# Electronic Supplementary Material (ESI) for RSC Advances. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # 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_Au_MF _database_code_depnum_ccdc_archive 'CCDC 2091847' loop_ _audit_author_name _audit_author_address 'Simon J. Teat' ;Lawrence Berkeley National Laboratory United States of America ; _audit_update_record ; 2021-06-24 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _audit_creation_date 2020-12-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic 'Gold 3-formyl-5,10,15-tris(p-fluorophenyl)corrole' _chemical_formula_moiety 'C38 H20 Au F3 N4 O' _chemical_formula_sum 'C38 H20 Au F3 N4 O' _chemical_formula_weight 802.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0037 0.0017 'Olex2 (Dolomanov et al., 2009)' H H 0.0000 0.0000 'Olex2 (Dolomanov et al., 2009)' Au Au -2.1181 9.2243 'Olex2 (Dolomanov et al., 2009)' F F 0.0189 0.0109 'Olex2 (Dolomanov et al., 2009)' N N 0.0070 0.0034 'Olex2 (Dolomanov et al., 2009)' O O 0.0123 0.0065 'Olex2 (Dolomanov et al., 2009)' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.9037(12) _cell_length_b 19.7169(12) _cell_length_c 15.8376(10) _cell_angle_alpha 90 _cell_angle_beta 91.467(3) _cell_angle_gamma 90 _cell_volume 6525.4(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9801 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.44 _cell_measurement_theta_min 2.49 _shelx_estimated_absorpt_T_max 0.953 _shelx_estimated_absorpt_T_min 0.643 _exptl_absorpt_coefficient_mu 4.852 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.5333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 - Bruker AXS, Madison WI' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 3120 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 84580 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.930 _diffrn_reflns_theta_max 31.600 _diffrn_reflns_theta_min 2.913 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 with PHOTON II detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7288 _diffrn_source 'Advanced Light Source, beamline 12.2.1' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8633 _reflns_number_total 10078 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40A (Bruker, 2016)' _computing_data_collection 'Bruker APEX3 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.40A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.925 _refine_diff_density_min -1.512 _refine_diff_density_rms 0.154 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 10078 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0377 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+49.3848P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.1001 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Au1 Au 0.50310(2) 0.54114(2) 0.62518(2) 0.02490(5) Uani 1 1 d . . . . . F1 F 0.26176(19) 0.1787(2) 0.7418(3) 0.0725(11) Uani 1 1 d . . . . . F2 F 0.84528(16) 0.30410(18) 0.4754(3) 0.0612(9) Uani 1 1 d . . . . . F3 F 0.6742(2) 0.95356(16) 0.5510(3) 0.0737(13) Uani 1 1 d . . . . . O1 O 0.4162(2) 0.8558(2) 0.6482(3) 0.0699(13) Uani 1 1 d . . . . . N1 N 0.41927(15) 0.52417(17) 0.6704(2) 0.0274(6) Uani 1 1 d . . . . . N2 N 0.52098(17) 0.44344(16) 0.6128(2) 0.0276(6) Uani 1 1 d . . . . . N3 N 0.58430(15) 0.57038(17) 0.5781(2) 0.0255(6) Uani 1 1 d . . . . . N4 N 0.47692(16) 0.63453(18) 0.6456(2) 0.0303(7) Uani 1 1 d . . . . . C1 C 0.3863(2) 0.5802(2) 0.6962(3) 0.0321(8) Uani 1 1 d . . . . . C2 C 0.3309(2) 0.5547(2) 0.7352(3) 0.0354(9) Uani 1 1 d . . . . . H2 H 0.2983 0.5811 0.7599 0.043 Uiso 1 1 calc R . . . . C3 C 0.33264(19) 0.4851(2) 0.7310(3) 0.0323(8) Uani 1 1 d . . . . . H3 H 0.3014 0.4552 0.7526 0.039 Uiso 1 1 calc R . . . . C4 C 0.3891(2) 0.4653(2) 0.6890(3) 0.0295(8) Uani 1 1 d . . . . . C5 C 0.41503(19) 0.4024(2) 0.6662(2) 0.0295(8) Uani 1 1 d . . . . . C6 C 0.47499(19) 0.3941(2) 0.6281(2) 0.0278(7) Uani 1 1 d . . . . . C7 C 0.50301(19) 0.3327(2) 0.5973(3) 0.0290(8) Uani 1 1 d . . . . . H7 H 0.4833 0.2893 0.5976 0.035 Uiso 1 1 calc R . . . . C8 C 0.56191(19) 0.3463(2) 0.5680(3) 0.0306(8) Uani 1 1 d . . . . . H8 H 0.5907 0.3146 0.5446 0.037 Uiso 1 1 calc R . . . . C9 C 0.57266(18) 0.4179(2) 0.5788(2) 0.0264(7) Uani 1 1 d . . . . . C10 C 0.62795(19) 0.4550(2) 0.5590(2) 0.0265(7) Uani 1 1 d . . . . . C11 C 0.63260(18) 0.5262(2) 0.5612(2) 0.0260(7) Uani 1 1 d . . . . . C12 C 0.68797(19) 0.5682(2) 0.5483(3) 0.0300(8) Uani 1 1 d . . . . . H12 H 0.7295 0.5524 0.5354 0.036 Uiso 1 1 calc R . . . . C13 C 0.67096(19) 0.6339(2) 0.5577(3) 0.0308(8) Uani 1 1 d . . . . . H13 H 0.6985 0.6719 0.5524 0.037 Uiso 1 1 calc R . . . . C14 C 0.60450(19) 0.6365(2) 0.5770(3) 0.0283(7) Uani 1 1 d . . . . . C15 C 0.56758(19) 0.6952(2) 0.5932(3) 0.0292(8) Uani 1 1 d . . . . . C16 C 0.5043(2) 0.6949(2) 0.6222(3) 0.0336(9) Uani 1 1 d . . . . . C17 C 0.4562(2) 0.7442(2) 0.6390(3) 0.0365(9) Uani 1 1 d . . . . . C18 C 0.4035(2) 0.7112(2) 0.6730(3) 0.0377(9) Uani 1 1 d . . . . . H18 H 0.3653 0.7323 0.6907 0.045 Uiso 1 1 calc R . . . . C19 C 0.41671(19) 0.6417(2) 0.6763(3) 0.0312(8) Uani 1 1 d . . . . . C20 C 0.37575(19) 0.3413(2) 0.6836(3) 0.0313(8) Uani 1 1 d . . . . . C21 C 0.3117(2) 0.3395(2) 0.6573(3) 0.0347(9) Uani 1 1 d . . . . . H21 H 0.2941 0.3764 0.6260 0.042 Uiso 1 1 calc R . . . . C22 C 0.2731(2) 0.2839(3) 0.6765(3) 0.0419(10) Uani 1 1 d . . . . . H22 H 0.2294 0.2824 0.6586 0.050 Uiso 1 1 calc R . . . . C23 C 0.3001(3) 0.2320(3) 0.7217(3) 0.0450(11) Uani 1 1 d . . . . . C24 C 0.3626(3) 0.2307(3) 0.7486(3) 0.0441(11) Uani 1 1 d . . . . . H24 H 0.3796 0.1934 0.7797 0.053 Uiso 1 1 calc R . . . . C25 C 0.4003(2) 0.2858(2) 0.7289(3) 0.0376(9) Uani 1 1 d . . . . . H25 H 0.4440 0.2860 0.7466 0.045 Uiso 1 1 calc R . . . . C26 C 0.68605(19) 0.4152(2) 0.5367(3) 0.0286(7) Uani 1 1 d . . . . . C27 C 0.7077(2) 0.3626(2) 0.5887(3) 0.0354(9) Uani 1 1 d . . . . . H27 H 0.6857 0.3525 0.6389 0.042 Uiso 1 1 calc R . . . . C28 C 0.7611(2) 0.3247(3) 0.5683(4) 0.0442(11) Uani 1 1 d . . . . . H28 H 0.7754 0.2884 0.6034 0.053 Uiso 1 1 calc R . . . . C29 C 0.7927(2) 0.3412(3) 0.4961(4) 0.0444(11) Uani 1 1 d . . . . . C30 C 0.7736(2) 0.3931(3) 0.4425(3) 0.0403(10) Uani 1 1 d . . . . . H30 H 0.7965 0.4033 0.3930 0.048 Uiso 1 1 calc R . . . . C31 C 0.7195(2) 0.4299(2) 0.4640(3) 0.0335(8) Uani 1 1 d . . . . . H31 H 0.7051 0.4657 0.4282 0.040 Uiso 1 1 calc R . . . . C32 C 0.5977(2) 0.7626(2) 0.5813(3) 0.0322(8) Uani 1 1 d . . . . . C33 C 0.5976(2) 0.8105(2) 0.6472(3) 0.0384(9) Uani 1 1 d . . . . . H33 H 0.5794 0.7987 0.6995 0.046 Uiso 1 1 calc R . . . . C34 C 0.6237(3) 0.8755(3) 0.6368(4) 0.0486(12) Uani 1 1 d . . . . . H34 H 0.6233 0.9079 0.6812 0.058 Uiso 1 1 calc R . . . . C35 C 0.6496(3) 0.8905(3) 0.5616(4) 0.0506(13) Uani 1 1 d . . . . . C36 C 0.6514(2) 0.8460(3) 0.4947(4) 0.0443(11) Uani 1 1 d . . . . . H36 H 0.6699 0.8587 0.4428 0.053 Uiso 1 1 calc R . . . . C37 C 0.6253(2) 0.7816(2) 0.5057(3) 0.0372(9) Uani 1 1 d . . . . . H37 H 0.6264 0.7499 0.4606 0.045 Uiso 1 1 calc R . . . . C38 C 0.4550(3) 0.8154(3) 0.6177(4) 0.0501(12) Uani 1 1 d . . . . . H38 H 0.4852 0.8321 0.5789 0.060 Uiso 1 1 calc R . . . . 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 Au1 0.02447(8) 0.02466(8) 0.02542(8) -0.00104(5) -0.00233(5) -0.00111(5) F1 0.072(2) 0.060(2) 0.085(3) 0.0210(19) -0.009(2) -0.0382(19) F2 0.0445(17) 0.0508(19) 0.089(3) -0.0106(18) 0.0106(17) 0.0174(14) F3 0.073(2) 0.0352(17) 0.115(3) -0.0137(18) 0.043(2) -0.0199(16) O1 0.075(3) 0.041(2) 0.094(4) 0.000(2) 0.014(3) 0.016(2) N1 0.0208(14) 0.0284(16) 0.0333(17) -0.0013(13) 0.0054(12) -0.0033(11) N2 0.0289(15) 0.0178(14) 0.0360(17) -0.0056(12) -0.0003(13) 0.0011(11) N3 0.0203(13) 0.0280(16) 0.0282(15) -0.0007(12) 0.0010(11) -0.0025(11) N4 0.0247(15) 0.0322(18) 0.0341(17) -0.0058(14) 0.0011(13) 0.0040(12) C1 0.0285(18) 0.036(2) 0.0313(19) -0.0045(16) -0.0028(15) 0.0004(15) C2 0.0299(19) 0.046(2) 0.030(2) -0.0054(18) 0.0017(15) 0.0043(17) C3 0.0276(18) 0.040(2) 0.0293(19) 0.0003(17) 0.0016(15) -0.0028(16) C4 0.0277(18) 0.036(2) 0.0246(17) -0.0007(15) -0.0009(14) -0.0021(15) C5 0.0314(18) 0.032(2) 0.0244(17) 0.0005(15) -0.0037(14) -0.0048(15) C6 0.0308(18) 0.0256(17) 0.0266(17) -0.0011(14) -0.0066(14) 0.0050(14) C7 0.0306(18) 0.0242(18) 0.0321(19) 0.0048(15) -0.0020(14) -0.0040(14) C8 0.0266(17) 0.034(2) 0.0313(19) -0.0032(16) -0.0003(14) 0.0041(15) C9 0.0268(17) 0.0280(18) 0.0241(16) 0.0003(14) -0.0020(13) -0.0020(14) C10 0.0264(17) 0.0263(18) 0.0265(17) -0.0020(14) -0.0024(13) 0.0000(13) C11 0.0249(16) 0.0284(18) 0.0246(17) -0.0005(13) -0.0027(13) -0.0003(13) C12 0.0263(17) 0.0293(19) 0.034(2) -0.0005(15) -0.0003(14) -0.0021(14) C13 0.0291(18) 0.030(2) 0.0328(19) -0.0004(15) -0.0012(15) -0.0050(14) C14 0.0295(18) 0.0272(18) 0.0280(18) 0.0006(14) -0.0022(14) -0.0035(14) C15 0.0288(18) 0.0272(18) 0.0315(19) 0.0006(15) -0.0038(14) -0.0020(14) C16 0.036(2) 0.0241(18) 0.040(2) -0.0040(16) -0.0066(17) -0.0029(15) C17 0.036(2) 0.032(2) 0.042(2) -0.0048(18) -0.0018(17) 0.0041(16) C18 0.0289(19) 0.039(2) 0.045(2) -0.0057(19) 0.0003(17) 0.0043(17) C19 0.0277(18) 0.034(2) 0.0317(19) -0.0032(16) 0.0000(15) 0.0031(15) C20 0.0290(18) 0.037(2) 0.0284(19) -0.0005(16) 0.0002(14) -0.0057(15) C21 0.0298(19) 0.040(2) 0.034(2) 0.0014(17) -0.0004(16) -0.0062(16) C22 0.036(2) 0.045(3) 0.044(2) 0.000(2) -0.0029(18) -0.0144(19) C23 0.049(3) 0.040(3) 0.046(3) 0.004(2) -0.001(2) -0.017(2) C24 0.055(3) 0.034(2) 0.042(3) 0.0092(19) -0.002(2) -0.008(2) C25 0.037(2) 0.041(2) 0.034(2) 0.0028(18) -0.0043(17) -0.0060(18) C26 0.0279(17) 0.0273(18) 0.0305(18) -0.0029(15) -0.0032(14) 0.0004(14) C27 0.033(2) 0.032(2) 0.040(2) 0.0024(17) -0.0001(17) 0.0021(16) C28 0.038(2) 0.034(2) 0.060(3) 0.005(2) -0.002(2) 0.0073(18) C29 0.036(2) 0.040(3) 0.058(3) -0.011(2) 0.004(2) 0.0087(19) C30 0.038(2) 0.039(2) 0.044(3) -0.0089(19) 0.0090(19) -0.0009(18) C31 0.036(2) 0.033(2) 0.032(2) -0.0021(16) 0.0006(16) -0.0015(16) C32 0.0297(19) 0.0270(19) 0.040(2) -0.0005(16) -0.0016(16) 0.0011(15) C33 0.040(2) 0.030(2) 0.045(2) -0.0071(18) 0.0011(19) -0.0028(17) C34 0.046(3) 0.036(2) 0.064(3) -0.015(2) 0.010(2) -0.006(2) C35 0.041(3) 0.028(2) 0.084(4) -0.003(2) 0.015(3) -0.0071(18) C36 0.042(2) 0.033(2) 0.058(3) -0.002(2) 0.010(2) -0.0072(19) C37 0.037(2) 0.031(2) 0.043(2) -0.0026(18) 0.0028(18) -0.0044(17) C38 0.044(3) 0.041(3) 0.066(4) 0.006(2) 0.001(2) 0.004(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 Au1 N1 1.939(3) . ? Au1 N2 1.973(3) . ? Au1 N3 1.958(3) . ? Au1 N4 1.950(4) . ? F1 C23 1.366(6) . ? F2 C29 1.366(5) . ? F3 C35 1.358(6) . ? O1 C38 1.244(7) . ? N1 C1 1.369(5) . ? N1 C4 1.358(5) . ? N2 C6 1.393(5) . ? N2 C9 1.320(5) . ? N3 C11 1.365(5) . ? N3 C14 1.371(5) . ? N4 C16 1.376(6) . ? N4 C19 1.368(5) . ? C1 C2 1.418(6) . ? C1 C19 1.409(6) . ? C2 H2 0.9500 . ? C2 C3 1.374(7) . ? C3 H3 0.9500 . ? C3 C4 1.424(6) . ? C4 C5 1.404(6) . ? C5 C6 1.414(6) . ? C5 C20 1.489(6) . ? C6 C7 1.435(6) . ? C7 H7 0.9500 . ? C7 C8 1.354(6) . ? C8 H8 0.9500 . ? C8 C9 1.438(6) . ? C9 C10 1.410(5) . ? C10 C11 1.409(5) . ? C10 C26 1.496(6) . ? C11 C12 1.441(5) . ? C12 H12 0.9500 . ? C12 C13 1.351(6) . ? C13 H13 0.9500 . ? C13 C14 1.431(6) . ? C14 C15 1.417(6) . ? C15 C16 1.410(6) . ? C15 C32 1.486(6) . ? C16 C17 1.429(6) . ? C17 C18 1.399(7) . ? C17 C38 1.444(7) . ? C18 H18 0.9500 . ? C18 C19 1.398(6) . ? C20 C21 1.392(6) . ? C20 C25 1.398(6) . ? C21 H21 0.9500 . ? C21 C22 1.398(6) . ? C22 H22 0.9500 . ? C22 C23 1.363(7) . ? C23 C24 1.364(7) . ? C24 H24 0.9500 . ? C24 C25 1.381(7) . ? C25 H25 0.9500 . ? C26 C27 1.392(6) . ? C26 C31 1.393(6) . ? C27 H27 0.9500 . ? C27 C28 1.388(6) . ? C28 H28 0.9500 . ? C28 C29 1.375(8) . ? C29 C30 1.383(7) . ? C30 H30 0.9500 . ? C30 C31 1.394(6) . ? C31 H31 0.9500 . ? C32 C33 1.407(6) . ? C32 C37 1.394(6) . ? C33 H33 0.9500 . ? C33 C34 1.404(7) . ? C34 H34 0.9500 . ? C34 C35 1.354(8) . ? C35 C36 1.377(8) . ? C36 H36 0.9500 . ? C36 C37 1.395(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? 