# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_r150 _database_code_depnum_ccdc_archive 'CCDC 871234' #TrackingRef 'R150-7a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H34 Cu N2 P' _chemical_formula_weight 697.25 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' P P 0.1023 0.0942 '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' _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 12.4918(18) _cell_length_b 14.252(2) _cell_length_c 21.345(3) _cell_angle_alpha 90.005(2) _cell_angle_beta 86.958(2) _cell_angle_gamma 89.993(3) _cell_volume 3794.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7943 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7888 _exptl_absorpt_correction_T_max 0.8596 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21357 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.12 _reflns_number_total 14623 _reflns_number_gt 11363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data set was corrected using the program SQUEEZE. There are two seriously disordered Et2O solvate molecules in one structural unit estimated based on the chemical analyses of elemental analyses and 1H NMR spectra. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 241 49 ' ' 2 0.500 0.500 1.000 266 55 ' ' _platon_squeeze_details ; ; _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^)+(0.0650P)^2^+6.3827P] 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 14623 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.49056(3) 0.67202(3) 0.41582(2) 0.02622(12) Uani 1 1 d . . . Cu2 Cu 0.00101(3) 0.17296(3) 0.08400(2) 0.02610(12) Uani 1 1 d . . . N1 N 0.6219(2) 0.7412(2) 0.43305(14) 0.0307(7) Uani 1 1 d . . . N2 N 0.4225(2) 0.6867(2) 0.50191(14) 0.0309(7) Uani 1 1 d . . . N3 N 0.0521(2) 0.1967(2) -0.00466(14) 0.0297(7) Uani 1 1 d . . . N4 N -0.1389(2) 0.2338(2) 0.07775(15) 0.0320(7) Uani 1 1 d . . . P1 P 0.39905(7) 0.63638(6) 0.33550(4) 0.0252(2) Uani 1 1 d . . . P2 P 0.09671(7) 0.13623(6) 0.16202(4) 0.0245(2) Uani 1 1 d . . . C1 C 0.7130(3) 0.7515(3) 0.39846(18) 0.0332(9) Uani 1 1 d . . . C2 C 0.7735(3) 0.8283(3) 0.4216(2) 0.0413(10) Uani 1 1 d . . . H2A H 0.8392 0.8501 0.4049 0.050 Uiso 1 1 calc R . . C3 C 0.7171(3) 0.8634(3) 0.4723(2) 0.0396(10) Uani 1 1 d . . . H3A H 0.7372 0.9134 0.4971 0.047 Uiso 1 1 calc R . . C4 C 0.6214(3) 0.8094(3) 0.48063(18) 0.0317(8) Uani 1 1 d . . . C5 C 0.5377(3) 0.8209(3) 0.52678(17) 0.0324(8) Uani 1 1 d . . . C6 C 0.4448(3) 0.7680(3) 0.53525(18) 0.0346(9) Uani 1 1 d . . . C7 C 0.3580(4) 0.7815(3) 0.58171(19) 0.0463(11) Uani 1 1 d . . . H7A H 0.3524 0.8301 0.6108 0.056 Uiso 1 1 calc R . . C8 C 0.2868(4) 0.7120(3) 0.5759(2) 0.0498(12) Uani 1 1 d . . . H8A H 0.2225 0.7042 0.5993 0.060 Uiso 1 1 calc R . . C9 C 0.3283(3) 0.6528(3) 0.52719(17) 0.0347(9) Uani 1 1 d . . . C10 C 0.7431(3) 0.6879(3) 0.34738(18) 0.0340(9) Uani 1 1 d . . . C11 C 0.8047(3) 0.7196(4) 0.2946(2) 0.0472(11) Uani 1 1 d . . . H11A H 0.8261 0.7821 0.2924 0.057 Uiso 1 1 calc R . . C12 C 0.8336(4) 0.6599(4) 0.2465(2) 0.0631(15) Uani 1 1 d . . . H12A H 0.8756 0.6820 0.2123 0.076 Uiso 1 1 calc R . . C13 C 0.8012(4) 0.5666(5) 0.2478(2) 0.0666(15) Uani 1 1 d . . . H13A H 0.8199 0.5267 0.2146 0.080 Uiso 1 1 calc R . . C14 C 0.7404(4) 0.5338(4) 0.2996(2) 0.0533(12) Uani 1 1 d . . . H14A H 0.7184 0.4715 0.3013 0.064 Uiso 1 1 calc R . . C15 C 0.7127(3) 0.5937(3) 0.34854(19) 0.0393(10) Uani 1 1 d . . . H15A H 0.6728 0.5707 0.3832 0.047 Uiso 1 1 calc R . . C16 C 0.2832(3) 0.5631(3) 0.50861(18) 0.0347(9) Uani 1 1 d . . . C17 C 0.3473(3) 0.4941(3) 0.47968(19) 0.0379(9) Uani 1 1 d . . . H17A H 0.4196 0.5063 0.4706 0.045 Uiso 1 1 calc R . . C18 C 0.3058(4) 0.4074(3) 0.4640(2) 0.0437(10) Uani 1 1 d . . . H18A H 0.3503 0.3625 0.4446 0.052 Uiso 1 1 calc R . . C19 C 0.1986(4) 0.3875(3) 0.4771(2) 0.0519(12) Uani 1 1 d . . . H19A H 0.1705 0.3295 0.4668 0.062 Uiso 1 1 calc R . . C20 C 0.1344(4) 0.4549(4) 0.5057(2) 0.0520(12) Uani 1 1 d . . . H20A H 0.0625 0.4416 0.5151 0.062 Uiso 1 1 calc R . . C21 C 0.1734(3) 0.5410(3) 0.5206(2) 0.0450(11) Uani 1 1 d . . . H21A H 0.1274 0.5858 0.5388 0.054 Uiso 1 1 calc R . . C22 C 0.5552(3) 0.8964(3) 0.57477(19) 0.0364(9) Uani 1 1 d . . . C23 C 0.4932(4) 0.9775(3) 0.57939(19) 0.0426(10) Uani 1 1 d . . . H23A H 0.4385 0.9858 0.5520 0.051 Uiso 1 1 calc R . . C24 C 0.5105(4) 1.0451(3) 0.6229(2) 0.0477(11) Uani 1 1 d . . . H24A H 0.4677 1.0985 0.6252 0.057 Uiso 1 1 calc R . . C25 C 0.5929(5) 1.0339(3) 0.6641(2) 0.0592(14) Uani 1 1 d . . . H25A H 0.6068 1.0802 0.6933 0.071 Uiso 1 1 calc R . . C26 C 0.6514(4) 0.9553(4) 0.6607(2) 0.0560(13) Uani 1 1 d . . . H26A H 0.7055 0.9469 0.6884 0.067 Uiso 1 1 calc R . . C27 C 0.6338(4) 0.8860(3) 0.6170(2) 0.0457(11) Uani 1 1 d . . . H27A H 0.6755 0.8319 0.6161 0.055 Uiso 1 1 calc R . . C28 C 0.4161(3) 0.7154(2) 0.26799(16) 0.0274(8) Uani 1 1 d . . . C29 C 0.5182(3) 0.7457(3) 0.25028(19) 0.0376(9) Uani 1 1 d . . . H29A H 0.5758 0.7274 0.2734 0.045 Uiso 1 1 calc R . . C30 C 0.5359(4) 0.8039(3) 0.1978(2) 0.0482(11) Uani 1 1 d . . . H30A H 0.6051 0.8233 0.1859 0.058 Uiso 1 1 calc R . . C31 C 0.4517(4) 0.8321(3) 0.1641(2) 0.0476(11) Uani 1 1 d . . . H31A H 0.4633 0.8705 0.1291 0.057 Uiso 1 1 calc R . . C32 C 0.3488(4) 0.8031(3) 0.1824(2) 0.0450(11) Uani 1 1 d . . . H32A H 0.2912 0.8232 0.1600 0.054 Uiso 1 1 calc R . . C33 C 0.3308(3) 0.7450(3) 0.23327(19) 0.0372(9) Uani 1 1 d . . . H33A H 0.2615 0.7252 0.2446 0.045 Uiso 1 1 calc R . . C34 C 0.2560(3) 0.6478(3) 0.35638(16) 0.0270(8) Uani 1 1 d . . . C35 C 0.1769(3) 0.5850(3) 0.33952(19) 0.0369(9) Uani 1 1 d . . . H35A H 0.1958 0.5311 0.3171 0.044 Uiso 1 1 calc R . . C36 C 0.0696(3) 0.6032(3) 0.3563(2) 0.0483(11) Uani 1 1 d . . . H36A H 0.0168 0.5620 0.3442 0.058 Uiso 1 1 calc R . . C37 C 0.0415(3) 0.6821(3) 0.3909(2) 0.0496(12) Uani 1 1 d . . . H37A H -0.0301 0.6938 0.4023 0.059 Uiso 1 1 calc R . . C38 C 0.1189(3) 0.7431(3) 0.4083(2) 0.0449(11) Uani 1 1 d . . . H38A H 0.0995 0.7959 0.4319 0.054 Uiso 1 1 calc R . . C39 C 0.2255(3) 0.7272(3) 0.39139(18) 0.0365(9) Uani 1 1 d . . . H39A H 0.2773 0.7695 0.4033 0.044 Uiso 1 1 calc R . . C40 C 0.4168(3) 0.5211(3) 0.29998(17) 0.0280(8) Uani 1 1 d . . . C41 C 0.3822(4) 0.4995(3) 0.2407(2) 0.0435(10) Uani 1 1 d . . . H41A H 0.3502 0.5459 0.2175 0.052 Uiso 1 1 calc R . . C42 C 0.3947(4) 0.4099(3) 0.2155(2) 0.0536(12) Uani 1 1 d . . . H42A H 0.3707 0.3966 0.1759 0.064 Uiso 1 1 calc R . . C43 C 0.4427(3) 0.3407(3) 0.2495(2) 0.0445(11) Uani 1 1 d . . . H43A H 0.4500 0.2804 0.2332 0.053 Uiso 1 1 calc R . . C44 C 0.4797(4) 0.3612(3) 0.3076(2) 0.0452(11) Uani 1 1 d . . . H44A H 0.5134 0.3150 0.3302 0.054 Uiso 1 1 calc R . . C45 C 0.4667(3) 0.4499(3) 0.3322(2) 0.0374(9) Uani 1 1 d . . . H45A H 0.4919 0.4626 0.3715 0.045 Uiso 1 1 calc R . . C46 C 0.1472(3) 0.1764(3) -0.03347(18) 0.0346(9) Uani 1 1 d . . . C47 C 0.1750(4) 0.2480(3) -0.07889(19) 0.0432(10) Uani 1 1 d . . . H47A H 0.2378 0.2508 -0.1043 0.052 Uiso 1 1 calc R . . C48 C 0.0945(4) 0.3102(3) -0.07802(19) 0.0425(10) Uani 1 1 d . . . H48A H 0.0906 0.3635 -0.1030 0.051 Uiso 1 1 calc R . . C49 C 0.0162(3) 0.2796(3) -0.03200(17) 0.0326(8) Uani 1 1 d . . . C50 C -0.0815(3) 0.3250(3) -0.01527(19) 0.0353(9) Uani 1 1 d . . . C51 C -0.1536(3) 0.3039(3) 0.0344(2) 0.0364(9) Uani 1 1 d . . . C52 C -0.2566(4) 0.3460(3) 0.0480(2) 0.0490(12) Uani 1 1 d . . . H52A H -0.2869 0.3945 0.0258 0.059 Uiso 1 1 calc R . . C53 C -0.3018(4) 0.3021(3) 0.0995(2) 0.0519(12) Uani 1 1 d . . . H53A H -0.3678 0.3156 0.1197 0.062 Uiso 1 1 calc R . . C54 C -0.2284(3) 0.2317(3) 0.1161(2) 0.0383(10) Uani 1 1 d . . . C55 C 0.2056(3) 0.0909(3) -0.02085(18) 0.0353(9) Uani 1 1 d . . . C56 C 0.3146(3) 0.0842(4) -0.0402(2) 0.0463(11) Uani 1 1 d . . . H56A H 0.3490 0.1350 -0.0598 0.056 Uiso 1 1 calc R . . C57 C 0.3698(4) 0.0043(4) -0.0304(2) 0.0513(12) Uani 1 1 d . . . H57A H 0.4418 0.0009 -0.0438 0.062 Uiso 1 1 calc R . . C58 C 0.3217(4) -0.0726(4) -0.0009(2) 0.0555(14) Uani 1 1 d . . . H58A H 0.3613 -0.1266 0.0059 0.067 Uiso 1 1 calc R . . C59 C 0.2125(4) -0.0683(3) 0.0186(2) 0.0447(11) Uani 1 1 d . . . H59A H 0.1786 -0.1192 0.0383 0.054 Uiso 1 1 calc R . . C60 C 0.1567(3) 0.0131(3) 0.00767(19) 0.0359(9) Uani 1 1 d . . . H60A H 0.0841 0.0161 0.0198 0.043 Uiso 1 1 calc R . . C61 C -0.2489(3) 0.1599(3) 0.16458(19) 0.0388(10) Uani 1 1 d . . . C62 C -0.2046(3) 0.0719(3) 0.1592(2) 0.0413(10) Uani 1 1 d . . . H62A H -0.1579 0.0582 0.1250 0.050 Uiso 1 1 calc R . . C63 C -0.2283(4) 0.0034(4) 0.2036(2) 0.0551(13) Uani 1 1 d . . . H63A H -0.1960 -0.0553 0.1993 0.066 Uiso 1 1 calc R . . C64 C -0.2988(4) 0.0205(5) 0.2542(2) 0.0651(15) Uani 1 1 d . . . H64A H -0.3143 -0.0257 0.2841 0.078 Uiso 1 1 calc R . . C65 C -0.3448(4) 0.1060(5) 0.2591(2) 0.0644(16) Uani 1 1 d . . . H65A H -0.3942 0.1178 0.2923 0.077 Uiso 1 1 calc R . . C66 C -0.3210(3) 0.1761(4) 0.2165(2) 0.0547(13) Uani 1 1 d . . . H66A H -0.3526 0.2348 0.2220 0.066 Uiso 1 1 calc R . . C67 C -0.1085(4) 0.4049(3) -0.0571(2) 0.0411(10) Uani 1 1 d . . . C68 C -0.1189(4) 0.4950(3) -0.0330(2) 0.0524(12) Uani 1 1 d . . . H68A H -0.1147 0.5049 0.0098 0.063 Uiso 1 1 calc R . . C69 C -0.1352(5) 0.5697(3) -0.0720(3) 0.0738(19) Uani 1 1 d . . . H69A H -0.1434 0.6298 -0.0553 0.089 Uiso 1 1 calc R . . C70 C -0.1394(5) 0.5557(4) -0.1366(3) 0.082(2) Uani 1 1 d . . . H70A H -0.1440 0.6066 -0.1636 0.099 Uiso 1 1 calc R . . C71 C -0.1366(5) 0.4646(4) -0.1599(3) 0.0679(16) Uani 1 1 d . . . H71A H -0.1458 0.4540 -0.2022 0.081 Uiso 1 1 calc R . . C72 C -0.1203(4) 0.3903(3) -0.1205(2) 0.0505(12) Uani 1 1 d . . . H72A H -0.1172 0.3296 -0.1366 0.061 Uiso 1 1 calc R . . C73 C 0.0826(3) 0.2192(2) 0.22791(16) 0.0268(8) Uani 1 1 d . . . C74 C -0.0180(3) 0.2567(3) 0.2430(2) 0.0422(10) Uani 1 1 d . . . H74A H -0.0757 0.2398 0.2197 0.051 Uiso 1 1 calc R . . C75 C -0.0333(4) 0.3185(3) 0.2921(2) 0.0515(12) Uani 1 1 d . . . H75A H -0.1012 0.3431 0.3017 0.062 Uiso 1 1 calc R . . C76 C 0.0514(4) 0.3440(3) 0.3271(2) 0.0472(11) Uani 1 1 d . . . H76A H 0.0404 0.3853 0.3606 0.057 Uiso 1 1 calc R . . C77 C 0.1526(4) 0.3086(3) 0.3128(2) 0.0431(10) Uani 1 1 d . . . H77A H 0.2100 0.3264 0.3361 0.052 Uiso 1 1 calc R . . C78 C 0.1679(3) 0.2461(3) 0.26299(18) 0.0345(9) Uani 1 1 d . . . H78A H 0.2359 0.2220 0.2531 0.041 Uiso 1 1 calc R . . C79 C 0.0722(3) 0.0221(2) 0.19913(17) 0.0283(8) Uani 1 1 d . . . C80 C 0.0441(3) -0.0528(3) 0.1623(2) 0.0375(9) Uani 1 1 d . . . H80A H 0.0334 -0.0433 0.1200 0.045 Uiso 1 1 calc R . . C81 C 0.0317(4) -0.1418(3) 0.1876(2) 0.0473(11) Uani 1 1 d . . . H81A H 0.0134 -0.1916 0.1621 0.057 Uiso 1 1 calc R . . C82 C 0.0464(3) -0.1567(3) 0.2499(2) 0.0450(11) Uani 1 1 d . . . H82A H 0.0399 -0.2167 0.2668 0.054 Uiso 1 1 calc R . . C83 C 0.0706(4) -0.0830(3) 0.2869(2) 0.0563(13) Uani 1 1 d . . . H83A H 0.0797 -0.0928 0.3293 0.068 Uiso 1 1 calc R . . C84 C 0.0820(4) 0.0069(3) 0.2622(2) 0.0486(12) Uani 1 1 d . . . H84A H 0.0963 0.0569 0.2885 0.058 Uiso 1 1 calc R . . C85 C 0.2421(3) 0.1372(3) 0.14475(17) 0.0274(8) Uani 1 1 d . . . C86 C 0.2839(3) 0.2084(3) 0.10653(19) 0.0362(9) Uani 1 1 d . . . H86A H 0.2377 0.2513 0.0893 0.043 Uiso 1 1 calc R . . C87 C 0.3926(3) 0.2166(3) 0.0937(2) 0.0463(11) Uani 1 1 d . . . H87A H 0.4196 0.2645 0.0679 0.056 Uiso 1 1 calc R . . C88 C 0.4613(3) 0.1531(3) 0.1193(2) 0.0476(12) Uani 1 1 d . . . H88A H 0.5349 0.1589 0.1115 0.057 Uiso 1 1 calc R . . C89 C 0.4215(3) 0.0823(3) 0.1559(2) 0.0471(11) Uani 1 1 d . . . H89A H 0.4681 0.0393 0.1727 0.057 Uiso 1 1 calc R . . C90 C 0.3123(3) 0.0733(3) 0.1688(2) 0.0376(9) Uani 1 1 d . . . H90A H 0.2860 0.0240 0.1937 0.045 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 0.0232(2) 0.0305(2) 0.0248(2) -0.00168(18) 0.00084(17) -0.00113(18) Cu2 0.0226(2) 0.0306(2) 0.0249(2) 0.00145(18) 0.00051(17) 0.00427(18) N1 0.0270(16) 0.0335(17) 0.0318(17) 0.0019(14) -0.0051(13) 0.0000(13) N2 0.0318(17) 0.0367(18) 0.0239(16) 0.0005(13) 0.0020(13) 0.0020(14) N3 0.0325(17) 0.0313(17) 0.0249(16) 0.0013(13) 0.0014(13) 0.0023(13) N4 0.0275(17) 0.0334(17) 0.0355(18) -0.0035(14) -0.0041(13) 0.0066(13) P1 0.0225(5) 0.0275(5) 0.0255(5) -0.0013(4) 0.0005(4) 0.0000(4) P2 0.0217(4) 0.0256(5) 0.0260(5) 0.0018(4) -0.0001(4) 0.0018(4) C1 0.028(2) 0.036(2) 0.036(2) 0.0054(17) -0.0057(16) -0.0022(16) C2 0.027(2) 0.043(2) 0.054(3) 0.008(2) -0.0015(19) -0.0108(18) C3 0.035(2) 0.038(2) 0.047(2) -0.0018(19) -0.0057(19) -0.0008(18) C4 0.032(2) 0.031(2) 0.033(2) 0.0008(16) -0.0114(16) -0.0024(16) C5 0.037(2) 0.034(2) 0.0270(19) -0.0020(16) -0.0063(16) 0.0086(17) C6 0.036(2) 0.041(2) 0.027(2) -0.0059(17) -0.0028(16) 0.0042(18) C7 0.049(3) 0.058(3) 0.031(2) -0.012(2) 0.0085(19) 0.009(2) C8 0.045(3) 0.064(3) 0.039(2) -0.008(2) 0.015(2) -0.003(2) C9 0.030(2) 0.047(2) 0.0266(19) 0.0041(17) 0.0050(16) 0.0060(17) C10 0.0150(17) 0.055(3) 0.032(2) 0.0084(18) -0.0020(15) -0.0023(16) C11 0.036(2) 0.066(3) 0.039(2) 0.007(2) 0.0053(19) -0.008(2) C12 0.051(3) 0.099(4) 0.039(3) -0.007(3) 0.013(2) -0.017(3) C13 0.060(3) 0.096(4) 0.042(3) -0.026(3) 0.014(2) 0.001(3) C14 0.048(3) 0.056(3) 0.055(3) -0.010(2) 0.006(2) 0.002(2) C15 0.031(2) 0.052(3) 0.035(2) 0.0025(19) 0.0087(17) 0.0061(19) C16 0.027(2) 0.044(2) 0.033(2) 0.0131(18) -0.0007(16) 0.0017(17) C17 0.029(2) 0.046(2) 0.039(2) 0.0120(19) -0.0013(17) -0.0004(18) C18 0.046(3) 0.039(2) 0.046(3) 0.013(2) -0.007(2) -0.004(2) C19 0.050(3) 0.049(3) 0.057(3) 0.019(2) -0.014(2) -0.014(2) C20 0.035(2) 0.059(3) 0.063(3) 0.023(2) -0.006(2) -0.016(2) C21 0.035(2) 0.054(3) 0.045(3) 0.013(2) 0.0016(19) 0.008(2) C22 0.042(2) 0.034(2) 0.034(2) -0.0015(17) -0.0044(18) 0.0020(18) C23 0.058(3) 0.037(2) 0.033(2) -0.0019(18) -0.0001(19) 0.014(2) C24 0.067(3) 0.034(2) 0.042(3) -0.0010(19) 0.006(2) 0.011(2) C25 0.087(4) 0.043(3) 0.048(3) -0.015(2) -0.009(3) -0.008(3) C26 0.063(3) 0.057(3) 0.050(3) -0.014(2) -0.023(2) 0.000(3) C27 0.052(3) 0.043(2) 0.043(2) -0.011(2) -0.018(2) 0.010(2) C28 0.0288(19) 0.0272(19) 0.0257(18) -0.0010(15) 0.0030(15) -0.0013(15) C29 0.030(2) 0.046(2) 0.036(2) 0.0037(18) 0.0045(17) -0.0026(18) C30 0.042(3) 0.056(3) 0.045(3) 0.010(2) 0.010(2) -0.009(2) C31 0.058(3) 0.045(3) 0.039(2) 0.015(2) 0.004(2) 0.003(2) C32 0.047(3) 0.044(3) 0.044(3) 0.010(2) -0.004(2) 0.005(2) C33 0.029(2) 0.042(2) 0.041(2) 0.0062(18) -0.0003(17) -0.0008(17) C34 0.0226(18) 0.033(2) 0.0254(18) 0.0058(15) -0.0019(14) 0.0002(15) C35 0.030(2) 0.039(2) 0.042(2) 0.0049(18) -0.0026(17) -0.0023(17) C36 0.031(2) 0.053(3) 0.061(3) 0.020(2) -0.006(2) -0.010(2) C37 0.029(2) 0.065(3) 0.053(3) 0.025(2) 0.012(2) 0.013(2) C38 0.040(2) 0.054(3) 0.040(2) 0.007(2) 0.0061(19) 0.018(2) C39 0.036(2) 0.039(2) 0.034(2) 0.0004(17) -0.0011(17) 0.0039(18) C40 0.0236(18) 0.0284(19) 0.0313(19) -0.0036(15) 0.0044(15) -0.0007(15) C41 0.051(3) 0.038(2) 0.042(2) -0.0083(19) -0.008(2) 0.007(2) C42 0.067(3) 0.046(3) 0.049(3) -0.021(2) -0.009(2) 0.005(2) C43 0.040(2) 0.032(2) 0.060(3) -0.016(2) 0.007(2) 0.0032(18) C44 0.040(2) 0.035(2) 0.060(3) 0.002(2) 0.002(2) 0.0082(19) C45 0.036(2) 0.038(2) 0.038(2) 0.0002(18) -0.0018(18) 0.0033(18) C46 0.032(2) 0.044(2) 0.027(2) -0.0032(17) -0.0010(16) -0.0040(17) C47 0.046(3) 0.052(3) 0.030(2) 0.0001(19) 0.0099(18) -0.011(2) C48 0.057(3) 0.041(2) 0.030(2) 0.0019(18) -0.0009(19) 0.001(2) C49 0.042(2) 0.031(2) 0.0242(19) -0.0014(15) -0.0031(16) -0.0039(17) C50 0.044(2) 0.0253(19) 0.038(2) -0.0044(16) -0.0172(18) 0.0040(17) C51 0.034(2) 0.032(2) 0.044(2) -0.0029(18) -0.0094(18) 0.0064(17) C52 0.036(2) 0.040(2) 0.073(3) -0.005(2) -0.015(2) 0.0169(19) C53 0.034(2) 0.052(3) 0.069(3) -0.002(2) 0.003(2) 0.012(2) C54 0.0228(19) 0.047(2) 0.045(2) -0.0174(19) -0.0034(17) 0.0080(17) C55 0.027(2) 0.048(2) 0.030(2) -0.0121(18) 0.0038(16) 0.0013(18) C56 0.031(2) 0.062(3) 0.045(3) -0.013(2) 0.0061(19) 0.003(2) C57 0.033(2) 0.072(3) 0.048(3) -0.010(2) 0.000(2) 0.011(2) C58 0.057(3) 0.064(3) 0.048(3) -0.023(2) -0.019(2) 0.039(3) C59 0.048(3) 0.043(2) 0.044(3) -0.009(2) -0.009(2) 0.011(2) C60 0.028(2) 0.042(2) 0.038(2) -0.0129(18) -0.0048(17) 0.0083(17) C61 0.025(2) 0.058(3) 0.034(2) -0.0110(19) -0.0025(16) 0.0013(18) C62 0.032(2) 0.052(3) 0.039(2) -0.003(2) 0.0069(18) -0.0040(19) C63 0.045(3) 0.071(3) 0.048(3) 0.010(2) 0.008(2) -0.012(2) C64 0.045(3) 0.102(5) 0.047(3) 0.015(3) 0.007(2) -0.009(3) C65 0.048(3) 0.116(5) 0.028(2) 0.001(3) 0.009(2) -0.010(3) C66 0.031(2) 0.087(4) 0.046(3) -0.022(3) 0.001(2) 0.012(2) C67 0.045(2) 0.031(2) 0.049(3) 0.0047(18) -0.017(2) 0.0008(18) C68 0.064(3) 0.034(2) 0.061(3) -0.002(2) -0.026(3) 0.005(2) C69 0.089(4) 0.034(3) 0.104(5) 0.004(3) -0.056(4) 0.002(3) C70 0.095(5) 0.049(3) 0.108(5) 0.035(3) -0.060(4) -0.014(3) C71 0.089(4) 0.071(4) 0.046(3) 0.014(3) -0.023(3) 0.012(3) C72 0.065(3) 0.045(3) 0.043(3) -0.002(2) -0.019(2) 0.015(2) C73 0.0296(19) 0.0234(18) 0.0273(19) 0.0038(14) 0.0013(15) -0.0009(15) C74 0.034(2) 0.051(3) 0.042(2) -0.009(2) -0.0029(18) 0.0033(19) C75 0.042(3) 0.058(3) 0.053(3) -0.015(2) 0.010(2) 0.012(2) C76 0.059(3) 0.038(2) 0.043(3) -0.009(2) 0.007(2) 0.008(2) C77 0.049(3) 0.039(2) 0.042(2) -0.0081(19) -0.007(2) -0.003(2) C78 0.033(2) 0.032(2) 0.039(2) -0.0025(17) -0.0009(17) 0.0036(16) C79 0.0253(18) 0.0270(19) 0.032(2) 0.0023(15) 0.0041(15) 0.0003(15) C80 0.041(2) 0.035(2) 0.036(2) -0.0006(17) 0.0041(18) -0.0038(18) C81 0.046(3) 0.028(2) 0.067(3) -0.004(2) 0.004(2) -0.0057(19) C82 0.039(2) 0.027(2) 0.069(3) 0.013(2) 0.003(2) -0.0021(18) C83 0.073(4) 0.048(3) 0.048(3) 0.018(2) -0.010(2) -0.011(3) C84 0.074(3) 0.035(2) 0.038(2) 0.0092(19) -0.017(2) -0.012(2) C85 0.0242(18) 0.0305(19) 0.0274(19) -0.0049(15) 0.0005(14) 0.0027(15) C86 0.031(2) 0.041(2) 0.036(2) 0.0045(18) -0.0031(17) -0.0040(17) C87 0.038(2) 0.061(3) 0.038(2) -0.006(2) 0.0064(19) -0.020(2) C88 0.025(2) 0.063(3) 0.054(3) -0.025(2) 0.0030(19) 0.002(2) C89 0.028(2) 0.044(3) 0.069(3) -0.011(2) -0.008(2) 0.0116(19) C90 0.032(2) 0.035(2) 0.046(2) -0.0033(18) -0.0051(18) 0.0048(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 N1 1.966(3) . ? Cu1 N2 1.994(3) . ? Cu1 P1 2.1708(10) . ? Cu2 N4 1.962(3) . ? Cu2 N3 1.994(3) . ? Cu2 P2 2.1650(10) . ? N1 C1 1.331(5) . ? N1 C4 1.406(5) . ? N2 C9 1.356(5) . ? N2 C6 1.396(5) . ? N3 C46 1.340(5) . ? N3 C49 1.401(5) . ? N4 C54 1.350(5) . ? N4 C51 1.382(5) . ? P1 C40 1.818(4) . ? P1 C34 1.826(4) . ? P1 C28 1.833(4) . ? P2 C79 1.828(4) . ? P2 C85 1.834(4) . ? P2 C73 1.839(4) . ? C1 C2 1.434(6) . ? C1 C10 1.451(6) . ? C2 C3 1.356(6) . ? C3 C4 1.425(6) . ? C4 C5 1.407(6) . ? C5 C6 1.387(6) . ? C5 C22 1.509(5) . ? C6 C7 1.443(6) . ? C7 C8 1.342(7) . ? C8 C9 1.416(6) . ? C9 C16 1.461(6) . ? C10 C15 1.395(6) . ? C10 C11 1.405(5) . ? C11 C12 1.368(7) . ? C12 C13 1.390(8) . ? C13 C14 1.388(7) . ? C14 C15 1.378(6) . ? C16 C17 1.392(6) . ? C16 C21 1.417(6) . ? C17 C18 1.387(6) . ? C18 C19 1.383(6) . ? C19 C20 1.373(7) . ? C20 C21 1.363(7) . ? C22 C27 1.375(6) . ? C22 C23 1.392(6) . ? C23 C24 1.363(6) . ? C24 C25 1.397(7) . ? C25 C26 1.338(7) . ? C26 C27 1.384(6) . ? C28 C29 1.380(5) . ? C28 C33 1.395(5) . ? C29 C30 1.401(6) . ? C30 C31 1.366(6) . ? C31 C32 1.387(6) . ? C32 C33 1.374(6) . ? C34 C39 1.398(5) . ? C34 C35 1.395(5) . ? C35 C36 1.393(6) . ? C36 C37 1.381(7) . ? C37 C38 1.366(7) . ? C38 C39 1.379(6) . ? C40 C45 1.391(5) . ? C40 C41 1.394(5) . ? C41 C42 1.391(6) . ? C42 C43 1.380(7) . ? C43 C44 1.378(6) . ? C44 C45 1.375(6) . ? C46 C47 1.438(6) . ? C46 C55 1.453(6) . ? C47 C48 1.340(6) . ? C48 C49 1.418(6) . ? C49 C50 1.410(6) . ? C50 C51 1.387(6) . ? C50 C67 1.497(5) . ? C51 C52 1.435(6) . ? C52 C53 1.361(7) . ? C53 C54 1.417(6) . ? C54 C61 1.468(6) . ? C55 C60 1.390(6) . ? C55 C56 1.405(5) . ? C56 C57 1.353(7) . ? C57 C58 1.385(7) . ? C58 C59 1.407(7) . ? C59 C60 1.379(6) . ? C61 C62 1.373(6) . ? C61 C66 1.410(6) . ? C62 C63 1.383(6) . ? C63 C64 1.379(7) . ? C64 C65 1.349(8) . ? C65 C66 1.373(8) . ? C67 C72 1.385(6) . ? C67 C68 1.387(6) . ? C68 C69 1.372(7) . ? C69 C70 1.397(9) . ? C70 C71 1.390(8) . ? C71 C72 1.373(6) . ? C73 C74 1.387(5) . ? C73 C78 1.388(5) . ? C74 C75 1.374(6) . ? C75 C76 1.376(7) . ? C76 C77 1.380(6) . ? C77 C78 1.392(6) . ? C79 C84 1.376(5) . ? C79 C80 1.382(5) . ? C80 C81 1.383(6) . ? C81 C82 1.370(6) . ? C82 C83 1.356(7) . ? C83 C84 1.389(6) . ? C85 C90 1.382(5) . ? C85 C86 1.387(5) . ? C86 C87 1.376(6) . ? C87 C88 1.380(7) . ? C88 C89 1.354(7) . ? C89 C90 1.383(6) . ? 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 N1 Cu1 N2 95.43(13) . . ? N1 Cu1 P1 138.15(10) . . ? N2 Cu1 P1 122.37(10) . . ? N4 Cu2 N3 95.83(13) . . ? N4 Cu2 P2 133.58(10) . . ? N3 Cu2 P2 127.55(9) . . ? C1 N1 C4 107.2(3) . . ? C1 N1 Cu1 130.4(3) . . ? C4 N1 Cu1 120.7(2) . . ? C9 N2 C6 106.6(3) . . ? C9 N2 Cu1 130.4(3) . . ? C6 N2 Cu1 118.0(2) . . ? C46 N3 C49 106.6(3) . . ? C46 N3 Cu2 129.0(3) . . ? C49 N3 Cu2 116.4(2) . . ? C54 N4 C51 106.7(3) . . ? C54 N4 Cu2 131.4(3) . . ? C51 N4 Cu2 121.0(3) . . ? C40 P1 C34 106.19(17) . . ? C40 P1 C28 102.78(17) . . ? C34 P1 C28 102.03(16) . . ? C40 P1 Cu1 118.88(13) . . ? C34 P1 Cu1 109.63(12) . . ? C28 P1 Cu1 115.66(12) . . ? C79 P2 C85 103.60(16) . . ? C79 P2 C73 103.52(16) . . ? C85 P2 C73 101.69(16) . . ? C79 P2 Cu2 117.52(13) . . ? C85 P2 Cu2 115.14(12) . . ? C73 P2 Cu2 113.47(12) . . ? N1 C1 C2 110.1(4) . . ? N1 C1 C10 121.8(3) . . ? C2 C1 C10 128.0(4) . . ? C3 C2 C1 107.2(4) . . ? C2 C3 C4 107.3(4) . . ? N1 C4 C5 124.1(3) . . ? N1 C4 C3 108.1(3) . . ? C5 C4 C3 127.7(4) . . ? C6 C5 C4 127.8(4) . . ? C6 C5 C22 116.7(3) . . ? C4 C5 C22 115.4(4) . . ? C5 C6 N2 125.0(3) . . ? C5 C6 C7 127.6(4) . . ? N2 C6 C7 107.3(4) . . ? C8 C7 C6 108.5(4) . . ? C7 C8 C9 106.7(4) . . ? N2 C9 C8 110.9(4) . . ? N2 C9 C16 122.9(3) . . ? C8 C9 C16 126.1(4) . . ? C15 C10 C11 117.4(4) . . ? C15 C10 C1 121.9(3) . . ? C11 C10 C1 120.7(4) . . ? C12 C11 C10 120.9(5) . . ? C11 C12 C13 120.9(5) . . ? C12 C13 C14 119.0(5) . . ? C15 C14 C13 120.0(5) . . ? C14 C15 C10 121.7(4) . . ? C17 C16 C21 116.9(4) . . ? C17 C16 C9 121.2(4) . . ? C21 C16 C9 122.0(4) . . ? C18 C17 C16 121.5(4) . . ? C19 C18 C17 120.3(5) . . ? C20 C19 C18 118.9(5) . . ? C21 C20 C19 121.7(4) . . ? C20 C21 C16 120.8(4) . . ? C27 C22 C23 117.2(4) . . ? C27 C22 C5 120.1(4) . . ? C23 C22 C5 122.7(4) . . ? C24 C23 C22 121.8(4) . . ? C23 C24 C25 119.8(4) . . ? C26 C25 C24 118.6(4) . . ? C25 C26 C27 121.9(5) . . ? C22 C27 C26 120.6(4) . . ? C29 C28 C33 118.8(3) . . ? C29 C28 P1 118.3(3) . . ? C33 C28 P1 122.9(3) . . ? C28 C29 C30 120.5(4) . . ? C31 C30 C29 120.2(4) . . ? C30 C31 C32 119.4(4) . . ? C33 C32 C31 120.9(4) . . ? C32 C33 C28 120.3(4) . . ? C39 C34 C35 118.7(4) . . ? C39 C34 P1 116.0(3) . . ? C35 C34 P1 125.3(3) . . ? C36 C35 C34 120.0(4) . . ? C35 C36 C37 120.1(4) . . ? C38 C37 C36 120.1(4) . . ? C37 C38 C39 120.7(4) . . ? C38 C39 C34 120.3(4) . . ? C45 C40 C41 117.1(4) . . ? C45 C40 P1 120.1(3) . . ? C41 C40 P1 122.8(3) . . ? C40 C41 C42 121.4(4) . . ? C43 C42 C41 119.7(4) . . ? C44 C43 C42 119.8(4) . . ? C43 C44 C45 120.0(4) . . ? C44 C45 C40 122.0(4) . . ? N3 C46 C47 109.4(4) . . ? N3 C46 C55 122.5(3) . . ? C47 C46 C55 127.9(4) . . ? C48 C47 C46 107.8(4) . . ? C47 C48 C49 107.2(4) . . ? N3 C49 C50 125.0(3) . . ? N3 C49 C48 108.9(4) . . ? C50 C49 C48 126.1(4) . . ? C51 C50 C49 127.7(4) . . ? C51 C50 C67 117.6(4) . . ? C49 C50 C67 114.7(4) . . ? N4 C51 C50 124.4(4) . . ? N4 C51 C52 108.4(4) . . ? C50 C51 C52 127.1(4) . . ? C53 C52 C51 107.5(4) . . ? C52 C53 C54 106.4(4) . . ? N4 C54 C53 111.0(4) . . ? N4 C54 C61 123.4(3) . . ? C53 C54 C61 125.4(4) . . ? C60 C55 C56 118.1(4) . . ? C60 C55 C46 122.4(3) . . ? C56 C55 C46 119.4(4) . . ? C57 C56 C55 120.3(5) . . ? C56 C57 C58 121.6(4) . . ? C57 C58 C59 119.4(4) . . ? C60 C59 C58 118.5(5) . . ? C59 C60 C55 122.0(4) . . ? C62 C61 C66 116.9(4) . . ? C62 C61 C54 121.5(4) . . ? C66 C61 C54 121.4(4) . . ? C61 C62 C63 121.1(4) . . ? C62 C63 C64 121.1(5) . . ? C65 C64 C63 118.2(5) . . ? C64 C65 C66 122.0(5) . . ? C65 C66 C61 120.6(5) . . ? C72 C67 C68 119.3(4) . . ? C72 C67 C50 120.5(4) . . ? C68 C67 C50 120.2(4) . . ? C69 C68 C67 120.5(5) . . ? C68 C69 C70 120.1(5) . . ? C71 C70 C69 119.0(5) . . ? C72 C71 C70 120.2(5) . . ? C71 C72 C67 120.5(5) . . ? C74 C73 C78 118.7(4) . . ? C74 C73 P2 118.4(3) . . ? C78 C73 P2 123.0(3) . . ? C75 C74 C73 120.8(4) . . ? C76 C75 C74 120.2(4) . . ? C75 C76 C77 120.3(4) . . ? C76 C77 C78 119.3(4) . . ? C73 C78 C77 120.7(4) . . ? C84 C79 C80 118.2(4) . . ? C84 C79 P2 122.9(3) . . ? C80 C79 P2 118.9(3) . . ? C81 C80 C79 120.9(4) . . ? C82 C81 C80 120.1(4) . . ? C83 C82 C81 119.3(4) . . ? C82 C83 C84 121.0(4) . . ? C79 C84 C83 120.2(4) . . ? C90 C85 C86 118.3(4) . . ? C90 C85 P2 124.1(3) . . ? C86 C85 P2 117.5(3) . . ? C87 C86 C85 121.1(4) . . ? C86 C87 C88 119.5(4) . . ? C89 C88 C87 120.0(4) . . ? C88 C89 C90 120.8(4) . . ? C89 C90 C85 120.2(4) . . ? 