#------------------------------------------------------------------------------ #$Date: 2020-08-01 04:44:00 +0300 (Sat, 01 Aug 2020) $ #$Revision: 254722 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/49/7704981.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_7704981 loop_ _publ_author_name 'Shamsieva, Aliia' 'Musina, Elvira I.' 'Gerasimova, Tatiana' 'Strelnik, Igor' 'Strelnik, Anna' 'Kolesnikov, Ilya' 'Kalinichev, Alexey' 'Islamov, Daut' 'Samigullina, Aida I.' 'L\"onnecke, Peter' 'Katsyuba, Sergey' 'Hey-Hawkins, Evamarie' 'Karasik, Andrey' 'Sinyashin, Oleg Geroldovich' _publ_section_title ; Triple-bridged helical binuclear copper(I) complexes. Head-to-head and head-to-tail isomerism and the solid-state luminescence ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT01843K _journal_year 2020 _chemical_formula_moiety 'C27 H36 Br Cu2 N3 P3 1+, 2(C2 H6 O), Br 1-' _chemical_formula_sum 'C31 H48 Br2 Cu2 N3 O2 P3' _chemical_formula_weight 874.53 _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-05-11 deposited with the CCDC. 2020-07-31 downloaded from the CCDC. ; _cell_angle_alpha 84.174(3) _cell_angle_beta 78.867(4) _cell_angle_gamma 76.930(4) _cell_formula_units_Z 2 _cell_length_a 9.2270(5) _cell_length_b 14.0796(6) _cell_length_c 14.6601(5) _cell_measurement_reflns_used 8899 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 30.9320 _cell_measurement_theta_min 2.3090 _cell_volume 1816.94(14) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics ; ORTEP3 for Windows L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. ; _computing_publication_material ; WINGX L.J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854. ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution ; SHELXT-2014 Program for Crystal Structure Analysis (Release 2014-4) G. M. Sheldrick, Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany. G. M. Sheldrick, Acta. Cryst., 2015, A71, 3 - 8 ; _diffrn_ambient_temperature 170(2) _diffrn_detector_area_resol_mean 16.3560 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.895 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.895 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 27187 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.895 _diffrn_reflns_theta_full 30.510 _diffrn_reflns_theta_max 32.635 _diffrn_reflns_theta_min 1.992 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.533 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.599 _exptl_crystal_description needle _exptl_crystal_F_000 888 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.262 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 427 _refine_ls_number_reflns 11896 _refine_ls_number_restraints 84 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0426 _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^)+(0.0438P)^2^+1.1150P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.1069 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8552 _reflns_number_total 11896 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01843k2.cif _cod_data_source_block 4HT_Br_x2331fin _cod_original_cell_volume 1816.94(15) _cod_database_code 7704981 _shelx_shelxl_version_number 2018/3 _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_res_file ; TITL x2331fin in P-1 4HT_Br_x2331fin.res created by SHELXL-2018/3 at 14:01:47 on 11-May-2020 CELL 0.71073 9.2270 14.0796 14.6601 84.174 78.867 76.930 ZERR 2.00 0.0005 0.0006 0.0005 0.003 0.004 0.004 LATT 1 SFAC BR CU P O N C H UNIT 4 4 6 4 6 62 96 MERG 2 EADP P2,P2' SADI P2,C26 P2,C29 P2',C26' P2',C29' EADP O1,O1' EADP C90,C90' EADP C92,C92' DFIX 1.53 0.001 C90,C91 C90',C91' C92,C93 C92',C93' DFIX 1.42 0.001 C90,O1 C90',O1' C92,O2 C92',O2' DFIX 2.41 0.001 C91,O1 C91',O1' C93,O2 C93',O2' HTAB O1,BR2 HTAB O2,BR2 SIMU 0.02 P2,C26,C27,C28,C29 SIMU 0.02 P2',C26',C27',C28',C29' FMAP 2 PLAN 5 ACTA 61.02 BOND $H L.S. 10 TEMP -103.00 WGHT 0.043800 1.115000 FVAR 0.36839 0.63278 0.61589 0.57955 MOLE 1 BR1 1 -0.007826 0.243075 0.653704 11.00000 0.01770 0.03038 = 0.03692 -0.00058 -0.00226 -0.00467 BR2 1 0.940789 0.250642 0.194266 11.00000 0.04316 0.04536 = 0.04008 -0.00389 -0.00830 0.00629 CU1 2 0.273458 0.234662 