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 Au1 N2 92.48(15) . . ? N1 Au1 N3 172.67(14) . . ? N1 Au1 N4 80.88(15) . . ? N3 Au1 N2 94.67(14) . . ? N4 Au1 N2 173.17(14) . . ? N4 Au1 N3 92.01(14) . . ? C1 N1 Au1 115.9(3) . . ? C4 N1 Au1 131.1(3) . . ? C4 N1 C1 112.6(3) . . ? C6 N2 Au1 122.1(3) . . ? C9 N2 Au1 124.9(3) . . ? C9 N2 C6 112.3(3) . . ? C11 N3 Au1 122.7(3) . . ? C11 N3 C14 112.0(3) . . ? C14 N3 Au1 123.7(3) . . ? C16 N4 Au1 130.6(3) . . ? C19 N4 Au1 114.9(3) . . ? C19 N4 C16 113.6(4) . . ? N1 C1 C2 105.5(4) . . ? N1 C1 C19 113.2(4) . . ? C19 C1 C2 141.3(4) . . ? C1 C2 H2 126.0 . . ? C3 C2 C1 108.1(4) . . ? C3 C2 H2 126.0 . . ? C2 C3 H3 125.7 . . ? C2 C3 C4 108.6(4) . . ? C4 C3 H3 125.7 . . ? N1 C4 C3 105.2(4) . . ? N1 C4 C5 120.9(4) . . ? C5 C4 C3 133.9(4) . . ? C4 C5 C6 124.4(4) . . ? C4 C5 C20 116.6(4) . . ? C6 C5 C20 119.0(4) . . ? N2 C6 C5 128.0(4) . . ? N2 C6 C7 103.9(3) . . ? C5 C6 C7 128.1(4) . . ? C6 C7 H7 125.3 . . ? C8 C7 C6 109.4(4) . . ? C8 C7 H7 125.3 . . ? C7 C8 H8 126.5 . . ? C7 C8 C9 107.1(4) . . ? C9 C8 H8 126.5 . . ? N2 C9 C8 107.2(3) . . ? N2 C9 C10 125.2(4) . . ? C10 C9 C8 127.5(4) . . ? C9 C10 C26 117.1(3) . . ? C11 C10 C9 124.6(4) . . ? C11 C10 C26 118.3(4) . . ? N3 C11 C10 126.2(4) . . ? N3 C11 C12 105.2(3) . . ? C10 C11 C12 128.6(4) . . ? C11 C12 H12 125.7 . . ? C13 C12 C11 108.7(4) . . ? C13 C12 H12 125.7 . . ? C12 C13 H13 125.7 . . ? C12 C13 C14 108.6(4) . . ? C14 C13 H13 125.7 . . ? N3 C14 C13 105.6(3) . . ? N3 C14 C15 127.2(4) . . ? C15 C14 C13 127.2(4) . . ? C14 C15 C32 118.2(4) . . ? C16 C15 C14 125.1(4) . . ? C16 C15 C32 116.7(4) . . ? N4 C16 C15 119.4(4) . . ? N4 C16 C17 103.8(4) . . ? C15 C16 C17 136.7(4) . . ? C16 C17 C38 128.7(5) . . ? C18 C17 C16 108.7(4) . . ? C18 C17 C38 122.3(4) . . ? C17 C18 H18 125.9 . . ? C19 C18 C17 108.3(4) . . ? C19 C18 H18 125.9 . . ? N4 C19 C1 114.5(4) . . ? N4 C19 C18 105.7(4) . . ? C18 C19 C1 139.7(4) . . ? C21 C20 C5 119.7(4) . . ? C21 C20 C25 118.1(4) . . ? C25 C20 C5 122.2(4) . . ? C20 C21 H21 119.6 . . ? C20 C21 C22 120.7(4) . . ? C22 C21 H21 119.6 . . ? C21 C22 H22 121.0 . . ? C23 C22 C21 118.0(4) . . ? C23 C22 H22 121.0 . . ? C22 C23 F1 117.6(5) . . ? C22 C23 C24 124.0(5) . . ? C24 C23 F1 118.5(5) . . ? C23 C24 H24 121.3 . . ? C23 C24 C25 117.4(5) . . ? C25 C24 H24 121.3 . . ? C20 C25 H25 119.1 . . ? C24 C25 C20 121.9(4) . . ? C24 C25 H25 119.1 . . ? C27 C26 C10 120.3(4) . . ? C27 C26 C31 118.8(4) . . ? C31 C26 C10 120.9(4) . . ? C26 C27 H27 119.5 . . ? C28 C27 C26 121.0(4) . . ? C28 C27 H27 119.5 . . ? C27 C28 H28 120.9 . . ? C29 C28 C27 118.2(5) . . ? C29 C28 H28 120.9 . . ? F2 C29 C28 118.7(5) . . ? F2 C29 C30 118.1(5) . . ? C28 C29 C30 123.3(4) . . ? C29 C30 H30 121.4 . . ? C29 C30 C31 117.3(4) . . ? C31 C30 H30 121.4 . . ? C26 C31 C30 121.4(4) . . ? C26 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C15 119.8(4) . . ? C37 C32 C15 122.4(4) . . ? C37 C32 C33 117.8(4) . . ? C32 C33 H33 119.4 . . ? C34 C33 C32 121.2(5) . . ? C34 C33 H33 119.4 . . ? C33 C34 H34 121.1 . . ? C35 C34 C33 117.9(5) . . ? C35 C34 H34 121.1 . . ? F3 C35 C36 118.1(5) . . ? C34 C35 F3 118.0(5) . . ? C34 C35 C36 123.9(5) . . ? C35 C36 H36 121.1 . . ? C35 C36 C37 117.7(5) . . ? C37 C36 H36 121.1 . . ? C32 C37 C36 121.6(5) . . ? C32 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? O1 C38 C17 122.6(5) . . ? O1 C38 H38 118.7 . . ? C17 C38 H38 118.7 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.500 -0.682 701.4 560.9 ? 2 0.500 0.000 -0.382 701.4 560.9 ? _shelx_res_file ; au_mf_10.res created by SHELXL-2014/7 TITL au_mf_10_a.res in C2/c REM Old TITL au_mf_10_a.res in C2/c REM SHELXT solution in C2/c REM R1 0.091, Rweak 0.003, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C36 Au N5 O6 CELL 0.7288 20.9037 19.7169 15.8376 90 91.467 90 ZERR 8 0.0012 0.0012 0.001 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Au F N O DISP Au -2.1181 9.2243 38823.3346 DISP C 0.0037 0.0017 12.0457 DISP F 0.0189 0.0109 54.6907 DISP H -0 0 0.6249 DISP N 0.007 0.0034 20.6663 DISP O 0.0123 0.0065 34.424 UNIT 304 160 8 24 32 8 L.S. 10 PLAN 10 SIZE 0.01 0.02 0.1 TEMP -173(2) BOND $H list 4 ABIN fmap 2 ACTA OMIT 1 1 0 OMIT 2 2 2 OMIT 0 0 2 OMIT 0 2 1 OMIT 1 3 1 OMIT 1 3 0 OMIT 2 0 2 OMIT -1 1 1 OMIT 0 4 0 OMIT 2 2 1 REM REM REM WGHT 0.036400 49.384804 FVAR 0.05360 AU1 3 0.503103 0.541142 0.625180 11.00000 0.02447 0.02466 = 0.02542 -0.00104 -0.00233 -0.00111 F1 4 0.261759 0.178681 0.741829 11.00000 0.07206 0.06019 = 0.08480 0.02099 -0.00914 -0.03824 F2 4 0.845282 0.304098 0.475430 11.00000 0.04448 0.05079 = 0.08889 -0.01063 0.01057 0.01742 F3 4 0.674172 0.953560 0.551024 11.00000 0.07338 0.03524 = 0.11463 -0.01370 0.04331 -0.01990 O1 6 0.416167 0.855798 0.648183 11.00000 0.07493 0.04114 = 0.09415 0.00012 0.01433 0.01574 N1 5 0.419267 0.524171 0.670362 11.00000 0.02079 0.02842 = 0.03331 -0.00128 0.00537 -0.00326 N2 5 0.520981 0.443440 0.612841 11.00000 0.02891 0.01783 = 0.03596 -0.00560 -0.00032 0.00108 N3 5 0.584295 0.570377 0.578085 11.00000 0.02030 0.02798 = 0.02820 -0.00074 0.00098 -0.00245 N4 5 0.476923 0.634526 0.645639 11.00000 0.02472 0.03217 = 0.03410 -0.00580 0.00110 0.00402 C1 1 0.386341 0.580162 0.696214 11.00000 0.02846 0.03627 = 0.03129 -0.00453 -0.00284 0.00038 C2 1 0.330938 0.554682 0.735223 11.00000 0.02993 0.04591 = 0.03049 -0.00540 0.00171 0.00427 AFIX 43 H2 2 0.298344 0.581112 0.759927 11.00000 -1.20000 AFIX 0 C3 1 0.332641 0.485104 0.731043 11.00000 0.02763 0.03996 = 0.02926 0.00028 0.00158 -0.00277 AFIX 43 H3 2 0.301385 0.455205 0.752609 11.00000 -1.20000 AFIX 0 C4 1 0.389063 0.465283 0.689000 11.00000 0.02775 0.03621 = 0.02458 -0.00074 -0.00088 -0.00208 C5 1 0.415027 0.402436 0.666172 11.00000 0.03142 0.03242 = 0.02443 0.00052 -0.00371 -0.00480 C6 1 0.474987 0.394115 0.628104 11.00000 0.03082 0.02563 = 0.02655 -0.00107 -0.00664 0.00496 C7 1 0.503013 0.332729 0.597346 11.00000 0.03058 0.02419 = 0.03209 0.00479 -0.00205 -0.00401 AFIX 43 H7 2 0.483307 0.289315 0.597572 11.00000 -1.20000 AFIX 0 C8 1 0.561907 0.346318 0.567957 11.00000 0.02657 0.03398 = 0.03130 -0.00323 -0.00030 0.00414 AFIX 43 H8 2 0.590702 0.314570 0.544591 11.00000 -1.20000 AFIX 0 C9 1 0.572656 0.417887 0.578783 11.00000 0.02675 0.02803 = 0.02414 0.00029 -0.00203 -0.00201 C10 1 0.627955 0.454980 0.559045 11.00000 0.02638 0.02630 = 0.02655 -0.00202 -0.00241 0.00003 C11 1 0.632603 0.526243 0.561241 11.00000 0.02495 0.02838 = 0.02461 -0.00053 -0.00265 -0.00027 C12 1 0.687966 0.568207 0.548341 11.00000 0.02626 0.02933 = 0.03429 -0.00054 -0.00025 -0.00207 AFIX 43 H12 2 0.729497 0.552355 0.535397 11.00000 -1.20000 AFIX 0 C13 1 0.670964 0.633855 0.557724 11.00000 0.02913 0.03030 = 0.03275 -0.00042 -0.00124 -0.00495 AFIX 43 H13 2 0.698513 0.671852 0.552399 11.00000 -1.20000 AFIX 0 C14 1 0.604500 0.636540 0.577025 11.00000 0.02951 0.02725 = 0.02803 0.00062 -0.00221 -0.00355 C15 1 0.567576 0.695182 0.593238 11.00000 0.02878 0.02715 = 0.03151 0.00064 -0.00377 -0.00198 C16 1 0.504349 0.694895 0.622208 11.00000 0.03636 0.02409 = 0.03990 -0.00397 -0.00661 -0.00291 C17 1 0.456211 0.744206 0.639011 11.00000 0.03554 0.03181 = 0.04195 -0.00478 -0.00177 0.00410 C18 1 0.403491 0.711161 0.672956 11.00000 0.02893 0.03864 = 0.04538 -0.00574 0.00031 0.00434 AFIX 43 H18 2 0.365271 0.732305 0.690690 11.00000 -1.20000 AFIX 0 C19 1 0.416714 0.641709 0.676290 11.00000 0.02773 0.03408 = 0.03169 -0.00318 0.00004 0.00309 C20 1 0.375747 0.341293 0.683631 11.00000 0.02904 0.03655 = 0.02838 -0.00055 0.00022 -0.00573 C21 1 0.311723 0.339476 0.657325 11.00000 0.02981 0.04035 = 0.03391 0.00145 -0.00040 -0.00616 AFIX 43 H21 2 0.294054 0.376366 0.625982 11.00000 -1.20000 AFIX 0 C22 1 0.273146 0.283948 0.676532 11.00000 0.03605 0.04524 = 0.04415 0.00050 -0.00288 -0.01442 AFIX 43 H22 2 0.229447 0.282435 0.658627 11.00000 -1.20000 AFIX 0 C23 1 0.300150 0.232037 0.721741 11.00000 0.04909 0.03951 = 0.04637 0.00442 -0.00092 -0.01665 C24 1 0.362637 0.230739 0.748625 11.00000 0.05541 0.03439 = 0.04246 0.00925 -0.00197 -0.00821 AFIX 43 H24 2 0.379647 0.193384 0.779723 11.00000 -1.20000 AFIX 0 C25 1 0.400251 0.285827 0.728902 11.00000 0.03692 0.04119 = 0.03449 0.00279 -0.00434 -0.00595 AFIX 43 H25 2 0.444016 0.286020 0.746611 11.00000 -1.20000 AFIX 0 C26 1 0.686048 0.415161 0.536699 11.00000 0.02786 0.02725 = 0.03052 -0.00288 -0.00325 0.00040 C27 1 0.707735 0.362606 0.588711 11.00000 0.03337 0.03249 = 0.04017 0.00238 -0.00008 0.00215 AFIX 43 H27 2 0.685667 0.352538 0.638888 11.00000 -1.20000 AFIX 0 C28 1 0.761120 0.324716 0.568323 11.00000 0.03794 0.03422 = 0.06010 0.00525 -0.00242 0.00728 AFIX 43 H28 2 0.775443 0.288383 0.603375 11.00000 -1.20000 AFIX 0 C29 1 0.792729 0.341155 0.496051 11.00000 0.03551 0.03971 = 0.05801 -0.01087 0.00401 0.00873 C30 1 0.773645 0.393103 0.442454 11.00000 0.03781 0.03922 = 0.04435 -0.00889 0.00903 -0.00089 AFIX 43 H30 2 0.796514 0.403327 0.392972 11.00000 -1.20000 AFIX 0 C31 1 0.719484 