# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address R.Farra ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; 'Klamroth, T.' ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; A.Winter ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; 'Thiel, K.' ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; A.Poppl ; University of Leipzig Institute of Experimental Physic Linn\'estr. 5 D-04103 Leipzig Germany ; A.Kelling ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; ; U.Schilde ; ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; A.Taubert ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; P.Strauch ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; _publ_contact_author_address ; University of Potsdam Institute of Chemistry Karl-Liebknecht-Str. 24-25 D-14476 Potsdam Germany ; _publ_contact_author_email us@chem.uni-potsdam.de _publ_contact_author_fax +49-331-977-5153 _publ_contact_author_phone +49-331-977-5188 #TrackingRef '- 818356_rev2.cif' _publ_contact_author_name 'Schilde, Uwe' _publ_section_title ; Tetrahalocuprates - Structure and EPR Spectroscopy. Part 1: Tetrabromocuprates(II) ; data_farra1 _database_code_depnum_ccdc_archive 'CCDC 818356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(hexadecyltrimethyammonium)tetrabromocuprate(II) ; _chemical_melting_point 486 _chemical_formula_moiety '2(C19 H42 N), Cu Br4' _chemical_formula_sum 'C38 H84 Br4 Cu N2' _chemical_formula_weight 952.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3459(15) _cell_length_b 17.513(3) _cell_length_c 30.135(5) _cell_angle_alpha 77.197(14) _cell_angle_beta 86.123(14) _cell_angle_gamma 84.763(13) _cell_volume 4783.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 9378 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 22.49 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 1.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 3.822 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.6806 _exptl_absorpt_correction_T_max 0.6829 _exptl_absorpt_process_details 'X-RED (Stoe, 2004)' _exptl_special_details ; A poor data set could only be obtained. ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method '\w scan, 1.0 \%' _diffrn_measurement_details ; 180 frames, exposure time per frame = 8 min ; _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 29666 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.2003 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 24.84 _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 24.84 _diffrn_measured_fraction_theta_full 0.927 _reflns_number_total 15318 _reflns_number_gt 5304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe, 2004)' _computing_cell_refinement 'X-AREA (Stoe, 2004)' _computing_data_reduction 'X-RED (Stoe, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2005) ; _refine_special_details ; The DFIX restraint was applied to improve the data-to-parameter ratio and to restrain the C-C bond lengths as well as the N-C bond lengths to chemically reasonable target values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15318 _refine_ls_number_parameters 825 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.2000 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.790 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.106 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.71908(16) 0.53777(8) 0.61596(5) 0.0757(5) Uani 1 1 d . . . Cu2 Cu 0.73928(14) 0.90975(7) 0.40314(5) 0.0612(4) Uani 1 1 d . . . Br1 Br 0.63739(17) 0.46450(8) 0.56515(5) 0.0982(5) Uani 1 1 d . . . Br2 Br 0.7888(2) 0.43407(8) 0.67675(5) 0.1110(6) Uani 1 1 d . . . Br3 Br 0.85556(19) 0.62738(8) 0.56020(6) 0.1095(5) Uani 1 1 d . . . Br4 Br 0.6031(2) 0.62779(12) 0.65676(6) 0.1504(8) Uani 1 1 d . . . Br5 Br 0.73642(14) 0.86061(7) 0.33628(4) 0.0805(4) Uani 1 1 d . . . Br6 Br 0.97476(14) 0.86314(8) 0.43001(5) 0.0919(5) Uani 1 1 d . . . Br7 Br 0.72596(16) 1.03766(7) 0.41756(6) 0.0992(5) Uani 1 1 d . . . Br8 Br 0.51767(14) 0.86254(7) 0.43987(4) 0.0769(4) Uani 1 1 d . . . N1 N 1.2777(11) 0.8016(5) 0.3296(3) 0.071(3) Uani 1 1 d D . . C1 C 1.3843(13) 0.7842(7) 0.2939(4) 0.075(4) Uani 1 1 d D . . H1A H 1.3794 0.7300 0.2918 0.090 Uiso 1 1 calc R . . H1B H 1.4797 0.7892 0.3033 0.090 Uiso 1 1 calc R . . C2 C 1.3644(17) 0.8365(9) 0.2470(5) 0.121(5) Uani 1 1 d D . . H2A H 1.2725 0.8284 0.2364 0.145 Uiso 1 1 calc R . . H2B H 1.3622 0.8910 0.2493 0.145 Uiso 1 1 calc R . . C3 C 1.4793(17) 0.8213(8) 0.2134(5) 0.110(5) Uani 1 1 d D . . H3A H 1.4903 0.7652 0.2148 0.132 Uiso 1 1 calc R . . H3B H 1.5687 0.8359 0.2225 0.132 Uiso 1 1 calc R . . C4 C 1.4596(17) 0.8617(9) 0.1653(5) 0.116(5) Uani 1 1 d D . . H4A H 1.3657 0.8514 0.1571 0.139 Uiso 1 1 calc R . . H4B H 1.4583 0.9178 0.1633 0.139 Uiso 1 1 calc R . . C5 C 1.5640(17) 0.8416(9) 0.1319(5) 0.118(5) Uani 1 1 d D . . H5A H 1.5656 0.7852 0.1348 0.141 Uiso 1 1 calc R . . H5B H 1.6571 0.8520 0.1406 0.141 Uiso 1 1 calc R . . C6 C 1.5535(17) 0.8778(8) 0.0833(5) 0.109(5) Uani 1 1 d D . . H6A H 1.4610 0.8668 0.0744 0.130 Uiso 1 1 calc R . . H6B H 1.5507 0.9342 0.0803 0.130 Uiso 1 1 calc R . . C7 C 1.6617(19) 0.8575(9) 0.0493(5) 0.122(6) Uani 1 1 d D . . H7A H 1.7533 0.8704 0.0578 0.146 Uiso 1 1 calc R . . H7B H 1.6672 0.8008 0.0534 0.146 Uiso 1 1 calc R . . C8 C 1.6534(18) 0.8893(9) 0.0011(6) 0.119(5) Uani 1 1 d D . . H8A H 1.5610 0.8771 -0.0073 0.143 Uiso 1 1 calc R . . H8B H 1.6494 0.9460 -0.0030 0.143 Uiso 1 1 calc R . . C9 C 1.7577(19) 0.8691(9) -0.0325(6) 0.124(6) Uani 1 1 d D . . H9A H 1.8497 0.8815 -0.0241 0.149 Uiso 1 1 calc R . . H9B H 1.7621 0.8124 -0.0280 0.149 Uiso 1 1 calc R . . C10 C 1.7526(19) 0.8986(10) -0.0800(5) 0.127(6) Uani 1 1 d D . . H10A H 1.7467 0.9554 -0.0846 0.153 Uiso 1 1 calc R . . H10B H 1.6615 0.8853 -0.0887 0.153 Uiso 1 1 calc R . . C11 C 1.8586(19) 0.8786(9) -0.1127(6) 0.122(6) Uani 1 1 d D . . H11A H 1.8647 0.8218 -0.1082 0.146 Uiso 1 1 calc R . . H11B H 1.9499 0.8920 -0.1042 0.146 Uiso 1 1 calc R . . C12 C 1.851(2) 0.9101(11) -0.1625(6) 0.143(7) Uani 1 1 d D . . H12A H 1.7624 0.8946 -0.1714 0.172 Uiso 1 1 calc R . . H12B H 1.8409 0.9669 -0.1669 0.172 Uiso 1 1 calc R . . C13 C 1.960(2) 0.8922(11) -0.1945(7) 0.148(7) Uani 1 1 d D A . H13A H 1.9661 0.8361 -0.1928 0.178 Uiso 1 1 calc R . . H13B H 2.0515 0.9045 -0.1853 0.178 Uiso 1 1 calc R . . C14 C 1.944(2) 0.9314(13) -0.2409(8) 0.183(10) Uani 1 1 d D . . H14A H 1.8940 0.9876 -0.2372 0.220 Uiso 0.50 1 d PD . . H14B H 1.8345 0.9272 -0.2493 0.220 Uiso 0.50 1 d PD . . H14C H 1.8675 0.9066 -0.2589 0.220 Uiso 0.50 1 d PD . . H14D H 1.9103 0.9872 -0.2332 0.220 Uiso 0.50 1 d PD . . C151 C 2.063(4) 0.883(2) -0.2678(13) 0.17(2) Uani 0.50 1 d PD A . H151 H 2.1636 0.8889 -0.2572 0.208 Uiso 0.50 1 d PD . . H152 H 2.0747 0.8233 -0.2732 0.208 Uiso 0.50 1 d PD . . C161 C 2.066(7) 0.925(3) -0.3121(15) 0.17(2) Uani 0.50 1 d PD . . H161 H 2.1477 0.8924 -0.3320 0.206 Uiso 0.50 1 d P . . H162 H 2.0954 0.9849 -0.3265 0.206 Uiso 0.50 1 d P . . H163 H 1.9610 0.9259 -0.3250 0.206 Uiso 0.50 1 d P . . C152 C 2.057(5) 0.947(3) -0.278(2) 0.16(2) Uani 0.50 1 d PD A 1 H153 H 2.1291 0.9883 -0.2712 0.195 Uiso 0.50 1 d P B 1 H154 H 2.0518 0.9775 -0.3167 0.195 Uiso 0.50 1 d P C 1 C162 C 2.090(10) 0.878(3) -0.2942(19) 0.28(5) Uani 0.50 1 d PD A 1 H164 H 2.1387 0.8360 -0.2648 0.335 Uiso 0.50 1 d P D 1 H165 H 2.0297 0.8415 -0.3076 0.335 Uiso 0.50 1 d P E 1 H166 H 2.1801 0.8886 -0.3219 0.335 Uiso 0.50 1 d P F 1 C17 C 1.3102(14) 0.7472(6) 0.3738(4) 0.090(4) Uani 1 1 d D . . H17A H 1.4074 0.7514 0.3809 0.136 Uiso 1 1 calc R . . H17B H 1.2988 0.6942 0.3716 0.136 Uiso 1 1 calc R . . H17C H 1.2454 0.7608 0.3975 0.136 Uiso 1 1 calc R . . C18 C 1.1296(13) 0.7941(7) 0.3194(4) 0.091(4) Uani 1 1 d D . . H18A H 1.0653 0.8065 0.3434 0.137 Uiso 1 1 calc R . . H18B H 1.1197 0.7413 0.3167 0.137 Uiso 1 1 calc R . . H18C H 1.1067 0.8297 0.2912 0.137 Uiso 1 1 calc R . . C19 C 1.2908(16) 0.8841(6) 0.3366(5) 0.102(5) Uani 1 1 d D . . H19A H 1.3880 0.8892 0.3433 0.154 Uiso 1 1 calc R . . H19B H 1.2269 0.8933 0.3616 0.154 Uiso 1 1 calc R . . H19C H 1.2657 0.9219 0.3094 0.154 Uiso 1 1 calc R . . N2 N 1.3077(9) 0.7066(4) 0.5505(3) 0.056(2) Uani 1 1 d D . . C20 C 1.2426(12) 0.6581(6) 0.5923(4) 0.066(3) Uani 1 1 d D . . H20A H 1.1831 0.6224 0.5830 0.079 Uiso 1 1 calc R . . H20B H 1.3201 0.6262 0.6091 0.079 Uiso 1 1 calc R . . C21 C 1.1546(13) 0.6979(6) 0.6242(4) 0.079(4) Uani 1 1 d D . . H21A H 1.0759 0.7297 0.6081 0.094 Uiso 1 1 calc R . . H21B H 1.2131 0.7329 0.6346 0.094 Uiso 1 1 calc R . . C22 C 1.0953(14) 0.6435(6) 0.6641(4) 0.075(4) Uani 1 1 d D . . H22A H 1.1747 0.6143 0.6811 0.090 Uiso 1 1 calc R . . H22B H 1.0434 0.6061 0.6534 0.090 Uiso 1 1 calc R . . C23 C 0.9970(16) 0.6806(8) 0.6958(4) 0.105(5) Uani 1 1 d D . . H23A H 0.9152 0.7071 0.6789 0.126 Uiso 1 1 calc R . . H23B H 1.0473 0.7207 0.7044 0.126 Uiso 1 1 calc R . . C24 C 0.9399(15) 0.6287(8) 0.7387(4) 0.094(4) Uani 1 1 d D . . H24A H 0.8796 0.5924 0.7304 0.113 Uiso 1 1 calc R . . H24B H 1.0205 0.5979 0.7543 0.113 Uiso 1 1 calc R . . C25 C 0.8556(17) 0.6702(8) 0.7710(5) 0.111(5) Uani 1 1 d D . . H25A H 0.7689 0.6957 0.7566 0.133 Uiso 1 1 calc R . . H25B H 0.9116 0.7110 0.7763 0.133 Uiso 1 1 calc R . . C26 C 0.8132(16) 0.6202(8) 0.8162(4) 0.103(5) Uani 1 1 d D . . H26A H 0.8989 0.5905 0.8291 0.123 Uiso 1 1 calc R . . H26B H 0.7492 0.5827 0.8111 0.123 Uiso 1 1 calc R . . C27 C 0.7409(17) 0.6626(8) 0.8505(5) 0.111(5) Uani 1 1 d D . . H27A H 0.8026 0.7022 0.8541 0.133 Uiso 1 1 calc R . . H27B H 0.6526 0.6899 0.8380 0.133 Uiso 1 1 calc R . . C28 C 0.7043(16) 0.6153(7) 0.8966(4) 0.101(5) Uani 1 1 d D . . H28A H 0.6387 0.5775 0.8931 0.121 Uiso 1 1 calc R . . H28B H 0.7918 0.5857 0.9083 0.121 Uiso 1 1 calc R . . C29 C 0.6399(17) 0.6557(8) 0.9318(5) 0.113(5) Uani 1 1 d D . . H29A H 0.5528 0.6858 0.9201 0.135 Uiso 1 1 calc R . . H29B H 0.7059 0.6930 0.9358 0.135 Uiso 1 1 calc R . . C30 C 0.6030(18) 0.6085(8) 0.9767(5) 0.115(5) Uani 1 1 d D . . H30A H 0.6896 0.5773 0.9879 0.138 Uiso 1 1 calc R . . H30B H 0.5351 0.5721 0.9727 0.138 Uiso 1 1 calc R . . C31 C 0.5406(18) 0.6490(8) 1.0134(5) 0.111(5) Uani 1 1 d D . . H31A H 0.6089 0.6848 1.0179 0.133 Uiso 1 1 calc R . . H31B H 0.4544 0.6806 1.0023 0.133 Uiso 1 1 calc R . . C32 C 0.5028(19) 0.5993(9) 1.0584(5) 0.124(6) Uani 1 1 d D . . H32A H 0.4366 0.5626 1.0537 0.148 Uiso 1 1 calc R . . H32B H 0.5896 0.5686 1.0697 0.148 Uiso 1 1 calc R . . C33 C 0.4383(19) 0.6380(9) 1.0944(5) 0.128(6) Uani 1 1 d D . . H33A H 0.5030 0.6759 1.0985 0.154 Uiso 1 1 calc R . . H33B H 0.3497 0.6673 1.0835 0.154 Uiso 1 1 calc R . . C34 C 0.405(2) 0.5889(10) 1.1390(6) 0.151(7) Uani 1 1 d D . . H34A H 0.4939 0.5588 1.1493 0.181 Uiso 1 1 calc R . . H34B H 0.3400 0.5515 1.1346 0.181 Uiso 1 1 calc R . . C35 C 0.341(2) 0.6253(11) 1.1779(6) 0.169(8) Uani 1 1 d D . . H35A H 0.4123 0.6526 1.1882 0.254 Uiso 1 1 calc R . . H35B H 0.3091 0.5847 1.2026 0.254 Uiso 1 1 calc R . . H35C H 0.2605 0.6615 1.1676 0.254 Uiso 1 1 calc R . . C36 C 1.1986(15) 0.7570(10) 0.5218(5) 0.144(7) Uani 1 1 d D . . H36A H 1.1316 0.7249 0.5135 0.216 Uiso 1 1 calc R . . H36B H 1.2451 0.7863 0.4949 0.216 Uiso 1 1 calc R . . H36C H 1.1482 0.7927 0.5386 0.216 Uiso 1 1 calc R . . C37 C 1.3930(19) 0.6599(7) 0.5232(5) 0.143(7) Uani 1 1 d D . . H37A H 1.3339 0.6240 0.5146 0.215 Uiso 1 1 calc R . . H37B H 1.4706 0.6309 0.5405 0.215 Uiso 1 1 calc R . . H37C H 1.4313 0.6936 0.4963 0.215 Uiso 1 1 calc R . . C38 C 1.401(2) 0.7585(9) 0.5614(5) 0.140(7) Uani 1 1 d D . . H38A H 1.3482 0.7913 0.5796 0.210 Uiso 1 1 calc R . . H38B H 1.4384 0.7908 0.5338 0.210 Uiso 1 1 calc R . . H38C H 1.4786 0.7287 0.5782 0.210 Uiso 1 1 calc R . . N3 N 0.2327(10) 1.0897(6) 0.4304(4) 0.073(3) Uani 1 1 d D . . C55 C 0.176(4) 1.0199(16) 0.4632(10) 0.161(12) Uiso 0.60 1 d PD . . H55A H 0.1436 1.0345 0.4913 0.241 Uiso 0.60 1 calc PR . . H55B H 0.2507 0.9782 0.4688 0.241 Uiso 0.60 1 calc PR . . H55C H 0.0967 1.0026 0.4503 0.241 Uiso 0.60 1 calc PR . . C55A C 0.361(3) 1.058(2) 0.4605(10) 0.153(12) Uiso 0.60 1 d PD . . H55D H 0.3410 1.0690 0.4902 0.229 Uiso 0.60 1 calc PR . . H55E H 0.4459 1.0827 0.4468 