Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Garcia Fernandez, Esther' 'Fernandez, Damian' 'Garcia-Seijo, M Ines' 'Gould, Roberts O.' 'Montes, Jose A.' 'Rodriguez, Susana' _publ_contact_author_name 'Dr Esther Garcia Fernandez' _publ_contact_author_address ; Department of Inorganic Chemistry University of Santiago de Compostels Ava. del las Ciencias s/n Santiago de Compostela E-15782 SPAIN ; _publ_contact_author_email 'QIEGFQ@USC.ES' _publ_section_title ; Comparative structural studies on silver(I) complexes with tripodal polyphosphines. Crystallographic characterisation of the first infinite chain structures in 2:1 adducts of silver(I) halides with 1, 1, 1- Tris(diphenylphosphinomethyl)ethane ; data_jose_1 _database_code_CSD 173819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ag2(tripod)I2.3DMSO ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H39 Ag2 I2 P3' _chemical_formula_sum 'C47 H57 Ag2 I2 O3 P3 S3' _chemical_formula_weight 1328.56 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' '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' 'I' 'I' -0.4742 1.8119 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.926(4) _cell_length_b 19.209(5) _cell_length_c 19.642(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.190(5) _cell_angle_gamma 90.00 _cell_volume 5201(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 941 _cell_measurement_theta_min 2.365 _cell_measurement_theta_max 19.491 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5230 _exptl_absorpt_correction_T_max 0.8618 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Ag2(tripod)I2.3DMSO ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23626 _diffrn_reflns_av_R_equivalents 0.1791 _diffrn_reflns_av_sigmaI/netI 0.3021 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 23.35 _reflns_number_total 7508 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for windows' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1383P)^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 7508 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2818 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.3008 _refine_ls_wR_factor_gt 0.2137 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.298 _refine_ls_shift/su_mean 0.008 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 S1 S 0.2056(8) 0.6971(5) 0.4738(5) 0.119(3) Uiso 1 1 d . . . O1 O 0.2490(17) 0.7223(12) 0.4165(13) 0.133(8) Uiso 1 1 d . . . C100 C 0.179(3) 0.6114(17) 0.451(2) 0.145(15) Uiso 1 1 d . . . H10A H 0.2383 0.5860 0.4504 0.217 Uiso 1 1 calc R . . H10B H 0.1417 0.6101 0.4058 0.217 Uiso 1 1 calc R . . H10C H 0.1424 0.5907 0.4834 0.217 Uiso 1 1 calc R . . C101 C 0.086(2) 0.7307(16) 0.4705(17) 0.113(11) Uiso 1 1 d . . . H10D H 0.0888 0.7793 0.4818 0.169 Uiso 1 1 calc R . . H10E H 0.0527 0.7062 0.5029 0.169 Uiso 1 1 calc R . . H10F H 0.0512 0.7247 0.4250 0.169 Uiso 1 1 calc R . . S3 S 0.5733(11) 0.7950(8) 0.6938(8) 0.183(5) Uiso 1 1 d . . . O3 O 0.4875(17) 0.7659(12) 0.7250(12) 0.126(8) Uiso 1 1 d . . . C104 C 0.628(4) 0.848(3) 0.760(3) 0.23(2) Uiso 1 1 d . . . H10G H 0.5860 0.8865 0.7660 0.341 Uiso 1 1 calc R . . H10H H 0.6883 0.8659 0.7478 0.341 Uiso 1 1 calc R . . H10I H 0.6410 0.8219 0.8015 0.341 Uiso 1 1 calc R . . C105 C 0.653(3) 0.736(2) 0.689(3) 0.21(2) Uiso 1 1 d . . . H10J H 0.6289 0.7037 0.6538 0.319 Uiso 1 1 calc R . . H10K H 0.6653 0.7124 0.7326 0.319 Uiso 1 1 calc R . . H10L H 0.7113 0.7573 0.6790 0.319 Uiso 1 1 calc R . . S2 S 0.5885(17) 0.7256(12) 0.4530(12) 0.253(8) Uiso 1 1 d . . . O2 O 0.470(5) 0.695(4) 0.395(4) 0.41(3) Uiso 1 1 d . . . C102 C 0.620(12) 0.683(8) 0.498(8) 0.81(16) Uiso 1 1 d . . . H10M H 0.6420 0.6421 0.4776 1.220 Uiso 1 1 calc R . . H10N H 0.5701 0.6715 0.5251 1.220 Uiso 1 1 calc R . . H10O H 0.6739 0.7039 0.5279 1.220 Uiso 1 1 calc R . . C103 C 0.505(6) 0.788(5) 0.436(4) 0.43(6) Uiso 1 1 d . . . H10P H 0.5056 0.8041 0.3894 0.652 Uiso 1 1 calc R . . H10Q H 0.5200 0.8256 0.4671 0.652 Uiso 1 1 calc R . . H10R H 0.4425 0.7692 0.4400 0.652 Uiso 1 1 calc R . . I1 I 0.14499(13) 0.42189(9) 0.87867(9) 0.0680(6) Uani 1 1 d . . . I2 I 0.08609(14) 0.40080(10) 0.66544(10) 0.0742(7) Uani 1 1 d . . . Ag2 Ag 0.14650(17) 0.51162(11) 0.76088(12) 0.0817(8) Uani 1 1 d . . . Ag1 Ag 0.00673(15) 0.87797(14) 0.72050(13) 0.0925(9) Uani 1 1 d . . . P1 P 0.1773(4) 0.8628(3) 0.7142(3) 0.0477(17) Uani 1 1 d . . . P3 P 0.3011(5) 0.5732(3) 0.7474(3) 0.0520(18) Uani 1 1 d . . . P2 P 0.0397(5) 0.6226(4) 0.7502(4) 0.071(2) Uani 1 1 d . . . C41 C 0.1124(18) 0.6989(11) 0.7669(12) 0.058(7) Uani 1 1 d . . . H41A H 0.0705 0.7385 0.7540 0.069 Uiso 1 1 calc R . . H41B H 0.1313 0.7014 0.8163 0.069 Uiso 1 1 calc R . . C32 C 0.3170(19) 0.5056(16) 0.6262(14) 0.072(8) Uani 1 1 d . . . H32 H 0.2827 0.4704 0.6447 0.086 Uiso 1 1 calc R . . C35 C 0.4230(18) 0.6042(16) 0.5706(17) 0.069(8) Uani 1 1 d . . . H35 H 0.4585 0.6378 0.5510 0.083 Uiso 1 1 calc R . . C13 C -0.0334(18) 0.6366(19) 0.6643(16) 0.075(10) Uani 1 1 d . . . C25 C 0.4087(18) 0.5534(12) 0.8055(15) 0.061(8) Uani 1 1 d . . . C38 C 0.2932(17) 0.6670(10) 0.7651(12) 0.051(7) Uani 1 1 d . . . H38A H 0.2969 0.6720 0.8146 0.061 Uiso 1 1 calc R . . H38B H 0.3511 0.6884 0.7524 0.061 Uiso 1 1 calc R . . C31 C 0.3386(16) 0.5666(14) 0.6621(13) 0.053(7) Uani 1 1 d . . . C33 C 0.347(2) 0.4972(19) 0.5617(17) 0.088(11) Uani 1 1 d . . . H33 H 0.3275 0.4580 0.5355 0.105 Uiso 1 1 calc R . . C30 C 0.407(3) 0.5090(18) 0.8554(19) 0.113(13) Uani 1 1 d . . . H30 H 0.3496 0.4858 0.8584 0.135 Uiso 1 1 calc R . . C26 C 0.501(2) 0.5780(18) 0.795(2) 0.121(13) Uani 1 1 d . . . H26 H 0.5074 0.6010 0.7545 0.146 Uiso 1 1 calc R . . C18 C -0.036(2) 0.5852(18) 0.6173(19) 0.088(10) Uani 1 1 d . . . H18 H -0.0013 0.5446 0.6287 0.105 Uiso 1 1 calc R . . C34 C 0.402(3) 0.543(2) 0.5381(18) 0.107(13) Uani 1 1 d . . . H34 H 0.4267 0.5333 0.4978 0.128 Uiso 1 1 calc R . . C39 C 0.2424(15) 0.7855(9) 0.7508(11) 0.041(6) Uani 1 1 d . . . H39A H 0.3079 0.7890 0.7397 0.050 Uiso 1 1 calc R . . H39B H 0.2475 0.7899 0.8004 0.050 Uiso 1 1 calc R . . C37 C 0.2078(15) 0.7103(11) 0.7329(12) 0.044(6) Uani 1 1 d . . . C36 C 0.3913(19) 0.6166(16) 0.6341(15) 0.075(9) Uani 1 1 d . . . H36 H 0.4059 0.6585 0.6570 0.090 Uiso 1 1 calc R . . C40 C 0.1861(17) 0.7002(13) 0.6555(13) 0.067(8) Uani 1 1 d . . . H40A H 0.1308 0.7277 0.6375 0.101 Uiso 1 1 calc R . . H40B H 0.1726 0.6519 0.6455 0.101 Uiso 1 1 calc R . . H40C H 0.2412 0.7144 0.6347 0.101 Uiso 1 1 calc R . . C19 C -0.0452(17) 0.6348(18) 0.8148(15) 0.062(8) Uani 1 1 d . . . C20 C -0.094(3) 0.6933(16) 0.8209(16) 0.101(12) Uani 1 1 d . . . H20 H -0.0842 0.7317 0.7938 0.121 Uiso 1 1 calc R . . C24 C -0.057(3) 0.5854(19) 0.861(2) 0.120(13) Uani 1 1 d . . . H24 H -0.0224 0.5442 0.8592 0.144 Uiso 1 1 calc R . . C23 C -0.112(4) 0.591(2) 0.905(3) 0.20(3) Uani 1 1 d . . . H23 H -0.1196 0.5539 0.9337 0.234 Uiso 1 1 calc R . . C14 C -0.079(2) 0.6967(17) 0.6463(19) 0.084(10) Uani 1 1 d . . . H14 H -0.0730 0.7332 0.6778 0.101 Uiso 1 1 calc R . . C17 C -0.090(3) 0.5912(18) 0.5530(16) 0.093(11) Uani 1 1 d . . . H17 H -0.0955 0.5547 0.5215 0.112 Uiso 1 1 calc R . . C16 C -0.135(2) 0.655(2) 0.5381(16) 0.094(12) Uani 1 1 d . . . H16 H -0.1676 0.6622 0.4939 0.113 Uiso 1 1 calc R . . C28 C 0.573(3) 0.522(2) 0.894(2) 0.107(12) Uani 1 1 d . . . H28 H 0.6273 0.5068 0.9231 0.129 Uiso 1 1 calc R . . C29 C 0.484(4) 0.4945(19) 0.902(2) 0.134(16) Uani 1 1 d . . . H29 H 0.4770 0.4666 0.9401 0.161 Uiso 1 1 calc R . . C21 C -0.160(3) 0.697(2) 0.869(2) 0.126(14) Uani 1 1 d . . . H21 H -0.2033 0.7341 0.8696 0.151 Uiso 1 1 calc R . . C15 C -0.134(3) 0.707(3) 0.583(2) 0.130(17) Uani 1 1 d . . . H15 H -0.1685 0.7475 0.5719 0.155 Uiso 1 1 calc R . . C27 C 0.583(3) 0.569(2) 0.845(2) 0.134(16) Uani 1 1 d . . . H27 H 0.6405 0.5933 0.8446 0.161 Uiso 1 1 calc R . . C22 C -0.157(3) 0.646(2) 0.9110(19) 0.105(12) Uani 1 1 d . . . H22 H -0.1910 0.6499 0.9485 0.126 Uiso 1 1 calc R . . C7 C 0.2445(16) 0.9324(12) 0.7644(12) 0.049(6) Uani 1 1 d . . . C2 C 0.295(2) 0.8536(13) 0.6090(14) 0.074(9) Uani 1 1 d . . . H2 H 0.3415 0.8343 0.6421 0.089 Uiso 1 1 calc R . . C3 C 0.313(3) 0.8609(17) 0.543(2) 0.092(11) Uani 1 1 d . . . H3 H 0.3711 0.8443 0.5311 0.111 Uiso 1 1 calc R . . C1 C 0.206(2) 0.8749(14) 0.6270(17) 0.072(9) Uani 1 1 d . . . C4 C 0.248(3) 0.8918(18) 0.493(2) 0.103(13) Uani 1 1 d . . . H4 H 0.2629 0.8988 0.4487 0.124 Uiso 1 1 calc R . . C8 C 0.202(2) 0.9878(15) 0.7862(18) 0.096(12) Uani 1 1 d . . . H8 H 0.1348 0.9932 0.7748 0.115 Uiso 1 1 calc R . . C10 C 0.349(2) 1.0360(15) 0.8429(17) 0.085(10) Uani 1 1 d . . . H10 H 0.3811 1.0716 0.8687 0.102 Uiso 1 1 calc R . . C11 C 0.394(2) 0.9824(16) 0.8223(19) 0.109(13) Uani 1 1 d . . . H11 H 0.4612 0.9801 0.8338 0.131 Uiso 1 1 calc R . . C12 C 0.347(2) 0.9289(14) 0.7840(17) 0.094(11) Uani 1 1 d . . . H12 H 0.3818 0.8909 0.7711 0.113 Uiso 1 1 calc R . . C5 C 0.163(3) 0.9116(17) 0.5100(17) 0.098(11) Uani 1 1 d . . . H5 H 0.1166 0.9307 0.4767 0.118 Uiso 1 1 calc R . . C6 C 0.143(2) 0.9039(15) 0.5788(14) 0.080(10) Uani 1 1 d . . . H6 H 0.0838 0.9195 0.5899 0.096 Uiso 1 1 calc R . . C9 C 0.254(3) 1.0370(16) 0.825(2) 0.151(19) Uani 1 1 d . . . H9 H 0.2204 1.0743 0.8406 0.181 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 I1 0.0649(12) 0.0725(13) 0.0647(12) 0.0085(10) 0.0023(10) -0.0105(11) I2 0.0704(14) 0.0809(14) 0.0716(13) -0.0192(11) 0.0117(11) -0.0162(11) Ag2 0.0947(18) 0.0744(16) 0.0767(17) -0.0024(13) 0.0142(14) -0.0327(14) Ag1 0.0450(14) 0.141(2) 0.0908(19) -0.0104(16) 0.0068(13) 0.0139(14) P1 0.034(4) 0.053(4) 0.056(4) 0.007(3) 0.006(3) 0.001(3) P3 0.040(4) 0.047(4) 0.068(5) 0.004(4) 0.005(4) 0.001(3) P2 0.055(5) 0.074(5) 0.083(6) 0.003(4) 0.007(4) -0.003(4) C41 0.09(2) 0.040(15) 0.048(16) -0.008(12) 0.008(15) -0.032(14) C32 0.07(2) 0.10(2) 0.057(19) -0.015(17) 0.026(16) 0.020(18) C35 0.037(16) 0.08(2) 0.10(3) 0.015(19) 0.020(17) 0.010(17) C13 0.038(17) 0.11(3) 0.08(2) 0.00(2) 0.012(16) 0.062(18) C25 0.041(17) 0.037(16) 0.11(2) 0.025(16) 0.014(16) 