# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yanxiang Cheng' _publ_contact_author_email YANXIANG@CIAC.JL.CN _publ_section_title ; Neutral Copper(I) Phosphorescent Complexes from Their Ionic Counterparts with 2-(2'-Quinolyl)benzimidazole and Phosphine Mixed Ligands ; loop_ _publ_author_name 'Junhui Min.' 'Qisheng Zhang' 'Wei Sun.' 'Yanxiang Cheng.' 'Lixiang Wang.' data_q022 _database_code_depnum_ccdc_archive 'CCDC 724902' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H42 Cu N3 O2 P2' _chemical_formula_weight 878.38 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 Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 27.5890(7) _cell_length_b 27.5890(7) _cell_length_c 13.7636(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10476.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8702 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details ? _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 31391 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.03 _reflns_number_total 10291 _reflns_number_gt 7986 _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^)+(0.1112P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(17) _refine_ls_number_reflns 10291 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1919 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.67137(2) 0.61895(2) 0.17903(5) 0.03082(18) Uani 1 1 d . . . N1 N 0.67742(18) 0.63857(17) 0.0361(3) 0.0355(11) Uani 1 1 d . . . N2 N 0.72661(16) 0.57161(17) 0.1377(3) 0.0356(11) Uani 1 1 d . . . N3 N 0.7167(2) 0.6202(2) -0.1066(4) 0.0492(14) Uani 1 1 d . . . O1 O 0.66736(14) 0.61081(13) 0.4108(2) 0.0331(8) Uani 1 1 d . . . P1 P 0.60377(5) 0.59055(5) 0.24587(10) 0.0290(3) Uani 1 1 d . . . P2 P 0.71176(5) 0.67775(5) 0.26180(10) 0.0309(3) Uani 1 1 d . . . C1 C 0.6597(2) 0.6706(2) -0.0369(4) 0.0389(14) Uani 1 1 d . . . C2 C 0.6270(3) 0.7082(3) -0.0340(5) 0.0523(17) Uani 1 1 d . . . H2 H 0.6116 0.7170 0.0234 0.052 Uiso 1 1 calc R . . C3 C 0.6182(3) 0.7318(3) -0.1197(5) 0.0540(18) Uani 1 1 d . . . H3 H 0.5960 0.7572 -0.1198 0.054 Uiso 1 1 calc R . . C4 C 0.6403(3) 0.7199(3) -0.2045(5) 0.0572(19) Uani 1 1 d . . . H4 H 0.6324 0.7368 -0.2607 0.057 Uiso 1 1 calc R . . C5 C 0.6744(3) 0.6831(3) -0.2094(5) 0.059(2) Uani 1 1 d . . . H5 H 0.6903 0.6755 -0.2670 0.059 Uiso 1 1 calc R . . C6 C 0.6836(2) 0.6581(3) -0.1238(4) 0.0470(16) Uani 1 1 d . . . C7 C 0.7110(2) 0.6118(2) -0.0100(4) 0.0383(14) Uani 1 1 d . . . C8 C 0.7387(2) 0.5771(2) 0.0442(4) 0.0399(14) Uani 1 1 d . . . C9 C 0.7786(3) 0.5523(3) 0.0019(6) 0.066(2) Uani 1 1 d . . . H9 H 0.7864 0.5568 -0.0632 0.066 Uiso 1 1 calc R . . C10 C 0.8049(3) 0.5219(3) 0.0585(6) 0.069(2) Uani 1 1 d . . . H10 H 0.8306 0.5049 0.0312 0.069 Uiso 1 1 calc R . . C11 C 0.7941(2) 0.5153(3) 0.1577(6) 0.0571(19) Uani 1 1 d . . . C12 C 0.8223(3) 0.4867(3) 0.2219(6) 0.070(2) Uani 1 1 d . . . H12 H 0.8492 0.4703 0.1979 0.070 Uiso 1 1 calc R . . C13 C 0.8112(3) 0.4828(3) 0.3157(8) 0.077(2) Uani 1 1 d . . . H13 H 0.8298 0.4635 0.3565 0.077 Uiso 1 1 calc R . . C14 C 0.7696(3) 0.5091(3) 0.3536(6) 0.061(2) Uani 1 1 d . . . H14 H 0.7618 0.5071 0.4193 0.061 Uiso 1 1 calc R . . C15 C 0.7420(2) 0.5366(2) 0.2931(5) 0.0439(15) Uani 1 1 d . . . H15 H 0.7151 0.5527 0.3174 0.044 Uiso 1 1 calc R . . C16 C 0.7537(2) 0.5408(2) 0.1952(5) 0.0393(14) Uani 1 1 d . . . C17 C 0.6009(2) 0.5257(2) 0.2799(4) 0.0347(13) Uani 1 1 d . . . C18 C 0.5709(2) 0.5093(2) 0.3534(4) 0.0426(14) Uani 1 1 d . . . H18 H 0.5532 0.5311 0.3909 0.043 Uiso 1 1 calc R . . C19 C 0.5674(3) 0.4592(3) 0.3708(5) 0.0588(19) Uani 1 1 d . . . H19 H 0.5484 0.4478 0.4216 0.059 Uiso 1 1 calc R . . C20 C 0.5918(3) 0.4272(2) 0.3136(6) 0.0610(19) Uani 1 1 d . . . H20 H 0.5882 0.3940 0.3230 0.061 Uiso 1 1 calc R . . C21 C 0.6222(3) 0.4446(2) 0.2407(6) 0.0573(18) Uani 1 1 d . . . H21 H 0.6397 0.4229 0.2028 0.057 Uiso 1 1 calc R . . C22 C 0.6266(2) 0.4938(2) 0.2244(5) 0.0415(14) Uani 1 1 d . . . H22 H 0.6469 0.5051 0.1756 0.041 Uiso 1 1 calc R . . C23 C 0.55010(19) 0.59812(18) 0.1683(4) 0.0301(11) Uani 1 1 d . . . C24 C 0.5148(2) 0.5653(3) 0.1577(5) 0.0511(17) Uani 1 1 d . . . H24 H 0.5160 0.5369 0.1940 0.051 Uiso 1 1 calc R . . C25 C 0.4761(3) 0.5726(3) 0.0932(5) 0.0573(19) Uani 1 1 d . . . H25 H 0.4518 0.5494 0.0876 0.057 Uiso 1 1 calc R . . C26 C 0.4740(2) 0.6139(2) 0.0387(5) 0.0467(16) Uani 1 1 d . . . H26 H 0.4481 0.6195 -0.0032 0.047 Uiso 1 1 calc R . . C27 C 0.5106(3) 0.6466(3) 0.0474(7) 0.078(3) Uani 1 1 d . . . H27 H 0.5099 0.6749 0.0106 0.078 Uiso 1 1 calc R . . C28 C 0.5484(3) 0.6384(3) 0.1095(6) 0.066(2) Uani 1 1 d . . . H28 H 0.5737 0.6607 0.1121 0.066 Uiso 1 1 calc R . . C29 C 0.5875(2) 0.6226(2) 0.3579(4) 0.0341(12) Uani 1 1 d . . . C30 C 0.5406(2) 0.6403(2) 0.3766(4) 0.0424(14) Uani 1 1 d . . . H30 H 0.5155 0.6325 0.3345 0.042 Uiso 1 1 calc R . . C31 C 0.5314(3) 0.6689(3) 0.4559(5) 0.0560(18) Uani 1 1 d . . . H31 H 0.5002 0.6805 0.4667 0.056 Uiso 1 1 calc R . . C32 C 0.5682(2) 0.6807(3) 0.5198(5) 0.0492(16) Uani 1 1 d . . . H32 H 0.5619 0.7003 0.5733 0.049 Uiso 1 1 calc R . . C33 C 0.6145(2) 0.6632(2) 0.5040(4) 0.0410(14) Uani 1 1 d . . . H33 H 0.6397 0.6715 0.5457 0.041 Uiso 1 1 calc R . . C34 C 0.6227(2) 0.6335(2) 0.4257(4) 0.0336(13) Uani 1 1 d . . . C35 C 0.7093(2) 0.6343(2) 0.4458(4) 0.0346(13) Uani 1 1 d . . . C36 C 0.7267(2) 0.6213(2) 0.5365(4) 0.0441(15) Uani 1 1 d . . . H36 H 0.7100 0.5992 0.5751 0.044 Uiso 1 1 calc R . . C37 C 0.7696(2) 0.6420(3) 0.5682(5) 0.0508(17) Uani 1 1 d . . . H37 H 0.7820 0.6333 0.6286 0.051 Uiso 1 1 calc R . . C38 C 0.7940(2) 0.6751(2) 0.5124(5) 0.0457(15) Uani 1 1 d . . . H38 H 0.8220 0.6898 0.5356 0.046 Uiso 1 1 calc R . . C39 C 0.7762(2) 0.6862(2) 0.4203(4) 0.0415(14) Uani 1 1 d . . . H39 H 0.7933 0.7079 0.3814 0.042 Uiso 1 1 calc R . . C40 C 0.7341(2) 0.6661(2) 0.3855(4) 0.0317(12) Uani 1 1 d . . . C41 C 0.76687(19) 0.68949(19) 0.1938(4) 0.0313(12) Uani 1 1 d . . . C42 C 0.7679(2) 0.7247(2) 0.1215(4) 0.0413(14) Uani 1 1 d . . . H42 H 0.7419 0.7460 0.1142 0.041 Uiso 1 1 calc R . . C43 C 0.8081(3) 0.7281(3) 0.0597(5) 0.0551(19) Uani 1 1 d . . . H43 H 0.8089 0.7521 0.0122 0.055 Uiso 1 1 calc R . . C44 C 0.8461(3) 0.6968(3) 0.0683(5) 0.059(2) Uani 1 1 d . . . H44 H 0.8722 0.6989 0.0258 0.059 Uiso 1 1 calc R . . C45 C 0.8456(3) 0.6623(3) 0.1399(6) 0.0596(19) Uani 1 1 d . . . H45 H 0.8720 0.6417 0.1474 0.060 Uiso 1 1 calc R . . C46 C 0.8057(2) 0.6580(2) 0.2018(4) 0.0454(15) Uani 1 1 d . . . H46 H 0.8053 0.6338 0.2488 0.045 Uiso 1 1 calc R . . C47 C 0.6813(2) 0.73628(19) 0.2706(4) 0.0340(12) Uani 1 1 d . . . C48 C 0.6335(3) 0.7394(3) 0.2418(7) 0.065(2) Uani 1 1 d . . . H48 H 0.6182 0.7121 0.2165 0.065 Uiso 1 1 calc R . . C49 C 0.6079(3) 0.7821(3) 0.2498(9) 0.088(3) Uani 1 1 d . . . H49 H 0.5751 0.7828 0.2343 0.088 Uiso 1 1 calc R . . C50 C 0.6310(3) 0.8245(3) 0.2812(7) 0.070(2) Uani 1 1 d . . . H50 H 0.6150 0.8541 0.2800 0.070 Uiso 1 1 calc R . . C51 C 0.6783(3) 0.8210(2) 0.3140(5) 0.0518(16) Uani 1 1 d . . . H51 H 0.6930 0.8480 0.3417 0.052 Uiso 1 1 calc R . . C52 C 0.7042(2) 0.7780(2) 0.3062(5) 0.0433(14) Uani 1 1 d . . . H52 H 0.7366 0.7769 0.3246 0.043 Uiso 1 1 calc R . . O2 O 0.7575(3) 0.5675(2) -0.2440(4) 0.095(2) Uani 1 1 d . . . C53 C 0.7281(6) 0.5279(5) -0.2540(9) 0.150(6) Uani 1 1 d . . . H53A H 0.7313 0.5075 -0.1979 0.150 Uiso 1 1 calc R . . H53B H 0.7374 0.5101 -0.3110 0.150 Uiso 1 1 calc R . . H53C H 0.6950 0.5383 -0.2603 0.150 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 0.0312(4) 0.0334(4) 0.0279(3) 0.0003(3) 0.0007(3) -0.0054(3) N1 0.039(3) 0.038(3) 0.028(2) -0.001(2) -0.001(2) -0.006(2) N2 0.032(3) 0.036(3) 0.039(3) -0.007(2) 0.000(2) -0.004(2) N3 0.049(3) 0.062(4) 0.036(3) 0.002(3) 0.005(2) -0.015(3) O1 0.032(2) 0.035(2) 0.0320(19) -0.0017(16) -0.0030(16) -0.0062(17) P1 0.0296(7) 0.0302(7) 0.0273(7) -0.0009(6) -0.0007(6) -0.0039(5) P2 0.0331(8) 0.0323(7) 0.0271(7) 0.0031(6) -0.0025(6) -0.0083(6) C1 0.041(3) 0.045(3) 0.031(3) 0.000(3) -0.003(3) -0.019(3) C2 0.051(4) 0.055(4) 0.051(4) 0.009(3) 0.001(3) -0.003(3) C3 0.054(4) 0.046(4) 0.063(5) 0.013(3) -0.007(4) -0.011(3) C4 0.060(4) 0.070(5) 0.042(4) 0.019(3) -0.013(3) -0.026(4) C5 0.065(5) 0.078(5) 0.035(3) 0.013(3) -0.006(3) -0.031(4) C6 0.048(4) 0.060(4) 0.033(3) 0.003(3) -0.001(3) -0.027(3) C7 0.035(3) 0.050(4) 0.030(3) -0.005(3) 