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 N2 Cu1 N1 C1 171.1(3) . . . . ? P1 Cu1 N1 C1 -33.1(4) . . . . ? N2 Cu1 N1 C4 -25.7(3) . . . . ? P1 Cu1 N1 C4 130.1(2) . . . . ? N1 Cu1 N2 C9 -177.1(3) . . . . ? P1 Cu1 N2 C9 21.7(4) . . . . ? N1 Cu1 N2 C6 31.7(3) . . . . ? P1 Cu1 N2 C6 -129.4(2) . . . . ? N4 Cu2 N3 C46 177.1(3) . . . . ? P2 Cu2 N3 C46 14.8(4) . . . . ? N4 Cu2 N3 C49 32.5(3) . . . . ? P2 Cu2 N3 C49 -129.8(2) . . . . ? N3 Cu2 N4 C54 166.2(4) . . . . ? P2 Cu2 N4 C54 -33.3(4) . . . . ? N3 Cu2 N4 C51 -26.3(3) . . . . ? P2 Cu2 N4 C51 134.3(3) . . . . ? N1 Cu1 P1 C40 98.6(2) . . . . ? N2 Cu1 P1 C40 -110.31(17) . . . . ? N1 Cu1 P1 C34 -139.12(18) . . . . ? N2 Cu1 P1 C34 12.02(17) . . . . ? N1 Cu1 P1 C28 -24.5(2) . . . . ? N2 Cu1 P1 C28 126.65(17) . . . . ? N4 Cu2 P2 C79 87.74(19) . . . . ? N3 Cu2 P2 C79 -116.96(17) . . . . ? N4 Cu2 P2 C85 -149.76(18) . . . . ? N3 Cu2 P2 C85 5.54(18) . . . . ? N4 Cu2 P2 C73 -33.16(19) . . . . ? N3 Cu2 P2 C73 122.14(17) . . . . ? C4 N1 C1 C2 -1.4(4) . . . . ? Cu1 N1 C1 C2 163.6(3) . . . . ? C4 N1 C1 C10 175.9(3) . . . . ? Cu1 N1 C1 C10 -19.2(5) . . . . ? N1 C1 C2 C3 1.2(5) . . . . ? C10 C1 C2 C3 -175.8(4) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C1 N1 C4 C5 179.9(4) . . . . ? Cu1 N1 C4 C5 13.2(5) . . . . ? C1 N1 C4 C3 1.0(4) . . . . ? Cu1 N1 C4 C3 -165.7(3) . . . . ? C2 C3 C4 N1 -0.3(4) . . . . ? C2 C3 C4 C5 -179.1(4) . . . . ? N1 C4 C5 C6 1.9(6) . . . . ? C3 C4 C5 C6 -179.4(4) . . . . ? N1 C4 C5 C22 178.0(3) . . . . ? C3 C4 C5 C22 -3.4(6) . . . . ? C4 C5 C6 N2 6.3(6) . . . . ? C22 C5 C6 N2 -169.7(3) . . . . ? C4 C5 C6 C7 -178.4(4) . . . . ? C22 C5 C6 C7 5.6(6) . . . . ? C9 N2 C6 C5 175.6(4) . . . . ? Cu1 N2 C6 C5 -26.9(5) . . . . ? C9 N2 C6 C7 -0.5(4) . . . . ? Cu1 N2 C6 C7 157.0(3) . . . . ? C5 C6 C7 C8 -176.6(4) . . . . ? N2 C6 C7 C8 -0.6(5) . . . . ? C6 C7 C8 C9 1.4(5) . . . . ? C6 N2 C9 C8 1.4(4) . . . . ? Cu1 N2 C9 C8 -152.2(3) . . . . ? C6 N2 C9 C16 -174.1(3) . . . . ? Cu1 N2 C9 C16 32.3(5) . . . . ? C7 C8 C9 N2 -1.8(5) . . . . ? C7 C8 C9 C16 173.5(4) . . . . ? N1 C1 C10 C15 -31.1(6) . . . . ? C2 C1 C10 C15 145.5(4) . . . . ? N1 C1 C10 C11 149.1(4) . . . . ? C2 C1 C10 C11 -34.2(6) . . . . ? C15 C10 C11 C12 -0.1(6) . . . . ? C1 C10 C11 C12 179.7(4) . . . . ? C10 C11 C12 C13 1.2(8) . . . . ? C11 C12 C13 C14 -1.3(9) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C13 C14 C15 C10 0.9(7) . . . . ? C11 C10 C15 C14 -0.9(6) . . . . ? C1 C10 C15 C14 179.3(4) . . . . ? N2 C9 C16 C17 20.7(6) . . . . ? C8 C9 C16 C17 -154.1(4) . . . . ? N2 C9 C16 C21 -161.0(4) . . . . ? C8 C9 C16 C21 24.2(6) . . . . ? C21 C16 C17 C18 -0.7(6) . . . . ? C9 C16 C17 C18 177.6(4) . . . . ? C16 C17 C18 C19 -0.2(6) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 0.9(7) . . . . ? C19 C20 C21 C16 -1.9(7) . . . . ? C17 C16 C21 C20 1.7(6) . . . . ? C9 C16 C21 C20 -176.6(4) . . . . ? C6 C5 C22 C27 109.0(5) . . . . ? C4 C5 C22 C27 -67.5(5) . . . . ? C6 C5 C22 C23 -69.9(5) . . . . ? C4 C5 C22 C23 113.6(5) . . . . ? C27 C22 C23 C24 1.3(7) . . . . ? C5 C22 C23 C24 -179.7(4) . . . . ? C22 C23 C24 C25 0.4(7) . . . . ? C23 C24 C25 C26 -1.6(8) . . . . ? C24 C25 C26 C27 1.1(8) . . . . ? C23 C22 C27 C26 -1.8(7) . . . . ? C5 C22 C27 C26 179.2(4) . . . . ? C25 C26 C27 C22 0.6(8) . . . . ? C40 P1 C28 C29 -88.2(3) . . . . ? C34 P1 C28 C29 161.9(3) . . . . ? Cu1 P1 C28 C29 43.0(3) . . . . ? C40 P1 C28 C33 90.8(3) . . . . ? C34 P1 C28 C33 -19.2(4) . . . . ? Cu1 P1 C28 C33 -138.1(3) . . . . ? C33 C28 C29 C30 -1.0(6) . . . . ? P1 C28 C29 C30 178.0(3) . . . . ? C28 C29 C30 C31 0.8(7) . . . . ? C29 C30 C31 C32 0.3(7) . . . . ? C30 C31 C32 C33 -1.2(7) . . . . ? C31 C32 C33 C28 1.1(7) . . . . ? C29 C28 C33 C32 0.0(6) . . . . ? P1 C28 C33 C32 -178.9(3) . . . . ? C40 P1 C34 C39 172.6(3) . . . . ? C28 P1 C34 C39 -80.1(3) . . . . ? Cu1 P1 C34 C39 43.0(3) . . . . ? C40 P1 C34 C35 -8.2(4) . . . . ? C28 P1 C34 C35 99.1(3) . . . . ? Cu1 P1 C34 C35 -137.8(3) . . . . ? C39 C34 C35 C36 1.5(6) . . . . ? P1 C34 C35 C36 -177.6(3) . . . . ? C34 C35 C36 C37 -1.5(6) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C36 C37 C38 C39 0.5(6) . . . . ? C37 C38 C39 C34 -0.4(6) . . . . ? C35 C34 C39 C38 -0.6(6) . . . . ? P1 C34 C39 C38 178.6(3) . . . . ? C34 P1 C40 C45 -108.4(3) . . . . ? C28 P1 C40 C45 144.8(3) . . . . ? Cu1 P1 C40 C45 15.6(4) . . . . ? C34 P1 C40 C41 71.5(4) . . . . ? C28 P1 C40 C41 -35.3(4) . . . . ? Cu1 P1 C40 C41 -164.5(3) . . . . ? C45 C40 C41 C42 1.6(6) . . . . ? P1 C40 C41 C42 -178.4(4) . . . . ? C40 C41 C42 C43 -0.3(7) . . . . ? C41 C42 C43 C44 -1.2(7) . . . . ? C42 C43 C44 C45 1.4(7) . . . . ? C43 C44 C45 C40 -0.1(7) . . . . ? C41 C40 C45 C44 -1.3(6) . . . . ? P1 C40 C45 C44 178.6(3) . . . . ? C49 N3 C46 C47 1.6(4) . . . . ? Cu2 N3 C46 C47 -145.7(3) . . . . ? C49 N3 C46 C55 -175.2(3) . . . . ? Cu2 N3 C46 C55 37.6(5) . . . . ? N3 C46 C47 C48 -1.5(5) . . . . ? C55 C46 C47 C48 175.1(4) . . . . ? C46 C47 C48 C49 0.7(5) . . . . ? C46 N3 C49 C50 179.7(4) . . . . ? Cu2 N3 C49 C50 -28.3(5) . . . . ? C46 N3 C49 C48 -1.1(4) . . . . ? Cu2 N3 C49 C48 150.9(3) . . . . ? C47 C48 C49 N3 0.2(5) . . . . ? C47 C48 C49 C50 179.3(4) . . . . ? N3 C49 C50 C51 7.6(6) . . . . ? C48 C49 C50 C51 -171.4(4) . . . . ? N3 C49 C50 C67 -172.1(3) . . . . ? C48 C49 C50 C67 9.0(6) . . . . ? C54 N4 C51 C50 -176.6(4) . . . . ? Cu2 N4 C51 C50 13.1(5) . . . . ? C54 N4 C51 C52 0.5(4) . . . . ? Cu2 N4 C51 C52 -169.8(3) . . . . ? C49 C50 C51 N4 1.8(7) . . . . ? C67 C50 C51 N4 -178.5(4) . . . . ? C49 C50 C51 C52 -174.8(4) . . . . ? C67 C50 C51 C52 4.9(6) . . . . ? N4 C51 C52 C53 0.8(5) . . . . ? C50 C51 C52 C53 177.8(4) . . . . ? C51 C52 C53 C54 -1.7(5) . . . . ? C51 N4 C54 C53 -1.5(5) . . . . ? Cu2 N4 C54 C53 167.4(3) . . . . ? C51 N4 C54 C61 173.4(4) . . . . ? Cu2 N4 C54 C61 -17.7(6) . . . . ? C52 C53 C54 N4 2.0(5) . . . . ? C52 C53 C54 C61 -172.8(4) . . . . ? N3 C46 C55 C60 18.3(6) . . . . ? C47 C46 C55 C60 -157.9(4) . . . . ? N3 C46 C55 C56 -164.3(4) . . . . ? C47 C46 C55 C56 19.5(6) . . . . ? C60 C55 C56 C57 -0.7(6) . . . . ? C46 C55 C56 C57 -178.2(4) . . . . ? C55 C56 C57 C58 -0.5(7) . . . . ? C56 C57 C58 C59 0.9(7) . . . . ? C57 C58 C59 C60 -0.2(6) . . . . ? C58 C59 C60 C55 -1.1(6) . . . . ? C56 C55 C60 C59 1.5(6) . . . . ? C46 C55 C60 C59 179.0(4) . . . . ? N4 C54 C61 C62 -26.7(6) . . . . ? C53 C54 C61 C62 147.5(4) . . . . ? N4 C54 C61 C66 157.9(4) . . . . ? C53 C54 C61 C66 -27.9(6) . . . . ? C66 C61 C62 C63 -1.4(6) . . . . ? C54 C61 C62 C63 -177.0(4) . . . . ? C61 C62 C63 C64 1.4(7) . . . . ? C62 C63 C64 C65 0.3(8) . . . . ? C63 C64 C65 C66 -1.9(8) . . . . ? C64 C65 C66 C61 1.8(8) . . . . ? C62 C61 C66 C65 -0.2(6) . . . . ? C54 C61 C66 C65 175.4(4) . . . . ? C51 C50 C67 C72 -119.8(5) . . . . ? C49 C50 C67 C72 59.9(6) . . . . ? C51 C50 C67 C68 62.1(6) . . . . ? C49 C50 C67 C68 -118.2(5) . . . . ? C72 C67 C68 C69 -3.3(8) . . . . ? C50 C67 C68 C69 174.8(5) . . . . ? C67 C68 C69 C70 -1.3(9) . . . . ? C68 C69 C70 C71 5.8(10) . . . . ? C69 C70 C71 C72 -5.8(10) . . . . ? C70 C71 C72 C67 1.2(9) . . . . ? C68 C67 C72 C71 3.4(8) . . . . ? C50 C67 C72 C71 -174.8(5) . . . . ? C79 P2 C73 C74 -90.1(3) . . . . ? C85 P2 C73 C74 162.6(3) . . . . ? Cu2 P2 C73 C74 38.3(3) . . . . ? C79 P2 C73 C78 90.0(3) . . . . ? C85 P2 C73 C78 -17.3(3) . . . . ? Cu2 P2 C73 C78 -141.5(3) . . . . ? C78 C73 C74 C75 -0.6(6) . . . . ? P2 C73 C74 C75 179.5(4) . . . . ? C73 C74 C75 C76 -0.1(7) . . . . ? C74 C75 C76 C77 0.7(7) . . . . ? C75 C76 C77 C78 -0.7(7) . . . . ? C74 C73 C78 C77 0.6(6) . . . . ? P2 C73 C78 C77 -179.5(3) . . . . ? C76 C77 C78 C73 0.0(6) . . . . ? C85 P2 C79 C84 85.2(4) . . . . ? C73 P2 C79 C84 -20.6(4) . . . . ? Cu2 P2 C79 C84 -146.6(3) . . . . ? C85 P2 C79 C80 -93.8(3) . . . . ? C73 P2 C79 C80 160.3(3) . . . . ? Cu2 P2 C79 C80 34.4(3) . . . . ? C84 C79 C80 C81 -3.4(6) . . . . ? P2 C79 C80 C81 175.7(3) . . . . ? C79 C80 C81 C82 0.6(7) . . . . ? C80 C81 C82 C83 1.6(7) . . . . ? C81 C82 C83 C84 -0.8(8) . . . . ? C80 C79 C84 C83 4.1(7) . . . . ? P2 C79 C84 C83 -174.9(4) . . . . ? C82 C83 C84 C79 -2.1(8) . . . . ? C79 P2 C85 C90 -12.7(4) . . . . ? C73 P2 C85 C90 94.5(3) . . . . ? Cu2 P2 C85 C90 -142.4(3) . . . . ? C79 P2 C85 C86 169.2(3) . . . . ? C73 P2 C85 C86 -83.6(3) . . . . ? Cu2 P2 C85 C86 39.5(3) . . . . ? C90 C85 C86 C87 -1.2(6) . . . . ? P2 C85 C86 C87 177.0(3) . . . . ? C85 C86 C87 C88 -0.2(6) . . . . ? C86 C87 C88 C89 1.2(7) . . . . ? C87 C88 C89 C90 -0.8(7) . . . . ? C88 C89 C90 C85 -0.6(7) . . . . ? C86 C85 C90 C89 1.6(6) . . . . ? P2 C85 C90 C89 -176.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.12 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.779 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.073 data_s226 _database_code_depnum_ccdc_archive 'CCDC 871235' #TrackingRef 's226-5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Br2 Cu N2 O P2' _chemical_formula_weight 997.18 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' P P 0.1023 0.0942 '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 11.374(3) _cell_length_b 11.686(3) _cell_length_c 18.175(4) _cell_angle_alpha 80.042(3) _cell_angle_beta 85.355(4) _cell_angle_gamma 75.425(4) _cell_volume 2301.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3210 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 23.68 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 2.316 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5414 _exptl_absorpt_correction_T_max 0.8048 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12936 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.03 _reflns_number_total 8817 _reflns_number_gt 6067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data set was corrected using the program SQUEEZE. There is one seriously disordered MeOH solvate molecule estimated based on the elemental analyses and 1H NMR spectra. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 180 40 ' ' _platon_squeeze_details ; ; _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^)+(0.0450P)^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 8817 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.32839(3) 0.32329(3) 0.28748(2) 0.03816(11) Uani 1 1 d . . . N1 N 0.2326(2) 0.1994(2) 0.33522(14) 0.0388(6) Uani 1 1 d . . . N2 N 0.3170(2) 0.3943(2) 0.38472(13) 0.0387(6) Uani 1 1 d . . . P1 P 0.52832(7) 0.22612(7) 0.27310(5) 0.0407(2) Uani 1 1 d . . . P2 P 0.22040(7) 0.44825(7) 0.19262(4) 0.03722(19) Uani 1 1 d . . . Br1 Br 0.23604(4) 0.09167(3) 0.20817(2) 0.06677(13) Uani 1 1 d . . . Br2 Br 0.48017(4) 0.54024(4) 0.33819(2) 0.06655(13) Uani 1 1 d . . . C1 C 0.1929(3) 0.1197(3) 0.30668(18) 0.0454(8) Uani 1 1 d . . . C2 C 0.1156(3) 0.0633(3) 0.3549(2) 0.0624(10) Uani 1 1 d . . . H2A H 0.0785 0.0052 0.3453 0.075 Uiso 1 1 calc R . . C3 C 0.1057(3) 0.1111(3) 0.4189(2) 0.0574(9) Uani 1 1 d . . . H3A H 0.0602 0.0915 0.4620 0.069 Uiso 1 1 calc R . . C4 C 0.1777(3) 0.1966(3) 0.40779(18) 0.0414(8) Uani 1 1 d . . . C5 C 0.1870(3) 0.2698(3) 0.45851(17) 0.0409(7) Uani 1 1 d . . . C6 C 0.2512(3) 0.3598(3) 0.44957(17) 0.0399(7) Uani 1 1 d . . . C7 C 0.2682(3) 0.4224(3) 0.50664(19) 0.0535(9) Uani 1 1 d . . . H7A H 0.2334 0.4161 0.5548 0.064 Uiso 1 1 calc R . . C8 C 0.3449(3) 0.4937(3) 0.47790(18) 0.0544(9) Uani 1 1 d . . . H8A H 0.3734 0.5450 0.5018 0.065 Uiso 1 1 calc R . . C9 C 0.3709(3) 0.4718(3) 0.40395(18) 0.0455(8) Uani 1 1 d . . . C10 C 0.1224(3) 0.2481(3) 0.53222(18) 0.0460(8) Uani 1 1 d . . . C11 C 0.1715(3) 0.1533(3) 0.5862(2) 0.0667(11) Uani 1 1 d . . . H11A H 0.2459 0.1020 0.5763 0.080 Uiso 1 1 calc R . . C12 C 0.1118(4) 0.1333(4) 0.6552(2) 0.0786(12) Uani 1 1 d . . . H12A H 0.1467 0.0697 0.6913 0.094 Uiso 1 1 calc R . . C13 C 0.0020(4) 0.2071(4) 0.6698(2) 0.0721(12) Uani 1 1 d . . . H13A H -0.0391 0.1931 0.7156 0.087 Uiso 1 1 calc R . . C14 C -0.0471(4) 0.3007(4) 0.6176(3) 0.0786(13) Uani 1 1 d . . . H14A H -0.1215 0.3517 0.6280 0.094 Uiso 1 1 calc R . . C15 C 0.0123(3) 0.3212(3) 0.5490(2) 0.0659(11) Uani 1 1 d . . . H15A H -0.0230 0.3857 0.5136 0.079 Uiso 1 1 calc R . . C16 C 0.5555(3) 0.0778(3) 0.24545(19) 0.0457(8) Uani 1 1 d . . . C17 C 0.5417(3) -0.0202(3) 0.2965(2) 0.0656(10) Uani 1 1 d . . . H17A H 0.5279 -0.0125 0.3467 0.079 Uiso 1 1 calc R . . C18 C 0.5479(4) -0.1296(3) 0.2753(3) 0.0819(13) Uani 1 1 d . . . H18A H 0.5390 -0.1945 0.3111 0.098 Uiso 1 1 calc R . . C19 C 0.5671(4) -0.1420(4) 0.2022(3) 0.0822(14) Uani 1 1 d . . . H19A H 0.5709 -0.2153 0.1876 0.099 Uiso 1 1 calc R . . C20 C 0.5810(4) -0.0459(4) 0.1495(3) 0.0796(13) Uani 1 1 d . . . H20A H 0.5942 -0.0542 0.0994 0.096 Uiso 1 1 calc R . . C21 C 0.5754(3) 0.0627(3) 0.1713(2) 0.0654(11) Uani 1 1 d . . . H21A H 0.5852 0.1271 0.1354 0.078 Uiso 1 1 calc R . . C22 C 0.5991(3) 0.1973(3) 0.36348(19) 0.0468(8) Uani 1 1 d . . . C23 C 0.5293(3) 0.1639(3) 0.4264(2) 0.0575(9) Uani 1 1 d . . . H23A H 0.4528 0.1524 0.4207 0.069 Uiso 1 1 calc R . . C24 C 0.5723(5) 0.1477(4) 0.4967(2) 0.0805(13) Uani 1 1 d . . . H24A H 0.5254 0.1236 0.5380 0.097 Uiso 1 1 calc R . . C25 C 0.6835(6) 0.1668(4) 0.5069(3) 0.0945(16) Uani 1 1 d . . . H25A H 0.7113 0.1569 0.5549 0.113 Uiso 1 1 calc R . . C26 C 0.7534(4) 0.2004(4) 0.4461(3) 0.0879(14) Uani 1 1 d . . . H26A H 0.8291 0.2130 0.4527 0.105 Uiso 1 1 calc R . . C27 C 0.7110(3) 0.2158(3) 0.3744(2) 0.0644(10) Uani 1 1 d . . . H27A H 0.7589 0.2389 0.3334 0.077 Uiso 1 1 calc R . . C28 C 0.6294(3) 0.2969(3) 0.20736(18) 0.0449(8) Uani 1 1 d . . . C29 C 0.7492(3) 0.2399(3) 0.1909(2) 0.0631(10) Uani 1 1 d . . . H29A H 0.7809 0.1612 0.2128 0.076 Uiso 1 1 calc R . . C30 C 0.8212(4) 0.2999(4) 0.1422(2) 0.0739(12) Uani 1 1 d . . . H30A H 0.9013 0.2614 0.1316 0.089 Uiso 1 1 calc R . . C31 C 0.7755(4) 0.4157(4) 0.1091(2) 0.0702(11) Uani 1 1 d . . . H31A H 0.8246 0.4556 0.0764 0.084 Uiso 1 1 calc R . . C32 C 0.6583(4) 0.4720(3) 0.1242(2) 0.0643(10) Uani 1 1 d . . . H32A H 0.6273 0.5504 0.1016 0.077 Uiso 1 1 calc R . . C33 C 0.5849(3) 0.4131(3) 0.17315(18) 0.0489(8) Uani 1 1 d . . . H33A H 0.5048 0.4523 0.1830 0.059 Uiso 1 1 calc R . . C34 C 0.2167(3) 0.3788(3) 0.11029(17) 0.0403(7) Uani 1 1 d . . . C35 C 0.3265(3) 0.3151(3) 0.08160(19) 0.0534(9) Uani 1 1 d . . . H35A H 0.3989 0.3129 0.1028 0.064 Uiso 1 1 calc R . . C36 C 0.3290(4) 0.2554(3) 0.0223(2) 0.0642(10) Uani 1 1 d . . . H36A H 0.4029 0.2146 0.0031 0.077 Uiso 1 1 calc R . . C37 C 0.2214(4) 0.2561(3) -0.0087(2) 0.0673(11) Uani 1 1 d . . . H37A H 0.2224 0.2136 -0.0476 0.081 Uiso 1 1 calc R . . C38 C 0.1139(4) 0.3200(3) 0.0184(2) 0.0648(10) Uani 1 1 d . . . H38A H 0.0416 0.3220 -0.0028 0.078 Uiso 1 1 calc R . . C39 C 0.1116(3) 0.3819(3) 0.07718(19) 0.0513(9) Uani 1 1 d . . . H39A H 0.0378 0.4261 0.0944 0.062 Uiso 1 1 calc R . . C40 C 0.0589(3) 0.5053(3) 0.21896(17) 0.0410(7) Uani 1 1 d . . . C41 C -0.0105(3) 0.6146(3) 0.18655(19) 0.0550(9) Uani 1 1 d . . . H41A H 0.0235 0.6620 0.1486 0.066 Uiso 1 1 calc R . . C42 C -0.1304(3) 0.6537(3) 0.2104(2) 0.0628(10) Uani 1 1 d . . . H42A H -0.1767 0.7272 0.1882 0.075 Uiso 1 1 calc R . . C43 C -0.1813(3) 0.5851(4) 0.2664(2) 0.0641(10) Uani 1 1 d . . . H43A H -0.2617 0.6124 0.2825 0.077 Uiso 1 1 calc R . . C44 C -0.1142(3) 0.4767(4) 0.2986(2) 0.0656(11) Uani 1 1 d . . . H44A H -0.1489 0.4296 0.3364 0.079 Uiso 1 1 calc R . . C45 C 0.0058(3) 0.4366(3) 0.2750(2) 0.0552(9) Uani 1 1 d . . . H45A H 0.0512 0.3626 0.2972 0.066 Uiso 1 1 calc R . . C46 C 0.2639(3) 0.5868(3) 0.15124(18) 0.0413(8) Uani 1 1 d . . . C47 C 0.2929(4) 0.6161(3) 0.0765(2) 0.0656(11) Uani 1 1 d . . . H47A H 0.2917 0.5631 0.0440 0.079 Uiso 1 1 calc R . . C48 C 0.3240(4) 0.7237(4) 0.0489(3) 0.0920(15) Uani 1 1 d . . . H48A H 0.3442 0.7422 -0.0016 0.110 Uiso 1 1 calc R . . C49 C 0.3247(4) 0.8020(4) 0.0965(3) 0.0945(16) Uani 1 1 d . . . H49A H 0.3437 0.8748 0.0783 0.113 Uiso 1 1 calc R . . C50 C 0.2977(4) 0.7733(4) 0.1704(3) 0.0770(12) Uani 1 1 d . . . H50A H 0.3001 0.8261 0.2028 0.092 Uiso 1 1 calc R . . C51 C 0.2668(3) 0.6675(3) 0.1978(2) 0.0559(9) Uani 1 1 d . . . H51A H 0.2476 0.6499 0.2486 0.067 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 Cu 0.0390(2) 0.0392(2) 0.0384(2) -0.00852(17) -0.00046(16) -0.01223(17) N1 0.0374(14) 0.0344(14) 0.0469(16) -0.0096(12) -0.0004(12) -0.0112(11) N2 0.0425(15) 0.0398(14) 0.0377(15) -0.0101(12) -0.0022(12) -0.0142(12) P1 0.0368(5) 0.0408(5) 0.0431(5) -0.0039(4) 0.0019(4) -0.0094(4) P2 0.0363(5) 0.0397(4) 0.0366(5) -0.0107(4) -0.0001(3) -0.0082(4) Br1 0.0917(3) 0.0548(2) 0.0636(3) -0.0238(2) -0.0020(2) -0.0263(2) Br2 0.0792(3) 0.0742(3) 0.0611(3) -0.0106(2) 0.0012(2) -0.0471(2) C1 0.048(2) 0.0390(18) 0.050(2) -0.0081(16) -0.0029(16) -0.0120(15) C2 0.071(3) 0.053(2) 0.077(3) -0.011(2) -0.003(2) -0.0390(19) C3 0.058(2) 0.055(2) 0.063(3) -0.0045(19) 0.0093(18) -0.0279(18) C4 0.0390(18) 0.0386(17) 0.046(2) -0.0026(15) 0.0012(15) -0.0124(14) C5 0.0341(17) 0.0395(17) 0.0442(19) -0.0042(15) 0.0012(14) -0.0027(14) C6 0.0420(18) 0.0402(17) 0.0364(18) -0.0067(14) -0.0001(14) -0.0077(14) C7 0.059(2) 0.066(2) 0.039(2) -0.0185(18) 0.0039(16) -0.0177(19) C8 0.065(2) 0.061(2) 0.045(2) -0.0228(18) -0.0035(18) -0.0204(19) C9 0.050(2) 0.0461(19) 0.044(2) -0.0104(16) -0.0013(15) -0.0162(16) C10 0.043(2) 0.049(2) 0.047(2) -0.0089(17) 0.0057(16) -0.0150(16) C11 0.057(2) 0.072(3) 0.059(3) 0.003(2) 0.0081(19) -0.006(2) C12 0.095(4) 0.079(3) 0.055(3) 0.009(2) 0.002(2) -0.024(3) C13 0.078(3) 0.088(3) 0.059(3) -0.020(2) 0.024(2) -0.038(3) C14 0.065(3) 0.089(3) 0.075(3) -0.020(3) 0.023(2) -0.007(2) C15 0.059(3) 0.068(2) 0.061(3) -0.007(2) 0.008(2) -0.003(2) C16 0.0381(19) 0.0401(18) 0.056(2) -0.0094(17) 0.0009(16) -0.0037(14) C17 0.078(3) 0.048(2) 0.071(3) -0.007(2) -0.005(2) -0.016(2) C18 0.088(3) 0.044(2) 0.113(4) -0.008(3) -0.016(3) -0.013(2) C19 0.060(3) 0.057(3) 0.135(5) -0.046(3) -0.017(3) 0.001(2) C20 0.064(3) 0.078(3) 0.100(4) -0.049(3) 0.000(2) -0.001(2) C21 0.062(3) 0.061(2) 0.074(3) -0.027(2) 0.007(2) -0.0079(19) C22 0.047(2) 0.0395(18) 0.051(2) -0.0028(16) -0.0062(16) -0.0055(15) C23 0.064(2) 0.057(2) 0.047(2) -0.0052(18) -0.0046(19) -0.0074(18) C24 0.101(4) 0.078(3) 0.050(3) 0.005(2) -0.005(2) -0.007(3) C25 0.120(5) 0.093(4) 0.058(3) -0.007(3) -0.036(3) 0.004(3) C26 0.080(3) 0.094(3) 0.093(4) -0.022(3) -0.036(3) -0.013(3) C27 0.053(2) 0.071(3) 0.068(3) -0.009(2) -0.012(2) -0.012(2) C28 0.0398(19) 0.051(2) 0.043(2) -0.0042(16) 0.0019(15) -0.0120(15) C29 0.052(2) 0.063(2) 0.070(3) -0.007(2) 0.0132(19) -0.0127(19) C30 0.047(2) 0.099(3) 0.075(3) -0.015(3) 0.016(2) -0.023(2) C31 0.064(3) 0.098(3) 0.056(3) 0.002(2) 0.007(2) -0.045(2) C32 0.074(3) 0.066(2) 0.054(2) 0.0084(19) -0.005(2) -0.030(2) C33 0.0430(19) 0.057(2) 0.047(2) -0.0041(17) -0.0009(16) -0.0154(16) C34 0.0436(19) 0.0405(17) 0.0378(18) -0.0084(14) 0.0006(14) -0.0112(15) C35 0.047(2) 0.058(2) 0.057(2) -0.0219(19) -0.0009(17) -0.0079(17) C36 0.064(3) 0.069(2) 0.057(2) -0.026(2) 0.012(2) -0.005(2) C37 0.087(3) 0.072(3) 0.053(2) -0.030(2) 0.003(2) -0.026(2) C38 0.061(3) 0.084(3) 0.060(2) -0.026(2) -0.015(2) -0.023(2) C39 0.042(2) 0.061(2) 0.054(2) -0.0222(18) -0.0011(16) -0.0101(17) C40 0.0372(18) 0.0482(19) 0.0369(18) -0.0140(15) -0.0042(14) -0.0032(15) C41 0.047(2) 0.061(2) 0.052(2) -0.0088(18) -0.0007(17) -0.0037(18) C42 0.042(2) 0.066(2) 0.067(3) -0.001(2) -0.0075(19) 0.0074(18) C43 0.037(2) 0.075(3) 0.077(3) -0.023(2) 0.0008(19) 0.0008(19) C44 0.049(2) 0.074(3) 0.070(3) -0.008(2) 0.0150(19) -0.014(2) C45 0.045(2) 0.051(2) 0.061(2) -0.0014(18) 0.0050(17) -0.0040(16) C46 0.0356(18) 0.0413(18) 0.048(2) -0.0086(16) -0.0061(15) -0.0082(14) C47 0.094(3) 0.059(2) 0.051(2) -0.0070(19) 0.001(2) -0.033(2) C48 0.125(4) 0.079(3) 0.075(3) 0.008(3) 0.011(3) -0.050(3) C49 0.100(4) 0.052(3) 0.136(5) 0.003(3) -0.009(3) -0.037(3) C50 0.084(3) 0.057(3) 0.100(4) -0.024(3) -0.007(3) -0.025(2) C51 0.056(2) 0.052(2) 0.063(2) -0.0176(19) -0.0011(18) -0.0131(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 Cu N1 2.059(2) . ? Cu N2 2.061(2) . ? Cu P2 2.2765(10) . ? Cu P1 2.2882(10) . ? N1 C1 1.326(4) . ? N1 C4 1.412(4) . ? N2 C9 1.319(4) . ? N2 C6 1.399(4) . ? P1 C22 1.829(3) . ? P1 C28 1.830(3) . ? P1 C16 1.832(3) . ? P2 C34 1.829(3) . ? P2 C46 1.831(3) . ? P2 C40 1.844(3) . ? Br1 C1 1.879(3) . ? Br2 C9 1.882(3) . ? C1 C2 1.394(4) . ? C2 C3 1.360(5) . ? C3 C4 1.424(4) . ? C4 C5 1.388(4) . ? C5 C6 1.406(4) . ? C5 C10 1.488(4) . ? C6 C7 1.419(4) . ? C7 C8 1.368(5) . ? C8 C9 1.406(4) . ? C10 C15 1.372(4) . ? C10 C11 1.380(5) . ? C11 C12 1.388(5) . ? C12 C13 1.364(6) . ? C13 C14 1.352(5) . ? C14 C15 1.382(5) . ? C16 C17 1.377(4) . ? C16 C21 1.383(5) . ? C17 C18 1.381(5) . ? C18 C19 1.357(6) . ? C19 C20 1.376(6) . ? C20 C21 1.378(5) . ? C22 C27 1.379(5) . ? C22 C23 1.395(4) . ? C23 C24 1.370(5) . ? C24 C25 1.370(6) . ? C25 C26 1.368(6) . ? C26 C27 1.393(5) . ? C28 C33 1.378(4) . ? C28 C29 1.392(4) . ? C29 C30 1.379(5) . ? C30 C31 1.370(5) . ? C31 C32 1.359(5) . ? C32 C33 1.385(4) . ? C34 C39 1.371(4) . ? C34 C35 1.395(4) . ? C35 C36 1.375(5) . ? C36 C37 1.386(5) . ? C37 C38 1.366(5) . ? C38 C39 1.385(5) . ? C40 C45 1.381(4) . ? C40 C41 1.382(4) . ? C41 C42 1.385(4) . ? C42 C43 1.366(5) . ? C43 C44 1.365(5) . ? C44 C45 1.385(5) . ? C46 C47 1.376(4) . ? C46 C51 1.380(4) . ? C47 C48 1.391(5) . ? C48 C49 1.365(6) . ? C49 C50 1.356(6) . ? C50 C51 1.370(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 N1 Cu N2 92.57(10) . . ? N1 Cu P2 108.77(7) . . ? N2 Cu P2 114.41(7) . . ? N1 Cu P1 108.55(7) . . ? N2 Cu P1 105.29(7) . . ? P2 Cu P1 122.95(3) . . ? C1 N1 C4 104.0(2) . . ? C1 N1 Cu 131.7(2) . . ? C4 N1 Cu 123.74(19) . . ? C9 N2 C6 104.0(2) . . ? C9 N2 Cu 131.4(2) . . ? C6 N2 Cu 124.41(19) . . ? C22 P1 C28 104.97(15) . . ? C22 P1 C16 104.24(15) . . ? C28 P1 C16 102.15(15) . . ? C22 P1 Cu 108.68(11) . . ? C28 P1 Cu 119.87(11) . . ? C16 P1 Cu 115.42(11) . . ? C34 P2 C46 102.03(14) . . ? C34 P2 C40 104.25(14) . . ? C46 P2 C40 101.56(14) . . ? C34 P2 Cu 114.09(10) . . ? C46 P2 Cu 119.74(10) . . ? C40 P2 Cu 113.21(10) . . ? N1 C1 C2 114.3(3) . . ? N1 C1 Br1 121.4(2) . . ? C2 C1 Br1 124.3(3) . . ? C3 C2 C1 105.5(3) . . ? C2 C3 C4 107.4(3) . . ? C5 C4 N1 125.6(3) . . ? C5 C4 C3 125.5(3) . . ? N1 C4 C3 108.8(3) . . ? C4 C5 C6 128.3(3) . . ? C4 C5 C10 115.5(3) . . ? C6 C5 C10 116.2(3) . . ? N2 C6 C5 125.1(3) . . ? N2 C6 C7 109.4(3) . . ? C5 C6 C7 125.3(3) . . ? C8 C7 C6 107.6(3) . . ? C7 C8 C9 104.3(3) . . ? N2 C9 C8 114.7(3) . . ? N2 C9 Br2 121.9(2) . . ? C8 C9 Br2 123.3(2) . . ? C15 C10 C11 117.6(3) . . ? C15 C10 C5 121.4(3) . . ? C11 C10 C5 121.0(3) . . ? C10 C11 C12 121.1(4) . . ? C13 C12 C11 119.8(4) . . ? C14 C13 C12 119.8(4) . . ? C13 C14 C15 120.5(4) . . ? C10 C15 C14 121.2(4) . . ? C17 C16 C21 117.1(3) . . ? C17 C16 P1 121.1(3) . . ? C21 C16 P1 121.3(3) . . ? C16 C17 C18 122.0(4) . . ? C19 C18 C17 119.6(4) . . ? C18 C19 C20 120.0(4) . . ? C19 C20 C21 119.9(4) . . ? C20 C21 C16 121.3(4) . . ? C27 C22 C23 117.9(3) . . ? C27 C22 P1 125.0(3) . . ? C23 C22 P1 116.8(3) . . ? C24 C23 C22 120.7(4) . . ? C25 C24 C23 120.8(4) . . ? C26 C25 C24 119.6(4) . . ? C25 C26 C27 120.0(5) . . ? C22 C27 C26 120.9(4) . . ? C33 C28 C29 118.4(3) . . ? C33 C28 P1 118.2(2) . . ? C29 C28 P1 123.4(3) . . ? C30 C29 C28 120.2(4) . . ? C31 C30 C29 120.5(4) . . ? C32 C31 C30 119.9(3) . . ? C31 C32 C33 120.3(4) . . ? C28 C33 C32 120.7(3) . . ? C39 C34 C35 118.3(3) . . ? C39 C34 P2 123.6(2) . . ? C35 C34 P2 118.1(2) . . ? C36 C35 C34 120.8(3) . . ? C35 C36 C37 120.0(3) . . ? C38 C37 C36 119.3(3) . . ? C37 C38 C39 120.6(4) . . ? C34 C39 C38 120.8(3) . . ? C45 C40 C41 118.6(3) . . ? C45 C40 P2 118.3(2) . . ? C41 C40 P2 123.1(2) . . ? C40 C41 C42 120.2(3) . . ? C43 C42 C41 120.5(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 120.0(3) . . ? C40 C45 C44 120.8(3) . . ? C47 C46 C51 117.9(3) . . ? C47 C46 P2 124.2(3) . . ? C51 C46 P2 117.9(3) . . ? C46 C47 C48 121.0(4) . . ? C49 C48 C47 119.6(4) . . ? C50 C49 C48 119.9(4) . . ? C49 C50 C51 120.8(4) . . ? C50 C51 C46 120.9(4) . . ? 