0.015(13) C38 0.063(17) 0.033(14) 0.058(17) 0.029(12) 0.012(14) 0.010(13) C31 0.023(14) 0.069(18) 0.073(19) -0.017(16) 0.025(14) 0.008(14) C33 0.037(19) 0.14(3) 0.08(3) -0.05(2) 0.000(17) 0.01(2) C30 0.09(3) 0.10(3) 0.13(3) 0.05(3) -0.04(2) -0.01(2) C26 0.06(2) 0.13(3) 0.17(4) 0.04(3) 0.01(3) 0.00(2) C18 0.08(2) 0.10(3) 0.10(3) 0.04(2) 0.04(2) 0.01(2) C34 0.07(3) 0.17(4) 0.09(3) -0.01(3) 0.05(2) 0.04(3) C39 0.043(14) 0.023(13) 0.056(16) 0.008(11) -0.001(13) 0.009(11) C37 0.032(14) 0.037(14) 0.060(17) -0.005(13) 0.002(13) -0.005(12) C36 0.043(17) 0.12(3) 0.06(2) 0.000(19) 0.000(16) -0.005(18) C40 0.054(17) 0.069(19) 0.07(2) 0.001(15) -0.031(15) 0.005(15) C19 0.039(16) 0.07(2) 0.08(2) -0.012(19) 0.019(15) 0.022(16) C20 0.16(3) 0.06(2) 0.10(3) -0.019(19) 0.08(3) -0.05(2) C24 0.16(4) 0.09(3) 0.12(3) 0.02(3) 0.06(3) 0.03(3) C23 0.27(6) 0.09(3) 0.29(7) -0.04(4) 0.24(6) -0.02(3) C14 0.08(2) 0.08(2) 0.10(3) -0.05(2) 0.04(2) -0.02(2) C17 0.13(3) 0.09(3) 0.05(2) 0.010(19) -0.02(2) 0.02(2) C16 0.06(2) 0.18(4) 0.03(2) 0.01(2) -0.011(17) -0.02(3) C28 0.12(4) 0.08(3) 0.11(3) 0.00(2) -0.02(3) 0.03(3) C29 0.12(4) 0.10(3) 0.18(5) 0.04(3) 0.00(4) -0.02(3) C21 0.11(3) 0.12(4) 0.14(4) 0.01(3) 0.02(3) 0.06(3) C15 0.12(3) 0.21(5) 0.06(3) 0.05(3) 0.03(3) 0.06(3) C27 0.08(3) 0.17(4) 0.13(4) 0.03(3) -0.05(3) -0.06(3) C22 0.11(3) 0.13(4) 0.10(3) -0.02(3) 0.07(3) -0.02(3) C7 0.028(15) 0.047(16) 0.066(17) -0.003(13) -0.009(13) -0.008(13) C2 0.13(3) 0.053(18) 0.042(18) 0.000(14) 0.023(19) -0.034(19) C3 0.10(3) 0.10(3) 0.09(3) -0.03(2) 0.02(2) -0.03(2) C1 0.06(2) 0.054(18) 0.11(3) -0.009(18) 0.05(2) -0.025(16) C4 0.15(4) 0.09(3) 0.09(3) 0.00(2) 0.05(3) -0.05(3) C8 0.037(17) 0.06(2) 0.18(4) -0.06(2) 0.01(2) -0.008(16) C10 0.05(2) 0.06(2) 0.14(3) -0.03(2) 0.01(2) -0.006(17) C11 0.06(2) 0.06(2) 0.20(4) -0.04(2) 0.01(2) -0.034(19) C12 0.08(2) 0.059(19) 0.15(3) -0.06(2) 0.01(2) -0.018(18) C5 0.10(3) 0.13(3) 0.06(2) 0.01(2) 0.00(2) -0.01(2) C6 0.09(2) 0.10(2) 0.039(18) 0.021(16) -0.021(17) 0.027(19) C9 0.06(2) 0.07(2) 0.30(6) -0.09(3) -0.03(3) 0.02(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 S1 O1 1.43(2) . ? S1 C100 1.73(3) . ? S1 C101 1.78(3) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 H10D 0.9600 . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? S3 O3 1.52(2) . ? S3 C105 1.59(4) . ? S3 C104 1.74(5) . ? C104 H10G 0.9600 . ? C104 H10H 0.9600 . ? C104 H10I 0.9600 . ? C105 H10J 0.9600 . ? C105 H10K 0.9600 . ? C105 H10L 0.9600 . ? S2 C102 1.24(15) . ? S2 C103 1.66(8) . ? S2 O2 1.95(7) . ? C102 H10M 0.9600 . ? C102 H10N 0.9600 . ? C102 H10O 0.9600 . ? C103 H10P 0.9600 . ? C103 H10Q 0.9600 . ? C103 H10R 0.9600 . ? I1 Ag1 2.792(3) 2_546 ? I1 Ag2 2.888(3) . ? I2 Ag1 2.776(3) 2_546 ? I2 Ag2 2.882(3) . ? Ag2 P3 2.504(7) . ? Ag2 P2 2.591(8) . ? Ag2 Ag1 3.391(3) 2_546 ? Ag1 P1 2.413(6) . ? Ag1 I2 2.776(3) 2_556 ? Ag1 I1 2.792(3) 2_556 ? P1 C1 1.83(3) . ? P1 C39 1.832(19) . ? P1 C7 1.84(2) . ? P3 C25 1.79(3) . ? P3 C31 1.83(2) . ? P3 C38 1.84(2) . ? P2 C41 1.79(2) . ? P2 C13 1.86(3) . ? P2 C19 1.87(3) . ? C41 C37 1.58(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C32 C31 1.38(3) . ? C32 C33 1.40(4) . ? C32 H32 0.9300 . ? C35 C34 1.36(4) . ? C35 C36 1.40(4) . ? C35 H35 0.9300 . ? C13 C14 1.34(4) . ? C13 C18 1.35(4) . ? C25 C30 1.30(4) . ? C25 C26 1.41(4) . ? C38 C37 1.51(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C31 C36 1.37(3) . ? C33 C34 1.29(4) . ? C33 H33 0.9300 . ? C30 C29 1.33(4) . ? C30 H30 0.9300 . ? C26 C27 1.41(4) . ? C26 H26 0.9300 . ? C18 C17 1.38(4) . ? C18 H18 0.9300 . ? C34 H34 0.9300 . ? C39 C37 1.55(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C37 C40 1.52(3) . ? C36 H36 0.9300 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C19 C20 1.33(4) . ? C19 C24 1.33(4) . ? C20 C21 1.41(4) . ? C20 H20 0.9300 . ? C24 C23 1.24(4) . ? C24 H24 0.9300 . ? C23 C22 1.24(5) . ? C23 H23 0.9300 . ? C14 C15 1.38(4) . ? C14 H14 0.9300 . ? C17 C16 1.39(4) . ? C17 H17 0.9300 . ? C16 C15 1.32(5) . ? C16 H16 0.9300 . ? C28 C27 1.34(4) . ? C28 C29 1.37(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C21 C22 1.29(4) . ? C21 H21 0.9300 . ? C15 H15 0.9300 . ? C27 H27 0.9300 . ? C22 H22 0.9300 . ? C7 C8 1.32(3) . ? C7 C12 1.43(3) . ? C2 C3 1.37(4) . ? C2 C1 1.39(4) . ? C2 H2 0.9300 . ? C3 C4 1.37(4) . ? C3 H3 0.9300 . ? C1 C6 1.32(3) . ? C4 C5 1.33(4) . ? C4 H4 0.9300 . ? C8 C9 1.36(4) . ? C8 H8 0.9300 . ? C10 C9 1.31(4) . ? C10 C11 1.30(3) . ? C10 H10 0.9300 . ? C11 C12 1.38(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C5 C6 1.43(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C9 H9 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 O1 S1 C100 102.4(17) . . ? O1 S1 C101 110.2(16) . . ? C100 S1 C101 99.8(17) . . ? S1 C100 H10A 109.5 . . ? S1 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? S1 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? S1 C101 H10D 109.5 . . ? S1 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? S1 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? O3 S3 C105 111(2) . . ? O3 S3 C104 102(2) . . ? C105 S3 C104 103(3) . . ? S3 C104 H10G 109.5 . . ? S3 C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? S3 C104 H10I 109.4 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? S3 C105 H10J 109.5 . . ? S3 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? S3 C105 H10L 109.4 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? C102 S2 C103 142(8) . . ? C102 S2 O2 114(8) . . ? C103 S2 O2 66(3) . . ? S2 C102 H10M 108.3 . . ? S2 C102 H10N 109.7 . . ? H10M C102 H10N 109.5 . . ? S2 C102 H10O 110.4 . . ? H10M C102 H10O 109.5 . . ? H10N C102 H10O 109.5 . . ? S2 C103 H10P 109.7 . . ? S2 C103 H10Q 108.7 . . ? H10P C103 H10Q 109.5 . . ? S2 C103 H10R 110.0 . . ? H10P C103 H10R 109.5 . . ? H10Q C103 H10R 109.5 . . ? Ag1 I1 Ag2 73.30(8) 2_546 . ? Ag1 I2 Ag2 73.63(8) 2_546 . ? P3 Ag2 P2 95.5(2) . . ? P3 Ag2 I2 117.14(18) . . ? P2 Ag2 I2 116.4(2) . . ? P3 Ag2 I1 118.12(18) . . ? P2 Ag2 I1 119.1(2) . . ? I2 Ag2 I1 92.60(8) . . ? P3 Ag2 Ag1 158.90(18) . 2_546 ? P2 Ag2 Ag1 105.58(18) . 2_546 ? I2 Ag2 Ag1 51.76(7) . 2_546 ? I1 Ag2 Ag1 52.06(6) . 2_546 ? P1 Ag1 I2 129.42(19) . 2_556 ? P1 Ag1 I1 130.78(19) . 2_556 ? I2 Ag1 I1 97.02(9) 2_556 2_556 ? C1 P1 C39 107.8(13) . . ? C1 P1 C7 104.3(11) . . ? C39 P1 C7 101.1(11) . . ? C1 P1 Ag1 112.6(11) . . ? C39 P1 Ag1 120.9(7) . . ? C7 P1 Ag1 108.3(8) . . ? C25 P3 C31 104.3(12) . . ? C25 P3 C38 98.9(11) . . ? C31 P3 C38 105.9(12) . . ? C25 P3 Ag2 119.1(9) . . ? C31 P3 Ag2 115.2(9) . . ? C38 P3 Ag2 111.5(8) . . ? C41 P2 C13 105.7(14) . . ? C41 P2 C19 99.7(13) . . ? C13 P2 C19 106.3(12) . . ? C41 P2 Ag2 110.9(9) . . ? C13 P2 Ag2 115.2(11) . . ? C19 P2 Ag2 117.4(11) . . ? C37 C41 P2 121.6(16) . . ? C37 C41 H41A 106.9 . . ? P2 C41 H41A 106.9 . . ? C37 C41 H41B 106.9 . . ? P2 C41 H41B 106.9 . . ? H41A C41 H41B 106.7 . . ? C31 C32 C33 119(3) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C35 C36 119(3) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C14 C13 C18 119(3) . . ? C14 C13 P2 123(3) . . ? C18 C13 P2 118(2) . . ? C30 C25 C26 116(3) . . ? C30 C25 P3 121(2) . . ? C26 C25 P3 122(2) . . ? C37 C38 P3 121.5(17) . . ? C37 C38 H38A 106.9 . . ? P3 C38 H38A 106.9 . . ? C37 C38 H38B 106.9 . . ? P3 C38 H38B 106.9 . . ? H38A C38 H38B 106.7 . . ? C36 C31 C32 119(2) . . ? C36 C31 P3 124(2) . . ? C32 C31 P3 117(2) . . ? C34 C33 C32 121(3) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C25 C30 C29 124(4) . . ? C25 C30 H30 117.9 . . ? C29 C30 H30 117.9 . . ? C25 C26 C27 122(3) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C13 C18 C17 122(3) . . ? C13 C18 H18 119.1 . . ? C17 C18 H18 119.2 . . ? C33 C34 C35 122(3) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C37 C39 P1 123.1(15) . . ? C37 C39 H39A 106.6 . . ? P1 C39 H39A 106.5 . . ? C37 C39 H39B 106.5 . . ? P1 C39 H39B 106.5 . . ? H39A C39 H39B 106.5 . . ? C40 C37 C38 112.4(19) . . ? C40 C37 C39 111.0(19) . . ? C38 C37 C39 102.5(17) . . ? C40 C37 C41 110.2(19) . . ? C38 C37 C41 113.8(19) . . ? C39 C37 C41 106.6(17) . . ? C31 C36 C35 119(3) . . ? C31 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C20 C19 C24 115(3) . . ? C20 C19 P2 123(3) . . ? C24 C19 P2 121(3) . . ? C19 C20 C21 120(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C23 C24 C19 124(4) . . ? C23 C24 H24 118.1 . . ? C19 C24 H24 118.1 . . ? C22 C23 C24 121(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.4 . . ? C13 C14 C15 122(3) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.8 . . ? C18 C17 C16 116(3) . . ? C18 C17 H17 122.1 . . ? C16 C17 H17 122.1 . . ? C15 C16 C17 124(3) . . ? C15 C16 H16 118.0 . . ? C17 C16 H16 118.0 . . ? C27 C28 C29 122(4) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C30 C29 C28 119(4) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C22 C21 C20 115(3) . . ? C22 C21 H21 122.4 . . ? C20 C21 H21 122.4 . . ? C16 C15 C14 117(4) . . ? C16 C15 H15 121.6 . . ? C14 C15 H15 121.6 . . ? C28 C27 C26 115(3) . . ? C28 C27 H27 122.5 . . ? C26 C27 H27 122.5 . . ? C23 C22 C21 124(4) . . ? C23 C22 H22 118.2 . . ? C21 C22 H22 118.1 . . ? C8 C7 C12 116(2) . . ? C8 C7 P1 123(2) . . ? C12 C7 P1 122(2) . . ? C3 C2 C1 120(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 122(3) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C6 C1 C2 118(3) . . ? C6 C1 P1 120(2) . . ? C2 C1 P1 122(3) . . ? C5 C4 C3 117(3) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.2 . . ? C7 C8 C9 121(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C9 C10 C11 116(3) . . ? C9 C10 H10 121.8 . . ? C11 C10 H10 121.8 . . ? C10 C11 C12 123(3) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.7 . . ? C11 C12 C7 119(3) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C4 C5 C6 121(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 121(3) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C10 C9 C8 125(3) . . ? C10 C9 H9 117.4 . . ? C8 C9 H9 117.4 . . ? 