0.229 Uiso 0.60 1 calc PR . . H55F H 0.3775 1.0021 0.4633 0.229 Uiso 0.60 1 calc PR . . C56 C 0.081(3) 1.1083(19) 0.4179(11) 0.167(12) Uiso 0.60 1 d PD . . H56A H 0.0253 1.1252 0.4424 0.251 Uiso 0.60 1 calc PR . . H56B H 0.0434 1.0623 0.4123 0.251 Uiso 0.60 1 calc PR . . H56C H 0.0760 1.1494 0.3909 0.251 Uiso 0.60 1 calc PR . . C57 C 0.177(4) 1.1630(17) 0.4391(11) 0.169(13) Uiso 0.60 1 d PD . . H57A H 0.1551 1.1577 0.4712 0.253 Uiso 0.60 1 calc PR . . H57B H 0.0912 1.1803 0.4228 0.253 Uiso 0.60 1 calc PR . . H57C H 0.2473 1.2007 0.4292 0.253 Uiso 0.60 1 calc PR . . C57A C 0.330(5) 1.122(3) 0.4582(14) 0.23(2) Uiso 0.60 1 d PD . . H57D H 0.2775 1.1320 0.4852 0.346 Uiso 0.60 1 calc PR . . H57E H 0.3628 1.1707 0.4405 0.346 Uiso 0.60 1 calc PR . . H57F H 0.4107 1.0853 0.4665 0.346 Uiso 0.60 1 calc PR . . C39 C 0.278(2) 1.0711(18) 0.3904(6) 0.246(16) Uani 1 1 d D . . H39A H 0.3300 1.0202 0.3996 0.295 Uiso 1 1 calc R . . H39B H 0.1897 1.0607 0.3784 0.295 Uiso 1 1 calc R . . C40 C 0.3526(16) 1.1051(10) 0.3536(6) 0.121(6) Uani 1 1 d D . . H40A H 0.4347 1.1190 0.3673 0.145 Uiso 1 1 calc R . . H40B H 0.2945 1.1543 0.3447 0.145 Uiso 1 1 calc R . . C41 C 0.412(2) 1.0969(15) 0.3128(6) 0.202(12) Uani 1 1 d D . . H41A H 0.4854 1.0562 0.3253 0.243 Uiso 1 1 calc R . . H41B H 0.3370 1.0674 0.3059 0.243 Uiso 1 1 calc R . . C42 C 0.4681(19) 1.1096(12) 0.2737(6) 0.157(8) Uani 1 1 d D . . H42A H 0.5535 1.1313 0.2808 0.188 Uiso 1 1 calc R . . H42B H 0.4057 1.1558 0.2616 0.188 Uiso 1 1 calc R . . C43 C 0.519(2) 1.0948(14) 0.2334(7) 0.185(10) Uani 1 1 d D . . H43A H 0.5856 1.0501 0.2448 0.222 Uiso 1 1 calc R . . H43B H 0.4360 1.0712 0.2262 0.222 Uiso 1 1 calc R . . C44 C 0.576(2) 1.1137(14) 0.1924(6) 0.187(11) Uani 1 1 d D . . H44A H 0.5141 1.1608 0.1817 0.225 Uiso 1 1 calc R . . H44B H 0.6629 1.1335 0.1999 0.225 Uiso 1 1 calc R . . C45 C 0.621(2) 1.1004(14) 0.1533(7) 0.180(10) Uani 1 1 d D . . H45A H 0.5333 1.0820 0.1452 0.216 Uiso 1 1 calc R . . H45B H 0.6810 1.0525 0.1638 0.216 Uiso 1 1 calc R . . C46 C 0.681(2) 1.1216(14) 0.1118(6) 0.172(9) Uani 1 1 d D . . H46A H 0.6257 1.1714 0.1021 0.207 Uiso 1 1 calc R . . H46B H 0.7717 1.1362 0.1200 0.207 Uiso 1 1 calc R . . C47 C 0.721(2) 1.1090(13) 0.0728(7) 0.166(9) Uani 1 1 d D . . H47A H 0.6299 1.0935 0.0653 0.199 Uiso 1 1 calc R . . H47B H 0.7766 1.0595 0.0830 0.199 Uiso 1 1 calc R . . C48 C 0.778(2) 1.1264(14) 0.0317(7) 0.183(10) Uani 1 1 d D . . H48A H 0.7185 1.1749 0.0215 0.220 Uiso 1 1 calc R . . H48B H 0.8662 1.1441 0.0394 0.220 Uiso 1 1 calc R . . C49 C 0.821(2) 1.1158(16) -0.0077(8) 0.201(12) Uani 1 1 d D . . H49A H 0.7337 1.0967 -0.0154 0.241 Uiso 1 1 calc R . . H49B H 0.8829 1.0683 0.0021 0.241 Uiso 1 1 calc R . . C50 C 0.877(2) 1.1361(14) -0.0487(7) 0.175(9) Uani 1 1 d D . . H50A H 0.9640 1.1539 -0.0401 0.210 Uiso 1 1 calc R . . H50B H 0.8156 1.1842 -0.0574 0.210 Uiso 1 1 calc R . . C51 C 0.924(2) 1.1320(15) -0.0904(7) 0.195(11) Uani 1 1 d D . . H51A H 0.9734 1.0803 -0.0815 0.234 Uiso 1 1 calc R . . H51B H 0.8320 1.1211 -0.0997 0.234 Uiso 1 1 calc R . . C52 C 0.982(2) 1.1461(15) -0.1305(7) 0.183(10) Uani 1 1 d D . . H52A H 1.0778 1.1519 -0.1222 0.219 Uiso 1 1 calc R . . H52B H 0.9407 1.1998 -0.1397 0.219 Uiso 1 1 calc R . . C53 C 1.015(3) 1.1348(17) -0.1703(8) 0.230(14) Uani 1 1 d D . . H53A H 0.9197 1.1349 -0.1809 0.276 Uiso 1 1 calc R . . H53B H 1.0483 1.0795 -0.1623 0.276 Uiso 1 1 calc R . . C54 C 1.088(2) 1.1544(16) -0.2111(7) 0.219(12) Uani 1 1 d D . . H54A H 1.0331 1.1959 -0.2307 0.329 Uiso 1 1 calc R . . H54B H 1.1022 1.1095 -0.2247 0.329 Uiso 1 1 calc R . . H54C H 1.1794 1.1718 -0.2069 0.329 Uiso 1 1 calc R . . N4 N 1.1800(11) 1.3876(5) -0.4192(3) 0.073(3) Uani 1 1 d D . . C74 C 1.183(2) 1.4666(7) -0.4477(6) 0.159(8) Uani 1 1 d D . . H74A H 1.2728 1.4874 -0.4446 0.238 Uiso 1 1 calc R . . H74B H 1.1050 1.4999 -0.4383 0.238 Uiso 1 1 calc R . . H74C H 1.1743 1.4646 -0.4790 0.238 Uiso 1 1 calc R . . C75 C 1.3012(15) 1.3404(8) -0.4350(5) 0.109(5) Uani 1 1 d D . . H75A H 1.3892 1.3625 -0.4319 0.163 Uiso 1 1 calc R . . H75B H 1.2915 1.3400 -0.4665 0.163 Uiso 1 1 calc R . . H75C H 1.3027 1.2876 -0.4172 0.163 Uiso 1 1 calc R . . C76 C 1.0443(16) 1.3545(10) -0.4235(6) 0.139(6) Uani 1 1 d . . . H76A H 0.9654 1.3862 -0.4131 0.208 Uiso 1 1 calc R . . H76B H 1.0451 1.3019 -0.4054 0.208 Uiso 1 1 calc R . . H76C H 1.0336 1.3536 -0.4549 0.208 Uiso 1 1 calc R . . C58 C 1.182(2) 1.3875(15) -0.3683(9) 0.191(12) Uani 1 1 d D . . H58A H 1.1017 1.4235 -0.3621 0.229 Uiso 1 1 calc R . . H58B H 1.1580 1.3355 -0.3522 0.229 Uiso 1 1 calc R . . C59 C 1.283(3) 1.4028(15) -0.3488(9) 0.203(12) Uani 1 1 d D . . H59A H 1.2960 1.4577 -0.3620 0.243 Uiso 1 1 calc R . . H59B H 1.3664 1.3735 -0.3597 0.243 Uiso 1 1 calc R . . C60 C 1.304(3) 1.3941(15) -0.3001(9) 0.238(14) Uani 1 1 d D . . H60A H 1.3539 1.3427 -0.2900 0.285 Uiso 1 1 calc R . . H60B H 1.3706 1.4322 -0.2978 0.285 Uiso 1 1 calc R . . C61 C 1.193(2) 1.4006(13) -0.2677(9) 0.175(9) Uani 1 1 d D . . H61A H 1.1304 1.3594 -0.2678 0.210 Uiso 1 1 calc R . . H61B H 1.1377 1.4501 -0.2788 0.210 Uiso 1 1 calc R . . C62 C 1.220(3) 1.3974(13) -0.2186(7) 0.176(9) Uani 1 1 d D . . H62A H 1.2825 1.3503 -0.2083 0.211 Uiso 1 1 calc R . . H62B H 1.2758 1.4415 -0.2183 0.211 Uiso 1 1 calc R . . C63 C 1.112(2) 1.3981(12) -0.1858(8) 0.164(8) Uani 1 1 d D . . H63A H 1.0531 1.3559 -0.1876 0.196 Uiso 1 1 calc R . . H63B H 1.0525 1.4467 -0.1957 0.196 Uiso 1 1 calc R . . C64 C 1.131(2) 1.3914(11) -0.1380(7) 0.143(7) Uani 1 1 d D . . H64A H 1.1965 1.3449 -0.1290 0.171 Uiso 1 1 calc R . . H64B H 1.1848 1.4356 -0.1364 0.171 Uiso 1 1 calc R . . C65 C 1.023(2) 1.3873(12) -0.1023(7) 0.166(8) Uani 1 1 d D . . H65A H 0.9576 1.4331 -0.1123 0.199 Uiso 1 1 calc R . . H65B H 0.9717 1.3426 -0.1042 0.199 Uiso 1 1 calc R . . C66 C 1.031(2) 1.3820(11) -0.0554(6) 0.133(6) Uani 1 1 d D . . H66A H 1.0960 1.3358 -0.0454 0.159 Uiso 1 1 calc R . . H66B H 1.0841 1.4263 -0.0536 0.159 Uiso 1 1 calc R . . C67 C 0.926(2) 1.3788(13) -0.0203(7) 0.172(9) Uani 1 1 d D . . H67A H 0.8600 1.4242 -0.0309 0.207 Uiso 1 1 calc R . . H67B H 0.8751 1.3337 -0.0217 0.207 Uiso 1 1 calc R . . C68 C 0.931(2) 1.3754(12) 0.0245(7) 0.148(7) Uani 1 1 d D . . H68A H 0.9797 1.4212 0.0259 0.178 Uiso 1 1 calc R . . H68B H 0.9986 1.3308 0.0348 0.178 Uiso 1 1 calc R . . C69 C 0.827(2) 1.3708(11) 0.0603(8) 0.156(8) Uani 1 1 d D . . H69A H 0.7587 1.4150 0.0496 0.187 Uiso 1 1 calc R . . H69B H 0.7791 1.3246 0.0590 0.187 Uiso 1 1 calc R . . C70 C 0.829(3) 1.3679(13) 0.1063(9) 0.169(8) Uani 1 1 d D . . H70A H 0.8816 1.4124 0.1076 0.203 Uiso 1 1 calc R . . H70B H 0.8931 1.3219 0.1172 0.203 Uiso 1 1 calc R . . C71 C 0.725(2) 1.3664(14) 0.1415(10) 0.170(9) Uani 1 1 d D . . H71A H 0.6615 1.4128 0.1309 0.204 Uiso 1 1 calc R . . H71B H 0.6713 1.3223 0.1400 0.204 Uiso 1 1 calc R . . C72 C 0.729(3) 1.3627(17) 0.1869(9) 0.213(12) Uani 1 1 d D . . H72A H 0.7788 1.4079 0.1887 0.256 Uiso 1 1 calc R . . H72B H 0.7944 1.3173 0.1977 0.256 Uiso 1 1 calc R . . C73 C 0.616(2) 1.3591(13) 0.2227(8) 0.189(9) Uani 1 1 d D . . H73A H 0.5636 1.4094 0.2196 0.283 Uiso 1 1 calc R . . H73B H 0.6588 1.3449 0.2518 0.283 Uiso 1 1 calc R . . H73C H 0.5524 1.3204 0.2203 0.283 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 Cu1 0.0702(10) 0.0665(9) 0.0902(11) -0.0165(8) -0.0192(9) 0.0056(8) Cu2 0.0598(9) 0.0466(7) 0.0780(10) -0.0157(6) -0.0096(8) 0.0009(6) Br1 0.1174(12) 0.0739(8) 0.1078(11) -0.0114(7) -0.0346(10) -0.0297(8) Br2 0.1473(15) 0.0848(9) 0.0930(10) -0.0056(8) -0.0265(10) 0.0147(10) Br3 0.1270(14) 0.0851(10) 0.1178(12) -0.0051(8) -0.0270(11) -0.0414(9) Br4 0.1528(17) 0.1659(17) 0.1399(15) -0.0755(13) -0.0504(13) 0.0852(15) Br5 0.0831(10) 0.0820(8) 0.0815(9) -0.0283(7) -0.0107(8) -0.0027(7) Br6 0.0696(9) 0.0941(9) 0.1177(11) -0.0361(8) -0.0346(8) 0.0180(7) Br7 0.1039(11) 0.0561(7) 0.1465(13) -0.0388(8) -0.0188(10) -0.0015(7) Br8 0.0706(9) 0.0698(7) 0.0893(9) -0.0127(6) -0.0001(7) -0.0137(6) N1 0.072(7) 0.050(5) 0.084(7) -0.003(5) -0.022(6) 0.006(5) C1 0.065(8) 0.072(8) 0.082(9) -0.010(7) -0.004(7) 0.016(7) C2 0.115(13) 0.121(12) 0.115(13) -0.003(10) -0.017(11) 0.006(11) C3 0.122(13) 0.109(11) 0.086(11) -0.007(9) 0.014(10) 0.016(10) C4 0.114(13) 0.131(13) 0.091(12) -0.014(10) 0.015(11) 0.005(10) C5 0.117(13) 0.134(13) 0.089(12) -0.008(10) -0.003(10) 0.016(11) C6 0.116(13) 0.099(11) 0.099(12) 0.006(9) -0.011(10) -0.007(9) C7 0.152(16) 0.122(12) 0.085(12) -0.023(10) -0.001(11) 0.013(11) C8 0.132(15) 0.103(11) 0.113(14) -0.006(10) -0.014(12) -0.007(10) C9 0.140(16) 0.126(13) 0.106(14) -0.033(11) -0.007(12) 0.008(12) C10 0.144(16) 0.135(14) 0.092(13) -0.008(11) 0.000(12) 0.003(12) C11 0.136(15) 0.116(12) 0.112(14) -0.036(11) -0.001(12) 0.021(11) C12 0.157(18) 0.146(15) 0.116(15) -0.007(12) -0.008(14) -0.003(13) C13 0.156(19) 0.162(17) 0.130(17) -0.048(15) 0.012(16) -0.004(14) C14 0.19(2) 0.22(2) 0.122(18) -0.023(17) 0.014(17) 0.029(19) C151 0.32(8) 0.12(4) 0.09(4) -0.03(3) -0.02(4) -0.02(4) C161 0.26(6) 0.05(2) 0.18(5) 0.02(3) 0.03(4) -0.03(3) C152 0.15(4) 0.11(4) 0.23(6) -0.05(4) 0.01(4) 0.00(3) C162 0.64(14) 0.09(3) 0.10(4) 0.03(3) 0.01(6) -0.14(6) C17 0.105(11) 0.070(8) 0.085(9) 0.018(7) -0.020(8) -0.023(7) C18 0.069(9) 0.093(9) 0.108(11) -0.008(8) -0.012(8) -0.010(7) C19 0.126(13) 0.054(7) 0.129(12) -0.018(7) -0.028(10) -0.002(8) N2 0.059(6) 0.043(5) 0.069(6) -0.015(5) -0.006(5) -0.006(4) C20 0.072(8) 0.054(6) 0.065(7) -0.005(6) 0.002(7) 0.000(6) C21 0.093(10) 0.050(7) 0.079(9) 0.011(6) 0.006(8) -0.004(7) C22 0.101(10) 0.061(7) 0.061(8) -0.006(6) -0.019(7) 0.004(7) C23 0.133(13) 0.090(10) 0.079(10) -0.004(8) 0.016(10) 0.003(9) C24 0.100(11) 0.100(10) 0.078(10) -0.010(8) -0.007(9) -0.005(9) C25 0.129(13) 0.088(10) 0.100(11) 0.004(9) 0.007(10) 0.004(9) C26 0.122(13) 0.096(10) 0.082(10) -0.004(9) -0.005(9) -0.005(9) C27 0.130(14) 0.096(10) 0.096(11) -0.008(9) 0.010(10) 0.004(10) C28 0.128(13) 0.089(10) 0.079(10) -0.006(8) 0.007(9) -0.011(9) C29 0.135(14) 0.105(11) 0.095(11) -0.027(9) 0.022(10) 0.001(10) C30 0.146(15) 0.117(12) 0.073(10) -0.002(9) 0.020(10) -0.032(10) C31 0.150(15) 0.106(11) 0.072(10) -0.013(9) -0.007(10) 0.002(10) C32 0.150(16) 0.138(13) 0.079(11) -0.022(10) 0.003(11) -0.002(12) C33 0.162(17) 0.120(13) 0.092(12) -0.011(10) 0.014(11) 0.001(11) C34 0.21(2) 0.137(14) 0.100(13) -0.020(12) 0.028(14) -0.009(14) C35 0.21(2) 0.191(19) 0.115(14) -0.052(14) 0.040(15) -0.059(16) C36 0.089(11) 0.206(18) 0.095(11) 0.060(11) -0.027(9) 0.003(12) C37 0.196(18) 0.058(8) 0.154(14) -0.012(9) 0.069(14) 0.019(10) C38 0.199(19) 0.124(12) 0.102(11) 0.004(9) -0.019(12) -0.102(13) N3 0.056(7) 0.081(7) 0.086(8) -0.033(6) -0.018(6) 0.009(5) C39 0.16(2) 0.50(5) 0.072(14) -0.07(2) -0.008(14) 0.03(3) C40 0.080(11) 0.177(16) 0.095(12) -0.019(11) -0.012(10) 0.033(11) C41 0.129(18) 0.38(4) 0.080(13) -0.041(18) 0.010(13) 0.039(19) C42 0.094(14) 0.26(2) 0.113(15) -0.058(16) 0.001(12) 0.024(14) C43 0.126(18) 0.30(3) 0.135(18) -0.09(2) -0.005(15) 0.042(18) C44 0.118(16) 0.35(3) 0.097(15) -0.072(18) 0.040(13) 0.002(17) C45 0.097(15) 0.33(3) 0.127(17) -0.10(2) 0.000(13) 0.002(17) C46 0.118(17) 0.31(3) 0.093(14) -0.054(17) 0.005(13) 0.001(17) C47 0.140(18) 0.27(3) 0.101(15) -0.074(17) 0.020(14) -0.027(16) C48 0.107(16) 0.33(3) 0.119(17) -0.08(2) 0.002(14) 0.021(17) C49 0.112(17) 0.38(4) 0.121(18) -0.09(2) 0.017(15) -0.027(19) C50 0.121(17) 0.30(3) 0.107(16) -0.064(18) -0.005(14) 0.018(17) C51 0.119(18) 0.36(3) 0.121(18) -0.09(2) -0.019(16) 0.00(2) C52 0.139(19) 0.32(3) 0.110(16) -0.10(2) -0.009(15) 0.005(19) C53 0.18(2) 0.40(4) 0.14(2) -0.12(3) -0.029(19) 0.06(2) C54 0.16(2) 0.40(4) 0.113(17) -0.10(2) 0.021(16) -0.05(2) N4 0.079(8) 0.059(6) 0.083(7) -0.023(5) 0.010(6) -0.011(5) C74 0.189(19) 0.043(8) 0.23(2) 0.021(10) -0.060(16) -0.021(10) C75 0.105(12) 0.114(11) 0.110(11) -0.044(9) 0.004(10) 0.019(10) C76 0.078(11) 0.176(16) 0.185(18) -0.079(14) 0.006(12) -0.044(11) C58 0.096(16) 0.28(3) 0.25(3) -0.17(2) -0.071(18) 0.021(17) C59 0.22(3) 0.21(3) 0.16(2) -0.017(19) -0.07(2) 0.06(2) C60 0.38(5) 0.18(2) 0.16(2) -0.037(19) 0.04(3) -0.05(3) C61 0.15(2) 0.20(2) 0.18(2) -0.085(19) -0.009(18) 