# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # 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_compound2 _database_code_depnum_ccdc_archive 'CCDC 1949887' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-07-01 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' beate.neumann@uni-bielefeld.de _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C54 H72 Cl N3 P, C F3 O3 S' _chemical_formula_sum 'C55 H72 Cl F3 N3 O3 P S' _chemical_formula_weight 978.63 _chemical_melting_point ? _chemical_oxdiff_formula C55H72ClF3N3O3PS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0592(4) _cell_length_b 12.9006(3) _cell_length_c 18.7834(5) _cell_angle_alpha 98.063(2) _cell_angle_beta 91.131(2) _cell_angle_gamma 103.315(3) _cell_volume 2578.25(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 21348 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.2750 _cell_measurement_theta_min 3.4950 _shelx_estimated_absorpt_T_max 0.948 _shelx_estimated_absorpt_T_min 0.470 _exptl_absorpt_coefficient_mu 1.785 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.451 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear pink' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1044 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0148 1 8 -3 0.1074 6 2 -1 0.1738 2 -8 3 0.1396 -7 -1 0 0.1824 0 0 -1 0.0148 _exptl_crystal_size_max 0.499 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.03 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0005 0.0065 0.9979 -0.0828 -0.0012 -0.0036 0.9707 7.7982 -2.5539 0.0763 -0.9609 -0.2661 6.2610 2.3035 -0.9767 0.0299 -0.3655 -0.9303 2.1712 -8.3236 2.6066 -0.0775 0.9818 -0.1733 -6.8585 -0.5536 0.4340 -0.0138 0.1610 0.9869 -0.0005 -0.0065 -0.9979 0.0828 0.0012 0.0036 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_unetI/netI 0.0302 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 46168 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.693 _diffrn_reflns_theta_min 2.379 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -60.00 29.00 1.00 12.50 -- -38.50 57.00 30.00 89 2 \w -58.00 33.00 1.00 12.50 -- -38.50 38.00 -60.00 91 3 \w -50.00 31.00 1.00 12.50 -- -38.50 77.00 150.00 81 4 \w -66.00 -18.00 1.00 12.50 -- -38.50 -38.00 -30.00 48 5 \w 19.00 74.00 1.00 12.50 -- 42.70 57.00 150.00 55 6 \w 3.00 75.00 1.00 12.50 -- 42.70 -99.00 -90.00 72 7 \w 15.00 43.00 1.00 12.50 -- 42.70 77.00 120.00 28 8 \w 65.00 108.00 1.00 12.50 -- 42.70 77.00 120.00 43 9 \w 15.00 52.00 1.00 12.50 -- 42.70 77.00 0.00 37 10 \w 20.00 96.00 1.00 12.50 -- 42.70 57.00 30.00 76 11 \w 10.00 67.00 1.00 12.50 -- 42.70 -99.00 90.00 57 12 \w 17.00 61.00 1.00 12.50 -- 42.70 77.00-180.00 44 13 \w 13.00 60.00 1.00 12.50 -- 42.70 77.00 -60.00 47 14 \w 64.00 114.00 1.00 12.50 -- 42.70 77.00-180.00 50 15 \w 13.00 114.00 1.00 12.50 -- 42.70 77.00-120.00 101 16 \w 29.00 57.00 1.00 12.50 -- 42.70 38.00 0.00 28 17 \w 13.00 80.00 1.00 12.50 -- 42.70 77.00 60.00 67 18 \w 31.00 89.00 1.00 49.50 -- 111.00 -94.00 0.00 58 19 \w 81.00 177.00 1.00 49.50 -- 111.00 77.00 -30.00 96 20 \w 41.00 102.00 1.00 49.50 -- 111.00-125.00 -30.00 61 21 \w 43.00 137.00 1.00 49.50 -- 111.00 -61.00 150.00 94 22 \w 81.00 108.00 1.00 49.50 -- 111.00 77.00 90.00 27 23 \w 81.00 176.00 1.00 49.50 -- 111.00 77.00 150.00 95 24 \w 81.00 164.00 1.00 49.50 -- 111.00 77.00-120.00 83 25 \w 85.00 130.00 1.00 49.50 -- 111.00 61.00-120.00 45 26 \w 85.00 177.00 1.00 49.50 -- 111.00 61.00 -60.00 92 27 \w 83.00 110.00 1.00 49.50 -- 111.00 68.00 -51.76 27 28 \w 85.00 178.00 1.00 49.50 -- 111.00 62.00 93.47 93 29 \w 112.00 146.00 1.00 49.50 -- 111.00 77.00 60.00 34 30 \w 81.00 171.00 1.00 49.50 -- 111.00 77.00 30.00 90 31 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00 30.00 27 32 \w 81.00 107.00 1.00 49.50 -- 111.00 77.00 60.00 26 33 \w 43.00 121.00 1.00 49.50 -- 111.00-129.00 143.00 78 34 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00 90.00 27 35 \w 31.00 106.00 1.00 49.50 -- 111.00 -94.00 150.00 75 36 \w 88.00 152.00 1.00 49.50 -- 111.00 48.00-154.30 64 37 \w 81.00 175.00 1.00 49.50 -- 111.00 77.00 0.00 94 38 \w 82.00 108.00 1.00 49.50 -- 111.00 77.00-180.00 26 39 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00 120.00 27 40 \w 81.00 107.00 1.00 49.50 -- 111.00 77.00 -90.00 26 41 \w 91.00 116.00 1.00 49.50 -- 111.00-125.00 -90.00 25 42 \w 81.00 151.00 1.00 49.50 -- 111.00 77.00 120.00 70 43 \w 85.00 111.00 1.00 49.50 -- 111.00 61.00 60.00 26 44 \w 85.00 111.00 1.00 49.50 -- 111.00 61.00 150.00 26 45 \w 81.00 107.00 1.00 49.50 -- 111.00 77.00-150.00 26 46 \w 85.00 111.00 1.00 49.50 -- 111.00 61.00-150.00 26 47 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00 0.00 27 48 \w 85.00 122.00 1.00 49.50 -- 111.00 61.00 -30.00 37 49 \w 45.00 118.00 1.00 49.50 -- 111.00-125.00 90.00 73 50 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00 -90.00 27 51 \w 85.00 112.00 1.00 49.50 -- 111.00 61.00-180.00 27 52 \w 88.00 118.00 1.00 49.50 -- 111.00-125.00 0.00 30 53 \w 58.00 87.00 1.00 49.50 -- 111.00-125.00 0.00 29 54 \w 82.00 178.00 1.00 49.50 -- 111.00 73.00-158.66 96 55 \w 84.00 157.00 1.00 49.50 -- 111.00 66.00 -84.59 73 56 \w 83.00 107.00 1.00 49.50 -- 111.00 68.00 120.11 24 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0018531000 _diffrn_orient_matrix_UB_12 -0.0171295000 _diffrn_orient_matrix_UB_13 -0.0828872000 _diffrn_orient_matrix_UB_21 -0.0136864000 _diffrn_orient_matrix_UB_22 -0.1216643000 _diffrn_orient_matrix_UB_23 -0.0004385000 _diffrn_orient_matrix_UB_31 -0.1426921000 _diffrn_orient_matrix_UB_32 -0.0174640000 _diffrn_orient_matrix_UB_33 -0.0033826000 _diffrn_oxdiff_digest_frames ; 01b398728a16ea12b9fc2eda7727766f6d0314356fd ; _diffrn_oxdiff_digest_hkl ; 0123ca9911f43a4794f9ebcb5eeb0c47a3ff5e ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9327 _reflns_number_total 10686 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 42.14 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _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 0.445 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.051 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 675 _refine_ls_number_reflns 10686 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0420 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.9870P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.1182 _refine_special_details ; Disorder of one i-propylgroup (C13, C14, C15) over two sites (78:22). Disorder of CF3-group over two sites (79:21) ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C55B) = Uanis(C55) Uanis(C13) = Uanis(C13B) 3. Rigid body (RIGU) restrains F1, F1B, F2, F2B, F3, F3B, O1, O2, O3, C55, C55B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)= Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1) Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)= Sof(H15B)=Sof(H15C)=FVAR(1) Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(C55B)=1-FVAR(2) Sof(F1)=Sof(F2)=Sof(F3)=Sof(C55)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C13B(H13B), C22(H22), C25(H25), C49(H49), C52(H52) 5.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 5.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C14B(H14D,H14E, H14F), C15(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C39(H39A,H39B, H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A, H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C) ; _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 Cl1 Cl 0.86131(4) 0.57571(3) 0.38621(2) 0.02716(10) Uani 1 1 d . . . . . P1 P 0.76081(4) 0.55263(3) 0.28406(2) 0.02046(9) Uani 1 1 d . . . . . N1 N 0.63005(13) 0.30592(11) 0.22222(8) 0.0253(3) Uani 1 1 d . . . . . N2 N 0.80657(12) 0.26134(10) 0.20542(7) 0.0207(3) Uani 1 1 d . . . . . N3 N 0.87492(12) 0.77814(10) 0.28621(7) 0.0197(3) Uani 1 1 d . . . . . C1 C 0.75510(14) 0.34921(12) 0.21856(8) 0.0202(3) Uani 1 1 d . . . . . C2 C 0.60541(17) 0.19383(13) 0.21099(10) 0.0301(4) Uani 1 1 d . . . . . H2 H 0.527835 0.146735 0.210972 0.036 Uiso 1 1 calc R . . . . C3 C 0.71287(16) 0.16662(12) 0.20033(9) 0.0266(3) Uani 1 1 d . . . . . H3 H 0.724000 0.096791 0.191093 0.032 Uiso 1 1 calc R . . . . C4 C 0.53007(15) 0.35966(13) 0.23415(9) 0.0271(3) Uani 1 1 d . . . . . C5 C 0.49668(16) 0.38283(14) 0.30539(10) 0.0300(4) Uani 1 1 d . . . . . C6 C 0.39990(18) 0.43481(15) 0.31571(12) 0.0379(4) Uani 1 1 d . . . . . H6 H 0.376848 0.454230 0.362126 0.046 Uiso 1 1 calc R . . . . C7 C 0.33748(19) 0.45791(17) 0.25731(14) 0.0469(5) Uani 1 1 d . . . . . H7 H 0.274987 0.495018 0.265088 0.056 Uiso 1 1 calc R . . . . C8 C 0.36700(19) 0.42653(19) 0.18795(14) 0.0468(5) Uani 1 1 d . . . . . H8 H 0.321306 0.439672 0.149502 0.056 Uiso 1 1 calc R . . . . C9 C 0.46441(17) 0.37528(17) 0.17430(11) 0.0374(4) Uani 1 1 d . . . . . C10 C 0.55781(19) 0.34617(16) 0.36690(10) 0.0366(4) Uani 1 1 d . . . . . H10 H 0.642128 0.342167 0.353811 0.044 Uiso 1 1 calc R . . . . C11 C 0.4861(3) 0.23200(18) 0.37798(13) 0.0514(6) Uani 1 1 d . . . . . H11A H 0.402058 0.233265 0.389233 0.077 Uiso 1 1 calc GR . . . . H11B H 0.526115 0.209450 0.416903 0.077 Uiso 1 1 calc GR . . . . H11C H 0.485497 0.182500 0.334686 0.077 Uiso 1 1 calc GR . . . . C12 C 0.5684(2) 0.42215(19) 0.43781(11) 0.0490(5) Uani 1 1 d . . . . . H12A H 0.605501 0.494404 0.430155 0.074 Uiso 1 1 calc GR . . . . H12B H 0.619445 0.400876 0.472370 0.074 Uiso 1 1 calc GR . . . . H12C H 0.487071 0.419010 0.455576 0.074 Uiso 1 1 calc GR . . . . C13 C 0.4903(2) 0.3248(2) 0.09772(14) 0.0324(6) Uani 0.783(5) 1 d . . P A 1 H13 H 0.572199 0.307962 0.099919 0.039 Uiso 0.783(5) 1 calc R . P A 1 C13B C 0.4775(9) 0.3702(9) 0.0970(6) 0.0324(6) Uani 0.217(5) 1 d . . P A 2 H13B H 0.458397 0.435124 0.082675 0.039 Uiso 0.217(5) 1 calc R . P A 2 C14 C 0.3933(3) 0.2203(3) 0.0723(2) 0.0465(8) Uani 0.783(5) 1 d . . P A 1 H14A H 0.393578 0.170870 0.106055 0.070 Uiso 0.783(5) 1 calc GR . P A 1 H14B H 0.412808 0.188934 0.025847 0.070 Uiso 0.783(5) 1 calc GR . P A 1 H14C H 0.312454 0.235349 0.069173 0.070 Uiso 0.783(5) 1 calc GR . P A 1 C14B C 0.3738(13) 0.2746(14) 0.0652(7) 0.056(3) Uani 0.217(5) 1 d . . P A 2 H14D H 0.380030 0.212690 0.086817 0.084 Uiso 0.217(5) 1 calc GR . P A 2 H14E H 0.381125 0.259620 0.014172 0.084 Uiso 0.217(5) 1 calc GR . P A 2 H14F H 0.294708 0.290955 0.074611 0.084 Uiso 0.217(5) 1 calc GR . P A 2 C15 C 0.4928(3) 0.4041(2) 0.04419(14) 0.0451(7) Uani 0.783(5) 1 d . . P A 1 H15A H 0.413197 0.421426 0.041216 0.068 Uiso 0.783(5) 1 calc GR . P A 1 H15B H 0.511160 0.372006 -0.002384 0.068 Uiso 0.783(5) 1 calc GR . P A 1 H15C H 0.555765 0.468587 0.060115 0.068 Uiso 0.783(5) 1 calc GR . P A 1 C15B C 0.6011(9) 0.3625(8) 0.0702(5) 0.038(2) Uani 0.217(5) 1 d . . P A 2 H15D H 0.663895 0.422170 0.094190 0.057 Uiso 0.217(5) 1 calc GR . P A 2 H15E H 0.600425 0.364022 0.019281 0.057 Uiso 0.217(5) 1 calc GR . P A 2 H15F H 0.618927 0.296272 0.079964 0.057 Uiso 0.217(5) 1 calc GR . P A 2 C16 C 0.93408(15) 0.24969(11) 0.20882(9) 0.0222(3) Uani 1 1 d . . . . . C17 C 0.97444(16) 0.19394(12) 0.14759(9) 0.0251(3) Uani 1 1 d . . . . . C18 C 1.08715(17) 0.16337(13) 0.15556(10) 0.0301(4) Uani 1 1 d . . . . . H18 H 1.116268 0.125913 0.116192 0.036 Uiso 1 1 calc R . . . . C19 C 1.15570(17) 0.18738(14) 0.22013(11) 0.0337(4) Uani 1 1 d . . . . . H19 H 1.229964 0.165908 0.224084 0.040 Uiso 1 1 calc R . . . . C20 C 1.11400(17) 0.24369(14) 0.27940(10) 0.0312(4) Uani 1 1 d . . . . . H20 H 1.161601 0.260552 0.322637 0.037 Uiso 1 1 calc R . . . . C21 C 1.00227(16) 0.27538(12) 0.27532(9) 0.0251(3) Uani 1 1 d . . . . . C22 C 0.90282(17) 0.16398(13) 0.07491(9) 0.0279(3) Uani 1 1 d . . . . . H22 H 0.833661 0.199882 0.076806 0.033 Uiso 1 1 calc R . . . . C23 C 0.84841(19) 0.04157(14) 0.05657(10) 0.0343(4) Uani 1 1 d . . . . . H23A H 0.914443 0.004646 0.057097 0.051 Uiso 1 1 calc GR . . . . H23B H 0.806820 0.025489 0.009602 0.051 Uiso 1 1 calc GR . . . . H23C H 0.790081 0.018347 0.091590 0.051 Uiso 1 1 calc GR . . . . C24 C 0.9859(2) 0.20249(15) 0.01474(10) 0.0379(4) Uani 1 1 d . . . . . H24A H 1.023393 0.277992 0.027155 0.057 Uiso 1 1 calc GR . . . . H24B H 0.936356 0.190413 -0.029523 0.057 Uiso 1 1 calc GR . . . . H24C H 1.049765 0.163154 0.008949 0.057 Uiso 1 1 calc GR . . . . C25 C 0.95264(18) 0.32868(14) 0.34199(9) 0.0302(4) Uani 1 1 d . . . . . H25 H 0.909921 0.381215 0.326806 0.036 Uiso 1 1 calc R . . . . C26 C 0.8554(2) 0.24452(17) 0.37419(10) 0.0371(4) Uani 1 1 d . . . . . H26A H 0.787875 0.212729 0.339231 0.056 Uiso 1 1 calc GR . . . . H26B H 0.824435 0.278890 0.416274 0.056 Uiso 1 1 calc GR . . . . H26C H 0.893436 0.189472 0.387121 0.056 Uiso 1 1 calc GR . . . . C27 C 1.0547(2) 0.38976(16) 0.39921(10) 0.0406(5) Uani 1 1 d . . . . . H27A H 1.092703 0.339375 0.418836 0.061 Uiso 1 1 calc GR . . . . H27B H 1.018735 0.428973 0.437016 0.061 Uiso 1 1 calc GR . . . . H27C H 1.116571 0.439129 0.377581 0.061 Uiso 1 1 calc GR . . . . C28 C 0.81989(15) 0.46062(12) 0.22544(8) 0.0202(3) Uani 1 1 d . . . . . C29 C 0.94152(14) 0.49053(11) 0.19284(8) 0.0201(3) Uani 1 1 d . . . . . C30 C 0.95926(16) 0.44735(12) 0.12198(9) 0.0241(3) Uani 1 1 d . . . . . H30 H 0.898488 0.390643 0.097531 0.029 Uiso 1 1 calc R . . . . C31 C 1.06646(17) 0.48833(13) 0.08798(10) 0.0299(4) Uani 1 1 d . . . . . H31 H 1.076601 0.458856 0.041010 0.036 Uiso 1 1 calc R . . . . C32 C 1.15854(17) 0.57275(14) 0.12333(11) 0.0336(4) Uani 1 1 d . . . . . H32 H 1.228784 0.601596 0.099744 0.040 Uiso 1 1 calc R . . . . C33 C 1.14474(16) 0.61369(13) 0.19424(10) 0.0308(4) Uani 1 1 d . . . . . H33 H 1.206933 0.669039 0.218827 0.037 Uiso 1 1 calc R . . . . C34 C 1.03837(15) 0.57218(12) 0.22848(9) 0.0243(3) Uani 1 1 d . . . . . H34 H 1.031152 0.599273 0.276362 0.029 Uiso 1 1 calc R . . . . C35 C 0.81893(14) 0.68335(12) 0.25080(8) 0.0199(3) Uani 1 1 d . . . . . C36 C 0.76679(16) 0.69578(12) 0.17626(8) 0.0235(3) Uani 1 1 d . . . . . C37 C 0.79923(17) 0.81914(13) 0.17806(8) 0.0262(3) Uani 1 1 d . . . . . H37A H 0.827649 0.837252 0.131843 0.031 Uiso 1 1 calc R . . . . H37B H 0.726582 0.847561 0.188626 0.031 Uiso 1 1 calc R . . . . C38 C 0.90181(16) 0.86649(12) 0.23675(8) 0.0230(3) Uani 1 1 d . . . . . C39 C 0.81750(19) 0.63794(14) 0.11086(9) 0.0302(4) Uani 1 1 d . . . . . H39A H 0.906756 0.659329 0.113834 0.045 Uiso 1 1 calc GR . . . . H39B H 0.786231 0.656739 0.067601 0.045 Uiso 1 1 calc GR . . . . H39C H 0.791330 0.561474 0.110139 0.045 Uiso 1 1 calc GR . . . . C40 C 0.62432(17) 0.65360(14) 0.17352(9) 0.0301(4) Uani 1 1 d . . . . . H40A H 0.604274 0.577248 0.174025 0.045 Uiso 1 1 calc GR . . . . H40B H 0.588598 0.668655 0.130240 0.045 Uiso 1 1 calc GR . . . . H40C H 0.591339 0.688631 0.214590 0.045 Uiso 1 1 calc GR . . . . C41 C 1.03099(17) 0.87349(13) 0.20743(9) 0.0283(3) Uani 1 1 d . . . . . H41A H 1.093330 0.906344 0.245269 0.042 Uiso 1 1 calc GR . . . . H41B H 1.040645 0.916134 0.169034 0.042 Uiso 1 1 calc GR . . . . H41C H 1.040101 0.802381 0.189591 0.042 Uiso 1 1 calc GR . . . . C42 C 0.89321(17) 0.97531(12) 0.27655(9) 0.0271(3) Uani 1 1 d . . . . . H42A H 0.809924 0.971371 0.291427 0.041 Uiso 1 1 calc GR . . . . H42B H 0.914174 1.028810 0.245231 0.041 Uiso 1 1 calc GR . . . . H42C H 0.950089 0.994517 0.318126 0.041 Uiso 1 1 calc GR . . . . C43 C 0.89335(15) 0.80839(11) 0.36466(8) 0.0205(3) Uani 1 1 d . . . . . C44 C 0.78771(15) 0.82519(12) 0.40126(8) 0.0231(3) Uani 1 1 d . . . . . C45 C 0.80155(17) 0.85055(13) 0.47619(9) 0.0266(3) Uani 1 1 d . . . . . H45 H 0.732740 0.858705 0.502140 0.032 Uiso 1 1 calc R . . . . C46 C 0.91477(18) 0.86377(14) 0.51258(9) 0.0289(3) Uani 1 1 d . . . . . H46 H 0.921636 0.879899 0.562545 0.035 Uiso 1 1 calc R . . . . C47 C 1.01815(17) 0.85298(13) 0.47463(9) 0.0273(3) Uani 1 1 d . . . . . H47 H 1.094848 0.865157 0.499503 0.033 Uiso 1 1 calc R . . . . C48 C 1.01026(15) 0.82431(12) 0.39998(8) 0.0229(3) Uani 1 1 d . . . . . C49 C 0.66116(16) 0.81977(13) 0.36549(9) 0.0264(3) Uani 1 1 d . . . . . H49 H 0.670218 0.814786 0.313410 0.032 Uiso 1 1 calc R . . . . C50 C 0.56356(17) 0.72067(15) 0.37942(10) 0.0347(4) Uani 1 1 d . . . . . H50A H 0.591682 0.656823 0.362881 0.052 Uiso 1 1 calc GR . . . . H50B H 0.486471 0.718040 0.354035 0.052 Uiso 1 1 calc GR . . . . H50C H 0.551261 0.724907 0.430103 0.052 Uiso 1 1 calc GR . . . . C51 C 0.61462(18) 0.92202(15) 0.39089(10) 0.0345(4) Uani 1 1 d . . . . . H51A H 0.594029 0.923377 0.440372 0.052 Uiso 1 1 calc GR . . . . H51B H 0.542087 0.921692 0.361850 0.052 Uiso 1 1 calc GR . . . . H51C H 0.678779 0.984630 0.386263 0.052 Uiso 1 1 calc GR . . . . C52 C 1.12914(15) 0.81244(13) 0.36385(9) 0.0260(3) Uani 1 1 d . . . . . H52 H 1.108603 0.787074 0.312421 0.031 Uiso 1 1 calc R . . . . C53 C 1.18895(18) 0.73106(16) 0.39473(10) 0.0353(4) Uani 1 1 d . . . . . H53A H 1.218868 0.758837 0.443601 0.053 Uiso 1 1 calc GR . . . . H53B H 1.257189 0.719158 0.366454 0.053 Uiso 1 1 calc GR . . . . H53C H 1.128228 0.664240 0.393473 0.053 Uiso 1 1 calc GR . . . . C54 C 1.22320(18) 0.92202(16) 0.37188(10) 0.0360(4) Uani 1 1 d . . . . . H54A H 1.184752 0.973933 0.354579 0.054 Uiso 1 1 calc GR . . . . H54B H 1.293958 0.915267 0.344376 0.054 Uiso 1 1 calc GR . . . . H54C H 1.249668 0.945348 0.421701 0.054 Uiso 1 1 calc GR . . . . S1 S 0.43407(4) 0.91198(3) 0.20197(2) 0.03101(11) Uani 1 1 d . . . . . F1 F 0.2593(4) 0.8403(3) 0.09856(17) 0.0593(8) Uani 0.789(13) 1 d . U P B 1 F1B F 0.313(2) 0.8444(13) 0.0778(14) 0.100(6) Uani 0.211(13) 1 d . U P B 2 F2 F 0.4244(5) 0.7827(2) 0.08004(17) 0.0602(9) Uani 0.789(13) 1 d . U P B 1 F2B F 0.497(3) 0.8149(15) 0.0826(6) 0.078(5) Uani 0.211(13) 1 d . U P B 2 F3 F 0.4253(5) 0.9462(4) 0.0687(3) 0.0663(10) Uani 0.789(13) 1 d . U P B 1 F3B F 0.473(2) 0.9732(15) 0.0731(11) 0.074(5) Uani 0.211(13) 1 d . U P B 2 O1 O 0.38493(14) 0.81605(11) 0.23302(8) 0.0420(3) Uani 1 1 d . U . . . O2 O 0.56716(13) 0.94320(11) 0.20399(10) 0.0496(4) Uani 1 1 d . U . . . O3 O 0.37434(13) 0.99921(11) 0.22047(9) 0.0422(3) Uani 1 1 d . U . . . C55 C 0.3827(6) 0.8685(3) 0.1086(2) 0.0405(9) Uani 0.789(13) 1 d . U P B 1 C55B C 0.4261(18) 0.8839(14) 0.1019(10) 0.0405(9) Uani 0.211(13) 1 d . U P B 2 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 Cl1 0.0368(2) 0.02142(18) 0.02342(17) 0.00181(13) 0.00102(15) 0.00813(15) P1 0.0223(2) 0.01706(18) 0.02185(18) 0.00066(13) 0.00432(14) 0.00529(15) N1 0.0196(7) 0.0188(6) 0.0351(7) -0.0018(5) 0.0068(5) 0.0023(5) N2 0.0206(7) 0.0141(6) 0.0263(6) 0.0007(5) 0.0055(5) 0.0028(5) N3 0.0207(6) 0.0171(6) 0.0221(6) 0.0013(5) 0.0040(5) 0.0069(5) C1 0.0194(7) 0.0182(7) 0.0217(7) 0.0004(5) 0.0043(6) 0.0034(6) C2 0.0252(9) 0.0180(7) 0.0416(9) -0.0024(6) 0.0094(7) -0.0027(6) C3 0.0261(9) 0.0157(7) 0.0352(8) 0.0007(6) 0.0086(7) 0.0004(6) C4 0.0166(8) 0.0234(8) 0.0387(9) 0.0002(6) 0.0067(6) 0.0015(6) C5 0.0229(8) 0.0239(8) 0.0414(9) 0.0016(7) 0.0103(7) 0.0031(7) C6 0.0280(9) 0.0291(9) 0.0555(11) 0.0008(8) 0.0167(8) 0.0066(8) C7 0.0243(10) 0.0406(11) 0.0806(16) 0.0141(10) 0.0146(10) 0.0134(9) C8 0.0217(9) 0.0565(13) 0.0662(14) 0.0216(11) 0.0046(9) 0.0097(9) C9 0.0190(8) 0.0435(10) 0.0463(10) 0.0060(8) 0.0033(8) 0.0010(8) C10 0.0353(10) 0.0380(10) 0.0378(9) 0.0061(8) 0.0139(8) 0.0099(8) C11 0.0671(16) 0.0370(11) 0.0523(12) 0.0115(9) 0.0202(11) 0.0125(11) C12 0.0540(14) 0.0508(12) 0.0373(10) 0.0018(9) 0.0156(10) 0.0038(11) C13 0.0257(11) 0.0291(15) 0.0410(11) 0.0006(11) 0.0008(9) 0.0067(11) C13B 0.0257(11) 0.0291(15) 0.0410(11) 0.0006(11) 0.0008(9) 0.0067(11) C14 0.0376(16) 0.0374(17) 0.0542(18) -0.0088(14) 0.0076(13) -0.0031(14) C14B 0.045(7) 0.066(9) 0.046(6) 0.010(6) -0.006(5) -0.007(7) C15 0.0543(18) 0.0391(14) 0.0352(13) -0.0026(10) -0.0082(12) 0.0033(12) C15B 0.040(5) 0.040(5) 0.029(4) 0.000(3) -0.001(4) 0.003(4) C16 0.0219(8) 0.0136(6) 0.0316(8) 0.0043(6) 0.0076(6) 0.0039(6) C17 0.0264(8) 0.0153(7) 0.0331(8) 0.0039(6) 0.0110(7) 0.0030(6) C18 0.0269(9) 0.0211(7) 0.0430(9) 0.0034(7) 0.0136(7) 0.0069(7) C19 0.0231(9) 0.0264(8) 0.0524(11) 0.0052(7) 0.0072(8) 0.0072(7) C20 0.0255(9) 0.0240(8) 0.0432(10) 0.0039(7) -0.0003(7) 0.0048(7) C21 0.0276(9) 0.0155(7) 0.0317(8) 0.0027(6) 0.0033(7) 0.0044(6) C22 0.0353(9) 0.0196(7) 0.0288(8) 0.0006(6) 0.0094(7) 0.0078(7) C23 0.0434(11) 0.0214(8) 0.0362(9) -0.0013(7) 0.0055(8) 0.0070(7) C24 0.0560(13) 0.0264(8) 0.0326(9) 0.0019(7) 0.0183(8) 0.0126(8) C25 0.0387(10) 0.0277(8) 0.0270(8) 0.0021(6) 0.0002(7) 0.0148(7) C26 0.0411(11) 0.0469(11) 0.0293(8) 0.0108(8) 0.0069(8) 0.0189(9) C27 0.0559(13) 0.0320(9) 0.0348(9) -0.0024(7) -0.0096(9) 0.0179(9) C28 0.0212(8) 0.0165(7) 0.0224(7) 0.0011(5) 0.0043(6) 0.0041(6) C29 0.0197(8) 0.0153(6) 0.0269(7) 0.0047(5) 0.0047(6) 0.0063(6) C30 0.0263(8) 0.0177(7) 0.0289(8) 0.0033(6) 0.0066(6) 0.0063(6) C31 0.0348(10) 0.0224(8) 0.0352(8) 0.0061(6) 0.0147(7) 0.0102(7) C32 0.0271(9) 0.0243(8) 0.0515(11) 0.0098(7) 0.0180(8) 0.0064(7) C33 0.0216(8) 0.0207(7) 0.0486(10) 0.0029(7) 0.0049(7) 0.0030(6) C34 0.0219(8) 0.0181(7) 0.0333(8) 0.0016(6) 0.0030(6) 0.0063(6) C35 0.0183(7) 0.0196(7) 0.0225(7) 0.0001(5) 0.0040(6) 0.0073(6) C36 0.0288(9) 0.0201(7) 0.0225(7) 0.0009(5) -0.0001(6) 0.0089(6) C37 0.0344(9) 0.0212(7) 0.0255(7) 0.0034(6) 0.0018(7) 0.0115(7) C38 0.0291(9) 0.0169(7) 0.0248(7) 0.0047(6) 0.0051(6) 0.0079(6) C39 0.0433(11) 0.0287(8) 0.0225(7) 0.0021(6) 0.0024(7) 0.0175(8) C40 0.0298(9) 0.0267(8) 0.0326(8) -0.0031(6) -0.0070(7) 0.0094(7) C41 0.0323(9) 0.0239(8) 0.0311(8) 0.0073(6) 0.0096(7) 0.0089(7) C42 0.0329(9) 0.0174(7) 0.0314(8) 0.0029(6) 0.0056(7) 0.0071(6) C43 0.0254(8) 0.0149(6) 0.0210(7) 0.0008(5) 0.0023(6) 0.0054(6) C44 0.0246(8) 0.0184(7) 0.0256(7) 0.0006(6) 0.0035(6) 0.0049(6) C45 0.0287(9) 0.0249(8) 0.0263(8) 0.0002(6) 0.0069(6) 0.0084(7) C46 0.0373(10) 0.0272(8) 0.0220(7) -0.0005(6) 0.0021(7) 0.0096(7) C47 0.0284(9) 0.0269(8) 0.0263(8) 0.0009(6) -0.0013(6) 0.0077(7) C48 0.0245(8) 0.0182(7) 0.0257(7) 0.0010(6) 0.0020(6) 0.0055(6) C49 0.0234(8) 0.0290(8) 0.0269(7) -0.0010(6) 0.0039(6) 0.0090(7) C50 0.0255(9) 0.0346(9) 0.0416(10) -0.0018(7) 0.0081(7) 0.0059(7) C51 0.0335(10) 0.0350(9) 0.0373(9) -0.0005(7) 0.0044(8) 0.0161(8) C52 0.0217(8) 0.0265(8) 0.0282(8) -0.0023(6) 0.0008(6) 0.0061(6) C53 0.0307(10) 0.0415(10) 0.0358(9) -0.0015(7) -0.0035(7) 0.0174(8) C54 0.0277(9) 0.0358(9) 0.0380(9) -0.0056(7) 0.0060(7) 0.0006(8) S1 0.0247(2) 0.02180(19) 0.0443(2) 0.00424(16) 0.00499(17) 0.00110(16) F1 0.0483(16) 0.0639(14) 0.0590(13) 0.0056(10) -0.0141(12) 0.0032(12) F1B 0.083(8) 0.098(8) 0.102(13) 0.026(7) -0.055(10) -0.013(7) F2 0.083(2) 0.0458(12) 0.0522(12) -0.0031(9) 0.0222(14) 0.0217(14) F2B 0.124(13) 0.069(8) 0.053(4) -0.014(5) -0.005(6) 0.059(9) F3 0.093(3) 0.054(2) 0.0558(16) 0.0275(16) 0.0200(18) 0.0129(16) F3B 0.130(14) 0.056(7) 0.042(5) 0.019(5) 0.018(9) 0.024(7) O1 0.0415(8) 0.0267(6) 0.0528(8) 0.0094(6) 0.0041(6) -0.0041(6) O2 0.0259(7) 0.0284(7) 0.0949(12) 0.0168(7) 0.0035(7) 0.0025(6) O3 0.0336(7) 0.0271(6) 0.0642(9) 0.0014(6) 0.0148(7) 0.0058(6) C55 0.044(3) 0.0358(15) 0.0422(14) 0.0094(11) 0.0145(17) 0.0081(18) C55B 0.044(3) 0.0358(15) 0.0422(14) 0.0094(11) 0.0145(17) 0.0081(18) _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 Cl1 P1 2.1467(5) . ? P1 C28 1.7514(15) . ? P1 C35 1.8599(16) . ? N1 C1 1.374(2) . ? N1 C2 1.393(2) . ? N1 C4 1.440(2) . ? N2 C1 1.3762(19) . ? N2 C3 1.399(2) . ? N2 C16 1.453(2) . ? N3 C35 1.314(2) . ? N3 C38 1.5499(19) . ? N3 C43 1.4681(18) . ? C1 C28 1.437(2) . ? C2 H2 0.9300 . ? C2 C3 1.326(2) . ? C3 H3 0.9300 . ? C4 C5 1.405(2) . ? C4 C9 1.389(3) . ? C5 C6 1.391(3) . ? C5 C10 1.512(3) . ? C6 H6 0.9300 . ? C6 C7 1.388(3) . ? C7 H7 0.9300 . ? C7 C8 1.378(3) . ? C8 H8 0.9300 . ? C8 C9 1.398(3) . ? C9 C13 1.554(3) . ? C9 C13B 1.456(11) . ? C10 H10 0.9800 . ? C10 C11 1.548(3) . ? C10 C12 1.524(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.526(4) . ? C13 C15 1.528(4) . ? C13B H13B 0.9800 . ? C13B C14B 1.519(16) . ? C13B C15B 1.486(14) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16 C17 1.405(2) . ? C16 C21 1.404(2) . ? C17 C18 1.403(2) . ? C17 C22 1.519(2) . ? C18 H18 0.9300 . ? C18 C19 1.375(3) . ? C19 H19 0.9300 . ? C19 C20 1.388(3) . ? C20 H20 0.9300 . ? C20 C21 1.392(2) . ? C21 C25 1.517(2) . ? C22 H22 0.9800 . ? C22 C23 1.541(2) . ? C22 C24 1.535(2) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.540(3) . ? C25 C27 1.535(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.481(2) . ? C29 C30 1.405(2) . ? C29 C34 1.400(2) . ? C30 H30 0.9300 . ? C30 C31 1.389(2) . ? C31 H31 0.9300 . ? C31 C32 1.387(3) . ? C32 H32 0.9300 . ? C32 C33 1.387(3) . ? C33 H33 0.9300 . ? C33 C34 1.386(2) . ? C34 H34 0.9300 . ? C35 C36 1.547(2) . ? C36 C37 1.544(2) . ? C36 C39 1.531(2) . ? C36 C40 1.541(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.522(2) . ? C38 C41 1.529(2) . ? C38 C42 1.519(2) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.411(2) . ? C43 C48 1.400(2) . ? C44 C45 1.397(2) . ? C44 C49 1.523(2) . ? C45 H45 0.9300 . ? C45 C46 1.378(3) . ? C46 H46 0.9300 . ? C46 C47 1.383(3) . ? C47 H47 0.9300 . ? C47 C48 1.395(2) . ? C48 C52 1.520(2) . ? C49 H49 0.9800 . ? C49 C50 1.529(3) . ? C49 C51 1.542(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.534(2) . ? C52 C54 1.536(2) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? S1 O1 1.4395(14) . ? S1 O2 1.4320(15) . ? S1 O3 1.4371(14) . ? S1 C55 1.803(4) . ? S1 C55B 1.860(18) . ? F1 C55 1.331(5) . ? F1B C55B 1.282(19) . ? F2 C55 1.343(4) . ? F2B C55B 1.337(19) . ? F3 C55 1.341(5) . ? F3B C55B 1.341(18) . ? 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 C28 P1 Cl1 107.27(5) . . ? C28 P1 C35 104.10(7) . . ? C35 P1 Cl1 102.97(5) . . ? C1 N1 C2 110.38(13) . . ? C1 N1 C4 129.35(13) . . ? C2 N1 C4 120.26(14) . . ? C1 N2 C3 109.64(13) . . ? C1 N2 C16 132.70(13) . . ? C3 N2 C16 116.59(12) . . ? C35 N3 C38 112.33(12) . . ? C35 N3 C43 126.97(13) . . ? C43 N3 C38 119.88(11) . . ? N1 C1 N2 104.54(13) . . ? N1 C1 C28 128.74(14) . . ? N2 C1 C28 126.71(14) . . ? N1 C2 H2 126.3 . . ? C3 C2 N1 107.41(15) . . ? C3 C2 H2 126.3 . . ? N2 C3 H3 126.0 . . ? C2 C3 N2 108.02(14) . . ? C2 C3 H3 126.0 . . ? C5 C4 N1 117.74(16) . . ? C9 C4 N1 118.02(15) . . ? C9 C4 C5 123.88(16) . . ? C4 C5 C10 121.16(16) . . ? C6 C5 C4 116.80(18) . . ? C6 C5 C10 121.92(17) . . ? C5 C6 H6 119.7 . . ? C7 C6 C5 120.54(19) . . ? C7 C6 H6 119.7 . . ? C6 C7 H7 119.6 . . ? C8 C7 C6 120.77(18) . . ? C8 C7 H7 119.6 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.2(2) . . ? C9 C8 H8 119.4 . . ? C4 C9 C8 116.44(19) . . ? C4 C9 C13 119.99(19) . . ? C4 C9 C13B 138.3(5) . . ? C8 C9 C13 123.2(2) . . ? C8 C9 C13B 104.3(5) . . ? C5 C10 H10 107.9 . . ? C5 C10 C11 110.28(18) . . ? C5 C10 C12 113.64(17) . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C12 C10 C11 109.14(17) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 108.3 . . ? C14 C13 C9 110.8(2) . . ? C14 C13 H13 108.3 . . ? C14 C13 C15 110.4(2) . . ? C15 C13 C9 110.9(2) . . ? C15 C13 H13 108.3 . . ? C9 C13B H13B 107.8 . . ? C9 C13B C14B 103.5(8) . . ? C9 C13B C15B 116.7(8) . . ? C14B C13B H13B 107.8 . . ? C15B C13B H13B 107.8 . . ? C15B C13B C14B 112.8(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14E 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15E 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C17 C16 N2 116.98(14) . . ? C21 C16 N2 119.34(14) . . ? C21 C16 C17 122.57(15) . . ? C16 C17 C22 124.10(15) . . ? C18 C17 C16 116.94(16) . . ? C18 C17 C22 118.96(15) . . ? C17 C18 H18 119.2 . . ? C19 C18 C17 121.67(16) . . ? C19 C18 H18 119.2 . . ? C18 C19 H19 120.0 . . ? C18 C19 C20 119.97(17) . . ? C20 C19 H19 120.0 . . ? C19 C20 H20 119.4 . . ? C19 C20 C21 121.24(17) . . ? C21 C20 H20 119.4 . . ? C16 C21 C25 121.63(15) . . ? C20 C21 C16 117.60(15) . . ? C20 C21 C25 120.63(16) . . ? C17 C22 H22 108.2 . . ? C17 C22 C23 111.88(14) . . ? C17 C22 C24 111.03(15) . . ? C23 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C24 C22 C23 109.21(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.4 . . ? C21 C25 C26 110.00(14) . . ? C21 C25 C27 113.56(16) . . ? C26 C25 H25 107.4 . . ? C27 C25 H25 107.4 . . ? C27 C25 C26 110.70(15) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 117.01(11) . . ? C1 C28 C29 119.62(13) . . ? C29 C28 P1 122.66(11) . . ? C30 C29 C28 121.31(14) . . ? C34 C29 C28 120.92(14) . . ? C34 C29 C30 117.35(14) . . ? C29 C30 H30 119.6 . . ? C31 C30 C29 120.80(16) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 119.7 . . ? C32 C31 C30 120.69(16) . . ? C32 C31 H31 119.7 . . ? C31 C32 H32 120.4 . . ? C31 C32 C33 119.29(16) . . ? C33 C32 H32 120.4 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 120.06(17) . . ? C34 C33 H33 120.0 . . ? C29 C34 H34 119.2 . . ? C33 C34 C29 121.68(16) . . ? C33 C34 H34 119.2 . . ? N3 C35 P1 130.02(12) . . ? N3 C35 C36 110.22(13) . . ? C36 C35 P1 117.55(11) . . ? C37 C36 C35 102.60(12) . . ? C39 C36 C35 116.05(13) . . ? C39 C36 C37 112.01(14) . . ? C39 C36 C40 108.58(14) . . ? C40 C36 C35 107.82(13) . . ? C40 C36 C37 109.51(13) . . ? C36 C37 H37A 110.3 . . ? C36 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? C38 C37 C36 107.14(12) . . ? C38 C37 H37A 110.3 . . ? C38 C37 H37B 110.3 . . ? C37 C38 N3 100.07(12) . . ? C37 C38 C41 111.65(13) . . ? C41 C38 N3 109.41(12) . . ? C42 C38 N3 111.51(12) . . ? C42 C38 C37 113.56(14) . . ? C42 C38 C41 110.24(14) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 115.85(14) . . ? C48 C43 N3 121.59(14) . . ? C48 C43 C44 122.50(14) . . ? C43 C44 C49 125.23(14) . . ? C45 C44 C43 117.05(15) . . ? C45 C44 C49 117.71(14) . . ? C44 C45 H45 119.2 . . ? C46 C45 C44 121.55(16) . . ? C46 C45 H45 119.2 . . ? C45 C46 H46 120.1 . . ? C45 C46 C47 119.84(15) . . ? C47 C46 H46 120.1 . . ? C46 C47 H47 119.2 . . ? C46 C47 C48 121.65(16) . . ? C48 C47 H47 119.2 . . ? C43 C48 C52 125.48(14) . . ? C47 C48 C43 117.22(15) . . ? C47 C48 C52 117.30(15) . . ? C44 C49 H49 108.0 . . ? C44 C49 C50 111.93(14) . . ? C44 C49 C51 111.47(14) . . ? C50 C49 H49 108.0 . . ? C50 C49 C51 109.32(14) . . ? C51 C49 H49 108.0 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52 108.3 . . ? C48 C52 C53 112.29(15) . . ? C48 C52 C54 110.17(13) . . ? C53 C52 H52 108.3 . . ? C53 C52 C54 109.31(15) . . ? C54 C52 H52 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O1 S1 C55 101.61(16) . . ? O1 S1 C55B 111.6(6) . . ? O2 S1 O1 114.33(9) . . ? O2 S1 O3 114.74(9) . . ? O2 S1 C55 106.5(2) . . ? O2 S1 C55B 91.1(6) . . ? O3 S1 O1 115.75(9) . . ? O3 S1 C55 101.53(15) . . ? O3 S1 C55B 106.2(6) . . ? F1 C55 S1 112.9(3) . . ? F1 C55 F2 106.4(3) . . ? F1 C55 F3 107.7(4) . . ? F2 C55 S1 112.1(3) . . ? F3 C55 S1 111.2(3) . . ? F3 C55 F2 106.3(4) . . ? F1B C55B S1 110.3(12) . . ? F1B C55B F2B 111.0(16) . . ? F1B C55B F3B 109.3(16) . . ? F2B C55B S1 107.7(12) . . ? F2B C55B F3B 106.9(16) . . ? F3B C55B S1 111.5(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 P1 C28 C1 94.74(12) . . . . ? Cl1 P1 C28 C29 -75.55(13) . . . . ? Cl1 P1 C35 N3 -19.48(15) . . . . ? Cl1 P1 C35 C36 179.23(10) . . . . ? P1 C28 C29 C30 -143.17(13) . . . . ? P1 C28 C29 C34 29.3(2) . . . . ? P1 C35 C36 C37 162.06(11) . . . . ? P1 C35 C36 C39 -75.48(17) . . . . ? P1 C35 C36 C40 46.50(15) . . . . ? N1 C1 C28 P1 33.1(2) . . . . ? N1 C1 C28 C29 -156.25(15) . . . . ? N1 C2 C3 N2 0.6(2) . . . . ? N1 C4 C5 C6 179.98(15) . . . . ? N1 C4 C5 C10 -3.9(2) . . . . ? N1 C4 C9 C8 179.23(17) . . . . ? N1 C4 C9 C13 6.4(3) . . . . ? N1 C4 C9 C13B -14.1(7) . . . . ? N2 C1 C28 P1 -148.02(13) . . . . ? N2 C1 C28 C29 22.6(2) . . . . ? N2 C16 C17 C18 -167.30(14) . . . . ? N2 C16 C17 C22 11.7(2) . . . . ? N2 C16 C21 C20 167.67(14) . . . . ? N2 C16 C21 C25 -8.1(2) . . . . ? N3 C35 C36 C37 -2.77(17) . . . . ? N3 C35 C36 C39 119.69(16) . . . . ? N3 C35 C36 C40 -118.32(14) . . . . ? N3 C43 C44 C45 177.93(13) . . . . ? N3 C43 C44 C49 -3.2(2) . . . . ? N3 C43 C48 C47 179.94(13) . . . . ? N3 C43 C48 C52 -0.4(2) . . . . ? C1 N1 C2 C3 -0.1(2) . . . . ? C1 N1 C4 C5 -92.3(2) . . . . ? C1 N1 C4 C9 94.3(2) . . . . ? C1 N2 C3 C2 -0.87(19) . . . . ? C1 N2 C16 C17 -127.77(17) . . . . ? C1 N2 C16 C21 64.0(2) . . . . ? C1 C28 C29 C30 46.8(2) . . . . ? C1 C28 C29 C34 -140.78(15) . . . . ? C2 N1 C1 N2 -0.45(18) . . . . ? C2 N1 C1 C28 178.58(15) . . . . ? C2 N1 C4 C5 89.0(2) . . . . ? C2 N1 C4 C9 -84.5(2) . . . . ? C3 N2 C1 N1 0.79(17) . . . . ? C3 N2 C1 C28 -178.26(15) . . . . ? C3 N2 C16 C17 65.48(18) . . . . ? C3 N2 C16 C21 -102.78(17) . . . . ? C4 N1 C1 N2 -179.31(15) . . . . ? C4 N1 C1 C28 -0.3(3) . . . . ? C4 N1 C2 C3 178.91(15) . . . . ? C4 C5 C6 C7 2.5(3) . . . . ? C4 C5 C10 C11 -88.7(2) . . . . ? C4 C5 C10 C12 148.37(17) . . . . ? C4 C9 C13 C14 98.8(3) . . . . ? C4 C9 C13 C15 -138.4(2) . . . . ? C4 C9 C13B C14B 112.4(9) . . . . ? C4 C9 C13B C15B -12.1(13) . . . . ? C5 C4 C9 C8 6.2(3) . . . . ? C5 C4 C9 C13 -166.62(19) . . . . ? C5 C4 C9 C13B 172.8(7) . . . . ? C5 C6 C7 C8 2.3(3) . . . . ? C6 C5 C10 C11 87.2(2) . . . . ? C6 C5 C10 C12 -35.7(3) . . . . ? C6 C7 C8 C9 -3.1(3) . . . . ? C7 C8 C9 C4 -1.0(3) . . . . ? C7 C8 C9 C13 171.6(2) . . . . ? C7 C8 C9 C13B -171.8(5) . . . . ? C8 C9 C13 C14 -73.5(3) . . . . ? C8 C9 C13 C15 49.3(3) . . . . ? C8 C9 C13B C14B -79.9(9) . . . . ? C8 C9 C13B C15B 155.6(8) . . . . ? C9 C4 C5 C6 -7.0(3) . . . . ? C9 C4 C5 C10 169.12(18) . . . . ? C10 C5 C6 C7 -173.57(18) . . . . ? C16 N2 C1 N1 -166.63(15) . . . . ? C16 N2 C1 C28 14.3(3) . . . . ? C16 N2 C3 C2 168.82(14) . . . . ? C16 C17 C18 C19 -0.4(2) . . . . ? C16 C17 C22 C23 -110.14(18) . . . . ? C16 C17 C22 C24 127.56(16) . . . . ? C16 C21 C25 C26 78.23(19) . . . . ? C16 C21 C25 C27 -157.08(15) . . . . ? C17 C16 C21 C20 0.1(2) . . . . ? C17 C16 C21 C25 -175.67(15) . . . . ? C17 C18 C19 C20 -0.3(3) . . . . ? C18 C17 C22 C23 68.8(2) . . . . ? C18 C17 C22 C24 -53.48(19) . . . . ? C18 C19 C20 C21 1.0(3) . . . . ? C19 C20 C21 C16 -0.9(2) . . . . ? C19 C20 C21 C25 174.93(16) . . . . ? C20 C21 C25 C26 -97.40(19) . . . . ? C20 C21 C25 C27 27.3(2) . . . . ? C21 C16 C17 C18 0.6(2) . . . . ? C21 C16 C17 C22 179.53(14) . . . . ? C22 C17 C18 C19 -179.48(15) . . . . ? C28 P1 C35 N3 -131.32(14) . . . . ? C28 P1 C35 C36 67.39(12) . . . . ? C28 C29 C30 C31 169.63(15) . . . . ? C28 C29 C34 C33 -168.99(15) . . . . ? C29 C30 C31 C32 0.1(3) . . . . ? C30 C29 C34 C33 3.7(2) . . . . ? C30 C31 C32 C33 2.3(3) . . . . ? C31 C32 C33 C34 -1.7(3) . . . . ? C32 C33 C34 C29 -1.4(3) . . . . ? C34 C29 C30 C31 -3.1(2) . . . . ? C35 P1 C28 C1 -156.57(12) . . . . ? C35 P1 C28 C29 33.14(14) . . . . ? C35 N3 C38 C37 26.27(16) . . . . ? C35 N3 C38 C41 -91.11(16) . . . . ? C35 N3 C38 C42 146.68(14) . . . . ? C35 N3 C43 C44 -76.10(19) . . . . ? C35 N3 C43 C48 106.80(18) . . . . ? C35 C36 C37 C38 19.29(16) . . . . ? C36 C37 C38 N3 -26.37(15) . . . . ? C36 C37 C38 C41 89.33(15) . . . . ? C36 C37 C38 C42 -145.29(14) . . . . ? C38 N3 C35 P1 -177.38(11) . . . . ? C38 N3 C35 C36 -15.02(17) . . . . ? C38 N3 C43 C44 92.67(17) . . . . ? C38 N3 C43 C48 -84.43(18) . . . . ? C39 C36 C37 C38 -105.86(15) . . . . ? C40 C36 C37 C38 133.61(14) . . . . ? C43 N3 C35 P1 -7.9(2) . . . . ? C43 N3 C35 C36 154.45(14) . . . . ? C43 N3 C38 C37 -144.05(13) . . . . ? C43 N3 C38 C41 98.58(15) . . . . ? C43 N3 C38 C42 -23.6(2) . . . . ? C43 C44 C45 C46 3.1(2) . . . . ? C43 C44 C49 C50 109.47(18) . . . . ? C43 C44 C49 C51 -127.74(16) . . . . ? C43 C48 C52 C53 -123.41(17) . . . . ? C43 C48 C52 C54 114.49(18) . . . . ? C44 C43 C48 C47 3.0(2) . . . . ? C44 C43 C48 C52 -177.28(15) . . . . ? C44 C45 C46 C47 0.7(3) . . . . ? C45 C44 C49 C50 -71.67(18) . . . . ? C45 C44 C49 C51 51.1(2) . . . . ? C45 C46 C47 C48 -2.8(3) . . . . ? C46 C47 C48 C43 1.0(2) . . . . ? C46 C47 C48 C52 -178.76(15) . . . . ? C47 C48 C52 C53 56.3(2) . . . . ? C47 C48 C52 C54 -65.83(19) . . . . ? C48 C43 C44 C45 -5.0(2) . . . . ? C48 C43 C44 C49 173.88(15) . . . . ? C49 C44 C45 C46 -175.89(15) . . . . ? O1 S1 C55 F1 62.1(3) . . . . ? O1 S1 C55 F2 -58.0(3) . . . . ? O1 S1 C55 F3 -176.7(3) . . . . ? O1 S1 C55B F1B 58.8(15) . . . . ? O1 S1 C55B F2B -62.5(12) . . . . ? O1 S1 C55B F3B -179.4(12) . . . . ? O2 S1 C55 F1 -177.9(2) . . . . ? O2 S1 C55 F2 62.0(3) . . . . ? O2 S1 C55 F3 -56.8(4) . . . . ? O2 S1 C55B F1B 175.7(14) . . . . ? O2 S1 C55B F2B 54.3(12) . . . . ? O2 S1 C55B F3B -62.6(13) . . . . ? O3 S1 C55 F1 -57.5(3) . . . . ? O3 S1 C55 F2 -177.6(2) . . . . ? O3 S1 C55 F3 63.6(4) . . . . ? O3 S1 C55B F1B -68.1(15) . . . . ? O3 S1 C55B F2B 170.6(11) . . . . ? O3 S1 C55B F3B 53.6(14) . . . . ? _shelx_res_file ; TITL sharma43_a.res in P-1 sharma43.res created by SHELXL-2018/3 at 10:32:37 on 01-Jul-2019 REM Old TITL sharma43 in P-1 REM SHELXT solution in P-1: R1 0.143, Rweak 0.006, Alpha 0.048 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C30 N1 O2 F1 P Cl2 CELL 1.54184 11.0592 12.9006 18.7834 98.063 91.131 103.315 ZERR 2 0.0004 0.0003 0.0005 0.002 0.002 0.003 LATT 1 SFAC C H Cl F N O P S UNIT 110 144 2 6 6 6 2 2 RIGU F1 > C55B EADP C55B C55 EADP C13 C13B L.S. 11 PLAN 5 SIZE 0.03 0.312 0.499 MORE -1 BOND $H CONF fmap 2 acta OMIT 0 0 4 OMIT -10 11 9 OMIT 8 5 14 OMIT 8 -3 19 REM REM REM WGHT 0.060400 0.987000 FVAR 4.90107 0.78271 0.78925 CL1 3 0.861307 0.575710 0.386207 11.00000 0.03678 0.02142 = 0.02342 0.00181 0.00102 0.00813 P1 7 0.760813 0.552633 0.284061 11.00000 0.02226 0.01706 = 0.02185 0.00066 0.00432 0.00529 N1 5 0.630050 0.305917 0.222218 11.00000 0.01958 0.01881 = 0.03509 -0.00179 0.00680 0.00233 N2 5 0.806569 0.261343 0.205424 11.00000 0.02062 0.01409 = 0.02634 0.00074 0.00547 0.00279 N3 5 0.874920 0.778145 0.286211 11.00000 0.02070 0.01709 = 0.02211 0.00128 0.00395 0.00688 C1 1 0.755101 0.349209 0.218559 11.00000 0.01942 0.01823 = 0.02173 0.00045 0.00430 0.00339 C2 1 0.605407 0.193825 0.210990 11.00000 0.02524 0.01797 = 0.04156 -0.00235 0.00939 -0.00273 AFIX 43 H2 2 0.527835 0.146735 0.210972 11.00000 -1.20000 AFIX 0 C3 1 0.712867 0.166622 0.200334 11.00000 0.02610 0.01574 = 0.03519 0.00069 0.00861 0.00041 AFIX 43 H3 2 0.724000 0.096791 0.191093 11.00000 -1.20000 AFIX 0 C4 1 0.530074 0.359664 0.234149 11.00000 0.01663 0.02341 = 0.03871 0.00020 0.00667 0.00148 C5 1 0.496682 0.382829 0.305394 11.00000 0.02286 0.02385 = 0.04137 0.00156 0.01032 0.00311 C6 1 0.399901 0.434807 0.315708 11.00000 0.02804 0.02915 = 0.05554 0.00075 0.01670 0.00660 AFIX 43 H6 2 0.376848 0.454230 0.362126 11.00000 -1.20000 AFIX 0 C7 1 0.337481 0.457913 0.257311 11.00000 0.02435 0.04062 = 0.08056 0.01408 0.01462 0.01341 AFIX 43 H7 2 0.274987 0.495018 0.265088 11.00000 -1.20000 AFIX 0 C8 1 0.366996 0.426532 0.187947 11.00000 0.02170 0.05654 = 0.06619 0.02165 0.00461 0.00966 AFIX 43 H8 2 0.321306 0.439672 0.149502 11.00000 -1.20000 AFIX 0 C9 1 0.464406 0.375282 0.174305 11.00000 0.01904 0.04346 = 0.04630 0.00595 0.00328 0.00096 C10 1 0.557807 0.346168 0.366904 11.00000 0.03531 0.03797 = 0.03776 0.00608 0.01394 0.00991 AFIX 13 H10 2 0.642128 0.342167 0.353811 11.00000 -1.20000 AFIX 0 C11 1 0.486056 0.232005 0.377984 11.00000 0.06713 0.03704 = 0.05232 0.01148 0.02025 0.01251 AFIX 137 H11A 2 0.402058 0.233265 0.389233 11.00000 -1.50000 H11B 2 0.526115 0.209450 0.416903 11.00000 -1.50000 H11C 2 0.485497 0.182500 0.334686 11.00000 -1.50000 AFIX 0 C12 1 0.568440 0.422145 0.437813 11.00000 0.05402 0.05078 = 0.03727 0.00182 0.01561 0.00383 AFIX 137 H12A 2 0.605501 0.494404 0.430155 11.00000 -1.50000 H12B 2 0.619445 0.400876 0.472370 11.00000 -1.50000 H12C 2 0.487071 0.419010 0.455576 11.00000 -1.50000 AFIX 0 PART 1 C13 1 0.490323 0.324796 0.097716 21.00000 0.02573 0.02909 = 0.04097 0.00063 0.00078 0.00672 AFIX 13 H13 2 0.572199 0.307962 0.099919 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C13B 1 0.477469 0.370195 0.096968 -21.00000 0.02573 0.02909 = 0.04097 0.00063 0.00078 0.00672 AFIX 13 H13B 2 0.458397 0.435124 0.082675 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C14 1 0.393291 0.220295 0.072345 21.00000 0.03761 0.03740 = 0.05421 -0.00884 0.00761 -0.00306 AFIX 137 H14A 2 0.393578 0.170870 0.106055 21.00000 -1.50000 H14B 2 0.412808 0.188934 0.025847 21.00000 -1.50000 H14C 2 0.312454 0.235349 0.069173 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C14B 1 0.373796 0.274568 0.065221 -21.00000 0.04544 0.06634 = 0.04628 0.00950 -0.00632 -0.00661 AFIX 137 H14D 2 0.380030 0.212690 0.086817 -21.00000 -1.50000 H14E 2 0.381125 0.259620 0.014172 -21.00000 -1.50000 H14F 2 0.294708 0.290955 0.074611 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C15 1 0.492845 0.404067 0.044194 21.00000 0.05432 0.03913 = 0.03522 -0.00260 -0.00820 0.00332 AFIX 137 H15A 2 0.413197 0.421426 0.041216 21.00000 -1.50000 H15B 2 0.511160 0.372006 -0.002384 21.00000 -1.50000 H15C 2 0.555765 0.468587 0.060115 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C15B 1 0.601119 0.362482 0.070236 -21.00000 0.04016 0.03993 = 0.02907 0.00050 -0.00102 0.00316 AFIX 137 H15D 2 0.663895 0.422170 0.094190 -21.00000 -1.50000 H15E 2 0.600425 0.364022 0.019281 -21.00000 -1.50000 H15F 2 0.618927 0.296272 0.079964 -21.00000 -1.50000 AFIX 0 PART 0 C16 1 0.934080 0.249687 0.208819 11.00000 0.02193 0.01359 = 0.03160 0.00428 0.00765 0.00394 C17 1 0.974436 0.193941 0.147587 11.00000 0.02636 0.01528 = 0.03312 0.00392 0.01100 0.00299 C18 1 1.087150 0.163370 0.155562 11.00000 0.02687 0.02111 = 0.04303 0.00344 0.01363 0.00692 AFIX 43 H18 2 1.116268 0.125913 0.116192 11.00000 -1.20000 AFIX 0 C19 1 1.155703 0.187382 0.220129 11.00000 0.02310 0.02641 = 0.05243 0.00525 0.00717 0.00720 AFIX 43 H19 2 1.229964 0.165908 0.224084 11.00000 -1.20000 AFIX 0 C20 1 1.113998 