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 Ag1 I2 Ag2 P3 158.6(2) 2_546 . . . ? Ag1 I2 Ag2 P2 -89.5(2) 2_546 . . . ? Ag1 I2 Ag2 I1 34.97(8) 2_546 . . . ? Ag1 I1 Ag2 P3 -157.6(2) 2_546 . . . ? Ag1 I1 Ag2 P2 87.5(2) 2_546 . . . ? Ag1 I1 Ag2 I2 -34.80(8) 2_546 . . . ? I2 Ag1 P1 C1 -163.0(9) 2_556 . . . ? I1 Ag1 P1 C1 -6.4(10) 2_556 . . . ? I2 Ag1 P1 C39 67.5(9) 2_556 . . . ? I1 Ag1 P1 C39 -135.8(8) 2_556 . . . ? I2 Ag1 P1 C7 -48.3(9) 2_556 . . . ? I1 Ag1 P1 C7 108.3(8) 2_556 . . . ? P2 Ag2 P3 C25 133.5(10) . . . . ? I2 Ag2 P3 C25 -103.1(10) . . . . ? I1 Ag2 P3 C25 6.3(10) . . . . ? Ag1 Ag2 P3 C25 -50.3(12) 2_546 . . . ? P2 Ag2 P3 C31 -101.4(9) . . . . ? I2 Ag2 P3 C31 22.0(9) . . . . ? I1 Ag2 P3 C31 131.4(9) . . . . ? Ag1 Ag2 P3 C31 74.9(10) 2_546 . . . ? P2 Ag2 P3 C38 19.3(8) . . . . ? I2 Ag2 P3 C38 142.7(8) . . . . ? I1 Ag2 P3 C38 -107.9(8) . . . . ? Ag1 Ag2 P3 C38 -164.4(8) 2_546 . . . ? P3 Ag2 P2 C41 -19.5(9) . . . . ? I2 Ag2 P2 C41 -143.5(8) . . . . ? I1 Ag2 P2 C41 107.0(9) . . . . ? Ag1 Ag2 P2 C41 161.9(8) 2_546 . . . ? P3 Ag2 P2 C13 100.4(11) . . . . ? I2 Ag2 P2 C13 -23.6(11) . . . . ? I1 Ag2 P2 C13 -133.1(11) . . . . ? Ag1 Ag2 P2 C13 -78.2(11) 2_546 . . . ? P3 Ag2 P2 C19 -133.2(10) . . . . ? I2 Ag2 P2 C19 102.8(10) . . . . ? I1 Ag2 P2 C19 -6.7(11) . . . . ? Ag1 Ag2 P2 C19 48.2(10) 2_546 . . . ? C13 P2 C41 C37 -79(2) . . . . ? C19 P2 C41 C37 171(2) . . . . ? Ag2 P2 C41 C37 47(2) . . . . ? C41 P2 C13 C14 -45(3) . . . . ? C19 P2 C13 C14 60(3) . . . . ? Ag2 P2 C13 C14 -168(2) . . . . ? C41 P2 C13 C18 131(3) . . . . ? C19 P2 C13 C18 -123(2) . . . . ? Ag2 P2 C13 C18 9(3) . . . . ? C31 P3 C25 C30 -132(3) . . . . ? C38 P3 C25 C30 119(3) . . . . ? Ag2 P3 C25 C30 -2(3) . . . . ? C31 P3 C25 C26 40(3) . . . . ? C38 P3 C25 C26 -69(3) . . . . ? Ag2 P3 C25 C26 171(2) . . . . ? C25 P3 C38 C37 -174.9(19) . . . . ? C31 P3 C38 C37 77(2) . . . . ? Ag2 P3 C38 C37 -48.7(19) . . . . ? C33 C32 C31 C36 -2(4) . . . . ? C33 C32 C31 P3 -177.8(19) . . . . ? C25 P3 C31 C36 -77(2) . . . . ? C38 P3 C31 C36 27(2) . . . . ? Ag2 P3 C31 C36 150.5(19) . . . . ? C25 P3 C31 C32 99(2) . . . . ? C38 P3 C31 C32 -157.2(19) . . . . ? Ag2 P3 C31 C32 -34(2) . . . . ? C31 C32 C33 C34 6(4) . . . . ? C26 C25 C30 C29 11(6) . . . . ? P3 C25 C30 C29 -177(3) . . . . ? C30 C25 C26 C27 -15(5) . . . . ? P3 C25 C26 C27 173(3) . . . . ? C14 C13 C18 C17 -4(5) . . . . ? P2 C13 C18 C17 179(2) . . . . ? C32 C33 C34 C35 -8(5) . . . . ? C36 C35 C34 C33 5(5) . . . . ? C1 P1 C39 C37 -79(2) . . . . ? C7 P1 C39 C37 172.4(18) . . . . ? Ag1 P1 C39 C37 53(2) . . . . ? P3 C38 C37 C40 -50(2) . . . . ? P3 C38 C37 C39 -169.4(15) . . . . ? P3 C38 C37 C41 76(2) . . . . ? P1 C39 C37 C40 50(2) . . . . ? P1 C39 C37 C38 170.3(16) . . . . ? P1 C39 C37 C41 -70(2) . . . . ? P2 C41 C37 C40 52(3) . . . . ? P2 C41 C37 C38 -76(2) . . . . ? P2 C41 C37 C39 172.1(16) . . . . ? C32 C31 C36 C35 -1(4) . . . . ? P3 C31 C36 C35 174.9(19) . . . . ? C34 C35 C36 C31 0(4) . . . . ? C41 P2 C19 C20 51(3) . . . . ? C13 P2 C19 C20 -59(3) . . . . ? Ag2 P2 C19 C20 170(2) . . . . ? C41 P2 C19 C24 -126(3) . . . . ? C13 P2 C19 C24 124(3) . . . . ? Ag2 P2 C19 C24 -6(3) . . . . ? C24 C19 C20 C21 -6(5) . . . . ? P2 C19 C20 C21 177(3) . . . . ? C20 C19 C24 C23 2(6) . . . . ? P2 C19 C24 C23 179(4) . . . . ? C19 C24 C23 C22 -3(9) . . . . ? C18 C13 C14 C15 4(5) . . . . ? P2 C13 C14 C15 -179(3) . . . . ? C13 C18 C17 C16 4(5) . . . . ? C18 C17 C16 C15 -5(5) . . . . ? C25 C30 C29 C28 -8(7) . . . . ? C27 C28 C29 C30 8(6) . . . . ? C19 C20 C21 C22 11(6) . . . . ? C17 C16 C15 C14 5(6) . . . . ? C13 C14 C15 C16 -4(5) . . . . ? C29 C28 C27 C26 -12(6) . . . . ? C25 C26 C27 C28 15(6) . . . . ? C24 C23 C22 C21 8(9) . . . . ? C20 C21 C22 C23 -11(7) . . . . ? C1 P1 C7 C8 107(3) . . . . ? C39 P1 C7 C8 -141(3) . . . . ? Ag1 P1 C7 C8 -13(3) . . . . ? C1 P1 C7 C12 -75(3) . . . . ? C39 P1 C7 C12 37(2) . . . . ? Ag1 P1 C7 C12 165(2) . . . . ? C1 C2 C3 C4 3(4) . . . . ? C3 C2 C1 C6 -2(4) . . . . ? C3 C2 C1 P1 178(2) . . . . ? C39 P1 C1 C6 150(2) . . . . ? C7 P1 C1 C6 -103(2) . . . . ? Ag1 P1 C1 C6 14(3) . . . . ? C39 P1 C1 C2 -29(2) . . . . ? C7 P1 C1 C2 77(2) . . . . ? Ag1 P1 C1 C2 -165.4(18) . . . . ? C2 C3 C4 C5 -4(5) . . . . ? C12 C7 C8 C9 0(5) . . . . ? P1 C7 C8 C9 178(3) . . . . ? C9 C10 C11 C12 0(6) . . . . ? C10 C11 C12 C7 2(5) . . . . ? C8 C7 C12 C11 -1(4) . . . . ? P1 C7 C12 C11 -180(2) . . . . ? C3 C4 C5 C6 3(5) . . . . ? C2 C1 C6 C5 1(4) . . . . ? P1 C1 C6 C5 -178(2) . . . . ? C4 C5 C6 C1 -2(5) . . . . ? C11 C10 C9 C8 -2(7) . . . . ? C7 C8 C9 C10 2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.256 _refine_diff_density_min -1.891 _refine_diff_density_rms 0.189 data_agin01 _database_code_CSD 173820 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Ag Cl N P3' _chemical_formula_weight 797.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.895(4) _cell_length_b 10.339(4) _cell_length_c 10.809(4) _cell_angle_alpha 74.50(2) _cell_angle_beta 80.92(2) _cell_angle_gamma 79.66(2) _cell_volume 936.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 0.769 _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 'Stoe Stadi-4' _diffrn_measurement_method '\w\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8884 _diffrn_reflns_av_R_equivalents 0.0102 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6564 _reflns_number_gt 6498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _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^)+(0.0328P)^2^+0.1370P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(10) _refine_ls_number_reflns 6564 _refine_ls_number_parameters 433 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.005 _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 Ag1 Ag 0.113001(8) 0.063138(8) 0.477246(8) 0.02169(5) Uani 1 1 d . . . Cl1 Cl 0.34457(6) -0.09464(6) 0.58189(6) 0.03232(14) Uani 1 1 d . . . N1 N -0.1831(2) 0.25385(18) 0.38308(17) 0.0203(4) Uani 1 1 d . . . C14 C -0.2957(2) 0.0528(2) 0.5260(2) 0.0230(4) Uani 1 1 d . . . H14A H -0.3809 0.0025 0.5364 0.028 Uiso 1 1 calc R . . H14B H -0.3063 0.0915 0.5998 0.028 Uiso 1 1 calc R . . C24 C -0.0381(2) 0.2208(2) 0.1734(2) 0.0254(4) Uani 1 1 d . . . H24A H -0.0205 0.2673 0.0829 0.031 Uiso 1 1 calc R . . H24B H -0.0913 0.1450 0.1790 0.031 Uiso 1 1 calc R . . C34 C -0.0843(3) 0.4031(2) 0.4890(2) 0.0243(4) Uani 1 1 d . . . H34A H -0.1181 0.4721 0.5371 0.029 Uiso 1 1 calc R . . H34B H -0.0264 0.4436 0.4083 0.029 Uiso 1 1 calc R . . C41 C -0.3035(2) 0.1680(2) 0.4017(2) 0.0243(4) Uani 1 1 d . . . H41A H -0.2931 0.1290 0.3280 0.029 Uiso 1 1 calc R . . H41B H -0.4034 0.2237 0.4056 0.029 Uiso 1 1 calc R . . C42 C -0.1414(2) 0.3182(2) 0.2460(2) 0.0234(4) Uani 1 1 d . . . H42A H -0.0886 0.3944 0.2401 0.028 Uiso 1 1 calc R . . H42B H -0.2346 0.3532 0.2047 0.028 Uiso 1 1 calc R . . C43 C -0.2247(2) 0.3552(2) 0.4600(2) 0.0235(4) Uani 1 1 d . . . H43A H -0.2834 0.3165 0.5409 0.028 Uiso 1 1 calc R . . H43B H -0.2899 0.4327 0.4135 0.028 Uiso 1 1 calc R . . P1 P -0.11373(6) -0.06420(5) 0.52264(5) 0.01865(11) Uani 1 1 d . . . C11A C -0.1390(3) -0.1939(2) 0.6744(2) 0.0201(5) Uani 1 1 d . . . C12A C -0.2786(3) -0.2429(2) 0.7237(2) 0.0257(5) Uani 1 1 d . . . H12A H -0.3642 -0.2102 0.6789 0.031 Uiso 1 1 calc R . . C13A C -0.2886(3) -0.3411(2) 0.8402(2) 0.0303(5) Uani 1 1 d . . . H13A H -0.3815 -0.3737 0.8729 0.036 Uiso 1 1 calc R . . C14A C -0.1637(3) -0.3902(2) 0.9073(2) 0.0307(6) Uani 1 1 d . . . H14C H -0.1723 -0.4556 0.9851 0.037 Uiso 1 1 calc R . . C15A C -0.0247(3) -0.3429(2) 0.8598(2) 0.0339(5) Uani 1 1 d . . . H15A H 0.0601 -0.3760 0.9056 0.041 Uiso 1 1 calc R . . C16A C -0.0124(3) -0.2448(2) 0.7423(2) 0.0263(5) Uani 1 1 d . . . H16A H 0.0812 -0.2136 0.7096 0.032 Uiso 1 1 calc R . . C11B C -0.1306(3) -0.1550(2) 0.4022(2) 0.0260(5) Uani 1 1 d . . . C12B C 0.0022(4) -0.1884(3) 0.3227(3) 0.0373(7) Uani 1 1 d . . . H12B H 0.0952 -0.1649 0.3317 0.045 Uiso 1 1 calc R . . C13B C -0.0052(5) -0.2574(3) 0.2293(3) 0.0577(9) Uani 1 1 d . . . H13B H 0.0826 -0.2786 0.1750 0.069 Uiso 1 1 calc R . . C14B C -0.1431(6) -0.2939(3) 0.2181(3) 0.0620(10) Uani 1 1 d . . . H14D H -0.1478 -0.3396 0.1559 0.074 Uiso 1 1 calc R . . C15B C -0.2747(5) -0.2634(3) 0.2982(3) 0.0534(8) Uani 1 1 d . . . H15B H -0.3664 -0.2906 0.2911 0.064 Uiso 1 1 calc R . . C16B C -0.2697(3) -0.1922(3) 0.3891(3) 0.0381(6) Uani 1 1 d . . . H16B H -0.3587 -0.1692 0.4413 0.046 Uiso 1 1 calc R . . P2 P 0.14958(6) 0.15480(5) 0.23594(5) 0.02242(11) Uani 1 1 d . . . C21A C 0.2434(3) 0.0526(2) 0.1226(2) 0.0271(5) Uani 1 1 d . . . C22A C 0.1807(3) 0.0469(3) 0.0155(2) 0.0412(6) Uani 1 1 d . . . H22A H 0.0845 0.0959 -0.0010 0.049 Uiso 1 1 calc R . . C23A C 0.2587(4) -0.0309(3) -0.0681(3) 0.0467(7) Uani 1 1 d . . . H23A H 0.2135 -0.0361 -0.1382 0.056 Uiso 1 1 calc R . . C24A C 0.4022(3) -0.0997(3) -0.0465(3) 0.0450(7) Uani 1 1 d . . . H24C H 0.4571 -0.1479 -0.1046 0.054 Uiso 1 1 calc R . . C25A C 0.4654(3) -0.0977(3) 0.0609(3) 0.0485(8) Uani 1 1 d . . . H25A H 0.5619 -0.1467 0.0762 0.058 Uiso 1 1 calc R . . C26A C 0.3859(3) -0.0227(3) 0.1477(3) 0.0383(6) Uani 1 1 d . . . H26A H 0.4282 -0.0233 0.2213 0.046 Uiso 1 1 calc R . . C21B C 0.2501(2) 0.3040(2) 0.1833(2) 0.0249(5) Uani 1 1 d . . . C22B C 0.3053(3) 0.3478(3) 0.2755(2) 0.0298(6) Uani 1 1 d . . . H22B H 0.2938 0.2993 0.3614 0.036 Uiso 1 1 calc R . . C23B C 0.3777(3) 0.4629(3) 0.2423(3) 0.0391(6) Uani 1 1 d . . . H23B H 0.4135 0.4916 0.3054 0.047 Uiso 1 1 calc R . . C24B C 0.3957(3) 0.5342(3) 0.1138(3) 0.0377(6) Uani 1 1 d . . . H24D H 0.4439 0.6114 0.0905 0.045 Uiso 1 1 calc R . . C25B C 0.3431(3) 0.4918(3) 0.0211(3) 0.0369(6) Uani 1 1 d . . . H25B H 0.3558 0.5406 -0.0647 0.044 Uiso 1 1 calc R . . C26B C 0.2711(3) 0.3767(3) 0.0536(2) 0.0324(5) Uani 1 1 d . . . H26B H 0.2370 0.3480 -0.0103 0.039 Uiso 1 1 calc R . . P3 P 0.04127(6) 0.26204(5) 0.58306(5) 0.02088(11) Uani 1 1 d . . . C31A C -0.0800(2) 0.2217(2) 0.7388(2) 0.0241(4) Uani 1 1 d . . . C32A C -0.1612(3) 0.3210(2) 0.7992(2) 0.0286(5) Uani 1 1 d . . . H32A H -0.1496 0.4116 0.7638 0.034 Uiso 1 1 calc R . . C33A C -0.2597(3) 0.2848(3) 0.9121(2) 0.0349(6) Uani 1 1 d . . . H33A H -0.3142 0.3515 0.9516 0.042 Uiso 1 1 calc R . . C34A C -0.2771(3) 0.1518(3) 0.9657(2) 0.0434(6) Uani 1 1 d . . . H34C H -0.3437 0.1285 1.0410 0.052 Uiso 1 1 calc R . . C35A C -0.1953(4) 0.0517(3) 0.9077(3) 0.0453(7) Uani 1 1 d . . . H35A H -0.2063 -0.0388 0.9443 0.054 Uiso 1 1 calc R . . C36A C -0.0968(3) 0.0873(3) 0.7946(2) 0.0329(5) Uani 1 1 d . . . H36A H -0.0417 0.0201 0.7560 0.039 Uiso 1 1 calc R . . C31B C 0.1893(3) 0.3444(3) 0.6177(2) 0.0262(5) Uani 1 1 d . . . C32B C 0.3139(3) 0.2576(3) 0.6744(2) 0.0322(5) Uani 1 1 d . . . H32B H 0.3178 0.1641 0.6908 0.039 Uiso 1 1 calc R . . C33B C 0.4318(3) 0.3110(3) 0.7062(3) 0.0396(6) Uani 1 1 d . . . H33B H 0.5122 0.2534 0.7467 0.047 Uiso 1 1 calc R . . C34B C 0.4286(3) 0.4499(3) 0.6771(3) 0.0419(7) Uani 1 1 d . . . H34D H 0.5077 0.4853 0.6978 0.050 Uiso 1 1 calc R . . C35B C 0.3103(3) 0.5362(3) 0.6182(3) 0.0489(7) Uani 1 1 d . . . H35B H 0.3106 0.6294 0.5973 0.059 Uiso 1 1 calc R . . C36B C 0.1893(3) 0.4836(3) 0.5898(3) 0.0403(6) Uani 1 1 d . . . H36B H 0.1079 0.5424 0.5519 0.048 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 Ag1 0.01952(7) 0.02248(7) 0.02142(7) -0.00245(5) -0.00160(5) -0.00393(5) Cl1 0.0189(3) 0.0277(3) 0.0485(4) -0.0031(3) -0.0102(2) -0.0028(2) N1 0.0180(9) 0.0207(9) 0.0207(9) -0.0015(7) -0.0012(7) -0.0050(7) C14 0.0187(10) 0.0220(10) 0.0275(11) -0.0029(9) -0.0020(8) -0.0057(8) C24 0.0250(11) 0.0313(12) 0.0195(10) -0.0044(9) -0.0034(8) -0.0049(9) C34 0.0295(11) 0.0179(10) 0.0248(10) -0.0038(8) -0.0042(8) -0.0031(8) C41 0.0175(10) 0.0258(11) 0.0280(11) -0.0028(9) -0.0051(8) -0.0028(8) C42 0.0235(10) 0.0234(10) 0.0199(10) 0.0018(8) -0.0056(8) -0.0025(8) C43 0.0223(10) 0.0208(10) 0.0241(10) -0.0035(8) -0.0023(8) 0.0016(8) P1 0.0166(2) 0.0194(3) 0.0188(3) -0.0023(2) -0.00123(19) -0.00417(19) C11A 0.0237(12) 0.0193(10) 0.0173(10) -0.0067(8) 0.0000(9) -0.0020(9) C12A 0.0210(10) 0.0250(11) 0.0276(11) -0.0015(9) 0.0006(8) -0.0051(8) C13A 0.0329(12) 0.0253(11) 0.0279(12) -0.0031(9) 0.0103(9) -0.0089(9) C14A 0.0520(16) 0.0226(12) 0.0168(12) -0.0010(9) -0.0048(11) -0.0090(11) C15A 0.0397(13) 0.0291(13) 0.0313(12) 0.0012(10) -0.0139(11) -0.0053(10) C16A 0.0254(11) 0.0206(11) 0.0306(12) -0.0005(9) -0.0066(10) -0.0036(9) C11B 0.0372(12) 0.0202(10) 0.0195(10) -0.0019(8) -0.0056(9) -0.0039(9) C12B 0.0506(17) 0.0255(13) 0.0314(14) -0.0065(11) 0.0045(12) -0.0024(12) C13B 0.097(3) 0.0350(15) 0.0321(15) -0.0123(12) 0.0090(16) 0.0051(16) C14B 0.126(3) 0.0323(15) 0.0334(16) -0.0101(12) -0.0264(19) -0.0080(18) C15B 0.084(2) 0.0412(16) 0.0445(17) -0.0092(14) -0.0331(17) -0.0123(16) C16B 0.0491(15) 0.0333(13) 0.0366(14) -0.0079(11) -0.0178(11) -0.0080(11) P2 0.0207(3) 0.0247(3) 0.0190(3) -0.0011(2) -0.0006(2) -0.0038(2) C21A 0.0276(12) 0.0217(11) 0.0259(12) -0.0005(9) 0.0052(9) -0.0030(9) C22A 0.0443(15) 0.0457(15) 0.0290(13) -0.0116(11) -0.0049(11) 0.0097(12) C23A 0.0657(19) 0.0405(15) 0.0292(13) -0.0115(11) -0.0007(12) 0.0047(14) C24A 0.0553(17) 0.0306(13) 0.0380(15) -0.0064(11) 0.0196(13) -0.0026(12) C25A 0.0372(15) 0.0330(15) 0.066(2) -0.0110(14) 0.0099(14) 0.0034(12) C26A 0.0314(14) 0.0334(14) 0.0463(15) -0.0054(12) -0.0020(11) -0.0035(11) C21B 0.0188(10) 0.0264(12) 0.0238(11) 0.0008(9) 0.0012(8) -0.0026(9) C22B 0.0266(13) 0.0340(14) 0.0249(12) 0.0014(10) 0.0011(10) -0.0105(10) C23B 0.0362(13) 0.0457(15) 0.0397(14) -0.0132(12) 0.0003(11) -0.0169(11) C24B 0.0327(13) 0.0311(13) 0.0442(16) 0.0007(12) 0.0023(11) -0.0123(11) C25B 0.0320(13) 0.0393(15) 0.0303(13) 0.0054(11) 0.0023(11) -0.0078(11) C26B 0.0294(12) 0.0376(13) 0.0264(12) -0.0002(10) -0.0004(9) -0.0087(10) P3 0.0221(3) 0.0188(3) 0.0221(3) -0.0047(2) -0.0038(2) -0.0033(2) C31A 0.0248(11) 0.0266(11) 0.0225(10) -0.0063(9) -0.0062(8) -0.0049(9) C32A 0.0284(12) 0.0311(12) 0.0278(11) -0.0087(9) -0.0051(9) -0.0045(9) C33A 0.0308(13) 0.0479(16) 0.0296(12) -0.0172(12) -0.0014(10) -0.0051(12) C34A 0.0494(16) 0.0618(17) 0.0245(13) -0.0129(12) 0.0060(11) -0.0281(14) C35A 0.069(2) 0.0394(15) 0.0302(13) -0.0041(11) -0.0004(13) -0.0255(14) C36A 0.0446(15) 0.0278(13) 0.0273(12) -0.0062(10) -0.0052(11) -0.0078(11) C31B 0.0247(12) 0.0293(13) 0.0254(12) -0.0100(10) 0.0017(9) -0.0051(10) C32B 0.0276(12) 0.0364(13) 0.0330(13) -0.0079(10) -0.0029(10) -0.0067(10) C33B 0.0271(12) 0.0601(17) 0.0369(14) -0.0176(12) -0.0046(10) -0.0109(11) C34B 0.0262(13) 0.0603(19) 0.0534(18) -0.0372(15) 0.0018(12) -0.0133(13) C35B 0.0437(16) 0.0406(15) 0.075(2) -0.0331(15) 0.0018(14) -0.0169(13) C36B 0.0338(13) 0.0307(13) 0.0615(17) -0.0184(12) -0.0084(12) -0.0045(10) _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 Ag1 P2 2.5158(10) . ? Ag1 P1 2.5174(10) . ? Ag1 P3 2.5494(10) . ? Ag1 Cl1 2.5935(11) . ? N1 C41 1.467(3) . ? N1 C43 1.468(3) . ? N1 C42 1.471(3) . ? C14 C41 1.540(3) . ? C14 P1 1.840(2) . ? C24 C42 1.529(3) . ? C24 P2 1.847(2) . ? C34 C43 1.527(3) . ? C34 P3 1.841(2) . ? P1 C11A 1.832(2) . ? P1 C11B 1.834(2) . ? C11A C16A 1.388(3) . ? C11A C12A 1.398(3) . ? C12A C13A 1.392(3) . ? C13A C14A 1.368(4) . ? C14A C15A 1.384(4) . ? C15A C16A 1.400(3) . ? C11B C12B 1.394(4) . ? C11B C16B 1.398(4) . ? C12B C13B 1.398(4) . ? C13B C14B 1.378(6) . ? C14B C15B 1.383(6) . ? C15B C16B 1.385(4) . ? P2 C21A 1.834(2) . ? P2 C21B 1.836(2) . ? C21A C22A 1.381(4) . ? C21A C26A 1.388(4) . ? C22A C23A 1.391(4) . ? C23A C24A 1.367(4) . ? C24A C25A 1.374(5) . ? C25A C26A 1.401(4) . ? C21B C22B 1.384(4) . ? C21B C26B 1.404(3) . ? C22B C23B 1.390(4) . ? C23B C24B 1.387(4) . ? C24B C25B 1.368(4) . ? C25B C26B 1.389(4) . ? P3 C31B 1.824(3) . ? P3 C31A 1.840(2) . ? C31A C36A 1.385(3) . ? C31A C32A 1.394(3) . ? C32A C33A 1.391(3) . ? C33A C34A 1.368(4) . ? C34A C35A 1.388(4) . ? C35A C36A 1.391(4) . ? C31B C36B 1.389(4) . ? C31B C32B 1.405(4) . ? C32B C33B 1.395(4) . ? C33B C34B 1.382(4) . ? C34B C35B 1.370(5) . ? C35B C36B 1.397(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 P2 Ag1 P1 105.63(3) . . ? P2 Ag1 P3 108.66(3) . . ? P1 Ag1 P3 108.16(3) . . ? P2 Ag1 Cl1 116.76(3) . . ? P1 Ag1 Cl1 109.32(3) . . ? P3 Ag1 Cl1 108.03(3) . . ? C41 N1 C43 111.87(17) . . ? C41 N1 C42 112.46(17) . . ? C43 N1 C42 111.10(17) . . ? C41 C14 P1 112.04(14) . . ? C42 C24 P2 113.55(15) . . ? C43 C34 P3 111.51(15) . . ? N1 C41 C14 112.50(17) . . ? N1 C42 C24 112.88(17) . . ? N1 C43 C34 112.65(17) . . ? C11A P1 C11B 102.14(10) . . ? C11A P1 C14 103.03(10) . . ? C11B P1 C14 103.67(11) . . ? C11A P1 Ag1 119.49(8) . . ? C11B P1 Ag1 115.85(8) . . ? C14 P1 Ag1 110.78(7) . . ? C16A C11A C12A 119.3(2) . . ? C16A C11A P1 117.62(17) . . ? C12A C11A P1 123.12(18) . . ? C13A C12A C11A 119.6(2) . . ? C14A C13A C12A 120.9(2) . . ? C13A C14A C15A 120.3(2) . . ? C14A C15A C16A 119.5(2) . . ? C11A C16A C15A 120.4(2) . . ? C12B C11B C16B 119.8(2) . . ? C12B C11B P1 117.7(2) . . ? C16B C11B P1 122.48(18) . . ? C11B C12B C13B 119.7(3) . . ? C14B C13B C12B 119.7(3) . . ? C13B C14B C15B 120.9(3) . . ? C14B C15B C16B 119.9(3) . . ? C15B C16B C11B 119.9(3) . . ? C21A P2 C21B 102.32(11) . . ? C21A P2 C24 101.33(11) . . ? C21B P2 C24 102.55(11) . . ? C21A P2 Ag1 123.75(8) . . ? C21B P2 Ag1 113.78(8) . . ? C24 P2 Ag1 110.52(7) . . ? C22A C21A C26A 119.0(2) . . ? C22A C21A P2 123.91(19) . . ? C26A C21A P2 117.1(2) . . ? C21A C22A C23A 121.2(3) . . ? C24A C23A C22A 119.6(3) . . ? C23A C24A C25A 120.1(2) . . ? C24A C25A C26A 120.7(3) . . ? C21A C26A C25A 119.3(3) . . ? C22B C21B C26B 118.7(2) . . ? C22B C21B P2 118.67(17) . . ? C26B C21B P2 122.65(19) . . ? C21B C22B C23B 121.4(2) . . ? C24B C23B C22B 119.0(3) . . ? C25B C24B C23B 120.5(2) . . ? C24B C25B C26B 120.8(2) . . ? C25B C26B C21B 119.7(2) . . ? C31B P3 C31A 103.45(11) . . ? C31B P3 C34 103.72(11) . . ? C31A P3 C34 101.39(10) . . ? C31B P3 Ag1 120.99(8) . . ? C31A P3 Ag1 113.10(8) . . ? C34 P3 Ag1 111.99(8) . . ? C36A C31A C32A 119.0(2) . . ? C36A C31A P3 118.12(17) . . ? C32A C31A P3 122.84(17) . . ? C33A C32A C31A 120.1(2) . . ? C34A C33A C32A 120.6(3) . . ? C33A C34A C35A 120.0(2) . . ? C34A C35A C36A 119.8(3) . . ? C31A C36A C35A 120.6(2) . . ? C36B C31B C32B 118.6(2) . . ? C36B C31B P3 125.4(2) . . ? C32B C31B P3 116.0(2) . . ? C33B C32B C31B 120.3(3) . . ? C34B C33B C32B 119.7(3) . . ? C35B C34B C33B 120.8(2) . . ? C34B C35B C36B 119.8(3) . . ? C31B C36B C35B 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.368 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.043 data_jose_2 _database_code_CSD 173821 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ag(tripod)Cl.2DMF ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H53 Ag2 Cl2 N2 O2 P3' _chemical_formula_weight 1057.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 18.060(3) _cell_length_b 14.866(3) _cell_length_c 18.468(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.862(4) _cell_angle_gamma 90.00 _cell_volume 4769.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 905 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 27.08 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 1.