#------------------------------------------------------------------------------ #$Date: 2024-05-05 05:10:00 +0300 (Sun, 05 May 2024) $ #$Revision: 291589 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248358.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_7248358 loop_ _publ_author_name 'Mou, Wen-Long' 'Gao, Cheng-Jie' 'Li, Zi-Xi' 'Fan, Si-Jie' 'Hou, Chuan-Bin' 'Zhao, Jing-Tong' 'Zhang, Shuai' 'Li, Zhong-Feng' 'Han, Hong-Liang' 'Duan, Chun-Bo' 'Wang, Guo' 'Jin, Qiong-Hua' _publ_section_title ; Synthesis and luminescent properties of three excellent yellow emissive Cu(i) complexes based on the diphosphine ligand and the diimine ligand ; _journal_issue 17 _journal_name_full CrystEngComm _journal_page_first 2297 _journal_page_last 2305 _journal_paper_doi 10.1039/D4CE00206G _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C82 H64 Br2 Cu2 N2 O2 P4, 4(C H2 Cl2)' _chemical_formula_sum 'C86 H72 Br2 Cl8 Cu2 N2 O2 P4' _chemical_formula_weight 1859.83 _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 _audit_creation_date 2022-10-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-11-09 deposited with the CCDC. 2024-03-28 downloaded from the CCDC. ; _cell_angle_alpha 101.2510(10) _cell_angle_beta 104.3770(10) _cell_angle_gamma 105.0070(10) _cell_formula_units_Z 1 _cell_length_a 9.69430(10) _cell_length_b 13.05540(10) _cell_length_c 18.6809(2) _cell_measurement_reflns_used 16645 _cell_measurement_temperature 293 _cell_measurement_theta_max 74.2670 _cell_measurement_theta_min 4.9620 _cell_volume 2125.44(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.33c (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)' _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.966 _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 -89.00 13.00 0.50 1.00 -- 0.00 -19.00 90.00 204 2 \w -28.00 89.00 0.50 1.00 -- 0.00 77.00 -30.00 234 3 \w -28.00 89.00 0.50 1.00 -- 0.00 77.00 120.00 234 4 \w 31.00 89.00 0.50 1.00 -- 0.00 19.00-120.00 116 5 \w 88.00 116.00 0.50 1.00 -- 94.00 -82.00 -30.00 56 6 \w 5.00 40.00 0.50 1.00 -- 94.00 -82.00 -30.00 70 7 \w 5.00 116.00 0.50 1.00 -- 94.00 -61.00 -90.00 222 8 \w 76.00 102.00 0.50 1.00 -- 94.00 -82.00-150.00 52 9 \w 75.00 169.00 0.50 1.00 -- 94.00 52.00 22.57 188 10 \w 27.00 117.00 0.50 1.00 -- 94.00 -82.00 60.00 180 11 \w 108.00 161.00 0.50 1.00 -- 94.00 45.00 120.00 106 12 \w 46.00 107.00 0.50 1.00 -- 94.00 -30.00 30.00 122 13 \w 7.00 105.00 0.50 1.00 -- 94.00 -82.00-180.00 196 14 \w 5.00 112.00 0.50 1.00 -- 94.00 -82.00 -90.00 214 15 \w 5.00 87.00 0.50 1.00 -- 94.00 -61.00-180.00 164 16 \w 90.00 116.00 0.50 1.00 -- 94.00 30.00 120.00 52 17 \w 142.00 182.00 0.50 1.00 -- 94.00 30.00 120.00 80 18 \w 83.00 108.00 0.50 1.00 -- 94.00 -30.00 -60.00 50 19 \w 9.00 116.00 0.50 1.00 -- 94.00 -61.00 60.00 214 20 \w 71.00 97.00 0.50 1.00 -- 94.00 -82.00 120.00 52 21 \w 96.00 177.00 0.50 1.00 -- 94.00 45.00 0.00 162 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0683939000 _diffrn_orient_matrix_UB_12 0.1264322000 _diffrn_orient_matrix_UB_13 0.0199943000 _diffrn_orient_matrix_UB_21 0.0131923000 _diffrn_orient_matrix_UB_22 0.0087988000 _diffrn_orient_matrix_UB_23 0.0850359000 _diffrn_orient_matrix_UB_31 0.1587703000 _diffrn_orient_matrix_UB_32 -0.0102695000 _diffrn_orient_matrix_UB_33 