0.636334 11.00000 0.01887 0.02002 = 0.02485 -0.00002 -0.00329 -0.00356 CU2 2 0.552687 0.241413 0.663447 11.00000 0.02261 0.01910 = 0.02466 -0.00339 -0.00360 -0.00268 P1 3 0.302157 0.134064 0.762807 11.00000 0.01881 0.02292 = 0.02077 -0.00129 -0.00172 -0.00424 PART 1 P2 3 0.270066 0.396605 0.636287 21.00000 0.01922 0.01813 = 0.03119 -0.00094 -0.00163 -0.00236 PART 2 P2' 3 0.250797 0.395474 0.657877 -21.00000 0.01922 0.01813 = 0.03119 -0.00094 -0.00163 -0.00236 PART 0 P3 3 0.627184 0.177957 0.527100 11.00000 0.01775 0.01786 = 0.02272 -0.00248 -0.00264 -0.00347 N1 5 0.596126 0.123402 0.757260 11.00000 0.02177 0.02304 = 0.02295 0.00069 -0.00397 -0.00683 N2 5 0.522451 0.374013 0.708309 11.00000 0.02295 0.02318 = 0.03030 -0.00618 -0.00252 -0.00422 N3 5 0.342511 0.210763 0.494137 11.00000 0.02004 0.02058 = 0.02413 -0.00010 -0.00492 -0.00263 C11 6 0.488681 0.070343 0.787189 11.00000 0.02326 0.02410 = 0.01912 -0.00136 -0.00390 -0.00542 C12 6 0.522373 -0.021983 0.830618 11.00000 0.02825 0.02555 = 0.03349 0.00495 -0.00783 -0.00782 AFIX 43 H12 7 0.445208 -0.057731 0.852026 11.00000 -1.20000 AFIX 0 C13 6 0.669639 -0.061708 0.842545 11.00000 0.03226 0.02594 = 0.03921 0.00537 -0.01355 -0.00481 AFIX 43 H13 7 0.694995 -0.125384 0.871282 11.00000 -1.20000 AFIX 0 C14 6 0.778552 -0.007822 0.812274 11.00000 0.02449 0.03336 = 0.03707 0.00158 -0.01139 -0.00249 AFIX 43 H14 7 0.880381 -0.033580 0.819558 11.00000 -1.20000 AFIX 0 C15 6 0.737299 0.084143 0.771218 11.00000 0.02200 0.03478 = 0.03275 0.00185 -0.00543 -0.00847 AFIX 43 H15 7 0.812544 0.121731 0.751777 11.00000 -1.20000 AFIX 0 C16 6 0.182919 0.042989 0.794520 11.00000 0.02701 0.03354 = 0.02656 0.00361 -0.00532 -0.01332 AFIX 23 H16A 7 0.112460 0.049467 0.750081 11.00000 -1.20000 H16B 7 0.246536 -0.023853 0.792969 11.00000 -1.20000 AFIX 0 C17 6 0.094918 0.061767 0.892494 11.00000 0.05200 0.07949 = 0.03604 -0.00405 0.01372 -0.03236 AFIX 23 H17A 7 -0.009348 0.098020 0.889044 11.00000 -1.20000 H17B 7 0.089024 -0.001281 0.928090 11.00000 -1.20000 AFIX 0 C18 6 0.170705 0.119595 0.941250 11.00000 0.05288 0.08106 = 0.02325 -0.00932 0.00235 -0.01534 AFIX 23 H18A 7 0.258130 0.076547 0.964714 11.00000 -1.20000 H18B 7 0.099139 0.150466 0.994779 11.00000 -1.20000 AFIX 0 C19 6 0.223667 0.198146 0.870398 11.00000 0.03175 0.04043 = 0.03252 -0.01463 -0.00413 -0.00011 AFIX 23 H19A 7 0.301734 0.224399 0.891445 11.00000 -1.20000 H19B 7 0.137907 0.252640 0.860964 11.00000 -1.20000 AFIX 0 C21 6 0.390993 0.439061 0.703495 11.00000 0.02821 0.02061 = 0.03174 -0.00377 -0.00306 -0.00262 C22 6 0.362709 0.530297 0.738889 11.00000 0.04239 0.02221 = 0.04683 -0.00925 -0.00688 0.00015 AFIX 43 H22 7 0.269263 0.574865 0.736118 11.00000 -1.20000 AFIX 0 C23 6 0.472200 0.555732 0.778328 11.00000 0.06047 0.03186 = 0.05187 -0.01710 -0.01266 -0.01158 AFIX 43 H23 7 0.453884 0.617626 0.803800 11.00000 -1.20000 AFIX 0 C24 6 0.607131 0.491128 0.780414 11.00000 0.04900 0.04397 = 0.05000 -0.01823 -0.01351 -0.01582 AFIX 43 H24 7 0.684652 0.508133 0.805590 11.00000 -1.20000 AFIX 0 C25 6 0.628241 0.400486 0.745061 11.00000 0.03038 0.03748 = 0.03810 -0.01132 -0.00497 -0.00827 AFIX 43 H25 7 0.721435 0.355360 0.746978 11.00000 -1.20000 AFIX 0 C31 6 0.487459 0.202000 0.449703 11.00000 0.02084 0.01982 = 0.02536 -0.00249 -0.00275 -0.00432 C32 6 0.523748 0.209097 0.353534 11.00000 0.02716 0.03242 = 0.02508 -0.00224 -0.00079 -0.00628 AFIX 43 H32 7 0.625925 0.204726 0.323886 11.00000 -1.20000 AFIX 0 C33 6 0.410283 0.222650 0.300341 11.00000 0.03620 0.03642 = 0.02302 -0.00237 -0.00797 -0.00598 AFIX 43 H33 7 0.433405 0.228198 0.234259 11.00000 -1.20000 AFIX 0 C34 6 0.263984 0.227819 0.345648 11.00000 0.02956 0.03460 = 0.03062 -0.00113 -0.01304 -0.00389 AFIX 43 H34 7 0.184274 0.235376 0.311304 11.00000 -1.20000 AFIX 0 C35 6 0.234398 0.221861 0.442035 11.00000 0.02206 0.02886 = 0.03253 -0.00149 -0.00896 -0.00365 AFIX 43 H35 7 0.132849 0.225808 0.472762 11.00000 -1.20000 AFIX 0 C36 6 0.806829 0.187905 0.450748 11.00000 0.02179 0.03541 = 0.03172 -0.00295 -0.00253 -0.01061 AFIX 23 H36A 7 0.787954 0.235174 0.397369 11.00000 -1.20000 H36B 7 0.872644 0.211130 0.485588 11.00000 -1.20000 AFIX 0 C37 6 0.883481 0.086863 