# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'co3ph.cif' # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; _publ_contact_author_email brian.skelton@uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 loop_ _publ_author_name _publ_author_footnote _publ_author_address G.A.Bowmaker . ; Chemistry, School of Biomedical, Biomolecular and Chemical Science, M313, University of Western Australia, Perth, WA 6009, Australia ; 'C. Pettinari' '' '' Effendy '' '' 'B. W. Skelton' '' '' 'A. H. White' '' '' _publ_section_references ; Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Enraf-Nonius (1989). CAD-4 Software. Version 5.0. Enraf-Nonius, Delft, The Netherlands. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_co3ph _database_code_depnum_ccdc_archive 'CCDC 795571' #TrackingRef 'co3ph.cif' _audit_creation_date 2010-09-30T09:54:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C74 H62 Ag2 O6 P4' _chemical_formula_moiety 'C74 H62 Ag2 O6 P4' _chemical_formula_weight 1386.86 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P_21_21_2 _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 14.990(7) _cell_length_b 23.435(7) _cell_length_c 9.296(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3266(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 14.6 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.75 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ; XTAL absorb ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius Cad4 diffractometer' _diffrn_reflns_av_unetI/netI 0.049 _diffrn_reflns_number 3229 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.95 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3229 _reflns_number_gt 2669 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction xtal _computing_structure_solution 'xtal gentan' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0109P)^2^+0.6928P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3229 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.21(4) _refine_diff_density_max 0.317 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' 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 0.61069(3) 0.534998(18) 0.52262(4) 0.04792(13) Uani 1 1 d . . . C1 C 0.5 0.5 0.2318(9) 0.050(2) Uani 1 2 d S . . O11 O 0.5 0.5 0.3663(6) 0.0627(18) Uani 1 2 d S . . O12 O 0.5659(3) 0.5224(2) 0.1616(4) 0.0719(15) Uani 1 1 d . . . H12 H 0.5487 0.5324 0.0818 0.07(4) Uiso 0.5 1 calc PR . . C2 C 0.5 0.5 0.8150(8) 0.049(2) Uani 1 2 d S . . O21 O 0.5 0.5 0.6785(5) 0.0591(18) Uani 1 2 d S . . O22 O 0.5620(3) 0.5258(2) 0.8830(4) 0.0716(15) Uani 1 1 d . . . H22 H 0.5668 0.5122 0.964 0.03(3) Uiso 0.5 1 calc PR . . P1 P 0.60931(11) 0.63740(6) 0.46575(16) 0.0495(3) Uani 1 1 d . . . C111 C 0.5154(4) 0.6663(2) 0.3635(6) 0.0477(15) Uani 1 1 d . . . C112 C 0.5230(4) 0.7000(3) 0.2436(7) 0.0661(18) Uani 1 1 d . . . H112 H 0.5792 0.7076 0.2058 0.079 Uiso 1 1 calc R . . C113 C 0.4481(5) 0.7227(3) 0.1781(9) 0.085(2) Uani 1 1 d . . . H113 H 0.4542 0.7449 0.0958 0.102 Uiso 1 1 calc R . . C114 C 0.3648(5) 0.7127(3) 0.2341(10) 0.085(3) Uani 1 1 d . . . H114 H 0.3146 0.729 0.192 0.103 Uiso 1 1 calc R . . C115 C 0.3567(5) 0.6791(4) 0.3504(10) 0.089(3) Uani 1 1 d . . . H115 H 0.3003 0.6715 0.3877 0.106 Uiso 1 1 calc R . . C116 C 0.4318(4) 0.6555(3) 0.4160(8) 0.078(2) Uani 1 1 d . . . H116 H 0.425 0.6322 0.4962 0.093 Uiso 1 1 calc R . . C121 C 0.6133(4) 0.6862(2) 0.6191(6) 0.0522(14) Uani 1 1 d . . . C122 C 0.6021(5) 0.7437(3) 0.6054(7) 0.0694(18) Uani 1 1 d . . . H122 H 0.5929 0.7591 0.5144 0.083 Uiso 1 1 calc R . . C123 C 0.6040(5) 0.7794(3) 0.7221(9) 0.087(2) Uani 1 1 d . . . H123 H 0.596 0.8185 0.7105 0.104 Uiso 1 1 calc R . . C124 C 0.6178(6) 0.7568(4) 0.8559(9) 0.101(3) Uani 1 1 d . . . H124 H 0.619 0.7806 0.936 0.122 Uiso 1 1 calc R . . C125 C 0.6296(6) 0.7002(4) 0.8717(9) 0.111(3) Uani 1 1 d . . . H125 H 0.6395 0.6854 0.9631 0.134 Uiso 1 1 calc R . . C126 C 0.6273(6) 0.6636(3) 0.7553(8) 0.083(2) Uani 1 1 d . . . H126 H 0.635 0.6245 0.7679 0.099 Uiso 1 1 calc R . . C131 C 0.7074(4) 0.6553(3) 0.3591(7) 0.0520(16) Uani 1 1 d . . . C132 C 0.7726(4) 0.6935(3) 0.3990(8) 0.0669(18) Uani 1 1 d . . . H132 H 0.7654 0.7146 0.4829 0.08 Uiso 1 1 calc R . . C133 C 0.8480(5) 0.7011(3) 0.3174(12) 0.093(3) Uani 1 1 d . . . H133 H 0.8913 0.7271 0.3466 0.111 Uiso 1 1 calc R . . C134 C 0.8599(5) 0.6704(4) 0.1928(11) 0.097(3) Uani 1 1 d . . . H134 H 0.9108 0.6756 0.1372 0.117 Uiso 1 1 calc R . . C135 C 0.7958(6) 0.6319(4) 0.1513(10) 0.101(3) Uani 1 1 d . . . H135 H 0.8035 0.611 0.0672 0.122 Uiso 1 1 calc R . . C136 C 0.7200(5) 0.6238(3) 0.2333(8) 0.078(2) Uani 1 1 d . . . H136 H 0.6772 0.5974 0.2046 0.094 Uiso 1 1 calc R . . P2 P 0.75156(10) 0.48452(6) 0.55642(15) 0.0466(4) Uani 1 1 d . . . C211 C 0.8071(4) 0.4642(3) 0.3894(6) 0.0503(14) Uani 1 1 d . . . C212 C 0.7541(5) 0.4558(3) 0.2684(7) 0.0656(18) Uani 1 1 d . . . H212 H 0.6928 0.4618 0.2736 0.079 Uiso 1 1 calc R . . C213 C 0.7925(6) 0.4386(3) 0.1406(8) 0.087(3) Uani 1 1 d . . . H213 H 0.7568 0.4329 0.06 0.105 Uiso 1 1 calc R . . C214 C 0.8830(6) 0.4296(3) 0.1315(8) 0.081(2) Uani 1 1 d . . . H214 H 0.9083 0.4178 0.0451 0.097 Uiso 1 1 calc R . . C215 C 0.9353(5) 0.4380(3) 0.2479(8) 0.074(2) Uani 1 1 d . . . H215 H 0.9965 0.4322 0.2405 0.089 Uiso 1 1 calc R . . C216 C 0.8993(4) 0.4550(2) 0.3785(7) 0.0581(16) Uani 1 1 d . . . H216 H 0.936 0.4603 0.4581 0.07 Uiso 1 1 calc R . . C221 C 0.8334(3) 0.5286(2) 0.6491(6) 0.0466(13) Uani 1 1 d . . . C222 C 0.8660(4) 0.5772(3) 0.5813(8) 0.0666(19) Uani 1 1 d . . . H222 H 0.8495 0.5847 0.4868 0.08 Uiso 1 1 calc R . . C223 C 0.9225(5) 0.6147(3) 0.6513(9) 0.083(2) Uani 1 1 d . . . H223 H 0.9444 0.6466 0.6036 0.1 Uiso 1 1 calc R . . C224 C 0.9462(5) 0.6044(3) 0.7921(10) 0.082(2) Uani 1 1 d . . . H224 H 0.983 0.6298 0.841 0.098 Uiso 1 1 calc R . . C225 C 0.9155(5) 0.5576(3) 0.8578(8) 0.082(2) Uani 1 1 d . . . H225 H 0.9324 0.5505 0.9524 0.098 Uiso 1 1 calc R . . C226 C 0.8598(4) 0.5199(3) 0.7899(7) 0.0661(19) Uani 1 1 d . . . H226 H 0.8393 0.488 0.8394 0.079 Uiso 1 1 calc R . . C231 C 0.7490(4) 0.4192(2) 0.6629(6) 0.0471(14) Uani 1 1 d . . . C232 C 0.8176(5) 0.3798(3) 0.6685(8) 0.076(2) Uani 1 1 d . . . H232 H 0.8683 0.3855 0.6126 0.091 Uiso 1 1 calc R . . C233 C 0.8122(6) 0.3329(3) 0.7547(9) 0.086(2) Uani 1 1 d . . . H233 H 0.86 0.3077 0.7591 0.103 Uiso 1 1 calc R . . C234 C 0.7380(6) 0.3225(3) 0.8343(8) 0.083(2) Uani 1 1 d . . . H234 H 0.734 0.2897 0.8903 0.1 Uiso 1 1 calc R . . C235 C 0.6714(6) 0.3596(3) 0.8311(9) 0.091(3) Uani 1 1 d . . . H235 H 0.6214 0.3532 0.8882 0.109 Uiso 1 1 calc R . . C236 C 0.6747(5) 0.4081(3) 0.7436(8) 0.072(2) Uani 1 1 d . . . H236 H 0.6263 0.4329 0.7402 0.087 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 0.03924(19) 0.0529(2) 0.0517(2) 0.0085(2) -0.0016(2) -0.0004(2) C1 0.043(5) 0.064(6) 0.043(5) 0 0 -0.009(5) O11 0.062(4) 0.098(5) 0.028(3) 0 0 -0.018(4) O12 0.056(3) 0.123(5) 0.037(2) 0.010(3) 0.000(2) -0.030(3) C2 0.042(5) 0.074(6) 0.030(5) 0 0 -0.005(5) O21 0.040(3) 0.107(5) 0.030(3) 0 0 -0.010(4) O22 0.068(3) 0.114(4) 0.032(2) 0.005(3) -0.006(2) -0.030(3) P1 0.0491(7) 0.0495(8) 0.0501(8) 0.0025(7) -0.0001(10) 0.0042(8) C111 0.045(3) 0.053(4) 0.045(3) -0.003(3) -0.001(3) 0.003(3) C112 0.058(4) 0.082(5) 0.058(4) 0.017(4) -0.002(4) -0.005(4) C113 0.076(5) 0.107(6) 0.072(5) 0.025(5) -0.022(4) 0.002(5) C114 0.060(5) 0.095(6) 0.102(7) 0.004(5) -0.027(5) 0.014(4) C115 0.045(4) 