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7983 _exptl_absorpt_correction_T_max 0.8821 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Ag(tripod)Cl.2DMF ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28519 _diffrn_reflns_av_R_equivalents 0.1558 _diffrn_reflns_av_sigmaI/netI 0.3282 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.08 _reflns_number_total 9827 _reflns_number_gt 2820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0291P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9827 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2436 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.811 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C13 C 0.1893(6) 0.2185(6) 0.1617(6) 0.040(3) Uani 1 1 d . . . C30 C 0.1952(6) 0.6483(6) 0.1515(5) 0.043(3) Uani 1 1 d . . . H30 H 0.2384 0.6626 0.1904 0.052 Uiso 1 1 calc R . . C40 C 0.3205(5) 0.3258(5) 0.2445(4) 0.036(3) Uani 1 1 d . . . H40A H 0.3082 0.2895 0.2833 0.044 Uiso 1 1 calc R . . H40B H 0.3759 0.3225 0.2528 0.044 Uiso 1 1 calc R . . C16 C 0.0580(8) 0.1279(8) 0.1592(8) 0.078(4) Uani 1 1 d . . . H16 H 0.0134 0.0961 0.1580 0.094 Uiso 1 1 calc R . . C38 C 0.2154(5) 0.4386(5) 0.2474(5) 0.034(3) Uani 1 1 d . . . H38A H 0.1887 0.4141 0.1986 0.041 Uiso 1 1 calc R . . H38B H 0.2065 0.5030 0.2449 0.041 Uiso 1 1 calc R . . C15 C 0.1225(8) 0.1128(8) 0.2176(7) 0.073(4) Uani 1 1 d . . . H15 H 0.1211 0.0733 0.2562 0.088 Uiso 1 1 calc R . . C41 C 0.3441(5) 0.4449(6) 0.3423(4) 0.041(3) Uani 1 1 d . . . H41A H 0.3320 0.5050 0.3541 0.062 Uiso 1 1 calc R . . H41B H 0.3986 0.4396 0.3496 0.062 Uiso 1 1 calc R . . H41C H 0.3280 0.4032 0.3747 0.062 Uiso 1 1 calc R . . C37 C 0.3014(5) 0.4235(6) 0.2587(5) 0.030(2) Uani 1 1 d . . . C29 C 0.1312(7) 0.6951(7) 0.1459(6) 0.053(3) Uani 1 1 d . . . H29 H 0.1304 0.7410 0.1799 0.063 Uiso 1 1 calc R . . C14 C 0.1893(6) 0.1572(7) 0.2178(6) 0.055(3) Uani 1 1 d . . . H14 H 0.2343 0.1461 0.2557 0.066 Uiso 1 1 calc R . . C19 C 0.3342(6) 0.1689(6) 0.1587(6) 0.038(3) Uani 1 1 d . . . C18 C 0.1240(6) 0.2349(7) 0.1040(5) 0.050(3) Uani 1 1 d . . . H18 H 0.1249 0.2765 0.0666 0.060 Uiso 1 1 calc R . . C2 C 0.1456(6) 0.4553(7) 0.4511(5) 0.064(4) Uani 1 1 d . . . H2 H 0.1350 0.3951 0.4576 0.077 Uiso 1 1 calc R . . C6 C 0.1841(6) 0.5686(6) 0.3798(6) 0.049(3) Uani 1 1 d . . . H6 H 0.1987 0.5881 0.3379 0.059 Uiso 1 1 calc R . . C1 C 0.1671(5) 0.4814(7) 0.3856(5) 0.041(3) Uani 1 1 d . . . C39 C 0.3282(5) 0.4938(6) 0.2086(4) 0.035(2) Uani 1 1 d . . . H39A H 0.3817 0.4801 0.2130 0.042 Uiso 1 1 calc R . . H39B H 0.3278 0.5515 0.2330 0.042 Uiso 1 1 calc R . . C20 C 0.3835(6) 0.1339(7) 0.2251(6) 0.058(3) Uani 1 1 d . . . H20 H 0.3921 0.1654 0.2701 0.070 Uiso 1 1 calc R . . C24 C 0.3243(6) 0.1181(8) 0.0926(6) 0.071(4) Uani 1 1 d . . . H24 H 0.2919 0.1406 0.0482 0.085 Uiso 1 1 calc R . . C10 C -0.0760(7) 0.3817(9) 0.1691(7) 0.067(4) Uani 1 1 d . . . H10 H -0.1267 0.3782 0.1395 0.081 Uiso 1 1 calc R . . C26 C 0.1343(6) 0.5589(7) 0.0462(6) 0.052(3) Uani 1 1 d . . . H26 H 0.1343 0.5131 0.0119 0.063 Uiso 1 1 calc R . . C9 C -0.0454(7) 0.3098(8) 0.2141(7) 0.070(4) Uani 1 1 d . . . H9 H -0.0748 0.2582 0.2132 0.083 Uiso 1 1 calc R . . C27 C 0.0684(7) 0.6069(7) 0.0413(6) 0.067(4) Uani 1 1 d . . . H27 H 0.0239 0.5926 0.0040 0.081 Uiso 1 1 calc R . . C5 C 0.1802(7) 0.6315(8) 0.4365(7) 0.074(4) Uani 1 1 d . . . H5 H 0.1936 0.6912 0.4318 0.089 Uiso 1 1 calc R . . C3 C 0.1400(7) 0.5172(9) 0.5055(6) 0.083(4) Uani 1 1 d . . . H3 H 0.1247 0.4991 0.5474 0.099 Uiso 1 1 calc R . . C17 C 0.0566(7) 0.1882(8) 0.1024(7) 0.075(4) Uani 1 1 d . . . H17 H 0.0119 0.1975 0.0639 0.091 Uiso 1 1 calc R . . C11 C -0.0363(8) 0.4558(9) 0.1664(7) 0.075(4) Uani 1 1 d . . . H11 H -0.0574 0.5032 0.1345 0.090 Uiso 1 1 calc R . . C12 C 0.0383(7) 0.4600(7) 0.2132(6) 0.051(3) Uani 1 1 d . . . H12 H 0.0665 0.5123 0.2132 0.061 Uiso 1 1 calc R . . C7 C 0.0731(6) 0.3890(7) 0.2606(5) 0.039(3) Uani 1 1 d . . . C32 C 0.4191(6) 0.5637(7) 0.0839(5) 0.053(3) Uani 1 1 d . . . H32 H 0.4309 0.5029 0.0912 0.063 Uiso 1 1 calc R . . C28 C 0.0668(7) 0.6751(7) 0.0898(7) 0.066(4) Uani 1 1 d . . . H28 H 0.0219 0.7080 0.0846 0.079 Uiso 1 1 calc R . . C33 C 0.4724(7) 0.6221(10) 0.0725(6) 0.086(4) Uani 1 1 d . . . H33 H 0.5207 0.6003 0.0729 0.103 Uiso 1 1 calc R . . C21 C 0.4193(6) 0.0519(7) 0.2228(7) 0.065(4) Uani 1 1 d . . . H21 H 0.4528 0.0286 0.2663 0.078 Uiso 1 1 calc R . . C22 C 0.4051(8) 0.0037(8) 0.1548(8) 0.084(4) Uani 1 1 d . . . H22 H 0.4274 -0.0527 0.1546 0.101 Uiso 1 1 calc R . . C4 C 0.1575(8) 0.6060(9) 0.4963(7) 0.084(5) Uani 1 1 d . . . H4 H 0.1535 0.6484 0.5321 0.101 Uiso 1 1 calc R . . C23 C 0.3597(8) 0.0375(8) 0.0898(7) 0.086(5) Uani 1 1 d . . . H23 H 0.3527 0.0068 0.0446 0.103 Uiso 1 1 calc R . . C25 C 0.2013(6) 0.5788(6) 0.1025(5) 0.034(3) Uani 1 1 d . . . C35 C 0.3882(8) 0.7450(8) 0.0576(6) 0.069(4) Uani 1 1 d . . . H35 H 0.3767 0.8055 0.0478 0.083 Uiso 1 1 calc R . . C36 C 0.3341(6) 0.6856(7) 0.0700(5) 0.057(3) Uani 1 1 d . . . H36 H 0.2856 0.7078 0.0683 0.068 Uiso 1 1 calc R . . C34 C 0.4579(7) 0.7117(10) 0.0604(7) 0.083(5) Uani 1 1 d . . . H34 H 0.4965 0.7498 0.0541 0.100 Uiso 1 1 calc R . . N2 N 0.5283(5) 0.2474(6) 0.1632(5) 0.065(3) Uiso 1 1 d . . . N1 N 0.7196(5) 0.3943(6) 0.1819(5) 0.067(3) Uiso 1 1 d . . . O1 O 0.7332(5) 0.2456(6) 0.1829(4) 0.096(3) Uiso 1 1 d . . . O2 O 0.4719(5) 0.3746(6) 0.1766(4) 0.102(3) Uiso 1 1 d . . . C102 C 0.7126(7) 0.3164(8) 0.1490(7) 0.083(4) Uiso 1 1 d . . . H102 H 0.6909 0.3140 0.0972 0.100 Uiso 1 1 calc R . . C101 C 0.7501(7) 0.4068(8) 0.2639(6) 0.097(4) Uiso 1 1 d . . . H10A H 0.7369 0.3556 0.2895 0.146 Uiso 1 1 calc R . . H10B H 0.7280 0.4600 0.2790 0.146 Uiso 1 1 calc R . . H10C H 0.8050 0.4130 0.2767 0.146 Uiso 1 1 calc R . . C105 C 0.5688(7) 0.2421(8) 0.2435(6) 0.100(4) Uiso 1 1 d . . . H10D H 0.6229 0.2515 0.2503 0.150 Uiso 1 1 calc R . . H10E H 0.5607 0.1838 0.2624 0.150 Uiso 1 1 calc R . . H10F H 0.5493 0.2875 0.2703 0.150 Uiso 1 1 calc R . . C104 C 0.5366(7) 0.1717(7) 0.1147(6) 0.097(4) Uiso 1 1 d . . . H10G H 0.4980 0.1761 0.0674 0.146 Uiso 1 1 calc R . . H10H H 0.5305 0.1161 0.1388 0.146 Uiso 1 1 calc R . . H10I H 0.5868 0.1736 0.1063 0.146 Uiso 1 1 calc R . . C100 C 0.6935(7) 0.4729(8) 0.1330(7) 0.116(5) Uiso 1 1 d . . . H10J H 0.7367 0.5111 0.1342 0.174 Uiso 1 1 calc R . . H10K H 0.6561 0.5058 0.1507 0.174 Uiso 1 1 calc R . . H10L H 0.6707 0.4531 0.0824 0.174 Uiso 1 1 calc R . . C103 C 0.4820(7) 0.3105(8) 0.1350(7) 0.090(4) Uiso 1 1 d . . . H103 H 0.4555 0.3097 0.0842 0.108 Uiso 1 1 calc R . . Ag2 Ag 0.26425(5) 0.36775(5) 0.03972(4) 0.0427(2) Uani 1 1 d . . . Ag1 Ag 0.21370(5) 0.25644(5) 0.38015(4) 0.0505(3) Uani 1 1 d . . . P3 P 0.28197(15) 0.51365(16) 0.10542(13) 0.0332(7) Uani 1 1 d . . . P1 P 0.16915(16) 0.39243(17) 0.31684(14) 0.0385(7) Uani 1 1 d . . . P2 P 0.27558(15) 0.26945(17) 0.15221(14) 0.0369(7) Uani 1 1 d . . . Cl1 Cl 0.13698(15) 0.35536(17) -0.06977(13) 0.0517(7) Uani 1 1 d . . . Cl2 Cl 0.33943(15) 0.31113(16) -0.05590(14) 0.0506(8) Uani 1 1 d . . . C31 C 0.3480(6) 0.5942(7) 0.0848(5) 0.037(3) Uani 1 1 d . . . C8 C 0.0288(7) 0.3138(7) 0.2606(6) 0.052(3) Uani 1 1 d . . . H8 H 0.0489 0.2656 0.2919 0.062 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 C13 0.034(7) 0.034(6) 0.049(7) 0.003(5) 0.007(6) 0.001(5) C30 0.043(8) 0.036(7) 0.050(7) 0.004(5) 0.011(6) 0.010(6) C40 0.038(7) 0.031(6) 0.039(6) 0.003(5) 0.009(5) 0.001(5) C16 0.073(11) 0.073(10) 0.102(11) -0.020(10) 0.044(10) -0.034(9) C38 0.049(7) 0.020(5) 0.033(6) 0.004(4) 0.009(6) -0.010(5) C15 0.089(12) 0.066(9) 0.070(9) 0.012(8) 0.030(9) 0.003(9) C41 0.043(7) 0.050(7) 0.028(5) -0.005(5) 0.004(5) -0.006(5) C37 0.027(6) 0.032(6) 0.031(6) 0.001(5) 0.007(5) -0.003(5) C29 0.048(8) 0.048(8) 0.061(8) -0.009(6) 0.013(7) 0.009(7) C14 0.049(8) 0.057(8) 0.062(8) -0.002(6) 0.023(7) -0.025(6) C19 0.045(8) 0.028(6) 0.046(6) -0.003(5) 0.021(6) -0.001(5) C18 0.045(8) 0.068(8) 0.040(6) 0.005(6) 0.019(6) -0.007(7) C2 0.089(10) 0.067(8) 0.050(7) -0.005(7) 0.044(8) -0.002(7) C6 0.067(9) 0.032(6) 0.053(7) -0.001(6) 0.024(7) 0.001(6) C1 0.038(7) 0.046(7) 0.039(6) 0.007(6) 0.011(6) 0.006(6) C39 0.032(6) 0.040(6) 0.028(5) -0.011(5) 0.002(5) 0.005(5) C20 0.043(8) 0.049(7) 0.077(8) 0.009(7) 0.008(7) 0.011(6) C24 0.064(9) 0.065(9) 0.061(8) 0.008(7) -0.021(7) 0.029(7) C10 0.036(8) 0.087(11) 0.068(9) -0.006(9) -0.005(7) -0.001(8) C26 0.046(8) 0.048(7) 0.064(8) -0.009(6) 0.015(7) 0.014(6) C9 0.042(9) 0.096(11) 0.078(10) -0.013(8) 0.029(8) -0.027(8) C27 0.054(9) 0.072(9) 0.069(9) 0.003(7) 0.006(7) 0.018(7) C5 0.105(11) 0.041(7) 0.073(9) -0.011(8) 0.017(9) 0.000(8) C3 0.107(12) 0.111(12) 0.044(8) -0.025(9) 0.045(8) 0.008(10) C17 0.048(9) 0.105(11) 0.067(9) -0.002(8) 0.005(8) -0.017(8) C11 0.068(11) 0.076(10) 0.075(9) 0.012(8) 0.009(9) 0.021(9) C12 0.054(8) 0.038(7) 0.060(8) 0.004(6) 0.014(7) 0.002(6) C7 0.033(7) 0.043(7) 0.046(6) 0.009(5) 0.019(6) 0.004(6) C32 0.033(8) 0.069(8) 0.056(7) 0.020(6) 0.012(7) 0.000(7) C28 0.049(9) 0.057(8) 0.099(11) 0.000(8) 0.034(9) 0.026(7) C33 0.032(8) 0.130(13) 0.094(10) 0.046(10) 0.016(8) 0.003(9) C21 0.062(9) 0.049(8) 0.074(9) 0.016(7) 0.004(8) 0.015(7) C22 0.093(12) 0.054(9) 0.101(11) -0.017(9) 0.019(10) 0.002(8) C4 0.113(13) 0.074(11) 0.058(9) -0.024(8) 0.012(9) -0.003(9) C23 0.125(14) 0.060(10) 0.076(10) -0.014(8) 0.035(10) 0.022(9) C25 0.043(7) 0.028(6) 0.029(6) -0.004(5) 0.005(6) 0.002(5) C35 0.097(11) 0.060(8) 0.060(8) 0.013(7) 0.037(8) -0.029(9) C36 0.054(9) 0.063(8) 0.054(7) 0.012(7) 0.014(7) -0.001(7) C34 0.041(9) 0.121(14) 0.093(10) 0.039(10) 0.025(9) -0.015(9) Ag2 0.0445(5) 0.0437(5) 0.0380(4) -0.0030(4) 0.0079(4) 0.0021(5) Ag1 0.0527(6) 0.0436(5) 0.0553(5) 0.0140(5) 0.0151(5) 0.0062(5) P3 0.0342(17) 0.0313(15) 0.0335(15) 0.0004(13) 0.0085(14) 0.0006(13) P1 0.0350(18) 0.0400(18) 0.0442(16) 0.0064(14) 0.0168(15) -0.0008(14) P2 0.0372(18) 0.0352(17) 0.0374(15) 0.0032(13) 0.0085(14) 0.0002(13) Cl1 0.0423(18) 0.0564(18) 0.0491(16) -0.0115(15) 0.0000(14) 0.0123(15) Cl2 0.0386(18) 0.0605(18) 0.0532(17) -0.0125(15) 0.0134(15) -0.0070(14) C31 0.043(8) 0.042(7) 0.029(6) 0.012(5) 0.016(6) -0.005(6) C8 0.043(8) 0.067(8) 0.046(7) 0.005(6) 0.014(7) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 C18 1.377(12) . ? C13 C14 1.380(11) . ? C13 P2 1.784(10) . ? C30 C29 1.328(12) . ? C30 C25 1.397(11) . ? C40 C37 1.532(10) . ? C40 P2 1.873(8) . ? C16 C15 1.373(15) . ? C16 C17 1.373(14) . ? C38 C37 1.526(11) . ? C38 P1 1.843(8) . ? C15 C14 1.374(14) . ? C41 C37 1.558(10) . ? C37 C39 1.558(10) . ? C29 C28 1.363(13) . ? C19 C20 1.403(12) . ? C19 C24 1.406(12) . ? C19 P2 1.817(9) . ? C18 C17 1.394(13) . ? C2 C3 1.385(12) . ? C2 C1 1.421(11) . ? C6 C1 1.343(11) . ? C6 C5 1.420(12) . ? C1 P1 1.841(9) . ? C39 P3 1.882(8) . ? C20 C21 1.387(12) . ? C24 C23 1.365(13) . ? C10 C11 1.323(13) . ? C10 C9 1.374(14) . ? C26 C27 1.368(12) . ? C26 C25 1.396(12) . ? C9 C8 1.382(13) . ? C27 C28 1.357(12) . ? C5 C4 1.335(13) . ? C3 C4 1.379(14) . ? C11 C12 1.388(14) . ? C12 C7 1.405(12) . ? C7 C8 1.374(12) . ? C7 P1 1.763(10) . ? C32 C33 1.355(13) . ? C32 C31 1.366(12) . ? C33 C34 1.363(15) . ? C21 C22 1.406(13) . ? C22 C23 1.353(14) . ? C25 P3 1.738(9) . ? C35 C34 1.340(14) . ? C35 C36 1.382(13) . ? C36 C31 1.394(11) . ? N2 C103 1.270(12) . ? N2 C105 1.465(11) . ? N2 C104 1.471(11) . ? N1 C102 1.298(11) . ? N1 C100 1.473(12) . ? N1 C101 1.476(12) . ? O1 C102 1.229(12) . ? O2 C103 1.267(12) . ? Ag2 P3 2.463(2) . ? Ag2 P2 2.502(3) . ? Ag2 Cl1 2.620(3) . ? Ag2 Cl2 2.642(3) . ? Ag2 Ag1 3.3847(12) 4_565 ? Ag1 P1 2.364(3) . ? Ag1 Cl2 2.469(3) 4_566 ? Ag1 Cl1 2.498(3) 4_566 ? P3 C31 1.803(9) . ? Cl1 Ag1 2.498(3) 4_565 ? Cl2 Ag1 2.469(3) 4_565 ? 