0.429868 0.463969 11.00000 0.03568 0.03267 = 0.03207 -0.00206 0.00062 -0.00153 AFIX 43 H31 2 0.705058 0.465741 0.428249 11.00000 -1.20000 AFIX 0 C32 1 0.597711 0.762623 0.581315 11.00000 0.02974 0.02703 = 0.03985 -0.00050 -0.00157 0.00107 C33 1 0.597559 0.810527 0.647151 11.00000 0.03995 0.03024 = 0.04487 -0.00713 0.00106 -0.00276 AFIX 43 H33 2 0.579416 0.798714 0.699535 11.00000 -1.20000 AFIX 0 C34 1 0.623737 0.875463 0.636806 11.00000 0.04641 0.03573 = 0.06418 -0.01499 0.00969 -0.00620 AFIX 43 H34 2 0.623319 0.907855 0.681194 11.00000 -1.20000 AFIX 0 C35 1 0.649598 0.890468 0.561579 11.00000 0.04077 0.02812 = 0.08371 -0.00276 0.01486 -0.00705 C36 1 0.651444 0.845958 0.494700 11.00000 0.04250 0.03318 = 0.05767 -0.00167 0.00978 -0.00721 AFIX 43 H36 2 0.669882 0.858674 0.442829 11.00000 -1.20000 AFIX 0 C37 1 0.625328 0.781573 0.505696 11.00000 0.03707 0.03142 = 0.04310 -0.00262 0.00278 -0.00436 AFIX 43 H37 2 0.626387 0.749878 0.460575 11.00000 -1.20000 AFIX 0 C38 1 0.455045 0.815395 0.617720 11.00000 0.04352 0.04117 = 0.06572 0.00635 0.00146 0.00433 AFIX 43 H38 2 0.485171 0.832059 0.578892 11.00000 -1.20000 AFIX 0 HKLF 4 REM au_mf_10_a.res in C2/c REM R1 = 0.0377 for 8633 Fo > 4sig(Fo) and 0.0453 for all 10078 data REM 424 parameters refined using 0 restraints END WGHT 0.0363 49.2088 REM Highest difference peak 1.925, deepest hole -1.512, 1-sigma level 0.154 Q1 1 0.4900 0.4578 0.6246 11.00000 0.05 1.92 Q2 1 0.4806 0.5730 0.6356 11.00000 0.05 1.74 Q3 1 0.5277 0.5701 0.6110 11.00000 0.05 1.26 Q4 1 0.2725 0.4630 0.7612 11.00000 0.05 1.13 Q5 1 0.4262 0.9179 0.6586 11.00000 0.05 1.07 Q6 1 0.4957 0.4923 0.5794 11.00000 0.05 1.04 Q7 1 0.5574 0.5362 0.6205 11.00000 0.05 0.93 Q8 1 0.5501 0.5216 0.6021 11.00000 0.05 0.89 Q9 1 0.5304 0.4894 0.6258 11.00000 0.05 0.88 Q10 1 0.4668 0.4971 0.6395 11.00000 0.05 0.87 ; _shelx_res_checksum 19723 _shelx_fab_file ; -30 0 2 0.7109 -4.5392 -29 1 1 1.0437 -2.1134 -29 1 2 -0.3008 1.3810 -29 1 3 -0.9810 0.2968 -29 1 4 2.0986 -0.3642 -29 1 5 1.2151 0.4637 -29 1 6 -0.4720 0.0936 -29 3 1 1.7769 -0.3669 -29 3 2 3.0346 -3.1749 -29 3 3 -3.0980 -5.0438 -29 3 4 -0.1733 4.0491 -29 3 5 3.2711 1.2515 -29 3 6 -0.7698 1.2420 -29 5 1 1.8803 -0.1081 -29 5 2 4.7971 -0.7721 -29 5 3 2.4626 -2.3846 -29 5 4 -1.8382 0.7118 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0.4797 24 12 8 1.0758 -0.5684 24 12 9 -0.1927 -0.6013 24 14 0 1.6673 0.7327 24 14 1 0.8312 0.3194 24 14 2 0.3409 0.4248 24 14 3 -3.1793 -0.1107 24 14 4 -0.4058 -1.2803 24 14 5 0.3847 0.4461 24 14 6 2.0899 -0.0433 24 14 7 0.6092 -0.6815 24 16 0 3.0482 0.0949 24 16 1 0.7273 -0.2046 24 16 2 0.8408 0.3657 24 16 3 -0.5141 0.7718 24 16 4 -2.2833 -2.7584 25 1 0 1.8062 6.4144 25 1 1 0.5493 3.6653 25 1 2 1.1146 -4.0216 25 1 3 1.1614 1.5890 25 1 4 -1.0865 -5.7481 25 1 5 0.5413 -4.2837 25 1 6 0.5501 2.3440 25 1 7 -1.4436 -1.4266 25 1 8 -0.3587 5.4060 25 1 9 0.1223 2.8129 25 1 10 -2.0284 -3.6653 25 1 11 1.3430 -0.0600 25 1 12 0.9656 -1.3993 25 3 0 0.4124 -0.9934 25 3 1 -0.9507 -2.8881 25 3 2 -1.2769 -0.2644 25 3 3 1.5739 -0.5351 25 3 4 -0.1305 0.8919 25 3 5 -0.6619 2.7805 25 3 6 0.7245 -0.9929 25 3 7 -1.4985 -0.4188 25 3 8 -1.6737 0.1566 25 3 9 -0.9059 -1.5716 25 3 10 -1.8339 -1.4647 25 3 11 -0.0699 -2.5537 25 5 0 1.5839 -0.0963 25 5 1 -1.6087 -0.2464 25 5 2 -2.8136 0.1628 25 5 3 0.3866 0.1922 25 5 4 0.5087 -1.0127 25 5 5 -1.3253 0.2385 25 5 6 -2.2151 -0.0962 25 5 7 1.4260 -0.2002 25 5 8 0.0177 0.9485 25 5 9 -0.1407 2.0434 25 5 10 0.3344 0.2458 25 5 11 -1.5695 -1.2822 25 7 0 1.1631 -1.6610 25 7 1 -1.8124 -0.1024 25 7 2 -2.9607 0.8990 25 7 3 2.5608 1.1116 25 7 4 -0.3026 2.2466 25 7 5 1.4613 0.1016 25 7 6 -3.1184 -1.5327 25 7 7 -0.2987 0.5771 25 7 8 1.9503 -2.1619 25 7 9 2.3676 -0.7994 25 7 10 2.6864 2.0845 25 9 0 0.1333 0.1832 25 9 1 -3.8628 0.2860 25 9 2 -4.7450 -1.3723 25 9 3 2.1857 0.9201 25 9 4 -0.1790 -1.3121 25 9 5 1.0919 -0.3148 25 9 6 1.4793 0.3410 25 9 7 -3.0571 1.0171 25 9 8 1.0619 2.6467 25 9 9 3.0126 -2.9569 25 11 0 0.2330 -0.6914 25 11 1 -4.6213 -0.0517 25 11 2 -3.9248 -0.4636 25 11 3 -0.3141 0.9470 25 11 4 -0.1678 -0.2825 25 11 5 -0.7568 -1.1314 25 11 6 -0.6462 0.6781 25 11 7 -2.8468 -1.0676 25 11 8 -1.0528 2.4858 25 13 0 0.1381 -0.4222 25 13 1 -3.2356 -0.7056 25 13 2 -1.7554 -0.6073 25 13 3 1.5823 0.7378 25 13 4 -0.1702 0.1484 25 13 5 1.5311 -0.2520 25 13 6 -1.7499 1.2432 25 15 0 -2.6224 -0.7926 25 15 1 -2.3350 -0.5271 25 15 2 -2.0455 -1.2645 25 15 3 1.0705 0.2703 26 0 0 -5.8244 -10.7427 26 0 2 1.4090 6.5034 26 0 4 4.0138 9.9515 26 0 6 -0.0601 -5.5111 26 0 8 -1.8707 -8.2595 26 0 10 2.7967 4.8500 26 2 0 -3.6302 -0.1055 26 2 1 -1.0144 -1.0721 26 2 2 1.8102 1.5296 26 2 3 -1.3995 -0.5249 26 2 4 2.7374 0.0133 26 2 5 0.0925 1.4334 26 2 6 -0.7946 0.3008 26 2 7 3.2783 0.8849 26 2 8 0.3401 -0.0586 26 2 9 -0.0654 -0.1269 26 2 10 2.8626 2.5817 26 4 0 -3.3293 -0.2244 26 4 1 0.8841 2.0291 26 4 2 2.4370 0.6930 26 4 3 -0.4585 2.2574 26 4 4 -0.0828 0.5045 26 4 5 1.4468 -2.3204 26 4 6 -0.0884 -0.2463 26 4 7 0.9882 0.0384 26 4 8 1.3229 -0.4514 26 4 9 1.2796 -0.4566 26 4 10 2.3326 2.2153 26 6 0 -2.9854 0.7574 26 6 1 0.7968 -1.3431 26 6 2 1.5814 -1.3737 26 6 3 -0.9011 0.6193 26 6 4 0.6013 -1.6514 26 6 5 -0.0042 0.5548 26 6 6 2.1799 1.2189 26 6 7 -0.5122 0.9047 26 6 8 -1.2136 2.2945 26 6 9 -1.2213 -3.7583 26 8 0 -2.0654 0.0405 26 8 1 0.9446 0.0306 26 8 2 2.4370 0.5811 26 8 3 -1.6648 0.3108 26 8 4 0.7218 -0.6836 26 8 5 -1.3677 -2.5238 26 8 6 0.1235 -0.0421 26 8 7 2.2898 -0.7226 26 8 8 -0.9454 1.0239 26 10 0 -0.6640 1.1715 26 10 1 1.1205 -0.6288 26 10 2 3.3409 1.5138 26 10 3 2.6819 -0.8781 26 10 4 0.3576 2.1770 26 10 5 -0.7433 0.5520 26 10 6 -0.7525 -1.1942 26 10 7 2.6642 0.2133 26 12 0 -0.3892 1.4103 26 12 1 1.8403 0.8245 26 12 2 1.4677 0.5663 26 12 3 2.4477 -1.2880 26 12 4 1.0210 0.9756 26 12 5 -1.9009 0.4185 26 14 0 0.6409 1.8432 26 14 1 2.7899 0.9672 27 1 0 4.7640 5.2577 27 1 1 0.9619 3.5983 27 1 2 -0.5337 -3.3019 27 1 3 0.5836 1.4364 27 1 4 -5.0590 -5.1014 27 1 5 0.3899 -3.2876 27 1 6 -0.7523 3.9529 27 1 7 -2.5938 -0.3613 27 1 8 1.9912 0.7814 27 1 9 0.6712 0.5570 27 3 0 2.8548 -0.9875 27 3 1 -0.1058 -2.2946 27 3 2 -0.7067 -0.1207 27 3 3 0.2373 -1.2288 27 3 4 -1.4263 0.2515 27 3 5 -0.5905 0.0932 27 3 6 0.7146 1.6238 27 3 7 -3.5854 1.1414 27 3 8 -1.5630 -2.6378 27 3 9 -0.7531 -2.3004 27 5 0 2.3873 0.8770 27 5 1 -0.5755 0.2311 27 5 2 0.3539 1.0186 27 5 3 -0.6166 -1.9342 27 5 4 0.5898 -0.4823 27 5 5 -0.0158 -2.0561 27 5 6 -0.3257 1.0806 27 5 7 -0.3524 0.4589 27 5 8 -0.5568 -1.4106 27 7 0 0.5259 -0.0376 27 7 1 -0.2607 1.1605 27 7 2 0.7585 1.3283 27 7 3 1.2992 -1.2111 27 7 4 -0.3798 2.4138 27 7 5 0.3274 1.0698 27 7 6 -0.9007 -0.4568 27 7 7 -0.6419 -0.4971 27 9 0 0.1678 -0.0626 27 9 1 1.0007 1.6788 27 9 2 -1.1338 -1.4795 27 9 3 -0.8204 -1.2297 27 9 4 0.8333 -2.0507 27 9 5 -0.4565 2.7313 27 9 6 -0.2206 1.9641 27 11 0 -1.0429 -1.8089 27 11 1 1.5806 0.4929 27 11 2 -0.1940 -0.8887 27 11 3 -3.8587 0.1355 27 11 4 -0.4589 -2.5153 28 0 0 -1.5726 -9.7354 28 0 2 -2.3908 4.7019 28 0 4 4.5418 7.6345 28 0 6 2.0856 -5.0595 28 2 0 -0.0980 0.1495 28 2 1 0.0858 0.7134 28 2 2 -1.6732 -1.0543 28 2 3 0.4578 -1.1170 28 2 4 2.5811 1.1412 28 2 5 -0.7821 2.5281 28 2 6 0.1304 -3.6014 28 2 7 3.8597 -0.9305 28 4 0 -0.2695 0.3145 28 4 1 0.6435 4.6112 28 4 2 -1.4247 -1.5783 28 4 3 2.5480 0.5945 28 4 4 -1.3034 1.0823 28 4 5 -0.9407 2.7775 28 4 6 -1.0096 -3.1732 28 4 7 2.0646 -2.2184 28 6 0 1.9649 0.1854 28 6 1 0.1702 0.8646 28 6 2 -2.2369 -2.4731 28 6 3 1.4523 -0.5379 28 6 4 -0.9825 -1.4886 28 6 5 -1.7055 4.0429 28 6 6 -0.4778 -0.0306 28 8 0 2.1716 -0.0619 28 8 1 0.4758 -1.0616 28 8 2 -0.3722 0.0967 28 8 3 -0.7299 0.5887 28 8 4 -1.2256 -0.7205 28 10 0 1.8398 1.3219 28 10 1 -1.6351 -2.3150 29 1 0 -1.4159 3.9278 29 1 1 -0.2680 1.0202 29 1 2 3.2992 0.1368 29 1 3 -0.4115 0.9438 29 1 4 -1.9584 -2.2188 29 1 5 0.9614 -1.6231 29 3 0 -1.1827 -2.8532 29 3 1 -0.9266 -6.5138 29 3 2 1.4114 2.8042 29 3 3 -2.9302 0.2204 29 3 4 0.7356 0.7867 29 5 0 -1.5302 -1.2391 29 5 1 0.7366 -5.9285 29 5 2 1.5366 2.2185 29 5 3 -4.1951 1.0424 29 7 0 -3.9253 -1.0696 29 7 1 -0.6405 -2.6005 30 0 0 0.3149 -6.8256 0 0 0 0.0 0.0 ; _shelx_fab_checksum 51752 _olex2_submission_special_instructions 'No special instructions were received' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' ####################################################################### # # 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_Bi_CHO_DCMHex_a _database_code_depnum_ccdc_archive 'CCDC 2091848' loop_ _audit_author_name _audit_author_address 'Simon J. Teat' ;Lawrence Berkeley National Laboratory United States of America ; _audit_update_record ; 2021-06-24 deposited with the CCDC. 2021-09-29 downloaded from the CCDC. ; _audit_creation_method SHELXL-2018/1 _shelx_SHELXL_version_number 2018/1 _chemical_name_systematic 'Rhenium-oxo 3,17-diformyl-5,10,15-tris(p-methylphenyl)corrole' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 N4 O3 Re' _chemical_formula_weight 866.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0034 0.0017 'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992' H H 0.0000 0.0000 'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992' N N 0.0065 0.0035 'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992' O O 0.0115 0.0064 'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992' Re Re -1.0625 7.5606 'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992' _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 9.5807(4) _cell_length_b 12.6649(6) _cell_length_c 29.1467(13) _cell_angle_alpha 95.279(2) _cell_angle_beta 91.627(2) _cell_angle_gamma 90.341(2) _cell_volume 3520.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2.5978 _cell_measurement_theta_max 31.3995 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_F_000 1732 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 3.707 _shelx_estimated_absorpt_T_min 0.483 _shelx_estimated_absorpt_T_max 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS 2016/2 Bruker AXS Madison WI USA' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7288 _diffrn_radiation_type synchrotron _diffrn_source 'Advanced Light Source beamline 12.2.1' _diffrn_measurement_device_type 'Bruker D8 with PHOTONII detector' _diffrn_measurement_method '\w/\q shutterless scans' _diffrn_detector_area_resol_mean 7.39 _diffrn_reflns_number 131064 _diffrn_reflns_av_unetI/netI 0.0249 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.744 _diffrn_reflns_theta_max 31.439 _diffrn_reflns_theta_full 25.930 _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 21566 _reflns_number_gt 19296 _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 APEX 3' _computing_cell_refinement 'Bruker SAINT v8.38a' _computing_data_reduction 'Bruker SAINT v8.38a' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _refine_special_details ; All non-hydrogen atoms were refined anisotropically, except the disordered CHO groups. Hydrogen atoms placed geometrically constrained and refined using a riding model. The disordered CHO groups were modelled with geometrical restraints. The lowest occupied CHO group was fixed at 7%. ; _vrf_PLAT411_Bi_CHO_DCMHex_a ; PROBLEM: Short Inter H...H Contact H37A ..H2A . 