0.114(7) 0.107(7) -0.009(6) -0.002(5) 0.009(4) C116 0.056(4) 0.101(6) 0.075(5) 0.020(5) 0.010(4) 0.002(4) C121 0.050(3) 0.059(4) 0.048(3) 0.003(3) 0.002(4) 0.009(3) C122 0.076(5) 0.067(4) 0.064(4) -0.012(4) -0.004(4) 0.006(4) C123 0.077(5) 0.081(5) 0.102(6) -0.032(5) 0.000(6) 0.004(5) C124 0.090(6) 0.135(8) 0.079(6) -0.051(6) -0.003(6) 0.007(7) C125 0.138(9) 0.145(8) 0.052(5) -0.012(5) -0.013(6) 0.025(8) C126 0.104(7) 0.083(5) 0.060(5) 0.006(4) 0.000(5) 0.006(5) C131 0.048(4) 0.052(4) 0.056(4) 0.010(3) 0.004(3) 0.007(3) C132 0.050(4) 0.065(4) 0.086(5) 0.011(4) 0.000(4) -0.004(3) C133 0.058(5) 0.073(5) 0.148(9) 0.023(6) 0.007(6) -0.005(4) C134 0.063(5) 0.107(7) 0.122(8) 0.034(6) 0.035(6) 0.009(5) C135 0.083(6) 0.117(7) 0.104(7) -0.011(6) 0.037(6) 0.013(6) C136 0.059(4) 0.096(6) 0.080(5) -0.004(5) 0.008(4) 0.002(4) P2 0.0440(8) 0.0490(9) 0.0469(9) 0.0032(6) -0.0027(7) 0.0026(7) C211 0.061(4) 0.046(3) 0.044(3) 0.007(3) -0.002(3) 0.003(3) C212 0.067(4) 0.074(5) 0.056(4) 0.001(4) 0.003(4) 0.006(4) C213 0.107(7) 0.111(7) 0.044(4) -0.004(4) -0.011(5) -0.004(6) C214 0.106(6) 0.077(5) 0.059(5) -0.002(4) 0.024(6) -0.009(6) C215 0.066(4) 0.066(5) 0.090(6) -0.004(4) 0.021(5) 0.002(4) C216 0.052(4) 0.058(4) 0.064(4) -0.005(3) 0.012(3) 0.004(3) C221 0.043(3) 0.042(3) 0.055(3) -0.006(3) -0.004(3) 0.005(3) C222 0.070(5) 0.058(4) 0.072(4) 0.005(3) -0.018(4) -0.002(3) C223 0.080(5) 0.062(5) 0.107(7) 0.005(5) -0.021(5) -0.016(4) C224 0.069(5) 0.072(5) 0.104(7) -0.029(5) -0.012(5) -0.004(4) C225 0.090(6) 0.086(5) 0.070(5) -0.016(4) -0.024(4) -0.003(4) C226 0.074(5) 0.071(5) 0.054(4) 0.004(3) -0.014(3) -0.010(3) C231 0.049(3) 0.044(3) 0.048(4) 0.001(3) -0.005(3) -0.001(3) C232 0.077(5) 0.066(4) 0.085(5) 0.023(4) 0.011(4) 0.019(4) C233 0.095(6) 0.072(5) 0.091(6) 0.020(5) -0.002(5) 0.029(5) C234 0.116(7) 0.060(5) 0.074(5) 0.017(4) -0.027(5) -0.010(5) C235 0.081(6) 0.109(6) 0.082(6) 0.039(5) 0.006(5) -0.007(5) C236 0.065(4) 0.071(5) 0.082(5) 0.027(4) 0.005(4) 0.006(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O21 2.351(3) . ? Ag1 O11 2.353(3) . ? Ag1 P2 2.4409(17) . ? Ag1 P1 2.4574(16) . ? C1 O11 1.251(9) . ? C1 O12 1.295(5) 2_665 ? C1 O12 1.295(5) . ? O11 Ag1 2.353(3) 2_665 ? O12 H12 0.82 . ? C2 O21 1.269(9) . ? C2 O22 1.277(5) . ? C2 O22 1.277(5) 2_665 ? O21 Ag1 2.351(3) 2_665 ? O22 H22 0.82 . ? P1 C131 1.823(6) . ? P1 C121 1.828(6) . ? P1 C111 1.829(6) . ? C111 C116 1.368(8) . ? C111 C112 1.371(8) . ? C112 C113 1.384(9) . ? C112 H112 0.93 . ? C113 C114 1.373(10) . ? C113 H113 0.93 . ? C114 C115 1.343(11) . ? C114 H114 0.93 . ? C115 C116 1.395(9) . ? C115 H115 0.93 . ? C116 H116 0.93 . ? C121 C122 1.365(8) . ? C121 C126 1.388(8) . ? C122 C123 1.370(9) . ? C122 H122 0.93 . ? C123 C124 1.368(11) . ? C123 H123 0.93 . ? C124 C125 1.347(11) . ? C124 H124 0.93 . ? C125 C126 1.381(10) . ? C125 H125 0.93 . ? C126 H126 0.93 . ? C131 C132 1.376(8) . ? C131 C136 1.395(9) . ? C132 C133 1.373(10) . ? C132 H132 0.93 . ? C133 C134 1.375(12) . ? C133 H133 0.93 . ? C134 C135 1.373(11) . ? C134 H134 0.93 . ? C135 C136 1.381(10) . ? C135 H135 0.93 . ? C136 H136 0.93 . ? P2 C221 1.821(5) . ? P2 C231 1.824(6) . ? P2 C211 1.824(6) . ? C211 C212 1.391(8) . ? C211 C216 1.403(8) . ? C212 C213 1.380(9) . ? C212 H212 0.93 . ? C213 C214 1.376(10) . ? C213 H213 0.93 . ? C214 C215 1.350(10) . ? C214 H214 0.93 . ? C215 C216 1.387(8) . ? C215 H215 0.93 . ? C216 H216 0.93 . ? C221 C226 1.382(8) . ? C221 C222 1.391(8) . ? C222 C223 1.383(9) . ? C222 H222 0.93 . ? C223 C224 1.377(10) . ? C223 H223 0.93 . ? C224 C225 1.337(10) . ? C224 H224 0.93 . ? C225 C226 1.370(8) . ? C225 H225 0.93 . ? C226 H226 0.93 . ? C231 C236 1.368(8) . ? C231 C232 1.381(8) . ? C232 C233 1.363(9) . ? C232 H232 0.93 . ? C233 C234 1.358(10) . ? C233 H233 0.93 . ? C234 C235 1.323(10) . ? C234 H234 0.93 . ? C235 C236 1.399(9) . ? C235 H235 0.93 . ? C236 H236 0.93 . ? 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 O21 Ag1 O11 76.19(14) . . ? O21 Ag1 P2 111.24(6) . . ? O11 Ag1 P2 121.37(5) . . ? O21 Ag1 P1 117.87(4) . . ? O11 Ag1 P1 101.63(6) . . ? P2 Ag1 P1 120.55(5) . . ? O11 C1 O12 120.3(4) . 2_665 ? O11 C1 O12 120.3(4) . . ? O12 C1 O12 119.5(7) 2_665 . ? C1 O11 Ag1 128.13(10) . . ? C1 O11 Ag1 128.13(10) . 2_665 ? Ag1 O11 Ag1 103.7(2) . 2_665 ? C1 O12 H12 109.5 . . ? O21 C2 O22 119.7(4) . . ? O21 C2 O22 119.7(4) . 2_665 ? O22 C2 O22 120.6(7) . 2_665 ? C2 O21 Ag1 128.06(10) . 2_665 ? C2 O21 Ag1 128.06(10) . . ? Ag1 O21 Ag1 103.9(2) 2_665 . ? C2 O22 H22 109.5 . . ? C131 P1 C121 104.7(3) . . ? C131 P1 C111 104.7(2) . . ? C121 P1 C111 101.5(3) . . ? C131 P1 Ag1 109.6(2) . . ? C121 P1 Ag1 116.27(18) . . ? C111 P1 Ag1 118.7(2) . . ? C116 C111 C112 118.2(6) . . ? C116 C111 P1 116.8(5) . . ? C112 C111 P1 124.9(5) . . ? C111 C112 C113 120.8(6) . . ? C111 C112 H112 119.6 . . ? C113 C112 H112 119.6 . . ? C114 C113 C112 120.3(7) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 119.2(7) . . ? C115 C114 H114 120.4 . . ? C113 C114 H114 120.4 . . ? C114 C115 C116 120.8(7) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C111 C116 C115 120.6(7) . . ? C111 C116 H116 119.7 . . ? C115 C116 H116 119.7 . . ? C122 C121 C126 118.7(6) . . ? C122 C121 P1 122.8(5) . . ? C126 C121 P1 118.5(5) . . ? C121 C122 C123 121.8(7) . . ? C121 C122 H122 119.1 . . ? C123 C122 H122 119.1 . . ? C124 C123 C122 119.1(7) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C125 C124 C123 120.1(8) . . ? C125 C124 H124 120 . . ? C123 C124 H124 120 . . ? C124 C125 C126 121.5(8) . . ? C124 C125 H125 119.2 . . ? C126 C125 H125 119.2 . . ? C125 C126 C121 118.8(7) . . ? C125 C126 H126 120.6 . . ? C121 C126 H126 120.6 . . ? C132 C131 C136 118.3(6) . . ? C132 C131 P1 125.1(5) . . ? C136 C131 P1 116.3(5) . . ? C133 C132 C131 121.3(8) . . ? C133 C132 H132 119.3 . . ? C131 C132 H132 119.3 . . ? C132 C133 C134 120.3(8) . . ? C132 C133 H133 119.9 . . ? C134 C133 H133 119.9 . . ? C135 C134 C133 119.3(8) . . ? C135 C134 H134 120.3 . . ? C133 C134 H134 120.3 . . ? C134 C135 C136 120.7(9) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C135 C136 C131 120.1(8) . . ? C135 C136 H136 120 . . ? C131 C136 H136 120 . . ? C221 P2 C231 103.5(3) . . ? C221 P2 C211 104.1(3) . . ? C231 P2 C211 104.6(3) . . ? C221 P2 Ag1 111.65(18) . . ? C231 P2 Ag1 117.3(2) . . ? C211 P2 Ag1 114.28(18) . . ? C212 C211 C216 118.9(6) . . ? C212 C211 P2 117.7(4) . . ? C216 C211 P2 123.4(4) . . ? C213 C212 C211 120.0(7) . . ? C213 C212 H212 120 . . ? C211 C212 H212 120 . . ? C214 C213 C212 120.6(7) . . ? C214 C213 H213 119.7 . . ? C212 C213 H213 119.7 . . ? C215 C214 C213 120.0(7) . . ? C215 C214 H214 120 . . ? C213 C214 H214 120 . . ? C214 C215 C216 121.2(7) . . ? C214 C215 H215 119.4 . . ? C216 C215 H215 119.4 . . ? C215 C216 C211 119.4(6) . . ? C215 C216 H216 120.3 . . ? C211 C216 H216 120.3 . . ? C226 C221 C222 116.7(6) . . ? C226 C221 P2 123.9(5) . . ? C222 C221 P2 119.2(4) . . ? C223 C222 C221 121.5(7) . . ? C223 C222 H222 119.2 . . ? C221 C222 H222 119.2 . . ? C224 C223 C222 119.6(8) . . ? C224 C223 H223 120.2 . . ? C222 C223 H223 120.2 . . ? C225 C224 C223 119.3(8) . . ? C225 C224 H224 120.4 . . ? C223 C224 H224 120.4 . . ? C224 C225 C226 121.9(7) . . ? C224 C225 H225 119.1 . . ? C226 C225 H225 119.1 . . ? C225 C226 C221 121.1(7) . . ? C225 C226 H226 119.5 . . ? C221 C226 H226 119.5 . . ? C236 C231 C232 117.3(6) . . ? C236 C231 P2 118.3(5) . . ? C232 C231 P2 124.4(5) . . ? C233 C232 C231 121.1(7) . . ? C233 C232 H232 119.5 . . ? C231 C232 H232 119.5 . . ? C234 C233 C232 120.9(7) . . ? C234 C233 H233 119.5 . . ? C232 C233 H233 119.5 . . ? C235 C234 C233 119.2(7) . . ? C235 C234 H234 120.4 . . ? C233 C234 H234 120.4 . . ? C234 C235 C236 121.3(8) . . ? C234 C235 H235 119.4 . . ? C236 C235 H235 119.4 . . ? C231 C236 C235 120.2(7) . . ? C231 C236 H236 119.9 . . ? C235 C236 H236 119.