Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_pm2am _publ_contact_author 'Stuart L. James' _publ_contact_author_email 'S.James@qub.ac.uk' loop_ _publ_author_name 'Philip Miller' 'Xingling Xu' 'Mark Nieuwenhuyzen' 'Stuart L. James' _journal_name_full Chemical Communications _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C326 H270 Ag6 N6 O18 P12' _chemical_formula_weight 5578.34 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 30.564(5) _cell_length_b 30.564(5) _cell_length_c 30.564(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 28553(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11496 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8649 _exptl_absorpt_correction_T_max 0.9147 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42984 _diffrn_reflns_av_R_equivalents 0.3440 _diffrn_reflns_av_sigmaI/netI 0.3311 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 20.00 _reflns_number_total 8890 _reflns_number_gt 2997 _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, 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^)+(0.1554P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(11) _refine_ls_number_reflns 8890 _refine_ls_number_parameters 323 _refine_ls_number_restraints 974 _refine_ls_R_factor_all 0.2734 _refine_ls_R_factor_gt 0.1159 _refine_ls_wR_factor_ref 0.3419 _refine_ls_wR_factor_gt 0.2738 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 2.608 _refine_ls_shift/su_mean 0.070 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 3.07673(8) 0.93128(9) 0.93242(8) 0.0875(9) Uani 1 1 d . . . Ag2 Ag 3.12897(8) 0.98211(9) 1.10152(8) 0.0918(10) Uani 1 1 d . . . P1 P 3.0142(3) 0.9092(3) 0.8893(3) 0.087(3) Uani 1 1 d . . . P2 P 3.1520(3) 0.9427(3) 0.9201(3) 0.097(3) Uani 1 1 d . . . P3 P 3.1077(3) 0.9422(4) 1.1668(3) 0.106(4) Uani 1 1 d . . . P4 P 3.1949(3) 1.0032(3) 1.0646(3) 0.091(3) Uani 1 1 d . . . C1 C 3.1666(8) 0.9670(6) 0.8648(5) 0.087(10) Uiso 1 1 d GDU . . C2 C 3.1291(6) 0.9829(7) 0.8427(7) 0.120(12) Uiso 1 1 d GDU . . H2 H 3.1008 0.9779 0.8546 0.144 Uiso 1 1 calc R . . C3 C 3.1337(6) 1.0060(7) 0.8033(7) 0.155(15) Uiso 1 1 d GDU . . H3 H 3.1093 1.0183 0.7884 0.186 Uiso 1 1 calc R . . C4 C 3.1751(7) 1.0099(6) 0.7878(5) 0.097(11) Uiso 1 1 d GDU . . C5 C 3.2145(6) 0.9989(8) 0.8078(7) 0.158(15) Uiso 1 1 d GDU . . H5 H 3.2425 1.0061 0.7963 0.190 Uiso 1 1 calc R . . C6 C 3.2076(7) 0.9738(7) 0.8508(7) 0.102(11) Uiso 1 1 d GDU . . H6 H 3.2318 0.9633 0.8671 0.123 Uiso 1 1 calc R . . C7 C 3.1783(9) 1.0403(9) 0.7466(7) 0.175(16) Uiso 1 1 d GDU . . C8 C 3.1450(8) 1.0312(10) 0.7157(10) 0.23(2) Uiso 1 1 d GDU . . H8 H 3.1213 1.0127 0.7234 0.279 Uiso 1 1 calc R . . C9 C 3.1472(11) 1.0498(12) 0.6735(8) 0.26(2) Uiso 1 1 d GDU . . H9 H 3.1259 1.0452 0.6514 0.318 Uiso 1 1 calc R . . C10 C 3.1829(12) 1.0748(10) 0.6682(7) 0.218(19) Uiso 1 1 d GDU . . H10 H 3.1865 1.0847 0.6390 0.262 Uiso 1 1 calc R . . C11 C 3.2160(11) 1.0895(9) 0.6959(11) 0.23(2) Uiso 1 1 d GDU . . H11 H 3.2362 1.1121 0.6893 0.279 Uiso 1 1 calc R . . C12 C 3.2147(9) 1.0630(9) 0.7391(9) 0.207(19) Uiso 1 1 d GDU . . H12 H 3.2385 1.0629 0.7591 0.249 Uiso 1 1 calc R . . C13 C 3.0260(9) 0.9178(8) 0.8295(6) 0.101(11) Uiso 1 1 d GDU . . C14 C 3.0570(9) 0.8905(7) 0.8088(8) 0.179(17) Uiso 1 1 d GDU . . H14 H 3.0681 0.8658 0.8240 0.215 Uiso 1 1 calc R . . C15 C 3.0718(8) 0.8992(9) 0.7658(9) 0.231(19) Uiso 1 1 d GDU . . H15 H 3.0926 0.8815 0.7510 0.277 Uiso 1 1 calc R . . C16 C 3.0536(8) 0.9351(9) 0.7479(6) 0.166(15) Uiso 1 1 d GDU . . C17 C 3.0227(8) 0.9640(7) 0.7645(7) 0.127(13) Uiso 1 1 d GDU . . H17 H 3.0122 0.9887 0.7489 0.152 Uiso 1 1 calc R . . C18 C 3.0077(7) 0.9520(8) 0.8104(7) 0.125(13) Uiso 1 1 d GDU . . H18 H 2.9857 0.9685 0.8249 0.150 Uiso 1 1 calc R . . C19 C 3.0657(11) 0.9450(12) 0.6986(7) 0.238(19) Uiso 1 1 d GDU . . C20 C 3.1026(11) 0.9226(12) 0.6814(11) 0.32(3) Uiso 1 1 d GDU . . H20 H 3.1186 0.9032 0.6996 0.386 Uiso 1 1 calc R . . C21 C 3.1156(12) 0.9288(14) 0.6375(12) 0.34(3) Uiso 1 1 d GDU . . H21 H 3.1398 0.9138 0.6250 0.407 Uiso 1 1 calc R . . C22 C 3.0914(15) 0.9574(14) 0.6146(8) 0.30(3) Uiso 1 1 d GDU . . H22 H 3.1015 0.9629 0.5858 0.363 Uiso 1 1 calc R . . C23 C 3.0536(15) 0.9803(13) 0.6264(11) 0.32(3) Uiso 1 1 d GDU . . H23 H 3.0370 0.9979 0.6069 0.390 Uiso 1 1 calc R . . C24 C 3.0419(11) 0.9736(11) 0.6752(11) 0.31(3) Uiso 1 1 d GDU . . H24 H 3.0185 0.9893 0.6883 0.373 Uiso 1 1 calc R . . C25 C 3.0077(7) 0.8494(5) 0.8895(7) 0.086(10) Uiso 1 1 d GDU . . C26 C 2.9723(7) 0.8286(7) 0.8680(7) 0.138(13) Uiso 1 1 d GDU . . H26 H 2.9527 0.8447 0.8500 0.165 Uiso 1 1 calc R . . C27 C 2.9669(6) 0.7826(7) 0.8743(7) 0.126(13) Uiso 1 1 d GDU . . H27 H 2.9439 0.7665 0.8610 0.152 Uiso 1 1 calc R . . C28 C 2.9966(7) 0.7639(5) 0.9003(7) 0.133(13) Uiso 1 1 d GDU . . C29 C 3.0342(7) 0.7805(7) 0.9224(7) 0.109(11) Uiso 1 1 d GDU . . H29 H 3.0545 0.7635 0.9386 0.131 Uiso 1 1 calc R . . C30 C 3.0366(6) 0.8300(6) 0.9159(7) 0.104(11) Uiso 1 1 d GDU . . H30 H 3.0584 0.8468 0.9304 0.125 Uiso 1 1 calc R . . C31 C 2.9959(10) 0.7117(6) 0.9025(9) 0.168(15) Uiso 1 1 d GDU . . C32 C 2.9542(9) 0.6922(10) 0.9041(11) 0.27(2) Uiso 1 1 d GDU . . H32 H 2.9289 0.7091 0.8977 0.330 Uiso 1 1 calc R . . C33 C 2.9499(12) 0.6476(11) 0.9151(13) 0.36(3) Uiso 1 1 d GDU . . H33 H 2.9223 0.6336 0.9177 0.438 Uiso 1 1 calc R . . C34 C 2.9879(15) 0.6264(6) 0.9215(11) 0.28(2) Uiso 1 1 d GDU . . H34 H 2.9852 0.5956 0.9239 0.336 Uiso 1 1 calc R . . C35 C 3.0306(13) 0.6421(10) 0.9253(12) 0.29(2) Uiso 1 1 d GDU . . H35 H 3.0548 0.6251 0.9349 0.349 Uiso 1 1 calc R . . C36 C 3.0333(8) 0.6909(10) 0.9119(12) 0.27(2) Uiso 1 1 d GDU . . H36 H 3.0607 0.7056 0.9103 0.320 Uiso 1 1 calc R . . C37 C 3.1756(9) 0.8878(6) 0.9206(10) 0.109(12) Uiso 1 1 d GDU . . C38 C 3.2087(9) 0.8734(8) 0.9498(8) 0.167(16) Uiso 1 1 d GDU . . H38 H 3.2200 0.8931 0.9710 0.200 Uiso 1 1 calc R . . C39 C 3.2249(8) 0.8305(9) 0.9476(8) 0.189(17) Uiso 1 1 d GDU . . H39 H 