1.70 Ang. RESPONSE: H2A and H2'a are on the low occupancy CHO group at 10 and 7% occupancy. While these showed unclearly in the different map the disorder in the phenyl rings containing H37a and H37b. ; _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^)+(0.0109P)^2^+8.9113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Dual space' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 21566 _refine_ls_number_parameters 975 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.104 _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 Re1 Re 0.54163(2) 0.19934(2) 0.58285(2) 0.02058(3) Uani 1 1 d . . . . . O1 O 0.4181(2) 0.13045(16) 0.60741(7) 0.0270(4) Uani 1 1 d . . . . . C1 C 0.5454(3) 0.1421(2) 0.48340(9) 0.0248(5) Uani 1 1 d D . . . . N1 N 0.4944(2) 0.21704(18) 0.51649(7) 0.0224(4) Uani 1 1 d . . . . . C2 C 0.4934(3) 0.1643(2) 0.44028(9) 0.0273(6) Uani 1 1 d D . . . . H2B H 0.510116 0.124603 0.411729 0.033 Uiso 0.918(5) 1 calc R U P A 1 C3 C 0.4121(3) 0.2556(2) 0.44658(9) 0.0267(6) Uani 1 1 d D . . . . H3A H 0.364755 0.289680 0.423041 0.032 Uiso 0.082(5) 1 calc R U P A 2 C4 C 0.4131(3) 0.2883(2) 0.49495(9) 0.0242(5) Uani 1 1 d D . . . . C5 C 0.3581(3) 0.3780(2) 0.52011(9) 0.0243(5) Uani 1 1 d . . . . . C6 C 0.4017(3) 0.4086(2) 0.56578(9) 0.0235(5) Uani 1 1 d . . . . . N2 N 0.5000(2) 0.35529(17) 0.59182(8) 0.0212(4) Uani 1 1 d . . . . . C7 C 0.3651(3) 0.5034(2) 0.59310(10) 0.0262(5) Uani 1 1 d . . . . . H7A H 0.297703 0.553346 0.584668 0.031 Uiso 1 1 calc R U . . . C8 C 0.4425(3) 0.5104(2) 0.63309(10) 0.0250(5) Uani 1 1 d . . . . . H8A H 0.439686 0.566236 0.657155 0.030 Uiso 1 1 calc R U . . . C9 C 0.5287(3) 0.4188(2) 0.63242(9) 0.0222(5) Uani 1 1 d . . . . . C10 C 0.6290(3) 0.3970(2) 0.66604(9) 0.0222(5) Uani 1 1 d . . . . . N3 N 0.7055(2) 0.22672(18) 0.62721(8) 0.0220(4) Uani 1 1 d . . . . . C11 C 0.7143(3) 0.3084(2) 0.66275(9) 0.0225(5) Uani 1 1 d . . . . . C12 C 0.8246(3) 0.2855(2) 0.69402(9) 0.0243(5) Uani 1 1 d . . . . . H12A H 0.852851 0.328056 0.721283 0.029 Uiso 1 1 calc R U . . . C13 C 0.8824(3) 0.1917(2) 0.67792(10) 0.0258(5) Uani 1 1 d . . . . . H13A H 0.957344 0.157108 0.692262 0.031 Uiso 1 1 calc R U . . . C14 C 0.8110(3) 0.1544(2) 0.63577(9) 0.0243(5) Uani 1 1 d . . . . . C15 C 0.8452(3) 0.0640(2) 0.60679(9) 0.0233(5) Uani 1 1 d . . . . . C16 C 0.7831(3) 0.0419(2) 0.56279(10) 0.0248(5) Uani 1 1 d . . . . . N4 N 0.6740(2) 0.10216(18) 0.54841(8) 0.0230(4) Uani 1 1 d . . . . . C17 C 0.8190(3) -0.0293(2) 0.52356(10) 0.0262(5) Uani 1 1 d . . . . . C18 C 0.7341(3) -0.0063(2) 0.48631(10) 0.0267(6) Uani 1 1 d . . . . . H18A H 0.736193 -0.040276 0.455893 0.032 Uiso 1 1 calc R U . . . C19 C 0.6455(3) 0.0756(2) 0.50162(9) 0.0250(5) Uani 1 1 d . . . . . C20 C 0.3627(3) 0.3098(3) 0.40683(10) 0.0289(7) Uani 0.918(5) 1 d D . P A 1 H20A H 0.331321 0.380869 0.411862 0.035 Uiso 0.918(5) 1 calc R U P A 1 O2 O 0.3604(3) 0.2668(2) 0.36747(8) 0.0368(7) Uani 0.918(5) 1 d D . P A 1 C20A C 0.516(3) 0.1089(18) 0.3949(4) 0.023(7) Uiso 0.082(5) 1 d D . P A 2 H2A H 0.572031 0.047370 0.390440 0.028 Uiso 0.082(5) 1 calc R U P A 2 O2A O 0.456(3) 0.149(2) 0.3629(8) 0.038(7) Uiso 0.082(5) 1 d D . P A 2 C21 C 0.2584(3) 0.4445(2) 0.49559(9) 0.0247(5) Uani 1 1 d . . . . . C22 C 0.2816(3) 0.5523(2) 0.49236(10) 0.0271(6) Uani 1 1 d . . . . . H22A H 0.359350 0.586668 0.508447 0.033 Uiso 1 1 calc R U . . . C23 C 0.1926(3) 0.6104(2) 0.46596(10) 0.0272(6) Uani 1 1 d . . . . . H23A H 0.209216 0.684114 0.464897 0.033 Uiso 1 1 calc R U . . . C24 C 0.0796(3) 0.5621(2) 0.44103(9) 0.0258(5) Uani 1 1 d . . . . . C25 C 0.0549(3) 0.4551(2) 0.44521(10) 0.0261(5) Uani 1 1 d . . . . . H25A H -0.022727 0.420884 0.429027 0.031 Uiso 1 1 calc R U . . . C26 C 0.1407(3) 0.3973(2) 0.47236(10) 0.0253(5) Uani 1 1 d . . . . . H26A H 0.119556 0.324932 0.475268 0.030 Uiso 1 1 calc R U . . . C27 C -0.0105(3) 0.6243(2) 0.41067(10) 0.0302(6) Uani 1 1 d . . . . . H27A H -0.018106 0.697356 0.424693 0.045 Uiso 1 1 calc R U . . . H27B H -0.103715 0.591778 0.407073 0.045 Uiso 1 1 calc R U . . . H27C H 0.031270 0.624630 0.380383 0.045 Uiso 1 1 calc R U . . . C28 C 0.6492(3) 0.4756(2) 0.70714(9) 0.0230(5) Uani 1 1 d . . . . . C29 C 0.7460(4) 0.5560(3) 0.70745(13) 0.0466(9) Uani 1 1 d . . . . . H29A H 0.800268 0.562309 0.681054 0.056 Uiso 1 1 calc R U . . . C30 C 0.7654(4) 0.6283(3) 0.74600(14) 0.0460(9) Uani 1 1 d . . . . . H30A H 0.834562 0.682322 0.745621 0.055 Uiso 1 1 calc R U . . . C31 C 0.6881(3) 0.6240(2) 0.78432(10) 0.0298(6) Uani 1 1 d . . . . . C32 C 0.5922(4) 0.5427(3) 0.78407(11) 0.0440(9) Uani 1 1 d . . . . . H32A H 0.538243 0.536792 0.810565 0.053 Uiso 1 1 calc R U . . . C33 C 0.5724(4) 0.4691(3) 0.74601(11) 0.0395(8) Uani 1 1 d . . . . . H33A H 0.505244 0.413807 0.746825 0.047 Uiso 1 1 calc R U . . . C34 C 0.7080(4) 0.7047(3) 0.82569(11) 0.0377(7) Uani 1 1 d . . . . . H34A H 0.618778 0.738969 0.832783 0.057 Uiso 1 1 calc R U . . . H34B H 0.776574 0.758320 0.818784 0.057 Uiso 1 1 calc R U . . . H34C H 0.741675 0.669025 0.852279 0.057 Uiso 1 1 calc R U . . . C35 C 0.9530(3) -0.0096(2) 0.62280(10) 0.0247(5) Uani 1 1 d . . . . . C36 C 1.0941(3) 0.0174(2) 0.62735(10) 0.0272(6) Uani 1 1 d . . . . . H36A H 1.124111 0.086218 0.621250 0.033 Uiso 1 1 calc R U . . . C37 C 1.1911(3) -0.0553(2) 0.64069(11) 0.0323(6) Uani 1 1 d . . . . . H37A H 1.287017 -0.035725 0.643515 0.039 Uiso 1 1 calc R U . . . C38 C 1.1502(4) -0.1572(2) 0.65009(11) 0.0328(6) Uani 1 1 d . . . . . C39 C 1.0090(4) -0.1835(2) 0.64568(11) 0.0329(6) Uani 1 1 d . . . . . H39A H 0.978908 -0.252115 0.652023 0.039 Uiso 1 1 calc R U . . . C40 C 0.9112(3) -0.1112(2) 0.63220(11) 0.0299(6) Uani 1 1 d . . . . . H40A H 0.815246 -0.130842 0.629345 0.036 Uiso 1 1 calc R U . . . C41 C 1.2562(4) -0.2361(3) 0.66491(15) 0.0471(9) Uani 1 1 d . . . . . H41A H 1.215395 -0.307662 0.660850 0.071 Uiso 1 1 calc R U . . . H41B H 1.282880 -0.218477 0.697429 0.071 Uiso 1 1 calc R U . . . H41C H 1.339007 -0.233483 0.646066 0.071 Uiso 1 1 calc R U . . . C42 C 0.9315(3) -0.1067(2) 0.51865(11) 0.0306(6) Uani 1 1 d . . . . . H42A H 0.993398 -0.113630 0.544209 0.037 Uiso 1 1 calc R U . . . O3 O 0.9486(3) -0.16229(18) 0.48312(8) 0.0379(5) Uani 1 1 d . . . . . Re1' Re 0.03967(2) 0.81365(2) 0.91438(2) 0.02485(3) Uani 1 1 d . . . . . O1' O -0.0903(2) 0.88202(17) 0.89099(7) 0.0290(4) Uani 1 1 d . . . . . C1' C 0.0644(3) 0.8710(3) 1.01360(10) 0.0318(6) Uani 1 1 d D . . . . N1' N 0.0060(3) 0.7957(2) 0.98058(8) 0.0288(5) Uani 1 1 d . . . . . C2' C 0.0199(3) 0.8491(3) 1.05688(10) 0.0342(7) Uani 1 1 d D . . . . H2'B H 0.041512 0.889245 1.085384 0.041 Uiso 0.93 1 calc R U P B 1 C3' C -0.0622(3) 0.7575(3) 1.05057(10) 0.0328(7) Uani 1 1 d D . . . . H3'A H -0.104655 0.723085 1.074281 0.039 Uiso 0.07 1 calc R U P C 2 C4' C -0.0717(3) 0.7238(2) 1.00212(10) 0.0296(6) Uani 1 1 d D . . . . C5' C -0.1326(3) 0.6339(2) 0.97693(10) 0.0290(6) Uani 1 1 d . . . . . C6' C -0.0964(3) 0.6035(2) 0.93131(10) 0.0277(6) Uani 1 1 d . . . . . N2' N -0.0013(3) 0.65663(19) 0.90545(8) 0.0256(5) Uani 1 1 d . . . . . C7' C -0.1385(3) 0.5083(2) 0.90417(10) 0.0293(6) Uani 1 1 d . . . . . H7'A H -0.206224 0.458717 0.912320 0.035 Uiso 1 1 calc R U . . . C8' C -0.0651(3) 0.5006(2) 0.86459(10) 0.0289(6) Uani 1 1 d . . . . . H8'A H -0.071395 0.444192 0.840751 0.035 Uiso 1 1 calc R U . . . C9' C 0.0225(3) 0.5919(2) 0.86527(10) 0.0268(6) Uani 1 1 d . . . . . C10' C 0.1183(3) 0.6133(2) 0.83203(10) 0.0261(5) Uani 1 1 d . . . . . C11' C 0.1993(3) 0.7057(2) 0.83419(9) 0.0259(5) Uani 1 1 d . . . . . N3' N 0.1935(3) 0.78872(19) 0.86913(8) 0.0260(5) Uani 1 1 d . . . . . C12' C 0.3028(3) 0.7320(2) 0.80279(10) 0.0293(6) Uani 1 1 d . . . . . H12B H 0.328557 0.689408 0.775860 0.035 Uiso 1 1 calc R U . . . C13' C 0.3584(3) 0.8284(2) 0.81802(10) 0.0301(6) Uani 1 1 d . . . . . H13B H 0.427438 0.865780 0.803047 0.036 Uiso 1 1 calc R U . . . C14' C 0.2950(3) 0.8638(2) 0.86033(10) 0.0277(6) Uani 1 1 d . . . . . C15' C 0.3366(3) 0.9532(2) 0.88948(10) 0.0292(6) Uani 1 1 d . . . . . C16' C 0.2853(3) 0.9732(2) 0.93416(10) 0.0303(6) Uani 1 1 d . . . . . N4' N 0.1786(3) 0.9122(2) 0.94859(8) 0.0277(5) Uani 1 1 d . . . . . C17' C 0.3323(3) 1.0426(2) 0.97331(11) 0.0319(6) Uani 1 1 d . . . . . C18' C 0.2536(3) 1.0197(3) 1.01071(11) 0.0331(7) Uani 1 1 d . . . . . H18B H 0.261947 1.053408 1.041162 0.040 Uiso 1 1 calc R U . . . C19' C 0.1608(3) 0.9383(3) 0.99534(10) 0.0311(6) Uani 1 1 d . . . . . C20' C -0.1042(4) 0.7025(3) 1.08998(10) 0.0309(7) Uani 0.93 1 d D . P D 1 H20B H -0.136936 0.631357 1.084823 0.037 Uiso 0.93 1 calc R U P D 1 O2' O -0.0985(3) 0.7451(2) 1.12931(8) 0.0380(6) Uani 0.93 1 d D . P D 1 C20" C 0.059(8) 0.902(4) 1.1024(5) 0.09(3) Uiso 0.07 1 d D . P E 2 H2'A H 0.121098 0.959808 1.109741 0.109 Uiso 0.07 1 calc R U P E 2 O2" O -0.010(6) 0.853(4) 1.1289(17) 0.087(16) Uiso 0.07 1 d D . P E 2 C21' C -0.2281(3) 0.5666(3) 1.00131(10) 0.0309(6) Uani 1 1 d . . . . . C22' C -0.2051(3) 0.4596(3) 1.00489(10) 0.0326(6) Uani 1 1 d . . . . . H22B H -0.130468 0.425548 0.988823 0.039 Uiso 1 1 calc R U . . . C23' C -0.2888(3) 0.4016(3) 1.03138(10) 0.0323(6) Uani 1 1 d . . . . . H23B H -0.271682 0.328090 1.032666 0.039 Uiso 1 1 calc R U . . . C24' C -0.3978(3) 0.4488(3) 1.05624(10) 0.0320(6) Uani 1 1 d . . . . . C25' C -0.4232(3) 0.5552(3) 1.05183(10) 0.0335(7) Uani 1 1 d . . . . . H25B H -0.498269 0.588909 1.067804 0.040 Uiso 1 1 calc R U . . . C26' C -0.3416(3) 0.6130(3) 1.02465(10) 0.0326(6) Uani 1 1 d . . . . . H26B H -0.362753 0.685343 1.021739 0.039 Uiso 1 1 calc R U . . . C27' C -0.4843(4) 0.3860(3) 1.08673(11) 0.0364(7) Uani 1 1 d . . . . . H27D H -0.450643 0.312856 1.085313 0.055 Uiso 1 1 calc R U . . . H27E H -0.476290 0.418236 1.118580 0.055 Uiso 