#------------------------------------------------------------------------------ #$Date: 2022-01-18 03:03:35 +0200 (Tue, 18 Jan 2022) $ #$Revision: 272092 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/12/7061201.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_7061201 loop_ _publ_author_name 'Liu, Nian' 'Liu, Li' 'Zhong, Xinxin' 'Li, Fa-Bao' 'Li, Fengyan' 'Qin, Hai-Mei' _publ_section_title ; Ethynyl \p-Coordinated and Non-Coordinated Mononuclear Cu(I) Halide Diphosphine Complexes: Synthesis and Photophysical Studies ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ05578J _journal_year 2022 _chemical_formula_moiety 'C40 H32 Br Cu O2 P2' _chemical_formula_sum 'C40 H32 Br Cu O2 P2' _chemical_formula_weight 750.04 _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 2020-09-02 _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 90.6640(10) _cell_angle_beta 114.373(2) _cell_angle_gamma 108.705(2) _cell_formula_units_Z 2 _cell_length_a 12.1192(2) _cell_length_b 12.5675(3) _cell_length_c 12.6953(2) _cell_measurement_reflns_used 15757 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 74.0330 _cell_measurement_theta_min 3.7290 _cell_volume 1644.87(7) _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_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.937 _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 8.00 46.00 0.50 1.74 -- 37.97 57.00 -30.00 76 2 \w 49.00 110.00 0.50 1.74 -- 37.97 57.00 -30.00 122 3 \w 60.00 115.00 0.50 1.74 -- 37.97 57.00 -90.00 110 4 \w 134.00 160.00 0.50 1.74 -- 112.45 109.00 -80.00 52 5 \w 77.00 124.00 0.50 1.74 -- 37.97 178.00-150.00 94 6 \w 60.00 126.00 0.50 1.74 -- 37.97 178.00 -60.00 132 7 \w 75.00 177.00 0.50 1.74 -- 112.45 77.00-150.00 204 8 \w 67.00 92.00 0.50 1.74 -- 37.97-109.00-176.00 50 9 \w 28.00 55.00 0.50 1.74 -- 37.97-109.00-176.00 54 10 \w 67.00 108.00 0.50 1.74 -- 112.45-109.00-176.00 82 11 \w 65.00 106.00 0.50 1.74 -- 112.45 -94.00 -90.00 82 12 \w 49.00 105.00 0.50 1.74 -- 112.45 -94.00 0.00 112 13 \w 32.00 115.00 0.50 1.74 -- 112.45-111.00 150.00 166 14 \w 28.00 105.00 0.50 1.74 -- 112.45 -94.00 60.00 154 15 \w 31.00 108.00 0.50 1.74 -- 112.45 -94.00 -60.00 154 16 \w 34.00 59.00 0.50 1.74 -- 112.45 -94.00 -90.00 50 17 \w 33.00 95.00 0.50 1.74 -- 112.45 -94.00-120.00 124 18 \w 14.00 40.00 0.50 1.74 -- 37.97 57.00 -90.00 52 19 \w 6.00 37.00 0.50 1.74 -- 37.97 94.00 -98.34 62 20 \w 8.00 111.00 0.50 1.74 -- 37.97 57.00-150.00 206 21 \w 12.00 111.00 0.50 1.74 -- 37.97 77.00 0.00 198 22 \w 42.00 68.00 0.50 1.74 -- 37.97 57.00 150.00 52 23 \w 83.00 115.00 0.50 1.74 -- 37.97 57.00 150.00 64 24 \w 8.00 83.00 0.50 1.74 -- 37.97 57.00 120.00 150 25 \w -5.00 41.00 0.50 1.74 -- 37.97 90.00 177.01 92 26 \w -65.00 38.00 0.50 1.74 -- -37.97 57.00 90.00 206 27 \w -54.00 -29.00 0.50 0.43 -- 0.00 109.00 -80.00 50 28 \w -48.00 -10.00 0.50 1.74 -- -37.97 109.00 -80.00 76 29 \w -62.00 39.00 0.50 1.74 -- -37.97 57.00 -30.00 202 30 \w -60.00 -2.00 0.50 1.74 -- -37.97 -77.00 60.00 116 31 \w -52.00 -1.00 0.50 1.74 -- -37.97 -77.00 -60.00 102 32 \w -84.00 -58.00 0.50 1.74 -- -98.50 -83.00 -19.14 52 33 \w -90.00 -60.00 0.50 1.74 -- -98.50 -77.00 -90.00 60 34 \w -85.00 -58.00 0.50 1.74 -- -98.50 -83.00-128.82 54 35 \w -87.00 -60.00 0.50 1.74 -- -98.50 -77.00-150.00 54 36 \w -88.00 -60.00 0.50 1.74 -- -98.50 -77.00-120.00 56 37 \w -93.00 -60.00 0.50 1.74 -- -98.50 -77.00-180.00 66 38 \w -113.00 -88.00 0.50 1.74 -- -37.97 -77.00 -60.00 50 39 \w -143.00-115.00 0.50 1.74 -- -98.50-109.00-176.00 56 40 \w -139.00-112.00 0.50 1.74 -- -98.50 -77.00-180.00 54 41 \w -130.00 -60.00 0.50 1.74 -- -98.50 -77.00 -98.40 140 42 \w -104.00 -58.00 0.50 1.74 -- -98.50 -83.00 -39.38 92 43 \w -98.00 -63.00 0.50 1.74 -- -98.50 -70.00 35.43 70 44 \w -83.00 -58.00 0.50 1.74 -- -98.50 -83.00 85.56 50 45 \w -83.00 -58.00 0.50 1.74 -- -98.50 -81.00 113.98 50 46 \w -85.00 -60.00 0.50 1.74 -- -98.50 -77.00 60.00 50 47 \w -88.00 -61.00 0.50 1.74 -- -98.50 -74.00 135.65 54 48 \w -84.00 -58.00 0.50 1.74 -- -98.50 -82.00 167.07 52 49 \w -95.00 -60.00 0.50 1.74 -- -98.50 -77.00 90.00 70 50 \w -109.00 -60.00 0.50 1.74 -- -98.50 -77.00 30.00 98 51 \w -115.00 -60.00 0.50 1.74 -- -98.50 -77.00 5.04 110 52 \w -116.00 -79.00 0.50 1.74 -- -37.97 -77.00 60.00 74 53 \w -129.00 -59.00 0.50 1.74 -- -98.50 -79.00 -75.98 140 54 \w -134.00 -61.00 0.50 1.74 -- -98.50 -74.00 -16.41 146 55 \w -155.00-129.00 0.50 1.74 -- -98.50 -82.00 167.07 52 56 \w -123.00 -60.00 0.50 1.74 -- -98.50 -78.00 173.17 126 57 \w -150.00 -62.00 0.50 1.74 -- -98.50 -72.00 144.15 176 58 \w -157.00-131.00 0.50 1.74 -- -98.50 -77.00 90.00 52 59 \w -161.00 -63.00 0.50 1.74 -- -98.50 -70.00 116.58 196 60 \w -151.00 -63.00 0.50 1.74 -- -98.50 -71.00 64.29 176 61 \w -171.00-126.00 0.50 1.74 -- -98.50 -83.00 -39.38 90 62 \w -170.00-118.00 0.50 1.74 -- -98.50 -70.00 35.43 104 63 \w -158.00-133.00 0.50 1.74 -- -98.50 -81.00 113.98 50 64 \w -177.00-151.00 0.50 1.74 -- -98.50 -78.00 173.17 52 65 \w -174.00-107.00 0.50 1.74 -- -98.50 -83.00 85.56 134 66 \w -162.00-132.00 0.50 1.74 -- -98.50 -77.00 5.04 60 67 \w -167.00-102.00 0.50 1.74 -- -98.50 -83.00 -19.14 130 68 \w -171.00 -62.00 0.50 1.74 -- -98.50 -73.00 12.64 218 69 \w -176.00-113.00 0.50 1.74 -- -98.50 -83.00-128.82 126 70 \w -176.00 -60.00 0.50 1.74 -- -98.50 -78.00 -64.86 232 71 \w -167.00 -58.00 0.50 1.74 -- -98.50 -82.00 106.04 218 72 \w -176.00-105.00 0.50 1.74 -- -98.50 -77.00 60.00 142 73 \w -163.00-104.00 0.50 1.74 -- -98.50 -74.00 135.65 118 74 \w -175.00-114.00 0.50 1.74 -- -98.50 -77.00 30.00 122 75 \w -174.00-147.00 0.50 1.74 -- -98.50 -77.00 -98.40 54 76 \w -177.00-106.00 0.50 1.74 -- -98.50 -77.00-150.00 142 77 \w -127.00 -61.00 0.50 1.74 -- -98.50 -75.00 -37.94 132 78 \w -163.00-103.00 0.50 1.74 -- -98.50 -77.00-120.00 120 79 \w -172.00 -62.00 0.50 1.74 -- -98.50 -73.00-164.63 220 80 \w -74.00 -49.00 0.50 1.74 -- -98.50 109.00 -80.00 50 ; _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 0.0933141000 _diffrn_orient_matrix_UB_12 0.0797287000 _diffrn_orient_matrix_UB_13 0.1182367000 _diffrn_orient_matrix_UB_21 0.0286178000 _diffrn_orient_matrix_UB_22 0.1001170000 _diffrn_orient_matrix_UB_23 -0.0653446000 _diffrn_orient_matrix_UB_31 -0.1131384000 _diffrn_orient_matrix_UB_32 0.0291342000 _diffrn_orient_matrix_UB_33 0.0025373000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_unetI/netI 0.0168 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.937 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 33367 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.937 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.354 _diffrn_reflns_theta_min 3.766 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.557 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74626 _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 colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.514 _exptl_crystal_description block _exptl_crystal_F_000 764 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.635 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 6283 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+1.5536P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.0899 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5788 _reflns_number_total 6283 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj05578j2.cif _cod_data_source_block exp_4148-liuli-1 _cod_original_cell_volume 1644.87(6) _cod_database_code 7061201 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C H O P Br Cu' _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 0.965 _shelx_estimated_absorpt_t_min 0.901 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C28(H28), C8(H8), C32(H32), C17(H17), C36(H36), C42(H42), C11(H11), C27(H27), C25(H25), C15(H15), C34(H34), C21(H21), C33(H33), C41(H41), C14(H14), C19(H19), C26(H26), C38(H38), C13(H13), C35(H35), C20(H20), C12(H12), C18(H18), C40(H40), C39(H39) 2.b Idealised Me refined as rotating group: C46(H46A,H46B,H46C), C44(H44A,H44B,H44C) ; _shelx_res_file ; exp_4148-liuli-1.res created by SHELXL-2014/7 TITL exp_4148-liuli-1_a.res in P-1 REM Old TITL exp_4148-liuli-1 in P-1 REM SHELXT solution in P-1 REM R1 0.090, Rweak 0.004, Alpha 0.036, Orientation as input REM Formula found by SHELXT: C40 O2 P2 Cu Br CELL 1.54184 12.1192 12.5675 12.6953 90.664 114.373 108.705 ZERR 2 0.0002 0.0003 0.0002 0.001 0.002 0.002 LATT 1 SFAC C H Br Cu O P UNIT 80 64 2 2 4 4 L.S. 4 PLAN 8 SIZE 0.01 0.02 0.03 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.044900 1.553600 FVAR 3.33500 BR1 3 0.354652 0.200496 0.356843 11.00000 0.03165 0.02845 = 0.03347 0.00897 0.01903 0.00726 CU2 4 0.238965 0.256506 0.452676 11.00000 0.02765 0.03005 = 0.02914 0.00911 0.01490 0.00579 P9 6 0.270182 0.213725 0.632690 11.00000 0.02583 0.02232 = 0.02670 0.00662 0.01345 0.00327 P30 6 0.077931 0.302966 0.313460 11.00000 0.02685 0.02605 = 0.02830 0.00828 0.01410 0.00542 O45 5 0.635296 0.419819 1.051701 11.00000 0.04000 0.03479 = 0.02559 0.00919 0.01174 0.00224 O43 5 0.714062 0.608010 0.979123 11.00000 0.04170 0.02965 = 0.02895 0.00547 0.01223 -0.00577 C23 1 0.333575 0.470293 0.480992 11.00000 0.02432 0.02398 = 0.03080 0.00529 0.01429 0.00492 C4 1 0.444624 0.437915 0.699432 11.00000 0.02401 0.02554 = 0.02828 0.00686 0.01411 0.00667 C29 1 0.278245 0.508352 0.371368 11.00000 0.02564 0.03011 = 0.02836 0.00838 0.01490 0.00974 C5 1 0.549477 0.531903 0.779542 11.00000 0.03000 0.02228 = 0.03238 0.00740 0.01788 0.00379 AFIX 43 H5 2 0.576844 0.600041 0.753715 11.00000 -1.20000 AFIX 0 C28 1 0.343040 0.618151 0.358002 11.00000 0.02670 0.02917 = 0.03192 0.00695 0.01467 0.00711 AFIX 43 H28 2 0.420646 0.664703 0.419303 11.00000 -1.20000 AFIX 0 C10 1 0.329512 0.097877 0.680962 11.00000 0.03032 0.02288 = 0.03199 0.00673 0.01279 0.00420 C3 1 0.402756 0.335778 0.738422 11.00000 0.02525 0.02447 = 0.02990 0.00638 0.01541 0.00497 C16 1 0.140792 0.194145 0.677583 11.00000 0.02664 0.02820 = 0.02826 0.01019 0.01414 0.00396 C8 1 0.465181 0.329110 0.856877 11.00000 0.02822 0.02512 = 0.03112 0.00962 0.01574 0.00483 AFIX 43 H8 2 0.436662 0.261683 0.883335 11.00000 -1.20000 AFIX 0 C31 1 -0.033319 0.333538 0.360695 11.00000 0.02635 0.02794 = 0.02552 0.00528 0.01140 0.00449 C7 1 0.568251 0.420424 0.935468 11.00000 0.03158 0.03114 = 0.02745 0.00894 0.01457 0.00714 C6 1 0.611424 0.523382 0.895517 11.00000 0.03097 0.02669 = 0.02938 0.00453 0.01495 0.00240 C22 1 0.382898 0.449597 0.578639 11.00000 0.02509 0.02297 = 0.03219 0.00604 0.01601 0.00491 C32 1 -0.091278 0.249237 0.411916 11.00000 0.03292 0.02887 = 0.03397 0.00838 0.01697 0.00792 AFIX 43 H32 2 -0.067201 0.185609 0.424995 11.00000 -1.20000 AFIX 0 C24 1 0.159334 0.438754 0.280222 11.00000 0.02796 0.02898 = 0.03100 0.00901 0.01523 0.00610 C37 1 -0.034797 0.211304 0.171397 11.00000 0.03138 0.02835 = 0.03043 0.00600 0.01824 0.00207 C17 1 0.137413 0.283120 0.739839 11.00000 0.03016 0.02987 = 0.03055 0.00902 0.01502 0.00526 AFIX 43 H17 2 0.206932 0.352092 0.767232 11.00000 -1.20000 AFIX 0 C36 1 -0.065834 0.430251 0.346114 11.00000 0.03765 0.02871 = 0.03339 0.00895 