0.042(16) C62 0.22(3) 0.20(2) 0.117(17) -0.063(16) 0.005(18) 0.018(18) C63 0.18(2) 0.18(2) 0.14(2) -0.071(16) -0.019(18) -0.001(16) C64 0.17(2) 0.137(15) 0.125(16) -0.029(13) -0.030(15) 0.005(13) C65 0.20(2) 0.177(19) 0.128(18) -0.048(15) 0.007(18) -0.033(16) C66 0.138(17) 0.159(16) 0.098(14) -0.013(12) -0.032(13) -0.018(13) C67 0.22(3) 0.21(2) 0.103(16) -0.065(15) 0.018(17) -0.029(18) C68 0.147(19) 0.174(18) 0.135(18) -0.048(15) -0.010(16) -0.029(14) C69 0.19(2) 0.145(16) 0.145(19) -0.065(15) 0.024(18) -0.028(14) C70 0.18(2) 0.18(2) 0.16(2) -0.060(18) -0.026(19) -0.012(17) C71 0.15(2) 0.19(2) 0.19(3) -0.07(2) 0.00(2) -0.021(16) C72 0.23(3) 0.28(3) 0.14(2) -0.06(2) -0.02(2) -0.04(2) C73 0.18(2) 0.19(2) 0.20(2) -0.060(18) 0.036(19) -0.041(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 Br4 2.353(2) . ? Cu1 Br2 2.356(2) . ? Cu1 Br1 2.404(2) . ? Cu1 Br3 2.412(2) . ? Cu2 Br5 2.3627(18) . ? Cu2 Br7 2.3653(17) . ? Cu2 Br6 2.4053(19) . ? Cu2 Br8 2.4073(19) . ? N1 C18 1.462(14) . ? N1 C1 1.479(13) . ? N1 C17 1.488(12) . ? N1 C19 1.523(13) . ? C1 C2 1.518(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.474(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.481(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.433(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.467(16) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.466(16) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.442(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.436(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.411(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.427(17) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.482(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.417(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.43(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C152 1.47(4) . ? C14 C151 1.62(4) . ? C14 H14A 1.0744 . ? C14 H14B 1.0790 . ? C14 H14C 1.0952 . ? C14 H14D 1.0683 . ? C151 C161 1.37(4) . ? C151 H151 1.0383 . ? C151 H152 1.0870 . ? C151 H164 1.0292 . ? C151 H165 1.5928 . ? C161 H161 1.1245 . ? C161 H162 1.0990 . ? C161 H163 1.0794 . ? C161 H154 0.9040 . ? C161 H165 1.5013 . ? C161 H166 1.2377 . ? C152 C162 1.41(4) . ? C152 H151 1.4215 . ? C152 H162 1.5128 . ? C152 H153 1.0937 . ? C152 H154 1.1855 . ? C162 H151 1.4064 . ? C162 H152 1.0365 . ? C162 H161 1.2109 . ? C162 H164 1.1096 . ? C162 H165 1.0458 . ? C162 H166 1.1422 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N2 C38 1.417(15) . ? N2 C37 1.439(13) . ? N2 C36 1.477(13) . ? N2 C20 1.482(12) . ? C20 C21 1.474(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.468(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.492(14) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.503(15) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.483(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.496(15) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.495(15) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.487(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.467(15) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.459(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.500(16) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.478(16) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.471(16) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.456(17) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.521(17) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N3 C39 1.348(19) . ? N3 C57 1.41(3) . ? N3 C56 1.48(3) . ? N3 C57A 1.50(3) . ? N3 C55 1.50(3) . ? N3 C55A 1.54(3) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C55A H55D 0.9600 . ? C55A H55E 0.9600 . ? C55A H55F 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C57A H57D 0.9600 . ? C57A H57E 0.9600 . ? C57A H57F 0.9600 . ? C39 C40 1.32(2) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.347(19) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.235(19) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.35(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.29(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.286(19) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.33(2) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.266(19) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.30(2) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.28(2) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.29(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.32(2) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.27(2) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.27(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.35(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? N4 C74 1.461(14) . ? N4 C75 1.458(12) . ? N4 C76 1.467(16) . ? N4 C58 1.54(2) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C58 C59 1.23(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.46(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.39(2) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.51(2) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.37(2) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.45(2) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.42(2) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.40(2) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.39(2) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.34(2) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.39(2) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.38(2) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.38(2) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.36(2) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.45(2) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br4 Cu1 Br2 100.17(8) . . ? Br4 Cu1 Br1 133.51(9) . . ? Br2 Cu1 Br1 100.05(7) . . ? Br4 Cu1 Br3 98.88(9) . . ? Br2 Cu1 Br3 132.22(9) . . ? Br1 Cu1 Br3 97.66(8) . . ? Br5 Cu2 Br7 133.72(8) . . ? Br5 Cu2 Br6 102.71(7) . . ? Br7 Cu2 Br6 99.21(7) . . ? Br5 Cu2 Br8 98.70(7) . . ? Br7 Cu2 Br8 101.43(7) . . ? Br6 Cu2 Br8 124.70(7) . . ? C18 N1 C1 113.1(9) . . ? C18 N1 C17 108.7(10) . . ? C1 N1 C17 109.3(9) . . ? C18 N1 C19 109.3(9) . . ? C1 N1 C19 110.0(10) . . ? C17 N1 C19 106.2(9) . . ? N1 C1 C2 114.7(10) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 112.9(12) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 C4 117.0(12) . . ? C2 C3 H3A 108.1 . . ? C4 C3 H3A 108.1 . . ? C2 C3 H3B 108.1 . . ? C4 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C5 C4 C3 117.2(13) . . ? C5 C4 H4A 108.0 . . ? C3 C4 H4A 108.0 . . ? C5 C4 H4B 108.0 . . ? C3 C4 H4B 108.0 . . ? H4A C4 H4B 107.2 . . ? C4 C5 C6 121.5(13) . . ? C4 C5 H5A 107.0 . . ? C6 C5 H5A 107.0 . . ? C4 C5 H5B 107.0 . . ? C6 C5 H5B 107.0 . . ? H5A C5 H5B 106.7 . . ? C7 C6 C5 121.2(13) . . ? C7 C6 H6A 107.0 . . ? C5 C6 H6A 107.0 . . ? C7 C6 H6B 107.0 . . ? C5 C6 H6B 107.0 . . ? H6A C6 H6B 106.8 . . ? C8 C7 C6 123.3(14) . . ? C8 C7 H7A 106.5 . . ? C6 C7 H7A 106.5 . . ? C8 C7 H7B 106.5 . . ? C6 C7 H7B 106.5 . . ? H7A C7 H7B 106.5 . . ? C9 C8 C7 123.8(15) . . ? C9 C8 H8A 106.4 . . ? C7 C8 H8A 106.4 . . ? C9 C8 H8B 106.4 . . ? C7 C8 H8B 106.4 . . ? H8A C8 H8B 106.5 . . ? C10 C9 C8 125.4(15) . . ? C10 C9 H9A 106.0 . . ? C8 C9 H9A 106.0 . . ? C10 C9 H9B 106.0 . . ? C8 C9 H9B 106.0 . . ? H9A C9 H9B 106.3 . . ? C9 C10 C11 124.4(16) . . ? C9 C10 H10A 106.2 . . ? C11 C10 H10A 106.2 . . ? C9 C10 H10B 106.2 . . ? C11 C10 H10B 106.2 . . ? H10A C10 H10B 106.4 . . ? C10 C11 C12 123.6(15) . . ? C10 C11 H11A 106.4 . . ? C12 C11 H11A 106.4 . . ? C10 C11 H11B 106.4 . . ? C12 C11 H11B 106.4 . . ? H11A C11 H11B 106.5 . . ? C13 C12 C11 123.0(17) . . ? C13 C12 H12A 106.6 . . ? C11 C12 H12A 106.6 . . ? C13 C12 H12B 106.6 . . ? C11 C12 H12B 106.6 . . ? H12A C12 H12B 106.5 . . ? C12 C13 C14 116.7(18) . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 C152 128(3) . . ? C13 C14 C151 103(2) . . ? C152 C14 C151 41(2) . . ? C13 C14 H14A 101.3 . . ? C152 C14 H14A 106.9 . . ? C151 C14 H14A 147.7 . . ? C13 C14 H14B 108.2 . . ? C152 C14 H14B 119.8 . . ? C151 C14 H14B 113.6 . . ? H14A C14 H14B 78.8 . . ? C13 C14 H14C 114.8 . . ? C152 C14 H14C 98.6 . . ? C151 C14 H14C 83.4 . . ? H14A C14 H14C 105.9 . . ? H14B C14 H14C 30.3 . . ? C13 C14 H14D 94.5 . . ? C152 C14 H14D 105.6 . . ? C151 C14 H14D 145.5 . . ? H14A C14 H14D 10.7 . . ? H14B C14 H14D 88.6 . . ? H14C C14 H14D 116.4 . . ? C161 C151 C14 105(3) . . ? C161 C151 H151 102.8 . . ? C14 C151 H151 108.5 . . ? C161 C151 H152 100.2 . . ? C14 C151 H152 134.3 . . ? H151 C151 H152 101.7 . . ? C161 C151 H164 108.8 . . ? C14 C151 H164 145.7 . . ? H151 C151 H164 61.1 . . ? H152 C151 H164 40.6 . . ? C161 C151 H165 60.3 . . ? C14 C151 H165 125.0 . . ? H151 C151 H165 126.2 . . ? H152 C151 H165 44.3 . . ? H164 C151 H165 76.2 . . ? C151 C161 H161 107.5 . . ? C151 C161 H162 130.1 . . ? H161 C161 H162 98.9 . . ? C151 C161 H163 107.7 . . ? H161 C161 H163 109.8 . . ? H162 C161 H163 101.7 . . ? C151 C161 H154 117.0 . . ? H161 C161 H154 124.8 . . ? H162 C161 H154 26.5 . . ? H163 C161 H154 86.6 . . ? C151 C161 H165 67.1 . . ? H161 C161 H165 69.4 . . ? H162 C161 H165 162.5 . . ? H163 C161 H165 71.7 . . ? H154 C161 H165 157.8 . . ? C151 C161 H166 92.8 . . ? H161 C161 H166 20.5 . . ? H162 C161 H166 98.8 . . ? H163 C161 H166 129.1 . . ? H154 C161 H166 124.9 . . ? H165 C161 H166 74.8 . . ? C162 C152 C14 108(4) . . ? C162 C152 H151 59.6 . . ? C14 C152 H151 97.9 . . ? C162 C152 H162 81.9 . . ? C14 C152 H162 147.4 . . ? H151 C152 H162 113.5 . . ? C162 C152 H153 129.0 . . ? C14 C152 H153 111.2 . . ? H151 C152 H153 84.2 . . ? H162 C152 H153 81.5 . . ? C162 C152 H154 83.9 . . ? C14 C152 H154 131.9 . . ? H151 C152 H154 126.7 . . ? H162 C152 H154 16.0 . . ? H153 C152 H154 92.4 . . ? C152 C162 H151 60.7 . . ? C152 C162 H152 120.1 . . ? H151 C162 H152 83.4 . . ? C152 C162 H161 111.0 . . ? H151 C162 H161 118.9 . . ? H152 C162 H161 128.6 . . ? C152 C162 H164 103.2 . . ? H151 C162 H164 47.6 . . ? H152 C162 H164 39.9 . . ? H161 C162 H164 123.7 . . ? C152 C162 H165 134.1 . . ? H151 C162 H165 148.0 . . ? H152 C162 H165 64.7 . . ? H161 C162 H165 84.8 . . ? H164 C162 H165 102.2 . . ? C152 C162 H166 108.8 . . ? H151 C162 H166 99.1 . . ? H152 C162 H166 123.9 . . ? H161 C162 H166 21.0 . . ? H164 C162 H166 105.9 . . ? H165 C162 H166 100.0 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C38 N2 C37 106.4(11) . . ? C38 N2 C36 105.6(11) . . ? C37 N2 C36 108.7(11) . . ? C38 N2 C20 111.0(9) . . ? C37 N2 C20 112.5(8) . . ? C36 N2 C20 112.3(9) . . ? C21 C20 N2 118.7(8) . . ? C21 C20 H20A 107.6 . . ? N2 C20 H20A 107.6 . . ? C21 C20 H20B 107.6 . . ? N2 C20 H20B 107.6 . . ? H20A C20 H20B 107.1 . . ? C20 C21 C22 113.5(9) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 115.5(10) . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C22 C23 C24 118.1(11) . . ? C22 C23 H23A 107.8 . . ? C24 C23 H23A 107.8 . . ? C22 C23 H23B 107.8 . . ? C24 C23 H23B 107.8 . . ? H23A C23 H23B 107.1 . . ? C25 C24 C23 115.4(11) . . ? C25 C24 H24A 108.4 . . ? C23 C24 H24A 108.4 . . ? C25 C24 H24B 108.4 . . ? C23 C24 H24B 108.4 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 116.0(11) . . ? C24 C25 H25A 108.3 . . ? C26 C25 H25A 108.3 . . ? C24 C25 H25B 108.3 . . ? C26 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C27 116.2(12) . . ? C25 C26 H26A 108.2 . . ? C27 C26 H26A 108.2 . . ? C25 C26 H26B 108.2 . . ? C27 C26 H26B 108.2 . . ? H26A C26 H26B 107.4 . . ? C28 C27 C26 117.7(11) . . ? C28 C27 H27A 107.9 . . ? C26 C27 H27A 107.9 . . ? C28 C27 H27B 107.9 . . ? C26 C27 H27B 107.9 . . ? H27A C27 H27B 107.2 . . ? C29 C28 C27 119.0(12) . . ? C29 C28 H28A 107.6 . . ? C27 C28 H28A 107.6 . . ? C29 C28 H28B 107.6 . . ? C27 C28 H28B 107.6 . . ? H28A C28 H28B 107.0 . . ? C28 C29 C30 118.4(12) . . ? C28 C29 H29A 107.7 . . ? C30 C29 H29A 107.7 . . ? C28 C29 H29B 107.7 . . ? C30 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? C29 C30 C31 119.1(12) . . ? C29 C30 H30A 107.5 . . ? C31 C30 H30A 107.5 . . ? C29 C30 H30B 107.5 . . ? C31 C30 H30B 107.5 . . ? H30A C30 H30B 107.0 . . ? C32 C31 C30 117.7(12) . . ? C32 C31 H31A 107.9 . . ? C30 C31 H31A 107.9 . . ? C32 C31 H31B 107.9 . . ? C30 C31 H31B 107.9 . . ? H31A C31 H31B 107.2 . . ? C33 C32 C31 118.4(13) . . ? C33 C32 H32A 107.7 . . ? C31 C32 H32A 107.7 . . ? C33 C32 H32B 107.7 . . ? C31 C32 H32B 107.7 . . ? H32A C32 H32B 107.1 . . ? C34 C33 C32 118.1(14) . . ? C34 C33 H33A 107.8 . . ? C32 C33 H33A 107.8 . . ? C34 C33 H33B 107.8 . . ? C32 C33 H33B 107.8 . . ? H33A C33 H33B 107.1 . . ? C33 C34 C35 120.7(15) . . ? C33 C34 H34A 107.2 . . ? C35 C34 H34A 107.2 . . ? C33 C34 H34B 107.2 . . ? C35 C34 H34B 107.2 . . ? H34A C34 H34B 106.