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 N2 Cu N1 C1 175.3(3) . . . . ? P2 Cu N1 C1 58.5(3) . . . . ? P1 Cu N1 C1 -77.6(3) . . . . ? N2 Cu N1 C4 6.0(2) . . . . ? P2 Cu N1 C4 -110.9(2) . . . . ? P1 Cu N1 C4 113.1(2) . . . . ? N1 Cu N2 C9 170.2(3) . . . . ? P2 Cu N2 C9 -77.9(3) . . . . ? P1 Cu N2 C9 60.1(3) . . . . ? N1 Cu N2 C6 -4.9(2) . . . . ? P2 Cu N2 C6 107.1(2) . . . . ? P1 Cu N2 C6 -114.9(2) . . . . ? N1 Cu P1 C22 -78.61(13) . . . . ? N2 Cu P1 C22 19.49(13) . . . . ? P2 Cu P1 C22 152.93(11) . . . . ? N1 Cu P1 C28 160.82(14) . . . . ? N2 Cu P1 C28 -101.09(14) . . . . ? P2 Cu P1 C28 32.36(13) . . . . ? N1 Cu P1 C16 38.02(15) . . . . ? N2 Cu P1 C16 136.11(14) . . . . ? P2 Cu P1 C16 -90.44(13) . . . . ? N1 Cu P2 C34 -71.44(13) . . . . ? N2 Cu P2 C34 -173.34(13) . . . . ? P1 Cu P2 C34 56.93(12) . . . . ? N1 Cu P2 C46 167.32(13) . . . . ? N2 Cu P2 C46 65.42(14) . . . . ? P1 Cu P2 C46 -64.31(13) . . . . ? N1 Cu P2 C40 47.58(13) . . . . ? N2 Cu P2 C40 -54.32(13) . . . . ? P1 Cu P2 C40 175.94(11) . . . . ? C4 N1 C1 C2 -0.1(4) . . . . ? Cu N1 C1 C2 -171.0(2) . . . . ? C4 N1 C1 Br1 178.1(2) . . . . ? Cu N1 C1 Br1 7.2(4) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? Br1 C1 C2 C3 -178.2(2) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C1 N1 C4 C5 -176.4(3) . . . . ? Cu N1 C4 C5 -4.6(4) . . . . ? C1 N1 C4 C3 0.2(3) . . . . ? Cu N1 C4 C3 172.1(2) . . . . ? C2 C3 C4 C5 176.4(3) . . . . ? C2 C3 C4 N1 -0.3(4) . . . . ? N1 C4 C5 C6 -0.3(5) . . . . ? C3 C4 C5 C6 -176.5(3) . . . . ? N1 C4 C5 C10 -179.0(3) . . . . ? C3 C4 C5 C10 4.9(5) . . . . ? C9 N2 C6 C5 -174.1(3) . . . . ? Cu N2 C6 C5 2.1(4) . . . . ? C9 N2 C6 C7 0.9(3) . . . . ? Cu N2 C6 C7 177.1(2) . . . . ? C4 C5 C6 N2 1.8(5) . . . . ? C10 C5 C6 N2 -179.6(3) . . . . ? C4 C5 C6 C7 -172.5(3) . . . . ? C10 C5 C6 C7 6.1(5) . . . . ? N2 C6 C7 C8 -0.8(4) . . . . ? C5 C6 C7 C8 174.2(3) . . . . ? C6 C7 C8 C9 0.3(4) . . . . ? C6 N2 C9 C8 -0.8(4) . . . . ? Cu N2 C9 C8 -176.5(2) . . . . ? C6 N2 C9 Br2 176.2(2) . . . . ? Cu N2 C9 Br2 0.4(4) . . . . ? C7 C8 C9 N2 0.3(4) . . . . ? C7 C8 C9 Br2 -176.6(2) . . . . ? C4 C5 C10 C15 -101.7(4) . . . . ? C6 C5 C10 C15 79.5(4) . . . . ? C4 C5 C10 C11 78.4(4) . . . . ? C6 C5 C10 C11 -100.4(4) . . . . ? C15 C10 C11 C12 -0.3(6) . . . . ? C5 C10 C11 C12 179.6(4) . . . . ? C10 C11 C12 C13 1.0(6) . . . . ? C11 C12 C13 C14 -1.3(7) . . . . ? C12 C13 C14 C15 1.0(7) . . . . ? C11 C10 C15 C14 0.1(6) . . . . ? C5 C10 C15 C14 -179.9(4) . . . . ? C13 C14 C15 C10 -0.4(7) . . . . ? C22 P1 C16 C17 42.4(3) . . . . ? C28 P1 C16 C17 151.5(3) . . . . ? Cu P1 C16 C17 -76.7(3) . . . . ? C22 P1 C16 C21 -145.8(3) . . . . ? C28 P1 C16 C21 -36.7(3) . . . . ? Cu P1 C16 C21 95.1(3) . . . . ? C21 C16 C17 C18 0.3(6) . . . . ? P1 C16 C17 C18 172.4(3) . . . . ? C16 C17 C18 C19 -0.5(6) . . . . ? C17 C18 C19 C20 0.4(7) . . . . ? C18 C19 C20 C21 0.0(6) . . . . ? C19 C20 C21 C16 -0.3(6) . . . . ? C17 C16 C21 C20 0.1(5) . . . . ? P1 C16 C21 C20 -171.9(3) . . . . ? C28 P1 C22 C27 -5.8(3) . . . . ? C16 P1 C22 C27 101.2(3) . . . . ? Cu P1 C22 C27 -135.2(3) . . . . ? C28 P1 C22 C23 168.4(2) . . . . ? C16 P1 C22 C23 -84.6(3) . . . . ? Cu P1 C22 C23 39.0(3) . . . . ? C27 C22 C23 C24 -1.3(5) . . . . ? P1 C22 C23 C24 -176.0(3) . . . . ? C22 C23 C24 C25 1.6(6) . . . . ? C23 C24 C25 C26 -1.1(7) . . . . ? C24 C25 C26 C27 0.4(7) . . . . ? C23 C22 C27 C26 0.6(5) . . . . ? P1 C22 C27 C26 174.8(3) . . . . ? C25 C26 C27 C22 -0.2(6) . . . . ? C22 P1 C28 C33 -116.2(3) . . . . ? C16 P1 C28 C33 135.3(3) . . . . ? Cu P1 C28 C33 6.2(3) . . . . ? C22 P1 C28 C29 63.1(3) . . . . ? C16 P1 C28 C29 -45.5(3) . . . . ? Cu P1 C28 C29 -174.5(3) . . . . ? C33 C28 C29 C30 0.9(6) . . . . ? P1 C28 C29 C30 -178.3(3) . . . . ? C28 C29 C30 C31 -0.4(6) . . . . ? C29 C30 C31 C32 -0.2(6) . . . . ? C30 C31 C32 C33 0.3(6) . . . . ? C29 C28 C33 C32 -0.8(5) . . . . ? P1 C28 C33 C32 178.5(3) . . . . ? C31 C32 C33 C28 0.2(6) . . . . ? C46 P2 C34 C39 -101.2(3) . . . . ? C40 P2 C34 C39 4.2(3) . . . . ? Cu P2 C34 C39 128.2(3) . . . . ? C46 P2 C34 C35 81.5(3) . . . . ? C40 P2 C34 C35 -173.1(3) . . . . ? Cu P2 C34 C35 -49.1(3) . . . . ? C39 C34 C35 C36 -0.9(5) . . . . ? P2 C34 C35 C36 176.5(3) . . . . ? C34 C35 C36 C37 -1.3(6) . . . . ? C35 C36 C37 C38 2.3(6) . . . . ? C36 C37 C38 C39 -1.2(6) . . . . ? C35 C34 C39 C38 2.1(5) . . . . ? P2 C34 C39 C38 -175.1(3) . . . . ? C37 C38 C39 C34 -1.1(6) . . . . ? C34 P2 C40 C45 97.7(3) . . . . ? C46 P2 C40 C45 -156.6(3) . . . . ? Cu P2 C40 C45 -26.9(3) . . . . ? C34 P2 C40 C41 -84.0(3) . . . . ? C46 P2 C40 C41 21.8(3) . . . . ? Cu P2 C40 C41 151.4(2) . . . . ? C45 C40 C41 C42 0.2(5) . . . . ? P2 C40 C41 C42 -178.1(3) . . . . ? C40 C41 C42 C43 0.3(6) . . . . ? C41 C42 C43 C44 -0.7(6) . . . . ? C42 C43 C44 C45 0.6(6) . . . . ? C41 C40 C45 C44 -0.3(5) . . . . ? P2 C40 C45 C44 178.1(3) . . . . ? C43 C44 C45 C40 -0.1(6) . . . . ? C34 P2 C46 C47 -4.2(3) . . . . ? C40 P2 C46 C47 -111.7(3) . . . . ? Cu P2 C46 C47 122.9(3) . . . . ? C34 P2 C46 C51 175.3(3) . . . . ? C40 P2 C46 C51 67.8(3) . . . . ? Cu P2 C46 C51 -57.7(3) . . . . ? C51 C46 C47 C48 -0.1(6) . . . . ? P2 C46 C47 C48 179.4(3) . . . . ? C46 C47 C48 C49 -0.6(7) . . . . ? C47 C48 C49 C50 1.4(7) . . . . ? C48 C49 C50 C51 -1.5(7) . . . . ? C49 C50 C51 C46 0.8(6) . . . . ? C47 C46 C51 C50 0.0(5) . . . . ? P2 C46 C51 C50 -179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.616 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.062 data_s263 _database_code_depnum_ccdc_archive 'CCDC 871236' #TrackingRef 's263-4a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Cl2 Cu N2 O P2' _chemical_formula_weight 908.26 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' 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' Cu Cu 0.3201 1.2651 '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 11.4320(9) _cell_length_b 11.5639(9) _cell_length_c 18.0545(15) _cell_angle_alpha 80.6820(10) _cell_angle_beta 85.9190(10) _cell_angle_gamma 75.1940(10) _cell_volume 2276.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5038 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7270 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12891 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.02 _reflns_number_total 8764 _reflns_number_gt 7110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data set was corrected using the program SQUEEZE. There is one seriously disordered MeOH solvate molecule estimated based on the elemental analyses and 1H NMR spectra. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 180 40 ' ' _platon_squeeze_details ; ; _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^)+(0.0665P)^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 8764 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.83238(2) 0.82666(2) 0.286617(13) 0.03981(9) Uani 1 1 d . . . P1 P 0.72222(5) 0.95212(5) 0.19249(3) 0.03933(13) Uani 1 1 d . . . P2 P 1.03144(5) 0.73045(5) 0.27402(3) 0.04263(14) Uani 1 1 d . . . N1 N 0.81639(14) 0.89682(14) 0.38465(9) 0.0416(4) Uani 1 1 d . . . N2 N 0.74074(15) 0.69913(14) 0.33146(10) 0.0431(4) Uani 1 1 d . . . Cl1 Cl 0.96531(6) 1.04146(6) 0.34554(4) 0.06801(18) Uani 1 1 d . . . Cl2 Cl 0.75001(7) 0.59554(6) 0.20909(4) 0.06925(19) Uani 1 1 d . . . C1 C 0.87023(19) 0.97445(19) 0.40615(13) 0.0475(5) Uani 1 1 d . . . C2 C 0.8444(2) 0.9929(2) 0.48107(14) 0.0572(6) Uani 1 1 d . . . H2A H 0.8723 1.0438 0.5066 0.069 Uiso 1 1 calc R . . C3 C 0.7700(2) 0.9203(2) 0.50810(13) 0.0538(6) Uani 1 1 d . . . H3A H 0.7363 0.9122 0.5565 0.065 Uiso 1 1 calc R . . C4 C 0.75277(18) 0.85886(18) 0.44920(12) 0.0431(5) Uani 1 1 d . . . C5 C 0.68991(17) 0.76869(18) 0.45559(12) 0.0438(5) Uani 1 1 d . . . C6 C 0.68292(18) 0.69533(18) 0.40231(13) 0.0449(5) Uani 1 1 d . . . C7 C 0.6104(2) 0.6103(2) 0.40967(15) 0.0615(6) Uani 1 1 d . . . H7A H 0.5623 0.5909 0.4512 0.074 Uiso 1 1 calc R . . C8 C 0.6248(2) 0.5629(2) 0.34437(16) 0.0674(7) Uani 1 1 d . . . H8A H 0.5893 0.5047 0.3323 0.081 Uiso 1 1 calc R . . C9 C 0.7039(2) 0.61985(18) 0.29944(13) 0.0494(5) Uani 1 1 d . . . C10 C 0.62367(19) 0.7459(2) 0.52878(13) 0.0493(5) Uani 1 1 d . . . C11 C 0.5143(2) 0.8236(2) 0.54442(15) 0.0637(7) Uani 1 1 d . . . H11A H 0.4810 0.8900 0.5092 0.076 Uiso 1 1 calc R . . C12 C 0.4539(3) 0.8020(3) 0.61310(17) 0.0755(8) Uani 1 1 d . . . H12A H 0.3803 0.8545 0.6234 0.091 Uiso 1 1 calc R . . C13 C 0.5010(3) 0.7058(3) 0.66504(16) 0.0709(7) Uani 1 1 d . . . H13A H 0.4599 0.6924 0.7107 0.085 Uiso 1 1 calc R . . C14 C 0.6095(3) 0.6282(3) 0.65006(16) 0.0795(8) Uani 1 1 d . . . H14A H 0.6425 0.5627 0.6859 0.095 Uiso 1 1 calc R . . C15 C 0.6701(2) 0.6469(2) 0.58180(15) 0.0696(7) Uani 1 1 d . . . H15A H 0.7425 0.5925 0.5715 0.084 Uiso 1 1 calc R . . C16 C 0.76298(18) 1.09242(19) 0.15105(13) 0.0471(5) Uani 1 1 d . . . C17 C 0.7685(2) 1.1735(2) 0.19918(15) 0.0602(6) Uani 1 1 d . . . H17A H 0.7515 1.1552 0.2502 0.072 Uiso 1 1 calc R . . C18 C 0.7988(3) 1.2802(2) 0.1718(2) 0.0825(9) Uani 1 1 d . . . H18A H 0.8028 1.3331 0.2047 0.099 Uiso 1 1 calc R . . C19 C 0.8232(3) 1.3099(3) 0.0971(2) 0.1003(11) Uani 1 1 d . . . H19A H 0.8411 1.3835 0.0789 0.120 Uiso 1 1 calc R . . C20 C 0.8208(4) 1.2301(3) 0.0495(2) 0.1017(11) Uani 1 1 d . . . H20A H 0.8396 1.2488 -0.0013 0.122 Uiso 1 1 calc R . . C21 C 0.7906(3) 1.1213(3) 0.07592(15) 0.0743(8) Uani 1 1 d . . . H21A H 0.7890 1.0679 0.0428 0.089 Uiso 1 1 calc R . . C22 C 0.56207(18) 1.00868(19) 0.21925(12) 0.0443(5) Uani 1 1 d . . . C23 C 0.5108(2) 0.9390(2) 0.27541(14) 0.0582(6) Uani 1 1 d . . . H23A H 0.5573 0.8648 0.2976 0.070 Uiso 1 1 calc R . . C24 C 0.3911(2) 0.9784(3) 0.29911(16) 0.0696(7) Uani 1 1 d . . . H24A H 0.3575 0.9308 0.3368 0.083 Uiso 1 1 calc R . . C25 C 0.3230(2) 1.0874(3) 0.26669(16) 0.0672(7) Uani 1 1 d . . . H25A H 0.2426 1.1139 0.2822 0.081 Uiso 1 1 calc R . . C26 C 0.3723(2) 1.1576(3) 0.21180(16) 0.0688(7) Uani 1 1 d . . . H26A H 0.3254 1.2321 0.1905 0.083 Uiso 1 1 calc R . . C27 C 0.4914(2) 1.1192(2) 0.18732(14) 0.0571(6) Uani 1 1 d . . . H27A H 0.5240 1.1677 0.1495 0.068 Uiso 1 1 calc R . . C28 C 0.71787(18) 0.87968(18) 0.11022(12) 0.0419(5) Uani 1 1 d . . . C29 C 0.6115(2) 0.8802(2) 0.07789(13) 0.0555(6) Uani 1 1 d . . . H29A H 0.5379 0.9240 0.0958 0.067 Uiso 1 1 calc R . . C30 C 0.6138(2) 0.8165(3) 0.01964(15) 0.0704(7) Uani 1 1 d . . . H30A H 0.5415 0.8169 -0.0012 0.084 Uiso 1 1 calc R . . C31 C 0.7209(3) 0.7526(3) -0.00813(15) 0.0711(7) Uani 1 1 d . . . H31A H 0.7214 0.7089 -0.0471 0.085 Uiso 1 1 calc R . . C32 C 0.8279(2) 0.7533(2) 0.02192(15) 0.0677(7) Uani 1 1 d . . . H32A H 0.9013 0.7117 0.0024 0.081 Uiso 1 1 calc R . . C33 C 0.8260(2) 0.8157(2) 0.08088(13) 0.0577(6) Uani 1 1 d . . . H33A H 0.8986 0.8151 0.1014 0.069 Uiso 1 1 calc R . . C34 C 1.10250(19) 0.70070(18) 0.36550(13) 0.0475(5) Uani 1 1 d . . . C35 C 1.2145(2) 0.7188(2) 0.37672(16) 0.0664(7) Uani 1 1 d . . . H35A H 1.2618 0.7416 0.3356 0.080 Uiso 1 1 calc R . . C36 C 1.2569(3) 0.7033(3) 0.4480(2) 0.0868(9) Uani 1 1 d . . . H36A H 1.3318 0.7172 0.4547 0.104 Uiso 1 1 calc R . . C37 C 1.1901(4) 0.6680(3) 0.5088(2) 0.0930(11) Uani 1 1 d . . . H37A H 1.2201 0.6563 0.5568 0.112 Uiso 1 1 calc R . . C38 C 1.0786(3) 0.6495(3) 0.49935(16) 0.0836(9) Uani 1 1 d . . . H38A H 1.0326 0.6257 0.5409 0.100 Uiso 1 1 calc R . . C39 C 1.0347(2) 0.6665(2) 0.42796(14) 0.0631(6) Uani 1 1 d . . . H39A H 0.9587 0.6548 0.4218 0.076 Uiso 1 1 calc R . . C40 C 1.13042(19) 0.8029(2) 0.20921(13) 0.0491(5) Uani 1 1 d . . . C41 C 1.2491(2) 0.7448(3) 0.19065(15) 0.0671(7) Uani 1 1 d . . . H41A H 1.2809 0.6645 0.2109 0.080 Uiso 1 1 calc R . . C42 C 1.3196(2) 0.8063(3) 0.14222(17) 0.0786(8) Uani 1 1 d . . . H42A H 1.3990 0.7674 0.1306 0.094 Uiso 1 1 calc R . . C43 C 1.2735(3) 0.9236(3) 0.11138(16) 0.0759(8) Uani 1 1 d . . . H43A H 1.3214 0.9643 0.0788 0.091 Uiso 1 1 calc R . . C44 C 1.1565(3) 0.9816(3) 0.12828(15) 0.0695(7) Uani 1 1 d . . . H44A H 1.1250 1.0614 0.1068 0.083 Uiso 1 1 calc R . . C45 C 1.0856(2) 0.9215(2) 0.17716(13) 0.0528(5) Uani 1 1 d . . . H45A H 1.0065 0.9616 0.1886 0.063 Uiso 1 1 calc R . . C46 C 1.05892(18) 0.57999(19) 0.24538(14) 0.0501(5) Uani 1 1 d . . . C47 C 1.0758(2) 0.5663(2) 0.17031(16) 0.0678(7) Uani 1 1 d . . . H47A H 1.0833 0.6317 0.1345 0.081 Uiso 1 1 calc R . . C48 C 1.0816(3) 0.4558(3) 0.1484(2) 0.0875(10) Uani 1 1 d . . . H48A H 1.0935 0.4475 0.0979 0.105 Uiso 1 1 calc R . . C49 C 1.0701(2) 0.3581(3) 0.2001(2) 0.0867(10) Uani 1 1 d . . . H49A H 1.0731 0.2843 0.1848 0.104 Uiso 1 1 calc R . . C50 C 1.0543(3) 0.3707(3) 0.2734(2) 0.0891(10) Uani 1 1 d . . . H50A H 1.0473 0.3047 0.3088 0.107 Uiso 1 1 calc R . . C51 C 1.0483(2) 0.4809(2) 0.29672(17) 0.0681(7) Uani 1 1 d . . . H51A H 1.0371 0.4878 0.3475 0.082 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 Cu 0.03980(15) 0.04062(15) 0.04083(15) -0.00985(11) 0.00106(11) -0.01151(10) P1 0.0377(3) 0.0421(3) 0.0388(3) -0.0114(2) -0.0002(2) -0.0078(2) P2 0.0382(3) 0.0425(3) 0.0453(3) -0.0056(2) 0.0042(2) -0.0085(2) N1 0.0421(9) 0.0418(9) 0.0444(10) -0.0125(8) -0.0003(8) -0.0134(7) N2 0.0441(9) 0.0382(9) 0.0492(10) -0.0104(8) 0.0016(8) -0.0126(7) Cl1 0.0800(4) 0.0780(4) 0.0620(4) -0.0123(3) 0.0023(3) -0.0487(4) Cl2 0.0938(5) 0.0571(4) 0.0668(4) -0.0261(3) 0.0014(4) -0.0273(3) C1 0.0496(12) 0.0472(12) 0.0491(13) -0.0119(10) -0.0017(10) -0.0156(9) C2 0.0634(15) 0.0609(14) 0.0554(14) -0.0271(12) -0.0015(12) -0.0189(12) C3 0.0561(13) 0.0633(14) 0.0437(13) -0.0177(11) 0.0045(10) -0.0133(11) C4 0.0420(11) 0.0436(11) 0.0424(12) -0.0103(9) 0.0023(9) -0.0068(9) C5 0.0356(10) 0.0437(11) 0.0473(12) -0.0051(9) 0.0024(9) -0.0031(8) C6 0.0407(11) 0.0401(11) 0.0540(13) -0.0045(9) 0.0029(10) -0.0129(9) C7 0.0589(15) 0.0572(14) 0.0730(17) -0.0066(13) 0.0099(13) -0.0278(12) C8 0.0760(17) 0.0572(14) 0.0827(19) -0.0144(14) -0.0007(15) -0.0395(13) C9 0.0563(13) 0.0385(11) 0.0566(14) -0.0118(10) -0.0035(11) -0.0143(9) C10 0.0461(12) 0.0507(12) 0.0512(13) -0.0093(10) 0.0078(10) -0.0137(10) C11 0.0544(14) 0.0652(15) 0.0637(16) -0.0086(13) 0.0104(12) -0.0045(12) C12 0.0592(16) 0.086(2) 0.079(2) -0.0239(17) 0.0265(15) -0.0155(14) C13 0.0809(19) 0.0846(19) 0.0567(16) -0.0217(15) 0.0239(14) -0.0376(16) C14 0.091(2) 0.0769(19) 0.0598(17) 0.0075(14) 0.0125(15) -0.0174(16) C15 0.0597(15) 0.0691(16) 0.0652(17) 0.0042(13) 0.0138(13) -0.0022(12) C16 0.0421(11) 0.0451(11) 0.0542(13) -0.0080(10) -0.0036(10) -0.0099(9) C17 0.0614(15) 0.0514(13) 0.0697(16) -0.0180(12) -0.0041(12) -0.0111(11) C18 0.084(2) 0.0554(16) 0.117(3) -0.0257(17) -0.0026(19) -0.0260(14) C19 0.115(3) 0.0645(19) 0.130(3) 0.006(2) -0.012(2) -0.0479(19) C20 0.141(3) 0.091(2) 0.081(2) 0.0150(19) 0.005(2) -0.062(2) C21 0.100(2) 0.0760(18) 0.0570(16) -0.0060(14) 0.0031(15) -0.0432(16) C22 0.0420(11) 0.0494(12) 0.0427(12) -0.0180(10) -0.0007(9) -0.0066(9) C23 0.0453(12) 0.0553(13) 0.0651(16) -0.0033(12) 0.0096(11) -0.0029(10) C24 0.0544(15) 0.0794(18) 0.0695(18) -0.0080(14) 0.0126(13) -0.0128(13) C25 0.0421(13) 0.0846(19) 0.0700(17) -0.0247(15) 0.0047(12) -0.0005(12) C26 0.0486(14) 0.0709(17) 0.0743(18) -0.0115(14) -0.0059(13) 0.0098(12) C27 0.0503(13) 0.0598(14) 0.0559(14) -0.0075(11) -0.0039(11) -0.0042(11) C28 0.0444(11) 0.0405(10) 0.0413(11) -0.0099(9) 0.0011(9) -0.0097(8) C29 0.0471(13) 0.0689(15) 0.0553(14) -0.0222(12) 0.0013(11) -0.0158(11) C30 0.0666(17) 0.095(2) 0.0634(17) -0.0348(15) -0.0029(13) -0.0306(15) C31 0.092(2) 0.0766(18) 0.0546(15) -0.0344(14) 0.0074(15) -0.0256(15) C32 0.0685(17) 0.0732(17) 0.0593(16) -0.0300(13) 0.0120(13) -0.0052(13) C33 0.0490(13) 0.0686(15) 0.0554(14) -0.0220(12) 0.0018(11) -0.0077(11) C34 0.0480(12) 0.0423(11) 0.0491(13) -0.0059(10) -0.0037(10) -0.0057(9) C35 0.0580(15) 0.0701(16) 0.0708(18) -0.0128(13) -0.0106(13) -0.0116(12) C36 0.080(2) 0.088(2) 0.096(3) -0.0217(19) -0.0316(19) -0.0138(16) C37 0.117(3) 0.083(2) 0.069(2) -0.0098(17) -0.040(2) 0.0036(19) C38 0.108(3) 0.0760(19) 0.0522(17) 0.0018(14) -0.0008(17) -0.0035(17) C39 0.0650(15) 0.0610(15) 0.0543(15) -0.0007(12) -0.0010(12) -0.0048(12) C40 0.0409(11) 0.0583(13) 0.0490(13) -0.0087(11) 0.0059(10) -0.0155(10) C41 0.0531(14) 0.0678(16) 0.0747(18) -0.0052(13) 0.0145(13) -0.0126(12) C42 0.0501(15) 0.103(2) 0.084(2) -0.0166(18) 0.0232(14) -0.0259(15) C43 0.0682(18) 0.107(2) 0.0617(17) -0.0035(16) 0.0116(14) -0.0467(17) C44 0.0753(18) 0.0764(17) 0.0599(16) 0.0084(13) -0.0050(14) -0.0353(14) C45 0.0495(13) 0.0577(14) 0.0516(13) -0.0028(11) -0.0011(10) -0.0173(10) C46 0.0346(11) 0.0495(12) 0.0630(15) -0.0146(11) 0.0025(10) -0.0022(9) C47 0.0635(16) 0.0665(16) 0.0704(18) -0.0239(14) 0.0054(13) -0.0042(12) C48 0.0694(19) 0.092(2) 0.103(2) -0.057(2) -0.0020(17) 0.0034(16) C49 0.0631(18) 0.0611(18) 0.140(3) -0.048(2) -0.0149(19) 0.0004(14) C50 0.091(2) 0.0464(15) 0.128(3) -0.0149(17) -0.011(2) -0.0105(14) C51 0.0763(17) 0.0514(14) 0.0762(18) -0.0109(13) -0.0007(14) -0.0143(12) _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 Cu N1 2.0414(16) . ? Cu N2 2.0519(17) . ? Cu P1 2.2696(6) . ? Cu P2 2.2765(6) . ? P1 C16 1.831(2) . ? P1 C28 1.829(2) . ? P1 C22 1.838(2) . ? P2 C40 1.825(2) . ? P2 C46 1.839(2) . ? P2 C34 1.836(2) . ? N1 C1 1.328(2) . ? N1 C4 1.399(3) . ? N2 C9 1.325(2) . ? N2 C6 1.397(3) . ? Cl1 C1 1.722(2) . ? Cl2 C9 1.723(2) . ? C1 C2 1.402(3) . ? C2 C3 1.357(3) . ? C3 C4 1.422(3) . ? C4 C5 1.396(3) . ? C5 C6 1.400(3) . ? C5 C10 1.495(3) . ? C6 C7 1.425(3) . ? C7 C8 1.362(4) . ? C8 C9 1.392(3) . ? C10 C11 1.381(3) . ? C10 C15 1.384(3) . ? C11 C12 1.393(4) . ? C12 C13 1.355(4) . ? C13 C14 1.370(4) . ? C14 C15 1.383(4) . ? C16 C21 1.377(3) . ? C16 C17 1.393(3) . ? C17 C18 1.373(4) . ? C18 C19 1.363(5) . ? C19 C20 1.366(5) . ? C20 C21 1.391(4) . ? C22 C23 1.383(3) . ? C22 C27 1.385(3) . ? C23 C24 1.387(3) . ? C24 C25 1.365(4) . ? C25 C26 1.360(4) . ? C26 C27 1.384(3) . ? C28 C33 1.386(3) . ? C28 C29 1.384(3) . ? C29 C30 1.373(3) . ? C30 C31 1.366(4) . ? C31 C32 1.376(4) . ? C32 C33 1.376(3) . ? C34 C35 1.383(3) . ? C34 C39 1.384(3) . ? C35 C36 1.376(4) . ? C36 C37 1.360(5) . ? C37 C38 1.372(5) . ? C38 C39 1.382(4) . ? C40 C45 1.380(3) . ? C40 C41 1.396(3) . ? C41 C42 1.382(4) . ? C42 C43 1.364(4) . ? C43 C44 1.371(4) . ? C44 C45 1.381(3) . ? C46 C51 1.378(3) . ? C46 C47 1.384(3) . ? C47 C48 1.382(4) . ? C48 C49 1.371(5) . ? C49 C50 1.349(5) . ? C50 C51 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu N2 92.45(7) . . ? N1 Cu P1 113.85(5) . . ? N2 Cu P1 108.27(5) . . ? N1 Cu P2 105.69(5) . . ? N2 Cu P2 107.83(5) . . ? P1 Cu P2 124.06(2) . . ? C16 P1 C28 102.53(10) . . ? C16 P1 C22 101.55(10) . . ? C28 P1 C22 104.15(9) . . ? C16 P1 Cu 120.00(7) . . ? C28 P1 Cu 113.32(7) . . ? C22 P1 Cu 113.39(7) . . ? C40 P2 C46 102.77(10) . . ? C40 P2 C34 105.10(10) . . ? C46 P2 C34 104.03(10) . . ? C40 P2 Cu 119.51(7) . . ? C46 P2 Cu 114.49(7) . . ? C34 P2 Cu 109.48(7) . . ? C1 N1 C4 104.09(17) . . ? C1 N1 Cu 130.73(15) . . ? C4 N1 Cu 124.80(13) . . ? C9 N2 C6 104.33(17) . . ? C9 N2 Cu 130.51(15) . . ? C6 N2 Cu 124.15(13) . . ? N1 C1 C2 114.2(2) . . ? N1 C1 Cl1 121.13(16) . . ? C2 C1 Cl1 124.69(17) . . ? C3 C2 C1 104.9(2) . . ? C2 C3 C4 107.8(2) . . ? C5 C4 N1 124.95(18) . . ? C5 C4 C3 125.8(2) . . ? N1 C4 C3 109.07(18) . . ? C4 C5 C6 128.0(2) . . ? C4 C5 C10 116.13(19) . . ? C6 C5 C10 115.88(19) . . ? N2 C6 C5 125.18(18) . . ? N2 C6 C7 109.1(2) . . ? C5 C6 C7 125.6(2) . . ? C8 C7 C6 107.0(2) . . ? C7 C8 C9 105.5(2) . . ? N2 C9 C8 114.1(2) . . ? N2 C9 Cl2 121.16(17) . . ? C8 C9 Cl2 124.72(17) . . ? C11 C10 C15 118.8(2) . . ? C11 C10 C5 120.3(2) . . ? C15 C10 C5 120.89(19) . . ? C10 C11 C12 119.8(2) . . ? C13 C12 C11 120.9(3) . . ? C12 C13 C14 119.7(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C10 120.4(2) . . ? C21 C16 C17 118.3(2) . . ? C21 C16 P1 124.14(18) . . ? C17 C16 P1 117.50(19) . . ? C18 C17 C16 120.5(3) . . ? C19 C18 C17 121.1(3) . . ? C20 C19 C18 119.1(3) . . ? C19 C20 C21 120.8(3) . . ? C16 C21 C20 120.1(3) . . ? C23 C22 C27 118.6(2) . . ? C23 C22 P1 118.35(16) . . ? C27 C22 P1 123.07(18) . . ? C22 C23 C24 120.9(2) . . ? C25 C24 C23 119.6(3) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 120.8(2) . . ? C26 C27 C22 119.9(2) . . ? C33 C28 C29 118.1(2) . . ? C33 C28 P1 118.50(16) . . ? C29 C28 P1 123.33(16) . . ? C30 C29 C28 120.5(2) . . ? C31 C30 C29 120.8(2) . . ? C30 C31 C32 119.7(2) . . ? C31 C32 C33 119.7(2) . . ? C32 C33 C28 121.2(2) . . ? C35 C34 C39 118.0(2) . . ? C35 C34 P2 124.58(19) . . ? C39 C34 P2 117.19(18) . . ? C36 C35 C34 120.8(3) . . ? C37 C36 C35 120.6(3) . . ? C36 C37 C38 119.9(3) . . ? C37 C38 C39 119.8(3) . . ? C38 C39 C34 120.9(3) . . ? C45 C40 C41 118.4(2) . . ? C45 C40 P2 118.24(16) . . ? C41 C40 P2 123.41(18) . . ? C42 C41 C40 120.2(3) . . ? C43 C42 C41 120.4(3) . . ? C42 C43 C44 120.2(2) . . ? C43 C44 C45 119.9(3) . . ? C40 C45 C44 120.9(2) . . ? C51 C46 C47 118.1(2) . . ? C51 C46 P2 120.83(19) . . ? C47 C46 P2 120.62(19) . . ? C48 C47 C46 120.3(3) . . ? C49 C48 C47 121.1(3) . . ? C50 C49 C48 119.0(3) . . ? C49 C50 C51 121.0(3) . . ? C46 C51 C50 120.6(3) . . ? 