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12 H12 O22 0.82 1.86 2.591(5) 147.1 1_554 O22 H22 O12 0.82 1.85 2.591(5) 149.2 1_556 #===END # Attachment 'gb1038.cif' data_gb1038 _database_code_depnum_ccdc_archive 'CCDC 795572' #TrackingRef 'gb1038.cif' _audit_creation_date 2010-06-15T08:55:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C73 H64 Ag2 O5 P4' _chemical_formula_moiety 'C73 H60 Ag2 O3 P4,2(H2 O)' _chemical_formula_weight 1360.86 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1730(3) _cell_length_b 13.1340(6) _cell_length_c 21.6602(10) _cell_angle_alpha 88.890(4) _cell_angle_beta 82.094(3) _cell_angle_gamma 62.430(4) _cell_volume 3036.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13107 _cell_measurement_theta_min 3.488 _cell_measurement_theta_max 29.2591 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.1711 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.0601 _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 2 0.0432 0 -1 -2 0.0323 -13 8 18 0.0506 -1 0 -1 0.0341 1 0 1 0.0382 0 0 -2 0.0344 0 0 2 0.0257 0 1 0 0.0806 0 -1 0 0.0561 2 -27 11 0.0605 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.965 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0048029637 _diffrn_orient_matrix_ub_12 0.0214397698 _diffrn_orient_matrix_ub_13 0.022272158 _diffrn_orient_matrix_ub_21 0.0034805832 _diffrn_orient_matrix_ub_22 0.0248370354 _diffrn_orient_matrix_ub_23 -0.0205636991 _diffrn_orient_matrix_ub_31 -0.0584785913 _diffrn_orient_matrix_ub_32 0.0042629455 _diffrn_orient_matrix_ub_33 -0.0032507129 _diffrn_measurement_device_type 'Oxford Diffraction Gemini, Ruby ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_av_unetI/netI 0.1399 _diffrn_reflns_number 28935 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 29.43 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.868 _reflns_number_total 12361 _reflns_number_gt 8081 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. Solvent modelled as two water molecules of which one is disordered over two sites with sof 0.730(14) and its complement. The oxygen atoms of the disordered water molecules were refined with isotropic displacement parameters since refinement as aniso gave unacceptable values even with reasonable restraints. Water molecule hydrogen atoms were not included. ADP restraints were applied to one Ph ring and to the carbonate O(3). Although there are voids in the lattice no further significant e-density was observed and use of the program SQUEEZE did not provide an improvement. ; _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^)+(0.0750P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12361 _refine_ls_number_parameters 757 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1579 _refine_ls_wR_factor_gt 0.139 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.419 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.155 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.85117(4) 0.64516(4) 0.850765(19) 0.02184(11) Uani 1 1 d . . . Ag2 Ag 0.99585(4) 0.66130(3) 0.648531(18) 0.01640(10) Uani 1 1 d . . . P1 P 0.70135(13) 0.58330(12) 0.90049(7) 0.0194(3) Uani 1 1 d . . . C111 C 0.7104(6) 0.4518(5) 0.8701(3) 0.0265(13) Uani 1 1 d U . . C112 C 0.7259(7) 0.4375(6) 0.8067(3) 0.0453(15) Uani 1 1 d U . . H112 H 0.7378 0.4925 0.7815 0.054 Uiso 1 1 calc R . . C113 C 0.7246(8) 0.3404(6) 0.7771(4) 0.0535(16) Uani 1 1 d U . . H113 H 0.7294 0.3335 0.7332 0.064 Uiso 1 1 calc R . . C114 C 0.7163(7) 0.2589(6) 0.8149(3) 0.0440(16) Uani 1 1 d U . . H114 H 0.7186 0.1925 0.7968 0.053 Uiso 1 1 calc R . . C115 C 0.7048(5) 0.2716(5) 0.8781(3) 0.0309(15) Uani 1 1 d . . . H115 H 0.6985 0.2143 0.9036 0.037 Uiso 1 1 calc R . . C116 C 0.7021(5) 0.3676(5) 0.9059(3) 0.0246(13) Uani 1 1 d . . . H116 H 0.6945 0.3748 0.95 0.03 Uiso 1 1 calc R . . C121 C 0.7184(5) 0.5555(5) 0.9813(3) 0.0198(12) Uani 1 1 d . . . C122 C 0.8411(5) 0.4972(5) 0.9983(3) 0.0265(14) Uani 1 1 d . . . H122 H 0.9117 0.4704 0.9666 0.032 Uiso 1 1 calc R . . C123 C 0.8594(6) 0.4789(5) 1.0594(3) 0.0334(16) Uani 1 1 d . . . H123 H 0.9421 0.4375 1.0692 0.04 Uiso 1 1 calc R . . C124 C 0.7603(6) 0.5194(5) 1.1066(3) 0.0276(14) Uani 1 1 d . . . H124 H 0.7733 0.5092 1.149 0.033 Uiso 1 1 calc R . . C125 C 0.6388(6) 0.5765(5) 1.0908(3) 0.0267(14) Uani 1 1 d . . . H125 H 0.5689 0.6026 1.123 0.032 Uiso 1 1 calc R . . C126 C 0.6193(5) 0.5950(5) 1.0304(3) 0.0231(13) Uani 1 1 d . . . H126 H 0.5359 0.6359 1.0213 0.028 Uiso 1 1 calc R . . C131 C 0.5381(5) 0.6888(5) 0.9031(2) 0.0177(11) Uani 1 1 d . . . C132 C 0.4408(5) 0.6595(5) 0.9084(3) 0.0313(15) Uani 1 1 d . . . H132 H 0.4595 0.5809 0.9103 0.038 Uiso 1 1 calc R . . C133 C 0.3184(5) 0.7424(5) 0.9111(3) 0.0314(15) Uani 1 1 d . . . H133 H 0.2532 0.7212 0.9147 0.038 Uiso 1 1 calc R . . C134 C 0.2904(5) 0.8577(5) 0.9085(3) 0.0261(13) Uani 1 1 d . . . H134 H 0.2057 0.9156 0.9119 0.031 Uiso 1 1 calc R . . C135 C 0.3852(5) 0.8877(5) 0.9011(2) 0.0216(12) Uani 1 1 d . . . H135 H 0.3663 0.9661 0.8974 0.026 Uiso 1 1 calc R . . C136 C 0.5093(5) 0.8035(5) 0.8991(2) 0.0217(12) Uani 1 1 d . . . H136 H 0.5743 0.825 0.895 0.026 Uiso 1 1 calc R . . P2 P 0.86638(13) 0.81303(12) 0.88388(7) 0.0201(3) Uani 1 1 d . . . C211 C 0.9037(5) 0.8149(5) 0.9616(3) 0.0210(12) Uani 1 1 d . . . C212 C 0.8516(5) 0.7697(5) 1.0087(3) 0.0258(13) Uani 1 1 d . . . H212 H 0.7979 0.7402 0.9986 0.031 Uiso 1 1 calc R . . C213 C 0.8750(6) 0.7662(5) 1.0688(3) 0.0328(15) Uani 1 1 d . . . H213 H 0.8356 0.7378 1.1004 0.039 Uiso 1 1 calc R . . C214 C 0.9574(6) 0.8048(5) 1.0827(3) 0.0329(15) Uani 1 1 d . . . H214 H 0.9768 0.801 1.124 0.04 Uiso 1 1 calc R . . C215 C 1.0121(6) 0.8495(6) 1.0363(3) 0.0351(15) Uani 1 1 d . . . H215 H 1.0682 0.8765 1.0461 0.042 Uiso 1 1 calc R . . C216 C 0.9846(5) 0.8543(5) 0.9771(3) 0.0260(13) Uani 1 1 d . . . H216 H 1.0217 0.8853 0.9459 0.031 Uiso 1 1 calc R . . C221 C 0.7196(5) 0.9451(5) 0.8830(3) 0.0199(12) Uani 1 1 d . . . C222 C 0.6478(5) 1.0092(5) 0.9388(2) 0.0230(12) Uani 1 1 d . . . H222 H 0.6799 0.9903 0.9773 0.028 Uiso 1 1 calc R . . C223 C 0.5293(6) 1.1002(5) 0.9364(3) 0.0292(14) Uani 1 1 d . . . H223 H 0.4786 1.1413 0.9739 0.035 Uiso 1 1 calc R . . C224 C 0.4848(6) 1.1314(5) 0.8808(3) 0.0271(14) Uani 1 1 d . . . H224 H 0.4047 1.1953 0.8797 0.033 Uiso 1 1 calc R . . C225 C 0.5568(6) 1.0694(5) 0.8255(3) 0.0284(14) Uani 1 1 d . . . H225 H 0.5262 1.0917 0.7868 0.034 Uiso 1 1 calc R . . C226 C 0.6714(5) 0.9767(5) 0.8273(3) 0.0254(13) Uani 1 1 d . . . H226 H 0.7188 0.9334 0.7897 0.031 Uiso 1 1 calc R . . C231 C 0.9838(5) 0.8385(5) 0.8333(3) 0.0239(13) Uani 1 1 d . . . C232 C 0.9808(6) 0.9448(6) 0.8301(3) 0.0293(14) Uani 1 1 d . . . H232 H 0.914 1.0099 0.8532 0.035 Uiso 1 1 calc R . . C233 C 1.0780(7) 0.9554(7) 0.7922(3) 0.047(2) Uani 1 1 d . . . H233 H 1.0786 1.0275 0.7902 0.057 Uiso 1 1 calc R . . C234 C 1.1731(7) 0.8600(8) 0.7577(3) 0.048(2) Uani 1 1 d . . . H234 H 1.2377 0.8675 0.7313 0.058 Uiso 1 1 calc R . . C235 C 1.1751(6) 0.7562(7) 0.7613(3) 0.0420(18) Uani 1 1 d . . . H235 H 1.2416 