0.415980 11.00000 0.03297 0.03559 = 0.04832 0.00298 0.01422 0.00593 AFIX 23 H37A 7 0.917089 0.092297 0.347671 11.00000 -1.20000 H37B 7 0.973732 0.060436 0.445165 11.00000 -1.20000 AFIX 0 C38 6 0.774393 0.017383 0.439893 11.00000 0.04118 0.02306 = 0.03403 -0.00724 0.00199 0.00576 AFIX 23 H38A 7 0.710494 0.024677 0.391531 11.00000 -1.20000 H38B 7 0.831246 -0.051143 0.443373 11.00000 -1.20000 AFIX 0 C39 6 0.676607 0.043690 0.533807 11.00000 0.02862 0.01952 = 0.02895 -0.00130 -0.00339 -0.00542 AFIX 23 H39A 7 0.733400 0.018666 0.585143 11.00000 -1.20000 H39B 7 0.584644 0.016192 0.544006 11.00000 -1.20000 AFIX 0 PART 1 SAME C26' > C29' C26 6 0.316832 0.455362 0.519785 21.00000 0.03511 0.02193 = 0.03327 0.00156 -0.00813 -0.00654 AFIX 23 H26A 7 0.427645 0.447089 0.500510 21.00000 -1.20000 H26B 7 0.276825 0.426963 0.473286 21.00000 -1.20000 AFIX 0 C27 6 0.242143 0.562647 0.528768 21.00000 0.04872 0.02252 = 0.04351 0.00555 -0.01283 -0.00546 AFIX 23 H27A 7 0.229911 0.594944 0.466693 21.00000 -1.20000 H27B 7 0.304996 0.596125 0.556662 21.00000 -1.20000 AFIX 0 C28 6 0.083907 0.567804 0.592860 21.00000 0.03882 0.02873 = 0.05236 -0.00745 -0.01765 0.01142 AFIX 23 H28A 7 0.054791 0.629355 0.625414 21.00000 -1.20000 H28B 7 0.007096 0.568006 0.554070 21.00000 -1.20000 AFIX 0 C29 6 0.087006 0.483019 0.662983 21.00000 0.02625 0.02235 = 0.05719 -0.00471 -0.00315 0.00223 AFIX 23 H29A 7 0.003515 0.450267 0.660837 21.00000 -1.20000 H29B 7 0.073656 0.505903 0.726333 21.00000 -1.20000 AFIX 0 PART 2 SAME C26 > C29 C26' 6 0.236580 0.476870 0.551860 -21.00000 0.04674 0.03767 = 0.04171 0.00622 -0.01781 -0.01712 AFIX 23 H26C 7 0.330691 0.501572 0.531297 -21.00000 -1.20000 H26D 7 0.221822 0.440700 0.501058 -21.00000 -1.20000 AFIX 0 C27' 6 0.101589 0.562461 0.574315 -21.00000 0.04924 0.03257 = 0.04973 0.00545 -0.01364 -0.01496 AFIX 23 H27C 7 0.057382 0.587656 0.517955 -21.00000 -1.20000 H27D 7 0.133091 0.616300 0.598589 -21.00000 -1.20000 AFIX 0 C28' 6 -0.016451 0.519274 0.650820 -21.00000 0.04664 0.02960 = 0.08010 -0.01126 -0.02219 0.00765 AFIX 23 H28C 7 -0.094203 0.572986 0.680801 -21.00000 -1.20000 H28D 7 -0.067443 0.478561 0.621780 -21.00000 -1.20000 AFIX 0 C29' 6 0.068500 0.457878 0.722705 -21.00000 0.03104 0.02304 = 0.04441 -0.01047 -0.00452 0.00202 AFIX 23 H29C 7 0.011026 0.409620 0.756351 -21.00000 -1.20000 H29D 7 0.084607 0.499806 0.768506 -21.00000 -1.20000 AFIX 0 MOLE 2 PART 1 O1 4 0.659458 0.211325 0.113345 31.00000 0.05249 AFIX 147 H1O1 7 0.732550 0.216796 0.137374 31.00000 -1.50000 AFIX 0 C90 6 0.681437 0.246243 0.018468 31.00000 0.05777 AFIX 23 H90A 7 0.783665 0.215449 -0.013206 31.00000 -1.20000 H90B 7 0.673244 0.317828 0.014301 31.00000 -1.20000 AFIX 0 C91 6 0.561995 0.221790 -0.029234 31.00000 0.09096 AFIX 137 H91A 7 0.580222 0.150911 -0.033393 31.00000 -1.50000 H91B 7 0.567919 0.253826 -0.091993 31.00000 -1.50000 H91C 7 0.461329 0.244969 0.007125 31.00000 -1.50000 AFIX 0 PART 2 O1' 4 0.686689 0.191218 0.102381 -31.00000 0.05249 AFIX 147 H1O' 7 0.772498 0.163011 0.113494 -31.00000 -1.50000 AFIX 0 C90' 6 0.687895 0.195672 0.005053 -31.00000 0.05777 AFIX 23 H90C 7 0.582984 0.208268 -0.006835 -31.00000 -1.20000 H90D 7 0.742879 0.132451 -0.020501 -31.00000 -1.20000 AFIX 0 C91' 6 0.765103 0.277441 -0.042882 -31.00000 0.07406 AFIX 137 H91D 7 0.691817 0.339909 -0.038958 -31.00000 -1.50000 H91E 7 0.804061 0.264162 -0.108435 -31.00000 -1.50000 H91F 7 0.848891 0.280634 -0.011962 -31.00000 -1.50000 AFIX 0 MOLE 3 PART 1 O2 4 1.235013 0.348465 0.115224 41.00000 0.11047 AFIX 83 H2O2 7 1.164267 0.334756 0.156152 41.00000 -1.50000 AFIX 0 C92 6 1.174568 0.419716 0.049042 41.00000 0.18262 AFIX 23 H92A 7 1.113289 0.478102 0.080960 41.00000 -1.20000 H92B 7 1.108216 0.392984 0.017450 41.00000 -1.20000 AFIX 0 C93 6 1.304044 0.448227 -0.022766 41.00000 0.11425 AFIX 137 H93A 7 1.332899 0.504377 -0.002278 41.00000 -1.50000 H93B 7 1.271124 0.465535 -0.083096 41.00000 -1.50000 H93C 7 1.391019 0.393026 -0.028908 41.00000 -1.50000 AFIX 0 PART 2 O2' 4 1.180765 0.390882 0.135275 -41.00000 0.06433 AFIX 83 H2O' 7 1.199259 0.331602 0.153588 -41.00000 -1.50000 AFIX 0 C92' 6 1.208940 0.399405 0.036402 -41.00000 0.18262 AFIX 