0.243691 0.279398 11.00000 0.02549 0.02396 = 0.04319 0.00390 -0.00032 0.00477 AFIX 43 H20 2 1.161601 0.260552 0.322637 11.00000 -1.20000 AFIX 0 C21 1 1.002274 0.275381 0.275317 11.00000 0.02755 0.01546 = 0.03173 0.00267 0.00332 0.00443 C22 1 0.902823 0.163984 0.074909 11.00000 0.03534 0.01956 = 0.02878 0.00065 0.00945 0.00780 AFIX 13 H22 2 0.833661 0.199882 0.076806 11.00000 -1.20000 AFIX 0 C23 1 0.848411 0.041573 0.056570 11.00000 0.04337 0.02137 = 0.03624 -0.00133 0.00552 0.00702 AFIX 137 H23A 2 0.914443 0.004646 0.057097 11.00000 -1.50000 H23B 2 0.806820 0.025489 0.009602 11.00000 -1.50000 H23C 2 0.790081 0.018347 0.091590 11.00000 -1.50000 AFIX 0 C24 1 0.985859 0.202491 0.014739 11.00000 0.05601 0.02644 = 0.03257 0.00193 0.01825 0.01262 AFIX 137 H24A 2 1.023393 0.277992 0.027155 11.00000 -1.50000 H24B 2 0.936356 0.190413 -0.029523 11.00000 -1.50000 H24C 2 1.049765 0.163154 0.008949 11.00000 -1.50000 AFIX 0 C25 1 0.952639 0.328676 0.341995 11.00000 0.03866 0.02766 = 0.02703 0.00209 0.00016 0.01479 AFIX 13 H25 2 0.909921 0.381215 0.326806 11.00000 -1.20000 AFIX 0 C26 1 0.855443 0.244516 0.374187 11.00000 0.04107 0.04687 = 0.02927 0.01083 0.00693 0.01885 AFIX 137 H26A 2 0.787875 0.212729 0.339231 11.00000 -1.50000 H26B 2 0.824435 0.278890 0.416274 11.00000 -1.50000 H26C 2 0.893436 0.189472 0.387121 11.00000 -1.50000 AFIX 0 C27 1 1.054718 0.389756 0.399213 11.00000 0.05590 0.03200 = 0.03483 -0.00238 -0.00962 0.01791 AFIX 137 H27A 2 1.092703 0.339375 0.418836 11.00000 -1.50000 H27B 2 1.018735 0.428973 0.437016 11.00000 -1.50000 H27C 2 1.116571 0.439129 0.377581 11.00000 -1.50000 AFIX 0 C28 1 0.819887 0.460622 0.225436 11.00000 0.02116 0.01652 = 0.02239 0.00110 0.00433 0.00411 C29 1 0.941523 0.490529 0.192838 11.00000 0.01971 0.01534 = 0.02685 0.00475 0.00467 0.00634 C30 1 0.959263 0.447354 0.121975 11.00000 0.02634 0.01772 = 0.02894 0.00331 0.00661 0.00633 AFIX 43 H30 2 0.898488 0.390643 0.097531 11.00000 -1.20000 AFIX 0 C31 1 1.066455 0.488330 0.087977 11.00000 0.03482 0.02242 = 0.03517 0.00612 0.01466 0.01025 AFIX 43 H31 2 1.076601 0.458856 0.041010 11.00000 -1.20000 AFIX 0 C32 1 1.158541 0.572748 0.123329 11.00000 0.02707 0.02427 = 0.05149 0.00980 0.01804 0.00642 AFIX 43 H32 2 1.228784 0.601596 0.099744 11.00000 -1.20000 AFIX 0 C33 1 1.144745 0.613689 0.194241 11.00000 0.02164 0.02073 = 0.04862 0.00287 0.00485 0.00304 AFIX 43 H33 2 1.206933 0.669039 0.218827 11.00000 -1.20000 AFIX 0 C34 1 1.038371 0.572182 0.228481 11.00000 0.02185 0.01806 = 0.03330 0.00160 0.00302 0.00625 AFIX 43 H34 2 1.031152 0.599273 0.276362 11.00000 -1.20000 AFIX 0 C35 1 0.818931 0.683355 0.250805 11.00000 0.01834 0.01955 = 0.02247 0.00011 0.00402 0.00732 C36 1 0.766792 0.695776 0.176256 11.00000 0.02881 0.02008 = 0.02255 0.00086 -0.00013 0.00893 C37 1 0.799229 0.819136 0.178061 11.00000 0.03443 0.02118 = 0.02546 0.00336 0.00183 0.01148 AFIX 23 H37A 2 0.827649 0.837252 0.131843 11.00000 -1.20000 H37B 2 0.726582 0.847561 0.188626 11.00000 -1.20000 AFIX 0 C38 1 0.901807 0.866485 0.236749 11.00000 0.02909 0.01686 = 0.02481 0.00470 0.00510 0.00791 C39 1 0.817504 0.637939 0.110863 11.00000 0.04329 0.02874 = 0.02253 0.00213 0.00243 0.01749 AFIX 137 H39A 2 0.906756 0.659329 0.113834 11.00000 -1.50000 H39B 2 0.786231 0.656739 0.067601 11.00000 -1.50000 H39C 2 0.791330 0.561474 0.110139 11.00000 -1.50000 AFIX 0 C40 1 0.624318 0.653601 0.173520 11.00000 0.02985 0.02669 = 0.03263 -0.00310 -0.00703 0.00943 AFIX 137 H40A 2 0.604274 0.577248 0.174025 11.00000 -1.50000 H40B 2 0.588598 0.668655 0.130240 11.00000 -1.50000 H40C 2 0.591339 0.688631 0.214590 11.00000 -1.50000 AFIX 0 C41 1 1.030990 0.873487 0.207433 11.00000 0.03230 0.02389 = 0.03107 0.00726 0.00962 0.00892 AFIX 137 H41A 2 1.093330 0.906344 0.245269 11.00000 -1.50000 H41B 2 1.040645 0.916134 0.169034 11.00000 -1.50000 H41C 2 1.040101 0.802381 0.189591 11.00000 -1.50000 AFIX 0 C42 1 0.893207 0.975313 0.276547 11.00000 0.03293 0.01737 = 0.03144 0.00292 0.00563 0.00710 AFIX 137 H42A 2 0.809924 0.971371 0.291427 11.00000 -1.50000 H42B 2 0.914174 1.028810 0.245231 11.00000 -1.50000 H42C 2 0.950089 0.994517 0.318126 11.00000 -1.50000 AFIX 0 C43 1 0.893352 0.808389 0.364657 11.00000 0.02537 0.01491 = 0.02099 0.00079 0.00225 0.00536 C44 1 0.787714 0.825188 0.401262 11.00000 0.02461 0.01840 = 0.02564 0.00062 0.00345 0.00494 C45 1 0.801551 0.850547 0.476191 11.00000 0.02871 0.02491 = 0.02626 0.00019 0.00692 0.00839 AFIX 43 H45 2 0.732740 0.858705 0.502140 11.00000 -1.20000 AFIX 0 C46 1 0.914774 0.863766 0.512583 11.00000 0.03728 0.02722 = 0.02200 -0.00049 0.00208 0.00956 AFIX 43 H46 2 0.921636 0.879899 0.562545 11.00000 -1.20000 AFIX 0 C47 1 1.018146 0.852985 0.474631 11.00000 0.02840 0.02688 = 0.02628 0.00090 -0.00132 0.00774 AFIX 43 H47 2 1.094848 0.865157 0.499503 11.00000 -1.20000 AFIX 0 C48 1 1.010262 0.824313 0.399984 11.00000 0.02452 0.01819 = 0.02567 0.00098 0.00200 0.00547 C49 1 0.661157 0.819774 0.365493 11.00000 0.02340 0.02897 = 0.02690 -0.00096 0.00389 0.00902 AFIX 13 H49 2 0.670218 0.814786 0.313410 11.00000 -1.20000 AFIX 0 C50 1 0.563565 0.720667 0.379424 11.00000 0.02551 0.03458 = 0.04158 -0.00176 0.00814 0.00595 AFIX 137 H50A 2 0.591682 0.656823 0.362881 11.00000 -1.50000 H50B 2 0.486471 0.718040 0.354035 11.00000 -1.50000 H50C 2 0.551261 0.724907 0.430103 11.00000 -1.50000 AFIX 0 C51 1 0.614622 0.922016 0.390891 11.00000 0.03350 0.03500 = 0.03728 -0.00048 0.00436 0.01608 AFIX 137 H51A 2 0.594029 0.923377 0.440372 11.00000 -1.50000 H51B 2 0.542087 0.921692 0.361850 11.00000 -1.50000 H51C 2 0.678779 0.984630 0.386263 11.00000 -1.50000 AFIX 0 C52 1 1.129140 0.812444 0.363853 11.00000 0.02170 0.02646 = 0.02823 -0.00233 0.00082 0.00607 AFIX 13 H52 2 1.108603 0.787074 0.312421 11.00000 -1.20000 AFIX 0 C53 1 1.188948 0.731060 0.394732 11.00000 0.03068 0.04155 = 0.03583 -0.00152 -0.00353 0.01741 AFIX 137 H53A 2 1.218868 0.758837 0.443601 11.00000 -1.50000 H53B 2 1.257189 0.719158 0.366454 11.00000 -1.50000 H53C 2 1.128228 0.664240 0.393473 11.00000 -1.50000 AFIX 0 C54 1 1.223199 0.922023 0.371880 11.00000 0.02771 0.03585 = 0.03796 -0.00557 0.00597 0.00065 AFIX 137 H54A 2 1.184752 0.973933 0.354579 11.00000 -1.50000 H54B 2 1.293958 0.915267 0.344376 11.00000 -1.50000 H54C 2 1.249668 0.945348 0.421701 11.00000 -1.50000 AFIX 0 S1 8 0.434070 0.911981 0.201970 11.00000 0.02467 0.02180 = 0.04433 0.00424 0.00499 0.00110 PART 1 F1 4 0.259324 0.840266 0.098562 31.00000 0.04826 0.06387 = 0.05898 0.00559 -0.01412 0.00318 PART 0 PART 2 F1B 4 0.313258 0.844444 0.077769 -31.00000 0.08307 0.09789 = 0.10182 0.02569 -0.05457 -0.01255 PART 0 PART 1 F2 4 0.424388 0.782719 0.080040 31.00000 0.08339 0.04584 = 0.05223 -0.00314 0.02222 0.02165 PART 0 PART 2 F2B 4 0.497358 0.814875 0.082624 -31.00000 0.12428 0.06900 = 0.05282 -0.01364 -0.00484 0.05892 PART 0 PART 1 F3 4 0.425283 0.946248 0.068690 31.00000 0.09322 0.05404 = 0.05577 0.02747 0.01999 0.01294 PART 0 PART 2 F3B 4 0.472946 0.973160 0.073117 -31.00000 0.12978 0.05569 = 0.04215 0.01896 0.01842 0.02402 PART 0 O1 6 0.384933 0.816050 0.233019 11.00000 0.04152 0.02665 = 0.05284 0.00945 0.00414 -0.00410 O2 6 0.567163 0.943202 0.203988 11.00000 0.02593 0.02842 = 0.09493 0.01682 0.00351 0.00248 O3 6 0.374340 0.999209 0.220472 11.00000 0.03364 0.02708 = 0.06419 0.00136 0.01483 0.00580 PART 1 C55 1 0.382673 0.868497 0.108626 31.00000 0.04448 0.03579 = 0.04221 0.00935 0.01446 0.00813 PART 0 PART 2 C55B 1 0.426105 0.883871 0.101924 -31.00000 0.04448 0.03579 = 0.04221 0.00935 0.01446 0.00813 HKLF 4 REM sharma43_a.res in P-1 REM wR2 = 0.1182, GooF = S = 1.082, Restrained GooF = 1.082 for all data REM R1 = 0.0420 for 9327 Fo > 4sig(Fo) and 0.0483 for all 10686 data REM 675 parameters refined using 36 restraints END WGHT 0.0604 0.9873 REM Highest difference peak 0.445, deepest hole -0.475, 1-sigma level 0.051 Q1 1 0.4414 0.8956 0.1527 11.00000 0.05 0.45 Q2 1 0.3819 0.4817 0.2131 11.00000 0.05 0.39 Q3 1 0.3952 0.8000 0.1861 11.00000 0.05 0.36 Q4 1 0.5644 0.9364 0.1543 11.00000 0.05 0.34 Q5 1 0.4416 0.4229 0.1847 11.00000 0.05 0.31 ; _shelx_res_checksum 61266 _olex2_date_sample_data_collection 2019-06-28 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.878 _oxdiff_exptl_absorpt_empirical_full_min 0.376 ####################################################################### # # 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_compound9 _database_code_depnum_ccdc_archive 'CCDC 1951632' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-09-05 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-08-27 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' ? _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'Cl7 Ga2, Cl4 Ga, 2(C H2 Cl2), C57 H76 N3 P' _chemical_formula_sum 'C59 H80 Cl15 Ga3 N3 P' _chemical_formula_weight 1603.14 _chemical_melting_point ? _chemical_oxdiff_formula 'C236 H320 Cl60 Ga12 N12 P4 ' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.16275(15) _cell_length_b 13.46701(10) _cell_length_c 28.2924(2) _cell_angle_alpha 90 _cell_angle_beta 94.5840(7) _cell_angle_gamma 90 _cell_volume 7277.92(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 76826 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 76.2540 _cell_measurement_theta_min 3.0950 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 6.866 _exptl_absorpt_correction_T_max 0.716 _exptl_absorpt_correction_T_min 0.169 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 3272 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -11 3 7 0.1027 11 -3 -7 0.1027 10 0 -12 0.0937 0 -8 7 0.1903 0 8 -7 0.1903 -12 0 -4 0.1033 12 0 4 0.1033 1 -6 13 0.1754 7 6 -10 0.1613 -3 6 -13 0.1769 -7 2 15 0.1034 7 -2 -15 0.1034 6 2 -17 0.0983 -3 -5 14 0.1776 -7 6 11 0.1164 -1 2 -18 0.1083 5 5 13 0.1278 2 -1 18 0.1611 -4 -4 -15 0.1566 2 -3 -17 0.1212 -1 8 8 0.1363 -3 -1 18 0.1383 -2 6 14 0.1166 _exptl_crystal_size_max 0.423 _exptl_crystal_size_mid 0.291 _exptl_crystal_size_min 0.205 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -11.0186 2.8425 7.3667 -0.4252 -0.8921 -0.1526 11.0186 -2.8425 -7.3667 0.4252 0.8921 0.1526 10.2751 0.2361 -11.5253 0.3595 0.7537 0.5501 0.0146 -8.0837 6.9631 -0.0728 0.3891 -0.9183 -0.0146 8.0837 -6.9631 0.0728 -0.3891 0.9183 -11.8134 -0.1726 -4.3328 -0.9235 -0.3830 0.0225 11.8134 0.1726 4.3328 0.9235 0.3830 -0.0225 1.1277 -5.9270 13.2145 0.2583 0.1078 -0.9600 7.0412 5.8217 -9.7344 0.3868 0.1597 0.9082 -2.7406 5.5957 -13.1432 -0.3755 -0.1564 0.9135 -6.8275 2.3957 15.2618 0.0707 -0.8971 -0.4362 6.8275 -2.3957 -15.2618 -0.0707 0.8971 0.4362 5.6855 1.6656 -16.5750 -0.0463 0.5910 0.8053 -3.2263 -5.3495 14.0574 0.0111 -0.1476 -0.9890 -6.5270 5.5518 11.1456 0.0788 -0.9966 -0.0230 -1.2042 1.5117 -17.7956 -0.5486 0.3350 0.7661 4.6074 5.1709 12.5660 0.8528 -0.5221 0.0092 1.7128 -0.6816 17.8680 0.6132 -0.3747 -0.6954 -4.1362 -3.9820 -14.6264 -0.8407 0.5145 0.1689 2.4397 -3.2216 -16.9196 -0.4413 0.8111 0.3839 -0.8757 7.7807 8.3470 0.4519 -0.8322 0.3212 -2.8290 -0.6988 18.0972 0.3152 -0.5783 -0.7525 -1.8018 5.7901 13.6664 0.4770 -0.8776 -0.0472 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 160048 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.755 _diffrn_reflns_theta_min 3.134 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -64.00 30.00 1.00 2.50 -- -38.50 57.00-120.00 94 2 \w -59.00 33.00 1.00 2.50 -- -38.50 38.00 60.00 92 3 \w 12.00 42.00 1.00 2.50 -- 42.70 80.00 31.89 30 4 \w 27.00 97.00 1.00 2.50 -- 42.70-125.00 90.00 70 5 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 -90.00 92 6 \w -28.00 63.00 1.00 2.50 -- 42.70 -38.00 60.00 91 7 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 120.00 92 8 \w 6.00 81.00 1.00 2.50 -- 42.70 -99.00 -60.00 75 9 \w 11.00 42.00 1.00 2.50 -- 42.70 81.00-144.67 31 10 \w 12.00 42.00 1.00 2.50 -- 42.70 78.00 69.28 30 11 \w 16.00 111.00 1.00 2.50 -- 42.70 63.00 147.36 95 12 \w 12.00 42.00 1.00 2.50 -- 42.70 80.00 -73.76 30 13 \w 13.00 42.00 1.00 2.50 -- 42.70 77.00-102.84 29 14 \w 11.00 42.00 1.00 2.50 -- 42.70 82.00 104.52 31 15 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 -30.00 92 16 \w 18.00 111.00 1.00 2.50 -- 42.70 57.00 0.00 93 17 \w 12.00 42.00 1.00 2.50 -- 42.70 79.00 -16.56 30 18 \w 11.00 42.00 1.00 2.50 -- 42.70 81.00 153.00 31 19 \w 85.00 178.00 1.00 10.00 -- 111.00 60.00-138.31 93 20 \w 86.00 178.00 1.00 10.00 -- 111.00 57.00 -98.41 92 21 \w 85.00 156.00 1.00 10.00 -- 111.00 61.00 -49.16 71 22 \w 82.00 108.00 1.00 10.00 -- 111.00 72.00 55.67 26 23 \w 86.00 162.00 1.00 10.00 -- 111.00 55.00 86.24 76 24 \w 82.00 109.00 1.00 10.00 -- 111.00 72.00 -85.23 27 25 \w 146.00 173.00 1.00 10.00 -- 111.00 72.00 55.67 27 26 \w 82.00 176.00 1.00 10.00 -- 111.00 72.00 36.97 94 27 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 -39.74 27 28 \w 82.00 109.00 1.00 10.00 -- 111.00 72.00 -30.57 27 29 \w 83.00 109.00 1.00 10.00 -- 111.00 68.00 -13.20 26 30 \w 44.00 136.00 1.00 10.00 -- 111.00 -61.00 0.00 92 31 \w 86.00 159.00 1.00 10.00 -- 111.00 61.00 -83.73 73 32 \w 85.00 158.00 1.00 10.00 -- 111.00 62.00 -66.44 73 33 \w 87.00 114.00 1.00 10.00 -- 111.00 53.00-152.47 27 34 \w 144.00 177.00 1.00 10.00 -- 111.00 57.00-122.94 33 35 \w 86.00 112.00 1.00 10.00 -- 111.00 57.00-122.94 26 36 \w 88.00 170.00 1.00 10.00 -- 111.00 47.00 30.60 82 37 \w 120.00 176.00 1.00 10.00 -- 111.00 58.00 137.18 56 38 \w 86.00 112.00 1.00 10.00 -- 111.00 58.00 137.18 26 39 \w 87.00 178.00 1.00 10.00 -- 111.00 50.00 154.95 91 40 \w 83.00 176.00 1.00 10.00 -- 111.00 67.00 170.59 93 41 \w 31.00 107.00 1.00 10.00 -- 111.00 -94.00-180.00 76 42 \w 31.00 105.00 1.00 10.00 -- 111.00 -94.00 0.00 74 43 \w 83.00 109.00 1.00 10.00 -- 111.00 69.00 -64.25 26 44 \w 61.00 107.00 1.00 10.00 -- 111.00-104.00 -34.71 46 45 \w 81.00 108.00 1.00 10.00 -- 111.00-103.00 -95.02 27 46 \w 123.00 178.00 1.00 10.00 -- 111.00 65.00 1.26 55 47 \w 82.00 109.00 1.00 10.00 -- 111.00 73.00 20.39 27 48 \w 83.00 113.00 1.00 10.00 -- 111.00 68.00 157.81 30 49 \w 85.00 177.00 1.00 10.00 -- 111.00 61.00-150.00 92 50 \w 43.00 134.00 1.00 10.00 -- 111.00 -61.00-180.00 91 51 \w 85.00 111.00 1.00 10.00 -- 111.00 61.00 90.00 26 52 \w 84.00 110.00 1.00 10.00 -- 111.00 64.00 24.00 26 53 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 -90.00 27 54 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 60.00 27 55 \w 83.00 109.00 1.00 10.00 -- 111.00-110.00 80.98 26 56 \w 86.00 113.00 1.00 10.00 -- 111.00 61.00-120.00 27 57 \w 152.00 178.00 1.00 10.00 -- 111.00 61.00-120.00 26 58 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 150.00 27 59 \w 84.00 110.00 1.00 10.00 -- 111.00 65.00 1.26 26 60 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 120.00 27 61 \w 42.00 113.00 1.00 10.00 -- 111.00-125.00-180.00 71 62 \w 39.00 66.00 1.00 10.00 -- 111.00-110.00 80.98 27 63 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00 -30.00 93 64 \w 82.00 177.00 1.00 10.00 -- 111.00 74.00 90.37 95 65 \w 85.00 111.00 1.00 10.00 -- 111.00 60.00 117.47 26 66 \w 86.00 112.00 1.00 10.00 -- 111.00 55.00-162.16 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0669592000 _diffrn_orient_matrix_UB_12 0.0342859000 _diffrn_orient_matrix_UB_13 0.0292074000 _diffrn_orient_matrix_UB_21 0.0437088000 _diffrn_orient_matrix_UB_22 -0.0720993000 _diffrn_orient_matrix_UB_23 -0.0279082000 _diffrn_orient_matrix_UB_31 0.0103903000 _diffrn_orient_matrix_UB_32 0.0819262000 _diffrn_orient_matrix_UB_33 -0.0367911000 _diffrn_oxdiff_digest_frames ; 01daf365e99f952ddea88f8f2f0b0a13620353757c2 ; _diffrn_oxdiff_digest_hkl ; 01b4283c6e2c41b5797aef955c991bd4411373 ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _diffrn_special_details ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 14273 _reflns_number_total 15269 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _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 0.680 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef 0.000055(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 745 _refine_ls_number_reflns 15269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0360 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+7.1390P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.0974 _refine_special_details 'Hydrogen atoms were taken into account using a riding model.' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C20(H20), C23(H23), C32(H32), C35(H35), C50(H50), C53(H53) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C58(H58A,H58B), C59(H59A,H59B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29), C30(H30), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48) 2.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B, H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A, H37B,H37C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C) ; _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 Ga1 Ga 0.33334(2) 0.03730(2) 0.35547(2) 0.02802(7) Uani 1 1 d . . . . . Ga2 Ga 0.38626(2) 0.30060(2) 0.39481(2) 0.02400(7) Uani 1 1 d . . . . . Ga3 Ga 0.00011(2) 0.27450(2) 0.61325(2) 0.02036(7) Uani 1 1 d . . . . . Cl1 Cl 0.25572(4) 0.12190(5) 0.31471(3) 0.05227(19) Uani 1 1 d . . . . . Cl2 Cl 0.42581(4) 0.01327(5) 0.31869(2) 0.04114(14) Uani 1 1 d . . . . . Cl3 Cl 0.29617(4) -0.09217(5) 0.38937(2) 0.04318(15) Uani 1 1 d . . . . . Cl4 Cl 0.36993(3) 0.13809(4) 0.41940(2) 0.02630(11) Uani 1 1 d . . . . . Cl5 Cl 0.28477(3) 0.36585(5) 0.38626(3) 0.04275(15) Uani 1 1 d . . . . . Cl6 Cl 0.44323(4) 0.29271(6) 0.33321(2) 0.04900(18) Uani 1 1 d . . . . . Cl7 Cl 0.44666(3) 0.35896(4) 0.45570(2) 0.03709(13) Uani 1 1 d . . . . . Cl8 Cl 0.00733(3) 0.30873(5) 0.53850(2) 0.03464(13) Uani 1 1 d . . . . . Cl9 Cl 0.10540(3) 0.27472(4) 0.64844(2) 0.02626(11) Uani 1 1 d . . . . . Cl10 Cl -0.05733(3) 0.39166(4) 0.64662(2) 0.02369(10) Uani 1 1 d . . . . . Cl11 Cl -0.05208(3) 0.13406(4) 0.62126(2) 0.03223(12) Uani 1 1 d . . . . . Cl12 Cl 0.20415(3) 0.27656(5) 0.54048(2) 0.04006(14) Uani 1 1 d . . . . . Cl13 Cl 0.35679(3) 0.26816(5) 0.55513(3) 0.04128(15) Uani 1 1 d . . . . . Cl14 Cl 0.51756(4) 0.19010(5) 0.60785(3) 0.04695(16) Uani 1 1 d . . . . . Cl15 Cl 0.54597(3) 0.39445(4) 0.58089(2) 0.03536(13) Uani 1 1 d . . . . . P1 P 0.74059(2) 0.22033(3) 0.33895(2) 0.01584(10) Uani 1 1 d . . . . . N1 N 0.90791(8) 0.35114(12) 0.37203(6) 0.0159(3) Uani 1 1 d . . . . . N2 N 0.81830(8) 0.40495(12) 0.40712(6) 0.0153(3) Uani 1 1 d . . . . . N3 N 0.69435(8) 0.03333(12) 0.31077(6) 0.0163(3) Uani 1 1 d . . . . . C1 C 0.84391(10) 0.32600(14) 0.38428(6) 0.0145(3) Uani 1 1 d . . . . . C2 C 0.92381(10) 0.44618(15) 0.38777(7) 0.0199(4) Uani 1 1 d . . . . . H2 H 0.965753 0.481699 0.383724 0.024 Uiso 1 1 calc R . . . . C3 C 0.86835(11) 0.47912(15) 0.41005(7) 0.0199(4) Uani 1 1 d . . . . . H3 H 0.864501 0.541836 0.424993 0.024 Uiso 1 1 calc R . . . . C4 C 0.81290(10) 0.22605(14) 0.37727(6) 0.0147(3) Uani 1 1 d . . . . . C5 C 0.70449(9) 0.09416(14) 0.34642(6) 0.0152(3) Uani 1 1 d . . . . . C6 C 0.65503(11) -0.06144(15) 0.32414(7) 0.0224(4) Uani 1 1 d . . . . . C7 C 0.61911(11) -0.02256(16) 0.36691(7) 0.0219(4) Uani 1 1 d . . . . . H7A H 0.616131 -0.075829 0.390778 0.026 Uiso 1 1 calc R . . . . H7B H 0.571081 0.000199 0.356864 0.026 Uiso 1 1 calc R . . . . C8 C 0.66336(10) 0.06477(15) 0.38823(7) 0.0168(4) Uani 1 1 d . . . . . C9 C 0.70928(11) 0.03718(16) 0.43370(7) 0.0210(4) Uani 1 1 d . . . . . H9A H 0.738331 -0.021356 0.427315 0.025 Uiso 1 1 calc R . . . . H9B H 0.741149 0.093081 0.442738 0.025 Uiso 1 1 calc R . . . . C10 C 0.66452(12) 0.01363(18) 0.47503(7) 0.0258(4) Uani 1 1 d . . . . . H10A H 0.636374 -0.046744 0.467393 0.031 Uiso 1 1 calc R . . . . H10B H 0.695635 -0.000095 0.503925 0.031 Uiso 1 1 calc R . . . . C11 C 0.61594(13) 0.09919(19) 0.48464(8) 0.0308(5) Uani 1 1 d . . . . . H11A H 0.644069 0.157261 0.496152 0.037 Uiso 1 1 calc R . . . . H11B H 0.585494 0.079746 0.509758 0.037 Uiso 1 1 calc R . . . . C12 C 0.57068(12) 0.12771(19) 0.44002(9) 0.0306(5) Uani 1 1 d . . . . . H12A H 0.540994 0.185291 0.446861 0.037 Uiso 1 1 calc R . . . . H12B H 0.539499 0.071597 0.430094 0.037 Uiso 1 1 calc R . . . . C13 C 0.61622(11) 0.15418(16) 0.39975(8) 0.0240(4) Uani 1 1 d . . . . . H13A H 0.645973 0.212124 0.409121 0.029 Uiso 1 1 calc R . . . . H13B H 0.585875 0.172511 0.371116 0.029 Uiso 1 1 calc R . . . . C14 C 0.94579(10) 0.29837(14) 0.33698(7) 0.0168(4) Uani 1 1 d . . . . . C15 C 0.92073(11) 0.31068(15) 0.28943(7) 0.0201(4) Uani 1 1 d . . . . . C16 C 0.95734(12) 0.26146(16) 0.25565(8) 0.0253(4) Uani 1 1 d . . . . . H16 H 0.941866 0.267000 0.223012 0.030 Uiso 1 1 calc R . . . . C17 C 1.01576(12) 0.20483(17) 0.26905(8) 0.0270(4) Uani 1 1 d . . . . . H17 H 1.039436 0.171011 0.245570 0.032 Uiso 1 1 calc R . . . . C18 C 1.04012(11) 0.19685(16) 0.31621(8) 0.0238(4) Uani 1 1 d . . . . . H18 H 1.080879 0.158578 0.324608 0.029 Uiso 1 1 calc R . . . . C19 C 1.00584(10) 0.24410(15) 0.35176(7) 0.0190(4) Uani 1 1 d . . . . . C20 C 0.86136(11) 0.38095(16) 0.27351(7) 0.0226(4) Uani 1 1 d . . . . . H20 H 0.833165 0.392914 0.301217 0.027 Uiso 1 1 calc R . . . . C21 C 0.81231(13) 0.3389(2) 0.23316(8) 0.0319(5) Uani 1 1 d . . . . . H21A H 0.836989 0.335539 0.204170 0.048 Uiso 1 1 calc GR . . . . H21B H 0.771288 0.382140 0.227814 0.048 Uiso 1 1 calc GR . . . . H21C H 0.797199 0.272177 0.241617 0.048 Uiso 1 1 calc GR . . . . C22 C 0.89245(13) 0.48052(18) 0.25957(9) 0.0308(5) Uani 1 1 d . . . . . H22A H 0.922261 0.506979 0.286402 0.046 Uiso 1 1 calc GR . . . . H22B H 0.854507 0.527503 0.250928 0.046 Uiso 1 1 calc GR . . . . H22C H 0.920481 0.470778 0.232443 0.046 Uiso 1 1 calc GR . . . . C23 C 1.03597(11) 0.24107(16) 0.40291(8) 0.0229(4) Uani 1 1 d . . . . . H23 H 0.998090 0.259679 0.423594 0.027 Uiso 1 1 calc R . . . . C24 C 1.06344(13) 0.13831(18) 0.41800(9) 0.0314(5) Uani 1 1 d . . . . . H24A H 1.026990 0.088547 0.410289 0.047 Uiso 1 1 calc GR . . . . H24B H 1.076167 0.137957 0.452245 0.047 Uiso 1 1 calc GR . . . . H24C H 1.104782 0.122585 0.401137 0.047 Uiso 1 1 calc GR . . . . C25 C 1.09489(14) 0.3179(2) 0.41021(10) 0.0368(6) Uani 1 1 d . . . . . H25A H 1.132991 0.300204 0.390662 0.055 Uiso 1 1 calc GR . . . . H25B H 1.112555 0.318959 0.443680 0.055 Uiso 1 1 calc GR . . . . H25C H 1.076779 0.383756 0.400942 0.055 Uiso 1 1 calc GR . . . . C26 C 0.75041(10) 0.41505(14) 0.42668(7) 0.0174(4) Uani 1 1 d . . . . . C27 C 0.69304(11) 0.45008(15) 0.39710(8) 0.0215(4) Uani 1 1 d . . . . . C28 C 0.63000(11) 0.46096(17) 0.41843(9) 0.0284(5) Uani 1 1 d . . . . . H28 H 0.589404 0.481999 0.399621 0.034 Uiso 1 1 calc R . . . . C29 C 0.62518(12) 0.44194(18) 0.46609(9) 0.0310(5) Uani 1 1 d . . . . . H29 H 0.581606 0.449841 0.479473 0.037 Uiso 1 1 calc R . . . . C30 C 0.68323(12) 0.41161(17) 0.49428(8) 0.0278(4) Uani 1 1 d . . . . . H30 H 0.679578 0.400356 0.527134 0.033 Uiso 1 1 calc R . . . . C31 C 0.74735(11) 0.39722(15) 0.47509(7) 0.0203(4) Uani 1 1 d . . . . . C32 C 0.69788(12) 0.47988(16) 0.34573(8) 0.0260(4) Uani 1 1 d . . . . . H32 H 0.725497 0.427980 0.330144 0.031 Uiso 1 1 calc R . . . . C33 C 0.73518(17) 0.5796(2) 0.34155(9) 0.0407(6) Uani 1 1 d . . . . . H33A H 0.712507 0.629737 0.360208 0.061 Uiso 1 1 calc GR . . . . H33B H 0.732574 0.600083 0.308221 0.061 Uiso 1 1 calc GR . . . . H33C H 0.784355 0.572772 0.353548 0.061 Uiso 1 1 calc GR . . . . C34 C 0.62596(15) 0.4875(3) 0.31848(10) 0.0440(7) Uani 1 1 d . . . . . H34A H 0.598680 0.427750 0.324178 0.066 Uiso 1 1 calc GR . . . . H34B H 0.631693 0.493610 0.284493 0.066 Uiso 1 1 calc GR . . . . H34C H 0.601378 0.546061 0.329298 0.066 Uiso 1 1 calc GR . . . . C35 C 0.81085(12) 0.37263(16) 0.50855(7) 0.0228(4) Uani 1 1 d . . . . . H35 H 0.850464 0.356682 0.488863 0.027 Uiso 1 1 calc R . . . . C36 C 0.79847(14) 0.28208(18) 0.53942(8) 0.0305(5) Uani 1 1 d . . . . . H36A H 0.841552 0.266326 0.559006 0.046 Uiso 1 1 calc GR . . . . H36B H 0.784990 0.225215 0.519089 0.046 Uiso 1 1 calc GR . . . . H36C H 0.760935 0.296682 0.559960 0.046 Uiso 1 1 calc GR . . . . C37 C 0.83171(15) 0.46398(18) 0.53863(9) 0.0354(5) Uani 1 1 d . . . . . H37A H 0.839562 0.520314 0.517780 0.053 Uiso 1 1 calc GR . . . . H37B H 0.874803 0.449812 0.558511 0.053 Uiso 1 1 calc GR . . . . H37C H 0.794125 0.480284 0.558856 0.053 Uiso 1 1 calc GR . . . . C38 C 0.85149(9) 0.14478(14) 0.40272(7) 0.0156(3) Uani 1 1 d . . . . . C39 C 0.88042(10) 0.15662(15) 0.44927(7) 0.0192(4) Uani 1 1 d . . . . . H39 H 0.880660 0.220337 0.463695 0.023 Uiso 1 1 calc R . . . . C40 C 0.90879(11) 0.07612(17) 0.47460(8) 0.0248(4) Uani 1 1 d . . . . . H40 H 0.926518 0.084114 0.506697 0.030 Uiso 1 1 calc R . . . . C41 C 0.91125(12) -0.01641(17) 0.45290(9) 0.0284(5) Uani 1 1 d . . . . . H41 H 0.930106 -0.071830 0.470337 0.034 Uiso 1 1 calc R . . . . C42 C 0.88631(12) -0.02781(16) 0.40601(9) 0.0286(5) Uani 1 1 d . . . . . H42 H 0.889530 -0.090500 0.390939 0.034 Uiso 1 1 calc R . . . . C43 C 0.85659(11) 0.05217(15) 0.38096(8) 0.0220(4) Uani 1 1 d . . . . . H43 H 0.839550 0.043961 0.348735 0.026 Uiso 1 1 calc R . . . . C44 C 0.71035(10) 0.05921(15) 0.26213(7) 0.0186(4) Uani 1 1 d . . . . . C45 C 0.77068(11) 0.02266(16) 0.24300(7) 0.0220(4) Uani 1 1 d . . . . . C46 C 0.78263(13) 0.05438(19) 0.19738(8) 0.0291(5) Uani 1 1 d . . . . . H46 H 0.823297 0.031806 0.183514 0.035 Uiso 1 1 calc R . . . . C47 C 0.73739(13) 0.1173(2) 0.17192(8) 0.0321(5) Uani 1 1 d . . . . . H47 H 0.747641 0.138712 0.141244 0.039 Uiso 1 1 calc R . . . . C48 C 0.67707(12) 0.14939(18) 0.19079(8) 0.0286(5) Uani 1 1 d . . . . . H48 H 0.645737 0.191872 0.172637 0.034 Uiso 1 1 calc R . . . . C49 C 0.66136(11) 0.12032(16) 0.23628(7) 0.0224(4) Uani 1 1 d . . . . . C50 C 0.82179(11) -0.05229(17) 0.26632(7) 0.0247(4) Uani 1 1 d . . . . . H50 H 0.809318 -0.063062 0.299586 0.030 Uiso 1 1 calc R . . . . C51 C 0.81378(15) -0.1520(2) 0.23977(8) 0.0358(5) Uani 1 1 d . . . . . H51A H 0.764252 -0.170878 0.236283 0.054 Uiso 1 1 calc GR . . . . H51B H 0.840632 -0.203310 0.257795 0.054 Uiso 1 1 calc GR . . . . H51C H 0.831373 -0.145225 0.208345 0.054 Uiso 1 1 calc GR . . . . C52 C 0.89786(13) -0.0172(2) 0.26822(9) 0.0398(6) Uani 1 1 d . . . . . H52A H 0.913676 -0.016852 0.236127 0.060 Uiso 1 1 calc GR . . . . H52B H 0.927383 -0.062261 0.288314 0.060 Uiso 1 1 calc GR . . . . H52C H 0.901262 0.050065 0.281440 0.060 Uiso 1 1 calc GR . . . . C53 C 0.59245(11) 0.15689(19) 0.25328(8) 0.0274(4) Uani 1 1 d . . . . . H53 H 0.588182 0.131486 0.286138 0.033 Uiso 1 1 calc R . . . . C54 C 0.59030(13) 0.2702(2) 0.25428(10) 0.0361(5) Uani 1 1 d . . . . . H54A H 0.631406 0.295280 0.273435 0.054 Uiso 1 1 calc GR . . . . H54B H 0.547662 0.292104 0.268165 0.054 Uiso 1 1 calc GR . . . . H54C H 0.590438 0.295852 0.221878 0.054 Uiso 1 1 calc GR . . . . C55 C 0.52971(13) 0.1190(2) 0.22100(9) 0.0383(6) Uani 1 1 d . . . . . H55A H 0.529206 0.151688 0.190026 0.057 Uiso 1 1 calc GR . . . . H55B H 0.486185 0.134130 0.235510 0.057 Uiso 1 1 calc GR . . . . H55C H 0.533744 0.047025 0.216884 0.057 Uiso 1 1 calc GR . . . . C56 C 0.60433(14) -0.09574(19) 0.28364(8) 0.0335(5) Uani 1 1 d . . . . . H56A H 0.568912 -0.044274 0.276443 0.050 Uiso 1 1 calc GR . . . . H56B H 0.581387 -0.157125 0.292710 0.050 Uiso 1 1 calc GR . . . . H56C H 0.629865 -0.108033 0.255558 0.050 Uiso 1 1 calc GR . . . . C57 C 0.70766(14) -0.14344(16) 0.33841(9) 0.0313(5) Uani 1 1 d . . . . . H57A H 0.729432 -0.166901 0.310283 0.047 Uiso 1 1 calc GR . . . . H57B H 0.683455 -0.198744 0.352585 0.047 Uiso 1 1 calc GR . . . . H57C H 0.743854 -0.117256 0.361525 0.047 Uiso 1 1 calc GR . . . . C58 C 0.28456(15) 0.3058(3) 0.51730(10) 0.0454(7) Uani 1 1 d . . . . . H58A H 0.286597 0.272923 0.486151 0.054 Uiso 1 1 calc R . . . . H58B H 0.287094 0.378418 0.512234 0.054 Uiso 1 1 calc R . . . . C59 C 0.54675(16) 0.26889(19) 0.56456(10) 0.0373(6) Uani 1 1 d . . . . . H59A H 0.516620 0.259923 0.534780 0.045 Uiso 1 1 calc R . . . . H59B H 0.595037 0.249836 0.558268 0.045 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 Ga1 0.03392(15) 0.02331(14) 0.02581(14) -0.00114(10) -0.00407(11) -0.00135(11) Ga2 0.02462(13) 0.02428(14) 0.02333(13) 0.00330(10) 0.00335(10) 0.00134(10) Ga3 0.02157(13) 0.01879(13) 0.02133(13) -0.00328(9) 0.00545(9) -0.00154(9) Cl1 0.0551(4) 0.0364(3) 0.0596(4) 0.0006(3) -0.0311(3) 0.0023(3) Cl2 0.0551(4) 0.0394(3) 0.0301(3) -0.0027(2) 0.0101(3) 0.0054(3) Cl3 0.0548(4) 0.0322(3) 0.0416(3) 0.0036(2) -0.0019(3) -0.0151(3) Cl4 0.0344(3) 0.0241(2) 0.0202(2) -0.00032(17) 0.00166(18) -0.00577(19) Cl5 0.0330(3) 0.0439(4) 0.0500(4) 0.0001(3) -0.0048(3) 0.0144(3) Cl6 0.0616(4) 0.0526(4) 0.0362(3) 0.0142(3) 0.0257(3) 0.0081(3) Cl7 0.0407(3) 0.0268(3) 0.0419(3) -0.0026(2) -0.0089(2) -0.0055(2) Cl8 0.0360(3) 0.0481(3) 0.0208(2) -0.0027(2) 0.0082(2) -0.0022(2) Cl9 0.0233(2) 0.0221(2) 0.0332(3) -0.00405(19) 0.00096(19) -0.00053(18) Cl10 0.0263(2) 0.0214(2) 0.0244(2) -0.00073(17) 0.00896(18) 0.00272(18) Cl11 0.0316(3) 0.0212(2) 0.0446(3) -0.0048(2) 0.0075(2) -0.0072(2) Cl12 0.0374(3) 0.0417(3) 0.0422(3) -0.0008(3) 0.0100(2) -0.0004(2) Cl13 0.0383(3) 0.0359(3) 0.0512(4) 0.0132(3) 0.0130(3) 0.0067(2) Cl14 0.0490(4) 0.0362(3) 0.0546(4) 0.0169(3) -0.0021(3) -0.0098(3) Cl15 0.0434(3) 0.0257(3) 0.0382(3) 0.0015(2) 0.0111(2) -0.0004(2) P1 0.0181(2) 0.0128(2) 0.0163(2) 0.00158(16) -0.00089(17) -0.00173(16) N1 0.0183(7) 0.0121(7) 0.0174(7) -0.0020(6) 0.0024(6) -0.0007(6) N2 0.0180(7) 0.0106(7) 0.0174(7) -0.0020(6) 0.0025(6) -0.0003(6) N3 0.0188(7) 0.0149(8) 0.0152(7) 0.0005(6) 0.0020(6) -0.0036(6) C1 0.0168(8) 0.0125(9) 0.0141(8) -0.0005(6) 0.0008(6) 0.0009(7) C2 0.0208(9) 0.0136(9) 0.0255(10) -0.0028(7) 0.0036(7) -0.0038(7) C3 0.0230(9) 0.0125(9) 0.0245(9) -0.0036(7) 0.0037(7) -0.0026(7) C4 0.0169(8) 0.0128(9) 0.0147(8) -0.0014(6) 0.0032(6) -0.0005(7) C5 0.0153(8) 0.0149(9) 0.0152(8) 0.0016(7) -0.0003(6) 0.0003(7) C6 0.0311(10) 0.0158(9) 0.0209(9) -0.0008(7) 0.0064(8) -0.0108(8) C7 0.0250(10) 0.0218(10) 0.0194(9) 0.0006(7) 0.0047(7) -0.0068(8) C8 0.0178(8) 0.0168(9) 0.0163(8) 0.0010(7) 0.0038(7) -0.0006(7) C9 0.0216(9) 0.0259(10) 0.0159(9) 0.0014(7) 0.0035(7) 0.0014(8) C10 0.0301(10) 0.0316(11) 0.0166(9) 0.0033(8) 0.0072(8) -0.0014(9) C11 0.0336(12) 0.0363(13) 0.0243(10) -0.0037(9) 0.0143(9) -0.0031(10) C12 0.0263(11) 0.0336(12) 0.0337(12) -0.0009(9) 0.0139(9) 0.0043(9) C13 0.0234(10) 0.0229(10) 0.0264(10) 0.0014(8) 0.0058(8) 0.0042(8) C14 0.0194(9) 0.0118(8) 0.0201(9) -0.0018(7) 0.0068(7) -0.0027(7) C15 0.0241(9) 0.0159(9) 0.0207(9) -0.0002(7) 0.0053(7) -0.0036(7) C16 0.0345(11) 0.0220(10) 0.0205(10) -0.0018(8) 0.0082(8) -0.0013(9) C17 0.0337(11) 0.0220(10) 0.0272(11) -0.0040(8) 0.0139(9) 0.0004(9) C18 0.0245(10) 0.0183(10) 0.0296(11) -0.0010(8) 0.0087(8) 0.0017(8) C19 0.0185(9) 0.0148(9) 0.0242(10) -0.0007(7) 0.0052(7) -0.0024(7) C20 0.0261(10) 0.0216(10) 0.0201(9) 0.0033(8) 0.0021(8) -0.0003(8) C21 0.0338(12) 0.0360(13) 0.0249(11) 0.0044(9) -0.0033(9) -0.0057(10) C22 0.0348(12) 0.0230(11) 0.0342(12) 0.0085(9) 0.0006(9) -0.0004(9) C23 0.0224(9) 0.0221(10) 0.0241(10) -0.0001(8) 0.0015(8) 0.0003(8) C24 0.0323(12) 0.0280(12) 0.0341(12) 0.0058(9) 0.0030(9) 0.0058(9) C25 0.0333(12) 0.0340(13) 0.0413(14) -0.0004(10) -0.0076(10) -0.0097(10) C26 0.0162(8) 0.0128(8) 0.0234(9) -0.0025(7) 0.0033(7) 0.0010(7) C27 0.0207(9) 0.0149(9) 0.0279(10) -0.0033(7) -0.0038(8) 0.0003(7) C28 0.0194(10) 0.0262(11) 0.0391(12) -0.0044(9) -0.0017(9) 0.0039(8) C29 0.0238(10) 0.0302(12) 0.0401(13) -0.0023(10) 0.0101(9) 0.0002(9) C30 0.0282(11) 0.0266(11) 0.0299(11) -0.0002(9) 0.0109(9) 0.0001(9) C31 0.0231(9) 0.0145(9) 0.0238(10) -0.0018(7) 0.0049(8) -0.0006(7) C32 0.0319(11) 0.0208(10) 0.0247(10) -0.0011(8) -0.0027(8) 0.0070(8) C33 0.0609(17) 0.0298(13) 0.0305(12) 0.0065(10) -0.0025(11) -0.0087(12) C34 0.0382(14) 0.0569(18) 0.0349(13) -0.0024(12) -0.0093(11) 0.0131(13) C35 0.0300(10) 0.0194(10) 0.0190(9) -0.0020(7) 0.0021(8) 0.0027(8) C36 0.0422(13) 0.0266(11) 0.0232(10) 0.0033(8) 0.0061(9) 0.0055(9) C37 0.0479(14) 0.0250(12) 0.0313(12) -0.0097(9) -0.0088(10) 0.0061(10) C38 0.0153(8) 0.0135(9) 0.0180(9) 0.0000(7) 0.0015(7) 0.0002(7) C39 0.0222(9) 0.0173(9) 0.0183(9) -0.0017(7) 0.0022(7) 0.0016(7) C40 0.0260(10) 0.0266(11) 0.0214(9) 0.0051(8) -0.0001(8) 0.0028(8) C41 0.0257(10) 0.0200(10) 0.0390(12) 0.0086(9) -0.0010(9) 0.0030(8) C42 0.0252(10) 0.0144(10) 0.0454(13) -0.0045(9) -0.0030(9) 0.0032(8) C43 0.0214(9) 0.0165(9) 0.0276(10) -0.0059(8) -0.0018(8) 0.0013(7) C44 0.0232(9) 0.0191(9) 0.0138(8) -0.0005(7) 0.0024(7) -0.0080(7) C45 0.0253(10) 0.0230(10) 0.0178(9) -0.0031(7) 0.0034(7) -0.0059(8) C46 0.0327(11) 0.0360(13) 0.0194(10) -0.0021(9) 0.0083(8) -0.0053(9) C47 0.0381(12) 0.0407(13) 0.0183(10) 0.0050(9) 0.0071(9) -0.0072(10) C48 0.0321(11) 0.0326(12) 0.0206(10) 0.0068(9) -0.0004(8) -0.0044(9) C49 0.0249(10) 0.0246(10) 0.0175(9) 0.0020(8) 0.0006(7) -0.0066(8) C50 0.0261(10) 0.0303(11) 0.0181(9) -0.0049(8) 0.0043(8) -0.0005(9) C51 0.0480(14) 0.0356(13) 0.0235(11) -0.0101(9) 0.0011(10) 0.0118(11) C52 0.0256(11) 0.0657(19) 0.0282(12) 0.0069(12) 0.0037(9) -0.0058(11) C53 0.0234(10) 0.0366(12) 0.0219(10) 0.0071(9) -0.0004(8) -0.0008(9) C54 0.0302(12) 0.0382(14) 0.0388(13) 0.0024(10) -0.0040(10) 0.0086(10) C55 0.0276(11) 0.0566(17) 0.0297(12) 0.0090(11) -0.0035(9) -0.0110(11) C56 0.0426(13) 0.0332(13) 0.0251(11) -0.0054(9) 0.0053(9) -0.0222(10) C57 0.0453(13) 0.0158(10) 0.0348(12) 0.0011(8) 0.0157(10) -0.0037(9) C58 0.0430(15) 0.0576(18) 0.0367(14) 0.0157(13) 0.0100(11) 0.0034(13) C59 0.0505(15) 0.0280(13) 0.0344(13) 0.0002(10) 0.0093(11) 0.0004(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl1 2.1367(7) . ? Ga1 Cl2 2.1499(7) . ? Ga1 Cl3 2.1393(7) . ? Ga1 Cl4 2.3244(6) . ? Ga2 Cl4 2.3251(6) . ? Ga2 Cl5 2.1303(6) . ? Ga2 Cl6 2.1318(7) . ? Ga2 Cl7 2.1462(6) . ? Ga3 Cl8 2.1795(6) . ? Ga3 Cl9 2.1773(6) . ? Ga3 Cl10 2.1815(5) . ? Ga3 Cl11 2.1598(6) . ? Cl12 C58 1.767(3) . ? Cl13 C58 1.755(3) . ? Cl14 C59 1.746(3) . ? Cl15 C59 1.753(3) . ? P1 C4 1.6916(19) . ? P1 C5 1.8530(19) . ? N1 C1 1.344(2) . ? N1 C2 1.381(2) . ? N1 C14 1.460(2) . ? N2 C1 1.356(2) . ? N2 C3 1.383(2) . ? N2 C26 1.460(2) . ? N3 C5 1.302(2) . ? N3 C6 1.544(2) . ? N3 C44 1.475(2) . ? C1 C4 1.478(2) . ? C2 H2 0.9500 . ? C2 C3 1.353(3) . ? C3 H3 0.9500 . ? C4 C38 1.476(3) . ? C5 C8 1.525(2) . ? C6 C7 1.531(3) . ? C6 C56 1.514(3) . ? C6 C57 1.528(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.544(3) . ? C8 C9 1.545(3) . ? C8 C13 1.555(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.537(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.520(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.523(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.531(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.402(3) . ? C14 C19 1.399(3) . ? C15 C16 1.397(3) . ? C15 C20 1.520(3) . ? C16 H16 0.9500 . ? C16 C17 1.382(3) . ? C17 H17 0.9500 . ? C17 C18 1.382(3) . ? C18 H18 0.9500 . ? C18 C19 1.398(3) . ? C19 C23 1.515(3) . ? C20 H20 1.0000 . ? C20 C21 1.528(3) . ? C20 C22 1.532(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23 1.0000 . ? C23 C24 1.529(3) . ? C23 C25 1.533(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.409(3) . ? C26 C31 1.397(3) . ? C27 C28 1.400(3) . ? C27 C32 1.518(3) . ? C28 H28 0.9500 . ? C28 C29 1.383(4) . ? C29 H29 0.9500 . ? C29 C30 1.378(3) . ? C30 H30 0.9500 . ? C30 C31 1.396(3) . ? C31 C35 1.517(3) . ? C32 H32 1.0000 . ? C32 C33 1.530(3) . ? C32 C34 1.528(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35 1.0000 . ? C35 C36 1.530(3) . ? C35 C37 1.531(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.397(3) . ? C38 C43 1.398(3) . ? C39 H39 0.9500 . ? C39 C40 1.386(3) . ? C40 H40 0.9500 . ? C40 C41 1.392(3) . ? C41 H41 0.9500 . ? C41 C42 1.382(3) . ? C42 H42 0.9500 . ? C42 C43 1.387(3) . ? C43 H43 0.9500 . ? C44 C45 1.404(3) . ? C44 C49 1.409(3) . ? C45 C46 1.396(3) . ? C45 C50 1.520(3) . ? C46 H46 0.9500 . ? C46 C47 1.374(4) . ? C47 H47 0.9500 . ? C47 C48 1.381(4) . ? C48 H48 0.9500 . ? C48 C49 1.401(3) . ? C49 C53 1.523(3) . ? C50 H50 1.0000 . ? C50 C51 1.540(3) . ? C50 C52 1.529(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53 1.0000 . ? C53 C54 1.526(4) . ? C53 C55 1.538(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? 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 Cl1 Ga1 Cl2 112.60(3) . . ? Cl1 Ga1 Cl3 115.73(3) . . ? Cl1 Ga1 Cl4 105.20(3) . . ? Cl2 Ga1 Cl4 104.80(3) . . ? Cl3 Ga1 Cl2 114.28(3) . . ? Cl3 Ga1 Cl4 102.57(2) . . ? Cl5 Ga2 Cl4 106.19(3) . . ? Cl5 Ga2 Cl6 116.76(3) . . ? Cl5 Ga2 Cl7 111.65(3) . . ? Cl6 Ga2 Cl4 106.72(3) . . ? Cl6 Ga2 Cl7 113.32(3) . . ? Cl7 Ga2 Cl4 100.46(2) . . ? Cl8 Ga3 Cl10 109.90(2) . . ? Cl9 Ga3 Cl8 108.36(2) . . ? Cl9 Ga3 Cl10 106.40(2) . . ? Cl11 Ga3 Cl8 110.66(3) . . ? Cl11 Ga3 Cl9 111.91(2) . . ? Cl11 Ga3 Cl10 109.52(2) . . ? Ga1 Cl4 Ga2 110.87(2) . . ? C4 P1 C5 105.24(9) . . ? C1 N1 C2 109.42(16) . . ? C1 N1 C14 124.48(16) . . ? C2 N1 C14 124.15(16) . . ? C1 N2 C3 108.61(16) . . ? C1 N2 C26 128.38(16) . . ? C3 N2 C26 123.01(16) . . ? C5 N3 C6 112.07(15) . . ? C5 N3 C44 123.00(16) . . ? C44 N3 C6 124.45(15) . . ? N1 C1 N2 107.33(16) . . ? N1 C1 C4 124.06(16) . . ? N2 C1 C4 128.36(17) . . ? N1 C2 H2 126.5 . . ? C3 C2 N1 107.02(17) . . ? C3 C2 H2 126.5 . . ? N2 C3 H3 126.2 . . ? C2 C3 N2 107.59(17) . . ? C2 C3 H3 126.2 . . ? C1 C4 P1 115.30(13) . . ? C38 C4 P1 129.18(14) . . ? C38 C4 C1 115.44(16) . . ? N3 C5 P1 121.51(14) . . ? N3 C5 C8 112.54(16) . . ? C8 C5 P1 123.17(14) . . ? C7 C6 N3 99.78(15) . . ? C56 C6 N3 111.27(17) . . ? C56 C6 C7 113.62(19) . . ? C56 C6 C57 110.5(2) . . ? C57 C6 N3 109.71(17) . . ? C57 C6 C7 111.54(18) . . ? C6 C7 H7A 110.2 . . ? C6 C7 H7B 110.2 . . ? C6 C7 C8 107.56(16) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? C5 C8 C7 101.32(15) . . ? C5 C8 C9 114.40(15) . . ? C5 C8 C13 107.85(16) . . ? C7 C8 C9 113.61(17) . . ? C7 C8 C13 111.19(16) . . ? C9 C8 C13 108.26(16) . . ? C8 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C10 C9 C8 111.58(17) . . ? C10 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C11 C10 C9 111.52(18) . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C10 C11 C12 111.06(19) . . ? H11A C11 H11B 108.0 . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 C13 110.79(19) . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C12 C13 C8 110.53(18) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 N1 116.34(17) . . ? C19 C14 N1 119.55(17) . . ? C19 C14 C15 124.02(18) . . ? C14 C15 C20 123.29(18) . . ? C16 C15 C14 116.63(19) . . ? C16 C15 C20 119.83(19) . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 120.9(2) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.4 . . ? C17 C18 C19 121.2(2) . . ? C19 C18 H18 119.4 . . ? C14 C19 C23 122.77(18) . . ? C18 C19 C14 116.45(19) . . ? C18 C19 C23 120.67(19) . . ? C15 C20 H20 107.9 . . ? C15 C20 C21 113.07(19) . . ? C15 C20 C22 108.91(18) . . ? C21 C20 H20 107.9 . . ? C21 C20 C22 111.12(18) . . ? C22 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23 108.3 . . ? C19 C23 C24 112.79(18) . . ? C19 C23 C25 109.31(18) . . ? C24 C23 H23 108.3 . . ? C24 C23 C25 109.87(19) . . ? C25 C23 H23 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N2 118.87(18) . . ? C31 C26 N2 117.66(17) . . ? C31 C26 C27 123.25(18) . . ? C26 C27 C32 123.56(19) . . ? C28 C27 C26 116.0(2) . . ? C28 C27 C32 120.39(19) . . ? C27 C28 H28 119.1 . . ? C29 C28 C27 121.9(2) . . ? C29 C28 H28 119.1 . . ? C28 C29 H29 119.8 . . ? C30 C29 C28 120.4(2) . . ? C30 C29 H29 119.8 . . ? C29 C30 H30 119.6 . . ? C29 C30 C31 120.7(2) . . ? C31 C30 H30 119.6 . . ? C26 C31 C35 123.70(18) . . ? C30 C31 C26 117.7(2) . . ? C30 C31 C35 118.35(19) . . ? C27 C32 H32 108.2 . . ? C27 C32 C33 111.76(19) . . ? C27 C32 C34 112.3(2) . . ? C33 C32 H32 108.2 . . ? C34 C32 H32 108.2 . . ? C34 C32 C33 108.1(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35 107.8 . . ? C31 C35 C36 112.15(19) . . ? C31 C35 C37 109.40(18) . . ? C36 C35 H35 107.8 . . ? C36 C35 C37 111.63(19) . . ? C37 C35 H35 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C4 121.40(17) . . ? C39 C38 C43 118.74(18) . . ? C43 C38 C4 119.79(17) . . ? C38 C39 H39 119.7 . . ? C40 C39 C38 120.52(19) . . ? C40 C39 H39 119.7 . . ? C39 C40 H40 120.1 . . ? C39 C40 C41 119.9(2) . . ? C41 C40 H40 120.1 . . ? C40 C41 H41 119.9 . . ? C42 C41 C40 120.1(2) . . ? C42 C41 H41 119.9 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 120.0(2) . . ? C43 C42 H42 120.0 . . ? C38 C43 H43 119.7 . . ? C42 C43 C38 120.6(2) . . ? C42 C43 H43 119.7 . . ? C45 C44 N3 121.05(18) . . ? C45 C44 C49 122.67(18) . . ? C49 C44 N3 116.28(17) . . ? C44 C45 C50 125.97(18) . . ? C46 C45 C44 116.8(2) . . ? C46 C45 C50 117.19(19) . . ? C45 C46 H46 119.0 . . ? C47 C46 C45 122.0(2) . . ? C47 C46 H46 119.0 . . ? C46 C47 H47 119.9 . . ? C46 C47 C48 120.2(2) . . ? C48 C47 H47 119.9 . . ? C47 C48 H48 119.5 . . ? C47 C48 C49 121.0(2) . . ? C49 C48 H48 119.5 . . ? C44 C49 C53 125.72(18) . . ? C48 C49 C44 117.2(2) . . ? C48 C49 C53 117.1(2) . . ? C45 C50 H50 108.1 . . ? C45 C50 C51 109.37(18) . . ? C45 C50 C52 112.9(2) . . ? C51 C50 H50 108.1 . . ? C52 C50 H50 108.1 . . ? C52 C50 C51 110.1(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53 108.7 . . ? C49 C53 C54 110.76(19) . . ? C49 C53 C55 111.2(2) . . ? C54 C53 H53 108.7 . . ? C54 C53 C55 108.8(2) . . ? C55 C53 H53 108.