0.0148427000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 24662 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.553 _diffrn_reflns_theta_min 4.822 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.115 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.33107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 1.453 _exptl_crystal_description block _exptl_crystal_F_000 942 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _refine_diff_density_max 1.467 _refine_diff_density_min -1.479 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 478 _refine_ls_number_reflns 8412 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0603 _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^)+(0.1162P)^2^+1.8719P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1748 _refine_ls_wR_factor_ref 0.1779 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7679 _reflns_number_total 8412 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00206g12.cif _cod_data_source_block lzx-147 _cod_depositor_comments 'Adding full bibliography for 7248357--7248359.cif.' _cod_database_code 7248358 _shelxl_version_number 2013-2 _chemical_oxdiff_formula 'C H N O P Cu Br Cl ' _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 0.386 _shelx_estimated_absorpt_t_min 0.240 _reflns_odcompleteness_completeness 99.61 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C42(H42A,H42B), C43(H43A,H43B) 2.b Aromatic/amide H refined with riding coordinates: C41(H41), C38(H38), C40(H40), C37(H37), C30(H30), C14(H14), C12(H12), C6(H6), C23(H23), C2(H2), C36(H36), C17(H17), C8(H8), C20(H20), C5(H5), C22(H22), C29(H29), C3(H3), C4(H4), C32(H32), C21(H21), C9(H9), C10(H10), C16(H16), C11(H11), C15(H15), C28(H28), C26(H26), C35(H35), C34(H34), C27(H27), C33(H33) ; _shelx_res_file ; TITL lzx-147_a.res in P-1 REM Old TITL lzx-147 in P-1 REM SHELXT solution in P-1 REM R1 0.164, Rweak 0.012, Alpha 0.082, Orientation as input REM Formula found by SHELXT: C41 N O4 P Cl3 Cu Br CELL 1.54184 9.6943 13.0554 18.6809 101.251 104.377 105.007 ZERR 1 0.0001 0.0001 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H Br Cl Cu N O P UNIT 86 72 2 8 2 2 2 4 L.S. 10 PLAN 5 SIZE 0.23 0.25 0.39 TEMP 19.85 list 4 fmap 2 53 ACTA REM REM REM WGHT 0.116200 1.871900 FVAR 0.50929 BR1 3 0.714670 0.049233 0.678126 11.00000 0.05437 0.05688 = 0.05475 0.00979 0.01458 0.03230 CU1 5 0.591893 0.185233 0.713261 11.00000 0.03127 0.03508 = 0.03376 0.00795 0.00840 0.00946 P1 8 0.585343 0.221174 0.836230 11.00000 0.02716 0.03591 = 0.03018 0.01101 0.00823 0.01028 P2 8 0.697692 0.343252 0.684317 11.00000 0.03377 0.03624 = 0.03468 0.01264 0.01004 0.00973 CL2 4 0.251573 0.277252 0.481034 11.00000 0.10778 0.11382 = 0.10667 0.03719 0.02385 0.02579 CL1 4 0.060810 0.270670 0.335117 11.00000 0.15835 0.09763 = 0.10286 0.03846 0.01769 0.00371 O1 7 0.476766 0.379669 0.769569 11.00000 0.04367 0.03773 = 0.03469 0.01326 0.01035 0.01470 N1 6 0.368686 0.116800 0.636007 11.00000 0.03123 0.03763 = 0.03611 0.00729 0.00266 0.00830 C13 1 0.645503 0.369719 0.881421 11.00000 0.03663 0.03776 = 0.03214 0.00912 0.01020 0.00731 C39 1 0.077106 0.023982 0.528433 11.00000 0.03068 0.03504 = 0.03315 0.00862 0.00184 0.00714 C1 1 0.684948 0.170889 0.911374 11.00000 0.03119 0.03813 = 0.03658 0.01204 0.00791 0.01160 C7 1 0.393138 