23 H92C 7 1.152563 0.358523 0.011927 -41.00000 -1.20000 H92D 7 1.318075 0.376116 0.012856 -41.00000 -1.20000 AFIX 0 C93' 6 1.158971 0.506300 0.002975 -41.00000 0.25470 AFIX 137 H93D 7 1.122039 0.509400 -0.055833 -41.00000 -1.50000 H93E 7 1.244969 0.538425 -0.006570 -41.00000 -1.50000 H93F 7 1.077904 0.539535 0.049921 -41.00000 -1.50000 AFIX 0 HKLF 4 REM x2331fin in P-1 REM wR2 = 0.1069, GooF = S = 1.023, Restrained GooF = 1.020 for all data REM R1 = 0.0426 for 8552 Fo > 4sig(Fo) and 0.0712 for all 11896 data REM 427 parameters refined using 84 restraints END WGHT 0.0438 1.1150 REM Highest difference peak 1.262, deepest hole -0.977, 1-sigma level 0.104 Q1 1 1.2598 0.3414 0.0494 11.00000 0.05 1.26 Q2 1 0.8788 0.2361 0.1764 11.00000 0.05 1.15 Q3 1 0.9858 0.2815 0.1590 11.00000 0.05 1.12 Q4 1 1.3373 0.4141 -0.0077 11.00000 0.05 0.92 Q5 1 0.6228 0.2239 0.0918 11.00000 0.05 0.87 ; _shelx_res_checksum 94780 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 -0.00783(3) 0.24308(2) 0.65370(2) 0.02885(7) Uani 1 1 d . . . . . Br2 Br 0.94079(4) 0.25064(3) 0.19427(3) 0.04517(10) Uani 1 1 d . . . . . Cu1 Cu 0.27346(4) 0.23466(2) 0.63633(2) 0.02150(8) Uani 1 1 d . . . . . Cu2 Cu 0.55269(4) 0.24141(2) 0.66345(2) 0.02233(8) Uani 1 1 d . . . . . P1 P 0.30216(8) 0.13406(5) 0.76281(5) 0.02110(14) Uani 1 1 d . . . . . P2 P 0.2701(5) 0.3966(4) 0.6363(3) 0.0235(5) Uani 0.633(7) 1 d D U P A 1 P2' P 0.2508(9) 0.3955(7) 0.6579(5) 0.0235(5) Uani 0.367(7) 1 d D U P A 2 P3 P 0.62718(8) 0.17796(5) 0.52710(5) 0.01953(13) Uani 1 1 d . . . . . N1 N 0.5961(3) 0.12340(17) 0.75726(16) 0.0224(5) Uani 1 1 d . . . . . N2 N 0.5225(3) 0.37401(17) 0.70831(17) 0.0256(5) Uani 1 1 d . . . . . N3 N 0.3425(3) 0.21076(16) 0.49414(16) 0.0218(4) Uani 1 1 d . . . . . C11 C 0.4887(3) 0.0703(2) 0.78719(18) 0.0221(5) Uani 1 1 d . . . . . C12 C 0.5224(3) -0.0220(2) 0.8306(2) 0.0289(6) Uani 1 1 d . . . . . H12 H 0.445208 -0.057731 0.852026 0.035 Uiso 1 1 calc R U . . . C13 C 0.6696(4) -0.0617(2) 0.8425(2) 0.0322(7) Uani 1 1 d . . . . . H13 H 0.694995 -0.125384 0.871282 0.039 Uiso 1 1 calc R U . . . C14 C 0.7786(4) -0.0078(2) 0.8123(2) 0.0317(7) Uani 1 1 d . . . . . H14 H 0.880381 -0.033580 0.819558 0.038 Uiso 1 1 calc R U . . . C15 C 0.7373(3) 0.0841(2) 0.7712(2) 0.0296(6) Uani 1 1 d . . . . . H15 H 0.812544 0.121731 0.751777 0.036 Uiso 1 1 calc R U . . . C16 C 0.1829(3) 0.0430(2) 0.7945(2) 0.0282(6) Uani 1 1 d . . . . . H16A H 0.112460 0.049467 0.750081 0.034 Uiso 1 1 calc R U . . . H16B H 0.246536 -0.023853 0.792969 0.034 Uiso 1 1 calc R U . . . C17 C 0.0949(5) 0.0618(4) 0.8925(3) 0.0558(11) Uani 1 1 d . . . . . H17A H -0.009348 0.098020 0.889044 0.067 Uiso 1 1 calc R U . . . H17B H 0.089024 -0.001281 0.928090 0.067 Uiso 1 1 calc R U . . . C18 C 0.1707(5) 0.1196(3) 0.9413(2) 0.0530(10) Uani 1 1 d . . . . . H18A H 0.258130 0.076547 0.964714 0.064 Uiso 1 1 calc R U . . . H18B H 0.099139 0.150466 0.994779 0.064 Uiso 1 1 calc R U . . . C19 C 0.2237(4) 0.1981(2) 0.8704(2) 0.0354(7) Uani 1 1 d . . . . . H19A H 0.301734 0.224399 0.891445 0.043 Uiso 1 1 calc R U . . . H19B H 0.137907 0.252640 0.860964 0.043 Uiso 1 1 calc R U . . . C21 C 0.3910(3) 0.4391(2) 0.7035(2) 0.0274(6) Uani 1 1 d . . . . . C22 C 0.3627(4) 0.5303(2) 0.7389(2) 0.0379(7) Uani 1 1 d . . . . . H22 H 0.269263 0.574865 0.736118 0.045 Uiso 1 1 calc R U . . . C23 C 0.4722(5) 0.5557(3) 0.7783(3) 0.0464(9) Uani 1 1 d . . . . . H23 H 0.453884 0.617626 0.803800 0.056 Uiso 1 1 calc R U . . . C24 C 0.6071(5) 0.4911(3) 0.7804(3) 0.0449(9) Uani 1 1 d . . . . . H24 H 0.684652 0.508133 0.805590 0.054 Uiso 1 1 calc R U . . . C25 C 0.6282(4) 0.4005(2) 0.7451(2) 0.0346(7) Uani 1 1 d . . . . . H25 H 0.721435 0.355360 0.746978 0.042 Uiso 1 1 calc R U . . . C31 C 0.4875(3) 0.20200(19) 0.44970(19) 0.0221(5) Uani 1 1 d . . . . . C32 C 0.5237(3) 0.2091(2) 0.3535(2) 0.0287(6) Uani 1 1 d . . . . . H32 H 0.625925 0.204726 0.323886 0.034 Uiso 1 1 calc R U . . . C33 C 0.4103(4) 0.2226(2) 0.3003(2) 0.0317(7) Uani 1 1 d . . . . . H33 H 0.433405 0.228198 0.234259 0.038 Uiso 1 1 calc R U . . . C34 C 0.2640(4) 0.2278(2) 0.3456(2) 0.0311(6) Uani 1 1 d . . . . . H34 H 0.184274 0.235376 0.311304 0.037 