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C6 C56 H56A 109.5 . . ? C6 C56 H56B 109.5 . . ? C6 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C6 C57 H57A 109.5 . . ? C6 C57 H57B 109.5 . . ? C6 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Cl12 C58 H58A 109.2 . . ? Cl12 C58 H58B 109.2 . . ? Cl13 C58 Cl12 112.21(15) . . ? Cl13 C58 H58A 109.2 . . ? Cl13 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? Cl14 C59 Cl15 113.04(15) . . ? Cl14 C59 H59A 109.0 . . ? Cl14 C59 H59B 109.0 . . ? Cl15 C59 H59A 109.0 . . ? Cl15 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? _shelx_res_file ; TITL sharma53_a.res in P2(1)/c sharma53.res created by SHELXL-2018/3 at 11:11:11 on 27-Aug-2019 REM Old TITL Sharma53 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.095, Rweak 0.005, Alpha 0.024 REM 0.791 for 277 systematic absences, Orientation as input REM Formula found by SHELXT: C59 N3 Cl16 Ga3 CELL 1.54184 19.162745 13.467009 28.292392 90 94.584 90 ZERR 4 0.000149 0.000104 0.000224 0 0.0007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ga N P UNIT 236 320 60 12 12 4 L.S. 4 0 0 PLAN 5 TEMP -173.15(10) BOND $h more -1 list 4 fmap 2 53 acta REM REM REM WGHT 0.052900 7.139000 EXTI 0.000055 FVAR 1.71836 GA1 4 0.333337 0.037301 0.355465 11.00000 0.03392 0.02331 = 0.02581 -0.00114 -0.00407 -0.00135 GA2 4 0.386264 0.300596 0.394812 11.00000 0.02462 0.02428 = 0.02333 0.00330 0.00335 0.00134 GA3 4 0.000112 0.274500 0.613247 11.00000 0.02157 0.01879 = 0.02133 -0.00328 0.00545 -0.00154 CL1 3 0.255716 0.121903 0.314715 11.00000 0.05511 0.03636 = 0.05959 0.00064 -0.03114 0.00230 CL2 3 0.425808 0.013266 0.318690 11.00000 0.05505 0.03939 = 0.03007 -0.00267 0.01015 0.00540 CL3 3 0.296165 -0.092166 0.389367 11.00000 0.05481 0.03220 = 0.04162 0.00363 -0.00189 -0.01513 CL4 3 0.369932 0.138086 0.419395 11.00000 0.03443 0.02415 = 0.02024 -0.00032 0.00166 -0.00577 CL5 3 0.284771 0.365854 0.386259 11.00000 0.03296 0.04394 = 0.05003 0.00013 -0.00478 0.01435 CL6 3 0.443235 0.292712 0.333213 11.00000 0.06164 0.05263 = 0.03624 0.01424 0.02574 0.00811 CL7 3 0.446662 0.358962 0.455698 11.00000 0.04068 0.02676 = 0.04186 -0.00262 -0.00888 -0.00554 CL8 3 0.007334 0.308731 0.538504 11.00000 0.03605 0.04806 = 0.02077 -0.00270 0.00825 -0.00221 CL9 3 0.105396 0.274718 0.648437 11.00000 0.02325 0.02213 = 0.03318 -0.00405 0.00096 -0.00053 CL10 3 -0.057333 0.391665 0.646617 11.00000 0.02634 0.02145 = 0.02439 -0.00073 0.00896 0.00272 CL11 3 -0.052079 0.134061 0.621255 11.00000 0.03158 0.02123 = 0.04460 -0.00484 0.00749 -0.00722 CL12 3 0.204146 0.276565 0.540481 11.00000 0.03740 0.04170 = 0.04217 -0.00078 0.01000 -0.00038 CL13 3 0.356788 0.268159 0.555127 11.00000 0.03828 0.03594 = 0.05115 0.01318 0.01303 0.00670 CL14 3 0.517558 0.190097 0.607848 11.00000 0.04903 0.03617 = 0.05464 0.01690 -0.00210 -0.00980 CL15 3 0.545966 0.394446 0.580885 11.00000 0.04344 0.02573 = 0.03818 0.00149 0.01115 -0.00036 P1 6 0.740588 0.220328 0.338951 11.00000 0.01807 0.01279 = 0.01629 0.00158 -0.00089 -0.00173 N1 5 0.907911 0.351135 0.372029 11.00000 0.01830 0.01206 = 0.01737 -0.00200 0.00238 -0.00072 N2 5 0.818298 0.404949 0.407123 11.00000 0.01799 0.01061 = 0.01745 -0.00200 0.00250 -0.00027 N3 5 0.694347 0.033326 0.310766 11.00000 0.01879 0.01494 = 0.01524 0.00050 0.00198 -0.00362 C1 1 0.843913 0.326000 0.384277 11.00000 0.01684 0.01249 = 0.01409 -0.00047 0.00085 0.00089 C2 1 0.923814 0.446181 0.387772 11.00000 0.02082 0.01359 = 0.02552 -0.00277 0.00356 -0.00378 AFIX 43 H2 2 0.965753 0.481699 0.383724 11.00000 -1.20000 AFIX 0 C3 1 0.868353 0.479121 0.410049 11.00000 0.02295 0.01251 = 0.02449 -0.00363 0.00365 -0.00256 AFIX 43 H3 2 0.864501 0.541836 0.424993 11.00000 -1.20000 AFIX 0 C4 1 0.812901 0.226048 0.377274 11.00000 0.01686 0.01275 = 0.01470 -0.00142 0.00322 -0.00049 C5 1 0.704491 0.094158 0.346416 11.00000 0.01533 0.01491 = 0.01523 0.00159 -0.00031 0.00033 C6 1 0.655027 -0.061443 0.324144 11.00000 0.03109 0.01584 = 0.02090 -0.00084 0.00644 -0.01083 C7 1 0.619114 -0.022560 0.366910 11.00000 0.02505 0.02177 = 0.01944 0.00058 0.00469 -0.00685 AFIX 23 H7A 2 0.616131 -0.075829 0.390778 11.00000 -1.20000 H7B 2 0.571081 0.000199 0.356864 11.00000 -1.20000 AFIX 0 C8 1 0.663364 0.064772 0.388231 11.00000 0.01782 0.01683 = 0.01626 0.00096 0.00384 -0.00061 C9 1 0.709279 0.037179 0.433704 11.00000 0.02158 0.02589 = 0.01590 0.00141 0.00345 0.00137 AFIX 23 H9A 2 0.738331 -0.021356 0.427315 11.00000 -1.20000 H9B 2 0.741149 0.093081 0.442738 11.00000 -1.20000 AFIX 0 C10 1 0.664524 0.013631 0.475027 11.00000 0.03010 0.03156 = 0.01656 0.00332 0.00721 -0.00143 AFIX 23 H10A 2 0.636374 -0.046744 0.467393 11.00000 -1.20000 H10B 2 0.695635 -0.000095 0.503925 11.00000 -1.20000 AFIX 0 C11 1 0.615939 0.099191 0.484643 11.00000 0.03357 0.03629 = 0.02433 -0.00372 0.01429 -0.00312 AFIX 23 H11A 2 0.644069 0.157261 0.496152 11.00000 -1.20000 H11B 2 0.585494 0.079746 0.509758 11.00000 -1.20000 AFIX 0 C12 1 0.570683 0.127707 0.440019 11.00000 0.02630 0.03363 = 0.03366 -0.00089 0.01389 0.00426 AFIX 23 H12A 2 0.540994 0.185291 0.446861 11.00000 -1.20000 H12B 2 0.539499 0.071597 0.430094 11.00000 -1.20000 AFIX 0 C13 1 0.616218 0.154182 0.399752 11.00000 0.02339 0.02288 = 0.02638 0.00137 0.00583 0.00417 AFIX 23 H13A 2 0.645973 0.212124 0.409121 11.00000 -1.20000 H13B 2 0.585875 0.172511 0.371116 11.00000 -1.20000 AFIX 0 C14 1 0.945792 0.298374 0.336977 11.00000 0.01937 0.01181 = 0.02009 -0.00179 0.00683 -0.00268 C15 1 0.920732 0.310682 0.289433 11.00000 0.02415 0.01587 = 0.02071 -0.00021 0.00530 -0.00364 C16 1 0.957343 0.261463 0.255652 11.00000 0.03452 0.02201 = 0.02046 -0.00183 0.00824 -0.00134 AFIX 43 H16 2 0.941866 0.267000 0.223012 11.00000 -1.20000 AFIX 0 C17 1 1.015763 0.204829 0.269046 11.00000 0.03368 0.02199 = 0.02724 -0.00396 0.01385 0.00043 AFIX 43 H17 2 1.039436 0.171011 0.245570 11.00000 -1.20000 AFIX 0 C18 1 1.040121 0.196851 0.316207 11.00000 0.02452 0.01827 = 0.02957 -0.00100 0.00872 0.00168 AFIX 43 H18 2 1.080879 0.158578 0.324608 11.00000 -1.20000 AFIX 0 C19 1 1.005844 0.244100 0.351762 11.00000 0.01851 0.01480 = 0.02425 -0.00070 0.00520 -0.00239 C20 1 0.861364 0.380951 0.273513 11.00000 0.02610 0.02156 = 0.02010 0.00332 0.00208 -0.00029 AFIX 13 H20 2 0.833165 0.392914 0.301217 11.00000 -1.20000 AFIX 0 C21 1 0.812310 0.338933 0.233159 11.00000 0.03381 0.03597 = 0.02489 0.00440 -0.00327 -0.00569 AFIX 137 H21A 2 0.836989 0.335539 0.204170 11.00000 -1.50000 H21B 2 0.771288 0.382140 0.227814 11.00000 -1.50000 H21C 2 0.797199 0.272177 0.241617 11.00000 -1.50000 AFIX 0 C22 1 0.892453 0.480519 0.259566 11.00000 0.03482 0.02296 = 0.03418 0.00848 0.00063 -0.00038 AFIX 137 H22A 2 0.922261 0.506979 0.286402 11.00000 -1.50000 H22B 2 0.854507 0.527503 0.250928 11.00000 -1.50000 H22C 2 0.920481 0.470778 0.232443 11.00000 -1.50000 AFIX 0 C23 1 1.035969 0.241073 0.402911 11.00000 0.02244 0.02211 = 0.02414 -0.00008 0.00146 0.00029 AFIX 13 H23 2 0.998090 0.259679 0.423594 11.00000 -1.20000 AFIX 0 C24 1 1.063444 0.138314 0.418000 11.00000 0.03226 0.02803 = 0.03411 0.00577 0.00304 0.00582 AFIX 137 H24A 2 1.026990 0.088547 0.410289 11.00000 -1.50000 H24B 2 1.076167 0.137957 0.452245 11.00000 -1.50000 H24C 2 1.104782 0.122585 0.401137 11.00000 -1.50000 AFIX 0 C25 1 1.094890 0.317933 0.410207 11.00000 0.03328 0.03404 = 0.04126 -0.00037 -0.00760 -0.00966 AFIX 137 H25A 2 1.132991 0.300204 0.390662 11.00000 -1.50000 H25B 2 1.112555 0.318959 0.443680 11.00000 -1.50000 H25C 2 1.076779 0.383756 0.400942 11.00000 -1.50000 AFIX 0 C26 1 0.750413 0.415049 0.426678 11.00000 0.01624 0.01278 = 0.02339 -0.00248 0.00329 0.00105 C27 1 0.693038 0.450076 0.397098 11.00000 0.02070 0.01492 = 0.02789 -0.00325 -0.00381 0.00026 C28 1 0.630003 0.460958 0.418427 11.00000 0.01938 0.02619 = 0.03909 -0.00439 -0.00167 0.00386 AFIX 43 H28 2 0.589404 0.481999 0.399621 11.00000 -1.20000 AFIX 0 C29 1 0.625182 0.441944 0.466091 11.00000 0.02381 0.03024 = 0.04008 -0.00226 0.01011 0.00021 AFIX 43 H29 2 0.581606 0.449841 0.479473 11.00000 -1.20000 AFIX 0 C30 1 0.683233 0.411607 0.494276 11.00000 0.02823 0.02655 = 0.02991 -0.00016 0.01092 0.00014 AFIX 43 H30 2 0.679578 0.400356 0.527134 11.00000 -1.20000 AFIX 0 C31 1 0.747350 0.397221 0.475095 11.00000 0.02314 0.01452 = 0.02376 -0.00175 0.00491 -0.00058 C32 1 0.697885 0.479875 0.345725 11.00000 0.03187 0.02079 = 0.02467 -0.00105 -0.00275 0.00703 AFIX 13 H32 2 0.725497 0.427980 0.330144 11.00000 -1.20000 AFIX 0 C33 1 0.735183 0.579578 0.341550 11.00000 0.06087 0.02977 = 0.03049 0.00648 -0.00248 -0.00873 AFIX 137 H33A 2 0.712507 0.629737 0.360208 11.00000 -1.50000 H33B 2 0.732574 0.600083 0.308221 11.00000 -1.50000 H33C 2 0.784355 0.572772 0.353548 11.00000 -1.50000 AFIX 0 C34 1 0.625961 0.487508 0.318481 11.00000 0.03818 0.05685 = 0.03492 -0.00244 -0.00926 0.01310 AFIX 137 H34A 2 0.598680 0.427750 0.324178 11.00000 -1.50000 H34B 2 0.631693 0.493610 0.284493 11.00000 -1.50000 H34C 2 0.601378 0.546061 0.329298 11.00000 -1.50000 AFIX 0 C35 1 0.810852 0.372630 0.508547 11.00000 0.02995 0.01943 = 0.01904 -0.00199 0.00205 0.00273 AFIX 13 H35 2 0.850464 0.356682 0.488863 11.00000 -1.20000 AFIX 0 C36 1 0.798470 0.282079 0.539424 11.00000 0.04217 0.02661 = 0.02316 0.00326 0.00607 0.00554 AFIX 137 H36A 2 0.841552 0.266326 0.559006 11.00000 -1.50000 H36B 2 0.784990 0.225215 0.519089 11.00000 -1.50000 H36C 2 0.760935 0.296682 0.559960 11.00000 -1.50000 AFIX 0 C37 1 0.831712 0.463976 0.538629 11.00000 0.04789 0.02501 = 0.03132 -0.00968 -0.00880 0.00607 AFIX 137 H37A 2 0.839562 0.520314 0.517780 11.00000 -1.50000 H37B 2 0.874803 0.449812 0.558511 11.00000 -1.50000 H37C 2 0.794125 0.480284 0.558856 11.00000 -1.50000 AFIX 0 C38 1 0.851489 0.144779 0.402721 11.00000 0.01528 0.01352 = 0.01800 -0.00002 0.00146 0.00017 C39 1 0.880421 0.156621 0.449273 11.00000 0.02221 0.01728 = 0.01830 -0.00175 0.00221 0.00156 AFIX 43 H39 2 0.880660 0.220337 0.463695 11.00000 -1.20000 AFIX 0 C40 1 0.908792 0.076125 0.474596 11.00000 0.02598 0.02659 = 0.02138 0.00512 -0.00011 0.00282 AFIX 43 H40 2 0.926518 0.084114 0.506697 11.00000 -1.20000 AFIX 0 C41 1 0.911252 -0.016412 0.452896 11.00000 0.02568 0.01998 = 0.03904 0.00863 -0.00097 0.00303 AFIX 43 H41 2 0.930106 -0.071830 0.470337 11.00000 -1.20000 AFIX 0 C42 1 0.886309 -0.027815 0.406011 11.00000 0.02518 0.01439 = 0.04541 -0.00454 -0.00301 0.00324 AFIX 43 H42 2 0.889530 -0.090500 0.390939 11.00000 -1.20000 AFIX 0 C43 1 0.856589 0.052171 0.380960 11.00000 0.02139 0.01651 = 0.02760 -0.00592 -0.00181 0.00134 AFIX 43 H43 2 0.839550 0.043961 0.348735 11.00000 -1.20000 AFIX 0 C44 1 0.710355 0.059206 0.262134 11.00000 0.02317 0.01911 = 0.01378 -0.00051 0.00235 -0.00796 C45 1 0.770676 0.022658 0.243002 11.00000 0.02531 0.02301 = 0.01785 -0.00308 0.00336 -0.00594 C46 1 0.782633 0.054383 0.197383 11.00000 0.03271 0.03604 = 0.01944 -0.00210 0.00826 -0.00528 AFIX 43 H46 2 0.823297 0.031806 0.183514 11.00000 -1.20000 AFIX 0 C47 1 0.737393 0.117268 0.171921 11.00000 0.03807 0.04069 = 0.01832 0.00495 0.00707 -0.00722 AFIX 43 H47 2 0.747641 0.138712 0.141244 11.00000 -1.20000 AFIX 0 C48 1 0.677075 0.149388 0.190793 11.00000 0.03205 0.03259 = 0.02061 0.00682 -0.00040 -0.00445 AFIX 43 H48 2 0.645737 0.191872 0.172637 11.00000 -1.20000 AFIX 0 C49 1 0.661360 0.120320 0.236283 11.00000 0.02492 0.02462 = 0.01749 0.00199 0.00063 -0.00659 C50 1 0.821792 -0.052293 0.266319 11.00000 0.02615 0.03025 = 0.01807 -0.00488 0.00429 -0.00051 AFIX 13 H50 2 0.809318 -0.063062 0.299586 11.00000 -1.20000 AFIX 0 C51 1 0.813784 -0.151991 0.239772 11.00000 0.04801 0.03556 = 0.02351 -0.01013 0.00112 0.01177 AFIX 137 H51A 2 0.764252 -0.170878 0.236283 11.00000 -1.50000 H51B 2 0.840632 -0.203310 0.257795 11.00000 -1.50000 H51C 2 0.831373 -0.145225 0.208345 11.00000 -1.50000 AFIX 0 C52 1 0.897858 -0.017183 0.268221 11.00000 0.02558 0.06574 = 0.02820 0.00692 0.00369 -0.00584 AFIX 137 H52A 2 0.913676 -0.016852 0.236127 11.00000 -1.50000 H52B 2 0.927383 -0.062261 0.288314 11.00000 -1.50000 H52C 2 0.901262 0.050065 0.281440 11.00000 -1.50000 AFIX 0 C53 1 0.592453 0.156890 0.253282 11.00000 0.02342 0.03662 = 0.02192 0.00713 -0.00042 -0.00084 AFIX 13 H53 2 0.588182 0.131486 0.286138 11.00000 -1.20000 AFIX 0 C54 1 0.590297 0.270169 0.254279 11.00000 0.03022 0.03819 = 0.03884 0.00244 -0.00404 0.00863 AFIX 137 H54A 2 0.631406 0.295280 0.273435 11.00000 -1.50000 H54B 2 0.547662 0.292104 0.268165 11.00000 -1.50000 H54C 2 0.590438 0.295852 0.221878 11.00000 -1.50000 AFIX 0 C55 1 0.529707 0.118997 0.220998 11.00000 0.02759 0.05662 = 0.02972 0.00898 -0.00351 -0.01105 AFIX 137 H55A 2 0.529206 0.151688 0.190026 11.00000 -1.50000 H55B 2 0.486185 0.134130 0.235510 11.00000 -1.50000 H55C 2 0.533744 0.047025 0.216884 11.00000 -1.50000 AFIX 0 C56 1 0.604327 -0.095744 0.283642 11.00000 0.04264 0.03317 = 0.02512 -0.00545 0.00529 -0.02215 AFIX 137 H56A 2 0.568912 -0.044274 0.276443 11.00000 -1.50000 H56B 2 0.581387 -0.157125 0.292710 11.00000 -1.50000 H56C 2 0.629865 -0.108033 0.255558 11.00000 -1.50000 AFIX 0 C57 1 0.707660 -0.143437 0.338413 11.00000 0.04529 0.01583 = 0.03484 0.00112 0.01567 -0.00373 AFIX 137 H57A 2 0.729432 -0.166901 0.310283 11.00000 -1.50000 H57B 2 0.683455 -0.198744 0.352585 11.00000 -1.50000 H57C 2 0.743854 -0.117256 0.361525 11.00000 -1.50000 AFIX 0 C58 1 0.284562 0.305813 0.517305 11.00000 0.04296 0.05760 = 0.03670 0.01570 0.00996 0.00339 AFIX 23 H58A 2 0.286597 0.272923 0.486151 11.00000 -1.20000 H58B 2 0.287094 0.378418 0.512234 11.00000 -1.20000 AFIX 0 C59 1 0.546749 0.268888 0.564561 11.00000 0.05049 0.02802 = 0.03440 0.00015 0.00931 0.00043 AFIX 23 H59A 2 0.516620 0.259923 0.534780 11.00000 -1.20000 H59B 2 0.595037 0.249836 0.558268 11.00000 -1.20000 AFIX 0 HKLF 4 REM sharma53_a.res in P2(1)/c REM wR2 = 0.0974, GooF = S = 1.034, Restrained GooF = 1.034 for all data REM R1 = 0.0360 for 14273 Fo > 4sig(Fo) and 0.0384 for all 15269 data REM 745 parameters refined using 0 restraints END WGHT 0.0530 7.2037 REM Highest difference peak 0.680, deepest hole -0.771, 1-sigma level 0.075 Q1 1 0.2517 -0.0641 0.3942 11.00000 0.05 0.68 Q2 1 0.4221 -0.0527 0.3481 11.00000 0.05 0.53 Q3 1 0.4019 0.0937 0.4403 11.00000 0.05 0.50 Q4 1 0.3041 0.1080 0.3052 11.00000 0.05 0.48 Q5 1 0.2047 0.2172 0.5344 11.00000 0.05 0.43 ; _shelx_res_checksum 65402 _olex2_date_sample_data_collection 2019-08-26 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.332 _oxdiff_exptl_absorpt_empirical_full_min 0.377 ####################################################################### # # 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_compound5 _database_code_depnum_ccdc_archive 'CCDC 1949889' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-08-02 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' georg.stammler@uni-bielefeld.de _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C57 H76 N3 P' _chemical_formula_sum 'C57 H76 N3 P' _chemical_formula_weight 834.17 _chemical_melting_point ? _chemical_oxdiff_formula C57H76N3P loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.56527(11) _cell_length_b 11.96597(7) _cell_length_c 22.85445(16) _cell_angle_alpha 90 _cell_angle_beta 101.6144(6) _cell_angle_gamma 90 _cell_volume 4973.19(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 64190 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 76.3380 _cell_measurement_theta_min 3.6430 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear brownish orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier brownish _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1816 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 -2 0.0657 2 -1 0 0.1346 0 0 -1 0.1276 2 1 -1 0.1653 -1 -2 -1 0.1628 -2 -1 1 0.1726 0 1 1 0.1321 1 0 -2 0.1431 -1 1 2 0.1980 -1 -1 2 0.1679 0 -1 0 0.1614 0 1 0 0.1203 0 -1 2 0.1484 -1 2 -1 0.0995 1 0 1 0.1824 -1 0 0 0.1558 1 0 0 0.1735 -2 -1 -2 0.1571 -1 -1 -2 0.1364 _exptl_crystal_size_max 0.428 _exptl_crystal_size_mid 0.332 _exptl_crystal_size_min 0.245 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.9762 1.0312 -1.9687 -0.1102 -0.1869 0.0165 1.9405 -1.0531 -0.0501 0.1227 0.1282 0.1170 -0.0195 0.0026 -0.9948 -0.0327 -0.0332 0.0506 2.0530 0.9469 -1.0615 0.1562 -0.1305 0.0625 -1.1547 -1.9676 -0.9490 -0.1768 0.1846 0.1236 -2.0530 -0.9469 1.0615 -0.1562 0.1305 -0.0625 0.0854 0.9961 0.9865 0.0658 -0.0796 -0.1032 0.9644 -0.0219 -2.0188 0.0125 -0.0586 0.1335 -0.8984 1.0206 2.0105 0.0206 -0.0541 -0.1860 -1.0303 -0.9768 2.0271 -0.0456 0.1714 -0.0809 -0.0660 -0.9987 0.0083 -0.0331 0.1127 0.0526 0.0660 0.9987 -0.0083 0.0331 -0.1127 -0.0526 -0.0271 -1.0040 1.9979 0.0323 0.1791 -0.0487 -0.8907 2.0273 -0.9822 -0.0444 -0.2664 -0.0868 1.0227 -0.0299 0.9656 0.1106 0.0409 -0.0184 -1.0033 0.0272 0.0292 -0.0779 -0.0077 -0.0322 1.0033 -0.0272 -0.0292 0.0779 0.0077 0.0322 -2.1114 -0.9390 -1.9229 -0.2543 0.0309 0.0894 -1.1081 -0.9662 -1.9521 -0.1764 0.0386 0.1216 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 142708 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.911 _diffrn_reflns_theta_min 2.430 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -64.00 30.00 1.00 2.50 -- -38.50 57.00 120.00 94 2 \w -124.00 47.00 1.00 2.50 -- -38.50 0.00 60.00 171 3 \w -87.00 -6.00 1.00 2.50 -- -38.50 125.00 150.00 81 4 \w 18.00 111.00 1.00 2.50 -- 42.89 57.00-120.00 93 5 \w 18.00 111.00 1.00 2.50 -- 42.89 57.00 120.00 93 6 \w 22.00 114.00 1.00 2.50 -- 42.89 38.00 30.00 92 7 \w 14.00 113.00 1.00 2.50 -- 42.89 73.00-101.60 99 8 \w 27.00 97.00 1.00 2.50 -- 42.89-125.00 30.00 70 9 \w 14.00 113.00 1.00 2.50 -- 42.89 72.00 140.00 99 10 \w 12.00 42.00 1.00 2.50 -- 42.89 81.00 178.39 30 11 \w 12.00 42.00 1.00 2.50 -- 42.89 81.00 101.76 30 12 \w 12.00 42.00 1.00 2.50 -- 42.89 80.00 -52.82 30 13 \w 12.00 42.00 1.00 2.50 -- 42.89 81.00 34.54 30 14 \w 15.00 112.00 1.00 2.50 -- 42.89 68.00 -21.87 97 15 \w 14.00 113.00 1.00 2.50 -- 42.89 72.00 29.88 99 16 \w 27.00 97.00 1.00 2.50 -- 42.89-125.00 -30.00 70 17 \w 82.00 178.00 1.00 10.00 -- 111.00 72.00 163.64 96 18 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00-175.96 93 19 \w 84.00 178.00 1.00 10.00 -- 111.00 63.00 136.57 94 20 \w 82.00 178.00 1.00 10.00 -- 111.00 74.00 107.27 96 21 \w 86.00 178.00 1.00 10.00 -- 111.00 55.00 174.59 92 22 \w 85.00 178.00 1.00 10.00 -- 111.00 60.00 45.28 93 23 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00 47.09 93 24 \w 86.00 178.00 1.00 10.00 -- 111.00 58.00 -76.64 92 25 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00-126.03 93 26 \w 82.00 178.00 1.00 10.00 -- 111.00 72.00 -82.85 96 27 \w 85.00 178.00 1.00 10.00 -- 111.00 62.00-168.96 93 28 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00-150.00 93 29 \w 83.00 178.00 1.00 10.00 -- 111.00 70.00 4.84 95 30 \w 84.00 178.00 1.00 10.00 -- 111.00 65.00-161.95 94 31 \w 86.00 178.00 1.00 10.00 -- 111.00 58.00 -0.31 92 32 \w 83.00 178.00 1.00 10.00 -- 111.00 68.00-111.86 95 33 \w 31.00 107.00 1.00 10.00 -- 111.00 -94.00 150.00 76 34 \w 83.00 178.00 1.00 10.00 -- 111.00 67.00 61.43 95 35 \w 83.00 178.00 1.00 10.00 -- 111.00 69.00 -26.70 95 36 \w 86.00 178.00 1.00 10.00 -- 111.00 58.00 100.14 92 37 \w 40.00 141.00 1.00 10.00 -- 111.00 -77.00 -60.00 101 38 \w 31.00 107.00 1.00 10.00 -- 111.00 -94.00 -90.00 76 39 \w 31.00 107.00 1.00 10.00 -- 111.00 -94.00 90.00 76 40 \w 85.00 178.00 1.00 10.00 -- 111.00 62.00-140.37 93 41 \w 34.00 107.00 1.00 10.00 -- 111.00-101.00-139.95 73 42 \w 84.00 178.00 1.00 10.00 -- 111.00 64.00 -39.03 94 43 \w 41.00 133.00 1.00 10.00 -- 111.00 -45.00 120.00 92 44 \w 85.00 165.00 1.00 10.00 -- 111.00 61.00 30.00 80 45 \w 33.00 107.00 1.00 10.00 -- 111.00 -94.00 60.00 74 46 \w 85.00 111.00 1.00 10.00 -- 111.00 61.00 90.00 26 47 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 0.00 27 48 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 -30.00 27 49 \w 87.00 112.00 1.00 10.00 -- 111.00 56.00 82.08 25 50 \w 89.00 116.00 1.00 10.00 -- 111.00 45.00-180.00 27 51 \w 86.00 122.00 1.00 10.00 -- 111.00 55.00 117.00 36 52 \w 85.00 165.00 1.00 10.00 -- 111.00 61.00-120.00 80 53 \w 53.00 80.00 1.00 10.00 -- 111.00 -94.00 120.00 27 54 \w 82.00 107.00 1.00 10.00 -- 111.00 -94.00 120.00 25 55 \w 49.00 108.00 1.00 10.00 -- 111.00-105.00 18.55 59 56 \w 86.00 112.00 1.00 10.00 -- 111.00 55.00 67.05 26 57 \w 84.00 110.00 1.00 10.00 -- 111.00 63.00 -51.59 26 58 \w 119.00 177.00 1.00 10.00 -- 111.00 70.00 142.33 58 59 \w 85.00 176.00 1.00 10.00 -- 111.00 61.00 -60.00 91 60 \w 86.00 111.00 1.00 10.00 -- 111.00 61.00 -90.00 25 61 \w 83.00 109.00 1.00 10.00 -- 111.00 70.00 142.33 26 62 \w 85.00 111.00 1.00 10.00 -- 111.00 59.00 -91.60 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0793358000 _diffrn_orient_matrix_UB_12 0.0281599000 _diffrn_orient_matrix_UB_13 0.0314052000 _diffrn_orient_matrix_UB_21 0.0056074000 _diffrn_orient_matrix_UB_22 -0.1129886000 _diffrn_orient_matrix_UB_23 0.0329524000 _diffrn_orient_matrix_UB_31 0.0291181000 _diffrn_orient_matrix_UB_32 -0.0550007000 _diffrn_orient_matrix_UB_33 -0.0516063000 _diffrn_oxdiff_digest_frames ; 012caedbe09c26fa864cd64709c4de2f4304536cee8 ; _diffrn_oxdiff_digest_hkl ; 0155ef85aaaa70260cfd703a959ba82dba7b28 ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9389 _reflns_number_total 10414 _reflns_odcompleteness_completeness 99.99 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _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 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.669 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.049 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 564 _refine_ls_number_reflns 10414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0419 _refine_ls_restrained_S_all 1.037 _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^)+(0.0766P)^2^+1.1302P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1173 _refine_ls_wR_factor_ref 0.1215 _refine_special_details 'Hydrogen atoms were taken into account using a riding model.' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C20(H20), C23(H23), C32(H32), C35(H35), C50(H50), C53(H53) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29), C30(H30), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46), C47(H47), C48(H48) 2.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B, H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A, H37B,H37C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 P1 P 0.27082(2) 0.53303(2) 0.14106(2) 0.01600(8) Uani 1 1 d . . . . . N1 N 0.13070(5) 0.62785(8) 0.18616(4) 0.01654(19) Uani 1 1 d . . . . . N2 N 0.11881(5) 0.48645(8) 0.24544(4) 0.01628(19) Uani 1 1 d . . . . . N3 N 0.39790(5) 0.53036(8) 0.10419(4) 0.01702(19) Uani 1 1 d . . . . . C1 C 0.16883(6) 0.53435(8) 0.21360(5) 0.0151(2) Uani 1 1 d . . . . . C2 C 0.06105(6) 0.63422(9) 0.20059(5) 0.0199(2) Uani 1 1 d . . . . . H2 H 0.024904 0.689559 0.186866 0.024 Uiso 1 1 calc R . . . . C3 C 0.05408(6) 0.54962(10) 0.23677(5) 0.0199(2) Uani 1 1 d . . . . . H3 H 0.012417 0.534673 0.253786 0.024 Uiso 1 1 calc R . . . . C4 C 0.23705(6) 0.49459(9) 0.20776(5) 0.0154(2) Uani 1 1 d . . . . . C5 C 0.36613(6) 0.52744(8) 0.15421(5) 0.0153(2) Uani 1 1 d . . . . . C6 C 0.47990(6) 0.52651(9) 0.11766(5) 0.0194(2) Uani 1 1 d . . . . . C7 C 0.49534(6) 0.56674(10) 0.18238(5) 0.0201(2) Uani 1 1 d . . . . . H7A H 0.500552 0.649081 0.183949 0.024 Uiso 1 1 calc R . . . . H7B H 0.541424 0.533077 0.204777 0.024 Uiso 1 1 calc R . . . . C8 C 0.42939(6) 0.53009(9) 0.20985(5) 0.0166(2) Uani 1 1 d . . . . . C9 C 0.41197(6) 0.61716(9) 0.25452(5) 0.0208(2) Uani 1 1 d . . . . . H9A H 0.404895 0.690978 0.234631 0.025 Uiso 1 1 calc R . . . . H9B H 0.365285 0.596543 0.266383 0.025 Uiso 1 1 calc R . . . . C10 C 0.47263(7) 0.62665(11) 0.31066(6) 0.0271(3) Uani 1 1 d . . . . . H10A H 0.518085 0.655151 0.299504 0.033 Uiso 1 1 calc R . . . . H10B H 0.457410 0.680900 0.338552 0.033 Uiso 1 1 calc R . . . . C11 C 0.48848(8) 0.51395(11) 0.34193(5) 0.0290(3) Uani 1 1 d . . . . . H11A H 0.529863 0.521908 0.376532 0.035 Uiso 1 1 calc R . . . . H11B H 0.444714 0.489033 0.356986 0.035 Uiso 1 1 calc R . . . . C12 C 0.50786(7) 0.42678(10) 0.29898(5) 0.0243(2) Uani 1 1 d . . . . . H12A H 0.515155 0.353381 0.319294 0.029 Uiso 1 1 calc R . . . . H12B H 0.554511 0.447931 0.287215 0.029 Uiso 1 1 calc R . . . . C13 C 0.44668(6) 0.41708(9) 0.24286(5) 0.0180(2) Uani 1 1 d . . . . . H13A H 0.401464 0.388673 0.254465 0.022 Uiso 1 1 calc R . . . . H13B H 0.461714 0.362121 0.215233 0.022 Uiso 1 1 calc R . . . . C14 C 0.15373(6) 0.72256(9) 0.15568(5) 0.0174(2) Uani 1 1 d . . . . . C15 C 0.12318(6) 0.73545(10) 0.09465(5) 0.0204(2) Uani 1 1 d . . . . . C16 C 0.13037(7) 0.83945(10) 0.06878(5) 0.0261(3) Uani 1 1 d . . . . . H16 H 0.108871 0.851036 0.027868 0.031 Uiso 1 1 calc R . . . . C17 C 0.16807(8) 0.92574(10) 0.10142(6) 0.0291(3) Uani 1 1 d . . . . . H17 H 0.171322 0.996465 0.083243 0.035 Uiso 1 1 calc R . . . . C18 C 0.20131(8) 0.90914(10) 0.16095(6) 0.0268(3) Uani 1 1 d . . . . . H18 H 0.229204 0.967814 0.182585 0.032 Uiso 1 1 calc R . . . . C19 C 0.19439(6) 0.80775(9) 0.18941(5) 0.0204(2) Uani 1 1 d . . . . . C20 C 0.08437(7) 0.64136(11) 0.05632(5) 0.0241(2) Uani 1 1 d . . . . . H20 H 0.087497 0.572761 0.081706 0.029 Uiso 1 1 calc R . . . . C21 C 0.12282(7) 0.61648(11) 0.00420(5) 0.0274(3) Uani 1 1 d . . . . . H21A H 0.120437 0.682686 -0.021354 0.041 Uiso 1 1 calc GR . . . . H21B H 0.098171 0.553768 -0.019222 0.041 Uiso 1 1 calc GR . . . . H21C H 0.174367 0.597107 0.019932 0.041 Uiso 1 1 calc GR . . . . C22 C 0.00274(8) 0.66844(14) 0.03344(6) 0.0354(3) Uani 1 1 d . . . . . H22A H -0.021810 0.675656 0.067405 0.053 Uiso 1 1 calc GR . . . . H22B H -0.020358 0.608135 0.007210 0.053 Uiso 1 1 calc GR . . . . H22C H -0.001730 0.738836 0.011076 0.053 Uiso 1 1 calc GR . . . . C23 C 0.22691(7) 0.79134(10) 0.25535(5) 0.0231(2) Uani 1 1 d . . . . . H23 H 0.239673 0.710453 0.261644 0.028 Uiso 1 1 calc R . . . . C24 C 0.29720(7) 0.85886(11) 0.27668(6) 0.0288(3) Uani 1 1 d . . . . . H24A H 0.331035 0.846564 0.249467 0.043 Uiso 1 1 calc GR . . . . H24B H 0.320614 0.834803 0.317019 0.043 Uiso 1 1 calc GR . . . . H24C H 0.285004 0.938483 0.277231 0.043 Uiso 1 1 calc GR . . . . C25 C 0.17009(8) 0.81976(14) 0.29333(6) 0.0348(3) Uani 1 1 d . . . . . H25A H 0.156843 0.898955 0.288321 0.052 Uiso 1 1 calc GR . . . . H25B H 0.191054 0.804701 0.335472 0.052 Uiso 1 1 calc GR . . . . H25C H 0.126064 0.773776 0.280493 0.052 Uiso 1 1 calc GR . . . . C26 C 0.12159(6) 0.37918(9) 0.27422(5) 0.0166(2) Uani 1 1 d . . . . . C27 C 0.11446(6) 0.28190(9) 0.23905(5) 0.0186(2) Uani 1 1 d . . . . . C28 C 0.11987(6) 0.17920(10) 0.26857(6) 0.0231(2) Uani 1 1 d . . . . . H28 H 0.117683 0.112083 0.246077 0.028 Uiso 1 1 calc R . . . . C29 C 0.12839(6) 0.17348(10) 0.33017(6) 0.0247(2) Uani 1 1 d . . . . . H29 H 0.132696 0.102863 0.349551 0.030 Uiso 1 1 calc R . . . . C30 C 0.13063(6) 0.27043(10) 0.36346(5) 0.0228(2) Uani 1 1 d . . . . . H30 H 0.134259 0.265497 0.405436 0.027 Uiso 1 1 calc R . . . . C31 C 0.12765(6) 0.37539(10) 0.33640(5) 0.0195(2) Uani 1 1 d . . . . . C32 C 0.09687(6) 0.28958(10) 0.17118(5) 0.0219(2) Uani 1 1 d . . . . . H32 H 0.125617 0.353254 0.159152 0.026 Uiso 1 1 calc R . . . . C33 C 0.11658(7) 0.18423(11) 0.14001(6) 0.0267(3) Uani 1 1 d . . . . . H33A H 0.084307 0.122819 0.146794 0.040 Uiso 1 1 calc GR . . . . H33B H 0.167867 0.163982 0.156219 0.040 Uiso 1 1 calc GR . . . . H33C H 0.110216 0.198317 0.097034 0.040 Uiso 1 1 calc GR . . . . C34 C 0.01467(7) 0.31509(12) 0.14932(6) 0.0316(3) Uani 1 1 d . . . . . H34A H 0.003986 0.322808 0.105742 0.047 Uiso 1 1 calc GR . . . . H34B H 0.002299 0.384864 0.167481 0.047 Uiso 1 1 calc GR . . . . H34C H -0.014674 0.253844 0.160820 0.047 Uiso 1 1 calc GR . . . . C35 C 0.12907(7) 0.47999(11) 0.37422(5) 0.0264(3) Uani 1 1 d . . . . . H35 H 0.134245 0.546087 0.348611 0.032 Uiso 1 1 calc R . . . . C36 C 0.19298(8) 0.48173(14) 0.42830(6) 0.0361(3) Uani 1 1 d . . . . . H36A H 0.186658 0.421251 0.455743 0.054 Uiso 1 1 calc GR . . . . H36B H 0.193721 0.553682 0.448901 0.054 Uiso 1 1 calc GR . . . . H36C H 0.239444 0.471375 0.414875 0.054 Uiso 1 1 calc GR . . . . C37 C 0.05605(9) 0.49123(14) 0.39554(7) 0.0395(3) Uani 1 1 d . . . . . H37A H 0.015040 0.486929 0.361108 0.059 Uiso 1 1 calc GR . . . . H37B H 0.054695 0.563323 0.415632 0.059 Uiso 1 1 calc GR . . . . H37C H 0.051837 0.430601 0.423483 0.059 Uiso 1 1 calc GR . . . . C38 C 0.28698(6) 0.39836(10) 0.30526(5) 0.0203(2) Uani 1 1 d . . . . . H38 H 0.279223 0.464828 0.325868 0.024 Uiso 1 1 calc R . . . . C39 C 0.31658(7) 0.30475(11) 0.33767(5) 0.0256(3) Uani 1 1 d . . . . . H39 H 0.328449 0.307881 0.380055 0.031 Uiso 1 1 calc R . . . . C40 C 0.32884(7) 0.20706(11) 0.30854(6) 0.0261(3) Uani 1 1 d . . . . . H40 H 0.348337 0.143018 0.330769 0.031 Uiso 1 1 calc R . . . . C41 C 0.31234(6) 0.20378(10) 0.24657(6) 0.0228(2) Uani 1 1 d . . . . . H41 H 0.321420 0.137699 0.226175 0.027 Uiso 1 1 calc R . . . . C42 C 0.28262(6) 0.29689(9) 0.21443(5) 0.0183(2) Uani 1 1 d . . . . . H42 H 0.271517 0.293532 0.172031 0.022 Uiso 1 1 calc R . . . . C43 C 0.26856(6) 0.39594(9) 0.24301(5) 0.0162(2) Uani 1 1 d . . . . . C44 C 0.35619(6) 0.52673(10) 0.04400(5) 0.0183(2) Uani 1 1 d . . . . . C45 C 0.34495(6) 0.62776(10) 0.01136(5) 0.0223(2) Uani 1 1 d . . . . . C46 C 0.30821(7) 0.62317(11) -0.04830(6) 0.0273(3) Uani 1 1 d . . . . . H46 H 0.300812 0.690056 -0.071112 0.033 Uiso 1 1 calc R . . . . C47 C 0.28241(7) 0.52310(12) -0.07475(6) 0.0286(3) Uani 1 1 d . . . . . H47 H 0.258403 0.521433 -0.115589 0.034 Uiso 1 1 calc R . . . . C48 C 0.29158(7) 0.42542(11) -0.04171(5) 0.0251(2) Uani 1 1 d . . . . . H48 H 0.272793 0.357363 -0.060107 0.030 Uiso 1 1 calc R . . . . C49 C 0.32784(6) 0.42462(10) 0.01809(5) 0.0201(2) Uani 1 1 d . . . . . C50 C 0.36762(7) 0.74096(10) 0.03952(6) 0.0265(3) Uani 1 1 d . . . . . H50 H 0.402369 0.727325 0.078357 0.032 Uiso 1 1 calc R . . . . C51 C 0.40728(8) 0.81486(12) 0.00106(7) 0.0343(3) Uani 1 1 d . . . . . H51A H 0.448469 0.773316 -0.009279 0.051 Uiso 1 1 calc GR . . . . H51B H 0.425886 0.882214 0.023490 0.051 Uiso 1 1 calc GR . . . . H51C H 0.372802 0.836210 -0.035580 0.051 Uiso 1 1 calc GR . . . . C52 C 0.30093(8) 0.80237(12) 0.05304(7) 0.0348(3) Uani 1 1 d . . . . . H52A H 0.265019 0.814404 0.015817 0.052 Uiso 1 1 calc GR . . . . H52B H 0.316398 0.874673 0.071508 0.052 Uiso 1 1 calc GR . . . . H52C H 0.278472 0.757522 0.080480 0.052 Uiso 1 1 calc GR . . . . C53 C 0.33094(7) 0.31514(10) 0.05219(5) 0.0232(2) Uani 1 1 d . . . . . H53 H 0.355738 0.329160 0.094600 0.028 Uiso 1 1 calc R . . . . C54 C 0.37409(9) 0.22414(11) 0.02654(6) 0.0326(3) Uani 1 1 d . . . . . H54A H 0.348201 0.204728 -0.013899 0.049 Uiso 1 1 calc GR . . . . H54B H 0.378258 0.157653 0.052039 0.049 Uiso 1 1 calc GR . . . . H54C H 0.423354 0.251997 0.025127 0.049 Uiso 1 1 calc GR . . . . C55 C 0.51561(7) 0.60139(12) 0.07722(6) 0.0262(3) Uani 1 1 d . . . . . H55A H 0.491608 0.589110 0.035441 0.039 Uiso 1 1 calc GR . . . . H55B H 0.567983 0.583102 0.082575 0.039 Uiso 1 1 calc GR . . . . H55C H 0.510094 0.679876 0.087743 0.039 Uiso 1 1 calc GR . . . . C56 C 0.50662(7) 0.40722(11) 0.10966(6) 0.0254(3) Uani 1 1 d . . . . . H56A H 0.481076 0.354841 0.131436 0.038 Uiso 1 1 calc GR . . . . H56B H 0.559710 0.402706 0.125315 0.038 Uiso 1 1 calc GR . . . . H56C H 0.496145 0.387903 0.067119 0.038 Uiso 1 1 calc GR . . . . C57 C 0.25252(8) 0.27301(12) 0.05151(6) 0.0304(3) Uani 1 1 d . . . . . H57A H 0.224721 0.330995 0.067645 0.046 Uiso 1 1 calc GR . . . . H57B H 0.254775 0.205474 0.076063 0.046 Uiso 1 1 calc GR . . . . H57C H 0.228087 0.255722 0.010379 0.046 Uiso 1 1 calc GR . . . . 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 P1 0.01825(14) 0.01861(15) 0.01238(14) 0.00260(9) 0.00606(10) 0.00203(9) N1 0.0199(4) 0.0150(4) 0.0159(4) 0.0020(3) 0.0064(3) 0.0021(3) N2 0.0195(4) 0.0154(4) 0.0157(4) 0.0012(3) 0.0076(3) 0.0017(3) N3 0.0189(4) 0.0207(5) 0.0126(4) 0.0017(3) 0.0060(3) 0.0013(3) C1 0.0214(5) 0.0136(5) 0.0111(5) 0.0001(4) 0.0049(4) -0.0008(4) C2 0.0206(5) 0.0193(5) 0.0209(5) 0.0007(4) 0.0068(4) 0.0041(4) C3 0.0202(5) 0.0206(5) 0.0208(5) 0.0006(4) 0.0084(4) 0.0030(4) C4 0.0198(5) 0.0153(5) 0.0123(5) 0.0004(4) 0.0060(4) -0.0004(4) C5 0.0216(5) 0.0130(5) 0.0129(5) 0.0012(4) 0.0072(4) 0.0005(4) C6 0.0188(5) 0.0237(6) 0.0169(5) 0.0020(4) 0.0064(4) 0.0006(4) C7 0.0216(5) 0.0219(5) 0.0177(5) 0.0011(4) 0.0062(4) -0.0026(4) C8 0.0200(5) 0.0161(5) 0.0144(5) -0.0005(4) 0.0052(4) -0.0011(4) C9 0.0272(5) 0.0168(5) 0.0197(5) -0.0027(4) 0.0080(4) -0.0015(4) C10 0.0363(6) 0.0243(6) 0.0207(6) -0.0074(5) 0.0055(5) -0.0073(5) C11 0.0369(7) 0.0323(7) 0.0157(6) -0.0015(5) 0.0002(5) -0.0084(5) C12 0.0250(5) 0.0258(6) 0.0205(6) 0.0047(5) 0.0004(4) -0.0023(4) C13 0.0211(5) 0.0171(5) 0.0158(5) 0.0002(4) 0.0039(4) -0.0003(4) C14 0.0239(5) 0.0147(5) 0.0152(5) 0.0016(4) 0.0081(4) 0.0031(4) C15 0.0271(5) 0.0203(5) 0.0153(5) 0.0015(4) 0.0080(4) 0.0053(4) C16 0.0394(7) 0.0239(6) 0.0166(5) 0.0049(5) 0.0099(5) 0.0084(5) C17 0.0487(8) 0.0169(6) 0.0262(6) 0.0054(5) 0.0183(6) 0.0049(5) C18 0.0417(7) 0.0163(5) 0.0252(6) -0.0018(5) 0.0139(5) -0.0021(5) C19 0.0288(6) 0.0172(5) 0.0173(5) -0.0010(4) 0.0095(4) 0.0011(4) C20 0.0294(6) 0.0271(6) 0.0159(5) -0.0016(4) 0.0045(4) 0.0020(5) C21 0.0317(6) 0.0334(7) 0.0175(6) -0.0050(5) 0.0056(5) 0.0035(5) C22 0.0291(6) 0.0509(9) 0.0263(7) -0.0065(6) 0.0060(5) 0.0029(6) C23 0.0318(6) 0.0200(5) 0.0177(5) -0.0025(4) 0.0054(4) -0.0039(4) C24 0.0322(6) 0.0275(6) 0.0278(6) -0.0100(5) 0.0087(5) -0.0047(5) C25 0.0364(7) 0.0512(9) 0.0186(6) -0.0076(6) 0.0097(5) -0.0123(6) C26 0.0170(5) 0.0166(5) 0.0173(5) 0.0033(4) 0.0063(4) 0.0006(4) C27 0.0168(5) 0.0187(5) 0.0215(6) 0.0002(4) 0.0069(4) -0.0012(4) C28 0.0226(5) 0.0175(5) 0.0309(6) 0.0009(5) 0.0095(4) -0.0019(4) C29 0.0225(5) 0.0208(6) 0.0325(6) 0.0100(5) 0.0092(5) 0.0003(4) C30 0.0219(5) 0.0280(6) 0.0199(5) 0.0085(5) 0.0074(4) 0.0011(4) C31 0.0196(5) 0.0228(6) 0.0175(5) 0.0027(4) 0.0074(4) 0.0012(4) C32 0.0256(6) 0.0206(5) 0.0204(6) -0.0036(4) 0.0066(4) -0.0028(4) C33 0.0279(6) 0.0253(6) 0.0286(6) -0.0101(5) 0.0095(5) -0.0050(5) C34 0.0309(6) 0.0378(7) 0.0238(6) -0.0074(5) 0.0001(5) 0.0051(5) C35 0.0386(7) 0.0259(6) 0.0164(6) 0.0002(5) 0.0094(5) 0.0022(5) C36 0.0426(8) 0.0468(8) 0.0190(6) -0.0082(6) 0.0064(5) -0.0003(6) C37 0.0436(8) 0.0464(8) 0.0313(7) -0.0035(6) 0.0140(6) 0.0171(7) C38 0.0217(5) 0.0241(6) 0.0168(5) 0.0019(4) 0.0083(4) 0.0022(4) C39 0.0250(6) 0.0345(7) 0.0187(5) 0.0093(5) 0.0075(4) 0.0035(5) C40 0.0233(5) 0.0250(6) 0.0317(7) 0.0135(5) 0.0095(5) 0.0049(4) C41 0.0212(5) 0.0167(5) 0.0324(6) 0.0028(5) 0.0097(4) 0.0006(4) C42 0.0196(5) 0.0173(5) 0.0190(5) 0.0014(4) 0.0064(4) -0.0012(4) C43 0.0160(5) 0.0177(5) 0.0162(5) 0.0030(4) 0.0062(4) -0.0006(4) C44 0.0193(5) 0.0244(6) 0.0129(5) 0.0022(4) 0.0076(4) 0.0020(4) C45 0.0239(5) 0.0266(6) 0.0187(6) 0.0045(5) 0.0096(4) 0.0046(4) C46 0.0303(6) 0.0343(7) 0.0183(6) 0.0099(5) 0.0073(5) 0.0063(5) C47 0.0272(6) 0.0449(8) 0.0139(5) 0.0049(5) 0.0048(4) 0.0026(5) C48 0.0262(6) 0.0349(7) 0.0157(5) -0.0019(5) 0.0075(4) -0.0030(5) C49 0.0222(5) 0.0258(6) 0.0144(5) 0.0001(4) 0.0086(4) 0.0003(4) C50 0.0338(6) 0.0227(6) 0.0255(6) 0.0060(5) 0.0119(5) 0.0041(5) C51 0.0439(8) 0.0268(6) 0.0367(7) 0.0062(6) 0.0189(6) -0.0004(5) C52 0.0430(8) 0.0261(6) 0.0403(8) 0.0067(6) 0.0200(6) 0.0070(5) C53 0.0327(6) 0.0232(6) 0.0150(5) -0.0017(4) 0.0082(4) -0.0031(5) C54 0.0480(8) 0.0263(6) 0.0260(6) -0.0037(5) 0.0132(6) 0.0026(5) C55 0.0242(6) 0.0360(7) 0.0209(6) 0.0051(5) 0.0102(4) -0.0023(5) C56 0.0253(6) 0.0298(6) 0.0225(6) -0.0011(5) 0.0079(4) 0.0072(5) C57 0.0397(7) 0.0325(7) 0.0205(6) -0.0042(5) 0.0095(5) -0.0131(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C4 1.8203(11) . ? P1 C5 1.7354(11) . ? N1 C1 1.4025(13) . ? N1 C2 1.3994(14) . ? N1 C14 1.4396(14) . ? N2 C1 1.4115(14) . ? N2 C3 1.3996(14) . ? N2 C26 1.4386(14) . ? N3 C5 1.3884(14) . ? N3 C6 1.4918(14) . ? N3 C44 1.4370(14) . ? C1 C4 1.3844(15) . ? C2 H2 0.9500 . ? C2 C3 1.3299(17) . ? C3 H3 0.9500 . ? C4 C43 1.4814(14) . ? C5 C8 1.5480(14) . ? C6 C7 1.5266(16) . ? C6 C55 1.5308(16) . ? C6 C56 1.5342(16) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.5475(15) . ? C8 C9 1.5381(15) . ? C8 C13 1.5503(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.5315(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.5268(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.5243(18) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.5369(15) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.4044(15) . ? C14 C19 1.4032(16) . ? C15 C16 1.3957(17) . ? C15 C20 1.5166(16) . ? C16 H16 0.9500 . ? C16 C17 1.3792(19) . ? C17 H17 0.9500 . ? C17 C18 1.3904(18) . ? C18 H18 0.9500 . ? C18 C19 1.3948(16) . ? C19 C23 1.5190(16) . ? C20 H20 1.0000 . ? C20 C21 1.5360(17) . ? C20 C22 1.5350(17) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23 1.0000 . ? C23 C24 1.5288(16) . ? C23 C25 1.5332(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.4056(16) . ? C26 C31 1.4034(16) . ? C27 C28 1.3959(16) . ? C27 C32 1.5222(16) . ? C28 H28 0.9500 . ? C28 C29 1.3863(18) . ? C29 H29 0.9500 . ? C29 C30 1.3833(18) . ? C30 H30 0.9500 . ? C30 C31 1.3962(16) . ? C31 C35 1.5183(17) . ? C32 H32 1.0000 . ? C32 C33 1.5283(16) . ? C32 C34 1.5378(17) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35 1.0000 . ? C35 C36 1.5315(18) . ? C35 C37 1.5358(19) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38 0.9500 . ? C38 C39 1.3933(16) . ? C38 C43 1.3950(15) . ? C39 H39 0.9500 . ? C39 C40 1.3865(19) . ? C40 H40 0.9500 . ? C40 C41 1.3879(19) . ? C41 H41 0.9500 . ? C41 C42 1.3865(16) . ? C42 H42 0.9500 . ? C42 C43 1.4030(16) . ? C44 C45 1.4137(16) . ? C44 C49 1.4124(16) . ? C45 C46 1.3976(17) . ? C45 C50 1.5221(18) . ? C46 H46 0.9500 . ? C46 C47 1.383(2) . ? C47 H47 0.9500 . ? C47 C48 1.3833(19) . ? C48 H48 0.9500 . ? C48 C49 1.3967(16) . ? C49 C53 1.5195(16) . ? C50 H50 1.0000 . ? C50 C51 1.5354(18) . ? C50 C52 1.5240(18) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53 1.0000 . ? C53 C54 1.5363(18) . ? C53 C57 1.5378(17) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 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 C5 P1 C4 110.87(5) . . ? C1 N1 C14 132.23(9) . . ? C2 N1 C1 110.19(9) . . ? C2 N1 C14 116.72(9) . . ? C1 N2 C26 129.15(9) . . ? C3 N2 C1 110.06(9) . . ? C3 N2 C26 119.82(9) . . ? C5 N3 C6 114.48(9) . . ? C5 N3 C44 123.44(9) . . ? C44 N3 C6 121.84(9) . . ? N1 C1 N2 103.26(9) . . ? C4 C1 N1 128.33(10) . . ? C4 C1 N2 128.29(10) . . ? N1 C2 H2 125.8 . . ? C3 C2 N1 108.38(10) . . ? C3 C2 H2 125.8 . . ? N2 C3 H3 125.9 . . ? C2 C3 N2 108.10(10) . . ? C2 C3 H3 125.9 . . ? C1 C4 P1 118.02(8) . . ? C1 C4 C43 119.36(9) . . ? C43 C4 P1 119.46(8) . . ? N3 C5 P1 116.35(8) . . ? N3 C5 C8 107.33(9) . . ? C8 C5 P1 136.06(8) . . ? N3 C6 C7 100.08(9) . . ? N3 C6 C55 113.91(9) . . ? N3 C6 C56 110.19(9) . . ? C7 C6 C55 112.38(10) . . ? C7 C6 C56 114.00(9) . . ? C55 C6 C56 106.43(10) . . ? C6 C7 H7A 110.3 . . ? C6 C7 H7B 110.3 . . ? C6 C7 C8 107.11(9) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? C5 C8 C13 115.49(8) . . ? C7 C8 C5 101.77(9) . . ? C7 C8 C13 109.97(9) . . ? C9 C8 C5 109.45(9) . . ? C9 C8 C7 111.51(9) . . ? C9 C8 C13 108.56(9) . . ? C8 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C10 C9 C8 112.88(10) . . ? C10 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C11 C10 C9 111.50(10) . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C12 C11 C10 110.56(10) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C11 C12 C13 111.01(10) . . ? H12A C12 H12B 108.0 . . ? C13 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C8 C13 H13A 109.1 . . ? C8 C13 H13B 109.1 . . ? C12 C13 C8 112.71(9) . . ? C12 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 N1 117.85(10) . . ? C19 C14 N1 119.04(10) . . ? C19 C14 C15 122.06(10) . . ? C14 C15 C20 122.82(10) . . ? C16 C15 C14 117.70(11) . . ? C16 C15 C20 119.48(10) . . ? C15 C16 H16 119.3 . . ? C17 C16 C15 121.32(11) . . ? C17 C16 H16 119.3 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 119.95(11) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.5 . . ? C17 C18 C19 121.08(12) . . ? C19 C18 H18 119.5 . . ? C14 C19 C23 120.90(10) . . ? C18 C19 C14 117.74(11) . . ? C18 C19 C23 121.31(10) . . ? C15 C20 H20 108.0 . . ? C15 C20 C21 110.54(10) . . ? C15 C20 C22 111.20(10) . . ? C21 C20 H20 108.0 . . ? C22 C20 H20 108.0 . . ? C22 C20 C21 110.96(10) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23 107.7 . . ? C19 C23 C24 113.04(10) . . ? C19 C23 C25 110.59(10) . . ? C24 C23 H23 107.7 . . ? C24 C23 C25 110.03(10) . . ? C25 C23 H23 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N2 119.13(10) . . ? C31 C26 N2 118.69(10) . . ? C31 C26 C27 122.10(10) . . ? C26 C27 C32 120.60(10) . . ? C28 C27 C26 117.60(10) . . ? C28 C27 C32 121.70(10) . . ? C27 C28 H28 119.4 . . ? C29 C28 C27 121.11(11) . . ? C29 C28 H28 119.4 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.12(11) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 119.4 . . ? C29 C30 C31 121.11(11) . . ? C31 C30 H30 119.4 . . ? C26 C31 C35 122.58(10) . . ? C30 C31 C26 117.74(11) . . ? C30 C31 C35 119.66(10) . . ? C27 C32 H32 108.0 . . ? C27 C32 C33 113.75(10) . . ? C27 C32 C34 109.77(10) . . ? C33 C32 H32 108.0 . . ? C33 C32 C34 109.11(10) . . ? C34 C32 H32 108.