0.002(2) -0.016(3) C8 0.032(3) 0.045(4) 0.043(3) -0.009(3) 0.003(3) -0.006(3) C9 0.047(4) 0.095(6) 0.056(5) -0.022(4) 0.008(3) 0.004(4) C10 0.065(5) 0.072(5) 0.070(5) -0.006(4) 0.012(4) 0.025(4) C11 0.048(4) 0.055(4) 0.067(5) -0.007(4) 0.012(3) 0.009(3) C12 0.062(5) 0.073(5) 0.077(6) 0.002(4) 0.013(4) 0.031(4) C13 0.074(5) 0.059(5) 0.096(7) 0.020(5) -0.011(5) 0.022(4) C14 0.063(5) 0.063(5) 0.058(5) 0.014(4) 0.001(4) -0.007(4) C15 0.043(4) 0.036(3) 0.053(4) 0.006(3) 0.002(3) 0.004(3) C16 0.037(3) 0.032(3) 0.049(4) 0.004(3) -0.001(3) -0.003(2) C17 0.036(3) 0.037(3) 0.031(3) 0.008(2) -0.006(2) -0.005(2) C18 0.051(4) 0.040(3) 0.037(3) 0.009(3) -0.005(3) -0.006(3) C19 0.067(5) 0.063(5) 0.046(4) 0.018(4) 0.000(4) -0.021(4) C20 0.066(5) 0.039(4) 0.078(5) 0.013(4) -0.008(4) -0.002(3) C21 0.056(4) 0.041(4) 0.075(5) -0.006(4) -0.004(4) 0.010(3) C22 0.039(3) 0.040(3) 0.045(3) -0.001(3) 0.005(3) 0.002(3) C23 0.032(3) 0.030(3) 0.028(3) -0.002(2) 0.003(2) -0.003(2) C24 0.046(4) 0.057(4) 0.050(4) 0.011(3) -0.018(3) -0.019(3) C25 0.048(4) 0.076(5) 0.048(4) -0.001(4) -0.003(3) -0.020(4) C26 0.043(4) 0.055(4) 0.042(3) -0.006(3) -0.009(3) 0.007(3) C27 0.098(7) 0.048(4) 0.088(6) 0.017(4) -0.053(5) -0.007(4) C28 0.070(5) 0.054(5) 0.075(5) 0.020(4) -0.036(4) -0.028(4) C29 0.040(3) 0.032(3) 0.030(3) 0.000(2) 0.002(2) -0.008(2) C30 0.038(3) 0.053(4) 0.037(3) -0.008(3) -0.001(3) 0.007(3) C31 0.042(4) 0.069(5) 0.057(4) -0.011(4) 0.004(3) 0.010(3) C32 0.052(4) 0.058(4) 0.037(4) -0.011(3) 0.004(3) 0.010(3) C33 0.045(4) 0.050(4) 0.028(3) -0.007(3) 0.002(3) -0.008(3) C34 0.035(3) 0.035(3) 0.030(3) 0.004(2) 0.005(2) -0.001(2) C35 0.033(3) 0.039(3) 0.032(3) -0.001(2) -0.006(2) 0.001(2) C36 0.050(4) 0.054(4) 0.028(3) 0.005(3) -0.003(3) -0.007(3) C37 0.054(4) 0.069(5) 0.029(3) -0.003(3) -0.012(3) 0.004(3) C38 0.041(4) 0.050(4) 0.047(4) -0.003(3) -0.013(3) -0.005(3) C39 0.036(3) 0.047(4) 0.041(3) -0.003(3) 0.003(3) -0.009(3) C40 0.029(3) 0.035(3) 0.031(3) 0.003(2) -0.006(2) 0.001(2) C41 0.033(3) 0.034(3) 0.027(3) -0.001(2) -0.002(2) -0.012(2) C42 0.049(4) 0.044(4) 0.032(3) 0.000(3) -0.002(3) -0.014(3) C43 0.067(5) 0.064(5) 0.035(4) 0.004(3) -0.002(3) -0.028(4) C44 0.051(4) 0.082(5) 0.044(4) -0.010(4) 0.015(3) -0.026(4) C45 0.045(4) 0.061(5) 0.072(5) -0.015(4) 0.012(4) -0.010(3) C46 0.050(4) 0.046(4) 0.040(4) -0.002(3) 0.004(3) -0.014(3) C47 0.040(3) 0.031(3) 0.031(3) 0.001(2) -0.001(2) -0.008(2) C48 0.050(4) 0.041(4) 0.105(7) -0.003(4) -0.025(4) 0.000(3) C49 0.054(5) 0.057(5) 0.153(9) -0.006(6) -0.032(6) 0.002(4) C50 0.072(5) 0.041(4) 0.096(6) -0.008(4) 0.000(4) 0.007(4) C51 0.067(4) 0.037(3) 0.051(4) -0.002(3) 0.003(4) -0.006(3) C52 0.045(3) 0.039(3) 0.046(4) 0.002(3) -0.003(3) -0.003(3) O2 0.145(6) 0.079(4) 0.061(4) -0.004(3) 0.022(4) -0.007(4) C53 0.221(16) 0.145(12) 0.083(8) -0.027(8) -0.039(10) -0.070(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1 2.048(5) . ? Cu N2 2.086(5) . ? Cu P1 2.2223(15) . ? Cu P2 2.2741(15) . ? N1 C7 1.344(8) . ? N1 C1 1.424(8) . ? N2 C8 1.338(8) . ? N2 C16 1.382(7) . ? N3 C7 1.359(7) . ? N3 C6 1.410(9) . ? O1 C34 1.397(7) . ? O1 C35 1.411(7) . ? P1 C29 1.833(6) . ? P1 C23 1.838(5) . ? P1 C17 1.851(6) . ? P2 C41 1.815(5) . ? P2 C47 1.824(6) . ? P2 C40 1.838(5) . ? C1 C2 1.374(9) . ? C1 C6 1.409(9) . ? C2 C3 1.370(10) . ? C3 C4 1.357(11) . ? C4 C5 1.385(11) . ? C5 C6 1.388(9) . ? C7 C8 1.434(9) . ? C8 C9 1.420(9) . ? C9 C10 1.355(11) . ? C10 C11 1.410(11) . ? C11 C16 1.413(9) . ? C11 C12 1.417(11) . ? C12 C13 1.330(12) . ? C13 C14 1.454(11) . ? C14 C15 1.359(9) . ? C15 C16 1.391(9) . ? C17 C22 1.364(8) . ? C17 C18 1.384(8) . ? C18 C19 1.406(9) . ? C19 C20 1.361(11) . ? C20 C21 1.392(11) . ? C21 C22 1.380(9) . ? C23 C24 1.337(8) . ? C23 C28 1.376(9) . ? C24 C25 1.405(9) . ? C25 C26 1.364(10) . ? C26 C27 1.360(10) . ? C27 C28 1.368(10) . ? C29 C34 1.381(8) . ? C29 C30 1.404(8) . ? C30 C31 1.371(9) . ? C31 C32 1.382(10) . ? C32 C33 1.383(9) . ? C33 C34 1.374(8) . ? C35 C36 1.384(8) . ? C35 C40 1.390(8) . ? C36 C37 1.384(9) . ? C37 C38 1.371(9) . ? C38 C39 1.395(9) . ? C39 C40 1.373(8) . ? C41 C46 1.383(9) . ? C41 C42 1.391(8) . ? C42 C43 1.401(9) . ? C43 C44 1.363(11) . ? C44 C45 1.370(11) . ? C45 C46 1.396(9) . ? C47 C48 1.382(9) . ? C47 C52 1.400(8) . ? C48 C49 1.379(10) . ? C49 C50 1.399(11) . ? C50 C51 1.384(11) . ? C51 C52 1.390(9) . ? O2 C53 1.368(13) . ? 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 81.0(2) . . ? N1 Cu P1 124.01(14) . . ? N2 Cu P1 120.36(14) . . ? N1 Cu P2 104.65(13) . . ? N2 Cu P2 103.02(13) . . ? P1 Cu P2 117.08(6) . . ? C7 N1 C1 104.2(5) . . ? C7 N1 Cu 111.3(4) . . ? C1 N1 Cu 144.5(4) . . ? C8 N2 C16 119.1(5) . . ? C8 N2 Cu 111.9(4) . . ? C16 N2 Cu 128.6(4) . . ? C7 N3 C6 102.5(5) . . ? C34 O1 C35 117.9(4) . . ? C29 P1 C23 103.7(2) . . ? C29 P1 C17 104.1(3) . . ? C23 P1 C17 102.8(2) . . ? C29 P1 Cu 112.58(18) . . ? C23 P1 Cu 113.30(17) . . ? C17 P1 Cu 118.77(19) . . ? C41 P2 C47 105.2(2) . . ? C41 P2 C40 103.2(2) . . ? C47 P2 C40 104.3(3) . . ? C41 P2 Cu 106.22(17) . . ? C47 P2 Cu 116.07(19) . . ? C40 P2 Cu 120.24(19) . . ? C2 C1 C6 121.1(6) . . ? C2 C1 N1 132.3(6) . . ? C6 C1 N1 106.7(6) . . ? C3 C2 C1 116.8(7) . . ? C4 C3 C2 123.0(7) . . ? C3 C4 C5 121.7(7) . . ? C4 C5 C6 116.5(7) . . ? C5 C6 C1 120.9(7) . . ? C5 C6 N3 129.0(7) . . ? C1 C6 N3 110.0(6) . . ? N1 C7 N3 116.6(6) . . ? N1 C7 C8 119.3(5) . . ? N3 C7 C8 124.1(6) . . ? N2 C8 C9 122.2(6) . . ? N2 C8 C7 116.3(5) . . ? C9 C8 C7 121.4(6) . . ? C10 C9 C8 118.5(7) . . ? C9 C10 C11 121.5(7) . . ? C10 C11 C16 117.1(7) . . ? C10 C11 C12 124.0(7) . . ? C16 C11 C12 118.8(7) . . ? C13 C12 C11 121.6(7) . . ? C12 C13 C14 119.3(7) . . ? C15 C14 C13 119.9(7) . . ? C14 C15 C16 120.8(6) . . ? N2 C16 C15 118.8(5) . . ? N2 C16 C11 121.5(6) . . ? C15 C16 C11 119.6(6) . . ? C22 C17 C18 120.6(5) . . ? C22 C17 P1 117.4(4) . . ? C18 C17 P1 121.7(5) . . ? C17 C18 C19 119.1(6) . . ? C20 C19 C18 120.4(7) . . ? C19 C20 C21 119.4(6) . . ? C22 C21 C20 120.6(6) . . ? C17 C22 C21 119.9(6) . . ? C24 C23 C28 117.3(6) . . ? C24 C23 P1 124.9(4) . . ? C28 C23 P1 117.4(4) . . ? C23 C24 C25 121.7(6) . . ? C26 C25 C24 120.0(6) . . ? C27 C26 C25 118.3(6) . . ? C26 C27 C28 120.8(7) . . ? C27 C28 C23 121.7(7) . . ? C34 C29 C30 116.6(5) . . ? C34 C29 P1 120.0(4) . . ? C30 C29 P1 123.2(4) . . ? C31 C30 C29 121.1(6) . . ? C30 C31 C32 120.3(6) . . ? C31 C32 C33 119.8(6) . . ? C34 C33 C32 118.9(6) . . ? C33 C34 C29 123.0(5) . . ? C33 C34 O1 121.8(5) . . ? C29 C34 O1 115.1(5) . . ? C36 C35 C40 122.2(5) . . ? C36 C35 O1 118.3(5) . . ? C40 C35 O1 119.3(5) . . ? C35 C36 C37 118.3(6) . . ? C38 C37 C36 121.2(6) . . ? C37 C38 C39 118.9(6) . . ? C40 C39 C38 121.8(6) . . ? C39 C40 C35 117.6(5) . . ? C39 C40 P2 122.4(4) . . ? C35 C40 P2 119.9(4) . . ? C46 C41 C42 118.7(5) . . ? C46 C41 P2 119.7(4) . . ? C42 C41 P2 120.7(5) . . ? C41 C42 C43 119.7(6) . . ? C44 C43 C42 120.9(7) . . ? C43 C44 C45 119.6(7) . . ? C44 C45 C46 120.4(7) . . ? C41 C46 C45 120.5(6) . . ? C48 C47 C52 118.7(6) . . ? C48 C47 P2 118.4(5) . . ? C52 C47 P2 122.9(5) . . ? C49 C48 C47 121.2(7) . . ? C48 C49 C50 120.4(8) . . ? C51 C50 C49 118.2(7) . . ? C50 C51 C52 121.2(6) . . ? C51 C52 C47 119.9(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.945 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.113 data_q023 _database_code_depnum_ccdc_archive 'CCDC 724903' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 Cu N3 O2 P2' _chemical_formula_weight 896.43 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' 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' O O 0.0106 0.0060 '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 10.6781(5) _cell_length_b 11.5317(5) _cell_length_c 19.6402(8) _cell_angle_alpha 81.2940(10) _cell_angle_beta 79.7000(10) _cell_angle_gamma 77.3000(10) _cell_volume 2305.37(17) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8617 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details ? _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 13135 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.03 _reflns_number_total 8891 _reflns_number_gt 7209 _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^)+(0.0734P)^2^+0.9381P] 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 8891 _refine_ls_number_parameters 561 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.09530(3) 0.07283(3) 0.243762(16) 0.02690(11) Uani 1 1 d . . . N1 N 0.1358(2) 0.0297(2) 0.34733(12) 0.0363(6) Uani 1 1 d . . . N2 N 0.2243(2) 0.1838(2) 0.24069(13) 0.0340(5) Uani 1 1 d . . . N3 N 0.3244(3) 0.2657(2) 0.31009(16) 0.0477(7) Uani 1 1 d . . . P1 P 0.18001(6) -0.08563(6) 0.18315(3) 0.02527(16) Uani 1 1 d . . . P2 P -0.10385(6) 0.19088(6) 0.23600(3) 0.02599(16) Uani 1 1 d . . . C1 C 0.0998(3) -0.0587(3) 0.39715(15) 0.0413(7) Uani 1 1 d . . . C2 C 0.0198(3) -0.1299(3) 0.38333(16) 0.0464(8) Uani 1 1 d . . . H2 H -0.0087 -0.1165 0.3402 0.046 Uiso 1 1 calc R . . C3 C -0.0180(4) -0.2191(3) 0.4315(2) 0.0582(9) Uani 1 1 d . . . H3 H -0.0727 -0.2648 0.4215 0.058 Uiso 1 1 calc R . . C4 C 0.0269(4) -0.2415(4) 0.49725(19) 0.0645(11) Uani 1 1 d . . . H4 H 0.0026 -0.3028 0.5301 0.064 Uiso 1 1 calc R . . C5 C 0.1045(4) -0.1739(4) 0.51189(18) 0.0608(10) Uani 1 1 d . . . H5 H 0.1331 -0.1890 0.5550 0.061 Uiso 1 1 calc R . . C6 C 0.1436(3) -0.0800(3) 0.46271(16) 0.0502(9) Uani 1 1 d . . . C7 C 0.2248(4) -0.0063(4) 0.47536(19) 0.0595(10) Uani 1 1 d . . . H7 H 0.2542 -0.0175 0.5181 0.059 Uiso 1 1 calc R . . C8 C 0.2600(4) 0.0802(4) 0.42582(18) 0.0547(9) Uani 1 1 d . . . H8 H 0.3132 0.1286 0.4344 0.055 Uiso 1 1 calc R . . C9 C 0.2151(3) 0.0969(3) 0.36027(16) 0.0403(7) Uani 1 1 d . . . C10 C 0.2542(3) 0.1840(3) 0.30426(16) 0.0379(7) Uani 1 1 d . . . C11 C 0.3424(3) 0.3226(3) 0.24349(19) 0.0426(8) Uani 1 1 d . . . C12 C 0.4108(3) 0.4142(3) 0.2158(2) 0.0512(9) Uani 1 1 d . . . H12 H 0.4508 0.4479 0.2440 0.051 Uiso 1 1 calc R . . C13 C 0.4170(3) 0.4521(3) 0.1467(2) 0.0553(9) Uani 1 1 d . . . H13 H 0.4635 0.5117 0.1276 0.055 Uiso 1 1 calc R . . C14 C 0.3561(3) 0.4047(3) 0.1035(2) 0.0503(8) Uani 1 1 d . . . H14 H 0.3631 0.4328 0.0563 0.050 Uiso 1 1 calc R . . C15 C 0.2855(3) 0.3168(3) 0.12946(18) 0.0429(7) Uani 1 1 d . . . H15 H 0.2426 0.2871 0.1008 0.043 Uiso 1 1 calc R . . C16 C 0.2802(3) 0.2734(3) 0.20008(17) 0.0365(7) Uani 1 1 d . . . C17 C 0.3321(2) -0.1812(2) 0.20513(14) 0.0276(6) Uani 1 1 d . . . C18 C 0.3365(3) -0.2294(3) 0.27403(16) 0.0401(7) Uani 1 1 d . . . H18 H 0.2642 -0.2103 0.3076 0.040 Uiso 1 1 calc R . . C19 C 0.4476(3) -0.3059(3) 0.29350(18) 0.0486(8) Uani 1 1 d . . . H19 H 0.4488 -0.3385 0.3397 0.049 Uiso 1 1 calc R . . C20 C 0.5561(3) -0.3337(3) 0.24433(18) 0.0418(7) Uani 1 1 d . . . H20 H 0.6306 -0.3848 0.2572 0.042 Uiso 1 1 calc R . . C21 C 0.5527(3) -0.2851(3) 0.17634(17) 0.0399(7) Uani 1 1 d . . . H21 H 0.6260 -0.3028 0.1432 0.040 Uiso 1 1 calc R . . C22 C 0.4421(3) -0.2100(3) 0.15620(16) 0.0348(6) Uani 1 1 d . . . H22 H 0.4412 -0.1786 0.1097 0.035 Uiso 1 1 calc R . . C23 C 0.2217(2) -0.0386(2) 0.09049(14) 0.0284(6) Uani 1 1 d . . . C24 C 0.3043(3) 0.0433(3) 0.07116(15) 0.0340(6) Uani 1 1 d . . . H24 H 0.3388 0.0687 0.1052 0.034 Uiso 1 1 calc R . . C25 C 0.3352(3) 0.0869(3) 0.00236(16) 0.0442(8) Uani 1 1 d . . . H25 H 0.3919 0.1399 -0.0098 0.044 Uiso 1 1 calc R . . C26 C 0.2826(4) 0.0522(3) -0.04839(17) 0.0545(9) Uani 1 1 d . . . H26 H 0.3028 0.0823 -0.0948 0.054 Uiso 1 1 calc R . . C27 C 0.2004(4) -0.0271(4) -0.03031(17) 0.0612(10) Uani 1 1 d . . . H27 H 0.1649 -0.0505 -0.0647 0.061 Uiso 1 1 calc R . . C28 C 0.1694(3) -0.0729(3) 0.03871(16) 0.0456(8) Uani 1 1 d . . . H28 H 0.1135 -0.1266 0.0503 0.046 Uiso 1 1 calc R . . C29 C 0.0795(3) -0.1958(2) 0.18556(13) 0.0276(6) Uani 1 1 d . . . C30 C 0.1311(3) -0.3144(3) 0.17433(16) 0.0376(7) Uani 1 1 d . . . H30 H 0.2206 -0.3407 0.1657 0.038 Uiso 1 1 calc R . . C31 C 0.0496(3) -0.3933(3) 0.17595(17) 0.0423(7) Uani 1 1 d . . . H31 H 0.0847 -0.4724 0.1683 0.042 Uiso 1 1 calc R . . C32 C -0.0819(3) -0.3559(3) 0.18876(17) 0.0423(7) Uani 1 1 d . . . H32 H -0.1360 -0.4095 0.1898 0.042 Uiso 1 1 calc R . . C33 C -0.1348(3) -0.2386(3) 0.20016(18) 0.0442(8) Uani 1 1 d . . . H33 H -0.2244 -0.2131 0.2089 0.044 Uiso 1 1 calc R . . C34 C -0.0540(3) -0.1595(3) 0.19854(16) 0.0346(6) Uani 1 1 d . . . H34 H -0.0899 -0.0807 0.2063 0.035 Uiso 1 1 calc R . . C35 C -0.1566(3) 0.3066(2) 0.29554(14) 0.0297(6) Uani 1 1 d . . . C36 C -0.0647(3) 0.3694(3) 0.30514(15) 0.0370(7) Uani 1 1 d . . . H36 H 0.0207 0.3496 0.2834 0.037 Uiso 1 1 calc R . . C37 C -0.1003(3) 0.4619(3) 0.34728(17) 0.0472(8) Uani 1 1 d . . . H37 H -0.0390 0.5046 0.3527 0.047 Uiso 1 1 calc R . . C38 C -0.2252(4) 0.4902(3) 0.38076(17) 0.0495(8) Uani 1 1 d . . . H38 H -0.2485 0.5517 0.4091 0.049 Uiso 1 1 calc R . . C39 C -0.3168(3) 0.4272(3) 0.37234(16) 0.0458(8) Uani 1 1 d . . . H39 H -0.4014 0.4459 0.3954 0.046 Uiso 1 1 calc R . . C40 C -0.2827(3) 0.3360(3) 0.32959(14) 0.0369(7) Uani 1 1 d . . . H40 H -0.3448 0.2945 0.3238 0.037 Uiso 1 1 calc R . . C41 C -0.2437(3) 0.1180(2) 0.25166(15) 0.0311(6) Uani 1 1 d . . . C42 C -0.3284(3) 0.1278(3) 0.20441(18) 0.0412(7) Uani 1 1 d . . . H42 H -0.3190 0.1772 0.1625 0.041 Uiso 1 1 calc R . . C43 C -0.4287(3) 0.0624(3) 0.2201(2) 0.0564(10) Uani 1 1 d . . . H43 H -0.4855 0.0683 0.1884 0.056 Uiso 1 1 calc R . . C44 C -0.4431(3) -0.0102(3) 0.2821(2) 0.0622(11) Uani 1 1 d . . . H44 H -0.5098 -0.0529 0.2922 0.062 Uiso 1 1 calc R . . C45 C -0.3599(4) -0.0201(3) 0.3291(2) 0.0582(10) Uani 1 1 d . . . H45 H -0.3699 -0.0694 0.3710 0.058 Uiso 1 1 calc R . . C46 C -0.2607(3) 0.0438(3) 0.31396(17) 0.0443(8) Uani 1 1 d . . . H46 H -0.2044 0.0370 0.3461 0.044 Uiso 1 1 calc R . . C47 C -0.1137(3) 0.2789(2) 0.15064(14) 0.0286(6) Uani 1 1 d . . . C48 C -0.0236(3) 0.2422(3) 0.09403(15) 0.0353(6) Uani 1 1 d . . . H48 H 0.0408 0.1744 0.1003 0.035 Uiso 1 1 calc R . . C49 C -0.0281(3) 0.3048(3) 0.02856(16) 0.0448(8) Uani 1 1 d . . . H49 H 0.0322 0.2782 -0.0090 0.045 Uiso 1 1 calc R . . C50 C -0.1211(4) 0.4061(3) 0.01863(17) 0.0498(8) Uani 1 1 d . . . H50 H -0.1234 0.4488 -0.0254 0.050 Uiso 1 1 calc R . . C51 C -0.2116(4) 0.4444(3) 0.07465(17) 0.0537(9) Uani 1 1 d . . . H51 H -0.2751 0.5129 0.0680 0.054 Uiso 1 1 calc R . . C52 C -0.2082(3) 0.3816(3) 0.14047(16) 0.0433(7) Uani 1 1 d . . . H52 H -0.2690 0.4081 0.1779 0.043 Uiso 1 1 calc R . . O1 O 0.3425(3) 0.3977(3) 0.40926(17) 0.0905(10) Uani 1 1 d . . . C53 C 0.2363(4) 0.4941(4) 0.4105(2) 0.0762(12) Uani 1 1 d . . . H53A H 0.1595 0.4668 0.4342 0.076 Uiso 1 1 calc R . . H53B H 0.2244 0.5268 0.3636 0.076 Uiso 1 1 calc R . . H53C H 0.2524 0.5547 0.4345 0.076 Uiso 1 1 calc R . . O2 O 0.3814(4) 0.2617(4) 0.53009(19) 0.1072(12) Uani 1 1 d . . . C54 C 0.5110(6) 0.2368(7) 0.5244(3) 0.145(3) Uani 1 1 d . . . H54A H 0.5422 0.3096 0.5219 0.145 Uiso 1 1 calc R . . H54B H 0.5473 0.1991 0.4830 0.145 Uiso 1 1 calc R . . H54C H 0.5366 0.1838 0.5644 0.145 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 0.02745(19) 0.02725(19) 0.02660(18) -0.00329(13) -0.00578(13) -0.00520(14) N1 0.0353(13) 0.0386(14) 0.0295(13) -0.0044(11) -0.0025(10) 0.0026(11) N2 0.0288(12) 0.0311(13) 0.0439(14) -0.0107(11) -0.0074(10) -0.0038(10) N3 0.0396(15) 0.0428(16) 0.0659(19) -0.0214(14) -0.0140(13) -0.0040(12) P1 0.0234(3) 0.0250(3) 0.0274(3) -0.0035(3) -0.0028(3) -0.0054(3) P2 0.0264(3) 0.0251(3) 0.0263(3) -0.0027(3) -0.0043(3) -0.0045(3) C1 0.0389(17) 0.0467(18) 0.0301(15) -0.0042(13) -0.0010(13) 0.0056(14) C2 0.0493(19) 0.049(2) 0.0297(16) 0.0034(14) 0.0021(14) 0.0021(16) C3 0.058(2) 0.052(2) 0.058(2) -0.0026(18) 0.0012(18) -0.0067(18) C4 0.070(3) 0.060(2) 0.043(2) 0.0187(18) 0.0056(18) 0.002(2) C5 0.060(2) 0.072(3) 0.0362(19) 0.0091(18) -0.0094(17) 0.010(2) C6 0.049(2) 0.059(2) 0.0313(17) -0.0031(15) -0.0049(14) 0.0130(17) C7 0.059(2) 0.076(3) 0.0385(19) -0.0087(18) -0.0167(17) 0.006(2) C8 0.055(2) 0.066(2) 0.047(2) -0.0146(18) -0.0222(17) -0.0021(18) C9 0.0351(16) 0.0469(18) 0.0394(17) -0.0196(14) -0.0128(13) 0.0064(14) C10 0.0301(15) 0.0387(17) 0.0474(18) -0.0162(14) -0.0104(13) -0.0008(13) C11 0.0324(16) 0.0300(16) 0.066(2) -0.0146(15) -0.0087(15) -0.0012(13) C12 0.0359(17) 0.0353(18) 0.088(3) -0.0182(18) -0.0131(17) -0.0096(14) C13 0.0393(19) 0.0359(19) 0.089(3) -0.0006(18) -0.0086(18) -0.0093(15) C14 0.0426(19) 0.0365(18) 0.065(2) 0.0037(16) -0.0024(16) -0.0037(15) C15 0.0378(17) 0.0373(17) 0.053(2) -0.0077(15) -0.0092(14) -0.0036(14) C16 0.0244(14) 0.0267(15) 0.060(2) -0.0132(14) -0.0062(13) -0.0023(12) C17 0.0239(13) 0.0237(13) 0.0366(15) -0.0024(11) -0.0063(11) -0.0069(11) C18 0.0354(16) 0.0425(18) 0.0371(17) -0.0009(13) -0.0012(13) -0.0025(14) C19 0.0476(19) 0.047(2) 0.0466(19) 0.0074(15) -0.0129(15) -0.0036(16) C20 0.0276(15) 0.0327(16) 0.064(2) 0.0020(15) -0.0127(14) -0.0047(13) C21 0.0259(15) 0.0363(17) 0.055(2) -0.0042(14) -0.0010(13) -0.0063(13) C22 0.0291(15) 0.0340(16) 0.0397(16) -0.0018(13) -0.0037(12) -0.0059(12) C23 0.0255(13) 0.0269(14) 0.0306(14) -0.0040(11) -0.0015(11) -0.0020(11) C24 0.0347(15) 0.0326(15) 0.0337(15) -0.0039(12) -0.0018(12) -0.0074(12) C25 0.0397(17) 0.0454(19) 0.0419(18) 0.0037(14) 0.0052(14) -0.0119(15) C26 0.068(2) 0.062(2) 0.0291(17) 0.0046(15) 0.0018(16) -0.0163(19) C27 0.079(3) 0.084(3) 0.0302(17) -0.0065(18) -0.0092(17) -0.035(2) C28 0.052(2) 0.054(2) 0.0359(17) -0.0038(15) -0.0044(14) -0.0253(17) C29 0.0281(14) 0.0282(14) 0.0266(13) -0.0024(11) -0.0033(10) -0.0074(11) C30 0.0277(14) 0.0300(15) 0.0522(19) -0.0083(13) 0.0032(13) -0.0052(12) C31 0.0456(18) 0.0260(15) 0.055(2) -0.0101(14) -0.0014(15) -0.0072(13) C32 0.0415(18) 0.0365(17) 0.054(2) -0.0051(14) -0.0055(14) -0.0204(14) C33 0.0267(15) 0.0420(18) 0.065(2) -0.0094(16) -0.0063(14) -0.0085(13) C34 0.0283(14) 0.0270(15) 0.0493(18) -0.0098(13) -0.0061(12) -0.0031(12) C35 0.0344(15) 0.0250(14) 0.0268(14) -0.0028(11) -0.0052(11) 0.0008(11) C36 0.0390(16) 0.0328(16) 0.0385(16) -0.0083(13) -0.0052(13) -0.0034(13) C37 0.059(2) 0.0375(18) 0.0500(19) -0.0126(15) -0.0148(16) -0.0098(16) C38 0.071(2) 0.0368(18) 0.0378(18) -0.0135(14) -0.0121(16) 0.0037(17) C39 0.0486(19) 0.0401(18) 0.0379(17) -0.0063(14) 0.0009(14) 0.0092(15) C40 0.0383(16) 0.0376(17) 0.0307(15) -0.0029(12) -0.0029(12) -0.0017(13) C41 0.0245(13) 0.0272(14) 0.0407(16) -0.0083(12) -0.0005(11) -0.0036(11) C42 0.0334(16) 0.0360(17) 0.056(2) -0.0123(15) -0.0097(14) -0.0039(13) C43 0.0307(17) 0.053(2) 0.093(3) -0.031(2) -0.0133(17) -0.0061(16) C44 0.039(2) 0.045(2) 0.103(3) -0.025(2) 0.013(2) -0.0179(17) C45 0.052(2) 0.045(2) 0.072(3) -0.0034(18) 0.0137(19) -0.0187(17) C46 0.0416(18) 0.0408(18) 0.0478(19) 0.0033(14) -0.0011(14) -0.0128(15) C47 0.0309(14) 0.0279(14) 0.0289(14) -0.0024(11) -0.0060(11) -0.0091(12) C48 0.0325(15) 0.0353(16) 0.0349(16) -0.0007(12) -0.0047(12) -0.0026(13) C49 0.0479(19) 0.049(2) 0.0329(16) -0.0017(14) 0.0017(14) -0.0088(16) C50 0.065(2) 0.048(2) 0.0329(17) 0.0063(14) -0.0122(15) -0.0086(17) C51 0.066(2) 0.0430(19) 0.0410(19) 0.0022(15) -0.0167(16) 0.0152(17) C52 0.0496(19) 0.0414(18) 0.0320(16) -0.0044(13) -0.0061(13) 0.0056(15) O1 0.103(3) 0.082(2) 0.096(2) -0.0311(19) -0.050(2) 0.0030(19) C53 0.074(3) 0.067(3) 0.085(3) -0.015(2) -0.010(2) -0.007(2) O2 0.098(3) 0.115(3) 0.089(3) -0.011(2) -0.002(2) 0.009(2) C54 0.081(4) 0.215(8) 0.112(5) 0.069(5) -0.017(4) -0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N2 2.064(2) . ? Cu N1 2.118(2) . ? Cu P1 2.2630(7) . ? Cu P2 2.2757(8) . ? N1 C9 1.345(4) . ? N1 C1 1.371(4) . ? N2 C10 1.343(4) . ? N2 C16 1.382(4) . ? N3 C10 1.356(4) . ? N3 C11 1.373(4) . ? P1 C23 1.823(3) . ? P1 C29 1.825(3) . ? P1 C17 1.833(3) . ? P2 C41 1.827(3) . ? P2 C47 1.831(3) . ? P2 C35 1.836(3) . ? C1 C2 1.392(5) . ? C1 C6 1.416(4) . ? C2 C3 1.367(5) . ? C3 C4 1.424(5) . ? C4 C5 1.347(6) . ? C5 C6 1.421(5) . ? C6 C7 1.414(5) . ? C7 C8 1.350(5) . ? C8 C9 1.424(4) . ? C9 C10 1.441(5) . ? C11 C12 1.403(4) . ? C11 C16 1.416(4) . ? C12 C13 1.356(5) . ? C13 C14 1.392(5) . ? C14 C15 1.377(4) . ? C15 C16 1.397(4) . ? C17 C18 1.388(4) . ? C17 C22 1.391(4) . ? C18 C19 1.390(4) . ? C19 C20 1.382(5) . ? C20 C21 1.371(4) . ? C21 C22 1.384(4) . ? C23 C28 1.387(4) . ? C23 C24 1.397(4) . ? C24 C25 1.377(4) . ? C25 C26 1.375(5) . ? C26 C27 1.369(5) . ? C27 C28 1.388(4) . ? C29 C34 1.383(4) . ? C29 C30 1.393(4) . ? C30 C31 1.384(4) . ? C31 C32 1.364(4) . ? C32 C33 1.382(4) . ? C33 C34 1.380(4) . ? C35 C40 1.386(4) . ? C35 C36 1.394(4) . ? C36 C37 1.394(4) . ? C37 C38 1.371(5) . ? C38 C39 1.386(5) . ? C39 C40 1.390(4) . ? C41 C42 1.384(4) . ? C41 C46 1.391(4) . ? C42 C43 1.406(4) . ? C43 C44 1.374(6) . ? C44 C45 1.367(6) . ? C45 C46 1.385(4) . ? C47 C48 1.386(4) . ? C47 C52 1.391(4) . ? C48 C49 1.379(4) . ? C49 C50 1.371(5) . ? C50 C51 1.385(5) . ? C51 C52 1.385(4) . ? O1 C53 1.402(5) . ? O2 C54 1.338(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 80.76(10) . . ? N2 Cu P1 113.16(7) . . ? N1 Cu P1 109.88(7) . . ? N2 Cu P2 107.59(7) . . ? N1 Cu P2 113.21(7) . . ? P1 Cu P2 124.00(3) . . ? C9 N1 C1 119.8(3) . . ? C9 N1 Cu 111.1(2) . . ? C1 N1 Cu 128.9(2) . . ? C10 N2 C16 104.0(2) . . ? C10 N2 Cu 111.2(2) . . ? C16 N2 Cu 143.9(2) . . ? C10 N3 C11 102.8(3) . . ? C23 P1 C29 103.88(12) . . ? C23 P1 C17 102.63(12) . . ? C29 P1 C17 101.65(12) . . ? C23 P1 Cu 111.67(9) . . ? C29 P1 Cu 117.77(9) . . ? C17 P1 Cu 117.29(9) . . ? C41 P2 C47 104.22(13) . . ? C41 P2 C35 101.77(12) . . ? C47 P2 C35 102.30(12) . . ? C41 P2 Cu 117.75(9) . . ? C47 P2 Cu 112.98(9) . . ? C35 P2 Cu 115.89(9) . . ? N1 C1 C2 119.9(3) . . ? N1 C1 C6 121.1(3) . . ? C2 C1 C6 119.0(3) . . ? C3 C2 C1 121.6(3) . . ? C2 C3 C4 119.5(4) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 121.3(4) . . ? C7 C6 C1 117.8(3) . . ? C7 C6 C5 123.6(3) . . ? C1 C6 C5 118.6(4) . . ? C8 C7 C6 120.5(3) . . ? C7 C8 C9 119.6(4) . . ? N1 C9 C8 121.1(3) . . ? N1 C9 C10 116.7(3) . . ? C8 C9 C10 122.1(3) . . ? N2 C10 N3 116.1(3) . . ? N2 C10 C9 119.3(3) . . ? N3 C10 C9 124.5(3) . . ? N3 C11 C12 130.2(3) . . ? N3 C11 C16 109.5(3) . . ? C12 C11 C16 120.3(3) . . ? C13 C12 C11 118.2(3) . . ? C12 C13 C14 122.0(3) . . ? C15 C14 C13 121.1(4) . . ? C14 C15 C16 118.2(3) . . ? N2 C16 C15 132.4(3) . . ? N2 C16 C11 107.5(3) . . ? C15 C16 C11 120.1(3) . . ? C18 C17 C22 118.4(3) . . ? C18 C17 P1 118.1(2) . . ? C22 C17 P1 123.4(2) . . ? C17 C18 C19 120.8(3) . . ? C20 C19 C18 120.2(3) . . ? C21 C20 C19 119.3(3) . . ? C20 C21 C22 121.1(3) . . ? C21 C22 C17 120.3(3) . . ? C28 C23 C24 118.2(3) . . ? C28 C23 P1 123.9(2) . . ? C24 C23 P1 117.7(2) . . ? C25 C24 C23 120.9(3) . . ? C26 C25 C24 120.2(3) . . ? C27 C26 C25 119.7(3) . . ? C26 C27 C28 120.8(3) . . ? C23 C28 C27 120.2(3) . . ? C34 C29 C30 118.5(2) . . ? C34 C29 P1 118.5(2) . . ? C30 C29 P1 123.0(2) . . ? C31 C30 C29 120.3(3) . . ? C32 C31 C30 120.4(3) . . ? C31 C32 C33 120.1(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C29 121.0(3) . . ? C40 C35 C36 119.0(3) . . ? C40 C35 P2 123.4(2) . . ? C36 C35 P2 117.6(2) . . ? C37 C36 C35 120.3(3) . . ? C38 C37 C36 120.3(3) . . ? C37 C38 C39 119.9(3) . . ? C38 C39 C40 120.2(3) . . ? C35 C40 C39 120.4(3) . . ? C42 C41 C46 118.8(3) . . ? C42 C41 P2 124.2(2) . . ? C46 C41 P2 116.9(2) . . ? C41 C42 C43 119.5(3) . . ? C44 C43 C42 120.3(3) . . ? C45 C44 C43 120.5(3) . . ? C44 C45 C46 119.6(4) . . ? C45 C46 C41 121.3(3) . . ? C48 C47 C52 118.7(3) . . ? C48 C47 P2 118.9(2) . . ? C52 C47 P2 122.4(2) . . ? C49 C48 C47 121.0(3) . . ? C50 C49 C48 120.3(3) . . ? C49 C50 C51 119.6(3) . . ? C50 C51 C52 120.5(3) . . ? C51 C52 C47 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.760 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.068 data_q060 _database_code_depnum_ccdc_archive 'CCDC 724904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H46 B Cl4 Cu F4 N3 P2' _chemical_formula_weight 1091.03 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' B B 0.0013 0.0007 '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' 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 10.7530(9) _cell_length_b 14.0616(11) _cell_length_c 17.4536(14) _cell_angle_alpha 103.1480(10) _cell_angle_beta 97.9120(10) _cell_angle_gamma 90.4040(10) _cell_volume 2543.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour plate _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1118 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7282 _exptl_absorpt_correction_T_max 0.9517 _exptl_absorpt_process_details ? _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 14847 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.05 _reflns_number_total 9828 _reflns_number_gt 6448 _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^)+(0.0400P)^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 9828 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.38894(4) 0.21836(3) 0.27757(2) 0.02769(13) Uani 1 1 d . . . P1 P 0.32657(8) 0.23208(6) 0.15143(5) 0.0275(2) Uani 1 1 d . . . P2 P 0.56239(8) 0.14043(6) 0.31573(5) 0.0267(2) Uani 1 1 d . . . N1 N 0.2382(3) 0.1775(2) 0.32831(15) 0.0301(7) Uani 1 1 d . . . N2 N 0.3623(3) 0.35209(19) 0.35920(15) 0.0308(7) Uani 1 1 d . . . N3 N 0.1184(3) 0.2244(2) 0.42548(17) 0.0379(8) Uani 1 1 d . . . C1 C 0.1679(3) 0.0963(3) 0.3339(2) 0.0321(8) Uani 1 1 d . . . C2 C 0.1642(3) -0.0004(3) 0.2918(2) 0.0383(9) Uani 1 1 d . . . H2 H 0.2144 -0.0211 0.2522 0.038 Uiso 1 1 calc R . . C3 C 0.0827(4) -0.0643(3) 0.3113(2) 0.0460(10) Uani 1 1 d . . . H3 H 0.0774 -0.1293 0.2834 0.046 Uiso 1 1 calc R . . C4 C 0.0085(4) -0.0359(3) 0.3706(2) 0.0488(11) Uani 1 1 d . . . H4 H -0.0448 -0.0820 0.3815 0.049 Uiso 1 1 calc R . . C5 C 0.0119(3) 0.0578(3) 0.4132(2) 0.0466(11) Uani 1 1 d . . . H5 H -0.0373 0.0768 0.4535 0.047 Uiso 1 1 calc R . . C6 C 0.0923(3) 0.1250(3) 0.3943(2) 0.0350(9) Uani 1 1 d . . . C7 C 0.2063(3) 0.2516(3) 0.38362(19) 0.0317(8) Uani 1 1 d . . . C8 C 0.2649(3) 0.3488(3) 0.39758(19) 0.0337(9) Uani 1 1 d . . . C9 C 0.2209(4) 0.4317(3) 0.4470(2) 0.0459(10) Uani 1 1 d . . . H9 H 0.1506 0.4266 0.4717 0.046 Uiso 1 1 calc R . . C10 C 0.2833(4) 0.5189(3) 0.4578(2) 0.0494(11) Uani 1 1 d . . . H10 H 0.2551 0.5746 0.4896 0.049 Uiso 1 1 calc R . . C11 C 0.3908(4) 0.5255(3) 0.4210(2) 0.0396(9) Uani 1 1 d . . . C12 C 0.4639(4) 0.6126(3) 0.4320(2) 0.0503(11) Uani 1 1 d . . . H12 H 0.4422 0.6692 0.4659 0.050 Uiso 1 1 calc R . . C13 C 0.5649(4) 0.6152(3) 0.3942(2) 0.0529(11) Uani 1 1 d . . . H13 H 0.6129 0.6729 0.4032 0.053 Uiso 1 1 calc R . . C14 C 0.5979(4) 0.5309(3) 0.3413(2) 0.0464(10) Uani 1 1 d . . . H14 H 0.6663 0.5333 0.3145 0.046 Uiso 1 1 calc R . . C15 C 0.5294(3) 0.4461(3) 0.3297(2) 0.0400(9) Uani 1 1 d . . . H15 H 0.5511 0.3907 0.2944 0.040 Uiso 1 1 calc R . . C16 C 0.4268(3) 0.4405(2) 0.36989(19) 0.0327(8) Uani 1 1 d . . . C17 C 0.2797(3) 0.1136(2) 0.08474(19) 0.0302(8) Uani 1 1 d . . . C18 C 0.1859(3) 0.0592(3) 0.1036(2) 0.0388(9) Uani 1 1 d . . . H18 H 0.1462 0.0855 0.1474 0.039 Uiso 1 1 calc R . . C19 C 0.1498(4) -0.0335(3) 0.0587(2) 0.0527(11) Uani 1 1 d . . . H19 H 0.0859 -0.0688 0.0721 0.053 Uiso 1 1 calc R . . C20 C 0.2088(4) -0.0736(3) -0.0060(3) 0.0589(12) Uani 1 1 d . . . H20 H 0.1850 -0.1360 -0.0362 0.059 Uiso 1 1 calc R . . C21 C 0.3034(4) -0.0206(3) -0.0256(2) 0.0569(12) Uani 1 1 d . . . H21 H 0.3434 -0.0475 -0.0691 0.057 Uiso 1 1 calc R . . C22 C 0.3388(4) 0.0724(3) 0.0192(2) 0.0415(10) Uani 1 1 d . . . H22 H 0.4024 0.1078 0.0056 0.042 Uiso 1 1 calc R . . C23 C 0.4413(3) 0.2845(2) 0.10287(18) 0.0268(8) Uani 1 1 d . . . C24 C 0.5679(3) 0.2797(3) 0.1304(2) 0.0348(9) Uani 1 1 d . . . H24 H 0.5920 0.2491 0.1718 0.035 Uiso 1 1 calc R . . C25 C 0.6580(3) 0.3196(3) 0.0973(2) 0.0428(10) Uani 1 1 d . . . H25 H 0.7424 0.3169 0.1172 0.043 Uiso 1 1 calc R . . C26 C 0.6256(4) 0.3631(3) 0.0359(2) 0.0417(10) Uani 1 1 d . . . H26 H 0.6874 0.3892 0.0133 0.042 Uiso 1 1 calc R . . C27 C 0.4999(4) 0.3684(3) 0.0071(2) 0.0419(10) Uani 1 1 d . . . H27 H 0.4768 0.3983 -0.0348 0.042 Uiso 1 1 calc R . . C28 C 0.4089(3) 0.3290(3) 0.0409(2) 0.0348(9) Uani 1 1 d . . . H28 H 0.3245 0.3327 0.0215 0.035 Uiso 1 1 calc R . . C29 C 0.1877(3) 0.3031(2) 0.13501(19) 0.0295(8) Uani 1 1 d . . . C30 C 0.1721(3) 0.3877(2) 0.1914(2) 0.0349(9) Uani 1 1 d . . . H30 H 0.2309 0.4058 0.2370 0.035 Uiso 1 1 calc R . . C31 C 0.0700(4) 0.4457(3) 0.1807(2) 0.0462(10) Uani 1 1 d . . . H31 H 0.0600 0.5020 0.2190 0.046 Uiso 1 1 calc R . . C32 C -0.0160(4) 0.4190(3) 0.1130(3) 0.0517(11) Uani 1 1 d . . . H32 H -0.0844 0.4575 0.1050 0.052 Uiso 1 1 calc R . . C33 C -0.0013(4) 0.3359(3) 0.0574(3) 0.0541(11) Uani 1 1 d . . . H33 H -0.0592 0.3185 0.0113 0.054 Uiso 1 1 calc R . . C34 C 0.0987(3) 0.2775(3) 0.0689(2) 0.0436(10) Uani 1 1 d . . . H34 H 0.1058 0.2199 0.0314 0.044 Uiso 1 1 calc R . . C35 C 0.5562(3) 0.0097(2) 0.27255(19) 0.0286(8) Uani 1 1 d . . . C36 C 0.6305(4) -0.0544(3) 0.3069(2) 0.0379(9) Uani 1 1 d . . . H36 H 0.6833 -0.0306 0.3544 0.038 Uiso 1 1 calc R . . C37 C 0.6270(4) -0.1526(3) 0.2714(2) 0.0518(11) Uani 1 1 d . . . H37 H 0.6764 -0.1949 0.2953 0.052 Uiso 1 1 calc R . . C38 C 0.5499(4) -0.1882(3) 0.2001(3) 0.0550(12) Uani 1 1 d . . . H38 H 0.5474 -0.2545 0.1760 0.055 Uiso 1 1 calc R . . C39 C 0.4774(4) -0.1260(3) 0.1652(2) 0.0524(11) Uani 1 1 d . . . H39 H 0.4262 -0.1499 0.1170 0.052 Uiso 1 1 calc R . . C40 C 0.4800(3) -0.0274(3) 0.2013(2) 0.0397(9) Uani 1 1 d . . . H40 H 0.4298 0.0143 0.1773 0.040 Uiso 1 1 calc R . . C41 C 0.7141(3) 0.1798(2) 0.29571(19) 0.0293(8) Uani 1 1 d . . . C42 C 0.7816(3) 0.1199(3) 0.2427(2) 0.0389(9) Uani 1 1 d . . . H42 H 0.7533 0.0557 0.2204 0.039 Uiso 1 1 calc R . . C43 C 0.8907(4) 0.1549(4) 0.2228(2) 0.0559(12) Uani 1 1 d . . . H43 H 0.9354 0.1137 0.1878 0.056 Uiso 1 1 calc R . . C44 C 0.9329(4) 0.2488(4) 0.2540(3) 0.0603(13) Uani 1 1 d . . . H44 H 1.0054 0.2720 0.2395 0.060 Uiso 1 1 calc R . . C45 C 0.8681(4) 0.3098(3) 0.3071(3) 0.0589(13) Uani 1 1 d . . . H45 H 0.8973 0.3740 0.3290 0.059 Uiso 1 1 calc R . . C46 C 0.7591(4) 0.2751(3) 0.3277(2) 0.0440(10) Uani 1 1 d . . . H46 H 0.7157 0.3165 0.3635 0.044 Uiso 1 1 calc R . . C47 C 0.5872(3) 0.1445(2) 0.42275(19) 0.0291(8) Uani 1 1 d . . . C48 C 0.4843(3) 0.1235(2) 0.4562(2) 0.0331(9) Uani 1 1 d . . . H48 H 0.4060 0.1106 0.4250 0.033 Uiso 1 1 calc R . . C49 C 0.4961(4) 0.1216(3) 0.5350(2) 0.0405(10) Uani 1 1 d . . . H49 H 0.4259 0.1072 0.5566 0.041 Uiso 1 1 calc R . . C50 C 0.6108(4) 0.1407(3) 0.5823(2) 0.0434(10) Uani 1 1 d . . . H50 H 0.6186 0.1377 0.6354 0.043 Uiso 1 1 calc R . . C51 C 0.7139(4) 0.1643(3) 0.5507(2) 0.0474(10) Uani 1 1 d . . . H51 H 0.7910 0.1794 0.5829 0.047 Uiso 1 1 calc R . . C52 C 0.7035(4) 0.1658(3) 0.4713(2) 0.0411(10) Uani 1 1 d . . . H52 H 0.7738 0.1809 0.4500 0.041 Uiso 1 1 calc R . . B B 1.0257(5) 0.3462(4) 0.6150(3) 0.0546(14) Uani 1 1 d . . . F1 F 1.0764(3) 0.4358(2) 0.6354(2) 0.1271(14) Uani 1 1 d . . . F2 F 1.1181(4) 0.2812(3) 0.62175(19) 0.1179(12) Uani 1 1 d . . . F3 F 0.9738(3) 0.3268(2) 0.53529(14) 0.0883(9) Uani 1 1 d . . . F4 F 0.9368(3) 0.3384(2) 0.66060(15) 0.1042(12) Uani 1 1 d . . . C53 C 0.3067(5) 0.6528(4) 0.2272(3) 0.0770(16) Uani 1 1 d . . . H53A H 0.2569 0.6237 0.2589 0.077 Uiso 1 1 calc R . . H53B H 0.3691 0.6977 0.2633 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.20989(14) 0.71690(12) 0.17031(10) 0.1016(5) Uani 1 1 d . . . Cl2 Cl 0.38276(13) 0.56075(9) 0.16707(8) 0.0762(4) Uani 1 1 d . . . C54 C 0.8775(6) -0.2958(5) 0.1873(4) 0.134(3) Uani 1 1 d . . . H54A H 0.9568 -0.3257 0.1784 0.134 Uiso 1 1 calc R . . H54B H 0.8817 -0.2686 0.2440 0.134 Uiso 1 1 calc R . . Cl3 Cl 0.85852(16) -0.20060(15) 0.13744(9) 0.1215(7) Uani 1 1 d . . . Cl4 Cl 0.75803(14) -0.38551(12) 0.15769(11) 0.1132(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0265(3) 0.0286(2) 0.0276(2) 0.00229(18) 0.00920(18) 0.00350(18) P1 0.0237(5) 0.0317(5) 0.0271(5) 0.0036(4) 0.0088(4) 0.0019(4) P2 0.0260(5) 0.0259(5) 0.0284(5) 0.0040(4) 0.0085(4) 0.0026(4) N1 0.0274(17) 0.0342(17) 0.0299(15) 0.0071(13) 0.0089(13) 0.0061(13) N2 0.0369(18) 0.0268(17) 0.0270(15) 0.0029(13) 0.0040(14) 0.0070(13) N3 0.0323(18) 0.046(2) 0.0413(18) 0.0159(16) 0.0143(15) 0.0103(15) C1 0.021(2) 0.045(2) 0.034(2) 0.0152(18) 0.0059(16) 0.0036(17) C2 0.033(2) 0.043(2) 0.040(2) 0.0108(19) 0.0087(18) 0.0064(18) C3 0.042(3) 0.043(2) 0.053(2) 0.014(2) 0.001(2) -0.0041(19) C4 0.035(2) 0.055(3) 0.064(3) 0.030(2) 0.008(2) -0.001(2) C5 0.030(2) 0.068(3) 0.055(3) 0.035(2) 0.018(2) 0.013(2) C6 0.031(2) 0.044(2) 0.036(2) 0.0173(18) 0.0103(17) 0.0106(17) C7 0.033(2) 0.039(2) 0.0263(18) 0.0087(16) 0.0110(16) 0.0133(17) C8 0.036(2) 0.040(2) 0.0243(18) 0.0040(16) 0.0071(16) 0.0131(17) C9 0.052(3) 0.047(3) 0.041(2) 0.0060(19) 0.019(2) 0.020(2) C10 0.066(3) 0.037(2) 0.041(2) -0.0031(19) 0.013(2) 0.020(2) C11 0.049(3) 0.029(2) 0.035(2) -0.0013(17) 0.0013(19) 0.0095(18) C12 0.065(3) 0.026(2) 0.051(3) -0.0053(19) -0.001(2) 0.015(2) C13 0.058(3) 0.031(2) 0.063(3) 0.007(2) -0.008(2) -0.004(2) C14 0.043(3) 0.042(3) 0.052(2) 0.008(2) 0.005(2) 0.000(2) C15 0.042(2) 0.031(2) 0.041(2) -0.0010(17) 0.0026(19) 0.0041(18) C16 0.038(2) 0.028(2) 0.0282(19) 0.0013(16) -0.0007(17) 0.0072(17) C17 0.028(2) 0.033(2) 0.0283(18) 0.0040(16) 0.0042(16) 0.0035(16) C18 0.034(2) 0.041(2) 0.040(2) 0.0034(18) 0.0064(18) -0.0005(18) C19 0.041(3) 0.053(3) 0.060(3) 0.010(2) 0.000(2) -0.014(2) C20 0.070(3) 0.037(3) 0.057(3) -0.008(2) -0.003(3) -0.007(2) C21 0.065(3) 0.053(3) 0.045(2) -0.008(2) 0.015(2) 0.002(2) C22 0.044(2) 0.041(2) 0.037(2) 0.0015(18) 0.0090(19) -0.0023(18) C23 0.028(2) 0.0259(19) 0.0253(18) 0.0005(15) 0.0087(15) 0.0020(15) C24 0.030(2) 0.045(2) 0.032(2) 0.0116(17) 0.0064(17) 0.0044(17) C25 0.020(2) 0.061(3) 0.049(2) 0.014(2) 0.0067(18) 0.0007(18) C26 0.033(2) 0.052(3) 0.044(2) 0.014(2) 0.0125(19) -0.0087(19) C27 0.048(3) 0.048(3) 0.034(2) 0.0190(18) 0.0067(19) 0.001(2) C28 0.027(2) 0.043(2) 0.035(2) 0.0089(17) 0.0048(16) 0.0007(17) C29 0.023(2) 0.035(2) 0.0331(19) 0.0098(16) 0.0107(16) -0.0006(16) C30 0.031(2) 0.033(2) 0.041(2) 0.0085(17) 0.0071(17) 0.0000(17) C31 0.041(3) 0.035(2) 0.063(3) 0.006(2) 0.018(2) 0.0041(19) C32 0.025(2) 0.051(3) 0.081(3) 0.018(2) 0.008(2) 0.0108(19) C33 0.029(2) 0.062(3) 0.065(3) 0.009(2) -0.007(2) 0.006(2) C34 0.033(2) 0.049(3) 0.043(2) -0.0011(19) 0.0054(19) 0.0077(19) C35 0.0254(19) 0.028(2) 0.0328(19) 0.0034(16) 0.0125(16) 0.0001(15) C36 0.045(2) 0.033(2) 0.037(2) 0.0044(17) 0.0124(18) 0.0046(18) C37 0.069(3) 0.033(2) 0.059(3) 0.013(2) 0.025(3) 0.017(2) C38 0.065(3) 0.028(2) 0.068(3) -0.006(2) 0.025(3) 0.000(2) C39 0.050(3) 0.044(3) 0.053(3) -0.008(2) 0.005(2) -0.005(2) C40 0.032(2) 0.035(2) 0.048(2) 0.0002(18) 0.0042(19) 0.0044(17) C41 0.0240(19) 0.032(2) 0.0332(19) 0.0117(16) 0.0023(16) 0.0027(15) C42 0.028(2) 0.052(3) 0.040(2) 0.0147(19) 0.0083(18) 0.0015(18) C43 0.033(3) 0.088(4) 0.056(3) 0.029(3) 0.019(2) 0.008(2) C44 0.028(2) 0.092(4) 0.075(3) 0.050(3) 0.004(2) -0.008(3) C45 0.044(3) 0.053(3) 0.079(3) 0.032(3) -0.018(3) -0.021(2) C46 0.034(2) 0.040(2) 0.058(3) 0.014(2) 0.001(2) 0.0021(18) C47 0.037(2) 0.0198(18) 0.0297(19) 0.0021(15) 0.0079(17) 0.0064(15) C48 0.036(2) 0.028(2) 0.036(2) 0.0095(16) 0.0049(17) -0.0022(16) C49 0.052(3) 0.034(2) 0.040(2) 0.0105(18) 0.015(2) -0.0019(19) C50 0.062(3) 0.036(2) 0.032(2) 0.0076(18) 0.004(2) 0.005(2) C51 0.042(3) 0.060(3) 0.036(2) 0.009(2) -0.0044(19) 0.011(2) C52 0.034(2) 0.046(2) 0.042(2) 0.0069(19) 0.0082(19) 0.0068(18) B 0.061(4) 0.049(3) 0.049(3) -0.006(3) 0.020(3) -0.005(3) F1 0.110(3) 0.080(2) 0.176(4) -0.011(2) 0.039(3) -0.038(2) F2 0.143(3) 0.124(3) 0.094(2) 0.032(2) 0.028(2) 0.061(2) F3 0.071(2) 0.137(3) 0.0521(16) 0.0005(16) 0.0251(14) 0.0242(18) F4 0.094(2) 0.148(3) 0.0627(17) -0.0075(18) 0.0414(17) -0.041(2) C53 0.083(4) 0.089(4) 0.057(3) 0.008(3) 0.018(3) -0.019(3) Cl1 0.0741(10) 0.1061(12) 0.1299(13) 0.0272(10) 0.0319(10) 0.0182(8) Cl2 0.0817(10) 0.0688(9) 0.0849(9) 0.0228(7) 0.0270(8) -0.0048(7) C54 0.071(4) 0.210(8) 0.136(6) 0.087(6) -0.013(4) -0.011(5) Cl3 0.0967(13) 0.1943(19) 0.0707(9) 0.0215(11) 0.0187(9) -0.0272(12) Cl4 0.0759(11) 0.0978(12) 0.1433(15) -0.0050(11) -0.0086(10) 0.0308(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 2.087(3) . ? Cu N2 2.133(3) . ? Cu P1 2.2633(10) . ? Cu P2 2.2676(10) . ? P1 C17 1.824(3) . ? P1 C23 1.828(3) . ? P1 C29 1.828(4) . ? P2 C41 1.822(3) . ? P2 C35 1.819(3) . ? P2 C47 1.838(3) . ? N1 C7 1.332(4) . ? N1 C1 1.393(4) . ? N2 C8 1.324(4) . ? N2 C16 1.382(4) . ? N3 C7 1.374(4) . ? N3 C6 1.391(4) . ? C1 C2 1.389(5) . ? C1 C6 1.407(4) . ? C2 C3 1.380(5) . ? C3 C4 1.382(5) . ? C4 C5 1.356(5) . ? C5 C6 1.399(5) . ? C7 C8 1.455(5) . ? C8 C9 1.411(5) . ? C9 C10 1.356(5) . ? C10 C11 1.410(5) . ? C11 C12 1.411(5) . ? C11 C16 1.411(5) . ? C12 C13 1.350(5) . ? C13 C14 1.408(5) . ? C14 C15 1.357(5) . ? C15 C16 1.397(5) . ? C17 C18 1.381(4) . ? C17 C22 1.397(5) . ? C18 C19 1.381(5) . ? C19 C20 1.382(6) . ? C20 C21 1.382(6) . ? C21 C22 1.383(5) . ? C23 C28 1.374(5) . ? C23 C24 1.388(5) . ? C24 C25 1.372(4) . ? C25 C26 1.358(5) . ? C26 C27 1.384(5) . ? C27 C28 1.384(5) . ? C29 C34 1.371(5) . ? C29 C30 1.388(4) . ? C30 C31 1.390(5) . ? C31 C32 1.373(5) . ? C32 C33 1.364(5) . ? C33 C34 1.378(5) . ? C35 C40 1.381(5) . ? C35 C36 1.390(5) . ? C36 C37 1.377(5) . ? C37 C38 1.383(6) . ? C38 C39 1.366(6) . ? C39 C40 1.384(5) . ? C41 C46 1.386(5) . ? C41 C42 1.389(5) . ? C42 C43 1.386(5) . ? C43 C44 1.357(6) . ? C44 C45 1.380(6) . ? C45 C46 1.389(5) . ? C47 C48 1.380(4) . ? C47 C52 1.400(5) . ? C48 C49 1.370(5) . ? C49 C50 1.375(5) . ? C50 C51 1.375(5) . ? C51 C52 1.379(5) . ? B F1 1.320(5) . ? B F4 1.345(5) . ? B F2 1.365(6) . ? B F3 1.390(6) . ? C53 Cl1 1.737(5) . ? C53 Cl2 1.755(5) . ? C54 Cl4 1.733(6) . ? C54 Cl3 1.755(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 N1 Cu N2 79.31(11) . . ? N1 Cu P1 111.23(8) . . ? N2 Cu P1 109.97(8) . . ? N1 Cu P2 109.49(8) . . ? N2 Cu P2 113.68(8) . . ? P1 Cu P2 124.24(3) . . ? C17 P1 C23 104.46(14) . . ? C17 P1 C29 102.03(16) . . ? C23 P1 C29 102.94(15) . . ? C17 P1 Cu 111.73(11) . . ? C23 P1 Cu 117.09(11) . . ? C29 P1 Cu 116.80(11) . . ? C41 P2 C35 102.64(15) . . ? C41 P2 C47 104.27(15) . . ? C35 P2 C47 101.94(15) . . ? C41 P2 Cu 118.60(11) . . ? C35 P2 Cu 114.40(12) . . ? C47 P2 Cu 113.06(11) . . ? C7 N1 C1 105.6(3) . . ? C7 N1 Cu 111.0(2) . . ? C1 N1 Cu 142.6(2) . . ? C8 N2 C16 118.5(3) . . ? C8 N2 Cu 113.8(2) . . ? C16 N2 Cu 127.3(2) . . ? C7 N3 C6 106.3(3) . . ? C2 C1 N1 130.9(3) . . ? C2 C1 C6 120.1(3) . . ? N1 C1 C6 109.0(3) . . ? C3 C2 C1 116.9(3) . . ? C2 C3 C4 122.8(4) . . ? C5 C4 C3 121.2(4) . . ? C4 C5 C6 117.5(4) . . ? N3 C6 C5 132.2(3) . . ? N3 C6 C1 106.4(3) . . ? C5 C6 C1 121.4(4) . . ? N1 C7 N3 112.7(3) . . ? N1 C7 C8 121.5(3) . . ? N3 C7 C8 125.8(3) . . ? N2 C8 C9 123.4(3) . . ? N2 C8 C7 113.8(3) . . ? C9 C8 C7 122.8(3) . . ? C10 C9 C8 118.6(4) . . ? C9 C10 C11 120.2(3) . . ? C12 C11 C16 118.2(4) . . ? C12 C11 C10 123.6(3) . . ? C16 C11 C10 118.2(3) . . ? C13 C12 C11 121.2(4) . . ? C12 C13 C14 120.3(4) . . ? C15 C14 C13 119.7(4) . . ? C14 C15 C16 121.2(4) . . ? N2 C16 C15 119.7(3) . . ? N2 C16 C11 121.0(3) . . ? C15 C16 C11 119.3(3) . . ? C18 C17 C22 118.4(3) . . ? C18 C17 P1 117.6(3) . . ? C22 C17 P1 123.8(3) . . ? C17 C18 C19 121.2(4) . . ? C20 C19 C18 119.9(4) . . ? C21 C20 C19 119.8(4) . . ? C20 C21 C22 120.2(4) . . ? C21 C22 C17 120.5(4) . . ? C28 C23 C24 118.2(3) . . ? C28 C23 P1 123.6(3) . . ? C24 C23 P1 118.2(3) . . ? C25 C24 C23 120.7(3) . . ? C26 C25 C24 120.9(4) . . ? C25 C26 C27 119.5(3) . . ? C28 C27 C26 119.7(3) . . ? C23 C28 C27 121.0(3) . . ? C34 C29 C30 118.2(3) . . ? C34 C29 P1 123.1(3) . . ? C30 C29 P1 118.7(3) . . ? C31 C30 C29 121.0(3) . . ? C32 C31 C30 119.3(4) . . ? C33 C32 C31 120.0(4) . . ? C32 C33 C34 120.5(4) . . ? C29 C34 C33 120.9(4) . . ? C40 C35 C36 118.3(3) . . ? C40 C35 P2 119.4(3) . . ? C36 C35 P2 122.2(3) . . ? C37 C36 C35 120.9(4) . . ? C36 C37 C38 119.8(4) . . ? C39 C38 C37 120.0(4) . . ? C38 C39 C40 120.2(4) . . ? C35 C40 C39 120.8(4) . . ? C46 C41 C42 117.9(3) . . ? C46 C41 P2 119.8(3) . . ? C42 C41 P2 122.0(3) . . ? C43 C42 C41 120.8(4) . . ? C44 C43 C42 120.6(4) . . ? C43 C44 C45 119.9(4) . . ? C44 C45 C46 119.8(4) . . ? C41 C46 C45 121.0(4) . . ? C48 C47 C52 118.7(3) . . ? C48 C47 P2 117.3(3) . . ? C52 C47 P2 124.1(3) . . ? C49 C48 C47 120.7(3) . . ? C48 C49 C50 120.6(4) . . ? C49 C50 C51 119.6(3) . . ? C52 C51 C50 120.4(4) . . ? C51 C52 C47 120.0(4) . . ? F1 B F4 109.7(4) . . ? F1 B F2 109.1(5) . . ? F4 B F2 111.9(5) . . ? F1 B F3 108.6(5) . . ? F4 B F3 110.4(4) . . ? F2 B F3 107.0(4) . . ? Cl1 C53 Cl2 111.3(2) . . ? Cl4 C54 Cl3 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.576 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.072 data_q110 _database_code_depnum_ccdc_archive 'CCDC 724905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H47 B Cl1.50 Cu F4 N3 O5 P2' _chemical_formula_weight 1095.42 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' B B 0.0013 0.0007 '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 12.5097(9) _cell_length_b 13.1767(9) _cell_length_c 18.4459(13) _cell_angle_alpha 100.9810(10) _cell_angle_beta 93.1070(10) _cell_angle_gamma 114.8320(10) _cell_volume 2678.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1127 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7589 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details ? _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 15564 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.06 _reflns_number_total 10315 _reflns_number_gt 7122 _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^)+(0.1263P)^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 10315 _refine_ls_number_parameters 655 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2037 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.977 _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 0.21830(4) 0.36848(4) 0.23051(3) 0.03111(17) Uani 1 1 d . . . P1 P 0.32491(9) 0.40010(9) 0.13755(6) 0.0302(2) Uani 1 1 d . . . P2 P 0.17083(8) 0.51634(9) 0.27550(5) 0.0290(2) Uani 1 1 d . . . O1 O 0.4238(2) 0.6199(2) 0.24781(15) 0.0336(6) Uani 1 1 d . . . N1 N 0.0650(3) 0.2268(3) 0.2381(2) 0.0366(8) Uani 1 1 d . . . N2 N -0.0276(3) 0.1317(3) 0.3220(2) 0.0456(9) Uani 1 1 d . . . N3 N 0.2817(3) 0.3282(3) 0.32483(18) 0.0341(8) Uani 1 1 d . . . C1 C -0.0570(4) 0.1748(4) 0.2145(3) 0.0414(10) Uani 1 1 d . . . C2 C -0.1225(4) 0.1761(4) 0.1514(3) 0.0506(12) Uani 1 1 d . . . H2 H -0.0852 0.2134 0.1154 0.051 Uiso 1 1 calc R . . C3 C -0.2450(4) 0.1197(5) 0.1444(3) 0.0627(15) Uani 1 1 d . . . H3 H -0.2911 0.1210 0.1037 0.063 Uiso 1 1 calc R . . C4 C -0.3013(4) 0.0607(5) 0.1972(4) 0.0688(17) Uani 1 1 d . . . H4 H -0.3840 0.0225 0.1899 0.069 Uiso 1 1 calc R . . C5 C -0.2391(4) 0.0573(4) 0.2591(3) 0.0579(14) Uani 1 1 d . . . H5 H -0.2772 0.0183 0.2942 0.058 Uiso 1 1 calc R . . C6 C -0.1158(4) 0.1151(4) 0.2667(3) 0.0449(11) Uani 1 1 d . . . C7 C 0.0788(4) 0.2007(3) 0.3024(2) 0.0380(10) Uani 1 1 d . . . C8 C 0.1946(4) 0.2447(4) 0.3475(2) 0.0378(10) Uani 1 1 d . . . C9 C 0.2129(4) 0.2033(4) 0.4104(3) 0.0496(12) Uani 1 1 d . . . H9 H 0.1498 0.1464 0.4253 0.050 Uiso 1 1 calc R . . C10 C 0.3263(4) 0.2494(4) 0.4488(3) 0.0525(12) Uani 1 1 d . . . H10 H 0.3407 0.2239 0.4903 0.053 Uiso 1 1 calc R . . C11 C 0.4194(4) 0.3339(4) 0.4257(3) 0.0425(10) Uani 1 1 d . . . C12 C 0.5399(4) 0.3851(4) 0.4630(3) 0.0519(12) Uani 1 1 d . . . H12 H 0.5587 0.3602 0.5037 0.052 Uiso 1 1 calc R . . C13 C 0.6257(4) 0.4687(5) 0.4391(3) 0.0522(12) Uani 1 1 d . . . H13 H 0.7039 0.5000 0.4629 0.052 Uiso 1 1 calc R . . C14 C 0.5997(4) 0.5100(4) 0.3790(3) 0.0493(12) Uani 1 1 d . . . H14 H 0.6603 0.5686 0.3637 0.049 Uiso 1 1 calc R . . C15 C 0.4859(4) 0.4646(4) 0.3430(2) 0.0385(10) Uani 1 1 d . . . H15 H 0.4691 0.4938 0.3041 0.038 Uiso 1 1 calc R . . C16 C 0.3950(4) 0.3754(4) 0.3638(2) 0.0340(9) Uani 1 1 d . . . C17 C 0.2658(4) 0.2991(3) 0.0459(2) 0.0341(9) Uani 1 1 d . . . C18 C 0.3347(4) 0.2968(4) -0.0099(3) 0.0467(11) Uani 1 1 d . . . H18 H 0.4147 0.3495 -0.0016 0.047 Uiso 1 1 calc R . . C19 C 0.2869(5) 0.2174(4) -0.0779(3) 0.0579(13) Uani 1 1 d . . . H19 H 0.3345 0.2166 -0.1147 0.058 Uiso 1 1 calc R . . C20 C 0.1682(5) 0.1396(4) -0.0906(3) 0.0573(13) Uani 1 1 d . . . H20 H 0.1353 0.0875 -0.1366 0.057 Uiso 1 1 calc R . . C21 C 0.0983(4) 0.1388(4) -0.0356(3) 0.0561(13) Uani 1 1 d . . . H21 H 0.0188 0.0849 -0.0440 0.056 Uiso 1 1 calc R . . C22 C 0.1465(4) 0.2186(4) 0.0329(3) 0.0454(11) Uani 1 1 d . . . H22 H 0.0990 0.2181 0.0699 0.045 Uiso 1 1 calc R . . C23 C 0.4718(3) 0.4033(4) 0.1538(2) 0.0352(9) Uani 1 1 d . . . C24 C 0.4752(4) 0.3075(5) 0.1720(3) 0.0532(12) Uani 1 1 d . . . H24 H 0.4048 0.2470 0.1768 0.053 Uiso 1 1 calc R . . C25 C 0.5820(5) 0.3002(6) 0.1832(3) 0.0673(16) Uani 1 1 d . . . H25 H 0.5829 0.2345 0.1941 0.067 Uiso 1 1 calc R . . C26 C 0.6853(5) 0.3897(6) 0.1781(3) 0.0709(18) Uani 1 1 d . . . H26 H 0.7570 0.3847 0.1848 0.071 Uiso 1 1 calc R . . C27 C 0.6844(4) 0.4870(6) 0.1630(3) 0.0656(16) Uani 1 1 d . . . H27 H 0.7561 0.5483 0.1611 0.066 Uiso 1 1 calc R . . C28 C 0.5776(4) 0.4961(4) 0.1504(3) 0.0477(12) Uani 1 1 d . . . H28 H 0.5776 0.5625 0.1401 0.048 Uiso 1 1 calc R . . C29 C 0.3546(3) 0.5402(3) 0.1183(2) 0.0323(9) Uani 1 1 d . . . C30 C 0.3297(4) 0.5552(4) 0.0470(2) 0.0408(10) Uani 1 1 d . . . H30 H 0.3030 0.4930 0.0058 0.041 Uiso 1 1 calc R . . C31 C 0.3447(5) 0.6619(5) 0.0377(3) 0.0547(13) Uani 1 1 d . . . H31 H 0.3299 0.6715 -0.0099 0.055 Uiso 1 1 calc R . . C32 C 0.3815(5) 0.7544(4) 0.0986(3) 0.0545(13) Uani 1 1 d . . . H32 H 0.3888 0.8251 0.0918 0.054 Uiso 1 1 calc R . . C33 C 0.4075(4) 0.7428(4) 0.1695(3) 0.0442(11) Uani 1 1 d . . . H33 H 0.4333 0.8052 0.2105 0.044 Uiso 1 1 calc R . . C34 C 0.3940(3) 0.6358(3) 0.1783(2) 0.0322(9) Uani 1 1 d . . . C35 C 0.4060(3) 0.6845(3) 0.3111(2) 0.0331(9) Uani 1 1 d . . . C36 C 0.5041(4) 0.7795(4) 0.3539(2) 0.0403(10) Uani 1 1 d . . . H36 H 0.5796 0.8012 0.3402 0.040 Uiso 1 1 calc R . . C37 C 0.4857(4) 0.8415(4) 0.4184(3) 0.0467(11) Uani 1 1 d . . . H37 H 0.5503 0.9050 0.4483 0.047 Uiso 1 1 calc R . . C38 C 0.3750(4) 0.8109(4) 0.4385(3) 0.0448(11) Uani 1 1 d . . . H38 H 0.3645 0.8548 0.4808 0.045 Uiso 1 1 calc R . . C39 C 0.2782(4) 0.7146(4) 0.3960(2) 0.0376(10) Uani 1 1 d . . . H39 H 0.2030 0.6936 0.4101 0.038 Uiso 1 1 calc R . . C40 C 0.2933(3) 0.6490(3) 0.3318(2) 0.0314(9) Uani 1 1 d . . . C41 C 0.0610(3) 0.4696(3) 0.3373(2) 0.0315(9) Uani 1 1 d . . . C42 C -0.0581(4) 0.4446(4) 0.3168(3) 0.0445(11) Uani 1 1 d . . . H42 H -0.0798 0.4662 0.2753 0.045 Uiso 1 1 calc R . . C43 C -0.1451(4) 0.3874(5) 0.3582(3) 0.0552(13) Uani 1 1 d . . . H43 H -0.2242 0.3710 0.3438 0.055 Uiso 1 1 calc R . . C44 C -0.1154(5) 0.3555(4) 0.4193(3) 0.0562(14) Uani 1 1 d . . . H44 H -0.1739 0.3162 0.4460 0.056 Uiso 1 1 calc R . . C45 C 0.0030(5) 0.3822(4) 0.4413(3) 0.0540(13) Uani 1 1 d . . . H45 H 0.0242 0.3623 0.4837 0.054 Uiso 1 1 calc R . . C46 C 0.0898(4) 0.4384(4) 0.4005(2) 0.0423(10) Uani 1 1 d . . . H46 H 0.1687 0.4554 0.4158 0.042 Uiso 1 1 calc R . . C47 C 0.1015(3) 0.5650(4) 0.2088(2) 0.0353(9) Uani 1 1 d . . . C48 C 0.1019(4) 0.6711(4) 0.2225(3) 0.0514(12) Uani 1 1 d . . . H48 H 0.1433 0.7249 0.2668 0.051 Uiso 1 1 calc R . . C49 C 0.0405(5) 0.6983(6) 0.1704(4) 0.0724(18) Uani 1 1 d . . . H49 H 0.0418 0.7707 0.1793 0.072 Uiso 1 1 calc R . . C50 C -0.0232(5) 0.6166(6) 0.1044(4) 0.0708(18) Uani 1 1 d . . . H50 H -0.0654 0.6346 0.0699 0.071 Uiso 1 1 calc R . . C51 C -0.0242(4) 0.5131(6) 0.0902(3) 0.0657(16) Uani 1 1 d . . . H51 H -0.0671 0.4593 0.0461 0.066 Uiso 1 1 calc R . . C52 C 0.0392(4) 0.4857(5) 0.1416(2) 0.0499(12) Uani 1 1 d . . . H52 H 0.0400 0.4141 0.1310 0.050 Uiso 1 1 calc R . . C53 C 0.9208(7) 0.8192(6) 0.3615(4) 0.092(2) Uani 1 1 d . . . H53A H 0.8936 0.8485 0.4053 0.092 Uiso 1 1 calc R . . H53B H 1.0022 0.8739 0.3612 0.092 Uiso 1 1 calc R . . Cl1 Cl 0.8308(2) 0.8070(2) 0.28127(11) 0.1160(7) Uani 1 1 d . . . Cl2 Cl 0.91757(14) 0.68721(13) 0.36656(10) 0.0781(5) Uani 1 1 d . . . B B 0.8289(5) 0.0421(6) 0.4770(4) 0.0544(15) Uani 1 1 d . . . F1 F 0.7725(3) -0.0753(3) 0.4459(3) 0.1075(14) Uani 1 1 d . . . F2 F 0.7687(4) 0.0864(4) 0.4401(3) 0.1142(16) Uani 1 1 d . . . F3 F 0.8209(4) 0.0501(4) 0.5514(2) 0.1079(14) Uani 1 1 d . . . F4 F 0.9452(2) 0.0792(3) 0.46219(18) 0.0682(9) Uani 1 1 d . . . C54 C 0.2866(11) 0.0082(8) 0.0579(6) 0.138(4) Uani 1 1 d . . . O2 O 0.2108(5) -0.1056(8) 0.0473(3) 0.136(3) Uani 1 1 d . . . O4 O 0.4586(4) 0.0282(4) 0.0245(3) 0.116(2) Uani 1 1 d . . . C55 C 0.2540(13) 0.0039(16) 0.1469(10) 0.119(6) Uiso 0.50 1 d PD . . O3 O 0.3526(10) 0.0223(9) 0.2032(6) 0.106(3) Uiso 0.50 1 d PD . . C56 C 0.3641(9) 0.0017(13) 0.3308(8) 0.117(5) Uiso 0.50 1 d PD . . Cl3 Cl 0.2936(6) 0.0192(6) 0.2565(4) 0.172(2) Uiso 0.50 1 d PD . . Cl4 Cl 0.5091(5) 0.0942(5) 0.3411(3) 0.1468(19) Uiso 0.50 1 d PD . . O5 O 1.0401(19) 0.912(2) 0.3005(13) 0.243(9) Uiso 0.50 1 d P . . 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 0.0266(3) 0.0349(3) 0.0322(3) 0.0115(2) 0.00801(19) 0.0120(2) P1 0.0272(5) 0.0348(6) 0.0299(5) 0.0098(4) 0.0081(4) 0.0135(4) P2 0.0260(5) 0.0345(6) 0.0267(5) 0.0095(4) 0.0055(4) 0.0125(4) O1 0.0317(14) 0.0354(15) 0.0345(16) 0.0105(12) 0.0076(12) 0.0142(12) N1 0.0278(18) 0.0350(19) 0.043(2) 0.0073(16) 0.0091(15) 0.0103(15) N2 0.037(2) 0.035(2) 0.059(3) 0.0114(18) 0.0159(18) 0.0091(16) N3 0.0339(18) 0.0369(19) 0.0349(19) 0.0119(15) 0.0090(14) 0.0168(15) C1 0.031(2) 0.031(2) 0.056(3) 0.004(2) 0.007(2) 0.0107(18) C2 0.036(2) 0.051(3) 0.059(3) 0.012(2) 0.008(2) 0.013(2) C3 0.038(3) 0.059(3) 0.081(4) 0.009(3) -0.007(3) 0.018(2) C4 0.025(2) 0.061(3) 0.100(5) 0.005(3) 0.010(3) 0.005(2) C5 0.034(3) 0.045(3) 0.082(4) 0.013(3) 0.020(3) 0.006(2) C6 0.033(2) 0.037(2) 0.059(3) 0.005(2) 0.015(2) 0.0108(19) C7 0.035(2) 0.029(2) 0.049(3) 0.0118(19) 0.0168(19) 0.0109(18) C8 0.040(2) 0.036(2) 0.043(2) 0.0158(19) 0.0140(19) 0.0179(19) C9 0.049(3) 0.049(3) 0.058(3) 0.030(2) 0.020(2) 0.019(2) C10 0.059(3) 0.057(3) 0.051(3) 0.028(2) 0.010(2) 0.028(3) C11 0.039(2) 0.051(3) 0.044(3) 0.017(2) 0.0119(19) 0.024(2) C12 0.059(3) 0.066(3) 0.041(3) 0.017(2) -0.001(2) 0.038(3) C13 0.038(3) 0.068(3) 0.049(3) 0.012(2) -0.005(2) 0.023(2) C14 0.037(2) 0.060(3) 0.045(3) 0.014(2) 0.007(2) 0.014(2) C15 0.035(2) 0.049(3) 0.034(2) 0.0150(19) 0.0085(18) 0.017(2) C16 0.037(2) 0.039(2) 0.031(2) 0.0072(18) 0.0053(17) 0.0219(18) C17 0.039(2) 0.039(2) 0.027(2) 0.0071(17) 0.0035(17) 0.0197(19) C18 0.039(2) 0.051(3) 0.042(3) 0.005(2) 0.013(2) 0.012(2) C19 0.070(4) 0.058(3) 0.038(3) 0.006(2) 0.018(2) 0.022(3) C20 0.078(4) 0.051(3) 0.034(3) 0.003(2) -0.004(2) 0.025(3) C21 0.040(3) 0.057(3) 0.051(3) 0.001(2) -0.007(2) 0.009(2) C22 0.035(2) 0.054(3) 0.042(3) 0.008(2) 0.0049(19) 0.016(2) C23 0.033(2) 0.049(3) 0.026(2) 0.0044(18) 0.0064(16) 0.0222(19) C24 0.049(3) 0.062(3) 0.055(3) 0.012(2) 0.002(2) 0.032(2) C25 0.074(4) 0.096(4) 0.058(3) 0.015(3) 0.005(3) 0.063(4) C26 0.051(3) 0.122(6) 0.049(3) 0.001(3) -0.006(3) 0.057(4) C27 0.034(3) 0.095(5) 0.053(3) 0.003(3) 0.005(2) 0.021(3) C28 0.028(2) 0.067(3) 0.043(3) 0.008(2) 0.0097(18) 0.017(2) C29 0.027(2) 0.038(2) 0.036(2) 0.0171(18) 0.0129(16) 0.0139(17) C30 0.043(2) 0.045(3) 0.035(2) 0.014(2) 0.0075(19) 0.018(2) C31 0.067(3) 0.065(3) 0.043(3) 0.030(3) 0.011(2) 0.032(3) C32 0.069(3) 0.047(3) 0.059(3) 0.028(3) 0.019(3) 0.028(3) C33 0.051(3) 0.036(2) 0.046(3) 0.010(2) 0.013(2) 0.019(2) C34 0.028(2) 0.035(2) 0.034(2) 0.0140(18) 0.0122(16) 0.0110(17) C35 0.033(2) 0.035(2) 0.035(2) 0.0116(18) 0.0038(17) 0.0165(18) C36 0.034(2) 0.034(2) 0.046(3) 0.0079(19) 0.0053(19) 0.0091(18) C37 0.043(3) 0.035(2) 0.050(3) 0.004(2) -0.003(2) 0.009(2) C38 0.053(3) 0.037(2) 0.038(2) 0.0003(19) 0.004(2) 0.017(2) C39 0.039(2) 0.039(2) 0.037(2) 0.0097(19) 0.0088(18) 0.0182(19) C40 0.033(2) 0.033(2) 0.028(2) 0.0079(16) 0.0038(16) 0.0134(17) C41 0.032(2) 0.032(2) 0.029(2) 0.0071(16) 0.0101(16) 0.0121(17) C42 0.030(2) 0.061(3) 0.041(3) 0.019(2) 0.0086(18) 0.014(2) C43 0.034(2) 0.067(3) 0.048(3) 0.010(3) 0.013(2) 0.008(2) C44 0.061(3) 0.046(3) 0.050(3) 0.013(2) 0.032(3) 0.009(2) C45 0.086(4) 0.052(3) 0.037(3) 0.019(2) 0.027(3) 0.037(3) C46 0.050(3) 0.052(3) 0.034(2) 0.015(2) 0.0105(19) 0.029(2) C47 0.027(2) 0.050(3) 0.033(2) 0.0200(19) 0.0101(16) 0.0158(18) C48 0.047(3) 0.055(3) 0.060(3) 0.025(2) 0.008(2) 0.024(2) C49 0.061(3) 0.081(4) 0.100(5) 0.060(4) 0.018(3) 0.037(3) C50 0.043(3) 0.114(5) 0.075(4) 0.064(4) 0.011(3) 0.034(3) C51 0.045(3) 0.105(5) 0.045(3) 0.031(3) 0.001(2) 0.026(3) C52 0.046(3) 0.068(3) 0.034(2) 0.020(2) 0.003(2) 0.021(2) C53 0.113(6) 0.066(4) 0.091(5) 0.002(4) -0.022(4) 0.046(4) Cl1 0.167(2) 0.1357(18) 0.0751(12) 0.0200(12) -0.0085(12) 0.0995(16) Cl2 0.0755(10) 0.0686(9) 0.0933(12) 0.0273(8) 0.0107(8) 0.0314(8) B 0.049(3) 0.062(4) 0.053(4) 0.022(3) 0.019(3) 0.021(3) F1 0.072(2) 0.077(3) 0.157(4) 0.029(3) 0.026(2) 0.015(2) F2 0.096(3) 0.151(4) 0.171(4) 0.116(4) 0.069(3) 0.086(3) F3 0.092(3) 0.154(4) 0.085(3) 0.046(3) 0.042(2) 0.050(3) F4 0.0410(16) 0.081(2) 0.084(2) 0.0382(18) 0.0242(15) 0.0187(15) C54 0.175(10) 0.084(6) 0.148(9) -0.026(6) -0.033(7) 0.079(6) O2 0.091(4) 0.256(9) 0.102(4) 0.077(5) 0.024(3) 0.100(5) O4 0.094(4) 0.092(4) 0.112(5) 0.058(3) -0.047(3) -0.015(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 N1 2.075(3) . ? Cu N3 2.120(3) . ? Cu P1 2.2239(11) . ? Cu P2 2.2906(11) . ? P1 C23 1.828(4) . ? P1 C17 1.832(4) . ? P1 C29 1.832(4) . ? P2 C41 1.815(4) . ? P2 C47 1.825(4) . ? P2 C40 1.835(4) . ? O1 C35 1.394(5) . ? O1 C34 1.394(5) . ? N1 C7 1.318(5) . ? N1 C1 1.388(5) . ? N2 C7 1.375(5) . ? N2 C6 1.377(6) . ? N3 C8 1.338(5) . ? N3 C16 1.375(5) . ? C1 C2 1.395(7) . ? C1 C6 1.401(6) . ? C2 C3 1.379(6) . ? C3 C4 1.396(8) . ? C4 C5 1.366(8) . ? C5 C6 1.388(6) . ? C7 C8 1.451(6) . ? C8 C9 1.420(6) . ? C9 C10 1.373(7) . ? C10 C11 1.386(6) . ? C11 C16 1.426(6) . ? C11 C12 1.435(6) . ? C12 C13 1.343(7) . ? C13 C14 1.404(7) . ? C14 C15 1.362(6) . ? C15 C16 1.385(6) . ? C17 C18 1.382(6) . ? C17 C22 1.395(6) . ? C18 C19 1.385(6) . ? C19 C20 1.379(7) . ? C20 C21 1.373(7) . ? C21 C22 1.394(6) . ? C23 C24 1.383(6) . ? C23 C28 1.389(6) . ? C24 C25 1.386(7) . ? C25 C26 1.358(8) . ? C26 C27 1.367(9) . ? C27 C28 1.401(7) . ? C29 C34 1.393(6) . ? C29 C30 1.404(6) . ? C30 C31 1.385(6) . ? C31 C32 1.382(7) . ? C32 C33 1.384(7) . ? C33 C34 1.390(6) . ? C35 C36 1.387(5) . ? C35 C40 1.389(5) . ? C36 C37 1.398(6) . ? C37 C38 1.364(6) . ? C38 C39 1.386(6) . ? C39 C40 1.398(6) . ? C41 C46 1.385(6) . ? C41 C42 1.398(6) . ? C42 C43 1.399(6) . ? C43 C44 1.359(7) . ? C44 C45 1.388(8) . ? C45 C46 1.385(6) . ? C47 C48 1.370(6) . ? C47 C52 1.398(6) . ? C48 C49 1.388(7) . ? C49 C50 1.397(9) . ? C50 C51 1.333(9) . ? C51 C52 1.396(7) . ? C53 Cl1 1.749(6) . ? C53 Cl2 1.744(6) . ? B F2 1.354(7) . ? B F3 1.369(7) . ? B F4 1.389(6) . ? B F1 1.386(7) . ? C54 O2 1.364(10) . ? C54 C55 1.72(2) . ? O4 O4 1.712(13) 2_655 ? C55 O3 1.474(9) . ? C55 Cl3 2.006(17) . ? O3 Cl3 1.257(11) . ? C56 Cl4 1.682(9) . ? C56 Cl3 1.695(9) . ? 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 N3 80.62(13) . . ? N1 Cu P1 130.62(10) . . ? N3 Cu P1 119.93(9) . . ? N1 Cu P2 101.47(10) . . ? N3 Cu P2 106.55(10) . . ? P1 Cu P2 112.33(4) . . ? C23 P1 C17 100.49(18) . . ? C23 P1 C29 104.71(19) . . ? C17 P1 C29 104.26(18) . . ? C23 P1 Cu 115.50(13) . . ? C17 P1 Cu 119.17(14) . . ? C29 P1 Cu 111.07(13) . . ? C41 P2 C47 103.69(18) . . ? C41 P2 C40 105.08(18) . . ? C47 P2 C40 104.31(18) . . ? C41 P2 Cu 108.29(13) . . ? C47 P2 Cu 118.08(15) . . ? C40 P2 Cu 116.02(13) . . ? C35 O1 C34 118.1(3) . . ? C7 N1 C1 105.4(3) . . ? C7 N1 Cu 109.0(3) . . ? C1 N1 Cu 140.7(3) . . ? C7 N2 C6 106.6(4) . . ? C8 N3 C16 118.5(3) . . ? C8 N3 Cu 112.0(3) . . ? C16 N3 Cu 129.6(3) . . ? N1 C1 C2 130.4(4) . . ? N1 C1 C6 109.5(4) . . ? C2 C1 C6 120.1(4) . . ? C3 C2 C1 117.2(5) . . ? C2 C3 C4 121.5(5) . . ? C5 C4 C3 122.3(5) . . ? C4 C5 C6 116.3(5) . . ? N2 C6 C5 131.5(5) . . ? N2 C6 C1 105.9(4) . . ? C5 C6 C1 122.6(5) . . ? N1 C7 N2 112.6(4) . . ? N1 C7 C8 122.4(4) . . ? N2 C7 C8 124.9(4) . . ? N3 C8 C9 123.2(4) . . ? N3 C8 C7 114.0(4) . . ? C9 C8 C7 122.7(4) . . ? C10 C9 C8 118.3(4) . . ? C9 C10 C11 120.1(4) . . ? C10 C11 C16 119.3(4) . . ? C10 C11 C12 122.8(4) . . ? C16 C11 C12 117.9(4) . . ? C13 C12 C11 120.0(4) . . ? C12 C13 C14 121.3(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 120.7(4) . . ? N3 C16 C15 119.5(4) . . ? N3 C16 C11 120.6(4) . . ? C15 C16 C11 119.8(4) . . ? C18 C17 C22 118.6(4) . . ? C18 C17 P1 123.1(3) . . ? C22 C17 P1 118.3(3) . . ? C19 C18 C17 121.2(4) . . ? C20 C19 C18 119.7(5) . . ? C21 C20 C19 120.3(5) . . ? C20 C21 C22 120.0(4) . . ? C17 C22 C21 120.2(4) . . ? C24 C23 C28 119.5(4) . . ? C24 C23 P1 116.7(3) . . ? C28 C23 P1 123.8(4) . . ? C25 C24 C23 121.0(5) . . ? C26 C25 C24 119.5(6) . . ? C25 C26 C27 120.4(5) . . ? C26 C27 C28 121.3(5) . . ? C23 C28 C27 118.2(5) . . ? C34 C29 C30 117.6(4) . . ? C34 C29 P1 118.6(3) . . ? C30 C29 P1 123.5(3) . . ? C31 C30 C29 120.4(4) . . ? C32 C31 C30 120.5(4) . . ? C31 C32 C33 120.6(4) . . ? C34 C33 C32 118.5(4) . . ? C33 C34 C29 122.3(4) . . ? C33 C34 O1 121.2(4) . . ? C29 C34 O1 116.5(3) . . ? C36 C35 C40 121.8(4) . . ? C36 C35 O1 118.4(4) . . ? C40 C35 O1 119.7(3) . . ? C35 C36 C37 117.8(4) . . ? C38 C37 C36 121.4(4) . . ? C37 C38 C39 120.2(4) . . ? C38 C39 C40 120.2(4) . . ? C35 C40 C39 118.5(4) . . ? C35 C40 P2 118.9(3) . . ? C39 C40 P2 122.6(3) . . ? C46 C41 C42 117.9(4) . . ? C46 C41 P2 119.4(3) . . ? C42 C41 P2 121.7(3) . . ? C41 C42 C43 120.4(4) . . ? C44 C43 C42 120.8(5) . . ? C43 C44 C45 119.4(4) . . ? C46 C45 C44 120.3(5) . . ? C45 C46 C41 121.2(4) . . ? C48 C47 C52 119.0(4) . . ? C48 C47 P2 124.0(3) . . ? C52 C47 P2 117.0(3) . . ? C47 C48 C49 120.1(5) . . ? C48 C49 C50 119.7(6) . . ? C51 C50 C49 120.8(5) . . ? C50 C51 C52 119.9(5) . . ? C47 C52 C51 120.4(5) . . ? Cl1 C53 Cl2 111.6(4) . . ? F2 B F3 116.4(5) . . ? F2 B F4 111.6(5) . . ? F3 B F4 113.1(5) . . ? F2 B F1 104.9(5) . . ? F3 B F1 103.7(5) . . ? F4 B F1 105.9(5) . . ? O2 C54 C55 79.7(10) . . ? O3 C55 C54 116.0(13) . . ? O3 C55 Cl3 38.7(6) . . ? C54 C55 Cl3 154.5(10) . . ? Cl3 O3 C55 94.2(11) . . ? Cl4 C56 Cl3 107.3(7) . . ? O3 Cl3 C56 109.5(9) . . ? O3 Cl3 C55 47.1(6) . . ? C56 Cl3 C55 153.3(9) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.546 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.100