Uiso 1 1 calc R U . . . C35 C 0.2344(3) 0.2219(2) 0.4420(2) 0.0276(6) Uani 1 1 d . . . . . H35 H 0.132849 0.225808 0.472762 0.033 Uiso 1 1 calc R U . . . C36 C 0.8068(3) 0.1879(2) 0.4507(2) 0.0291(6) Uani 1 1 d . . . . . H36A H 0.787954 0.235174 0.397369 0.035 Uiso 1 1 calc R U . . . H36B H 0.872644 0.211130 0.485588 0.035 Uiso 1 1 calc R U . . . C37 C 0.8835(4) 0.0869(3) 0.4160(3) 0.0444(9) Uani 1 1 d . . . . . H37A H 0.917089 0.092297 0.347671 0.053 Uiso 1 1 calc R U . . . H37B H 0.973732 0.060436 0.445165 0.053 Uiso 1 1 calc R U . . . C38 C 0.7744(4) 0.0174(2) 0.4399(2) 0.0356(7) Uani 1 1 d . . . . . H38A H 0.710494 0.024677 0.391531 0.043 Uiso 1 1 calc R U . . . H38B H 0.831246 -0.051143 0.443373 0.043 Uiso 1 1 calc R U . . . C39 C 0.6766(3) 0.0437(2) 0.5338(2) 0.0259(6) Uani 1 1 d . . . . . H39A H 0.733400 0.018666 0.585143 0.031 Uiso 1 1 calc R U . . . H39B H 0.584644 0.016192 0.544006 0.031 Uiso 1 1 calc R U . . . C26 C 0.3168(7) 0.4554(4) 0.5198(4) 0.0300(12) Uani 0.633(7) 1 d D U P A 1 H26A H 0.427645 0.447089 0.500510 0.036 Uiso 0.633(7) 1 calc R U P A 1 H26B H 0.276825 0.426963 0.473286 0.036 Uiso 0.633(7) 1 calc R U P A 1 C27 C 0.2421(7) 0.5626(4) 0.5288(4) 0.0385(14) Uani 0.633(7) 1 d D U P A 1 H27A H 0.229911 0.594944 0.466693 0.046 Uiso 0.633(7) 1 calc R U P A 1 H27B H 0.304996 0.596125 0.556662 0.046 Uiso 0.633(7) 1 calc R U P A 1 C28 C 0.0839(16) 0.5678(9) 0.5929(10) 0.041(3) Uani 0.633(7) 1 d D U P A 1 H28A H 0.054791 0.629355 0.625414 0.050 Uiso 0.633(7) 1 calc R U P A 1 H28B H 0.007096 0.568006 0.554070 0.050 Uiso 0.633(7) 1 calc R U P A 1 C29 C 0.0870(6) 0.4830(4) 0.6630(5) 0.0369(14) Uani 0.633(7) 1 d D U P A 1 H29A H 0.003515 0.450267 0.660837 0.044 Uiso 0.633(7) 1 calc R U P A 1 H29B H 0.073656 0.505903 0.726333 0.044 Uiso 0.633(7) 1 calc R U P A 1 C26' C 0.2366(14) 0.4769(7) 0.5519(7) 0.040(2) Uani 0.367(7) 1 d D U P A 2 H26C H 0.330691 0.501572 0.531297 0.048 Uiso 0.367(7) 1 calc R U P A 2 H26D H 0.221822 0.440700 0.501058 0.048 Uiso 0.367(7) 1 calc R U P A 2 C27' C 0.102(3) 0.5625(15) 0.5743(18) 0.043(5) Uani 0.367(7) 1 d D U P A 2 H27C H 0.057382 0.587656 0.517955 0.051 Uiso 0.367(7) 1 calc R U P A 2 H27D H 0.133091 0.616300 0.598589 0.051 Uiso 0.367(7) 1 calc R U P A 2 C28' C -0.0165(12) 0.5193(7) 0.6508(8) 0.053(3) Uani 0.367(7) 1 d D U P A 2 H28C H -0.094203 0.572986 0.680801 0.063 Uiso 0.367(7) 1 calc R U P A 2 H28D H -0.067443 0.478561 0.621780 0.063 Uiso 0.367(7) 1 calc R U P A 2 C29' C 0.0685(9) 0.4579(6) 0.7227(7) 0.034(2) Uani 0.367(7) 1 d D U P A 2 H29C H 0.011026 0.409620 0.756351 0.041 Uiso 0.367(7) 1 calc R U P A 2 H29D H 0.084607 0.499806 0.768506 0.041 Uiso 0.367(7) 1 calc R U P A 2 O1 O 0.6595(7) 0.2113(4) 0.1133(3) 0.0525(10) Uiso 0.616(7) 1 d D . P B 1 H1O1 H 0.732550 0.216796 0.137374 0.079 Uiso 0.616(7) 1 calc R U P B 1 C90 C 0.6814(7) 0.2462(6) 0.0185(3) 0.0578(16) Uiso 0.616(7) 1 d D . P B 1 H90A H 0.783665 0.215449 -0.013206 0.069 Uiso 0.616(7) 1 calc R U P B 1 H90B H 0.673244 0.317828 0.014301 0.069 Uiso 0.616(7) 1 calc R U P B 1 C91 C 0.5620(10) 0.2218(7) -0.0292(5) 0.091(3) Uiso 0.616(7) 1 d D . P B 1 H91A H 0.580222 0.150911 -0.033393 0.136 Uiso 0.616(7) 1 calc R U P B 1 H91B H 0.567919 0.253826 -0.091993 0.136 Uiso 0.616(7) 1 calc R U P B 1 H91C H 0.461329 0.244969 0.007125 0.136 Uiso 0.616(7) 1 calc R U P B 1 O1' O 0.6867(12) 0.1912(7) 0.1024(5) 0.0525(10) Uiso 0.384(7) 1 d D . P B 2 H1O' H 0.772498 0.163011 0.113494 0.079 Uiso 0.384(7) 1 calc R U P B 2 C90' C 0.6879(13) 0.1957(7) 0.0051(5) 0.0578(16) Uiso 0.384(7) 1 d D . P B 2 H90C H 0.582984 0.208268 -0.006835 0.069 Uiso 0.384(7) 1 calc R U P B 2 H90D H 0.742879 0.132451 -0.020501 0.069 Uiso 0.384(7) 1 calc R U P B 2 C91' C 0.7651(15) 0.2774(8) -0.0429(6) 0.074(4) Uiso 0.384(7) 1 d D . P B 2 H91D H 0.691817 0.339909 -0.038958 0.111 Uiso 0.384(7) 1 calc R U P B 2 H91E H 0.804061 0.264162 -0.108435 0.111 Uiso 0.384(7) 1 calc R U P B 2 H91F H 0.848891 0.280634 -0.011962 0.111 Uiso 0.384(7) 1 calc R U P B 2 O2 O 1.2350(11) 0.3485(7) 0.1152(6) 0.110(3) Uiso 0.580(13) 1 d D . P C 1 H2O2 H 1.164267 0.334756 0.156152 0.166 Uiso 0.580(13) 1 calc R U P C 1 C92 C 1.1746(10) 