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 C18 C13 C14 121.5(10) . . ? C18 C13 P2 115.8(8) . . ? C14 C13 P2 122.2(8) . . ? C29 C30 C25 124.0(10) . . ? C37 C40 P2 121.2(6) . . ? C15 C16 C17 122.8(12) . . ? C37 C38 P1 119.2(6) . . ? C16 C15 C14 118.6(12) . . ? C38 C37 C40 112.7(7) . . ? C38 C37 C41 108.3(7) . . ? C40 C37 C41 106.8(7) . . ? C38 C37 C39 106.8(7) . . ? C40 C37 C39 114.4(7) . . ? C41 C37 C39 107.6(7) . . ? C30 C29 C28 119.2(11) . . ? C15 C14 C13 119.7(11) . . ? C20 C19 C24 117.3(9) . . ? C20 C19 P2 125.6(8) . . ? C24 C19 P2 116.8(8) . . ? C13 C18 C17 119.0(10) . . ? C3 C2 C1 121.8(11) . . ? C1 C6 C5 121.2(10) . . ? C6 C1 C2 116.9(9) . . ? C6 C1 P1 126.1(8) . . ? C2 C1 P1 117.0(8) . . ? C37 C39 P3 125.7(6) . . ? C21 C20 C19 119.3(10) . . ? C23 C24 C19 123.7(11) . . ? C11 C10 C9 122.6(12) . . ? C27 C26 C25 120.0(10) . . ? C10 C9 C8 120.2(11) . . ? C28 C27 C26 121.4(12) . . ? C4 C5 C6 120.8(11) . . ? C4 C3 C2 118.8(11) . . ? C16 C17 C18 118.3(12) . . ? C10 C11 C12 117.2(12) . . ? C11 C12 C7 123.1(11) . . ? C8 C7 C12 116.7(10) . . ? C8 C7 P1 120.1(8) . . ? C12 C7 P1 123.1(8) . . ? C33 C32 C31 119.9(11) . . ? C27 C28 C29 119.8(11) . . ? C32 C33 C34 122.6(12) . . ? C20 C21 C22 120.2(11) . . ? C23 C22 C21 121.4(12) . . ? C5 C4 C3 120.4(12) . . ? C22 C23 C24 118.0(12) . . ? C26 C25 C30 115.6(9) . . ? C26 C25 P3 117.0(7) . . ? C30 C25 P3 127.4(8) . . ? C34 C35 C36 117.1(12) . . ? C35 C36 C31 123.9(11) . . ? C35 C34 C33 120.2(12) . . ? C103 N2 C105 123.0(11) . . ? C103 N2 C104 118.8(10) . . ? C105 N2 C104 118.0(10) . . ? C102 N1 C100 116.6(10) . . ? C102 N1 C101 123.7(10) . . ? C100 N1 C101 119.8(9) . . ? O1 C102 N1 123.3(12) . . ? O2 C103 N2 119.7(12) . . ? P3 Ag2 P2 97.77(8) . . ? P3 Ag2 Cl1 114.24(8) . . ? P2 Ag2 Cl1 117.07(9) . . ? P3 Ag2 Cl2 126.05(8) . . ? P2 Ag2 Cl2 115.37(9) . . ? Cl1 Ag2 Cl2 87.96(8) . . ? P3 Ag2 Ag1 151.29(6) . 4_565 ? P2 Ag2 Ag1 110.22(7) . 4_565 ? Cl1 Ag2 Ag1 47.06(6) . 4_565 ? Cl2 Ag2 Ag1 46.36(6) . 4_565 ? P1 Ag1 Cl2 136.80(9) . 4_566 ? P1 Ag1 Cl1 127.15(9) . 4_566 ? Cl2 Ag1 Cl1 94.75(9) 4_566 4_566 ? C25 P3 C31 102.7(5) . . ? C25 P3 C39 104.7(4) . . ? C31 P3 C39 100.5(4) . . ? C25 P3 Ag2 118.8(3) . . ? C31 P3 Ag2 119.0(3) . . ? C39 P3 Ag2 108.8(3) . . ? C7 P1 C1 103.0(4) . . ? C7 P1 C38 99.3(4) . . ? C1 P1 C38 108.1(4) . . ? C7 P1 Ag1 114.5(3) . . ? C1 P1 Ag1 110.0(3) . . ? C38 P1 Ag1 120.3(3) . . ? C13 P2 C19 98.8(4) . . ? C13 P2 C40 105.9(4) . . ? C19 P2 C40 102.0(4) . . ? C13 P2 Ag2 117.0(4) . . ? C19 P2 Ag2 116.7(3) . . ? C40 P2 Ag2 114.2(3) . . ? Ag1 Cl1 Ag2 82.77(8) 4_565 . ? Ag1 Cl2 Ag2 82.87(8) 4_565 . ? C32 C31 C36 116.1(9) . . ? C32 C31 P3 117.4(8) . . ? C36 C31 P3 126.5(9) . . ? C7 C8 C9 120.0(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 C17 C16 C15 C14 -2.5(19) . . . . ? P1 C38 C37 C40 71.5(9) . . . . ? P1 C38 C37 C41 -46.4(9) . . . . ? P1 C38 C37 C39 -162.1(5) . . . . ? P2 C40 C37 C38 57.0(9) . . . . ? P2 C40 C37 C41 175.9(6) . . . . ? P2 C40 C37 C39 -65.2(10) . . . . ? C25 C30 C29 C28 0.4(16) . . . . ? C16 C15 C14 C13 2.8(17) . . . . ? C18 C13 C14 C15 -1.5(16) . . . . ? P2 C13 C14 C15 -172.9(8) . . . . ? C14 C13 C18 C17 -0.2(15) . . . . ? P2 C13 C18 C17 171.7(8) . . . . ? C5 C6 C1 C2 -0.4(16) . . . . ? C5 C6 C1 P1 179.7(8) . . . . ? C3 C2 C1 C6 1.9(16) . . . . ? C3 C2 C1 P1 -178.1(9) . . . . ? C38 C37 C39 P3 -51.6(9) . . . . ? C40 C37 C39 P3 73.8(10) . . . . ? C41 C37 C39 P3 -167.8(6) . . . . ? C24 C19 C20 C21 -0.5(15) . . . . ? P2 C19 C20 C21 173.9(8) . . . . ? C20 C19 C24 C23 0.1(17) . . . . ? P2 C19 C24 C23 -174.8(10) . . . . ? C11 C10 C9 C8 2.0(19) . . . . ? C25 C26 C27 C28 1.0(17) . . . . ? C1 C6 C5 C4 -1.7(18) . . . . ? C1 C2 C3 C4 -1.5(19) . . . . ? C15 C16 C17 C18 0.8(19) . . . . ? C13 C18 C17 C16 0.5(16) . . . . ? C9 C10 C11 C12 -2.0(19) . . . . ? C10 C11 C12 C7 1.9(17) . . . . ? C11 C12 C7 C8 -1.7(15) . . . . ? C11 C12 C7 P1 177.1(8) . . . . ? C26 C27 C28 C29 -1.8(17) . . . . ? C30 C29 C28 C27 1.2(17) . . . . ? C31 C32 C33 C34 -1.1(19) . . . . ? C19 C20 C21 C22 -1.2(17) . . . . ? C20 C21 C22 C23 3(2) . . . . ? C6 C5 C4 C3 2(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C21 C22 C23 C24 -4(2) . . . . ? C19 C24 C23 C22 2(2) . . . . ? C27 C26 C25 C30 0.5(14) . . . . ? C27 C26 C25 P3 179.2(8) . . . . ? C29 C30 C25 C26 -1.2(14) . . . . ? C29 C30 C25 P3 -179.7(8) . . . . ? C34 C35 C36 C31 -0.1(17) . . . . ? C36 C35 C34 C33 2(2) . . . . ? C32 C33 C34 C35 -2(2) . . . . ? C100 N1 C102 O1 178.9(11) . . . . ? C101 N1 C102 O1 -3(2) . . . . ? C105 N2 C103 O2 3.2(18) . . . . ? C104 N2 C103 O2 177.3(10) . . . . ? C26 C25 P3 C31 115.4(8) . . . . ? C30 C25 P3 C31 -66.1(9) . . . . ? C26 C25 P3 C39 -140.0(7) . . . . ? C30 C25 P3 C39 38.5(9) . . . . ? C26 C25 P3 Ag2 -18.4(9) . . . . ? C30 C25 P3 Ag2 160.1(7) . . . . ? C37 C39 P3 C25 79.0(8) . . . . ? C37 C39 P3 C31 -174.7(7) . . . . ? C37 C39 P3 Ag2 -48.9(8) . . . . ? P2 Ag2 P3 C25 -100.9(3) . . . . ? Cl1 Ag2 P3 C25 23.5(4) . . . . ? Cl2 Ag2 P3 C25 129.8(3) . . . . ? Ag1 Ag2 P3 C25 66.4(4) 4_565 . . . ? P2 Ag2 P3 C31 132.8(4) . . . . ? Cl1 Ag2 P3 C31 -102.7(4) . . . . ? Cl2 Ag2 P3 C31 3.5(4) . . . . ? Ag1 Ag2 P3 C31 -59.9(4) 4_565 . . . ? P2 Ag2 P3 C39 18.7(3) . . . . ? Cl1 Ag2 P3 C39 143.1(3) . . . . ? Cl2 Ag2 P3 C39 -110.7(3) . . . . ? Ag1 Ag2 P3 C39 -174.1(3) 4_565 . . . ? C8 C7 P1 C1 -114.5(8) . . . . ? C12 C7 P1 C1 66.7(8) . . . . ? C8 C7 P1 C38 134.3(8) . . . . ? C12 C7 P1 C38 -44.5(8) . . . . ? C8 C7 P1 Ag1 4.8(9) . . . . ? C12 C7 P1 Ag1 -174.0(7) . . . . ? C6 C1 P1 C7 -94.2(10) . . . . ? C2 C1 P1 C7 85.9(8) . . . . ? C6 C1 P1 C38 10.2(11) . . . . ? C2 C1 P1 C38 -169.7(8) . . . . ? C6 C1 P1 Ag1 143.4(9) . . . . ? C2 C1 P1 Ag1 -36.5(9) . . . . ? C37 C38 P1 C7 -158.0(7) . . . . ? C37 C38 P1 C1 95.0(7) . . . . ? C37 C38 P1 Ag1 -32.4(8) . . . . ? Cl2 Ag1 P1 C7 163.3(3) 4_566 . . . ? Cl1 Ag1 P1 C7 -33.2(4) 4_566 . . . ? Cl2 Ag1 P1 C1 -81.3(4) 4_566 . . . ? Cl1 Ag1 P1 C1 82.2(4) 4_566 . . . ? Cl2 Ag1 P1 C38 45.2(4) 4_566 . . . ? Cl1 Ag1 P1 C38 -151.3(3) 4_566 . . . ? C18 C13 P2 C19 -123.4(8) . . . . ? C14 C13 P2 C19 48.4(9) . . . . ? C18 C13 P2 C40 131.3(8) . . . . ? C14 C13 P2 C40 -56.8(9) . . . . ? C18 C13 P2 Ag2 2.7(9) . . . . ? C14 C13 P2 Ag2 174.5(7) . . . . ? C20 C19 P2 C13 -92.2(9) . . . . ? C24 C19 P2 C13 82.2(9) . . . . ? C20 C19 P2 C40 16.2(10) . . . . ? C24 C19 P2 C40 -169.3(8) . . . . ? C20 C19 P2 Ag2 141.5(8) . . . . ? C24 C19 P2 Ag2 -44.1(9) . . . . ? C37 C40 P2 C13 -90.0(8) . . . . ? C37 C40 P2 C19 167.1(7) . . . . ? C37 C40 P2 Ag2 40.3(8) . . . . ? P3 Ag2 P2 C13 107.4(3) . . . . ? Cl1 Ag2 P2 C13 -15.0(4) . . . . ? Cl2 Ag2 P2 C13 -116.4(3) . . . . ? Ag1 Ag2 P2 C13 -66.2(3) 4_565 . . . ? P3 Ag2 P2 C19 -136.0(4) . . . . ? Cl1 Ag2 P2 C19 101.7(4) . . . . ? Cl2 Ag2 P2 C19 0.3(4) . . . . ? Ag1 Ag2 P2 C19 50.5(4) 4_565 . . . ? P3 Ag2 P2 C40 -17.1(3) . . . . ? Cl1 Ag2 P2 C40 -139.5(3) . . . . ? Cl2 Ag2 P2 C40 119.1(3) . . . . ? Ag1 Ag2 P2 C40 169.4(3) 4_565 . . . ? P3 Ag2 Cl1 Ag1 153.50(8) . . . 4_565 ? P2 Ag2 Cl1 Ag1 -93.13(9) . . . 4_565 ? Cl2 Ag2 Cl1 Ag1 24.47(8) . . . 4_565 ? P3 Ag2 Cl2 Ag1 -143.60(9) . . . 4_565 ? P2 Ag2 Cl2 Ag1 94.38(10) . . . 4_565 ? Cl1 Ag2 Cl2 Ag1 -24.77(8) . . . 4_565 ? C33 C32 C31 C36 2.9(16) . . . . ? C33 C32 C31 P3 -176.7(8) . . . . ? C35 C36 C31 C32 -2.4(16) . . . . ? C35 C36 C31 P3 177.2(8) . . . . ? C25 P3 C31 C32 179.0(8) . . . . ? C39 P3 C31 C32 71.2(9) . . . . ? Ag2 P3 C31 C32 -47.4(9) . . . . ? C25 P3 C31 C36 -0.5(10) . . . . ? C39 P3 C31 C36 -108.4(9) . . . . ? Ag2 P3 C31 C36 133.0(8) . . . . ? C12 C7 C8 C9 1.6(14) . . . . ? P1 C7 C8 C9 -177.3(8) . . . . ? C10 C9 C8 C7 -1.7(16) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.587 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.115 data_jose_3 _database_code_CSD 173822 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ag(tripod)Br ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H39 Ag2 Br2 P3' _chemical_formula_sum 'C41 H39 Ag2 Br2 P3' _chemical_formula_weight 1000.19 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 19.486(3) _cell_length_b 9.7523(13) _cell_length_c 20.388(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.638(4) _cell_angle_gamma 90.00 _cell_volume 3855.