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N2 C36 H36A 109.5 . . ? N2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2 C37 H37A 109.5 . . ? N2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 N3 C57 129(2) . . ? C39 N3 C56 94.3(16) . . ? C57 N3 C56 68.3(17) . . ? C39 N3 C57A 122(2) . . ? C57 N3 C57A 67.3(19) . . ? C56 N3 C57A 134(2) . . ? C39 N3 C55 110.9(18) . . ? C57 N3 C55 114.3(18) . . ? C56 N3 C55 84.3(18) . . ? C57A N3 C55 104(2) . . ? C39 N3 C55A 102.5(15) . . ? C57 N3 C55A 109.3(19) . . ? C56 N3 C55A 158.6(19) . . ? C57A N3 C55A 43.5(18) . . ? C55 N3 C55A 77.4(17) . . ? N3 C55 H55A 109.5 . . ? N3 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N3 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C55A H55D 109.5 . . ? N3 C55A H55E 109.5 . . ? H55D C55A H55E 109.5 . . ? N3 C55A H55F 109.5 . . ? H55D C55A H55F 109.5 . . ? H55E C55A H55F 109.5 . . ? N3 C56 H56A 109.5 . . ? N3 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N3 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N3 C57 H57A 109.5 . . ? N3 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N3 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N3 C57A H57D 109.5 . . ? N3 C57A H57E 109.5 . . ? H57D C57A H57E 109.5 . . ? N3 C57A H57F 109.5 . . ? H57D C57A H57F 109.5 . . ? H57E C57A H57F 109.5 . . ? C40 C39 N3 136(3) . . ? C40 C39 H39A 103.3 . . ? N3 C39 H39A 103.3 . . ? C40 C39 H39B 103.3 . . ? N3 C39 H39B 103.3 . . ? H39A C39 H39B 105.2 . . ? C39 C40 C41 145(2) . . ? C39 C40 H40A 100.5 . . ? C41 C40 H40A 100.5 . . ? C39 C40 H40B 100.5 . . ? C41 C40 H40B 100.5 . . ? H40A C40 H40B 104.3 . . ? C42 C41 C40 164(3) . . ? C42 C41 H41A 95.0 . . ? C40 C41 H41A 95.0 . . ? C42 C41 H41B 95.0 . . ? C40 C41 H41B 95.0 . . ? H41A C41 H41B 103.2 . . ? C41 C42 C43 158(3) . . ? C41 C42 H42A 96.7 . . ? C43 C42 H42A 96.7 . . ? C41 C42 H42B 96.7 . . ? C43 C42 H42B 96.7 . . ? H42A C42 H42B 103.5 . . ? C44 C43 C42 154(3) . . ? C44 C43 H43A 97.9 . . ? C42 C43 H43A 97.9 . . ? C44 C43 H43B 97.9 . . ? C42 C43 H43B 97.9 . . ? H43A C43 H43B 103.7 . . ? C45 C44 C43 154(3) . . ? C45 C44 H44A 97.9 . . ? C43 C44 H44A 97.9 . . ? C45 C44 H44B 97.9 . . ? C43 C44 H44B 97.9 . . ? H44A C44 H44B 103.7 . . ? C44 C45 C46 153(3) . . ? C44 C45 H45A 98.4 . . ? C46 C45 H45A 98.4 . . ? C44 C45 H45B 98.4 . . ? C46 C45 H45B 98.4 . . ? H45A C45 H45B 103.8 . . ? C47 C46 C45 152(3) . . ? C47 C46 H46A 98.5 . . ? C45 C46 H46A 98.5 . . ? C47 C46 H46B 98.5 . . ? C45 C46 H46B 98.5 . . ? H46A C46 H46B 103.8 . . ? C46 C47 C48 155(2) . . ? C46 C47 H47A 97.6 . . ? C48 C47 H47A 97.6 . . ? C46 C47 H47B 97.6 . . ? C48 C47 H47B 97.6 . . ? H47A C47 H47B 103.6 . . ? C49 C48 C47 157(3) . . ? C49 C48 H48A 97.0 . . ? C47 C48 H48A 97.0 . . ? C49 C48 H48B 97.0 . . ? C47 C48 H48B 97.0 . . ? H48A C48 H48B 103.5 . . ? C48 C49 C50 155(3) . . ? C48 C49 H49A 97.6 . . ? C50 C49 H49A 97.6 . . ? C48 C49 H49B 97.6 . . ? C50 C49 H49B 97.6 . . ? H49A C49 H49B 103.6 . . ? C49 C50 C51 160(3) . . ? C49 C50 H50A 96.1 . . ? C51 C50 H50A 96.1 . . ? C49 C50 H50B 96.1 . . ? C51 C50 H50B 96.1 . . ? H50A C50 H50B 103.4 . . ? C52 C51 C50 164(3) . . ? C52 C51 H51A 94.8 . . ? C50 C51 H51A 94.8 . . ? C52 C51 H51B 94.8 . . ? C50 C51 H51B 94.8 . . ? H51A C51 H51B 103.2 . . ? C51 C52 C53 157(3) . . ? C51 C52 H52A 97.2 . . ? C53 C52 H52A 97.2 . . ? C51 C52 H52B 97.2 . . ? C53 C52 H52B 97.2 . . ? H52A C52 H52B 103.6 . . ? C52 C53 C54 151(3) . . ? C52 C53 H53A 99.0 . . ? C54 C53 H53A 99.0 . . ? C52 C53 H53B 99.0 . . ? C54 C53 H53B 99.0 . . ? H53A C53 H53B 103.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C74 N4 C75 106.7(11) . . ? C74 N4 C76 110.4(13) . . ? C75 N4 C76 110.3(10) . . ? C74 N4 C58 112.1(14) . . ? C75 N4 C58 113.0(12) . . ? C76 N4 C58 104.3(12) . . ? N4 C74 H74A 109.5 . . ? N4 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N4 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N4 C75 H75A 109.5 . . ? N4 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N4 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N4 C76 H76A 109.5 . . ? N4 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N4 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C59 C58 N4 126(2) . . ? C59 C58 H58A 105.8 . . ? N4 C58 H58A 105.8 . . ? C59 C58 H58B 105.8 . . ? N4 C58 H58B 105.8 . . ? H58A C58 H58B 106.2 . . ? C58 C59 C60 130(3) . . ? C58 C59 H59A 104.7 . . ? C60 C59 H59A 104.7 . . ? C58 C59 H59B 104.7 . . ? C60 C59 H59B 104.7 . . ? H59A C59 H59B 105.7 . . ? C61 C60 C59 124(3) . . ? C61 C60 H60A 106.3 . . ? C59 C60 H60A 106.3 . . ? C61 C60 H60B 106.3 . . ? C59 C60 H60B 106.3 . . ? H60A C60 H60B 106.4 . . ? C60 C61 C62 122(2) . . ? C60 C61 H61A 106.8 . . ? C62 C61 H61A 106.8 . . ? C60 C61 H61B 106.8 . . ? C62 C61 H61B 106.8 . . ? H61A C61 H61B 106.6 . . ? C63 C62 C61 123(2) . . ? C63 C62 H62A 106.7 . . ? C61 C62 H62A 106.7 . . ? C63 C62 H62B 106.7 . . ? C61 C62 H62B 106.7 . . ? H62A C62 H62B 106.6 . . ? C62 C63 C64 125(2) . . ? C62 C63 H63A 106.1 . . ? C64 C63 H63A 106.1 . . ? C62 C63 H63B 106.1 . . ? C64 C63 H63B 106.1 . . ? H63A C63 H63B 106.3 . . ? C65 C64 C63 127(2) . . ? C65 C64 H64A 105.5 . . ? C63 C64 H64A 105.5 . . ? C65 C64 H64B 105.5 . . ? C63 C64 H64B 105.5 . . ? H64A C64 H64B 106.0 . . ? C66 C65 C64 132(2) . . ? C66 C65 H65A 104.3 . . ? C64 C65 H65A 104.3 . . ? C66 C65 H65B 104.3 . . ? C64 C65 H65B 104.3 . . ? H65A C65 H65B 105.6 . . ? C67 C66 C65 132.2(19) . . ? C67 C66 H66A 104.2 . . ? C65 C66 H66A 104.2 . . ? C67 C66 H66B 104.2 . . ? C65 C66 H66B 104.2 . . ? H66A C66 H66B 105.5 . . ? C68 C67 C66 133(2) . . ? C68 C67 H67A 103.9 . . ? C66 C67 H67A 103.9 . . ? C68 C67 H67B 103.9 . . ? C66 C67 H67B 103.9 . . ? H67A C67 H67B 105.4 . . ? C67 C68 C69 134(2) . . ? C67 C68 H68A 103.7 . . ? C69 C68 H68A 103.7 . . ? C67 C68 H68B 103.7 . . ? C69 C68 H68B 103.7 . . ? H68A C68 H68B 105.3 . . ? C70 C69 C68 135(2) . . ? C70 C69 H69A 103.3 . . ? C68 C69 H69A 103.3 . . ? C70 C69 H69B 103.3 . . ? C68 C69 H69B 103.3 . . ? H69A C69 H69B 105.2 . . ? C69 C70 C71 135(2) . . ? C69 C70 H70A 103.3 . . ? C71 C70 H70A 103.3 . . ? C69 C70 H70B 103.3 . . ? C71 C70 H70B 103.3 . . ? H70A C70 H70B 105.2 . . ? C72 C71 C70 135(3) . . ? C72 C71 H71A 103.5 . . ? C70 C71 H71A 103.5 . . ? C72 C71 H71B 103.5 . . ? C70 C71 H71B 103.5 . . ? H71A C71 H71B 105.3 . . ? C71 C72 C73 132(3) . . ? C71 C72 H72A 104.2 . . ? C73 C72 H72A 104.2 . . ? C71 C72 H72B 104.2 . . ? C73 C72 H72B 104.2 . . ? H72A C72 H72B 105.5 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 N1 C1 C2 59.6(14) . . . . ? C17 N1 C1 C2 -179.3(12) . . . . ? C19 N1 C1 C2 -63.0(14) . . . . ? N1 C1 C2 C3 175.5(12) . . . . ? C1 C2 C3 C4 172.1(14) . . . . ? C2 C3 C4 C5 -174.3(15) . . . . ? C3 C4 C5 C6 179.5(16) . . . . ? C4 C5 C6 C7 179.3(16) . . . . ? C5 C6 C7 C8 177.7(17) . . . . ? C6 C7 C8 C9 -179.1(16) . . . . ? C7 C8 C9 C10 179.6(18) . . . . ? C8 C9 C10 C11 179.0(17) . . . . ? C9 C10 C11 C12 179.9(19) . . . . ? C10 C11 C12 C13 177.4(18) . . . . ? C11 C12 C13 C14 -175.6(19) . . . . ? C12 C13 C14 C152 156(3) . . . . ? C12 C13 C14 C151 -167(2) . . . . ? C13 C14 C151 C161 -172(3) . . . . ? C152 C14 C151 C161 -37(5) . . . . ? C13 C14 C152 C162 80(7) . . . . ? C151 C14 C152 C162 19(4) . . . . ? C38 N2 C20 C21 59.7(15) . . . . ? C37 N2 C20 C21 178.7(12) . . . . ? C36 N2 C20 C21 -58.3(15) . . . . ? N2 C20 C21 C22 179.5(10) . . . . ? C20 C21 C22 C23 -175.9(11) . . . . ? C21 C22 C23 C24 -176.3(12) . . . . ? C22 C23 C24 C25 173.7(13) . . . . ? C23 C24 C25 C26 -173.0(14) . . . . ? C24 C25 C26 C27 174.2(13) . . . . ? C25 C26 C27 C28 -176.8(14) . . . . ? C26 C27 C28 C29 176.9(14) . . . . ? C27 C28 C29 C30 179.3(15) . . . . ? C28 C29 C30 C31 178.4(14) . . . . ? C29 C30 C31 C32 179.3(16) . . . . ? C30 C31 C32 C33 -178.6(15) . . . . ? C31 C32 C33 C34 -178.2(17) . . . . ? C32 C33 C34 C35 179.0(17) . . . . ? C57 N3 C39 C40 40(4) . . . . ? C56 N3 C39 C40 106(3) . . . . ? C57A N3 C39 C40 -45(4) . . . . ? C55 N3 C39 C40 -169(3) . . . . ? C55A N3 C39 C40 -88(3) . . . . ? N3 C39 C40 C41 176(2) . . . . ? C39 C40 C41 C42 164(6) . . . . ? C40 C41 C42 C43 -171(5) . . . . ? C41 C42 C43 C44 178(5) . . . . ? C42 C43 C44 C45 -176(4) . . . . ? C43 C44 C45 C46 -179(4) . . . . ? C44 C45 C46 C47 -176(4) . . . . ? C45 C46 C47 C48 179(4) . . . . ? C46 C47 C48 C49 178(5) . . . . ? C47 C48 C49 C50 178(4) . . . . ? C48 C49 C50 C51 -179(5) . . . . ? C49 C50 C51 C52 -173(7) . . . . ? C50 C51 C52 C53 -175(6) . . . . ? C51 C52 C53 C54 -174(5) . . . . ? C74 N4 C58 C59 -69(3) . . . . ? C75 N4 C58 C59 52(3) . . . . ? C76 N4 C58 C59 172(3) . . . . ? N4 C58 C59 C60 -170(2) . . . . ? C58 C59 C60 C61 -31(5) . . . . ? C59 C60 C61 C62 -175(2) . . . . ? C60 C61 C62 C63 -175(2) . . . . ? C61 C62 C63 C64 177(2) . . . . ? C62 C63 C64 C65 -176(2) . . . . ? C63 C64 C65 C66 -179(2) . . . . ? C64 C65 C66 C67 179(2) . . . . ? C65 C66 C67 C68 -178(2) . . . . ? C66 C67 C68 C69 -179(2) . . . . ? C67 C68 C69 C70 -179(3) . . . . ? C68 C69 C70 C71 177(3) . . . . ? C69 C70 C71 C72 179(3) . . . . ? C70 C71 C72 C73 -178(3) . . . . ? _chemical_name_common Bis(hexadecyltrimethyammonium)tetrabromocuprate(ii) # Attachment 'farra6.cif' data_farra6 _database_code_depnum_ccdc_archive 'CCDC 818357' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetraphenylphosphonium)tetrabromocuprate(II) ; _chemical_melting_point 459-462 _chemical_formula_moiety '2(C24 H20 P), Cu Br4' _chemical_formula_sum 'C48 H40 Br4 Cu P2' _chemical_formula_weight 1061.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.8617(17) _cell_length_b 19.554(2) _cell_length_c 21.072(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.914(12) _cell_angle_gamma 90.00 _cell_volume 4473.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 8317 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 28.95 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 1.1 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 4.165 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.5199 _exptl_absorpt_correction_T_max 0.5282 _exptl_absorpt_process_details 'X-RED (Stoe, 2004)' _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method '\w scan, 1.0 \%' _diffrn_measurement_details ; 180 frames, exposure time per frame = 5 min ; _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 14297 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 3952 _reflns_number_gt 2532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe, 2004)' _computing_cell_refinement 'X-AREA (Stoe, 2004)' _computing_data_reduction 'X-RED (Stoe, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2005) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00048(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3952 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.763 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.083 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5264(4) -0.1590(3) 0.9797(3) 0.0425(13) Uani 1 1 d . . . C2 C -0.6449(4) -0.1332(3) 0.9811(3) 0.0526(15) Uani 1 1 d . . . H2 H -0.6726 -0.1012 0.9514 0.063 Uiso 1 1 calc R . . C3 C -0.7228(5) -0.1567(4) 1.0287(3) 0.070(2) Uani 1 1 d . . . H3 H -0.8023 -0.1394 1.0307 0.084 Uiso 1 1 calc R . . C4 C -0.6828(6) -0.2046(4) 1.0717(3) 0.069(2) Uani 1 1 d . . . H4 H -0.7358 -0.2206 1.1021 0.083 Uiso 1 1 calc R . . C5 C -0.5663(6) -0.2290(3) 1.0704(3) 0.0628(17) Uani 1 1 d . . . H5 H -0.5391 -0.2608 1.1005 0.075 Uiso 1 1 calc R . . C6 C -0.4876(6) -0.2069(3) 1.0246(3) 0.0560(16) Uani 1 1 d . . . H6 H -0.4080 -0.2242 1.0238 0.067 Uiso 1 1 calc R . . C7 C -0.3883(4) -0.1961(3) 0.8671(3) 0.0372(12) Uani 