3.2455 0.8194 0.9680 0.227 Uiso 1 1 calc R . . C40 C 3.2092(9) 0.8064(6) 0.9145(9) 0.181(16) Uiso 1 1 d GDU . . C41 C 3.1713(9) 0.8142(8) 0.8899(8) 0.178(17) Uiso 1 1 d GDU . . H41 H 3.1542 0.7920 0.8764 0.214 Uiso 1 1 calc R . . C42 C 3.1610(8) 0.8635(9) 0.8876(9) 0.206(18) Uiso 1 1 d GDU . . H42 H 3.1452 0.8759 0.8639 0.247 Uiso 1 1 calc R . . C43 C 3.2245(9) 0.7562(7) 0.9137(10) 0.177(15) Uiso 1 1 d GDU . . C44 C 3.2627(8) 0.7463(8) 0.9378(8) 0.139(14) Uiso 1 1 d GDU . . H44 H 3.2775 0.7683 0.9540 0.167 Uiso 1 1 calc R . . C45 C 3.2786(8) 0.7026(10) 0.9373(9) 0.182(17) Uiso 1 1 d GDU . . H45 H 3.3039 0.6937 0.9530 0.218 Uiso 1 1 calc R . . C46 C 3.2551(11) 0.6749(6) 0.9132(10) 0.22(2) Uiso 1 1 d GDU . . H46 H 3.2675 0.6465 0.9109 0.264 Uiso 1 1 calc R . . C47 C 3.2158(12) 0.6798(9) 0.8905(11) 0.33(3) Uiso 1 1 d GDU . . H47 H 3.1992 0.6564 0.8785 0.395 Uiso 1 1 calc R . . C48 C 3.2031(9) 0.7284(10) 0.8879(10) 0.27(2) Uiso 1 1 d GDU . . H48 H 3.1808 0.7382 0.8686 0.326 Uiso 1 1 calc R . . C49 C 3.2326(8) 0.9520(6) 1.0579(8) 0.133(13) Uiso 1 1 d GDU . . C50 C 3.2137(6) 0.9117(8) 1.0715(7) 0.111(11) Uiso 1 1 d GDU . . H50 H 3.1846 0.9115 1.0825 0.134 Uiso 1 1 calc R . . C51 C 3.2371(7) 0.8722(6) 1.0692(7) 0.117(12) Uiso 1 1 d GDU . . H51 H 3.2257 0.8449 1.0787 0.140 Uiso 1 1 calc R . . C52 C 3.2772(7) 0.8771(6) 1.0521(7) 0.114(12) Uiso 1 1 d GDU . . C53 C 3.3007(6) 0.9146(8) 1.0408(8) 0.173(16) Uiso 1 1 d GDU . . H53 H 3.3311 0.9146 1.0343 0.207 Uiso 1 1 calc R . . C54 C 3.2722(9) 0.9560(6) 1.0400(8) 0.138(14) Uiso 1 1 d GDU . . H54 H 3.2821 0.9828 1.0276 0.165 Uiso 1 1 calc R . . C55 C 3.3064(9) 0.8340(7) 1.0485(10) 0.186(16) Uiso 1 1 d GDU . . C56 C 3.2896(9) 0.7959(10) 1.0685(9) 0.224(19) Uiso 1 1 d GDU . . H56 H 3.2670 0.7985 1.0897 0.269 Uiso 1 1 calc R . . C57 C 3.3056(11) 0.7538(7) 1.0578(12) 0.221(19) Uiso 1 1 d GDU . . H57 H 3.2941 0.7275 1.0698 0.265 Uiso 1 1 calc R . . C58 C 3.3387(11) 0.7547(8) 1.0289(12) 0.22(2) Uiso 1 1 d GDU . . H58 H 3.3537 0.7277 1.0255 0.259 Uiso 1 1 calc R . . C59 C 3.3545(10) 0.7884(12) 1.0033(10) 0.29(2) Uiso 1 1 d GDU . . H59 H 3.3722 0.7844 0.9782 0.353 Uiso 1 1 calc R . . C60 C 3.3399(9) 0.8335(9) 1.0206(11) 0.25(2) Uiso 1 1 d GDU . . H60 H 3.3541 0.8597 1.0117 0.301 Uiso 1 1 calc R . . C61 C 3.1296(9) 0.8869(6) 1.1688(8) 0.109(11) Uiso 1 1 d GDU . . C62 C 3.1686(9) 0.8764(7) 1.1919(8) 0.164(15) Uiso 1 1 d GDU . . H62 H 3.1824 0.8980 1.2094 0.197 Uiso 1 1 calc R . . C63 C 3.1869(7) 0.8342(9) 1.1892(7) 0.157(15) Uiso 1 1 d GDU . . H63 H 3.2128 0.8263 1.2047 0.189 Uiso 1 1 calc R . . C64 C 3.1656(7) 0.8062(6) 1.1636(7) 0.108(11) Uiso 1 1 d GDU . . C65 C 3.1275(8) 0.8115(7) 1.1390(7) 0.145(14) Uiso 1 1 d GDU . . H65 H 3.1151 0.7894 1.1210 0.174 Uiso 1 1 calc R . . C66 C 3.1084(7) 0.8573(8) 1.1446(8) 0.132(13) Uiso 1 1 d GDU . . H66 H 3.0814 0.8647 1.1310 0.158 Uiso 1 1 calc R . . C67 C 3.1913(10) 0.7619(8) 1.1558(11) 0.210(18) Uiso 1 1 d GDU . . C68 C 3.1659(9) 0.7235(11) 1.1523(13) 0.31(2) Uiso 1 1 d GDU . . H68 H 3.1349 0.7255 1.1527 0.372 Uiso 1 1 calc R . . C69 C 3.1858(14) 0.6822(8) 1.1484(13) 0.30(2) Uiso 1 1 d GDU . . H69 H 3.1703 0.6559 1.1425 0.358 Uiso 1 1 calc R . . C70 C 3.2295(14) 0.6842(9) 1.1539(10) 0.202(19) Uiso 1 1 d GDU . . H70 H 3.2425 0.6579 1.1641 0.243 Uiso 1 1 calc R . . C71 C 3.2585(9) 0.7184(14) 1.1472(13) 0.32(3) Uiso 1 1 d GDU . . H71 H 3.2884 0.7152 1.1390 0.383 Uiso 1 1 calc R . . C72 C 3.2350(10) 0.7626(10) 1.1549(13) 0.35(3) Uiso 1 1 d GDU . . H72 H 3.2509 0.7890 1.1588 0.418 Uiso 1 1 calc R . . C73 C 3.2265(11) 1.0465(10) 1.0999(9) 0.206(18) Uiso 1 1 d GDU . . C74 C 3.2102(7) 1.0897(11) 1.1073(8) 0.128(13) Uiso 1 1 d GDU . . H74 H 3.1860 1.1000 1.0907 0.154 Uiso 1 1 calc R . . C75 C 3.2294(9) 1.1173(8) 1.1389(9) 0.174(17) Uiso 1 1 d GDU . . H75 H 3.2205 1.1468 1.1429 0.208 Uiso 1 1 calc R . . C76 C 3.2613(9) 1.0988(9) 1.1629(8) 0.221(18) Uiso 1 1 d GDU . . C77 C 3.2832(9) 1.0592(10) 1.1560(10) 0.27(2) Uiso 1 1 d GDU . . H77 H 3.3094 1.0512 1.1707 0.322 Uiso 1 1 calc R . . C78 C 3.2604(12) 1.0300(8) 1.1220(11) 0.26(2) Uiso 1 1 d GDU . . H78 H 3.2701 1.0010 1.1168 0.317 Uiso 1 1 calc R . . C79 C 3.2839(10) 1.1286(10) 1.1990(9) 0.219(18) Uiso 1 1 d GDU . . C80 C 3.2915(12) 1.1073(10) 1.2401(11) 0.28(2) Uiso 1 1 d GDU . . H80 H 3.2857 1.0770 1.2433 0.334 Uiso 1 1 calc R . . C81 C 3.3077(12) 1.1318(15) 1.2757(9) 0.30(3) Uiso 1 1 d GDU . . H81 H 3.3137 1.1194 1.3036 0.365 Uiso 1 1 calc R . . C82 C 3.3139(11) 1.1744(14) 1.2666(12) 0.30(3) Uiso 1 1 d GDU . . H82 H 3.3236 1.1909 1.2911 0.361 Uiso 1 1 calc R . . C83 C 3.3090(13) 1.1993(9) 1.2288(16) 0.31(3) Uiso 1 1 d GDU . . H83 H 3.3159 1.2295 1.2266 0.373 Uiso 1 1 calc R . . C84 C 3.2910(12) 1.1710(11) 1.1910(11) 0.29(2) Uiso 1 1 d GDU . . H84 H 3.2853 1.1833 1.1630 0.350 Uiso 1 1 calc R . . C85 C 3.1325(8) 0.9712(10) 1.2178(7) 0.124(12) Uiso 1 1 d GDU . . C86 C 3.1190(8) 0.9498(8) 1.2567(10) 0.181(17) Uiso 1 1 d GDU . . H86 H 3.1031 0.9231 1.2557 0.217 Uiso 1 1 calc R . . C87 C 3.1299(9) 0.9697(10) 1.2974(8) 0.190(17) Uiso 1 1 d GDU . . H87 H 3.1227 0.9574 1.3251 0.228 Uiso 1 1 calc R . . C88 C 3.1512(9) 1.0075(9) 1.2925(7) 0.221(18) Uiso 1 1 d GDU . . C89 C 3.1686(9) 1.0314(8) 1.2571(10) 0.207(18) Uiso 1 1 d GDU . . H89 H 3.1862 1.0569 1.2592 0.248 Uiso 1 1 calc R . . C90 C 3.1541(9) 1.0088(10) 1.2140(7) 0.149(14) Uiso 1 1 d GDU . . H90 H 3.1603 1.0213 1.1862 0.179 Uiso 1 1 calc R . . C91 C 3.1604(13) 1.0313(11) 1.3383(8) 0.35(2) Uiso 1 1 d GDU . . C92 C 3.1604(15) 1.0016(11) 1.3740(12) 0.40(3) Uiso 1 1 d GDU . . H92 H 3.1518 0.9720 1.3703 0.476 Uiso 1 1 calc R . . C93 C 3.1737(14) 1.0177(16) 1.4154(9) 0.37(3) Uiso 1 1 d GDU . . H93 H 3.1758 1.0004 1.4411 0.441 Uiso 1 1 calc R . . C94 C 3.1831(11) 1.0606(16) 1.4134(10) 0.26(2) Uiso 1 1 d GDU . . H94 H 3.1896 1.0720 1.4416 0.314 Uiso 1 1 calc R . . C95 C 3.1858(13) 1.0930(12) 1.3815(15) 0.32(3) Uiso 1 1 d GDU . . H95 H 3.1938 1.1226 