0.6912 0.7381 0.05 Uiso 1 1 calc R . . C236 C 1.0797(5) 0.7444(6) 0.7991(3) 0.0287(14) Uani 1 1 d . . . H236 H 1.0808 0.6716 0.8012 0.034 Uiso 1 1 calc R . . P3 P 1.21170(12) 0.58677(12) 0.59819(6) 0.0167(3) Uani 1 1 d . . . C311 C 1.3343(5) 0.4573(5) 0.6242(3) 0.0191(12) Uani 1 1 d . . . C312 C 1.4343(5) 0.3780(5) 0.5841(3) 0.0206(12) Uani 1 1 d . . . H312 H 1.4378 0.3873 0.5403 0.025 Uiso 1 1 calc R . . C313 C 1.5306(5) 0.2840(5) 0.6073(3) 0.0260(14) Uani 1 1 d . . . H313 H 1.5991 0.2294 0.5793 0.031 Uiso 1 1 calc R . . C314 C 1.5265(6) 0.2704(5) 0.6700(3) 0.0306(15) Uani 1 1 d . . . H314 H 1.5941 0.2086 0.6859 0.037 Uiso 1 1 calc R . . C315 C 1.4250(7) 0.3459(6) 0.7099(3) 0.052(2) Uani 1 1 d . . . H315 H 1.4204 0.3348 0.7534 0.062 Uiso 1 1 calc R . . C316 C 1.3287(6) 0.4386(6) 0.6873(3) 0.0395(17) Uani 1 1 d . . . H316 H 1.2579 0.4899 0.7154 0.047 Uiso 1 1 calc R . . C321 C 1.2215(4) 0.5527(4) 0.5165(2) 0.0150(11) Uani 1 1 d . . . C322 C 1.2793(5) 0.5901(5) 0.4676(3) 0.0209(12) Uani 1 1 d . . . H322 H 1.3216 0.6318 0.477 0.025 Uiso 1 1 calc R . . C323 C 1.2766(5) 0.5682(5) 0.4063(3) 0.0235(13) Uani 1 1 d . . . H323 H 1.3161 0.5955 0.3741 0.028 Uiso 1 1 calc R . . C324 C 1.2165(5) 0.5063(5) 0.3909(3) 0.0224(12) Uani 1 1 d . . . H324 H 1.2143 0.4915 0.3484 0.027 Uiso 1 1 calc R . . C325 C 1.1602(5) 0.4667(5) 0.4380(3) 0.0270(14) Uani 1 1 d . . . H325 H 1.1197 0.4237 0.428 0.032 Uiso 1 1 calc R . . C326 C 1.1623(5) 0.4891(5) 0.4994(3) 0.0237(13) Uani 1 1 d . . . H326 H 1.123 0.461 0.5312 0.028 Uiso 1 1 calc R . . C331 C 1.2727(5) 0.6900(5) 0.5961(2) 0.0164(11) Uani 1 1 d . . . C332 C 1.1915(5) 0.8062(5) 0.5964(2) 0.0176(11) Uani 1 1 d . . . H332 H 1.1042 0.8306 0.5992 0.021 Uiso 1 1 calc R . . C333 C 1.2329(5) 0.8874(5) 0.5926(2) 0.0189(12) Uani 1 1 d . . . H333 H 1.1748 0.9667 0.5926 0.023 Uiso 1 1 calc R . . C334 C 1.3592(5) 0.8535(5) 0.5888(2) 0.0218(12) Uani 1 1 d . . . H334 H 1.3884 0.9094 0.5855 0.026 Uiso 1 1 calc R . . C335 C 1.4427(5) 0.7392(5) 0.5900(3) 0.0273(14) Uani 1 1 d . . . H335 H 1.5295 0.7163 0.5882 0.033 Uiso 1 1 calc R . . C336 C 1.4011(5) 0.6568(5) 0.5937(3) 0.0241(13) Uani 1 1 d . . . H336 H 1.4594 0.5778 0.5947 0.029 Uiso 1 1 calc R . . P4 P 0.81796(12) 0.82730(11) 0.61373(6) 0.0154(3) Uani 1 1 d . . . C411 C 0.6672(5) 0.8720(5) 0.6617(2) 0.0186(12) Uani 1 1 d . . . C412 C 0.6516(5) 0.7909(5) 0.7004(2) 0.0208(12) Uani 1 1 d . . . H412 H 0.7187 0.7159 0.7023 0.025 Uiso 1 1 calc R . . C413 C 0.5349(5) 0.8241(6) 0.7360(3) 0.0272(14) Uani 1 1 d . . . H413 H 0.5221 0.7708 0.7624 0.033 Uiso 1 1 calc R . . C414 C 0.4376(6) 0.9331(6) 0.7335(3) 0.0323(15) Uani 1 1 d . . . H414 H 0.359 0.9542 0.7584 0.039 Uiso 1 1 calc R . . C415 C 0.4535(5) 1.0122(5) 0.6950(2) 0.0243(13) Uani 1 1 d . . . H415 H 0.3859 1.0869 0.6932 0.029 Uiso 1 1 calc R . . C416 C 0.5684(5) 0.9816(5) 0.6594(2) 0.0172(11) Uani 1 1 d . . . H416 H 0.5799 1.0358 0.6332 0.021 Uiso 1 1 calc R . . C421 C 0.8428(4) 0.9537(4) 0.6148(2) 0.0156(11) Uani 1 1 d . . . C422 C 0.8730(5) 0.9836(5) 0.6687(3) 0.0216(12) Uani 1 1 d . . . H422 H 0.8751 0.9404 0.7046 0.026 Uiso 1 1 calc R . . C423 C 0.9001(5) 1.0742(5) 0.6718(3) 0.0252(13) Uani 1 1 d . . . H423 H 0.9195 1.0939 0.7094 0.03 Uiso 1 1 calc R . . C424 C 0.8986(5) 1.1358(5) 0.6190(3) 0.0248(13) Uani 1 1 d . . . H424 H 0.9168 1.1986 0.6206 0.03 Uiso 1 1 calc R . . C425 C 0.8708(5) 1.1073(5) 0.5640(3) 0.0258(13) Uani 1 1 d . . . H425 H 0.8713 1.1494 0.5279 0.031 Uiso 1 1 calc R . . C426 C 0.8422(5) 1.0170(5) 0.5619(2) 0.0183(11) Uani 1 1 d . . . H426 H 0.8222 0.9979 0.5244 0.022 Uiso 1 1 calc R . . C431 C 0.7888(5) 0.8157(4) 0.5346(2) 0.0145(11) Uani 1 1 d . . . C432 C 0.6714(5) 0.8510(5) 0.5188(3) 0.0211(12) Uani 1 1 d . . . H432 H 0.5998 0.888 0.5496 0.025 Uiso 1 1 calc R . . C433 C 0.6560(6) 0.8334(5) 0.4582(3) 0.0251(13) Uani 1 1 d . . . H433 H 0.5742 0.8598 0.4477 0.03 Uiso 1 1 calc R . . C434 C 0.7595(5) 0.7774(5) 0.4132(3) 0.0239(13) Uani 1 1 d . . . H434 H 0.7488 0.764 0.372 0.029 Uiso 1 1 calc R . . C435 C 0.8788(5) 0.7409(5) 0.4281(3) 0.0238(13) Uani 1 1 d . . . H435 H 0.9501 0.703 0.3971 0.029 Uiso 1 1 calc R . . C436 C 0.8933(5) 0.7601(5) 0.4880(2) 0.0190(12) Uani 1 1 d . . . H436 H 0.9751 0.7354 0.4981 0.023 Uiso 1 1 calc R . . C1 C 0.9973(6) 0.5052(6) 0.7441(3) 0.0351(14) Uani 1 1 d U . . O1 O 0.9217(3) 0.6146(4) 0.73863(19) 0.0427(13) Uani 1 1 d U . . O2 O 1.0172(4) 0.4741(4) 0.79940(18) 0.0303(10) Uani 1 1 d U . . O3 O 1.0439(5) 0.4387(5) 0.6977(2) 0.0626(16) Uani 1 1 d DU . . O4 O 1.2330(5) 0.2753(5) 0.7931(2) 0.0626(16) Uani 1 1 d . . . O5 O 1.0718(8) 0.2152(8) 0.7308(4) 0.075(3) Uiso 0.730(14) 1 d P . . O6 O 0.9602(19) 0.2941(16) 0.7147(9) 0.057(7) Uiso 0.270(14) 1 d PD . . 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 0.0196(2) 0.0223(2) 0.0279(3) 0.00345(19) -0.00396(17) -0.01334(19) Ag2 0.0155(2) 0.0179(2) 0.0165(2) 0.00122(17) -0.00225(15) -0.00831(17) P1 0.0172(7) 0.0194(7) 0.0247(8) 0.0016(6) -0.0027(6) -0.0112(6) C111 0.036(3) 0.026(3) 0.030(3) 0.004(2) -0.008(2) -0.023(3) C112 0.078(4) 0.032(3) 0.038(3) 0.006(2) -0.020(3) -0.032(3) C113 0.088(4) 0.039(3) 0.042(3) 0.004(3) -0.021(3) -0.033(3) C114 0.065(4) 0.035(3) 0.049(4) 0.006(3) -0.016(3) -0.036(3) C115 0.018(3) 0.021(3) 0.053(5) 0.004(3) 0.002(3) -0.010(3) C116 0.016(3) 0.025(3) 0.031(3) 0.002(3) 0.002(2) -0.009(3) C121 0.019(3) 0.017(3) 0.026(3) 0.001(2) -0.005(2) -0.011(2) C122 0.020(3) 0.032(3) 0.026(4) 0.002(3) -0.002(2) -0.011(3) C123 0.023(3) 0.030(4) 0.046(4) 0.015(3) -0.010(3) -0.010(3) C124 0.034(3) 0.032(3) 0.025(3) 0.009(3) -0.019(3) -0.019(3) C125 0.029(3) 0.027(3) 0.025(3) 0.001(3) 0.002(3) -0.014(3) C126 0.014(3) 0.017(3) 0.036(4) 0.006(2) -0.005(2) -0.006(2) C131 0.021(3) 0.025(3) 0.011(3) 0.002(2) -0.005(2) -0.013(2) C132 0.024(3) 0.025(3) 0.052(4) 0.007(3) -0.011(3) -0.016(3) C133 0.022(3) 0.033(4) 0.047(4) 0.011(3) -0.020(3) -0.016(3) C134 0.020(3) 0.031(3) 0.023(3) 0.002(3) -0.010(2) -0.006(3) C135 0.034(3) 0.021(3) 0.011(3) 0.002(2) -0.003(2) -0.013(3) C136 0.024(3) 0.027(3) 0.021(3) 0.000(2) -0.004(2) -0.017(3) P2 0.0184(7) 0.0215(7) 0.0223(8) 0.0034(6) -0.0028(6) -0.0111(6) C211 0.013(3) 0.021(3) 0.024(3) 0.005(2) -0.004(2) -0.005(2) C212 0.023(3) 0.027(3) 0.027(3) 0.006(3) -0.004(2) -0.012(3) C213 0.025(3) 0.032(4) 0.034(4) 0.013(3) -0.003(3) -0.007(3) C214 0.038(4) 0.032(4) 0.023(3) -0.002(3) -0.011(3) -0.009(3) C215 0.033(4) 0.031(4) 0.046(4) 0.004(3) -0.015(3) -0.016(3) C216 0.019(3) 0.021(3) 0.036(4) 0.003(3) -0.006(2) -0.007(2) C221 0.018(3) 0.016(3) 0.029(3) 0.003(2) 0.000(2) -0.012(2) C222 0.035(3) 0.028(3) 0.013(3) 0.002(2) -0.011(2) -0.019(3) C223 0.026(3) 0.024(3) 0.038(4) 0.000(3) -0.003(3) -0.012(3) C224 0.024(3) 0.018(3) 0.043(4) -0.001(3) -0.008(3) -0.013(3) C225 0.037(4) 0.032(3) 0.029(4) 0.009(3) -0.019(3) -0.024(3) C226 0.029(3) 0.017(3) 0.034(4) -0.002(2) -0.005(3) -0.013(3) C231 0.021(3) 0.040(4) 0.021(3) 0.013(3) -0.009(2) -0.021(3) C232 0.033(3) 0.039(4) 0.030(3) 0.016(3) -0.023(3) -0.024(3) C233 0.069(5) 0.067(5) 0.044(5) 0.035(4) -0.034(4) -0.059(5) C234 0.051(5) 0.102(7) 0.020(4) 0.009(4) -0.008(3) -0.058(5) C235 0.044(4) 0.082(6) 0.018(3) -0.007(3) 0.004(3) -0.047(4) C236 0.028(3) 0.049(4) 0.018(3) 0.005(3) -0.007(2) -0.024(3) P3 0.0146(7) 0.0169(7) 0.0172(8) 0.0018(5) -0.0021(5) -0.0063(6) C311 0.013(3) 0.018(3) 0.029(3) 0.002(2) -0.005(2) -0.008(2) C312 0.019(3) 0.018(3) 0.027(3) 