0.01652 0.00880 AFIX 43 H36 2 -0.026161 0.487735 0.314014 11.00000 -1.20000 AFIX 0 C42 1 -0.144564 0.231293 0.093723 11.00000 0.03209 0.03264 = 0.03206 0.00572 0.01547 0.00417 AFIX 43 H42 2 -0.161016 0.294591 0.112366 11.00000 -1.20000 AFIX 0 C11 1 0.403471 0.072853 0.630808 11.00000 0.03636 0.02869 = 0.03548 0.00960 0.01684 0.00842 AFIX 43 H11 2 0.411917 0.108450 0.569308 11.00000 -1.20000 AFIX 0 C27 1 0.291551 0.657066 0.253812 11.00000 0.03081 0.03010 = 0.03791 0.01251 0.01739 0.00586 AFIX 43 H27 2 0.333951 0.730153 0.245289 11.00000 -1.20000 AFIX 0 C25 1 0.110557 0.479646 0.175128 11.00000 0.03044 0.03706 = 0.03194 0.01136 0.00980 0.00126 AFIX 43 H25 2 0.032780 0.434096 0.113325 11.00000 -1.20000 AFIX 0 C15 1 0.316654 0.043181 0.772575 11.00000 0.03283 0.02761 = 0.03751 0.01056 0.01655 0.00443 AFIX 43 H15 2 0.266941 0.058499 0.806076 11.00000 -1.20000 AFIX 0 C34 1 -0.218627 0.355274 0.425675 11.00000 0.03430 0.04097 = 0.02984 0.00333 0.01569 0.01316 AFIX 43 H34 2 -0.282705 0.361715 0.444859 11.00000 -1.20000 AFIX 0 C21 1 0.035911 0.089823 0.639306 11.00000 0.03238 0.03017 = 0.03589 0.00744 0.01502 0.00343 AFIX 43 H21 2 0.037474 0.028746 0.598592 11.00000 -1.20000 AFIX 0 C33 1 -0.184471 0.260054 0.443299 11.00000 0.03443 0.03460 = 0.03330 0.00821 0.01866 0.00733 AFIX 43 H33 2 -0.223865 0.203215 0.476166 11.00000 -1.20000 AFIX 0 C41 1 -0.229531 0.157223 -0.011370 11.00000 0.03392 0.04199 = 0.03174 0.00574 0.01525 -0.00002 AFIX 43 H41 2 -0.301369 0.172128 -0.063748 11.00000 -1.20000 AFIX 0 C14 1 0.378481 -0.034458 0.813759 11.00000 0.03953 0.03194 = 0.04314 0.01837 0.01686 0.00580 AFIX 43 H14 2 0.370467 -0.070322 0.875262 11.00000 -1.20000 AFIX 0 C19 1 -0.072993 0.167508 0.722569 11.00000 0.03376 0.05134 = 0.04598 0.02109 0.02464 0.01282 AFIX 43 H19 2 -0.144441 0.159005 0.736863 11.00000 -1.20000 AFIX 0 C26 1 0.176647 0.587169 0.161921 11.00000 0.03522 0.04108 = 0.03259 0.01732 0.01176 0.00624 AFIX 43 H26 2 0.143762 0.612658 0.090979 11.00000 -1.20000 AFIX 0 C38 1 -0.013836 0.114676 0.143762 11.00000 0.03134 0.03424 = 0.04971 0.00591 0.02258 0.00471 AFIX 43 H38 2 0.058991 0.100301 0.194863 11.00000 -1.20000 AFIX 0 C13 1 0.451608 -0.058458 0.763753 11.00000 0.03613 0.02969 = 0.05315 0.01484 0.01435 0.00936 AFIX 43 H13 2 0.492277 -0.110579 0.791427 11.00000 -1.20000 AFIX 0 C46 1 0.588213 0.317624 1.093063 11.00000 0.04478 0.03440 = 0.02953 0.01155 0.01537 0.00813 AFIX 137 H46A 2 0.593905 0.255190 1.053898 11.00000 -1.50000 H46B 2 0.499446 0.302413 1.077002 11.00000 -1.50000 H46C 2 0.639672 0.326642 1.176062 11.00000 -1.50000 AFIX 0 C35 1 -0.157903 0.441177 0.379577 11.00000 0.04416 0.03424 = 0.03725 0.00610 0.01803 0.01691 AFIX 43 H35 2 -0.178742 0.506628 0.370899 11.00000 -1.20000 AFIX 0 C20 1 -0.069609 0.077365 0.661770 11.00000 0.02975 0.03922 = 0.04864 0.01780 0.01979 0.00107 AFIX 43 H20 2 -0.138604 0.008083 0.635893 11.00000 -1.20000 AFIX 0 C12 1 0.464393 -0.004820 0.672249 11.00000 0.03866 0.03281 = 0.05096 0.01094 0.02164 0.01249 AFIX 43 H12 2 0.513727 -0.020900 0.638729 11.00000 -1.20000 AFIX 0 C18 1 0.030123 0.270251 0.762010 11.00000 0.03965 0.04393 = 0.03833 0.01421 0.02267 0.01648 AFIX 43 H18 2 0.028261 0.330791 0.803241 11.00000 -1.20000 AFIX 0 C40 1 -0.207422 0.061268 -0.038238 11.00000 0.04146 0.04441 = 0.03983 -0.00494 0.02207 -0.00658 AFIX 43 H40 2 -0.263966 0.011857 -0.108781 11.00000 -1.20000 AFIX 0 C39 1 -0.101226 0.039297 0.040038 11.00000 0.04321 0.03538 = 0.06161 -0.00683 0.03049 0.00130 AFIX 43 H39 2 -0.087954 -0.026526 0.023287 11.00000 -1.20000 AFIX 0 C44 1 0.766856 0.710875 0.940394 11.00000 0.04394 0.03253 = 0.03453 0.00602 0.01557 -0.00675 AFIX 137 H44A 2 0.790560 0.692986 