1.3865 0.387 Uiso 1 1 calc R . . C96 C 3.1735(14) 1.0730(11) 1.3367(11) 0.32(3) Uiso 1 1 d GDU . . H96 H 3.1752 1.0890 1.3102 0.387 Uiso 1 1 calc R . . C1A C 3.1867(9) 0.9705(8) 0.9610(9) 0.067(9) Uiso 1 1 d D . . H1A1 H 3.1886 0.9517 0.9873 0.081 Uiso 1 1 calc R . . H1A2 H 3.2166 0.9733 0.9489 0.081 Uiso 1 1 calc R . . C2A C 3.1771(10) 1.0480(8) 0.9353(9) 0.082(10) Uiso 1 1 d D . . H2A1 H 3.1579 1.0375 0.9114 0.099 Uiso 1 1 calc R . . H2A2 H 3.2076 1.0445 0.9251 0.099 Uiso 1 1 calc R . . C3A C 2.9626(8) 0.9334(10) 0.8956(7) 0.078(9) Uiso 1 1 d D . . H3A1 H 2.9638 0.9621 0.8806 0.093 Uiso 1 1 calc R . . H3A2 H 2.9416 0.9151 0.8789 0.093 Uiso 1 1 calc R . . C4A C 2.9716(7) 0.9716(7) 0.9716(7) 0.064(15) Uiso 1 3 d SD . . H4A1 H 2.9547 0.9969 0.9816 0.096 Uiso 0.33 1 calc PR . . H4A2 H 2.9969 0.9816 0.9547 0.096 Uiso 0.33 1 calc PR . . H4A3 H 2.9816 0.9547 0.9969 0.096 Uiso 0.33 1 calc PR . . C5A C 3.1975(9) 1.0334(9) 1.0147(9) 0.086(10) Uiso 1 1 d D . . H5A1 H 3.1881 1.0638 1.0211 0.103 Uiso 1 1 calc R . . H5A2 H 3.2285 1.0347 1.0056 0.103 Uiso 1 1 calc R . . C6A C 2.9417(6) 0.9417(6) 0.9417(6) 0.066(15) Uiso 1 3 d SD . . C7A C 3.1209(8) 1.0164(10) 0.9890(10) 0.102(11) Uiso 1 1 d D . . H7A1 H 3.1138 0.9881 1.0023 0.153 Uiso 1 1 calc R . . H7A2 H 3.1025 1.0209 0.9631 0.153 Uiso 1 1 calc R . . H7A3 H 3.1155 1.0398 1.0102 0.153 Uiso 1 1 calc R . . C8A C 3.1705(7) 1.0169(7) 0.9752(7) 0.071(9) Uiso 1 1 d D . . N1 N 3.0587(13) 0.9092(12) 1.0308(13) 0.136(13) Uiso 1 1 d D . . O11 O 3.0490(11) 0.8952(11) 1.0692(12) 0.203(13) Uiso 1 1 d D . . O12 O 3.0507(8) 0.8953(9) 0.9989(10) 0.131(10) Uiso 1 1 d . . . O13 O 3.0967(10) 0.9231(9) 1.0358(8) 0.146(10) Uiso 1 1 d . . . N2 N 3.0927(8) 1.0927(8) 1.0927(8) 0.095(15) Uiso 1 3 d SD . . O21 O 3.1162(6) 1.0951(6) 1.0582(6) 0.099(7) Uiso 1 1 d D . . N3 N 2.8593(11) 0.8593(11) 0.8593(11) 0.14(2) Uiso 1 3 d SD . . O31 O 2.8586(10) 0.8253(8) 0.8844(9) 0.175(12) Uiso 1 1 d D . . N4 N 3.172(3) 0.828(3) 1.328(3) 0.54(7) Uiso 1 3 d SD . . O41 O 3.1769(12) 0.7972(10) 1.3587(12) 0.224(15) Uiso 1 1 d D . . C1S C 3.1599(8) 0.7701(13) 1.0174(12) 0.38(4) Uiso 1 1 d GDU . . H1S H 3.1889 0.7813 1.0180 0.454 Uiso 1 1 calc R . . C2S C 3.1249(13) 0.8006(8) 1.0214(10) 0.146(15) Uiso 1 1 d GDU . . H2S H 3.1295 0.8312 1.0186 0.176 Uiso 1 1 calc R . . C3S C 3.0834(10) 0.7834(12) 1.0297(9) 0.20(2) Uiso 1 1 d GDU . . H3S H 3.0579 0.8011 1.0290 0.237 Uiso 1 1 calc R . . C4S C 3.0816(9) 0.7407(12) 1.0385(9) 0.182(19) Uiso 1 1 d GDU . . H4S H 3.0579 0.7316 1.0565 0.218 Uiso 1 1 calc R . . C5S C 3.1103(15) 0.7071(8) 1.0249(11) 0.22(2) Uiso 1 1 d GDU . . H5S H 3.1031 0.6769 1.0233 0.270 Uiso 1 1 calc R . . C6S C 3.1551(11) 0.7269(13) 1.0130(12) 0.26(3) Uiso 1 1 d GDU . . H6S H 3.1784 0.7090 1.0028 0.315 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 0.079(2) 0.104(2) 0.079(2) 0.0001(18) 0.0007(16) 0.0104(17) Ag2 0.082(2) 0.113(2) 0.080(2) 0.0040(17) -0.0021(16) 0.0127(17) P1 0.087(7) 0.099(8) 0.074(7) -0.005(5) 0.001(6) 0.005(6) P2 0.097(8) 0.107(8) 0.088(8) 0.026(6) 0.004(6) 0.017(6) P3 0.085(8) 0.169(11) 0.064(7) 0.027(7) 0.008(6) 0.018(7) P4 0.082(7) 0.081(7) 0.110(8) 0.015(6) 0.006(6) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.357(10) . ? Ag1 P1 2.419(10) . ? Ag1 O12 2.44(3) . ? Ag2 P4 2.397(10) . ? Ag2 P3 2.428(10) . ? Ag2 O21 2.585(18) 9_753 ? P1 C3A 1.75(3) . ? P1 C25 1.839(17) . ? P1 C13 1.881(19) . ? P2 C37 1.824(19) . ? P2 C1A 1.85(3) . ? P2 C1 1.900(17) . ? P3 C61 1.817(19) . ? P3 C2A 1.86(3) 9_753 ? P3 C85 1.95(2) . ? P4 C5A 1.79(3) . ? P4 C49 1.954(17) . ? P4 C73 1.96(2) . ? C1 C6 1.3380 . ? C1 C2 1.4169 . ? C2 C3 1.4053 . ? C3 C4 1.3564 . ? C4 C5 1.3922 . ? C4 C7 1.569(12) . ? C5 C6 1.5355 . ? C7 C12 1.3298 . ? C7 C8 1.4148 . ? C8 C9 1.4116 . ? C9 C10 1.3420 . ? C10 C11 1.3917 . ? C11 C12 1.5499 . ? C13 C18 1.3214 . ? C13 C14 1.4119 . ? C14 C15 1.4145 . ? C15 C16 1.3442 . ? C16 C17 1.3891 . ? C16 C19 1.584(14) . ? C17 C18 1.5210 . ? C19 C24 1.3416 . ? C19 C20 1.4190 . ? C20 C21 1.4126 . ? C21 C22 1.3419 . ? C22 C23 1.3996 . ? C23 C24 1.5463 . ? C25 C30 1.3354 . ? C25 C26 1.4169 . ? C26 C27 1.4275 . ? C27 C28 1.3343 . ? C28 C29 1.4263 . ? C28 C31 1.596(14) . ? C29 C30 1.5272 . ? C31 C36 1.3400 . ? C31 C32 1.4069 . ? C32 C33 1.4102 . ? C33 C34 1.3428 . ? C34 C35 1.3953 . ? C35 C36 1.5509 . ? C37 C42 1.3311 . ? C37 C38 1.4171 . ? C38 C39 1.4036 . ? C39 C40 1.3399 . ? C40 C41 1.4025 . ? C40 C43 1.603(14) . ? C41 C42 1.5410 . ? C43 C48 1.3328 . ? C43 C44 1.4136 . ? C44 C45 1.4205 . ? C45 C46 1.3323 . ? C46 C47 1.3940 . ? C47 C48 1.5375 . ? C49 C54 1.3333 . ? C49 C50 1.4217 . ? C50 C51 1.4055 . ? C51 C52 1.3414 . ? C52 C53 1.3965 . ? C52 C55 1.594(14) . ? C53 C54 1.5379 . ? C55 C60 1.3320 . ? C55 C56 1.4145 . ? C56 C57 1.4150 . ? C57 C58 1.3406 . ? C58 C59 1.3826 . ? C59 C60 1.5402 . ? C61 C66 1.3375 . ? C61 C62 1.4224 . ? C62 C63 1.4063 . ? C63 C64 1.3331 . ? C64 C65 1.3939 . ? C64 C67 1.583(14) . ? C65 C66 1.5274 . ? C67 C72 1.3382 . ? C67 C68 1.4093 . ? C68 C69 1.4068 . ? C69 C70 1.3456 . ? C70 C71 1.3871 . ? C71 C72 1.5464 . ? C73 C78 1.3341 . ? C73 C74 1.4295 . ? C74 C75 1.4094 . ? C75 C76 1.3426 . ? C76 C77 1.3994 . ? C76 C79 1.591(14) . ? C77 C78 1.5382 . ? C79 C84 1.3390 . ? C79 C80 1.4315 . ? C80 C81 1.4115 . ? C81 C82 1.3435 . ? C82 C83 1.3920 . ? C83 C84 1.5448 . ? C85 C90 1.3303 . ? C85 C86 1.4192 . ? C86 C87 1.4238 . ? C87 C88 1.3340 . ? C88 C89 1.4115 . ? C88 C91 1.601(14) . ? C89 C90 1.5510 . ? C91 C96 1.3355 . ? C91 C92 1.4210 . ? C92 C93 1.4167 . ? C93 C94 1.3445 . ? C94 C95 1.3919 . ? C95 C96 1.5455 . ? C1A C8A 1.564(17) . ? C2A C8A 1.559(17) . ? C2A P3 1.86(3) 5_735 ? C3A C6A 1.568(17) . ? C4A C6A 1.584(19) . ? C5A C8A 1.548(17) . ? C6A C3A 1.568(17) 9_753 ? C6A C3A 1.568(17) 5_735 ? C7A C8A 1.574(17) . ? N1 O12 1.09(4) . ? N1 O13 1.25(4) . ? N1 O11 1.28(2) . ? N2 O21 1.278(16) . ? N2 O21 1.278(16) 9_753 ? N2 O21 1.279(16) 5_735 ? O21 Ag2 2.585(18) 5_735 ? N3 O31 1.290(19) 9_753 ? N3 O31 1.291(19) . ? N3 O31 1.292(19) 5_735 ? N4 O41 1.35(2) 7_995 ? N4 O41 1.33(2) 10_949 ? N4 O41 1.34(2) . ? C1S C6S 1.3361 . ? C1S C2S 1.4260 . ? C2S C3S 1.3956 . ? C3S C4S 1.3350 . ? C4S C5S 1.4137 . ? C5S C6S 1.5385 . ? 