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 N1 Cu P1 C16 67.81(10) . . . . ? N2 Cu P1 C16 169.06(9) . . . . ? P2 Cu P1 C16 -63.17(9) . . . . ? N1 Cu P1 C28 -170.75(9) . . . . ? N2 Cu P1 C28 -69.50(9) . . . . ? P2 Cu P1 C28 58.27(8) . . . . ? N1 Cu P1 C22 -52.29(9) . . . . ? N2 Cu P1 C22 48.96(9) . . . . ? P2 Cu P1 C22 176.73(7) . . . . ? N1 Cu P2 C40 -102.24(10) . . . . ? N2 Cu P2 C40 159.89(10) . . . . ? P1 Cu P2 C40 31.93(9) . . . . ? N1 Cu P2 C46 135.28(10) . . . . ? N2 Cu P2 C46 37.41(10) . . . . ? P1 Cu P2 C46 -90.54(9) . . . . ? N1 Cu P2 C34 18.93(9) . . . . ? N2 Cu P2 C34 -78.94(9) . . . . ? P1 Cu P2 C34 153.11(8) . . . . ? N2 Cu N1 C1 168.06(18) . . . . ? P1 Cu N1 C1 -80.71(18) . . . . ? P2 Cu N1 C1 58.77(18) . . . . ? N2 Cu N1 C4 -3.67(16) . . . . ? P1 Cu N1 C4 107.55(15) . . . . ? P2 Cu N1 C4 -112.96(15) . . . . ? N1 Cu N2 C9 174.04(18) . . . . ? P1 Cu N2 C9 57.91(18) . . . . ? P2 Cu N2 C9 -78.62(18) . . . . ? N1 Cu N2 C6 7.39(16) . . . . ? P1 Cu N2 C6 -108.73(15) . . . . ? P2 Cu N2 C6 114.73(15) . . . . ? C4 N1 C1 C2 -1.3(2) . . . . ? Cu N1 C1 C2 -174.30(15) . . . . ? C4 N1 C1 Cl1 177.35(15) . . . . ? Cu N1 C1 Cl1 4.3(3) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? Cl1 C1 C2 C3 -177.94(17) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C1 N1 C4 C5 -174.37(19) . . . . ? Cu N1 C4 C5 -0.8(3) . . . . ? C1 N1 C4 C3 1.4(2) . . . . ? Cu N1 C4 C3 174.98(13) . . . . ? C2 C3 C4 C5 174.6(2) . . . . ? C2 C3 C4 N1 -1.1(3) . . . . ? N1 C4 C5 C6 3.7(3) . . . . ? C3 C4 C5 C6 -171.4(2) . . . . ? N1 C4 C5 C10 -177.50(18) . . . . ? C3 C4 C5 C10 7.4(3) . . . . ? C9 N2 C6 C5 -176.79(19) . . . . ? Cu N2 C6 C5 -7.2(3) . . . . ? C9 N2 C6 C7 -0.2(2) . . . . ? Cu N2 C6 C7 169.33(15) . . . . ? C4 C5 C6 N2 0.7(3) . . . . ? C10 C5 C6 N2 -178.05(18) . . . . ? C4 C5 C6 C7 -175.3(2) . . . . ? C10 C5 C6 C7 5.9(3) . . . . ? N2 C6 C7 C8 0.4(3) . . . . ? C5 C6 C7 C8 176.9(2) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C6 N2 C9 C8 0.0(3) . . . . ? Cu N2 C9 C8 -168.63(17) . . . . ? C6 N2 C9 Cl2 178.60(15) . . . . ? Cu N2 C9 Cl2 10.0(3) . . . . ? C7 C8 C9 N2 0.2(3) . . . . ? C7 C8 C9 Cl2 -178.31(19) . . . . ? C4 C5 C10 C11 77.6(3) . . . . ? C6 C5 C10 C11 -103.4(2) . . . . ? C4 C5 C10 C15 -102.7(3) . . . . ? C6 C5 C10 C15 76.2(3) . . . . ? C15 C10 C11 C12 0.9(4) . . . . ? C5 C10 C11 C12 -179.4(2) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? C13 C14 C15 C10 1.9(5) . . . . ? C11 C10 C15 C14 -1.9(4) . . . . ? C5 C10 C15 C14 178.5(3) . . . . ? C28 P1 C16 C21 -4.3(2) . . . . ? C22 P1 C16 C21 -111.8(2) . . . . ? Cu P1 C16 C21 122.3(2) . . . . ? C28 P1 C16 C17 176.98(17) . . . . ? C22 P1 C16 C17 69.46(18) . . . . ? Cu P1 C16 C17 -56.40(19) . . . . ? C21 C16 C17 C18 1.0(4) . . . . ? P1 C16 C17 C18 179.8(2) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? C17 C18 C19 C20 -2.0(5) . . . . ? C18 C19 C20 C21 1.9(6) . . . . ? C17 C16 C21 C20 -1.2(4) . . . . ? P1 C16 C21 C20 -179.9(2) . . . . ? C19 C20 C21 C16 -0.2(5) . . . . ? C16 P1 C22 C23 -156.86(18) . . . . ? C28 P1 C22 C23 96.89(19) . . . . ? Cu P1 C22 C23 -26.75(19) . . . . ? C16 P1 C22 C27 21.2(2) . . . . ? C28 P1 C22 C27 -85.0(2) . . . . ? Cu P1 C22 C27 151.32(17) . . . . ? C27 C22 C23 C24 0.4(3) . . . . ? P1 C22 C23 C24 178.5(2) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C25 C26 C27 C22 -0.5(4) . . . . ? C23 C22 C27 C26 -0.1(3) . . . . ? P1 C22 C27 C26 -178.15(18) . . . . ? C16 P1 C28 C33 81.36(19) . . . . ? C22 P1 C28 C33 -173.13(18) . . . . ? Cu P1 C28 C33 -49.4(2) . . . . ? C16 P1 C28 C29 -102.0(2) . . . . ? C22 P1 C28 C29 3.5(2) . . . . ? Cu P1 C28 C29 127.18(18) . . . . ? C33 C28 C29 C30 1.5(4) . . . . ? P1 C28 C29 C30 -175.1(2) . . . . ? C28 C29 C30 C31 -0.7(4) . . . . ? C29 C30 C31 C32 -0.9(5) . . . . ? C30 C31 C32 C33 1.7(4) . . . . ? C31 C32 C33 C28 -0.8(4) . . . . ? C29 C28 C33 C32 -0.8(4) . . . . ? P1 C28 C33 C32 176.0(2) . . . . ? C40 P2 C34 C35 -6.7(2) . . . . ? C46 P2 C34 C35 100.9(2) . . . . ? Cu P2 C34 C35 -136.25(18) . . . . ? C40 P2 C34 C39 168.21(17) . . . . ? C46 P2 C34 C39 -84.12(18) . . . . ? Cu P2 C34 C39 38.68(19) . . . . ? C39 C34 C35 C36 -0.1(4) . . . . ? P2 C34 C35 C36 174.8(2) . . . . ? C34 C35 C36 C37 1.1(4) . . . . ? C35 C36 C37 C38 -1.2(5) . . . . ? C36 C37 C38 C39 0.3(5) . . . . ? C37 C38 C39 C34 0.7(4) . . . . ? C35 C34 C39 C38 -0.8(4) . . . . ? P2 C34 C39 C38 -176.1(2) . . . . ? C46 P2 C40 C45 136.84(19) . . . . ? C34 P2 C40 C45 -114.58(19) . . . . ? Cu P2 C40 C45 8.8(2) . . . . ? C46 P2 C40 C41 -43.4(2) . . . . ? C34 P2 C40 C41 65.2(2) . . . . ? Cu P2 C40 C41 -171.51(18) . . . . ? C45 C40 C41 C42 1.0(4) . . . . ? P2 C40 C41 C42 -178.7(2) . . . . ? C40 C41 C42 C43 -0.9(4) . . . . ? C41 C42 C43 C44 0.1(5) . . . . ? C42 C43 C44 C45 0.6(4) . . . . ? C41 C40 C45 C44 -0.4(4) . . . . ? P2 C40 C45 C44 179.36(19) . . . . ? C43 C44 C45 C40 -0.4(4) . . . . ? C40 P2 C46 C51 150.2(2) . . . . ? C34 P2 C46 C51 40.8(2) . . . . ? Cu P2 C46 C51 -78.7(2) . . . . ? C40 P2 C46 C47 -37.9(2) . . . . ? C34 P2 C46 C47 -147.32(19) . . . . ? Cu P2 C46 C47 93.23(19) . . . . ? C51 C46 C47 C48 0.0(4) . . . . ? P2 C46 C47 C48 -172.1(2) . . . . ? C46 C47 C48 C49 0.4(4) . . . . ? C47 C48 C49 C50 -0.8(5) . . . . ? C48 C49 C50 C51 0.7(5) . . . . ? C47 C46 C51 C50 -0.1(4) . . . . ? P2 C46 C51 C50 172.0(2) . . . . ? C49 C50 C51 C46 -0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.474 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.047 data_s288 _database_code_depnum_ccdc_archive 'CCDC 871237' #TrackingRef 'S288.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H43 Br2 Cu N2 P2' _chemical_formula_weight 945.15 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' P P 0.1023 0.0942 '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 11.0123(19) _cell_length_b 11.935(2) _cell_length_c 17.701(3) _cell_angle_alpha 82.839(2) _cell_angle_beta 80.293(3) _cell_angle_gamma 71.108(2) _cell_volume 2163.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 4139 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.67 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 2.462 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5139 _exptl_absorpt_correction_T_max 0.6197 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12155 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.05 _reflns_number_total 8278 _reflns_number_gt 6293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0627P)^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 8278 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.33354(3) -0.76347(3) 0.258807(19) 0.03239(11) Uani 1 1 d . . . Br1 Br 0.37299(4) -0.89738(3) 0.595840(18) 0.05914(13) Uani 1 1 d . . . Br2 Br 0.06500(4) -0.97482(4) 0.07170(2) 0.06351(13) Uani 1 1 d . . . P1 P 0.22550(7) -0.56482(7) 0.26921(4) 0.03378(18) Uani 1 1 d . . . P2 P 0.53359(7) -0.82182(7) 0.18453(4) 0.03183(17) Uani 1 1 d . . . N1 N 0.3313(2) -0.8454(2) 0.36878(13) 0.0340(5) Uani 1 1 d . . . N2 N 0.2222(2) -0.8515(2) 0.22234(13) 0.0332(5) Uani 1 1 d . . . C1 C 0.3745(3) -0.8264(3) 0.43086(16) 0.0382(7) Uani 1 1 d . . . C2 C 0.3308(3) -0.8920(3) 0.49598(16) 0.0411(7) Uani 1 1 d . . . C3 C 0.2591(3) -0.9543(3) 0.47474(16) 0.0415(7) Uani 1 1 d . . . C4 C 0.2601(3) -0.9242(3) 0.39382(16) 0.0352(6) Uani 1 1 d . . . C5 C 0.1966(3) -0.9656(3) 0.34727(16) 0.0380(7) Uani 1 1 d . . . H5A H 0.1567 -1.0222 0.3726 0.046 Uiso 1 1 calc R . . C6 C 0.1814(3) -0.9386(3) 0.27034(16) 0.0346(6) Uani 1 1 d . . . C7 C 0.1200(3) -0.9966(3) 0.22879(18) 0.0415(7) Uani 1 1 d . . . C8 C 0.1280(3) -0.9422(3) 0.15616(17) 0.0397(7) Uani 1 1 d . . . C9 C 0.1880(3) -0.8538(3) 0.15353(16) 0.0361(7) Uani 1 1 d . . . C10 C 0.4544(4) -0.7470(3) 0.4295(2) 0.0554(9) Uani 1 1 d . . . H10A H 0.4713 -0.7136 0.3768 0.083 Uiso 1 1 calc R . . H10B H 0.5367 -0.7925 0.4480 0.083 Uiso 1 1 calc R . . H10C H 0.4078 -0.6825 0.4629 0.083 Uiso 1 1 calc R . . C11 C 0.1922(4) -1.0346(3) 0.52420(19) 0.0628(10) Uani 1 1 d . . . H11A H 0.2087 -1.0392 0.5774 0.094 Uiso 1 1 calc R . . H11B H 0.2255 -1.1142 0.5053 0.094 Uiso 1 1 calc R . . H11C H 0.0987 -1.0028 0.5222 0.094 Uiso 1 1 calc R . . C12 C 0.2096(3) -0.7733(3) 0.08526(18) 0.0497(8) Uani 1 1 d . . . H12A H 0.2536 -0.7204 0.0984 0.074 Uiso 1 1 calc R . . H12B H 0.1261 -0.7259 0.0690 0.074 Uiso 1 1 calc R . . H12C H 0.2635 -0.8205 0.0433 0.074 Uiso 1 1 calc R . . C13 C 0.0612(4) -1.0935(3) 0.2585(2) 0.0654(11) Uani 1 1 d . . . H13A H 0.0262 -1.1149 0.2170 0.098 Uiso 1 1 calc R . . H13B H -0.0088 -1.0657 0.3006 0.098 Uiso 1 1 calc R . . H13C H 0.1277 -1.1633 0.2774 0.098 Uiso 1 1 calc R . . C14 C 0.0699(3) -0.5361(3) 0.33220(17) 0.0396(7) Uani 1 1 d . . . C15 C 0.0514(3) -0.6249(3) 0.38629(19) 0.0550(9) Uani 1 1 d . . . H15A H 0.1186 -0.6984 0.3901 0.066 Uiso 1 1 calc R . . C16 C -0.0645(4) -0.6076(4) 0.4350(2) 0.0779(13) Uani 1 1 d . . . H16A H -0.0758 -0.6692 0.4723 0.093 Uiso 1 1 calc R . . C17 C -0.1615(4) -0.5044(4) 0.4303(2) 0.0826(14) Uani 1 1 d . . . H17A H -0.2403 -0.4931 0.4643 0.099 Uiso 1 1 calc R . . C18 C -0.1456(4) -0.4160(4) 0.3761(3) 0.0807(14) Uani 1 1 d . . . H18A H -0.2143 -0.3436 0.3720 0.097 Uiso 1 1 calc R . . C19 C -0.0304(3) -0.4315(3) 0.3276(2) 0.0619(10) Uani 1 1 d . . . H19A H -0.0202 -0.3694 0.2904 0.074 Uiso 1 1 calc R . . C20 C 0.3127(3) -0.4835(3) 0.30991(17) 0.0398(7) Uani 1 1 d . . . C21 C 0.2551(4) -0.4028(3) 0.3647(2) 0.0629(10) Uani 1 1 d . . . H21A H 0.1646 -0.3835 0.3814 0.075 Uiso 1 1 calc R . . C22 C 0.3279(5) -0.3498(4) 0.3955(2) 0.0863(15) Uani 1 1 d . . . H22A H 0.2869 -0.2940 0.4330 0.104 Uiso 1 1 calc R . . C23 C 0.4588(5) -0.3769(4) 0.3725(2) 0.0790(14) Uani 1 1 d . . . H23A H 0.5085 -0.3409 0.3946 0.095 Uiso 1 1 calc R . . C24 C 0.5171(4) -0.4555(4) 0.3180(2) 0.0681(11) Uani 1 1 d . . . H24A H 0.6075 -0.4738 0.3012 0.082 Uiso 1 1 calc R . . C25 C 0.4444(3) -0.5087(3) 0.2871(2) 0.0547(9) Uani 1 1 d . . . H25A H 0.4859 -0.5638 0.2493 0.066 Uiso 1 1 calc R . . C26 C 0.1766(3) -0.4713(3) 0.18235(16) 0.0366(7) Uani 1 1 d . . . C27 C 0.0818(3) -0.4893(3) 0.14776(18) 0.0513(8) Uani 1 1 d . . . H27A H 0.0426 -0.5479 0.1702 0.062 Uiso 1 1 calc R . . C28 C 0.0427(4) -0.4238(3) 0.08109(19) 0.0580(9) Uani 1 1 d . . . H28A H -0.0246 -0.4360 0.0592 0.070 Uiso 1 1 calc R . . C29 C 0.1011(4) -0.3410(3) 0.0464(2) 0.0602(10) Uani 1 1 d . . . H29A H 0.0756 -0.2965 0.0002 0.072 Uiso 1 1 calc R . . C30 C 0.1961(4) -0.3238(3) 0.0795(2) 0.0594(10) Uani 1 1 d . . . H30A H 0.2371 -0.2671 0.0556 0.071 Uiso 1 1 calc R . . C31 C 0.2345(3) -0.3870(3) 0.14704(19) 0.0487(8) Uani 1 1 d . . . H31A H 0.3003 -0.3727 0.1693 0.058 Uiso 1 1 calc R . . C32 C 0.5235(3) -0.7805(3) 0.08205(16) 0.0369(7) Uani 1 1 d . . . C33 C 0.5625(3) -0.8620(3) 0.02608(18) 0.0504(8) Uani 1 1 d . . . H33A H 0.6043 -0.9435 0.0393 0.060 Uiso 1 1 calc R . . C34 C 0.5401(4) -0.8235(4) -0.0492(2) 0.0685(11) Uani 1 1 d . . . H34A H 0.5659 -0.8794 -0.0872 0.082 Uiso 1 1 calc R . . C35 C 0.4812(4) -0.7060(4) -0.0694(2) 0.0687(12) Uani 1 1 d . . . H35A H 0.4664 -0.6809 -0.1210 0.082 Uiso 1 1 calc R . . C36 C 0.4437(4) -0.6244(3) -0.0145(2) 0.0584(10) Uani 1 1 d . . . H36A H 0.4037 -0.5427 -0.0284 0.070 Uiso 1 1 calc R . . C37 C 0.4642(3) -0.6617(3) 0.06024(18) 0.0449(8) Uani 1 1 d . . . H37A H 0.4373 -0.6051 0.0978 0.054 Uiso 1 1 calc R . . C38 C 0.6673(3) -0.7719(3) 0.20174(16) 0.0345(6) Uani 1 1 d . . . C39 C 0.7193(3) -0.8129(3) 0.27016(18) 0.0478(8) Uani 1 1 d . . . H39A H 0.6880 -0.8682 0.3047 0.057 Uiso 1 1 calc R . . C40 C 0.8153(3) -0.7747(3) 0.2888(2) 0.0583(9) Uani 1 1 d . . . H40A H 0.8504 -0.8050 0.3353 0.070 Uiso 1 1 calc R . . C41 C 0.8607(4) -0.6928(4) 0.2402(2) 0.0611(10) Uani 1 1 d . . . H41A H 0.9255 -0.6652 0.2534 0.073 Uiso 1 1 calc R . . C42 C 0.8106(4) -0.6519(4) 0.1722(2) 0.0630(11) Uani 1 1 d . . . H42A H 0.8416 -0.5961 0.1382 0.076 Uiso 1 1 calc R . . C43 C 0.7152(3) -0.6912(3) 0.15296(19) 0.0492(8) Uani 1 1 d . . . H43A H 0.6822 -0.6624 0.1056 0.059 Uiso 1 1 calc R . . C44 C 0.6098(3) -0.9831(3) 0.18918(16) 0.0355(6) Uani 1 1 d . . . C45 C 0.5363(3) -1.0551(3) 0.22272(17) 0.0414(7) Uani 1 1 d . . . H45A H 0.4482 -1.0205 0.2431 0.050 Uiso 1 1 calc R . . C46 C 0.5905(4) -1.1774(3) 0.22678(19) 0.0530(9) Uani 1 1 d . . . H46A H 0.5393 -1.2265 0.2497 0.064 Uiso 1 1 calc R . . C47 C 0.7175(4) -1.2278(3) 0.1979(2) 0.0617(10) Uani 1 1 d . . . H47A H 0.7545 -1.3117 0.2009 0.074 Uiso 1 1 calc R . . C48 C 0.7917(4) -1.1566(4) 0.1643(3) 0.0702(11) Uani 1 1 d . . . H48A H 0.8799 -1.1917 0.1443 0.084 Uiso 1 1 calc R . . C49 C 0.7382(3) -1.0345(3) 0.1598(2) 0.0558(9) Uani 1 1 d . . . H49A H 0.7895 -0.9858 0.1366 0.067 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 Cu 0.0369(2) 0.0344(2) 0.02878(19) -0.00049(15) -0.00705(15) -0.01442(15) Br1 0.0857(3) 0.0549(2) 0.03190(18) -0.00361(15) -0.02414(17) -0.00685(19) Br2 0.0793(3) 0.0798(3) 0.0510(2) -0.00990(19) -0.02828(19) -0.0398(2) P1 0.0372(4) 0.0321(4) 0.0323(4) -0.0006(3) -0.0043(3) -0.0119(3) P2 0.0341(4) 0.0327(4) 0.0305(4) -0.0015(3) -0.0038(3) -0.0134(3) N1 0.0385(14) 0.0348(13) 0.0289(12) 0.0009(10) -0.0096(10) -0.0101(11) N2 0.0350(13) 0.0371(13) 0.0302(12) 0.0016(10) -0.0107(10) -0.0133(11) C1 0.0423(17) 0.0375(17) 0.0315(16) -0.0036(13) -0.0121(13) -0.0039(14) C2 0.0500(19) 0.0434(18) 0.0246(15) -0.0028(13) -0.0112(13) -0.0042(15) C3 0.0468(18) 0.0449(18) 0.0299(16) 0.0042(14) -0.0059(14) -0.0123(15) C4 0.0382(16) 0.0362(16) 0.0297(15) -0.0009(13) -0.0070(12) -0.0088(13) C5 0.0431(17) 0.0375(17) 0.0352(16) 0.0026(13) -0.0058(13) -0.0166(14) C6 0.0345(15) 0.0380(16) 0.0348(15) 0.0000(13) -0.0106(12) -0.0141(13) C7 0.0443(18) 0.0424(18) 0.0436(18) 0.0000(14) -0.0146(14) -0.0183(15) C8 0.0434(17) 0.0478(18) 0.0352(16) -0.0057(14) -0.0151(13) -0.0184(15) C9 0.0336(16) 0.0426(17) 0.0335(16) -0.0023(13) -0.0090(12) -0.0116(13) C10 0.074(2) 0.053(2) 0.049(2) -0.0018(17) -0.0269(18) -0.0260(19) C11 0.079(3) 0.077(3) 0.0360(18) 0.0164(18) -0.0132(18) -0.035(2) C12 0.053(2) 0.066(2) 0.0382(17) 0.0082(16) -0.0164(15) -0.0281(18) C13 0.087(3) 0.066(2) 0.066(2) 0.008(2) -0.031(2) -0.049(2) C14 0.0400(17) 0.0409(18) 0.0349(16) -0.0059(14) -0.0033(13) -0.0081(14) C15 0.046(2) 0.051(2) 0.052(2) 0.0075(17) 0.0100(16) -0.0053(16) C16 0.066(3) 0.073(3) 0.071(3) 0.010(2) 0.021(2) -0.011(2) C17 0.054(3) 0.097(3) 0.071(3) -0.001(3) 0.017(2) -0.003(2) C18 0.058(3) 0.068(3) 0.079(3) 0.001(2) 0.011(2) 0.019(2) C19 0.059(2) 0.051(2) 0.055(2) 0.0050(18) 0.0044(19) 0.0010(18) C20 0.0517(19) 0.0326(16) 0.0373(16) 0.0012(13) -0.0086(14) -0.0164(14) C21 0.067(2) 0.071(3) 0.057(2) -0.023(2) 0.0056(19) -0.031(2) C22 0.120(4) 0.098(4) 0.066(3) -0.035(3) 0.008(3) -0.067(3) C23 0.113(4) 0.091(3) 0.066(3) -0.007(2) -0.021(3) -0.071(3) C24 0.068(3) 0.066(3) 0.085(3) 0.000(2) -0.016(2) -0.040(2) C25 0.053(2) 0.0437(19) 0.071(2) -0.0112(18) -0.0072(18) -0.0172(16) C26 0.0405(17) 0.0319(16) 0.0330(15) -0.0001(13) -0.0028(13) -0.0070(13) C27 0.057(2) 0.057(2) 0.0439(19) 0.0064(16) -0.0133(16) -0.0243(18) C28 0.059(2) 0.069(3) 0.045(2) 0.0015(18) -0.0162(17) -0.0155(19) C29 0.064(2) 0.063(2) 0.0377(19) 0.0093(17) -0.0097(17) -0.0014(19) C30 0.069(2) 0.052(2) 0.052(2) 0.0168(18) -0.0041(19) -0.0206(19) C31 0.053(2) 0.0465(19) 0.0469(19) 0.0072(16) -0.0083(16) -0.0194(16) C32 0.0378(16) 0.0471(18) 0.0310(15) -0.0006(14) -0.0039(13) -0.0216(14) C33 0.064(2) 0.052(2) 0.0414(19) -0.0067(16) -0.0085(16) -0.0237(18) C34 0.090(3) 0.089(3) 0.037(2) -0.014(2) -0.0090(19) -0.038(3) C35 0.087(3) 0.093(3) 0.043(2) 0.018(2) -0.024(2) -0.052(3) C36 0.069(2) 0.061(2) 0.055(2) 0.0179(19) -0.0211(19) -0.034(2) C37 0.0496(19) 0.048(2) 0.0413(18) 0.0046(15) -0.0095(15) -0.0225(16) C38 0.0347(15) 0.0372(16) 0.0322(15) -0.0061(13) -0.0006(12) -0.0130(13) C39 0.057(2) 0.052(2) 0.0418(18) 0.0105(15) -0.0142(16) -0.0287(17) C40 0.063(2) 0.070(2) 0.053(2) 0.0118(19) -0.0226(18) -0.035(2) C41 0.059(2) 0.081(3) 0.060(2) -0.001(2) -0.0143(18) -0.043(2) C42 0.071(2) 0.089(3) 0.049(2) 0.009(2) -0.0082(19) -0.057(2) C43 0.052(2) 0.063(2) 0.0403(18) 0.0056(16) -0.0069(15) -0.0323(18) C44 0.0402(17) 0.0326(16) 0.0340(15) -0.0014(13) -0.0084(13) -0.0107(13) C45 0.0509(19) 0.0407(18) 0.0348(16) -0.0001(14) -0.0101(14) -0.0163(15) C46 0.078(3) 0.0388(19) 0.048(2) 0.0013(16) -0.0171(18) -0.0236(19) C47 0.076(3) 0.0366(19) 0.073(3) -0.0063(18) -0.034(2) -0.0047(19) C48 0.048(2) 0.060(3) 0.096(3) -0.031(2) -0.011(2) 0.0017(19) C49 0.0426(19) 0.046(2) 0.078(3) -0.0178(19) -0.0005(18) -0.0112(16) _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 Cu N1 2.067(2) . ? Cu N2 2.072(2) . ? Cu P1 2.2976(9) . ? Cu P2 2.3075(8) . ? Br1 C2 1.890(3) . ? Br2 C8 1.881(3) . ? P1 C26 1.833(3) . ? P1 C14 1.835(3) . ? P1 C20 1.843(3) . ? P2 C44 1.832(3) . ? P2 C32 1.832(3) . ? P2 C38 1.838(3) . ? N1 C1 1.340(3) . ? N1 C4 1.397(3) . ? N2 C9 1.340(3) . ? N2 C6 1.400(3) . ? C1 C2 1.416(4) . ? C1 C10 1.483(4) . ? C2 C3 1.367(4) . ? C3 C4 1.432(4) . ? C3 C11 1.503(4) . ? C4 C5 1.389(4) . ? C5 C6 1.385(4) . ? C6 C7 1.440(4) . ? C7 C8 1.369(4) . ? C7 C13 1.501(4) . ? C8 C9 1.407(4) . ? C9 C12 1.484(4) . ? C14 C19 1.377(4) . ? C14 C15 1.380(4) . ? C15 C16 1.386(5) . ? C16 C17 1.348(6) . ? C17 C18 1.368(6) . ? C18 C19 1.380(5) . ? C20 C21 1.379(4) . ? C20 C25 1.381(5) . ? C21 C22 1.378(5) . ? C22 C23 1.372(6) . ? C23 C24 1.361(6) . ? C24 C25 1.380(5) . ? C26 C27 1.379(4) . ? C26 C31 1.391(4) . ? C27 C28 1.383(5) . ? C28 C29 1.376(5) . ? C29 C30 1.362(5) . ? C30 C31 1.384(5) . ? C32 C33 1.392(4) . ? C32 C37 1.392(4) . ? C33 C34 1.391(5) . ? C34 C35 1.371(6) . ? C35 C36 1.380(5) . ? C36 C37 1.375(4) . ? C38 C43 1.386(4) . ? C38 C39 1.392(4) . ? C39 C40 1.378(4) . ? C40 C41 1.382(5) . ? C41 C42 1.376(5) . ? C42 C43 1.385(4) . ? C44 C45 1.381(4) . ? C44 C49 1.384(4) . ? C45 C46 1.385(4) . ? C46 C47 1.367(5) . ? C47 C48 1.379(5) . ? C48 C49 1.381(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 N1 Cu N2 95.05(9) . . ? N1 Cu P1 107.29(7) . . ? N2 Cu P1 112.36(7) . . ? N1 Cu P2 113.55(7) . . ? N2 Cu P2 106.18(7) . . ? P1 Cu P2 119.71(3) . . ? C26 P1 C14 101.22(14) . . ? C26 P1 C20 103.07(13) . . ? C14 P1 C20 103.74(14) . . ? C26 P1 Cu 118.70(10) . . ? C14 P1 Cu 113.34(10) . . ? C20 P1 Cu 114.80(11) . . ? C44 P2 C32 103.89(13) . . ? C44 P2 C38 101.04(13) . . ? C32 P2 C38 103.42(12) . . ? C44 P2 Cu 113.30(9) . . ? C32 P2 Cu 112.26(10) . . ? C38 P2 Cu 120.99(9) . . ? C1 N1 C4 106.4(2) . . ? C1 N1 Cu 131.2(2) . . ? C4 N1 Cu 121.69(18) . . ? C9 N2 C6 105.9(2) . . ? C9 N2 Cu 132.35(19) . . ? C6 N2 Cu 121.31(18) . . ? N1 C1 C2 109.5(3) . . ? N1 C1 C10 123.9(3) . . ? C2 C1 C10 126.6(3) . . ? C3 C2 C1 109.7(2) . . ? C3 C2 Br1 125.6(2) . . ? C1 C2 Br1 124.6(2) . . ? C2 C3 C4 104.0(3) . . ? C2 C3 C11 128.6(3) . . ? C4 C3 C11 127.3(3) . . ? C5 C4 N1 124.9(3) . . ? C5 C4 C3 124.7(3) . . ? N1 C4 C3 110.4(2) . . ? C6 C5 C4 131.3(3) . . ? C5 C6 N2 125.1(3) . . ? C5 C6 C7 124.3(3) . . ? N2 C6 C7 110.6(2) . . ? C8 C7 C6 103.5(3) . . ? C8 C7 C13 128.5(3) . . ? C6 C7 C13 128.0(3) . . ? C7 C8 C9 109.9(2) . . ? C7 C8 Br2 126.2(2) . . ? C9 C8 Br2 123.9(2) . . ? N2 C9 C8 110.1(2) . . ? N2 C9 C12 124.4(3) . . ? C8 C9 C12 125.5(3) . . ? C19 C14 C15 118.2(3) . . ? C19 C14 P1 123.7(2) . . ? C15 C14 P1 118.2(2) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 120.9(4) . . ? C16 C17 C18 119.6(4) . . ? C17 C18 C19 120.3(4) . . ? C14 C19 C18 120.8(3) . . ? C21 C20 C25 117.9(3) . . ? C21 C20 P1 123.7(3) . . ? C25 C20 P1 118.3(2) . . ? C22 C21 C20 120.5(4) . . ? C23 C22 C21 120.7(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 119.8(4) . . ? C24 C25 C20 121.5(3) . . ? C27 C26 C31 117.9(3) . . ? C27 C26 P1 118.5(2) . . ? C31 C26 P1 123.5(2) . . ? C26 C27 C28 121.4(3) . . ? C29 C28 C27 120.1(3) . . ? C30 C29 C28 118.9(3) . . ? C29 C30 C31 121.6(3) . . ? C30 C31 C26 120.0(3) . . ? C33 C32 C37 118.4(3) . . ? C33 C32 P2 123.8(2) . . ? C37 C32 P2 117.5(2) . . ? C34 C33 C32 119.7(3) . . ? C35 C34 C33 120.9(4) . . ? C34 C35 C36 119.8(3) . . ? C37 C36 C35 119.8(4) . . ? C36 C37 C32 121.4(3) . . ? C43 C38 C39 117.7(3) . . ? C43 C38 P2 124.3(2) . . ? C39 C38 P2 117.9(2) . . ? C40 C39 C38 121.2(3) . . ? C39 C40 C41 120.4(3) . . ? C42 C41 C40 118.9(3) . . ? C41 C42 C43 120.7(3) . . ? C42 C43 C38 121.0(3) . . ? C45 C44 C49 119.3(3) . . ? C45 C44 P2 118.7(2) . . ? C49 C44 P2 121.9(2) . . ? C44 C45 C46 120.3(3) . . ? C47 C46 C45 120.2(3) . . ? C46 C47 C48 119.9(3) . . ? C47 C48 C49 120.2(4) . . ? C48 C49 C44 120.0(3) . . ? 