 21.00000 -1.50000 H63B 2 0.040164 0.484934 0.786996 21.00000 -1.50000 H63C 2 0.090438 0.399265 0.772443 21.00000 -1.50000 AFIX 0 C64 1 0.409487 0.646867 0.725660 21.00000 0.07098 0.03400 = 0.06712 -0.01025 -0.00159 -0.02705 AFIX 137 H64A 2 0.472365 0.639936 0.693903 21.00000 -1.50000 H64B 2 0.434126 0.650574 0.762426 21.00000 -1.50000 H64C 2 0.370056 0.697332 0.712163 21.00000 -1.50000 AFIX 0 C65 1 0.147738 0.636874 0.725427 21.00000 0.06241 0.02005 = 0.04935 -0.00182 -0.01453 0.00741 AFIX 137 H65A 2 0.184581 0.689893 0.710900 21.00000 -1.50000 H65B 2 0.092907 0.638939 0.762120 21.00000 -1.50000 H65C 2 0.112561 0.625264 0.694202 21.00000 -1.50000 AFIX 0 PART 2 -21 GA1' 6 0.226845 0.287513 0.888220 -21.00000 0.01999 0.02682 = 0.01766 -0.00452 -0.00468 -0.00037 GA2' 6 0.336128 0.349873 0.635647 -21.00000 0.02008 0.01925 = 0.01709 -0.00543 -0.00305 0.00409 CL1' 4 0.086615 0.371516 0.884175 -21.00000 0.02631 0.02665 = 0.03048 -0.00905 -0.00784 0.00685 CL2' 4 0.481426 0.427787 0.612329 -21.00000 0.02103 0.02348 = 0.03246 -0.00651 0.00056 -0.00228 P1' 8 0.316790 0.257158 0.795740 -21.00000 0.02607 0.02131 = 0.02074 -0.00571 -0.00444 0.00751 P2' 8 0.239401 0.343090 0.734983 -21.00000 0.01834 0.01834 = 0.01745 -0.00503 -0.00273 0.00090 N5' 7 0.345496 0.487152 0.747632 -21.00000 0.01912 0.02529 = 0.02603 -0.01321 -0.00762 0.00347 N6' 7 0.177551 0.504867 0.742889 -21.00000 0.02321 0.02084 = 0.02220 -0.00583 -0.00534 0.00904 C59' 1 0.256957 0.448781 0.744160 -21.00000 0.01603 0.01394 = 0.02303 -0.00112 -0.00305 0.00039 C60' 1 0.319313 0.569207 0.750123 -21.00000 0.04073 0.01826 = 0.01394 -0.00528 0.00023 -0.00743 C61' 1 0.215810 0.581701 0.741711 -21.00000 0.03273 0.01680 = 0.03037 -0.00889 -0.00217 -0.00084 C62' 1 0.452773 0.452476 0.752553 -21.00000 0.02385 0.03517 = 0.03166 -0.00381 -0.01027 -0.00133 AFIX 137 H62D 2 0.454064 0.394082 0.750816 -21.00000 -1.50000 H62E 2 0.468945 0.458373 0.791044 -21.00000 -1.50000 H62F 2 0.507336 0.481691 0.719102 -21.00000 -1.50000 AFIX 0 C63' 1 0.063907 0.489367 0.744410 -21.00000 0.02184 0.03636 = 0.03227 -0.01424 -0.01070 0.00524 AFIX 137 H63D 2 0.039069 0.528892 0.712075 -21.00000 -1.50000 H63E 2 0.019646 0.495428 0.783578 -21.00000 -1.50000 H63F 2 0.056835 0.433391 0.738596 -21.00000 -1.50000 AFIX 0 C64' 1 0.403646 0.630653 0.746229 -21.00000 0.03897 0.02619 = 0.06050 -0.01449 -0.01021 -0.00443 AFIX 137 H64D 2 0.369438 0.684854 0.746835 -21.00000 -1.20000 H64E 2 0.457647 0.633130 0.708573 -21.00000 -1.20000 H64F 2 0.439279 0.614359 0.780720 -21.00000 -1.20000 AFIX 0 C65' 1 0.144342 0.656226 0.742218 -21.00000 0.06179 0.02817 = 0.06562 -0.01513 -0.02820 0.02332 AFIX 137 H65D 2 0.187114 0.703328 0.742910 -21.00000 -1.50000 H65E 2 0.085720 0.646413 0.778190 -21.00000 -1.50000 H65F 2 0.113304 0.667832 0.705887 -21.00000 -1.50000 AFIX 0 PART 0 N1 7 0.173813 0.194465 0.935442 11.00000 0.02088 0.03168 = 0.02453 -0.01072 -0.00340 0.00160 N2 7 0.297446 0.332649 0.944995 11.00000 0.02200 0.03640 = 0.02023 -0.00836 -0.00642 -0.00015 N3 7 0.384068 0.239419 0.605238 11.00000 0.01872 0.02862 = 0.02071 -0.00255 -0.00314 0.00036 N4 7 0.246757 0.383088 0.577142 11.00000 0.02182 0.04126 = 0.01954 -0.00618 -0.00471 0.01063 C1 1 0.162180 0.178818 0.995562 11.00000 0.02634 0.03085 = 0.02506 -0.00734 -0.00315 0.00534 C2 1 0.198249 0.231983 1.026836 11.00000 0.03056 0.03733 = 0.01854 -0.00718 -0.00462 0.00296 AFIX 43 H2 2 0.171797 0.220984 1.069325 11.00000 -1.20000 AFIX 0 C3 1 0.267731 0.298848 1.003997 11.00000 0.02614 0.03744 = 0.02096 -0.00960 -0.00701 0.00680 C4 1 0.110995 0.099706 1.032388 11.00000 0.05582 0.03254 = 0.02933 -0.00401 -0.00782 -0.00090 AFIX 137 H4A 2 0.042619 0.092108 1.020613 11.00000 -1.50000 H4B 2 0.096672 0.101795 1.075375 11.00000 -1.50000 H4C 2 0.160339 0.053661 1.025174 11.00000 -1.50000 AFIX 0 C5 1 0.312301 0.333030 1.049465 11.00000 0.04120 0.04657 = 0.02390 -0.01028 -0.01239 -0.00206 AFIX 137 H5A 2 0.389670 0.344588 1.034028 11.00000 -1.50000 H5B 2 0.302765 0.292732 1.087705 11.00000 -1.50000 H5C 2 0.273369 0.383935 1.056146 11.00000 -1.50000 AFIX 0 C6 1 0.155078 0.129217 0.906123 11.00000 0.02612 0.03228 = 0.02375 -0.01049 -0.00127 0.00009 C7 1 0.054540 0.123605 0.890502 11.00000 0.02549 0.03238 = 0.02667 -0.00877 -0.00046 -0.00266 C8 1 0.040896 0.060710 0.861302 11.00000 0.03130 0.03949 = 0.03410 -0.01304 -0.00368 -0.00652 AFIX 43 H8 2 -0.026113 0.056624 0.849656 11.00000 -1.20000 AFIX 0 C9 1 0.122341 0.004404 0.848969 11.00000 0.04242 0.03995 = 0.03713 -0.01959 -0.00101 -0.00486 AFIX 43 H9 2 0.111228 -0.038249 0.829362 11.00000 -1.20000 AFIX 0 C10 1 0.220406 0.010465 0.865358 11.00000 0.03671 0.03982 = 0.03922 -0.01908 -0.00088 0.00625 AFIX 43 H10 2 0.276281 -0.028572 0.856884 11.00000 -1.20000 AFIX 0 C11 1 0.239144 0.072497 0.894007 11.00000 0.02808 0.04036 = 0.03109 -0.01527 -0.00260 0.00417 C12 1 -0.038307 0.182828 0.903921 11.00000 0.02368 0.03206 = 0.03693 -0.01216 -0.00643 -0.00207 AFIX 13 H12 2 -0.015551 0.220688 0.927275 11.00000 -1.20000 AFIX 0 C13 1 -0.140177 0.138010 0.942544 11.00000 0.02645 0.04420 = 0.04252 -0.01821 0.00090 -0.00403 AFIX 137 H13A 2 -0.197394 0.178317 0.951942 11.00000 -1.50000 H13B 2 -0.123399 0.105752 0.980184 11.00000 -1.50000 H13C 2 -0.164984 0.101256 0.920241 11.00000 -1.50000 AFIX 0 C14 1 -0.063461 0.235174 0.845334 11.00000 0.03140 0.04404 = 0.04672 -0.00499 -0.01219 -0.00276 AFIX 137 H14A 2 0.003606 0.259835 0.819526 11.00000 -1.50000 H14B 2 -0.115408 0.278777 0.855000 11.00000 -1.50000 H14C 2 -0.094654 0.200360 0.824038 11.00000 -1.50000 AFIX 0 C15 1 0.349382 0.077182 0.910264 11.00000 0.02901 0.05196 = 0.04465 -0.02616 -0.00862 0.01154 AFIX 13 H15 2 0.346531 0.124116 0.931381 11.00000 -1.20000 AFIX 0 C16 1 0.374733 -0.000832 0.953447 11.00000 0.06192 0.06300 = 0.09927 -0.02109 -0.04618 0.02132 AFIX 137 H16A 2 0.373884 -0.048384 0.934745 11.00000 -1.50000 H16B 2 0.319988 -0.007894 0.991125 11.00000 -1.50000 H16C 2 0.446602 0.003696 0.962193 11.00000 -1.50000 AFIX 0 C17 1 0.438453 0.095459 0.852678 11.00000 0.02737 0.12770 = 0.06563 -0.05391 0.00042 0.00207 AFIX 137 H17A 2 0.447491 0.048179 0.832921 11.00000 -1.50000 H17B 2 0.506931 0.105799 0.863302 11.00000 -1.50000 H17C 2 0.417755 0.144059 0.825076 11.00000 -1.50000 AFIX 0 C18 1 0.380298 0.395201 0.926209 11.00000 0.02617 0.03976 = 0.02176 -0.00863 -0.00790 -0.00408 C19 1 0.352059 0.477039 0.930197 11.00000 0.03577 0.04190 = 0.02852 -0.01249 -0.00702 -0.00290 C20 1 0.435439 0.534651 0.914004 11.00000 0.04958 0.04484 = 0.04394 -0.01705 -0.00379 -0.01192 AFIX 43 H20 2 0.418431 0.590631 0.915365 11.00000 -1.20000 AFIX 0 C21 1 0.541956 0.511421 0.896097 11.00000 0.04245 0.06095 = 0.05103 -0.02083 -0.00288 -0.02157 AFIX 43 H21 2 0.597693 0.551185 0.886118 11.00000 -1.20000 AFIX 0 C22 1 0.567985 0.430900 0.892597 11.00000 0.02740 0.06391 = 0.04103 -0.01733 -0.00639 -0.00863 AFIX 43 H22 2 0.641854 0.415872 0.880522 11.00000 -1.20000 AFIX 0 C23 1 0.488362 0.370894 0.906377 11.00000 0.02452 0.04799 = 0.02674 -0.01038 -0.00975 -0.00214 C24 1 0.236110 0.504927 0.951357 11.00000 0.03905 0.03900 = 0.03139 -0.01384 -0.00557 0.00269 AFIX 13 H24 2 0.189657 0.454959 0.966392 11.00000 -1.20000 AFIX 0 C25 1 0.225997 0.551174 1.003496 11.00000 0.05466 0.05514 = 0.03705 -0.02094 -0.00934 0.00749 AFIX 137 H25A 2 0.269181 0.601391 0.989362 11.00000 -1.50000 H25B 2 0.252627 0.515882 1.037128 11.00000 -1.50000 H25C 2 0.149757 0.565638 1.017129 11.00000 -1.50000 AFIX 0 C26 1 0.194424 0.558827 0.898485 11.00000 0.05082 0.03631 = 0.03678 -0.01427 -0.01224 0.00414 AFIX 137 H26A 2 0.239975 0.607623 0.882376 11.00000 -1.50000 H26B 2 0.119382 0.575827 0.912489 11.00000 -1.50000 H26C 2 0.197193 0.527580 0.866700 11.00000 -1.50000 AFIX 0 C27 1 0.518359 0.282475 0.900981 11.00000 0.02189 0.04928 = 0.03434 -0.01041 -0.00997 0.00459 AFIX 13 H27 2 0.455989 0.259102 0.889767 11.00000 -1.20000 AFIX 0 C28 1 0.534896 0.229044 0.961094 11.00000 0.04979 0.07165 = 0.04130 -0.00510 -0.01396 0.02118 AFIX 137 H28A 2 0.557811 0.173611 0.955188 11.00000 -1.50000 H28B 2 0.466616 0.225999 0.991022 11.00000 -1.50000 H28C 2 0.590833 0.253368 0.975496 11.00000 -1.50000 AFIX 0 C29 1 0.618369 0.275546 0.851726 11.00000 0.02683 0.06250 = 0.04637 -0.01576 -0.00567 0.00754 AFIX 137 H29A 2 0.628183 0.218331 0.846889 11.00000 -1.50000 H29B 2 0.682530 0.293136 0.863177 11.00000 -1.50000 H29C 2 0.608574 0.310723 0.813505 11.00000 -1.50000 AFIX 0 C30 1 0.406153 0.247781 0.545117 11.00000 0.02092 0.02836 = 0.02428 -0.00665 -0.00368 -0.00183 C31 1 0.363920 0.311821 0.506794 11.00000 0.02681 0.03378 = 0.01890 -0.00635 -0.00207 0.00396 AFIX 43 H31 2 0.394185 0.316916 0.464936 11.00000 -1.20000 AFIX 0 C32 1 0.283301 0.369560 0.521343 11.00000 0.02860 0.04308 = 0.01910 -0.00551 -0.00546 0.00773 C33 1 0.478735 0.185650 0.517056 11.00000 0.03877 0.02823 = 0.02647 -0.00843 -0.00628 0.00428 AFIX 137 H33A 2 0.478477 0.195280 0.473811 11.00000 -1.50000 H33B 2 0.452283 0.130187 0.536536 11.00000 -1.50000 H33C 2 0.552799 0.190947 0.522512 11.00000 -1.50000 AFIX 0 C34 1 0.236523 0.417169 0.469166 11.00000 0.05247 0.07074 = 0.02242 -0.01106 -0.01223 0.03334 AFIX 137 H34A 2 0.286051 0.461423 0.446064 11.00000 -1.50000 H34B 2 0.166056 0.440803 0.484740 11.00000 -1.50000 H34C 2 0.227118 0.380164 0.442849 11.00000 -1.50000 AFIX 0 C35 1 0.402620 0.160938 0.643380 11.00000 0.02488 0.02905 = 0.02113 -0.00332 -0.00230 0.00094 C36 1 0.501648 0.144083 0.662347 11.00000 0.02454 0.02919 = 0.02186 -0.00621 -0.00201 0.00260 C37 1 0.513150 0.067887 0.699805 11.00000 0.03191 0.03323 = 0.02660 -0.00587 -0.00826 0.00604 AFIX 43 H37 2 0.579616 0.054479 0.712834 11.00000 -1.20000 AFIX 0 C38 1 0.429943 0.011564 0.718331 11.00000 0.03999 0.03146 = 0.02582 -0.00044 -0.00530 0.00114 AFIX 43 H38 2 0.439514 -0.039715 0.744064 11.00000 -1.20000 AFIX 0 C39 1 0.332618 0.029619 0.699506 11.00000 0.03431 0.03500 = 0.02949 -0.00109 -0.00207 -0.00720 AFIX 43 H39 2 0.275824 -0.009427 0.712658 11.00000 -1.20000 AFIX 0 C40 1 0.316929 0.104206 0.661580 11.00000 0.02650 0.03557 = 0.02620 -0.00354 -0.00271 -0.00455 C41 1 0.593632 0.205236 0.644724 11.00000 0.02134 0.02914 = 0.03000 -0.00661 -0.00562 0.00471 AFIX 13 H41 2 0.573728 0.252933 0.614543 11.00000 -1.20000 AFIX 0 C42 1 0.700536 0.168677 0.615648 11.00000 0.02458 0.03419 = 0.03553 -0.00595 -0.00172 0.00547 AFIX 137 H42A 2 0.690925 0.149502 0.579853 11.00000 -1.50000 H42B 2 0.722372 0.122310 0.644710 11.00000 -1.50000 H42C 2 0.756809 0.210794 0.603751 11.00000 -1.50000 AFIX 0 C43 1 0.607669 0.237328 0.700123 11.00000 0.02831 0.04180 = 0.04270 -0.01651 -0.01072 0.00451 AFIX 137 H43A 2 0.661601 0.281191 0.687505 11.00000 -1.50000 H43B 2 0.632238 0.192306 0.729177 11.00000 -1.50000 H43C 2 0.538133 0.258986 0.719072 11.00000 -1.50000 AFIX 0 C44 1 0.210482 0.122225 0.639638 11.00000 0.02736 0.04127 = 0.03905 0.00061 -0.00798 -0.00863 AFIX 13 H44 2 0.203553 0.183138 0.626357 11.00000 -1.20000 AFIX 0 C45 1 0.210910 0.082967 0.584998 11.00000 0.04646 0.04558 = 0.05468 -0.00672 -0.02281 -0.00910 AFIX 137 H45A 2 0.140268 0.092190 0.573338 11.00000 -1.50000 H45B 2 0.224886 0.023758 0.595803 11.00000 -1.50000 H45C 2 0.267850 0.107959 0.551063 11.00000 -1.50000 AFIX 0 C46 1 0.111474 0.092625 0.688917 11.00000 0.02830 0.07154 = 0.05598 0.00455 -0.00378 -0.01206 AFIX 137 H46A 2 0.045459 0.106990 0.672894 11.00000 -1.50000 H46B 2 0.109391 0.119035 0.723221 11.00000 -1.50000 H46C 2 0.115971 0.032836 0.702291 11.00000 -1.50000 AFIX 0 C47 1 0.161237 0.443308 0.587682 11.00000 0.02374 0.04712 = 0.01927 -0.00851 -0.00672 0.01346 C48 1 0.184993 0.527381 0.571609 11.00000 0.02890 0.04720 = 0.02277 -0.00373 -0.00122 0.01434 C49 1 0.099379 0.583003 0.582173 11.00000 0.03629 0.04712 = 0.03276 -0.01028 -0.00346 0.01618 AFIX 43 H49 2 0.113552 0.640302 0.572194 11.00000 -1.20000 AFIX 0 C50 1 -0.005184 0.556172 0.606802 11.00000 0.02903 0.05960 = 0.04216 -0.02499 -0.00887 0.02091 AFIX 43 H50 2 -0.062301 0.595027 0.613014 11.00000 -1.20000 AFIX 0 C51 1 -0.027236 0.473426 0.622429 11.00000 0.02069 0.06162 = 0.04100 -0.02605 -0.00861 0.01162 AFIX 43 H51 2 -0.099626 0.455828 0.639479 11.00000 -1.20000 AFIX 0 C52 1 0.055007 0.414810 0.613655 11.00000 0.02296 0.05161 = 0.02712 -0.01695 -0.01056 0.00870 C53 1 0.297285 0.562249 0.541883 11.00000 0.03675 0.04152 = 0.04011 0.01031 0.01193 0.01433 AFIX 13 H53 2 0.347338 0.515518 0.533426 11.00000 -1.20000 AFIX 0 C54 1 0.294932 0.621804 0.481578 11.00000 0.07689 0.07409 = 0.05941 0.03583 0.03126 0.04352 AFIX 137 H54A 2 0.369338 0.635980 0.460063 11.00000 -1.50000 H54B 2 0.254921 0.671873 0.489370 11.00000 -1.50000 H54C 2 0.259038 0.595540 0.456842 11.00000 -1.50000 AFIX 0 C55 1 0.342131 0.606002 0.583407 11.00000 0.03432 0.03183 = 0.08900 -0.00548 0.01072 -0.00185 AFIX 137 H55A 2 0.415281 0.625898 0.563622 11.00000 -1.50000 H55B 2 0.345064 0.567476 0.621445 11.00000 -1.50000 H55C 2 0.294761 0.652644 0.591738 11.00000 -1.50000 AFIX 0 C56 1 0.028623 0.323869 0.629827 11.00000 0.02209 0.05425 = 0.03987 -0.01739 -0.01199 0.00498 AFIX 13 H56 2 0.092272 0.293885 0.643959 11.00000 -1.20000 AFIX 0 C57 1 0.014101 0.292213 0.574233 11.00000 0.04754 0.06281 = 0.05397 -0.02818 -0.02327 0.00496 AFIX 137 H57A 2 -0.043336 0.324049 0.556827 11.00000 -1.50000 H57B 2 -0.005872 0.234062 0.586321 11.00000 -1.50000 H57C 2 0.082249 0.298337 0.544096 11.00000 -1.50000 AFIX 0 C58 1 -0.070497 0.302205 0.680965 11.00000 0.02894 0.06736 = 0.05781 -0.01882 -0.00385 -0.00545 AFIX 137 H58A 2 -0.135694 0.326441 0.667275 11.00000 -1.50000 H58B 2 -0.061555 0.323957 0.715831 11.00000 -1.50000 H58C 2 -0.077830 0.242318 0.692594 11.00000 -1.50000 AFIX 0 RESI 1 F12 5 0.293868 0.304674 0.353190 11.00000 0.03492 0.02986 = 0.03594 -0.01163 -0.00978 0.00285 F13 5 0.284290 0.464290 0.311339 11.00000 0.03360 0.02812 = 0.05601 -0.01643 0.00329 -0.00281 F14 5 0.192911 0.526258 0.214163 11.00000 0.04997 0.02278 = 0.05650 0.00534 0.00698 0.00343 F15 5 0.107618 0.420267 0.160511 11.00000 0.05606 0.03967 = 0.03949 0.00730 -0.01275 0.01373 F16 5 0.109149 0.259792 0.204013 11.00000 0.03479 0.03365 = 0.03856 -0.00339 -0.01749 0.00576 F22 5 0.166942 0.042727 0.425779 11.00000 0.02572 0.03475 = 0.03335 0.00489 -0.00422 -0.00535 F23 5 0.324571 -0.023838 0.479587 11.00000 0.04305 0.03193 = 0.02916 0.00414 -0.01179 0.00275 F24 5 0.533291 0.030258 0.436945 11.00000 0.03273 0.04097 = 0.03948 -0.00469 -0.02096 0.01150 F25 5 0.577670 0.152900 0.337432 11.00000 0.01796 0.03835 = 0.05027 -0.00365 -0.01053 0.00083 F26 5 0.423919 0.214353 0.278073 11.00000 0.01915 0.03046 = 0.03100 0.00248 -0.00299 -0.00003 F32 5 0.115755 0.212120 0.425808 11.00000 0.02767 0.04967 = 0.03524 -0.01939 -0.00209 -0.00140 F33 5 -0.087964 0.211020 0.486914 11.00000 0.03719 0.05550 = 0.03752 -0.01619 0.00932 0.00328 F34 5 -0.253136 0.172217 0.438736 11.00000 0.01972 0.04127 = 0.05588 -0.00019 0.01052 0.00379 F35 5 -0.206047 0.127240 0.329272 11.00000 0.01694 0.04176 = 0.05834 -0.00498 -0.01014 0.00041 F36 5 -0.004410 0.119132 0.270441 11.00000 0.02206 0.04173 = 0.03863 -0.01128 -0.01000 0.00238 F41 5 0.131187 0.000167 0.322289 11.00000 0.03372 0.02540 = 0.03603 -0.00378 -0.00437 0.00093 F42 5 0.176655 -0.096614 0.241939 11.00000 0.04567 0.02981 = 0.05929 -0.01874 -0.01756 0.00317 F43 5 0.297861 -0.040080 0.129689 11.00000 0.04311 0.05942 = 0.05008 -0.03704 -0.01854 0.01602 F44 5 0.374151 0.116641 0.100384 11.00000 0.03992 0.06057 = 0.02796 -0.01582 -0.00053 0.00890 F45 5 0.328079 0.215354 0.178815 11.00000 0.03043 0.03546 = 0.02751 -0.00506 0.00199 0.00015 C11 1 0.204782 0.271261 0.279924 11.00000 0.01524 0.02352 = 0.02667 -0.00366 0.00157 0.00305 C12 1 0.246547 0.328534 0.304894 11.00000 0.01990 0.02700 = 0.02931 -0.00593 0.00159 0.00304 C13 1 0.243491 0.412888 0.283689 11.00000 0.02249 0.02481 = 0.04013 -0.01022 0.00657 -0.00027 C14 1 0.197579 0.444503 0.234964 11.00000 0.03012 0.02068 = 0.04055 0.00284 0.00958 0.00367 C15 1 0.154043 0.391287 0.208323 11.00000 0.03091 0.03099 = 0.03175 0.00391 -0.00151 0.00870 C16 1 0.157170 0.307577 0.231511 11.00000 0.02312 0.02721 = 0.03042 -0.00242 -0.00259 0.00349 C21 1 0.285458 0.134432 0.349121 11.00000 0.02028 0.02085 = 0.02355 -0.00617 -0.00473 0.00270 C22 1 0.267266 0.072498 0.400946 11.00000 0.02204 0.02557 = 0.02585 -0.00530 -0.00380 -0.00081 C23 1 0.348263 0.036997 0.430635 11.00000 0.03447 0.02249 = 0.02311 -0.00339 -0.00874 0.00333 C24 1 0.452999 0.063744 0.409649 11.00000 0.02767 0.02846 = 0.03001 -0.00937 -0.01470 0.00930 C25 1 0.475583 0.125462 0.358999 11.00000 0.01847 0.02716 = 0.03511 -0.00922 -0.00728 0.00286 C26 1 0.393469 0.157155 0.329664 11.00000 0.02180 0.02072 = 0.02457 -0.00330 -0.00422 0.00207 C31 1 0.068665 0.163188 0.345384 11.00000 0.01747 0.02072 = 0.02958 -0.00252 -0.00254 0.00283 C32 1 0.039190 0.187296 0.400549 11.00000 0.02174 0.02674 = 0.03237 -0.00638 -0.00166 0.00116 C33 1 -0.066306 0.188500 0.433111 11.00000 0.02742 0.03006 = 0.03217 -0.00537 0.00466 0.00395 C34 1 -0.149744 0.168074 0.409291 11.00000 0.01868 0.02320 = 0.04247 0.00242 0.00500 0.00350 C35 1 -0.125778 0.145651 0.354294 11.00000 0.01668 0.02308 = 0.04419 0.00138 -0.00639 0.00111 C36 1 -0.018525 0.142851 0.323940 11.00000 0.02026 0.02250 = 0.03219 -0.00315 -0.00407 0.00370 C41 1 0.223124 0.114435 0.254861 11.00000 0.01632 0.02822 = 0.02623 -0.00631 -0.00797 0.00660 C42 1 0.190417 0.032969 0.267361 11.00000 0.02084 0.02818 = 0.03254 -0.00722 -0.00993 0.00645 C43 1 0.213627 -0.019168 0.226693 11.00000 0.02642 0.02944 = 0.04395 -0.01239 -0.01637 0.00764 C44 1 0.275080 0.008978 0.170179 11.00000 0.02852 0.04274 = 0.03942 -0.02376 -0.01736 0.01443 C45 1 0.313092 0.088342 0.155466 11.00000 0.02364 0.04560 = 0.02622 -0.01088 -0.00662 0.00890 C46 1 0.287095 0.138488 0.197410 11.00000 0.02044 0.03027 = 0.02868 -0.00628 -0.00773 0.00560 B1 3 0.195934 0.170620 0.307382 11.00000 0.01571 0.02175 = 0.02385 -0.00429 -0.00414 0.00290 RESI 2 SOLV PART 3 31 C1 1 0.695324 0.209028 0.131310 31.00000 0.02778 0.02585 = 0.03721 -0.01176 -0.00564 0.00288 C2 1 0.738086 0.199756 0.182634 31.00000 0.03216 0.03096 = 0.03360 -0.00584 -0.00623 0.00417 AFIX 43 H2 2 0.691753 0.185238 0.221307 31.00000 -1.20000 AFIX 0 C3 1 0.847565 0.211346 0.178435 31.00000 0.03762 0.03666 = 0.04353 -0.01146 -0.01919 0.01064 AFIX 43 H3 2 0.875472 0.205074 0.214190 31.00000 -1.20000 AFIX 0 C4 1 0.916029 0.231819 0.123029 31.00000 0.02445 0.03869 = 0.05992 -0.02216 -0.00980 0.00874 AFIX 43 H4 2 0.990918 0.240397 0.120323 31.00000 -1.20000 AFIX 0 C5 1 0.875247 0.239838 0.071318 31.00000 0.03469 0.04165 = 0.03852 -0.01588 0.00644 0.00256 AFIX 43 H5 2 0.922357 0.253333 0.032809 31.00000 -1.20000 AFIX 0 C6 1 0.766198 0.228322 0.075318 31.00000 0.03765 0.03900 = 0.02679 -0.01517 -0.00723 0.00625 AFIX 43 H6 2 0.739030 0.233617 0.039403 31.00000 -1.20000 AFIX 0 C7 1 0.576041 0.198423 0.136269 31.00000 0.03102 0.04521 = 0.05526 -0.01277 -0.00846 -0.00137 AFIX 137 H7A 2 0.558881 0.213280 0.095963 31.00000 -1.50000 H7B 2 0.534886 0.234088 0.162009 31.00000 -1.50000 H7C 2 0.556520 0.140981 0.154071 31.00000 -1.50000 AFIX 0 PART 0 RESI 0 RESI 3 SOLV PART 4 -31 C1 1 0.817797 0.227829 0.103911 -31.00000 0.03679 0.02680 = 0.05901 -0.02119 0.00805 -0.00139 C2 1 0.794847 0.200994 0.168451 -31.00000 0.02326 0.02861 = 0.05263 -0.01445 -0.01563 -0.00164 AFIX 43 H2 2 0.851317 0.195242 0.190472 -31.00000 -1.20000 AFIX 0 C3 1 0.689876 0.183927 0.197445 -31.00000 0.03803 0.02899 = 0.03677 -0.01233 -0.00960 0.00723 AFIX 43 H3 2 0.674861 0.164266 0.239964 -31.00000 -1.20000 AFIX 0 C6 1 0.730128 0.238400 0.075117 -31.00000 0.05065 0.02980 = 0.04215 -0.01780 0.00008 0.00153 AFIX 43 H6 2 0.742908 0.258665 0.032687 -31.00000 -1.20000 AFIX 0 C7 1 0.930064 0.246814 0.070562 -31.00000 0.04950 0.06767 = 0.08028 -0.03555 0.02211 -0.01231 AFIX 137 H7A 2 0.929979 0.296620 0.039194 -31.00000 -1.50000 H7B 2 0.960232 0.200744 0.051750 -31.00000 -1.50000 H7C 2 0.974458 0.255672 0.098619 -31.00000 -1.50000 AFIX 0 C5 1 0.625624 0.220431 0.106159 -31.00000 0.04069 0.03412 = 0.03581 -0.01139 -0.00987 -0.00172 AFIX 43 H5 2 0.567629 0.226242 0.085221 -31.00000 -1.20000 AFIX 0 C4 1 0.606120 0.193856 0.168108 -31.00000 0.03462 0.02931 = 0.03997 -0.01141 -0.01147 0.00477 AFIX 43 H4 2 0.534120 0.182519 0.190206 -31.00000 -1.20000 PART 0 RESI 0 AFIX 0 HKLF 4 REM mks_057m in P-1 REM R1 = 0.0382 for 18999 Fo > 4sig(Fo) and 0.0407 for all 20142 data REM 1392 parameters refined using 266 restraints END WGHT 0.0183 4.4979 REM Highest difference peak 0.580, deepest hole -0.506, 1-sigma level 0.048 Q1 1 0.4408 0.0443 0.8692 11.00000 0.05 0.58 Q2 1 0.1044 0.1408 0.7029 11.00000 0.05 0.55 Q3 1 0.3755 0.2835 0.6146 11.00000 0.05 0.34 Q4 1 0.2420 0.1546 0.3290 11.00000 0.05 0.34 Q5 1 0.5436 0.1773 0.6501 11.00000 0.05 0.29 Q6 1 0.0999 0.0550 1.0119 11.00000 0.05 0.28 Q7 1 0.2109 0.1410 0.2807 11.00000 0.05 0.28 Q8 1 0.2466 0.4269 0.2510 11.00000 0.05 0.28 Q9 1 0.2155 0.2093 1.0684 11.00000 0.05 0.28 Q10 1 0.2104 0.2209 0.2863 11.00000 0.05 0.27 Q11 1 -0.2606 0.1503 0.4086 11.00000 0.05 0.27 Q12 1 0.3555 0.3839 1.0289 11.00000 0.05 0.27 Q13 1 0.4615 0.1134 0.3930 11.00000 0.05 0.27 Q14 1 0.3366 0.1491 0.3446 11.00000 0.05 0.26 Q15 1 0.1201 0.1674 0.3257 11.00000 0.05 0.26 Q16 1 0.3589 0.3030 0.4683 11.00000 0.05 0.25 Q17 1 0.2039 0.4178 0.2101 11.00000 0.05 0.25 Q18 1 0.2224 0.0039 0.2515 11.00000 0.05 0.25 Q19 1 0.2418 0.5438 0.5585 11.00000 0.05 0.25 Q20 1 0.1968 0.2339 0.9220 11.00000 0.05 0.25 ; _shelx_res_checksum 80198 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_073m_sq _database_code_depnum_ccdc_archive 'CCDC 2184019' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H95 B Cl2 F20 Ga2 N6 P2' _chemical_formula_weight 1911.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5203(3) _cell_length_b 16.6728(5) _cell_length_c 23.1865(7) _cell_angle_alpha 78.0634(15) _cell_angle_beta 77.1747(12) _cell_angle_gamma 87.3124(14) _cell_volume 4617.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9506 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 79.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_F_000 1964 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.261 _exptl_crystal_size_mid 0.171 _exptl_crystal_size_min 0.142 _exptl_absorpt_coefficient_mu 2.327 _shelx_estimated_absorpt_T_min 0.582 _shelx_estimated_absorpt_T_max 0.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 Venture (Photon II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/Queen' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 267036 _diffrn_reflns_av_unetI/netI 0.0148 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.709 _diffrn_reflns_theta_max 80.534 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 20020 _reflns_number_gt 18937 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX3(v2017.3-0)' _computing_cell_refinement 'Bruker APEX3(v2017.3-0)' _computing_data_reduction 'Bruker APEX3(v2017.3-0)' _computing_structure_solution 'Bruker APEX3(v2017.3-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The PH hydrogen atoms were refined freely with their P--H bond lengths restrained to be equal (SADI). Disorder: The central Ga(Cl)--PH--P(carbene)--Ga(Cl) moiety is disordered over two positions. For Ga1 and Cl1 a third orientation can be found but a refinement failed due to the low occupancy. The corresponding bond lengths of the carbene were restrained to be equal (SADI) and RIGU restraints were applied to its displacement parameters. For atoms in close proximity additional SIMU restraints were used. SQUEEZE: The structure contains highly disordered solvent - possibly fluoro benzene or toluene. The final refinement was done with a solvent free dataset from a PLATON/SQUEEZE run. (For details see: A.~L.~Spek, Acta Cryst. A46 (1990),194--201). Since the nature and amount of the solvent is not clear it was not included in the sum formula. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+10.5655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 20020 _refine_ls_number_parameters 1274 _refine_ls_number_restraints 200 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.70307(11) 0.81136(7) 0.39311(6) 0.0267(2) Uani 0.7390(19) 1 d . . P A 3 Ga2 Ga 0.81990(11) 0.82523(6) 0.14207(6) 0.0201(2) Uani 0.7390(19) 1 d . . P A 3 Cl1 Cl 0.55015(9) 0.88040(7) 0.41418(7) 0.0345(3) Uani 0.7390(19) 1 d . . P A 3 Cl2 Cl 0.95453(10) 0.90829(7) 0.13768(6) 0.0277(2) Uani 0.7390(19) 1 d . . P A 3 P1 P 0.80341(7) 0.83676(6) 0.29189(4) 0.0235(2) Uani 0.7390(19) 1 d . . P A 3 P2 P 0.71054(8) 0.78084(6) 0.23890(4) 0.0250(3) Uani 0.7390(19) 1 d D . P A 3 H2A H 0.758(5) 0.716(3) 0.248(3) 0.08(2) Uiso 0.7390(19) 1 d D . P A 3 N5 N 0.8561(4) 1.0032(3) 0.2596(3) 0.0326(12) Uani 0.7390(19) 1 d D . P A 3 N6 N 0.6846(4) 0.9895(3) 0.2621(2) 0.0266(10) Uani 0.7390(19) 1 d D . P A 3 C59 C 0.7761(3) 0.9469(3) 0.2703(2) 0.0248(8) Uani 0.7390(19) 1 d D . P A 3 C60 C 0.8162(9) 1.0812(5) 0.2439(9) 0.039(3) Uani 0.7390(19) 1 d D U P A 3 C61 C 0.7065(9) 1.0725(5) 0.2490(10) 0.033(2) Uani 0.7390(19) 1 d D U P A 3 C62 C 0.9718(4) 0.9850(4) 0.2601(3) 0.0440(13) Uani 0.7390(19) 1 d D . P A 3 H62A H 1.017577 1.011730 0.221425 0.066 Uiso 0.7390(19) 1 calc R U P A 3 H62B H 0.983532 0.925627 0.266075 0.066 Uiso 0.7390(19) 1 calc R U P A 3 H62C H 0.991431 1.005624 0.292963 0.066 Uiso 0.7390(19) 1 calc R U P A 3 C63 C 0.5763(4) 0.9577(3) 0.2667(2) 0.0292(10) Uani 0.7390(19) 1 d D . P A 3 H63A H 0.559127 0.968173 0.226557 0.044 Uiso 0.7390(19) 1 calc R U P A 3 H63B H 0.521923 0.984911 0.293656 0.044 Uiso 0.7390(19) 1 calc R U P A 3 H63C H 0.574881 0.898529 0.282934 0.044 Uiso 0.7390(19) 1 calc R U P A 3 C64 C 0.8874(12) 1.1554(6) 0.2310(6) 0.071(4) Uani 0.7390(19) 1 d D U P A 3 H64A H 0.949553 1.151546 0.197485 0.107 Uiso 0.7390(19) 1 calc R U P A 3 H64B H 0.914479 1.158534 0.266973 0.107 Uiso 0.7390(19) 1 calc R U P A 3 H64C H 0.844662 1.204769 0.219917 0.107 Uiso 0.7390(19) 1 calc R U P A 3 C65 C 0.6231(11) 1.1364(6) 0.2366(8) 0.052(3) Uani 0.7390(19) 1 d D . P A 3 H65A H 0.659150 1.189781 0.220623 0.078 Uiso 0.7390(19) 1 calc R U P A 3 H65B H 0.569511 1.138632 0.274159 0.078 Uiso 0.7390(19) 1 calc R U P A 3 H65C H 0.585689 1.122905 0.206965 0.078 Uiso 0.7390(19) 1 calc R U P A 3 Ga1' Ga 0.7189(3) 0.7843(3) 0.38739(17) 0.0363(8) Uani 0.2610(19) 1 d . . P A 4 Ga2' Ga 0.8323(3) 0.85225(19) 0.13467(17) 0.0214(6) Uani 0.2610(19) 1 d . . P A 4 Cl1' Cl 0.5750(3) 0.8655(2) 0.38427(18) 0.0389(8) Uani 0.2610(19) 1 d . . P A 4 Cl2' Cl 0.9799(3) 0.9302(2) 0.11027(19) 0.0281(7) Uani 0.2610(19) 1 d . . P A 4 P1' P 0.8237(2) 0.76754(19) 0.29425(12) 0.0271(7) Uani 0.2610(19) 1 d D . P A 4 H1A' H 0.773(9) 0.706(5) 0.296(6) 0.03(3) Uiso 0.2610(19) 1 d D . P A 4 P2' P 0.7272(2) 0.84406(16) 0.23379(11) 0.0194(7) Uani 0.2610(19) 1 d . . P A 4 N6' N 0.6675(9) 1.0048(8) 0.2437(6) 0.023(3) Uani 0.2610(19) 1 d D . P A 4 N5' N 0.8370(10) 0.9889(8) 0.2466(7) 0.023(3) Uani 0.2610(19) 1 d D . P A 4 C59' C 0.7492(8) 0.9495(6) 0.2420(6) 0.021(2) Uani 0.2610(19) 1 d D . P A 4 C60' C 0.809(2) 1.0690(12) 0.251(2) 0.025(4) Uani 0.2610(19) 1 d D U P A 4 C61' C 0.707(3) 1.0825(12) 0.239(3) 0.029(5) Uani 0.2610(19) 1 d D U P A 4 C62' C 0.9462(10) 0.9560(9) 0.2496(6) 0.035(3) Uani 0.2610(19) 1 d D . P A 4 H62D H 1.001415 0.993627 0.221842 0.052 Uiso 0.2610(19) 1 calc R U P A 4 H62E H 0.953639 0.902417 0.237963 0.052 Uiso 0.2610(19) 1 calc R U P A 4 H62F H 0.956932 0.949951 0.290851 0.052 Uiso 0.2610(19) 1 calc R U P A 4 C63' C 0.5529(9) 0.9877(9) 0.2462(6) 0.029(3) Uani 0.2610(19) 1 d D . P A 4 H63D H 0.527445 1.026187 0.213961 0.043 Uiso 0.2610(19) 1 calc R U P A 4 H63E H 0.508210 0.994027 0.285461 0.043 Uiso 0.2610(19) 1 calc R U P A 4 H63F H 0.546203 0.931485 0.240919 0.043 Uiso 0.2610(19) 1 calc R U P A 4 C64' C 0.892(2) 1.1326(14) 0.2469(13) 0.044(6) Uani 0.2610(19) 1 d D U P A 4 H64D H 0.940334 1.141852 0.206650 0.065 Uiso 0.2610(19) 1 calc R U P A 4 H64E H 0.935355 1.113999 0.277516 0.065 Uiso 0.2610(19) 1 calc R U P A 4 H64F H 0.854420 1.183866 0.253672 0.065 Uiso 0.2610(19) 1 calc R U P A 4 C65' C 0.632(3) 1.1541(19) 0.245(3) 0.057(8) Uani 0.2610(19) 1 d D . P A 4 H65D H 0.672423 1.200805 0.248447 0.085 Uiso 0.2610(19) 1 calc R U P A 4 H65E H 0.572091 1.139646 0.280396 0.085 Uiso 0.2610(19) 1 calc R U P A 4 H65F H 0.600807 1.168962 0.208491 0.085 Uiso 0.2610(19) 1 calc R U P A 4 N1 N 0.6663(2) 0.69613(19) 0.43514(12) 0.0375(6) Uani 1 1 d . . . . . N2 N 0.7906(2) 0.8336(2) 0.44592(12) 0.0396(7) Uani 1 1 d . . . . . N3 N 0.88322(19) 0.74068(16) 0.10473(11) 0.0277(5) Uani 1 1 d . . . . . N4 N 0.74760(19) 0.88516(17) 0.07757(11) 0.0296(5) Uani 1 1 d . . . . . C1 C 0.6537(3) 0.6799(2) 0.49545(15) 0.0403(8) Uani 1 1 d . . . . . C2 C 0.6897(3) 0.7313(2) 0.52685(15) 0.0429(8) Uani 1 1 d . . . . . H2 H 0.662614 0.719448 0.569347 0.051 Uiso 1 1 calc R U . . . C3 C 0.7604(3) 0.7984(3) 0.50467(15) 0.0418(8) Uani 1 1 d . . . . . C4 C 0.6017(3) 0.6004(2) 0.53116(16) 0.0499(9) Uani 1 1 d . . . . . H4A H 0.532178 0.593469 0.519938 0.075 Uiso 1 1 calc R U . . . H4B H 0.588019 0.600862 0.574370 0.075 Uiso 1 1 calc R U . . . H4C H 0.650904 0.554849 0.522473 0.075 Uiso 1 1 calc R U . . . C5 C 0.8065(3) 0.8317(3) 0.55010(16) 0.0555(11) Uani 1 1 d . . . . . H5A H 0.885642 0.839733 0.535407 0.083 Uiso 1 1 calc R U . . . H5B H 0.792165 0.792664 0.588849 0.083 Uiso 1 1 calc R U . . . H5C H 0.771385 0.884234 0.555466 0.083 Uiso 1 1 calc R U . . . C6 C 0.6484(3) 0.6323(3) 0.40523(15) 0.0415(8) Uani 1 1 d . . . . . C7 C 0.5477(3) 0.6256(2) 0.38929(16) 0.0423(8) Uani 1 1 d . . . . . C8 C 0.5364(3) 0.5650(3) 0.35851(18) 0.0506(10) Uani 1 1 d . . . . . H8 H 0.469269 0.560799 0.346624 0.061 Uiso 1 1 calc R U . . . C9 C 0.6200(3) 0.5100(3) 0.34443(18) 0.0549(10) Uani 1 1 d . . . . . H9 H 0.610107 0.468306 0.323684 0.066 Uiso 1 1 calc R U . . . C10 C 0.7179(3) 0.5170(3) 0.36114(18) 0.0544(10) Uani 1 1 d . . . . . H10 H 0.775217 0.479317 0.351688 0.065 Uiso 1 1 calc R U . . . C11 C 0.7351(3) 0.5772(3) 0.39120(16) 0.0445(9) Uani 1 1 d . . . . . C12 C 0.4521(3) 0.6822(2) 0.40497(19) 0.0467(9) Uani 1 1 d . . . . . H12 H 0.473216 0.718584 0.429871 0.056 Uiso 1 1 calc R U . . . C13 C 0.3511(3) 0.6324(3) 0.4429(2) 0.0564(11) Uani 1 1 d . . . . . H13A H 0.329492 0.595586 0.419605 0.085 Uiso 1 1 calc R U . . . H13B H 0.290589 0.669808 0.453477 0.085 Uiso 1 1 calc R U . . . H13C H 0.368995 0.599971 0.479956 0.085 Uiso 1 1 calc R U . . . C14 C 0.4236(3) 0.7367(3) 0.3486(2) 0.0666(13) Uani 1 1 d . . . . . H14A H 0.489040 0.766818 0.324024 0.100 Uiso 1 1 calc R U . . . H14B H 0.366226 0.775706 0.360751 0.100 Uiso 1 1 calc R U . . . H14C H 0.397399 0.702526 0.324939 0.100 Uiso 1 1 calc R U . . . C15 C 0.8454(3) 0.5830(3) 0.40757(17) 0.0488(10) Uani 1 1 d . . . . . H15 H 0.840924 0.628619 0.430069 0.059 Uiso 1 1 calc R U . . . C16 C 0.9358(3) 0.6043(4) 0.3500(2) 0.0804(17) Uani 1 1 d . . . . . H16A H 0.944342 0.559100 0.328207 0.121 Uiso 1 1 calc R U . . . H16B H 1.005035 0.612970 0.360918 0.121 Uiso 1 1 calc R U . . . H16C H 0.915787 0.654403 0.324116 0.121 Uiso 1 1 calc R U . . . C17 C 0.8738(4) 0.5049(3) 0.4480(2) 0.0708(14) Uani 1 1 d . . . . . H17A H 0.879485 0.459409 0.426660 0.106 Uiso 1 1 calc R U . . . H17B H 0.816290 0.492981 0.484924 0.106 Uiso 1 1 calc R U . . . H17C H 0.943901 0.511969 0.458489 0.106 Uiso 1 1 calc R U . . . C18 C 0.8735(3) 0.8970(3) 0.42719(15) 0.0458(9) Uani 1 1 d . . . . . C19 C 0.8464(3) 0.9780(3) 0.43219(17) 0.0548(10) Uani 1 1 d . . . . . C20 C 0.9297(4) 1.0360(3) 0.4155(2) 0.0700(13) Uani 1 1 d . . . . . H20 H 0.912234 1.091505 0.417495 0.084 Uiso 1 1 calc R U . . . C21 C 1.0372(4) 1.0143(4) 0.3960(2) 0.0765(16) Uani 1 1 d . . . . . H21 H 1.093260 1.054526 0.385684 0.092 Uiso 1 1 calc R U . . . C22 C 1.0632(3) 0.9345(4) 0.39159(19) 0.0649(13) Uani 1 1 d . . . . . H22 H 1.137840 0.920481 0.378551 0.078 Uiso 1 1 calc R U . . . C23 C 0.9837(3) 0.8731(3) 0.40559(16) 0.0503(10) Uani 1 1 d . . . . . C24 C 0.7292(3) 1.0042(3) 0.45551(17) 0.0544(10) Uani 1 1 d . . . . . H24 H 0.682552 0.953917 0.470795 0.065 Uiso 1 1 calc R U . . . C25 C 0.6852(4) 1.0588(3) 0.40418(19) 0.0593(11) Uani 1 1 d . . . . . H25A H 0.734733 1.105343 0.385631 0.089 Uiso 1 1 calc R U . . . H25B H 0.612230 1.079068 0.420329 0.089 Uiso 1 1 calc R U . . . H25C H 0.680476 1.026962 0.373731 0.089 Uiso 1 1 calc R U . . . C26 C 0.7218(4) 1.0496(4) 0.5079(2) 0.0713(14) Uani 1 1 d . . . . . H26A H 0.760310 1.102141 0.492645 0.107 Uiso 1 1 calc R U . . . H26B H 0.755681 1.016078 0.539037 0.107 Uiso 1 1 calc R U . . . H26C H 0.644732 1.059455 0.525299 0.107 Uiso 1 1 calc R U . . . C27 C 1.0143(3) 0.7859(3) 0.39907(17) 0.0524(11) Uani 1 1 d . . . . . H27 H 0.949902 0.761060 0.390383 0.063 Uiso 1 1 calc R U . . . C28 C 1.1117(3) 0.7809(3) 0.34688(19) 0.0624(13) Uani 1 1 d . . . . . H28A H 1.121389 0.724121 0.341326 0.094 Uiso 1 1 calc R U . . . H28B H 1.178111 0.799320 0.356050 0.094 Uiso 1 1 calc R U . . . H28C H 1.098036 0.816102 0.309787 0.094 Uiso 1 1 calc R U . . . C29 C 1.0377(4) 0.7337(4) 0.4576(2) 0.095(2) Uani 1 1 d . . . . . H29A H 1.061777 0.678929 0.450894 0.142 Uiso 1 1 calc R U . . . H29B H 0.970861 0.729033 0.489459 0.142 Uiso 1 1 calc R U . . . H29C H 1.095328 0.759723 0.469769 0.142 Uiso 1 1 calc R U . . . C30 C 0.9064(2) 0.74984(19) 0.04426(13) 0.0280(6) Uani 1 1 d . . . . . C31 C 0.8659(2) 0.8142(2) 0.00658(13) 0.0296(6) Uani 1 1 d . . . . . H31 H 0.897236 0.819695 -0.035298 0.036 Uiso 1 1 calc R U . . . C32 C 0.7851(2) 0.8722(2) 0.02166(13) 0.0325(7) Uani 1 1 d . . . . . C33 C 0.9793(3) 0.6879(2) 0.01568(14) 0.0349(7) Uani 1 1 d . . . . . H33A H 0.979645 0.697829 -0.027530 0.052 Uiso 1 1 calc R U . . . H33B H 0.951649 0.632559 0.034895 0.052 Uiso 1 1 calc R U . . . H33C H 1.053936 0.692930 0.021058 0.052 Uiso 1 1 calc R U . . . C34 C 0.7410(3) 0.9217(3) -0.03025(15) 0.0470(9) Uani 1 1 d . . . . . H34A H 0.793250 0.965025 -0.052884 0.070 Uiso 1 1 calc R U . . . H34B H 0.670809 0.946487 -0.014570 0.070 Uiso 1 1 calc R U . . . H34C H 0.730162 0.885818 -0.057025 0.070 Uiso 1 1 calc R U . . . C35 C 0.9010(2) 0.6623(2) 0.14193(13) 0.0302(6) Uani 1 1 d . . . . . C36 C 1.0004(2) 0.64524(19) 0.16105(13) 0.0288(6) Uani 1 1 d . . . . . C37 C 1.0104(3) 0.5699(2) 0.19879(14) 0.0345(7) Uani 1 1 d . . . . . H37 H 1.076859 0.556888 0.212006 0.041 Uiso 1 1 calc R U . . . C38 C 0.9257(3) 0.5134(2) 0.21752(15) 0.0394(8) Uani 1 1 d . . . . . H38 H 0.934188 0.462616 0.243630 0.047 Uiso 1 1 calc R U . . . C39 C 0.8288(3) 0.5311(2) 0.19810(15) 0.0397(8) Uani 1 1 d . . . . . H39 H 0.771116 0.492038 0.211049 0.048 Uiso 1 1 calc R U . . . C40 C 0.8144(3) 0.6054(2) 0.15979(14) 0.0342(7) Uani 1 1 d . . . . . C41 C 1.0937(2) 0.70626(19) 0.14340(14) 0.0291(6) Uani 1 1 d . . . . . H41 H 1.074170 0.753965 0.113565 0.035 Uiso 1 1 calc R U . . . C42 C 1.1080(3) 0.7378(2) 0.19874(16) 0.0400(8) Uani 1 1 d . . . . . H42A H 1.162854 0.781571 0.186110 0.060 Uiso 1 1 calc R U . . . H42B H 1.132343 0.692716 0.227395 0.060 Uiso 1 1 calc R U . . . H42C H 1.037952 0.759148 0.218134 0.060 Uiso 1 1 calc R U . . . C43 C 1.2015(2) 0.6700(2) 0.11373(16) 0.0362(7) Uani 1 1 d . . . . . H43A H 1.191573 0.650533 0.078167 0.054 Uiso 1 1 calc R U . . . H43B H 1.223357 0.624029 0.142616 0.054 Uiso 1 1 calc R U . . . H43C H 1.258521 0.712209 0.101410 0.054 Uiso 1 1 calc R U . . . C44 C 0.7079(3) 0.6225(2) 0.13709(16) 0.0420(8) Uani 1 1 d . . . . . H44 H 0.702479 0.682947 0.122231 0.050 Uiso 1 1 calc R U . . . C45 C 0.6064(3) 0.5953(3) 0.1866(2) 0.0606(12) Uani 1 1 d . . . . . H45A H 0.540605 0.608196 0.170113 0.091 Uiso 1 1 calc R U . . . H45B H 0.603422 0.624147 0.219736 0.091 Uiso 1 1 calc R U . . . H45C H 0.609908 0.536055 0.201866 0.091 Uiso 1 1 calc R U . . . C46 C 0.7102(3) 0.5800(3) 0.08386(19) 0.0534(10) Uani 1 1 d . . . . . H46A H 0.640314 0.589232 0.071106 0.080 Uiso 1 1 calc R U . . . H46B H 0.721822 0.521057 0.096494 0.080 Uiso 1 1 calc R U . . . H46C H 0.769958 0.602808 0.050095 0.080 Uiso 1 1 calc R U . . . C47 C 0.6612(2) 0.9440(2) 0.08895(13) 0.0323(7) Uani 1 1 d . . . . . C48 C 0.6849(3) 1.0281(2) 0.07512(14) 0.0373(7) Uani 1 1 d . . . . . C49 C 0.5983(3) 1.0829(3) 0.08649(16) 0.0455(9) Uani 1 1 d . . . . . H49 H 0.612752 1.140057 0.078164 0.055 Uiso 1 1 calc R U . . . C50 C 0.4919(3) 1.0551(3) 0.10966(18) 0.0493(10) Uani 1 1 d . . . . . H50 H 0.433837 1.093160 0.116245 0.059 Uiso 1 1 calc R U . . . C51 C 0.4700(3) 0.9724(3) 0.12318(17) 0.0437(9) Uani 1 1 d . . . . . H51 H 0.396691 0.954152 0.139361 0.052 Uiso 1 1 calc R U . . . C52 C 0.5531(3) 0.9146(2) 0.11369(15) 0.0366(7) Uani 1 1 d . . . . . C53 C 0.7997(3) 1.0636(2) 0.04769(16) 0.0435(9) Uani 1 1 d . . . . . H53 H 0.850520 1.017571 0.038608 0.052 Uiso 1 1 calc R U . . . C54 C 0.8417(3) 1.1050(2) 0.0913(2) 0.0519(10) Uani 1 1 d . . . . . H54A H 0.916373 1.124919 0.072960 0.078 Uiso 1 1 calc R U . . . H54B H 0.841738 1.065296 0.128940 0.078 Uiso 1 1 calc R U . . . H54C H 0.793859 1.151182 0.099985 0.078 Uiso 1 1 calc R U . . . C55 C 0.8019(4) 1.1260(3) -0.0118(2) 0.0700(15) Uani 1 1 d . . . . . H55A H 0.878006 1.140353 -0.031878 0.105 Uiso 1 1 calc R U . . . H55B H 0.761675 1.175413 -0.002975 0.105 Uiso 1 1 calc R U . . . H55C H 0.767546 1.101750 -0.038207 0.105 Uiso 1 1 calc R U . . . C56 C 0.5262(3) 0.8246(2) 0.12720(16) 0.0411(8) Uani 1 1 d . . . . . H56 H 0.590966 0.794067 0.139463 0.049 Uiso 1 1 calc R U . . . C57 C 0.4275(3) 0.8003(3) 0.1792(2) 0.0550(11) Uani 1 1 d . . . . . H57A H 0.361102 0.825047 0.167234 0.083 Uiso 1 1 calc R U . . . H57B H 0.437867 0.819651 0.214657 0.083 Uiso 1 1 calc R U . . . H57C H 0.420013 0.740444 0.188965 0.083 Uiso 1 1 calc R U . . . C58 C 0.5097(3) 0.7966(3) 0.07065(19) 0.0566(11) Uani 1 1 d . . . . . H58A H 0.450234 0.828372 0.055507 0.085 Uiso 1 1 calc R U . . . H58B H 0.490893 0.738232 0.080973 0.085 Uiso 1 1 calc R U . . . H58C H 0.577456 0.805405 0.039421 0.085 Uiso 1 1 calc R U . . . F12_1 F 0.05713(12) 0.28533(10) 0.22175(7) 0.0280(4) Uani 1 1 d . . . . . F13_1 F -0.09160(13) 0.34961(12) 0.16052(9) 0.0378(4) Uani 1 1 d . . . . . F14_1 F -0.03794(15) 0.47303(12) 0.06245(9) 0.0406(5) Uani 1 1 d . . . . . F15_1 F 0.17466(15) 0.52495(11) 0.02322(8) 0.0361(4) Uani 1 1 d . . . . . F16_1 F 0.32735(13) 0.45601(11) 0.07960(8) 0.0325(4) Uani 1 1 d . . . . . F22_1 F 0.14285(14) 0.27600(12) 0.32315(8) 0.0364(4) Uani 1 1 d . . . . . F23_1 F 0.09552(18) 0.36844(16) 0.40532(10) 0.0558(6) Uani 1 1 d . . . . . F24_1 F 0.1789(2) 0.52296(17) 0.38244(11) 0.0648(7) Uani 1 1 d . . . . . F25_1 F 0.3060(2) 0.58509(13) 0.27161(11) 0.0560(6) Uani 1 1 d . . . . . F26_1 F 0.35262(16) 0.49416(11) 0.18757(9) 0.0383(4) Uani 1 1 d . . . . . F32_1 F 0.37579(14) 0.28654(12) 0.07845(9) 0.0379(4) Uani 1 1 d . . . . . F33_1 F 0.58345(16) 0.29037(14) 0.01860(9) 0.0478(5) Uani 1 1 d . . . . . F34_1 F 0.74562(14) 0.33025(13) 0.06872(10) 0.0482(5) Uani 1 1 d . . . . . F35_1 F 0.69171(14) 0.37154(13) 0.17962(10) 0.0460(5) Uani 1 1 d . . . . . F36_1 F 0.48669(14) 0.37510(12) 0.23782(8) 0.0356(4) Uani 1 1 d . . . . . F42_1 F 0.19123(14) 0.19510(11) 0.14566(8) 0.0326(4) Uani 1 1 d . . . . . F43_1 F 0.20392(15) 0.03511(12) 0.18215(9) 0.0414(5) Uani 1 1 d . . . . . F44_1 F 0.29118(18) -0.03054(12) 0.27915(10) 0.0506(6) Uani 1 1 d . . . . . F45_1 F 0.36851(18) 0.07180(13) 0.33885(8) 0.0469(5) Uani 1 1 d . . . . . F46_1 F 0.36735(14) 0.23254(11) 0.29985(8) 0.0331(4) Uani 1 1 d . . . . . C11_1 C 0.2017(2) 0.36429(17) 0.15345(12) 0.0227(5) Uani 1 1 d . . . . . C12_1 C 0.0920(2) 0.34262(17) 0.17117(12) 0.0236(5) Uani 1 1 d . . . . . C13_1 C 0.0125(2) 0.37595(19) 0.14053(14) 0.0275(6) Uani 1 1 d . . . . . C14_1 C 0.0394(2) 0.43794(19) 0.09060(14) 0.0295(6) Uani 1 1 d . . . . . C15_1 C 0.1464(2) 0.46376(18) 0.07146(13) 0.0279(6) Uani 1 1 d . . . . . C16_1 C 0.2245(2) 0.42691(18) 0.10251(13) 0.0252(6) Uani 1 1 d . . . . . C21_1 C 0.2558(2) 0.37858(19) 0.25120(13) 0.0273(6) Uani 1 1 d . . . . . C22_1 C 0.1877(2) 0.3522(2) 0.30733(14) 0.0322(7) Uani 1 1 d . . . . . C23_1 C 0.1609(3) 0.3988(2) 0.35148(15) 0.0404(8) Uani 1 1 d . . . . . C24_1 C 0.2020(3) 0.4772(3) 0.33954(18) 0.0465(10) Uani 1 1 d . . . . . C25_1 C 0.2665(3) 0.5080(2) 0.28416(18) 0.0407(8) Uani 1 1 d . . . . . C26_1 C 0.2906(3) 0.4595(2) 0.24110(16) 0.0338(7) Uani 1 1 d . . . . . C31_1 C 0.4177(2) 0.33344(18) 0.16061(14) 0.0262(6) Uani 1 1 d . . . . . C32_1 C 0.4508(2) 0.31106(19) 0.10488(14) 0.0300(6) Uani 1 1 d . . . . . C33_1 C 0.5583(3) 0.3113(2) 0.07306(15) 0.0352(7) Uani 1 1 d . . . . . C34_1 C 0.6402(2) 0.3323(2) 0.09783(16) 0.0353(7) Uani 1 1 d . . . . . C35_1 C 0.6128(2) 0.35265(19) 0.15314(16) 0.0335(7) Uani 1 1 d . . . . . C36_1 C 0.5039(2) 0.35367(18) 0.18347(14) 0.0285(6) Uani 1 1 d . . . . . C41_1 C 0.2765(2) 0.22470(18) 0.22153(12) 0.0242(6) Uani 1 1 d . . . . . C42_1 C 0.2367(2) 0.16911(19) 0.19410(13) 0.0272(6) Uani 1 1 d . . . . . C43_1 C 0.2413(2) 0.08496(19) 0.21266(15) 0.0320(7) Uani 1 1 d . . . . . C44_1 C 0.2855(3) 0.05130(19) 0.26131(15) 0.0359(7) Uani 1 1 d . . . . . C45_1 C 0.3249(3) 0.1025(2) 0.29084(14) 0.0341(7) Uani 1 1 d . . . . . C46_1 C 0.3217(2) 0.18668(19) 0.27002(13) 0.0287(6) Uani 1 1 d . . . . . B1_1 B 0.2874(2) 0.3258(2) 0.19642(14) 0.0223(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0161(4) 0.0434(5) 0.0203(4) -0.0082(3) -0.0022(3) 0.0031(3) Ga2 0.0167(4) 0.0241(5) 0.0190(4) -0.0052(4) -0.0028(3) 0.0035(4) Cl1 0.0242(5) 0.0402(6) 0.0397(7) -0.0126(5) -0.0057(5) 0.0084(4) Cl2 0.0247(5) 0.0265(6) 0.0316(6) -0.0082(5) -0.0021(5) -0.0038(4) P1 0.0172(4) 0.0320(6) 0.0220(5) -0.0067(4) -0.0045(3) 0.0013(4) P2 0.0232(5) 0.0295(6) 0.0215(5) -0.0053(4) -0.0016(4) -0.0053(4) N5 0.027(2) 0.040(3) 0.032(3) -0.0110(19) -0.0009(17) -0.0160(18) N6 0.027(2) 0.024(2) 0.028(3) -0.0039(19) -0.0061(17) -0.0022(16) C59 0.0199(18) 0.030(2) 0.026(2) -0.0102(17) -0.0034(17) -0.0039(16) C60 0.044(3) 0.034(3) 0.034(7) -0.003(4) 0.001(3) -0.016(3) C61 0.044(3) 0.026(3) 0.026(7) 0.000(4) -0.006(3) -0.004(2) C62 0.023(2) 0.065(4) 0.049(3) -0.026(3) -0.002(2) -0.014(2) C63 0.025(2) 0.029(2) 0.035(3) -0.0047(19) -0.0101(18) 0.0020(17) C64 0.079(6) 0.055(6) 0.075(8) -0.007(5) -0.003(5) -0.043(5) C65 0.062(4) 0.027(4) 0.061(6) 0.003(4) -0.011(4) 0.003(4) Ga1' 0.0137(10) 0.075(3) 0.0155(9) -0.0052(14) 0.0029(7) 0.0050(14) Ga2' 0.0179(10) 0.0279(16) 0.0170(10) -0.0039(12) -0.0018(7) 0.0031(12) Cl1' 0.0306(16) 0.053(2) 0.0315(18) -0.0099(15) -0.0038(13) 0.0116(14) Cl2' 0.0205(14) 0.0283(16) 0.0331(18) -0.0063(14) 0.0004(13) -0.0031(11) P1' 0.0240(14) 0.0328(17) 0.0217(13) -0.0036(11) -0.0023(10) 0.0080(11) P2' 0.0153(11) 0.0226(15) 0.0202(12) -0.0057(10) -0.0020(9) -0.0012(9) N6' 0.021(4) 0.023(5) 0.024(7) -0.003(5) -0.004(4) 0.003(3) N5' 0.022(5) 0.022(5) 0.029(7) -0.010(5) -0.008(4) -0.002(4) C59' 0.018(4) 0.022(5) 0.023(6) -0.005(4) -0.006(4) -0.001(4) C60' 0.040(7) 0.017(6) 0.013(8) 0.005(6) -0.004(7) -0.013(5) C61' 0.043(7) 0.017(6) 0.023(15) 0.008(7) -0.011(7) -0.007(4) C62' 0.021(5) 0.049(8) 0.034(7) 0.001(6) -0.012(5) -0.009(5) C63' 0.021(5) 0.036(8) 0.032(7) -0.014(6) -0.004(5) -0.001(5) C64' 0.041(8) 0.040(11) 0.053(14) -0.028(12) 0.002(9) -0.017(8) C65' 0.064(13) 0.031(11) 0.08(2) -0.009(12) -0.033(12) 0.010(11) N1 0.0229(12) 0.0604(19) 0.0267(13) -0.0090(13) -0.0016(10) 0.0067(12) N2 0.0253(13) 0.071(2) 0.0221(12) -0.0091(13) -0.0057(10) 0.0006(13) N3 0.0200(11) 0.0399(14) 0.0214(11) -0.0037(10) -0.0027(9) -0.0034(10) N4 0.0211(11) 0.0458(15) 0.0221(12) -0.0086(11) -0.0047(9) 0.0070(10) C1 0.0282(16) 0.058(2) 0.0295(16) -0.0042(15) -0.0015(13) 0.0108(15) C2 0.0345(17) 0.066(2) 0.0238(15) -0.0056(15) -0.0031(13) 0.0099(16) C3 0.0333(17) 0.067(2) 0.0249(15) -0.0110(16) -0.0064(13) 0.0098(16) C4 0.058(2) 0.052(2) 0.0321(18) -0.0029(16) -0.0020(16) 0.0119(19) C5 0.052(2) 0.092(3) 0.0254(17) -0.0148(19) -0.0120(16) 0.002(2) C6 0.0274(16) 0.067(2) 0.0278(16) -0.0099(16) -0.0008(13) 0.0014(15) C7 0.0261(16) 0.061(2) 0.0355(18) -0.0045(16) -0.0014(13) -0.0016(15) C8 0.0324(18) 0.072(3) 0.046(2) -0.0112(19) -0.0043(16) -0.0076(18) C9 0.047(2) 0.074(3) 0.046(2) -0.020(2) -0.0037(18) -0.012(2) C10 0.0367(19) 0.082(3) 0.048(2) -0.030(2) -0.0009(16) 0.0051(19) C11 0.0269(16) 0.069(3) 0.0370(18) -0.0175(17) -0.0002(14) 0.0035(16) C12 0.0263(16) 0.053(2) 0.058(2) -0.0035(18) -0.0112(16) -0.0014(15) C13 0.0289(18) 0.060(3) 0.073(3) -0.009(2) 0.0008(18) -0.0034(17) C14 0.041(2) 0.072(3) 0.082(3) 0.013(3) -0.027(2) -0.012(2) C15 0.0277(17) 0.076(3) 0.046(2) -0.027(2) -0.0043(15) 0.0117(17) C16 0.030(2) 0.154(6) 0.062(3) -0.047(3) 0.0035(19) -0.002(3) C17 0.047(2) 0.082(3) 0.094(4) -0.034(3) -0.025(2) 0.015(2) C18 0.0374(18) 0.078(3) 0.0236(16) -0.0115(17) -0.0078(14) -0.0058(18) C19 0.050(2) 0.081(3) 0.0339(19) -0.016(2) -0.0042(17) -0.007(2) C20 0.075(3) 0.077(3) 0.057(3) -0.025(2) 0.003(2) -0.019(3) C21 0.058(3) 0.113(5) 0.060(3) -0.031(3) 0.003(2) -0.031(3) C22 0.038(2) 0.113(4) 0.047(2) -0.028(3) -0.0045(18) -0.013(2) C23 0.0313(17) 0.094(3) 0.0267(17) -0.0109(18) -0.0088(14) -0.0059(19) C24 0.053(2) 0.072(3) 0.0344(19) -0.0114(19) -0.0012(17) 0.004(2) C25 0.073(3) 0.064(3) 0.043(2) -0.013(2) -0.013(2) 0.000(2) C26 0.072(3) 0.103(4) 0.040(2) -0.024(2) -0.007(2) 0.012(3) C27 0.0251(17) 0.094(3) 0.0373(19) -0.010(2) -0.0085(14) 0.0036(18) C28 0.0290(19) 0.110(4) 0.050(2) -0.030(2) -0.0006(17) -0.002(2) C29 0.074(3) 0.151(6) 0.044(3) 0.001(3) -0.010(2) 0.054(4) C30 0.0231(14) 0.0349(16) 0.0264(14) -0.0081(12) -0.0032(11) -0.0057(12) C31 0.0263(14) 0.0415(17) 0.0209(13) -0.0083(12) -0.0031(11) 0.0009(12) C32 0.0280(15) 0.0459(19) 0.0234(14) -0.0072(13) -0.0051(12) 0.0008(13) C33 0.0439(18) 0.0307(16) 0.0302(16) -0.0075(13) -0.0076(14) 0.0007(14) C34 0.050(2) 0.067(3) 0.0252(16) -0.0113(16) -0.0119(15) 0.0243(19) C35 0.0250(14) 0.0385(17) 0.0242(14) -0.0030(12) -0.0021(11) -0.0013(12) C36 0.0237(14) 0.0368(16) 0.0244(14) -0.0073(12) -0.0016(11) 0.0007(12) C37 0.0298(15) 0.0444(19) 0.0271(15) -0.0048(13) -0.0047(12) 0.0029(13) C38 0.0410(18) 0.045(2) 0.0266(16) 0.0015(14) -0.0029(13) -0.0011(15) C39 0.0349(17) 0.044(2) 0.0341(17) 0.0011(15) -0.0013(14) -0.0099(15) C40 0.0268(15) 0.0428(18) 0.0300(16) -0.0037(13) -0.0024(12) -0.0049(13) C41 0.0201(13) 0.0357(16) 0.0310(15) -0.0087(13) -0.0034(11) 0.0031(12) C42 0.0299(16) 0.052(2) 0.0441(19) -0.0203(16) -0.0128(14) 0.0073(15) C43 0.0231(15) 0.0400(18) 0.0409(18) -0.0072(14) 0.0007(13) 0.0039(13) C44 0.0293(16) 0.048(2) 0.045(2) 0.0036(16) -0.0107(14) -0.0102(15) C45 0.0312(19) 0.078(3) 0.064(3) 0.005(2) -0.0066(18) -0.0125(19) C46 0.051(2) 0.052(2) 0.062(3) -0.004(2) -0.027(2) -0.0116(18) C47 0.0230(14) 0.053(2) 0.0227(14) -0.0126(13) -0.0056(11) 0.0087(13) C48 0.0316(16) 0.051(2) 0.0273(15) -0.0092(14) -0.0023(13) 0.0107(14) C49 0.0368(18) 0.055(2) 0.0414(19) -0.0152(17) 0.0003(15) 0.0155(16) C50 0.0313(18) 0.071(3) 0.049(2) -0.028(2) -0.0060(16) 0.0213(18) C51 0.0242(16) 0.068(3) 0.046(2) -0.0293(19) -0.0067(14) 0.0082(16) C52 0.0238(15) 0.061(2) 0.0315(16) -0.0198(15) -0.0105(12) 0.0066(14) C53 0.0329(17) 0.047(2) 0.0385(18) 0.0018(15) 0.0065(14) 0.0105(15) C54 0.0358(19) 0.043(2) 0.068(3) -0.0109(19) 0.0085(18) -0.0038(16) C55 0.063(3) 0.069(3) 0.050(2) 0.015(2) 0.016(2) 0.025(2) C56 0.0223(15) 0.065(2) 0.0418(19) -0.0190(17) -0.0121(13) 