0.880832 11.00000 -1.50000 H44B 2 0.842232 0.762288 1.005553 11.00000 -1.50000 H44C 2 0.703036 0.746050 0.908932 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_4148-liuli-1_a.res in P-1 REM R1 = 0.0335 for 5788 Fo > 4sig(Fo) and 0.0362 for all 6283 data REM 417 parameters refined using 0 restraints END WGHT 0.0447 1.5651 REM Highest difference peak 0.635, deepest hole -0.982, 1-sigma level 0.063 Q1 1 0.4035 0.1970 0.4317 11.00000 0.05 0.63 Q2 1 0.0125 0.2777 0.2494 11.00000 0.05 0.57 Q3 1 0.3045 0.1972 0.2693 11.00000 0.05 0.49 Q4 1 0.1228 0.2764 0.3884 11.00000 0.05 0.49 Q5 1 0.3897 0.1504 0.3357 11.00000 0.05 0.49 Q6 1 0.2809 0.2374 0.5354 11.00000 0.05 0.46 Q7 1 0.1158 0.2247 0.3564 11.00000 0.05 0.45 Q8 1 0.2731 0.2004 0.4486 11.00000 0.05 0.43 ; _shelx_res_checksum 91272 _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 1.364 _oxdiff_exptl_absorpt_empirical_full_min 0.766 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 0.35465(2) 0.20050(2) 0.35684(2) 0.03039(8) Uani 1 1 d . . . . . Cu2 Cu 0.23896(3) 0.25651(3) 0.45268(3) 0.02925(10) Uani 1 1 d . . . . . P9 P 0.27018(5) 0.21373(5) 0.63269(5) 0.02567(13) Uani 1 1 d . . . . . P30 P 0.07793(6) 0.30297(5) 0.31346(5) 0.02740(13) Uani 1 1 d . . . . . O45 O 0.63530(17) 0.41982(15) 1.05170(14) 0.0374(4) Uani 1 1 d . . . . . O43 O 0.71406(18) 0.60801(15) 0.97912(15) 0.0396(4) Uani 1 1 d . . . . . C23 C 0.3336(2) 0.47029(18) 0.4810(2) 0.0266(5) Uani 1 1 d . . . . . C4 C 0.4446(2) 0.43792(19) 0.69943(19) 0.0256(4) Uani 1 1 d . . . . . C29 C 0.2782(2) 0.50835(19) 0.3714(2) 0.0270(5) Uani 1 1 d . . . . . C5 C 0.5495(2) 0.53190(19) 0.7795(2) 0.0282(5) Uani 1 1 d . . . . . H5 H 0.5768 0.6000 0.7537 0.034 Uiso 1 1 calc R . . . . C28 C 0.3430(2) 0.6182(2) 0.3580(2) 0.0294(5) Uani 1 1 d . . . . . H28 H 0.4206 0.6647 0.4193 0.035 Uiso 1 1 calc R . . . . C10 C 0.3295(2) 0.09788(19) 0.6810(2) 0.0301(5) Uani 1 1 d . . . . . C3 C 0.4028(2) 0.33578(19) 0.7384(2) 0.0264(4) Uani 1 1 d . . . . . C16 C 0.1408(2) 0.19415(19) 0.6776(2) 0.0285(5) Uani 1 1 d . . . . . C8 C 0.4652(2) 0.32911(19) 0.8569(2) 0.0284(5) Uani 1 1 d . . . . . H8 H 0.4367 0.2617 0.8833 0.034 Uiso 1 1 calc R . . . . C31 C -0.0333(2) 0.33354(19) 0.36070(19) 0.0280(5) Uani 1 1 d . . . . . C7 C 0.5683(2) 0.4204(2) 0.9355(2) 0.0305(5) Uani 1 1 d . . . . . C6 C 0.6114(2) 0.5234(2) 0.8955(2) 0.0305(5) Uani 1 1 d . . . . . C22 C 0.3829(2) 0.44960(18) 0.5786(2) 0.0265(5) Uani 1 1 d . . . . . C32 C -0.0913(2) 0.2492(2) 0.4119(2) 0.0319(5) Uani 1 1 d . . . . . H32 H -0.0672 0.1856 0.4250 0.038 Uiso 1 1 calc R . . . . C24 C 0.1593(2) 0.4388(2) 0.2802(2) 0.0296(5) Uani 1 1 d . . . . . C37 C -0.0348(2) 0.2113(2) 0.1714(2) 0.0307(5) Uani 1 1 d . . . . . C17 C 0.1374(2) 0.2831(2) 0.7398(2) 0.0310(5) Uani 1 1 d . . . . . H17 H 0.2069 0.3521 0.7672 0.037 Uiso 1 1 calc R . . . . C36 C -0.0658(2) 0.4303(2) 0.3461(2) 0.0337(5) Uani 1 1 d . . . . . H36 H -0.0262 0.4877 0.3140 0.040 Uiso 1 1 calc R . . . . C42 C -0.1446(2) 0.2313(2) 0.0937(2) 0.0338(5) Uani 1 1 d . . . . . H42 H -0.1610 0.2946 0.1124 0.041 Uiso 1 1 calc R . . . . C11 C 0.4035(2) 0.0729(2) 0.6308(2) 0.0340(5) Uani 1 1 d . . . . . H11 H 0.4119 0.1084 0.5693 0.041 Uiso 1 1 calc R . . . . C27 C 0.2916(2) 0.6571(2) 0.2538(2) 0.0334(5) Uani 1 1 d . . . . . H27 H 0.3340 0.7302 0.2453 0.040 Uiso 1 1 calc R . . . . C25 C 0.1106(2) 0.4796(2) 0.1751(2) 0.0374(6) Uani 1 1 d . . . . . H25 H 0.0328 0.4341 0.1133 0.045 Uiso 1 1 calc R . . . . C15 C 0.3167(2) 0.0432(2) 0.7726(2) 0.0339(5) Uani 1 1 d . . . . . H15 H 0.2669 0.0585 0.8061 0.041 Uiso 1 1 calc R . . . . C34 C -0.2186(2) 0.3553(2) 0.4257(2) 0.0346(5) Uani 1 1 d . . . . . H34 H -0.2827 0.3617 