0.168447 0.837010 11.00000 0.02967 0.03973 = 0.03686 0.01451 0.00878 0.01089 C41 1 0.252706 0.147568 0.647728 11.00000 0.03599 0.05023 = 0.03295 0.00147 0.00253 0.01466 AFIX 43 H41 2 0.270664 0.201628 0.692631 11.00000 -1.20000 AFIX 0 C18 1 0.588402 0.435026 0.839832 11.00000 0.04459 0.03650 = 0.03183 0.00812 0.01208 0.00972 C25 1 0.740323 0.321096 0.593531 11.00000 0.04433 0.04573 = 0.04318 0.01741 0.01628 0.01795 C38 1 0.196949 -0.007654 0.516155 11.00000 0.03801 0.04289 = 0.03851 -0.00427 0.00141 0.01297 AFIX 43 H38 2 0.182486 -0.060969 0.471497 11.00000 -1.20000 AFIX 0 C40 1 0.107881 0.103526 0.596871 11.00000 0.03343 0.05342 = 0.03853 0.00227 0.00672 0.01641 AFIX 43 H40 2 0.031204 0.127033 0.608395 11.00000 -1.20000 AFIX 0 C19 1 0.474901 0.432540 0.711503 11.00000 0.04559 0.03859 = 0.03592 0.01404 0.00973 0.01695 C37 1 0.338057 0.040084 0.570333 11.00000 0.03138 0.04464 = 0.04684 0.00172 0.00291 0.01291 AFIX 43 H37 2 0.416480 0.017389 0.560448 11.00000 -1.20000 AFIX 0 C24 1 0.577508 0.430265 0.670698 11.00000 0.04062 0.03607 = 0.03558 0.01233 0.00640 0.01112 C31 1 0.877373 0.435896 0.752310 11.00000 0.03849 0.04655 = 0.03729 0.01458 0.01047 0.00792 C30 1 0.626803 0.247205 0.528778 11.00000 0.05973 0.05002 = 0.04421 0.01422 0.01366 0.01746 AFIX 43 H30 2 0.533843 0.212252 0.533131 11.00000 -1.20000 AFIX 0 C14 1 0.757967 0.422967 0.952370 11.00000 0.05601 0.04687 = 0.03460 0.01124 0.00369 0.00797 AFIX 43 H14 2 0.797534 0.381303 0.981782 11.00000 -1.20000 AFIX 0 C12 1 0.316382 0.232974 0.866840 11.00000 0.03853 0.04794 = 0.06248 0.01641 0.02221 0.01686 AFIX 43 H12 2 0.365216 0.307645 0.891632 11.00000 -1.20000 AFIX 0 C6 1 0.630099 0.145805 0.969842 11.00000 0.04353 0.06768 = 0.04646 0.02780 0.01746 0.02279 AFIX 43 H6 2 0.539524 0.155623 0.972228 11.00000 -1.20000 AFIX 0 C23 1 0.574024 0.488956 0.615316 11.00000 0.06404 0.04868 = 0.04133 0.02039 0.01823 0.02428 AFIX 43 H23 2 0.643095 0.491362 0.588389 11.00000 -1.20000 AFIX 0 C2 1 0.821485 0.157440 0.909487 11.00000 0.04203 0.07034 = 0.04991 0.02713 0.01721 0.02628 AFIX 43 H2 2 0.859557 0.173254 0.870409 11.00000 -1.20000 AFIX 0 C36 1 0.987189 0.388925 0.777942 11.00000 0.04670 0.05896 = 0.05358 0.02328 0.01076 0.01434 AFIX 43 H36 2 0.964657 0.312672 0.763453 11.00000 -1.20000 AFIX 0 C17 1 0.635816 0.548950 0.868089 11.00000 0.08288 0.03847 = 0.04438 0.01308 0.01657 0.01737 AFIX 43 H17 2 0.592450 0.590916 0.840474 11.00000 -1.20000 AFIX 0 C8 1 0.317528 0.056522 0.801435 11.00000 0.04237 0.04446 = 0.05460 0.00715 0.01414 0.00777 AFIX 43 H8 2 0.367700 0.012379 0.781073 11.00000 -1.20000 AFIX 0 C20 1 0.368320 0.484279 0.695374 11.00000 0.05867 0.06173 = 0.05422 0.02473 0.02136 0.03575 AFIX 43 H20 2 0.298730 0.482219 0.721968 11.00000 -1.20000 AFIX 0 C5 1 0.708589 0.106242 1.024844 11.00000 0.06427 0.07456 = 0.05151 0.03712 0.01825 0.02512 AFIX 43 H5 2 0.669381 0.087980 1.063050 11.00000 -1.20000 AFIX 0 C22 1 0.469673 0.543502 0.599865 11.00000 0.08463 0.05787 = 0.04490 0.02685 0.01421 0.03541 AFIX 43 H22 2 0.469704 0.582614 0.563250 11.00000 -1.20000 AFIX 0 C29 1 0.650157 0.225023 0.458163 11.00000 0.09842 0.05901 = 0.04316 0.01376 0.01882 0.03614 AFIX 43 H29 2 0.572715 0.176528 0.415202 11.00000 -1.20000 AFIX 0 C3 1 0.901492 0.120396 0.965848 11.00000 0.05062 0.08271 = 