0.4197(13) 0.0490(11) 0.183(5) Uiso 0.580(13) 1 d D . P C 1 H92A H 1.113289 0.478102 0.080960 0.219 Uiso 0.580(13) 1 calc R U P C 1 H92B H 1.108216 0.392984 0.017450 0.219 Uiso 0.580(13) 1 calc R U P C 1 C93 C 1.3040(14) 0.4482(9) -0.0228(7) 0.114(5) Uiso 0.580(13) 1 d D . P C 1 H93A H 1.332899 0.504377 -0.002278 0.171 Uiso 0.580(13) 1 calc R U P C 1 H93B H 1.271124 0.465535 -0.083096 0.171 Uiso 0.580(13) 1 calc R U P C 1 H93C H 1.391019 0.393026 -0.028908 0.171 Uiso 0.580(13) 1 calc R U P C 1 O2' O 1.1808(10) 0.3909(7) 0.1353(5) 0.064(3) Uiso 0.420(13) 1 d D . P C 2 H2O' H 1.199259 0.331602 0.153588 0.096 Uiso 0.420(13) 1 calc R U P C 2 C92' C 1.209(3) 0.3994(12) 0.0364(5) 0.183(5) Uiso 0.420(13) 1 d D . P C 2 H92C H 1.152563 0.358523 0.011927 0.219 Uiso 0.420(13) 1 calc R U P C 2 H92D H 1.318075 0.376116 0.012856 0.219 Uiso 0.420(13) 1 calc R U P C 2 C93' C 1.159(4) 0.5063(14) 0.0030(12) 0.255(19) Uiso 0.420(13) 1 d D . P C 2 H93D H 1.122039 0.509400 -0.055833 0.382 Uiso 0.420(13) 1 calc R U P C 2 H93E H 1.244969 0.538425 -0.006570 0.382 Uiso 0.420(13) 1 calc R U P C 2 H93F H 1.077904 0.539535 0.049921 0.382 Uiso 0.420(13) 1 calc R U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01770(13) 0.03038(15) 0.03692(17) -0.00058(12) -0.00226(11) -0.00467(11) Br2 0.0432(2) 0.0454(2) 0.0401(2) -0.00389(15) -0.00830(16) 0.00629(16) Cu1 0.01887(16) 0.02002(16) 0.02485(17) -0.00002(12) -0.00329(13) -0.00356(12) Cu2 0.02261(17) 0.01910(16) 0.02466(17) -0.00339(12) -0.00360(13) -0.00268(13) P1 0.0188(3) 0.0229(3) 0.0208(3) -0.0013(3) -0.0017(3) -0.0042(3) P2 0.0192(12) 0.0181(4) 0.0312(18) -0.0009(12) -0.0016(11) -0.0024(7) P2' 0.0192(12) 0.0181(4) 0.0312(18) -0.0009(12) -0.0016(11) -0.0024(7) P3 0.0178(3) 0.0179(3) 0.0227(3) -0.0025(2) -0.0026(3) -0.0035(2) N1 0.0218(11) 0.0230(11) 0.0230(11) 0.0007(9) -0.0040(9) -0.0068(9) N2 0.0230(12) 0.0232(12) 0.0303(13) -0.0062(9) -0.0025(10) -0.0042(9) N3 0.0200(11) 0.0206(11) 0.0241(11) -0.0001(9) -0.0049(9) -0.0026(9) C11 0.0233(13) 0.0241(13) 0.0191(12) -0.0014(10) -0.0039(10) -0.0054(10) C12 0.0283(15) 0.0256(14) 0.0335(16) 0.0050(12) -0.0078(12) -0.0078(12) C13 0.0323(16) 0.0259(15) 0.0392(17) 0.0054(13) -0.0135(14) -0.0048(12) C14 0.0245(15) 0.0334(16) 0.0371(17) 0.0016(13) -0.0114(13) -0.0025(12) C15 0.0220(14) 0.0348(16) 0.0328(16) 0.0019(12) -0.0054(12) -0.0085(12) C16 0.0270(15) 0.0335(16) 0.0266(14) 0.0036(12) -0.0053(12) -0.0133(12) C17 0.052(2) 0.079(3) 0.036(2) -0.0040(19) 0.0137(18) -0.032(2) C18 0.053(2) 0.081(3) 0.0233(17) -0.0093(18) 0.0024(16) -0.015(2) C19 0.0318(17) 0.0404(18) 0.0325(17) -0.0146(13) -0.0041(13) -0.0001(14) C21 0.0282(15) 0.0206(13) 0.0317(15) -0.0038(11) -0.0031(12) -0.0026(11) C22 0.0424(19) 0.0222(15) 0.047(2) -0.0093(13) -0.0069(16) 0.0002(13) C23 0.060(2) 0.0319(18) 0.052(2) -0.0171(16) -0.0127(19) -0.0116(17) C24 0.049(2) 0.044(2) 0.050(2) -0.0182(16) -0.0135(18) -0.0158(17) C25 0.0304(16) 0.0375(18) 0.0381(18) -0.0113(14) -0.0050(13) -0.0083(14) C31 0.0208(13) 0.0198(13) 0.0254(13) -0.0025(10) -0.0027(10) -0.0043(10) C32 0.0272(15) 0.0324(16) 0.0251(14) -0.0022(12) -0.0008(12) -0.0063(12) C33 0.0362(17) 0.0364(17) 0.0230(14) -0.0024(12) -0.0080(12) -0.0060(13) C34 0.0296(16) 0.0346(16) 0.0306(16) -0.0011(12) -0.0130(13) -0.0039(13) C35 0.0221(14) 0.0289(15) 0.0325(15) -0.0015(12) -0.0090(12) -0.0037(11) C36 0.0218(14) 0.0354(16) 0.0317(15) -0.0029(12) -0.0025(12) -0.0106(12) C37 0.0330(18) 0.0356(19) 0.048(2) 0.0030(15) 0.0142(15) 0.0059(14) C38 0.0412(18) 0.0231(15) 0.0340(17) -0.0072(12) 0.0020(14) 0.0058(13) C39 0.0286(15) 0.0195(13) 0.0290(14) -0.0013(10) -0.0034(12) -0.0054(11) C26 0.035(3) 0.022(2) 0.033(3) 0.002(2) -0.008(2) -0.007(2) C27 0.049(3) 0.023(2) 0.044(3) 0.006(2) -0.013(3) -0.005(2) C28 0.039(5) 0.029(4) 0.052(6) -0.007(3) -0.018(4) 0.011(3) C29 0.026(3) 0.022(2) 0.057(4) -0.005(2) -0.003(3) 0.002(2) C26' 0.047(6) 0.038(5) 0.042(6) 0.006(4) -0.018(5) -0.017(5) C27' 0.049(9) 0.033(8) 0.050(9) 0.005(6) -0.014(7) -0.015(6) C28' 0.047(6) 0.030(5) 0.080(7) -0.011(5) -0.022(5) 0.008(4) C29' 0.031(4) 0.023(4) 0.044(6) -0.010(4) -0.005(4) 0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N3 