1 1 calc R U . . . H27F H -0.582323 0.385967 1.076122 0.055 Uiso 1 1 calc R U . . . C28' C 0.1440(3) 0.5294(2) 0.79390(10) 0.0257(5) Uani 1 1 d . . . . . C29' C 0.1916(3) 0.4303(2) 0.80399(10) 0.0294(6) Uani 1 1 d . . . . . H29B H 0.205118 0.416153 0.835242 0.035 Uiso 1 1 calc R U . . . C30' C 0.2196(3) 0.3517(2) 0.76900(11) 0.0311(6) Uani 1 1 d . . . . . H30B H 0.249922 0.284148 0.776778 0.037 Uiso 1 1 calc R U . . . C31' C 0.2041(3) 0.3702(2) 0.72291(10) 0.0294(6) Uani 1 1 d . . . . . C32' C 0.1557(3) 0.4688(3) 0.71285(11) 0.0321(6) Uani 1 1 d . . . . . H32B H 0.143010 0.482845 0.681557 0.039 Uiso 1 1 calc R U . . . C33' C 0.1252(3) 0.5477(2) 0.74767(10) 0.0296(6) Uani 1 1 d . . . . . H33B H 0.091452 0.614250 0.739827 0.036 Uiso 1 1 calc R U . . . C34' C 0.2428(4) 0.2869(3) 0.68532(12) 0.0368(7) Uani 1 1 d . . . . . H34D H 0.274457 0.223117 0.699072 0.055 Uiso 1 1 calc R U . . . H34E H 0.161056 0.269257 0.665002 0.055 Uiso 1 1 calc R U . . . H34F H 0.317930 0.313970 0.667403 0.055 Uiso 1 1 calc R U . . . C35' C 0.4409(3) 1.0277(2) 0.87309(10) 0.0302(6) Uani 1 1 d . . . . . C36' C 0.5813(3) 1.0013(3) 0.86895(11) 0.0338(7) Uani 1 1 d . . . . . H36B H 0.611525 0.932663 0.875266 0.041 Uiso 1 1 calc R U . . . C37' C 0.6770(4) 1.0741(3) 0.85572(13) 0.0386(7) Uani 1 1 d . . . . . H37B H 0.772383 1.054921 0.853188 0.046 Uiso 1 1 calc R U . . . C38' C 0.6353(4) 1.1758(3) 0.84602(13) 0.0402(8) Uani 1 1 d . . . . . C39' C 0.4951(4) 1.2010(3) 0.84992(12) 0.0388(7) Uani 1 1 d . . . . . H39B H 0.464680 1.269500 0.843520 0.047 Uiso 1 1 calc R U . . . C40' C 0.3982(4) 1.1283(3) 0.86298(12) 0.0350(7) Uani 1 1 d . . . . . H40B H 0.302544 1.147094 0.865040 0.042 Uiso 1 1 calc R U . . . C41' C 0.7395(5) 1.2545(3) 0.83080(17) 0.0563(11) Uani 1 1 d . . . . . H41D H 0.832585 1.222814 0.830099 0.085 Uiso 1 1 calc R U . . . H41E H 0.712515 1.273359 0.799933 0.085 Uiso 1 1 calc R U . . . H41F H 0.741040 1.318413 0.852498 0.085 Uiso 1 1 calc R U . . . C42' C 0.4509(4) 1.1164(3) 0.97831(12) 0.0379(7) Uani 1 1 d . . . . . H42B H 0.505419 1.125536 0.952219 0.045 Uiso 1 1 calc R U . . . O3' O 0.4822(3) 1.16685(19) 1.01509(9) 0.0459(6) Uani 1 1 d . . . . . C1S C 1.0674(5) 0.0097(5) 0.7778(2) 0.0784(16) Uani 1 1 d . . . . . H1SA H 1.141254 -0.026252 0.794137 0.118 Uiso 1 1 calc R U . . . H1SB H 1.100961 0.026870 0.747866 0.118 Uiso 1 1 calc R U . . . H1SC H 1.041930 0.075115 0.796102 0.118 Uiso 1 1 calc R U . . . C2S C 0.9386(5) -0.0637(4) 0.77021(15) 0.0573(11) Uani 1 1 d . . . . . H2SA H 0.965673 -0.130235 0.752290 0.069 Uiso 1 1 calc R U . . . H2SB H 0.906668 -0.082011 0.800505 0.069 Uiso 1 1 calc R U . . . C3S C 0.8177(5) -0.0136(3) 0.74474(14) 0.0479(9) Uani 1 1 d . . . . . H3SA H 0.792996 0.053819 0.762497 0.058 Uiso 1 1 calc R U . . . H3SB H 0.850434 0.004064 0.714432 0.058 Uiso 1 1 calc R U . . . C4S C 0.6872(5) -0.0810(4) 0.73687(16) 0.0585(11) Uani 1 1 d . . . . . H4SA H 0.647612 -0.091587 0.767136 0.070 Uiso 1 1 calc R U . . . H4SB H 0.713090 -0.151476 0.722205 0.070 Uiso 1 1 calc R U . . . C5S C 0.5758(6) -0.0346(4) 0.70712(19) 0.0677(13) Uani 1 1 d . . . . . H5SA H 0.615573 -0.024174 0.676870 0.081 Uiso 1 1 calc R U . . . H5SB H 0.498276 -0.086696 0.701622 0.081 Uiso 1 1 calc R U . . . C6S C 0.5179(5) 0.0678(4) 0.72674(17) 0.0687(13) Uani 1 1 d . . . . . H6SA H 0.446769 0.092057 0.705357 0.103 Uiso 1 1 calc R U . . . H6SB H 0.475565 0.058170 0.756308 0.103 Uiso 1 1 calc R U . . . H6SC H 0.593095 0.120816 0.731507 0.103 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 Re1 0.02278(5) 0.01993(5) 0.01852(5) -0.00161(4) 0.00360(4) -0.00329(4) O1 0.0289(10) 0.0279(10) 0.0238(9) -0.0008(8) 0.0041(8) -0.0037(8) C1 0.0271(13) 0.0249(13) 0.0216(12) -0.0027(10) 0.0052(10) -0.0076(10) N1 0.0249(11) 0.0249(11) 0.0171(10) -0.0005(8) 0.0016(8) -0.0037(9) C2 0.0302(14) 0.0310(14) 0.0200(12) -0.0015(10) 0.0033(10) -0.0094(11) C3 0.0274(14) 0.0290(14) 0.0235(13) 0.0011(10) 0.0005(10) -0.0098(11) C4 0.0242(13) 0.0251(13) 0.0231(12) 0.0011(10) 0.0002(10) -0.0076(10) C5 0.0222(12) 0.0260(13) 0.0244(12) 0.0019(10) -0.0004(10) -0.0050(10) C6 0.0214(12) 0.0241(12) 0.0247(12) 0.0012(10) 0.0012(10) -0.0027(10) N2 0.0225(10) 0.0183(10) 0.0223(10) -0.0004(8) 0.0015(8) -0.0017(8) C7 0.0236(13) 0.0261(13) 0.0287(14) 0.0006(11) 0.0007(10) 0.0019(10) C8 0.0241(13) 0.0224(12) 0.0280(13) -0.0014(10) 0.0008(10) 0.0009(10) C9 0.0216(12) 0.0217(12) 0.0227(12) -0.0019(9) 0.0030(9) -0.0020(9) C10 0.0241(12) 0.0209(12) 0.0207(12) -0.0030(9) 0.0021(9) -0.0023(10) N3 0.0224(11) 0.0211(10) 0.0216(10) -0.0023(8) 0.0007(8) -0.0013(8) C11 0.0246(13) 0.0207(12) 0.0220(12) 0.0001(9) 0.0027(10) -0.0008(10) C12 0.0272(13) 0.0233(12) 0.0218(12) -0.0012(10) -0.0005(10) 0.0000(10) C13 0.0286(14) 0.0237(13) 0.0249(13) 0.0004(10) -0.0002(10) 0.0018(10) C14 0.0276(13) 0.0220(12) 0.0232(12) 0.0013(10) 0.0021(10) 0.0002(10) C15 0.0255(13) 0.0186(11) 0.0255(13) -0.0003(10) 0.0039(10) -0.0015(10) C16 0.0284(13) 0.0188(12) 0.0269(13) -0.0003(10) 0.0063(10) -0.0013(10) N4 0.0258(11) 0.0218(10) 0.0205(10) -0.0034(8) 0.0038(8) -0.0012(9) C17 0.0306(14) 0.0200(12) 0.0272(13) -0.0038(10) 0.0072(11) -0.0047(10) C18 0.0285(14) 0.0255(13) 0.0252(13) -0.0041(10) 0.0067(11) -0.0056(11) C19 0.0270(13) 0.0259(13) 0.0214(12) -0.0034(10) 0.0066(10) -0.0063(10) C20 0.0275(15) 0.0329(16) 0.0261(15) 0.0020(12) 0.0017(12) -0.0089(12) O2 0.0457(15) 0.0412(14) 0.0231(11) 0.0017(10) -0.0005(10) -0.0137(11) C21 0.0234(13) 0.0272(13) 0.0235(12) 0.0020(10) 0.0006(10) -0.0031(10) C22 0.0246(13) 0.0298(14) 0.0268(13) 0.0026(11) 0.0004(10) -0.0069(11) C23 0.0279(14) 0.0272(14) 0.0269(13) 0.0048(11) 0.0033(11) -0.0051(11) C24 0.0254(13) 0.0313(14) 0.0207(12) 0.0023(10) 0.0037(10) -0.0008(11) C25 0.0236(13) 0.0307(14) 0.0230(12) -0.0021(11) 0.0001(10) -0.0031(11) C26 0.0253(13) 0.0247(13) 0.0255(13) 0.0004(10) 0.0014(10) -0.0058(10) C27 0.0326(15) 0.0327(15) 0.0250(13) 0.0025(11) -0.0014(11) 0.0013(12) C28 0.0216(12) 0.0230(12) 0.0234(12) -0.0032(10) -0.0005(9) 0.0036(10) C29 0.054(2) 0.0384(18) 0.045(2) -0.0149(15) 0.0220(17) -0.0186(16) C30 0.044(2) 0.0390(19) 0.051(2) -0.0162(16) 0.0133(16) -0.0150(15) C31 0.0310(15) 0.0276(14) 0.0289(14) -0.0054(11) -0.0079(11) 0.0055(11) C32 0.068(3) 0.0395(18) 0.0228(14) -0.0068(13) 0.0084(15) -0.0137(17) C33 0.053(2) 0.0363(17) 0.0273(15) -0.0091(13) 0.0091(14) -0.0183(15) C34 0.0469(19) 0.0303(16) 0.0334(16) -0.0079(13) -0.0114(14) 0.0043(14) C35 0.0305(14) 0.0192(12) 0.0242(12) -0.0001(10) 0.0032(10) 0.0014(10) C36 0.0308(14) 0.0195(12) 0.0315(14) 0.0017(10) 0.0046(11) 0.0014(10) C37 0.0306(15) 0.0267(14) 0.0403(17) 0.0055(12) 0.0046(12) 0.0018(12) C38 0.0375(16) 0.0252(14) 0.0366(16) 0.0060(12) 0.0050(13) 0.0052(12) C39 0.0419(17) 0.0210(13) 0.0367(16) 0.0065(12) 0.0075(13) -0.0002(12) C40 0.0327(15) 0.0223(13) 0.0344(15) 0.0011(11) 0.0042(12) -0.0010(11) C41 0.048(2) 0.0345(18) 0.062(2) 0.0164(17) 0.0041(18) 0.0106(15) C42 0.0371(16) 0.0232(13) 0.0314(15) 0.0005(11) 0.0080(12) -0.0017(12) O3 0.0493(14) 0.0276(11) 0.0359(12) -0.0047(9) 0.0115(10) 0.0033(10) Re1' 0.02862(6) 0.02620(6) 0.01890(5) -0.00260(4) -0.00010(4) 0.00701(4) O1' 0.0322(11) 0.0310(11) 0.0235(10) 0.0006(8) -0.0015(8) 0.0064(9) C1' 0.0365(16) 0.0358(16) 0.0216(13) -0.0043(11) -0.0039(11) 0.0150(13) N1' 0.0348(13) 0.0327(13) 0.0184(10) -0.0015(9) 0.0011(9) 0.0107(10) C2' 0.0407(17) 0.0394(17) 0.0216(13) -0.0022(12) 0.0004(12) 0.0166(14) C3' 0.0379(16) 0.0386(16) 0.0225(13) 0.0028(12) 0.0047(12) 0.0191(13) C4' 0.0328(15) 0.0321(15) 0.0240(13) 0.0019(11) 0.0030(11) 0.0151(12) C5' 0.0307(14) 0.0323(15) 0.0244(13) 0.0036(11) 0.0052(11) 0.0131(12) C6' 0.0276(14) 0.0295(14) 0.0262(13) 0.0014(11) 0.0040(11) 0.0062(11) N2' 0.0280(12) 0.0262(11) 0.0224(11) 0.0001(9) 0.0034(9) 0.0061(9) C7' 0.0271(14) 0.0316(15) 0.0291(14) 0.0020(11) 0.0051(11) 0.0020(11) C8' 0.0303(14) 0.0273(14) 0.0284(14) -0.0023(11) 0.0055(11) 0.0027(11) C9' 0.0286(14) 0.0287(14) 0.0224(12) -0.0017(10) 0.0022(10) 0.0055(11) C10' 0.0307(14) 0.0248(13) 0.0220(12) -0.0031(10) 0.0027(10) 0.0033(11) C11' 0.0278(13) 0.0267(13) 0.0221(12) -0.0029(10) 0.0005(10) 0.0020(11) N3' 0.0292(12) 0.0261(11) 0.0217(11) -0.0035(9) 0.0025(9) 0.0024(9) C12' 0.0330(15) 0.0289(14) 0.0251(13) -0.0030(11) 0.0054(11) 0.0008(12) C13' 0.0314(15) 0.0292(14) 0.0292(14) -0.0014(11) 0.0036(11) -0.0004(12) C14' 0.0289(14) 0.0258(13) 0.0276(14) -0.0018(11) -0.0009(11) 0.0030(11) C15' 0.0327(15) 0.0250(13) 0.0285(14) -0.0038(11) -0.0042(11) 0.0048(11) C16' 0.0346(15) 0.0255(14) 0.0292(14) -0.0043(11) -0.0041(12) 0.0081(12) N4' 0.0313(13) 0.0274(12) 0.0228(11) -0.0061(9) -0.0034(9) 0.0044(10) C17' 0.0373(16) 0.0259(14) 0.0309(15) -0.0047(11) -0.0064(12) 0.0084(12) C18' 0.0380(16) 0.0318(15) 0.0272(14) -0.0082(12) -0.0071(12) 0.0117(13) C19' 0.0352(16) 0.0334(15) 0.0232(13) -0.0048(11) -0.0030(11) 0.0135(12) C20' 0.0340(17) 0.0327(16) 0.0265(15) 0.0046(12) 0.0018(12) 0.0083(13) O2' 0.0461(15) 0.0441(14) 0.0241(11) 0.0023(10) 0.0040(10) 0.0092(12) C21' 0.0312(15) 0.0379(16) 0.0239(13) 0.0025(12) 0.0047(11) 0.0105(12) C22' 0.0328(15) 0.0387(17) 0.0271(14) 0.0042(12) 0.0058(12) 0.0137(13) C23' 0.0335(16) 0.0363(16) 0.0276(14) 0.0050(12) 0.0012(12) 0.0089(13) C24' 0.0305(15) 0.0431(17) 0.0221(13) 0.0009(12) 0.0008(11) 0.0051(13) C25' 0.0294(15) 0.0440(18) 0.0261(14) -0.0030(13) 0.0043(11) 0.0084(13) C26' 0.0335(16) 0.0373(16) 0.0269(14) 0.0007(12) 0.0039(12) 0.0110(13) C27' 0.0355(17) 0.0469(19) 0.0272(15) 0.0050(13) 0.0030(12) 0.0022(14) C28' 0.0270(13) 0.0248(13) 0.0244(13) -0.0038(10) 0.0041(10) -0.0023(10) C29' 0.0330(15) 0.0294(14) 0.0256(13) 0.0004(11) 0.0049(11) 0.0020(12) C30' 0.0352(16) 0.0239(13) 0.0338(15) -0.0015(11) 0.0062(12) 0.0027(12) C31' 0.0295(14) 0.0290(14) 0.0280(14) -0.0079(11) 0.0059(11) -0.0051(11) C32' 0.0383(16) 0.0320(15) 0.0248(14) -0.0038(11) 0.0020(12) -0.0023(13) C33' 0.0352(15) 0.0267(14) 0.0261(14) -0.0016(11) 0.0008(11) -0.0008(12) C34' 0.0397(17) 0.0334(16) 0.0351(16) -0.0105(13) 0.0073(13) -0.0005(13) C35' 0.0363(16) 0.0257(14) 0.0271(14) -0.0037(11) -0.0037(12) 0.0018(12) C36' 0.0362(16) 0.0261(14) 0.0373(16) -0.0045(12) -0.0052(13) 0.0014(12) C37' 0.0337(17) 0.0346(17) 0.0453(19) -0.0060(14) -0.0028(14) -0.0031(13) C38' 0.046(2) 0.0312(16) 0.0422(18) -0.0027(14) -0.0036(15) -0.0054(14) C39' 0.0458(19) 0.0275(15) 0.0423(18) 0.0017(13) -0.0065(15) -0.0002(14) C40' 0.0378(17) 0.0287(15) 0.0374(17) -0.0013(12) -0.0054(13) 