1 1 d . . . C8 C -0.4275(5) -0.2629(3) 0.8749(3) 0.0498(14) Uani 1 1 d . . . H8 H -0.4717 -0.2747 0.9103 0.060 Uiso 1 1 calc R . . C9 C -0.4013(6) -0.3118(3) 0.8304(3) 0.0613(17) Uani 1 1 d . . . H9 H -0.4279 -0.3565 0.8361 0.074 Uiso 1 1 calc R . . C10 C -0.3360(6) -0.2953(3) 0.7776(3) 0.0606(17) Uani 1 1 d . . . H10 H -0.3186 -0.3288 0.7478 0.073 Uiso 1 1 calc R . . C11 C -0.2972(6) -0.2297(3) 0.7693(3) 0.0595(16) Uani 1 1 d . . . H11 H -0.2536 -0.2183 0.7335 0.071 Uiso 1 1 calc R . . C12 C -0.3219(5) -0.1799(3) 0.8134(3) 0.0494(14) Uani 1 1 d . . . H12 H -0.2943 -0.1354 0.8075 0.059 Uiso 1 1 calc R . . C13 C -0.2808(4) -0.1060(3) 0.9671(2) 0.0366(12) Uani 1 1 d . . . C14 C -0.1650(4) -0.1183(3) 0.9431(3) 0.0432(13) Uani 1 1 d . . . H14 H -0.1570 -0.1401 0.9042 0.052 Uiso 1 1 calc R . . C15 C -0.0617(5) -0.0973(3) 0.9784(3) 0.0543(16) Uani 1 1 d . . . H15 H 0.0163 -0.1057 0.9632 0.065 Uiso 1 1 calc R . . C16 C -0.0729(5) -0.0646(3) 1.0349(3) 0.0496(14) Uani 1 1 d . . . H16 H -0.0026 -0.0509 1.0578 0.060 Uiso 1 1 calc R . . C17 C -0.1862(5) -0.0518(3) 1.0583(3) 0.0524(15) Uani 1 1 d . . . H17 H -0.1930 -0.0299 1.0972 0.063 Uiso 1 1 calc R . . C18 C -0.2908(5) -0.0714(3) 1.0239(3) 0.0474(14) Uani 1 1 d . . . H18 H -0.3682 -0.0613 1.0390 0.057 Uiso 1 1 calc R . . C19 C -0.4778(4) -0.0585(3) 0.8798(2) 0.0380(12) Uani 1 1 d . . . C20 C -0.4240(4) 0.0058(3) 0.8850(2) 0.0407(13) Uani 1 1 d . . . H20 H -0.3539 0.0123 0.9109 0.049 Uiso 1 1 calc R . . C21 C -0.4754(5) 0.0600(3) 0.8516(3) 0.0528(15) Uani 1 1 d . . . H21 H -0.4400 0.1032 0.8548 0.063 Uiso 1 1 calc R . . C22 C -0.5796(5) 0.0498(3) 0.8134(3) 0.0554(17) Uani 1 1 d . . . H22 H -0.6151 0.0869 0.7920 0.066 Uiso 1 1 calc R . . C23 C -0.6316(5) -0.0132(4) 0.8064(3) 0.0541(16) Uani 1 1 d . . . H23 H -0.7014 -0.0191 0.7803 0.065 Uiso 1 1 calc R . . C24 C -0.5799(5) -0.0677(3) 0.8383(3) 0.0503(14) Uani 1 1 d . . . H24 H -0.6129 -0.1112 0.8323 0.060 Uiso 1 1 calc R . . Br1 Br 0.11576(5) 0.03058(3) 0.68504(3) 0.04515(18) Uani 1 1 d . . . Br2 Br -0.08907(6) -0.11973(4) 0.67278(4) 0.0668(2) Uani 1 1 d . . . Cu1 Cu 0.0000 -0.04347(5) 0.7500 0.0387(2) Uani 1 2 d S . . P1 P -0.41754(11) -0.13016(7) 0.92285(7) 0.0363(3) Uani 1 1 d . . . 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 C1 0.038(3) 0.040(3) 0.049(3) 0.001(3) 0.002(2) -0.005(2) C2 0.040(3) 0.065(4) 0.053(4) -0.005(3) -0.006(2) -0.003(3) C3 0.043(3) 0.100(6) 0.068(5) -0.004(5) 0.009(3) -0.017(3) C4 0.080(5) 0.077(5) 0.051(4) 0.001(4) 0.013(3) -0.034(4) C5 0.079(4) 0.049(4) 0.061(5) 0.011(4) 0.012(3) -0.009(3) C6 0.065(4) 0.047(4) 0.057(4) 0.006(3) 0.005(3) 0.006(3) C7 0.043(3) 0.031(3) 0.037(3) -0.001(3) -0.007(2) -0.003(2) C8 0.055(3) 0.040(3) 0.055(4) 0.001(3) -0.003(3) -0.009(3) C9 0.075(4) 0.035(3) 0.072(5) -0.003(4) -0.015(3) -0.014(3) C10 0.078(4) 0.052(4) 0.051(4) -0.011(4) -0.007(3) 0.007(3) C11 0.085(4) 0.048(4) 0.046(4) -0.003(3) 0.007(3) -0.004(3) C12 0.070(4) 0.036(3) 0.043(4) -0.002(3) 0.005(3) -0.008(3) C13 0.042(3) 0.034(3) 0.034(3) 0.004(3) 0.000(2) 0.002(2) C14 0.043(3) 0.050(4) 0.036(3) -0.003(3) 0.001(2) 0.005(2) C15 0.035(3) 0.080(5) 0.048(4) -0.009(4) -0.003(2) 0.001(3) C16 0.051(3) 0.058(4) 0.039(3) -0.001(3) -0.010(2) -0.006(3) C17 0.055(3) 0.066(4) 0.036(3) -0.012(3) -0.001(2) 0.004(3) C18 0.040(3) 0.060(4) 0.042(3) -0.005(3) 0.003(2) 0.008(2) C19 0.040(3) 0.037(3) 0.037(3) 0.004(3) 0.000(2) 0.003(2) C20 0.046(3) 0.044(3) 0.032(3) 0.004(3) 0.003(2) 0.000(2) C21 0.074(4) 0.033(3) 0.052(4) 0.007(3) 0.013(3) 0.007(3) C22 0.064(4) 0.064(4) 0.040(3) 0.017(3) 0.013(3) 0.030(3) C23 0.044(3) 0.073(5) 0.045(4) 0.006(3) -0.008(2) 0.009(3) C24 0.049(3) 0.054(4) 0.047(4) 0.008(3) -0.008(3) -0.004(3) Br1 0.0483(3) 0.0480(3) 0.0390(3) 0.0092(3) -0.0011(2) -0.0037(2) Br2 0.0696(4) 0.0646(5) 0.0674(5) -0.0302(4) 0.0202(3) -0.0226(3) Cu1 0.0400(4) 0.0380(6) 0.0382(5) 0.000 0.0040(4) 0.000 P1 0.0371(6) 0.0334(8) 0.0382(8) 0.0021(7) -0.0022(5) -0.0009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.383(7) . ? C1 C6 1.387(8) . ? C1 P1 1.801(5) . ? C2 C3 1.409(8) . ? C2 H2 0.9300 . ? C3 C4 1.364(10) . ? C3 H3 0.9300 . ? C4 C5 1.353(9) . ? C4 H4 0.9300 . ? C5 C6 1.380(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.386(7) . ? C7 C12 1.397(7) . ? C7 P1 1.780(5) . ? C8 C9 1.373(8) . ? C8 H8 0.9300 . ? C9 C10 1.379(9) . ? C9 H9 0.9300 . ? C10 C11 1.365(9) . ? C10 H10 0.9300 . ? C11 C12 1.379(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.383(7) . ? C13 C14 1.393(7) . ? C13 P1 1.790(5) . ? C14 C15 1.387(7) . ? C14 H14 0.9300 . ? C15 C16 1.361(8) . ? C15 H15 0.9300 . ? C16 C17 1.364(7) . ? C16 H16 0.9300 . ? C17 C18 1.382(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.389(7) . ? C19 C24 1.401(7) . ? C19 P1 1.783(5) . ? C20 C21 1.380(7) . ? C20 H20 0.9300 . ? C21 C22 1.381(8) . ? C21 H21 0.9300 . ? C22 C23 1.361(9) . ? C22 H22 0.9300 . ? C23 C24 1.370(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? Br1 Cu1 2.3805(8) . ? Br2 Cu1 2.3880(9) . ? Cu1 Br1 2.3805(8) 2_556 ? Cu1 Br2 2.3880(9) 2_556 ? 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 C2 C1 C6 119.5(5) . . ? C2 C1 P1 122.2(5) . . ? C6 C1 P1 118.3(4) . . ? C1 C2 C3 118.6(6) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 120.7(6) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.4(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.5(6) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 118.6(5) . . ? C8 C7 P1 122.8(4) . . ? C12 C7 P1 118.6(4) . . ? C9 C8 C7 120.2(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.8(6) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.2(5) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C18 C13 C14 119.8(5) . . ? C18 C13 P1 119.5(4) . . ? C14 C13 P1 120.6(4) . . ? C15 C14 C13 118.6(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 120.9(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.8(5) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 119.7(5) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C13 120.2(5) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C20 C19 C24 119.3(5) . . ? C20 C19 P1 121.6(4) . . ? C24 C19 P1 119.1(4) . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 119.8(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 121.5(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C19 120.6(6) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? Br1 Cu1 Br1 105.07(5) 2_556 . ? Br1 Cu1 Br2 124.19(2) 2_556 . ? Br1 Cu1 Br2 101.41(2) . . ? Br1 Cu1 Br2 101.41(2) 2_556 2_556 ? Br1 Cu1 Br2 124.19(2) . 2_556 ? Br2 Cu1 Br2 102.71(5) . 2_556 ? C7 P1 C19 107.7(2) . . ? C7 P1 C13 111.8(2) . . ? C19 P1 C13 110.0(2) . . ? C7 P1 C1 110.4(2) . . ? C19 P1 C1 110.3(2) . . ? C13 P1 C1 106.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.1(9) . . . . ? P1 C1 C2 C3 -177.7(5) . . . . ? C1 C2 C3 C4 -1.0(10) . . . . ? C2 C3 C4 C5 1.7(11) . . . . ? C3 C4 C5 C6 -1.5(11) . . . . ? C4 C5 C6 C1 0.6(10) . . . . ? C2 C1 C6 C5 0.1(9) . . . . ? P1 C1 C6 C5 178.0(5) . . . . ? C12 C7 C8 C9 -0.1(8) . . . . ? P1 C7 C8 C9 -179.5(4) . . . . ? C7 C8 C9 C10 -0.1(9) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? C9 C10 C11 C12 0.4(10) . . . . ? C10 C11 C12 C7 -0.6(9) . . . . ? C8 C7 C12 C11 0.4(8) . . . . ? P1 C7 C12 C11 179.9(5) . . . . ? C18 C13 C14 C15 2.3(8) . . . . ? P1 C13 C14 C15 178.5(4) . . . . ? C13 C14 C15 C16 -0.8(9) . . . . ? C14 C15 C16 C17 0.1(10) . . . . ? C15 C16 C17 C18 -0.8(10) . . . . ? C16 C17 C18 C13 2.3(9) . . . . ? C14 C13 C18 C17 -3.1(9) . . . . ? P1 C13 C18 C17 -179.3(5) . . . . ? C24 C19 C20 C21 3.0(8) . . . . ? P1 C19 C20 C21 -178.8(4) . . . . ? C19 C20 C21 C22 0.1(8) . . . . ? C20 C21 C22 C23 -1.9(9) . . . . ? C21 C22 C23 C24 0.5(9) . . . . ? C22 C23 C24 C19 2.7(9) . . . . ? C20 C19 C24 C23 -4.4(8) . . . . ? P1 C19 C24 C23 177.3(4) . . . . ? C8 C7 P1 C19 -131.3(5) . . . . ? C12 C7 P1 C19 49.3(5) . . . . ? C8 C7 P1 C13 107.8(5) . . . . ? C12 C7 P1 C13 -71.6(5) . . . . ? C8 C7 P1 C1 -10.8(5) . . . . ? C12 C7 P1 C1 169.8(4) . . . . ? C20 C19 P1 C7 -124.9(4) . . . . ? C24 C19 P1 C7 53.3(5) . . . . ? C20 C19 P1 C13 -2.9(5) . . . . ? C24 C19 P1 C13 175.3(4) . . . . ? C20 C19 P1 C1 114.5(5) . . . . ? C24 C19 P1 C1 -67.3(5) . . . . ? C18 C13 P1 C7 -161.0(4) . . . . ? C14 C13 P1 C7 22.7(5) . . . . ? C18 C13 P1 C19 79.4(5) . . . . ? C14 C13 P1 C19 -96.9(5) . . . . ? C18 C13 P1 C1 -40.2(5) . . . . ? C14 C13 P1 C1 143.5(4) . . . . ? C2 C1 P1 C7 -110.6(5) . . . . ? C6 C1 P1 C7 71.6(5) . . . . ? C2 C1 P1 C19 8.3(6) . . . . ? C6 C1 P1 C19 -169.5(4) . . . . ? C2 C1 P1 C13 127.7(5) . . . . ? C6 C1 P1 C13 -50.1(5) . . . . ? # Attachment 'farra7.cif' data_farra7 _database_code_depnum_ccdc_archive 'CCDC 818358' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(methyltriphenylphosphonium)tetrabromocuprate(II) ; _chemical_melting_point 402 _chemical_formula_moiety '2(C19 H18 P), Cu Br4' _chemical_formula_sum 'C38 H36 Br4 Cu P2' _chemical_formula_weight 937.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.9966(11) _cell_length_b 24.702(3) _cell_length_c 17.481(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.553(10) _cell_angle_gamma 90.00 _cell_volume 3806.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 11533 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.74 _exptl_crystal_description needle _exptl_crystal_colour violet _exptl_crystal_size_max 0.95 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 4.883 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.2275 _exptl_absorpt_correction_T_max 0.2490 _exptl_absorpt_process_details 'X-RED (Stoe, 2004)' _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method '\w scan, 1.0 \%' _diffrn_measurement_details ; 180 frames, exposure time per frame = 5 min ; _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 12264 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 6424 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe, 2004)' _computing_cell_refinement 'X-AREA (Stoe, 2004)' _computing_data_reduction 'X-RED (Stoe, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2005) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00056(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(14) _refine_ls_number_reflns 6424 _refine_ls_number_parameters 407 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.862 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.096 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5293(11) 0.1532(4) -0.1689(6) 0.049(2) Uani 1 1 d . . . C2 C -0.5986(14) 0.1027(5) -0.1895(8) 0.072(3) Uani 1 1 d . . . H2 H -0.6480 0.0846 -0.1551 0.086 Uiso 1 1 calc R . . C3 C -0.5924(18) 0.0807(6) -0.2606(10) 0.093(5) Uani 1 1 d . . . H3 H -0.6418 0.0482 -0.2756 0.111 Uiso 1 1 calc R . . C4 C -0.5146(19) 0.1060(6) -0.3093(9) 0.091(5) Uani 1 1 d . . . H4 H -0.5085 0.0895 -0.3563 0.110 Uiso 1 1 calc R . . C5 C -0.4456(15) 0.1543(6) -0.2918(6) 0.073(3) Uani 1 1 d . . . H5 H -0.3927 0.1704 -0.3264 0.088 Uiso 1 1 calc R . . C6 C -0.4542(12) 0.1802(5) -0.2208(6) 0.057(3) Uani 1 1 d . . . H6 H -0.4113 0.2142 -0.2087 0.068 Uiso 1 1 calc R . . C7 C -0.4438(11) 0.2441(4) -0.0588(5) 0.042(2) Uani 1 1 d . . . C8 C -0.3313(10) 0.2455(4) 0.0091(5) 0.049(2) Uani 1 1 d . . . H8 H -0.3158 0.2153 0.0415 0.059 Uiso 1 1 calc R . . C9 C -0.2445(12) 0.2901(5) 0.0285(6) 0.056(3) Uani 1 1 d . . . H9 H -0.1708 0.2906 0.0741 0.068 Uiso 1 1 calc R . . C10 C -0.2659(13) 0.3354(5) -0.0202(6) 0.061(3) Uani 1 1 d . . . H10 H -0.2055 0.3660 -0.0076 0.073 Uiso 1 1 calc R . . C11 C -0.3762(13) 0.3347(4) -0.0864(6) 0.054(2) Uani 1 1 d . . . H11 H -0.3905 0.3649 -0.1187 0.065 Uiso 1 1 calc R . . C12 C -0.4665(11) 0.2897(4) -0.1061(5) 0.045(2) Uani 1 1 d . . . H12 H -0.5423 0.2899 -0.1509 0.054 Uiso 1 1 calc R . . C13 C -0.7586(10) 0.2037(3) -0.1020(5) 0.0395(18) Uani 1 1 d . . . C14 C -0.8229(11) 0.2210(4) -0.1758(5) 0.051(2) Uani 1 1 d . . . H14 H -0.7653 0.2233 -0.2143 0.061 Uiso 1 1 calc R . . C15 C -0.9736(12) 0.2349(5) -0.1919(8) 0.068(3) Uani 1 1 d . . . H15 H -1.0191 0.2468 -0.2415 0.082 Uiso 1 1 calc R . . C16 C -1.0587(13) 0.2311(5) -0.1328(9) 0.079(4) Uani 1 1 d . . . H16 