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 N1 Cu P1 C26 -166.10(13) . . . . ? N2 Cu P1 C26 -62.93(13) . . . . ? P2 Cu P1 C26 62.65(12) . . . . ? N1 Cu P1 C14 -47.55(13) . . . . ? N2 Cu P1 C14 55.62(13) . . . . ? P2 Cu P1 C14 -178.81(11) . . . . ? N1 Cu P1 C20 71.43(13) . . . . ? N2 Cu P1 C20 174.60(12) . . . . ? P2 Cu P1 C20 -59.83(11) . . . . ? N1 Cu P2 C44 47.13(13) . . . . ? N2 Cu P2 C44 -55.96(12) . . . . ? P1 Cu P2 C44 175.60(10) . . . . ? N1 Cu P2 C32 164.44(12) . . . . ? N2 Cu P2 C32 61.35(12) . . . . ? P1 Cu P2 C32 -67.10(11) . . . . ? N1 Cu P2 C38 -72.99(14) . . . . ? N2 Cu P2 C38 -176.09(13) . . . . ? P1 Cu P2 C38 55.47(12) . . . . ? N2 Cu N1 C1 -173.1(3) . . . . ? P1 Cu N1 C1 -57.7(3) . . . . ? P2 Cu N1 C1 76.8(3) . . . . ? N2 Cu N1 C4 -3.8(2) . . . . ? P1 Cu N1 C4 111.5(2) . . . . ? P2 Cu N1 C4 -113.9(2) . . . . ? N1 Cu N2 C9 -173.9(3) . . . . ? P1 Cu N2 C9 75.1(3) . . . . ? P2 Cu N2 C9 -57.6(3) . . . . ? N1 Cu N2 C6 -3.1(2) . . . . ? P1 Cu N2 C6 -114.1(2) . . . . ? P2 Cu N2 C6 113.2(2) . . . . ? C4 N1 C1 C2 -0.4(3) . . . . ? Cu N1 C1 C2 170.1(2) . . . . ? C4 N1 C1 C10 -179.7(3) . . . . ? Cu N1 C1 C10 -9.2(5) . . . . ? N1 C1 C2 C3 0.3(4) . . . . ? C10 C1 C2 C3 179.6(3) . . . . ? N1 C1 C2 Br1 177.6(2) . . . . ? C10 C1 C2 Br1 -3.1(5) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? Br1 C2 C3 C4 -177.4(2) . . . . ? C1 C2 C3 C11 -179.2(3) . . . . ? Br1 C2 C3 C11 3.5(5) . . . . ? C1 N1 C4 C5 178.9(3) . . . . ? Cu N1 C4 C5 7.3(4) . . . . ? C1 N1 C4 C3 0.3(3) . . . . ? Cu N1 C4 C3 -171.33(19) . . . . ? C2 C3 C4 C5 -178.7(3) . . . . ? C11 C3 C4 C5 0.3(5) . . . . ? C2 C3 C4 N1 -0.1(3) . . . . ? C11 C3 C4 N1 179.0(3) . . . . ? N1 C4 C5 C6 -3.4(5) . . . . ? C3 C4 C5 C6 175.0(3) . . . . ? C4 C5 C6 N2 -5.2(5) . . . . ? C4 C5 C6 C7 175.1(3) . . . . ? C9 N2 C6 C5 -179.5(3) . . . . ? Cu N2 C6 C5 7.6(4) . . . . ? C9 N2 C6 C7 0.2(3) . . . . ? Cu N2 C6 C7 -172.7(2) . . . . ? C5 C6 C7 C8 -179.6(3) . . . . ? N2 C6 C7 C8 0.7(3) . . . . ? C5 C6 C7 C13 0.5(5) . . . . ? N2 C6 C7 C13 -179.2(3) . . . . ? C6 C7 C8 C9 -1.3(3) . . . . ? C13 C7 C8 C9 178.5(3) . . . . ? C6 C7 C8 Br2 -179.6(2) . . . . ? C13 C7 C8 Br2 0.2(5) . . . . ? C6 N2 C9 C8 -1.0(3) . . . . ? Cu N2 C9 C8 170.8(2) . . . . ? C6 N2 C9 C12 178.3(3) . . . . ? Cu N2 C9 C12 -9.8(4) . . . . ? C7 C8 C9 N2 1.5(4) . . . . ? Br2 C8 C9 N2 179.9(2) . . . . ? C7 C8 C9 C12 -177.8(3) . . . . ? Br2 C8 C9 C12 0.6(4) . . . . ? C26 P1 C14 C19 -28.5(3) . . . . ? C20 P1 C14 C19 78.2(3) . . . . ? Cu P1 C14 C19 -156.7(3) . . . . ? C26 P1 C14 C15 150.3(3) . . . . ? C20 P1 C14 C15 -103.1(3) . . . . ? Cu P1 C14 C15 22.1(3) . . . . ? C19 C14 C15 C16 -1.0(6) . . . . ? P1 C14 C15 C16 -179.8(3) . . . . ? C14 C15 C16 C17 0.5(7) . . . . ? C15 C16 C17 C18 0.6(8) . . . . ? C16 C17 C18 C19 -1.1(8) . . . . ? C15 C14 C19 C18 0.5(6) . . . . ? P1 C14 C19 C18 179.3(3) . . . . ? C17 C18 C19 C14 0.5(7) . . . . ? C26 P1 C20 C21 93.6(3) . . . . ? C14 P1 C20 C21 -11.6(3) . . . . ? Cu P1 C20 C21 -135.8(3) . . . . ? C26 P1 C20 C25 -89.6(3) . . . . ? C14 P1 C20 C25 165.2(3) . . . . ? Cu P1 C20 C25 40.9(3) . . . . ? C25 C20 C21 C22 -0.2(5) . . . . ? P1 C20 C21 C22 176.6(3) . . . . ? C20 C21 C22 C23 -0.4(7) . . . . ? C21 C22 C23 C24 1.0(7) . . . . ? C22 C23 C24 C25 -1.0(7) . . . . ? C23 C24 C25 C20 0.4(6) . . . . ? C21 C20 C25 C24 0.2(5) . . . . ? P1 C20 C25 C24 -176.8(3) . . . . ? C14 P1 C26 C27 -56.8(3) . . . . ? C20 P1 C26 C27 -163.9(3) . . . . ? Cu P1 C26 C27 67.9(3) . . . . ? C14 P1 C26 C31 126.6(3) . . . . ? C20 P1 C26 C31 19.4(3) . . . . ? Cu P1 C26 C31 -108.8(3) . . . . ? C31 C26 C27 C28 -1.6(5) . . . . ? P1 C26 C27 C28 -178.4(3) . . . . ? C26 C27 C28 C29 2.0(5) . . . . ? C27 C28 C29 C30 -0.9(6) . . . . ? C28 C29 C30 C31 -0.4(6) . . . . ? C29 C30 C31 C26 0.7(5) . . . . ? C27 C26 C31 C30 0.2(5) . . . . ? P1 C26 C31 C30 176.9(3) . . . . ? C44 P2 C32 C33 2.6(3) . . . . ? C38 P2 C32 C33 107.8(3) . . . . ? Cu P2 C32 C33 -120.2(2) . . . . ? C44 P2 C32 C37 177.6(2) . . . . ? C38 P2 C32 C37 -77.3(2) . . . . ? Cu P2 C32 C37 54.8(2) . . . . ? C37 C32 C33 C34 -0.8(5) . . . . ? P2 C32 C33 C34 174.0(3) . . . . ? C32 C33 C34 C35 0.7(6) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C34 C35 C36 C37 -0.7(6) . . . . ? C35 C36 C37 C32 0.6(5) . . . . ? C33 C32 C37 C36 0.2(4) . . . . ? P2 C32 C37 C36 -175.0(2) . . . . ? C44 P2 C38 C43 124.8(3) . . . . ? C32 P2 C38 C43 17.4(3) . . . . ? Cu P2 C38 C43 -109.3(3) . . . . ? C44 P2 C38 C39 -58.8(3) . . . . ? C32 P2 C38 C39 -166.2(2) . . . . ? Cu P2 C38 C39 67.1(3) . . . . ? C43 C38 C39 C40 -0.1(5) . . . . ? P2 C38 C39 C40 -176.7(3) . . . . ? C38 C39 C40 C41 1.1(6) . . . . ? C39 C40 C41 C42 -1.4(6) . . . . ? C40 C41 C42 C43 0.6(6) . . . . ? C41 C42 C43 C38 0.5(6) . . . . ? C39 C38 C43 C42 -0.7(5) . . . . ? P2 C38 C43 C42 175.7(3) . . . . ? C32 P2 C44 C45 -110.4(2) . . . . ? C38 P2 C44 C45 142.7(2) . . . . ? Cu P2 C44 C45 11.7(3) . . . . ? C32 P2 C44 C49 69.3(3) . . . . ? C38 P2 C44 C49 -37.6(3) . . . . ? Cu P2 C44 C49 -168.6(2) . . . . ? C49 C44 C45 C46 -0.1(5) . . . . ? P2 C44 C45 C46 179.6(2) . . . . ? C44 C45 C46 C47 0.3(5) . . . . ? C45 C46 C47 C48 -0.3(5) . . . . ? C46 C47 C48 C49 0.0(6) . . . . ? C47 C48 C49 C44 0.1(6) . . . . ? C45 C44 C49 C48 -0.1(5) . . . . ? P2 C44 C49 C48 -179.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.587 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.102 data_s311 _database_code_depnum_ccdc_archive 'CCDC 871238' #TrackingRef 'S311.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H43 Cu N2 O P2' _chemical_formula_weight 801.33 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0197(15) _cell_length_b 23.423(3) _cell_length_c 15.859(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.414(2) _cell_angle_gamma 90.00 _cell_volume 4075.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 2317 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 20.64 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8406 _exptl_absorpt_correction_T_max 0.9134 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22773 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.07 _reflns_number_total 8024 _reflns_number_gt 4858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0588P)^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 8024 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.82980(4) 0.84613(2) 0.82134(3) 0.03916(16) Uani 1 1 d . . . N1 N 0.9950(3) 0.85932(13) 0.88736(19) 0.0385(8) Uani 1 1 d . . . N2 N 0.7264(3) 0.88338(13) 0.90520(19) 0.0392(8) Uani 1 1 d . . . P1 P 0.80760(10) 0.90095(4) 0.70007(6) 0.0362(3) Uani 1 1 d . . . P2 P 0.78243(10) 0.75055(4) 0.80503(6) 0.0371(3) Uani 1 1 d . . . O1 O 0.6377(2) 0.81208(11) 0.65805(16) 0.0409(7) Uani 1 1 d . . . C1 C 1.1104(4) 0.84782(17) 0.8727(3) 0.0423(10) Uani 1 1 d . . . C2 C 1.1934(4) 0.86919(18) 0.9386(3) 0.0482(11) Uani 1 1 d . . . H2A H 1.2796 0.8658 0.9422 0.058 Uiso 1 1 calc R . . C3 C 1.1278(4) 0.89543(18) 0.9956(3) 0.0472(11) Uani 1 1 d . . . C4 C 1.0031(4) 0.88961(17) 0.9639(2) 0.0405(10) Uani 1 1 d . . . C5 C 0.9050(4) 0.91347(17) 0.9996(2) 0.0438(11) Uani 1 1 d . . . H5A H 0.9271 0.9347 1.0498 0.053 Uiso 1 1 calc R . . C6 C 0.7806(4) 0.91230(16) 0.9759(2) 0.0399(10) Uani 1 1 d . . . C7 C 0.6882(4) 0.93963(17) 1.0186(3) 0.0461(11) Uani 1 1 d . . . C8 C 0.5805(4) 0.92705(18) 0.9735(3) 0.0524(12) Uani 1 1 d . . . H8A H 0.5019 0.9395 0.9856 0.063 Uiso 1 1 calc R . . C9 C 0.6073(4) 0.89196(17) 0.9050(3) 0.0442(11) Uani 1 1 d . . . C10 C 1.1428(4) 0.8212(2) 0.7927(3) 0.0573(12) Uani 1 1 d . . . H10A H 1.0682 0.8103 0.7579 0.086 Uiso 1 1 calc R . . H10B H 1.1928 0.7872 0.8059 0.086 Uiso 1 1 calc R . . H10C H 1.1888 0.8486 0.7615 0.086 Uiso 1 1 calc R . . C11 C 1.1751(4) 0.9263(2) 1.0758(3) 0.0675(14) Uani 1 1 d . . . H11A H 1.2643 0.9242 1.0828 0.101 Uiso 1 1 calc R . . H11B H 1.1420 0.9083 1.1245 0.101 Uiso 1 1 calc R . . H11C H 1.1495 0.9664 1.0721 0.101 Uiso 1 1 calc R . . C12 C 0.5166(4) 0.8660(2) 0.8392(3) 0.0627(13) Uani 1 1 d . . . H12A H 0.5598 0.8435 0.7993 0.094 Uiso 1 1 calc R . . H12B H 0.4700 0.8964 0.8085 0.094 Uiso 1 1 calc R . . H12C H 0.4608 0.8411 0.8669 0.094 Uiso 1 1 calc R . . C13 C 0.7096(5) 0.9764(2) 1.0967(3) 0.0709(15) Uani 1 1 d . . . H13A H 0.6312 0.9901 1.1133 0.106 Uiso 1 1 calc R . . H13B H 0.7607 1.0091 1.0847 0.106 Uiso 1 1 calc R . . H13C H 0.7507 0.9539 1.1431 0.106 Uiso 1 1 calc R . . C14 C 0.6717(4) 0.94591(16) 0.6885(3) 0.0402(10) Uani 1 1 d . . . C15 C 0.5833(4) 0.9453(2) 0.6216(3) 0.0615(13) Uani 1 1 d . . . H15A H 0.5877 0.9179 0.5778 0.074 Uiso 1 1 calc R . . C16 C 0.4874(5) 0.9841(2) 0.6168(4) 0.0805(17) Uani 1 1 d . . . H16A H 0.4274 0.9837 0.5696 0.097 Uiso 1 1 calc R . . C17 C 0.4801(5) 1.0229(2) 0.6808(4) 0.0777(17) Uani 1 1 d . . . H17A H 0.4142 1.0492 0.6782 0.093 Uiso 1 1 calc R . . C18 C 0.5663(5) 1.0242(2) 0.7480(4) 0.0700(15) Uani 1 1 d . . . H18A H 0.5614 1.0516 0.7917 0.084 Uiso 1 1 calc R . . C19 C 0.6605(4) 0.98560(18) 0.7522(3) 0.0551(12) Uani 1 1 d . . . H19A H 0.7194 0.9861 0.7999 0.066 Uiso 1 1 calc R . . C20 C 0.9214(4) 0.95511(16) 0.6782(2) 0.0383(10) Uani 1 1 d . . . C21 C 0.8952(4) 0.99838(19) 0.6197(3) 0.0586(13) Uani 1 1 d . . . H21A H 0.8151 1.0016 0.5921 0.070 Uiso 1 1 calc R . . C22 C 0.9830(5) 1.0365(2) 0.6011(3) 0.0723(15) Uani 1 1 d . . . H22A H 0.9628 1.0665 0.5618 0.087 Uiso 1 1 calc R . . C23 C 1.0988(5) 1.0318(2) 0.6383(3) 0.0660(14) Uani 1 1 d . . . H23A H 1.1601 1.0575 0.6235 0.079 Uiso 1 1 calc R . . C24 C 1.1267(5) 0.9901(2) 0.6971(3) 0.0688(14) Uani 1 1 d . . . H24A H 1.2074 0.9868 0.7234 0.083 Uiso 1 1 calc R . . C25 C 1.0368(4) 0.9526(2) 0.7182(3) 0.0578(13) Uani 1 1 d . . . H25A H 1.0557 0.9247 0.7610 0.069 Uiso 1 1 calc R . . C26 C 0.8005(4) 0.85811(15) 0.6033(2) 0.0355(9) Uani 1 1 d . . . C27 C 0.8829(4) 0.86280(18) 0.5425(3) 0.0511(12) Uani 1 1 d . . . H27A H 0.9415 0.8927 0.5467 0.061 Uiso 1 1 calc R . . C28 C 0.8808(5) 0.8243(2) 0.4755(3) 0.0576(13) Uani 1 1 d . . . H28A H 0.9384 0.8275 0.4348 0.069 Uiso 1 1 calc R . . C29 C 0.7951(4) 0.78190(19) 0.4687(3) 0.0541(12) Uani 1 1 d . . . H29A H 0.7931 0.7560 0.4225 0.065 Uiso 1 1 calc R . . C30 C 0.7114(4) 0.77615(18) 0.5276(2) 0.0475(11) Uani 1 1 d . . . H30A H 0.6518 0.7468 0.5221 0.057 Uiso 1 1 calc R . . C31 C 0.7162(4) 0.81358(16) 0.5941(2) 0.0372(10) Uani 1 1 d . . . C32 C 0.5852(4) 0.75993(17) 0.6772(2) 0.0407(10) Uani 1 1 d . . . C33 C 0.4773(4) 0.7442(2) 0.6323(3) 0.0546(12) Uani 1 1 d . . . H33A H 0.4420 0.7679 0.5879 0.066 Uiso 1 1 calc R . . C34 C 0.4207(4) 0.6943(2) 0.6519(3) 0.0610(13) Uani 1 1 d . . . H34A H 0.3465 0.6832 0.6209 0.073 Uiso 1 1 calc R . . C35 C 0.4718(5) 0.6608(2) 0.7161(3) 0.0597(13) Uani 1 1 d . . . H35A H 0.4329 0.6263 0.7299 0.072 Uiso 1 1 calc R . . C36 C 0.5793(4) 0.67679(18) 0.7608(3) 0.0518(12) Uani 1 1 d . . . H36A H 0.6134 0.6528 0.8052 0.062 Uiso 1 1 calc R . . C37 C 0.6404(3) 0.72731(17) 0.7432(2) 0.0378(10) Uani 1 1 d . . . C38 C 0.8982(4) 0.70841(16) 0.7577(3) 0.0411(10) Uani 1 1 d . . . C39 C 0.8854(4) 0.69194(17) 0.6734(3) 0.0520(12) Uani 1 1 d . . . H39A H 0.8101 0.6984 0.6405 0.062 Uiso 1 1 calc R . . C40 C 0.9794(6) 0.6665(2) 0.6364(3) 0.0682(15) Uani 1 1 d . . . H40A H 0.9687 0.6558 0.5783 0.082 Uiso 1 1 calc R . . C41 C 1.0873(5) 0.6564(2) 0.6823(4) 0.0728(16) Uani 1 1 d . . . H41A H 1.1523 0.6393 0.6562 0.087 Uiso 1 1 calc R . . C42 C 1.1033(5) 0.6711(2) 0.7669(4) 0.0709(15) Uani 1 1 d . . . H42A H 1.1780 0.6631 0.7997 0.085 Uiso 1 1 calc R . . C43 C 1.0089(4) 0.69768(19) 0.8034(3) 0.0598(13) Uani 1 1 d . . . H43A H 1.0205 0.7088 0.8612 0.072 Uiso 1 1 calc R . . C44 C 0.7668(4) 0.71256(17) 0.9047(2) 0.0410(10) Uani 1 1 d . . . C45 C 0.7097(4) 0.74095(19) 0.9670(3) 0.0495(11) Uani 1 1 d . . . H45A H 0.6860 0.7797 0.9589 0.059 Uiso 1 1 calc R . . C46 C 0.6873(5) 0.7130(2) 1.0409(3) 0.0660(14) Uani 1 1 d . . . H46A H 0.6476 0.7327 1.0828 0.079 Uiso 1 1 calc R . . C47 C 0.7215(5) 0.6572(3) 1.0543(3) 0.0709(15) Uani 1 1 d . . . H47A H 0.7049 0.6383 1.1049 0.085 Uiso 1 1 calc R . . C48 C 0.7794(5) 0.6294(2) 0.9946(3) 0.0708(15) Uani 1 1 d . . . H48A H 0.8043 0.5909 1.0043 0.085 Uiso 1 1 calc R . . C49 C 0.8027(4) 0.6561(2) 0.9198(3) 0.0590(13) Uani 1 1 d . . . H49A H 0.8433 0.6359 0.8787 0.071 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 Cu 0.0387(3) 0.0430(3) 0.0358(3) -0.0057(2) 0.0037(2) -0.0009(2) N1 0.042(2) 0.0361(19) 0.0375(18) -0.0027(15) 0.0021(16) -0.0066(16) N2 0.039(2) 0.0397(19) 0.0410(19) -0.0037(16) 0.0127(17) -0.0008(16) P1 0.0401(7) 0.0329(6) 0.0355(6) -0.0016(5) 0.0038(5) -0.0035(5) P2 0.0381(7) 0.0364(6) 0.0368(6) -0.0021(5) 0.0031(5) -0.0020(5) O1 0.0431(18) 0.0387(16) 0.0407(15) -0.0025(13) 0.0024(14) -0.0092(13) C1 0.041(3) 0.039(2) 0.047(2) 0.006(2) 0.002(2) 0.000(2) C2 0.035(3) 0.048(3) 0.060(3) 0.009(2) -0.005(2) -0.003(2) C3 0.049(3) 0.045(3) 0.045(3) 0.010(2) -0.008(2) -0.012(2) C4 0.046(3) 0.041(2) 0.034(2) 0.0045(19) -0.002(2) -0.006(2) C5 0.059(3) 0.040(2) 0.032(2) 0.0006(19) 0.002(2) -0.009(2) C6 0.055(3) 0.032(2) 0.034(2) 0.0031(18) 0.011(2) -0.005(2) C7 0.062(3) 0.037(2) 0.044(2) 0.002(2) 0.025(2) -0.001(2) C8 0.054(3) 0.050(3) 0.058(3) 0.007(2) 0.030(3) 0.010(2) C9 0.045(3) 0.047(3) 0.042(2) 0.006(2) 0.015(2) 0.003(2) C10 0.051(3) 0.057(3) 0.065(3) -0.006(2) 0.009(2) 0.000(2) C11 0.068(4) 0.075(3) 0.056(3) -0.003(3) -0.015(3) -0.017(3) C12 0.041(3) 0.080(4) 0.068(3) -0.008(3) 0.010(3) -0.003(3) C13 0.106(4) 0.053(3) 0.059(3) -0.015(2) 0.038(3) -0.002(3) C14 0.039(3) 0.036(2) 0.045(2) -0.001(2) 0.002(2) -0.0053(19) C15 0.061(3) 0.052(3) 0.070(3) -0.016(3) -0.007(3) 0.008(3) C16 0.062(4) 0.067(4) 0.106(4) -0.021(3) -0.028(3) 0.014(3) C17 0.046(3) 0.053(3) 0.133(5) -0.017(3) 0.004(3) 0.012(3) C18 0.064(4) 0.055(3) 0.092(4) -0.026(3) 0.006(3) 0.007(3) C19 0.055(3) 0.050(3) 0.060(3) -0.015(2) 0.002(2) -0.001(2) C20 0.044(3) 0.032(2) 0.039(2) 0.0000(18) 0.006(2) -0.0075(19) C21 0.051(3) 0.057(3) 0.067(3) 0.020(3) 0.002(3) -0.012(2) C22 0.071(4) 0.062(3) 0.085(4) 0.027(3) 0.015(3) -0.009(3) C23 0.072(4) 0.053(3) 0.075(4) 0.004(3) 0.017(3) -0.025(3) C24 0.052(3) 0.077(4) 0.075(3) 0.008(3) -0.009(3) -0.021(3) C25 0.052(3) 0.058(3) 0.060(3) 0.016(2) -0.010(2) -0.014(2) C26 0.045(3) 0.030(2) 0.031(2) 0.0036(17) -0.0022(19) 0.0009(18) C27 0.060(3) 0.044(3) 0.051(3) 0.000(2) 0.016(2) -0.008(2) C28 0.069(4) 0.060(3) 0.047(3) -0.007(2) 0.023(3) -0.004(3) C29 0.075(4) 0.050(3) 0.037(2) -0.012(2) 0.007(3) 0.001(3) C30 0.058(3) 0.042(2) 0.041(2) -0.006(2) -0.004(2) -0.007(2) C31 0.040(3) 0.039(2) 0.033(2) 0.0019(18) 0.0018(19) -0.0012(19) C32 0.041(3) 0.041(2) 0.042(2) -0.005(2) 0.008(2) -0.011(2) C33 0.045(3) 0.063(3) 0.054(3) 0.004(2) -0.007(2) -0.006(2) C34 0.047(3) 0.068(3) 0.067(3) -0.002(3) -0.002(3) -0.022(3) C35 0.060(3) 0.052(3) 0.067(3) -0.001(3) 0.007(3) -0.030(3) C36 0.062(3) 0.048(3) 0.046(3) -0.002(2) 0.008(2) -0.016(2) C37 0.033(2) 0.042(2) 0.039(2) -0.0060(19) 0.0095(19) -0.0079(19) C38 0.039(3) 0.030(2) 0.055(3) -0.0013(19) 0.008(2) -0.0023(19) C39 0.058(3) 0.046(3) 0.055(3) 0.001(2) 0.017(2) 0.004(2) C40 0.082(4) 0.058(3) 0.070(3) -0.012(3) 0.033(3) -0.002(3) C41 0.062(4) 0.044(3) 0.119(5) -0.013(3) 0.043(4) -0.005(3) C42 0.042(3) 0.053(3) 0.117(5) -0.010(3) 0.003(3) 0.002(2) C43 0.048(3) 0.056(3) 0.075(3) -0.017(3) 0.004(3) 0.001(2) C44 0.039(3) 0.042(2) 0.041(2) 0.0027(19) -0.001(2) -0.005(2) C45 0.048(3) 0.055(3) 0.046(3) 0.003(2) 0.005(2) -0.003(2) C46 0.069(4) 0.081(4) 0.049(3) 0.001(3) 0.008(3) -0.014(3) C47 0.083(4) 0.081(4) 0.048(3) 0.018(3) 0.004(3) -0.021(3) C48 0.085(4) 0.055(3) 0.070(4) 0.022(3) -0.010(3) -0.005(3) C49 0.070(3) 0.052(3) 0.054(3) 0.001(2) 0.003(3) 0.003(3) _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 Cu N2 2.028(3) . ? Cu N1 2.036(3) . ? Cu P1 2.3061(11) . ? Cu P2 2.3078(12) . ? N1 C1 1.342(5) . ? N1 C4 1.402(5) . ? N2 C9 1.327(5) . ? N2 C6 1.395(5) . ? P1 C14 1.825(4) . ? P1 C26 1.828(4) . ? P1 C20 1.839(4) . ? P2 C38 1.830(4) . ? P2 C44 1.837(4) . ? P2 C37 1.849(4) . ? O1 C31 1.394(4) . ? O1 C32 1.397(4) . ? C1 C2 1.413(5) . ? C1 C10 1.488(6) . ? C2 C3 1.357(6) . ? C3 C4 1.425(5) . ? C3 C11 1.512(6) . ? C4 C5 1.384(5) . ? C5 C6 1.387(5) . ? C6 C7 1.427(5) . ? C7 C8 1.360(6) . ? C7 C13 1.509(6) . ? C8 C9 1.415(5) . ? C9 C12 1.504(6) . ? C14 C15 1.371(6) . ? C14 C19 1.387(5) . ? C15 C16 1.391(6) . ? C16 C17 1.370(7) . ? C17 C18 1.359(7) . ? C18 C19 1.374(6) . ? C20 C25 1.368(5) . ? C20 C21 1.386(5) . ? C21 C22 1.370(6) . ? C22 C23 1.359(7) . ? C23 C24 1.365(7) . ? C24 C25 1.389(6) . ? C26 C27 1.390(5) . ? C26 C31 1.396(5) . ? C27 C28 1.391(6) . ? C28 C29 1.368(6) . ? C29 C30 1.379(6) . ? C30 C31 1.369(5) . ? C32 C33 1.377(5) . ? C32 C37 1.390(5) . ? C33 C34 1.374(6) . ? C34 C35 1.365(6) . ? C35 C36 1.375(6) . ? C36 C37 1.402(5) . ? C38 C43 1.382(6) . ? C38 C39 1.386(6) . ? C39 C40 1.374(6) . ? C40 C41 1.355(7) . ? C41 C42 1.381(7) . ? C42 C43 1.384(6) . ? C44 C45 1.389(5) . ? C44 C49 1.395(6) . ? C45 C46 1.384(6) . ? C46 C47 1.370(7) . ? C47 C48 1.357(7) . ? C48 C49 1.387(6) . ? 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 N2 Cu N1 97.35(13) . . ? N2 Cu P1 106.58(10) . . ? N1 Cu P1 111.33(9) . . ? N2 Cu P2 110.82(9) . . ? N1 Cu P2 112.74(9) . . ? P1 Cu P2 116.20(4) . . ? C1 N1 C4 105.5(3) . . ? C1 N1 Cu 134.2(3) . . ? C4 N1 Cu 120.2(3) . . ? C9 N2 C6 106.1(3) . . ? C9 N2 Cu 132.9(3) . . ? C6 N2 Cu 120.7(3) . . ? C14 P1 C26 105.23(18) . . ? C14 P1 C20 98.65(18) . . ? C26 P1 C20 101.31(17) . . ? C14 P1 Cu 115.23(13) . . ? C26 P1 Cu 112.76(12) . . ? C20 P1 Cu 121.38(14) . . ? C38 P2 C44 102.59(19) . . ? C38 P2 C37 102.23(18) . . ? C44 P2 C37 99.80(18) . . ? C38 P2 Cu 114.22(13) . . ? C44 P2 Cu 114.34(13) . . ? C37 P2 Cu 121.09(14) . . ? C31 O1 C32 118.5(3) . . ? N1 C1 C2 111.1(4) . . ? N1 C1 C10 122.6(4) . . ? C2 C1 C10 126.0(4) . . ? C3 C2 C1 107.7(4) . . ? C2 C3 C4 106.1(4) . . ? C2 C3 C11 127.9(4) . . ? C4 C3 C11 125.9(4) . . ? C5 C4 N1 124.7(4) . . ? C5 C4 C3 125.6(4) . . ? N1 C4 C3 109.6(4) . . ? C4 C5 C6 132.2(4) . . ? C5 C6 N2 124.4(4) . . ? C5 C6 C7 126.4(4) . . ? N2 C6 C7 109.2(4) . . ? C8 C7 C6 106.2(4) . . ? C8 C7 C13 128.1(4) . . ? C6 C7 C13 125.7(4) . . ? C7 C8 C9 107.1(4) . . ? N2 C9 C8 111.4(4) . . ? N2 C9 C12 122.2(4) . . ? C8 C9 C12 126.5(4) . . ? C15 C14 C19 117.7(4) . . ? C15 C14 P1 126.0(3) . . ? C19 C14 P1 116.3(3) . . ? C14 C15 C16 121.1(4) . . ? C17 C16 C15 119.3(5) . . ? C18 C17 C16 120.7(5) . . ? C17 C18 C19 119.5(5) . . ? C18 C19 C14 121.7(5) . . ? C25 C20 C21 117.9(4) . . ? C25 C20 P1 120.2(3) . . ? C21 C20 P1 121.9(3) . . ? C22 C21 C20 121.0(5) . . ? C23 C22 C21 120.4(5) . . ? C22 C23 C24 119.8(5) . . ? C23 C24 C25 119.9(5) . . ? C20 C25 C24 120.9(4) . . ? C27 C26 C31 117.3(4) . . ? C27 C26 P1 124.0(3) . . ? C31 C26 P1 118.3(3) . . ? C26 C27 C28 120.9(4) . . ? C29 C28 C27 119.5(4) . . ? C28 C29 C30 121.2(4) . . ? C31 C30 C29 118.7(4) . . ? C30 C31 O1 124.3(4) . . ? C30 C31 C26 122.4(4) . . ? O1 C31 C26 113.3(3) . . ? C33 C32 C37 122.5(4) . . ? C33 C32 O1 118.5(4) . . ? C37 C32 O1 118.9(4) . . ? C34 C33 C32 119.9(4) . . ? C35 C34 C33 119.6(4) . . ? C34 C35 C36 120.2(4) . . ? C35 C36 C37 122.3(4) . . ? C32 C37 C36 115.5(4) . . ? C32 C37 P2 121.7(3) . . ? C36 C37 P2 122.8(3) . . ? C43 C38 C39 117.4(4) . . ? C43 C38 P2 119.9(3) . . ? C39 C38 P2 122.3(4) . . ? C40 C39 C38 121.4(5) . . ? C41 C40 C39 120.3(5) . . ? C40 C41 C42 120.3(5) . . ? C43 C42 C41 119.1(5) . . ? C38 C43 C42 121.6(5) . . ? C45 C44 C49 118.2(4) . . ? C45 C44 P2 117.8(3) . . ? C49 C44 P2 123.9(3) . . ? C46 C45 C44 120.3(4) . . ? C47 C46 C45 120.9(5) . . ? C48 C47 C46 119.4(5) . . ? C47 C48 C49 121.1(5) . . ? C48 C49 C44 120.1(4) . . ? 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 N2 Cu N1 C1 -178.3(4) . . . . ? P1 Cu N1 C1 -67.3(4) . . . . ? P2 Cu N1 C1 65.4(4) . . . . ? N2 Cu N1 C4 -2.9(3) . . . . ? P1 Cu N1 C4 108.1(3) . . . . ? P2 Cu N1 C4 -119.2(3) . . . . ? N1 Cu N2 C9 179.0(4) . . . . ? P1 Cu N2 C9 64.1(4) . . . . ? P2 Cu N2 C9 -63.3(4) . . . . ? N1 Cu N2 C6 6.7(3) . . . . ? P1 Cu N2 C6 -108.2(3) . . . . ? P2 Cu N2 C6 124.5(3) . . . . ? N2 Cu P1 C14 -20.84(18) . . . . ? N1 Cu P1 C14 -125.89(17) . . . . ? P2 Cu P1 C14 103.21(15) . . . . ? N2 Cu P1 C26 -141.68(17) . . . . ? N1 Cu P1 C26 113.27(17) . . . . ? P2 Cu P1 C26 -17.63(15) . . . . ? N2 Cu P1 C20 97.98(18) . . . . ? N1 Cu P1 C20 -7.07(18) . . . . ? P2 Cu P1 C20 -137.97(15) . . . . ? N2 Cu P2 C38 -162.31(18) . . . . ? N1 Cu P2 C38 -54.38(19) . . . . ? P1 Cu P2 C38 75.85(17) . . . . ? N2 Cu P2 C44 -44.55(18) . . . . ? N1 Cu P2 C44 63.38(18) . . . . ? P1 Cu P2 C44 -166.39(15) . . . . ? N2 Cu P2 C37 74.85(17) . . . . ? N1 Cu P2 C37 -177.22(17) . . . . ? P1 Cu P2 C37 -46.99(15) . . . . ? C4 N1 C1 C2 0.8(4) . . . . ? Cu N1 C1 C2 176.7(3) . . . . ? C4 N1 C1 C10 -173.4(4) . . . . ? Cu N1 C1 C10 2.4(6) . . . . ? N1 C1 C2 C3 -0.7(5) . . . . ? C10 C1 C2 C3 173.3(4) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C1 C2 C3 C11 -178.3(4) . . . . ? C1 N1 C4 C5 175.2(4) . . . . ? Cu N1 C4 C5 -1.4(5) . . . . ? C1 N1 C4 C3 -0.7(4) . . . . ? Cu N1 C4 C3 -177.3(2) . . . . ? C2 C3 C4 C5 -175.5(4) . . . . ? C11 C3 C4 C5 3.0(7) . . . . ? C2 C3 C4 N1 0.3(4) . . . . ? C11 C3 C4 N1 178.8(4) . . . . ? N1 C4 C5 C6 3.8(7) . . . . ? C3 C4 C5 C6 179.0(4) . . . . ? C4 C5 C6 N2 0.9(7) . . . . ? C4 C5 C6 C7 -179.4(4) . . . . ? C9 N2 C6 C5 179.2(4) . . . . ? Cu N2 C6 C5 -6.7(5) . . . . ? C9 N2 C6 C7 -0.6(4) . . . . ? Cu N2 C6 C7 173.5(2) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? N2 C6 C7 C8 -0.1(4) . . . . ? C5 C6 C7 C13 1.8(6) . . . . ? N2 C6 C7 C13 -178.4(4) . . . . ? C6 C7 C8 C9 0.8(4) . . . . ? C13 C7 C8 C9 179.0(4) . . . . ? C6 N2 C9 C8 1.1(4) . . . . ? Cu N2 C9 C8 -172.0(3) . . . . ? C6 N2 C9 C12 -178.3(4) . . . . ? Cu N2 C9 C12 8.6(6) . . . . ? C7 C8 C9 N2 -1.2(5) . . . . ? C7 C8 C9 C12 178.2(4) . . . . ? C26 P1 C14 C15 1.7(4) . . . . ? C20 P1 C14 C15 106.0(4) . . . . ? Cu P1 C14 C15 -123.2(4) . . . . ? C26 P1 C14 C19 -175.7(3) . . . . ? C20 P1 C14 C19 -71.4(3) . . . . ? Cu P1 C14 C19 59.4(3) . . . . ? C19 C14 C15 C16 1.5(7) . . . . ? P1 C14 C15 C16 -175.8(4) . . . . ? C14 C15 C16 C17 -1.1(8) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? C16 C17 C18 C19 -1.0(8) . . . . ? C17 C18 C19 C14 1.5(7) . . . . ? C15 C14 C19 C18 -1.7(7) . . . . ? P1 C14 C19 C18 175.9(4) . . . . ? C14 P1 C20 C25 146.7(4) . . . . ? C26 P1 C20 C25 -105.8(4) . . . . ? Cu P1 C20 C25 19.9(4) . . . . ? C14 P1 C20 C21 -35.3(4) . . . . ? C26 P1 C20 C21 72.3(4) . . . . ? Cu P1 C20 C21 -162.0(3) . . . . ? C25 C20 C21 C22 1.6(7) . . . . ? P1 C20 C21 C22 -176.6(4) . . . . ? C20 C21 C22 C23 1.6(8) . . . . ? C21 C22 C23 C24 -2.5(8) . . . . ? C22 C23 C24 C25 0.3(8) . . . . ? C21 C20 C25 C24 -3.8(7) . . . . ? P1 C20 C25 C24 174.4(4) . . . . ? C23 C24 C25 C20 2.9(8) . . . . ? C14 P1 C26 C27 113.7(4) . . . . ? C20 P1 C26 C27 11.4(4) . . . . ? Cu P1 C26 C27 -119.9(3) . . . . ? C14 P1 C26 C31 -73.9(3) . . . . ? C20 P1 C26 C31 -176.2(3) . . . . ? Cu P1 C26 C31 52.5(3) . . . . ? C31 C26 C27 C28 -0.2(6) . . . . ? P1 C26 C27 C28 172.3(3) . . . . ? C26 C27 C28 C29 1.1(7) . . . . ? C27 C28 C29 C30 -0.8(7) . . . . ? C28 C29 C30 C31 -0.5(7) . . . . ? C29 C30 C31 O1 -179.5(4) . . . . ? C29 C30 C31 C26 1.5(6) . . . . ? C32 O1 C31 C30 26.6(6) . . . . ? C32 O1 C31 C26 -154.3(3) . . . . ? C27 C26 C31 C30 -1.2(6) . . . . ? P1 C26 C31 C30 -174.1(3) . . . . ? C27 C26 C31 O1 179.7(3) . . . . ? P1 C26 C31 O1 6.8(5) . . . . ? C31 O1 C32 C33 -87.6(5) . . . . ? C31 O1 C32 C37 95.6(4) . . . . ? C37 C32 C33 C34 -0.6(7) . . . . ? O1 C32 C33 C34 -177.3(4) . . . . ? C32 C33 C34 C35 0.3(7) . . . . ? C33 C34 C35 C36 -0.1(7) . . . . ? C34 C35 C36 C37 0.1(7) . . . . ? C33 C32 C37 C36 0.6(6) . . . . ? O1 C32 C37 C36 177.3(3) . . . . ? C33 C32 C37 P2 -177.8(3) . . . . ? O1 C32 C37 P2 -1.1(5) . . . . ? C35 C36 C37 C32 -0.4(6) . . . . ? C35 C36 C37 P2 178.0(3) . . . . ? C38 P2 C37 C32 -100.2(3) . . . . ? C44 P2 C37 C32 154.5(3) . . . . ? Cu P2 C37 C32 28.1(4) . . . . ? C38 P2 C37 C36 81.5(4) . . . . ? C44 P2 C37 C36 -23.8(4) . . . . ? Cu P2 C37 C36 -150.1(3) . . . . ? C44 P2 C38 C43 -53.9(4) . . . . ? C37 P2 C38 C43 -157.0(3) . . . . ? Cu P2 C38 C43 70.4(4) . . . . ? C44 P2 C38 C39 133.7(3) . . . . ? C37 P2 C38 C39 30.6(4) . . . . ? Cu P2 C38 C39 -102.0(3) . . . . ? C43 C38 C39 C40 -0.7(6) . . . . ? P2 C38 C39 C40 171.9(3) . . . . ? C38 C39 C40 C41 0.5(7) . . . . ? C39 C40 C41 C42 0.8(7) . . . . ? C40 C41 C42 C43 -1.9(8) . . . . ? C39 C38 C43 C42 -0.5(6) . . . . ? P2 C38 C43 C42 -173.3(4) . . . . ? C41 C42 C43 C38 1.8(7) . . . . ? C38 P2 C44 C45 163.6(3) . . . . ? C37 P2 C44 C45 -91.4(3) . . . . ? Cu P2 C44 C45 39.4(4) . . . . ? C38 P2 C44 C49 -20.0(4) . . . . ? C37 P2 C44 C49 85.0(4) . . . . ? Cu P2 C44 C49 -144.2(3) . . . . ? C49 C44 C45 C46 -1.5(6) . . . . ? P2 C44 C45 C46 175.2(3) . . . . ? C44 C45 C46 C47 0.5(7) . . . . ? C45 C46 C47 C48 0.7(8) . . . . ? C46 C47 C48 C49 -1.0(8) . . . . ? C47 C48 C49 C44 0.1(8) . . . . ? C45 C44 C49 C48 1.2(7) . . . . ? P2 C44 C49 C48 -175.