0.06449 0.03014 0.01307 0.03852 AFIX 43 H3 2 0.994188 0.113352 0.965078 11.00000 -1.20000 AFIX 0 C4 1 0.844236 0.094050 1.022859 11.00000 0.06347 0.06419 = 0.05301 0.02855 0.00435 0.02943 AFIX 43 H4 2 0.897344 0.068057 1.059929 11.00000 -1.20000 AFIX 0 C32 1 0.911032 0.548972 0.777158 11.00000 0.05136 0.04874 = 0.06257 0.01197 0.00792 0.00753 AFIX 43 H32 2 0.837840 0.581207 0.761615 11.00000 -1.20000 AFIX 0 C21 1 0.366302 0.539620 0.638761 11.00000 0.07812 0.06899 = 0.05538 0.02840 0.01691 0.04691 AFIX 43 H21 2 0.294327 0.574265 0.627177 11.00000 -1.20000 AFIX 0 C9 1 0.168840 0.010416 0.796083 11.00000 0.04709 0.05266 = 0.06317 0.01178 0.00913 -0.00405 AFIX 43 H9 2 0.120110 -0.064848 0.773651 11.00000 -1.20000 AFIX 0 C10 1 0.092600 0.076453 0.824166 11.00000 0.03123 0.07946 = 0.07267 0.02860 0.01447 0.00705 AFIX 43 H10 2 -0.008662 0.046223 0.818846 11.00000 -1.20000 AFIX 0 C16 1 0.747878 0.599091 0.937527 11.00000 0.10154 0.03763 = 0.04850 0.00363 0.00703 0.00323 AFIX 43 H16 2 0.781556 0.675563 0.956601 11.00000 -1.20000 AFIX 0 C11 1 0.165434 0.185071 0.859387 11.00000 0.04078 0.07140 = 0.09212 0.03022 0.03209 0.02388 AFIX 43 H11 2 0.113829 0.228623 0.879004 11.00000 -1.20000 AFIX 0 C15 1 0.810789 0.536697 0.979154 11.00000 0.08142 0.05011 = 0.04104 0.00245 -0.00129 0.00024 AFIX 43 H15 2 0.888757 0.571328 1.025241 11.00000 -1.20000 AFIX 0 C28 1 0.787816 0.274680 0.451550 11.00000 0.10836 0.08677 = 0.05093 0.03058 0.04085 0.06039 AFIX 43 H28 2 0.804123 0.258939 0.404202 11.00000 -1.20000 AFIX 0 C26 1 0.878499 0.371554 0.585613 11.00000 0.05370 0.08691 = 0.05303 0.02093 0.02432 0.01179 AFIX 43 H26 2 0.955939 0.421595 0.627920 11.00000 -1.20000 AFIX 0 C35 1 1.129810 0.455495 0.824940 11.00000 0.04295 0.09205 = 0.05791 0.03155 0.00567 0.01367 AFIX 43 H35 2 1.203542 0.423935 0.840995 11.00000 -1.20000 AFIX 0 C34 1 1.163102 0.568754 0.848120 11.00000 0.04857 0.09187 = 0.05352 0.01812 0.00178 -0.00421 AFIX 43 H34 2 1.259457 0.613358 0.879100 11.00000 -1.20000 AFIX 0 C27 1 0.900968 0.347171 0.514324 11.00000 0.07683 0.10657 = 0.07344 0.03776 0.04794 0.03646 AFIX 43 H27 2 0.993969 0.380580 0.509390 11.00000 -1.20000 AFIX 0 C33 1 1.054656 0.614873 0.825533 11.00000 0.06963 0.05546 = 0.07493 0.00138 0.00617 -0.00808 AFIX 43 H33 2 1.076445 0.690870 0.842467 11.00000 -1.20000 AFIX 0 C42 1 0.134449 0.193131 0.393486 11.00000 0.16069 0.08104 = 0.12429 0.03136 0.02193 0.01752 AFIX 23 H42A 2 0.052370 0.139127 0.400282 11.00000 -1.20000 H42B 2 0.189247 0.153782 0.368178 11.00000 -1.20000 AFIX 0 CL3 4 0.439132 0.793555 0.797553 11.00000 0.21191 0.10242 = 0.31228 0.05006 0.16928 0.05299 CL4 4 0.761087 0.817770 0.825349 11.00000 0.14770 0.11502 = 0.33304 0.10833 0.06021 0.04031 C43 1 0.608811 0.855368 0.793788 11.00000 0.12602 0.22128 = 0.34875 0.21594 0.06882 0.05709 AFIX 23 H43A 2 0.635537 0.932530 0.821102 11.00000 -1.20000 H43B 2 0.596578 0.852539 0.740228 11.00000 -1.20000 AFIX 0 HKLF 4 REM lzx-147_a.res in P-1 REM R1 = 0.0603 for 7679 Fo > 4sig(Fo) and 0.0634 for all 8412 data REM 478 parameters refined using 0 restraints END WGHT 0.1162 1.8717 REM Highest difference peak 1.467, deepest hole -1.479, 1-sigma level 0.122 Q1 1 0.1625 0.2199 0.3099 11.00000 0.05 1.47 Q2 1 0.6740 0.8362 0.8819 11.00000 0.05 1.00 Q3 1 0.5364 0.8392 0.8654 11.00000 0.05 0.75 Q4 1 0.4778 0.8006 0.7581 11.00000 0.05 0.40 Q5 1 0.2831 0.2235 0.4347 11.00000 0.05 0.36 ; _shelx_res_checksum 16183 _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 1.785 _oxdiff_exptl_absorpt_empirical_full_min 0.553 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 0.71467(4) 0.04923(3) 0.67813(2) 0.05379(15) Uani 1 1 d . . . . . Cu1 Cu 0.59189(5) 0.18523(3) 0.71326(2) 0.03423(15) Uani 1 1 d . . . . . P1 P 0.58534(8) 0.22117(6) 0.83623(4) 0.03095(17) Uani 1 1 d . . . . . P2 P 0.69769(8) 0.34325(6) 0.68432(4) 0.03494(18) Uani 1 1 d . . . . . Cl2 Cl 0.2516(2) 0.27725(17) 0.48103(12) 0.1124(5) Uani 1 1 d . . . . . Cl1 Cl 0.0608(3) 0.27067(17) 0.33512(12) 0.1302(8) Uani 1 1 d . . . . . O1 O 0.4768(3) 0.37967(18) 0.76957(12) 0.0383(5) Uani 1 1 d . . . . . N1 N 0.3687(3) 0.1168(2) 0.63601(15) 0.0376(5) Uani 1 1 d . . . . . C13 C 0.6455(3) 0.3697(3) 0.88142(17) 0.0367(6) Uani 1 1 d . . . . . C39 C 0.0771(3) 0.0240(2) 0.52843(17) 0.0354(6) Uani 1 1 d . . . . . C1 C 0.6849(3) 0.1709(2) 0.91137(17) 0.0355(6) Uani 1 1 d . . . . . C7 C 0.3931(3) 0.1684(2) 0.83701(17) 0.0352(6) Uani 1 1 d . . . . . C41 C 0.2527(4) 0.1476(3) 0.64773(18) 0.0427(7) Uani 1 1 d . . . . . H41 H 0.2707 0.2016 0.6926 0.051 Uiso 1 1 calc R . . . . C18 C 0.5884(4) 0.4350(3) 0.83983(17) 0.0385(6) Uani 1 1 d . . . . . C25 C 0.7403(4) 0.3211(3) 0.5935(2) 0.0425(7) Uani 1 1 d . . . . . C38 C 0.1969(4) -0.0077(3) 0.51616(19) 0.0442(7) Uani 1 1 d . . . . . H38 H 0.1825 -0.0610 0.4715 0.053 Uiso 1 1 calc R . . . . C40 C 0.1079(4) 0.1035(3) 0.59687(19) 0.0438(7) Uani 1 1 d . . . . . H40 H 0.0312 0.1270 0.6084 0.053 Uiso 1 1 calc R . . . . C19 C 0.4749(4) 0.4325(3) 0.71150(18) 0.0394(6) Uani 1 1 d . . . . . C37 C 0.3381(4) 0.0401(3) 0.5703(2) 0.0443(7) Uani 1 1 d . . . . . H37 H 0.4165 0.0174 0.5604 0.053 Uiso 1 1 calc R . . . . C24 C 0.5775(4) 0.4303(2) 0.67070(18) 0.0384(6) Uani 1 1 d . . . . . C31 C 0.8774(4) 0.4359(3) 0.75231(19) 0.0418(7) Uani 1 1 d . . . . . C30 C 0.6268(5) 0.2472(3) 0.5288(2) 0.0517(8) Uani 1 1 d . . . . . H30 H 0.5338 0.2123 0.5331 0.062 Uiso 1 1 calc R . . . . C14 C 0.7580(4) 0.4230(3) 0.95237(19) 0.0497(8) Uani 1 1 d . . . . . H14 H 0.7975 0.3813 0.9818 0.060 Uiso 1 1 calc R . . . . C12 C 0.3164(4) 0.2330(3) 0.8668(2) 0.0477(8) Uani 1 1 d . . . . . H12 H 0.3652 0.3076 0.8916 0.057 Uiso 1 1 calc R . . . . C6 C 0.6301(4) 0.1458(3) 0.9698(2) 0.0491(8) Uani 1 1 d . . . . . H6 H 0.5395 0.1556 0.9722 0.059 Uiso 1 1 calc R . . . . C23 C 0.5740(5) 0.4890(3) 0.6153(2) 0.0486(8) Uani 1 1 d . . . . . H23 H 0.6431 0.4914 0.5884 0.058 Uiso 1 1 calc R . . . . C2 C 0.8215(4) 0.1574(3) 0.9095(2) 0.0503(8) Uani 1 1 d . . . . . H2 H 0.8596 0.1733 0.8704 0.060 Uiso 1 1 calc R . . . . C36 C 0.9872(4) 0.3889(3) 0.7779(2) 0.0535(9) Uani 1 1 d . . . . . H36 H 0.9647 0.3127 0.7635 0.064 Uiso 1 1 calc R . . . . C17 C 0.6358(5) 0.5489(3) 0.8681(2) 0.0561(9) Uani 1 1 d . . . . . H17 H 0.5925 0.5909 0.8405 0.067 Uiso 1 1 calc R . . . . C8 C 0.3175(4) 0.0565(3) 0.8014(2) 0.0496(8) Uani 1 1 d . . . . . H8 H 0.3677 0.0124 0.7811 0.060 Uiso 1 1 calc R . . . . C20 C 0.3683(5) 0.4843(3) 0.6954(2) 0.0529(9) Uani 1 1 d . . . . . H20 H 0.2987 0.4822 0.7220 0.063 Uiso 1 1 calc R . . . . C5 C 0.7086(5) 0.1062(4) 1.0248(2) 0.0600(10) Uani 1 1 d . . . . . H5 H 