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 136.5(3) . . ? P2 Ag1 O12 121.1(7) . . ? P1 Ag1 O12 94.0(7) . . ? P4 Ag2 P3 138.3(3) . . ? P4 Ag2 O21 100.2(5) . 9_753 ? P3 Ag2 O21 101.7(5) . 9_753 ? C3A P1 C25 108.9(13) . . ? C3A P1 C13 102.8(12) . . ? C25 P1 C13 99.3(11) . . ? C3A P1 Ag1 122.3(10) . . ? C25 P1 Ag1 111.1(9) . . ? C13 P1 Ag1 109.7(9) . . ? C37 P2 C1A 100.9(13) . . ? C37 P2 C1 106.0(12) . . ? C1A P2 C1 106.7(12) . . ? C37 P2 Ag1 104.4(9) . . ? C1A P2 Ag1 121.3(9) . . ? C1 P2 Ag1 115.5(9) . . ? C61 P3 C2A 104.5(13) . 9_753 ? C61 P3 C85 104.7(13) . . ? C2A P3 C85 107.3(13) 9_753 . ? C61 P3 Ag2 113.3(8) . . ? C2A P3 Ag2 117.2(10) 9_753 . ? C85 P3 Ag2 108.9(11) . . ? C5A P4 C49 107.3(13) . . ? C5A P4 C73 95.7(14) . . ? C49 P4 C73 107.9(14) . . ? C5A P4 Ag2 125.4(10) . . ? C49 P4 Ag2 109.3(9) . . ? C73 P4 Ag2 109.7(10) . . ? C6 C1 C2 123.6 . . ? C6 C1 P2 124.4(14) . . ? C2 C1 P2 111.5(14) . . ? C3 C2 C1 119.9 . . ? C4 C3 C2 116.0 . . ? C3 C4 C5 129.2 . . ? C3 C4 C7 113.0(14) . . ? C5 C4 C7 116.2(14) . . ? C4 C5 C6 112.1 . . ? C1 C6 C5 118.7 . . ? C12 C7 C8 126.2 . . ? C12 C7 C4 119.9(17) . . ? C8 C7 C4 111.9(17) . . ? C9 C8 C7 119.7 . . ? C10 C9 C8 112.1 . . ? C9 C10 C11 134.6 . . ? C10 C11 C12 109.3 . . ? C7 C12 C11 116.0 . . ? C18 C13 C14 123.6 . . ? C18 C13 P1 117.2(16) . . ? C14 C13 P1 118.8(16) . . ? C13 C14 C15 121.2 . . ? C16 C15 C14 113.6 . . ? C15 C16 C17 130.6 . . ? C15 C16 C19 116.6(14) . . ? C17 C16 C19 112.6(14) . . ? C16 C17 C18 112.8 . . ? C13 C18 C17 118.1 . . ? C24 C19 C20 123.2 . . ? C24 C19 C16 120.3(18) . . ? C20 C19 C16 116.5(18) . . ? C21 C20 C19 120.7 . . ? C22 C21 C20 115.2 . . ? C21 C22 C23 130.4 . . ? C22 C23 C24 111.8 . . ? C19 C24 C23 118.4 . . ? C30 C25 C26 126.0 . . ? C30 C25 P1 111.8(14) . . ? C26 C25 P1 121.7(14) . . ? C25 C26 C27 117.7 . . ? C28 C27 C26 115.2 . . ? C27 C28 C29 132.5 . . ? C27 C28 C31 116.4(13) . . ? C29 C28 C31 110.3(13) . . ? C28 C29 C30 109.3 . . ? C25 C30 C29 119.0 . . ? C36 C31 C32 124.3 . . ? C36 C31 C28 118.1(18) . . ? C32 C31 C28 116.0(18) . . ? C31 C32 C33 120.2 . . ? C34 C33 C32 114.8 . . ? C33 C34 C35 131.0 . . ? C34 C35 C36 110.9 . . ? C31 C36 C35 117.9 . . ? C42 C37 C38 122.8 . . ? C42 C37 P2 111.9(18) . . ? C38 C37 P2 124.9(18) . . ? C39 C38 C37 120.8 . . ? C40 C39 C38 115.1 . . ? C39 C40 C41 127.3 . . ? C39 C40 C43 115.7(15) . . ? C41 C40 C43 113.3(15) . . ? C40 C41 C42 111.1 . . ? C37 C42 C41 116.3 . . ? C48 C43 C44 125.2 . . ? C48 C43 C40 118.5(16) . . ? C44 C43 C40 116.1(16) . . ? C43 C44 C45 118.6 . . ? C46 C45 C44 114.7 . . ? C45 C46 C47 132.3 . . ? C46 C47 C48 110.2 . . ? C43 C48 C47 117.6 . . ? C54 C49 C50 124.7 . . ? C54 C49 P4 120.3(15) . . ? C50 C49 P4 115.0(15) . . ? C51 C50 C49 121.5 . . ? C52 C51 C50 112.9 . . ? C51 C52 C53 131.2 . . ? C51 C52 C55 116.5(13) . . ? C53 C52 C55 111.9(13) . . ? C52 C53 C54 112.8 . . ? C49 C54 C53 115.7 . . ? C60 C55 C56 123.1 . . ? C60 C55 C52 118.9(17) . . ? C56 C55 C52 116.6(17) . . ? C55 C56 C57 121.5 . . ? C58 C57 C56 113.4 . . ? C57 C58 C59 130.5 . . ? C58 C59 C60 111.9 . . ? C55 C60 C59 117.0 . . ? C66 C61 C62 121.9 . . ? C66 C61 P3 115.6(18) . . ? C62 C61 P3 122.4(18) . . ? C63 C62 C61 120.8 . . ? C64 C63 C62 115.4 . . ? C63 C64 C65 130.5 . . ? C63 C64 C67 113.4(13) . . ? C65 C64 C67 115.6(14) . . ? C64 C65 C66 111.5 . . ? C61 C66 C65 119.7 . . ? C72 C67 C68 124.1 . . ? C72 C67 C64 119.0(17) . . ? C68 C67 C64 116.8(18) . . ? C69 C68 C67 121.0 . . ? C70 C69 C68 112.1 . . ? C69 C70 C71 130.6 . . ? C70 C71 C72 109.7 . . ? C67 C72 C71 117.0 . . ? C78 C73 C74 122.7 . . ? C78 C73 P4 114(2) . . ? C74 C73 P4 123(2) . . ? C75 C74 C73 121.0 . . ? C76 C75 C74 115.2 . . ? C75 C76 C77 129.0 . . ? C75 C76 C79 117.0(15) . . ? C77 C76 C79 113.0(16) . . ? C76 C77 C78 112.7 . . ? C73 C78 C77 118.3 . . ? C84 C79 C80 125.1 . . ? C84 C79 C76 119.8(18) . . ? C80 C79 C76 114.9(18) . . ? C81 C80 C79 119.5 . . ? C82 C81 C80 113.8 . . ? C81 C82 C83 133.3 . . ? C82 C83 C84 110.8 . . ? C79 C84 C83 117.5 . . ? C90 C85 C86 128.0 . . ? C90 C85 P3 121.2(18) . . ? C86 C85 P3 110.3(18) . . ? C85 C86 C87 117.9 . . ? C88 C87 C86 112.7 . . ? C87 C88 C89 135.9 . . ? C87 C88 C91 112.5(14) . . ? C89 C88 C91 111.6(14) . . ? C88 C89 C90 108.3 . . ? C85 C90 C89 116.9 . . ? C96 C91 C92 129.5 . . ? C96 C91 C88 117.1(18) . . ? C92 C91 C88 112.4(18) . . ? C93 C92 C91 117.7 . . ? C94 C93 C92 111.1 . . ? C93 C94 C95 137.6 . . ? C94 C95 C96 108.9 . . ? C91 C96 C95 114.8 . . ? C8A C1A P2 115.0(18) . . ? C8A C2A P3 119.2(19) . 5_735 ? C6A C3A P1 122.2(16) . . ? C8A C5A P4 118.3(19) . . ? C3A C6A C3A 106.7(17) . 9_753 ? C3A C6A C3A 106.7(17) . 5_735 ? C3A C6A C3A 106.7(17) 9_753 5_735 ? C3A C6A C4A 112.1(15) . . ? C3A C6A C4A 112.1(15) 9_753 . ? C3A C6A C4A 112.1(15) 5_735 . ? C5A C8A C2A 110(2) . . ? C5A C8A C1A 110(2) . . ? C2A C8A C1A 107(2) . . ? C5A C8A C7A 108(2) . . ? C2A C8A C7A 110(2) . . ? C1A C8A C7A 112(2) . . ? O12 N1 O13 117(4) . . ? O12 N1 O11 130(5) . . ? O13 N1 O11 102(4) . . ? N1 O12 Ag1 120(3) . . ? O21 N2 O21 118.7(9) . 9_753 ? O21 N2 O21 118.6(9) . 5_735 ? O21 N2 O21 118.6(9) 9_753 5_735 ? N2 O21 Ag2 131.9(15) . 5_735 ? O31 N3 O31 118.3(15) 9_753 . ? O31 N3 O31 118.3(15) 9_753 5_735 ? O31 N3 O31 118.2(15) . 5_735 ? O41 N4 O41 119(2) 7_995 10_949 ? O41 N4 O41 118(2) 7_995 . ? O41 N4 O41 120(2) 10_949 . ? C6S C1S C2S 124.8 . . ? C3S C2S C1S 116.8 . . ? C4S C3S C2S 116.3 . . ? C3S C4S C5S 128.7 . . ? C4S C5S C6S 109.6 . . ? C1S C6S C5S 117.