0.4449 0.041 Uiso 1 1 calc R . . . . C21 C 0.0359(2) 0.0898(2) 0.6393(2) 0.0349(5) Uani 1 1 d . . . . . H21 H 0.0375 0.0287 0.5986 0.042 Uiso 1 1 calc R . . . . C33 C -0.1845(2) 0.2601(2) 0.4433(2) 0.0341(5) Uani 1 1 d . . . . . H33 H -0.2239 0.2032 0.4762 0.041 Uiso 1 1 calc R . . . . C41 C -0.2295(3) 0.1572(2) -0.0114(2) 0.0392(6) Uani 1 1 d . . . . . H41 H -0.3014 0.1721 -0.0637 0.047 Uiso 1 1 calc R . . . . C14 C 0.3785(3) -0.0345(2) 0.8138(2) 0.0404(6) Uani 1 1 d . . . . . H14 H 0.3705 -0.0703 0.8753 0.049 Uiso 1 1 calc R . . . . C19 C -0.0730(3) 0.1675(2) 0.7226(2) 0.0417(6) Uani 1 1 d . . . . . H19 H -0.1444 0.1590 0.7369 0.050 Uiso 1 1 calc R . . . . C26 C 0.1766(3) 0.5872(2) 0.1619(2) 0.0393(6) Uani 1 1 d . . . . . H26 H 0.1438 0.6127 0.0910 0.047 Uiso 1 1 calc R . . . . C38 C -0.0138(3) 0.1147(2) 0.1438(2) 0.0386(6) Uani 1 1 d . . . . . H38 H 0.0590 0.1003 0.1949 0.046 Uiso 1 1 calc R . . . . C13 C 0.4516(3) -0.0585(2) 0.7638(3) 0.0421(6) Uani 1 1 d . . . . . H13 H 0.4923 -0.1106 0.7914 0.051 Uiso 1 1 calc R . . . . C46 C 0.5882(3) 0.3176(2) 1.0931(2) 0.0381(6) Uani 1 1 d . . . . . H46A H 0.5939 0.2552 1.0539 0.057 Uiso 1 1 calc GR . . . . H46B H 0.4994 0.3024 1.0770 0.057 Uiso 1 1 calc GR . . . . H46C H 0.6397 0.3266 1.1761 0.057 Uiso 1 1 calc GR . . . . C35 C -0.1579(3) 0.4412(2) 0.3796(2) 0.0377(6) Uani 1 1 d . . . . . H35 H -0.1787 0.5066 0.3709 0.045 Uiso 1 1 calc R . . . . C20 C -0.0696(2) 0.0774(2) 0.6618(2) 0.0412(6) Uani 1 1 d . . . . . H20 H -0.1386 0.0081 0.6359 0.049 Uiso 1 1 calc R . . . . C12 C 0.4644(3) -0.0048(2) 0.6722(3) 0.0401(6) Uani 1 1 d . . . . . H12 H 0.5137 -0.0209 0.6387 0.048 Uiso 1 1 calc R . . . . C18 C 0.0301(3) 0.2703(2) 0.7620(2) 0.0382(6) Uani 1 1 d . . . . . H18 H 0.0283 0.3308 0.8032 0.046 Uiso 1 1 calc R . . . . C40 C -0.2074(3) 0.0613(2) -0.0382(3) 0.0464(7) Uani 1 1 d . . . . . H40 H -0.2640 0.0119 -0.1088 0.056 Uiso 1 1 calc R . . . . C39 C -0.1012(3) 0.0393(2) 0.0400(3) 0.0476(7) Uani 1 1 d . . . . . H39 H -0.0880 -0.0265 0.0233 0.057 Uiso 1 1 calc R . . . . C44 C 0.7669(3) 0.7109(2) 0.9404(2) 0.0431(6) Uani 1 1 d . . . . . H44A H 0.7906 0.6930 0.8808 0.065 Uiso 1 1 calc GR . . . . H44B H 0.8422 0.7623 1.0056 0.065 Uiso 1 1 calc GR . . . . H44C H 0.7030 0.7460 0.9089 0.065 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 Br1 0.03165(14) 0.02845(13) 0.03347(14) 0.00897(10) 0.01903(11) 0.00726(10) Cu2 0.02765(18) 0.03005(19) 0.02914(19) 0.00911(14) 0.01490(15) 0.00579(14) P9 0.0258(3) 0.0223(3) 0.0267(3) 0.0066(2) 0.0134(2) 0.0033(2) P30 0.0268(3) 0.0261(3) 0.0283(3) 0.0083(2) 0.0141(2) 0.0054(2) O45 0.0400(10) 0.0348(9) 0.0256(8) 0.0092(7) 0.0117(7) 0.0022(8) O43 0.0417(10) 0.0296(9) 0.0290(9) 0.0055(7) 0.0122(8) -0.0058(7) C23 0.0243(10) 0.0240(10) 0.0308(12) 0.0053(9) 0.0143(9) 0.0049(9) C4 0.0240(10) 0.0255(11) 0.0283(11) 0.0069(9) 0.0141(9) 0.0067(9) C29 0.0256(11) 0.0301(11) 0.0284(11) 0.0084(9) 0.0149(9) 0.0097(9) C5 0.0300(11) 0.0223(10) 0.0324(12) 0.0074(9) 0.0179(10) 0.0038(9) C28 0.0267(11) 0.0292(11) 0.0319(12) 0.0070(9) 0.0147(10) 0.0071(9) C10 0.0303(12) 0.0229(10) 0.0320(12) 0.0067(9) 0.0128(10) 0.0042(9) C3 0.0253(11) 0.0245(10) 0.0299(11) 0.0064(9) 0.0154(9) 0.0050(9) C16 0.0266(11) 0.0282(11) 0.0283(11) 0.0102(9) 0.0141(9) 0.0040(9) C8 0.0282(11) 0.0251(11) 0.0311(12) 0.0096(9) 0.0157(10) 0.0048(9) C31 0.0264(11) 0.0279(11) 0.0255(11) 0.0053(9) 0.0114(9) 0.0045(9) C7 0.0316(12) 0.0311(12) 0.0275(12) 0.0089(9) 0.0146(10) 0.0071(10) C6 0.0310(12) 0.0267(11) 0.0294(12) 0.0045(9) 0.0150(10) 0.0024(9) C22 0.0251(11) 0.0230(10) 0.0322(12) 0.0060(9) 0.0160(10) 0.0049(9) C32 0.0329(12) 0.0289(11) 0.0340(12) 0.0084(10) 0.0170(10) 0.0079(10) C24 