0.0023(15) C57 0.0263(17) 0.077(3) 0.062(3) -0.022(2) -0.0029(17) -0.0082(18) C58 0.050(2) 0.075(3) 0.057(2) -0.028(2) -0.025(2) 0.000(2) F12_1 0.0183(7) 0.0321(9) 0.0299(9) 0.0008(7) -0.0037(6) -0.0005(6) F13_1 0.0173(8) 0.0451(11) 0.0498(11) -0.0026(9) -0.0116(8) 0.0009(7) F14_1 0.0333(10) 0.0467(11) 0.0437(11) 0.0005(9) -0.0230(8) 0.0084(8) F15_1 0.0419(10) 0.0340(10) 0.0297(9) 0.0041(7) -0.0118(8) -0.0009(8) F16_1 0.0235(8) 0.0353(10) 0.0344(9) 0.0019(8) -0.0043(7) -0.0068(7) F22_1 0.0276(9) 0.0502(11) 0.0302(9) -0.0121(8) -0.0006(7) 0.0017(8) F23_1 0.0435(12) 0.0897(18) 0.0384(11) -0.0323(12) -0.0033(9) 0.0180(12) F24_1 0.0660(15) 0.0831(18) 0.0682(16) -0.0569(14) -0.0308(13) 0.0350(13) F25_1 0.0709(15) 0.0359(11) 0.0789(16) -0.0289(11) -0.0402(13) 0.0139(10) F26_1 0.0439(11) 0.0281(9) 0.0462(11) -0.0059(8) -0.0186(9) 0.0022(8) F32_1 0.0254(9) 0.0521(12) 0.0395(10) -0.0217(9) -0.0015(8) -0.0028(8) F33_1 0.0334(10) 0.0601(14) 0.0445(12) -0.0191(10) 0.0101(9) 0.0037(9) F34_1 0.0172(8) 0.0502(12) 0.0634(14) 0.0030(10) 0.0061(8) 0.0021(8) F35_1 0.0195(9) 0.0525(12) 0.0654(14) -0.0002(10) -0.0177(9) -0.0040(8) F36_1 0.0246(9) 0.0438(11) 0.0423(10) -0.0084(8) -0.0161(8) 0.0017(7) F42_1 0.0305(9) 0.0344(10) 0.0373(10) -0.0140(8) -0.0104(7) 0.0014(7) F43_1 0.0351(10) 0.0340(10) 0.0537(12) -0.0200(9) 0.0050(9) -0.0055(8) F44_1 0.0570(13) 0.0251(10) 0.0529(13) 0.0034(9) 0.0121(10) 0.0032(9) F45_1 0.0546(12) 0.0471(12) 0.0289(10) 0.0048(8) -0.0034(9) 0.0183(10) F46_1 0.0307(9) 0.0406(10) 0.0296(9) -0.0062(8) -0.0118(7) 0.0069(8) C11_1 0.0198(12) 0.0245(14) 0.0253(13) -0.0079(11) -0.0060(10) 0.0027(10) C12_1 0.0216(13) 0.0251(14) 0.0236(13) -0.0039(11) -0.0054(10) 0.0021(10) C13_1 0.0186(13) 0.0316(15) 0.0345(16) -0.0099(12) -0.0077(11) 0.0017(11) C14_1 0.0274(14) 0.0331(16) 0.0321(15) -0.0072(12) -0.0158(12) 0.0068(12) C15_1 0.0307(15) 0.0287(15) 0.0245(14) -0.0035(11) -0.0086(12) 0.0022(12) C16_1 0.0203(13) 0.0277(14) 0.0280(14) -0.0073(11) -0.0041(11) -0.0014(11) C21_1 0.0206(13) 0.0360(16) 0.0308(15) -0.0131(12) -0.0140(11) 0.0111(11) C22_1 0.0229(14) 0.0442(18) 0.0344(16) -0.0154(14) -0.0115(12) 0.0099(13) C23_1 0.0276(16) 0.063(2) 0.0345(17) -0.0191(16) -0.0081(13) 0.0149(15) C24_1 0.0401(19) 0.062(2) 0.055(2) -0.041(2) -0.0264(17) 0.0286(17) C25_1 0.0400(18) 0.0378(18) 0.057(2) -0.0234(16) -0.0282(17) 0.0179(15) C26_1 0.0303(15) 0.0355(17) 0.0442(18) -0.0162(14) -0.0212(14) 0.0120(13) C31_1 0.0175(12) 0.0252(14) 0.0344(15) -0.0029(12) -0.0061(11) 0.0013(10) C32_1 0.0212(14) 0.0313(16) 0.0351(16) -0.0051(13) -0.0024(12) 0.0000(11) C33_1 0.0262(15) 0.0360(17) 0.0377(17) -0.0052(14) 0.0023(13) 0.0030(13) C34_1 0.0171(13) 0.0308(16) 0.0482(19) 0.0044(14) 0.0017(13) 0.0009(11) C35_1 0.0191(13) 0.0285(15) 0.0505(19) 0.0038(14) -0.0127(13) -0.0028(11) C36_1 0.0239(14) 0.0248(14) 0.0368(16) -0.0021(12) -0.0110(12) 0.0019(11) C41_1 0.0154(12) 0.0297(15) 0.0241(13) -0.0045(11) 0.0015(10) 0.0019(10) C42_1 0.0179(13) 0.0322(15) 0.0294(15) -0.0082(12) 0.0007(11) 0.0021(11) C43_1 0.0234(14) 0.0306(16) 0.0376(17) -0.0124(13) 0.0081(12) -0.0020(12) C44_1 0.0323(16) 0.0269(15) 0.0376(17) -0.0013(13) 0.0100(13) 0.0029(12) C45_1 0.0310(16) 0.0343(17) 0.0264(15) 0.0054(12) 0.0033(12) 0.0103(13) C46_1 0.0216(13) 0.0369(16) 0.0249(14) -0.0055(12) -0.0008(11) 0.0029(12) B1_1 0.0166(13) 0.0247(15) 0.0264(15) -0.0061(12) -0.0058(11) 0.0021(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.913(3) . ? Ga1 N1 1.991(3) . ? Ga1 Cl1 2.2000(14) . ? Ga1 P1 2.3655(16) . ? Ga2 N3 1.860(3) . ? Ga2 N4 1.988(3) . ? Ga2 Cl2 2.2032(15) . ? Ga2 P2 2.3466(16) . ? P1 C59 1.838(4) . ? P1 P2 2.2227(14) . ? N5 C59 1.351(5) . ? N5 C60 1.378(8) . ? N5 C62 1.468(6) . ? N6 C59 1.348(6) . ? N6 C61 1.380(7) . ? N6 C63 1.453(6) . ? C60 C61 1.364(9) . ? C60 C64 1.498(8) . ? C61 C65 1.487(9) . ? Ga1' N1 1.707(5) . ? Ga1' N2 2.097(5) . ? Ga1' Cl1' 2.207(4) . ? Ga1' P1' 2.328(4) . ? Ga2' N4 1.856(5) . ? Ga2' N3 2.139(4) . ? Ga2' Cl2' 2.210(4) . ? Ga2' P2' 2.361(5) . ? P1' P2' 2.218(4) . ? P2' C59' 1.846(11) . ? N6' C59' 1.344(12) . ? N6' C61' 1.384(15) . ? N6' C63' 1.462(12) . ? N5' C59' 1.342(12) . ? N5' C60' 1.383(15) . ? N5' C62' 1.460(12) . ? C60' C61' 1.369(17) . ? C60' C64' 1.489(14) . ? C61' C65' 1.496(16) . ? N1 C1 1.343(4) . ? N1 C6 1.435(5) . ? N2 C3 1.343(4) . ? N2 C18 1.448(5) . ? N3 C30 1.345(4) . ? N3 C35 1.447(4) . ? N4 C32 1.336(4) . ? N4 C47 1.443(4) . ? C1 C2 1.381(5) . ? C1 C4 1.502(5) . ? C2 C3 1.398(5) . ? C3 C5 1.513(5) . ? C6 C7 1.405(5) . ? C6 C11 1.415(5) . ? C7 C8 1.381(6) . ? C7 C12 1.517(5) . ? C8 C9 1.387(6) . ? C9 C10 1.382(6) . ? C10 C11 1.384(6) . ? C11 C15 1.523(5) . ? C12 C14 1.532(6) . ? C12 C13 1.537(5) . ? C15 C17 1.516(6) . ? C15 C16 1.537(5) . ? C18 C19 1.399(6) . ? C18 C23 1.427(5) . ? C19 C20 1.390(6) . ? C19 C24 1.524(6) . ? C20 C21 1.377(7) . ? C21 C22 1.375(8) . ? C22 C23 1.400(6) . ? C23 C27 1.516(6) . ? C24 C25 1.531(6) . ? C24 C26 1.543(6) . ? C27 C28 1.528(5) . ? C27 C29 1.532(6) . ? C30 C31 1.389(4) . ? C30 C33 1.505(4) . ? C31 C32 1.405(4) . ? C32 C34 1.509(4) . ? C35 C40 1.408(4) . ? C35 C36 1.409(4) . ? C36 C37 1.393(4) . ? C36 C41 1.514(4) . ? C37 C38 1.385(5) . ? C38 C39 1.385(5) . ? C39 C40 1.397(5) . ? C40 C44 1.532(4) . ? C41 C43 1.531(4) . ? C41 C42 1.531(4) . ? C44 C45 1.527(5) . ? C44 C46 1.539(6) . ? C47 C48 1.403(5) . ? C47 C52 1.415(4) . ? C48 C49 1.400(5) . ? C48 C53 1.529(5) . ? C49 C50 1.384(5) . ? C50 C51 1.376(6) . ? C51 C52 1.397(5) . ? C52 C56 1.506(5) . ? C53 C54 1.527(6) . ? C53 C55 1.541(5) . ? C56 C57 1.526(5) . ? C56 C58 1.537(5) . ? F12_1 C12_1 1.352(3) . ? F13_1 C13_1 1.344(3) . ? F14_1 C14_1 1.332(3) . ? F15_1 C15_1 1.343(3) . ? F16_1 C16_1 1.350(3) . ? F22_1 C22_1 1.359(4) . ? F23_1 C23_1 1.345(4) . ? F24_1 C24_1 1.350(4) . ? F25_1 C25_1 1.350(4) . ? F26_1 C26_1 1.339(4) . ? F32_1 C32_1 1.349(3) . ? F33_1 C33_1 1.345(4) . ? F34_1 C34_1 1.345(3) . ? F35_1 C35_1 1.353(4) . ? F36_1 C36_1 1.349(4) . ? F42_1 C42_1 1.354(3) . ? F43_1 C43_1 1.355(4) . ? F44_1 C44_1 1.345(4) . ? F45_1 C45_1 1.344(4) . ? F46_1 C46_1 1.351(4) . ? C11_1 C12_1 1.386(4) . ? C11_1 C16_1 1.391(4) . ? C11_1 B1_1 1.644(4) . ? C12_1 C13_1 1.380(4) . ? C13_1 C14_1 1.374(4) . ? C14_1 C15_1 1.374(4) . ? C15_1 C16_1 1.388(4) . ? C21_1 C22_1 1.385(4) . ? C21_1 C26_1 1.395(4) . ? C21_1 B1_1 1.659(4) . ? C22_1 C23_1 1.385(4) . ? C23_1 C24_1 1.377(6) . ? C24_1 C25_1 1.368(6) . ? C25_1 C26_1 1.385(4) . ? C31_1 C36_1 1.386(4) . ? C31_1 C32_1 1.389(4) . ? C31_1 B1_1 1.655(4) . ? C32_1 C33_1 1.383(4) . ? C33_1 C34_1 1.373(5) . ? C34_1 C35_1 1.361(5) . ? C35_1 C36_1 1.390(4) . ? C41_1 C46_1 1.392(4) . ? C41_1 C42_1 1.393(4) . ? C41_1 B1_1 1.667(4) . ? C42_1 C43_1 1.382(4) . ? C43_1 C44_1 1.371(5) . ? C44_1 C45_1 1.369(5) . ? C45_1 C46_1 1.388(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 96.48(14) . . ? N2 Ga1 Cl1 105.43(10) . . ? N1 Ga1 Cl1 104.99(10) . . ? N2 Ga1 P1 110.68(10) . . ? N1 Ga1 P1 118.85(9) . . ? Cl1 Ga1 P1 117.68(7) . . ? N3 Ga2 N4 98.82(12) . . ? N3 Ga2 Cl2 106.26(10) . . ? N4 Ga2 Cl2 102.64(9) . . ? N3 Ga2 P2 114.16(9) . . ? N4 Ga2 P2 118.06(10) . . ? Cl2 Ga2 P2 114.93(7) . . ? C59 P1 P2 103.18(16) . . ? C59 P1 Ga1 99.66(14) . . ? P2 P1 Ga1 107.23(6) . . ? P1 P2 Ga2 99.12(5) . . ? C59 N5 C60 110.8(6) . . ? C59 N5 C62 125.6(5) . . ? C60 N5 C62 123.5(6) . . ? C59 N6 C61 109.7(5) . . ? C59 N6 C63 128.0(4) . . ? C61 N6 C63 122.3(5) . . ? N6 C59 N5 106.0(4) . . ? N6 C59 P1 132.6(4) . . ? N5 C59 P1 121.3(4) . . ? C61 C60 N5 105.8(7) . . ? C61 C60 C64 132.2(9) . . ? N5 C60 C64 121.8(8) . . ? C60 C61 N6 107.4(7) . . ? C60 C61 C65 129.0(9) . . ? N6 C61 C65 123.2(8) . . ? N1 Ga1' N2 99.4(2) . . ? N1 Ga1' Cl1' 103.9(2) . . ? N2 Ga1' Cl1' 100.03(18) . . ? N1 Ga1' P1' 115.2(2) . . ? N2 Ga1' P1' 119.8(2) . . ? Cl1' Ga1' P1' 115.8(2) . . ? N4 Ga2' N3 93.8(2) . . ? N4 Ga2' Cl2' 109.14(18) . . ? N3 Ga2' Cl2' 105.98(19) . . ? N4 Ga2' P2' 111.5(2) . . ? N3 Ga2' P2' 118.45(15) . . ? Cl2' Ga2' P2' 115.7(2) . . ? P2' P1' Ga1' 99.61(15) . . ? C59' P2' P1' 103.6(4) . . ? C59' P2' Ga2' 98.5(4) . . ? P1' P2' Ga2' 105.94(15) . . ? C59' N6' C61' 110.9(15) . . ? C59' N6' C63' 125.6(12) . . ? C61' N6' C63' 123.5(15) . . ? C59' N5' C60' 109.9(13) . . ? C59' N5' C62' 128.1(12) . . ? C60' N5' C62' 122.0(14) . . ? N5' C59' N6' 105.7(10) . . ? N5' C59' P2' 133.2(9) . . ? N6' C59' P2' 121.1(9) . . ? C61' C60' N5' 106.8(19) . . ? C61' C60' C64' 126(2) . . ? N5' C60' C64' 123(2) . . ? C60' C61' N6' 104.3(18) . . ? C60' C61' C65' 130(3) . . ? N6' C61' C65' 122(2) . . ? C1 N1 C6 119.5(3) . . ? C1 N1 Ga1' 125.7(3) . . ? C6 N1 Ga1' 114.2(2) . . ? C1 N1 Ga1 116.4(3) . . ? C6 N1 Ga1 124.0(2) . . ? C3 N2 C18 119.2(3) . . ? C3 N2 Ga1 117.5(2) . . ? C18 N2 Ga1 122.3(2) . . ? C3 N2 Ga1' 115.5(3) . . ? C18 N2 Ga1' 125.1(2) . . ? C30 N3 C35 119.9(3) . . ? C30 N3 Ga2 121.1(2) . . ? C35 N3 Ga2 118.89(19) . . ? C30 N3 Ga2' 113.1(2) . . ? C35 N3 Ga2' 126.9(2) . . ? C32 N4 C47 120.0(3) . . ? C32 N4 Ga2' 119.0(2) . . ? C47 N4 Ga2' 118.5(2) . . ? C32 N4 Ga2 117.7(2) . . ? C47 N4 Ga2 122.22(19) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 C4 119.0(3) . . ? C2 C1 C4 117.5(3) . . ? C1 C2 C3 128.9(3) . . ? N2 C3 C2 123.9(3) . . ? N2 C3 C5 118.9(4) . . ? C2 C3 C5 117.3(3) . . ? C7 C6 C11 120.7(4) . . ? C7 C6 N1 120.8(3) . . ? C11 C6 N1 118.5(3) . . ? C8 C7 C6 118.4(3) . . ? C8 C7 C12 119.4(3) . . ? C6 C7 C12 122.2(4) . . ? C7 C8 C9 122.0(4) . . ? C10 C9 C8 118.8(4) . . ? C9 C10 C11 122.1(4) . . ? C10 C11 C6 118.1(3) . . ? C10 C11 C15 119.9(3) . . ? C6 C11 C15 122.0(3) . . ? C7 C12 C14 112.1(4) . . ? C7 C12 C13 110.4(3) . . ? C14 C12 C13 110.1(3) . . ? C17 C15 C11 112.1(4) . . ? C17 C15 C16 110.5(4) . . ? C11 C15 C16 110.2(3) . . ? C19 C18 C23 121.7(4) . . ? C19 C18 N2 120.8(3) . . ? C23 C18 N2 117.5(4) . . ? C20 C19 C18 118.4(4) . . ? C20 C19 C24 119.4(5) . . ? C18 C19 C24 122.1(4) . . ? C21 C20 C19 121.3(5) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C23 122.4(4) . . ? C22 C23 C18 116.3(4) . . ? C22 C23 C27 121.3(4) . . ? C18 C23 C27 122.4(4) . . ? C19 C24 C25 110.1(3) . . ? C19 C24 C26 111.3(4) . . ? C25 C24 C26 110.1(4) . . ? C23 C27 C28 113.1(4) . . ? C23 C27 C29 111.8(4) . . ? C28 C27 C29 109.5(4) . . ? N3 C30 C31 123.0(3) . . ? N3 C30 C33 119.0(3) . . ? C31 C30 C33 118.1(3) . . ? C30 C31 C32 129.1(3) . . ? N4 C32 C31 124.2(3) . . ? N4 C32 C34 120.2(3) . . ? C31 C32 C34 115.7(3) . . ? C40 C35 C36 121.6(3) . . ? C40 C35 N3 117.6(3) . . ? C36 C35 N3 120.7(3) . . ? C37 C36 C35 117.7(3) . . ? C37 C36 C41 119.8(3) . . ? C35 C36 C41 122.5(3) . . ? C38 C37 C36 121.6(3) . . ? C39 C38 C37 119.9(3) . . ? C38 C39 C40 121.1(3) . . ? C39 C40 C35 118.0(3) . . ? C39 C40 C44 120.2(3) . . ? C35 C40 C44 121.7(3) . . ? C36 C41 C43 112.3(3) . . ? C36 C41 C42 110.1(3) . . ? C43 C41 C42 110.2(3) . . ? C45 C44 C40 112.6(3) . . ? C45 C44 C46 109.6(3) . . ? C40 C44 C46 110.4(3) . . ? C48 C47 C52 121.5(3) . . ? C48 C47 N4 120.2(3) . . ? C52 C47 N4 118.3(3) . . ? C49 C48 C47 118.1(3) . . ? C49 C48 C53 118.0(3) . . ? C47 C48 C53 123.9(3) . . ? C50 C49 C48 121.0(4) . . ? C51 C50 C49 120.1(3) . . ? C50 C51 C52 121.6(3) . . ? C51 C52 C47 117.6(3) . . ? C51 C52 C56 120.4(3) . . ? C47 C52 C56 121.9(3) . . ? C54 C53 C48 111.7(3) . . ? C54 C53 C55 109.1(4) . . ? C48 C53 C55 111.3(3) . . ? C52 C56 C57 113.6(3) . . ? C52 C56 C58 111.3(3) . . ? C57 C56 C58 110.1(3) . . ? C12_1 C11_1 C16_1 113.4(2) . . ? C12_1 C11_1 B1_1 120.2(2) . . ? C16_1 C11_1 B1_1 125.9(2) . . ? F12_1 C12_1 C13_1 115.8(2) . . ? F12_1 C12_1 C11_1 119.8(2) . . ? C13_1 C12_1 C11_1 124.5(3) . . ? F13_1 C13_1 C14_1 120.1(3) . . ? F13_1 C13_1 C12_1 120.1(3) . . ? C14_1 C13_1 C12_1 119.7(3) . . ? F14_1 C14_1 C13_1 120.1(3) . . ? F14_1 C14_1 C15_1 121.2(3) . . ? C13_1 C14_1 C15_1 118.7(3) . . ? F15_1 C15_1 C14_1 119.9(3) . . ? F15_1 C15_1 C16_1 120.3(3) . . ? C14_1 C15_1 C16_1 119.7(3) . . ? F16_1 C16_1 C15_1 115.1(3) . . ? F16_1 C16_1 C11_1 121.0(2) . . ? C15_1 C16_1 C11_1 123.9(3) . . ? C22_1 C21_1 C26_1 113.8(3) . . ? C22_1 C21_1 B1_1 125.8(3) . . ? C26_1 C21_1 B1_1 120.3(3) . . ? F22_1 C22_1 C23_1 114.8(3) . . ? F22_1 C22_1 C21_1 121.0(3) . . ? C23_1 C22_1 C21_1 124.2(3) . . ? F23_1 C23_1 C24_1 120.2(3) . . ? F23_1 C23_1 C22_1 120.7(4) . . ? C24_1 C23_1 C22_1 119.1(3) . . ? F24_1 C24_1 C25_1 120.3(4) . . ? F24_1 C24_1 C23_1 120.0(4) . . ? C25_1 C24_1 C23_1 119.6(3) . . ? F25_1 C25_1 C24_1 120.2(3) . . ? F25_1 C25_1 C26_1 120.3(4) . . ? C24_1 C25_1 C26_1 119.4(3) . . ? F26_1 C26_1 C25_1 116.2(3) . . ? F26_1 C26_1 C21_1 120.0(3) . . ? C25_1 C26_1 C21_1 123.8(3) . . ? C36_1 C31_1 C32_1 113.5(3) . . ? C36_1 C31_1 B1_1 125.9(3) . . ? C32_1 C31_1 B1_1 120.3(2) . . ? F32_1 C32_1 C33_1 115.6(3) . . ? F32_1 C32_1 C31_1 119.9(2) . . ? C33_1 C32_1 C31_1 124.5(3) . . ? F33_1 C33_1 C34_1 119.7(3) . . ? F33_1 C33_1 C32_1 120.9(3) . . ? C34_1 C33_1 C32_1 119.4(3) . . ? F34_1 C34_1 C35_1 120.8(3) . . ? F34_1 C34_1 C33_1 120.5(3) . . ? C35_1 C34_1 C33_1 118.7(3) . . ? F35_1 C35_1 C34_1 120.3(3) . . ? F35_1 C35_1 C36_1 119.0(3) . . ? C34_1 C35_1 C36_1 120.7(3) . . ? F36_1 C36_1 C31_1 121.4(3) . . ? F36_1 C36_1 C35_1 115.4(3) . . ? C31_1 C36_1 C35_1 123.2(3) . . ? C46_1 C41_1 C42_1 112.9(3) . . ? C46_1 C41_1 B1_1 120.4(3) . . ? C42_1 C41_1 B1_1 126.2(3) . . ? F42_1 C42_1 C43_1 115.0(3) . . ? F42_1 C42_1 C41_1 121.1(3) . . ? C43_1 C42_1 C41_1 123.9(3) . . ? F43_1 C43_1 C44_1 119.5(3) . . ? F43_1 C43_1 C42_1 120.1(3) . . ? C44_1 C43_1 C42_1 120.3(3) . . ? F44_1 C44_1 C45_1 120.7(3) . . ? F44_1 C44_1 C43_1 120.6(3) . . ? C45_1 C44_1 C43_1 118.8(3) . . ? F45_1 C45_1 C44_1 120.5(3) . . ? F45_1 C45_1 C46_1 120.1(3) . . ? C44_1 C45_1 C46_1 119.4(3) . . ? F46_1 C46_1 C45_1 115.5(3) . . ? F46_1 C46_1 C41_1 119.8(3) . . ? C45_1 C46_1 C41_1 124.6(3) . . ? C11_1 B1_1 C31_1 113.8(2) . . ? C11_1 B1_1 C21_1 101.8(2) . . ? C31_1 B1_1 C21_1 113.8(2) . . ? C11_1 B1_1 C41_1 114.1(2) . . ? C31_1 B1_1 C41_1 100.7(2) . . ? C21_1 B1_1 C41_1 113.2(2) . . ? _refine_diff_density_max 1.084 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.067 _shelx_res_file ; TITL mks_073m in P-1 mks_073m_sq.res created by SHELXL-2017/1 at 15:39:11 on 23-Feb-2022 CELL 1.54178 12.52030 16.67280 23.18650 78.0634 77.1747 87.3124 ZERR 2.00000 0.00030 0.00050 0.00070 0.0015 0.0012 0.0014 LATT 1 SFAC C H B Cl F Ga N P UNIT 178 190 2 4 40 4 12 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.142 0.171 0.261 L.S. 16 0 53 ACTA FMAP 2 SADI_SOLV c1 c2 c2 c3 c3 c4 c4 c5 c5 c6 c6 c1 SADI_SOLV c1 c3 c3 c5 c5 c1 c2 c4 c4 c6 c6 c2 RIGU_SOLV SADI c59 n5 c59 n6 c59' n5' c59' n6' SADI n5 c60 n6 c61 n5' c60' n6' c61' SADI c60 c61 c60' c61' SADI c60 c64 c61 c65 c60' c64' c61' c65' SADI n5 c62 n6 c63 n5' c62' n6' c63' RIGU n5 n6 c59 c60 c61 c62 c63 c64 c65 = N5' N6' C59' C60' C61' C62' C63' C64' C65' SIMU c64 c64' c56 c65' SIMU c60 c61 c60' c61' PLAN 20 SADI p2 h2a p1' h1a' ABIN WGHT 0.000000 10.565500 FVAR 0.10470 0.40480 0.73898 0.25457 0.02441 PART 3 31 GA1 6 0.703066 0.811363 0.393106 31.00000 0.01613 0.04343 = 0.02028 -0.00815 -0.00221 0.00307 GA2 6 0.819897 0.825234 0.142068 31.00000 0.01668 0.02406 = 0.01905 -0.00519 -0.00278 0.00345 CL1 4 0.550146 0.880397 0.414177 31.00000 0.02424 0.04021 = 0.03973 -0.01260 -0.00571 0.00836 CL2 4 0.954534 0.908287 0.137685 31.00000 0.02468 0.02645 = 0.03156 -0.00822 -0.00209 -0.00382 P1 8 0.803412 0.836760 0.291886 31.00000 0.01717 0.03203 = 0.02199 -0.00672 -0.00454 0.00134 P2 8 0.710537 0.780838 0.238903 31.00000 0.02318 0.02946 = 0.02148 -0.00533 -0.00164 -0.00530 H2A 2 0.757736 0.715521 0.248409 31.00000 0.07857 N5 7 0.856052 1.003173 0.259613 31.00000 0.02674 0.03961 = 0.03216 -0.01100 -0.00088 -0.01602 N6 7 0.684616 0.989538 0.262055 31.00000 0.02730 0.02376 = 0.02831 -0.00394 -0.00613 -0.00224 C59 1 0.776105 0.946929 0.270254 31.00000 0.01991 0.03040 = 0.02567 -0.01020 -0.00337 -0.00392 C60 1 0.816193 1.081249 0.243945 31.00000 0.04376 0.03390 = 0.03423 -0.00315 0.00121 -0.01568 C61 1 0.706495 1.072466 0.249033 31.00000 0.04361 0.02585 = 0.02558 0.00027 -0.00563 -0.00390 C62 1 0.971763 0.985031 0.260056 31.00000 0.02279 0.06525 = 0.04902 -0.02603 -0.00223 -0.01436 AFIX 137 H62A 2 1.017577 1.011730 0.221425 31.00000 -1.50000 H62B 2 0.983532 0.925627 0.266075 31.00000 -1.50000 H62C 2 0.991431 1.005624 0.292963 31.00000 -1.50000 AFIX 0 C63 1 0.576324 0.957696 0.266677 31.00000 0.02454 0.02861 = 0.03520 -0.00473 -0.01011 0.00196 AFIX 137 H63A 2 0.559127 0.968173 0.226557 31.00000 -1.50000 H63B 2 0.521923 0.984911 0.293656 31.00000 -1.50000 H63C 2 0.574881 0.898529 0.282934 31.00000 -1.50000 AFIX 0 C64 1 0.887379 1.155442 0.230956 31.00000 0.07920 0.05494 = 0.07529 -0.00703 -0.00337 -0.04340 AFIX 137 H64A 2 0.949553 1.151546 0.197485 31.00000 -1.50000 H64B 2 0.914479 1.158534 0.266973 31.00000 -1.50000 H64C 2 0.844662 1.204769 0.219917 31.00000 -1.50000 AFIX 0 C65 1 0.623104 1.136394 0.236639 31.00000 0.06198 0.02668 = 0.06120 0.00333 -0.01149 0.00320 AFIX 137 H65A 2 0.659150 1.189781 0.220623 31.00000 -1.50000 H65B 2 0.569511 1.138632 0.274159 31.00000 -1.50000 H65C 2 0.585689 1.122905 0.206965 31.00000 -1.50000 AFIX 0 PART 0 PART 4 -31 GA1' 6 0.718860 0.784310 0.387389 -31.00000 0.01373 0.07451 = 0.01548 -0.00522 0.00292 0.00502 GA2' 6 0.832276 0.852249 0.134673 -31.00000 0.01787 0.02792 = 0.01696 -0.00389 -0.00184 0.00311 CL1' 4 0.575007 0.865483 0.384271 -31.00000 0.03055 0.05268 = 0.03155 -0.00987 -0.00376 0.01163 CL2' 4 0.979930 0.930176 0.110266 -31.00000 0.02045 0.02834 = 0.03305 -0.00631 0.00040 -0.00311 P1' 8 0.823663 0.767540 0.294247 -31.00000 0.02403 0.03281 = 0.02166 -0.00362 -0.00226 0.00798 H1A' 2 0.773188 0.705986 0.296448 -31.00000 0.02860 P2' 8 0.727180 0.844060 0.233793 -31.00000 0.01527 0.02261 = 0.02017 -0.00565 -0.00198 -0.00116 N6' 7 0.667522 1.004772 0.243663 -31.00000 0.02087 0.02311 = 0.02368 -0.00278 -0.00410 0.00328 N5' 7 0.836959 0.988934 0.246619 -31.00000 0.02164 0.02195 = 0.02914 -0.00958 -0.00829 -0.00247 C59' 1 0.749209 0.949472 0.242036 -31.00000 0.01807 0.02248 = 0.02331 -0.00505 -0.00554 -0.00107 C60' 1 0.809346 1.069005 0.251261 -31.00000 0.04017 0.01750 = 0.01321 0.00482 -0.00388 -0.01290 C61' 1 0.706956 1.082460 0.239396 -31.00000 0.04313 0.01704 = 0.02295 0.00820 -0.01084 -0.00681 C62' 1 0.946221 0.956026 0.249561 -31.00000 0.02095 0.04864 = 0.03382 0.00148 -0.01206 -0.00861 AFIX 137 H62D 2 1.001415 0.993627 0.221842 -31.00000 -1.50000 H62E 2 0.953639 0.902417 0.237963 -31.00000 -1.50000 H62F 2 0.956932 0.949951 0.290851 -31.00000 -1.50000 AFIX 0 C63' 1 0.552896 0.987712 0.246211 -31.00000 0.02086 0.03612 = 0.03219 -0.01357 -0.00434 -0.00137 AFIX 137 H63D 2 0.527445 1.026187 0.213961 -31.00000 -1.50000 H63E 2 0.508210 0.994027 0.285461 -31.00000 -1.50000 H63F 2 0.546203 0.931485 0.240919 -31.00000 -1.50000 AFIX 0 C64' 1 0.891916 1.132613 0.246903 -31.00000 0.04133 0.04042 = 0.05325 -0.02843 0.00215 -0.01706 AFIX 137 H64D 2 0.940334 1.141852 0.206650 -31.00000 -1.50000 H64E 2 0.935355 1.113999 0.277516 -31.00000 -1.50000 H64F 2 0.854420 1.183866 0.253672 -31.00000 -1.50000 AFIX 0 C65' 1 0.631570 1.154149 0.244634 -31.00000 0.06426 0.03090 = 0.08150 -0.00905 -0.03255 0.00990 AFIX 137 H65D 2 0.672423 1.200805 0.248447 -31.00000 -1.50000 H65E 2 0.572091 1.139646 0.280396 -31.00000 -1.50000 H65F 2 0.600807 1.168962 0.208491 -31.00000 -1.50000 AFIX 0 PART 0 N1 7 0.666303 0.696129 0.435143 11.00000 0.02290 0.06040 = 0.02667 -0.00899 -0.00155 0.00672 N2 7 0.790605 0.833607 0.445919 11.00000 0.02527 0.07147 = 0.02208 -0.00912 -0.00572 0.00063 N3 7 0.883225 0.740678 0.104732 11.00000 0.02004 0.03995 = 0.02143 -0.00368 -0.00268 -0.00339 N4 7 0.747602 0.885161 0.077570 11.00000 0.02112 0.04577 = 0.02214 -0.00858 -0.00471 0.00700 C1 1 0.653694 0.679889 0.495452 11.00000 0.02816 0.05789 = 0.02954 -0.00420 -0.00155 0.01082 C2 1 0.689678 0.731319 0.526845 11.00000 0.03452 0.06624 = 0.02377 -0.00559 -0.00306 0.00988 AFIX 43 H2 2 0.662614 0.719448 0.569347 11.00000 -1.20000 AFIX 0 C3 1 0.760445 0.798432 0.504672 11.00000 0.03333 0.06694 = 0.02489 -0.01102 -0.00645 0.00984 C4 1 0.601681 0.600359 0.531160 11.00000 0.05773 0.05239 = 0.03212 -0.00286 -0.00202 0.01191 AFIX 137 H4A 2 0.532178 0.593469 0.519938 11.00000 -1.50000 H4B 2 0.588019 0.600862 0.574370 11.00000 -1.50000 H4C 2 0.650904 0.554849 0.522473 11.00000 -1.50000 AFIX 0 C5 1 0.806464 0.831696 0.550101 11.00000 0.05222 0.09167 = 0.02538 -0.01484 -0.01205 0.00241 AFIX 137 H5A 2 0.885642 0.839733 0.535407 11.00000 -1.50000 H5B 2 0.792165 0.792664 0.588849 11.00000 -1.50000 H5C 2 0.771385 0.884234 0.555466 11.00000 -1.50000 AFIX 0 C6 1 0.648418 0.632294 0.405232 11.00000 0.02742 0.06686 = 0.02782 -0.00990 -0.00077 0.00135 C7 1 0.547742 0.625573 0.389293 11.00000 0.02611 0.06053 = 0.03547 -0.00446 -0.00143 -0.00163 C8 1 0.536358 0.564965 0.358509 11.00000 0.03237 0.07216 = 0.04562 -0.01121 -0.00432 -0.00762 AFIX 43 H8 2 0.469269 0.560799 0.346624 11.00000 -1.20000 AFIX 0 C9 1 0.619980 0.509993 0.344429 11.00000 0.04711 0.07357 = 0.04583 -0.02030 -0.00366 -0.01153 AFIX 43 H9 2 0.610107 0.468306 0.323684 11.00000 -1.20000 AFIX 0 C10 1 0.717900 0.516996 0.361138 11.00000 0.03666 0.08197 = 0.04752 -0.02995 -0.00091 0.00513 AFIX 43 H10 2 0.775217 0.479317 0.351688 11.00000 -1.20000 AFIX 0 C11 1 0.735078 0.577169 0.391200 11.00000 0.02689 0.06896 = 0.03702 -0.01747 -0.00022 0.00350 C12 1 0.452056 0.682175 0.404971 11.00000 0.02633 0.05336 = 0.05822 -0.00347 -0.01125 -0.00143 AFIX 13 H12 2 0.473216 0.718584 0.429871 11.00000 -1.20000 AFIX 0 C13 1 0.351137 0.632371 0.442944 11.00000 0.02889 0.06016 = 0.07278 -0.00867 0.00077 -0.00343 AFIX 137 H13A 2 0.329492 0.595586 0.419605 11.00000 -1.50000 H13B 2 0.290589 0.669808 0.453477 11.00000 -1.50000 H13C 2 0.368995 0.599971 0.479956 11.00000 -1.50000 AFIX 0 C14 1 0.423618 0.736720 0.348592 11.00000 0.04086 0.07204 = 0.08203 0.01257 -0.02708 -0.01176 AFIX 137 H14A 2 0.489040 0.766818 0.324024 11.00000 -1.50000 H14B 2 0.366226 0.775706 0.360751 11.00000 -1.50000 H14C 2 0.397399 0.702526 0.324939 11.00000 -1.50000 AFIX 0 C15 1 0.845353 0.583032 0.407573 11.00000 0.02773 0.07647 = 0.04600 -0.02733 -0.00432 0.01170 AFIX 13 H15 2 0.840924 0.628619 0.430069 11.00000 -1.20000 AFIX 0 C16 1 0.935825 0.604303 0.349987 11.00000 0.03025 0.15389 = 0.06202 -0.04709 0.00353 -0.00202 AFIX 137 H16A 2 0.944342 0.559100 0.328207 11.00000 -1.50000 H16B 2 1.005035 0.612970 0.360918 11.00000 -1.50000 H16C 2 0.915787 0.654403 0.324116 11.00000 -1.50000 AFIX 0 C17 1 0.873770 0.504941 0.447986 11.00000 0.04661 0.08175 = 0.09415 -0.03376 -0.02485 0.01510 AFIX 137 H17A 2 0.879485 0.459409 0.426660 11.00000 -1.50000 H17B 2 0.816290 0.492981 0.484924 11.00000 -1.50000 H17C 2 0.943901 0.511969 0.458489 11.00000 -1.50000 AFIX 0 C18 1 0.873518 0.897048 0.427194 11.00000 0.03740 0.07805 = 0.02362 -0.01154 -0.00776 -0.00580 C19 1 0.846364 0.978040 0.432185 11.00000 0.04993 0.08086 = 0.03387 -0.01577 -0.00417 -0.00743 C20 1 0.929731 1.035952 0.415466 11.00000 0.07467 0.07690 = 0.05717 -0.02534 0.00310 -0.01876 AFIX 43 H20 2 0.912234 1.091505 0.417495 11.00000 -1.20000 AFIX 0 C21 1 1.037183 1.014331 0.396021 11.00000 0.05808 0.11289 = 0.06009 -0.03114 0.00317 -0.03098 AFIX 43 H21 2 1.093260 1.054526 0.385684 11.00000 -1.20000 AFIX 0 C22 1 1.063202 0.934486 0.391588 11.00000 0.03833 0.11349 = 0.04705 -0.02828 -0.00447 -0.01251 AFIX 43 H22 2 1.137840 0.920481 0.378551 11.00000 -1.20000 AFIX 0 C23 1 0.983677 0.873075 0.405593 11.00000 0.03132 0.09410 = 0.02674 -0.01091 -0.00885 -0.00585 C24 1 0.729160 1.004194 0.455507 11.00000 0.05298 0.07175 = 0.03443 -0.01139 -0.00116 0.00366 AFIX 13 H24 2 0.682552 0.953917 0.470795 11.00000 -1.20000 AFIX 0 C25 1 0.685194 1.058805 0.404182 11.00000 0.07255 0.06360 = 0.04269 -0.01281 -0.01291 0.00023 AFIX 137 H25A 2 0.734733 1.105343 0.385631 11.00000 -1.50000 H25B 2 0.612230 1.079068 0.420329 11.00000 -1.50000 H25C 2 0.680476 1.026962 0.373731 11.00000 -1.50000 AFIX 0 C26 1 0.721799 1.049612 0.507904 11.00000 0.07190 0.10271 = 0.04012 -0.02408 -0.00721 0.01190 AFIX 137 H26A 2 0.760310 1.102141 0.492645 11.00000 -1.50000 H26B 2 0.755681 1.016078 0.539037 11.00000 -1.50000 H26C 2 0.644732 1.059455 0.525299 11.00000 -1.50000 AFIX 0 C27 1 1.014324 0.785857 0.399073 11.00000 0.02510 0.09367 = 0.03734 -0.00981 -0.00845 0.00362 AFIX 13 H27 2 0.949902 0.761060 0.390383 11.00000 -1.20000 AFIX 0 C28 1 1.111694 0.780906 0.346880 11.00000 0.02900 0.11038 = 0.05037 -0.03020 -0.00061 -0.00217 AFIX 137 H28A 2 1.121389 0.724121 0.341326 11.00000 -1.50000 H28B 2 1.178111 0.799320 0.356050 11.00000 -1.50000 H28C 2 1.098036 0.816102 0.309787 11.00000 -1.50000 AFIX 0 C29 1 1.037675 0.733689 0.457565 11.00000 0.07380 0.15078 = 0.04361 0.00101 -0.00980 0.05449 AFIX 137 H29A 2 1.061777 0.678929 0.450894 11.00000 -1.50000 H29B 2 0.970861 0.729033 0.489459 11.00000 -1.50000 H29C 2 1.095328 0.759723 0.469769 11.00000 -1.50000 AFIX 0 C30 1 0.906357 0.749839 0.044264 11.00000 0.02315 0.03487 = 0.02642 -0.00811 -0.00316 -0.00572 C31 1 0.865868 0.814161 0.006576 11.00000 0.02626 0.04150 = 0.02086 -0.00830 -0.00312 0.00092 AFIX 43 H31 2 0.897236 0.819695 -0.035298 11.00000 -1.20000 AFIX 0 C32 1 0.785063 0.872187 0.021663 11.00000 0.02802 0.04590 = 0.02343 -0.00720 -0.00511 0.00075 C33 1 0.979256 0.687885 0.015678 11.00000 0.04393 0.03072 = 0.03022 -0.00754 -0.00756 0.00067 AFIX 137 H33A 2 0.979645 0.697829 -0.027530 11.00000 -1.50000 H33B 2 0.951649 0.632559 0.034895 11.00000 -1.50000 H33C 2 1.053936 0.692930 0.021058 11.00000 -1.50000 AFIX 0 C34 1 0.740955 0.921721 -0.030255 11.00000 0.04957 0.06656 = 0.02517 -0.01126 -0.01192 0.02426 AFIX 137 H34A 2 0.793250 0.965025 -0.052884 11.00000 -1.50000 H34B 2 0.670809 0.946487 -0.014570 11.00000 -1.50000 H34C 2 0.730162 0.885818 -0.057025 11.00000 -1.50000 AFIX 0 C35 1 0.900989 0.662307 0.141930 11.00000 0.02498 0.03851 = 0.02419 -0.00300 -0.00215 -0.00128 C36 1 1.000392 0.645236 0.161046 11.00000 0.02373 0.03681 = 0.02441 -0.00729 -0.00162 0.00068 C37 1 1.010383 0.569875 0.198786 11.00000 0.02980 0.04444 = 0.02712 -0.00477 -0.00472 0.00286 AFIX 43 H37 2 1.076859 0.556888 0.212006 11.00000 -1.20000 AFIX 0 C38 1 0.925741 0.513392 0.217515 11.00000 0.04098 0.04478 = 0.02664 0.00155 -0.00287 -0.00105 AFIX 43 H38 2 0.934188 0.462616 0.243630 11.00000 -1.20000 AFIX 0 C39 1 0.828794 0.531088 0.198099 11.00000 0.03487 0.04423 = 0.03412 0.00109 -0.00130 -0.00991 AFIX 43 H39 2 0.771116 0.492038 0.211049 11.00000 -1.20000 AFIX 0 C40 1 0.814356 0.605396 0.159785 11.00000 0.02678 0.04284 = 0.03000 -0.00372 -0.00240 -0.00492 C41 1 1.093676 0.706257 0.143398 11.00000 0.02007 0.03572 = 0.03096 -0.00870 -0.00342 0.00306 AFIX 13 H41 2 1.074170 0.753965 0.113565 11.00000 -1.20000 AFIX 0 C42 1 1.107995 0.737758 0.198739 11.00000 0.02986 0.05235 = 0.04414 -0.02032 -0.01277 0.00725 AFIX 137 H42A 2 1.162854 0.781571 0.186110 11.00000 -1.50000 H42B 2 1.132343 0.692716 0.227395 11.00000 -1.50000 H42C 2 1.037952 0.759148 0.218134 11.00000 -1.50000 AFIX 0 C43 1 1.201481 0.669994 0.113728 11.00000 0.02310 0.03999 = 0.04091 -0.00717 0.00074 0.00388 AFIX 137 H43A 2 1.191573 0.650533 0.078167 11.00000 -1.50000 H43B 2 1.223357 0.624029 0.142616 11.00000 -1.50000 H43C 2 1.258521 0.712209 0.101410 11.00000 -1.50000 AFIX 0 C44 1 0.707910 0.622479 0.137089 11.00000 0.02934 0.04811 = 0.04501 0.00360 -0.01068 -0.01015 AFIX 13 H44 2 0.702479 0.682947 0.122231 11.00000 -1.20000 AFIX 0 C45 1 0.606366 0.595284 0.186639 11.00000 0.03117 0.07760 = 0.06395 0.00490 -0.00659 -0.01249 AFIX 137 H45A 2 0.540605 0.608196 0.170113 11.00000 -1.50000 H45B 2 0.603422 0.624147 0.219736 11.00000 -1.50000 H45C 2 0.609908 0.536055 0.201866 11.00000 -1.50000 AFIX 0 C46 1 0.710210 0.580041 0.083864 11.00000 0.05069 0.05224 = 0.06216 -0.00397 -0.02689 -0.01157 AFIX 137 H46A 2 0.640314 0.589232 0.071106 11.00000 -1.50000 H46B 2 0.721822 0.521057 0.096494 11.00000 -1.50000 H46C 2 0.769958 0.602808 0.050095 11.00000 -1.50000 AFIX 0 C47 1 0.661189 0.944009 0.088948 11.00000 0.02296 0.05294 = 0.02267 -0.01260 -0.00560 0.00872 C48 1 0.684934 1.028108 0.075119 11.00000 0.03158 0.05062 = 0.02728 -0.00922 -0.00228 0.01072 C49 1 0.598287 1.082909 0.086486 11.00000 0.03679 0.05508 = 0.04139 -0.01522 0.00031 0.01554 AFIX 43 H49 2 0.612752 1.140057 0.078164 11.00000 -1.20000 AFIX 0 C50 1 0.491900 1.055077 0.109659 11.00000 0.03133 0.07073 = 0.04930 -0.02762 -0.00597 0.02129 AFIX 43 H50 2 0.433837 1.093160 0.116245 11.00000 -1.20000 AFIX 0 C51 1 0.470041 0.972373 0.123179 11.00000 0.02421 0.06787 = 0.04573 -0.02929 -0.00674 0.00821 AFIX 43 H51 2 0.396691 0.954152 0.139361 11.00000 -1.20000 AFIX 0 C52 1 0.553091 0.914553 0.113685 11.00000 0.02381 0.06058 = 0.03151 -0.01977 -0.01053 0.00664 C53 1 0.799679 1.063600 0.047691 11.00000 0.03290 0.04666 = 0.03854 0.00183 0.00649 0.01047 AFIX 13 H53 2 0.850520 1.017571 0.038608 11.00000 -1.20000 AFIX 0 C54 1 0.841675 1.104954 0.091301 11.00000 0.03577 0.04269 = 0.06815 -0.01090 0.00848 -0.00379 AFIX 137 H54A 2 0.916373 1.124919 0.072960 11.00000 -1.50000 H54B 2 0.841738 1.065296 0.128940 11.00000 -1.50000 H54C 2 0.793859 1.151182 0.099985 11.00000 -1.50000 AFIX 0 C55 1 0.801931 1.125952 -0.011751 11.00000 0.06336 0.06876 = 0.05020 0.01473 0.01610 0.02468 AFIX 137 H55A 2 0.878006 1.140353 -0.031878 11.00000 -1.50000 H55B 2 0.761675 1.175413 -0.002975 11.00000 -1.50000 H55C 2 0.767546 1.101750 -0.038207 11.00000 -1.50000 AFIX 0 C56 1 0.526250 0.824586 0.127203 11.00000 0.02225 0.06510 = 0.04182 -0.01899 -0.01212 0.00228 AFIX 13 H56 2 0.590966 0.794067 0.139463 11.00000 -1.20000 AFIX 0 C57 1 0.427471 0.800255 0.179163 11.00000 0.02630 0.07732 = 0.06249 -0.02195 -0.00290 -0.00815 AFIX 137 H57A 2 0.361102 0.825047 0.167234 11.00000 -1.50000 H57B 2 0.437867 0.819651 0.214657 11.00000 -1.50000 H57C 2 0.420013 0.740444 0.188965 11.00000 -1.50000 AFIX 0 C58 1 0.509710 0.796615 0.070653 11.00000 0.05009 0.07519 = 0.05710 -0.02768 -0.02455 0.00006 AFIX 137 H58A 2 0.450234 0.828372 0.055507 11.00000 -1.50000 H58B 2 0.490893 0.738232 0.080973 11.00000 -1.50000 H58C 2 0.577456 0.805405 0.039421 11.00000 -1.50000 AFIX 0 RESI 1 AN F12 5 0.057126 0.285326 0.221753 11.00000 0.01827 0.03212 = 0.02993 0.00082 -0.00374 -0.00051 F13 5 -0.091600 0.349614 0.160524 11.00000 0.01729 0.04513 = 0.04982 -0.00262 -0.01161 0.00086 F14 5 -0.037939 0.473031 0.062449 11.00000 0.03330 0.04666 = 0.04365 0.00053 -0.02305 0.00838 F15 5 0.174656 0.524954 0.023217 11.00000 0.04195 0.03397 = 0.02966 0.00408 -0.01179 -0.00088 F16 5 0.327349 0.456012 0.079602 11.00000 0.02349 0.03528 = 0.03439 0.00185 -0.00433 -0.00677 F22 5 0.142846 0.276004 0.323152 11.00000 0.02759 0.05021 = 0.03018 -0.01209 -0.00055 0.00168 F23 5 0.095516 0.368445 0.405325 11.00000 0.04346 0.08971 = 0.03838 -0.03226 -0.00326 0.01797 F24 5 0.178877 0.522963 0.382435 11.00000 0.06598 0.08312 = 0.06818 -0.05693 -0.03081 0.03505 F25 5 0.306021 0.585095 0.271614 11.00000 0.07088 0.03590 = 0.07893 -0.02886 -0.04018 0.01387 F26 5 0.352622 0.494159 0.187574 11.00000 0.04392 0.02808 = 0.04624 -0.00592 -0.01857 0.00216 F32 5 0.375785 0.286539 0.078447 11.00000 0.02535 0.05207 = 0.03953 -0.02174 -0.00145 -0.00278 F33 5 0.583451 0.290374 0.018604 11.00000 0.03341 0.06007 = 0.04453 -0.01910 0.01006 0.00369 F34 5 0.745620 0.330253 0.068724 11.00000 0.01718 0.05023 = 0.06342 0.00297 0.00609 0.00212 F35 5 0.691710 0.371536 0.179619 11.00000 0.01953 0.05246 = 0.06536 -0.00025 -0.01769 -0.00396 F36 5 0.486686 0.375098 0.237824 11.00000 0.02465 0.04378 = 0.04228 -0.00839 -0.01606 0.00170 F42 5 0.191226 0.195105 0.145656 11.00000 0.03050 0.03445 = 0.03725 -0.01398 -0.01041 0.00142 F43 5 0.203925 0.035115 0.182154 11.00000 0.03510 0.03400 = 0.05368 -0.01997 0.00499 -0.00551 F44 5 0.291181 -0.030539 0.279155 11.00000 0.05697 0.02508 = 0.05287 0.00337 0.01214 0.00324 F45 5 0.368512 0.071798 0.338846 11.00000 0.05459 0.04713 = 0.02890 0.00481 -0.00336 0.01829 F46 5 0.367346 0.232542 0.299849 11.00000 0.03067 0.04057 = 0.02962 -0.00623 -0.01185 0.00688 C11 1 0.201683 0.364293 0.153453 11.00000 0.01980 0.02453 = 0.02525 -0.00787 -0.00605 0.00272 C12 1 0.092000 0.342615 0.171174 11.00000 0.02163 0.02510 = 0.02362 -0.00385 -0.00543 0.00209 C13 1 0.012464 0.375950 0.140531 11.00000 0.01862 0.03157 = 0.03455 -0.00991 -0.00766 0.00171 C14 1 0.039395 0.437945 0.090597 11.00000 0.02743 0.03308 = 0.03212 -0.00720 -0.01581 0.00678 C15 1 0.146394 0.463759 0.071464 11.00000 0.03066 0.02868 = 0.02445 -0.00351 -0.00860 0.00223 C16 1 0.224534 0.426907 0.102513 11.00000 0.02033 0.02768 = 0.02798 -0.00728 -0.00406 -0.00140 C21 1 0.255757 0.378583 0.251200 11.00000 0.02063 0.03603 = 0.03084 -0.01309 -0.01399 0.01109 C22 1 0.187722 0.352174 0.307332 11.00000 0.02288 0.04423 = 0.03444 -0.01543 -0.01145 0.00988 C23 1 0.160910 0.398815 0.351484 11.00000 0.02761 0.06251 = 0.03451 -0.01910 -0.00806 0.01490 C24 1 0.201971 0.477154 0.339542 11.00000 0.04012 0.06232 = 0.05490 -0.04143 -0.02638 0.02859 C25 1 0.266462 0.507990 0.284164 11.00000 0.04001 0.03785 = 0.05711 -0.02342 -0.02818 0.01788 C26 1 0.290632 0.459546 0.241102 11.00000 0.03032 0.03554 = 0.04417 -0.01623 -0.02123 0.01200 C31 1 0.417710 0.333443 0.160614 11.00000 0.01751 0.02524 = 0.03439 -0.00286 -0.00606 0.00132 C32 1 0.450791 0.311062 0.104881 11.00000 0.02118 0.03127 = 0.03510 -0.00508 -0.00242 -0.00005 C33 1 0.558265 0.311270 0.073055 11.00000 0.02618 0.03600 = 0.03774 -0.00520 0.00225 0.00301 C34 1 0.640226 0.332287 0.097826 11.00000 0.01708 0.03084 = 0.04817 0.00436 0.00171 0.00090 C35 1 0.612835 0.352648 0.153137 11.00000 0.01909 0.02851 = 0.05049 0.00382 -0.01265 -0.00276 C36 1 0.503906 0.353674 0.183468 11.00000 0.02389 0.02481 = 0.03676 -0.00214 -0.01099 0.00193 C41 1 0.276528 0.224702 0.221528 11.00000 0.01543 0.02972 = 0.02410 -0.00455 0.00149 0.00190 C42 1 0.236662 0.169110 0.194097 11.00000 0.01786 0.03219 = 0.02935 -0.00816 0.00070 0.00207 C43 1 0.241281 0.084959 0.212659 11.00000 0.02335 0.03062 = 0.03758 -0.01236 0.00811 -0.00201 C44 1 0.285455 0.051299 0.261310 11.00000 0.03228 0.02687 = 0.03756 -0.00127 0.00997 0.00293 C45 1 0.324918 0.102509 0.290841 11.00000 0.03102 0.03431 = 0.02638 0.00543 0.00326 0.01032 C46 1 0.321652 0.186677 0.270017 11.00000 0.02165 0.03688 = 0.02490 -0.00554 -0.00079 0.00288 B1 3 0.287437 0.325769 0.196422 11.00000 0.01659 0.02475 = 0.02643 -0.00605 -0.00585 0.00210 RESI 0 HKLF 4 REM mks_073m in P-1 REM R1 = 0.0584 for 18937 Fo > 4sig(Fo) and 0.0610 for all 20020 data REM 1274 parameters refined using 200 restraints END WGHT 0.0000 10.5655 REM Highest difference peak 1.084, deepest hole -0.641, 1-sigma level 0.067 Q1 1 0.7208 0.8657 0.3895 11.00000 0.05 1.08 Q2 1 0.5663 0.9307 0.4056 11.00000 0.05 0.99 Q3 1 0.9384 0.5556 0.3684 11.00000 0.05 0.55 Q4 1 0.8177 0.8895 0.2832 11.00000 0.05 0.49 Q5 1 0.6024 0.6428 0.1993 11.00000 0.05 0.46 Q6 1 0.7553 0.3624 0.0923 11.00000 0.05 0.43 Q7 1 0.7652 0.8229 0.4229 11.00000 0.05 0.39 Q8 1 0.5617 0.5753 0.3886 11.00000 0.05 0.39 Q9 1 0.7361 0.5321 0.4078 11.00000 0.05 0.37 Q10 1 0.8631 0.7756 0.1126 11.00000 0.05 0.36 Q11 1 0.6658 0.3929 0.2124 11.00000 0.05 0.35 Q12 1 0.2826 0.2715 0.2125 11.00000 0.05 0.35 Q13 1 0.8838 1.0139 0.4069 11.00000 0.05 0.34 Q14 1 0.7724 0.8161 0.3401 11.00000 0.05 0.33 Q15 1 0.4565 0.6939 0.3329 11.00000 0.05 0.33 Q16 1 0.6729 0.7545 0.4398 11.00000 0.05 0.33 Q17 1 0.6895 0.9635 0.4538 11.00000 0.05 0.33 Q18 1 0.7460 1.3058 0.3183 11.00000 0.05 0.32 Q19 1 0.2803 0.2072 0.2513 11.00000 0.05 0.32 Q20 1 0.5555 0.5149 0.3663 11.00000 0.05 0.32 ; _shelx_res_checksum 33219 _shelx_fab_file ; 1 0 0 -10.08 0.00 2 0 0 -24.19 0.00 3 0 0 -2.81 0.00 4 0 0 -8.52 0.00 5 0 0 3.91 0.00 6 0 0 -0.11 0.00 7 0 0 -2.84 0.00 8 0 0 1.37 0.00 9 0 0 0.95 0.00 10 0 0 -4.17 0.00 11 0 0 1.64 0.00 12 0 0 2.65 0.00 13 0 0 0.60 0.00 14 0 0 0.71 0.00 15 0 0 -0.03 0.00 -15 1 0 -0.86 0.00 -14 1 0 -0.50 0.00 -13 1 0 -1.23 0.00 -12 1 0 -1.20 0.00 -11 1 0 2.90 0.00 -10 1 0 1.98 0.00 -9 1 0 -3.60 0.00 -8 1 0 2.78 0.00 -7 1 0 1.00 0.00 -6 1 0 -1.13 0.00 -5 1 0 2.44 0.00 -4 1 0 6.71 0.00 -3 1 0 -3.02 0.00 -2 1 0 12.32 0.00 -1 1 0 -68.83 0.00 0 1 0 -21.83 0.00 1 1 0 68.56 0.00 2 1 0 -1.32 0.00 3 1 0 7.23 0.00 4 1 0 -4.92 0.00 5 1 0 -3.21 0.00 6 1 0 3.23 0.00 7 1 0 1.47 0.00 8 1 0 -2.81 0.00 9 1 0 3.23 0.00 10 1 0 -0.39 0.00 11 1 0 -4.24 0.00 12 1 0 -0.51 0.00 13 1 0 0.45 0.00 14 1 0 0.09 0.00 15 1 0 1.18 0.00 -15 2 0 0.29 0.00 -14 2 0 0.21 0.00 -13 2 0 0.29 0.00 -12 2 0 -1.75 0.00 -11 2 0 -3.04 0.00 -10 2 0 2.57 0.00 -9 2 0 -0.28 0.00 -8 2 0 -3.37 0.00 -7 2 0 1.46 0.00 -6 2 0 -0.54 0.00 -5 2 0 -3.14 0.00 -4 2 0 5.16 0.00 -3 2 0 2.04 0.00 -2 2 0 22.22 0.00 -1 2 0 38.16 0.00 0 2 0 -75.74 0.00 1 2 0 -19.02 0.00 2 2 0 18.27 0.00 3 2 0 -0.90 0.00 4 2 0 10.84 0.00 5 2 0 -5.38 0.00 6 2 0 -2.41 0.00 7 2 0 2.09 0.00 8 2 0 0.80 0.00 9 2 0 -1.62 0.00 10 2 0 5.00 0.00 11 2 0 0.68 0.00 12 2 0 -1.85 0.00 13 2 0 -0.92 0.00 14 2 0 -0.96 0.00 15 2 0 -0.65 0.00 -15 3 0 0.29 0.00 -14 3 0 0.02 0.00 -13 3 0 1.25 0.00 -12 3 0 2.01 0.00 -11 3 0 -0.46 0.00 -10 3 0 -2.40 0.00 -9 3 0 3.84 0.00 -8 3 0 -1.10 0.00 -7 3 0 -1.51 0.00 -6 3 0 0.84 0.00 -5 3 0 -2.70 0.00 -4 3 0 -7.54 0.00 -3 3 0 -0.81 0.00 -2 3 0 -22.82 0.00 -1 3 0 42.45 0.00 0 3 0 44.65 0.00 1 3 0 -41.61 0.00 2 3 0 -3.91 0.00 3 3 0 -7.08 0.00 4 3 0 1.78 0.00 5 3 0 6.65 0.00 6 3 0 -2.98 0.00 7 3 0 -3.30 0.00 8 3 0 0.67 0.00 9 3 0 -2.29 0.00 10 3 0 -2.35 0.00 11 3 0 3.86 0.00 12 3 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17 0.13 0.00 11 15 17 -0.35 0.00 -6 16 17 -0.23 0.00 10 16 17 0.39 0.00 -5 17 17 0.08 0.00 9 17 17 -0.15 0.00 6 19 17 -0.07 0.00 1 -14 18 0.33 0.00 2 -14 18 0.57 0.00 3 -14 18 -0.06 0.00 -2 -13 18 0.21 0.00 8 -12 18 0.08 0.00 -5 -11 18 -0.43 0.00 -6 -10 18 0.60 0.00 11 -9 18 -0.03 0.00 -8 -7 18 -0.61 0.00 -9 -5 18 -0.15 0.00 13 -5 18 0.74 0.00 -10 -1 18 0.29 0.00 -10 3 18 0.11 0.00 -10 4 18 0.50 0.00 -10 5 18 0.03 0.00 -10 6 18 -0.39 0.00 -9 8 18 0.02 0.00 14 8 18 -0.28 0.00 -9 9 18 0.22 0.00 -9 10 18 -0.05 0.00 13 11 18 0.11 0.00 -8 12 18 0.06 0.00 12 13 18 0.23 0.00 -7 14 18 -0.69 0.00 -4 17 18 0.00 0.00 7 18 18 -0.22 0.00 0 19 18 -0.26 0.00 5 19 18 0.09 0.00 0 -13 19 0.43 0.00 4 -13 19 0.61 0.00 5 -13 19 -0.12 0.00 7 -12 19 0.03 0.00 -4 -11 19 -0.14 0.00 -5 -10 19 0.03 0.00 -6 -9 19 0.25 0.00 -9 -3 19 -0.20 0.00 14 -1 19 0.68 0.00 -9 6 19 -0.30 0.00 14 6 19 0.33 0.00 -9 7 19 0.41 0.00 14 7 19 -0.37 0.00 -9 8 19 0.09 0.00 13 10 19 -0.14 0.00 -8 11 19 0.22 0.00 -7 13 19 -0.30 0.00 11 14 19 0.04 0.00 8 17 19 0.09 0.00 -2 18 19 0.52 0.00 6 18 19 0.27 0.00 2 19 19 -0.79 0.00 3 19 19 -0.26 0.00 -4 -10 20 -0.13 0.00 -5 -9 20 0.46 0.00 -7 -6 20 -0.05 0.00 -8 -4 20 0.48 0.00 13 -3 20 0.12 0.00 -9 0 20 -0.32 0.00 14 1 20 0.70 0.00 14 2 20 -0.10 0.00 14 3 20 -0.54 0.00 -9 4 20 -0.43 0.00 14 4 20 0.35 0.00 -9 5 20 0.28 0.00 14 5 20 0.30 0.00 -9 6 20 0.34 0.00 -8 9 20 -0.30 0.00 13 9 20 -0.32 0.00 -8 10 20 0.42 0.00 -7 12 20 0.09 0.00 -5 15 20 0.43 0.00 -4 16 20 0.23 0.00 5 18 20 -0.34 0.00 -1 -11 21 -0.67 0.00 6 -11 21 -0.02 0.00 -4 -9 21 0.23 0.00 9 -9 21 -0.24 0.00 10 -8 21 -0.19 0.00 -8 -2 21 0.33 0.00 13 -2 21 0.29 0.00 -8 7 21 -0.62 0.00 -8 8 21 0.01 0.00 13 8 21 -0.28 0.00 -7 11 21 0.04 0.00 12 11 21 -0.02 0.00 -5 14 21 0.11 0.00 10 14 21 -0.43 0.00 -4 15 21 -0.29 0.00 9 15 21 0.84 0.00 -3 16 21 -0.51 0.00 8 16 21 -0.84 0.00 2 18 21 0.49 0.00 3 18 21 0.28 0.00 -1 -10 22 0.43 0.00 6 -10 22 -0.13 0.00 8 -9 22 -0.12 0.00 9 -8 22 0.43 0.00 10 -7 22 0.26 0.00 -6 -5 22 0.52 0.00 12 -3 22 0.01 0.00 -7 -2 22 0.43 0.00 13 0 22 -0.24 0.00 13 1 22 0.59 0.00 -8 3 22 0.74 0.00 -8 4 22 0.33 0.00 13 5 22 0.37 0.00 13 6 22 -0.39 0.00 -7 8 22 0.60 0.00 -7 9 22 0.51 0.00 12 10 22 -0.16 0.00 11 12 22 0.08 0.00 -5 13 22 -0.23 0.00 -4 14 22 -1.03 0.00 -2 16 22 -1.39 0.00 7 16 22 0.21 0.00 0 17 22 0.10 0.00 1 17 22 -0.05 0.00 5 17 22 0.01 0.00 3 -10 23 0.08 0.00 -1 -9 23 0.30 0.00 6 -9 23 0.24 0.00 8 -8 23 0.11 0.00 9 -7 23 0.01 0.00 -5 -5 23 0.03 0.00 11 -4 23 -0.08 0.00 -6 -3 23 0.41 0.00 -7 1 23 -0.57 0.00 -7 5 23 -0.79 0.00 -7 6 23 0.23 0.00 12 8 23 -0.48 0.00 -6 10 23 -0.59 0.00 11 11 23 -0.42 0.00 -4 13 23 -0.79 0.00 -3 14 23 -1.56 0.00 -2 15 23 -1.58 0.00 6 16 23 0.37 0.00 0 -8 24 0.04 0.00 6 -8 24 0.11 0.00 -2 -7 24 0.12 0.00 -3 -6 24 0.20 0.00 10 -4 24 0.03 0.00 -5 -3 24 0.09 0.00 -6 0 24 0.23 0.00 12 1 24 0.48 0.00 12 2 24 0.06 0.00 12 5 24 0.49 0.00 12 6 24 -0.09 0.00 -6 7 24 0.46 0.00 11 9 24 0.02 0.00 -5 10 24 -0.30 0.00 -4 12 24 -0.18 0.00 -3 13 24 -0.83 0.00 9 13 24 -0.27 0.00 -2 14 24 -0.95 0.00 8 14 24 0.99 0.00 2 16 24 0.71 0.00 3 16 24 -0.45 0.00 4 16 24 -0.54 0.00 0 -7 25 0.39 0.00 6 -7 25 -0.22 0.00 -1 -6 25 -0.60 0.00 8 -5 25 -0.28 0.00 9 -4 25 -0.44 0.00 -4 -3 25 -0.33 0.00 10 -3 25 -0.32 0.00 -5 0 25 0.15 0.00 11 0 25 -0.08 0.00 11 7 25 0.54 0.00 -5 8 25 -0.44 0.00 11 8 25 -0.36 0.00 -4 10 25 -0.21 0.00 10 10 25 0.29 0.00 -3 12 25 0.16 0.00 9 12 25 0.04 0.00 -2 13 25 0.10 0.00 8 13 25 0.46 0.00 2 15 25 0.64 0.00 3 15 25 0.04 0.00 4 15 25 -0.85 0.00 1 -6 26 0.10 0.00 4 -6 26 -0.05 0.00 5 -6 26 0.23 0.00 7 -5 26 -0.37 0.00 8 -4 26 -0.20 0.00 -2 -3 26 -0.02 0.00 -3 -2 26 0.31 0.00 -4 0 26 -0.07 0.00 10 0 26 0.13 0.00 -4 7 26 -0.41 0.00 -4 8 26 -0.27 0.00 10 8 26 0.45 0.00 -3 10 26 -0.02 0.00 0 13 26 -0.01 0.00 2 14 26 0.24 0.00 3 14 26 0.16 0.00 4 14 26 -0.58 0.00 3 -5 27 0.19 0.00 6 -4 27 -0.18 0.00 -1 -3 27 0.14 0.00 0 -3 27 0.17 0.00 7 -3 27 -0.34 0.00 8 -2 27 -0.10 0.00 -2 -1 27 0.26 0.00 9 0 27 -0.50 0.00 -3 1 27 0.69 0.00 -3 2 27 0.20 0.00 -3 6 27 -0.17 0.00 -3 7 27 -0.57 0.00 9 8 27 0.15 0.00 -2 9 27 0.05 0.00 8 10 27 0.21 0.00 -1 11 27 0.07 0.00 7 11 27 -0.43 0.00 6 12 27 0.11 0.00 3 13 27 0.04 0.00 3 -3 28 0.32 0.00 4 -3 28 0.73 0.00 1 -2 28 0.40 0.00 6 -2 28 -0.31 0.00 0 -1 28 -0.24 0.00 7 -1 28 -0.38 0.00 -1 0 28 -0.37 0.00 8 1 28 -0.20 0.00 -2 3 28 -0.91 0.00 -2 4 28 0.28 0.00 -2 5 28 0.66 0.00 8 6 28 0.39 0.00 8 7 28 -0.00 0.00 -1 8 28 -0.62 0.00 8 8 28 -0.29 0.00 0 9 28 -0.53 0.00 7 9 28 -0.16 0.00 0 10 28 0.45 0.00 2 11 28 0.06 0.00 3 11 28 -0.33 0.00 4 11 28 0.02 0.00 5 11 28 0.06 0.00 2 0 29 -0.29 0.00 4 0 29 0.07 0.00 5 0 29 0.65 0.00 1 1 29 0.33 0.00 6 1 29 0.28 0.00 1 2 29 -0.43 0.00 0 3 29 0.05 0.00 1 3 29 -0.04 0.00 6 3 29 -0.69 0.00 7 3 29 0.33 0.00 0 4 29 -0.18 0.00 7 4 29 -0.24 0.00 0 5 29 0.11 0.00 7 5 29 0.01 0.00 0 6 29 0.50 0.00 6 6 29 -0.04 0.00 7 6 29 0.08 0.00 1 8 29 -0.51 0.00 2 8 29 -0.15 0.00 6 8 29 0.08 0.00 2 9 29 -0.29 0.00 3 9 29 -0.22 0.00 4 9 29 -0.21 0.00 5 9 29 -0.14 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 110918) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.279 0.721 0.619 144 47 ' ' 2 0.450 0.512 0.967 7 0 ' ' 3 0.721 0.279 0.382 144 47 ' ' 4 0.551 0.488 0.034 7 0 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 0 1 1.995 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL mks_073m P -1 R = 0.10 CELL 12.5203 16.6728 23.1865 78.06 77.17 87.31 SPGR P-1 # Solvent Accessible Volume = 304 # Electrons Found in S.A.V. = 94 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.753 0.318 0.311 ! 5.82 eA-3 C102 0.657 0.263 0.428 ! 5.62 eA-3 C103 0.833 0.301 0.348 ! 5.13 eA-3 C104 0.627 0.281 0.374 ! 3.94 eA-3 C105 0.554 0.295 0.348 ! 3.76 eA-3 C106 0.656 0.298 0.326 ! 3.75 eA-3 C107 0.780 0.281 0.413 ! 3.54 eA-3 C108 0.840 0.284 0.397 ! 3.42 eA-3 C109 0.750 0.263 0.438 ! 3.34 eA-3 C110 0.916 0.330 0.341 ! 2.99 eA-3 C111 0.856 0.267 0.434 ! 1.82 eA-3 Q112 0.721 0.858 0.397 ! 1.11 eA-3 Q113 0.562 0.935 0.402 ! 1.06 eA-3 Q114 0.749 0.361 0.095 ! 0.62 eA-3 Q115 0.940 0.561 0.371 ! 0.61 eA-3 Q116 0.523 0.250 0.416 ! 0.60 eA-3 Q117 0.750 0.220 0.491 ! 0.57 eA-3 Q118 0.598 0.640 0.202 ! 0.56 eA-3 ) ; _shelx_fab_checksum 17036 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_049m _database_code_depnum_ccdc_archive 'CCDC 2184012' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H101 Br2 Ga2 N6 P2' _chemical_formula_weight 1363.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.7131(10) _cell_length_b 25.5509(18) _cell_length_c 18.5397(13) _cell_angle_alpha 90 _cell_angle_beta 99.6843(16) _cell_angle_gamma 90 _cell_volume 6870.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9687 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 32.95 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_F_000 2852 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.477 _exptl_crystal_size_mid 0.204 _exptl_crystal_size_min 0.122 _exptl_absorpt_coefficient_mu 2.037 _shelx_estimated_absorpt_T_min 0.443 _shelx_estimated_absorpt_T_max 0.789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_measurement_device_type 'Bruker D8 KAPPA II (APEX II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/QUEEN' _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 228807 _diffrn_reflns_av_unetI/netI 0.0301 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.934 _diffrn_reflns_theta_max 33.212 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 26297 _reflns_number_gt 20984 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'BRUKER APEX3(v2019.1-0)' _computing_cell_refinement 'BRUKER APEX3(v2019.1-0)' _computing_data_reduction 'BRUKER APEX3(v2019.1-0)' _computing_structure_solution 'BRUKER APEX3(v2019.1-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. Disorder: An isopropyl group is disordered over two positions. All its corresponding bond lengths and angles were restrained to be equal (SADI). RIGU and SIMU restraints were applied to its atoms' anisotropic displacement parameters. The solvent molecule is disordered over a centre of inversion. It bond lengths and angles were restrained to be equal (SADI) and RIGU restraints were used for the displacement parameters. Due to their close proximity C3\_1 and C3\_2 were refined with common displacement parameters (EADP). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+3.6477P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 26297 _refine_ls_number_parameters 799 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.35688(2) 0.55802(2) 0.82758(2) 0.01497(3) Uani 1 1 d . . . . . Br2 Br -0.03943(2) 0.56435(2) 0.94074(2) 0.01261(3) Uani 1 1 d . . . . . Ga1 Ga 0.23876(2) 0.60964(2) 0.75585(2) 0.00983(3) Uani 1 1 d . . . . . Ga2 Ga -0.10245(2) 0.61522(2) 0.83472(2) 0.00837(3) Uani 1 1 d . . . . . P1 P 0.10943(2) 0.59584(2) 0.80978(2) 0.00981(6) Uani 1 1 d . . . . . P2 P -0.01556(2) 0.62682(2) 0.74598(2) 0.01274(6) Uani 1 1 d . . . . . N1 N 0.28986(8) 0.68019(4) 0.76778(6) 0.0122(2) Uani 1 1 d . . . . . N2 N 0.26806(8) 0.59746(4) 0.65720(6) 0.0124(2) Uani 1 1 d . . . . . N3 N -0.22344(8) 0.57838(4) 0.80698(6) 0.01036(19) Uani 1 1 d . . . . . N4 N -0.15792(8) 0.67500(4) 0.87906(6) 0.0108(2) Uani 1 1 d . . . . . N5 N 0.07311(9) 0.48997(4) 0.75074(6) 0.0148(2) Uani 1 1 d . . . . . N6 N 0.14559(8) 0.49259(4) 0.86198(6) 0.0130(2) Uani 1 1 d . . . . . C1 C 0.36180(10) 0.69188(5) 0.73539(8) 0.0151(2) Uani 1 1 d . . . . . C2 C 0.38921(10) 0.66215(6) 0.67952(8) 0.0167(3) Uani 1 1 d . . . . . H2 H 0.447765 0.670593 0.667528 0.020 Uiso 1 1 calc R U . . . C3 C 0.34149(10) 0.62161(6) 0.63906(8) 0.0151(2) Uani 1 1 d . . . . . C4 C 0.41652(12) 0.74111(6) 0.75717(9) 0.0237(3) Uani 1 1 d . . . . . H4A H 0.451969 0.736872 0.806528 0.036 Uiso 1 1 calc R U . . . H4B H 0.374275 0.770824 0.756565 0.036 Uiso 1 1 calc R U . . . H4C H 0.458799 0.747567 0.722556 0.036 Uiso 1 1 calc R U . . . C5 C 0.37712(11) 0.60595(7) 0.57012(9) 0.0234(3) Uani 1 1 d . . . . . H5A H 0.418642 0.575898 0.580543 0.035 Uiso 1 1 calc R U . . . H5B H 0.410674 0.635365 0.553113 0.035 Uiso 1 1 calc R U . . . H5C H 0.325097 0.596446 0.532084 0.035 Uiso 1 1 calc R U . . . C6 C 0.26047(10) 0.71952(5) 0.81544(8) 0.0135(2) Uani 1 1 d . . . . . C7 C 0.30668(10) 0.72496(5) 0.88750(8) 0.0160(3) Uani 1 1 d . . . . . C8 C 0.28319(12) 0.76742(6) 0.92832(9) 0.0217(3) Uani 1 1 d . . . . . H8 H 0.314348 0.772258 0.977051 0.026 Uiso 1 1 calc R U . . . C9 C 0.21537(13) 0.80246(6) 0.89890(9) 0.0247(3) Uani 1 1 d . . . . . H9 H 0.201687 0.831725 0.926803 0.030 Uiso 1 1 calc R U . . . C10 C 0.16742(12) 0.79489(6) 0.82882(9) 0.0219(3) Uani 1 1 d . . . . . H10 H 0.119333 0.818417 0.809759 0.026 Uiso 1 1 calc R U . . . C11 C 0.18844(11) 0.75333(5) 0.78562(8) 0.0162(3) Uani 1 1 d . . . . . C12 C 0.37718(10) 0.68545(6) 0.92316(8) 0.0170(3) Uani 1 1 d . . . . . H12 H 0.395157 0.663018 0.883653 0.020 Uiso 1 1 calc R U . . . C13 C 0.46496(12) 0.71083(7) 0.96491(10) 0.0267(3) Uani 1 1 d . . . . . H13A H 0.510623 0.683612 0.981546 0.040 Uiso 1 1 calc R U . . . H13B H 0.450167 0.729898 1.007316 0.040 Uiso 1 1 calc R U . . . H13C H 0.490194 0.735202 0.932552 0.040 Uiso 1 1 calc R U . . . C14 C 0.33230(11) 0.65009(6) 0.97415(9) 0.0211(3) Uani 1 1 d . . . . . H14A H 0.316574 0.670961 1.014662 0.032 Uiso 1 1 calc R U . . . H14B H 0.375504 0.622336 0.993633 0.032 Uiso 1 1 calc R U . . . H14C H 0.276150 0.634411 0.946707 0.032 Uiso 1 1 calc R U . . . C15 C 0.13592(11) 0.74565(6) 0.70843(8) 0.0201(3) Uani 1 1 d . . . . . H15 H 0.130788 0.707076 0.699547 0.024 Uiso 1 1 calc R U . . . C16 C 0.18647(14) 0.76861(8) 0.65023(10) 0.0347(4) Uani 1 1 d . . . . . H16A H 0.243349 0.748856 0.649309 0.052 Uiso 1 1 calc R U . . . H16B H 0.201638 0.805341 0.661806 0.052 Uiso 1 1 calc R U . . . H16C H 0.146852 0.766381 0.602232 0.052 Uiso 1 1 calc R U . . . C17 C 0.03818(12) 0.76725(7) 0.69885(9) 0.0245(3) Uani 1 1 d . . . . . H17A H 0.040424 0.805526 0.702134 0.037 Uiso 1 1 calc R U . . . H17B H 0.006881 0.753280 0.737379 0.037 Uiso 1 1 calc R U . . . H17C H 0.004341 0.756861 0.650885 0.037 Uiso 1 1 calc R U . . . C18 C 0.21864(10) 0.56047(5) 0.60604(7) 0.0138(2) Uani 1 1 d . . . . . C19 C 0.24667(10) 0.50786(6) 0.60623(8) 0.0163(3) Uani 1 1 d . . . . . C20 C 0.19658(11) 0.47382(6) 0.55534(8) 0.0195(3) Uani 1 1 d . . . . . H20 H 0.212840 0.437820 0.556083 0.023 Uiso 1 1 calc R U . . . C21 C 0.12394(11) 0.49147(6) 0.50402(8) 0.0194(3) Uani 1 1 d . . . . . H21 H 0.091724 0.467938 0.469077 0.023 Uiso 1 1 calc R U . . . C22 C 0.09838(11) 0.54349(6) 0.50375(8) 0.0189(3) Uani 1 1 d . . . . . H22 H 0.048816 0.555528 0.468031 0.023 Uiso 1 1 calc R U . . . C23 C 0.14396(10) 0.57866(6) 0.55491(8) 0.0164(3) Uani 1 1 d D . . . . C24 C 0.33011(11) 0.48631(6) 0.65699(9) 0.0225(3) Uani 1 1 d . . . . . H24 H 0.360999 0.516002 0.686632 0.027 Uiso 1 1 calc R U . . . C25 C 0.40023(13) 0.46191(8) 0.61377(12) 0.0365(5) Uani 1 1 d . . . . . H25A H 0.456657 0.452808 0.647531 0.055 Uiso 1 1 calc R U . . . H25B H 0.414857 0.487137 0.577581 0.055 Uiso 1 1 calc R U . . . H25C H 0.373774 0.430268 0.588695 0.055 Uiso 1 1 calc R U . . . C26 C 0.30188(15) 0.44597(7) 0.70938(10) 0.0329(4) Uani 1 1 d . . . . . H26A H 0.259820 0.462140 0.738628 0.049 Uiso 1 1 calc R U . . . H26B H 0.356840 0.433148 0.741880 0.049 Uiso 1 1 calc R U . . . H26C H 0.270779 0.416641 0.681392 0.049 Uiso 1 1 calc R U . . . C27 C 0.1074(12) 0.6348(5) 0.5601(11) 0.024(3) Uani 0.32(3) 1 d D U P A 1 H27 H 0.129852 0.648012 0.610716 0.029 Uiso 0.32(3) 1 calc R U P A 1 C28 C 0.1490(9) 0.6691(9) 0.5066(19) 0.064(6) Uani 0.32(3) 1 d D U P A 1 H28A H 0.216145 0.670000 0.520999 0.097 Uiso 0.32(3) 1 calc R U P A 1 H28B H 0.124209 0.704621 0.507353 0.097 Uiso 0.32(3) 1 calc R U P A 1 H28C H 0.133166 0.654557 0.457156 0.097 Uiso 0.32(3) 1 calc R U P A 1 C29 C 0.0028(12) 0.6397(11) 0.5448(15) 0.018(2) Uani 0.32(3) 1 d D U P A 1 H29A H -0.014698 0.676064 0.552438 0.027 Uiso 0.32(3) 1 calc R U P A 1 H29B H -0.024012 0.616754 0.577964 0.027 Uiso 0.32(3) 1 calc R U P A 1 H29C H -0.020323 0.629572 0.494014 0.027 Uiso 0.32(3) 1 calc R U P A 1 C27' C 0.1179(6) 0.6363(2) 0.5468(5) 0.0198(10) Uani 0.68(3) 1 d D U P A 2 H27' H 0.153131 0.655492 0.589563 0.024 Uiso 0.68(3) 1 calc R U P A 2 C28' C 0.1434(5) 0.6600(2) 0.4772(4) 0.0365(12) Uani 0.68(3) 1 d D U P A 2 H28D H 0.112002 0.640727 0.434493 0.055 Uiso 0.68(3) 1 calc R U P A 2 H28E H 0.210248 0.657744 0.479137 0.055 Uiso 0.68(3) 1 calc R U P A 2 H28F H 0.124297 0.696802 0.473365 0.055 Uiso 0.68(3) 1 calc R U P A 2 C29' C 0.0157(6) 0.6440(5) 0.5480(7) 0.0235(16) Uani 0.68(3) 1 d D U P A 2 H29D H -0.020398 0.627101 0.505104 0.035 Uiso 0.68(3) 1 calc R U P A 2 H29E H 0.001653 0.681527 0.547126 0.035 Uiso 0.68(3) 1 calc R U P A 2 H29F H 0.000092 0.628409 0.592638 0.035 Uiso 0.68(3) 1 calc R U P A 2 C30 C -0.29210(10) 0.58594(5) 0.84382(8) 0.0134(2) Uani 1 1 d . . . . . C31 C -0.29022(10) 0.62456(5) 0.89835(8) 0.0156(3) Uani 1 1 d . . . . . H31 H -0.334067 0.620689 0.930188 0.019 Uiso 1 1 calc R U . . . C32 C -0.23202(10) 0.66763(5) 0.91122(7) 0.0135(2) Uani 1 1 d . . . . . C33 C -0.37912(11) 0.55374(6) 0.82843(9) 0.0215(3) Uani 1 1 d . . . . . H33A H -0.432077 0.575613 0.834349 0.032 Uiso 1 1 calc R U . . . H33B H -0.374612 0.524300 0.862735 0.032 Uiso 1 1 calc R U . . . H33C H -0.387202 0.540374 0.778210 0.032 Uiso 1 1 calc R U . . . C34 C -0.25713(11) 0.70884(6) 0.96286(9) 0.0211(3) Uani 1 1 d . . . . . H34A H -0.205917 0.713407 1.003597 0.032 Uiso 1 1 calc R U . . . H34B H -0.312340 0.697787 0.981878 0.032 Uiso 1 1 calc R U . . . H34C H -0.269420 0.742054 0.936601 0.032 Uiso 1 1 calc R U . . . C35 C -0.23416(9) 0.53967(5) 0.74948(7) 0.0116(2) Uani 1 1 d . . . . . C36 C -0.22371(10) 0.48589(5) 0.76674(8) 0.0142(2) Uani 1 1 d . . . . . C37 C -0.23545(12) 0.45019(6) 0.70878(9) 0.0210(3) Uani 1 1 d . . . . . H37 H -0.227797 0.413883 0.719078 0.025 Uiso 1 1 calc R U . . . C38 C -0.25788(13) 0.46638(6) 0.63699(9) 0.0247(3) Uani 1 1 d . . . . . H38 H -0.266228 0.441357 0.598550 0.030 Uiso 1 1 calc R U . . . C39 C -0.26820(11) 0.51933(6) 0.62114(8) 0.0207(3) Uani 1 1 d . . . . . H39 H -0.284110 0.530254 0.571642 0.025 Uiso 1 1 calc R U . . . C40 C -0.25560(10) 0.55678(5) 0.67663(7) 0.0142(2) Uani 1 1 d . . . . . C41 C -0.20036(11) 0.46532(5) 0.84440(8) 0.0171(3) Uani 1 1 d . . . . . H41 H -0.199954 0.495569 0.878676 0.021 Uiso 1 1 calc R U . . . C42 C -0.27163(14) 0.42531(7) 0.86189(10) 0.0293(4) Uani 1 1 d . . . . . H42A H -0.260199 0.417645 0.914437 0.044 Uiso 1 1 calc R U . . . H42B H -0.266310 0.393004 0.834406 0.044 Uiso 1 1 calc R U . . . H42C H -0.333801 0.439765 0.847986 0.044 Uiso 1 1 calc R U . . . C43 C -0.10435(13) 0.44049(6) 0.85770(10) 0.0266(3) Uani 1 1 d . . . . . H43A H -0.087750 0.430829 0.909393 0.040 Uiso 1 1 calc R U . . . H43B H -0.059281 0.465619 0.844958 0.040 Uiso 1 1 calc R U . . . H43C H -0.104523 0.409123 0.827254 0.040 Uiso 1 1 calc R U . . . C44 C -0.26809(10) 0.61473(6) 0.65877(8) 0.0159(3) Uani 1 1 d . . . . . H44 H -0.224772 0.634456 0.696517 0.019 Uiso 1 1 calc R U . . . C45 C -0.36611(12) 0.63269(8) 0.66422(12) 0.0327(4) Uani 1 1 d . . . . . H45A H -0.377715 0.627019 0.714159 0.049 Uiso 1 1 calc R U . . . H45B H -0.410651 0.612550 0.629828 0.049 Uiso 1 1 calc R U . . . H45C H -0.372635 0.669997 0.652173 0.049 Uiso 1 1 calc R U . . . C46 C -0.24472(15) 0.62909(7) 0.58423(9) 0.0309(4) Uani 1 1 d . . . . . H46A H -0.183022 0.616040 0.580598 0.046 Uiso 1 1 calc R U . . . H46B H -0.246095 0.667224 0.578538 0.046 Uiso 1 1 calc R U . . . H46C H -0.290032 0.613228 0.545620 0.046 Uiso 1 1 calc R U . . . C47 C -0.11891(10) 0.72701(5) 0.88176(7) 0.0127(2) Uani 1 1 d . . . . . C48 C -0.04689(10) 0.74103(5) 0.93839(8) 0.0150(2) Uani 1 1 d . . . . . C49 C -0.01431(11) 0.79254(6) 0.94019(9) 0.0199(3) Uani 1 1 d . . . . . H49 H 0.034255 0.802769 0.978035 0.024 Uiso 1 1 calc R U . . . C50 C -0.05120(11) 0.82888(6) 0.88815(9) 0.0223(3) Uani 1 1 d . . . . . H50 H -0.028488 0.863755 0.890688 0.027 Uiso 1 1 calc R U . . . C51 C -0.12133(11) 0.81427(6) 0.83235(9) 0.0214(3) Uani 1 1 d . . . . . H51 H -0.145954 0.839226 0.796329 0.026 Uiso 1 1 calc R U . . . C52 C -0.15648(10) 0.76331(5) 0.82818(8) 0.0161(3) Uani 1 1 d . . . . . C53 C -0.00453(11) 0.70233(6) 0.99631(8) 0.0167(3) Uani 1 1 d . . . . . H53 H -0.042746 0.669760 0.990184 0.020 Uiso 1 1 calc R U . . . C54 C -0.00378(13) 0.72290(7) 1.07429(9) 0.0261(3) Uani 1 1 d . . . . . H54A H 0.018392 0.695358 1.109693 0.039 Uiso 1 1 calc R U . . . H54B H -0.066404 0.733131 1.079915 0.039 Uiso 1 1 calc R U . . . H54C H 0.037134 0.753332 1.082998 0.039 Uiso 1 1 calc R U . . . C55 C 0.09328(11) 0.68779(6) 0.98561(9) 0.0236(3) Uani 1 1 d . . . . . H55A H 0.118303 0.661205 1.021639 0.035 Uiso 1 1 calc R U . . . H55B H 0.132519 0.719000 0.992185 0.035 Uiso 1 1 calc R U . . . H55C H 0.091627 0.673860 0.936155 0.035 Uiso 1 1 calc R U . . . C56 C -0.23563(11) 0.74952(6) 0.76690(9) 0.0194(3) Uani 1 1 d . . . . . H56 H -0.251175 0.711802 0.772561 0.023 Uiso 1 1 calc R U . . . C57 C -0.32212(12) 0.78182(8) 0.77258(11) 0.0325(4) Uani 1 1 d . . . . . H57A H -0.309444 0.818966 0.765618 0.049 Uiso 1 1 calc R U . . . H57B H -0.339118 0.776703 0.820984 0.049 Uiso 1 1 calc R U . . . H57C H -0.373009 0.770408 0.734772 0.049 Uiso 1 1 calc R U . . . C58 C -0.20869(13) 0.75624(7) 0.69144(9) 0.0283(4) Uani 1 1 d . . . . . H58A H -0.157938 0.732368 0.686588 0.042 Uiso 1 1 calc R U . . . H58B H -0.189007 0.792421 0.685665 0.042 Uiso 1 1 calc R U . . . H58C H -0.261844 0.748249 0.653618 0.042 Uiso 1 1 calc R U . . . C59 C 0.11064(9) 0.52328(5) 0.80439(7) 0.0111(2) Uani 1 1 d . . . . . C60 C 0.08564(12) 0.43847(5) 0.77441(9) 0.0197(3) Uani 1 1 d . . . . . C61 C 0.13182(11) 0.44015(5) 0.84423(8) 0.0178(3) Uani 1 1 d . . . . . C62 C 0.02582(11) 0.50451(6) 0.67799(8) 0.0195(3) Uani 1 1 d . . . . . H62A H 0.023236 0.542733 0.673800 0.029 Uiso 1 1 calc R U . . . H62B H -0.036975 0.490346 0.670215 0.029 Uiso 1 1 calc R U . . . H62C H 0.059397 0.490218 0.641043 0.029 Uiso 1 1 calc R U . . . C63 C 0.18894(10) 0.51127(6) 0.93410(7) 0.0167(3) Uani 1 1 d . . . . . H63A H 0.167307 0.490243 0.972055 0.025 Uiso 1 1 calc R U . . . H63B H 0.172517 0.548042 0.939747 0.025 Uiso 1 1 calc R U . . . H63C H 0.256057 0.508065 0.938875 0.025 Uiso 1 1 calc R U . . . C64 C 0.05126(16) 0.39335(6) 0.72650(11) 0.0335(4) Uani 1 1 d . . . . . H64A H 0.063912 0.360658 0.754008 0.050 Uiso 1 1 calc R U . . . H64B H 0.082595 0.392786 0.683860 0.050 Uiso 1 1 calc R U . . . H64C H -0.015338 0.396935 0.710143 0.050 Uiso 1 1 calc R U . . . C65 C 0.16390(13) 0.39721(6) 0.89686(9) 0.0252(3) Uani 1 1 d . . . . . H65A H 0.132768 0.400052 0.939455 0.038 Uiso 1 1 calc R U . . . H65B H 0.230693 0.400038 0.912746 0.038 Uiso 1 1 calc R U . . . H65C H 0.149313 0.363312 0.872965 0.038 Uiso 1 1 calc R U . . . C1_1 C 0.4425(4) 0.39713(15) 0.9062(3) 0.0392(12) Uani 0.731(17) 1 d D . P B 3 H1A_1 H 0.414845 0.416426 0.862314 0.059 Uiso 0.731(17) 1 calc R U P B 3 H1B_1 H 0.405597 0.365890 0.911557 0.059 Uiso 0.731(17) 1 calc R U P B 3 H1C_1 H 0.505412 0.386652 0.901748 0.059 Uiso 0.731(17) 1 calc R U P B 3 C2_1 C 0.4453(3) 0.43208(14) 0.9733(3) 0.0233(7) Uani 0.731(17) 1 d D . P B 3 H2A_1 H 0.381590 0.442575 0.977556 0.028 Uiso 0.731(17) 1 calc R U P B 3 H2AB_1 H 0.470724 0.411890 1.017742 0.028 Uiso 0.731(17) 1 calc R U P B 3 C3_1 C 0.5035(7) 0.4811(4) 0.9697(7) 0.0228(9) Uani 0.731(17) 1 d D . P B 3 H3A_1 H 0.568833 0.470725 0.972246 0.027 Uiso 0.731(17) 1 calc R U P B 3 H3AB_1 H 0.483431 0.498705 0.922152 0.027 Uiso 0.731(17) 1 calc R U P B 3 C1_2 C 0.4687(10) 0.4067(6) 0.8809(10) 0.047(3) Uani 0.269(17) 1 d D . P B 4 H1A_2 H 0.421152 0.380132 0.866048 0.071 Uiso 0.269(17) 1 calc R U P B 4 H1B_2 H 0.528824 0.389607 0.894048 0.071 Uiso 0.269(17) 1 calc R U P B 4 H1C_2 H 0.470475 0.431018 0.840321 0.071 Uiso 0.269(17) 1 calc R U P B 4 C2_2 C 0.4463(9) 0.4366(5) 0.9466(11) 0.036(3) Uani 0.269(17) 1 d D . P B 4 H2A_2 H 0.447101 0.412103 0.988044 0.043 Uiso 0.269(17) 1 calc R U P B 4 H2AB_2 H 0.383289 0.451283 0.934345 0.043 Uiso 0.269(17) 1 calc R U P B 4 C3_2 C 0.514(2) 0.4809(11) 0.9701(19) 0.0228(9) Uani 0.269(17) 1 d D . P B 4 H3A_2 H 0.520786 0.501779 0.926338 0.027 Uiso 0.269(17) 1 calc R U P B 4 H3AB_2 H 0.574909 0.465518 0.989494 0.027 Uiso 0.269(17) 1 calc R U P B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01224(6) 0.01630(6) 0.01561(6) -0.00030(5) 0.00017(5) 0.00252(5) Br2 0.01446(6) 0.01335(6) 0.00984(5) 0.00264(4) 0.00151(4) 0.00104(5) Ga1 0.00874(6) 0.01028(6) 0.01080(6) -0.00119(5) 0.00260(5) -0.00105(5) Ga2 0.00873(6) 0.00841(6) 0.00831(6) -0.00005(5) 0.00239(5) 0.00010(5) P1 0.00982(15) 0.00979(13) 0.01018(14) -0.00025(11) 0.00275(11) -0.00027(11) P2 0.01170(15) 0.01626(15) 0.01102(14) 0.00468(12) 0.00410(12) 0.00222(12) N1 0.0129(5) 0.0116(5) 0.0129(5) -0.0016(4) 0.0041(4) -0.0022(4) N2 0.0106(5) 0.0148(5) 0.0122(5) -0.0028(4) 0.0029(4) -0.0019(4) N3 0.0110(5) 0.0108(4) 0.0094(5) -0.0004(4) 0.0020(4) -0.0009(4) N4 0.0108(5) 0.0094(4) 0.0124(5) -0.0017(4) 0.0029(4) -0.0003(4) N5 0.0210(6) 0.0107(5) 0.0129(5) -0.0017(4) 0.0032(4) -0.0009(4) N6 0.0140(5) 0.0120(5) 0.0136(5) 0.0022(4) 0.0038(4) 0.0018(4) C1 0.0135(6) 0.0160(6) 0.0159(6) -0.0013(5) 0.0033(5) -0.0040(5) C2 0.0125(6) 0.0209(6) 0.0175(6) -0.0033(5) 0.0050(5) -0.0045(5) C3 0.0128(6) 0.0200(6) 0.0129(6) -0.0017(5) 0.0036(5) -0.0008(5) C4 0.0249(8) 0.0212(7) 0.0278(8) -0.0075(6) 0.0128(6) -0.0134(6) C5 0.0190(7) 0.0348(8) 0.0188(7) -0.0102(6) 0.0103(6) -0.0084(6) C6 0.0162(6) 0.0096(5) 0.0163(6) -0.0014(4) 0.0070(5) -0.0035(5) C7 0.0174(7) 0.0136(6) 0.0177(6) -0.0027(5) 0.0050(5) -0.0044(5) C8 0.0284(8) 0.0167(6) 0.0206(7) -0.0067(5) 0.0058(6) -0.0050(6) C9 0.0343(9) 0.0146(6) 0.0273(8) -0.0065(6) 0.0108(7) -0.0004(6) C10 0.0275(8) 0.0141(6) 0.0258(8) 0.0009(5) 0.0093(6) 0.0032(6) C11 0.0205(7) 0.0121(6) 0.0179(6) 0.0025(5) 0.0084(5) -0.0008(5) C12 0.0165(7) 0.0171(6) 0.0169(6) -0.0048(5) 0.0013(5) -0.0043(5) C13 0.0216(8) 0.0289(8) 0.0271(8) -0.0064(7) -0.0035(6) -0.0086(6) C14 0.0218(8) 0.0207(7) 0.0203(7) 0.0019(5) 0.0023(6) -0.0009(6) C15 0.0250(8) 0.0201(7) 0.0163(6) 0.0054(5) 0.0069(6) 0.0049(6) C16 0.0332(10) 0.0462(11) 0.0276(9) 0.0173(8) 0.0138(8) 0.0096(8) C17 0.0260(8) 0.0241(7) 0.0236(8) 0.0053(6) 0.0046(6) 0.0054(6) C18 0.0136(6) 0.0166(6) 0.0118(6) -0.0029(5) 0.0034(5) -0.0022(5) C19 0.0165(7) 0.0189(6) 0.0138(6) -0.0044(5) 0.0033(5) 0.0023(5) C20 0.0223(7) 0.0187(6) 0.0177(7) -0.0073(5) 0.0039(6) 0.0016(5) C21 0.0212(7) 0.0222(7) 0.0147(6) -0.0071(5) 0.0031(5) -0.0041(6) C22 0.0188(7) 0.0215(7) 0.0153(6) -0.0010(5) -0.0002(5) -0.0030(5) C23 0.0174(7) 0.0159(6) 0.0155(6) 0.0004(5) 0.0010(5) -0.0030(5) C24 0.0222(8) 0.0212(7) 0.0221(7) -0.0087(6) -0.0020(6) 0.0076(6) C25 0.0246(9) 0.0405(10) 0.0423(11) -0.0185(9) -0.0006(8) 0.0146(8) C26 0.0435(11) 0.0216(8) 0.0299(9) -0.0010(7) -0.0053(8) 0.0065(7) C27 0.025(4) 0.021(4) 0.024(6) 0.014(3) -0.006(3) -0.008(3) C28 0.021(4) 0.060(9) 0.112(15) 0.060(9) 0.010(7) 0.003(5) C29 0.014(3) 0.015(4) 0.024(5) -0.003(3) 0.000(3) 0.000(3) C27' 0.0221(19) 0.0128(15) 0.022(3) 0.0005(13) -0.0031(14) -0.0016(13) C28' 0.037(2) 0.0225(15) 0.055(3) 0.0180(18) 0.023(2) -0.0002(13) C29' 0.033(3) 0.019(3) 0.020(3) 0.005(2) 0.008(3) 0.003(3) C30 0.0125(6) 0.0134(5) 0.0150(6) 0.0001(5) 0.0046(5) -0.0018(5) C31 0.0158(6) 0.0166(6) 0.0165(6) -0.0022(5) 0.0089(5) -0.0015(5) C32 0.0154(6) 0.0137(5) 0.0123(6) -0.0011(4) 0.0050(5) 0.0017(5) C33 0.0159(7) 0.0233(7) 0.0274(8) -0.0060(6) 0.0093(6) -0.0076(6) C34 0.0231(8) 0.0192(7) 0.0241(7) -0.0078(6) 0.0130(6) -0.0003(6) C35 0.0103(6) 0.0138(5) 0.0107(5) -0.0022(4) 0.0020(4) -0.0015(4) C36 0.0161(6) 0.0127(5) 0.0140(6) -0.0011(5) 0.0036(5) -0.0030(5) C37 0.0295(8) 0.0130(6) 0.0208(7) -0.0045(5) 0.0055(6) -0.0040(6) C38 0.0347(9) 0.0219(7) 0.0175(7) -0.0080(6) 0.0041(6) -0.0058(6) C39 0.0268(8) 0.0237(7) 0.0112(6) -0.0033(5) 0.0023(6) -0.0043(6) C40 0.0140(6) 0.0168(6) 0.0116(6) -0.0003(5) 0.0016(5) -0.0021(5) C41 0.0232(7) 0.0120(6) 0.0162(6) 0.0011(5) 0.0037(5) -0.0025(5) C42 0.0434(11) 0.0202(7) 0.0263(8) 0.0032(6) 0.0114(8) -0.0113(7) C43 0.0317(9) 0.0186(7) 0.0269(8) -0.0025(6) -0.0029(7) 0.0067(6) C44 0.0173(7) 0.0179(6) 0.0118(6) 0.0027(5) 0.0007(5) 0.0007(5) C45 0.0205(8) 0.0322(9) 0.0442(11) 0.0111(8) 0.0025(8) 0.0070(7) C46 0.0541(12) 0.0243(8) 0.0155(7) 0.0044(6) 0.0096(7) -0.0009(8) C47 0.0135(6) 0.0095(5) 0.0160(6) -0.0027(4) 0.0050(5) -0.0005(4) C48 0.0146(6) 0.0137(6) 0.0173(6) -0.0039(5) 0.0042(5) 0.0000(5) C49 0.0204(7) 0.0151(6) 0.0239(7) -0.0059(5) 0.0031(6) -0.0036(5) C50 0.0239(8) 0.0113(6) 0.0319(8) -0.0028(6) 0.0053(6) -0.0029(5) C51 0.0228(8) 0.0119(6) 0.0293(8) 0.0030(5) 0.0037(6) 0.0010(5) C52 0.0160(6) 0.0117(5) 0.0206(7) 0.0000(5) 0.0030(5) 0.0008(5) C53 0.0190(7) 0.0151(6) 0.0151(6) -0.0037(5) 0.0004(5) -0.0024(5) C54 0.0339(9) 0.0270(8) 0.0164(7) -0.0063(6) 0.0009(6) -0.0039(7) C55 0.0203(8) 0.0221(7) 0.0276(8) 0.0011(6) 0.0017(6) 0.0014(6) C56 0.0182(7) 0.0149(6) 0.0233(7) 0.0048(5) -0.0021(6) 0.0009(5) C57 0.0199(8) 0.0368(10) 0.0386(10) 0.0000(8) -0.0011(7) 0.0050(7) C58 0.0286(9) 0.0319(9) 0.0229(8) 0.0019(7) 0.0002(7) -0.0032(7) C59 0.0111(6) 0.0116(5) 0.0111(5) 0.0000(4) 0.0033(4) 0.0002(4) C60 0.0282(8) 0.0105(6) 0.0222(7) -0.0019(5) 0.0091(6) -0.0006(5) C61 0.0217(7) 0.0109(5) 0.0225(7) 0.0026(5) 0.0090(6) 0.0033(5) C62 0.0268(8) 0.0186(6) 0.0120(6) -0.0033(5) 0.0005(5) -0.0028(6) C63 0.0162(7) 0.0207(6) 0.0124(6) 0.0042(5) 0.0004(5) 0.0011(5) C64 0.0554(13) 0.0137(7) 0.0324(9) -0.0085(6) 0.0100(9) -0.0059(7) C65 0.0330(9) 0.0165(7) 0.0286(8) 0.0086(6) 0.0122(7) 0.0070(6) C1_1 0.044(2) 0.0340(16) 0.032(2) -0.0048(13) -0.0141(16) -0.0032(14) C2_1 0.0189(12) 0.0196(12) 0.0300(18) 0.0010(12) 0.0004(13) -0.0024(9) C3_1 0.018(3) 0.0226(7) 0.0270(8) 0.0075(6) 0.0004(15) 0.0028(13) C1_2 0.037(6) 0.052(6) 0.049(7) -0.008(5) -0.004(5) -0.007(4) C2_2 0.023(4) 0.037(4) 0.051(7) 0.013(5) 0.012(5) 0.006(3) C3_2 0.018(3) 0.0226(7) 0.0270(8) 0.0075(6) 0.0004(15) 0.0028(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ga1 2.3981(2) . ? Br2 Ga2 2.4083(2) . ? Ga1 N1 1.9513(11) . ? Ga1 N2 1.9732(11) . ? Ga1 P1 2.3205(4) . ? Ga2 N4 1.9751(11) . ? Ga2 N3 2.0028(11) . ? Ga2 P2 2.2664(4) . ? P1 C59 1.8570(13) . ? P1 P2 2.1623(5) . ? N1 C1 1.3356(18) . ? N1 C6 1.4513(17) . ? N2 C3 1.3355(18) . ? N2 C18 1.4454(17) . ? N3 C30 1.3254(17) . ? N3 C35 1.4433(17) . ? N4 C32 1.3408(17) . ? N4 C47 1.4450(17) . ? N5 C59 1.3543(17) . ? N5 C60 1.3894(18) . ? N5 C62 1.4579(19) . ? N6 C59 1.3544(17) . ? N6 C61 1.3865(18) . ? N6 C63 1.4613(18) . ? C1 C2 1.398(2) . ? C1 C4 1.511(2) . ? C2 C3 1.397(2) . ? C3 C5 1.515(2) . ? C6 C7 1.400(2) . ? C6 C11 1.406(2) . ? C7 C8 1.399(2) . ? C7 C12 1.517(2) . ? C8 C9 1.383(2) . ? C9 C10 1.384(2) . ? C10 C11 1.396(2) . ? C11 C15 1.520(2) . ? C12 C13 1.533(2) . ? C12 C14 1.535(2) . ? C15 C17 1.522(2) . ? C15 C16 1.527(2) . ? C18 C23 1.404(2) . ? C18 C19 1.406(2) . ? C19 C20 1.398(2) . ? C19 C24 1.519(2) . ? C20 C21 1.382(2) . ? C21 C22 1.381(2) . ? C22 C23 1.394(2) . ? C23 C27' 1.523(5) . ? C23 C27 1.539(13) . ? C24 C26 1.521(3) . ? C24 C25 1.540(2) . ? C27 C29 1.524(12) . ? C27 C28 1.526(11) . ? C27' C29' 1.519(6) . ? C27' C28' 1.528(6) . ? C30 C31 1.4098(19) . ? C30 C33 1.508(2) . ? C31 C32 1.390(2) . ? C32 C34 1.5101(19) . ? C35 C40 1.4041(19) . ? C35 C36 1.4134(19) . ? C36 C37 1.3978(19) . ? C36 C41 1.517(2) . ? C37 C38 1.380(2) . ? C38 C39 1.387(2) . ? C39 C40 1.394(2) . ? C40 C44 1.522(2) . ? C41 C43 1.530(2) . ? C41 C42 1.538(2) . ? C44 C46 1.524(2) . ? C44 C45 1.533(2) . ? C47 C52 1.403(2) . ? C47 C48 1.407(2) . ? C48 C49 1.399(2) . ? C48 C53 1.515(2) . ? C49 C50 1.383(2) . ? C50 C51 1.384(2) . ? C51 C52 1.398(2) . ? C52 C56 1.525(2) . ? C53 C55 1.531(2) . ? C53 C54 1.537(2) . ? C56 C58 1.526(2) . ? C56 C57 1.535(2) . ? C60 C61 1.358(2) . ? C60 C64 1.491(2) . ? C61 C65 1.491(2) . ? C1_1 C2_1 1.526(4) . ? C2_1 C3_1 1.526(7) . ? C3_1 C3_1 1.498(16) 3_667 ? C1_2 C2_2 1.521(11) . ? C2_2 C3_2 1.522(13) . ? C3_2 C3_2 1.58(5) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ga1 N2 96.36(5) . . ? N1 Ga1 P1 114.82(3) . . ? N2 Ga1 P1 134.28(4) . . ? N1 Ga1 Br1 102.46(4) . . ? N2 Ga1 Br1 100.16(4) . . ? P1 Ga1 Br1 104.349(11) . . ? N4 Ga2 N3 93.36(5) . . ? N4 Ga2 P2 121.61(3) . . ? N3 Ga2 P2 117.42(3) . . ? N4 Ga2 Br2 101.94(3) . . ? N3 Ga2 Br2 99.17(3) . . ? P2 Ga2 Br2 118.447(12) . . ? C59 P1 P2 110.55(5) . . ? C59 P1 Ga1 96.46(4) . . ? P2 P1 Ga1 113.099(18) . . ? P1 P2 Ga2 94.977(17) . . ? C1 N1 C6 117.31(11) . . ? C1 N1 Ga1 118.36(9) . . ? C6 N1 Ga1 124.06(9) . . ? C3 N2 C18 118.42(11) . . ? C3 N2 Ga1 118.20(9) . . ? C18 N2 Ga1 123.17(9) . . ? C30 N3 C35 118.84(11) . . ? C30 N3 Ga2 121.39(9) . . ? C35 N3 Ga2 119.59(8) . . ? C32 N4 C47 117.50(11) . . ? C32 N4 Ga2 120.02(9) . . ? C47 N4 Ga2 122.41(9) . . ? C59 N5 C60 110.30(12) . . ? C59 N5 C62 126.27(12) . . ? C60 N5 C62 123.43(12) . . ? C59 N6 C61 110.57(12) . . ? C59 N6 C63 125.56(12) . . ? C61 N6 C63 123.83(12) . . ? N1 C1 C2 124.13(13) . . ? N1 C1 C4 119.52(13) . . ? C2 C1 C4 116.31(13) . . ? C3 C2 C1 128.27(13) . . ? N2 C3 C2 124.22(13) . . ? N2 C3 C5 119.99(13) . . ? C2 C3 C5 115.79(13) . . ? C7 C6 C11 121.80(13) . . ? C7 C6 N1 120.20(13) . . ? C11 C6 N1 117.90(12) . . ? C8 C7 C6 117.93(14) . . ? C8 C7 C12 119.57(13) . . ? C6 C7 C12 122.44(12) . . ? C9 C8 C7 121.09(15) . . ? C8 C9 C10 120.01(14) . . ? C9 C10 C11 121.18(15) . . ? C10 C11 C6 117.83(14) . . ? C10 C11 C15 120.77(14) . . ? C6 C11 C15 121.39(13) . . ? C7 C12 C13 113.24(13) . . ? C7 C12 C14 109.06(12) . . ? C13 C12 C14 110.55(13) . . ? C11 C15 C17 112.55(13) . . ? C11 C15 C16 112.62(15) . . ? C17 C15 C16 109.94(13) . . ? C23 C18 C19 120.94(13) . . ? C23 C18 N2 118.47(12) . . ? C19 C18 N2 120.56(13) . . ? C20 C19 C18 118.16(14) . . ? C20 C19 C24 118.15(13) . . ? C18 C19 C24 123.66(13) . . ? C21 C20 C19 121.36(14) . . ? C22 C21 C20 119.68(14) . . ? C21 C22 C23 121.24(14) . . ? C22 C23 C18 118.57(13) . . ? C22 C23 C27' 118.2(4) . . ? C18 C23 C27' 122.8(4) . . ? C22 C23 C27 120.6(8) . . ? C18 C23 C27 120.5(8) . . ? C19 C24 C26 111.23(15) . . ? C19 C24 C25 111.51(14) . . ? C26 C24 C25 109.67(15) . . ? C29 C27 C28 109.5(11) . . ? C29 C27 C23 114.7(16) . . ? C28 C27 C23 108.2(10) . . ? C29' C27' C23 110.9(7) . . ? C29' C27' C28' 110.2(5) . . ? C23 C27' C28' 111.9(5) . . ? N3 C30 C31 123.14(13) . . ? N3 C30 C33 121.30(12) . . ? C31 C30 C33 115.55(12) . . ? C32 C31 C30 127.91(13) . . ? N4 C32 C31 123.94(12) . . ? N4 C32 C34 119.20(12) . . ? C31 C32 C34 116.83(12) . . ? C40 C35 C36 121.25(12) . . ? C40 C35 N3 118.43(12) . . ? C36 C35 N3 120.32(12) . . ? C37 C36 C35 117.76(13) . . ? C37 C36 C41 118.84(13) . . ? C35 C36 C41 123.40(12) . . ? C38 C37 C36 121.62(14) . . ? C37 C38 C39 119.78(14) . . ? C38 C39 C40 121.11(14) . . ? C39 C40 C35 118.46(13) . . ? C39 C40 C44 120.74(13) . . ? C35 C40 C44 120.77(12) . . ? C36 C41 C43 110.61(13) . . ? C36 C41 C42 112.15(13) . . ? C43 C41 C42 109.53(13) . . ? C40 C44 C46 113.21(13) . . ? C40 C44 C45 110.95(13) . . ? C46 C44 C45 110.24(14) . . ? C52 C47 C48 121.17(12) . . ? C52 C47 N4 118.47(12) . . ? C48 C47 N4 120.33(12) . . ? C49 C48 C47 118.00(13) . . ? C49 C48 C53 119.91(13) . . ? C47 C48 C53 122.09(12) . . ? C50 C49 C48 121.49(14) . . ? C49 C50 C51 119.75(14) . . ? C50 C51 C52 120.99(14) . . ? C51 C52 C47 118.59(14) . . ? C51 C52 C56 119.03(13) . . ? C47 C52 C56 122.36(12) . . ? C48 C53 C55 110.50(13) . . ? C48 C53 C54 112.37(12) . . ? C55 C53 C54 110.29(13) . . ? C52 C56 C58 111.92(13) . . ? C52 C56 C57 111.25(14) . . ? C58 C56 C57 110.39(14) . . ? N5 C59 N6 105.61(11) . . ? N5 C59 P1 131.34(10) . . ? N6 C59 P1 122.78(10) . . ? C61 C60 N5 106.85(12) . . ? C61 C60 C64 131.12(14) . . ? N5 C60 C64 122.03(15) . . ? C60 C61 N6 106.65(12) . . ? C60 C61 C65 130.78(14) . . ? N6 C61 C65 122.56(14) . . ? C3_1 C2_1 C1_1 112.5(4) . . ? C3_1 C3_1 C2_1 112.7(10) 3_667 . ? C1_2 C2_2 C3_2 112.6(12) . . ? C2_2 C3_2 C3_2 115(3) . 3_667 ? _refine_diff_density_max 0.774 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.082 _shelx_res_file ; TITL mks_049m in P2(1)/n mks_049m.res created by SHELXL-2017/1 at 16:17:25 on 09-Mar-2021 CELL 0.71073 14.71310 25.55090 18.53970 90.0000 99.6843 90.0000 ZERR 4.00000 0.00100 0.00180 0.00130 0.0000 0.0016 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H Br Ga N P UNIT 272 404 8 8 24 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.130 SIZE 0.122 0.204 0.477 L.S. 16 ACTA FMAP 2 PLAN 20 SADI c27 c28 c27 c29 c27' c28' c27' c29' SADI c28 c29 c28' c29' SADI c23 c27 c23 c27' RIGU c27 c28 c29 c27' c28' c29' SIMU c27 c28 c29 c27' c28' c29' SADI_SOLV c1 c2 c2 c3 SADI_SOLV c1 c3 RIGU_SOLV EADP c3_1 c3_2 OMIT 1 1 0 WGHT 0.029800 3.647700 FVAR 0.04976 0.31943 0.73136 BR1 3 0.356883 0.558021 0.827580 11.00000 0.01224 0.01630 = 0.01561 -0.00030 0.00017 0.00252 BR2 3 -0.039435 0.564352 0.940742 11.00000 0.01446 0.01335 = 0.00984 0.00264 0.00151 0.00104 GA1 4 0.238764 0.609642 0.755853 11.00000 0.00874 0.01028 = 0.01080 -0.00119 0.00260 -0.00105 GA2 4 -0.102450 0.615224 0.834716 11.00000 0.00873 0.00841 = 0.00831 -0.00005 0.00239 0.00010 P1 6 0.109431 0.595841 0.809775 11.00000 0.00982 0.00979 = 0.01018 -0.00025 0.00275 -0.00027 P2 6 -0.015561 0.626820 0.745977 11.00000 0.01170 0.01626 = 0.01102 0.00468 0.00410 0.00222 N1 5 0.289859 0.680194 0.767776 11.00000 0.01288 0.01162 = 0.01286 -0.00155 0.00406 -0.00221 N2 5 0.268056 0.597458 0.657196 11.00000 0.01061 0.01476 = 0.01223 -0.00276 0.00293 -0.00190 N3 5 -0.223439 0.578383 0.806979 11.00000 0.01095 0.01080 = 0.00942 -0.00040 0.00198 -0.00090 N4 5 -0.157923 0.675004 0.879064 11.00000 0.01084 0.00937 = 0.01238 -0.00170 0.00286 -0.00033 N5 5 0.073109 0.489968 0.750736 11.00000 0.02103 0.01069 = 0.01289 -0.00166 0.00315 -0.00091 N6 5 0.145589 0.492591 0.861985 11.00000 0.01396 0.01201 = 0.01360 0.00216 0.00380 0.00179 C1 1 0.361800 0.691880 0.735393 11.00000 0.01354 0.01597 = 0.01595 -0.00132 0.00328 -0.00402 C2 1 0.389213 0.662154 0.679521 11.00000 0.01247 0.02093 = 0.01746 -0.00333 0.00502 -0.00447 AFIX 43 H2 2 0.447765 0.670593 0.667528 11.00000 -1.20000 AFIX 0 C3 1 0.341490 0.621614 0.639060 11.00000 0.01276 0.02003 = 0.01287 -0.00167 0.00357 -0.00075 C4 1 0.416521 0.741114 0.757175 11.00000 0.02491 0.02123 = 0.02783 -0.00746 0.01278 -0.01339 AFIX 137 H4A 2 0.451969 0.736872 0.806528 11.00000 -1.50000 H4B 2 0.374275 0.770824 0.756565 11.00000 -1.50000 H4C 2 0.458799 0.747567 0.722556 11.00000 -1.50000 AFIX 0 C5 1 0.377120 0.605948 0.570115 11.00000 0.01898 0.03478 = 0.01883 -0.01018 0.01034 -0.00845 AFIX 137 H5A 2 0.418642 0.575898 0.580543 11.00000 -1.50000 H5B 2 0.410674 0.635365 0.553113 11.00000 -1.50000 H5C 2 0.325097 0.596446 0.532084 11.00000 -1.50000 AFIX 0 C6 1 0.260465 0.719521 0.815440 11.00000 0.01617 0.00956 = 0.01634 -0.00142 0.00696 -0.00350 C7 1 0.306685 0.724959 0.887504 11.00000 0.01736 0.01357 = 0.01768 -0.00266 0.00500 -0.00442 C8 1 0.283187 0.767419 0.928316 11.00000 0.02837 0.01667 = 0.02063 -0.00669 0.00580 -0.00502 AFIX 43 H8 2 0.314348 0.772258 0.977051 11.00000 -1.20000 AFIX 0 C9 1 0.215370 0.802456 0.898899 11.00000 0.03432 0.01459 = 0.02727 -0.00651 0.01077 -0.00043 AFIX 43 H9 2 0.201687 0.831725 0.926803 11.00000 -1.20000 AFIX 0 C10 1 0.167419 0.794894 0.828815 11.00000 0.02746 0.01410 = 0.02584 0.00088 0.00934 0.00317 AFIX 43 H10 2 0.119333 0.818417 0.809759 11.00000 -1.20000 AFIX 0 C11 1 0.188435 0.753327 0.785621 11.00000 0.02046 0.01213 = 0.01792 0.00254 0.00839 -0.00080 C12 1 0.377179 0.685449 0.923156 11.00000 0.01646 0.01713 = 0.01689 -0.00479 0.00133 -0.00430 AFIX 13 H12 2 0.395157 0.663018 0.883653 11.00000 -1.20000 AFIX 0 C13 1 0.464962 0.710830 0.964910 11.00000 0.02156 0.02889 = 0.02714 -0.00635 -0.00349 -0.00864 AFIX 137 H13A 2 0.510623 0.683612 0.981546 11.00000 -1.50000 H13B 2 0.450167 0.729898 1.007316 11.00000 -1.50000 H13C 2 0.490194 0.735202 0.932552 11.00000 -1.50000 AFIX 0 C14 1 0.332295 0.650094 0.974148 11.00000 0.02183 0.02074 = 0.02033 0.00185 0.00234 -0.00092 AFIX 137 H14A 2 0.316574 0.670961 1.014662 11.00000 -1.50000 H14B 2 0.375504 0.622336 0.993633 11.00000 -1.50000 H14C 2 0.276150 0.634411 0.946707 11.00000 -1.50000 AFIX 0 C15 1 0.135915 0.745649 0.708432 11.00000 0.02501 0.02014 = 0.01626 0.00538 0.00695 0.00485 AFIX 13 H15 2 0.130788 0.707076 0.699547 11.00000 -1.20000 AFIX 0 C16 1 0.186466 0.768613 0.650233 11.00000 0.03318 0.04622 = 0.02765 0.01728 0.01377 0.00960 AFIX 137 H16A 2 0.243349 0.748856 0.649309 11.00000 -1.50000 H16B 2 0.201638 0.805341 0.661806 11.00000 -1.50000 H16C 2 0.146852 0.766381 0.602232 11.00000 -1.50000 AFIX 0 C17 1 0.038185 0.767254 0.698854 11.00000 0.02603 0.02411 = 0.02355 0.00534 0.00457 0.00538 AFIX 137 H17A 2 0.040424 0.805526 0.702134 11.00000 -1.50000 H17B 2 0.006881 0.753280 0.737379 11.00000 -1.50000 H17C 2 0.004341 0.756861 0.650885 11.00000 -1.50000 AFIX 0 C18 1 0.218636 0.560472 0.606041 11.00000 0.01360 0.01658 = 0.01180 -0.00292 0.00339 -0.00221 C19 1 0.246674 0.507863 0.606225 11.00000 0.01651 0.01889 = 0.01381 -0.00439 0.00333 0.00233 C20 1 0.196584 0.473822 0.555343 11.00000 0.02234 0.01870 = 0.01773 -0.00728 0.00387 0.00159 AFIX 43 H20 2 0.212840 0.437820 0.556083 11.00000 -1.20000 AFIX 0 C21 1 0.123938 0.491471 0.504015 11.00000 0.02121 0.02222 = 0.01471 -0.00708 0.00313 -0.00414 AFIX 43 H21 2 0.091724 0.467938 0.469077 11.00000 -1.20000 AFIX 0 C22 1 0.098384 0.543492 0.503750 11.00000 0.01876 0.02149 = 0.01531 -0.00098 -0.00018 -0.00301 AFIX 43 H22 2 0.048816 0.555528 0.468031 11.00000 -1.20000 AFIX 0 C23 1 0.143959 0.578663 0.554906 11.00000 0.01738 0.01585 = 0.01551 0.00042 0.00105 -0.00300 C24 1 0.330112 0.486312 0.656988 11.00000 0.02224 0.02124 = 0.02209 -0.00871 -0.00197 0.00756 AFIX 13 H24 2 0.360999 0.516002 0.686632 11.00000 -1.20000 AFIX 0 C25 1 0.400228 0.461912 0.613768 11.00000 0.02464 0.04046 = 0.04226 -0.01853 -0.00059 0.01456 AFIX 137 H25A 2 0.456657 0.452808 0.647531 11.00000 -1.50000 H25B 2 0.414857 0.487137 0.577581 11.00000 -1.50000 H25C 2 0.373774 0.430268 0.588695 11.00000 -1.50000 AFIX 0 C26 1 0.301876 0.445972 0.709383 11.00000 0.04345 0.02156 = 0.02986 -0.00100 -0.00531 0.00645 AFIX 137 H26A 2 0.259820 0.462140 0.738628 11.00000 -1.50000 H26B 2 0.356840 0.433148 0.741880 11.00000 -1.50000 H26C 2 0.270779 0.416641 0.681392 11.00000 -1.50000 AFIX 0 PART 1 21 C27 1 0.107430 0.634759 0.560098 21.00000 0.02460 0.02133 = 0.02391 0.01389 -0.00592 -0.00815 AFIX 13 H27 2 0.129852 0.648012 0.610716 21.00000 -1.20000 AFIX 0 C28 1 0.148950 0.669051 0.506620 21.00000 0.02097 0.05970 = 0.11202 0.05959 0.00982 0.00327 AFIX 137 H28A 2 0.216145 0.670000 0.520999 21.00000 -1.50000 H28B 2 0.124209 0.704621 0.507353 21.00000 -1.50000 H28C 2 0.133166 0.654557 0.457156 21.00000 -1.50000 AFIX 0 C29 1 0.002764 0.639730 0.544761 21.00000 0.01384 0.01451 = 0.02427 -0.00304 -0.00017 0.00013 AFIX 137 H29A 2 -0.014698 0.676064 0.552438 21.00000 -1.50000 H29B 2 -0.024012 0.616754 0.577964 21.00000 -1.50000 H29C 2 -0.020323 0.629572 0.494014 21.00000 -1.50000 AFIX 0 PART 2 -21 C27' 1 0.117867 0.636314 0.546780 -21.00000 0.02210 0.01284 = 0.02210 0.00046 -0.00308 -0.00164 AFIX 13 H27' 2 0.153131 0.655492 0.589563 -21.00000 -1.20000 AFIX 0 C28' 1 0.143392 0.660022 0.477206 -21.00000 0.03723 0.02245 = 0.05510 0.01796 0.02263 -0.00020 AFIX 137 H28D 2 0.112002 0.640727 0.434493 -21.00000 -1.50000 H28E 2 0.210248 0.657744 0.479137 -21.00000 -1.50000 H28F 2 0.124297 0.696802 0.473365 -21.00000 -1.50000 AFIX 0 C29' 1 0.015739 0.644022 0.548022 -21.00000 0.03276 0.01899 = 0.02012 0.00525 0.00842 0.00251 AFIX 137 H29D 2 -0.020398 0.627101 0.505104 -21.00000 -1.50000 H29E 2 0.001653 0.681527 0.547126 -21.00000 -1.50000 H29F 2 0.000092 0.628409 0.592638 -21.00000 -1.50000 AFIX 0 PART 0 C30 1 -0.292103 0.585936 0.843822 11.00000 0.01250 0.01337 = 0.01504 0.00013 0.00462 -0.00181 C31 1 -0.290217 0.624565 0.898353 11.00000 0.01577 0.01659 = 0.01651 -0.00215 0.00886 -0.00150 AFIX 43 H31 2 -0.334067 0.620689 0.930188 11.00000 -1.20000 AFIX 0 C32 1 -0.232015 0.667633 0.911219 11.00000 0.01535 0.01373 = 0.01227 -0.00109 0.00504 0.00175 C33 1 -0.379116 0.553737 0.828432 11.00000 0.01588 0.02328 = 0.02742 -0.00602 0.00928 -0.00763 AFIX 137 H33A 2 -0.432077 0.575613 0.834349 11.00000 -1.50000 H33B 2 -0.374612 0.524300 0.862735 11.00000 -1.50000 H33C 2 -0.387202 0.540374 0.778210 11.00000 -1.50000 AFIX 0 C34 1 -0.257127 0.708836 0.962855 11.00000 0.02307 0.01919 = 0.02407 -0.00780 0.01295 -0.00033 AFIX 137 H34A 2 -0.205917 0.713407 1.003597 11.00000 -1.50000 H34B 2 -0.312340 0.697787 0.981878 11.00000 -1.50000 H34C 2 -0.269420 0.742054 0.936601 11.00000 -1.50000 AFIX 0 C35 1 -0.234162 0.539672 0.749476 11.00000 0.01035 0.01383 = 0.01068 -0.00218 0.00198 -0.00155 C36 1 -0.223713 0.485892 0.766736 11.00000 0.01607 0.01273 = 0.01405 -0.00109 0.00359 -0.00303 C37 1 -0.235451 0.450191 0.708782 11.00000 0.02952 0.01305 = 0.02080 -0.00449 0.00546 -0.00396 AFIX 43 H37 2 -0.227797 0.413883 0.719078 11.00000 -1.20000 AFIX 0 C38 1 -0.257879 0.466383 0.636994 11.00000 0.03473 0.02187 = 0.01749 -0.00805 0.00411 -0.00579 AFIX 43 H38 2 -0.266228 0.441357 0.598550 11.00000 -1.20000 AFIX 0 C39 1 -0.268197 0.519330 0.621138 11.00000 0.02684 0.02370 = 0.01116 -0.00332 0.00234 -0.00433 AFIX 43 H39 2 -0.284110 0.530254 0.571642 11.00000 -1.20000 AFIX 0 C40 1 -0.255604 0.556779 0.676626 11.00000 0.01397 0.01681 = 0.01155 -0.00029 0.00163 -0.00206 C41 1 -0.200362 0.465315 0.844405 11.00000 0.02323 0.01203 = 0.01621 0.00105 0.00369 -0.00250 AFIX 13 H41 2 -0.199954 0.495569 0.878676 11.00000 -1.20000 AFIX 0 C42 1 -0.271629 0.425305 0.861894 11.00000 0.04339 0.02021 = 0.02629 0.00321 0.01138 -0.01130 AFIX 137 H42A 2 -0.260199 0.417645 0.914437 11.00000 -1.50000 H42B 2 -0.266310 0.393004 0.834406 11.00000 -1.50000 H42C 2 -0.333801 0.439765 0.847986 11.00000 -1.50000 AFIX 0 C43 1 -0.104348 0.440490 0.857697 11.00000 0.03174 0.01857 = 0.02692 -0.00246 -0.00289 0.00669 AFIX 137 H43A 2 -0.087750 0.430829 0.909393 11.00000 -1.50000 H43B 2 -0.059281 0.465619 0.844958 11.00000 -1.50000 H43C 2 -0.104523 0.409123 0.827254 11.00000 -1.50000 AFIX 0 C44 1 -0.268091 0.614728 0.658769 11.00000 0.01734 0.01794 = 0.01176 0.00271 0.00074 0.00065 AFIX 13 H44 2 -0.224772 0.634456 0.696517 11.00000 -1.20000 AFIX 0 C45 1 -0.366112 0.632694 0.664224 11.00000 0.02052 0.03224 = 0.04424 0.01112 0.00245 0.00697 AFIX 137 H45A 2 -0.377715 0.627019 0.714159 11.00000 -1.50000 H45B 2 -0.410651 0.612550 0.629828 11.00000 -1.50000 H45C 2 -0.372635 0.669997 0.652173 11.00000 -1.50000 AFIX 0 C46 1 -0.244725 0.629086 0.584230 11.00000 0.05407 0.02428 = 0.01553 0.00443 0.00956 -0.00095 AFIX 137 H46A 2 -0.183022 0.616040 0.580598 11.00000 -1.50000 H46B 2 -0.246095 0.667224 0.578538 11.00000 -1.50000 H46C 2 -0.290032 0.613228 0.545620 11.00000 -1.50000 AFIX 0 C47 1 -0.118914 0.727009 0.881760 11.00000 0.01350 0.00948 = 0.01599 -0.00274 0.00498 -0.00051 C48 1 -0.046894 0.741033 0.938386 11.00000 0.01458 0.01369 = 0.01726 -0.00391 0.00418 -0.00002 C49 1 -0.014312 0.792537 0.940193 11.00000 0.02041 0.01515 = 0.02393 -0.00590 0.00310 -0.00363 AFIX 43 H49 2 0.034255 0.802769 0.978035 11.00000 -1.20000 AFIX 0 C50 1 -0.051197 0.828883 0.888150 11.00000 0.02393 0.01126 = 0.03189 -0.00277 0.00529 -0.00295 AFIX 43 H50 2 -0.028488 0.863755 0.890688 11.00000 -1.20000 AFIX 0 C51 1 -0.121327 0.814265 0.832345 11.00000 0.02283 0.01187 = 0.02933 0.00297 0.00371 0.00098 AFIX 43 H51 2 -0.145954 0.839226 0.796329 11.00000 -1.20000 AFIX 0 C52 1 -0.156475 0.763310 0.828182 11.00000 0.01596 0.01169 = 0.02059 -0.00003 0.00296 0.00083 C53 1 -0.004526 0.702326 0.996307 11.00000 0.01901 0.01511 = 0.01505 -0.00372 0.00038 -0.00243 AFIX 13 H53 2 -0.042746 0.669760 0.990184 11.00000 -1.20000 AFIX 0 C54 1 -0.003784 0.722900 1.074291 11.00000 0.03390 0.02695 = 0.01642 -0.00629 0.00087 -0.00389 AFIX 137 H54A 2 0.018392 0.695358 1.109693 11.00000 -1.50000 H54B 2 -0.066404 0.733131 1.079915 11.00000 -1.50000 H54C 2 0.037134 0.753332 1.082998 11.00000 -1.50000 AFIX 0 C55 1 0.093282 0.687790 0.985609 11.00000 0.02027 0.02212 = 0.02758 0.00112 0.00166 0.00141 AFIX 137 H55A 2 0.118303 0.661205 1.021639 11.00000 -1.50000 H55B 2 0.132519 0.719000 0.992185 11.00000 -1.50000 H55C 2 0.091627 0.673860 0.936155 11.00000 -1.50000 AFIX 0 C56 1 -0.235627 0.749516 0.766897 11.00000 0.01817 0.01486 = 0.02335 0.00479 -0.00207 0.00093 AFIX 13 H56 2 -0.251175 0.711802 0.772561 11.00000 -1.20000 AFIX 0 C57 1 -0.322120 0.781819 0.772582 11.00000 0.01993 0.03682 = 0.03860 0.00003 -0.00115 0.00505 AFIX 137 H57A 2 -0.309444 0.818966 0.765618 11.00000 -1.50000 H57B 2 -0.339118 0.776703 0.820984 11.00000 -1.50000 H57C 2 -0.373009 0.770408 0.734772 11.00000 -1.50000 AFIX 0 C58 1 -0.208694 0.756240 0.691438 11.00000 0.02861 0.03191 = 0.02293 0.00191 0.00017 -0.00318 AFIX 137 H58A 2 -0.157938 0.732368 0.686588 11.00000 -1.50000 H58B 2 -0.189007 0.792421 0.685665 11.00000 -1.50000 H58C 2 -0.261844 0.748249 0.653618 11.00000 -1.50000 AFIX 0 C59 1 0.110645 0.523277 0.804394 11.00000 0.01108 0.01162 = 0.01109 -0.00001 0.00334 0.00022 C60 1 0.085637 0.438474 0.774411 11.00000 0.02818 0.01047 = 0.02222 -0.00192 0.00908 -0.00062 C61 1 0.131822 0.440151 0.844229 11.00000 0.02170 0.01087 = 0.02253 0.00258 0.00904 0.00333 C62 1 0.025816 0.504508 0.677987 11.00000 0.02677 0.01864 = 0.01202 -0.00333 0.00046 -0.00282 AFIX 137 H62A 2 0.023236 0.542733 0.673800 11.00000 -1.50000 H62B 2 -0.036975 0.490346 0.670215 11.00000 -1.50000 H62C 2 0.059397 0.490218 0.641043 11.00000 -1.50000 AFIX 0 C63 1 0.188937 0.511274 0.934104 11.00000 0.01619 0.02069 = 0.01242 0.00420 0.00040 0.00106 AFIX 137 H63A 2 0.167307 0.490243 0.972055 11.00000 -1.50000 H63B 2 0.172517 0.548042 0.939747 11.00000 -1.50000 H63C 2 0.256057 0.508065 0.938875 11.00000 -1.50000 AFIX 0 C64 1 0.051255 0.393347 0.726500 11.00000 0.05538 0.01374 = 0.03238 -0.00851 0.00998 -0.00590 AFIX 137 H64A 2 0.063912 0.360658 0.754008 11.00000 -1.50000 H64B 2 0.082595 0.392786 0.683860 11.00000 -1.50000 H64C 2 -0.015338 0.396935 0.710143 11.00000 -1.50000 AFIX 0 C65 1 0.163898 0.397207 0.896860 11.00000 0.03303 0.01653 = 0.02856 0.00859 0.01224 0.00696 AFIX 137 H65A 2 0.132768 0.400052 0.939455 11.00000 -1.50000 H65B 2 0.230693 0.400038 0.912746 11.00000 -1.50000 H65C 2 0.149313 0.363312 0.872965 11.00000 -1.50000 AFIX 0 RESI 1 SOLV PART 3 31 C1 1 0.442534 0.397134 0.906235 31.00000 0.04413 0.03404 = 0.03225 -0.00478 -0.01406 -0.00324 AFIX 137 H1A 2 0.414845 0.416426 0.862314 31.00000 -1.50000 H1B 2 0.405597 0.365890 0.911557 31.00000 -1.50000 H1C 2 0.505412 0.386652 0.901748 31.00000 -1.50000 AFIX 0 C2 1 0.445255 0.432076 0.973347 31.00000 0.01890 0.01958 = 0.02999 0.00100 0.00040 -0.00244 AFIX 23 H2A 2 0.381590 0.442575 0.977556 31.00000 -1.20000 H2AB 2 0.470724 0.411890 1.017742 31.00000 -1.20000 AFIX 0 C3 1 0.503541 0.481092 0.969723 31.00000 0.01758 0.02262 = 0.02697 0.00754 0.00039 0.00275 AFIX 23 H3A 2 0.568833 0.470725 0.972246 31.00000 -1.20000 H3AB 2 0.483431 0.498705 0.922152 31.00000 -1.20000 AFIX 0 PART 0 RESI 0 RESI 2 SOLV PART 4 -31 C1 1 0.468675 0.406687 0.880918 -31.00000 0.03657 0.05242 = 0.04909 -0.00826 -0.00357 -0.00679 AFIX 137 H1A 2 0.421152 0.380132 0.866048 -31.00000 -1.50000 H1B 2 0.528824 0.389607 0.894048 -31.00000 -1.50000 H1C 2 0.470475 0.431018 0.840321 -31.00000 -1.50000 AFIX 0 C2 1 0.446292 0.436638 0.946611 -31.00000 0.02316 0.03682 = 0.05052 0.01272 0.01168 0.00642 AFIX 23 H2A 2 0.447101 0.412103 0.988044 -31.00000 -1.20000 H2AB 2 0.383289 0.451283 0.934345 -31.00000 -1.20000 AFIX 0 C3 1 0.513953 0.480931 0.970118 -31.00000 0.01758 0.02262 = 0.02697 0.00754 0.00039 0.00275 AFIX 23 H3A 2 0.520786 0.501779 0.926338 -31.00000 -1.20000 H3AB 2 0.574909 0.465518 0.989494 -31.00000 -1.20000 PART 0 RESI 0 AFIX 0 HKLF 4 REM mks_049m in P2(1)/n REM R1 = 0.0314 for 20984 Fo > 4sig(Fo) and 0.0501 for all 26297 data REM 799 parameters refined using 117 restraints END WGHT 0.0298 3.6473 REM Highest difference peak 0.774, deepest hole -0.463, 1-sigma level 0.082 Q1 1 0.3570 0.5537 0.8671 11.00000 0.05 0.77 Q2 1 -0.0503 0.5632 0.9766 11.00000 0.05 0.73 Q3 1 0.3959 0.5499 0.8535 11.00000 0.05 0.69 Q4 1 0.2767 0.6026 0.7828 11.00000 0.05 0.68 Q5 1 0.2175 0.7907 0.6725 11.00000 0.05 0.66 Q6 1 0.3709 0.5683 0.7928 11.00000 0.05 0.66 Q7 1 -0.0942 0.6084 0.7994 11.00000 0.05 0.65 Q8 1 0.2924 0.5598 0.8391 11.00000 0.05 0.64 Q9 1 -0.2994 0.6098 0.8668 11.00000 0.05 0.58 Q10 1 -0.0350 0.5588 0.9002 11.00000 0.05 0.58 Q11 1 -0.1479 0.6146 0.8050 11.00000 0.05 0.58 Q12 1 -0.1453 0.7890 0.8323 11.00000 0.05 0.56 Q13 1 0.2316 0.6212 0.7923 11.00000 0.05 0.55 Q14 1 -0.1051 0.6038 0.8673 11.00000 0.05 0.55 Q15 1 0.0815 0.5077 0.7779 11.00000 0.05 0.54 Q16 1 0.2277 0.6003 0.7933 11.00000 0.05 0.54 Q17 1 0.1561 0.4832 0.5306 11.00000 0.05 0.53 Q18 1 0.3509 0.5823 0.8545 11.00000 0.05 0.53 Q19 1 0.0044 0.5699 0.9640 11.00000 0.05 0.51 Q20 1 -0.2506 0.4524 0.6697 11.00000 0.05 0.51 ; _shelx_res_checksum 40826 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_005m _database_code_depnum_ccdc_archive 'CCDC 2184010' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H82 Br2 Ga2 N4 P2' _chemical_formula_weight 1196.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6417(6) _cell_length_b 13.9614(6) _cell_length_c 15.7579(7) _cell_angle_alpha 90 _cell_angle_beta 105.1021(15) _cell_angle_gamma 90 _cell_volume 2897.