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.042 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.187 #===end data_pm6a129m _publ_contact_author 'Stuart L. James' _publ_contact_author_email 'S.James@qub.ac.uk' loop_ _publ_author_name 'Philip Miller' 'Xingling Xu' 'Mark Nieuwenhuyzen' 'Stuart L. James' _journal_name_full Chemical Communications _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C309 H269 Ag6 Cl3 N6 O26 P12' _chemical_formula_weight 5607.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 30.7586(10) _cell_length_b 30.7586(10) _cell_length_c 30.7586(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 29100.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11544 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74941 _diffrn_reflns_av_R_equivalents 0.1714 _diffrn_reflns_av_sigmaI/netI 0.1018 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 20.00 _reflns_number_total 9086 _reflns_number_gt 5001 _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, 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^)+(0.1435P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(9) _refine_ls_number_reflns 9086 _refine_ls_number_parameters 533 _refine_ls_number_restraints 955 _refine_ls_R_factor_all 0.1870 _refine_ls_R_factor_gt 0.1141 _refine_ls_wR_factor_ref 0.3296 _refine_ls_wR_factor_gt 0.2861 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_restrained_S_all 1.350 _refine_ls_shift/su_max 3.399 _refine_ls_shift/su_mean 0.142 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 -0.18302(6) -0.18176(6) 0.67459(5) 0.0940(6) Uani 1 1 d . . . Ag2 Ag -0.35228(7) -0.23246(7) 0.61934(6) 0.1103(8) Uani 1 1 d . . . P1 P -0.13874(19) -0.1624(2) 0.73554(19) 0.0862(19) Uani 1 1 d . . . P2 P -0.1709(2) -0.19446(19) 0.5989(2) 0.0875(19) Uani 1 1 d . . . P3 P -0.3141(2) -0.25325(19) 0.55439(19) 0.0890(19) Uani 1 1 d . . . P4 P -0.4181(2) -0.1951(2) 0.6414(2) 0.102(2) Uani 1 1 d . . . C1 C -0.1397(6) -0.1051(6) 0.7444(6) 0.081(6) Uiso 1 1 d DU . . C2 C -0.1640(6) -0.0782(7) 0.7177(7) 0.124(9) Uiso 1 1 d DU . . H2 H -0.1785 -0.0906 0.6934 0.149 Uiso 1 1 calc R . . C3 C -0.1681(7) -0.0317(7) 0.7255(7) 0.127(9) Uiso 1 1 d DU . . H3 H -0.1849 -0.0137 0.7068 0.153 Uiso 1 1 calc R . . C4 C -0.1469(8) -0.0152(7) 0.7608(8) 0.132(9) Uiso 1 1 d DU . . C5 C -0.1250(8) -0.0389(8) 0.7875(8) 0.145(10) Uiso 1 1 d DU . . H5 H -0.1125 -0.0264 0.8128 0.173 Uiso 1 1 calc R . . C6 C -0.1193(8) -0.0858(7) 0.7783(8) 0.142(10) Uiso 1 1 d DU . . H6 H -0.1010 -0.1027 0.7966 0.170 Uiso 1 1 calc R . . C7 C -0.1503(12) 0.0362(8) 0.7689(12) 0.271(18) Uiso 1 1 d DU . . C8 C -0.1795(14) 0.0563(13) 0.7442(14) 0.41(3) Uiso 1 1 d DU . . H8 H -0.2035 0.0404 0.7331 0.488 Uiso 1 1 calc R . . C9 C -0.175(2) 0.1039(15) 0.7337(18) 0.48(3) Uiso 1 1 d DU . . H9 H -0.1939 0.1208 0.7161 0.578 Uiso 1 1 calc R . . C10 C -0.139(2) 0.1176(14) 0.754(2) 0.50(3) Uiso 1 1 d DU . . H10 H -0.1366 0.1481 0.7497 0.597 Uiso 1 1 calc R . . C11 C -0.105(2) 0.1033(16) 0.779(2) 0.52(3) Uiso 1 1 d DU . . H11 H -0.0805 0.1199 0.7879 0.628 Uiso 1 1 calc R . . C12 C -0.1138(16) 0.0544(14) 0.7880(18) 0.47(3) Uiso 1 1 d DU . . H12 H -0.0951 0.0378 0.8062 0.567 Uiso 1 1 calc R . . C13 C -0.0837(6) -0.1741(8) 0.7253(8) 0.106(7) Uiso 1 1 d DU . . C14 C -0.0565(9) -0.1453(8) 0.7047(11) 0.177(13) Uiso 1 1 d DU . . H14 H -0.0646 -0.1155 0.7046 0.212 Uiso 1 1 calc R . . C15 C -0.0161(10) -0.1573(10) 0.6831(12) 0.222(15) Uiso 1 1 d DU . . H15 H -0.0041 -0.1413 0.6596 0.266 Uiso 1 1 calc R . . C16 C 0.0027(8) -0.1937(10) 0.6999(11) 0.181(12) Uiso 1 1 d DU . . C17 C -0.0200(9) -0.2231(9) 0.7197(11) 0.184(13) Uiso 1 1 d DU . . H17 H -0.0076 -0.2506 0.7262 0.221 Uiso 1 1 calc R . . C18 C -0.0654(8) -0.2134(8) 0.7318(10) 0.161(11) Uiso 1 1 d DU . . H18 H -0.0824 -0.2358 0.7446 0.193 Uiso 1 1 calc R . . C19 C 0.0487(9) -0.2078(12) 0.6803(12) 0.268(18) Uiso 1 1 d DU . . C20 C 0.0616(14) -0.1851(15) 0.6460(14) 0.38(3) Uiso 1 1 d DU . . H20 H 0.0411 -0.1694 0.6291 0.453 Uiso 1 1 calc R . . C21 C 0.1091(16) -0.1843(18) 0.6342(17) 0.45(3) Uiso 1 1 d DU . . H21 H 0.1227 -0.1671 0.6125 0.540 Uiso 1 1 calc R . . C22 C 0.1282(13) -0.2128(17) 0.6606(18) 0.43(3) Uiso 1 1 d DU . . H22 H 0.1585 -0.2129 0.6549 0.519 Uiso 1 1 calc R . . C23 C 0.1196(13) -0.2422(16) 0.6932(17) 0.38(3) Uiso 1 1 d DU . . H23 H 0.1403 -0.2606 0.7069 0.459 Uiso 1 1 calc R . . C24 C 0.0698(13) -0.2400(13) 0.7035(14) 0.33(2) Uiso 1 1 d DU . . H24 H 0.0557 -0.2587 0.7236 0.397 Uiso 1 1 calc R . . C25 C -0.1199(6) -0.2186(6) 0.5884(6) 0.083(6) Uiso 1 1 d DU . . C26 C -0.0950(7) -0.2388(8) 0.6193(7) 0.111(8) Uiso 1 1 d DU . . H26 H -0.1065 -0.2399 0.6479 0.133 Uiso 1 1 calc R . . C27 C -0.0526(7) -0.2588(9) 0.6127(7) 0.136(9) Uiso 1 1 d DU . . H27 H -0.0365 -0.2712 0.6360 0.163 Uiso 1 1 calc R . . C28 C -0.0371(7) -0.2589(8) 0.5706(7) 0.114(8) Uiso 1 1 d DU . . C29 C -0.0601(9) -0.2433(11) 0.5394(8) 0.186(13) Uiso 1 1 d DU . . H29 H -0.0500 -0.2462 0.5104 0.224 Uiso 1 1 calc R . . C30 C -0.1023(8) -0.2206(9) 0.5476(7) 0.129(9) Uiso 1 1 d DU . . H30 H -0.1172 -0.2073 0.5240 0.155 Uiso 1 1 calc R . . C31 C 0.0060(8) -0.2858(10) 0.5611(9) 0.198(14) Uiso 1 1 d DU . . C32 C 0.0341(11) -0.2844(12) 0.5943(11) 0.253(18) Uiso 1 1 d DU . . H32 H 0.0270 -0.2702 0.6208 0.303 Uiso 1 1 calc R . . C33 C 0.0774(11) -0.3063(13) 0.5879(13) 0.250(18) Uiso 1 1 d DU . . H33 H 0.1014 -0.3065 0.6073 0.299 Uiso 1 1 calc R . . C34 C 0.0746(10) -0.3255(10) 0.5491(12) 0.218(15) Uiso 1 1 d DU . . H34 H 0.1020 -0.3387 0.5436 0.261 Uiso 1 1 calc R . . C35 C 0.0488(12) -0.3342(10) 0.5138(11) 0.228(16) Uiso 1 1 d DU . . H35 H 0.0558 -0.3514 0.4890 0.273 Uiso 1 1 calc R . . C36 C 0.0052(10) -0.3097(10) 0.5232(10) 0.231(16) Uiso 1 1 d DU . . H36 H -0.0194 -0.3112 0.5046 0.277 Uiso 1 1 calc R . . C37 C -0.1711(7) -0.1440(6) 0.5734(7) 0.094(7) Uiso 1 1 d DU . . C38 C -0.2002(8) -0.1276(7) 0.5440(9) 0.151(10) Uiso 1 1 d DU . . H38 H -0.2244 -0.1452 0.5363 0.182 Uiso 1 1 calc R . . C39 C -0.1965(8) -0.0851(7) 0.5238(8) 0.123(9) Uiso 1 1 d DU . . H39 H -0.2162 -0.0764 0.5017 0.148 Uiso 1 1 calc R . . C40 C -0.1643(7) -0.0581(6) 0.5371(7) 