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35 108.1 . . ? C31 C35 C36 113.11(11) . . ? C31 C35 C37 109.73(11) . . ? C36 C35 H35 108.1 . . ? C36 C35 C37 109.43(11) . . ? C37 C35 H35 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38 119.5 . . ? C39 C38 C43 120.99(11) . . ? C43 C38 H38 119.5 . . ? C38 C39 H39 119.7 . . ? C40 C39 C38 120.52(11) . . ? C40 C39 H39 119.7 . . ? C39 C40 H40 120.3 . . ? C39 C40 C41 119.34(11) . . ? C41 C40 H40 120.3 . . ? C40 C41 H41 120.0 . . ? C42 C41 C40 120.03(11) . . ? C42 C41 H41 120.0 . . ? C41 C42 H42 119.2 . . ? C41 C42 C43 121.58(11) . . ? C43 C42 H42 119.2 . . ? C38 C43 C4 121.80(10) . . ? C38 C43 C42 117.51(10) . . ? C42 C43 C4 120.68(10) . . ? C45 C44 N3 118.23(10) . . ? C49 C44 N3 120.73(10) . . ? C49 C44 C45 121.04(10) . . ? C44 C45 C50 122.62(10) . . ? C46 C45 C44 118.18(11) . . ? C46 C45 C50 119.12(11) . . ? C45 C46 H46 119.4 . . ? C47 C46 C45 121.25(12) . . ? C47 C46 H46 119.4 . . ? C46 C47 H47 120.0 . . ? C46 C47 C48 119.95(11) . . ? C48 C47 H47 120.0 . . ? C47 C48 H48 119.3 . . ? C47 C48 C49 121.47(12) . . ? C49 C48 H48 119.3 . . ? C44 C49 C53 123.95(10) . . ? C48 C49 C44 118.02(11) . . ? C48 C49 C53 117.95(11) . . ? C45 C50 H50 107.7 . . ? C45 C50 C51 113.21(11) . . ? C45 C50 C52 110.37(11) . . ? C51 C50 H50 107.7 . . ? C52 C50 H50 107.7 . . ? C52 C50 C51 109.95(11) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53 108.4 . . ? C49 C53 C54 112.59(10) . . ? C49 C53 C57 109.85(10) . . ? C54 C53 H53 108.4 . . ? C54 C53 C57 109.22(11) . . ? C57 C53 H53 108.4 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C6 C55 H55A 109.5 . . ? C6 C55 H55B 109.5 . . ? C6 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C6 C56 H56A 109.5 . . ? C6 C56 H56B 109.5 . . ? C6 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C53 C57 H57A 109.5 . . ? C53 C57 H57B 109.5 . . ? C53 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C4 C43 C38 136.27(9) . . . . ? P1 C4 C43 C42 -42.16(13) . . . . ? P1 C5 C8 C7 -159.01(9) . . . . ? P1 C5 C8 C9 -40.93(14) . . . . ? P1 C5 C8 C13 81.92(13) . . . . ? N1 C1 C4 P1 -22.54(15) . . . . ? N1 C1 C4 C43 177.63(10) . . . . ? N1 C2 C3 N2 -0.91(13) . . . . ? N1 C14 C15 C16 164.10(10) . . . . ? N1 C14 C15 C20 -16.89(16) . . . . ? N1 C14 C19 C18 -165.40(10) . . . . ? N1 C14 C19 C23 12.08(16) . . . . ? N2 C1 C4 P1 152.84(9) . . . . ? N2 C1 C4 C43 -6.99(17) . . . . ? N2 C26 C27 C28 177.90(10) . . . . ? N2 C26 C27 C32 -5.70(15) . . . . ? N2 C26 C31 C30 -179.68(10) . . . . ? N2 C26 C31 C35 1.90(16) . . . . ? N3 C5 C8 C7 14.69(10) . . . . ? N3 C5 C8 C9 132.78(9) . . . . ? N3 C5 C8 C13 -104.37(10) . . . . ? N3 C6 C7 C8 29.78(11) . . . . ? N3 C44 C45 C46 176.23(10) . . . . ? N3 C44 C45 C50 -7.07(16) . . . . ? N3 C44 C49 C48 -176.21(10) . . . . ? N3 C44 C49 C53 7.08(17) . . . . ? C1 N1 C2 C3 0.98(13) . . . . ? C1 N1 C14 C15 115.73(13) . . . . ? C1 N1 C14 C19 -75.73(15) . . . . ? C1 N2 C3 C2 0.54(13) . . . . ? C1 N2 C26 C27 -66.52(15) . . . . ? C1 N2 C26 C31 116.64(12) . . . . ? C1 C4 C43 C38 -64.19(14) . . . . ? C1 C4 C43 C42 117.38(12) . . . . ? C2 N1 C1 N2 -0.62(11) . . . . ? C2 N1 C1 C4 175.66(11) . . . . ? C2 N1 C14 C15 -76.11(13) . . . . ? C2 N1 C14 C19 92.43(13) . . . . ? C3 N2 C1 N1 0.06(11) . . . . ? C3 N2 C1 C4 -176.21(11) . . . . ? C3 N2 C26 C27 101.03(12) . . . . ? C3 N2 C26 C31 -75.81(13) . . . . ? C4 P1 C5 N3 166.13(8) . . . . ? C4 P1 C5 C8 -20.58(12) . . . . ? C5 P1 C4 C1 155.40(8) . . . . ? C5 P1 C4 C43 -44.79(10) . . . . ? C5 N3 C6 C7 -21.41(11) . . . . ? C5 N3 C6 C55 -141.54(10) . . . . ? C5 N3 C6 C56 98.95(11) . . . . ? C5 N3 C44 C45 102.03(12) . . . . ? C5 N3 C44 C49 -78.55(14) . . . . ? C5 C8 C9 C10 -179.02(9) . . . . ? C5 C8 C13 C12 -177.71(10) . . . . ? C6 N3 C5 P1 179.42(7) . . . . ? C6 N3 C5 C8 4.29(12) . . . . ? C6 N3 C44 C45 -84.01(13) . . . . ? C6 N3 C44 C49 95.41(13) . . . . ? C6 C7 C8 C5 -28.06(11) . . . . ? C6 C7 C8 C9 -144.66(9) . . . . ? C6 C7 C8 C13 94.86(10) . . . . ? C7 C8 C9 C10 -67.20(12) . . . . ? C7 C8 C13 C12 67.85(12) . . . . ? C8 C9 C10 C11 -56.22(14) . . . . ? C9 C8 C13 C12 -54.40(12) . . . . ? C9 C10 C11 C12 55.78(14) . . . . ? C10 C11 C12 C13 -55.89(13) . . . . ? C11 C12 C13 C8 56.57(13) . . . . ? C13 C8 C9 C10 54.10(12) . . . . ? C14 N1 C1 N2 168.12(10) . . . . ? C14 N1 C1 C4 -15.61(19) . . . . ? C14 N1 C2 C3 -169.70(10) . . . . ? C14 C15 C16 C17 1.93(18) . . . . ? C14 C15 C20 C21 -120.63(12) . . . . ? C14 C15 C20 C22 115.66(13) . . . . ? C14 C19 C23 C24 150.67(11) . . . . ? C14 C19 C23 C25 -85.45(14) . . . . ? C15 C14 C19 C18 2.64(17) . . . . ? C15 C14 C19 C23 -179.89(11) . . . . ? C15 C16 C17 C18 1.5(2) . . . . ? C16 C15 C20 C21 58.37(14) . . . . ? C16 C15 C20 C22 -65.35(15) . . . . ? C16 C17 C18 C19 -3.1(2) . . . . ? C17 C18 C19 C14 0.99(19) . . . . ? C17 C18 C19 C23 -176.48(12) . . . . ? C18 C19 C23 C24 -31.95(16) . . . . ? C18 C19 C23 C25 91.94(14) . . . . ? C19 C14 C15 C16 -4.07(17) . . . . ? C19 C14 C15 C20 174.94(11) . . . . ? C20 C15 C16 C17 -177.11(12) . . . . ? C26 N2 C1 N1 168.57(10) . . . . ? C26 N2 C1 C4 -7.70(18) . . . . ? C26 N2 C3 C2 -169.21(10) . . . . ? C26 C27 C28 C29 3.07(16) . . . . ? C26 C27 C32 C33 160.10(10) . . . . ? C26 C27 C32 C34 -77.33(13) . . . . ? C26 C31 C35 C36 -129.84(12) . . . . ? C26 C31 C35 C37 107.66(13) . . . . ? C27 C26 C31 C30 3.58(16) . . . . ? C27 C26 C31 C35 -174.84(11) . . . . ? C27 C28 C29 C30 0.91(18) . . . . ? C28 C27 C32 C33 -23.65(15) . . . . ? C28 C27 C32 C34 98.92(13) . . . . ? C28 C29 C30 C31 -2.82(17) . . . . ? C29 C30 C31 C26 0.60(17) . . . . ? C29 C30 C31 C35 179.07(11) . . . . ? C30 C31 C35 C36 51.76(16) . . . . ? C30 C31 C35 C37 -70.73(14) . . . . ? C31 C26 C27 C28 -5.37(16) . . . . ? C31 C26 C27 C32 171.03(10) . . . . ? C32 C27 C28 C29 -173.29(11) . . . . ? C38 C39 C40 C41 0.95(18) . . . . ? C39 C38 C43 C4 -179.99(10) . . . . ? C39 C38 C43 C42 -1.51(16) . . . . ? C39 C40 C41 C42 -1.20(17) . . . . ? C40 C41 C42 C43 0.08(17) . . . . ? C41 C42 C43 C4 179.75(10) . . . . ? C41 C42 C43 C38 1.26(16) . . . . ? C43 C38 C39 C40 0.43(18) . . . . ? C44 N3 C5 P1 -6.22(13) . . . . ? C44 N3 C5 C8 178.65(9) . . . . ? C44 N3 C6 C7 164.12(9) . . . . ? C44 N3 C6 C55 44.00(14) . . . . ? C44 N3 C6 C56 -75.51(12) . . . . ? C44 C45 C46 C47 0.95(18) . . . . ? C44 C45 C50 C51 134.78(12) . . . . ? C44 C45 C50 C52 -101.50(13) . . . . ? C44 C49 C53 C54 -119.71(13) . . . . ? C44 C49 C53 C57 118.33(12) . . . . ? C45 C44 C49 C48 3.19(17) . . . . ? C45 C44 C49 C53 -173.52(11) . . . . ? C45 C46 C47 C48 1.2(2) . . . . ? C46 C45 C50 C51 -48.55(16) . . . . ? C46 C45 C50 C52 75.18(14) . . . . ? C46 C47 C48 C49 -1.23(19) . . . . ? C47 C48 C49 C44 -0.96(18) . . . . ? C47 C48 C49 C53 175.95(11) . . . . ? C48 C49 C53 C54 63.58(15) . . . . ? C48 C49 C53 C57 -58.38(14) . . . . ? C49 C44 C45 C46 -3.19(17) . . . . ? C49 C44 C45 C50 173.51(11) . . . . ? C50 C45 C46 C47 -175.87(12) . . . . ? C55 C6 C7 C8 151.01(9) . . . . ? C56 C6 C7 C8 -87.79(11) . . . . ? _shelx_res_file ; TITL Sharma44 in P21/c #14 sharma44.res created by SHELXL-2018/3 at 09:22:55 on 02-Aug-2019 REM reset to P21/c #14 CELL 1.54184 18.565274 11.965968 22.854448 90 101.6144 90 ZERR 4 0.000108 0.00007 0.000159 0 0.0006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N P UNIT 228 304 12 4 L.S. 4 PLAN 14 TEMP -173.15(10) MORE -1 BOND $H CONF fmap 2 acta OMIT -3 10 21 REM REM REM WGHT 0.076600 1.130200 FVAR 3.08279 P1 4 0.270816 0.533035 0.141057 11.00000 0.01825 0.01861 = 0.01238 0.00260 0.00606 0.00203 N1 3 0.130701 0.627846 0.186159 11.00000 0.01993 0.01496 = 0.01589 0.00201 0.00637 0.00212 N2 3 0.118810 0.486451 0.245435 11.00000 0.01946 0.01542 = 0.01568 0.00121 0.00762 0.00170 N3 3 0.397900 0.530363 0.104187 11.00000 0.01893 0.02068 = 0.01264 0.00170 0.00599 0.00133 C1 1 0.168825 0.534355 0.213597 11.00000 0.02135 0.01361 = 0.01108 0.00014 0.00492 -0.00078 C2 1 0.061053 0.634219 0.200587 11.00000 0.02064 0.01933 = 0.02091 0.00068 0.00678 0.00412 AFIX 43 H2 2 0.024904 0.689559 0.186866 11.00000 -1.20000 AFIX 0 C3 1 0.054080 0.549623 0.236775 11.00000 0.02021 0.02060 = 0.02082 0.00058 0.00842 0.00297 AFIX 43 H3 2 0.012417 0.534673 0.253786 11.00000 -1.20000 AFIX 0 C4 1 0.237052 0.494593 0.207763 11.00000 0.01978 0.01535 = 0.01234 0.00037 0.00597 -0.00036 C5 1 0.366126 0.527436 0.154206 11.00000 0.02165 0.01301 = 0.01285 0.00123 0.00721 0.00047 C6 1 0.479897 0.526513 0.117662 11.00000 0.01883 0.02371 = 0.01690 0.00201 0.00643 0.00062 C7 1 0.495336 0.566738 0.182376 11.00000 0.02158 0.02187 = 0.01771 0.00111 0.00620 -0.00263 AFIX 23 H7A 2 0.500552 0.649081 0.183949 11.00000 -1.20000 H7B 2 0.541424 0.533077 0.204777 11.00000 -1.20000 AFIX 0 C8 1 0.429394 0.530092 0.209846 11.00000 0.02000 0.01614 = 0.01439 -0.00052 0.00517 -0.00110 C9 1 0.411969 0.617159 0.254522 11.00000 0.02724 0.01680 = 0.01968 -0.00272 0.00804 -0.00152 AFIX 23 H9A 2 0.404895 0.690978 0.234631 11.00000 -1.20000 H9B 2 0.365285 0.596543 0.266383 11.00000 -1.20000 AFIX 0 C10 1 0.472631 0.626647 0.310662 11.00000 0.03633 0.02425 = 0.02068 -0.00736 0.00547 -0.00729 AFIX 23 H10A 2 0.518085 0.655151 0.299504 11.00000 -1.20000 H10B 2 0.457410 0.680900 0.338552 11.00000 -1.20000 AFIX 0 C11 1 0.488480 0.513953 0.341929 11.00000 0.03689 0.03229 = 0.01565 -0.00153 0.00020 -0.00842 AFIX 23 H11A 2 0.529863 0.521908 0.376532 11.00000 -1.20000 H11B 2 0.444714 0.489033 0.356986 11.00000 -1.20000 AFIX 0 C12 1 0.507860 0.426782 0.298975 11.00000 0.02501 0.02575 = 0.02050 0.00467 0.00042 -0.00234 AFIX 23 H12A 2 0.515155 0.353381 0.319294 11.00000 -1.20000 H12B 2 0.554511 0.447931 0.287215 11.00000 -1.20000 AFIX 0 C13 1 0.446675 0.417084 0.242859 11.00000 0.02106 0.01712 = 0.01581 0.00022 0.00393 -0.00032 AFIX 23 H13A 2 0.401464 0.388673 0.254465 11.00000 -1.20000 H13B 2 0.461714 0.362121 0.215233 11.00000 -1.20000 AFIX 0 C14 1 0.153727 0.722559 0.155679 11.00000 0.02393 0.01474 = 0.01517 0.00158 0.00815 0.00310 C15 1 0.123176 0.735454 0.094652 11.00000 0.02715 0.02033 = 0.01532 0.00152 0.00801 0.00526 C16 1 0.130371 0.839451 0.068779 11.00000 0.03942 0.02392 = 0.01663 0.00489 0.00992 0.00841 AFIX 43 H16 2 0.108871 0.851036 0.027868 11.00000 -1.20000 AFIX 0 C17 1 0.168072 0.925741 0.101420 11.00000 0.04873 0.01686 = 0.02618 0.00540 0.01825 0.00491 AFIX 43 H17 2 0.171322 0.996465 0.083243 11.00000 -1.20000 AFIX 0 C18 1 0.201315 0.909138 0.160946 11.00000 0.04174 0.01634 = 0.02521 -0.00178 0.01390 -0.00210 AFIX 43 H18 2 0.229204 0.967814 0.182585 11.00000 -1.20000 AFIX 0 C19 1 0.194389 0.807749 0.189413 11.00000 0.02877 0.01721 = 0.01731 -0.00095 0.00951 0.00106 C20 1 0.084371 0.641355 0.056325 11.00000 0.02938 0.02709 = 0.01586 -0.00162 0.00452 0.00204 AFIX 13 H20 2 0.087497 0.572761 0.081706 11.00000 -1.20000 AFIX 0 C21 1 0.122816 0.616477 0.004203 11.00000 0.03169 0.03336 = 0.01748 -0.00501 0.00556 0.00348 AFIX 137 H21A 2 0.120437 0.682686 -0.021354 11.00000 -1.50000 H21B 2 0.098171 0.553768 -0.019222 11.00000 -1.50000 H21C 2 0.174367 0.597107 0.019932 11.00000 -1.50000 AFIX 0 C22 1 0.002739 0.668444 0.033435 11.00000 0.02912 0.05091 = 0.02634 -0.00655 0.00596 0.00293 AFIX 137 H22A 2 -0.021810 0.675656 0.067405 11.00000 -1.50000 H22B 2 -0.020358 0.608135 0.007210 11.00000 -1.50000 H22C 2 -0.001730 0.738836 0.011076 11.00000 -1.50000 AFIX 0 C23 1 0.226908 0.791341 0.255345 11.00000 0.03183 0.01999 = 0.01769 -0.00248 0.00537 -0.00390 AFIX 13 H23 2 0.239673 0.710453 0.261644 11.00000 -1.20000 AFIX 0 C24 1 0.297198 0.858857 0.276680 11.00000 0.03222 0.02752 = 0.02782 -0.01001 0.00869 -0.00468 AFIX 137 H24A 2 0.331035 0.846564 0.249467 11.00000 -1.50000 H24B 2 0.320614 0.834803 0.317019 11.00000 -1.50000 H24C 2 0.285004 0.938483 0.277231 11.00000 -1.50000 AFIX 0 C25 1 0.170092 0.819756 0.293335 11.00000 0.03643 0.05124 = 0.01858 -0.00765 0.00972 -0.01233 AFIX 137 H25A 2 0.156843 0.898955 0.288321 11.00000 -1.50000 H25B 2 0.191054 0.804701 0.335472 11.00000 -1.50000 H25C 2 0.126064 0.773776 0.280493 11.00000 -1.50000 AFIX 0 C26 1 0.121587 0.379180 0.274221 11.00000 0.01699 0.01664 = 0.01733 0.00331 0.00625 0.00062 C27 1 0.114455 0.281904 0.239046 11.00000 0.01684 0.01870 = 0.02146 0.00015 0.00690 -0.00119 C28 1 0.119872 0.179197 0.268572 11.00000 0.02258 0.01746 = 0.03092 0.00091 0.00947 -0.00187 AFIX 43 H28 2 0.117683 0.112083 0.246077 11.00000 -1.20000 AFIX 0 C29 1 0.128389 0.173484 0.330167 11.00000 0.02253 0.02077 = 0.03246 0.01004 0.00916 0.00030 AFIX 43 H29 2 0.132696 0.102863 0.349551 11.00000 -1.20000 AFIX 0 C30 1 0.130630 0.270425 0.363456 11.00000 0.02190 0.02803 = 0.01988 0.00850 0.00743 0.00114 AFIX 43 H30 2 0.134259 0.265497 0.405436 11.00000 -1.20000 AFIX 0 C31 1 0.127648 0.375393 0.336399 11.00000 0.01959 0.02280 = 0.01754 0.00268 0.00744 0.00115 C32 1 0.096868 0.289582 0.171179 11.00000 0.02561 0.02063 = 0.02042 -0.00362 0.00661 -0.00283 AFIX 13 H32 2 0.125617 0.353254 0.159152 11.00000 -1.20000 AFIX 0 C33 1 0.116583 0.184226 0.140011 11.00000 0.02789 0.02532 = 0.02857 -0.01015 0.00955 -0.00501 AFIX 137 H33A 2 0.084307 0.122819 0.146794 11.00000 -1.50000 H33B 2 0.167867 0.163982 0.156219 11.00000 -1.50000 H33C 2 0.110216 0.198317 0.097034 11.00000 -1.50000 AFIX 0 C34 1 0.014666 0.315087 0.149324 11.00000 0.03092 0.03784 = 0.02384 -0.00740 0.00010 0.00508 AFIX 137 H34A 2 0.003986 0.322808 0.105742 11.00000 -1.50000 H34B 2 0.002299 0.384864 0.167481 11.00000 -1.50000 H34C 2 -0.014674 0.253844 0.160820 11.00000 -1.50000 AFIX 0 C35 1 0.129065 0.479992 0.374220 11.00000 0.03862 0.02590 = 0.01639 0.00022 0.00943 0.00217 AFIX 13 H35 2 0.134245 0.546087 0.348611 11.00000 -1.20000 AFIX 0 C36 1 0.192976 0.481732 0.428304 11.00000 0.04260 0.04679 = 0.01898 -0.00815 0.00643 -0.00026 AFIX 137 H36A 2 0.186658 0.421251 0.455743 11.00000 -1.50000 H36B 2 0.193721 0.553682 0.448901 11.00000 -1.50000 H36C 2 0.239444 0.471375 0.414875 11.00000 -1.50000 AFIX 0 C37 1 0.056053 0.491228 0.395540 11.00000 0.04364 0.04637 = 0.03125 -0.00349 0.01395 0.01707 AFIX 137 H37A 2 0.015040 0.486929 0.361108 11.00000 -1.50000 H37B 2 0.054695 0.563323 0.415632 11.00000 -1.50000 H37C 2 0.051837 0.430601 0.423483 11.00000 -1.50000 AFIX 0 C38 1 0.286978 0.398357 0.305260 11.00000 0.02172 0.02408 = 0.01684 0.00189 0.00831 0.00219 AFIX 43 H38 2 0.279223 0.464828 0.325868 11.00000 -1.20000 AFIX 0 C39 1 0.316576 0.304750 0.337667 11.00000 0.02501 0.03447 = 0.01866 0.00926 0.00752 0.00345 AFIX 43 H39 2 0.328449 0.307881 0.380055 11.00000 -1.20000 AFIX 0 C40 1 0.328838 0.207063 0.308535 11.00000 0.02333 0.02496 = 0.03174 0.01352 0.00947 0.00491 AFIX 43 H40 2 0.348337 0.143018 0.330769 11.00000 -1.20000 AFIX 0 C41 1 0.312344 0.203776 0.246572 11.00000 0.02123 0.01669 = 0.03239 0.00277 0.00969 0.00056 AFIX 43 H41 2 0.321420 0.137699 0.226175 11.00000 -1.20000 AFIX 0 C42 1 0.282624 0.296886 0.214426 11.00000 0.01955 0.01730 = 0.01899 0.00142 0.00641 -0.00123 AFIX 43 H42 2 0.271517 0.293532 0.172031 11.00000 -1.20000 AFIX 0 C43 1 0.268560 0.395943 0.243006 11.00000 0.01599 0.01774 = 0.01624 0.00298 0.00622 -0.00058 C44 1 0.356188 0.526731 0.043995 11.00000 0.01935 0.02443 = 0.01286 0.00220 0.00758 0.00204 C45 1 0.344955 0.627765 0.011365 11.00000 0.02389 0.02660 = 0.01874 0.00446 0.00963 0.00456 C46 1 0.308207 0.623167 -0.048299 11.00000 0.03034 0.03433 = 0.01834 0.00995 0.00729 0.00626 AFIX 43 H46 2 0.300812 0.690056 -0.071112 11.00000 -1.20000 AFIX 0 C47 1 0.282408 0.523098 -0.074754 11.00000 0.02715 0.04493 = 0.01393 0.00495 0.00483 0.00260 AFIX 43 H47 2 0.258403 0.521433 -0.115589 11.00000 -1.20000 AFIX 0 C48 1 0.291579 0.425419 -0.041713 11.00000 0.02618 0.03487 = 0.01574 -0.00189 0.00751 -0.00296 AFIX 43 H48 2 0.272793 0.357363 -0.060107 11.00000 -1.20000 AFIX 0 C49 1 0.327845 0.424623 0.018089 11.00000 0.02219 0.02582 = 0.01438 0.00008 0.00858 0.00034 C50 1 0.367620 0.740962 0.039522 11.00000 0.03385 0.02269 = 0.02545 0.00602 0.01188 0.00413 AFIX 13 H50 2 0.402369 0.727325 0.078357 11.00000 -1.20000 AFIX 0 C51 1 0.407281 0.814858 0.001060 11.00000 0.04391 0.02678 = 0.03674 0.00623 0.01888 -0.00036 AFIX 137 H51A 2 0.448469 0.773316 -0.009279 11.00000 -1.50000 H51B 2 0.425886 0.882214 0.023490 11.00000 -1.50000 H51C 2 0.372802 0.836210 -0.035580 11.00000 -1.50000 AFIX 0 C52 1 0.300926 0.802370 0.053038 11.00000 0.04296 0.02610 = 0.04027 0.00668 0.02003 0.00697 AFIX 137 H52A 2 0.265019 0.814404 0.015817 11.00000 -1.50000 H52B 2 0.316398 0.874673 0.071508 11.00000 -1.50000 H52C 2 0.278472 0.757522 0.080480 11.00000 -1.50000 AFIX 0 C53 1 0.330938 0.315142 0.052187 11.00000 0.03265 0.02323 = 0.01500 -0.00174 0.00820 -0.00313 AFIX 13 H53 2 0.355738 0.329160 0.094600 11.00000 -1.20000 AFIX 0 C54 1 0.374094 0.224142 0.026542 11.00000 0.04800 0.02628 = 0.02603 -0.00371 0.01322 0.00261 AFIX 137 H54A 2 0.348201 0.204728 -0.013899 11.00000 -1.50000 H54B 2 0.378258 0.157653 0.052039 11.00000 -1.50000 H54C 2 0.423354 0.251997 0.025127 11.00000 -1.50000 AFIX 0 C55 1 0.515608 0.601385 0.077217 11.00000 0.02419 0.03604 = 0.02088 0.00514 0.01022 -0.00233 AFIX 137 H55A 2 0.491608 0.589110 0.035441 11.00000 -1.50000 H55B 2 0.567983 0.583102 0.082575 11.00000 -1.50000 H55C 2 0.510094 0.679876 0.087743 11.00000 -1.50000 AFIX 0 C56 1 0.506620 0.407217 0.109660 11.00000 0.02528 0.02984 = 0.02250 -0.00108 0.00786 0.00720 AFIX 137 H56A 2 0.481076 0.354841 0.131436 11.00000 -1.50000 H56B 2 0.559710 0.402706 0.125315 11.00000 -1.50000 H56C 2 0.496145 0.387903 0.067119 11.00000 -1.50000 AFIX 0 C57 1 0.252519 0.273013 0.051507 11.00000 0.03966 0.03246 = 0.02050 -0.00421 0.00951 -0.01312 AFIX 137 H57A 2 0.224721 0.330995 0.067645 11.00000 -1.50000 H57B 2 0.254775 0.205474 0.076063 11.00000 -1.50000 H57C 2 0.228087 0.255722 0.010379 11.00000 -1.50000 AFIX 0 HKLF 4 REM Sharma44 in P21/c #14 REM wR2 = 0.1215, GooF = S = 1.037, Restrained GooF = 1.037 for all data REM R1 = 0.0419 for 9389 Fo > 4sig(Fo) and 0.0459 for all 10414 data REM 564 parameters refined using 0 restraints END WGHT 0.0753 1.1021 REM Highest difference peak 0.669, deepest hole -0.454, 1-sigma level 0.049 Q1 1 0.3223 0.5319 0.1490 11.00000 0.05 0.67 Q2 1 0.2147 0.5367 0.1319 11.00000 0.05 0.33 Q3 1 0.2191 0.9136 0.1093 11.00000 0.05 0.33 Q4 1 0.1932 0.4904 0.2027 11.00000 0.05 0.31 Q5 1 0.0547 0.2973 0.1614 11.00000 0.05 0.31 Q6 1 0.2175 0.5353 0.2230 11.00000 0.05 0.30 Q7 1 0.3864 0.9135 0.0201 11.00000 0.05 0.30 Q8 1 0.4985 0.4755 0.3196 11.00000 0.05 0.29 Q9 1 0.2468 0.6181 0.1168 11.00000 0.05 0.29 Q10 1 0.4223 0.5721 0.2320 11.00000 0.05 0.29 Q11 1 0.2560 0.4639 0.1134 11.00000 0.05 0.28 Q12 1 0.2930 0.2929 0.0514 11.00000 0.05 0.27 Q13 1 0.4398 0.5256 0.1094 11.00000 0.05 0.27 Q14 1 0.0485 0.6525 0.0474 11.00000 0.05 0.27 ; _shelx_res_checksum 95857 _olex2_date_sample_data_collection 2019-08-01 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 5.777 _oxdiff_exptl_absorpt_empirical_full_min 0.249 ####################################################################### # # 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_compound8 _database_code_depnum_ccdc_archive 'CCDC 1949892' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-06-26 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' beate.neumann@uni-bielefeld.de _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '2(Cl4 Ga1), C54 H72 N3 P' _chemical_formula_sum 'C54 H72 Cl8 Ga2 N3 P' _chemical_formula_weight 1217.15 _chemical_melting_point ? _chemical_oxdiff_formula 'C54 H72 Cl8 Ga2 N3 P' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.13916(17) _cell_length_b 18.90210(13) _cell_length_c 26.08922(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11904.01(15) _cell_formula_units_Z 8 _cell_measurement_reflns_used 108311 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.4020 _cell_measurement_theta_min 2.9260 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 4.946 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 5040 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -2 5 0.0837 -2 2 -5 0.0837 5 1 -1 0.0761 -4 5 5 0.1456 -5 -1 1 0.1134 -2 -5 -2 0.1345 1 -2 -5 0.1730 -5 -1 -5 0.1157 0 1 -5 0.1078 -1 -1 5 0.1138 -4 -4 5 0.0887 _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.189 _exptl_crystal_size_min 0.167 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.9718 -1.9863 5.0132 0.3499 0.0788 0.0327 -1.9718 1.9863 -5.0132 -0.3499 -0.0788 -0.0327 5.0102 0.9919 -0.9800 0.0503 -0.2042 0.2604 -4.0198 5.0026 4.9629 0.0751 -0.2772 -0.4854 -5.0102 -0.9919 0.9800 -0.0503 0.2042 -0.2604 -1.9996 -4.9917 -1.9918 -0.0623 0.4283 0.0913 1.0231 -2.0070 -4.9864 -0.2033 0.1360 0.2408 -4.9790 -1.0048 -5.0171 -0.3676 0.2225 -0.1040 0.0277 0.9871 -5.0008 -0.2828 -0.0585 0.1015 -1.0284 -0.9863 4.9962 0.2585 0.0852 -0.1541 -4.0355 -3.9774 4.9923 0.2408 0.3866 -0.2254 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_unetI/netI 0.0161 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 220917 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.871 _diffrn_reflns_theta_min 3.388 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -59.00 33.00 1.00 4.50 -- -38.50 38.00 30.00 92 2 \w -92.00 -2.00 1.00 4.50 -- -38.50 125.00 30.00 90 3 \w -116.00 -5.00 1.00 4.50 -- -38.50 -19.00-150.00 111 4 \w -59.00 33.00 1.00 4.50 -- -38.50 38.00 -60.00 92 5 \w -64.00 30.00 1.00 4.50 -- -38.50 57.00-150.00 94 6 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00 -90.00 101 7 \w 18.00 111.00 1.00 4.50 -- 42.89 57.00 60.00 93 8 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00 90.00 101 9 \w 22.00 114.00 1.00 4.50 -- 42.89 38.00 -60.00 92 10 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00-150.00 101 11 \w 22.00 114.00 1.00 4.50 -- 42.89 38.00 60.00 92 12 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00 -30.00 101 13 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00 30.00 101 14 \w 13.00 114.00 1.00 4.50 -- 42.89 77.00 150.00 101 15 \w 23.00 97.00 1.00 4.50 -- 42.89-125.00 -60.00 74 16 \w 82.00 178.00 1.00 17.50 -- 111.00 74.00 8.40 96 17 \w 83.00 178.00 1.00 17.50 -- 111.00 70.00 125.09 95 18 \w 84.00 178.00 1.00 17.50 -- 111.00 64.00 110.32 94 19 \w 83.00 178.00 1.00 17.50 -- 111.00 69.00 -2.26 95 20 \w 41.00 118.00 1.00 17.50 -- 111.00-125.00 0.00 77 21 \w 84.00 178.00 1.00 17.50 -- 111.00 65.00 146.61 94 22 \w 81.00 178.00 1.00 17.50 -- 111.00 77.00 30.00 97 23 \w 85.00 178.00 1.00 17.50 -- 111.00 61.00 0.00 93 24 \w 81.00 178.00 1.00 17.50 -- 111.00 77.00-120.00 97 25 \w 41.00 118.00 1.00 17.50 -- 111.00-125.00 60.00 77 26 \w 31.00 110.00 1.00 17.50 -- 111.00 -94.00 60.00 79 27 \w 81.00 178.00 1.00 17.50 -- 111.00 77.00 -30.00 97 28 \w 83.00 178.00 1.00 17.50 -- 111.00 67.00 91.75 95 29 \w 87.00 178.00 1.00 17.50 -- 111.00 51.00 78.52 91 30 \w 40.00 141.00 1.00 17.50 -- 111.00 -77.00 90.00 101 31 \w 81.00 178.00 1.00 17.50 -- 111.00 77.00 60.00 97 32 \w 85.00 178.00 1.00 17.50 -- 111.00 61.00-150.00 93 33 \w 81.00 178.00 1.00 17.50 -- 111.00 77.00 150.00 97 34 \w 84.00 116.00 1.00 17.50 -- 111.00 65.00 -59.94 32 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0240441000 _diffrn_orient_matrix_UB_12 -0.0183275000 _diffrn_orient_matrix_UB_13 0.0530738000 _diffrn_orient_matrix_UB_21 -0.0267311000 _diffrn_orient_matrix_UB_22 -0.0738777000 _diffrn_orient_matrix_UB_23 -0.0030308000 _diffrn_orient_matrix_UB_31 0.0527079000 _diffrn_orient_matrix_UB_32 -0.0291312000 _diffrn_orient_matrix_UB_33 -0.0257460000 _diffrn_oxdiff_digest_frames ; 019273a6e4b4457d42a2e5b88a3944337b032597384 ; _diffrn_oxdiff_digest_hkl ; 010d96ab57956881693c726fcba756e7001dd8 ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11792 _reflns_number_total 12495 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _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 2.495 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.078 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 669 _refine_ls_number_reflns 12495 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0476 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+22.7445P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1232 _refine_ls_wR_factor_ref 0.1251 _refine_special_details 'Disorder of Ga1, Cl2 to Cl4 over three sites. The occupation factors were added up to one (76:13:11). Disorder of Ga2, Cl6 to Cl8 over two sites (92:8). Bond lengths and anisotropic displacement parameters were restrained to give reasonable values.' _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Ga1B-Cl1 \\sim Ga1A-Cl1 \\sim Ga1C-Cl1 \\sim Ga1B-Cl4B \\sim Ga1A-Cl4A \\sim Ga1C-Cl4C \\sim Ga1C- Cl2C \\sim Ga1A-Cl2A \\sim Ga1B-Cl2B \\sim Ga1C-Cl3C \\sim Ga1A-Cl3A \\sim Ga1B-Cl3B with sigma of 0.02 Ga2B-Cl8B \\sim Ga2A-Cl8A \\sim Ga2A-Cl5 \\sim Ga2B-Cl5 \\sim Ga2B-Cl6B \\sim Ga2A-Cl6A \\sim Ga2B- Cl7B \\sim Ga2A-Cl7A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(Ga1C) = Uanis(Ga1A) = Uanis(Ga1B) Uanis(Cl2C) = Uanis(Cl2A) = Uanis(Cl2B) Uanis(Cl3C) = Uanis(Cl3A) = Uanis(Cl3B) Uanis(Cl4A) = Uanis(Cl4C) = Uanis(Cl4B) Uanis(Cl6B) = Uanis(Cl6A) Uanis(Cl7A) = Uanis(Cl7B) Uanis(Cl8B) = Uanis(Cl8A) Uanis(Ga2A) = Uanis(Ga2B) 4. Others 1*[Sof(Ga1A)+Sof(Cl2A)+Sof(Cl3A)+Sof(Cl4A)]+1*[Sof(Ga1B)+Sof(Cl2B)+Sof(Cl3B)+ Sof(Cl4B)]+1*[Sof(Ga1C)+Sof(Cl2C)+Sof(Cl3C)+Sof(Cl4C)]=1 with esd of 0 Sof(Ga1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(Cl4A)=FVAR(1) Sof(Ga1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(Cl4B)=FVAR(2) Sof(Ga1C)=Sof(Cl2C)=Sof(Cl3C)=Sof(Cl4C)=FVAR(3) Sof(Ga2B)=Sof(Cl6B)=Sof(Cl7B)=Sof(Cl8B)=1-FVAR(4) Sof(Ga2A)=Sof(Cl6A)=Sof(Cl7A)=Sof(Cl8A)=FVAR(4) 5.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52) 5.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 5.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B, H53C), C54(H54A,H54B,H54C) ; _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 Ga1A Ga 0.79209(4) 0.49362(5) 0.64289(4) 0.0262(2) Uani 0.7645(19) 1 d D . P A 1 Ga1B Ga 0.7965(3) 0.4787(4) 0.6425(3) 0.0262(2) Uani 0.1270(18) 1 d D . P A 2 Ga1C Ga 0.79701(13) 0.5298(2) 0.64638(13) 0.0262(2) Uani 0.1085(9) 1 d D . P A 3 Cl1 Cl 0.87531(3) 0.52350(4) 0.61683(3) 0.04013(16) Uani 1 1 d D . . . . Cl2A Cl 0.76324(5) 0.56567(8) 0.70068(5) 0.0646(4) Uani 0.7645(19) 1 d D . P A 1 Cl2B Cl 0.7858(3) 0.5236(6) 0.7173(3) 0.0646(4) Uani 0.1270(18) 1 d D . P A 2 Cl2C Cl 0.7749(3) 0.6280(5) 0.6726(3) 0.0646(4) Uani 0.1085(9) 1 d D . P A 3 Cl3A Cl 0.79513(5) 0.38640(9) 0.67499(7) 0.0601(5) Uani 0.7645(19) 1 d D . P A 1 Cl3B Cl 0.7990(4) 0.3685(5) 0.6544(5) 0.0601(5) Uani 0.1270(18) 1 d D . P A 2 Cl3C Cl 0.8016(3) 0.4382(5) 0.6983(4) 0.0601(5) Uani 0.1085(9) 1 d D . P A 3 Cl4A Cl 0.73392(8) 0.49536(19) 0.57999(11) 0.0422(5) Uani 0.7645(19) 1 d D . P A 1 Cl4B Cl 0.7444(7) 0.4913(13) 0.5771(8) 0.0422(5) Uani 0.1270(18) 1 d D . P A 2 Cl4C Cl 0.7283(4) 0.4934(5) 0.6019(3) 0.0422(5) Uani 0.1085(9) 1 d D . P A 3 Ga2A Ga 0.41432(3) 0.34879(4) 0.63097(2) 0.02445(12) Uani 0.917(2) 1 d D . P B 1 Ga2B Ga 0.4041(3) 0.3535(5) 0.6241(3) 0.02445(12) Uani 0.083(2) 1 d D . P B 2 Cl5 Cl 0.45729(4) 0.43818(4) 0.59770(3) 0.0484(2) Uani 1 1 d D . . . . Cl6A Cl 0.36493(4) 0.29680(9) 0.57281(4) 0.0638(4) Uani 0.917(2) 1 d D . P B 1 Cl6B Cl 0.3490(5) 0.3444(10) 0.5619(4) 0.0638(4) Uani 0.083(2) 1 d D . P B 2 Cl7A Cl 0.47690(5) 0.27525(6) 0.65866(4) 0.0515(3) Uani 0.917(2) 1 d D . P B 1 Cl7B Cl 0.4527(5) 0.2589(6) 0.6409(5) 0.0515(3) Uani 0.083(2) 1 d D . P B 2 Cl8A Cl 0.36174(4) 0.38621(6) 0.69273(3) 0.0309(2) Uani 0.917(2) 1 d D . P B 1 Cl8B Cl 0.3507(6) 0.3935(8) 0.6830(5) 0.0309(2) Uani 0.083(2) 1 d D . P B 2 P1 P 0.39173(2) 0.78401(3) 0.60953(2) 0.01625(11) Uani 1 1 d . . . . . N1 N 0.46904(7) 0.87812(9) 0.68849(7) 0.0158(3) Uani 1 1 d . . . . . N2 N 0.53300(7) 0.79975(9) 0.67296(7) 0.0144(3) Uani 1 1 d . . . . . N3 N 0.32295(7) 0.68771(10) 0.56485(8) 0.0197(4) Uani 1 1 d . . . . . C1 C 0.47770(8) 0.81174(11) 0.67102(8) 0.0139(4) Uani 1 1 d . . . . . C2 C 0.51926(9) 0.90725(12) 0.70253(9) 0.0219(4) Uani 1 1 d . . . . . H2 H 0.524767 0.952048 0.716368 0.026 Uiso 1 1 calc R . . . . C3 C 0.55907(9) 0.85859(12) 0.69246(9) 0.0198(4) Uani 1 1 d . . . . . H3 H 0.596932 0.863994 0.697742 0.024 Uiso 1 1 calc R . . . . C4 C 0.41709(9) 0.91733(11) 0.68799(8) 0.0171(4) Uani 1 1 d . . . . . C5 C 0.38199(10) 0.91293(11) 0.73070(9) 0.0194(4) Uani 1 1 d . . . . . C6 C 0.33132(10) 0.94798(13) 0.72710(9) 0.0236(5) Uani 1 1 d . . . . . H6 H 0.306277 0.945194 0.754116 0.028 Uiso 1 1 calc R . . . . C7 C 0.31770(10) 0.98692(13) 0.68385(10) 0.0256(5) Uani 1 1 d . . . . . H7 H 0.283199 1.008628 0.681693 0.031 Uiso 1 1 calc R . . . . C8 C 0.35506(10) 0.99378(13) 0.64380(9) 0.0240(5) Uani 1 1 d . . . . . H8 H 0.345871 1.021782 0.615748 0.029 Uiso 1 1 calc R . . . . C9 C 0.40623(9) 0.95939(12) 0.64483(9) 0.0191(4) Uani 1 1 d . . . . . C10 C 0.39787(10) 0.87628(12) 0.78029(9) 0.0232(5) Uani 1 1 d . . . . . H10 H 0.432725 0.850895 0.774563 0.028 Uiso 1 1 calc R . . . . C11 C 0.40760(15) 0.93143(16) 0.82238(11) 0.0401(7) Uani 1 1 d . . . . . H11A H 0.419659 0.908144 0.853117 0.060 Uiso 1 1 calc GR . . . . H11B H 0.373733 0.956423 0.829003 0.060 Uiso 1 1 calc GR . . . . H11C H 0.435515 0.964264 0.811378 0.060 Uiso 1 1 calc GR . . . . C12 C 0.35438(12) 0.82266(15) 0.79784(11) 0.0334(6) Uani 1 1 d . . . . . H12A H 0.347609 0.789234 0.770853 0.050 Uiso 1 1 calc GR . . . . H12B H 0.320585 0.846931 0.806039 0.050 Uiso 1 1 calc GR . . . . H12C H 0.367637 0.798161 0.827646 0.050 Uiso 1 1 calc GR . . . . C13 C 0.44882(10) 0.97311(12) 0.60268(9) 0.0229(5) Uani 1 1 d . . . . . H13 H 0.478760 0.938569 0.606825 0.028 Uiso 1 1 calc R . . . . C14 C 0.47381(11) 1.04694(14) 0.60948(11) 0.0315(5) Uani 1 1 d . . . . . H14A H 0.489065 1.051147 0.643322 0.047 Uiso 1 1 calc GR . . . . H14B H 0.445476 1.081979 0.604785 0.047 Uiso 1 1 calc GR . . . . H14C H 0.502579 1.053991 0.584585 0.047 Uiso 1 1 calc GR . . . . C15 C 0.42575(12) 0.96498(14) 0.54837(10) 0.0308(5) Uani 1 1 d . . . . . H15A H 0.411628 0.917890 0.543961 0.046 Uiso 1 1 calc GR . . . . H15B H 0.454731 0.973420 0.523924 0.046 Uiso 1 1 calc GR . . . . H15C H 0.396424 0.998513 0.543151 0.046 Uiso 1 1 calc GR . . . . C16 C 0.56151(8) 0.74215(11) 0.64670(8) 0.0157(4) Uani 1 1 d . . . . . C17 C 0.58436(9) 0.68660(11) 0.67505(9) 0.0177(4) Uani 1 1 d . . . . . C18 C 0.61074(9) 0.63309(12) 0.64746(9) 0.0213(4) Uani 1 1 d . . . . . H18 H 0.626321 0.595138 0.664979 0.026 Uiso 1 1 calc R . . . . C19 C 0.61417(9) 0.63537(12) 0.59452(9) 0.0223(5) Uani 1 1 d . . . . . H19 H 0.630587 0.598181 0.576803 0.027 Uiso 1 1 calc R . . . . C20 C 0.59323(9) 0.69287(13) 0.56778(9) 0.0222(5) Uani 1 1 d . . . . . H20 H 0.596676 0.694385 0.532292 0.027 Uiso 1 1 calc R . . . . C21 C 0.56709(9) 0.74843(12) 0.59326(9) 0.0183(4) Uani 1 1 d . . . . . C22 C 0.58493(10) 0.68501(13) 0.73315(9) 0.0229(5) Uani 1 1 d . . . . . H22 H 0.557719 0.719331 0.745742 0.027 Uiso 1 1 calc R . . . . C23 C 0.64236(11) 0.70705(15) 0.75248(11) 0.0337(6) Uani 1 1 d . . . . . H23A H 0.669517 0.673770 0.740598 0.051 Uiso 1 1 calc GR . . . . H23B H 0.642356 0.707865 0.789269 0.051 Uiso 1 1 calc GR . . . . H23C H 0.651164 0.753315 0.739672 0.051 Uiso 1 1 calc GR . . . . C24 C 0.56988(12) 0.61211(14) 0.75435(11) 0.0323(6) Uani 1 1 d . . . . . H24A H 0.536439 0.595730 0.738360 0.049 Uiso 1 1 calc GR . . . . H24B H 0.564372 0.615331 0.790715 0.049 Uiso 1 1 calc GR . . . . H24C H 0.599389 0.579480 0.747284 0.049 Uiso 1 1 calc GR . . . . C25 C 0.55128(10) 0.81440(13) 0.56337(9) 0.0235(5) Uani 1 1 d . . . . . H25 H 0.530928 0.845943 0.586479 0.028 Uiso 1 1 calc R . . . . C26 C 0.60441(13) 0.85266(16) 0.54636(13) 0.0395(7) Uani 1 1 d . . . . . H26A H 0.628615 0.858319 0.575268 0.059 Uiso 1 1 calc GR . . . . H26B H 0.595059 0.898318 0.532761 0.059 Uiso 1 1 calc GR . . . . H26C H 0.622723 0.825236 0.520437 0.059 Uiso 1 1 calc GR . . . . C27 C 0.51485(11) 0.79975(15) 0.51715(10) 0.0324(6) Uani 1 1 d . . . . . H27A H 0.534725 0.770888 0.493099 0.049 Uiso 1 1 calc GR . . . . H27B H 0.504838 0.843675 0.501160 0.049 Uiso 1 1 calc GR . . . . H27C H 0.481944 0.775440 0.527954 0.049 Uiso 1 1 calc GR . . . . C28 C 0.43525(8) 0.75877(11) 0.65695(8) 0.0145(4) Uani 1 1 d . . . . . C29 C 0.43544(9) 0.69267(11) 0.68726(9) 0.0171(4) Uani 1 1 d . . . . . C30 C 0.43960(10) 0.69642(12) 0.74082(9) 0.0217(4) Uani 1 1 d . . . . . H30 H 0.449717 0.738726 0.756422 0.026 Uiso 1 1 calc R . . . . C31 C 0.42867(11) 0.63724(14) 0.77061(10) 0.0290(5) Uani 1 1 d . . . . . H31 H 0.429643 0.640451 0.806173 0.035 Uiso 1 1 calc R . . . . C32 C 0.41634(11) 0.57346(14) 0.74729(11) 0.0313(6) Uani 1 1 d . . . . . H32 H 0.407234 0.534398 0.767257 0.038 Uiso 1 1 calc R . . . . C33 C 0.41744(10) 0.56735(13) 0.69439(11) 0.0288(5) Uani 1 1 d . . . . . H33 H 0.412238 0.523446 0.679033 0.035 Uiso 1 1 calc R . . . . C34 C 0.42636(9) 0.62715(12) 0.66422(10) 0.0219(4) Uani 1 1 d . . . . . H34 H 0.426261 0.623322 0.628684 0.026 Uiso 1 1 calc R . . . . C35 C 0.33506(9) 0.71697(11) 0.60830(9) 0.0183(4) Uani 1 1 d . . . . . C36 C 0.28802(9) 0.70914(13) 0.64744(10) 0.0233(5) Uani 1 1 d . . . . . C37 C 0.24353(10) 0.67114(14) 0.61495(11) 0.0278(5) Uani 1 1 d . . . . . H37A H 0.225353 0.634857 0.635165 0.033 Uiso 1 1 calc R . . . . H37B H 0.215747 0.704712 0.603544 0.033 Uiso 1 1 calc R . . . . C38 C 0.27253(10) 0.63789(13) 0.56885(11) 0.0265(5) Uani 1 1 d . . . . . C39 C 0.26961(10) 0.78515(14) 0.66134(11) 0.0287(5) Uani 1 1 d . . . . . H39A H 0.298312 0.807958 0.680731 0.043 Uiso 1 1 calc GR . . . . H39B H 0.236325 0.783238 0.681428 0.043 Uiso 1 1 calc GR . . . . H39C H 0.262784 0.811428 0.630494 0.043 Uiso 1 1 calc GR . . . . C40 C 0.30075(10) 0.66850(15) 0.69655(10) 0.0299(5) Uani 1 1 d . . . . . H40A H 0.310578 0.620663 0.688187 0.045 Uiso 1 1 calc GR . . . . H40B H 0.268649 0.668489 0.718269 0.045 Uiso 1 1 calc GR . . . . H40C H 0.331040 0.690779 0.714102 0.045 Uiso 1 1 calc GR . . . . C41 C 0.23856(11) 0.63847(16) 0.51990(12) 0.0363(6) Uani 1 1 d . . . . . H41A H 0.222515 0.684480 0.515141 0.054 Uiso 1 1 calc GR . . . . H41B H 0.209614 0.603800 0.522303 0.054 Uiso 1 1 calc GR . . . . H41C H 0.262051 0.627508 0.491293 0.054 Uiso 1 1 calc GR . . . . C42 C 0.29333(10) 0.56289(13) 0.57997(12) 0.0309(6) Uani 1 1 d . . . . . H42A H 0.311987 0.544647 0.550284 0.046 Uiso 1 1 calc GR . . . . H42B H 0.262462 0.532963 0.588221 0.046 Uiso 1 1 calc GR . . . . H42C H 0.318589 0.564045 0.608385 0.046 Uiso 1 1 calc GR . . . . C43 C 0.35020(9) 0.70837(12) 0.51671(9) 0.0215(4) Uani 1 1 d . . . . . C44 C 0.39429(10) 0.66891(13) 0.49652(9) 0.0230(5) Uani 1 1 d . . . . . C45 C 0.42010(11) 0.69479(15) 0.45237(10) 0.0303(5) Uani 1 1 d . . . . . H45 H 0.449073 0.669414 0.437744 0.036 Uiso 1 1 calc R . . . . C46 C 0.40315(12) 0.75769(16) 0.43010(10) 0.0349(6) Uani 1 1 d . . . . . H46 H 0.421721 0.775160 0.401549 0.042 Uiso 1 1 calc R . . . . C47 C 0.35867(12) 0.79459(15) 0.45018(11) 0.0345(6) Uani 1 1 d . . . . . H47 H 0.347537 0.836430 0.434508 0.041 Uiso 1 1 calc R . . . . C48 C 0.33015(10) 0.77082(13) 0.49320(10) 0.0263(5) Uani 1 1 d . . . . . C49 C 0.41550(9) 0.60045(12) 0.51966(9) 0.0225(5) Uani 1 1 d . . . . . H49 H 0.394676 0.591335 0.551218 0.027 Uiso 1 1 calc R . . . . C50 C 0.47697(10) 0.60633(14) 0.53354(10) 0.0258(5) Uani 1 1 d . . . . . H50A H 0.498322 0.613271 0.502904 0.039 Uiso 1 1 calc GR . . . . H50B H 0.488752 0.563648 0.550230 0.039 Uiso 1 1 calc GR . . . . H50C H 0.482362 0.645773 0.556178 0.039 Uiso 1 1 calc GR . . . . C51 C 0.40542(11) 0.53863(14) 0.48284(11) 0.0309(5) Uani 1 1 d . . . . . H51A H 0.366921 0.537080 0.473666 0.046 Uiso 1 1 calc GR . . . . H51B H 0.415609 0.495083 0.499267 0.046 Uiso 1 1 calc GR . . . . H51C H 0.427396 0.544976 0.452523 0.046 Uiso 1 1 calc GR . . . . C52 C 0.27842(11) 0.81050(14) 0.51046(12) 0.0333(6) Uani 1 1 d . . . . . H52 H 0.261297 0.783968 0.538578 0.040 Uiso 1 1 calc R . . . . C53 C 0.29107(13) 0.88553(15) 0.52950(14) 0.0408(7) Uani 1 1 d . . . . . H53A H 0.315268 0.883097 0.558644 0.061 Uiso 1 1 calc GR . . . . H53B H 0.257158 0.908504 0.539126 0.061 Uiso 1 1 calc GR . . . . H53C H 0.308691 0.911972 0.502645 0.061 Uiso 1 1 calc GR . . . . C54 C 0.23686(13) 0.81432(17) 0.46591(14) 0.0473(8) Uani 1 1 d . . . . . H54A H 0.251838 0.843250 0.439027 0.071 Uiso 1 1 calc GR . . . . H54B H 0.202738 0.834557 0.477849 0.071 Uiso 1 1 calc GR . . . . H54C H 0.230036 0.767554 0.453027 0.071 Uiso 1 1 calc GR . . . . 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 Ga1A 0.0188(3) 0.0335(6) 0.02618(19) -0.0034(4) -0.00197(16) 0.0026(3) Ga1B 0.0188(3) 0.0335(6) 0.02618(19) -0.0034(4) -0.00197(16) 0.0026(3) Ga1C 0.0188(3) 0.0335(6) 0.02618(19) -0.0034(4) -0.00197(16) 0.0026(3) Cl1 0.0298(3) 0.0429(4) 0.0477(4) 0.0014(3) 0.0067(3) -0.0029(3) Cl2A 0.0442(6) 0.0892(10) 0.0603(7) -0.0484(7) 0.0181(5) -0.0152(6) Cl2B 0.0442(6) 0.0892(10) 0.0603(7) -0.0484(7) 0.0181(5) -0.0152(6) Cl2C 0.0442(6) 0.0892(10) 0.0603(7) -0.0484(7) 0.0181(5) -0.0152(6) Cl3A 0.0216(4) 0.0668(9) 0.0919(12) 0.0485(9) 0.0058(7) 0.0043(5) Cl3B 0.0216(4) 0.0668(9) 0.0919(12) 0.0485(9) 0.0058(7) 0.0043(5) Cl3C 0.0216(4) 0.0668(9) 0.0919(12) 0.0485(9) 0.0058(7) 0.0043(5) Cl4A 0.0405(11) 0.0476(6) 0.0386(6) -0.0015(5) -0.0195(10) 0.0027(8) Cl4B 0.0405(11) 0.0476(6) 0.0386(6) -0.0015(5) -0.0195(10) 0.0027(8) Cl4C 0.0405(11) 0.0476(6) 0.0386(6) -0.0015(5) -0.0195(10) 0.0027(8) Ga2A 0.0240(3) 0.0310(2) 0.0184(2) 0.00327(16) -0.00140(17) -0.0104(2) Ga2B 0.0240(3) 0.0310(2) 0.0184(2) 0.00327(16) -0.00140(17) -0.0104(2) Cl5 0.0527(4) 0.0358(4) 0.0568(5) 0.0094(3) 0.0250(4) -0.0102(3) Cl6A 0.0437(5) 0.1173(11) 0.0305(4) -0.0266(5) 0.0081(4) -0.0439(6) Cl6B 0.0437(5) 0.1173(11) 0.0305(4) -0.0266(5) 0.0081(4) -0.0439(6) Cl7A 0.0434(5) 0.0647(6) 0.0464(5) 0.0277(4) 0.0099(4) 0.0122(4) Cl7B 0.0434(5) 0.0647(6) 0.0464(5) 0.0277(4) 0.0099(4) 0.0122(4) Cl8A 0.0356(5) 0.0327(4) 0.0244(4) 0.0003(3) 0.0044(3) -0.0101(3) Cl8B 0.0356(5) 0.0327(4) 0.0244(4) 0.0003(3) 0.0044(3) -0.0101(3) P1 0.0121(2) 0.0163(2) 0.0204(3) 0.00245(19) -0.00296(19) -0.00164(19) N1 0.0131(8) 0.0148(8) 0.0195(8) -0.0016(7) -0.0024(7) 0.0016(7) N2 0.0110(8) 0.0149(8) 0.0174(8) 0.0001(7) -0.0006(6) 0.0009(6) N3 0.0116(8) 0.0177(8) 0.0297(10) -0.0001(7) -0.0034(7) -0.0013(7) C1 0.0124(9) 0.0148(9) 0.0146(9) 0.0014(7) -0.0009(7) 0.0016(7) C2 0.0184(11) 0.0190(10) 0.0284(12) -0.0047(9) -0.0053(9) -0.0020(8) C3 0.0144(10) 0.0207(10) 0.0244(11) -0.0013(8) -0.0046(8) -0.0028(8) C4 0.0152(10) 0.0156(9) 0.0204(10) -0.0020(8) -0.0018(8) 0.0038(8) C5 0.0219(11) 0.0174(10) 0.0190(10) -0.0001(8) 0.0006(8) 0.0032(8) C6 0.0209(11) 0.0253(11) 0.0246(11) 0.0009(9) 0.0041(9) 0.0066(9) C7 0.0197(11) 0.0269(12) 0.0300(12) 0.0030(10) 0.0009(9) 0.0097(9) C8 0.0229(12) 0.0245(11) 0.0247(12) 0.0041(9) -0.0018(9) 0.0074(9) C9 0.0194(10) 0.0173(10) 0.0207(10) 0.0002(8) -0.0002(8) 0.0033(8) C10 0.0267(12) 0.0228(11) 0.0202(11) 0.0013(9) 0.0001(9) 0.0083(9) C11 0.065(2) 0.0321(14) 0.0235(13) -0.0039(11) -0.0090(13) 0.0111(13) C12 0.0315(14) 0.0362(14) 0.0326(13) 0.0122(11) 0.0080(11) 0.0092(11) C13 0.0225(11) 0.0216(11) 0.0248(11) 0.0025(9) 0.0038(9) 0.0046(9) C14 0.0276(13) 0.0295(13) 0.0374(14) -0.0009(11) 0.0053(11) -0.0043(10) C15 0.0368(14) 0.0319(13) 0.0236(12) 0.0051(10) 0.0043(10) -0.0027(11) C16 0.0097(9) 0.0162(9) 0.0213(10) -0.0011(8) 0.0009(7) 0.0012(7) C17 0.0125(9) 0.0177(10) 0.0229(11) 0.0011(8) 0.0001(8) 0.0000(8) C18 0.0166(10) 0.0170(10) 0.0302(12) 0.0022(9) 0.0021(9) 0.0026(8) C19 0.0168(10) 0.0202(10) 0.0298(12) -0.0036(9) 0.0050(9) 0.0016(8) C20 0.0182(10) 0.0253(11) 0.0232(11) -0.0005(9) 0.0051(9) 0.0023(9) C21 0.0136(9) 0.0202(10) 0.0212(10) 0.0020(8) 0.0019(8) 0.0002(8) C22 0.0238(11) 0.0232(11) 0.0216(11) 0.0022(9) -0.0014(9) 0.0081(9) C23 0.0305(14) 0.0374(14) 0.0333(14) -0.0051(11) -0.0119(11) 0.0083(11) C24 0.0376(14) 0.0291(13) 0.0304(13) 0.0107(10) 0.0056(11) 0.0098(11) C25 0.0249(12) 0.0232(11) 0.0223(11) 0.0042(9) 0.0052(9) 0.0062(9) C26 0.0390(16) 0.0318(14) 0.0477(17) 0.0140(12) 0.0003(13) -0.0081(12) C27 0.0291(13) 0.0392(14) 0.0290(13) 0.0107(11) -0.0006(10) 0.0030(11) C28 0.0116(9) 0.0149(9) 0.0169(9) -0.0010(7) 0.0022(7) 0.0012(7) C29 0.0122(9) 0.0156(10) 0.0236(11) 0.0035(8) 0.0018(8) 0.0022(7) C30 0.0215(11) 0.0209(10) 0.0226(11) 0.0044(9) 0.0016(9) 0.0046(9) C31 0.0293(13) 0.0304(13) 0.0273(12) 0.0111(10) 0.0062(10) 0.0086(10) C32 0.0261(13) 0.0238(12) 0.0440(15) 0.0166(11) 0.0084(11) 0.0057(10) C33 0.0236(12) 0.0156(11) 0.0471(15) 0.0045(10) 0.0034(11) 0.0005(9) C34 0.0184(10) 0.0178(10) 0.0296(12) -0.0007(9) 0.0018(9) -0.0006(8) C35 0.0115(9) 0.0156(10) 0.0277(11) 0.0025(8) -0.0020(8) 0.0018(8) C36 0.0121(10) 0.0230(11) 0.0348(13) -0.0008(9) 0.0038(9) -0.0015(8) C37 0.0126(10) 0.0255(12) 0.0454(15) -0.0035(11) 0.0010(10) -0.0026(9) C38 0.0149(10) 0.0229(11) 0.0418(14) -0.0032(10) -0.0028(10) -0.0064(9) C39 0.0168(11) 0.0286(12) 0.0408(14) -0.0068(11) 0.0039(10) 0.0016(9) C40 0.0189(11) 0.0361(14) 0.0346(13) 0.0072(11) 0.0082(10) -0.0013(10) C41 0.0231(13) 0.0357(14) 0.0500(17) -0.0093(12) -0.0120(12) -0.0070(11) C42 0.0212(12) 0.0203(11) 0.0513(16) -0.0030(11) 0.0041(11) -0.0060(9) C43 0.0192(11) 0.0224(11) 0.0230(11) 0.0009(9) -0.0072(9) -0.0028(8) C44 0.0218(11) 0.0254(11) 0.0219(11) -0.0004(9) -0.0062(9) -0.0014(9) C45 0.0309(13) 0.0368(14) 0.0232(12) -0.0008(10) -0.0032(10) -0.0005(11) C46 0.0393(15) 0.0426(15) 0.0229(12) 0.0071(11) -0.0068(11) -0.0044(12) C47 0.0409(15) 0.0307(13) 0.0318(14) 0.0083(11) -0.0161(12) -0.0031(11) C48 0.0242(12) 0.0228(11) 0.0320(13) 0.0017(9) -0.0129(10) -0.0010(9) C49 0.0193(11) 0.0230(11) 0.0252(11) -0.0018(9) -0.0016(9) 0.0015(9) C50 0.0188(11) 0.0291(12) 0.0295(12) 0.0029(10) -0.0013(9) -0.0005(9) C51 0.0292(13) 0.0295(13) 0.0340(13) -0.0089(11) -0.0033(11) 0.0018(10) C52 0.0251(12) 0.0269(13) 0.0478(16) 0.0029(11) -0.0152(12) 0.0045(10) C53 0.0340(15) 0.0265(13) 0.062(2) 0.0000(13) -0.0171(14) 0.0062(11) C54 0.0360(16) 0.0409(16) 0.065(2) 0.0074(15) -0.0288(15) 0.0019(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1A Cl1 2.1948(13) . ? Ga1A Cl2A 2.1476(13) . ? Ga1A Cl3A 2.1940(15) . ? Ga1A Cl4A 2.160(2) . ? Ga1B Cl1 2.188(8) . ? Ga1B Cl2B 2.143(9) . ? Ga1B Cl3B 2.107(10) . ? Ga1B Cl4B 2.131(13) . ? Ga1C Cl1 2.045(3) . ? Ga1C Cl2C 2.049(8) . ? Ga1C Cl3C 2.201(7) . ? Ga1C Cl4C 2.138(8) . ? Ga2A Cl5 2.1643(9) . ? Ga2A Cl6A 2.1655(10) . ? Ga2A Cl7A 2.1762(10) . ? Ga2A Cl8A 2.1698(10) . ? Ga2B Cl5 2.164(8) . ? Ga2B Cl6B 2.105(10) . ? Ga2B Cl7B 2.184(10) . ? Ga2B Cl8B 2.143(12) . ? P1 C28 1.692(2) . ? P1 C35 1.865(2) . ? N1 C1 1.351(3) . ? N1 C2 1.381(3) . ? N1 C4 1.457(3) . ? N2 C1 1.355(3) . ? N2 C3 1.375(3) . ? N2 C16 1.459(3) . ? N3 C35 1.295(3) . ? N3 C38 1.542(3) . ? N3 C43 1.471(3) . ? C1 C28 1.479(3) . ? C2 H2 0.9300 . ? C2 C3 1.356(3) . ? C3 H3 0.9300 . ? C4 C5 1.402(3) . ? C4 C9 1.403(3) . ? C5 C6 1.394(3) . ? C5 C10 1.517(3) . ? C6 H6 0.9300 . ? C6 C7 1.387(3) . ? C7 H7 0.9300 . ? C7 C8 1.386(4) . ? C8 H8 0.9300 . ? C8 C9 1.396(3) . ? C9 C13 1.527(3) . ? C10 H10 0.9800 . ? C10 C11 1.532(4) . ? C10 C12 1.529(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.531(3) . ? C13 C15 1.530(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.398(3) . ? C16 C21 1.406(3) . ? C17 C18 1.395(3) . ? C17 C22 1.516(3) . ? C18 H18 0.9300 . ? C18 C19 1.384(3) . ? C19 H19 0.9300 . ? C19 C20 1.387(3) . ? C20 H20 0.9300 . ? C20 C21 1.394(3) . ? C21 C25 1.520(3) . ? C22 H22 0.9800 . ? C22 C23 1.533(3) . ? C22 C24 1.529(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.538(4) . ? C25 C27 1.518(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.479(3) . ? C29 C30 1.403(3) . ? C29 C34 1.394(3) . ? C30 H30 0.9300 . ? C30 C31 1.387(3) . ? C31 H31 0.9300 . ? C31 C32 1.383(4) . ? C32 H32 0.9300 . ? C32 C33 1.385(4) . ? C33 H33 0.9300 . ? C33 C34 1.394(3) . ? C34 H34 0.9300 . ? C35 C36 1.534(3) . ? C36 C37 1.545(3) . ? C36 C39 1.547(3) . ? C36 C40 1.525(4) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.527(4) . ? C38 C41 1.518(4) . ? C38 C42 1.532(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.402(3) . ? C43 C48 1.415(3) . ? C44 C45 1.398(4) . ? C44 C49 1.517(3) . ? C45 H45 0.9300 . ? C45 C46 1.385(4) . ? C46 H46 0.9300 . ? C46 C47 1.383(4) . ? C47 H47 0.9300 . ? C47 C48 1.391(4) . ? C48 C52 1.525(4) . ? C49 H49 0.9800 . ? C49 C50 1.531(3) . ? C49 C51 1.532(3) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.533(4) . ? C52 C54 1.537(4) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? 