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 2.585 _cell_measurement_theta_max 28.21 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 3.242 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3645 _exptl_absorpt_correction_T_max 0.5930 _exptl_absorpt_process_details Sadabs _exptl_special_details ; Ag(tripod)Br ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47731 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 30.54 _reflns_number_total 11712 _reflns_number_gt 5373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Shelxtl' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0341P)^2^+0.5891P] 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 0.00001(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11712 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 Ag2 Ag 0.287902(17) 0.27415(3) 0.396567(15) 0.03805(9) Uani 1 1 d . . . Ag1 Ag 0.232809(18) 0.95193(4) 0.396193(19) 0.05016(11) Uani 1 1 d . . . Br2 Br 0.34821(3) 0.03772(5) 0.35973(3) 0.06487(17) Uani 1 1 d . . . P1 P 0.18320(5) 0.74640(11) 0.43475(5) 0.0350(3) Uani 1 1 d . . . P3 P 0.33967(5) 0.49184(11) 0.35970(5) 0.0301(2) Uani 1 1 d . . . P2 P 0.30147(5) 0.32041(11) 0.51694(5) 0.0320(2) Uani 1 1 d . . . C20 C 0.4299(2) 0.1995(5) 0.5383(2) 0.0511(12) Uani 1 1 d . . . H20 H 0.4400 0.2518 0.5023 0.061 Uiso 1 1 calc R . . C25 C 0.4278(2) 0.4823(4) 0.33631(17) 0.0303(9) Uani 1 1 d . . . C19 C 0.3655(2) 0.2096(4) 0.56068(18) 0.0345(9) Uani 1 1 d . . . C13 C 0.2298(2) 0.3245(4) 0.5692(2) 0.0373(10) Uani 1 1 d . . . C18 C 0.1647(2) 0.2884(5) 0.5426(2) 0.0489(12) Uani 1 1 d . . . H18 H 0.1579 0.2589 0.4991 0.059 Uiso 1 1 calc R . . C24 C 0.3511(2) 0.1255(5) 0.6118(2) 0.0480(12) Uani 1 1 d . . . H24 H 0.3073 0.1273 0.6262 0.058 Uiso 1 1 calc R . . C27 C 0.5308(2) 0.5867(5) 0.3019(2) 0.0506(12) Uani 1 1 d . . . H27 H 0.5546 0.6647 0.2910 0.061 Uiso 1 1 calc R . . C26 C 0.4640(2) 0.5980(5) 0.3198(2) 0.0450(11) Uani 1 1 d . . . H26 H 0.4433 0.6839 0.3206 0.054 Uiso 1 1 calc R . . C14 C 0.2388(3) 0.3669(5) 0.6348(2) 0.0518(12) Uani 1 1 d . . . H14 H 0.2821 0.3924 0.6540 0.062 Uiso 1 1 calc R . . C15 C 0.1820(4) 0.3706(6) 0.6709(3) 0.0781(19) Uani 1 1 d . . . H15 H 0.1878 0.3976 0.7149 0.094 Uiso 1 1 calc R . . C17 C 0.1090(3) 0.2955(6) 0.5800(3) 0.0719(16) Uani 1 1 d . . . H17 H 0.0652 0.2724 0.5611 0.086 Uiso 1 1 calc R . . C39 C 0.3412(2) 0.4928(4) 0.52958(18) 0.0359(10) Uani 1 1 d . . . H39A H 0.3384 0.5179 0.5753 0.043 Uiso 1 1 calc R . . H39B H 0.3898 0.4838 0.5236 0.043 Uiso 1 1 calc R . . C38 C 0.3489(2) 0.6295(4) 0.42263(19) 0.0365(10) Uani 1 1 d . . . H38A H 0.3978 0.6412 0.4356 0.044 Uiso 1 1 calc R . . H38B H 0.3326 0.7139 0.4013 0.044 Uiso 1 1 calc R . . C31 C 0.29033(19) 0.5698(4) 0.28834(18) 0.0322(9) Uani 1 1 d . . . C36 C 0.2452(2) 0.4873(5) 0.2493(2) 0.0445(11) Uani 1 1 d . . . H36 H 0.2403 0.3958 0.2609 0.053 Uiso 1 1 calc R . . C32 C 0.2952(2) 0.7070(4) 0.2702(2) 0.0426(11) Uani 1 1 d . . . H32 H 0.3248 0.7653 0.2956 0.051 Uiso 1 1 calc R . . C28 C 0.5614(2) 0.4605(5) 0.3005(2) 0.0478(12) Uani 1 1 d . . . H28 H 0.6058 0.4525 0.2877 0.057 Uiso 1 1 calc R . . C30 C 0.4603(2) 0.3570(5) 0.3353(2) 0.0484(12) Uani 1 1 d . . . H30 H 0.4372 0.2782 0.3465 0.058 Uiso 1 1 calc R . . C29 C 0.5269(2) 0.3470(5) 0.3177(2) 0.0592(14) Uani 1 1 d . . . H29 H 0.5482 0.2618 0.3176 0.071 Uiso 1 1 calc R . . C22 C 0.4643(3) 0.0331(5) 0.6206(3) 0.0596(14) Uani 1 1 d . . . H22 H 0.4978 -0.0245 0.6414 0.072 Uiso 1 1 calc R . . C21 C 0.4794(2) 0.1133(5) 0.5683(3) 0.0585(14) Uani 1 1 d . . . H21 H 0.5229 0.1092 0.5532 0.070 Uiso 1 1 calc R . . C33 C 0.2565(3) 0.7573(5) 0.2151(2) 0.0576(14) Uani 1 1 d . . . H33 H 0.2602 0.8491 0.2036 0.069 Uiso 1 1 calc R . . C23 C 0.4002(3) 0.0386(5) 0.6420(2) 0.0637(15) Uani 1 1 d . . . H23 H 0.3897 -0.0163 0.6769 0.076 Uiso 1 1 calc R . . C35 C 0.2073(2) 0.5369(6) 0.1938(2) 0.0575(14) Uani 1 1 d . . . H35 H 0.1783 0.4788 0.1677 0.069 Uiso 1 1 calc R . . C34 C 0.2126(2) 0.6725(6) 0.1773(2) 0.0593(14) Uani 1 1 d . . . H34 H 0.1864 0.7070 0.1404 0.071 Uiso 1 1 calc R . . C16 C 0.1181(3) 0.3356(6) 0.6434(4) 0.082(2) Uani 1 1 d . . . H16 H 0.0807 0.3393 0.6683 0.099 Uiso 1 1 calc R . . C40 C 0.31270(19) 0.6154(4) 0.48650(17) 0.0287(9) Uani 1 1 d . . . C41 C 0.3312(2) 0.7450(4) 0.5272(2) 0.0439(11) Uani 1 1 d . . . H41A H 0.3804 0.7521 0.5355 0.066 Uiso 1 1 calc R . . H41B H 0.3112 0.7398 0.5683 0.066 Uiso 1 1 calc R . . H41C H 0.3136 0.8242 0.5031 0.066 Uiso 1 1 calc R . . C37 C 0.23437(19) 0.6001(4) 0.4718(2) 0.0381(10) Uani 1 1 d . . . H37A H 0.2159 0.5769 0.5129 0.046 Uiso 1 1 calc R . . H37B H 0.2260 0.5221 0.4426 0.046 Uiso 1 1 calc R . . Br1 Br 0.15874(2) 0.17121(5) 0.35549(2) 0.04441(12) Uani 1 1 d . . . C7 C 0.1287(2) 0.6726(4) 0.36578(19) 0.0359(10) Uani 1 1 d . . . C1 C 0.1201(2) 0.7736(5) 0.49466(19) 0.0372(10) Uani 1 1 d . . . C12 C 0.1111(2) 0.5358(5) 0.3588(2) 0.0516(12) Uani 1 1 d . . . H12 H 0.1293 0.4735 0.3904 0.062 Uiso 1 1 calc R . . C8 C 0.1009(3) 0.7612(5) 0.3168(2) 0.0627(15) Uani 1 1 d . . . H8 H 0.1114 0.8542 0.3195 0.075 Uiso 1 1 calc R . . C2 C 0.1056(3) 0.9031(5) 0.5147(2) 0.0540(13) Uani 1 1 d . . . H2 H 0.1290 0.9777 0.4992 0.065 Uiso 1 1 calc R . . C11 C 0.0679(3) 0.4892(6) 0.3068(2) 0.0599(14) Uani 1 1 d . . . H11 H 0.0573 0.3964 0.3036 0.072 Uiso 1 1 calc R . . C6 C 0.0846(2) 0.6651(5) 0.5192(2) 0.0586(14) Uani 1 1 d . . . H6 H 0.0942 0.5761 0.5064 0.070 Uiso 1 1 calc R . . C10 C 0.0403(3) 0.5771(6) 0.2595(2) 0.0627(15) Uani 1 1 d . . . H10 H 0.0101 0.5454 0.2246 0.075 Uiso 1 1 calc R . . C9 C 0.0577(3) 0.7125(6) 0.2641(3) 0.0772(18) Uani 1 1 d . . . H9 H 0.0402 0.7729 0.2313 0.093 Uiso 1 1 calc R . . C4 C 0.0214(3) 0.8161(7) 0.5805(2) 0.0658(16) Uani 1 1 d . . . H4 H -0.0126 0.8311 0.6087 0.079 Uiso 1 1 calc R . . C3 C 0.0561(3) 0.9233(6) 0.5583(3) 0.0673(16) Uani 1 1 d . . . H3 H 0.0467 1.0115 0.5722 0.081 Uiso 1 1 calc R . . C5 C 0.0357(3) 0.6865(7) 0.5619(3) 0.0692(16) Uani 1 1 d . . . H5 H 0.0125 0.6125 0.5781 0.083 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 Ag2 0.0482(2) 0.03034(17) 0.03660(17) -0.00210(15) 0.00900(14) -0.00445(15) Ag1 0.0494(2) 0.0393(2) 0.0636(2) 0.01286(18) 0.01477(18) -0.00433(17) Br2 0.0492(3) 0.0352(3) 0.1167(5) -0.0151(3) 0.0410(3) -0.0049(2) P1 0.0316(6) 0.0310(6) 0.0437(6) 0.0086(5) 0.0104(5) 0.0043(5) P3 0.0372(6) 0.0271(5) 0.0277(5) -0.0010(4) 0.0111(5) -0.0019(5) P2 0.0363(6) 0.0326(6) 0.0278(5) 0.0044(5) 0.0058(5) 0.0035(5) C20 0.052(3) 0.054(3) 0.048(3) 0.014(2) 0.012(2) 0.013(2) C25 0.037(2) 0.029(2) 0.025(2) -0.0010(17) 0.0052(17) -0.0008(18) C19 0.040(2) 0.033(2) 0.031(2) 0.0009(18) 0.0063(18) 0.0029(19) C13 0.047(3) 0.028(2) 0.039(2) 0.0056(19) 0.014(2) 0.004(2) C18 0.050(3) 0.046(3) 0.051(3) 0.004(2) 0.011(2) -0.003(2) C24 0.049(3) 0.048(3) 0.049(3) 0.017(2) 0.016(2) 0.012(2) C27 0.038(3) 0.055(3) 0.060(3) 0.011(3) 0.013(2) -0.010(2) C26 0.042(3) 0.037(3) 0.058(3) 0.006(2) 0.016(2) 0.005(2) C14 0.069(3) 0.048(3) 0.040(3) -0.002(2) 0.014(2) 0.007(3) C15 0.131(6) 0.054(4) 0.060(3) 0.002(3) 0.063(4) 0.018(4) C17 0.053(3) 0.075(4) 0.092(4) 0.018(4) 0.031(3) 0.001(3) C39 0.040(2) 0.038(2) 0.028(2) 0.0023(19) -0.0005(18) -0.0001(19) C38 0.038(2) 0.034(2) 0.039(2) -0.0003(19) 0.0136(19) -0.0047(19) C31 0.030(2) 0.037(2) 0.031(2) -0.0017(18) 0.0129(18) 0.0014(18) C36 0.045(3) 0.044(3) 0.045(3) 0.001(2) 0.010(2) -0.006(2) C32 0.046(3) 0.036(3) 0.046(3) 0.005(2) 0.005(2) -0.005(2) C28 0.032(2) 0.067(4) 0.046(3) -0.006(2) 0.009(2) 0.000(2) C30 0.047(3) 0.037(3) 0.063(3) -0.006(2) 0.013(2) 0.003(2) C29 0.048(3) 0.050(3) 0.081(4) -0.015(3) 0.013(3) 0.012(3) C22 0.064(4) 0.047(3) 0.065(3) 0.014(3) -0.009(3) 0.016(3) C21 0.041(3) 0.061(3) 0.073(4) 0.003(3) 0.009(3) 0.015(3) C33 0.061(3) 0.047(3) 0.065(3) 0.024(3) 0.007(3) 0.004(3) C23 0.070(4) 0.063(4) 0.061(3) 0.033(3) 0.018(3) 0.017(3) C35 0.051(3) 0.072(4) 0.048(3) 0.003(3) -0.005(2) -0.004(3) C34 0.043(3) 0.086(4) 0.047(3) 0.014(3) -0.006(2) 0.010(3) C16 0.077(5) 0.075(4) 0.104(5) 0.015(4) 0.059(4) 0.009(4) C40 0.032(2) 0.028(2) 0.0261(19) 0.0001(17) 0.0039(17) 0.0014(17) C41 0.060(3) 0.034(3) 0.038(2) -0.0088(19) 0.005(2) -0.001(2) C37 0.033(2) 0.036(2) 0.046(2) 0.008(2) 0.009(2) 0.0032(19) Br1 0.0407(3) 0.0393(3) 0.0527(3) 0.0030(2) 0.0021(2) -0.0004(2) C7 0.036(2) 0.031(2) 0.042(2) 0.0085(19) 0.0142(19) 0.0062(19) C1 0.033(2) 0.042(3) 0.037(2) 0.002(2) 0.0036(19) 0.009(2) C12 0.055(3) 0.043(3) 0.055(3) 0.014(2) -0.003(2) 0.001(2) C8 0.084(4) 0.044(3) 0.058(3) 0.008(3) -0.008(3) 0.008(3) C2 0.067(3) 0.047(3) 0.050(3) 0.003(2) 0.013(3) 0.015(3) C11 0.059(3) 0.054(3) 0.064(3) 0.000(3) -0.010(3) -0.013(3) C6 0.056(3) 0.053(3) 0.072(3) -0.004(3) 0.031(3) -0.009(3) C10 0.058(3) 0.082(4) 0.047(3) -0.006(3) -0.004(3) -0.001(3) C9 0.097(5) 0.068(4) 0.060(3) 0.010(3) -0.022(3) 0.021(4) C4 0.044(3) 0.107(5) 0.048(3) -0.006(3) 0.011(2) 0.020(3) C3 0.078(4) 0.067(4) 0.060(3) -0.009(3) 0.022(3) 0.025(3) C5 0.057(3) 0.090(5) 0.066(3) -0.001(3) 0.034(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 P2 2.4837(11) . ? Ag2 P3 2.4977(11) . ? Ag2 Br2 2.7267(6) . ? Ag2 Br1 2.7622(6) . ? Ag2 Ag1 3.3205(6) 1_545 ? Ag2 Ag1 6.6964(10) . ? Ag1 P1 2.3915(11) . ? Ag1 Br2 2.5764(7) 1_565 ? Ag1 Br1 2.6664(6) 1_565 ? Ag1 Ag2 3.3205(6) 1_565 ? Br2 Ag1 2.5764(7) 1_545 ? P1 C7 1.825(4) . ? P1 C1 1.835(4) . ? P1 C37 1.858(4) . ? P3 C25 1.828(4) . ? P3 C31 1.829(4) . ? P3 C38 1.854(4) . ? P2 C19 1.816(4) . ? P2 C13 1.838(4) . ? P2 C39 1.859(4) . ? C20 C21 1.377(6) . ? C20 C19 1.380(6) . ? C20 H20 0.9300 . ? C25 C30 1.378(6) . ? C25 C26 1.390(6) . ? C19 C24 1.376(5) . ? C13 C18 1.376(6) . ? C13 C14 1.394(6) . ? C18 C17 1.386(6) . ? C18 H18 0.9300 . ? C24 C23 1.378(6) . ? C24 H24 0.9300 . ? C27 C28 1.370(6) . ? C27 C26 1.390(6) . ? C27 H27 0.9300 . ? C26 H26 0.9300 . ? C14 C15 1.390(7) . ? C14 H14 0.9300 . ? C15 C16 1.358(8) . ? C15 H15 0.9300 . ? C17 C16 1.345(8) . ? C17 H17 0.9300 . ? C39 C40 1.553(5) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C38 C40 1.546(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C31 C36 1.384(6) . ? C31 C32 1.394(6) . ? C36 C35 1.377(6) . ? C36 H36 0.9300 . ? C32 C33 1.380(6) . ? C32 H32 0.9300 . ? C28 C29 1.359(6) . ? C28 H28 0.9300 . ? C30 C29 1.383(6) . ? C30 H30 0.9300 . ? C29 H29 0.9300 . ? C22 C23 1.363(7) . ? C22 C21 1.378(7) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C33 C34 1.371(7) . ? C33 H33 0.9300 . ? C23 H23 0.9300 . ? C35 C34 1.371(7) . ? C35 H35 0.9300 . ? C34 H34 0.9300 . ? C16 H16 0.9300 . ? C40 C37 1.533(5) . ? C40 C41 1.535(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? Br1 Ag1 2.6664(6) 1_545 ? C7 C12 1.382(6) . ? C7 C8 1.389(6) . ? C1 C2 1.365(6) . ? C1 C6 1.384(6) . ? C12 C11 1.365(6) . ? C12 H12 0.9300 . ? C8 C9 1.382(7) . ? C8 H8 0.9300 . ? C2 C3 1.389(7) . ? C2 H2 0.9300 . ? C11 C10 1.361(7) . ? C11 H11 0.9300 . ? C6 C5 1.369(6) . ? C6 H6 0.9300 . ? C10 C9 1.364(7) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? C4 C3 1.347(8) . ? C4 C5 1.357(8) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C5 H5 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 P2 Ag2 P3 97.82(4) . . ? P2 Ag2 Br2 114.76(3) . . ? P3 Ag2 Br2 115.99(3) . . ? P2 Ag2 Br1 111.78(3) . . ? P3 Ag2 Br1 126.91(3) . . ? Br2 Ag2 Br1 90.782(19) . . ? P2 Ag2 Ag1 100.20(3) . 