0.114(8) Uiso 1 1 d DU . . C41 C -0.1431(9) -0.0680(7) 0.5726(9) 0.148(10) Uiso 1 1 d DU . . H41 H -0.1279 -0.0461 0.5884 0.177 Uiso 1 1 calc R . . C42 C -0.1431(9) -0.1135(7) 0.5881(9) 0.151(10) Uiso 1 1 d DU . . H42 H -0.1224 -0.1217 0.6094 0.181 Uiso 1 1 calc R . . C43 C -0.1646(8) -0.0088(7) 0.5228(8) 0.136(9) Uiso 1 1 d DU . . C44 C -0.1328(10) 0.0161(10) 0.5382(11) 0.215(16) Uiso 1 1 d DU . . H44 H -0.1115 0.0034 0.5567 0.258 Uiso 1 1 calc R . . C45 C -0.1296(12) 0.0635(11) 0.5274(13) 0.273(19) Uiso 1 1 d DU . . H45 H -0.1104 0.0842 0.5401 0.327 Uiso 1 1 calc R . . C46 C -0.1590(9) 0.0708(9) 0.4963(9) 0.179(12) Uiso 1 1 d DU . . H46 H -0.1560 0.0994 0.4852 0.215 Uiso 1 1 calc R . . C47 C -0.1922(9) 0.0494(8) 0.4755(8) 0.157(11) Uiso 1 1 d DU . . H47 H -0.2108 0.0621 0.4544 0.188 Uiso 1 1 calc R . . C48 C -0.1950(8) 0.0019(8) 0.4915(8) 0.143(10) Uiso 1 1 d DU . . H48 H -0.2159 -0.0182 0.4808 0.171 Uiso 1 1 calc R . . C49 C -0.3080(8) -0.2063(6) 0.5210(7) 0.109(8) Uiso 1 1 d DU . . C50 C -0.3183(9) -0.1654(7) 0.5374(7) 0.142(10) Uiso 1 1 d DU . . H50 H -0.3303 -0.1635 0.5658 0.171 Uiso 1 1 calc R . . C51 C -0.3114(8) -0.1255(7) 0.5129(7) 0.130(9) Uiso 1 1 d DU . . H51 H -0.3156 -0.0979 0.5261 0.156 Uiso 1 1 calc R . . C52 C -0.2987(9) -0.1284(6) 0.4706(7) 0.121(8) Uiso 1 1 d DU . . C53 C -0.2899(9) -0.1659(7) 0.4537(8) 0.140(10) Uiso 1 1 d DU . . H53 H -0.2821 -0.1678 0.4239 0.168 Uiso 1 1 calc R . . C54 C -0.2918(9) -0.2060(7) 0.4804(8) 0.142(10) Uiso 1 1 d DU . . H54 H -0.2812 -0.2324 0.4683 0.171 Uiso 1 1 calc R . . C55 C -0.2944(10) -0.0848(8) 0.4431(9) 0.172(12) Uiso 1 1 d DU . . C56 C -0.3080(10) -0.0487(9) 0.4614(10) 0.180(12) Uiso 1 1 d DU . . H56 H -0.3202 -0.0500 0.4898 0.216 Uiso 1 1 calc R . . C57 C -0.3049(13) -0.0054(10) 0.4391(14) 0.254(18) Uiso 1 1 d DU . . H57 H -0.3125 0.0222 0.4507 0.304 Uiso 1 1 calc R . . C58 C -0.2895(13) -0.0139(13) 0.3999(13) 0.30(2) Uiso 1 1 d DU . . H58 H -0.2895 0.0121 0.3833 0.361 Uiso 1 1 calc R . . C59 C -0.2734(14) -0.0473(15) 0.3748(12) 0.37(3) Uiso 1 1 d DU . . H59 H -0.2625 -0.0449 0.3460 0.447 Uiso 1 1 calc R . . C60 C -0.2763(14) -0.0898(12) 0.4020(11) 0.30(2) Uiso 1 1 d DU . . H60 H -0.2664 -0.1170 0.3914 0.361 Uiso 1 1 calc R . . C61 C -0.3496(11) -0.2913(10) 0.5230(11) 0.161(11) Uiso 1 1 d DU . . C62 C -0.3472(12) -0.3366(11) 0.5276(12) 0.232(16) Uiso 1 1 d DU . . H62 H -0.3227 -0.3490 0.5417 0.278 Uiso 1 1 calc R . . C63 C -0.3813(13) -0.3651(10) 0.5112(15) 0.269(19) Uiso 1 1 d DU . . H63 H -0.3835 -0.3947 0.5199 0.323 Uiso 1 1 calc R . . C64 C -0.4098(12) -0.3470(12) 0.4827(14) 0.253(17) Uiso 1 1 d DU . . C65 C -0.4029(14) -0.3093(12) 0.4659(12) 0.266(18) Uiso 1 1 d DU . . H65 H -0.4157 -0.3015 0.4389 0.319 Uiso 1 1 calc R . . C66 C -0.3744(14) -0.2781(10) 0.4894(14) 0.245(17) Uiso 1 1 d DU . . H66 H -0.3737 -0.2485 0.4806 0.294 Uiso 1 1 calc R . . C67 C -0.4529(11) -0.3732(12) 0.4708(14) 0.33(2) Uiso 1 1 d DU . . C68 C -0.4900(14) -0.3561(16) 0.4848(17) 0.39(3) Uiso 1 1 d DU . . H68 H -0.4899 -0.3364 0.5086 0.462 Uiso 1 1 calc R . . C69 C -0.5322(13) -0.3680(19) 0.463(2) 0.43(3) Uiso 1 1 d DU . . H69 H -0.5601 -0.3559 0.4681 0.520 Uiso 1 1 calc R . . C70 C -0.5217(16) -0.3992(18) 0.4349(18) 0.42(3) Uiso 1 1 d DU . . H70 H -0.5476 -0.4093 0.4214 0.510 Uiso 1 1 calc R . . C71 C -0.4874(19) -0.4223(15) 0.4181(15) 0.36(3) Uiso 1 1 d DU . . H71 H -0.4890 -0.4441 0.3963 0.435 Uiso 1 1 calc R . . C72 C -0.4452(15) -0.4063(14) 0.4414(16) 0.37(3) Uiso 1 1 d DU . . H72 H -0.4172 -0.4181 0.4360 0.448 Uiso 1 1 calc R . . C73 C -0.4658(8) -0.2199(9) 0.6184(9) 0.140(10) Uiso 1 1 d DU . . C74 C -0.4693(8) -0.2600(10) 0.5985(10) 0.173(12) Uiso 1 1 d DU . . H74 H -0.4437 -0.2767 0.5942 0.208 Uiso 1 1 calc R . . C75 C -0.5112(8) -0.2778(9) 0.5836(10) 0.173(12) Uiso 1 1 d DU . . H75 H -0.5137 -0.3031 0.5661 0.208 Uiso 1 1 calc R . . C76 C -0.5459(7) -0.2542(10) 0.5975(11) 0.183(12) Uiso 1 1 d DU . . C77 C -0.5456(9) -0.2191(10) 0.6198(12) 0.205(14) Uiso 1 1 d DU . . H77 H -0.5718 -0.2046 0.6272 0.246 Uiso 1 1 calc R . . C78 C -0.5030(10) -0.2019(11) 0.6336(13) 0.230(16) Uiso 1 1 d DU . . H78 H -0.5017 -0.1781 0.6532 0.275 Uiso 1 1 calc R . . C79 C -0.5931(9) -0.2725(11) 0.5858(12) 0.254(17) Uiso 1 1 d DU . . C80 C -0.5931(11) -0.3154(11) 0.5823(13) 0.249(18) Uiso 1 1 d DU . . H80 H -0.5676 -0.3324 0.5863 0.299 Uiso 1 1 calc R . . C81 C -0.6368(14) -0.3353(13) 0.5716(14) 0.31(2) Uiso 1 1 d DU . . H81 H -0.6431 -0.3654 0.5687 0.374 Uiso 1 1 calc R . . C82 C -0.6648(12) -0.3028(15) 0.5669(11) 0.30(2) Uiso 1 1 d DU . . H82 H -0.6919 -0.3154 0.5591 0.360 Uiso 1 1 calc R . . C83 C -0.6710(11) -0.2582(16) 0.5686(12) 0.30(2) Uiso 1 1 d DU . . H83 H -0.6970 -0.2422 0.5635 0.361 Uiso 1 1 calc R . . C84 C -0.6251(11) -0.2406(12) 0.5810(13) 0.28(2) Uiso 1 1 d DU . . H84 H -0.6193 -0.2106 0.5849 0.341 Uiso 1 1 calc R . . C85 C -0.4200(9) -0.1425(7) 0.6218(8) 0.120(8) Uiso 1 1 d DU . . C86 C -0.4438(11) -0.1304(9) 0.5849(11) 0.203(14) Uiso 1 1 d DU . . H86 H -0.4644 -0.1506 0.5738 0.244 Uiso 1 1 calc R . . C87 C -0.4390(11) -0.0889(9) 0.5622(10) 0.195(14) Uiso 1 1 d DU . . H87 H -0.4538 -0.0828 0.5358 0.234 Uiso 1 1 calc R . . C88 C -0.4122(9) -0.0597(7) 0.5812(8) 0.126(9) Uiso 1 1 d DU . . C89 C -0.3899(10) -0.0690(8) 0.6158(9) 0.172(12) Uiso 1 1 d DU . . H89 H -0.3717 -0.0473 0.6283 0.206 Uiso 1 1 calc R . . C90 C -0.3920(11) -0.1123(9) 0.6362(10) 0.181(13) Uiso 1 1 d DU . . H90 H -0.3733 -0.1189 0.6599 0.217 Uiso 1 1 calc R . . C91 C -0.4105(9) -0.0113(7) 0.5630(8) 0.148(10) Uiso 1 1 d DU . . C92 C -0.4093(10) -0.0088(10) 0.5196(9) 0.192(14) Uiso 1 1 d DU . . H92 H -0.4167 -0.0334 0.5024 0.231 Uiso 1 1 calc R . . C93 C -0.3963(11) 0.0326(11) 0.4983(11) 0.200(14) Uiso 1 1 d DU . . H93 H -0.3902 0.0368 0.4683 0.240 Uiso 1 1 calc R . . C94 C -0.3947(10) 0.0626(11) 0.5293(12) 0.219(16) Uiso 1 1 d DU . . H94 H -0.3900 0.0903 0.5163 0.263 Uiso 1 1 calc R . . C95 