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 Cl2A Ga1A Cl1 110.55(6) . . ? Cl2A Ga1A Cl3A 109.19(8) . . ? Cl2A Ga1A Cl4A 108.23(8) . . ? Cl3A Ga1A Cl1 108.98(5) . . ? Cl4A Ga1A Cl1 110.84(9) . . ? Cl4A Ga1A Cl3A 109.01(12) . . ? Cl2B Ga1B Cl1 103.3(4) . . ? Cl3B Ga1B Cl1 113.8(4) . . ? Cl3B Ga1B Cl2B 105.1(6) . . ? Cl3B Ga1B Cl4B 104.3(8) . . ? Cl4B Ga1B Cl1 103.0(7) . . ? Cl4B Ga1B Cl2B 127.8(7) . . ? Cl1 Ga1C Cl2C 114.8(3) . . ? Cl1 Ga1C Cl3C 98.0(2) . . ? Cl1 Ga1C Cl4C 119.6(3) . . ? Cl2C Ga1C Cl3C 121.3(5) . . ? Cl2C Ga1C Cl4C 105.7(4) . . ? Cl4C Ga1C Cl3C 96.9(4) . . ? Cl5 Ga2A Cl6A 109.70(5) . . ? Cl5 Ga2A Cl7A 107.41(4) . . ? Cl5 Ga2A Cl8A 108.89(5) . . ? Cl6A Ga2A Cl7A 108.95(6) . . ? Cl6A Ga2A Cl8A 110.26(4) . . ? Cl8A Ga2A Cl7A 111.58(4) . . ? Cl5 Ga2B Cl7B 110.5(5) . . ? Cl6B Ga2B Cl5 101.0(5) . . ? Cl6B Ga2B Cl7B 115.3(8) . . ? Cl6B Ga2B Cl8B 101.6(6) . . ? Cl8B Ga2B Cl5 108.9(6) . . ? Cl8B Ga2B Cl7B 117.9(6) . . ? C28 P1 C35 106.05(10) . . ? C1 N1 C2 108.91(18) . . ? C1 N1 C4 127.06(18) . . ? C2 N1 C4 123.72(18) . . ? C1 N2 C3 109.23(18) . . ? C1 N2 C16 124.88(18) . . ? C3 N2 C16 124.15(18) . . ? C35 N3 C38 112.3(2) . . ? C35 N3 C43 122.23(19) . . ? C43 N3 C38 124.95(19) . . ? N1 C1 N2 107.16(18) . . ? N1 C1 C28 127.25(18) . . ? N2 C1 C28 125.36(18) . . ? N1 C2 H2 126.3 . . ? C3 C2 N1 107.47(19) . . ? C3 C2 H2 126.3 . . ? N2 C3 H3 126.4 . . ? C2 C3 N2 107.22(19) . . ? C2 C3 H3 126.4 . . ? C5 C4 N1 118.88(19) . . ? C5 C4 C9 123.9(2) . . ? C9 C4 N1 117.15(19) . . ? C4 C5 C10 123.5(2) . . ? C6 C5 C4 116.6(2) . . ? C6 C5 C10 119.7(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 C5 121.0(2) . . ? C7 C6 H6 119.5 . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.6(2) . . ? C8 C7 H7 119.7 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.2(2) . . ? C9 C8 H8 119.4 . . ? C4 C9 C13 123.2(2) . . ? C8 C9 C4 116.4(2) . . ? C8 C9 C13 120.2(2) . . ? C5 C10 H10 108.1 . . ? C5 C10 C11 109.8(2) . . ? C5 C10 C12 112.6(2) . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C12 C10 C11 110.0(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.7 . . ? C9 C13 C14 109.7(2) . . ? C9 C13 C15 113.9(2) . . ? C14 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C15 C13 C14 110.0(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 119.89(19) . . ? C17 C16 C21 123.4(2) . . ? C21 C16 N2 116.61(18) . . ? C16 C17 C22 123.2(2) . . ? C18 C17 C16 116.9(2) . . ? C18 C17 C22 119.8(2) . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.3(2) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.3(2) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 119.5 . . ? C19 C20 C21 121.0(2) . . ? C21 C20 H20 119.5 . . ? C16 C21 C25 123.7(2) . . ? C20 C21 C16 116.9(2) . . ? C20 C21 C25 119.2(2) . . ? C17 C22 H22 108.4 . . ? C17 C22 C23 109.4(2) . . ? C17 C22 C24 112.2(2) . . ? C23 C22 H22 108.4 . . ? C24 C22 H22 108.4 . . ? C24 C22 C23 109.9(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 108.0 . . ? C21 C25 C26 108.9(2) . . ? C26 C25 H25 108.0 . . ? C27 C25 C21 113.8(2) . . ? C27 C25 H25 108.0 . . ? C27 C25 C26 109.9(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 114.89(15) . . ? C29 C28 P1 129.15(16) . . ? C29 C28 C1 115.93(18) . . ? C30 C29 C28 119.4(2) . . ? C34 C29 C28 121.3(2) . . ? C34 C29 C30 119.1(2) . . ? C29 C30 H30 119.9 . . ? C31 C30 C29 120.3(2) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 120.1 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C31 C32 H32 119.8 . . ? C31 C32 C33 120.5(2) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 120.1 . . ? C32 C33 C34 119.9(2) . . ? C34 C33 H33 120.1 . . ? C29 C34 C33 120.1(2) . . ? C29 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N3 C35 P1 118.09(17) . . ? N3 C35 C36 111.99(19) . . ? C36 C35 P1 126.65(17) . . ? C35 C36 C37 101.2(2) . . ? C35 C36 C39 106.19(19) . . ? C37 C36 C39 111.1(2) . . ? C40 C36 C35 117.29(19) . . ? C40 C36 C37 111.5(2) . . ? C40 C36 C39 109.2(2) . . ? C36 C37 H37A 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C38 C37 C36 107.74(19) . . ? C38 C37 H37A 110.2 . . ? C38 C37 H37B 110.2 . . ? C37 C38 N3 99.43(18) . . ? C37 C38 C42 112.5(2) . . ? C41 C38 N3 111.4(2) . . ? C41 C38 C37 114.3(2) . . ? C41 C38 C42 110.1(2) . . ? C42 C38 N3 108.62(18) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 121.3(2) . . ? C44 C43 C48 122.7(2) . . ? C48 C43 N3 116.0(2) . . ? C43 C44 C49 124.1(2) . . ? C45 C44 C43 117.5(2) . . ? C45 C44 C49 118.4(2) . . ? C44 C45 H45 119.5 . . ? C46 C45 C44 121.0(3) . . ? C46 C45 H45 119.5 . . ? C45 C46 H46 119.9 . . ? C47 C46 C45 120.2(3) . . ? C47 C46 H46 119.9 . . ? C46 C47 H47 119.1 . . ? C46 C47 C48 121.8(2) . . ? C48 C47 H47 119.1 . . ? C43 C48 C52 124.2(2) . . ? C47 C48 C43 116.7(2) . . ? C47 C48 C52 119.0(2) . . ? C44 C49 H49 108.1 . . ? C44 C49 C50 111.0(2) . . ? C44 C49 C51 110.3(2) . . ? C50 C49 H49 108.1 . . ? C50 C49 C51 111.0(2) . . ? C51 C49 H49 108.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52 108.3 . . ? C48 C52 C53 112.8(2) . . ? C48 C52 C54 109.5(3) . . ? C53 C52 H52 108.3 . . ? C53 C52 C54 109.4(2) . . ? C54 C52 H52 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C28 C29 C30 -131.6(2) . . . . ? P1 C28 C29 C34 42.3(3) . . . . ? P1 C35 C36 C37 156.03(17) . . . . ? P1 C35 C36 C39 39.9(3) . . . . ? P1 C35 C36 C40 -82.4(3) . . . . ? N1 C1 C28 P1 59.6(3) . . . . ? N1 C1 C28 C29 -118.4(2) . . . . ? N1 C2 C3 N2 -0.8(3) . . . . ? N1 C4 C5 C6 -176.3(2) . . . . ? N1 C4 C5 C10 7.3(3) . . . . ? N1 C4 C9 C8 176.9(2) . . . . ? N1 C4 C9 C13 -8.2(3) . . . . ? N2 C1 C28 P1 -126.77(19) . . . . ? N2 C1 C28 C29 55.3(3) . . . . ? N2 C16 C17 C18 179.63(19) . . . . ? N2 C16 C17 C22 -4.6(3) . . . . ? N2 C16 C21 C20 -178.66(19) . . . . ? N2 C16 C21 C25 7.2(3) . . . . ? N3 C35 C36 C37 -2.9(2) . . . . ? N3 C35 C36 C39 -119.1(2) . . . . ? N3 C35 C36 C40 118.6(2) . . . . ? N3 C43 C44 C45 -176.0(2) . . . . ? N3 C43 C44 C49 3.9(3) . . . . ? N3 C43 C48 C47 174.4(2) . . . . ? N3 C43 C48 C52 -8.7(3) . . . . ? C1 N1 C2 C3 1.3(3) . . . . ? C1 N1 C4 C5 91.3(3) . . . . ? C1 N1 C4 C9 -90.8(3) . . . . ? C1 N2 C3 C2 -0.1(3) . . . . ? C1 N2 C16 C17 -110.5(2) . . . . ? C1 N2 C16 C21 73.1(3) . . . . ? C1 C28 C29 C30 45.9(3) . . . . ? C1 C28 C29 C34 -140.2(2) . . . . ? C2 N1 C1 N2 -1.3(2) . . . . ? C2 N1 C1 C28 173.3(2) . . . . ? C2 N1 C4 C5 -95.9(3) . . . . ? C2 N1 C4 C9 82.1(3) . . . . ? C3 N2 C1 N1 0.9(2) . . . . ? C3 N2 C1 C28 -173.9(2) . . . . ? C3 N2 C16 C17 86.1(3) . . . . ? C3 N2 C16 C21 -90.2(3) . . . . ? C4 N1 C1 N2 172.36(19) . . . . ? C4 N1 C1 C28 -13.0(3) . . . . ? C4 N1 C2 C3 -172.6(2) . . . . ? C4 C5 C6 C7 -2.0(4) . . . . ? C4 C5 C10 C11 108.5(3) . . . . ? C4 C5 C10 C12 -128.6(2) . . . . ? C4 C9 C13 C14 -102.1(3) . . . . ? C4 C9 C13 C15 134.1(2) . . . . ? C5 C4 C9 C8 -5.3(3) . . . . ? C5 C4 C9 C13 169.7(2) . . . . ? C5 C6 C7 C8 -2.1(4) . . . . ? C6 C5 C10 C11 -67.8(3) . . . . ? C6 C5 C10 C12 55.1(3) . . . . ? C6 C7 C8 C9 2.8(4) . . . . ? C7 C8 C9 C4 0.8(4) . . . . ? C7 C8 C9 C13 -174.4(2) . . . . ? C8 C9 C13 C14 72.7(3) . . . . ? C8 C9 C13 C15 -51.1(3) . . . . ? C9 C4 C5 C6 5.9(3) . . . . ? C9 C4 C5 C10 -170.5(2) . . . . ? C10 C5 C6 C7 174.5(2) . . . . ? C16 N2 C1 N1 -164.60(18) . . . . ? C16 N2 C1 C28 20.7(3) . . . . ? C16 N2 C3 C2 165.5(2) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C16 C17 C22 C23 -100.6(2) . . . . ? C16 C17 C22 C24 137.2(2) . . . . ? C16 C21 C25 C26 106.7(3) . . . . ? C16 C21 C25 C27 -130.4(2) . . . . ? C17 C16 C21 C20 5.1(3) . . . . ? C17 C16 C21 C25 -169.0(2) . . . . ? C17 C18 C19 C20 2.7(4) . . . . ? C18 C17 C22 C23 75.1(3) . . . . ? C18 C17 C22 C24 -47.2(3) . . . . ? C18 C19 C20 C21 -1.7(4) . . . . ? C19 C20 C21 C16 -2.0(3) . . . . ? C19 C20 C21 C25 172.4(2) . . . . ? C20 C21 C25 C26 -67.3(3) . . . . ? C20 C21 C25 C27 55.7(3) . . . . ? C21 C16 C17 C18 -4.3(3) . . . . ? C21 C16 C17 C22 171.5(2) . . . . ? C22 C17 C18 C19 -175.7(2) . . . . ? C28 P1 C35 N3 -128.68(17) . . . . ? C28 P1 C35 C36 73.5(2) . . . . ? C28 C29 C30 C31 166.9(2) . . . . ? C28 C29 C34 C33 -169.2(2) . . . . ? C29 C30 C31 C32 3.2(4) . . . . ? C30 C29 C34 C33 4.8(3) . . . . ? C30 C31 C32 C33 3.2(4) . . . . ? C31 C32 C33 C34 -5.5(4) . . . . ? C32 C33 C34 C29 1.5(4) . . . . ? C34 C29 C30 C31 -7.1(3) . . . . ? C35 P1 C28 C1 -169.13(15) . . . . ? C35 P1 C28 C29 8.4(2) . . . . ? C35 N3 C38 C37 25.5(2) . . . . ? C35 N3 C38 C41 146.4(2) . . . . ? C35 N3 C38 C42 -92.2(2) . . . . ? C35 N3 C43 C44 98.6(3) . . . . ? C35 N3 C43 C48 -79.9(3) . . . . ? C35 C36 C37 C38 19.1(2) . . . . ? C36 C37 C38 N3 -25.9(2) . . . . ? C36 C37 C38 C41 -144.7(2) . . . . ? C36 C37 C38 C42 88.8(2) . . . . ? C38 N3 C35 P1 -175.57(15) . . . . ? C38 N3 C35 C36 -14.6(3) . . . . ? C38 N3 C43 C44 -90.2(3) . . . . ? C38 N3 C43 C48 91.4(3) . . . . ? C39 C36 C37 C38 131.5(2) . . . . ? C40 C36 C37 C38 -106.4(2) . . . . ? C43 N3 C35 P1 -3.3(3) . . . . ? C43 N3 C35 C36 157.64(19) . . . . ? C43 N3 C38 C37 -146.5(2) . . . . ? C43 N3 C38 C41 -25.6(3) . . . . ? C43 N3 C38 C42 95.8(3) . . . . ? C43 C44 C45 C46 1.0(4) . . . . ? C43 C44 C49 C50 -121.7(2) . . . . ? C43 C44 C49 C51 114.8(3) . . . . ? C43 C48 C52 C53 116.9(3) . . . . ? C43 C48 C52 C54 -121.1(3) . . . . ? C44 C43 C48 C47 -4.0(3) . . . . ? C44 C43 C48 C52 172.8(2) . . . . ? C44 C45 C46 C47 -2.6(4) . . . . ? C45 C44 C49 C50 58.1(3) . . . . ? C45 C44 C49 C51 -65.3(3) . . . . ? C45 C46 C47 C48 0.8(4) . . . . ? C46 C47 C48 C43 2.4(4) . . . . ? C46 C47 C48 C52 -174.6(2) . . . . ? C47 C48 C52 C53 -66.3(3) . . . . ? C47 C48 C52 C54 55.7(3) . . . . ? C48 C43 C44 C45 2.4(3) . . . . ? C48 C43 C44 C49 -177.8(2) . . . . ? C49 C44 C45 C46 -178.8(2) . . . . ? _shelx_res_file ; TITL sharma38_a.res in Pbca sharma38.res created by SHELXL-2018/3 at 11:47:18 on 26-Jun-2019 REM Old TITL sharma38 in Pbca REM SHELXT solution in Pbca: R1 0.182, Rweak 0.008, Alpha 0.026 REM 0.998 for 989 systematic absences, Orientation as input REM Formula found by SHELXT: C54 N3 Cl9 Ga1C CELL 1.54184 24.139159 18.902102 26.089223 90 90 90 ZERR 8 0.000174 0.00013 0.000183 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl Ga N P UNIT 432 576 64 16 24 8 SADI Ga1B Cl1 Ga1A Cl1 Ga1C Cl1 Ga1B Cl4B Ga1A Cl4A Ga1C Cl4C Ga1C Cl2C = GA1A CL2A GA1B CL2B GA1C CL3C GA1A CL3A GA1B CL3B SADI Ga2B Cl8B Ga2A Cl8A Ga2A Cl5 Ga2B Cl5 Ga2B Cl6B Ga2A Cl6A Ga2B Cl7B = GA2A CL7A EADP Ga1C Ga1A Ga1B EADP Cl2C Cl2A Cl2B EADP Cl3C Cl3A Cl3B EADP Cl4A Cl4C Cl4B EADP Cl6B Cl6A EADP Cl7A Cl7B EADP Cl8B Cl8A EADP Ga2A Ga2B SUMP 1 0 1 2 1 3 1 4 L.S. 11 PLAN 11 BOND $H list more -1 conf fmap 2 53 acta REM REM REM WGHT 0.061600 22.744501 FVAR 1.12829 0.76449 0.12700 0.10845 0.91715 PART 1 GA1A 4 0.792087 0.493620 0.642893 21.00000 0.01879 0.03349 = 0.02618 -0.00342 -0.00197 0.00261 PART 0 PART 2 GA1B 4 0.796488 0.478664 0.642492 31.00000 0.01879 0.03349 = 0.02618 -0.00342 -0.00197 0.00261 PART 0 PART 3 GA1C 4 0.797009 0.529781 0.646381 41.00000 0.01879 0.03349 = 0.02618 -0.00342 -0.00197 0.00261 PART 0 CL1 3 0.875311 0.523501 0.616832 11.00000 0.02980 0.04290 = 0.04769 0.00140 0.00671 -0.00292 PART 1 CL2A 3 0.763240 0.565673 0.700675 21.00000 0.04423 0.08915 = 0.06032 -0.04838 0.01815 -0.01518 PART 0 PART 2 CL2B 3 0.785756 0.523592 0.717251 31.00000 0.04423 0.08915 = 0.06032 -0.04838 0.01815 -0.01518 PART 0 PART 3 CL2C 3 0.774932 0.627991 0.672597 41.00000 0.04423 0.08915 = 0.06032 -0.04838 0.01815 -0.01518 PART 0 PART 1 CL3A 3 0.795129 0.386402 0.674988 21.00000 0.02157 0.06683 = 0.09187 0.04849 0.00582 0.00433 PART 0 PART 2 CL3B 3 0.798981 0.368474 0.654427 31.00000 0.02157 0.06683 = 0.09187 0.04849 0.00582 0.00433 PART 0 PART 3 CL3C 3 0.801637 0.438227 0.698333 41.00000 0.02157 0.06683 = 0.09187 0.04849 0.00582 0.00433 PART 0 PART 1 CL4A 3 0.733919 0.495355 0.579988 21.00000 0.04046 0.04762 = 0.03858 -0.00149 -0.01955 0.00266 PART 0 PART 2 CL4B 3 0.744445 0.491343 0.577135 31.00000 0.04046 0.04762 = 0.03858 -0.00149 -0.01955 0.00266 PART 0 PART 3 CL4C 3 0.728271 0.493412 0.601939 41.00000 0.04046 0.04762 = 0.03858 -0.00149 -0.01955 0.00266 PART 0 PART 1 GA2A 4 0.414320 0.348791 0.630971 51.00000 0.02404 0.03097 = 0.01835 0.00327 -0.00140 -0.01043 PART 0 PART 2 GA2B 4 0.404061 0.353528 0.624088 -51.00000 0.02404 0.03097 = 0.01835 0.00327 -0.00140 -0.01043 PART 0 CL5 3 0.457290 0.438177 0.597700 11.00000 0.05267 0.03579 = 0.05675 0.00942 0.02503 -0.01024 PART 1 CL6A 3 0.364931 0.296799 0.572815 51.00000 0.04375 0.11731 = 0.03046 -0.02662 0.00811 -0.04392 PART 0 PART 2 CL6B 3 0.348968 0.344412 0.561910 -51.00000 0.04375 0.11731 = 0.03046 -0.02662 0.00811 -0.04392 PART 0 PART 1 CL7A 3 0.476897 0.275246 0.658657 51.00000 0.04336 0.06470 = 0.04644 0.02774 0.00988 0.01216 PART 0 PART 2 CL7B 3 0.452680 0.258893 0.640865 -51.00000 0.04336 0.06470 = 0.04644 0.02774 0.00988 0.01216 PART 0 PART 1 CL8A 3 0.361739 0.386213 0.692734 51.00000 0.03559 0.03272 = 0.02438 0.00029 0.00444 -0.01007 PART 0 PART 2 CL8B 3 0.350691 0.393507 0.682994 -51.00000 0.03559 0.03272 = 0.02438 0.00029 0.00444 -0.01007 PART 0 P1 6 0.391725 0.784006 0.609527 11.00000 0.01213 0.01628 = 0.02036 0.00245 -0.00296 -0.00164 N1 5 0.469042 0.878122 0.688486 11.00000 0.01314 0.01483 = 0.01952 -0.00157 -0.00236 0.00161 N2 5 0.533004 0.799753 0.672962 11.00000 0.01105 0.01492 = 0.01735 0.00012 -0.00058 0.00088 N3 5 0.322948 0.687713 0.564848 11.00000 0.01160 0.01765 = 0.02972 -0.00007 -0.00337 -0.00133 C1 1 0.477700 0.811743 0.671015 11.00000 0.01240 0.01476 = 0.01464 0.00136 -0.00090 0.00157 C2 1 0.519258 0.907253 0.702532 11.00000 0.01838 0.01902 = 0.02837 -0.00474 -0.00528 -0.00200 AFIX 43 H2 2 0.524767 0.952048 0.716368 11.00000 -1.20000 AFIX 0 C3 1 0.559066 0.858590 0.692456 11.00000 0.01442 0.02065 = 0.02435 -0.00126 -0.00456 -0.00278 AFIX 43 H3 2 0.596932 0.863994 0.697742 11.00000 -1.20000 AFIX 0 C4 1 0.417095 0.917333 0.687990 11.00000 0.01523 0.01562 = 0.02039 -0.00197 -0.00184 0.00377 C5 1 0.381994 0.912933 0.730698 11.00000 0.02190 0.01735 = 0.01901 -0.00014 0.00059 0.00318 C6 1 0.331321 0.947977 0.727102 11.00000 0.02088 0.02525 = 0.02462 0.00085 0.00405 0.00662 AFIX 43 H6 2 0.306277 0.945194 0.754116 11.00000 -1.20000 AFIX 0 C7 1 0.317696 0.986924 0.683849 11.00000 0.01974 0.02692 = 0.03000 0.00303 0.00094 0.00967 AFIX 43 H7 2 0.283199 1.008628 0.681693 11.00000 -1.20000 AFIX 0 C8 1 0.355059 0.993780 0.643799 11.00000 0.02294 0.02452 = 0.02466 0.00410 -0.00176 0.00738 AFIX 43 H8 2 0.345871 1.021782 0.615748 11.00000 -1.20000 AFIX 0 C9 1 0.406233 0.959395 0.644828 11.00000 0.01936 0.01732 = 0.02067 0.00016 -0.00019 0.00334 C10 1 0.397869 0.876276 0.780286 11.00000 0.02670 0.02276 = 0.02019 0.00131 0.00015 0.00831 AFIX 13 H10 2 0.432725 0.850895 0.774563 11.00000 -1.20000 AFIX 0 C11 1 0.407603 0.931426 0.822376 11.00000 0.06465 0.03215 = 0.02346 -0.00394 -0.00898 0.01113 AFIX 137 H11A 2 0.419659 0.908144 0.853117 11.00000 -1.50000 H11B 2 0.373733 0.956423 0.829003 11.00000 -1.50000 H11C 2 0.435515 0.964264 0.811378 11.00000 -1.50000 AFIX 0 C12 1 0.354377 0.822661 0.797840 11.00000 0.03147 0.03621 = 0.03259 0.01218 0.00797 0.00916 AFIX 137 H12A 2 0.347609 0.789234 0.770853 11.00000 -1.50000 H12B 2 0.320585 0.846931 0.806039 11.00000 -1.50000 H12C 2 0.367637 0.798161 0.827646 11.00000 -1.50000 AFIX 0 C13 1 0.448816 0.973107 0.602675 11.00000 0.02247 0.02156 = 0.02476 0.00251 0.00380 0.00458 AFIX 13 H13 2 0.478760 0.938569 0.606825 11.00000 -1.20000 AFIX 0 C14 1 0.473814 1.046938 0.609476 11.00000 0.02764 0.02947 = 0.03738 -0.00088 0.00529 -0.00432 AFIX 137 H14A 2 0.489065 1.051147 0.643322 11.00000 -1.50000 H14B 2 0.445476 1.081979 0.604785 11.00000 -1.50000 H14C 2 0.502579 1.053991 0.584585 11.00000 -1.50000 AFIX 0 C15 1 0.425752 0.964975 0.548370 11.00000 0.03675 0.03194 = 0.02363 0.00509 0.00431 -0.00275 AFIX 137 H15A 2 0.411628 0.917890 0.543961 11.00000 -1.50000 H15B 2 0.454731 0.973420 0.523924 11.00000 -1.50000 H15C 2 0.396424 0.998513 0.543151 11.00000 -1.50000 AFIX 0 C16 1 0.561511 0.742148 0.646701 11.00000 0.00970 0.01623 = 0.02131 -0.00110 0.00088 0.00116 C17 1 0.584362 0.686597 0.675050 11.00000 0.01248 0.01770 = 0.02290 0.00111 0.00008 0.00001 C18 1 0.610738 0.633086 0.647460 11.00000 0.01664 0.01697 = 0.03020 0.00225 0.00205 0.00256 AFIX 43 H18 2 0.626321 0.595138 0.664979 11.00000 -1.20000 AFIX 0 C19 1 0.614167 0.635371 0.594518 11.00000 0.01682 0.02023 = 0.02984 -0.00360 0.00497 0.00161 AFIX 43 H19 2 0.630587 0.598181 0.576803 11.00000 -1.20000 AFIX 0 C20 1 0.593227 0.692871 0.567779 11.00000 0.01819 0.02530 = 0.02324 -0.00047 0.00507 0.00225 AFIX 43 H20 2 0.596676 0.694385 0.532292 11.00000 -1.20000 AFIX 0 C21 1 0.567092 0.748430 0.593265 11.00000 0.01358 0.02022 = 0.02121 0.00195 0.00194 0.00021 C22 1 0.584935 0.685013 0.733146 11.00000 0.02383 0.02322 = 0.02161 0.00215 -0.00136 0.00809 AFIX 13 H22 2 0.557719 0.719331 0.745742 11.00000 -1.20000 AFIX 0 C23 1 0.642357 0.707049 0.752477 11.00000 0.03047 0.03740 = 0.03333 -0.00506 -0.01191 0.00829 AFIX 137 H23A 2 0.669517 0.673770 0.740598 11.00000 -1.50000 H23B 2 0.642356 0.707865 0.789269 11.00000 -1.50000 H23C 2 0.651164 0.753315 0.739672 11.00000 -1.50000 AFIX 0 C24 1 0.569884 0.612108 0.754348 11.00000 0.03760 0.02907 = 0.03036 0.01068 0.00563 0.00984 AFIX 137 H24A 2 0.536439 0.595730 0.738360 11.00000 -1.50000 H24B 2 0.564372 0.615331 0.790715 11.00000 -1.50000 H24C 2 0.599389 0.579480 0.747284 11.00000 -1.50000 AFIX 0 C25 1 0.551277 0.814398 0.563367 11.00000 0.02494 0.02321 = 0.02225 0.00423 0.00522 0.00621 AFIX 13 H25 2 0.530928 0.845943 0.586479 11.00000 -1.20000 AFIX 0 C26 1 0.604410 0.852662 0.546361 11.00000 0.03896 0.03181 = 0.04766 0.01402 0.00032 -0.00805 AFIX 137 H26A 2 0.628615 0.858319 0.575268 11.00000 -1.50000 H26B 2 0.595059 0.898318 0.532761 11.00000 -1.50000 H26C 2 0.622723 0.825236 0.520437 11.00000 -1.50000 AFIX 0 C27 1 0.514849 0.799755 0.517148 11.00000 0.02910 0.03920 = 0.02898 0.01070 -0.00062 0.00304 AFIX 137 H27A 2 0.534725 0.770888 0.493099 11.00000 -1.50000 H27B 2 0.504838 0.843675 0.501160 11.00000 -1.50000 H27C 2 0.481944 0.775440 0.527954 11.00000 -1.50000 AFIX 0 C28 1 0.435250 0.758767 0.656949 11.00000 0.01161 0.01495 = 0.01693 -0.00099 0.00217 0.00119 C29 1 0.435437 0.692674 0.687263 11.00000 0.01217 0.01565 = 0.02360 0.00351 0.00176 0.00221 C30 1 0.439597 0.696416 0.740822 11.00000 0.02152 0.02090 = 0.02263 0.00443 0.00162 0.00464 AFIX 43 H30 2 0.449717 0.738726 0.756422 11.00000 -1.20000 AFIX 0 C31 1 0.428672 0.637237 0.770613 11.00000 0.02929 0.03037 = 0.02728 0.01105 0.00623 0.00862 AFIX 43 H31 2 0.429643 0.640451 0.806173 11.00000 -1.20000 AFIX 0 C32 1 0.416336 0.573461 0.747287 11.00000 0.02614 0.02383 = 0.04403 0.01660 0.00841 0.00565 AFIX 43 H32 2 0.407234 0.534398 0.767257 11.00000 -1.20000 AFIX 0 C33 1 0.417439 0.567347 0.694390 11.00000 0.02364 0.01556 = 0.04711 0.00448 0.00336 0.00052 AFIX 43 H33 2 0.412238 0.523446 0.679033 11.00000 -1.20000 AFIX 0 C34 1 0.426362 0.627148 0.664223 11.00000 0.01843 0.01776 = 0.02958 -0.00069 0.00184 -0.00060 AFIX 43 H34 2 0.426261 0.623322 0.628684 11.00000 -1.20000 AFIX 0 C35 1 0.335060 0.716971 0.608300 11.00000 0.01151 0.01564 = 0.02767 0.00252 -0.00202 0.00179 C36 1 0.288018 0.709138 0.647444 11.00000 0.01208 0.02304 = 0.03483 -0.00076 0.00381 -0.00154 C37 1 0.243526 0.671138 0.614949 11.00000 0.01258 0.02547 = 0.04537 -0.00352 0.00100 -0.00260 AFIX 23 H37A 2 0.225353 0.634857 0.635165 11.00000 -1.20000 H37B 2 0.215747 0.704712 0.603544 11.00000 -1.20000 AFIX 0 C38 1 0.272533 0.637891 0.568852 11.00000 0.01486 0.02290 = 0.04182 -0.00319 -0.00284 -0.00636 C39 1 0.269614 0.785151 0.661343 11.00000 0.01677 0.02860 = 0.04085 -0.00681 0.00388 0.00155 AFIX 137 H39A 2 0.298312 0.807958 0.680731 11.00000 -1.50000 H39B 2 0.236325 0.783238 0.681428 11.00000 -1.50000 H39C 2 0.262784 0.811428 0.630494 11.00000 -1.50000 AFIX 0 C40 1 0.300751 0.668503 0.696549 11.00000 0.01886 0.03610 = 0.03465 0.00716 0.00815 -0.00133 AFIX 137 H40A 2 0.310578 0.620663 0.688187 11.00000 -1.50000 H40B 2 0.268649 0.668489 0.718269 11.00000 -1.50000 H40C 2 0.331040 0.690779 0.714102 11.00000 -1.50000 AFIX 0 C41 1 0.238556 0.638473 0.519899 11.00000 0.02308 0.03569 = 0.05004 -0.00935 -0.01198 -0.00698 AFIX 137 H41A 2 0.222515 0.684480 0.515141 11.00000 -1.50000 H41B 2 0.209614 0.603800 0.522303 11.00000 -1.50000 H41C 2 0.262051 0.627508 0.491293 11.00000 -1.50000 AFIX 0 C42 1 0.293334 0.562887 0.579973 11.00000 0.02116 0.02034 = 0.05127 -0.00298 0.00413 -0.00603 AFIX 137 H42A 2 0.311987 0.544647 0.550284 11.00000 -1.50000 H42B 2 0.262462 0.532963 0.588221 11.00000 -1.50000 H42C 2 0.318589 0.564045 0.608385 11.00000 -1.50000 AFIX 0 C43 1 0.350195 0.708372 0.516709 11.00000 0.01923 0.02238 = 0.02299 0.00092 -0.00722 -0.00277 C44 1 0.394290 0.668913 0.496523 11.00000 0.02177 0.02540 = 0.02189 -0.00039 -0.00619 -0.00139 C45 1 0.420100 0.694793 0.452372 11.00000 0.03092 0.03684 = 0.02322 -0.00076 -0.00321 -0.00045 AFIX 43 H45 2 0.449073 0.669414 0.437744 11.00000 -1.20000 AFIX 0 C46 1 0.403147 0.757685 0.430098 11.00000 0.03935 0.04258 = 0.02290 0.00714 -0.00680 -0.00440 AFIX 43 H46 2 0.421721 0.775160 0.401549 11.00000 -1.20000 AFIX 0 C47 1 0.358671 0.794592 0.450185 11.00000 0.04095 0.03067 = 0.03175 0.00828 -0.01614 -0.00306 AFIX 43 H47 2 0.347537 0.836430 0.434508 11.00000 -1.20000 AFIX 0 C48 1 0.330151 0.770815 0.493197 11.00000 0.02418 0.02277 = 0.03200 0.00173 -0.01288 -0.00099 C49 1 0.415502 0.600449 0.519657 11.00000 0.01928 0.02299 = 0.02517 -0.00175 -0.00157 0.00154 AFIX 13 H49 2 0.394676 0.591335 0.551218 11.00000 -1.20000 AFIX 0 C50 1 0.476967 0.606334 0.533537 11.00000 0.01881 0.02906 = 0.02948 0.00290 -0.00132 -0.00045 AFIX 137 H50A 2 0.498322 0.613271 0.502904 11.00000 -1.50000 H50B 2 0.488752 0.563648 0.550230 11.00000 -1.50000 H50C 2 0.482362 0.645773 0.556178 11.00000 -1.50000 AFIX 0 C51 1 0.405415 0.538625 0.482841 11.00000 0.02917 0.02953 = 0.03405 -0.00894 -0.00334 0.00185 AFIX 137 H51A 2 0.366921 0.537080 0.473666 11.00000 -1.50000 H51B 2 0.415609 0.495083 0.499267 11.00000 -1.50000 H51C 2 0.427396 0.544976 0.452523 11.00000 -1.50000 AFIX 0 C52 1 0.278420 0.810498 0.510461 11.00000 0.02513 0.02691 = 0.04779 0.00285 -0.01521 0.00449 AFIX 13 H52 2 0.261297 0.783968 0.538578 11.00000 -1.20000 AFIX 0 C53 1 0.291066 0.885533 0.529499 11.00000 0.03404 0.02651 = 0.06180 0.00000 -0.01707 0.00621 AFIX 137 H53A 2 0.315268 0.883097 0.558644 11.00000 -1.50000 H53B 2 0.257158 0.908504 0.539126 11.00000 -1.50000 H53C 2 0.308691 0.911972 0.502645 11.00000 -1.50000 AFIX 0 C54 1 0.236856 0.814324 0.465909 11.00000 0.03604 0.04085 = 0.06508 0.00738 -0.02877 0.00193 AFIX 137 H54A 2 0.251838 0.843250 0.439027 11.00000 -1.50000 H54B 2 0.202738 0.834557 0.477849 11.00000 -1.50000 H54C 2 0.230036 0.767554 0.453027 11.00000 -1.50000 AFIX 0 HKLF 4 REM sharma38_a.res in Pbca REM wR2 = 0.1251, GooF = S = 1.030, Restrained GooF = 1.067 for all data REM R1 = 0.0476 for 11792 Fo > 4sig(Fo) and 0.0497 for all 12495 data REM 669 parameters refined using 95 restraints END WGHT 0.0616 22.7395 REM Highest difference peak 2.495, deepest hole -0.866, 1-sigma level 0.078 Q1 1 0.7609 0.6942 0.6611 11.00000 0.05 2.49 Q2 1 0.7882 0.5526 0.6578 11.00000 0.05 1.74 Q3 1 0.7744 0.6018 0.6804 11.00000 0.05 1.28 Q4 1 0.7408 0.3201 0.6020 11.00000 0.05 1.08 Q5 1 0.7884 0.3341 0.6819 11.00000 0.05 0.97 Q6 1 0.7987 0.4962 0.7353 11.00000 0.05 0.92 Q7 1 0.8194 0.5211 0.6373 11.00000 0.05 0.92 Q8 1 0.7445 0.5606 0.6981 11.00000 0.05 0.61 Q9 1 0.7759 0.2670 0.6413 11.00000 0.05 0.54 Q10 1 0.4763 0.3243 0.6685 11.00000 0.05 0.50 Q11 1 0.3809 0.2433 0.5879 11.00000 0.05 0.46 ; _shelx_res_checksum 53162 _olex2_date_sample_data_collection 2019-06-24 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.643 _oxdiff_exptl_absorpt_empirical_full_min 0.444 ####################################################################### # # 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_compound6 _database_code_depnum_ccdc_archive 'CCDC 1949890' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-04-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C54 H72 N3 P, Cl4 Ga' _chemical_formula_sum 'C54 H72 Cl4 Ga N3 P' _chemical_formula_weight 1005.63 _chemical_melting_point ? _chemical_oxdiff_formula 'C54 H92 Cl4 Ga N3 P' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5123(2) _cell_length_b 12.8811(2) _cell_length_c 37.2397(5) _cell_angle_alpha 90 _cell_angle_beta 97.7240(10) _cell_angle_gamma 90 _cell_volume 5472.21(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60415 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 32.7800 _cell_measurement_theta_min 3.0020 _shelx_estimated_absorpt_T_max 0.843 _shelx_estimated_absorpt_T_min 0.744 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 2124 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4 -16 -16 0.1601 -6 4 49 0.1651 5 -2 -1 0.1254 1 5 5 0.1595 0 1 -1 0.0842 4 -9 43 0.1251 -1 0 1 0.1030 4 -15 -30 0.1378 1 0 -1 0.1471 0 1 2 0.1608 5 -14 27 0.1054 -4 -1 -48 0.2102 -1 -1 2 0.1210 _exptl_crystal_size_max 0.411 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.231 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -4.0774 -16.4149 -16.1841 0.1213 0.1267 -0.9845 -6.3382 4.3142 49.0311 0.8194 -0.2901 0.4944 5.0101 -2.0128 -1.0026 -0.0522 0.3239 0.0202 1.0092 5.0136 5.0644 -0.0315 -0.0514 0.2962 0.0014 1.0042 -0.9944 -0.0364 -0.0283 0.0360 3.7160 -8.5193 42.7814 0.8197 0.5639 0.1007 -1.0026 0.0006 0.9996 0.0317 -0.0521 -0.0148 3.6062 -14.7310 -29.6881 -0.2514 0.4640 -0.8494 1.0026 -0.0006 -0.9996 -0.0317 0.0521 0.0148 0.0013 1.0023 2.0155 0.0133 -0.0179 0.0637 4.5846 -14.1188 27.2715 0.6620 0.6980 -0.2732 -4.3572 -0.6396 -48.1927 -0.7170 -0.3904 -0.5775 -1.0039 -1.0036 1.9941 0.0681 -0.0238 -0.0507 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 120621 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.788 _diffrn_reflns_theta_min 2.727 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.940 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -87.00 12.00 1.00 81.50 -- -17.14 -77.00 -90.00 99 2 \w 17.00 91.00 1.00 81.50 -- 17.14-154.00-127.09 74 3 \w -8.00 82.00 1.00 81.50 -- 17.14 57.00-150.00 90 4 \w -4.00 83.00 1.00 81.50 -- 17.14 38.00 120.00 87 5 \w -4.00 88.00 1.00 81.50 -- 17.14 38.00 30.00 92 6 \w -53.00 28.00 1.00 81.50 -- 17.14 -38.00 -60.00 81 7 \w 6.00 75.00 1.00 81.50 -- 17.14-131.00 -95.76 69 8 \w -47.00 47.00 1.00 81.50 -- 17.14 -77.00 60.00 94 9 \w 47.00 74.00 1.00 81.50 -- 17.14-130.00 42.13 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0151221000 _diffrn_orient_matrix_UB_12 -0.0199088000 _diffrn_orient_matrix_UB_13 0.0165089000 _diffrn_orient_matrix_UB_21 0.0553588000 _diffrn_orient_matrix_UB_22 -0.0248448000 _diffrn_orient_matrix_UB_23 0.0034246000 _diffrn_orient_matrix_UB_31 0.0239389000 _diffrn_orient_matrix_UB_32 0.0449363000 _diffrn_orient_matrix_UB_33 0.0092232000 _diffrn_oxdiff_digest_frames ; 017d6918fea4acc13ab1afa85533e8547500476707a ; _diffrn_oxdiff_digest_hkl ; 015b83f5ac0d0b8e089321f4f3e997e0cac464 ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 16638 _reflns_number_total 19071 _reflns_odcompleteness_completeness 99.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _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 0.689 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 584 _refine_ls_number_reflns 19071 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0544 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.9843P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1072 _refine_ls_wR_factor_ref 0.1106 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52) 2.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B, H53C), C54(H54A,H54B,H54C) ; _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 Ga1 Ga 0.05768(2) 0.81961(2) 0.36582(2) 0.02175(5) Uani 1 1 d . . . . . Cl1 Cl 0.14558(5) 0.96763(4) 0.37522(2) 0.04142(13) Uani 1 1 d . . . . . Cl2 Cl 0.05929(5) 0.73241(4) 0.41583(2) 0.03149(10) Uani 1 1 d . . . . . Cl3 Cl -0.12335(4) 0.84917(4) 0.34206(2) 0.03105(10) Uani 1 1 d . . . . . Cl4 Cl 0.14075(5) 0.72449(4) 0.32808(2) 0.03523(11) Uani 1 1 d . . . . . P1 P 0.67177(4) 0.27822(3) 0.39116(2) 0.01609(8) Uani 1 1 d . . . . . N1 N 0.72492(12) 0.51327(11) 0.37233(4) 0.0159(2) Uani 1 1 d . . . . . N2 N 0.85566(11) 0.47333(10) 0.33717(4) 0.0141(2) Uani 1 1 d . . . . . N3 N 0.58825(12) 0.09438(11) 0.40846(4) 0.0164(3) Uani 1 1 d . . . . . C1 C 0.76517(13) 0.43196(12) 0.35352(4) 0.0139(3) Uani 1 1 d . . . . . C2 C 0.79015(15) 0.60186(13) 0.36787(5) 0.0192(3) Uani 1 1 d . . . . . H2 H 0.780050 0.666698 0.377991 0.023 Uiso 1 1 calc R . . . . C3 C 0.87055(15) 0.57693(12) 0.34628(5) 0.0180(3) Uani 1 1 d . . . . . H3 H 0.926233 0.621436 0.338814 0.022 Uiso 1 1 calc R . . . . C4 C 0.62087(15) 0.52472(13) 0.39013(5) 0.0182(3) Uani 1 1 d . . . . . C5 C 0.51465(15) 0.54727(14) 0.36862(5) 0.0216(3) Uani 1 1 d . . . . . C6 C 0.42045(17) 0.57728(16) 0.38648(6) 0.0282(4) Uani 1 1 d . . . . . H6 H 0.348229 0.592001 0.373071 0.034 Uiso 1 1 calc R . . . . C7 C 0.43375(18) 0.58528(16) 0.42391(6) 0.0322(4) Uani 1 1 d . . . . . H7 H 0.370611 0.606079 0.435355 0.039 Uiso 1 1 calc R . . . . C8 C 0.53978(18) 0.56268(16) 0.44440(6) 0.0298(4) Uani 1 1 d . . . . . H8 H 0.546749 0.568031 0.469500 0.036 Uiso 1 1 calc R . . . . C9 C 0.63720(16) 0.53181(14) 0.42809(5) 0.0220(3) Uani 1 1 d . . . . . C10 C 0.50224(17) 0.54600(17) 0.32747(5) 0.0277(4) Uani 1 1 d . . . . . H10 H 0.566340 0.503992 0.320338 0.033 Uiso 1 1 calc R . . . . C11 C 0.5144(2) 0.6563(2) 0.31281(7) 0.0460(6) Uani 1 1 d . . . . . H11A H 0.453762 0.699631 0.320056 0.069 Uiso 1 1 calc GR . . . . H11B H 0.507399 0.654297 0.286841 0.069 Uiso 1 1 calc GR . . . . H11C H 0.589623 0.684077 0.322376 0.069 Uiso 1 1 calc GR . . . . C12 C 0.38648(19) 0.49763(18) 0.31028(6) 0.0357(5) Uani 1 1 d . . . . . H12A H 0.376441 0.431241 0.321174 0.054 Uiso 1 1 calc GR . . . . H12B H 0.387743 0.488923 0.284737 0.054 Uiso 1 1 calc GR . . . . H12C H 0.322663 0.542385 0.314169 0.054 Uiso 1 1 calc GR . . . . C13 C 0.75441(18) 0.51019(16) 0.45084(5) 0.0273(4) Uani 1 1 d . . . . . H13 H 0.806487 0.479703 0.434925 0.033 Uiso 1 1 calc R . . . . C14 C 0.8115(2) 0.61102(19) 0.46668(7) 0.0404(5) Uani 1 1 d . . . . . H14A H 0.819044 0.658958 0.447390 0.061 Uiso 1 1 calc GR . . . . H14B H 0.887696 0.595852 0.479455 0.061 Uiso 1 1 calc GR . . . . H14C H 0.763454 0.641221 0.483087 0.061 Uiso 1 1 calc GR . . . . C15 C 0.7428(2) 0.43222(19) 0.48129(6) 0.0384(5) Uani 1 1 d . . . . . H15A H 0.694709 0.461495 0.497866 0.058 Uiso 1 1 calc GR . . . . H15B H 0.819064 0.416847 0.493954 0.058 Uiso 1 1 calc GR . . . . H15C H 0.707297 0.369520 0.471092 0.058 Uiso 1 1 calc GR . . . . C16 C 0.93162(13) 0.42943(12) 0.31290(4) 0.0149(3) Uani 1 1 d . . . . . C17 C 0.90662(15) 0.45540(12) 0.27600(4) 0.0171(3) Uani 1 1 d . . . . . C18 C 0.98730(16) 0.42337(13) 0.25342(5) 0.0222(3) Uani 1 1 d . . . . . H18 H 0.972902 0.437722 0.228750 0.027 Uiso 1 1 calc R . . . . C19 C 1.08829(17) 0.37064(14) 0.26713(5) 0.0244(4) Uani 1 1 d . . . . . H19 H 1.141823 0.351447 0.251732 0.029 Uiso 1 1 calc R . . . . C20 C 1.11019(15) 0.34627(13) 0.30358(5) 0.0222(3) Uani 1 1 d . . . . . H20 H 1.177905 0.309870 0.312296 0.027 Uiso 1 1 calc R . . . . C21 C 1.03221(14) 0.37541(12) 0.32764(5) 0.0173(3) Uani 1 1 d . . . . . C22 C 0.79933(16) 0.51751(13) 0.26073(5) 0.0203(3) Uani 1 1 d . . . . . H22 H 0.742582 0.513949 0.278094 0.024 Uiso 1 1 calc R . . . . C23 C 0.83102(18) 0.63199(14) 0.25606(6) 0.0274(4) Uani 1 1 d . . . . . H23A H 0.867671 0.659171 0.278794 0.041 Uiso 1 1 calc GR . . . . H23B H 0.761111 0.670806 0.248091 0.041 Uiso 1 1 calc GR . . . . H23C H 0.884113 0.637601 0.238354 0.041 Uiso 1 1 calc GR . . . . C24 C 0.7399(2) 0.47543(15) 0.22430(5) 0.0293(4) Uani 1 1 d . . . . . H24A H 0.787829 0.490640 0.205754 0.044 Uiso 1 1 calc GR . . . . H24B H 0.664626 0.507654 0.218329 0.044 Uiso 1 1 calc GR . . . . H24C H 0.730182 0.401655 0.226006 0.044 Uiso 1 1 calc GR . . . . C25 C 1.05742(15) 0.35183(14) 0.36787(5) 0.0210(3) Uani 1 1 d . . . . . H25 H 0.982216 0.339459 0.376729 0.025 Uiso 1 1 calc R . . . . C26 C 1.11623(19) 0.44467(16) 0.38887(6) 0.0325(4) Uani 1 1 d . . . . . H26A H 1.191192 0.457448 0.381136 0.049 Uiso 1 1 calc GR . . . . H26B H 1.126648 0.429568 0.414346 0.049 Uiso 1 1 calc GR . . . . H26C H 1.067625 0.505048 0.384260 0.049 Uiso 1 1 calc GR . . . . C27 C 1.13333(17) 0.25490(16) 0.37628(6) 0.0285(4) Uani 1 1 d . . . . . H27A H 1.099355 0.197727 0.362013 0.043 Uiso 1 1 calc GR . . . . H27B H 1.137355 0.238247 0.401541 0.043 Uiso 1 1 calc GR . . . . H27C H 1.210848 0.267976 0.370543 0.043 Uiso 1 1 calc GR . . . . C28 C 0.72762(13) 0.32591(12) 0.35268(4) 0.0142(3) Uani 1 1 d . . . . . C29 C 0.76452(14) 0.25921(12) 0.32377(4) 0.0147(3) Uani 1 1 d . . . . . C30 C 0.72170(15) 0.27665(13) 0.28734(4) 0.0174(3) Uani 1 1 d . . . . . H30 H 0.667982 0.329717 0.281109 0.021 Uiso 1 1 calc R . . . . C31 C 0.75890(16) 0.21509(13) 0.26028(5) 0.0204(3) Uani 1 1 d . . . . . H31 H 0.729178 0.226775 0.236142 0.024 Uiso 1 1 calc R . . . . C32 C 0.84001(16) 0.13653(13) 0.26918(5) 0.0226(3) Uani 1 1 d . . . . . H32 H 0.865806 0.096403 0.251053 0.027 Uiso 1 1 calc R . . . . C33 C 0.88259(15) 0.11803(14) 0.30536(5) 0.0219(3) Uani 1 1 d . . . . . H33 H 0.936724 0.065201 0.311451 0.026 Uiso 1 1 calc R . . . . C34 C 0.84441(14) 0.17833(13) 0.33244(5) 0.0186(3) Uani 1 1 d . . . . . H34 H 0.872309 0.164732 0.356584 0.022 Uiso 1 1 calc R . . . . C35 C 0.60224(13) 0.15630(12) 0.38015(4) 0.0154(3) Uani 1 1 d . . . . . C36 C 0.53013(14) 0.11143(13) 0.34563(4) 0.0163(3) Uani 1 1 d . . . . . C37 C 0.45199(15) 0.03164(14) 0.36231(5) 0.0204(3) Uani 1 1 d . . . . . H37A H 0.379263 0.063774 0.366936 0.024 Uiso 1 1 calc R . . . . H37B H 0.433580 -0.026439 0.345949 0.024 Uiso 1 1 calc R . . . . C38 C 0.52250(15) -0.00508(14) 0.39775(5) 0.0202(3) Uani 1 1 d . . . . . C39 C 0.45581(15) 0.19850(14) 0.32604(5) 0.0218(3) Uani 1 1 d . . . . . H39A H 0.410666 0.231591 0.342665 0.033 Uiso 1 1 calc GR . . . . H39B H 0.403938 0.169733 0.306190 0.033 Uiso 1 1 calc GR . . . . H39C H 0.506327 0.248663 0.317000 0.033 Uiso 1 1 calc GR . . . . C40 C 0.60063(16) 0.05586(14) 0.31877(5) 0.0213(3) Uani 1 1 d . . . . . H40A H 0.631600 0.106443 0.303676 0.032 Uiso 1 1 calc GR . . . . H40B H 0.550101 0.009020 0.303931 0.032 Uiso 1 1 calc GR . . . . H40C H 0.663979 0.017621 0.332037 0.032 Uiso 1 1 calc GR . . . . C41 C 0.44485(18) -0.04105(16) 0.42551(5) 0.0284(4) Uani 1 1 d . . . . . H41A H 0.491174 -0.047077 0.448856 0.043 Uiso 1 1 calc GR . . . . H41B H 0.411199 -0.107305 0.418368 0.043 Uiso 1 1 calc GR . . . . H41C H 0.383365 0.008631 0.426766 0.043 Uiso 1 1 calc GR . . . . C42 C 0.60918(18) -0.09317(15) 0.39330(6) 0.0284(4) Uani 1 1 d . . . . . H42A H 0.666607 -0.069494 0.378720 0.043 Uiso 1 1 calc GR . . . . H42B H 0.567581 -0.151339 0.381708 0.043 Uiso 1 1 calc GR . . . . H42C H 0.647561 -0.113783 0.416703 0.043 Uiso 1 1 calc GR . . . . C43 C 0.62953(14) 0.12157(13) 0.44571(4) 0.0173(3) Uani 1 1 d . . . . . C44 C 0.55048(14) 0.17066(13) 0.46607(4) 0.0188(3) Uani 1 1 d . . . . . C45 C 0.59103(16) 0.19625(14) 0.50202(5) 0.0221(3) Uani 1 1 d . . . . . H45 H 0.540619 0.228787 0.516008 0.027 Uiso 1 1 calc R . . . . C46 C 0.70489(16) 0.17414(15) 0.51728(5) 0.0245(4) Uani 1 1 d . . . . . H46 H 0.729917 0.190983 0.541360 0.029 Uiso 1 1 calc R . . . . C47 C 0.78114(16) 0.12704(15) 0.49666(5) 0.0236(3) Uani 1 1 d . . . . . H47 H 0.857497 0.112977 0.507104 0.028 Uiso 1 1 calc R . . . . C48 C 0.74615(15) 0.10003(14) 0.46046(4) 0.0197(3) Uani 1 1 d . . . . . C49 C 0.42593(15) 0.20172(14) 0.45070(5) 0.0212(3) Uani 1 1 d . . . . . H49 H 0.407585 0.170158 0.426663 0.025 Uiso 1 1 calc R . . . . C50 C 0.41642(17) 0.31965(15) 0.44630(5) 0.0265(4) Uani 1 1 d . . . . . H50A H 0.437858 0.352334 0.469413 0.040 Uiso 1 1 calc GR . . . . H50B H 0.337247 0.337960 0.436992 0.040 Uiso 1 1 calc GR . . . . H50C H 0.468176 0.342647 0.429750 0.040 Uiso 1 1 calc GR . . . . C51 C 0.33578(17) 0.16191(18) 0.47464(5) 0.0301(4) Uani 1 1 d . . . . . H51A H 0.347115 0.088864 0.478873 0.045 Uiso 1 1 calc GR . . . . H51B H 0.257921 0.173962 0.462553 0.045 Uiso 1 1 calc GR . . . . H51C H 0.346238 0.198133 0.497372 0.045 Uiso 1 1 calc GR . . . . C52 C 0.83575(16) 0.05179(16) 0.43903(5) 0.0252(4) Uani 1 1 d . . . . . H52 H 0.797923 0.039915 0.414186 0.030 Uiso 1 1 calc R . . . . C53 C 0.94017(17) 0.12524(19) 0.43755(6) 0.0330(4) Uani 1 1 d . . . . . H53A H 0.912321 0.190845 0.427627 0.049 Uiso 1 1 calc GR . . . . H53B H 0.992925 0.095358 0.422516 0.049 Uiso 1 1 calc GR . . . . H53C H 0.980511 0.135398 0.461572 0.049 Uiso 1 1 calc GR . . . . C54 C 0.87885(19) -0.05329(18) 0.45526(6) 0.0347(5) Uani 1 1 d . . . . . H54A H 0.917060 -0.043129 0.479550 0.052 Uiso 1 1 calc GR . . . . H54B H 0.933171 -0.083266 0.440785 0.052 Uiso 1 1 calc GR . . . . H54C H 0.813223 -0.099098 0.455601 0.052 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.02084(9) 0.01906(9) 0.02606(10) -0.00101(7) 0.00578(7) -0.00263(7) Cl1 0.0354(3) 0.0275(2) 0.0617(4) -0.0031(2) 0.0077(3) -0.0146(2) Cl2 0.0408(3) 0.0303(2) 0.0223(2) -0.00060(17) 0.00021(18) -0.0081(2) Cl3 0.0231(2) 0.0227(2) 0.0466(3) 0.00534(19) 0.00224(19) 0.00097(16) Cl4 0.0384(3) 0.0335(2) 0.0379(3) 0.0006(2) 0.0199(2) 0.0064(2) P1 0.01852(19) 0.01747(18) 0.01267(17) 0.00029(14) 0.00348(14) -0.00412(15) N1 0.0168(6) 0.0159(6) 0.0157(6) -0.0019(5) 0.0045(5) -0.0022(5) N2 0.0143(6) 0.0133(6) 0.0151(6) -0.0004(5) 0.0039(5) -0.0025(5) N3 0.0177(6) 0.0185(6) 0.0130(6) 0.0029(5) 0.0016(5) -0.0036(5) C1 0.0136(6) 0.0166(7) 0.0116(6) 0.0006(5) 0.0019(5) -0.0012(5) C2 0.0219(8) 0.0147(7) 0.0219(8) -0.0028(6) 0.0059(6) -0.0032(6) C3 0.0194(7) 0.0140(7) 0.0212(7) -0.0013(6) 0.0053(6) -0.0046(6) C4 0.0188(7) 0.0177(7) 0.0196(7) -0.0022(6) 0.0080(6) -0.0013(6) C5 0.0195(8) 0.0212(8) 0.0251(8) -0.0011(6) 0.0064(6) -0.0006(6) C6 0.0200(8) 0.0282(9) 0.0379(11) -0.0011(8) 0.0096(7) 0.0011(7) C7 0.0296(10) 0.0307(10) 0.0407(11) -0.0070(8) 0.0203(9) 0.0002(8) C8 0.0353(10) 0.0320(10) 0.0255(9) -0.0077(8) 0.0163(8) -0.0022(8) C9 0.0257(8) 0.0217(8) 0.0200(8) -0.0043(6) 0.0081(6) -0.0037(7) C10 0.0208(8) 0.0373(10) 0.0241(9) 0.0010(8) -0.0001(7) 0.0040(7) C11 0.0441(13) 0.0554(15) 0.0353(12) 0.0169(11) -0.0056(10) -0.0145(11) C12 0.0294(10) 0.0365(11) 0.0383(12) -0.0030(9) -0.0063(9) 0.0027(9) C13 0.0303(9) 0.0340(10) 0.0182(8) -0.0040(7) 0.0052(7) -0.0031(8) C14 0.0421(12) 0.0438(13) 0.0345(11) -0.0083(10) 0.0026(10) -0.0141(10) C15 0.0466(13) 0.0455(13) 0.0217(9) 0.0037(9) -0.0011(9) -0.0081(10) C16 0.0148(7) 0.0141(6) 0.0166(7) 0.0002(5) 0.0057(5) -0.0022(5) C17 0.0211(7) 0.0146(7) 0.0163(7) 0.0008(5) 0.0049(6) -0.0029(6) C18 0.0313(9) 0.0175(7) 0.0199(8) 0.0007(6) 0.0115(7) -0.0044(7) C19 0.0274(9) 0.0186(8) 0.0305(9) -0.0017(7) 0.0165(7) -0.0026(7) C20 0.0184(7) 0.0174(7) 0.0322(9) 0.0011(6) 0.0089(7) 0.0008(6) C21 0.0156(7) 0.0153(7) 0.0213(7) 0.0013(6) 0.0038(6) -0.0022(5) C22 0.0244(8) 0.0179(7) 0.0181(7) 0.0034(6) 0.0016(6) -0.0006(6) C23 0.0336(10) 0.0180(8) 0.0291(9) 0.0039(7) -0.0008(8) -0.0004(7) C24 0.0431(11) 0.0226(8) 0.0195(8) 0.0036(7) -0.0065(8) -0.0018(8) C25 0.0180(7) 0.0217(8) 0.0228(8) 0.0026(6) 0.0006(6) 0.0001(6) C26 0.0359(11) 0.0287(10) 0.0294(10) -0.0015(8) -0.0086(8) -0.0013(8) C27 0.0225(9) 0.0274(9) 0.0340(10) 0.0075(8) -0.0019(7) 0.0021(7) C28 0.0136(6) 0.0155(7) 0.0136(6) 0.0002(5) 0.0019(5) -0.0019(5) C29 0.0155(7) 0.0141(6) 0.0153(7) -0.0008(5) 0.0044(5) -0.0039(5) C30 0.0211(7) 0.0151(7) 0.0164(7) 0.0004(5) 0.0045(6) -0.0024(6) C31 0.0274(8) 0.0178(7) 0.0171(7) -0.0005(6) 0.0071(6) -0.0040(6) C32 0.0282(9) 0.0184(8) 0.0233(8) -0.0048(6) 0.0116(7) -0.0030(6) C33 0.0208(8) 0.0185(7) 0.0273(9) -0.0014(6) 0.0067(7) 0.0003(6) C34 0.0180(7) 0.0172(7) 0.0206(7) 0.0004(6) 0.0025(6) -0.0020(6) C35 0.0146(7) 0.0187(7) 0.0128(6) 0.0027(5) 0.0016(5) -0.0010(5) C36 0.0165(7) 0.0189(7) 0.0133(6) 0.0017(5) 0.0013(5) -0.0050(6) C37 0.0190(7) 0.0248(8) 0.0171(7) 0.0021(6) 0.0015(6) -0.0097(6) C38 0.0221(8) 0.0224(8) 0.0157(7) 0.0038(6) 0.0007(6) -0.0080(6) C39 0.0203(8) 0.0244(8) 0.0194(8) 0.0037(6) -0.0022(6) -0.0030(6) C40 0.0245(8) 0.0209(8) 0.0192(8) -0.0032(6) 0.0064(6) -0.0084(6) C41 0.0356(10) 0.0306(10) 0.0194(8) 0.0047(7) 0.0050(7) -0.0160(8) C42 0.0353(10) 0.0210(8) 0.0275(9) 0.0040(7) -0.0007(8) -0.0033(7) C43 0.0182(7) 0.0216(7) 0.0120(6) 0.0038(6) 0.0014(5) -0.0045(6) C44 0.0182(7) 0.0230(8) 0.0152(7) 0.0044(6) 0.0026(6) -0.0037(6) C45 0.0248(8) 0.0274(9) 0.0149(7) 0.0014(6) 0.0051(6) -0.0028(7) C46 0.0266(9) 0.0330(9) 0.0135(7) 0.0040(7) 0.0006(6) -0.0063(7) C47 0.0190(8) 0.0330(9) 0.0177(8) 0.0062(7) -0.0013(6) -0.0037(7) C48 0.0182(7) 0.0254(8) 0.0152(7) 0.0051(6) 0.0015(6) -0.0024(6) C49 0.0174(7) 0.0283(9) 0.0182(7) 0.0034(6) 0.0038(6) -0.0007(6) C50 0.0245(9) 0.0302(9) 0.0251(9) 0.0026(7) 0.0038(7) 0.0040(7) C51 0.0212(8) 0.0441(12) 0.0265(9) 0.0041(8) 0.0084(7) -0.0019(8) C52 0.0188(8) 0.0367(10) 0.0200(8) 0.0047(7) 0.0019(6) 0.0028(7) C53 0.0195(8) 0.0527(13) 0.0269(9) 0.0081(9) 0.0042(7) -0.0010(8) C54 0.0312(10) 0.0387(11) 0.0332(11) 0.0046(9) 0.0009(8) 0.0113(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl1 2.1648(5) . ? Ga1 Cl2 2.1729(5) . ? Ga1 Cl3 2.1853(5) . ? Ga1 Cl4 2.1800(5) . ? P1 C28 1.7581(15) . ? P1 C35 1.7852(17) . ? N1 C1 1.375(2) . ? N1 C2 1.388(2) . ? N1 C4 1.452(2) . ? N2 C1 1.3823(19) . ? N2 C3 1.382(2) . ? N2 C16 1.4539(19) . ? N3 C35 1.349(2) . ? N3 C38 1.514(2) . ? N3 C43 1.447(2) . ? C1 C28 1.432(2) . ? C2 H2 0.9300 . ? C2 C3 1.344(2) . ? C3 H3 0.9300 . ? C4 C5 1.399(2) . ? C4 C9 1.404(2) . ? C5 C6 1.401(2) . ? C5 C10 1.520(3) . ? C6 H6 0.9300 . ? C6 C7 1.386(3) . ? C7 H7 0.9300 . ? C7 C8 1.381(3) . ? C8 H8 0.9300 . ? C8 C9 1.403(2) . ? C9 C13 1.519(3) . ? C10 H10 0.9800 . ? C10 C11 1.536(3) . ? C10 C12 1.531(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.537(3) . ? C13 C15 1.534(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.406(2) . ? C16 C21 1.398(2) . ? C17 C18 1.396(2) . ? C17 C22 1.517(2) . ? C18 H18 0.9300 . ? C18 C19 1.384(3) . ? C19 H19 0.9300 . ? C19 C20 1.383(3) . ? C20 H20 0.9300 . ? C20 C21 1.402(2) . ? C21 C25 1.518(2) . ? C22 H22 0.9800 . ? C22 C23 1.535(2) . ? C22 C24 1.534(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.536(3) . ? C25 C27 1.532(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.484(2) . ? C29 C30 1.398(2) . ? C29 C34 1.398(2) . ? C30 H30 0.9300 . ? C30 C31 1.394(2) . ? C31 H31 0.9300 . ? C31 C32 1.387(3) . ? C32 H32 0.9300 . ? C32 C33 1.391(3) . ? C33 H33 0.9300 . ? C33 C34 1.390(2) . ? C34 H34 0.9300 . ? C35 C36 1.546(2) . ? C36 C37 1.550(2) . ? C36 C39 1.534(2) . ? C36 C40 1.546(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.528(2) . ? C38 C41 1.527(2) . ? C38 C42 1.535(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.410(2) . ? C43 C48 1.408(2) . ? C44 C45 1.397(2) . ? C44 C49 1.524(2) . ? C45 H45 0.9300 . ? C45 C46 1.386(3) . ? C46 H46 0.9300 . ? C46 C47 1.382(3) . ? C47 H47 0.9300 . ? C47 C48 1.398(2) . ? C48 C52 1.519(2) . ? C49 H49 0.9800 . ? C49 C50 1.530(3) . ? C49 C51 1.544(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.537(3) . ? C52 C54 1.537(3) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? 