0.004(2) -0.007(2) -0.010(2) C313 0.021(3) 0.013(3) 0.043(4) 0.001(3) -0.002(3) -0.007(2) C314 0.029(3) 0.021(3) 0.047(4) 0.007(3) -0.020(3) -0.012(3) C315 0.058(5) 0.046(5) 0.030(4) 0.008(3) -0.022(3) -0.003(4) C316 0.037(4) 0.033(4) 0.024(4) -0.004(3) -0.010(3) 0.006(3) C321 0.011(2) 0.010(2) 0.018(3) 0.002(2) -0.001(2) 0.000(2) C322 0.012(3) 0.017(3) 0.031(3) 0.002(2) 0.000(2) -0.006(2) C323 0.022(3) 0.019(3) 0.022(3) 0.000(2) 0.007(2) -0.006(2) C324 0.026(3) 0.021(3) 0.018(3) -0.005(2) -0.011(2) -0.008(3) C325 0.028(3) 0.020(3) 0.035(4) -0.002(3) -0.004(3) -0.014(3) C326 0.025(3) 0.022(3) 0.025(3) 0.000(2) -0.003(2) -0.011(3) C331 0.020(3) 0.023(3) 0.009(3) 0.002(2) -0.005(2) -0.013(2) C332 0.017(3) 0.023(3) 0.014(3) 0.002(2) -0.004(2) -0.010(2) C333 0.028(3) 0.020(3) 0.008(3) 0.005(2) -0.005(2) -0.010(2) C334 0.029(3) 0.027(3) 0.017(3) -0.002(2) -0.006(2) -0.018(3) C335 0.018(3) 0.029(3) 0.037(4) -0.004(3) -0.004(2) -0.013(3) C336 0.015(3) 0.013(3) 0.038(4) 0.000(2) -0.003(2) -0.001(2) P4 0.0149(7) 0.0166(7) 0.0169(8) 0.0011(5) -0.0025(5) -0.0091(6) C411 0.018(3) 0.026(3) 0.017(3) -0.002(2) -0.001(2) -0.014(2) C412 0.022(3) 0.029(3) 0.018(3) 0.003(2) -0.009(2) -0.015(3) C413 0.034(3) 0.043(4) 0.021(3) 0.004(3) -0.003(3) -0.031(3) C414 0.025(3) 0.055(4) 0.026(3) -0.010(3) 0.004(3) -0.028(3) C415 0.015(3) 0.041(4) 0.019(3) -0.007(3) -0.005(2) -0.014(3) C416 0.014(3) 0.025(3) 0.015(3) -0.004(2) -0.005(2) -0.011(2) C421 0.007(2) 0.013(3) 0.027(3) 0.000(2) -0.005(2) -0.004(2) C422 0.029(3) 0.016(3) 0.021(3) 0.001(2) -0.001(2) -0.012(2) C423 0.026(3) 0.024(3) 0.028(3) -0.002(2) -0.012(2) -0.012(3) C424 0.019(3) 0.020(3) 0.040(4) 0.003(3) -0.010(2) -0.011(2) C425 0.025(3) 0.020(3) 0.034(4) 0.009(3) -0.005(3) -0.012(3) C426 0.015(3) 0.027(3) 0.016(3) 0.002(2) -0.009(2) -0.010(2) C431 0.017(3) 0.016(3) 0.013(3) 0.003(2) -0.001(2) -0.010(2) C432 0.025(3) 0.019(3) 0.020(3) -0.002(2) -0.002(2) -0.011(2) C433 0.026(3) 0.031(3) 0.022(3) 0.003(3) -0.015(2) -0.013(3) C434 0.039(4) 0.025(3) 0.011(3) 0.003(2) -0.008(2) -0.017(3) C435 0.028(3) 0.024(3) 0.018(3) -0.001(2) 0.002(2) -0.011(3) C436 0.017(3) 0.022(3) 0.022(3) -0.001(2) -0.001(2) -0.013(2) C1 0.017(3) 0.056(3) 0.028(3) 0.009(3) 0.002(2) -0.016(3) O1 0.015(2) 0.056(3) 0.033(3) 0.026(2) 0.0046(17) 0.001(2) O2 0.039(2) 0.032(2) 0.017(2) 0.0026(17) -0.0031(18) -0.014(2) O3 0.038(3) 0.101(4) 0.016(2) -0.017(3) 0.003(2) -0.006(3) O4 0.040(3) 0.093(5) 0.038(3) 0.002(3) 0.001(2) -0.018(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 2.376(4) . ? Ag1 P2 2.4261(15) . ? Ag1 O1 2.438(4) . ? Ag1 P1 2.4379(13) . ? Ag2 O1 2.232(4) . ? Ag2 P3 2.4338(13) . ? Ag2 P4 2.4548(14) . ? P1 C121 1.802(6) . ? P1 C111 1.810(6) . ? P1 C131 1.815(6) . ? C111 C112 1.365(8) . ? C111 C116 1.372(8) . ? C112 C113 1.445(10) . ? C112 H112 0.95 . ? C113 C114 1.366(9) . ? C113 H113 0.95 . ? C114 C115 1.363(9) . ? C114 H114 0.95 . ? C115 C116 1.392(8) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.394(7) . ? C121 C122 1.426(8) . ? C122 C123 1.370(8) . ? C122 H122 0.95 . ? C123 C124 1.367(8) . ? C123 H123 0.95 . ? C124 C125 1.402(8) . ? C124 H124 0.95 . ? C125 C126 1.360(8) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.383(8) . ? C131 C132 1.395(8) . ? C132 C133 1.373(8) . ? C132 H132 0.95 . ? C133 C134 1.391(8) . ? C133 H133 0.95 . ? C134 C135 1.370(8) . ? C134 H134 0.95 . ? C135 C136 1.394(8) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C211 1.806(6) . ? P2 C221 1.828(6) . ? P2 C231 1.830(5) . ? C211 C216 1.386(8) . ? C211 C212 1.394(7) . ? C212 C213 1.367(8) . ? C212 H212 0.95 . ? C213 C214 1.383(9) . ? C213 H213 0.95 . ? C214 C215 1.397(9) . ? C214 H214 0.95 . ? C215 C216 1.362(8) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.386(8) . ? C221 C222 1.415(8) . ? C222 C223 1.391(8) . ? C222 H222 0.95 . ? C223 C224 1.365(8) . ? C223 H223 0.95 . ? C224 C225 1.398(8) . ? C224 H224 0.95 . ? C225 C226 1.368(8) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C236 1.379(8) . ? C231 C232 1.381(8) . ? C232 C233 1.405(9) . ? C232 H232 0.95 . ? C233 C234 1.388(11) . ? C233 H233 0.95 . ? C234 C235 1.353(11) . ? C234 H234 0.95 . ? C235 C236 1.393(8) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? P3 C321 1.808(5) . ? P3 C311 1.812(6) . ? P3 C331 1.820(5) . ? C311 C312 1.375(7) . ? C311 C316 1.382(8) . ? C312 C313 1.396(8) . ? C312 H312 0.95 . ? C313 C314 1.365(8) . ? C313 H313 0.95 . ? C314 C315 1.364(9) . ? C314 H314 0.95 . ? C315 C316 1.381(9) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 C322 1.398(7) . ? C321 C326 1.413(8) . ? C322 C323 1.371(8) . ? C322 H322 0.95 . ? C323 C324 1.392(8) . ? C323 H323 0.95 . ? C324 C325 1.378(8) . ? C324 H324 0.95 . ? C325 C326 1.373(8) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C331 C332 1.382(7) . ? C331 C336 1.409(7) . ? C332 C333 1.372(7) . ? C332 H332 0.95 . ? C333 C334 1.379(8) . ? C333 H333 0.95 . ? C334 C335 1.372(8) . ? C334 H334 0.95 . ? C335 C336 1.388(8) . ? C335 H335 0.95 . ? C336 H336 0.95 . ? P4 C411 1.815(5) . ? P4 C431 1.820(5) . ? P4 C421 1.821(5) . ? C411 C416 1.390(7) . ? C411 C412 1.408(7) . ? C412 C413 1.394(7) . ? C412 H412 0.95 . ? C413 C414 1.378(9) . ? C413 H413 0.95 . ? C414 C415 1.385(8) . ? C414 H414 0.95 . ? C415 C416 1.381(7) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C422 1.387(8) . ? C421 C426 1.400(7) . ? C422 C423 1.378(8) . ? C422 H422 0.95 . ? C423 C424 1.386(8) . ? C423 H423 0.95 . ? C424 C425 1.386(8) . ? C424 H424 0.95 . ? C425 C426 1.384(8) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C431 C432 1.375(8) . ? C431 C436 1.410(7) . ? C432 C433 1.388(7) . ? C432 H432 0.95 . ? C433 C434 1.382(8) . ? C433 H433 0.95 . ? C434 C435 1.386(8) . ? C434 H434 0.95 . ? C435 C436 1.377(7) . ? C435 H435 0.95 . ? C436 H436 0.95 . ? C1 O3 1.231(8) . ? C1 O2 1.277(7) . ? C1 O1 1.314(7) . ? O5 O6 1.36(2) . ? 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 O2 Ag1 P2 126.33(11) . . ? O2 Ag1 O1 54.32(14) . . ? P2 Ag1 O1 106.82(12) . . ? O2 Ag1 P1 103.72(11) . . ? P2 Ag1 P1 125.15(5) . . ? O1 Ag1 P1 121.16(12) . . ? O1 Ag2 P3 129.02(11) . . ? O1 Ag2 P4 106.39(11) . . ? P3 Ag2 P4 124.09(5) . . ? C121 P1 C111 102.9(3) . . ? C121 P1 C131 103.8(2) . . ? C111 P1 C131 104.6(3) . . ? C121 P1 Ag1 111.21(18) . . ? C111 P1 Ag1 117.93(19) . . ? C131 P1 Ag1 114.79(17) . . ? C112 C111 C116 118.6(6) . . ? C112 C111 P1 116.4(4) . . ? C116 C111 P1 125.0(5) . . ? C111 C112 C113 121.4(6) . . ? C111 C112 H112 119.3 . . ? C113 C112 H112 119.3 . . ? C114 C113 C112 117.4(7) . . ? C114 C113 H113 121.3 . . ? C112 C113 H113 121.3 . . ? C115 C114 C113 120.9(6) . . ? C115 C114 H114 119.5 . . ? C113 C114 H114 119.5 . . ? C114 C115 C116 120.8(6) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C111 C116 C115 120.7(6) . . ? C111 C116 H116 119.7 . . ? C115 C116 H116 119.7 . . ? C126 C121 C122 116.2(5) . . ? C126 C121 P1 124.5(4) . . ? C122 C121 P1 119.1(4) . . ? C123 C122 C121 121.5(5) . . ? C123 C122 H122 119.3 . . ? C121 C122 H122 119.3 . . ? C124 C123 C122 121.0(6) . . ? C124 C123 H123 119.5 . . ? C122 C123 H123 119.5 . . ? C123 C124 C125 118.4(6) . . ? C123 C124 H124 120.8 . . ? C125 C124 H124 120.8 . . ? C126 C125 C124 121.2(5) . . ? C126 C125 H125 119.4 . . ? C124 C125 H125 119.4 . . ? C125 C126 C121 121.7(5) . . ? C125 C126 H126 119.1 . . ? C121 C126 H126 119.1 . . ? C136 C131 C132 118.6(5) . . ? C136 C131 P1 118.3(4) . . ? C132 C131 P1 123.1(4) . . ? C133 