C -0.3975(11) 0.0675(10) 0.5740(13) 0.258(19) Uiso 1 1 d DU . . H95 H -0.3939 0.0937 0.5899 0.310 Uiso 1 1 calc R . . C96 C -0.4077(10) 0.0220(9) 0.5934(9) 0.190(13) Uiso 1 1 d DU . . H96 H -0.4118 0.0173 0.6236 0.228 Uiso 1 1 calc R . . C1A C -0.2118(7) -0.2220(7) 0.5671(7) 0.093(7) Uiso 1 1 d . . . H1AA H -0.2379 -0.2033 0.5666 0.112 Uiso 1 1 calc R . . H1AB H -0.2009 -0.2238 0.5368 0.112 Uiso 1 1 calc R . . C2A C -0.2271(6) -0.2700(6) 0.5811(6) 0.063(5) Uiso 1 1 d . . . C3A C -0.2392(7) -0.2690(7) 0.6289(6) 0.083(6) Uiso 1 1 d . . . H3AA H -0.2564 -0.2948 0.6360 0.124 Uiso 1 1 calc R . . H3AB H -0.2562 -0.2428 0.6350 0.124 Uiso 1 1 calc R . . H3AC H -0.2126 -0.2688 0.6465 0.124 Uiso 1 1 calc R . . C4A C -0.2644(7) -0.2854(7) 0.5550(7) 0.089(7) Uiso 1 1 d . . . H4AA H -0.2720 -0.3149 0.5653 0.107 Uiso 1 1 calc R . . H4AB H -0.2543 -0.2883 0.5246 0.107 Uiso 1 1 calc R . . C5A C -0.1890(7) -0.2983(6) 0.5730(7) 0.086(6) Uiso 1 1 d . . . H5A1 H -0.1650 -0.2879 0.5918 0.103 Uiso 1 1 calc R . . H5A2 H -0.1798 -0.2937 0.5425 0.103 Uiso 1 1 calc R . . C6A C -0.1441(6) -0.1864(7) 0.7908(6) 0.077(6) Uiso 1 1 d . . . H6AA H -0.1301 -0.2153 0.7907 0.093 Uiso 1 1 calc R . . H6AB H -0.1278 -0.1679 0.8115 0.093 Uiso 1 1 calc R . . C7A C -0.1917(6) -0.1917(6) 0.8083(6) 0.074(10) Uiso 1 3 d S . . C8A C -0.2225(7) -0.2225(7) 0.7775(7) 0.102(13) Uiso 1 3 d S . . H8A1 H -0.2088 -0.2510 0.7738 0.153 Uiso 0.33 1 calc PR . . H8A2 H -0.2262 -0.2088 0.7490 0.153 Uiso 0.33 1 calc PR . . H8A3 H -0.2510 -0.2262 0.7912 0.153 Uiso 0.33 1 calc PR . . N1 N -0.2835(9) -0.1611(8) 0.6822(10) 0.135(8) Uiso 1 1 d D . . O11 O -0.3188(9) -0.1463(9) 0.6978(9) 0.215(10) Uiso 1 1 d D . . O12 O -0.2509(7) -0.1464(6) 0.6985(6) 0.134(6) Uiso 1 1 d . . . O13 O -0.2853(8) -0.1750(9) 0.6501(10) 0.188(9) Uiso 1 1 d . . . N2 N -0.1030(8) -0.1030(8) 0.8970(8) 0.128(13) Uiso 1 3 d SD . . O21 O -0.0705(6) -0.1083(8) 0.8712(7) 0.178(8) Uiso 1 1 d D . . N3 N -0.3425(6) -0.3425(6) 0.6575(6) 0.100(10) Uiso 1 3 d SD . . O31 O -0.3120(5) -0.3493(5) 0.6305(5) 0.122(5) Uiso 1 1 d D . . N4 N -0.0763(17) -0.4237(17) 0.4237(17) 0.43(4) Uiso 1 3 d SD . . O41 O -0.0699(9) -0.3888(7) 0.4525(8) 0.203(10) Uiso 1 1 d D . . O1W O -0.6592(12) -0.1592(12) 0.6592(12) 0.28(3) Uiso 1 3 d S . . O2W O -0.7646(12) -0.2016(11) 0.6030(11) 0.267(15) Uiso 1 1 d . . . O3W O -0.7348(13) -0.2809(12) 0.6514(12) 0.285(16) Uiso 1 1 d . . . O4W O -0.221(4) 0.029(4) 0.621(4) 0.29(5) Uiso 0.33 1 d P A 2 C1S C -0.263(2) -0.0119(14) 0.6188(8) 0.11(2) Uiso 0.33 1 d PD B 1 H1SA H -0.2349 0.0037 0.6160 0.127 Uiso 0.33 1 calc PR B 1 Cl1 Cl -0.2575(10) -0.0620(9) 0.6309(9) 0.195(12) Uiso 0.33 1 d PD B 1 Cl2 Cl -0.2938(11) 0.0078(9) 0.6566(9) 0.200(13) Uiso 0.33 1 d PD B 1 Cl3 Cl -0.2914(7) -0.0107(7) 0.5750(7) 0.133(7) Uiso 0.33 1 d PD B 1 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 0.0922(13) 0.1147(15) 0.0752(12) 0.0050(11) 0.0024(10) 0.0048(11) Ag2 0.1125(16) 0.1366(18) 0.0817(14) 0.0087(12) 0.0050(11) 0.0143(13) P1 0.073(4) 0.110(5) 0.076(4) 0.017(4) 0.016(3) 0.007(3) P2 0.097(5) 0.077(4) 0.089(4) 0.010(3) -0.004(3) 0.007(3) P3 0.110(5) 0.076(4) 0.081(4) 0.004(3) 0.005(4) -0.003(4) P4 0.088(5) 0.146(6) 0.072(4) 0.027(4) -0.011(3) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.389(6) . ? Ag1 P1 2.393(7) . ? Ag1 O12 2.467(19) . ? Ag2 P3 2.403(6) . ? Ag2 P4 2.423(7) . ? P1 C13 1.76(2) . ? P1 C1 1.782(18) . ? P1 C6A 1.86(2) . ? P2 C37 1.740(19) . ? P2 C25 1.764(18) . ? P2 C1A 1.81(2) . ? P3 C49 1.78(2) . ? P3 C4A 1.82(2) . ? P3 C61 1.87(3) . ? P4 C85 1.73(2) . ? P4 C73 1.80(2) . ? P4 C5A 1.89(2) 5_456 ? C1 C6 1.354(17) . ? C1 C2 1.384(17) . ? C2 C3 1.455(18) . ? C3 C4 1.366(17) . ? C4 C5 1.289(18) . ? C4 C7 1.60(2) . ? C5 C6 1.481(19) . ? C7 C8 1.33(2) . ? C7 C12 1.39(2) . ? C8 C9 1.51(3) . ? C9 C10 1.33(3) . ? C10 C11 1.38(3) . ? C11 C12 1.55(3) . ? C13 C18 1.350(17) . ? C13 C14 1.373(18) . ? C14 C15 1.456(19) . ? C15 C16 1.363(18) . ? C16 C17 1.294(19) . ? C16 C19 1.60(2) . ? C17 C18 1.476(19) . ? C19 C20 1.33(2) . ? C19 C24 1.38(2) . ? C20 C21 1.51(3) . ? C21 C22 1.33(3) . ? C22 C23 1.37(3) . ? C23 C24 1.57(3) . ? C25 C26 1.372(16) . ? C25 C30 1.368(17) . ? C26 C27 1.456(18) . ? C27 C28 1.379(17) . ? C28 C29 1.283(18) . ? C28 C31 1.59(2) . ? C29 C30 1.496(19) . ? C31 C32 1.34(2) . ? C31 C36 1.38(2) . ? C32 C33 1.51(3) . ? C33 C34 1.34(3) . ? C34 C35 1.37(3) . ? C35 C36 1.57(2) . ? C37 C42 1.350(18) . ? C37 C38 1.370(17) . ? C38 C39 1.452(18) . ? C39 C40 1.358(17) . ? C40 C41 1.307(18) . ? C40 C43 1.580(19) . ? C41 C42 1.478(19) . ? C43 C44 1.33(2) . ? C43 C48 1.38(2) . ? C44 C45 1.50(3) . ? C45 C46 1.34(3) . ? C46 C47 1.37(3) . ? C47 C48 1.54(2) . ? C49 C54 1.346(17) . ? C49 C50 1.390(17) . ? C50 C51 1.459(18) . ? C51 C52 1.360(17) . ? C52 C53 1.294(18) . ? C52 C55 1.59(2) . ? C53 C54 1.481(19) . ? C55 C56 1.32(2) . ? C55 C60 1.39(2) . ? C56 C57 1.50(3) . ? C57 C58 1.32(3) . ? C58 C59 1.38(3) . ? C59 C60 1.55(3) . ? C61 C66 1.349(19) . ? C61 C62 1.401(18) . ? C62 C63 1.46(2) . ? C63 C64 1.360(19) . ? C64 C65 1.288(19) . ? C64 C67 1.59(2) . ? C65 C66 1.48(2) . ? C67 C68 1.33(2) . ? C67 C72 1.38(2) . ? C68 C69 1.51(3) . ? C69 C70 1.33(3) . ? C70 C71 1.37(3) . ? C71 C72 1.56(3) . ? C73 C78 1.354(18) . ? C73 C74 1.380(18) . ? C74 C75 1.474(19) . ? C75 C76 1.358(18) . ? C76 C77 1.279(19) . ? C76 C79 1.60(2) . ? C77 C78 1.47(2) . ? C79 C80 1.33(2) . ? C79 C84 1.40(2) . ? C80 C81 1.51(3) . ? C81 C82 1.33(3) . ? C82 C83 1.39(3) . ? C83 C84 1.56(3) . ? C85 C90 1.340(18) . ? C85 C86 1.403(18) . ? C86 C87 1.463(19) . ? C87 C88 1.353(18) . ? C88 C89 1.299(18) . ? C88 C91 1.59(2) . ? C89 C90 1.474(19) . ? C91 C92 1.34(2) . ? C91 C96 1.39(2) . ? C92 C93 1.49(3) . ? C93 C94 1.33(3) . ? C94 C95 1.39(3) . ? C95 C96 1.55(2) . ? C1A C2A 1.61(3) . ? C2A C5A 1.48(3) . ? C2A C4A 1.48(3) . ? C2A C3A 1.52(2) . ? C5A P4 1.89(2) 9_546 ? C6A C7A 1.57(2) . ? C7A C6A 1.57(2) 9_546 ? C7A C6A 1.57(2) 