Cu1 P1 131.16(6) . . ? N3 Cu1 P2 101.19(12) . . ? P1 Cu1 P2 121.74(12) . . ? N3 Cu1 P2' 109.32(17) . . ? P1 Cu1 P2' 115.03(19) . . ? N3 Cu1 Br1 100.49(6) . . ? P1 Cu1 Br1 94.81(2) . . ? P2 Cu1 Br1 99.29(12) . . ? P2' Cu1 Br1 95.5(2) . . ? N3 Cu1 Cu2 94.28(6) . . ? P1 Cu1 Cu2 76.93(2) . . ? P2 Cu1 Cu2 75.37(12) . . ? P2' Cu1 Cu2 77.3(2) . . ? Br1 Cu1 Cu2 165.056(18) . . ? N2 Cu2 N1 117.77(10) . . ? N2 Cu2 P3 134.82(8) . . ? N1 Cu2 P3 103.89(7) . . ? N2 Cu2 Cu1 102.80(7) . . ? N1 Cu2 Cu1 101.60(6) . . ? P3 Cu2 Cu1 84.09(2) . . ? C11 P1 C19 100.78(14) . . ? C11 P1 C16 104.80(13) . . ? C19 P1 C16 93.46(15) . . ? C11 P1 Cu1 122.39(9) . . ? C19 P1 Cu1 111.48(11) . . ? C16 P1 Cu1 118.81(9) . . ? C26 P2 C29 93.0(3) . . ? C26 P2 C21 102.7(3) . . ? C29 P2 C21 103.3(3) . . ? C26 P2 Cu1 114.1(3) . . ? C29 P2 Cu1 119.1(3) . . ? C21 P2 Cu1 120.3(2) . . ? C21 P2' C29' 104.6(5) . . ? C21 P2' C26' 100.6(5) . . ? C29' P2' C26' 94.4(6) . . ? C21 P2' Cu1 122.1(4) . . ? C29' P2' Cu1 116.1(5) . . ? C26' P2' Cu1 114.6(5) . . ? C31 P3 C36 105.03(13) . . ? C31 P3 C39 101.24(13) . . ? C36 P3 C39 92.78(14) . . ? C31 P3 Cu2 116.18(10) . . ? C36 P3 Cu2 123.44(10) . . ? C39 P3 Cu2 113.84(10) . . ? C15 N1 C11 118.0(2) . . ? C15 N1 Cu2 121.16(19) . . ? C11 N1 Cu2 118.75(17) . . ? C25 N2 C21 118.8(3) . . ? C25 N2 Cu2 121.5(2) . . ? C21 N2 Cu2 119.66(19) . . ? C35 N3 C31 118.0(2) . . ? C35 N3 Cu1 117.6(2) . . ? C31 N3 Cu1 123.37(17) . . ? N1 C11 C12 121.5(3) . . ? N1 C11 P1 112.68(19) . . ? C12 C11 P1 125.8(2) . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 118.7(3) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N1 C15 C14 123.3(3) . . ? N1 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C17 C16 P1 107.4(2) . . ? C17 C16 H16A 110.2 . . ? P1 C16 H16A 110.2 . . ? C17 C16 H16B 110.2 . . ? P1 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C18 C17 C16 110.2(3) . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C17 C18 C19 107.4(3) . . ? C17 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? C17 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 P1 104.4(2) . . ? C18 C19 H19A 110.9 . . ? P1 C19 H19A 110.9 . . ? C18 C19 H19B 110.9 . . ? P1 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? N2 C21 C22 121.2(3) . . ? N2 C21 P2' 115.9(3) . . ? C22 C21 P2' 122.7(4) . . ? N2 C21 P2 112.7(2) . . ? C22 C21 P2 125.8(3) . . ? C23 C22 C21 119.2(3) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 118.6(3) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N2 C25 C24 122.5(3) . . ? N2 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N3 C31 C32 121.5(2) . . ? N3 C31 P3 114.5(2) . . ? C32 C31 P3 124.0(2) . . ? C31 C32 C33 119.9(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 118.4(3) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N3 C35 C34 123.1(3) . . ? N3 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C37 C36 P3 108.1(2) . . ? C37 C36 H36A 110.1 . . ? P3 C36 H36A 110.1 . . ? C37 C36 H36B 110.1 . . ? P3 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C38 C37 C36 110.4(3) . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C39 C38 C37 107.3(3) . . ? C39 C38 H38A 110.3 . . ? C37 C38 H38A 110.3 . . ? C39 C38 H38B 110.3 . . ? C37 C38 H38B 110.3 . . ? H38A C38 H38B 108.5 . . ? C38 C39 P3 104.66(19) . . ? C38 C39 H39A 110.8 . . ? P3 C39 H39A 110.8 . . ? C38 C39 H39B 110.8 . . ? P3 C39 H39B 110.8 . . ? H39A C39 H39B 108.9 . . ? C27 C26 P2 105.2(4) . . ? C27 C26 H26A 110.7 . . ? P2 C26 H26A 110.7 . . ? C27 C26 H26B 110.7 . . ? P2 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C26 C27 C28 107.4(6) . . ? C26 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? C26 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C29 C28 C27 111.1(7) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 P2 108.8(6) . . ? C28 C29 H29A 109.9 . . ? P2 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? P2 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? C27' C26' P2' 108.3(11) . . ? C27' C26' H26C 110.0 . . ? P2' C26' H26C 110.0 . . ? C27' C26' H26D 110.0 . . ? P2' C26' H26D 110.0 . . ? H26C C26' H26D 108.4 . . ? C26' C27' C28' 105.4(13) . . ? C26' C27' H27C 110.7 . . ? C28' C27' H27C 110.7 . . ? C26' C27' H27D 110.7 . . ? C28' C27' H27D 110.7 . . ? H27C C27' H27D 108.8 . . ? C29' C28' C27' 108.1(12) . . ? C29' C28' H28C 110.1 . . ? C27' C28' H28C 110.1 . . ? C29' C28' H28D 110.1 . . ? C27' C28' H28D 110.1 . . ? H28C C28' H28D 108.4 . . ? C28' C29' P2' 106.2(7) . . ? C28' C29' H29C 110.5 . . ? P2' C29' H29C 110.5 . . ? C28' C29' H29D 110.5 . . ? P2' C29' H29D 110.5 . . ? H29C C29' H29D 108.7 . . ? C90 O1 H1O1 109.5 . . ? O1 C90 C91 109.47(10) . . ? O1 C90 H90A 109.8 . . ? C91 C90 H90A 109.8 . . ? O1 C90 H90B 109.8 . . ? C91 C90 H90B 109.8 . . ? H90A C90 H90B 108.2 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90' O1' H1O' 109.5 . . ? O1' C90' C91' 109.55(10) . . ? O1' C90' H90C 109.8 . . ? C91' C90' H90C 109.8 . . ? O1' C90' H90D 109.8 . . ? C91' C90' H90D 109.8 . . ? H90C C90' H90D 108.2 . . ? C90' C91' H91D 109.5 . . ? C90' C91' H91E 109.5 . . ? H91D C91' H91E 109.5 . . ? C90' C91' H91F 109.5 . . ? H91D C91' H91F 109.5 . . ? H91E C91' H91F 109.5 . . ? C92 O2 H2O2 109.5 . . ? O2 C92 C93 109.37(10) . . ? O2 C92 H92A 109.8 . . ? C93 C92 H92A 109.8 . . ? O2 C92 H92B 109.8 . . ? C93 C92 H92B 109.8 . . ? H92A C92 H92B 108.2 . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C92' O2' H2O' 109.5 . . ? O2' C92' C93' 109.47(10) . . ? O2' C92' H92C 109.8 . . ? C93' C92' H92C 109.8 . . ? O2' C92' H92D 109.8 . . ? C93' C92' H92D 109.8 . . ? H92C C92' H92D 108.2 . . ? C92' C93' H93D 109.5 . . ? C92' C93' H93E 109.5 . . ? H93D C93' H93E 109.5 . . ? C92' C93' H93F 109.5 . . ? H93D C93' H93F 109.5 . . ? H93E C93' H93F 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 Cu1 2.5351(4) . ? Cu1 N3 2.097(2) . ? Cu1 P1 2.2362(7) . ? Cu1 P2 2.273(5) . ? Cu1 P2' 2.275(10) . ? Cu1 Cu2 2.7054(5) . ? Cu2 N2 1.985(2) . ? Cu2 N1 2.064(2) . ? Cu2 P3 2.1955(8) . ? P1 C11 1.835(3) . ? P1 C19 1.838(3) . ? P1 C16 1.841(3) . ? P2 C26 1.838(6) . ? P2 C29 1.843(6) . ? P2 C21 1.849(6) . ? P2' C21 1.809(11) . ? P2' C29' 1.841(10) . ? P2' C26' 1.843(10) . ? P3 C31 1.831(3) . ? P3 C36 1.838(3) . ? P3 C39 1.839(3) . ? N1 C15 1.341(4) . ? N1 C11 1.354(3) . ? N2 C25 1.338(4) . ? N2 C21 1.354(4) . ? N3 C35 1.343(3) . ? N3 C31 1.354(4) . ? C11 C12 1.385(4) . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.374(4) . ? C13 H13 0.9500 . ? C14 C15 1.375(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.524(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.494(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.535(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 C22 1.385(4) . ? C22 C23 1.384(5) . ? C22 H22 0.9500 . ? C23 C24 1.369(5) . ? C23 H23 0.9500 . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C31 C32 1.383(4) . ? C32 C33 1.391(4) . ? C32 H32 0.9500 . ? C33 C34 1.374(5) . ? C33 H33 0.9500 . ? C34 C35 1.384(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.529(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.527(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.523(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C26 C27 1.519(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.567(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.493(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C26' C27' 1.535(18) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? C27' C28' 1.58(2) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28' C29' 1.517(12) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' H29C 0.9900 . ? C29' H29D 0.9900 . ? O1 C90 1.4194(10) . ? O1 H1O1 0.8400 . ? C90 C91 1.5298(10) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? O1' C90' 1.4198(10) . ? O1' H1O' 0.8400 . ? C90' C91' 1.5298(10) . ? C90' H90C 0.9900 . ? C90' H90D 0.9900 . ? C91' H91D 0.9800 . ? C91' H91E 0.9800 . ? C91' H91F 0.9800 . ? O2 C92 1.4203(10) . ? O2 H2O2 0.8400 . ? C92 C93 1.5304(10) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? O2' C92' 1.4200(10) . ? O2' H2O' 0.8400 . ? C92' C93' 1.5302(10) . ? C92' H92C 0.9900 . ? C92' H92D 0.9900 . ? C93' H93D 0.9800 . ? C93' H93E 0.9800 . ? C93' H93F 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1O1 Br2 0.84 2.39 3.229(6) 173.0 . yes O2 H2O2 Br2 0.84 2.55 3.281(8) 146.4 . yes