# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Shaojin Gu' 'Wanzhi Chen' _publ_contact_author_name 'Shaojin Gu' _publ_contact_author_email gushaojin2005@163.com data_080514g _database_code_depnum_ccdc_archive 'CCDC 792158' #TrackingRef 'web_deposit_cif_file_0_ShaojinGu_1283865305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 F12 N10 Ni P2' _chemical_formula_weight 1023.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.664(5) _cell_length_b 12.003(7) _cell_length_c 20.703(11) _cell_angle_alpha 82.101(7) _cell_angle_beta 89.724(7) _cell_angle_gamma 78.062(7) _cell_volume 2327(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8022 _exptl_absorpt_correction_T_max 0.9134 _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 11833 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.1838 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8017 _reflns_number_gt 3001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1525P)^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 8017 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2259 _refine_ls_R_factor_gt 0.1227 _refine_ls_wR_factor_ref 0.3393 _refine_ls_wR_factor_gt 0.3064 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Ni1 Ni 0.46520(15) 0.34129(10) 0.23232(6) 0.0584(5) Uani 1 1 d . . . F1 F 0.8464(16) 0.8410(11) 0.4755(6) 0.210(5) Uani 1 1 d . . . F2 F 0.7693(17) 0.6122(10) 0.5045(6) 0.226(6) Uani 1 1 d . . . F3 F 0.7299(15) 0.7560(10) 0.4239(6) 0.229(6) Uani 1 1 d . . . F4 F 0.6990(14) 0.7864(13) 0.5257(7) 0.245(7) Uani 1 1 d . . . F5 F 0.8966(10) 0.6969(7) 0.5533(4) 0.134(3) Uani 1 1 d . . . F6 F 0.9417(19) 0.6722(15) 0.4569(6) 0.285(9) Uani 1 1 d . . . F7 F 0.8350(13) 1.0575(11) 0.9928(6) 0.221(6) Uani 1 1 d . . . F8 F 0.9462(17) 0.8808(10) 1.0008(6) 0.230(6) Uani 1 1 d . . . F9 F 1.0136(15) 1.0022(10) 0.9265(5) 0.220(7) Uani 1 1 d . . . F10 F 0.441(3) 0.129(2) 0.8621(15) 0.235(12) Uani 0.50 1 d P . . F11 F 0.258(2) 0.246(2) 0.7341(15) 0.223(12) Uani 0.50 1 d P . . F12 F 0.398(2) 0.0833(17) 0.7664(13) 0.198(10) Uani 0.50 1 d P . . F13 F 0.486(3) 0.2350(18) 0.7589(15) 0.211(10) Uani 0.50 1 d P . . F14 F 0.3394(19) 0.3054(14) 0.8191(12) 0.157(7) Uani 0.50 1 d P . . F15 F 0.246(2) 0.1514(16) 0.8343(13) 0.190(10) Uani 0.50 1 d P . . N1 N 0.4405(9) 0.4852(6) 0.1684(4) 0.055(2) Uani 1 1 d . . . N2 N 0.2874(9) 0.4612(7) 0.2720(5) 0.066(2) Uani 1 1 d . . . N3 N 0.6225(10) 0.3929(8) 0.1182(4) 0.066(2) Uani 1 1 d . . . N4 N 0.7293(11) 0.2206(8) 0.1510(5) 0.068(2) Uani 1 1 d . . . N5 N 0.9180(10) 0.2003(8) 0.2557(5) 0.079(3) Uani 1 1 d . . . N6 N 0.4913(8) 0.2088(6) 0.3060(4) 0.054(2) Uani 1 1 d . . . N7 N 0.6036(8) 0.3906(7) 0.3042(4) 0.057(2) Uani 1 1 d . . . N8 N 0.3546(9) 0.1349(6) 0.2428(4) 0.061(2) Uani 1 1 d . . . N9 N 0.2699(9) 0.2171(7) 0.1495(4) 0.065(2) Uani 1 1 d . . . N10 N 0.1422(10) 0.4961(8) 0.0577(4) 0.074(3) Uani 1 1 d . . . P1 P 0.8126(5) 0.7282(3) 0.4889(2) 0.1012(14) Uani 1 1 d . . . P2 P 1.0000 1.0000 1.0000 0.152(3) Uani 1 2 d S . . P3 P 0.3667(9) 0.1965(8) 0.7937(6) 0.117(3) Uani 0.50 1 d P . . C1 C 0.5239(13) 0.4967(9) 0.1188(5) 0.062(3) Uani 1 1 d . . . C2 C 0.5160(15) 0.5934(11) 0.0742(5) 0.083(4) Uani 1 1 d . . . H2 H 0.5771 0.5974 0.0396 0.100 Uiso 1 1 calc R . . C3 C 0.4075(16) 0.6860(11) 0.0853(6) 0.086(4) Uani 1 1 d . . . H3 H 0.3948 0.7526 0.0553 0.103 Uiso 1 1 calc R . . C4 C 0.3178(14) 0.6852(9) 0.1380(6) 0.070(3) Uani 1 1 d . . . C5 C 0.3398(12) 0.5775(9) 0.1790(6) 0.064(3) Uani 1 1 d . . . C6 C 0.2580(12) 0.5636(10) 0.2338(6) 0.068(3) Uani 1 1 d . . . C7 C 0.1507(12) 0.6581(10) 0.2496(7) 0.072(3) Uani 1 1 d . . . C8 C 0.0783(14) 0.6361(11) 0.3043(7) 0.092(4) Uani 1 1 d . . . H8 H 0.0047 0.6934 0.3150 0.110 Uiso 1 1 calc R . . C9 C 0.1073(13) 0.5372(12) 0.3433(7) 0.091(4) Uani 1 1 d . . . H9 H 0.0578 0.5265 0.3815 0.109 Uiso 1 1 calc R . . C10 C 0.2174(13) 0.4452(10) 0.3257(7) 0.082(4) Uani 1 1 d . . . H10 H 0.2383 0.3748 0.3525 0.098 Uiso 1 1 calc R . . C11 C 0.2112(15) 0.7743(10) 0.1562(7) 0.082(4) Uani 1 1 d . . . H11 H 0.1966 0.8461 0.1308 0.098 Uiso 1 1 calc R . . C12 C 0.1355(15) 0.7615(11) 0.2048(8) 0.088(4) Uani 1 1 d . . . H12 H 0.0648 0.8236 0.2121 0.106 Uiso 1 1 calc R . . C13 C 0.6264(12) 0.3010(9) 0.1681(5) 0.059(3) Uani 1 1 d . . . C14 C 0.7930(13) 0.2571(10) 0.0958(6) 0.075(3) Uani 1 1 d . . . H14 H 0.8691 0.2136 0.0767 0.090 Uiso 1 1 calc R . . C15 C 0.7307(14) 0.3634(10) 0.0736(5) 0.073(3) Uani 1 1 d . . . H15 H 0.7528 0.4092 0.0367 0.088 Uiso 1 1 calc R . . C16 C 0.7712(13) 0.1085(9) 0.1920(6) 0.079(3) Uani 1 1 d . . . H16A H 0.8214 0.0534 0.1654 0.095 Uiso 1 1 calc R . . H16B H 0.6863 0.0827 0.2069 0.095 Uiso 1 1 calc R . . C17 C 0.8628(12) 0.1078(9) 0.2505(5) 0.067(3) Uani 1 1 d . . . C18 C 0.8843(13) 0.0104(10) 0.2937(6) 0.082(4) Uani 1 1 d . . . H18 H 0.8458 -0.0525 0.2877 0.098 Uiso 1 1 calc R . . C19 C 0.9706(16) 0.0112(13) 0.3496(8) 0.110(5) Uani 1 1 d . . . H19 H 0.9845 -0.0526 0.3817 0.132 Uiso 1 1 calc R . . C20 C 1.0342(15) 0.1003(14) 0.3587(7) 0.103(4) Uani 1 1 d . . . H20 H 1.0929 0.0992 0.3944 0.124 Uiso 1 1 calc R . . C21 C 1.0010(15) 0.1939(12) 0.3081(7) 0.095(4) Uani 1 1 d . . . H21 H 1.0407 0.2571 0.3115 0.115 Uiso 1 1 calc R . . C22 C 0.4332(11) 0.1202(8) 0.3018(5) 0.058(3) Uani 1 1 d . . . C23 C 0.4562(13) 0.0259(9) 0.3501(6) 0.077(3) Uani 1 1 d . . . H23 H 0.4151 -0.0364 0.3459 0.093 Uiso 1 1 calc R . . C24 C 0.5370(12) 0.0239(9) 0.4027(6) 0.073(3) Uani 1 1 d . . . H24 H 0.5534 -0.0402 0.4347 0.087 Uiso 1 1 calc R . . C25 C 0.5983(11) 0.1208(9) 0.4096(5) 0.062(3) Uani 1 1 d . . . C26 C 0.5700(11) 0.2097(9) 0.3559(5) 0.059(3) Uani 1 1 d . . . C27 C 0.6322(10) 0.3099(9) 0.3559(5) 0.055(3) Uani 1 1 d . . . C28 C 0.7217(11) 0.3157(9) 0.4071(6) 0.068(3) Uani 1 1 d . . . C29 C 0.7770(11) 0.4170(11) 0.4034(6) 0.076(3) Uani 1 1 d . . . H29 H 0.8352 0.4271 0.4368 0.092 Uiso 1 1 calc R . . C30 C 0.7458(13) 0.4952(10) 0.3530(6) 0.079(3) Uani 1 1 d . . . H30 H 0.7830 0.5611 0.3504 0.095 Uiso 1 1 calc R . . C31 C 0.6577(11) 0.4825(9) 0.3028(5) 0.066(3) Uani 1 1 d . . . H31 H 0.6367 0.5405 0.2674 0.079 Uiso 1 1 calc R . . C32 C 0.6912(13) 0.1267(11) 0.4615(6) 0.078(3) Uani 1 1 d . . . H32 H 0.7130 0.0656 0.4952 0.094 Uiso 1 1 calc R . . C33 C 0.7470(12) 0.2193(10) 0.4622(5) 0.077(3) Uani 1 1 d . . . H33 H 0.8029 0.2238 0.4978 0.092 Uiso 1 1 calc R . . C34 C 0.3455(12) 0.2345(9) 0.1995(5) 0.066(3) Uani 1 1 d . . . C35 C 0.2401(13) 0.1076(9) 0.1615(7) 0.078(3) Uani 1 1 d . . . H35 H 0.1917 0.0757 0.1326 0.094 Uiso 1 1 calc R . . C36 C 0.2885(12) 0.0569(9) 0.2177(6) 0.070(3) Uani 1 1 d . . . H36 H 0.2811 -0.0160 0.2374 0.084 Uiso 1 1 calc R . . C37 C 0.2436(12) 0.2971(9) 0.0919(5) 0.071(3) Uani 1 1 d . . . H37A H 0.2087 0.2611 0.0580 0.085 Uiso 1 1 calc R . . H37B H 0.3319 0.3176 0.0776 0.085 Uiso 1 1 calc R . . C38 C 0.1375(12) 0.4052(9) 0.1009(6) 0.065(3) Uani 1 1 d . . . C39 C 0.0400(14) 0.4104(11) 0.1492(6) 0.083(4) Uani 1 1 d . . . H39 H 0.0368 0.3459 0.1792 0.099 Uiso 1 1 calc R . . C40 C -0.0544(13) 0.5143(12) 0.1524(6) 0.085(4) Uani 1 1 d . . . H40 H -0.1200 0.5203 0.1854 0.102 Uiso 1 1 calc R . . C41 C -0.0504(15) 0.6035(11) 0.1085(7) 0.087(4) Uani 1 1 d . . . H41 H -0.1167 0.6717 0.1085 0.104 Uiso 1 1 calc R . . C42 C 0.0504(16) 0.5949(11) 0.0637(7) 0.086(4) Uani 1 1 d . . . H42 H 0.0574 0.6606 0.0354 0.104 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 Ni1 0.0549(9) 0.0441(7) 0.0795(10) -0.0066(6) 0.0017(7) -0.0188(6) F1 0.265(15) 0.158(10) 0.212(11) 0.036(8) -0.035(11) -0.096(10) F2 0.299(17) 0.148(10) 0.241(13) 0.017(9) -0.105(12) -0.100(11) F3 0.278(15) 0.203(11) 0.186(10) -0.034(8) -0.141(10) 0.000(10) F4 0.169(12) 0.272(16) 0.261(15) -0.087(13) 0.040(11) 0.059(12) F5 0.142(8) 0.134(7) 0.115(6) 0.013(5) -0.036(6) -0.020(6) F6 0.288(19) 0.305(19) 0.203(13) -0.080(12) 0.054(13) 0.103(16) F7 0.178(11) 0.217(12) 0.214(11) -0.044(9) -0.085(9) 0.092(9) F8 0.34(2) 0.127(9) 0.237(13) -0.094(9) -0.001(12) -0.023(10) F9 0.308(16) 0.207(11) 0.097(7) -0.063(7) -0.043(8) 0.089(10) F10 0.18(3) 0.22(3) 0.27(3) -0.03(2) -0.07(2) 0.04(2) F11 0.113(17) 0.21(2) 0.31(3) 0.06(2) -0.01(2) -0.015(17) F12 0.151(19) 0.130(16) 0.35(3) -0.108(18) 0.06(2) -0.074(14) F13 0.16(2) 0.137(17) 0.35(3) -0.049(19) -0.01(2) -0.066(16) F14 0.097(13) 0.088(12) 0.29(2) -0.026(13) 0.023(15) -0.023(10) F15 0.135(18) 0.121(15) 0.34(3) -0.079(17) 0.07(2) -0.064(13) N1 0.053(6) 0.041(5) 0.075(6) -0.015(4) -0.010(5) -0.009(4) N2 0.057(6) 0.057(6) 0.091(7) -0.010(5) -0.005(5) -0.024(5) N3 0.066(7) 0.073(6) 0.063(6) -0.018(5) -0.003(5) -0.020(5) N4 0.076(7) 0.060(6) 0.074(7) -0.013(5) 0.003(6) -0.021(5) N5 0.069(7) 0.079(7) 0.095(7) -0.018(6) -0.001(6) -0.025(5) N6 0.043(5) 0.043(4) 0.077(6) -0.014(4) 0.011(5) -0.006(4) N7 0.048(5) 0.057(5) 0.069(6) -0.011(5) 0.013(4) -0.015(4) N8 0.058(6) 0.041(5) 0.089(6) -0.012(4) 0.009(5) -0.016(4) N9 0.064(6) 0.062(6) 0.080(6) -0.026(5) -0.001(5) -0.028(5) N10 0.075(7) 0.067(6) 0.080(6) -0.015(5) -0.004(5) -0.014(5) P1 0.121(4) 0.073(2) 0.099(3) -0.027(2) -0.029(3) 0.014(2) P2 0.194(8) 0.100(5) 0.140(7) -0.053(4) -0.063(6) 0.045(5) P3 0.067(6) 0.092(6) 0.201(10) -0.033(6) 0.020(7) -0.032(5) C1 0.071(8) 0.057(7) 0.060(7) -0.014(6) -0.011(6) -0.014(6) C2 0.107(11) 0.077(8) 0.060(7) 0.008(7) -0.006(7) -0.022(8) C3 0.102(11) 0.069(8) 0.084(10) 0.001(7) -0.022(8) -0.017(8) C4 0.078(9) 0.057(7) 0.074(8) -0.002(6) -0.009(7) -0.018(6) C5 0.060(8) 0.062(7) 0.078(8) -0.016(6) -0.009(6) -0.031(6) C6 0.060(8) 0.063(7) 0.087(9) -0.012(7) -0.012(7) -0.023(6) C7 0.052(8) 0.062(7) 0.103(10) -0.016(7) -0.004(7) -0.013(6) C8 0.069(9) 0.074(9) 0.134(12) -0.010(8) 0.002(9) -0.019(7) C9 0.058(9) 0.090(9) 0.121(11) -0.018(9) 0.021(8) -0.004(7) C10 0.059(8) 0.070(8) 0.118(11) -0.004(7) 0.009(8) -0.024(7) C11 0.080(10) 0.054(7) 0.104(11) 0.003(7) -0.020(8) -0.008(7) C12 0.073(10) 0.073(9) 0.119(12) -0.012(9) -0.013(9) -0.014(7) C13 0.068(8) 0.055(6) 0.060(7) -0.012(6) -0.006(6) -0.022(6) C14 0.080(9) 0.073(8) 0.077(8) -0.021(7) 0.017(7) -0.022(7) C15 0.093(10) 0.069(8) 0.064(8) -0.010(6) -0.002(7) -0.028(7) C16 0.075(9) 0.057(7) 0.104(9) -0.024(6) 0.012(7) -0.004(6) C17 0.068(8) 0.064(7) 0.076(8) -0.018(6) 0.013(6) -0.023(6) C18 0.082(10) 0.066(8) 0.103(10) -0.008(7) 0.005(8) -0.032(7) C19 0.097(12) 0.095(11) 0.126(13) 0.010(9) 0.017(10) -0.011(9) C20 0.090(11) 0.102(11) 0.116(12) -0.036(10) 0.006(9) -0.004(9) C21 0.093(11) 0.083(10) 0.113(11) -0.031(9) 0.007(9) -0.015(8) C22 0.057(7) 0.045(6) 0.076(8) -0.017(6) 0.014(6) -0.016(5) C23 0.077(9) 0.061(7) 0.097(9) -0.005(7) -0.001(8) -0.025(6) C24 0.069(8) 0.057(7) 0.086(9) 0.009(6) 0.014(7) -0.011(6) C25 0.049(7) 0.061(7) 0.077(8) -0.005(6) 0.008(6) -0.019(5) C26 0.045(7) 0.065(7) 0.071(7) -0.019(6) 0.009(6) -0.014(5) C27 0.040(6) 0.064(6) 0.067(7) -0.023(6) 0.000(5) -0.017(5) C28 0.046(7) 0.073(7) 0.087(8) -0.017(7) 0.005(6) -0.011(6) C29 0.053(8) 0.094(9) 0.092(9) -0.025(7) -0.011(6) -0.029(7) C30 0.071(9) 0.080(8) 0.101(9) -0.014(7) -0.006(7) -0.046(7) C31 0.047(7) 0.062(7) 0.089(8) -0.007(6) 0.007(6) -0.016(6) C32 0.065(8) 0.080(8) 0.081(8) 0.000(7) -0.002(7) 0.000(7) C33 0.064(8) 0.084(9) 0.080(8) -0.017(7) -0.004(6) -0.006(7) C34 0.067(8) 0.058(7) 0.077(8) -0.011(6) 0.010(6) -0.021(6) C35 0.083(9) 0.060(7) 0.102(10) -0.027(7) 0.006(8) -0.027(7) C36 0.078(9) 0.046(6) 0.097(9) -0.015(6) 0.006(7) -0.035(6) C37 0.076(8) 0.060(7) 0.082(8) -0.019(6) -0.005(6) -0.019(6) C38 0.065(8) 0.060(7) 0.074(8) -0.012(6) -0.008(7) -0.023(6) C39 0.082(10) 0.073(8) 0.100(10) -0.009(7) 0.002(8) -0.035(8) C40 0.059(9) 0.088(9) 0.108(10) -0.012(8) 0.014(7) -0.019(7) C41 0.078(10) 0.079(9) 0.100(10) -0.016(8) -0.006(8) -0.005(7) C42 0.088(11) 0.076(9) 0.089(10) -0.008(7) -0.007(8) -0.007(8) _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 Ni1 N1 1.999(8) . ? Ni1 N6 2.022(8) . ? Ni1 C13 2.068(12) . ? Ni1 C34 2.075(11) . ? Ni1 N7 2.223(8) . ? Ni1 N2 2.233(10) . ? F1 P1 1.448(11) . ? F2 P1 1.528(11) . ? F3 P1 1.528(10) . ? F4 P1 1.448(12) . ? F5 P1 1.526(8) . ? F6 P1 1.488(14) . ? F7 P2 1.600(11) . ? F8 P2 1.618(13) . ? F9 P2 1.524(10) . ? F10 P3 1.62(3) . ? F11 P3 1.59(3) . ? F12 P3 1.52(2) . ? F13 P3 1.48(3) . ? F14 P3 1.45(2) . ? F15 P3 1.58(2) . ? N1 C1 1.311(12) . ? N1 C5 1.356(13) . ? N2 C10 1.311(13) . ? N2 C6 1.344(12) . ? N3 C13 1.398(12) . ? N3 C1 1.405(13) . ? N3 C15 1.414(13) . ? N4 C13 1.319(12) . ? N4 C14 1.358(13) . ? N4 C16 1.470(12) . ? N5 C21 1.335(15) . ? N5 C17 1.346(12) . ? N6 C26 1.288(12) . ? N6 C22 1.314(11) . ? N7 C31 1.312(11) . ? N7 C27 1.330(11) . ? N8 C34 1.379(11) . ? N8 C36 1.393(12) . ? N8 C22 1.413(12) . ? N9 C34 1.333(12) . ? N9 C35 1.393(12) . ? N9 C37 1.413(12) . ? N10 C38 1.321(12) . ? N10 C42 1.347(14) . ? P2 F9 1.524(10) 2_777 ? P2 F7 1.600(11) 2_777 ? P2 F8 1.618(13) 2_777 ? C1 C2 1.369(14) . ? C2 C3 1.405(16) . ? C2 H2 0.9300 . ? C3 C4 1.390(16) . ? C3 H3 0.9300 . ? C4 C11 1.414(16) . ? C4 C5 1.422(14) . ? C5 C6 1.391(14) . ? C6 C7 1.443(15) . ? C7 C8 1.352(15) . ? C7 C12 1.426(16) . ? C8 C9 1.320(15) . ? C8 H8 0.9300 . ? C9 C10 1.451(16) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.251(15) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C15 1.313(13) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.500(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.351(13) . ? C18 C19 1.432(18) . ? C18 H18 0.9300 . ? C19 C20 1.374(18) . ? C19 H19 0.9300 . ? C20 C21 1.411(17) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.385(13) . ? C23 C24 1.338(14) . ? C23 H23 0.9300 . ? C24 C25 1.434(14) . ? C24 H24 0.9300 . ? C25 C26 1.416(13) . ? C25 C32 1.423(14) . ? C26 C27 1.452(13) . ? C27 C28 1.390(13) . ? C28 C29 1.418(14) . ? C28 C33 1.491(14) . ? C29 C30 1.295(14) . ? C29 H29 0.9300 . ? C30 C31 1.391(14) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.334(14) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C35 C36 1.277(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.511(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.369(15) . ? C39 C40 1.394(15) . ? C39 H39 0.9300 . ? C40 C41 1.312(15) . ? C40 H40 0.9300 . ? C41 C42 1.340(16) . ? C41 H41 0.9300 . ? C42 H42 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 Ni1 N6 172.6(3) . . ? N1 Ni1 C13 77.4(4) . . ? N6 Ni1 C13 106.8(4) . . ? N1 Ni1 C34 108.4(4) . . ? N6 Ni1 C34 77.7(4) . . ? C13 Ni1 C34 93.9(4) . . ? N1 Ni1 N7 97.5(3) . . ? N6 Ni1 N7 76.2(3) . . ? C13 Ni1 N7 94.1(3) . . ? C34 Ni1 N7 153.9(4) . . ? N1 Ni1 N2 76.2(4) . . ? N6 Ni1 N2 99.2(3) . . ? C13 Ni1 N2 153.4(4) . . ? C34 Ni1 N2 97.2(4) . . ? N7 Ni1 N2 86.3(3) . . ? C1 N1 C5 118.4(9) . . ? C1 N1 Ni1 122.6(7) . . ? C5 N1 Ni1 118.8(8) . . ? C10 N2 C6 119.7(11) . . ? C10 N2 Ni1 129.3(8) . . ? C6 N2 Ni1 111.0(8) . . ? C13 N3 C1 120.6(10) . . ? C13 N3 C15 109.8(9) . . ? C1 N3 C15 129.6(10) . . ? C13 N4 C14 112.5(9) . . ? C13 N4 C16 121.0(10) . . ? C14 N4 C16 126.4(11) . . ? C21 N5 C17 116.6(11) . . ? C26 N6 C22 120.1(9) . . ? C26 N6 Ni1 119.6(7) . . ? C22 N6 Ni1 120.2(7) . . ? C31 N7 C27 118.4(9) . . ? C31 N7 Ni1 130.8(7) . . ? C27 N7 Ni1 110.9(6) . . ? C34 N8 C36 111.6(9) . . ? C34 N8 C22 119.6(8) . . ? C36 N8 C22 128.7(9) . . ? C34 N9 C35 109.4(9) . . ? C34 N9 C37 121.7(8) . . ? C35 N9 C37 128.4(10) . . ? C38 N10 C42 117.8(11) . . ? F4 P1 F1 83.6(8) . . ? F4 P1 F6 172.8(10) . . ? F1 P1 F6 93.1(11) . . ? F4 P1 F5 86.1(7) . . ? F1 P1 F5 93.8(6) . . ? F6 P1 F5 87.8(7) . . ? F4 P1 F3 95.1(8) . . ? F1 P1 F3 87.5(7) . . ? F6 P1 F3 91.1(8) . . ? F5 P1 F3 178.3(6) . . ? F4 P1 F2 93.3(10) . . ? F1 P1 F2 176.9(10) . . ? F6 P1 F2 90.0(9) . . ? F5 P1 F2 86.6(6) . . ? F3 P1 F2 92.2(7) . . ? F9 P2 F9 180.000(6) 2_777 . ? F9 P2 F7 87.9(7) 2_777 . ? F9 P2 F7 92.1(7) . . ? F9 P2 F7 92.1(7) 2_777 2_777 ? F9 P2 F7 87.9(7) . 2_777 ? F7 P2 F7 180.000(5) . 2_777 ? F9 P2 F8 87.0(7) 2_777 2_777 ? F9 P2 F8 93.0(7) . 2_777 ? F7 P2 F8 95.9(7) . 2_777 ? F7 P2 F8 84.1(7) 2_777 2_777 ? F9 P2 F8 93.0(7) 2_777 . ? F9 P2 F8 87.0(7) . . ? F7 P2 F8 84.1(7) . . ? F7 P2 F8 95.9(7) 2_777 . ? F8 P2 F8 180.000(5) 2_777 . ? F14 P3 F13 86.9(12) . . ? F14 P3 F12 178.6(13) . . ? F13 P3 F12 91.7(14) . . ? F14 P3 F15 93.4(12) . . ? F13 P3 F15 176.4(17) . . ? F12 P3 F15 88.0(11) . . ? F14 P3 F11 92.2(14) . . ? F13 P3 F11 93.6(15) . . ? F12 P3 F11 88.0(16) . . ? F15 P3 F11 90.0(13) . . ? F14 P3 F10 91.9(15) . . ? F13 P3 F10 102.3(16) . . ? F12 P3 F10 88.3(15) . . ? F15 P3 F10 74.0(15) . . ? F11 P3 F10 163.8(15) . . ? N1 C1 C2 125.9(11) . . ? N1 C1 N3 109.0(9) . . ? C2 C1 N3 125.1(12) . . ? C1 C2 C3 114.2(12) . . ? C1 C2 H2 122.9 . . ? C3 C2 H2 122.9 . . ? C4 C3 C2 124.7(11) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C3 C4 C11 129.8(12) . . ? C3 C4 C5 113.5(11) . . ? C11 C4 C5 116.7(12) . . ? N1 C5 C6 116.7(10) . . ? N1 C5 C4 123.2(11) . . ? C6 C5 C4 120.1(12) . . ? N2 C6 C5 117.3(11) . . ? N2 C6 C7 122.3(12) . . ? C5 C6 C7 120.4(11) . . ? C8 C7 C12 129.2(13) . . ? C8 C7 C6 115.7(12) . . ? C12 C7 C6 115.1(12) . . ? C9 C8 C7 123.1(13) . . ? C9 C8 H8 118.5 . . ? C7 C8 H8 118.5 . . ? C8 C9 C10 119.0(13) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 120.1(11) . . ? N2 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C4 123.4(13) . . ? C12 C11 H11 118.3 . . ? C4 C11 H11 118.3 . . ? C11 C12 C7 124.3(14) . . ? C11 C12 H12 117.8 . . ? C7 C12 H12 117.8 . . ? N4 C13 N3 103.3(9) . . ? N4 C13 Ni1 146.2(8) . . ? N3 C13 Ni1 110.2(8) . . ? C15 C14 N4 109.5(11) . . ? C15 C14 H14 125.3 . . ? N4 C14 H14 125.3 . . ? C14 C15 N3 104.9(10) . . ? C14 C15 H15 127.5 . . ? N3 C15 H15 127.5 . . ? N4 C16 C17 115.1(9) . . ? N4 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? N4 C16 H16B 108.5 . . ? C17 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N5 C17 C18 125.3(11) . . ? N5 C17 C16 119.2(10) . . ? C18 C17 C16 115.5(10) . . ? C17 C18 C19 115.0(11) . . ? C17 C18 H18 122.5 . . ? C19 C18 H18 122.5 . . ? C20 C19 C18 124.1(13) . . ? C20 C19 H19 118.0 . . ? C18 C19 H19 118.0 . . ? C19 C20 C21 112.7(14) . . ? C19 C20 H20 123.6 . . ? C21 C20 H20 123.6 . . ? N5 C21 C20 126.3(13) . . ? N5 C21 H21 116.8 . . ? C20 C21 H21 116.8 . . ? N6 C22 C23 121.1(10) . . ? N6 C22 N8 111.2(9) . . ? C23 C22 N8 127.6(9) . . ? C24 C23 C22 120.4(10) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.7(10) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C32 120.8(10) . . ? C26 C25 C24 114.0(10) . . ? C32 C25 C24 124.9(10) . . ? N6 C26 C25 124.5(9) . . ? N6 C26 C27 116.5(9) . . ? C25 C26 C27 119.0(10) . . ? N7 C27 C28 123.2(9) . . ? N7 C27 C26 116.8(9) . . ? C28 C27 C26 120.0(10) . . ? C27 C28 C29 116.2(10) . . ? C27 C28 C33 118.3(10) . . ? C29 C28 C33 125.4(11) . . ? C30 C29 C28 119.4(11) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 121.4(10) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? N7 C31 C30 121.5(10) . . ? N7 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C25 120.4(11) . . ? C33 C32 H32 119.8 . . ? C25 C32 H32 119.8 . . ? C32 C33 C28 121.4(11) . . ? C32 C33 H33 119.3 . . ? C28 C33 H33 119.3 . . ? N9 C34 N8 103.4(9) . . ? N9 C34 Ni1 145.1(8) . . ? N8 C34 Ni1 111.2(8) . . ? C36 C35 N9 110.8(11) . . ? C36 C35 H35 124.6 . . ? N9 C35 H35 124.6 . . ? C35 C36 N8 104.7(10) . . ? C35 C36 H36 127.6 . . ? N8 C36 H36 127.6 . . ? N9 C37 C38 112.8(9) . . ? N9 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? N9 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N10 C38 C39 121.1(11) . . ? N10 C38 C37 115.4(11) . . ? C39 C38 C37 123.5(11) . . ? C38 C39 C40 118.7(11) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? C41 C40 C39 119.7(13) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 119.2(13) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C41 C42 N10 123.3(12) . . ? C41 C42 H42 118.3 . . ? N10 C42 H42 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ni1 N1 C1 125(3) . . . . ? C13 Ni1 N1 C1 -0.6(7) . . . . ? C34 Ni1 N1 C1 -90.6(8) . . . . ? N7 Ni1 N1 C1 91.9(8) . . . . ? N2 Ni1 N1 C1 176.3(8) . . . . ? N6 Ni1 N1 C5 -51(3) . . . . ? C13 Ni1 N1 C5 -176.1(7) . . . . ? C34 Ni1 N1 C5 94.0(7) . . . . ? N7 Ni1 N1 C5 -83.5(7) . . . . ? N2 Ni1 N1 C5 0.8(6) . . . . ? N1 Ni1 N2 C10 -177.5(9) . . . . ? N6 Ni1 N2 C10 -3.4(9) . . . . ? C13 Ni1 N2 C10 -170.7(9) . . . . ? C34 Ni1 N2 C10 75.2(9) . . . . ? N7 Ni1 N2 C10 -78.8(9) . . . . ? N1 Ni1 N2 C6 -0.2(6) . . . . ? N6 Ni1 N2 C6 173.9(6) . . . . ? C13 Ni1 N2 C6 6.6(11) . . . . ? C34 Ni1 N2 C6 -107.5(7) . . . . ? N7 Ni1 N2 C6 98.5(7) . . . . ? N1 Ni1 N6 C26 -35(3) . . . . ? C13 Ni1 N6 C26 88.9(8) . . . . ? C34 Ni1 N6 C26 179.3(8) . . . . ? N7 Ni1 N6 C26 -1.3(7) . . . . ? N2 Ni1 N6 C26 -85.2(8) . . . . ? N1 Ni1 N6 C22 148(3) . . . . ? C13 Ni1 N6 C22 -88.3(8) . . . . ? C34 Ni1 N6 C22 2.1(7) . . . . ? N7 Ni1 N6 C22 -178.5(8) . . . . ? N2 Ni1 N6 C22 97.6(7) . . . . ? N1 Ni1 N7 C31 -3.4(9) . . . . ? N6 Ni1 N7 C31 -179.3(9) . . . . ? C13 Ni1 N7 C31 74.5(9) . . . . ? C34 Ni1 N7 C31 -177.8(9) . . . . ? N2 Ni1 N7 C31 -78.9(9) . . . . ? N1 Ni1 N7 C27 176.7(7) . . . . ? N6 Ni1 N7 C27 0.8(6) . . . . ? C13 Ni1 N7 C27 -105.5(7) . . . . ? C34 Ni1 N7 C27 2.2(12) . . . . ? N2 Ni1 N7 C27 101.2(7) . . . . ? C5 N1 C1 C2 -2.7(15) . . . . ? Ni1 N1 C1 C2 -178.1(8) . . . . ? C5 N1 C1 N3 178.0(8) . . . . ? Ni1 N1 C1 N3 2.6(11) . . . . ? C13 N3 C1 N1 -4.0(12) . . . . ? C15 N3 C1 N1 178.5(9) . . . . ? C13 N3 C1 C2 176.6(9) . . . . ? C15 N3 C1 C2 -0.9(17) . . . . ? N1 C1 C2 C3 0.5(16) . . . . ? N3 C1 C2 C3 179.7(10) . . . . ? C1 C2 C3 C4 2.9(18) . . . . ? C2 C3 C4 C11 176.0(12) . . . . ? C2 C3 C4 C5 -3.6(17) . . . . ? C1 N1 C5 C6 -177.0(9) . . . . ? Ni1 N1 C5 C6 -1.4(11) . . . . ? C1 N1 C5 C4 1.7(14) . . . . ? Ni1 N1 C5 C4 177.3(7) . . . . ? C3 C4 C5 N1 1.2(15) . . . . ? C11 C4 C5 N1 -178.4(9) . . . . ? C3 C4 C5 C6 179.9(9) . . . . ? C11 C4 C5 C6 0.3(15) . . . . ? C10 N2 C6 C5 177.2(9) . . . . ? Ni1 N2 C6 C5 -0.4(11) . . . . ? C10 N2 C6 C7 -0.2(15) . . . . ? Ni1 N2 C6 C7 -177.8(8) . . . . ? N1 C5 C6 N2 1.2(13) . . . . ? C4 C5 C6 N2 -177.6(9) . . . . ? N1 C5 C6 C7 178.6(9) . . . . ? C4 C5 C6 C7 -0.1(15) . . . . ? N2 C6 C7 C8 -1.9(15) . . . . ? C5 C6 C7 C8 -179.2(10) . . . . ? N2 C6 C7 C12 178.5(9) . . . . ? C5 C6 C7 C12 1.2(15) . . . . ? C12 C7 C8 C9 -177.0(12) . . . . ? C6 C7 C8 C9 3.4(18) . . . . ? C7 C8 C9 C10 -3(2) . . . . ? C6 N2 C10 C9 0.9(16) . . . . ? Ni1 N2 C10 C9 178.0(8) . . . . ? C8 C9 C10 N2 0.5(18) . . . . ? C3 C4 C11 C12 178.7(13) . . . . ? C5 C4 C11 C12 -1.7(18) . . . . ? C4 C11 C12 C7 3(2) . . . . ? C8 C7 C12 C11 177.7(13) . . . . ? C6 C7 C12 C11 -2.7(18) . . . . ? C14 N4 C13 N3 2.4(11) . . . . ? C16 N4 C13 N3 178.4(8) . . . . ? C14 N4 C13 Ni1 175.8(10) . . . . ? C16 N4 C13 Ni1 -8.2(19) . . . . ? C1 N3 C13 N4 179.7(8) . . . . ? C15 N3 C13 N4 -2.4(10) . . . . ? C1 N3 C13 Ni1 3.6(11) . . . . ? C15 N3 C13 Ni1 -178.5(6) . . . . ? N1 Ni1 C13 N4 -174.7(14) . . . . ? N6 Ni1 C13 N4 11.6(14) . . . . ? C34 Ni1 C13 N4 -66.7(14) . . . . ? N7 Ni1 C13 N4 88.5(14) . . . . ? N2 Ni1 C13 N4 178.6(10) . . . . ? N1 Ni1 C13 N3 -1.5(6) . . . . ? N6 Ni1 C13 N3 -175.2(6) . . . . ? C34 Ni1 C13 N3 106.5(7) . . . . ? N7 Ni1 C13 N3 -98.3(6) . . . . ? N2 Ni1 C13 N3 -8.3(12) . . . . ? C13 N4 C14 C15 -1.6(13) . . . . ? C16 N4 C14 C15 -177.3(10) . . . . ? N4 C14 C15 N3 0.0(12) . . . . ? C13 N3 C15 C14 1.5(11) . . . . ? C1 N3 C15 C14 179.2(10) . . . . ? C13 N4 C16 C17 -78.6(13) . . . . ? C14 N4 C16 C17 96.8(12) . . . . ? C21 N5 C17 C18 0.3(17) . . . . ? C21 N5 C17 C16 -178.7(10) . . . . ? N4 C16 C17 N5 -10.5(15) . . . . ? N4 C16 C17 C18 170.4(10) . . . . ? N5 C17 C18 C19 1.6(18) . . . . ? C16 C17 C18 C19 -179.4(10) . . . . ? C17 C18 C19 C20 -3(2) . . . . ? C18 C19 C20 C21 2(2) . . . . ? C17 N5 C21 C20 -1.1(19) . . . . ? C19 C20 C21 N5 0(2) . . . . ? C26 N6 C22 C23 -0.8(15) . . . . ? Ni1 N6 C22 C23 176.5(8) . . . . ? C26 N6 C22 N8 -178.4(9) . . . . ? Ni1 N6 C22 N8 -1.2(11) . . . . ? C34 N8 C22 N6 -1.2(13) . . . . ? C36 N8 C22 N6 173.7(9) . . . . ? C34 N8 C22 C23 -178.7(10) . . . . ? C36 N8 C22 C23 -3.7(17) . . . . ? N6 C22 C23 C24 0.8(17) . . . . ? N8 C22 C23 C24 178.1(10) . . . . ? C22 C23 C24 C25 1.1(17) . . . . ? C23 C24 C25 C26 -2.8(15) . . . . ? C23 C24 C25 C32 -176.9(11) . . . . ? C22 N6 C26 C25 -1.3(15) . . . . ? Ni1 N6 C26 C25 -178.6(8) . . . . ? C22 N6 C26 C27 178.8(8) . . . . ? Ni1 N6 C26 C27 1.6(12) . . . . ? C32 C25 C26 N6 177.4(10) . . . . ? C24 C25 C26 N6 3.1(15) . . . . ? C32 C25 C26 C27 -2.7(15) . . . . ? C24 C25 C26 C27 -177.1(9) . . . . ? C31 N7 C27 C28 -3.0(14) . . . . ? Ni1 N7 C27 C28 176.9(8) . . . . ? C31 N7 C27 C26 179.7(9) . . . . ? Ni1 N7 C27 C26 -0.3(10) . . . . ? N6 C26 C27 N7 -0.8(13) . . . . ? C25 C26 C27 N7 179.4(9) . . . . ? N6 C26 C27 C28 -178.1(9) . . . . ? C25 C26 C27 C28 2.1(14) . . . . ? N7 C27 C28 C29 3.3(15) . . . . ? C26 C27 C28 C29 -179.6(9) . . . . ? N7 C27 C28 C33 -179.3(9) . . . . ? C26 C27 C28 C33 -2.2(15) . . . . ? C27 C28 C29 C30 -2.0(16) . . . . ? C33 C28 C29 C30 -179.3(11) . . . . ? C28 C29 C30 C31 0.7(19) . . . . ? C27 N7 C31 C30 1.6(15) . . . . ? Ni1 N7 C31 C30 -178.4(8) . . . . ? C29 C30 C31 N7 -0.5(18) . . . . ? C26 C25 C32 C33 3.7(17) . . . . ? C24 C25 C32 C33 177.4(10) . . . . ? C25 C32 C33 C28 -3.8(17) . . . . ? C27 C28 C33 C32 3.2(16) . . . . ? C29 C28 C33 C32 -179.7(11) . . . . ? C35 N9 C34 N8 -2.6(11) . . . . ? C37 N9 C34 N8 -175.8(9) . . . . ? C35 N9 C34 Ni1 169.1(11) . . . . ? C37 N9 C34 Ni1 -4(2) . . . . ? C36 N8 C34 N9 2.0(11) . . . . ? C22 N8 C34 N9 177.7(8) . . . . ? C36 N8 C34 Ni1 -173.0(7) . . . . ? C22 N8 C34 Ni1 2.8(11) . . . . ? N1 Ni1 C34 N9 10.6(15) . . . . ? N6 Ni1 C34 N9 -173.8(15) . . . . ? C13 Ni1 C34 N9 -67.5(14) . . . . ? N7 Ni1 C34 N9 -175.2(10) . . . . ? N2 Ni1 C34 N9 88.4(14) . . . . ? N1 Ni1 C34 N8 -178.1(7) . . . . ? N6 Ni1 C34 N8 -2.4(7) . . . . ? C13 Ni1 C34 N8 103.9(7) . . . . ? N7 Ni1 C34 N8 -3.9(13) . . . . ? N2 Ni1 C34 N8 -100.3(7) . . . . ? C34 N9 C35 C36 2.5(14) . . . . ? C37 N9 C35 C36 175.2(11) . . . . ? N9 C35 C36 N8 -1.2(13) . . . . ? C34 N8 C36 C35 -0.5(13) . . . . ? C22 N8 C36 C35 -175.7(10) . . . . ? C34 N9 C37 C38 -73.0(13) . . . . ? C35 N9 C37 C38 115.2(11) . . . . ? C42 N10 C38 C39 1.9(15) . . . . ? C42 N10 C38 C37 -179.6(9) . . . . ? N9 C37 C38 N10 158.8(9) . . . . ? N9 C37 C38 C39 -22.7(14) . . . . ? N10 C38 C39 C40 -0.5(16) . . . . ? C37 C38 C39 C40 -179.0(10) . . . . ? C38 C39 C40 C41 1.7(18) . . . . ? C39 C40 C41 C42 -4.1(19) . . . . ? C40 C41 C42 N10 6(2) . . . . ? C38 N10 C42 C41 -4.5(18) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.616 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.104 # Attachment 'web_deposit_cif_file_1_ShaojinGu_1283865305.cif' data_080602c _database_code_depnum_ccdc_archive 'CCDC 792159' #TrackingRef 'web_deposit_cif_file_1_ShaojinGu_1283865305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 Co F18 N12 P3' _chemical_formula_weight 1250.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6398(10) _cell_length_b 13.6787(14) _cell_length_c 16.929(2) _cell_angle_alpha 81.067(2) _cell_angle_beta 73.9700(10) _cell_angle_gamma 81.180(2) _cell_volume 2541.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_T_max 0.8531 _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 12406 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.1216 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8655 _reflns_number_gt 4294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1000P)^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 8655 _refine_ls_number_parameters 761 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2115 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Co1 Co 0.73926(7) 0.74961(5) 0.70022(5) 0.0342(3) Uani 1 1 d . . . F1 F 0.1218(5) 0.6903(4) 0.5634(3) 0.1115(18) Uani 1 1 d . . . F2 F 0.3172(6) 0.5439(4) 0.4585(3) 0.147(3) Uani 1 1 d . . . F3 F 0.1248(5) 0.5446(4) 0.5220(4) 0.139(2) Uani 1 1 d . . . F4 F 0.1865(4) 0.6744(3) 0.4300(3) 0.0872(14) Uani 1 1 d . . . F5 F 0.3133(5) 0.6930(4) 0.5015(4) 0.129(2) Uani 1 1 d . . . F6 F 0.2584(4) 0.5615(3) 0.5921(3) 0.0901(15) Uani 1 1 d . . . F7 F 0.2143(6) 0.9754(5) 0.1375(5) 0.182(4) Uani 1 1 d . . . F8 F 0.0275(5) 0.8228(4) 0.1835(4) 0.129(2) Uani 1 1 d . . . F9 F 0.2015(7) 0.8292(6) 0.0954(5) 0.206(4) Uani 1 1 d . . . F10 F 0.0628(5) 0.9545(4) 0.0878(3) 0.1148(18) Uani 1 1 d . . . F11 F 0.0394(7) 0.9654(5) 0.2198(4) 0.171(3) Uani 1 1 d . . . F12 F 0.1840(6) 0.8383(4) 0.2258(4) 0.145(3) Uani 1 1 d . . . F13 F 0.6075(5) 0.6230(3) 0.2412(3) 0.1166(19) Uani 1 1 d . A . F14 F 0.5893(7) 0.8346(4) 0.1365(4) 0.157(3) Uani 1 1 d . A . F15 F 0.557(2) 0.7897(12) 0.2637(9) 0.120(9) Uani 0.62(3) 1 d P A 1 F16 F 0.4637(12) 0.7385(16) 0.1864(14) 0.153(8) Uani 0.62(3) 1 d P A 1 F17 F 0.635(2) 0.6831(9) 0.1040(7) 0.123(9) Uani 0.62(3) 1 d P A 1 F18 F 0.7331(11) 0.7293(11) 0.1874(15) 0.126(7) Uani 0.62(3) 1 d P A 1 F15' F 0.668(4) 0.768(2) 0.240(2) 0.146(17) Uani 0.38(3) 1 d P A 2 F16' F 0.4816(19) 0.7367(16) 0.2631(14) 0.099(10) Uani 0.38(3) 1 d P A 2 F17' F 0.519(3) 0.6729(17) 0.1497(17) 0.108(10) Uani 0.38(3) 1 d P A 2 F18' F 0.707(2) 0.696(2) 0.1240(19) 0.145(13) Uani 0.38(3) 1 d P A 2 N1 N 0.5934(4) 0.6125(4) 0.6887(3) 0.0381(12) Uani 1 1 d . . . N2 N 0.4968(4) 0.7541(4) 0.6565(3) 0.0430(13) Uani 1 1 d . . . N3 N 0.7642(4) 0.6108(3) 0.7241(3) 0.0345(11) Uani 1 1 d . . . N4 N 0.8975(4) 0.7398(3) 0.7295(3) 0.0351(12) Uani 1 1 d . . . N5 N 0.3553(5) 0.8224(4) 0.7955(3) 0.0554(15) Uani 1 1 d . . . N6 N 0.6258(4) 0.8959(3) 0.8031(3) 0.0373(12) Uani 1 1 d . . . N7 N 0.6054(4) 0.7606(3) 0.8865(3) 0.0400(12) Uani 1 1 d . . . N8 N 0.7248(4) 0.8876(3) 0.6699(3) 0.0364(12) Uani 1 1 d . . . N9 N 0.8230(4) 0.7502(3) 0.5770(3) 0.0349(12) Uani 1 1 d . . . N10 N 0.4657(5) 0.5797(4) 0.8769(3) 0.0526(14) Uani 1 1 d . . . N11 N 0.5834(8) 0.8522(7) 0.4575(5) 0.115(3) Uani 1 1 d . . . N12' N 0.8750(10) 0.6618(10) 0.9367(7) 0.128(6) Uani 0.76(2) 1 d P B 2 P1 P 0.22046(17) 0.61605(14) 0.51124(12) 0.0544(5) Uani 1 1 d . . . P2 P 0.1253(2) 0.89837(15) 0.15594(13) 0.0641(6) Uani 1 1 d . . . P3 P 0.5978(2) 0.73014(15) 0.18747(13) 0.0644(6) Uani 1 1 d . . . C1 C 0.5951(5) 0.7150(5) 0.6819(3) 0.0401(15) Uani 1 1 d . . . C2 C 0.4313(6) 0.6787(6) 0.6508(4) 0.0575(19) Uani 1 1 d . . . H2 H 0.3585 0.6881 0.6363 0.069 Uiso 1 1 calc R . . C3 C 0.4921(6) 0.5909(5) 0.6697(4) 0.0516(17) Uani 1 1 d . . . H3 H 0.4707 0.5280 0.6701 0.062 Uiso 1 1 calc R . . C4 C 0.6884(5) 0.5528(4) 0.7148(3) 0.0359(14) Uani 1 1 d . . . C5 C 0.7115(6) 0.4485(4) 0.7267(4) 0.0453(16) Uani 1 1 d . . . H5 H 0.6578 0.4084 0.7202 0.054 Uiso 1 1 calc R . . C6 C 0.8161(7) 0.4071(5) 0.7483(4) 0.0532(18) Uani 1 1 d . . . H6 H 0.8316 0.3382 0.7584 0.064 Uiso 1 1 calc R . . C7 C 0.9008(6) 0.4679(4) 0.7553(4) 0.0419(15) Uani 1 1 d . . . C8 C 0.8682(5) 0.5717(4) 0.7419(3) 0.0332(14) Uani 1 1 d . . . C9 C 0.9432(5) 0.6420(4) 0.7459(3) 0.0349(14) Uani 1 1 d . . . C10 C 1.0504(5) 0.6108(5) 0.7662(4) 0.0458(16) Uani 1 1 d . . . C11 C 1.1181(6) 0.6874(6) 0.7708(4) 0.0558(19) Uani 1 1 d . . . H11 H 1.1917 0.6715 0.7841 0.067 Uiso 1 1 calc R . . C12 C 1.0726(6) 0.7843(5) 0.7555(4) 0.0531(18) Uani 1 1 d . . . H12 H 1.1157 0.8348 0.7589 0.064 Uiso 1 1 calc R . . C13 C 0.9641(5) 0.8091(5) 0.7352(4) 0.0447(16) Uani 1 1 d . . . H13 H 0.9361 0.8761 0.7252 0.054 Uiso 1 1 calc R . . C14 C 1.0125(6) 0.4367(5) 0.7760(4) 0.0559(19) Uani 1 1 d . . . H14 H 1.0368 0.3690 0.7866 0.067 Uiso 1 1 calc R . . C15 C 1.0842(6) 0.5044(5) 0.7805(4) 0.060(2) Uani 1 1 d . . . H15 H 1.1572 0.4817 0.7931 0.072 Uiso 1 1 calc R . . C16 C 0.4513(5) 0.8603(5) 0.6486(4) 0.0474(17) Uani 1 1 d . . . H16A H 0.4055 0.8735 0.6073 0.057 Uiso 1 1 calc R . . H16B H 0.5189 0.8992 0.6294 0.057 Uiso 1 1 calc R . . C17 C 0.3719(5) 0.8930(5) 0.7298(4) 0.0417(15) Uani 1 1 d . . . C18 C 0.3191(7) 0.9892(5) 0.7335(5) 0.067(2) Uani 1 1 d . . . H18 H 0.3320 1.0356 0.6865 0.081 Uiso 1 1 calc R . . C19 C 0.2464(7) 1.0164(6) 0.8078(6) 0.076(2) Uani 1 1 d . . . H19 H 0.2100 1.0816 0.8118 0.091 Uiso 1 1 calc R . . C20 C 0.2283(6) 0.9457(6) 0.8763(5) 0.065(2) Uani 1 1 d . . . H20 H 0.1798 0.9622 0.9272 0.078 Uiso 1 1 calc R . . C21 C 0.2826(6) 0.8522(6) 0.8677(4) 0.063(2) Uani 1 1 d . . . H21 H 0.2696 0.8049 0.9141 0.076 Uiso 1 1 calc R . . C22 C 0.6517(5) 0.7937(4) 0.8069(4) 0.0319(13) Uani 1 1 d . . . C23 C 0.5536(6) 0.8396(5) 0.9319(4) 0.0552(18) Uani 1 1 d . . . H23 H 0.5165 0.8349 0.9884 0.066 Uiso 1 1 calc R . . C24 C 0.5667(6) 0.9244(5) 0.8797(4) 0.0539(18) Uani 1 1 d . . . H24 H 0.5410 0.9891 0.8928 0.065 Uiso 1 1 calc R . . C25 C 0.6702(5) 0.9510(4) 0.7253(4) 0.0381(14) Uani 1 1 d . . . C26 C 0.6622(6) 1.0535(4) 0.7035(4) 0.0510(17) Uani 1 1 d . . . H26 H 0.6230 1.0968 0.7424 0.061 Uiso 1 1 calc R . . C27 C 0.7137(7) 1.0897(5) 0.6224(5) 0.061(2) Uani 1 1 d . . . H27 H 0.7093 1.1581 0.6069 0.073 Uiso 1 1 calc R . . C28 C 0.7729(6) 1.0247(4) 0.5630(4) 0.0478(17) Uani 1 1 d . . . C29 C 0.7763(5) 0.9228(4) 0.5909(4) 0.0362(14) Uani 1 1 d . . . C30 C 0.8292(5) 0.8474(4) 0.5399(4) 0.0354(14) Uani 1 1 d . . . C31 C 0.8816(6) 0.8729(5) 0.4553(4) 0.0463(16) Uani 1 1 d . . . C32 C 0.9266(6) 0.7941(5) 0.4064(4) 0.0559(18) Uani 1 1 d . . . H32 H 0.9618 0.8066 0.3500 0.067 Uiso 1 1 calc R . . C33 C 0.9171(6) 0.6991(5) 0.4440(4) 0.0542(18) Uani 1 1 d . . . H33 H 0.9452 0.6464 0.4124 0.065 Uiso 1 1 calc R . . C34 C 0.8658(5) 0.6786(4) 0.5296(4) 0.0416(15) Uani 1 1 d . . . H34 H 0.8621 0.6127 0.5532 0.050 Uiso 1 1 calc R . . C35 C 0.8294(7) 1.0503(5) 0.4763(5) 0.065(2) Uani 1 1 d . . . H35 H 0.8306 1.1170 0.4544 0.078 Uiso 1 1 calc R . . C36 C 0.8805(7) 0.9788(5) 0.4269(4) 0.063(2) Uani 1 1 d . . . H36 H 0.9171 0.9982 0.3717 0.076 Uiso 1 1 calc R . . C37 C 0.6049(6) 0.6545(4) 0.9250(4) 0.0472(17) Uani 1 1 d . . . H37A H 0.6262 0.6479 0.9772 0.057 Uiso 1 1 calc R . . H37B H 0.6644 0.6124 0.8888 0.057 Uiso 1 1 calc R . . C38 C 0.4828(6) 0.6216(4) 0.9394(4) 0.0413(15) Uani 1 1 d . . . C39 C 0.3930(6) 0.6342(5) 1.0110(4) 0.0571(19) Uani 1 1 d . . . H39 H 0.4074 0.6632 1.0531 0.069 Uiso 1 1 calc R . . C40 C 0.2814(7) 0.6037(5) 1.0202(5) 0.068(2) Uani 1 1 d . . . H40 H 0.2197 0.6121 1.0679 0.081 Uiso 1 1 calc R . . C41 C 0.2647(7) 0.5610(5) 0.9569(5) 0.066(2) Uani 1 1 d . . . H41 H 0.1912 0.5390 0.9612 0.079 Uiso 1 1 calc R . . C42 C 0.3568(7) 0.5508(5) 0.8876(5) 0.062(2) Uani 1 1 d . . . H42 H 0.3434 0.5222 0.8451 0.075 Uiso 1 1 calc R . . C43 C 0.5961(8) 0.7718(8) 0.4439(5) 0.079(3) Uani 1 1 d . . . C44 C 0.6115(8) 0.6694(7) 0.4275(6) 0.093(3) Uani 1 1 d . . . H44A H 0.6116 0.6260 0.4778 0.139 Uiso 1 1 calc R . . H44B H 0.6866 0.6562 0.3872 0.139 Uiso 1 1 calc R . . H44C H 0.5466 0.6581 0.4065 0.139 Uiso 1 1 calc R . . C45 C 0.9019(9) 0.7220(9) 0.9685(6) 0.101(3) Uani 1 1 d . . . C46 C 0.9269(10) 0.8044(8) 1.0008(7) 0.141(5) Uani 1 1 d . B . H46A H 0.9857 0.8393 0.9592 0.212 Uiso 1 1 calc R . . H46B H 0.9576 0.7806 1.0483 0.212 Uiso 1 1 calc R . . H46C H 0.8543 0.8487 1.0166 0.212 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 Co1 0.0392(5) 0.0354(5) 0.0269(5) 0.0048(3) -0.0079(4) -0.0103(3) F1 0.139(5) 0.098(4) 0.074(4) -0.017(3) -0.007(3) 0.024(3) F2 0.173(6) 0.174(6) 0.055(4) -0.024(3) -0.027(3) 0.103(4) F3 0.153(5) 0.086(4) 0.207(7) 0.017(4) -0.089(5) -0.059(3) F4 0.104(3) 0.100(3) 0.065(3) 0.000(2) -0.046(3) 0.003(3) F5 0.137(5) 0.142(5) 0.133(5) 0.068(4) -0.088(4) -0.081(4) F6 0.127(4) 0.093(3) 0.051(3) 0.017(2) -0.036(3) -0.017(3) F7 0.180(6) 0.181(6) 0.226(8) 0.103(6) -0.129(6) -0.130(5) F8 0.153(5) 0.123(4) 0.129(5) 0.045(4) -0.068(4) -0.072(4) F9 0.209(8) 0.234(8) 0.132(7) -0.072(6) -0.013(6) 0.099(7) F10 0.141(5) 0.123(4) 0.083(4) 0.037(3) -0.055(4) -0.026(3) F11 0.238(8) 0.121(5) 0.133(6) -0.054(5) -0.003(6) -0.003(5) F12 0.210(6) 0.114(4) 0.158(6) 0.055(4) -0.139(5) -0.064(4) F13 0.194(6) 0.078(3) 0.072(4) 0.005(3) -0.021(4) -0.034(3) F14 0.291(9) 0.078(4) 0.117(5) 0.025(3) -0.098(6) -0.019(5) F15 0.180(18) 0.102(11) 0.084(8) -0.050(7) -0.059(10) 0.051(12) F16 0.096(9) 0.184(16) 0.21(2) -0.055(13) -0.066(10) -0.024(8) F17 0.23(3) 0.092(8) 0.048(7) -0.024(5) -0.044(12) -0.003(11) F18 0.077(8) 0.135(11) 0.17(2) -0.017(11) -0.047(9) 0.000(7) F15' 0.26(5) 0.08(2) 0.15(3) 0.033(16) -0.12(3) -0.11(2) F16' 0.095(14) 0.087(13) 0.085(14) -0.001(10) 0.016(10) -0.002(9) F17' 0.14(2) 0.108(16) 0.10(2) -0.012(12) -0.071(17) -0.038(14) F18' 0.088(17) 0.23(3) 0.08(2) -0.017(18) 0.044(12) -0.016(15) N1 0.037(3) 0.049(3) 0.030(3) -0.007(2) -0.007(2) -0.012(2) N2 0.038(3) 0.062(4) 0.027(3) -0.004(2) -0.007(2) -0.005(3) N3 0.041(3) 0.035(3) 0.027(3) 0.006(2) -0.010(2) -0.007(2) N4 0.038(3) 0.038(3) 0.026(3) 0.002(2) -0.004(2) -0.009(2) N5 0.057(4) 0.059(4) 0.040(4) 0.005(3) -0.004(3) -0.001(3) N6 0.047(3) 0.033(3) 0.032(3) -0.001(2) -0.011(2) -0.006(2) N7 0.048(3) 0.044(3) 0.028(3) 0.002(2) -0.009(2) -0.012(2) N8 0.042(3) 0.034(3) 0.032(3) 0.006(2) -0.011(2) -0.006(2) N9 0.029(3) 0.046(3) 0.032(3) 0.000(2) -0.010(2) -0.011(2) N10 0.071(4) 0.056(4) 0.032(3) -0.006(3) -0.011(3) -0.010(3) N11 0.157(8) 0.112(7) 0.056(6) -0.005(5) 0.010(5) -0.031(6) N12' 0.128(10) 0.189(14) 0.071(9) -0.047(8) 0.021(7) -0.089(9) P1 0.0654(12) 0.0581(12) 0.0415(12) -0.0013(9) -0.0166(10) -0.0120(10) P2 0.0853(15) 0.0556(12) 0.0534(14) 0.0038(10) -0.0234(12) -0.0144(11) P3 0.0775(16) 0.0646(14) 0.0500(13) -0.0077(10) -0.0128(11) -0.0110(11) C1 0.044(4) 0.052(4) 0.019(3) 0.002(3) 0.001(3) -0.010(3) C2 0.046(4) 0.091(6) 0.042(4) -0.014(4) -0.013(3) -0.018(4) C3 0.049(4) 0.066(5) 0.042(4) -0.010(3) -0.004(3) -0.025(4) C4 0.045(4) 0.038(4) 0.022(3) -0.004(3) -0.003(3) -0.009(3) C5 0.069(5) 0.040(4) 0.027(4) -0.005(3) -0.006(3) -0.017(3) C6 0.083(5) 0.031(4) 0.040(4) 0.004(3) -0.013(4) -0.005(4) C7 0.054(4) 0.039(4) 0.026(4) 0.003(3) -0.003(3) -0.005(3) C8 0.040(3) 0.039(3) 0.017(3) -0.001(2) -0.007(3) 0.000(3) C9 0.039(3) 0.040(3) 0.022(3) 0.002(3) -0.005(3) -0.002(3) C10 0.039(4) 0.064(5) 0.031(4) -0.001(3) -0.009(3) -0.001(3) C11 0.037(4) 0.085(6) 0.044(4) 0.002(4) -0.015(3) -0.007(4) C12 0.046(4) 0.066(5) 0.051(5) 0.003(4) -0.013(3) -0.027(4) C13 0.045(4) 0.050(4) 0.040(4) 0.005(3) -0.013(3) -0.016(3) C14 0.066(5) 0.043(4) 0.048(5) 0.008(3) -0.012(4) 0.008(4) C15 0.054(4) 0.066(5) 0.050(5) 0.007(4) -0.015(4) 0.014(4) C16 0.035(4) 0.069(5) 0.034(4) 0.003(3) -0.011(3) -0.001(3) C17 0.032(3) 0.056(4) 0.036(4) 0.001(3) -0.008(3) -0.010(3) C18 0.076(5) 0.054(5) 0.062(6) 0.012(4) -0.010(4) -0.010(4) C19 0.072(5) 0.056(5) 0.083(7) -0.015(5) 0.007(5) -0.004(4) C20 0.059(5) 0.080(6) 0.050(5) -0.015(4) 0.002(4) -0.009(4) C21 0.062(5) 0.078(6) 0.041(5) 0.010(4) -0.010(4) -0.006(4) C22 0.027(3) 0.040(3) 0.032(4) -0.004(3) -0.011(3) -0.007(2) C23 0.074(5) 0.059(5) 0.028(4) -0.010(3) 0.000(3) -0.014(4) C24 0.066(5) 0.052(4) 0.044(5) -0.013(4) -0.009(4) -0.007(4) C25 0.040(3) 0.041(4) 0.034(4) -0.001(3) -0.009(3) -0.009(3) C26 0.067(5) 0.035(4) 0.051(5) -0.004(3) -0.017(4) -0.002(3) C27 0.088(5) 0.035(4) 0.060(5) 0.006(4) -0.028(4) -0.007(4) C28 0.062(4) 0.037(4) 0.048(4) 0.011(3) -0.023(4) -0.013(3) C29 0.043(3) 0.039(3) 0.028(4) 0.008(3) -0.014(3) -0.011(3) C30 0.038(3) 0.041(4) 0.028(3) 0.005(3) -0.012(3) -0.009(3) C31 0.053(4) 0.057(4) 0.023(4) 0.007(3) -0.004(3) -0.013(3) C32 0.060(4) 0.075(5) 0.026(4) 0.003(4) -0.002(3) -0.014(4) C33 0.058(4) 0.068(5) 0.032(4) -0.008(3) -0.001(3) -0.013(4) C34 0.042(4) 0.044(4) 0.034(4) 0.002(3) -0.005(3) -0.006(3) C35 0.095(6) 0.049(4) 0.045(5) 0.020(4) -0.017(4) -0.021(4) C36 0.084(5) 0.058(5) 0.037(4) 0.017(4) -0.006(4) -0.019(4) C37 0.062(4) 0.049(4) 0.028(4) 0.004(3) -0.014(3) -0.003(3) C38 0.058(4) 0.035(3) 0.024(4) 0.008(3) -0.007(3) -0.003(3) C39 0.077(5) 0.061(5) 0.035(4) 0.003(3) -0.016(4) -0.018(4) C40 0.064(5) 0.082(6) 0.041(5) 0.009(4) 0.009(4) -0.018(4) C41 0.070(5) 0.068(5) 0.059(6) 0.019(4) -0.022(5) -0.025(4) C42 0.079(6) 0.061(5) 0.051(5) -0.004(4) -0.020(4) -0.014(4) C43 0.085(6) 0.102(8) 0.037(5) 0.001(5) -0.004(4) -0.008(6) C44 0.110(7) 0.096(7) 0.073(7) 0.004(5) -0.032(6) -0.012(6) C45 0.108(8) 0.124(9) 0.061(7) -0.019(6) 0.026(6) -0.061(7) C46 0.177(12) 0.146(10) 0.099(10) -0.030(8) 0.012(8) -0.084(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N8 1.871(4) . ? Co1 N3 1.874(4) . ? Co1 C1 1.927(6) . ? Co1 C22 1.949(6) . ? Co1 N4 2.016(5) . ? Co1 N9 2.043(5) . ? F1 P1 1.579(5) . ? F2 P1 1.554(5) . ? F3 P1 1.547(5) . ? F4 P1 1.596(4) . ? F5 P1 1.581(5) . ? F6 P1 1.595(4) . ? F7 P2 1.528(5) . ? F8 P2 1.581(5) . ? F9 P2 1.508(6) . ? F10 P2 1.570(5) . ? F11 P2 1.562(6) . ? F12 P2 1.585(5) . ? F13 P3 1.606(5) . ? F14 P3 1.555(5) . ? F15 P3 1.557(10) . ? F16 P3 1.552(11) . ? F17 P3 1.567(11) . ? F18 P3 1.573(12) . ? F15' P3 1.553(19) . ? F16' P3 1.587(14) . ? F17' P3 1.597(15) . ? F18' P3 1.486(18) . ? N1 C3 1.388(7) . ? N1 C1 1.392(7) . ? N1 C4 1.403(7) . ? N2 C1 1.339(7) . ? N2 C2 1.403(8) . ? N2 C16 1.467(7) . ? N3 C4 1.328(7) . ? N3 C8 1.340(7) . ? N4 C13 1.344(7) . ? N4 C9 1.377(7) . ? N5 C17 1.346(7) . ? N5 C21 1.362(8) . ? N6 C24 1.375(7) . ? N6 C22 1.380(6) . ? N6 C25 1.415(7) . ? N7 C22 1.340(7) . ? N7 C23 1.388(7) . ? N7 C37 1.495(7) . ? N8 C25 1.338(7) . ? N8 C29 1.352(7) . ? N9 C34 1.314(7) . ? N9 C30 1.383(6) . ? N10 C42 1.341(8) . ? N10 C38 1.351(7) . ? N11 C43 1.137(10) . ? N12' C45 1.174(12) . ? C2 C3 1.338(9) . ? C4 C5 1.404(7) . ? C5 C6 1.381(9) . ? C6 C7 1.423(8) . ? C7 C8 1.411(7) . ? C7 C14 1.425(9) . ? C8 C9 1.415(8) . ? C9 C10 1.373(8) . ? C10 C11 1.427(9) . ? C10 C15 1.448(8) . ? C11 C12 1.364(8) . ? C12 C13 1.378(8) . ? C14 C15 1.362(9) . ? C16 C17 1.519(8) . ? C17 C18 1.367(8) . ? C18 C19 1.378(10) . ? C19 C20 1.379(10) . ? C20 C21 1.348(9) . ? C23 C24 1.346(8) . ? C25 C26 1.389(8) . ? C26 C27 1.383(9) . ? C27 C28 1.408(9) . ? C28 C29 1.398(7) . ? C28 C35 1.445(9) . ? C29 C30 1.406(8) . ? C30 C31 1.404(8) . ? C31 C32 1.410(9) . ? C31 C36 1.453(8) . ? C32 C33 1.362(8) . ? C33 C34 1.407(8) . ? C35 C36 1.345(9) . ? C37 C38 1.501(8) . ? C38 C39 1.380(8) . ? C39 C40 1.386(9) . ? C40 C41 1.368(10) . ? C41 C42 1.363(10) . ? C43 C44 1.445(12) . ? C45 C46 1.425(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Co1 N3 175.7(2) . . ? N8 Co1 C1 101.6(2) . . ? N3 Co1 C1 80.4(2) . . ? N8 Co1 C22 80.3(2) . . ? N3 Co1 C22 103.5(2) . . ? C1 Co1 C22 92.0(2) . . ? N8 Co1 N4 96.25(19) . . ? N3 Co1 N4 81.8(2) . . ? C1 Co1 N4 162.1(2) . . ? C22 Co1 N4 91.2(2) . . ? N8 Co1 N9 81.7(2) . . ? N3 Co1 N9 94.53(19) . . ? C1 Co1 N9 90.4(2) . . ? C22 Co1 N9 162.0(2) . . ? N4 Co1 N9 91.94(18) . . ? C3 N1 C1 110.8(5) . . ? C3 N1 C4 133.1(5) . . ? C1 N1 C4 116.1(5) . . ? C1 N2 C2 110.6(6) . . ? C1 N2 C16 125.5(5) . . ? C2 N2 C16 123.2(5) . . ? C4 N3 C8 121.0(5) . . ? C4 N3 Co1 121.4(4) . . ? C8 N3 Co1 117.3(4) . . ? C13 N4 C9 116.1(5) . . ? C13 N4 Co1 132.4(4) . . ? C9 N4 Co1 111.4(4) . . ? C17 N5 C21 116.0(6) . . ? C24 N6 C22 111.2(5) . . ? C24 N6 C25 132.3(5) . . ? C22 N6 C25 116.3(5) . . ? C22 N7 C23 110.7(5) . . ? C22 N7 C37 127.1(5) . . ? C23 N7 C37 122.2(5) . . ? C25 N8 C29 120.0(5) . . ? C25 N8 Co1 121.5(4) . . ? C29 N8 Co1 118.4(4) . . ? C34 N9 C30 117.7(5) . . ? C34 N9 Co1 132.7(4) . . ? C30 N9 Co1 109.6(4) . . ? C42 N10 C38 116.9(6) . . ? F3 P1 F2 90.3(4) . . ? F3 P1 F1 89.7(3) . . ? F2 P1 F1 179.0(3) . . ? F3 P1 F5 177.3(4) . . ? F2 P1 F5 92.2(4) . . ? F1 P1 F5 87.7(3) . . ? F3 P1 F6 91.8(3) . . ? F2 P1 F6 89.4(3) . . ? F1 P1 F6 91.6(3) . . ? F5 P1 F6 89.0(3) . . ? F3 P1 F4 90.8(3) . . ? F2 P1 F4 90.9(3) . . ? F1 P1 F4 88.1(3) . . ? F5 P1 F4 88.4(3) . . ? F6 P1 F4 177.4(3) . . ? F9 P2 F7 96.4(5) . . ? F9 P2 F11 176.1(5) . . ? F7 P2 F11 87.5(4) . . ? F9 P2 F10 90.2(4) . . ? F7 P2 F10 91.8(3) . . ? F11 P2 F10 89.3(4) . . ? F9 P2 F8 88.9(5) . . ? F7 P2 F8 174.3(4) . . ? F11 P2 F8 87.2(4) . . ? F10 P2 F8 90.3(3) . . ? F9 P2 F12 89.7(4) . . ? F7 P2 F12 90.8(3) . . ? F11 P2 F12 90.7(4) . . ? F10 P2 F12 177.4(3) . . ? F8 P2 F12 87.1(3) . . ? F18' P3 F16 128.8(15) . . ? F18' P3 F15' 94.9(17) . . ? F16 P3 F15' 135.5(18) . . ? F18' P3 F14 90.7(10) . . ? F16 P3 F14 81.8(8) . . ? F15' P3 F14 91.0(8) . . ? F18' P3 F15 141.5(15) . . ? F16 P3 F15 88.4(8) . . ? F15' P3 F15 47.2(14) . . ? F14 P3 F15 84.4(7) . . ? F18' P3 F17 39.4(11) . . ? F16 P3 F17 89.6(9) . . ? F15' P3 F17 134.3(17) . . ? F14 P3 F17 88.4(5) . . ? F15 P3 F17 172.7(7) . . ? F18' P3 F18 52.4(12) . . ? F16 P3 F18 176.2(9) . . ? F15' P3 F18 42.8(14) . . ? F14 P3 F18 94.7(6) . . ? F15 P3 F18 89.9(8) . . ? F17 P3 F18 91.7(9) . . ? F18' P3 F16' 165.2(12) . . ? F16 P3 F16' 51.6(9) . . ? F15' P3 F16' 88.6(14) . . ? F14 P3 F16' 103.6(7) . . ? F15 P3 F16' 45.9(7) . . ? F17 P3 F16' 135.8(12) . . ? F18 P3 F16' 128.5(11) . . ? F18' P3 F17' 89.3(13) . . ? F16 P3 F17' 43.9(8) . . ? F15' P3 F17' 167.4(10) . . ? F14 P3 F17' 100.9(8) . . ? F15 P3 F17' 129.2(12) . . ? F17 P3 F17' 51.4(8) . . ? F18 P3 F17' 138.8(11) . . ? F16' P3 F17' 84.4(12) . . ? F18' P3 F13 89.5(10) . . ? F16 P3 F13 98.8(8) . . ? F15' P3 F13 88.1(8) . . ? F14 P3 F13 179.0(3) . . ? F15 P3 F13 94.9(7) . . ? F17 P3 F13 92.4(5) . . ? F18 P3 F13 84.7(6) . . ? F16' P3 F13 76.2(6) . . ? F17' P3 F13 80.1(7) . . ? N2 C1 N1 104.4(5) . . ? N2 C1 Co1 142.5(5) . . ? N1 C1 Co1 112.6(4) . . ? C3 C2 N2 107.9(6) . . ? C2 C3 N1 106.2(6) . . ? N3 C4 N1 109.2(5) . . ? N3 C4 C5 121.5(5) . . ? N1 C4 C5 129.3(6) . . ? C6 C5 C4 118.2(6) . . ? C5 C6 C7 121.2(6) . . ? C8 C7 C6 115.7(6) . . ? C8 C7 C14 116.5(6) . . ? C6 C7 C14 127.8(6) . . ? N3 C8 C7 122.4(5) . . ? N3 C8 C9 115.1(5) . . ? C7 C8 C9 122.5(5) . . ? C10 C9 N4 125.5(6) . . ? C10 C9 C8 120.3(6) . . ? N4 C9 C8 114.2(5) . . ? C9 C10 C11 116.1(6) . . ? C9 C10 C15 117.5(6) . . ? C11 C10 C15 126.4(6) . . ? C12 C11 C10 118.7(6) . . ? C11 C12 C13 121.4(6) . . ? N4 C13 C12 122.2(6) . . ? C15 C14 C7 120.9(6) . . ? C14 C15 C10 122.2(6) . . ? N2 C16 C17 112.4(5) . . ? N5 C17 C18 123.1(6) . . ? N5 C17 C16 116.5(6) . . ? C18 C17 C16 120.4(6) . . ? C17 C18 C19 119.1(7) . . ? C18 C19 C20 119.0(7) . . ? C21 C20 C19 118.5(7) . . ? C20 C21 N5 124.2(7) . . ? N7 C22 N6 104.3(5) . . ? N7 C22 Co1 142.9(4) . . ? N6 C22 Co1 112.7(4) . . ? C24 C23 N7 107.8(6) . . ? C23 C24 N6 106.0(6) . . ? N8 C25 C26 121.6(6) . . ? N8 C25 N6 109.0(5) . . ? C26 C25 N6 129.4(6) . . ? C27 C26 C25 118.4(6) . . ? C26 C27 C28 121.2(6) . . ? C29 C28 C27 116.2(6) . . ? C29 C28 C35 115.8(6) . . ? C27 C28 C35 127.9(6) . . ? N8 C29 C28 122.6(6) . . ? N8 C29 C30 113.4(5) . . ? C28 C29 C30 124.0(6) . . ? N9 C30 C31 123.5(5) . . ? N9 C30 C29 116.6(5) . . ? C31 C30 C29 119.8(5) . . ? C30 C31 C32 117.1(6) . . ? C30 C31 C36 116.1(6) . . ? C32 C31 C36 126.8(6) . . ? C33 C32 C31 118.3(6) . . ? C32 C33 C34 121.7(6) . . ? N9 C34 C33 121.7(6) . . ? C36 C35 C28 120.7(6) . . ? C35 C36 C31 123.5(6) . . ? N7 C37 C38 110.3(5) . . ? N10 C38 C39 121.9(6) . . ? N10 C38 C37 115.6(6) . . ? C39 C38 C37 122.5(6) . . ? C38 C39 C40 119.8(7) . . ? C41 C40 C39 118.1(7) . . ? C42 C41 C40 119.3(7) . . ? N10 C42 C41 124.0(7) . . ? N11 C43 C44 179.4(11) . . ? N12' C45 C46 172.7(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Co1 N3 C4 -114(3) . . . . ? C1 Co1 N3 C4 4.0(4) . . . . ? C22 Co1 N3 C4 93.7(4) . . . . ? N4 Co1 N3 C4 -177.0(4) . . . . ? N9 Co1 N3 C4 -85.6(4) . . . . ? N8 Co1 N3 C8 59(3) . . . . ? C1 Co1 N3 C8 176.7(4) . . . . ? C22 Co1 N3 C8 -93.6(4) . . . . ? N4 Co1 N3 C8 -4.2(4) . . . . ? N9 Co1 N3 C8 87.1(4) . . . . ? N8 Co1 N4 C13 7.1(5) . . . . ? N3 Co1 N4 C13 -176.8(5) . . . . ? C1 Co1 N4 C13 -173.7(6) . . . . ? C22 Co1 N4 C13 -73.3(5) . . . . ? N9 Co1 N4 C13 88.9(5) . . . . ? N8 Co1 N4 C9 -172.7(4) . . . . ? N3 Co1 N4 C9 3.5(4) . . . . ? C1 Co1 N4 C9 6.6(9) . . . . ? C22 Co1 N4 C9 106.9(4) . . . . ? N9 Co1 N4 C9 -90.8(4) . . . . ? N3 Co1 N8 C25 -152(3) . . . . ? C1 Co1 N8 C25 90.9(5) . . . . ? C22 Co1 N8 C25 0.8(4) . . . . ? N4 Co1 N8 C25 -89.4(4) . . . . ? N9 Co1 N8 C25 179.6(5) . . . . ? N3 Co1 N8 C29 25(3) . . . . ? C1 Co1 N8 C29 -92.4(4) . . . . ? C22 Co1 N8 C29 177.5(4) . . . . ? N4 Co1 N8 C29 87.3(4) . . . . ? N9 Co1 N8 C29 -3.7(4) . . . . ? N8 Co1 N9 C34 -174.8(5) . . . . ? N3 Co1 N9 C34 7.3(5) . . . . ? C1 Co1 N9 C34 -73.1(5) . . . . ? C22 Co1 N9 C34 -170.7(6) . . . . ? N4 Co1 N9 C34 89.2(5) . . . . ? N8 Co1 N9 C30 2.9(3) . . . . ? N3 Co1 N9 C30 -175.1(4) . . . . ? C1 Co1 N9 C30 104.5(4) . . . . ? C22 Co1 N9 C30 6.9(8) . . . . ? N4 Co1 N9 C30 -93.2(4) . . . . ? C2 N2 C1 N1 2.6(6) . . . . ? C16 N2 C1 N1 173.1(5) . . . . ? C2 N2 C1 Co1 173.8(6) . . . . ? C16 N2 C1 Co1 -15.7(10) . . . . ? C3 N1 C1 N2 -1.8(6) . . . . ? C4 N1 C1 N2 -179.9(5) . . . . ? C3 N1 C1 Co1 -176.1(4) . . . . ? C4 N1 C1 Co1 5.8(6) . . . . ? N8 Co1 C1 N2 0.3(7) . . . . ? N3 Co1 C1 N2 -175.9(7) . . . . ? C22 Co1 C1 N2 80.8(7) . . . . ? N4 Co1 C1 N2 -179.0(5) . . . . ? N9 Co1 C1 N2 -81.3(7) . . . . ? N8 Co1 C1 N1 171.1(4) . . . . ? N3 Co1 C1 N1 -5.1(4) . . . . ? C22 Co1 C1 N1 -108.4(4) . . . . ? N4 Co1 C1 N1 -8.2(9) . . . . ? N9 Co1 C1 N1 89.5(4) . . . . ? C1 N2 C2 C3 -2.5(7) . . . . ? C16 N2 C2 C3 -173.2(5) . . . . ? N2 C2 C3 N1 1.2(7) . . . . ? C1 N1 C3 C2 0.4(7) . . . . ? C4 N1 C3 C2 178.1(6) . . . . ? C8 N3 C4 N1 -174.3(5) . . . . ? Co1 N3 C4 N1 -1.8(6) . . . . ? C8 N3 C4 C5 2.7(8) . . . . ? Co1 N3 C4 C5 175.2(4) . . . . ? C3 N1 C4 N3 179.7(5) . . . . ? C1 N1 C4 N3 -2.8(7) . . . . ? C3 N1 C4 C5 3.0(10) . . . . ? C1 N1 C4 C5 -179.4(5) . . . . ? N3 C4 C5 C6 -0.2(8) . . . . ? N1 C4 C5 C6 176.1(6) . . . . ? C4 C5 C6 C7 -2.4(9) . . . . ? C5 C6 C7 C8 2.3(9) . . . . ? C5 C6 C7 C14 -179.3(6) . . . . ? C4 N3 C8 C7 -2.7(8) . . . . ? Co1 N3 C8 C7 -175.5(4) . . . . ? C4 N3 C8 C9 176.9(5) . . . . ? Co1 N3 C8 C9 4.1(6) . . . . ? C6 C7 C8 N3 0.2(8) . . . . ? C14 C7 C8 N3 -178.3(5) . . . . ? C6 C7 C8 C9 -179.4(5) . . . . ? C14 C7 C8 C9 2.1(8) . . . . ? C13 N4 C9 C10 -1.0(8) . . . . ? Co1 N4 C9 C10 178.8(5) . . . . ? C13 N4 C9 C8 177.9(5) . . . . ? Co1 N4 C9 C8 -2.4(6) . . . . ? N3 C8 C9 C10 178.0(5) . . . . ? C7 C8 C9 C10 -2.4(8) . . . . ? N3 C8 C9 N4 -0.9(7) . . . . ? C7 C8 C9 N4 178.7(5) . . . . ? N4 C9 C10 C11 0.5(9) . . . . ? C8 C9 C10 C11 -178.3(5) . . . . ? N4 C9 C10 C15 -179.3(5) . . . . ? C8 C9 C10 C15 1.9(8) . . . . ? C9 C10 C11 C12 0.2(9) . . . . ? C15 C10 C11 C12 -179.9(6) . . . . ? C10 C11 C12 C13 -0.5(10) . . . . ? C9 N4 C13 C12 0.7(8) . . . . ? Co1 N4 C13 C12 -179.0(5) . . . . ? C11 C12 C13 N4 0.0(10) . . . . ? C8 C7 C14 C15 -1.5(9) . . . . ? C6 C7 C14 C15 -179.8(6) . . . . ? C7 C14 C15 C10 1.2(10) . . . . ? C9 C10 C15 C14 -1.3(9) . . . . ? C11 C10 C15 C14 178.8(7) . . . . ? C1 N2 C16 C17 -84.8(7) . . . . ? C2 N2 C16 C17 84.6(7) . . . . ? C21 N5 C17 C18 -0.7(9) . . . . ? C21 N5 C17 C16 -179.1(5) . . . . ? N2 C16 C17 N5 0.2(8) . . . . ? N2 C16 C17 C18 -178.3(6) . . . . ? N5 C17 C18 C19 0.8(11) . . . . ? C16 C17 C18 C19 179.2(6) . . . . ? C17 C18 C19 C20 -0.4(12) . . . . ? C18 C19 C20 C21 -0.1(12) . . . . ? C19 C20 C21 N5 0.3(12) . . . . ? C17 N5 C21 C20 0.1(10) . . . . ? C23 N7 C22 N6 -1.0(6) . . . . ? C37 N7 C22 N6 178.2(5) . . . . ? C23 N7 C22 Co1 178.6(5) . . . . ? C37 N7 C22 Co1 -2.2(10) . . . . ? C24 N6 C22 N7 1.2(6) . . . . ? C25 N6 C22 N7 177.2(5) . . . . ? C24 N6 C22 Co1 -178.5(4) . . . . ? C25 N6 C22 Co1 -2.5(6) . . . . ? N8 Co1 C22 N7 -178.6(7) . . . . ? N3 Co1 C22 N7 -0.6(7) . . . . ? C1 Co1 C22 N7 79.9(7) . . . . ? N4 Co1 C22 N7 -82.5(7) . . . . ? N9 Co1 C22 N7 177.4(5) . . . . ? N8 Co1 C22 N6 1.0(4) . . . . ? N3 Co1 C22 N6 179.0(4) . . . . ? C1 Co1 C22 N6 -100.5(4) . . . . ? N4 Co1 C22 N6 97.1(4) . . . . ? N9 Co1 C22 N6 -3.1(9) . . . . ? C22 N7 C23 C24 0.5(7) . . . . ? C37 N7 C23 C24 -178.8(5) . . . . ? N7 C23 C24 N6 0.3(7) . . . . ? C22 N6 C24 C23 -0.9(7) . . . . ? C25 N6 C24 C23 -176.1(6) . . . . ? C29 N8 C25 C26 1.6(8) . . . . ? Co1 N8 C25 C26 178.2(4) . . . . ? C29 N8 C25 N6 -179.0(5) . . . . ? Co1 N8 C25 N6 -2.3(6) . . . . ? C24 N6 C25 N8 178.0(6) . . . . ? C22 N6 C25 N8 3.0(7) . . . . ? C24 N6 C25 C26 -2.6(11) . . . . ? C22 N6 C25 C26 -177.6(6) . . . . ? N8 C25 C26 C27 -0.9(9) . . . . ? N6 C25 C26 C27 179.8(6) . . . . ? C25 C26 C27 C28 0.2(10) . . . . ? C26 C27 C28 C29 -0.2(10) . . . . ? C26 C27 C28 C35 179.1(7) . . . . ? C25 N8 C29 C28 -1.6(8) . . . . ? Co1 N8 C29 C28 -178.4(4) . . . . ? C25 N8 C29 C30 -179.5(5) . . . . ? Co1 N8 C29 C30 3.7(6) . . . . ? C27 C28 C29 N8 0.9(9) . . . . ? C35 C28 C29 N8 -178.4(6) . . . . ? C27 C28 C29 C30 178.6(6) . . . . ? C35 C28 C29 C30 -0.8(9) . . . . ? C34 N9 C30 C31 -1.9(8) . . . . ? Co1 N9 C30 C31 -179.9(5) . . . . ? C34 N9 C30 C29 176.3(5) . . . . ? Co1 N9 C30 C29 -1.7(6) . . . . ? N8 C29 C30 N9 -1.0(7) . . . . ? C28 C29 C30 N9 -178.9(5) . . . . ? N8 C29 C30 C31 177.2(5) . . . . ? C28 C29 C30 C31 -0.7(9) . . . . ? N9 C30 C31 C32 1.9(9) . . . . ? C29 C30 C31 C32 -176.2(5) . . . . ? N9 C30 C31 C36 -179.8(5) . . . . ? C29 C30 C31 C36 2.1(8) . . . . ? C30 C31 C32 C33 -0.4(9) . . . . ? C36 C31 C32 C33 -178.5(6) . . . . ? C31 C32 C33 C34 -1.0(10) . . . . ? C30 N9 C34 C33 0.4(8) . . . . ? Co1 N9 C34 C33 177.9(4) . . . . ? C32 C33 C34 N9 1.0(10) . . . . ? C29 C28 C35 C36 0.6(10) . . . . ? C27 C28 C35 C36 -178.7(7) . . . . ? C28 C35 C36 C31 0.9(12) . . . . ? C30 C31 C36 C35 -2.3(10) . . . . ? C32 C31 C36 C35 175.8(7) . . . . ? C22 N7 C37 C38 -102.9(6) . . . . ? C23 N7 C37 C38 76.2(7) . . . . ? C42 N10 C38 C39 0.1(9) . . . . ? C42 N10 C38 C37 -179.1(5) . . . . ? N7 C37 C38 N10 91.1(6) . . . . ? N7 C37 C38 C39 -88.1(7) . . . . ? N10 C38 C39 C40 -0.2(9) . . . . ? C37 C38 C39 C40 178.9(6) . . . . ? C38 C39 C40 C41 0.5(10) . . . . ? C39 C40 C41 C42 -0.7(11) . . . . ? C38 N10 C42 C41 -0.4(10) . . . . ? C40 C41 C42 N10 0.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.883 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.095 # Attachment 'web_deposit_cif_file_2_ShaojinGu_1283865305.cif' data_090425a _database_code_depnum_ccdc_archive 'CCDC 792160' #TrackingRef 'web_deposit_cif_file_2_ShaojinGu_1283865305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H15 Cl F6 N5 P Pt' _chemical_formula_weight 712.89 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' F F 0.0171 0.0103 '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 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 14.2205(15) _cell_length_b 10.3577(10) _cell_length_c 15.2229(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.3910(10) _cell_angle_gamma 90.00 _cell_volume 2198.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 6.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5025 _exptl_absorpt_correction_T_max 0.6532 _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 11070 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3864 _reflns_number_gt 2613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0556P)^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 3864 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.39950(3) 0.58719(4) 0.06187(3) 0.04887(19) Uani 1 1 d . . . P1 P 0.1689(3) 0.4042(4) 0.2124(3) 0.0758(10) Uani 1 1 d . . . Cl1 Cl 0.4274(3) 0.8025(3) 0.0800(2) 0.0704(9) Uani 1 1 d . . . F1 F 0.2475(8) 0.3133(11) 0.1982(8) 0.150(4) Uani 1 1 d . . . F2 F 0.0841(8) 0.4973(11) 0.2234(8) 0.143(4) Uani 1 1 d . . . F3 F 0.2124(11) 0.4362(13) 0.3094(8) 0.183(6) Uani 1 1 d . . . F4 F 0.2198(7) 0.5176(10) 0.1766(7) 0.122(3) Uani 1 1 d . . . F5 F 0.1183(9) 0.3787(12) 0.1157(8) 0.158(4) Uani 1 1 d . . . F6 F 0.1141(10) 0.2941(11) 0.2454(9) 0.175(5) Uani 1 1 d . . . N1 N 0.2429(7) 0.4521(10) -0.0388(7) 0.059(3) Uani 1 1 d . . . N2 N 0.2018(8) 0.6507(10) -0.0626(7) 0.063(3) Uani 1 1 d . . . N3 N 0.3813(7) 0.4042(9) 0.0507(6) 0.055(3) Uani 1 1 d . . . N4 N 0.5288(7) 0.5233(10) 0.1433(7) 0.055(3) Uani 1 1 d . . . N5 N 0.1542(7) 0.9718(11) 0.0159(7) 0.068(3) Uani 1 1 d . . . C1 C 0.2737(8) 0.5769(12) -0.0181(8) 0.055(3) Uani 1 1 d . . . C2 C 0.1293(10) 0.5725(15) -0.1069(9) 0.071(4) Uani 1 1 d . . . H2 H 0.0719 0.6009 -0.1420 0.085 Uiso 1 1 calc R . . C3 C 0.1546(10) 0.4506(14) -0.0913(9) 0.070(4) Uani 1 1 d . . . H3 H 0.1187 0.3780 -0.1124 0.083 Uiso 1 1 calc R . . C4 C 0.3034(9) 0.3534(13) -0.0004(9) 0.060(3) Uani 1 1 d . . . C5 C 0.2915(9) 0.2213(12) -0.0073(9) 0.064(3) Uani 1 1 d . . . H5 H 0.2369 0.1850 -0.0424 0.077 Uiso 1 1 calc R . . C6 C 0.3649(10) 0.1442(14) 0.0407(9) 0.067(4) Uani 1 1 d . . . H6 H 0.3590 0.0549 0.0361 0.080 Uiso 1 1 calc R . . C7 C 0.4440(10) 0.1943(12) 0.0934(9) 0.055(3) Uani 1 1 d . . . C8 C 0.4491(9) 0.3273(12) 0.0948(8) 0.056(3) Uani 1 1 d . . . C9 C 0.5308(9) 0.3951(13) 0.1468(8) 0.058(3) Uani 1 1 d . . . C10 C 0.6063(9) 0.3239(13) 0.1963(9) 0.059(3) Uani 1 1 d . . . C11 C 0.6841(9) 0.3961(13) 0.2429(8) 0.064(3) Uani 1 1 d . . . H11 H 0.7380 0.3544 0.2751 0.077 Uiso 1 1 calc R . . C12 C 0.6801(10) 0.5228(16) 0.2408(9) 0.073(4) Uani 1 1 d . . . H12 H 0.7304 0.5699 0.2742 0.088 Uiso 1 1 calc R . . C13 C 0.6024(9) 0.5887(13) 0.1896(8) 0.059(3) Uani 1 1 d . . . H13 H 0.6022 0.6785 0.1880 0.071 Uiso 1 1 calc R . . C14 C 0.5250(10) 0.1235(13) 0.1429(9) 0.065(4) Uani 1 1 d . . . H14 H 0.5253 0.0338 0.1418 0.078 Uiso 1 1 calc R . . C15 C 0.6017(10) 0.1900(14) 0.1919(9) 0.067(4) Uani 1 1 d . . . H15 H 0.6531 0.1428 0.2235 0.080 Uiso 1 1 calc R . . C16 C 0.1986(9) 0.7909(12) -0.0597(9) 0.066(3) Uani 1 1 d . . . H16A H 0.1660 0.8223 -0.1178 0.079 Uiso 1 1 calc R . . H16B H 0.2637 0.8236 -0.0492 0.079 Uiso 1 1 calc R . . C17 C 0.1492(8) 0.8447(13) 0.0105(8) 0.058(3) Uani 1 1 d . . . C18 C 0.1058(9) 0.7703(14) 0.0659(8) 0.069(4) Uani 1 1 d . . . H18 H 0.1076 0.6807 0.0627 0.083 Uiso 1 1 calc R . . C19 C 0.0593(9) 0.8305(15) 0.1264(9) 0.072(4) Uani 1 1 d . . . H19 H 0.0266 0.7825 0.1624 0.086 Uiso 1 1 calc R . . C20 C 0.0626(9) 0.9608(15) 0.1320(9) 0.072(4) Uani 1 1 d . . . H20 H 0.0322 1.0047 0.1718 0.087 Uiso 1 1 calc R . . C21 C 0.1118(10) 1.0259(15) 0.0775(10) 0.078(4) Uani 1 1 d . . . H21 H 0.1161 1.1152 0.0838 0.093 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 0.0468(3) 0.0495(3) 0.0512(3) -0.0017(3) 0.0120(2) -0.0025(2) P1 0.077(3) 0.080(3) 0.075(3) -0.006(2) 0.026(2) -0.004(2) Cl1 0.084(2) 0.0515(17) 0.077(2) -0.0008(16) 0.0192(19) -0.0047(16) F1 0.136(10) 0.146(10) 0.175(11) 0.016(8) 0.052(9) 0.050(7) F2 0.123(9) 0.147(10) 0.170(11) 0.002(8) 0.055(8) 0.022(7) F3 0.215(15) 0.219(14) 0.095(8) -0.001(9) -0.017(9) -0.006(11) F4 0.109(8) 0.127(8) 0.131(8) 0.017(7) 0.030(6) -0.022(6) F5 0.152(11) 0.187(12) 0.120(9) -0.026(8) -0.010(8) -0.026(9) F6 0.226(14) 0.122(9) 0.208(13) 0.007(9) 0.117(11) -0.051(9) N1 0.052(6) 0.068(7) 0.056(7) -0.004(5) 0.010(5) -0.006(5) N2 0.056(7) 0.071(7) 0.061(7) -0.004(6) 0.011(6) 0.005(6) N3 0.053(6) 0.054(6) 0.058(6) -0.001(5) 0.013(5) 0.006(5) N4 0.054(7) 0.060(7) 0.055(6) 0.003(5) 0.019(5) -0.003(5) N5 0.060(7) 0.072(8) 0.069(8) -0.001(6) 0.006(6) 0.007(6) C1 0.050(7) 0.065(8) 0.053(7) -0.004(7) 0.012(6) 0.000(6) C2 0.056(8) 0.084(10) 0.069(9) -0.007(8) 0.006(7) -0.002(8) C3 0.059(9) 0.077(10) 0.069(9) -0.010(8) 0.004(7) -0.006(7) C4 0.055(8) 0.067(8) 0.061(8) -0.006(7) 0.019(7) 0.001(7) C5 0.062(8) 0.063(9) 0.068(9) -0.010(7) 0.014(7) -0.009(7) C6 0.075(9) 0.058(8) 0.069(9) -0.002(7) 0.020(8) 0.004(8) C7 0.060(8) 0.056(8) 0.055(8) 0.004(6) 0.023(7) 0.005(6) C8 0.059(8) 0.065(9) 0.052(8) 0.005(7) 0.028(7) 0.009(7) C9 0.058(8) 0.069(10) 0.054(8) 0.003(7) 0.023(7) 0.000(7) C10 0.058(8) 0.069(9) 0.054(8) 0.006(7) 0.019(7) 0.005(7) C11 0.057(8) 0.077(10) 0.057(8) 0.007(7) 0.009(7) 0.003(7) C12 0.062(9) 0.089(11) 0.064(9) -0.001(8) 0.004(7) -0.001(8) C13 0.056(8) 0.075(9) 0.046(7) -0.005(7) 0.008(6) -0.004(7) C14 0.073(10) 0.066(9) 0.060(8) 0.002(7) 0.021(8) 0.008(7) C15 0.067(9) 0.075(9) 0.061(9) 0.009(7) 0.018(7) 0.011(7) C16 0.057(8) 0.074(9) 0.066(9) 0.004(7) 0.009(7) 0.001(7) C17 0.043(7) 0.070(9) 0.062(9) 0.000(7) 0.012(6) -0.001(6) C18 0.063(8) 0.076(9) 0.069(9) 0.002(8) 0.013(7) 0.002(7) C19 0.055(8) 0.089(11) 0.073(10) 0.009(8) 0.018(7) -0.009(7) C20 0.049(8) 0.101(12) 0.064(9) -0.006(8) 0.005(7) 0.008(7) C21 0.065(9) 0.084(10) 0.079(11) 0.000(9) 0.002(8) 0.001(8) _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 N3 1.916(10) . ? Pt1 C1 1.959(12) . ? Pt1 N4 2.111(10) . ? Pt1 Cl1 2.272(3) . ? P1 F1 1.510(10) . ? P1 F3 1.519(12) . ? P1 F6 1.521(10) . ? P1 F5 1.529(12) . ? P1 F4 1.534(10) . ? P1 F2 1.579(11) . ? N1 C3 1.348(16) . ? N1 C1 1.381(14) . ? N1 C4 1.389(16) . ? N2 C1 1.347(15) . ? N2 C2 1.378(16) . ? N2 C16 1.453(15) . ? N3 C8 1.327(15) . ? N3 C4 1.330(15) . ? N4 C13 1.326(15) . ? N4 C9 1.329(15) . ? N5 C17 1.320(15) . ? N5 C21 1.335(16) . ? C2 C3 1.322(17) . ? C4 C5 1.380(17) . ? C5 C6 1.401(18) . ? C6 C7 1.349(19) . ? C7 C8 1.379(16) . ? C7 C14 1.445(18) . ? C8 C9 1.451(18) . ? C9 C10 1.394(17) . ? C10 C15 1.389(17) . ? C10 C11 1.406(17) . ? C11 C12 1.314(17) . ? C12 C13 1.399(18) . ? C14 C15 1.378(19) . ? C16 C17 1.497(16) . ? C17 C18 1.375(16) . ? C18 C19 1.384(16) . ? C19 C20 1.352(19) . ? C20 C21 1.364(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pt1 C1 78.5(5) . . ? N3 Pt1 N4 80.1(4) . . ? C1 Pt1 N4 158.6(5) . . ? N3 Pt1 Cl1 177.3(3) . . ? C1 Pt1 Cl1 104.2(4) . . ? N4 Pt1 Cl1 97.2(3) . . ? F1 P1 F3 96.0(8) . . ? F1 P1 F6 91.2(7) . . ? F3 P1 F6 88.8(8) . . ? F1 P1 F5 88.6(7) . . ? F3 P1 F5 175.4(8) . . ? F6 P1 F5 90.7(8) . . ? F1 P1 F4 90.7(6) . . ? F3 P1 F4 92.8(7) . . ? F6 P1 F4 177.3(8) . . ? F5 P1 F4 87.5(7) . . ? F1 P1 F2 177.5(8) . . ? F3 P1 F2 86.4(8) . . ? F6 P1 F2 88.3(7) . . ? F5 P1 F2 89.0(7) . . ? F4 P1 F2 89.7(6) . . ? C3 N1 C1 111.2(11) . . ? C3 N1 C4 132.0(12) . . ? C1 N1 C4 116.8(11) . . ? C1 N2 C2 109.4(11) . . ? C1 N2 C16 125.2(11) . . ? C2 N2 C16 125.3(12) . . ? C8 N3 C4 119.8(12) . . ? C8 N3 Pt1 118.5(9) . . ? C4 N3 Pt1 121.7(9) . . ? C13 N4 C9 118.7(12) . . ? C13 N4 Pt1 131.0(9) . . ? C9 N4 Pt1 110.3(9) . . ? C17 N5 C21 115.9(12) . . ? N2 C1 N1 104.0(11) . . ? N2 C1 Pt1 142.3(10) . . ? N1 C1 Pt1 113.7(9) . . ? C3 C2 N2 108.8(13) . . ? C2 C3 N1 106.5(13) . . ? N3 C4 C5 120.8(13) . . ? N3 C4 N1 109.4(11) . . ? C5 C4 N1 129.8(13) . . ? C4 C5 C6 117.2(13) . . ? C7 C6 C5 122.6(13) . . ? C6 C7 C8 115.4(13) . . ? C6 C7 C14 126.9(13) . . ? C8 C7 C14 117.6(13) . . ? N3 C8 C7 124.1(13) . . ? N3 C8 C9 114.1(11) . . ? C7 C8 C9 121.8(13) . . ? N4 C9 C10 124.0(13) . . ? N4 C9 C8 117.0(12) . . ? C10 C9 C8 119.1(12) . . ? C15 C10 C9 118.6(14) . . ? C15 C10 C11 125.4(14) . . ? C9 C10 C11 115.9(13) . . ? C12 C11 C10 119.5(13) . . ? C11 C12 C13 121.8(14) . . ? N4 C13 C12 120.0(13) . . ? C15 C14 C7 119.6(13) . . ? C14 C15 C10 123.3(14) . . ? N2 C16 C17 114.6(11) . . ? N5 C17 C18 123.1(12) . . ? N5 C17 C16 112.9(11) . . ? C18 C17 C16 124.0(12) . . ? C17 C18 C19 119.1(13) . . ? C20 C19 C18 118.5(13) . . ? C19 C20 C21 118.1(14) . . ? N5 C21 C20 125.2(14) . . ? 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 N3 C8 -179.5(9) . . . . ? N4 Pt1 N3 C8 0.9(8) . . . . ? Cl1 Pt1 N3 C8 -6(6) . . . . ? C1 Pt1 N3 C4 1.2(9) . . . . ? N4 Pt1 N3 C4 -178.5(9) . . . . ? Cl1 Pt1 N3 C4 175(5) . . . . ? N3 Pt1 N4 C13 -179.9(10) . . . . ? C1 Pt1 N4 C13 179.1(11) . . . . ? Cl1 Pt1 N4 C13 -0.3(10) . . . . ? N3 Pt1 N4 C9 -1.3(7) . . . . ? C1 Pt1 N4 C9 -2.3(15) . . . . ? Cl1 Pt1 N4 C9 178.4(7) . . . . ? C2 N2 C1 N1 1.3(13) . . . . ? C16 N2 C1 N1 177.7(10) . . . . ? C2 N2 C1 Pt1 -178.2(11) . . . . ? C16 N2 C1 Pt1 -2(2) . . . . ? C3 N1 C1 N2 -1.9(13) . . . . ? C4 N1 C1 N2 -179.1(9) . . . . ? C3 N1 C1 Pt1 177.8(8) . . . . ? C4 N1 C1 Pt1 0.6(13) . . . . ? N3 Pt1 C1 N2 178.7(15) . . . . ? N4 Pt1 C1 N2 179.6(10) . . . . ? Cl1 Pt1 C1 N2 -1.0(15) . . . . ? N3 Pt1 C1 N1 -0.9(8) . . . . ? N4 Pt1 C1 N1 0.1(17) . . . . ? Cl1 Pt1 C1 N1 179.5(7) . . . . ? C1 N2 C2 C3 -0.3(15) . . . . ? C16 N2 C2 C3 -176.7(12) . . . . ? N2 C2 C3 N1 -0.9(15) . . . . ? C1 N1 C3 C2 1.8(15) . . . . ? C4 N1 C3 C2 178.4(12) . . . . ? C8 N3 C4 C5 0.8(17) . . . . ? Pt1 N3 C4 C5 -179.8(9) . . . . ? C8 N3 C4 N1 179.5(9) . . . . ? Pt1 N3 C4 N1 -1.1(13) . . . . ? C3 N1 C4 N3 -176.2(12) . . . . ? C1 N1 C4 N3 0.3(14) . . . . ? C3 N1 C4 C5 2(2) . . . . ? C1 N1 C4 C5 178.8(12) . . . . ? N3 C4 C5 C6 -0.7(18) . . . . ? N1 C4 C5 C6 -179.0(11) . . . . ? C4 C5 C6 C7 1.3(19) . . . . ? C5 C6 C7 C8 -1.9(19) . . . . ? C5 C6 C7 C14 -177.7(11) . . . . ? C4 N3 C8 C7 -1.6(18) . . . . ? Pt1 N3 C8 C7 179.0(9) . . . . ? C4 N3 C8 C9 179.1(10) . . . . ? Pt1 N3 C8 C9 -0.3(13) . . . . ? C6 C7 C8 N3 2.1(19) . . . . ? C14 C7 C8 N3 178.3(10) . . . . ? C6 C7 C8 C9 -178.6(10) . . . . ? C14 C7 C8 C9 -2.4(18) . . . . ? C13 N4 C9 C10 -0.3(17) . . . . ? Pt1 N4 C9 C10 -179.1(9) . . . . ? C13 N4 C9 C8 -179.7(10) . . . . ? Pt1 N4 C9 C8 1.5(12) . . . . ? N3 C8 C9 N4 -0.9(15) . . . . ? C7 C8 C9 N4 179.8(11) . . . . ? N3 C8 C9 C10 179.7(10) . . . . ? C7 C8 C9 C10 0.3(17) . . . . ? N4 C9 C10 C15 -177.5(11) . . . . ? C8 C9 C10 C15 1.9(18) . . . . ? N4 C9 C10 C11 -1.1(18) . . . . ? C8 C9 C10 C11 178.3(10) . . . . ? C15 C10 C11 C12 178.9(13) . . . . ? C9 C10 C11 C12 2.8(18) . . . . ? C10 C11 C12 C13 -3(2) . . . . ? C9 N4 C13 C12 0.0(17) . . . . ? Pt1 N4 C13 C12 178.6(8) . . . . ? C11 C12 C13 N4 1.8(19) . . . . ? C6 C7 C14 C15 178.1(13) . . . . ? C8 C7 C14 C15 2.4(18) . . . . ? C7 C14 C15 C10 0(2) . . . . ? C9 C10 C15 C14 -2(2) . . . . ? C11 C10 C15 C14 -177.9(11) . . . . ? C1 N2 C16 C17 -92.2(14) . . . . ? C2 N2 C16 C17 83.6(15) . . . . ? C21 N5 C17 C18 -1.7(19) . . . . ? C21 N5 C17 C16 -179.8(11) . . . . ? N2 C16 C17 N5 175.1(11) . . . . ? N2 C16 C17 C18 -3.0(18) . . . . ? N5 C17 C18 C19 4(2) . . . . ? C16 C17 C18 C19 -177.7(12) . . . . ? C17 C18 C19 C20 -3(2) . . . . ? C18 C19 C20 C21 0(2) . . . . ? C17 N5 C21 C20 -2(2) . . . . ? C19 C20 C21 N5 3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.797 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.170 # Attachment 'web_deposit_cif_file_3_ShaojinGu_1283865305.cif' data_080712d _database_code_depnum_ccdc_archive 'CCDC 792161' #TrackingRef 'web_deposit_cif_file_3_ShaojinGu_1283865305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Ag F18 N10 P3 Pd' _chemical_formula_weight 1323.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' Ag Ag -0.8971 1.1015 '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 20.7545(19) _cell_length_b 8.1456(14) _cell_length_c 28.866(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.547(2) _cell_angle_gamma 90.00 _cell_volume 4864.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6493 _exptl_absorpt_correction_T_max 0.7566 _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 23846 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8573 _reflns_number_gt 5272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0161P)^2^+47.7995P] 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 8573 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Pd1 Pd 0.25020(4) 0.73168(10) 0.23986(3) 0.0420(2) Uani 1 1 d . . . Ag1 Ag 0.22925(5) 0.77552(15) 0.04200(3) 0.0768(4) Uani 1 1 d . . . F1 F 0.0039(4) 0.8462(11) 0.3479(3) 0.093(3) Uani 1 1 d . . . F2 F 0.1188(4) 0.9330(13) 0.2873(3) 0.112(3) Uani 1 1 d . . . F3 F 0.0933(4) 0.7187(11) 0.3276(4) 0.123(3) Uani 1 1 d . . . F4 F 0.1024(4) 0.9603(12) 0.3623(3) 0.101(3) Uani 1 1 d . . . F5 F 0.0299(4) 1.0652(10) 0.3102(3) 0.113(3) Uani 1 1 d . . . F6 F 0.0205(4) 0.8217(13) 0.2744(3) 0.115(3) Uani 1 1 d . . . F7 F 0.1740(5) 0.2051(18) 0.5205(3) 0.166(5) Uani 1 1 d . . . F8 F 0.2925(5) 0.2552(13) 0.4618(3) 0.124(3) Uani 1 1 d . . . F9 F 0.2563(8) 0.0652(17) 0.5048(7) 0.253(9) Uani 1 1 d . . . F10 F 0.2720(7) 0.313(2) 0.5314(4) 0.220(8) Uani 1 1 d . . . F11 F 0.2086(7) 0.4041(15) 0.4764(6) 0.193(6) Uani 1 1 d . . . F12 F 0.1925(6) 0.1702(16) 0.4483(3) 0.159(5) Uani 1 1 d . . . F13 F 0.4156(4) 1.0713(10) 0.8539(3) 0.094(3) Uani 1 1 d . . . F14 F 0.4920(5) 0.8565(13) 0.7870(4) 0.149(5) Uani 1 1 d . . . F15 F 0.4120(5) 0.8167(12) 0.8320(4) 0.147(4) Uani 1 1 d . . . F16 F 0.5030(5) 0.9254(17) 0.8613(4) 0.166(5) Uani 1 1 d . . . F17 F 0.4948(5) 1.1167(12) 0.8101(4) 0.141(4) Uani 1 1 d . . . F18 F 0.4023(6) 1.005(2) 0.7811(3) 0.178(6) Uani 1 1 d . . . N1 N 0.2383(4) 0.5502(11) 0.1472(3) 0.040(2) Uani 1 1 d . . . N2 N 0.1578(4) 0.5263(11) 0.1879(3) 0.048(2) Uani 1 1 d . . . N3 N 0.3088(4) 0.6407(11) 0.0943(3) 0.050(2) Uani 1 1 d . . . N4 N 0.3271(6) 0.7846(14) 0.0127(4) 0.085(4) Uani 1 1 d . . . N5 N 0.2164(4) 0.5527(11) 0.2829(3) 0.045(2) Uani 1 1 d . . . N6 N 0.2484(5) 0.9595(11) 0.1577(3) 0.054(2) Uani 1 1 d . . . N7 N 0.3356(4) 0.9662(11) 0.2015(3) 0.054(2) Uani 1 1 d . . . N8 N 0.1637(5) 0.8901(11) 0.1020(3) 0.054(2) Uani 1 1 d . . . N9 N 0.1241(5) 0.7600(14) 0.0174(3) 0.069(3) Uani 1 1 d . . . N10 N 0.2910(4) 0.8821(11) 0.2922(3) 0.043(2) Uani 1 1 d . . . P1 P 0.06169(15) 0.8902(4) 0.31825(11) 0.0570(8) Uani 1 1 d . . . P2 P 0.2342(2) 0.2312(5) 0.49151(12) 0.0858(12) Uani 1 1 d . . . P3 P 0.45405(19) 0.9657(5) 0.81998(14) 0.0757(11) Uani 1 1 d . . . C1 C 0.2157(5) 0.5923(12) 0.1878(3) 0.039(2) Uani 1 1 d . . . C2 C 0.1417(6) 0.4434(16) 0.1465(4) 0.064(3) Uani 1 1 d . . . H2 H 0.1037 0.3867 0.1379 0.077 Uiso 1 1 calc R . . C3 C 0.1933(6) 0.4636(15) 0.1219(4) 0.061(3) Uani 1 1 d . . . H3 H 0.1972 0.4239 0.0920 0.073 Uiso 1 1 calc R . . C4 C 0.3039(5) 0.5781(14) 0.1361(4) 0.049(3) Uani 1 1 d . . . C5 C 0.3553(7) 0.5259(16) 0.1674(4) 0.068(4) Uani 1 1 d . . . H5 H 0.3488 0.4889 0.1972 0.081 Uiso 1 1 calc R . . C6 C 0.4150(7) 0.5330(19) 0.1514(5) 0.083(4) Uani 1 1 d . . . H6 H 0.4504 0.4965 0.1704 0.100 Uiso 1 1 calc R . . C7 C 0.4247(6) 0.5929(19) 0.1076(4) 0.074(4) Uani 1 1 d . . . C8 C 0.3705(6) 0.6503(16) 0.0805(4) 0.063(3) Uani 1 1 d . . . C9 C 0.3777(8) 0.7267(18) 0.0361(4) 0.078(4) Uani 1 1 d . . . C10 C 0.4418(8) 0.732(2) 0.0212(6) 0.094(5) Uani 1 1 d . . . C11 C 0.4464(11) 0.795(3) -0.0241(7) 0.128(7) Uani 1 1 d . . . H11 H 0.4858 0.7914 -0.0375 0.153 Uiso 1 1 calc R . . C12 C 0.3957(12) 0.857(3) -0.0472(7) 0.149(10) Uani 1 1 d . . . H12 H 0.4000 0.9079 -0.0757 0.178 Uiso 1 1 calc R . . C13 C 0.3348(9) 0.8483(19) -0.0297(5) 0.100(5) Uani 1 1 d . . . H13 H 0.2989 0.8872 -0.0477 0.120 Uiso 1 1 calc R . . C14 C 0.4856(7) 0.603(3) 0.0901(6) 0.122(7) Uani 1 1 d . . . H14 H 0.5219 0.5690 0.1086 0.147 Uiso 1 1 calc R . . C15 C 0.4930(9) 0.660(3) 0.0476(6) 0.113(7) Uani 1 1 d . . . H15 H 0.5331 0.6525 0.0355 0.136 Uiso 1 1 calc R . . C16 C 0.1189(5) 0.5371(15) 0.2288(3) 0.050(3) Uani 1 1 d . . . H16A H 0.0807 0.4688 0.2237 0.061 Uiso 1 1 calc R . . H16B H 0.1050 0.6496 0.2328 0.061 Uiso 1 1 calc R . . C17 C 0.1589(5) 0.4807(14) 0.2721(4) 0.049(3) Uani 1 1 d . . . C18 C 0.1344(6) 0.3606(15) 0.2998(4) 0.060(3) Uani 1 1 d . . . H18 H 0.0949 0.3105 0.2914 0.072 Uiso 1 1 calc R . . C19 C 0.1698(8) 0.3184(17) 0.3394(5) 0.082(4) Uani 1 1 d . . . H19 H 0.1543 0.2388 0.3587 0.098 Uiso 1 1 calc R . . C20 C 0.2288(6) 0.3922(15) 0.3514(4) 0.062(3) Uani 1 1 d . . . H20 H 0.2528 0.3649 0.3789 0.075 Uiso 1 1 calc R . . C21 C 0.2508(5) 0.5053(13) 0.3220(4) 0.049(3) Uani 1 1 d . . . H21 H 0.2913 0.5519 0.3292 0.059 Uiso 1 1 calc R . . C22 C 0.2767(5) 0.8970(13) 0.1966(3) 0.043(3) Uani 1 1 d . . . C23 C 0.3439(6) 1.0694(16) 0.1637(4) 0.065(4) Uani 1 1 d . . . H23 H 0.3806 1.1306 0.1588 0.077 Uiso 1 1 calc R . . C24 C 0.2901(6) 1.0638(15) 0.1362(4) 0.065(4) Uani 1 1 d . . . H24 H 0.2817 1.1186 0.1081 0.078 Uiso 1 1 calc R . . C25 C 0.1798(6) 0.9457(14) 0.1444(4) 0.050(3) Uani 1 1 d . . . C26 C 0.1373(6) 0.9900(15) 0.1762(4) 0.056(3) Uani 1 1 d . . . H26 H 0.1525 1.0271 0.2055 0.068 Uiso 1 1 calc R . . C27 C 0.0743(6) 0.9794(16) 0.1646(4) 0.068(4) Uani 1 1 d . . . H27 H 0.0449 1.0096 0.1858 0.082 Uiso 1 1 calc R . . C28 C 0.0519(6) 0.9220(15) 0.1200(4) 0.056(3) Uani 1 1 d . . . C29 C 0.0988(6) 0.8784(14) 0.0898(4) 0.054(3) Uani 1 1 d . . . C30 C 0.0789(7) 0.8074(15) 0.0450(4) 0.065(3) Uani 1 1 d . . . C31 C 0.0121(7) 0.7942(19) 0.0322(5) 0.077(4) Uani 1 1 d . . . C32 C -0.0061(8) 0.730(2) -0.0112(5) 0.103(5) Uani 1 1 d . . . H32 H -0.0496 0.7254 -0.0216 0.124 Uiso 1 1 calc R . . C33 C 0.0396(9) 0.674(2) -0.0394(5) 0.109(6) Uani 1 1 d . . . H33 H 0.0276 0.6254 -0.0680 0.131 Uiso 1 1 calc R . . C34 C 0.1028(9) 0.6916(19) -0.0239(5) 0.089(5) Uani 1 1 d . . . H34 H 0.1338 0.6541 -0.0430 0.107 Uiso 1 1 calc R . . C35 C -0.0151(7) 0.9099(19) 0.1040(5) 0.081(4) Uani 1 1 d . . . H35 H -0.0464 0.9429 0.1234 0.097 Uiso 1 1 calc R . . C36 C -0.0330(7) 0.8525(19) 0.0621(5) 0.087(4) Uani 1 1 d . . . H36 H -0.0767 0.8507 0.0522 0.104 Uiso 1 1 calc R . . C37 C 0.3789(5) 0.9390(16) 0.2427(4) 0.056(3) Uani 1 1 d . . . H37A H 0.4151 1.0139 0.2424 0.067 Uiso 1 1 calc R . . H37B H 0.3957 0.8279 0.2420 0.067 Uiso 1 1 calc R . . C38 C 0.3460(5) 0.9635(14) 0.2873(4) 0.053(3) Uani 1 1 d . . . C39 C 0.3732(5) 1.0666(15) 0.3206(4) 0.060(3) Uani 1 1 d . . . H39 H 0.4101 1.1265 0.3155 0.071 Uiso 1 1 calc R . . C40 C 0.3447(6) 1.0802(17) 0.3624(5) 0.073(4) Uani 1 1 d . . . H40 H 0.3632 1.1460 0.3862 0.088 Uiso 1 1 calc R . . C41 C 0.2892(6) 0.9958(16) 0.3680(4) 0.066(3) Uani 1 1 d . . . H41 H 0.2691 1.0030 0.3955 0.079 Uiso 1 1 calc R . . C42 C 0.2634(6) 0.8990(13) 0.3317(4) 0.051(3) Uani 1 1 d . . . H42 H 0.2250 0.8435 0.3352 0.061 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 Pd1 0.0432(5) 0.0481(5) 0.0352(4) 0.0028(4) 0.0064(3) -0.0053(4) Ag1 0.0843(8) 0.0905(8) 0.0583(6) 0.0112(6) 0.0230(5) 0.0227(6) F1 0.072(5) 0.125(7) 0.086(5) -0.005(5) 0.032(4) -0.012(5) F2 0.064(5) 0.202(10) 0.072(5) 0.017(6) 0.021(4) -0.013(6) F3 0.108(7) 0.089(7) 0.172(9) 0.018(6) 0.010(6) 0.025(6) F4 0.077(6) 0.148(8) 0.077(5) -0.022(5) 0.001(4) -0.022(5) F5 0.101(7) 0.075(6) 0.162(9) 0.012(6) -0.007(6) 0.003(5) F6 0.090(6) 0.171(9) 0.081(6) -0.040(6) -0.002(5) -0.007(6) F7 0.140(9) 0.272(15) 0.090(7) 0.056(8) 0.034(6) -0.014(10) F8 0.137(8) 0.139(8) 0.103(6) -0.009(6) 0.049(6) 0.005(7) F9 0.227(16) 0.142(11) 0.40(2) 0.170(15) 0.086(16) 0.058(11) F10 0.202(13) 0.36(2) 0.095(7) -0.117(11) 0.014(8) -0.095(14) F11 0.198(14) 0.112(10) 0.277(17) 0.016(10) 0.070(13) 0.013(9) F12 0.185(11) 0.211(13) 0.080(6) -0.034(7) 0.004(7) -0.021(10) F13 0.108(6) 0.091(6) 0.089(6) -0.005(5) 0.043(5) 0.008(5) F14 0.125(8) 0.140(9) 0.195(11) -0.082(8) 0.099(8) -0.036(7) F15 0.126(8) 0.111(8) 0.216(12) -0.052(8) 0.086(8) -0.061(7) F16 0.098(8) 0.198(13) 0.197(12) 0.001(10) -0.017(8) 0.025(8) F17 0.162(10) 0.110(8) 0.167(9) -0.031(7) 0.111(8) -0.046(7) F18 0.144(10) 0.326(18) 0.062(6) -0.009(8) -0.003(6) 0.039(11) N1 0.039(5) 0.057(6) 0.024(4) -0.002(4) 0.003(4) -0.005(4) N2 0.043(6) 0.071(6) 0.028(5) -0.004(4) 0.002(4) -0.004(5) N3 0.055(6) 0.053(6) 0.045(5) -0.003(4) 0.016(5) 0.004(5) N4 0.109(10) 0.074(8) 0.079(8) 0.014(7) 0.055(8) 0.015(8) N5 0.041(5) 0.054(6) 0.040(5) 0.000(4) 0.007(4) -0.001(4) N6 0.061(7) 0.056(6) 0.046(6) 0.014(5) 0.004(5) 0.000(5) N7 0.052(6) 0.061(6) 0.052(6) 0.007(5) 0.018(5) 0.001(5) N8 0.062(7) 0.061(6) 0.039(5) 0.006(4) 0.012(5) 0.008(5) N9 0.077(7) 0.082(8) 0.046(5) 0.002(6) 0.001(5) 0.013(6) N10 0.033(5) 0.056(6) 0.041(5) -0.013(4) 0.002(4) -0.003(4) P1 0.0415(18) 0.076(2) 0.0537(19) -0.0005(16) 0.0058(15) 0.0018(16) P2 0.129(4) 0.083(3) 0.0475(18) -0.001(2) 0.020(2) -0.015(3) P3 0.058(2) 0.086(3) 0.087(3) -0.021(2) 0.029(2) -0.013(2) C1 0.047(7) 0.042(6) 0.029(5) -0.001(4) 0.003(5) 0.000(5) C2 0.051(8) 0.087(10) 0.053(7) -0.011(7) 0.000(6) -0.022(7) C3 0.065(8) 0.079(9) 0.038(6) -0.015(6) -0.004(6) 0.000(7) C4 0.048(7) 0.056(7) 0.042(6) -0.008(5) 0.006(6) 0.007(6) C5 0.074(10) 0.081(9) 0.050(7) -0.002(7) 0.011(7) -0.001(8) C6 0.052(9) 0.116(13) 0.080(10) -0.017(9) -0.008(8) -0.010(8) C7 0.050(8) 0.118(12) 0.054(8) -0.018(8) 0.010(7) -0.010(8) C8 0.070(9) 0.071(9) 0.052(7) -0.008(6) 0.025(7) -0.003(7) C9 0.112(13) 0.067(9) 0.058(8) -0.001(7) 0.024(8) -0.028(9) C10 0.090(11) 0.113(13) 0.087(11) 0.009(10) 0.051(10) -0.012(11) C11 0.15(2) 0.127(18) 0.113(16) -0.002(13) 0.080(15) 0.004(15) C12 0.20(2) 0.146(19) 0.116(16) 0.067(14) 0.115(18) 0.032(18) C13 0.127(14) 0.100(12) 0.078(10) 0.028(9) 0.039(10) 0.035(11) C14 0.059(10) 0.22(2) 0.088(12) -0.048(14) 0.015(9) -0.004(12) C15 0.082(12) 0.18(2) 0.086(12) -0.014(12) 0.045(10) -0.029(13) C16 0.032(6) 0.074(8) 0.046(6) -0.005(6) 0.003(5) -0.011(6) C17 0.035(6) 0.057(7) 0.055(7) -0.003(6) 0.014(5) 0.001(6) C18 0.062(8) 0.063(8) 0.058(8) 0.009(6) 0.017(7) -0.009(7) C19 0.109(12) 0.076(10) 0.064(9) 0.023(7) 0.033(9) -0.003(9) C20 0.066(9) 0.069(8) 0.051(7) 0.022(6) 0.006(6) -0.001(7) C21 0.044(7) 0.058(7) 0.047(7) 0.005(5) 0.015(6) -0.006(6) C22 0.045(7) 0.049(6) 0.038(6) -0.001(5) 0.016(5) -0.003(5) C23 0.054(8) 0.080(9) 0.061(8) 0.034(7) 0.012(7) -0.004(7) C24 0.071(9) 0.074(9) 0.053(7) 0.033(7) 0.013(7) -0.001(7) C25 0.051(7) 0.057(7) 0.042(6) 0.015(5) 0.011(6) 0.002(6) C26 0.043(7) 0.077(9) 0.049(7) -0.010(6) 0.003(6) 0.009(6) C27 0.070(9) 0.089(10) 0.047(7) 0.010(7) 0.016(7) 0.020(8) C28 0.054(8) 0.076(8) 0.040(6) 0.007(6) 0.014(6) 0.018(6) C29 0.058(8) 0.065(8) 0.041(6) 0.016(6) 0.008(6) 0.011(6) C30 0.086(10) 0.070(9) 0.040(6) 0.011(6) 0.012(7) 0.000(7) C31 0.067(9) 0.098(11) 0.064(8) 0.011(8) -0.002(7) -0.009(8) C32 0.088(11) 0.139(15) 0.081(11) -0.033(11) -0.009(9) -0.017(11) C33 0.114(15) 0.157(18) 0.053(9) -0.012(10) -0.012(10) -0.003(13) C34 0.114(13) 0.097(12) 0.058(9) -0.002(8) 0.022(9) 0.007(10) C35 0.066(10) 0.114(12) 0.065(9) 0.001(8) 0.018(8) -0.002(9) C36 0.059(9) 0.115(13) 0.088(11) -0.005(9) 0.012(8) -0.002(9) C37 0.042(7) 0.078(9) 0.048(7) 0.000(6) 0.004(6) -0.003(6) C38 0.045(7) 0.045(7) 0.069(8) 0.006(6) 0.005(6) -0.003(6) C39 0.037(7) 0.060(8) 0.081(9) 0.000(7) -0.002(6) 0.001(6) C40 0.057(9) 0.088(10) 0.072(9) -0.037(8) -0.009(7) 0.008(8) C41 0.052(8) 0.083(9) 0.064(8) -0.016(7) 0.009(7) 0.013(7) C42 0.054(7) 0.051(7) 0.046(7) -0.006(5) -0.007(6) -0.003(6) _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 Pd1 C22 1.945(10) . ? Pd1 C1 1.972(10) . ? Pd1 N5 2.073(8) . ? Pd1 N10 2.074(8) . ? Ag1 N9 2.244(10) . ? Ag1 N4 2.262(11) . ? Ag1 N3 2.411(9) . ? Ag1 N8 2.469(9) . ? F1 P1 1.571(7) . ? F2 P1 1.580(8) . ? F3 P1 1.558(9) . ? F4 P1 1.578(8) . ? F5 P1 1.581(9) . ? F6 P1 1.573(8) . ? F7 P2 1.572(10) . ? F8 P2 1.551(9) . ? F9 P2 1.469(12) . ? F10 P2 1.499(11) . ? F11 P2 1.555(13) . ? F12 P2 1.542(11) . ? F13 P3 1.567(8) . ? F14 P3 1.561(9) . ? F15 P3 1.550(9) . ? F16 P3 1.540(12) . ? F17 P3 1.533(9) . ? F18 P3 1.526(11) . ? N1 C1 1.340(11) . ? N1 C3 1.341(13) . ? N1 C4 1.441(13) . ? N2 C1 1.317(12) . ? N2 C2 1.390(13) . ? N2 C16 1.482(12) . ? N3 C4 1.321(13) . ? N3 C8 1.373(14) . ? N4 C9 1.292(17) . ? N4 C13 1.351(16) . ? N5 C21 1.344(13) . ? N5 C17 1.344(13) . ? N6 C22 1.327(13) . ? N6 C24 1.393(14) . ? N6 C25 1.449(14) . ? N7 C22 1.344(13) . ? N7 C23 1.399(13) . ? N7 C37 1.450(13) . ? N8 C25 1.322(13) . ? N8 C29 1.369(14) . ? N9 C30 1.335(14) . ? N9 C34 1.358(16) . ? N10 C42 1.322(12) . ? N10 C38 1.337(13) . ? C2 C3 1.343(15) . ? C4 C5 1.409(16) . ? C5 C6 1.357(17) . ? C6 C7 1.384(18) . ? C7 C8 1.400(17) . ? C7 C14 1.402(18) . ? C8 C9 1.442(16) . ? C9 C10 1.432(19) . ? C10 C15 1.39(2) . ? C10 C11 1.42(2) . ? C11 C12 1.30(3) . ? C12 C13 1.40(2) . ? C14 C15 1.33(2) . ? C16 C17 1.516(14) . ? C17 C18 1.385(14) . ? C18 C19 1.354(17) . ? C19 C20 1.383(17) . ? C20 C21 1.357(14) . ? C23 C24 1.318(16) . ? C25 C26 1.370(14) . ? C26 C27 1.328(16) . ? C27 C28 1.411(16) . ? C28 C29 1.405(14) . ? C28 C35 1.432(17) . ? C29 C30 1.445(16) . ? C30 C31 1.411(18) . ? C31 C32 1.382(18) . ? C31 C36 1.406(18) . ? C32 C33 1.38(2) . ? C33 C34 1.36(2) . ? C35 C36 1.322(18) . ? C37 C38 1.517(14) . ? C38 C39 1.365(15) . ? C39 C40 1.389(16) . ? C40 C41 1.361(17) . ? C41 C42 1.384(15) . ? 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 C22 Pd1 C1 90.8(4) . . ? C22 Pd1 N5 176.1(4) . . ? C1 Pd1 N5 86.1(4) . . ? C22 Pd1 N10 86.5(4) . . ? C1 Pd1 N10 176.5(4) . . ? N5 Pd1 N10 96.7(3) . . ? N9 Ag1 N4 139.7(4) . . ? N9 Ag1 N3 140.6(3) . . ? N4 Ag1 N3 70.0(4) . . ? N9 Ag1 N8 70.6(3) . . ? N4 Ag1 N8 144.2(4) . . ? N3 Ag1 N8 96.9(3) . . ? C1 N1 C3 109.5(9) . . ? C1 N1 C4 123.9(9) . . ? C3 N1 C4 126.2(9) . . ? C1 N2 C2 110.7(8) . . ? C1 N2 C16 122.2(8) . . ? C2 N2 C16 127.1(9) . . ? C4 N3 C8 115.3(10) . . ? C4 N3 Ag1 130.5(7) . . ? C8 N3 Ag1 113.6(7) . . ? C9 N4 C13 117.6(13) . . ? C9 N4 Ag1 120.6(9) . . ? C13 N4 Ag1 121.8(11) . . ? C21 N5 C17 118.2(9) . . ? C21 N5 Pd1 121.5(7) . . ? C17 N5 Pd1 120.3(7) . . ? C22 N6 C24 111.2(10) . . ? C22 N6 C25 123.7(9) . . ? C24 N6 C25 124.2(9) . . ? C22 N7 C23 109.7(10) . . ? C22 N7 C37 121.3(9) . . ? C23 N7 C37 128.8(10) . . ? C25 N8 C29 115.7(9) . . ? C25 N8 Ag1 131.8(8) . . ? C29 N8 Ag1 112.2(7) . . ? C30 N9 C34 116.6(12) . . ? C30 N9 Ag1 120.5(8) . . ? C34 N9 Ag1 122.8(10) . . ? C42 N10 C38 118.2(9) . . ? C42 N10 Pd1 120.6(7) . . ? C38 N10 Pd1 121.2(7) . . ? F3 P1 F1 91.7(5) . . ? F3 P1 F6 91.0(6) . . ? F1 P1 F6 88.2(5) . . ? F3 P1 F4 89.6(5) . . ? F1 P1 F4 91.5(4) . . ? F6 P1 F4 179.3(6) . . ? F3 P1 F2 88.4(5) . . ? F1 P1 F2 178.6(5) . . ? F6 P1 F2 90.5(5) . . ? F4 P1 F2 89.9(5) . . ? F3 P1 F5 178.4(6) . . ? F1 P1 F5 87.6(5) . . ? F6 P1 F5 90.4(5) . . ? F4 P1 F5 89.0(5) . . ? F2 P1 F5 92.4(5) . . ? F9 P2 F10 94.3(11) . . ? F9 P2 F12 93.3(10) . . ? F10 P2 F12 172.3(10) . . ? F9 P2 F8 91.1(8) . . ? F10 P2 F8 89.1(7) . . ? F12 P2 F8 90.3(6) . . ? F9 P2 F11 178.0(11) . . ? F10 P2 F11 87.6(9) . . ? F12 P2 F11 84.8(8) . . ? F8 P2 F11 89.7(7) . . ? F9 P2 F7 88.9(8) . . ? F10 P2 F7 92.4(7) . . ? F12 P2 F7 88.2(6) . . ? F8 P2 F7 178.5(6) . . ? F11 P2 F7 90.3(7) . . ? F18 P3 F17 93.4(8) . . ? F18 P3 F16 176.5(7) . . ? F17 P3 F16 88.6(7) . . ? F18 P3 F15 87.4(8) . . ? F17 P3 F15 177.5(6) . . ? F16 P3 F15 90.5(7) . . ? F18 P3 F14 91.8(7) . . ? F17 P3 F14 91.8(5) . . ? F16 P3 F14 91.0(7) . . ? F15 P3 F14 90.6(5) . . ? F18 P3 F13 88.8(6) . . ? F17 P3 F13 89.5(5) . . ? F16 P3 F13 88.3(6) . . ? F15 P3 F13 88.1(5) . . ? F14 P3 F13 178.5(6) . . ? N2 C1 N1 106.4(8) . . ? N2 C1 Pd1 120.6(7) . . ? N1 C1 Pd1 133.0(8) . . ? C3 C2 N2 104.4(10) . . ? N1 C3 C2 109.0(10) . . ? N3 C4 C5 126.4(11) . . ? N3 C4 N1 114.0(9) . . ? C5 C4 N1 119.4(10) . . ? C6 C5 C4 115.7(12) . . ? C5 C6 C7 121.9(13) . . ? C6 C7 C8 117.4(12) . . ? C6 C7 C14 123.5(15) . . ? C8 C7 C14 119.1(14) . . ? N3 C8 C7 123.0(11) . . ? N3 C8 C9 116.6(13) . . ? C7 C8 C9 120.4(13) . . ? N4 C9 C10 124.7(13) . . ? N4 C9 C8 118.9(13) . . ? C10 C9 C8 116.4(15) . . ? C15 C10 C11 123.8(16) . . ? C15 C10 C9 120.8(14) . . ? C11 C10 C9 114.9(17) . . ? C12 C11 C10 120.2(18) . . ? C11 C12 C13 120.7(17) . . ? N4 C13 C12 121.6(16) . . ? C15 C14 C7 121.7(17) . . ? C14 C15 C10 121.0(15) . . ? N2 C16 C17 110.0(8) . . ? N5 C17 C18 122.3(11) . . ? N5 C17 C16 118.4(9) . . ? C18 C17 C16 119.3(10) . . ? C19 C18 C17 117.9(12) . . ? C18 C19 C20 120.8(12) . . ? C21 C20 C19 118.2(12) . . ? N5 C21 C20 122.5(11) . . ? N6 C22 N7 105.4(9) . . ? N6 C22 Pd1 132.8(8) . . ? N7 C22 Pd1 121.6(8) . . ? C24 C23 N7 107.3(11) . . ? C23 C24 N6 106.3(10) . . ? N8 C25 C26 125.5(11) . . ? N8 C25 N6 116.3(9) . . ? C26 C25 N6 118.2(10) . . ? C27 C26 C25 119.2(11) . . ? C26 C27 C28 119.9(11) . . ? C29 C28 C27 117.1(11) . . ? C29 C28 C35 118.9(11) . . ? C27 C28 C35 123.9(11) . . ? N8 C29 C28 122.5(11) . . ? N8 C29 C30 117.7(10) . . ? C28 C29 C30 119.6(11) . . ? N9 C30 C31 123.0(12) . . ? N9 C30 C29 119.0(12) . . ? C31 C30 C29 118.1(12) . . ? C32 C31 C36 122.6(14) . . ? C32 C31 C30 117.3(13) . . ? C36 C31 C30 120.1(13) . . ? C33 C32 C31 120.8(15) . . ? C34 C33 C32 117.5(15) . . ? N9 C34 C33 124.8(14) . . ? C36 C35 C28 121.0(13) . . ? C35 C36 C31 121.9(14) . . ? N7 C37 C38 112.7(9) . . ? N10 C38 C39 122.6(11) . . ? N10 C38 C37 118.0(10) . . ? C39 C38 C37 119.4(10) . . ? C38 C39 C40 118.7(12) . . ? C41 C40 C39 119.0(12) . . ? C40 C41 C42 118.6(12) . . ? N10 C42 C41 122.9(11) . . ? 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 N9 Ag1 N3 C4 -38.6(12) . . . . ? N4 Ag1 N3 C4 174.7(10) . . . . ? N8 Ag1 N3 C4 29.1(10) . . . . ? N9 Ag1 N3 C8 150.8(8) . . . . ? N4 Ag1 N3 C8 4.0(8) . . . . ? N8 Ag1 N3 C8 -141.5(8) . . . . ? N9 Ag1 N4 C9 -150.9(11) . . . . ? N3 Ag1 N4 C9 -3.4(11) . . . . ? N8 Ag1 N4 C9 70.1(13) . . . . ? N9 Ag1 N4 C13 28.4(15) . . . . ? N3 Ag1 N4 C13 175.8(13) . . . . ? N8 Ag1 N4 C13 -110.7(12) . . . . ? C22 Pd1 N5 C21 177(5) . . . . ? C1 Pd1 N5 C21 139.5(8) . . . . ? N10 Pd1 N5 C21 -38.5(8) . . . . ? C22 Pd1 N5 C17 -3(6) . . . . ? C1 Pd1 N5 C17 -40.5(8) . . . . ? N10 Pd1 N5 C17 141.5(8) . . . . ? N9 Ag1 N8 C25 175.5(11) . . . . ? N4 Ag1 N8 C25 -31.2(13) . . . . ? N3 Ag1 N8 C25 34.0(10) . . . . ? N9 Ag1 N8 C29 2.3(7) . . . . ? N4 Ag1 N8 C29 155.6(8) . . . . ? N3 Ag1 N8 C29 -139.2(7) . . . . ? N4 Ag1 N9 C30 -159.2(9) . . . . ? N3 Ag1 N9 C30 73.6(11) . . . . ? N8 Ag1 N9 C30 -3.2(9) . . . . ? N4 Ag1 N9 C34 26.0(14) . . . . ? N3 Ag1 N9 C34 -101.2(11) . . . . ? N8 Ag1 N9 C34 -178.0(11) . . . . ? C22 Pd1 N10 C42 141.9(9) . . . . ? C1 Pd1 N10 C42 180(100) . . . . ? N5 Pd1 N10 C42 -35.9(9) . . . . ? C22 Pd1 N10 C38 -38.6(9) . . . . ? C1 Pd1 N10 C38 -1(7) . . . . ? N5 Pd1 N10 C38 143.7(8) . . . . ? C2 N2 C1 N1 -1.4(12) . . . . ? C16 N2 C1 N1 175.9(9) . . . . ? C2 N2 C1 Pd1 175.7(8) . . . . ? C16 N2 C1 Pd1 -7.0(14) . . . . ? C3 N1 C1 N2 2.2(12) . . . . ? C4 N1 C1 N2 -170.8(9) . . . . ? C3 N1 C1 Pd1 -174.4(9) . . . . ? C4 N1 C1 Pd1 12.6(16) . . . . ? C22 Pd1 C1 N2 -132.5(9) . . . . ? N5 Pd1 C1 N2 45.1(8) . . . . ? N10 Pd1 C1 N2 -170(6) . . . . ? C22 Pd1 C1 N1 43.6(10) . . . . ? N5 Pd1 C1 N1 -138.7(10) . . . . ? N10 Pd1 C1 N1 6(7) . . . . ? C1 N2 C2 C3 0.1(14) . . . . ? C16 N2 C2 C3 -177.1(11) . . . . ? C1 N1 C3 C2 -2.2(14) . . . . ? C4 N1 C3 C2 170.6(11) . . . . ? N2 C2 C3 N1 1.3(14) . . . . ? C8 N3 C4 C5 1.8(17) . . . . ? Ag1 N3 C4 C5 -168.7(9) . . . . ? C8 N3 C4 N1 -172.5(9) . . . . ? Ag1 N3 C4 N1 17.0(14) . . . . ? C1 N1 C4 N3 -134.3(10) . . . . ? C3 N1 C4 N3 53.8(15) . . . . ? C1 N1 C4 C5 50.9(15) . . . . ? C3 N1 C4 C5 -120.9(12) . . . . ? N3 C4 C5 C6 -4.0(19) . . . . ? N1 C4 C5 C6 170.1(11) . . . . ? C4 C5 C6 C7 2(2) . . . . ? C5 C6 C7 C8 1(2) . . . . ? C5 C6 C7 C14 179.5(15) . . . . ? C4 N3 C8 C7 2.2(17) . . . . ? Ag1 N3 C8 C7 174.3(10) . . . . ? C4 N3 C8 C9 -176.6(11) . . . . ? Ag1 N3 C8 C9 -4.4(13) . . . . ? C6 C7 C8 N3 -4(2) . . . . ? C14 C7 C8 N3 178.0(13) . . . . ? C6 C7 C8 C9 174.9(13) . . . . ? C14 C7 C8 C9 -3(2) . . . . ? C13 N4 C9 C10 3(2) . . . . ? Ag1 N4 C9 C10 -177.9(11) . . . . ? C13 N4 C9 C8 -176.8(13) . . . . ? Ag1 N4 C9 C8 2.4(19) . . . . ? N3 C8 C9 N4 1.7(19) . . . . ? C7 C8 C9 N4 -177.1(13) . . . . ? N3 C8 C9 C10 -178.1(12) . . . . ? C7 C8 C9 C10 3(2) . . . . ? N4 C9 C10 C15 -177.3(17) . . . . ? C8 C9 C10 C15 2(2) . . . . ? N4 C9 C10 C11 -5(2) . . . . ? C8 C9 C10 C11 174.8(15) . . . . ? C15 C10 C11 C12 179(2) . . . . ? C9 C10 C11 C12 7(3) . . . . ? C10 C11 C12 C13 -6(4) . . . . ? C9 N4 C13 C12 -2(2) . . . . ? Ag1 N4 C13 C12 178.5(14) . . . . ? C11 C12 C13 N4 4(3) . . . . ? C6 C7 C14 C15 179.5(18) . . . . ? C8 C7 C14 C15 -2(3) . . . . ? C7 C14 C15 C10 8(3) . . . . ? C11 C10 C15 C14 -179.9(19) . . . . ? C9 C10 C15 C14 -8(3) . . . . ? C1 N2 C16 C17 -51.5(14) . . . . ? C2 N2 C16 C17 125.4(12) . . . . ? C21 N5 C17 C18 -0.1(15) . . . . ? Pd1 N5 C17 C18 179.9(8) . . . . ? C21 N5 C17 C16 178.3(9) . . . . ? Pd1 N5 C17 C16 -1.7(13) . . . . ? N2 C16 C17 N5 54.3(13) . . . . ? N2 C16 C17 C18 -127.3(10) . . . . ? N5 C17 C18 C19 1.4(17) . . . . ? C16 C17 C18 C19 -176.9(11) . . . . ? C17 C18 C19 C20 -0.7(19) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C17 N5 C21 C20 -2.1(16) . . . . ? Pd1 N5 C21 C20 177.9(9) . . . . ? C19 C20 C21 N5 2.8(18) . . . . ? C24 N6 C22 N7 2.6(12) . . . . ? C25 N6 C22 N7 -166.4(10) . . . . ? C24 N6 C22 Pd1 -173.6(9) . . . . ? C25 N6 C22 Pd1 17.4(17) . . . . ? C23 N7 C22 N6 -1.9(12) . . . . ? C37 N7 C22 N6 174.1(9) . . . . ? C23 N7 C22 Pd1 174.8(8) . . . . ? C37 N7 C22 Pd1 -9.1(14) . . . . ? C1 Pd1 C22 N6 42.2(11) . . . . ? N5 Pd1 C22 N6 5(6) . . . . ? N10 Pd1 C22 N6 -139.9(11) . . . . ? C1 Pd1 C22 N7 -133.5(9) . . . . ? N5 Pd1 C22 N7 -171(5) . . . . ? N10 Pd1 C22 N7 44.4(8) . . . . ? C22 N7 C23 C24 0.5(14) . . . . ? C37 N7 C23 C24 -175.2(11) . . . . ? N7 C23 C24 N6 1.1(14) . . . . ? C22 N6 C24 C23 -2.4(14) . . . . ? C25 N6 C24 C23 166.6(11) . . . . ? C29 N8 C25 C26 0.5(17) . . . . ? Ag1 N8 C25 C26 -172.5(9) . . . . ? C29 N8 C25 N6 -179.6(9) . . . . ? Ag1 N8 C25 N6 7.3(15) . . . . ? C22 N6 C25 N8 -128.9(11) . . . . ? C24 N6 C25 N8 63.5(15) . . . . ? C22 N6 C25 C26 51.0(16) . . . . ? C24 N6 C25 C26 -116.7(13) . . . . ? N8 C25 C26 C27 -0.6(19) . . . . ? N6 C25 C26 C27 179.5(11) . . . . ? C25 C26 C27 C28 0.3(19) . . . . ? C26 C27 C28 C29 0.0(18) . . . . ? C26 C27 C28 C35 -178.5(13) . . . . ? C25 N8 C29 C28 -0.2(16) . . . . ? Ag1 N8 C29 C28 174.2(9) . . . . ? C25 N8 C29 C30 -175.7(10) . . . . ? Ag1 N8 C29 C30 -1.3(12) . . . . ? C27 C28 C29 N8 0.0(17) . . . . ? C35 C28 C29 N8 178.5(12) . . . . ? C27 C28 C29 C30 175.4(11) . . . . ? C35 C28 C29 C30 -6.1(18) . . . . ? C34 N9 C30 C31 -2.2(19) . . . . ? Ag1 N9 C30 C31 -177.3(10) . . . . ? C34 N9 C30 C29 179.0(11) . . . . ? Ag1 N9 C30 C29 3.8(15) . . . . ? N8 C29 C30 N9 -1.4(16) . . . . ? C28 C29 C30 N9 -177.1(11) . . . . ? N8 C29 C30 C31 179.7(11) . . . . ? C28 C29 C30 C31 4.0(17) . . . . ? N9 C30 C31 C32 -1(2) . . . . ? C29 C30 C31 C32 178.2(13) . . . . ? N9 C30 C31 C36 -177.5(13) . . . . ? C29 C30 C31 C36 1(2) . . . . ? C36 C31 C32 C33 -179.7(16) . . . . ? C30 C31 C32 C33 4(3) . . . . ? C31 C32 C33 C34 -3(3) . . . . ? C30 N9 C34 C33 2(2) . . . . ? Ag1 N9 C34 C33 177.4(13) . . . . ? C32 C33 C34 N9 0(3) . . . . ? C29 C28 C35 C36 3(2) . . . . ? C27 C28 C35 C36 -178.9(14) . . . . ? C28 C35 C36 C31 3(2) . . . . ? C32 C31 C36 C35 178.4(16) . . . . ? C30 C31 C36 C35 -5(2) . . . . ? C22 N7 C37 C38 -48.3(14) . . . . ? C23 N7 C37 C38 126.9(12) . . . . ? C42 N10 C38 C39 -2.1(17) . . . . ? Pd1 N10 C38 C39 178.3(9) . . . . ? C42 N10 C38 C37 177.8(10) . . . . ? Pd1 N10 C38 C37 -1.7(14) . . . . ? N7 C37 C38 N10 52.5(14) . . . . ? N7 C37 C38 C39 -127.6(12) . . . . ? N10 C38 C39 C40 3.8(18) . . . . ? C37 C38 C39 C40 -176.2(11) . . . . ? C38 C39 C40 C41 -2.7(19) . . . . ? C39 C40 C41 C42 0(2) . . . . ? C38 N10 C42 C41 -0.6(17) . . . . ? Pd1 N10 C42 C41 179.0(9) . . . . ? C40 C41 C42 N10 1.5(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.707 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.106 # Attachment 'web_deposit_cif_file_4_ShaojinGu_1283865305.cif' data_100113_gsjr1292 _database_code_depnum_ccdc_archive 'CCDC 792162' #TrackingRef 'web_deposit_cif_file_4_ShaojinGu_1283865305.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 Cu F18 N12 P3 Pd' _chemical_formula_weight 1361.72 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' Pd Pd -0.9988 1.0072 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/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 21.9896(6) _cell_length_b 13.9782(4) _cell_length_c 17.6873(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.695(2) _cell_angle_gamma 90.00 _cell_volume 5342.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7417 _exptl_absorpt_correction_T_max 0.7798 _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 ? _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 23861 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9387 _reflns_number_gt 5494 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0463P)^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 9387 _refine_ls_number_parameters 732 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.257286(14) 0.62457(3) 0.060848(19) 0.03785(12) Uani 1 1 d . . . Cu1 Cu 0.23081(3) 0.26576(5) 0.15545(3) 0.05620(19) Uani 1 1 d . . . N1 N 0.33819(15) 0.7048(3) 0.0648(2) 0.0419(9) Uani 1 1 d . . . N2 N 0.19674(16) 0.7270(3) 0.0031(2) 0.0459(10) Uani 1 1 d . . . N3 N 0.13741(16) 0.5402(3) 0.0016(2) 0.0469(10) Uani 1 1 d . . . N4 N 0.16644(15) 0.4872(3) 0.1163(2) 0.0403(9) Uani 1 1 d . . . N5 N 0.31695(14) 0.4291(3) 0.0909(2) 0.0379(9) Uani 1 1 d . . . N6 N 0.36045(15) 0.5406(3) 0.1653(2) 0.0391(9) Uani 1 1 d . . . N7 N 0.29192(18) 0.2347(3) 0.2497(2) 0.0559(11) Uani 1 1 d . . . N8 N 0.22651(16) 0.3965(3) 0.2137(2) 0.0421(10) Uani 1 1 d . . . N9 N 0.16648(17) 0.1850(3) 0.0916(2) 0.0523(11) Uani 1 1 d . . . N10 N 0.24286(15) 0.3134(3) 0.0484(2) 0.0391(9) Uani 1 1 d . . . N12 N 0.0190(6) 0.6996(9) 0.0182(7) 0.166(5) Uani 1 1 d . . . N13 N 0.5830(3) 0.0260(5) 0.5014(4) 0.103(2) Uani 1 1 d . . . C1 C 0.1288(3) 0.1207(4) 0.1132(3) 0.0729(17) Uani 1 1 d . . . H1 H 0.1325 0.1073 0.1653 0.088 Uiso 1 1 calc R . . C2 C 0.0839(3) 0.0723(5) 0.0613(4) 0.085(2) Uani 1 1 d . . . H2 H 0.0589 0.0271 0.0790 0.101 Uiso 1 1 calc R . . C3 C 0.0766(2) 0.0909(4) -0.0150(4) 0.0729(17) Uani 1 1 d . . . H3 H 0.0460 0.0600 -0.0498 0.087 Uiso 1 1 calc R . . C4 C 0.1161(2) 0.1582(4) -0.0408(3) 0.0538(14) Uani 1 1 d . . . C5 C 0.1116(2) 0.1858(4) -0.1202(3) 0.0634(15) Uani 1 1 d . . . H5 H 0.0836 0.1543 -0.1579 0.076 Uiso 1 1 calc R . . C6 C 0.1462(2) 0.2546(4) -0.1407(3) 0.0609(15) Uani 1 1 d . . . H6 H 0.1407 0.2727 -0.1922 0.073 Uiso 1 1 calc R . . C7 C 0.1923(2) 0.3023(3) -0.0854(3) 0.0449(12) Uani 1 1 d . . . C8 C 0.2283(2) 0.3791(4) -0.1021(3) 0.0504(12) Uani 1 1 d . . . H8 H 0.2236 0.4017 -0.1523 0.060 Uiso 1 1 calc R . . C9 C 0.2703(2) 0.4210(3) -0.0453(3) 0.0479(12) Uani 1 1 d . . . H9 H 0.2946 0.4719 -0.0559 0.058 Uiso 1 1 calc R . . C10 C 0.27546(19) 0.3849(3) 0.0290(2) 0.0397(11) Uani 1 1 d . . . C11 C 0.20007(19) 0.2733(3) -0.0088(3) 0.0416(11) Uani 1 1 d . . . C12 C 0.16029(19) 0.2023(3) 0.0152(3) 0.0438(12) Uani 1 1 d . . . C13 C 0.36676(19) 0.3883(4) 0.1399(3) 0.0461(12) Uani 1 1 d . . . H13 H 0.3792 0.3247 0.1406 0.055 Uiso 1 1 calc R . . C14 C 0.3933(2) 0.4583(4) 0.1858(3) 0.0499(13) Uani 1 1 d . . . H14 H 0.4279 0.4523 0.2248 0.060 Uiso 1 1 calc R . . C15 C 0.31348(17) 0.5228(4) 0.1074(2) 0.0380(11) Uani 1 1 d . . . C16 C 0.3742(2) 0.6384(4) 0.1924(3) 0.0499(13) Uani 1 1 d . . . H16A H 0.4113 0.6386 0.2318 0.060 Uiso 1 1 calc R . . H16B H 0.3403 0.6625 0.2152 0.060 Uiso 1 1 calc R . . C17 C 0.3833(2) 0.7023(3) 0.1274(3) 0.0441(12) Uani 1 1 d . . . C18 C 0.4366(2) 0.7560(4) 0.1311(3) 0.0634(15) Uani 1 1 d . . . H18 H 0.4671 0.7551 0.1753 0.076 Uiso 1 1 calc R . . C19 C 0.4442(3) 0.8099(4) 0.0700(4) 0.0788(19) Uani 1 1 d . . . H19 H 0.4797 0.8467 0.0724 0.095 Uiso 1 1 calc R . . C20 C 0.3997(3) 0.8107(4) 0.0045(4) 0.0708(17) Uani 1 1 d . . . H20 H 0.4046 0.8465 -0.0382 0.085 Uiso 1 1 calc R . . C21 C 0.3477(2) 0.7570(4) 0.0044(3) 0.0525(13) Uani 1 1 d . . . H21 H 0.3173 0.7567 -0.0399 0.063 Uiso 1 1 calc R . . C22 C 0.2068(2) 0.8201(4) 0.0181(3) 0.0570(14) Uani 1 1 d . . . H22 H 0.2384 0.8374 0.0582 0.068 Uiso 1 1 calc R . . C23 C 0.1726(3) 0.8910(4) -0.0229(3) 0.0731(17) Uani 1 1 d . . . H23 H 0.1808 0.9552 -0.0112 0.088 Uiso 1 1 calc R . . C24 C 0.1256(3) 0.8644(5) -0.0820(3) 0.0815(19) Uani 1 1 d . . . H24 H 0.1024 0.9108 -0.1122 0.098 Uiso 1 1 calc R . . C25 C 0.1133(2) 0.7692(5) -0.0961(3) 0.0681(17) Uani 1 1 d . . . H25 H 0.0806 0.7507 -0.1347 0.082 Uiso 1 1 calc R . . C26 C 0.1496(2) 0.7006(4) -0.0528(3) 0.0488(13) Uani 1 1 d . . . C27 C 0.1379(2) 0.5965(4) -0.0683(3) 0.0578(15) Uani 1 1 d . . . H27A H 0.0983 0.5890 -0.1027 0.069 Uiso 1 1 calc R . . H27B H 0.1696 0.5714 -0.0944 0.069 Uiso 1 1 calc R . . C28 C 0.0925(2) 0.4772(4) 0.0151(3) 0.0563(14) Uani 1 1 d . . . H28 H 0.0564 0.4613 -0.0189 0.068 Uiso 1 1 calc R . . C29 C 0.1105(2) 0.4434(4) 0.0864(3) 0.0510(13) Uani 1 1 d . . . H29 H 0.0896 0.3990 0.1113 0.061 Uiso 1 1 calc R . . C30 C 0.18346(18) 0.5464(3) 0.0627(2) 0.0414(12) Uani 1 1 d . . . C31 C 0.2013(2) 0.4799(4) 0.1930(3) 0.0424(12) Uani 1 1 d . . . C32 C 0.2081(2) 0.5616(4) 0.2390(3) 0.0559(13) Uani 1 1 d . . . H32 H 0.1892 0.6189 0.2211 0.067 Uiso 1 1 calc R . . C33 C 0.2431(3) 0.5551(4) 0.3107(3) 0.0674(16) Uani 1 1 d . . . H33 H 0.2476 0.6079 0.3432 0.081 Uiso 1 1 calc R . . C34 C 0.2723(2) 0.4691(4) 0.3354(3) 0.0609(15) Uani 1 1 d . . . C35 C 0.3132(3) 0.4581(6) 0.4085(3) 0.093(2) Uani 1 1 d . . . H35 H 0.3175 0.5077 0.4441 0.112 Uiso 1 1 calc R . . C36 C 0.3448(3) 0.3776(6) 0.4253(4) 0.100(2) Uani 1 1 d . . . H36 H 0.3703 0.3720 0.4733 0.120 Uiso 1 1 calc R . . C37 C 0.3412(2) 0.2998(5) 0.3734(3) 0.0677(16) Uani 1 1 d . . . C38 C 0.3768(3) 0.2175(6) 0.3863(5) 0.093(2) Uani 1 1 d . . . H38 H 0.4048 0.2101 0.4323 0.111 Uiso 1 1 calc R . . C39 C 0.3708(3) 0.1477(6) 0.3324(4) 0.092(2) Uani 1 1 d . . . H39 H 0.3957 0.0935 0.3404 0.110 Uiso 1 1 calc R . . C40 C 0.3270(3) 0.1573(4) 0.2643(3) 0.0740(17) Uani 1 1 d . . . H40 H 0.3223 0.1080 0.2284 0.089 Uiso 1 1 calc R . . C41 C 0.2989(2) 0.3058(4) 0.3030(3) 0.0507(13) Uani 1 1 d . . . C42 C 0.2643(2) 0.3922(4) 0.2844(3) 0.0453(12) Uani 1 1 d . . . C43 C 0.5418(3) 0.1083(5) 0.6119(4) 0.111(2) Uani 1 1 d . . . H43A H 0.5284 0.0601 0.6439 0.167 Uiso 1 1 calc R . . H43B H 0.5076 0.1492 0.5915 0.167 Uiso 1 1 calc R . . H43C H 0.5742 0.1456 0.6420 0.167 Uiso 1 1 calc R . . C44 C 0.5647(3) 0.0631(5) 0.5495(4) 0.0760(18) Uani 1 1 d . . . C45 C 0.0734(5) 0.7707(8) 0.1471(8) 0.157(4) Uani 1 1 d . . . H45A H 0.0606 0.8358 0.1511 0.235 Uiso 1 1 calc R . . H45B H 0.1175 0.7685 0.1503 0.235 Uiso 1 1 calc R . . H45C H 0.0623 0.7338 0.1883 0.235 Uiso 1 1 calc R . . C46 C 0.0437(6) 0.7322(9) 0.0756(10) 0.134(5) Uani 1 1 d . . . P1 P 0.26453(8) 0.85779(12) 0.26891(10) 0.0751(5) Uani 1 1 d . . . P2 P 0.46509(6) 0.11009(13) 0.13673(8) 0.0675(4) Uani 1 1 d . . . P3 P 0.00682(6) 0.02630(12) 0.26267(7) 0.0582(4) Uani 1 1 d . . . F1 F 0.2431(2) 0.7848(3) 0.2019(2) 0.1492(18) Uani 1 1 d . . . F2 F 0.3110(3) 0.7779(4) 0.3082(3) 0.161(2) Uani 1 1 d . . . F3 F 0.3144(3) 0.8875(6) 0.2302(5) 0.251(4) Uani 1 1 d . . . F4 F 0.2876(3) 0.9230(5) 0.3361(4) 0.251(4) Uani 1 1 d . . . F5 F 0.2205(3) 0.9329(4) 0.2357(5) 0.250(4) Uani 1 1 d . . . F6 F 0.2174(4) 0.8117(6) 0.3076(5) 0.258(4) Uani 1 1 d . . . F7 F 0.4523(3) 0.0398(4) 0.0721(3) 0.219(3) Uani 1 1 d . . . F8 F 0.53476(19) 0.1065(6) 0.1445(2) 0.234(4) Uani 1 1 d . . . F9 F 0.4622(2) 0.1851(4) 0.0696(3) 0.170(2) Uani 1 1 d . . . F10 F 0.4763(3) 0.1933(5) 0.1952(3) 0.215(3) Uani 1 1 d . . . F11 F 0.39615(18) 0.1300(5) 0.1273(3) 0.195(3) Uani 1 1 d . . . F12 F 0.4702(3) 0.0502(5) 0.2060(3) 0.227(3) Uani 1 1 d . . . F13 F 0.00700(17) -0.0782(3) 0.2940(2) 0.1167(13) Uani 1 1 d . . . F14 F -0.00356(18) -0.0105(3) 0.17758(19) 0.1139(13) Uani 1 1 d . . . F15 F -0.06471(15) 0.0326(4) 0.2551(2) 0.1397(18) Uani 1 1 d . . . F16 F 0.00792(19) 0.1306(3) 0.2306(2) 0.1238(14) Uani 1 1 d . . . F17 F 0.0166(2) 0.0615(4) 0.3471(2) 0.1480(18) Uani 1 1 d . . . F18 F 0.07867(14) 0.0218(3) 0.2689(2) 0.1190(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03431(19) 0.0422(2) 0.0347(2) 0.00184(18) 0.00038(13) 0.00296(16) Cu1 0.0712(4) 0.0549(5) 0.0419(4) -0.0007(3) 0.0088(3) -0.0135(3) N1 0.038(2) 0.037(3) 0.048(2) 0.000(2) 0.0030(18) 0.0021(17) N2 0.043(2) 0.054(3) 0.038(2) 0.007(2) 0.0014(17) 0.0117(19) N3 0.035(2) 0.063(3) 0.039(2) 0.003(2) -0.0015(17) -0.0011(19) N4 0.034(2) 0.050(3) 0.036(2) 0.003(2) 0.0054(16) 0.0027(18) N5 0.036(2) 0.035(3) 0.042(2) -0.0005(19) 0.0053(16) -0.0014(17) N6 0.036(2) 0.036(3) 0.042(2) -0.0013(19) -0.0016(16) 0.0015(18) N7 0.065(3) 0.050(3) 0.055(3) 0.017(2) 0.018(2) 0.001(2) N8 0.044(2) 0.048(3) 0.033(2) 0.0032(19) 0.0029(16) -0.0085(19) N9 0.062(3) 0.046(3) 0.052(3) -0.002(2) 0.018(2) -0.017(2) N10 0.045(2) 0.032(2) 0.041(2) 0.0001(19) 0.0100(17) -0.0062(18) N12 0.170(10) 0.134(10) 0.225(13) 0.014(8) 0.119(9) -0.002(7) N13 0.079(4) 0.117(6) 0.122(5) 0.000(4) 0.038(4) 0.000(3) C1 0.088(4) 0.067(4) 0.069(4) -0.006(3) 0.029(3) -0.029(3) C2 0.088(4) 0.086(5) 0.085(5) -0.009(4) 0.028(4) -0.051(4) C3 0.063(4) 0.074(5) 0.084(5) -0.017(4) 0.018(3) -0.033(3) C4 0.052(3) 0.050(4) 0.060(3) -0.010(3) 0.011(3) -0.009(2) C5 0.056(3) 0.071(4) 0.058(4) -0.018(3) -0.001(3) -0.008(3) C6 0.067(3) 0.071(4) 0.044(3) -0.004(3) 0.007(3) -0.010(3) C7 0.050(3) 0.042(3) 0.044(3) -0.005(2) 0.011(2) -0.004(2) C8 0.065(3) 0.053(4) 0.036(3) -0.003(3) 0.017(2) -0.003(3) C9 0.059(3) 0.045(3) 0.044(3) 0.002(3) 0.018(2) -0.012(2) C10 0.041(2) 0.037(3) 0.043(3) -0.005(2) 0.012(2) -0.002(2) C11 0.044(3) 0.039(3) 0.042(3) -0.005(2) 0.009(2) -0.003(2) C12 0.045(3) 0.043(3) 0.046(3) -0.010(2) 0.015(2) -0.006(2) C13 0.043(3) 0.036(3) 0.058(3) 0.010(3) 0.007(2) 0.010(2) C14 0.039(3) 0.054(4) 0.053(3) 0.013(3) -0.001(2) 0.006(3) C15 0.028(2) 0.047(3) 0.037(3) 0.001(2) 0.0031(19) -0.003(2) C16 0.046(3) 0.053(4) 0.045(3) -0.006(3) -0.007(2) -0.001(2) C17 0.046(3) 0.031(3) 0.053(3) -0.006(2) 0.003(2) -0.001(2) C18 0.057(3) 0.051(4) 0.078(4) -0.005(3) 0.000(3) -0.012(3) C19 0.060(4) 0.051(4) 0.123(6) 0.007(4) 0.009(4) -0.017(3) C20 0.064(4) 0.056(4) 0.098(5) 0.021(3) 0.028(3) 0.002(3) C21 0.056(3) 0.045(3) 0.057(3) 0.003(3) 0.013(2) 0.006(3) C22 0.060(3) 0.059(4) 0.050(3) 0.004(3) 0.006(2) 0.015(3) C23 0.082(4) 0.059(4) 0.075(4) 0.014(3) 0.006(3) 0.022(3) C24 0.082(4) 0.085(6) 0.070(4) 0.024(4) -0.002(3) 0.031(4) C25 0.053(3) 0.099(6) 0.047(3) 0.016(4) -0.005(2) 0.016(3) C26 0.041(3) 0.069(4) 0.035(3) 0.008(3) 0.004(2) 0.011(3) C27 0.047(3) 0.081(5) 0.041(3) 0.007(3) -0.004(2) -0.003(3) C28 0.035(3) 0.079(4) 0.051(3) -0.005(3) 0.000(2) -0.005(3) C29 0.040(3) 0.061(4) 0.051(3) 0.000(3) 0.007(2) -0.007(2) C30 0.033(2) 0.052(3) 0.037(3) -0.004(2) 0.002(2) 0.003(2) C31 0.046(3) 0.045(4) 0.036(3) 0.001(3) 0.009(2) -0.005(2) C32 0.076(4) 0.046(4) 0.048(3) -0.003(3) 0.017(3) 0.007(3) C33 0.092(4) 0.060(4) 0.050(3) -0.018(3) 0.012(3) -0.012(3) C34 0.078(4) 0.057(4) 0.044(3) -0.002(3) 0.001(3) -0.018(3) C35 0.125(6) 0.090(6) 0.050(4) -0.005(4) -0.023(4) -0.026(4) C36 0.115(6) 0.108(6) 0.057(4) 0.016(5) -0.037(4) -0.034(5) C37 0.066(4) 0.073(5) 0.056(4) 0.023(3) -0.009(3) -0.013(3) C38 0.069(4) 0.111(7) 0.092(6) 0.056(5) -0.003(4) 0.002(4) C39 0.078(4) 0.102(7) 0.097(6) 0.055(5) 0.022(4) 0.034(4) C40 0.089(4) 0.063(4) 0.075(4) 0.028(3) 0.029(3) 0.016(3) C41 0.053(3) 0.053(4) 0.044(3) 0.012(3) 0.004(2) -0.013(3) C42 0.050(3) 0.048(4) 0.036(3) 0.004(3) 0.003(2) -0.012(2) C43 0.105(5) 0.098(6) 0.141(7) -0.013(5) 0.051(5) 0.018(4) C44 0.056(4) 0.068(5) 0.107(6) 0.011(4) 0.022(4) 0.000(3) C45 0.135(8) 0.117(9) 0.227(13) 0.015(9) 0.056(9) 0.000(6) C46 0.126(11) 0.088(10) 0.217(17) 0.022(10) 0.106(11) 0.018(7) P1 0.0905(12) 0.0631(12) 0.0778(11) -0.0182(10) 0.0317(9) -0.0016(9) P2 0.0615(9) 0.0857(13) 0.0494(9) -0.0022(9) -0.0055(7) -0.0033(8) P3 0.0576(9) 0.0750(12) 0.0386(8) 0.0059(8) 0.0003(6) 0.0056(7) F1 0.207(5) 0.128(4) 0.095(3) -0.034(3) -0.016(3) 0.004(3) F2 0.220(5) 0.120(4) 0.121(4) -0.023(3) -0.027(4) 0.041(4) F3 0.211(6) 0.255(8) 0.330(9) 0.053(7) 0.164(7) -0.046(6) F4 0.291(8) 0.184(6) 0.234(7) -0.165(6) -0.064(6) 0.064(5) F5 0.217(6) 0.127(5) 0.349(9) -0.023(6) -0.094(6) 0.096(5) F6 0.303(9) 0.249(8) 0.290(8) -0.003(7) 0.228(7) -0.035(7) F7 0.293(7) 0.122(5) 0.181(5) -0.076(4) -0.113(5) 0.086(4) F8 0.072(3) 0.551(12) 0.073(3) 0.010(5) 0.002(2) 0.051(5) F9 0.189(5) 0.183(5) 0.112(4) 0.056(4) -0.043(3) -0.069(4) F10 0.293(8) 0.187(6) 0.124(4) -0.058(4) -0.066(5) 0.016(5) F11 0.077(3) 0.408(10) 0.099(3) 0.004(4) 0.014(2) 0.007(4) F12 0.209(6) 0.273(8) 0.176(5) 0.170(6) -0.022(4) -0.024(5) F13 0.116(3) 0.104(3) 0.122(3) 0.041(3) 0.004(2) -0.009(2) F14 0.141(3) 0.140(4) 0.055(2) -0.021(2) 0.006(2) -0.016(3) F15 0.065(2) 0.237(5) 0.117(3) 0.057(3) 0.015(2) 0.036(3) F16 0.149(4) 0.086(3) 0.124(3) 0.025(3) -0.007(3) 0.005(2) F17 0.195(4) 0.192(5) 0.047(2) -0.026(3) -0.001(2) 0.032(4) F18 0.060(2) 0.167(4) 0.126(3) 0.037(3) 0.007(2) -0.001(2) _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 Pd1 C30 1.962(4) . ? Pd1 C15 1.963(4) . ? Pd1 N2 2.088(4) . ? Pd1 N1 2.093(3) . ? Cu1 N7 1.985(4) . ? Cu1 N9 1.989(4) . ? Cu1 N10 2.071(3) . ? Cu1 N8 2.109(4) . ? N1 C21 1.342(6) . ? N1 C17 1.344(5) . ? N2 C22 1.338(6) . ? N2 C26 1.344(5) . ? N3 C30 1.341(5) . ? N3 C28 1.377(6) . ? N3 C27 1.467(6) . ? N4 C30 1.362(5) . ? N4 C29 1.388(5) . ? N4 C31 1.432(5) . ? N5 C15 1.346(5) . ? N5 C13 1.387(5) . ? N5 C10 1.430(5) . ? N6 C15 1.336(5) . ? N6 C14 1.372(5) . ? N6 C16 1.461(6) . ? N7 C40 1.326(6) . ? N7 C41 1.358(6) . ? N8 C31 1.313(6) . ? N8 C42 1.368(5) . ? N9 C1 1.325(6) . ? N9 C12 1.356(6) . ? N10 C10 1.312(5) . ? N10 C11 1.367(5) . ? N12 C46 1.153(15) . ? N13 C44 1.131(8) . ? C1 C2 1.392(7) . ? C1 H1 0.9300 . ? C2 C3 1.353(8) . ? C2 H2 0.9300 . ? C3 C4 1.412(7) . ? C3 H3 0.9300 . ? C4 C12 1.395(6) . ? C4 C5 1.443(7) . ? C5 C6 1.318(7) . ? C5 H5 0.9300 . ? C6 C7 1.436(6) . ? C6 H6 0.9300 . ? C7 C11 1.394(6) . ? C7 C8 1.398(6) . ? C8 C9 1.364(6) . ? C8 H8 0.9300 . ? C9 C10 1.393(6) . ? C9 H9 0.9300 . ? C11 C12 1.439(6) . ? C13 C14 1.335(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.499(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.384(6) . ? C18 C19 1.353(7) . ? C18 H18 0.9300 . ? C19 C20 1.370(7) . ? C19 H19 0.9300 . ? C20 C21 1.367(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.368(7) . ? C22 H22 0.9300 . ? C23 C24 1.377(8) . ? C23 H23 0.9300 . ? C24 C25 1.373(8) . ? C24 H24 0.9300 . ? C25 C26 1.385(7) . ? C25 H25 0.9300 . ? C26 C27 1.495(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.337(6) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 C32 1.395(6) . ? C32 C33 1.359(7) . ? C32 H32 0.9300 . ? C33 C34 1.394(7) . ? C33 H33 0.9300 . ? C34 C42 1.394(7) . ? C34 C35 1.439(7) . ? C35 C36 1.328(9) . ? C35 H35 0.9300 . ? C36 C37 1.416(9) . ? C36 H36 0.9300 . ? C37 C38 1.386(9) . ? C37 C41 1.412(6) . ? C38 C39 1.354(9) . ? C38 H38 0.9300 . ? C39 C40 1.402(8) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.433(7) . ? C43 C44 1.442(9) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C45 C46 1.417(14) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? P1 F3 1.458(5) . ? P1 F5 1.475(5) . ? P1 F6 1.491(6) . ? P1 F4 1.509(5) . ? P1 F1 1.568(4) . ? P1 F2 1.585(5) . ? P2 F12 1.471(4) . ? P2 F7 1.494(5) . ? P2 F8 1.513(4) . ? P2 F11 1.520(4) . ? P2 F10 1.545(5) . ? P2 F9 1.576(5) . ? P3 F17 1.549(4) . ? P3 F15 1.556(3) . ? P3 F13 1.562(4) . ? P3 F18 1.565(3) . ? P3 F16 1.566(4) . ? P3 F14 1.567(3) . ? 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 C30 Pd1 C15 92.74(18) . . ? C30 Pd1 N2 86.30(17) . . ? C15 Pd1 N2 175.43(17) . . ? C30 Pd1 N1 176.83(16) . . ? C15 Pd1 N1 84.80(16) . . ? N2 Pd1 N1 96.31(15) . . ? N7 Cu1 N9 130.66(18) . . ? N7 Cu1 N10 131.06(15) . . ? N9 Cu1 N10 82.06(15) . . ? N7 Cu1 N8 82.16(17) . . ? N9 Cu1 N8 132.66(15) . . ? N10 Cu1 N8 101.14(14) . . ? C21 N1 C17 118.0(4) . . ? C21 N1 Pd1 121.5(3) . . ? C17 N1 Pd1 120.4(3) . . ? C22 N2 C26 119.2(4) . . ? C22 N2 Pd1 120.2(3) . . ? C26 N2 Pd1 120.4(4) . . ? C30 N3 C28 111.1(4) . . ? C30 N3 C27 121.5(4) . . ? C28 N3 C27 127.4(4) . . ? C30 N4 C29 110.0(4) . . ? C30 N4 C31 122.3(4) . . ? C29 N4 C31 127.6(4) . . ? C15 N5 C13 109.6(4) . . ? C15 N5 C10 122.2(4) . . ? C13 N5 C10 128.2(4) . . ? C15 N6 C14 109.9(4) . . ? C15 N6 C16 120.7(4) . . ? C14 N6 C16 129.1(4) . . ? C40 N7 C41 118.3(5) . . ? C40 N7 Cu1 128.4(4) . . ? C41 N7 Cu1 113.3(3) . . ? C31 N8 C42 116.6(4) . . ? C31 N8 Cu1 133.4(3) . . ? C42 N8 Cu1 109.5(3) . . ? C1 N9 C12 117.1(4) . . ? C1 N9 Cu1 129.7(4) . . ? C12 N9 Cu1 113.2(3) . . ? C10 N10 C11 117.0(4) . . ? C10 N10 Cu1 130.8(3) . . ? C11 N10 Cu1 110.9(3) . . ? N9 C1 C2 123.0(5) . . ? N9 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 118.9(5) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C12 C4 C3 117.0(5) . . ? C12 C4 C5 119.0(5) . . ? C3 C4 C5 123.9(5) . . ? C6 C5 C4 121.6(5) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 121.5(5) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C11 C7 C8 117.2(4) . . ? C11 C7 C6 118.1(4) . . ? C8 C7 C6 124.6(5) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 117.7(4) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? N10 C10 C9 124.7(4) . . ? N10 C10 N5 115.5(4) . . ? C9 C10 N5 119.7(4) . . ? N10 C11 C7 122.9(4) . . ? N10 C11 C12 116.0(4) . . ? C7 C11 C12 121.0(4) . . ? N9 C12 C4 123.8(4) . . ? N9 C12 C11 117.6(4) . . ? C4 C12 C11 118.5(4) . . ? C14 C13 N5 106.5(4) . . ? C14 C13 H13 126.7 . . ? N5 C13 H13 126.7 . . ? C13 C14 N6 107.7(4) . . ? C13 C14 H14 126.2 . . ? N6 C14 H14 126.2 . . ? N6 C15 N5 106.3(4) . . ? N6 C15 Pd1 121.5(4) . . ? N5 C15 Pd1 132.1(3) . . ? N6 C16 C17 110.7(4) . . ? N6 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N1 C17 C18 121.0(5) . . ? N1 C17 C16 117.7(4) . . ? C18 C17 C16 121.4(4) . . ? C19 C18 C17 119.5(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.4(5) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 117.6(5) . . ? C21 C20 H20 121.2 . . ? C19 C20 H20 121.2 . . ? N1 C21 C20 123.4(5) . . ? N1 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N2 C22 C23 123.1(5) . . ? N2 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C22 C23 C24 117.8(6) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.7(5) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? N2 C26 C25 120.3(5) . . ? N2 C26 C27 119.1(4) . . ? C25 C26 C27 120.6(5) . . ? N3 C27 C26 113.3(4) . . ? N3 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? N3 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C29 C28 N3 107.1(4) . . ? C29 C28 H28 126.5 . . ? N3 C28 H28 126.5 . . ? C28 C29 N4 106.8(4) . . ? C28 C29 H29 126.6 . . ? N4 C29 H29 126.6 . . ? N3 C30 N4 104.9(4) . . ? N3 C30 Pd1 121.7(3) . . ? N4 C30 Pd1 133.3(3) . . ? N8 C31 C32 124.7(4) . . ? N8 C31 N4 116.9(4) . . ? C32 C31 N4 118.4(4) . . ? C33 C32 C31 118.1(5) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C32 C33 C34 119.9(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C42 C34 C33 117.8(5) . . ? C42 C34 C35 118.8(6) . . ? C33 C34 C35 123.3(6) . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 122.8(6) . . ? C35 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C38 C37 C41 117.0(6) . . ? C38 C37 C36 124.7(6) . . ? C41 C37 C36 118.4(6) . . ? C39 C38 C37 120.3(6) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.8(6) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? N7 C40 C39 121.9(6) . . ? N7 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N7 C41 C37 122.7(5) . . ? N7 C41 C42 118.1(4) . . ? C37 C41 C42 119.1(5) . . ? N8 C42 C34 122.7(5) . . ? N8 C42 C41 117.0(4) . . ? C34 C42 C41 120.3(4) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N13 C44 C43 178.6(8) . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N12 C46 C45 178.6(15) . . ? F3 P1 F5 96.1(5) . . ? F3 P1 F6 170.9(5) . . ? F5 P1 F6 91.6(5) . . ? F3 P1 F4 91.5(5) . . ? F5 P1 F4 89.1(4) . . ? F6 P1 F4 93.5(5) . . ? F3 P1 F1 88.7(4) . . ? F5 P1 F1 94.6(3) . . ? F6 P1 F1 85.9(4) . . ? F4 P1 F1 176.3(3) . . ? F3 P1 F2 85.7(4) . . ? F5 P1 F2 177.5(4) . . ? F6 P1 F2 86.7(4) . . ? F4 P1 F2 89.2(3) . . ? F1 P1 F2 87.2(2) . . ? F12 P2 F7 103.7(4) . . ? F12 P2 F8 89.2(3) . . ? F7 P2 F8 95.2(4) . . ? F12 P2 F11 96.7(3) . . ? F7 P2 F11 89.7(3) . . ? F8 P2 F11 171.2(4) . . ? F12 P2 F10 83.9(4) . . ? F7 P2 F10 172.3(4) . . ? F8 P2 F10 86.0(4) . . ? F11 P2 F10 88.2(4) . . ? F12 P2 F9 172.8(4) . . ? F7 P2 F9 83.4(3) . . ? F8 P2 F9 89.4(3) . . ? F11 P2 F9 84.0(3) . . ? F10 P2 F9 89.0(4) . . ? F17 P3 F15 91.3(3) . . ? F17 P3 F13 88.0(3) . . ? F15 P3 F13 91.1(2) . . ? F17 P3 F18 89.3(2) . . ? F15 P3 F18 178.7(2) . . ? F13 P3 F18 90.1(2) . . ? F17 P3 F16 92.5(3) . . ? F15 P3 F16 90.0(2) . . ? F13 P3 F16 178.8(3) . . ? F18 P3 F16 88.8(2) . . ? F17 P3 F14 179.2(3) . . ? F15 P3 F14 88.4(2) . . ? F13 P3 F14 91.4(2) . . ? F18 P3 F14 91.1(2) . . ? F16 P3 F14 88.1(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 C30 Pd1 N1 C21 174(3) . . . . ? C15 Pd1 N1 C21 134.6(4) . . . . ? N2 Pd1 N1 C21 -40.9(4) . . . . ? C30 Pd1 N1 C17 -4(3) . . . . ? C15 Pd1 N1 C17 -42.8(3) . . . . ? N2 Pd1 N1 C17 141.7(3) . . . . ? C30 Pd1 N2 C22 141.7(4) . . . . ? C15 Pd1 N2 C22 -140(2) . . . . ? N1 Pd1 N2 C22 -36.5(4) . . . . ? C30 Pd1 N2 C26 -42.4(3) . . . . ? C15 Pd1 N2 C26 36(2) . . . . ? N1 Pd1 N2 C26 139.4(3) . . . . ? N9 Cu1 N7 C40 43.6(5) . . . . ? N10 Cu1 N7 C40 -76.8(5) . . . . ? N8 Cu1 N7 C40 -174.8(5) . . . . ? N9 Cu1 N7 C41 -139.3(3) . . . . ? N10 Cu1 N7 C41 100.3(3) . . . . ? N8 Cu1 N7 C41 2.3(3) . . . . ? N7 Cu1 N8 C31 169.3(4) . . . . ? N9 Cu1 N8 C31 -50.5(5) . . . . ? N10 Cu1 N8 C31 38.9(4) . . . . ? N7 Cu1 N8 C42 -2.3(3) . . . . ? N9 Cu1 N8 C42 137.9(3) . . . . ? N10 Cu1 N8 C42 -132.7(3) . . . . ? N7 Cu1 N9 C1 40.5(6) . . . . ? N10 Cu1 N9 C1 179.5(5) . . . . ? N8 Cu1 N9 C1 -82.6(5) . . . . ? N7 Cu1 N9 C12 -141.7(3) . . . . ? N10 Cu1 N9 C12 -2.7(3) . . . . ? N8 Cu1 N9 C12 95.2(4) . . . . ? N7 Cu1 N10 C10 -50.9(5) . . . . ? N9 Cu1 N10 C10 170.5(4) . . . . ? N8 Cu1 N10 C10 38.4(4) . . . . ? N7 Cu1 N10 C11 143.0(3) . . . . ? N9 Cu1 N10 C11 4.3(3) . . . . ? N8 Cu1 N10 C11 -127.7(3) . . . . ? C12 N9 C1 C2 -0.6(9) . . . . ? Cu1 N9 C1 C2 177.1(5) . . . . ? N9 C1 C2 C3 -0.9(10) . . . . ? C1 C2 C3 C4 1.6(10) . . . . ? C2 C3 C4 C12 -0.7(8) . . . . ? C2 C3 C4 C5 -178.2(6) . . . . ? C12 C4 C5 C6 -3.2(8) . . . . ? C3 C4 C5 C6 174.3(6) . . . . ? C4 C5 C6 C7 3.1(8) . . . . ? C5 C6 C7 C11 0.6(8) . . . . ? C5 C6 C7 C8 -176.5(5) . . . . ? C11 C7 C8 C9 1.8(7) . . . . ? C6 C7 C8 C9 178.9(5) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C11 N10 C10 C9 -1.3(7) . . . . ? Cu1 N10 C10 C9 -166.8(3) . . . . ? C11 N10 C10 N5 176.1(4) . . . . ? Cu1 N10 C10 N5 10.7(6) . . . . ? C8 C9 C10 N10 0.0(7) . . . . ? C8 C9 C10 N5 -177.3(4) . . . . ? C15 N5 C10 N10 -121.5(4) . . . . ? C13 N5 C10 N10 61.7(6) . . . . ? C15 N5 C10 C9 56.1(6) . . . . ? C13 N5 C10 C9 -120.7(5) . . . . ? C10 N10 C11 C7 3.0(6) . . . . ? Cu1 N10 C11 C7 171.2(3) . . . . ? C10 N10 C11 C12 -173.5(4) . . . . ? Cu1 N10 C11 C12 -5.2(5) . . . . ? C8 C7 C11 N10 -3.2(7) . . . . ? C6 C7 C11 N10 179.5(4) . . . . ? C8 C7 C11 C12 173.0(4) . . . . ? C6 C7 C11 C12 -4.3(7) . . . . ? C1 N9 C12 C4 1.5(7) . . . . ? Cu1 N9 C12 C4 -176.6(4) . . . . ? C1 N9 C12 C11 178.7(5) . . . . ? Cu1 N9 C12 C11 0.7(5) . . . . ? C3 C4 C12 N9 -0.9(8) . . . . ? C5 C4 C12 N9 176.8(5) . . . . ? C3 C4 C12 C11 -178.1(5) . . . . ? C5 C4 C12 C11 -0.4(7) . . . . ? N10 C11 C12 N9 3.2(6) . . . . ? C7 C11 C12 N9 -173.3(4) . . . . ? N10 C11 C12 C4 -179.4(4) . . . . ? C7 C11 C12 C4 4.1(7) . . . . ? C15 N5 C13 C14 -0.2(5) . . . . ? C10 N5 C13 C14 177.0(4) . . . . ? N5 C13 C14 N6 -0.1(5) . . . . ? C15 N6 C14 C13 0.4(5) . . . . ? C16 N6 C14 C13 -173.2(4) . . . . ? C14 N6 C15 N5 -0.5(5) . . . . ? C16 N6 C15 N5 173.7(4) . . . . ? C14 N6 C15 Pd1 -178.5(3) . . . . ? C16 N6 C15 Pd1 -4.3(5) . . . . ? C13 N5 C15 N6 0.4(5) . . . . ? C10 N5 C15 N6 -177.0(3) . . . . ? C13 N5 C15 Pd1 178.1(3) . . . . ? C10 N5 C15 Pd1 0.8(6) . . . . ? C30 Pd1 C15 N6 -133.9(3) . . . . ? N2 Pd1 C15 N6 148.3(19) . . . . ? N1 Pd1 C15 N6 44.1(3) . . . . ? C30 Pd1 C15 N5 48.6(4) . . . . ? N2 Pd1 C15 N5 -29(2) . . . . ? N1 Pd1 C15 N5 -133.4(4) . . . . ? C15 N6 C16 C17 -54.9(5) . . . . ? C14 N6 C16 C17 118.0(5) . . . . ? C21 N1 C17 C18 3.4(7) . . . . ? Pd1 N1 C17 C18 -179.1(4) . . . . ? C21 N1 C17 C16 -175.8(4) . . . . ? Pd1 N1 C17 C16 1.7(5) . . . . ? N6 C16 C17 N1 54.0(5) . . . . ? N6 C16 C17 C18 -125.2(5) . . . . ? N1 C17 C18 C19 -1.8(8) . . . . ? C16 C17 C18 C19 177.4(5) . . . . ? C17 C18 C19 C20 -0.6(9) . . . . ? C18 C19 C20 C21 1.3(9) . . . . ? C17 N1 C21 C20 -2.8(7) . . . . ? Pd1 N1 C21 C20 179.7(4) . . . . ? C19 C20 C21 N1 0.5(8) . . . . ? C26 N2 C22 C23 -2.6(7) . . . . ? Pd1 N2 C22 C23 173.3(4) . . . . ? N2 C22 C23 C24 0.3(8) . . . . ? C22 C23 C24 C25 2.2(9) . . . . ? C23 C24 C25 C26 -2.4(9) . . . . ? C22 N2 C26 C25 2.3(7) . . . . ? Pd1 N2 C26 C25 -173.6(4) . . . . ? C22 N2 C26 C27 -178.9(4) . . . . ? Pd1 N2 C26 C27 5.2(5) . . . . ? C24 C25 C26 N2 0.2(8) . . . . ? C24 C25 C26 C27 -178.6(5) . . . . ? C30 N3 C27 C26 -50.5(6) . . . . ? C28 N3 C27 C26 128.6(5) . . . . ? N2 C26 C27 N3 47.8(6) . . . . ? C25 C26 C27 N3 -133.4(4) . . . . ? C30 N3 C28 C29 0.2(6) . . . . ? C27 N3 C28 C29 -179.0(4) . . . . ? N3 C28 C29 N4 0.7(5) . . . . ? C30 N4 C29 C28 -1.3(5) . . . . ? C31 N4 C29 C28 174.4(4) . . . . ? C28 N3 C30 N4 -0.9(5) . . . . ? C27 N3 C30 N4 178.3(4) . . . . ? C28 N3 C30 Pd1 176.6(3) . . . . ? C27 N3 C30 Pd1 -4.2(6) . . . . ? C29 N4 C30 N3 1.4(5) . . . . ? C31 N4 C30 N3 -174.6(4) . . . . ? C29 N4 C30 Pd1 -175.8(4) . . . . ? C31 N4 C30 Pd1 8.2(7) . . . . ? C15 Pd1 C30 N3 -133.8(4) . . . . ? N2 Pd1 C30 N3 41.7(4) . . . . ? N1 Pd1 C30 N3 -173(3) . . . . ? C15 Pd1 C30 N4 42.9(5) . . . . ? N2 Pd1 C30 N4 -141.5(4) . . . . ? N1 Pd1 C30 N4 4(3) . . . . ? C42 N8 C31 C32 -3.0(6) . . . . ? Cu1 N8 C31 C32 -174.2(3) . . . . ? C42 N8 C31 N4 174.3(3) . . . . ? Cu1 N8 C31 N4 3.2(6) . . . . ? C30 N4 C31 N8 -116.5(5) . . . . ? C29 N4 C31 N8 68.3(6) . . . . ? C30 N4 C31 C32 61.1(6) . . . . ? C29 N4 C31 C32 -114.2(5) . . . . ? N8 C31 C32 C33 -0.3(7) . . . . ? N4 C31 C32 C33 -177.6(4) . . . . ? C31 C32 C33 C34 1.7(8) . . . . ? C32 C33 C34 C42 0.2(8) . . . . ? C32 C33 C34 C35 176.0(5) . . . . ? C42 C34 C35 C36 3.1(10) . . . . ? C33 C34 C35 C36 -172.7(6) . . . . ? C34 C35 C36 C37 1.0(11) . . . . ? C35 C36 C37 C38 175.0(7) . . . . ? C35 C36 C37 C41 -4.7(10) . . . . ? C41 C37 C38 C39 1.0(9) . . . . ? C36 C37 C38 C39 -178.7(6) . . . . ? C37 C38 C39 C40 -2.3(10) . . . . ? C41 N7 C40 C39 -0.5(8) . . . . ? Cu1 N7 C40 C39 176.4(4) . . . . ? C38 C39 C40 N7 2.1(9) . . . . ? C40 N7 C41 C37 -0.9(7) . . . . ? Cu1 N7 C41 C37 -178.2(4) . . . . ? C40 N7 C41 C42 175.4(4) . . . . ? Cu1 N7 C41 C42 -1.9(5) . . . . ? C38 C37 C41 N7 0.6(8) . . . . ? C36 C37 C41 N7 -179.7(5) . . . . ? C38 C37 C41 C42 -175.6(5) . . . . ? C36 C37 C41 C42 4.1(7) . . . . ? C31 N8 C42 C34 5.0(6) . . . . ? Cu1 N8 C42 C34 178.2(4) . . . . ? C31 N8 C42 C41 -171.3(4) . . . . ? Cu1 N8 C42 C41 1.9(5) . . . . ? C33 C34 C42 N8 -3.7(7) . . . . ? C35 C34 C42 N8 -179.7(5) . . . . ? C33 C34 C42 C41 172.5(5) . . . . ? C35 C34 C42 C41 -3.5(7) . . . . ? N7 C41 C42 N8 -0.1(6) . . . . ? C37 C41 C42 N8 176.3(4) . . . . ? N7 C41 C42 C34 -176.5(4) . . . . ? C37 C41 C42 C34 -0.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.758 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.073 #===END data_080908d _database_code_depnum_ccdc_archive 'CCDC 792163' #TrackingRef '- hebing.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cl2 F12 N12 O P2 Pd2' _chemical_formula_weight 1348.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 8.3080(11) _cell_length_b 23.423(2) _cell_length_c 26.169(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.390(2) _cell_angle_gamma 90.00 _cell_volume 5050.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6787 _exptl_absorpt_correction_T_max 0.7582 _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 25279 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8870 _reflns_number_gt 6144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0908P)^2^+61.1247P] 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 8870 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2014 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Pd1 Pd 0.28551(9) 0.26676(3) 0.40972(3) 0.0316(2) Uani 1 1 d . . . Pd2 Pd -0.12773(10) 0.26094(3) 0.39488(3) 0.0445(3) Uani 1 1 d . . . Cl1 Cl -0.1243(4) 0.29414(13) 0.31334(12) 0.0607(8) Uani 1 1 d . . . Cl2 Cl -0.2516(5) 0.34286(14) 0.41344(14) 0.0733(10) Uani 1 1 d . . . F1 F 1.1172(17) 0.4203(6) 0.6130(5) 0.163(5) Uani 1 1 d . . . F2 F 0.8639(17) 0.3336(6) 0.6348(6) 0.157(5) Uani 1 1 d . . . F3 F 1.0037(19) 0.3508(6) 0.5690(5) 0.160(5) Uani 1 1 d . . . F4 F 0.8547(16) 0.4192(5) 0.5999(5) 0.138(4) Uani 1 1 d . . . F5 F 0.9810(15) 0.4014(5) 0.6772(4) 0.132(4) Uani 1 1 d . . . F6 F 1.1269(15) 0.3352(5) 0.6454(4) 0.135(5) Uani 1 1 d . . . F7 F 0.3773(13) 0.3726(5) 0.1136(4) 0.119(4) Uani 1 1 d . . . F8 F 0.1181(18) 0.4173(7) 0.1785(5) 0.168(6) Uani 1 1 d . . . F9 F 0.3827(16) 0.3885(6) 0.1950(4) 0.145(5) Uani 1 1 d . . . F10 F 0.1929(19) 0.3315(6) 0.1501(6) 0.169(6) Uani 1 1 d . . . F11 F 0.1262(15) 0.4016(6) 0.0983(4) 0.141(4) Uani 1 1 d . . . F12 F 0.3009(17) 0.4550(5) 0.1427(6) 0.166(5) Uani 1 1 d . . . N1 N 0.1248(10) 0.1963(3) 0.3176(3) 0.0355(18) Uani 1 1 d . . . N2 N 0.2726(10) 0.2659(3) 0.2996(3) 0.0364(18) Uani 1 1 d . . . N3 N -0.0367(9) 0.1791(3) 0.3824(3) 0.0335(17) Uani 1 1 d . . . N4 N -0.1679(10) 0.2220(3) 0.4627(3) 0.0383(19) Uani 1 1 d . . . N5 N 0.2385(10) 0.3488(3) 0.3798(3) 0.041(2) Uani 1 1 d . . . N6 N 0.3863(10) 0.1401(3) 0.4160(3) 0.0355(18) Uani 1 1 d . . . N7 N 0.2895(10) 0.1731(4) 0.4822(3) 0.0394(19) Uani 1 1 d . . . N8 N 0.4014(10) 0.0876(3) 0.3423(3) 0.0379(19) Uani 1 1 d . . . N9 N 0.2883(12) -0.0051(4) 0.2857(4) 0.052(2) Uani 1 1 d . . . N10 N 0.3594(10) 0.2958(3) 0.4854(3) 0.0385(19) Uani 1 1 d . . . N11 N 0.560(3) 0.2471(10) 0.6960(9) 0.149(8) Uani 1 1 d . . . N12 N 0.504(4) 0.9763(13) 0.0631(12) 0.208(13) Uani 1 1 d . . . O1 O 0.3573(17) 0.9669(4) 0.3983(4) 0.107(4) Uani 1 1 d . . . H1C H 0.3304 0.9774 0.3673 0.128 Uiso 1 1 d R . . H1D H 0.4295 0.9411 0.3985 0.128 Uiso 1 1 d R . . P1 P 0.9927(5) 0.37555(17) 0.62126(16) 0.0742(10) Uani 1 1 d . . . P2 P 0.2427(6) 0.39297(18) 0.14826(14) 0.0803(12) Uani 1 1 d . . . C1 C 0.2158(11) 0.2398(4) 0.3380(3) 0.034(2) Uani 1 1 d . . . C2 C 0.2161(13) 0.2389(5) 0.2533(4) 0.046(3) Uani 1 1 d . . . H2 H 0.2382 0.2496 0.2207 0.055 Uiso 1 1 calc R . . C3 C 0.1256(13) 0.1954(5) 0.2642(4) 0.043(2) Uani 1 1 d . . . H3 H 0.0729 0.1694 0.2409 0.052 Uiso 1 1 calc R . . C4 C 0.0372(12) 0.1573(4) 0.3453(4) 0.038(2) Uani 1 1 d . . . C5 C 0.0357(13) 0.0994(4) 0.3337(4) 0.044(2) Uani 1 1 d . . . H5 H 0.0780 0.0865 0.3046 0.052 Uiso 1 1 calc R . . C6 C -0.0270(13) 0.0620(4) 0.3649(4) 0.048(3) Uani 1 1 d . . . H6 H -0.0288 0.0232 0.3573 0.058 Uiso 1 1 calc R . . C7 C -0.0895(13) 0.0819(4) 0.4087(4) 0.047(3) Uani 1 1 d . . . C8 C -0.0963(12) 0.1411(4) 0.4158(4) 0.039(2) Uani 1 1 d . . . C9 C -0.1589(12) 0.1646(4) 0.4591(4) 0.039(2) Uani 1 1 d . . . C10 C -0.2072(14) 0.1278(5) 0.4971(4) 0.051(3) Uani 1 1 d . . . C11 C -0.2592(16) 0.1547(6) 0.5405(5) 0.061(3) Uani 1 1 d . . . H11 H -0.2905 0.1325 0.5670 0.074 Uiso 1 1 calc R . . C12 C -0.2641(16) 0.2134(6) 0.5440(5) 0.063(3) Uani 1 1 d . . . H12 H -0.2951 0.2312 0.5730 0.076 Uiso 1 1 calc R . . C13 C -0.2215(14) 0.2453(5) 0.5030(4) 0.052(3) Uani 1 1 d . . . H13 H -0.2313 0.2849 0.5041 0.063 Uiso 1 1 calc R . . C14 C -0.1446(15) 0.0463(5) 0.4484(5) 0.057(3) Uani 1 1 d . . . H14 H -0.1431 0.0068 0.4446 0.069 Uiso 1 1 calc R . . C15 C -0.1972(15) 0.0683(5) 0.4901(5) 0.059(3) Uani 1 1 d . . . H15 H -0.2281 0.0440 0.5151 0.070 Uiso 1 1 calc R . . C16 C 0.3692(13) 0.3183(4) 0.3061(4) 0.042(2) Uani 1 1 d . . . H16A H 0.3899 0.3322 0.2727 0.051 Uiso 1 1 calc R . . H16B H 0.4727 0.3103 0.3264 0.051 Uiso 1 1 calc R . . C17 C 0.2804(12) 0.3632(4) 0.3326(4) 0.041(2) Uani 1 1 d . . . C18 C 0.2403(14) 0.4148(5) 0.3115(4) 0.052(3) Uani 1 1 d . . . H18 H 0.2721 0.4244 0.2798 0.062 Uiso 1 1 calc R . . C19 C 0.1528(16) 0.4532(5) 0.3366(5) 0.059(3) Uani 1 1 d . . . H19 H 0.1230 0.4884 0.3217 0.071 Uiso 1 1 calc R . . C20 C 0.1106(16) 0.4387(5) 0.3836(5) 0.061(3) Uani 1 1 d . . . H20 H 0.0540 0.4645 0.4017 0.073 Uiso 1 1 calc R . . C21 C 0.1519(13) 0.3865(4) 0.4038(4) 0.047(3) Uani 1 1 d . . . H21 H 0.1192 0.3764 0.4353 0.056 Uiso 1 1 calc R . . C22 C 0.3290(11) 0.1887(4) 0.4354(3) 0.034(2) Uani 1 1 d . . . C23 C 0.3752(13) 0.0947(4) 0.4493(4) 0.045(3) Uani 1 1 d . . . H23 H 0.4027 0.0569 0.4438 0.054 Uiso 1 1 calc R . . C24 C 0.3180(13) 0.1153(4) 0.4903(4) 0.046(3) Uani 1 1 d . . . H24 H 0.3001 0.0948 0.5194 0.055 Uiso 1 1 calc R . . C25 C 0.4485(12) 0.1346(4) 0.3676(4) 0.035(2) Uani 1 1 d . . . C26 C 0.5456(12) 0.1760(4) 0.3505(4) 0.040(2) Uani 1 1 d . . . H26 H 0.5731 0.2088 0.3696 0.048 Uiso 1 1 calc R . . C27 C 0.6005(12) 0.1667(4) 0.3035(4) 0.043(2) Uani 1 1 d . . . H27 H 0.6684 0.1934 0.2910 0.051 Uiso 1 1 calc R . . C28 C 0.5562(12) 0.1184(4) 0.2749(4) 0.041(2) Uani 1 1 d . . . C29 C 0.4524(12) 0.0792(4) 0.2961(4) 0.038(2) Uani 1 1 d . . . C30 C 0.3945(13) 0.0304(4) 0.2663(4) 0.043(2) Uani 1 1 d . . . C31 C 0.4445(14) 0.0219(5) 0.2170(4) 0.052(3) Uani 1 1 d . . . C32 C 0.3805(16) -0.0257(5) 0.1883(5) 0.058(3) Uani 1 1 d . . . H32 H 0.4110 -0.0332 0.1560 0.070 Uiso 1 1 calc R . . C33 C 0.2744(17) -0.0603(6) 0.2083(5) 0.066(4) Uani 1 1 d . . . H33 H 0.2312 -0.0919 0.1898 0.080 Uiso 1 1 calc R . . C34 C 0.2298(17) -0.0482(5) 0.2571(5) 0.066(3) Uani 1 1 d . . . H34 H 0.1548 -0.0720 0.2698 0.079 Uiso 1 1 calc R . . C35 C 0.6099(14) 0.1064(5) 0.2258(4) 0.051(3) Uani 1 1 d . . . H35 H 0.6829 0.1309 0.2129 0.061 Uiso 1 1 calc R . . C36 C 0.5567(15) 0.0609(5) 0.1990(5) 0.055(3) Uani 1 1 d . . . H36 H 0.5933 0.0541 0.1675 0.066 Uiso 1 1 calc R . . C37 C 0.2211(13) 0.2131(5) 0.5165(4) 0.044(2) Uani 1 1 d . . . H37A H 0.2135 0.1946 0.5492 0.053 Uiso 1 1 calc R . . H37B H 0.1123 0.2237 0.5015 0.053 Uiso 1 1 calc R . . C38 C 0.3230(12) 0.2662(4) 0.5256(4) 0.037(2) Uani 1 1 d . . . C39 C 0.3744(14) 0.2835(5) 0.5755(4) 0.053(3) Uani 1 1 d . . . H39 H 0.3498 0.2620 0.6033 0.063 Uiso 1 1 calc R . . C40 C 0.4631(16) 0.3334(6) 0.5834(5) 0.062(3) Uani 1 1 d . . . H40 H 0.4969 0.3462 0.6167 0.075 Uiso 1 1 calc R . . C41 C 0.5011(15) 0.3640(5) 0.5418(5) 0.058(3) Uani 1 1 d . . . H41 H 0.5608 0.3977 0.5461 0.070 Uiso 1 1 calc R . . C42 C 0.4477(13) 0.3432(4) 0.4935(4) 0.045(2) Uani 1 1 d . . . H42 H 0.4746 0.3631 0.4651 0.054 Uiso 1 1 calc R . . C43 C 0.675(3) 0.2224(10) 0.6886(9) 0.123(7) Uani 1 1 d . . . C44 C 0.828(3) 0.1937(11) 0.6803(9) 0.149(9) Uani 1 1 d . . . H44A H 0.8870 0.2173 0.6590 0.223 Uiso 1 1 calc R . . H44B H 0.8045 0.1577 0.6637 0.223 Uiso 1 1 calc R . . H44C H 0.8934 0.1876 0.7130 0.223 Uiso 1 1 calc R . . C45 C 0.374(5) 0.9857(14) 0.0424(15) 0.187(14) Uani 1 1 d . . . C46 C 0.203(4) 0.9917(13) 0.0173(11) 0.179(12) Uani 1 1 d . . . H46A H 0.2023 1.0032 -0.0179 0.269 Uiso 1 1 calc R . . H46B H 0.1482 1.0200 0.0353 0.269 Uiso 1 1 calc R . . H46C H 0.1479 0.9558 0.0185 0.269 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 Pd1 0.0369(4) 0.0334(4) 0.0240(4) -0.0021(3) 0.0010(3) -0.0052(3) Pd2 0.0454(5) 0.0396(5) 0.0485(5) 0.0006(4) 0.0063(4) -0.0008(4) Cl1 0.071(2) 0.0545(17) 0.0562(17) 0.0105(14) 0.0062(15) 0.0070(15) Cl2 0.086(2) 0.0533(18) 0.087(2) 0.0077(16) 0.036(2) 0.0174(17) F1 0.161(12) 0.168(12) 0.163(12) 0.030(10) 0.033(10) -0.064(10) F2 0.148(11) 0.127(10) 0.200(14) 0.010(9) 0.038(10) -0.018(9) F3 0.200(14) 0.176(12) 0.097(8) -0.032(8) -0.010(8) 0.029(11) F4 0.144(10) 0.118(9) 0.138(10) 0.009(7) -0.032(8) 0.039(8) F5 0.152(10) 0.156(10) 0.094(7) 0.009(7) 0.032(7) 0.064(8) F6 0.144(10) 0.172(11) 0.094(7) 0.022(7) 0.029(7) 0.096(9) F7 0.120(8) 0.154(10) 0.083(6) -0.019(6) 0.016(6) 0.009(7) F8 0.169(12) 0.212(15) 0.135(10) -0.031(10) 0.070(9) 0.040(11) F9 0.157(11) 0.191(13) 0.083(7) 0.008(8) 0.001(7) 0.038(10) F10 0.190(14) 0.116(9) 0.209(15) 0.046(10) 0.059(12) -0.011(9) F11 0.139(10) 0.166(11) 0.108(8) -0.013(8) -0.017(7) 0.018(9) F12 0.150(12) 0.111(9) 0.224(15) 0.004(10) -0.027(11) 0.006(8) N1 0.039(5) 0.034(4) 0.032(4) -0.006(3) 0.001(3) -0.004(4) N2 0.043(5) 0.039(4) 0.027(4) 0.000(3) 0.006(3) -0.006(4) N3 0.033(4) 0.030(4) 0.038(4) 0.002(3) 0.003(3) -0.006(3) N4 0.041(5) 0.039(5) 0.037(4) 0.002(4) 0.012(4) 0.000(4) N5 0.046(5) 0.035(4) 0.041(5) 0.001(4) 0.004(4) -0.006(4) N6 0.039(5) 0.033(4) 0.033(4) 0.000(3) 0.001(3) -0.003(3) N7 0.045(5) 0.045(5) 0.028(4) 0.001(4) 0.005(4) -0.006(4) N8 0.043(5) 0.036(4) 0.035(4) 0.003(4) 0.004(4) -0.001(4) N9 0.060(6) 0.042(5) 0.057(6) -0.011(4) 0.019(5) -0.006(4) N10 0.035(5) 0.043(5) 0.036(4) -0.009(4) 0.000(4) 0.002(4) N11 0.135(18) 0.161(19) 0.143(18) 0.003(14) -0.009(14) 0.030(15) N12 0.21(3) 0.18(2) 0.22(3) -0.02(2) -0.04(2) 0.05(2) O1 0.186(13) 0.062(6) 0.080(7) 0.022(5) 0.047(8) 0.019(7) P1 0.071(2) 0.072(2) 0.079(3) 0.014(2) 0.009(2) 0.005(2) P2 0.124(4) 0.070(2) 0.046(2) 0.0032(17) 0.012(2) 0.009(2) C1 0.037(5) 0.032(5) 0.032(5) 0.000(4) 0.003(4) 0.001(4) C2 0.054(7) 0.053(6) 0.030(5) -0.006(5) 0.005(5) 0.001(5) C3 0.049(6) 0.050(6) 0.029(5) -0.015(5) 0.001(4) 0.001(5) C4 0.037(5) 0.040(5) 0.036(5) -0.007(4) -0.001(4) -0.004(4) C5 0.043(6) 0.041(6) 0.046(6) -0.008(5) 0.006(5) -0.001(5) C6 0.048(7) 0.034(5) 0.062(7) -0.007(5) 0.004(5) -0.002(5) C7 0.046(6) 0.038(6) 0.056(7) 0.002(5) 0.006(5) -0.002(5) C8 0.038(6) 0.036(5) 0.041(6) 0.003(4) 0.000(4) -0.001(4) C9 0.039(6) 0.040(6) 0.040(6) 0.004(4) 0.012(4) -0.003(4) C10 0.050(7) 0.053(7) 0.050(7) 0.010(5) 0.008(5) -0.001(5) C11 0.064(8) 0.068(8) 0.056(7) 0.013(6) 0.018(6) 0.000(6) C12 0.065(8) 0.071(9) 0.057(8) 0.001(6) 0.019(6) 0.013(7) C13 0.053(7) 0.054(7) 0.050(7) 0.004(5) 0.008(5) 0.007(5) C14 0.060(8) 0.042(6) 0.069(8) 0.007(6) 0.007(6) -0.008(5) C15 0.060(8) 0.053(7) 0.064(8) 0.016(6) 0.012(6) -0.008(6) C16 0.046(6) 0.043(6) 0.038(5) 0.002(4) 0.008(5) -0.008(5) C17 0.042(6) 0.041(6) 0.040(6) 0.003(4) -0.002(5) -0.012(4) C18 0.062(8) 0.047(6) 0.046(6) 0.009(5) 0.003(5) -0.010(6) C19 0.067(8) 0.045(7) 0.064(8) 0.007(6) -0.001(6) -0.003(6) C20 0.069(8) 0.043(7) 0.069(8) -0.001(6) 0.005(7) 0.003(6) C21 0.049(6) 0.044(6) 0.048(6) -0.001(5) 0.005(5) -0.003(5) C22 0.035(5) 0.037(5) 0.029(5) -0.002(4) -0.004(4) 0.001(4) C23 0.055(7) 0.038(5) 0.040(6) 0.005(5) 0.000(5) -0.004(5) C24 0.053(7) 0.044(6) 0.039(6) 0.008(5) 0.001(5) -0.006(5) C25 0.039(5) 0.034(5) 0.032(5) 0.000(4) 0.001(4) -0.002(4) C26 0.041(6) 0.036(5) 0.042(6) -0.004(4) -0.002(5) -0.006(4) C27 0.040(6) 0.043(6) 0.045(6) 0.006(5) 0.007(5) -0.007(5) C28 0.040(6) 0.042(6) 0.041(6) 0.001(4) 0.007(5) 0.003(5) C29 0.038(6) 0.037(5) 0.039(5) -0.002(4) 0.007(4) 0.004(4) C30 0.048(6) 0.040(6) 0.043(6) -0.004(5) 0.010(5) 0.006(5) C31 0.056(7) 0.050(6) 0.050(7) -0.006(5) 0.006(5) 0.008(5) C32 0.068(8) 0.054(7) 0.053(7) -0.017(6) 0.007(6) 0.011(6) C33 0.071(9) 0.057(8) 0.069(9) -0.020(7) 0.003(7) 0.003(7) C34 0.076(9) 0.055(7) 0.068(8) -0.012(6) 0.012(7) -0.011(7) C35 0.054(7) 0.052(7) 0.050(7) 0.002(5) 0.017(5) 0.003(5) C36 0.065(8) 0.053(7) 0.048(7) -0.004(5) 0.010(6) 0.009(6) C37 0.049(6) 0.052(6) 0.033(5) -0.003(5) 0.010(5) -0.008(5) C38 0.038(5) 0.044(6) 0.030(5) -0.008(4) 0.001(4) 0.003(4) C39 0.060(7) 0.061(7) 0.036(6) -0.013(5) 0.002(5) -0.003(6) C40 0.067(8) 0.072(8) 0.045(7) -0.020(6) -0.004(6) 0.002(7) C41 0.063(8) 0.058(7) 0.052(7) -0.023(6) -0.001(6) -0.009(6) C42 0.044(6) 0.047(6) 0.042(6) -0.009(5) 0.001(5) -0.007(5) C43 0.13(2) 0.118(17) 0.112(17) -0.011(13) -0.006(15) 0.019(15) C44 0.16(2) 0.16(2) 0.122(18) -0.022(16) -0.010(16) 0.037(19) C45 0.20(4) 0.14(2) 0.21(4) -0.01(2) -0.02(3) 0.03(3) C46 0.18(3) 0.19(3) 0.17(3) 0.00(2) 0.00(2) 0.05(2) _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 Pd1 C22 1.966(9) . ? Pd1 C1 1.993(9) . ? Pd1 N5 2.094(8) . ? Pd1 N10 2.109(8) . ? Pd2 N4 2.060(8) . ? Pd2 N3 2.102(8) . ? Pd2 Cl2 2.260(3) . ? Pd2 Cl1 2.275(3) . ? F1 P1 1.507(12) . ? F2 P1 1.528(13) . ? F3 P1 1.498(12) . ? F4 P1 1.583(11) . ? F5 P1 1.599(11) . ? F6 P1 1.534(10) . ? F7 P2 1.601(11) . ? F8 P2 1.495(12) . ? F9 P2 1.580(12) . ? F10 P2 1.501(13) . ? F11 P2 1.537(11) . ? F12 P2 1.543(14) . ? N1 C1 1.339(12) . ? N1 C3 1.400(12) . ? N1 C4 1.423(12) . ? N2 C1 1.315(12) . ? N2 C2 1.393(12) . ? N2 C16 1.464(12) . ? N3 C4 1.315(12) . ? N3 C8 1.384(12) . ? N4 C13 1.316(14) . ? N4 C9 1.351(12) . ? N5 C21 1.345(13) . ? N5 C17 1.367(13) . ? N6 C22 1.357(12) . ? N6 C23 1.386(12) . ? N6 C25 1.435(12) . ? N7 C22 1.356(12) . ? N7 C24 1.386(13) . ? N7 C37 1.463(13) . ? N8 C25 1.319(12) . ? N8 C29 1.346(12) . ? N9 C34 1.312(15) . ? N9 C30 1.356(13) . ? N10 C38 1.328(13) . ? N10 C42 1.332(13) . ? N11 C43 1.15(3) . ? N12 C45 1.16(4) . ? C2 C3 1.318(15) . ? C4 C5 1.391(14) . ? C5 C6 1.345(15) . ? C6 C7 1.398(15) . ? C7 C8 1.400(14) . ? C7 C14 1.452(15) . ? C8 C9 1.417(14) . ? C9 C10 1.413(14) . ? C10 C15 1.409(16) . ? C10 C11 1.413(16) . ? C11 C12 1.379(18) . ? C12 C13 1.390(17) . ? C14 C15 1.331(17) . ? C16 C17 1.504(14) . ? C17 C18 1.352(15) . ? C18 C19 1.374(17) . ? C19 C20 1.366(17) . ? C20 C21 1.360(16) . ? C23 C24 1.320(15) . ? C25 C26 1.372(13) . ? C26 C27 1.383(14) . ? C27 C28 1.381(14) . ? C28 C29 1.421(14) . ? C28 C35 1.441(14) . ? C29 C30 1.432(14) . ? C30 C31 1.420(15) . ? C31 C32 1.409(16) . ? C31 C36 1.428(17) . ? C32 C33 1.351(18) . ? C33 C34 1.404(17) . ? C35 C36 1.319(16) . ? C37 C38 1.505(14) . ? C38 C39 1.382(14) . ? C39 C40 1.383(17) . ? C40 C41 1.374(18) . ? C41 C42 1.372(14) . ? C43 C44 1.48(3) . ? C45 C46 1.50(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Pd1 C1 92.7(4) . . ? C22 Pd1 N5 178.0(3) . . ? C1 Pd1 N5 85.4(3) . . ? C22 Pd1 N10 87.7(3) . . ? C1 Pd1 N10 179.6(3) . . ? N5 Pd1 N10 94.2(3) . . ? N4 Pd2 N3 80.3(3) . . ? N4 Pd2 Cl2 93.6(2) . . ? N3 Pd2 Cl2 172.3(2) . . ? N4 Pd2 Cl1 169.2(3) . . ? N3 Pd2 Cl1 96.7(2) . . ? Cl2 Pd2 Cl1 88.41(12) . . ? C1 N1 C3 109.5(8) . . ? C1 N1 C4 125.8(8) . . ? C3 N1 C4 124.6(8) . . ? C1 N2 C2 109.9(8) . . ? C1 N2 C16 123.1(8) . . ? C2 N2 C16 126.9(8) . . ? C4 N3 C8 117.1(8) . . ? C4 N3 Pd2 132.8(6) . . ? C8 N3 Pd2 108.9(6) . . ? C13 N4 C9 119.8(9) . . ? C13 N4 Pd2 128.0(7) . . ? C9 N4 Pd2 111.4(6) . . ? C21 N5 C17 118.3(9) . . ? C21 N5 Pd1 120.8(7) . . ? C17 N5 Pd1 120.5(7) . . ? C22 N6 C23 110.7(8) . . ? C22 N6 C25 126.2(8) . . ? C23 N6 C25 123.1(8) . . ? C22 N7 C24 110.2(8) . . ? C22 N7 C37 122.7(8) . . ? C24 N7 C37 127.1(8) . . ? C25 N8 C29 117.7(8) . . ? C34 N9 C30 117.9(10) . . ? C38 N10 C42 119.0(9) . . ? C38 N10 Pd1 120.5(6) . . ? C42 N10 Pd1 120.5(7) . . ? F3 P1 F1 90.9(9) . . ? F3 P1 F2 95.1(9) . . ? F1 P1 F2 173.9(9) . . ? F3 P1 F6 90.6(7) . . ? F1 P1 F6 90.6(8) . . ? F2 P1 F6 90.1(8) . . ? F3 P1 F4 93.1(7) . . ? F1 P1 F4 88.9(8) . . ? F2 P1 F4 90.0(8) . . ? F6 P1 F4 176.2(7) . . ? F3 P1 F5 179.5(8) . . ? F1 P1 F5 89.5(8) . . ? F2 P1 F5 84.5(8) . . ? F6 P1 F5 89.0(6) . . ? F4 P1 F5 87.3(6) . . ? F8 P2 F10 97.8(9) . . ? F8 P2 F11 89.8(8) . . ? F10 P2 F11 90.4(9) . . ? F8 P2 F12 86.4(9) . . ? F10 P2 F12 175.5(9) . . ? F11 P2 F12 88.1(8) . . ? F8 P2 F9 96.1(8) . . ? F10 P2 F9 95.2(8) . . ? F11 P2 F9 171.2(8) . . ? F12 P2 F9 85.8(8) . . ? F8 P2 F7 174.7(8) . . ? F10 P2 F7 87.0(7) . . ? F11 P2 F7 88.1(6) . . ? F12 P2 F7 88.6(8) . . ? F9 P2 F7 85.5(6) . . ? N2 C1 N1 106.8(8) . . ? N2 C1 Pd1 118.9(7) . . ? N1 C1 Pd1 134.2(7) . . ? C3 C2 N2 107.6(9) . . ? C2 C3 N1 106.2(9) . . ? N3 C4 C5 123.2(9) . . ? N3 C4 N1 116.4(8) . . ? C5 C4 N1 120.4(9) . . ? C6 C5 C4 119.7(10) . . ? C5 C6 C7 119.6(10) . . ? C6 C7 C8 117.6(10) . . ? C6 C7 C14 125.4(10) . . ? C8 C7 C14 116.9(10) . . ? N3 C8 C7 122.0(9) . . ? N3 C8 C9 116.9(8) . . ? C7 C8 C9 121.1(9) . . ? N4 C9 C10 122.4(9) . . ? N4 C9 C8 118.1(8) . . ? C10 C9 C8 119.5(9) . . ? C15 C10 C11 125.1(11) . . ? C15 C10 C9 118.9(10) . . ? C11 C10 C9 115.9(10) . . ? C12 C11 C10 120.8(11) . . ? C11 C12 C13 118.2(12) . . ? N4 C13 C12 122.8(11) . . ? C15 C14 C7 122.0(11) . . ? C14 C15 C10 121.5(11) . . ? N2 C16 C17 110.2(8) . . ? C18 C17 N5 120.7(10) . . ? C18 C17 C16 123.2(10) . . ? N5 C17 C16 116.1(9) . . ? C17 C18 C19 120.6(11) . . ? C20 C19 C18 118.7(11) . . ? C21 C20 C19 119.5(12) . . ? N5 C21 C20 122.1(11) . . ? N7 C22 N6 104.5(8) . . ? N7 C22 Pd1 120.3(7) . . ? N6 C22 Pd1 135.2(7) . . ? C24 C23 N6 106.8(9) . . ? C23 C24 N7 107.8(9) . . ? N8 C25 C26 125.2(9) . . ? N8 C25 N6 113.6(8) . . ? C26 C25 N6 121.2(8) . . ? C25 C26 C27 117.0(9) . . ? C28 C27 C26 121.0(9) . . ? C27 C28 C29 116.8(9) . . ? C27 C28 C35 123.5(10) . . ? C29 C28 C35 119.7(9) . . ? N8 C29 C28 122.3(9) . . ? N8 C29 C30 118.9(9) . . ? C28 C29 C30 118.8(9) . . ? N9 C30 C31 122.3(10) . . ? N9 C30 C29 118.3(9) . . ? C31 C30 C29 119.3(10) . . ? C32 C31 C30 117.4(11) . . ? C32 C31 C36 123.3(11) . . ? C30 C31 C36 119.3(10) . . ? C33 C32 C31 119.3(11) . . ? C32 C33 C34 119.4(12) . . ? N9 C34 C33 123.6(13) . . ? C36 C35 C28 120.7(11) . . ? C35 C36 C31 122.0(11) . . ? N7 C37 C38 111.8(8) . . ? N10 C38 C39 121.5(10) . . ? N10 C38 C37 119.2(8) . . ? C39 C38 C37 119.4(9) . . ? C38 C39 C40 118.9(11) . . ? C41 C40 C39 119.7(11) . . ? C42 C41 C40 117.5(11) . . ? N10 C42 C41 123.4(11) . . ? N11 C43 C44 177(3) . . ? N12 C45 C46 174(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Pd2 N3 C4 -175.1(9) . . . . ? Cl2 Pd2 N3 C4 147.2(15) . . . . ? Cl1 Pd2 N3 C4 15.4(9) . . . . ? N4 Pd2 N3 C8 18.3(6) . . . . ? Cl2 Pd2 N3 C8 -19(2) . . . . ? Cl1 Pd2 N3 C8 -151.2(6) . . . . ? N3 Pd2 N4 C13 174.5(10) . . . . ? Cl2 Pd2 N4 C13 -10.2(9) . . . . ? Cl1 Pd2 N4 C13 -110.5(14) . . . . ? N3 Pd2 N4 C9 -16.2(7) . . . . ? Cl2 Pd2 N4 C9 159.1(7) . . . . ? Cl1 Pd2 N4 C9 58.8(16) . . . . ? C22 Pd1 N5 C21 144(10) . . . . ? C1 Pd1 N5 C21 132.7(8) . . . . ? N10 Pd1 N5 C21 -47.4(8) . . . . ? C22 Pd1 N5 C17 -29(11) . . . . ? C1 Pd1 N5 C17 -40.4(8) . . . . ? N10 Pd1 N5 C17 139.5(7) . . . . ? C22 Pd1 N10 C38 -37.1(8) . . . . ? C1 Pd1 N10 C38 159(64) . . . . ? N5 Pd1 N10 C38 143.3(7) . . . . ? C22 Pd1 N10 C42 140.7(8) . . . . ? C1 Pd1 N10 C42 -24(51) . . . . ? N5 Pd1 N10 C42 -38.9(8) . . . . ? C2 N2 C1 N1 0.5(11) . . . . ? C16 N2 C1 N1 175.8(9) . . . . ? C2 N2 C1 Pd1 177.0(7) . . . . ? C16 N2 C1 Pd1 -7.7(12) . . . . ? C3 N1 C1 N2 0.1(11) . . . . ? C4 N1 C1 N2 -178.6(9) . . . . ? C3 N1 C1 Pd1 -175.7(8) . . . . ? C4 N1 C1 Pd1 5.6(15) . . . . ? C22 Pd1 C1 N2 -133.6(8) . . . . ? N5 Pd1 C1 N2 46.0(8) . . . . ? N10 Pd1 C1 N2 31(51) . . . . ? C22 Pd1 C1 N1 41.7(10) . . . . ? N5 Pd1 C1 N1 -138.7(10) . . . . ? N10 Pd1 C1 N1 -154(64) . . . . ? C1 N2 C2 C3 -0.8(12) . . . . ? C16 N2 C2 C3 -175.9(10) . . . . ? N2 C2 C3 N1 0.8(12) . . . . ? C1 N1 C3 C2 -0.6(11) . . . . ? C4 N1 C3 C2 178.1(9) . . . . ? C8 N3 C4 C5 10.1(14) . . . . ? Pd2 N3 C4 C5 -155.6(8) . . . . ? C8 N3 C4 N1 -168.2(8) . . . . ? Pd2 N3 C4 N1 26.0(13) . . . . ? C1 N1 C4 N3 40.0(13) . . . . ? C3 N1 C4 N3 -138.5(9) . . . . ? C1 N1 C4 C5 -138.4(10) . . . . ? C3 N1 C4 C5 43.1(14) . . . . ? N3 C4 C5 C6 -8.0(16) . . . . ? N1 C4 C5 C6 170.3(9) . . . . ? C4 C5 C6 C7 -0.3(16) . . . . ? C5 C6 C7 C8 5.4(16) . . . . ? C5 C6 C7 C14 -173.0(11) . . . . ? C4 N3 C8 C7 -4.5(14) . . . . ? Pd2 N3 C8 C7 164.5(8) . . . . ? C4 N3 C8 C9 172.9(9) . . . . ? Pd2 N3 C8 C9 -18.1(10) . . . . ? C6 C7 C8 N3 -3.1(16) . . . . ? C14 C7 C8 N3 175.5(9) . . . . ? C6 C7 C8 C9 179.6(10) . . . . ? C14 C7 C8 C9 -1.9(16) . . . . ? C13 N4 C9 C10 0.7(16) . . . . ? Pd2 N4 C9 C10 -169.6(8) . . . . ? C13 N4 C9 C8 -178.3(10) . . . . ? Pd2 N4 C9 C8 11.4(12) . . . . ? N3 C8 C9 N4 5.0(14) . . . . ? C7 C8 C9 N4 -177.5(10) . . . . ? N3 C8 C9 C10 -174.0(9) . . . . ? C7 C8 C9 C10 3.4(15) . . . . ? N4 C9 C10 C15 178.7(11) . . . . ? C8 C9 C10 C15 -2.3(16) . . . . ? N4 C9 C10 C11 -2.6(16) . . . . ? C8 C9 C10 C11 176.4(10) . . . . ? C15 C10 C11 C12 179.7(13) . . . . ? C9 C10 C11 C12 1.1(18) . . . . ? C10 C11 C12 C13 2(2) . . . . ? C9 N4 C13 C12 2.8(17) . . . . ? Pd2 N4 C13 C12 171.3(9) . . . . ? C11 C12 C13 N4 -4.1(19) . . . . ? C6 C7 C14 C15 177.5(12) . . . . ? C8 C7 C14 C15 -0.9(18) . . . . ? C7 C14 C15 C10 2(2) . . . . ? C11 C10 C15 C14 -179.0(12) . . . . ? C9 C10 C15 C14 -0.4(19) . . . . ? C1 N2 C16 C17 -54.0(12) . . . . ? C2 N2 C16 C17 120.5(10) . . . . ? C21 N5 C17 C18 2.2(15) . . . . ? Pd1 N5 C17 C18 175.4(8) . . . . ? C21 N5 C17 C16 -176.7(9) . . . . ? Pd1 N5 C17 C16 -3.5(12) . . . . ? N2 C16 C17 C18 -121.4(11) . . . . ? N2 C16 C17 N5 57.4(11) . . . . ? N5 C17 C18 C19 -1.7(17) . . . . ? C16 C17 C18 C19 177.1(10) . . . . ? C17 C18 C19 C20 1.5(18) . . . . ? C18 C19 C20 C21 -1.8(19) . . . . ? C17 N5 C21 C20 -2.5(16) . . . . ? Pd1 N5 C21 C20 -175.7(9) . . . . ? C19 C20 C21 N5 2.3(18) . . . . ? C24 N7 C22 N6 -1.8(11) . . . . ? C37 N7 C22 N6 -179.6(8) . . . . ? C24 N7 C22 Pd1 174.9(7) . . . . ? C37 N7 C22 Pd1 -2.9(12) . . . . ? C23 N6 C22 N7 2.8(10) . . . . ? C25 N6 C22 N7 -178.1(8) . . . . ? C23 N6 C22 Pd1 -173.2(8) . . . . ? C25 N6 C22 Pd1 5.9(15) . . . . ? C1 Pd1 C22 N7 -140.5(8) . . . . ? N5 Pd1 C22 N7 -152(10) . . . . ? N10 Pd1 C22 N7 39.6(7) . . . . ? C1 Pd1 C22 N6 35.0(10) . . . . ? N5 Pd1 C22 N6 23(11) . . . . ? N10 Pd1 C22 N6 -144.9(10) . . . . ? C22 N6 C23 C24 -2.8(12) . . . . ? C25 N6 C23 C24 178.1(9) . . . . ? N6 C23 C24 N7 1.5(12) . . . . ? C22 N7 C24 C23 0.2(12) . . . . ? C37 N7 C24 C23 177.9(10) . . . . ? C29 N8 C25 C26 0.1(15) . . . . ? C29 N8 C25 N6 179.2(8) . . . . ? C22 N6 C25 N8 -138.8(9) . . . . ? C23 N6 C25 N8 40.3(13) . . . . ? C22 N6 C25 C26 40.4(14) . . . . ? C23 N6 C25 C26 -140.6(10) . . . . ? N8 C25 C26 C27 -1.4(15) . . . . ? N6 C25 C26 C27 179.6(9) . . . . ? C25 C26 C27 C28 1.3(15) . . . . ? C26 C27 C28 C29 0.0(15) . . . . ? C26 C27 C28 C35 -179.9(10) . . . . ? C25 N8 C29 C28 1.3(14) . . . . ? C25 N8 C29 C30 -175.9(9) . . . . ? C27 C28 C29 N8 -1.3(15) . . . . ? C35 C28 C29 N8 178.5(10) . . . . ? C27 C28 C29 C30 175.9(9) . . . . ? C35 C28 C29 C30 -4.3(15) . . . . ? C34 N9 C30 C31 -0.6(17) . . . . ? C34 N9 C30 C29 176.8(11) . . . . ? N8 C29 C30 N9 1.0(15) . . . . ? C28 C29 C30 N9 -176.3(10) . . . . ? N8 C29 C30 C31 178.5(9) . . . . ? C28 C29 C30 C31 1.2(15) . . . . ? N9 C30 C31 C32 -0.6(17) . . . . ? C29 C30 C31 C32 -178.0(10) . . . . ? N9 C30 C31 C36 179.9(11) . . . . ? C29 C30 C31 C36 2.5(16) . . . . ? C30 C31 C32 C33 0.9(17) . . . . ? C36 C31 C32 C33 -179.7(12) . . . . ? C31 C32 C33 C34 0.0(19) . . . . ? C30 N9 C34 C33 1.6(19) . . . . ? C32 C33 C34 N9 -1(2) . . . . ? C27 C28 C35 C36 -176.4(11) . . . . ? C29 C28 C35 C36 3.8(16) . . . . ? C28 C35 C36 C31 0.1(18) . . . . ? C32 C31 C36 C35 177.4(12) . . . . ? C30 C31 C36 C35 -3.2(18) . . . . ? C22 N7 C37 C38 -52.5(12) . . . . ? C24 N7 C37 C38 130.1(10) . . . . ? C42 N10 C38 C39 0.1(15) . . . . ? Pd1 N10 C38 C39 178.0(8) . . . . ? C42 N10 C38 C37 179.1(9) . . . . ? Pd1 N10 C38 C37 -3.0(12) . . . . ? N7 C37 C38 N10 53.8(13) . . . . ? N7 C37 C38 C39 -127.2(10) . . . . ? N10 C38 C39 C40 1.2(17) . . . . ? C37 C38 C39 C40 -177.8(11) . . . . ? C38 C39 C40 C41 -1.3(18) . . . . ? C39 C40 C41 C42 0.1(19) . . . . ? C38 N10 C42 C41 -1.4(16) . . . . ? Pd1 N10 C42 C41 -179.3(9) . . . . ? C40 C41 C42 N10 1.3(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.705 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.158