#------------------------------------------------------------------------------ #$Date: 2022-03-05 00:20:23 +0200 (Sat, 05 Mar 2022) $ #$Revision: 273396 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/12/7061200.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7061200 loop_ _publ_author_name 'Liu, Nian' 'Liu, Li' 'Zhong, Xin-Xin' 'Li, Fa-Bao' 'Li, Feng-Yan' 'Qin, Hai-Mei' _publ_section_title ; Ethynyl \p-coordinated and non-coordinated mononuclear Cu(i) halide diphosphine complexes: synthesis and photophysical studies ; _journal_issue 7 _journal_name_full 'New Journal of Chemistry' _journal_page_first 3236 _journal_page_last 3247 _journal_paper_doi 10.1039/D1NJ05578J _journal_volume 46 _journal_year 2022 _chemical_formula_moiety 'C38 H28 Br Cu P2' _chemical_formula_sum 'C38 H28 Br Cu P2' _chemical_formula_weight 689.99 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-10-09 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-21 deposited with the CCDC. 2022-01-12 downloaded from the CCDC. ; _cell_angle_alpha 94.9990(10) _cell_angle_beta 101.4460(10) _cell_angle_gamma 92.0070(10) _cell_formula_units_Z 2 _cell_length_a 9.44410(10) _cell_length_b 10.0937(2) _cell_length_c 16.8020(3) _cell_measurement_reflns_used 21423 _cell_measurement_temperature 100 _cell_measurement_theta_max 73.6590 _cell_measurement_theta_min 2.6870 _cell_volume 1561.59(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _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)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.938 _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 -35.00 66.00 0.50 0.10 -- 37.97 -50.00 3.00 202 2 \w -7.00 19.00 0.50 0.10 -- -37.97 50.00 150.00 52 3 \w 15.00 42.00 0.50 0.05 -- 0.00 50.00 150.00 54 4 \w 80.00 111.00 0.50 0.10 -- 37.97 50.00 150.00 62 5 \w 41.00 67.00 0.50 0.10 -- 37.97 50.00 150.00 52 6 \w 33.00 146.00 0.50 1.00 -- 112.45 -50.00 3.00 226 7 \w 83.00 178.00 0.50 1.00 -- 112.45 50.00 150.00 190 8 \w 62.00 125.00 0.50 0.10 -- 37.97 178.00 0.00 126 9 \w 61.00 116.00 0.50 0.10 -- 37.97 178.00 -60.00 110 10 \w 63.00 125.00 0.50 0.10 -- 37.97 178.00-180.00 124 11 \w 113.00 149.00 0.50 1.00 -- 112.45 178.00-120.00 72 12 \w 81.00 107.00 0.50 1.00 -- 112.45 178.00-120.00 52 13 \w 60.00 140.00 0.50 1.00 -- 112.45 178.00 30.00 160 14 \w 60.00 120.00 0.50 0.10 -- 37.97 178.00 120.00 120 15 \w 10.00 113.00 0.50 0.10 -- 37.97 57.00 -30.00 206 16 \w 31.00 104.00 0.50 1.00 -- 112.45 -94.00 0.00 146 17 \w 57.00 113.00 0.50 1.00 -- 112.45-111.00-120.00 112 18 \w 65.00 108.00 0.50 1.00 -- 112.45 -94.00-180.00 86 19 \w 31.00 112.00 0.50 1.00 -- 112.45-111.00 0.00 162 20 \w 59.00 107.00 0.50 1.00 -- 112.45-111.00 120.00 96 21 \w -34.00 -8.00 0.50 0.05 -- 0.00 50.00 150.00 52 22 \w -6.00 34.00 0.50 0.10 -- 37.97 95.00 39.55 80 23 \w -5.00 44.00 0.50 0.10 -- 37.97 91.00 -51.28 98 24 \w -6.00 44.00 0.50 0.10 -- 37.97 91.00-132.38 100 25 \w -50.00 -12.00 0.50 0.10 -- -37.97 -50.00 3.00 76 26 \w -26.00 0.00 0.50 0.10 -- -37.97 -77.00 -60.00 52 27 \w -48.00 -23.00 0.50 0.05 -- 0.00 -50.00 3.00 50 28 \w -33.00 -8.00 0.50 0.10 -- -37.97 -57.00 90.00 50 29 \w -59.00 -33.00 0.50 0.10 -- -37.97 -57.00 60.00 52 30 \w -71.00 -46.00 0.50 0.10 -- -37.97 -77.00 -60.00 50 31 \w -116.00 -74.00 0.50 0.10 -- -37.97 -77.00-180.00 84 32 \w -67.00 -1.00 0.50 0.10 -- -37.97 -77.00-180.00 132 33 \w -95.00 -59.00 0.50 1.00 -- -98.50 -80.00 -38.84 72 34 \w -85.00 -60.00 0.50 1.00 -- -98.50 -78.00 -0.99 50 35 \w -88.00 -59.00 0.50 1.00 -- -98.50 -80.00 43.82 58 36 \w -83.00 -58.00 0.50 1.00 -- -98.50 -82.00 88.20 50 37 \w -97.00 -60.00 0.50 1.00 -- -98.50 -78.00 54.19 74 38 \w -101.00 -58.00 0.50 1.00 -- -98.50 -83.00 -12.89 86 39 \w -90.00 -58.00 0.50 1.00 -- -98.50 -83.00 -24.55 64 40 \w -97.00 -60.00 0.50 1.00 -- -98.50 -77.00-103.70 74 41 \w -91.00 -60.00 0.50 1.00 -- -98.50 -80.00-162.75 62 42 \w -94.00 -60.00 0.50 1.00 -- -98.50 -77.00-120.00 68 43 \w -105.00 -61.00 0.50 1.00 -- -98.50 -74.00 -74.57 88 44 \w -105.00 -59.00 0.50 1.00 -- -98.50 -79.00 27.39 92 45 \w -90.00 -60.00 0.50 1.00 -- -98.50 -77.00 139.45 60 46 \w -96.00 -58.00 0.50 1.00 -- -98.50 -81.00 119.40 76 47 \w -106.00 -67.00 0.50 1.00 -- -98.50 -66.00 148.59 78 48 \w -116.00 -61.00 0.50 1.00 -- -98.50 -75.00 102.62 110 49 \w -116.00 -55.00 0.50 0.10 -- -37.97 -50.00 3.00 122 50 \w -100.00 -75.00 0.50 1.00 -- -98.50 50.00 150.00 50 51 \w -131.00 -97.00 0.50 1.00 -- -98.50 -50.00 3.00 68 52 \w -127.00-102.00 0.50 1.00 -- -98.50 -78.00 -0.99 50 53 \w -139.00-103.00 0.50 1.00 -- -98.50 -80.00 43.82 72 54 \w -140.00 -60.00 0.50 1.00 -- -98.50 -77.00 90.00 160 55 \w -115.00 -74.00 0.50 0.10 -- -37.97 -57.00 90.00 82 56 \w -112.00 -13.00 0.50 0.10 -- -37.97 -77.00 120.00 198 57 \w -110.00 -82.00 0.50 0.10 -- -37.97 -57.00 60.00 56 58 \w -116.00 -91.00 0.50 0.10 -- -37.97 -77.00 -60.00 50 59 \w -147.00 -61.00 0.50 1.00 -- -98.50 -74.00 9.60 172 60 \w -138.00 -58.00 0.50 1.00 -- -98.50 -81.00-149.90 160 61 \w -132.00 -59.00 0.50 1.00 -- -98.50 -81.00-174.90 146 62 \w -139.00 -96.00 0.50 1.00 -- -98.50 -83.00 -24.55 86 63 \w -148.00 -59.00 0.50 1.00 -- -98.50 -79.00-137.03 178 64 \w -165.00-102.00 0.50 1.00 -- -98.50 -80.00 -38.84 126 65 \w -155.00-102.00 0.50 1.00 -- -98.50 -77.00-103.70 106 66 \w -170.00 -60.00 0.50 1.00 -- -98.50 -77.00 -60.00 220 67 \w -164.00-113.00 0.50 1.00 -- -98.50 -82.00 88.20 102 68 \w -169.00 -64.00 0.50 1.00 -- -98.50 -67.00 116.30 210 69 \w -170.00 -60.00 0.50 1.00 -- -98.50 -77.00 -90.00 220 70 \w -162.00-136.00 0.50 1.00 -- -98.50 -78.00 54.19 52 71 \w -177.00 -61.00 0.50 1.00 -- -98.50 -76.00 65.96 232 72 \w -169.00-111.00 0.50 1.00 -- -98.50 -77.00-120.00 116 73 \w -176.00-144.00 0.50 1.00 -- -98.50 -80.00 43.82 64 74 \w -174.00-148.00 0.50 1.00 -- -98.50 -75.00 102.62 52 75 \w -174.00 -62.00 0.50 1.00 -- -98.50 -72.00 166.07 224 76 \w -176.00-126.00 0.50 1.00 -- -98.50 -77.00 139.45 100 77 \w -175.00-147.00 0.50 1.00 -- -98.50 -81.00 119.40 56 78 \w -130.00 -41.00 0.50 1.00 -- -98.50 178.00 60.00 178 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1546324000 _diffrn_orient_matrix_UB_12 -0.0281544000 _diffrn_orient_matrix_UB_13 0.0132137000 _diffrn_orient_matrix_UB_21 0.0123553000 _diffrn_orient_matrix_UB_22 0.1306157000 _diffrn_orient_matrix_UB_23 0.0562505000 _diffrn_orient_matrix_UB_31 -0.0609608000 _diffrn_orient_matrix_UB_32 0.0754158000 _diffrn_orient_matrix_UB_33 -0.0741240000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_unetI/netI 0.0149 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.938 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 31420 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.938 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.350 _diffrn_reflns_theta_min 2.696 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.646 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.467 _exptl_crystal_description