H -1.1608 0.2405 -0.1434 0.095 Uiso 1 1 calc R . . C17 C -0.9927(16) 0.2138(6) -0.0608(10) 0.090(4) Uani 1 1 d . . . H17 H -1.0498 0.2112 -0.0221 0.108 Uiso 1 1 calc R . . C18 C -0.8419(14) 0.2000(5) -0.0443(7) 0.066(3) Uani 1 1 d . . . H18 H -0.7964 0.1883 0.0055 0.079 Uiso 1 1 calc R . . C19 C -0.5261(16) 0.1406(5) -0.0006(7) 0.069(3) Uani 1 1 d . . . H19C H -0.4209 0.1305 0.0109 0.104 Uiso 1 1 calc R . . H19B H -0.5874 0.1087 -0.0130 0.104 Uiso 1 1 calc R . . H19A H -0.5517 0.1580 0.0442 0.104 Uiso 1 1 calc R . . C20 C 0.4839(11) 0.0388(4) 0.4343(5) 0.046(2) Uani 1 1 d . . . C21 C 0.3359(12) 0.0342(5) 0.3910(5) 0.055(3) Uani 1 1 d . . . H21 H 0.3123 0.0487 0.3409 0.066 Uiso 1 1 calc R . . C22 C 0.2242(12) 0.0085(5) 0.4214(6) 0.055(2) Uani 1 1 d . . . H22 H 0.1276 0.0040 0.3910 0.066 Uiso 1 1 calc R . . C23 C 0.2570(12) -0.0102(4) 0.4970(6) 0.054(2) Uani 1 1 d . . . H23 H 0.1807 -0.0256 0.5187 0.065 Uiso 1 1 calc R . . C24 C 0.4017(13) -0.0064(4) 0.5406(5) 0.052(2) Uani 1 1 d . . . H24 H 0.4232 -0.0206 0.5909 0.062 Uiso 1 1 calc R . . C25 C 0.5178(11) 0.0188(4) 0.5101(5) 0.045(2) Uani 1 1 d . . . H25 H 0.6152 0.0219 0.5401 0.055 Uiso 1 1 calc R . . C26 C 0.7119(11) 0.0230(4) 0.3384(5) 0.043(2) Uani 1 1 d . . . C27 C 0.7385(11) -0.0279(4) 0.3664(5) 0.047(2) Uani 1 1 d . . . H27 H 0.7047 -0.0380 0.4112 0.056 Uiso 1 1 calc R . . C28 C 0.8158(13) -0.0655(4) 0.3291(5) 0.052(2) Uani 1 1 d . . . H28 H 0.8350 -0.1001 0.3494 0.063 Uiso 1 1 calc R . . C29 C 0.8627(15) -0.0506(5) 0.2626(6) 0.069(3) Uani 1 1 d . . . H29 H 0.9139 -0.0755 0.2374 0.083 Uiso 1 1 calc R . . C30 C 0.8350(18) 0.0008(6) 0.2323(7) 0.084(4) Uani 1 1 d . . . H30 H 0.8678 0.0104 0.1870 0.101 Uiso 1 1 calc R . . C31 C 0.7591(15) 0.0380(5) 0.2690(6) 0.071(3) Uani 1 1 d . . . H31 H 0.7392 0.0725 0.2483 0.086 Uiso 1 1 calc R . . C32 C 0.7640(10) 0.0986(4) 0.4690(5) 0.042(2) Uani 1 1 d . . . C33 C 0.8873(12) 0.0675(4) 0.5075(5) 0.052(2) Uani 1 1 d . . . H33 H 0.9021 0.0330 0.4890 0.062 Uiso 1 1 calc R . . C34 C 0.9860(14) 0.0867(5) 0.5717(6) 0.064(3) Uani 1 1 d . . . H34 H 1.0651 0.0652 0.5977 0.076 Uiso 1 1 calc R . . C35 C 0.9656(16) 0.1381(5) 0.5965(6) 0.069(3) Uani 1 1 d . . . H35 H 1.0341 0.1517 0.6391 0.083 Uiso 1 1 calc R . . C36 C 0.8483(18) 0.1700(5) 0.5610(7) 0.074(4) Uani 1 1 d . . . H36 H 0.8372 0.2046 0.5800 0.088 Uiso 1 1 calc R . . C37 C 0.7459(14) 0.1512(5) 0.4969(7) 0.061(3) Uani 1 1 d . . . H37 H 0.6660 0.1729 0.4725 0.074 Uiso 1 1 calc R . . C38 C 0.5402(15) 0.1238(5) 0.3269(7) 0.068(3) Uani 1 1 d . . . H38A H 0.6160 0.1411 0.3037 0.102 Uiso 1 1 calc R . . H38B H 0.4951 0.1501 0.3558 0.102 Uiso 1 1 calc R . . H38C H 0.4634 0.1085 0.2866 0.102 Uiso 1 1 calc R . . Br1 Br -0.17711(10) 0.17837(4) 0.19588(5) 0.0505(3) Uani 1 1 d . . . Br2 Br -0.12267(12) 0.08979(5) 0.04295(6) 0.0623(3) Uani 1 1 d . . . Br3 Br 0.19915(14) 0.06079(6) 0.18584(6) 0.0770(4) Uani 1 1 d . . . Br4 Br 0.20711(16) 0.20513(6) 0.17316(7) 0.0823(4) Uani 1 1 d . . . Cu1 Cu 0.02659(11) 0.13437(4) 0.15098(5) 0.0407(3) Uani 1 1 d . . . P1 P -0.5605(3) 0.18597(9) -0.08176(13) 0.0411(5) Uani 1 1 d . . . P2 P 0.6259(3) 0.07146(10) 0.39123(13) 0.0452(6) Uani 1 1 d . . . 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 C1 0.034(5) 0.043(5) 0.069(5) -0.016(4) 0.008(4) 0.010(4) C2 0.057(8) 0.042(6) 0.111(9) -0.014(6) 0.005(6) 0.001(5) C3 0.068(9) 0.058(8) 0.140(13) -0.045(9) -0.006(9) 0.007(7) C4 0.093(11) 0.084(11) 0.087(8) -0.048(8) -0.005(8) 0.013(9) C5 0.069(8) 0.096(10) 0.054(6) -0.024(6) 0.011(5) 0.011(7) C6 0.046(6) 0.057(6) 0.066(6) -0.012(5) 0.009(5) 0.002(5) C7 0.041(5) 0.045(5) 0.043(4) -0.006(3) 0.019(4) -0.003(4) C8 0.035(5) 0.063(6) 0.046(4) -0.006(4) 0.003(4) -0.004(5) C9 0.043(6) 0.071(7) 0.054(5) -0.017(5) 0.007(4) -0.013(5) C10 0.055(7) 0.063(7) 0.063(6) -0.018(5) 0.011(5) -0.016(6) C11 0.061(7) 0.043(6) 0.064(6) 0.001(4) 0.024(5) -0.005(5) C12 0.046(6) 0.041(5) 0.048(4) -0.004(4) 0.012(4) 0.001(4) C13 0.029(4) 0.035(5) 0.056(4) 0.001(4) 0.011(4) -0.001(4) C14 0.040(6) 0.051(6) 0.061(5) 0.006(4) 0.006(4) 0.009(5) C15 0.034(6) 0.051(7) 0.105(8) -0.005(6) -0.019(5) 0.016(5) C16 0.031(6) 0.056(7) 0.151(13) -0.015(8) 0.020(7) 0.005(5) C17 0.053(8) 0.091(10) 0.139(13) 0.017(9) 0.050(8) 0.011(7) C18 0.055(7) 0.071(8) 0.078(7) 0.008(5) 0.028(6) 0.002(6) C19 0.080(9) 0.050(6) 0.073(6) 0.021(5) 0.006(6) 0.003(6) C20 0.052(6) 0.050(5) 0.040(4) 0.001(4) 0.020(4) -0.007(4) C21 0.054(6) 0.065(7) 0.052(5) 0.001(4) 0.023(5) 0.003(5) C22 0.036(5) 0.064(7) 0.068(6) -0.012(5) 0.018(4) -0.006(5) C23 0.049(6) 0.054(6) 0.065(6) -0.010(5) 0.028(5) -0.003(5) C24 0.072(8) 0.038(5) 0.050(4) -0.003(4) 0.024(5) -0.004(5) C25 0.039(5) 0.052(6) 0.047(4) -0.004(4) 0.011(4) -0.005(4) C26 0.054(6) 0.036(5) 0.042(4) 0.013(3) 0.017(4) -0.002(4) C27 0.054(6) 0.055(6) 0.036(4) 0.003(4) 0.020(4) 0.001(5) C28 0.063(7) 0.047(6) 0.050(5) -0.008(4) 0.017(4) 0.002(5) C29 0.080(9) 0.075(8) 0.059(6) -0.025(6) 0.029(5) -0.012(7) C30 0.126(12) 0.079(9) 0.068(6) -0.001(6) 0.071(8) -0.019(8) C31 0.095(9) 0.079(8) 0.049(5) 0.012(5) 0.036(6) -0.014(7) C32 0.040(5) 0.040(5) 0.050(4) -0.004(4) 0.017(4) -0.008(4) C33 0.055(6) 0.054(6) 0.050(5) -0.015(4) 0.020(4) -0.008(5) C34 0.066(7) 0.071(8) 0.053(5) -0.012(5) 0.011(5) -0.015(6) C35 0.083(9) 0.076(8) 0.056(5) -0.023(6) 0.033(6) -0.036(7) C36 0.098(11) 0.050(7) 0.087(8) -0.031(6) 0.051(8) -0.022(7) C37 0.065(7) 0.048(6) 0.079(6) -0.010(5) 0.034(6) 0.001(5) C38 0.074(8) 0.056(7) 0.078(7) 0.014(5) 0.023(6) -0.001(6) Br1 0.0552(6) 0.0532(5) 0.0443(4) -0.0025(4) 0.0125(4) 0.0091(5) Br2 0.0620(7) 0.0625(7) 0.0546(5) -0.0214(5) -0.0070(4) 0.0001(5) Br3 0.0723(8) 0.0964(10) 0.0590(6) -0.0006(6) 0.0052(5) 0.0395(7) Br4 0.0789(9) 0.0933(10) 0.0763(7) -0.0257(6) 0.0192(6) -0.0452(8) Cu1 0.0388(6) 0.0492(6) 0.0323(4) -0.0042(4) 0.0030(4) -0.0026(5) P1 0.0351(12) 0.0360(12) 0.0519(11) 0.0069(9) 0.0080(9) 0.0031(10) P2 0.0481(15) 0.0401(13) 0.0507(11) 0.0068(10) 0.0182(10) 0.0009(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.402(15) . ? C1 C2 1.408(15) . ? C1 P1 1.797(9) . ? C2 C3 1.37(2) . ? C2 H2 0.9300 . ? C3 C4 1.36(2) . ? C3 H3 0.9300 . ? C4 C5 1.35(2) . ? C4 H4 0.9300 . ? C5 C6 1.413(14) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.389(13) . ? C7 C8 1.397(13) . ? C7 P1 1.776(9) . ? C8 C9 1.354(14) . ? C8 H8 0.9300 . ? C9 C10 1.395(16) . ? C9 H9 0.9300 . ? C10 C11 1.365(16) . ? C10 H10 0.9300 . ? C11 C12 1.379(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.371(13) . ? C13 C18 1.376(13) . ? C13 P1 1.800(9) . ? C14 C15 1.372(14) . ? C14 H14 0.9300 . ? C15 C16 1.407(18) . ? C15 H15 0.9300 . ? C16 C17 1.35(2) . ? C16 H16 0.9300 . ? C17 C18 1.373(18) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 P1 1.787(10) . ? C19 H19C 0.9600 . ? C19 H19B 0.9600 . ? C19 H19A 0.9600 . ? C20 C25 1.389(12) . ? C20 C21 1.398(14) . ? C20 P2 1.800(9) . ? C21 C22 1.381(14) . ? C21 H21 0.9300 . ? C22 C23 1.375(14) . ? C22 H22 0.9300 . ? C23 C24 1.374(15) . ? C23 H23 0.9300 . ? C24 C25 1.408(14) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.353(13) . ? C26 C31 1.413(12) . ? C26 P2 1.780(10) . ? C27 C28 1.397(13) . ? C27 H27 0.9300 . ? C28 C29 1.363(14) . ? C28 H28 0.9300 . ? C29 C30 1.380(18) . ? C29 H29 0.9300 . ? C30 C31 1.377(18) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.406(14) . ? C32 C37 1.408(14) . ? C32 P2 1.778(9) . ? C33 C34 1.368(15) . ? C33 H33 0.9300 . ? C34 C35 1.366(17) . ? C34 H34 0.9300 . ? C35 C36 1.36(2) . ? C35 H35 0.9300 . ? C36 C37 1.380(18) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 P2 1.785(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? Br1 Cu1 2.3941(14) . ? Br2 Cu1 2.3593(13) . ? Br3 Cu1 2.3887(16) . ? Br4 Cu1 2.3644(16) . ? 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 C6 C1 C2 120.2(10) . . ? C6 C1 P1 120.8(8) . . ? C2 C1 P1 118.6(9) . . ? C3 C2 C1 119.2(13) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 120.4(13) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 122.5(12) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 119.6(13) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 118.1(11) . . ? C1 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C12 C7 C8 118.7(9) . . ? C12 C7 P1 120.7(7) . . ? C8 C7 P1 120.5(8) . . ? C9 C8 C7 121.1(10) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.9(10) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.6(10) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.0(10) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 119.7(9) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 121.4(10) . . ? C14 C13 P1 118.4(7) . . ? C18 C13 P1 120.2(8) . . ? C13 C14 C15 119.0(10) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 119.5(11) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.3(11) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.5(12) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.3(12) . . ? C17 C18 H18 120.3 . . ? C13 C18 H18 120.3 . . ? P1 C19 H19C 109.5 . . ? P1 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? P1 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? C25 C20 C21 119.4(8) . . ? C25 C20 P2 121.3(7) . . ? C21 C20 P2 119.2(7) . . ? C22 C21 C20 121.0(9) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 119.4(10) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 120.5(9) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.9(9) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C20 C25 C24 118.6(9) . . ? C20 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C31 119.5(9) . . ? C27 C26 P2 120.0(6) . . ? C31 C26 P2 120.4(8) . . ? C26 C27 C28 121.2(8) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 119.1(10) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C28 C29 C30 120.8(10) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.2(9) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C26 119.2(11) . . ? C30 C31 H31 120.4 . . ? C26 C31 H31 120.4 . . ? C33 C32 C37 118.2(9) . . ? C33 C32 P2 121.6(7) . . ? C37 C32 P2 120.1(8) . . ? C34 C33 C32 121.6(10) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C33 118.5(12) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C36 C35 C34 122.2(11) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C35 C36 C37 120.3(11) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 119.2(12) . . ? C36 C37 H37 120.4 . . ? C32 C37 H37 120.4 . . ? P2 C38 H38A 109.5 . . ? P2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Br2 Cu1 Br4 137.59(6) . . ? Br2 Cu1 Br3 94.91(6) . . ? Br4 Cu1 Br3 97.51(7) . . ? Br2 Cu1 Br1 97.12(5) . . ? Br4 Cu1 Br1 99.00(6) . . ? Br3 Cu1 Br1 139.71(6) . . ? C7 P1 C19 109.1(5) . . ? C7 P1 C1 111.7(4) . . ? C19 P1 C1 111.1(6) . . ? C7 P1 C13 111.4(4) . . ? C19 P1 C13 108.4(5) . . ? C1 P1 C13 105.0(4) . . ? C32 P2 C26 109.9(4) . . ? C32 P2 C38 110.8(5) . . ? C26 P2 C38 109.8(5) . . ? C32 P2 C20 107.2(4) . . ? C26 P2 C20 109.5(4) . . ? C38 P2 C20 109.