0.0035(13) C41' 0.054(2) 0.042(2) 0.072(3) 0.003(2) 0.002(2) -0.0153(18) C42' 0.050(2) 0.0269(15) 0.0354(17) -0.0021(12) -0.0083(14) 0.0078(14) O3' 0.0607(17) 0.0321(12) 0.0416(14) -0.0094(10) -0.0147(12) 0.0046(11) C1S 0.052(3) 0.086(4) 0.102(4) 0.035(3) -0.010(3) 0.008(3) C2S 0.073(3) 0.053(2) 0.048(2) 0.0106(19) 0.003(2) 0.009(2) C3S 0.062(3) 0.042(2) 0.0407(19) 0.0078(16) 0.0030(17) -0.0018(18) C4S 0.065(3) 0.056(3) 0.055(3) 0.010(2) -0.006(2) -0.005(2) C5S 0.064(3) 0.068(3) 0.071(3) 0.008(3) -0.013(2) 0.001(2) C6S 0.061(3) 0.083(4) 0.059(3) -0.004(3) -0.011(2) 0.012(3) _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 Re1 O1 1.681(2) . ? Re1 N4 1.999(2) . ? Re1 N1 2.007(2) . ? Re1 N2 2.012(2) . ? Re1 N3 2.013(2) . ? C1 N1 1.391(3) . ? C1 C2 1.392(4) . ? C1 C19 1.405(4) . ? N1 C4 1.378(4) . ? C2 C3 1.399(4) . ? C2 C20A 1.463(8) . ? C2 H2B 0.9500 . ? C3 C4 1.432(4) . ? C3 C20 1.469(4) . ? C3 H3A 0.9500 . ? C4 C5 1.408(4) . ? C5 C6 1.403(4) . ? C5 C21 1.489(4) . ? C6 N2 1.407(4) . ? C6 C7 1.429(4) . ? N2 C9 1.388(3) . ? C7 C8 1.359(4) . ? C7 H7A 0.9500 . ? C8 C9 1.427(4) . ? C8 H8A 0.9500 . ? C9 C10 1.400(4) . ? C10 C11 1.389(4) . ? C10 C28 1.493(4) . ? N3 C11 1.395(3) . ? N3 C14 1.401(4) . ? C11 C12 1.425(4) . ? C12 C13 1.363(4) . ? C12 H12A 0.9500 . ? C13 C14 1.429(4) . ? C13 H13A 0.9500 . ? C14 C15 1.404(4) . ? C15 C16 1.402(4) . ? C15 C35 1.490(4) . ? C16 N4 1.377(4) . ? C16 C17 1.440(4) . ? N4 C19 1.393(3) . ? C17 C18 1.392(4) . ? C17 C42 1.462(4) . ? C18 C19 1.394(4) . ? C18 H18A 0.9500 . ? C20 O2 1.224(4) . ? C20 H20A 0.9500 . ? C20A O2A 1.229(9) . ? C20A H2A 0.9500 . ? C21 C22 1.395(4) . ? C21 C26 1.400(4) . ? C22 C23 1.390(4) . ? C22 H22A 0.9500 . ? C23 C24 1.393(4) . ? C23 H23A 0.9500 . ? C24 C25 1.390(4) . ? C24 C27 1.498(4) . ? C25 C26 1.383(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.372(4) . ? C28 C33 1.377(4) . ? C29 C30 1.390(5) . ? C29 H29A 0.9500 . ? C30 C31 1.363(5) . ? C30 H30A 0.9500 . ? C31 C32 1.374(5) . ? C31 C34 1.515(4) . ? C32 C33 1.390(4) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.392(4) . ? C35 C40 1.398(4) . ? C36 C37 1.385(4) . ? C36 H36A 0.9500 . ? C37 C38 1.400(4) . ? C37 H37A 0.9500 . ? C38 C39 1.391(5) . ? C38 C41 1.511(5) . ? C39 C40 1.388(4) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 O3 1.214(4) . ? C42 H42A 0.9500 . ? Re1' O1' 1.685(2) . ? Re1' N1' 1.999(2) . ? Re1' N4' 2.000(2) . ? Re1' N3' 2.013(2) . ? Re1' N2' 2.016(2) . ? C1' N1' 1.394(4) . ? C1' C2' 1.394(4) . ? C1' C19' 1.401(5) . ? N1' C4' 1.378(4) . ? C2' C3' 1.393(5) . ? C2' C20" 1.466(8) . ? C2' H2'B 0.9500 . ? C3' C4' 1.437(4) . ? C3' C20' 1.462(4) . ? C3' H3'A 0.9500 . ? C4' C5' 1.411(5) . ? C5' C6' 1.404(4) . ? C5' C21' 1.485(4) . ? C6' N2' 1.405(4) . ? C6' C7' 1.430(4) . ? N2' C9' 1.392(3) . ? C7' C8' 1.364(4) . ? C7' H7'A 0.9500 . ? C8' C9' 1.423(4) . ? C8' H8'A 0.9500 . ? C9' C10' 1.396(4) . ? C10' C11' 1.396(4) . ? C10' C28' 1.492(4) . ? C11' N3' 1.397(3) . ? C11' C12' 1.427(4) . ? N3' C14' 1.402(4) . ? C12' C13' 1.361(4) . ? C12' H12B 0.9500 . ? C13' C14' 1.426(4) . ? C13' H13B 0.9500 . ? C14' C15' 1.400(4) . ? C15' C16' 1.407(4) . ? C15' C35' 1.489(5) . ? C16' N4' 1.376(4) . ? C16' C17' 1.435(4) . ? N4' C19' 1.388(4) . ? C17' C18' 1.394(5) . ? C17' C42' 1.463(5) . ? C18' C19' 1.392(5) . ? C18' H18B 0.9500 . ? C20' O2' 1.221(4) . ? C20' H20B 0.9500 . ? C20" O2" 1.232(9) . ? C20" H2'A 0.9500 . ? C21' C22' 1.388(4) . ? C21' C26' 1.402(4) . ? C22' C23' 1.383(5) . ? C22' H22B 0.9500 . ? C23' C24' 1.394(4) . ? C23' H23B 0.9500 . ? C24' C25' 1.387(5) . ? C24' C27' 1.508(5) . ? C25' C26' 1.383(5) . ? C25' H25B 0.9500 . ? C26' H26B 0.9500 . ? C27' H27D 0.9800 . ? C27' H27E 0.9800 . ? C27' H27F 0.9800 . ? C28' C29' 1.392(4) . ? C28' C33' 1.395(4) . ? C29' C30' 1.391(4) . ? C29' H29B 0.9500 . ? C30' C31' 1.389(4) . ? C30' H30B 0.9500 . ? C31' C32' 1.388(5) . ? C31' C34' 1.506(4) . ? C32' C33' 1.395(4) . ? C32' H32B 0.9500 . ? C33' H33B 0.9500 . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35' C36' 1.393(5) . ? C35' C40' 1.395(4) . ? C36' C37' 1.385(5) . ? C36' H36B 0.9500 . ? C37' C38' 1.401(5) . ? C37' H37B 0.9500 . ? C38' C39' 1.388(5) . ? C38' C41' 1.511(5) . ? C39' C40' 1.389(5) . ? C39' H39B 0.9500 . ? C40' H40B 0.9500 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42' O3' 1.225(4) . ? C42' H42B 0.9500 . ? C1S C2S 1.538(7) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S C3S 1.531(6) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S C4S 1.509(6) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S C5S 1.511(6) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? C5S C6S 1.486(7) . ? C5S H5SA 0.9900 . ? C5S H5SB 0.9900 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? 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 O1 Re1 N4 111.05(10) . . ? O1 Re1 N1 112.14(10) . . ? N4 Re1 N1 76.37(10) . . ? O1 Re1 N2 109.78(9) . . ? N4 Re1 N2 138.80(9) . . ? N1 Re1 N2 83.59(9) . . ? O1 Re1 N3 109.54(10) . . ? N4 Re1 N3 83.55(9) . . ? N1 Re1 N3 137.89(9) . . ? N2 Re1 N3 88.04(9) . . ? N1 C1 C2 108.6(3) . . ? N1 C1 C19 112.7(2) . . ? C2 C1 C19 138.1(3) . . ? C4 N1 C1 109.1(2) . . ? C4 N1 Re1 133.26(18) . . ? C1 N1 Re1 117.62(19) . . ? C1 C2 C3 107.7(2) . . ? C1 C2 C20A 129.6(7) . . ? C3 C2 C20A 122.7(7) . . ? C1 C2 H2B 126.2 . . ? C3 C2 H2B 126.2 . . ? C2 C3 C4 107.6(2) . . ? C2 C3 C20 120.6(3) . . ? C4 C3 C20 130.9(3) . . ? C2 C3 H3A 126.2 . . ? C4 C3 H3A 126.2 . . ? N1 C4 C5 120.8(2) . . ? N1 C4 C3 107.1(2) . . ? C5 C4 C3 131.9(3) . . ? C6 C5 C4 121.8(3) . . ? C6 C5 C21 120.4(3) . . ? C4 C5 C21 117.7(2) . . ? C5 C6 N2 125.7(2) . . ? C5 C6 C7 127.0(3) . . ? N2 C6 C7 107.1(2) . . ? C9 N2 C6 107.6(2) . . ? C9 N2 Re1 124.07(18) . . ? C6 N2 Re1 125.49(18) . . ? C8 C7 C6 108.9(3) . . ? C8 C7 H7A 125.5 . . ? C6 C7 H7A 125.5 . . ? C7 C8 C9 107.6(2) . . ? C7 C8 H8A 126.2 . . ? C9 C8 H8A 126.2 . . ? N2 C9 C10 125.0(2) . . ? N2 C9 C8 108.6(2) . . ? C10 C9 C8 126.4(2) . . ? C11 C10 C9 124.0(2) . . ? C11 C10 C28 118.0(2) . . ? C9 C10 C28 118.0(2) . . ? C11 N3 C14 107.2(2) . . ? C11 N3 Re1 125.09(18) . . ? C14 N3 Re1 125.84(18) . . ? C10 C11 N3 124.7(2) . . ? C10 C11 C12 126.7(2) . . ? N3 C11 C12 108.6(2) . . ? C13 C12 C11 107.9(2) . . ? C13 C12 H12A 126.0 . . ? C11 C12 H12A 126.0 . . ? C12 C13 C14 108.3(3) . . ? C12 C13 H13A 125.9 . . ? C14 C13 H13A 125.9 . . ? N3 C14 C15 125.9(3) . . ? N3 C14 C13 108.0(2) . . ? C15 C14 C13 126.0(3) . . ? C16 C15 C14 122.1(3) . . ? C16 C15 C35 118.8(2) . . ? C14 C15 C35 119.1(2) . . ? N4 C16 C15 120.5(2) . . ? N4 C16 C17 106.4(2) . . ? C15 C16 C17 132.7(3) . . ? C16 N4 C19 109.5(2) . . ? C16 N4 Re1 132.25(18) . . ? C19 N4 Re1 117.66(19) . . ? C18 C17 C16 108.0(3) . . ? C18 C17 C42 122.0(3) . . ? C16 C17 C42 129.7(3) . . ? C17 C18 C19 107.7(2) . . ? C17 C18 H18A 126.1 . . ? C19 C18 H18A 126.1 . . ? N4 C19 C18 108.3(3) . . ? N4 C19 C1 112.6(2) . . ? C18 C19 C1 138.9(3) . . ? O2 C20 C3 122.3(3) . . ? O2 C20 H20A 118.8 . . ? C3 C20 H20A 118.8 . . ? O2A C20A C2 114.2(17) . . ? O2A C20A H2A 122.9 . . ? C2 C20A H2A 122.9 . . ? C22 C21 C26 117.8(3) . . ? C22 C21 C5 122.4(3) . . ? C26 C21 C5 119.7(3) . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 121.1(3) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C25 C24 C23 117.7(3) . . ? C25 C24 C27 121.9(3) . . ? C23 C24 C27 120.4(3) . . ? C26 C25 C24 121.6(3) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C25 C26 C21 120.7(3) . . ? C25 C26 H26A 119.7 . . ? C21 C26 H26A 119.7 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.0(3) . . ? C29 C28 C10 120.9(3) . . ? C33 C28 C10 121.0(3) . . ? C28 C29 C30 120.7(3) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C31 C30 C29 121.8(3) . . ? C31 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? C30 C31 C32 117.3(3) . . ? C30 C31 C34 121.3(3) . . ? C32 C31 C34 121.4(3) . . ? C31 C32 C33 121.6(3) . . ? C31 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C28 C33 C32 120.5(3) . . ? C28 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 118.7(3) . . ? C36 C35 C15 122.7(2) . . ? C40 C35 C15 118.5(3) . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C38 121.1(3) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C39 C38 C37 118.0(3) . . ? C39 C38 C41 121.0(3) . . ? C37 C38 C41 121.0(3) . . ? C40 C39 C38 121.2(3) . . ? C40 C39 H39A 119.4 . . ? C38 C39 H39A 119.4 . . ? C39 C40 C35 120.4(3) . . ? C39 C40 H40A 119.8 . . ? C35 C40 H40A 119.8 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 C17 122.4(3) . . ? O3 C42 H42A 118.8 . . ? C17 C42 H42A 118.8 . . ? O1' Re1' N1' 111.17(10) . . ? O1' Re1' N4' 110.76(10) . . ? N1' Re1' N4' 76.25(11) . . ? O1' Re1' N3' 109.87(10) . . ? N1' Re1' N3' 138.49(10) . . ? N4' Re1' N3' 83.83(10) . . ? O1' Re1' N2' 110.49(10) . . ? N1' Re1' N2' 83.75(10) . . ? N4' Re1' N2' 138.33(10) . . ? N3' Re1' N2' 87.78(10) . . ? N1' C1' C2' 108.6(3) . . ? N1' C1' C19' 113.0(3) . . ? C2' C1' C19' 137.9(3) . . ? C4' N1' C1' 109.4(2) . . ? C4' N1' Re1' 133.0(2) . . ? C1' N1' Re1' 117.6(2) . . ? C3' C2' C1' 107.3(3) . . ? C3' C2' C20" 123.3(9) . . ? C1' C2' C20" 129.2(10) . . ? C3' C2' H2'B 126.4 . . ? C1' C2' H2'B 126.4 . . ? C2' C3' C4' 108.5(3) . . ? C2' C3' C20' 120.8(3) . . ? C4' C3' C20' 129.9(3) . . ? C2' C3' H3'A 125.8 . . ? C4' C3' H3'A 125.8 . . ? N1' C4' C5' 121.0(3) . . ? N1' C4' C3' 106.3(3) . . ? C5' C4' C3' 132.6(3) . . ? C6' C5' C4' 121.4(3) . . ? C6' C5' C21' 120.4(3) . . ? C4' C5' C21' 118.0(3) . . ? C5' C6' N2' 125.9(3) . . ? C5' C6' C7' 126.5(3) . . ? N2' C6' C7' 107.3(2) . . ? C9' N2' C6' 107.7(2) . . ? C9' N2' Re1' 124.8(2) . . ? C6' N2' Re1' 124.61(18) . . ? C8' C7' C6' 108.5(3) . . ? C8' C7' H7'A 125.8 . . ? C6' C7' H7'A 125.8 . . ? C7' C8' C9' 108.0(3) . . ? C7' C8' H8'A 126.0 . . ? C9' C8' H8'A 126.0 . . ? N2' C9' C10' 125.1(3) . . ? N2' C9' C8' 108.4(2) . . ? C10' C9' C8' 126.5(3) . . ? C11' C10' C9' 123.8(3) . . ? C11' C10' C28' 117.7(3) . . ? C9' C10' C28' 118.3(3) . . ? C10' C11' N3' 124.6(3) . . ? C10' C11' C12' 127.3(3) . . ? N3' C11' C12' 108.0(3) . . ? C11' N3' C14' 107.4(2) . . ? C11' N3' Re1' 126.0(2) . . ? C14' N3' Re1' 125.06(19) . . ? C13' C12' C11' 108.3(3) . . ? C13' C12' H12B 125.8 . . ? C11' C12' H12B 125.8 . . ? C12' C13' C14' 108.2(3) . . ? C12' C13' H13B 125.9 . . ? C14' C13' H13B 125.9 . . ? C15' C14' N3' 126.6(3) . . ? C15' C14' C13' 125.3(3) . . ? N3' C14' C13' 107.9(2) . . ? C14' C15' C16' 122.0(3) . . ? C14' C15' C35' 118.9(3) . . ? C16' C15' C35' 