C132 C131 121.1(6) . . ? C133 C132 H132 119.4 . . ? C131 C132 H132 119.4 . . ? C132 C133 C134 119.7(5) . . ? C132 C133 H133 120.2 . . ? C134 C133 H133 120.2 . . ? C135 C134 C133 119.9(5) . . ? C135 C134 H134 120 . . ? C133 C134 H134 120 . . ? C134 C135 C136 120.2(5) . . ? C134 C135 H135 119.9 . . ? C136 C135 H135 119.9 . . ? C131 C136 C135 120.4(5) . . ? C131 C136 H136 119.8 . . ? C135 C136 H136 119.8 . . ? C211 P2 C221 104.3(3) . . ? C211 P2 C231 104.5(3) . . ? C221 P2 C231 104.8(3) . . ? C211 P2 Ag1 116.73(18) . . ? C221 P2 Ag1 111.87(18) . . ? C231 P2 Ag1 113.5(2) . . ? C216 C211 C212 117.6(6) . . ? C216 C211 P2 124.4(4) . . ? C212 C211 P2 117.9(5) . . ? C213 C212 C211 122.4(6) . . ? C213 C212 H212 118.8 . . ? C211 C212 H212 118.8 . . ? C212 C213 C214 118.6(5) . . ? C212 C213 H213 120.7 . . ? C214 C213 H213 120.7 . . ? C213 C214 C215 120.3(6) . . ? C213 C214 H214 119.9 . . ? C215 C214 H214 119.9 . . ? C216 C215 C214 119.7(6) . . ? C216 C215 H215 120.1 . . ? C214 C215 H215 120.1 . . ? C215 C216 C211 121.3(6) . . ? C215 C216 H216 119.3 . . ? C211 C216 H216 119.3 . . ? C226 C221 C222 119.2(6) . . ? C226 C221 P2 119.1(4) . . ? C222 C221 P2 121.4(5) . . ? C223 C222 C221 118.9(5) . . ? C223 C222 H222 120.6 . . ? C221 C222 H222 120.6 . . ? C224 C223 C222 120.9(6) . . ? C224 C223 H223 119.5 . . ? C222 C223 H223 119.5 . . ? C223 C224 C225 120.1(6) . . ? C223 C224 H224 119.9 . . ? C225 C224 H224 119.9 . . ? C226 C225 C224 119.8(6) . . ? C226 C225 H225 120.1 . . ? C224 C225 H225 120.1 . . ? C225 C226 C221 121.0(6) . . ? C225 C226 H226 119.5 . . ? C221 C226 H226 119.5 . . ? C236 C231 C232 120.5(5) . . ? C236 C231 P2 116.6(4) . . ? C232 C231 P2 122.8(5) . . ? C231 C232 C233 119.0(7) . . ? C231 C232 H232 120.5 . . ? C233 C232 H232 120.5 . . ? C234 C233 C232 119.6(6) . . ? C234 C233 H233 120.2 . . ? C232 C233 H233 120.2 . . ? C235 C234 C233 120.8(6) . . ? C235 C234 H234 119.6 . . ? C233 C234 H234 119.6 . . ? C234 C235 C236 120.1(7) . . ? C234 C235 H235 119.9 . . ? C236 C235 H235 119.9 . . ? C231 C236 C235 119.9(6) . . ? C231 C236 H236 120 . . ? C235 C236 H236 120 . . ? C321 P3 C311 103.4(2) . . ? C321 P3 C331 103.1(2) . . ? C311 P3 C331 104.2(2) . . ? C321 P3 Ag2 109.48(17) . . ? C311 P3 Ag2 120.42(17) . . ? C331 P3 Ag2 114.41(17) . . ? C312 C311 C316 118.5(5) . . ? C312 C311 P3 122.9(4) . . ? C316 C311 P3 118.6(4) . . ? C311 C312 C313 120.3(5) . . ? C311 C312 H312 119.8 . . ? C313 C312 H312 119.8 . . ? C314 C313 C312 120.2(5) . . ? C314 C313 H313 119.9 . . ? C312 C313 H313 119.9 . . ? C315 C314 C313 119.7(6) . . ? C315 C314 H314 120.2 . . ? C313 C314 H314 120.2 . . ? C314 C315 C316 120.5(6) . . ? C314 C315 H315 119.8 . . ? C316 C315 H315 119.8 . . ? C315 C316 C311 120.7(6) . . ? C315 C316 H316 119.7 . . ? C311 C316 H316 119.7 . . ? C322 C321 C326 116.4(5) . . ? C322 C321 P3 124.3(4) . . ? C326 C321 P3 119.3(4) . . ? C323 C322 C321 121.8(5) . . ? C323 C322 H322 119.1 . . ? C321 C322 H322 119.1 . . ? C322 C323 C324 120.5(5) . . ? C322 C323 H323 119.7 . . ? C324 C323 H323 119.7 . . ? C325 C324 C323 119.0(5) . . ? C325 C324 H324 120.5 . . ? C323 C324 H324 120.5 . . ? C326 C325 C324 120.5(6) . . ? C326 C325 H325 119.8 . . ? C324 C325 H325 119.8 . . ? C325 C326 C321 121.8(5) . . ? C325 C326 H326 119.1 . . ? C321 C326 H326 119.1 . . ? C332 C331 C336 117.6(5) . . ? C332 C331 P3 119.7(4) . . ? C336 C331 P3 122.7(4) . . ? C333 C332 C331 122.1(5) . . ? C333 C332 H332 119 . . ? C331 C332 H332 119 . . ? C332 C333 C334 119.7(5) . . ? C332 C333 H333 120.1 . . ? C334 C333 H333 120.1 . . ? C335 C334 C333 120.1(5) . . ? C335 C334 H334 120 . . ? C333 C334 H334 120 . . ? C334 C335 C336 120.4(5) . . ? C334 C335 H335 119.8 . . ? C336 C335 H335 119.8 . . ? C335 C336 C331 120.1(5) . . ? C335 C336 H336 119.9 . . ? C331 C336 H336 119.9 . . ? C411 P4 C431 104.5(2) . . ? C411 P4 C421 104.3(2) . . ? C431 P4 C421 104.3(2) . . ? C411 P4 Ag2 115.91(18) . . ? C431 P4 Ag2 116.59(17) . . ? C421 P4 Ag2 109.99(17) . . ? C416 C411 C412 120.5(5) . . ? C416 C411 P4 121.6(4) . . ? C412 C411 P4 118.0(4) . . ? C413 C412 C411 118.0(5) . . ? C413 C412 H412 121 . . ? C411 C412 H412 121 . . ? C414 C413 C412 121.0(5) . . ? C414 C413 H413 119.5 . . ? C412 C413 H413 119.5 . . ? C413 C414 C415 120.6(5) . . ? C413 C414 H414 119.7 . . ? C415 C414 H414 119.7 . . ? C416 C415 C414 119.5(6) . . ? C416 C415 H415 120.2 . . ? C414 C415 H415 120.2 . . ? C415 C416 C411 120.3(5) . . ? C415 C416 H416 119.8 . . ? C411 C416 H416 119.8 . . ? C422 C421 C426 118.3(5) . . ? C422 C421 P4 118.8(4) . . ? C426 C421 P4 122.8(4) . . ? C423 C422 C421 122.1(5) . . ? C423 C422 H422 119 . . ? C421 C422 H422 119 . . ? C422 C423 C424 118.6(6) . . ? C422 C423 H423 120.7 . . ? C424 C423 H423 120.7 . . ? C423 C424 C425 121.0(6) . . ? C423 C424 H424 119.5 . . ? C425 C424 H424 119.5 . . ? C426 C425 C424 119.6(5) . . ? C426 C425 H425 120.2 . . ? C424 C425 H425 120.2 . . ? C425 C426 C421 120.5(5) . . ? C425 C426 H426 119.8 . . ? C421 C426 H426 119.8 . . ? C432 C431 C436 118.3(5) . . ? C432 C431 P4 123.7(4) . . ? C436 C431 P4 117.8(4) . . ? C431 C432 C433 120.9(5) . . ? C431 C432 H432 119.6 . . ? C433 C432 H432 119.6 . . ? C434 C433 C432 120.1(5) . . ? C434 C433 H433 119.9 . . ? C432 C433 H433 119.9 . . ? C433 C434 C435 120.1(5) . . ? C433 C434 H434 120 . . ? C435 C434 H434 120 . . ? C436 C435 C434 119.5(5) . . ? C436 C435 H435 120.3 . . ? C434 C435 H435 120.3 . . ? C435 C436 C431 121.1(5) . . ? C435 C436 H436 119.5 . . ? C431 C436 H436 119.5 . . ? O3 C1 O2 123.5(6) . . ? O3 C1 O1 120.4(6) . . ? O2 C1 O1 116.1(6) . . ? C1 O1 Ag2 105.8(3) . . ? C1 O1 Ag1 92.0(3) . . ? Ag2 O1 Ag1 151.9(2) . . ? C1 O2 Ag1 95.8(4) . . ? #===END # Attachment 'gb1050b.cif' data_gb1050b _database_code_depnum_ccdc_archive 'CCDC 795573' #TrackingRef 'gb1050b.cif' _audit_creation_date 2010-08-13T15:00:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C77 H79 Ag O8 P4' _chemical_formula_moiety 'C72 H60 Ag P4, 2(C2 H6 O),C H O3, 3(H2 O)' _chemical_formula_weight 1364.15 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.2112(5) _cell_length_b 20.6996(12) _cell_length_c 20.3860(13) _cell_angle_alpha 90 _cell_angle_beta 108.315(5) _cell_angle_gamma 90 _cell_volume 7295.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40487 _cell_measurement_theta_min 2.8623 _cell_measurement_theta_max 39.8352 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 18 -14 -20 0.1877 10 -8 -27 0.3008 21 -16 -3 0.1016 0 1 3 0.3817 1 1 0 0.0366 -1 -1 0 0.1287 -1 3 0 0.0277 -1 1 0 0.0923 -14 24 10 0.0607 -11 -15 24 0.4087 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.946 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0147246042 _diffrn_orient_matrix_ub_12 0.0224465949 _diffrn_orient_matrix_ub_13 -0.0189493378 _diffrn_orient_matrix_ub_21 -0.0175714692 _diffrn_orient_matrix_ub_22 -0.0176731252 _diffrn_orient_matrix_ub_23 -0.0307262528 _diffrn_orient_matrix_ub_31 -0.0340562341 _diffrn_orient_matrix_ub_32 0.0188455402 _diffrn_orient_matrix_ub_33 -0.006184146 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_number 158838 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 39.95 _diffrn_reflns_theta_full 39.75 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 22140 _reflns_number_gt 15154 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The geometries of the disordered ethanol solvent molecules were restrained to ideal values and with ADP restraints. The program Squeeze