0.6694 0.0880 1.0631 0.072 Uiso 1 1 calc R . . . . C22 C 0.4697(5) 0.5435(3) 0.5999(2) 0.0593(10) Uani 1 1 d . . . . . H22 H 0.4697 0.5826 0.5632 0.071 Uiso 1 1 calc R . . . . C29 C 0.6502(6) 0.2250(4) 0.4582(2) 0.0654(11) Uani 1 1 d . . . . . H29 H 0.5727 0.1765 0.4152 0.079 Uiso 1 1 calc R . . . . C3 C 0.9015(5) 0.1204(4) 0.9658(3) 0.0620(10) Uani 1 1 d . . . . . H3 H 0.9942 0.1134 0.9651 0.074 Uiso 1 1 calc R . . . . C4 C 0.8442(5) 0.0940(4) 1.0229(2) 0.0593(10) Uani 1 1 d . . . . . H4 H 0.8973 0.0681 1.0599 0.071 Uiso 1 1 calc R . . . . C32 C 0.9110(5) 0.5490(3) 0.7772(3) 0.0585(9) Uani 1 1 d . . . . . H32 H 0.8378 0.5812 0.7616 0.070 Uiso 1 1 calc R . . . . C21 C 0.3663(5) 0.5396(4) 0.6388(2) 0.0619(11) Uani 1 1 d . . . . . H21 H 0.2943 0.5743 0.6272 0.074 Uiso 1 1 calc R . . . . C9 C 0.1688(5) 0.0104(3) 0.7961(3) 0.0606(10) Uani 1 1 d . . . . . H9 H 0.1201 -0.0648 0.7737 0.073 Uiso 1 1 calc R . . . . C10 C 0.0926(4) 0.0765(4) 0.8242(3) 0.0626(11) Uani 1 1 d . . . . . H10 H -0.0087 0.0462 0.8188 0.075 Uiso 1 1 calc R . . . . C16 C 0.7479(6) 0.5991(3) 0.9375(2) 0.0710(13) Uani 1 1 d . . . . . H16 H 0.7816 0.6756 0.9566 0.085 Uiso 1 1 calc R . . . . C11 C 0.1654(5) 0.1851(4) 0.8594(3) 0.0636(11) Uani 1 1 d . . . . . H11 H 0.1138 0.2286 0.8790 0.076 Uiso 1 1 calc R . . . . C15 C 0.8108(6) 0.5367(3) 0.9792(2) 0.0673(12) Uani 1 1 d . . . . . H15 H 0.8888 0.5713 1.0252 0.081 Uiso 1 1 calc R . . . . C28 C 0.7878(7) 0.2747(4) 0.4516(3) 0.0714(13) Uani 1 1 d . . . . . H28 H 0.8041 0.2589 0.4042 0.086 Uiso 1 1 calc R . . . . C26 C 0.8785(5) 0.3716(4) 0.5856(3) 0.0651(11) Uani 1 1 d . . . . . H26 H 0.9559 0.4216 0.6279 0.078 Uiso 1 1 calc R . . . . C35 C 1.1298(5) 0.4555(4) 0.8249(3) 0.0663(12) Uani 1 1 d . . . . . H35 H 1.2035 0.4239 0.8410 0.080 Uiso 1 1 calc R . . . . C34 C 1.1631(5) 0.5688(5) 0.8481(3) 0.0732(13) Uani 1 1 d . . . . . H34 H 1.2595 0.6134 0.8791 0.088 Uiso 1 1 calc R . . . . C27 C 0.9010(6) 0.3472(5) 0.5143(3) 0.0776(14) Uani 1 1 d . . . . . H27 H 0.9940 0.3806 0.5094 0.093 Uiso 1 1 calc R . . . . C33 C 1.0547(6) 0.6149(4) 0.8255(3) 0.0782(14) Uani 1 1 d . . . . . H33 H 1.0764 0.6909 0.8425 0.094 Uiso 1 1 calc R . . . . C42 C 0.1344(11) 0.1931(6) 0.3935(5) 0.130(3) Uani 1 1 d . . . . . H42A H 0.0524 0.1391 0.4003 0.157 Uiso 1 1 calc R . . . . H42B H 0.1892 0.1538 0.3682 0.157 Uiso 1 1 calc R . . . . Cl3 Cl 0.4391(4) 0.7936(2) 0.7976(3) 0.1927(16) Uani 1 1 d . . . . . Cl4 Cl 0.7611(3) 0.8178(2) 0.8253(3) 0.1951(16) Uani 1 1 d . . . . . C43 C 0.6088(12) 0.8554(11) 0.7938(10) 0.212(7) Uani 1 1 d . . . . . H43A H 0.6355 0.9325 0.8211 0.255 Uiso 1 1 calc R . . . . H43B H 0.5966 0.8525 0.7402 0.255 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 0.0544(3) 0.0569(2) 0.0547(2) 0.00979(18) 0.01458(18) 0.03230(19) Cu1 0.0313(2) 0.0351(2) 0.0338(2) 0.00795(18) 0.00840(18) 0.00946(18) P1 0.0272(3) 0.0359(4) 0.0302(3) 0.0110(3) 0.0082(3) 0.0103(3) P2 0.0338(4) 0.0362(4) 0.0347(4) 0.0126(3) 0.0100(3) 0.0097(3) Cl2 0.1078(12) 0.1138(13) 0.1067(12) 0.0372(10) 0.0238(10) 0.0258(10) Cl1 0.1583(18) 0.0976(12) 0.1029(12) 0.0385(10) 0.0177(12) 0.0037(12) O1 0.0437(12) 0.0377(10) 0.0347(10) 0.0133(8) 0.0103(9) 0.0147(9) N1 0.0312(12) 0.0376(12) 0.0361(13) 0.0073(10) 0.0027(10) 0.0083(10) C13 0.0366(15) 0.0378(14) 0.0321(14) 