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9533 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 80.80 _exptl_crystal_description tablet _exptl_crystal_colour 'greenish yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_F_000 1240 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.151 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.096 _exptl_absorpt_coefficient_mu 3.569 _shelx_estimated_absorpt_T_min 0.615 _shelx_estimated_absorpt_T_max 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 Venture (Photon II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/Queen' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 113993 _diffrn_reflns_av_unetI/netI 0.0134 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.824 _diffrn_reflns_theta_max 80.790 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6312 _reflns_number_gt 5955 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX3(v2017.3-0)' _computing_cell_refinement 'Bruker APEX3(v2017.3-0)' _computing_data_reduction 'Bruker APEX3(v2017.3-0)' _computing_structure_solution 'Bruker APEX3(v2017.3-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+1.8037P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6312 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.68060(2) 0.06158(2) 0.23136(2) 0.02288(5) Uani 1 1 d . . . . . Ga1 Ga 0.55060(2) 0.13265(2) 0.11952(2) 0.01396(5) Uani 1 1 d . . . . . P1 P 0.44385(3) 0.03052(3) 0.02210(3) 0.02193(8) Uani 1 1 d . . . . . N1 N 0.62027(8) 0.23179(8) 0.07113(7) 0.0148(2) Uani 1 1 d . . . . . N2 N 0.47787(8) 0.21586(9) 0.18006(7) 0.0158(2) Uani 1 1 d . . . . . C1 C 0.64117(10) 0.31420(10) 0.11476(9) 0.0179(3) Uani 1 1 d . . . . . C2 C 0.60105(11) 0.34056(11) 0.18513(9) 0.0202(3) Uani 1 1 d . . . . . H2 H 0.633404 0.393073 0.219605 0.024 Uiso 1 1 calc R U . . . C3 C 0.51955(10) 0.29949(10) 0.21105(9) 0.0185(3) Uani 1 1 d . . . . . C4 C 0.71150(12) 0.38518(11) 0.08884(11) 0.0253(3) Uani 1 1 d . . . . . H4A H 0.709088 0.376637 0.026596 0.038 Uiso 1 1 calc R U . . . H4B H 0.780996 0.374615 0.124660 0.038 Uiso 1 1 calc R U . . . H4C H 0.690118 0.450423 0.098401 0.038 Uiso 1 1 calc R U . . . C5 C 0.47849(12) 0.35357(12) 0.27728(11) 0.0265(3) Uani 1 1 d . . . . . H5A H 0.474939 0.422004 0.262947 0.040 Uiso 1 1 calc R U . . . H5B H 0.523471 0.343948 0.336230 0.040 Uiso 1 1 calc R U . . . H5C H 0.410408 0.329890 0.275675 0.040 Uiso 1 1 calc R U . . . C6 C 0.65353(10) 0.21252(10) -0.00743(8) 0.0155(2) Uani 1 1 d . . . . . C7 C 0.75006(10) 0.17349(10) -0.00108(9) 0.0178(3) Uani 1 1 d . . . . . C8 C 0.77639(11) 0.15125(12) -0.07869(10) 0.0231(3) Uani 1 1 d . . . . . H8 H 0.841167 0.124199 -0.075427 0.028 Uiso 1 1 calc R U . . . C9 C 0.71040(12) 0.16769(13) -0.16002(10) 0.0271(3) Uani 1 1 d . . . . . H9 H 0.730057 0.152936 -0.212105 0.033 Uiso 1 1 calc R U . . . C10 C 0.61548(12) 0.20579(13) -0.16517(10) 0.0267(3) Uani 1 1 d . . . . . H10 H 0.570390 0.217113 -0.221310 0.032 Uiso 1 1 calc R U . . . C11 C 0.58439(11) 0.22796(11) -0.09008(9) 0.0212(3) Uani 1 1 d . . . . . C12 C 0.82695(11) 0.15346(12) 0.08585(9) 0.0220(3) Uani 1 1 d . . . . . H12 H 0.796955 0.174129 0.134427 0.026 Uiso 1 1 calc R U . . . C13 C 0.92517(11) 0.20968(15) 0.09386(10) 0.0316(4) Uani 1 1 d . . . . . H13A H 0.956503 0.189418 0.047450 0.047 Uiso 1 1 calc R U . . . H13B H 0.972113 0.197344 0.151442 0.047 Uiso 1 1 calc R U . . . H13C H 0.909819 0.278302 0.087811 0.047 Uiso 1 1 calc R U . . . C14 C 0.85102(14) 0.04650(14) 0.09690(12) 0.0337(4) Uani 1 1 d . . . . . H14A H 0.787621 0.010181 0.087543 0.051 Uiso 1 1 calc R U . . . H14B H 0.893492 0.034397 0.156407 0.051 Uiso 1 1 calc R U . . . H14C H 0.887365 0.026387 0.053845 0.051 Uiso 1 1 calc R U . . . C15 C 0.47841(13) 0.26787(15) -0.09941(10) 0.0325(4) Uani 1 1 d . . . . . H15 H 0.458653 0.252797 -0.044061 0.039 Uiso 1 1 calc R U . . . C16 C 0.39883(12) 0.22381(15) -0.17563(11) 0.0352(4) Uani 1 1 d . . . . . H16A H 0.414134 0.240669 -0.231173 0.053 Uiso 1 1 calc R U . . . H16B H 0.331554 0.248422 -0.175617 0.053 Uiso 1 1 calc R U . . . H16C H 0.399598 0.153982 -0.169125 0.053 Uiso 1 1 calc R U . . . C17 C 0.4780(2) 0.37632(18) -0.1093(2) 0.0779(11) Uani 1 1 d . . . . . H17A H 0.501543 0.393351 -0.161018 0.117 Uiso 1 1 calc R U . . . H17B H 0.523250 0.404874 -0.056721 0.117 Uiso 1 1 calc R U . . . H17C H 0.408861 0.400551 -0.116558 0.117 Uiso 1 1 calc R U . . . C18 C 0.38104(10) 0.18382(10) 0.19088(9) 0.0168(3) Uani 1 1 d . . . . . C19 C 0.37662(11) 0.12270(11) 0.26080(10) 0.0206(3) Uani 1 1 d . . . . . C20 C 0.28177(12) 0.08721(12) 0.26389(11) 0.0270(3) Uani 1 1 d . . . . . H20 H 0.277273 0.045744 0.310527 0.032 Uiso 1 1 calc R U . . . C21 C 0.19461(12) 0.11118(14) 0.20062(12) 0.0308(4) Uani 1 1 d . . . . . H21 H 0.130950 0.085882 0.203606 0.037 Uiso 1 1 calc R U . . . C22 C 0.20006(11) 0.17205(14) 0.13289(11) 0.0291(3) Uani 1 1 d . . . . . H22 H 0.139521 0.188903 0.090056 0.035 Uiso 1 1 calc R U . . . C23 C 0.29251(11) 0.20925(11) 0.12608(10) 0.0215(3) Uani 1 1 d . . . . . C24 C 0.46936(11) 0.09460(12) 0.33332(10) 0.0246(3) Uani 1 1 d . . . . . H24 H 0.529778 0.127726 0.322134 0.030 Uiso 1 1 calc R U . . . C25 C 0.45781(14) 0.12753(16) 0.42293(11) 0.0375(4) Uani 1 1 d . . . . . H25A H 0.446721 0.196922 0.421864 0.056 Uiso 1 1 calc R U . . . H25B H 0.519643 0.111822 0.468549 0.056 Uiso 1 1 calc R U . . . H25C H 0.399661 0.094917 0.435725 0.056 Uiso 1 1 calc R U . . . C26 C 0.48822(13) -0.01350(13) 0.33368(13) 0.0336(4) Uani 1 1 d . . . . . H26A H 0.430112 -0.047384 0.345215 0.050 Uiso 1 1 calc R U . . . H26B H 0.549740 -0.029149 0.379673 0.050 Uiso 1 1 calc R U . . . H26C H 0.496892 -0.033160 0.276373 0.050 Uiso 1 1 calc R U . . . C27 C 0.29479(12) 0.27701(14) 0.05097(11) 0.0294(3) Uani 1 1 d . . . . . H27 H 0.365704 0.278146 0.044313 0.035 Uiso 1 1 calc R U . . . C28 C 0.26715(17) 0.37956(15) 0.07267(14) 0.0435(5) Uani 1 1 d . . . . . H28A H 0.268743 0.422256 0.023680 0.065 Uiso 1 1 calc R U . . . H28B H 0.316253 0.401829 0.126100 0.065 Uiso 1 1 calc R U . . . H28C H 0.198888 0.379793 0.082016 0.065 Uiso 1 1 calc R U . . . C29 C 0.22453(15) 0.24487(16) -0.03636(11) 0.0384(4) Uani 1 1 d . . . . . H29A H 0.232918 0.287532 -0.083354 0.058 Uiso 1 1 calc R U . . . H29B H 0.153939 0.247274 -0.032727 0.058 Uiso 1 1 calc R U . . . H29C H 0.241584 0.179165 -0.049103 0.058 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01910(8) 0.02706(9) 0.02174(8) 0.00778(5) 0.00402(6) 0.00430(5) Ga1 0.01327(8) 0.01468(9) 0.01372(8) -0.00212(6) 0.00315(6) -0.00039(6) P1 0.01669(16) 0.02257(18) 0.02601(18) -0.01043(14) 0.00463(14) -0.00346(13) N1 0.0136(5) 0.0171(5) 0.0136(5) -0.0007(4) 0.0030(4) 0.0003(4) N2 0.0143(5) 0.0178(6) 0.0156(5) -0.0028(4) 0.0044(4) -0.0009(4) C1 0.0150(6) 0.0181(6) 0.0201(6) -0.0011(5) 0.0037(5) -0.0016(5) C2 0.0196(6) 0.0193(7) 0.0219(7) -0.0070(5) 0.0058(5) -0.0045(5) C3 0.0180(6) 0.0192(7) 0.0182(6) -0.0047(5) 0.0046(5) -0.0001(5) C4 0.0271(7) 0.0215(7) 0.0304(8) -0.0054(6) 0.0128(6) -0.0081(6) C5 0.0260(7) 0.0273(8) 0.0292(8) -0.0127(6) 0.0128(6) -0.0045(6) C6 0.0162(6) 0.0164(6) 0.0144(6) -0.0001(5) 0.0046(5) -0.0008(5) C7 0.0148(6) 0.0206(7) 0.0177(6) -0.0007(5) 0.0037(5) -0.0016(5) C8 0.0170(6) 0.0322(8) 0.0208(7) -0.0031(6) 0.0060(5) 0.0022(6) C9 0.0237(7) 0.0415(9) 0.0174(7) -0.0047(6) 0.0075(6) 0.0011(7) C10 0.0227(7) 0.0414(9) 0.0147(6) 0.0010(6) 0.0026(5) 0.0041(6) C11 0.0186(6) 0.0271(7) 0.0174(6) 0.0020(5) 0.0038(5) 0.0035(5) C12 0.0149(6) 0.0328(8) 0.0178(6) 0.0016(6) 0.0034(5) 0.0037(6) C13 0.0159(7) 0.0558(11) 0.0219(7) -0.0019(7) 0.0025(6) -0.0043(7) C14 0.0329(9) 0.0376(10) 0.0318(8) 0.0080(7) 0.0105(7) 0.0154(7) C15 0.0243(8) 0.0527(11) 0.0189(7) 0.0020(7) 0.0027(6) 0.0169(7) C16 0.0202(7) 0.0534(12) 0.0303(8) 0.0107(8) 0.0034(6) 0.0057(7) C17 0.0519(14) 0.0458(14) 0.109(2) -0.0283(14) -0.0274(15) 0.0285(11) C18 0.0149(6) 0.0181(6) 0.0182(6) -0.0042(5) 0.0060(5) -0.0007(5) C19 0.0185(6) 0.0233(7) 0.0207(7) -0.0019(5) 0.0065(5) -0.0001(5) C20 0.0238(7) 0.0289(8) 0.0307(8) 0.0028(6) 0.0112(6) -0.0024(6) C21 0.0183(7) 0.0388(9) 0.0372(9) 0.0002(7) 0.0105(6) -0.0055(6) C22 0.0155(7) 0.0417(10) 0.0291(8) 0.0009(7) 0.0038(6) 0.0001(6) C23 0.0167(6) 0.0267(7) 0.0219(7) -0.0003(6) 0.0065(5) 0.0027(5) C24 0.0215(7) 0.0330(8) 0.0198(7) 0.0048(6) 0.0065(6) 0.0013(6) C25 0.0333(9) 0.0592(13) 0.0202(7) 0.0015(7) 0.0071(7) -0.0004(8) C26 0.0276(8) 0.0334(9) 0.0424(9) 0.0139(7) 0.0137(7) 0.0048(7) C27 0.0169(7) 0.0432(10) 0.0283(8) 0.0116(7) 0.0063(6) 0.0076(6) C28 0.0475(11) 0.0350(10) 0.0417(10) 0.0080(8) 0.0003(9) -0.0004(8) C29 0.0399(10) 0.0505(11) 0.0235(8) 0.0042(7) 0.0056(7) 0.0154(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ga1 2.3680(2) . ? Ga1 N2 1.9331(12) . ? Ga1 N1 1.9439(12) . ? Ga1 P1 2.3120(4) . ? P1 P1 2.0282(8) 3_655 ? N1 C1 1.3325(18) . ? N1 C6 1.4503(17) . ? N2 C3 1.3343(18) . ? N2 C18 1.4462(17) . ? C1 C2 1.407(2) . ? C1 C4 1.508(2) . ? C2 C3 1.403(2) . ? C3 C5 1.509(2) . ? C6 C7 1.4044(19) . ? C6 C11 1.4115(19) . ? C7 C8 1.396(2) . ? C7 C12 1.5186(18) . ? C8 C9 1.380(2) . ? C9 C10 1.383(2) . ? C10 C11 1.392(2) . ? C11 C15 1.520(2) . ? C12 C14 1.529(2) . ? C12 C13 1.529(2) . ? C15 C17 1.522(3) . ? C15 C16 1.523(2) . ? C18 C19 1.407(2) . ? C18 C23 1.4088(19) . ? C19 C20 1.398(2) . ? C19 C24 1.519(2) . ? C20 C21 1.379(2) . ? C21 C22 1.381(2) . ? C22 C23 1.394(2) . ? C23 C27 1.522(2) . ? C24 C26 1.531(2) . ? C24 C25 1.532(2) . ? C27 C29 1.525(2) . ? C27 C28 1.541(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 97.58(5) . . ? N2 Ga1 P1 112.51(3) . . ? N1 Ga1 P1 117.80(3) . . ? N2 Ga1 Br1 105.41(3) . . ? N1 Ga1 Br1 104.03(3) . . ? P1 Ga1 Br1 117.114(13) . . ? P1 P1 Ga1 94.92(2) 3_655 . ? C1 N1 C6 121.88(12) . . ? C1 N1 Ga1 118.24(9) . . ? C6 N1 Ga1 119.76(9) . . ? C3 N2 C18 122.87(12) . . ? C3 N2 Ga1 118.81(9) . . ? C18 N2 Ga1 118.31(9) . . ? N1 C1 C2 123.88(13) . . ? N1 C1 C4 119.56(13) . . ? C2 C1 C4 116.56(13) . . ? C3 C2 C1 128.53(13) . . ? N2 C3 C2 123.06(13) . . ? N2 C3 C5 119.43(13) . . ? C2 C3 C5 117.51(13) . . ? C7 C6 C11 120.91(13) . . ? C7 C6 N1 120.48(12) . . ? C11 C6 N1 118.48(12) . . ? C8 C7 C6 118.31(13) . . ? C8 C7 C12 118.31(13) . . ? C6 C7 C12 123.38(12) . . ? C9 C8 C7 121.47(14) . . ? C8 C9 C10 119.52(14) . . ? C9 C10 C11 121.60(14) . . ? C10 C11 C6 118.17(13) . . ? C10 C11 C15 119.47(13) . . ? C6 C11 C15 122.36(13) . . ? C7 C12 C14 111.10(13) . . ? C7 C12 C13 111.37(13) . . ? C14 C12 C13 109.53(14) . . ? C11 C15 C17 110.65(18) . . ? C11 C15 C16 113.12(14) . . ? C17 C15 C16 109.76(16) . . ? C19 C18 C23 121.11(13) . . ? C19 C18 N2 120.44(12) . . ? C23 C18 N2 118.26(12) . . ? C20 C19 C18 118.10(13) . . ? C20 C19 C24 118.64(14) . . ? C18 C19 C24 123.26(13) . . ? C21 C20 C19 121.34(15) . . ? C20 C21 C22 119.87(15) . . ? C21 C22 C23 121.38(14) . . ? C22 C23 C18 118.19(14) . . ? C22 C23 C27 119.59(13) . . ? C18 C23 C27 122.21(13) . . ? C19 C24 C26 111.33(14) . . ? C19 C24 C25 110.51(13) . . ? C26 C24 C25 110.49(14) . . ? C23 C27 C29 112.55(15) . . ? C23 C27 C28 110.43(15) . . ? C29 C27 C28 109.93(14) . . ? _refine_diff_density_max 0.502 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.053 _shelx_res_file ; TITL mks_005m in P2(1)/n mks_005m.res created by SHELXL-2017/1 at 09:43:34 on 06-Aug-2020 CELL 1.54178 13.64170 13.96140 15.75790 90.0000 105.1021 90.0000 ZERR 2.00000 0.00060 0.00060 0.00070 0.0000 0.0015 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H Br Ga N P UNIT 116 164 4 4 8 4 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.096 0.136 0.151 L.S. 16 ACTA FMAP 2 PLAN 20 WGHT 0.030700 1.803700 FVAR 0.10313 BR1 3 0.680602 0.061575 0.231363 11.00000 0.01910 0.02706 = 0.02174 0.00778 0.00402 0.00430 GA1 4 0.550596 0.132649 0.119522 11.00000 0.01327 0.01468 = 0.01372 -0.00212 0.00315 -0.00039 P1 6 0.443853 0.030518 0.022097 11.00000 0.01669 0.02257 = 0.02601 -0.01043 0.00463 -0.00346 N1 5 0.620274 0.231794 0.071132 11.00000 0.01356 0.01707 = 0.01359 -0.00065 0.00302 0.00033 N2 5 0.477873 0.215862 0.180058 11.00000 0.01429 0.01775 = 0.01561 -0.00283 0.00443 -0.00089 C1 1 0.641173 0.314202 0.114760 11.00000 0.01505 0.01810 = 0.02009 -0.00110 0.00369 -0.00155 C2 1 0.601048 0.340562 0.185128 11.00000 0.01963 0.01931 = 0.02190 -0.00704 0.00584 -0.00446 AFIX 43 H2 2 0.633404 0.393073 0.219605 11.00000 -1.20000 AFIX 0 C3 1 0.519554 0.299490 0.211051 11.00000 0.01800 0.01916 = 0.01823 -0.00467 0.00456 -0.00012 C4 1 0.711498 0.385181 0.088836 11.00000 0.02711 0.02152 = 0.03036 -0.00538 0.01280 -0.00809 AFIX 137 H4A 2 0.709088 0.376637 0.026596 11.00000 -1.50000 H4B 2 0.780996 0.374615 0.124660 11.00000 -1.50000 H4C 2 0.690118 0.450423 0.098401 11.00000 -1.50000 AFIX 0 C5 1 0.478494 0.353574 0.277282 11.00000 0.02601 0.02725 = 0.02922 -0.01267 0.01276 -0.00449 AFIX 137 H5A 2 0.474939 0.422004 0.262947 11.00000 -1.50000 H5B 2 0.523471 0.343948 0.336230 11.00000 -1.50000 H5C 2 0.410408 0.329890 0.275675 11.00000 -1.50000 AFIX 0 C6 1 0.653533 0.212523 -0.007427 11.00000 0.01623 0.01636 = 0.01437 -0.00007 0.00456 -0.00077 C7 1 0.750057 0.173487 -0.001083 11.00000 0.01483 0.02063 = 0.01772 -0.00071 0.00373 -0.00159 C8 1 0.776388 0.151248 -0.078691 11.00000 0.01701 0.03221 = 0.02081 -0.00312 0.00601 0.00223 AFIX 43 H8 2 0.841167 0.124199 -0.075427 11.00000 -1.20000 AFIX 0 C9 1 0.710402 0.167690 -0.160024 11.00000 0.02371 0.04152 = 0.01741 -0.00465 0.00754 0.00110 AFIX 43 H9 2 0.730057 0.152936 -0.212105 11.00000 -1.20000 AFIX 0 C10 1 0.615481 0.205790 -0.165166 11.00000 0.02274 0.04143 = 0.01468 0.00104 0.00257 0.00413 AFIX 43 H10 2 0.570390 0.217113 -0.221310 11.00000 -1.20000 AFIX 0 C11 1 0.584387 0.227958 -0.090079 11.00000 0.01857 0.02708 = 0.01738 0.00202 0.00382 0.00346 C12 1 0.826952 0.153459 0.085846 11.00000 0.01488 0.03277 = 0.01776 0.00157 0.00338 0.00372 AFIX 13 H12 2 0.796955 0.174129 0.134427 11.00000 -1.20000 AFIX 0 C13 1 0.925167 0.209680 0.093857 11.00000 0.01586 0.05576 = 0.02186 -0.00191 0.00253 -0.00434 AFIX 137 H13A 2 0.956503 0.189418 0.047450 11.00000 -1.50000 H13B 2 0.972113 0.197344 0.151442 11.00000 -1.50000 H13C 2 0.909819 0.278302 0.087811 11.00000 -1.50000 AFIX 0 C14 1 0.851018 0.046505 0.096903 11.00000 0.03291 0.03762 = 0.03176 0.00803 0.01050 0.01540 AFIX 137 H14A 2 0.787621 0.010181 0.087543 11.00000 -1.50000 H14B 2 0.893492 0.034397 0.156407 11.00000 -1.50000 H14C 2 0.887365 0.026387 0.053845 11.00000 -1.50000 AFIX 0 C15 1 0.478406 0.267872 -0.099408 11.00000 0.02432 0.05266 = 0.01887 0.00195 0.00270 0.01692 AFIX 13 H15 2 0.458653 0.252797 -0.044061 11.00000 -1.20000 AFIX 0 C16 1 0.398829 0.223808 -0.175625 11.00000 0.02015 0.05341 = 0.03028 0.01066 0.00343 0.00566 AFIX 137 H16A 2 0.414134 0.240669 -0.231173 11.00000 -1.50000 H16B 2 0.331554 0.248422 -0.175617 11.00000 -1.50000 H16C 2 0.399598 0.153982 -0.169125 11.00000 -1.50000 AFIX 0 C17 1 0.477977 0.376315 -0.109308 11.00000 0.05186 0.04583 = 0.10905 -0.02825 -0.02745 0.02851 AFIX 137 H17A 2 0.501543 0.393351 -0.161018 11.00000 -1.50000 H17B 2 0.523250 0.404874 -0.056721 11.00000 -1.50000 H17C 2 0.408861 0.400551 -0.116558 11.00000 -1.50000 AFIX 0 C18 1 0.381043 0.183816 0.190877 11.00000 0.01487 0.01811 = 0.01820 -0.00419 0.00595 -0.00070 C19 1 0.376617 0.122700 0.260803 11.00000 0.01848 0.02332 = 0.02069 -0.00187 0.00652 -0.00013 C20 1 0.281774 0.087213 0.263892 11.00000 0.02379 0.02888 = 0.03073 0.00283 0.01120 -0.00242 AFIX 43 H20 2 0.277273 0.045744 0.310527 11.00000 -1.20000 AFIX 0 C21 1 0.194610 0.111183 0.200616 11.00000 0.01833 0.03883 = 0.03716 0.00022 0.01053 -0.00553 AFIX 43 H21 2 0.130950 0.085882 0.203606 11.00000 -1.20000 AFIX 0 C22 1 0.200059 0.172047 0.132890 11.00000 0.01546 0.04172 = 0.02914 0.00088 0.00382 0.00012 AFIX 43 H22 2 0.139521 0.188903 0.090056 11.00000 -1.20000 AFIX 0 C23 1 0.292508 0.209249 0.126077 11.00000 0.01674 0.02669 = 0.02193 -0.00029 0.00646 0.00271 C24 1 0.469359 0.094598 0.333319 11.00000 0.02149 0.03304 = 0.01982 0.00484 0.00645 0.00128 AFIX 13 H24 2 0.529778 0.127726 0.322134 11.00000 -1.20000 AFIX 0 C25 1 0.457806 0.127531 0.422935 11.00000 0.03326 0.05918 = 0.02022 0.00152 0.00709 -0.00035 AFIX 137 H25A 2 0.446721 0.196922 0.421864 11.00000 -1.50000 H25B 2 0.519643 0.111822 0.468549 11.00000 -1.50000 H25C 2 0.399661 0.094917 0.435725 11.00000 -1.50000 AFIX 0 C26 1 0.488222 -0.013496 0.333677 11.00000 0.02760 0.03340 = 0.04239 0.01394 0.01374 0.00483 AFIX 137 H26A 2 0.430112 -0.047384 0.345215 11.00000 -1.50000 H26B 2 0.549740 -0.029149 0.379673 11.00000 -1.50000 H26C 2 0.496892 -0.033160 0.276373 11.00000 -1.50000 AFIX 0 C27 1 0.294788 0.277012 0.050967 11.00000 0.01693 0.04317 = 0.02828 0.01157 0.00632 0.00759 AFIX 13 H27 2 0.365704 0.278146 0.044313 11.00000 -1.20000 AFIX 0 C28 1 0.267152 0.379561 0.072667 11.00000 0.04747 0.03495 = 0.04169 0.00804 0.00034 -0.00040 AFIX 137 H28A 2 0.268743 0.422256 0.023680 11.00000 -1.50000 H28B 2 0.316253 0.401829 0.126100 11.00000 -1.50000 H28C 2 0.198888 0.379793 0.082016 11.00000 -1.50000 AFIX 0 C29 1 0.224528 0.244874 -0.036358 11.00000 0.03986 0.05045 = 0.02353 0.00420 0.00564 0.01541 AFIX 137 H29A 2 0.232918 0.287532 -0.083354 11.00000 -1.50000 H29B 2 0.153939 0.247274 -0.032727 11.00000 -1.50000 H29C 2 0.241584 0.179165 -0.049103 11.00000 -1.50000 AFIX 0 HKLF 4 REM mks_005m in P2(1)/n REM R1 = 0.0228 for 5955 Fo > 4sig(Fo) and 0.0243 for all 6312 data REM 317 parameters refined using 0 restraints END WGHT 0.0307 1.8037 REM Highest difference peak 0.502, deepest hole -0.377, 1-sigma level 0.053 Q1 1 0.6558 0.0136 0.1921 11.00000 0.05 0.50 Q2 1 0.3001 0.3591 0.0414 11.00000 0.05 0.48 Q3 1 0.4983 0.0182 -0.0018 11.00000 0.05 0.45 Q4 1 0.5236 0.4210 -0.1123 11.00000 0.05 0.44 Q5 1 0.4956 0.3218 -0.0929 11.00000 0.05 0.41 Q6 1 0.2942 0.2406 0.0893 11.00000 0.05 0.35 Q7 1 0.4639 0.0757 -0.0171 11.00000 0.05 0.35 Q8 1 0.5014 0.0797 0.0698 11.00000 0.05 0.33 Q9 1 0.5013 0.1914 0.1522 11.00000 0.05 0.32 Q10 1 0.5625 0.3216 0.1927 11.00000 0.05 0.32 Q11 1 0.6197 0.3227 0.1531 11.00000 0.05 0.29 Q12 1 0.7579 0.1593 -0.0373 11.00000 0.05 0.28 Q13 1 0.7030 0.1839 -0.0029 11.00000 0.05 0.28 Q14 1 0.6798 0.3491 0.1055 11.00000 0.05 0.28 Q15 1 0.4326 0.2051 0.1875 11.00000 0.05 0.28 Q16 1 0.5827 0.1887 0.0868 11.00000 0.05 0.28 Q17 1 0.5984 0.0990 0.1940 11.00000 0.05 0.27 Q18 1 0.4992 0.3284 0.2441 11.00000 0.05 0.27 Q19 1 0.4994 0.2563 0.1949 11.00000 0.05 0.27 Q20 1 0.3802 0.1535 0.2257 11.00000 0.05 0.27 ; _shelx_res_checksum 77466 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_037am_sq _database_code_depnum_ccdc_archive 'CCDC 2184011' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT934_mks_037am_sq ; PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers .. 6 Check RESPONSE: Diffuse scattering at low angle caused by the mounting material. ; # end Validation Reply Form _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H94 Cl2 Ga2 N6 P2' _chemical_formula_weight 1231.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.863(2) _cell_length_b 20.330(5) _cell_length_c 25.712(6) _cell_angle_alpha 83.603(4) _cell_angle_beta 75.258(6) _cell_angle_gamma 72.565(4) _cell_volume 7163(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9899 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.26 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_F_000 2608 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.152 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.094 _exptl_absorpt_coefficient_mu 0.910 _shelx_estimated_absorpt_T_min 0.874 _shelx_estimated_absorpt_T_max 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_measurement_device_type 'Bruker D8 KAPPA II (APEX II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/QUEEN' _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 264320 _diffrn_reflns_av_unetI/netI 0.0640 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.639 _diffrn_reflns_theta_max 30.528 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 43665 _reflns_number_gt 30501 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'BRUKER APEX3(v2019.1-0)' _computing_cell_refinement 'BRUKER APEX3(v2019.1-0)' _computing_data_reduction 'BRUKER APEX3(v2019.1-0)' _computing_structure_solution 'BRUKER APEX3(v2019.1-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. SQUEEZE: The structure contains highly disordered solvent - possibly n-hexane. The final refinement was done with a solvent free dataset from a PLATON/SQUEEZE run. (For details see: A.~L.~Spek, Acta Cryst. A46 (1990),194--201). Since the nature and amount of the solvent is not clear it was not included in the sum formula. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 43665 _refine_ls_number_parameters 1435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ga1_1 Ga 0.76529(2) 0.30388(2) 0.68895(2) 0.01298(5) Uani 1 1 d . . . . . Ga2_1 Ga 0.94908(2) 0.31180(2) 0.47835(2) 0.01340(5) Uani 1 1 d . . . . . Cl1_1 Cl 0.86377(4) 0.24692(3) 0.74149(2) 0.02164(11) Uani 1 1 d . . . . . Cl2_1 Cl 0.95391(4) 0.42104(2) 0.48260(2) 0.01826(10) Uani 1 1 d . . . . . P1_1 P 0.83203(4) 0.34684(3) 0.60471(2) 0.01362(10) Uani 1 1 d . . . . . P2_1 P 0.88323(4) 0.25729(3) 0.55406(2) 0.01627(10) Uani 1 1 d . . . . . N1_1 N 0.68052(11) 0.24476(8) 0.69617(6) 0.0141(3) Uani 1 1 d . . . . . N2_1 N 0.67579(12) 0.37239(8) 0.74083(6) 0.0160(3) Uani 1 1 d . . . . . N3_1 N 0.90563(12) 0.31669(9) 0.41077(7) 0.0169(3) Uani 1 1 d . . . . . N4_1 N 1.08939(12) 0.27027(8) 0.44188(7) 0.0155(3) Uani 1 1 d . . . . . N5_1 N 0.93854(12) 0.42728(8) 0.63035(7) 0.0173(3) Uani 1 1 d . . . . . N6_1 N 1.01712(12) 0.32003(8) 0.63772(7) 0.0167(3) Uani 1 1 d . . . . . C1_1 C 0.62064(14) 0.23992(10) 0.74424(8) 0.0175(4) Uani 1 1 d . . . . . C2_1 C 0.59586(15) 0.28749(11) 0.78499(8) 0.0206(4) Uani 1 1 d . . . . . H2_1 H 0.563318 0.273949 0.819457 0.025 Uiso 1 1 calc R U . . . C3_1 C 0.61286(15) 0.35187(11) 0.78132(8) 0.0196(4) Uani 1 1 d . . . . . C4_1 C 0.57364(16) 0.18180(12) 0.75624(9) 0.0247(5) Uani 1 1 d . . . . . H4A_1 H 0.539124 0.182048 0.728394 0.037 Uiso 1 1 calc R U . . . H4B_1 H 0.527663 0.188013 0.791425 0.037 Uiso 1 1 calc R U . . . H4C_1 H 0.623642 0.137651 0.756686 0.037 Uiso 1 1 calc R U . . . C5_1 C 0.55411(18) 0.40038(12) 0.82656(9) 0.0311(5) Uani 1 1 d . . . . . H5A_1 H 0.526809 0.446203 0.811256 0.047 Uiso 1 1 calc R U . . . H5B_1 H 0.596247 0.403708 0.849329 0.047 Uiso 1 1 calc R U . . . H5C_1 H 0.501389 0.382495 0.848259 0.047 Uiso 1 1 calc R U . . . C6_1 C 0.68968(14) 0.19811(10) 0.65491(8) 0.0169(4) Uani 1 1 d . . . . . C7_1 C 0.64023(15) 0.22429(11) 0.61351(8) 0.0196(4) Uani 1 1 d . . . . . C8_1 C 0.64703(18) 0.17825(12) 0.57523(9) 0.0282(5) Uani 1 1 d . . . . . H8_1 H 0.612776 0.194083 0.547598 0.034 Uiso 1 1 calc R U . . . C9_1 C 0.70244(19) 0.11013(13) 0.57656(9) 0.0322(6) Uani 1 1 d . . . . . H9_1 H 0.705062 0.079605 0.550443 0.039 Uiso 1 1 calc R U . . . C10_1 C 0.75378(17) 0.08678(12) 0.61590(9) 0.0271(5) Uani 1 1 d . . . . . H10_1 H 0.793502 0.040438 0.615790 0.032 Uiso 1 1 calc R U . . . C11_1 C 0.74865(15) 0.12971(10) 0.65586(8) 0.0191(4) Uani 1 1 d . . . . . C12_1 C 0.58241(16) 0.29956(11) 0.61037(9) 0.0226(5) Uani 1 1 d . . . . . H12_1 H 0.618807 0.327468 0.621687 0.027 Uiso 1 1 calc R U . . . C13_1 C 0.48202(17) 0.31449(12) 0.64874(10) 0.0318(6) Uani 1 1 d . . . . . H13A_1 H 0.447789 0.363593 0.645586 0.048 Uiso 1 1 calc R U . . . H13B_1 H 0.488982 0.302643 0.685795 0.048 Uiso 1 1 calc R U . . . H13C_1 H 0.444935 0.286816 0.639445 0.048 Uiso 1 1 calc R U . . . C14_1 C 0.57295(19) 0.32423(13) 0.55276(10) 0.0324(6) Uani 1 1 d . . . . . H14A_1 H 0.637366 0.312913 0.528232 0.049 Uiso 1 1 calc R U . . . H14B_1 H 0.543520 0.374268 0.551642 0.049 Uiso 1 1 calc R U . . . H14C_1 H 0.531926 0.301218 0.541694 0.049 Uiso 1 1 calc R U . . . C15_1 C 0.80938(16) 0.10118(10) 0.69696(9) 0.0217(4) Uani 1 1 d . . . . . H15_1 H 0.789171 0.135128 0.725985 0.026 Uiso 1 1 calc R U . . . C16_1 C 0.7964(2) 0.03169(11) 0.72288(10) 0.0327(6) Uani 1 1 d . . . . . H16A_1 H 0.818053 -0.002646 0.695103 0.049 Uiso 1 1 calc R U . . . H16B_1 H 0.727826 0.037198 0.740096 0.049 Uiso 1 1 calc R U . . . H16C_1 H 0.835069 0.016233 0.749961 0.049 Uiso 1 1 calc R U . . . C17_1 C 0.91711(17) 0.09257(13) 0.66980(11) 0.0328(6) Uani 1 1 d . . . . . H17A_1 H 0.937813 0.060001 0.640796 0.049 Uiso 1 1 calc R U . . . H17B_1 H 0.956245 0.074875 0.696468 0.049 Uiso 1 1 calc R U . . . H17C_1 H 0.925816 0.137347 0.654864 0.049 Uiso 1 1 calc R U . . . C18_1 C 0.67964(16) 0.44348(10) 0.73642(8) 0.0201(4) Uani 1 1 d . . . . . C19_1 C 0.62303(17) 0.49091(11) 0.70473(8) 0.0248(5) Uani 1 1 d . . . . . C20_1 C 0.6291(2) 0.55865(11) 0.69875(9) 0.0325(6) Uani 1 1 d . . . . . H20_1 H 0.590536 0.591564 0.678164 0.039 Uiso 1 1 calc R U . . . C21_1 C 0.6897(2) 0.57861(12) 0.72205(10) 0.0385(7) Uani 1 1 d . . . . . H21_1 H 0.695084 0.624396 0.716066 0.046 Uiso 1 1 calc R U . . . C22_1 C 0.7431(2) 0.53227(11) 0.75419(9) 0.0340(6) Uani 1 1 d . . . . . H22_1 H 0.783857 0.546914 0.770656 0.041 Uiso 1 1 calc R U . . . C23_1 C 0.73799(18) 0.46422(11) 0.76289(8) 0.0256(5) Uani 1 1 d . . . . . C24_1 C 0.55400(17) 0.47080(12) 0.67928(9) 0.0278(5) Uani 1 1 d . . . . . H24_1 H 0.564961 0.419785 0.684752 0.033 Uiso 1 1 calc R U . . . C25_1 C 0.44818(19) 0.50603(16) 0.70625(10) 0.0451(7) Uani 1 1 d . . . . . H25A_1 H 0.434494 0.556010 0.699247 0.068 Uiso 1 1 calc R U . . . H25B_1 H 0.437152 0.495908 0.745152 0.068 Uiso 1 1 calc R U . . . H25C_1 H 0.405225 0.488689 0.691610 0.068 Uiso 1 1 calc R U . . . C26_1 C 0.57451(17) 0.48776(13) 0.61873(9) 0.0308(5) Uani 1 1 d . . . . . H26A_1 H 0.643445 0.467391 0.602647 0.046 Uiso 1 1 calc R U . . . H26B_1 H 0.557913 0.537935 0.612404 0.046 Uiso 1 1 calc R U . . . H26C_1 H 0.535334 0.468831 0.602335 0.046 Uiso 1 1 calc R U . . . C27_1 C 0.79227(18) 0.41665(11) 0.80234(9) 0.0253(5) Uani 1 1 d . . . . . H27_1 H 0.774557 0.372280 0.806852 0.030 Uiso 1 1 calc R U . . . C28_1 C 0.7609(2) 0.44930(13) 0.85799(10) 0.0409(7) Uani 1 1 d . . . . . H28A_1 H 0.781117 0.491542 0.854871 0.061 Uiso 1 1 calc R U . . . H28B_1 H 0.791592 0.416570 0.883685 0.061 Uiso 1 1 calc R U . . . H28C_1 H 0.690272 0.460489 0.870668 0.061 Uiso 1 1 calc R U . . . C29_1 C 0.9016(2) 0.40048(13) 0.78169(11) 0.0359(6) Uani 1 1 d . . . . . H29A_1 H 0.921317 0.377272 0.747486 0.054 Uiso 1 1 calc R U . . . H29B_1 H 0.933612 0.370255 0.808084 0.054 Uiso 1 1 calc R U . . . H29C_1 H 0.920384 0.443468 0.776194 0.054 Uiso 1 1 calc R U . . . C30_1 C 0.96322(16) 0.32519(11) 0.36268(8) 0.0205(4) Uani 1 1 d . . . . . C31_1 C 1.06329(16) 0.31285(11) 0.35387(8) 0.0209(4) Uani 1 1 d . . . . . H31_1 H 1.094966 0.327786 0.319674 0.025 Uiso 1 1 calc R U . . . C32_1 C 1.12354(15) 0.28081(10) 0.38956(8) 0.0174(4) Uani 1 1 d . . . . . C33_1 C 0.91915(18) 0.34693(13) 0.31396(9) 0.0298(5) Uani 1 1 d . . . . . H33A_1 H 0.969929 0.351657 0.282125 0.045 Uiso 1 1 calc R U . . . H33B_1 H 0.869142 0.391236 0.320326 0.045 Uiso 1 1 calc R U . . . H33C_1 H 0.890005 0.311899 0.308056 0.045 Uiso 1 1 calc R U . . . C34_1 C 1.23090(16) 0.25731(11) 0.36437(9) 0.0238(5) Uani 1 1 d . . . . . H34A_1 H 1.240954 0.246118 0.326844 0.036 Uiso 1 1 calc R U . . . H34B_1 H 1.261435 0.216280 0.384294 0.036 Uiso 1 1 calc R U . . . H34C_1 H 1.259996 0.294288 0.365631 0.036 Uiso 1 1 calc R U . . . C35_1 C 0.80841(16) 0.31526(11) 0.41145(8) 0.0200(4) Uani 1 1 d . . . . . C36_1 C 0.73136(16) 0.37613(11) 0.41812(8) 0.0207(4) Uani 1 1 d . . . . . C37_1 C 0.64044(17) 0.37255(12) 0.41567(9) 0.0275(5) Uani 1 1 d . . . . . H37_1 H 0.587472 0.413252 0.420161 0.033 Uiso 1 1 calc R U . . . C38_1 C 0.62533(19) 0.31126(14) 0.40688(11) 0.0345(6) Uani 1 1 d . . . . . H38_1 H 0.563011 0.310327 0.404435 0.041 Uiso 1 1 calc R U . . . C39_1 C 0.70077(19) 0.25168(13) 0.40170(10) 0.0330(6) Uani 1 1 d . . . . . H39_1 H 0.689589 0.209564 0.396373 0.040 Uiso 1 1 calc R U . . . C40_1 C 0.79376(17) 0.25179(11) 0.40410(9) 0.0244(5) Uani 1 1 d . . . . . C41_1 C 0.74479(16) 0.44430(11) 0.42959(8) 0.0208(4) Uani 1 1 d . . . . . H41_1 H 0.815919 0.438245 0.423637 0.025 Uiso 1 1 calc R U . . . C42_1 C 0.69770(17) 0.46152(12) 0.48841(9) 0.0278(5) Uani 1 1 d . . . . . H42A_1 H 0.709885 0.503815 0.496090 0.042 Uiso 1 1 calc R U . . . H42B_1 H 0.725348 0.423432 0.511760 0.042 Uiso 1 1 calc R U . . . H42C_1 H 0.627638 0.468383 0.495116 0.042 Uiso 1 1 calc R U . . . C43_1 C 0.70409(18) 0.50471(12) 0.39267(10) 0.0318(6) Uani 1 1 d . . . . . H43A_1 H 0.730769 0.491977 0.355021 0.048 Uiso 1 1 calc R U . . . H43B_1 H 0.722314 0.545332 0.398532 0.048 Uiso 1 1 calc R U . . . H43C_1 H 0.633255 0.515348 0.400926 0.048 Uiso 1 1 calc R U . . . C44_1 C 0.87512(18) 0.18493(12) 0.39848(10) 0.0288(5) Uani 1 1 d . . . . . H44_1 H 0.933751 0.195460 0.403655 0.035 Uiso 1 1 calc R U . . . C45_1 C 0.8511(2) 0.13183(14) 0.44198(13) 0.0464(7) Uani 1 1 d . . . . . H45A_1 H 0.793887 0.120148 0.437983 0.070 Uiso 1 1 calc R U . . . H45B_1 H 0.837590 0.150867 0.477445 0.070 Uiso 1 1 calc R U . . . H45C_1 H 0.906225 0.090193 0.438613 0.070 Uiso 1 1 calc R U . . . C46_1 C 0.9017(3) 0.15540(16) 0.34217(13) 0.0617(10) Uani 1 1 d . . . . . H46A_1 H 0.919116 0.189942 0.314822 0.093 Uiso 1 1 calc R U . . . H46B_1 H 0.846077 0.143592 0.336048 0.093 Uiso 1 1 calc R U . . . H46C_1 H 0.956947 0.113888 0.339809 0.093 Uiso 1 1 calc R U . . . C47_1 C 1.15618(14) 0.23375(10) 0.47451(8) 0.0169(4) Uani 1 1 d . . . . . C48_1 C 1.21861(15) 0.26563(10) 0.48784(8) 0.0195(4) Uani 1 1 d . . . . . C49_1 C 1.28377(16) 0.22673(11) 0.51838(9) 0.0250(5) Uani 1 1 d . . . . . H49_1 H 1.327019 0.247087 0.527730 0.030 Uiso 1 1 calc R U . . . C50_1 C 1.28617(17) 0.15909(12) 0.53517(10) 0.0285(5) Uani 1 1 d . . . . . H50_1 H 1.332004 0.133177 0.554977 0.034 Uiso 1 1 calc R U . . . C51_1 C 1.22228(16) 0.12951(11) 0.52317(9) 0.0259(5) Uani 1 1 d . . . . . H51_1 H 1.223478 0.083597 0.535797 0.031 Uiso 1 1 calc R U . . . C52_1 C 1.15576(15) 0.16526(10) 0.49294(8) 0.0190(4) Uani 1 1 d . . . . . C53_1 C 1.21739(15) 0.34037(10) 0.47190(9) 0.0195(4) Uani 1 1 d . . . . . H53_1 H 1.175265 0.357643 0.445683 0.023 Uiso 1 1 calc R U . . . C54_1 C 1.17304(17) 0.38508(11) 0.52150(9) 0.0246(5) Uani 1 1 d . . . . . H54A_1 H 1.166946 0.433615 0.510356 0.037 Uiso 1 1 calc R U . . . H54B_1 H 1.215083 0.370653 0.546951 0.037 Uiso 1 1 calc R U . . . H54C_1 H 1.108780 0.379519 0.538832 0.037 Uiso 1 1 calc R U . . . C55_1 C 1.31867(17) 0.34839(13) 0.44491(10) 0.0302(5) Uani 1 1 d . . . . . H55A_1 H 1.349690 0.316083 0.415696 0.045 Uiso 1 1 calc R U . . . H55B_1 H 1.358286 0.338489 0.471561 0.045 Uiso 1 1 calc R U . . . H55C_1 H 1.312585 0.395728 0.430263 0.045 Uiso 1 1 calc R U . . . C56_1 C 1.08757(16) 0.13101(10) 0.47838(9) 0.0221(4) Uani 1 1 d . . . . . H56_1 H 1.025429 0.167533 0.477595 0.027 Uiso 1 1 calc R U . . . C57_1 C 1.06331(19) 0.07446(12) 0.51928(11) 0.0353(6) Uani 1 1 d . . . . . H57A_1 H 1.011760 0.059641 0.510925 0.053 Uiso 1 1 calc R U . . . H57B_1 H 1.041385 0.092496 0.555557 0.053 Uiso 1 1 calc R U . . . H57C_1 H 1.121238 0.035046 0.517549 0.053 Uiso 1 1 calc R U . . . C58_1 C 1.12919(18) 0.10191(12) 0.42192(10) 0.0317(6) Uani 1 1 d . . . . . H58A_1 H 1.139819 0.139197 0.395604 0.047 Uiso 1 1 calc R U . . . H58B_1 H 1.083369 0.081504 0.412927 0.047 Uiso 1 1 calc R U . . . H58C_1 H 1.190965 0.066461 0.421182 0.047 Uiso 1 1 calc R U . . . C59_1 C 0.93469(14) 0.36259(10) 0.62559(8) 0.0146(4) Uani 1 1 d . . . . . C60_1 C 1.02090(16) 0.42579(11) 0.64710(8) 0.0201(4) Uani 1 1 d . . . . . C61_1 C 1.07004(15) 0.35814(11) 0.65173(8) 0.0196(4) Uani 1 1 d . . . . . C62_1 C 0.87050(16) 0.49121(10) 0.61522(9) 0.0225(5) Uani 1 1 d . . . . . H62A_1 H 0.905748 0.516391 0.586528 0.034 Uiso 1 1 calc R U . . . H62B_1 H 0.840000 0.520030 0.646616 0.034 Uiso 1 1 calc R U . . . H62C_1 H 0.820433 0.479821 0.602430 0.034 Uiso 1 1 calc R U . . . C63_1 C 1.05014(15) 0.24458(10) 0.63455(9) 0.0205(4) Uani 1 1 d . . . . . H63A_1 H 1.005464 0.229127 0.619894 0.031 Uiso 1 1 calc R U . . . H63B_1 H 1.051636 0.223520 0.670628 0.031 Uiso 1 1 calc R U . . . H63C_1 H 1.115341 0.230750 0.611029 0.031 Uiso 1 1 calc R U . . . C64_1 C 1.04141(19) 0.48998(12) 0.65747(10) 0.0297(5) Uani 1 1 d . . . . . H64A_1 H 1.051128 0.517589 0.623843 0.045 Uiso 1 1 calc R U . . . H64B_1 H 1.100083 0.477757 0.671425 0.045 Uiso 1 1 calc R U . . . H64C_1 H 0.986489 0.516784 0.683970 0.045 Uiso 1 1 calc R U . . . C65_1 C 1.16355(17) 0.32508(13) 0.66820(10) 0.0308(5) Uani 1 1 d . . . . . H65A_1 H 1.211189 0.299062 0.638325 0.046 Uiso 1 1 calc R U . . . H65B_1 H 1.152713 0.293688 0.699455 0.046 Uiso 1 1 calc R U . . . H65C_1 H 1.187976 0.360822 0.677603 0.046 Uiso 1 1 calc R U . . . Ga1_2 Ga 0.40664(2) 0.99504(2) 0.80066(2) 0.01192(5) Uani 1 1 d . . . . . Ga2_2 Ga 0.23905(2) 0.82313(2) 0.94447(2) 0.01381(5) Uani 1 1 d . . . . . Cl1_2 Cl 0.49842(4) 1.04119(3) 0.83207(2) 0.02480(11) Uani 1 1 d . . . . . Cl2_2 Cl 0.09685(3) 0.90661(2) 0.96383(2) 0.01843(10) Uani 1 1 d . . . . . P1_2 P 0.28973(4) 0.95134(3) 0.86156(2) 0.01309(10) Uani 1 1 d . . . . . P2_2 P 0.36831(4) 0.84831(3) 0.88620(2) 0.01702(11) Uani 1 1 d . . . . . N1_2 N 0.35695(11) 1.07141(8) 0.75176(6) 0.0130(3) Uani 1 1 d . . . . . N2_2 N 0.50627(12) 0.93796(8) 0.74544(6) 0.0140(3) Uani 1 1 d . . . . . N3_2 N 0.25551(12) 0.79230(9) 1.01942(6) 0.0166(3) Uani 1 1 d . . . . . N4_2 N 0.19339(12) 0.74212(8) 0.93728(7) 0.0174(3) Uani 1 1 d . . . . . N5_2 N 0.18748(12) 1.06635(8) 0.92595(6) 0.0153(3) Uani 1 1 d . . . . . N6_2 N 0.32507(12) 1.02002(8) 0.94681(6) 0.0154(3) Uani 1 1 d . . . . . C1_2 C 0.41633(14) 1.08301(10) 0.70506(8) 0.0149(4) Uani 1 1 d . . . . . C2_2 C 0.50597(14) 1.03737(10) 0.68396(8) 0.0178(4) Uani 1 1 d . . . . . H2_2 H 0.546685 1.055223 0.654713 0.021 Uiso 1 1 calc R U . . . C3_2 C 0.54461(14) 0.96816(10) 0.70010(8) 0.0169(4) Uani 1 1 d . . . . . C4_2 C 0.38497(15) 1.14779(10) 0.67163(8) 0.0202(4) Uani 1 1 d . . . . . H4A_2 H 0.436748 1.149074 0.639461 0.030 Uiso 1 1 calc R U . . . H4B_2 H 0.371637 1.188223 0.692865 0.030 Uiso 1 1 calc R U . . . H4C_2 H 0.326141 1.148163 0.660844 0.030 Uiso 1 1 calc R U . . . C5_2 C 0.63413(16) 0.92776(11) 0.66191(8) 0.0236(5) Uani 1 1 d . . . . . H5A_2 H 0.634851 0.947203 0.625221 0.035 Uiso 1 1 calc R U . . . H5B_2 H 0.633826 0.879457 0.663322 0.035 Uiso 1 1 calc R U . . . H5C_2 H 0.691939 0.930352 0.672335 0.035 Uiso 1 1 calc R U . . . C6_2 C 0.25921(14) 1.11660(10) 0.76557(7) 0.0142(4) Uani 1 1 d . . . . . C7_2 C 0.18548(14) 1.09775(10) 0.75079(8) 0.0162(4) Uani 1 1 d . . . . . C8_2 C 0.09093(14) 1.14110(10) 0.76400(8) 0.0183(4) Uani 1 1 d . . . . . H8_2 H 0.040426 1.129327 0.754169 0.022 Uiso 1 1 calc R U . . . C9_2 C 0.06953(15) 1.20111(11) 0.79128(8) 0.0199(4) Uani 1 1 d . . . . . H9_2 H 0.004695 1.229837 0.800296 0.024 Uiso 1 1 calc R U . . . C10_2 C 0.14287(14) 1.21907(10) 0.80533(8) 0.0178(4) Uani 1 1 d . . . . . H10_2 H 0.127460 1.260127 0.824156 0.021 Uiso 1 1 calc R U . . . C11_2 C 0.23913(14) 1.17803(10) 0.79239(8) 0.0149(4) Uani 1 1 d . . . . . C12_2 C 0.20694(15) 1.03288(11) 0.71948(9) 0.0214(4) Uani 1 1 d . . . . . H12_2 H 0.275176 1.005149 0.719117 0.026 Uiso 1 1 calc R U . . . C13_2 C 0.14079(19) 0.98808(12) 0.74651(9) 0.0294(5) Uani 1 1 d . . . . . H13A_2 H 0.073551 1.013121 0.745822 0.044 Uiso 1 1 calc R U . . . H13B_2 H 0.146060 0.977054 0.783901 0.044 Uiso 1 1 calc R U . . . H13C_2 H 0.160274 0.945280 0.727168 0.044 Uiso 1 1 calc R U . . . C14_2 C 0.20005(19) 1.05128(13) 0.66096(9) 0.0327(6) Uani 1 1 d . . . . . H14A_2 H 0.247736 1.076014 0.643293 0.049 Uiso 1 1 calc R U . . . H14B_2 H 0.134728 1.080678 0.660106 0.049 Uiso 1 1 calc R U . . . H14C_2 H 0.213262 1.008923 0.642030 0.049 Uiso 1 1 calc R U . . . C15_2 C 0.31750(14) 1.20244(10) 0.80590(8) 0.0165(4) Uani 1 1 d . . . . . H15_2 H 0.381840 1.171231 0.788443 0.020 Uiso 1 1 calc R U . . . C16_2 C 0.31018(16) 1.19833(11) 0.86649(8) 0.0226(4) Uani 1 1 d . . . . . H16A_2 H 0.318914 1.150287 0.879820 0.034 Uiso 1 1 calc R U . . . H16B_2 H 0.246261 1.226634 0.884792 0.034 Uiso 1 1 calc R U . . . H16C_2 H 0.360687 1.215436 0.873702 0.034 Uiso 1 1 calc R U . . . C17_2 C 0.31444(16) 1.27644(11) 0.78382(10) 0.0252(5) Uani 1 1 d . . . . . H17A_2 H 0.370980 1.288061 0.788886 0.038 Uiso 1 1 calc R U . . . H17B_2 H 0.254997 1.308754 0.803140 0.038 Uiso 1 1 calc R U . . . H17C_2 H 0.315399 1.279619 0.745381 0.038 Uiso 1 1 calc R U . . . C18_2 C 0.54518(14) 0.86467(10) 0.75705(8) 0.0165(4) Uani 1 1 d . . . . . C19_2 C 0.49388(16) 0.81953(11) 0.74971(8) 0.0208(4) Uani 1 1 d . . . . . C20_2 C 0.52669(17) 0.75005(11) 0.76467(9) 0.0257(5) Uani 1 1 d . . . . . H20_2 H 0.494576 0.718439 0.758983 0.031 Uiso 1 1 calc R U . . . C21_2 C 0.60609(17) 0.72669(11) 0.78785(9) 0.0262(5) Uani 1 1 d . . . . . H21_2 H 0.626121 0.679630 0.799362 0.031 Uiso 1 1 calc R U . . . C22_2 C 0.65547(16) 0.77099(11) 0.79417(9) 0.0234(5) Uani 1 1 d . . . . . H22_2 H 0.710129 0.753868 0.809613 0.028 Uiso 1 1 calc R U . . . C23_2 C 0.62785(15) 0.84062(10) 0.77859(8) 0.0188(4) Uani 1 1 d . . . . . C24_2 C 0.40325(18) 0.84605(12) 0.72698(10) 0.0280(5) Uani 1 1 d . . . . . H24_2 H 0.366841 0.892009 0.742757 0.034 Uiso 1 1 calc R U . . . C25_2 C 0.33460(19) 0.80115(13) 0.74289(10) 0.0345(6) Uani 1 1 d . . . . . H25A_2 H 0.273586 0.825065 0.732490 0.052 Uiso 1 1 calc R U . . . H25B_2 H 0.321620 0.791991 0.781926 0.052 Uiso 1 1 calc R U . . . H25C_2 H 0.364257 0.757417 0.724539 0.052 Uiso 1 1 calc R U . . . C26_2 C 0.4277(2) 0.85833(17) 0.66667(11) 0.0491(8) Uani 1 1 d . . . . . H26A_2 H 0.467142 0.814987 0.649501 0.074 Uiso 1 1 calc R U . . . H26B_2 H 0.464074 0.892667 0.657411 0.074 Uiso 1 1 calc R U . . . H26C_2 H 0.367665 0.875293 0.653949 0.074 Uiso 1 1 calc R U . . . C27_2 C 0.68786(15) 0.88589(11) 0.78644(8) 0.0209(4) Uani 1 1 d . . . . . H27_2 H 0.661097 0.933316 0.771549 0.025 Uiso 1 1 calc R U . . . C28_2 C 0.68270(18) 0.89084(12) 0.84643(9) 0.0294(5) Uani 1 1 d . . . . . H28A_2 H 0.710822 0.844985 0.861398 0.044 Uiso 1 1 calc R U . . . H28B_2 H 0.614842 0.908474 0.865742 0.044 Uiso 1 1 calc R U . . . H28C_2 H 0.719149 0.922228 0.850373 0.044 Uiso 1 1 calc R U . . . C29_2 C 0.79490(16) 0.85834(12) 0.75632(9) 0.0262(5) Uani 1 1 d . . . . . H29A_2 H 0.798930 0.857788 0.717725 0.039 Uiso 1 1 calc R U . . . H29B_2 H 0.821923 0.811401 0.769856 0.039 Uiso 1 1 calc R U . . . H29C_2 H 0.831848 0.888325 0.762254 0.039 Uiso 1 1 calc R U . . . C30_2 C 0.20286(15) 0.75450(10) 1.05121(8) 0.0191(4) Uani 1 1 d . . . . . C31_2 C 0.14356(15) 0.72374(11) 1.03328(8) 0.0208(4) Uani 1 1 d . . . . . H31_2 H 0.097445 0.707928 1.060574 0.025 Uiso 1 1 calc R U . . . C32_2 C 0.14407(15) 0.71357(10) 0.98034(9) 0.0201(4) Uani 1 1 d . . . . . C33_2 C 0.20740(17) 0.74029(12) 1.10993(9) 0.0259(5) Uani 1 1 d . . . . . H33A_2 H 0.170713 0.707391 1.126283 0.039 Uiso 1 1 calc R U . . . H33B_2 H 0.179263 0.783466 1.129122 0.039 Uiso 1 1 calc R U . . . H33C_2 H 0.275140 0.720837 1.112255 0.039 Uiso 1 1 calc R U . . . C34_2 C 0.08855(18) 0.66522(12) 0.97233(10) 0.0284(5) Uani 1 1 d . . . . . H34A_2 H 0.040846 0.689456 0.951410 0.043 Uiso 1 1 calc R U . . . H34B_2 H 0.055080 0.649995 1.007461 0.043 Uiso 1 1 calc R U . . . H34C_2 H 0.133892 0.625011 0.952949 0.043 Uiso 1 1 calc R U . . . C35_2 C 0.31872(15) 0.81767(10) 1.04140(8) 0.0176(4) Uani 1 1 d . . . . . C36_2 C 0.27967(15) 0.87291(11) 1.07661(8) 0.0193(4) Uani 1 1 d . . . . . C37_2 C 0.34398(17) 0.89415(12) 1.09774(9) 0.0253(5) Uani 1 1 d . . . . . H37_2 H 0.319427 0.931446 1.121412 0.030 Uiso 1 1 calc R U . . . C38_2 C 0.44272(18) 0.86184(13) 1.08479(10) 0.0297(5) Uani 1 1 d . . . . . H38_2 H 0.485020 0.876356 1.100178 0.036 Uiso 1 1 calc R U . . . C39_2 C 0.47979(17) 0.80841(13) 1.04945(9) 0.0274(5) Uani 1 1 d . . . . . H39_2 H 0.547697 0.786897 1.040692 0.033 Uiso 1 1 calc R U . . . C40_2 C 0.41960(16) 0.78534(11) 1.02632(8) 0.0222(4) Uani 1 1 d . . . . . C41_2 C 0.17209(15) 0.91108(11) 1.09118(8) 0.0189(4) Uani 1 1 d . . . . . H41_2 H 0.136253 0.884341 1.078012 0.023 Uiso 1 1 calc R U . . . C42_2 C 0.13169(19) 0.91843(13) 1.15211(9) 0.0318(5) Uani 1 1 d . . . . . H42A_2 H 0.160480 0.949013 1.165130 0.048 Uiso 1 1 calc R U . . . H42B_2 H 0.147719 0.872958 1.170382 0.048 Uiso 1 1 calc R U . . . H42C_2 H 0.061094 0.938020 1.159701 0.048 Uiso 1 1 calc R U . . . C43_2 C 0.15369(17) 0.98266(11) 1.06304(9) 0.0240(5) Uani 1 1 d . . . . . H43A_2 H 0.181091 0.978082 1.024255 0.036 Uiso 1 1 calc R U . . . H43B_2 H 0.184475 1.010840 1.077267 0.036 Uiso 1 1 calc R U . . . H43C_2 H 0.083707 1.004874 1.069599 0.036 Uiso 1 1 calc R U . . . C44_2 C 0.46269(16) 0.72561(11) 0.98837(9) 0.0243(5) Uani 1 1 d . . . . . H44_2 H 0.417224 0.730481 0.964511 0.029 Uiso 1 1 calc R U . . . C45_2 C 0.4680(2) 0.65643(13) 1.02014(11) 0.0409(7) Uani 1 1 d . . . . . H45A_2 H 0.493001 0.618690 0.995048 0.061 Uiso 1 1 calc R U . . . H45B_2 H 0.403089 0.656271 1.041206 0.061 Uiso 1 1 calc R U . . . H45C_2 H 0.511417 0.650201 1.044436 0.061 Uiso 1 1 calc R U . . . C46_2 C 0.56122(18) 0.72622(15) 0.95196(10) 0.0374(6) Uani 1 1 d . . . . . H46A_2 H 0.582081 0.689690 0.926000 0.056 Uiso 1 1 calc R U . . . H46B_2 H 0.608891 0.718311 0.973881 0.056 Uiso 1 1 calc R U . . . H46C_2 H 0.555910 0.771071 0.932627 0.056 Uiso 1 1 calc R U . . . C47_2 C 0.20816(16) 0.71424(11) 0.88536(8) 0.0210(4) Uani 1 1 d . . . . . C48_2 C 0.14140(16) 0.74297(11) 0.85268(9) 0.0224(4) Uani 1 1 d . . . . . C49_2 C 0.15972(19) 0.71428(13) 0.80266(10) 0.0319(5) Uani 1 1 d . . . . . H49_2 H 0.116071 0.733061 0.779945 0.038 Uiso 1 1 calc R U . . . C50_2 C 0.2401(2) 0.65913(14) 0.78565(11) 0.0393(6) Uani 1 1 d . . . . . H50_2 H 0.251396 0.640383 0.751567 0.047 Uiso 1 1 calc R U . . . C51_2 C 0.3036(2) 0.63158(13) 0.81842(11) 0.0365(6) Uani 1 1 d . . . . . H51_2 H 0.358440 0.593569 0.806553 0.044 Uiso 1 1 calc R U . . . C52_2 C 0.28970(18) 0.65792(11) 0.86839(10) 0.0272(5) Uani 1 1 d . . . . . C53_2 C 0.05383(16) 0.80413(11) 0.86947(9) 0.0225(4) Uani 1 1 d . . . . . H53_2 H 0.047370 0.812210 0.908077 0.027 Uiso 1 1 calc R U . . . C54_2 C -0.04048(18) 0.79170(15) 0.86477(11) 0.0382(6) Uani 1 1 d . . . . . H54A_2 H -0.037258 0.785898 0.826947 0.057 Uiso 1 1 calc R U . . . H54B_2 H -0.095361 0.831314 0.878396 0.057 Uiso 1 1 calc R U . . . H54C_2 H -0.049125 0.749954 0.885957 0.057 Uiso 1 1 calc R U . . . C55_2 C 0.06929(19) 0.86894(12) 0.83629(9) 0.0306(5) Uani 1 1 d . . . . . H55A_2 H 0.076024 0.862272 0.798171 0.046 Uiso 1 1 calc R U . . . H55B_2 H 0.128249 0.877383 0.840974 0.046 Uiso 1 1 calc R U . . . H55C_2 H 0.013473 0.908627 0.848494 0.046 Uiso 1 1 calc R U . . . C56_2 C 0.36158(17) 0.62463(12) 0.90332(10) 0.0287(5) Uani 1 1 d . . . . . H56_2 H 0.341933 0.651881 0.936462 0.034 Uiso 1 1 calc R U . . . C57_2 C 0.3592(2) 0.55005(13) 0.92084(13) 0.0470(7) Uani 1 1 d . . . . . H57A_2 H 0.376230 0.522660 0.888898 0.070 Uiso 1 1 calc R U . . . H57B_2 H 0.293941 0.550242 0.941595 0.070 Uiso 1 1 calc R U . . . H57C_2 H 0.405932 0.529822 0.943176 0.070 Uiso 1 1 calc R U . . . C58_2 C 0.46432(19) 0.62609(14) 0.87426(11) 0.0387(6) Uani 1 1 d . . . . . H58A_2 H 0.484020 0.601530 0.840679 0.058 Uiso 1 1 calc R U . . . H58B_2 H 0.509026 0.603635 0.897336 0.058 Uiso 1 1 calc R U . . . H58C_2 H 0.465856 0.674054 0.866118 0.058 Uiso 1 1 calc R U . . . C59_2 C 0.27045(14) 1.01389(10) 0.91389(7) 0.0137(4) Uani 1 1 d . . . . . C60_2 C 0.19134(15) 1.10650(10) 0.96528(8) 0.0181(4) Uani 1 1 d . . . . . C61_2 C 0.27834(15) 1.07734(11) 0.97849(8) 0.0187(4) Uani 1 1 d . . . . . C62_2 C 0.10198(14) 1.07753(11) 0.90373(8) 0.0193(4) Uani 1 1 d . . . . . H62A_2 H 0.096496 1.118233 0.879130 0.029 Uiso 1 1 calc R U . . . H62B_2 H 0.043602 1.084835 0.933130 0.029 Uiso 1 1 calc R U . . . H62C_2 H 0.108835 1.036994 0.884103 0.029 Uiso 1 1 calc R U . . . C63_2 C 0.41860(15) 0.97223(11) 0.95199(8) 0.0208(4) Uani 1 1 d . . . . . H63A_2 H 0.435436 0.933524 0.928416 0.031 Uiso 1 1 calc R U . . . H63B_2 H 0.414036 0.954788 0.989395 0.031 Uiso 1 1 calc R U . . . H63C_2 H 0.468831 0.996442 0.941631 0.031 Uiso 1 1 calc R U . . . C64_2 C 0.11181(17) 1.16894(11) 0.98522(10) 0.0277(5) Uani 1 1 d . . . . . H64A_2 H 0.099662 1.201311 0.954879 0.042 Uiso 1 1 calc R U . . . H64B_2 H 0.130565 1.191049 1.011147 0.042 Uiso 1 1 calc R U . . . H64C_2 H 0.052776 1.155636 1.002784 0.042 Uiso 1 1 calc R U . . . C65_2 C 0.32231(17) 1.09649(13) 1.01822(9) 0.0285(5) Uani 1 1 d . . . . . H65A_2 H 0.382710 1.107283 0.999481 0.043 Uiso 1 1 calc R U . . . H65B_2 H 0.336228 1.057856 1.044150 0.043 Uiso 1 1 calc R U . . . H65C_2 H 0.277030 1.136986 1.037261 0.043 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1_1 0.01318(10) 0.01173(10) 0.01319(10) -0.00033(8) -0.00101(8) -0.00405(8) Ga2_1 0.01601(11) 0.01223(10) 0.01150(10) -0.00087(8) -0.00260(8) -0.00368(8) Cl1_1 0.0197(2) 0.0216(2) 0.0243(3) 0.0014(2) -0.0084(2) -0.0047(2) Cl2_1 0.0217(2) 0.0132(2) 0.0210(2) -0.00106(18) -0.00669(19) -0.00506(18) P1_1 0.0140(2) 0.0133(2) 0.0131(2) 0.00010(18) -0.00266(18) -0.00363(19) P2_1 0.0201(3) 0.0139(2) 0.0146(2) -0.00113(19) -0.0008(2) -0.0070(2) N1_1 0.0125(8) 0.0146(8) 0.0150(8) 0.0007(6) -0.0019(6) -0.0049(6) N2_1 0.0189(9) 0.0143(8) 0.0125(8) -0.0004(6) -0.0024(6) -0.0022(7) N3_1 0.0189(9) 0.0183(8) 0.0156(8) -0.0023(7) -0.0043(7) -0.0078(7) N4_1 0.0192(9) 0.0101(7) 0.0156(8) -0.0002(6) -0.0020(7) -0.0036(6) N5_1 0.0213(9) 0.0148(8) 0.0181(9) -0.0001(7) -0.0060(7) -0.0076(7) N6_1 0.0178(9) 0.0149(8) 0.0179(8) 0.0034(6) -0.0053(7) -0.0057(7) C1_1 0.0125(9) 0.0202(10) 0.0188(10) 0.0046(8) -0.0032(8) -0.0053(8) C2_1 0.0178(10) 0.0269(11) 0.0132(10) 0.0024(8) 0.0020(8) -0.0064(9) C3_1 0.0191(10) 0.0207(10) 0.0140(10) -0.0012(8) -0.0018(8) 0.0001(8) C4_1 0.0183(11) 0.0290(12) 0.0254(12) 0.0046(9) 0.0012(9) -0.0121(9) C5_1 0.0380(14) 0.0275(12) 0.0175(11) -0.0057(9) 0.0063(10) -0.0032(10) C6_1 0.0164(10) 0.0209(10) 0.0161(10) 0.0006(8) -0.0008(8) -0.0120(8) C7_1 0.0199(11) 0.0233(11) 0.0180(10) 0.0035(8) -0.0034(8) -0.0119(9) C8_1 0.0361(14) 0.0348(13) 0.0205(11) 0.0021(10) -0.0101(10) -0.0181(11) C9_1 0.0478(16) 0.0329(13) 0.0213(12) -0.0068(10) -0.0063(11) -0.0188(12) C10_1 0.0326(13) 0.0200(11) 0.0281(12) -0.0033(9) -0.0033(10) -0.0090(10) C11_1 0.0199(10) 0.0170(10) 0.0210(10) 0.0003(8) -0.0015(8) -0.0093(8) C12_1 0.0241(11) 0.0258(11) 0.0220(11) 0.0054(9) -0.0094(9) -0.0118(9) C13_1 0.0233(12) 0.0291(13) 0.0383(14) 0.0100(11) -0.0072(10) -0.0046(10) C14_1 0.0432(15) 0.0333(13) 0.0279(13) 0.0111(10) -0.0166(11) -0.0189(12) C15_1 0.0235(11) 0.0154(10) 0.0268(11) -0.0018(8) -0.0056(9) -0.0064(8) C16_1 0.0481(16) 0.0192(11) 0.0330(13) 0.0038(10) -0.0148(12) -0.0101(11) C17_1 0.0229(12) 0.0277(13) 0.0468(16) -0.0068(11) -0.0090(11) -0.0032(10) C18_1 0.0279(12) 0.0137(9) 0.0143(10) -0.0030(7) -0.0016(8) -0.0012(8) C19_1 0.0325(13) 0.0166(10) 0.0154(10) -0.0018(8) -0.0023(9) 0.0056(9) C20_1 0.0486(16) 0.0151(11) 0.0223(12) 0.0004(9) -0.0047(11) 0.0048(10) C21_1 0.074(2) 0.0151(11) 0.0220(12) -0.0020(9) -0.0052(12) -0.0103(12) C22_1 0.0642(18) 0.0183(11) 0.0233(12) -0.0026(9) -0.0121(12) -0.0150(11) C23_1 0.0426(14) 0.0171(10) 0.0157(10) -0.0020(8) -0.0050(9) -0.0074(10) C24_1 0.0275(12) 0.0264(12) 0.0196(11) 0.0008(9) -0.0037(9) 0.0050(10) C25_1 0.0306(14) 0.066(2) 0.0258(13) -0.0078(13) 0.0018(11) 0.0013(13) C26_1 0.0242(12) 0.0379(14) 0.0220(12) -0.0014(10) -0.0044(9) 0.0028(10) C27_1 0.0437(14) 0.0190(11) 0.0181(11) 0.0013(8) -0.0110(10) -0.0134(10) C28_1 0.076(2) 0.0296(13) 0.0230(13) 0.0008(10) -0.0204(13) -0.0165(14) C29_1 0.0483(16) 0.0327(14) 0.0355(14) 0.0084(11) -0.0178(12) -0.0210(12) C30_1 0.0295(12) 0.0192(10) 0.0154(10) -0.0028(8) -0.0058(8) -0.0096(9) C31_1 0.0279(12) 0.0231(11) 0.0112(9) -0.0012(8) 0.0000(8) -0.0103(9) C32_1 0.0221(11) 0.0108(9) 0.0179(10) -0.0035(7) 0.0017(8) -0.0068(8) C33_1 0.0359(14) 0.0418(14) 0.0153(11) 0.0018(10) -0.0071(9) -0.0165(11) C34_1 0.0257(12) 0.0225(11) 0.0188(11) -0.0022(8) 0.0034(9) -0.0072(9) C35_1 0.0248(11) 0.0258(11) 0.0135(10) 0.0001(8) -0.0071(8) -0.0114(9) C36_1 0.0248(11) 0.0251(11) 0.0164(10) 0.0038(8) -0.0093(8) -0.0112(9) C37_1 0.0237(12) 0.0330(13) 0.0287(12) 0.0027(10) -0.0120(10) -0.0090(10) C38_1 0.0288(13) 0.0443(15) 0.0419(15) 0.0007(12) -0.0197(11) -0.0185(12) C39_1 0.0400(15) 0.0354(14) 0.0359(14) -0.0030(11) -0.0180(12) -0.0207(12) C40_1 0.0345(13) 0.0260(11) 0.0193(11) -0.0019(9) -0.0104(9) -0.0147(10) C41_1 0.0211(11) 0.0208(10) 0.0225(11) 0.0020(8) -0.0085(9) -0.0071(9) C42_1 0.0286(13) 0.0255(12) 0.0308(13) -0.0025(10) -0.0063(10) -0.0097(10) C43_1 0.0299(13) 0.0289(13) 0.0391(14) 0.0105(11) -0.0155(11) -0.0102(10) C44_1 0.0369(14) 0.0239(12) 0.0309(13) -0.0049(10) -0.0104(10) -0.0130(10) C45_1 0.0410(16) 0.0324(15) 0.062(2) 0.0108(13) -0.0081(14) -0.0122(12) C46_1 0.086(3) 0.0477(19) 0.0464(19) -0.0222(15) -0.0268(18) 0.0047(17) C47_1 0.0154(10) 0.0136(9) 0.0162(10) -0.0004(7) 0.0013(7) -0.0002(7) C48_1 0.0160(10) 0.0164(10) 0.0209(10) 0.0008(8) -0.0002(8) -0.0009(8) C49_1 0.0190(11) 0.0256(12) 0.0285(12) -0.0011(9) -0.0048(9) -0.0041(9) C50_1 0.0232(12) 0.0234(11) 0.0320(13) 0.0053(10) -0.0082(10) 0.0027(9) C51_1 0.0281(12) 0.0148(10) 0.0270(12) 0.0038(9) -0.0023(9) 0.0003(9) C52_1 0.0194(10) 0.0132(9) 0.0188(10) -0.0011(8) 0.0023(8) -0.0017(8) C53_1 0.0189(10) 0.0181(10) 0.0225(11) 0.0018(8) -0.0058(8) -0.0066(8) C54_1 0.0280(12) 0.0210(11) 0.0276(12) -0.0009(9) -0.0105(9) -0.0077(9) C55_1 0.0279(13) 0.0306(13) 0.0339(13) 0.0035(10) -0.0039(10) -0.0154(10) C56_1 0.0226(11) 0.0128(10) 0.0253(11) -0.0031(8) 0.0048(9) -0.0044(8) C57_1 0.0376(15) 0.0223(12) 0.0431(15) 0.0074(11) -0.0023(12) -0.0131(11) C58_1 0.0318(13) 0.0245(12) 0.0344(13) -0.0152(10) 0.0095(10) -0.0112(10) C59_1 0.0174(10) 0.0133(9) 0.0134(9) 0.0012(7) -0.0041(7) -0.0052(7) C60_1 0.0232(11) 0.0241(11) 0.0173(10) 0.0021(8) -0.0061(8) -0.0128(9) C61_1 0.0201(11) 0.0251(11) 0.0165(10) 0.0039(8) -0.0064(8) -0.0104(9) C62_1 0.0272(12) 0.0125(10) 0.0270(12) -0.0002(8) -0.0079(9) -0.0033(8) C63_1 0.0160(10) 0.0163(10) 0.0255(11) 0.0018(8) -0.0041(8) -0.0009(8) C64_1 0.0401(14) 0.0303(13) 0.0287(13) 0.0006(10) -0.0114(11) -0.0223(11) C65_1 0.0261(12) 0.0384(14) 0.0335(13) 0.0121(11) -0.0157(10) -0.0152(11) Ga1_2 0.01134(10) 0.01259(10) 0.01020(10) -0.00022(8) -0.00091(8) -0.00239(8) Ga2_2 0.01577(11) 0.01437(10) 0.01166(10) 0.00057(8) -0.00285(8) -0.00549(8) Cl1_2 0.0275(3) 0.0243(3) 0.0241(3) -0.0030(2) -0.0078(2) -0.0071(2) Cl2_2 0.0164(2) 0.0188(2) 0.0185(2) 0.00000(18) -0.00276(18) -0.00386(18) P1_2 0.0137(2) 0.0154(2) 0.0103(2) -0.00040(18) -0.00188(18) -0.00507(19) P2_2 0.0162(3) 0.0157(2) 0.0159(2) 0.00094(19) -0.0002(2) -0.0034(2) N1_2 0.0107(8) 0.0137(8) 0.0133(8) -0.0001(6) -0.0016(6) -0.0029(6) N2_2 0.0140(8) 0.0120(8) 0.0135(8) -0.0018(6) -0.0014(6) -0.0011(6) N3_2 0.0177(9) 0.0193(9) 0.0126(8) 0.0015(6) -0.0031(6) -0.0062(7) N4_2 0.0208(9) 0.0167(8) 0.0166(8) 0.0005(7) -0.0059(7) -0.0072(7) N5_2 0.0141(8) 0.0170(8) 0.0132(8) -0.0001(6) 0.0002(6) -0.0050(7) N6_2 0.0155(8) 0.0195(8) 0.0123(8) -0.0018(6) -0.0018(6) -0.0074(7) C1_2 0.0159(10) 0.0170(9) 0.0134(9) 0.0018(7) -0.0043(7) -0.0071(8) C2_2 0.0156(10) 0.0229(10) 0.0120(9) 0.0015(8) 0.0022(7) -0.0064(8) C3_2 0.0147(10) 0.0215(10) 0.0133(9) -0.0039(8) -0.0011(7) -0.0041(8) C4_2 0.0199(11) 0.0199(10) 0.0179(10) 0.0048(8) -0.0025(8) -0.0047(8) C5_2 0.0213(11) 0.0253(11) 0.0149(10) -0.0019(8) 0.0034(8) 0.0014(9) C6_2 0.0121(9) 0.0152(9) 0.0134(9) 0.0050(7) -0.0026(7) -0.0031(7) C7_2 0.0166(10) 0.0163(9) 0.0155(9) 0.0032(7) -0.0054(8) -0.0044(8) C8_2 0.0133(10) 0.0228(10) 0.0197(10) 0.0055(8) -0.0070(8) -0.0060(8) C9_2 0.0110(9) 0.0213(10) 0.0228(11) 0.0041(8) -0.0027(8) -0.0005(8) C10_2 0.0165(10) 0.0159(10) 0.0190(10) -0.0009(8) -0.0018(8) -0.0038(8) C11_2 0.0133(9) 0.0165(9) 0.0141(9) 0.0040(7) -0.0028(7) -0.0052(7) C12_2 0.0180(11) 0.0212(11) 0.0277(12) -0.0028(9) -0.0115(9) -0.0037(8) C13_2 0.0438(15) 0.0235(12) 0.0271(12) 0.0041(9) -0.0137(11) -0.0161(11) C14_2 0.0428(15) 0.0391(14) 0.0217(12) -0.0023(10) -0.0029(10) -0.0231(12) C15_2 0.0127(9) 0.0163(9) 0.0196(10) -0.0009(8) -0.0024(8) -0.0039(8) C16_2 0.0192(11) 0.0268(11) 0.0222(11) -0.0033(9) -0.0042(8) -0.0067(9) C17_2 0.0218(11) 0.0189(11) 0.0355(13) 0.0024(9) -0.0061(9) -0.0085(9) C18_2 0.0179(10) 0.0148(9) 0.0115(9) -0.0036(7) 0.0017(7) 0.0002(8) C19_2 0.0239(11) 0.0172(10) 0.0185(10) -0.0056(8) -0.0024(8) -0.0020(8) C20_2 0.0317(13) 0.0182(11) 0.0230(11) -0.0056(9) 0.0011(9) -0.0054(9) C21_2 0.0293(12) 0.0163(10) 0.0242(11) -0.0008(9) 0.0021(9) -0.0003(9) C22_2 0.0196(11) 0.0215(11) 0.0211(11) 0.0008(8) -0.0009(8) 0.0023(9) C23_2 0.0198(10) 0.0185(10) 0.0128(9) -0.0023(8) 0.0010(8) -0.0009(8) C24_2 0.0362(14) 0.0231(11) 0.0315(13) -0.0027(10) -0.0156(11) -0.0111(10) C25_2 