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.4(17) . . . . ? P1 C1 C2 C3 171.5(10) . . . . ? C1 C2 C3 C4 3(2) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C2 C1 C6 C5 -2.4(16) . . . . ? P1 C1 C6 C5 -174.2(8) . . . . ? C4 C5 C6 C1 2.8(18) . . . . ? C12 C7 C8 C9 -0.6(14) . . . . ? P1 C7 C8 C9 -178.1(7) . . . . ? C7 C8 C9 C10 -0.7(15) . . . . ? C8 C9 C10 C11 1.1(16) . . . . ? C9 C10 C11 C12 -0.2(16) . . . . ? C10 C11 C12 C7 -1.1(15) . . . . ? C8 C7 C12 C11 1.5(13) . . . . ? P1 C7 C12 C11 178.9(7) . . . . ? C18 C13 C14 C15 0.0(16) . . . . ? P1 C13 C14 C15 -179.6(8) . . . . ? C13 C14 C15 C16 -0.1(16) . . . . ? C14 C15 C16 C17 0.0(19) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C16 C17 C18 C13 0(2) . . . . ? C14 C13 C18 C17 0.3(18) . . . . ? P1 C13 C18 C17 179.9(10) . . . . ? C25 C20 C21 C22 -2.2(15) . . . . ? P2 C20 C21 C22 178.8(8) . . . . ? C20 C21 C22 C23 3.6(16) . . . . ? C21 C22 C23 C24 -3.8(16) . . . . ? C22 C23 C24 C25 2.7(15) . . . . ? C21 C20 C25 C24 1.0(14) . . . . ? P2 C20 C25 C24 179.9(7) . . . . ? C23 C24 C25 C20 -1.2(14) . . . . ? C31 C26 C27 C28 1.9(16) . . . . ? P2 C26 C27 C28 -175.2(8) . . . . ? C26 C27 C28 C29 -1.2(16) . . . . ? C27 C28 C29 C30 0.2(18) . . . . ? C28 C29 C30 C31 0(2) . . . . ? C29 C30 C31 C26 1(2) . . . . ? C27 C26 C31 C30 -1.7(18) . . . . ? P2 C26 C31 C30 175.4(10) . . . . ? C37 C32 C33 C34 1.5(14) . . . . ? P2 C32 C33 C34 -174.2(8) . . . . ? C32 C33 C34 C35 -2.2(15) . . . . ? C33 C34 C35 C36 1.9(17) . . . . ? C34 C35 C36 C37 -0.9(17) . . . . ? C35 C36 C37 C32 0.2(16) . . . . ? C33 C32 C37 C36 -0.5(14) . . . . ? P2 C32 C37 C36 175.3(8) . . . . ? C12 C7 P1 C19 -168.9(8) . . . . ? C8 C7 P1 C19 8.5(9) . . . . ? C12 C7 P1 C1 67.9(8) . . . . ? C8 C7 P1 C1 -114.7(8) . . . . ? C12 C7 P1 C13 -49.2(8) . . . . ? C8 C7 P1 C13 128.2(8) . . . . ? C6 C1 P1 C7 -16.2(10) . . . . ? C2 C1 P1 C7 171.9(8) . . . . ? C6 C1 P1 C19 -138.3(9) . . . . ? C2 C1 P1 C19 49.9(10) . . . . ? C6 C1 P1 C13 104.7(8) . . . . ? C2 C1 P1 C13 -67.2(9) . . . . ? C14 C13 P1 C7 83.4(8) . . . . ? C18 C13 P1 C7 -96.2(9) . . . . ? C14 C13 P1 C19 -156.5(8) . . . . ? C18 C13 P1 C19 23.8(10) . . . . ? C14 C13 P1 C1 -37.7(9) . . . . ? C18 C13 P1 C1 142.6(9) . . . . ? C33 C32 P2 C26 -31.9(8) . . . . ? C37 C32 P2 C26 152.5(7) . . . . ? C33 C32 P2 C38 -153.5(7) . . . . ? C37 C32 P2 C38 31.0(9) . . . . ? C33 C32 P2 C20 87.0(8) . . . . ? C37 C32 P2 C20 -88.6(8) . . . . ? C27 C26 P2 C32 80.0(9) . . . . ? C31 C26 P2 C32 -97.2(10) . . . . ? C27 C26 P2 C38 -157.9(9) . . . . ? C31 C26 P2 C38 25.0(11) . . . . ? C27 C26 P2 C20 -37.5(10) . . . . ? C31 C26 P2 C20 145.4(9) . . . . ? C25 C20 P2 C32 -25.8(9) . . . . ? C21 C20 P2 C32 153.1(8) . . . . ? C25 C20 P2 C26 93.3(8) . . . . ? C21 C20 P2 C26 -87.7(9) . . . . ? C25 C20 P2 C38 -146.2(8) . . . . ? C21 C20 P2 C38 32.8(10) . . . . ? # Attachment 'thiel2.cif' data_thiel2 _database_code_depnum_ccdc_archive 'CCDC 818359' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(benzyltriphenylphosphonium)tetrabromocuprate(II) chloroform solvate ; _chemical_melting_point 414-415 _chemical_formula_moiety '2(C25 H22 P), Cu Br4, 2(C H Cl3)' _chemical_formula_sum 'C52 H46 Br4 Cl6 Cu P2' _chemical_formula_weight 1328.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6843(11) _cell_length_b 10.2238(6) _cell_length_c 28.5236(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.612(5) _cell_angle_gamma 90.00 _cell_volume 5446.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 24443 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 27.13 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 3.723 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.2976 _exptl_absorpt_correction_T_max 0.3129 _exptl_absorpt_process_details 'X-RED (Stoe, 2004)' _exptl_special_details ; The crystal was embedded in perfluoropolyalkylether oil. ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method '\w scan, 1.0 \%' _diffrn_measurement_details ; 180 frames, exposure time per frame = 3 min ; _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_reflns_number 34342 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 9574 _reflns_number_gt 6886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe, 2004)' _computing_cell_refinement 'X-AREA (Stoe, 2004)' _computing_data_reduction 'X-RED (Stoe, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2005) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00077(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9574 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.519 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.067 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.51638(18) 1.3840(4) 0.18272(12) 0.0366(8) Uani 1 1 d . . . H1A H 0.5329 1.3371 0.2105 0.044 Uiso 1 1 calc R . . H1B H 0.5583 1.4178 0.1674 0.044 Uiso 1 1 calc R . . C2 C 0.47110(17) 1.4981(4) 0.19774(12) 0.0336(8) Uani 1 1 d . . . C3 C 0.42897(19) 1.4897(4) 0.23708(12) 0.0441(9) Uani 1 1 d . . . H3 H 0.4287 1.4133 0.2548 0.053 Uiso 1 1 calc R . . C4 C 0.3871(2) 1.5961(5) 0.24988(14) 0.0511(11) Uani 1 1 d . . . H4 H 0.3593 1.5905 0.2764 0.061 Uiso 1 1 calc R . . C5 C 0.3865(2) 1.7074(4) 0.22415(15) 0.0528(11) Uani 1 1 d . . . H5 H 0.3576 1.7772 0.2325 0.063 Uiso 1 1 calc R . . C6 C 0.4285(2) 1.7170(4) 0.18569(15) 0.0549(11) Uani 1 1 d . . . H6 H 0.4285 1.7937 0.1681 0.066 Uiso 1 1 calc R . . C7 C 0.4711(2) 1.6127(4) 0.17299(14) 0.0471(10) Uani 1 1 d . . . H7 H 0.5001 1.6206 0.1472 0.057 Uiso 1 1 calc R . . C8 C 0.43962(17) 1.3474(4) 0.09089(11) 0.0337(8) Uani 1 1 d . . . C9 C 0.4677(2) 1.3128(4) 0.04811(12) 0.0496(10) Uani 1 1 d . . . H9 H 0.5042 1.2513 0.0466 0.060 Uiso 1 1 calc R . . C10 C 0.4404(3) 1.3715(5) 0.00765(13) 0.0659(13) Uani 1 1 d . . . H10 H 0.4592 1.3490 -0.0211 0.079 Uiso 1 1 calc R . . C11 C 0.3866(2) 1.4615(5) 0.00902(14) 0.0586(12) Uani 1 1 d . . . H11 H 0.3686 1.4992 -0.0186 0.070 Uiso 1 1 calc R . . C12 C 0.3591(2) 1.4960(4) 0.05129(14) 0.0483(10) Uani 1 1 d . . . H12 H 0.3228 1.5582 0.0524 0.058 Uiso 1 1 calc R . . C13 C 0.38500(18) 1.4390(4) 0.09249(13) 0.0417(9) Uani 1 1 d . . . H13 H 0.3658 1.4621 0.1211 0.050 Uiso 1 1 calc R . . C14 C 0.39713(17) 1.1981(3) 0.17219(11) 0.0326(8) Uani 1 1 d . . . C15 C 0.33393(18) 1.1725(4) 0.14799(13) 0.0426(9) Uani 1 1 d . . . H15 H 0.3285 1.1970 0.1167 0.051 Uiso 1 1 calc R . . C16 C 0.2784(2) 1.1102(5) 0.17020(16) 0.0615(13) Uani 1 1 d . . . H16 H 0.2358 1.0921 0.1539 0.074 Uiso 1 1 calc R . . C17 C 0.2869(2) 1.0754(5) 0.21645(17) 0.0624(13) Uani 1 1 d . . . H17 H 0.2492 1.0354 0.2315 0.075 Uiso 1 1 calc R . . C18 C 0.3490(2) 1.0982(4) 0.24060(14) 0.0546(11) Uani 1 1 d . . . H18 H 0.3538 1.0732 0.2719 0.066 Uiso 1 1 calc R . . C19 C 0.40581(19) 1.1590(4) 0.21882(12) 0.0419(9) Uani 1 1 d . . . H19 H 0.4489 1.1733 0.2351 0.050 Uiso 1 1 calc R . . C20 C 0.53386(17) 1.1431(3) 0.13031(11) 0.0325(8) Uani 1 1 d . . . C21 C 0.50942(19) 1.0167(4) 0.12538(15) 0.0493(11) Uani 1 1 d . . . H21 H 0.4611 0.9985 0.1288 0.059 Uiso 1 1 calc R . . C22 C 0.5562(2) 0.9172(4) 0.11538(16) 0.0584(12) Uani 1 1 d . . . H22 H 0.5394 0.8322 0.1116 0.070 Uiso 1 1 calc R . . C23 C 0.6280(2) 0.9439(4) 0.11104(14) 0.0496(10) Uani 1 1 d . . . H23 H 0.6600 0.8764 0.1053 0.059 Uiso 1 1 calc R . . C24 C 0.65218(19) 1.0690(4) 0.11511(13) 0.0462(10) Uani 1 1 d . . . H24 H 0.7005 1.0867 0.1114 0.055 Uiso 1 1 calc R . . C25 C 0.60585(18) 1.1696(4) 0.12467(12) 0.0400(9) Uani 1 1 d . . . H25 H 0.6228 1.2549 0.1273 0.048 Uiso 1 1 calc R . . C26 C 0.92589(18) 1.1406(4) 0.09363(12) 0.0380(8) Uani 1 1 d . . . H26A H 0.9118 1.2236 0.1070 0.046 Uiso 1 1 calc R . . H26B H 0.9183 1.1461 0.0599 0.046 Uiso 1 1 calc R . . C27 C 0.87901(16) 1.0341(4) 0.11244(12) 0.0332(8) Uani 1 1 d . . . C28 C 0.85291(19) 0.9357(4) 0.08342(13) 0.0424(9) Uani 1 1 d . . . H28 H 0.8622 0.9384 0.0516 0.051 Uiso 1 1 calc R . . C29 C 0.8137(2) 0.8343(4) 0.10070(15) 0.0495(10) Uani 1 1 d . . . H29 H 0.7959 0.7695 0.0806 0.059 Uiso 1 1 calc R . . C30 C 0.8005(2) 0.8287(4) 0.14802(15) 0.0526(11) Uani 1 1 d . . . H30 H 0.7751 0.7586 0.1601 0.063 Uiso 1 1 calc R . . C31 C 0.8246(2) 0.9256(4) 0.17699(14) 0.0517(11) Uani 1 1 d . . . H31 H 0.8148 0.9221 0.2088 0.062 Uiso 1 1 calc R . . C50 C 1.13240(19) 1.2836(4) 0.09508(13) 0.0448(10) Uani 1 1 d . . . H50 H 1.1438 1.2675 0.1265 0.054 Uiso 1 1 calc R . . C32 C 0.86361(18) 1.0296(4) 0.15985(13) 0.0431(9) Uani 1 1 d . . . H32 H 0.8794 1.0960 0.1799 0.052 Uiso 1 1 calc R . . C33 C 1.04656(17) 0.9544(4) 0.08835(11) 0.0338(8) Uani 1 1 d . . . C34 C 1.01627(18) 0.8426(4) 0.10693(13) 0.0407(9) Uani 1 1 d . . . H34 H 0.9818 0.8500 0.1297 0.049 Uiso 1 1 calc R . . C35 C 1.0369(2) 0.7208(4) 0.09192(15) 0.0526(11) Uani 1 1 d . . . H35 H 1.0156 0.6462 0.1039 0.063 Uiso 1 1 calc R . . C36 C 1.0895(2) 0.7098(5) 0.05883(16) 0.0618(12) Uani 1 1 d . . . H36 H 1.1038 0.6275 0.0488 0.074 Uiso 1 1 calc R . . C37 C 1.1204(2) 0.8189(5) 0.04085(15) 0.0569(12) Uani 1 1 d . . . H37 H 1.1554 0.8104 0.0185 0.068 Uiso 1 1 calc R . . C46 C 1.0538(2) 1.2572(5) 0.02824(13) 0.0564(12) Uani 1 1 d . . . H46 H 1.0122 1.2230 0.0144 0.068 Uiso 1 1 calc R . . C38 C 1.10043(19) 0.9411(4) 0.05542(12) 0.0427(9) Uani 1 1 d . . . H38 H 1.1225 1.0150 0.0435 0.051 Uiso 1 1 calc R . . C49 C 1.1770(2) 1.3611(4) 0.06866(15) 0.0546(11) Uani 1 1 d . . . H49 H 1.2184 1.3966 0.0823 0.065 Uiso 1 1 calc R . . C39 C 1.03979(16) 1.1324(4) 0.16846(11) 0.0318(8) Uani 1 1 d . . . C40 C 1.07566(17) 1.0358(4) 0.19379(12) 0.0373(8) Uani 1 1 d . . . H40 H 1.0894 0.9589 0.1791 0.045 Uiso 1 1 calc R . . C45 C 1.07135(18) 1.2304(4) 0.07484(12) 0.0365(8) Uani 1 1 d . . . C41 C 1.09101(18) 1.0548(4) 0.24138(12) 0.0425(9) Uani 1 1 d . . . H41 H 1.1147 0.9901 0.2587 0.051 Uiso 1 1 calc R . . C42 C 1.07119(19) 1.1686(4) 0.26262(13) 0.0467(10) Uani 1 1 d . . . H42 H 1.0812 1.1809 0.2944 0.056 Uiso 1 1 calc R . . C43 C 1.0367(2) 1.2643(4) 0.23731(13) 0.0481(10) Uani 1 1 d . . . H43 H 1.0243 1.3419 0.2520 0.058 Uiso 1 1 calc R . . C44 C 1.01999(19) 1.2475(4) 0.19011(12) 0.0410(9) Uani 1 1 d . . . H44 H 0.9959 1.3125 0.1732 0.049 Uiso 1 1 calc R . . C47 C 1.0989(2) 1.3354(4) 0.00250(14) 0.0574(12) Uani 1 1 d . . . H47 H 1.0873 1.3536 -0.0287 0.069 Uiso 1 1 calc R . . C48 C 1.1598(2) 1.3855(4) 0.02239(14) 0.0511(11) Uani 1 1 d . . . H48 H 1.1900 1.4366 0.0046 0.061 Uiso 1 1 calc R . . C51 C 0.1982(2) 1.6133(5) 0.20187(15) 0.0606(12) Uani 1 1 d . . . H51 H 0.224(2) 1.642(4) 0.2317(15) 0.073 Uiso 1 1 d . . . C52 C 0.3297(2) 0.9353(5) 0.01925(16) 0.0612(13) Uani 1 1 d . . . H52 H 0.305(2) 0.888(5) -0.0050(15) 0.073 Uiso 1 1 d . . . Br1 Br 0.241953(19) 0.82389(4) 0.453813(12) 0.03986(10) Uani 1 1 d . . . Br2 Br 0.23873(2) 0.82630(4) 0.303121(12) 0.04482(11) Uani 1 1 d . . . Br3 Br 0.338400(18) 1.05456(4) 0.380136(13) 0.04065(10) Uani 1 1 d . . . Br4 Br 0.109239(18) 0.98672(4) 0.378037(13) 0.04127(10) Uani 1 1 d . . . Cu1 Cu 0.23184(2) 0.92584(4) 0.378502(13) 0.03096(11) Uani 1 1 d . . . P1 P 0.47165(4) 1.26995(9) 0.14357(3) 0.0298(2) Uani 1 1 d . . . P2 P 1.02009(5) 1.11354(9) 0.10665(3) 0.0316(2) Uani 1 1 d . . . Cl1 Cl 0.23226(7) 1.45511(15) 0.19248(4) 0.0823(4) Uani 1 1 d . . . Cl2 Cl 0.10663(6) 1.60897(17) 0.20906(5) 0.0880(5) Uani 1 1 d . . . Cl3 Cl 0.21902(8) 1.7171(2) 0.15529(5) 0.1139(7) Uani 1 1 d . . . Cl4 Cl 0.42060(7) 0.94854(18) 0.01120(5) 0.0984(5) Uani 1 1 d . . . Cl5 Cl 0.31355(8) 0.86637(16) 0.07379(5) 0.0915(5) Uani 1 1 d . . . Cl6 Cl 0.28838(8) 1.08850(17) 0.01538(5) 0.0944(5) Uani 1 1 d . . . 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 C1 0.0351(18) 0.037(2) 0.0378(18) 0.0006(17) 0.0007(15) -0.0010(16) C2 0.0282(17) 0.039(2) 0.0334(18) -0.0047(16) -0.0015(14) -0.0029(16) C3 0.049(2) 0.047(2) 0.0361(19) -0.0030(18) 0.0027(17) -0.0054(19) C4 0.046(2) 0.064(3) 0.044(2) -0.022(2) 0.0096(18) 0.000(2) C5 0.039(2) 0.050(3) 0.069(3) -0.020(2) -0.002(2) 0.006(2) C6 0.058(3) 0.037(2) 0.070(3) -0.002(2) 0.006(2) 0.007(2) C7 0.049(2) 0.043(2) 0.050(2) 0.003(2) 0.0094(19) 0.0024(19) C8 0.0311(17) 0.036(2) 0.0345(18) 0.0056(16) 0.0031(15) -0.0017(15) C9 0.057(2) 0.055(3) 0.037(2) 0.0061(19) 0.0068(18) 0.010(2) C10 0.086(3) 0.083(4) 0.029(2) 0.008(2) 0.008(2) 0.011(3) C11 0.066(3) 0.064(3) 0.045(2) 0.022(2) -0.007(2) 0.004(2) C12 0.041(2) 0.047(3) 0.056(2) 0.014(2) -0.0075(19) 0.0043(19) C13 0.0359(19) 0.045(2) 0.044(2) 0.0051(18) 0.0002(16) 0.0017(18) C14 0.0330(18) 0.030(2) 0.0354(18) 0.0051(15) 0.0039(15) 0.0015(15) C15 0.037(2) 0.048(3) 0.042(2) 0.0096(18) -0.0005(17) -0.0053(18) C16 0.033(2) 0.068(3) 0.083(3) 0.029(3) -0.005(2) -0.015(2) C17 0.041(2) 0.066(3) 0.081(3) 0.031(3) 0.018(2) -0.003(2) C18 0.058(3) 0.058(3) 0.048(2) 0.023(2) 0.012(2) 0.002(2) C19 0.042(2) 0.045(2) 0.039(2) 0.0109(18) 0.0015(17) 0.0001(18) C20 0.0299(17) 0.033(2) 0.0347(18) 0.0056(15) 0.0019(15) 0.0000(15) C21 0.036(2) 0.036(2) 0.076(3) -0.002(2) 0.017(2) -0.0017(18) C22 0.057(3) 0.028(2) 0.091(3) 0.000(2) 0.019(2) -0.0017(19) C23 0.043(2) 0.046(3) 0.061(2) 0.004(2) 0.0138(19) 0.0124(19) C24 0.0332(19) 0.049(3) 0.057(2) 0.000(2) 0.0068(18) 0.0034(19) C25 0.0340(19) 0.038(2) 0.049(2) -0.0031(18) 0.0023(17) -0.0039(17) C26 0.040(2) 0.035(2) 0.0392(19) 0.0000(17) -0.0047(16) 0.0013(17) C27 0.0264(16) 0.035(2) 0.0375(18) -0.0010(16) 0.0003(14) 0.0062(15) C28 0.039(2) 0.046(2) 