0.0091(11) 0.0102(12) 0.0073(12) C39 0.0307(15) 0.0350(14) 0.0331(14) 0.0086(11) 0.0018(12) 0.0071(11) C1 0.0312(14) 0.0381(14) 0.0366(14) 0.0120(12) 0.0079(11) 0.0116(11) C7 0.0297(14) 0.0397(15) 0.0369(14) 0.0145(12) 0.0088(11) 0.0109(11) C41 0.0360(16) 0.0502(17) 0.0329(15) 0.0015(13) 0.0025(12) 0.0147(13) C18 0.0446(17) 0.0365(15) 0.0318(14) 0.0081(12) 0.0121(12) 0.0097(12) C25 0.0443(17) 0.0457(17) 0.0432(17) 0.0174(14) 0.0163(14) 0.0179(14) C38 0.0380(16) 0.0429(16) 0.0385(16) -0.0043(13) 0.0014(13) 0.0130(13) C40 0.0334(15) 0.0534(18) 0.0385(16) 0.0023(14) 0.0067(12) 0.0164(14) C19 0.0456(17) 0.0386(15) 0.0359(15) 0.0140(12) 0.0097(13) 0.0169(13) C37 0.0314(15) 0.0446(17) 0.0468(18) 0.0017(14) 0.0029(13) 0.0129(13) C24 0.0406(16) 0.0361(14) 0.0356(15) 0.0123(12) 0.0064(12) 0.0111(12) C31 0.0385(16) 0.0466(17) 0.0373(15) 0.0146(13) 0.0105(12) 0.0079(13) C30 0.060(2) 0.0500(19) 0.0442(18) 0.0142(15) 0.0137(16) 0.0175(16) C14 0.056(2) 0.0469(18) 0.0346(16) 0.0112(14) 0.0037(14) 0.0080(15) C12 0.0385(17) 0.0479(18) 0.062(2) 0.0164(16) 0.0222(15) 0.0169(14) C6 0.0435(18) 0.068(2) 0.0465(18) 0.0278(17) 0.0175(15) 0.0228(16) C23 0.064(2) 0.0487(18) 0.0413(17) 0.0204(15) 0.0182(16) 0.0243(16) C2 0.0420(18) 0.070(2) 0.0499(19) 0.0271(17) 0.0172(15) 0.0263(17) C36 0.0467(19) 0.059(2) 0.054(2) 0.0233(17) 0.0108(16) 0.0143(16) C17 0.083(3) 0.0385(17) 0.0444(19) 0.0131(14) 0.0166(18) 0.0174(17) C8 0.0424(18) 0.0445(17) 0.055(2) 0.0072(15) 0.0141(15) 0.0078(14) C20 0.059(2) 0.062(2) 0.054(2) 0.0247(17) 0.0214(17) 0.0357(18) C5 0.064(2) 0.075(3) 0.052(2) 0.037(2) 0.0183(18) 0.025(2) C22 0.085(3) 0.058(2) 0.0449(19) 0.0269(17) 0.0142(19) 0.035(2) C29 0.098(3) 0.059(2) 0.043(2) 0.0138(17) 0.019(2) 0.036(2) C3 0.051(2) 0.083(3) 0.064(2) 0.030(2) 0.0131(18) 0.039(2) C4 0.063(2) 0.064(2) 0.053(2) 0.0285(18) 0.0043(18) 0.0294(19) C32 0.051(2) 0.049(2) 0.063(2) 0.0120(17) 0.0079(18) 0.0075(16) C21 0.078(3) 0.069(2) 0.055(2) 0.0284(19) 0.017(2) 0.047(2) C9 0.047(2) 0.053(2) 0.063(2) 0.0118(18) 0.0091(17) -0.0041(17) C10 0.0312(17) 0.079(3) 0.073(3) 0.029(2) 0.0145(17) 0.0071(18) C16 0.102(4) 0.0376(18) 0.048(2) 0.0036(16) 0.007(2) 0.003(2) C11 0.041(2) 0.071(3) 0.092(3) 0.030(2) 0.032(2) 0.0239(19) C15 0.081(3) 0.050(2) 0.0410(19) 0.0024(16) -0.0013(19) 0.000(2) C28 0.108(4) 0.087(3) 0.051(2) 0.031(2) 0.041(3) 0.060(3) C26 0.054(2) 0.087(3) 0.053(2) 0.021(2) 0.0243(18) 0.012(2) C35 0.043(2) 0.092(3) 0.058(2) 0.032(2) 0.0057(17) 0.014(2) C34 0.049(2) 0.092(3) 0.054(2) 0.018(2) 0.0018(18) -0.004(2) C27 0.077(3) 0.107(4) 0.073(3) 0.038(3) 0.048(3) 0.036(3) C33 0.070(3) 0.055(2) 0.075(3) 0.001(2) 0.006(2) -0.008(2) C42 0.161(8) 0.081(4) 0.124(6) 0.031(4) 0.022(6) 0.018(5) Cl3 0.212(3) 0.1024(15) 0.312(4) 0.050(2) 0.169(3) 0.0530(18) Cl4 0.148(2) 0.1150(17) 0.333(5) 0.108(3) 0.060(3) 0.0403(16) C43 0.126(8) 0.221(13) 0.35(2) 0.216(15) 0.069(10) 0.057(8) 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' Cl Cl 0.3639 0.7018 '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' 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' 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 115.74(3) . . ? P1 Cu1 P2 111.45(3) . . ? P2 Cu1 Br1 109.24(3) . . ? N1 Cu1 Br1 104.46(8) . . ? N1 Cu1 P1 109.42(8) . . ? N1 Cu1 P2 105.86(7) . . ? C13 P1 Cu1 