0.0280(11) 0.0290(11) 0.0310(12) 0.0090(9) 0.0152(10) 0.0061(9) C37 0.0314(12) 0.0284(11) 0.0304(12) 0.0060(9) 0.0182(10) 0.0021(9) C17 0.0302(12) 0.0299(11) 0.0306(12) 0.0090(9) 0.0150(10) 0.0053(9) C36 0.0376(13) 0.0287(12) 0.0334(12) 0.0090(10) 0.0165(11) 0.0088(10) C42 0.0321(12) 0.0326(12) 0.0321(12) 0.0057(10) 0.0155(10) 0.0042(10) C11 0.0364(13) 0.0287(12) 0.0355(13) 0.0096(10) 0.0168(11) 0.0084(10) C27 0.0308(12) 0.0301(12) 0.0379(13) 0.0125(10) 0.0174(10) 0.0059(10) C25 0.0304(12) 0.0371(13) 0.0319(13) 0.0114(10) 0.0098(10) 0.0013(10) C15 0.0328(12) 0.0276(12) 0.0375(13) 0.0106(10) 0.0166(11) 0.0044(10) C34 0.0343(13) 0.0410(13) 0.0298(12) 0.0033(10) 0.0157(10) 0.0132(11) C21 0.0324(12) 0.0302(12) 0.0359(13) 0.0074(10) 0.0150(10) 0.0034(10) C33 0.0344(13) 0.0346(12) 0.0333(12) 0.0082(10) 0.0187(11) 0.0073(10) C41 0.0339(13) 0.0420(14) 0.0317(13) 0.0057(11) 0.0152(11) 0.0000(11) C14 0.0395(14) 0.0319(13) 0.0431(14) 0.0184(11) 0.0169(12) 0.0058(11) C19 0.0338(13) 0.0513(16) 0.0460(15) 0.0211(13) 0.0246(12) 0.0128(12) C26 0.0352(13) 0.0411(14) 0.0326(13) 0.0173(11) 0.0118(11) 0.0062(11) C38 0.0313(13) 0.0342(13) 0.0497(15) 0.0059(11) 0.0226(12) 0.0047(10) C13 0.0361(14) 0.0297(13) 0.0531(16) 0.0148(11) 0.0143(12) 0.0094(11) C46 0.0448(15) 0.0344(13) 0.0295(12) 0.0116(10) 0.0154(11) 0.0081(11) C35 0.0442(14) 0.0342(13) 0.0372(13) 0.0061(10) 0.0180(12) 0.0169(11) C20 0.0298(12) 0.0392(14) 0.0486(15) 0.0178(12) 0.0198(12) 0.0011(11) C12 0.0387(14) 0.0328(13) 0.0510(16) 0.0109(11) 0.0216(12) 0.0125(11) C18 0.0397(14) 0.0439(14) 0.0383(14) 0.0142(11) 0.0227(12) 0.0165(12) C40 0.0415(15) 0.0444(15) 0.0398(15) -0.0049(12) 0.0221(13) -0.0066(12) C39 0.0432(15) 0.0354(14) 0.0616(19) -0.0068(13) 0.0305(14) 0.0013(12) C44 0.0439(15) 0.0325(13) 0.0345(13) 0.0060(11) 0.0156(12) -0.0068(11) 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' 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' 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 Br1 Cu2 C23 101.86(5) . . ? Br1 Cu2 C22 108.01(5) . . ? P9 Cu2 Br1 118.91(2) . . ? P9 Cu2 P30 131.54(3) . . ? P9 Cu2 C23 105.56(6) . . ? P9 Cu2 C22 79.22(5) . . ? P30 Cu2 Br1 107.41(2) . . ? P30 Cu2 C23 76.45(5) . . ? P30 Cu2 C22 100.24(6) . . ? C23 Cu2 C22 27.71(7) . . ? C10 P9 Cu2 119.37(8) . . ? C3 P9 Cu2 106.71(7) . . ? C3 P9 C10 101.27(11) . . ? C3 P9 C16 102.99(11) . . ? C16 P9 Cu2 119.01(8) . . ? C16 P9 C10 104.86(11) . . ? C31 P30 Cu2 115.60(8) . . ? C31 P30 C24 103.90(11) . . ? C31 P30 C37 101.43(11) . . ? C24 P30 Cu2 105.58(8) . . ? C24 P30 C37 105.84(10) . . ? C37 P30 Cu2 122.75(9) . . ? C7 O45 C46 115.83(19) . . ? C6 O43 C44 116.74(19) . . ? C29 C23 Cu2 109.68(15) . . ? C22 C23 Cu2 76.67(15) . . ? C22 C23 C29 173.1(2) . . ? C5 C4 C22 118.8(2) . . ? C3 C4 C5 119.8(2) . . ? C3 C4 C22 121.3(2) . . ? C28 C29 C23 118.8(2) . . ? C28 C29 C24 120.3(2) . . ? C24 C29 C23 120.9(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 C4 120.3(2) . . ? C6 C5 H5 119.8 . . ? C29 C28 H28 120.0 . . ? C27 C28 C29 120.0(2) . . ? C27 C28 H28 120.0 . . ? C11 C10 P9 116.92(17) . . ? C15 C10 P9 123.4(2) . . ? C15 C10 C11 119.3(2) . . ? C4 C3 P9 119.22(17) . . ? C8 C3 P9 121.65(16) . . ? C8 C3 C4 119.1(2) . . ? C17 C16 P9 121.35(17) . . ? C17 C16 C21 118.7(2) . . ? C21 C16 P9 119.65(19) . . ? C3 C8 H8 119.3 . . ? C7 C8 C3 121.3(2) . . ? C7 C8 H8 119.3 . . ? C32 C31 P30 115.55(18) . . ? C36 C31 P30 125.02(18) . . ? C36 C31 C32 119.4(2) . . ? O45 C7 C8 124.7(2) . . ? O45 C7 C6 115.8(2) . . ? C8 C7 C6 119.5(2) . . ? O43 C6 C5 125.0(2) . . ? O43 C6 C7 115.1(2) . . ? C5 C6 C7 119.9(2) . . ? C23 C22 Cu2 75.62(15) . . ? C23 C22 C4 173.6(2) . . ? C4 C22 Cu2 110.38(14) . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.8 . . ? C29 C24 P30 115.90(17) . . ? C25 C24 P30 125.57(18) . . ? C25 C24 C29 118.5(2) . . ? C42 C37 P30 122.49(19) . . ? C38 C37 P30 118.4(2) . . ? C38 C37 C42 119.0(2) . . ? C16 C17 H17 119.7 . . ? C16 C17 C18 120.6(2) . . ? C18 C17 H17 119.7 . . ? C31 C36 H36 120.1 . . ? C31 C36 C35 119.8(2) . . ? C35 C36 H36 120.1 . . ? C37 C42 H42 119.8 . . ? C41 C42 C37 120.4(3) . . ? C41 C42 H42 119.8 . . ? C10 C11 H11 119.8 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C28 C27 H27 120.0 . . ? C28 C27 C26 120.0(2) . . ? C26 C27 H27 120.0 . . ? C24 C25 H25 119.6 . . ? C26 C25 C24 120.8(2) . . ? C26 C25 H25 119.6 . . ? C10 C15 H15 120.1 . . ? C14 C15 C10 119.9(2) . . ? C14 C15 H15 120.1 . . ? C33 C34 H34 119.9 . . ? C33 C34 C35 120.2(2) . . ? C35 C34 H34 119.9 . . ? C16 C21 H21 119.8 . . ? C20 C21 C16 120.5(3) . . ? C20 C21 H21 119.8 . . ? C32 C33 H33 120.1 . . ? C34 C33 C32 119.8(2) . . ? C34 C33 H33 120.1 . . ? C42 C41 H41 120.0 . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H41 120.0 . . ? C15 C14 H14 119.8 . . ? C13 C14 C15 120.4(2) . . ? C13 C14 H14 119.8 . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.9(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26 119.8 . . ? C37 C38 H38 119.9 . . ? C37 C38 C39 120.2(3) . . ? C39 C38 H38 119.9 . . ? C14 C13 H13 120.0 . . ? C14 C13 C12 120.1(2) . . ? C12 C13 H13 120.0 . . ? O45 C46 H46A 109.5 . . ? O45 C46 H46B 109.5 . . ? O45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C36 C35 H35 119.8 . . ? C34 C35 C36 120.3(2) . . ? C34 C35 H35 119.8 . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18 120.0 . . ? C41 C40 H40 120.2 . . ? C39 C40 C41 119.7(3) . . ? C39 C40 H40 120.2 . . ? C38 C39 H39 119.7 . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39 119.7 . . ? O43 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? O43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? 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 Cu2 2.4418(4) . ? Cu2 P9 2.2584(6) . ? Cu2 P30 2.2762(7) . ? Cu2 C23 2.515(2) . ? Cu2 C22 2.526(2) . ? P9 C10 1.828(2) . ? P9 C3 1.824(2) . ? P9 C16 1.827(2) . ? P30 C31 1.822(2) . ? P30 C24 1.829(2) . ? P30 C37 1.832(2) . ? O45 C7 1.361(3) . ? O45 C46 1.430(3) . ? O43 C6 1.357(3) . ? O43 C44 1.437(3) . ? C23 C29 1.437(3) . ? C23 C22 1.207(3) . ? C4 C5 1.410(3) . ? C4 C3 1.398(3) . ? C4 C22 1.436(3) . ? C29 C28 1.404(3) . ? C29 C24 1.404(3) . ? C5 H5 0.9300 . ? C5 C6 1.373(3) . ? C28 H28 0.9300 . ? C28 C27 1.381(3) . ? C10 C11 1.398(4) . ? C10 C15 1.396(3) . ? C3 C8 1.395(3) . ? C16 C17 1.383(3) . ? C16 C21 1.406(3) . ? C8 H8 0.9300 . ? C8 C7 1.378(3) . ? C31 C32 1.398(3) . ? C31 C36 1.385(3) . ? C7 C6 1.416(3) . ? C32 H32 0.9300 . ? C32 C33 1.386(4) . ? C24 C25 1.398(3) . ? C37 C42 1.394(4) . ? C37 C38 1.387(4) . ? C17 H17 0.9300 . ? C17 C18 1.402(3) . ? C36 H36 0.9300 . ? C36 C35 1.390(4) . ? C42 H42 0.9300 . ? C42 C41 1.389(4) . ? C11 H11 0.9300 . ? C11 C12 1.389(4) . ? C27 H27 0.9300 . ? C27 C26 1.387(4) . ? C25 H25 0.9300 . ? C25 C26 1.385(3) . ? C15 H15 0.9300 . ? C15 C14 1.394(4) . ? C34 H34 0.9300 . ? C34 C33 1.379(4) . ? C34 C35 1.382(4) . ? C21 H21 0.9300 . ? C21 C20 1.384(4) . ? C33 H33 0.9300 . ? C41 H41 0.9300 . ? C41 C40 1.384(4) . ? C14 H14 0.9300 . ? C14 C13 1.382(4) . ? C19 H19 0.9300 . ? C19 C20 1.384(4) . ? C19 C18 1.383(4) . ? C26 H26 0.9300 . ? C38 H38 0.9300 . ? C38 C39 1.389(4) . ? C13 H13 0.9300 . ? C13 C12 1.388(4) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C35 H35 0.9300 . ? C20 H20 0.9300 . ? C12 H12 0.9300 . ? C18 H18 0.9300 . ? C40 H40 0.9300 . ? C40 C39 1.378(5) . ? C39 H39 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ?