Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Chen, Zhong-Ning' 'Ishizaka, Shoji' 'Kitamura, Noboru' 'Wu, Ji-Gui' 'Xu, Hong-Wu' _publ_requested_journal ' ChemComm' _publ_contact_author_name 'Prof Zhong-Ning Chen' _publ_contact_author_address ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Yangqiao Xi Lu No.155 Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email ' czn@ms.fjirsm.ac.cn ' _publ_section_title ; Self-assembly luminescent heteroheptanuclear complexes with metal diphosphine and metal thiolate as components ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ; data_Cu4Ni3 _database_code_CSD 185408 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H94 Cl4 Cu4 N6 Ni3 O17 P6 S6' _chemical_formula_weight 2445.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ni' 'Ni' 0.3393 1.1124 '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 24.534(5) _cell_length_b 19.431(4) _cell_length_c 26.881(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.59(3) _cell_angle_gamma 90.00 _cell_volume 12455(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27548 _cell_measurement_theta_min 0.85 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'prism' _exptl_crystal_colour 'black red' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4992 _exptl_absorpt_coefficient_mu 1.430 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27548 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 22.50 _reflns_number_total 15806 _reflns_number_gt 9459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15806 _refine_ls_number_parameters 1156 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2887 _refine_ls_wR_factor_gt 0.2501 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.16321(5) 1.69120(6) 0.79072(5) 0.0603(4) Uani 1 1 d . . . Cu2 Cu 0.30186(5) 1.67492(6) 0.77157(5) 0.0592(4) Uani 1 1 d . . . Cu3 Cu 0.31329(5) 1.87316(6) 0.76841(5) 0.0607(4) Uani 1 1 d . . . Cu4 Cu 0.17248(5) 1.88985(6) 0.78414(5) 0.0594(4) Uani 1 1 d . . . Ni1 Ni 0.18934(6) 1.78546(7) 0.67016(5) 0.0645(4) Uani 1 1 d . . . Ni2 Ni 0.25166(6) 1.78648(7) 0.88957(5) 0.0625(4) Uani 1 1 d . . . Ni3 Ni 0.06344(6) 1.80507(8) 0.86784(6) 0.0759(5) Uani 1 1 d . . . Cl1 Cl 0.1353(2) 0.8389(3) 0.01887(17) 0.1286(15) Uani 1 1 d D . . Cl2 Cl 0.3817(3) 0.7175(5) 0.5261(3) 0.187(3) Uani 1 1 d D . . Cl3 Cl 0.1393(3) 0.9191(4) 0.5139(3) 0.206(3) Uiso 1 1 d D . . Cl4 Cl 0.1226(6) 2.3066(7) 0.6235(5) 0.276(4) Uiso 1 1 d D . . S1 S 0.15275(10) 1.78783(13) 0.73598(10) 0.0557(6) Uani 1 1 d . . . S2 S 0.27420(10) 1.77463(13) 0.71864(10) 0.0564(6) Uani 1 1 d . . . S3 S 0.26234(10) 1.86567(14) 0.83484(10) 0.0580(6) Uani 1 1 d . . . S4 S 0.25590(11) 1.70077(14) 0.83839(10) 0.0597(7) Uani 1 1 d . . . S5 S 0.10334(18) 1.87997(17) 0.82996(16) 0.1039(13) Uani 1 1 d . . . S6 S 0.1010(2) 1.71853(19) 0.8396(2) 0.141(2) Uani 1 1 d . . . P1 P 0.14281(11) 1.59482(14) 0.74309(11) 0.0603(7) Uani 1 1 d . . . P2 P 0.26473(11) 1.57534(14) 0.73099(11) 0.0625(7) Uani 1 1 d . . . P3 P 0.39560(11) 1.68493(15) 0.80908(12) 0.0633(7) Uani 1 1 d . . . P4 P 0.40546(11) 1.84743(15) 0.80623(12) 0.0664(8) Uani 1 1 d . . . P5 P 0.29026(11) 1.97622(14) 0.72616(11) 0.0616(7) Uani 1 1 d . . . P6 P 0.16560(11) 1.98530(13) 0.73499(11) 0.0579(7) Uani 1 1 d . . . O11 O 0.1528(5) 0.8419(8) 0.0727(2) 0.168(5) Uani 1 1 d D . . O12 O 0.0780(4) 0.8227(13) 0.0100(8) 0.293(12) Uani 1 1 d D . . O13 O 0.1699(7) 0.7897(7) 0.0032(6) 0.227(9) Uani 1 1 d D . . O14 O 0.1458(9) 0.9019(6) -0.0030(8) 0.276(11) Uani 1 1 d D . . O21 O 0.3273(7) 0.7056(11) 0.5307(6) 0.238(9) Uani 1 1 d D . . O22 O 0.3854(10) 0.7292(12) 0.4777(7) 0.301(13) Uani 1 1 d D . . O23 O 0.3996(12) 0.7703(17) 0.5634(13) 0.53(4) Uani 1 1 d D . . O24 O 0.4152(14) 0.6624(14) 0.5500(13) 0.51(3) Uani 1 1 d D . . O31 O 0.1669(9) 0.9200(11) 0.5678(6) 0.274(9) Uiso 1 1 d D . . O32 O 0.0946(10) 0.8739(14) 0.5142(11) 0.384(16) Uiso 1 1 d D . . O33 O 0.1327(15) 0.9833(11) 0.4958(12) 0.47(2) Uiso 1 1 d D . . O34 O 0.1837(13) 0.890(2) 0.4955(15) 0.58(3) Uiso 1 1 d D . . O41 O 0.0770(14) 2.310(2) 0.5772(12) 0.231(15) Uiso 0.50 1 d PD . . O41' O 0.148(2) 2.277(3) 0.5853(17) 0.31(2) Uiso 0.50 1 d PD . . O42 O 0.0847(13) 2.3003(18) 0.6570(12) 0.207(13) Uiso 0.50 1 d PD . . O42' O 0.1250(16) 2.3816(13) 0.6295(14) 0.229(15) Uiso 0.50 1 d PD . . O43 O 0.1175(18) 2.2328(12) 0.6250(17) 0.43(2) Uiso 1 1 d D . . O44 O 0.1797(12) 2.303(2) 0.6537(16) 0.52(3) Uiso 1 1 d D . . O100 O 0.4468(16) 1.3014(19) 0.9342(11) 0.44(2) Uani 1 1 d . . . N1 N 0.1143(4) 1.7895(6) 0.6266(4) 0.100(4) Uani 1 1 d . . . H1A H 0.1074 1.7776 0.5950 0.120 Uiso 1 1 calc R . . N2 N 0.2208(5) 1.7858(6) 0.6099(4) 0.107(4) Uani 1 1 d . . . H2A H 0.2004 1.7843 0.5792 0.128 Uiso 1 1 calc R . . N3 N 0.2458(5) 1.8573(5) 0.9376(4) 0.091(3) Uani 1 1 d . . . H3A H 0.2451 1.8480 0.9687 0.109 Uiso 1 1 calc R . . N4 N 0.2415(5) 1.7211(5) 0.9404(4) 0.091(3) Uani 1 1 d . . . H4A H 0.2353 1.7341 0.9691 0.109 Uiso 1 1 calc R . . N5 N 0.0265(5) 1.8807(6) 0.8935(5) 0.109(4) Uani 1 1 d . . . H5A H 0.0113 1.8765 0.9191 0.131 Uiso 1 1 calc R . . N6 N 0.0280(6) 1.7374(7) 0.9038(6) 0.131(5) Uani 1 1 d . . . H6A H 0.0159 1.7480 0.9304 0.158 Uiso 1 1 calc R . . C1 C 0.0783(4) 1.7910(6) 0.7036(5) 0.078(3) Uani 1 1 d . . . H1B H 0.0618 1.7458 0.7046 0.094 Uiso 1 1 calc R . . H1C H 0.0591 1.8228 0.7215 0.094 Uiso 1 1 calc R . . C2 C 0.0706(5) 1.8134(7) 0.6498(5) 0.093(4) Uani 1 1 d . . . H2B H 0.0348 1.7964 0.6301 0.112 Uiso 1 1 calc R . . H2C H 0.0695 1.8633 0.6485 0.112 Uiso 1 1 calc R . . C3 C 0.3111(6) 1.7661(8) 0.6671(5) 0.094(4) Uani 1 1 d . . . H3B H 0.3459 1.7918 0.6763 0.113 Uiso 1 1 calc R . . H3C H 0.3205 1.7180 0.6640 0.113 Uiso 1 1 calc R . . C4 C 0.2810(8) 1.7886(14) 0.6214(6) 0.205(13) Uani 1 1 d . . . H4B H 0.2931 1.7625 0.5951 0.245 Uiso 1 1 calc R . . H4C H 0.2916 1.8361 0.6177 0.245 Uiso 1 1 calc R . . C5 C 0.2780(5) 1.9366(6) 0.8803(4) 0.075(3) Uani 1 1 d . . . H5B H 0.3176 1.9368 0.8972 0.090 Uiso 1 1 calc R . . H5C H 0.2688 1.9802 0.8628 0.090 Uiso 1 1 calc R . . C6 C 0.2428(6) 1.9259(7) 0.9191(5) 0.093(4) Uani 1 1 d . . . H6B H 0.2556 1.9570 0.9477 0.111 Uiso 1 1 calc R . . H6C H 0.2041 1.9371 0.9034 0.111 Uiso 1 1 calc R . . C7 C 0.2652(5) 1.6311(6) 0.8859(5) 0.083(4) Uani 1 1 d . . . H7A H 0.2462 1.5902 0.8697 0.099 Uiso 1 1 calc R . . H7B H 0.3048 1.6205 0.8971 0.099 Uiso 1 1 calc R . . C8 C 0.2449(12) 1.6472(9) 0.9277(7) 0.212(14) Uani 1 1 d . . . H8A H 0.2336 1.6131 0.9474 0.254 Uiso 1 1 calc R . . C9 C 0.0772(7) 1.9537(7) 0.8544(7) 0.119(5) Uani 1 1 d . . . H9A H 0.1044 1.9687 0.8848 0.143 Uiso 1 1 calc R . . H9B H 0.0732 1.9902 0.8292 0.143 Uiso 1 1 calc R . . C10 C 0.0265(7) 1.9437(8) 0.8667(8) 0.147(7) Uani 1 1 d . . . H10A H -0.0032 1.9430 0.8357 0.176 Uiso 1 1 calc R . . H10B H 0.0193 1.9815 0.8878 0.176 Uiso 1 1 calc R . . C11 C 0.0703(6) 1.6501(8) 0.8662(5) 0.108(5) Uani 1 1 d . . . H11A H 0.0589 1.6146 0.8405 0.130 Uiso 1 1 calc R . . H11B H 0.0981 1.6303 0.8943 0.130 Uiso 1 1 calc R . . C12 C 0.0235(10) 1.6712(9) 0.8841(11) 0.211(14) Uani 1 1 d . . . H12A H -0.0096 1.6686 0.8561 0.253 Uiso 1 1 calc R . . H12B H 0.0183 1.6395 0.9105 0.253 Uiso 1 1 calc R . . C20 C 0.4154(5) 1.7657(6) 0.8422(4) 0.073(3) Uani 1 1 d . . . H20A H 0.4306 1.7660 0.8773 0.088 Uiso 1 1 calc R . . C30 C 0.2156(4) 1.9884(5) 0.6946(4) 0.058(3) Uani 1 1 d . . . H30A H 0.2116 2.0326 0.6773 0.070 Uiso 1 1 calc R . . H30B H 0.2051 1.9533 0.6684 0.070 Uiso 1 1 calc R . . C40 C 0.1899(4) 1.5795(6) 0.7005(4) 0.065(3) Uani 1 1 d . . . H40A H 0.1791 1.5366 0.6825 0.078 Uiso 1 1 calc R . . H40B H 0.1841 1.6159 0.6751 0.078 Uiso 1 1 calc R . . C111 C 0.0755(4) 1.6042(5) 0.6983(5) 0.066(3) Uani 1 1 d . . . C112 C 0.0666(5) 1.6103(7) 0.6464(5) 0.085(4) Uani 1 1 d . . . H11C H 0.0964 1.6042 0.6309 0.103 Uiso 1 1 calc R . . C113 C 0.0140(7) 1.6255(8) 0.6163(6) 0.115(5) Uani 1 1 d . . . H11D H 0.0085 1.6292 0.5810 0.138 Uiso 1 1 calc R . . C114 C -0.0297(5) 1.6351(8) 0.6389(7) 0.109(5) Uani 1 1 d . . . H11E H -0.0649 1.6456 0.6185 0.131 Uiso 1 1 calc R . . C115 C -0.0233(5) 1.6297(7) 0.6900(6) 0.095(4) Uani 1 1 d . . . H11F H -0.0535 1.6360 0.7049 0.114 Uiso 1 1 calc R . . C116 C 0.0288(5) 1.6146(6) 0.7192(5) 0.086(4) Uani 1 1 d . . . H11G H 0.0336 1.6112 0.7545 0.103 Uiso 1 1 calc R . . C121 C 0.1349(4) 1.5101(5) 0.7719(5) 0.069(3) Uani 1 1 d . . . C122 C 0.1136(5) 1.4551(6) 0.7426(6) 0.088(4) Uani 1 1 d . . . H12C H 0.1032 1.4588 0.7072 0.105 Uiso 1 1 calc R . . C123 C 0.1076(8) 1.3935(7) 0.7665(9) 0.119(6) Uani 1 1 d . . . H12D H 0.0931 1.3557 0.7465 0.142 Uiso 1 1 calc R . . C124 C 0.1217(8) 1.3867(9) 0.8160(10) 0.132(7) Uani 1 1 d . . . H12E H 0.1160 1.3448 0.8307 0.158 Uiso 1 1 calc R . . C125 C 0.1452(6) 1.4418(9) 0.8473(7) 0.112(5) Uani 1 1 d . . . H12F H 0.1560 1.4372 0.8827 0.135 Uiso 1 1 calc R . . C126 C 0.1515(5) 1.5009(7) 0.8242(5) 0.082(3) Uani 1 1 d . . . H12G H 0.1677 1.5378 0.8443 0.098 Uiso 1 1 calc R . . C131 C 0.2721(5) 1.4936(6) 0.7647(5) 0.076(3) Uani 1 1 d . . . C132 C 0.2481(5) 1.4335(6) 0.7427(6) 0.092(4) Uani 1 1 d . . . H13A H 0.2253 1.4362 0.7098 0.110 Uiso 1 1 calc R . . C133 C 0.2548(8) 1.3719(9) 0.7649(10) 0.142(7) Uani 1 1 d . . . H13B H 0.2393 1.3324 0.7477 0.171 Uiso 1 1 calc R . . C134 C 0.2863(8) 1.3699(8) 0.8148(10) 0.139(8) Uani 1 1 d . . . H13C H 0.2919 1.3275 0.8313 0.167 Uiso 1 1 calc R . . C135 C 0.3096(7) 1.4276(9) 0.8412(7) 0.117(5) Uani 1 1 d . . . H13D H 0.3289 1.4252 0.8754 0.141 Uiso 1 1 calc R . . C136 C 0.3030(5) 1.4898(6) 0.8144(6) 0.087(4) Uani 1 1 d . . . H13E H 0.3198 1.5294 0.8305 0.104 Uiso 1 1 calc R . . C141 C 0.2959(5) 1.5528(6) 0.6783(5) 0.074(3) Uani 1 1 d . . . C142 C 0.3467(5) 1.5198(8) 0.6887(6) 0.105(5) Uani 1 1 d . . . H14A H 0.3634 1.5067 0.7221 0.126 Uiso 1 1 calc R . . C143 C 0.3729(8) 1.5058(11) 0.6501(9) 0.141(7) Uani 1 1 d . . . H14B H 0.4064 1.4814 0.6580 0.169 Uiso 1 1 calc R . . C144 C 0.3540(9) 1.5243(12) 0.6047(10) 0.149(8) Uani 1 1 d . . . H14C H 0.3743 1.5150 0.5804 0.179 Uiso 1 1 calc R . . C145 C 0.3024(10) 1.5588(10) 0.5901(7) 0.157(8) Uani 1 1 d . . . H14D H 0.2881 1.5728 0.5565 0.188 Uiso 1 1 calc R . . C146 C 0.2725(7) 1.5716(7) 0.6295(6) 0.112(5) Uani 1 1 d . . . H14E H 0.2375 1.5927 0.6214 0.134 Uiso 1 1 calc R . . C151 C 0.4476(5) 1.6713(6) 0.7731(5) 0.071(3) Uani 1 1 d . . . C152 C 0.4310(6) 1.6632(6) 0.7210(6) 0.096(4) Uani 1 1 d . . . H15A H 0.3924 1.6625 0.7073 0.116 Uiso 1 1 calc R . . C153 C 0.4641(8) 1.6561(10) 0.6863(8) 0.131(6) Uani 1 1 d . . . H15B H 0.4500 1.6504 0.6513 0.157 Uiso 1 1 calc R . . C154 C 0.5154(13) 1.6581(12) 0.7076(9) 0.169(11) Uani 1 1 d . . . H15C H 0.5397 1.6565 0.6857 0.203 Uiso 1 1 calc R . . C155 C 0.5397(7) 1.6622(9) 0.7570(12) 0.175(11) Uani 1 1 d . . . H15D H 0.5784 1.6594 0.7685 0.210 Uiso 1 1 calc R . . C156 C 0.5028(5) 1.6715(8) 0.7941(6) 0.103(5) Uani 1 1 d . . . H15E H 0.5173 1.6769 0.8291 0.124 Uiso 1 1 calc R . . C161 C 0.4191(4) 1.6244(6) 0.8615(5) 0.079(3) Uani 1 1 d . . . C162 C 0.4352(5) 1.5573(7) 0.8497(6) 0.099(4) Uani 1 1 d . . . H16A H 0.4376 1.5450 0.8169 0.119 Uiso 1 1 calc R . . C163 C 0.4475(7) 1.5101(8) 0.8913(9) 0.127(6) Uani 1 1 d . . . H16B H 0.4582 1.4658 0.8846 0.153 Uiso 1 1 calc R . . C164 C 0.4448(8) 1.5243(11) 0.9390(8) 0.134(7) Uani 1 1 d . . . H16C H 0.4524 1.4907 0.9643 0.160 Uiso 1 1 calc R . . C165 C 0.4308(7) 1.5885(10) 0.9494(6) 0.121(5) Uani 1 1 d . . . H16D H 0.4297 1.5997 0.9828 0.145 Uiso 1 1 calc R . . C166 C 0.4178(5) 1.6389(7) 0.9118(6) 0.095(4) Uani 1 1 d . . . H16E H 0.4082 1.6829 0.9205 0.114 Uiso 1 1 calc R . . C171 C 0.4606(5) 1.8487(6) 0.7712(6) 0.086(4) Uani 1 1 d . . . C172 C 0.4449(7) 1.8556(7) 0.7188(6) 0.105(4) Uani 1 1 d . . . H17A H 0.4073 1.8602 0.7019 0.126 Uiso 1 1 calc R . . C173 C 0.4885(11) 1.8554(11) 0.6909(9) 0.161(9) Uani 1 1 d . . . H17B H 0.4793 1.8569 0.6553 0.193 Uiso 1 1 calc R . . C174 C 0.5422(12) 1.8531(13) 0.7164(14) 0.200(15) Uani 1 1 d . . . H17C H 0.5696 1.8575 0.6978 0.240 Uiso 1 1 calc R . . C175 C 0.5611(10) 1.8438(12) 0.7736(14) 0.210(14) Uani 1 1 d . . . H17D H 0.5984 1.8390 0.7911 0.252 Uiso 1 1 calc R . . C176 C 0.5166(6) 1.8433(9) 0.7969(8) 0.141(7) Uani 1 1 d . . . H17E H 0.5247 1.8390 0.8323 0.169 Uiso 1 1 calc R . . C181 C 0.4334(5) 1.9083(6) 0.8567(5) 0.073(3) Uani 1 1 d . . . C182 C 0.4612(6) 1.9671(8) 0.8472(7) 0.114(5) Uani 1 1 d . . . H18A H 0.4692 1.9728 0.8153 0.137 Uiso 1 1 calc R . . C183 C 0.4778(7) 2.0191(9) 0.8853(8) 0.138(7) Uani 1 1 d . . . H18B H 0.4962 2.0583 0.8778 0.166 Uiso 1 1 calc R . . C184 C 0.4669(8) 2.0117(9) 0.9324(8) 0.132(6) Uani 1 1 d . . . H18C H 0.4782 2.0460 0.9568 0.159 Uiso 1 1 calc R . . C185 C 0.4393(7) 1.9540(9) 0.9449(6) 0.118(5) Uani 1 1 d . . . H18D H 0.4318 1.9483 0.9770 0.141 Uiso 1 1 calc R . . C186 C 0.4230(5) 1.9033(7) 0.9043(6) 0.094(4) Uani 1 1 d . . . H18E H 0.4040 1.8644 0.9113 0.113 Uiso 1 1 calc R . . C191 C 0.3085(4) 2.0567(5) 0.7608(5) 0.072(3) Uani 1 1 d . . . C192 C 0.2958(5) 2.1181(6) 0.7373(6) 0.093(4) Uani 1 1 d . . . H19A H 0.2781 2.1196 0.7027 0.111 Uiso 1 1 calc R . . C193 C 0.3091(7) 2.1796(8) 0.7648(9) 0.123(6) Uani 1 1 d . . . H19B H 0.3005 2.2220 0.7488 0.148 Uiso 1 1 calc R . . C194 C 0.3346(7) 2.1757(10) 0.8149(10) 0.132(7) Uani 1 1 d . . . H19C H 0.3427 2.2164 0.8334 0.158 Uiso 1 1 calc R . . C195 C 0.3489(6) 2.1146(9) 0.8398(7) 0.114(5) Uani 1 1 d . . . H19D H 0.3673 2.1136 0.8742 0.137 Uiso 1 1 calc R . . C196 C 0.3354(5) 2.0539(7) 0.8121(5) 0.086(4) Uani 1 1 d . . . H19E H 0.3444 2.0116 0.8281 0.103 Uiso 1 1 calc R . . C201 C 0.3232(5) 1.9886(6) 0.6724(5) 0.078(3) Uani 1 1 d . . . C202 C 0.3799(6) 2.0058(8) 0.6858(6) 0.116(5) Uani 1 1 d . . . H20B H 0.3975 2.0128 0.7200 0.139 Uiso 1 1 calc R . . C203 C 0.4107(8) 2.0126(11) 0.6483(8) 0.152(7) Uani 1 1 d . . . H20C H 0.4480 2.0265 0.6566 0.182 Uiso 1 1 calc R . . C204 C 0.3824(11) 1.9973(13) 0.5972(10) 0.173(9) Uani 1 1 d . . . H20D H 0.4029 1.9967 0.5722 0.207 Uiso 1 1 calc R . . C205 C 0.3258(11) 1.9835(13) 0.5828(8) 0.178(9) Uani 1 1 d . . . H20E H 0.3075 1.9792 0.5485 0.213 Uiso 1 1 calc R . . C206 C 0.2967(7) 1.9762(9) 0.6218(6) 0.120(5) Uani 1 1 d . . . H20F H 0.2592 1.9629 0.6134 0.145 Uiso 1 1 calc R . . C211 C 0.1683(4) 2.0719(5) 0.7639(5) 0.064(3) Uani 1 1 d . . . C212 C 0.1820(5) 2.0772(6) 0.8166(5) 0.077(3) Uani 1 1 d . . . H21A H 0.1902 2.0379 0.8367 0.092 Uiso 1 1 calc R . . C213 C 0.1832(6) 2.1392(8) 0.8385(6) 0.108(5) Uani 1 1 d . . . H21B H 0.1924 2.1427 0.8740 0.130 Uiso 1 1 calc R . . C214 C 0.1713(6) 2.1966(8) 0.8100(8) 0.104(5) Uani 1 1 d . . . H21C H 0.1724 2.2394 0.8257 0.125 Uiso 1 1 calc R . . C215 C 0.1583(7) 2.1917(7) 0.7604(8) 0.110(5) Uani 1 1 d . . . H21D H 0.1510 2.2318 0.7412 0.132 Uiso 1 1 calc R . . C216 C 0.1549(5) 2.1293(6) 0.7350(5) 0.081(3) Uani 1 1 d . . . H21E H 0.1438 2.1269 0.6995 0.097 Uiso 1 1 calc R . . C221 C 0.1000(4) 1.9905(5) 0.6883(4) 0.059(3) Uani 1 1 d . . . C222 C 0.0937(5) 1.9984(7) 0.6360(5) 0.091(4) Uani 1 1 d . . . H22A H 0.1252 2.0032 0.6227 0.109 Uiso 1 1 calc R . . C223 C 0.0395(6) 1.9992(8) 0.6028(5) 0.102(4) Uani 1 1 d . . . H22B H 0.0354 2.0059 0.5678 0.123 Uiso 1 1 calc R . . C224 C -0.0069(5) 1.9902(7) 0.6223(6) 0.096(4) Uani 1 1 d . . . H22C H -0.0424 1.9883 0.6005 0.115 Uiso 1 1 calc R . . C225 C -0.0005(5) 1.9841(7) 0.6736(6) 0.093(4) Uani 1 1 d . . . H22D H -0.0324 1.9800 0.6865 0.112 Uiso 1 1 calc R . . C226 C 0.0516(4) 1.9836(6) 0.7073(5) 0.075(3) Uani 1 1 d . . . H22E H 0.0545 1.9788 0.7423 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0546(7) 0.0549(8) 0.0744(9) -0.0003(6) 0.0212(6) 0.0003(6) Cu2 0.0464(7) 0.0576(8) 0.0766(9) 0.0000(6) 0.0203(6) 0.0035(6) Cu3 0.0481(7) 0.0592(8) 0.0773(9) -0.0005(6) 0.0199(6) 0.0006(6) Cu4 0.0568(7) 0.0525(8) 0.0718(8) 0.0008(6) 0.0204(6) 0.0019(6) Ni1 0.0581(8) 0.0765(10) 0.0582(8) -0.0046(7) 0.0121(6) 0.0058(7) Ni2 0.0644(9) 0.0683(9) 0.0600(8) 0.0020(6) 0.0251(7) 0.0039(7) Ni3 0.0706(10) 0.0748(10) 0.0933(11) 0.0030(8) 0.0412(8) 0.0065(8) Cl1 0.141(4) 0.155(4) 0.100(3) 0.011(3) 0.050(3) 0.015(3) Cl2 0.158(6) 0.287(10) 0.117(4) 0.022(5) 0.035(4) -0.014(6) S1 0.0462(14) 0.0531(15) 0.0672(16) 0.0003(12) 0.0123(12) 0.0024(11) S2 0.0487(14) 0.0593(16) 0.0637(16) -0.0030(12) 0.0184(12) 0.0018(12) S3 0.0538(15) 0.0615(16) 0.0612(15) -0.0011(12) 0.0185(12) 0.0023(12) S4 0.0520(15) 0.0617(16) 0.0689(17) 0.0037(13) 0.0218(13) 0.0032(12) S5 0.129(3) 0.066(2) 0.147(3) -0.003(2) 0.093(3) 0.003(2) S6 0.178(5) 0.065(2) 0.236(5) 0.000(3) 0.162(5) -0.003(2) P1 0.0492(15) 0.0522(16) 0.0829(19) -0.0021(14) 0.0225(13) -0.0021(12) P2 0.0531(16) 0.0541(17) 0.0860(19) -0.0043(14) 0.0280(14) 0.0029(13) P3 0.0428(14) 0.0634(18) 0.085(2) 0.0010(15) 0.0188(13) 0.0057(13) P4 0.0459(15) 0.0664(18) 0.089(2) -0.0004(15) 0.0197(14) -0.0027(13) P5 0.0505(15) 0.0529(16) 0.087(2) 0.0017(14) 0.0271(14) -0.0007(12) P6 0.0486(15) 0.0485(15) 0.0786(18) 0.0016(13) 0.0193(13) 0.0024(12) O11 0.173(12) 0.238(15) 0.103(9) -0.030(9) 0.055(8) -0.011(11) O12 0.137(14) 0.48(4) 0.28(2) -0.08(2) 0.077(15) -0.037(18) O13 0.30(2) 0.226(17) 0.211(16) 0.005(13) 0.177(17) 0.074(15) O14 0.36(3) 0.24(2) 0.246(19) 0.112(17) 0.110(19) 0.022(19) O21 0.27(2) 0.30(2) 0.149(14) -0.027(13) 0.077(15) -0.01(2) O22 0.42(4) 0.30(3) 0.25(2) 0.070(19) 0.20(3) 0.08(2) O23 0.29(4) 0.76(8) 0.57(6) -0.45(6) 0.14(4) -0.06(4) O24 0.70(8) 0.34(4) 0.62(7) 0.13(4) 0.45(6) 0.21(5) O100 0.43(5) 0.54(5) 0.30(3) -0.07(3) -0.04(3) 0.09(4) N1 0.074(7) 0.157(11) 0.054(6) -0.015(6) -0.014(5) 0.012(7) N2 0.098(8) 0.171(12) 0.050(6) -0.010(6) 0.013(6) 0.027(8) N3 0.145(10) 0.071(7) 0.065(6) 0.004(5) 0.042(6) 0.006(7) N4 0.134(10) 0.085(8) 0.067(6) 0.006(5) 0.051(6) 0.007(7) N5 0.125(10) 0.091(8) 0.138(10) -0.003(7) 0.082(8) 0.017(7) N6 0.164(13) 0.101(10) 0.170(12) 0.002(9) 0.124(11) -0.021(9) C1 0.048(6) 0.077(8) 0.107(10) -0.008(7) 0.014(6) 0.004(6) C2 0.063(8) 0.104(10) 0.105(11) 0.016(8) 0.004(7) 0.002(7) C3 0.080(9) 0.134(12) 0.077(9) -0.009(8) 0.034(7) 0.006(8) C4 0.109(14) 0.44(4) 0.067(11) 0.006(16) 0.033(10) 0.054(19) C5 0.075(7) 0.066(7) 0.079(8) -0.014(6) 0.008(6) 0.004(6) C6 0.096(9) 0.113(11) 0.070(8) -0.031(8) 0.023(7) 0.011(8) C7 0.088(8) 0.067(8) 0.085(8) 0.011(6) 0.003(7) 0.000(6) C8 0.46(4) 0.100(13) 0.148(16) 0.053(12) 0.21(2) 0.064(18) C9 0.117(12) 0.100(11) 0.167(14) 0.017(10) 0.090(11) 0.024(9) C10 0.145(15) 0.074(10) 0.26(2) 0.024(12) 0.129(16) 0.031(10) C11 0.082(9) 0.154(14) 0.102(10) 0.010(9) 0.048(8) -0.005(9) C12 0.25(3) 0.084(12) 0.39(4) 0.010(17) 0.26(3) 0.009(14) C20 0.073(7) 0.068(7) 0.067(7) -0.010(6) -0.004(6) 0.002(6) C30 0.049(6) 0.062(6) 0.066(6) 0.003(5) 0.016(5) -0.001(5) C40 0.057(6) 0.067(7) 0.076(7) -0.008(6) 0.028(5) 0.001(5) C111 0.060(7) 0.052(6) 0.087(8) -0.004(6) 0.021(6) -0.006(5) C112 0.056(7) 0.099(10) 0.105(10) 0.007(8) 0.026(7) 0.000(6) C113 0.098(12) 0.134(14) 0.102(11) 0.029(10) 0.003(9) 0.009(10) C114 0.043(7) 0.113(12) 0.164(16) 0.034(11) 0.010(9) -0.001(7) C115 0.070(9) 0.089(10) 0.121(12) 0.005(9) 0.014(8) 0.003(7) C116 0.053(7) 0.082(9) 0.120(10) -0.006(7) 0.014(7) -0.006(6) C121 0.054(6) 0.046(6) 0.112(10) 0.005(6) 0.029(6) 0.003(5) C122 0.089(9) 0.057(8) 0.128(11) -0.007(7) 0.048(8) -0.011(7) C123 0.135(15) 0.053(9) 0.181(18) -0.010(11) 0.064(14) -0.007(9) C124 0.113(14) 0.072(11) 0.22(2) 0.042(15) 0.068(16) 0.019(10) C125 0.077(9) 0.105(12) 0.160(15) 0.063(12) 0.039(9) 0.020(9) C126 0.062(7) 0.095(10) 0.091(9) 0.015(8) 0.024(6) -0.004(6) C131 0.060(7) 0.061(8) 0.109(10) 0.007(7) 0.027(7) 0.004(6) C132 0.084(9) 0.052(8) 0.140(12) 0.003(8) 0.026(8) 0.007(7) C133 0.115(15) 0.071(12) 0.25(3) 0.012(14) 0.062(16) 0.019(10) C134 0.112(14) 0.052(10) 0.26(3) 0.037(14) 0.058(15) 0.019(9) C135 0.107(12) 0.116(14) 0.134(13) 0.029(11) 0.038(10) 0.023(10) C136 0.088(9) 0.055(8) 0.118(11) 0.012(7) 0.028(8) 0.018(6) C141 0.074(8) 0.069(8) 0.090(9) -0.011(6) 0.043(7) -0.010(6) C142 0.069(8) 0.124(12) 0.136(12) -0.027(10) 0.052(8) 0.008(8) C143 0.120(15) 0.147(17) 0.174(19) -0.017(16) 0.072(15) 0.031(12) C144 0.134(17) 0.17(2) 0.18(2) 0.000(17) 0.103(17) 0.040(14) C145 0.22(2) 0.168(18) 0.115(13) 0.017(12) 0.103(15) 0.013(17) C146 0.140(13) 0.100(11) 0.122(12) 0.003(9) 0.084(11) 0.023(10) C151 0.057(7) 0.076(8) 0.084(8) -0.008(6) 0.025(6) 0.007(6) C152 0.075(8) 0.078(9) 0.155(14) -0.016(9) 0.064(9) 0.008(7) C153 0.110(13) 0.154(17) 0.142(16) -0.046(13) 0.055(13) -0.018(13) C154 0.21(3) 0.18(2) 0.145(19) -0.090(17) 0.097(19) -0.07(2) C155 0.060(9) 0.115(14) 0.38(4) -0.037(19) 0.107(17) -0.011(9) C156 0.050(7) 0.128(12) 0.133(12) -0.025(10) 0.025(7) 0.003(7) C161 0.046(6) 0.076(8) 0.109(10) 0.006(7) 0.004(6) 0.012(6) C162 0.075(8) 0.091(10) 0.133(12) 0.012(9) 0.027(8) 0.022(8) C163 0.099(11) 0.070(10) 0.194(19) 0.050(12) -0.003(12) 0.025(8) C164 0.143(16) 0.124(17) 0.119(15) 0.025(13) 0.003(13) 0.019(12) C165 0.123(13) 0.132(15) 0.094(11) 0.034(11) 0.001(9) 0.006(11) C166 0.085(9) 0.091(10) 0.109(11) 0.011(9) 0.022(8) 0.013(8) C171 0.058(7) 0.079(9) 0.131(12) 0.008(8) 0.042(7) -0.002(6) C172 0.110(11) 0.095(10) 0.125(12) 0.002(9) 0.057(10) -0.019(9) C173 0.19(2) 0.163(18) 0.178(19) -0.007(15) 0.15(2) -0.003(17) C174 0.19(3) 0.137(18) 0.35(4) 0.03(2) 0.22(3) 0.026(18) C175 0.123(17) 0.16(2) 0.40(4) 0.08(3) 0.17(3) 0.036(15) C176 0.075(10) 0.163(16) 0.200(18) 0.078(14) 0.065(11) 0.023(10) C181 0.057(7) 0.061(7) 0.096(9) 0.005(6) 0.007(6) -0.007(5) C182 0.084(9) 0.097(11) 0.148(14) 0.024(10) -0.001(9) -0.020(8) C183 0.134(14) 0.106(13) 0.140(15) 0.016(12) -0.038(13) -0.062(11) C184 0.144(15) 0.096(13) 0.130(15) -0.021(11) -0.024(13) -0.028(11) C185 0.118(12) 0.116(13) 0.097(11) -0.022(10) -0.018(9) 0.003(10) C186 0.071(8) 0.088(10) 0.115(11) 0.006(9) 0.007(8) -0.013(7) C191 0.055(6) 0.050(7) 0.117(10) -0.007(7) 0.032(7) -0.007(5) C192 0.083(9) 0.060(8) 0.131(11) -0.008(8) 0.016(8) 0.002(7) C193 0.092(11) 0.067(10) 0.21(2) -0.006(12) 0.026(12) 0.009(8) C194 0.086(12) 0.088(13) 0.22(2) -0.058(15) 0.043(13) -0.011(10) C195 0.087(10) 0.114(13) 0.143(14) -0.031(12) 0.032(9) -0.020(10) C196 0.085(9) 0.072(9) 0.106(10) -0.019(8) 0.030(8) -0.020(7) C201 0.075(8) 0.074(8) 0.097(9) 0.024(7) 0.045(7) 0.005(6) C202 0.069(9) 0.153(15) 0.135(13) 0.020(11) 0.045(9) -0.005(9) C203 0.104(13) 0.22(2) 0.151(16) 0.012(16) 0.076(13) -0.003(13) C204 0.17(2) 0.23(2) 0.16(2) 0.016(18) 0.122(18) -0.019(19) C205 0.19(2) 0.26(3) 0.121(14) -0.027(15) 0.099(16) -0.04(2) C206 0.120(12) 0.153(15) 0.100(11) -0.012(10) 0.048(10) -0.028(11) C211 0.043(6) 0.061(7) 0.092(8) -0.011(6) 0.023(5) 0.001(5) C212 0.071(7) 0.059(7) 0.099(10) -0.014(7) 0.018(6) 0.005(6) C213 0.106(11) 0.094(11) 0.121(12) -0.031(10) 0.018(9) 0.014(9) C214 0.089(10) 0.071(10) 0.155(16) -0.032(11) 0.033(11) 0.011(8) C215 0.116(12) 0.058(9) 0.162(16) 0.019(10) 0.044(12) 0.016(8) C216 0.087(9) 0.052(7) 0.112(10) 0.012(7) 0.039(7) 0.005(6) C221 0.047(6) 0.049(6) 0.084(8) 0.001(5) 0.023(5) 0.000(5) C222 0.068(8) 0.102(10) 0.103(10) 0.010(8) 0.022(7) 0.000(7) C223 0.084(10) 0.127(12) 0.087(9) -0.009(8) 0.003(8) 0.009(9) C224 0.044(7) 0.104(10) 0.135(13) -0.020(9) 0.010(8) 0.011(7) C225 0.063(8) 0.109(11) 0.111(11) 0.005(9) 0.029(8) 0.016(7) C226 0.057(7) 0.089(9) 0.082(8) -0.005(6) 0.021(6) 0.007(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 Cu1 P1 2.257(3) . ? Cu1 S6 2.298(4) . ? Cu1 S4 2.341(3) . ? Cu1 S1 2.362(3) . ? Cu2 P3 2.292(3) . ? Cu2 P2 2.301(3) . ? Cu2 S4 2.388(3) . ? Cu2 S2 2.405(3) . ? Cu3 P4 2.306(3) . ? Cu3 P5 2.306(3) . ? Cu3 S2 2.403(3) . ? Cu3 S3 2.413(3) . ? Cu4 P6 2.260(3) . ? Cu4 S5 2.327(4) . ? Cu4 S3 2.351(3) . ? Cu4 S1 2.355(3) . ? Ni1 N1 1.937(9) . ? Ni1 N2 1.950(10) . ? Ni1 S1 2.164(3) . ? Ni1 S2 2.191(3) . ? Ni2 N3 1.914(10) . ? Ni2 N4 1.925(9) . ? Ni2 S4 2.178(3) . ? Ni2 S3 2.187(3) . ? Ni3 N5 1.937(10) . ? Ni3 N6 1.954(11) . ? Ni3 S6 2.140(4) . ? Ni3 S5 2.141(4) . ? Cl1 O13 1.406(5) . ? Cl1 O12 1.406(5) . ? Cl1 O14 1.408(5) . ? Cl1 O11 1.412(5) . ? Cl2 O22 1.344(13) . ? Cl2 O21 1.388(14) . ? Cl2 O24 1.408(16) . ? Cl2 O23 1.430(16) . ? Cl3 O33 1.335(16) . ? Cl3 O32 1.407(16) . ? Cl3 O34 1.416(17) . ? Cl3 O31 1.448(14) . ? Cl4 O43 1.440(18) . ? Cl4 O41' 1.44(2) . ? Cl4 O42 1.444(18) . ? Cl4 O44 1.45(2) . ? Cl4 O41 1.467(18) . ? Cl4 O42' 1.467(18) . ? S1 C1 1.830(11) . ? S2 C3 1.831(12) . ? S3 C5 1.822(11) . ? S4 C7 1.838(11) . ? S5 C9 1.758(14) . ? S6 C11 1.760(14) . ? P1 C111 1.811(11) . ? P1 C40 1.832(10) . ? P1 C121 1.849(11) . ? P2 C141 1.813(11) . ? P2 C131 1.815(12) . ? P2 C40 1.828(10) . ? P3 C151 1.792(11) . ? P3 C20 1.814(11) . ? P3 C161 1.823(13) . ? P4 C181 1.810(12) . ? P4 C171 1.821(13) . ? P4 C20 1.845(12) . ? P5 C191 1.821(11) . ? P5 C201 1.830(11) . ? P5 C30 1.845(9) . ? P6 C221 1.796(10) . ? P6 C30 1.820(10) . ? P6 C211 1.848(11) . ? O41' O43 1.67(5) . ? N1 C2 1.437(16) . ? N2 C4 1.44(2) . ? N3 C6 1.419(16) . ? N4 C8 1.482(19) . ? N5 C10 1.420(17) . ? N6 C12 1.39(2) . ? C1 C2 1.480(17) . ? C3 C4 1.35(2) . ? C5 C6 1.518(16) . ? C7 C8 1.369(18) . ? C9 C10 1.375(19) . ? C11 C12 1.407(19) . ? C111 C112 1.366(16) . ? C111 C116 1.404(16) . ? C112 C113 1.382(17) . ? C113 C114 1.36(2) . ? C114 C115 1.349(19) . ? C115 C116 1.366(16) . ? C121 C122 1.356(16) . ? C121 C126 1.381(15) . ? C122 C123 1.381(19) . ? C123 C124 1.30(2) . ? C124 C125 1.40(2) . ? C125 C126 1.332(17) . ? C131 C136 1.376(17) . ? C131 C132 1.378(16) . ? C132 C133 1.33(2) . ? C133 C134 1.38(3) . ? C134 C135 1.38(2) . ? C135 C136 1.398(19) . ? C141 C146 1.354(18) . ? C141 C142 1.371(17) . ? C142 C143 1.37(2) . ? C143 C144 1.25(2) . ? C144 C145 1.40(3) . ? C145 C146 1.44(2) . ? C151 C156 1.340(16) . ? C151 C152 1.373(17) . ? C152 C153 1.38(2) . ? C153 C154 1.26(3) . ? C154 C155 1.33(3) . ? C155 C156 1.51(2) . ? C161 C166 1.388(17) . ? C161 C162 1.419(17) . ? C162 C163 1.42(2) . ? C163 C164 1.33(2) . ? C164 C165 1.34(2) . ? C165 C166 1.388(19) . ? C171 C172 1.378(19) . ? C171 C176 1.389(19) . ? C172 C173 1.44(2) . ? C173 C174 1.33(3) . ? C174 C175 1.51(4) . ? C175 C176 1.38(2) . ? C181 C186 1.365(17) . ? C181 C182 1.384(17) . ? C182 C183 1.43(2) . ? C183 C184 1.36(2) . ? C184 C185 1.39(2) . ? C185 C186 1.456(18) . ? C191 C192 1.351(16) . ? C191 C196 1.383(16) . ? C192 C193 1.40(2) . ? C193 C194 1.35(2) . ? C194 C195 1.37(2) . ? C195 C196 1.393(18) . ? C201 C206 1.385(18) . ? C201 C202 1.392(17) . ? C202 C203 1.40(2) . ? C203 C204 1.42(3) . ? C204 C205 1.38(3) . ? C205 C206 1.41(2) . ? C211 C216 1.355(15) . ? C211 C212 1.381(15) . ? C212 C213 1.339(17) . ? C213 C214 1.35(2) . ? C214 C215 1.30(2) . ? C215 C216 1.384(19) . ? C221 C222 1.387(15) . ? C221 C226 1.405(14) . ? C222 C223 1.417(17) . ? C223 C224 1.372(18) . ? C224 C225 1.355(17) . ? C225 C226 1.383(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 S6 115.29(15) . . ? P1 Cu1 S4 115.71(11) . . ? S6 Cu1 S4 111.08(19) . . ? P1 Cu1 S1 109.21(11) . . ? S6 Cu1 S1 100.53(14) . . ? S4 Cu1 S1 103.14(10) . . ? P3 Cu2 P2 121.62(11) . . ? P3 Cu2 S4 104.69(11) . . ? P2 Cu2 S4 109.22(11) . . ? P3 Cu2 S2 107.83(11) . . ? P2 Cu2 S2 111.81(11) . . ? S4 Cu2 S2 99.10(10) . . ? P4 Cu3 P5 120.45(11) . . ? P4 Cu3 S2 107.12(11) . . ? P5 Cu3 S2 113.47(11) . . ? P4 Cu3 S3 106.59(11) . . ? P5 Cu3 S3 107.90(10) . . ? S2 Cu3 S3 98.95(10) . . ? P6 Cu4 S5 114.44(12) . . ? P6 Cu4 S3 115.72(11) . . ? S5 Cu4 S3 112.19(14) . . ? P6 Cu4 S1 113.07(11) . . ? S5 Cu4 S1 98.07(12) . . ? S3 Cu4 S1 101.19(10) . . ? N1 Ni1 N2 90.2(5) . . ? N1 Ni1 S1 88.6(3) . . ? N2 Ni1 S1 178.2(4) . . ? N1 Ni1 S2 176.8(4) . . ? N2 Ni1 S2 89.3(3) . . ? S1 Ni1 S2 91.98(11) . . ? N3 Ni2 N4 87.3(4) . . ? N3 Ni2 S4 175.9(3) . . ? N4 Ni2 S4 88.7(3) . . ? N3 Ni2 S3 89.3(3) . . ? N4 Ni2 S3 176.6(3) . . ? S4 Ni2 S3 94.71(11) . . ? N5 Ni3 N6 92.0(5) . . ? N5 Ni3 S6 177.3(4) . . ? N6 Ni3 S6 85.7(4) . . ? N5 Ni3 S5 87.6(4) . . ? N6 Ni3 S5 178.8(5) . . ? S6 Ni3 S5 94.72(15) . . ? O13 Cl1 O12 116.5(13) . . ? O13 Cl1 O14 106.5(11) . . ? O12 Cl1 O14 113.3(14) . . ? O13 Cl1 O11 106.1(10) . . ? O12 Cl1 O11 103.6(10) . . ? O14 Cl1 O11 110.6(11) . . ? O22 Cl2 O21 113.6(14) . . ? O22 Cl2 O24 113.8(16) . . ? O21 Cl2 O24 107.6(16) . . ? O22 Cl2 O23 118.6(19) . . ? O21 Cl2 O23 101.6(14) . . ? O24 Cl2 O23 100.1(19) . . ? O33 Cl3 O32 124.0(19) . . ? O33 Cl3 O34 106.5(19) . . ? O32 Cl3 O34 114.6(19) . . ? O33 Cl3 O31 110.0(17) . . ? O32 Cl3 O31 100.6(15) . . ? O34 Cl3 O31 97.9(17) . . ? O43 Cl4 O41' 71(2) . . ? O43 Cl4 O42 80(2) . . ? O41' Cl4 O42 149(3) . . ? O43 Cl4 O44 91(3) . . ? O41' Cl4 O44 82(3) . . ? O42 Cl4 O44 109(3) . . ? O43 Cl4 O41 91(2) . . ? O41' Cl4 O41 78(3) . . ? O42 Cl4 O41 93(2) . . ? O44 Cl4 O41 157(3) . . ? O43 Cl4 O42' 171(3) . . ? O41' Cl4 O42' 118(3) . . ? O42 Cl4 O42' 92(2) . . ? O44 Cl4 O42' 89(3) . . ? O41 Cl4 O42' 93(2) . . ? C1 S1 Ni1 99.9(4) . . ? C1 S1 Cu4 106.6(4) . . ? Ni1 S1 Cu4 113.34(12) . . ? C1 S1 Cu1 105.8(4) . . ? Ni1 S1 Cu1 119.15(12) . . ? Cu4 S1 Cu1 110.39(11) . . ? C3 S2 Ni1 97.4(4) . . ? C3 S2 Cu3 106.9(5) . . ? Ni1 S2 Cu3 116.98(12) . . ? C3 S2 Cu2 104.7(5) . . ? Ni1 S2 Cu2 121.72(12) . . ? Cu3 S2 Cu2 107.00(11) . . ? C5 S3 Ni2 97.0(4) . . ? C5 S3 Cu4 105.0(4) . . ? Ni2 S3 Cu4 106.64(11) . . ? C5 S3 Cu3 112.7(4) . . ? Ni2 S3 Cu3 134.84(13) . . ? Cu4 S3 Cu3 97.89(10) . . ? C7 S4 Ni2 98.1(4) . . ? C7 S4 Cu1 105.5(4) . . ? Ni2 S4 Cu1 102.83(11) . . ? C7 S4 Cu2 111.4(4) . . ? Ni2 S4 Cu2 137.48(13) . . ? Cu1 S4 Cu2 98.12(11) . . ? C9 S5 Ni3 97.4(5) . . ? C9 S5 Cu4 120.4(5) . . ? Ni3 S5 Cu4 141.24(17) . . ? C11 S6 Ni3 100.9(5) . . ? C11 S6 Cu1 117.5(5) . . ? Ni3 S6 Cu1 141.58(18) . . ? C111 P1 C40 102.2(5) . . ? C111 P1 C121 101.5(5) . . ? C40 P1 C121 105.1(5) . . ? C111 P1 Cu1 109.9(4) . . ? C40 P1 Cu1 113.6(4) . . ? C121 P1 Cu1 122.2(4) . . ? C141 P2 C131 99.6(6) . . ? C141 P2 C40 102.9(5) . . ? C131 P2 C40 103.6(5) . . ? C141 P2 Cu2 112.4(4) . . ? C131 P2 Cu2 121.1(4) . . ? C40 P2 Cu2 114.8(4) . . ? C151 P3 C20 104.5(6) . . ? C151 P3 C161 100.7(6) . . ? C20 P3 C161 100.3(6) . . ? C151 P3 Cu2 121.2(4) . . ? C20 P3 Cu2 114.5(4) . . ? C161 P3 Cu2 112.8(4) . . ? C181 P4 C171 100.5(6) . . ? C181 P4 C20 100.9(5) . . ? C171 P4 C20 105.1(6) . . ? C181 P4 Cu3 110.4(4) . . ? C171 P4 Cu3 122.7(5) . . ? C20 P4 Cu3 114.4(4) . . ? C191 P5 C201 100.9(6) . . ? C191 P5 C30 102.9(5) . . ? C201 P5 C30 101.3(5) . . ? C191 P5 Cu3 119.4(4) . . ? C201 P5 Cu3 113.6(4) . . ? C30 P5 Cu3 116.1(3) . . ? C221 P6 C30 101.6(5) . . ? C221 P6 C211 100.4(5) . . ? C30 P6 C211 105.0(5) . . ? C221 P6 Cu4 112.7(3) . . ? C30 P6 Cu4 114.0(3) . . ? C211 P6 Cu4 120.7(4) . . ? Cl4 O41' O43 54.4(14) . . ? Cl4 O43 O41' 54.6(14) . . ? C2 N1 Ni1 116.8(8) . . ? C4 N2 Ni1 114.2(9) . . ? C6 N3 Ni2 116.5(7) . . ? C8 N4 Ni2 116.9(8) . . ? C10 N5 Ni3 114.7(9) . . ? C12 N6 Ni3 116.1(11) . . ? C2 C1 S1 110.9(8) . . ? N1 C2 C1 113.1(10) . . ? C4 C3 S2 113.6(11) . . ? C3 C4 N2 119.7(16) . . ? C6 C5 S3 107.0(8) . . ? N3 C6 C5 112.2(10) . . ? C8 C7 S4 113.1(10) . . ? C7 C8 N4 117.5(13) . . ? C10 C9 S5 113.9(12) . . ? C9 C10 N5 110.6(13) . . ? C12 C11 S6 112.3(12) . . ? N6 C12 C11 113.8(17) . . ? P3 C20 P4 120.0(6) . . ? P6 C30 P5 117.2(5) . . ? P2 C40 P1 116.2(6) . . ? C112 C111 C116 116.6(11) . . ? C112 C111 P1 126.2(9) . . ? C116 C111 P1 116.7(9) . . ? C111 C112 C113 121.2(13) . . ? C114 C113 C112 119.4(14) . . ? C115 C114 C113 121.8(13) . . ? C114 C115 C116 118.1(14) . . ? C115 C116 C111 122.7(14) . . ? C122 C121 C126 118.1(11) . . ? C122 C121 P1 121.5(10) . . ? C126 C121 P1 120.4(9) . . ? C121 C122 C123 118.8(14) . . ? C124 C123 C122 122.1(17) . . ? C123 C124 C125 120.7(17) . . ? C126 C125 C124 117.1(17) . . ? C125 C126 C121 123.2(14) . . ? C136 C131 C132 117.0(12) . . ? C136 C131 P2 119.9(9) . . ? C132 C131 P2 123.1(11) . . ? C133 C132 C131 125.1(16) . . ? C132 C133 C134 116.3(18) . . ? C135 C134 C133 123.1(17) . . ? C134 C135 C136 117.1(16) . . ? C131 C136 C135 121.2(14) . . ? C146 C141 C142 118.7(12) . . ? C146 C141 P2 122.1(10) . . ? C142 C141 P2 119.0(11) . . ? C143 C142 C141 120.3(16) . . ? C144 C143 C142 123(2) . . ? C143 C144 C145 121.0(19) . . ? C144 C145 C146 117.1(18) . . ? C141 C146 C145 119.6(16) . . ? C156 C151 C152 117.3(12) . . ? C156 C151 P3 123.4(11) . . ? C152 C151 P3 119.3(9) . . ? C151 C152 C153 128.3(15) . . ? C154 C153 C152 112(2) . . ? C153 C154 C155 129(2) . . ? C154 C155 C156 118.3(17) . . ? C151 C156 C155 115.3(15) . . ? C166 C161 C162 118.4(13) . . ? C166 C161 P3 123.1(10) . . ? C162 C161 P3 118.3(11) . . ? C161 C162 C163 115.8(15) . . ? C164 C163 C162 125.1(17) . . ? C163 C164 C165 117.9(19) . . ? C164 C165 C166 122.0(18) . . ? C165 C166 C161 120.7(15) . . ? C172 C171 C176 121.5(14) . . ? C172 C171 P4 117.8(10) . . ? C176 C171 P4 120.7(13) . . ? C171 C172 C173 117.8(17) . . ? C174 C173 C172 120(2) . . ? C173 C174 C175 124(2) . . ? C176 C175 C174 112(2) . . ? C175 C176 C171 125(2) . . ? C186 C181 C182 116.2(13) . . ? C186 C181 P4 122.3(9) . . ? C182 C181 P4 121.1(12) . . ? C181 C182 C183 121.5(16) . . ? C184 C183 C182 120.3(16) . . ? C183 C184 C185 121.5(16) . . ? C184 C185 C186 115.4(16) . . ? C181 C186 C185 125.0(14) . . ? C192 C191 C196 120.3(11) . . ? C192 C191 P5 121.2(11) . . ? C196 C191 P5 118.6(9) . . ? C191 C192 C193 120.5(15) . . ? C194 C193 C192 118.3(16) . . ? C193 C194 C195 122.8(17) . . ? C194 C195 C196 118.3(16) . . ? C191 C196 C195 119.8(14) . . ? C206 C201 C202 120.4(13) . . ? C206 C201 P5 124.0(10) . . ? C202 C201 P5 115.3(11) . . ? C201 C202 C203 120.8(16) . . ? C202 C203 C204 116.9(17) . . ? C205 C204 C203 123.0(17) . . ? C204 C205 C206 118(2) . . ? C201 C206 C205 120.6(17) . . ? C216 C211 C212 119.6(11) . . ? C216 C211 P6 121.9(10) . . ? C212 C211 P6 118.4(9) . . ? C213 C212 C211 119.6(13) . . ? C212 C213 C214 121.0(15) . . ? C215 C214 C213 119.5(15) . . ? C214 C215 C216 122.9(14) . . ? C211 C216 C215 117.4(13) . . ? C222 C221 C226 118.5(10) . . ? C222 C221 P6 125.6(8) . . ? C226 C221 P6 115.9(8) . . ? C221 C222 C223 120.3(12) . . ? C224 C223 C222 119.8(13) . . ? C225 C224 C223 119.5(12) . . ? C224 C225 C226 122.4(12) . . ? C225 C226 C221 119.4(11) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.457 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.263 #==END data_Ag2Ni _database_code_CSD 185409 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H59 Ag2 F12 N3 Ni P4 S2 Sb2' _chemical_formula_weight 1708.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6320(2) _cell_length_b 16.2589(1) _cell_length_c 16.3912(3) _cell_angle_alpha 76.32(0) _cell_angle_beta 80.38(0) _cell_angle_gamma 87.409(1) _cell_volume 3224.86(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 25.06 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max .40 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.947 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .6538 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16678 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.06 _reflns_number_total 11187 _reflns_number_gt 8837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens 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^)+(0.0306P)^2^+15.4908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11187 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.009 _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 Sb1 Sb 0.76617(6) 0.43159(5) 0.49402(6) 0.0962(3) Uani 1 1 d . . . Sb2 Sb 1.0000 0.0000 1.0000 0.0661(2) Uani 1 2 d S . . Sb3 Sb 0.5000 0.0000 0.5000 0.0524(2) Uani 1 2 d S . . Ni Ni 0.54510(8) 0.57754(6) 0.72860(7) 0.0569(3) Uani 1 1 d . . . Ag1 Ag 0.68733(5) 0.65278(3) 0.84293(4) 0.05034(16) Uani 1 1 d . . . Ag2 Ag 0.67217(4) 0.79909(3) 0.69929(3) 0.04448(15) Uani 1 1 d . . . F11 F 0.7482(9) 0.3467(9) 0.4455(10) 0.271(8) Uani 1 1 d . . . F12 F 0.8928(10) 0.3874(11) 0.5104(14) 0.315(10) Uani 1 1 d . . . F13 F 0.8374(16) 0.4945(10) 0.4023(9) 0.305(10) Uani 1 1 d . . . F14 F 0.7125(16) 0.3661(8) 0.5990(9) 0.296(9) Uani 1 1 d . . . F15 F 0.6325(9) 0.4636(9) 0.4872(11) 0.262(8) Uani 1 1 d . . . F16 F 0.7740(8) 0.5117(6) 0.5539(7) 0.183(4) Uani 1 1 d . . . F21 F 1.1336(5) 0.0332(5) 1.0127(4) 0.117(2) Uani 1 1 d . . . F22 F 1.0579(9) -0.0995(7) 0.9996(13) 0.290(9) Uani 1 1 d . . . F23 F 1.0389(7) 0.0298(12) 0.8894(5) 0.291(10) Uani 1 1 d . . . F31 F 0.5856(4) -0.0682(3) 0.5719(3) 0.0736(14) Uani 1 1 d . . . F32 F 0.4986(8) -0.0845(5) 0.4432(5) 0.148(3) Uani 1 1 d . . . F33 F 0.6191(5) 0.0460(6) 0.4263(5) 0.144(3) Uani 1 1 d . . . S1 S 0.50026(16) 0.70896(12) 0.72248(13) 0.0531(5) Uani 1 1 d . . . S2 S 0.53341(18) 0.55231(14) 0.86590(15) 0.0647(6) Uani 1 1 d . . . P1 P 0.64773(15) 0.75216(11) 0.93672(12) 0.0439(4) Uani 1 1 d . . . P2 P 0.65466(14) 0.90572(11) 0.78836(11) 0.0401(4) Uani 1 1 d . . . P3 P 0.83812(15) 0.75977(12) 0.61424(12) 0.0451(4) Uani 1 1 d . . . P4 P 0.86503(16) 0.62043(12) 0.77098(13) 0.0493(5) Uani 1 1 d . . . C1 C 0.7006(6) 0.8599(4) 0.8904(4) 0.0429(16) Uani 1 1 d . . . H1B H 0.6769 0.8956 0.9298 0.051 Uiso 1 1 calc R . . H1C H 0.7785 0.8580 0.8816 0.051 Uiso 1 1 calc R . . C01 C 0.4448(15) 0.2826(17) 0.6892(12) 0.146(7) Uani 1 1 d . . . C2 C 0.8762(6) 0.6491(4) 0.6549(5) 0.0491(17) Uani 1 1 d . . . H2B H 0.8304 0.6123 0.6375 0.059 Uiso 1 1 calc R . . H2C H 0.9496 0.6400 0.6298 0.059 Uiso 1 1 calc R . . C02 C 0.451(2) 0.1971(13) 0.6936(14) 0.221(11) Uani 1 1 d . . . H02A H 0.4919 0.1702 0.7369 0.331 Uiso 1 1 calc R . . H02B H 0.4845 0.1875 0.6397 0.331 Uiso 1 1 calc R . . H02C H 0.3795 0.1740 0.7074 0.331 Uiso 1 1 calc R . . C3 C 0.4625(9) 0.7327(6) 0.6169(7) 0.087(3) Uani 1 1 d . . . H3A H 0.3887 0.7160 0.6208 0.104 Uiso 1 1 calc R . . H3B H 0.4680 0.7931 0.5922 0.104 Uiso 1 1 calc R . . C4 C 0.5352(10) 0.6858(8) 0.5622(7) 0.102(4) Uani 1 1 d . . . H4A H 0.5089 0.6903 0.5090 0.122 Uiso 1 1 calc R . . H4B H 0.6067 0.7097 0.5495 0.122 Uiso 1 1 calc R . . C5 C 0.5931(10) 0.4458(6) 0.8849(9) 0.102(4) Uani 1 1 d . . . H5A H 0.6691 0.4496 0.8868 0.123 Uiso 1 1 calc R . . H5B H 0.5591 0.4122 0.9393 0.123 Uiso 1 1 calc R . . C6 C 0.5792(12) 0.4058(7) 0.8183(10) 0.126(5) Uani 1 1 d . . . H6A H 0.6307 0.3598 0.8177 0.152 Uiso 1 1 calc R . . H6B H 0.5079 0.3815 0.8311 0.152 Uiso 1 1 calc R . . C11 C 0.5129(6) 0.7719(4) 0.9892(4) 0.0450(16) Uani 1 1 d . . . C12 C 0.4968(7) 0.8031(5) 1.0621(5) 0.0565(19) Uani 1 1 d . . . H12A H 0.5553 0.8093 1.0878 0.068 Uiso 1 1 calc R . . C13 C 0.3962(7) 0.8249(5) 1.0973(5) 0.063(2) Uani 1 1 d . . . H13A H 0.3867 0.8453 1.1464 0.076 Uiso 1 1 calc R . . C14 C 0.3093(7) 0.8163(6) 1.0591(6) 0.069(2) Uani 1 1 d . . . H14A H 0.2410 0.8320 1.0818 0.082 Uiso 1 1 calc R . . C15 C 0.3238(7) 0.7846(6) 0.9877(6) 0.066(2) Uani 1 1 d . . . H15A H 0.2651 0.7783 0.9622 0.079 Uiso 1 1 calc R . . C16 C 0.4260(6) 0.7616(5) 0.9531(5) 0.0542(19) Uani 1 1 d . . . H16A H 0.4352 0.7392 0.9052 0.065 Uiso 1 1 calc R . . C21 C 0.7205(6) 0.7089(5) 1.0246(5) 0.0526(18) Uani 1 1 d . . . C22 C 0.7841(7) 0.7565(6) 1.0576(6) 0.067(2) Uani 1 1 d . . . H22A H 0.7923 0.8142 1.0341 0.080 Uiso 1 1 calc R . . C23 C 0.8348(9) 0.7184(8) 1.1248(7) 0.090(3) Uani 1 1 d . . . H23A H 0.8791 0.7500 1.1455 0.108 Uiso 1 1 calc R . . C24 C 0.8202(10) 0.6339(10) 1.1615(8) 0.107(4) Uani 1 1 d . . . H24A H 0.8519 0.6090 1.2087 0.128 Uiso 1 1 calc R . . C25 C 0.7598(10) 0.5866(8) 1.1294(8) 0.106(4) Uani 1 1 d . . . H25A H 0.7522 0.5289 1.1536 0.127 Uiso 1 1 calc R . . C26 C 0.7094(8) 0.6231(6) 1.0608(6) 0.077(3) Uani 1 1 d . . . H26A H 0.6681 0.5901 1.0391 0.092 Uiso 1 1 calc R . . C31 C 0.5165(5) 0.9402(4) 0.8149(4) 0.0427(16) Uani 1 1 d . . . C32 C 0.4423(6) 0.9252(5) 0.7674(5) 0.0519(18) Uani 1 1 d . . . H32A H 0.4630 0.8966 0.7244 0.062 Uiso 1 1 calc R . . C33 C 0.3375(7) 0.9524(6) 0.7833(5) 0.064(2) Uani 1 1 d . . . H33A H 0.2879 0.9415 0.7512 0.077 Uiso 1 1 calc R . . C34 C 0.3057(7) 0.9952(6) 0.8457(6) 0.073(3) Uani 1 1 d . . . H34A H 0.2351 1.0141 0.8552 0.088 Uiso 1 1 calc R . . C35 C 0.3778(7) 1.0102(6) 0.8941(6) 0.074(3) Uani 1 1 d . . . H35A H 0.3558 1.0378 0.9376 0.089 Uiso 1 1 calc R . . C36 C 0.4828(7) 0.9844(5) 0.8784(5) 0.059(2) Uani 1 1 d . . . H36A H 0.5320 0.9964 0.9102 0.071 Uiso 1 1 calc R . . C41 C 0.7267(6) 1.0057(4) 0.7501(5) 0.0463(17) Uani 1 1 d . . . C42 C 0.8105(7) 1.0281(5) 0.7844(6) 0.065(2) Uani 1 1 d . . . H42A H 0.8315 0.9915 0.8318 0.078 Uiso 1 1 calc R . . C43 C 0.8643(8) 1.1041(6) 0.7498(7) 0.080(3) Uani 1 1 d . . . H43A H 0.9196 1.1182 0.7749 0.096 Uiso 1 1 calc R . . C44 C 0.8372(9) 1.1570(6) 0.6809(7) 0.092(3) Uani 1 1 d . . . H44A H 0.8760 1.2064 0.6560 0.110 Uiso 1 1 calc R . . C45 C 0.7519(11) 1.1381(7) 0.6470(7) 0.113(5) Uani 1 1 d . . . H45A H 0.7303 1.1762 0.6007 0.135 Uiso 1 1 calc R . . C46 C 0.6976(9) 1.0625(6) 0.6813(6) 0.090(3) Uani 1 1 d . . . H46A H 0.6404 1.0500 0.6572 0.108 Uiso 1 1 calc R . . C51 C 0.9554(6) 0.8231(4) 0.6114(5) 0.0472(17) Uani 1 1 d . . . C52 C 1.0578(7) 0.7978(6) 0.5867(6) 0.073(3) Uani 1 1 d . . . H52A H 1.0701 0.7459 0.5721 0.087 Uiso 1 1 calc R . . C53 C 1.1438(7) 0.8495(7) 0.5835(7) 0.085(3) Uani 1 1 d . . . H53A H 1.2135 0.8318 0.5671 0.101 Uiso 1 1 calc R . . C54 C 1.1267(8) 0.9250(7) 0.6038(8) 0.091(3) Uani 1 1 d . . . H54A H 1.1848 0.9586 0.6029 0.110 Uiso 1 1 calc R . . C55 C 1.0261(10) 0.9524(8) 0.6255(11) 0.137(6) Uani 1 1 d . . . H55A H 1.0143 1.0056 0.6372 0.165 Uiso 1 1 calc R . . C56 C 0.9395(8) 0.9001(7) 0.6301(8) 0.100(4) Uani 1 1 d . . . H56A H 0.8700 0.9183 0.6462 0.120 Uiso 1 1 calc R . . C61 C 0.8359(6) 0.7679(5) 0.5010(5) 0.0532(19) Uani 1 1 d . . . C62 C 0.7992(10) 0.8430(7) 0.4584(7) 0.091(3) Uani 1 1 d . . . H62A H 0.7738 0.8846 0.4874 0.109 Uiso 1 1 calc R . . C63 C 0.7997(13) 0.8573(8) 0.3711(8) 0.126(5) Uani 1 1 d . . . H63A H 0.7766 0.9091 0.3413 0.151 Uiso 1 1 calc R . . C64 C 0.8334(12) 0.7963(10) 0.3300(8) 0.118(5) Uani 1 1 d . . . H64A H 0.8327 0.8060 0.2719 0.141 Uiso 1 1 calc R . . C65 C 0.8679(11) 0.7218(10) 0.3718(8) 0.113(4) Uani 1 1 d . . . H65A H 0.8899 0.6797 0.3428 0.135 Uiso 1 1 calc R . . C66 C 0.8711(8) 0.7069(7) 0.4582(6) 0.081(3) Uani 1 1 d . . . H66A H 0.8970 0.6556 0.4868 0.097 Uiso 1 1 calc R . . C71 C 0.9870(6) 0.6624(5) 0.7917(5) 0.0532(18) Uani 1 1 d . . . C72 C 0.9815(8) 0.7284(7) 0.8307(7) 0.094(3) Uani 1 1 d . . . H72A H 0.9148 0.7498 0.8498 0.112 Uiso 1 1 calc R . . C73 C 1.0741(12) 0.7638(9) 0.8423(9) 0.118(5) Uani 1 1 d . . . H73A H 1.0698 0.8095 0.8677 0.142 Uiso 1 1 calc R . . C74 C 1.1706(11) 0.7312(9) 0.8162(8) 0.100(4) Uani 1 1 d . . . H74A H 1.2328 0.7552 0.8236 0.121 Uiso 1 1 calc R . . C75 C 1.1787(8) 0.6640(8) 0.7793(7) 0.090(3) Uani 1 1 d . . . H75A H 1.2457 0.6415 0.7630 0.108 Uiso 1 1 calc R . . C76 C 1.0871(7) 0.6295(6) 0.7663(6) 0.072(2) Uani 1 1 d . . . H76A H 1.0924 0.5840 0.7404 0.086 Uiso 1 1 calc R . . C81 C 0.8887(6) 0.5062(5) 0.7989(7) 0.068(2) Uani 1 1 d . . . C82 C 0.8897(8) 0.4698(7) 0.8849(8) 0.095(4) Uani 1 1 d . . . H82A H 0.8846 0.5037 0.9239 0.114 Uiso 1 1 calc R . . C83 C 0.8984(11) 0.3835(9) 0.9113(11) 0.131(6) Uani 1 1 d . . . H83A H 0.9018 0.3595 0.9683 0.158 Uiso 1 1 calc R . . C84 C 0.9022(11) 0.3324(9) 0.8562(16) 0.152(9) Uani 1 1 d . . . H84A H 0.9058 0.2739 0.8758 0.182 Uiso 1 1 calc R . . C85 C 0.9007(11) 0.3667(8) 0.7730(13) 0.128(6) Uani 1 1 d . . . H85A H 0.9035 0.3316 0.7353 0.153 Uiso 1 1 calc R . . C86 C 0.8947(8) 0.4549(6) 0.7426(9) 0.092(3) Uani 1 1 d . . . H86A H 0.8949 0.4782 0.6850 0.110 Uiso 1 1 calc R . . N1 N 0.5384(7) 0.5963(5) 0.6083(5) 0.085(2) Uani 1 1 d . . . H1A H 0.5959 0.5714 0.5835 0.102 Uiso 1 1 calc R . . H1D H 0.4795 0.5705 0.6024 0.102 Uiso 1 1 calc R . . N01 N 0.4376(16) 0.3512(16) 0.6898(16) 0.240(11) Uani 1 1 d . . . N2 N 0.5919(8) 0.4611(5) 0.7361(7) 0.106(3) Uani 1 1 d . . . H2A H 0.5558 0.4391 0.7034 0.127 Uiso 1 1 calc R . . H2D H 0.6619 0.4615 0.7133 0.127 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 Sb1 0.0743(5) 0.1076(6) 0.1292(7) -0.0776(6) -0.0116(4) 0.0119(4) Sb2 0.0465(4) 0.0880(6) 0.0722(5) -0.0359(5) -0.0077(4) -0.0023(4) Sb3 0.0495(4) 0.0593(5) 0.0459(4) -0.0027(3) -0.0129(3) -0.0058(3) Ni 0.0578(6) 0.0436(6) 0.0698(7) -0.0199(5) -0.0006(5) -0.0062(5) Ag1 0.0523(3) 0.0436(3) 0.0534(3) -0.0127(3) -0.0014(3) -0.0015(2) Ag2 0.0429(3) 0.0457(3) 0.0455(3) -0.0152(2) -0.0029(2) 0.0022(2) F11 0.174(10) 0.320(16) 0.42(2) -0.312(16) -0.014(11) -0.024(10) F12 0.149(10) 0.35(2) 0.52(3) -0.23(2) -0.115(14) 0.118(12) F13 0.42(2) 0.273(16) 0.185(12) -0.077(11) 0.117(14) -0.113(17) F14 0.45(3) 0.187(12) 0.202(13) -0.042(10) 0.066(14) 0.024(14) F15 0.157(9) 0.305(16) 0.42(2) -0.218(16) -0.158(12) 0.109(10) F16 0.190(9) 0.170(8) 0.229(10) -0.140(8) -0.002(8) -0.035(7) F21 0.067(4) 0.174(7) 0.124(5) -0.056(5) -0.016(4) -0.025(4) F22 0.148(9) 0.149(9) 0.64(3) -0.189(14) -0.109(14) 0.039(7) F23 0.077(5) 0.68(3) 0.089(6) -0.021(11) -0.021(4) -0.040(10) F31 0.073(3) 0.084(3) 0.060(3) -0.001(2) -0.027(2) 0.014(3) F32 0.237(9) 0.105(5) 0.149(7) -0.065(5) -0.125(7) 0.047(6) F33 0.067(4) 0.204(8) 0.113(5) 0.050(5) -0.002(4) -0.017(4) S1 0.0503(11) 0.0430(10) 0.0679(12) -0.0138(9) -0.0120(9) -0.0064(8) S2 0.0636(13) 0.0533(12) 0.0700(14) -0.0021(10) -0.0042(11) -0.0148(10) P1 0.0469(10) 0.0397(10) 0.0454(10) -0.0118(8) -0.0053(8) -0.0010(8) P2 0.0412(10) 0.0379(9) 0.0418(10) -0.0137(8) -0.0017(8) -0.0010(7) P3 0.0399(10) 0.0480(11) 0.0504(11) -0.0221(9) 0.0006(8) -0.0031(8) P4 0.0433(10) 0.0446(11) 0.0594(12) -0.0152(9) -0.0015(9) -0.0017(8) C1 0.046(4) 0.040(4) 0.043(4) -0.011(3) -0.007(3) 0.001(3) C01 0.133(13) 0.20(2) 0.129(13) -0.091(15) -0.011(10) -0.034(15) C2 0.044(4) 0.045(4) 0.061(5) -0.021(4) -0.002(3) -0.003(3) C02 0.33(3) 0.156(19) 0.20(2) -0.047(17) -0.11(2) -0.01(2) C3 0.107(8) 0.063(6) 0.093(8) -0.001(5) -0.045(7) -0.020(6) C4 0.106(9) 0.130(11) 0.067(7) -0.009(7) -0.019(6) -0.049(8) C5 0.103(9) 0.048(6) 0.140(11) 0.022(6) -0.036(8) -0.015(5) C6 0.144(12) 0.051(7) 0.169(14) -0.002(8) -0.022(11) 0.017(7) C11 0.048(4) 0.037(4) 0.047(4) -0.008(3) -0.002(3) -0.005(3) C12 0.058(5) 0.057(5) 0.056(5) -0.019(4) -0.004(4) -0.009(4) C13 0.069(6) 0.059(5) 0.060(5) -0.022(4) 0.008(4) -0.005(4) C14 0.054(5) 0.073(6) 0.072(6) -0.016(5) 0.009(4) -0.002(4) C15 0.048(5) 0.083(6) 0.064(5) -0.009(5) -0.008(4) -0.014(4) C16 0.052(5) 0.060(5) 0.051(4) -0.013(4) -0.005(4) -0.009(4) C21 0.050(4) 0.055(5) 0.052(4) -0.012(4) -0.009(3) 0.009(4) C22 0.068(6) 0.075(6) 0.068(6) -0.025(5) -0.028(5) 0.005(4) C23 0.089(8) 0.108(9) 0.090(8) -0.036(7) -0.046(6) 0.016(6) C24 0.089(8) 0.143(12) 0.085(8) -0.005(8) -0.041(7) 0.011(8) C25 0.102(9) 0.089(8) 0.105(9) 0.029(7) -0.033(7) -0.001(7) C26 0.079(6) 0.065(6) 0.081(6) 0.004(5) -0.028(5) 0.004(5) C31 0.043(4) 0.039(4) 0.045(4) -0.010(3) -0.003(3) 0.001(3) C32 0.056(5) 0.053(4) 0.048(4) -0.016(4) -0.007(4) 0.007(4) C33 0.053(5) 0.078(6) 0.060(5) -0.015(4) -0.013(4) 0.011(4) C34 0.050(5) 0.078(6) 0.083(7) -0.012(5) 0.002(5) 0.016(4) C35 0.060(6) 0.075(6) 0.082(6) -0.030(5) 0.012(5) 0.014(5) C36 0.066(5) 0.061(5) 0.054(5) -0.027(4) -0.001(4) -0.003(4) C41 0.048(4) 0.046(4) 0.046(4) -0.016(3) -0.001(3) -0.008(3) C42 0.066(5) 0.057(5) 0.069(5) -0.007(4) -0.015(4) -0.015(4) C43 0.078(7) 0.068(6) 0.095(7) -0.018(6) -0.011(6) -0.028(5) C44 0.113(9) 0.066(6) 0.092(8) -0.010(6) -0.003(7) -0.050(6) C45 0.164(12) 0.083(8) 0.083(7) 0.025(6) -0.044(8) -0.061(8) C46 0.123(9) 0.078(7) 0.067(6) 0.012(5) -0.040(6) -0.046(6) C51 0.039(4) 0.047(4) 0.056(4) -0.018(3) 0.001(3) -0.006(3) C52 0.051(5) 0.062(5) 0.107(7) -0.036(5) 0.009(5) -0.007(4) C53 0.043(5) 0.089(7) 0.119(9) -0.033(6) 0.010(5) -0.012(5) C54 0.056(6) 0.084(7) 0.137(10) -0.041(7) 0.000(6) -0.021(5) C55 0.074(8) 0.114(10) 0.246(18) -0.112(11) 0.021(9) -0.031(7) C56 0.054(6) 0.092(8) 0.169(12) -0.078(8) 0.012(6) -0.013(5) C61 0.051(4) 0.059(5) 0.051(4) -0.018(4) -0.001(4) -0.009(4) C62 0.139(10) 0.073(7) 0.073(7) -0.031(5) -0.032(7) 0.009(6) C63 0.223(17) 0.086(8) 0.071(7) -0.010(6) -0.048(9) 0.009(9) C64 0.165(14) 0.127(11) 0.070(8) -0.038(8) -0.024(8) 0.009(10) C65 0.138(11) 0.138(12) 0.081(8) -0.066(8) -0.023(8) 0.030(9) C66 0.103(8) 0.083(7) 0.066(6) -0.036(5) -0.017(5) 0.019(6) C71 0.055(5) 0.050(4) 0.055(5) -0.009(4) -0.011(4) -0.007(4) C72 0.066(6) 0.113(9) 0.122(9) -0.068(8) -0.013(6) -0.008(6) C73 0.113(11) 0.124(11) 0.153(13) -0.087(10) -0.041(9) -0.007(8) C74 0.092(9) 0.115(10) 0.100(9) -0.017(7) -0.035(7) -0.033(8) C75 0.054(6) 0.106(9) 0.102(8) -0.005(7) -0.014(5) -0.009(6) C76 0.059(6) 0.065(6) 0.089(7) -0.018(5) -0.004(5) 0.001(4) C81 0.043(4) 0.054(5) 0.101(7) -0.012(5) -0.003(4) -0.005(4) C82 0.070(7) 0.071(7) 0.116(9) 0.019(6) 0.003(6) -0.001(5) C83 0.093(9) 0.082(9) 0.171(15) 0.051(10) -0.001(9) -0.004(8) C84 0.060(7) 0.059(9) 0.29(3) 0.030(12) 0.011(11) -0.006(6) C85 0.100(10) 0.048(7) 0.238(19) -0.049(9) -0.012(11) 0.001(6) C86 0.075(7) 0.054(6) 0.152(11) -0.042(6) -0.011(7) -0.004(5) N1 0.090(6) 0.092(6) 0.085(6) -0.049(5) -0.012(5) -0.002(5) N01 0.163(16) 0.28(3) 0.34(3) -0.19(2) -0.047(16) -0.040(17) N2 0.119(8) 0.051(5) 0.140(9) -0.035(5) 0.019(6) -0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F13 1.738(12) . ? Sb1 F15 1.758(9) . ? Sb1 F12 1.759(11) . ? Sb1 F11 1.788(8) . ? Sb1 F16 1.822(7) . ? Sb1 F14 1.834(13) . ? Sb2 F22 1.746(9) 2_757 ? Sb2 F22 1.746(9) . ? Sb2 F23 1.752(9) 2_757 ? Sb2 F23 1.752(9) . ? Sb2 F21 1.854(6) . ? Sb2 F21 1.854(6) 2_757 ? Sb3 F33 1.830(6) . ? Sb3 F33 1.830(6) 2_656 ? Sb3 F32 1.835(6) 2_656 ? Sb3 F32 1.835(6) . ? Sb3 F31 1.867(4) . ? Sb3 F31 1.867(4) 2_656 ? Ni N1 1.939(8) . ? Ni N2 1.939(8) . ? Ni S1 2.169(2) . ? Ni S2 2.171(3) . ? Ag1 P4 2.451(2) . ? Ag1 P1 2.4636(19) . ? Ag1 S2 2.518(2) . ? Ag1 Ag2 2.9495(8) . ? Ag2 P3 2.4636(19) . ? Ag2 P2 2.4981(18) . ? Ag2 S1 2.5993(19) . ? S1 C3 1.821(10) . ? S2 C5 1.835(11) . ? P1 C21 1.822(8) . ? P1 C11 1.826(7) . ? P1 C1 1.844(7) . ? P2 C31 1.823(7) . ? P2 C41 1.823(7) . ? P2 C1 1.840(7) . ? P3 C51 1.831(7) . ? P3 C61 1.833(8) . ? P3 C2 1.837(7) . ? P4 C71 1.825(8) . ? P4 C81 1.828(9) . ? P4 C2 1.831(8) . ? C01 N01 1.12(3) . ? C01 C02 1.37(2) . ? C3 C4 1.488(16) . ? C4 N1 1.476(14) . ? C5 C6 1.434(17) . ? C6 N2 1.421(15) . ? C11 C16 1.365(10) . ? C11 C12 1.386(10) . ? C12 C13 1.372(11) . ? C13 C14 1.379(12) . ? C14 C15 1.369(12) . ? C15 C16 1.393(11) . ? C21 C26 1.385(11) . ? C21 C22 1.391(11) . ? C22 C23 1.372(13) . ? C23 C24 1.370(16) . ? C24 C25 1.353(16) . ? C25 C26 1.382(14) . ? C31 C32 1.378(10) . ? C31 C36 1.399(10) . ? C32 C33 1.380(11) . ? C33 C34 1.365(12) . ? C34 C35 1.368(13) . ? C35 C36 1.374(12) . ? C41 C46 1.370(11) . ? C41 C42 1.379(11) . ? C42 C43 1.387(12) . ? C43 C44 1.333(14) . ? C44 C45 1.370(15) . ? C45 C46 1.386(13) . ? C51 C56 1.356(11) . ? C51 C52 1.364(11) . ? C52 C53 1.390(12) . ? C53 C54 1.346(13) . ? C54 C55 1.346(15) . ? C55 C56 1.397(14) . ? C61 C62 1.359(12) . ? C61 C66 1.364(11) . ? C62 C63 1.394(14) . ? C63 C64 1.341(17) . ? C64 C65 1.336(17) . ? C65 C66 1.386(14) . ? C71 C72 1.367(12) . ? C71 C76 1.388(11) . ? C72 C73 1.387(15) . ? C73 C74 1.351(17) . ? C74 C75 1.361(16) . ? C75 C76 1.377(13) . ? C81 C86 1.375(14) . ? C81 C82 1.397(14) . ? C82 C83 1.372(16) . ? C83 C84 1.36(2) . ? C84 C85 1.35(2) . ? C85 C86 1.405(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 F13 Sb1 F15 102.9(10) . . ? F13 Sb1 F12 84.3(9) . . ? F15 Sb1 F12 172.4(9) . . ? F13 Sb1 F11 94.7(7) . . ? F15 Sb1 F11 89.6(6) . . ? F12 Sb1 F11 87.3(7) . . ? F13 Sb1 F16 91.8(6) . . ? F15 Sb1 F16 88.0(5) . . ? F12 Sb1 F16 94.3(6) . . ? F11 Sb1 F16 173.5(6) . . ? F13 Sb1 F14 169.8(10) . . ? F15 Sb1 F14 85.9(8) . . ? F12 Sb1 F14 87.2(9) . . ? F11 Sb1 F14 90.5(7) . . ? F16 Sb1 F14 83.3(6) . . ? F22 Sb2 F22 180.0(14) 2_757 . ? F22 Sb2 F23 89.3(8) 2_757 2_757 ? F22 Sb2 F23 90.7(8) . 2_757 ? F22 Sb2 F23 90.7(8) 2_757 . ? F22 Sb2 F23 89.3(8) . . ? F23 Sb2 F23 180.000(2) 2_757 . ? F22 Sb2 F21 93.5(4) 2_757 . ? F22 Sb2 F21 86.5(4) . . ? F23 Sb2 F21 91.1(4) 2_757 . ? F23 Sb2 F21 88.9(4) . . ? F22 Sb2 F21 86.5(4) 2_757 2_757 ? F22 Sb2 F21 93.5(4) . 2_757 ? F23 Sb2 F21 88.9(4) 2_757 2_757 ? F23 Sb2 F21 91.1(4) . 2_757 ? F21 Sb2 F21 180.000(1) . 2_757 ? F33 Sb3 F33 180.0(6) . 2_656 ? F33 Sb3 F32 89.6(5) . 2_656 ? F33 Sb3 F32 90.4(5) 2_656 2_656 ? F33 Sb3 F32 90.4(5) . . ? F33 Sb3 F32 89.6(5) 2_656 . ? F32 Sb3 F32 180.000(1) 2_656 . ? F33 Sb3 F31 91.0(3) . . ? F33 Sb3 F31 89.0(3) 2_656 . ? F32 Sb3 F31 90.5(3) 2_656 . ? F32 Sb3 F31 89.5(3) . . ? F33 Sb3 F31 89.0(3) . 2_656 ? F33 Sb3 F31 91.0(3) 2_656 2_656 ? F32 Sb3 F31 89.5(3) 2_656 2_656 ? F32 Sb3 F31 90.5(3) . 2_656 ? F31 Sb3 F31 180.0(2) . 2_656 ? N1 Ni N2 92.4(4) . . ? N1 Ni S1 89.1(3) . . ? N2 Ni S1 177.1(3) . . ? N1 Ni S2 173.4(3) . . ? N2 Ni S2 87.7(3) . . ? S1 Ni S2 91.04(9) . . ? P4 Ag1 P1 126.32(7) . . ? P4 Ag1 S2 120.53(7) . . ? P1 Ag1 S2 110.51(7) . . ? P4 Ag1 Ag2 89.01(5) . . ? P1 Ag1 Ag2 87.12(5) . . ? S2 Ag1 Ag2 111.48(6) . . ? P3 Ag2 P2 126.56(6) . . ? P3 Ag2 S1 119.53(6) . . ? P2 Ag2 S1 113.17(6) . . ? P3 Ag2 Ag1 93.02(5) . . ? P2 Ag2 Ag1 94.57(5) . . ? S1 Ag2 Ag1 72.44(5) . . ? C3 S1 Ni 97.3(4) . . ? C3 S1 Ag2 102.7(3) . . ? Ni S1 Ag2 109.52(8) . . ? C5 S2 Ni 99.0(5) . . ? C5 S2 Ag1 105.6(4) . . ? Ni S2 Ag1 87.85(8) . . ? C21 P1 C11 103.8(3) . . ? C21 P1 C1 105.4(3) . . ? C11 P1 C1 102.7(3) . . ? C21 P1 Ag1 104.3(3) . . ? C11 P1 Ag1 123.7(2) . . ? C1 P1 Ag1 115.0(2) . . ? C31 P2 C41 102.6(3) . . ? C31 P2 C1 106.1(3) . . ? C41 P2 C1 103.3(3) . . ? C31 P2 Ag2 113.0(2) . . ? C41 P2 Ag2 120.4(2) . . ? C1 P2 Ag2 110.2(2) . . ? C51 P3 C61 102.4(3) . . ? C51 P3 C2 106.0(3) . . ? C61 P3 C2 104.2(4) . . ? C51 P3 Ag2 114.6(2) . . ? C61 P3 Ag2 117.0(3) . . ? C2 P3 Ag2 111.5(2) . . ? C71 P4 C81 102.3(4) . . ? C71 P4 C2 104.3(3) . . ? C81 P4 C2 105.6(4) . . ? C71 P4 Ag1 121.3(3) . . ? C81 P4 Ag1 109.4(3) . . ? C2 P4 Ag1 112.6(2) . . ? P2 C1 P1 111.2(4) . . ? N01 C01 C02 176(3) . . ? P4 C2 P3 112.6(4) . . ? C4 C3 S1 109.1(8) . . ? N1 C4 C3 108.3(8) . . ? C6 C5 S2 109.9(8) . . ? N2 C6 C5 114.1(10) . . ? C16 C11 C12 118.7(7) . . ? C16 C11 P1 119.7(6) . . ? C12 C11 P1 121.5(6) . . ? C13 C12 C11 121.4(8) . . ? C12 C13 C14 119.5(8) . . ? C15 C14 C13 119.8(8) . . ? C14 C15 C16 120.3(8) . . ? C11 C16 C15 120.3(8) . . ? C26 C21 C22 118.8(8) . . ? C26 C21 P1 116.8(7) . . ? C22 C21 P1 124.4(6) . . ? C23 C22 C21 120.2(9) . . ? C24 C23 C22 120.1(10) . . ? C25 C24 C23 120.4(10) . . ? C24 C25 C26 120.6(11) . . ? C25 C26 C21 119.8(10) . . ? C32 C31 C36 118.2(7) . . ? C32 C31 P2 118.2(5) . . ? C36 C31 P2 123.5(6) . . ? C31 C32 C33 120.4(7) . . ? C34 C33 C32 120.7(8) . . ? C33 C34 C35 119.9(8) . . ? C34 C35 C36 120.1(8) . . ? C35 C36 C31 120.6(8) . . ? C46 C41 C42 117.0(7) . . ? C46 C41 P2 118.2(6) . . ? C42 C41 P2 124.8(6) . . ? C41 C42 C43 121.6(9) . . ? C44 C43 C42 120.4(9) . . ? C43 C44 C45 119.5(9) . . ? C44 C45 C46 120.3(10) . . ? C41 C46 C45 121.1(9) . . ? C56 C51 C52 118.8(7) . . ? C56 C51 P3 118.6(6) . . ? C52 C51 P3 122.5(6) . . ? C51 C52 C53 120.0(8) . . ? C54 C53 C52 120.4(9) . . ? C53 C54 C55 120.4(9) . . ? C54 C55 C56 119.3(10) . . ? C51 C56 C55 120.9(9) . . ? C62 C61 C66 119.7(8) . . ? C62 C61 P3 115.1(6) . . ? C66 C61 P3 125.2(7) . . ? C61 C62 C63 119.5(10) . . ? C64 C63 C62 120.1(12) . . ? C65 C64 C63 120.7(12) . . ? C64 C65 C66 120.4(11) . . ? C61 C66 C65 119.6(10) . . ? C72 C71 C76 118.7(8) . . ? C72 C71 P4 120.4(7) . . ? C76 C71 P4 120.9(6) . . ? C71 C72 C73 120.8(10) . . ? C74 C73 C72 119.3(11) . . ? C73 C74 C75 121.3(11) . . ? C74 C75 C76 119.7(11) . . ? C75 C76 C71 120.2(9) . . ? C86 C81 C82 119.4(10) . . ? C86 C81 P4 124.1(8) . . ? C82 C81 P4 116.2(8) . . ? C83 C82 C81 119.3(14) . . ? C84 C83 C82 121.6(17) . . ? C85 C84 C83 119.7(14) . . ? C84 C85 C86 120.7(15) . . ? C81 C86 C85 119.3(13) . . ? C4 N1 Ni 115.3(6) . . ? C6 N2 Ni 117.2(8) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.978 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.110 #==END data_Ag2Pd _database_code_CSD 185410 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H59 Ag2 F12 N3 P4 Pd S2 Sb2' _chemical_formula_weight 1755.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6483(2) _cell_length_b 16.3639(3) _cell_length_c 16.4721(3) _cell_angle_alpha 76.519(1) _cell_angle_beta 80.332(1) _cell_angle_gamma 87.382(1) _cell_volume 3268.22(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7652 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 24.98 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max .42 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .7992 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 16940 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 24.98 _reflns_number_total 11332 _reflns_number_gt 8319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens 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^)+(0.0492P)^2^+14.8209P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11332 _refine_ls_number_parameters 742 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1283 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.009 _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 Sb1 Sb 0.76689(7) 0.43126(6) 0.49295(7) 0.0995(3) Uani 1 1 d . . . Sb2 Sb 1.0000 0.0000 1.0000 0.0712(3) Uani 1 2 d S . . Sb3 Sb 0.5000 0.0000 0.5000 0.0551(2) Uani 1 2 d S . . Pd Pd 0.54663(6) 0.57967(4) 0.72746(5) 0.0586(2) Uani 1 1 d . . . Ag1 Ag 0.68652(5) 0.65267(4) 0.84317(4) 0.05168(18) Uani 1 1 d . . . Ag2 Ag 0.67102(5) 0.80000(4) 0.69903(4) 0.04605(17) Uani 1 1 d . . . F11 F 0.7505(10) 0.3451(10) 0.4456(11) 0.266(9) Uani 1 1 d . . . F12 F 0.8970(11) 0.3937(14) 0.5024(17) 0.342(13) Uani 1 1 d . . . F13 F 0.828(2) 0.4971(12) 0.3978(10) 0.330(12) Uani 1 1 d . . . F14 F 0.7212(19) 0.3654(9) 0.5970(10) 0.311(11) Uani 1 1 d . . . F15 F 0.6283(9) 0.4586(10) 0.4911(12) 0.260(8) Uani 1 1 d . . . F16 F 0.7723(9) 0.5127(7) 0.5519(8) 0.181(5) Uani 1 1 d . . . F21 F 1.1344(5) 0.0319(6) 1.0133(5) 0.124(3) Uani 1 1 d . . . F22 F 1.0561(10) -0.0991(8) 0.9970(16) 0.309(12) Uani 1 1 d . . . F23 F 1.0380(8) 0.0333(14) 0.8903(6) 0.296(11) Uani 1 1 d . . . F31 F 0.5857(4) -0.0687(4) 0.5725(4) 0.0788(16) Uani 1 1 d . . . F32 F 0.4947(8) -0.0853(5) 0.4447(5) 0.138(3) Uani 1 1 d . . . F33 F 0.6201(5) 0.0425(6) 0.4251(5) 0.137(3) Uani 1 1 d . . . S1 S 0.49533(17) 0.71570(13) 0.72218(15) 0.0538(5) Uani 1 1 d . . . S2 S 0.5352(2) 0.54848(15) 0.87114(17) 0.0681(7) Uani 1 1 d . . . P1 P 0.64672(17) 0.75314(13) 0.93559(13) 0.0453(5) Uani 1 1 d . . . P2 P 0.65447(16) 0.90669(12) 0.78832(13) 0.0415(5) Uani 1 1 d . . . P3 P 0.83738(16) 0.75973(13) 0.61477(14) 0.0450(5) Uani 1 1 d . . . P4 P 0.86435(17) 0.62040(14) 0.77058(15) 0.0516(5) Uani 1 1 d . . . C1 C 0.7004(6) 0.8605(5) 0.8894(5) 0.0450(18) Uani 1 1 d . . . H1B H 0.6772 0.8960 0.9288 0.054 Uiso 1 1 calc R . . H1C H 0.7781 0.8582 0.8804 0.054 Uiso 1 1 calc R . . C01 C 0.445(2) 0.275(2) 0.6917(14) 0.159(9) Uani 1 1 d . . . C2 C 0.8753(6) 0.6500(5) 0.6547(5) 0.0486(19) Uani 1 1 d . . . H2B H 0.9486 0.6410 0.6295 0.058 Uiso 1 1 calc R . . H2C H 0.8295 0.6136 0.6371 0.058 Uiso 1 1 calc R . . C02 C 0.448(3) 0.1902(16) 0.7013(17) 0.244(14) Uani 1 1 d . . . H02A H 0.4899 0.1656 0.7447 0.366 Uiso 1 1 calc R . . H02B H 0.4810 0.1769 0.6490 0.366 Uiso 1 1 calc R . . H02C H 0.3769 0.1682 0.7170 0.366 Uiso 1 1 calc R . . C3 C 0.4550(9) 0.7367(7) 0.6175(7) 0.078(3) Uani 1 1 d . . . H3A H 0.3836 0.7150 0.6225 0.094 Uiso 1 1 calc R . . H3B H 0.4530 0.7969 0.5945 0.094 Uiso 1 1 calc R . . C4 C 0.5317(10) 0.6965(8) 0.5588(7) 0.094(4) Uani 1 1 d . . . H4A H 0.5057 0.7035 0.5054 0.113 Uiso 1 1 calc R . . H4B H 0.6011 0.7233 0.5477 0.113 Uiso 1 1 calc R . . C5 C 0.5979(10) 0.4419(6) 0.8824(9) 0.098(4) Uani 1 1 d . . . H5A H 0.6747 0.4466 0.8792 0.118 Uiso 1 1 calc R . . H5B H 0.5696 0.4072 0.9374 0.118 Uiso 1 1 calc R . . C6 C 0.5767(12) 0.4012(7) 0.8158(10) 0.111(5) Uani 1 1 d . . . H6A H 0.6218 0.3516 0.8166 0.133 Uiso 1 1 calc R . . H6B H 0.5025 0.3832 0.8280 0.133 Uiso 1 1 calc R . . C11 C 0.5120(6) 0.7730(5) 0.9877(5) 0.0443(18) Uani 1 1 d . . . C12 C 0.4962(7) 0.8054(6) 1.0600(6) 0.058(2) Uani 1 1 d . . . H12A H 0.5548 0.8128 1.0849 0.070 Uiso 1 1 calc R . . C13 C 0.3948(8) 0.8266(6) 1.0952(6) 0.069(3) Uani 1 1 d . . . H13A H 0.3853 0.8470 1.1441 0.083 Uiso 1 1 calc R . . C14 C 0.3079(8) 0.8179(6) 1.0581(6) 0.067(3) Uani 1 1 d . . . H14A H 0.2398 0.8333 1.0811 0.081 Uiso 1 1 calc R . . C15 C 0.3220(7) 0.7866(7) 0.9877(7) 0.072(3) Uani 1 1 d . . . H15A H 0.2628 0.7806 0.9629 0.086 Uiso 1 1 calc R . . C16 C 0.4234(7) 0.7631(5) 0.9516(6) 0.058(2) Uani 1 1 d . . . H16A H 0.4315 0.7410 0.9038 0.070 Uiso 1 1 calc R . . C21 C 0.7188(7) 0.7109(5) 1.0240(6) 0.054(2) Uani 1 1 d . . . C22 C 0.7827(8) 0.7577(7) 1.0561(7) 0.074(3) Uani 1 1 d . . . H22A H 0.7926 0.8148 1.0322 0.089 Uiso 1 1 calc R . . C23 C 0.8317(9) 0.7187(9) 1.1239(8) 0.093(4) Uani 1 1 d . . . H23A H 0.8758 0.7504 1.1444 0.112 Uiso 1 1 calc R . . C24 C 0.8184(10) 0.6370(10) 1.1615(8) 0.103(4) Uani 1 1 d . . . H24A H 0.8510 0.6130 1.2081 0.123 Uiso 1 1 calc R . . C25 C 0.7559(11) 0.5898(9) 1.1300(9) 0.106(4) Uani 1 1 d . . . H25A H 0.7464 0.5330 1.1551 0.127 Uiso 1 1 calc R . . C26 C 0.7060(9) 0.6262(7) 1.0602(7) 0.082(3) Uani 1 1 d . . . H26A H 0.6647 0.5935 1.0384 0.099 Uiso 1 1 calc R . . C31 C 0.5172(6) 0.9420(5) 0.8148(5) 0.0440(18) Uani 1 1 d . . . C32 C 0.4420(7) 0.9278(5) 0.7668(6) 0.055(2) Uani 1 1 d . . . H32A H 0.4625 0.9000 0.7233 0.066 Uiso 1 1 calc R . . C33 C 0.3363(7) 0.9549(6) 0.7835(7) 0.068(3) Uani 1 1 d . . . H33A H 0.2865 0.9446 0.7515 0.082 Uiso 1 1 calc R . . C34 C 0.3053(8) 0.9964(6) 0.8465(7) 0.073(3) Uani 1 1 d . . . H34A H 0.2351 1.0157 0.8565 0.088 Uiso 1 1 calc R . . C35 C 0.3784(9) 1.0096(7) 0.8952(7) 0.077(3) Uani 1 1 d . . . H35A H 0.3561 1.0362 0.9393 0.092 Uiso 1 1 calc R . . C36 C 0.4835(8) 0.9843(5) 0.8801(6) 0.060(2) Uani 1 1 d . . . H36A H 0.5322 0.9950 0.9128 0.072 Uiso 1 1 calc R . . C41 C 0.7277(7) 1.0058(5) 0.7511(5) 0.048(2) Uani 1 1 d . . . C42 C 0.8101(8) 1.0284(5) 0.7858(6) 0.064(3) Uani 1 1 d . . . H42A H 0.8299 0.9927 0.8337 0.077 Uiso 1 1 calc R . . C43 C 0.8641(9) 1.1032(7) 0.7508(8) 0.079(3) Uani 1 1 d . . . H43A H 0.9198 1.1172 0.7752 0.095 Uiso 1 1 calc R . . C44 C 0.8368(10) 1.1558(7) 0.6818(8) 0.091(4) Uani 1 1 d . . . H44A H 0.8759 1.2046 0.6568 0.110 Uiso 1 1 calc R . . C45 C 0.7522(13) 1.1377(8) 0.6485(8) 0.121(5) Uani 1 1 d . . . H45A H 0.7304 1.1761 0.6031 0.145 Uiso 1 1 calc R . . C46 C 0.6975(10) 1.0620(7) 0.6819(7) 0.092(4) Uani 1 1 d . . . H46A H 0.6408 1.0493 0.6576 0.111 Uiso 1 1 calc R . . C51 C 0.9544(6) 0.8223(5) 0.6130(5) 0.050(2) Uani 1 1 d . . . C52 C 1.0575(8) 0.7986(6) 0.5878(7) 0.077(3) Uani 1 1 d . . . H52A H 1.0702 0.7469 0.5736 0.093 Uiso 1 1 calc R . . C53 C 1.1420(8) 0.8496(8) 0.5830(8) 0.088(4) Uani 1 1 d . . . H53A H 1.2113 0.8326 0.5647 0.106 Uiso 1 1 calc R . . C54 C 1.1260(9) 0.9244(8) 0.6047(8) 0.091(4) Uani 1 1 d . . . H54A H 1.1837 0.9582 0.6035 0.110 Uiso 1 1 calc R . . C55 C 1.0236(10) 0.9492(9) 0.6283(12) 0.142(7) Uani 1 1 d . . . H55A H 1.0110 1.0008 0.6429 0.171 Uiso 1 1 calc R . . C56 C 0.9383(9) 0.8989(8) 0.6307(10) 0.109(5) Uani 1 1 d . . . H56A H 0.8687 0.9179 0.6447 0.131 Uiso 1 1 calc R . . C61 C 0.8347(7) 0.7691(6) 0.5013(5) 0.053(2) Uani 1 1 d . . . C62 C 0.8004(11) 0.8440(7) 0.4572(7) 0.091(4) Uani 1 1 d . . . H62A H 0.7769 0.8862 0.4854 0.109 Uiso 1 1 calc R . . C63 C 0.8001(15) 0.8578(9) 0.3719(9) 0.129(6) Uani 1 1 d . . . H63A H 0.7773 0.9096 0.3429 0.154 Uiso 1 1 calc R . . C64 C 0.8323(14) 0.7977(11) 0.3297(9) 0.120(5) Uani 1 1 d . . . H64A H 0.8315 0.8080 0.2718 0.144 Uiso 1 1 calc R . . C65 C 0.8656(12) 0.7228(11) 0.3707(9) 0.116(5) Uani 1 1 d . . . H65A H 0.8866 0.6809 0.3417 0.139 Uiso 1 1 calc R . . C66 C 0.8685(10) 0.7078(8) 0.4588(7) 0.087(3) Uani 1 1 d . . . H66A H 0.8933 0.6566 0.4874 0.104 Uiso 1 1 calc R . . C71 C 0.9860(7) 0.6624(6) 0.7917(6) 0.057(2) Uani 1 1 d . . . C72 C 0.9811(9) 0.7281(8) 0.8315(8) 0.091(4) Uani 1 1 d . . . H72A H 0.9145 0.7479 0.8527 0.110 Uiso 1 1 calc R . . C73 C 1.0745(13) 0.7658(10) 0.8406(10) 0.121(5) Uani 1 1 d . . . H73A H 1.0707 0.8138 0.8620 0.145 Uiso 1 1 calc R . . C74 C 1.1702(12) 0.7306(10) 0.8175(9) 0.104(4) Uani 1 1 d . . . H74A H 1.2323 0.7525 0.8273 0.125 Uiso 1 1 calc R . . C75 C 1.1783(9) 0.6634(8) 0.7800(8) 0.093(4) Uani 1 1 d . . . H75A H 1.2453 0.6408 0.7642 0.111 Uiso 1 1 calc R . . C76 C 1.0876(7) 0.6293(7) 0.7657(7) 0.076(3) Uani 1 1 d . . . H76A H 1.0933 0.5847 0.7391 0.091 Uiso 1 1 calc R . . C81 C 0.8874(7) 0.5076(6) 0.7964(7) 0.068(3) Uani 1 1 d . . . C82 C 0.8908(9) 0.4696(8) 0.8805(9) 0.098(4) Uani 1 1 d . . . H82A H 0.8876 0.5020 0.9204 0.117 Uiso 1 1 calc R . . C83 C 0.8993(11) 0.3808(11) 0.9051(13) 0.134(7) Uani 1 1 d . . . H83A H 0.9026 0.3552 0.9613 0.160 Uiso 1 1 calc R . . C84 C 0.9026(13) 0.3323(10) 0.8474(18) 0.150(10) Uani 1 1 d . . . H84A H 0.9069 0.2741 0.8641 0.180 Uiso 1 1 calc R . . C85 C 0.8996(12) 0.3694(9) 0.7678(15) 0.134(7) Uani 1 1 d . . . H85A H 0.9019 0.3361 0.7288 0.161 Uiso 1 1 calc R . . C86 C 0.8933(8) 0.4560(6) 0.7393(9) 0.089(4) Uani 1 1 d . . . H86A H 0.8930 0.4796 0.6822 0.107 Uiso 1 1 calc R . . N1 N 0.5426(7) 0.6056(6) 0.5975(6) 0.086(3) Uani 1 1 d . . . H1A H 0.6033 0.5859 0.5714 0.103 Uiso 1 1 calc R . . H1D H 0.4872 0.5780 0.5887 0.103 Uiso 1 1 calc R . . N01 N 0.439(2) 0.3474(18) 0.682(2) 0.252(13) Uani 1 1 d . . . N2 N 0.5963(8) 0.4554(5) 0.7329(7) 0.099(3) Uani 1 1 d . . . H2A H 0.5625 0.4346 0.6984 0.118 Uiso 1 1 calc R . . H2D H 0.6671 0.4550 0.7132 0.118 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 Sb1 0.0761(5) 0.1106(7) 0.1352(8) -0.0809(6) -0.0124(5) 0.0121(5) Sb2 0.0492(5) 0.0967(8) 0.0776(7) -0.0394(6) -0.0103(5) -0.0027(5) Sb3 0.0509(5) 0.0624(5) 0.0500(5) -0.0029(4) -0.0144(4) -0.0060(4) Pd 0.0577(4) 0.0460(4) 0.0741(5) -0.0202(3) -0.0064(4) -0.0038(3) Ag1 0.0526(4) 0.0447(4) 0.0564(4) -0.0132(3) -0.0026(3) -0.0020(3) Ag2 0.0433(3) 0.0473(4) 0.0488(4) -0.0159(3) -0.0045(3) 0.0017(3) F11 0.179(11) 0.309(17) 0.41(2) -0.290(18) -0.045(12) -0.004(11) F12 0.146(11) 0.41(3) 0.57(4) -0.29(3) -0.109(16) 0.120(14) F13 0.49(3) 0.269(19) 0.190(14) -0.066(13) 0.118(18) -0.09(2) F14 0.50(3) 0.190(13) 0.203(14) -0.041(11) 0.044(17) 0.058(16) F15 0.139(9) 0.291(16) 0.45(2) -0.227(17) -0.141(12) 0.089(10) F16 0.175(9) 0.172(9) 0.234(12) -0.142(9) 0.004(8) -0.031(7) F21 0.070(4) 0.185(8) 0.133(6) -0.059(6) -0.025(4) -0.030(5) F22 0.141(10) 0.168(11) 0.69(4) -0.214(18) -0.100(16) 0.028(8) F23 0.086(6) 0.66(3) 0.105(7) -0.005(13) -0.024(5) -0.058(12) F31 0.074(4) 0.087(4) 0.072(4) 0.001(3) -0.030(3) 0.010(3) F32 0.211(9) 0.098(5) 0.138(7) -0.046(5) -0.103(7) 0.036(6) F33 0.070(4) 0.199(9) 0.101(5) 0.039(5) -0.001(4) -0.007(5) S1 0.0492(12) 0.0448(12) 0.0688(14) -0.0139(10) -0.0103(10) -0.0065(9) S2 0.0613(15) 0.0559(14) 0.0791(17) -0.0017(12) -0.0039(12) -0.0152(11) P1 0.0474(12) 0.0428(11) 0.0458(12) -0.0108(9) -0.0064(9) -0.0013(9) P2 0.0440(11) 0.0381(11) 0.0434(11) -0.0130(9) -0.0034(9) -0.0035(9) P3 0.0398(11) 0.0450(12) 0.0526(13) -0.0202(10) -0.0021(9) 0.0000(9) P4 0.0432(12) 0.0471(12) 0.0635(14) -0.0141(11) -0.0039(10) -0.0002(10) C1 0.051(5) 0.040(4) 0.046(5) -0.012(4) -0.010(4) -0.001(4) C01 0.155(18) 0.21(3) 0.136(16) -0.09(2) 0.000(13) -0.03(2) C2 0.042(4) 0.046(5) 0.061(5) -0.020(4) -0.007(4) -0.001(4) C02 0.38(4) 0.18(2) 0.22(3) -0.07(2) -0.13(3) 0.03(3) C3 0.082(7) 0.064(6) 0.092(8) -0.001(6) -0.040(6) -0.015(6) C4 0.097(9) 0.114(10) 0.071(8) -0.004(7) -0.026(7) -0.033(8) C5 0.090(9) 0.046(6) 0.137(12) 0.019(7) -0.012(8) -0.004(6) C6 0.119(11) 0.051(7) 0.155(14) -0.028(8) 0.003(10) -0.002(7) C11 0.050(5) 0.037(4) 0.046(5) -0.011(3) -0.005(4) -0.003(3) C12 0.055(5) 0.062(6) 0.061(6) -0.021(5) -0.009(4) -0.005(4) C13 0.076(7) 0.064(6) 0.067(6) -0.025(5) 0.005(5) -0.004(5) C14 0.051(6) 0.075(7) 0.069(7) -0.015(5) 0.008(5) -0.001(5) C15 0.045(5) 0.091(8) 0.077(7) -0.014(6) -0.007(5) -0.007(5) C16 0.064(6) 0.051(5) 0.056(5) -0.011(4) 0.000(4) -0.008(4) C21 0.050(5) 0.054(5) 0.056(5) -0.008(4) -0.010(4) 0.000(4) C22 0.076(7) 0.072(7) 0.081(7) -0.024(6) -0.025(6) 0.009(5) C23 0.080(8) 0.120(11) 0.089(9) -0.025(8) -0.043(7) 0.014(7) C24 0.089(9) 0.140(13) 0.077(8) -0.003(8) -0.044(7) 0.014(9) C25 0.103(10) 0.093(9) 0.102(10) 0.022(8) -0.030(8) 0.016(8) C26 0.070(7) 0.088(8) 0.084(8) 0.000(6) -0.024(6) -0.007(6) C31 0.043(4) 0.033(4) 0.053(5) -0.008(4) -0.003(4) -0.004(3) C32 0.054(5) 0.056(5) 0.054(5) -0.011(4) -0.007(4) -0.003(4) C33 0.047(5) 0.078(7) 0.077(7) -0.013(6) -0.010(5) -0.002(5) C34 0.052(6) 0.076(7) 0.082(7) -0.016(6) 0.008(5) 0.020(5) C35 0.076(7) 0.075(7) 0.081(7) -0.037(6) 0.006(6) 0.015(6) C36 0.066(6) 0.052(5) 0.068(6) -0.026(5) -0.007(5) 0.002(4) C41 0.055(5) 0.042(4) 0.050(5) -0.019(4) 0.001(4) -0.008(4) C42 0.078(7) 0.046(5) 0.069(6) -0.006(4) -0.016(5) -0.021(5) C43 0.080(7) 0.072(7) 0.091(8) -0.020(6) -0.021(6) -0.019(6) C44 0.105(9) 0.076(8) 0.086(8) -0.004(7) -0.004(7) -0.047(7) C45 0.173(14) 0.095(9) 0.090(9) 0.023(7) -0.052(10) -0.063(10) C46 0.105(9) 0.078(7) 0.089(8) 0.012(6) -0.038(7) -0.045(7) C51 0.040(4) 0.048(5) 0.064(5) -0.023(4) 0.002(4) -0.008(4) C52 0.054(6) 0.063(6) 0.116(9) -0.039(6) 0.009(6) -0.003(5) C53 0.042(6) 0.102(9) 0.120(10) -0.037(8) 0.006(6) -0.016(6) C54 0.058(7) 0.093(9) 0.132(11) -0.047(8) -0.005(6) -0.026(6) C55 0.068(8) 0.108(10) 0.28(2) -0.131(13) 0.027(10) -0.022(7) C56 0.050(6) 0.096(9) 0.193(15) -0.082(10) 0.019(7) -0.017(6) C61 0.047(5) 0.072(6) 0.047(5) -0.027(5) -0.002(4) -0.008(4) C62 0.146(11) 0.070(7) 0.063(7) -0.019(6) -0.031(7) 0.012(7) C63 0.234(19) 0.084(9) 0.078(9) -0.018(8) -0.058(11) 0.014(10) C64 0.181(16) 0.123(12) 0.063(8) -0.026(9) -0.032(9) 0.006(11) C65 0.138(13) 0.144(14) 0.081(9) -0.062(10) -0.013(9) 0.008(11) C66 0.106(9) 0.092(8) 0.070(7) -0.040(6) -0.011(6) 0.020(7) C71 0.050(5) 0.064(6) 0.054(5) -0.004(4) -0.012(4) -0.003(4) C72 0.071(7) 0.121(10) 0.103(9) -0.066(8) -0.017(6) -0.003(7) C73 0.118(12) 0.124(12) 0.153(14) -0.077(11) -0.049(11) 0.003(10) C74 0.095(10) 0.120(11) 0.113(11) -0.027(9) -0.051(8) -0.026(9) C75 0.054(6) 0.107(10) 0.108(10) -0.005(8) -0.012(6) -0.013(6) C76 0.049(6) 0.074(7) 0.104(8) -0.019(6) -0.011(5) -0.007(5) C81 0.043(5) 0.051(6) 0.101(8) -0.007(6) -0.001(5) -0.002(4) C82 0.067(7) 0.086(9) 0.121(11) 0.004(8) 0.002(7) -0.001(6) C83 0.078(9) 0.094(11) 0.180(18) 0.049(11) 0.003(10) 0.001(9) C84 0.082(10) 0.050(9) 0.29(3) 0.000(13) -0.015(14) 0.006(8) C85 0.105(11) 0.058(9) 0.24(2) -0.034(11) -0.037(13) 0.004(8) C86 0.063(7) 0.054(6) 0.151(12) -0.034(7) -0.006(7) -0.001(5) N1 0.081(6) 0.108(8) 0.082(6) -0.050(6) -0.016(5) 0.007(5) N01 0.19(2) 0.27(3) 0.35(3) -0.16(3) -0.05(2) -0.02(2) N2 0.101(7) 0.056(6) 0.135(9) -0.032(6) 0.006(7) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 F12 1.750(13) . ? Sb1 F13 1.759(15) . ? Sb1 F15 1.793(10) . ? Sb1 F11 1.798(10) . ? Sb1 F14 1.815(15) . ? Sb1 F16 1.832(8) . ? Sb2 F22 1.749(11) 2_757 ? Sb2 F22 1.749(11) . ? Sb2 F23 1.751(10) . ? Sb2 F23 1.751(10) 2_757 ? Sb2 F21 1.862(6) 2_757 ? Sb2 F21 1.862(6) . ? Sb3 F33 1.839(7) . ? Sb3 F33 1.839(7) 2_656 ? Sb3 F32 1.845(7) . ? Sb3 F32 1.845(7) 2_656 ? Sb3 F31 1.888(5) . ? Sb3 F31 1.888(5) 2_656 ? Pd N2 2.086(8) . ? Pd N1 2.092(9) . ? Pd S1 2.276(2) . ? Pd S2 2.283(3) . ? Pd Ag1 3.2524(10) . ? Ag1 P4 2.460(2) . ? Ag1 P1 2.471(2) . ? Ag1 S2 2.534(2) . ? Ag1 Ag2 2.9887(9) . ? Ag2 P3 2.471(2) . ? Ag2 P2 2.513(2) . ? Ag2 S1 2.595(2) . ? S1 C3 1.832(10) . ? S2 C5 1.865(11) . ? P1 C11 1.827(8) . ? P1 C21 1.830(9) . ? P1 C1 1.854(8) . ? P2 C31 1.819(8) . ? P2 C41 1.830(8) . ? P2 C1 1.837(8) . ? P3 C51 1.831(8) . ? P3 C2 1.834(8) . ? P3 C61 1.845(8) . ? P4 C81 1.817(10) . ? P4 C71 1.829(9) . ? P4 C2 1.840(9) . ? C01 N01 1.15(3) . ? C01 C02 1.36(3) . ? C3 C4 1.494(16) . ? C4 N1 1.485(15) . ? C5 C6 1.475(18) . ? C6 N2 1.433(16) . ? C11 C16 1.385(12) . ? C11 C12 1.394(11) . ? C12 C13 1.381(13) . ? C13 C14 1.371(14) . ? C14 C15 1.356(14) . ? C15 C16 1.398(13) . ? C21 C26 1.381(13) . ? C21 C22 1.381(13) . ? C22 C23 1.379(15) . ? C23 C24 1.341(17) . ? C24 C25 1.369(18) . ? C25 C26 1.401(15) . ? C31 C32 1.394(11) . ? C31 C36 1.408(11) . ? C32 C33 1.392(12) . ? C33 C34 1.364(14) . ? C34 C35 1.375(15) . ? C35 C36 1.374(13) . ? C41 C42 1.372(12) . ? C41 C46 1.384(13) . ? C42 C43 1.384(13) . ? C43 C44 1.342(15) . ? C44 C45 1.354(17) . ? C45 C46 1.396(15) . ? C51 C56 1.350(13) . ? C51 C52 1.367(12) . ? C52 C53 1.367(14) . ? C53 C54 1.350(15) . ? C54 C55 1.361(16) . ? C55 C56 1.376(15) . ? C61 C62 1.363(13) . ? C61 C66 1.367(13) . ? C62 C63 1.370(16) . ? C63 C64 1.344(18) . ? C64 C65 1.340(19) . ? C65 C66 1.420(17) . ? C71 C72 1.378(14) . ? C71 C76 1.410(13) . ? C72 C73 1.403(17) . ? C73 C74 1.351(19) . ? C74 C75 1.375(18) . ? C75 C76 1.375(15) . ? C81 C82 1.388(16) . ? C81 C86 1.393(15) . ? C82 C83 1.419(19) . ? C83 C84 1.37(3) . ? C84 C85 1.32(3) . ? C85 C86 1.388(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 F12 Sb1 F13 84.9(11) . . ? F12 Sb1 F15 173.5(10) . . ? F13 Sb1 F15 101.1(11) . . ? F12 Sb1 F11 87.4(7) . . ? F13 Sb1 F11 94.4(8) . . ? F15 Sb1 F11 89.6(6) . . ? F12 Sb1 F14 88.4(11) . . ? F13 Sb1 F14 171.8(11) . . ? F15 Sb1 F14 85.8(9) . . ? F11 Sb1 F14 90.0(8) . . ? F12 Sb1 F16 95.0(7) . . ? F13 Sb1 F16 92.1(7) . . ? F15 Sb1 F16 87.5(5) . . ? F11 Sb1 F16 173.2(7) . . ? F14 Sb1 F16 83.7(7) . . ? F22 Sb2 F22 180.000(2) 2_757 . ? F22 Sb2 F23 89.7(10) 2_757 . ? F22 Sb2 F23 90.3(10) . . ? F22 Sb2 F23 90.3(10) 2_757 2_757 ? F22 Sb2 F23 89.7(10) . 2_757 ? F23 Sb2 F23 180.000(2) . 2_757 ? F22 Sb2 F21 87.1(5) 2_757 2_757 ? F22 Sb2 F21 92.9(5) . 2_757 ? F23 Sb2 F21 91.2(4) . 2_757 ? F23 Sb2 F21 88.8(4) 2_757 2_757 ? F22 Sb2 F21 92.9(5) 2_757 . ? F22 Sb2 F21 87.1(5) . . ? F23 Sb2 F21 88.8(4) . . ? F23 Sb2 F21 91.2(4) 2_757 . ? F21 Sb2 F21 180.000(1) 2_757 . ? F33 Sb3 F33 180.0(7) . 2_656 ? F33 Sb3 F32 90.2(5) . . ? F33 Sb3 F32 89.8(5) 2_656 . ? F33 Sb3 F32 89.8(5) . 2_656 ? F33 Sb3 F32 90.2(5) 2_656 2_656 ? F32 Sb3 F32 180.0(4) . 2_656 ? F33 Sb3 F31 90.9(3) . . ? F33 Sb3 F31 89.1(3) 2_656 . ? F32 Sb3 F31 89.8(3) . . ? F32 Sb3 F31 90.2(3) 2_656 . ? F33 Sb3 F31 89.1(3) . 2_656 ? F33 Sb3 F31 90.9(3) 2_656 2_656 ? F32 Sb3 F31 90.2(3) . 2_656 ? F32 Sb3 F31 89.8(3) 2_656 2_656 ? F31 Sb3 F31 180.0(3) . 2_656 ? N2 Pd N1 93.6(4) . . ? N2 Pd S1 178.9(3) . . ? N1 Pd S1 86.9(3) . . ? N2 Pd S2 86.7(3) . . ? N1 Pd S2 174.9(3) . . ? S1 Pd S2 92.92(9) . . ? N2 Pd Ag1 106.5(3) . . ? N1 Pd Ag1 133.6(3) . . ? S1 Pd Ag1 72.54(6) . . ? S2 Pd Ag1 50.87(6) . . ? P4 Ag1 P1 126.42(8) . . ? P4 Ag1 S2 119.91(8) . . ? P1 Ag1 S2 110.57(8) . . ? P4 Ag1 Ag2 88.91(6) . . ? P1 Ag1 Ag2 86.32(5) . . ? S2 Ag1 Ag2 113.95(7) . . ? P4 Ag1 Pd 96.80(6) . . ? P1 Ag1 Pd 133.43(6) . . ? S2 Ag1 Pd 44.34(6) . . ? Ag2 Ag1 Pd 77.12(2) . . ? P3 Ag2 P2 126.35(7) . . ? P3 Ag2 S1 121.18(7) . . ? P2 Ag2 S1 111.84(7) . . ? P3 Ag2 Ag1 92.51(6) . . ? P2 Ag2 Ag1 94.69(5) . . ? S1 Ag2 Ag1 73.71(5) . . ? C3 S1 Pd 96.6(4) . . ? C3 S1 Ag2 104.5(4) . . ? Pd S1 Ag2 106.02(9) . . ? C5 S2 Pd 97.2(5) . . ? C5 S2 Ag1 106.9(4) . . ? Pd S2 Ag1 84.78(8) . . ? C11 P1 C21 103.4(4) . . ? C11 P1 C1 102.9(4) . . ? C21 P1 C1 105.1(4) . . ? C11 P1 Ag1 123.7(3) . . ? C21 P1 Ag1 104.5(3) . . ? C1 P1 Ag1 115.4(3) . . ? C31 P2 C41 102.4(4) . . ? C31 P2 C1 106.3(4) . . ? C41 P2 C1 103.1(4) . . ? C31 P2 Ag2 113.2(3) . . ? C41 P2 Ag2 120.8(3) . . ? C1 P2 Ag2 109.8(3) . . ? C51 P3 C2 105.9(4) . . ? C51 P3 C61 102.7(4) . . ? C2 P3 C61 104.8(4) . . ? C51 P3 Ag2 114.2(3) . . ? C2 P3 Ag2 111.9(3) . . ? C61 P3 Ag2 116.3(3) . . ? C81 P4 C71 103.0(4) . . ? C81 P4 C2 105.3(5) . . ? C71 P4 C2 104.3(4) . . ? C81 P4 Ag1 109.5(3) . . ? C71 P4 Ag1 120.8(3) . . ? C2 P4 Ag1 112.5(3) . . ? P2 C1 P1 111.5(4) . . ? N01 C01 C02 178(3) . . ? P3 C2 P4 113.1(4) . . ? C4 C3 S1 110.7(8) . . ? N1 C4 C3 109.6(9) . . ? C6 C5 S2 111.4(9) . . ? N2 C6 C5 112.9(10) . . ? C16 C11 C12 118.4(8) . . ? C16 C11 P1 120.2(6) . . ? C12 C11 P1 121.2(6) . . ? C13 C12 C11 120.9(9) . . ? C14 C13 C12 120.3(9) . . ? C15 C14 C13 119.6(9) . . ? C14 C15 C16 121.4(9) . . ? C11 C16 C15 119.4(9) . . ? C26 C21 C22 119.3(9) . . ? C26 C21 P1 116.1(7) . . ? C22 C21 P1 124.6(7) . . ? C23 C22 C21 119.1(11) . . ? C24 C23 C22 122.8(12) . . ? C23 C24 C25 118.7(11) . . ? C24 C25 C26 120.7(12) . . ? C21 C26 C25 119.4(11) . . ? C32 C31 C36 118.4(8) . . ? C32 C31 P2 118.2(6) . . ? C36 C31 P2 123.4(7) . . ? C33 C32 C31 120.4(9) . . ? C34 C33 C32 120.4(9) . . ? C33 C34 C35 119.7(9) . . ? C36 C35 C34 121.4(9) . . ? C35 C36 C31 119.6(9) . . ? C42 C41 C46 117.8(8) . . ? C42 C41 P2 125.3(7) . . ? C46 C41 P2 116.9(7) . . ? C41 C42 C43 121.1(9) . . ? C44 C43 C42 120.6(10) . . ? C43 C44 C45 119.8(10) . . ? C44 C45 C46 120.6(12) . . ? C41 C46 C45 119.9(10) . . ? C56 C51 C52 117.9(8) . . ? C56 C51 P3 118.6(7) . . ? C52 C51 P3 123.2(7) . . ? C51 C52 C53 121.2(9) . . ? C54 C53 C52 120.7(10) . . ? C53 C54 C55 118.5(10) . . ? C54 C55 C56 120.7(11) . . ? C51 C56 C55 120.8(10) . . ? C62 C61 C66 118.6(9) . . ? C62 C61 P3 116.9(7) . . ? C66 C61 P3 124.4(8) . . ? C61 C62 C63 120.9(11) . . ? C64 C63 C62 121.0(13) . . ? C65 C64 C63 120.1(13) . . ? C64 C65 C66 119.8(13) . . ? C61 C66 C65 119.6(12) . . ? C72 C71 C76 118.3(9) . . ? C72 C71 P4 121.1(8) . . ? C76 C71 P4 120.6(8) . . ? C71 C72 C73 121.4(11) . . ? C74 C73 C72 118.4(13) . . ? C73 C74 C75 121.7(12) . . ? C74 C75 C76 120.2(12) . . ? C75 C76 C71 119.7(11) . . ? C82 C81 C86 117.9(11) . . ? C82 C81 P4 117.1(9) . . ? C86 C81 P4 124.8(9) . . ? C81 C82 C83 119.3(15) . . ? C84 C83 C82 121.0(18) . . ? C85 C84 C83 118.9(16) . . ? C84 C85 C86 122.9(19) . . ? C85 C86 C81 119.9(15) . . ? C4 N1 Pd 113.7(7) . . ? C6 N2 Pd 114.6(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.968 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.131 #==END