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.449 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.065 data_s313 _database_code_depnum_ccdc_archive 'CCDC 871239' #TrackingRef 'S313.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H47 Cu N2 O P2' _chemical_formula_weight 877.43 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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 9.934(2) _cell_length_b 12.945(3) _cell_length_c 19.804(4) _cell_angle_alpha 105.232(4) _cell_angle_beta 94.756(4) _cell_angle_gamma 109.758(4) _cell_volume 2270.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 1121 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 18.31 _exptl_crystal_description flake _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8279 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12927 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.1376 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.11 _reflns_number_total 8797 _reflns_number_gt 4629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0554P)^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 8797 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1535 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cu Cu -0.04058(7) 0.78216(6) 0.73061(3) 0.0403(2) Uani 1 1 d . . . N1 N -0.1681(4) 0.6142(3) 0.69517(19) 0.0352(10) Uani 1 1 d . . . N2 N -0.1268(4) 0.8179(4) 0.8172(2) 0.0373(10) Uani 1 1 d . . . P1 P 0.18500(15) 0.78379(12) 0.78255(7) 0.0392(4) Uani 1 1 d . . . P2 P -0.02783(16) 0.88632(13) 0.65559(7) 0.0422(4) Uani 1 1 d . . . O1 O 0.2532(4) 1.0031(3) 0.74047(18) 0.0451(9) Uani 1 1 d . . . C1 C -0.1659(6) 0.5315(5) 0.6386(3) 0.0411(13) Uani 1 1 d . . . C2 C -0.2393(6) 0.4222(5) 0.6440(3) 0.0476(14) Uani 1 1 d . . . H2A H -0.2500 0.3510 0.6105 0.057 Uiso 1 1 calc R . . C3 C -0.2931(6) 0.4345(4) 0.7053(3) 0.0394(13) Uani 1 1 d . . . C4 C -0.2488(5) 0.5564(4) 0.7387(2) 0.0336(12) Uani 1 1 d . . . C5 C -0.2809(5) 0.6148(4) 0.8028(3) 0.0357(12) Uani 1 1 d . . . C6 C -0.2325(5) 0.7335(5) 0.8384(2) 0.0352(12) Uani 1 1 d . . . C7 C -0.2695(6) 0.7932(5) 0.9024(3) 0.0458(14) Uani 1 1 d . . . C8 C -0.1837(7) 0.9068(5) 0.9190(3) 0.0528(16) Uani 1 1 d . . . H8A H -0.1818 0.9669 0.9592 0.063 Uiso 1 1 calc R . . C9 C -0.0980(6) 0.9199(5) 0.8662(3) 0.0413(13) Uani 1 1 d . . . C10 C -0.0929(6) 0.5572(5) 0.5778(3) 0.0567(16) Uani 1 1 d . . . H10A H -0.0512 0.6408 0.5867 0.085 Uiso 1 1 calc R . . H10B H -0.1648 0.5209 0.5332 0.085 Uiso 1 1 calc R . . H10C H -0.0152 0.5264 0.5739 0.085 Uiso 1 1 calc R . . C11 C -0.3799(7) 0.3325(5) 0.7268(3) 0.0590(17) Uani 1 1 d . . . H11A H -0.3880 0.2611 0.6909 0.089 Uiso 1 1 calc R . . H11B H -0.4774 0.3331 0.7304 0.089 Uiso 1 1 calc R . . H11C H -0.3308 0.3368 0.7730 0.089 Uiso 1 1 calc R . . C12 C 0.0202(7) 1.0284(5) 0.8669(3) 0.0598(17) Uani 1 1 d . . . H12A H 0.0626 1.0137 0.8240 0.090 Uiso 1 1 calc R . . H12B H 0.0960 1.0548 0.9093 0.090 Uiso 1 1 calc R . . H12C H -0.0202 1.0880 0.8676 0.090 Uiso 1 1 calc R . . C13 C -0.3796(8) 0.7487(5) 0.9460(3) 0.075(2) Uani 1 1 d . . . H13A H -0.3751 0.8128 0.9868 0.112 Uiso 1 1 calc R . . H13B H -0.3578 0.6905 0.9632 0.112 Uiso 1 1 calc R . . H13C H -0.4774 0.7138 0.9165 0.112 Uiso 1 1 calc R . . C14 C -0.3797(6) 0.5386(4) 0.8378(3) 0.0397(13) Uani 1 1 d . . . C15 C -0.3212(7) 0.5093(5) 0.8931(3) 0.0529(16) Uani 1 1 d . . . H15A H -0.2186 0.5382 0.9087 0.064 Uiso 1 1 calc R . . C16 C -0.4124(8) 0.4383(5) 0.9252(3) 0.0663(19) Uani 1 1 d . . . H16A H -0.3725 0.4186 0.9630 0.080 Uiso 1 1 calc R . . C17 C -0.5598(9) 0.3964(6) 0.9026(4) 0.072(2) Uani 1 1 d . . . H17A H -0.6219 0.3477 0.9249 0.086 Uiso 1 1 calc R . . C18 C -0.6187(7) 0.4239(5) 0.8481(3) 0.0646(18) Uani 1 1 d . . . H18A H -0.7213 0.3936 0.8323 0.078 Uiso 1 1 calc R . . C19 C -0.5288(6) 0.4956(5) 0.8165(3) 0.0546(16) Uani 1 1 d . . . H19A H -0.5701 0.5158 0.7793 0.065 Uiso 1 1 calc R . . C20 C 0.1563(6) 0.7259(5) 0.8578(3) 0.0406(13) Uani 1 1 d . . . C21 C 0.1662(7) 0.6217(5) 0.8588(3) 0.0634(18) Uani 1 1 d . . . H21A H 0.1941 0.5782 0.8198 0.076 Uiso 1 1 calc R . . C22 C 0.1362(8) 0.5808(6) 0.9153(4) 0.075(2) Uani 1 1 d . . . H22A H 0.1435 0.5092 0.9147 0.090 Uiso 1 1 calc R . . C23 C 0.0960(7) 0.6410(6) 0.9727(3) 0.0628(18) Uani 1 1 d . . . H23A H 0.0749 0.6116 1.0114 0.075 Uiso 1 1 calc R . . C24 C 0.0870(6) 0.7437(6) 0.9730(3) 0.0554(16) Uani 1 1 d . . . H24A H 0.0607 0.7871 1.0127 0.066 Uiso 1 1 calc R . . C25 C 0.1155(6) 0.7854(5) 0.9163(3) 0.0505(15) Uani 1 1 d . . . H25A H 0.1069 0.8567 0.9174 0.061 Uiso 1 1 calc R . . C26 C 0.2829(6) 0.7021(5) 0.7317(3) 0.0432(14) Uani 1 1 d . . . C27 C 0.4325(6) 0.7463(5) 0.7347(3) 0.0490(15) Uani 1 1 d . . . H27A H 0.4886 0.8220 0.7655 0.059 Uiso 1 1 calc R . . C28 C 0.5013(7) 0.6839(6) 0.6945(3) 0.0585(17) Uani 1 1 d . . . H28A H 0.6036 0.7164 0.6969 0.070 Uiso 1 1 calc R . . C29 C 0.4204(8) 0.5733(6) 0.6503(3) 0.0650(19) Uani 1 1 d . . . H29A H 0.4671 0.5295 0.6222 0.078 Uiso 1 1 calc R . . C30 C 0.2716(8) 0.5262(6) 0.6468(3) 0.0655(18) Uani 1 1 d . . . H30A H 0.2162 0.4503 0.6162 0.079 Uiso 1 1 calc R . . C31 C 0.2036(7) 0.5901(5) 0.6880(3) 0.0535(16) Uani 1 1 d . . . H31A H 0.1017 0.5569 0.6863 0.064 Uiso 1 1 calc R . . C32 C 0.3349(6) 0.9246(4) 0.8261(3) 0.0401(13) Uani 1 1 d . . . C33 C 0.4343(6) 0.9432(5) 0.8864(3) 0.0492(15) Uani 1 1 d . . . H33A H 0.4252 0.8823 0.9061 0.059 Uiso 1 1 calc R . . C34 C 0.5457(6) 1.0495(5) 0.9175(3) 0.0591(17) Uani 1 1 d . . . H34A H 0.6121 1.0612 0.9588 0.071 Uiso 1 1 calc R . . C35 C 0.5613(7) 1.1381(5) 0.8893(3) 0.0640(18) Uani 1 1 d . . . H35A H 0.6389 1.2107 0.9106 0.077 Uiso 1 1 calc R . . C36 C 0.4642(6) 1.1215(5) 0.8303(3) 0.0552(16) Uani 1 1 d . . . H36A H 0.4732 1.1834 0.8116 0.066 Uiso 1 1 calc R . . C37 C 0.3537(6) 1.0155(5) 0.7981(3) 0.0399(13) Uani 1 1 d . . . C38 C 0.2700(6) 0.9559(5) 0.6719(3) 0.0432(14) Uani 1 1 d . . . C39 C 0.4031(7) 0.9616(5) 0.6547(3) 0.0602(17) Uani 1 1 d . . . H39A H 0.4891 0.9979 0.6903 0.072 Uiso 1 1 calc R . . C40 C 0.4093(8) 0.9132(6) 0.5839(4) 0.080(2) Uani 1 1 d . . . H40A H 0.4996 0.9145 0.5709 0.096 Uiso 1 1 calc R . . C41 C 0.2835(9) 0.8632(6) 0.5328(4) 0.082(2) Uani 1 1 d . . . H41A H 0.2882 0.8313 0.4844 0.099 Uiso 1 1 calc R . . C42 C 0.1508(7) 0.8588(5) 0.5509(3) 0.0668(18) Uani 1 1 d . . . H42A H 0.0653 0.8241 0.5150 0.080 Uiso 1 1 calc R . . C43 C 0.1416(6) 0.9048(5) 0.6214(3) 0.0467(14) Uani 1 1 d . . . C44 C -0.0316(6) 1.0318(5) 0.6870(3) 0.0464(14) Uani 1 1 d . . . C45 C 0.0716(7) 1.1295(6) 0.6797(3) 0.0701(19) Uani 1 1 d . . . H45A H 0.1537 1.1245 0.6596 0.084 Uiso 1 1 calc R . . C46 C 0.0551(10) 1.2357(6) 0.7018(4) 0.093(2) Uani 1 1 d . . . H46A H 0.1258 1.3024 0.6964 0.112 Uiso 1 1 calc R . . C47 C -0.0620(10) 1.2442(7) 0.7312(5) 0.104(3) Uani 1 1 d . . . H47A H -0.0731 1.3164 0.7458 0.125 Uiso 1 1 calc R . . C48 C -0.1634(9) 1.1477(7) 0.7394(4) 0.095(3) Uani 1 1 d . . . H48A H -0.2441 1.1533 0.7605 0.114 Uiso 1 1 calc R . . C49 C -0.1482(7) 1.0424(6) 0.7169(3) 0.0687(19) Uani 1 1 d . . . H49A H -0.2198 0.9760 0.7221 0.082 Uiso 1 1 calc R . . C50 C -0.1699(6) 0.8293(5) 0.5753(3) 0.0466(14) Uani 1 1 d . . . C51 C -0.1724(7) 0.8921(6) 0.5282(3) 0.0670(19) Uani 1 1 d . . . H51A H -0.0962 0.9646 0.5356 0.080 Uiso 1 1 calc R . . C52 C -0.2857(8) 0.8490(6) 0.4707(3) 0.072(2) Uani 1 1 d . . . H52A H -0.2868 0.8917 0.4384 0.087 Uiso 1 1 calc R . . C53 C -0.3963(7) 0.7455(6) 0.4598(3) 0.0671(19) Uani 1 1 d . . . H53A H -0.4731 0.7165 0.4197 0.081 Uiso 1 1 calc R . . C54 C -0.3979(7) 0.6832(5) 0.5059(3) 0.0632(17) Uani 1 1 d . . . H54A H -0.4758 0.6118 0.4986 0.076 Uiso 1 1 calc R . . C55 C -0.2832(6) 0.7261(5) 0.5640(3) 0.0463(14) Uani 1 1 d . . . H55A H -0.2834 0.6831 0.5962 0.056 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 Cu 0.0427(4) 0.0381(4) 0.0372(4) 0.0114(3) 0.0123(3) 0.0108(3) N1 0.038(3) 0.037(3) 0.028(2) 0.007(2) 0.0060(19) 0.012(2) N2 0.037(3) 0.041(3) 0.036(3) 0.011(2) 0.010(2) 0.016(2) P1 0.0371(9) 0.0377(9) 0.0431(9) 0.0129(7) 0.0072(7) 0.0141(7) P2 0.0403(9) 0.0445(10) 0.0399(9) 0.0180(7) 0.0062(7) 0.0099(7) O1 0.041(2) 0.051(3) 0.044(2) 0.0183(19) 0.0090(18) 0.016(2) C1 0.040(3) 0.045(4) 0.032(3) 0.005(3) 0.006(2) 0.013(3) C2 0.047(4) 0.033(3) 0.048(4) -0.001(3) 0.004(3) 0.008(3) C3 0.038(3) 0.034(3) 0.044(3) 0.012(3) 0.004(3) 0.010(3) C4 0.027(3) 0.038(3) 0.036(3) 0.011(2) 0.002(2) 0.014(3) C5 0.031(3) 0.041(3) 0.035(3) 0.012(3) 0.000(2) 0.015(3) C6 0.032(3) 0.044(4) 0.033(3) 0.014(3) 0.008(2) 0.018(3) C7 0.058(4) 0.053(4) 0.039(3) 0.018(3) 0.018(3) 0.032(3) C8 0.079(5) 0.044(4) 0.044(4) 0.010(3) 0.022(3) 0.033(4) C9 0.047(4) 0.039(4) 0.039(3) 0.011(3) 0.007(3) 0.018(3) C10 0.064(4) 0.063(4) 0.041(3) 0.012(3) 0.015(3) 0.023(4) C11 0.072(5) 0.036(4) 0.067(4) 0.019(3) 0.017(3) 0.015(3) C12 0.069(5) 0.044(4) 0.058(4) 0.009(3) 0.010(3) 0.017(3) C13 0.102(6) 0.065(5) 0.069(5) 0.018(4) 0.048(4) 0.040(4) C14 0.048(4) 0.039(3) 0.039(3) 0.015(3) 0.018(3) 0.020(3) C15 0.063(4) 0.060(4) 0.042(3) 0.023(3) 0.009(3) 0.025(3) C16 0.094(6) 0.064(5) 0.050(4) 0.027(3) 0.018(4) 0.031(4) C17 0.094(6) 0.068(5) 0.064(5) 0.033(4) 0.041(4) 0.028(5) C18 0.056(4) 0.067(5) 0.072(5) 0.029(4) 0.025(4) 0.015(4) C19 0.042(4) 0.071(5) 0.060(4) 0.037(3) 0.016(3) 0.019(3) C20 0.035(3) 0.042(4) 0.045(3) 0.013(3) 0.003(2) 0.017(3) C21 0.083(5) 0.054(4) 0.071(4) 0.026(4) 0.037(4) 0.037(4) C22 0.104(6) 0.055(5) 0.088(5) 0.043(4) 0.034(5) 0.037(4) C23 0.061(5) 0.068(5) 0.056(4) 0.030(4) 0.010(3) 0.012(4) C24 0.065(5) 0.063(5) 0.038(3) 0.015(3) 0.009(3) 0.025(4) C25 0.050(4) 0.056(4) 0.045(4) 0.015(3) 0.000(3) 0.022(3) C26 0.051(4) 0.045(4) 0.039(3) 0.015(3) 0.009(3) 0.023(3) C27 0.046(4) 0.059(4) 0.050(4) 0.022(3) 0.015(3) 0.025(3) C28 0.060(4) 0.072(5) 0.058(4) 0.027(4) 0.023(3) 0.035(4) C29 0.078(5) 0.083(6) 0.056(4) 0.024(4) 0.026(4) 0.051(5) C30 0.087(6) 0.056(4) 0.049(4) 0.004(3) 0.003(4) 0.031(4) C31 0.054(4) 0.053(4) 0.051(4) 0.010(3) 0.010(3) 0.024(3) C32 0.036(3) 0.039(3) 0.042(3) 0.009(3) 0.003(2) 0.013(3) C33 0.047(4) 0.049(4) 0.050(4) 0.014(3) -0.001(3) 0.018(3) C34 0.042(4) 0.056(4) 0.060(4) 0.004(3) -0.011(3) 0.011(3) C35 0.048(4) 0.041(4) 0.079(5) 0.008(3) -0.003(3) -0.001(3) C36 0.045(4) 0.041(4) 0.074(5) 0.022(3) 0.006(3) 0.008(3) C37 0.033(3) 0.041(4) 0.044(3) 0.011(3) 0.007(3) 0.014(3) C38 0.045(4) 0.040(4) 0.051(4) 0.022(3) 0.016(3) 0.016(3) C39 0.045(4) 0.068(5) 0.062(4) 0.019(3) 0.014(3) 0.014(3) C40 0.062(5) 0.092(6) 0.089(6) 0.022(5) 0.036(5) 0.032(5) C41 0.082(6) 0.093(6) 0.061(5) 0.011(4) 0.039(4) 0.024(5) C42 0.064(5) 0.068(5) 0.051(4) 0.012(3) 0.012(3) 0.008(4) C43 0.053(4) 0.048(4) 0.044(4) 0.020(3) 0.016(3) 0.020(3) C44 0.041(4) 0.045(4) 0.050(4) 0.015(3) -0.002(3) 0.015(3) C45 0.063(5) 0.050(5) 0.092(5) 0.025(4) 0.011(4) 0.013(4) C46 0.096(7) 0.050(5) 0.131(7) 0.035(5) 0.011(5) 0.020(5) C47 0.082(7) 0.072(7) 0.158(9) 0.030(6) -0.003(6) 0.040(6) C48 0.072(6) 0.070(6) 0.144(8) 0.017(5) 0.018(5) 0.041(5) C49 0.053(5) 0.058(5) 0.091(5) 0.020(4) 0.008(4) 0.021(4) C50 0.045(4) 0.055(4) 0.038(3) 0.021(3) 0.006(3) 0.013(3) C51 0.058(5) 0.071(5) 0.060(4) 0.035(4) -0.004(3) 0.001(4) C52 0.068(5) 0.089(6) 0.060(4) 0.041(4) 0.006(4) 0.016(4) C53 0.055(5) 0.089(6) 0.047(4) 0.018(4) -0.005(3) 0.019(4) C54 0.056(5) 0.059(4) 0.053(4) 0.009(3) -0.001(3) 0.003(3) C55 0.041(4) 0.049(4) 0.043(3) 0.015(3) 0.007(3) 0.008(3) _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 Cu N2 1.996(4) . ? Cu N1 2.003(4) . ? Cu P2 2.2383(15) . ? Cu P1 2.3780(16) . ? N1 C1 1.339(6) . ? N1 C4 1.412(6) . ? N2 C9 1.340(6) . ? N2 C6 1.418(6) . ? P1 C20 1.838(5) . ? P1 C26 1.837(5) . ? P1 C32 1.847(6) . ? P2 C43 1.830(6) . ? P2 C50 1.836(5) . ? P2 C44 1.836(6) . ? O1 C38 1.385(6) . ? O1 C37 1.391(6) . ? C1 C2 1.393(7) . ? C1 C10 1.509(6) . ? C2 C3 1.359(6) . ? C3 C4 1.434(7) . ? C3 C11 1.501(7) . ? C4 C5 1.418(6) . ? C5 C6 1.402(7) . ? C5 C14 1.494(7) . ? C6 C7 1.446(6) . ? C7 C8 1.360(7) . ? C7 C13 1.505(7) . ? C8 C9 1.410(7) . ? C9 C12 1.492(7) . ? C14 C19 1.378(7) . ? C14 C15 1.393(7) . ? C15 C16 1.383(8) . ? C16 C17 1.366(9) . ? C17 C18 1.368(8) . ? C18 C19 1.376(7) . ? C20 C21 1.390(7) . ? C20 C25 1.386(7) . ? C21 C22 1.373(8) . ? C22 C23 1.370(8) . ? C23 C24 1.361(7) . ? C24 C25 1.378(7) . ? C26 C31 1.388(7) . ? C26 C27 1.390(7) . ? C27 C28 1.372(7) . ? C28 C29 1.382(8) . ? C29 C30 1.383(8) . ? C30 C31 1.386(7) . ? C32 C37 1.391(7) . ? C32 C33 1.397(7) . ? C33 C34 1.382(7) . ? C34 C35 1.372(8) . ? C35 C36 1.372(7) . ? C36 C37 1.379(7) . ? C38 C39 1.375(7) . ? C38 C43 1.391(7) . ? C39 C40 1.393(8) . ? C40 C41 1.380(9) . ? C41 C42 1.381(8) . ? C42 C43 1.389(7) . ? C44 C49 1.374(8) . ? C44 C45 1.385(8) . ? C45 C46 1.399(9) . ? C46 C47 1.367(10) . ? C47 C48 1.372(10) . ? C48 C49 1.382(8) . ? C50 C55 1.373(7) . ? C50 C51 1.394(7) . ? C51 C52 1.380(8) . ? C52 C53 1.365(8) . ? C53 C54 1.366(8) . ? C54 C55 1.396(7) . ? 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 N2 Cu N1 95.17(16) . . ? N2 Cu P2 119.70(12) . . ? N1 Cu P2 118.33(12) . . ? N2 Cu P1 100.56(12) . . ? N1 Cu P1 103.60(12) . . ? P2 Cu P1 115.95(6) . . ? C1 N1 C4 106.0(4) . . ? C1 N1 Cu 129.1(3) . . ? C4 N1 Cu 122.6(3) . . ? C9 N2 C6 106.9(4) . . ? C9 N2 Cu 129.0(4) . . ? C6 N2 Cu 124.0(3) . . ? C20 P1 C26 103.1(2) . . ? C20 P1 C32 101.2(2) . . ? C26 P1 C32 100.9(3) . . ? C20 P1 Cu 108.56(17) . . ? C26 P1 Cu 121.94(18) . . ? C32 P1 Cu 118.36(17) . . ? C43 P2 C50 104.3(3) . . ? C43 P2 C44 105.5(3) . . ? C50 P2 C44 97.9(2) . . ? C43 P2 Cu 108.70(18) . . ? C50 P2 Cu 118.81(19) . . ? C44 P2 Cu 119.91(18) . . ? C38 O1 C37 119.5(4) . . ? N1 C1 C2 111.1(4) . . ? N1 C1 C10 122.9(5) . . ? C2 C1 C10 126.0(5) . . ? C3 C2 C1 108.6(5) . . ? C2 C3 C4 105.9(4) . . ? C2 C3 C11 122.1(5) . . ? C4 C3 C11 132.0(5) . . ? N1 C4 C5 123.1(4) . . ? N1 C4 C3 108.4(4) . . ? C5 C4 C3 128.5(5) . . ? C6 C5 C4 129.4(5) . . ? C6 C5 C14 115.3(4) . . ? C4 C5 C14 115.3(4) . . ? C5 C6 N2 123.1(4) . . ? C5 C6 C7 129.3(5) . . ? N2 C6 C7 107.5(4) . . ? C8 C7 C6 106.6(5) . . ? C8 C7 C13 122.6(5) . . ? C6 C7 C13 130.8(5) . . ? C7 C8 C9 108.3(5) . . ? N2 C9 C8 110.7(5) . . ? N2 C9 C12 122.9(5) . . ? C8 C9 C12 126.1(5) . . ? C19 C14 C15 118.6(5) . . ? C19 C14 C5 121.4(5) . . ? C15 C14 C5 119.9(5) . . ? C16 C15 C14 120.0(6) . . ? C17 C16 C15 120.0(6) . . ? C16 C17 C18 120.7(6) . . ? C17 C18 C19 119.7(6) . . ? C18 C19 C14 121.0(6) . . ? C21 C20 C25 116.8(5) . . ? C21 C20 P1 124.0(4) . . ? C25 C20 P1 119.1(4) . . ? C22 C21 C20 120.9(6) . . ? C23 C22 C21 121.4(6) . . ? C24 C23 C22 118.6(6) . . ? C23 C24 C25 120.7(6) . . ? C24 C25 C20 121.6(5) . . ? C31 C26 C27 118.0(5) . . ? C31 C26 P1 118.4(4) . . ? C27 C26 P1 123.5(4) . . ? C28 C27 C26 121.9(6) . . ? C27 C28 C29 119.3(6) . . ? C28 C29 C30 120.3(6) . . ? C31 C30 C29 119.9(6) . . ? C30 C31 C26 120.6(6) . . ? C37 C32 C33 117.9(5) . . ? C37 C32 P1 120.2(4) . . ? C33 C32 P1 122.0(4) . . ? C34 C33 C32 120.5(5) . . ? C35 C34 C33 120.5(6) . . ? C36 C35 C34 119.7(6) . . ? C35 C36 C37 120.4(6) . . ? C36 C37 O1 118.9(5) . . ? C36 C37 C32 120.9(5) . . ? O1 C37 C32 120.0(5) . . ? C39 C38 O1 122.8(5) . . ? C39 C38 C43 122.7(5) . . ? O1 C38 C43 114.4(5) . . ? C38 C39 C40 118.6(6) . . ? C41 C40 C39 119.7(6) . . ? C40 C41 C42 120.9(6) . . ? C41 C42 C43 120.5(6) . . ? C38 C43 C42 117.6(5) . . ? C38 C43 P2 116.5(4) . . ? C42 C43 P2 125.3(5) . . ? C49 C44 C45 118.5(6) . . ? C49 C44 P2 117.3(5) . . ? C45 C44 P2 124.2(5) . . ? C44 C45 C46 120.0(7) . . ? C47 C46 C45 120.6(8) . . ? C46 C47 C48 119.5(8) . . ? C47 C48 C49 120.1(8) . . ? C44 C49 C48 121.4(7) . . ? C55 C50 C51 118.7(5) . . ? C55 C50 P2 119.4(4) . . ? C51 C50 P2 121.7(5) . . ? C52 C51 C50 119.9(6) . . ? C53 C52 C51 120.5(6) . . ? C54 C53 C52 120.8(6) . . ? C53 C54 C55 119.0(6) . . ? C50 C55 C54 121.1(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 N2 Cu N1 C1 -176.3(4) . . . . ? P2 Cu N1 C1 55.9(4) . . . . ? P1 Cu N1 C1 -74.1(4) . . . . ? N2 Cu N1 C4 -15.9(4) . . . . ? P2 Cu N1 C4 -143.8(3) . . . . ? P1 Cu N1 C4 86.3(3) . . . . ? N1 Cu N2 C9 -176.1(4) . . . . ? P2 Cu N2 C9 -49.2(5) . . . . ? P1 Cu N2 C9 79.0(4) . . . . ? N1 Cu N2 C6 5.3(4) . . . . ? P2 Cu N2 C6 132.1(3) . . . . ? P1 Cu N2 C6 -99.6(4) . . . . ? N2 Cu P1 C20 35.1(2) . . . . ? N1 Cu P1 C20 -62.9(2) . . . . ? P2 Cu P1 C20 165.71(19) . . . . ? N2 Cu P1 C26 154.5(2) . . . . ? N1 Cu P1 C26 56.5(2) . . . . ? P2 Cu P1 C26 -74.9(2) . . . . ? N2 Cu P1 C32 -79.4(2) . . . . ? N1 Cu P1 C32 -177.4(2) . . . . ? P2 Cu P1 C32 51.2(2) . . . . ? N2 Cu P2 C43 143.6(2) . . . . ? N1 Cu P2 C43 -101.2(2) . . . . ? P1 Cu P2 C43 22.8(2) . . . . ? N2 Cu P2 C50 -97.5(2) . . . . ? N1 Cu P2 C50 17.7(2) . . . . ? P1 Cu P2 C50 141.7(2) . . . . ? N2 Cu P2 C44 22.3(3) . . . . ? N1 Cu P2 C44 137.5(2) . . . . ? P1 Cu P2 C44 -98.5(2) . . . . ? C4 N1 C1 C2 -1.2(6) . . . . ? Cu N1 C1 C2 161.7(4) . . . . ? C4 N1 C1 C10 178.5(5) . . . . ? Cu N1 C1 C10 -18.6(7) . . . . ? N1 C1 C2 C3 1.2(6) . . . . ? C10 C1 C2 C3 -178.4(5) . . . . ? C1 C2 C3 C4 -0.7(6) . . . . ? C1 C2 C3 C11 179.3(5) . . . . ? C1 N1 C4 C5 -177.3(4) . . . . ? Cu N1 C4 C5 18.5(6) . . . . ? C1 N1 C4 C3 0.7(5) . . . . ? Cu N1 C4 C3 -163.5(3) . . . . ? C2 C3 C4 N1 0.0(6) . . . . ? C11 C3 C4 N1 180.0(5) . . . . ? C2 C3 C4 C5 177.8(5) . . . . ? C11 C3 C4 C5 -2.2(9) . . . . ? N1 C4 C5 C6 -6.3(8) . . . . ? C3 C4 C5 C6 176.1(5) . . . . ? N1 C4 C5 C14 174.3(4) . . . . ? C3 C4 C5 C14 -3.2(7) . . . . ? C4 C5 C6 N2 -6.1(8) . . . . ? C14 C5 C6 N2 173.3(4) . . . . ? C4 C5 C6 C7 177.5(5) . . . . ? C14 C5 C6 C7 -3.1(8) . . . . ? C9 N2 C6 C5 -174.8(5) . . . . ? Cu N2 C6 C5 4.0(6) . . . . ? C9 N2 C6 C7 2.2(5) . . . . ? Cu N2 C6 C7 -178.9(3) . . . . ? C5 C6 C7 C8 174.4(5) . . . . ? N2 C6 C7 C8 -2.4(6) . . . . ? C5 C6 C7 C13 -6.5(9) . . . . ? N2 C6 C7 C13 176.7(6) . . . . ? C6 C7 C8 C9 1.7(6) . . . . ? C13 C7 C8 C9 -177.5(5) . . . . ? C6 N2 C9 C8 -1.2(6) . . . . ? Cu N2 C9 C8 180.0(3) . . . . ? C6 N2 C9 C12 173.0(5) . . . . ? Cu N2 C9 C12 -5.8(7) . . . . ? C7 C8 C9 N2 -0.3(6) . . . . ? C7 C8 C9 C12 -174.3(5) . . . . ? C6 C5 C14 C19 97.7(6) . . . . ? C4 C5 C14 C19 -82.9(6) . . . . ? C6 C5 C14 C15 -82.6(6) . . . . ? C4 C5 C14 C15 96.8(6) . . . . ? C19 C14 C15 C16 0.1(8) . . . . ? C5 C14 C15 C16 -179.6(5) . . . . ? C14 C15 C16 C17 0.3(9) . . . . ? C15 C16 C17 C18 0.1(10) . . . . ? C16 C17 C18 C19 -0.8(10) . . . . ? C17 C18 C19 C14 1.3(9) . . . . ? C15 C14 C19 C18 -0.9(8) . . . . ? C5 C14 C19 C18 178.8(5) . . . . ? C26 P1 C20 C21 -18.1(6) . . . . ? C32 P1 C20 C21 -122.2(5) . . . . ? Cu P1 C20 C21 112.6(5) . . . . ? C26 P1 C20 C25 165.2(4) . . . . ? C32 P1 C20 C25 61.1(5) . . . . ? Cu P1 C20 C25 -64.2(5) . . . . ? C25 C20 C21 C22 0.2(9) . . . . ? P1 C20 C21 C22 -176.7(5) . . . . ? C20 C21 C22 C23 -0.2(11) . . . . ? C21 C22 C23 C24 -0.4(10) . . . . ? C22 C23 C24 C25 1.0(9) . . . . ? C23 C24 C25 C20 -1.0(9) . . . . ? C21 C20 C25 C24 0.4(8) . . . . ? P1 C20 C25 C24 177.4(4) . . . . ? C20 P1 C26 C31 78.6(5) . . . . ? C32 P1 C26 C31 -177.0(4) . . . . ? Cu P1 C26 C31 -43.4(5) . . . . ? C20 P1 C26 C27 -101.4(5) . . . . ? C32 P1 C26 C27 3.0(5) . . . . ? Cu P1 C26 C27 136.6(4) . . . . ? C31 C26 C27 C28 1.8(8) . . . . ? P1 C26 C27 C28 -178.1(4) . . . . ? C26 C27 C28 C29 -0.8(8) . . . . ? C27 C28 C29 C30 0.0(9) . . . . ? C28 C29 C30 C31 -0.3(9) . . . . ? C29 C30 C31 C26 1.4(9) . . . . ? C27 C26 C31 C30 -2.1(8) . . . . ? P1 C26 C31 C30 177.8(4) . . . . ? C20 P1 C32 C37 -154.4(4) . . . . ? C26 P1 C32 C37 99.7(4) . . . . ? Cu P1 C32 C37 -36.0(5) . . . . ? C20 P1 C32 C33 27.1(5) . . . . ? C26 P1 C32 C33 -78.8(5) . . . . ? Cu P1 C32 C33 145.5(4) . . . . ? C37 C32 C33 C34 1.2(8) . . . . ? P1 C32 C33 C34 179.6(4) . . . . ? C32 C33 C34 C35 -0.6(9) . . . . ? C33 C34 C35 C36 0.9(9) . . . . ? C34 C35 C36 C37 -1.8(9) . . . . ? C35 C36 C37 O1 177.0(5) . . . . ? C35 C36 C37 C32 2.4(9) . . . . ? C38 O1 C37 C36 98.3(6) . . . . ? C38 O1 C37 C32 -87.0(6) . . . . ? C33 C32 C37 C36 -2.1(8) . . . . ? P1 C32 C37 C36 179.4(4) . . . . ? C33 C32 C37 O1 -176.6(4) . . . . ? P1 C32 C37 O1 4.9(6) . . . . ? C37 O1 C38 C39 -26.5(7) . . . . ? C37 O1 C38 C43 155.2(5) . . . . ? O1 C38 C39 C40 -178.9(5) . . . . ? C43 C38 C39 C40 -0.8(9) . . . . ? C38 C39 C40 C41 1.4(10) . . . . ? C39 C40 C41 C42 -1.1(11) . . . . ? C40 C41 C42 C43 0.0(11) . . . . ? C39 C38 C43 C42 -0.3(8) . . . . ? O1 C38 C43 C42 178.0(5) . . . . ? C39 C38 C43 P2 171.4(4) . . . . ? O1 C38 C43 P2 -10.3(6) . . . . ? C41 C42 C43 C38 0.7(9) . . . . ? C41 C42 C43 P2 -170.2(5) . . . . ? C50 P2 C43 C38 175.3(4) . . . . ? C44 P2 C43 C38 72.8(5) . . . . ? Cu P2 C43 C38 -57.0(4) . . . . ? C50 P2 C43 C42 -13.7(6) . . . . ? C44 P2 C43 C42 -116.3(5) . . . . ? Cu P2 C43 C42 113.9(5) . . . . ? C43 P2 C44 C49 -178.9(5) . . . . ? C50 P2 C44 C49 73.9(5) . . . . ? Cu P2 C44 C49 -56.0(5) . . . . ? C43 P2 C44 C45 4.0(6) . . . . ? C50 P2 C44 C45 -103.2(5) . . . . ? Cu P2 C44 C45 126.9(5) . . . . ? C49 C44 C45 C46 -0.6(9) . . . . ? P2 C44 C45 C46 176.5(5) . . . . ? C44 C45 C46 C47 0.4(11) . . . . ? C45 C46 C47 C48 0.4(13) . . . . ? C46 C47 C48 C49 -1.1(13) . . . . ? C45 C44 C49 C48 -0.1(9) . . . . ? P2 C44 C49 C48 -177.3(5) . . . . ? C47 C48 C49 C44 1.0(11) . . . . ? C43 P2 C50 C55 123.2(5) . . . . ? C44 P2 C50 C55 -128.6(5) . . . . ? Cu P2 C50 C55 2.0(5) . . . . ? C43 P2 C50 C51 -61.9(5) . . . . ? C44 P2 C50 C51 46.3(5) . . . . ? Cu P2 C50 C51 176.9(4) . . . . ? C55 C50 C51 C52 -1.3(9) . . . . ? P2 C50 C51 C52 -176.3(5) . . . . ? C50 C51 C52 C53 0.5(10) . . . . ? C51 C52 C53 C54 0.7(11) . . . . ? C52 C53 C54 C55 -1.0(10) . . . . ? C51 C50 C55 C54 1.0(9) . . . . ? P2 C50 C55 C54 176.1(4) . . . . ? C53 C54 C55 C50 0.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.488 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.071 data_t064 _database_code_depnum_ccdc_archive 'CCDC 871240' #TrackingRef 'T064.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 Cl2 Cu F5 N2 O P2' _chemical_formula_weight 1052.31 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7878(10) _cell_length_b 13.0429(10) _cell_length_c 17.5091(13) _cell_angle_alpha 87.8530(10) _cell_angle_beta 72.3730(10) _cell_angle_gamma 61.4550(10) _cell_volume 2424.