5_456 ? C7A C8A 1.64(5) . ? N1 O13 1.08(3) . ? N1 O11 1.272(17) . ? N1 O12 1.21(3) . ? N2 O21 1.288(16) 9_546 ? N2 O21 1.290(16) . ? N2 O21 1.286(16) 5_456 ? N3 O31 1.269(14) 9_546 ? N3 O31 1.271(14) . ? N3 O31 1.268(14) 5_456 ? N4 O41 1.343(17) 12_455 ? N4 O41 1.461(17) 6_445 ? N4 O41 1.420(17) . ? C1S Cl1 1.60(4) . ? C1S Cl3 1.60(4) . ? C1S Cl2 1.61(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 135.6(2) . . ? P2 Ag1 O12 119.7(5) . . ? P1 Ag1 O12 97.9(5) . . ? P3 Ag2 P4 140.0(2) . . ? C13 P1 C1 104.2(10) . . ? C13 P1 C6A 99.7(10) . . ? C1 P1 C6A 104.5(9) . . ? C13 P1 Ag1 110.9(8) . . ? C1 P1 Ag1 110.9(7) . . ? C6A P1 Ag1 124.5(7) . . ? C37 P2 C25 107.2(10) . . ? C37 P2 C1A 99.9(10) . . ? C25 P2 C1A 108.8(10) . . ? C37 P2 Ag1 107.0(8) . . ? C25 P2 Ag1 112.8(7) . . ? C1A P2 Ag1 119.7(8) . . ? C49 P3 C4A 110.9(11) . . ? C49 P3 C61 105.8(14) . . ? C4A P3 C61 99.0(13) . . ? C49 P3 Ag2 108.4(8) . . ? C4A P3 Ag2 123.1(7) . . ? C61 P3 Ag2 108.1(11) . . ? C85 P4 C73 103.4(13) . . ? C85 P4 C5A 104.1(12) . 5_456 ? C73 P4 C5A 108.0(12) . 5_456 ? C85 P4 Ag2 112.0(9) . . ? C73 P4 Ag2 111.8(10) . . ? C5A P4 Ag2 116.4(7) 5_456 . ? C6 C1 C2 116.3(16) . . ? C6 C1 P1 122.9(15) . . ? C2 C1 P1 120.6(14) . . ? C1 C2 C3 122.6(17) . . ? C4 C3 C2 117.0(17) . . ? C5 C4 C3 123.0(18) . . ? C5 C4 C7 119.6(18) . . ? C3 C4 C7 117.4(17) . . ? C4 C5 C6 119.5(19) . . ? C1 C6 C5 121.3(18) . . ? C8 C7 C12 127(3) . . ? C8 C7 C4 114(2) . . ? C12 C7 C4 114(2) . . ? C7 C8 C9 121(3) . . ? C10 C9 C8 107(3) . . ? C9 C10 C11 142(3) . . ? C10 C11 C12 106(3) . . ? C7 C12 C11 117(2) . . ? C18 C13 C14 112.9(17) . . ? C18 C13 P1 124.0(18) . . ? C14 C13 P1 122.5(18) . . ? C13 C14 C15 125(2) . . ? C16 C15 C14 113(2) . . ? C17 C16 C15 122(2) . . ? C17 C16 C19 118(2) . . ? C15 C16 C19 117.1(19) . . ? C16 C17 C18 119(2) . . ? C13 C18 C17 122.7(19) . . ? C20 C19 C24 130(3) . . ? C20 C19 C16 115(2) . . ? C24 C19 C16 115(2) . . ? C19 C20 C21 119(3) . . ? C22 C21 C20 106(3) . . ? C21 C22 C23 143(3) . . ? C22 C23 C24 108(3) . . ? C19 C24 C23 113(2) . . ? C26 C25 C30 113.3(16) . . ? C26 C25 P2 124.0(15) . . ? C30 C25 P2 122.6(15) . . ? C25 C26 C27 126.5(17) . . ? C28 C27 C26 116.2(17) . . ? C29 C28 C27 120.7(18) . . ? C29 C28 C31 121.2(18) . . ? C27 C28 C31 117.3(17) . . ? C28 C29 C30 122(2) . . ? C25 C30 C29 121.2(18) . . ? C32 C31 C36 132(2) . . ? C32 C31 C28 113(2) . . ? C36 C31 C28 115(2) . . ? C31 C32 C33 117(2) . . ? C34 C33 C32 105(3) . . ? C33 C34 C35 146(3) . . ? C34 C35 C36 105(2) . . ? C31 C36 C35 114(2) . . ? C42 C37 C38 112.5(17) . . ? C42 C37 P2 117.8(16) . . ? C38 C37 P2 128.9(16) . . ? C37 C38 C39 124.2(18) . . ? C40 C39 C38 118.6(18) . . ? C41 C40 C39 118.3(18) . . ? C41 C40 C43 117.3(16) . . ? C39 C40 C43 119.9(16) . . ? C40 C41 C42 119.2(19) . . ? C37 C42 C41 123.4(19) . . ? C44 C43 C48 128(2) . . ? C44 C43 C40 116.6(19) . . ? C48 C43 C40 115.3(17) . . ? C43 C44 C45 122(2) . . ? C46 C45 C44 106(3) . . ? C45 C46 C47 139(3) . . ? C46 C47 C48 110(2) . . ? C43 C48 C47 114(2) . . ? C54 C49 C50 114.5(17) . . ? C54 C49 P3 125.5(16) . . ? C50 C49 P3 120.0(16) . . ? C49 C50 C51 122.8(18) . . ? C52 C51 C50 118.7(17) . . ? C53 C52 C51 120.2(18) . . ? C53 C52 C55 121.3(18) . . ? C51 C52 C55 118.4(16) . . ? C52 C53 C54 120.7(19) . . ? C49 C54 C53 122.3(18) . . ? C56 C55 C60 128(2) . . ? C56 C55 C52 117(2) . . ? C60 C55 C52 115(2) . . ? C55 C56 C57 122(2) . . ? C58 C57 C56 105(3) . . ? C57 C58 C59 142(3) . . ? C58 C59 C60 108(3) . . ? C55 C60 C59 115(2) . . ? C66 C61 C62 114(2) . . ? C66 C61 P3 122(2) . . ? C62 C61 P3 123(2) . . ? C61 C62 C63 122(2) . . ? C64 C63 C62 116(2) . . ? C65 C64 C63 121(2) . . ? C65 C64 C67 120(2) . . ? C63 C64 C67 119(2) . . ? C64 C65 C66 119(2) . . ? C61 C66 C65 121(2) . . ? C68 C67 C72 131(3) . . ? C68 C67 C64 116(2) . . ? C72 C67 C64 112(2) . . ? C67 C68 C69 120(3) . . ? C70 C69 C68 105(3) . . ? C69 C70 C71 143(3) . . ? C70 C71 C72 108(3) . . ? C67 C72 C71 113(2) . . ? C78 C73 C74 116.8(19) . . ? C78 C73 P4 112(2) . . ? C74 C73 P4 128(2) . . ? C73 C74 C75 122.6(19) . . ? C76 C75 C74 113.0(18) . . ? C77 C76 C75 128(2) . . ? C77 C76 C79 115.1(19) . . ? C75 C76 C79 117.1(19) . . ? C76 C77 C78 118(2) . . ? C73 C78 C77 120(2) . . ? C80 C79 C84 134(2) . . ? C80 C79 C76 112(2) . . ? C84 C79 C76 115(2) . . ? C79 C80 C81 115(2) . . ? C82 C81 C80 107(3) . . ? C81 C82 C83 146(3) . . ? C82 C83 C84 103(2) . . ? C79 C84 C83 115(2) . . ? C90 C85 C86 114.8(18) . . ? C90 C85 P4 120.8(19) . . ? C86 C85 P4 123.2(19) . . ? C85 C86 C87 124(2) . . ? C88 C87 C86 115.8(19) . . ? C89 C88 C87 122.0(19) . . ? C89 C88 C91 118.5(18) . . ? C87 C88 C91 119.3(18) . . ? C88 C89 C90 122(2) . . ? C85 C90 C89 121.0(19) . . ? C92 C91 C96 129(2) . . ? C92 C91 C88 114(2) . . ? C96 C91 C88 117(2) . . ? C91 C92 C93 120(2) . . ? C94 C93 C92 107(3) . . ? C93 C94 C95 142(3) . . ? C94 C95 C96 107(2) . . ? C91 C96 C95 115(2) . . ? C2A C1A P2 119.3(14) . . ? C5A C2A C4A 109.6(17) . . ? C5A C2A C3A 111.7(16) . . ? C4A C2A C3A 110.1(17) . . ? C5A C2A C1A 105.1(16) . . ? C4A C2A C1A 112.0(16) . . ? C3A C2A C1A 108.3(15) . . ? C2A C4A P3 119.0(15) . . ? C2A C5A P4 118.3(15) . 9_546 ? C7A C6A P1 116.0(12) . . ? C6A C7A C6A 104.9(15) 9_546 . ? C6A C7A C6A 105.0(15) 9_546 5_456 ? C6A C7A C6A 104.9(15) . 5_456 ? C6A C7A C8A 113.7(13) 9_546 . ? C6A C7A C8A 113.6(13) . . ? C6A C7A C8A 113.7(13) 5_456 . ? O13 N1 O11 116(4) . . ? O13 N1 O12 125(3) . . ? O11 N1 O12 115(3) . . ? N1 O12 Ag1 114.4(19) . . ? O21 N2 O21 119.84(14) 9_546 . ? O21 N2 O21 120.14(14) 9_546 5_456 ? O21 N2 O21 119.94(14) . 5_456 ? O31 N3 O31 119.7(3) 9_546 . ? O31 N3 O31 119.9(3) 9_546 5_456 ? O31 N3 O31 119.8(3) . 5_456 ? O41 N4 O41 120.2(10) 12_455 6_445 ? O41 N4 O41 123.3(11) 12_455 . ? O41 N4 O41 115.1(9) 6_445 . ? Cl1 C1S Cl3 106(3) . . ? Cl1 C1S Cl2 105(3) . . ? Cl3 C1S Cl2 106(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.930 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.152