0.0342(14) 0.0405(15) 0.0331(14) -0.0068(11) -0.0093(11) -0.0140(12) C26_2 0.068(2) 0.065(2) 0.0342(15) 0.0102(14) -0.0241(15) -0.0419(17) C27_2 0.0180(10) 0.0203(10) 0.0214(11) -0.0008(8) -0.0066(8) 0.0005(8) C28_2 0.0322(13) 0.0311(13) 0.0224(12) -0.0015(10) -0.0115(10) -0.0010(10) C29_2 0.0188(11) 0.0254(12) 0.0303(12) 0.0029(9) -0.0053(9) -0.0020(9) C30_2 0.0206(11) 0.0166(10) 0.0172(10) 0.0030(8) -0.0034(8) -0.0030(8) C31_2 0.0206(11) 0.0236(11) 0.0186(10) 0.0039(8) -0.0016(8) -0.0107(9) C32_2 0.0190(11) 0.0166(10) 0.0246(11) 0.0007(8) -0.0053(8) -0.0053(8) C33_2 0.0336(13) 0.0283(12) 0.0183(11) 0.0078(9) -0.0074(9) -0.0144(10) C34_2 0.0334(13) 0.0288(12) 0.0298(13) 0.0014(10) -0.0075(10) -0.0197(10) C35_2 0.0197(10) 0.0221(10) 0.0121(9) 0.0043(8) -0.0056(8) -0.0075(8) C36_2 0.0233(11) 0.0237(11) 0.0124(9) 0.0052(8) -0.0056(8) -0.0096(9) C37_2 0.0323(13) 0.0310(12) 0.0182(11) 0.0027(9) -0.0114(9) -0.0141(10) C38_2 0.0306(13) 0.0385(14) 0.0282(12) 0.0047(10) -0.0170(10) -0.0155(11) C39_2 0.0205(11) 0.0387(14) 0.0259(12) 0.0054(10) -0.0121(9) -0.0096(10) C40_2 0.0232(11) 0.0260(11) 0.0173(10) 0.0061(8) -0.0063(8) -0.0078(9) C41_2 0.0231(11) 0.0221(10) 0.0123(9) -0.0015(8) -0.0015(8) -0.0096(9) C42_2 0.0377(14) 0.0382(14) 0.0171(11) -0.0015(10) 0.0015(10) -0.0134(11) C43_2 0.0271(12) 0.0245(11) 0.0216(11) 0.0008(9) -0.0050(9) -0.0100(9) C44_2 0.0220(11) 0.0273(12) 0.0216(11) 0.0026(9) -0.0062(9) -0.0044(9) C45_2 0.0518(18) 0.0275(13) 0.0325(14) 0.0042(11) -0.0074(12) 0.0009(12) C46_2 0.0241(13) 0.0488(16) 0.0336(14) -0.0046(12) -0.0030(10) -0.0040(11) C47_2 0.0274(12) 0.0196(10) 0.0196(10) -0.0020(8) -0.0063(9) -0.0108(9) C48_2 0.0263(12) 0.0236(11) 0.0216(11) -0.0020(9) -0.0074(9) -0.0117(9) C49_2 0.0408(15) 0.0335(13) 0.0285(13) -0.0069(10) -0.0131(11) -0.0150(11) C50_2 0.0529(18) 0.0364(14) 0.0334(14) -0.0188(12) -0.0123(13) -0.0115(13) C51_2 0.0455(16) 0.0259(13) 0.0367(14) -0.0150(11) -0.0090(12) -0.0036(11) C52_2 0.0327(13) 0.0196(11) 0.0295(12) -0.0041(9) -0.0076(10) -0.0062(9) C53_2 0.0212(11) 0.0284(12) 0.0210(11) -0.0015(9) -0.0086(9) -0.0081(9) C54_2 0.0289(14) 0.0562(18) 0.0358(15) 0.0026(13) -0.0137(11) -0.0178(13) C55_2 0.0356(14) 0.0293(13) 0.0245(12) -0.0009(10) -0.0065(10) -0.0061(10) C56_2 0.0308(13) 0.0219(11) 0.0303(13) -0.0026(9) -0.0067(10) -0.0024(10) C57_2 0.0472(18) 0.0299(14) 0.060(2) 0.0097(13) -0.0134(15) -0.0077(13) C58_2 0.0365(15) 0.0401(15) 0.0355(15) -0.0015(12) -0.0067(12) -0.0064(12) C59_2 0.0131(9) 0.0168(9) 0.0108(9) 0.0010(7) -0.0005(7) -0.0060(7) C60_2 0.0214(11) 0.0174(10) 0.0140(9) -0.0018(8) 0.0039(8) -0.0094(8) C61_2 0.0226(11) 0.0231(11) 0.0121(9) -0.0028(8) 0.0000(8) -0.0118(9) C62_2 0.0139(10) 0.0206(10) 0.0202(10) 0.0014(8) -0.0030(8) -0.0018(8) C63_2 0.0167(10) 0.0271(11) 0.0194(10) 0.0010(8) -0.0078(8) -0.0052(9) C64_2 0.0261(12) 0.0225(11) 0.0307(13) -0.0075(9) 0.0046(10) -0.0083(9) C65_2 0.0304(13) 0.0397(14) 0.0216(11) -0.0096(10) -0.0028(9) -0.0188(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1_1 N1_1 1.9506(16) . ? Ga1_1 N2_1 1.9722(17) . ? Ga1_1 Cl1_1 2.2249(6) . ? Ga1_1 P1_1 2.3328(7) . ? Ga2_1 N3_1 1.9851(17) . ? Ga2_1 N4_1 2.0167(17) . ? Ga2_1 Cl2_1 2.2590(7) . ? Ga2_1 P2_1 2.2747(6) . ? P1_1 C59_1 1.862(2) . ? P1_1 P2_1 2.1871(8) . ? N1_1 C1_1 1.340(3) . ? N1_1 C6_1 1.455(3) . ? N2_1 C3_1 1.332(3) . ? N2_1 C18_1 1.454(3) . ? N3_1 C30_1 1.339(3) . ? N3_1 C35_1 1.450(3) . ? N4_1 C32_1 1.329(3) . ? N4_1 C47_1 1.444(2) . ? N5_1 C59_1 1.354(2) . ? N5_1 C60_1 1.389(3) . ? N5_1 C62_1 1.471(3) . ? N6_1 C59_1 1.359(2) . ? N6_1 C61_1 1.386(3) . ? N6_1 C63_1 1.469(3) . ? C1_1 C2_1 1.409(3) . ? C1_1 C4_1 1.511(3) . ? C2_1 C3_1 1.394(3) . ? C3_1 C5_1 1.520(3) . ? C6_1 C11_1 1.405(3) . ? C6_1 C7_1 1.412(3) . ? C7_1 C8_1 1.398(3) . ? C7_1 C12_1 1.519(3) . ? C8_1 C9_1 1.385(3) . ? C9_1 C10_1 1.378(3) . ? C10_1 C11_1 1.394(3) . ? C11_1 C15_1 1.518(3) . ? C12_1 C13_1 1.529(3) . ? C12_1 C14_1 1.537(3) . ? C15_1 C16_1 1.538(3) . ? C15_1 C17_1 1.540(3) . ? C18_1 C23_1 1.406(3) . ? C18_1 C19_1 1.410(3) . ? C19_1 C20_1 1.396(3) . ? C19_1 C24_1 1.517(3) . ? C20_1 C21_1 1.372(4) . ? C21_1 C22_1 1.382(3) . ? C22_1 C23_1 1.398(3) . ? C23_1 C27_1 1.532(3) . ? C24_1 C26_1 1.529(3) . ? C24_1 C25_1 1.532(3) . ? C27_1 C29_1 1.520(4) . ? C27_1 C28_1 1.546(3) . ? C30_1 C31_1 1.394(3) . ? C30_1 C33_1 1.521(3) . ? C31_1 C32_1 1.416(3) . ? C32_1 C34_1 1.510(3) . ? C35_1 C36_1 1.404(3) . ? C35_1 C40_1 1.411(3) . ? C36_1 C37_1 1.392(3) . ? C36_1 C41_1 1.528(3) . ? C37_1 C38_1 1.382(3) . ? C38_1 C39_1 1.374(4) . ? C39_1 C40_1 1.400(3) . ? C40_1 C44_1 1.517(3) . ? C41_1 C42_1 1.527(3) . ? C41_1 C43_1 1.537(3) . ? C44_1 C45_1 1.517(3) . ? C44_1 C46_1 1.541(4) . ? C47_1 C48_1 1.404(3) . ? C47_1 C52_1 1.421(3) . ? C48_1 C49_1 1.403(3) . ? C48_1 C53_1 1.525(3) . ? C49_1 C50_1 1.387(3) . ? C50_1 C51_1 1.375(3) . ? C51_1 C52_1 1.394(3) . ? C52_1 C56_1 1.525(3) . ? C53_1 C54_1 1.536(3) . ? C53_1 C55_1 1.538(3) . ? C56_1 C57_1 1.531(3) . ? C56_1 C58_1 1.535(3) . ? C60_1 C61_1 1.358(3) . ? C60_1 C64_1 1.491(3) . ? C61_1 C65_1 1.496(3) . ? Ga1_2 N2_2 1.9551(16) . ? Ga1_2 N1_2 1.9714(15) . ? Ga1_2 Cl1_2 2.2113(6) . ? Ga1_2 P1_2 2.3433(6) . ? Ga2_2 N4_2 2.0023(17) . ? Ga2_2 N3_2 2.0113(16) . ? Ga2_2 Cl2_2 2.2579(6) . ? Ga2_2 P2_2 2.2695(7) . ? P1_2 C59_2 1.864(2) . ? P1_2 P2_2 2.1835(8) . ? N1_2 C1_2 1.341(2) . ? N1_2 C6_2 1.446(2) . ? N2_2 C3_2 1.331(2) . ? N2_2 C18_2 1.455(2) . ? N3_2 C30_2 1.329(3) . ? N3_2 C35_2 1.447(3) . ? N4_2 C32_2 1.341(3) . ? N4_2 C47_2 1.448(3) . ? N5_2 C59_2 1.358(2) . ? N5_2 C60_2 1.391(3) . ? N5_2 C62_2 1.470(3) . ? N6_2 C59_2 1.351(2) . ? N6_2 C61_2 1.394(3) . ? N6_2 C63_2 1.466(3) . ? C1_2 C2_2 1.391(3) . ? C1_2 C4_2 1.508(3) . ? C2_2 C3_2 1.410(3) . ? C3_2 C5_2 1.506(3) . ? C6_2 C7_2 1.410(3) . ? C6_2 C11_2 1.410(3) . ? C7_2 C8_2 1.396(3) . ? C7_2 C12_2 1.531(3) . ? C8_2 C9_2 1.388(3) . ? C9_2 C10_2 1.386(3) . ? C10_2 C11_2 1.399(3) . ? C11_2 C15_2 1.521(3) . ? C12_2 C13_2 1.525(3) . ? C12_2 C14_2 1.531(3) . ? C15_2 C16_2 1.528(3) . ? C15_2 C17_2 1.539(3) . ? C18_2 C23_2 1.408(3) . ? C18_2 C19_2 1.411(3) . ? C19_2 C20_2 1.394(3) . ? C19_2 C24_2 1.530(3) . ? C20_2 C21_2 1.390(3) . ? C21_2 C22_2 1.366(3) . ? C22_2 C23_2 1.394(3) . ? C23_2 C27_2 1.519(3) . ? C24_2 C26_2 1.510(4) . ? C24_2 C25_2 1.518(3) . ? C27_2 C28_2 1.538(3) . ? C27_2 C29_2 1.543(3) . ? C30_2 C31_2 1.408(3) . ? C30_2 C33_2 1.520(3) . ? C31_2 C32_2 1.397(3) . ? C32_2 C34_2 1.519(3) . ? C35_2 C36_2 1.409(3) . ? C35_2 C40_2 1.415(3) . ? C36_2 C37_2 1.400(3) . ? C36_2 C41_2 1.522(3) . ? C37_2 C38_2 1.385(3) . ? C38_2 C39_2 1.384(3) . ? C39_2 C40_2 1.399(3) . ? C40_2 C44_2 1.522(3) . ? C41_2 C43_2 1.531(3) . ? C41_2 C42_2 1.535(3) . ? C44_2 C46_2 1.527(3) . ? C44_2 C45_2 1.537(3) . ? C47_2 C52_2 1.407(3) . ? C47_2 C48_2 1.414(3) . ? C48_2 C49_2 1.401(3) . ? C48_2 C53_2 1.513(3) . ? C49_2 C50_2 1.384(4) . ? C50_2 C51_2 1.378(4) . ? C51_2 C52_2 1.390(3) . ? C52_2 C56_2 1.525(3) . ? C53_2 C54_2 1.532(3) . ? C53_2 C55_2 1.532(3) . ? C56_2 C58_2 1.527(4) . ? C56_2 C57_2 1.541(3) . ? C60_2 C61_2 1.363(3) . ? C60_2 C64_2 1.486(3) . ? C61_2 C65_2 1.484(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1_1 Ga1_1 N2_1 96.53(7) . . ? N1_1 Ga1_1 Cl1_1 101.43(5) . . ? N2_1 Ga1_1 Cl1_1 97.97(5) . . ? N1_1 Ga1_1 P1_1 120.93(5) . . ? N2_1 Ga1_1 P1_1 116.64(5) . . ? Cl1_1 Ga1_1 P1_1 118.81(2) . . ? N3_1 Ga2_1 N4_1 92.72(7) . . ? N3_1 Ga2_1 Cl2_1 101.85(5) . . ? N4_1 Ga2_1 Cl2_1 98.33(5) . . ? N3_1 Ga2_1 P2_1 121.02(5) . . ? N4_1 Ga2_1 P2_1 118.33(5) . . ? Cl2_1 Ga2_1 P2_1 119.33(2) . . ? C59_1 P1_1 P2_1 110.67(7) . . ? C59_1 P1_1 Ga1_1 95.21(6) . . ? P2_1 P1_1 Ga1_1 103.70(3) . . ? P1_1 P2_1 Ga2_1 95.93(3) . . ? C1_1 N1_1 C6_1 118.35(16) . . ? C1_1 N1_1 Ga1_1 117.85(14) . . ? C6_1 N1_1 Ga1_1 123.10(12) . . ? C3_1 N2_1 C18_1 120.12(17) . . ? C3_1 N2_1 Ga1_1 118.60(14) . . ? C18_1 N2_1 Ga1_1 121.26(13) . . ? C30_1 N3_1 C35_1 117.05(17) . . ? C30_1 N3_1 Ga2_1 121.34(14) . . ? C35_1 N3_1 Ga2_1 121.52(13) . . ? C32_1 N4_1 C47_1 119.10(17) . . ? C32_1 N4_1 Ga2_1 121.84(14) . . ? C47_1 N4_1 Ga2_1 118.78(12) . . ? C59_1 N5_1 C60_1 110.94(16) . . ? C59_1 N5_1 C62_1 125.33(17) . . ? C60_1 N5_1 C62_1 123.50(17) . . ? C59_1 N6_1 C61_1 110.30(16) . . ? C59_1 N6_1 C63_1 126.29(17) . . ? C61_1 N6_1 C63_1 123.36(17) . . ? N1_1 C1_1 C2_1 123.76(19) . . ? N1_1 C1_1 C4_1 119.59(19) . . ? C2_1 C1_1 C4_1 116.63(18) . . ? C3_1 C2_1 C1_1 128.46(19) . . ? N2_1 C3_1 C2_1 123.81(19) . . ? N2_1 C3_1 C5_1 119.63(19) . . ? C2_1 C3_1 C5_1 116.56(19) . . ? C11_1 C6_1 C7_1 121.61(19) . . ? C11_1 C6_1 N1_1 120.32(17) . . ? C7_1 C6_1 N1_1 118.04(18) . . ? C8_1 C7_1 C6_1 117.3(2) . . ? C8_1 C7_1 C12_1 121.17(19) . . ? C6_1 C7_1 C12_1 121.48(19) . . ? C9_1 C8_1 C7_1 121.7(2) . . ? C10_1 C9_1 C8_1 119.8(2) . . ? C9_1 C10_1 C11_1 121.4(2) . . ? C10_1 C11_1 C6_1 118.09(19) . . ? C10_1 C11_1 C15_1 118.57(19) . . ? C6_1 C11_1 C15_1 123.31(18) . . ? C7_1 C12_1 C13_1 112.40(18) . . ? C7_1 C12_1 C14_1 112.25(19) . . ? C13_1 C12_1 C14_1 110.01(19) . . ? C11_1 C15_1 C16_1 112.49(18) . . ? C11_1 C15_1 C17_1 109.44(19) . . ? C16_1 C15_1 C17_1 109.53(19) . . ? C23_1 C18_1 C19_1 121.1(2) . . ? C23_1 C18_1 N2_1 121.03(18) . . ? C19_1 C18_1 N2_1 117.88(19) . . ? C20_1 C19_1 C18_1 118.1(2) . . ? C20_1 C19_1 C24_1 120.0(2) . . ? C18_1 C19_1 C24_1 121.8(2) . . ? C21_1 C20_1 C19_1 121.3(2) . . ? C20_1 C21_1 C22_1 120.2(2) . . ? C21_1 C22_1 C23_1 121.1(2) . . ? C22_1 C23_1 C18_1 118.0(2) . . ? C22_1 C23_1 C27_1 119.0(2) . . ? C18_1 C23_1 C27_1 122.94(19) . . ? C19_1 C24_1 C26_1 110.8(2) . . ? C19_1 C24_1 C25_1 111.1(2) . . ? C26_1 C24_1 C25_1 110.75(19) . . ? C29_1 C27_1 C23_1 111.96(19) . . ? C29_1 C27_1 C28_1 110.0(2) . . ? C23_1 C27_1 C28_1 110.35(19) . . ? N3_1 C30_1 C31_1 123.67(19) . . ? N3_1 C30_1 C33_1 119.1(2) . . ? C31_1 C30_1 C33_1 117.14(19) . . ? C30_1 C31_1 C32_1 128.05(19) . . ? N4_1 C32_1 C31_1 123.17(19) . . ? N4_1 C32_1 C34_1 121.04(18) . . ? C31_1 C32_1 C34_1 115.77(18) . . ? C36_1 C35_1 C40_1 121.1(2) . . ? C36_1 C35_1 N3_1 120.39(18) . . ? C40_1 C35_1 N3_1 118.50(19) . . ? C37_1 C36_1 C35_1 118.1(2) . . ? C37_1 C36_1 C41_1 120.2(2) . . ? C35_1 C36_1 C41_1 121.66(19) . . ? C38_1 C37_1 C36_1 121.6(2) . . ? C39_1 C38_1 C37_1 119.7(2) . . ? C38_1 C39_1 C40_1 121.3(2) . . ? C39_1 C40_1 C35_1 118.0(2) . . ? C39_1 C40_1 C44_1 119.8(2) . . ? C35_1 C40_1 C44_1 122.1(2) . . ? C42_1 C41_1 C36_1 109.83(18) . . ? C42_1 C41_1 C43_1 109.85(19) . . ? C36_1 C41_1 C43_1 113.17(18) . . ? C40_1 C44_1 C45_1 111.2(2) . . ? C40_1 C44_1 C46_1 112.5(2) . . ? C45_1 C44_1 C46_1 110.9(2) . . ? C48_1 C47_1 C52_1 121.47(18) . . ? C48_1 C47_1 N4_1 120.57(17) . . ? C52_1 C47_1 N4_1 117.95(18) . . ? C49_1 C48_1 C47_1 117.84(19) . . ? C49_1 C48_1 C53_1 118.81(19) . . ? C47_1 C48_1 C53_1 123.34(18) . . ? C50_1 C49_1 C48_1 121.2(2) . . ? C51_1 C50_1 C49_1 120.1(2) . . ? C50_1 C51_1 C52_1 121.6(2) . . ? C51_1 C52_1 C47_1 117.7(2) . . ? C51_1 C52_1 C56_1 121.06(19) . . ? C47_1 C52_1 C56_1 121.18(18) . . ? C48_1 C53_1 C54_1 110.05(17) . . ? C48_1 C53_1 C55_1 112.86(18) . . ? C54_1 C53_1 C55_1 109.63(18) . . ? C52_1 C56_1 C57_1 113.37(19) . . ? C52_1 C56_1 C58_1 110.81(18) . . ? C57_1 C56_1 C58_1 110.00(19) . . ? N5_1 C59_1 N6_1 105.30(16) . . ? N5_1 C59_1 P1_1 121.56(14) . . ? N6_1 C59_1 P1_1 133.13(15) . . ? C61_1 C60_1 N5_1 106.21(18) . . ? C61_1 C60_1 C64_1 131.6(2) . . ? N5_1 C60_1 C64_1 122.17(19) . . ? C60_1 C61_1 N6_1 107.21(18) . . ? C60_1 C61_1 C65_1 130.4(2) . . ? N6_1 C61_1 C65_1 122.39(19) . . ? N2_2 Ga1_2 N1_2 96.77(7) . . ? N2_2 Ga1_2 Cl1_2 99.52(5) . . ? N1_2 Ga1_2 Cl1_2 99.49(5) . . ? N2_2 Ga1_2 P1_2 121.58(5) . . ? N1_2 Ga1_2 P1_2 115.92(5) . . ? Cl1_2 Ga1_2 P1_2 119.10(2) . . ? N4_2 Ga2_2 N3_2 92.39(7) . . ? N4_2 Ga2_2 Cl2_2 101.06(5) . . ? N3_2 Ga2_2 Cl2_2 99.84(5) . . ? N4_2 Ga2_2 P2_2 123.21(5) . . ? N3_2 Ga2_2 P2_2 115.96(5) . . ? Cl2_2 Ga2_2 P2_2 119.08(2) . . ? C59_2 P1_2 P2_2 109.99(6) . . ? C59_2 P1_2 Ga1_2 93.53(6) . . ? P2_2 P1_2 Ga1_2 105.42(3) . . ? P1_2 P2_2 Ga2_2 96.41(3) . . ? C1_2 N1_2 C6_2 119.04(15) . . ? C1_2 N1_2 Ga1_2 119.07(13) . . ? C6_2 N1_2 Ga1_2 121.86(12) . . ? C3_2 N2_2 C18_2 120.94(16) . . ? C3_2 N2_2 Ga1_2 119.18(13) . . ? C18_2 N2_2 Ga1_2 119.49(12) . . ? C30_2 N3_2 C35_2 118.78(16) . . ? C30_2 N3_2 Ga2_2 121.62(14) . . ? C35_2 N3_2 Ga2_2 119.29(12) . . ? C32_2 N4_2 C47_2 117.49(17) . . ? C32_2 N4_2 Ga2_2 120.93(14) . . ? C47_2 N4_2 Ga2_2 121.52(13) . . ? C59_2 N5_2 C60_2 110.63(16) . . ? C59_2 N5_2 C62_2 125.57(17) . . ? C60_2 N5_2 C62_2 123.68(17) . . ? C59_2 N6_2 C61_2 110.79(16) . . ? C59_2 N6_2 C63_2 126.31(17) . . ? C61_2 N6_2 C63_2 122.82(16) . . ? N1_2 C1_2 C2_2 123.83(17) . . ? N1_2 C1_2 C4_2 119.54(17) . . ? C2_2 C1_2 C4_2 116.60(17) . . ? C1_2 C2_2 C3_2 128.75(18) . . ? N2_2 C3_2 C2_2 124.16(18) . . ? N2_2 C3_2 C5_2 120.09(18) . . ? C2_2 C3_2 C5_2 115.74(18) . . ? C7_2 C6_2 C11_2 121.37(17) . . ? C7_2 C6_2 N1_2 118.01(17) . . ? C11_2 C6_2 N1_2 120.61(17) . . ? C8_2 C7_2 C6_2 118.35(19) . . ? C8_2 C7_2 C12_2 119.68(18) . . ? C6_2 C7_2 C12_2 121.94(17) . . ? C9_2 C8_2 C7_2 121.06(19) . . ? C10_2 C9_2 C8_2 119.90(19) . . ? C9_2 C10_2 C11_2 121.42(19) . . ? C10_2 C11_2 C6_2 117.88(18) . . ? C10_2 C11_2 C15_2 119.10(18) . . ? C6_2 C11_2 C15_2 122.98(17) . . ? C13_2 C12_2 C7_2 111.80(19) . . ? C13_2 C12_2 C14_2 110.75(18) . . ? C7_2 C12_2 C14_2 111.21(18) . . ? C11_2 C15_2 C16_2 111.79(17) . . ? C11_2 C15_2 C17_2 111.79(16) . . ? C16_2 C15_2 C17_2 109.59(17) . . ? C23_2 C18_2 C19_2 121.30(18) . . ? C23_2 C18_2 N2_2 120.46(18) . . ? C19_2 C18_2 N2_2 118.10(17) . . ? C20_2 C19_2 C18_2 118.3(2) . . ? C20_2 C19_2 C24_2 120.5(2) . . ? C18_2 C19_2 C24_2 121.13(18) . . ? C21_2 C20_2 C19_2 120.5(2) . . ? C22_2 C21_2 C20_2 120.4(2) . . ? C21_2 C22_2 C23_2 121.8(2) . . ? C22_2 C23_2 C18_2 117.7(2) . . ? C22_2 C23_2 C27_2 118.17(19) . . ? C18_2 C23_2 C27_2 124.15(18) . . ? C26_2 C24_2 C25_2 110.4(2) . . ? C26_2 C24_2 C19_2 112.3(2) . . ? C25_2 C24_2 C19_2 113.93(19) . . ? C23_2 C27_2 C28_2 111.28(18) . . ? C23_2 C27_2 C29_2 111.27(18) . . ? C28_2 C27_2 C29_2 109.13(18) . . ? N3_2 C30_2 C31_2 123.55(19) . . ? N3_2 C30_2 C33_2 120.11(19) . . ? C31_2 C30_2 C33_2 116.30(18) . . ? C32_2 C31_2 C30_2 128.08(19) . . ? N4_2 C32_2 C31_2 123.35(19) . . ? N4_2 C32_2 C34_2 119.55(19) . . ? C31_2 C32_2 C34_2 117.06(19) . . ? C36_2 C35_2 C40_2 121.87(19) . . ? C36_2 C35_2 N3_2 120.27(18) . . ? C40_2 C35_2 N3_2 117.86(18) . . ? C37_2 C36_2 C35_2 117.8(2) . . ? C37_2 C36_2 C41_2 119.20(19) . . ? C35_2 C36_2 C41_2 122.97(18) . . ? C38_2 C37_2 C36_2 121.3(2) . . ? C39_2 C38_2 C37_2 120.0(2) . . ? C38_2 C39_2 C40_2 121.6(2) . . ? C39_2 C40_2 C35_2 117.4(2) . . ? C39_2 C40_2 C44_2 120.1(2) . . ? C35_2 C40_2 C44_2 122.39(19) . . ? C36_2 C41_2 C43_2 110.12(17) . . ? C36_2 C41_2 C42_2 112.63(18) . . ? C43_2 C41_2 C42_2 109.43(18) . . ? C40_2 C44_2 C46_2 113.2(2) . . ? C40_2 C44_2 C45_2 110.48(19) . . ? C46_2 C44_2 C45_2 111.2(2) . . ? C52_2 C47_2 C48_2 120.9(2) . . ? C52_2 C47_2 N4_2 118.70(19) . . ? C48_2 C47_2 N4_2 120.40(19) . . ? C49_2 C48_2 C47_2 118.0(2) . . ? C49_2 C48_2 C53_2 119.9(2) . . ? C47_2 C48_2 C53_2 122.13(19) . . ? C50_2 C49_2 C48_2 121.4(2) . . ? C51_2 C50_2 C49_2 119.6(2) . . ? C50_2 C51_2 C52_2 121.8(2) . . ? C51_2 C52_2 C47_2 118.4(2) . . ? C51_2 C52_2 C56_2 119.4(2) . . ? C47_2 C52_2 C56_2 122.1(2) . . ? C48_2 C53_2 C54_2 112.6(2) . . ? C48_2 C53_2 C55_2 110.07(19) . . ? C54_2 C53_2 C55_2 110.41(19) . . ? C52_2 C56_2 C58_2 111.3(2) . . ? C52_2 C56_2 C57_2 111.0(2) . . ? C58_2 C56_2 C57_2 110.4(2) . . ? N6_2 C59_2 N5_2 105.46(16) . . ? N6_2 C59_2 P1_2 133.01(15) . . ? N5_2 C59_2 P1_2 121.53(14) . . ? C61_2 C60_2 N5_2 106.60(17) . . ? C61_2 C60_2 C64_2 130.8(2) . . ? N5_2 C60_2 C64_2 122.57(19) . . ? C60_2 C61_2 N6_2 106.48(17) . . ? C60_2 C61_2 C65_2 131.3(2) . . ? N6_2 C61_2 C65_2 122.19(19) . . ? _refine_diff_density_max 1.550 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.082 _shelx_res_file ; TITL mks_037am in P-1 mks_037am_sq.res created by SHELXL-2017/1 at 15:31:57 on 07-Jan-2021 CELL 0.71073 14.86260 20.32990 25.71150 83.6029 75.2580 72.5648 ZERR 4.00 0.00230 0.00480 0.00560 0.0043 0.0062 0.0039 LATT 1 SFAC C H Cl Ga N P UNIT 260 376 8 8 24 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.160 SIZE 0.094 0.098 0.152 L.S. 16 0 183 ACTA FMAP 2 PLAN 20 ABIN OMIT 0 1 1 OMIT 0 1 0 OMIT 0 0 1 OMIT 0 2 1 OMIT 1 -1 1 OMIT 0 2 0 OMIT 1 1 3 WGHT 0.056800 FVAR 0.06331 RESI 1 GA1 4 0.765287 0.303882 0.688951 11.00000 0.01318 0.01173 = 0.01319 -0.00033 -0.00101 -0.00405 GA2 4 0.949078 0.311796 0.478355 11.00000 0.01601 0.01223 = 0.01150 -0.00087 -0.00260 -0.00368 CL1 3 0.863768 0.246923 0.741490 11.00000 0.01966 0.02157 = 0.02425 0.00143 -0.00844 -0.00467 CL2 3 0.953906 0.421037 0.482604 11.00000 0.02174 0.01324 = 0.02097 -0.00106 -0.00669 -0.00506 P1 6 0.832025 0.346843 0.604713 11.00000 0.01396 0.01326 = 0.01307 0.00010 -0.00266 -0.00363 P2 6 0.883231 0.257290 0.554063 11.00000 0.02008 0.01389 = 0.01462 -0.00113 -0.00076 -0.00700 N1 5 0.680523 0.244764 0.696171 11.00000 0.01246 0.01460 = 0.01499 0.00067 -0.00195 -0.00491 N2 5 0.675786 0.372393 0.740834 11.00000 0.01890 0.01426 = 0.01246 -0.00036 -0.00236 -0.00223 N3 5 0.905632 0.316692 0.410768 11.00000 0.01886 0.01835 = 0.01563 -0.00227 -0.00429 -0.00775 N4 5 1.089390 0.270270 0.441877 11.00000 0.01920 0.01012 = 0.01565 -0.00020 -0.00201 -0.00364 N5 5 0.938538 0.427283 0.630349 11.00000 0.02129 0.01484 = 0.01811 -0.00015 -0.00600 -0.00757 N6 5 1.017118 0.320035 0.637722 11.00000 0.01783 0.01486 = 0.01792 0.00345 -0.00534 -0.00568 C1 1 0.620642 0.239915 0.744242 11.00000 0.01249 0.02015 = 0.01884 0.00463 -0.00321 -0.00530 C2 1 0.595859 0.287494 0.784986 11.00000 0.01780 0.02693 = 0.01319 0.00238 0.00196 -0.00636 AFIX 43 H2 2 0.563318 0.273949 0.819457 11.00000 -1.20000 AFIX 0 C3 1 0.612859 0.351871 0.781321 11.00000 0.01905 0.02071 = 0.01398 -0.00119 -0.00175 0.00013 C4 1 0.573639 0.181802 0.756241 11.00000 0.01834 0.02901 = 0.02539 0.00458 0.00120 -0.01208 AFIX 137 H4A 2 0.539124 0.182048 0.728394 11.00000 -1.50000 H4B 2 0.527663 0.188013 0.791425 11.00000 -1.50000 H4C 2 0.623642 0.137651 0.756686 11.00000 -1.50000 AFIX 0 C5 1 0.554108 0.400378 0.826559 11.00000 0.03803 0.02755 = 0.01752 -0.00573 0.00633 -0.00324 AFIX 137 H5A 2 0.526809 0.446203 0.811256 11.00000 -1.50000 H5B 2 0.596247 0.403708 0.849329 11.00000 -1.50000 H5C 2 0.501389 0.382495 0.848259 11.00000 -1.50000 AFIX 0 C6 1 0.689676 0.198107 0.654909 11.00000 0.01641 0.02085 = 0.01610 0.00064 -0.00083 -0.01201 C7 1 0.640228 0.224293 0.613512 11.00000 0.01988 0.02327 = 0.01801 0.00348 -0.00345 -0.01193 C8 1 0.647033 0.178248 0.575230 11.00000 0.03610 0.03480 = 0.02048 0.00213 -0.01008 -0.01814 AFIX 43 H8 2 0.612776 0.194083 0.547598 11.00000 -1.20000 AFIX 0 C9 1 0.702442 0.110130 0.576557 11.00000 0.04775 0.03292 = 0.02129 -0.00679 -0.00627 -0.01877 AFIX 43 H9 2 0.705062 0.079605 0.550443 11.00000 -1.20000 AFIX 0 C10 1 0.753779 0.086777 0.615904 11.00000 0.03261 0.02000 = 0.02808 -0.00327 -0.00333 -0.00898 AFIX 43 H10 2 0.793502 0.040438 0.615790 11.00000 -1.20000 AFIX 0 C11 1 0.748650 0.129711 0.655861 11.00000 0.01993 0.01700 = 0.02100 0.00033 -0.00145 -0.00929 C12 1 0.582414 0.299561 0.610366 11.00000 0.02405 0.02580 = 0.02201 0.00544 -0.00940 -0.01175 AFIX 13 H12 2 0.618807 0.327468 0.621687 11.00000 -1.20000 AFIX 0 C13 1 0.482016 0.314494 0.648743 11.00000 0.02330 0.02913 = 0.03834 0.00997 -0.00719 -0.00465 AFIX 137 H13A 2 0.447789 0.363593 0.645586 11.00000 -1.50000 H13B 2 0.488982 0.302643 0.685795 11.00000 -1.50000 H13C 2 0.444935 0.286816 0.639445 11.00000 -1.50000 AFIX 0 C14 1 0.572949 0.324225 0.552764 11.00000 0.04318 0.03332 = 0.02794 0.01108 -0.01664 -0.01891 AFIX 137 H14A 2 0.637366 0.312913 0.528232 11.00000 -1.50000 H14B 2 0.543520 0.374268 0.551642 11.00000 -1.50000 H14C 2 0.531926 0.301218 0.541694 11.00000 -1.50000 AFIX 0 C15 1 0.809382 0.101180 0.696958 11.00000 0.02353 0.01538 = 0.02680 -0.00184 -0.00563 -0.00637 AFIX 13 H15 2 0.789171 0.135128 0.725985 11.00000 -1.20000 AFIX 0 C16 1 0.796406 0.031688 0.722880 11.00000 0.04808 0.01921 = 0.03301 0.00375 -0.01477 -0.01012 AFIX 137 H16A 2 0.818053 -0.002646 0.695103 11.00000 -1.50000 H16B 2 0.727826 0.037198 0.740096 11.00000 -1.50000 H16C 2 0.835069 0.016233 0.749961 11.00000 -1.50000 AFIX 0 C17 1 0.917109 0.092568 0.669802 11.00000 0.02288 0.02772 = 0.04683 -0.00678 -0.00895 -0.00324 AFIX 137 H17A 2 0.937813 0.060001 0.640796 11.00000 -1.50000 H17B 2 0.956245 0.074875 0.696468 11.00000 -1.50000 H17C 2 0.925816 0.137347 0.654864 11.00000 -1.50000 AFIX 0 C18 1 0.679645 0.443477 0.736418 11.00000 0.02795 0.01371 = 0.01432 -0.00297 -0.00162 -0.00124 C19 1 0.623035 0.490914 0.704728 11.00000 0.03248 0.01658 = 0.01537 -0.00185 -0.00227 0.00563 C20 1 0.629116 0.558646 0.698754 11.00000 0.04863 0.01507 = 0.02228 0.00038 -0.00473 0.00480 AFIX 43 H20 2 0.590536 0.591564 0.678164 11.00000 -1.20000 AFIX 0 C21 1 0.689742 0.578611 0.722046 11.00000 0.07364 0.01515 = 0.02196 -0.00199 -0.00517 -0.01030 AFIX 43 H21 2 0.695084 0.624396 0.716066 11.00000 -1.20000 AFIX 0 C22 1 0.743062 0.532266 0.754190 11.00000 0.06418 0.01832 = 0.02327 -0.00262 -0.01214 -0.01501 AFIX 43 H22 2 0.783857 0.546914 0.770656 11.00000 -1.20000 AFIX 0 C23 1 0.737994 0.464216 0.762887 11.00000 0.04258 0.01709 = 0.01568 -0.00204 -0.00503 -0.00736 C24 1 0.554004 0.470803 0.679284 11.00000 0.02748 0.02636 = 0.01960 0.00077 -0.00371 0.00496 AFIX 13 H24 2 0.564961 0.419785 0.684752 11.00000 -1.20000 AFIX 0 C25 1 0.448184 0.506026 0.706254 11.00000 0.03058 0.06555 = 0.02576 -0.00783 0.00179 0.00127 AFIX 137 H25A 2 0.434494 0.556010 0.699247 11.00000 -1.50000 H25B 2 0.437152 0.495908 0.745152 11.00000 -1.50000 H25C 2 0.405225 0.488689 0.691610 11.00000 -1.50000 AFIX 0 C26 1 0.574515 0.487762 0.618733 11.00000 0.02421 0.03794 = 0.02195 -0.00141 -0.00440 0.00278 AFIX 137 H26A 2 0.643445 0.467391 0.602647 11.00000 -1.50000 H26B 2 0.557913 0.537935 0.612404 11.00000 -1.50000 H26C 2 0.535334 0.468831 0.602335 11.00000 -1.50000 AFIX 0 C27 1 0.792275 0.416651 0.802345 11.00000 0.04369 0.01896 = 0.01809 0.00129 -0.01102 -0.01337 AFIX 13 H27 2 0.774557 0.372280 0.806852 11.00000 -1.20000 AFIX 0 C28 1 0.760945 0.449303 0.857988 11.00000 0.07581 0.02964 = 0.02295 0.00081 -0.02044 -0.01650 AFIX 137 H28A 2 0.781117 0.491542 0.854871 11.00000 -1.50000 H28B 2 0.791592 0.416570 0.883685 11.00000 -1.50000 H28C 2 0.690272 0.460489 0.870668 11.00000 -1.50000 AFIX 0 C29 1 0.901606 0.400475 0.781693 11.00000 0.04831 0.03268 = 0.03552 0.00845 -0.01779 -0.02100 AFIX 137 H29A 2 0.921317 0.377272 0.747486 11.00000 -1.50000 H29B 2 0.933612 0.370255 0.808084 11.00000 -1.50000 H29C 2 0.920384 0.443468 0.776194 11.00000 -1.50000 AFIX 0 C30 1 0.963218 0.325186 0.362678 11.00000 0.02955 0.01924 = 0.01536 -0.00284 -0.00575 -0.00963 C31 1 1.063290 0.312845 0.353870 11.00000 0.02788 0.02314 = 0.01124 -0.00115 0.00001 -0.01035 AFIX 43 H31 2 1.094966 0.327786 0.319674 11.00000 -1.20000 AFIX 0 C32 1 1.123544 0.280815 0.389562 11.00000 0.02214 0.01076 = 0.01793 -0.00347 0.00165 -0.00676 C33 1 0.919155 0.346928 0.313964 11.00000 0.03592 0.04185 = 0.01531 0.00181 -0.00710 -0.01649 AFIX 137 H33A 2 0.969929 0.351657 0.282125 11.00000 -1.50000 H33B 2 0.869142 0.391236 0.320326 11.00000 -1.50000 H33C 2 0.890005 0.311899 0.308056 11.00000 -1.50000 AFIX 0 C34 1 1.230902 0.257313 0.364373 11.00000 0.02574 0.02251 = 0.01879 -0.00218 0.00340 -0.00723 AFIX 137 H34A 2 1.240954 0.246118 0.326844 11.00000 -1.50000 H34B 2 1.261435 0.216280 0.384294 11.00000 -1.50000 H34C 2 1.259996 0.294288 0.365631 11.00000 -1.50000 AFIX 0 C35 1 0.808408 0.315256 0.411448 11.00000 0.02482 0.02584 = 0.01354 0.00005 -0.00712 -0.01141 C36 1 0.731361 0.376129 0.418119 11.00000 0.02482 0.02511 = 0.01643 0.00377 -0.00933 -0.01115 C37 1 0.640445 0.372550 0.415674 11.00000 0.02374 0.03304 = 0.02869 0.00269 -0.01203 -0.00897 AFIX 43 H37 2 0.587472 0.413252 0.420161 11.00000 -1.20000 AFIX 0 C38 1 0.625325 0.311259 0.406882 11.00000 0.02885 0.04430 = 0.04185 0.00070 -0.01969 -0.01854 AFIX 43 H38 2 0.563011 0.310327 0.404435 11.00000 -1.20000 AFIX 0 C39 1 0.700770 0.251683 0.401696 11.00000 0.04002 0.03541 = 0.03588 -0.00295 -0.01804 -0.02067 AFIX 43 H39 2 0.689589 0.209564 0.396373 11.00000 -1.20000 AFIX 0 C40 1 0.793762 0.251789 0.404096 11.00000 0.03454 0.02601 = 0.01927 -0.00192 -0.01042 -0.01465 C41 1 0.744791 0.444299 0.429592 11.00000 0.02110 0.02078 = 0.02250 0.00200 -0.00847 -0.00714 AFIX 13 H41 2 0.815919 0.438245 0.423637 11.00000 -1.20000 AFIX 0 C42 1 0.697698 0.461525 0.488407 11.00000 0.02856 0.02546 = 0.03079 -0.00249 -0.00632 -0.00972 AFIX 137 H42A 2 0.709885 0.503815 0.496090 11.00000 -1.50000 H42B 2 0.725348 0.423432 0.511760 11.00000 -1.50000 H42C 2 0.627638 0.468383 0.495116 11.00000 -1.50000 AFIX 0 C43 1 0.704095 0.504713 0.392673 11.00000 0.02995 0.02890 = 0.03909 0.01046 -0.01546 -0.01020 AFIX 137 H43A 2 0.730769 0.491977 0.355021 11.00000 -1.50000 H43B 2 0.722314 0.545332 0.398532 11.00000 -1.50000 H43C 2 0.633255 0.515348 0.400926 11.00000 -1.50000 AFIX 0 C44 1 0.875116 0.184933 0.398484 11.00000 0.03688 0.02395 = 0.03087 -0.00490 -0.01039 -0.01300 AFIX 13 H44 2 0.933751 0.195460 0.403655 11.00000 -1.20000 AFIX 0 C45 1 0.851076 0.131834 0.441983 11.00000 0.04100 0.03243 = 0.06189 0.01082 -0.00811 -0.01223 AFIX 137 H45A 2 0.793887 0.120148 0.437983 11.00000 -1.50000 H45B 2 0.837590 0.150867 0.477445 11.00000 -1.50000 H45C 2 0.906225 0.090193 0.438613 11.00000 -1.50000 AFIX 0 C46 1 0.901736 0.155402 0.342167 11.00000 0.08641 0.04774 = 0.04635 -0.02220 -0.02679 0.00470 AFIX 137 H46A 2 0.919116 0.189942 0.314822 11.00000 -1.50000 H46B 2 0.846077 0.143592 0.336048 11.00000 -1.50000 H46C 2 0.956947 0.113888 0.339809 11.00000 -1.50000 AFIX 0 C47 1 1.156175 0.233749 0.474509 11.00000 0.01542 0.01363 = 0.01620 -0.00038 0.00130 -0.00020 C48 1 1.218609 0.265626 0.487839 11.00000 0.01596 0.01636 = 0.02093 0.00082 -0.00017 -0.00093 C49 1 1.283769 0.226728 0.518382 11.00000 0.01897 0.02561 = 0.02847 -0.00107 -0.00477 -0.00407 AFIX 43 H49 2 1.327019 0.247087 0.527730 11.00000 -1.20000 AFIX 0 C50 1 1.286173 0.159089 0.535172 11.00000 0.02322 0.02343 = 0.03203 0.00534 -0.00816 0.00272 AFIX 43 H50 2 1.332004 0.133177 0.554977 11.00000 -1.20000 AFIX 0 C51 1 1.222276 0.129514 0.523174 11.00000 0.02811 0.01476 = 0.02700 0.00379 -0.00234 0.00032 AFIX 43 H51 2 1.223478 0.083597 0.535797 11.00000 -1.20000 AFIX 0 C52 1 1.155765 0.165258 0.492938 11.00000 0.01942 0.01324 = 0.01878 -0.00111 0.00234 -0.00171 C53 1 1.217390 0.340365 0.471901 11.00000 0.01891 0.01806 = 0.02251 0.00177 -0.00581 -0.00659 AFIX 13 H53 2 1.175265 0.357643 0.445683 11.00000 -1.20000 AFIX 0 C54 1 1.173037 0.385084 0.521497 11.00000 0.02797 0.02102 = 0.02765 -0.00091 -0.01048 -0.00769 AFIX 137 H54A 2 1.166946 0.433615 0.510356 11.00000 -1.50000 H54B 2 1.215083 0.370653 0.546951 11.00000 -1.50000 H54C 2 1.108780 0.379519 0.538832 11.00000 -1.50000 AFIX 0 C55 1 1.318671 0.348394 0.444908 11.00000 0.02791 0.03061 = 0.03393 0.00348 -0.00392 -0.01537 AFIX 137 H55A 2 1.349690 0.316083 0.415696 11.00000 -1.50000 H55B 2 1.358286 0.338489 0.471561 11.00000 -1.50000 H55C 2 1.312585 0.395728 0.430263 11.00000 -1.50000 AFIX 0 C56 1 1.087574 0.131012 0.478382 11.00000 0.02259 0.01283 = 0.02527 -0.00311 0.00478 -0.00442 AFIX 13 H56 2 1.025429 0.167533 0.477595 11.00000 -1.20000 AFIX 0 C57 1 1.063306 0.074461 0.519283 11.00000 0.03763 0.02229 = 0.04312 0.00737 -0.00231 -0.01307 AFIX 137 H57A 2 1.011760 0.059641 0.510925 11.00000 -1.50000 H57B 2 1.041385 0.092496 0.555557 11.00000 -1.50000 H57C 2 1.121238 0.035046 0.517549 11.00000 -1.50000 AFIX 0 C58 1 1.129192 0.101914 0.421923 11.00000 0.03184 0.02455 = 0.03441 -0.01515 0.00948 -0.01123 AFIX 137 H58A 2 1.139819 0.139197 0.395604 11.00000 -1.50000 H58B 2 1.083369 0.081504 0.412927 11.00000 -1.50000 H58C 2 1.190965 0.066461 0.421182 11.00000 -1.50000 AFIX 0 C59 1 0.934692 0.362595 0.625592 11.00000 0.01737 0.01328 = 0.01344 0.00120 -0.00406 -0.00520 C60 1 1.020899 0.425795 0.647101 11.00000 0.02324 0.02407 = 0.01735 0.00206 -0.00614 -0.01276 C61 1 1.070042 0.358141 0.651732 11.00000 0.02010 0.02512 = 0.01651 0.00387 -0.00639 -0.01044 C62 1 0.870505 0.491214 0.615219 11.00000 0.02723 0.01252 = 0.02705 -0.00021 -0.00788 -0.00330 AFIX 137 H62A 2 0.905748 0.516391 0.586528 11.00000 -1.50000 H62B 2 0.840000 0.520030 0.646616 11.00000 -1.50000 H62C 2 0.820433 0.479821 0.602430 11.00000 -1.50000 AFIX 0 C63 1 1.050136 0.244582 0.634555 11.00000 0.01601 0.01629 = 0.02554 0.00183 -0.00406 -0.00092 AFIX 137 H63A 2 1.005464 0.229127 0.619894 11.00000 -1.50000 H63B 2 1.051636 0.223520 0.670628 11.00000 -1.50000 H63C 2 1.115341 0.230750 0.611029 11.00000 -1.50000 AFIX 0 C64 1 1.041408 0.489984 0.657474 11.00000 0.04010 0.03033 = 0.02866 0.00063 -0.01141 -0.02231 AFIX 137 H64A 2 1.051128 0.517589 0.623843 11.00000 -1.50000 H64B 2 1.100083 0.477757 0.671425 11.00000 -1.50000 H64C 2 0.986489 0.516784 0.683970 11.00000 -1.50000 AFIX 0 C65 1 1.163545 0.325076 0.668199 11.00000 0.02614 0.03845 = 0.03352 0.01208 -0.01565 -0.01518 AFIX 137 H65A 2 1.211189 0.299062 0.638325 11.00000 -1.50000 H65B 2 1.152713 0.293688 0.699455 11.00000 -1.50000 H65C 2 1.187976 0.360822 0.677603 11.00000 -1.50000 AFIX 0 RESI 2 GA1 4 0.406638 0.995040 0.800656 11.00000 0.01134 0.01259 = 0.01020 -0.00022 -0.00091 -0.00239 GA2 4 0.239055 0.823135 0.944473 11.00000 0.01577 0.01437 = 0.01166 0.00057 -0.00285 -0.00549 CL1 3 0.498416 1.041190 0.832069 11.00000 0.02748 0.02429 = 0.02406 -0.00299 -0.00783 -0.00712 CL2 3 0.096848 0.906607 0.963830 11.00000 0.01638 0.01877 = 0.01848 0.00000 -0.00276 -0.00386 P1 6 0.289726 0.951340 0.861564 11.00000 0.01370 0.01541 = 0.01028 -0.00040 -0.00188 -0.00507 P2 6 0.368312 0.848306 0.886201 11.00000 0.01622 0.01572 = 0.01595 0.00094 -0.00016 -0.00342 N1 5 0.356947 1.071405 0.751762 11.00000 0.01068 0.01372 = 0.01333 -0.00006 -0.00159 -0.00295 N2 5 0.506266 0.937960 0.745437 11.00000 0.01403 0.01205 = 0.01349 -0.00182 -0.00135 -0.00115 N3 5 0.255512 0.792298 1.019424 11.00000 0.01772 0.01930 = 0.01263 0.00146 -0.00310 -0.00624 N4 5 0.193387 0.742123 0.937278 11.00000 0.02081 0.01665 = 0.01656 0.00050 -0.00590 -0.00716 N5 5 0.187483 1.066348 0.925948 11.00000 0.01413 0.01703 = 0.01317 -0.00014 0.00017 -0.00500 N6 5 0.325071 1.020020 0.946809 11.00000 0.01551 0.01950 = 0.01226 -0.00177 -0.00181 -0.00740 C1 1 0.416330 1.083009 0.705062 11.00000 0.01589 0.01700 = 0.01341 0.00179 -0.00430 -0.00714 C2 1 0.505974 1.037368 0.683958 11.00000 0.01564 0.02286 = 0.01197 0.00154 0.00223 -0.00638 AFIX 43 H2 2 0.546685 1.055223 0.654713 11.00000 -1.20000 AFIX 0 C3 1 0.544605 0.968161 0.700104 11.00000 0.01472 0.02148 = 0.01330 -0.00394 -0.00115 -0.00407 C4 1 0.384969 1.147788 0.671632 11.00000 0.01989 0.01988 = 0.01791 0.00479 -0.00247 -0.00472 AFIX 137 H4A 2 0.436748 1.149074 0.639461 11.00000 -1.50000 H4B 2 0.371637 1.188223 0.692865 11.00000 -1.50000 H4C 2 0.326141 1.148163 0.660844 11.00000 -1.50000 AFIX 0 C5 1 0.634126 0.927764 0.661909 11.00000 0.02127 0.02528 = 0.01493 -0.00191 0.00339 0.00138 AFIX 137 H5A 2 0.634851 0.947203 0.625221 11.00000 -1.50000 H5B 2 0.633826 0.879457 0.663322 11.00000 -1.50000 H5C 2 0.691939 0.930352 0.672335 11.00000 -1.50000 AFIX 0 C6 1 0.259211 1.116599 0.765568 11.00000 0.01208 0.01518 = 0.01335 0.00501 -0.00263 -0.00311 C7 1 0.185483 1.097754 0.750793 11.00000 0.01659 0.01630 = 0.01548 0.00320 -0.00540 -0.00439 C8 1 0.090934 1.141098 0.764004 11.00000 0.01334 0.02282 = 0.01969 0.00547 -0.00698 -0.00601 AFIX 43 H8 2 0.040426 1.129327 0.754169 11.00000 -1.20000 AFIX 0 C9 1 0.069525 1.201112 0.791276 11.00000 0.01104 0.02126 = 0.02285 0.00405 -0.00270 -0.00051 AFIX 43 H9 2 0.004695 1.229837 0.800296 11.00000 -1.20000 AFIX 0 C10 1 0.142867 1.219070 0.805330 11.00000 0.01655 0.01593 = 0.01897 -0.00088 -0.00180 -0.00381 AFIX 43 H10 2 0.127460 1.260127 0.824156 11.00000 -1.20000 AFIX 0 C11 1 0.239131 1.178029 0.792388 11.00000 0.01335 0.01653 = 0.01409 0.00401 -0.00284 -0.00517 C12 1 0.206945 1.032879 0.719484 11.00000 0.01802 0.02125 = 0.02773 -0.00277 -0.01151 -0.00368 AFIX 13 H12 2 0.275176 1.005149 0.719117 11.00000 -1.20000 AFIX 0 C13 1 0.140795 0.988079 0.746509 11.00000 0.04377 0.02353 = 0.02709 0.00409 -0.01370 -0.01608 AFIX 137 H13A 2 0.073551 1.013121 0.745822 11.00000 -1.50000 H13B 2 0.146060 0.977054 0.783901 11.00000 -1.50000 H13C 2 0.160274 0.945280 0.727168 11.00000 -1.50000 AFIX 0 C14 1 0.200046 1.051279 0.660961 11.00000 0.04278 0.03914 = 0.02174 -0.00230 -0.00288 -0.02313 AFIX 137 H14A 2 0.247736 1.076014 0.643293 11.00000 -1.50000 H14B 2 0.134728 1.080678 0.660106 11.00000 -1.50000 H14C 2 0.213262 1.008923 0.642030 11.00000 -1.50000 AFIX 0 C15 1 0.317496 1.202439 0.805904 11.00000 0.01272 0.01634 = 0.01960 -0.00089 -0.00243 -0.00391 AFIX 13 H15 2 0.381840 1.171231 0.788443 11.00000 -1.20000 AFIX 0 C16 1 0.310184 1.198330 0.866488 11.00000 0.01917 0.02684 = 0.02216 -0.00326 -0.00424 -0.00666 AFIX 137 H16A 2 0.318914 1.150287 0.879820 11.00000 -1.50000 H16B 2 0.246261 1.226634 0.884792 11.00000 -1.50000 H16C 2 0.360687 1.215436 0.873702 11.00000 -1.50000 AFIX 0 C17 1 0.314440 1.276441 0.783822 11.00000 0.02181 0.01886 = 0.03554 0.00243 -0.00605 -0.00849 AFIX 137 H17A 2 0.370980 1.288061 0.788886 11.00000 -1.50000 H17B 2 0.254997 1.308754 0.803140 11.00000 -1.50000 H17C 2 0.315399 1.279619 0.745381 11.00000 -1.50000 AFIX 0 C18 1 0.545181 0.864671 0.757051 11.00000 0.01789 0.01477 = 0.01147 -0.00362 0.00166 0.00023 C19 1 0.493882 0.819531 0.749713 11.00000 0.02394 0.01722 = 0.01850 -0.00561 -0.00243 -0.00199 C20 1 0.526694 0.750049 0.764670 11.00000 0.03165 0.01818 = 0.02303 -0.00563 0.00108 -0.00541 AFIX 43 H20 2 0.494576 0.718439 0.758983 11.00000 -1.20000 AFIX 0 C21 1 0.606088 0.726686 0.787850 11.00000 0.02931 0.01626 = 0.02422 -0.00076 0.00206 -0.00030 AFIX 43 H21 2 0.626121 0.679630 0.799362 11.00000 -1.20000 AFIX 0 C22 1 0.655472 0.770988 0.794175 11.00000 0.01956 0.02151 = 0.02106 0.00081 -0.00085 0.00227 AFIX 43 H22 2 0.710129 0.753868 0.809613 11.00000 -1.20000 AFIX 0 C23 1 0.627846 0.840622 0.778592 11.00000 0.01977 0.01845 = 0.01282 -0.00233 0.00101 -0.00091 C24 1 0.403253 0.846054 0.726981 11.00000 0.03621 0.02308 = 0.03148 -0.00274 -0.01557 -0.01114 AFIX 13 H24 2 0.366841 0.892009 0.742757 11.00000 -1.20000 AFIX 0 C25 1 0.334595 0.801153 0.742894 11.00000 0.03422 0.04049 = 0.03315 -0.00678 -0.00931 -0.01401 AFIX 137 H25A 2 0.273586 0.825065 0.732490 11.00000 -1.50000 H25B 2 0.321620 0.791991 0.781926 11.00000 -1.50000 H25C 2 0.364257 0.757417 0.724539 11.00000 -1.50000 AFIX 0 C26 1 0.427677 0.858327 0.666667 11.00000 0.06792 0.06489 = 0.03422 0.01018 -0.02407 -0.04189 AFIX 137 H26A 2 0.467142 0.814987 0.649501 11.00000 -1.50000 H26B 2 0.464074 0.892667 0.657411 11.00000 -1.50000 H26C 2 0.367665 0.875293 0.653949 11.00000 -1.50000 AFIX 0 C27 1 0.687858 0.885886 0.786441 11.00000 0.01804 0.02034 = 0.02139 -0.00077 -0.00658 0.00051 AFIX 13 H27 2 0.661097 0.933316 0.771549 11.00000 -1.20000 AFIX 0 C28 1 0.682700 0.890842 0.846428 11.00000 0.03221 0.03113 = 0.02239 -0.00150 -0.01146 -0.00105 AFIX 137 H28A 2 0.710822 0.844985 0.861398 11.00000 -1.50000 H28B 2 0.614842 0.908474 0.865742 11.00000 -1.50000 H28C 2 0.719149 0.922228 0.850373 11.00000 -1.50000 AFIX 0 C29 1 0.794902 0.858338 0.756322 11.00000 0.01875 0.02541 = 0.03027 0.00287 -0.00526 -0.00199 AFIX 137 H29A 2 0.798930 0.857788 0.717725 11.00000 -1.50000 H29B 2 0.821923 0.811401 0.769856 11.00000 -1.50000 H29C 2 0.831848 0.888325 0.762254 11.00000 -1.50000 AFIX 0 C30 1 0.202857 0.754499 1.051215 11.00000 0.02062 0.01663 = 0.01723 0.00303 -0.00344 -0.00303 C31 1 0.143557 0.723740 1.033280 11.00000 0.02056 0.02359 = 0.01859 0.00391 -0.00164 -0.01075 AFIX 43 H31 2 0.097445 0.707928 1.060574 11.00000 -1.20000 AFIX 0 C32 1 0.144074 0.713569 0.980342 11.00000 0.01901 0.01659 = 0.02461 0.00067 -0.00535 -0.00526 C33 1 0.207396 0.740286 1.109934 11.00000 0.03362 0.02827 = 0.01830 0.00784 -0.00739 -0.01436 AFIX 137 H33A 2 0.170713 0.707391 1.126283 11.00000 -1.50000 H33B 2 0.179263 0.783466 1.129122 11.00000 -1.50000 H33C 2 0.275140 0.720837 1.112255 11.00000 -1.50000 AFIX 0 C34 1 0.088547 0.665218 0.972330 11.00000 0.03345 0.02885 = 0.02985 0.00142 -0.00750 -0.01967 AFIX 137 H34A 2 0.040846 0.689456 0.951410 11.00000 -1.50000 H34B 2 0.055080 0.649995 1.007461 11.00000 -1.50000 H34C 2 0.133892 0.625011 0.952949 11.00000 -1.50000 AFIX 0 C35 1 0.318715 0.817673 1.041397 11.00000 0.01965 0.02208 = 0.01208 0.00434 -0.00560 -0.00749 C36 1 0.279670 0.872907 1.076605 11.00000 0.02326 0.02368 = 0.01237 0.00518 -0.00561 -0.00961 C37 1 0.343976 0.894152 1.097738 11.00000 0.03226 0.03103 = 0.01820 0.00272 -0.01138 -0.01408 AFIX 43 H37 2 0.319427 0.931446 1.121412 11.00000 -1.20000 AFIX 0 C38 1 0.442722 0.861840 1.084793 11.00000 0.03061 0.03849 = 0.02825 0.00473 -0.01702 -0.01553 AFIX 43 H38 2 0.485020 0.876356 1.100178 11.00000 -1.20000 AFIX 0 C39 1 0.479787 0.808415 1.049454 11.00000 0.02053 0.03873 = 0.02586 0.00542 -0.01206 -0.00964 AFIX 43 H39 2 0.547697 0.786897 1.040692 11.00000 -1.20000 AFIX 0 C40 1 0.419605 0.785339 1.026322 11.00000 0.02317 0.02602 = 0.01729 0.00609 -0.00631 -0.00783 C41 1 0.172095 0.911075 1.091176 11.00000 0.02312 0.02208 = 0.01231 -0.00147 -0.00148 -0.00958 AFIX 13 H41 2 0.136253 0.884341 1.078012 11.00000 -1.20000 AFIX 0 C42 1 0.131694 0.918432 1.152106 11.00000 0.03765 0.03816 = 0.01708 -0.00152 0.00148 -0.01340 AFIX 137 H42A 2 0.160480 0.949013 1.165130 11.00000 -1.50000 H42B 2 0.147719 0.872958 1.170382 11.00000 -1.50000 H42C 2 0.061094 0.938020 1.159701 11.00000 -1.50000 AFIX 0 C43 1 0.153686 0.982657 1.063044 11.00000 0.02711 0.02450 = 0.02155 0.00078 -0.00501 -0.00999 AFIX 137 H43A 2 0.181091 0.978082 1.024255 11.00000 -1.50000 H43B 2 0.184475 1.010840 1.077267 11.00000 -1.50000 H43C 2 0.083707 1.004874 1.069599 11.00000 -1.50000 AFIX 0 C44 1 0.462689 0.725606 0.988368 11.00000 0.02202 0.02735 = 0.02162 0.00257 -0.00624 -0.00438 AFIX 13 H44 2 0.417224 0.730481 0.964511 11.00000 -1.20000 AFIX 0 C45 1 0.468033 0.656426 1.020143 11.00000 0.05183 0.02747 = 0.03251 0.00423 -0.00743 0.00093 AFIX 137 H45A 2 0.493001 0.618690 0.995048 11.00000 -1.50000 H45B 2 0.403089 0.656271 1.041206 11.00000 -1.50000 H45C 2 0.511417 0.650201 1.044436 11.00000 -1.50000 AFIX 0 C46 1 0.561216 0.726225 0.951958 11.00000 0.02408 0.04883 = 0.03358 -0.00460 -0.00295 -0.00397 AFIX 137 H46A 2 0.582081 0.689690 0.926000 11.00000 -1.50000 H46B 2 0.608891 0.718311 0.973881 11.00000 -1.50000 H46C 2 0.555910 0.771071 0.932627 11.00000 -1.50000 AFIX 0 C47 1 0.208158 0.714239 0.885365 11.00000 0.02738 0.01958 = 0.01959 -0.00196 -0.00632 -0.01076 C48 1 0.141402 0.742968 0.852676 11.00000 0.02630 0.02361 = 0.02163 -0.00201 -0.00744 -0.01166 C49 1 0.159717 0.714282 0.802663 11.00000 0.04083 0.03352 = 0.02849 -0.00695 -0.01307 -0.01501 AFIX 43 H49 2 0.116071 0.733061 0.779945 11.00000 -1.20000 AFIX 0 C50 1 0.240105 0.659130 0.785647 11.00000 0.05289 0.03639 = 0.03344 -0.01881 -0.01232 -0.01149 AFIX 43 H50 2 0.251396 0.640383 0.751567 11.00000 -1.20000 AFIX 0 C51 1 0.303645 0.631581 0.818424 11.00000 0.04554 0.02589 = 0.03666 -0.01499 -0.00896 -0.00356 AFIX 43 H51 2 0.358440 0.593569 0.806553 11.00000 -1.20000 AFIX 0 C52 1 0.289704 0.657924 0.868386 11.00000 0.03274 0.01958 = 0.02950 -0.00406 -0.00761 -0.00623 C53 1 0.053828 0.804125 0.869470 11.00000 0.02118 0.02841 = 0.02102 -0.00153 -0.00860 -0.00813 AFIX 13 H53 2 0.047370 0.812210 0.908077 11.00000 -1.20000 AFIX 0 C54 1 -0.040477 0.791703 0.864769 11.00000 0.02892 0.05620 = 0.03584 0.00265 -0.01368 -0.01775 AFIX 137 H54A 2 -0.037258 0.785898 0.826947 11.00000 -1.50000 H54B 2 -0.095361 0.831314 0.878396 11.00000 -1.50000 H54C 2 -0.049125 0.749954 0.885957 11.00000 -1.50000 AFIX 0 C55 1 0.069287 0.868943 0.836287 11.00000 0.03558 0.02929 = 0.02452 -0.00092 -0.00645 -0.00614 AFIX 137 H55A 2 0.076024 0.862272 0.798171 11.00000 -1.50000 H55B 2 0.128249 0.877383 0.840974 11.00000 -1.50000 H55C 2 0.013473 0.908627 0.848494 11.00000 -1.50000 AFIX 0 C56 1 0.361579 0.624633 0.903317 11.00000 0.03079 0.02186 = 0.03029 -0.00261 -0.00672 -0.00242 AFIX 13 H56 2 0.341933 0.651881 0.936462 11.00000 -1.20000 AFIX 0 C57 1 0.359204 0.550051 0.920842 11.00000 0.04725 0.02986 = 0.05951 0.00966 -0.01339 -0.00774 AFIX 137 H57A 2 0.376230 0.522660 0.888898 11.00000 -1.50000 H57B 2 0.293941 0.550242 0.941595 11.00000 -1.50000 H57C 2 0.405932 0.529822 0.943176 11.00000 -1.50000 AFIX 0 C58 1 0.464325 0.626094 0.874259 11.00000 0.03653 0.04011 = 0.03554 -0.00152 -0.00671 -0.00642 AFIX 137 H58A 2 0.484020 0.601530 0.840679 11.00000 -1.50000 H58B 2 0.509026 0.603635 0.897336 11.00000 -1.50000 H58C 2 0.465856 0.674054 0.866118 11.00000 -1.50000 AFIX 0 C59 1 0.270448 1.013889 0.913892 11.00000 0.01312 0.01678 = 0.01083 0.00098 -0.00054 -0.00597 C60 1 0.191342 1.106502 0.965283 11.00000 0.02144 0.01738 = 0.01399 -0.00178 0.00386 -0.00943 C61 1 0.278342 1.077344 0.978493 11.00000 0.02261 0.02312 = 0.01208 -0.00279 0.00000 -0.01176 C62 1 0.101980 1.077535 0.903726 11.00000 0.01389 0.02056 = 0.02023 0.00139 -0.00302 -0.00184 AFIX 137 H62A 2 0.096496 1.118233 0.879130 11.00000 -1.50000 H62B 2 0.043602 1.084835 0.933130 11.00000 -1.50000 H62C 2 0.108835 1.036994 0.884103 11.00000 -1.50000 AFIX 0 C63 1 0.418598 0.972231 0.951993 11.00000 0.01673 0.02709 = 0.01941 0.00102 -0.00784 -0.00519 AFIX 137 H63A 2 0.435436 0.933524 0.928416 11.00000 -1.50000 H63B 2 0.414036 0.954788 0.989395 11.00000 -1.50000 H63C 2 0.468831 0.996442 0.941631 11.00000 -1.50000 AFIX 0 C64 1 0.111815 1.168941 0.985221 11.00000 0.02608 0.02252 = 0.03074 -0.00749 0.00464 -0.00825 AFIX 137 H64A 2 0.099662 1.201311 0.954879 11.00000 -1.50000 H64B 2 0.130565 1.191049 1.011147 11.00000 -1.50000 H64C 2 0.052776 1.155636 1.002784 11.00000 -1.50000 AFIX 0 C65 1 0.322312 1.096493 1.018220 11.00000 0.03038 0.03971 = 0.02159 -0.00961 -0.00276 -0.01881 AFIX 137 H65A 2 0.382710 1.107283 0.999481 11.00000 -1.50000 H65B 2 0.336228 1.057856 1.044150 11.00000 -1.50000 H65C 2 0.277030 1.136986 1.037261 11.00000 -1.50000 RESI 0 AFIX 0 HKLF 4 REM mks_037am in P-1 REM R1 = 0.0436 for 30501 Fo > 4sig(Fo) and 0.0756 for all 43665 data REM 1435 parameters refined using 0 restraints END WGHT 0.0567 0.0000 REM Highest difference peak 1.550, deepest hole -0.921, 1-sigma level 0.082 Q1 1 0.9997 0.3212 0.4817 11.00000 0.05 1.55 Q2 1 0.9956 0.4279 0.4552 11.00000 0.05 0.93 Q3 1 0.8866 0.2548 0.7076 11.00000 0.05 0.92 Q4 1 0.7773 0.3451 0.5899 11.00000 0.05 0.81 Q5 1 0.9376 0.2922 0.5704 11.00000 0.05 0.80 Q6 1 0.9790 0.3180 0.4495 11.00000 0.05 0.72 Q7 1 0.4388 1.0006 0.7729 11.00000 0.05 0.67 Q8 1 0.3726 0.9874 0.8272 11.00000 0.05 0.66 Q9 1 0.2791 0.8192 0.9173 11.00000 0.05 0.65 Q10 1 0.7227 0.3072 0.7141 11.00000 0.05 0.62 Q11 1 0.2807 0.8314 0.9526 11.00000 0.05 0.58 Q12 1 0.7671 0.3223 0.6569 11.00000 0.05 0.58 Q13 1 0.7187 0.2989 0.6767 11.00000 0.05 0.57 Q14 1 0.3604 0.9896 0.7940 11.00000 0.05 0.55 Q15 1 0.4396 1.0424 0.8303 11.00000 0.05 0.53 Q16 1 0.8140 0.3008 0.6629 11.00000 0.05 0.52 Q17 1 0.8012 0.3166 0.6984 11.00000 0.05 0.51 Q18 1 0.4548 1.0176 0.8359 11.00000 0.05 0.50 Q19 1 0.8839 0.3580 0.6125 11.00000 0.05 0.50 Q20 1 0.2438 1.0537 0.9086 11.00000 0.05 0.50 ; _shelx_res_checksum 86663 _shelx_fab_file ; 2 0 0 11.40 0.00 3 0 0 -70.23 0.00 4 0 0 -5.88 0.00 5 0 0 -8.48 0.00 6 0 0 4.77 0.00 7 0 0 -1.85 0.00 8 0 0 1.51 0.00 9 0 0 0.78 0.00 10 0 0 1.44 0.00 11 0 0 1.86 0.00 12 0 0 1.24 0.00 13 0 0 1.52 0.00 14 0 0 -0.51 0.00 15 0 0 0.08 0.00 16 0 0 0.15 0.00 17 0 0 0.79 0.00 18 0 0 -2.37 0.00 19 0 0 0.80 0.00 -19 1 0 1.25 0.00 -18 1 0 -0.08 0.00 -17 1 0 0.55 0.00 -16 1 0 -0.31 0.00 -15 1 0 -0.12 0.00 -14 1 0 -0.24 0.00 -13 1 0 -0.55 0.00 -12 1 0 0.00 0.00 -11 1 0 -1.06 0.00 -10 1 0 -2.42 0.00 -9 1 0 -2.53 0.00 -8 1 0 1.37 0.00 -7 1 0 -4.10 0.00 -6 1 0 5.22 0.00 -5 1 0 -12.73 0.00 -4 1 0 21.35 0.00 -3 1 0 13.82 0.00 -2 1 0 99.47 0.00 -1 1 0 -86.38 0.00 0 1 0 -163.72 0.00 2 1 0 -2.69 0.00 3 1 0 17.21 0.00 4 1 0 32.44 0.00 5 1 0 1.19 0.00 6 1 0 4.18 0.00 7 1 0 -0.50 0.00 8 1 0 -1.94 0.00 9 1 0 1.24 0.00 10 1 0 -2.81 0.00 11 1 0 0.01 0.00 12 1 0 -2.36 0.00 13 1 0 -0.92 0.00 14 1 0 -0.48 0.00 15 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-1.44 0.00 17 13 28 0.80 0.00 -3 15 28 -1.01 0.00 -2 16 28 1.59 0.00 -1 17 28 -0.16 0.00 15 17 28 -2.51 0.00 0 18 28 -0.43 0.00 3 20 28 0.81 0.00 12 20 28 0.32 0.00 5 21 28 1.15 0.00 6 21 28 -0.54 0.00 10 21 28 0.53 0.00 -2 -15 29 -0.40 0.00 -1 -15 29 -1.61 0.00 3 -15 29 -1.26 0.00 -5 -13 29 0.41 0.00 7 -13 29 2.09 0.00 -7 -10 29 -0.22 0.00 12 -8 29 -0.72 0.00 -8 -7 29 2.21 0.00 15 -2 29 -0.08 0.00 16 1 29 0.03 0.00 -8 2 29 0.93 0.00 -7 6 29 1.74 0.00 17 6 29 -1.28 0.00 17 7 29 1.44 0.00 17 8 29 0.24 0.00 17 9 29 -0.34 0.00 16 14 29 -1.10 0.00 -2 15 29 -1.35 0.00 -1 16 29 1.09 0.00 15 16 29 0.46 0.00 0 17 29 -0.85 0.00 1 18 29 0.37 0.00 3 19 29 -1.79 0.00 12 19 29 1.28 0.00 5 20 29 -1.47 0.00 10 20 29 -0.67 0.00 -1 -14 30 2.41 0.00 0 -14 30 0.97 0.00 2 -14 30 -0.70 0.00 3 -14 30 0.75 0.00 -3 -13 30 0.86 0.00 -4 -12 30 0.10 0.00 7 -12 30 -1.64 0.00 -5 -11 30 1.85 0.00 11 -8 30 -0.65 0.00 -7 -7 30 0.28 0.00 12 -7 30 0.90 0.00 13 -5 30 -0.44 0.00 14 -3 30 -1.03 0.00 15 -1 30 -0.30 0.00 -7 3 30 -0.21 0.00 16 3 30 -0.34 0.00 16 4 30 0.44 0.00 -5 9 30 0.65 0.00 16 10 30 2.24 0.00 -4 11 30 0.31 0.00 16 11 30 -2.04 0.00 16 12 30 0.97 0.00 15 14 30 0.40 0.00 -1 15 30 -0.31 0.00 0 16 30 1.51 0.00 14 16 30 -0.50 0.00 13 17 30 1.88 0.00 3 18 30 1.71 0.00 12 18 30 -1.38 0.00 5 19 30 1.50 0.00 10 19 30 1.16 0.00 0 -13 31 -1.48 0.00 1 -13 31 0.47 0.00 2 -13 31 1.31 0.00 -2 -12 31 -0.96 0.00 5 -12 31 2.43 0.00 7 -11 31 0.73 0.00 8 -10 31 -0.62 0.00 -5 -9 31 -0.93 0.00 10 -8 31 0.94 0.00 11 -7 31 -0.18 0.00 -6 -6 31 1.07 0.00 13 -4 31 0.25 0.00 14 -1 31 0.02 0.00 15 2 31 0.39 0.00 -6 3 31 0.60 0.00 -5 7 31 -2.74 0.00 -4 9 31 -1.78 0.00 -3 11 31 -1.21 0.00 15 12 31 -0.20 0.00 14 14 31 -0.13 0.00 13 16 31 0.02 0.00 3 17 31 -0.54 0.00 12 17 31 0.80 0.00 5 18 31 -1.92 0.00 6 18 31 -2.45 0.00 10 18 31 0.12 0.00 -1 -11 32 0.16 0.00 4 -11 32 0.12 0.00 5 -11 32 -0.62 0.00 -2 -10 32 -0.17 0.00 8 -9 32 0.75 0.00 -4 -8 32 -0.87 0.00 9 -8 32 0.39 0.00 10 -7 32 -0.64 0.00 -5 -6 32 0.30 0.00 -5 -5 32 0.86 0.00 12 -4 32 0.65 0.00 13 -2 32 1.11 0.00 14 1 32 -0.48 0.00 -5 3 32 -3.37 0.00 15 5 32 0.19 0.00 15 6 32 -0.90 0.00 -4 7 32 -1.52 0.00 15 7 32 1.14 0.00 15 8 32 -1.69 0.00 -3 9 32 -0.28 0.00 -1 12 32 -2.10 0.00 14 12 32 -1.90 0.00 0 13 32 1.73 0.00 1 14 32 -0.98 0.00 13 14 32 0.33 0.00 2 15 32 -0.55 0.00 12 15 32 0.83 0.00 11 16 32 -1.98 0.00 6 17 32 -0.23 0.00 7 17 32 -2.38 0.00 8 17 32 -0.75 0.00 9 17 32 0.47 0.00 1 -10 33 0.40 0.00 2 -10 33 0.34 0.00 3 -10 33 -1.41 0.00 4 -10 33 -0.39 0.00 -1 -9 33 0.24 0.00 6 -9 33 -0.67 0.00 -2 -8 33 1.32 0.00 7 -8 33 -0.91 0.00 -3 -7 33 0.50 0.00 10 -5 33 -1.46 0.00 -4 -4 33 -1.05 0.00 11 -4 33 2.06 0.00 12 -2 33 1.75 0.00 13 0 33 0.46 0.00 13 1 33 -1.37 0.00 -4 2 33 1.61 0.00 -4 3 33 -3.45 0.00 14 4 33 2.57 0.00 14 5 33 -1.33 0.00 -3 6 33 -0.33 0.00 14 6 33 1.05 0.00 14 7 33 -1.00 0.00 14 8 33 0.54 0.00 14 9 33 -1.07 0.00 -1 10 33 -1.05 0.00 13 12 33 -0.74 0.00 3 14 33 0.23 0.00 4 15 33 0.82 0.00 10 15 33 -0.79 0.00 7 16 33 -0.49 0.00 8 16 33 0.50 0.00 1 -8 34 -0.66 0.00 2 -8 34 -0.83 0.00 3 -8 34 1.72 0.00 4 -8 34 0.63 0.00 5 -8 34 0.97 0.00 0 -7 34 -0.33 0.00 6 -7 34 -0.28 0.00 8 -6 34 -0.76 0.00 -2 -5 34 -0.42 0.00 9 -5 34 0.80 0.00 10 -3 34 -0.66 0.00 -3 -2 34 -0.92 0.00 11 -2 34 1.62 0.00 -3 -1 34 -1.23 0.00 11 -1 34 2.10 0.00 -3 0 34 1.39 0.00 -3 1 34 -1.35 0.00 12 1 34 0.71 0.00 -3 2 34 1.03 0.00 13 4 34 1.78 0.00 -2 5 34 -0.77 0.00 13 5 34 0.80 0.00 13 6 34 -1.13 0.00 13 7 34 0.61 0.00 -1 8 34 -0.08 0.00 13 8 34 0.22 0.00 0 9 34 0.04 0.00 1 11 34 -0.13 0.00 12 11 34 -1.92 0.00 2 12 34 0.82 0.00 11 12 34 0.65 0.00 4 13 34 -0.33 0.00 10 13 34 -0.44 0.00 5 14 34 2.36 0.00 6 14 34 0.59 0.00 7 14 34 1.94 0.00 8 14 34 -2.06 0.00 9 14 34 -0.70 0.00 2 -6 35 -0.29 0.00 3 -6 35 -1.39 0.00 4 -6 35 1.23 0.00 5 -6 35 1.05 0.00 1 -5 35 -0.42 0.00 6 -5 35 -0.06 0.00 0 -4 35 -0.16 0.00 -1 -3 35 -0.17 0.00 -1 -2 35 1.65 0.00 9 -2 35 1.03 0.00 -1 -1 35 -0.83 0.00 10 -1 35 1.21 0.00 10 0 35 0.52 0.00 11 1 35 0.25 0.00 -1 2 35 -1.50 0.00 11 2 35 -0.21 0.00 -1 3 35 0.54 0.00 11 3 35 -1.04 0.00 -1 4 35 -0.68 0.00 0 6 35 0.03 0.00 1 8 35 -0.92 0.00 11 8 35 0.26 0.00 2 9 35 0.08 0.00 11 9 35 0.44 0.00 4 11 35 -1.23 0.00 10 11 35 -0.91 0.00 5 12 35 1.54 0.00 6 12 35 0.03 0.00 7 12 35 -1.09 0.00 8 12 35 -1.21 0.00 9 12 35 -0.27 0.00 3 -3 36 -1.38 0.00 4 -3 36 -0.52 0.00 5 -3 36 -0.68 0.00 2 -2 36 -0.83 0.00 6 -2 36 -2.06 0.00 7 -2 36 0.27 0.00 1 -1 36 0.09 0.00 7 -1 36 1.95 0.00 8 -1 36 -3.27 0.00 1 0 36 0.68 0.00 8 0 36 0.50 0.00 1 1 36 -0.88 0.00 9 1 36 -0.46 0.00 1 2 36 2.42 0.00 9 2 36 1.18 0.00 1 3 36 -0.97 0.00 9 3 36 -0.90 0.00 1 4 36 1.68 0.00 10 4 36 0.16 0.00 2 5 36 -1.21 0.00 10 5 36 -0.20 0.00 2 6 36 -0.10 0.00 10 6 36 -1.98 0.00 3 7 36 -0.19 0.00 9 7 36 0.63 0.00 4 8 36 -0.93 0.00 9 8 36 -0.16 0.00 5 9 36 0.57 0.00 6 9 36 -0.10 0.00 7 9 36 -0.15 0.00 8 9 36 2.31 0.00 5 3 37 -0.99 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 110918) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.000 0.500 -0.000 816 266 ' ' 2 0.500 1.000 0.500 221 60 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 1.477 1 1 0 1.552 -1 -1 1 1.926 0 -1 1 1.357 -1 0 1 1.849 1 0 1 1.513 1 1 1 1.565 1 0 2 1.934 0 1 2 1.913 1 1 2 1.959 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL mks_037am P -1 R = 0.06 CELL 14.8630 20.3300 25.7120 83.60 75.26 72.57 SPGR P-1 # Solvent Accessible Volume = 1033 # Electrons Found in S.A.V. = 326 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.502 0.019 0.455 ! 