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 2392 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 22.58 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8225 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13757 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.03 _reflns_number_total 9369 _reflns_number_gt 6663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0613P)^2^+0.5078P] 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 9369 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu Cu 0.44490(4) 0.19953(4) 0.25063(2) 0.02426(13) Uani 1 1 d . . . P1 P 0.28410(8) 0.23472(8) 0.20735(5) 0.0248(2) Uani 1 1 d . . . P2 P 0.47535(8) 0.36454(8) 0.24245(5) 0.0232(2) Uani 1 1 d . . . F1 F 0.8421(2) -0.17840(18) 0.34267(14) 0.0430(6) Uani 1 1 d . . . F2 F 1.0388(2) -0.23564(19) 0.39452(16) 0.0537(7) Uani 1 1 d . . . F3 F 1.0971(2) -0.0686(2) 0.42227(14) 0.0462(6) Uani 1 1 d . . . F4 F 0.9603(2) 0.1544(2) 0.39427(15) 0.0502(6) Uani 1 1 d . . . F5 F 0.7661(2) 0.21229(18) 0.33943(14) 0.0427(6) Uani 1 1 d . . . O O 0.2109(2) 0.4674(2) 0.28903(14) 0.0286(6) Uani 1 1 d . . . N1 N 0.4525(3) 0.1516(2) 0.36071(16) 0.0237(6) Uani 1 1 d . . . N2 N 0.6127(3) 0.0462(2) 0.19945(17) 0.0255(7) Uani 1 1 d . . . C1 C 0.3629(3) 0.1897(3) 0.4327(2) 0.0287(8) Uani 1 1 d . . . C2 C 0.4149(3) 0.1675(3) 0.4964(2) 0.0324(9) Uani 1 1 d . . . H2A H 0.3690 0.1858 0.5525 0.039 Uiso 1 1 calc R . . C3 C 0.5434(3) 0.1148(3) 0.4625(2) 0.0269(8) Uani 1 1 d . . . C4 C 0.5679(3) 0.1037(3) 0.3762(2) 0.0233(7) Uani 1 1 d . . . C5 C 0.6844(3) 0.0533(3) 0.3136(2) 0.0243(8) Uani 1 1 d . . . C6 C 0.7090(3) 0.0272(3) 0.2303(2) 0.0249(8) Uani 1 1 d . . . C7 C 0.8275(3) -0.0333(3) 0.1670(2) 0.0324(9) Uani 1 1 d . . . C8 C 0.8008(3) -0.0551(3) 0.1015(2) 0.0348(9) Uani 1 1 d . . . H8A H 0.8605 -0.0956 0.0502 0.042 Uiso 1 1 calc R . . C9 C 0.6694(3) -0.0072(3) 0.1230(2) 0.0282(8) Uani 1 1 d . . . C10 C 0.2260(3) 0.2514(4) 0.4411(2) 0.0392(10) Uani 1 1 d . . . H10A H 0.2166 0.2546 0.3874 0.059 Uiso 1 1 calc R . . H10B H 0.1855 0.3316 0.4684 0.059 Uiso 1 1 calc R . . H10C H 0.1863 0.2085 0.4730 0.059 Uiso 1 1 calc R . . C11 C 0.6295(4) 0.0777(3) 0.5125(2) 0.0371(9) Uani 1 1 d . . . H11A H 0.5793 0.0992 0.5700 0.056 Uiso 1 1 calc R . . H11B H 0.6800 0.1175 0.4990 0.056 Uiso 1 1 calc R . . H11C H 0.6853 -0.0077 0.5012 0.056 Uiso 1 1 calc R . . C12 C 0.6001(4) -0.0182(3) 0.0721(2) 0.0372(10) Uani 1 1 d . . . H12A H 0.5096 0.0234 0.1018 0.056 Uiso 1 1 calc R . . H12B H 0.6281 -0.1015 0.0587 0.056 Uiso 1 1 calc R . . H12C H 0.6168 0.0163 0.0222 0.056 Uiso 1 1 calc R . . C13 C 0.9580(3) -0.0654(4) 0.1663(3) 0.0505(12) Uani 1 1 d . . . H13A H 1.0190 -0.1071 0.1132 0.076 Uiso 1 1 calc R . . H13B H 0.9791 -0.1163 0.2081 0.076 Uiso 1 1 calc R . . H13C H 0.9606 0.0064 0.1771 0.076 Uiso 1 1 calc R . . C14 C 0.7974(3) 0.0189(3) 0.3393(2) 0.0251(8) Uani 1 1 d . . . C15 C 0.8701(3) -0.0937(3) 0.3539(2) 0.0307(8) Uani 1 1 d . . . C16 C 0.9706(3) -0.1249(3) 0.3809(2) 0.0344(9) Uani 1 1 d . . . C17 C 1.0009(3) -0.0409(3) 0.3947(2) 0.0333(9) Uani 1 1 d . . . C18 C 0.9311(4) 0.0726(3) 0.3804(2) 0.0334(9) Uani 1 1 d . . . C19 C 0.8319(3) 0.1006(3) 0.3525(2) 0.0292(8) Uani 1 1 d . . . C20 C 0.2688(3) 0.1023(3) 0.2007(2) 0.0299(8) Uani 1 1 d . . . C21 C 0.2250(4) 0.0760(4) 0.1449(2) 0.0400(10) Uani 1 1 d . . . H21A H 0.1963 0.1302 0.1085 0.048 Uiso 1 1 calc R . . C22 C 0.2232(4) -0.0294(4) 0.1423(3) 0.0556(13) Uani 1 1 d . . . H22A H 0.1945 -0.0473 0.1032 0.067 Uiso 1 1 calc R . . C23 C 0.2618(4) -0.1075(4) 0.1950(3) 0.0570(14) Uani 1 1 d . . . H23A H 0.2585 -0.1786 0.1934 0.068 Uiso 1 1 calc R . . C24 C 0.3058(4) -0.0828(4) 0.2508(3) 0.0525(12) Uani 1 1 d . . . H24A H 0.3331 -0.1371 0.2876 0.063 Uiso 1 1 calc R . . C25 C 0.3102(4) 0.0213(3) 0.2533(2) 0.0380(10) Uani 1 1 d . . . H25A H 0.3417 0.0373 0.2913 0.046 Uiso 1 1 calc R . . C26 C 0.2873(3) 0.2851(3) 0.1082(2) 0.0271(8) Uani 1 1 d . . . C27 C 0.1809(4) 0.3404(4) 0.0837(2) 0.0397(10) Uani 1 1 d . . . H27A H 0.1023 0.3519 0.1191 0.048 Uiso 1 1 calc R . . C28 C 0.1882(4) 0.3785(4) 0.0086(3) 0.0490(11) Uani 1 1 d . . . H28A H 0.1148 0.4163 -0.0070 0.059 Uiso 1 1 calc R . . C29 C 0.3012(4) 0.3620(4) -0.0437(2) 0.0465(11) Uani 1 1 d . . . H29A H 0.3060 0.3881 -0.0954 0.056 Uiso 1 1 calc R . . C30 C 0.4072(4) 0.3076(4) -0.0208(2) 0.0398(10) Uani 1 1 d . . . H30A H 0.4857 0.2950 -0.0571 0.048 Uiso 1 1 calc R . . C31 C 0.4001(3) 0.2713(3) 0.0544(2) 0.0304(8) Uani 1 1 d . . . H31A H 0.4736 0.2361 0.0700 0.036 Uiso 1 1 calc R . . C32 C 0.1251(3) 0.3449(3) 0.2703(2) 0.0254(8) Uani 1 1 d . . . C33 C 0.0206(3) 0.3290(3) 0.2896(2) 0.0328(9) Uani 1 1 d . . . H33A H 0.0287 0.2596 0.2668 0.039 Uiso 1 1 calc R . . C34 C -0.0952(3) 0.4125(3) 0.3415(2) 0.0389(10) Uani 1 1 d . . . H34A H -0.1658 0.4003 0.3537 0.047 Uiso 1 1 calc R . . C35 C -0.1076(3) 0.5125(4) 0.3750(2) 0.0399(10) Uani 1 1 d . . . H35A H -0.1868 0.5689 0.4112 0.048 Uiso 1 1 calc R . . C36 C -0.0061(3) 0.5325(3) 0.3567(2) 0.0354(9) Uani 1 1 d . . . H36A H -0.0150 0.6020 0.3800 0.043 Uiso 1 1 calc R . . C37 C 0.1078(3) 0.4496(3) 0.3042(2) 0.0278(8) Uani 1 1 d . . . C38 C 0.2496(3) 0.5092(3) 0.2181(2) 0.0265(8) Uani 1 1 d . . . C39 C 0.1679(3) 0.5834(3) 0.1797(2) 0.0336(9) Uani 1 1 d . . . H39A H 0.0808 0.6070 0.2006 0.040 Uiso 1 1 calc R . . C40 C 0.2143(4) 0.6234(3) 0.1100(2) 0.0367(9) Uani 1 1 d . . . H40A H 0.1593 0.6723 0.0818 0.044 Uiso 1 1 calc R . . C41 C 0.3403(4) 0.5924(3) 0.0813(2) 0.0354(9) Uani 1 1 d . . . H41A H 0.3710 0.6225 0.0348 0.043 Uiso 1 1 calc R . . C42 C 0.4213(3) 0.5175(3) 0.1205(2) 0.0293(8) Uani 1 1 d . . . H42A H 0.5078 0.4962 0.1003 0.035 Uiso 1 1 calc R . . C43 C 0.3779(3) 0.4726(3) 0.1893(2) 0.0254(8) Uani 1 1 d . . . C44 C 0.6338(3) 0.3411(3) 0.1872(2) 0.0266(8) Uani 1 1 d . . . C45 C 0.7080(3) 0.2496(3) 0.1236(2) 0.0334(9) Uani 1 1 d . . . H45A H 0.6755 0.2034 0.1100 0.040 Uiso 1 1 calc R . . C46 C 0.8296(4) 0.2257(4) 0.0800(2) 0.0412(10) Uani 1 1 d . . . H46A H 0.8788 0.1644 0.0359 0.049 Uiso 1 1 calc R . . C47 C 0.8793(4) 0.2897(4) 0.0998(3) 0.0435(10) Uani 1 1 d . . . H47A H 0.9626 0.2729 0.0699 0.052 Uiso 1 1 calc R . . C48 C 0.8066(4) 0.3788(4) 0.1638(3) 0.0438(11) Uani 1 1 d . . . H48A H 0.8407 0.4229 0.1784 0.053 Uiso 1 1 calc R . . C49 C 0.6843(4) 0.4051(3) 0.2073(2) 0.0354(9) Uani 1 1 d . . . H49A H 0.6352 0.4671 0.2509 0.043 Uiso 1 1 calc R . . C50 C 0.4268(3) 0.4591(3) 0.3358(2) 0.0263(8) Uani 1 1 d . . . C51 C 0.4367(3) 0.4083(3) 0.4060(2) 0.0311(9) Uani 1 1 d . . . H51A H 0.4730 0.3253 0.4046 0.037 Uiso 1 1 calc R . . C52 C 0.3938(4) 0.4782(4) 0.4787(2) 0.0392(10) Uani 1 1 d . . . H52A H 0.4003 0.4433 0.5268 0.047 Uiso 1 1 calc R . . C53 C 0.3418(4) 0.5988(4) 0.4801(3) 0.0436(11) Uani 1 1 d . . . H53A H 0.3117 0.6470 0.5297 0.052 Uiso 1 1 calc R . . C54 C 0.3335(4) 0.6492(4) 0.4110(3) 0.0452(11) Uani 1 1 d . . . H54A H 0.2989 0.7321 0.4124 0.054 Uiso 1 1 calc R . . C55 C 0.3754(4) 0.5798(3) 0.3387(2) 0.0387(10) Uani 1 1 d . . . H55A H 0.3689 0.6154 0.2908 0.046 Uiso 1 1 calc R . . C56 C 0.3028(5) 0.2382(4) -0.2318(4) 0.0748(17) Uani 1 1 d . . . H56A H 0.3048 0.1778 -0.2658 0.090 Uiso 1 1 calc R . . H56B H 0.3416 0.1990 -0.1905 0.090 Uiso 1 1 calc R . . Cl1 Cl 0.39145(13) 0.29873(11) -0.29280(8) 0.0695(4) Uani 1 1 d . . . Cl2 Cl 0.14655(13) 0.34507(13) -0.18399(9) 0.0731(4) 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 Cu 0.0236(2) 0.0230(2) 0.0235(2) 0.00157(18) -0.00690(18) -0.00978(19) P1 0.0233(5) 0.0250(5) 0.0247(5) 0.0001(4) -0.0062(4) -0.0116(4) P2 0.0243(5) 0.0207(5) 0.0248(5) 0.0018(4) -0.0067(4) -0.0117(4) F1 0.0449(13) 0.0219(12) 0.0710(17) 0.0079(11) -0.0299(12) -0.0166(11) F2 0.0487(15) 0.0302(13) 0.088(2) 0.0201(13) -0.0414(14) -0.0132(12) F3 0.0374(13) 0.0512(15) 0.0576(15) 0.0094(12) -0.0264(12) -0.0213(12) F4 0.0585(16) 0.0435(15) 0.0739(18) 0.0122(12) -0.0359(14) -0.0360(13) F5 0.0541(14) 0.0235(12) 0.0610(16) 0.0133(11) -0.0322(13) -0.0195(11) O 0.0243(13) 0.0287(14) 0.0326(14) 0.0066(11) -0.0068(11) -0.0144(11) N1 0.0260(16) 0.0209(15) 0.0224(15) 0.0031(12) -0.0063(13) -0.0111(13) N2 0.0256(16) 0.0228(16) 0.0252(16) -0.0003(13) -0.0064(13) -0.0104(13) C1 0.031(2) 0.026(2) 0.0246(19) 0.0038(16) -0.0042(16) -0.0133(17) C2 0.038(2) 0.034(2) 0.0186(18) 0.0049(16) -0.0055(16) -0.0149(19) C3 0.035(2) 0.0199(18) 0.0252(19) 0.0045(15) -0.0110(16) -0.0123(17) C4 0.0296(19) 0.0175(18) 0.0230(18) 0.0030(14) -0.0083(15) -0.0119(16) C5 0.0270(19) 0.0160(17) 0.030(2) 0.0037(15) -0.0110(16) -0.0098(15) C6 0.0231(18) 0.0166(18) 0.028(2) -0.0008(15) -0.0068(15) -0.0055(15) C7 0.0241(19) 0.031(2) 0.030(2) -0.0033(17) -0.0032(16) -0.0069(17) C8 0.033(2) 0.032(2) 0.027(2) -0.0074(17) -0.0025(17) -0.0100(18) C9 0.029(2) 0.0241(19) 0.0229(19) -0.0033(15) -0.0042(16) -0.0087(16) C10 0.029(2) 0.050(3) 0.027(2) 0.0048(18) -0.0014(17) -0.014(2) C11 0.042(2) 0.040(2) 0.029(2) 0.0049(18) -0.0127(18) -0.019(2) C12 0.039(2) 0.035(2) 0.030(2) -0.0076(17) -0.0110(18) -0.0117(19) C13 0.026(2) 0.069(3) 0.038(2) -0.007(2) -0.0030(19) -0.012(2) C14 0.0248(18) 0.0231(19) 0.0233(19) 0.0010(15) -0.0059(15) -0.0096(16) C15 0.030(2) 0.025(2) 0.036(2) 0.0008(17) -0.0111(17) -0.0129(17) C16 0.030(2) 0.026(2) 0.042(2) 0.0095(17) -0.0150(18) -0.0079(18) C17 0.030(2) 0.039(2) 0.035(2) 0.0081(18) -0.0145(17) -0.0178(19) C18 0.038(2) 0.031(2) 0.040(2) 0.0032(18) -0.0145(18) -0.0222(19) C19 0.033(2) 0.025(2) 0.028(2) 0.0063(16) -0.0100(17) -0.0136(17) C20 0.0221(18) 0.029(2) 0.032(2) -0.0053(17) -0.0002(16) -0.0122(17) C21 0.034(2) 0.046(3) 0.042(2) -0.003(2) -0.0085(19) -0.023(2) C22 0.054(3) 0.063(3) 0.056(3) -0.017(3) 0.000(2) -0.042(3) C23 0.048(3) 0.043(3) 0.076(4) -0.011(3) 0.006(3) -0.033(2) C24 0.049(3) 0.034(3) 0.070(3) 0.010(2) -0.010(2) -0.022(2) C25 0.038(2) 0.031(2) 0.041(2) 0.0000(18) -0.0082(19) -0.0161(19) C26 0.0286(19) 0.026(2) 0.0271(19) 0.0000(15) -0.0102(16) -0.0129(17) C27 0.031(2) 0.046(3) 0.033(2) -0.0003(19) -0.0087(18) -0.013(2) C28 0.049(3) 0.051(3) 0.041(3) 0.006(2) -0.023(2) -0.014(2) C29 0.072(3) 0.048(3) 0.029(2) 0.013(2) -0.021(2) -0.034(3) C30 0.052(3) 0.048(3) 0.030(2) 0.0055(19) -0.008(2) -0.035(2) C31 0.033(2) 0.033(2) 0.030(2) 0.0023(17) -0.0114(17) -0.0189(18) C32 0.0227(18) 0.026(2) 0.0229(19) 0.0040(15) -0.0058(15) -0.0094(16) C33 0.034(2) 0.032(2) 0.033(2) 0.0027(17) -0.0078(17) -0.0186(18) C34 0.027(2) 0.041(2) 0.046(3) 0.003(2) -0.0033(18) -0.0193(19) C35 0.023(2) 0.036(2) 0.045(3) -0.0021(19) 0.0041(18) -0.0102(18) C36 0.029(2) 0.026(2) 0.042(2) -0.0021(17) -0.0018(18) -0.0109(17) C37 0.0252(19) 0.027(2) 0.030(2) 0.0071(16) -0.0066(16) -0.0126(16) C38 0.031(2) 0.0213(19) 0.028(2) 0.0038(15) -0.0078(16) -0.0152(16) C39 0.029(2) 0.027(2) 0.043(2) 0.0054(18) -0.0126(18) -0.0120(17) C40 0.040(2) 0.034(2) 0.040(2) 0.0150(18) -0.0211(19) -0.0160(19) C41 0.047(2) 0.033(2) 0.026(2) 0.0062(17) -0.0111(18) -0.020(2) C42 0.033(2) 0.029(2) 0.028(2) 0.0036(16) -0.0085(17) -0.0169(17) C43 0.0295(19) 0.0241(19) 0.0261(19) 0.0002(15) -0.0089(16) -0.0155(16) C44 0.0248(19) 0.026(2) 0.030(2) 0.0045(16) -0.0068(16) -0.0144(16) C45 0.033(2) 0.032(2) 0.033(2) -0.0005(17) -0.0050(17) -0.0172(18) C46 0.032(2) 0.042(3) 0.038(2) -0.0024(19) 0.0025(18) -0.017(2) C47 0.028(2) 0.046(3) 0.052(3) 0.008(2) -0.009(2) -0.018(2) C48 0.036(2) 0.048(3) 0.061(3) 0.008(2) -0.019(2) -0.029(2) C49 0.035(2) 0.031(2) 0.042(2) -0.0033(18) -0.0084(18) -0.0193(19) C50 0.0260(19) 0.0241(19) 0.0266(19) -0.0028(15) -0.0048(15) -0.0124(16) C51 0.031(2) 0.033(2) 0.032(2) 0.0000(17) -0.0090(17) -0.0176(18) C52 0.046(2) 0.053(3) 0.028(2) 0.0038(19) -0.0098(19) -0.032(2) C53 0.041(2) 0.040(3) 0.043(3) -0.015(2) -0.007(2) -0.018(2) C54 0.044(3) 0.023(2) 0.055(3) -0.011(2) -0.017(2) -0.0048(19) C55 0.048(2) 0.029(2) 0.038(2) 0.0042(18) -0.019(2) -0.016(2) C56 0.104(5) 0.053(3) 0.104(5) 0.023(3) -0.059(4) -0.052(3) Cl1 0.0738(9) 0.0537(8) 0.0745(9) 0.0021(7) -0.0172(7) -0.0297(7) Cl2 0.0779(9) 0.0953(11) 0.0776(9) 0.0207(8) -0.0401(8) -0.0583(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 Cu N1 2.020(3) . ? Cu N2 2.068(3) . ? Cu P1 2.2424(10) . ? Cu P2 2.3555(10) . ? P1 C26 1.829(4) . ? P1 C32 1.840(3) . ? P1 C20 1.841(4) . ? P2 C43 1.826(4) . ? P2 C44 1.837(3) . ? P2 C50 1.840(3) . ? F1 C15 1.351(4) . ? F2 C16 1.341(4) . ? F3 C17 1.340(4) . ? F4 C18 1.339(4) . ? F5 C19 1.343(4) . ? O C38 1.384(4) . ? O C37 1.392(4) . ? N1 C1 1.333(4) . ? N1 C4 1.411(4) . ? N2 C9 1.342(4) . ? N2 C6 1.405(4) . ? C1 C2 1.418(5) . ? C1 C10 1.497(5) . ? C2 C3 1.373(5) . ? C3 C4 1.445(5) . ? C3 C11 1.501(5) . ? C4 C5 1.409(5) . ? C5 C6 1.414(5) . ? C5 C14 1.500(5) . ? C6 C7 1.433(5) . ? C7 C8 1.367(5) . ? C7 C13 1.510(5) . ? C8 C9 1.409(5) . ? C9 C12 1.487(5) . ? C14 C15 1.378(5) . ? C14 C19 1.383(5) . ? C15 C16 1.376(5) . ? C16 C17 1.376(5) . ? C17 C18 1.377(5) . ? C18 C19 1.378(5) . ? C20 C21 1.386(5) . ? C20 C25 1.391(5) . ? C21 C22 1.389(6) . ? C22 C23 1.364(7) . ? C23 C24 1.379(6) . ? C24 C25 1.388(5) . ? C26 C31 1.394(5) . ? C26 C27 1.396(5) . ? C27 C28 1.380(6) . ? C28 C29 1.374(6) . ? C29 C30 1.376(6) . ? C30 C31 1.374(5) . ? C32 C33 1.388(5) . ? C32 C37 1.400(5) . ? C33 C34 1.386(5) . ? C34 C35 1.370(5) . ? C35 C36 1.385(5) . ? C36 C37 1.377(5) . ? C38 C39 1.375(5) . ? C38 C43 1.395(5) . ? C39 C40 1.387(5) . ? C40 C41 1.384(5) . ? C41 C42 1.382(5) . ? C42 C43 1.398(5) . ? C44 C49 1.384(5) . ? C44 C45 1.394(5) . ? C45 C46 1.390(5) . ? C46 C47 1.374(5) . ? C47 C48 1.380(6) . ? C48 C49 1.389(5) . ? C50 C55 1.382(5) . ? C50 C51 1.385(5) . ? C51 C52 1.391(5) . ? C52 C53 1.383(6) . ? C53 C54 1.364(6) . ? C54 C55 1.386(5) . ? C56 Cl2 1.746(6) . ? C56 Cl1 1.763(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 N1 Cu N2 88.63(11) . . ? N1 Cu P1 123.25(8) . . ? N2 Cu P1 117.03(8) . . ? N1 Cu P2 104.82(8) . . ? N2 Cu P2 111.28(8) . . ? P1 Cu P2 109.89(4) . . ? C26 P1 C32 101.08(15) . . ? C26 P1 C20 104.17(16) . . ? C32 P1 C20 102.61(15) . . ? C26 P1 Cu 117.90(12) . . ? C32 P1 Cu 117.53(11) . . ? C20 P1 Cu 111.58(12) . . ? C43 P2 C44 103.00(16) . . ? C43 P2 C50 99.62(16) . . ? C44 P2 C50 103.91(15) . . ? C43 P2 Cu 110.78(11) . . ? C44 P2 Cu 117.77(12) . . ? C50 P2 Cu 119.19(12) . . ? C38 O C37 119.7(3) . . ? C1 N1 C4 106.1(3) . . ? C1 N1 Cu 130.5(2) . . ? C4 N1 Cu 119.6(2) . . ? C9 N2 C6 106.5(3) . . ? C9 N2 Cu 130.4(2) . . ? C6 N2 Cu 114.6(2) . . ? N1 C1 C2 111.4(3) . . ? N1 C1 C10 122.0(3) . . ? C2 C1 C10 126.6(3) . . ? C3 C2 C1 107.9(3) . . ? C2 C3 C4 105.4(3) . . ? C2 C3 C11 122.5(3) . . ? C4 C3 C11 132.1(3) . . ? C5 C4 N1 122.0(3) . . ? C5 C4 C3 128.8(3) . . ? N1 C4 C3 109.2(3) . . ? C4 C5 C6 128.4(3) . . ? C4 C5 C14 115.5(3) . . ? C6 C5 C14 116.0(3) . . ? N2 C6 C5 121.6(3) . . ? N2 C6 C7 108.8(3) . . ? C5 C6 C7 129.1(3) . . ? C8 C7 C6 105.8(3) . . ? C8 C7 C13 124.1(3) . . ? C6 C7 C13 130.0(3) . . ? C7 C8 C9 108.3(3) . . ? N2 C9 C8 110.5(3) . . ? N2 C9 C12 123.0(3) . . ? C8 C9 C12 126.4(3) . . ? C15 C14 C19 116.0(3) . . ? C15 C14 C5 122.6(3) . . ? C19 C14 C5 121.3(3) . . ? F1 C15 C16 117.4(3) . . ? F1 C15 C14 119.5(3) . . ? C16 C15 C14 123.1(3) . . ? F2 C16 C17 119.5(3) . . ? F2 C16 C15 121.1(3) . . ? C17 C16 C15 119.4(3) . . ? F3 C17 C16 120.5(3) . . ? F3 C17 C18 120.0(3) . . ? C16 C17 C18 119.4(3) . . ? F4 C18 C17 119.4(3) . . ? F4 C18 C19 120.9(3) . . ? C17 C18 C19 119.7(3) . . ? F5 C19 C18 117.9(3) . . ? F5 C19 C14 119.7(3) . . ? C18 C19 C14 122.4(3) . . ? C21 C20 C25 118.6(4) . . ? C21 C20 P1 124.7(3) . . ? C25 C20 P1 116.6(3) . . ? C20 C21 C22 120.1(4) . . ? C23 C22 C21 120.9(4) . . ? C22 C23 C24 119.7(4) . . ? C23 C24 C25 120.0(5) . . ? C24 C25 C20 120.6(4) . . ? C31 C26 C27 117.5(3) . . ? C31 C26 P1 119.2(3) . . ? C27 C26 P1 123.3(3) . . ? C28 C27 C26 120.9(4) . . ? C29 C28 C27 120.4(4) . . ? C28 C29 C30 119.7(4) . . ? C31 C30 C29 120.2(4) . . ? C30 C31 C26 121.3(4) . . ? C33 C32 C37 117.2(3) . . ? C33 C32 P1 124.1(3) . . ? C37 C32 P1 118.7(3) . . ? C34 C33 C32 121.3(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.8(3) . . ? C37 C36 C35 118.7(4) . . ? C36 C37 O 118.5(3) . . ? C36 C37 C32 122.1(3) . . ? O C37 C32 119.2(3) . . ? C39 C38 O 123.0(3) . . ? C39 C38 C43 122.1(3) . . ? O C38 C43 114.9(3) . . ? C38 C39 C40 119.2(4) . . ? C41 C40 C39 120.2(4) . . ? C42 C41 C40 119.9(4) . . ? C41 C42 C43 121.0(3) . . ? C38 C43 C42 117.5(3) . . ? C38 C43 P2 116.6(3) . . ? C42 C43 P2 125.9(3) . . ? C49 C44 C45 118.9(3) . . ? C49 C44 P2 123.9(3) . . ? C45 C44 P2 117.1(3) . . ? C46 C45 C44 120.1(4) . . ? C47 C46 C45 120.8(4) . . ? C46 C47 C48 119.0(4) . . ? C47 C48 C49 121.0(4) . . ? C44 C49 C48 120.1(4) . . ? C55 C50 C51 119.2(3) . . ? C55 C50 P2 121.8(3) . . ? C51 C50 P2 119.0(3) . . ? C50 C51 C52 120.4(4) . . ? C53 C52 C51 119.4(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 C55 120.1(4) . . ? C50 C55 C54 120.4(4) . . ? Cl2 C56 Cl1 112.0(3) . . ? 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 N1 Cu P1 C26 176.73(15) . . . . ? N2 Cu P1 C26 -75.66(16) . . . . ? P2 Cu P1 C26 52.50(13) . . . . ? N1 Cu P1 C32 55.32(16) . . . . ? N2 Cu P1 C32 162.92(15) . . . . ? P2 Cu P1 C32 -68.92(13) . . . . ? N1 Cu P1 C20 -62.78(15) . . . . ? N2 Cu P1 C20 44.82(15) . . . . ? P2 Cu P1 C20 172.98(12) . . . . ? N1 Cu P2 C43 -142.82(14) . . . . ? N2 Cu P2 C43 122.79(14) . . . . ? P1 Cu P2 C43 -8.48(13) . . . . ? N1 Cu P2 C44 99.04(15) . . . . ? N2 Cu P2 C44 4.65(16) . . . . ? P1 Cu P2 C44 -126.62(13) . . . . ? N1 Cu P2 C50 -28.20(16) . . . . ? N2 Cu P2 C50 -122.59(15) . . . . ? P1 Cu P2 C50 106.14(13) . . . . ? N2 Cu N1 C1 -162.6(3) . . . . ? P1 Cu N1 C1 -40.8(3) . . . . ? P2 Cu N1 C1 85.7(3) . . . . ? N2 Cu N1 C4 42.7(2) . . . . ? P1 Cu N1 C4 164.6(2) . . . . ? P2 Cu N1 C4 -69.0(2) . . . . ? N1 Cu N2 C9 165.7(3) . . . . ? P1 Cu N2 C9 38.6(3) . . . . ? P2 Cu N2 C9 -88.9(3) . . . . ? N1 Cu N2 C6 -51.3(2) . . . . ? P1 Cu N2 C6 -178.4(2) . . . . ? P2 Cu N2 C6 54.1(2) . . . . ? C4 N1 C1 C2 -0.6(4) . . . . ? Cu N1 C1 C2 -157.8(3) . . . . ? C4 N1 C1 C10 177.3(3) . . . . ? Cu N1 C1 C10 20.1(5) . . . . ? N1 C1 C2 C3 1.1(4) . . . . ? C10 C1 C2 C3 -176.7(4) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C1 C2 C3 C11 -179.4(3) . . . . ? C1 N1 C4 C5 179.3(3) . . . . ? Cu N1 C4 C5 -20.5(4) . . . . ? C1 N1 C4 C3 -0.1(4) . . . . ? Cu N1 C4 C3 160.1(2) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? C11 C3 C4 C5 -0.5(6) . . . . ? C2 C3 C4 N1 0.7(4) . . . . ? C11 C3 C4 N1 178.8(4) . . . . ? N1 C4 C5 C6 -9.4(5) . . . . ? C3 C4 C5 C6 169.9(3) . . . . ? N1 C4 C5 C14 173.2(3) . . . . ? C3 C4 C5 C14 -7.6(5) . . . . ? C9 N2 C6 C5 -168.7(3) . . . . ? Cu N2 C6 C5 39.9(4) . . . . ? C9 N2 C6 C7 4.2(4) . . . . ? Cu N2 C6 C7 -147.3(2) . . . . ? C4 C5 C6 N2 -2.6(6) . . . . ? C14 C5 C6 N2 174.8(3) . . . . ? C4 C5 C6 C7 -173.9(4) . . . . ? C14 C5 C6 C7 3.5(5) . . . . ? N2 C6 C7 C8 -3.4(4) . . . . ? C5 C6 C7 C8 168.7(4) . . . . ? N2 C6 C7 C13 174.4(4) . . . . ? C5 C6 C7 C13 -13.5(7) . . . . ? C6 C7 C8 C9 1.3(4) . . . . ? C13 C7 C8 C9 -176.6(4) . . . . ? C6 N2 C9 C8 -3.4(4) . . . . ? Cu N2 C9 C8 141.8(3) . . . . ? C6 N2 C9 C12 173.3(3) . . . . ? Cu N2 C9 C12 -41.5(5) . . . . ? C7 C8 C9 N2 1.3(5) . . . . ? C7 C8 C9 C12 -175.3(4) . . . . ? C4 C5 C14 C15 95.6(4) . . . . ? C6 C5 C14 C15 -82.2(4) . . . . ? C4 C5 C14 C19 -82.2(4) . . . . ? C6 C5 C14 C19 100.0(4) . . . . ? C19 C14 C15 F1 179.8(3) . . . . ? C5 C14 C15 F1 1.9(5) . . . . ? C19 C14 C15 C16 0.8(5) . . . . ? C5 C14 C15 C16 -177.1(3) . . . . ? F1 C15 C16 F2 0.9(5) . . . . ? C14 C15 C16 F2 179.8(3) . . . . ? F1 C15 C16 C17 -178.7(3) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? F2 C16 C17 F3 -0.6(6) . . . . ? C15 C16 C17 F3 179.0(3) . . . . ? F2 C16 C17 C18 179.7(3) . . . . ? C15 C16 C17 C18 -0.7(6) . . . . ? F3 C17 C18 F4 0.0(6) . . . . ? C16 C17 C18 F4 179.7(3) . . . . ? F3 C17 C18 C19 -179.6(3) . . . . ? C16 C17 C18 C19 0.0(6) . . . . ? F4 C18 C19 F5 0.3(5) . . . . ? C17 C18 C19 F5 179.9(3) . . . . ? F4 C18 C19 C14 -178.5(3) . . . . ? C17 C18 C19 C14 1.1(6) . . . . ? C15 C14 C19 F5 179.7(3) . . . . ? C5 C14 C19 F5 -2.4(5) . . . . ? C15 C14 C19 C18 -1.5(5) . . . . ? C5 C14 C19 C18 176.4(3) . . . . ? C26 P1 C20 C21 -20.2(3) . . . . ? C32 P1 C20 C21 84.9(3) . . . . ? Cu P1 C20 C21 -148.4(3) . . . . ? C26 P1 C20 C25 156.6(3) . . . . ? C32 P1 C20 C25 -98.3(3) . . . . ? Cu P1 C20 C25 28.4(3) . . . . ? C25 C20 C21 C22 0.0(6) . . . . ? P1 C20 C21 C22 176.7(3) . . . . ? C20 C21 C22 C23 1.2(6) . . . . ? C21 C22 C23 C24 -1.3(7) . . . . ? C22 C23 C24 C25 0.2(7) . . . . ? C23 C24 C25 C20 0.9(6) . . . . ? C21 C20 C25 C24 -1.0(6) . . . . ? P1 C20 C25 C24 -178.0(3) . . . . ? C32 P1 C26 C31 146.0(3) . . . . ? C20 P1 C26 C31 -107.8(3) . . . . ? Cu P1 C26 C31 16.5(3) . . . . ? C32 P1 C26 C27 -32.2(3) . . . . ? C20 P1 C26 C27 74.0(3) . . . . ? Cu P1 C26 C27 -161.7(3) . . . . ? C31 C26 C27 C28 0.6(6) . . . . ? P1 C26 C27 C28 178.9(3) . . . . ? C26 C27 C28 C29 0.4(6) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C28 C29 C30 C31 -0.9(6) . . . . ? C29 C30 C31 C26 2.0(6) . . . . ? C27 C26 C31 C30 -1.8(5) . . . . ? P1 C26 C31 C30 179.9(3) . . . . ? C26 P1 C32 C33 95.6(3) . . . . ? C20 P1 C32 C33 -11.9(4) . . . . ? Cu P1 C32 C33 -134.7(3) . . . . ? C26 P1 C32 C37 -87.4(3) . . . . ? C20 P1 C32 C37 165.2(3) . . . . ? Cu P1 C32 C37 42.4(3) . . . . ? C37 C32 C33 C34 -1.2(5) . . . . ? P1 C32 C33 C34 175.9(3) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C33 C34 C35 C36 1.1(6) . . . . ? C34 C35 C36 C37 -0.1(6) . . . . ? C35 C36 C37 O -177.0(3) . . . . ? C35 C36 C37 C32 -1.5(6) . . . . ? C38 O C37 C36 -101.6(4) . . . . ? C38 O C37 C32 82.8(4) . . . . ? C33 C32 C37 C36 2.1(5) . . . . ? P1 C32 C37 C36 -175.1(3) . . . . ? C33 C32 C37 O 177.6(3) . . . . ? P1 C32 C37 O 0.3(4) . . . . ? C37 O C38 C39 31.1(5) . . . . ? C37 O C38 C43 -150.5(3) . . . . ? O C38 C39 C40 178.3(3) . . . . ? C43 C38 C39 C40 0.0(5) . . . . ? C38 C39 C40 C41 -2.4(6) . . . . ? C39 C40 C41 C42 2.6(6) . . . . ? C40 C41 C42 C43 -0.4(5) . . . . ? C39 C38 C43 C42 2.1(5) . . . . ? O C38 C43 C42 -176.3(3) . . . . ? C39 C38 C43 P2 -175.0(3) . . . . ? O C38 C43 P2 6.5(4) . . . . ? C41 C42 C43 C38 -1.9(5) . . . . ? C41 C42 C43 P2 174.9(3) . . . . ? C44 P2 C43 C38 -179.8(3) . . . . ? C50 P2 C43 C38 -73.0(3) . . . . ? Cu P2 C43 C38 53.4(3) . . . . ? C44 P2 C43 C42 3.3(3) . . . . ? C50 P2 C43 C42 110.1(3) . . . . ? Cu P2 C43 C42 -123.5(3) . . . . ? C43 P2 C44 C49 90.7(3) . . . . ? C50 P2 C44 C49 -12.8(4) . . . . ? Cu P2 C44 C49 -147.1(3) . . . . ? C43 P2 C44 C45 -92.1(3) . . . . ? C50 P2 C44 C45 164.3(3) . . . . ? Cu P2 C44 C45 30.1(3) . . . . ? C49 C44 C45 C46 -1.7(6) . . . . ? P2 C44 C45 C46 -179.0(3) . . . . ? C44 C45 C46 C47 1.5(6) . . . . ? C45 C46 C47 C48 -0.2(6) . . . . ? C46 C47 C48 C49 -0.8(7) . . . . ? C45 C44 C49 C48 0.7(6) . . . . ? P2 C44 C49 C48 177.8(3) . . . . ? C47 C48 C49 C44 0.5(6) . . . . ? C43 P2 C50 C55 -22.9(3) . . . . ? C44 P2 C50 C55 83.2(3) . . . . ? Cu P2 C50 C55 -143.3(3) . . . . ? C43 P2 C50 C51 154.2(3) . . . . ? C44 P2 C50 C51 -99.7(3) . . . . ? Cu P2 C50 C51 33.7(3) . . . . ? C55 C50 C51 C52 0.9(5) . . . . ? P2 C50 C51 C52 -176.2(3) . . . . ? C50 C51 C52 C53 -0.4(6) . . . . ? C51 C52 C53 C54 -0.6(6) . . . . ? C52 C53 C54 C55 1.0(6) . . . . ? C51 C50 C55 C54 -0.5(6) . . . . ? P2 C50 C55 C54 176.5(3) . . . . ? C53 C54 C55 C50 -0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.541 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.073 data_t101 _database_code_depnum_ccdc_archive 'CCDC 871241' #TrackingRef 'T101.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H44 Cu F5 N2 P2' _chemical_formula_weight 953.40 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 '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 12.774(11) _cell_length_b 13.536(12) _cell_length_c 14.094(12) _cell_angle_alpha 76.654(15) _cell_angle_beta 87.587(16) _cell_angle_gamma 79.347(14) _cell_volume 2330(4) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 2059 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 21.51 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8849 _exptl_absorpt_correction_T_max 0.9105 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13174 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.07 _reflns_number_total 8950 _reflns_number_gt 6174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0583P)^2^+0.4278P] 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 8950 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu Cu -0.29062(4) 0.63185(3) 0.72341(3) 0.03561(15) Uani 1 1 d . . . P1 P -0.22848(8) 0.78540(8) 0.69640(8) 0.0375(3) Uani 1 1 d . . . P2 P -0.46991(8) 0.63446(7) 0.71982(7) 0.0346(2) Uani 1 1 d . . . N1 N -0.2070(2) 0.5382(2) 0.6402(2) 0.0388(8) Uani 1 1 d . . . N2 N -0.2285(2) 0.5366(2) 0.8499(2) 0.0346(7) Uani 1 1 d . . . F1 F 0.1079(2) 0.3724(2) 0.7552(2) 0.0764(9) Uani 1 1 d . . . F2 F 0.2357(2) 0.1862(2) 0.8023(2) 0.0899(10) Uani 1 1 d . . . F3 F 0.1507(2) 0.0151(2) 0.8710(2) 0.0917(10) Uani 1 1 d . . . F4 F -0.0636(3) 0.0304(2) 0.8935(3) 0.0980(11) Uani 1 1 d . . . F5 F -0.1917(2) 0.2170(2) 0.8475(2) 0.0775(9) Uani 1 1 d . . . C1 C -0.2111(3) 0.5502(3) 0.5440(3) 0.0482(11) Uani 1 1 d . . . C2 C -0.1572(4) 0.4594(4) 0.5158(4) 0.0697(15) Uani 1 1 d . . . H2A H -0.1504 0.4496 0.4511 0.084 Uiso 1 1 calc R . . C3 C -0.1174(4) 0.3896(4) 0.5970(3) 0.0577(13) Uani 1 1 d . . . C4 C -0.1470(3) 0.4391(3) 0.6776(3) 0.0420(10) Uani 1 1 d . . . C5 C -0.1175(3) 0.4046(3) 0.7754(3) 0.0365(9) Uani 1 1 d . . . C6 C -0.1457(3) 0.4506(3) 0.8546(3) 0.0355(9) Uani 1 1 d . . . C7 C -0.1063(3) 0.4178(3) 0.9535(3) 0.0421(10) Uani 1 1 d . . . C8 C -0.1668(3) 0.4823(3) 1.0041(3) 0.0456(10) Uani 1 1 d . . . H8A H -0.1592 0.4804 1.0713 0.055 Uiso 1 1 calc R . . C9 C -0.2424(3) 0.5522(3) 0.9402(3) 0.0399(10) Uani 1 1 d . . . C10 C -0.2605(4) 0.6479(4) 0.4764(3) 0.0674(14) Uani 1 1 d . . . H10A H -0.2922 0.6983 0.5142 0.101 Uiso 1 1 calc R . . H10B H -0.3160 0.6342 0.4378 0.101 Uiso 1 1 calc R . . H10C H -0.2059 0.6756 0.4327 0.101 Uiso 1 1 calc R . . C11 C -0.0566(5) 0.2835(4) 0.5928(4) 0.091(2) Uani 1 1 d . . . H11A H -0.0514 0.2768 0.5249 0.137 Uiso 1 1 calc R . . H11B H -0.0942 0.2307 0.6313 0.137 Uiso 1 1 calc R . . H11C H 0.0151 0.2742 0.6194 0.137 Uiso 1 1 calc R . . C12 C -0.3318(4) 0.6294(3) 0.9667(3) 0.0549(12) Uani 1 1 d . . . H12A H -0.3719 0.6680 0.9078 0.082 Uiso 1 1 calc R . . H12B H -0.3028 0.6772 0.9965 0.082 Uiso 1 1 calc R . . H12C H -0.3792 0.5934 1.0131 0.082 Uiso 1 1 calc R . . C13 C -0.0151(4) 0.3344(3) 0.9982(3) 0.0610(13) Uani 1 1 d . . . H13A H -0.0102 0.3326 1.0678 0.092 Uiso 1 1 calc R . . H13B H 0.0515 0.3490 0.9658 0.092 Uiso 1 1 calc R . . H13C H -0.0275 0.2675 0.9901 0.092 Uiso 1 1 calc R . . C14 C -0.0462(3) 0.3003(3) 0.8001(3) 0.0437(10) Uani 1 1 d . . . C15 C 0.0634(3) 0.2888(3) 0.7890(3) 0.0495(11) Uani 1 1 d . . . C16 C 0.1296(4) 0.1941(4) 0.8131(4) 0.0583(13) Uani 1 1 d . . . C17 C 0.0870(4) 0.1081(4) 0.8474(4) 0.0628(14) Uani 1 1 d . . . C18 C -0.0212(4) 0.1153(3) 0.8600(4) 0.0624(13) Uani 1 1 d . . . C19 C -0.0854(3) 0.2117(3) 0.8355(3) 0.0529(12) Uani 1 1 d . . . C20 C -0.2808(3) 0.8821(3) 0.7680(3) 0.0422(10) Uani 1 1 d . . . C21 C -0.2600(4) 0.8580(4) 0.8669(3) 0.0613(13) Uani 1 1 d . . . H21A H -0.2137 0.7955 0.8950 0.074 Uiso 1 1 calc R . . C22 C -0.3058(5) 0.9237(5) 0.9262(4) 0.0841(18) Uani 1 1 d . . . H22A H -0.2915 0.9056 0.9942 0.101 Uiso 1 1 calc R . . C23 C -0.3719(5) 1.0152(4) 0.8854(5) 0.0815(17) Uani 1 1 d . . . H23A H -0.4037 1.0601 0.9255 0.098 Uiso 1 1 calc R . . C24 C -0.3918(5) 1.0410(4) 0.7881(4) 0.0763(16) Uani 1 1 d . . . H24A H -0.4371 1.1042 0.7601 0.092 Uiso 1 1 calc R . . C25 C -0.3460(4) 0.9752(3) 0.7296(3) 0.0568(12) Uani 1 1 d . . . H25A H -0.3598 0.9946 0.6614 0.068 Uiso 1 1 calc R . . C26 C -0.2429(4) 0.8614(3) 0.5706(3) 0.0444(10) Uani 1 1 d . . . C27 C -0.1587(4) 0.8935(3) 0.5137(3) 0.0615(13) Uani 1 1 d . . . H27A H -0.0898 0.8805 0.5418 0.074 Uiso 1 1 calc R . . C28 C -0.1735(5) 0.9440(4) 0.4170(4) 0.0867(19) Uani 1 1 d . . . H28A H -0.1147 0.9640 0.3788 0.104 Uiso 1 1 calc R . . C29 C -0.2719(6) 0.9649(5) 0.3767(4) 0.093(2) Uani 1 1 d . . . H29A H -0.2820 1.0006 0.3104 0.112 Uiso 1 1 calc R . . C30 C -0.3568(5) 0.9349(4) 0.4310(4) 0.0808(18) Uani 1 1 d . . . H30A H -0.4255 0.9498 0.4021 0.097 Uiso 1 1 calc R . . C31 C -0.3435(4) 0.8831(3) 0.5276(3) 0.0582(13) Uani 1 1 d . . . H31A H -0.4027 0.8622 0.5647 0.070 Uiso 1 1 calc R . . C32 C -0.0842(3) 0.7648(3) 0.7169(3) 0.0417(10) Uani 1 1 d . . . C33 C -0.0346(4) 0.8396(4) 0.7379(4) 0.0624(13) Uani 1 1 d . . . H33A H -0.0752 0.9042 0.7438 0.075 Uiso 1 1 calc R . . C34 C 0.0760(4) 0.8193(4) 0.7504(4) 0.0748(16) Uani 1 1 d . . . H34A H 0.1107 0.8704 0.7646 0.090 Uiso 1 1 calc R . . C35 C 0.1349(4) 0.7253(5) 0.7422(4) 0.0684(15) Uani 1 1 d . . . H35A H 0.2100 0.7121 0.7505 0.082 Uiso 1 1 calc R . . C36 C 0.0855(4) 0.6516(4) 0.7223(3) 0.0598(13) Uani 1 1 d . . . H36A H 0.1264 0.5870 0.7166 0.072 Uiso 1 1 calc R . . C37 C -0.0240(3) 0.6699(3) 0.7103(3) 0.0482(11) Uani 1 1 d . . . H37A H -0.0581 0.6176 0.6976 0.058 Uiso 1 1 calc R . . C38 C -0.5447(3) 0.6863(3) 0.6056(3) 0.0385(9) Uani 1 1 d . . . C39 C -0.5213(4) 0.6329(3) 0.5317(3) 0.0567(12) Uani 1 1 d . . . H39A H -0.4676 0.5727 0.5419 0.068 Uiso 1 1 calc R . . C40 C -0.5747(4) 0.6659(4) 0.4442(3) 0.0666(14) Uani 1 1 d . . . H40A H -0.5577 0.6285 0.3946 0.080 Uiso 1 1 calc R . . C41 C -0.6523(4) 0.7528(4) 0.4283(4) 0.0689(15) Uani 1 1 d . . . H41A H -0.6898 0.7750 0.3681 0.083 Uiso 1 1 calc R . . C42 C -0.6756(4) 0.8072(4) 0.4990(4) 0.0714(15) Uani 1 1 d . . . H42A H -0.7288 0.8677 0.4878 0.086 Uiso 1 1 calc R . . C43 C -0.6218(4) 0.7744(3) 0.5874(3) 0.0536(12) Uani 1 1 d . . . H43A H -0.6383 0.8132 0.6360 0.064 Uiso 1 1 calc R . . C44 C -0.5488(3) 0.7029(3) 0.8051(3) 0.0358(9) Uani 1 1 d . . . C45 C -0.5405(3) 0.8053(3) 0.7996(3) 0.0450(10) Uani 1 1 d . . . H45A H -0.4949 0.8375 0.7521 0.054 Uiso 1 1 calc R . . C46 C -0.5970(4) 0.8611(3) 0.8619(3) 0.0515(11) Uani 1 1 d . . . H46A H -0.5906 0.9311 0.8563 0.062 Uiso 1 1 calc R . . C47 C -0.6627(4) 0.8155(4) 0.9320(3) 0.0534(12) Uani 1 1 d . . . H47A H -0.7022 0.8540 0.9743 0.064 Uiso 1 1 calc R . . C48 C -0.6704(3) 0.7144(4) 0.9403(3) 0.0522(11) Uani 1 1 d . . . H48A H -0.7145 0.6822 0.9893 0.063 Uiso 1 1 calc R . . C49 C -0.6144(3) 0.6585(3) 0.8775(3) 0.0441(10) Uani 1 1 d . . . H49A H -0.6208 0.5884 0.8842 0.053 Uiso 1 1 calc R . . C50 C -0.5052(3) 0.5055(3) 0.7533(3) 0.0358(9) Uani 1 1 d . . . C51 C -0.4303(3) 0.4223(3) 0.7980(3) 0.0438(10) Uani 1 1 d . . . H51A H -0.3611 0.4324 0.8110 0.053 Uiso 1 1 calc R . . C52 C -0.4551(4) 0.3240(3) 0.8241(3) 0.0494(11) Uani 1 1 d . . . H52A H -0.4027 0.2672 0.8544 0.059 Uiso 1 1 calc R . . C53 C -0.5547(4) 0.3087(3) 0.8065(3) 0.0490(11) Uani 1 1 d . . . H53A H -0.5716 0.2414 0.8245 0.059 Uiso 1 1 calc R . . C54 C -0.6302(3) 0.3910(3) 0.7628(3) 0.0471(11) Uani 1 1 d . . . H54A H -0.6997 0.3806 0.7513 0.057 Uiso 1 1 calc R . . C55 C -0.6057(3) 0.4883(3) 0.7355(3) 0.0435(10) Uani 1 1 d . . . H55A H -0.6580 0.5445 0.7041 0.052 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 Cu 0.0353(3) 0.0365(3) 0.0340(3) -0.0088(2) -0.0001(2) -0.0027(2) P1 0.0360(6) 0.0349(6) 0.0390(6) -0.0041(5) -0.0037(5) -0.0044(4) P2 0.0325(6) 0.0330(5) 0.0373(6) -0.0082(4) -0.0008(4) -0.0032(4) N1 0.0377(19) 0.0447(19) 0.0347(19) -0.0144(15) 0.0013(15) -0.0027(15) N2 0.0318(18) 0.0385(18) 0.0322(18) -0.0071(14) 0.0006(14) -0.0045(14) F1 0.0404(16) 0.0603(17) 0.124(3) -0.0112(17) 0.0104(15) -0.0127(13) F2 0.0352(16) 0.083(2) 0.145(3) -0.028(2) -0.0037(17) 0.0106(15) F3 0.081(2) 0.0533(18) 0.127(3) -0.0189(17) -0.0177(19) 0.0243(16) F4 0.093(2) 0.0439(17) 0.153(3) -0.0101(18) 0.009(2) -0.0203(16) F5 0.0431(17) 0.0603(17) 0.132(3) -0.0252(17) 0.0105(16) -0.0147(13) C1 0.049(3) 0.062(3) 0.034(2) -0.016(2) 0.002(2) -0.005(2) C2 0.073(4) 0.090(4) 0.051(3) -0.045(3) 0.004(3) 0.008(3) C3 0.054(3) 0.066(3) 0.057(3) -0.035(3) -0.003(2) 0.006(2) C4 0.034(2) 0.042(2) 0.052(3) -0.020(2) 0.0052(19) -0.0035(18) C5 0.028(2) 0.035(2) 0.047(3) -0.0107(18) -0.0011(18) -0.0050(16) C6 0.029(2) 0.037(2) 0.040(2) -0.0068(18) -0.0037(17) -0.0045(17) C7 0.037(2) 0.040(2) 0.045(3) -0.0001(19) -0.0059(19) -0.0055(18) C8 0.049(3) 0.052(3) 0.033(2) -0.006(2) -0.005(2) -0.008(2) C9 0.043(2) 0.041(2) 0.037(2) -0.0116(19) -0.0010(19) -0.0049(18) C10 0.094(4) 0.070(3) 0.035(3) -0.010(2) -0.006(3) -0.007(3) C11 0.104(5) 0.088(4) 0.081(4) -0.054(3) -0.013(3) 0.034(3) C12 0.062(3) 0.065(3) 0.035(2) -0.017(2) 0.001(2) 0.002(2) C13 0.061(3) 0.058(3) 0.055(3) -0.007(2) -0.018(2) 0.008(2) C14 0.035(2) 0.043(2) 0.053(3) -0.017(2) -0.001(2) -0.0004(19) C15 0.039(3) 0.045(3) 0.065(3) -0.014(2) 0.002(2) -0.006(2) C16 0.034(3) 0.059(3) 0.079(4) -0.020(3) -0.003(2) 0.005(2) C17 0.059(3) 0.045(3) 0.078(4) -0.018(3) -0.011(3) 0.013(2) C18 0.063(3) 0.039(3) 0.085(4) -0.015(2) 0.004(3) -0.008(2) C19 0.038(3) 0.050(3) 0.072(3) -0.020(2) 0.005(2) -0.004(2) C20 0.045(3) 0.039(2) 0.046(3) -0.0133(19) 0.001(2) -0.0130(19) C21 0.069(3) 0.063(3) 0.054(3) -0.016(3) -0.008(3) -0.012(3) C22 0.106(5) 0.103(5) 0.056(4) -0.037(3) 0.002(3) -0.029(4) C23 0.103(5) 0.071(4) 0.086(5) -0.046(3) 0.018(4) -0.023(3) C24 0.097(5) 0.054(3) 0.078(4) -0.023(3) 0.010(3) -0.005(3) C25 0.070(3) 0.042(3) 0.058(3) -0.014(2) 0.004(2) -0.006(2) C26 0.055(3) 0.035(2) 0.037(2) -0.0037(18) -0.003(2) 0.001(2) C27 0.064(3) 0.050(3) 0.059(3) 0.002(2) 0.004(3) 0.001(2) C28 0.105(5) 0.069(4) 0.062(4) 0.011(3) 0.024(3) 0.008(3) C29 0.132(6) 0.074(4) 0.047(4) -0.004(3) -0.003(4) 0.034(4) C30 0.096(5) 0.070(4) 0.065(4) -0.017(3) -0.033(3) 0.025(3) C31 0.064(3) 0.051(3) 0.051(3) -0.008(2) -0.009(2) 0.007(2) C32 0.039(2) 0.046(2) 0.038(2) -0.0011(19) -0.0063(19) -0.0124(19) C33 0.053(3) 0.052(3) 0.081(4) -0.006(3) -0.012(3) -0.015(2) C34 0.062(4) 0.075(4) 0.091(4) -0.004(3) -0.016(3) -0.035(3) C35 0.036(3) 0.095(4) 0.069(4) -0.004(3) -0.008(2) -0.015(3) C36 0.041(3) 0.081(4) 0.056(3) -0.020(3) -0.003(2) -0.001(3) C37 0.040(3) 0.058(3) 0.048(3) -0.014(2) -0.002(2) -0.009(2) C38 0.036(2) 0.040(2) 0.038(2) -0.0067(18) -0.0022(18) -0.0062(18) C39 0.070(3) 0.052(3) 0.045(3) -0.014(2) -0.012(2) 0.003(2) C40 0.093(4) 0.069(3) 0.039(3) -0.013(2) -0.010(3) -0.014(3) C41 0.077(4) 0.078(4) 0.044(3) 0.001(3) -0.024(3) -0.006(3) C42 0.070(4) 0.072(4) 0.060(3) -0.007(3) -0.018(3) 0.013(3) C43 0.057(3) 0.054(3) 0.045(3) -0.012(2) -0.004(2) 0.003(2) C44 0.030(2) 0.040(2) 0.037(2) -0.0101(18) -0.0041(17) -0.0029(17) C45 0.048(3) 0.040(2) 0.047(3) -0.007(2) 0.004(2) -0.0100(19) C46 0.060(3) 0.042(2) 0.053(3) -0.018(2) -0.003(2) -0.001(2) C47 0.048(3) 0.064(3) 0.049(3) -0.028(2) 0.001(2) 0.005(2) C48 0.048(3) 0.069(3) 0.045(3) -0.023(2) 0.012(2) -0.014(2) C49 0.046(3) 0.044(2) 0.046(3) -0.014(2) 0.002(2) -0.013(2) C50 0.036(2) 0.036(2) 0.036(2) -0.0103(17) -0.0004(17) -0.0061(17) C51 0.041(2) 0.042(2) 0.050(3) -0.010(2) -0.008(2) -0.0101(19) C52 0.054(3) 0.039(2) 0.051(3) -0.002(2) -0.009(2) -0.007(2) C53 0.055(3) 0.043(2) 0.054(3) -0.017(2) 0.007(2) -0.016(2) C54 0.039(3) 0.055(3) 0.055(3) -0.021(2) 0.003(2) -0.017(2) C55 0.036(2) 0.044(2) 0.050(3) -0.013(2) -0.0040(19) -0.0007(19) _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 Cu N2 2.038(3) . ? Cu N1 2.050(3) . ? Cu P2 2.287(2) . ? Cu P1 2.305(2) . ? P1 C26 1.831(4) . ? P1 C32 1.837(4) . ? P1 C20 1.846(4) . ? P2 C38 1.833(4) . ? P2 C50 1.835(4) . ? P2 C44 1.840(4) . ? N1 C1 1.329(5) . ? N1 C4 1.412(5) . ? N2 C9 1.336(5) . ? N2 C6 1.411(4) . ? F1 C15 1.340(5) . ? F2 C16 1.345(5) . ? F3 C17 1.344(5) . ? F4 C18 1.339(5) . ? F5 C19 1.352(5) . ? C1 C2 1.425(6) . ? C1 C10 1.489(6) . ? C2 C3 1.354(6) . ? C3 C4 1.449(5) . ? C3 C11 1.515(6) . ? C4 C5 1.394(5) . ? C5 C6 1.404(5) . ? C5 C14 1.505(5) . ? C6 C7 1.444(5) . ? C7 C8 1.364(5) . ? C7 C13 1.508(5) . ? C8 C9 1.407(5) . ? C9 C12 1.496(5) . ? C14 C19 1.364(6) . ? C14 C15 1.386(6) . ? C15 C16 1.377(6) . ? C16 C17 1.355(7) . ? C17 C18 1.375(7) . ? C18 C19 1.383(6) . ? C20 C25 1.382(6) . ? C20 C21 1.382(6) . ? C21 C22 1.393(7) . ? C22 C23 1.380(7) . ? C23 C24 1.358(7) . ? C24 C25 1.386(6) . ? C26 C27 1.389(6) . ? C26 C31 1.396(6) . ? C27 C28 1.379(7) . ? C28 C29 1.356(8) . ? C29 C30 1.371(9) . ? C30 C31 1.381(7) . ? C32 C33 1.381(6) . ? C32 C37 1.390(6) . ? C33 C34 1.400(6) . ? C34 C35 1.380(7) . ? C35 C36 1.360(7) . ? C36 C37 1.386(6) . ? C38 C43 1.380(5) . ? C38 C39 1.391(5) . ? C39 C40 1.374(6) . ? C40 C41 1.372(7) . ? C41 C42 1.364(7) . ? C42 C43 1.386(6) . ? C44 C49 1.391(6) . ? C44 C45 1.395(5) . ? C45 C46 1.384(6) . ? C46 C47 1.379(6) . ? C47 C48 1.369(6) . ? C48 C49 1.386(5) . ? C50 C51 1.381(5) . ? C50 C55 1.389(5) . ? C51 C52 1.387(6) . ? C52 C53 1.369(6) . ? C53 C54 1.374(6) . ? C54 C55 1.375(6) . ? 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 N2 Cu N1 92.49(14) . . ? N2 Cu P2 109.39(9) . . ? N1 Cu P2 112.20(10) . . ? N2 Cu P1 109.88(10) . . ? N1 Cu P1 110.10(11) . . ? P2 Cu P1 119.46(5) . . ? C26 P1 C32 102.62(19) . . ? C26 P1 C20 102.74(19) . . ? C32 P1 C20 102.48(19) . . ? C26 P1 Cu 114.48(14) . . ? C32 P1 Cu 111.96(14) . . ? C20 P1 Cu 120.43(15) . . ? C38 P2 C50 99.70(17) . . ? C38 P2 C44 102.81(18) . . ? C50 P2 C44 103.24(18) . . ? C38 P2 Cu 120.52(14) . . ? C50 P2 Cu 113.34(13) . . ? C44 P2 Cu 114.83(13) . . ? C1 N1 C4 106.8(3) . . ? C1 N1 Cu 127.7(3) . . ? C4 N1 Cu 124.8(3) . . ? C9 N2 C6 107.0(3) . . ? C9 N2 Cu 127.7(3) . . ? C6 N2 Cu 124.2(2) . . ? N1 C1 C2 110.6(4) . . ? N1 C1 C10 123.6(4) . . ? C2 C1 C10 125.6(4) . . ? C3 C2 C1 108.3(4) . . ? C2 C3 C4 106.0(4) . . ? C2 C3 C11 121.8(4) . . ? C4 C3 C11 132.2(4) . . ? C5 C4 N1 122.3(3) . . ? C5 C4 C3 129.2(4) . . ? N1 C4 C3 108.3(4) . . ? C4 C5 C6 130.1(3) . . ? C4 C5 C14 114.7(3) . . ? C6 C5 C14 115.1(3) . . ? C5 C6 N2 122.9(3) . . ? C5 C6 C7 129.0(3) . . ? N2 C6 C7 108.0(3) . . ? C8 C7 C6 105.9(3) . . ? C8 C7 C13 123.4(4) . . ? C6 C7 C13 130.7(4) . . ? C7 C8 C9 108.6(4) . . ? N2 C9 C8 110.4(3) . . ? N2 C9 C12 122.7(3) . . ? C8 C9 C12 126.7(4) . . ? C19 C14 C15 116.0(4) . . ? C19 C14 C5 122.1(4) . . ? C15 C14 C5 121.8(4) . . ? F1 C15 C16 118.1(4) . . ? F1 C15 C14 119.5(4) . . ? C16 C15 C14 122.4(4) . . ? F2 C16 C17 119.8(4) . . ? F2 C16 C15 120.7(5) . . ? C17 C16 C15 119.5(4) . . ? F3 C17 C16 120.1(5) . . ? F3 C17 C18 119.5(5) . . ? C16 C17 C18 120.4(4) . . ? F4 C18 C17 120.5(4) . . ? F4 C18 C19 120.9(5) . . ? C17 C18 C19 118.6(4) . . ? F5 C19 C14 119.3(4) . . ? F5 C19 C18 117.7(4) . . ? C14 C19 C18 123.1(4) . . ? C25 C20 C21 117.6(4) . . ? C25 C20 P1 123.6(3) . . ? C21 C20 P1 118.6(3) . . ? C20 C21 C22 121.2(5) . . ? C23 C22 C21 119.5(5) . . ? C24 C23 C22 120.1(5) . . ? C23 C24 C25 120.0(5) . . ? C20 C25 C24 121.6(5) . . ? C27 C26 C31 118.1(4) . . ? C27 C26 P1 123.9(4) . . ? C31 C26 P1 117.9(4) . . ? C28 C27 C26 121.1(5) . . ? C29 C28 C27 120.0(6) . . ? C28 C29 C30 120.4(6) . . ? C29 C30 C31 120.5(6) . . ? C30 C31 C26 119.9(5) . . ? C33 C32 C37 119.7(4) . . ? C33 C32 P1 122.5(3) . . ? C37 C32 P1 117.9(3) . . ? C32 C33 C34 119.3(5) . . ? C35 C34 C33 120.4(5) . . ? C36 C35 C34 120.0(5) . . ? C35 C36 C37 120.5(5) . . ? C36 C37 C32 120.1(4) . . ? C43 C38 C39 117.8(4) . . ? C43 C38 P2 124.8(3) . . ? C39 C38 P2 117.4(3) . . ? C40 C39 C38 121.0(4) . . ? C41 C40 C39 120.2(5) . . ? C42 C41 C40 119.8(4) . . ? C41 C42 C43 120.3(5) . . ? C38 C43 C42 120.9(4) . . ? C49 C44 C45 117.1(4) . . ? C49 C44 P2 124.5(3) . . ? C45 C44 P2 118.4(3) . . ? C46 C45 C44 121.4(4) . . ? C47 C46 C45 120.2(4) . . ? C48 C47 C46 119.5(4) . . ? C47 C48 C49 120.4(4) . . ? C48 C49 C44 121.4(4) . . ? C51 C50 C55 118.4(4) . . ? C51 C50 P2 119.5(3) . . ? C55 C50 P2 122.1(3) . . ? C50 C51 C52 120.6(4) . . ? C53 C52 C51 120.2(4) . . ? C52 C53 C54 119.8(4) . . ? C53 C54 C55 120.3(4) . . ? C54 C55 C50 120.8(4) . . ? 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 N2 Cu P1 C26 161.96(17) . . . . ? N1 Cu P1 C26 61.51(19) . . . . ? P2 Cu P1 C26 -70.47(16) . . . . ? N2 Cu P1 C32 45.70(17) . . . . ? N1 Cu P1 C32 -54.76(17) . . . . ? P2 Cu P1 C32 173.27(14) . . . . ? N2 Cu P1 C20 -74.78(19) . . . . ? N1 Cu P1 C20 -175.23(18) . . . . ? P2 Cu P1 C20 52.79(17) . . . . ? N2 Cu P2 C38 -165.03(17) . . . . ? N1 Cu P2 C38 -63.88(19) . . . . ? P1 Cu P2 C38 67.17(15) . . . . ? N2 Cu P2 C50 -47.17(16) . . . . ? N1 Cu P2 C50 53.98(17) . . . . ? P1 Cu P2 C50 -174.97(13) . . . . ? N2 Cu P2 C44 71.16(18) . . . . ? N1 Cu P2 C44 172.31(17) . . . . ? P1 Cu P2 C44 -56.64(15) . . . . ? N2 Cu N1 C1 177.0(4) . . . . ? P2 Cu N1 C1 64.9(4) . . . . ? P1 Cu N1 C1 -70.7(4) . . . . ? N2 Cu N1 C4 8.1(3) . . . . ? P2 Cu N1 C4 -104.0(3) . . . . ? P1 Cu N1 C4 120.4(3) . . . . ? N1 Cu N2 C9 175.0(3) . . . . ? P2 Cu N2 C9 -70.4(3) . . . . ? P1 Cu N2 C9 62.6(3) . . . . ? N1 Cu N2 C6 8.1(3) . . . . ? P2 Cu N2 C6 122.7(3) . . . . ? P1 Cu N2 C6 -104.3(3) . . . . ? C4 N1 C1 C2 1.6(5) . . . . ? Cu N1 C1 C2 -168.8(3) . . . . ? C4 N1 C1 C10 -175.3(4) . . . . ? Cu N1 C1 C10 14.2(6) . . . . ? N1 C1 C2 C3 -0.8(6) . . . . ? C10 C1 C2 C3 176.0(5) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C11 179.1(5) . . . . ? C1 N1 C4 C5 173.3(4) . . . . ? Cu N1 C4 C5 -15.8(5) . . . . ? C1 N1 C4 C3 -1.9(5) . . . . ? Cu N1 C4 C3 169.0(3) . . . . ? C2 C3 C4 C5 -173.4(5) . . . . ? C11 C3 C4 C5 7.3(9) . . . . ? C2 C3 C4 N1 1.4(5) . . . . ? C11 C3 C4 N1 -178.0(5) . . . . ? N1 C4 C5 C6 6.4(7) . . . . ? C3 C4 C5 C6 -179.5(4) . . . . ? N1 C4 C5 C14 -175.3(4) . . . . ? C3 C4 C5 C14 -1.2(6) . . . . ? C4 C5 C6 N2 12.1(7) . . . . ? C14 C5 C6 N2 -166.2(3) . . . . ? C4 C5 C6 C7 -173.7(4) . . . . ? C14 C5 C6 C7 8.0(6) . . . . ? C9 N2 C6 C5 172.5(4) . . . . ? Cu N2 C6 C5 -18.3(5) . . . . ? C9 N2 C6 C7 -2.8(4) . . . . ? Cu N2 C6 C7 166.4(2) . . . . ? C5 C6 C7 C8 -173.7(4) . . . . ? N2 C6 C7 C8 1.2(4) . . . . ? C5 C6 C7 C13 8.9(7) . . . . ? N2 C6 C7 C13 -176.2(4) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C13 C7 C8 C9 178.4(4) . . . . ? C6 N2 C9 C8 3.3(4) . . . . ? Cu N2 C9 C8 -165.4(3) . . . . ? C6 N2 C9 C12 -172.9(4) . . . . ? Cu N2 C9 C12 18.4(6) . . . . ? C7 C8 C9 N2 -2.6(5) . . . . ? C7 C8 C9 C12 173.4(4) . . . . ? C4 C5 C14 C19 -95.5(5) . . . . ? C6 C5 C14 C19 83.1(5) . . . . ? C4 C5 C14 C15 85.2(5) . . . . ? C6 C5 C14 C15 -96.2(5) . . . . ? C19 C14 C15 F1 -179.5(4) . . . . ? C5 C14 C15 F1 -0.2(6) . . . . ? C19 C14 C15 C16 -0.7(7) . . . . ? C5 C14 C15 C16 178.7(4) . . . . ? F1 C15 C16 F2 -0.4(7) . . . . ? C14 C15 C16 F2 -179.3(4) . . . . ? F1 C15 C16 C17 -179.9(4) . . . . ? C14 C15 C16 C17 1.2(8) . . . . ? F2 C16 C17 F3 0.4(8) . . . . ? C15 C16 C17 F3 179.9(4) . . . . ? F2 C16 C17 C18 179.1(5) . . . . ? C15 C16 C17 C18 -1.4(8) . . . . ? F3 C17 C18 F4 -1.5(8) . . . . ? C16 C17 C18 F4 179.8(5) . . . . ? F3 C17 C18 C19 179.8(4) . . . . ? C16 C17 C18 C19 1.0(8) . . . . ? C15 C14 C19 F5 -179.5(4) . . . . ? C5 C14 C19 F5 1.1(7) . . . . ? C15 C14 C19 C18 0.3(7) . . . . ? C5 C14 C19 C18 -179.0(4) . . . . ? F4 C18 C19 F5 0.6(7) . . . . ? C17 C18 C19 F5 179.3(4) . . . . ? F4 C18 C19 C14 -179.3(4) . . . . ? C17 C18 C19 C14 -0.5(8) . . . . ? C26 P1 C20 C25 19.3(4) . . . . ? C32 P1 C20 C25 125.6(4) . . . . ? Cu P1 C20 C25 -109.4(4) . . . . ? C26 P1 C20 C21 -165.2(4) . . . . ? C32 P1 C20 C21 -59.0(4) . . . . ? Cu P1 C20 C21 66.1(4) . . . . ? C25 C20 C21 C22 1.9(7) . . . . ? P1 C20 C21 C22 -173.8(4) . . . . ? C20 C21 C22 C23 -0.9(8) . . . . ? C21 C22 C23 C24 -0.3(9) . . . . ? C22 C23 C24 C25 0.3(9) . . . . ? C21 C20 C25 C24 -1.9(7) . . . . ? P1 C20 C25 C24 173.6(4) . . . . ? C23 C24 C25 C20 0.8(8) . . . . ? C32 P1 C26 C27 -1.9(4) . . . . ? C20 P1 C26 C27 104.2(4) . . . . ? Cu P1 C26 C27 -123.4(4) . . . . ? C32 P1 C26 C31 174.2(3) . . . . ? C20 P1 C26 C31 -79.7(3) . . . . ? Cu P1 C26 C31 52.7(3) . . . . ? C31 C26 C27 C28 -1.0(7) . . . . ? P1 C26 C27 C28 175.1(4) . . . . ? C26 C27 C28 C29 1.4(8) . . . . ? C27 C28 C29 C30 -0.9(9) . . . . ? C28 C29 C30 C31 0.1(9) . . . . ? C29 C30 C31 C26 0.3(8) . . . . ? C27 C26 C31 C30 0.1(6) . . . . ? P1 C26 C31 C30 -176.2(4) . . . . ? C26 P1 C32 C33 79.2(4) . . . . ? C20 P1 C32 C33 -27.1(4) . . . . ? Cu P1 C32 C33 -157.5(3) . . . . ? C26 P1 C32 C37 -100.5(3) . . . . ? C20 P1 C32 C37 153.2(3) . . . . ? Cu P1 C32 C37 22.7(4) . . . . ? C37 C32 C33 C34 1.2(7) . . . . ? P1 C32 C33 C34 -178.6(4) . . . . ? C32 C33 C34 C35 -0.2(8) . . . . ? C33 C34 C35 C36 -0.3(8) . . . . ? C34 C35 C36 C37 -0.1(8) . . . . ? C35 C36 C37 C32 1.1(7) . . . . ? C33 C32 C37 C36 -1.7(6) . . . . ? P1 C32 C37 C36 178.1(3) . . . . ? C50 P2 C38 C43 121.8(4) . . . . ? C44 P2 C38 C43 15.7(4) . . . . ? Cu P2 C38 C43 -113.6(4) . . . . ? C50 P2 C38 C39 -58.7(4) . . . . ? C44 P2 C38 C39 -164.7(3) . . . . ? Cu P2 C38 C39 65.9(4) . . . . ? C43 C38 C39 C40 -1.2(7) . . . . ? P2 C38 C39 C40 179.2(4) . . . . ? C38 C39 C40 C41 0.1(8) . . . . ? C39 C40 C41 C42 0.9(9) . . . . ? C40 C41 C42 C43 -0.7(9) . . . . ? C39 C38 C43 C42 1.4(7) . . . . ? P2 C38 C43 C42 -179.1(4) . . . . ? C41 C42 C43 C38 -0.5(8) . . . . ? C38 P2 C44 C49 105.3(4) . . . . ? C50 P2 C44 C49 2.0(4) . . . . ? Cu P2 C44 C49 -121.9(3) . . . . ? C38 P2 C44 C45 -76.8(3) . . . . ? C50 P2 C44 C45 179.9(3) . . . . ? Cu P2 C44 C45 56.0(3) . . . . ? C49 C44 C45 C46 -1.6(6) . . . . ? P2 C44 C45 C46 -179.6(3) . . . . ? C44 C45 C46 C47 0.7(6) . . . . ? C45 C46 C47 C48 0.8(7) . . . . ? C46 C47 C48 C49 -1.2(7) . . . . ? C47 C48 C49 C44 0.2(6) . . . . ? C45 C44 C49 C48 1.2(6) . . . . ? P2 C44 C49 C48 179.1(3) . . . . ? C38 P2 C50 C51 144.0(3) . . . . ? C44 P2 C50 C51 -110.3(3) . . . . ? Cu P2 C50 C51 14.6(4) . . . . ? C38 P2 C50 C55 -36.3(4) . . . . ? C44 P2 C50 C55 69.5(3) . . . . ? Cu P2 C50 C55 -165.7(3) . . . . ? C55 C50 C51 C52 0.1(6) . . . . ? P2 C50 C51 C52 179.9(3) . . . . ? C50 C51 C52 C53 -0.5(6) . . . . ? C51 C52 C53 C54 0.0(6) . . . . ? C52 C53 C54 C55 0.9(6) . . . . ? C53 C54 C55 C50 -1.2(6) . . . . ? C51 C50 C55 C54 0.7(6) . . . . ? P2 C50 C55 C54 -179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.502 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.064