was used to effectively remove the electron density in the voids. Bicarbonate, ethanol and water molecule OH hydrogen atoms were not located. ; _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^)+(0.0886P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 22140 _refine_ls_number_parameters 468 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.449 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.132 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.666924(7) 0.75 0.01927(4) Uani 1 2 d S . . P1 P 0.12249(2) 0.739994(19) 0.780207(19) 0.02273(7) Uani 1 1 d . . . C11 C 0.13773(9) 0.79729(8) 0.85124(8) 0.0256(3) Uani 1 1 d . . . C12 C 0.07562(11) 0.83613(9) 0.85233(9) 0.0336(3) Uani 1 1 d . . . H12 H 0.0262 0.8292 0.8194 0.04 Uiso 1 1 calc R . . C13 C 0.08537(13) 0.88491(10) 0.90106(10) 0.0397(4) Uani 1 1 d . . . H13 H 0.043 0.9119 0.9007 0.048 Uiso 1 1 calc R . . C14 C 0.15722(13) 0.89429(10) 0.95048(10) 0.0414(4) Uani 1 1 d . . . H14 H 0.164 0.9279 0.9836 0.05 Uiso 1 1 calc R . . C15 C 0.21846(13) 0.85488(11) 0.95138(10) 0.0416(4) Uani 1 1 d . . . H15 H 0.2671 0.8606 0.9859 0.05 Uiso 1 1 calc R . . C16 C 0.20928(10) 0.80654(9) 0.90163(9) 0.0324(3) Uani 1 1 d . . . H16 H 0.2519 0.7799 0.9021 0.039 Uiso 1 1 calc R . . C21 C 0.12605(9) 0.79305(8) 0.70948(8) 0.0278(3) Uani 1 1 d . . . C22 C 0.14587(14) 0.85822(10) 0.71826(11) 0.0424(4) Uani 1 1 d . . . H22 H 0.1592 0.8769 0.7631 0.051 Uiso 1 1 calc R . . C23 C 0.14630(16) 0.89621(12) 0.66231(13) 0.0499(5) Uani 1 1 d . . . H23 H 0.1602 0.9405 0.6691 0.06 Uiso 1 1 calc R . . C24 C 0.12660(12) 0.86994(12) 0.59653(11) 0.0447(5) Uani 1 1 d . . . H24 H 0.1262 0.8961 0.5581 0.054 Uiso 1 1 calc R . . C25 C 0.10772(14) 0.80567(14) 0.58754(10) 0.0495(6) Uani 1 1 d . . . H25 H 0.0949 0.7871 0.5427 0.059 Uiso 1 1 calc R . . C26 C 0.10723(12) 0.76734(11) 0.64354(9) 0.0410(5) Uani 1 1 d . . . H26 H 0.0938 0.723 0.6364 0.049 Uiso 1 1 calc R . . C31 C 0.21483(9) 0.69727(9) 0.80198(8) 0.0278(3) Uani 1 1 d . . . C32 C 0.27573(10) 0.71770(11) 0.77935(10) 0.0368(4) Uani 1 1 d . . . H32 H 0.2697 0.7549 0.7509 0.044 Uiso 1 1 calc R . . C33 C 0.34541(11) 0.68391(13) 0.79823(11) 0.0450(5) Uani 1 1 d . . . H33 H 0.3866 0.698 0.7825 0.054 Uiso 1 1 calc R . . C34 C 0.35460(12) 0.62985(14) 0.83984(11) 0.0491(6) Uani 1 1 d . . . H34 H 0.4023 0.607 0.8529 0.059 Uiso 1 1 calc R . . C35 C 0.29446(14) 0.60892(13) 0.86252(11) 0.0481(5) Uani 1 1 d . . . H35 H 0.3008 0.5717 0.891 0.058 Uiso 1 1 calc R . . C36 C 0.22451(12) 0.64252(11) 0.84348(10) 0.0390(4) Uani 1 1 d . . . H36 H 0.1833 0.628 0.8589 0.047 Uiso 1 1 calc R . . P2 P -0.00235(2) 0.595042(18) 0.643767(19) 0.02093(7) Uani 1 1 d . . . C41 C -0.01242(8) 0.63958(7) 0.56398(7) 0.0225(2) Uani 1 1 d . . . C42 C -0.06693(9) 0.68981(8) 0.54659(9) 0.0281(3) Uani 1 1 d . . . H42 H -0.0975 0.699 0.5756 0.034 Uiso 1 1 calc R . . C43 C -0.07643(10) 0.72624(9) 0.48723(10) 0.0336(3) Uani 1 1 d . . . H43 H -0.1139 0.7598 0.4756 0.04 Uiso 1 1 calc R . . C44 C -0.03123(11) 0.71383(9) 0.44465(9) 0.0350(4) Uani 1 1 d . . . H44 H -0.0375 0.7391 0.4043 0.042 Uiso 1 1 calc R . . C45 C 0.02297(11) 0.66439(9) 0.46158(9) 0.0334(3) Uani 1 1 d . . . H45 H 0.0538 0.6559 0.4326 0.04 Uiso 1 1 calc R . . C46 C 0.03262(9) 0.62703(8) 0.52084(8) 0.0272(3) Uani 1 1 d . . . H46 H 0.0697 0.5931 0.5319 0.033 Uiso 1 1 calc R . . C51 C 0.08245(9) 0.54473(7) 0.65177(7) 0.0241(2) Uani 1 1 d . . . C52 C 0.15561(10) 0.57378(9) 0.67670(9) 0.0332(3) Uani 1 1 d . . . H52 H 0.16 0.6177 0.691 0.04 Uiso 1 1 calc R . . C53 C 0.22197(11) 0.53826(12) 0.68046(10) 0.0413(4) Uani 1 1 d . . . H53 H 0.2714 0.5581 0.6973 0.05 Uiso 1 1 calc R . . C54 C 0.21606(13) 0.47437(12) 0.65980(10) 0.0441(5) Uani 1 1 d . . . H54 H 0.2613 0.4507 0.6614 0.053 Uiso 1 1 calc R . . C55 C 0.14457(14) 0.44493(10) 0.63686(12) 0.0428(5) Uani 1 1 d . . . H55 H 0.141 0.4007 0.6239 0.051 Uiso 1 1 calc R . . C56 C 0.07736(12) 0.47974(8) 0.63249(9) 0.0322(3) Uani 1 1 d . . . H56 H 0.0283 0.4592 0.6164 0.039 Uiso 1 1 calc R . . C61 C -0.08195(9) 0.53734(8) 0.61677(8) 0.0255(3) Uani 1 1 d . . . C62 C -0.12108(9) 0.52363(8) 0.54733(8) 0.0271(3) Uani 1 1 d . . . H62 H -0.1072 0.5455 0.512 0.033 Uiso 1 1 calc R . . C63 C -0.18040(11) 0.47805(9) 0.52980(10) 0.0361(4) Uani 1 1 d . . . H63 H -0.2071 0.4693 0.4826 0.043 Uiso 1 1 calc R . . C64 C -0.20049(14) 0.44546(12) 0.58084(13) 0.0481(5) Uani 1 1 d . . . H64 H -0.2407 0.4142 0.5686 0.058 Uiso 1 1 calc R . . C65 C -0.16195(17) 0.45844(14) 0.65014(13) 0.0584(7) Uani 1 1 d . . . H65 H -0.1759 0.436 0.6851 0.07 Uiso 1 1 calc R . . C66 C -0.10314(14) 0.50412(11) 0.66818(11) 0.0444(5) Uani 1 1 d . . . H66 H -0.0771 0.513 0.7155 0.053 Uiso 1 1 calc R . . C1 C 0.4417(6) 0.6751(4) 0.6618(6) 0.091(3) Uani 0.5 1 d P A -1 O11 O 0.3870(3) 0.7232(2) 0.6473(3) 0.0740(12) Uani 0.5 1 d P A -1 O12 O 0.4872(3) 0.6741(3) 0.7184(4) 0.093(2) Uani 0.5 1 d P A -1 O13 O 0.4328(6) 0.6415(4) 0.6076(6) 0.197(6) Uani 0.5 1 d P A -1 O101 O 0.4205(3) 0.53115(19) 0.5381(2) 0.0676(11) Uani 0.5 1 d PDU B -1 C101 C 0.5037(11) 0.5216(6) 0.5343(7) 0.101(4) Uani 0.5 1 d PDU B -1 H10A H 0.5376 0.5022 0.5776 0.121 Uiso 0.5 1 calc PR B -1 H10B H 0.5261 0.5635 0.5267 0.121 Uiso 0.5 1 calc PR B -1 C102 C 0.4947(7) 0.4750(4) 0.4715(3) 0.0460(16) Uani 0.5 1 d PDU B -1 H10C H 0.4858 0.4309 0.4847 0.069 Uiso 0.5 1 calc PR B -1 H10D H 0.542 0.4762 0.4583 0.069 Uiso 0.5 1 calc PR B -1 H10E H 0.4507 0.4889 0.4323 0.069 Uiso 0.5 1 calc PR B -1 O1 O 0.2692(4) 0.6789(3) 0.5858(3) 0.0884(16) Uani 0.5 1 d PU C -1 O201 O 0.5644(4) 0.5751(4) 0.7901(5) 0.155(4) Uani 0.5 1 d PD D -2 C201 C 0.5277(6) 0.5044(6) 0.7434(5) 0.076(3) Uani 0.5 1 d PDU D -2 H20A H 0.5387 0.5026 0.6989 0.091 Uiso 0.5 1 calc PR D -2 H20B H 0.5474 0.4649 0.7705 0.091 Uiso 0.5 1 calc PR D -2 C202 C 0.4471(6) 0.5153(5) 0.7342(6) 0.082(3) Uani 0.5 1 d PDU D -2 H20C H 0.4397 0.5213 0.7794 0.123 Uiso 0.5 1 calc PR D -2 H20D H 0.4169 0.478 0.7108 0.123 Uiso 0.5 1 calc PR D -2 H20E H 0.4297 0.5542 0.7061 0.123 Uiso 0.5 1 calc PR D -2 O2 O 0.4719(4) 0.7610(4) 0.6904(4) 0.129(3) Uani 0.5 1 d PU E 2 O3 O 0.3221(6) 0.7265(4) 0.5867(3) 0.160(4) Uani 0.5 1 d PU F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01868(6) 0.02035(6) 0.01892(6) 0 0.00612(4) 0 P1 0.02027(15) 0.02694(17) 0.02015(15) -0.00163(12) 0.00517(12) -0.00610(12) C11 0.0250(6) 0.0289(7) 0.0219(6) -0.0024(5) 0.0059(5) -0.0082(5) C12 0.0311(8) 0.0376(9) 0.0285(7) -0.0061(6) 0.0045(6) -0.0025(6) C13 0.0437(10) 0.0392(9) 0.0339(9) -0.0083(7) 0.0090(8) 0.0011(8) C14 0.0512(11) 0.0393(10) 0.0305(8) -0.0115(7) 0.0082(8) -0.0087(8) C15 0.0415(10) 0.0450(10) 0.0305(8) -0.0099(7) 0.0002(7) -0.0124(8) C16 0.0276(7) 0.0393(9) 0.0265(7) -0.0057(6) 0.0032(6) -0.0073(6) C21 0.0235(6) 0.0350(8) 0.0225(6) 0.0000(5) 0.0038(5) -0.0115(5) C22 0.0580(12) 0.0365(9) 0.0333(9) 0.0004(7) 0.0155(8) -0.0165(9) C23 0.0628(15) 0.0419(11) 0.0496(12) 0.0107(9) 0.0242(11) -0.0121(10) C24 0.0333(9) 0.0618(13) 0.0368(9) 0.0178(9) 0.0080(7) -0.0096(9) C25 0.0465(11) 0.0735(16) 0.0230(7) 0.0029(8) 0.0028(7) -0.0263(11) C26 0.0446(10) 0.0512(11) 0.0241(7) -0.0033(7) 0.0063(7) -0.0255(9) C31 0.0232(6) 0.0373(8) 0.0219(6) -0.0027(5) 0.0058(5) -0.0032(5) C32 0.0237(7) 0.0514(11) 0.0357(9) -0.0045(8) 0.0097(6) -0.0062(7) C33 0.0230(7) 0.0716(14) 0.0399(10) -0.0114(10) 0.0090(7) -0.0001(8) C34 0.0337(9) 0.0784(17) 0.0313(9) -0.0080(10) 0.0045(7) 0.0177(10) C35 0.0486(12) 