1_545 ? P3 Ag2 Ag1 160.69(3) . 1_545 ? Br2 Ag2 Ag1 49.239(15) . 1_545 ? Br1 Ag2 Ag1 50.994(12) . 1_545 ? P2 Ag2 Ag1 79.83(3) . . ? P3 Ag2 Ag1 39.65(3) . . ? Br2 Ag2 Ag1 155.197(15) . . ? Br1 Ag2 Ag1 102.545(14) . . ? Ag1 Ag2 Ag1 151.931(13) 1_545 . ? P1 Ag1 Br2 139.42(3) . 1_565 ? P1 Ag1 Br1 123.41(3) . 1_565 ? Br2 Ag1 Br1 96.36(2) 1_565 1_565 ? P1 Ag1 Ag2 158.98(3) . 1_565 ? Br2 Ag1 Ag2 53.287(14) 1_565 1_565 ? Br1 Ag1 Ag2 53.609(15) 1_565 1_565 ? P1 Ag1 Ag2 40.73(3) . . ? Br2 Ag1 Ag2 100.166(15) 1_565 . ? Br1 Ag1 Ag2 150.906(15) 1_565 . ? Ag2 Ag1 Ag2 151.931(13) 1_565 . ? Ag1 Br2 Ag2 77.474(18) 1_545 . ? C7 P1 C1 101.10(18) . . ? C7 P1 C37 105.03(19) . . ? C1 P1 C37 102.01(19) . . ? C7 P1 Ag1 107.50(13) . . ? C1 P1 Ag1 114.60(15) . . ? C37 P1 Ag1 124.00(13) . . ? C25 P3 C31 104.31(17) . . ? C25 P3 C38 100.84(18) . . ? C31 P3 C38 104.91(19) . . ? C25 P3 Ag2 116.91(13) . . ? C31 P3 Ag2 113.35(13) . . ? C38 P3 Ag2 114.95(13) . . ? C19 P2 C13 104.62(18) . . ? C19 P2 C39 102.32(18) . . ? C13 P2 C39 103.30(19) . . ? C19 P2 Ag2 112.23(13) . . ? C13 P2 Ag2 124.30(14) . . ? C39 P2 Ag2 107.68(13) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C30 C25 C26 118.1(4) . . ? C30 C25 P3 119.6(3) . . ? C26 C25 P3 122.3(3) . . ? C24 C19 C20 117.9(4) . . ? C24 C19 P2 123.0(3) . . ? C20 C19 P2 118.9(3) . . ? C18 C13 C14 118.5(4) . . ? C18 C13 P2 119.3(3) . . ? C14 C13 P2 122.1(4) . . ? C13 C18 C17 120.8(5) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C19 C24 C23 121.4(4) . . ? C19 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C28 C27 C26 119.9(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C15 C14 C13 119.1(5) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C40 C39 P2 119.8(3) . . ? C40 C39 H39A 107.4 . . ? P2 C39 H39A 107.4 . . ? C40 C39 H39B 107.4 . . ? P2 C39 H39B 107.4 . . ? H39A C39 H39B 106.9 . . ? C40 C38 P3 119.8(3) . . ? C40 C38 H38A 107.4 . . ? P3 C38 H38A 107.4 . . ? C40 C38 H38B 107.4 . . ? P3 C38 H38B 107.4 . . ? H38A C38 H38B 106.9 . . ? C36 C31 C32 117.5(4) . . ? C36 C31 P3 118.1(3) . . ? C32 C31 P3 124.4(3) . . ? C35 C36 C31 121.8(4) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C29 C28 C27 119.9(4) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C25 C30 C29 120.7(4) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C28 C29 C30 120.7(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C34 C35 C36 119.5(5) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C37 C40 C41 111.2(3) . . ? C37 C40 C38 111.8(3) . . ? C41 C40 C38 106.2(3) . . ? C37 C40 C39 109.3(3) . . ? C41 C40 C39 106.0(3) . . ? C38 C40 C39 112.2(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C37 P1 119.3(3) . . ? C40 C37 H37A 107.5 . . ? P1 C37 H37A 107.5 . . ? C40 C37 H37B 107.5 . . ? P1 C37 H37B 107.5 . . ? H37A C37 H37B 107.0 . . ? Ag1 Br1 Ag2 75.397(17) 1_545 . ? C12 C7 C8 116.8(4) . . ? C12 C7 P1 125.5(3) . . ? C8 C7 P1 117.7(3) . . ? C2 C1 C6 118.3(4) . . ? C2 C1 P1 120.3(4) . . ? C6 C1 P1 121.4(3) . . ? C11 C12 C7 122.0(4) . . ? C11 C12 H12 119.0 . . ? C7 C12 H12 119.0 . . ? C9 C8 C7 120.6(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C1 C2 C3 120.0(5) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C10 C11 C12 120.8(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C5 C6 C1 121.1(5) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C11 C10 C9 118.8(5) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C9 C8 121.0(5) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C4 C5 C6 119.6(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? 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 P2 Ag2 Ag1 P1 -62.23(5) . . . . ? P3 Ag2 Ag1 P1 -177.90(6) . . . . ? Br2 Ag2 Ag1 P1 169.01(6) . . . . ? Br1 Ag2 Ag1 P1 48.02(4) . . . . ? Ag1 Ag2 Ag1 P1 30.40(5) 1_545 . . . ? P2 Ag2 Ag1 Br2 104.72(3) . . . 1_565 ? P3 Ag2 Ag1 Br2 -10.95(4) . . . 1_565 ? Br2 Ag2 Ag1 Br2 -24.04(3) . . . 1_565 ? Br1 Ag2 Ag1 Br2 -145.03(2) . . . 1_565 ? Ag1 Ag2 Ag1 Br2 -162.65(2) 1_545 . . 1_565 ? P2 Ag2 Ag1 Br1 -131.65(4) . . . 1_565 ? P3 Ag2 Ag1 Br1 112.68(5) . . . 1_565 ? Br2 Ag2 Ag1 Br1 99.59(5) . . . 1_565 ? Br1 Ag2 Ag1 Br1 -21.40(3) . . . 1_565 ? Ag1 Ag2 Ag1 Br1 -39.02(5) 1_545 . . 1_565 ? P2 Ag2 Ag1 Ag2 87.37(4) . . . 1_565 ? P3 Ag2 Ag1 Ag2 -28.30(5) . . . 1_565 ? Br2 Ag2 Ag1 Ag2 -41.39(5) . . . 1_565 ? Br1 Ag2 Ag1 Ag2 -162.38(2) . . . 1_565 ? Ag1 Ag2 Ag1 Ag2 180.0 1_545 . . 1_565 ? P2 Ag2 Br2 Ag1 81.95(3) . . . 1_545 ? P3 Ag2 Br2 Ag1 -165.00(3) . . . 1_545 ? Br1 Ag2 Br2 Ag1 -32.562(19) . . . 1_545 ? Ag1 Ag2 Br2 Ag1 -155.75(3) . . . 1_545 ? Br2 Ag1 P1 C7 -102.66(14) 1_565 . . . ? Br1 Ag1 P1 C7 64.27(14) 1_565 . . . ? Ag2 Ag1 P1 C7 138.91(14) 1_565 . . . ? Ag2 Ag1 P1 C7 -82.68(14) . . . . ? Br2 Ag1 P1 C1 145.86(14) 1_565 . . . ? Br1 Ag1 P1 C1 -47.21(15) 1_565 . . . ? Ag2 Ag1 P1 C1 27.42(18) 1_565 . . . ? Ag2 Ag1 P1 C1 165.83(16) . . . . ? Br2 Ag1 P1 C37 20.07(19) 1_565 . . . ? Br1 Ag1 P1 C37 -173.00(17) 1_565 . . . ? Ag2 Ag1 P1 C37 -98.36(19) 1_565 . . . ? Ag2 Ag1 P1 C37 40.05(17) . . . . ? P2 Ag2 P3 C25 102.68(14) . . . . ? Br2 Ag2 P3 C25 -19.82(14) . . . . ? Br1 Ag2 P3 C25 -132.47(13) . . . . ? Ag1 Ag2 P3 C25 -56.17(17) 1_545 . . . ? Ag1 Ag2 P3 C25 166.25(15) . . . . ? P2 Ag2 P3 C31 -135.92(13) . . . . ? Br2 Ag2 P3 C31 101.58(13) . . . . ? Br1 Ag2 P3 C31 -11.07(14) . . . . ? Ag1 Ag2 P3 C31 65.23(17) 1_545 . . . ? Ag1 Ag2 P3 C31 -72.35(13) . . . . ? P2 Ag2 P3 C38 -15.27(16) . . . . ? Br2 Ag2 P3 C38 -137.77(15) . . . . ? Br1 Ag2 P3 C38 109.58(15) . . . . ? Ag1 Ag2 P3 C38 -174.12(15) 1_545 . . . ? Ag1 Ag2 P3 C38 48.30(15) . . . . ? P3 Ag2 P2 C19 -110.68(15) . . . . ? Br2 Ag2 P2 C19 12.72(15) . . . . ? Br1 Ag2 P2 C19 114.28(15) . . . . ? Ag1 Ag2 P2 C19 62.36(15) 1_545 . . . ? Ag1 Ag2 P2 C19 -146.17(15) . . . . ? P3 Ag2 P2 C13 121.82(16) . . . . ? Br2 Ag2 P2 C13 -114.79(16) . . . . ? Br1 Ag2 P2 C13 -13.22(17) . . . . ? Ag1 Ag2 P2 C13 -65.14(16) 1_545 . . . ? Ag1 Ag2 P2 C13 86.33(16) . . . . ? P3 Ag2 P2 C39 1.18(14) . . . . ? Br2 Ag2 P2 C39 124.57(14) . . . . ? Br1 Ag2 P2 C39 -133.87(14) . . . . ? Ag1 Ag2 P2 C39 174.21(14) 1_545 . . . ? Ag1 Ag2 P2 C39 -34.32(14) . . . . ? C31 P3 C25 C30 -121.6(3) . . . . ? C38 P3 C25 C30 129.8(3) . . . . ? Ag2 P3 C25 C30 4.5(4) . . . . ? C31 P3 C25 C26 58.9(4) . . . . ? C38 P3 C25 C26 -49.7(4) . . . . ? Ag2 P3 C25 C26 -175.0(3) . . . . ? C21 C20 C19 C24 -3.3(7) . . . . ? C21 C20 C19 P2 -177.7(4) . . . . ? C13 P2 C19 C24 14.3(4) . . . . ? C39 P2 C19 C24 121.8(4) . . . . ? Ag2 P2 C19 C24 -123.1(3) . . . . ? C13 P2 C19 C20 -171.7(4) . . . . ? C39 P2 C19 C20 -64.2(4) . . . . ? Ag2 P2 C19 C20 51.0(4) . . . . ? C19 P2 C13 C18 -124.7(4) . . . . ? C39 P2 C13 C18 128.6(4) . . . . ? Ag2 P2 C13 C18 6.0(4) . . . . ? C19 P2 C13 C14 57.2(4) . . . . ? C39 P2 C13 C14 -49.5(4) . . . . ? Ag2 P2 C13 C14 -172.1(3) . . . . ? C14 C13 C18 C17 0.7(7) . . . . ? P2 C13 C18 C17 -177.5(4) . . . . ? C20 C19 C24 C23 3.1(7) . . . . ? P2 C19 C24 C23 177.3(4) . . . . ? C28 C27 C26 C25 0.1(7) . . . . ? C30 C25 C26 C27 0.8(6) . . . . ? P3 C25 C26 C27 -179.7(3) . . . . ? C18 C13 C14 C15 0.3(7) . . . . ? P2 C13 C14 C15 178.5(4) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C13 C18 C17 C16 -1.2(8) . . . . ? C19 P2 C39 C40 165.1(3) . . . . ? C13 P2 C39 C40 -86.4(3) . . . . ? Ag2 P2 C39 C40 46.7(3) . . . . ? C25 P3 C38 C40 -138.5(3) . . . . ? C31 P3 C38 C40 113.3(3) . . . . ? Ag2 P3 C38 C40 -11.9(4) . . . . ? C25 P3 C31 C36 108.0(3) . . . . ? C38 P3 C31 C36 -146.4(3) . . . . ? Ag2 P3 C31 C36 -20.2(3) . . . . ? C25 P3 C31 C32 -71.8(4) . . . . ? C38 P3 C31 C32 33.8(4) . . . . ? Ag2 P3 C31 C32 160.0(3) . . . . ? C32 C31 C36 C35 1.4(6) . . . . ? P3 C31 C36 C35 -178.4(3) . . . . ? C36 C31 C32 C33 -0.4(6) . . . . ? P3 C31 C32 C33 179.3(3) . . . . ? C26 C27 C28 C29 -1.2(7) . . . . ? C26 C25 C30 C29 -0.6(6) . . . . ? P3 C25 C30 C29 179.9(4) . . . . ? C27 C28 C29 C30 1.5(7) . . . . ? C25 C30 C29 C28 -0.6(7) . . . . ? C19 C20 C21 C22 1.5(8) . . . . ? C23 C22 C21 C20 0.7(8) . . . . ? C31 C32 C33 C34 0.0(7) . . . . ? C21 C22 C23 C24 -0.9(8) . . . . ? C19 C24 C23 C22 -1.1(8) . . . . ? C31 C36 C35 C34 -1.8(7) . . . . ? C36 C35 C34 C33 1.4(8) . . . . ? C32 C33 C34 C35 -0.5(8) . . . . ? C18 C17 C16 C15 0.6(9) . . . . ? C14 C15 C16 C17 0.4(9) . . . . ? P3 C38 C40 C37 -58.9(4) . . . . ? P3 C38 C40 C41 179.7(3) . . . . ? P3 C38 C40 C39 64.3(4) . . . . ? P2 C39 C40 C37 34.9(4) . . . . ? P2 C39 C40 C41 154.9(3) . . . . ? P2 C39 C40 C38 -89.6(4) . . . . ? C41 C40 C37 P1 51.9(4) . . . . ? C38 C40 C37 P1 -66.6(4) . . . . ? C39 C40 C37 P1 168.7(3) . . . . ? C7 P1 C37 C40 131.2(3) . . . . ? C1 P1 C37 C40 -123.7(3) . . . . ? Ag1 P1 C37 C40 7.4(4) . . . . ? P2 Ag2 Br1 Ag1 -85.52(3) . . . 1_545 ? P3 Ag2 Br1 Ag1 155.58(3) . . . 1_545 ? Br2 Ag2 Br1 Ag1 31.642(19) . . . 1_545 ? Ag1 Ag2 Br1 Ag1 -169.437(14) . . . 1_545 ? C1 P1 C7 C12 -84.4(4) . . . . ? C37 P1 C7 C12 21.4(4) . . . . ? Ag1 P1 C7 C12 155.2(4) . . . . ? C1 P1 C7 C8 93.9(4) . . . . ? C37 P1 C7 C8 -160.3(4) . . . . ? Ag1 P1 C7 C8 -26.5(4) . . . . ? C7 P1 C1 C2 -116.4(4) . . . . ? C37 P1 C1 C2 135.4(4) . . . . ? Ag1 P1 C1 C2 -1.1(4) . . . . ? C7 P1 C1 C6 61.7(4) . . . . ? C37 P1 C1 C6 -46.5(4) . . . . ? Ag1 P1 C1 C6 177.0(3) . . . . ? C8 C7 C12 C11 -0.7(7) . . . . ? P1 C7 C12 C11 177.6(4) . . . . ? C12 C7 C8 C9 0.1(7) . . . . ? P1 C7 C8 C9 -178.3(4) . . . . ? C6 C1 C2 C3 -0.4(7) . . . . ? P1 C1 C2 C3 177.7(4) . . . . ? C7 C12 C11 C10 0.0(8) . . . . ? C2 C1 C6 C5 0.7(7) . . . . ? P1 C1 C6 C5 -177.5(4) . . . . ? C12 C11 C10 C9 1.4(8) . . . . ? C11 C10 C9 C8 -2.0(9) . . . . ? C7 C8 C9 C10 1.3(9) . . . . ? C5 C4 C3 C2 1.8(8) . . . . ? C1 C2 C3 C4 -0.8(8) . . . . ? C3 C4 C5 C6 -1.5(8) . . . . ? C1 C6 C5 C4 0.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.626 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.102