119.1(3) . . ? N4' C16' C15' 120.4(3) . . ? N4' C16' C17' 107.0(3) . . ? C15' C16' C17' 132.2(3) . . ? C16' N4' C19' 108.9(3) . . ? C16' N4' Re1' 132.4(2) . . ? C19' N4' Re1' 118.1(2) . . ? C18' C17' C16' 107.6(3) . . ? C18' C17' C42' 122.2(3) . . ? C16' C17' C42' 129.8(3) . . ? C19' C18' C17' 107.6(3) . . ? C19' C18' H18B 126.2 . . ? C17' C18' H18B 126.2 . . ? N4' C19' C18' 108.8(3) . . ? N4' C19' C1' 112.1(3) . . ? C18' C19' C1' 138.8(3) . . ? O2' C20' C3' 122.1(3) . . ? O2' C20' H20B 118.9 . . ? C3' C20' H20B 118.9 . . ? O2" C20" C2' 103(3) . . ? O2" C20" H2'A 128.3 . . ? C2' C20" H2'A 128.3 . . ? C22' C21' C26' 117.4(3) . . ? C22' C21' C5' 122.8(3) . . ? C26' C21' C5' 119.6(3) . . ? C23' C22' C21' 121.3(3) . . ? C23' C22' H22B 119.4 . . ? C21' C22' H22B 119.4 . . ? C22' C23' C24' 121.3(3) . . ? C22' C23' H23B 119.3 . . ? C24' C23' H23B 119.3 . . ? C25' C24' C23' 117.5(3) . . ? C25' C24' C27' 121.6(3) . . ? C23' C24' C27' 120.9(3) . . ? C26' C25' C24' 121.3(3) . . ? C26' C25' H25B 119.3 . . ? C24' C25' H25B 119.3 . . ? C25' C26' C21' 121.0(3) . . ? C25' C26' H26B 119.5 . . ? C21' C26' H26B 119.5 . . ? C24' C27' H27D 109.5 . . ? C24' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C24' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C29' C28' C33' 118.0(3) . . ? C29' C28' C10' 119.9(3) . . ? C33' C28' C10' 122.0(3) . . ? C30' C29' C28' 121.0(3) . . ? C30' C29' H29B 119.5 . . ? C28' C29' H29B 119.5 . . ? C31' C30' C29' 121.2(3) . . ? C31' C30' H30B 119.4 . . ? C29' C30' H30B 119.4 . . ? C32' C31' C30' 117.8(3) . . ? C32' C31' C34' 121.4(3) . . ? C30' C31' C34' 120.8(3) . . ? C31' C32' C33' 121.5(3) . . ? C31' C32' H32B 119.3 . . ? C33' C32' H32B 119.3 . . ? C28' C33' C32' 120.5(3) . . ? C28' C33' H33B 119.8 . . ? C32' C33' H33B 119.8 . . ? C31' C34' H34D 109.5 . . ? C31' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C31' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C36' C35' C40' 118.8(3) . . ? C36' C35' C15' 121.9(3) . . ? C40' C35' C15' 119.2(3) . . ? C37' C36' C35' 120.6(3) . . ? C37' C36' H36B 119.7 . . ? C35' C36' H36B 119.7 . . ? C36' C37' C38' 121.0(3) . . ? C36' C37' H37B 119.5 . . ? C38' C37' H37B 119.5 . . ? C39' C38' C37' 117.9(3) . . ? C39' C38' C41' 121.2(3) . . ? C37' C38' C41' 120.9(4) . . ? C38' C39' C40' 121.5(3) . . ? C38' C39' H39B 119.2 . . ? C40' C39' H39B 119.2 . . ? C39' C40' C35' 120.1(3) . . ? C39' C40' H40B 119.9 . . ? C35' C40' H40B 119.9 . . ? C38' C41' H41D 109.5 . . ? C38' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C38' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? O3' C42' C17' 122.1(4) . . ? O3' C42' H42B 119.0 . . ? C17' C42' H42B 119.0 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C3S C2S C1S 113.0(4) . . ? C3S C2S H2SA 109.0 . . ? C1S C2S H2SA 109.0 . . ? C3S C2S H2SB 109.0 . . ? C1S C2S H2SB 109.0 . . ? H2SA C2S H2SB 107.8 . . ? C4S C3S C2S 115.6(4) . . ? C4S C3S H3SA 108.4 . . ? C2S C3S H3SA 108.4 . . ? C4S C3S H3SB 108.4 . . ? C2S C3S H3SB 108.4 . . ? H3SA C3S H3SB 107.4 . . ? C3S C4S C5S 114.3(4) . . ? C3S C4S H4SA 108.7 . . ? C5S C4S H4SA 108.7 . . ? C3S C4S H4SB 108.7 . . ? C5S C4S H4SB 108.7 . . ? H4SA C4S H4SB 107.6 . . ? C6S C5S C4S 114.9(4) . . ? C6S C5S H5SA 108.6 . . ? C4S C5S H5SA 108.6 . . ? C6S C5S H5SB 108.6 . . ? C4S C5S H5SB 108.6 . . ? H5SA C5S H5SB 107.5 . . ? C5S C6S H6SA 109.5 . . ? C5S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? _refine_diff_density_max 2.379 _refine_diff_density_min -2.218 _refine_diff_density_rms 0.103 _shelx_res_file ; TITL Bi_CHO_DCMHex_a.res in P-1 Bi_CHO_DCMHex_a.res created by SHELXL-2018/1 at 05:20:21 on 19-Jul-2019 REM Old TITL Bi_CHO_DCMhex in P-1 REM SHELXT solution in P-1 REM R1 0.584, Rweak 0.074, Alpha 0.166, Orientation as input REM Formula found by SHELXT: C285 N82 O12 Re6 CELL 0.7288 9.5807 12.6649 29.1467 95.279 91.627 90.341 ZERR 4.000 0.0004 0.0006 0.0013 0.002 0.002 0.002 LATT 1 SFAC C H N O RE DISP C 0.00337 0.00172 11.92 DISP H 0.00000 0.00000 0.67 DISP N 0.00654 0.00351 20.58 DISP O 0.01151 0.00644 34.18 DISP Re -1.06252 7.56058 31875.07 UNIT 180 144 16 12 4 ACTA OMIT -2 2 0 OMIT 0 -1 2 TEMP -173 SIZE 0.230 0.080 0.020 REM dark green plates L.S. 10 BOND $H FMAP 2 PLAN 20 SADI 0.01 C2 C20a C3 C20 C2' C20" C3' C20' SADI 0.01 C20 O2 C20a O2a C20' O2' C20" o2" SADI 0.02 C1 C20a C3 C20a C2 C20 C4 C20 C1' C20" C3' C20" C2' C20' C4' C20' WGHT 0.010900 8.911301 FVAR 0.07270 0.91753 RE1 5 0.541634 0.199343 0.582853 11.00000 0.02278 0.01993 = 0.01852 -0.00161 0.00360 -0.00329 O1 4 0.418129 0.130449 0.607413 11.00000 0.02892 0.02794 = 0.02376 -0.00076 0.00415 -0.00369 C1 1 0.545398 0.142108 0.483402 11.00000 0.02708 0.02490 = 0.02164 -0.00270 0.00525 -0.00757 N1 3 0.494384 0.217036 0.516493 11.00000 0.02487 0.02493 = 0.01707 -0.00054 0.00160 -0.00373 C2 1 0.493399 0.164292 0.440283 11.00000 0.03024 0.03097 = 0.01998 -0.00150 0.00331 -0.00944 AFIX 43 PART 1 H2B 2 0.510116 0.124603 0.411729 21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.412094 0.255563 0.446584 11.00000 0.02739 0.02895 = 0.02346 0.00112 0.00050 -0.00984 AFIX 43 PART 2 H3A 2 0.364755 0.289680 0.423041 -21.00000 -1.20000 AFIX 0 PART 0 C4 1 0.413137 0.288265 0.494953 11.00000 0.02423 0.02507 = 0.02306 0.00110 0.00022 -0.00756 C5 1 0.358144 0.377950 0.520112 11.00000 0.02225 0.02598 = 0.02436 0.00193 -0.00038 -0.00498 C6 1 0.401707 0.408628 0.565781 11.00000 0.02135 0.02414 = 0.02473 0.00121 0.00117 -0.00272 N2 3 0.499999 0.355290 0.591822 11.00000 0.02251 0.01832 = 0.02231 -0.00039 0.00150 -0.00166 C7 1 0.365130 0.503384 0.593095 11.00000 0.02359 0.02606 = 0.02870 0.00057 0.00069 0.00185 AFIX 43 H7A 2 0.297703 0.553346 0.584668 11.00000 -1.20000 AFIX 0 C8 1 0.442486 0.510414 0.633092 11.00000 0.02406 0.02241 = 0.02799 -0.00137 0.00081 0.00086 AFIX 43 H8A 2 0.439686 0.566236 0.657155 11.00000 -1.20000 AFIX 0 C9 1 0.528666 0.418809 0.632415 11.00000 0.02160 0.02169 = 0.02275 -0.00188 0.00302 -0.00199 C10 1 0.628994 0.396956 0.666042 11.00000 0.02409 0.02093 = 0.02069 -0.00296 0.00208 -0.00232 N3 3 0.705500 0.226717 0.627214 11.00000 0.02242 0.02115 = 0.02164 -0.00228 0.00071 -0.00133 C11 1 0.714283 0.308408 0.662750 11.00000 0.02462 0.02067 = 0.02203 0.00005 0.00275 -0.00076 C12 1 0.824590 0.285492 0.694021 11.00000 0.02719 0.02334 = 0.02175 -0.00116 -0.00051 0.00002 AFIX 43 H12A 2 0.852851 0.328056 0.721283 11.00000 -1.20000 AFIX 0 C13 1 0.882421 0.191715 0.677921 11.00000 0.02858 0.02370 = 0.02487 0.00041 -0.00019 0.00178 AFIX 43 H13A 2 0.957344 0.157108 0.692262 11.00000 -1.20000 AFIX 0 C14 1 0.811035 0.154371 0.635769 11.00000 0.02759 0.02205 = 0.02316 0.00125 0.00210 0.00021 C15 1 0.845162 0.064000 0.606790 11.00000 0.02551 0.01857 = 0.02551 -0.00029 0.00391 -0.00151 C16 1 0.783147 0.041865 0.562787 11.00000 0.02844 0.01875 = 0.02692 -0.00025 0.00625 -0.00131 N4 3 0.674012 0.102162 0.548407 11.00000 0.02579 0.02183 = 0.02045 -0.00342 0.00377 -0.00123 C17 1 0.818976 -0.029296 0.523564 11.00000 0.03057 0.01999 = 0.02719 -0.00378 0.00720 -0.00474 C18 1 0.734111 -0.006270 0.486306 11.00000 0.02853 0.02553 = 0.02523 -0.00413 0.00673 -0.00562 AFIX 43 H18A 2 0.736193 -0.040276 0.455893 11.00000 -1.20000 AFIX 0 C19 1 0.645501 0.075641 0.501615 11.00000 0.02697 0.02593 = 0.02136 -0.00340 0.00661 -0.00634 PART 1 C20 1 0.362662 0.309832 0.406832 21.00000 0.02751 0.03288 = 0.02610 0.00201 0.00167 -0.00893 AFIX 43 H20A 2 0.331321 0.380869 0.411862 21.00000 -1.20000 AFIX 0 O2 4 0.360431 0.266765 0.367470 21.00000 0.04568 0.04118 = 0.02308 0.00167 -0.00046 -0.01369 PART 2 C20A 1 0.515967 0.108884 0.394859 -21.00000 0.02308 AFIX 43 H2A 2 0.572031 0.047370 0.390440 -21.00000 -1.20000 AFIX 0 O2A 4 0.456182 0.148731 0.362898 -21.00000 0.03754 PART 0 C21 1 0.258378 0.444493 0.495592 11.00000 0.02336 0.02720 = 0.02352 0.00198 0.00065 -0.00310 C22 1 0.281595 0.552343 0.492364 11.00000 0.02460 0.02983 = 0.02682 0.00257 0.00042 -0.00688 AFIX 43 H22A 2 0.359350 0.586668 0.508447 11.00000 -1.20000 AFIX 0 C23 1 0.192639 0.610361 0.465959 11.00000 0.02794 0.02718 = 0.02685 0.00478 0.00325 -0.00506 AFIX 43 H23A 2 0.209216 0.684114 0.464897 11.00000 -1.20000 AFIX 0 C24 1 0.079560 0.562067 0.441027 11.00000 0.02543 0.03132 = 0.02071 0.00227 0.00369 -0.00078 C25 1 0.054921 0.455119 0.445210 11.00000 0.02358 0.03073 = 0.02297 -0.00214 0.00009 -0.00305 AFIX 43 H25A 2 -0.022727 0.420884 0.429027 11.00000 -1.20000 AFIX 0 C26 1 0.140708 0.397349 0.472359 11.00000 0.02532 0.02470 = 0.02554 0.00043 0.00139 -0.00578 AFIX 43 H26A 2 0.119556 0.324932 0.475268 11.00000 -1.20000 AFIX 0 C27 1 -0.010533 0.624339 0.410671 11.00000 0.03264 0.03269 = 0.02500 0.00247 -0.00137 0.00129 AFIX 137 H27A 2 -0.018106 0.697356 0.424693 11.00000 -1.50000 H27B 2 -0.103715 0.591778 0.407073 11.00000 -1.50000 H27C 2 0.031270 0.624630 0.380383 11.00000 -1.50000 AFIX 0 C28 1 0.649208 0.475620 0.707140 11.00000 0.02162 0.02303 = 0.02336 -0.00324 -0.00049 0.00364 C29 1 0.745984 0.556012 0.707455 11.00000 0.05368 0.03843 = 0.04517 -0.01492 0.02199 -0.01859 AFIX 43 H29A 2 0.800268 0.562309 0.681054 11.00000 -1.20000 AFIX 0 C30 1 0.765436 0.628343 0.746000 11.00000 0.04422 0.03902 = 0.05147 -0.01624 0.01331 -0.01500 AFIX 43 H30A 2 0.834562 0.682322 0.745621 11.00000 -1.20000 AFIX 0 C31 1 0.688066 0.623952 0.784318 11.00000 0.03100 0.02760 = 0.02890 -0.00545 -0.00792 0.00553 C32 1 0.592244 0.542749 0.784073 11.00000 0.06817 0.03952 = 0.02283 -0.00681 0.00838 -0.01373 AFIX 43 H32A 2 0.538243 0.536792 0.810565 11.00000 -1.20000 AFIX 0 C33 1 0.572354 0.469076 0.746011 11.00000 0.05307 0.03628 = 0.02727 -0.00910 0.00907 -0.01829 AFIX 43 H33A 2 0.505244 0.413807 0.746825 11.00000 -1.20000 AFIX 0 C34 1 0.708035 0.704692 0.825692 11.00000 0.04688 0.03029 = 0.03339 -0.00787 -0.01139 0.00427 AFIX 137 H34A 2 0.618778 0.738969 0.832783 11.00000 -1.50000 H34B 2 0.776574 0.758320 0.818784 11.00000 -1.50000 H34C 2 0.741675 0.669025 0.852279 11.00000 -1.50000 AFIX 0 C35 1 0.952993 -0.009632 0.622799 11.00000 0.03048 0.01916 = 0.02424 -0.00009 0.00316 0.00143 C36 1 1.094112 0.017387 0.627346 11.00000 0.03080 0.01951 = 0.03151 0.00173 0.00461 0.00137 AFIX 43 H36A 2 1.124111 0.086218 0.621250 11.00000 -1.20000 AFIX 0 C37 1 1.191083 -0.055341 0.640690 11.00000 0.03064 0.02667 = 0.04031 0.00553 0.00460 0.00180 AFIX 43 H37A 2 1.287017 -0.035725 0.643515 11.00000 -1.20000 AFIX 0 C38 1 1.150177 -0.157244 0.650086 11.00000 0.03753 0.02518 = 0.03663 0.00603 