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 Cl1 Ga1 Cl2 111.52(2) . . ? Cl1 Ga1 Cl3 108.16(2) . . ? Cl1 Ga1 Cl4 111.29(2) . . ? Cl2 Ga1 Cl3 109.57(2) . . ? Cl2 Ga1 Cl4 107.94(2) . . ? Cl4 Ga1 Cl3 108.30(2) . . ? C28 P1 C35 108.79(7) . . ? C1 N1 C2 109.92(13) . . ? C1 N1 C4 131.69(13) . . ? C2 N1 C4 117.62(13) . . ? C1 N2 C16 132.51(13) . . ? C3 N2 C1 109.88(13) . . ? C3 N2 C16 117.60(13) . . ? C35 N3 C38 113.73(13) . . ? C35 N3 C43 123.20(14) . . ? C43 N3 C38 123.06(13) . . ? N1 C1 N2 104.85(13) . . ? N1 C1 C28 128.06(14) . . ? N2 C1 C28 126.98(14) . . ? N1 C2 H2 126.2 . . ? C3 C2 N1 107.59(14) . . ? C3 C2 H2 126.2 . . ? N2 C3 H3 126.1 . . ? C2 C3 N2 107.76(14) . . ? C2 C3 H3 126.1 . . ? C5 C4 N1 118.09(15) . . ? C5 C4 C9 123.45(15) . . ? C9 C4 N1 117.34(15) . . ? C4 C5 C6 117.29(17) . . ? C4 C5 C10 122.09(15) . . ? C6 C5 C10 120.52(17) . . ? C5 C6 H6 119.7 . . ? C7 C6 C5 120.68(19) . . ? C7 C6 H6 119.7 . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.67(17) . . ? C8 C7 H7 119.7 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.29(18) . . ? C9 C8 H8 119.4 . . ? C4 C9 C13 122.56(15) . . ? C8 C9 C4 116.60(17) . . ? C8 C9 C13 120.82(17) . . ? C5 C10 H10 107.9 . . ? C5 C10 C11 110.34(18) . . ? C5 C10 C12 112.60(17) . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C12 C10 C11 110.11(18) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.8 . . ? C9 C13 C14 111.17(18) . . ? C9 C13 C15 111.90(17) . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C15 C13 C14 110.18(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 116.98(14) . . ? C21 C16 N2 119.01(14) . . ? C21 C16 C17 123.52(14) . . ? C16 C17 C22 122.78(14) . . ? C18 C17 C16 116.93(16) . . ? C18 C17 C22 120.28(15) . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.12(17) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.46(16) . . ? C20 C19 H19 119.8 . . ? C19 C20 H20 119.4 . . ? C19 C20 C21 121.24(16) . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 116.73(16) . . ? C16 C21 C25 121.71(14) . . ? C20 C21 C25 121.55(15) . . ? C17 C22 H22 108.0 . . ? C17 C22 C23 110.82(15) . . ? C17 C22 C24 112.89(15) . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C24 C22 C23 108.88(15) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.7 . . ? C21 C25 C26 111.07(15) . . ? C21 C25 C27 113.13(15) . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C27 C25 C26 109.29(15) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 117.26(11) . . ? C1 C28 C29 116.95(13) . . ? C29 C28 P1 124.11(11) . . ? C30 C29 C28 120.87(14) . . ? C30 C29 C34 118.62(15) . . ? C34 C29 C28 120.50(14) . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.50(16) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 119.8 . . ? C32 C31 C30 120.31(16) . . ? C32 C31 H31 119.8 . . ? C31 C32 H32 120.2 . . ? C31 C32 C33 119.66(16) . . ? C33 C32 H32 120.2 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.15(16) . . ? C34 C33 H33 119.9 . . ? C29 C34 H34 119.6 . . ? C33 C34 C29 120.74(16) . . ? C33 C34 H34 119.6 . . ? N3 C35 P1 115.96(12) . . ? N3 C35 C36 108.77(13) . . ? C36 C35 P1 133.95(11) . . ? C35 C36 C37 100.99(12) . . ? C35 C36 C40 116.18(13) . . ? C39 C36 C35 108.97(13) . . ? C39 C36 C37 111.03(14) . . ? C39 C36 C40 109.78(14) . . ? C40 C36 C37 109.61(14) . . ? C36 C37 H37A 110.5 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.6 . . ? C38 C37 C36 106.36(13) . . ? C38 C37 H37A 110.5 . . ? C38 C37 H37B 110.5 . . ? N3 C38 C37 98.89(13) . . ? N3 C38 C41 113.31(14) . . ? N3 C38 C42 110.17(14) . . ? C37 C38 C42 114.41(15) . . ? C41 C38 C37 112.79(15) . . ? C41 C38 C42 107.28(15) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 118.12(14) . . ? C48 C43 N3 119.94(15) . . ? C48 C43 C44 121.93(15) . . ? C43 C44 C49 123.93(15) . . ? C45 C44 C43 117.68(15) . . ? C45 C44 C49 118.32(15) . . ? C44 C45 H45 119.3 . . ? C46 C45 C44 121.34(17) . . ? C46 C45 H45 119.3 . . ? C45 C46 H46 120.0 . . ? C47 C46 C45 119.92(16) . . ? C47 C46 H46 120.0 . . ? C46 C47 H47 119.2 . . ? C46 C47 C48 121.52(16) . . ? C48 C47 H47 119.2 . . ? C43 C48 C52 123.69(15) . . ? C47 C48 C43 117.59(16) . . ? C47 C48 C52 118.71(15) . . ? C44 C49 H49 108.1 . . ? C44 C49 C50 110.55(15) . . ? C44 C49 C51 111.56(15) . . ? C50 C49 H49 108.1 . . ? C50 C49 C51 110.34(15) . . ? C51 C49 H49 108.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52 108.2 . . ? C48 C52 C53 110.90(17) . . ? C48 C52 C54 111.07(15) . . ? C53 C52 H52 108.2 . . ? C53 C52 C54 110.09(16) . . ? C54 C52 H52 108.2 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C28 C29 C30 128.18(14) . . . . ? P1 C28 C29 C34 -52.7(2) . . . . ? P1 C35 C36 C37 -152.31(14) . . . . ? P1 C35 C36 C39 -35.4(2) . . . . ? P1 C35 C36 C40 89.23(19) . . . . ? N1 C1 C28 P1 -28.2(2) . . . . ? N1 C1 C28 C29 165.91(15) . . . . ? N1 C2 C3 N2 0.1(2) . . . . ? N1 C4 C5 C6 -168.24(16) . . . . ? N1 C4 C5 C10 8.1(2) . . . . ? N1 C4 C9 C8 168.08(16) . . . . ? N1 C4 C9 C13 -10.4(2) . . . . ? N2 C1 C28 P1 147.36(14) . . . . ? N2 C1 C28 C29 -18.5(2) . . . . ? N2 C16 C17 C18 172.71(14) . . . . ? N2 C16 C17 C22 -5.8(2) . . . . ? N2 C16 C21 C20 -172.02(14) . . . . ? N2 C16 C21 C25 6.5(2) . . . . ? N3 C35 C36 C37 13.58(17) . . . . ? N3 C35 C36 C39 130.53(14) . . . . ? N3 C35 C36 C40 -104.88(16) . . . . ? N3 C43 C44 C45 179.78(15) . . . . ? N3 C43 C44 C49 -3.2(2) . . . . ? N3 C43 C48 C47 -179.42(15) . . . . ? N3 C43 C48 C52 2.1(3) . . . . ? C1 N1 C2 C3 0.3(2) . . . . ? C1 N1 C4 C5 -79.7(2) . . . . ? C1 N1 C4 C9 112.0(2) . . . . ? C1 N2 C3 C2 -0.55(19) . . . . ? C1 N2 C16 C17 103.0(2) . . . . ? C1 N2 C16 C21 -84.7(2) . . . . ? C1 C28 C29 C30 -67.0(2) . . . . ? C1 C28 C29 C34 112.06(17) . . . . ? C2 N1 C1 N2 -0.63(18) . . . . ? C2 N1 C1 C28 175.73(16) . . . . ? C2 N1 C4 C5 89.11(19) . . . . ? C2 N1 C4 C9 -79.2(2) . . . . ? C3 N2 C1 N1 0.72(17) . . . . ? C3 N2 C1 C28 -175.69(15) . . . . ? C3 N2 C16 C17 -75.51(19) . . . . ? C3 N2 C16 C21 96.71(18) . . . . ? C4 N1 C1 N2 168.81(16) . . . . ? C4 N1 C1 C28 -14.8(3) . . . . ? C4 N1 C2 C3 -170.80(15) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C4 C5 C10 C11 -97.0(2) . . . . ? C4 C5 C10 C12 139.55(18) . . . . ? C4 C9 C13 C14 107.7(2) . . . . ? C4 C9 C13 C15 -128.60(19) . . . . ? C5 C4 C9 C8 0.4(3) . . . . ? C5 C4 C9 C13 -178.04(17) . . . . ? C5 C6 C7 C8 -0.7(3) . . . . ? C6 C5 C10 C11 79.3(2) . . . . ? C6 C5 C10 C12 -44.2(3) . . . . ? C6 C7 C8 C9 0.5(3) . . . . ? C7 C8 C9 C4 -0.3(3) . . . . ? C7 C8 C9 C13 178.20(19) . . . . ? C8 C9 C13 C14 -70.7(2) . . . . ? C8 C9 C13 C15 53.0(2) . . . . ? C9 C4 C5 C6 -0.7(3) . . . . ? C9 C4 C5 C10 175.70(17) . . . . ? C10 C5 C6 C7 -175.62(19) . . . . ? C16 N2 C1 N1 -177.92(15) . . . . ? C16 N2 C1 C28 5.7(3) . . . . ? C16 N2 C3 C2 178.32(14) . . . . ? C16 C17 C18 C19 -1.5(2) . . . . ? C16 C17 C22 C23 99.27(19) . . . . ? C16 C17 C22 C24 -138.29(17) . . . . ? C16 C21 C25 C26 -83.4(2) . . . . ? C16 C21 C25 C27 153.27(16) . . . . ? C17 C16 C21 C20 -0.3(2) . . . . ? C17 C16 C21 C25 178.14(15) . . . . ? C17 C18 C19 C20 1.5(3) . . . . ? C18 C17 C22 C23 -79.2(2) . . . . ? C18 C17 C22 C24 43.2(2) . . . . ? C18 C19 C20 C21 -1.0(3) . . . . ? C19 C20 C21 C16 0.4(2) . . . . ? C19 C20 C21 C25 -178.11(16) . . . . ? C20 C21 C25 C26 95.0(2) . . . . ? C20 C21 C25 C27 -28.3(2) . . . . ? C21 C16 C17 C18 0.9(2) . . . . ? C21 C16 C17 C22 -177.66(15) . . . . ? C22 C17 C18 C19 177.12(16) . . . . ? C28 P1 C35 N3 159.59(12) . . . . ? C28 P1 C35 C36 -35.29(18) . . . . ? C28 C29 C30 C31 178.52(15) . . . . ? C28 C29 C34 C33 -177.61(15) . . . . ? C29 C30 C31 C32 -0.8(2) . . . . ? C30 C29 C34 C33 1.5(2) . . . . ? C30 C31 C32 C33 1.2(3) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C32 C33 C34 C29 -1.1(3) . . . . ? C34 C29 C30 C31 -0.6(2) . . . . ? C35 P1 C28 C1 167.46(12) . . . . ? C35 P1 C28 C29 -27.79(15) . . . . ? C35 N3 C38 C37 -25.75(18) . . . . ? C35 N3 C38 C41 -145.37(16) . . . . ? C35 N3 C38 C42 94.45(17) . . . . ? C35 N3 C43 C44 93.93(19) . . . . ? C35 N3 C43 C48 -85.3(2) . . . . ? C35 C36 C37 C38 -29.52(17) . . . . ? C36 C37 C38 N3 32.92(16) . . . . ? C36 C37 C38 C41 152.93(15) . . . . ? C36 C37 C38 C42 -84.09(17) . . . . ? C38 N3 C35 P1 176.57(11) . . . . ? C38 N3 C35 C36 7.83(18) . . . . ? C38 N3 C43 C44 -84.4(2) . . . . ? C38 N3 C43 C48 96.37(19) . . . . ? C39 C36 C37 C38 -144.94(15) . . . . ? C40 C36 C37 C38 93.60(16) . . . . ? C43 N3 C35 P1 -1.9(2) . . . . ? C43 N3 C35 C36 -170.66(14) . . . . ? C43 N3 C38 C37 152.74(15) . . . . ? C43 N3 C38 C41 33.1(2) . . . . ? C43 N3 C38 C42 -87.06(18) . . . . ? C43 C44 C45 C46 -0.1(3) . . . . ? C43 C44 C49 C50 -107.51(19) . . . . ? C43 C44 C49 C51 129.32(18) . . . . ? C43 C48 C52 C53 118.96(19) . . . . ? C43 C48 C52 C54 -118.28(19) . . . . ? C44 C43 C48 C47 1.4(2) . . . . ? C44 C43 C48 C52 -177.12(16) . . . . ? C44 C45 C46 C47 0.8(3) . . . . ? C45 C44 C49 C50 69.5(2) . . . . ? C45 C44 C49 C51 -53.6(2) . . . . ? C45 C46 C47 C48 -0.4(3) . . . . ? C46 C47 C48 C43 -0.6(3) . . . . ? C46 C47 C48 C52 177.95(17) . . . . ? C47 C48 C52 C53 -59.5(2) . . . . ? C47 C48 C52 C54 63.2(2) . . . . ? C48 C43 C44 C45 -1.0(2) . . . . ? C48 C43 C44 C49 176.02(16) . . . . ? C49 C44 C45 C46 -177.33(16) . . . . ? _shelx_res_file ; TITL sharma29_a.res in P2(1)/c sharma29.res created by SHELXL-2018/3 at 09:24:24 on 10-Apr-2019 REM Old TITL sharma29 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.112, Rweak 0.141, Alpha 0.038 REM 2.043 for 498 systematic absences, Orientation as input REM Formula found by SHELXT: C54 N3 Cl5 Ga CELL 0.71073 11.5123 12.8811 37.2397 90 97.724 90 ZERR 4 0.0002 0.0002 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ga N P UNIT 216 288 16 4 12 4 L.S. 11 PLAN 5 SIZE 0.231 0.25 0.411 MORE -1 BOND $H CONF fmap 2 acta OMIT 0 0 12 OMIT -3 6 12 OMIT -3 6 3 REM REM REM WGHT 0.028800 4.984300 FVAR 0.27290 GA1 4 0.057677 0.819615 0.365821 11.00000 0.02084 0.01906 = 0.02606 -0.00101 0.00578 -0.00263 CL1 3 0.145582 0.967629 0.375215 11.00000 0.03539 0.02752 = 0.06167 -0.00313 0.00771 -0.01457 CL2 3 0.059289 0.732410 0.415832 11.00000 0.04076 0.03032 = 0.02228 -0.00060 0.00021 -0.00815 CL3 3 -0.123355 0.849168 0.342061 11.00000 0.02312 0.02272 = 0.04663 0.00534 0.00224 0.00097 CL4 3 0.140755 0.724491 0.328083 11.00000 0.03839 0.03351 = 0.03786 0.00061 0.01990 0.00639 P1 6 0.671771 0.278220 0.391155 11.00000 0.01852 0.01747 = 0.01267 0.00029 0.00348 -0.00412 N1 5 0.724923 0.513268 0.372326 11.00000 0.01682 0.01591 = 0.01568 -0.00192 0.00453 -0.00220 N2 5 0.855661 0.473334 0.337166 11.00000 0.01435 0.01325 = 0.01509 -0.00039 0.00387 -0.00246 N3 5 0.588249 0.094377 0.408462 11.00000 0.01770 0.01849 = 0.01298 0.00293 0.00157 -0.00355 C1 1 0.765166 0.431957 0.353517 11.00000 0.01362 0.01663 = 0.01158 0.00063 0.00190 -0.00116 C2 1 0.790153 0.601858 0.367871 11.00000 0.02187 0.01469 = 0.02186 -0.00285 0.00589 -0.00320 AFIX 43 H2 2 0.780050 0.666698 0.377991 11.00000 -1.20000 AFIX 0 C3 1 0.870546 0.576931 0.346283 11.00000 0.01937 0.01404 = 0.02116 -0.00133 0.00526 -0.00459 AFIX 43 H3 2 0.926233 0.621436 0.338814 11.00000 -1.20000 AFIX 0 C4 1 0.620875 0.524718 0.390125 11.00000 0.01880 0.01769 = 0.01958 -0.00220 0.00802 -0.00129 C5 1 0.514655 0.547267 0.368621 11.00000 0.01952 0.02116 = 0.02513 -0.00106 0.00636 -0.00059 C6 1 0.420451 0.577284 0.386477 11.00000 0.02000 0.02822 = 0.03792 -0.00113 0.00958 0.00106 AFIX 43 H6 2 0.348229 0.592001 0.373071 11.00000 -1.20000 AFIX 0 C7 1 0.433746 0.585279 0.423912 11.00000 0.02955 0.03065 = 0.04075 -0.00704 0.02035 0.00017 AFIX 43 H7 2 0.370611 0.606079 0.435355 11.00000 -1.20000 AFIX 0 C8 1 0.539779 0.562680 0.444398 11.00000 0.03534 0.03198 = 0.02549 -0.00772 0.01635 -0.00222 AFIX 43 H8 2 0.546749 0.568031 0.469500 11.00000 -1.20000 AFIX 0 C9 1 0.637197 0.531808 0.428090 11.00000 0.02569 0.02174 = 0.01999 -0.00432 0.00807 -0.00369 C10 1 0.502243 0.545998 0.327467 11.00000 0.02081 0.03727 = 0.02412 0.00101 -0.00013 0.00399 AFIX 13 H10 2 0.566340 0.503992 0.320338 11.00000 -1.20000 AFIX 0 C11 1 0.514396 0.656341 0.312811 11.00000 0.04412 0.05543 = 0.03533 0.01690 -0.00556 -0.01446 AFIX 137 H11A 2 0.453762 0.699631 0.320056 11.00000 -1.50000 H11B 2 0.507399 0.654297 0.286841 11.00000 -1.50000 H11C 2 0.589623 0.684077 0.322376 11.00000 -1.50000 AFIX 0 C12 1 0.386475 0.497625 0.310284 11.00000 0.02940 0.03654 = 0.03827 -0.00303 -0.00630 0.00272 AFIX 137 H12A 2 0.376441 0.431241 0.321174 11.00000 -1.50000 H12B 2 0.387743 0.488923 0.284737 11.00000 -1.50000 H12C 2 0.322663 0.542385 0.314169 11.00000 -1.50000 AFIX 0 C13 1 0.754411 0.510192 0.450840 11.00000 0.03026 0.03398 = 0.01822 -0.00397 0.00522 -0.00315 AFIX 13 H13 2 0.806487 0.479703 0.434925 11.00000 -1.20000 AFIX 0 C14 1 0.811511 0.611019 0.466679 11.00000 0.04210 0.04376 = 0.03449 -0.00829 0.00255 -0.01411 AFIX 137 H14A 2 0.819044 0.658958 0.447390 11.00000 -1.50000 H14B 2 0.887696 0.595852 0.479455 11.00000 -1.50000 H14C 2 0.763454 0.641221 0.483087 11.00000 -1.50000 AFIX 0 C15 1 0.742782 0.432220 0.481286 11.00000 0.04656 0.04552 = 0.02167 0.00374 -0.00110 -0.00810 AFIX 137 H15A 2 0.694709 0.461495 0.497866 11.00000 -1.50000 H15B 2 0.819064 0.416847 0.493954 11.00000 -1.50000 H15C 2 0.707297 0.369520 0.471092 11.00000 -1.50000 AFIX 0 C16 1 0.931623 0.429426 0.312897 11.00000 0.01477 0.01414 = 0.01665 0.00024 0.00573 -0.00222 C17 1 0.906619 0.455398 0.276003 11.00000 0.02108 0.01457 = 0.01627 0.00078 0.00490 -0.00295 C18 1 0.987298 0.423367 0.253422 11.00000 0.03130 0.01746 = 0.01989 0.00075 0.01148 -0.00438 AFIX 43 H18 2 0.972902 0.437722 0.228750 11.00000 -1.20000 AFIX 0 C19 1 1.088291 0.370636 0.267134 11.00000 0.02744 0.01864 = 0.03049 -0.00168 0.01651 -0.00260 AFIX 43 H19 2 1.141823 0.351447 0.251732 11.00000 -1.20000 AFIX 0 C20 1 1.110187 0.346267 0.303581 11.00000 0.01835 0.01740 = 0.03223 0.00105 0.00887 0.00080 AFIX 43 H20 2 1.177905 0.309870 0.312296 11.00000 -1.20000 AFIX 0 C21 1 1.032205 0.375406 0.327644 11.00000 0.01561 0.01527 = 0.02132 0.00128 0.00384 -0.00218 C22 1 0.799333 0.517506 0.260734 11.00000 0.02444 0.01795 = 0.01809 0.00339 0.00161 -0.00059 AFIX 13 H22 2 0.742582 0.513949 0.278094 11.00000 -1.20000 AFIX 0 C23 1 0.831024 0.631988 0.256055 11.00000 0.03362 0.01798 = 0.02911 0.00393 -0.00084 -0.00037 AFIX 137 H23A 2 0.867671 0.659171 0.278794 11.00000 -1.50000 H23B 2 0.761111 0.670806 0.248091 11.00000 -1.50000 H23C 2 0.884113 0.637601 0.238354 11.00000 -1.50000 AFIX 0 C24 1 0.739936 0.475427 0.224297 11.00000 0.04310 0.02255 = 0.01947 0.00363 -0.00647 -0.00178 AFIX 137 H24A 2 0.787829 0.490640 0.205754 11.00000 -1.50000 H24B 2 0.664626 0.507654 0.218329 11.00000 -1.50000 H24C 2 0.730182 0.401655 0.226006 11.00000 -1.50000 AFIX 0 C25 1 1.057418 0.351827 0.367873 11.00000 0.01802 0.02168 = 0.02279 0.00263 0.00059 0.00007 AFIX 13 H25 2 0.982216 0.339459 0.376729 11.00000 -1.20000 AFIX 0 C26 1 1.116232 0.444673 0.388871 11.00000 0.03586 0.02866 = 0.02943 -0.00146 -0.00863 -0.00130 AFIX 137 H26A 2 1.191192 0.457448 0.381136 11.00000 -1.50000 H26B 2 1.126648 0.429568 0.414346 11.00000 -1.50000 H26C 2 1.067625 0.505048 0.384260 11.00000 -1.50000 AFIX 0 C27 1 1.133330 0.254896 0.376277 11.00000 0.02247 0.02743 = 0.03398 0.00745 -0.00191 0.00209 AFIX 137 H27A 2 1.099355 0.197727 0.362013 11.00000 -1.50000 H27B 2 1.137355 0.238247 0.401541 11.00000 -1.50000 H27C 2 1.210848 0.267976 0.370543 11.00000 -1.50000 AFIX 0 C28 1 0.727616 0.325914 0.352682 11.00000 0.01363 0.01547 = 0.01356 0.00016 0.00188 -0.00185 C29 1 0.764525 0.259207 0.323768 11.00000 0.01548 0.01407 = 0.01530 -0.00076 0.00442 -0.00394 C30 1 0.721696 0.276650 0.287340 11.00000 0.02107 0.01512 = 0.01643 0.00040 0.00451 -0.00244 AFIX 43 H30 2 0.667982 0.329717 0.281109 11.00000 -1.20000 AFIX 0 C31 1 0.758900 0.215090 0.260278 11.00000 0.02744 0.01779 = 0.01709 -0.00047 0.00713 -0.00404 AFIX 43 H31 2 0.729178 0.226775 0.236142 11.00000 -1.20000 AFIX 0 C32 1 0.840007 0.136526 0.269180 11.00000 0.02822 0.01840 = 0.02335 -0.00479 0.01162 -0.00304 AFIX 43 H32 2 0.865806 0.096403 0.251053 11.00000 -1.20000 AFIX 0 C33 1 0.882589 0.118030 0.305362 11.00000 0.02076 0.01845 = 0.02732 -0.00142 0.00671 0.00034 AFIX 43 H33 2 0.936724 0.065201 0.311451 11.00000 -1.20000 AFIX 0 C34 1 0.844412 0.178328 0.332435 11.00000 0.01800 0.01720 = 0.02060 0.00041 0.00254 -0.00198 AFIX 43 H34 2 0.872309 0.164732 0.356584 11.00000 -1.20000 AFIX 0 C35 1 0.602235 0.156298 0.380153 11.00000 0.01457 0.01870 = 0.01284 0.00268 0.00162 -0.00095 C36 1 0.530126 0.111431 0.345634 11.00000 0.01653 0.01891 = 0.01328 0.00171 0.00132 -0.00499 C37 1 0.451991 0.031635 0.362307 11.00000 0.01904 0.02478 = 0.01710 0.00214 0.00149 -0.00967 AFIX 23 H37A 2 0.379263 0.063774 0.366936 11.00000 -1.20000 H37B 2 0.433580 -0.026439 0.345949 11.00000 -1.20000 AFIX 0 C38 1 0.522495 -0.005078 0.397745 11.00000 0.02210 0.02240 = 0.01571 0.00378 0.00067 -0.00802 C39 1 0.455809 0.198504 0.326038 11.00000 0.02029 0.02443 = 0.01942 0.00373 -0.00222 -0.00303 AFIX 137 H39A 2 0.410666 0.231591 0.342665 11.00000 -1.50000 H39B 2 0.403938 0.169733 0.306190 11.00000 -1.50000 H39C 2 0.506327 0.248663 0.317000 11.00000 -1.50000 AFIX 0 C40 1 0.600632 0.055864 0.318774 11.00000 0.02453 0.02093 = 0.01924 -0.00321 0.00637 -0.00840 AFIX 137 H40A 2 0.631600 0.106443 0.303676 11.00000 -1.50000 H40B 2 0.550101 0.009020 0.303931 11.00000 -1.50000 H40C 2 0.663979 0.017621 0.332037 11.00000 -1.50000 AFIX 0 C41 1 0.444852 -0.041045 0.425511 11.00000 0.03564 0.03063 = 0.01944 0.00474 0.00503 -0.01599 AFIX 137 H41A 2 0.491174 -0.047077 0.448856 11.00000 -1.50000 H41B 2 0.411199 -0.107305 0.418368 11.00000 -1.50000 H41C 2 0.383365 0.008631 0.426766 11.00000 -1.50000 AFIX 0 C42 1 0.609175 -0.093170 0.393303 11.00000 0.03529 0.02098 = 0.02750 0.00403 -0.00069 -0.00330 AFIX 137 H42A 2 0.666607 -0.069494 0.378720 11.00000 -1.50000 H42B 2 0.567581 -0.151339 0.381708 11.00000 -1.50000 H42C 2 0.647561 -0.113783 0.416703 11.00000 -1.50000 AFIX 0 C43 1 0.629533 0.121565 0.445708 11.00000 0.01822 0.02155 = 0.01197 0.00384 0.00143 -0.00454 C44 1 0.550480 0.170660 0.466074 11.00000 0.01823 0.02301 = 0.01521 0.00441 0.00262 -0.00369 C45 1 0.591026 0.196252 0.502022 11.00000 0.02483 0.02739 = 0.01489 0.00142 0.00512 -0.00282 AFIX 43 H45 2 0.540619 0.228787 0.516008 11.00000 -1.20000 AFIX 0 C46 1 0.704885 0.174139 0.517278 11.00000 0.02656 0.03295 = 0.01347 0.00402 0.00059 -0.00626 AFIX 43 H46 2 0.729917 0.190983 0.541360 11.00000 -1.20000 AFIX 0 C47 1 0.781140 0.127037 0.496659 11.00000 0.01899 0.03300 = 0.01766 0.00622 -0.00125 -0.00367 AFIX 43 H47 2 0.857497 0.112977 0.507104 11.00000 -1.20000 AFIX 0 C48 1 0.746154 0.100030 0.460458 11.00000 0.01823 0.02539 = 0.01517 0.00506 0.00150 -0.00236 C49 1 0.425929 0.201719 0.450701 11.00000 0.01737 0.02831 = 0.01816 0.00343 0.00380 -0.00068 AFIX 13 H49 2 0.407585 0.170158 0.426663 11.00000 -1.20000 AFIX 0 C50 1 0.416416 0.319652 0.446304 11.00000 0.02445 0.03015 = 0.02512 0.00260 0.00380 0.00396 AFIX 137 H50A 2 0.437858 0.352334 0.469413 11.00000 -1.50000 H50B 2 0.337247 0.337960 0.436992 11.00000 -1.50000 H50C 2 0.468176 0.342647 0.429750 11.00000 -1.50000 AFIX 0 C51 1 0.335777 0.161906 0.474638 11.00000 0.02118 0.04409 = 0.02647 0.00415 0.00843 -0.00193 AFIX 137 H51A 2 0.347115 0.088864 0.478873 11.00000 -1.50000 H51B 2 0.257921 0.173962 0.462553 11.00000 -1.50000 H51C 2 0.346238 0.198133 0.497372 11.00000 -1.50000 AFIX 0 C52 1 0.835747 0.051793 0.439025 11.00000 0.01877 0.03666 = 0.02000 0.00474 0.00193 0.00276 AFIX 13 H52 2 0.797923 0.039915 0.414186 11.00000 -1.20000 AFIX 0 C53 1 0.940172 0.125238 0.437546 11.00000 0.01952 0.05271 = 0.02692 0.00808 0.00415 -0.00104 AFIX 137 H53A 2 0.912321 0.190845 0.427627 11.00000 -1.50000 H53B 2 0.992925 0.095358 0.422516 11.00000 -1.50000 H53C 2 0.980511 0.135398 0.461572 11.00000 -1.50000 AFIX 0 C54 1 0.878847 -0.053291 0.455265 11.00000 0.03121 0.03867 = 0.03320 0.00458 0.00092 0.01130 AFIX 137 H54A 2 0.917060 -0.043129 0.479550 11.00000 -1.50000 H54B 2 0.933171 -0.083266 0.440785 11.00000 -1.50000 H54C 2 0.813223 -0.099098 0.455601 11.00000 -1.50000 AFIX 0 HKLF 4 REM sharma29_a.res in P2(1)/c REM wR2 = 0.1106, GooF = S = 1.174, Restrained GooF = 1.174 for all data REM R1 = 0.0544 for 16638 Fo > 4sig(Fo) and 0.0642 for all 19071 data REM 584 parameters refined using 0 restraints END WGHT 0.0288 4.9868 REM Highest difference peak 0.689, deepest hole -0.638, 1-sigma level 0.066 Q1 1 0.1210 0.8422 0.3731 11.00000 0.05 0.69 Q2 1 0.1966 0.7543 0.3384 11.00000 0.05 0.66 Q3 1 0.0917 0.8725 0.3668 11.00000 0.05 0.57 Q4 1 -0.0556 0.8439 0.3306 11.00000 0.05 0.54 Q5 1 0.6459 0.2081 0.3858 11.00000 0.05 0.49 ; _shelx_res_checksum 65051 _olex2_date_sample_data_collection 2019-04-08 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.208 _oxdiff_exptl_absorpt_empirical_full_min 0.841 ####################################################################### # # 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_compound4 _database_code_depnum_ccdc_archive 'CCDC 1949888' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-06-26 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' beate.neumann@uni-bielefeld.de _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C54 H72 N3 P' _chemical_formula_sum 'C54 H72 N3 P' _chemical_formula_weight 794.11 _chemical_melting_point ? _chemical_oxdiff_formula 'C54 H72 N3 P' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.56270(10) _cell_length_b 15.9337(2) _cell_length_c 23.6169(2) _cell_angle_alpha 90 _cell_angle_beta 93.5540(10) _cell_angle_gamma 90 _cell_volume 4718.31(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 52810 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 76.3720 _cell_measurement_theta_min 3.2990 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 1728 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 4 5 0.1096 0 -4 -5 0.1096 -1 -2 5 0.1415 1 2 -5 0.1415 -1 0 0 0.1836 1 0 0 0.1836 0 -5 -1 0.1587 0 5 1 0.1587 1 -1 -5 0.1064 2 1 5 0.1967 -1 2 -5 0.1298 -2 -1 -5 0.1065 -2 -5 -1 0.1505 3 5 -2 0.1708 _exptl_crystal_size_max 0.449 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.219 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0006 4.0039 4.9960 -0.4627 -0.0085 0.2055 -0.0006 -4.0039 -4.9960 0.4627 0.0085 -0.2055 -1.0004 -1.9996 4.9954 -0.2096 0.0564 -0.3271 1.0004 1.9996 -4.9954 0.2096 -0.0564 0.3271 -1.0000 -0.0003 0.0002 -0.0035 0.1219 -0.0152 1.0000 0.0003 -0.0002 0.0035 -0.1219 0.0152 -0.0008 -5.0030 -0.9997 0.2722 -0.0382 -0.4033 0.0008 5.0030 0.9997 -0.2722 0.0382 0.4033 0.9999 -1.0020 -4.9958 0.3379 -0.0849 0.0684 2.0001 1.0028 4.9953 -0.3273 -0.2807 -0.0228 -0.9996 1.9991 -4.9951 0.2025 0.1873 0.2967 -2.0001 -1.0028 -4.9953 0.3273 0.2807 0.0228 -2.0008 -5.0036 -0.9994 0.2651 0.2055 -0.4337 3.0008 5.0028 -1.9980 -0.0866 -0.2995 0.5326 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 86959 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.717 _diffrn_reflns_theta_min 3.348 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -85.00 -19.00 1.00 3.00 -- -38.50 -38.00 60.00 66 2 \w -51.00 33.00 1.00 3.00 -- -38.50 38.00 30.00 84 3 \w -107.00 -19.00 1.00 3.00 -- -38.50 -38.00-150.00 88 4 \w -69.00 29.00 1.00 3.00 -- -38.50 88.00-112.00 98 5 \w -47.00 30.00 1.00 3.00 -- -38.50 38.00-150.00 77 6 \w 17.00 80.00 1.00 3.00 -- 42.89 77.00 150.00 63 7 \w 1.00 78.00 1.00 3.00 -- 42.89 -99.00 90.00 77 8 \w 13.00 114.00 1.00 3.00 -- 42.89 77.00 -60.00 101 9 \w 16.00 65.00 1.00 3.00 -- 42.89 77.00-150.00 49 10 \w 85.00 111.00 1.00 3.00 -- 42.89 57.00 -90.00 26 11 \w 16.00 60.00 1.00 3.00 -- 42.89 77.00 0.00 44 12 \w 18.00 64.00 1.00 3.00 -- 42.89 57.00 -90.00 46 13 \w 13.00 78.00 1.00 3.00 -- 42.89 77.00 90.00 65 14 \w 21.00 95.00 1.00 3.00 -- 42.89 57.00 60.00 74 15 \w 40.00 77.00 1.00 11.98 -- 111.00 -77.00 -90.00 37 16 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 -60.00 27 17 \w 81.00 107.00 1.00 11.98 -- 111.00 76.00 86.29 26 18 \w 113.00 175.00 1.00 11.98 -- 111.00 77.00 -30.00 62 19 \w 85.00 112.00 1.00 11.98 -- 111.00 61.00 -60.00 27 20 \w 119.00 153.00 1.00 11.98 -- 111.00 51.00-160.62 34 21 \w 84.00 111.00 1.00 11.98 -- 111.00 64.00 -82.88 27 22 \w 81.00 177.00 1.00 11.98 -- 111.00 77.00 60.00 96 23 \w 48.00 141.00 1.00 11.98 -- 111.00 -77.00 60.00 93 24 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00 -30.00 26 25 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 0.00 26 26 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 60.00 26 27 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00-120.00 27 28 \w 89.00 115.00 1.00 11.98 -- 111.00 45.00 90.00 26 29 \w 85.00 178.00 1.00 11.98 -- 111.00 61.00 120.00 93 30 \w 58.00 117.00 1.00 11.98 -- 111.00-125.00 30.00 59 31 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 120.00 27 32 \w 82.00 118.00 1.00 11.98 -- 111.00-125.00 -60.00 36 33 \w 86.00 177.00 1.00 11.98 -- 111.00 61.00 30.00 91 34 \w 83.00 178.00 1.00 11.98 -- 111.00 68.00-144.88 95 35 \w 87.00 115.00 1.00 11.98 -- 111.00 51.00-160.62 28 36 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00-120.00 26 37 \w 81.00 176.00 1.00 11.98 -- 111.00 77.00 150.00 95 38 \w 41.00 118.00 1.00 11.98 -- 111.00-125.00 90.00 77 39 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 90.00 26 40 \w 116.00 178.00 1.00 11.98 -- 111.00 77.00 -90.00 62 41 \w 81.00 108.00 1.00 11.98 -- 111.00 77.00 0.00 27 42 \w 111.00 178.00 1.00 11.98 -- 111.00 77.00 0.00 67 43 \w 84.00 110.00 1.00 11.98 -- 111.00 65.00-109.92 26 44 \w 81.00 110.00 1.00 11.98 -- 111.00 77.00 90.00 29 45 \w 121.00 171.00 1.00 11.98 -- 111.00 77.00 90.00 50 46 \w 85.00 120.00 1.00 11.98 -- 111.00 61.00 -30.00 35 47 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00 -90.00 26 48 \w 83.00 109.00 1.00 11.98 -- 111.00 77.00 30.00 26 49 \w 81.00 107.00 1.00 11.98 -- 111.00 77.00-180.00 26 50 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00-180.00 26 51 \w 85.00 147.00 1.00 11.98 -- 111.00 61.00-150.00 62 52 \w 42.00 93.00 1.00 11.98 -- 111.00 -77.00-150.00 51 53 \w 107.00 141.00 1.00 11.98 -- 111.00 -77.00-150.00 34 54 \w 85.00 111.00 1.00 11.98 -- 111.00 61.00 -90.00 26 55 \w 85.00 125.00 1.00 11.98 -- 111.00 61.00 150.00 40 56 \w 109.00 178.00 1.00 11.98 -- 111.00 77.00-120.00 69 57 \w 114.00 139.00 1.00 11.98 -- 111.00 -77.00 -90.00 25 58 \w 82.00 108.00 1.00 11.98 -- 111.00 72.00 0.65 26 59 \w 85.00 177.00 1.00 11.98 -- 111.00 59.00 46.28 92 60 \w 63.00 64.00 1.00 11.98 -- 111.00-125.00-150.00 1 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0035436000 _diffrn_orient_matrix_UB_12 -0.0427493000 _diffrn_orient_matrix_UB_13 -0.0583530000 _diffrn_orient_matrix_UB_21 -0.1218682000 _diffrn_orient_matrix_UB_22 0.0095195000 _diffrn_orient_matrix_UB_23 -0.0093074000 _diffrn_orient_matrix_UB_31 0.0151921000 _diffrn_orient_matrix_UB_32 0.0861936000 _diffrn_orient_matrix_UB_33 -0.0279417000 _diffrn_oxdiff_digest_frames ; 0180a4d5b456edcbad7a27c7fc6e55b281000283ddf ; _diffrn_oxdiff_digest_hkl ; 01c9c8e4428880672235094ca7806e94f101d2 ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9416 _reflns_number_total 9876 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)' _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 0.267 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 539 _refine_ls_number_reflns 9876 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0358 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+1.7295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.0933 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52) 2.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B, H53C), C54(H54A,H54B,H54C) ; _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 P1 P 0.71737(2) 0.26153(2) 0.40868(2) 0.01588(7) Uani 1 1 d . . . . . N1 N 0.70907(7) 0.40828(6) 0.31528(4) 0.01735(17) Uani 1 1 d . . . . . N2 N 0.54374(7) 0.38351(5) 0.28366(3) 0.01679(17) Uani 1 1 d . . . . . N3 N 0.76674(7) 0.18389(5) 0.50732(3) 0.01695(17) Uani 1 1 d . . . . . C1 C 0.61652(7) 0.36664(6) 0.33002(4) 0.01558(19) Uani 1 1 d . . . . . C2 C 0.69157(8) 0.44810(7) 0.26280(4) 0.0213(2) Uani 1 1 d . . . . . H2 H 0.741501 0.479205 0.244258 0.026 Uiso 1 1 calc R . . . . C3 C 0.59131(8) 0.43388(7) 0.24396(4) 0.0212(2) Uani 1 1 d . . . . . H3 H 0.558570 0.453951 0.210244 0.025 Uiso 1 1 calc R . . . . C4 C 0.80968(8) 0.42459(6) 0.34584(4) 0.0178(2) Uani 1 1 d . . . . . C5 C 0.90044(8) 0.38670(7) 0.32528(4) 0.0199(2) Uani 1 1 d . . . . . C6 C 0.99996(8) 0.41761(7) 0.34513(5) 0.0233(2) Uani 1 1 d . . . . . H6 H 1.061587 0.394875 0.331510 0.028 Uiso 1 1 calc R . . . . C7 C 1.00799(9) 0.48150(7) 0.38472(5) 0.0258(2) Uani 1 1 d . . . . . H7 H 1.074722 0.502479 0.396677 0.031 Uiso 1 1 calc R . . . . C8 C 0.91712(9) 0.51454(7) 0.40674(5) 0.0247(2) Uani 1 1 d . . . . . H8 H 0.923985 0.555387 0.434863 0.030 Uiso 1 1 calc R . . . . C9 C 0.81559(8) 0.48756(7) 0.38744(4) 0.0207(2) Uani 1 1 d . . . . . C10 C 0.89249(9) 0.31386(7) 0.28366(5) 0.0241(2) Uani 1 1 d . . . . . H10 H 0.817086 0.298300 0.278183 0.029 Uiso 1 1 calc R . . . . C11 C 0.93092(10) 0.33862(9) 0.22562(5) 0.0332(3) Uani 1 1 d . . . . . H11A H 0.888994 0.384743 0.210512 0.050 Uiso 1 1 calc GR . . . . H11B H 0.923294 0.291657 0.200223 0.050 Uiso 1 1 calc GR . . . . H11C H 1.004547 0.354951 0.229769 0.050 Uiso 1 1 calc GR . . . . C12 C 0.95340(10) 0.23698(8) 0.30748(5) 0.0303(3) Uani 1 1 d . . . . . H12A H 1.027850 0.250287 0.312990 0.045 Uiso 1 1 calc GR . . . . H12B H 0.944157 0.191159 0.281240 0.045 Uiso 1 1 calc GR . . . . H12C H 0.926338 0.221350 0.343116 0.045 Uiso 1 1 calc GR . . . . C13 C 0.71489(9) 0.52568(7) 0.40932(5) 0.0249(2) Uani 1 1 d . . . . . H13 H 0.661461 0.480947 0.410050 0.030 Uiso 1 1 calc R . . . . C14 C 0.66881(11) 0.59486(8) 0.36982(6) 0.0349(3) Uani 1 1 d . . . . . H14A H 0.719423 0.639822 0.368287 0.052 Uiso 1 1 calc GR . . . . H14B H 0.603919 0.615744 0.384020 0.052 Uiso 1 1 calc GR . . . . H14C H 0.654258 0.572315 0.332450 0.052 Uiso 1 1 calc GR . . . . C15 C 0.73130(11) 0.56049(8) 0.46959(5) 0.0329(3) Uani 1 1 d . . . . . H15A H 0.769210 0.520105 0.493311 0.049 Uiso 1 1 calc GR . . . . H15B H 0.663214 0.571652 0.484347 0.049 Uiso 1 1 calc GR . . . . H15C H 0.771762 0.611551 0.468942 0.049 Uiso 1 1 calc GR . . . . C16 C 0.43991(8) 0.34874(7) 0.26973(4) 0.01649(19) Uani 1 1 d . . . . . C17 C 0.35281(8) 0.40410(7) 0.26634(4) 0.01724(19) Uani 1 1 d . . . . . C18 C 0.25230(8) 0.37105(7) 0.25069(4) 0.0196(2) Uani 1 1 d . . . . . H18 H 0.193394 0.406487 0.247627 0.024 Uiso 1 1 calc R . . . . C19 C 0.23926(8) 0.28635(7) 0.23969(4) 0.0218(2) Uani 1 1 d . . . . . H19 H 0.171555 0.264913 0.230422 0.026 Uiso 1 1 calc R . . . . C20 C 0.32690(9) 0.23327(7) 0.24243(4) 0.0214(2) Uani 1 1 d . . . . . H20 H 0.316931 0.176465 0.234765 0.026 Uiso 1 1 calc R . . . . C21 C 0.42951(8) 0.26293(7) 0.25638(4) 0.0183(2) Uani 1 1 d . . . . . C22 C 0.36383(8) 0.49750(7) 0.27852(5) 0.0206(2) Uani 1 1 d . . . . . H22 H 0.437043 0.507998 0.293619 0.025 Uiso 1 1 calc R . . . . C23 C 0.34516(10) 0.54839(7) 0.22358(5) 0.0277(2) Uani 1 1 d . . . . . H23A H 0.393852 0.529953 0.196388 0.041 Uiso 1 1 calc GR . . . . H23B H 0.356725 0.606872 0.231558 0.041 Uiso 1 1 calc GR . . . . H23C H 0.273222 0.540151 0.208447 0.041 Uiso 1 1 calc GR . . . . C24 C 0.28791(9) 0.52756(7) 0.32272(5) 0.0254(2) Uani 1 1 d . . . . . H24A H 0.215483 0.520651 0.308009 0.038 Uiso 1 1 calc GR . . . . H24B H 0.301181 0.585733 0.331037 0.038 Uiso 1 1 calc GR . . . . H24C H 0.299558 0.495092 0.356786 0.038 Uiso 1 1 calc GR . . . . C25 C 0.52620(9) 0.20542(7) 0.25549(4) 0.0217(2) Uani 1 1 d . . . . . H25 H 0.571716 0.216451 0.289890 0.026 Uiso 1 1 calc R . . . . C26 C 0.59157(10) 0.22455(9) 0.20418(5) 0.0333(3) Uani 1 1 d . . . . . H26A H 0.549581 0.212245 0.169837 0.050 Uiso 1 1 calc GR . . . . H26B H 0.654803 0.190572 0.206043 0.050 Uiso 1 1 calc GR . . . . H26C H 0.611200 0.282782 0.204597 0.050 Uiso 1 1 calc GR . . . . C27 C 0.49797(10) 0.11210(7) 0.25488(5) 0.0293(3) Uani 1 1 d . . . . . H27A H 0.453983 0.099938 0.285667 0.044 Uiso 1 1 calc GR . . . . H27B H 0.562198 0.079437 0.259002 0.044 Uiso 1 1 calc GR . . . . H27C H 0.460004 0.098311 0.219572 0.044 Uiso 1 1 calc GR . . . . C28 C 0.60194(8) 0.31695(6) 0.37705(4) 0.01601(19) Uani 1 1 d . . . . . C29 C 0.49250(8) 0.28794(7) 0.38706(4) 0.01694(19) Uani 1 1 d . . . . . C30 C 0.41044(8) 0.34508(7) 0.39537(4) 0.0198(2) Uani 1 1 d . . . . . H30 H 0.425443 0.402235 0.396395 0.024 Uiso 1 1 calc R . . . . C31 C 0.30669(9) 0.31791(8) 0.40211(5) 0.0254(2) Uani 1 1 d . . . . . H31 H 0.253116 0.356919 0.407341 0.031 Uiso 1 1 calc R . . . . C32 C 0.28291(9) 0.23303(8) 0.40108(5) 0.0284(3) Uani 1 1 d . . . . . H32 H 0.213289 0.214940 0.404737 0.034 Uiso 1 1 calc R . . . . C33 C 0.36384(9) 0.17521(8) 0.39454(5) 0.0259(2) Uani 1 1 d . . . . . H33 H 0.348626 0.118083 0.394453 0.031 Uiso 1 1 calc R . . . . C34 C 0.46732(8) 0.20229(7) 0.38812(4) 0.0203(2) Uani 1 1 d . . . . . H34 H 0.521030 0.162860 0.384442 0.024 Uiso 1 1 calc R . . . . C35 C 0.69940(8) 0.24174(6) 0.47968(4) 0.01651(19) Uani 1 1 d . . . . . C36 C 0.62579(8) 0.27686(7) 0.52384(4) 0.0188(2) Uani 1 1 d . . . . . C37 C 0.68881(9) 0.25341(7) 0.57983(4) 0.0210(2) Uani 1 1 d . . . . . H37A H 0.737814 0.298144 0.591401 0.025 Uiso 1 1 calc R . . . . H37B H 0.640355 0.244589 0.609695 0.025 Uiso 1 1 calc R . . . . C38 C 0.75018(8) 0.17296(7) 0.56906(4) 0.0193(2) Uani 1 1 d . . . . . C39 C 0.61351(9) 0.37203(7) 0.51930(5) 0.0244(2) Uani 1 1 d . . . . . H39A H 0.682706 0.397816 0.521968 0.037 Uiso 1 1 calc GR . . . . H39B H 0.572624 0.392005 0.549566 0.037 Uiso 1 1 calc GR . . . . H39C H 0.577499 0.386076 0.483519 0.037 Uiso 1 1 calc GR . . . . C40 C 0.51406(8) 0.23620(8) 0.52166(5) 0.0236(2) Uani 1 1 d . . . . . H40A H 0.468337 0.263966 0.493473 0.035 Uiso 1 1 calc GR . . . . H40B H 0.484624 0.241467 0.558049 0.035 Uiso 1 1 calc GR . . . . H40C H 0.519746 0.177871 0.512117 0.035 Uiso 1 1 calc GR . . . . C41 C 0.85430(9) 0.16774(7) 0.60603(4) 0.0230(2) Uani 1 1 d . . . . . H41A H 0.900884 0.127536 0.590106 0.035 Uiso 1 1 calc GR . . . . H41B H 0.839218 0.150625 0.643675 0.035 Uiso 1 1 calc GR . . . . H41C H 0.888147 0.221777 0.607513 0.035 Uiso 1 1 calc GR . . . . C42 C 0.68750(9) 0.09229(7) 0.57979(5) 0.0260(2) Uani 1 1 d . . . . . H42A H 0.623482 0.091311 0.555398 0.039 Uiso 1 1 calc GR . . . . H42B H 0.669312 0.090791 0.618667 0.039 Uiso 1 1 calc GR . . . . H42C H 0.730553 0.044364 0.572025 0.039 Uiso 1 1 calc GR . . . . C43 C 0.84467(8) 0.13640(6) 0.47871(4) 0.01763(19) Uani 1 1 d . . . . . C44 C 0.81472(9) 0.06302(7) 0.44827(4) 0.0197(2) Uani 1 1 d . . . . . C45 C 0.89383(10) 0.01744(7) 0.42299(5) 0.0243(2) Uani 1 1 d . . . . . H45 H 0.875300 -0.031299 0.403080 0.029 Uiso 1 1 calc R . . . . C46 C 0.99912(10) 0.04304(7) 0.42685(5) 0.0262(2) Uani 1 1 d . . . . . H46 H 1.050827 0.011269 0.410184 0.031 Uiso 1 1 calc R . . . . C47 C 1.02718(9) 0.11598(7) 0.45554(5) 0.0238(2) Uani 1 1 d . . . . . H47 H 1.098043 0.133224 0.457725 0.029 Uiso 1 1 calc R . . . . C48 C 0.95135(8) 0.16428(7) 0.48131(4) 0.0194(2) Uani 1 1 d . . . . . C49 C 0.70005(9) 0.03342(7) 0.43932(5) 0.0236(2) Uani 1 1 d . . . . . H49 H 0.654055 0.073520 0.457651 0.028 Uiso 1 1 calc R . . . . C50 C 0.66691(10) 0.03111(8) 0.37575(5) 0.0313(3) Uani 1 1 d . . . . . H50A H 0.680138 0.084861 0.359222 0.047 Uiso 1 1 calc GR . . . . H50B H 0.592337 0.018077 0.370580 0.047 Uiso 1 1 calc GR . . . . H50C H 0.707523 -0.011067 0.357651 0.047 Uiso 1 1 calc GR . . . . C51 C 0.68319(11) -0.05361(8) 0.46487(6) 0.0334(3) Uani 1 1 d . . . . . H51A H 0.723337 -0.094426 0.445225 0.050 Uiso 1 1 calc GR . . . . H51B H 0.608811 -0.067754 0.461078 0.050 Uiso 1 1 calc GR . . . . H51C H 0.706862 -0.053167 0.504304 0.050 Uiso 1 1 calc GR . . . . C52 C 0.98644(8) 0.24709(7) 0.50845(4) 0.0206(2) Uani 1 1 d . . . . . H52 H 0.928440 0.267630 0.530657 0.025 Uiso 1 1 calc R . . . . C53 C 1.00590(9) 0.31203(7) 0.46264(5) 0.0237(2) Uani 1 1 d . . . . . H53A H 1.062587 0.293167 0.440336 0.036 Uiso 1 1 calc GR . . . . H53B H 1.025288 0.364652 0.480191 0.036 Uiso 1 1 calc GR . . . . H53C H 0.942047 0.319076 0.438618 0.036 Uiso 1 1 calc GR . . . . C54 C 1.08630(9) 0.23711(7) 0.54870(5) 0.0260(2) Uani 1 1 d . . . . . H54A H 1.075885 0.191759 0.574535 0.039 Uiso 1 1 calc GR . . . . H54B H 1.098788 0.288125 0.569692 0.039 Uiso 1 1 calc GR . . . . H54C H 1.146702 0.225203 0.527035 0.039 Uiso 1 1 calc GR . . . . 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 P1 0.01624(12) 0.01828(13) 0.01303(12) 0.00163(9) 0.00016(9) 0.00062(9) N1 0.0147(4) 0.0211(4) 0.0161(4) 0.0039(3) -0.0002(3) -0.0012(3) N2 0.0150(4) 0.0210(4) 0.0142(4) 0.0029(3) -0.0010(3) -0.0006(3) N3 0.0200(4) 0.0181(4) 0.0125(4) 0.0012(3) -0.0002(3) 0.0001(3) C1 0.0139(4) 0.0174(5) 0.0153(4) -0.0011(4) -0.0003(3) 0.0006(3) C2 0.0189(5) 0.0264(5) 0.0187(5) 0.0076(4) 0.0023(4) -0.0005(4) C3 0.0197(5) 0.0269(5) 0.0168(5) 0.0068(4) 0.0009(4) 0.0013(4) C4 0.0153(4) 0.0197(5) 0.0182(5) 0.0051(4) -0.0007(4) -0.0030(4) C5 0.0179(5) 0.0227(5) 0.0188(5) 0.0058(4) 0.0005(4) 0.0002(4) C6 0.0158(5) 0.0285(6) 0.0257(5) 0.0087(4) 0.0011(4) -0.0003(4) C7 0.0196(5) 0.0281(6) 0.0289(6) 0.0080(4) -0.0043(4) -0.0071(4) C8 0.0265(5) 0.0222(5) 0.0250(5) 0.0016(4) -0.0028(4) -0.0065(4) C9 0.0214(5) 0.0195(5) 0.0213(5) 0.0033(4) 0.0011(4) -0.0030(4) C10 0.0201(5) 0.0284(6) 0.0238(5) -0.0007(4) 0.0021(4) 0.0029(4) C11 0.0326(6) 0.0443(7) 0.0229(6) 0.0022(5) 0.0022(5) 0.0103(5) C12 0.0330(6) 0.0287(6) 0.0295(6) 0.0003(5) 0.0057(5) 0.0072(5) C13 0.0248(5) 0.0225(5) 0.0282(6) -0.0036(4) 0.0062(4) -0.0045(4) C14 0.0330(6) 0.0321(7) 0.0405(7) 0.0000(5) 0.0079(5) 0.0085(5) C15 0.0374(7) 0.0292(6) 0.0331(6) -0.0100(5) 0.0103(5) -0.0121(5) C16 0.0153(4) 0.0219(5) 0.0120(4) 0.0004(4) -0.0010(3) -0.0004(4) C17 0.0178(5) 0.0207(5) 0.0131(4) 0.0000(4) 0.0002(3) 0.0006(4) C18 0.0163(4) 0.0256(5) 0.0167(4) 0.0009(4) -0.0004(4) 0.0017(4) C19 0.0184(5) 0.0279(6) 0.0186(5) 0.0001(4) -0.0022(4) -0.0041(4) C20 0.0250(5) 0.0201(5) 0.0188(5) -0.0015(4) -0.0017(4) -0.0029(4) C21 0.0208(5) 0.0214(5) 0.0126(4) -0.0002(4) -0.0010(4) 0.0016(4) C22 0.0191(5) 0.0197(5) 0.0229(5) -0.0014(4) -0.0004(4) 0.0011(4) C23 0.0310(6) 0.0229(5) 0.0296(6) 0.0042(4) 0.0065(5) 0.0036(4) C24 0.0295(6) 0.0236(5) 0.0231(5) -0.0019(4) 0.0008(4) 0.0070(4) C25 0.0244(5) 0.0221(5) 0.0181(5) -0.0027(4) -0.0022(4) 0.0048(4) C26 0.0351(6) 0.0396(7) 0.0261(6) -0.0002(5) 0.0079(5) 0.0137(5) C27 0.0350(6) 0.0232(6) 0.0286(6) -0.0072(4) -0.0079(5) 0.0061(5) C28 0.0160(4) 0.0175(5) 0.0143(4) -0.0002(4) -0.0006(3) -0.0011(4) C29 0.0178(5) 0.0221(5) 0.0107(4) 0.0012(4) -0.0011(3) -0.0027(4) C30 0.0195(5) 0.0244(5) 0.0154(5) 0.0020(4) 0.0004(4) -0.0007(4) C31 0.0187(5) 0.0374(6) 0.0203(5) 0.0037(4) 0.0022(4) 0.0013(4) C32 0.0193(5) 0.0419(7) 0.0241(5) 0.0050(5) 0.0019(4) -0.0094(5) C33 0.0279(6) 0.0284(6) 0.0211(5) 0.0033(4) -0.0004(4) -0.0109(4) C34 0.0224(5) 0.0225(5) 0.0158(5) 0.0010(4) -0.0008(4) -0.0032(4) C35 0.0168(4) 0.0160(5) 0.0164(5) -0.0005(4) -0.0014(4) -0.0029(4) C36 0.0203(5) 0.0219(5) 0.0141(4) -0.0007(4) 0.0006(4) 0.0002(4) C37 0.0233(5) 0.0254(5) 0.0140(5) -0.0013(4) -0.0002(4) 0.0009(4) C38 0.0230(5) 0.0227(5) 0.0122(4) 0.0008(4) -0.0001(4) -0.0010(4) C39 0.0300(6) 0.0228(5) 0.0203(5) -0.0022(4) 0.0008(4) 0.0045(4) C40 0.0206(5) 0.0332(6) 0.0172(5) 0.0023(4) 0.0027(4) -0.0010(4) C41 0.0255(5) 0.0281(6) 0.0150(5) 0.0016(4) -0.0019(4) 0.0024(4) C42 0.0318(6) 0.0266(6) 0.0194(5) 0.0056(4) 0.0011(4) -0.0042(4) C43 0.0222(5) 0.0172(5) 0.0134(4) 0.0031(4) -0.0002(4) 0.0021(4) C44 0.0266(5) 0.0177(5) 0.0147(4) 0.0027(4) -0.0011(4) -0.0001(4) C45 0.0358(6) 0.0176(5) 0.0196(5) -0.0009(4) 0.0015(4) 0.0023(4) C46 0.0320(6) 0.0238(6) 0.0237(5) 0.0024(4) 0.0079(4) 0.0074(4) C47 0.0232(5) 0.0244(5) 0.0242(5) 0.0049(4) 0.0044(4) 0.0015(4) C48 0.0230(5) 0.0192(5) 0.0159(4) 0.0041(4) 0.0004(4) 0.0004(4) C49 0.0273(5) 0.0201(5) 0.0227(5) -0.0021(4) -0.0030(4) -0.0020(4) C50 0.0382(6) 0.0273(6) 0.0268(6) -0.0067(5) -0.0099(5) 0.0014(5) C51 0.0362(6) 0.0240(6) 0.0398(7) 0.0021(5) -0.0007(5) -0.0078(5) C52 0.0202(5) 0.0209(5) 0.0204(5) 0.0017(4) -0.0007(4) -0.0014(4) C53 0.0232(5) 0.0225(5) 0.0250(5) 0.0042(4) -0.0027(4) -0.0032(4) C54 0.0261(5) 0.0263(6) 0.0247(5) 0.0035(4) -0.0049(4) -0.0021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C28 1.8183(10) . ? P1 C35 1.7346(10) . ? N1 C1 1.4012(12) . ? N1 C2 1.3975(13) . ? N1 C4 1.4399(12) . ? N2 C1 1.4082(12) . ? N2 C3 1.3963(13) . ? N2 C16 1.4364(12) . ? N3 C35 1.3867(13) . ? N3 C38 1.4959(12) . ? N3 C43 1.4385(13) . ? C1 C28 1.3855(14) . ? C2 H2 0.9300 . ? C2 C3 1.3291(15) . ? C3 H3 0.9300 . ? C4 C5 1.4031(14) . ? C4 C9 1.4029(15) . ? C5 C6 1.3973(15) . ? C5 C10 1.5203(15) . ? C6 H6 0.9300 . ? C6 C7 1.3817(17) . ? C7 H7 0.9300 . ? C7 C8 1.3873(17) . ? C8 H8 0.9300 . ? C8 C9 1.3956(15) . ? C9 C13 1.5223(15) . ? C10 H10 0.9800 . ? C10 C11 1.5328(16) . ? C10 C12 1.5327(16) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.5341(17) . ? C13 C15 1.5296(16) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.4038(14) . ? C16 C21 1.4075(15) . ? C17 C18 1.3967(14) . ? C17 C22 1.5205(14) . ? C18 H18 0.9300 . ? C18 C19 1.3822(16) . ? C19 H19 0.9300 . ? C19 C20 1.3867(15) . ? C20 H20 0.9300 . ? C20 C21 1.3931(15) . ? C21 C25 1.5229(14) . ? C22 H22 0.9800 . ? C22 C23 1.5356(15) . ? C22 C24 1.5337(15) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.5358(16) . ? C25 C27 1.5285(16) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.4833(13) . ? C29 C30 1.3982(15) . ? C29 C34 1.4015(15) . ? C30 H30 0.9300 . ? C30 C31 1.3919(15) . ? C31 H31 0.9300 . ? C31 C32 1.3849(18) . ? C32 H32 0.9300 . ? C32 C33 1.3878(18) . ? C33 H33 0.9300 . ? C33 C34 1.3870(15) . ? C34 H34 0.9300 . ? C35 C36 1.5413(14) . ? C36 C37 1.5445(14) . ? C36 C39 1.5273(15) . ? C36 C40 1.5439(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.5252(15) . ? C38 C41 1.5292(14) . ? C38 C42 1.5367(15) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.4113(14) . ? C43 C48 1.4097(14) . ? C44 C45 1.3947(15) . ? C44 C49 1.5180(15) . ? C45 H45 0.9300 . ? C45 C46 1.3817(17) . ? C46 H46 0.9300 . ? C46 C47 1.3801(17) . ? C47 H47 0.9300 . ? C47 C48 1.3935(15) . ? C48 C52 1.5203(15) . ? C49 H49 0.9800 . ? C49 C50 1.5334(15) . ? C49 C51 1.5322(16) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.5276(15) . ? C52 C54 1.5344(15) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? 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 C35 P1 C28 109.70(5) . . ? C1 N1 C4 132.61(8) . . ? C2 N1 C1 110.37(8) . . ? C2 N1 C4 116.59(8) . . ? C1 N2 C16 129.87(8) . . ? C3 N2 C1 110.33(8) . . ? C3 N2 C16 119.23(8) . . ? C35 N3 C38 114.74(8) . . ? C35 N3 C43 122.80(8) . . ? C43 N3 C38 122.45(8) . . ? N1 C1 N2 103.01(8) . . ? C28 C1 N1 128.52(9) . . ? C28 C1 N2 128.37(9) . . ? N1 C2 H2 125.9 . . ? C3 C2 N1 108.25(9) . . ? C3 C2 H2 125.9 . . ? N2 C3 H3 126.0 . . ? C2 C3 N2 108.02(9) . . ? C2 C3 H3 126.0 . . ? C5 C4 N1 117.11(9) . . ? C9 C4 N1 119.13(9) . . ? C9 C4 C5 122.76(9) . . ? C4 C5 C10 122.01(9) . . ? C6 C5 C4 117.50(10) . . ? C6 C5 C10 120.49(10) . . ? C5 C6 H6 119.6 . . ? C7 C6 C5 120.86(10) . . ? C7 C6 H6 119.6 . . ? C6 C7 H7 119.8 . . ? C6 C7 C8 120.40(10) . . ? C8 C7 H7 119.8 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.15(11) . . ? C9 C8 H8 119.4 . . ? C4 C9 C13 120.94(9) . . ? C8 C9 C4 117.17(10) . . ? C8 C9 C13 121.87(10) . . ? C5 C10 H10 107.6 . . ? C5 C10 C11 111.72(10) . . ? C5 C10 C12 111.19(9) . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C12 C10 C11 110.86(9) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.5 . . ? C9 C13 C14 111.75(9) . . ? C9 C13 C15 113.19(10) . . ? C14 C13 H13 107.5 . . ? C15 C13 H13 107.5 . . ? C15 C13 C14 109.23(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 117.66(9) . . ? C17 C16 C21 122.44(9) . . ? C21 C16 N2 119.76(9) . . ? C16 C17 C22 122.87(9) . . ? C18 C17 C16 117.83(9) . . ? C18 C17 C22 119.29(9) . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.83(10) . . ? C19 C18 H18 119.6 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.15(10) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 119.2 . . ? C19 C20 C21 121.63(10) . . ? C21 C20 H20 119.2 . . ? C16 C21 C25 121.64(9) . . ? C20 C21 C16 117.01(9) . . ? C20 C21 C25 121.32(10) . . ? C17 C22 H22 108.0 . . ? C17 C22 C23 110.47(9) . . ? C17 C22 C24 112.41(9) . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C24 C22 C23 109.96(9) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.8 . . ? C21 C25 C26 110.95(9) . . ? C21 C25 C27 113.62(9) . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C27 C25 C26 108.71(10) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 117.72(7) . . ? C1 C28 C29 118.41(8) . . ? C29 C28 P1 120.45(7) . . ? C30 C29 C28 121.21(9) . . ? C30 C29 C34 117.54(9) . . ? C34 C29 C28 121.24(9) . . ? C29 C30 H30 119.4 . . ? C31 C30 C29 121.15(10) . . ? C31 C30 H30 119.4 . . ? C30 C31 H31 119.9 . . ? C32 C31 C30 120.28(11) . . ? C32 C31 H31 119.9 . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.45(10) . . ? C33 C32 H32 120.3 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.24(11) . . ? C34 C33 H33 119.9 . . ? C29 C34 H34 119.4 . . ? C33 C34 C29 121.27(10) . . ? C33 C34 H34 119.4 . . ? N3 C35 P1 117.62(7) . . ? N3 C35 C36 107.28(8) . . ? C36 C35 P1 135.04(8) . . ? C35 C36 C37 101.20(8) . . ? C35 C36 C40 114.05(8) . . ? C39 C36 C35 112.04(9) . . ? C39 C36 C37 110.15(9) . . ? C39 C36 C40 109.07(9) . . ? C40 C36 C37 110.10(9) . . ? C36 C37 H37A 110.2 . . ? C36 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C38 C37 C36 107.34(8) . . ? C38 C37 H37A 110.2 . . ? C38 C37 H37B 110.2 . . ? N3 C38 C37 99.62(8) . . ? N3 C38 C41 113.40(8) . . ? N3 C38 C42 111.22(8) . . ? C37 C38 C41 111.95(9) . . ? C37 C38 C42 113.95(9) . . ? C41 C38 C42 106.81(9) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 120.49(9) . . ? C48 C43 N3 119.12(9) . . ? C48 C43 C44 120.40(9) . . ? C43 C44 C49 123.30(10) . . ? C45 C44 C43 118.35(10) . . ? C45 C44 C49 118.29(10) . . ? C44 C45 H45 119.2 . . ? C46 C45 C44 121.51(10) . . ? C46 C45 H45 119.2 . . ? C45 C46 H46 120.2 . . ? C47 C46 C45 119.69(10) . . ? C47 C46 H46 120.2 . . ? C46 C47 H47 119.4 . . ? C46 C47 C48 121.25(10) . . ? C48 C47 H47 119.4 . . ? C43 C48 C52 122.81(9) . . ? C47 C48 C43 118.74(10) . . ? C47 C48 C52 118.38(10) . . ? C44 C49 H49 108.4 . . ? C44 C49 C50 109.96(9) . . ? C44 C49 C51 112.30(9) . . ? C50 C49 H49 108.4 . . ? C51 C49 H49 108.4 . . ? C51 C49 C50 109.15(10) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52 108.0 . . ? C48 C52 C53 110.13(9) . . ? C48 C52 C54 112.07(9) . . ? C53 C52 H52 108.0 . . ? C53 C52 C54 110.38(9) . . ? C54 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C28 C29 C30 140.89(8) . . . . ? P1 C28 C29 C34 -39.61(12) . . . . ? P1 C35 C36 C37 -158.21(9) . . . . ? P1 C35 C36 C39 -40.88(14) . . . . ? P1 C35 C36 C40 83.62(12) . . . . ? N1 C1 C28 P1 -28.15(14) . . . . ? N1 C1 C28 C29 172.60(9) . . . . ? N1 C2 C3 N2 -1.02(13) . . . . ? N1 C4 C5 C6 164.47(9) . . . . ? N1 C4 C5 C10 -16.43(14) . . . . ? N1 C4 C9 C8 -165.77(9) . . . . ? N1 C4 C9 C13 12.95(15) . . . . ? N2 C1 C28 P1 147.63(9) . . . . ? N2 C1 C28 C29 -11.61(16) . . . . ? N2 C16 C17 C18 177.60(8) . . . . ? N2 C16 C17 C22 -1.97(14) . . . . ? N2 C16 C21 C20 -179.08(9) . . . . ? N2 C16 C21 C25 -0.82(14) . . . . ? N3 C35 C36 C37 18.75(10) . . . . ? N3 C35 C36 C39 136.08(9) . . . . ? N3 C35 C36 C40 -99.41(10) . . . . ? N3 C43 C44 C45 -177.68(9) . . . . ? N3 C43 C44 C49 5.29(15) . . . . ? N3 C43 C48 C47 177.27(9) . . . . ? N3 C43 C48 C52 -5.91(14) . . . . ? C1 N1 C2 C3 0.50(13) . . . . ? C1 N1 C4 C5 115.15(12) . . . . ? C1 N1 C4 C9 -75.93(14) . . . . ? C1 N2 C3 C2 1.20(12) . . . . ? C1 N2 C16 C17 119.32(11) . . . . ? C1 N2 C16 C21 -64.91(14) . . . . ? C1 C28 C29 C30 -60.45(13) . . . . ? C1 C28 C29 C34 119.05(11) . . . . ? C2 N1 C1 N2 0.23(11) . . . . ? C2 N1 C1 C28 176.84(10) . . . . ? C2 N1 C4 C5 -73.28(12) . . . . ? C2 N1 C4 C9 95.65(12) . . . . ? C3 N2 C1 N1 -0.85(11) . . . . ? C3 N2 C1 C28 -177.47(10) . . . . ? C3 N2 C16 C17 -70.22(12) . . . . ? C3 N2 C16 C21 105.56(11) . . . . ? C4 N1 C1 N2 172.20(10) . . . . ? C4 N1 C1 C28 -11.19(18) . . . . ? C4 N1 C2 C3 -172.90(9) . . . . ? C4 C5 C6 C7 1.78(15) . . . . ? C4 C5 C10 C11 113.20(11) . . . . ? C4 C5 C10 C12 -122.35(11) . . . . ? C4 C9 C13 C14 -82.51(13) . . . . ? C4 C9 C13 C15 153.68(10) . . . . ? C5 C4 C9 C8 2.50(15) . . . . ? C5 C4 C9 C13 -178.79(10) . . . . ? C5 C6 C7 C8 1.86(17) . . . . ? C6 C5 C10 C11 -67.73(13) . . . . ? C6 C5 C10 C12 56.72(13) . . . . ? C6 C7 C8 C9 -3.48(17) . . . . ? C7 C8 C9 C4 1.31(16) . . . . ? C7 C8 C9 C13 -177.39(10) . . . . ? C8 C9 C13 C14 96.15(13) . . . . ? C8 C9 C13 C15 -27.67(15) . . . . ? C9 C4 C5 C6 -4.02(15) . . . . ? C9 C4 C5 C10 175.08(10) . . . . ? C10 C5 C6 C7 -177.34(10) . . . . ? C16 N2 C1 N1 170.28(9) . . . . ? C16 N2 C1 C28 -6.33(17) . . . . ? C16 N2 C3 C2 -171.01(9) . . . . ? C16 C17 C18 C19 0.85(15) . . . . ? C16 C17 C22 C23 109.90(11) . . . . ? C16 C17 C22 C24 -126.86(10) . . . . ? C16 C21 C25 C26 -71.65(13) . . . . ? C16 C21 C25 C27 165.52(9) . . . . ? C17 C16 C21 C20 -3.51(15) . . . . ? C17 C16 C21 C25 174.75(9) . . . . ? C17 C18 C19 C20 -1.95(16) . . . . ? C18 C17 C22 C23 -69.66(12) . . . . ? C18 C17 C22 C24 53.57(13) . . . . ? C18 C19 C20 C21 0.26(16) . . . . ? C19 C20 C21 C16 2.38(15) . . . . ? C19 C20 C21 C25 -175.89(10) . . . . ? C20 C21 C25 C26 106.54(12) . . . . ? C20 C21 C25 C27 -16.30(14) . . . . ? C21 C16 C17 C18 1.94(15) . . . . ? C21 C16 C17 C22 -177.63(9) . . . . ? C22 C17 C18 C19 -179.56(9) . . . . ? C28 P1 C35 N3 165.51(7) . . . . ? C28 P1 C35 C36 -17.77(11) . . . . ? C28 C29 C30 C31 176.97(9) . . . . ? C28 C29 C34 C33 -176.61(9) . . . . ? C29 C30 C31 C32 0.42(16) . . . . ? C30 C29 C34 C33 2.91(15) . . . . ? C30 C31 C32 C33 1.44(17) . . . . ? C31 C32 C33 C34 -1.10(17) . . . . ? C32 C33 C34 C29 -1.13(16) . . . . ? C34 C29 C30 C31 -2.55(14) . . . . ? C35 P1 C28 C1 154.73(8) . . . . ? C35 P1 C28 C29 -46.47(9) . . . . ? C35 N3 C38 C37 -18.34(11) . . . . ? C35 N3 C38 C41 -137.45(9) . . . . ? C35 N3 C38 C42 102.16(10) . . . . ? C35 N3 C43 C44 -82.11(12) . . . . ? C35 N3 C43 C48 97.69(11) . . . . ? C35 C36 C37 C38 -30.53(10) . . . . ? C36 C37 C38 N3 29.67(10) . . . . ? C36 C37 C38 C41 149.84(9) . . . . ? C36 C37 C38 C42 -88.81(10) . . . . ? C38 N3 C35 P1 177.21(7) . . . . ? C38 N3 C35 C36 -0.36(11) . . . . ? C38 N3 C43 C44 96.24(11) . . . . ? C38 N3 C43 C48 -83.96(12) . . . . ? C39 C36 C37 C38 -149.22(9) . . . . ? C40 C36 C37 C38 90.46(10) . . . . ? C43 N3 C35 P1 -4.32(13) . . . . ? C43 N3 C35 C36 178.10(9) . . . . ? C43 N3 C38 C37 163.18(9) . . . . ? C43 N3 C38 C41 44.08(13) . . . . ? C43 N3 C38 C42 -76.32(12) . . . . ? C43 C44 C45 C46 -0.54(16) . . . . ? C43 C44 C49 C50 118.83(11) . . . . ? C43 C44 C49 C51 -119.43(11) . . . . ? C43 C48 C52 C53 -103.90(11) . . . . ? C43 C48 C52 C54 132.81(10) . . . . ? C44 C43 C48 C47 -2.93(15) . . . . ? C44 C43 C48 C52 173.89(9) . . . . ? C44 C45 C46 C47 -1.01(17) . . . . ? C45 C44 C49 C50 -58.21(13) . . . . ? C45 C44 C49 C51 63.54(13) . . . . ? C45 C46 C47 C48 0.59(17) . . . . ? C46 C47 C48 C43 1.37(16) . . . . ? C46 C47 C48 C52 -175.59(10) . . . . ? C47 C48 C52 C53 72.93(12) . . . . ? C47 C48 C52 C54 -50.36(13) . . . . ? C48 C43 C44 C45 2.52(15) . . . . ? C48 C43 C44 C49 -174.51(9) . . . . ? C49 C44 C45 C46 176.64(10) . . . . ? _shelx_res_file ; TITL sharma40_a.res in P2(1)/n sharma40.res created by SHELXL-2018/3 at 09:40:48 on 26-Jun-2019 REM Old TITL sharma40 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.111, Rweak 0.007, Alpha 0.040 REM 0.994 for 371 systematic absences, Orientation as input REM Formula found by SHELXT: C54 N1 P1 CELL 1.54184 12.5627 15.9337 23.6169 90 93.554 90 ZERR 4 0.0001 0.0002 0.0002 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N P UNIT 216 288 12 4 L.S. 11 PLAN 13 MORE -1 BOND $H CONF fmap 2 acta OMIT -6 18 5 OMIT -6 18 6 OMIT -6 18 7 REM REM REM WGHT 0.047700 1.729500 FVAR 3.30703 P1 4 0.717372 0.261528 0.408684 11.00000 0.01624 0.01828 = 0.01303 0.00163 0.00016 0.00062 N1 3 0.709070 0.408277 0.315277 11.00000 0.01468 0.02110 = 0.01614 0.00385 -0.00017 -0.00116 N2 3 0.543736 0.383506 0.283659 11.00000 0.01497 0.02095 = 0.01421 0.00288 -0.00103 -0.00059 N3 3 0.766744 0.183892 0.507316 11.00000 0.02005 0.01813 = 0.01253 0.00115 -0.00019 0.00008 C1 1 0.616518 0.366640 0.330023 11.00000 0.01393 0.01740 = 0.01528 -0.00111 -0.00029 0.00064 C2 1 0.691575 0.448101 0.262803 11.00000 0.01892 0.02643 = 0.01872 0.00764 0.00226 -0.00050 AFIX 43 H2 2 0.741501 0.479205 0.244258 11.00000 -1.20000 AFIX 0 C3 1 0.591306 0.433876 0.243960 11.00000 0.01974 0.02691 = 0.01679 0.00681 0.00088 0.00133 AFIX 43 H3 2 0.558570 0.453951 0.210244 11.00000 -1.20000 AFIX 0 C4 1 0.809684 0.424587 0.345845 11.00000 0.01531 0.01969 = 0.01818 0.00511 -0.00070 -0.00296 C5 1 0.900438 0.386704 0.325283 11.00000 0.01794 0.02273 = 0.01882 0.00582 0.00053 0.00019 C6 1 0.999959 0.417606 0.345127 11.00000 0.01582 0.02849 = 0.02567 0.00874 0.00107 -0.00033 AFIX 43 H6 2 1.061587 0.394875 0.331510 11.00000 -1.20000 AFIX 0 C7 1 1.007992 0.481499 0.384720 11.00000 0.01956 0.02809 = 0.02888 0.00797 -0.00430 -0.00715 AFIX 43 H7 2 1.074722 0.502479 0.396677 11.00000 -1.20000 AFIX 0 C8 1 0.917122 0.514542 0.406744 11.00000 0.02653 0.02216 = 0.02498 0.00159 -0.00278 -0.00648 AFIX 43 H8 2 0.923985 0.555387 0.434863 11.00000 -1.20000 AFIX 0 C9 1 0.815588 0.487557 0.387437 11.00000 0.02141 0.01948 = 0.02132 0.00326 0.00106 -0.00298 C10 1 0.892492 0.313864 0.283656 11.00000 0.02006 0.02840 = 0.02379 -0.00072 0.00207 0.00289 AFIX 13 H10 2 0.817086 0.298300 0.278183 11.00000 -1.20000 AFIX 0 C11 1 0.930922 0.338616 0.225618 11.00000 0.03264 0.04427 = 0.02288 0.00221 0.00224 0.01027 AFIX 137 H11A 2 0.888994 0.384743 0.210512 11.00000 -1.50000 H11B 2 0.923294 0.291657 0.200223 11.00000 -1.50000 H11C 2 1.004547 0.354951 0.229769 11.00000 -1.50000 AFIX 0 C12 1 0.953399 0.236983 0.307475 11.00000 0.03302 0.02869 = 0.02951 0.00034 0.00566 0.00724 AFIX 137 H12A 2 1.027850 0.250287 0.312990 11.00000 -1.50000 H12B 2 0.944157 0.191159 0.281240 11.00000 -1.50000 H12C 2 0.926338 0.221350 0.343116 11.00000 -1.50000 AFIX 0 C13 1 0.714895 0.525681 0.409320 11.00000 0.02476 0.02247 = 0.02816 -0.00360 0.00618 -0.00452 AFIX 13 H13 2 0.661461 0.480947 0.410050 11.00000 -1.20000 AFIX 0 C14 1 0.668813 0.594863 0.369824 11.00000 0.03296 0.03208 = 0.04049 -0.00001 0.00791 0.00846 AFIX 137 H14A 2 0.719423 0.639822 0.368287 11.00000 -1.50000 H14B 2 0.603919 0.615744 0.384020 11.00000 -1.50000 H14C 2 0.654258 0.572315 0.332450 11.00000 -1.50000 AFIX 0 C15 1 0.731297 0.560488 0.469591 11.00000 0.03738 0.02921 = 0.03309 -0.00997 0.01032 -0.01211 AFIX 137 H15A 2 0.769210 0.520105 0.493311 11.00000 -1.50000 H15B 2 0.663214 0.571652 0.484347 11.00000 -1.50000 H15C 2 0.771762 0.611551 0.468942 11.00000 -1.50000 AFIX 0 C16 1 0.439907 0.348743 0.269732 11.00000 0.01534 0.02193 = 0.01197 0.00045 -0.00100 -0.00043 C17 1 0.352814 0.404102 0.266342 11.00000 0.01780 0.02072 = 0.01310 -0.00001 0.00021 0.00063 C18 1 0.252297 0.371055 0.250687 11.00000 0.01626 0.02564 = 0.01668 0.00094 -0.00042 0.00172 AFIX 43 H18 2 0.193394 0.406487 0.247627 11.00000 -1.20000 AFIX 0 C19 1 0.239259 0.286352 0.239685 11.00000 0.01835 0.02787 = 0.01864 0.00005 -0.00221 -0.00411 AFIX 43 H19 2 0.171555 0.264913 0.230422 11.00000 -1.20000 AFIX 0 C20 1 0.326898 0.233271 0.242428 11.00000 0.02500 0.02008 = 0.01884 -0.00145 -0.00172 -0.00294 AFIX 43 H20 2 0.316931 0.176465 0.234765 11.00000 -1.20000 AFIX 0 C21 1 0.429505 0.262929 0.256378 11.00000 0.02079 0.02138 = 0.01258 -0.00018 -0.00096 0.00162 C22 1 0.363831 0.497505 0.278517 11.00000 0.01909 0.01975 = 0.02287 -0.00144 -0.00041 0.00110 AFIX 13 H22 2 0.437043 0.507998 0.293619 11.00000 -1.20000 AFIX 0 C23 1 0.345158 0.548388 0.223580 11.00000 0.03105 0.02290 = 0.02962 0.00421 0.00646 0.00359 AFIX 137 H23A 2 0.393852 0.529953 0.196388 11.00000 -1.50000 H23B 2 0.356725 0.606872 0.231558 11.00000 -1.50000 H23C 2 0.273222 0.540151 0.208447 11.00000 -1.50000 AFIX 0 C24 1 0.287914 0.527555 0.322721 11.00000 0.02947 0.02358 = 0.02315 -0.00191 0.00077 0.00699 AFIX 137 H24A 2 0.215483 0.520651 0.308009 11.00000 -1.50000 H24B 2 0.301181 0.585733 0.331037 11.00000 -1.50000 H24C 2 0.299558 0.495092 0.356786 11.00000 -1.50000 AFIX 0 C25 1 0.526205 0.205416 0.255486 11.00000 0.02443 0.02213 = 0.01806 -0.00272 -0.00215 0.00483 AFIX 13 H25 2 0.571716 0.216451 0.289890 11.00000 -1.20000 AFIX 0 C26 1 0.591574 0.224547 0.204182 11.00000 0.03512 0.03957 = 0.02606 -0.00019 0.00789 0.01371 AFIX 137 H26A 2 0.549581 0.212245 0.169837 11.00000 -1.50000 H26B 2 0.654803 0.190572 0.206043 11.00000 -1.50000 H26C 2 0.611200 0.282782 0.204597 11.00000 -1.50000 AFIX 0 C27 1 0.497973 0.112099 0.254875 11.00000 0.03498 0.02315 = 0.02858 -0.00724 -0.00791 0.00609 AFIX 137 H27A 2 0.453983 0.099938 0.285667 11.00000 -1.50000 H27B 2 0.562198 0.079437 0.259002 11.00000 -1.50000 H27C 2 0.460004 0.098311 0.219572 11.00000 -1.50000 AFIX 0 C28 1 0.601939 0.316945 0.377054 11.00000 0.01603 0.01748 = 0.01432 -0.00019 -0.00056 -0.00106 C29 1 0.492498 0.287942 0.387064 11.00000 0.01778 0.02207 = 0.01074 0.00118 -0.00105 -0.00274 C30 1 0.410440 0.345080 0.395365 11.00000 0.01947 0.02443 = 0.01542 0.00198 0.00039 -0.00070 AFIX 43 H30 2 0.425443 0.402235 0.396395 11.00000 -1.20000 AFIX 0 C31 1 0.306693 0.317910 0.402114 11.00000 0.01870 0.03738 = 0.02032 0.00369 0.00219 0.00130 AFIX 43 H31 2 0.253116 0.356919 0.407341 11.00000 -1.20000 AFIX 0 C32 1 0.282909 0.233033 0.401078 11.00000 0.01925 0.04191 = 0.02405 0.00502 0.00189 -0.00941 AFIX 43 H32 2 0.213289 0.214940 0.404737 11.00000 -1.20000 AFIX 0 C33 1 0.363836 0.175206 0.394535 11.00000 0.02787 0.02835 = 0.02114 0.00333 -0.00041 -0.01091 AFIX 43 H33 2 0.348626 0.118083 0.394453 11.00000 -1.20000 AFIX 0 C34 1 0.467318 0.202293 0.388117 11.00000 0.02239 0.02245 = 0.01581 0.00100 -0.00075 -0.00321 AFIX 43 H34 2 0.521030 0.162860 0.384442 11.00000 -1.20000 AFIX 0 C35 1 0.699397 0.241737 0.479682 11.00000 0.01680 0.01603 = 0.01638 -0.00054 -0.00138 -0.00289 C36 1 0.625787 0.276857 0.523841 11.00000 0.02026 0.02193 = 0.01413 -0.00073 0.00058 0.00016 C37 1 0.688811 0.253405 0.579833 11.00000 0.02335 0.02536 = 0.01398 -0.00134 -0.00020 0.00090 AFIX 23 H37A 2 0.737814 0.298144 0.591401 11.00000 -1.20000 H37B 2 0.640355 0.244589 0.609695 11.00000 -1.20000 AFIX 0 C38 1 0.750178 0.172962 0.569061 11.00000 0.02300 0.02267 = 0.01220 0.00075 -0.00013 -0.00098 C39 1 0.613515 0.372026 0.519302 11.00000 0.03002 0.02282 = 0.02035 -0.00221 0.00083 0.00445 AFIX 137 H39A 2 0.682706 0.397816 0.521968 11.00000 -1.50000 H39B 2 0.572624 0.392005 0.549566 11.00000 -1.50000 H39C 2 0.577499 0.386076 0.483519 11.00000 -1.50000 AFIX 0 C40 1 0.514060 0.236196 0.521664 11.00000 0.02065 0.03316 = 0.01725 0.00230 0.00273 -0.00099 AFIX 137 H40A 2 0.468337 0.263966 0.493473 11.00000 -1.50000 H40B 2 0.484624 0.241467 0.558049 11.00000 -1.50000 H40C 2 0.519746 0.177871 0.512117 11.00000 -1.50000 AFIX 0 C41 1 0.854295 0.167739 0.606029 11.00000 0.02551 0.02815 = 0.01498 0.00160 -0.00187 0.00243 AFIX 137 H41A 2 0.900884 0.127536 0.590106 11.00000 -1.50000 H41B 2 0.839218 0.150625 0.643675 11.00000 -1.50000 H41C 2 0.888147 0.221777 0.607513 11.00000 -1.50000 AFIX 0 C42 1 0.687501 0.092288 0.579795 11.00000 0.03175 0.02663 = 0.01942 0.00564 0.00114 -0.00421 AFIX 137 H42A 2 0.623482 0.091311 0.555398 11.00000 -1.50000 H42B 2 0.669312 0.090791 0.618667 11.00000 -1.50000 H42C 2 0.730553 0.044364 0.572025 11.00000 -1.50000 AFIX 0 C43 1 0.844666 0.136404 0.478705 11.00000 0.02216 0.01719 = 0.01339 0.00308 -0.00019 0.00205 C44 1 0.814717 0.063021 0.448269 11.00000 0.02658 0.01770 = 0.01467 0.00271 -0.00112 -0.00009 C45 1 0.893835 0.017443 0.422990 11.00000 0.03575 0.01764 = 0.01956 -0.00089 0.00150 0.00226 AFIX 43 H45 2 0.875300 -0.031299 0.403080 11.00000 -1.20000 AFIX 0 C46 1 0.999115 0.043043 0.426847 11.00000 0.03201 0.02379 = 0.02370 0.00236 0.00788 0.00739 AFIX 43 H46 2 1.050827 0.011269 0.410184 11.00000 -1.20000 AFIX 0 C47 1 1.027183 0.115981 0.455542 11.00000 0.02323 0.02435 = 0.02419 0.00492 0.00437 0.00146 AFIX 43 H47 2 1.098043 0.133224 0.457725 11.00000 -1.20000 AFIX 0 C48 1 0.951352 0.164282 0.481307 11.00000 0.02299 0.01923 = 0.01587 0.00414 0.00036 0.00045 C49 1 0.700051 0.033424 0.439323 11.00000 0.02730 0.02006 = 0.02272 -0.00211 -0.00301 -0.00202 AFIX 13 H49 2 0.654055 0.073520 0.457651 11.00000 -1.20000 AFIX 0 C50 1 0.666914 0.031107 0.375751 11.00000 0.03815 0.02734 = 0.02685 -0.00671 -0.00990 0.00141 AFIX 137 H50A 2 0.680138 0.084861 0.359222 11.00000 -1.50000 H50B 2 0.592337 0.018077 0.370580 11.00000 -1.50000 H50C 2 0.707523 -0.011067 0.357651 11.00000 -1.50000 AFIX 0 C51 1 0.683191 -0.053606 0.464868 11.00000 0.03616 0.02401 = 0.03977 0.00212 -0.00066 -0.00781 AFIX 137 H51A 2 0.723337 -0.094426 0.445225 11.00000 -1.50000 H51B 2 0.608811 -0.067754 0.461078 11.00000 -1.50000 H51C 2 0.706862 -0.053167 0.504304 11.00000 -1.50000 AFIX 0 C52 1 0.986443 0.247091 0.508454 11.00000 0.02019 0.02087 = 0.02043 0.00173 -0.00070 -0.00143 AFIX 13 H52 2 0.928440 0.267630 0.530657 11.00000 -1.20000 AFIX 0 C53 1 1.005898 0.312029 0.462644 11.00000 0.02319 0.02249 = 0.02502 0.00417 -0.00266 -0.00318 AFIX 137 H53A 2 1.062587 0.293167 0.440336 11.00000 -1.50000 H53B 2 1.025288 0.364652 0.480191 11.00000 -1.50000 H53C 2 0.942047 0.319076 0.438618 11.00000 -1.50000 AFIX 0 C54 1 1.086299 0.237110 0.548695 11.00000 0.02610 0.02630 = 0.02469 0.00347 -0.00495 -0.00208 AFIX 137 H54A 2 1.075885 0.191759 0.574535 11.00000 -1.50000 H54B 2 1.098788 0.288125 0.569692 11.00000 -1.50000 H54C 2 1.146702 0.225203 0.527035 11.00000 -1.50000 AFIX 0 HKLF 4 REM sharma40_a.res in P2(1)/n REM wR2 = 0.0933, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0358 for 9416 Fo > 4sig(Fo) and 0.0373 for all 9876 data REM 539 parameters refined using 0 restraints END WGHT 0.0477 1.7295 REM Highest difference peak 0.267, deepest hole -0.275, 1-sigma level 0.039 Q1 1 0.6587 0.2607 0.4983 11.00000 0.05 0.27 Q2 1 0.5465 0.3013 0.3801 11.00000 0.05 0.25 Q3 1 0.7255 0.2748 0.4563 11.00000 0.05 0.24 Q4 1 0.4797 0.2380 0.2552 11.00000 0.05 0.23 Q5 1 0.8956 0.3524 0.3038 11.00000 0.05 0.23 Q6 1 0.6110 0.3377 0.3538 11.00000 0.05 0.23 Q7 1 0.5542 0.2196 0.2316 11.00000 0.05 0.23 Q8 1 0.6960 0.2558 0.4505 11.00000 0.05 0.22 Q9 1 0.9671 0.1987 0.4950 11.00000 0.05 0.22 Q10 1 0.6486 0.3009 0.3922 11.00000 0.05 0.22 Q11 1 0.3278 0.5138 0.2978 11.00000 0.05 0.22 Q12 1 0.7652 0.5070 0.3991 11.00000 0.05 0.22 Q13 1 0.8975 0.1600 0.4697 11.00000 0.05 0.21 ; _shelx_res_checksum 20090 _olex2_date_sample_data_collection 2019-06-25 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.523 _oxdiff_exptl_absorpt_empirical_full_min 0.471 ####################################################################### # # 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_compound7 _database_code_depnum_ccdc_archive 'CCDC 1949891' loop_ _audit_author_name _audit_author_address 'Hans Georg Stammler' ;University of Bielefeld Germany ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _audit_creation_date 2019-06-07 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '2(C57 H76 N3 P), C H2 Cl2, 2(Cl4 Ga)' _chemical_formula_sum 'C115 H154 Cl10 Ga2 N6 P2' _chemical_formula_weight 2176.31 _chemical_melting_point ? _chemical_oxdiff_formula 'C60 H83 Cl4 Ga N3 P' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 40.7612(6) _cell_length_b 12.3237(2) _cell_length_c 23.4798(3) _cell_angle_alpha 90 _cell_angle_beta 101.3980(10) _cell_angle_gamma 90 _cell_volume 11562.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 19995 _cell_measurement_temperature 100.00(13) _cell_measurement_theta_max 30.0650 _cell_measurement_theta_min 1.7150 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'metallic blue' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 4592 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -5 -4 0 0.0128 5 4 0 0.0128 37 -13 1 0.0210 -4 10 27 0.0888 -36 13 2 0.0755 -27 1 -25 0.0714 _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.026 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5.0689 -3.9958 0.0230 -0.1898 -0.0281 0.1555 5.0689 3.9958 -0.0230 0.1898 0.0281 -0.1555 37.1533 -13.0002 0.5563 -0.0515 0.6296 0.7752 -4.1335 10.1765 26.6734 -0.0372 0.4888 -0.8716 -36.2911 13.3985 1.6003 0.0469 -0.5702 -0.8202 -27.1027 1.3118 -25.4303 0.0778 -0.9824 0.1696 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_unetI/netI 0.0444 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.939 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 114564 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.939 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.141 _diffrn_reflns_theta_min 1.729 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(13) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0951 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.939 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 4.00 94.00 1.00 50.00 -- 26.03 77.00 -60.00 90 2 \w 6.00 81.00 1.00 50.00 -- 26.03 57.00 60.00 75 3 \w -20.00 68.00 1.00 50.00 -- 26.03 -99.00 30.00 88 4 \w 65.00 92.00 1.00 50.00 -- 26.03 57.00 -90.00 27 5 \w -4.00 40.00 1.00 50.00 -- 26.03 77.00 120.00 44 6 \w -46.00 43.00 1.00 50.00 -- 26.03 -38.00 150.00 89 7 \w -3.00 96.00 1.00 50.00 -- 26.03 77.00-150.00 99 8 \w -20.00 64.00 1.00 50.00 -- 26.03 -99.00 120.00 84 9 \w 6.00 98.00 1.00 50.00 -- 26.03 38.00-180.00 92 10 \w 31.00 68.00 1.00 50.00 -- 26.03 -99.00-120.00 37 11 \w -46.00 50.00 1.00 50.00 -- 26.03 -38.00-120.00 96 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0106635000 _diffrn_orient_matrix_UB_12 0.0338969000 _diffrn_orient_matrix_UB_13 -0.0126739000 _diffrn_orient_matrix_UB_21 0.0132270000 _diffrn_orient_matrix_UB_22 -0.0096027000 _diffrn_orient_matrix_UB_23 0.0240404000 _diffrn_orient_matrix_UB_31 0.0051517000 _diffrn_orient_matrix_UB_32 -0.0455260000 _diffrn_orient_matrix_UB_33 -0.0145084000 _diffrn_oxdiff_digest_frames ; 019ce2a469788d27ea216cb61690ebaa25008590398 ; _diffrn_oxdiff_digest_hkl ; 01d24ad9bc4e9761f5017a8e86266a2763205b ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 13305 _reflns_number_total 19086 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _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 0.897 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 770 _refine_ls_number_reflns 19086 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0517 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+16.7374P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.1194 _refine_special_details ; Two half occupied anions are disordered near symmetry elements. The second anion share the same site with a half CH2Cl2. Disorder of C39 to C50 over two sites (61:39). ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C44) = Uanis(C44B) Uanis(C43) = Uanis(C43B) Uanis(C42) = Uanis(C42B) Uanis(C41) = Uanis(C41B) 3. Others Sof(C39B)=Sof(C40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42B)=Sof(C43B)= Sof(H43B)=Sof(C44B)=Sof(C45B)=Sof(H45B)=Sof(C46B)=Sof(H46D)=Sof(H46E)= Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48B)= Sof(C49B)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C50B)=Sof(H50D)=Sof(H50E)= Sof(H50F)=1-FVAR(1) Sof(C39)=Sof(C40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)= Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)= Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49A)=Sof(H49B)= Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1) Fixed Sof: Cl9(0.5) Cl10(0.5) C58(0.5) H58A(0.5) H58B(0.5) Ga1(0.5) Cl1(0.5) Cl2(0.5) Cl3(0.5) Cl4(0.5) Ga2(0.5) Cl5(0.5) Cl6(0.5) Cl7(0.5) Cl8(0.5) 4.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C45(H45), C48(H48), C45B(H45B), C48B(H48B) 4.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A, H56B), C57(H57A,H57B), C58(H58A,H58B) 4.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C41(H41), C42(H42), C43(H43), C41B(H41B), C42B(H42B), C43B(H43B) 4.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C46B(H46D,H46E, H46F), C47B(H47D,H47E,H47F), C49B(H49D,H49E,H49F), C50B(H50D,H50E,H50F) ; _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 P1 P 0.61177(2) 0.73960(3) 0.63124(2) 0.01754(8) Uani 1 1 d . . . . . N1 N 0.57238(3) 0.83039(11) 0.50988(6) 0.0203(3) Uani 1 1 d . . . . . N2 N 0.60797(3) 0.76609(11) 0.45983(5) 0.0180(2) Uani 1 1 d . . . . . N3 N 0.63784(4) 0.70302(11) 0.74256(5) 0.0209(3) Uani 1 1 d . . . . . C1 C 0.60421(4) 0.78911(12) 0.51590(6) 0.0162(3) Uani 1 1 d . . . . . C2 C 0.55681(4) 0.83026(15) 0.45157(7) 0.0261(3) Uani 1 1 d . . . . . H2 H 0.535071 0.852977 0.436521 0.031 Uiso 1 1 calc R . . . . C3 C 0.57873(4) 0.79155(15) 0.42091(7) 0.0251(3) Uani 1 1 d . . . . . H3 H 0.574997 0.783273 0.380777 0.030 Uiso 1 1 calc R . . . . C4 C 0.55364(4) 0.87366(13) 0.55130(7) 0.0212(3) Uani 1 1 d . . . . . C5 C 0.52705(4) 0.81019(14) 0.56244(7) 0.0237(3) Uani 1 1 d . . . . . C6 C 0.50444(4) 0.86120(16) 0.59143(8) 0.0301(4) Uani 1 1 d . . . . . H6 H 0.486096 0.822578 0.598679 0.036 Uiso 1 1 calc R . . . . C7 C 0.50882(5) 0.96807(17) 0.60956(9) 0.0357(4) Uani 1 1 d . . . . . H7 H 0.493278 1.000717 0.628227 0.043 Uiso 1 1 calc R . . . . C8 C 0.53625(5) 1.02656(16) 0.60002(9) 0.0349(4) Uani 1 1 d . . . . . H8 H 0.539313 1.097337 0.613790 0.042 Uiso 1 1 calc R . . . . C9 C 0.55940(4) 0.98156(14) 0.57016(8) 0.0267(4) Uani 1 1 d . . . . . C10 C 0.52251(4) 0.69119(14) 0.54571(8) 0.0266(3) Uani 1 1 d . . . . . H10 H 0.541886 0.668473 0.529728 0.032 Uiso 1 1 calc R . . . . C11 C 0.49091(5) 0.67329(17) 0.49869(9) 0.0386(5) Uani 1 1 d . . . . . H11A H 0.471550 0.695096 0.513380 0.058 Uiso 1 1 calc GR . . . . H11B H 0.489069 0.597857 0.488340 0.058 Uiso 1 1 calc GR . . . . H11C H 0.492390 0.715721 0.465007 0.058 Uiso 1 1 calc GR . . . . C12 C 0.52132(5) 0.62040(16) 0.59917(8) 0.0347(4) Uani 1 1 d . . . . . H12A H 0.540796 0.634239 0.628667 0.052 Uiso 1 1 calc GR . . . . H12B H 0.520846 0.545222 0.588322 0.052 Uiso 1 1 calc GR . . . . H12C H 0.501583 0.637521 0.613904 0.052 Uiso 1 1 calc GR . . . . C13 C 0.58924(4) 1.04626(15) 0.55829(9) 0.0308(4) Uani 1 1 d . . . . . H13 H 0.608219 0.996191 0.561990 0.037 Uiso 1 1 calc R . . . . C14 C 0.58286(5) 1.09211(18) 0.49629(10) 0.0446(5) Uani 1 1 d . . . . . H14A H 0.578261 1.033604 0.468874 0.067 Uiso 1 1 calc GR . . . . H14B H 0.602294 1.130985 0.490261 0.067 Uiso 1 1 calc GR . . . . H14C H 0.564021 1.140429 0.490949 0.067 Uiso 1 1 calc GR . . . . C15 C 0.59948(6) 1.13789(17) 0.60249(11) 0.0441(5) Uani 1 1 d . . . . . H15A H 0.582927 1.194311 0.595779 0.066 Uiso 1 1 calc GR . . . . H15B H 0.620732 1.166823 0.598231 0.066 Uiso 1 1 calc GR . . . . H15C H 0.601198 1.109860 0.641116 0.066 Uiso 1 1 calc GR . . . . C16 C 0.63537(4) 0.71367(13) 0.43941(6) 0.0186(3) Uani 1 1 d . . . . . C17 C 0.65541(4) 0.77771(14) 0.41025(6) 0.0220(3) Uani 1 1 d . . . . . C18 C 0.68106(4) 0.72484(15) 0.38967(7) 0.0259(3) Uani 1 1 d . . . . . H18 H 0.694613 0.764238 0.369625 0.031 Uiso 1 1 calc R . . . . C19 C 0.68664(4) 0.61518(15) 0.39856(7) 0.0276(4) Uani 1 1 d . . . . . H19 H 0.704545 0.582316 0.386188 0.033 Uiso 1 1 calc R . . . . C20 C 0.66586(4) 0.55368(14) 0.42569(7) 0.0259(3) Uani 1 1 d . . . . . H20 H 0.669774 0.479618 0.430694 0.031 Uiso 1 1 calc R . . . . C21 C 0.63908(4) 0.60077(13) 0.44572(6) 0.0211(3) Uani 1 1 d . . . . . C22 C 0.64954(5) 0.89825(15) 0.39887(8) 0.0300(4) Uani 1 1 d . . . . . H22 H 0.635404 0.925239 0.425050 0.036 Uiso 1 1 calc R . . . . C23 C 0.63062(6) 0.9148(2) 0.33580(10) 0.0482(6) Uani 1 1 d . . . . . H23A H 0.644606 0.892656 0.309449 0.072 Uiso 1 1 calc GR . . . . H23B H 0.624945 0.990084 0.329600 0.072 Uiso 1 1 calc GR . . . . H23C H 0.610543 0.872057 0.329078 0.072 Uiso 1 1 calc GR . . . . C24 C 0.68187(5) 0.96548(16) 0.40898(8) 0.0346(4) Uani 1 1 d . . . . . H24A H 0.694923 0.949354 0.446729 0.052 Uiso 1 1 calc GR . . . . H24B H 0.676385 1.041312 0.406709 0.052 Uiso 1 1 calc GR . . . . H24C H 0.694531 0.947805 0.379836 0.052 Uiso 1 1 calc GR . . . . C25 C 0.61474(4) 0.53162(14) 0.47198(7) 0.0265(3) Uani 1 1 d . . . . . H25 H 0.609008 0.571670 0.504728 0.032 Uiso 1 1 calc R . . . . C26 C 0.58235(5) 0.51241(19) 0.42706(10) 0.0458(5) Uani 1 1 d . . . . . H26A H 0.567316 0.468693 0.444059 0.069 Uiso 1 1 calc GR . . . . H26B H 0.587512 0.475664 0.393864 0.069 Uiso 1 1 calc GR . . . . H26C H 0.571974 0.580861 0.415179 0.069 Uiso 1 1 calc GR . . . . C27 C 0.62925(6) 0.42182(15) 0.49451(8) 0.0347(4) Uani 1 1 d . . . . . H27A H 0.632343 0.377515 0.462353 0.052 Uiso 1 1 calc GR . . . . H27B H 0.614102 0.386365 0.515024 0.052 Uiso 1 1 calc GR . . . . H27C H 0.650406 0.432614 0.520287 0.052 Uiso 1 1 calc GR . . . . C28 C 0.62785(4) 0.76918(12) 0.56868(6) 0.0155(3) Uani 1 1 d . . . . . C29 C 0.66335(4) 0.75221(14) 0.56472(6) 0.0195(3) Uani 1 1 d . . . . . C30 C 0.68237(4) 0.83578(16) 0.54726(7) 0.0262(4) Uani 1 1 d . . . . . H30 H 0.672498 0.902618 0.536410 0.031 Uiso 1 1 calc R . . . . C31 C 0.71611(4) 0.8194(2) 0.54602(7) 0.0367(5) Uani 1 1 d . . . . . H31 H 0.728832 0.875917 0.535603 0.044 Uiso 1 1 calc R . . . . C32 C 0.73062(5) 0.7190(2) 0.56029(8) 0.0418(6) Uani 1 1 d . . . . . H32 H 0.753017 0.707991 0.558864 0.050 Uiso 1 1 calc R . . . . C33 C 0.71202(5) 0.63478(19) 0.57668(8) 0.0379(5) Uani 1 1 d . . . . . H33 H 0.721812 0.567167 0.585655 0.045 Uiso 1 1 calc R . . . . C34 C 0.67860(4) 0.65140(15) 0.57973(7) 0.0261(4) Uani 1 1 d . . . . . H34 H 0.666319 0.595284 0.591793 0.031 Uiso 1 1 calc R . . . . C35 C 0.64372(4) 0.75490(12) 0.69501(6) 0.0167(3) Uani 1 1 d . . . . . C36 C 0.66461(4) 0.72203(13) 0.79609(6) 0.0224(3) Uani 1 1 d . . . . . C37 C 0.67795(4) 0.83151(14) 0.78073(6) 0.0220(3) Uani 1 1 d . . . . . H37A H 0.701433 0.838846 0.798537 0.026 Uiso 1 1 calc R . . . . H37B H 0.665634 0.890114 0.794420 0.026 Uiso 1 1 calc R . . . . C38 C 0.67326(4) 0.83508(13) 0.71337(6) 0.0196(3) Uani 1 1 d . . . . . C51 C 0.69002(5) 0.62927(16) 0.80178(8) 0.0356(4) Uani 1 1 d . . . . . H51A H 0.679690 0.563268 0.811000 0.053 Uiso 1 1 calc GR . . . . H51B H 0.708813 0.645803 0.832170 0.053 Uiso 1 1 calc GR . . . . H51C H 0.697479 0.620560 0.765750 0.053 Uiso 1 1 calc GR . . . . C52 C 0.65091(5) 0.72617(15) 0.85242(7) 0.0275(4) Uani 1 1 d . . . . . H52A H 0.636237 0.787400 0.851302 0.041 Uiso 1 1 calc GR . . . . H52B H 0.669165 0.733007 0.885019 0.041 Uiso 1 1 calc GR . . . . H52C H 0.638758 0.660684 0.856171 0.041 Uiso 1 1 calc GR . . . . C53 C 0.66147(4) 0.94859(13) 0.68945(7) 0.0251(3) Uani 1 1 d . . . . . H53A H 0.655850 0.945398 0.647364 0.030 Uiso 1 1 calc R . . . . H53B H 0.641362 0.968270 0.703275 0.030 Uiso 1 1 calc R . . . . C54 C 0.68804(5) 1.03630(16) 0.70780(8) 0.0368(5) Uani 1 1 d . . . . . H54A H 0.679779 1.105209 0.690776 0.044 Uiso 1 1 calc R . . . . H54B H 0.692404 1.044138 0.749724 0.044 Uiso 1 1 calc R . . . . C55 C 0.72035(5) 1.00705(19) 0.68824(9) 0.0440(5) Uani 1 1 d . . . . . H55A H 0.737160 1.061852 0.701822 0.053 Uiso 1 1 calc R . . . . H55B H 0.716425 1.005777 0.646131 0.053 Uiso 1 1 calc R . . . . C56 C 0.73314(5) 0.89673(19) 0.71190(8) 0.0376(5) Uani 1 1 d . . . . . H56A H 0.739442 0.900708 0.753905 0.045 Uiso 1 1 calc R . . . . H56B H 0.752973 0.878151 0.696967 0.045 Uiso 1 1 calc R . . . . C57 C 0.70664(4) 0.80686(16) 0.69501(7) 0.0257(3) Uani 1 1 d . . . . . H57A H 0.715218 0.739369 0.713405 0.031 Uiso 1 1 calc R . . . . H57B H 0.702580 0.796117 0.653284 0.031 Uiso 1 1 calc R . . . . C39 C 0.60608(16) 0.6432(6) 0.7441(4) 0.0216(11) Uani 0.614(3) 1 d . . P A 1 C40 C 0.60418(11) 0.5328(3) 0.73049(16) 0.0278(7) Uani 0.614(3) 1 d . . P A 1 C41 C 0.57545(12) 0.4764(3) 0.73841(17) 0.0453(10) Uani 0.614(3) 1 d . . P A 1 H41 H 0.573541 0.402816 0.729589 0.054 Uiso 0.614(3) 1 calc R . P A 1 C42 C 0.54982(11) 0.5279(4) 0.75909(17) 0.0501(10) Uani 0.614(3) 1 d . . P A 1 H42 H 0.531316 0.488659 0.765079 0.060 Uiso 0.614(3) 1 calc R . P A 1 C43 C 0.55199(9) 0.6374(4) 0.77066(15) 0.0405(8) Uani 0.614(3) 1 d . . P A 1 H43 H 0.534427 0.671730 0.783352 0.049 Uiso 0.614(3) 1 calc R . P A 1 C44 C 0.57989(10) 0.6985(4) 0.76387(16) 0.0247(7) Uani 0.614(3) 1 d . . P A 1 C45 C 0.63000(12) 0.4723(3) 0.70468(15) 0.0317(8) Uani 0.614(3) 1 d . . P A 1 H45 H 0.648820 0.521210 0.703620 0.038 Uiso 0.614(3) 1 calc R . P A 1 C46 C 0.61494(13) 0.4365(3) 0.64194(16) 0.0417(10) Uani 0.614(3) 1 d . . P A 1 H46A H 0.596970 0.386327 0.642416 0.063 Uiso 0.614(3) 1 calc GR . P A 1 H46B H 0.631928 0.401988 0.625235 0.063 Uiso 0.614(3) 1 calc GR . P A 1 H46C H 0.606546 0.498858 0.619173 0.063 Uiso 0.614(3) 1 calc GR . P A 1 C47 C 0.64333(14) 0.3716(3) 0.74097(16) 0.0509(11) Uani 0.614(3) 1 d . . P A 1 H47A H 0.649598 0.391568 0.781172 0.076 Uiso 0.614(3) 1 calc GR . P A 1 H47B H 0.662509 0.343479 0.727826 0.076 Uiso 0.614(3) 1 calc GR . P A 1 H47C H 0.626193 0.317080 0.736495 0.076 Uiso 0.614(3) 1 calc GR . P A 1 C48 C 0.57924(13) 0.8198(4) 0.7726(2) 0.0281(9) Uani 0.614(3) 1 d . . P A 1 H48 H 0.601836 0.847898 0.773567 0.034 Uiso 0.614(3) 1 calc R . P A 1 C49 C 0.55547(13) 0.8727(4) 0.7212(2) 0.0431(11) Uani 0.614(3) 1 d . . P A 1 H49A H 0.561424 0.849952 0.685466 0.065 Uiso 0.614(3) 1 calc GR . P A 1 H49B H 0.557254 0.950215 0.724510 0.065 Uiso 0.614(3) 1 calc GR . P A 1 H49C H 0.532886 0.851040 0.721490 0.065 Uiso 0.614(3) 1 calc GR . P A 1 C50 C 0.56839(13) 0.8533(4) 0.8299(2) 0.0446(10) Uani 0.614(3) 1 d . . P A 1 H50A H 0.545214 0.835694 0.827427 0.067 Uiso 0.614(3) 1 calc GR . P A 1 H50B H 0.571533 0.930022 0.835715 0.067 Uiso 0.614(3) 1 calc GR . P A 1 H50C H 0.581717 0.815022 0.861886 0.067 Uiso 0.614(3) 1 calc GR . P A 1 C39B C 0.6146(3) 0.6196(10) 0.7457(6) 0.0251(19) Uani 0.386(3) 1 d . . P A 2 C40B C 0.61918(17) 0.5091(5) 0.7301(2) 0.0256(11) Uani 0.386(3) 1 d . . P A 2 C41B C 0.59476(18) 0.4361(5) 0.7383(3) 0.0453(10) Uani 0.386(3) 1 d . . P A 2 H41B H 0.597011 0.363222 0.729453 0.054 Uiso 0.386(3) 1 calc R . P A 2 C42B C 0.56699(19) 0.4698(7) 0.7594(3) 0.0501(10) Uani 0.386(3) 1 d . . P A 2 H42B H 0.551284 0.418427 0.765339 0.060 Uiso 0.386(3) 1 calc R . P A 2 C43B C 0.56203(16) 0.5751(6) 0.7716(3) 0.0405(8) Uani 0.386(3) 1 d . . P A 2 H43B H 0.542818 0.595444 0.784662 0.049 Uiso 0.386(3) 1 calc R . P A 2 C44B C 0.58583(17) 0.6539(5) 0.7646(3) 0.0247(7) Uani 0.386(3) 1 d . . P A 2 C45B C 0.64769(16) 0.4709(4) 0.7029(2) 0.0256(11) Uani 0.386(3) 1 d . . P A 2 H45B H 0.663008 0.531785 0.701599 0.031 Uiso 0.386(3) 1 calc R . P A 2 C46B C 0.63385(18) 0.4317(5) 0.6401(3) 0.0348(13) Uani 0.386(3) 1 d . . P A 2 H46D H 0.618260 0.373608 0.640901 0.052 Uiso 0.386(3) 1 calc GR . P A 2 H46E H 0.651992 0.406450 0.623057 0.052 Uiso 0.386(3) 1 calc GR . P A 2 H46F H 0.622728 0.490741 0.617527 0.052 Uiso 0.386(3) 1 calc GR . P A 2 C47B C 0.6674(2) 0.3764(5) 0.7368(2) 0.0435(16) Uani 0.386(3) 1 d . . P A 2 H47D H 0.673818 0.395673 0.777078 0.065 Uiso 0.386(3) 1 calc GR . P A 2 H47E H 0.687070 0.361908 0.721332 0.065 Uiso 0.386(3) 1 calc GR . P A 2 H47F H 0.653564 0.312706 0.733068 0.065 Uiso 0.386(3) 1 calc GR . P A 2 C48B C 0.57829(18) 0.7712(7) 0.7749(3) 0.0290(15) Uani 0.386(3) 1 d . . P A 2 H48B H 0.598776 0.812979 0.775258 0.035 Uiso 0.386(3) 1 calc R . P A 2 C49B C 0.5511(2) 0.8160(7) 0.7259(3) 0.0478(19) Uani 0.386(3) 1 d . . P A 2 H49D H 0.558900 0.814000 0.689970 0.072 Uiso 0.386(3) 1 calc GR . P A 2 H49E H 0.546059 0.889585 0.734621 0.072 Uiso 0.386(3) 1 calc GR . P A 2 H49F H 0.531235 0.772566 0.722532 0.072 Uiso 0.386(3) 1 calc GR . P A 2 C50B C 0.56705(18) 0.7923(7) 0.8336(3) 0.0413(15) Uani 0.386(3) 1 d . . P A 2 H50D H 0.545043 0.762962 0.831766 0.062 Uiso 0.386(3) 1 calc GR . P A 2 H50E H 0.566712 0.868971 0.840624 0.062 Uiso 0.386(3) 1 calc GR . P A 2 H50F H 0.582450 0.757924 0.864556 0.062 Uiso 0.386(3) 1 calc GR . P A 2 Cl9 Cl 0.67905(7) 0.1646(2) 0.54557(9) 0.0682(6) Uani 0.5 1 d . . P B -2 Cl10 Cl 0.70460(5) 0.31877(13) 0.63627(6) 0.0719(4) Uani 0.5 1 d . . P B -2 C58 C 0.71249(14) 0.2471(5) 0.5785(2) 0.0646(16) Uani 0.5 1 d . . P B -2 H58A H 0.732029 0.201845 0.591376 0.077 Uiso 0.5 1 calc R . P B -2 H58B H 0.717728 0.297437 0.549839 0.077 Uiso 0.5 1 calc R . P B -2 Ga1 Ga 0.49542(2) 0.77341(3) 0.25889(3) 0.03242(15) Uani 0.5 1 d . . P C -1 Cl1 Cl 0.44438(3) 0.83051(10) 0.24946(6) 0.0530(3) Uani 0.5 1 d . . P C -1 Cl2 Cl 0.50445(4) 0.66131(14) 0.33176(7) 0.0397(3) Uani 0.5 1 d . . P C -1 Cl3 Cl 0.53219(3) 0.90318(10) 0.27926(5) 0.0521(3) Uani 0.5 1 d . . P C -1 Cl4 Cl 0.50079(5) 0.70147(13) 0.17655(7) 0.0442(4) Uani 0.5 1 d . . P C -1 Ga2 Ga 0.72201(2) 0.23942(3) 0.54560(2) 0.02781(9) Uani 0.5 1 d . . P D -1 Cl5 Cl 0.67354(4) 0.16287(18) 0.52279(7) 0.0433(4) Uani 0.5 1 d . . P D -1 Cl6 Cl 0.72899(4) 0.31054(12) 0.63136(5) 0.0574(4) Uani 0.5 1 d . . P D -1 Cl7 Cl 0.76009(3) 0.11618(8) 0.54163(5) 0.0354(2) Uani 0.5 1 d . . P D -1 Cl8 Cl 0.72676(3) 0.36756(9) 0.48341(6) 0.0462(3) Uani 0.5 1 d . . P D -1 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 P1 0.01651(17) 0.02174(19) 0.01453(16) -0.00026(14) 0.00348(13) -0.00144(15) N1 0.0169(6) 0.0231(7) 0.0201(6) 0.0027(5) 0.0019(5) 0.0042(5) N2 0.0164(6) 0.0236(6) 0.0132(5) 0.0021(5) 0.0011(4) 0.0017(5) N3 0.0285(7) 0.0211(6) 0.0132(6) -0.0018(5) 0.0038(5) -0.0061(5) C1 0.0136(6) 0.0176(7) 0.0167(6) 0.0006(5) 0.0016(5) 0.0011(5) C2 0.0180(7) 0.0343(9) 0.0231(8) 0.0051(7) -0.0032(6) 0.0059(7) C3 0.0202(8) 0.0367(9) 0.0158(7) 0.0044(6) -0.0032(6) 0.0026(7) C4 0.0149(7) 0.0230(8) 0.0252(8) -0.0013(6) 0.0028(6) 0.0063(6) C5 0.0168(7) 0.0282(8) 0.0255(8) -0.0004(7) 0.0025(6) 0.0028(6) C6 0.0195(8) 0.0390(10) 0.0326(9) -0.0020(8) 0.0071(7) 0.0040(7) C7 0.0249(9) 0.0404(11) 0.0426(11) -0.0068(9) 0.0089(8) 0.0133(8) C8 0.0299(9) 0.0269(9) 0.0462(11) -0.0095(8) 0.0038(8) 0.0102(8) C9 0.0210(8) 0.0222(8) 0.0347(9) -0.0011(7) 0.0005(7) 0.0059(6) C10 0.0246(8) 0.0262(8) 0.0295(9) -0.0015(7) 0.0063(7) -0.0011(7) C11 0.0398(11) 0.0347(10) 0.0366(10) -0.0017(8) -0.0042(8) -0.0062(9) C12 0.0362(10) 0.0330(10) 0.0340(10) 0.0027(8) 0.0048(8) -0.0073(8) C13 0.0223(8) 0.0230(8) 0.0443(11) 0.0001(8) -0.0003(7) 0.0014(7) C14 0.0354(11) 0.0389(11) 0.0541(13) 0.0144(10) -0.0046(9) -0.0095(9) C15 0.0380(11) 0.0271(10) 0.0627(14) -0.0079(10) -0.0010(10) -0.0011(8) C16 0.0166(7) 0.0266(8) 0.0117(6) -0.0004(5) 0.0005(5) 0.0026(6) C17 0.0240(8) 0.0287(8) 0.0129(6) 0.0011(6) 0.0021(6) 0.0002(6) C18 0.0233(8) 0.0378(10) 0.0172(7) -0.0024(7) 0.0052(6) -0.0026(7) C19 0.0240(8) 0.0376(10) 0.0207(8) -0.0098(7) 0.0034(6) 0.0020(7) C20 0.0291(9) 0.0253(8) 0.0223(8) -0.0070(6) 0.0021(6) 0.0031(7) C21 0.0237(8) 0.0250(8) 0.0126(6) -0.0031(6) -0.0008(6) -0.0006(6) C22 0.0332(9) 0.0306(9) 0.0276(9) 0.0093(7) 0.0095(7) 0.0016(7) C23 0.0440(12) 0.0519(13) 0.0442(12) 0.0276(11) -0.0026(10) -0.0056(10) C24 0.0439(11) 0.0323(10) 0.0280(9) 0.0068(8) 0.0083(8) -0.0061(8) C25 0.0322(9) 0.0238(8) 0.0238(8) -0.0019(6) 0.0065(7) -0.0045(7) C26 0.0388(11) 0.0416(12) 0.0523(13) 0.0052(10) -0.0022(10) -0.0174(10) C27 0.0564(13) 0.0253(9) 0.0241(8) -0.0037(7) 0.0118(8) -0.0032(9) C28 0.0152(6) 0.0173(7) 0.0137(6) 0.0004(5) 0.0022(5) 0.0030(5) C29 0.0151(7) 0.0304(8) 0.0119(6) -0.0040(6) 0.0004(5) 0.0033(6) C30 0.0205(8) 0.0444(10) 0.0134(7) 0.0019(7) 0.0031(6) -0.0010(7) C31 0.0212(8) 0.0736(15) 0.0159(7) 0.0006(8) 0.0051(6) -0.0070(9) C32 0.0170(8) 0.0885(17) 0.0196(8) -0.0101(9) 0.0029(6) 0.0099(10) C33 0.0264(9) 0.0557(13) 0.0281(9) -0.0155(9) -0.0031(7) 0.0196(9) C34 0.0217(8) 0.0328(9) 0.0209(7) -0.0077(7) -0.0024(6) 0.0098(7) C35 0.0199(7) 0.0169(7) 0.0139(6) -0.0008(5) 0.0049(5) 0.0011(5) C36 0.0295(8) 0.0249(8) 0.0117(6) -0.0015(6) 0.0017(6) -0.0013(6) C37 0.0234(8) 0.0276(8) 0.0146(7) -0.0032(6) 0.0032(6) -0.0041(6) C38 0.0216(7) 0.0238(8) 0.0132(6) -0.0021(6) 0.0034(5) -0.0040(6) C51 0.0465(12) 0.0343(10) 0.0248(9) 0.0044(7) 0.0041(8) 0.0107(9) C52 0.0340(9) 0.0353(10) 0.0134(7) 0.0016(6) 0.0050(6) -0.0054(7) C53 0.0323(9) 0.0216(8) 0.0211(7) -0.0014(6) 0.0044(6) -0.0059(7) C54 0.0517(12) 0.0299(10) 0.0277(9) -0.0030(7) 0.0055(8) -0.0181(9) C55 0.0459(12) 0.0554(13) 0.0299(10) -0.0005(9) 0.0054(9) -0.0327(11) C56 0.0252(9) 0.0667(14) 0.0210(8) -0.0051(9) 0.0045(7) -0.0177(9) C57 0.0195(8) 0.0421(10) 0.0154(7) -0.0021(7) 0.0029(6) -0.0027(7) C39 0.027(3) 0.024(3) 0.0134(15) 0.0038(18) 0.002(2) -0.0079(19) C40 0.041(2) 0.0229(18) 0.0175(14) 0.0022(12) 0.0000(16) -0.0045(16) C41 0.068(3) 0.033(2) 0.0325(14) 0.0010(15) 0.006(2) -0.0259(16) C42 0.046(2) 0.064(3) 0.0391(16) 0.0051(19) 0.0071(17) -0.0326(17) C43 0.0336(18) 0.058(2) 0.0307(12) 0.0044(18) 0.0092(13) -0.0172(16) C44 0.0267(17) 0.030(2) 0.0182(9) 0.0002(19) 0.0062(11) -0.0045(17) C45 0.050(2) 0.0215(15) 0.0206(16) 0.0005(12) -0.0012(18) 0.0005(18) C46 0.072(3) 0.0255(17) 0.0226(16) -0.0045(12) -0.002(2) 0.000(2) C47 0.087(3) 0.0289(18) 0.0291(17) 0.0004(14) -0.007(2) 0.013(2) C48 0.0294(17) 0.036(2) 0.0222(16) -0.004(2) 0.0131(12) 0.001(2) C49 0.049(3) 0.052(3) 0.0313(19) 0.002(2) 0.0151(16) 0.019(2) C50 0.048(2) 0.059(3) 0.0321(19) -0.011(2) 0.0212(16) 0.001(2) C39B 0.025(5) 0.035(6) 0.014(2) 0.003(3) 0.000(3) -0.004(3) C40B 0.039(3) 0.020(3) 0.018(2) -0.003(2) 0.006(3) -0.004(2) C41B 0.068(3) 0.033(2) 0.0325(14) 0.0010(15) 0.006(2) -0.0259(16) C42B 0.046(2) 0.064(3) 0.0391(16) 0.0051(19) 0.0071(17) -0.0326(17) C43B 0.0336(18) 0.058(2) 0.0307(12) 0.0044(18) 0.0092(13) -0.0172(16) C44B 0.0267(17) 0.030(2) 0.0182(9) 0.0002(19) 0.0062(11) -0.0045(17) C45B 0.040(3) 0.020(2) 0.016(2) -0.0037(16) 0.006(2) -0.001(2) C46B 0.056(4) 0.024(3) 0.022(2) -0.0021(18) 0.003(3) 0.004(3) C47B 0.081(5) 0.026(3) 0.019(2) 0.0031(19) -0.001(3) 0.016(3) C48B 0.022(2) 0.047(5) 0.020(2) 0.002(4) 0.0077(18) 0.003(4) C49B 0.037(4) 0.075(6) 0.032(3) -0.001(4) 0.010(3) 0.024(4) C50B 0.036(3) 0.062(4) 0.029(3) -0.013(3) 0.015(2) 0.005(4) Cl9 0.0684(13) 0.0590(10) 0.0692(14) -0.0013(12) -0.0058(10) -0.0022(8) Cl10 0.1105(14) 0.0602(9) 0.0454(7) -0.0016(6) 0.0160(8) -0.0024(9) C58 0.060(3) 0.090(4) 0.054(3) -0.009(3) 0.036(3) -0.001(3) Ga1 0.0294(4) 0.0371(2) 0.0255(4) -0.00626(18) -0.0076(2) 0.0084(2) Cl1 0.0363(5) 0.0464(6) 0.0652(7) -0.0130(5) -0.0167(5) 0.0148(5) Cl2 0.0354(6) 0.0596(11) 0.0213(6) 0.0036(6) -0.0012(4) 0.0068(7) Cl3 0.0513(7) 0.0542(7) 0.0443(6) -0.0102(5) -0.0064(5) -0.0103(5) Cl4 0.0660(11) 0.0426(9) 0.0203(6) -0.0018(6) -0.0006(6) 0.0055(7) Ga2 0.02420(19) 0.0324(2) 0.02407(19) -0.00413(16) -0.00204(15) 0.00827(16) Cl5 0.0299(7) 0.0437(7) 0.0547(10) -0.0071(8) 0.0047(7) 0.0032(5) Cl6 0.0567(7) 0.0728(9) 0.0358(6) -0.0264(6) -0.0078(5) 0.0196(7) Cl7 0.0321(5) 0.0362(5) 0.0376(5) 0.0060(4) 0.0061(4) 0.0146(4) Cl8 0.0412(6) 0.0412(6) 0.0572(7) 0.0158(5) 0.0119(5) 0.0177(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C28 1.7608(15) . ? P1 C35 1.7896(15) . ? N1 C1 1.3747(19) . ? N1 C2 1.390(2) . ? N1 C4 1.452(2) . ? N2 C1 1.3845(19) . ? N2 C3 1.3869(19) . ? N2 C16 1.451(2) . ? N3 C35 1.3486(19) . ? N3 C36 1.511(2) . ? N3 C39 1.496(8) . ? N3 C39B 1.410(15) . ? C1 C28 1.4325(19) . ? C2 H2 0.9300 . ? C2 C3 1.341(2) . ? C3 H3 0.9300 . ? C4 C5 1.402(2) . ? C4 C9 1.407(2) . ? C5 C6 1.399(2) . ? C5 C10 1.520(2) . ? C6 H6 0.9300 . ? C6 C7 1.385(3) . ? C7 H7 0.9300 . ? C7 C8 1.385(3) . ? C8 H8 0.9300 . ? C8 C9 1.397(2) . ? C9 C13 1.525(3) . ? C10 H10 0.9800 . ? C10 C11 1.537(3) . ? C10 C12 1.537(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.535(3) . ? C13 C15 1.535(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.407(2) . ? C16 C21 1.404(2) . ? C17 C18 1.397(2) . ? C17 C22 1.520(2) . ? C18 H18 0.9300 . ? C18 C19 1.379(3) . ? C19 H19 0.9300 . ? C19 C20 1.382(3) . ? C20 H20 0.9300 . ? C20 C21 1.397(2) . ? C21 C25 1.527(2) . ? C22 H22 0.9800 . ? C22 C23 1.542(3) . ? C22 C24 1.535(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.537(3) . ? C25 C27 1.529(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.483(2) . ? C29 C30 1.399(2) . ? C29 C34 1.403(2) . ? C30 H30 0.9300 . ? C30 C31 1.396(2) . ? C31 H31 0.9300 . ? C31 C32 1.384(3) . ? C32 H32 0.9300 . ? C32 C33 1.384(3) . ? C33 H33 0.9300 . ? C33 C34 1.393(2) . ? C34 H34 0.9300 . ? C35 C38 1.551(2) . ? C36 C37 1.524(2) . ? C36 C51 1.531(2) . ? C36 C52 1.535(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.556(2) . ? C38 C53 1.548(2) . ? C38 C57 1.546(2) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 C54 1.531(2) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 C55 1.521(3) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C55 C56 1.521(3) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 C57 1.543(3) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C39 C40 1.397(8) . ? C39 C44 1.419(7) . ? C40 C41 1.405(6) . ? C40 C45 1.511(5) . ? C41 H41 0.9300 . ? C41 C42 1.390(7) . ? C42 H42 0.9300 . ? C42 C43 1.375(6) . ? C43 H43 0.9300 . ? C43 C44 1.399(5) . ? C44 C48 1.510(5) . ? C45 H45 0.9800 . ? C45 C46 1.544(5) . ? C45 C47 1.542(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48 0.9800 . ? C48 C49 1.536(7) . ? C48 C50 1.553(6) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C39B C40B 1.432(13) . ? C39B C44B 1.398(11) . ? C40B C41B 1.383(8) . ? C40B C45B 1.508(8) . ? C41B H41B 0.9300 . ? C41B C42B 1.386(11) . ? C42B H42B 0.9300 . ? C42B C43B 1.354(11) . ? C43B H43B 0.9300 . ? C43B C44B 1.405(9) . ? C44B C48B 1.507(8) . ? C45B H45B 0.9800 . ? C45B C46B 1.548(8) . ? C45B C47B 1.544(8) . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? C47B H47D 0.9600 . ? C47B H47E 0.9600 . ? C47B H47F 0.9600 . ? C48B H48B 0.9800 . ? C48B C49B 1.535(10) . ? C48B C50B 1.557(9) . ? C49B H49D 0.9600 . ? C49B H49E 0.9600 . ? C49B H49F 0.9600 . ? C50B H50D 0.9600 . ? C50B H50E 0.9600 . ? C50B H50F 0.9600 . ? Cl9 C58 1.753(6) . ? Cl10 C58 1.702(5) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? Ga1 Cl1 2.1657(13) . ? Ga1 Cl2 2.1731(15) . ? Ga1 Cl3 2.1792(13) . ? Ga1 Cl4 2.1767(17) . ? Ga2 Cl5 2.159(2) . ? Ga2 Cl6 2.1628(11) . ? Ga2 Cl7 2.1867(10) . ? Ga2 Cl8 2.1852(13) . ? 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 C28 P1 C35 110.29(7) . . ? C1 N1 C2 109.80(13) . . ? C1 N1 C4 132.69(13) . . ? C2 N1 C4 117.50(13) . . ? C1 N2 C3 109.76(13) . . ? C1 N2 C16 129.97(12) . . ? C3 N2 C16 120.01(13) . . ? C35 N3 C36 113.44(13) . . ? C35 N3 C39 123.4(3) . . ? C35 N3 C39B 128.3(6) . . ? C39 N3 C36 122.8(3) . . ? C39B N3 C36 116.9(5) . . ? N1 C1 N2 104.92(12) . . ? N1 C1 C28 127.74(13) . . ? N2 C1 C28 127.27(13) . . ? N1 C2 H2 126.1 . . ? C3 C2 N1 107.83(14) . . ? C3 C2 H2 126.1 . . ? N2 C3 H3 126.2 . . ? C2 C3 N2 107.68(14) . . ? C2 C3 H3 126.2 . . ? C5 C4 N1 116.65(14) . . ? C5 C4 C9 123.76(15) . . ? C9 C4 N1 118.74(15) . . ? C4 C5 C10 123.31(15) . . ? C6 C5 C4 116.62(16) . . ? C6 C5 C10 120.07(16) . . ? C5 C6 H6 119.3 . . ? C7 C6 C5 121.32(17) . . ? C7 C6 H6 119.3 . . ? C6 C7 H7 119.9 . . ? C6 C7 C8 120.29(17) . . ? C8 C7 H7 119.9 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.43(17) . . ? C9 C8 H8 119.3 . . ? C4 C9 C13 121.75(15) . . ? C8 C9 C4 116.49(17) . . ? C8 C9 C13 121.76(16) . . ? C5 C10 H10 108.0 . . ? C5 C10 C11 111.48(15) . . ? C5 C10 C12 111.00(15) . . ? C11 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C12 C10 C11 110.35(15) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.4 . . ? C9 C13 C14 111.96(15) . . ? C9 C13 C15 112.41(17) . . ? C14 C13 H13 107.4 . . ? C15 C13 H13 107.4 . . ? C15 C13 C14 110.05(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 118.02(14) . . ? C21 C16 N2 118.69(14) . . ? C21 C16 C17 123.12(15) . . ? C16 C17 C22 123.19(15) . . ? C18 C17 C16 116.93(16) . . ? C18 C17 C22 119.85(15) . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.12(16) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.7 . . ? C18 C19 C20 120.62(16) . . ? C20 C19 H19 119.7 . . ? C19 C20 H20 119.4 . . ? C19 C20 C21 121.19(16) . . ? C21 C20 H20 119.4 . . ? C16 C21 C25 122.04(15) . . ? C20 C21 C16 116.81(15) . . ? C20 C21 C25 121.14(15) . . ? C17 C22 H22 108.2 . . ? C17 C22 C23 109.25(16) . . ? C17 C22 C24 113.56(15) . . ? C23 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C24 C22 C23 109.16(15) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 108.1 . . ? C21 C25 C26 110.33(15) . . ? C21 C25 C27 113.32(15) . . ? C26 C25 H25 108.1 . . ? C27 C25 H25 108.1 . . ? C27 C25 C26 108.80(16) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 C28 P1 117.36(11) . . ? C1 C28 C29 117.88(12) . . ? C29 C28 P1 123.48(11) . . ? C30 C29 C28 121.26(15) . . ? C30 C29 C34 118.82(15) . . ? C34 C29 C28 119.91(15) . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.33(18) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 120.02(19) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.40(17) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 119.95(19) . . ? C34 C33 H33 120.0 . . ? C29 C34 H34 119.8 . . ? C33 C34 C29 120.43(19) . . ? C33 C34 H34 119.8 . . ? N3 C35 P1 115.06(11) . . ? N3 C35 C38 109.09(12) . . ? C38 C35 P1 134.12(11) . . ? N3 C36 C37 99.97(12) . . ? N3 C36 C51 108.78(13) . . ? N3 C36 C52 113.33(14) . . ? C37 C36 C51 114.51(15) . . ? C37 C36 C52 112.46(13) . . ? C51 C36 C52 107.74(14) . . ? C36 C37 H37A 110.4 . . ? C36 C37 H37B 110.4 . . ? C36 C37 C38 106.71(12) . . ? H37A C37 H37B 108.6 . . ? C38 C37 H37A 110.4 . . ? C38 C37 H37B 110.4 . . ? C35 C38 C37 101.38(12) . . ? C53 C38 C35 107.84(13) . . ? C53 C38 C37 111.18(13) . . ? C57 C38 C35 117.18(13) . . ? C57 C38 C37 109.81(13) . . ? C57 C38 C53 109.23(13) . . ? C36 C51 H51A 109.5 . . ? C36 C51 H51B 109.5 . . ? C36 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C36 C52 H52A 109.5 . . ? C36 C52 H52B 109.5 . . ? C36 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C38 C53 H53A 109.1 . . ? C38 C53 H53B 109.1 . . ? H53A C53 H53B 107.8 . . ? C54 C53 C38 112.60(15) . . ? C54 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? C55 C54 C53 110.75(16) . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? C54 C55 C56 110.87(16) . . ? H55A C55 H55B 108.1 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? C55 C56 H56A 109.2 . . ? C55 C56 H56B 109.2 . . ? C55 C56 C57 112.06(16) . . ? H56A C56 H56B 107.9 . . ? C57 C56 H56A 109.2 . . ? C57 C56 H56B 109.2 . . ? C38 C57 H57A 109.2 . . ? C38 C57 H57B 109.2 . . ? C56 C57 C38 112.14(15) . . ? C56 C57 H57A 109.2 . . ? C56 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C40 C39 N3 118.9(4) . . ? C40 C39 C44 122.1(6) . . ? C44 C39 N3 118.8(6) . . ? C39 C40 C41 117.5(5) . . ? C39 C40 C45 124.1(4) . . ? C41 C40 C45 118.3(4) . . ? C40 C41 H41 119.2 . . ? C42 C41 C40 121.6(4) . . ? C42 C41 H41 119.2 . . ? C41 C42 H42 120.2 . . ? C43 C42 C41 119.6(4) . . ? C43 C42 H42 120.2 . . ? C42 C43 H43 119.1 . . ? C42 C43 C44 121.8(4) . . ? C44 C43 H43 119.1 . . ? C39 C44 C48 123.6(5) . . ? C43 C44 C39 117.4(5) . . ? C43 C44 C48 118.8(4) . . ? C40 C45 H45 108.5 . . ? C40 C45 C46 110.3(3) . . ? C40 C45 C47 111.9(3) . . ? C46 C45 H45 108.5 . . ? C47 C45 H45 108.5 . . ? C47 C45 C46 109.1(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48 108.2 . . ? C44 C48 C49 109.9(4) . . ? C44 C48 C50 113.4(3) . . ? C49 C48 H48 108.2 . . ? C49 C48 C50 108.9(4) . . ? C50 C48 H48 108.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C39B C40B 123.8(8) . . ? C44B C39B N3 114.2(9) . . ? C44B C39B C40B 122.0(11) . . ? C39B C40B C45B 123.7(7) . . ? C41B C40B C39B 116.7(8) . . ? C41B C40B C45B 119.5(6) . . ? C40B C41B H41B 119.5 . . ? C40B C41B C42B 121.0(7) . . ? C42B C41B H41B 119.5 . . ? C41B C42B H42B 119.0 . . ? C43B C42B C41B 122.0(6) . . ? C43B C42B H42B 119.0 . . ? C42B C43B H43B 119.9 . . ? C42B C43B C44B 120.2(6) . . ? C44B C43B H43B 119.9 . . ? C39B C44B C43B 118.0(8) . . ? C39B C44B C48B 123.5(8) . . ? C43B C44B C48B 118.4(6) . . ? C40B C45B H45B 108.9 . . ? C40B C45B C46B 109.5(5) . . ? C40B C45B C47B 112.5(5) . . ? C46B C45B H45B 108.9 . . ? C47B C45B H45B 108.9 . . ? C47B C45B C46B 108.0(4) . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46E 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C45B C47B H47D 109.5 . . ? C45B C47B H47E 109.5 . . ? C45B C47B H47F 109.5 . . ? H47D C47B H47E 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C44B C48B H48B 107.7 . . ? C44B C48B C49B 111.4(6) . . ? C44B C48B C50B 114.1(6) . . ? C49B C48B H48B 107.7 . . ? C49B C48B C50B 107.9(6) . . ? C50B C48B H48B 107.7 . . ? C48B C49B H49D 109.5 . . ? C48B C49B H49E 109.5 . . ? C48B C49B H49F 109.5 . . ? H49D C49B H49E 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? C48B C50B H50D 109.5 . . ? C48B C50B H50E 109.5 . . ? C48B C50B H50F 109.5 . . ? H50D C50B H50E 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? Cl9 C58 H58A 108.9 . . ? Cl9 C58 H58B 108.9 . . ? Cl10 C58 Cl9 113.6(3) . . ? Cl10 C58 H58A 108.9 . . ? Cl10 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? Cl1 Ga1 Cl2 107.26(6) . . ? Cl1 Ga1 Cl3 112.89(5) . . ? Cl1 Ga1 Cl4 107.74(7) . . ? Cl2 Ga1 Cl3 106.96(7) . . ? Cl2 Ga1 Cl4 114.16(5) . . ? Cl4 Ga1 Cl3 107.96(6) . . ? Cl5 Ga2 Cl6 110.71(7) . . ? Cl5 Ga2 Cl7 107.96(6) . . ? Cl5 Ga2 Cl8 110.35(6) . . ? Cl6 Ga2 Cl7 110.92(5) . . ? Cl6 Ga2 Cl8 108.45(6) . . ? Cl8 Ga2 Cl7 108.43(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C28 C29 C30 -127.11(14) . . . . ? P1 C28 C29 C34 51.66(19) . . . . ? P1 C35 C38 C37 154.10(13) . . . . ? P1 C35 C38 C53 37.23(19) . . . . ? P1 C35 C38 C57 -86.43(18) . . . . ? N1 C1 C28 P1 28.3(2) . . . . ? N1 C1 C28 C29 -164.12(15) . . . . ? N1 C2 C3 N2 0.7(2) . . . . ? N1 C4 C5 C6 -165.87(14) . . . . ? N1 C4 C5 C10 15.3(2) . . . . ? N1 C4 C9 C8 167.04(15) . . . . ? N1 C4 C9 C13 -12.6(2) . . . . ? N2 C1 C28 P1 -148.38(13) . . . . ? N2 C1 C28 C29 19.2(2) . . . . ? N2 C16 C17 C18 -178.35(13) . . . . ? N2 C16 C17 C22 -0.5(2) . . . . ? N2 C16 C21 C20 -179.76(13) . . . . ? N2 C16 C21 C25 1.5(2) . . . . ? N3 C35 C38 C37 -9.64(16) . . . . ? N3 C35 C38 C53 -126.51(14) . . . . ? N3 C35 C38 C57 109.83(15) . . . . ? N3 C36 C37 C38 -30.29(16) . . . . ? N3 C39 C40 C41 173.3(4) . . . . ? N3 C39 C40 C45 -10.4(8) . . . . ? N3 C39 C44 C43 -173.4(4) . . . . ? N3 C39 C44 C48 12.3(8) . . . . ? N3 C39B C40B C41B 177.0(8) . . . . ? N3 C39B C40B C45B -6.4(15) . . . . ? N3 C39B C44B C43B -177.0(7) . . . . ? N3 C39B C44B C48B 6.1(13) . . . . ? C1 N1 C2 C3 -1.3(2) . . . . ? C1 N1 C4 C5 -109.45(19) . . . . ? C1 N1 C4 C9 80.7(2) . . . . ? C1 N2 C3 C2 0.1(2) . . . . ? C1 N2 C16 C17 -109.87(18) . . . . ? C1 N2 C16 C21 74.8(2) . . . . ? C1 C28 C29 C30 66.14(19) . . . . ? C1 C28 C29 C34 -115.09(16) . . . . ? C2 N1 C1 N2 1.30(17) . . . . ? C2 N1 C1 C28 -175.97(15) . . . . ? C2 N1 C4 C5 72.14(19) . . . . ? C2 N1 C4 C9 -97.71(18) . . . . ? C3 N2 C1 N1 -0.89(17) . . . . ? C3 N2 C1 C28 176.41(15) . . . . ? C3 N2 C16 C17 76.64(19) . . . . ? C3 N2 C16 C21 -98.65(17) . . . . ? C4 N1 C1 N2 -177.20(16) . . . . ? C4 N1 C1 C28 5.5(3) . . . . ? C4 N1 C2 C3 177.49(15) . . . . ? C4 C5 C6 C7 -1.8(3) . . . . ? C4 C5 C10 C11 -113.77(19) . . . . ? C4 C5 C10 C12 122.77(18) . . . . ? C4 C9 C13 C14 80.2(2) . . . . ? C4 C9 C13 C15 -155.28(17) . . . . ? C5 C4 C9 C8 -2.0(3) . . . . ? C5 C4 C9 C13 178.35(16) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? C6 C5 C10 C11 67.5(2) . . . . ? C6 C5 C10 C12 -56.0(2) . . . . ? C6 C7 C8 C9 2.5(3) . . . . ? C7 C8 C9 C4 -1.0(3) . . . . ? C7 C8 C9 C13 178.61(18) . . . . ? C8 C9 C13 C14 -99.4(2) . . . . ? C8 C9 C13 C15 25.1(2) . . . . ? C9 C4 C5 C6 3.4(2) . . . . ? C9 C4 C5 C10 -175.38(16) . . . . ? C10 C5 C6 C7 177.01(17) . . . . ? C16 N2 C1 N1 -174.90(15) . . . . ? C16 N2 C1 C28 2.4(3) . . . . ? C16 N2 C3 C2 174.84(15) . . . . ? C16 C17 C18 C19 -1.0(2) . . . . ? C16 C17 C22 C23 -99.69(19) . . . . ? C16 C17 C22 C24 138.20(16) . . . . ? C16 C21 C25 C26 78.1(2) . . . . ? C16 C21 C25 C27 -159.64(15) . . . . ? C17 C16 C21 C20 5.2(2) . . . . ? C17 C16 C21 C25 -173.53(14) . . . . ? C17 C18 C19 C20 3.2(3) . . . . ? C18 C17 C22 C23 78.1(2) . . . . ? C18 C17 C22 C24 -44.0(2) . . . . ? C18 C19 C20 C21 -1.1(2) . . . . ? C19 C20 C21 C16 -2.9(2) . . . . ? C19 C20 C21 C25 175.83(15) . . . . ? C20 C21 C25 C26 -100.60(19) . . . . ? C20 C21 C25 C27 21.7(2) . . . . ? C21 C16 C17 C18 -3.3(2) . . . . ? C21 C16 C17 C22 174.60(15) . . . . ? C22 C17 C18 C19 -178.98(15) . . . . ? C28 P1 C35 N3 -159.98(11) . . . . ? C28 P1 C35 C38 37.00(17) . . . . ? C28 C29 C30 C31 177.47(14) . . . . ? C28 C29 C34 C33 -179.43(14) . . . . ? C29 C30 C31 C32 2.1(3) . . . . ? C30 C29 C34 C33 -0.6(2) . . . . ? C30 C31 C32 C33 -1.0(3) . . . . ? C31 C32 C33 C34 -1.0(3) . . . . ? C32 C33 C34 C29 1.8(3) . . . . ? C34 C29 C30 C31 -1.3(2) . . . . ? C35 P1 C28 C1 -163.83(11) . . . . ? C35 P1 C28 C29 29.35(15) . . . . ? C35 N3 C36 C37 25.66(17) . . . . ? C35 N3 C36 C51 -94.65(16) . . . . ? C35 N3 C36 C52 145.55(15) . . . . ? C35 N3 C39 C40 91.3(6) . . . . ? C35 N3 C39 C44 -93.6(6) . . . . ? C35 N3 C39B C40B 75.9(10) . . . . ? C35 N3 C39B C44B -103.1(10) . . . . ? C35 C38 C53 C54 176.82(13) . . . . ? C35 C38 C57 C56 175.81(14) . . . . ? C36 N3 C35 P1 -177.40(11) . . . . ? C36 N3 C35 C38 -10.22(18) . . . . ? C36 N3 C39 C40 -96.1(6) . . . . ? C36 N3 C39 C44 79.0(6) . . . . ? C36 N3 C39B C40B -89.9(11) . . . . ? C36 N3 C39B C44B 91.1(8) . . . . ? C36 C37 C38 C35 25.38(16) . . . . ? C36 C37 C38 C53 139.78(14) . . . . ? C36 C37 C38 C57 -99.21(15) . . . . ? C37 C38 C53 C54 66.51(18) . . . . ? C37 C38 C57 C56 -69.31(18) . . . . ? C38 C53 C54 C55 57.3(2) . . . . ? C51 C36 C37 C38 85.77(16) . . . . ? C52 C36 C37 C38 -150.81(14) . . . . ? C53 C38 C57 C56 52.86(17) . . . . ? C53 C54 C55 C56 -56.5(2) . . . . ? C54 C55 C56 C57 55.5(2) . . . . ? C55 C56 C57 C38 -54.6(2) . . . . ? C57 C38 C53 C54 -54.83(18) . . . . ? C39 N3 C35 P1 -4.2(3) . . . . ? C39 N3 C35 C38 163.0(3) . . . . ? C39 N3 C36 C37 -147.6(3) . . . . ? C39 N3 C36 C51 92.1(3) . . . . ? C39 N3 C36 C52 -27.7(3) . . . . ? C39 C40 C41 C42 -0.1(7) . . . . ? C39 C40 C45 C46 -112.4(5) . . . . ? C39 C40 C45 C47 125.9(5) . . . . ? C39 C44 C48 C49 101.6(6) . . . . ? C39 C44 C48 C50 -136.3(5) . . . . ? C40 C39 C44 C43 1.5(8) . . . . ? C40 C39 C44 C48 -172.8(5) . . . . ? C40 C41 C42 C43 1.9(6) . . . . ? C41 C40 C45 C46 63.9(4) . . . . ? C41 C40 C45 C47 -57.8(4) . . . . ? C41 C42 C43 C44 -2.0(6) . . . . ? C42 C43 C44 C39 0.3(6) . . . . ? C42 C43 C44 C48 175.0(4) . . . . ? C43 C44 C48 C49 -72.6(5) . . . . ? C43 C44 C48 C50 49.4(6) . . . . ? C44 C39 C40 C41 -1.6(8) . . . . ? C44 C39 C40 C45 174.8(5) . . . . ? C45 C40 C41 C42 -176.7(4) . . . . ? C39B N3 C35 P1 16.5(5) . . . . ? C39B N3 C35 C38 -176.4(5) . . . . ? C39B N3 C36 C37 -166.5(5) . . . . ? C39B N3 C36 C51 73.2(5) . . . . ? C39B N3 C36 C52 -46.6(5) . . . . ? C39B C40B C41B C42B 1.3(10) . . . . ? C39B C40B C45B C46B -113.5(8) . . . . ? C39B C40B C45B C47B 126.3(8) . . . . ? C39B C44B C48B C49B 104.7(9) . . . . ? C39B C44B C48B C50B -132.9(9) . . . . ? C40B C39B C44B C43B 3.9(14) . . . . ? C40B C39B C44B C48B -172.9(8) . . . . ? C40B C41B C42B C43B 1.6(11) . . . . ? C41B C40B C45B C46B 63.0(7) . . . . ? C41B C40B C45B C47B -57.2(7) . . . . ? C41B C42B C43B C44B -1.8(11) . . . . ? C42B C43B C44B C39B -0.9(11) . . . . ? C42B C43B C44B C48B 176.1(6) . . . . ? C43B C44B C48B C49B -72.2(8) . . . . ? C43B C44B C48B C50B 50.3(8) . . . . ? C44B C39B C40B C41B -4.1(14) . . . . ? C44B C39B C40B C45B 172.5(8) . . . . ? C45B C40B C41B C42B -175.5(6) . . . . ? _shelx_res_file ; TITL sharma36_a.res in C2/c sharma36.res created by SHELXL-2018/3 at 10:05:03 on 07-Jun-2019 REM Old TITL sharma36_a.res in C2/c REM SHELXT solution in C2/c: R1 0.303, Rweak 0.071, Alpha 0.080 REM 0.592 for 576 systematic absences, Orientation as input REM Formula found by SHELXT: C116 N12 P2 Cl8 Ga1 CELL 0.71073 40.7612 12.3237 23.4798 90 101.398 90 ZERR 4 0.0006 0.0002 0.0003 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Ga N P UNIT 460 616 40 8 24 8 EADP C44 C44B EADP C43 C43B EADP C42 C42B EADP C41 C41B L.S. 11 PLAN 16 BOND $H list more -1 conf fmap 2 acta OMIT 0 0 18 OMIT -9 9 3 OMIT 0 0 12 OMIT 18 0 6 OMIT 18 0 12 REM REM REM WGHT 0.033700 16.737402 FVAR 0.13520 0.61382 P1 6 0.611768 0.739601 0.631240 11.00000 0.01651 0.02174 = 0.01453 -0.00026 0.00348 -0.00144 N1 5 0.572380 0.830389 0.509878 11.00000 0.01690 0.02307 = 0.02010 0.00267 0.00188 0.00418 N2 5 0.607971 0.766092 0.459832 11.00000 0.01637 0.02363 = 0.01321 0.00209 0.00111 0.00174 N3 5 0.637837 0.703024 0.742559 11.00000 0.02848 0.02108 = 0.01315 -0.00182 0.00381 -0.00609 C1 1 0.604213 0.789114 0.515901 11.00000 0.01362 0.01762 = 0.01665 0.00057 0.00162 0.00113 C2 1 0.556813 0.830261 0.451574 11.00000 0.01803 0.03428 = 0.02311 0.00507 -0.00320 0.00591 AFIX 43 H2 2 0.535071 0.852977 0.436521 11.00000 -1.20000 AFIX 0 C3 1 0.578731 0.791553 0.420911 11.00000 0.02024 0.03665 = 0.01577 0.00439 -0.00317 0.00257 AFIX 43 H3 2 0.574997 0.783273 0.380777 11.00000 -1.20000 AFIX 0 C4 1 0.553637 0.873655 0.551298 11.00000 0.01495 0.02296 = 0.02521 -0.00128 0.00281 0.00630 C5 1 0.527054 0.810191 0.562444 11.00000 0.01679 0.02821 = 0.02551 -0.00040 0.00246 0.00285 C6 1 0.504440 0.861203 0.591434 11.00000 0.01953 0.03898 = 0.03261 -0.00197 0.00705 0.00400 AFIX 43 H6 2 0.486096 0.822578 0.598679 11.00000 -1.20000 AFIX 0 C7 1 0.508819 0.968073 0.609563 11.00000 0.02489 0.04036 = 0.04265 -0.00681 0.00890 0.01329 AFIX 43 H7 2 0.493278 1.000717 0.628227 11.00000 -1.20000 AFIX 0 C8 1 0.536247 1.026564 0.600020 11.00000 0.02990 0.02693 = 0.04619 -0.00953 0.00378 0.01016 AFIX 43 H8 2 0.539313 1.097337 0.613790 11.00000 -1.20000 AFIX 0 C9 1 0.559401 0.981556 0.570162 11.00000 0.02103 0.02224 = 0.03473 -0.00107 0.00046 0.00589 C10 1 0.522506 0.691193 0.545709 11.00000 0.02458 0.02624 = 0.02951 -0.00151 0.00628 -0.00111 AFIX 13 H10 2 0.541886 0.668473 0.529728 11.00000 -1.20000 AFIX 0 C11 1 0.490912 0.673285 0.498694 11.00000 0.03980 0.03466 = 0.03661 -0.00171 -0.00425 -0.00618 AFIX 137 H11A 2 0.471550 0.695096 0.513380 11.00000 -1.50000 H11B 2 0.489069 0.597857 0.488340 11.00000 -1.50000 H11C 2 0.492390 0.715721 0.465007 11.00000 -1.50000 AFIX 0 C12 1 0.521321 0.620398 0.599169 11.00000 0.03624 0.03295 = 0.03402 0.00271 0.00485 -0.00726 AFIX 137 H12A 2 0.540796 0.634239 0.628667 11.00000 -1.50000 H12B 2 0.520846 0.545222 0.588322 11.00000 -1.50000 H12C 2 0.501583 0.637521 0.613904 11.00000 -1.50000 AFIX 0 C13 1 0.589236 1.046259 0.558288 11.00000 0.02234 0.02297 = 0.04435 0.00015 -0.00030 0.00140 AFIX 13 H13 2 0.608219 0.996191 0.561990 11.00000 -1.20000 AFIX 0 C14 1 0.582856 1.092114 0.496286 11.00000 0.03538 0.03886 = 0.05415 0.01437 -0.00457 -0.00952 AFIX 137 H14A 2 0.578261 1.033604 0.468874 11.00000 -1.50000 H14B 2 0.602294 1.130985 0.490261 11.00000 -1.50000 H14C 2 0.564021 1.140429 0.490949 11.00000 -1.50000 AFIX 0 C15 1 0.599483 1.137892 0.602492 11.00000 0.03796 0.02713 = 0.06273 -0.00786 -0.00100 -0.00112 AFIX 137 H15A 2 0.582927 1.194311 0.595779 11.00000 -1.50000 H15B 2 0.620732 1.166823 0.598231 11.00000 -1.50000 H15C 2 0.601198 1.109860 0.641116 11.00000 -1.50000 AFIX 0 C16 1 0.635375 0.713669 0.439407 11.00000 0.01656 0.02663 = 0.01174 -0.00040 0.00054 0.00255 C17 1 0.655411 0.777708 0.410249 11.00000 0.02396 0.02866 = 0.01287 0.00106 0.00213 0.00019 C18 1 0.681063 0.724838 0.389665 11.00000 0.02332 0.03778 = 0.01720 -0.00242 0.00521 -0.00264 AFIX 43 H18 2 0.694613 0.764238 0.369625 11.00000 -1.20000 AFIX 0 C19 1 0.686639 0.615177 0.398559 11.00000 0.02399 0.03756 = 0.02072 -0.00985 0.00337 0.00196 AFIX 43 H19 2 0.704545 0.582316 0.386188 11.00000 -1.20000 AFIX 0 C20 1 0.665861 0.553680 0.425686 11.00000 0.02905 0.02526 = 0.02228 -0.00699 0.00213 0.00312 AFIX 43 H20 2 0.669774 0.479618 0.430694 11.00000 -1.20000 AFIX 0 C21 1 0.639084 0.600774 0.445718 11.00000 0.02374 0.02503 = 0.01256 -0.00311 -0.00085 -0.00061 C22 1 0.649539 0.898253 0.398870 11.00000 0.03316 0.03061 = 0.02757 0.00928 0.00952 0.00156 AFIX 13 H22 2 0.635404 0.925239 0.425050 11.00000 -1.20000 AFIX 0 C23 1 0.630623 0.914827 0.335797 11.00000 0.04395 0.05193 = 0.04421 0.02756 -0.00256 -0.00565 AFIX 137 H23A 2 0.644606 0.892656 0.309449 11.00000 -1.50000 H23B 2 0.624945 0.990084 0.329600 11.00000 -1.50000 H23C 2 0.610543 0.872057 0.329078 11.00000 -1.50000 AFIX 0 C24 1 0.681872 0.965475 0.408983 11.00000 0.04389 0.03229 = 0.02799 0.00683 0.00831 -0.00609 AFIX 137 H24A 2 0.694923 0.949354 0.446729 11.00000 -1.50000 H24B 2 0.676385 1.041312 0.406709 11.00000 -1.50000 H24C 2 0.694531 0.947805 0.379836 11.00000 -1.50000 AFIX 0 C25 1 0.614741 0.531616 0.471984 11.00000 0.03224 0.02384 = 0.02378 -0.00194 0.00650 -0.00453 AFIX 13 H25 2 0.609008 0.571670 0.504728 11.00000 -1.20000 AFIX 0 C26 1 0.582346 0.512406 0.427056 11.00000 0.03878 0.04162 = 0.05225 0.00518 -0.00222 -0.01744 AFIX 137 H26A 2 0.567316 0.468693 0.444059 11.00000 -1.50000 H26B 2 0.587512 0.475664 0.393864 11.00000 -1.50000 H26C 2 0.571974 0.580861 0.415179 11.00000 -1.50000 AFIX 0 C27 1 0.629247 0.421817 0.494507 11.00000 0.05638 0.02533 = 0.02409 -0.00368 0.01181 -0.00324 AFIX 137 H27A 2 0.632343 0.377515 0.462353 11.00000 -1.50000 H27B 2 0.614102 0.386365 0.515024 11.00000 -1.50000 H27C 2 0.650406 0.432614 0.520287 11.00000 -1.50000 AFIX 0 C28 1 0.627846 0.769176 0.568679 11.00000 0.01522 0.01733 = 0.01369 0.00038 0.00218 0.00305 C29 1 0.663347 0.752206 0.564723 11.00000 0.01507 0.03041 = 0.01195 -0.00402 0.00037 0.00333 C30 1 0.682372 0.835776 0.547256 11.00000 0.02050 0.04445 = 0.01340 0.00189 0.00307 -0.00097 AFIX 43 H30 2 0.672498 0.902618 0.536410 11.00000 -1.20000 AFIX 0 C31 1 0.716106 0.819359 0.546022 11.00000 0.02122 0.07362 = 0.01591 0.00055 0.00515 -0.00703 AFIX 43 H31 2 0.728832 0.875917 0.535603 11.00000 -1.20000 AFIX 0 C32 1 0.730621 0.718957 0.560295 11.00000 0.01702 0.08846 = 0.01957 -0.01006 0.00292 0.00992 AFIX 43 H32 2 0.753017 0.707991 0.558864 11.00000 -1.20000 AFIX 0 C33 1 0.712017 0.634782 0.576682 11.00000 0.02638 0.05574 = 0.02811 -0.01550 -0.00307 0.01959 AFIX 43 H33 2 0.721812 0.567167 0.585655 11.00000 -1.20000 AFIX 0 C34 1 0.678595 0.651400 0.579730 11.00000 0.02168 0.03281 = 0.02094 -0.00765 -0.00245 0.00976 AFIX 43 H34 2 0.666319 0.595284 0.591793 11.00000 -1.20000 AFIX 0 C35 1 0.643721 0.754900 0.695006 11.00000 0.01990 0.01693 = 0.01392 -0.00077 0.00491 0.00107 C36 1 0.664608 0.722032 0.796087 11.00000 0.02952 0.02488 = 0.01172 -0.00149 0.00166 -0.00129 C37 1 0.677952 0.831511 0.780725 11.00000 0.02344 0.02764 = 0.01457 -0.00323 0.00316 -0.00405 AFIX 23 H37A 2 0.701433 0.838846 0.798537 11.00000 -1.20000 H37B 2 0.665634 0.890114 0.794420 11.00000 -1.20000 AFIX 0 C38 1 0.673260 0.835076 0.713369 11.00000 0.02164 0.02382 = 0.01320 -0.00206 0.00340 -0.00400 C51 1 0.690015 0.629271 0.801782 11.00000 0.04649 0.03430 = 0.02484 0.00439 0.00410 0.01072 AFIX 137 H51A 2 0.679690 0.563268 0.811000 11.00000 -1.50000 H51B 2 0.708813 0.645803 0.832170 11.00000 -1.50000 H51C 2 0.697479 0.620560 0.765750 11.00000 -1.50000 AFIX 0 C52 1 0.650909 0.726168 0.852420 11.00000 0.03400 0.03535 = 0.01337 0.00163 0.00500 -0.00540 AFIX 137 H52A 2 0.636237 0.787400 0.851302 11.00000 -1.50000 H52B 2 0.669165 0.733007 0.885019 11.00000 -1.50000 H52C 2 0.638758 0.660684 0.856171 11.00000 -1.50000 AFIX 0 C53 1 0.661466 0.948589 0.689448 11.00000 0.03228 0.02164 = 0.02108 -0.00137 0.00437 -0.00595 AFIX 23 H53A 2 0.655850 0.945398 0.647364 11.00000 -1.20000 H53B 2 0.641362 0.968270 0.703275 11.00000 -1.20000 AFIX 0 C54 1 0.688037 1.036304 0.707796 11.00000 0.05175 0.02989 = 0.02769 -0.00300 0.00552 -0.01813 AFIX 23 H54A 2 0.679779 1.105209 0.690776 11.00000 -1.20000 H54B 2 0.692404 1.044138 0.749724 11.00000 -1.20000 AFIX 0 C55 1 0.720349 1.007055 0.688240 11.00000 0.04588 0.05541 = 0.02994 -0.00046 0.00542 -0.03266 AFIX 23 H55A 2 0.737160 1.061852 0.701822 11.00000 -1.20000 H55B 2 0.716425 1.005777 0.646131 11.00000 -1.20000 AFIX 0 C56 1 0.733140 0.896726 0.711902 11.00000 0.02516 0.06667 = 0.02100 -0.00509 0.00450 -0.01768 AFIX 23 H56A 2 0.739442 0.900708 0.753905 11.00000 -1.20000 H56B 2 0.752973 0.878151 0.696967 11.00000 -1.20000 AFIX 0 C57 1 0.706639 0.806862 0.695014 11.00000 0.01950 0.04207 = 0.01542 -0.00211 0.00294 -0.00273 AFIX 23 H57A 2 0.715218 0.739369 0.713405 11.00000 -1.20000 H57B 2 0.702580 0.796117 0.653284 11.00000 -1.20000 AFIX 0 PART 1 C39 1 0.606081 0.643224 0.744130 21.00000 0.02663 0.02384 = 0.01340 0.00383 0.00169 -0.00790 C40 1 0.604176 0.532786 0.730486 21.00000 0.04072 0.02291 = 0.01749 0.00218 0.00000 -0.00449 C41 1 0.575449 0.476401 0.738406 21.00000 0.06825 0.03343 = 0.03245 0.00102 0.00583 -0.02593 AFIX 43 H41 2 0.573541 0.402816 0.729589 21.00000 -1.20000 AFIX 0 C42 1 0.549821 0.527938 0.759094 21.00000 0.04636 0.06420 = 0.03914 0.00512 0.00714 -0.03261 AFIX 43 H42 2 0.531316 0.488659 0.765079 21.00000 -1.20000 AFIX 0 C43 1 0.551992 0.637378 0.770663 21.00000 0.03359 0.05842 = 0.03068 0.00438 0.00920 -0.01717 AFIX 43 H43 2 0.534427 0.671730 0.783352 21.00000 -1.20000 AFIX 0 C44 1 0.579886 0.698455 0.763873 21.00000 0.02670 0.02990 = 0.01818 0.00020 0.00624 -0.00446 C45 1 0.630002 0.472263 0.704684 21.00000 0.04960 0.02151 = 0.02057 0.00051 -0.00118 0.00053 AFIX 13 H45 2 0.648820 0.521210 0.703620 21.00000 -1.20000 AFIX 0 C46 1 0.614937 0.436475 0.641944 21.00000 0.07243 0.02546 = 0.02265 -0.00446 -0.00174 -0.00015 AFIX 137 H46A 2 0.596970 0.386327 0.642416 21.00000 -1.50000 H46B 2 0.631928 0.401988 0.625235 21.00000 -1.50000 H46C 2 0.606546 0.498858 0.619173 21.00000 -1.50000 AFIX 0 C47 1 0.643333 0.371602 0.740967 21.00000 0.08708 0.02893 = 0.02910 0.00036 -0.00676 0.01310 AFIX 137 H47A 2 0.649598 0.391568 0.781172 21.00000 -1.50000 H47B 2 0.662509 0.343479 0.727826 21.00000 -1.50000 H47C 2 0.626193 0.317080 0.736495 21.00000 -1.50000 AFIX 0 C48 1 0.579244 0.819753 0.772575 21.00000 0.02935 0.03591 = 0.02219 -0.00406 0.01307 0.00104 AFIX 13 H48 2 0.601836 0.847898 0.773567 21.00000 -1.20000 AFIX 0 C49 1 0.555475 0.872701 0.721196 21.00000 0.04925 0.05178 = 0.03132 0.00250 0.01510 0.01858 AFIX 137 H49A 2 0.561424 0.849952 0.685466 21.00000 -1.50000 H49B 2 0.557254 0.950215 0.724510 21.00000 -1.50000 H49C 2 0.532886 0.851040 0.721490 21.00000 -1.50000 AFIX 0 C50 1 0.568391 0.853328 0.829871 21.00000 0.04828 0.05879 = 0.03209 -0.01138 0.02116 0.00064 AFIX 137 H50A 2 0.545214 0.835694 0.827427 21.00000 -1.50000 H50B 2 0.571533 0.930022 0.835715 21.00000 -1.50000 H50C 2 0.581717 0.815022 0.861886 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C39B 1 0.614570 0.619616 0.745671 -21.00000 0.02521 0.03451 = 0.01410 0.00332 0.00014 -0.00400 C40B 1 0.619177 0.509097 0.730108 -21.00000 0.03904 0.02015 = 0.01802 -0.00326 0.00647 -0.00440 C41B 1 0.594762 0.436078 0.738269 -21.00000 0.06825 0.03343 = 0.03245 0.00102 0.00583 -0.02593 AFIX 43 H41B 2 0.597011 0.363222 0.729453 -21.00000 -1.20000 AFIX 0 C42B 1 0.566985 0.469771 0.759385 -21.00000 0.04636 0.06420 = 0.03914 0.00512 0.00714 -0.03261 AFIX 43 H42B 2 0.551284 0.418427 0.765339 -21.00000 -1.20000 AFIX 0 C43B 1 0.562029 0.575141 0.771597 -21.00000 0.03359 0.05842 = 0.03068 0.00438 0.00920 -0.01717 AFIX 43 H43B 2 0.542818 0.595444 0.784662 -21.00000 -1.20000 AFIX 0 C44B 1 0.585832 0.653936 0.764588 -21.00000 0.02670 0.02990 = 0.01818 0.00020 0.00624 -0.00446 C45B 1 0.647691 0.470946 0.702902 -21.00000 0.04026 0.02023 = 0.01621 -0.00372 0.00561 -0.00061 AFIX 13 H45B 2 0.663008 0.531785 0.701599 -21.00000 -1.20000 AFIX 0 C46B 1 0.633854 0.431712 0.640139 -21.00000 0.05595 0.02420 = 0.02247 -0.00211 0.00316 0.00382 AFIX 137 H46D 2 0.618260 0.373608 0.640901 -21.00000 -1.50000 H46E 2 0.651992 0.406450 0.623057 -21.00000 -1.50000 H46F 2 0.622728 0.490741 0.617527 -21.00000 -1.50000 AFIX 0 C47B 1 0.667400 0.376361 0.736801 -21.00000 0.08094 0.02628 = 0.01859 0.00312 -0.00144 0.01611 AFIX 137 H47D 2 0.673818 0.395673 0.777078 -21.00000 -1.50000 H47E 2 0.687070 0.361908 0.721332 -21.00000 -1.50000 H47F 2 0.653564 0.312706 0.733068 -21.00000 -1.50000 AFIX 0 C48B 1 0.578291 0.771162 0.774942 -21.00000 0.02198 0.04676 = 0.01975 0.00182 0.00766 0.00342 AFIX 13 H48B 2 0.598776 0.812979 0.775258 -21.00000 -1.20000 AFIX 0 C49B 1 0.551072 0.816031 0.725925 -21.00000 0.03717 0.07504 = 0.03246 -0.00052 0.00972 0.02435 AFIX 137 H49D 2 0.558900 0.814000 0.689970 -21.00000 -1.50000 H49E 2 0.546059 0.889585 0.734621 -21.00000 -1.50000 H49F 2 0.531235 0.772566 0.722532 -21.00000 -1.50000 AFIX 0 C50B 1 0.567046 0.792279 0.833593 -21.00000 0.03634 0.06203 = 0.02905 -0.01338 0.01515 0.00451 AFIX 137 H50D 2 0.545043 0.762962 0.831766 -21.00000 -1.50000 H50E 2 0.566712 0.868971 0.840624 -21.00000 -1.50000 H50F 2 0.582450 0.757924 0.864556 -21.00000 -1.50000 AFIX 0 PART 0 PART -2 CL9 3 0.679046 0.164600 0.545568 10.50000 0.06835 0.05904 = 0.06916 -0.00129 -0.00582 -0.00216 CL10 3 0.704600 0.318768 0.636271 10.50000 0.11049 0.06020 = 0.04537 -0.00163 0.01604 -0.00242 C58 1 0.712493 0.247076 0.578517 10.50000 0.06008 0.08968 = 0.05391 -0.00927 0.03554 -0.00119 AFIX 23 H58A 2 0.732029 0.201845 0.591376 10.50000 -1.20000 H58B 2 0.717728 0.297437 0.549839 10.50000 -1.20000 AFIX 0 PART 0 PART -1 GA1 4 0.495424 0.773410 0.258888 10.50000 0.02936 0.03711 = 0.02546 -0.00626 -0.00756 0.00843 CL1 3 0.444385 0.830511 0.249465 10.50000 0.03629 0.04642 = 0.06522 -0.01299 -0.01675 0.01484 CL2 3 0.504447 0.661309 0.331756 10.50000 0.03540 0.05956 = 0.02127 0.00362 -0.00123 0.00679 CL3 3 0.532189 0.903179 0.279260 10.50000 0.05126 0.05417 = 0.04433 -0.01024 -0.00637 -0.01032 CL4 3 0.500789 0.701471 0.176553 10.50000 0.06602 0.04265 = 0.02030 -0.00180 -0.00056 0.00548 GA2 4 0.722006 0.239415 0.545599 10.50000 0.02420 0.03236 = 0.02407 -0.00413 -0.00204 0.00827 CL5 3 0.673543 0.162867 0.522795 10.50000 0.02988 0.04371 = 0.05466 -0.00711 0.00466 0.00324 CL6 3 0.728993 0.310543 0.631362 10.50000 0.05668 0.07276 = 0.03576 -0.02644 -0.00777 0.01956 CL7 3 0.760087 0.116183 0.541635 10.50000 0.03207 0.03619 = 0.03761 0.00600 0.00609 0.01460 CL8 3 0.726758 0.367562 0.483414 10.50000 0.04123 0.04123 = 0.05715 0.01579 0.01192 0.01771 HKLF 4 REM sharma36_a.res in C2/c REM wR2 = 0.1194, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0517 for 13305 Fo > 4sig(Fo) and 0.0873 for all 19086 data REM 770 parameters refined using 0 restraints END WGHT 0.0337 16.7497 REM Highest difference peak 0.897, deepest hole -0.567, 1-sigma level 0.058 Q1 1 0.4537 0.8825 0.2384 11.00000 0.05 0.90 Q2 1 0.5209 0.9250 0.2612 11.00000 0.05 0.34 Q3 1 0.6076 0.7730 0.4891 11.00000 0.05 0.32 Q4 1 0.6583 0.7229 0.8226 11.00000 0.05 0.31 Q5 1 0.6766 0.8397 0.7476 11.00000 0.05 0.30 Q6 1 0.5301 0.8891 0.2903 11.00000 0.05 0.30 Q7 1 0.6707 0.7001 0.5748 11.00000 0.05 0.30 Q8 1 0.5229 0.7608 0.5498 11.00000 0.05 0.30 Q9 1 0.6509 0.8370 0.4081 11.00000 0.05 0.29 Q10 1 0.5398 0.8355 0.5604 11.00000 0.05 0.29 Q11 1 0.6132 0.7692 0.5459 11.00000 0.05 0.29 Q12 1 0.5215 0.6616 0.5710 11.00000 0.05 0.29 Q13 1 0.6166 0.8046 0.5437 11.00000 0.05 0.29 Q14 1 0.6385 0.6591 0.4487 11.00000 0.05 0.29 Q15 1 0.5299 0.9906 0.6203 11.00000 0.05 0.28 Q16 1 0.4994 0.6108 0.3171 11.00000 0.05 0.28 ; _shelx_res_checksum 623 _olex2_date_sample_data_collection 2019-06-05 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.312 _oxdiff_exptl_absorpt_empirical_full_min 0.825