4.72 eA-3 C102 0.478 0.955 0.461 ! 4.00 eA-3 C103 0.107 0.379 0.168 ! 3.83 eA-3 C104 0.462 0.986 0.491 ! 3.49 eA-3 C105 0.169 0.358 0.129 ! 3.32 eA-3 C106 0.559 0.052 0.480 ! 3.06 eA-3 C107 0.814 0.514 0.221 ! 2.75 eA-3 C108 0.200 0.388 0.024 ! 2.59 eA-3 C109 0.786 0.636 0.036 ! 2.31 eA-3 C110 0.126 0.392 0.080 ! 2.30 eA-3 C111 0.888 0.545 0.201 ! 2.30 eA-3 C112 0.721 0.624 0.070 ! 2.20 eA-3 C113 0.159 0.362 0.073 ! 2.03 eA-3 C114 0.062 0.421 0.203 ! 1.99 eA-3 C115 0.915 0.561 0.147 ! 1.96 eA-3 C116 0.771 0.529 0.181 ! 1.92 eA-3 Q117 0.988 0.325 0.483 ! 1.83 eA-3 C118 0.919 0.497 0.120 ! 1.82 eA-3 C119 0.848 0.580 0.017 ! 1.75 eA-3 C120 0.846 0.637 0.041 ! 1.74 eA-3 C121 0.877 0.465 0.150 ! 1.72 eA-3 C122 0.192 0.340 0.002 ! 1.70 eA-3 C123 0.981 0.451 0.178 ! 1.61 eA-3 C124 0.114 0.394 0.114 ! 1.56 eA-3 C125 0.862 0.518 0.164 ! 1.55 eA-3 C126 0.774 0.593 0.017 ! 1.55 eA-3 C127 0.023 0.440 0.112 ! 1.49 eA-3 C128 0.545 0.125 0.474 ! 1.48 eA-3 C129 0.870 0.499 0.136 ! 1.45 eA-3 C130 0.842 0.556 0.132 ! 1.37 eA-3 C131 0.897 0.543 0.147 ! 1.37 eA-3 C132 0.767 0.549 0.149 ! 1.28 eA-3 C133 0.999 0.426 0.159 ! 1.26 eA-3 Q134 0.108 0.754 0.288 ! 1.24 eA-3 Q135 0.999 0.425 0.455 ! 1.21 eA-3 C136 0.182 0.419 0.066 ! 1.12 eA-3 C137 0.156 0.469 0.011 ! 1.12 eA-3 C138 0.261 0.408 0.024 ! 1.08 eA-3 C139 0.840 0.541 0.070 ! 1.06 eA-3 C140 0.177 0.314 0.035 ! 1.06 eA-3 Q141 0.982 0.312 0.454 ! 1.02 eA-3 Q142 0.535 0.190 0.345 ! 1.02 eA-3 Q143 0.220 0.660 0.407 ! 1.02 eA-3 Q144 0.064 0.704 0.433 ! 1.02 eA-3 C145 0.151 0.450 0.053 ! 1.01 eA-3 C146 0.948 0.502 0.164 ! 0.97 eA-3 C147 0.893 0.546 0.080 ! 0.97 eA-3 C148 0.033 0.374 0.147 ! 0.94 eA-3 C149 0.837 0.546 0.099 ! 0.93 eA-3 Q150 0.200 0.687 0.304 ! 0.92 eA-3 Q151 0.267 0.684 0.291 ! 0.91 eA-3 Q152 0.627 0.018 0.169 ! 0.89 eA-3 C153 0.750 0.668 0.060 ! 0.89 eA-3 C154 0.923 0.610 0.109 ! 0.89 eA-3 Q155 0.564 0.996 0.227 ! 0.88 eA-3 C156 0.875 0.607 0.084 ! 0.88 eA-3 C157 0.032 0.386 0.179 ! 0.88 eA-3 C158 0.919 0.421 0.127 ! 0.87 eA-3 Q159 0.251 0.343 0.110 ! 0.86 eA-3 C160 1.000 0.500 0.000 ! 0.86 eA-3 C161 0.915 0.500 0.090 ! 0.86 eA-3 Q162 0.730 0.177 0.080 ! 0.86 eA-3 Q163 0.737 0.156 0.051 ! 0.86 eA-3 C164 0.903 0.612 0.058 ! 0.85 eA-3 C165 0.711 0.545 0.182 ! 0.83 eA-3 C166 0.913 0.519 0.010 ! 0.83 eA-3 C167 0.046 0.445 0.074 ! 0.83 eA-3 C168 0.516 1.010 0.417 ! 0.82 eA-3 C169 0.427 0.034 0.449 ! 0.81 eA-3 C170 0.969 0.471 0.090 ! 0.81 eA-3 Q171 0.123 0.143 0.485 ! 0.79 eA-3 C172 0.799 0.517 0.113 ! 0.78 eA-3 C173 1.000 0.455 0.053 ! 0.78 eA-3 C174 0.724 0.548 0.232 ! 0.78 eA-3 C175 0.017 0.536 0.062 ! 0.78 eA-3 C176 0.934 0.538 0.017 ! 0.78 eA-3 C177 0.124 0.349 0.016 ! 0.77 eA-3 Q178 0.705 0.361 0.156 ! 0.77 eA-3 C179 0.082 0.483 0.061 ! 0.76 eA-3 Q180 0.128 0.559 0.031 ! 0.76 eA-3 Q181 0.816 0.264 0.134 ! 0.76 eA-3 Q182 0.083 0.708 0.492 ! 0.76 eA-3 Q183 0.795 0.173 0.034 ! 0.76 eA-3 C184 0.770 0.554 0.026 ! 0.76 eA-3 Q185 0.719 0.504 0.235 ! 0.75 eA-3 C186 0.846 0.593 0.153 ! 0.75 eA-3 C187 0.932 0.597 0.018 ! 0.74 eA-3 C188 0.063 0.453 0.045 ! 0.74 eA-3 C189 0.963 0.529 0.108 ! 0.74 eA-3 C190 0.970 0.462 0.227 ! 0.74 eA-3 C191 0.021 0.486 0.078 ! 0.73 eA-3 C192 0.015 0.543 0.105 ! 0.72 eA-3 Q193 0.562 0.985 0.200 ! 0.72 eA-3 C194 0.884 0.638 0.083 ! 0.72 eA-3 C195 0.983 0.512 0.142 ! 0.72 eA-3 C196 0.139 0.436 0.145 ! 0.71 eA-3 Q197 0.999 0.203 0.124 ! 0.71 eA-3 C198 0.816 0.638 0.107 ! 0.71 eA-3 C199 0.077 0.426 0.048 ! 0.71 eA-3 ) ; _shelx_fab_checksum 49399 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_077m_sq _database_code_depnum_ccdc_archive 'CCDC 2184020' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H95 B Br2 F20 Ga2 N6 P2' _chemical_formula_weight 2000.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5498(4) _cell_length_b 16.6890(7) _cell_length_c 23.2672(9) _cell_angle_alpha 77.921(2) _cell_angle_beta 77.403(2) _cell_angle_gamma 87.595(2) _cell_volume 4650.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9759 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 74.40 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_F_000 2036 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.144 _exptl_crystal_size_mid 0.124 _exptl_crystal_size_min 0.015 _exptl_absorpt_coefficient_mu 2.789 _shelx_estimated_absorpt_T_min 0.690 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 Crystal faces: H K L d(mm) 0.000 0.000 -1.000 0.00700 0.000 0.000 1.000 0.00700 0.000 1.000 -1.000 0.03900 -1.000 1.000 1.000 0.05600 1.000 -1.000 -1.000 0.06500 -1.000 -1.000 1.000 0.03800 0.000 -1.000 0.000 0.05900 0.000 1.000 0.000 0.05200 -1.000 -1.000 0.000 0.04600 1.000 1.000 0.000 0.04600 -1.000 0.000 0.000 0.05500 1.000 -1.000 0.000 0.07000 -1.000 1.000 0.000 0.06000 13 Faces + 22 Corners = 33 Edges + 2 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 Venture (Photon II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/Queen' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 234649 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_av_R_equivalents 0.1279 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.988 _diffrn_reflns_theta_max 75.216 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 19037 _reflns_number_gt 14631 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX3(v2017.3-0)' _computing_cell_refinement 'Bruker APEX3(v2017.3-0)' _computing_data_reduction 'Bruker APEX3(v2017.3-0)' _computing_structure_solution 'Bruker APEX3(v2017.3-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The PH hydrogen atoms could not be identified in the residual electron density. Their positions were taken form the isomorphous chloro compound. The H atom of the larger disorder component was refined freely, the co-ordinates of the one of the smaller were refined by a riding model (AFIX 3) and its displacement parameter was refined freely. The P--H bond lengths were restrained to be equal to 1.42\,\AA{} (DFIX). The proper assignment of these hydrogen atoms should be confirmed by other means. Disorder: The central Ga(Br)--PH--P(carbene)--Ga(Br) moiety is disordered over two positions. The corresponding bond lengths of the carbene were restrained to be equal (SADI) and RIGU restraints were applied to its displacement parameters. For atoms in close proximity additional SIMU restraints were used. The alternate positions of N5 were refined with common displacement parameters (EADP). SQUEEZE: The structure contains highly disordered solvent - possibly fluoro benzene or toluene. The final refinement was done with a solvent free dataset from a PLATON/SQUEEZE run. (For details see: A.~L.~Spek, Acta Cryst. A46 (1990),194--201). Since the nature and amount of the solvent is not clear it was not included in the sum formula. Weak data: The crystal was a very thin plate and diffracted rather poorly, esp. at higher angles. In addition, the highly anisotropic shape of the crystal hampered the absorption correction. This leads to a rather high $R_{int}$. Due to the weak data quantitative results should be carefully scrutinised and my be unreliable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+30.0612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 19037 _refine_ls_number_parameters 1263 _refine_ls_number_restraints 195 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1684 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.70675(19) 0.81283(12) 0.39178(11) 0.0271(4) Uani 0.731(3) 1 d . . P A 1 Ga2 Ga 0.8217(2) 0.82495(12) 0.14183(12) 0.0239(4) Uani 0.731(3) 1 d . . P A 1 Br1 Br 0.54397(9) 0.88607(7) 0.41549(7) 0.0352(3) Uani 0.731(3) 1 d . . P A 1 Br2 Br 0.96566(10) 0.91543(8) 0.13373(8) 0.0348(3) Uani 0.731(3) 1 d . . P A 1 P1 P 0.80593(15) 0.83827(12) 0.29078(9) 0.0264(5) Uani 0.731(3) 1 d . . P A 1 P2 P 0.71476(16) 0.77998(13) 0.23837(9) 0.0288(5) Uani 0.731(3) 1 d D . P A 1 H2A H 0.782(11) 0.710(6) 0.245(8) 0.15(6) Uiso 0.731(3) 1 d D . P A 1 N5 N 0.8562(6) 1.0040(5) 0.2587(4) 0.0345(18) Uani 0.731(3) 1 d D . P A 1 N6 N 0.6857(6) 0.9883(5) 0.2593(4) 0.0263(18) Uani 0.731(3) 1 d D . P A 1 C59 C 0.7774(6) 0.9476(5) 0.2698(4) 0.0274(16) Uani 0.731(3) 1 d D . P A 1 C60 C 0.8118(11) 1.0817(7) 0.2472(10) 0.037(4) Uani 0.731(3) 1 d D U P A 1 C61 C 0.7062(11) 1.0723(7) 0.2450(14) 0.038(3) Uani 0.731(3) 1 d D U P A 1 C62 C 0.9695(7) 0.9893(7) 0.2626(5) 0.046(3) Uani 0.731(3) 1 d D . P A 1 H62A H 1.017217 1.016298 0.224889 0.070 Uiso 0.731(3) 1 calc R U P A 1 H62B H 0.983522 0.930233 0.269707 0.070 Uiso 0.731(3) 1 calc R U P A 1 H62C H 0.984152 1.011472 0.295962 0.070 Uiso 0.731(3) 1 calc R U P A 1 C63 C 0.5792(6) 0.9559(5) 0.2616(4) 0.0327(18) Uani 0.731(3) 1 d D . P A 1 H63A H 0.562661 0.969536 0.221428 0.049 Uiso 0.731(3) 1 calc R U P A 1 H63B H 0.523672 0.979912 0.289691 0.049 Uiso 0.731(3) 1 calc R U P A 1 H63C H 0.579100 0.896190 0.275291 0.049 Uiso 0.731(3) 1 calc R U P A 1 C64 C 0.8805(15) 1.1576(8) 0.2300(12) 0.071(5) Uani 0.731(3) 1 d D . P A 1 H64A H 0.944209 1.150986 0.198452 0.106 Uiso 0.731(3) 1 calc R U P A 1 H64B H 0.904940 1.167050 0.265273 0.106 Uiso 0.731(3) 1 calc R U P A 1 H64C H 0.837438 1.204558 0.214964 0.106 Uiso 0.731(3) 1 calc R U P A 1 C65 C 0.6219(12) 1.1352(7) 0.2315(8) 0.053(4) Uani 0.731(3) 1 d D . P A 1 H65A H 0.657034 1.188984 0.215360 0.080 Uiso 0.731(3) 1 calc R U P A 1 H65B H 0.567591 1.137244 0.268436 0.080 Uiso 0.731(3) 1 calc R U P A 1 H65C H 0.585831 1.120673 0.201676 0.080 Uiso 0.731(3) 1 calc R U P A 1 Ga1' Ga 0.7201(5) 0.7848(4) 0.3879(3) 0.0298(12) Uani 0.269(3) 1 d . . P A 2 Ga2' Ga 0.8295(6) 0.8534(3) 0.1338(3) 0.0223(11) Uani 0.269(3) 1 d . . P A 2 Br1' Br 0.5669(2) 0.87188(19) 0.38752(19) 0.0373(8) Uani 0.269(3) 1 d . . P A 2 Br2' Br 0.9860(3) 0.9385(2) 0.1059(2) 0.0354(8) Uani 0.269(3) 1 d . . P A 2 P1' P 0.8223(4) 0.7688(3) 0.2940(2) 0.0296(14) Uani 0.269(3) 1 d D . P A 2 P2' P 0.7274(4) 0.8466(3) 0.2341(2) 0.0233(13) Uani 0.269(3) 1 d . . P A 2 H2A' H 0.760280 0.698015 0.297345 0.4(6) Uiso 0.269(3) 1 d DR . P A 2 N6' N 0.6743(15) 1.0095(13) 0.2407(11) 0.025(5) Uani 0.269(3) 1 d D . P A 2 N5' N 0.8407(17) 0.9894(16) 0.2466(15) 0.0345(18) Uani 0.269(3) 1 d D . P A 2 C59' C 0.7519(15) 0.9522(11) 0.2427(11) 0.026(4) Uani 0.269(3) 1 d D . P A 2 C60' C 0.823(3) 1.0734(17) 0.236(3) 0.033(7) Uani 0.269(3) 1 d D U P A 2 C61' C 0.715(3) 1.0866(16) 0.239(4) 0.033(7) Uani 0.269(3) 1 d D U P A 2 C62' C 0.9465(19) 0.9542(19) 0.2523(13) 0.045(6) Uani 0.269(3) 1 d D . P A 2 H62D H 1.004055 0.993568 0.229699 0.068 Uiso 0.269(3) 1 calc R U P A 2 H62E H 0.956214 0.903952 0.236212 0.068 Uiso 0.269(3) 1 calc R U P A 2 H62F H 0.950608 0.941220 0.294824 0.068 Uiso 0.269(3) 1 calc R U P A 2 C63' C 0.5591(15) 0.9948(16) 0.2424(11) 0.032(5) Uani 0.269(3) 1 d D . P A 2 H63D H 0.534893 1.035241 0.210862 0.049 Uiso 0.269(3) 1 calc R U P A 2 H63E H 0.514954 0.999860 0.281817 0.049 Uiso 0.269(3) 1 calc R U P A 2 H63F H 0.550581 0.939568 0.235835 0.049 Uiso 0.269(3) 1 calc R U P A 2 C64' C 0.903(4) 1.1336(17) 0.243(3) 0.048(10) Uani 0.269(3) 1 d D . P A 2 H64D H 0.958620 1.147506 0.205728 0.073 Uiso 0.269(3) 1 calc R U P A 2 H64E H 0.938065 1.109045 0.276275 0.073 Uiso 0.269(3) 1 calc R U P A 2 H64F H 0.864197 1.183324 0.251704 0.073 Uiso 0.269(3) 1 calc R U P A 2 C65' C 0.642(3) 1.1601(17) 0.240(2) 0.039(7) Uani 0.269(3) 1 d D . P A 2 H65D H 0.686111 1.209617 0.232274 0.059 Uiso 0.269(3) 1 calc R U P A 2 H65E H 0.591449 1.154170 0.279123 0.059 Uiso 0.269(3) 1 calc R U P A 2 H65F H 0.599524 1.164655 0.208343 0.059 Uiso 0.269(3) 1 calc R U P A 2 N1 N 0.6693(4) 0.6966(4) 0.4342(2) 0.0378(12) Uani 1 1 d . . . . . N2 N 0.7964(4) 0.8341(4) 0.4438(2) 0.0396(13) Uani 1 1 d . . . . . N3 N 0.8836(4) 0.7404(3) 0.1049(2) 0.0344(11) Uani 1 1 d . . . . . N4 N 0.7459(4) 0.8840(4) 0.0779(2) 0.0385(12) Uani 1 1 d . . . . . C1 C 0.6571(5) 0.6807(4) 0.4943(3) 0.0410(15) Uani 1 1 d . . . . . C2 C 0.6940(5) 0.7332(4) 0.5249(3) 0.0421(15) Uani 1 1 d . . . . . H2 H 0.666199 0.722109 0.567134 0.051 Uiso 1 1 calc R U . . . C3 C 0.7655(5) 0.7994(5) 0.5032(3) 0.0429(16) Uani 1 1 d . . . . . C4 C 0.6044(6) 0.6020(4) 0.5298(3) 0.0536(19) Uani 1 1 d . . . . . H4A H 0.538768 0.592766 0.515661 0.080 Uiso 1 1 calc R U . . . H4B H 0.584301 0.604670 0.572457 0.080 Uiso 1 1 calc R U . . . H4C H 0.655633 0.556762 0.524545 0.080 Uiso 1 1 calc R U . . . C5 C 0.8119(6) 0.8322(5) 0.5480(3) 0.0510(18) Uani 1 1 d . . . . . H5A H 0.891563 0.835723 0.535038 0.077 Uiso 1 1 calc R U . . . H5B H 0.792201 0.795430 0.587528 0.077 Uiso 1 1 calc R U . . . H5C H 0.782121 0.886849 0.550733 0.077 Uiso 1 1 calc R U . . . C6 C 0.6512(5) 0.6317(5) 0.4048(3) 0.0430(16) Uani 1 1 d . . . . . C7 C 0.5508(5) 0.6241(5) 0.3896(3) 0.0449(16) Uani 1 1 d . . . . . C8 C 0.5387(6) 0.5632(5) 0.3599(3) 0.0530(19) Uani 1 1 d . . . . . H8 H 0.471232 0.558262 0.348663 0.064 Uiso 1 1 calc R U . . . C9 C 0.6215(6) 0.5089(5) 0.3458(4) 0.059(2) Uani 1 1 d . . . . . H9 H 0.610894 0.466919 0.325634 0.071 Uiso 1 1 calc R U . . . C10 C 0.7204(6) 0.5165(5) 0.3616(4) 0.058(2) Uani 1 1 d . . . . . H10 H 0.777602 0.479252 0.351965 0.070 Uiso 1 1 calc R U . . . C11 C 0.7377(5) 0.5767(5) 0.3908(3) 0.0475(17) Uani 1 1 d . . . . . C12 C 0.4547(5) 0.6799(4) 0.4049(3) 0.0455(16) Uani 1 1 d . . . . . H12 H 0.475542 0.717360 0.429060 0.055 Uiso 1 1 calc R U . . . C13 C 0.3545(5) 0.6304(5) 0.4427(4) 0.0541(19) Uani 1 1 d . . . . . H13A H 0.326799 0.598786 0.417944 0.081 Uiso 1 1 calc R U . . . H13B H 0.297644 0.667708 0.457426 0.081 Uiso 1 1 calc R U . . . H13C H 0.374878 0.592831 0.476995 0.081 Uiso 1 1 calc R U . . . C14 C 0.4252(6) 0.7327(6) 0.3481(4) 0.065(2) Uani 1 1 d . . . . . H14A H 0.491509 0.758088 0.320935 0.097 Uiso 1 1 calc R U . . . H14B H 0.373932 0.775560 0.359423 0.097 Uiso 1 1 calc R U . . . H14C H 0.391203 0.698175 0.327796 0.097 Uiso 1 1 calc R U . . . C15 C 0.8479(6) 0.5839(5) 0.4067(3) 0.055(2) Uani 1 1 d . . . . . H15 H 0.844341 0.631046 0.427501 0.066 Uiso 1 1 calc R U . . . C16 C 0.9375(6) 0.6024(7) 0.3490(4) 0.085(3) Uani 1 1 d . . . . . H16A H 0.940347 0.557950 0.327085 0.128 Uiso 1 1 calc R U . . . H16B H 1.008131 0.607069 0.359490 0.128 Uiso 1 1 calc R U . . . H16C H 0.921039 0.654094 0.323569 0.128 Uiso 1 1 calc R U . . . C17 C 0.8744(7) 0.5067(6) 0.4495(5) 0.075(3) Uani 1 1 d . . . . . H17A H 0.876782 0.459478 0.430347 0.113 Uiso 1 1 calc R U . . . H17B H 0.817909 0.497711 0.486714 0.113 Uiso 1 1 calc R U . . . H17C H 0.945463 0.513351 0.458975 0.113 Uiso 1 1 calc R U . . . C18 C 0.8803(5) 0.8951(5) 0.4254(3) 0.0455(17) Uani 1 1 d . . . . . C19 C 0.8562(6) 0.9778(5) 0.4302(3) 0.0511(18) Uani 1 1 d . . . . . C20 C 0.9415(7) 1.0346(6) 0.4136(4) 0.063(2) Uani 1 1 d . . . . . H20 H 0.925850 1.090340 0.415355 0.075 Uiso 1 1 calc R U . . . C21 C 1.0483(7) 1.0115(6) 0.3947(4) 0.069(2) Uani 1 1 d . . . . . H21 H 1.105796 1.050582 0.385001 0.083 Uiso 1 1 calc R U . . . C22 C 1.0705(6) 0.9317(6) 0.3902(3) 0.062(2) Uani 1 1 d . . . . . H22 H 1.144318 0.916662 0.377041 0.074 Uiso 1 1 calc R U . . . C23 C 0.9895(5) 0.8710(5) 0.4041(3) 0.0463(17) Uani 1 1 d . . . . . C24 C 0.7407(6) 1.0066(5) 0.4526(3) 0.0513(18) Uani 1 1 d . . . . . H24 H 0.692143 0.957275 0.467639 0.062 Uiso 1 1 calc R U . . . C25 C 0.7000(6) 1.0612(5) 0.4010(3) 0.0554(19) Uani 1 1 d . . . . . H25A H 0.752442 1.105818 0.381660 0.083 Uiso 1 1 calc R U . . . H25B H 0.629031 1.084265 0.416431 0.083 Uiso 1 1 calc R U . . . H25C H 0.692324 1.028894 0.371443 0.083 Uiso 1 1 calc R U . . . C26 C 0.7354(7) 1.0504(6) 0.5044(4) 0.070(3) Uani 1 1 d . . . . . H26A H 0.784008 1.098212 0.490851 0.105 Uiso 1 1 calc R U . . . H26B H 0.758535 1.012829 0.537819 0.105 Uiso 1 1 calc R U . . . H26C H 0.660387 1.068178 0.517842 0.105 Uiso 1 1 calc R U . . . C27 C 1.0173(5) 0.7838(5) 0.3974(3) 0.0501(18) Uani 1 1 d . . . . . H27 H 0.952162 0.759524 0.388999 0.060 Uiso 1 1 calc R U . . . C28 C 1.1140(6) 0.7788(6) 0.3454(4) 0.063(2) Uani 1 1 d . . . . . H28A H 1.125071 0.721616 0.341135 0.094 Uiso 1 1 calc R U . . . H28B H 1.179887 0.799397 0.353574 0.094 Uiso 1 1 calc R U . . . H28C H 1.098885 0.812024 0.307997 0.094 Uiso 1 1 calc R U . . . C29 C 1.0419(8) 0.7311(7) 0.4560(4) 0.086(3) Uani 1 1 d . . . . . H29A H 1.061010 0.675423 0.450022 0.129 Uiso 1 1 calc R U . . . H29B H 0.977248 0.729114 0.488637 0.129 Uiso 1 1 calc R U . . . H29C H 1.103115 0.755322 0.466371 0.129 Uiso 1 1 calc R U . . . C30 C 0.9067(5) 0.7497(4) 0.0450(3) 0.0334(13) Uani 1 1 d . . . . . C31 C 0.8663(5) 0.8143(4) 0.0071(3) 0.0378(14) Uani 1 1 d . . . . . H31 H 0.898954 0.821146 -0.034473 0.045 Uiso 1 1 calc R U . . . C32 C 0.7841(5) 0.8705(4) 0.0222(3) 0.0397(15) Uani 1 1 d . . . . . C33 C 0.9789(6) 0.6885(4) 0.0165(3) 0.0434(15) Uani 1 1 d . . . . . H33A H 0.976983 0.697587 -0.026307 0.065 Uiso 1 1 calc R U . . . H33B H 0.952855 0.632956 0.036420 0.065 Uiso 1 1 calc R U . . . H33C H 1.053903 0.694944 0.020604 0.065 Uiso 1 1 calc R U . . . C34 C 0.7386(6) 0.9194(5) -0.0296(3) 0.060(2) Uani 1 1 d . . . . . H34A H 0.790477 0.962727 -0.052741 0.089 Uiso 1 1 calc R U . . . H34B H 0.668998 0.944009 -0.013828 0.089 Uiso 1 1 calc R U . . . H34C H 0.727029 0.883001 -0.055730 0.089 Uiso 1 1 calc R U . . . C35 C 0.9010(5) 0.6620(4) 0.1423(3) 0.0364(14) Uani 1 1 d . . . . . C36 C 1.0006(5) 0.6452(4) 0.1609(3) 0.0333(13) Uani 1 1 d . . . . . C37 C 1.0113(5) 0.5702(4) 0.1982(3) 0.0393(14) Uani 1 1 d . . . . . H37 H 1.078448 0.557480 0.210538 0.047 Uiso 1 1 calc R U . . . C38 C 0.9271(6) 0.5131(5) 0.2181(3) 0.0474(17) Uani 1 1 d . . . . . H38 H 0.935431 0.462372 0.244272 0.057 Uiso 1 1 calc R U . . . C39 C 0.8293(6) 0.5325(5) 0.1985(3) 0.0521(19) Uani 1 1 d . . . . . H39 H 0.770637 0.494280 0.212420 0.063 Uiso 1 1 calc R U . . . C40 C 0.8152(5) 0.6043(5) 0.1603(3) 0.0428(16) Uani 1 1 d . . . . . C41 C 1.0949(4) 0.7058(4) 0.1426(3) 0.0337(13) Uani 1 1 d . . . . . H41 H 1.075432 0.753666 0.112886 0.040 Uiso 1 1 calc R U . . . C42 C 1.1106(5) 0.7369(5) 0.1973(3) 0.0467(17) Uani 1 1 d . . . . . H42A H 1.168372 0.778683 0.184772 0.070 Uiso 1 1 calc R U . . . H42B H 1.131392 0.691211 0.226684 0.070 Uiso 1 1 calc R U . . . H42C H 1.042299 0.760918 0.215600 0.070 Uiso 1 1 calc R U . . . C43 C 1.2015(5) 0.6700(4) 0.1130(3) 0.0423(15) Uani 1 1 d . . . . . H43A H 1.190051 0.648251 0.078753 0.063 Uiso 1 1 calc R U . . . H43B H 1.225274 0.625720 0.142295 0.063 Uiso 1 1 calc R U . . . H43C H 1.257540 0.712947 0.098812 0.063 Uiso 1 1 calc R U . . . C44 C 0.7092(6) 0.6205(5) 0.1377(4) 0.0539(19) Uani 1 1 d . . . . . H44 H 0.703718 0.680994 0.123055 0.065 Uiso 1 1 calc R U . . . C45 C 0.6087(6) 0.5935(6) 0.1873(4) 0.068(2) Uani 1 1 d . . . . . H45A H 0.542846 0.606271 0.171040 0.103 Uiso 1 1 calc R U . . . H45B H 0.606633 0.622469 0.220073 0.103 Uiso 1 1 calc R U . . . H45C H 0.612060 0.534307 0.202707 0.103 Uiso 1 1 calc R U . . . C46 C 0.7119(7) 0.5792(5) 0.0842(4) 0.061(2) Uani 1 1 d . . . . . H46A H 0.641667 0.587190 0.071968 0.092 Uiso 1 1 calc R U . . . H46B H 0.725552 0.520465 0.096088 0.092 Uiso 1 1 calc R U . . . H46C H 0.770336 0.603711 0.050461 0.092 Uiso 1 1 calc R U . . . C47 C 0.6575(5) 0.9395(5) 0.0891(3) 0.0411(16) Uani 1 1 d . . . . . C48 C 0.6785(5) 1.0257(5) 0.0745(3) 0.0450(17) Uani 1 1 d . . . . . C49 C 0.5900(6) 1.0787(5) 0.0857(3) 0.055(2) Uani 1 1 d . . . . . H49 H 0.602250 1.136196 0.076658 0.066 Uiso 1 1 calc R U . . . C50 C 0.4853(6) 1.0484(6) 0.1098(3) 0.058(2) Uani 1 1 d . . . . . H50 H 0.426102 1.085086 0.116599 0.069 Uiso 1 1 calc R U . . . C51 C 0.4666(5) 0.9646(5) 0.1240(3) 0.0497(19) Uani 1 1 d . . . . . H51 H 0.394354 0.944399 0.140633 0.060 Uiso 1 1 calc R U . . . C52 C 0.5515(5) 0.9096(5) 0.1144(3) 0.0436(16) Uani 1 1 d . . . . . C53 C 0.7910(6) 1.0640(5) 0.0455(3) 0.053(2) Uani 1 1 d . . . . . H53 H 0.844010 1.019699 0.036225 0.064 Uiso 1 1 calc R U . . . C54 C 0.8307(6) 1.1089(5) 0.0879(4) 0.069(3) Uani 1 1 d . . . . . H54A H 0.907964 1.123398 0.072112 0.103 Uiso 1 1 calc R U . . . H54B H 0.821760 1.073287 0.127834 0.103 Uiso 1 1 calc R U . . . H54C H 0.787822 1.158941 0.090791 0.103 Uiso 1 1 calc R U . . . C55 C 0.7882(8) 1.1261(6) -0.0130(4) 0.095(4) Uani 1 1 d . . . . . H55A H 0.862329 1.146011 -0.032452 0.142 Uiso 1 1 calc R U . . . H55B H 0.741496 1.172318 -0.003865 0.142 Uiso 1 1 calc R U . . . H55C H 0.758921 1.099554 -0.040142 0.142 Uiso 1 1 calc R U . . . C56 C 0.5284(5) 0.8178(5) 0.1282(3) 0.0491(18) Uani 1 1 d . . . . . H56 H 0.594029 0.789069 0.140291 0.059 Uiso 1 1 calc R U . . . C57 C 0.4308(6) 0.7917(6) 0.1800(4) 0.064(2) Uani 1 1 d . . . . . H57A H 0.363239 0.810412 0.166901 0.096 Uiso 1 1 calc R U . . . H57B H 0.437041 0.816124 0.213989 0.096 Uiso 1 1 calc R U . . . H57C H 0.429397 0.731869 0.192548 0.096 Uiso 1 1 calc R U . . . C58 C 0.5135(7) 0.7901(6) 0.0721(4) 0.066(2) Uani 1 1 d . . . . . H58A H 0.451747 0.819260 0.057853 0.099 Uiso 1 1 calc R U . . . H58B H 0.499092 0.730992 0.081806 0.099 Uiso 1 1 calc R U . . . H58C H 0.580013 0.802170 0.040621 0.099 Uiso 1 1 calc R U . . . F12_1 F 0.0587(2) 0.2862(2) 0.22216(15) 0.0322(7) Uani 1 1 d . . . . . F13_1 F -0.0900(3) 0.3500(2) 0.16102(18) 0.0428(9) Uani 1 1 d . . . . . F14_1 F -0.0359(3) 0.4716(2) 0.06263(18) 0.0478(10) Uani 1 1 d . . . . . F15_1 F 0.1758(3) 0.5236(2) 0.02272(16) 0.0415(8) Uani 1 1 d . . . . . F16_1 F 0.3285(3) 0.4552(2) 0.07889(16) 0.0380(8) Uani 1 1 d . . . . . F22_1 F 0.1468(3) 0.2754(2) 0.32296(15) 0.0405(8) Uani 1 1 d . . . . . F23_1 F 0.1002(3) 0.3687(3) 0.40421(18) 0.0608(12) Uani 1 1 d . . . . . F24_1 F 0.1830(4) 0.5235(3) 0.3803(2) 0.0676(14) Uani 1 1 d . . . . . F25_1 F 0.3071(4) 0.5852(2) 0.2698(2) 0.0616(12) Uani 1 1 d . . . . . F26_1 F 0.3533(3) 0.4943(2) 0.18622(17) 0.0427(9) Uani 1 1 d . . . . . F32_1 F 0.3759(3) 0.2856(2) 0.07899(16) 0.0404(8) Uani 1 1 d . . . . . F33_1 F 0.5825(3) 0.2893(3) 0.01995(18) 0.0534(10) Uani 1 1 d . . . . . F34_1 F 0.7446(3) 0.3306(2) 0.06909(19) 0.0525(11) Uani 1 1 d . . . . . F35_1 F 0.6920(3) 0.3723(2) 0.17894(19) 0.0494(10) Uani 1 1 d . . . . . F36_1 F 0.4879(3) 0.3768(2) 0.23666(16) 0.0401(8) Uani 1 1 d . . . . . F42_1 F 0.1905(3) 0.1952(2) 0.14623(16) 0.0378(8) Uani 1 1 d . . . . . F43_1 F 0.2034(3) 0.0354(2) 0.18210(18) 0.0449(9) Uani 1 1 d . . . . . F44_1 F 0.2931(3) -0.0300(2) 0.27833(19) 0.0552(11) Uani 1 1 d . . . . . F45_1 F 0.3708(3) 0.0714(2) 0.33754(17) 0.0518(10) Uani 1 1 d . . . . . F46_1 F 0.3694(3) 0.2326(2) 0.29884(15) 0.0394(8) Uani 1 1 d . . . . . C11_1 C 0.2028(4) 0.3642(3) 0.1533(2) 0.0256(11) Uani 1 1 d . . . . . C12_1 C 0.0935(4) 0.3432(3) 0.1710(2) 0.0267(11) Uani 1 1 d . . . . . C13_1 C 0.0142(4) 0.3764(3) 0.1408(3) 0.0295(12) Uani 1 1 d . . . . . C14_1 C 0.0408(5) 0.4380(4) 0.0905(3) 0.0341(13) Uani 1 1 d . . . . . C15_1 C 0.1476(5) 0.4625(4) 0.0714(3) 0.0316(12) Uani 1 1 d . . . . . C16_1 C 0.2259(4) 0.4267(3) 0.1021(3) 0.0301(12) Uani 1 1 d . . . . . C21_1 C 0.2579(4) 0.3784(4) 0.2502(3) 0.0308(13) Uani 1 1 d . . . . . C22_1 C 0.1908(5) 0.3525(4) 0.3064(3) 0.0361(14) Uani 1 1 d . . . . . C23_1 C 0.1646(5) 0.3988(5) 0.3503(3) 0.0434(16) Uani 1 1 d . . . . . C24_1 C 0.2049(6) 0.4771(5) 0.3379(3) 0.0497(19) Uani 1 1 d . . . . . C25_1 C 0.2681(5) 0.5082(4) 0.2826(3) 0.0435(16) Uani 1 1 d . . . . . C26_1 C 0.2925(5) 0.4602(4) 0.2397(3) 0.0374(14) Uani 1 1 d . . . . . C31_1 C 0.4179(4) 0.3337(3) 0.1604(3) 0.0285(12) Uani 1 1 d . . . . . C32_1 C 0.4513(5) 0.3112(4) 0.1050(3) 0.0340(13) Uani 1 1 d . . . . . C33_1 C 0.5575(5) 0.3112(4) 0.0740(3) 0.0393(14) Uani 1 1 d . . . . . C34_1 C 0.6402(5) 0.3324(4) 0.0981(3) 0.0390(15) Uani 1 1 d . . . . . C35_1 C 0.6124(5) 0.3537(4) 0.1533(3) 0.0374(14) Uani 1 1 d . . . . . C36_1 C 0.5045(5) 0.3544(4) 0.1828(3) 0.0324(13) Uani 1 1 d . . . . . C41_1 C 0.2775(4) 0.2256(3) 0.2211(2) 0.0272(11) Uani 1 1 d . . . . . C42_1 C 0.2365(4) 0.1694(4) 0.1942(3) 0.0326(13) Uani 1 1 d . . . . . C43_1 C 0.2415(5) 0.0853(4) 0.2125(3) 0.0367(14) Uani 1 1 d . . . . . C44_1 C 0.2867(5) 0.0524(4) 0.2603(3) 0.0399(15) Uani 1 1 d . . . . . C45_1 C 0.3261(5) 0.1039(4) 0.2897(3) 0.0395(15) Uani 1 1 d . . . . . C46_1 C 0.3232(5) 0.1872(4) 0.2693(3) 0.0326(13) Uani 1 1 d . . . . . B1_1 B 0.2886(5) 0.3259(4) 0.1960(3) 0.0257(13) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0193(7) 0.0378(11) 0.0263(7) -0.0112(7) -0.0056(5) 0.0056(7) Ga2 0.0214(6) 0.0270(10) 0.0216(9) -0.0034(8) -0.0033(6) 0.0035(9) Br1 0.0260(5) 0.0407(5) 0.0399(7) -0.0133(5) -0.0060(5) 0.0089(4) Br2 0.0311(5) 0.0316(6) 0.0414(7) -0.0132(5) -0.0009(5) -0.0026(4) P1 0.0207(9) 0.0340(12) 0.0263(10) -0.0090(8) -0.0063(7) 0.0005(8) P2 0.0271(10) 0.0331(12) 0.0263(10) -0.0079(8) -0.0031(8) -0.0059(8) N5 0.030(3) 0.036(4) 0.040(5) -0.014(3) -0.005(3) -0.004(2) N6 0.030(3) 0.020(4) 0.027(5) 0.000(3) -0.004(3) -0.003(3) C59 0.030(4) 0.032(4) 0.021(4) -0.007(3) -0.005(3) -0.003(3) C60 0.045(5) 0.034(4) 0.035(9) -0.016(4) -0.005(6) -0.007(3) C61 0.046(5) 0.023(5) 0.042(8) 0.002(6) -0.013(5) -0.006(4) C62 0.027(4) 0.058(7) 0.057(7) -0.024(5) 0.000(4) -0.011(4) C63 0.028(4) 0.030(5) 0.042(5) -0.007(4) -0.010(4) 0.000(3) C64 0.071(11) 0.043(8) 0.095(15) -0.014(10) -0.008(10) -0.024(8) C65 0.062(7) 0.021(6) 0.075(10) 0.002(6) -0.023(6) 0.001(6) Ga1' 0.0203(18) 0.048(3) 0.0198(16) -0.011(2) 0.0004(12) 0.008(2) Ga2' 0.0200(17) 0.025(3) 0.0157(18) 0.005(2) -0.0008(13) 0.005(2) Br1' 0.0285(13) 0.0418(15) 0.0393(19) -0.0055(13) -0.0073(13) 0.0128(11) Br2' 0.0287(14) 0.0286(15) 0.043(2) -0.0046(14) 0.0016(14) 0.0021(11) P1' 0.030(3) 0.033(3) 0.024(3) -0.007(2) -0.004(2) 0.015(2) P2' 0.016(2) 0.027(3) 0.027(3) -0.009(2) -0.0041(19) 0.0047(19) N6' 0.032(7) 0.015(8) 0.027(14) 0.006(8) -0.012(8) 0.002(5) N5' 0.030(3) 0.036(4) 0.040(5) -0.014(3) -0.005(3) -0.004(2) C59' 0.031(7) 0.017(7) 0.032(12) 0.001(8) -0.013(8) 0.001(5) C60' 0.039(8) 0.032(6) 0.028(18) -0.018(9) 0.005(9) -0.005(5) C61' 0.043(8) 0.017(8) 0.036(17) -0.002(11) -0.005(10) -0.004(6) C62' 0.038(9) 0.061(16) 0.041(15) -0.009(14) -0.020(11) 0.005(10) C63' 0.027(8) 0.034(13) 0.035(13) -0.008(11) -0.005(9) 0.001(8) C64' 0.048(15) 0.014(11) 0.09(3) -0.014(16) -0.024(16) 0.002(12) C65' 0.053(16) 0.020(12) 0.050(17) -0.005(13) -0.025(14) 0.005(11) N1 0.028(3) 0.060(3) 0.030(3) -0.020(2) -0.007(2) 0.008(2) N2 0.029(3) 0.066(4) 0.025(3) -0.012(2) -0.008(2) 0.004(2) N3 0.026(2) 0.046(3) 0.029(3) -0.002(2) -0.006(2) -0.006(2) N4 0.030(3) 0.058(3) 0.027(3) -0.009(2) -0.004(2) 0.008(2) C1 0.029(3) 0.054(4) 0.035(3) -0.002(3) -0.004(3) 0.013(3) C2 0.037(3) 0.059(4) 0.028(3) -0.008(3) -0.005(3) 0.009(3) C3 0.034(3) 0.066(5) 0.029(3) -0.011(3) -0.008(3) 0.015(3) C4 0.064(5) 0.050(4) 0.042(4) -0.006(3) -0.005(4) 0.010(4) C5 0.052(4) 0.076(5) 0.030(3) -0.017(3) -0.015(3) 0.005(4) C6 0.031(3) 0.067(5) 0.034(3) -0.019(3) -0.004(3) 0.004(3) C7 0.029(3) 0.070(5) 0.034(3) -0.011(3) -0.003(3) 0.000(3) C8 0.040(4) 0.072(5) 0.051(4) -0.018(4) -0.009(3) -0.007(4) C9 0.044(4) 0.076(6) 0.064(5) -0.034(4) -0.007(4) -0.001(4) C10 0.041(4) 0.077(6) 0.064(5) -0.034(4) -0.009(4) 0.011(4) C11 0.030(3) 0.070(5) 0.047(4) -0.027(4) -0.004(3) 0.005(3) C12 0.029(3) 0.049(4) 0.059(4) -0.009(3) -0.013(3) -0.003(3) C13 0.030(3) 0.058(5) 0.070(5) -0.011(4) -0.002(3) 0.001(3) C14 0.042(4) 0.080(6) 0.071(6) 0.004(5) -0.025(4) -0.008(4) C15 0.039(4) 0.079(6) 0.052(4) -0.032(4) -0.006(3) 0.013(4) C16 0.035(4) 0.154(10) 0.078(6) -0.061(7) -0.001(4) 0.005(5) C17 0.055(5) 0.070(6) 0.112(8) -0.032(6) -0.032(5) 0.011(4) C18 0.033(3) 0.079(5) 0.027(3) -0.013(3) -0.008(3) -0.004(3) C19 0.047(4) 0.074(5) 0.034(4) -0.013(4) -0.008(3) -0.002(4) C20 0.062(5) 0.067(5) 0.058(5) -0.021(4) -0.001(4) -0.005(4) C21 0.054(5) 0.091(7) 0.068(6) -0.030(5) -0.007(4) -0.014(5) C22 0.034(4) 0.105(7) 0.048(5) -0.017(5) -0.008(3) -0.007(4) C23 0.029(3) 0.080(5) 0.034(3) -0.016(3) -0.013(3) 0.004(3) C24 0.049(4) 0.067(5) 0.036(4) -0.013(3) -0.003(3) 0.007(4) C25 0.054(4) 0.065(5) 0.048(4) -0.010(4) -0.015(4) 0.012(4) C26 0.063(5) 0.105(7) 0.044(5) -0.028(5) -0.005(4) 0.014(5) C27 0.027(3) 0.082(6) 0.044(4) -0.014(4) -0.013(3) 0.008(3) C28 0.032(4) 0.101(7) 0.061(5) -0.036(5) -0.003(3) 0.004(4) C29 0.075(6) 0.122(9) 0.052(5) -0.007(5) -0.013(5) 0.052(6) C30 0.032(3) 0.040(3) 0.031(3) -0.013(3) -0.007(2) -0.003(3) C31 0.039(3) 0.048(4) 0.028(3) -0.012(3) -0.009(3) 0.009(3) C32 0.034(3) 0.060(4) 0.026(3) -0.010(3) -0.008(3) 0.006(3) C33 0.053(4) 0.040(4) 0.038(4) -0.008(3) -0.013(3) 0.006(3) C34 0.063(5) 0.090(6) 0.026(3) -0.013(4) -0.015(3) 0.038(4) C35 0.032(3) 0.045(4) 0.029(3) -0.002(3) -0.004(2) -0.004(3) C36 0.027(3) 0.044(3) 0.029(3) -0.010(3) -0.003(2) 0.001(3) C37 0.035(3) 0.048(4) 0.035(3) -0.009(3) -0.007(3) 0.002(3) C38 0.048(4) 0.059(4) 0.030(3) 0.003(3) -0.008(3) -0.009(3) C39 0.040(4) 0.075(5) 0.035(4) -0.001(3) 0.000(3) -0.022(4) C40 0.027(3) 0.061(4) 0.039(4) -0.007(3) -0.003(3) -0.012(3) C41 0.022(3) 0.039(3) 0.039(3) -0.008(3) -0.004(2) -0.001(2) C42 0.029(3) 0.056(4) 0.060(5) -0.022(4) -0.013(3) 0.008(3) C43 0.030(3) 0.048(4) 0.045(4) -0.009(3) 0.000(3) 0.006(3) C44 0.035(4) 0.062(5) 0.060(5) 0.008(4) -0.017(3) -0.013(3) C45 0.039(4) 0.074(6) 0.084(6) 0.004(5) -0.013(4) -0.014(4) C46 0.062(5) 0.064(5) 0.064(5) -0.009(4) -0.031(4) -0.006(4) C47 0.030(3) 0.071(5) 0.023(3) -0.011(3) -0.008(2) 0.008(3) C48 0.035(3) 0.064(5) 0.033(3) -0.012(3) 0.001(3) 0.014(3) C49 0.043(4) 0.079(6) 0.042(4) -0.023(4) 0.003(3) 0.019(4) C50 0.040(4) 0.090(6) 0.048(4) -0.030(4) -0.009(3) 0.026(4) C51 0.031(3) 0.088(6) 0.039(4) -0.034(4) -0.008(3) 0.009(4) C52 0.031(3) 0.075(5) 0.030(3) -0.018(3) -0.012(3) 0.006(3) C53 0.044(4) 0.049(4) 0.049(4) 0.003(3) 0.013(3) 0.016(3) C54 0.046(4) 0.048(5) 0.103(7) -0.024(5) 0.015(4) -0.005(4) C55 0.081(6) 0.100(8) 0.058(6) 0.029(5) 0.031(5) 0.043(6) C56 0.027(3) 0.074(5) 0.050(4) -0.015(4) -0.014(3) -0.003(3) C57 0.028(4) 0.092(7) 0.072(6) -0.017(5) -0.008(4) -0.006(4) C58 0.055(5) 0.088(6) 0.068(6) -0.035(5) -0.027(4) 0.005(4) F12_1 0.0241(16) 0.0344(18) 0.0350(18) -0.0008(14) -0.0057(13) 0.0010(13) F13_1 0.0197(16) 0.048(2) 0.061(2) -0.0037(18) -0.0166(16) 0.0025(15) F14_1 0.039(2) 0.049(2) 0.059(2) 0.0015(19) -0.0318(18) 0.0105(17) F15_1 0.049(2) 0.0372(19) 0.0356(19) 0.0038(15) -0.0141(16) 0.0005(16) F16_1 0.0267(17) 0.043(2) 0.041(2) 0.0011(16) -0.0079(15) -0.0049(15) F22_1 0.0386(19) 0.049(2) 0.0334(19) -0.0135(16) -0.0019(15) 0.0052(17) F23_1 0.056(3) 0.089(3) 0.041(2) -0.029(2) -0.0048(19) 0.021(2) F24_1 0.069(3) 0.085(3) 0.074(3) -0.056(3) -0.037(2) 0.034(3) F25_1 0.075(3) 0.040(2) 0.088(3) -0.030(2) -0.043(3) 0.012(2) F26_1 0.049(2) 0.0310(18) 0.050(2) -0.0052(16) -0.0187(18) 0.0008(16) F32_1 0.0286(17) 0.055(2) 0.041(2) -0.0207(17) -0.0035(15) 0.0000(16) F33_1 0.039(2) 0.068(3) 0.049(2) -0.021(2) 0.0089(18) 0.0045(19) F34_1 0.0213(17) 0.051(2) 0.068(3) 0.007(2) 0.0070(17) 0.0018(16) F35_1 0.0233(17) 0.055(2) 0.071(3) -0.004(2) -0.0212(18) -0.0022(16) F36_1 0.0306(18) 0.049(2) 0.048(2) -0.0139(17) -0.0192(16) 0.0049(16) F42_1 0.0349(18) 0.040(2) 0.044(2) -0.0170(16) -0.0130(16) 0.0027(15) F43_1 0.039(2) 0.037(2) 0.055(2) -0.0183(18) 0.0048(17) -0.0050(16) F44_1 0.061(3) 0.0293(19) 0.059(3) 0.0031(18) 0.010(2) 0.0051(18) F45_1 0.059(2) 0.049(2) 0.038(2) 0.0043(17) -0.0085(18) 0.023(2) F46_1 0.0365(19) 0.048(2) 0.0362(19) -0.0092(16) -0.0147(15) 0.0110(16) C11_1 0.022(3) 0.029(3) 0.029(3) -0.011(2) -0.009(2) 0.004(2) C12_1 0.025(3) 0.030(3) 0.026(3) -0.005(2) -0.008(2) 0.003(2) C13_1 0.022(3) 0.029(3) 0.038(3) -0.008(2) -0.008(2) 0.002(2) C14_1 0.030(3) 0.037(3) 0.042(3) -0.013(3) -0.021(3) 0.013(3) C15_1 0.034(3) 0.033(3) 0.028(3) -0.003(2) -0.011(2) -0.002(2) C16_1 0.026(3) 0.030(3) 0.034(3) -0.005(2) -0.006(2) -0.003(2) C21_1 0.025(3) 0.036(3) 0.037(3) -0.013(3) -0.018(2) 0.015(2) C22_1 0.030(3) 0.041(3) 0.041(4) -0.013(3) -0.012(3) 0.011(3) C23_1 0.034(3) 0.061(5) 0.039(4) -0.019(3) -0.012(3) 0.018(3) C24_1 0.049(4) 0.062(5) 0.055(4) -0.038(4) -0.029(4) 0.030(4) C25_1 0.042(4) 0.042(4) 0.060(4) -0.022(3) -0.031(3) 0.018(3) C26_1 0.033(3) 0.035(3) 0.053(4) -0.016(3) -0.023(3) 0.012(3) C31_1 0.020(3) 0.030(3) 0.037(3) -0.007(2) -0.009(2) 0.002(2) C32_1 0.024(3) 0.039(3) 0.039(3) -0.009(3) -0.004(2) 0.000(2) C33_1 0.031(3) 0.043(4) 0.042(4) -0.008(3) -0.005(3) 0.005(3) C34_1 0.019(3) 0.037(3) 0.052(4) 0.002(3) 0.000(3) 0.000(2) C35_1 0.022(3) 0.037(3) 0.053(4) 0.001(3) -0.015(3) 0.001(2) C36_1 0.027(3) 0.035(3) 0.037(3) -0.006(3) -0.014(2) 0.007(2) C41_1 0.019(2) 0.034(3) 0.025(3) -0.004(2) 0.000(2) 0.003(2) C42_1 0.023(3) 0.036(3) 0.036(3) -0.009(3) -0.001(2) 0.006(2) C43_1 0.028(3) 0.036(3) 0.043(4) -0.014(3) 0.002(3) 0.003(3) C44_1 0.039(3) 0.027(3) 0.041(4) 0.000(3) 0.009(3) 0.006(3) C45_1 0.033(3) 0.043(4) 0.032(3) 0.006(3) 0.001(3) 0.012(3) C46_1 0.025(3) 0.042(3) 0.028(3) -0.007(3) -0.003(2) 0.006(2) B1_1 0.020(3) 0.028(3) 0.030(3) -0.007(3) -0.007(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2 1.914(5) . ? Ga1 N1 2.007(6) . ? Ga1 Br1 2.356(2) . ? Ga1 P1 2.367(3) . ? Ga2 N3 1.859(6) . ? Ga2 N4 2.004(6) . ? Ga2 P2 2.339(3) . ? Ga2 Br2 2.354(2) . ? P1 C59 1.829(8) . ? P1 P2 2.223(3) . ? N5 C59 1.340(10) . ? N5 C60 1.387(10) . ? N5 C62 1.452(9) . ? N6 C59 1.354(9) . ? N6 C61 1.391(10) . ? N6 C63 1.450(9) . ? C60 C61 1.354(12) . ? C60 C64 1.496(12) . ? C61 C65 1.496(11) . ? Ga1' N1 1.688(9) . ? Ga1' N2 2.084(8) . ? Ga1' P1' 2.342(7) . ? Ga1' Br1' 2.361(6) . ? Ga2' N4 1.823(8) . ? Ga2' N3 2.166(8) . ? Ga2' Br2' 2.365(7) . ? Ga2' P2' 2.386(9) . ? P1' P2' 2.211(7) . ? P2' C59' 1.86(2) . ? N6' C59' 1.337(15) . ? N6' C61' 1.392(16) . ? N6' C63' 1.466(15) . ? N5' C59' 1.327(15) . ? N5' C60' 1.388(16) . ? N5' C62' 1.451(16) . ? C60' C61' 1.359(18) . ? C60' C64' 1.504(17) . ? C61' C65' 1.502(17) . ? N1 C1 1.342(8) . ? N1 C6 1.445(8) . ? N2 C3 1.358(8) . ? N2 C18 1.427(9) . ? N3 C30 1.337(7) . ? N3 C35 1.449(8) . ? N4 C32 1.341(7) . ? N4 C47 1.430(8) . ? C1 C2 1.389(10) . ? C1 C4 1.492(10) . ? C2 C3 1.391(10) . ? C3 C5 1.503(9) . ? C6 C7 1.398(9) . ? C6 C11 1.420(9) . ? C7 C8 1.374(10) . ? C7 C12 1.518(9) . ? C8 C9 1.380(10) . ? C9 C10 1.387(10) . ? C10 C11 1.373(10) . ? C11 C15 1.523(9) . ? C12 C13 1.530(9) . ? C12 C14 1.535(10) . ? C15 C17 1.528(12) . ? C15 C16 1.537(11) . ? C18 C19 1.422(11) . ? C18 C23 1.423(9) . ? C19 C20 1.395(11) . ? C19 C24 1.524(10) . ? C20 C21 1.381(11) . ? C21 C22 1.371(13) . ? C22 C23 1.404(11) . ? C23 C27 1.515(11) . ? C24 C25 1.518(10) . ? C24 C26 1.524(10) . ? C27 C28 1.529(9) . ? C27 C29 1.544(10) . ? C30 C31 1.395(8) . ? C30 C33 1.500(8) . ? C31 C32 1.403(8) . ? C32 C34 1.514(8) . ? C35 C40 1.407(9) . ? C35 C36 1.408(8) . ? C36 C37 1.387(9) . ? C36 C41 1.518(8) . ? C37 C38 1.388(9) . ? C38 C39 1.403(10) . ? C39 C40 1.366(10) . ? C40 C44 1.527(9) . ? C41 C43 1.525(8) . ? C41 C42 1.525(9) . ? C44 C45 1.523(10) . ? C44 C46 1.538(11) . ? C47 C52 1.398(9) . ? C47 C48 1.430(10) . ? C48 C49 1.404(9) . ? C48 C53 1.528(10) . ? C49 C50 1.383(11) . ? C50 C51 1.386(11) . ? C51 C52 1.389(9) . ? C52 C56 1.526(11) . ? C53 C54 1.529(12) . ? C53 C55 1.534(10) . ? C56 C58 1.522(10) . ? C56 C57 1.525(10) . ? F12_1 C12_1 1.358(6) . ? F13_1 C13_1 1.349(6) . ? F14_1 C14_1 1.319(6) . ? F15_1 C15_1 1.349(6) . ? F16_1 C16_1 1.348(6) . ? F22_1 C22_1 1.367(7) . ? F23_1 C23_1 1.345(8) . ? F24_1 C24_1 1.354(7) . ? F25_1 C25_1 1.345(8) . ? F26_1 C26_1 1.335(8) . ? F32_1 C32_1 1.356(7) . ? F33_1 C33_1 1.350(7) . ? F34_1 C34_1 1.338(6) . ? F35_1 C35_1 1.348(7) . ? F36_1 C36_1 1.352(7) . ? F42_1 C42_1 1.351(7) . ? F43_1 C43_1 1.360(7) . ? F44_1 C44_1 1.355(7) . ? F45_1 C45_1 1.357(7) . ? F46_1 C46_1 1.346(7) . ? C11_1 C12_1 1.381(7) . ? C11_1 C16_1 1.395(8) . ? C11_1 B1_1 1.643(8) . ? C12_1 C13_1 1.374(7) . ? C13_1 C14_1 1.375(8) . ? C14_1 C15_1 1.367(8) . ? C15_1 C16_1 1.382(8) . ? C21_1 C22_1 1.386(9) . ? C21_1 C26_1 1.404(9) . ? C21_1 B1_1 1.653(8) . ? C22_1 C23_1 1.381(9) . ? C23_1 C24_1 1.372(11) . ? C24_1 C25_1 1.365(11) . ? C25_1 C26_1 1.383(9) . ? C31_1 C36_1 1.388(8) . ? C31_1 C32_1 1.391(8) . ? C31_1 B1_1 1.649(8) . ? C32_1 C33_1 1.370(8) . ? C33_1 C34_1 1.373(9) . ? C34_1 C35_1 1.373(9) . ? C35_1 C36_1 1.378(8) . ? C41_1 C46_1 1.395(8) . ? C41_1 C42_1 1.400(8) . ? C41_1 B1_1 1.655(8) . ? C42_1 C43_1 1.382(8) . ? C43_1 C44_1 1.362(9) . ? C44_1 C45_1 1.372(10) . ? C45_1 C46_1 1.374(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 96.3(2) . . ? N2 Ga1 Br1 105.73(17) . . ? N1 Ga1 Br1 104.58(17) . . ? N2 Ga1 P1 110.26(19) . . ? N1 Ga1 P1 118.78(17) . . ? Br1 Ga1 P1 118.34(11) . . ? N3 Ga2 N4 98.9(2) . . ? N3 Ga2 P2 113.78(18) . . ? N4 Ga2 P2 117.50(19) . . ? N3 Ga2 Br2 106.04(19) . . ? N4 Ga2 Br2 102.13(18) . . ? P2 Ga2 Br2 116.34(13) . . ? C59 P1 P2 104.1(3) . . ? C59 P1 Ga1 98.9(3) . . ? P2 P1 Ga1 107.51(11) . . ? P1 P2 Ga2 99.43(11) . . ? C59 N5 C60 109.5(8) . . ? C59 N5 C62 126.9(8) . . ? C60 N5 C62 123.4(9) . . ? C59 N6 C61 109.5(8) . . ? C59 N6 C63 129.1(7) . . ? C61 N6 C63 121.4(8) . . ? N5 C59 N6 106.8(7) . . ? N5 C59 P1 121.2(6) . . ? N6 C59 P1 131.9(6) . . ? C61 C60 N5 107.3(10) . . ? C61 C60 C64 129.7(12) . . ? N5 C60 C64 122.2(11) . . ? C60 C61 N6 106.5(10) . . ? C60 C61 C65 130.0(10) . . ? N6 C61 C65 123.4(9) . . ? N1 Ga1' N2 101.1(4) . . ? N1 Ga1' P1' 114.4(3) . . ? N2 Ga1' P1' 118.6(4) . . ? N1 Ga1' Br1' 104.0(3) . . ? N2 Ga1' Br1' 99.6(2) . . ? P1' Ga1' Br1' 116.7(3) . . ? N4 Ga2' N3 94.4(4) . . ? N4 Ga2' Br2' 108.6(3) . . ? N3 Ga2' Br2' 105.3(3) . . ? N4 Ga2' P2' 112.4(4) . . ? N3 Ga2' P2' 118.8(3) . . ? Br2' Ga2' P2' 115.1(3) . . ? P2' P1' Ga1' 100.2(3) . . ? C59' P2' P1' 103.6(7) . . ? C59' P2' Ga2' 99.5(8) . . ? P1' P2' Ga2' 106.4(3) . . ? C59' N6' C61' 111.7(19) . . ? C59' N6' C63' 126(2) . . ? C61' N6' C63' 123(2) . . ? C59' N5' C60' 109(2) . . ? C59' N5' C62' 128(2) . . ? C60' N5' C62' 122(2) . . ? N5' C59' N6' 106.2(18) . . ? N5' C59' P2' 132.2(16) . . ? N6' C59' P2' 121.3(16) . . ? C61' C60' N5' 108(2) . . ? C61' C60' C64' 126(3) . . ? N5' C60' C64' 123(3) . . ? C60' C61' N6' 104(2) . . ? C60' C61' C65' 135(2) . . ? N6' C61' C65' 122(2) . . ? C1 N1 C6 119.2(6) . . ? C1 N1 Ga1' 124.7(5) . . ? C6 N1 Ga1' 115.6(5) . . ? C1 N1 Ga1 116.1(5) . . ? C6 N1 Ga1 124.6(4) . . ? C3 N2 C18 118.8(5) . . ? C3 N2 Ga1 117.2(5) . . ? C18 N2 Ga1 123.1(4) . . ? C3 N2 Ga1' 114.4(5) . . ? C18 N2 Ga1' 126.7(4) . . ? C30 N3 C35 120.0(5) . . ? C30 N3 Ga2 121.1(4) . . ? C35 N3 Ga2 118.8(4) . . ? C30 N3 Ga2' 112.3(4) . . ? C35 N3 Ga2' 127.6(4) . . ? C32 N4 C47 120.4(5) . . ? C32 N4 Ga2' 118.6(5) . . ? C47 N4 Ga2' 119.0(5) . . ? C32 N4 Ga2 116.4(4) . . ? C47 N4 Ga2 123.2(4) . . ? N1 C1 C2 123.0(7) . . ? N1 C1 C4 118.7(7) . . ? C2 C1 C4 118.3(6) . . ? C1 C2 C3 129.9(6) . . ? N2 C3 C2 123.2(6) . . ? N2 C3 C5 119.1(7) . . ? C2 C3 C5 117.7(6) . . ? C7 C6 C11 120.6(6) . . ? C7 C6 N1 120.6(6) . . ? C11 C6 N1 118.8(6) . . ? C8 C7 C6 118.5(6) . . ? C8 C7 C12 118.8(6) . . ? C6 C7 C12 122.7(6) . . ? C7 C8 C9 122.0(7) . . ? C8 C9 C10 119.1(7) . . ? C11 C10 C9 121.5(7) . . ? C10 C11 C6 118.3(6) . . ? C10 C11 C15 120.1(6) . . ? C6 C11 C15 121.5(6) . . ? C7 C12 C13 111.0(6) . . ? C7 C12 C14 111.8(6) . . ? C13 C12 C14 109.3(6) . . ? C11 C15 C17 111.5(7) . . ? C11 C15 C16 109.8(6) . . ? C17 C15 C16 111.1(7) . . ? C19 C18 C23 120.5(7) . . ? C19 C18 N2 120.8(6) . . ? C23 C18 N2 118.7(7) . . ? C20 C19 C18 118.8(7) . . ? C20 C19 C24 118.8(8) . . ? C18 C19 C24 122.4(7) . . ? C21 C20 C19 121.4(8) . . ? C22 C21 C20 119.3(8) . . ? C21 C22 C23 123.1(8) . . ? C22 C23 C18 116.9(7) . . ? C22 C23 C27 121.4(6) . . ? C18 C23 C27 121.7(7) . . ? C25 C24 C19 109.9(6) . . ? C25 C24 C26 111.2(7) . . ? C19 C24 C26 111.3(6) . . ? C23 C27 C28 112.8(7) . . ? C23 C27 C29 111.3(7) . . ? C28 C27 C29 109.0(6) . . ? N3 C30 C31 122.9(5) . . ? N3 C30 C33 119.3(6) . . ? C31 C30 C33 117.7(5) . . ? C30 C31 C32 128.7(6) . . ? N4 C32 C31 124.8(6) . . ? N4 C32 C34 119.4(6) . . ? C31 C32 C34 115.7(5) . . ? C40 C35 C36 121.4(6) . . ? C40 C35 N3 118.2(5) . . ? C36 C35 N3 120.4(5) . . ? C37 C36 C35 117.8(6) . . ? C37 C36 C41 119.2(5) . . ? C35 C36 C41 123.0(6) . . ? C36 C37 C38 122.1(6) . . ? C37 C38 C39 118.0(7) . . ? C40 C39 C38 122.4(7) . . ? C39 C40 C35 118.1(6) . . ? C39 C40 C44 120.3(6) . . ? C35 C40 C44 121.6(6) . . ? C36 C41 C43 113.0(5) . . ? C36 C41 C42 109.8(5) . . ? C43 C41 C42 109.9(5) . . ? C45 C44 C40 112.4(6) . . ? C45 C44 C46 110.8(7) . . ? C40 C44 C46 110.5(6) . . ? C52 C47 C48 120.3(6) . . ? C52 C47 N4 120.3(7) . . ? C48 C47 N4 119.4(6) . . ? C49 C48 C47 118.1(7) . . ? C49 C48 C53 117.8(7) . . ? C47 C48 C53 124.1(6) . . ? C50 C49 C48 121.0(8) . . ? C49 C50 C51 120.1(7) . . ? C50 C51 C52 121.1(7) . . ? C51 C52 C47 119.4(7) . . ? C51 C52 C56 120.2(6) . . ? C47 C52 C56 120.3(6) . . ? C48 C53 C54 110.9(6) . . ? C48 C53 C55 111.2(7) . . ? C54 C53 C55 107.8(8) . . ? C58 C56 C57 110.6(6) . . ? C58 C56 C52 110.7(6) . . ? C57 C56 C52 113.2(6) . . ? C12_1 C11_1 C16_1 113.2(5) . . ? C12_1 C11_1 B1_1 120.4(5) . . ? C16_1 C11_1 B1_1 125.7(5) . . ? F12_1 C12_1 C13_1 115.9(5) . . ? F12_1 C12_1 C11_1 119.4(5) . . ? C13_1 C12_1 C11_1 124.8(5) . . ? F13_1 C13_1 C12_1 120.2(5) . . ? F13_1 C13_1 C14_1 120.0(5) . . ? C12_1 C13_1 C14_1 119.9(5) . . ? F14_1 C14_1 C15_1 122.2(6) . . ? F14_1 C14_1 C13_1 119.8(5) . . ? C15_1 C14_1 C13_1 118.0(5) . . ? F15_1 C15_1 C14_1 119.3(5) . . ? F15_1 C15_1 C16_1 119.9(5) . . ? C14_1 C15_1 C16_1 120.8(5) . . ? F16_1 C16_1 C15_1 115.7(5) . . ? F16_1 C16_1 C11_1 121.1(5) . . ? C15_1 C16_1 C11_1 123.3(5) . . ? C22_1 C21_1 C26_1 113.2(5) . . ? C22_1 C21_1 B1_1 126.3(5) . . ? C26_1 C21_1 B1_1 120.3(5) . . ? F22_1 C22_1 C23_1 114.5(6) . . ? F22_1 C22_1 C21_1 120.6(5) . . ? C23_1 C22_1 C21_1 124.9(6) . . ? F23_1 C23_1 C24_1 119.9(6) . . ? F23_1 C23_1 C22_1 121.3(7) . . ? C24_1 C23_1 C22_1 118.8(7) . . ? F24_1 C24_1 C25_1 119.8(7) . . ? F24_1 C24_1 C23_1 120.4(7) . . ? C25_1 C24_1 C23_1 119.8(6) . . ? F25_1 C25_1 C24_1 120.2(6) . . ? F25_1 C25_1 C26_1 119.9(7) . . ? C24_1 C25_1 C26_1 119.8(7) . . ? F26_1 C26_1 C25_1 117.1(6) . . ? F26_1 C26_1 C21_1 119.5(5) . . ? C25_1 C26_1 C21_1 123.4(7) . . ? C36_1 C31_1 C32_1 112.8(5) . . ? C36_1 C31_1 B1_1 126.2(5) . . ? C32_1 C31_1 B1_1 120.8(5) . . ? F32_1 C32_1 C33_1 115.9(5) . . ? F32_1 C32_1 C31_1 119.4(5) . . ? C33_1 C32_1 C31_1 124.8(6) . . ? F33_1 C33_1 C32_1 120.8(6) . . ? F33_1 C33_1 C34_1 119.1(6) . . ? C32_1 C33_1 C34_1 120.1(6) . . ? F34_1 C34_1 C35_1 121.3(6) . . ? F34_1 C34_1 C33_1 120.9(6) . . ? C35_1 C34_1 C33_1 117.8(5) . . ? F35_1 C35_1 C34_1 119.1(5) . . ? F35_1 C35_1 C36_1 120.3(6) . . ? C34_1 C35_1 C36_1 120.6(6) . . ? F36_1 C36_1 C35_1 114.8(5) . . ? F36_1 C36_1 C31_1 121.2(5) . . ? C35_1 C36_1 C31_1 124.0(6) . . ? C46_1 C41_1 C42_1 112.4(5) . . ? C46_1 C41_1 B1_1 120.7(5) . . ? C42_1 C41_1 B1_1 126.4(5) . . ? F42_1 C42_1 C43_1 114.8(5) . . ? F42_1 C42_1 C41_1 120.9(5) . . ? C43_1 C42_1 C41_1 124.3(6) . . ? F43_1 C43_1 C44_1 120.0(6) . . ? F43_1 C43_1 C42_1 120.1(6) . . ? C44_1 C43_1 C42_1 119.9(6) . . ? F44_1 C44_1 C43_1 120.5(6) . . ? F44_1 C44_1 C45_1 120.6(6) . . ? C43_1 C44_1 C45_1 119.0(6) . . ? F45_1 C45_1 C44_1 119.2(6) . . ? F45_1 C45_1 C46_1 121.0(6) . . ? C44_1 C45_1 C46_1 119.8(6) . . ? F46_1 C46_1 C45_1 115.6(5) . . ? F46_1 C46_1 C41_1 119.9(5) . . ? C45_1 C46_1 C41_1 124.6(6) . . ? C11_1 B1_1 C31_1 113.9(5) . . ? C11_1 B1_1 C21_1 101.8(4) . . ? C31_1 B1_1 C21_1 113.7(5) . . ? C11_1 B1_1 C41_1 114.1(5) . . ? C31_1 B1_1 C41_1 100.6(4) . . ? C21_1 B1_1 C41_1 113.2(5) . . ? _refine_diff_density_max 0.577 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.098 _shelx_res_file ; TITL mks_077m in P-1 mks_077m_sq.res created by SHELXL-2017/1 at 11:25:18 on 29-Apr-2022 CELL 1.54178 12.54980 16.68900 23.26720 77.9214 77.4027 87.5950 ZERR 2.00 0.00040 0.00070 0.00090 0.0024 0.0022 0.0024 LATT 1 SFAC C H B Br F Ga N P UNIT 178 190 2 4 40 4 12 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.015 0.124 0.144 L.S. 16 0 56 ACTA FMAP 2 SADI_SOLV c1 c2 c2 c3 c3 c4 c4 c5 c5 c6 c6 c1 SADI_SOLV c1 c3 c3 c5 c5 c1 c2 c4 c4 c6 c6 c2 RIGU_SOLV SADI c59 n5 c59 n6 c59' n5' c59' n6' SADI n5 c60 n6 c61 n5' c60' n6' c61' SADI c60 c61 c60' c61' SADI c60 c64 c61 c65 c60' c64' c61' c65' SADI n5 c62 n6 c63 n5' c62' n6' c63' RIGU n5 n6 c59 c60 c61 c62 c63 c64 c65 = N5' N6' C59' C60' C61' C62' C63' C64' C65' SIMU c60 c61 c60' c61' EADP n5 n5' DFIX 1.42 P2 H2a P1' H2a' PLAN 100 ABIN WGHT 0.000000 30.061199 FVAR 0.10728 0.73092 0.49818 PART 1 21 GA1 6 0.706754 0.812835 0.391780 21.00000 0.01927 0.03784 = 0.02630 -0.01122 -0.00564 0.00560 GA2 6 0.821677 0.824947 0.141834 21.00000 0.02143 0.02705 = 0.02158 -0.00344 -0.00329 0.00352 BR1 4 0.543966 0.886075 0.415489 21.00000 0.02601 0.04072 = 0.03990 -0.01333 -0.00597 0.00894 BR2 4 0.965660 0.915430 