0.00504 0.00524 C39 1 1.008965 -0.183470 0.645684 11.00000 0.04190 0.02102 = 0.03673 0.00650 0.00752 -0.00022 AFIX 43 H39A 2 0.978908 -0.252115 0.652023 11.00000 -1.20000 AFIX 0 C40 1 0.911169 -0.111202 0.632203 11.00000 0.03274 0.02232 = 0.03439 0.00112 0.00419 -0.00101 AFIX 43 H40A 2 0.815246 -0.130842 0.629345 11.00000 -1.20000 AFIX 0 C41 1 1.256178 -0.236150 0.664910 11.00000 0.04764 0.03445 = 0.06172 0.01635 0.00412 0.01055 AFIX 137 H41A 2 1.215395 -0.307662 0.660850 11.00000 -1.50000 H41B 2 1.282880 -0.218477 0.697429 11.00000 -1.50000 H41C 2 1.339007 -0.233483 0.646066 11.00000 -1.50000 AFIX 0 C42 1 0.931450 -0.106654 0.518653 11.00000 0.03715 0.02316 = 0.03136 0.00050 0.00799 -0.00173 AFIX 43 H42A 2 0.993398 -0.113630 0.544209 11.00000 -1.20000 AFIX 0 O3 4 0.948565 -0.162289 0.483116 11.00000 0.04934 0.02758 = 0.03592 -0.00467 0.01153 0.00327 RE1' 5 0.039666 0.813650 0.914385 11.00000 0.02862 0.02620 = 0.01890 -0.00260 -0.00010 0.00701 O1' 4 -0.090343 0.882019 0.890991 11.00000 0.03221 0.03101 = 0.02350 0.00060 -0.00153 0.00639 C1' 1 0.064364 0.871007 1.013599 11.00000 0.03648 0.03579 = 0.02162 -0.00433 -0.00388 0.01498 N1' 3 0.005965 0.795701 0.980584 11.00000 0.03476 0.03265 = 0.01840 -0.00152 0.00105 0.01069 C2' 1 0.019882 0.849125 1.056883 11.00000 0.04075 0.03939 = 0.02161 -0.00215 0.00041 0.01660 AFIX 43 PART 1 10.93 H2'B 2 0.041512 0.889245 1.085384 10.93000 -1.20000 AFIX 0 PART 0 C3' 1 -0.062172 0.757502 1.050571 11.00000 0.03793 0.03856 = 0.02249 0.00283 0.00466 0.01906 AFIX 43 PART 2 10.07 H3'A 2 -0.104655 0.723085 1.074281 10.07000 -1.20000 AFIX 0 PART 0 C4' 1 -0.071701 0.723835 1.002125 11.00000 0.03282 0.03209 = 0.02396 0.00186 0.00304 0.01506 C5' 1 -0.132614 0.633903 0.976927 11.00000 0.03072 0.03230 = 0.02442 0.00361 0.00516 0.01312 C6' 1 -0.096356 0.603533 0.931314 11.00000 0.02756 0.02946 = 0.02615 0.00142 0.00398 0.00619 N2' 3 -0.001266 0.656631 0.905454 11.00000 0.02804 0.02621 = 0.02243 0.00008 0.00341 0.00607 C7' 1 -0.138524 0.508279 0.904168 11.00000 0.02712 0.03165 = 0.02912 0.00200 0.00506 0.00198 AFIX 43 H7'A 2 -0.206224 0.458717 0.912320 11.00000 -1.20000 AFIX 0 C8' 1 -0.065115 0.500597 0.864590 11.00000 0.03030 0.02727 = 0.02841 -0.00232 0.00547 0.00274 AFIX 43 H8'A 2 -0.071395 0.444192 0.840751 11.00000 -1.20000 AFIX 0 C9' 1 0.022510 0.591878 0.865270 11.00000 0.02863 0.02870 = 0.02244 -0.00171 0.00217 0.00549 C10' 1 0.118254 0.613322 0.832029 11.00000 0.03066 0.02481 = 0.02204 -0.00312 0.00266 0.00335 C11' 1 0.199287 0.705734 0.834187 11.00000 0.02782 0.02674 = 0.02213 -0.00292 0.00054 0.00201 N3' 3 0.193511 0.788716 0.869130 11.00000 0.02921 0.02612 = 0.02171 -0.00353 0.00249 0.00235 C12' 1 0.302811 0.731986 0.802792 11.00000 0.03300 0.02893 = 0.02514 -0.00298 0.00542 0.00076 AFIX 43 H12B 2 0.328557 0.689408 0.775860 11.00000 -1.20000 AFIX 0 C13' 1 0.358374 0.828442 0.818018 11.00000 0.03136 0.02919 = 0.02921 -0.00142 0.00363 -0.00040 AFIX 43 H13B 2 0.427438 0.865780 0.803047 11.00000 -1.20000 AFIX 0 C14' 1 0.295038 0.863799 0.860326 11.00000 0.02891 0.02582 = 0.02760 -0.00182 -0.00094 0.00305 C15' 1 0.336608 0.953169 0.889478 11.00000 0.03268 0.02503 = 0.02852 -0.00377 -0.00422 0.00477 C16' 1 0.285311 0.973210 0.934162 11.00000 0.03464 0.02551 = 0.02921 -0.00432 -0.00406 0.00806 N4' 3 0.178580 0.912217 0.948590 11.00000 0.03130 0.02741 = 0.02275 -0.00607 -0.00341 0.00442 C17' 1 0.332275 1.042647 0.973313 11.00000 0.03732 0.02592 = 0.03086 -0.00468 -0.00643 0.00840 C18' 1 0.253642 1.019653 1.010713 11.00000 0.03796 0.03177 = 0.02718 -0.00823 -0.00715 0.01172 AFIX 43 H18B 2 0.261947 1.053408 1.041162 11.00000 -1.20000 AFIX 0 C19' 1 0.160762 0.938260 0.995339 11.00000 0.03518 0.03341 = 0.02319 -0.00480 -0.00301 0.01354 PART 1 10.93 C20' 1 -0.104157 0.702519 1.089980 10.93000 0.03401 0.03268 = 0.02653 0.00456 0.00178 0.00826 AFIX 43 H20B 2 -0.136936 0.631357 1.084823 10.93000 -1.20000 AFIX 0 O2' 4 -0.098457 0.745102 1.129315 10.93000 0.04606 0.04408 = 0.02411 0.00229 0.00396 0.00924 PART 2 10.07 C20" 1 0.058502 0.901863 1.102410 10.07000 0.09084 AFIX 43 H2'A 2 0.121098 0.959808 1.109741 10.07000 -1.20000 AFIX 0 O2" 4 -0.009754 0.852952 1.128865 10.07000 0.08711 PART 0 C21' 1 -0.228104 0.566649 1.001307 11.00000 0.03125 0.03793 = 0.02392 0.00249 0.00466 0.01050 C22' 1 -0.205128 0.459614 1.004885 11.00000 0.03277 0.03870 = 0.02707 0.00420 0.00579 0.01375 AFIX 43 H22B 2 -0.130468 0.425548 0.988823 11.00000 -1.20000 AFIX 0 C23' 1 -0.288803 0.401581 1.031378 11.00000 0.03354 0.03626 = 0.02759 0.00499 0.00119 0.00889 AFIX 43 H23B 2 -0.271682 0.328090 1.032666 11.00000 -1.20000 AFIX 0 C24' 1 -0.397799 0.448781 1.056238 11.00000 0.03054 0.04312 = 0.02212 0.00088 0.00076 0.00509 C25' 1 -0.423236 0.555152 1.051825 11.00000 0.02940 0.04405 = 0.02606 -0.00300 0.00429 0.00844 AFIX 43 H25B 2 -0.498269 0.588909 1.067804 11.00000 -1.20000 AFIX 0 C26' 1 -0.341613 0.613029 1.024647 11.00000 0.03349 0.03734 = 0.02695 0.00066 0.00387 0.01105 AFIX 43 H26B 2 -0.362753 0.685343 1.021739 11.00000 -1.20000 AFIX 0 C27' 1 -0.484341 0.385960 1.086733 11.00000 0.03552 0.04686 = 0.02725 0.00500 0.00301 0.00220 AFIX 33 H27D 2 -0.450643 0.312856 1.085313 11.00000 -1.50000 H27E 2 -0.476290 0.418236 1.118580 11.00000 -1.50000 H27F 2 -0.582323 0.385967 1.076122 11.00000 -1.50000 AFIX 0 C28' 1 0.143953 0.529442 0.793898 11.00000 0.02695 0.02484 = 0.02437 -0.00381 0.00414 -0.00232 C29' 1 0.191571 0.430326 0.803989 11.00000 0.03301 0.02940 = 0.02558 0.00038 0.00494 0.00201 AFIX 43 H29B 2 0.205118 0.416153 0.835242 11.00000 -1.20000 AFIX 0 C30' 1 0.219625 0.351703 0.769004 11.00000 0.03517 0.02394 = 0.03379 -0.00153 0.00621 0.00269 AFIX 43 H30B 2 0.249922 0.284148 0.776778 11.00000 -1.20000 AFIX 0 C31' 1 0.204120 0.370231 0.722914 11.00000 0.02953 0.02901 = 0.02798 -0.00791 0.00593 -0.00507 C32' 1 0.155695 0.468772 0.712853 11.00000 0.03833 0.03199 = 0.02482 -0.00384 0.00200 -0.00229 AFIX 43 H32B 2 0.143010 0.482845 0.681557 11.00000 -1.20000 AFIX 0 C33' 1 0.125209 0.547665 0.747669 11.00000 0.03521 0.02674 = 0.02605 -0.00158 0.00078 -0.00077 AFIX 43 H33B 2 0.091452 0.614250 0.739827 11.00000 -1.20000 AFIX 0 C34' 1 0.242764 0.286866 0.685315 11.00000 0.03969 0.03336 = 0.03506 -0.01050 0.00730 -0.00047 AFIX 33 H34D 2 0.274457 0.223117 0.699072 11.00000 -1.50000 H34E 2 0.161056 0.269257 0.665002 11.00000 -1.50000 H34F 2 0.317930 0.313970 0.667403 11.00000 -1.50000 AFIX 0 C35' 1 0.440924 1.027692 0.873089 11.00000 0.03627 0.02572 = 0.02711 -0.00371 -0.00372 0.00183 C36' 1 0.581266 1.001279 0.868952 11.00000 0.03617 0.02612 = 0.03728 -0.00451 -0.00518 0.00143 AFIX 43 H36B 2 0.611525 0.932663 0.875266 11.00000 -1.20000 AFIX 0 C37' 1 0.677023 1.074128 0.855722 11.00000 0.03369 0.03461 = 0.04534 -0.00602 -0.00278 -0.00313 AFIX 43 H37B 2 0.772383 1.054921 0.853188 11.00000 -1.20000 AFIX 0 C38' 1 0.635319 1.175786 0.846016 11.00000 0.04571 0.03124 = 0.04223 -0.00268 -0.00356 -0.00541 C39' 1 0.495061 1.200975 0.849925 11.00000 0.04579 0.02754 = 0.04226 0.00168 -0.00648 -0.00023 AFIX 43 H39B 2 0.464680 1.269500 0.843520 11.00000 -1.20000 AFIX 0 C40' 1 0.398152 1.128279 0.862984 11.00000 0.03778 0.02874 = 0.03744 -0.00133 -0.00537 0.00355 AFIX 43 H40B 2 0.302544 1.147094 0.865040 11.00000 -1.20000 AFIX 0 C41' 1 0.739514 1.254505 0.830801 11.00000 0.05398 0.04226 = 0.07210 0.00271 0.00180 -0.01527 AFIX 33 H41D 2 0.832585 1.222814 0.830099 11.00000 -1.50000 H41E 2 0.712515 1.273359 0.799933 11.00000 -1.50000 H41F 2 0.741040 1.318413 0.852498 11.00000 -1.50000 AFIX 0 C42' 1 0.450904 1.116434 0.978314 11.00000 0.04997 0.02693 = 0.03545 -0.00212 -0.00829 0.00781 AFIX 43 H42B 2 0.505419 1.125536 0.952219 11.00000 -1.20000 AFIX 0 O3' 4 0.482154 1.166852 1.015089 11.00000 0.06073 0.03214 = 0.04158 -0.00942 -0.01469 0.00464 C1S 1 1.067372 0.009670 0.777763 11.00000 0.05230 0.08565 = 0.10163 0.03501 -0.00959 0.00810 AFIX 33 H1SA 2 1.141254 -0.026252 0.794137 11.00000 -1.50000 H1SB 2 1.100961 0.026870 0.747866 11.00000 -1.50000 H1SC 2 1.041930 0.075115 0.796102 11.00000 -1.50000 AFIX 0 C2S 1 0.938637 -0.063653 0.770206 11.00000 0.07253 0.05284 = 0.04791 0.01058 0.00339 0.00855 AFIX 23 H2SA 2 0.965673 -0.130235 0.752290 11.00000 -1.20000 H2SB 2 0.906668 -0.082011 0.800505 11.00000 -1.20000 AFIX 0 C3S 1 0.817654 -0.013568 0.744741 11.00000 0.06177 0.04220 = 0.04068 0.00778 0.00304 -0.00176 AFIX 23 H3SA 2 0.792996 0.053819 0.762497 11.00000 -1.20000 H3SB 2 0.850434 0.004064 0.714432 11.00000 -1.20000 AFIX 0 C4S 1 0.687200 -0.080970 0.736874 11.00000 0.06521 0.05573 = 0.05505 0.01034 -0.00625 -0.00487 AFIX 23 H4SA 2 0.647612 -0.091587 0.767136 11.00000 -1.20000 H4SB 2 0.713090 -0.151476 0.722205 11.00000 -1.20000 AFIX 0 C5S 1 0.575802 -0.034633 0.707121 11.00000 0.06380 0.06761 = 0.07131 0.00821 -0.01312 0.00097 AFIX 23 H5SA 2 0.615573 -0.024174 0.676870 11.00000 -1.20000 H5SB 2 0.498276 -0.086696 0.701622 11.00000 -1.20000 AFIX 0 C6S 1 0.517875 0.067828 0.726744 11.00000 0.06145 0.08302 = 0.05902 -0.00434 -0.01148 0.01163 AFIX 33 H6SA 2 0.446769 0.092057 0.705357 11.00000 -1.50000 H6SB 2 0.475565 0.058170 0.756308 11.00000 -1.50000 H6SC 2 0.593095 0.120816 0.731507 11.00000 -1.50000 AFIX 0 HKLF 4 REM Bi_CHO_DCMHex_a.res in P-1 REM R1 = 0.0312 for 19296 Fo > 4sig(Fo) and 0.0361 for all 21566 data REM 975 parameters refined using 40 restraints END WGHT 0.0109 8.9113 REM Highest difference peak 2.379, deepest hole -2.218, 1-sigma level 0.103 Q1 1 -0.0015 0.7666 0.9187 11.00000 0.05 2.38 Q2 1 0.5906 0.1744 0.5969 11.00000 0.05 2.24 Q3 1 0.0902 0.7838 0.9250 11.00000 0.05 1.61 Q4 1 -0.0786 0.8235 0.9132 11.00000 0.05 1.07 Q5 1 -0.0288 0.8367 1.1414 11.00000 0.05 0.96 Q6 1 0.4143 0.2131 0.5818 11.00000 0.05 0.93 Q7 1 0.0153 0.8685 1.1024 11.00000 0.05 0.83 Q8 1 0.4974 0.1759 0.5814 11.00000 0.05 0.81 Q9 1 0.0330 0.8399 0.9245 11.00000 0.05 0.76 Q10 1 0.5759 0.2233 0.5752 11.00000 0.05 0.75 Q11 1 0.1012 0.8414 0.8953 11.00000 0.05 0.72 Q12 1 0.1149 0.8586 0.9047 11.00000 0.05 0.70 Q13 1 0.4496 0.1645 0.5832 11.00000 0.05 0.69 Q14 1 -0.1976 0.2770 1.0550 11.00000 0.05 0.68 Q15 1 -0.0263 0.8775 0.9047 11.00000 0.05 0.68 Q16 1 0.1637 0.8367 0.9227 11.00000 0.05 0.65 Q17 1 0.6837 0.2197 0.5852 11.00000 0.05 0.61 Q18 1 0.1086 0.8814 0.9412 11.00000 0.05 0.59 Q19 1 0.5011 0.1375 0.3981 11.00000 0.05 0.58 Q20 1 0.4825 0.2510 0.5700 11.00000 0.05 0.56 ; _shelx_res_checksum 69322 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'