0.041(2) -0.0050(19) -0.0045(16) -0.0012(18) C29 0.043(2) 0.046(3) 0.059(3) -0.009(2) -0.0046(19) -0.0020(19) C30 0.039(2) 0.051(3) 0.067(3) 0.011(2) 0.001(2) -0.003(2) C31 0.046(2) 0.063(3) 0.047(2) -0.005(2) 0.0099(19) -0.006(2) C50 0.043(2) 0.048(3) 0.043(2) 0.0078(19) -0.0006(18) -0.0072(19) C32 0.0349(19) 0.051(3) 0.043(2) -0.0127(19) 0.0043(16) -0.0006(18) C33 0.0316(17) 0.035(2) 0.0343(18) -0.0007(16) -0.0009(14) -0.0012(16) C34 0.0325(19) 0.038(2) 0.052(2) 0.0038(18) -0.0015(17) 0.0010(16) C35 0.044(2) 0.035(2) 0.078(3) -0.008(2) -0.015(2) -0.0017(19) C36 0.060(3) 0.053(3) 0.072(3) -0.025(3) -0.015(2) 0.022(2) C37 0.047(2) 0.074(3) 0.049(2) -0.016(2) 0.0034(19) 0.014(2) C46 0.062(3) 0.065(3) 0.042(2) 0.013(2) -0.008(2) -0.021(2) C38 0.040(2) 0.050(3) 0.039(2) -0.0031(18) 0.0072(16) -0.0005(18) C49 0.048(2) 0.055(3) 0.061(3) 0.007(2) 0.002(2) -0.021(2) C39 0.0278(17) 0.036(2) 0.0311(17) 0.0022(16) -0.0011(14) 0.0023(15) C40 0.0353(18) 0.041(2) 0.0359(19) 0.0017(17) 0.0029(15) -0.0016(17) C45 0.043(2) 0.031(2) 0.0362(19) -0.0002(16) 0.0025(16) -0.0045(17) C41 0.0356(19) 0.052(3) 0.040(2) 0.0115(19) -0.0075(16) -0.0006(18) C42 0.045(2) 0.063(3) 0.0325(19) 0.000(2) -0.0051(17) -0.006(2) C43 0.055(2) 0.050(3) 0.039(2) -0.0097(19) 0.0006(19) 0.005(2) C44 0.044(2) 0.040(2) 0.0383(19) 0.0019(17) -0.0037(17) 0.0063(18) C47 0.078(3) 0.057(3) 0.038(2) 0.014(2) 0.001(2) -0.016(2) C48 0.066(3) 0.037(2) 0.052(2) 0.006(2) 0.022(2) -0.005(2) C51 0.058(3) 0.082(4) 0.042(2) 0.001(2) -0.001(2) -0.010(2) C52 0.051(3) 0.077(4) 0.056(3) -0.017(2) 0.002(2) -0.013(2) Br1 0.0464(2) 0.0427(2) 0.03063(18) 0.00754(16) 0.00394(15) 0.00051(17) Br2 0.0613(2) 0.0419(2) 0.03143(18) -0.00463(16) 0.00455(17) 0.00416(19) Br3 0.03534(19) 0.0410(2) 0.0460(2) 0.00003(17) 0.00715(15) -0.00566(16) Br4 0.03338(18) 0.0390(2) 0.0513(2) -0.00037(18) 0.00035(16) 0.00294(16) Cu1 0.0317(2) 0.0340(2) 0.0274(2) 0.00112(18) 0.00375(16) -0.00051(18) P1 0.0275(4) 0.0302(5) 0.0320(4) 0.0028(4) 0.0026(4) -0.0006(4) P2 0.0331(5) 0.0318(5) 0.0298(4) 0.0014(4) 0.0008(4) -0.0006(4) Cl1 0.0753(8) 0.1001(11) 0.0718(8) -0.0355(8) 0.0077(6) -0.0063(7) Cl2 0.0556(7) 0.1322(14) 0.0768(8) 0.0284(9) 0.0129(6) 0.0038(8) Cl3 0.0763(9) 0.1771(19) 0.0877(10) 0.0654(11) -0.0106(7) -0.0406(10) Cl4 0.0563(7) 0.1438(16) 0.0959(10) -0.0221(10) 0.0162(7) -0.0094(8) Cl5 0.1079(11) 0.0939(11) 0.0735(8) 0.0079(8) 0.0161(8) -0.0270(9) Cl6 0.1015(10) 0.0973(12) 0.0834(9) -0.0012(9) -0.0154(8) 0.0169(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.510(5) . ? C1 P1 1.804(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.367(5) . ? C2 C3 1.391(4) . ? C3 C4 1.394(5) . ? C3 H3 0.9300 . ? C4 C5 1.355(6) . ? C4 H4 0.9300 . ? C5 C6 1.371(5) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.387(5) . ? C8 C9 1.387(5) . ? C8 P1 1.787(4) . ? C9 C10 1.385(6) . ? C9 H9 0.9300 . ? C10 C11 1.364(6) . ? C10 H10 0.9300 . ? C11 C12 1.370(5) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.376(5) . ? C14 C19 1.394(5) . ? C14 P1 1.791(3) . ? C15 C16 1.386(5) . ? C15 H15 0.9300 . ? C16 C17 1.371(6) . ? C16 H16 0.9300 . ? C17 C18 1.353(6) . ? C17 H17 0.9300 . ? C18 C19 1.391(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.376(5) . ? C20 C25 1.386(5) . ? C20 P1 1.789(3) . ? C21 C22 1.377(5) . ? C21 H21 0.9300 . ? C22 C23 1.378(5) . ? C22 H22 0.9300 . ? C23 C24 1.359(5) . ? C23 H23 0.9300 . ? C24 C25 1.377(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.506(5) . ? C26 P2 1.810(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.383(5) . ? C27 C32 1.391(5) . ? C28 C29 1.369(5) . ? C28 H28 0.9300 . ? C29 C30 1.380(5) . ? C29 H29 0.9300 . ? C30 C31 1.359(6) . ? C30 H30 0.9300 . ? C31 C32 1.386(5) . ? C31 H31 0.9300 . ? C50 C45 1.376(5) . ? C50 C49 1.388(5) . ? C50 H50 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.388(5) . ? C33 C38 1.402(4) . ? C33 P2 1.783(4) . ? C34 C35 1.375(5) . ? C34 H34 0.9300 . ? C35 C36 1.387(6) . ? C35 H35 0.9300 . ? C36 C37 1.363(6) . ? C36 H36 0.9300 . ? C37 C38 1.372(6) . ? C37 H37 0.9300 . ? C46 C47 1.387(5) . ? C46 C45 1.387(5) . ? C46 H46 0.9300 . ? C38 H38 0.9300 . ? C49 C48 1.372(6) . ? C49 H49 0.9300 . ? C39 C44 1.385(5) . ? C39 C40 1.385(5) . ? C39 P2 1.801(3) . ? C40 C41 1.393(5) . ? C40 H40 0.9300 . ? C45 P2 1.794(3) . ? C41 C42 1.368(5) . ? C41 H41 0.9300 . ? C42 C43 1.367(6) . ? C42 H42 0.9300 . ? C43 C44 1.384(5) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C47 C48 1.358(6) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C51 Cl2 1.730(4) . ? C51 Cl3 1.752(5) . ? C51 Cl1 1.761(5) . ? C51 H51 1.01(5) . ? C52 Cl4 1.725(4) . ? C52 Cl5 1.742(5) . ? C52 Cl6 1.748(5) . ? C52 H52 0.96(5) . ? Br1 Cu1 2.3904(5) . ? Br2 Cu1 2.3855(5) . ? Br3 Cu1 2.3860(5) . ? Br4 Cu1 2.3735(5) . ? 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 C2 C1 P1 114.9(2) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 118.5(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 121.0(3) . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.8(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 121.1(3) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C13 C8 C9 119.8(3) . . ? C13 C8 P1 120.1(3) . . ? C9 C8 P1 120.1(3) . . ? C10 C9 C8 118.9(4) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.6(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? C15 C14 C19 119.9(3) . . ? C15 C14 P1 121.1(3) . . ? C19 C14 P1 118.8(3) . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 119.0(4) . . ? C18 C19 H19 120.5 . . ? C14 C19 H19 120.5 . . ? C21 C20 C25 119.5(3) . . ? C21 C20 P1 119.1(2) . . ? C25 C20 P1 121.4(3) . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 119.9(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.0(4) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.7(3) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C24 C25 C20 119.6(4) . . ? C24 C25 H25 120.2 . . ? C20 C25 H25 120.2 . . ? C27 C26 P2 112.9(2) . . ? C27 C26 H26A 109.0 . . ? P2 C26 H26A 109.0 . . ? C27 C26 H26B 109.0 . . ? P2 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C32 118.6(3) . . ? C28 C27 C26 120.8(3) . . ? C32 C27 C26 120.6(3) . . ? C29 C28 C27 121.2(4) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 119.7(4) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.9(4) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C45 C50 C49 120.1(4) . . ? C45 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C31 C32 C27 119.6(4) . . ? C31 C32 H32 120.2 . . ? C27 C32 H32 120.2 . . ? C34 C33 C38 118.9(3) . . ? C34 C33 P2 121.4(3) . . ? C38 C33 P2 119.7(3) . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.7(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.6(4) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C47 C46 C45 119.3(4) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C37 C38 C33 119.9(4) . . ? C37 C38 H38 120.1 . . ? C33 C38 H38 120.1 . . ? C48 C49 C50 119.9(4) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C44 C39 C40 120.3(3) . . ? C44 C39 P2 118.5(3) . . ? C40 C39 P2 121.1(3) . . ? C39 C40 C41 119.5(4) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C50 C45 C46 119.7(3) . . ? C50 C45 P2 119.9(3) . . ? C46 C45 P2 120.1(3) . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120.3(4) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 121.0(4) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C39 118.9(4) . . ? C43 C44 H44 120.5 . . ? C39 C44 H44 120.5 . . ? C48 C47 C46 120.8(4) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 120.2(4) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? Cl2 C51 Cl3 110.3(3) . . ? Cl2 C51 Cl1 110.9(3) . . ? Cl3 C51 Cl1 110.6(2) . . ? Cl2 C51 H51 111(2) . . ? Cl3 C51 H51 110(3) . . ? Cl1 C51 H51 103(3) . . ? Cl4 C52 Cl5 110.3(3) . . ? Cl4 C52 Cl6 110.9(3) . . ? Cl5 C52 Cl6 109.4(2) . . ? Cl4 C52 H52 114(3) . . ? Cl5 C52 H52 110(3) . . ? Cl6 C52 H52 102(3) . . ? Br4 Cu1 Br2 100.56(2) . . ? Br4 Cu1 Br3 131.31(2) . . ? Br2 Cu1 Br3 100.764(19) . . ? Br4 Cu1 Br1 99.861(18) . . ? Br2 Cu1 Br1 128.25(2) . . ? Br3 Cu1 Br1 100.26(2) . . ? C8 P1 C20 110.34(15) . . ? C8 P1 C14 108.58(16) . . ? C20 P1 C14 108.49(16) . . ? C8 P1 C1 111.88(17) . . ? C20 P1 C1 107.88(17) . . ? C14 P1 C1 109.61(16) . . ? C33 P2 C45 107.65(16) . . ? C33 P2 C39 109.48(17) . . ? C45 P2 C39 109.06(16) . . ? C33 P2 C26 110.82(17) . . ? C45 P2 C26 108.94(17) . . ? C39 P2 C26 110.81(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C1 C2 C7 -92.0(4) . . . . ? P1 C1 C2 C3 88.5(4) . . . . ? C7 C2 C3 C4 1.1(5) . . . . ? C1 C2 C3 C4 -179.3(4) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C3 C4 C5 C6 -1.4(6) . . . . ? C4 C5 C6 C7 0.5(6) . . . . ? C3 C2 C7 C6 -2.0(6) . . . . ? C1 C2 C7 C6 178.4(4) . . . . ? C5 C6 C7 C2 1.2(6) . . . . ? C13 C8 C9 C10 0.2(6) . . . . ? P1 C8 C9 C10 178.1(4) . . . . ? C8 C9 C10 C11 -0.3(7) . . . . ? C9 C10 C11 C12 0.6(8) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C11 C12 C13 C8 0.7(6) . . . . ? C9 C8 C13 C12 -0.4(6) . . . . ? P1 C8 C13 C12 -178.2(3) . . . . ? C19 C14 C15 C16 1.3(6) . . . . ? P1 C14 C15 C16 176.4(3) . . . . ? C14 C15 C16 C17 0.5(7) . . . . ? C15 C16 C17 C18 -1.4(7) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C17 C18 C19 C14 1.3(6) . . . . ? C15 C14 C19 C18 -2.2(6) . . . . ? P1 C14 C19 C18 -177.4(3) . . . . ? C25 C20 C21 C22 0.6(6) . . . . ? P1 C20 C21 C22 -179.7(3) . . . . ? C20 C21 C22 C23 1.1(7) . . . . ? C21 C22 C23 C24 -2.1(7) . . . . ? C22 C23 C24 C25 1.5(6) . . . . ? C23 C24 C25 C20 0.2(6) . . . . ? C21 C20 C25 C24 -1.2(6) . . . . ? P1 C20 C25 C24 179.1(3) . . . . ? P2 C26 C27 C28 -100.0(4) . . . . ? P2 C26 C27 C32 77.2(4) . . . . ? C32 C27 C28 C29 -1.1(5) . . . . ? C26 C27 C28 C29 176.2(3) . . . . ? C27 C28 C29 C30 -0.9(6) . . . . ? C28 C29 C30 C31 2.0(6) . . . . ? C29 C30 C31 C32 -1.2(6) . . . . ? C30 C31 C32 C27 -0.8(6) . . . . ? C28 C27 C32 C31 1.9(5) . . . . ? C26 C27 C32 C31 -175.4(3) . . . . ? C38 C33 C34 C35 -2.5(6) . . . . ? P2 C33 C34 C35 179.3(3) . . . . ? C33 C34 C35 C36 1.5(6) . . . . ? C34 C35 C36 C37 -0.5(6) . . . . ? C35 C36 C37 C38 0.5(7) . . . . ? C36 C37 C38 C33 -1.4(6) . . . . ? C34 C33 C38 C37 2.4(6) . . . . ? P2 C33 C38 C37 -179.3(3) . . . . ? C45 C50 C49 C48 0.4(7) . . . . ? C44 C39 C40 C41 0.7(5) . . . . ? P2 C39 C40 C41 178.9(3) . . . . ? C49 C50 C45 C46 -1.4(6) . . . . ? C49 C50 C45 P2 171.9(3) . . . . ? C47 C46 C45 C50 1.2(6) . . . . ? C47 C46 C45 P2 -172.2(3) . . . . ? C39 C40 C41 C42 -0.6(5) . . . . ? C40 C41 C42 C43 -0.4(6) . . . . ? C41 C42 C43 C44 1.2(6) . . . . ? C42 C43 C44 C39 -1.0(6) . . . . ? C40 C39 C44 C43 0.1(5) . . . . ? P2 C39 C44 C43 -178.2(3) . . . . ? C45 C46 C47 C48 0.1(7) . . . . ? C46 C47 C48 C49 -1.1(7) . . . . ? C50 C49 C48 C47 0.8(7) . . . . ? C13 C8 P1 C20 173.0(3) . . . . ? C9 C8 P1 C20 -4.9(4) . . . . ? C13 C8 P1 C14 54.2(3) . . . . ? C9 C8 P1 C14 -123.7(3) . . . . ? C13 C8 P1 C1 -66.9(3) . . . . ? C9 C8 P1 C1 115.2(3) . . . . ? C21 C20 P1 C8 -94.1(3) . . . . ? C25 C20 P1 C8 85.5(3) . . . . ? C21 C20 P1 C14 24.7(4) . . . . ? C25 C20 P1 C14 -155.6(3) . . . . ? C21 C20 P1 C1 143.4(3) . . . . ? C25 C20 P1 C1 -37.0(3) . . . . ? C15 C14 P1 C8 19.6(4) . . . . ? C19 C14 P1 C8 -165.2(3) . . . . ? C15 C14 P1 C20 -100.3(3) . . . . ? C19 C14 P1 C20 74.8(3) . . . . ? C15 C14 P1 C1 142.1(3) . . . . ? C19 C14 P1 C1 -42.7(3) . . . . ? C2 C1 P1 C8 58.6(3) . . . . ? C2 C1 P1 C20 -179.8(2) . . . . ? C2 C1 P1 C14 -61.9(3) . . . . ? C34 C33 P2 C45 179.8(3) . . . . ? C38 C33 P2 C45 1.6(3) . . . . ? C34 C33 P2 C39 61.4(3) . . . . ? C38 C33 P2 C39 -116.9(3) . . . . ? C34 C33 P2 C26 -61.1(3) . . . . ? C38 C33 P2 C26 120.6(3) . . . . ? C50 C45 P2 C33 -96.8(3) . . . . ? C46 C45 P2 C33 76.5(4) . . . . ? C50 C45 P2 C39 21.9(4) . . . . ? C46 C45 P2 C39 -164.8(3) . . . . ? C50 C45 P2 C26 142.9(3) . . . . ? C46 C45 P2 C26 -43.7(4) . . . . ? C44 C39 P2 C33 -176.9(3) . . . . ? C40 C39 P2 C33 4.8(3) . . . . ? C44 C39 P2 C45 65.6(3) . . . . ? C40 C39 P2 C45 -112.7(3) . . . . ? C44 C39 P2 C26 -54.4(3) . . . . ? C40 C39 P2 C26 127.4(3) . . . . ? C27 C26 P2 C33 52.5(3) . . . . ? C27 C26 P2 C45 170.7(2) . . . . ? C27 C26 P2 C39 -69.3(3) . . . . ?