111.26(10) . . ? C13 P1 C1 102.76(14) . . ? C1 P1 Cu1 124.63(11) . . ? C7 P1 Cu1 110.03(10) . . ? C7 P1 C13 105.24(14) . . ? C7 P1 C1 101.02(14) . . ? C25 P2 Cu1 114.60(11) . . ? C25 P2 C24 101.87(15) . . ? C24 P2 Cu1 114.51(11) . . ? C31 P2 Cu1 116.70(11) . . ? C31 P2 C25 102.26(16) . . ? C31 P2 C24 105.09(15) . . ? C18 O1 C19 116.4(2) . . ? C41 N1 Cu1 124.0(2) . . ? C37 N1 Cu1 120.0(2) . . ? C37 N1 C41 116.0(3) . . ? C18 C13 P1 118.4(2) . . ? C18 C13 C14 117.7(3) . . ? C14 C13 P1 123.5(3) . . ? C38 C39 C39 122.2(4) . 2_556 ? C38 C39 C40 116.5(3) . . ? C40 C39 C39 121.4(4) . 2_556 ? C6 C1 P1 122.9(2) . . ? C6 C1 C2 118.8(3) . . ? C2 C1 P1 118.3(2) . . ? C12 C7 P1 124.4(2) . . ? C12 C7 C8 118.8(3) . . ? C8 C7 P1 116.7(3) . . ? N1 C41 C40 123.7(3) . . ? C13 C18 O1 116.4(3) . . ? C17 C18 O1 121.8(3) . . ? C17 C18 C13 121.8(3) . . ? C30 C25 P2 117.3(3) . . ? C26 C25 P2 124.3(3) . . ? C26 C25 C30 118.4(4) . . ? C37 C38 C39 119.9(3) . . ? C41 C40 C39 119.8(3) . . ? O1 C19 C24 119.9(3) . . ? C20 C19 O1 118.0(3) . . ? C20 C19 C24 122.0(3) . . ? N1 C37 C38 124.0(3) . . ? C19 C24 P2 120.2(2) . . ? C19 C24 C23 117.1(3) . . ? C23 C24 P2 122.5(3) . . ? C36 C31 P2 117.2(3) . . ? C32 C31 P2 123.7(3) . . ? C32 C31 C36 119.1(3) . . ? C29 C30 C25 121.0(4) . . ? C15 C14 C13 120.7(3) . . ? C7 C12 C11 119.5(4) . . ? C1 C6 C5 120.8(3) . . ? C22 C23 C24 121.3(4) . . ? C1 C2 C3 120.2(3) . . ? C35 C36 C31 120.1(4) . . ? C16 C17 C18 119.1(4) . . ? C9 C8 C7 120.7(4) . . ? C19 C20 C21 119.1(4) . . ? C4 C5 C6 120.0(4) . . ? C21 C22 C23 119.8(3) . . ? C28 C29 C30 119.9(4) . . ? C4 C3 C2 120.4(4) . . ? C5 C4 C3 119.9(3) . . ? C31 C32 C33 120.1(4) . . ? C22 C21 C20 120.5(4) . . ? C8 C9 C10 119.8(4) . . ? C11 C10 C9 119.9(3) . . ? C17 C16 C15 120.5(4) . . ? C10 C11 C12 121.2(4) . . ? C14 C15 C16 120.0(4) . . ? C27 C28 C29 120.2(4) . . ? C25 C26 C27 120.0(4) . . ? C34 C35 C36 120.2(4) . . ? C33 C34 C35 119.9(4) . . ? C28 C27 C26 120.7(5) . . ? C34 C33 C32 120.5(5) . . ? Cl2 C42 Cl1 110.7(4) . . ? Cl3 C43 Cl4 124.4(6) . . ? 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 2.4551(5) . ? Cu1 P1 2.2734(8) . ? Cu1 P2 2.2837(8) . ? Cu1 N1 2.123(3) . ? P1 C13 1.829(3) . ? P1 C1 1.830(3) . ? P1 C7 1.816(3) . ? P2 C25 1.830(3) . ? P2 C24 1.834(3) . ? P2 C31 1.822(3) . ? Cl2 C42 1.703(9) . ? Cl1 C42 1.773(8) . ? O1 C18 1.391(4) . ? O1 C19 1.394(4) . ? N1 C41 1.340(4) . ? N1 C37 1.335(4) . ? C13 C18 1.388(4) . ? C13 C14 1.400(4) . ? C39 C39 1.491(5) 2_556 ? C39 C38 1.384(5) . ? C39 C40 1.391(4) . ? C1 C6 1.386(5) . ? C1 C2 1.388(5) . ? C7 C12 1.386(5) . ? C7 C8 1.392(5) . ? C41 C40 1.382(4) . ? C18 C17 1.386(5) . ? C25 C30 1.392(5) . ? C25 C26 1.389(5) . ? C38 C37 1.382(4) . ? C19 C24 1.398(5) . ? C19 C20 1.379(5) . ? C24 C23 1.401(4) . ? C31 C36 1.392(5) . ? C31 C32 1.382(5) . ? C30 C29 1.381(6) . ? C14 C15 1.381(6) . ? C12 C11 1.394(5) . ? C6 C5 1.387(5) . ? C23 C22 1.386(6) . ? C2 C3 1.390(5) . ? C36 C35 1.384(6) . ? C17 C16 1.375(6) . ? C8 C9 1.380(5) . ? C20 C21 1.391(5) . ? C5 C4 1.373(6) . ? C22 C21 1.373(6) . ? C29 C28 1.372(8) . ? C3 C4 1.378(6) . ? C32 C33 1.395(6) . ? C9 C10 1.382(7) . ? C10 C11 1.352(7) . ? C16 C15 1.382(7) . ? C28 C27 1.365(8) . ? C26 C27 1.392(6) . ? C35 C34 1.383(8) . ? C34 C33 1.361(8) . ? Cl3 C43 1.660(10) . ? Cl4 C43 1.680(11) . ?