block _exptl_crystal_F_000 700 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _refine_diff_density_max 1.034 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 379 _refine_ls_number_reflns 5980 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0286 _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^)+(0.0413P)^2^+0.9534P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.0800 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5801 _reflns_number_total 5980 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj05578j2.cif _cod_data_source_block s1-pe _cod_depositor_comments 'Adding full bibliography for 7061196--7061202.cif.' _cod_database_code 7061200 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_max 0.964 _shelx_estimated_absorpt_t_min 0.899 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C14(H14), C25(H25), C22(H22), C15(H15), C28(H28), C8(H8), C12(H12), C17(H17), C16(H16), C34(H34), C6(H6), C23(H23), C2(H2), C38(H38), C32(H32), C29(H29), C10(H10), C24(H24), C11(H11), C9(H9), C4(H4), C30(H30), C35(H35), C36(H36), C31(H31), C37(H37), C5(H5), C3(H3) ; _shelx_res_file ; s1-pe.res created by SHELXL-2014/7 TITL s1-pe_a.res in P-1 REM Old TITL s1-PE in P-1 REM SHELXT solution in P-1 REM R1 0.227, Rweak 0.016, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C37 N3 O2 Br2 CELL 1.54184 9.4441 10.0937 16.802 94.999 101.446 92.007 ZERR 2 0.0001 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H Br Cu P UNIT 76 56 2 2 4 L.S. 4 PLAN 10 SIZE 0.01 0.03 0.02 TEMP -173.15 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.041300 0.953400 FVAR 5.00523 BR1 3 0.072908 0.510459 0.285479 11.00000 0.05775 0.05466 = 0.05994 0.01316 0.02449 0.02225 CU1 4 0.276780 0.385940 0.272776 11.00000 0.03834 0.04285 = 0.03223 0.01039 0.00945 0.00607 P1 5 0.380055 0.435118 0.168286 11.00000 0.03043 0.03928 = 0.02596 0.00487 0.00538 0.00200 P2 5 0.345739 0.246664 0.367740 11.00000 0.03156 0.03444 = 0.02787 0.00554 0.00368 0.00177 C7 1 0.444099 0.607248 0.166021 11.00000 0.03762 0.04182 = 0.02503 0.00435 0.00450 -0.00076 C26 1 0.230753 0.093060 0.339693 11.00000 0.03392 0.03455 = 0.03653 0.00493 0.00840 0.00348 C21 1 0.144770 0.069395 0.260740 11.00000 0.03190 0.03209 = 0.03913 0.00345 0.00712 0.00317 C13 1 0.240876 0.402877 0.075218 11.00000 0.02892 0.04447 = 0.02756 0.00413 0.00646 0.00717 C20 1 0.151368 0.155241 0.197610 11.00000 0.03263 0.03833 = 0.03602 0.00057 0.00208 0.00024 C18 1 0.144142 0.292324 0.070388 11.00000 0.03235 0.04554 = 0.02940 0.00389 0.00536 0.00574 C19 1 0.148782 0.215997 0.139053 11.00000 0.03200 0.04296 = 0.03570 0.00186 0.00192 -0.00134 C1 1 0.525396 0.333588 0.144342 11.00000 0.03188 0.04093 = 0.03471 0.00815 0.00689 0.00246 C33 1 0.531637 0.195572 0.382140 11.00000 0.03355 0.04317 = 0.03457 0.00839 0.00430 0.00313 C14 1 0.230076 0.479146 0.009463 11.00000 0.03880 0.05178 = 0.03271 0.00912 0.01022 0.00767 AFIX 43 H14 2 0.294032 0.555134 0.012887 11.00000 -1.20000 AFIX 0 C25 1 0.221351 0.000597 0.395691 11.00000 0.05480 0.04503 = 0.04185 0.01252 0.00526 -0.00177 AFIX 43 H25 2 0.279009 0.015103 0.449165 11.00000 -1.20000 AFIX 0 C22 1 0.049394 -0.044288 0.241339 11.00000 0.04382 0.03662 = 0.05074 0.00065 0.00189 -0.00258 AFIX 43 H22 2 -0.010605 -0.059618 0.188538 11.00000 -1.20000 AFIX 0 C27 1 0.319664 0.292895 0.471399 11.00000 0.04289 0.03620 = 0.02869 0.00554 0.00475 -0.00197 C15 1 0.126189 0.444992 -0.061404 11.00000 0.04215 0.06678 = 0.03039 0.01271 0.00802 0.01627 AFIX 43 H15 2 0.118258 0.498563 -0.105690 11.00000 -1.20000 AFIX 0 C28 1 0.185777 0.339204 0.479285 11.00000 0.04233 0.06025 = 0.03509 0.00479 0.00932 -0.00095 AFIX 43 H28 2 0.115119 0.350121 0.431829 11.00000 -1.20000 AFIX 0 C8 1 0.576866 0.643234 0.148646 11.00000 0.04759 0.04943 = 0.04403 0.00395 0.01932 -0.00057 AFIX 43 H8 2 0.638461 0.576303 0.134828 11.00000 -1.20000 AFIX 0 C12 1 0.355695 0.706593 0.186340 11.00000 0.03767 0.04721 = 0.04302 0.00345 0.00572 0.00334 AFIX 43 H12 2 0.265831 0.683271 0.200099 11.00000 -1.20000 AFIX 0 C17 1 0.042700 0.257407 -0.002130 11.00000 0.03741 0.05913 = 0.03797 0.00025 0.00136 -0.00064 AFIX 43 H17 2 -0.021204 0.181070 -0.006713 11.00000 -1.20000 AFIX 0 C16 1 0.035584 0.334270 -0.067206 11.00000 0.03849 0.07515 = 0.02959 0.00116 -0.00093 0.01126 AFIX 43 H16 2 -0.032944 0.309759 -0.116330 11.00000 -1.20000 AFIX 0 C34 1 0.570415 0.067180 0.367483 11.00000 0.04133 0.04582 = 0.05391 -0.00106 0.00779 0.00293 AFIX 43 H34 2 0.497722 -0.002868 0.351750 11.00000 -1.20000 AFIX 0 C6 1 0.514670 0.256859 0.070472 11.00000 0.04589 0.06507 = 0.03888 0.00276 0.00694 0.01632 AFIX 43 H6 2 0.430131 0.258002 0.029102 11.00000 -1.20000 AFIX 0 C23 1 0.042146 -0.132827 0.297595 11.00000 0.05668 0.03535 = 0.07031 0.00664 0.01143 -0.00930 AFIX 43 H23 2 -0.022992 -0.208999 0.283819 11.00000 -1.20000 AFIX 0 C2 1 0.650078 0.330195 0.203277 11.00000 0.04063 0.06182 = 0.04762 0.00158 -0.00138 0.00650 AFIX 43 H2 2 0.658683 0.381406 0.254359 11.00000 -1.20000 AFIX 0 C38 1 0.640434 0.296528 0.407149 11.00000 0.03917 0.04276 = 0.07473 0.00963 0.00490 0.00135 AFIX 43 H38 2 0.615537 0.385688 0.418162 11.00000 -1.20000 AFIX 0 C32 1 0.423363 0.282318 0.541346 11.00000 0.05775 0.05979 = 0.03613 0.00391 -0.00086 0.01270 AFIX 43 H32 2 0.516209 0.252452 0.537363 11.00000 -1.20000 AFIX 0 C29 1 0.154363 0.369637 0.555833 11.00000 0.05759 0.05953 = 0.04447 -0.00068 0.02144 -0.00507 AFIX 43 H29 2 0.061609 0.398981 0.560487 11.00000 -1.20000 AFIX 0 C10 1 0.531315 0.874147 0.169881 11.00000 0.07397 0.04392 = 0.05266 0.00382 0.01211 -0.01012 AFIX 43 H10 2 0.561098 0.965336 0.171236 11.00000 -1.20000 AFIX 0 C24 1 0.129166 -0.111956 0.374386 11.00000 0.07029 0.04217 = 0.06310 0.02103 0.01304 -0.00407 AFIX 43 H24 2 0.125742 -0.175152 0.412774 11.00000 -1.20000 AFIX 0 C11 1 0.397936 0.839310 0.186625 11.00000 0.05959 0.04385 = 0.05731 0.00159 0.01043 0.00805 AFIX 43 H11 2 0.335266 0.906677 0.198337 11.00000 -1.20000 AFIX 0 C9 1 0.620230 0.776774 0.151354 11.00000 0.05626 0.05824 = 0.05523 0.00552 0.02141 -0.01309 AFIX 43 H9 2 0.712083 0.800700 0.140292 11.00000 -1.20000 AFIX 0 C4 1 0.749544 0.176854 0.115411 11.00000 0.04388 0.06536 = 0.07078 0.02130 0.02288 0.01966 AFIX 43 H4 2 0.825979 0.123058 0.105565 11.00000 -1.20000 AFIX 0 C30 1 0.256528 0.357527 0.624642 11.00000 0.08368 0.04967 = 0.03466 -0.00025 0.01985 -0.00330 AFIX 43 H30 2 0.234580 0.377946 0.676980 11.00000 -1.20000 AFIX 0 C35 1 0.715746 0.039058 0.375554 11.00000 0.05073 0.05343 = 0.07481 0.00247 0.01355 0.01594 AFIX 43 H35 2 0.741382 -0.049866 0.364551 11.00000 -1.20000 AFIX 0 C36 1 0.821645 0.138536 0.399189 11.00000 0.03640 0.07083 = 0.07208 0.01520 0.00802 0.01186 AFIX 43 H36 2 0.920531 0.119134 0.404053 11.00000 -1.20000 AFIX 0 C31 1 0.389979 0.316064 0.617917 11.00000 0.08737 0.06928 = 0.02991 0.00342 -0.00567 0.00899 AFIX 43 H31 2 0.461305 0.309989 0.665859 11.00000 -1.20000 AFIX 0 C37 1 0.784022 0.267089 0.415905 11.00000 0.03648 0.06020 = 0.08756 0.01250 0.00175 -0.00348 AFIX 43 H37 2 0.857485 0.336049 0.433603 11.00000 -1.20000 AFIX 0 C5 1 0.626951 0.178492 0.056816 11.00000 0.06257 0.07294 = 0.05201 0.00145 0.01951 0.02372 AFIX 43 H5 2 0.618384 0.125608 0.006305 11.00000 -1.20000 AFIX 0 C3 1 0.762560 0.253144 0.188827 11.00000 0.03561 0.07304 = 0.06981 0.01598 0.00070 0.01147 AFIX 43 H3 2 0.848354 0.252928 0.229406 11.00000 -1.20000 AFIX 0 HKLF 4 REM s1-pe_a.res in P-1 REM R1 = 0.0286 for 5801 Fo > 4sig(Fo) and 0.0293 for all 5980 data REM 379 parameters refined using 0 restraints END WGHT 0.0413 0.9533 REM Highest difference peak 1.034, deepest hole -0.860, 1-sigma level 0.049 Q1 1 0.1383 0.5419 0.3274 11.00000 0.05 1.03 Q2 1 0.3397 0.2709 0.4273 11.00000 0.05 0.28 Q3 1 0.4517 0.2175 0.3759 11.00000 0.05 0.26 Q4 1 0.2940 0.4237 0.1106 11.00000 0.05 0.24 Q5 1 0.4565 0.3849 0.1564 11.00000 0.05 0.23 Q6 1 0.3626 0.4406 0.2268 11.00000 0.05 0.23 Q7 1 0.4176 0.5406 0.1617 11.00000 0.05 0.22 Q8 1 0.2195 0.3349 0.5814 11.00000 0.05 0.22 Q9 1 0.1973 0.0810 0.2994 11.00000 0.05 0.21 Q10 1 0.0939 0.2740 0.0325 11.00000 0.05 0.21 ; _shelx_res_checksum 61540 _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 1.380 _oxdiff_exptl_absorpt_empirical_full_min 0.758 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.07291(3) 0.51046(2) 0.28548(2) 0.05479(9) Uani 1 1 d . . . . . Cu1 Cu 0.27678(3) 0.38594(3) 0.27278(2) 0.03699(9) Uani 1 1 d . . . . . P1 P 0.38005(5) 0.43512(5) 0.16829(3) 0.03183(10) Uani 1 1 d . . . . . P2 P 0.34574(5) 0.24666(4) 0.36774(3) 0.03146(10) Uani 1 1 d . . . . . C7 C 0.4441(2) 0.60725(19) 0.16602(10) 0.0351(4) Uani 1 1 d . . . . . C26 C 0.23075(19) 0.09306(18) 0.33969(11) 0.0347(4) Uani 1 1 d . . . . . C21 C 0.14477(19) 0.06939(18) 0.26074(12) 0.0343(4) Uani 1 1 d . . . . . C13 C 0.24088(19) 0.40288(19) 0.07522(11) 0.0334(4) Uani 1 1 d . . . . . C20 C 0.15137(19) 0.15524(19) 0.19761(12) 0.0366(4) Uani 1 1 d . . . . . C18 C 0.14414(19) 0.29232(19) 0.07039(11) 0.0358(4) Uani 1 1 d . . . . . C19 C 0.1488(2) 0.2160(2) 0.13905(12) 0.0378(4) Uani 1 1 d . . . . . C1 C 0.52540(19) 0.33359(19) 0.14434(11) 0.0355(4) Uani 1 1 d . . . . . C33 C 0.5316(2) 0.1956(2) 0.38214(11) 0.0372(4) Uani 1 1 d . . . . . C14 C 0.2301(2) 0.4791(2) 0.00946(12) 0.0403(4) Uani 1 1 d . . . . . H14 H 0.2940 0.5551 0.0129 0.048 Uiso 1 1 calc R . . . . C25 C 0.2214(2) 0.0006(2) 0.39569(13) 0.0475(5) Uani 1 1 d . . . . . H25 H 0.2790 0.0151 0.4492 0.057 Uiso 1 1 calc R . . . . C22 C 0.0494(2) -0.0443(2) 0.24134(14) 0.0451(5) Uani 1 1 d . . . . . H22 H -0.0106 -0.0596 0.1885 0.054 Uiso 1 1 calc R . . . . C27 C 0.3197(2) 0.29289(18) 0.47140(11) 0.0362(4) Uani 1 1 d . . . . . C15 C 0.1262(2) 0.4450(2) -0.06140(12) 0.0455(5) Uani 1 1 d . . . . . H15 H 0.1183 0.4986 -0.1057 0.055 Uiso 1 1 calc R . . . . C28 C 0.1858(2) 0.3392(2) 0.47929(13) 0.0458(5) Uani 1 1 d . . . . . H28 H 0.1151 0.3501 0.4318 0.055 Uiso 1 1 calc R . . . . C8 C 0.5769(2) 0.6432(2) 0.14865(13) 0.0457(5) Uani 1 1 d . . . . . H8 H 0.6385 0.5763 0.1348 0.055 Uiso 1 1 calc R . . . . C12 C 0.3557(2) 0.7066(2) 0.18634(13) 0.0430(4) Uani 1 1 d . . . . . H12 H 0.2658 0.6833 0.2001 0.052 Uiso 1 1 calc R . . . . C17 C 0.0427(2) 0.2574(2) -0.00213(13) 0.0460(5) Uani 1 1 d . . . . . H17 H -0.0212 0.1811 -0.0067 0.055 Uiso 1 1 calc R . . . . C16 C 0.0356(2) 0.3343(3) -0.06721(12) 0.0489(5) Uani 1 1 d . . . . . H16 H -0.0329 0.3098 -0.1163 0.059 Uiso 1 1 calc R . . . . C34 C 0.5704(2) 0.0672(2) 0.36748(14) 0.0476(5) Uani 1 1 d . . . . . H34 H 0.4977 -0.0029 0.3518 0.057 Uiso 1 1 calc R . . . . C6 C 0.5147(2) 0.2569(2) 0.07047(13) 0.0500(5) Uani 1 1 d . . . . . H6 H 0.4301 0.2580 0.0291 0.060 Uiso 1 1 calc R . . . . C23 C 0.0421(3) -0.1328(2) 0.29760(16) 0.0545(6) Uani 1 1 d . . . . . H23 H -0.0230 -0.2090 0.2838 0.065 Uiso 1 1 calc R . . . . C2 C 0.6501(2) 0.3302(2) 0.20328(14) 0.0516(5) Uani 1 1 d . . . . . H2 H 0.6587 0.3814 0.2544 0.062 Uiso 1 1 calc R . . . . C38 C 0.6404(2) 0.2965(2) 0.40715(16) 0.0529(5) Uani 1 1 d . . . . . H38 H 0.6155 0.3857 0.4182 0.064 Uiso 1 1 calc R . . . . C32 C 0.4234(3) 0.2823(2) 0.54135(13) 0.0525(5) Uani 1 1 d . . . . . H32 H 0.5162 0.2525 0.5374 0.063 Uiso 1 1 calc R . . . . C29 C 0.1544(3) 0.3696(2) 0.55583(14) 0.0529(5) Uani 1 1 d . . . . . H29 H 0.0616 0.3990 0.5605 0.063 Uiso 1 1 calc R . . . . C10 C 0.5313(3) 0.8741(2) 0.16988(15) 0.0573(6) Uani 1 1 d . . . . . H10 H 0.5611 0.9653 0.1712 0.069 Uiso 1 1 calc R . . . . C24 C 0.1292(3) -0.1120(2) 0.37439(16) 0.0578(6) Uani 1 1 d . . . . . H24 H 0.1257 -0.1752 0.4128 0.069 Uiso 1 1 calc R . . . . C11 C 0.3979(3) 0.8393(2) 0.18662(15) 0.0539(5) Uani 1 1 d . . . . . H11 H 0.3353 0.9067 0.1983 0.065 Uiso 1 1 calc R . . . . C9 C 0.6202(3) 0.7768(2) 0.15135(15) 0.0556(6) Uani 1 1 d . . . . . H9 H 0.7121 0.8007 0.1403 0.067 Uiso 1 1 calc R . . . . C4 C 0.7495(3) 0.1769(3) 0.11541(17) 0.0572(6) Uani 1 1 d . . . . . H4 H 0.8260 0.1231 0.1056 0.069 Uiso 1 1 calc R . . . . C30 C 0.2565(3) 0.3575(2) 0.62464(13) 0.0553(6) Uani 1 1 d . . . . . H30 H 0.2346 0.3779 0.6770 0.066 Uiso 1 1 calc R . . . . C35 C 0.7157(3) 0.0391(3) 0.37555(17) 0.0594(6) Uani 1 1 d . . . . . H35 H 0.7414 -0.0499 0.3646 0.071 Uiso 1 1 calc R . . . . C36 C 0.8216(2) 0.1385(3) 0.39919(17) 0.0595(6) Uani 1 1 d . . . . . H36 H 0.9205 0.1191 0.4041 0.071 Uiso 1 1 calc R . . . . C31 C 0.3900(3) 0.3161(3) 0.61792(14) 0.0646(7) Uani 1 1 d . . . . . H31 H 0.4613 0.3100 0.6659 0.078 Uiso 1 1 calc R . . . . C37 C 0.7840(2) 0.2671(3) 0.41590(19) 0.0627(7) Uani 1 1 d . . . . . H37 H 0.8575 0.3360 0.4336 0.075 Uiso 1 1 calc R . . . . C5 C 0.6270(3) 0.1785(3) 0.05682(16) 0.0612(6) Uani 1 1 d . . . . . H5 H 0.6184 0.1256 0.0063 0.073 Uiso 1 1 calc R . . . . C3 C 0.7626(2) 0.2531(3) 0.18883(17) 0.0601(6) Uani 1 1 d . . . . . H3 H 0.8484 0.2529 0.2294 0.072 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 Br1 0.05775(15) 0.05466(15) 0.05994(16) 0.01316(11) 0.02449(11) 0.02225(11) Cu1 0.03834(15) 0.04285(16) 0.03223(15) 0.01039(11) 0.00945(11) 0.00607(11) P1 0.0304(2) 0.0393(2) 0.0260(2) 0.00487(17) 0.00538(16) 0.00200(17) P2 0.0316(2) 0.0344(2) 0.0279(2) 0.00554(17) 0.00368(17) 0.00177(17) C7 0.0376(9) 0.0418(10) 0.0250(8) 0.0043(7) 0.0045(7) -0.0008(7) C26 0.0339(9) 0.0346(9) 0.0365(9) 0.0049(7) 0.0084(7) 0.0035(7) C21 0.0319(8) 0.0321(8) 0.0391(9) 0.0034(7) 0.0071(7) 0.0032(7) C13 0.0289(8) 0.0445(10) 0.0276(8) 0.0041(7) 0.0065(7) 0.0072(7) C20 0.0326(9) 0.0383(9) 0.0360(9) 0.0006(8) 0.0021(7) 0.0002(7) C18 0.0324(9) 0.0455(10) 0.0294(9) 0.0039(7) 0.0054(7) 0.0057(7) C19 0.0320(9) 0.0430(10) 0.0357(9) 0.0019(8) 0.0019(7) -0.0013(7) C1 0.0319(9) 0.0409(9) 0.0347(9) 0.0081(7) 0.0069(7) 0.0025(7) C33 0.0336(9) 0.0432(10) 0.0346(9) 0.0084(8) 0.0043(7) 0.0031(7) C14 0.0388(10) 0.0518(11) 0.0327(9) 0.0091(8) 0.0102(8) 0.0077(8) C25 0.0548(12) 0.0450(11) 0.0418(11) 0.0125(9) 0.0053(9) -0.0018(9) C22 0.0438(11) 0.0366(10) 0.0507(12) 0.0006(8) 0.0019(9) -0.0026(8) C27 0.0429(10) 0.0362(9) 0.0287(9) 0.0055(7) 0.0047(7) -0.0020(7) C15 0.0421(10) 0.0668(13) 0.0304(9) 0.0127(9) 0.0080(8) 0.0163(9) C28 0.0423(10) 0.0602(13) 0.0351(10) 0.0048(9) 0.0093(8) -0.0009(9) C8 0.0476(11) 0.0494(11) 0.0440(11) 0.0039(9) 0.0193(9) -0.0006(9) C12 0.0377(10) 0.0472(11) 0.0430(11) 0.0034(9) 0.0057(8) 0.0033(8) C17 0.0374(10) 0.0591(13) 0.0380(10) 0.0003(9) 0.0014(8) -0.0006(9) C16 0.0385(10) 0.0752(15) 0.0296(9) 0.0012(9) -0.0009(8) 0.0113(10) C34 0.0413(10) 0.0458(11) 0.0539(12) -0.0011(9) 0.0078(9) 0.0029(9) C6 0.0459(11) 0.0651(14) 0.0389(11) 0.0028(10) 0.0069(9) 0.0163(10) C23 0.0567(13) 0.0354(10) 0.0703(15) 0.0066(10) 0.0114(11) -0.0093(9) C2 0.0406(11) 0.0618(13) 0.0476(12) 0.0016(10) -0.0014(9) 0.0065(9) C38 0.0392(11) 0.0428(11) 0.0747(16) 0.0096(10) 0.0049(10) 0.0013(9) C32 0.0577(13) 0.0598(13) 0.0361(11) 0.0039(9) -0.0009(9) 0.0127(10) C29 0.0576(13) 0.0595(13) 0.0445(12) -0.0007(10) 0.0214(10) -0.0051(11) C10 0.0740(16) 0.0439(12) 0.0527(13) 0.0038(10) 0.0121(12) -0.0101(11) C24 0.0703(15) 0.0422(11) 0.0631(15) 0.0210(10) 0.0130(12) -0.0041(10) C11 0.0596(13) 0.0439(11) 0.0573(13) 0.0016(10) 0.0104(11) 0.0080(10) C9 0.0563(13) 0.0582(13) 0.0552(13) 0.0055(11) 0.0214(11) -0.0131(11) C4 0.0439(12) 0.0654(14) 0.0708(16) 0.0213(12) 0.0229(11) 0.0197(10) C30 0.0837(17) 0.0497(12) 0.0347(11) -0.0002(9) 0.0198(11) -0.0033(11) C35 0.0507(13) 0.0534(13) 0.0748(17) 0.0025(12) 0.0135(12) 0.0159(10) C36 0.0364(11) 0.0708(16) 0.0721(16) 0.0152(13) 0.0080(10) 0.0119(10) C31 0.0874(19) 0.0693(16) 0.0299(11) 0.0034(10) -0.0057(11) 0.0090(14) C37 0.0365(11) 0.0602(14) 0.0876(19) 0.0125(13) 0.0017(11) -0.0035(10) C5 0.0626(15) 0.0729(16) 0.0520(13) 0.0015(12) 0.0195(11) 0.0237(12) C3 0.0356(11) 0.0730(16) 0.0698(16) 0.0160(13) 0.0007(10) 0.0115(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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' 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 P1 Cu1 Br1 113.940(17) . . ? P2 Cu1 Br1 116.596(17) . . ? P2 Cu1 P1 129.38(2) . . ? C7 P1 Cu1 118.06(6) . . ? C7 P1 C13 103.87(8) . . ? C7 P1 C1 105.30(9) . . ? C13 P1 Cu1 106.91(6) . . ? C1 P1 Cu1 118.48(6) . . ? C1 P1 C13 102.14(8) . . ? C26 P2 Cu1 108.01(6) . . ? C33 P2 Cu1 117.29(6) . . ? C33 P2 C26 105.94(9) . . ? C33 P2 C27 104.07(9) . . ? C27 P2 Cu1 118.36(6) . . ? C27 P2 C26 101.45(8) . . ? C8 C7 P1 123.77(16) . . ? C8 C7 C12 119.02(19) . . ? C12 C7 P1 117.16(15) . . ? C21 C26 P2 119.60(14) . . ? C25 C26 P2 121.71(15) . . ? C25 C26 C21 118.64(17) . . ? C26 C21 C20 122.92(16) . . ? C26 C21 C22 119.29(18) . . ? C22 C21 C20 117.78(17) . . ? C18 C13 P1 117.12(13) . . ? C14 C13 P1 123.39(15) . . ? C14 C13 C18 119.46(17) . . ? C19 C20 C21 172.88(19) . . ? C13 C18 C19 120.38(16) . . ? C17 C18 C13 119.25(18) . . ? C17 C18 C19 120.36(18) . . ? C20 C19 C18 178.2(2) . . ? C6 C1 P1 122.92(15) . . ? C2 C1 P1 118.54(16) . . ? C2 C1 C6 118.51(19) . . ? C34 C33 P2 124.61(15) . . ? C34 C33 C38 118.82(19) . . ? C38 C33 P2 116.53(16) . . ? C13 C14 H14 119.7 . . ? C13 C14 C15 120.50(19) . . ? C15 C14 H14 119.7 . . ? C26 C25 H25 119.6 . . ? C24 C25 C26 120.9(2) . . ? C24 C25 H25 119.6 . . ? C21 C22 H22 119.6 . . ? C23 C22 C21 120.7(2) . . ? C23 C22 H22 119.6 . . ? C28 C27 P2 116.94(14) . . ? C32 C27 P2 124.19(17) . . ? C32 C27 C28 118.86(19) . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 119.97(19) . . ? C16 C15 H15 120.0 . . ? C27 C28 H28 119.7 . . ? C29 C28 C27 120.6(2) . . ? C29 C28 H28 119.7 . . ? C7 C8 H8 119.9 . . ? C7 C8 C9 120.3(2) . . ? C9 C8 H8 119.9 . . ? C7 C12 H12 119.8 . . ? C11 C12 C7 120.3(2) . . ? C11 C12 H12 119.8 . . ? C18 C17 H17 120.0 . . ? C16 C17 C18 120.0(2) . . ? C16 C17 H17 120.0 . . ? C15 C16 C17 120.71(19) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C33 C34 H34 119.8 . . ? C33 C34 C35 120.4(2) . . ? C35 C34 H34 119.8 . . ? C1 C6 H6 119.9 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.9 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.2(2) . . ? C24 C23 H23 119.9 . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 120.9(2) . . ? C3 C2 H2 119.5 . . ? C33 C38 H38 119.9 . . ? C37 C38 C33 120.2(2) . . ? C37 C38 H38 119.9 . . ? C27 C32 H32 120.3 . . ? C27 C32 C31 119.4(2) . . ? C31 C32 H32 120.3 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.2(2) . . ? C30 C29 H29 119.9 . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C9 C10 C11 119.8(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.9 . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C8 C9 H9 119.8 . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 119.8 . . ? C5 C4 H4 120.0 . . ? C5 C4 C3 120.1(2) . . ? C3 C4 H4 120.0 . . ? C29 C30 H30 120.1 . . ? C31 C30 C29 119.9(2) . . ? C31 C30 H30 120.1 . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.5(2) . . ? C36 C35 H35 119.8 . . ? C35 C36 H36 120.2 . . ? C35 C36 C37 119.6(2) . . ? C37 C36 H36 120.2 . . ? C32 C31 H31 119.5 . . ? C30 C31 C32 121.0(2) . . ? C30 C31 H31 119.5 . . ? C38 C37 H37 119.7 . . ? C36 C37 C38 120.5(2) . . ? C36 C37 H37 119.7 . . ? C6 C5 H5 119.8 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C2 C3 H3 120.1 . . ? C4 C3 C2 119.8(2) . . ? C4 C3 H3 120.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.3703(3) . ? Cu1 P1 2.2533(5) . ? Cu1 P2 2.2336(5) . ? P1 C7 1.8257(19) . ? P1 C13 1.8288(18) . ? P1 C1 1.8281(19) . ? P2 C26 1.8322(19) . ? P2 C33 1.8230(19) . ? P2 C27 1.8299(19) . ? C7 C8 1.386(3) . ? C7 C12 1.390(3) . ? C26 C21 1.407(3) . ? C26 C25 1.394(3) . ? C21 C20 1.436(3) . ? C21 C22 1.407(3) . ? C13 C18 1.403(3) . ? C13 C14 1.390(3) . ? C20 C19 1.201(3) . ? C18 C19 1.437(3) . ? C18 C17 1.402(3) . ? C1 C6 1.388(3) . ? C1 C2 1.384(3) . ? C33 C34 1.374(3) . ? C33 C38 1.397(3) . ? C14 H14 0.9500 . ? C14 C15 1.393(3) . ? C25 H25 0.9500 . ? C25 C24 1.383(3) . ? C22 H22 0.9500 . ? C22 C23 1.366(3) . ? C27 C28 1.390(3) . ? C27 C32 1.387(3) . ? C15 H15 0.9500 . ? C15 C16 1.368(3) . ? C28 H28 0.9500 . ? C28 C29 1.388(3) . ? C8 H8 0.9500 . ? C8 C9 1.389(3) . ? C12 H12 0.9500 . ? C12 C11 1.384(3) . ? C17 H17 0.9500 . ? C17 C16 1.387(3) . ? C16 H16 0.9500 . ? C34 H34 0.9500 . ? C34 C35 1.394(3) . ? C6 H6 0.9500 . ? C6 C5 1.388(3) . ? C23 H23 0.9500 . ? C23 C24 1.380(4) . ? C2 H2 0.9500 . ? C2 C3 1.386(3) . ? C38 H38 0.9500 . ? C38 C37 1.380(3) . ? C32 H32 0.9500 . ? C32 C31 1.401(4) . ? C29 H29 0.9500 . ? C29 C30 1.368(4) . ? C10 H10 0.9500 . ? C10 C11 1.384(4) . ? C10 C9 1.370(4) . ? C24 H24 0.9500 . ? C11 H11 0.9500 . ? C9 H9 0.9500 . ? C4 H4 0.9500 . ? C4 C5 1.364(4) . ? C4 C3 1.377(4) . ? C30 H30 0.9500 . ? C30 C31 1.364(4) . ? C35 H35 0.9500 . ? C35 C36 1.367(4) . ? C36 H36 0.9500 . ? C36 C37 1.377(4) . ? C31 H31 0.9500 . ? C37 H37 0.9500 . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ?