Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Fu Fu' _publ_contact_author_address ; Organometallic Photochemistry Technical Institute of Physica and Chemistry, Chginese Academy of Sciences zhong guan cun bei 1 tiao 2, CAS Beijing China 100080 COLUMBIA ; _publ_contact_author_email 'WF FU@YAHOO.COM.CN' _publ_section_title ; Synthesis, Structures and Photophysical Properties of Luminescent Copper(I) and Platinum(II) Complexes with a Flexible Naphthyridine-Phosphine Ligand ; _publ_author_name 'Fu Fu' data_060410d _database_code_depnum_ccdc_archive 'CCDC 666202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 B2 Cu2 F8 N6 P2' _chemical_formula_weight 1015.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.790(2) _cell_length_b 16.382(2) _cell_length_c 15.468(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.821(3) _cell_angle_gamma 90.00 _cell_volume 4466.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2340 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 20.0 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8023 _exptl_absorpt_correction_T_max 0.8796 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11353 _diffrn_reflns_av_R_equivalents 0.1425 _diffrn_reflns_av_sigmaI/netI 0.2023 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3924 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction Bruker _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^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3924 _refine_ls_number_parameters 352 _refine_ls_number_restraints 166 _refine_ls_R_factor_all 0.2169 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2603 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _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 0.41991(7) 0.56883(7) 0.71487(8) 0.0583(5) Uani 1 1 d . . . P1 P 0.35011(16) 0.67518(17) 0.73221(18) 0.0564(8) Uani 1 1 d D . . N1 N 0.5519(4) 0.4704(5) 0.8431(5) 0.048(2) Uani 1 1 d . . . N2 N 0.4396(4) 0.5372(5) 0.8602(5) 0.049(2) Uani 1 1 d . . . N3 N 0.3334(5) 0.6074(6) 0.8901(5) 0.060(2) Uani 1 1 d . . . H3 H 0.2881 0.5940 0.8601 0.072 Uiso 1 1 d R B . B1 B 0.8442(7) 0.6213(7) 0.5114(8) 0.072(4) Uani 1 1 d D . . F1 F 0.8060(5) 0.5534(5) 0.5294(7) 0.094(4) Uani 0.753(17) 1 d PDU A 1 F2 F 0.7985(6) 0.6845(6) 0.5361(9) 0.131(5) Uani 0.753(17) 1 d PDU A 1 F3 F 0.8481(7) 0.6278(8) 0.4268(6) 0.143(6) Uani 0.753(17) 1 d PDU A 1 F4 F 0.9105(6) 0.6263(8) 0.5622(9) 0.142(5) Uani 0.753(17) 1 d PDU A 1 F1' F 0.9108(13) 0.6645(17) 0.524(2) 0.097(13) Uani 0.247(17) 1 d PDU A 2 F2' F 0.857(2) 0.5561(19) 0.463(3) 0.18(2) Uani 0.247(17) 1 d PDU A 2 F3' F 0.824(2) 0.601(3) 0.5855(19) 0.26(3) Uani 0.247(17) 1 d PDU A 2 F4' F 0.7931(18) 0.670(2) 0.463(3) 0.19(2) Uani 0.247(17) 1 d PDU A 2 C1 C 0.4834(6) 0.4689(6) 0.8755(5) 0.043(2) Uani 1 1 d . B . C2 C 0.3750(6) 0.5382(7) 0.8954(6) 0.052(3) Uani 1 1 d . B . C3 C 0.3487(6) 0.4691(8) 0.9405(7) 0.071(3) Uani 1 1 d . . . H3A H 0.3024 0.4710 0.9621 0.085 Uiso 1 1 calc R B . C4 C 0.3916(7) 0.4026(8) 0.9507(8) 0.078(4) Uani 1 1 d . B . H4 H 0.3740 0.3575 0.9784 0.094 Uiso 1 1 calc R . . C5 C 0.4637(7) 0.3983(7) 0.9205(7) 0.068(3) Uani 1 1 d . . . C6 C 0.5132(8) 0.3327(7) 0.9304(7) 0.076(4) Uani 1 1 d . B . H6 H 0.5005 0.2857 0.9590 0.091 Uiso 1 1 calc R . . C7 C 0.5798(8) 0.3371(7) 0.8987(8) 0.077(4) Uani 1 1 d . . . H7 H 0.6135 0.2935 0.9063 0.093 Uiso 1 1 calc R B . C8 C 0.5980(7) 0.4054(7) 0.8552(7) 0.061(3) Uani 1 1 d . B . C9 C 0.6715(7) 0.4142(7) 0.8172(8) 0.087(4) Uani 1 1 d . . . H9A H 0.6732 0.4669 0.7904 0.131 Uiso 1 1 calc R B . H9B H 0.6744 0.3725 0.7742 0.131 Uiso 1 1 calc R . . H9C H 0.7135 0.4088 0.8628 0.131 Uiso 1 1 calc R . . C10 C 0.3556(6) 0.6821(6) 0.8520(6) 0.057(3) Uani 1 1 d . B . H10A H 0.4072 0.6955 0.8768 0.068 Uiso 1 1 calc R . . H10B H 0.3229 0.7260 0.8666 0.068 Uiso 1 1 calc R . . C11 C 0.2491(3) 0.6622(6) 0.6976(6) 0.050(9) Uani 0.59(3) 1 d PGDU B 1 C12 C 0.2253(5) 0.6175(12) 0.6225(12) 0.080(8) Uani 0.59(3) 1 d PGDU B 1 H12A H 0.2609 0.5946 0.5909 0.096 Uiso 0.59(3) 1 calc PR B 1 C13 C 0.1483(6) 0.6071(11) 0.5945(14) 0.101(9) Uani 0.59(3) 1 d PGU B 1 H13A H 0.1324 0.5772 0.5442 0.121 Uiso 0.59(3) 1 calc PR B 1 C14 C 0.0950(4) 0.6414(7) 0.6416(11) 0.103(10) Uani 0.59(3) 1 d PGU B 1 H14A H 0.0435 0.6344 0.6229 0.123 Uiso 0.59(3) 1 calc PR B 1 C15 C 0.1188(4) 0.6861(12) 0.7168(7) 0.118(11) Uani 0.59(3) 1 d PGU B 1 H15A H 0.0832 0.7090 0.7483 0.142 Uiso 0.59(3) 1 calc PR B 1 C16 C 0.1958(4) 0.6965(10) 0.7448(5) 0.079(8) Uani 0.59(3) 1 d PGDU B 1 H16A H 0.2117 0.7264 0.7951 0.094 Uiso 0.59(3) 1 calc PR B 1 C11' C 0.2518(3) 0.6705(7) 0.6869(6) 0.071(17) Uani 0.41(3) 1 d PGDU B 2 C12' C 0.2338(5) 0.6583(16) 0.5975(6) 0.096(12) Uani 0.41(3) 1 d PGDU B 2 H12B H 0.2719 0.6586 0.5619 0.115 Uiso 0.41(3) 1 calc PR B 2 C13' C 0.1588(6) 0.6457(17) 0.5613(8) 0.111(14) Uani 0.41(3) 1 d PGU B 2 H13B H 0.1468 0.6376 0.5016 0.133 Uiso 0.41(3) 1 calc PR B 2 C14' C 0.1018(4) 0.6452(8) 0.6145(10) 0.089(13) Uani 0.41(3) 1 d PGU B 2 H14B H 0.0517 0.6367 0.5903 0.107 Uiso 0.41(3) 1 calc PR B 2 C15' C 0.1198(4) 0.6573(10) 0.7039(9) 0.083(11) Uani 0.41(3) 1 d PGU B 2 H15B H 0.0817 0.6570 0.7395 0.100 Uiso 0.41(3) 1 calc PR B 2 C16' C 0.1948(4) 0.6700(10) 0.7401(5) 0.058(9) Uani 0.41(3) 1 d PGDU B 2 H16B H 0.2068 0.6781 0.7998 0.069 Uiso 0.41(3) 1 calc PR B 2 C17 C 0.3807(6) 0.7729(7) 0.6992(6) 0.061(3) Uani 1 1 d . B . C18 C 0.3466(7) 0.8459(8) 0.7202(9) 0.088(4) Uani 1 1 d . . . H18 H 0.3056 0.8439 0.7516 0.106 Uiso 1 1 calc R B . C19 C 0.3714(9) 0.9185(8) 0.6961(10) 0.101(5) Uani 1 1 d . B . H19 H 0.3482 0.9661 0.7119 0.121 Uiso 1 1 calc R . . C20 C 0.4307(10) 0.9233(10) 0.6486(9) 0.100(5) Uani 1 1 d . . . H20 H 0.4464 0.9737 0.6300 0.119 Uiso 1 1 calc R B . C21 C 0.4664(8) 0.8541(10) 0.6286(8) 0.096(4) Uani 1 1 d . B . H21 H 0.5084 0.8574 0.5989 0.115 Uiso 1 1 calc R . . C22 C 0.4410(7) 0.7788(8) 0.6520(7) 0.076(3) Uani 1 1 d . . . H22 H 0.4647 0.7317 0.6359 0.091 Uiso 1 1 calc R B . 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 0.0477(9) 0.0643(9) 0.0658(9) 0.0005(7) 0.0186(6) 0.0093(7) P1 0.0477(19) 0.0705(19) 0.0527(17) 0.0022(15) 0.0128(14) 0.0157(15) N1 0.033(5) 0.068(5) 0.043(5) -0.002(4) 0.005(4) 0.006(4) N2 0.035(5) 0.055(5) 0.059(5) 0.008(4) 0.014(4) 0.005(4) N3 0.045(6) 0.089(7) 0.047(5) -0.002(5) 0.009(4) 0.007(5) B1 0.083(12) 0.077(10) 0.061(10) 0.009(8) 0.028(8) 0.009(9) F1 0.085(7) 0.079(6) 0.123(8) 0.021(5) 0.035(5) -0.022(5) F2 0.122(8) 0.115(7) 0.162(9) -0.024(6) 0.045(6) 0.016(6) F3 0.152(9) 0.183(10) 0.103(8) 0.031(6) 0.051(6) -0.007(7) F4 0.113(8) 0.146(9) 0.158(9) 0.032(7) -0.020(7) -0.026(7) F1' 0.086(15) 0.092(15) 0.112(15) -0.002(9) 0.014(9) -0.019(9) F2' 0.20(2) 0.17(2) 0.19(2) -0.014(10) 0.030(11) 0.010(10) F3' 0.26(3) 0.26(3) 0.26(3) 0.009(10) 0.042(11) 0.000(10) F4' 0.19(2) 0.19(2) 0.19(2) -0.002(10) 0.019(11) 0.010(10) C1 0.051(7) 0.052(6) 0.027(5) 0.007(5) 0.008(5) 0.001(5) C2 0.041(7) 0.079(7) 0.039(6) 0.005(5) 0.009(5) 0.000(6) C3 0.047(8) 0.093(9) 0.077(8) 0.022(7) 0.029(6) -0.003(7) C4 0.071(9) 0.090(9) 0.076(9) 0.033(7) 0.021(7) -0.011(8) C5 0.083(10) 0.071(7) 0.051(7) 0.011(6) 0.015(6) -0.009(7) C6 0.086(10) 0.073(8) 0.067(8) 0.021(6) 0.005(7) 0.020(8) C7 0.085(11) 0.063(8) 0.083(9) 0.012(7) 0.009(8) 0.029(7) C8 0.073(9) 0.061(7) 0.046(6) 0.004(5) -0.002(6) 0.024(6) C9 0.067(9) 0.107(10) 0.092(9) 0.021(7) 0.027(7) 0.041(7) C10 0.049(7) 0.066(7) 0.057(7) -0.003(6) 0.011(5) 0.002(6) C11 0.044(12) 0.057(12) 0.046(11) -0.006(7) -0.001(7) 0.017(7) C12 0.076(11) 0.083(11) 0.078(11) -0.003(9) 0.005(8) 0.020(8) C13 0.103(12) 0.095(12) 0.099(12) -0.014(9) -0.005(9) -0.006(9) C14 0.097(13) 0.112(13) 0.099(12) -0.003(9) 0.012(9) 0.003(9) C15 0.113(14) 0.117(13) 0.124(13) -0.013(9) 0.010(9) 0.005(9) C16 0.066(11) 0.085(10) 0.084(11) -0.015(8) 0.006(8) 0.002(8) C11' 0.068(19) 0.076(19) 0.067(19) -0.002(9) 0.007(10) 0.004(10) C12' 0.097(15) 0.102(15) 0.087(14) -0.004(10) 0.006(9) 0.006(9) C13' 0.106(16) 0.116(16) 0.107(16) 0.002(10) -0.001(10) -0.003(10) C14' 0.080(15) 0.098(16) 0.087(14) -0.002(9) 0.008(10) -0.002(10) C15' 0.074(14) 0.088(14) 0.086(14) -0.007(9) 0.005(9) -0.006(9) C16' 0.046(12) 0.064(12) 0.061(12) -0.005(8) 0.002(9) -0.011(8) C17 0.051(7) 0.084(8) 0.052(7) 0.007(6) 0.014(5) 0.026(6) C18 0.069(10) 0.081(9) 0.119(12) 0.005(9) 0.027(8) 0.005(8) C19 0.107(13) 0.075(10) 0.125(13) 0.013(9) 0.029(10) 0.010(9) C20 0.103(13) 0.107(12) 0.085(10) 0.047(9) 0.000(9) -0.018(10) C21 0.097(12) 0.122(12) 0.075(10) 0.037(9) 0.032(8) 0.013(10) C22 0.058(8) 0.099(9) 0.074(8) 0.009(7) 0.020(7) 0.014(7) _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 1.944(8) 2_656 ? Cu1 P1 2.177(3) . ? Cu1 N2 2.287(8) . ? Cu1 Cu1 2.908(3) 2_656 ? P1 C17 1.788(11) . ? P1 C11' 1.795(5) . ? P1 C11 1.817(5) . ? P1 C10 1.846(10) . ? N1 C8 1.342(11) . ? N1 C1 1.380(11) . ? N1 Cu1 1.943(8) 2_656 ? N2 C2 1.338(11) . ? N2 C1 1.365(11) . ? N3 C2 1.350(12) . ? N3 C10 1.437(12) . ? N3 H3 0.9001 . ? B1 F3' 1.293(19) . ? B1 F3 1.325(12) . ? B1 F4 1.328(14) . ? B1 F2' 1.348(18) . ? B1 F4' 1.350(19) . ? B1 F1 1.352(12) . ? B1 F1' 1.371(18) . ? B1 F2 1.401(12) . ? C1 C5 1.419(13) . ? C2 C3 1.442(13) . ? C3 C4 1.326(14) . ? C3 H3A 0.9300 . ? C4 C5 1.426(15) . ? C4 H4 0.9300 . ? C5 C6 1.385(14) . ? C6 C7 1.344(15) . ? C6 H6 0.9300 . ? C7 C8 1.367(14) . ? C7 H7 0.9300 . ? C8 C9 1.511(14) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C11' C12' 1.3900 . ? C11' C16' 1.3900 . ? C12' C13' 1.3900 . ? C12' H12B 0.9300 . ? C13' C14' 1.3900 . ? C13' H13B 0.9300 . ? C14' C15' 1.3900 . ? C14' H14B 0.9300 . ? C15' C16' 1.3900 . ? C15' H15B 0.9300 . ? C16' H16B 0.9300 . ? C17 C22 1.380(13) . ? C17 C18 1.399(14) . ? C18 C19 1.340(16) . ? C18 H18 0.9300 . ? C19 C20 1.367(19) . ? C19 H19 0.9300 . ? C20 C21 1.356(18) . ? C20 H20 0.9300 . ? C21 C22 1.378(17) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? 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 P1 155.2(3) 2_656 . ? N1 Cu1 N2 104.6(3) 2_656 . ? P1 Cu1 N2 94.2(2) . . ? N1 Cu1 Cu1 82.6(2) 2_656 2_656 ? P1 Cu1 Cu1 120.01(9) . 2_656 ? N2 Cu1 Cu1 67.7(2) . 2_656 ? C17 P1 C11' 104.2(5) . . ? C17 P1 C11 110.4(5) . . ? C11' P1 C11 7.1 . . ? C17 P1 C10 104.8(5) . . ? C11' P1 C10 108.1(4) . . ? C11 P1 C10 102.6(4) . . ? C17 P1 Cu1 118.7(3) . . ? C11' P1 Cu1 117.3(3) . . ? C11 P1 Cu1 115.3(3) . . ? C10 P1 Cu1 102.7(3) . . ? C8 N1 C1 119.3(9) . . ? C8 N1 Cu1 122.1(7) . 2_656 ? C1 N1 Cu1 118.6(6) . 2_656 ? C2 N2 C1 116.2(8) . . ? C2 N2 Cu1 111.8(6) . . ? C1 N2 Cu1 111.3(5) . . ? C2 N3 C10 124.1(8) . . ? C2 N3 H3 105.7 . . ? C10 N3 H3 105.9 . . ? F3' B1 F3 162.9(19) . . ? F3' B1 F4 79.9(18) . . ? F3 B1 F4 114.7(10) . . ? F3' B1 F2' 112.5(15) . . ? F3 B1 F2' 58.2(18) . . ? F4 B1 F2' 99.9(18) . . ? F3' B1 F4' 113.0(15) . . ? F3 B1 F4' 62.0(19) . . ? F4 B1 F4' 140.0(17) . . ? F2' B1 F4' 108.3(14) . . ? F3' B1 F1 53(2) . . ? F3 B1 F1 111.4(10) . . ? F4 B1 F1 111.1(10) . . ? F2' B1 F1 66.1(18) . . ? F4' B1 F1 106.0(18) . . ? F3' B1 F1' 110.3(15) . . ? F3 B1 F1' 86.6(15) . . ? F4 B1 F1' 37.1(13) . . ? F2' B1 F1' 106.1(13) . . ? F4' B1 F1' 106.2(13) . . ? F1 B1 F1' 147.6(17) . . ? F3' B1 F2 73(2) . . ? F3 B1 F2 108.7(10) . . ? F4 B1 F2 107.1(10) . . ? F2' B1 F2 153.0(17) . . ? F4' B1 F2 49.0(19) . . ? F1 B1 F2 103.0(9) . . ? F1' B1 F2 95.8(14) . . ? N2 C1 N1 115.7(8) . . ? N2 C1 C5 125.5(9) . . ? N1 C1 C5 118.8(9) . . ? N2 C2 N3 118.7(9) . . ? N2 C2 C3 122.7(10) . . ? N3 C2 C3 118.6(9) . . ? C4 C3 C2 118.9(10) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 122.1(10) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C1 119.5(11) . . ? C6 C5 C4 126.2(11) . . ? C1 C5 C4 114.4(11) . . ? C7 C6 C5 119.7(11) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.2(11) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? N1 C8 C7 122.5(10) . . ? N1 C8 C9 114.5(9) . . ? C7 C8 C9 123.1(10) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 P1 112.3(7) . . ? N3 C10 H10A 109.2 . . ? P1 C10 H10A 109.2 . . ? N3 C10 H10B 109.2 . . ? P1 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 119.0(4) . . ? C16 C11 P1 121.0(4) . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C12' C11' C16' 120.0 . . ? C12' C11' P1 118.3(4) . . ? C16' C11' P1 121.3(5) . . ? C11' C12' C13' 120.0 . . ? C11' C12' H12B 120.0 . . ? C13' C12' H12B 120.0 . . ? C14' C13' C12' 120.0 . . ? C14' C13' H13B 120.0 . . ? C12' C13' H13B 120.0 . . ? C15' C14' C13' 120.0 . . ? C15' C14' H14B 120.0 . . ? C13' C14' H14B 120.0 . . ? C14' C15' C16' 120.0 . . ? C14' C15' H15B 120.0 . . ? C16' C15' H15B 120.0 . . ? C15' C16' C11' 120.0 . . ? C15' C16' H16B 120.0 . . ? C11' C16' H16B 120.0 . . ? C22 C17 C18 117.1(11) . . ? C22 C17 P1 120.2(9) . . ? C18 C17 P1 122.7(8) . . ? C19 C18 C17 121.6(12) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 120.5(13) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 119.6(13) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.5(12) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 120.5(12) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.697 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.097 # Attachment 'complex 2.cif' data_60530c _database_code_depnum_ccdc_archive 'CCDC 666203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H70 B2 Cu2 F8 N6 P4' _chemical_formula_weight 1540.00 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' _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 13.046(2) _cell_length_b 13.073(2) _cell_length_c 22.398(4) _cell_angle_alpha 88.669(3) _cell_angle_beta 88.968(4) _cell_angle_gamma 74.638(3) _cell_volume 3682.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2922 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 22.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.750139 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 18971 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.1324 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 25.02 _reflns_number_total 12951 _reflns_number_gt 6272 _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 12951 _refine_ls_number_parameters 921 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.003 _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 0.73623(5) 0.62001(5) 0.81526(3) 0.0435(2) Uani 1 1 d . . . Cu2 Cu 0.70952(5) 0.92488(5) 0.65699(3) 0.0435(2) Uani 1 1 d . . . P1 P 0.63952(11) 0.57256(11) 0.89253(6) 0.0386(4) Uani 1 1 d . . . P2 P 0.64109(10) 1.00163(11) 0.74153(6) 0.0359(4) Uani 1 1 d . . . P4 P 0.88956(10) 0.66171(11) 0.82255(6) 0.0391(4) Uani 1 1 d . . . P3 P 0.82500(11) 0.96627(11) 0.58834(6) 0.0388(4) Uani 1 1 d . . . N1 N 0.6905(3) 0.5342(3) 0.74245(17) 0.0388(11) Uani 1 1 d . . . N2 N 0.6016(3) 0.7055(3) 0.75694(16) 0.0334(10) Uani 1 1 d . . . N3 N 0.5106(3) 0.8790(3) 0.77647(18) 0.0437(12) Uani 1 1 d . . . H3 H 0.4489 0.9231 0.7800 0.052 Uiso 1 1 calc R . . N4 N 0.6412(3) 0.8194(3) 0.61746(17) 0.0406(11) Uani 1 1 d . . . N5 N 0.7963(3) 0.7278(3) 0.66032(17) 0.0383(11) Uani 1 1 d . . . N6 N 0.9530(3) 0.6369(4) 0.70529(19) 0.0528(13) Uani 1 1 d . . . H6 H 1.0104 0.5864 0.7021 0.063 Uiso 1 1 calc R . . C1 C 0.7980(5) 0.3522(5) 0.7359(3) 0.077(2) Uani 1 1 d . . . H1A H 0.8533 0.3551 0.7076 0.115 Uiso 1 1 calc R . . H1B H 0.7833 0.2842 0.7344 0.115 Uiso 1 1 calc R . . H1C H 0.8206 0.3628 0.7753 0.115 Uiso 1 1 calc R . . C2 C 0.6996(5) 0.4375(5) 0.7211(2) 0.0523(16) Uani 1 1 d . . . C3 C 0.6164(5) 0.4179(5) 0.6873(2) 0.0600(17) Uani 1 1 d . . . H3A H 0.6236 0.3504 0.6725 0.072 Uiso 1 1 calc R . . C4 C 0.5270(5) 0.4948(5) 0.6760(2) 0.0601(17) Uani 1 1 d . . . H4 H 0.4729 0.4806 0.6539 0.072 Uiso 1 1 calc R . . C5 C 0.5167(4) 0.5962(4) 0.6981(2) 0.0409(14) Uani 1 1 d . . . C6 C 0.4246(5) 0.6831(5) 0.6941(2) 0.0567(17) Uani 1 1 d . . . H6A H 0.3658 0.6766 0.6732 0.068 Uiso 1 1 calc R . . C7 C 0.4227(4) 0.7748(5) 0.7208(2) 0.0520(16) Uani 1 1 d . . . H7 H 0.3620 0.8313 0.7193 0.062 Uiso 1 1 calc R . . C8 C 0.5148(4) 0.7846(4) 0.7516(2) 0.0377(13) Uani 1 1 d . . . C9 C 0.6014(4) 0.6116(4) 0.7305(2) 0.0329(12) Uani 1 1 d . . . C10 C 0.6005(4) 0.9124(4) 0.7976(2) 0.0399(14) Uani 1 1 d . . . H10A H 0.6595 0.8507 0.8050 0.048 Uiso 1 1 calc R . . H10B H 0.5816 0.9493 0.8350 0.048 Uiso 1 1 calc R . . C11 C 0.5190(4) 1.1056(4) 0.7315(2) 0.0410(14) Uani 1 1 d . . . C12 C 0.4374(4) 1.1291(4) 0.7736(3) 0.0517(16) Uani 1 1 d . . . H12 H 0.4456 1.0929 0.8102 0.062 Uiso 1 1 calc R . . C13 C 0.3428(5) 1.2066(5) 0.7619(3) 0.071(2) Uani 1 1 d . . . H13 H 0.2882 1.2203 0.7903 0.086 Uiso 1 1 calc R . . C14 C 0.3303(6) 1.2619(5) 0.7092(4) 0.087(3) Uani 1 1 d . . . H14 H 0.2673 1.3133 0.7013 0.104 Uiso 1 1 calc R . . C15 C 0.4109(6) 1.2414(5) 0.6679(3) 0.083(2) Uani 1 1 d . . . H15 H 0.4038 1.2816 0.6326 0.100 Uiso 1 1 calc R . . C16 C 0.5029(5) 1.1617(5) 0.6777(3) 0.0578(17) Uani 1 1 d . . . H16 H 0.5548 1.1455 0.6478 0.069 Uiso 1 1 calc R . . C17 C 0.7259(4) 1.0610(4) 0.7849(2) 0.0335(13) Uani 1 1 d . . . C18 C 0.6898(4) 1.1255(4) 0.8329(2) 0.0531(16) Uani 1 1 d . . . H18 H 0.6181 1.1422 0.8436 0.064 Uiso 1 1 calc R . . C19 C 0.7592(5) 1.1654(5) 0.8653(3) 0.068(2) Uani 1 1 d . . . H19 H 0.7343 1.2082 0.8978 0.082 Uiso 1 1 calc R . . C20 C 0.8649(5) 1.1422(5) 0.8495(3) 0.0652(19) Uani 1 1 d . . . H20 H 0.9113 1.1688 0.8717 0.078 Uiso 1 1 calc R . . C21 C 0.9028(4) 1.0803(5) 0.8013(2) 0.0554(16) Uani 1 1 d . . . H21 H 0.9741 1.0655 0.7901 0.066 Uiso 1 1 calc R . . C22 C 0.8329(4) 1.0406(4) 0.7699(2) 0.0442(14) Uani 1 1 d . . . H22 H 0.8584 0.9983 0.7372 0.053 Uiso 1 1 calc R . . C23 C 0.4753(4) 0.9303(5) 0.5815(3) 0.079(2) Uani 1 1 d . . . H23A H 0.4534 0.9495 0.6218 0.118 Uiso 1 1 calc R . . H23B H 0.4154 0.9227 0.5595 0.118 Uiso 1 1 calc R . . H23C H 0.5027 0.9847 0.5630 0.118 Uiso 1 1 calc R . . C24 C 0.5598(4) 0.8276(5) 0.5820(2) 0.0537(16) Uani 1 1 d . . . C25 C 0.5525(5) 0.7443(6) 0.5448(3) 0.071(2) Uani 1 1 d . . . H25 H 0.4942 0.7511 0.5203 0.085 Uiso 1 1 calc R . . C26 C 0.6342(6) 0.6527(6) 0.5459(3) 0.074(2) Uani 1 1 d . . . H26 H 0.6320 0.5979 0.5206 0.088 Uiso 1 1 calc R . . C27 C 0.7206(5) 0.6402(5) 0.5841(2) 0.0514(16) Uani 1 1 d . . . C28 C 0.8120(5) 0.5527(5) 0.5871(3) 0.0613(18) Uani 1 1 d . . . H28 H 0.8181 0.4947 0.5628 0.074 Uiso 1 1 calc R . . C29 C 0.8891(5) 0.5541(4) 0.6252(3) 0.0576(17) Uani 1 1 d . . . H29 H 0.9505 0.4983 0.6265 0.069 Uiso 1 1 calc R . . C30 C 0.8766(4) 0.6423(4) 0.6642(2) 0.0405(14) Uani 1 1 d . . . C31 C 0.7194(4) 0.7261(4) 0.6205(2) 0.0378(13) Uani 1 1 d . . . C32 C 0.9456(4) 0.7094(4) 0.7541(2) 0.0471(15) Uani 1 1 d . . . H32A H 0.9008 0.7786 0.7424 0.057 Uiso 1 1 calc R . . H32B H 1.0157 0.7173 0.7625 0.057 Uiso 1 1 calc R . . C33 C 0.9933(4) 0.5452(4) 0.8454(2) 0.0413(14) Uani 1 1 d . . . C34 C 1.0067(4) 0.4529(5) 0.8142(3) 0.0597(17) Uani 1 1 d . . . H34 H 0.9687 0.4536 0.7794 0.072 Uiso 1 1 calc R . . C35 C 1.0763(5) 0.3581(5) 0.8341(3) 0.078(2) Uani 1 1 d . . . H35 H 1.0854 0.2972 0.8118 0.094 Uiso 1 1 calc R . . C36 C 1.1314(5) 0.3538(6) 0.8861(3) 0.085(2) Uani 1 1 d . . . H36 H 1.1760 0.2902 0.9000 0.102 Uiso 1 1 calc R . . C37 C 1.1192(5) 0.4445(6) 0.9167(3) 0.088(2) Uani 1 1 d . . . H37 H 1.1569 0.4430 0.9517 0.106 Uiso 1 1 calc R . . C38 C 1.0513(4) 0.5401(5) 0.8969(3) 0.0649(19) Uani 1 1 d . . . H38 H 1.0451 0.6012 0.9187 0.078 Uiso 1 1 calc R . . C39 C 0.8937(4) 0.7624(4) 0.8766(2) 0.0430(14) Uani 1 1 d . . . C40 C 0.9664(4) 0.8230(5) 0.8754(3) 0.0567(16) Uani 1 1 d . . . H40 H 1.0174 0.8136 0.8450 0.068 Uiso 1 1 calc R . . C41 C 0.9637(5) 0.8976(5) 0.9190(3) 0.071(2) Uani 1 1 d . . . H41 H 1.0134 0.9372 0.9179 0.085 Uiso 1 1 calc R . . C42 C 0.8893(6) 0.9128(6) 0.9631(3) 0.083(2) Uani 1 1 d . . . H42 H 0.8877 0.9634 0.9919 0.099 Uiso 1 1 calc R . . C43 C 0.8171(6) 0.8549(6) 0.9655(3) 0.094(3) Uani 1 1 d . . . H43 H 0.7663 0.8649 0.9960 0.113 Uiso 1 1 calc R . . C44 C 0.8201(5) 0.7808(5) 0.9220(3) 0.0697(19) Uani 1 1 d . . . H44 H 0.7699 0.7418 0.9237 0.084 Uiso 1 1 calc R . . C45 C 0.5212(4) 0.5391(4) 0.8648(2) 0.0413(14) Uani 1 1 d . . . C46 C 0.4222(5) 0.6119(5) 0.8615(2) 0.0594(17) Uani 1 1 d . . . H46 H 0.4122 0.6795 0.8767 0.071 Uiso 1 1 calc R . . C47 C 0.3385(5) 0.5835(6) 0.8355(3) 0.082(2) Uani 1 1 d . . . H47 H 0.2716 0.6315 0.8345 0.098 Uiso 1 1 calc R . . C48 C 0.3530(6) 0.4855(7) 0.8113(3) 0.079(2) Uani 1 1 d . . . H48 H 0.2966 0.4673 0.7935 0.095 Uiso 1 1 calc R . . C49 C 0.4511(6) 0.4142(6) 0.8133(3) 0.070(2) Uani 1 1 d . . . H49 H 0.4615 0.3476 0.7968 0.084 Uiso 1 1 calc R . . C50 C 0.5336(5) 0.4412(5) 0.8397(2) 0.0524(16) Uani 1 1 d . . . H50 H 0.5999 0.3922 0.8408 0.063 Uiso 1 1 calc R . . C51 C 0.5905(4) 0.6756(4) 0.9480(2) 0.0394(13) Uani 1 1 d . . . C52 C 0.6095(4) 0.6570(5) 1.0094(2) 0.0478(15) Uani 1 1 d . . . H52 H 0.6446 0.5897 1.0236 0.057 Uiso 1 1 calc R . . C53 C 0.5752(5) 0.7403(5) 1.0483(3) 0.0622(18) Uani 1 1 d . . . H53 H 0.5893 0.7286 1.0889 0.075 Uiso 1 1 calc R . . C54 C 0.5216(5) 0.8385(5) 1.0286(3) 0.073(2) Uani 1 1 d . . . H54 H 0.4993 0.8934 1.0555 0.088 Uiso 1 1 calc R . . C55 C 0.5004(5) 0.8565(5) 0.9691(3) 0.0656(18) Uani 1 1 d . . . H55 H 0.4620 0.9233 0.9557 0.079 Uiso 1 1 calc R . . C56 C 0.5356(4) 0.7768(5) 0.9294(3) 0.0528(16) Uani 1 1 d . . . H56 H 0.5223 0.7907 0.8889 0.063 Uiso 1 1 calc R . . C57 C 0.7062(4) 0.4568(4) 0.9365(2) 0.0401(14) Uani 1 1 d . . . C58 C 0.8162(4) 0.4231(5) 0.9360(2) 0.0503(15) Uani 1 1 d . . . H58 H 0.8553 0.4592 0.9125 0.060 Uiso 1 1 calc R . . C59 C 0.8688(5) 0.3352(5) 0.9704(3) 0.0596(17) Uani 1 1 d . . . H59 H 0.9427 0.3145 0.9705 0.072 Uiso 1 1 calc R . . C60 C 0.8130(5) 0.2791(5) 1.0040(3) 0.0630(18) Uani 1 1 d . . . H60 H 0.8488 0.2203 1.0266 0.076 Uiso 1 1 calc R . . C61 C 0.7030(5) 0.3104(5) 1.0043(2) 0.0564(16) Uani 1 1 d . . . H61 H 0.6646 0.2725 1.0270 0.068 Uiso 1 1 calc R . . C62 C 0.6505(4) 0.3976(5) 0.9709(2) 0.0509(15) Uani 1 1 d . . . H62 H 0.5766 0.4178 0.9711 0.061 Uiso 1 1 calc R . . C63 C 0.7797(4) 1.0910(4) 0.5470(2) 0.0385(13) Uani 1 1 d . . . C64 C 0.7309(4) 1.1814(5) 0.5775(2) 0.0567(16) Uani 1 1 d . . . H64 H 0.7188 1.1764 0.6184 0.068 Uiso 1 1 calc R . . C65 C 0.6991(5) 1.2803(5) 0.5489(3) 0.0721(19) Uani 1 1 d . . . H65 H 0.6671 1.3403 0.5706 0.087 Uiso 1 1 calc R . . C66 C 0.7150(4) 1.2890(5) 0.4891(3) 0.0608(17) Uani 1 1 d . . . H66 H 0.6927 1.3547 0.4698 0.073 Uiso 1 1 calc R . . C67 C 0.7638(4) 1.2009(5) 0.4573(3) 0.0587(17) Uani 1 1 d . . . H67 H 0.7747 1.2069 0.4164 0.070 Uiso 1 1 calc R . . C68 C 0.7974(4) 1.1020(5) 0.4860(2) 0.0500(15) Uani 1 1 d . . . H68 H 0.8320 1.0429 0.4642 0.060 Uiso 1 1 calc R . . C69 C 0.8578(4) 0.8652(4) 0.5309(2) 0.0388(13) Uani 1 1 d . . . C70 C 0.9532(5) 0.7918(5) 0.5257(2) 0.0561(17) Uani 1 1 d . . . H70 H 1.0092 0.7960 0.5497 0.067 Uiso 1 1 calc R . . C71 C 0.9679(6) 0.7113(5) 0.4852(3) 0.081(2) Uani 1 1 d . . . H71 H 1.0341 0.6626 0.4820 0.097 Uiso 1 1 calc R . . C72 C 0.8880(7) 0.7017(6) 0.4500(3) 0.083(2) Uani 1 1 d . . . H72 H 0.8985 0.6458 0.4237 0.099 Uiso 1 1 calc R . . C73 C 0.7905(6) 0.7758(6) 0.4535(3) 0.075(2) Uani 1 1 d . . . H73 H 0.7357 0.7722 0.4284 0.090 Uiso 1 1 calc R . . C74 C 0.7753(4) 0.8557(5) 0.4951(2) 0.0573(17) Uani 1 1 d . . . H74 H 0.7088 0.9035 0.4989 0.069 Uiso 1 1 calc R . . C75 C 0.9514(4) 0.9748(5) 0.6201(2) 0.0407(14) Uani 1 1 d . . . C76 C 0.9850(4) 1.0663(5) 0.6179(2) 0.0537(16) Uani 1 1 d . . . H76 H 0.9482 1.1239 0.5947 0.064 Uiso 1 1 calc R . . C77 C 1.0731(5) 1.0739(5) 0.6496(3) 0.0648(18) Uani 1 1 d . . . H77 H 1.0944 1.1364 0.6479 0.078 Uiso 1 1 calc R . . C78 C 1.1290(5) 0.9888(6) 0.6837(3) 0.071(2) Uani 1 1 d . . . H78 H 1.1871 0.9945 0.7055 0.085 Uiso 1 1 calc R . . C79 C 1.0989(4) 0.8955(6) 0.6854(2) 0.0635(18) Uani 1 1 d . . . H79 H 1.1377 0.8374 0.7074 0.076 Uiso 1 1 calc R . . C80 C 1.0108(4) 0.8888(5) 0.6543(2) 0.0504(15) Uani 1 1 d . . . H80 H 0.9902 0.8259 0.6561 0.061 Uiso 1 1 calc R . . B1 B 0.1951(5) 0.5381(5) 0.6281(3) 0.065(2) Uani 1 1 d D . . B2 B 0.2463(7) 0.9935(8) 0.8610(4) 0.097(3) Uani 1 1 d D . . F1 F 0.1965(4) 0.6294(4) 0.6544(3) 0.151(2) Uani 1 1 d DU . . F2 F 0.1346(4) 0.5659(4) 0.5790(2) 0.1447(19) Uani 1 1 d DU . . F3 F 0.1482(3) 0.4780(3) 0.66459(17) 0.0858(11) Uani 1 1 d DU . . F4 F 0.2949(3) 0.4858(3) 0.6119(2) 0.1211(16) Uani 1 1 d DU . . F5 F 0.2308(5) 0.9196(6) 0.8975(3) 0.221(3) Uani 1 1 d DU . . F6 F 0.3188(5) 1.0362(5) 0.8849(2) 0.182(2) Uani 1 1 d DU . . F7 F 0.2835(4) 0.9646(4) 0.8064(2) 0.1451(19) Uani 1 1 d DU . . F8 F 0.1559(4) 1.0670(5) 0.8542(3) 0.185(3) Uani 1 1 d DU . . 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 0.0368(4) 0.0609(5) 0.0392(4) 0.0007(3) -0.0009(3) -0.0245(4) Cu2 0.0432(4) 0.0519(5) 0.0395(4) -0.0096(3) 0.0066(3) -0.0192(3) P1 0.0381(9) 0.0472(10) 0.0360(8) -0.0023(7) 0.0051(7) -0.0210(7) P2 0.0340(8) 0.0359(9) 0.0379(8) -0.0037(7) 0.0037(6) -0.0097(7) P4 0.0312(8) 0.0513(10) 0.0377(8) 0.0042(7) -0.0024(6) -0.0163(7) P3 0.0382(9) 0.0460(10) 0.0339(8) -0.0026(7) 0.0051(7) -0.0141(7) N1 0.042(3) 0.036(3) 0.040(3) 0.000(2) 0.000(2) -0.012(2) N2 0.034(3) 0.032(3) 0.034(2) 0.002(2) -0.001(2) -0.010(2) N3 0.027(3) 0.034(3) 0.068(3) -0.004(2) 0.002(2) -0.002(2) N4 0.033(3) 0.050(3) 0.042(3) -0.007(2) 0.000(2) -0.015(2) N5 0.039(3) 0.038(3) 0.041(3) -0.005(2) 0.003(2) -0.014(2) N6 0.035(3) 0.064(3) 0.052(3) 0.004(3) 0.003(2) 0.000(2) C1 0.080(5) 0.042(4) 0.101(5) -0.010(4) -0.007(4) -0.004(4) C2 0.069(4) 0.047(4) 0.044(4) -0.009(3) 0.014(3) -0.019(3) C3 0.081(5) 0.048(4) 0.057(4) -0.020(3) 0.002(4) -0.027(4) C4 0.069(5) 0.068(5) 0.052(4) -0.009(4) -0.013(3) -0.033(4) C5 0.041(3) 0.049(4) 0.038(3) -0.002(3) -0.008(3) -0.021(3) C6 0.054(4) 0.072(5) 0.054(4) 0.003(3) -0.015(3) -0.033(4) C7 0.037(3) 0.051(4) 0.067(4) 0.006(3) -0.014(3) -0.010(3) C8 0.037(3) 0.037(4) 0.043(3) 0.008(3) -0.002(3) -0.017(3) C9 0.034(3) 0.036(3) 0.030(3) 0.000(3) 0.005(2) -0.012(3) C10 0.038(3) 0.033(3) 0.048(3) 0.000(3) -0.003(3) -0.007(3) C11 0.043(3) 0.034(3) 0.047(4) 0.003(3) -0.003(3) -0.013(3) C12 0.043(4) 0.036(4) 0.072(4) -0.006(3) 0.001(3) -0.002(3) C13 0.047(4) 0.051(5) 0.110(6) -0.017(4) 0.001(4) -0.001(4) C14 0.060(5) 0.041(5) 0.155(9) -0.012(5) -0.046(6) -0.002(4) C15 0.091(6) 0.057(5) 0.105(7) 0.025(4) -0.053(5) -0.023(5) C16 0.061(4) 0.055(4) 0.063(4) 0.009(3) -0.016(3) -0.024(4) C17 0.033(3) 0.029(3) 0.038(3) -0.004(3) 0.005(2) -0.007(2) C18 0.044(4) 0.059(4) 0.056(4) -0.022(3) 0.006(3) -0.010(3) C19 0.067(5) 0.068(5) 0.065(4) -0.030(4) -0.016(4) -0.005(4) C20 0.066(5) 0.056(4) 0.078(5) -0.011(4) -0.022(4) -0.022(4) C21 0.044(4) 0.065(4) 0.060(4) -0.008(3) -0.002(3) -0.017(3) C22 0.051(4) 0.039(4) 0.042(3) -0.008(3) 0.002(3) -0.010(3) C23 0.049(4) 0.091(6) 0.093(5) 0.006(4) -0.024(4) -0.011(4) C24 0.040(4) 0.077(5) 0.050(4) 0.001(3) -0.006(3) -0.026(3) C25 0.059(5) 0.088(6) 0.075(5) -0.009(4) -0.017(4) -0.036(4) C26 0.083(5) 0.082(6) 0.070(5) -0.028(4) 0.001(4) -0.044(4) C27 0.062(4) 0.053(4) 0.047(4) -0.016(3) 0.004(3) -0.029(4) C28 0.078(5) 0.046(4) 0.062(4) -0.020(3) 0.016(4) -0.021(4) C29 0.060(4) 0.046(4) 0.063(4) -0.013(3) 0.012(3) -0.008(3) C30 0.036(3) 0.049(4) 0.036(3) 0.004(3) 0.012(3) -0.011(3) C31 0.039(3) 0.046(4) 0.033(3) -0.001(3) 0.004(3) -0.022(3) C32 0.038(3) 0.059(4) 0.046(4) 0.010(3) -0.001(3) -0.018(3) C33 0.035(3) 0.051(4) 0.044(3) 0.002(3) 0.004(3) -0.021(3) C34 0.056(4) 0.061(5) 0.058(4) -0.001(4) 0.002(3) -0.008(4) C35 0.081(5) 0.048(5) 0.099(6) -0.012(4) 0.027(5) -0.008(4) C36 0.059(5) 0.087(6) 0.090(6) 0.016(5) -0.009(4) 0.013(4) C37 0.065(5) 0.082(6) 0.103(6) 0.008(5) -0.032(4) 0.006(4) C38 0.048(4) 0.071(5) 0.073(4) 0.000(4) -0.026(3) -0.008(4) C39 0.035(3) 0.054(4) 0.041(3) 0.006(3) -0.009(3) -0.013(3) C40 0.048(4) 0.066(5) 0.062(4) 0.006(4) -0.005(3) -0.025(3) C41 0.075(5) 0.053(5) 0.094(6) 0.003(4) -0.038(4) -0.032(4) C42 0.085(6) 0.076(6) 0.089(6) -0.028(5) -0.007(5) -0.022(5) C43 0.082(6) 0.116(7) 0.098(6) -0.053(5) 0.011(4) -0.047(5) C44 0.064(4) 0.084(5) 0.074(5) -0.025(4) 0.012(4) -0.042(4) C45 0.046(4) 0.046(4) 0.038(3) 0.001(3) 0.007(3) -0.023(3) C46 0.045(4) 0.075(5) 0.064(4) -0.022(4) 0.002(3) -0.025(4) C47 0.046(4) 0.116(7) 0.085(5) -0.021(5) 0.000(4) -0.023(4) C48 0.073(5) 0.123(7) 0.063(5) -0.003(5) -0.008(4) -0.064(5) C49 0.088(5) 0.077(5) 0.064(4) -0.006(4) -0.009(4) -0.056(5) C50 0.057(4) 0.051(4) 0.055(4) 0.004(3) -0.004(3) -0.025(3) C51 0.040(3) 0.049(4) 0.037(3) -0.002(3) 0.004(3) -0.024(3) C52 0.048(4) 0.055(4) 0.046(4) -0.005(3) -0.002(3) -0.023(3) C53 0.095(5) 0.067(5) 0.038(4) -0.015(4) 0.009(3) -0.044(4) C54 0.105(6) 0.045(5) 0.072(5) -0.023(4) 0.023(4) -0.025(4) C55 0.082(5) 0.046(4) 0.070(5) -0.002(4) 0.021(4) -0.020(4) C56 0.060(4) 0.055(4) 0.049(4) 0.006(3) 0.005(3) -0.026(3) C57 0.044(4) 0.050(4) 0.032(3) -0.008(3) 0.007(3) -0.023(3) C58 0.043(4) 0.062(4) 0.050(4) 0.003(3) 0.003(3) -0.023(3) C59 0.053(4) 0.062(5) 0.062(4) 0.002(4) -0.010(3) -0.012(4) C60 0.086(5) 0.058(5) 0.048(4) 0.006(3) -0.020(4) -0.023(4) C61 0.072(5) 0.057(5) 0.044(4) 0.007(3) 0.003(3) -0.025(4) C62 0.052(4) 0.057(4) 0.047(4) 0.002(3) 0.007(3) -0.020(3) C63 0.029(3) 0.049(4) 0.036(3) -0.005(3) 0.009(2) -0.007(3) C64 0.075(4) 0.049(4) 0.046(4) 0.001(3) 0.020(3) -0.017(3) C65 0.087(5) 0.054(5) 0.068(5) -0.002(4) 0.019(4) -0.007(4) C66 0.066(4) 0.053(4) 0.059(4) 0.021(4) 0.000(4) -0.011(4) C67 0.054(4) 0.072(5) 0.045(4) 0.012(4) 0.003(3) -0.008(4) C68 0.046(4) 0.055(4) 0.046(4) -0.001(3) 0.011(3) -0.008(3) C69 0.040(3) 0.044(4) 0.031(3) -0.001(3) 0.004(3) -0.010(3) C70 0.057(4) 0.061(4) 0.045(4) -0.011(3) 0.001(3) -0.005(3) C71 0.081(5) 0.068(5) 0.082(5) -0.031(4) 0.010(4) 0.006(4) C72 0.113(7) 0.070(5) 0.068(5) -0.024(4) 0.011(5) -0.029(5) C73 0.084(5) 0.097(6) 0.055(4) -0.021(4) -0.003(4) -0.044(5) C74 0.050(4) 0.071(5) 0.054(4) -0.011(3) 0.005(3) -0.022(3) C75 0.041(3) 0.057(4) 0.030(3) -0.004(3) 0.007(3) -0.023(3) C76 0.048(4) 0.069(5) 0.049(4) -0.001(3) -0.001(3) -0.023(3) C77 0.055(4) 0.080(5) 0.072(5) -0.015(4) 0.002(4) -0.038(4) C78 0.055(4) 0.097(6) 0.065(5) -0.007(4) -0.010(4) -0.028(4) C79 0.044(4) 0.090(6) 0.051(4) 0.005(4) -0.012(3) -0.009(4) C80 0.045(4) 0.067(4) 0.043(3) 0.004(3) 0.003(3) -0.022(3) B1 0.046(5) 0.057(6) 0.092(7) 0.017(5) -0.017(5) -0.011(4) B2 0.080(8) 0.135(11) 0.093(8) 0.013(8) 0.002(6) -0.059(8) F1 0.143(4) 0.110(4) 0.222(5) -0.041(4) 0.021(4) -0.069(3) F2 0.111(3) 0.177(5) 0.157(4) 0.074(4) -0.052(3) -0.061(3) F3 0.069(2) 0.063(2) 0.119(3) 0.029(2) 0.017(2) -0.008(2) F4 0.062(3) 0.118(4) 0.166(4) 0.031(3) 0.026(3) 0.003(2) F5 0.229(6) 0.223(6) 0.243(6) 0.091(5) 0.018(5) -0.127(5) F6 0.182(5) 0.258(6) 0.143(4) 0.025(4) -0.036(4) -0.122(5) F7 0.112(4) 0.182(5) 0.131(4) -0.053(4) 0.023(3) -0.019(3) F8 0.099(4) 0.193(5) 0.238(6) -0.037(5) 0.009(4) 0.009(4) _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 2.179(4) . ? Cu1 P4 2.2179(15) . ? Cu1 N2 2.239(4) . ? Cu1 P1 2.2931(15) . ? Cu2 N4 2.053(4) . ? Cu2 P2 2.2231(14) . ? Cu2 P3 2.2883(16) . ? P1 C57 1.812(5) . ? P1 C51 1.833(5) . ? P1 C45 1.834(5) . ? P2 C11 1.812(5) . ? P2 C17 1.815(5) . ? P2 C10 1.859(5) . ? P4 C33 1.819(5) . ? P4 C39 1.820(5) . ? P4 C32 1.852(5) . ? P3 C63 1.818(5) . ? P3 C69 1.829(5) . ? P3 C75 1.839(5) . ? N1 C2 1.338(6) . ? N1 C9 1.350(5) . ? N2 C8 1.322(6) . ? N2 C9 1.375(6) . ? N3 C8 1.352(6) . ? N3 C10 1.446(5) . ? N3 H3 0.8600 . ? N4 C24 1.318(6) . ? N4 C31 1.368(6) . ? N5 C30 1.316(6) . ? N5 C31 1.359(5) . ? N6 C30 1.357(6) . ? N6 C32 1.449(6) . ? N6 H6 0.8600 . ? C1 C2 1.497(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.416(7) . ? C3 C4 1.346(7) . ? C3 H3A 0.9300 . ? C4 C5 1.398(7) . ? C4 H4 0.9300 . ? C5 C9 1.393(6) . ? C5 C6 1.421(7) . ? C6 C7 1.345(7) . ? C6 H6A 0.9300 . ? C7 C8 1.433(6) . ? C7 H7 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.387(7) . ? C11 C12 1.387(7) . ? C12 C13 1.397(7) . ? C12 H12 0.9300 . ? C13 C14 1.360(9) . ? C13 H13 0.9300 . ? C14 C15 1.364(9) . ? C14 H14 0.9300 . ? C15 C16 1.383(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.380(6) . ? C17 C22 1.387(6) . ? C18 C19 1.382(7) . ? C18 H18 0.9300 . ? C19 C20 1.373(7) . ? C19 H19 0.9300 . ? C20 C21 1.369(7) . ? C20 H20 0.9300 . ? C21 C22 1.373(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.495(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.409(7) . ? C25 C26 1.376(8) . ? C25 H25 0.9300 . ? C26 C27 1.400(7) . ? C26 H26 0.9300 . ? C27 C31 1.401(7) . ? C27 C28 1.419(7) . ? C28 C29 1.334(7) . ? C28 H28 0.9300 . ? C29 C30 1.435(7) . ? C29 H29 0.9300 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.377(7) . ? C33 C38 1.383(6) . ? C34 C35 1.396(8) . ? C34 H34 0.9300 . ? C35 C36 1.372(8) . ? C35 H35 0.9300 . ? C36 C37 1.355(9) . ? C36 H36 0.9300 . ? C37 C38 1.394(8) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.367(7) . ? C39 C40 1.386(7) . ? C40 C41 1.391(7) . ? C40 H40 0.9300 . ? C41 C42 1.352(8) . ? C41 H41 0.9300 . ? C42 C43 1.356(9) . ? C42 H42 0.9300 . ? C43 C44 1.383(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.379(7) . ? C45 C46 1.388(7) . ? C46 C47 1.386(7) . ? C46 H46 0.9300 . ? C47 C48 1.367(9) . ? C47 H47 0.9300 . ? C48 C49 1.369(8) . ? C48 H48 0.9300 . ? C49 C50 1.367(7) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C56 1.386(7) . ? C51 C52 1.405(6) . ? C52 C53 1.385(7) . ? C52 H52 0.9300 . ? C53 C54 1.357(8) . ? C53 H53 0.9300 . ? C54 C55 1.369(8) . ? C54 H54 0.9300 . ? C55 C56 1.365(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.386(6) . ? C57 C62 1.402(7) . ? C58 C59 1.394(7) . ? C58 H58 0.9300 . ? C59 C60 1.368(8) . ? C59 H59 0.9300 . ? C60 C61 1.384(7) . ? C60 H60 0.9300 . ? C61 C62 1.376(7) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.377(6) . ? C63 C68 1.391(6) . ? C64 C65 1.394(7) . ? C64 H64 0.9300 . ? C65 C66 1.357(7) . ? C65 H65 0.9300 . ? C66 C67 1.369(7) . ? C66 H66 0.9300 . ? C67 C68 1.395(7) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.361(6) . ? C69 C74 1.387(6) . ? C70 C71 1.377(7) . ? C70 H70 0.9300 . ? C71 C72 1.351(8) . ? C71 H71 0.9300 . ? C72 C73 1.382(8) . ? C72 H72 0.9300 . ? C73 C74 1.386(7) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 C76 1.379(7) . ? C75 C80 1.404(7) . ? C76 C77 1.388(7) . ? C76 H76 0.9300 . ? C77 C78 1.379(8) . ? C77 H77 0.9300 . ? C78 C79 1.377(8) . ? C78 H78 0.9300 . ? C79 C80 1.377(7) . ? C79 H79 0.9300 . ? C80 H80 0.9300 . ? B1 F4 1.348(6) . ? B1 F1 1.348(6) . ? B1 F2 1.351(6) . ? B1 F3 1.366(6) . ? B2 F5 1.305(7) . ? B2 F8 1.318(7) . ? B2 F7 1.332(7) . ? B2 F6 1.343(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 Cu1 P4 125.94(12) . . ? N1 Cu1 N2 61.52(14) . . ? P4 Cu1 N2 124.94(11) . . ? N1 Cu1 P1 100.43(12) . . ? P4 Cu1 P1 126.31(5) . . ? N2 Cu1 P1 98.78(11) . . ? N4 Cu2 P2 119.87(12) . . ? N4 Cu2 P3 106.90(12) . . ? P2 Cu2 P3 131.59(6) . . ? C57 P1 C51 104.1(2) . . ? C57 P1 C45 103.9(2) . . ? C51 P1 C45 105.7(2) . . ? C57 P1 Cu1 116.29(17) . . ? C51 P1 Cu1 114.82(18) . . ? C45 P1 Cu1 110.90(16) . . ? C11 P2 C17 105.1(2) . . ? C11 P2 C10 102.2(2) . . ? C17 P2 C10 102.1(2) . . ? C11 P2 Cu2 113.72(18) . . ? C17 P2 Cu2 116.78(17) . . ? C10 P2 Cu2 115.16(16) . . ? C33 P4 C39 105.1(2) . . ? C33 P4 C32 103.5(2) . . ? C39 P4 C32 102.8(3) . . ? C33 P4 Cu1 109.86(17) . . ? C39 P4 Cu1 116.37(18) . . ? C32 P4 Cu1 117.82(16) . . ? C63 P3 C69 104.6(2) . . ? C63 P3 C75 103.3(2) . . ? C69 P3 C75 107.0(2) . . ? C63 P3 Cu2 117.25(17) . . ? C69 P3 Cu2 109.93(18) . . ? C75 P3 Cu2 113.95(17) . . ? C2 N1 C9 118.5(5) . . ? C2 N1 Cu1 143.9(4) . . ? C9 N1 Cu1 93.6(3) . . ? C8 N2 C9 117.1(4) . . ? C8 N2 Cu1 146.9(3) . . ? C9 N2 Cu1 90.4(3) . . ? C8 N3 C10 125.9(4) . . ? C8 N3 H3 117.1 . . ? C10 N3 H3 117.1 . . ? C24 N4 C31 119.5(5) . . ? C24 N4 Cu2 135.1(4) . . ? C31 N4 Cu2 103.0(3) . . ? C30 N5 C31 116.8(4) . . ? C30 N6 C32 125.2(4) . . ? C30 N6 H6 117.4 . . ? C32 N6 H6 117.4 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 120.0(5) . . ? N1 C2 C1 117.6(5) . . ? C3 C2 C1 122.4(5) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C9 C5 C4 117.2(5) . . ? C9 C5 C6 116.8(5) . . ? C4 C5 C6 125.8(5) . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 119.6(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? N2 C8 N3 119.7(4) . . ? N2 C8 C7 122.6(5) . . ? N3 C8 C7 117.7(5) . . ? N1 C9 N2 112.0(4) . . ? N1 C9 C5 123.8(5) . . ? N2 C9 C5 124.1(5) . . ? N3 C10 P2 110.4(3) . . ? N3 C10 H10A 109.6 . . ? P2 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? P2 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C16 C11 C12 117.4(5) . . ? C16 C11 P2 118.8(4) . . ? C12 C11 P2 123.7(4) . . ? C11 C12 C13 120.9(6) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 120.4(7) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.4(7) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 120.9(7) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.9(6) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C18 C17 C22 117.4(5) . . ? C18 C17 P2 123.4(4) . . ? C22 C17 P2 119.2(4) . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.3(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 118.4(5) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? C21 C22 C17 122.8(5) . . ? C21 C22 H22 118.6 . . ? C17 C22 H22 118.6 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 C25 122.1(6) . . ? N4 C24 C23 117.3(5) . . ? C25 C24 C23 120.6(5) . . ? C26 C25 C24 118.0(6) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 C27 121.5(6) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C26 C27 C31 116.3(6) . . ? C26 C27 C28 127.0(5) . . ? C31 C27 C28 116.6(5) . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 119.5(5) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? N5 C30 N6 119.6(5) . . ? N5 C30 C29 122.7(5) . . ? N6 C30 C29 117.7(5) . . ? N5 C31 N4 113.2(4) . . ? N5 C31 C27 124.3(5) . . ? N4 C31 C27 122.4(5) . . ? N6 C32 P4 111.6(4) . . ? N6 C32 H32A 109.3 . . ? P4 C32 H32A 109.3 . . ? N6 C32 H32B 109.3 . . ? P4 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C38 117.3(5) . . ? C34 C33 P4 118.9(4) . . ? C38 C33 P4 123.3(4) . . ? C33 C34 C35 121.1(6) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 120.9(6) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 118.3(7) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C36 C37 C38 121.4(6) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C33 C38 C37 120.9(6) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C44 C39 C40 116.7(5) . . ? C44 C39 P4 118.4(4) . . ? C40 C39 P4 124.9(5) . . ? C39 C40 C41 120.7(6) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 120.3(6) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.4(7) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 119.1(7) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C39 C44 C43 122.8(6) . . ? C39 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C50 C45 C46 118.2(5) . . ? C50 C45 P1 118.4(4) . . ? C46 C45 P1 123.0(4) . . ? C47 C46 C45 119.8(6) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C48 C47 C46 120.7(6) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 119.8(6) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C50 C49 C48 119.9(6) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C45 121.7(6) . . ? C49 C50 H50 119.1 . . ? C45 C50 H50 119.1 . . ? C56 C51 C52 118.0(5) . . ? C56 C51 P1 119.7(4) . . ? C52 C51 P1 122.3(4) . . ? C53 C52 C51 119.2(5) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? C54 C53 C52 121.3(6) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C53 C54 C55 119.8(6) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 120.2(6) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C51 121.5(5) . . ? C55 C56 H56 119.3 . . ? C51 C56 H56 119.3 . . ? C58 C57 C62 117.8(5) . . ? C58 C57 P1 119.6(4) . . ? C62 C57 P1 122.5(4) . . ? C57 C58 C59 120.4(6) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C60 C59 C58 120.9(6) . . ? C60 C59 H59 119.6 . . ? C58 C59 H59 119.6 . . ? C59 C60 C61 119.6(6) . . ? C59 C60 H60 120.2 . . ? C61 C60 H60 120.2 . . ? C62 C61 C60 119.9(6) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C57 121.4(5) . . ? C61 C62 H62 119.3 . . ? C57 C62 H62 119.3 . . ? C64 C63 C68 117.3(5) . . ? C64 C63 P3 119.0(4) . . ? C68 C63 P3 123.5(4) . . ? C63 C64 C65 121.7(5) . . ? C63 C64 H64 119.1 . . ? C65 C64 H64 119.1 . . ? C66 C65 C64 120.0(6) . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C67 119.9(6) . . ? C65 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C66 C67 C68 120.3(5) . . ? C66 C67 H67 119.8 . . ? C68 C67 H67 119.8 . . ? C63 C68 C67 120.7(5) . . ? C63 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C70 C69 C74 118.2(5) . . ? C70 C69 P3 124.5(4) . . ? C74 C69 P3 116.9(4) . . ? C69 C70 C71 120.8(6) . . ? C69 C70 H70 119.6 . . ? C71 C70 H70 119.6 . . ? C72 C71 C70 121.3(6) . . ? C72 C71 H71 119.3 . . ? C70 C71 H71 119.3 . . ? C71 C72 C73 119.3(6) . . ? C71 C72 H72 120.3 . . ? C73 C72 H72 120.3 . . ? C72 C73 C74 119.3(6) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C73 C74 C69 121.0(6) . . ? C73 C74 H74 119.5 . . ? C69 C74 H74 119.5 . . ? C76 C75 C80 117.8(5) . . ? C76 C75 P3 122.9(5) . . ? C80 C75 P3 118.9(4) . . ? C75 C76 C77 121.0(6) . . ? C75 C76 H76 119.5 . . ? C77 C76 H76 119.5 . . ? C78 C77 C76 120.1(6) . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C79 C78 C77 120.1(6) . . ? C79 C78 H78 119.9 . . ? C77 C78 H78 119.9 . . ? C78 C79 C80 119.5(6) . . ? C78 C79 H79 120.2 . . ? C80 C79 H79 120.2 . . ? C79 C80 C75 121.5(6) . . ? C79 C80 H80 119.3 . . ? C75 C80 H80 119.3 . . ? F4 B1 F1 109.4(6) . . ? F4 B1 F2 109.8(6) . . ? F1 B1 F2 106.2(6) . . ? F4 B1 F3 112.3(5) . . ? F1 B1 F3 111.0(6) . . ? F2 B1 F3 107.9(5) . . ? F5 B2 F8 108.9(7) . . ? F5 B2 F7 117.6(9) . . ? F8 B2 F7 106.9(7) . . ? F5 B2 F6 108.4(7) . . ? F8 B2 F6 109.7(8) . . ? F7 B2 F6 105.2(6) . . ? 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 Cu1 P1 C57 92.2(2) . . . . ? P4 Cu1 P1 C57 -58.95(19) . . . . ? N2 Cu1 P1 C57 154.7(2) . . . . ? N1 Cu1 P1 C51 -145.9(2) . . . . ? P4 Cu1 P1 C51 62.9(2) . . . . ? N2 Cu1 P1 C51 -83.4(2) . . . . ? N1 Cu1 P1 C45 -26.2(2) . . . . ? P4 Cu1 P1 C45 -177.4(2) . . . . ? N2 Cu1 P1 C45 36.3(2) . . . . ? N4 Cu2 P2 C11 -75.2(2) . . . . ? P3 Cu2 P2 C11 88.2(2) . . . . ? N4 Cu2 P2 C17 162.1(2) . . . . ? P3 Cu2 P2 C17 -34.5(2) . . . . ? N4 Cu2 P2 C10 42.3(2) . . . . ? P3 Cu2 P2 C10 -154.38(17) . . . . ? N1 Cu1 P4 C33 -76.6(2) . . . . ? N2 Cu1 P4 C33 -154.4(2) . . . . ? P1 Cu1 P4 C33 67.5(2) . . . . ? N1 Cu1 P4 C39 164.2(2) . . . . ? N2 Cu1 P4 C39 86.4(2) . . . . ? P1 Cu1 P4 C39 -51.7(2) . . . . ? N1 Cu1 P4 C32 41.4(3) . . . . ? N2 Cu1 P4 C32 -36.3(2) . . . . ? P1 Cu1 P4 C32 -174.4(2) . . . . ? N4 Cu2 P3 C63 100.0(2) . . . . ? P2 Cu2 P3 C63 -64.9(2) . . . . ? N4 Cu2 P3 C69 -19.2(2) . . . . ? P2 Cu2 P3 C69 175.89(18) . . . . ? N4 Cu2 P3 C75 -139.2(2) . . . . ? P2 Cu2 P3 C75 55.9(2) . . . . ? P4 Cu1 N1 C2 82.1(6) . . . . ? N2 Cu1 N1 C2 -163.6(7) . . . . ? P1 Cu1 N1 C2 -69.2(6) . . . . ? P4 Cu1 N1 C9 -123.9(3) . . . . ? N2 Cu1 N1 C9 -9.7(3) . . . . ? P1 Cu1 N1 C9 84.7(3) . . . . ? N1 Cu1 N2 C8 157.0(7) . . . . ? P4 Cu1 N2 C8 -87.1(6) . . . . ? P1 Cu1 N2 C8 59.9(6) . . . . ? N1 Cu1 N2 C9 9.5(3) . . . . ? P4 Cu1 N2 C9 125.3(2) . . . . ? P1 Cu1 N2 C9 -87.7(3) . . . . ? P2 Cu2 N4 C24 82.3(5) . . . . ? P3 Cu2 N4 C24 -84.7(5) . . . . ? P2 Cu2 N4 C31 -115.9(3) . . . . ? P3 Cu2 N4 C31 77.0(3) . . . . ? C9 N1 C2 C3 -0.6(7) . . . . ? Cu1 N1 C2 C3 149.5(5) . . . . ? C9 N1 C2 C1 -178.7(5) . . . . ? Cu1 N1 C2 C1 -28.6(9) . . . . ? N1 C2 C3 C4 -0.2(9) . . . . ? C1 C2 C3 C4 177.8(6) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C3 C4 C5 C9 0.5(8) . . . . ? C3 C4 C5 C6 -174.7(5) . . . . ? C9 C5 C6 C7 0.3(8) . . . . ? C4 C5 C6 C7 175.5(6) . . . . ? C5 C6 C7 C8 1.7(8) . . . . ? C9 N2 C8 N3 -179.7(4) . . . . ? Cu1 N2 C8 N3 37.3(9) . . . . ? C9 N2 C8 C7 1.1(7) . . . . ? Cu1 N2 C8 C7 -141.9(5) . . . . ? C10 N3 C8 N2 15.0(8) . . . . ? C10 N3 C8 C7 -165.7(4) . . . . ? C6 C7 C8 N2 -2.5(8) . . . . ? C6 C7 C8 N3 178.3(5) . . . . ? C2 N1 C9 N2 177.9(4) . . . . ? Cu1 N1 C9 N2 15.0(4) . . . . ? C2 N1 C9 C5 1.4(7) . . . . ? Cu1 N1 C9 C5 -161.5(4) . . . . ? C8 N2 C9 N1 -175.4(4) . . . . ? Cu1 N2 C9 N1 -14.6(4) . . . . ? C8 N2 C9 C5 1.1(7) . . . . ? Cu1 N2 C9 C5 161.9(4) . . . . ? C4 C5 C9 N1 -1.4(7) . . . . ? C6 C5 C9 N1 174.3(5) . . . . ? C4 C5 C9 N2 -177.4(5) . . . . ? C6 C5 C9 N2 -1.8(7) . . . . ? C8 N3 C10 P2 100.2(5) . . . . ? C11 P2 C10 N3 56.1(4) . . . . ? C17 P2 C10 N3 164.7(3) . . . . ? Cu2 P2 C10 N3 -67.7(3) . . . . ? C17 P2 C11 C16 100.2(4) . . . . ? C10 P2 C11 C16 -153.4(4) . . . . ? Cu2 P2 C11 C16 -28.7(5) . . . . ? C17 P2 C11 C12 -83.3(5) . . . . ? C10 P2 C11 C12 23.0(5) . . . . ? Cu2 P2 C11 C12 147.8(4) . . . . ? C16 C11 C12 C13 0.0(8) . . . . ? P2 C11 C12 C13 -176.5(4) . . . . ? C11 C12 C13 C14 -1.4(9) . . . . ? C12 C13 C14 C15 -0.2(10) . . . . ? C13 C14 C15 C16 3.2(11) . . . . ? C14 C15 C16 C11 -4.7(10) . . . . ? C12 C11 C16 C15 3.0(8) . . . . ? P2 C11 C16 C15 179.7(4) . . . . ? C11 P2 C17 C18 42.3(5) . . . . ? C10 P2 C17 C18 -64.0(5) . . . . ? Cu2 P2 C17 C18 169.4(4) . . . . ? C11 P2 C17 C22 -138.2(4) . . . . ? C10 P2 C17 C22 115.4(4) . . . . ? Cu2 P2 C17 C22 -11.1(5) . . . . ? C22 C17 C18 C19 -1.5(8) . . . . ? P2 C17 C18 C19 177.9(4) . . . . ? C17 C18 C19 C20 0.7(9) . . . . ? C18 C19 C20 C21 0.7(10) . . . . ? C19 C20 C21 C22 -1.1(9) . . . . ? C20 C21 C22 C17 0.2(8) . . . . ? C18 C17 C22 C21 1.1(8) . . . . ? P2 C17 C22 C21 -178.4(4) . . . . ? C31 N4 C24 C25 -2.7(8) . . . . ? Cu2 N4 C24 C25 156.8(5) . . . . ? C31 N4 C24 C23 178.5(5) . . . . ? Cu2 N4 C24 C23 -22.0(8) . . . . ? N4 C24 C25 C26 -0.6(9) . . . . ? C23 C24 C25 C26 178.2(6) . . . . ? C24 C25 C26 C27 2.2(10) . . . . ? C25 C26 C27 C31 -0.6(9) . . . . ? C25 C26 C27 C28 -176.3(6) . . . . ? C26 C27 C28 C29 178.2(6) . . . . ? C31 C27 C28 C29 2.5(8) . . . . ? C27 C28 C29 C30 2.4(9) . . . . ? C31 N5 C30 N6 -176.6(4) . . . . ? C31 N5 C30 C29 5.3(7) . . . . ? C32 N6 C30 N5 12.3(8) . . . . ? C32 N6 C30 C29 -169.5(5) . . . . ? C28 C29 C30 N5 -6.8(8) . . . . ? C28 C29 C30 N6 175.1(5) . . . . ? C30 N5 C31 N4 -177.5(4) . . . . ? C30 N5 C31 C27 0.1(7) . . . . ? C24 N4 C31 N5 -177.8(4) . . . . ? Cu2 N4 C31 N5 16.9(5) . . . . ? C24 N4 C31 C27 4.5(7) . . . . ? Cu2 N4 C31 C27 -160.8(4) . . . . ? C26 C27 C31 N5 179.8(5) . . . . ? C28 C27 C31 N5 -4.0(8) . . . . ? C26 C27 C31 N4 -2.8(8) . . . . ? C28 C27 C31 N4 173.3(5) . . . . ? C30 N6 C32 P4 91.3(5) . . . . ? C33 P4 C32 N6 68.7(4) . . . . ? C39 P4 C32 N6 177.8(3) . . . . ? Cu1 P4 C32 N6 -52.8(4) . . . . ? C39 P4 C33 C34 177.1(4) . . . . ? C32 P4 C33 C34 -75.5(5) . . . . ? Cu1 P4 C33 C34 51.2(5) . . . . ? C39 P4 C33 C38 5.3(5) . . . . ? C32 P4 C33 C38 112.8(5) . . . . ? Cu1 P4 C33 C38 -120.6(4) . . . . ? C38 C33 C34 C35 -0.1(9) . . . . ? P4 C33 C34 C35 -172.3(5) . . . . ? C33 C34 C35 C36 1.7(10) . . . . ? C34 C35 C36 C37 -2.1(11) . . . . ? C35 C36 C37 C38 1.0(12) . . . . ? C34 C33 C38 C37 -1.0(9) . . . . ? P4 C33 C38 C37 170.9(5) . . . . ? C36 C37 C38 C33 0.6(11) . . . . ? C33 P4 C39 C44 -100.4(5) . . . . ? C32 P4 C39 C44 151.6(5) . . . . ? Cu1 P4 C39 C44 21.3(5) . . . . ? C33 P4 C39 C40 79.7(5) . . . . ? C32 P4 C39 C40 -28.2(5) . . . . ? Cu1 P4 C39 C40 -158.5(4) . . . . ? C44 C39 C40 C41 0.7(8) . . . . ? P4 C39 C40 C41 -179.5(4) . . . . ? C39 C40 C41 C42 -0.7(9) . . . . ? C40 C41 C42 C43 0.6(11) . . . . ? C41 C42 C43 C44 -0.6(12) . . . . ? C40 C39 C44 C43 -0.7(9) . . . . ? P4 C39 C44 C43 179.5(5) . . . . ? C42 C43 C44 C39 0.6(11) . . . . ? C57 P1 C45 C50 -47.7(5) . . . . ? C51 P1 C45 C50 -157.0(4) . . . . ? Cu1 P1 C45 C50 78.0(4) . . . . ? C57 P1 C45 C46 140.0(5) . . . . ? C51 P1 C45 C46 30.7(5) . . . . ? Cu1 P1 C45 C46 -94.3(4) . . . . ? C50 C45 C46 C47 2.4(8) . . . . ? P1 C45 C46 C47 174.7(5) . . . . ? C45 C46 C47 C48 -2.1(10) . . . . ? C46 C47 C48 C49 0.7(11) . . . . ? C47 C48 C49 C50 0.3(10) . . . . ? C48 C49 C50 C45 0.1(9) . . . . ? C46 C45 C50 C49 -1.5(8) . . . . ? P1 C45 C50 C49 -174.1(4) . . . . ? C57 P1 C51 C56 179.3(4) . . . . ? C45 P1 C51 C56 -71.5(5) . . . . ? Cu1 P1 C51 C56 51.0(5) . . . . ? C57 P1 C51 C52 1.5(5) . . . . ? C45 P1 C51 C52 110.6(4) . . . . ? Cu1 P1 C51 C52 -126.8(4) . . . . ? C56 C51 C52 C53 -1.5(8) . . . . ? P1 C51 C52 C53 176.3(4) . . . . ? C51 C52 C53 C54 1.6(9) . . . . ? C52 C53 C54 C55 0.0(10) . . . . ? C53 C54 C55 C56 -1.7(10) . . . . ? C54 C55 C56 C51 1.8(9) . . . . ? C52 C51 C56 C55 -0.1(8) . . . . ? P1 C51 C56 C55 -178.1(4) . . . . ? C51 P1 C57 C58 -106.7(4) . . . . ? C45 P1 C57 C58 142.8(4) . . . . ? Cu1 P1 C57 C58 20.7(4) . . . . ? C51 P1 C57 C62 74.4(4) . . . . ? C45 P1 C57 C62 -36.0(5) . . . . ? Cu1 P1 C57 C62 -158.2(4) . . . . ? C62 C57 C58 C59 -2.2(7) . . . . ? P1 C57 C58 C59 178.9(4) . . . . ? C57 C58 C59 C60 1.7(8) . . . . ? C58 C59 C60 C61 -0.5(9) . . . . ? C59 C60 C61 C62 -0.2(8) . . . . ? C60 C61 C62 C57 -0.4(8) . . . . ? C58 C57 C62 C61 1.6(7) . . . . ? P1 C57 C62 C61 -179.5(4) . . . . ? C69 P3 C63 C64 168.4(4) . . . . ? C75 P3 C63 C64 -79.8(4) . . . . ? Cu2 P3 C63 C64 46.4(5) . . . . ? C69 P3 C63 C68 -15.7(5) . . . . ? C75 P3 C63 C68 96.1(5) . . . . ? Cu2 P3 C63 C68 -137.7(4) . . . . ? C68 C63 C64 C65 0.7(8) . . . . ? P3 C63 C64 C65 176.8(5) . . . . ? C63 C64 C65 C66 0.8(10) . . . . ? C64 C65 C66 C67 -1.1(9) . . . . ? C65 C66 C67 C68 0.0(9) . . . . ? C64 C63 C68 C67 -1.8(8) . . . . ? P3 C63 C68 C67 -177.7(4) . . . . ? C66 C67 C68 C63 1.5(9) . . . . ? C63 P3 C69 C70 125.8(5) . . . . ? C75 P3 C69 C70 16.7(6) . . . . ? Cu2 P3 C69 C70 -107.5(5) . . . . ? C63 P3 C69 C74 -62.2(5) . . . . ? C75 P3 C69 C74 -171.3(4) . . . . ? Cu2 P3 C69 C74 64.5(4) . . . . ? C74 C69 C70 C71 1.1(9) . . . . ? P3 C69 C70 C71 173.0(5) . . . . ? C69 C70 C71 C72 -0.9(10) . . . . ? C70 C71 C72 C73 1.8(11) . . . . ? C71 C72 C73 C74 -2.9(11) . . . . ? C72 C73 C74 C69 3.2(10) . . . . ? C70 C69 C74 C73 -2.3(8) . . . . ? P3 C69 C74 C73 -174.8(5) . . . . ? C63 P3 C75 C76 9.3(5) . . . . ? C69 P3 C75 C76 119.3(4) . . . . ? Cu2 P3 C75 C76 -119.0(4) . . . . ? C63 P3 C75 C80 -178.4(4) . . . . ? C69 P3 C75 C80 -68.4(4) . . . . ? Cu2 P3 C75 C80 53.3(4) . . . . ? C80 C75 C76 C77 -1.6(8) . . . . ? P3 C75 C76 C77 170.8(4) . . . . ? C75 C76 C77 C78 0.6(8) . . . . ? C76 C77 C78 C79 1.2(9) . . . . ? C77 C78 C79 C80 -1.9(9) . . . . ? C78 C79 C80 C75 0.8(8) . . . . ? C76 C75 C80 C79 0.9(7) . . . . ? P3 C75 C80 C79 -171.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.660 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.074 # Attachment 'complex 3.cif' data_060926e _database_code_depnum_ccdc_archive 'CCDC 666204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H32 B Cu F4 N5 P' _chemical_formula_weight 740.01 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.300(11) _cell_length_b 12.055(3) _cell_length_c 25.150(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.728(5) _cell_angle_gamma 90.00 _cell_volume 14069(5) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4155 _cell_measurement_theta_min 2.345 _cell_measurement_theta_max 21.426 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6080 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6469 _exptl_absorpt_correction_T_max 0.8809 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 36058 _diffrn_reflns_av_R_equivalents 0.1226 _diffrn_reflns_av_sigmaI/netI 0.1583 _diffrn_reflns_limit_h_min -58 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12389 _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^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12389 _refine_ls_number_parameters 957 _refine_ls_number_restraints 494 _refine_ls_R_factor_all 0.1917 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.026 _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 0.174309(17) 0.13623(6) 0.55326(3) 0.0466(3) Uani 1 1 d . . . Cu2 Cu 0.076480(18) 0.87609(6) 0.69870(4) 0.0508(3) Uani 1 1 d . . . B1 B 0.0321(2) 0.5085(8) 0.3606(5) 0.080(3) Uani 1 1 d DU . . B2 B 0.2847(2) 0.7518(8) 0.6107(4) 0.078(3) Uani 1 1 d DU . . F1 F 0.03573(13) 0.4078(4) 0.3858(3) 0.152(2) Uani 1 1 d DU A . F2 F 0.0113(3) 0.5537(10) 0.3772(6) 0.163(5) Uani 0.589(10) 1 d PDU A 1 F3 F 0.0218(3) 0.4887(9) 0.3047(4) 0.137(5) Uani 0.589(10) 1 d PDU A 1 F4 F 0.0560(2) 0.5664(9) 0.3766(6) 0.121(5) Uani 0.589(10) 1 d PDU A 1 F5 F 0.3019(3) 0.8079(8) 0.6578(4) 0.121(4) Uani 0.642(14) 1 d PDU B 1 F6 F 0.2592(2) 0.7871(12) 0.5919(7) 0.168(5) Uani 0.642(14) 1 d PDU B 1 F7 F 0.2988(3) 0.7576(9) 0.5716(5) 0.108(4) Uani 0.642(14) 1 d PDU B 1 F2' F 0.0486(4) 0.5006(11) 0.3251(7) 0.113(5) Uani 0.411(10) 1 d PDU A 2 F3' F 0.0443(4) 0.5947(12) 0.3951(6) 0.115(5) Uani 0.411(10) 1 d PDU A 2 F4' F 0.0054(2) 0.5399(12) 0.3284(8) 0.112(5) Uani 0.411(10) 1 d PDU A 2 F5' F 0.2617(4) 0.7497(14) 0.5588(7) 0.126(7) Uani 0.358(14) 1 d PDU B 2 F6' F 0.3079(3) 0.7904(18) 0.5995(11) 0.129(7) Uani 0.358(14) 1 d PDU B 2 F7' F 0.2775(6) 0.8170(14) 0.6447(8) 0.146(6) Uani 0.358(14) 1 d PDU B 2 F8 F 0.28770(12) 0.6424(4) 0.6259(2) 0.1231(19) Uani 1 1 d DU B . P1 P 0.17587(4) -0.04304(14) 0.55467(8) 0.0423(5) Uani 1 1 d . . . P2 P 0.07353(4) 0.69738(15) 0.69511(8) 0.0508(5) Uani 1 1 d . . . N1 N 0.17299(13) 0.2548(4) 0.6111(3) 0.0474(16) Uani 1 1 d . . . N2 N 0.14446(12) 0.2409(5) 0.5015(3) 0.0527(17) Uani 1 1 d . . . N3 N 0.20619(11) 0.1594(5) 0.5103(2) 0.0458(15) Uani 1 1 d . . . N4 N 0.21008(12) 0.3376(5) 0.5429(3) 0.0554(17) Uani 1 1 d . . . N5 N 0.20507(11) -0.0224(5) 0.4806(2) 0.0516(16) Uani 1 1 d . . . H5 H 0.2019 -0.0663 0.4522 0.062 Uiso 1 1 calc R . . N6 N 0.07900(12) 0.9952(4) 0.6413(3) 0.0502(16) Uani 1 1 d . . . N7 N 0.10700(12) 0.9766(5) 0.7518(3) 0.0565(17) Uani 1 1 d . . . N8 N 0.04354(11) 0.8977(5) 0.7391(2) 0.0546(16) Uani 1 1 d . . . N9 N 0.04242(12) 1.0798(6) 0.7119(3) 0.0636(18) Uani 1 1 d . . . N10 N 0.04117(13) 0.7157(6) 0.7634(3) 0.073(2) Uani 1 1 d . . . H10 H 0.0425 0.6690 0.7900 0.088 Uiso 1 1 calc R . . C1 C 0.18670(16) 0.2544(6) 0.6674(4) 0.052(2) Uani 1 1 d . . . C2 C 0.18068(19) 0.3342(7) 0.7023(4) 0.074(3) Uani 1 1 d . . . H2 H 0.1904 0.3331 0.7411 0.089 Uiso 1 1 calc R . . C3 C 0.1605(2) 0.4134(7) 0.6789(5) 0.092(3) Uani 1 1 d . . . H3 H 0.1557 0.4648 0.7019 0.110 Uiso 1 1 calc R . . C4 C 0.14717(19) 0.4171(7) 0.6216(4) 0.077(3) Uani 1 1 d . . . H4 H 0.1340 0.4731 0.6051 0.092 Uiso 1 1 calc R . . C5 C 0.15357(16) 0.3365(6) 0.5885(4) 0.053(2) Uani 1 1 d . . . C6 C 0.13987(15) 0.3335(6) 0.5268(3) 0.0497(19) Uani 1 1 d . . . C7 C 0.12276(18) 0.4182(7) 0.4959(4) 0.082(3) Uani 1 1 d . . . H7 H 0.1200 0.4822 0.5141 0.099 Uiso 1 1 calc R . . C8 C 0.1100(2) 0.4081(9) 0.4391(5) 0.099(3) Uani 1 1 d . . . H8 H 0.0982 0.4644 0.4183 0.119 Uiso 1 1 calc R . . C9 C 0.11455(19) 0.3147(9) 0.4129(4) 0.087(3) Uani 1 1 d . . . H9 H 0.1060 0.3055 0.3741 0.104 Uiso 1 1 calc R . . C10 C 0.13212(18) 0.2348(7) 0.4455(4) 0.075(3) Uani 1 1 d . . . H10A H 0.1357 0.1719 0.4274 0.090 Uiso 1 1 calc R . . C11 C 0.20798(16) 0.1654(6) 0.6903(3) 0.055(2) Uani 1 1 d . . . C12 C 0.20955(18) 0.1100(8) 0.7393(3) 0.082(3) Uani 1 1 d . . . H12 H 0.1969 0.1294 0.7581 0.098 Uiso 1 1 calc R . . C13 C 0.2290(2) 0.0280(8) 0.7609(4) 0.089(3) Uani 1 1 d . . . H13 H 0.2297 -0.0070 0.7943 0.107 Uiso 1 1 calc R . . C14 C 0.2477(2) -0.0038(7) 0.7337(4) 0.085(3) Uani 1 1 d . . . H14 H 0.2605 -0.0622 0.7473 0.102 Uiso 1 1 calc R . . C15 C 0.24710(17) 0.0526(7) 0.6858(4) 0.075(2) Uani 1 1 d . . . H15 H 0.2602 0.0341 0.6680 0.090 Uiso 1 1 calc R . . C16 C 0.22742(16) 0.1362(6) 0.6636(3) 0.061(2) Uani 1 1 d . . . H16 H 0.2272 0.1729 0.6309 0.073 Uiso 1 1 calc R . . C17 C 0.21054(14) 0.2704(7) 0.5015(3) 0.051(2) Uani 1 1 d . . . C18 C 0.21379(14) 0.4455(7) 0.5378(4) 0.058(2) Uani 1 1 d . . . C19 C 0.21760(17) 0.4900(7) 0.4898(4) 0.072(3) Uani 1 1 d . . . H19 H 0.2199 0.5661 0.4872 0.086 Uiso 1 1 calc R . . C20 C 0.21795(16) 0.4240(8) 0.4472(4) 0.074(3) Uani 1 1 d . . . H20 H 0.2207 0.4538 0.4153 0.089 Uiso 1 1 calc R . . C21 C 0.21413(14) 0.3089(7) 0.4512(3) 0.056(2) Uani 1 1 d . . . C22 C 0.21424(17) 0.2282(8) 0.4111(4) 0.075(3) Uani 1 1 d . . . H22 H 0.2167 0.2502 0.3776 0.090 Uiso 1 1 calc R . . C23 C 0.21086(15) 0.1198(7) 0.4199(3) 0.063(2) Uani 1 1 d . . . H23 H 0.2109 0.0673 0.3929 0.075 Uiso 1 1 calc R . . C24 C 0.20725(14) 0.0871(6) 0.4717(3) 0.0479(19) Uani 1 1 d . . . C25 C 0.21366(17) 0.5193(6) 0.5851(3) 0.082(3) Uani 1 1 d . . . H25A H 0.2109 0.4755 0.6148 0.122 Uiso 1 1 calc R . . H25B H 0.1983 0.5722 0.5718 0.122 Uiso 1 1 calc R . . H25C H 0.2317 0.5577 0.5994 0.122 Uiso 1 1 calc R . . C26 C 0.20775(14) -0.0709(5) 0.5350(3) 0.0498(19) Uani 1 1 d . . . H26A H 0.2246 -0.0406 0.5637 0.060 Uiso 1 1 calc R . . H26B H 0.2104 -0.1504 0.5334 0.060 Uiso 1 1 calc R . . C27 C 0.14787(14) -0.1208(6) 0.5021(3) 0.0489(18) Uani 1 1 d . . . C28 C 0.12118(17) -0.0729(7) 0.4784(3) 0.072(2) Uani 1 1 d . . . H28 H 0.1178 -0.0019 0.4893 0.087 Uiso 1 1 calc R . . C29 C 0.09929(18) -0.1307(9) 0.4382(4) 0.095(3) Uani 1 1 d . . . H29 H 0.0813 -0.0976 0.4221 0.114 Uiso 1 1 calc R . . C30 C 0.1038(3) -0.2357(10) 0.4219(4) 0.105(4) Uani 1 1 d . . . H30 H 0.0890 -0.2744 0.3955 0.125 Uiso 1 1 calc R . . C31 C 0.1305(3) -0.2828(8) 0.4453(4) 0.096(3) Uani 1 1 d . . . H31 H 0.1340 -0.3536 0.4343 0.115 Uiso 1 1 calc R . . C32 C 0.15224(19) -0.2253(6) 0.4850(3) 0.069(2) Uani 1 1 d . . . H32 H 0.1703 -0.2581 0.5005 0.083 Uiso 1 1 calc R . . C33 C 0.18097(15) -0.1231(5) 0.6181(3) 0.0508(18) Uani 1 1 d . . . C34 C 0.16259(19) -0.1035(7) 0.6466(4) 0.099(3) Uani 1 1 d . . . H34 H 0.1484 -0.0494 0.6338 0.119 Uiso 1 1 calc R . . C35 C 0.1649(3) -0.1648(10) 0.6953(5) 0.135(5) Uani 1 1 d . . . H35 H 0.1520 -0.1513 0.7145 0.162 Uiso 1 1 calc R . . C36 C 0.1852(3) -0.2420(9) 0.7147(5) 0.123(4) Uani 1 1 d . . . H36 H 0.1862 -0.2838 0.7463 0.147 Uiso 1 1 calc R . . C37 C 0.2041(2) -0.2585(7) 0.6880(4) 0.097(3) Uani 1 1 d . . . H37 H 0.2187 -0.3109 0.7018 0.116 Uiso 1 1 calc R . . C38 C 0.20237(17) -0.1986(6) 0.6402(3) 0.071(2) Uani 1 1 d . . . H38 H 0.2160 -0.2100 0.6228 0.085 Uiso 1 1 calc R . . C39 C 0.06492(17) 1.0017(6) 0.5862(4) 0.062(2) Uani 1 1 d . . . C40 C 0.0707(2) 1.0851(8) 0.5525(4) 0.098(3) Uani 1 1 d . . . H40 H 0.0602 1.0894 0.5141 0.118 Uiso 1 1 calc R . . C41 C 0.0919(2) 1.1592(9) 0.5768(5) 0.111(4) Uani 1 1 d . . . H41 H 0.0967 1.2123 0.5547 0.133 Uiso 1 1 calc R . . C42 C 0.1064(2) 1.1561(7) 0.6342(5) 0.097(3) Uani 1 1 d . . . H42 H 0.1206 1.2081 0.6514 0.116 Uiso 1 1 calc R . . C43 C 0.09926(15) 1.0737(6) 0.6659(4) 0.056(2) Uani 1 1 d . . . C44 C 0.11292(15) 1.0663(6) 0.7267(4) 0.058(2) Uani 1 1 d . . . C45 C 0.13117(18) 1.1485(7) 0.7591(5) 0.089(3) Uani 1 1 d . . . H45 H 0.1357 1.2105 0.7417 0.107 Uiso 1 1 calc R . . C46 C 0.1422(2) 1.1368(10) 0.8162(5) 0.104(4) Uani 1 1 d . . . H46 H 0.1539 1.1921 0.8380 0.124 Uiso 1 1 calc R . . C47 C 0.13629(19) 1.0451(9) 0.8413(4) 0.094(3) Uani 1 1 d . . . H47 H 0.1441 1.0350 0.8802 0.113 Uiso 1 1 calc R . . C48 C 0.11834(18) 0.9680(7) 0.8073(4) 0.077(3) Uani 1 1 d . . . H48 H 0.1138 0.9055 0.8243 0.093 Uiso 1 1 calc R . . C49 C 0.04202(16) 0.9207(7) 0.5598(3) 0.058(2) Uani 1 1 d . . . C50 C 0.02275(16) 0.8890(6) 0.5861(3) 0.066(2) Uani 1 1 d . . . H50 H 0.0244 0.9189 0.6212 0.079 Uiso 1 1 calc R . . C51 C 0.00106(18) 0.8138(8) 0.5614(4) 0.090(3) Uani 1 1 d . . . H51 H -0.0119 0.7949 0.5796 0.108 Uiso 1 1 calc R . . C52 C -0.0016(2) 0.7666(9) 0.5101(5) 0.115(4) Uani 1 1 d . . . H52 H -0.0163 0.7161 0.4936 0.138 Uiso 1 1 calc R . . C53 C 0.0176(3) 0.7948(11) 0.4836(5) 0.125(4) Uani 1 1 d . . . H53 H 0.0165 0.7623 0.4494 0.150 Uiso 1 1 calc R . . C54 C 0.0382(2) 0.8708(8) 0.5082(4) 0.093(3) Uani 1 1 d . . . H54 H 0.0507 0.8909 0.4892 0.112 Uiso 1 1 calc R . . C55 C 0.04057(15) 1.0073(7) 0.7510(4) 0.056(2) Uani 1 1 d . . . C56 C 0.04047(16) 1.1873(8) 0.7205(5) 0.077(3) Uani 1 1 d . . . C57 C 0.0363(2) 1.2308(9) 0.7683(5) 0.096(4) Uani 1 1 d . . . H57 H 0.0347 1.3069 0.7726 0.115 Uiso 1 1 calc R . . C58 C 0.03454(18) 1.1596(9) 0.8081(4) 0.092(3) Uani 1 1 d . . . H58 H 0.0324 1.1864 0.8411 0.110 Uiso 1 1 calc R . . C59 C 0.03591(17) 1.0442(9) 0.8000(4) 0.074(3) Uani 1 1 d . . . C60 C 0.03437(18) 0.9629(11) 0.8383(4) 0.095(4) Uani 1 1 d . . . H60 H 0.0322 0.9838 0.8723 0.114 Uiso 1 1 calc R . . C61 C 0.03600(18) 0.8545(9) 0.8268(4) 0.087(3) Uani 1 1 d . . . H61 H 0.0342 0.8007 0.8519 0.104 Uiso 1 1 calc R . . C62 C 0.04046(15) 0.8229(8) 0.7757(4) 0.060(2) Uani 1 1 d . . . C63 C 0.04262(19) 1.2635(7) 0.6747(4) 0.104(3) Uani 1 1 d . . . H63A H 0.0454 1.2204 0.6448 0.156 Uiso 1 1 calc R . . H63B H 0.0587 1.3128 0.6899 0.156 Uiso 1 1 calc R . . H63C H 0.0252 1.3059 0.6600 0.156 Uiso 1 1 calc R . . C64 C 0.03996(15) 0.6712(6) 0.7099(3) 0.070(2) Uani 1 1 d . . . H64A H 0.0239 0.7044 0.6804 0.084 Uiso 1 1 calc R . . H64B H 0.0366 0.5919 0.7096 0.084 Uiso 1 1 calc R . . C65 C 0.0683(2) 0.6307(7) 0.6291(4) 0.087(3) Uani 1 1 d U . . C66 C 0.0830(2) 0.6677(8) 0.5963(4) 0.110(3) Uani 1 1 d U . . H66 H 0.0960 0.7259 0.6091 0.132 Uiso 1 1 calc R . . C67 C 0.0793(3) 0.6206(9) 0.5435(5) 0.127(3) Uani 1 1 d U . . H67 H 0.0899 0.6460 0.5216 0.153 Uiso 1 1 calc R . . C68 C 0.0610(3) 0.5418(11) 0.5256(5) 0.145(4) Uani 1 1 d U . . H68 H 0.0582 0.5140 0.4897 0.174 Uiso 1 1 calc R . . C69 C 0.0454(3) 0.4959(11) 0.5554(6) 0.169(4) Uani 1 1 d U . . H69 H 0.0331 0.4361 0.5416 0.203 Uiso 1 1 calc R . . C70 C 0.0490(3) 0.5457(9) 0.6098(5) 0.141(4) Uani 1 1 d U . . H70 H 0.0383 0.5201 0.6315 0.169 Uiso 1 1 calc R . . C71 C 0.09943(16) 0.6109(6) 0.7459(3) 0.0531(19) Uani 1 1 d . . . C72 C 0.12653(18) 0.6493(7) 0.7714(3) 0.075(3) Uani 1 1 d . . . H72 H 0.1310 0.7211 0.7637 0.090 Uiso 1 1 calc R . . C73 C 0.14770(19) 0.5845(9) 0.8086(4) 0.097(3) Uani 1 1 d . . . H73 H 0.1664 0.6121 0.8237 0.117 Uiso 1 1 calc R . . C74 C 0.1419(3) 0.4829(10) 0.8232(4) 0.100(3) Uani 1 1 d . . . H74 H 0.1562 0.4397 0.8481 0.120 Uiso 1 1 calc R . . C75 C 0.1145(3) 0.4447(8) 0.8006(5) 0.107(4) Uani 1 1 d . . . H75 H 0.1099 0.3752 0.8110 0.129 Uiso 1 1 calc R . . C76 C 0.0935(2) 0.5077(7) 0.7623(4) 0.094(3) Uani 1 1 d . . . H76 H 0.0749 0.4796 0.7472 0.113 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 0.0481(5) 0.0417(5) 0.0530(6) -0.0001(4) 0.0211(4) 0.0035(4) Cu2 0.0504(6) 0.0438(5) 0.0607(6) -0.0004(5) 0.0220(5) -0.0084(5) B1 0.076(8) 0.061(7) 0.101(9) -0.013(7) 0.029(7) 0.007(6) B2 0.078(8) 0.094(8) 0.078(8) 0.029(6) 0.049(7) 0.039(6) F1 0.170(5) 0.089(4) 0.183(6) 0.033(4) 0.043(5) -0.021(4) F2 0.126(9) 0.201(10) 0.168(10) -0.066(8) 0.057(8) 0.056(8) F3 0.139(11) 0.151(9) 0.102(8) -0.051(6) 0.014(7) 0.004(8) F4 0.099(7) 0.090(7) 0.146(10) 0.006(7) 0.005(7) -0.030(6) F5 0.127(9) 0.132(7) 0.109(7) -0.050(6) 0.046(6) -0.027(6) F6 0.098(7) 0.229(11) 0.165(11) 0.007(9) 0.029(7) 0.090(7) F7 0.138(9) 0.121(7) 0.097(7) 0.009(6) 0.080(7) 0.014(6) F2' 0.132(11) 0.112(9) 0.123(11) -0.022(8) 0.080(9) 0.019(9) F3' 0.149(11) 0.106(9) 0.111(9) -0.037(7) 0.070(8) -0.049(9) F4' 0.074(9) 0.110(10) 0.140(12) -0.009(9) 0.020(9) 0.002(7) F5' 0.122(12) 0.125(11) 0.090(11) -0.016(9) -0.015(10) 0.035(9) F6' 0.092(11) 0.153(13) 0.136(14) 0.020(12) 0.031(11) 0.016(10) F7' 0.138(13) 0.182(12) 0.122(11) -0.067(10) 0.047(11) 0.058(11) F8 0.152(5) 0.089(4) 0.129(4) 0.021(3) 0.047(4) -0.002(4) P1 0.0405(11) 0.0368(10) 0.0526(12) 0.0003(10) 0.0196(9) 0.0013(9) P2 0.0588(13) 0.0392(11) 0.0553(13) -0.0024(11) 0.0203(10) -0.0083(10) N1 0.049(4) 0.043(4) 0.055(4) -0.001(3) 0.025(3) -0.017(3) N2 0.053(4) 0.051(4) 0.058(5) 0.000(3) 0.023(4) 0.002(3) N3 0.041(4) 0.050(4) 0.051(4) -0.001(3) 0.023(3) -0.004(3) N4 0.051(4) 0.043(4) 0.076(5) 0.007(4) 0.027(4) -0.008(3) N5 0.054(4) 0.051(4) 0.058(4) -0.011(3) 0.031(3) -0.005(3) N6 0.038(4) 0.051(4) 0.063(5) 0.002(3) 0.018(3) 0.006(3) N7 0.053(4) 0.055(4) 0.059(5) -0.001(4) 0.016(4) -0.003(3) N8 0.046(4) 0.059(5) 0.063(4) -0.007(4) 0.024(3) -0.001(3) N9 0.050(4) 0.051(4) 0.089(5) -0.012(4) 0.023(4) 0.004(3) N10 0.075(5) 0.078(5) 0.082(6) 0.019(5) 0.048(4) -0.008(4) C1 0.045(5) 0.058(5) 0.061(6) -0.011(4) 0.027(5) -0.016(4) C2 0.087(7) 0.078(7) 0.069(6) -0.036(5) 0.040(5) -0.026(5) C3 0.115(9) 0.060(6) 0.122(9) -0.040(7) 0.069(8) -0.007(6) C4 0.086(7) 0.052(6) 0.100(8) -0.008(6) 0.041(6) 0.002(5) C5 0.049(5) 0.035(5) 0.086(7) 0.001(4) 0.037(5) -0.005(4) C6 0.054(5) 0.040(5) 0.064(6) 0.008(4) 0.031(4) 0.001(4) C7 0.080(6) 0.058(6) 0.112(8) 0.019(6) 0.037(6) 0.029(5) C8 0.091(8) 0.104(9) 0.097(9) 0.048(7) 0.025(7) 0.042(7) C9 0.075(7) 0.099(8) 0.073(7) 0.027(7) 0.008(5) 0.012(6) C10 0.084(7) 0.068(6) 0.067(7) 0.010(5) 0.016(6) 0.014(5) C11 0.056(5) 0.072(6) 0.040(5) -0.003(4) 0.021(4) -0.014(4) C12 0.061(6) 0.123(8) 0.058(6) 0.007(6) 0.016(5) -0.007(6) C13 0.081(7) 0.121(9) 0.057(6) 0.018(6) 0.011(6) -0.001(6) C14 0.079(8) 0.087(7) 0.064(6) 0.012(6) -0.009(6) 0.018(5) C15 0.062(6) 0.098(7) 0.060(6) -0.006(6) 0.014(5) 0.006(5) C16 0.058(5) 0.082(6) 0.044(5) 0.002(5) 0.019(4) -0.009(5) C17 0.036(5) 0.055(5) 0.064(6) 0.010(5) 0.021(4) 0.002(4) C18 0.043(5) 0.054(5) 0.077(6) -0.001(5) 0.018(4) -0.009(4) C19 0.062(6) 0.058(6) 0.092(7) 0.027(6) 0.021(6) -0.009(5) C20 0.065(6) 0.079(7) 0.075(7) 0.042(6) 0.021(5) -0.013(5) C21 0.039(5) 0.074(6) 0.060(6) 0.015(5) 0.025(4) -0.004(4) C22 0.069(6) 0.108(8) 0.057(6) 0.025(6) 0.035(5) 0.003(6) C23 0.068(5) 0.078(6) 0.055(5) 0.001(5) 0.039(4) -0.001(5) C24 0.041(4) 0.059(5) 0.051(5) 0.002(4) 0.024(4) -0.010(4) C25 0.088(7) 0.059(6) 0.098(7) -0.010(5) 0.032(6) -0.017(5) C26 0.054(5) 0.029(4) 0.068(5) -0.002(4) 0.023(4) 0.002(3) C27 0.045(5) 0.045(5) 0.060(5) 0.007(4) 0.022(4) 0.001(4) C28 0.055(5) 0.091(7) 0.071(6) -0.020(5) 0.021(5) -0.012(5) C29 0.050(6) 0.135(10) 0.090(7) -0.027(7) 0.011(5) -0.020(6) C30 0.098(9) 0.124(10) 0.084(8) -0.034(7) 0.020(7) -0.052(7) C31 0.127(10) 0.069(7) 0.094(8) -0.023(6) 0.039(8) -0.031(7) C32 0.078(6) 0.049(5) 0.080(6) -0.013(5) 0.024(5) -0.009(5) C33 0.053(5) 0.043(4) 0.061(5) 0.005(4) 0.026(4) 0.004(4) C34 0.099(7) 0.107(8) 0.114(8) 0.061(6) 0.067(6) 0.049(6) C35 0.172(12) 0.139(10) 0.148(11) 0.066(9) 0.125(9) 0.051(9) C36 0.175(13) 0.094(9) 0.124(10) 0.060(7) 0.083(10) 0.029(8) C37 0.108(9) 0.077(7) 0.104(9) 0.035(6) 0.034(7) 0.037(6) C38 0.086(6) 0.067(6) 0.073(6) 0.027(5) 0.044(5) 0.030(5) C39 0.056(6) 0.065(6) 0.074(7) 0.019(5) 0.034(5) 0.003(4) C40 0.080(7) 0.116(9) 0.099(8) 0.048(7) 0.032(6) -0.007(6) C41 0.098(9) 0.119(10) 0.133(10) 0.059(8) 0.061(8) -0.001(7) C42 0.078(7) 0.078(7) 0.142(10) 0.028(7) 0.049(7) -0.026(5) C43 0.043(5) 0.044(5) 0.088(7) 0.005(5) 0.032(5) 0.000(4) C44 0.046(5) 0.048(5) 0.082(7) -0.001(5) 0.024(5) 0.003(4) C45 0.075(7) 0.079(7) 0.127(9) -0.032(7) 0.050(6) -0.044(5) C46 0.067(7) 0.109(9) 0.130(11) -0.064(9) 0.026(7) -0.033(6) C47 0.070(7) 0.117(9) 0.082(7) -0.039(7) 0.006(6) -0.019(6) C48 0.070(6) 0.084(7) 0.075(7) -0.006(6) 0.020(5) -0.011(5) C49 0.048(5) 0.073(6) 0.050(5) 0.010(5) 0.012(4) 0.012(4) C50 0.058(5) 0.079(6) 0.057(5) -0.010(5) 0.012(5) -0.007(5) C51 0.061(6) 0.100(8) 0.099(8) -0.016(6) 0.014(6) -0.022(5) C52 0.092(10) 0.119(9) 0.105(10) -0.052(8) -0.005(8) -0.015(7) C53 0.107(10) 0.168(12) 0.088(9) -0.047(9) 0.015(8) 0.001(9) C54 0.096(8) 0.131(9) 0.056(6) -0.010(6) 0.030(6) 0.011(7) C55 0.037(5) 0.069(6) 0.063(6) -0.011(5) 0.020(4) -0.002(4) C56 0.045(5) 0.070(7) 0.118(9) -0.018(7) 0.029(5) 0.001(5) C57 0.075(7) 0.076(8) 0.119(10) -0.032(7) 0.012(7) 0.022(6) C58 0.063(6) 0.109(9) 0.089(8) -0.054(7) 0.007(6) 0.022(6) C59 0.044(5) 0.109(9) 0.064(7) -0.017(7) 0.014(5) 0.010(5) C60 0.055(6) 0.159(11) 0.077(8) -0.040(8) 0.028(5) -0.002(7) C61 0.078(7) 0.137(10) 0.060(6) 0.005(6) 0.043(5) -0.011(7) C62 0.040(5) 0.074(6) 0.068(6) 0.006(5) 0.022(4) -0.001(4) C63 0.101(8) 0.056(6) 0.149(10) -0.006(6) 0.034(7) 0.007(5) C64 0.066(6) 0.048(5) 0.095(7) 0.000(5) 0.026(5) -0.010(4) C65 0.123(7) 0.060(5) 0.079(6) -0.012(5) 0.037(5) -0.002(5) C66 0.166(8) 0.092(6) 0.083(6) -0.009(5) 0.058(6) 0.035(6) C67 0.179(8) 0.102(7) 0.110(7) 0.005(6) 0.061(6) 0.046(6) C68 0.188(8) 0.135(8) 0.099(7) -0.020(6) 0.032(6) 0.019(7) C69 0.211(9) 0.129(8) 0.145(8) -0.043(7) 0.029(8) -0.020(7) C70 0.192(8) 0.116(7) 0.109(7) -0.041(6) 0.045(7) -0.021(7) C71 0.064(5) 0.043(5) 0.059(5) -0.005(4) 0.031(4) -0.010(4) C72 0.069(6) 0.076(6) 0.080(6) 0.030(5) 0.026(5) 0.011(5) C73 0.068(7) 0.111(8) 0.102(8) 0.023(7) 0.014(6) -0.006(6) C74 0.105(9) 0.113(10) 0.088(8) 0.047(7) 0.041(7) 0.042(8) C75 0.132(10) 0.066(7) 0.124(10) 0.040(7) 0.044(8) 0.009(7) C76 0.084(7) 0.056(6) 0.120(8) 0.025(6) 0.005(6) -0.002(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 Cu1 N2 2.040(6) . ? Cu1 N1 2.055(6) . ? Cu1 P1 2.1623(19) . ? Cu1 N3 2.205(5) . ? Cu2 N7 2.039(6) . ? Cu2 N6 2.070(6) . ? Cu2 P2 2.159(2) . ? Cu2 N8 2.202(6) . ? B1 F4 1.310(11) . ? B1 F3 1.345(11) . ? B1 F2 1.348(11) . ? B1 F4' 1.348(12) . ? B1 F1 1.353(9) . ? B1 F3' 1.357(13) . ? B1 F2' 1.397(12) . ? B2 F6 1.258(11) . ? B2 F7' 1.296(12) . ? B2 F6' 1.348(14) . ? B2 F8 1.367(9) . ? B2 F5 1.378(11) . ? B2 F7 1.382(11) . ? B2 F5' 1.411(13) . ? P1 C33 1.809(7) . ? P1 C27 1.817(7) . ? P1 C26 1.831(7) . ? P2 C65 1.784(9) . ? P2 C71 1.802(7) . ? P2 C64 1.842(8) . ? N1 C1 1.349(8) . ? N1 C5 1.358(8) . ? N2 C10 1.335(8) . ? N2 C6 1.341(8) . ? N3 C24 1.318(8) . ? N3 C17 1.385(8) . ? N4 C17 1.324(8) . ? N4 C18 1.326(8) . ? N5 C24 1.349(8) . ? N5 C26 1.451(8) . ? N5 H5 0.8600 . ? N6 C39 1.326(9) . ? N6 C43 1.364(8) . ? N7 C48 1.321(9) . ? N7 C44 1.333(8) . ? N8 C62 1.334(9) . ? N8 C55 1.374(9) . ? N9 C56 1.323(10) . ? N9 C55 1.343(9) . ? N10 C62 1.331(9) . ? N10 C64 1.430(9) . ? N10 H10 0.8600 . ? C1 C2 1.400(9) . ? C1 C11 1.474(9) . ? C2 C3 1.362(11) . ? C2 H2 0.9300 . ? C3 C4 1.369(11) . ? C3 H3 0.9300 . ? C4 C5 1.383(10) . ? C4 H4 0.9300 . ? C5 C6 1.468(9) . ? C6 C7 1.384(9) . ? C7 C8 1.360(11) . ? C7 H7 0.9300 . ? C8 C9 1.361(11) . ? C8 H8 0.9300 . ? C9 C10 1.368(10) . ? C9 H9 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.382(10) . ? C11 C16 1.388(9) . ? C12 C13 1.356(11) . ? C12 H12 0.9300 . ? C13 C14 1.377(11) . ? C13 H13 0.9300 . ? C14 C15 1.374(11) . ? C14 H14 0.9300 . ? C15 C16 1.379(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C21 1.414(9) . ? C18 C19 1.392(10) . ? C18 C25 1.488(10) . ? C19 C20 1.338(10) . ? C19 H19 0.9300 . ? C20 C21 1.408(10) . ? C20 H20 0.9300 . ? C21 C22 1.402(10) . ? C22 C23 1.345(9) . ? C22 H22 0.9300 . ? C23 C24 1.429(9) . ? C23 H23 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.371(9) . ? C27 C28 1.375(9) . ? C28 C29 1.391(10) . ? C28 H28 0.9300 . ? C29 C30 1.373(11) . ? C29 H29 0.9300 . ? C30 C31 1.370(12) . ? C30 H30 0.9300 . ? C31 C32 1.379(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.351(10) . ? C33 C38 1.362(9) . ? C34 C35 1.404(11) . ? C34 H34 0.9300 . ? C35 C36 1.333(12) . ? C35 H35 0.9300 . ? C36 C37 1.337(12) . ? C36 H36 0.9300 . ? C37 C38 1.378(10) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.406(10) . ? C39 C49 1.471(10) . ? C40 C41 1.352(12) . ? C40 H40 0.9300 . ? C41 C42 1.379(12) . ? C41 H41 0.9300 . ? C42 C43 1.391(10) . ? C42 H42 0.9300 . ? C43 C44 1.450(10) . ? C44 C45 1.399(10) . ? C45 C46 1.360(12) . ? C45 H45 0.9300 . ? C46 C47 1.354(12) . ? C46 H46 0.9300 . ? C47 C48 1.367(10) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.383(10) . ? C49 C54 1.383(10) . ? C50 C51 1.379(10) . ? C50 H50 0.9300 . ? C51 C52 1.375(12) . ? C51 H51 0.9300 . ? C52 C53 1.372(14) . ? C52 H52 0.9300 . ? C53 C54 1.353(13) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C59 1.399(10) . ? C56 C57 1.390(12) . ? C56 C63 1.506(11) . ? C57 C58 1.342(12) . ? C57 H57 0.9300 . ? C58 C59 1.410(12) . ? C58 H58 0.9300 . ? C59 C60 1.395(12) . ? C60 C61 1.347(11) . ? C60 H60 0.9300 . ? C61 C62 1.427(11) . ? C61 H61 0.9300 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.345(12) . ? C65 C70 1.369(12) . ? C66 C67 1.399(12) . ? C66 H66 0.9300 . ? C67 C68 1.281(14) . ? C67 H67 0.9300 . ? C68 C69 1.360(16) . ? C68 H68 0.9300 . ? C69 C70 1.449(15) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.354(9) . ? C71 C76 1.372(9) . ? C72 C73 1.384(10) . ? C72 H72 0.9300 . ? C73 C74 1.336(11) . ? C73 H73 0.9300 . ? C74 C75 1.355(12) . ? C74 H74 0.9300 . ? C75 C76 1.379(11) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? 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 Cu1 N1 80.4(3) . . ? N2 Cu1 P1 130.01(18) . . ? N1 Cu1 P1 133.85(17) . . ? N2 Cu1 N3 95.1(2) . . ? N1 Cu1 N3 117.2(2) . . ? P1 Cu1 N3 96.15(16) . . ? N7 Cu2 N6 80.8(3) . . ? N7 Cu2 P2 130.13(19) . . ? N6 Cu2 P2 133.00(18) . . ? N7 Cu2 N8 97.1(2) . . ? N6 Cu2 N8 117.8(2) . . ? P2 Cu2 N8 95.03(18) . . ? F4 B1 F3 113.6(11) . . ? F4 B1 F2 112.9(10) . . ? F3 B1 F2 109.7(10) . . ? F4 B1 F4' 129.1(11) . . ? F3 B1 F4' 58.3(8) . . ? F2 B1 F4' 51.7(8) . . ? F4 B1 F1 111.8(9) . . ? F3 B1 F1 105.9(9) . . ? F2 B1 F1 102.1(9) . . ? F4' B1 F1 118.7(10) . . ? F4 B1 F3' 40.4(8) . . ? F3 B1 F3' 137.3(12) . . ? F2 B1 F3' 73.1(9) . . ? F4' B1 F3' 107.5(11) . . ? F1 B1 F3' 115.2(11) . . ? F4 B1 F2' 65.1(9) . . ? F3 B1 F2' 54.3(8) . . ? F2 B1 F2' 153.3(11) . . ? F4' B1 F2' 107.2(11) . . ? F1 B1 F2' 103.0(8) . . ? F3' B1 F2' 103.7(11) . . ? F6 B2 F7' 65.3(9) . . ? F6 B2 F6' 127.9(14) . . ? F7' B2 F6' 111.6(13) . . ? F6 B2 F8 115.5(11) . . ? F7' B2 F8 115.3(11) . . ? F6' B2 F8 111.9(11) . . ? F6 B2 F5 113.8(10) . . ? F7' B2 F5 50.3(10) . . ? F6' B2 F5 72.1(12) . . ? F8 B2 F5 104.8(8) . . ? F6 B2 F7 113.1(10) . . ? F7' B2 F7 138.9(13) . . ? F6' B2 F7 34.0(9) . . ? F8 B2 F7 102.4(8) . . ? F5 B2 F7 106.1(9) . . ? F6 B2 F5' 43.1(8) . . ? F7' B2 F5' 108.0(12) . . ? F6' B2 F5' 106.6(12) . . ? F8 B2 F5' 102.6(10) . . ? F5 B2 F5' 150.7(11) . . ? F7 B2 F5' 77.4(11) . . ? C33 P1 C27 102.2(3) . . ? C33 P1 C26 105.3(3) . . ? C27 P1 C26 102.7(3) . . ? C33 P1 Cu1 122.8(2) . . ? C27 P1 Cu1 119.3(2) . . ? C26 P1 Cu1 102.0(2) . . ? C65 P2 C71 104.2(4) . . ? C65 P2 C64 104.7(4) . . ? C71 P2 C64 103.1(3) . . ? C65 P2 Cu2 118.4(3) . . ? C71 P2 Cu2 121.7(2) . . ? C64 P2 Cu2 102.4(3) . . ? C1 N1 C5 118.3(7) . . ? C1 N1 Cu1 128.1(5) . . ? C5 N1 Cu1 113.3(5) . . ? C10 N2 C6 117.3(7) . . ? C10 N2 Cu1 127.8(5) . . ? C6 N2 Cu1 114.4(5) . . ? C24 N3 C17 118.3(6) . . ? C24 N3 Cu1 119.3(4) . . ? C17 N3 Cu1 112.0(4) . . ? C17 N4 C18 119.0(7) . . ? C24 N5 C26 124.3(6) . . ? C24 N5 H5 117.9 . . ? C26 N5 H5 117.9 . . ? C39 N6 C43 118.6(7) . . ? C39 N6 Cu2 129.5(5) . . ? C43 N6 Cu2 111.8(5) . . ? C48 N7 C44 118.8(7) . . ? C48 N7 Cu2 126.9(6) . . ? C44 N7 Cu2 113.8(5) . . ? C62 N8 C55 117.0(7) . . ? C62 N8 Cu2 120.8(5) . . ? C55 N8 Cu2 111.4(5) . . ? C56 N9 C55 119.4(8) . . ? C62 N10 C64 125.9(7) . . ? C62 N10 H10 117.1 . . ? C64 N10 H10 117.1 . . ? N1 C1 C2 121.3(8) . . ? N1 C1 C11 116.8(7) . . ? C2 C1 C11 121.9(8) . . ? C3 C2 C1 119.4(8) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.9(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 119.0(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.1(8) . . ? N1 C5 C6 115.6(7) . . ? C4 C5 C6 122.4(8) . . ? N2 C6 C7 121.0(8) . . ? N2 C6 C5 115.5(7) . . ? C7 C6 C5 123.4(8) . . ? C8 C7 C6 120.2(9) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 119.3(9) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C10 117.8(9) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 124.4(8) . . ? N2 C10 H10A 117.8 . . ? C9 C10 H10A 117.8 . . ? C12 C11 C16 118.0(8) . . ? C12 C11 C1 121.2(8) . . ? C16 C11 C1 120.8(7) . . ? C13 C12 C11 121.9(9) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 120.4(9) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 118.5(8) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 121.4(9) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 119.7(7) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? N4 C17 N3 114.9(7) . . ? N4 C17 C21 122.9(7) . . ? N3 C17 C21 122.2(8) . . ? N4 C18 C19 121.7(8) . . ? N4 C18 C25 118.2(8) . . ? C19 C18 C25 120.2(8) . . ? C20 C19 C18 120.5(8) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.4(8) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 126.8(8) . . ? C22 C21 C17 116.6(8) . . ? C20 C21 C17 116.6(8) . . ? C23 C22 C21 121.7(8) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 118.6(8) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? N3 C24 N5 120.0(7) . . ? N3 C24 C23 122.5(7) . . ? N5 C24 C23 117.6(7) . . ? C18 C25 H25A 109.5 . . ? C18 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C18 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 P1 111.6(4) . . ? N5 C26 H26A 109.3 . . ? P1 C26 H26A 109.3 . . ? N5 C26 H26B 109.3 . . ? P1 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C32 C27 C28 118.7(7) . . ? C32 C27 P1 122.8(6) . . ? C28 C27 P1 118.6(6) . . ? C27 C28 C29 119.8(8) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 120.9(9) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 119.0(9) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 120.0(9) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 121.6(8) . . ? C27 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C34 C33 C38 117.8(7) . . ? C34 C33 P1 117.1(6) . . ? C38 C33 P1 125.1(6) . . ? C33 C34 C35 120.0(8) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.9(10) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.2(10) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C36 C37 C38 120.6(9) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C33 C38 C37 121.2(8) . . ? C33 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? N6 C39 C40 122.0(8) . . ? N6 C39 C49 119.0(7) . . ? C40 C39 C49 119.0(9) . . ? C41 C40 C39 118.9(9) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 120.3(9) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 118.5(9) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? N6 C43 C42 121.5(8) . . ? N6 C43 C44 116.4(7) . . ? C42 C43 C44 122.1(8) . . ? N7 C44 C45 120.0(8) . . ? N7 C44 C43 116.8(7) . . ? C45 C44 C43 123.2(8) . . ? C46 C45 C44 119.4(9) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C47 C46 C45 120.4(10) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 117.3(10) . . ? C46 C47 H47 121.3 . . ? C48 C47 H47 121.3 . . ? N7 C48 C47 124.2(9) . . ? N7 C48 H48 117.9 . . ? C47 C48 H48 117.9 . . ? C50 C49 C54 115.5(8) . . ? C50 C49 C39 120.9(8) . . ? C54 C49 C39 123.6(9) . . ? C51 C50 C49 121.3(8) . . ? C51 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C52 C51 C50 120.5(10) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C53 C52 C51 119.4(10) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C54 C53 C52 118.6(11) . . ? C54 C53 H53 120.7 . . ? C52 C53 H53 120.7 . . ? C53 C54 C49 124.6(10) . . ? C53 C54 H54 117.7 . . ? C49 C54 H54 117.7 . . ? N9 C55 N8 115.2(7) . . ? N9 C55 C59 120.7(9) . . ? N8 C55 C59 124.1(9) . . ? N9 C56 C57 123.5(10) . . ? N9 C56 C63 116.4(9) . . ? C57 C56 C63 120.1(10) . . ? C58 C57 C56 117.9(10) . . ? C58 C57 H57 121.0 . . ? C56 C57 H57 121.0 . . ? C57 C58 C59 120.3(10) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C60 C59 C55 116.7(10) . . ? C60 C59 C58 125.2(11) . . ? C55 C59 C58 118.1(10) . . ? C61 C60 C59 120.8(10) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 119.5(9) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? N10 C62 N8 118.5(8) . . ? N10 C62 C61 119.5(9) . . ? N8 C62 C61 121.9(8) . . ? C56 C63 H63A 109.5 . . ? C56 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C56 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N10 C64 P2 111.8(5) . . ? N10 C64 H64A 109.3 . . ? P2 C64 H64A 109.3 . . ? N10 C64 H64B 109.3 . . ? P2 C64 H64B 109.3 . . ? H64A C64 H64B 107.9 . . ? C66 C65 C70 119.0(10) . . ? C66 C65 P2 118.8(8) . . ? C70 C65 P2 122.1(9) . . ? C65 C66 C67 121.5(11) . . ? C65 C66 H66 119.3 . . ? C67 C66 H66 119.3 . . ? C68 C67 C66 119.0(14) . . ? C68 C67 H67 120.5 . . ? C66 C67 H67 120.5 . . ? C67 C68 C69 124.8(15) . . ? C67 C68 H68 117.6 . . ? C69 C68 H68 117.6 . . ? C68 C69 C70 116.1(13) . . ? C68 C69 H69 122.0 . . ? C70 C69 H69 122.0 . . ? C65 C70 C69 119.6(12) . . ? C65 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C72 C71 C76 116.3(7) . . ? C72 C71 P2 119.2(6) . . ? C76 C71 P2 124.5(6) . . ? C71 C72 C73 121.7(8) . . ? C71 C72 H72 119.2 . . ? C73 C72 H72 119.2 . . ? C74 C73 C72 121.3(9) . . ? C74 C73 H73 119.3 . . ? C72 C73 H73 119.3 . . ? C73 C74 C75 118.2(10) . . ? C73 C74 H74 120.9 . . ? C75 C74 H74 120.9 . . ? C74 C75 C76 120.8(9) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C71 C76 C75 121.6(9) . . ? C71 C76 H76 119.2 . . ? C75 C76 H76 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 P1 C33 -128.5(4) . . . . ? N1 Cu1 P1 C33 -8.2(4) . . . . ? N3 Cu1 P1 C33 129.5(3) . . . . ? N2 Cu1 P1 C27 2.2(4) . . . . ? N1 Cu1 P1 C27 122.4(3) . . . . ? N3 Cu1 P1 C27 -99.8(3) . . . . ? N2 Cu1 P1 C26 114.2(3) . . . . ? N1 Cu1 P1 C26 -125.5(3) . . . . ? N3 Cu1 P1 C26 12.3(3) . . . . ? N7 Cu2 P2 C65 -128.0(5) . . . . ? N6 Cu2 P2 C65 -8.0(5) . . . . ? N8 Cu2 P2 C65 128.3(4) . . . . ? N7 Cu2 P2 C71 3.4(4) . . . . ? N6 Cu2 P2 C71 123.4(4) . . . . ? N8 Cu2 P2 C71 -100.3(3) . . . . ? N7 Cu2 P2 C64 117.5(4) . . . . ? N6 Cu2 P2 C64 -122.4(3) . . . . ? N8 Cu2 P2 C64 13.9(3) . . . . ? N2 Cu1 N1 C1 175.3(6) . . . . ? P1 Cu1 N1 C1 37.5(6) . . . . ? N3 Cu1 N1 C1 -93.8(6) . . . . ? N2 Cu1 N1 C5 2.1(4) . . . . ? P1 Cu1 N1 C5 -135.8(4) . . . . ? N3 Cu1 N1 C5 92.9(5) . . . . ? N1 Cu1 N2 C10 174.6(7) . . . . ? P1 Cu1 N2 C10 -44.5(7) . . . . ? N3 Cu1 N2 C10 57.9(7) . . . . ? N1 Cu1 N2 C6 3.8(5) . . . . ? P1 Cu1 N2 C6 144.6(4) . . . . ? N3 Cu1 N2 C6 -112.9(5) . . . . ? N2 Cu1 N3 C24 -96.3(5) . . . . ? N1 Cu1 N3 C24 -178.1(5) . . . . ? P1 Cu1 N3 C24 34.9(5) . . . . ? N2 Cu1 N3 C17 48.1(5) . . . . ? N1 Cu1 N3 C17 -33.6(5) . . . . ? P1 Cu1 N3 C17 179.4(4) . . . . ? N7 Cu2 N6 C39 179.3(7) . . . . ? P2 Cu2 N6 C39 41.4(7) . . . . ? N8 Cu2 N6 C39 -87.5(7) . . . . ? N7 Cu2 N6 C43 2.1(5) . . . . ? P2 Cu2 N6 C43 -135.8(4) . . . . ? N8 Cu2 N6 C43 95.3(5) . . . . ? N6 Cu2 N7 C48 173.7(7) . . . . ? P2 Cu2 N7 C48 -46.2(8) . . . . ? N8 Cu2 N7 C48 56.5(7) . . . . ? N6 Cu2 N7 C44 2.1(5) . . . . ? P2 Cu2 N7 C44 142.2(4) . . . . ? N8 Cu2 N7 C44 -115.1(5) . . . . ? N7 Cu2 N8 C62 -97.9(6) . . . . ? N6 Cu2 N8 C62 178.8(6) . . . . ? P2 Cu2 N8 C62 33.6(6) . . . . ? N7 Cu2 N8 C55 45.3(5) . . . . ? N6 Cu2 N8 C55 -38.0(6) . . . . ? P2 Cu2 N8 C55 176.8(5) . . . . ? C5 N1 C1 C2 1.6(10) . . . . ? Cu1 N1 C1 C2 -171.4(5) . . . . ? C5 N1 C1 C11 -179.1(6) . . . . ? Cu1 N1 C1 C11 8.0(9) . . . . ? N1 C1 C2 C3 0.4(12) . . . . ? C11 C1 C2 C3 -178.9(7) . . . . ? C1 C2 C3 C4 -2.8(13) . . . . ? C2 C3 C4 C5 3.1(13) . . . . ? C1 N1 C5 C4 -1.2(10) . . . . ? Cu1 N1 C5 C4 172.7(6) . . . . ? C1 N1 C5 C6 178.8(6) . . . . ? Cu1 N1 C5 C6 -7.3(7) . . . . ? C3 C4 C5 N1 -1.1(12) . . . . ? C3 C4 C5 C6 178.9(7) . . . . ? C10 N2 C6 C7 0.7(11) . . . . ? Cu1 N2 C6 C7 172.5(5) . . . . ? C10 N2 C6 C5 179.4(6) . . . . ? Cu1 N2 C6 C5 -8.8(8) . . . . ? N1 C5 C6 N2 10.8(9) . . . . ? C4 C5 C6 N2 -169.2(7) . . . . ? N1 C5 C6 C7 -170.5(7) . . . . ? C4 C5 C6 C7 9.4(11) . . . . ? N2 C6 C7 C8 0.8(12) . . . . ? C5 C6 C7 C8 -177.8(8) . . . . ? C6 C7 C8 C9 -1.0(14) . . . . ? C7 C8 C9 C10 -0.3(15) . . . . ? C6 N2 C10 C9 -2.1(12) . . . . ? Cu1 N2 C10 C9 -172.7(6) . . . . ? C8 C9 C10 N2 1.9(14) . . . . ? N1 C1 C11 C12 -137.6(7) . . . . ? C2 C1 C11 C12 41.8(10) . . . . ? N1 C1 C11 C16 43.6(9) . . . . ? C2 C1 C11 C16 -137.0(8) . . . . ? C16 C11 C12 C13 -1.1(12) . . . . ? C1 C11 C12 C13 -180.0(8) . . . . ? C11 C12 C13 C14 -0.9(14) . . . . ? C12 C13 C14 C15 2.9(14) . . . . ? C13 C14 C15 C16 -2.8(13) . . . . ? C14 C15 C16 C11 0.8(12) . . . . ? C12 C11 C16 C15 1.2(11) . . . . ? C1 C11 C16 C15 -179.9(6) . . . . ? C18 N4 C17 N3 -179.4(6) . . . . ? C18 N4 C17 C21 -1.6(11) . . . . ? C24 N3 C17 N4 -177.9(6) . . . . ? Cu1 N3 C17 N4 37.3(7) . . . . ? C24 N3 C17 C21 4.3(10) . . . . ? Cu1 N3 C17 C21 -140.5(6) . . . . ? C17 N4 C18 C19 1.2(11) . . . . ? C17 N4 C18 C25 -179.0(7) . . . . ? N4 C18 C19 C20 -0.8(12) . . . . ? C25 C18 C19 C20 179.5(7) . . . . ? C18 C19 C20 C21 0.7(13) . . . . ? C19 C20 C21 C22 -179.2(8) . . . . ? C19 C20 C21 C17 -0.9(11) . . . . ? N4 C17 C21 C22 179.9(7) . . . . ? N3 C17 C21 C22 -2.5(10) . . . . ? N4 C17 C21 C20 1.4(11) . . . . ? N3 C17 C21 C20 179.1(6) . . . . ? C20 C21 C22 C23 178.8(7) . . . . ? C17 C21 C22 C23 0.6(12) . . . . ? C21 C22 C23 C24 -0.4(12) . . . . ? C17 N3 C24 N5 175.5(6) . . . . ? Cu1 N3 C24 N5 -42.3(8) . . . . ? C17 N3 C24 C23 -4.1(10) . . . . ? Cu1 N3 C24 C23 138.1(6) . . . . ? C26 N5 C24 N3 -13.9(10) . . . . ? C26 N5 C24 C23 165.7(6) . . . . ? C22 C23 C24 N3 2.2(11) . . . . ? C22 C23 C24 N5 -177.3(7) . . . . ? C24 N5 C26 P1 73.5(7) . . . . ? C33 P1 C26 N5 173.1(4) . . . . ? C27 P1 C26 N5 66.4(5) . . . . ? Cu1 P1 C26 N5 -57.7(5) . . . . ? C33 P1 C27 C32 -67.2(7) . . . . ? C26 P1 C27 C32 41.8(7) . . . . ? Cu1 P1 C27 C32 153.5(5) . . . . ? C33 P1 C27 C28 112.8(6) . . . . ? C26 P1 C27 C28 -138.2(6) . . . . ? Cu1 P1 C27 C28 -26.5(7) . . . . ? C32 C27 C28 C29 0.3(12) . . . . ? P1 C27 C28 C29 -179.7(6) . . . . ? C27 C28 C29 C30 0.5(14) . . . . ? C28 C29 C30 C31 -1.0(16) . . . . ? C29 C30 C31 C32 0.8(16) . . . . ? C28 C27 C32 C31 -0.5(12) . . . . ? P1 C27 C32 C31 179.5(7) . . . . ? C30 C31 C32 C27 0.0(14) . . . . ? C27 P1 C33 C34 -83.3(7) . . . . ? C26 P1 C33 C34 169.7(7) . . . . ? Cu1 P1 C33 C34 54.1(7) . . . . ? C27 P1 C33 C38 98.9(7) . . . . ? C26 P1 C33 C38 -8.1(7) . . . . ? Cu1 P1 C33 C38 -123.7(6) . . . . ? C38 C33 C34 C35 -3.7(14) . . . . ? P1 C33 C34 C35 178.3(8) . . . . ? C33 C34 C35 C36 0.7(18) . . . . ? C34 C35 C36 C37 2.1(19) . . . . ? C35 C36 C37 C38 -1.6(18) . . . . ? C34 C33 C38 C37 4.2(12) . . . . ? P1 C33 C38 C37 -178.1(7) . . . . ? C36 C37 C38 C33 -1.6(15) . . . . ? C43 N6 C39 C40 1.6(11) . . . . ? Cu2 N6 C39 C40 -175.5(6) . . . . ? C43 N6 C39 C49 -176.9(6) . . . . ? Cu2 N6 C39 C49 6.0(10) . . . . ? N6 C39 C40 C41 1.8(14) . . . . ? C49 C39 C40 C41 -179.7(9) . . . . ? C39 C40 C41 C42 -3.5(16) . . . . ? C40 C41 C42 C43 1.8(16) . . . . ? C39 N6 C43 C42 -3.4(11) . . . . ? Cu2 N6 C43 C42 174.2(6) . . . . ? C39 N6 C43 C44 176.8(6) . . . . ? Cu2 N6 C43 C44 -5.7(8) . . . . ? C41 C42 C43 N6 1.7(13) . . . . ? C41 C42 C43 C44 -178.4(8) . . . . ? C48 N7 C44 C45 0.9(11) . . . . ? Cu2 N7 C44 C45 173.3(6) . . . . ? C48 N7 C44 C43 -178.1(7) . . . . ? Cu2 N7 C44 C43 -5.7(8) . . . . ? N6 C43 C44 N7 7.8(10) . . . . ? C42 C43 C44 N7 -172.1(7) . . . . ? N6 C43 C44 C45 -171.2(7) . . . . ? C42 C43 C44 C45 8.9(12) . . . . ? N7 C44 C45 C46 -1.4(13) . . . . ? C43 C44 C45 C46 177.5(8) . . . . ? C44 C45 C46 C47 1.9(15) . . . . ? C45 C46 C47 C48 -1.8(15) . . . . ? C44 N7 C48 C47 -0.9(13) . . . . ? Cu2 N7 C48 C47 -172.1(6) . . . . ? C46 C47 C48 N7 1.3(14) . . . . ? N6 C39 C49 C50 41.4(10) . . . . ? C40 C39 C49 C50 -137.2(8) . . . . ? N6 C39 C49 C54 -138.2(8) . . . . ? C40 C39 C49 C54 43.2(12) . . . . ? C54 C49 C50 C51 -1.0(11) . . . . ? C39 C49 C50 C51 179.4(7) . . . . ? C49 C50 C51 C52 1.3(13) . . . . ? C50 C51 C52 C53 0.1(16) . . . . ? C51 C52 C53 C54 -1.7(18) . . . . ? C52 C53 C54 C49 2.1(18) . . . . ? C50 C49 C54 C53 -0.7(13) . . . . ? C39 C49 C54 C53 178.9(9) . . . . ? C56 N9 C55 N8 -178.5(6) . . . . ? C56 N9 C55 C59 1.6(11) . . . . ? C62 N8 C55 N9 -176.9(6) . . . . ? Cu2 N8 C55 N9 38.4(7) . . . . ? C62 N8 C55 C59 3.1(10) . . . . ? Cu2 N8 C55 C59 -141.6(6) . . . . ? C55 N9 C56 C57 -0.7(12) . . . . ? C55 N9 C56 C63 -179.8(7) . . . . ? N9 C56 C57 C58 1.1(14) . . . . ? C63 C56 C57 C58 -179.9(9) . . . . ? C56 C57 C58 C59 -2.4(15) . . . . ? N9 C55 C59 C60 -179.8(7) . . . . ? N8 C55 C59 C60 0.2(12) . . . . ? N9 C55 C59 C58 -2.8(11) . . . . ? N8 C55 C59 C58 177.2(7) . . . . ? C57 C58 C59 C60 180.0(9) . . . . ? C57 C58 C59 C55 3.2(13) . . . . ? C55 C59 C60 C61 -3.0(13) . . . . ? C58 C59 C60 C61 -179.7(8) . . . . ? C59 C60 C61 C62 2.4(14) . . . . ? C64 N10 C62 N8 -11.6(11) . . . . ? C64 N10 C62 C61 167.4(7) . . . . ? C55 N8 C62 N10 175.3(6) . . . . ? Cu2 N8 C62 N10 -43.5(9) . . . . ? C55 N8 C62 C61 -3.7(11) . . . . ? Cu2 N8 C62 C61 137.5(6) . . . . ? C60 C61 C62 N10 -177.9(8) . . . . ? C60 C61 C62 N8 1.1(13) . . . . ? C62 N10 C64 P2 71.3(9) . . . . ? C65 P2 C64 N10 177.4(6) . . . . ? C71 P2 C64 N10 68.7(6) . . . . ? Cu2 P2 C64 N10 -58.5(6) . . . . ? C71 P2 C65 C66 -97.3(8) . . . . ? C64 P2 C65 C66 154.7(8) . . . . ? Cu2 P2 C65 C66 41.6(9) . . . . ? C71 P2 C65 C70 85.0(9) . . . . ? C64 P2 C65 C70 -23.0(9) . . . . ? Cu2 P2 C65 C70 -136.2(8) . . . . ? C70 C65 C66 C67 -0.6(16) . . . . ? P2 C65 C66 C67 -178.4(7) . . . . ? C65 C66 C67 C68 1.3(17) . . . . ? C66 C67 C68 C69 -3(2) . . . . ? C67 C68 C69 C70 4(2) . . . . ? C66 C65 C70 C69 1.4(16) . . . . ? P2 C65 C70 C69 179.1(8) . . . . ? C68 C69 C70 C65 -2.7(19) . . . . ? C65 P2 C71 C72 109.7(7) . . . . ? C64 P2 C71 C72 -141.2(7) . . . . ? Cu2 P2 C71 C72 -27.4(7) . . . . ? C65 P2 C71 C76 -72.0(8) . . . . ? C64 P2 C71 C76 37.1(8) . . . . ? Cu2 P2 C71 C76 150.9(6) . . . . ? C76 C71 C72 C73 4.9(12) . . . . ? P2 C71 C72 C73 -176.7(7) . . . . ? C71 C72 C73 C74 -3.5(15) . . . . ? C72 C73 C74 C75 0.0(17) . . . . ? C73 C74 C75 C76 1.9(18) . . . . ? C72 C71 C76 C75 -3.1(13) . . . . ? P2 C71 C76 C75 178.6(7) . . . . ? C74 C75 C76 C71 -0.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.508 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.070 # Attachment 'complex 4.cif' data_060926a _database_code_depnum_ccdc_archive 'CCDC 666205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H44 Cl6 N6 P2 Pt' _chemical_formula_weight 1150.60 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 16.299(13) _cell_length_b 16.892(14) _cell_length_c 19.458(16) _cell_angle_alpha 90.00 _cell_angle_beta 113.498(9) _cell_angle_gamma 90.00 _cell_volume 4913(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7477 _cell_measurement_theta_min 2.458 _cell_measurement_theta_max 27.289 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 3.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3532 _exptl_absorpt_correction_T_max 0.3926 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 30802 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.80 _reflns_number_total 11678 _reflns_number_gt 7363 _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^)+(0.0423P)^2^+4.5310P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11678 _refine_ls_number_parameters 550 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _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 Pt1 Pt 1.490170(14) 0.507093(11) 0.258427(10) 0.03127(7) Uani 1 1 d . . . Cl1 Cl 1.27147(13) 0.48690(12) 0.39169(9) 0.0714(5) Uani 1 1 d . . . Cl2 Cl 1.36953(11) 0.61192(10) 0.90699(9) 0.0576(4) Uani 1 1 d . . . Cl3 Cl 1.0199(2) 0.4554(2) 0.3652(2) 0.1417(11) Uani 1 1 d DU . . Cl4 Cl 1.0866(2) 0.4096(3) 0.5198(2) 0.1735(15) Uani 1 1 d DU . . Cl5 Cl 1.1211(4) 0.4875(4) 0.8416(4) 0.271(3) Uani 1 1 d DU . . Cl6 Cl 1.1322(3) 0.6163(3) 0.9414(3) 0.236(2) Uani 1 1 d DU . . N1 N 1.5975(3) 0.5806(3) 0.3292(2) 0.0372(11) Uani 1 1 d . . . N2 N 1.6171(3) 0.6000(3) 0.2190(2) 0.0405(11) Uani 1 1 d . . . N3 N 1.5991(3) 0.5476(3) 0.4467(2) 0.0462(13) Uani 1 1 d . . . H3 H 1.6159 0.5633 0.4924 0.055 Uiso 1 1 calc R . . N4 N 1.4237(3) 0.6038(2) 0.1885(2) 0.0353(11) Uani 1 1 d . . . N5 N 1.4197(3) 0.6507(3) 0.2991(2) 0.0386(11) Uani 1 1 d . . . N6 N 1.4052(3) 0.5522(3) 0.0715(2) 0.0433(12) Uani 1 1 d . . . H6 H 1.3965 0.5650 0.0264 0.052 Uiso 1 1 calc R . . P1 P 1.54893(10) 0.41909(8) 0.34885(8) 0.0347(3) Uani 1 1 d . . . P2 P 1.39279(10) 0.43577(8) 0.16757(7) 0.0332(3) Uani 1 1 d . . . C1 C 1.6406(4) 0.6220(3) 0.2909(3) 0.0386(13) Uani 1 1 d . . . C2 C 1.6583(4) 0.6354(4) 0.1807(3) 0.0505(16) Uani 1 1 d . . . C3 C 1.7235(5) 0.6940(4) 0.2116(4) 0.063(2) Uani 1 1 d . . . H3A H 1.7520 0.7162 0.1833 0.076 Uiso 1 1 calc R . . C4 C 1.7446(4) 0.7178(4) 0.2831(4) 0.0589(19) Uani 1 1 d . . . H4 H 1.7862 0.7579 0.3040 0.071 Uiso 1 1 calc R . . C5 C 1.7032(4) 0.6816(4) 0.3249(3) 0.0467(15) Uani 1 1 d . . . C6 C 1.7221(4) 0.6995(4) 0.4010(4) 0.0559(18) Uani 1 1 d . . . H6A H 1.7595 0.7417 0.4243 0.067 Uiso 1 1 calc R . . C7 C 1.6865(4) 0.6561(4) 0.4391(3) 0.0521(17) Uani 1 1 d . . . H7 H 1.7012 0.6667 0.4895 0.063 Uiso 1 1 calc R . . C8 C 1.6255(4) 0.5928(3) 0.4029(3) 0.0397(14) Uani 1 1 d . . . C9 C 1.6300(5) 0.6107(4) 0.0993(3) 0.0616(19) Uani 1 1 d . . . H9A H 1.6357 0.5543 0.0967 0.092 Uiso 1 1 calc R . . H9B H 1.6676 0.6363 0.0786 0.092 Uiso 1 1 calc R . . H9C H 1.5689 0.6258 0.0713 0.092 Uiso 1 1 calc R . . C10 C 1.5463(4) 0.4763(3) 0.4281(3) 0.0446(15) Uani 1 1 d . . . H10A H 1.4847 0.4903 0.4171 0.054 Uiso 1 1 calc R . . H10B H 1.5667 0.4423 0.4719 0.054 Uiso 1 1 calc R . . C11 C 1.6645(4) 0.3921(3) 0.3714(3) 0.0407(14) Uani 1 1 d . . . C12 C 1.7012(4) 0.4077(4) 0.3197(4) 0.0551(17) Uani 1 1 d . . . H12 H 1.6664 0.4301 0.2736 0.066 Uiso 1 1 calc R . . C13 C 1.7899(5) 0.3896(5) 0.3375(5) 0.076(2) Uani 1 1 d . . . H13 H 1.8151 0.4005 0.3033 0.092 Uiso 1 1 calc R . . C14 C 1.8409(5) 0.3559(5) 0.4045(5) 0.083(3) Uani 1 1 d . . . H14 H 1.9005 0.3439 0.4157 0.100 Uiso 1 1 calc R . . C15 C 1.8056(5) 0.3398(5) 0.4549(4) 0.079(2) Uani 1 1 d . . . H15 H 1.8409 0.3159 0.5001 0.095 Uiso 1 1 calc R . . C16 C 1.7168(5) 0.3584(4) 0.4401(4) 0.0630(19) Uani 1 1 d . . . H16 H 1.6931 0.3484 0.4755 0.076 Uiso 1 1 calc R . . C17 C 1.4895(4) 0.3311(3) 0.3559(3) 0.0384(13) Uani 1 1 d . . . C18 C 1.4073(4) 0.3404(4) 0.3607(3) 0.0515(16) Uani 1 1 d . . . H18 H 1.3817 0.3904 0.3556 0.062 Uiso 1 1 calc R . . C19 C 1.3637(5) 0.2755(5) 0.3731(4) 0.064(2) Uani 1 1 d . . . H19 H 1.3099 0.2821 0.3784 0.076 Uiso 1 1 calc R . . C20 C 1.3992(6) 0.2017(5) 0.3777(4) 0.081(3) Uani 1 1 d . . . H20 H 1.3693 0.1582 0.3858 0.097 Uiso 1 1 calc R . . C21 C 1.4795(6) 0.1910(4) 0.3704(4) 0.072(2) Uani 1 1 d . . . H21 H 1.5027 0.1404 0.3725 0.087 Uiso 1 1 calc R . . C22 C 1.5251(4) 0.2560(4) 0.3599(3) 0.0532(17) Uani 1 1 d . . . H22 H 1.5795 0.2491 0.3555 0.064 Uiso 1 1 calc R . . C23 C 1.4108(4) 0.6669(3) 0.2285(3) 0.0370(13) Uani 1 1 d . . . C24 C 1.4091(4) 0.7087(4) 0.3405(3) 0.0472(15) Uani 1 1 d . . . C25 C 1.3884(5) 0.7859(4) 0.3125(4) 0.0584(18) Uani 1 1 d . . . H25 H 1.3820 0.8257 0.3430 0.070 Uiso 1 1 calc R . . C26 C 1.3776(5) 0.8032(4) 0.2408(4) 0.0581(18) Uani 1 1 d . . . H26 H 1.3631 0.8543 0.2220 0.070 Uiso 1 1 calc R . . C27 C 1.3886(4) 0.7427(3) 0.1964(3) 0.0446(15) Uani 1 1 d . . . C28 C 1.3790(4) 0.7517(4) 0.1205(4) 0.0570(18) Uani 1 1 d . . . H28 H 1.3676 0.8014 0.0982 0.068 Uiso 1 1 calc R . . C29 C 1.3861(4) 0.6898(4) 0.0817(3) 0.0501(16) Uani 1 1 d . . . H29 H 1.3779 0.6961 0.0319 0.060 Uiso 1 1 calc R . . C30 C 1.4065(4) 0.6129(3) 0.1157(3) 0.0374(13) Uani 1 1 d . . . C31 C 1.4190(5) 0.6883(4) 0.4179(4) 0.066(2) Uani 1 1 d . . . H31A H 1.3808 0.6443 0.4160 0.099 Uiso 1 1 calc R . . H31B H 1.4025 0.7331 0.4400 0.099 Uiso 1 1 calc R . . H31C H 1.4801 0.6743 0.4476 0.099 Uiso 1 1 calc R . . C32 C 1.4159(4) 0.4684(3) 0.0874(3) 0.0401(14) Uani 1 1 d . . . H32A H 1.4769 0.4538 0.0962 0.048 Uiso 1 1 calc R . . H32B H 1.3765 0.4400 0.0433 0.048 Uiso 1 1 calc R . . C33 C 1.4033(4) 0.3293(3) 0.1661(3) 0.0353(13) Uani 1 1 d . . . C34 C 1.4785(4) 0.2958(4) 0.1624(4) 0.0524(16) Uani 1 1 d . . . H34 H 1.5235 0.3279 0.1597 0.063 Uiso 1 1 calc R . . C35 C 1.4872(5) 0.2138(4) 0.1625(4) 0.069(2) Uani 1 1 d . . . H35 H 1.5374 0.1914 0.1588 0.083 Uiso 1 1 calc R . . C36 C 1.4225(6) 0.1660(4) 0.1681(4) 0.071(2) Uani 1 1 d . . . H36 H 1.4290 0.1113 0.1684 0.085 Uiso 1 1 calc R . . C37 C 1.3483(5) 0.1984(4) 0.1732(4) 0.068(2) Uani 1 1 d . . . H37 H 1.3049 0.1657 0.1779 0.082 Uiso 1 1 calc R . . C38 C 1.3374(4) 0.2800(4) 0.1715(3) 0.0514(16) Uani 1 1 d . . . H38 H 1.2862 0.3018 0.1739 0.062 Uiso 1 1 calc R . . C39 C 1.2765(4) 0.4563(3) 0.1459(3) 0.0359(13) Uani 1 1 d . . . C40 C 1.2517(4) 0.4871(3) 0.2001(3) 0.0433(14) Uani 1 1 d . . . H40 H 1.2952 0.4997 0.2471 0.052 Uiso 1 1 calc R . . C41 C 1.1616(4) 0.4998(4) 0.1852(4) 0.0544(16) Uani 1 1 d . . . H41 H 1.1454 0.5202 0.2224 0.065 Uiso 1 1 calc R . . C42 C 1.0978(5) 0.4826(4) 0.1171(4) 0.0587(19) Uani 1 1 d . . . H42 H 1.0380 0.4915 0.1075 0.070 Uiso 1 1 calc R . . C43 C 1.1210(5) 0.4521(4) 0.0616(4) 0.0634(19) Uani 1 1 d . . . H43 H 1.0768 0.4409 0.0147 0.076 Uiso 1 1 calc R . . C44 C 1.2097(4) 0.4382(4) 0.0756(3) 0.0534(17) Uani 1 1 d . . . H44 H 1.2252 0.4168 0.0384 0.064 Uiso 1 1 calc R . . C45 C 1.0965(8) 0.4751(7) 0.4546(6) 0.136(4) Uani 1 1 d DU . . H45A H 1.0877 0.5288 0.4681 0.163 Uiso 1 1 calc R . . H45B H 1.1564 0.4715 0.4557 0.163 Uiso 1 1 calc R . . C46 C 1.1229(10) 0.5965(7) 0.8481(7) 0.192(6) Uani 1 1 d DU . . H46A H 1.1736 0.6181 0.8403 0.230 Uiso 1 1 calc R . . H46B H 1.0683 0.6190 0.8114 0.230 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 Pt1 0.04120(13) 0.02403(11) 0.02703(10) 0.00040(9) 0.01199(8) -0.00143(10) Cl1 0.0748(12) 0.0947(15) 0.0394(8) 0.0039(9) 0.0174(8) 0.0227(11) Cl2 0.0709(11) 0.0612(11) 0.0495(9) 0.0156(8) 0.0334(9) 0.0129(9) Cl3 0.118(2) 0.115(2) 0.197(3) 0.017(2) 0.069(2) -0.0161(19) Cl4 0.122(2) 0.233(4) 0.165(3) 0.010(3) 0.057(2) 0.060(3) Cl5 0.197(5) 0.355(8) 0.299(7) -0.087(6) 0.139(5) -0.104(5) Cl6 0.202(4) 0.239(5) 0.268(5) 0.041(4) 0.095(4) -0.082(4) N1 0.039(3) 0.026(2) 0.039(2) -0.003(2) 0.008(2) -0.002(2) N2 0.050(3) 0.031(3) 0.042(3) -0.003(2) 0.021(2) -0.008(2) N3 0.073(4) 0.040(3) 0.024(2) -0.008(2) 0.017(2) -0.012(3) N4 0.051(3) 0.024(2) 0.034(2) 0.006(2) 0.021(2) 0.006(2) N5 0.050(3) 0.028(2) 0.040(3) -0.002(2) 0.020(2) 0.005(2) N6 0.071(4) 0.033(3) 0.028(2) 0.002(2) 0.022(2) -0.001(2) P1 0.0448(9) 0.0269(7) 0.0315(7) 0.0027(6) 0.0142(7) 0.0018(6) P2 0.0436(9) 0.0261(7) 0.0288(7) -0.0015(6) 0.0134(6) -0.0035(6) C1 0.041(3) 0.028(3) 0.041(3) 0.002(3) 0.011(3) 0.002(3) C2 0.066(4) 0.040(3) 0.049(4) 0.000(3) 0.026(3) -0.008(3) C3 0.076(5) 0.058(4) 0.061(4) 0.000(4) 0.034(4) -0.024(4) C4 0.067(5) 0.051(4) 0.058(4) -0.009(3) 0.023(4) -0.031(3) C5 0.051(4) 0.036(3) 0.050(4) -0.003(3) 0.017(3) -0.011(3) C6 0.067(5) 0.042(4) 0.052(4) -0.011(3) 0.016(4) -0.019(3) C7 0.067(5) 0.047(4) 0.034(3) -0.013(3) 0.011(3) -0.009(3) C8 0.047(4) 0.032(3) 0.037(3) -0.002(3) 0.013(3) 0.002(3) C9 0.079(5) 0.072(5) 0.046(4) -0.012(3) 0.038(4) -0.023(4) C10 0.067(4) 0.035(3) 0.036(3) -0.001(3) 0.025(3) -0.004(3) C11 0.044(4) 0.032(3) 0.045(3) 0.001(3) 0.016(3) 0.003(3) C12 0.059(4) 0.050(4) 0.061(4) 0.002(3) 0.030(4) 0.004(3) C13 0.068(5) 0.073(6) 0.102(7) 0.002(5) 0.048(5) 0.000(4) C14 0.044(5) 0.089(7) 0.110(7) -0.010(6) 0.023(5) 0.003(4) C15 0.058(5) 0.080(6) 0.069(5) -0.006(5) -0.007(4) 0.010(4) C16 0.061(5) 0.066(5) 0.050(4) -0.002(4) 0.010(4) 0.007(4) C17 0.052(4) 0.031(3) 0.032(3) 0.006(2) 0.016(3) -0.002(3) C18 0.056(4) 0.045(4) 0.058(4) 0.004(3) 0.027(3) -0.004(3) C19 0.069(5) 0.068(5) 0.066(5) -0.007(4) 0.040(4) -0.020(4) C20 0.113(7) 0.053(5) 0.087(6) 0.000(4) 0.051(6) -0.038(5) C21 0.104(7) 0.034(4) 0.082(5) 0.001(4) 0.040(5) -0.007(4) C22 0.065(4) 0.033(3) 0.065(4) 0.008(3) 0.028(4) 0.000(3) C23 0.041(3) 0.027(3) 0.039(3) -0.002(2) 0.012(3) 0.001(2) C24 0.052(4) 0.037(3) 0.053(4) -0.007(3) 0.021(3) 0.003(3) C25 0.077(5) 0.041(4) 0.064(4) -0.007(3) 0.034(4) 0.008(3) C26 0.077(5) 0.030(3) 0.064(4) 0.002(3) 0.024(4) 0.004(3) C27 0.052(4) 0.030(3) 0.050(3) 0.007(3) 0.018(3) 0.009(3) C28 0.079(5) 0.031(3) 0.057(4) 0.013(3) 0.023(4) 0.005(3) C29 0.070(4) 0.037(3) 0.040(3) 0.013(3) 0.018(3) 0.008(3) C30 0.044(3) 0.032(3) 0.037(3) 0.005(3) 0.016(3) -0.002(3) C31 0.091(6) 0.060(5) 0.056(4) -0.009(4) 0.038(4) 0.014(4) C32 0.058(4) 0.032(3) 0.037(3) 0.001(2) 0.026(3) 0.002(3) C33 0.045(3) 0.027(3) 0.033(3) -0.004(2) 0.014(3) -0.005(2) C34 0.059(4) 0.042(4) 0.063(4) 0.004(3) 0.031(4) 0.006(3) C35 0.087(6) 0.051(4) 0.080(5) 0.001(4) 0.045(5) 0.025(4) C36 0.103(7) 0.030(4) 0.079(5) -0.003(4) 0.036(5) 0.002(4) C37 0.080(5) 0.036(4) 0.078(5) 0.002(4) 0.020(4) -0.017(4) C38 0.055(4) 0.038(3) 0.059(4) 0.004(3) 0.020(3) -0.003(3) C39 0.042(3) 0.026(3) 0.036(3) 0.003(2) 0.012(3) -0.002(2) C40 0.048(4) 0.036(3) 0.045(3) 0.000(3) 0.018(3) 0.003(3) C41 0.057(4) 0.043(4) 0.067(4) 0.006(3) 0.029(4) 0.007(3) C42 0.047(4) 0.039(4) 0.085(5) 0.022(4) 0.022(4) 0.008(3) C43 0.052(4) 0.060(5) 0.057(4) 0.005(4) -0.001(4) -0.002(4) C44 0.054(4) 0.059(4) 0.040(3) 0.000(3) 0.011(3) -0.001(3) C45 0.132(9) 0.142(10) 0.157(10) -0.058(8) 0.083(8) -0.045(8) C46 0.272(14) 0.196(13) 0.171(11) -0.041(10) 0.155(11) -0.143(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 Pt1 N4 2.126(4) . ? Pt1 N1 2.139(4) . ? Pt1 P2 2.2042(17) . ? Pt1 P1 2.2089(18) . ? Cl3 C45 1.721(10) . ? Cl4 C45 1.739(10) . ? Cl5 C46 1.844(12) . ? Cl6 C46 1.791(10) . ? N1 C8 1.337(7) . ? N1 C1 1.399(7) . ? N2 C2 1.328(7) . ? N2 C1 1.346(7) . ? N3 C8 1.337(7) . ? N3 C10 1.440(7) . ? N3 H3 0.8600 . ? N4 C30 1.339(6) . ? N4 C23 1.386(6) . ? N5 C24 1.322(7) . ? N5 C23 1.350(7) . ? N6 C30 1.333(7) . ? N6 C32 1.444(7) . ? N6 H6 0.8600 . ? P1 C17 1.809(6) . ? P1 C11 1.814(6) . ? P1 C10 1.835(6) . ? P2 C39 1.804(6) . ? P2 C33 1.808(6) . ? P2 C32 1.831(5) . ? C1 C5 1.398(8) . ? C2 C3 1.400(8) . ? C2 C9 1.520(8) . ? C3 C4 1.356(9) . ? C3 H3A 0.9300 . ? C4 C5 1.388(8) . ? C4 H4 0.9300 . ? C5 C6 1.420(8) . ? C6 C7 1.328(8) . ? C6 H6A 0.9300 . ? C7 C8 1.438(8) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.384(8) . ? C11 C16 1.390(8) . ? C12 C13 1.380(9) . ? C12 H12 0.9300 . ? C13 C14 1.360(10) . ? C13 H13 0.9300 . ? C14 C15 1.347(10) . ? C14 H14 0.9300 . ? C15 C16 1.394(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.384(8) . ? C17 C18 1.389(8) . ? C18 C19 1.379(9) . ? C18 H18 0.9300 . ? C19 C20 1.362(10) . ? C19 H19 0.9300 . ? C20 C21 1.383(10) . ? C20 H20 0.9300 . ? C21 C22 1.386(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C27 1.408(7) . ? C24 C25 1.402(8) . ? C24 C31 1.490(8) . ? C25 C26 1.365(9) . ? C25 H25 0.9300 . ? C26 C27 1.396(8) . ? C26 H26 0.9300 . ? C27 C28 1.430(8) . ? C28 C29 1.321(8) . ? C28 H28 0.9300 . ? C29 C30 1.435(7) . ? C29 H29 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.380(8) . ? C33 C38 1.395(8) . ? C34 C35 1.391(9) . ? C34 H34 0.9300 . ? C35 C36 1.367(10) . ? C35 H35 0.9300 . ? C36 C37 1.367(10) . ? C36 H36 0.9300 . ? C37 C38 1.388(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.374(8) . ? C39 C44 1.401(7) . ? C40 C41 1.395(8) . ? C40 H40 0.9300 . ? C41 C42 1.350(9) . ? C41 H41 0.9300 . ? C42 C43 1.377(10) . ? C42 H42 0.9300 . ? C43 C44 1.381(9) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? 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 N4 Pt1 N1 92.49(18) . . ? N4 Pt1 P2 83.48(14) . . ? N1 Pt1 P2 167.42(13) . . ? N4 Pt1 P1 167.32(12) . . ? N1 Pt1 P1 83.92(14) . . ? P2 Pt1 P1 102.47(8) . . ? C8 N1 C1 117.7(5) . . ? C8 N1 Pt1 128.5(4) . . ? C1 N1 Pt1 113.7(3) . . ? C2 N2 C1 117.5(5) . . ? C8 N3 C10 129.0(4) . . ? C8 N3 H3 115.5 . . ? C10 N3 H3 115.5 . . ? C30 N4 C23 119.5(5) . . ? C30 N4 Pt1 127.2(4) . . ? C23 N4 Pt1 112.6(3) . . ? C24 N5 C23 118.8(5) . . ? C30 N6 C32 130.3(4) . . ? C30 N6 H6 114.8 . . ? C32 N6 H6 114.8 . . ? C17 P1 C11 108.1(3) . . ? C17 P1 C10 100.2(3) . . ? C11 P1 C10 107.4(3) . . ? C17 P1 Pt1 122.57(19) . . ? C11 P1 Pt1 116.1(2) . . ? C10 P1 Pt1 99.6(2) . . ? C39 P2 C33 106.5(3) . . ? C39 P2 C32 107.3(3) . . ? C33 P2 C32 103.5(3) . . ? C39 P2 Pt1 115.84(19) . . ? C33 P2 Pt1 120.93(18) . . ? C32 P2 Pt1 101.1(2) . . ? N2 C1 C5 122.8(5) . . ? N2 C1 N1 114.9(5) . . ? C5 C1 N1 122.3(5) . . ? N2 C2 C3 122.9(6) . . ? N2 C2 C9 116.8(5) . . ? C3 C2 C9 120.3(6) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C1 118.3(6) . . ? C4 C5 C6 124.3(6) . . ? C1 C5 C6 117.4(6) . . ? C7 C6 C5 120.2(6) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? N1 C8 N3 122.4(5) . . ? N1 C8 C7 120.9(5) . . ? N3 C8 C7 116.6(5) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 P1 116.2(4) . . ? N3 C10 H10A 108.2 . . ? P1 C10 H10A 108.2 . . ? N3 C10 H10B 108.2 . . ? P1 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C16 120.0(6) . . ? C12 C11 P1 119.0(5) . . ? C16 C11 P1 121.0(5) . . ? C13 C12 C11 119.2(7) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 120.8(8) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.4(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.9(8) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 118.6(7) . . ? C11 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C22 C17 C18 119.6(6) . . ? C22 C17 P1 122.2(5) . . ? C18 C17 P1 118.2(4) . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.2(7) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.5(7) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.8(7) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C17 C22 C21 119.7(7) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N5 C23 N4 115.9(5) . . ? N5 C23 C27 122.8(5) . . ? N4 C23 C27 121.3(5) . . ? N5 C24 C25 121.5(6) . . ? N5 C24 C31 117.2(6) . . ? C25 C24 C31 121.3(6) . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 118.7(6) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C26 C27 C23 117.6(6) . . ? C26 C27 C28 125.1(6) . . ? C23 C27 C28 117.2(5) . . ? C29 C28 C27 120.6(6) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.6(6) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? N6 C30 N4 122.4(5) . . ? N6 C30 C29 117.3(5) . . ? N4 C30 C29 120.3(5) . . ? C24 C31 H31A 109.5 . . ? C24 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C24 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 P2 115.4(4) . . ? N6 C32 H32A 108.4 . . ? P2 C32 H32A 108.4 . . ? N6 C32 H32B 108.4 . . ? P2 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C34 C33 C38 119.1(5) . . ? C34 C33 P2 120.0(4) . . ? C38 C33 P2 120.8(5) . . ? C33 C34 C35 120.0(6) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.5(7) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.3(7) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.0(6) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C40 C39 C44 118.8(5) . . ? C40 C39 P2 119.8(4) . . ? C44 C39 P2 121.4(5) . . ? C39 C40 C41 120.4(6) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.4(7) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.4(7) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 120.1(6) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.0(6) . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? Cl3 C45 Cl4 111.9(6) . . ? Cl3 C45 H45A 109.2 . . ? Cl4 C45 H45A 109.2 . . ? Cl3 C45 H45B 109.2 . . ? Cl4 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? Cl6 C46 Cl5 104.4(7) . . ? Cl6 C46 H46A 110.9 . . ? Cl5 C46 H46A 110.9 . . ? Cl6 C46 H46B 110.9 . . ? Cl5 C46 H46B 110.9 . . ? H46A C46 H46B 108.9 . . ? 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 N4 Pt1 N1 C8 121.6(5) . . . . ? P2 Pt1 N1 C8 -167.5(4) . . . . ? P1 Pt1 N1 C8 -46.2(5) . . . . ? N4 Pt1 N1 C1 -56.3(4) . . . . ? P2 Pt1 N1 C1 14.6(8) . . . . ? P1 Pt1 N1 C1 135.9(4) . . . . ? N1 Pt1 N4 C30 117.0(5) . . . . ? P2 Pt1 N4 C30 -51.1(5) . . . . ? P1 Pt1 N4 C30 -169.9(4) . . . . ? N1 Pt1 N4 C23 -52.9(4) . . . . ? P2 Pt1 N4 C23 139.1(4) . . . . ? P1 Pt1 N4 C23 20.2(8) . . . . ? N4 Pt1 P1 C17 91.1(6) . . . . ? N1 Pt1 P1 C17 165.2(3) . . . . ? P2 Pt1 P1 C17 -25.8(2) . . . . ? N4 Pt1 P1 C11 -132.5(6) . . . . ? N1 Pt1 P1 C11 -58.5(2) . . . . ? P2 Pt1 P1 C11 110.6(2) . . . . ? N4 Pt1 P1 C10 -17.6(6) . . . . ? N1 Pt1 P1 C10 56.4(2) . . . . ? P2 Pt1 P1 C10 -134.6(2) . . . . ? N4 Pt1 P2 C39 -58.5(2) . . . . ? N1 Pt1 P2 C39 -130.4(6) . . . . ? P1 Pt1 P2 C39 110.1(2) . . . . ? N4 Pt1 P2 C33 170.3(3) . . . . ? N1 Pt1 P2 C33 98.5(6) . . . . ? P1 Pt1 P2 C33 -21.0(2) . . . . ? N4 Pt1 P2 C32 57.1(2) . . . . ? N1 Pt1 P2 C32 -14.8(6) . . . . ? P1 Pt1 P2 C32 -134.3(2) . . . . ? C2 N2 C1 C5 2.4(9) . . . . ? C2 N2 C1 N1 -177.7(5) . . . . ? C8 N1 C1 N2 172.2(5) . . . . ? Pt1 N1 C1 N2 -9.7(6) . . . . ? C8 N1 C1 C5 -7.9(8) . . . . ? Pt1 N1 C1 C5 170.3(4) . . . . ? C1 N2 C2 C3 -0.4(9) . . . . ? C1 N2 C2 C9 -179.2(5) . . . . ? N2 C2 C3 C4 -1.9(11) . . . . ? C9 C2 C3 C4 176.8(7) . . . . ? C2 C3 C4 C5 2.2(11) . . . . ? C3 C4 C5 C1 -0.4(10) . . . . ? C3 C4 C5 C6 177.6(7) . . . . ? N2 C1 C5 C4 -2.0(9) . . . . ? N1 C1 C5 C4 178.1(6) . . . . ? N2 C1 C5 C6 179.9(6) . . . . ? N1 C1 C5 C6 -0.1(9) . . . . ? C4 C5 C6 C7 -172.7(7) . . . . ? C1 C5 C6 C7 5.4(10) . . . . ? C5 C6 C7 C8 -2.8(10) . . . . ? C1 N1 C8 N3 -169.2(5) . . . . ? Pt1 N1 C8 N3 13.0(8) . . . . ? C1 N1 C8 C7 10.6(8) . . . . ? Pt1 N1 C8 C7 -167.2(4) . . . . ? C10 N3 C8 N1 6.6(10) . . . . ? C10 N3 C8 C7 -173.1(6) . . . . ? C6 C7 C8 N1 -5.6(10) . . . . ? C6 C7 C8 N3 174.2(6) . . . . ? C8 N3 C10 P1 24.8(8) . . . . ? C17 P1 C10 N3 171.8(4) . . . . ? C11 P1 C10 N3 59.0(5) . . . . ? Pt1 P1 C10 N3 -62.4(5) . . . . ? C17 P1 C11 C12 123.5(5) . . . . ? C10 P1 C11 C12 -129.1(5) . . . . ? Pt1 P1 C11 C12 -18.7(6) . . . . ? C17 P1 C11 C16 -58.3(6) . . . . ? C10 P1 C11 C16 49.1(6) . . . . ? Pt1 P1 C11 C16 159.5(5) . . . . ? C16 C11 C12 C13 -0.2(10) . . . . ? P1 C11 C12 C13 178.0(5) . . . . ? C11 C12 C13 C14 0.8(11) . . . . ? C12 C13 C14 C15 -0.1(13) . . . . ? C13 C14 C15 C16 -1.1(13) . . . . ? C12 C11 C16 C15 -1.0(10) . . . . ? P1 C11 C16 C15 -179.1(5) . . . . ? C14 C15 C16 C11 1.7(12) . . . . ? C11 P1 C17 C22 -13.9(6) . . . . ? C10 P1 C17 C22 -126.1(5) . . . . ? Pt1 P1 C17 C22 125.4(5) . . . . ? C11 P1 C17 C18 163.2(5) . . . . ? C10 P1 C17 C18 51.0(5) . . . . ? Pt1 P1 C17 C18 -57.5(5) . . . . ? C22 C17 C18 C19 3.1(9) . . . . ? P1 C17 C18 C19 -174.0(5) . . . . ? C17 C18 C19 C20 -2.6(11) . . . . ? C18 C19 C20 C21 0.3(12) . . . . ? C19 C20 C21 C22 1.4(12) . . . . ? C18 C17 C22 C21 -1.5(9) . . . . ? P1 C17 C22 C21 175.6(5) . . . . ? C20 C21 C22 C17 -0.8(11) . . . . ? C24 N5 C23 N4 179.3(5) . . . . ? C24 N5 C23 C27 -1.5(9) . . . . ? C30 N4 C23 N5 172.7(5) . . . . ? Pt1 N4 C23 N5 -16.6(6) . . . . ? C30 N4 C23 C27 -6.5(8) . . . . ? Pt1 N4 C23 C27 164.2(4) . . . . ? C23 N5 C24 C25 0.4(9) . . . . ? C23 N5 C24 C31 179.7(6) . . . . ? N5 C24 C25 C26 0.7(10) . . . . ? C31 C24 C25 C26 -178.5(7) . . . . ? C24 C25 C26 C27 -0.8(11) . . . . ? C25 C26 C27 C23 -0.2(10) . . . . ? C25 C26 C27 C28 179.6(7) . . . . ? N5 C23 C27 C26 1.4(9) . . . . ? N4 C23 C27 C26 -179.4(6) . . . . ? N5 C23 C27 C28 -178.5(6) . . . . ? N4 C23 C27 C28 0.7(9) . . . . ? C26 C27 C28 C29 -176.4(7) . . . . ? C23 C27 C28 C29 3.5(10) . . . . ? C27 C28 C29 C30 -2.0(10) . . . . ? C32 N6 C30 N4 3.5(10) . . . . ? C32 N6 C30 C29 -174.9(6) . . . . ? C23 N4 C30 N6 -170.2(5) . . . . ? Pt1 N4 C30 N6 20.5(8) . . . . ? C23 N4 C30 C29 8.1(8) . . . . ? Pt1 N4 C30 C29 -161.1(4) . . . . ? C28 C29 C30 N6 174.4(6) . . . . ? C28 C29 C30 N4 -3.9(10) . . . . ? C30 N6 C32 P2 21.9(8) . . . . ? C39 P2 C32 N6 63.0(5) . . . . ? C33 P2 C32 N6 175.4(4) . . . . ? Pt1 P2 C32 N6 -58.8(4) . . . . ? C39 P2 C33 C34 164.1(5) . . . . ? C32 P2 C33 C34 51.1(5) . . . . ? Pt1 P2 C33 C34 -60.9(5) . . . . ? C39 P2 C33 C38 -18.2(5) . . . . ? C32 P2 C33 C38 -131.2(5) . . . . ? Pt1 P2 C33 C38 116.8(4) . . . . ? C38 C33 C34 C35 1.2(9) . . . . ? P2 C33 C34 C35 178.9(5) . . . . ? C33 C34 C35 C36 -1.5(11) . . . . ? C34 C35 C36 C37 0.3(12) . . . . ? C35 C36 C37 C38 1.1(12) . . . . ? C36 C37 C38 C33 -1.3(11) . . . . ? C34 C33 C38 C37 0.2(9) . . . . ? P2 C33 C38 C37 -177.5(5) . . . . ? C33 P2 C39 C40 111.6(5) . . . . ? C32 P2 C39 C40 -138.0(5) . . . . ? Pt1 P2 C39 C40 -26.0(5) . . . . ? C33 P2 C39 C44 -65.6(5) . . . . ? C32 P2 C39 C44 44.8(5) . . . . ? Pt1 P2 C39 C44 156.8(4) . . . . ? C44 C39 C40 C41 0.3(8) . . . . ? P2 C39 C40 C41 -177.0(4) . . . . ? C39 C40 C41 C42 -0.7(9) . . . . ? C40 C41 C42 C43 0.3(10) . . . . ? C41 C42 C43 C44 0.6(10) . . . . ? C42 C43 C44 C39 -1.0(10) . . . . ? C40 C39 C44 C43 0.6(9) . . . . ? P2 C39 C44 C43 177.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 2.862 _refine_diff_density_min -1.476 _refine_diff_density_rms 0.131 # Attachment 'complex 5.cif' data_060927c _database_code_depnum_ccdc_archive 'CCDC 666206' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H42 Cl4 N6 O8 P2 Pt' _chemical_formula_weight 1193.68 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' Pt Pt -1.7033 8.3905 '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' O O 0.0106 0.0060 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.624(11) _cell_length_b 17.326(12) _cell_length_c 20.341(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.453(7) _cell_angle_gamma 90.00 _cell_volume 4829(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 10055 _cell_measurement_theta_min 2.135 _cell_measurement_theta_max 26.982 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 3.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4226 _exptl_absorpt_correction_T_max 0.6243 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 23953 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8503 _reflns_number_gt 6520 _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^)+(0.0448P)^2^+0.6654P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8503 _refine_ls_number_parameters 639 _refine_ls_number_restraints 388 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.083 _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 Pt1 Pt 0.215956(13) 0.170003(11) 0.395041(9) 0.03007(8) Uani 1 1 d . . . Cl1 Cl 0.18304(15) 0.40881(14) 0.15551(10) 0.0862(6) Uani 1 1 d DU . . Cl2 Cl 0.32173(19) 0.79406(13) 0.10211(15) 0.0993(7) Uani 1 1 d DU . . Cl3 Cl 0.5389(3) 0.98986(18) 0.09801(18) 0.1739(15) Uani 1 1 d DU . . Cl4 Cl 0.5367(8) 1.0183(6) 0.2328(4) 0.207(3) Uani 0.591(8) 1 d PDU A 1 Cl4' Cl 0.6115(11) 1.0665(9) 0.2518(6) 0.207(3) Uani 0.409(8) 1 d PDU A 2 N1 N 0.1373(3) 0.0796(2) 0.3284(2) 0.0325(10) Uani 1 1 d . . . N2 N 0.2322(3) 0.1146(2) 0.2637(2) 0.0369(10) Uani 1 1 d . . . N3 N 0.0232(3) 0.0521(3) 0.3817(2) 0.0450(11) Uani 1 1 d . . . H3 H -0.0184 0.0183 0.3845 0.054 Uiso 1 1 calc R . . N4 N 0.3497(3) 0.1110(2) 0.4119(2) 0.0339(10) Uani 1 1 d . . . N5 N 0.2764(3) 0.0167(2) 0.4571(2) 0.0401(11) Uani 1 1 d . . . N6 N 0.4383(3) 0.2091(3) 0.3832(2) 0.0474(12) Uani 1 1 d . . . H6 H 0.4902 0.2185 0.3738 0.057 Uiso 1 1 calc R . . O1 O 0.0936(5) 0.4127(4) 0.0992(3) 0.127(2) Uani 1 1 d DU . . O2 O 0.1841(4) 0.4763(4) 0.1953(3) 0.130(2) Uani 1 1 d DU . . O3 O 0.1932(8) 0.3446(4) 0.1964(4) 0.192(4) Uani 1 1 d DU . . O4 O 0.2557(6) 0.4119(5) 0.1265(4) 0.186(4) Uani 1 1 d DU . . O5 O 0.3839(11) 0.7449(9) 0.1471(7) 0.156(5) Uani 0.599(10) 1 d PDU B 1 O6 O 0.3003(11) 0.8646(6) 0.1181(7) 0.153(5) Uani 0.599(10) 1 d PDU B 1 O7 O 0.3662(10) 0.8055(9) 0.0482(7) 0.149(5) Uani 0.599(10) 1 d PDU B 1 O8 O 0.2282(9) 0.7569(9) 0.0691(9) 0.197(6) Uani 0.599(10) 1 d PDU B 1 O5' O 0.3033(19) 0.7986(14) 0.0310(8) 0.174(7) Uani 0.401(10) 1 d PDU B 2 O6' O 0.3493(18) 0.7156(8) 0.1224(12) 0.155(7) Uani 0.401(10) 1 d PDU B 2 O7' O 0.2508(13) 0.8132(14) 0.1277(13) 0.175(7) Uani 0.401(10) 1 d PDU B 2 O8' O 0.4077(14) 0.8368(12) 0.1433(12) 0.188(7) Uani 0.401(10) 1 d PDU B 2 P1 P 0.07036(9) 0.20791(8) 0.39101(7) 0.0332(3) Uani 1 1 d . . . P2 P 0.30970(10) 0.27017(7) 0.44249(7) 0.0345(3) Uani 1 1 d . . . C1 C 0.1767(4) 0.0600(3) 0.2780(2) 0.0347(12) Uani 1 1 d . . . C2 C 0.2771(4) 0.0981(3) 0.2188(3) 0.0477(15) Uani 1 1 d . . . C3 C 0.2681(5) 0.0253(4) 0.1870(3) 0.0636(18) Uani 1 1 d . . . H3A H 0.3018 0.0144 0.1568 0.076 Uiso 1 1 calc R . . C4 C 0.2100(5) -0.0294(4) 0.2005(3) 0.0619(18) Uani 1 1 d . . . H4 H 0.2034 -0.0776 0.1792 0.074 Uiso 1 1 calc R . . C5 C 0.1606(4) -0.0129(3) 0.2461(3) 0.0431(13) Uani 1 1 d . . . C6 C 0.0971(5) -0.0645(3) 0.2639(3) 0.0548(16) Uani 1 1 d . . . H6A H 0.0875 -0.1142 0.2456 0.066 Uiso 1 1 calc R . . C7 C 0.0515(4) -0.0412(3) 0.3066(3) 0.0494(15) Uani 1 1 d . . . H7 H 0.0057 -0.0732 0.3150 0.059 Uiso 1 1 calc R . . C8 C 0.0726(4) 0.0326(3) 0.3398(3) 0.0364(12) Uani 1 1 d . . . C9 C 0.3387(5) 0.1595(4) 0.2036(3) 0.0626(18) Uani 1 1 d . . . H9A H 0.3209 0.2088 0.2169 0.094 Uiso 1 1 calc R . . H9B H 0.3286 0.1596 0.1544 0.094 Uiso 1 1 calc R . . H9C H 0.4062 0.1494 0.2298 0.094 Uiso 1 1 calc R . . C10 C 0.0287(4) 0.1210(3) 0.4229(3) 0.0437(13) Uani 1 1 d . . . H10A H 0.0724 0.1110 0.4704 0.052 Uiso 1 1 calc R . . H10B H -0.0355 0.1310 0.4250 0.052 Uiso 1 1 calc R . . C11 C 0.0561(4) 0.2795(3) 0.4517(3) 0.0374(12) Uani 1 1 d . . . C12 C -0.0020(5) 0.3432(4) 0.4309(4) 0.0656(19) Uani 1 1 d . . . H12 H -0.0339 0.3523 0.3833 0.079 Uiso 1 1 calc R . . C13 C -0.0136(6) 0.3933(4) 0.4788(4) 0.084(2) Uani 1 1 d . . . H13 H -0.0536 0.4362 0.4635 0.100 Uiso 1 1 calc R . . C14 C 0.0326(6) 0.3814(4) 0.5487(4) 0.077(2) Uani 1 1 d . . . H14 H 0.0238 0.4156 0.5813 0.092 Uiso 1 1 calc R . . C15 C 0.0917(5) 0.3190(4) 0.5705(3) 0.068(2) Uani 1 1 d . . . H15 H 0.1237 0.3107 0.6182 0.081 Uiso 1 1 calc R . . C16 C 0.1046(4) 0.2679(4) 0.5226(3) 0.0536(16) Uani 1 1 d . . . H16 H 0.1459 0.2257 0.5379 0.064 Uiso 1 1 calc R . . C17 C -0.0182(4) 0.2249(3) 0.3049(3) 0.0436(14) Uani 1 1 d . . . C18 C -0.1176(5) 0.2232(4) 0.2944(4) 0.072(2) Uani 1 1 d . . . H18 H -0.1384 0.2178 0.3325 0.086 Uiso 1 1 calc R . . C19 C -0.1839(6) 0.2295(6) 0.2282(5) 0.105(3) Uani 1 1 d . . . H19 H -0.2502 0.2276 0.2213 0.126 Uiso 1 1 calc R . . C20 C -0.1547(8) 0.2385(5) 0.1718(5) 0.106(4) Uani 1 1 d . . . H20 H -0.2008 0.2410 0.1268 0.127 Uiso 1 1 calc R . . C21 C -0.0571(7) 0.2437(4) 0.1818(3) 0.085(3) Uani 1 1 d . . . H21 H -0.0371 0.2523 0.1437 0.102 Uiso 1 1 calc R . . C22 C 0.0115(5) 0.2363(3) 0.2483(3) 0.0547(16) Uani 1 1 d . . . H22 H 0.0777 0.2389 0.2550 0.066 Uiso 1 1 calc R . . C23 C 0.3453(4) 0.0336(3) 0.4302(2) 0.0343(12) Uani 1 1 d . . . C24 C 0.2662(4) -0.0568(3) 0.4739(3) 0.0479(15) Uani 1 1 d . . . C25 C 0.3255(5) -0.1157(3) 0.4640(3) 0.0535(16) Uani 1 1 d . . . H25 H 0.3161 -0.1664 0.4750 0.064 Uiso 1 1 calc R . . C26 C 0.3972(5) -0.0981(3) 0.4380(3) 0.0557(17) Uani 1 1 d . . . H26 H 0.4372 -0.1370 0.4317 0.067 Uiso 1 1 calc R . . C27 C 0.4108(4) -0.0216(3) 0.4208(3) 0.0417(13) Uani 1 1 d . . . C28 C 0.4848(4) 0.0049(4) 0.3968(3) 0.0516(15) Uani 1 1 d . . . H28 H 0.5278 -0.0301 0.3886 0.062 Uiso 1 1 calc R . . C29 C 0.4934(4) 0.0803(3) 0.3858(3) 0.0483(15) Uani 1 1 d . . . H29 H 0.5447 0.0977 0.3726 0.058 Uiso 1 1 calc R . . C30 C 0.4244(4) 0.1341(3) 0.3940(3) 0.0388(13) Uani 1 1 d . . . C31 C 0.1896(5) -0.0731(4) 0.5046(4) 0.072(2) Uani 1 1 d . . . H31A H 0.1558 -0.0262 0.5068 0.108 Uiso 1 1 calc R . . H31B H 0.2194 -0.0938 0.5510 0.108 Uiso 1 1 calc R . . H31C H 0.1441 -0.1100 0.4757 0.108 Uiso 1 1 calc R . . C32 C 0.3809(4) 0.2764(3) 0.3846(3) 0.0435(14) Uani 1 1 d . . . H32A H 0.3366 0.2864 0.3373 0.052 Uiso 1 1 calc R . . H32B H 0.4245 0.3204 0.3990 0.052 Uiso 1 1 calc R . . C33 C 0.3972(4) 0.2584(3) 0.5301(3) 0.0379(13) Uani 1 1 d . . . C34 C 0.4810(4) 0.3025(3) 0.5529(3) 0.0547(16) Uani 1 1 d . . . H34 H 0.4939 0.3378 0.5228 0.066 Uiso 1 1 calc R . . C35 C 0.5453(5) 0.2939(4) 0.6207(4) 0.068(2) Uani 1 1 d . . . H35 H 0.6021 0.3233 0.6362 0.082 Uiso 1 1 calc R . . C36 C 0.5263(5) 0.2423(4) 0.6652(3) 0.0633(19) Uani 1 1 d . . . H36 H 0.5696 0.2376 0.7110 0.076 Uiso 1 1 calc R . . C37 C 0.4436(5) 0.1972(4) 0.6427(3) 0.0548(16) Uani 1 1 d . . . H37 H 0.4312 0.1621 0.6732 0.066 Uiso 1 1 calc R . . C38 C 0.3785(4) 0.2046(3) 0.5741(3) 0.0419(13) Uani 1 1 d . . . H38 H 0.3231 0.1737 0.5580 0.050 Uiso 1 1 calc R . . C39 C 0.2596(4) 0.3665(3) 0.4356(3) 0.0360(12) Uani 1 1 d . . . C40 C 0.2790(5) 0.4140(3) 0.4931(3) 0.0552(17) Uani 1 1 d . . . H40 H 0.3159 0.3958 0.5375 0.066 Uiso 1 1 calc R . . C41 C 0.2438(6) 0.4888(4) 0.4852(3) 0.076(2) Uani 1 1 d . . . H41 H 0.2551 0.5201 0.5243 0.091 Uiso 1 1 calc R . . C42 C 0.1924(5) 0.5168(4) 0.4198(4) 0.070(2) Uani 1 1 d . . . H42 H 0.1716 0.5679 0.4145 0.084 Uiso 1 1 calc R . . C43 C 0.1717(5) 0.4707(4) 0.3633(4) 0.070(2) Uani 1 1 d . . . H43 H 0.1350 0.4898 0.3192 0.084 Uiso 1 1 calc R . . C44 C 0.2046(4) 0.3946(4) 0.3701(3) 0.0551(16) Uani 1 1 d . . . H44 H 0.1895 0.3629 0.3309 0.066 Uiso 1 1 calc R . . C45 C 0.5521(17) 0.9540(10) 0.1845(8) 0.145(5) Uani 0.591(8) 1 d PDU A 1 H45A H 0.5051 0.9131 0.1800 0.174 Uiso 0.591(8) 1 calc PR A 1 H45B H 0.6169 0.9323 0.2060 0.174 Uiso 0.591(8) 1 calc PR A 1 C45' C 0.593(3) 0.9913(14) 0.1909(9) 0.145(5) Uani 0.409(8) 1 d PD A 2 H45C H 0.5564 0.9529 0.2064 0.174 Uiso 0.409(8) 1 calc PR A 2 H45D H 0.6571 0.9693 0.2005 0.174 Uiso 0.409(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02924(11) 0.02510(12) 0.03609(12) -0.00392(9) 0.01171(8) -0.00072(9) Cl1 0.0843(14) 0.1126(17) 0.0652(11) -0.0033(11) 0.0304(11) 0.0430(12) Cl2 0.0995(16) 0.0656(14) 0.156(2) -0.0150(15) 0.0742(17) 0.0182(13) Cl3 0.227(4) 0.106(2) 0.166(3) 0.015(2) 0.039(3) 0.050(2) Cl4 0.213(6) 0.265(7) 0.177(4) 0.030(5) 0.110(5) 0.094(5) Cl4' 0.213(6) 0.265(7) 0.177(4) 0.030(5) 0.110(5) 0.094(5) N1 0.033(2) 0.025(2) 0.037(2) -0.0059(18) 0.0095(19) -0.0032(18) N2 0.040(2) 0.036(3) 0.038(2) -0.0013(19) 0.017(2) -0.003(2) N3 0.043(3) 0.036(3) 0.062(3) -0.008(2) 0.026(2) -0.015(2) N4 0.028(2) 0.038(3) 0.038(2) -0.0032(19) 0.0140(19) 0.0038(19) N5 0.038(2) 0.035(3) 0.046(3) 0.000(2) 0.013(2) 0.001(2) N6 0.046(3) 0.039(3) 0.068(3) -0.006(2) 0.034(3) -0.009(2) O1 0.129(5) 0.155(5) 0.081(3) -0.025(4) 0.016(3) 0.051(4) O2 0.100(4) 0.150(6) 0.140(5) -0.056(5) 0.044(4) 0.022(4) O3 0.298(11) 0.141(7) 0.127(6) 0.057(5) 0.061(7) 0.073(7) O4 0.162(7) 0.241(9) 0.207(7) 0.017(7) 0.130(6) 0.087(6) O5 0.173(11) 0.132(11) 0.188(11) 0.032(9) 0.093(9) 0.076(9) O6 0.193(11) 0.082(8) 0.231(10) -0.050(7) 0.131(9) 0.025(7) O7 0.128(9) 0.172(10) 0.192(10) 0.013(9) 0.113(8) 0.029(9) O8 0.147(10) 0.171(11) 0.283(13) -0.052(11) 0.086(10) -0.008(9) O5' 0.206(15) 0.142(12) 0.210(13) -0.007(12) 0.116(13) 0.029(13) O6' 0.179(14) 0.076(11) 0.206(14) -0.033(10) 0.063(12) 0.002(11) O7' 0.135(11) 0.158(13) 0.280(14) -0.065(12) 0.132(11) 0.019(11) O8' 0.163(12) 0.156(12) 0.240(12) -0.036(11) 0.063(11) -0.047(10) P1 0.0302(7) 0.0322(7) 0.0375(7) -0.0021(6) 0.0120(6) 0.0021(6) P2 0.0347(7) 0.0253(7) 0.0422(7) -0.0050(6) 0.0118(6) -0.0017(6) C1 0.035(3) 0.035(3) 0.031(3) 0.000(2) 0.008(2) -0.002(2) C2 0.050(3) 0.054(4) 0.043(3) -0.001(3) 0.020(3) -0.008(3) C3 0.075(5) 0.076(5) 0.049(4) -0.023(3) 0.032(3) -0.011(4) C4 0.075(5) 0.055(4) 0.062(4) -0.026(3) 0.032(4) -0.010(3) C5 0.051(3) 0.034(3) 0.043(3) -0.009(3) 0.015(3) -0.002(3) C6 0.068(4) 0.034(3) 0.060(4) -0.017(3) 0.020(3) -0.014(3) C7 0.051(4) 0.038(3) 0.061(4) -0.013(3) 0.021(3) -0.019(3) C8 0.036(3) 0.037(3) 0.036(3) 0.003(2) 0.012(2) -0.002(2) C9 0.072(4) 0.070(5) 0.055(4) -0.002(3) 0.035(3) -0.013(4) C10 0.047(3) 0.040(3) 0.052(3) -0.001(3) 0.026(3) -0.001(3) C11 0.033(3) 0.035(3) 0.047(3) -0.010(2) 0.018(2) -0.003(2) C12 0.076(5) 0.052(4) 0.062(4) -0.003(3) 0.016(4) 0.023(3) C13 0.094(6) 0.060(5) 0.095(6) -0.015(4) 0.031(5) 0.037(4) C14 0.083(5) 0.072(5) 0.089(6) -0.032(4) 0.047(5) 0.005(4) C15 0.069(5) 0.084(6) 0.054(4) -0.022(4) 0.026(3) -0.012(4) C16 0.051(4) 0.056(4) 0.052(4) -0.011(3) 0.016(3) 0.006(3) C17 0.038(3) 0.039(3) 0.046(3) -0.002(3) 0.004(3) 0.003(2) C18 0.040(4) 0.086(5) 0.078(5) -0.001(4) 0.007(3) -0.003(4) C19 0.052(5) 0.128(8) 0.101(7) 0.014(6) -0.017(5) 0.000(5) C20 0.102(8) 0.097(7) 0.068(5) -0.003(5) -0.033(6) 0.023(6) C21 0.115(7) 0.077(5) 0.047(4) 0.001(4) 0.009(4) 0.045(5) C22 0.067(4) 0.051(4) 0.044(3) 0.000(3) 0.017(3) 0.016(3) C23 0.034(3) 0.032(3) 0.034(3) -0.003(2) 0.009(2) -0.001(2) C24 0.053(4) 0.038(3) 0.049(3) 0.008(3) 0.013(3) 0.002(3) C25 0.062(4) 0.035(3) 0.059(4) 0.005(3) 0.016(3) 0.001(3) C26 0.058(4) 0.035(4) 0.068(4) -0.002(3) 0.015(3) 0.013(3) C27 0.038(3) 0.037(3) 0.047(3) -0.004(3) 0.012(3) 0.008(2) C28 0.046(3) 0.048(4) 0.063(4) -0.010(3) 0.022(3) 0.013(3) C29 0.037(3) 0.054(4) 0.060(4) -0.011(3) 0.026(3) 0.000(3) C30 0.038(3) 0.039(3) 0.039(3) -0.009(2) 0.012(2) -0.003(2) C31 0.078(5) 0.057(4) 0.093(5) 0.026(4) 0.043(4) 0.005(4) C32 0.051(3) 0.025(3) 0.059(3) -0.003(3) 0.025(3) -0.006(2) C33 0.034(3) 0.033(3) 0.044(3) -0.005(2) 0.011(2) 0.003(2) C34 0.045(4) 0.044(3) 0.066(4) -0.002(3) 0.008(3) -0.009(3) C35 0.044(4) 0.058(4) 0.081(5) -0.010(4) -0.005(4) -0.006(3) C36 0.049(4) 0.071(5) 0.054(4) -0.015(4) 0.000(3) 0.013(4) C37 0.058(4) 0.060(4) 0.048(3) 0.001(3) 0.021(3) 0.021(3) C38 0.037(3) 0.043(3) 0.047(3) -0.002(3) 0.016(3) 0.007(3) C39 0.037(3) 0.024(3) 0.045(3) -0.002(2) 0.012(2) 0.000(2) C40 0.078(4) 0.041(4) 0.046(3) -0.005(3) 0.021(3) 0.015(3) C41 0.124(6) 0.047(4) 0.060(4) -0.012(3) 0.034(4) 0.020(4) C42 0.086(5) 0.040(4) 0.081(5) 0.012(4) 0.025(4) 0.021(4) C43 0.089(5) 0.049(4) 0.069(4) 0.023(4) 0.025(4) 0.020(4) C44 0.061(4) 0.047(4) 0.049(3) -0.005(3) 0.008(3) 0.004(3) C45 0.181(9) 0.104(8) 0.125(7) -0.035(7) 0.024(6) 0.058(7) C45' 0.181(9) 0.104(8) 0.125(7) -0.035(7) 0.024(6) 0.058(7) _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 Pt1 N4 2.126(4) . ? Pt1 N1 2.126(4) . ? Pt1 P1 2.202(2) . ? Pt1 P2 2.2131(17) . ? Cl1 O3 1.365(7) . ? Cl1 O4 1.385(7) . ? Cl1 O1 1.408(5) . ? Cl1 O2 1.419(6) . ? Cl2 O6 1.329(9) . ? Cl2 O5 1.345(10) . ? Cl2 O7' 1.355(13) . ? Cl2 O5' 1.378(14) . ? Cl2 O6' 1.437(14) . ? Cl2 O8' 1.448(13) . ? Cl2 O8 1.448(11) . ? Cl2 O7 1.471(10) . ? Cl3 C45' 1.775(17) . ? Cl3 C45 1.810(15) . ? Cl4 C45 1.554(14) . ? Cl4' C45' 1.753(17) . ? N1 C8 1.328(6) . ? N1 C1 1.383(6) . ? N2 C2 1.329(7) . ? N2 C1 1.343(6) . ? N3 C8 1.340(7) . ? N3 C10 1.444(7) . ? N3 H3 0.8600 . ? N4 C30 1.328(7) . ? N4 C23 1.399(6) . ? N5 C23 1.336(6) . ? N5 C24 1.341(7) . ? N6 C30 1.345(7) . ? N6 C32 1.443(7) . ? N6 H6 0.8600 . ? P1 C17 1.803(5) . ? P1 C11 1.813(5) . ? P1 C10 1.827(6) . ? P2 C33 1.806(5) . ? P2 C39 1.809(5) . ? P2 C32 1.827(6) . ? C1 C5 1.402(7) . ? C2 C3 1.402(8) . ? C2 C9 1.494(8) . ? C3 C4 1.363(9) . ? C3 H3A 0.9300 . ? C4 C5 1.391(8) . ? C4 H4 0.9300 . ? C5 C6 1.423(8) . ? C6 C7 1.330(8) . ? C6 H6A 0.9300 . ? C7 C8 1.428(7) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.366(8) . ? C11 C16 1.380(7) . ? C12 C13 1.360(9) . ? C12 H12 0.9300 . ? C13 C14 1.361(10) . ? C13 H13 0.9300 . ? C14 C15 1.358(9) . ? C14 H14 0.9300 . ? C15 C16 1.378(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.379(8) . ? C17 C18 1.393(8) . ? C18 C19 1.362(10) . ? C18 H18 0.9300 . ? C19 C20 1.366(13) . ? C19 H19 0.9300 . ? C20 C21 1.373(13) . ? C20 H20 0.9300 . ? C21 C22 1.380(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C27 1.414(7) . ? C24 C25 1.399(8) . ? C24 C31 1.487(9) . ? C25 C26 1.363(8) . ? C25 H25 0.9300 . ? C26 C27 1.403(8) . ? C26 H26 0.9300 . ? C27 C28 1.410(8) . ? C28 C29 1.338(8) . ? C28 H28 0.9300 . ? C29 C30 1.427(7) . ? C29 H29 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.379(7) . ? C33 C38 1.384(7) . ? C34 C35 1.379(8) . ? C34 H34 0.9300 . ? C35 C36 1.368(10) . ? C35 H35 0.9300 . ? C36 C37 1.377(9) . ? C36 H36 0.9300 . ? C37 C38 1.394(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.376(7) . ? C39 C44 1.382(7) . ? C40 C41 1.382(8) . ? C40 H40 0.9300 . ? C41 C42 1.367(9) . ? C41 H41 0.9300 . ? C42 C43 1.345(9) . ? C42 H42 0.9300 . ? C43 C44 1.394(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45' H45C 0.9700 . ? C45' H45D 0.9700 . ? 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 N4 Pt1 N1 90.63(16) . . ? N4 Pt1 P1 166.52(12) . . ? N1 Pt1 P1 83.97(12) . . ? N4 Pt1 P2 84.96(13) . . ? N1 Pt1 P2 165.96(12) . . ? P1 Pt1 P2 103.06(7) . . ? O3 Cl1 O4 110.8(5) . . ? O3 Cl1 O1 114.0(6) . . ? O4 Cl1 O1 106.5(5) . . ? O3 Cl1 O2 110.3(5) . . ? O4 Cl1 O2 110.7(5) . . ? O1 Cl1 O2 104.3(4) . . ? O6 Cl2 O5 125.2(9) . . ? O6 Cl2 O7' 53.4(9) . . ? O5 Cl2 O7' 108.6(14) . . ? O6 Cl2 O5' 103.2(12) . . ? O5 Cl2 O5' 126.0(13) . . ? O7' Cl2 O5' 119.6(12) . . ? O6 Cl2 O6' 149.9(11) . . ? O5 Cl2 O6' 31.8(10) . . ? O7' Cl2 O6' 107.2(13) . . ? O5' Cl2 O6' 106.7(11) . . ? O6 Cl2 O8' 67.6(10) . . ? O5 Cl2 O8' 71.7(11) . . ? O7' Cl2 O8' 106.2(11) . . ? O5' Cl2 O8' 113.0(12) . . ? O6' Cl2 O8' 102.6(11) . . ? O6 Cl2 O8 104.9(8) . . ? O5 Cl2 O8 109.8(10) . . ? O7' Cl2 O8 63.9(10) . . ? O5' Cl2 O8 74.5(12) . . ? O6' Cl2 O8 80.6(11) . . ? O8' Cl2 O8 170.1(11) . . ? O6 Cl2 O7 105.2(9) . . ? O5 Cl2 O7 102.9(8) . . ? O7' Cl2 O7 148.3(12) . . ? O5' Cl2 O7 35.4(11) . . ? O6' Cl2 O7 100.9(13) . . ? O8' Cl2 O7 80.9(11) . . ? O8 Cl2 O7 107.9(9) . . ? C45' Cl3 C45 27.6(13) . . ? C8 N1 C1 118.9(4) . . ? C8 N1 Pt1 126.9(3) . . ? C1 N1 Pt1 112.4(3) . . ? C2 N2 C1 118.6(5) . . ? C8 N3 C10 130.1(5) . . ? C8 N3 H3 114.9 . . ? C10 N3 H3 114.9 . . ? C30 N4 C23 118.8(4) . . ? C30 N4 Pt1 127.5(4) . . ? C23 N4 Pt1 112.3(3) . . ? C23 N5 C24 118.7(5) . . ? C30 N6 C32 130.9(5) . . ? C30 N6 H6 114.6 . . ? C32 N6 H6 114.6 . . ? C17 P1 C11 109.6(3) . . ? C17 P1 C10 105.3(3) . . ? C11 P1 C10 100.9(3) . . ? C17 P1 Pt1 116.2(2) . . ? C11 P1 Pt1 121.24(17) . . ? C10 P1 Pt1 100.31(19) . . ? C33 P2 C39 108.0(2) . . ? C33 P2 C32 106.0(3) . . ? C39 P2 C32 101.7(2) . . ? C33 P2 Pt1 117.33(18) . . ? C39 P2 Pt1 121.19(17) . . ? C32 P2 Pt1 99.87(18) . . ? N2 C1 N1 115.3(4) . . ? N2 C1 C5 123.4(5) . . ? N1 C1 C5 121.3(5) . . ? N2 C2 C3 121.5(6) . . ? N2 C2 C9 117.8(5) . . ? C3 C2 C9 120.7(6) . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C1 116.8(5) . . ? C4 C5 C6 125.3(5) . . ? C1 C5 C6 117.8(5) . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? N1 C8 N3 122.1(5) . . ? N1 C8 C7 121.1(5) . . ? N3 C8 C7 116.8(5) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 P1 115.7(4) . . ? N3 C10 H10A 108.4 . . ? P1 C10 H10A 108.4 . . ? N3 C10 H10B 108.4 . . ? P1 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C16 118.6(5) . . ? C12 C11 P1 123.2(4) . . ? C16 C11 P1 118.2(4) . . ? C13 C12 C11 120.9(6) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.8(7) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.8(6) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C22 C17 C18 119.5(6) . . ? C22 C17 P1 120.3(5) . . ? C18 C17 P1 120.1(5) . . ? C19 C18 C17 119.6(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 121.0(8) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.9(7) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 120.0(8) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 119.9(7) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? N5 C23 N4 115.5(4) . . ? N5 C23 C27 123.5(5) . . ? N4 C23 C27 121.1(5) . . ? N5 C24 C25 121.7(6) . . ? N5 C24 C31 117.1(5) . . ? C25 C24 C31 121.2(6) . . ? C26 C25 C24 119.6(6) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.2(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 126.0(5) . . ? C26 C27 C23 116.3(5) . . ? C28 C27 C23 117.7(5) . . ? C29 C28 C27 120.3(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.5(6) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? N4 C30 N6 121.6(5) . . ? N4 C30 C29 121.2(5) . . ? N6 C30 C29 117.2(5) . . ? C24 C31 H31A 109.5 . . ? C24 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C24 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 P2 115.6(4) . . ? N6 C32 H32A 108.4 . . ? P2 C32 H32A 108.4 . . ? N6 C32 H32B 108.4 . . ? P2 C32 H32B 108.4 . . ? H32A C32 H32B 107.4 . . ? C34 C33 C38 120.6(5) . . ? C34 C33 P2 120.6(4) . . ? C38 C33 P2 118.8(4) . . ? C35 C34 C33 119.4(6) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.6(6) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.6(6) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C33 C38 C37 119.3(5) . . ? C33 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C40 C39 C44 119.1(5) . . ? C40 C39 P2 121.9(4) . . ? C44 C39 P2 118.9(4) . . ? C39 C40 C41 120.2(6) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.2(6) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.2(6) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.6(6) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C39 C44 C43 119.6(6) . . ? C39 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? Cl4 C45 Cl3 112.3(10) . . ? Cl4 C45 H45A 109.1 . . ? Cl3 C45 H45A 109.1 . . ? Cl4 C45 H45B 109.1 . . ? Cl3 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? Cl4' C45' Cl3 131.7(15) . . ? Cl4' C45' H45C 104.3 . . ? Cl3 C45' H45C 104.3 . . ? Cl4' C45' H45D 104.3 . . ? Cl3 C45' H45D 104.3 . . ? H45C C45' H45D 105.6 . . ? 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 N4 Pt1 N1 C8 115.2(4) . . . . ? P1 Pt1 N1 C8 -52.4(4) . . . . ? P2 Pt1 N1 C8 -173.3(3) . . . . ? N4 Pt1 N1 C1 -49.4(3) . . . . ? P1 Pt1 N1 C1 142.9(3) . . . . ? P2 Pt1 N1 C1 22.0(7) . . . . ? N1 Pt1 N4 C30 116.6(4) . . . . ? P1 Pt1 N4 C30 -177.3(3) . . . . ? P2 Pt1 N4 C30 -50.0(4) . . . . ? N1 Pt1 N4 C23 -49.2(3) . . . . ? P1 Pt1 N4 C23 16.9(7) . . . . ? P2 Pt1 N4 C23 144.2(3) . . . . ? N4 Pt1 P1 C17 -122.9(5) . . . . ? N1 Pt1 P1 C17 -56.1(2) . . . . ? P2 Pt1 P1 C17 111.6(2) . . . . ? N4 Pt1 P1 C11 99.6(5) . . . . ? N1 Pt1 P1 C11 166.4(2) . . . . ? P2 Pt1 P1 C11 -25.9(2) . . . . ? N4 Pt1 P1 C10 -10.0(5) . . . . ? N1 Pt1 P1 C10 56.8(2) . . . . ? P2 Pt1 P1 C10 -135.52(18) . . . . ? N4 Pt1 P2 C33 -58.1(2) . . . . ? N1 Pt1 P2 C33 -130.2(5) . . . . ? P1 Pt1 P2 C33 110.9(2) . . . . ? N4 Pt1 P2 C39 166.0(2) . . . . ? N1 Pt1 P2 C39 93.8(5) . . . . ? P1 Pt1 P2 C39 -25.0(2) . . . . ? N4 Pt1 P2 C32 55.8(2) . . . . ? N1 Pt1 P2 C32 -16.4(5) . . . . ? P1 Pt1 P2 C32 -135.20(18) . . . . ? C2 N2 C1 N1 176.1(4) . . . . ? C2 N2 C1 C5 -2.4(7) . . . . ? C8 N1 C1 N2 172.3(4) . . . . ? Pt1 N1 C1 N2 -21.7(5) . . . . ? C8 N1 C1 C5 -9.2(7) . . . . ? Pt1 N1 C1 C5 156.8(4) . . . . ? C1 N2 C2 C3 -0.5(8) . . . . ? C1 N2 C2 C9 -179.9(5) . . . . ? N2 C2 C3 C4 2.0(9) . . . . ? C9 C2 C3 C4 -178.7(6) . . . . ? C2 C3 C4 C5 -0.6(10) . . . . ? C3 C4 C5 C1 -2.0(9) . . . . ? C3 C4 C5 C6 179.2(6) . . . . ? N2 C1 C5 C4 3.6(8) . . . . ? N1 C1 C5 C4 -174.7(5) . . . . ? N2 C1 C5 C6 -177.5(5) . . . . ? N1 C1 C5 C6 4.1(7) . . . . ? C4 C5 C6 C7 -177.9(6) . . . . ? C1 C5 C6 C7 3.4(8) . . . . ? C5 C6 C7 C8 -5.6(9) . . . . ? C1 N1 C8 N3 -172.1(4) . . . . ? Pt1 N1 C8 N3 24.2(7) . . . . ? C1 N1 C8 C7 6.9(7) . . . . ? Pt1 N1 C8 C7 -156.8(4) . . . . ? C10 N3 C8 N1 -2.0(8) . . . . ? C10 N3 C8 C7 179.0(5) . . . . ? C6 C7 C8 N1 0.5(8) . . . . ? C6 C7 C8 N3 179.5(5) . . . . ? C8 N3 C10 P1 26.2(7) . . . . ? C17 P1 C10 N3 61.2(5) . . . . ? C11 P1 C10 N3 175.2(4) . . . . ? Pt1 P1 C10 N3 -59.9(4) . . . . ? C17 P1 C11 C12 -10.3(6) . . . . ? C10 P1 C11 C12 -121.1(6) . . . . ? Pt1 P1 C11 C12 129.6(5) . . . . ? C17 P1 C11 C16 168.1(4) . . . . ? C10 P1 C11 C16 57.4(5) . . . . ? Pt1 P1 C11 C16 -51.9(5) . . . . ? C16 C11 C12 C13 -1.4(10) . . . . ? P1 C11 C12 C13 177.0(6) . . . . ? C11 C12 C13 C14 0.2(12) . . . . ? C12 C13 C14 C15 0.7(13) . . . . ? C13 C14 C15 C16 -0.3(12) . . . . ? C14 C15 C16 C11 -0.9(10) . . . . ? C12 C11 C16 C15 1.8(9) . . . . ? P1 C11 C16 C15 -176.8(5) . . . . ? C11 P1 C17 C22 123.3(5) . . . . ? C10 P1 C17 C22 -128.8(5) . . . . ? Pt1 P1 C17 C22 -18.8(5) . . . . ? C11 P1 C17 C18 -59.6(6) . . . . ? C10 P1 C17 C18 48.2(6) . . . . ? Pt1 P1 C17 C18 158.2(5) . . . . ? C22 C17 C18 C19 2.8(10) . . . . ? P1 C17 C18 C19 -174.3(6) . . . . ? C17 C18 C19 C20 -0.9(14) . . . . ? C18 C19 C20 C21 -2.0(15) . . . . ? C19 C20 C21 C22 3.1(13) . . . . ? C18 C17 C22 C21 -1.7(9) . . . . ? P1 C17 C22 C21 175.3(5) . . . . ? C20 C21 C22 C17 -1.2(11) . . . . ? C24 N5 C23 N4 178.1(4) . . . . ? C24 N5 C23 C27 -2.3(7) . . . . ? C30 N4 C23 N5 170.8(4) . . . . ? Pt1 N4 C23 N5 -22.0(5) . . . . ? C30 N4 C23 C27 -8.8(7) . . . . ? Pt1 N4 C23 C27 158.4(4) . . . . ? C23 N5 C24 C25 -0.1(8) . . . . ? C23 N5 C24 C31 179.2(5) . . . . ? N5 C24 C25 C26 1.6(9) . . . . ? C31 C24 C25 C26 -177.7(6) . . . . ? C24 C25 C26 C27 -0.6(9) . . . . ? C25 C26 C27 C28 176.8(5) . . . . ? C25 C26 C27 C23 -1.6(8) . . . . ? N5 C23 C27 C26 3.2(7) . . . . ? N4 C23 C27 C26 -177.3(5) . . . . ? N5 C23 C27 C28 -175.3(5) . . . . ? N4 C23 C27 C28 4.2(7) . . . . ? C26 C27 C28 C29 -176.3(5) . . . . ? C23 C27 C28 C29 2.1(8) . . . . ? C27 C28 C29 C30 -3.8(8) . . . . ? C23 N4 C30 N6 -172.8(4) . . . . ? Pt1 N4 C30 N6 22.2(7) . . . . ? C23 N4 C30 C29 7.1(7) . . . . ? Pt1 N4 C30 C29 -157.9(4) . . . . ? C32 N6 C30 N4 -2.8(8) . . . . ? C32 N6 C30 C29 177.3(5) . . . . ? C28 C29 C30 N4 -0.9(8) . . . . ? C28 C29 C30 N6 179.0(5) . . . . ? C30 N6 C32 P2 28.6(7) . . . . ? C33 P2 C32 N6 62.0(4) . . . . ? C39 P2 C32 N6 174.8(4) . . . . ? Pt1 P2 C32 N6 -60.3(4) . . . . ? C39 P2 C33 C34 -64.3(5) . . . . ? C32 P2 C33 C34 44.0(5) . . . . ? Pt1 P2 C33 C34 154.4(4) . . . . ? C39 P2 C33 C38 115.3(4) . . . . ? C32 P2 C33 C38 -136.4(4) . . . . ? Pt1 P2 C33 C38 -26.0(5) . . . . ? C38 C33 C34 C35 -1.4(9) . . . . ? P2 C33 C34 C35 178.3(5) . . . . ? C33 C34 C35 C36 -0.3(10) . . . . ? C34 C35 C36 C37 1.2(11) . . . . ? C35 C36 C37 C38 -0.3(10) . . . . ? C34 C33 C38 C37 2.2(8) . . . . ? P2 C33 C38 C37 -177.4(4) . . . . ? C36 C37 C38 C33 -1.4(8) . . . . ? C33 P2 C39 C40 -8.4(6) . . . . ? C32 P2 C39 C40 -119.6(5) . . . . ? Pt1 P2 C39 C40 131.2(5) . . . . ? C33 P2 C39 C44 168.2(5) . . . . ? C32 P2 C39 C44 56.9(5) . . . . ? Pt1 P2 C39 C44 -52.3(5) . . . . ? C44 C39 C40 C41 -0.1(10) . . . . ? P2 C39 C40 C41 176.4(6) . . . . ? C39 C40 C41 C42 -2.2(12) . . . . ? C40 C41 C42 C43 3.2(12) . . . . ? C41 C42 C43 C44 -1.8(12) . . . . ? C40 C39 C44 C43 1.5(9) . . . . ? P2 C39 C44 C43 -175.2(5) . . . . ? C42 C43 C44 C39 -0.5(11) . . . . ? C45' Cl3 C45 Cl4 56(2) . . . . ? C45 Cl3 C45' Cl4' -129(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.161 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.094 # Attachment 'complex 6.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 666207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H32 Cl N4 P Pt' _chemical_formula_weight 818.20 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.565(8) _cell_length_b 10.6978(19) _cell_length_c 22.217(5) _cell_angle_alpha 90.00 _cell_angle_beta 132.471(2) _cell_angle_gamma 90.00 _cell_volume 6586(2) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 4.426 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4164 _exptl_absorpt_correction_T_max 0.5030 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30213 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.89 _reflns_number_total 7843 _reflns_number_gt 6918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0321P)^2^+10.3565P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7843 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _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 Pt1 Pt 0.153105(4) 0.802843(12) 0.506996(7) 0.01304(5) Uani 1 1 d . . . Cl1 Cl 0.07572(3) 0.65458(10) 0.22431(5) 0.0293(2) Uani 1 1 d . . . P1 P 0.09253(3) 0.93285(8) 0.42944(5) 0.01427(17) Uani 1 1 d . . . N1 N 0.20338(10) 0.6560(3) 0.55164(16) 0.0163(6) Uani 1 1 d . . . N2 N 0.02960(11) 0.7512(3) 0.39987(17) 0.0186(6) Uani 1 1 d . . . N3 N 0.10834(10) 0.7201(3) 0.52626(16) 0.0149(6) Uani 1 1 d . . . N4 N 0.18384(10) 0.7067(3) 0.65464(17) 0.0181(6) Uani 1 1 d . . . C1 C 0.20515(11) 0.8948(3) 0.52329(18) 0.0169(7) Uani 1 1 d . . . C2 C 0.20597(13) 1.0208(4) 0.5076(2) 0.0234(8) Uani 1 1 d . . . H2 H 0.1771 1.0683 0.4767 0.028 Uiso 1 1 calc R . . C3 C 0.24827(13) 1.0782(4) 0.5362(2) 0.0271(8) Uani 1 1 d . . . H3 H 0.2478 1.1639 0.5245 0.032 Uiso 1 1 calc R . . C4 C 0.29112(13) 1.0112(4) 0.5818(2) 0.0273(9) Uani 1 1 d . . . H4 H 0.3198 1.0507 0.6007 0.033 Uiso 1 1 calc R . . C5 C 0.29196(13) 0.8872(4) 0.5996(2) 0.0233(8) Uani 1 1 d . . . H5 H 0.3212 0.8411 0.6308 0.028 Uiso 1 1 calc R . . C6 C 0.24957(12) 0.8292(3) 0.5716(2) 0.0185(7) Uani 1 1 d . . . C7 C 0.24813(12) 0.6972(3) 0.58779(19) 0.0183(7) Uani 1 1 d . . . C8 C 0.28759(13) 0.6165(4) 0.6345(2) 0.0248(8) Uani 1 1 d . . . H8 H 0.3190 0.6461 0.6608 0.030 Uiso 1 1 calc R . . C9 C 0.28043(13) 0.4932(4) 0.6421(2) 0.0291(9) Uani 1 1 d . . . H9 H 0.3071 0.4380 0.6761 0.035 Uiso 1 1 calc R . . C10 C 0.23389(14) 0.4501(4) 0.5996(2) 0.0263(8) Uani 1 1 d . . . H10 H 0.2283 0.3646 0.6024 0.032 Uiso 1 1 calc R . . C11 C 0.19548(12) 0.5338(3) 0.5529(2) 0.0192(7) Uani 1 1 d . . . C12 C 0.14445(12) 0.4919(3) 0.4978(2) 0.0191(7) Uani 1 1 d . . . C13 C 0.12808(14) 0.4140(3) 0.5251(2) 0.0261(8) Uani 1 1 d . . . H13 H 0.1502 0.3827 0.5794 0.031 Uiso 1 1 calc R . . C14 C 0.07985(15) 0.3820(4) 0.4736(3) 0.0333(9) Uani 1 1 d . . . H14 H 0.0688 0.3308 0.4930 0.040 Uiso 1 1 calc R . . C15 C 0.04742(15) 0.4244(4) 0.3933(3) 0.0329(9) Uani 1 1 d . . . H15 H 0.0142 0.4027 0.3581 0.040 Uiso 1 1 calc R . . C16 C 0.06364(13) 0.4983(4) 0.3650(2) 0.0265(8) Uani 1 1 d . . . H16 H 0.0418 0.5255 0.3098 0.032 Uiso 1 1 calc R . . C17 C 0.11184(13) 0.5328(3) 0.4172(2) 0.0215(7) Uani 1 1 d . . . H17 H 0.1227 0.5848 0.3977 0.026 Uiso 1 1 calc R . . C18 C 0.08756(11) 1.0275(3) 0.35646(18) 0.0157(7) Uani 1 1 d . . . C19 C 0.08205(14) 1.1571(3) 0.3516(2) 0.0246(8) Uani 1 1 d . . . H19 H 0.0779 1.1988 0.3843 0.030 Uiso 1 1 calc R . . C20 C 0.08262(15) 1.2255(4) 0.2989(2) 0.0279(9) Uani 1 1 d . . . H20 H 0.0794 1.3139 0.2964 0.034 Uiso 1 1 calc R . . C21 C 0.08785(14) 1.1657(4) 0.2502(2) 0.0272(8) Uani 1 1 d . . . H21 H 0.0885 1.2126 0.2147 0.033 Uiso 1 1 calc R . . C22 C 0.09217(12) 1.0362(4) 0.2535(2) 0.0219(8) Uani 1 1 d . . . H22 H 0.0950 0.9946 0.2191 0.026 Uiso 1 1 calc R . . C23 C 0.09244(12) 0.9673(3) 0.30672(19) 0.0197(7) Uani 1 1 d . . . H23 H 0.0960 0.8790 0.3093 0.024 Uiso 1 1 calc R . . C24 C 0.07790(12) 1.0250(3) 0.47827(19) 0.0163(7) Uani 1 1 d . . . C25 C 0.03083(12) 1.0653(3) 0.4369(2) 0.0208(7) Uani 1 1 d . . . H25 H 0.0059 1.0528 0.3797 0.025 Uiso 1 1 calc R . . C26 C 0.02070(13) 1.1231(3) 0.4793(2) 0.0253(8) Uani 1 1 d . . . H26 H -0.0114 1.1490 0.4512 0.030 Uiso 1 1 calc R . . C27 C 0.05681(14) 1.1440(4) 0.5626(2) 0.0272(8) Uani 1 1 d . . . H27 H 0.0495 1.1838 0.5913 0.033 Uiso 1 1 calc R . . C28 C 0.10327(14) 1.1068(4) 0.6033(2) 0.0270(8) Uani 1 1 d . . . H28 H 0.1283 1.1229 0.6601 0.032 Uiso 1 1 calc R . . C29 C 0.11366(13) 1.0456(3) 0.5617(2) 0.0218(7) Uani 1 1 d . . . H29 H 0.1456 1.0175 0.5906 0.026 Uiso 1 1 calc R . . C30 C 0.04062(12) 0.8270(3) 0.3603(2) 0.0177(7) Uani 1 1 d . . . H30A H 0.0118 0.8776 0.3172 0.021 Uiso 1 1 calc R . . H30B H 0.0472 0.7709 0.3333 0.021 Uiso 1 1 calc R . . C31 C 0.06056(12) 0.7041(3) 0.4762(2) 0.0175(7) Uani 1 1 d . . . C32 C 0.03909(12) 0.6381(3) 0.5012(2) 0.0199(7) Uani 1 1 d . . . H32 H 0.0051 0.6277 0.4637 0.024 Uiso 1 1 calc R . . C33 C 0.06665(12) 0.5909(3) 0.5772(2) 0.0219(7) Uani 1 1 d . . . H33 H 0.0525 0.5461 0.5934 0.026 Uiso 1 1 calc R . . C34 C 0.11771(12) 0.6096(4) 0.6328(2) 0.0212(7) Uani 1 1 d . . . C35 C 0.13670(12) 0.6783(3) 0.6061(2) 0.0161(7) Uani 1 1 d . . . C36 C 0.21454(13) 0.6597(4) 0.7301(2) 0.0252(8) Uani 1 1 d . . . C37 C 0.19913(14) 0.5830(4) 0.7601(2) 0.0333(10) Uani 1 1 d . . . H37 H 0.2220 0.5473 0.8130 0.040 Uiso 1 1 calc R . . C38 C 0.15073(14) 0.5601(4) 0.7121(2) 0.0291(9) Uani 1 1 d . . . H38 H 0.1397 0.5112 0.7324 0.035 Uiso 1 1 calc R . . C39 C 0.26683(14) 0.6891(4) 0.7800(2) 0.0342(10) Uani 1 1 d . . . H39A H 0.2702 0.7437 0.7486 0.041 Uiso 1 1 calc R . . H39B H 0.2847 0.6113 0.7934 0.041 Uiso 1 1 calc R . . H39C H 0.2798 0.7314 0.8304 0.041 Uiso 1 1 calc R . . H1 H -0.0007(18) 0.732(5) 0.367(3) 0.052(15) Uiso 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 Pt1 0.01041(7) 0.01681(7) 0.01130(7) 0.00089(5) 0.00710(6) 0.00045(5) Cl1 0.0183(4) 0.0404(5) 0.0196(4) 0.0013(4) 0.0090(4) 0.0101(4) P1 0.0128(4) 0.0157(4) 0.0127(4) 0.0004(3) 0.0079(4) 0.0008(3) N1 0.0170(14) 0.0216(14) 0.0128(13) 0.0010(11) 0.0111(12) 0.0034(12) N2 0.0109(14) 0.0207(15) 0.0167(14) 0.0001(12) 0.0063(13) -0.0024(12) N3 0.0144(14) 0.0174(14) 0.0155(13) 0.0021(11) 0.0112(12) 0.0009(11) N4 0.0155(14) 0.0270(16) 0.0141(13) 0.0019(11) 0.0110(13) 0.0008(12) C1 0.0146(16) 0.0266(18) 0.0110(15) -0.0025(13) 0.0093(14) -0.0049(14) C2 0.0220(19) 0.0279(19) 0.0183(17) 0.0014(15) 0.0128(16) -0.0031(15) C3 0.029(2) 0.032(2) 0.0239(18) -0.0023(16) 0.0190(17) -0.0098(17) C4 0.0226(19) 0.042(2) 0.0256(19) -0.0105(17) 0.0195(17) -0.0149(17) C5 0.0174(17) 0.039(2) 0.0173(17) -0.0079(15) 0.0130(15) -0.0047(16) C6 0.0172(17) 0.0293(19) 0.0132(16) -0.0019(13) 0.0120(15) -0.0012(14) C7 0.0155(17) 0.0307(19) 0.0113(15) -0.0023(13) 0.0101(14) 0.0020(14) C8 0.0157(17) 0.039(2) 0.0187(17) -0.0004(16) 0.0109(16) 0.0056(16) C9 0.023(2) 0.040(2) 0.0262(19) 0.0084(17) 0.0171(18) 0.0150(17) C10 0.032(2) 0.0243(19) 0.0275(19) 0.0077(15) 0.0219(18) 0.0098(16) C11 0.0226(18) 0.0227(17) 0.0186(17) 0.0046(14) 0.0164(16) 0.0064(15) C12 0.0234(18) 0.0164(16) 0.0244(18) -0.0015(13) 0.0189(17) 0.0004(14) C13 0.039(2) 0.0156(17) 0.034(2) 0.0025(15) 0.0287(19) 0.0044(16) C14 0.044(2) 0.0172(18) 0.055(3) -0.0072(17) 0.040(2) -0.0064(17) C15 0.029(2) 0.026(2) 0.046(2) -0.0130(18) 0.027(2) -0.0068(17) C16 0.024(2) 0.0228(19) 0.0277(19) -0.0068(15) 0.0157(17) -0.0008(16) C17 0.0235(19) 0.0158(16) 0.0269(18) -0.0012(14) 0.0177(17) 0.0033(14) C18 0.0119(16) 0.0208(17) 0.0103(15) 0.0003(12) 0.0058(13) 0.0016(13) C19 0.033(2) 0.0227(18) 0.0218(18) 0.0027(14) 0.0202(18) 0.0051(16) C20 0.035(2) 0.0218(19) 0.026(2) 0.0053(15) 0.0202(19) 0.0049(16) C21 0.025(2) 0.036(2) 0.0206(18) 0.0053(16) 0.0155(17) -0.0001(17) C22 0.0182(18) 0.034(2) 0.0162(16) -0.0013(14) 0.0126(15) 0.0004(15) C23 0.0150(17) 0.0231(18) 0.0172(16) 0.0000(13) 0.0093(15) 0.0012(14) C24 0.0179(17) 0.0164(16) 0.0179(16) 0.0007(13) 0.0135(15) -0.0013(13) C25 0.0177(17) 0.0199(17) 0.0199(17) -0.0033(14) 0.0107(15) -0.0004(14) C26 0.0218(19) 0.0255(19) 0.035(2) 0.0018(16) 0.0216(18) 0.0049(15) C27 0.039(2) 0.027(2) 0.035(2) 0.0007(16) 0.032(2) 0.0030(18) C28 0.029(2) 0.034(2) 0.0193(17) -0.0022(16) 0.0168(17) 0.0020(17) C29 0.0195(18) 0.0258(19) 0.0191(17) -0.0014(14) 0.0126(16) 0.0009(15) C30 0.0155(17) 0.0202(17) 0.0143(16) -0.0002(13) 0.0088(15) 0.0004(13) C31 0.0156(16) 0.0167(16) 0.0204(17) -0.0001(13) 0.0122(15) 0.0033(13) C32 0.0145(17) 0.0191(17) 0.0281(19) -0.0036(14) 0.0152(16) -0.0017(14) C33 0.0224(18) 0.0211(18) 0.0303(19) -0.0008(15) 0.0210(17) -0.0033(15) C34 0.0198(18) 0.0273(19) 0.0214(17) 0.0011(14) 0.0158(16) -0.0014(15) C35 0.0175(17) 0.0169(16) 0.0179(16) 0.0013(12) 0.0136(15) 0.0024(13) C36 0.0188(18) 0.041(2) 0.0140(17) 0.0009(15) 0.0102(16) 0.0015(16) C37 0.024(2) 0.056(3) 0.0172(18) 0.0124(18) 0.0126(17) 0.0026(19) C38 0.031(2) 0.041(2) 0.0232(19) 0.0060(17) 0.0211(18) -0.0010(18) C39 0.0178(19) 0.064(3) 0.0148(18) 0.0053(18) 0.0087(16) 0.0024(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 Pt1 C1 1.991(3) . ? Pt1 N1 2.118(3) . ? Pt1 N3 2.183(3) . ? Pt1 P1 2.1878(9) . ? P1 C24 1.805(3) . ? P1 C18 1.811(3) . ? P1 C30 1.844(3) . ? N1 C11 1.346(4) . ? N1 C7 1.357(4) . ? N2 C31 1.349(4) . ? N2 C30 1.448(4) . ? N2 H1 0.87(5) . ? N3 C31 1.339(4) . ? N3 C35 1.389(4) . ? N4 C36 1.336(4) . ? N4 C35 1.346(4) . ? C1 C2 1.398(5) . ? C1 C6 1.418(5) . ? C2 C3 1.393(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(6) . ? C4 H4 0.9500 . ? C5 C6 1.403(5) . ? C5 H5 0.9500 . ? C6 C7 1.467(5) . ? C7 C8 1.394(5) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.392(5) . ? C10 H10 0.9500 . ? C11 C12 1.485(5) . ? C12 C17 1.392(5) . ? C12 C13 1.395(5) . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.391(6) . ? C14 H14 0.9500 . ? C15 C16 1.382(6) . ? C15 H15 0.9500 . ? C16 C17 1.387(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.394(5) . ? C18 C19 1.396(5) . ? C19 C20 1.394(5) . ? C19 H19 0.9500 . ? C20 C21 1.380(5) . ? C20 H20 0.9500 . ? C21 C22 1.391(5) . ? C21 H21 0.9500 . ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.387(5) . ? C24 C25 1.401(5) . ? C25 C26 1.378(5) . ? C25 H25 0.9500 . ? C26 C27 1.387(5) . ? C26 H26 0.9500 . ? C27 C28 1.375(5) . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.435(5) . ? C32 C33 1.348(5) . ? C32 H32 0.9500 . ? C33 C34 1.430(5) . ? C33 H33 0.9500 . ? C34 C38 1.404(5) . ? C34 C35 1.405(5) . ? C36 C37 1.404(5) . ? C36 C39 1.499(5) . ? C37 C38 1.373(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? 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 C1 Pt1 N1 79.96(13) . . ? C1 Pt1 N3 163.00(11) . . ? N1 Pt1 N3 99.73(11) . . ? C1 Pt1 P1 101.56(10) . . ? N1 Pt1 P1 164.67(8) . . ? N3 Pt1 P1 83.27(8) . . ? C24 P1 C18 110.11(16) . . ? C24 P1 C30 104.88(16) . . ? C18 P1 C30 100.67(15) . . ? C24 P1 Pt1 116.80(11) . . ? C18 P1 Pt1 118.95(11) . . ? C30 P1 Pt1 102.61(11) . . ? C11 N1 C7 120.4(3) . . ? C11 N1 Pt1 126.2(2) . . ? C7 N1 Pt1 113.1(2) . . ? C31 N2 C30 128.0(3) . . ? C31 N2 H1 120(3) . . ? C30 N2 H1 112(3) . . ? C31 N3 C35 117.5(3) . . ? C31 N3 Pt1 131.8(2) . . ? C35 N3 Pt1 110.7(2) . . ? C36 N4 C35 118.3(3) . . ? C2 C1 C6 116.9(3) . . ? C2 C1 Pt1 128.0(3) . . ? C6 C1 Pt1 113.7(2) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.3(3) . . ? C5 C6 C7 122.4(3) . . ? C1 C6 C7 116.3(3) . . ? N1 C7 C8 120.6(3) . . ? N1 C7 C6 113.8(3) . . ? C8 C7 C6 125.6(3) . . ? C9 C8 C7 119.1(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N1 C11 C10 120.5(3) . . ? N1 C11 C12 117.1(3) . . ? C10 C11 C12 122.2(3) . . ? C17 C12 C13 119.0(3) . . ? C17 C12 C11 119.4(3) . . ? C13 C12 C11 121.6(3) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 120.6(4) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 119.4(3) . . ? C23 C18 P1 117.5(3) . . ? C19 C18 P1 123.0(3) . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 120.1(3) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C29 C24 C25 118.9(3) . . ? C29 C24 P1 118.4(3) . . ? C25 C24 P1 122.4(3) . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.8(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 120.7(3) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? N2 C30 P1 114.4(2) . . ? N2 C30 H30A 108.7 . . ? P1 C30 H30A 108.7 . . ? N2 C30 H30B 108.7 . . ? P1 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? N3 C31 N2 122.1(3) . . ? N3 C31 C32 122.0(3) . . ? N2 C31 C32 115.9(3) . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 118.5(3) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C38 C34 C35 117.2(3) . . ? C38 C34 C33 124.4(3) . . ? C35 C34 C33 118.3(3) . . ? N4 C35 N3 114.2(3) . . ? N4 C35 C34 123.2(3) . . ? N3 C35 C34 122.6(3) . . ? N4 C36 C37 122.2(3) . . ? N4 C36 C39 116.0(3) . . ? C37 C36 C39 121.8(3) . . ? C38 C37 C36 119.4(3) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C34 119.4(3) . . ? C37 C38 H38 120.3 . . ? C34 C38 H38 120.3 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt1 P1 C24 -102.59(15) . . . . ? N1 Pt1 P1 C24 163.2(3) . . . . ? N3 Pt1 P1 C24 60.89(14) . . . . ? C1 Pt1 P1 C18 33.44(16) . . . . ? N1 Pt1 P1 C18 -60.8(3) . . . . ? N3 Pt1 P1 C18 -163.08(14) . . . . ? C1 Pt1 P1 C30 143.35(15) . . . . ? N1 Pt1 P1 C30 49.1(3) . . . . ? N3 Pt1 P1 C30 -53.17(13) . . . . ? C1 Pt1 N1 C11 -170.2(3) . . . . ? N3 Pt1 N1 C11 27.1(3) . . . . ? P1 Pt1 N1 C11 -73.0(4) . . . . ? C1 Pt1 N1 C7 15.8(2) . . . . ? N3 Pt1 N1 C7 -146.9(2) . . . . ? P1 Pt1 N1 C7 113.0(3) . . . . ? C1 Pt1 N3 C31 144.5(4) . . . . ? N1 Pt1 N3 C31 -128.1(3) . . . . ? P1 Pt1 N3 C31 36.7(3) . . . . ? C1 Pt1 N3 C35 -35.6(5) . . . . ? N1 Pt1 N3 C35 51.9(2) . . . . ? P1 Pt1 N3 C35 -143.3(2) . . . . ? N1 Pt1 C1 C2 179.3(3) . . . . ? N3 Pt1 C1 C2 -90.2(5) . . . . ? P1 Pt1 C1 C2 14.8(3) . . . . ? N1 Pt1 C1 C6 -14.5(2) . . . . ? N3 Pt1 C1 C6 76.0(5) . . . . ? P1 Pt1 C1 C6 -179.0(2) . . . . ? C6 C1 C2 C3 1.7(5) . . . . ? Pt1 C1 C2 C3 167.5(3) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C1 1.5(5) . . . . ? C4 C5 C6 C7 179.3(3) . . . . ? C2 C1 C6 C5 -2.3(5) . . . . ? Pt1 C1 C6 C5 -170.1(3) . . . . ? C2 C1 C6 C7 179.7(3) . . . . ? Pt1 C1 C6 C7 11.9(4) . . . . ? C11 N1 C7 C8 -7.2(5) . . . . ? Pt1 N1 C7 C8 167.2(3) . . . . ? C11 N1 C7 C6 172.0(3) . . . . ? Pt1 N1 C7 C6 -13.6(3) . . . . ? C5 C6 C7 N1 -176.3(3) . . . . ? C1 C6 C7 N1 1.7(4) . . . . ? C5 C6 C7 C8 3.0(5) . . . . ? C1 C6 C7 C8 -179.1(3) . . . . ? N1 C7 C8 C9 1.4(5) . . . . ? C6 C7 C8 C9 -177.7(3) . . . . ? C7 C8 C9 C10 3.5(5) . . . . ? C8 C9 C10 C11 -2.8(5) . . . . ? C7 N1 C11 C10 7.9(5) . . . . ? Pt1 N1 C11 C10 -165.7(3) . . . . ? C7 N1 C11 C12 -167.3(3) . . . . ? Pt1 N1 C11 C12 19.1(4) . . . . ? C9 C10 C11 N1 -2.9(5) . . . . ? C9 C10 C11 C12 172.1(3) . . . . ? N1 C11 C12 C17 45.8(5) . . . . ? C10 C11 C12 C17 -129.4(4) . . . . ? N1 C11 C12 C13 -133.3(3) . . . . ? C10 C11 C12 C13 51.6(5) . . . . ? C17 C12 C13 C14 -2.5(5) . . . . ? C11 C12 C13 C14 176.6(3) . . . . ? C12 C13 C14 C15 1.8(6) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 -1.8(6) . . . . ? C15 C16 C17 C12 1.1(5) . . . . ? C13 C12 C17 C16 1.1(5) . . . . ? C11 C12 C17 C16 -178.0(3) . . . . ? C24 P1 C18 C23 -173.1(2) . . . . ? C30 P1 C18 C23 -62.7(3) . . . . ? Pt1 P1 C18 C23 48.2(3) . . . . ? C24 P1 C18 C19 10.9(4) . . . . ? C30 P1 C18 C19 121.2(3) . . . . ? Pt1 P1 C18 C19 -127.8(3) . . . . ? C23 C18 C19 C20 -1.5(5) . . . . ? P1 C18 C19 C20 174.5(3) . . . . ? C18 C19 C20 C21 1.0(6) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 -1.6(6) . . . . ? C21 C22 C23 C18 1.1(5) . . . . ? C19 C18 C23 C22 0.5(5) . . . . ? P1 C18 C23 C22 -175.7(3) . . . . ? C18 P1 C24 C29 -116.2(3) . . . . ? C30 P1 C24 C29 136.2(3) . . . . ? Pt1 P1 C24 C29 23.5(3) . . . . ? C18 P1 C24 C25 70.5(3) . . . . ? C30 P1 C24 C25 -37.1(3) . . . . ? Pt1 P1 C24 C25 -149.8(3) . . . . ? C29 C24 C25 C26 -0.6(5) . . . . ? P1 C24 C25 C26 172.6(3) . . . . ? C24 C25 C26 C27 1.1(6) . . . . ? C25 C26 C27 C28 0.1(6) . . . . ? C26 C27 C28 C29 -1.8(6) . . . . ? C25 C24 C29 C28 -1.0(5) . . . . ? P1 C24 C29 C28 -174.6(3) . . . . ? C27 C28 C29 C24 2.2(6) . . . . ? C31 N2 C30 P1 -33.0(5) . . . . ? C24 P1 C30 N2 -55.9(3) . . . . ? C18 P1 C30 N2 -170.2(3) . . . . ? Pt1 P1 C30 N2 66.6(3) . . . . ? C35 N3 C31 N2 174.0(3) . . . . ? Pt1 N3 C31 N2 -6.0(5) . . . . ? C35 N3 C31 C32 -4.6(5) . . . . ? Pt1 N3 C31 C32 175.4(2) . . . . ? C30 N2 C31 N3 -2.3(5) . . . . ? C30 N2 C31 C32 176.3(3) . . . . ? N3 C31 C32 C33 0.8(5) . . . . ? N2 C31 C32 C33 -177.8(3) . . . . ? C31 C32 C33 C34 1.0(5) . . . . ? C32 C33 C34 C38 -176.6(4) . . . . ? C32 C33 C34 C35 1.1(5) . . . . ? C36 N4 C35 N3 -173.5(3) . . . . ? C36 N4 C35 C34 5.0(5) . . . . ? C31 N3 C35 N4 -174.7(3) . . . . ? Pt1 N3 C35 N4 5.3(3) . . . . ? C31 N3 C35 C34 6.7(5) . . . . ? Pt1 N3 C35 C34 -173.2(3) . . . . ? C38 C34 C35 N4 -5.6(5) . . . . ? C33 C34 C35 N4 176.6(3) . . . . ? C38 C34 C35 N3 172.8(3) . . . . ? C33 C34 C35 N3 -5.0(5) . . . . ? C35 N4 C36 C37 -0.4(6) . . . . ? C35 N4 C36 C39 177.0(3) . . . . ? N4 C36 C37 C38 -3.4(6) . . . . ? C39 C36 C37 C38 179.4(4) . . . . ? C36 C37 C38 C34 2.6(6) . . . . ? C35 C34 C38 C37 1.6(6) . . . . ? C33 C34 C38 C37 179.3(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1 Cl1 0.87(5) 2.24(5) 3.097(3) 170(5) 2 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.135 _refine_diff_density_min -1.120 _refine_diff_density_rms 0.137