0.133729 21.00000 0.03110 0.03164 = 0.04142 -0.01325 -0.00092 -0.00265 P1 8 0.805927 0.838266 0.290777 21.00000 0.02065 0.03398 = 0.02632 -0.00903 -0.00634 0.00048 P2 8 0.714761 0.779979 0.238369 21.00000 0.02715 0.03308 = 0.02631 -0.00790 -0.00313 -0.00589 H2A 2 0.782033 0.709631 0.245425 21.00000 0.14572 N5 7 0.856222 1.004020 0.258654 21.00000 0.02961 0.03570 = 0.04005 -0.01418 -0.00461 -0.00418 N6 7 0.685703 0.988347 0.259308 21.00000 0.02974 0.01962 = 0.02681 -0.00046 -0.00368 -0.00339 C59 1 0.777369 0.947616 0.269840 21.00000 0.02991 0.03239 = 0.02055 -0.00726 -0.00470 -0.00256 C60 1 0.811780 1.081722 0.247218 21.00000 0.04535 0.03382 = 0.03450 -0.01646 -0.00535 -0.00735 C61 1 0.706214 1.072257 0.245042 21.00000 0.04638 0.02255 = 0.04218 0.00158 -0.01318 -0.00588 C62 1 0.969479 0.989311 0.262625 21.00000 0.02682 0.05752 = 0.05738 -0.02425 -0.00033 -0.01064 AFIX 137 H62A 2 1.017217 1.016298 0.224889 21.00000 -1.50000 H62B 2 0.983522 0.930233 0.269707 21.00000 -1.50000 H62C 2 0.984152 1.011472 0.295962 21.00000 -1.50000 AFIX 0 C63 1 0.579151 0.955864 0.261617 21.00000 0.02770 0.02976 = 0.04184 -0.00733 -0.01033 0.00022 AFIX 137 H63A 2 0.562661 0.969536 0.221428 21.00000 -1.50000 H63B 2 0.523672 0.979912 0.289691 21.00000 -1.50000 H63C 2 0.579100 0.896190 0.275291 21.00000 -1.50000 AFIX 0 C64 1 0.880518 1.157623 0.229991 21.00000 0.07088 0.04344 = 0.09502 -0.01373 -0.00826 -0.02398 AFIX 137 H64A 2 0.944209 1.150986 0.198452 21.00000 -1.50000 H64B 2 0.904940 1.167050 0.265273 21.00000 -1.50000 H64C 2 0.837438 1.204558 0.214964 21.00000 -1.50000 AFIX 0 C65 1 0.621900 1.135217 0.231458 21.00000 0.06209 0.02135 = 0.07518 0.00204 -0.02312 0.00122 AFIX 137 H65A 2 0.657034 1.188984 0.215360 21.00000 -1.50000 H65B 2 0.567591 1.137244 0.268436 21.00000 -1.50000 H65C 2 0.585831 1.120673 0.201676 21.00000 -1.50000 AFIX 0 PART 0 PART 2 -21 GA1' 6 0.720059 0.784809 0.387918 -21.00000 0.02029 0.04819 = 0.01980 -0.01104 0.00042 0.00847 GA2' 6 0.829490 0.853421 0.133776 -21.00000 0.02003 0.02495 = 0.01569 0.00540 -0.00079 0.00539 BR1' 4 0.566913 0.871879 0.387523 -21.00000 0.02846 0.04181 = 0.03928 -0.00545 -0.00727 0.01282 BR2' 4 0.986042 0.938541 0.105853 -21.00000 0.02866 0.02858 = 0.04324 -0.00455 0.00157 0.00205 P1' 8 0.822321 0.768758 0.294020 -21.00000 0.02986 0.03262 = 0.02437 -0.00668 -0.00365 0.01525 P2' 8 0.727426 0.846584 0.234059 -21.00000 0.01611 0.02737 = 0.02712 -0.00875 -0.00410 0.00466 AFIX 3 H2A' 2 0.760280 0.698015 0.297345 -21.00000 0.42096 AFIX 0 N6' 7 0.674272 1.009485 0.240683 -21.00000 0.03231 0.01456 = 0.02655 0.00558 -0.01170 0.00211 N5' 7 0.840666 0.989399 0.246618 -21.00000 0.02961 0.03570 = 0.04005 -0.01418 -0.00461 -0.00418 C59' 1 0.751873 0.952205 0.242698 -21.00000 0.03058 0.01689 = 0.03178 0.00146 -0.01344 0.00107 C60' 1 0.823142 1.073394 0.236014 -21.00000 0.03911 0.03150 = 0.02840 -0.01774 0.00487 -0.00550 C61' 1 0.714642 1.086556 0.239037 -21.00000 0.04261 0.01700 = 0.03555 -0.00232 -0.00512 -0.00428 C62' 1 0.946468 0.954178 0.252299 -21.00000 0.03801 0.06082 = 0.04124 -0.00904 -0.02006 0.00523 AFIX 137 H62D 2 1.004055 0.993568 0.229699 -21.00000 -1.50000 H62E 2 0.956214 0.903952 0.236212 -21.00000 -1.50000 H62F 2 0.950608 0.941220 0.294824 -21.00000 -1.50000 AFIX 0 C63' 1 0.559132 0.994823 0.242445 -21.00000 0.02731 0.03407 = 0.03546 -0.00846 -0.00526 0.00093 AFIX 137 H63D 2 0.534893 1.035241 0.210862 -21.00000 -1.50000 H63E 2 0.514954 0.999860 0.281817 -21.00000 -1.50000 H63F 2 0.550581 0.939568 0.235835 -21.00000 -1.50000 AFIX 0 C64' 1 0.902961 1.133560 0.243043 -21.00000 0.04844 0.01376 = 0.08898 -0.01424 -0.02398 0.00247 AFIX 137 H64D 2 0.958620 1.147506 0.205728 -21.00000 -1.50000 H64E 2 0.938065 1.109045 0.276275 -21.00000 -1.50000 H64F 2 0.864197 1.183324 0.251704 -21.00000 -1.50000 AFIX 0 C65' 1 0.641582 1.160145 0.239757 -21.00000 0.05309 0.02015 = 0.04978 -0.00485 -0.02461 0.00475 AFIX 137 H65D 2 0.686111 1.209617 0.232274 -21.00000 -1.50000 H65E 2 0.591449 1.154170 0.279123 -21.00000 -1.50000 H65F 2 0.599524 1.164655 0.208343 -21.00000 -1.50000 AFIX 0 PART 0 N1 7 0.669259 0.696623 0.434200 11.00000 0.02840 0.05952 = 0.02980 -0.01994 -0.00682 0.00848 N2 7 0.796441 0.834149 0.443782 11.00000 0.02923 0.06632 = 0.02518 -0.01247 -0.00776 0.00405 N3 7 0.883558 0.740402 0.104924 11.00000 0.02559 0.04649 = 0.02897 -0.00158 -0.00625 -0.00583 N4 7 0.745882 0.884006 0.077899 11.00000 0.02964 0.05777 = 0.02653 -0.00895 -0.00409 0.00821 C1 1 0.657115 0.680657 0.494260 11.00000 0.02938 0.05359 = 0.03467 -0.00224 -0.00426 0.01316 C2 1 0.694033 0.733150 0.524875 11.00000 0.03731 0.05872 = 0.02837 -0.00840 -0.00510 0.00917 AFIX 43 H2 2 0.666199 0.722109 0.567134 11.00000 -1.20000 AFIX 0 C3 1 0.765502 0.799403 0.503153 11.00000 0.03387 0.06608 = 0.02859 -0.01093 -0.00784 0.01525 C4 1 0.604437 0.601966 0.529776 11.00000 0.06395 0.04965 = 0.04186 -0.00645 -0.00476 0.01003 AFIX 137 H4A 2 0.538768 0.592766 0.515661 11.00000 -1.50000 H4B 2 0.584301 0.604670 0.572457 11.00000 -1.50000 H4C 2 0.655633 0.556762 0.524545 11.00000 -1.50000 AFIX 0 C5 1 0.811881 0.832205 0.548015 11.00000 0.05200 0.07627 = 0.02998 -0.01710 -0.01483 0.00495 AFIX 137 H5A 2 0.891563 0.835723 0.535038 11.00000 -1.50000 H5B 2 0.792201 0.795430 0.587528 11.00000 -1.50000 H5C 2 0.782121 0.886849 0.550733 11.00000 -1.50000 AFIX 0 C6 1 0.651151 0.631732 0.404834 11.00000 0.03068 0.06660 = 0.03365 -0.01879 -0.00376 0.00382 C7 1 0.550775 0.624085 0.389621 11.00000 0.02914 0.07013 = 0.03368 -0.01108 -0.00274 -0.00015 C8 1 0.538678 0.563167 0.359886 11.00000 0.03957 0.07192 = 0.05054 -0.01842 -0.00917 -0.00697 AFIX 43 H8 2 0.471232 0.558262 0.348663 11.00000 -1.20000 AFIX 0 C9 1 0.621490 0.508909 0.345831 11.00000 0.04376 0.07585 = 0.06399 -0.03360 -0.00659 -0.00132 AFIX 43 H9 2 0.610894 0.466919 0.325634 11.00000 -1.20000 AFIX 0 C10 1 0.720447 0.516524 0.361604 11.00000 0.04065 0.07662 = 0.06382 -0.03437 -0.00935 0.01093 AFIX 43 H10 2 0.777602 0.479252 0.351965 11.00000 -1.20000 AFIX 0 C11 1 0.737681 0.576685 0.390822 11.00000 0.02957 0.07028 = 0.04705 -0.02656 -0.00438 0.00533 C12 1 0.454747 0.679938 0.404865 11.00000 0.02921 0.04870 = 0.05945 -0.00883 -0.01289 -0.00277 AFIX 13 H12 2 0.475542 0.717360 0.429060 11.00000 -1.20000 AFIX 0 C13 1 0.354505 0.630358 0.442710 11.00000 0.03009 0.05754 = 0.06953 -0.01105 -0.00203 0.00123 AFIX 137 H13A 2 0.326799 0.598786 0.417944 11.00000 -1.50000 H13B 2 0.297644 0.667708 0.457426 11.00000 -1.50000 H13C 2 0.374878 0.592831 0.476995 11.00000 -1.50000 AFIX 0 C14 1 0.425175 0.732710 0.348127 11.00000 0.04195 0.07995 = 0.07057 0.00369 -0.02510 -0.00813 AFIX 137 H14A 2 0.491509 0.758088 0.320935 11.00000 -1.50000 H14B 2 0.373932 0.775560 0.359423 11.00000 -1.50000 H14C 2 0.391203 0.698175 0.327796 11.00000 -1.50000 AFIX 0 C15 1 0.847862 0.583936 0.406745 11.00000 0.03910 0.07858 = 0.05171 -0.03158 -0.00563 0.01267 AFIX 13 H15 2 0.844341 0.631046 0.427501 11.00000 -1.20000 AFIX 0 C16 1 0.937461 0.602439 0.348991 11.00000 0.03515 0.15406 = 0.07830 -0.06132 -0.00124 0.00543 AFIX 137 H16A 2 0.940347 0.557950 0.327085 11.00000 -1.50000 H16B 2 1.008131 0.607069 0.359490 11.00000 -1.50000 H16C 2 0.921039 0.654094 0.323569 11.00000 -1.50000 AFIX 0 C17 1 0.874382 0.506693 0.449532 11.00000 0.05536 0.07022 = 0.11201 -0.03242 -0.03184 0.01065 AFIX 137 H17A 2 0.876782 0.459478 0.430347 11.00000 -1.50000 H17B 2 0.817909 0.497711 0.486714 11.00000 -1.50000 H17C 2 0.945463 0.513351 0.458975 11.00000 -1.50000 AFIX 0 C18 1 0.880296 0.895113 0.425379 11.00000 0.03295 0.07922 = 0.02669 -0.01326 -0.00835 -0.00437 C19 1 0.856235 0.977783 0.430175 11.00000 0.04661 0.07396 = 0.03379 -0.01316 -0.00844 -0.00180 C20 1 0.941536 1.034606 0.413614 11.00000 0.06199 0.06651 = 0.05773 -0.02102 -0.00084 -0.00529 AFIX 43 H20 2 0.925850 1.090340 0.415355 11.00000 -1.20000 AFIX 0 C21 1 1.048338 1.011528 0.394737 11.00000 0.05372 0.09105 = 0.06777 -0.02990 -0.00688 -0.01391 AFIX 43 H21 2 1.105796 1.050582 0.385001 11.00000 -1.20000 AFIX 0 C22 1 1.070549 0.931666 0.390198 11.00000 0.03380 0.10503 = 0.04819 -0.01715 -0.00805 -0.00667 AFIX 43 H22 2 1.144318 0.916662 0.377041 11.00000 -1.20000 AFIX 0 C23 1 0.989452 0.871020 0.404071 11.00000 0.02943 0.07969 = 0.03419 -0.01612 -0.01270 0.00387 C24 1 0.740705 1.006596 0.452564 11.00000 0.04890 0.06670 = 0.03587 -0.01265 -0.00335 0.00720 AFIX 13 H24 2 0.692143 0.957275 0.467639 11.00000 -1.20000 AFIX 0 C25 1 0.700020 1.061234 0.400952 11.00000 0.05398 0.06452 = 0.04784 -0.01037 -0.01462 0.01195 AFIX 137 H25A 2 0.752442 1.105818 0.381660 11.00000 -1.50000 H25B 2 0.629031 1.084265 0.416431 11.00000 -1.50000 H25C 2 0.692324 1.028894 0.371443 11.00000 -1.50000 AFIX 0 C26 1 0.735439 1.050358 0.504393 11.00000 0.06273 0.10507 = 0.04366 -0.02818 -0.00484 0.01386 AFIX 137 H26A 2 0.784008 1.098212 0.490851 11.00000 -1.50000 H26B 2 0.758535 1.012829 0.537819 11.00000 -1.50000 H26C 2 0.660387 1.068178 0.517842 11.00000 -1.50000 AFIX 0 C27 1 1.017263 0.783787 0.397390 11.00000 0.02679 0.08219 = 0.04370 -0.01422 -0.01305 0.00764 AFIX 13 H27 2 0.952162 0.759524 0.388999 11.00000 -1.20000 AFIX 0 C28 1 1.113960 0.778754 0.345351 11.00000 0.03194 0.10108 = 0.06079 -0.03635 -0.00309 0.00435 AFIX 137 H28A 2 1.125071 0.721616 0.341135 11.00000 -1.50000 H28B 2 1.179887 0.799397 0.353574 11.00000 -1.50000 H28C 2 1.098885 0.812024 0.307997 11.00000 -1.50000 AFIX 0 C29 1 1.041911 0.731097 0.455956 11.00000 0.07497 0.12159 = 0.05167 -0.00671 -0.01257 0.05153 AFIX 137 H29A 2 1.061010 0.675423 0.450022 11.00000 -1.50000 H29B 2 0.977248 0.729114 0.488637 11.00000 -1.50000 H29C 2 1.103115 0.755322 0.466371 11.00000 -1.50000 AFIX 0 C30 1 0.906676 0.749691 0.045009 11.00000 0.03197 0.04020 = 0.03101 -0.01272 -0.00732 -0.00282 C31 1 0.866338 0.814309 0.007132 11.00000 0.03889 0.04841 = 0.02796 -0.01157 -0.00897 0.00875 AFIX 43 H31 2 0.898954 0.821146 -0.034473 11.00000 -1.20000 AFIX 0 C32 1 0.784082 0.870537 0.022238 11.00000 0.03436 0.05954 = 0.02612 -0.01021 -0.00837 0.00623 C33 1 0.978857 0.688493 0.016458 11.00000 0.05262 0.04014 = 0.03845 -0.00771 -0.01318 0.00610 AFIX 137 H33A 2 0.976983 0.697587 -0.026307 11.00000 -1.50000 H33B 2 0.952855 0.632956 0.036420 11.00000 -1.50000 H33C 2 1.053903 0.694944 0.020604 11.00000 -1.50000 AFIX 0 C34 1 0.738638 0.919377 -0.029587 11.00000 0.06270 0.09019 = 0.02566 -0.01293 -0.01473 0.03779 AFIX 137 H34A 2 0.790477 0.962727 -0.052741 11.00000 -1.50000 H34B 2 0.668998 0.944009 -0.013828 11.00000 -1.50000 H34C 2 0.727029 0.883001 -0.055730 11.00000 -1.50000 AFIX 0 C35 1 0.901010 0.661976 0.142295 11.00000 0.03179 0.04529 = 0.02918 -0.00248 -0.00417 -0.00387 C36 1 1.000597 0.645249 0.160854 11.00000 0.02697 0.04350 = 0.02945 -0.01050 -0.00308 0.00056 C37 1 1.011305 0.570209 0.198201 11.00000 0.03472 0.04764 = 0.03539 -0.00923 -0.00674 0.00244 AFIX 43 H37 2 1.078448 0.557480 0.210538 11.00000 -1.20000 AFIX 0 C38 1 0.927093 0.513105 0.218135 11.00000 0.04753 0.05903 = 0.03045 0.00348 -0.00759 -0.00878 AFIX 43 H38 2 0.935431 0.462372 0.244272 11.00000 -1.20000 AFIX 0 C39 1 0.829274 0.532515 0.198545 11.00000 0.03973 0.07478 = 0.03537 -0.00058 -0.00046 -0.02197 AFIX 43 H39 2 0.770637 0.494280 0.212420 11.00000 -1.20000 AFIX 0 C40 1 0.815242 0.604342 0.160268 11.00000 0.02672 0.06064 = 0.03875 -0.00686 -0.00303 -0.01248 C41 1 1.094878 0.705824 0.142553 11.00000 0.02157 0.03926 = 0.03902 -0.00778 -0.00401 -0.00062 AFIX 13 H41 2 1.075432 0.753666 0.112886 11.00000 -1.20000 AFIX 0 C42 1 1.110644 0.736940 0.197295 11.00000 0.02892 0.05623 = 0.06040 -0.02207 -0.01338 0.00832 AFIX 137 H42A 2 1.168372 0.778683 0.184772 11.00000 -1.50000 H42B 2 1.131392 0.691211 0.226684 11.00000 -1.50000 H42C 2 1.042299 0.760918 0.215600 11.00000 -1.50000 AFIX 0 C43 1 1.201453 0.669985 0.112961 11.00000 0.02962 0.04833 = 0.04459 -0.00930 -0.00020 0.00606 AFIX 137 H43A 2 1.190051 0.648251 0.078753 11.00000 -1.50000 H43B 2 1.225274 0.625720 0.142295 11.00000 -1.50000 H43C 2 1.257540 0.712947 0.098812 11.00000 -1.50000 AFIX 0 C44 1 0.709219 0.620526 0.137735 11.00000 0.03480 0.06234 = 0.05975 0.00834 -0.01731 -0.01311 AFIX 13 H44 2 0.703718 0.680994 0.123055 11.00000 -1.20000 AFIX 0 C45 1 0.608732 0.593482 0.187308 11.00000 0.03911 0.07394 = 0.08428 0.00436 -0.01323 -0.01367 AFIX 137 H45A 2 0.542846 0.606271 0.171040 11.00000 -1.50000 H45B 2 0.606633 0.622469 0.220073 11.00000 -1.50000 H45C 2 0.612060 0.534307 0.202707 11.00000 -1.50000 AFIX 0 C46 1 0.711941 0.579226 0.084207 11.00000 0.06223 0.06422 = 0.06373 -0.00864 -0.03105 -0.00646 AFIX 137 H46A 2 0.641667 0.587190 0.071968 11.00000 -1.50000 H46B 2 0.725552 0.520465 0.096088 11.00000 -1.50000 H46C 2 0.770336 0.603711 0.050461 11.00000 -1.50000 AFIX 0 C47 1 0.657452 0.939488 0.089089 11.00000 0.02998 0.07079 = 0.02330 -0.01086 -0.00763 0.00822 C48 1 0.678532 1.025711 0.074469 11.00000 0.03473 0.06379 = 0.03252 -0.01215 0.00085 0.01356 C49 1 0.590015 1.078695 0.085721 11.00000 0.04307 0.07873 = 0.04175 -0.02289 0.00284 0.01894 AFIX 43 H49 2 0.602250 1.136196 0.076658 11.00000 -1.20000 AFIX 0 C50 1 0.485280 1.048402 0.109803 11.00000 0.03958 0.09010 = 0.04771 -0.03031 -0.00887 0.02611 AFIX 43 H50 2 0.426102 1.085086 0.116599 11.00000 -1.20000 AFIX 0 C51 1 0.466565 0.964595 0.124033 11.00000 0.03090 0.08777 = 0.03946 -0.03411 -0.00836 0.00920 AFIX 43 H51 2 0.394354 0.944399 0.140633 11.00000 -1.20000 AFIX 0 C52 1 0.551544 0.909645 0.114441 11.00000 0.03055 0.07540 = 0.03045 -0.01849 -0.01250 0.00602 C53 1 0.790978 1.064049 0.045479 11.00000 0.04375 0.04876 = 0.04925 0.00288 0.01280 0.01619 AFIX 13 H53 2 0.844010 1.019699 0.036225 11.00000 -1.20000 AFIX 0 C54 1 0.830695 1.108948 0.087857 11.00000 0.04558 0.04772 = 0.10330 -0.02426 0.01539 -0.00548 AFIX 137 H54A 2 0.907964 1.123398 0.072112 11.00000 -1.50000 H54B 2 0.821760 1.073287 0.127834 11.00000 -1.50000 H54C 2 0.787822 1.158941 0.090791 11.00000 -1.50000 AFIX 0 C55 1 0.788178 1.126087 -0.013030 11.00000 0.08149 0.09970 = 0.05755 0.02936 0.03106 0.04333 AFIX 137 H55A 2 0.862329 1.146011 -0.032452 11.00000 -1.50000 H55B 2 0.741496 1.172318 -0.003865 11.00000 -1.50000 H55C 2 0.758921 1.099554 -0.040142 11.00000 -1.50000 AFIX 0 C56 1 0.528380 0.817811 0.128167 11.00000 0.02685 0.07431 = 0.04991 -0.01518 -0.01351 -0.00303 AFIX 13 H56 2 0.594029 0.789069 0.140291 11.00000 -1.20000 AFIX 0 C57 1 0.430794 0.791723 0.180036 11.00000 0.02850 0.09164 = 0.07222 -0.01663 -0.00848 -0.00637 AFIX 137 H57A 2 0.363239 0.810412 0.166901 11.00000 -1.50000 H57B 2 0.437041 0.816124 0.213989 11.00000 -1.50000 H57C 2 0.429397 0.731869 0.192548 11.00000 -1.50000 AFIX 0 C58 1 0.513482 0.790092 0.072125 11.00000 0.05549 0.08779 = 0.06845 -0.03489 -0.02677 0.00456 AFIX 137 H58A 2 0.451747 0.819260 0.057853 11.00000 -1.50000 H58B 2 0.499092 0.730992 0.081806 11.00000 -1.50000 H58C 2 0.580013 0.802170 0.040621 11.00000 -1.50000 AFIX 0 RESI 1 AN F12 5 0.058737 0.286217 0.222157 11.00000 0.02408 0.03439 = 0.03495 -0.00078 -0.00565 0.00098 F13 5 -0.090004 0.349970 0.161021 11.00000 0.01967 0.04751 = 0.06128 -0.00366 -0.01661 0.00251 F14 5 -0.035935 0.471608 0.062628 11.00000 0.03929 0.04861 = 0.05893 0.00148 -0.03177 0.01055 F15 5 0.175832 0.523602 0.022716 11.00000 0.04892 0.03721 = 0.03561 0.00379 -0.01413 0.00049 F16 5 0.328484 0.455221 0.078894 11.00000 0.02674 0.04308 = 0.04072 0.00106 -0.00785 -0.00488 F22 5 0.146757 0.275448 0.322958 11.00000 0.03857 0.04871 = 0.03343 -0.01351 -0.00192 0.00516 F23 5 0.100173 0.368683 0.404205 11.00000 0.05554 0.08871 = 0.04065 -0.02852 -0.00481 0.02056 F24 5 0.182956 0.523523 0.380292 11.00000 0.06904 0.08452 = 0.07438 -0.05649 -0.03666 0.03404 F25 5 0.307148 0.585218 0.269813 11.00000 0.07491 0.03999 = 0.08837 -0.03002 -0.04301 0.01218 F26 5 0.353251 0.494267 0.186216 11.00000 0.04901 0.03097 = 0.05030 -0.00521 -0.01865 0.00082 F32 5 0.375860 0.285622 0.078991 11.00000 0.02863 0.05475 = 0.04078 -0.02074 -0.00348 0.00002 F33 5 0.582536 0.289271 0.019947 11.00000 0.03865 0.06826 = 0.04858 -0.02130 0.00887 0.00454 F34 5 0.744605 0.330619 0.069088 11.00000 0.02126 0.05123 = 0.06840 0.00696 0.00700 0.00181 F35 5 0.692002 0.372337 0.178936 11.00000 0.02326 0.05513 = 0.07121 -0.00435 -0.02124 -0.00218 F36 5 0.487869 0.376796 0.236664 11.00000 0.03060 0.04854 = 0.04765 -0.01386 -0.01924 0.00490 F42 5 0.190474 0.195229 0.146229 11.00000 0.03491 0.04012 = 0.04396 -0.01701 -0.01300 0.00268 F43 5 0.203441 0.035407 0.182101 11.00000 0.03930 0.03742 = 0.05544 -0.01834 0.00483 -0.00498 F44 5 0.293065 -0.030001 0.278330 11.00000 0.06082 0.02935 = 0.05876 0.00314 0.00999 0.00514 F45 5 0.370769 0.071378 0.337543 11.00000 0.05924 0.04900 = 0.03823 0.00432 -0.00849 0.02302 F46 5 0.369392 0.232623 0.298844 11.00000 0.03649 0.04812 = 0.03619 -0.00916 -0.01472 0.01095 C11 1 0.202755 0.364190 0.153259 11.00000 0.02238 0.02906 = 0.02853 -0.01051 -0.00870 0.00396 C12 1 0.093477 0.343204 0.171036 11.00000 0.02475 0.02968 = 0.02598 -0.00465 -0.00751 0.00295 C13 1 0.014225 0.376409 0.140788 11.00000 0.02224 0.02882 = 0.03827 -0.00764 -0.00810 0.00157 C14 1 0.040821 0.438037 0.090543 11.00000 0.03049 0.03701 = 0.04200 -0.01261 -0.02092 0.01262 C15 1 0.147570 0.462460 0.071370 11.00000 0.03382 0.03333 = 0.02844 -0.00268 -0.01128 -0.00215 C16 1 0.225877 0.426693 0.102075 11.00000 0.02590 0.03015 = 0.03354 -0.00484 -0.00607 -0.00262 C21 1 0.257931 0.378437 0.250222 11.00000 0.02520 0.03650 = 0.03737 -0.01291 -0.01832 0.01477 C22 1 0.190844 0.352496 0.306445 11.00000 0.02990 0.04098 = 0.04116 -0.01349 -0.01240 0.01050 C23 1 0.164619 0.398763 0.350285 11.00000 0.03410 0.06138 = 0.03908 -0.01937 -0.01172 0.01775 C24 1 0.204938 0.477087 0.337911 11.00000 0.04873 0.06235 = 0.05543 -0.03816 -0.02888 0.02964 C25 1 0.268145 0.508184 0.282602 11.00000 0.04174 0.04221 = 0.05969 -0.02229 -0.03081 0.01836 C26 1 0.292485 0.460166 0.239724 11.00000 0.03301 0.03522 = 0.05267 -0.01629 -0.02285 0.01221 C31 1 0.417870 0.333710 0.160447 11.00000 0.01952 0.03022 = 0.03683 -0.00655 -0.00930 0.00240 C32 1 0.451340 0.311229 0.105010 11.00000 0.02409 0.03867 = 0.03851 -0.00855 -0.00448 0.00017 C33 1 0.557537 0.311214 0.073959 11.00000 0.03091 0.04258 = 0.04249 -0.00818 -0.00527 0.00518 C34 1 0.640234 0.332402 0.098066 11.00000 0.01945 0.03736 = 0.05172 0.00187 -0.00004 0.00027 C35 1 0.612354 0.353738 0.153276 11.00000 0.02165 0.03669 = 0.05253 0.00092 -0.01457 0.00057 C36 1 0.504535 0.354354 0.182828 11.00000 0.02720 0.03528 = 0.03730 -0.00641 -0.01441 0.00718 C41 1 0.277520 0.225593 0.221067 11.00000 0.01904 0.03374 = 0.02531 -0.00417 0.00039 0.00324 C42 1 0.236484 0.169427 0.194219 11.00000 0.02325 0.03615 = 0.03590 -0.00861 -0.00078 0.00550 C43 1 0.241450 0.085289 0.212519 11.00000 0.02831 0.03628 = 0.04324 -0.01408 0.00217 0.00308 C44 1 0.286665 0.052389 0.260315 11.00000 0.03912 0.02731 = 0.04148 -0.00042 0.00921 0.00637 C45 1 0.326136 0.103922 0.289698 11.00000 0.03308 0.04280 = 0.03186 0.00595 0.00065 0.01154 C46 1 0.323238 0.187234 0.269284 11.00000 0.02524 0.04228 = 0.02819 -0.00683 -0.00304 0.00603 B1 3 0.288592 0.325916 0.195996 11.00000 0.01982 0.02835 = 0.02970 -0.00717 -0.00700 0.00602 RESI 0 HKLF 4 REM mks_077m in P-1 REM R1 = 0.0793 for 14631 Fo > 4sig(Fo) and 0.1015 for all 19037 data REM 1263 parameters refined using 195 restraints END WGHT 0.0000 30.0587 REM Highest difference peak 0.577, deepest hole -0.795, 1-sigma level 0.098 Q1 1 0.7612 0.3684 0.0919 11.00000 0.05 0.58 Q2 1 0.8909 0.9024 0.1457 11.00000 0.05 0.46 Q3 1 0.7160 0.9411 0.3816 11.00000 0.05 0.45 Q4 1 0.8758 0.7278 0.3697 11.00000 0.05 0.45 Q5 1 0.6715 0.6717 0.6312 11.00000 0.05 0.43 Q6 1 0.9084 0.9851 0.1505 11.00000 0.05 0.43 Q7 1 0.6236 0.9160 0.4390 11.00000 0.05 0.40 Q8 1 0.8166 0.5697 0.2162 11.00000 0.05 0.40 Q9 1 0.9248 1.1924 0.1125 11.00000 0.05 0.40 Q10 1 0.5989 0.5893 0.4165 11.00000 0.05 0.40 Q11 1 0.6574 0.8737 0.2792 11.00000 0.05 0.40 Q12 1 -0.0965 0.4187 0.0673 11.00000 0.05 0.39 Q13 1 0.9568 0.9283 0.0700 11.00000 0.05 0.39 Q14 1 0.7588 0.8298 0.3319 11.00000 0.05 0.38 Q15 1 1.1348 0.8280 0.1198 11.00000 0.05 0.38 Q16 1 0.7665 0.4175 0.0598 11.00000 0.05 0.38 Q17 1 0.6194 0.4325 0.1186 11.00000 0.05 0.37 Q18 1 0.8251 1.0219 0.1260 11.00000 0.05 0.37 Q19 1 0.9853 0.4942 0.1797 11.00000 0.05 0.37 Q20 1 0.4762 0.8462 0.4125 11.00000 0.05 0.37 Q21 1 0.3419 0.3880 0.3457 11.00000 0.05 0.37 Q22 1 0.6825 0.7784 0.3542 11.00000 0.05 0.36 Q23 1 0.9220 0.8414 0.1217 11.00000 0.05 0.36 Q24 1 0.6045 0.4630 0.2686 11.00000 0.05 0.36 Q25 1 0.5529 0.9312 0.3288 11.00000 0.05 0.36 Q26 1 0.5538 0.7402 0.4091 11.00000 0.05 0.35 Q27 1 0.8754 0.8978 0.5229 11.00000 0.05 0.35 Q28 1 0.8609 0.3042 0.3427 11.00000 0.05 0.35 Q29 1 0.7820 0.6778 0.3804 11.00000 0.05 0.35 Q30 1 0.7673 0.7430 0.2468 11.00000 0.05 0.35 Q31 1 1.0513 0.9826 0.0979 11.00000 0.05 0.35 Q32 1 0.6500 0.9157 0.3196 11.00000 0.05 0.35 Q33 1 0.8338 0.9398 0.4203 11.00000 0.05 0.35 Q34 1 0.6660 0.7659 0.2870 11.00000 0.05 0.35 Q35 1 0.7224 0.7948 0.2866 11.00000 0.05 0.35 Q36 1 0.6018 1.0403 0.6001 11.00000 0.05 0.35 Q37 1 0.7495 1.3045 0.3166 11.00000 0.05 0.34 Q38 1 0.6597 0.7458 0.1706 11.00000 0.05 0.34 Q39 1 0.3211 0.0475 0.2288 11.00000 0.05 0.34 Q40 1 0.7516 1.0764 -0.0552 11.00000 0.05 0.34 Q41 1 0.9051 1.0927 0.1612 11.00000 0.05 0.34 Q42 1 0.5960 0.7561 0.3486 11.00000 0.05 0.34 Q43 1 0.6168 0.8184 0.2597 11.00000 0.05 0.34 Q44 1 0.4380 0.8808 0.2878 11.00000 0.05 0.33 Q45 1 0.9766 0.9435 0.0606 11.00000 0.05 0.33 Q46 1 0.8337 0.8280 0.3279 11.00000 0.05 0.33 Q47 1 0.8580 1.2553 0.1310 11.00000 0.05 0.33 Q48 1 0.5656 0.9338 0.4090 11.00000 0.05 0.33 Q49 1 0.9540 0.7859 -0.1000 11.00000 0.05 0.33 Q50 1 0.5975 0.4934 0.0880 11.00000 0.05 0.33 Q51 1 0.7523 0.6324 0.2293 11.00000 0.05 0.33 Q52 1 0.9236 0.8394 0.1501 11.00000 0.05 0.33 Q53 1 1.1436 0.7999 0.1082 11.00000 0.05 0.33 Q54 1 0.6451 0.3127 0.2059 11.00000 0.05 0.33 Q55 1 0.3649 0.4026 0.1323 11.00000 0.05 0.32 Q56 1 0.4536 0.8374 0.3577 11.00000 0.05 0.32 Q57 1 1.0092 0.8148 0.0825 11.00000 0.05 0.32 Q58 1 0.8919 0.9487 0.1194 11.00000 0.05 0.32 Q59 1 0.2479 0.7252 0.5708 11.00000 0.05 0.32 Q60 1 0.3208 0.3809 0.2261 11.00000 0.05 0.32 Q61 1 0.2616 0.7239 0.3991 11.00000 0.05 0.32 Q62 1 0.6778 0.3911 0.2109 11.00000 0.05 0.32 Q63 1 0.2949 0.4019 0.2577 11.00000 0.05 0.32 Q64 1 0.9128 0.7814 0.5457 11.00000 0.05 0.31 Q65 1 0.4761 0.4881 0.3358 11.00000 0.05 0.31 Q66 1 1.2167 0.5162 0.1439 11.00000 0.05 0.31 Q67 1 0.3165 -0.0859 0.2471 11.00000 0.05 0.31 Q68 1 0.5372 0.8291 0.3846 11.00000 0.05 0.31 Q69 1 0.6526 1.2526 0.4356 11.00000 0.05 0.31 Q70 1 0.1304 0.4185 0.1711 11.00000 0.05 0.31 Q71 1 0.8228 0.8150 0.2015 11.00000 0.05 0.31 Q72 1 0.8556 0.7703 0.1101 11.00000 0.05 0.31 Q73 1 1.0798 0.7652 0.0785 11.00000 0.05 0.31 Q74 1 1.1988 0.8309 0.3217 11.00000 0.05 0.31 Q75 1 1.0741 1.0900 0.1869 11.00000 0.05 0.31 Q76 1 0.5348 0.4855 0.1495 11.00000 0.05 0.31 Q77 1 1.0241 1.0007 0.0477 11.00000 0.05 0.31 Q78 1 0.4954 1.0304 0.4811 11.00000 0.05 0.31 Q79 1 0.9645 1.0131 0.1113 11.00000 0.05 0.31 Q80 1 0.7619 1.0579 0.0188 11.00000 0.05 0.31 Q81 1 0.6883 0.8334 0.5432 11.00000 0.05 0.31 Q82 1 1.0096 0.7861 0.2184 11.00000 0.05 0.31 Q83 1 0.3826 0.5752 0.2947 11.00000 0.05 0.30 Q84 1 0.9624 1.1715 -0.0716 11.00000 0.05 0.30 Q85 1 0.2436 0.1938 0.2182 11.00000 0.05 0.30 Q86 1 0.9215 0.8422 0.0406 11.00000 0.05 0.30 Q87 1 0.6609 0.9255 0.1405 11.00000 0.05 0.30 Q88 1 0.9950 0.7799 0.4899 11.00000 0.05 0.30 Q89 1 0.5332 0.9388 0.4470 11.00000 0.05 0.30 Q90 1 0.2804 0.7863 0.1603 11.00000 0.05 0.30 Q91 1 0.5766 0.9559 0.3712 11.00000 0.05 0.30 Q92 1 0.5530 0.3064 0.3513 11.00000 0.05 0.30 Q93 1 0.5572 0.2100 0.0492 11.00000 0.05 0.30 Q94 1 1.0604 0.5140 0.2395 11.00000 0.05 0.30 Q95 1 1.0622 0.9006 0.0820 11.00000 0.05 0.30 Q96 1 0.6626 0.8548 0.2082 11.00000 0.05 0.30 Q97 1 0.2963 0.4937 0.1185 11.00000 0.05 0.30 Q98 1 0.7541 1.1609 0.1330 11.00000 0.05 0.30 Q99 1 0.5452 0.9984 0.5472 11.00000 0.05 0.30 Q100 1 0.7731 1.1788 0.0292 11.00000 0.05 0.30 ; _shelx_res_checksum 79250 _shelx_fab_file ; 1 0 0 -14.32 0.00 2 0 0 -19.29 0.00 3 0 0 -2.48 0.00 4 0 0 -7.69 0.00 5 0 0 4.55 0.00 6 0 0 -2.98 0.00 7 0 0 -4.66 0.00 8 0 0 1.73 0.00 9 0 0 0.89 0.00 10 0 0 -2.49 0.00 11 0 0 2.09 0.00 12 0 0 2.68 0.00 13 0 0 0.28 0.00 14 0 0 0.30 0.00 15 0 0 -0.79 0.00 -15 1 0 0.26 0.00 -14 1 0 -0.79 0.00 -13 1 0 -0.80 0.00 -12 1 0 -2.02 0.00 -11 1 0 3.49 0.00 -10 1 0 1.24 0.00 -9 1 0 -0.72 0.00 -8 1 0 3.15 0.00 -7 1 0 4.39 0.00 -6 1 0 -2.86 0.00 -5 1 0 0.55 0.00 -4 1 0 5.63 0.00 -3 1 0 -4.70 0.00 -2 1 0 12.90 0.00 -1 1 0 -73.65 0.00 0 1 0 -23.33 0.00 1 1 0 70.23 0.00 2 1 0 -1.88 0.00 3 1 0 8.57 0.00 4 1 0 -2.87 0.00 5 1 0 -1.25 0.00 6 1 0 5.68 0.00 7 1 0 -0.64 0.00 8 1 0 -2.82 0.00 9 1 0 1.21 0.00 10 1 0 -0.54 0.00 11 1 0 -4.00 0.00 12 1 0 0.15 0.00 13 1 0 0.38 0.00 14 1 0 0.73 0.00 15 1 0 0.29 0.00 -15 2 0 0.79 0.00 -14 2 0 0.24 0.00 -13 2 0 0.53 0.00 -12 2 0 -2.14 0.00 -11 2 0 -3.56 0.00 -10 2 0 1.12 0.00 -9 2 0 -1.56 0.00 -8 2 0 -3.08 0.00 -7 2 0 1.22 0.00 -6 2 0 3.93 0.00 -5 2 0 -3.62 0.00 -4 2 0 4.17 0.00 -3 2 0 3.11 0.00 -2 2 0 21.20 0.00 -1 2 0 42.17 0.00 0 2 0 -81.08 0.00 1 2 0 -20.10 0.00 2 2 0 16.13 0.00 3 2 0 -3.71 0.00 4 2 0 8.57 0.00 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0.00 0 4 0 36.06 0.00 1 4 0 24.33 0.00 2 4 0 -7.48 0.00 3 4 0 3.39 0.00 4 4 0 -7.79 0.00 5 4 0 4.06 0.00 6 4 0 4.04 0.00 7 4 0 0.36 0.00 8 4 0 -1.27 0.00 9 4 0 1.25 0.00 10 4 0 -1.99 0.00 11 4 0 -2.92 0.00 12 4 0 1.27 0.00 13 4 0 0.15 0.00 14 4 0 1.09 0.00 15 4 0 -0.34 0.00 -14 5 0 0.03 0.00 -13 5 0 0.41 0.00 -12 5 0 -2.45 0.00 -11 5 0 -0.30 0.00 -10 5 0 -0.04 0.00 -9 5 0 0.67 0.00 -8 5 0 -2.93 0.00 -7 5 0 3.55 0.00 -6 5 0 -1.21 0.00 -5 5 0 -1.59 0.00 -4 5 0 6.41 0.00 -3 5 0 1.24 0.00 -2 5 0 26.81 0.00 -1 5 0 -11.62 0.00 0 5 0 -41.47 0.00 1 5 0 17.76 0.00 2 5 0 0.94 0.00 3 5 0 5.58 0.00 4 5 0 0.29 0.00 5 5 0 -7.02 0.00 6 5 0 1.06 0.00 7 5 0 1.75 0.00 8 5 0 1.61 0.00 9 5 0 0.37 0.00 10 5 0 3.07 0.00 11 5 0 -0.68 0.00 12 5 0 -1.60 0.00 13 5 0 -0.45 0.00 14 5 0 -0.22 0.00 -14 6 0 -0.44 0.00 -13 6 0 1.04 0.00 -12 6 0 0.57 0.00 -11 6 0 -0.32 0.00 -10 6 0 -1.63 0.00 -9 6 0 1.70 0.00 -8 6 0 -1.66 0.00 -7 6 0 -0.80 0.00 -6 6 0 0.04 0.00 -5 6 0 -3.69 0.00 -4 6 0 -3.78 0.00 -3 6 0 -5.39 0.00 -2 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0.00 -6 18 10 0.67 0.00 -5 19 10 0.07 0.00 7 19 10 -0.63 0.00 -3 20 10 1.15 0.00 5 20 10 1.07 0.00 -1 -17 11 0.20 0.00 4 -17 11 1.41 0.00 -4 -16 11 1.10 0.00 12 -11 11 -0.63 0.00 -10 -10 11 0.63 0.00 -11 -8 11 0.31 0.00 14 -7 11 0.06 0.00 -12 -5 11 -0.83 0.00 15 -4 11 0.52 0.00 -13 0 11 0.39 0.00 -13 1 11 -0.09 0.00 -13 2 11 0.08 0.00 -13 3 11 -0.03 0.00 15 7 11 0.51 0.00 12 14 11 -0.78 0.00 -9 15 11 0.30 0.00 -8 16 11 0.41 0.00 -7 17 11 0.13 0.00 -6 18 11 -0.01 0.00 7 19 11 0.15 0.00 5 20 11 -0.12 0.00 1 -17 12 -0.15 0.00 2 -17 12 0.32 0.00 -3 -16 12 0.91 0.00 6 -16 12 -0.37 0.00 -6 -14 12 0.73 0.00 9 -14 12 -0.36 0.00 10 -13 12 -1.06 0.00 -8 -12 12 0.12 0.00 11 -12 12 -0.63 0.00 -10 -9 12 0.69 0.00 13 -9 12 0.85 0.00 -11 -7 12 0.12 0.00 -12 -4 12 0.44 0.00 15 -3 12 -0.38 0.00 15 6 12 0.32 0.00 14 10 12 0.31 0.00 12 14 12 0.33 0.00 -4 19 12 -0.22 0.00 7 19 12 0.18 0.00 -2 20 12 -0.54 0.00 5 20 12 -0.98 0.00 -1 -16 13 0.08 0.00 7 -15 13 -0.29 0.00 -9 -10 13 -0.53 0.00 12 -10 13 0.25 0.00 -10 -8 13 -1.17 0.00 14 -6 13 -0.16 0.00 -12 -2 13 0.84 0.00 15 -2 13 -0.19 0.00 -12 -1 13 -0.41 0.00 -12 5 13 0.00 0.00 -12 6 13 -0.07 0.00 15 6 13 -0.28 0.00 -11 10 13 0.76 0.00 14 10 13 0.72 0.00 -10 12 13 -0.35 0.00 13 12 13 0.70 0.00 -9 14 13 -0.75 0.00 12 14 13 -0.12 0.00 -1 20 13 0.78 0.00 4 20 13 0.19 0.00 1 -16 14 -0.68 0.00 2 -16 14 0.98 0.00 6 -15 14 0.31 0.00 9 -13 14 0.54 0.00 10 -12 14 -0.43 0.00 11 -11 14 -0.49 0.00 -9 -9 14 -0.40 0.00 -10 -7 14 -0.16 0.00 -11 -4 14 -1.11 0.00 15 -1 14 0.39 0.00 15 0 14 0.16 0.00 15 4 14 -0.11 0.00 15 5 14 -0.12 0.00 13 12 14 -0.69 0.00 11 15 14 -0.49 0.00 -7 16 14 -1.34 0.00 -6 17 14 -0.92 0.00 8 18 14 0.43 0.00 -3 19 14 1.16 0.00 0 20 14 0.43 0.00 1 20 14 0.04 0.00 2 20 14 0.39 0.00 3 20 14 -0.04 0.00 -1 -15 15 -0.18 0.00 4 -15 15 1.21 0.00 7 -14 15 -1.06 0.00 -5 -13 15 -0.20 0.00 -6 -12 15 -0.30 0.00 -7 -11 15 0.15 0.00 12 -9 15 0.60 0.00 -9 -8 15 0.19 0.00 13 -7 15 0.43 0.00 -10 -6 15 1.20 0.00 -11 -2 15 -0.96 0.00 15 1 15 -0.12 0.00 15 2 15 0.08 0.00 15 3 15 0.10 0.00 15 4 15 -0.16 0.00 -11 7 15 0.27 0.00 14 9 15 -0.55 0.00 -8 14 15 -0.36 0.00 10 16 15 -0.41 0.00 9 17 15 0.16 0.00 6 19 15 0.88 0.00 -2 -14 16 -0.17 0.00 6 -14 16 0.61 0.00 -4 -13 16 -0.59 0.00 -5 -12 16 0.50 0.00 9 -12 16 0.37 0.00 -6 -11 16 -0.01 0.00 10 -11 16 -0.23 0.00 -7 -10 16 0.05 0.00 -9 -7 16 0.52 0.00 -10 -4 16 0.70 0.00 -11 1 16 0.14 0.00 -11 2 16 0.53 0.00 -11 3 16 -0.70 0.00 -11 4 16 -0.02 0.00 14 8 16 -0.27 0.00 -10 9 16 -0.16 0.00 13 11 16 0.10 0.00 12 13 16 -0.32 0.00 -7 15 16 1.42 0.00 -6 16 16 1.33 0.00 -5 17 16 0.59 0.00 5 19 16 -0.84 0.00 0 -14 17 -0.96 0.00 1 -14 17 0.74 0.00 3 -14 17 -0.86 0.00 4 -14 17 0.50 0.00 -4 -12 17 0.12 0.00 -7 -9 17 -0.09 0.00 11 -9 17 -0.07 0.00 -10 -2 17 0.57 0.00 14 -2 17 0.48 0.00 -10 7 17 -0.21 0.00 14 7 17 -0.09 0.00 11 14 17 0.18 0.00 -3 18 17 0.53 0.00 0 19 17 0.17 0.00 4 19 17 0.74 0.00 -1 -13 18 0.05 0.00 5 -13 18 -0.88 0.00 -3 -12 18 0.19 0.00 7 -12 18 -0.21 0.00 -7 -8 18 0.18 0.00 -8 -6 18 0.03 0.00 -9 -4 18 -0.09 0.00 14 -1 18 0.26 0.00 14 0 18 0.22 0.00 -10 1 18 -0.07 0.00 -10 2 18 -0.39 0.00 -10 3 18 0.48 0.00 -10 4 18 0.39 0.00 -10 5 18 -0.60 0.00 14 6 18 0.26 0.00 -9 9 18 0.34 0.00 13 10 18 -0.00 0.00 12 11 18 -0.69 0.00 12 12 18 -0.24 0.00 10 15 18 0.06 0.00 -5 16 18 -0.77 0.00 9 16 18 0.26 0.00 -2 18 18 -0.34 0.00 6 18 18 -0.18 0.00 2 19 18 -0.24 0.00 -1 -12 19 0.30 0.00 6 -12 19 0.45 0.00 -3 -11 19 -0.57 0.00 9 -10 19 0.14 0.00 10 -9 19 -0.49 0.00 12 -6 19 0.30 0.00 -9 -1 19 0.40 0.00 14 2 19 0.64 0.00 14 3 19 -0.31 0.00 14 4 19 -0.05 0.00 -9 7 19 0.24 0.00 13 9 19 0.03 0.00 11 13 19 -0.31 0.00 -6 14 19 -0.17 0.00 -4 16 19 0.35 0.00 -3 17 19 0.80 0.00 7 17 19 -1.17 0.00 -1 18 19 -0.05 0.00 5 18 19 -0.52 0.00 1 -12 20 1.03 0.00 2 -12 20 0.05 0.00 3 -12 20 -0.32 0.00 -3 -10 20 0.36 0.00 8 -10 20 -0.48 0.00 9 -9 20 -0.17 0.00 10 -8 20 -0.02 0.00 -6 -7 20 0.07 0.00 12 -5 20 0.16 0.00 -8 -3 20 -0.48 0.00 13 -2 20 -0.85 0.00 -9 3 20 -0.40 0.00 13 8 20 0.40 0.00 -8 9 20 -0.62 0.00 -6 13 20 -0.28 0.00 10 14 20 0.21 0.00 9 15 20 -0.36 0.00 8 16 20 0.32 0.00 6 17 20 0.72 0.00 1 18 20 0.43 0.00 2 18 20 -0.44 0.00 3 18 20 0.86 0.00 1 -11 21 -0.11 0.00 2 -11 21 -1.07 0.00 3 -11 21 0.41 0.00 4 -11 21 0.18 0.00 -3 -9 21 0.56 0.00 8 -9 21 -0.35 0.00 -4 -8 21 -0.58 0.00 -5 -7 21 -0.32 0.00 10 -7 21 1.03 0.00 -8 0 21 -0.23 0.00 13 0 21 -0.96 0.00 13 1 21 -0.29 0.00 13 5 21 -0.22 0.00 -8 6 21 0.48 0.00 13 6 21 0.49 0.00 -7 10 21 -0.30 0.00 -6 12 21 0.25 0.00 11 12 21 0.14 0.00 7 16 21 1.13 0.00 0 17 21 0.25 0.00 5 17 21 0.59 0.00 1 -10 22 -1.36 0.00 4 -10 22 -0.48 0.00 5 -10 22 -0.32 0.00 7 -9 22 0.65 0.00 -3 -8 22 -0.70 0.00 8 -8 22 0.80 0.00 -4 -7 22 -0.23 0.00 10 -6 22 -1.31 0.00 -6 -4 22 0.09 0.00 12 -2 22 -0.15 0.00 -7 -1 22 -0.91 0.00 -7 8 22 -0.15 0.00 12 8 22 0.99 0.00 11 11 22 0.25 0.00 -1 16 22 0.57 0.00 6 16 22 -0.21 0.00 1 -9 23 0.59 0.00 2 -9 23 0.68 0.00 4 -9 23 0.66 0.00 5 -9 23 0.30 0.00 7 -8 23 -0.15 0.00 8 -7 23 -0.16 0.00 9 -6 23 0.19 0.00 10 -5 23 0.53 0.00 -5 -4 23 0.15 0.00 11 -3 23 -0.38 0.00 -6 -2 23 -0.25 0.00 12 0 23 -0.12 0.00 12 1 23 -0.39 0.00 12 6 23 -0.33 0.00 -6 9 23 0.01 0.00 -5 11 23 -0.28 0.00 9 13 23 -0.23 0.00 8 14 23 0.43 0.00 1 16 23 -0.41 0.00 4 16 23 0.91 0.00 1 -8 24 1.13 0.00 2 -8 24 -0.69 0.00 3 -8 24 0.88 0.00 4 -8 24 0.00 0.00 -1 -7 24 0.75 0.00 -2 -6 24 -0.23 0.00 8 -6 24 -0.20 0.00 -3 -5 24 -0.40 0.00 9 -5 24 0.83 0.00 -4 -4 24 -0.11 0.00 10 -3 24 0.40 0.00 -5 -2 24 -0.46 0.00 11 -1 24 -0.06 0.00 -6 2 24 0.13 0.00 -6 3 24 -0.18 0.00 -6 4 24 0.51 0.00 -6 5 24 -0.62 0.00 11 8 24 1.08 0.00 -5 9 24 -0.35 0.00 -4 11 24 -0.61 0.00 9 12 24 -0.30 0.00 8 13 24 0.36 0.00 7 14 24 -1.26 0.00 5 15 24 -0.20 0.00 2 -7 25 -0.34 0.00 3 -7 25 -0.24 0.00 4 -7 25 -0.85 0.00 0 -6 25 1.34 0.00 6 -6 25 -0.40 0.00 9 -3 25 0.55 0.00 10 -1 25 0.35 0.00 -5 2 25 -0.28 0.00 -5 3 25 0.02 0.00 11 3 25 0.28 0.00 -5 4 25 0.67 0.00 11 4 25 0.29 0.00 -5 5 25 -0.86 0.00 11 5 25 -1.00 0.00 -5 6 25 -0.29 0.00 -4 9 25 -0.03 0.00 10 9 25 0.68 0.00 -3 11 25 -1.12 0.00 9 11 25 -0.15 0.00 8 12 25 1.04 0.00 -1 13 25 -0.77 0.00 7 13 25 -1.45 0.00 5 14 25 -0.61 0.00 1 -5 26 -1.12 0.00 5 -5 26 0.06 0.00 -1 -4 26 -0.16 0.00 7 -4 26 0.53 0.00 8 -3 26 -0.35 0.00 -3 -1 26 -0.28 0.00 9 -1 26 1.03 0.00 -4 2 26 -0.41 0.00 10 2 26 0.24 0.00 -4 3 26 0.87 0.00 10 3 26 -0.26 0.00 -4 4 26 -0.27 0.00 10 4 26 -0.00 0.00 -4 5 26 -0.71 0.00 10 5 26 0.51 0.00 -4 6 26 0.48 0.00 10 6 26 -0.72 0.00 -3 9 26 -0.76 0.00 9 9 26 -0.35 0.00 1 13 26 -0.20 0.00 5 13 26 0.01 0.00 3 -4 27 0.12 0.00 4 -4 27 0.30 0.00 6 -3 27 0.77 0.00 7 -2 27 -0.19 0.00 8 -1 27 -0.55 0.00 -2 0 27 0.56 0.00 9 2 27 0.18 0.00 9 3 27 -0.02 0.00 9 4 27 -0.41 0.00 9 5 27 -0.39 0.00 9 6 27 0.73 0.00 -2 8 27 -0.32 0.00 8 9 27 0.35 0.00 -1 10 27 -0.56 0.00 7 10 27 -0.26 0.00 0 11 27 0.10 0.00 6 11 27 -0.47 0.00 2 12 27 0.06 0.00 3 12 27 0.13 0.00 4 12 27 -0.23 0.00 3 -2 28 0.19 0.00 4 -2 28 -0.23 0.00 1 -1 28 1.00 0.00 5 -1 28 -0.26 0.00 6 -1 28 0.59 0.00 0 0 28 0.13 0.00 7 1 28 0.01 0.00 -1 2 28 -0.14 0.00 -1 3 28 0.72 0.00 -1 4 28 -0.21 0.00 8 4 28 0.11 0.00 -1 5 28 -0.80 0.00 -1 6 28 0.50 0.00 7 7 28 0.30 0.00 0 8 28 0.30 0.00 7 8 28 -0.45 0.00 6 9 28 -0.18 0.00 2 10 28 -0.34 0.00 3 10 28 0.56 0.00 4 10 28 -0.83 0.00 5 10 28 0.18 0.00 3 1 29 -0.18 0.00 4 1 29 -0.46 0.00 2 2 29 0.67 0.00 3 2 29 0.54 0.00 4 2 29 -0.12 0.00 5 2 29 -0.60 0.00 2 3 29 -0.21 0.00 5 3 29 -0.10 0.00 1 4 29 0.42 0.00 2 4 29 -0.54 0.00 5 4 29 0.46 0.00 1 5 29 -0.03 0.00 2 5 29 0.81 0.00 5 5 29 -0.32 0.00 2 6 29 -0.34 0.00 4 6 29 0.07 0.00 5 6 29 -0.28 0.00 2 7 29 -0.51 0.00 3 7 29 -0.27 0.00 4 7 29 0.31 0.00 5 7 29 0.42 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 230418) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.292 0.728 0.615 155 49 ' ' 2 0.708 0.272 0.385 155 49 ' ' 3 0.450 0.512 0.967 7 0 ' ' 4 0.450 0.595 0.075 8 0 ' ' 5 0.550 0.405 0.925 8 0 ' ' 6 0.551 0.488 0.034 7 0 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL mks_077m P -1 R = 0.11 CELL 12.5498 16.6890 23.2672 77.92 77.40 87.60 SPGR P-1 # Solvent Accessible Volume = 339 # Electrons Found in S.A.V. = 99 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.751 0.308 0.316 ! 5.54 eA-3 C102 0.658 0.264 0.429 ! 4.76 eA-3 C103 0.826 0.296 0.356 ! 4.61 eA-3 C104 0.653 0.295 0.324 ! 3.78 eA-3 C105 0.605 0.267 0.389 ! 3.39 eA-3 C106 0.752 0.282 0.421 ! 3.17 eA-3 C107 0.564 0.284 0.354 ! 3.09 eA-3 C108 0.915 0.345 0.332 ! 2.97 eA-3 C109 0.827 0.278 0.406 ! 2.89 eA-3 Q110 0.503 0.252 0.352 ! 1.01 eA-3 Q111 0.634 0.378 0.338 ! 0.88 eA-3 Q112 0.731 0.215 0.500 ! 0.77 eA-3 Q113 0.765 0.421 0.051 ! 0.76 eA-3 Q114 0.769 0.361 0.099 ! 0.76 eA-3 C115 0.778 0.248 0.336 ! 0.76 eA-3 Q116 0.448 0.169 0.442 ! 0.74 eA-3 Q117 0.328 0.330 0.366 ! 0.73 eA-3 Q118 0.811 0.911 0.276 ! 0.72 eA-3 Q119 0.583 0.283 0.305 ! 0.70 eA-3 Q120 0.922 0.985 0.156 ! 0.70 eA-3 Q121 0.048 0.982 0.102 ! 0.68 eA-3 Q122 0.766 0.829 0.327 ! 0.67 eA-3 Q123 0.771 0.752 0.243 ! 0.67 eA-3 Q124 0.623 0.920 0.433 ! 0.66 eA-3 Q125 0.753 0.063 0.026 ! 0.65 eA-3 Q126 0.527 0.114 0.402 ! 0.65 eA-3 Q127 0.489 0.323 0.385 ! 0.65 eA-3 Q128 0.899 0.905 0.137 ! 0.65 eA-3 Q129 0.575 0.373 0.275 ! 0.65 eA-3 Q130 0.486 0.127 0.469 ! 0.64 eA-3 Q131 0.487 0.488 0.331 ! 0.64 eA-3 Q132 0.656 0.926 0.142 ! 0.64 eA-3 Q133 0.657 0.221 0.384 ! 0.63 eA-3 Q134 0.406 0.513 0.020 ! 0.63 eA-3 Q135 0.890 1.001 0.125 ! 0.62 eA-3 Q136 0.714 0.936 0.384 ! 0.62 eA-3 Q137 0.533 0.250 0.468 ! 0.61 eA-3 Q138 0.874 0.734 0.362 ! 0.61 eA-3 Q139 0.286 0.938 0.328 ! 0.61 eA-3 Q140 0.749 0.157 0.134 ! 0.60 eA-3 Q141 0.830 0.831 0.330 ! 0.60 eA-3 Q142 0.833 0.251 0.061 ! 0.60 eA-3 Q143 0.543 0.828 0.228 ! 0.60 eA-3 Q144 0.137 0.563 0.087 ! 0.60 eA-3 Q145 0.049 0.636 0.282 ! 0.59 eA-3 Q146 0.888 0.803 0.368 ! 0.59 eA-3 Q147 0.328 0.621 0.184 ! 0.59 eA-3 Q148 0.860 0.736 0.084 ! 0.59 eA-3 Q149 0.771 0.845 0.130 ! 0.59 eA-3 Q150 0.267 0.280 0.132 ! 0.59 eA-3 Q151 0.562 0.736 0.432 ! 0.58 eA-3 Q152 0.248 0.278 0.489 ! 0.58 eA-3 Q153 0.188 0.686 0.487 ! 0.58 eA-3 Q154 0.078 0.097 0.177 ! 0.57 eA-3 Q155 0.641 0.213 0.477 ! 0.57 eA-3 Q156 0.910 0.918 0.330 ! 0.57 eA-3 Q157 0.605 0.455 0.265 ! 0.56 eA-3 Q158 0.516 0.375 0.022 ! 0.56 eA-3 Q159 0.604 0.595 0.416 ! 0.56 eA-3 Q160 0.681 0.296 0.046 ! 0.56 eA-3 C161 0.520 0.551 0.040 ! 0.55 eA-3 Q162 0.565 0.935 0.404 ! 0.55 eA-3 Q163 0.724 0.753 0.016 ! 0.55 eA-3 C164 0.548 0.199 0.392 ! 0.55 eA-3 Q165 0.553 0.301 0.186 ! 0.55 eA-3 Q166 0.302 0.407 0.259 ! 0.55 eA-3 Q167 0.499 0.033 0.478 ! 0.54 eA-3 Q168 0.144 0.703 0.360 ! 0.54 eA-3 Q169 0.652 0.329 0.202 ! 0.54 eA-3 Q170 0.485 0.601 0.293 ! 0.54 eA-3 Q171 0.315 0.049 0.231 ! 0.54 eA-3 Q172 0.577 0.818 0.491 ! 0.54 eA-3 Q173 0.422 0.324 0.094 ! 0.54 eA-3 Q174 0.690 0.778 0.356 ! 0.54 eA-3 Q175 0.505 0.436 0.287 ! 0.54 eA-3 Q176 0.689 0.652 0.033 ! 0.54 eA-3 Q177 0.623 0.729 0.300 ! 0.53 eA-3 Q178 0.221 0.204 0.016 ! 0.53 eA-3 Q179 0.769 0.802 0.437 ! 0.53 eA-3 Q180 0.246 0.920 0.056 ! 0.53 eA-3 Q181 0.955 0.192 0.285 ! 0.53 eA-3 Q182 0.545 0.933 0.325 ! 0.53 eA-3 Q183 0.020 0.169 0.139 ! 0.53 eA-3 Q184 0.346 0.828 0.128 ! 0.53 eA-3 Q185 0.855 0.718 0.407 ! 0.52 eA-3 Q186 0.360 0.399 0.129 ! 0.52 eA-3 Q187 0.901 0.279 0.476 ! 0.52 eA-3 Q188 0.172 0.420 0.036 ! 0.52 eA-3 Q189 0.920 0.193 0.114 ! 0.52 eA-3 Q190 0.311 0.955 0.348 ! 0.52 eA-3 Q191 0.472 0.848 0.412 ! 0.52 eA-3 Q192 0.188 0.893 0.140 ! 0.52 eA-3 Q193 0.250 0.589 0.218 ! 0.52 eA-3 Q194 0.012 0.514 0.373 ! 0.52 eA-3 Q195 0.358 0.142 0.270 ! 0.52 eA-3 Q196 0.748 0.624 0.233 ! 0.52 eA-3 Q197 0.915 0.653 0.223 ! 0.52 eA-3 Q198 0.872 0.264 0.229 ! 0.51 eA-3 Q199 1.004 0.030 0.504 ! 0.51 eA-3 ) ; _shelx_fab_checksum 66665 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mks_056m _database_code_depnum_ccdc_archive 'CCDC 2184142' loop_ _audit_author_name _audit_author_address 'Christoph Wolper' ;Universitaet Duisburg Essen Germany ; _audit_update_record ; 2022-07-05 deposited with the CCDC. 2022-10-12 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H94 B Br2 F20 Ga2 N6 P2' _chemical_formula_weight 1999.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.557(2) _cell_length_b 20.432(2) _cell_length_c 20.684(2) _cell_angle_alpha 90 _cell_angle_beta 99.720(5) _cell_angle_gamma 90 _cell_volume 8979.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9278 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 80.66 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_F_000 4068 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.112 _exptl_crystal_size_min 0.096 _exptl_absorpt_coefficient_mu 2.888 _shelx_estimated_absorpt_T_min 0.705 _shelx_estimated_absorpt_T_max 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 Venture (Photon II detector)' _diffrn_measurement_method 'Data collection strategy APEX 3/Queen' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 405733 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.079 _diffrn_reflns_theta_max 81.277 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 19684 _reflns_number_gt 16685 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX3(v2017.3-0)' _computing_cell_refinement 'Bruker APEX3(v2017.3-0)' _computing_data_reduction 'Bruker APEX3(v2017.3-0)' _computing_structure_solution 'Bruker APEX3(v2017.3-0)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _refine_special_details ; Treatment of hydrogen atoms: Riding model on idealized geometries with the 1.2 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. The methyl groups are idealized with tetrahedral angles in a combined rotating and rigid group refinement with the 1.5 fold isotropic displacement parameters of the equivalent Uij of the corresponding carbon atom. Disorder: A second orientation of the central Br--Ga--P--P--Ga--Br chain could be identified and refined. Hints on the carbene can be found in the residual electron density but due to the low occupancy (approx. 5\%) the second orientation could not completely be identified nor refined. RIGU and SIMU restraints were used to refine the displacement parameters of the minor component. For Ga2' and Br2' an additional ISOR restraint was neccessary. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+6.3518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary diffmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 19684 _refine_ls_number_parameters 1178 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.44180(2) 0.44026(2) 0.42288(2) 0.02075(6) Uani 0.9428(10) 1 d . . P A 1 Br2 Br 0.12293(2) 0.35576(2) 0.27377(2) 0.02434(7) Uani 0.9428(10) 1 d . . P A 1 Ga1 Ga 0.39957(3) 0.43862(3) 0.31046(2) 0.01400(8) Uani 0.9428(10) 1 d . . P A 1 Ga2 Ga 0.13358(2) 0.46948(2) 0.26769(2) 0.01544(8) Uani 0.9428(10) 1 d . . P A 1 P1 P 0.29005(2) 0.41986(2) 0.28835(2) 0.01639(10) Uani 0.9428(10) 1 d . . P A 1 P2 P 0.23657(2) 0.50748(2) 0.26760(2) 0.02009(11) Uani 0.9428(10) 1 d . . P A 1 Ga1' Ga 0.3916(6) 0.4405(6) 0.2886(5) 0.031(2) Uani 0.0572(10) 1 d . . P A 2 Br1' Br 0.4152(4) 0.4398(3) 0.4027(3) 0.0383(13) Uani 0.0572(10) 1 d . . P A 2 P1' P 0.2865(5) 0.4568(6) 0.2327(5) 0.041(3) Uani 0.0572(10) 1 d . . P A 2 Ga2' Ga 0.1297(6) 0.4546(5) 0.2762(6) 0.038(3) Uani 0.0572(10) 1 d . U P A 2 Br2' Br 0.0940(5) 0.3392(5) 0.2813(5) 0.104(3) Uani 0.0572(10) 1 d . U P A 2 P2' P 0.2372(5) 0.4727(5) 0.3111(5) 0.037(2) Uani 0.0572(10) 1 d . . P A 2 N1 N 0.44517(7) 0.36860(7) 0.27562(7) 0.0178(3) Uani 1 1 d . . . . . N2 N 0.43469(6) 0.51066(7) 0.26819(7) 0.0173(3) Uani 1 1 d . . . . . N3 N 0.08380(7) 0.50377(7) 0.33085(7) 0.0190(3) Uani 1 1 d . . . . . N4 N 0.07688(7) 0.49567(7) 0.18932(7) 0.0186(3) Uani 1 1 d . . . . . N5 N 0.28085(7) 0.41041(8) 0.42602(7) 0.0228(3) Uani 1 1 d . . . . . N6 N 0.26929(7) 0.31887(8) 0.37348(8) 0.0252(3) Uani 1 1 d . . . . . C1 C 0.50208(8) 0.38140(8) 0.26104(8) 0.0181(3) Uani 1 1 d . . . . . C2 C 0.52527(8) 0.44446(9) 0.25650(8) 0.0199(3) Uani 1 1 d . . . . . H2 H 0.568766 0.447489 0.253967 0.024 Uiso 1 1 calc R U . . . C3 C 0.49305(8) 0.50406(8) 0.25515(8) 0.0187(3) Uani 1 1 d . . . . . C4 C 0.54364(9) 0.32547(9) 0.24754(10) 0.0258(4) Uani 1 1 d . . . . . H4A H 0.522202 0.299943 0.210246 0.039 Uiso 1 1 calc R U . . . H4B H 0.552509 0.297307 0.286360 0.039 Uiso 1 1 calc R U . . . H4C H 0.583234 0.342783 0.237251 0.039 Uiso 1 1 calc R U . . . C5 C 0.52798(8) 0.56364(9) 0.23795(10) 0.0242(4) Uani 1 1 d . . . . . H5A H 0.559214 0.550593 0.211050 0.036 Uiso 1 1 calc R U . . . H5B H 0.549298 0.584583 0.278263 0.036 Uiso 1 1 calc R U . . . H5C H 0.498160 0.594526 0.213318 0.036 Uiso 1 1 calc R U . . . C6 C 0.41833(8) 0.30404(8) 0.26443(9) 0.0205(3) Uani 1 1 d . . . . . C7 C 0.42846(8) 0.25615(9) 0.31404(10) 0.0232(4) Uani 1 1 d . . . . . C8 C 0.39838(9) 0.19596(9) 0.30091(11) 0.0300(4) Uani 1 1 d . . . . . H8 H 0.403993 0.162849 0.333625 0.036 Uiso 1 1 calc R U . . . C9 C 0.36047(10) 0.18347(10) 0.24105(12) 0.0352(5) Uani 1 1 d . . . . . H9 H 0.339690 0.142497 0.233445 0.042 Uiso 1 1 calc R U . . . C10 C 0.35293(10) 0.23057(10) 0.19257(11) 0.0337(5) Uani 1 1 d . . . . . H10 H 0.327625 0.221139 0.151418 0.040 Uiso 1 1 calc R U . . . C11 C 0.38159(9) 0.29160(9) 0.20264(10) 0.0254(4) Uani 1 1 d . . . . . C12 C 0.47066(9) 0.26639(9) 0.37970(9) 0.0261(4) Uani 1 1 d . . . . . H12 H 0.489787 0.310994 0.379906 0.031 Uiso 1 1 calc R U . . . C13 C 0.52412(11) 0.21580(11) 0.39122(12) 0.0378(5) Uani 1 1 d . . . . . H13A H 0.506465 0.172180 0.395818 0.057 Uiso 1 1 calc R U . . . H13B H 0.553339 0.226922 0.431334 0.057 Uiso 1 1 calc R U . . . H13C H 0.546664 0.216025 0.353849 0.057 Uiso 1 1 calc R U . . . C14 C 0.43304(11) 0.26247(11) 0.43649(11) 0.0355(5) Uani 1 1 d . . . . . H14A H 0.399762 0.295687 0.430322 0.053 Uiso 1 1 calc R U . . . H14B H 0.461260 0.270312 0.478115 0.053 Uiso 1 1 calc R U . . . H14C H 0.414114 0.218922 0.437204 0.053 Uiso 1 1 calc R U . . . C15 C 0.37409(9) 0.34111(10) 0.14666(10) 0.0297(4) Uani 1 1 d . . . . . H15 H 0.393439 0.383199 0.164681 0.036 Uiso 1 1 calc R U . . . C16 C 0.40888(11) 0.31913(12) 0.09167(11) 0.0407(5) Uani 1 1 d . . . . . H16A H 0.391036 0.277705 0.073211 0.061 Uiso 1 1 calc R U . . . H16B H 0.453611 0.313070 0.109397 0.061 Uiso 1 1 calc R U . . . H16C H 0.404239 0.352553 0.057203 0.061 Uiso 1 1 calc R U . . . C17 C 0.30509(11) 0.35458(13) 0.11908(12) 0.0425(6) Uani 1 1 d . . . . . H17A H 0.302310 0.383438 0.080853 0.064 Uiso 1 1 calc R U . . . H17B H 0.285029 0.375740 0.152733 0.064 Uiso 1 1 calc R U . . . H17C H 0.283617 0.313203 0.105922 0.064 Uiso 1 1 calc R U . . . C18 C 0.40240(8) 0.57299(8) 0.25654(9) 0.0189(3) Uani 1 1 d . . . . . C19 C 0.41068(8) 0.62126(8) 0.30567(9) 0.0213(3) Uani 1 1 d . . . . . C20 C 0.37778(9) 0.67996(9) 0.29279(10) 0.0266(4) Uani 1 1 d . . . . . H20 H 0.381580 0.712916 0.325622 0.032 Uiso 1 1 calc R U . . . C21 C 0.33982(9) 0.69078(9) 0.23307(11) 0.0301(4) Uani 1 1 d . . . . . H21 H 0.318289 0.731293 0.224926 0.036 Uiso 1 1 calc R U . . . C22 C 0.33292(9) 0.64315(10) 0.18506(10) 0.0287(4) Uani 1 1 d . . . . . H22 H 0.306904 0.651514 0.144055 0.034 Uiso 1 1 calc R U . . . C23 C 0.36346(8) 0.58294(9) 0.19568(9) 0.0226(3) Uani 1 1 d . . . . . C24 C 0.45381(9) 0.61282(9) 0.37125(9) 0.0231(4) Uani 1 1 d . . . . . H24 H 0.474037 0.568727 0.371932 0.028 Uiso 1 1 calc R U . . . C25 C 0.50589(10) 0.66484(10) 0.38109(11) 0.0317(4) Uani 1 1 d . . . . . H25A H 0.527231 0.665366 0.342844 0.048 Uiso 1 1 calc R U . . . H25B H 0.536374 0.654454 0.420490 0.048 Uiso 1 1 calc R U . . . H25C H 0.487318 0.707915 0.386205 0.048 Uiso 1 1 calc R U . . . C26 C 0.41688(10) 0.61654(10) 0.42866(10) 0.0308(4) Uani 1 1 d . . . . . H26A H 0.398663 0.660332 0.430251 0.046 Uiso 1 1 calc R U . . . H26B H 0.445359 0.607767 0.469918 0.046 Uiso 1 1 calc R U . . . H26C H 0.383107 0.583872 0.422363 0.046 Uiso 1 1 calc R U . . . C27 C 0.35409(9) 0.53029(10) 0.14282(9) 0.0272(4) Uani 1 1 d . . . . . H27 H 0.354406 0.487093 0.165612 0.033 Uiso 1 1 calc R U . . . C28 C 0.40738(11) 0.52896(13) 0.10243(11) 0.0395(5) Uani 1 1 d . . . . . H28A H 0.399231 0.494423 0.069201 0.059 Uiso 1 1 calc R U . . . H28B H 0.447389 0.520244 0.131417 0.059 Uiso 1 1 calc R U . . . H28C H 0.409650 0.571363 0.080804 0.059 Uiso 1 1 calc R U . . . C29 C 0.29094(10) 0.53595(12) 0.09666(11) 0.0380(5) Uani 1 1 d . . . . . H29A H 0.291198 0.574879 0.069034 0.057 Uiso 1 1 calc R U . . . H29B H 0.256976 0.539687 0.122526 0.057 Uiso 1 1 calc R U . . . H29C H 0.284186 0.496900 0.068847 0.057 Uiso 1 1 calc R U . . . C30 C 0.02205(8) 0.51249(8) 0.31274(8) 0.0198(3) Uani 1 1 d . . . . . C31 C -0.00986(8) 0.50538(8) 0.24825(8) 0.0197(3) Uani 1 1 d . . . . . H31 H -0.054411 0.502730 0.243273 0.024 Uiso 1 1 calc R U . . . C32 C 0.01511(8) 0.50166(8) 0.19041(8) 0.0187(3) Uani 1 1 d . . . . . C33 C -0.01810(9) 0.53337(11) 0.36238(9) 0.0279(4) Uani 1 1 d . . . . . H33A H -0.042987 0.571860 0.345940 0.042 Uiso 1 1 calc R U . . . H33B H 0.009065 0.544239 0.403910 0.042 Uiso 1 1 calc R U . . . H33C H -0.046415 0.497527 0.369470 0.042 Uiso 1 1 calc R U . . . C34 C -0.03007(8) 0.50608(10) 0.12658(9) 0.0253(4) Uani 1 1 d . . . . . H34A H -0.022092 0.546440 0.103720 0.038 Uiso 1 1 calc R U . . . H34B H -0.073349 0.506430 0.135344 0.038 Uiso 1 1 calc R U . . . H34C H -0.024194 0.468262 0.099105 0.038 Uiso 1 1 calc R U . . . C35 C 0.11167(8) 0.51479(9) 0.39866(8) 0.0204(3) Uani 1 1 d . . . . . C36 C 0.10403(8) 0.46818(9) 0.44663(9) 0.0225(3) Uani 1 1 d . . . . . C37 C 0.12930(9) 0.48295(10) 0.51210(9) 0.0265(4) Uani 1 1 d . . . . . H37 H 0.125171 0.452095 0.545475 0.032 Uiso 1 1 calc R U . . . C38 C 0.16007(9) 0.54144(10) 0.52902(9) 0.0292(4) Uani 1 1 d . . . . . H38 H 0.175856 0.550978 0.573722 0.035 Uiso 1 1 calc R U . . . C39 C 0.16780(9) 0.58610(10) 0.48061(10) 0.0282(4) Uani 1 1 d . . . . . H39 H 0.189443 0.625928 0.492647 0.034 Uiso 1 1 calc R U . . . C40 C 0.14454(8) 0.57393(9) 0.41457(9) 0.0234(4) Uani 1 1 d . . . . . C41 C 0.06840(9) 0.40409(10) 0.43128(9) 0.0250(4) Uani 1 1 d . . . . . H41 H 0.050418 0.403728 0.383437 0.030 Uiso 1 1 calc R U . . . C42 C 0.01382(10) 0.39598(12) 0.46987(11) 0.0377(5) Uani 1 1 d . . . . . H42A H -0.012133 0.435629 0.465182 0.057 Uiso 1 1 calc R U . . . H42B H 0.030794 0.388792 0.516338 0.057 Uiso 1 1 calc R U . . . H42C H -0.011984 0.358335 0.452687 0.057 Uiso 1 1 calc R U . . . C43 C 0.11210(10) 0.34518(10) 0.44564(11) 0.0340(4) Uani 1 1 d . . . . . H43A H 0.088214 0.304861 0.433894 0.051 Uiso 1 1 calc R U . . . H43B H 0.130022 0.344343 0.492443 0.051 Uiso 1 1 calc R U . . . H43C H 0.146122 0.348499 0.419807 0.051 Uiso 1 1 calc R U . . . C44 C 0.15225(9) 0.62396(9) 0.36199(10) 0.0268(4) Uani 1 1 d . . . . . H44 H 0.155763 0.599213 0.321058 0.032 Uiso 1 1 calc R U . . . C45 C 0.09413(11) 0.66775(10) 0.34678(11) 0.0360(5) Uani 1 1 d . . . . . H45A H 0.100186 0.699707 0.313071 0.054 Uiso 1 1 calc R U . . . H45B H 0.087830 0.690811 0.386711 0.054 Uiso 1 1 calc R U . . . H45C H 0.057097 0.640803 0.330813 0.054 Uiso 1 1 calc R U . . . C46 C 0.21165(11) 0.66580(11) 0.37912(12) 0.0390(5) Uani 1 1 d . . . . . H46A H 0.248177 0.637277 0.392068 0.058 Uiso 1 1 calc R U . . . H46B H 0.207183 0.695204 0.415491 0.058 Uiso 1 1 calc R U . . . H46C H 0.217609 0.691720 0.340777 0.058 Uiso 1 1 calc R U . . . C47 C 0.09926(8) 0.51029(9) 0.12856(8) 0.0207(3) Uani 1 1 d . . . . . C48 C 0.10484(8) 0.46033(10) 0.08316(9) 0.0241(4) Uani 1 1 d . . . . . C49 C 0.12802(9) 0.47754(11) 0.02621(9) 0.0288(4) Uani 1 1 d . . . . . H49 H 0.133569 0.444512 -0.004633 0.035 Uiso 1 1 calc R U . . . C50 C 0.14296(9) 0.54144(12) 0.01397(9) 0.0322(4) Uani 1 1 d . . . . . H50 H 0.158508 0.551979 -0.025079 0.039 Uiso 1 1 calc R U . . . C51 C 0.13542(9) 0.59032(11) 0.05832(9) 0.0299(4) Uani 1 1 d . . . . . H51 H 0.144969 0.634341 0.048917 0.036 Uiso 1 1 calc R U . . . C52 C 0.11385(9) 0.57568(10) 0.11695(9) 0.0252(4) Uani 1 1 d . . . . . C53 C 0.08514(9) 0.39009(10) 0.09270(9) 0.0264(4) Uani 1 1 d . . . . . H53 H 0.065174 0.388376 0.132933 0.032 Uiso 1 1 calc R U . . . C54 C 0.03647(11) 0.36628(12) 0.03428(11) 0.0369(5) Uani 1 1 d . . . . . H54A H 0.056432 0.362970 -0.004796 0.055 Uiso 1 1 calc R U . . . H54B H 0.001502 0.397478 0.026038 0.055 Uiso 1 1 calc R U . . . H54C H 0.020505 0.323228 0.044407 0.055 Uiso 1 1 calc R U . . . C55 C 0.14202(11) 0.34431(12) 0.10302(12) 0.0403(5) Uani 1 1 d . . . . . H55A H 0.128177 0.299642 0.110369 0.060 Uiso 1 1 calc R U . . . H55B H 0.172077 0.358804 0.141273 0.060 Uiso 1 1 calc R U . . . H55C H 0.162294 0.345128 0.064036 0.060 Uiso 1 1 calc R U . . . C56 C 0.10570(9) 0.63081(10) 0.16454(10) 0.0284(4) Uani 1 1 d . . . . . H56 H 0.095473 0.610492 0.205453 0.034 Uiso 1 1 calc R U . . . C57 C 0.05107(12) 0.67581(13) 0.13644(14) 0.0497(6) Uani 1 1 d . . . . . H57A H 0.060144 0.696811 0.096474 0.075 Uiso 1 1 calc R U . . . H57B H 0.045730 0.709426 0.168847 0.075 Uiso 1 1 calc R U . . . H57C H 0.012342 0.650026 0.125998 0.075 Uiso 1 1 calc R U . . . C58 C 0.16564(11) 0.67077(11) 0.18332(12) 0.0386(5) Uani 1 1 d . . . . . H58A H 0.176473 0.691692 0.144079 0.058 Uiso 1 1 calc R U . . . H58B H 0.200066 0.641888 0.202806 0.058 Uiso 1 1 calc R U . . . H58C H 0.158952 0.704440 0.215182 0.058 Uiso 1 1 calc R U . . . C59 C 0.27851(8) 0.38314(9) 0.36593(9) 0.0217(3) Uani 1 1 d . . . . . C60 C 0.27432(9) 0.36246(10) 0.47139(9) 0.0273(4) Uani 1 1 d . . . . . C61 C 0.26659(9) 0.30522(10) 0.43823(10) 0.0301(4) Uani 1 1 d . . . . . C62 C 0.28925(9) 0.47949(10) 0.44248(9) 0.0273(4) Uani 1 1 d . . . . . H62A H 0.296595 0.503927 0.403714 0.041 Uiso 1 1 calc R U . . . H62B H 0.325468 0.484810 0.477713 0.041 Uiso 1 1 calc R U . . . H62C H 0.251320 0.496230 0.457108 0.041 Uiso 1 1 calc R U . . . C63 C 0.26112(10) 0.26930(10) 0.32171(11) 0.0327(4) Uani 1 1 d . . . . . H63A H 0.273033 0.287764 0.281825 0.049 Uiso 1 1 calc R U . . . H63B H 0.216973 0.255468 0.312605 0.049 Uiso 1 1 calc R U . . . H63C H 0.287868 0.231454 0.336010 0.049 Uiso 1 1 calc R U . . . C64 C 0.27502(11) 0.37799(13) 0.54224(10) 0.0405(5) Uani 1 1 d . . . . . H64A H 0.246958 0.415075 0.545809 0.061 Uiso 1 1 calc R U . . . H64B H 0.317930 0.389305 0.563083 0.061 Uiso 1 1 calc R U . . . H64C H 0.260617 0.339769 0.564211 0.061 Uiso 1 1 calc R U . . . C65 C 0.25362(13) 0.23826(12) 0.46138(13) 0.0468(6) Uani 1 1 d . . . . . H65A H 0.213631 0.222352 0.436730 0.070 Uiso 1 1 calc R U . . . H65B H 0.251075 0.239760 0.508210 0.070 Uiso 1 1 calc R U . . . H65C H 0.287650 0.208657 0.454392 0.070 Uiso 1 1 calc R U . . . F12_1 F 0.69199(5) 0.33147(5) 0.17452(5) 0.0249(2) Uani 1 1 d . . . . . F13_1 F 0.58562(6) 0.31972(6) 0.08860(6) 0.0350(3) Uani 1 1 d . . . . . F14_1 F 0.52332(6) 0.42794(7) 0.03515(6) 0.0428(3) Uani 1 1 d . . . . . F15_1 F 0.57208(6) 0.54911(7) 0.06935(6) 0.0394(3) Uani 1 1 d . . . . . F16_1 F 0.67763(5) 0.56224(5) 0.15273(5) 0.0275(2) Uani 1 1 d . . . . . F22_1 F 0.77439(5) 0.38094(5) 0.09386(5) 0.0249(2) Uani 1 1 d . . . . . F23_1 F 0.87698(5) 0.31789(6) 0.07515(5) 0.0302(2) Uani 1 1 d . . . . . F24_1 F 0.97645(5) 0.30313(6) 0.17450(6) 0.0321(3) Uani 1 1 d . . . . . F25_1 F 0.96804(5) 0.35108(6) 0.29650(6) 0.0317(3) Uani 1 1 d . . . . . F26_1 F 0.86765(5) 0.41877(5) 0.31562(5) 0.0251(2) Uani 1 1 d . . . . . F32_1 F 0.79734(5) 0.53960(5) 0.34453(5) 0.0282(2) Uani 1 1 d . . . . . F33_1 F 0.85897(6) 0.65004(6) 0.34439(7) 0.0408(3) Uani 1 1 d . . . . . F34_1 F 0.89344(7) 0.69697(6) 0.23139(8) 0.0479(4) Uani 1 1 d . . . . . F35_1 F 0.85871(6) 0.63008(6) 0.11689(7) 0.0407(3) Uani 1 1 d . . . . . F36_1 F 0.79374(5) 0.51941(5) 0.11504(5) 0.0276(2) Uani 1 1 d . . . . . F42_1 F 0.67428(5) 0.52555(5) 0.29061(5) 0.0262(2) Uani 1 1 d . . . . . F43_1 F 0.62396(6) 0.49327(6) 0.39525(6) 0.0358(3) Uani 1 1 d . . . . . F44_1 F 0.64920(7) 0.37400(7) 0.45384(6) 0.0472(3) Uani 1 1 d . . . . . F45_1 F 0.72584(7) 0.28886(6) 0.40395(6) 0.0382(3) Uani 1 1 d . . . . . F46_1 F 0.77612(5) 0.31948(5) 0.30037(5) 0.0246(2) Uani 1 1 d . . . . . C11_1 C 0.69255(8) 0.44693(9) 0.16710(8) 0.0198(3) Uani 1 1 d . . . . . C12_1 C 0.66452(8) 0.38712(9) 0.14849(8) 0.0215(3) Uani 1 1 d . . . . . C13_1 C 0.60905(9) 0.37953(10) 0.10451(9) 0.0262(4) Uani 1 1 d . . . . . C14_1 C 0.57756(9) 0.43420(11) 0.07733(9) 0.0300(4) Uani 1 1 d . . . . . C15_1 C 0.60234(9) 0.49488(10) 0.09470(9) 0.0277(4) Uani 1 1 d . . . . . C16_1 C 0.65830(8) 0.50012(9) 0.13842(9) 0.0230(4) Uani 1 1 d . . . . . C21_1 C 0.81447(8) 0.40281(8) 0.20661(8) 0.0185(3) Uani 1 1 d . . . . . C22_1 C 0.82092(8) 0.37566(9) 0.14633(9) 0.0205(3) Uani 1 1 d . . . . . C23_1 C 0.87410(9) 0.34253(9) 0.13507(9) 0.0233(4) Uani 1 1 d . . . . . C24_1 C 0.92453(8) 0.33454(9) 0.18507(10) 0.0245(4) Uani 1 1 d . . . . . C25_1 C 0.92049(8) 0.35938(9) 0.24622(9) 0.0237(4) Uani 1 1 d . . . . . C26_1 C 0.86703(8) 0.39323(8) 0.25485(9) 0.0207(3) Uani 1 1 d . . . . . C31_1 C 0.79051(8) 0.52263(8) 0.22925(9) 0.0203(3) Uani 1 1 d . . . . . C32_1 C 0.80950(8) 0.55946(9) 0.28561(9) 0.0236(4) Uani 1 1 d . . . . . C33_1 C 0.84264(9) 0.61783(9) 0.28702(11) 0.0299(4) Uani 1 1 d . . . . . C34_1 C 0.85980(9) 0.64173(9) 0.23054(12) 0.0327(4) Uani 1 1 d . . . . . C35_1 C 0.84254(9) 0.60747(10) 0.17314(11) 0.0295(4) Uani 1 1 d . . . . . C36_1 C 0.80904(8) 0.55007(9) 0.17357(9) 0.0238(4) Uani 1 1 d . . . . . C41_1 C 0.73013(8) 0.42595(8) 0.29048(8) 0.0190(3) Uani 1 1 d . . . . . C42_1 C 0.68956(8) 0.46615(9) 0.31795(8) 0.0216(3) Uani 1 1 d . . . . . C43_1 C 0.66225(9) 0.45058(10) 0.37178(9) 0.0274(4) Uani 1 1 d . . . . . C44_1 C 0.67457(10) 0.39057(11) 0.40132(9) 0.0308(4) Uani 1 1 d . . . . . C45_1 C 0.71329(9) 0.34780(10) 0.37585(9) 0.0270(4) Uani 1 1 d . . . . . C46_1 C 0.73979(8) 0.36569(9) 0.32170(8) 0.0213(3) Uani 1 1 d . . . . . B1_1 B 0.75668(9) 0.44944(9) 0.22351(9) 0.0181(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02224(13) 0.02259(10) 0.01625(12) -0.00073(8) -0.00008(9) 0.00309(10) Br2 0.02256(12) 0.01996(11) 0.02964(11) 0.00047(8) 0.00188(8) 0.00113(8) Ga1 0.01262(15) 0.01377(13) 0.01572(19) -0.00104(18) 0.00274(15) -0.00004(10) Ga2 0.01250(14) 0.01768(18) 0.01556(15) 0.00012(13) 0.00070(10) 0.00096(12) P1 0.0134(2) 0.0176(2) 0.0182(2) 0.00030(16) 0.00297(15) -0.00033(16) P2 0.0141(2) 0.0196(2) 0.0262(2) 0.00480(18) 0.00248(17) 0.00010(16) Ga1' 0.030(4) 0.027(3) 0.039(5) -0.015(5) 0.014(4) -0.008(3) Br1' 0.049(4) 0.035(2) 0.035(3) 0.000(2) 0.018(3) -0.002(2) P1' 0.030(5) 0.058(7) 0.035(5) 0.009(5) 0.006(4) -0.007(4) Ga2' 0.037(3) 0.041(4) 0.036(4) -0.004(2) 0.003(2) 0.005(2) Br2' 0.081(4) 0.109(5) 0.132(5) 0.011(4) 0.047(4) -0.028(4) P2' 0.045(5) 0.037(5) 0.028(5) 0.013(4) 0.000(4) 0.003(4) N1 0.0161(6) 0.0152(6) 0.0222(7) -0.0020(5) 0.0034(5) 0.0003(5) N2 0.0150(6) 0.0157(6) 0.0211(7) -0.0004(5) 0.0023(5) 0.0006(5) N3 0.0163(7) 0.0224(7) 0.0174(7) -0.0019(5) 0.0006(5) 0.0015(5) N4 0.0154(6) 0.0228(7) 0.0175(7) 0.0005(5) 0.0023(5) -0.0008(5) N5 0.0191(7) 0.0266(8) 0.0222(7) 0.0048(6) 0.0024(6) -0.0008(6) N6 0.0187(7) 0.0257(8) 0.0312(8) 0.0031(6) 0.0038(6) -0.0011(6) C1 0.0154(7) 0.0209(8) 0.0176(8) -0.0016(6) 0.0018(6) 0.0024(6) C2 0.0132(7) 0.0229(8) 0.0237(8) 0.0002(7) 0.0039(6) 0.0006(6) C3 0.0166(8) 0.0201(8) 0.0193(8) -0.0007(6) 0.0026(6) -0.0015(6) C4 0.0209(8) 0.0219(9) 0.0366(10) -0.0017(7) 0.0102(8) 0.0039(7) C5 0.0198(8) 0.0205(8) 0.0341(10) 0.0025(7) 0.0097(7) -0.0008(7) C6 0.0174(8) 0.0166(8) 0.0286(9) -0.0063(7) 0.0072(7) 0.0003(6) C7 0.0208(8) 0.0175(8) 0.0335(10) -0.0030(7) 0.0105(7) 0.0021(7) C8 0.0292(10) 0.0179(9) 0.0461(12) -0.0028(8) 0.0158(9) 0.0002(7) C9 0.0291(10) 0.0197(9) 0.0589(14) -0.0157(9) 0.0137(10) -0.0055(8) C10 0.0264(10) 0.0293(10) 0.0442(12) -0.0174(9) 0.0028(9) -0.0035(8) C11 0.0214(8) 0.0223(9) 0.0319(10) -0.0101(7) 0.0031(7) 0.0021(7) C12 0.0281(9) 0.0219(9) 0.0293(9) 0.0031(7) 0.0076(8) 0.0032(7) C13 0.0375(11) 0.0316(11) 0.0437(12) 0.0066(9) 0.0048(10) 0.0116(9) C14 0.0450(12) 0.0316(11) 0.0324(11) 0.0041(9) 0.0141(9) 0.0005(9) C15 0.0284(10) 0.0296(10) 0.0280(10) -0.0091(8) -0.0041(8) 0.0051(8) C16 0.0413(12) 0.0434(13) 0.0380(12) 0.0007(10) 0.0087(10) 0.0114(10) C17 0.0323(11) 0.0543(14) 0.0370(12) -0.0144(10) -0.0050(9) 0.0128(10) C18 0.0151(7) 0.0158(8) 0.0261(8) 0.0036(6) 0.0047(6) 0.0004(6) C19 0.0187(8) 0.0176(8) 0.0290(9) 0.0001(7) 0.0079(7) -0.0015(6) C20 0.0254(9) 0.0175(8) 0.0386(10) 0.0001(7) 0.0102(8) 0.0015(7) C21 0.0267(9) 0.0202(9) 0.0441(12) 0.0057(8) 0.0076(8) 0.0044(7) C22 0.0226(9) 0.0267(10) 0.0356(10) 0.0086(8) 0.0019(8) 0.0025(7) C23 0.0175(8) 0.0223(8) 0.0279(9) 0.0042(7) 0.0034(7) 0.0000(7) C24 0.0244(9) 0.0198(8) 0.0260(9) -0.0037(7) 0.0069(7) -0.0008(7) C25 0.0303(10) 0.0285(10) 0.0360(11) -0.0075(8) 0.0047(8) -0.0069(8) C26 0.0364(11) 0.0286(10) 0.0299(10) -0.0024(8) 0.0126(8) 0.0007(8) C27 0.0264(9) 0.0274(9) 0.0252(9) 0.0022(7) -0.0025(7) 0.0025(7) C28 0.0345(11) 0.0521(14) 0.0318(11) -0.0084(10) 0.0048(9) 0.0016(10) C29 0.0306(11) 0.0469(13) 0.0325(11) 0.0004(9) -0.0063(9) 0.0015(9) C30 0.0174(8) 0.0201(8) 0.0217(8) 0.0001(6) 0.0028(6) 0.0022(6) C31 0.0137(7) 0.0225(8) 0.0222(8) 0.0007(7) 0.0013(6) 0.0000(6) C32 0.0156(8) 0.0186(8) 0.0210(8) -0.0004(6) 0.0001(6) 0.0001(6) C33 0.0191(8) 0.0418(11) 0.0221(9) -0.0047(8) 0.0017(7) 0.0075(8) C34 0.0179(8) 0.0362(10) 0.0210(8) 0.0006(7) 0.0010(7) 0.0018(7) C35 0.0152(7) 0.0267(9) 0.0184(8) -0.0039(7) -0.0001(6) 0.0045(7) C36 0.0177(8) 0.0286(9) 0.0206(8) -0.0019(7) 0.0014(6) 0.0032(7) C37 0.0235(9) 0.0357(10) 0.0194(8) -0.0003(7) 0.0007(7) 0.0034(8) C38 0.0267(9) 0.0380(11) 0.0210(9) -0.0070(8) -0.0015(7) 0.0051(8) C39 0.0266(9) 0.0281(9) 0.0276(9) -0.0078(8) -0.0017(7) 0.0026(8) C40 0.0208(8) 0.0236(9) 0.0243(9) -0.0039(7) -0.0003(7) 0.0054(7) C41 0.0219(9) 0.0315(10) 0.0212(8) -0.0009(7) 0.0029(7) -0.0011(7) C42 0.0326(11) 0.0488(13) 0.0343(11) -0.0052(10) 0.0128(9) -0.0089(10) C43 0.0328(11) 0.0307(10) 0.0360(11) 0.0038(8) -0.0009(9) -0.0002(8) C44 0.0292(10) 0.0225(9) 0.0270(9) -0.0043(7) 0.0000(7) 0.0013(7) C45 0.0394(12) 0.0251(10) 0.0414(12) 0.0010(9) 0.0008(9) 0.0076(9) C46 0.0387(12) 0.0353(11) 0.0400(12) 0.0000(9) -0.0017(9) -0.0089(9) C47 0.0137(7) 0.0303(9) 0.0172(8) 0.0022(7) 0.0001(6) -0.0015(7) C48 0.0150(8) 0.0348(10) 0.0212(8) -0.0019(7) -0.0005(6) -0.0009(7) C49 0.0194(9) 0.0463(12) 0.0203(9) -0.0036(8) 0.0022(7) -0.0002(8) C50 0.0233(9) 0.0535(13) 0.0196(9) 0.0054(8) 0.0027(7) -0.0065(9) C51 0.0248(9) 0.0388(11) 0.0250(9) 0.0074(8) 0.0012(7) -0.0074(8) C52 0.0194(8) 0.0321(10) 0.0228(9) 0.0022(7) -0.0003(7) -0.0031(7) C53 0.0241(9) 0.0317(10) 0.0233(9) -0.0053(7) 0.0036(7) -0.0001(8) C54 0.0368(11) 0.0421(12) 0.0311(11) -0.0113(9) 0.0035(9) -0.0102(9) C55 0.0388(12) 0.0408(12) 0.0421(12) -0.0030(10) 0.0095(10) 0.0095(10) C56 0.0285(10) 0.0291(10) 0.0268(9) 0.0026(8) 0.0024(8) -0.0065(8) C57 0.0448(14) 0.0446(14) 0.0544(15) -0.0121(12) -0.0066(11) 0.0093(11) C58 0.0371(12) 0.0359(11) 0.0416(12) -0.0007(9) 0.0037(9) -0.0134(9) C59 0.0162(8) 0.0233(9) 0.0254(9) 0.0017(7) 0.0024(7) -0.0011(7) C60 0.0223(9) 0.0343(10) 0.0253(9) 0.0118(8) 0.0043(7) 0.0031(8) C61 0.0230(9) 0.0322(10) 0.0348(10) 0.0129(8) 0.0045(8) 0.0043(8) C62 0.0270(9) 0.0288(10) 0.0260(9) -0.0021(7) 0.0041(7) 0.0018(8) C63 0.0294(10) 0.0238(9) 0.0449(12) -0.0034(8) 0.0066(9) -0.0023(8) C64 0.0413(12) 0.0547(14) 0.0262(10) 0.0106(10) 0.0076(9) 0.0023(11) C65 0.0477(14) 0.0380(13) 0.0544(15) 0.0208(11) 0.0080(12) -0.0016(11) F12_1 0.0241(5) 0.0233(5) 0.0259(5) 0.0019(4) 0.0004(4) -0.0026(4) F13_1 0.0305(6) 0.0394(7) 0.0322(6) -0.0030(5) -0.0032(5) -0.0134(5) F14_1 0.0252(6) 0.0628(9) 0.0337(7) 0.0036(6) -0.0144(5) -0.0036(6) F15_1 0.0318(6) 0.0449(7) 0.0367(7) 0.0095(6) -0.0081(5) 0.0145(5) F16_1 0.0270(6) 0.0238(5) 0.0299(6) 0.0013(4) -0.0005(4) 0.0067(4) F22_1 0.0238(5) 0.0318(6) 0.0188(5) -0.0004(4) 0.0028(4) 0.0021(4) F23_1 0.0337(6) 0.0323(6) 0.0274(6) -0.0036(5) 0.0130(5) 0.0042(5) F24_1 0.0197(5) 0.0287(6) 0.0495(7) -0.0050(5) 0.0105(5) 0.0048(4) F25_1 0.0194(5) 0.0328(6) 0.0393(6) -0.0012(5) -0.0057(5) 0.0044(4) F26_1 0.0217(5) 0.0292(5) 0.0223(5) -0.0038(4) -0.0024(4) 0.0026(4) F32_1 0.0314(6) 0.0288(6) 0.0223(5) -0.0039(4) -0.0014(4) 0.0000(5) F33_1 0.0405(7) 0.0280(6) 0.0491(8) -0.0145(5) -0.0057(6) -0.0032(5) F34_1 0.0441(8) 0.0200(6) 0.0791(10) 0.0020(6) 0.0089(7) -0.0096(5) F35_1 0.0429(7) 0.0302(6) 0.0533(8) 0.0162(6) 0.0203(6) 0.0010(5) F36_1 0.0305(6) 0.0294(6) 0.0241(5) 0.0038(4) 0.0082(4) 0.0014(4) F42_1 0.0247(5) 0.0249(5) 0.0285(5) 0.0007(4) 0.0032(4) 0.0083(4) F43_1 0.0338(6) 0.0449(7) 0.0316(6) -0.0099(5) 0.0137(5) 0.0062(5) F44_1 0.0622(9) 0.0560(9) 0.0306(7) 0.0055(6) 0.0285(6) -0.0011(7) F45_1 0.0545(8) 0.0304(6) 0.0312(6) 0.0121(5) 0.0116(6) 0.0005(6) F46_1 0.0278(5) 0.0191(5) 0.0271(5) 0.0024(4) 0.0054(4) 0.0033(4) C11_1 0.0179(8) 0.0256(9) 0.0161(7) 0.0007(6) 0.0035(6) 0.0012(7) C12_1 0.0189(8) 0.0268(9) 0.0189(8) 0.0025(7) 0.0032(6) 0.0004(7) C13_1 0.0219(9) 0.0344(10) 0.0220(9) 0.0001(7) 0.0025(7) -0.0059(7) C14_1 0.0204(9) 0.0462(12) 0.0208(9) 0.0022(8) -0.0044(7) -0.0009(8) C15_1 0.0223(9) 0.0369(11) 0.0225(9) 0.0050(8) -0.0003(7) 0.0085(8) C16_1 0.0220(8) 0.0274(9) 0.0196(8) 0.0004(7) 0.0037(7) 0.0029(7) C21_1 0.0170(8) 0.0177(8) 0.0206(8) 0.0019(6) 0.0028(6) -0.0002(6) C22_1 0.0193(8) 0.0207(8) 0.0216(8) 0.0017(7) 0.0038(6) -0.0012(6) C23_1 0.0262(9) 0.0208(8) 0.0247(9) -0.0018(7) 0.0092(7) -0.0012(7) C24_1 0.0180(8) 0.0182(8) 0.0386(10) -0.0007(7) 0.0089(7) 0.0015(7) C25_1 0.0179(8) 0.0201(8) 0.0311(9) 0.0013(7) -0.0016(7) -0.0007(7) C26_1 0.0203(8) 0.0180(8) 0.0234(8) -0.0009(6) 0.0024(7) -0.0006(6) C31_1 0.0163(8) 0.0182(8) 0.0257(9) 0.0019(7) 0.0013(6) 0.0030(6) C32_1 0.0209(8) 0.0209(8) 0.0279(9) 0.0010(7) 0.0012(7) 0.0031(7) C33_1 0.0254(9) 0.0221(9) 0.0394(11) -0.0055(8) -0.0028(8) 0.0024(7) C34_1 0.0245(9) 0.0169(9) 0.0557(13) 0.0039(8) 0.0037(9) -0.0011(7) C35_1 0.0260(9) 0.0227(9) 0.0413(11) 0.0102(8) 0.0103(8) 0.0043(7) C36_1 0.0206(8) 0.0214(9) 0.0293(9) 0.0026(7) 0.0041(7) 0.0045(7) C41_1 0.0170(8) 0.0217(8) 0.0174(8) -0.0013(6) 0.0004(6) -0.0008(6) C42_1 0.0201(8) 0.0245(9) 0.0192(8) 0.0000(7) 0.0001(6) 0.0026(7) C43_1 0.0234(9) 0.0360(10) 0.0231(9) -0.0078(8) 0.0055(7) 0.0015(8) C44_1 0.0332(10) 0.0407(11) 0.0203(9) 0.0023(8) 0.0096(8) -0.0036(9) C45_1 0.0317(10) 0.0270(9) 0.0219(9) 0.0034(7) 0.0033(7) -0.0028(8) C46_1 0.0211(8) 0.0226(9) 0.0198(8) -0.0005(7) 0.0020(6) -0.0002(7) B1_1 0.0178(8) 0.0194(9) 0.0171(8) 0.0014(7) 0.0027(7) 0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ga1 2.3498(5) . ? Br2 Ga2 2.3403(6) . ? Ga1 N2 1.9308(15) . ? Ga1 N1 1.9422(15) . ? Ga1 P1 2.3591(8) . ? Ga2 N4 1.9336(15) . ? Ga2 N3 1.9553(15) . ? Ga2 P2 2.3522(7) . ? P1 C59 1.8262(19) . ? P1 P2 2.1336(7) . ? Ga1' N2 1.797(13) . ? Ga1' N1 1.915(13) . ? Ga1' Br1' 2.329(9) . ? Ga1' P1' 2.388(15) . ? P1' P2' 2.107(15) . ? Ga2' N3 1.910(12) . ? Ga2' N4 2.131(11) . ? Ga2' P2' 2.336(16) . ? Ga2' Br2' 2.488(13) . ? P2' C59 2.256(10) . ? N1 C1 1.338(2) . ? N1 C6 1.443(2) . ? N2 C3 1.337(2) . ? N2 C18 1.452(2) . ? N3 C30 1.333(2) . ? N3 C35 1.447(2) . ? N4 C32 1.341(2) . ? N4 C47 1.451(2) . ? N5 C59 1.355(2) . ? N5 C60 1.380(2) . ? N5 C62 1.456(2) . ? N6 C59 1.341(2) . ? N6 C61 1.379(3) . ? N6 C63 1.463(3) . ? C1 C2 1.391(2) . ? C1 C4 1.507(2) . ? C2 C3 1.400(2) . ? C3 C5 1.505(2) . ? C6 C7 1.408(3) . ? C6 C11 1.408(3) . ? C7 C8 1.395(3) . ? C7 C12 1.516(3) . ? C8 C9 1.387(3) . ? C9 C10 1.379(3) . ? C10 C11 1.392(3) . ? C11 C15 1.525(3) . ? C12 C13 1.537(3) . ? C12 C14 1.538(3) . ? C15 C17 1.525(3) . ? C15 C16 1.532(3) . ? C18 C23 1.405(2) . ? C18 C19 1.406(2) . ? C19 C20 1.396(2) . ? C19 C24 1.519(3) . ? C20 C21 1.380(3) . ? C21 C22 1.380(3) . ? C22 C23 1.395(3) . ? C23 C27 1.523(3) . ? C24 C25 1.534(3) . ? C24 C26 1.539(2) . ? C27 C29 1.529(3) . ? C27 C28 1.531(3) . ? C30 C31 1.401(2) . ? C30 C33 1.512(2) . ? C31 C32 1.394(2) . ? C32 C34 1.505(2) . ? C35 C36 1.405(3) . ? C35 C40 1.411(3) . ? C36 C37 1.404(2) . ? C36 C41 1.524(3) . ? C37 C38 1.383(3) . ? C38 C39 1.385(3) . ? C39 C40 1.396(3) . ? C40 C44 1.522(3) . ? C41 C43 1.527(3) . ? C41 C42 1.538(3) . ? C44 C45 1.528(3) . ? C44 C46 1.531(3) . ? C47 C52 1.403(3) . ? C47 C48 1.406(3) . ? C48 C49 1.400(3) . ? C48 C53 1.519(3) . ? C49 C50 1.378(3) . ? C50 C51 1.384(3) . ? C51 C52 1.403(3) . ? C52 C56 1.525(3) . ? C53 C55 1.528(3) . ? C53 C54 1.539(3) . ? C56 C58 1.522(3) . ? C56 C57 1.529(3) . ? C60 C61 1.352(3) . ? C60 C64 1.497(3) . ? C61 C65 1.491(3) . ? F12_1 C12_1 1.351(2) . ? F13_1 C13_1 1.342(2) . ? F14_1 C14_1 1.342(2) . ? F15_1 C15_1 1.346(2) . ? F16_1 C16_1 1.353(2) . ? F22_1 C22_1 1.352(2) . ? F23_1 C23_1 1.349(2) . ? F24_1 C24_1 1.340(2) . ? F25_1 C25_1 1.342(2) . ? F26_1 C26_1 1.359(2) . ? F32_1 C32_1 1.351(2) . ? F33_1 C33_1 1.351(2) . ? F34_1 C34_1 1.340(2) . ? F35_1 C35_1 1.351(2) . ? F36_1 C36_1 1.354(2) . ? F42_1 C42_1 1.356(2) . ? F43_1 C43_1 1.346(2) . ? F44_1 C44_1 1.340(2) . ? F45_1 C45_1 1.345(2) . ? F46_1 C46_1 1.348(2) . ? C11_1 C12_1 1.389(3) . ? C11_1 C16_1 1.389(2) . ? C11_1 B1_1 1.652(3) . ? C12_1 C13_1 1.384(3) . ? C13_1 C14_1 1.377(3) . ? C14_1 C15_1 1.374(3) . ? C15_1 C16_1 1.384(3) . ? C21_1 C26_1 1.391(2) . ? C21_1 C22_1 1.393(2) . ? C21_1 B1_1 1.652(2) . ? C22_1 C23_1 1.385(2) . ? C23_1 C24_1 1.378(3) . ? C24_1 C25_1 1.379(3) . ? C25_1 C26_1 1.381(2) . ? C31_1 C32_1 1.390(3) . ? C31_1 C36_1 1.398(2) . ? C31_1 B1_1 1.659(3) . ? C32_1 C33_1 1.388(3) . ? C33_1 C34_1 1.373(3) . ? C34_1 C35_1 1.374(3) . ? C35_1 C36_1 1.378(3) . ? C41_1 C42_1 1.389(2) . ? C41_1 C46_1 1.390(2) . ? C41_1 B1_1 1.657(2) . ? C42_1 C43_1 1.382(3) . ? C43_1 C44_1 1.376(3) . ? C44_1 C45_1 1.374(3) . ? C45_1 C46_1 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ga1 N1 97.57(6) . . ? N2 Ga1 Br1 108.74(5) . . ? N1 Ga1 Br1 104.00(5) . . ? N2 Ga1 P1 119.49(5) . . ? N1 Ga1 P1 111.16(5) . . ? Br1 Ga1 P1 113.71(3) . . ? N4 Ga2 N3 96.91(6) . . ? N4 Ga2 Br2 105.42(5) . . ? N3 Ga2 Br2 104.47(5) . . ? N4 Ga2 P2 111.79(5) . . ? N3 Ga2 P2 120.45(5) . . ? Br2 Ga2 P2 115.40(2) . . ? C59 P1 P2 111.85(6) . . ? C59 P1 Ga1 100.18(6) . . ? P2 P1 Ga1 113.07(3) . . ? P1 P2 Ga2 101.59(3) . . ? N2 Ga1' N1 103.4(6) . . ? N2 Ga1' Br1' 102.1(5) . . ? N1 Ga1' Br1' 96.0(5) . . ? N2 Ga1' P1' 105.1(6) . . ? N1 Ga1' P1' 125.8(6) . . ? Br1' Ga1' P1' 121.2(6) . . ? P2' P1' Ga1' 102.1(6) . . ? N3 Ga2' N4 92.0(5) . . ? N3 Ga2' P2' 108.7(6) . . ? N4 Ga2' P2' 124.0(5) . . ? N3 Ga2' Br2' 106.2(5) . . ? N4 Ga2' Br2' 106.5(5) . . ? P2' Ga2' Br2' 115.8(6) . . ? P1' P2' C59 93.1(5) . . ? P1' P2' Ga2' 109.9(6) . . ? C59 P2' Ga2' 108.3(5) . . ? C1 N1 C6 120.05(14) . . ? C1 N1 Ga1' 118.6(4) . . ? C6 N1 Ga1' 119.3(4) . . ? C1 N1 Ga1 118.72(11) . . ? C6 N1 Ga1 121.22(11) . . ? C3 N2 C18 119.74(14) . . ? C3 N2 Ga1' 120.5(4) . . ? C18 N2 Ga1' 119.1(4) . . ? C3 N2 Ga1 117.95(12) . . ? C18 N2 Ga1 122.01(11) . . ? C30 N3 C35 118.90(14) . . ? C30 N3 Ga2' 119.8(4) . . ? C35 N3 Ga2' 118.9(4) . . ? C30 N3 Ga2 119.67(12) . . ? C35 N3 Ga2 121.23(11) . . ? C32 N4 C47 118.16(14) . . ? C32 N4 Ga2 120.00(12) . . ? C47 N4 Ga2 121.83(11) . . ? C32 N4 Ga2' 114.4(3) . . ? C47 N4 Ga2' 127.1(3) . . ? C59 N5 C60 109.84(16) . . ? C59 N5 C62 126.65(15) . . ? C60 N5 C62 123.50(16) . . ? C59 N6 C61 110.03(17) . . ? C59 N6 C63 126.49(17) . . ? C61 N6 C63 123.46(17) . . ? N1 C1 C2 123.37(15) . . ? N1 C1 C4 119.34(15) . . ? C2 C1 C4 117.28(15) . . ? C1 C2 C3 128.65(15) . . ? N2 C3 C2 124.35(15) . . ? N2 C3 C5 119.42(15) . . ? C2 C3 C5 116.23(15) . . ? C7 C6 C11 122.02(16) . . ? C7 C6 N1 120.64(16) . . ? C11 C6 N1 117.34(16) . . ? C8 C7 C6 117.44(18) . . ? C8 C7 C12 119.00(18) . . ? C6 C7 C12 123.55(16) . . ? C9 C8 C7 121.3(2) . . ? C10 C9 C8 119.99(18) . . ? C9 C10 C11 121.4(2) . . ? C10 C11 C6 117.70(19) . . ? C10 C11 C15 119.55(18) . . ? C6 C11 C15 122.72(16) . . ? C7 C12 C13 111.53(16) . . ? C7 C12 C14 111.28(17) . . ? C13 C12 C14 108.96(17) . . ? C11 C15 C17 112.04(19) . . ? C11 C15 C16 111.53(17) . . ? C17 C15 C16 110.11(17) . . ? C23 C18 C19 122.01(16) . . ? C23 C18 N2 118.22(15) . . ? C19 C18 N2 119.77(15) . . ? C20 C19 C18 117.80(17) . . ? C20 C19 C24 118.85(16) . . ? C18 C19 C24 123.35(16) . . ? C21 C20 C19 120.94(18) . . ? C20 C21 C22 120.44(18) . . ? C21 C22 C23 121.18(19) . . ? C22 C23 C18 117.60(17) . . ? C22 C23 C27 120.53(17) . . ? C18 C23 C27 121.86(16) . . ? C19 C24 C25 111.32(15) . . ? C19 C24 C26 111.41(15) . . ? C25 C24 C26 109.01(16) . . ? C23 C27 C29 113.02(17) . . ? C23 C27 C28 112.56(17) . . ? C29 C27 C28 109.36(17) . . ? N3 C30 C31 124.07(15) . . ? N3 C30 C33 120.40(15) . . ? C31 C30 C33 115.50(15) . . ? C32 C31 C30 128.59(16) . . ? N4 C32 C31 123.21(15) . . ? N4 C32 C34 119.21(15) . . ? C31 C32 C34 117.57(15) . . ? C36 C35 C40 121.99(16) . . ? C36 C35 N3 120.01(16) . . ? C40 C35 N3 117.97(16) . . ? C37 C36 C35 117.57(17) . . ? C37 C36 C41 119.03(17) . . ? C35 C36 C41 123.38(16) . . ? C38 C37 C36 121.40(18) . . ? C37 C38 C39 119.83(18) . . ? C38 C39 C40 121.52(18) . . ? C39 C40 C35 117.65(17) . . ? C39 C40 C44 121.01(17) . . ? C35 C40 C44 121.31(16) . . ? C36 C41 C43 111.35(15) . . ? C36 C41 C42 112.78(16) . . ? C43 C41 C42 108.36(17) . . ? C40 C44 C45 110.83(17) . . ? C40 C44 C46 113.43(17) . . ? C45 C44 C46 110.21(17) . . ? C52 C47 C48 122.02(16) . . ? C52 C47 N4 117.48(16) . . ? C48 C47 N4 120.49(16) . . ? C49 C48 C47 117.56(18) . . ? C49 C48 C53 119.61(17) . . ? C47 C48 C53 122.81(16) . . ? C50 C49 C48 121.34(19) . . ? C49 C50 C51 120.30(18) . . ? C50 C51 C52 120.82(19) . . ? C51 C52 C47 117.90(18) . . ? C51 C52 C56 119.46(18) . . ? C47 C52 C56 122.63(16) . . ? C48 C53 C55 111.16(17) . . ? C48 C53 C54 111.41(17) . . ? C55 C53 C54 109.92(17) . . ? C58 C56 C52 112.05(17) . . ? C58 C56 C57 109.91(19) . . ? C52 C56 C57 111.34(17) . . ? N6 C59 N5 106.21(16) . . ? N6 C59 P1 123.32(14) . . ? N5 C59 P1 130.36(14) . . ? N6 C59 P2' 143.0(3) . . ? N5 C59 P2' 94.5(3) . . ? C61 C60 N5 106.69(17) . . ? C61 C60 C64 131.31(19) . . ? N5 C60 C64 121.99(19) . . ? C60 C61 N6 107.21(17) . . ? C60 C61 C65 130.1(2) . . ? N6 C61 C65 122.6(2) . . ? C12_1 C11_1 C16_1 113.27(16) . . ? C12_1 C11_1 B1_1 119.74(15) . . ? C16_1 C11_1 B1_1 126.73(16) . . ? F12_1 C12_1 C13_1 116.09(16) . . ? F12_1 C12_1 C11_1 119.28(15) . . ? C13_1 C12_1 C11_1 124.63(17) . . ? F13_1 C13_1 C14_1 119.97(17) . . ? F13_1 C13_1 C12_1 120.73(18) . . ? C14_1 C13_1 C12_1 119.30(18) . . ? F14_1 C14_1 C15_1 120.92(19) . . ? F14_1 C14_1 C13_1 120.24(19) . . ? C15_1 C14_1 C13_1 118.84(17) . . ? F15_1 C15_1 C14_1 119.97(17) . . ? F15_1 C15_1 C16_1 120.14(18) . . ? C14_1 C15_1 C16_1 119.88(18) . . ? F16_1 C16_1 C15_1 114.69(16) . . ? F16_1 C16_1 C11_1 121.24(16) . . ? C15_1 C16_1 C11_1 124.06(18) . . ? C26_1 C21_1 C22_1 113.18(15) . . ? C26_1 C21_1 B1_1 118.77(15) . . ? C22_1 C21_1 B1_1 127.72(15) . . ? F22_1 C22_1 C23_1 115.29(15) . . ? F22_1 C22_1 C21_1 120.94(15) . . ? C23_1 C22_1 C21_1 123.77(17) . . ? F23_1 C23_1 C24_1 119.51(16) . . ? F23_1 C23_1 C22_1 120.32(17) . . ? C24_1 C23_1 C22_1 120.17(17) . . ? F24_1 C24_1 C23_1 120.61(17) . . ? F24_1 C24_1 C25_1 120.65(17) . . ? C23_1 C24_1 C25_1 118.74(16) . . ? F25_1 C25_1 C24_1 120.40(16) . . ? F25_1 C25_1 C26_1 120.52(17) . . ? C24_1 C25_1 C26_1 119.08(17) . . ? F26_1 C26_1 C25_1 115.70(16) . . ? F26_1 C26_1 C21_1 119.27(15) . . ? C25_1 C26_1 C21_1 125.02(17) . . ? C32_1 C31_1 C36_1 112.89(16) . . ? C32_1 C31_1 B1_1 127.72(16) . . ? C36_1 C31_1 B1_1 119.05(15) . . ? F32_1 C32_1 C33_1 114.61(17) . . ? F32_1 C32_1 C31_1 121.28(16) . . ? C33_1 C32_1 C31_1 124.10(18) . . ? F33_1 C33_1 C34_1 120.42(18) . . ? F33_1 C33_1 C32_1 119.62(19) . . ? C34_1 C33_1 C32_1 119.95(19) . . ? F34_1 C34_1 C33_1 120.8(2) . . ? F34_1 C34_1 C35_1 120.5(2) . . ? C33_1 C34_1 C35_1 118.76(18) . . ? F35_1 C35_1 C34_1 119.88(18) . . ? F35_1 C35_1 C36_1 120.54(19) . . ? C34_1 C35_1 C36_1 119.58(18) . . ? F36_1 C36_1 C35_1 115.91(17) . . ? F36_1 C36_1 C31_1 119.38(16) . . ? C35_1 C36_1 C31_1 124.71(18) . . ? C42_1 C41_1 C46_1 112.90(16) . . ? C42_1 C41_1 B1_1 120.06(15) . . ? C46_1 C41_1 B1_1 126.83(15) . . ? F42_1 C42_1 C43_1 115.83(16) . . ? F42_1 C42_1 C41_1 118.95(15) . . ? C43_1 C42_1 C41_1 125.22(17) . . ? F43_1 C43_1 C44_1 120.08(17) . . ? F43_1 C43_1 C42_1 120.79(18) . . ? C44_1 C43_1 C42_1 119.12(17) . . ? F44_1 C44_1 C45_1 120.53(19) . . ? F44_1 C44_1 C43_1 120.72(18) . . ? C45_1 C44_1 C43_1 118.75(17) . . ? F45_1 C45_1 C44_1 119.68(17) . . ? F45_1 C45_1 C46_1 120.25(17) . . ? C44_1 C45_1 C46_1 120.07(18) . . ? F46_1 C46_1 C45_1 114.86(16) . . ? F46_1 C46_1 C41_1 121.22(15) . . ? C45_1 C46_1 C41_1 123.92(17) . . ? C21_1 B1_1 C11_1 113.81(14) . . ? C21_1 B1_1 C41_1 112.90(14) . . ? C11_1 B1_1 C41_1 102.44(13) . . ? C21_1 B1_1 C31_1 101.35(13) . . ? C11_1 B1_1 C31_1 112.57(14) . . ? C41_1 B1_1 C31_1 114.26(14) . . ? _refine_diff_density_max 0.430 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.054 _shelx_res_file ; TITL mks_056m in P2(1)/c mks_056m.res created by SHELXL-2017/1 at 16:28:58 on 28-Jul-2021 CELL 1.54178 21.55740 20.43160 20.68420 90.0000 99.7202 90.0000 ZERR 4.00000 0.00220 0.00220 0.00220 0.0000 0.0050 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H B Br F Ga N P UNIT 356 376 4 8 80 8 24 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! SIZE 0.096 0.112 0.130 TEMP -173.150 L.S. 16 ACTA FMAP 2 PLAN 20 RIGU ga1' ga2' p1' p2' br1' br2' SIMU ga1' ga2' p1' p2' br1' br2' ISOR 0.003 Br2' ga2' WGHT 0.030700 6.351800 FVAR 0.04168 0.94277 PART 1 21 BR1 4 0.441801 0.440257 0.422876 21.00000 0.02224 0.02259 = 0.01625 -0.00073 -0.00008 0.00309 BR2 4 0.122928 0.355758 0.273769 21.00000 0.02256 0.01996 = 0.02964 0.00047 0.00188 0.00113 GA1 6 0.399569 0.438620 0.310463 21.00000 0.01262 0.01377 = 0.01572 -0.00104 0.00274 -0.00004 GA2 6 0.133584 0.469478 0.267689 21.00000 0.01250 0.01768 = 0.01556 0.00012 0.00070 0.00096 P1 8 0.290054 0.419855 0.288345 21.00000 0.01343 0.01762 = 0.01822 0.00030 0.00297 -0.00033 P2 8 0.236567 0.507485 0.267603 21.00000 0.01410 0.01962 = 0.02623 0.00480 0.00248 0.00010 PART 0 PART 2 -21 GA1' 6 0.391636 0.440470 0.288636 -21.00000 0.02951 0.02651 = 0.03865 -0.01451 0.01391 -0.00800 BR1' 4 0.415194 0.439810 0.402731 -21.00000 0.04903 0.03457 = 0.03506 -0.00027 0.01787 -0.00228 P1' 8 0.286475 0.456826 0.232734 -21.00000 0.02971 0.05806 = 0.03535 0.00878 0.00650 -0.00691 GA2' 6 0.129739 0.454580 0.276173 -21.00000 0.03691 0.04118 = 0.03625 -0.00357 0.00313 0.00542 BR2' 4 0.094041 0.339163 0.281332 -21.00000 0.08089 0.10875 = 0.13184 0.01107 0.04654 -0.02847 P2' 8 0.237175 0.472698 0.311061 -21.00000 0.04520 0.03728 = 0.02768 0.01276 0.00009 0.00327 PART 0 N1 7 0.445175 0.368598 0.275617 11.00000 0.01615 0.01518 = 0.02221 -0.00203 0.00341 0.00027 N2 7 0.434691 0.510663 0.268193 11.00000 0.01497 0.01566 = 0.02106 -0.00035 0.00227 0.00058 N3 7 0.083796 0.503771 0.330849 11.00000 0.01629 0.02245 = 0.01737 -0.00195 0.00061 0.00153 N4 7 0.076880 0.495667 0.189322 11.00000 0.01542 0.02276 = 0.01753 0.00051 0.00229 -0.00079 N5 7 0.280855 0.410408 0.426020 11.00000 0.01912 0.02656 = 0.02222 0.00477 0.00236 -0.00084 N6 7 0.269290 0.318873 0.373475 11.00000 0.01874 0.02568 = 0.03116 0.00315 0.00379 -0.00106 C1 1 0.502083 0.381401 0.261041 11.00000 0.01540 0.02092 = 0.01758 -0.00164 0.00180 0.00235 C2 1 0.525266 0.444463 0.256497 11.00000 0.01323 0.02289 = 0.02374 0.00022 0.00387 0.00055 AFIX 43 H2 2 0.568766 0.447489 0.253967 11.00000 -1.20000 AFIX 0 C3 1 0.493054 0.504059 0.255154 11.00000 0.01656 0.02007 = 0.01929 -0.00068 0.00256 -0.00151 C4 1 0.543640 0.325469 0.247545 11.00000 0.02088 0.02190 = 0.03662 -0.00172 0.01020 0.00386 AFIX 137 H4A 2 0.522202 0.299943 0.210246 11.00000 -1.50000 H4B 2 0.552509 0.297307 0.286360 11.00000 -1.50000 H4C 2 0.583234 0.342783 0.237251 11.00000 -1.50000 AFIX 0 C5 1 0.527978 0.563638 0.237945 11.00000 0.01976 0.02050 = 0.03415 0.00247 0.00966 -0.00079 AFIX 137 H5A 2 0.559214 0.550593 0.211050 11.00000 -1.50000 H5B 2 0.549298 0.584583 0.278263 11.00000 -1.50000 H5C 2 0.498160 0.594526 0.213318 11.00000 -1.50000 AFIX 0 C6 1 0.418333 0.304041 0.264426 11.00000 0.01738 0.01660 = 0.02860 -0.00635 0.00719 0.00028 C7 1 0.428457 0.256149 0.314042 11.00000 0.02081 0.01749 = 0.03349 -0.00301 0.01046 0.00206 C8 1 0.398385 0.195956 0.300908 11.00000 0.02923 0.01786 = 0.04608 -0.00278 0.01582 0.00017 AFIX 43 H8 2 0.403993 0.162849 0.333625 11.00000 -1.20000 AFIX 0 C9 1 0.360465 0.183474 0.241050 11.00000 0.02913 0.01973 = 0.05893 -0.01572 0.01369 -0.00547 AFIX 43 H9 2 0.339690 0.142497 0.233445 11.00000 -1.20000 AFIX 0 C10 1 0.352930 0.230572 0.192571 11.00000 0.02639 0.02927 = 0.04420 -0.01740 0.00278 -0.00354 AFIX 43 H10 2 0.327625 0.221139 0.151418 11.00000 -1.20000 AFIX 0 C11 1 0.381593 0.291605 0.202637 11.00000 0.02139 0.02226 = 0.03194 -0.01012 0.00312 0.00206 C12 1 0.470656 0.266391 0.379695 11.00000 0.02813 0.02189 = 0.02934 0.00308 0.00758 0.00318 AFIX 13 H12 2 0.489787 0.310994 0.379906 11.00000 -1.20000 AFIX 0 C13 1 0.524122 0.215798 0.391217 11.00000 0.03749 0.03158 = 0.04370 0.00663 0.00478 0.01163 AFIX 137 H13A 2 0.506465 0.172180 0.395818 11.00000 -1.50000 H13B 2 0.553339 0.226922 0.431334 11.00000 -1.50000 H13C 2 0.546664 0.216025 0.353849 11.00000 -1.50000 AFIX 0 C14 1 0.433035 0.262472 0.436485 11.00000 0.04502 0.03162 = 0.03239 0.00410 0.01412 0.00054 AFIX 137 H14A 2 0.399762 0.295687 0.430322 11.00000 -1.50000 H14B 2 0.461260 0.270312 0.478115 11.00000 -1.50000 H14C 2 0.414114 0.218922 0.437204 11.00000 -1.50000 AFIX 0 C15 1 0.374091 0.341107 0.146662 11.00000 0.02842 0.02957 = 0.02795 -0.00912 -0.00405 0.00508 AFIX 13 H15 2 0.393439 0.383199 0.164681 11.00000 -1.20000 AFIX 0 C16 1 0.408877 0.319130 0.091666 11.00000 0.04132 0.04339 = 0.03797 0.00075 0.00866 0.01139 AFIX 137 H16A 2 0.391036 0.277705 0.073211 11.00000 -1.50000 H16B 2 0.453611 0.313070 0.109397 11.00000 -1.50000 H16C 2 0.404239 0.352553 0.057203 11.00000 -1.50000 AFIX 0 C17 1 0.305094 0.354576 0.119076 11.00000 0.03234 0.05428 = 0.03702 -0.01440 -0.00497 0.01277 AFIX 137 H17A 2 0.302310 0.383438 0.080853 11.00000 -1.50000 H17B 2 0.285029 0.375740 0.152733 11.00000 -1.50000 H17C 2 0.283617 0.313203 0.105922 11.00000 -1.50000 AFIX 0 C18 1 0.402396 0.572988 0.256542 11.00000 0.01514 0.01580 = 0.02610 0.00357 0.00467 0.00041 C19 1 0.410678 0.621259 0.305672 11.00000 0.01865 0.01755 = 0.02900 0.00012 0.00787 -0.00154 C20 1 0.377779 0.679956 0.292794 11.00000 0.02543 0.01753 = 0.03865 0.00007 0.01021 0.00151 AFIX 43 H20 2 0.381580 0.712916 0.325622 11.00000 -1.20000 AFIX 0 C21 1 0.339821 0.690783 0.233069 11.00000 0.02669 0.02019 = 0.04405 0.00572 0.00757 0.00445 AFIX 43 H21 2 0.318289 0.731293 0.224926 11.00000 -1.20000 AFIX 0 C22 1 0.332918 0.643145 0.185060 11.00000 0.02263 0.02668 = 0.03562 0.00863 0.00193 0.00247 AFIX 43 H22 2 0.306904 0.651514 0.144055 11.00000 -1.20000 AFIX 0 C23 1 0.363458 0.582936 0.195679 11.00000 0.01747 0.02229 = 0.02792 0.00416 0.00339 0.00002 C24 1 0.453807 0.612823 0.371246 11.00000 0.02438 0.01983 = 0.02595 -0.00369 0.00692 -0.00082 AFIX 13 H24 2 0.474037 0.568727 0.371932 11.00000 -1.20000 AFIX 0 C25 1 0.505886 0.664837 0.381085 11.00000 0.03033 0.02853 = 0.03597 -0.00753 0.00470 -0.00687 AFIX 137 H25A 2 0.527231 0.665366 0.342844 11.00000 -1.50000 H25B 2 0.536374 0.654454 0.420490 11.00000 -1.50000 H25C 2 0.487318 0.707915 0.386205 11.00000 -1.50000 AFIX 0 C26 1 0.416880 0.616536 0.428659 11.00000 0.03639 0.02862 = 0.02986 -0.00244 0.01255 0.00067 AFIX 137 H26A 2 0.398663 0.660332 0.430251 11.00000 -1.50000 H26B 2 0.445359 0.607767 0.469918 11.00000 -1.50000 H26C 2 0.383107 0.583872 0.422363 11.00000 -1.50000 AFIX 0 C27 1 0.354086 0.530288 0.142825 11.00000 0.02645 0.02745 = 0.02520 0.00223 -0.00252 0.00251 AFIX 13 H27 2 0.354406 0.487093 0.165612 11.00000 -1.20000 AFIX 0 C28 1 0.407383 0.528960 0.102428 11.00000 0.03449 0.05205 = 0.03178 -0.00838 0.00478 0.00164 AFIX 137 H28A 2 0.399231 0.494423 0.069201 11.00000 -1.50000 H28B 2 0.447389 0.520244 0.131417 11.00000 -1.50000 H28C 2 0.409650 0.571363 0.080804 11.00000 -1.50000 AFIX 0 C29 1 0.290940 0.535947 0.096662 11.00000 0.03058 0.04686 = 0.03254 0.00045 -0.00627 0.00149 AFIX 137 H29A 2 0.291198 0.574879 0.069034 11.00000 -1.50000 H29B 2 0.256976 0.539687 0.122526 11.00000 -1.50000 H29C 2 0.284186 0.496900 0.068847 11.00000 -1.50000 AFIX 0 C30 1 0.022048 0.512493 0.312738 11.00000 0.01740 0.02005 = 0.02171 0.00007 0.00276 0.00224 C31 1 -0.009860 0.505375 0.248246 11.00000 0.01373 0.02249 = 0.02220 0.00071 0.00129 0.00002 AFIX 43 H31 2 -0.054411 0.502730 0.243273 11.00000 -1.20000 AFIX 0 C32 1 0.015114 0.501660 0.190414 11.00000 0.01563 0.01856 = 0.02096 -0.00036 0.00011 0.00008 C33 1 -0.018103 0.533365 0.362380 11.00000 0.01907 0.04184 = 0.02210 -0.00473 0.00168 0.00754 AFIX 137 H33A 2 -0.042987 0.571860 0.345940 11.00000 -1.50000 H33B 2 0.009065 0.544239 0.403910 11.00000 -1.50000 H33C 2 -0.046415 0.497527 0.369470 11.00000 -1.50000 AFIX 0 C34 1 -0.030073 0.506084 0.126575 11.00000 0.01790 0.03619 = 0.02103 0.00060 0.00102 0.00178 AFIX 137 H34A 2 -0.022092 0.546440 0.103720 11.00000 -1.50000 H34B 2 -0.073349 0.506430 0.135344 11.00000 -1.50000 H34C 2 -0.024194 0.468262 0.099105 11.00000 -1.50000 AFIX 0 C35 1 0.111665 0.514786 0.398664 11.00000 0.01523 0.02665 = 0.01838 -0.00385 -0.00009 0.00453 C36 1 0.104031 0.468180 0.446633 11.00000 0.01773 0.02856 = 0.02064 -0.00189 0.00143 0.00318 C37 1 0.129301 0.482946 0.512103 11.00000 0.02351 0.03574 = 0.01938 -0.00032 0.00074 0.00340 AFIX 43 H37 2 0.125171 0.452095 0.545475 11.00000 -1.20000 AFIX 0 C38 1 0.160066 0.541441 0.529019 11.00000 0.02670 0.03800 = 0.02099 -0.00704 -0.00150 0.00510 AFIX 43 H38 2 0.175856 0.550978 0.573722 11.00000 -1.20000 AFIX 0 C39 1 0.167804 0.586101 0.480612 11.00000 0.02663 0.02812 = 0.02758 -0.00780 -0.00175 0.00264 AFIX 43 H39 2 0.189443 0.625928 0.492647 11.00000 -1.20000 AFIX 0 C40 1 0.144540 0.573929 0.414570 11.00000 0.02076 0.02364 = 0.02429 -0.00387 -0.00031 0.00544 C41 1 0.068398 0.404092 0.431278 11.00000 0.02191 0.03150 = 0.02120 -0.00087 0.00286 -0.00112 AFIX 13 H41 2 0.050418 0.403728 0.383437 11.00000 -1.20000 AFIX 0 C42 1 0.013816 0.395976 0.469873 11.00000 0.03262 0.04877 = 0.03427 -0.00520 0.01277 -0.00887 AFIX 137 H42A 2 -0.012133 0.435629 0.465182 11.00000 -1.50000 H42B 2 0.030794 0.388792 0.516338 11.00000 -1.50000 H42C 2 -0.011984 0.358335 0.452687 11.00000 -1.50000 AFIX 0 C43 1 0.112101 0.345175 0.445641 11.00000 0.03282 0.03072 = 0.03603 0.00378 -0.00089 -0.00018 AFIX 137 H43A 2 0.088214 0.304861 0.433894 11.00000 -1.50000 H43B 2 0.130022 0.344343 0.492443 11.00000 -1.50000 H43C 2 0.146122 0.348499 0.419807 11.00000 -1.50000 AFIX 0 C44 1 0.152247 0.623962 0.361992 11.00000 0.02916 0.02254 = 0.02700 -0.00430 0.00001 0.00125 AFIX 13 H44 2 0.155763 0.599213 0.321058 11.00000 -1.20000 AFIX 0 C45 1 0.094126 0.667749 0.346782 11.00000 0.03945 0.02507 = 0.04139 0.00101 0.00083 0.00764 AFIX 137 H45A 2 0.100186 0.699707 0.313071 11.00000 -1.50000 H45B 2 0.087830 0.690811 0.386711 11.00000 -1.50000 H45C 2 0.057097 0.640803 0.330813 11.00000 -1.50000 AFIX 0 C46 1 0.211646 0.665804 0.379123 11.00000 0.03866 0.03529 = 0.04001 0.00004 -0.00171 -0.00894 AFIX 137 H46A 2 0.248177 0.637277 0.392068 11.00000 -1.50000 H46B 2 0.207183 0.695204 0.415491 11.00000 -1.50000 H46C 2 0.217609 0.691720 0.340777 11.00000 -1.50000 AFIX 0 C47 1 0.099258 0.510293 0.128564 11.00000 0.01372 0.03026 = 0.01723 0.00221 0.00010 -0.00152 C48 1 0.104843 0.460329 0.083156 11.00000 0.01502 0.03477 = 0.02117 -0.00188 -0.00048 -0.00091 C49 1 0.128023 0.477544 0.026209 11.00000 0.01943 0.04633 = 0.02033 -0.00359 0.00221 -0.00017 AFIX 43 H49 2 0.133569 0.444512 -0.004633 11.00000 -1.20000 AFIX 0 C50 1 0.142962 0.541442 0.013972 11.00000 0.02329 0.05354 = 0.01962 0.00536 0.00275 -0.00646 AFIX 43 H50 2 0.158508 0.551979 -0.025079 11.00000 -1.20000 AFIX 0 C51 1 0.135419 0.590323 0.058315 11.00000 0.02475 0.03877 = 0.02504 0.00738 0.00120 -0.00739 AFIX 43 H51 2 0.144969 0.634341 0.048917 11.00000 -1.20000 AFIX 0 C52 1 0.113853 0.575685 0.116952 11.00000 0.01936 0.03205 = 0.02281 0.00225 -0.00034 -0.00314 C53 1 0.085137 0.390087 0.092697 11.00000 0.02415 0.03175 = 0.02326 -0.00533 0.00355 -0.00005 AFIX 13 H53 2 0.065174 0.388376 0.132933 11.00000 -1.20000 AFIX 0 C54 1 0.036474 0.366278 0.034281 11.00000 0.03677 0.04209 = 0.03106 -0.01128 0.00353 -0.01019 AFIX 137 H54A 2 0.056432 0.362970 -0.004796 11.00000 -1.50000 H54B 2 0.001502 0.397478 0.026038 11.00000 -1.50000 H54C 2 0.020505 0.323228 0.044407 11.00000 -1.50000 AFIX 0 C55 1 0.142024 0.344309 0.103020 11.00000 0.03885 0.04083 = 0.04211 -0.00305 0.00946 0.00952 AFIX 137 H55A 2 0.128177 0.299642 0.110369 11.00000 -1.50000 H55B 2 0.172077 0.358804 0.141273 11.00000 -1.50000 H55C 2 0.162294 0.345128 0.064036 11.00000 -1.50000 AFIX 0 C56 1 0.105700 0.630807 0.164541 11.00000 0.02853 0.02906 = 0.02684 0.00256 0.00244 -0.00650 AFIX 13 H56 2 0.095473 0.610492 0.205453 11.00000 -1.20000 AFIX 0 C57 1 0.051074 0.675808 0.136442 11.00000 0.04480 0.04459 = 0.05441 -0.01215 -0.00662 0.00928 AFIX 137 H57A 2 0.060144 0.696811 0.096474 11.00000 -1.50000 H57B 2 0.045730 0.709426 0.168847 11.00000 -1.50000 H57C 2 0.012342 0.650026 0.125998 11.00000 -1.50000 AFIX 0 C58 1 0.165636 0.670765 0.183325 11.00000 0.03711 0.03591 = 0.04165 -0.00074 0.00369 -0.01335 AFIX 137 H58A 2 0.176473 0.691692 0.144079 11.00000 -1.50000 H58B 2 0.200066 0.641888 0.202806 11.00000 -1.50000 H58C 2 0.158952 0.704440 0.215182 11.00000 -1.50000 AFIX 0 C59 1 0.278510 0.383142 0.365931 11.00000 0.01621 0.02326 = 0.02536 0.00169 0.00244 -0.00112 C60 1 0.274319 0.362456 0.471387 11.00000 0.02227 0.03434 = 0.02529 0.01183 0.00428 0.00308 C61 1 0.266590 0.305218 0.438235 11.00000 0.02301 0.03222 = 0.03481 0.01286 0.00445 0.00432 C62 1 0.289245 0.479491 0.442484 11.00000 0.02703 0.02885 = 0.02596 -0.00215 0.00406 0.00183 AFIX 137 H62A 2 0.296595 0.503927 0.403714 11.00000 -1.50000 H62B 2 0.325468 0.484810 0.477713 11.00000 -1.50000 H62C 2 0.251320 0.496230 0.457108 11.00000 -1.50000 AFIX 0 C63 1 0.261117 0.269299 0.321707 11.00000 0.02939 0.02376 = 0.04494 -0.00342 0.00657 -0.00227 AFIX 137 H63A 2 0.273033 0.287764 0.281825 11.00000 -1.50000 H63B 2 0.216973 0.255468 0.312605 11.00000 -1.50000 H63C 2 0.287868 0.231454 0.336010 11.00000 -1.50000 AFIX 0 C64 1 0.275016 0.377993 0.542241 11.00000 0.04127 0.05473 = 0.02620 0.01061 0.00757 0.00228 AFIX 137 H64A 2 0.246958 0.415075 0.545809 11.00000 -1.50000 H64B 2 0.317930 0.389305 0.563083 11.00000 -1.50000 H64C 2 0.260617 0.339769 0.564211 11.00000 -1.50000 AFIX 0 C65 1 0.253625 0.238257 0.461375 11.00000 0.04774 0.03801 = 0.05442 0.02083 0.00800 -0.00159 AFIX 137 H65A 2 0.213631 0.222352 0.436730 11.00000 -1.50000 H65B 2 0.251075 0.239760 0.508210 11.00000 -1.50000 H65C 2 0.287650 0.208657 0.454392 11.00000 -1.50000 AFIX 0 RESI 1 F12 5 0.691994 0.331466 0.174518 11.00000 0.02414 0.02329 = 0.02586 0.00187 0.00041 -0.00262 F13 5 0.585616 0.319718 0.088603 11.00000 0.03045 0.03938 = 0.03218 -0.00304 -0.00318 -0.01336 F14 5 0.523321 0.427939 0.035151 11.00000 0.02524 0.06285 = 0.03369 0.00364 -0.01436 -0.00363 F15 5 0.572083 0.549113 0.069348 11.00000 0.03179 0.04490 = 0.03666 0.00952 -0.00813 0.01446 F16 5 0.677631 0.562239 0.152729 11.00000 0.02702 0.02384 = 0.02985 0.00131 -0.00052 0.00669 F22 5 0.774392 0.380942 0.093855 11.00000 0.02379 0.03176 = 0.01879 -0.00044 0.00277 0.00207 F23 5 0.876984 0.317894 0.075149 11.00000 0.03367 0.03232 = 0.02736 -0.00361 0.01301 0.00423 F24 5 0.976449 0.303127 0.174497 11.00000 0.01967 0.02865 = 0.04947 -0.00502 0.01051 0.00483 F25 5 0.968041 0.351083 0.296500 11.00000 0.01944 0.03275 = 0.03928 -0.00123 -0.00567 0.00443 F26 5 0.867649 0.418774 0.315615 11.00000 0.02173 0.02923 = 0.02226 -0.00375 -0.00241 0.00261 F32 5 0.797337 0.539604 0.344525 11.00000 0.03142 0.02883 = 0.02229 -0.00386 -0.00142 -0.00004 F33 5 0.858973 0.650041 0.344387 11.00000 0.04052 0.02798 = 0.04913 -0.01454 -0.00572 -0.00321 F34 5 0.893440 0.696972 0.231386 11.00000 0.04406 0.01995 = 0.07914 0.00200 0.00892 -0.00965 F35 5 0.858715 0.630079 0.116893 11.00000 0.04291 0.03019 = 0.05333 0.01621 0.02026 0.00097 F36 5 0.793736 0.519408 0.115042 11.00000 0.03054 0.02940 = 0.02408 0.00378 0.00824 0.00144 F42 5 0.674283 0.525554 0.290606 11.00000 0.02466 0.02493 = 0.02846 0.00073 0.00322 0.00834 F43 5 0.623961 0.493267 0.395247 11.00000 0.03377 0.04492 = 0.03162 -0.00986 0.01366 0.00624 F44 5 0.649197 0.374002 0.453840 11.00000 0.06216 0.05602 = 0.03060 0.00553 0.02849 -0.00112 F45 5 0.725844 0.288863 0.403947 11.00000 0.05451 0.03036 = 0.03125 0.01209 0.01157 0.00048 F46 5 0.776115 0.319480 0.300367 11.00000 0.02779 0.01909 = 0.02707 0.00241 0.00543 0.00326 C11 1 0.692552 0.446929 0.167097 11.00000 0.01794 0.02562 = 0.01606 0.00066 0.00352 0.00115 C12 1 0.664517 0.387116 0.148487 11.00000 0.01887 0.02676 = 0.01889 0.00247 0.00324 0.00043 C13 1 0.609047 0.379529 0.104508 11.00000 0.02185 0.03440 = 0.02199 0.00015 0.00253 -0.00594 C14 1 0.577564 0.434200 0.077327 11.00000 0.02038 0.04617 = 0.02077 0.00218 -0.00442 -0.00095 C15 1 0.602336 0.494879 0.094699 11.00000 0.02225 0.03687 = 0.02252 0.00496 -0.00027 0.00851 C16 1 0.658301 0.500124 0.138424 11.00000 0.02197 0.02739 = 0.01963 0.00037 0.00371 0.00291 C21 1 0.814470 0.402814 0.206614 11.00000 0.01698 0.01771 = 0.02060 0.00185 0.00279 -0.00021 C22 1 0.820919 0.375656 0.146331 11.00000 0.01932 0.02074 = 0.02162 0.00170 0.00383 -0.00116 C23 1 0.874103 0.342534 0.135073 11.00000 0.02619 0.02078 = 0.02470 -0.00177 0.00921 -0.00117 C24 1 0.924528 0.334540 0.185071 11.00000 0.01802 0.01824 = 0.03861 -0.00068 0.00889 0.00146 C25 1 0.920489 0.359375 0.246220 11.00000 0.01791 0.02009 = 0.03115 0.00129 -0.00163 -0.00074 C26 1 0.867025 0.393233 0.254854 11.00000 0.02033 0.01804 = 0.02335 -0.00088 0.00242 -0.00056 C31 1 0.790513 0.522630 0.229250 11.00000 0.01631 0.01824 = 0.02566 0.00188 0.00127 0.00296 C32 1 0.809502 0.559463 0.285607 11.00000 0.02090 0.02086 = 0.02790 0.00097 0.00120 0.00305 C33 1 0.842636 0.617828 0.287022 11.00000 0.02539 0.02205 = 0.03938 -0.00545 -0.00279 0.00236 C34 1 0.859801 0.641730 0.230541 11.00000 0.02449 0.01694 = 0.05565 0.00386 0.00365 -0.00113 C35 1 0.842543 0.607469 0.173142 11.00000 0.02603 0.02268 = 0.04126 0.01024 0.01030 0.00433 C36 1 0.809038 0.550073 0.173571 11.00000 0.02056 0.02144 = 0.02928 0.00265 0.00410 0.00447 C41 1 0.730131 0.425948 0.290483 11.00000 0.01699 0.02174 = 0.01744 -0.00132 0.00038 -0.00081 C42 1 0.689563 0.466152 0.317950 11.00000 0.02006 0.02445 = 0.01924 0.00003 0.00009 0.00261 C43 1 0.662249 0.450580 0.371778 11.00000 0.02345 0.03605 = 0.02312 -0.00775 0.00550 0.00147 C44 1 0.674566 0.390575 0.401321 11.00000 0.03320 0.04071 = 0.02026 0.00232 0.00955 -0.00365 C45 1 0.713287 0.347798 0.375852 11.00000 0.03166 0.02696 = 0.02188 0.00342 0.00329 -0.00285 C46 1 0.739787 0.365687 0.321701 11.00000 0.02105 0.02258 = 0.01978 -0.00045 0.00197 -0.00023 B1 3 0.756684 0.449440 0.223505 11.00000 0.01778 0.01936 = 0.01715 0.00137 0.00266 0.00213 RESI 0 HKLF 4 REM mks_056m in P2(1)/c REM R1 = 0.0281 for 16685 Fo > 4sig(Fo) and 0.0369 for all 19684 data REM 1178 parameters refined using 39 restraints END WGHT 0.0307 6.3510 REM Highest difference peak 0.430, deepest hole -0.708, 1-sigma level 0.054 Q1 1 0.2578 0.3512 0.3598 11.00000 0.05 0.43 Q2 1 0.2575 0.4100 0.3797 11.00000 0.05 0.43 Q3 1 0.1508 0.4026 0.2757 11.00000 0.05 0.40 Q4 1 0.2543 0.3104 0.2963 11.00000 0.05 0.35 Q5 1 0.7434 0.4346 0.2604 11.00000 0.05 0.35 Q6 1 0.4335 0.6124 0.3384 11.00000 0.05 0.35 Q7 1 0.4186 0.3904 0.2814 11.00000 0.05 0.34 Q8 1 0.1321 0.4094 0.2523 11.00000 0.05 0.34 Q9 1 0.3761 0.5370 0.1208 11.00000 0.05 0.32 Q10 1 0.2720 0.4830 0.4761 11.00000 0.05 0.32 Q11 1 0.1010 0.4952 0.3102 11.00000 0.05 0.31 Q12 1 0.7833 0.4221 0.2134 11.00000 0.05 0.31 Q13 1 0.9160 0.3349 0.2184 11.00000 0.05 0.31 Q14 1 0.4220 0.4863 0.2777 11.00000 0.05 0.30 Q15 1 0.2381 0.5178 0.3037 11.00000 0.05 0.30 Q16 1 0.6392 0.3821 0.1226 11.00000 0.05 0.29 Q17 1 0.3903 0.3263 0.1203 11.00000 0.05 0.29 Q18 1 -0.0606 0.5336 0.3487 11.00000 0.05 0.29 Q19 1 0.0966 0.4791 0.2211 11.00000 0.05 0.29 Q20 1 0.7733 0.4921 0.2293 11.00000 0.05 0.29 ; _shelx_res_checksum 45675