0.0608(14) 0.0339(9) 0.0077(9) 0.0116(8) 0.0212(10) C36 0.0381(9) 0.0505(11) 0.0309(8) 0.0069(8) 0.0145(7) 0.0093(8) P2 0.02303(16) 0.02112(15) 0.01991(15) -0.00293(11) 0.00856(12) -0.00073(12) C41 0.0234(6) 0.0218(6) 0.0222(6) -0.0023(4) 0.0068(5) -0.0015(4) C42 0.0251(6) 0.0280(7) 0.0294(7) -0.0022(6) 0.0058(5) 0.0016(5) C43 0.0311(8) 0.0274(7) 0.0352(8) 0.0033(6) 0.0002(6) 0.0014(6) C44 0.0369(9) 0.0330(8) 0.0297(8) 0.0076(6) 0.0029(6) -0.0056(7) C45 0.0364(8) 0.0375(9) 0.0285(7) 0.0052(6) 0.0135(6) -0.0021(7) C46 0.0282(7) 0.0302(7) 0.0250(6) 0.0018(5) 0.0108(5) 0.0012(5) C51 0.0285(6) 0.0265(6) 0.0183(5) -0.0002(5) 0.0088(5) 0.0046(5) C52 0.0283(7) 0.0383(9) 0.0317(8) -0.0081(7) 0.0075(6) 0.0048(6) C53 0.0291(8) 0.0576(12) 0.0344(9) -0.0060(8) 0.0059(7) 0.0114(8) C54 0.0428(10) 0.0542(12) 0.0328(9) 0.0043(8) 0.0082(8) 0.0265(9) C55 0.0548(12) 0.0313(8) 0.0435(10) 0.0042(7) 0.0172(9) 0.0197(8) C56 0.0417(9) 0.0238(7) 0.0317(8) 0.0015(6) 0.0123(7) 0.0069(6) C61 0.0282(7) 0.0257(6) 0.0258(6) -0.0068(5) 0.0130(5) -0.0052(5) C62 0.0260(6) 0.0291(7) 0.0265(6) -0.0047(5) 0.0086(5) -0.0034(5) C63 0.0318(8) 0.0373(9) 0.0388(9) -0.0117(7) 0.0107(7) -0.0097(7) C64 0.0475(11) 0.0509(12) 0.0528(12) -0.0150(10) 0.0257(10) -0.0261(10) C65 0.0734(17) 0.0665(16) 0.0471(12) -0.0132(11) 0.0358(12) -0.0393(13) C66 0.0600(13) 0.0499(11) 0.0305(8) -0.0103(8) 0.0244(9) -0.0256(10) C1 0.094(6) 0.066(4) 0.155(9) -0.005(5) 0.100(7) 0.002(4) O11 0.081(3) 0.058(2) 0.081(3) 0.005(2) 0.022(2) -0.007(2) O12 0.038(3) 0.093(4) 0.152(7) 0.031(3) 0.032(3) 0.010(2) O13 0.206(9) 0.147(6) 0.340(14) -0.159(8) 0.230(10) -0.103(7) O101 0.090(3) 0.049(2) 0.075(3) 0.0071(18) 0.042(2) -0.010(2) C101 0.137(9) 0.040(4) 0.109(7) 0.028(4) 0.014(7) -0.024(5) C102 0.098(5) 0.025(2) 0.0161(14) -0.0005(14) 0.019(2) -0.010(3) O1 0.100(4) 0.102(4) 0.074(3) 0.000(3) 0.042(3) -0.032(3) O201 0.083(4) 0.123(6) 0.212(9) 0.107(6) -0.020(5) -0.039(4) C201 0.081(7) 0.099(6) 0.048(4) -0.006(4) 0.021(4) 0.015(5) C202 0.075(6) 0.083(6) 0.089(7) -0.037(5) 0.028(5) 0.000(4) O2 0.125(5) 0.160(6) 0.099(5) -0.057(4) 0.029(4) 0.031(5) O3 0.197(7) 0.182(7) 0.056(3) 0.040(4) -0.024(4) -0.102(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 P1 2.6037(4) . ? Ag1 P1 2.6037(4) 2_556 ? Ag1 P2 2.6168(4) . ? Ag1 P2 2.6168(4) 2_556 ? P1 C11 1.8243(16) . ? P1 C31 1.8270(17) . ? P1 C21 1.8298(16) . ? C11 C12 1.393(3) . ? C11 C16 1.396(2) . ? C12 C13 1.388(3) . ? C12 H12 0.95 . ? C13 C14 1.392(3) . ? C13 H13 0.95 . ? C14 C15 1.377(3) . ? C14 H14 0.95 . ? C15 C16 1.397(3) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C21 C26 1.385(2) . ? C21 C22 1.393(3) . ? C22 C23 1.387(3) . ? C22 H22 0.95 . ? C23 C24 1.386(4) . ? C23 H23 0.95 . ? C24 C25 1.372(4) . ? C24 H24 0.95 . ? C25 C26 1.393(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C31 C36 1.392(3) . ? C31 C32 1.394(2) . ? C32 C33 1.393(3) . ? C32 H32 0.95 . ? C33 C34 1.382(4) . ? C33 H33 0.95 . ? C34 C35 1.385(4) . ? C34 H34 0.95 . ? C35 C36 1.395(3) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? P2 C61 1.8247(16) . ? P2 C51 1.8269(15) . ? P2 C41 1.8280(15) . ? C41 C46 1.403(2) . ? C41 C42 1.404(2) . ? C42 C43 1.390(3) . ? C42 H42 0.95 . ? C43 C44 1.395(3) . ? C43 H43 0.95 . ? C44 C45 1.388(3) . ? C44 H44 0.95 . ? C45 C46 1.398(2) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C51 C56 1.396(2) . ? C51 C52 1.403(2) . ? C52 C53 1.396(3) . ? C52 H52 0.95 . ? C53 C54 1.382(3) . ? C53 H53 0.95 . ? C54 C55 1.379(4) . ? C54 H54 0.95 . ? C55 C56 1.399(3) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C61 C62 1.400(2) . ? C61 C66 1.405(2) . ? C62 C63 1.394(2) . ? C62 H62 0.95 . ? C63 C64 1.382(3) . ? C63 H63 0.95 . ? C64 C65 1.392(4) . ? C64 H64 0.95 . ? C65 C66 1.389(3) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C1 O12 1.190(12) . ? C1 O13 1.273(12) . ? C1 O11 1.373(10) . ? O101 C101 1.552(19) . ? C101 C102 1.570(9) . ? C101 H10A 0.99 . ? C101 H10B 0.99 . ? C102 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? O201 C201 1.758(13) . ? C201 C202 1.439(10) . ? C201 H20A 0.99 . ? C201 H20B 0.99 . ? C202 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P1 108.971(19) . 2_556 ? P1 Ag1 P2 108.422(12) . . ? P1 Ag1 P2 110.157(13) 2_556 . ? P1 Ag1 P2 110.157(13) . 2_556 ? P1 Ag1 P2 108.422(12) 2_556 2_556 ? P2 Ag1 P2 110.694(18) . 2_556 ? C11 P1 C31 102.89(7) . . ? C11 P1 C21 101.60(7) . . ? C31 P1 C21 102.95(8) . . ? C11 P1 Ag1 118.08(5) . . ? C31 P1 Ag1 115.53(6) . . ? C21 P1 Ag1 113.72(5) . . ? C12 C11 C16 118.93(15) . . ? C12 C11 P1 117.77(12) . . ? C16 C11 P1 123.19(13) . . ? C13 C12 C11 120.60(17) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.0(2) . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C15 C14 C13 120.02(18) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C14 C15 C16 120.19(18) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.25(18) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C26 C21 C22 118.15(16) . . ? C26 C21 P1 118.35(13) . . ? C22 C21 P1 123.49(13) . . ? C23 C22 C21 120.7(2) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.19(18) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.6(2) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 120.9(2) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C36 C31 C32 119.09(17) . . ? C36 C31 P1 118.23(13) . . ? C32 C31 P1 122.68(14) . . ? C33 C32 C31 120.4(2) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33 120 . . ? C32 C33 H33 120 . . ? C33 C34 C35 120.13(19) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.0(2) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C31 C36 C35 120.3(2) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C61 P2 C51 102.88(7) . . ? C61 P2 C41 102.34(7) . . ? C51 P2 C41 102.28(7) . . ? C61 P2 Ag1 115.25(5) . . ? C51 P2 Ag1 117.18(5) . . ? C41 P2 Ag1 114.87(5) . . ? C46 C41 C42 119.03(14) . . ? C46 C41 P2 123.34(12) . . ? C42 C41 P2 117.61(12) . . ? C43 C42 C41 120.43(16) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 120.37(16) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C45 C44 C43 119.58(16) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.60(17) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 119.99(16) . . ? C45 C46 H46 120 . . ? C41 C46 H46 120 . . ? C56 C51 C52 119.10(15) . . ? C56 C51 P2 122.99(13) . . ? C52 C51 P2 117.88(12) . . ? C53 C52 C51 120.07(18) . . ? C53 C52 H52 120 . . ? C51 C52 H52 120 . . ? C54 C53 C52 120.3(2) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 120.07(17) . . ? C55 C54 H54 120 . . ? C53 C54 H54 120 . . ? C54 C55 C56 120.51(19) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C51 C56 C55 119.94(19) . . ? C51 C56 H56 120 . . ? C55 C56 H56 120 . . ? C62 C61 C66 118.91(15) . . ? C62 C61 P2 122.79(12) . . ? C66 C61 P2 118.28(13) . . ? C63 C62 C61 120.26(16) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.30(18) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 120.10(18) . . ? C63 C64 H64 120 . . ? C65 C64 H64 120 . . ? C66 C65 C64 120.1(2) . . ? C66 C65 H65 120 . . ? C64 C65 H65 120 . . ? C65 C66 C61 120.36(19) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? O12 C1 O13 133.8(10) . . ? O12 C1 O11 117.4(7) . . ? O13 C1 O11 108.8(11) . . ? O101 C101 C102 105.4(7) . . ? O101 C101 H10A 110.7 . . ? C102 C101 H10A 110.7 . . ? O101 C101 H10B 110.7 . . ? C102 C101 H10B 110.7 . . ? H10A C101 H10B 108.8 . . ? C202 C201 O201 97.9(9) . . ? C202 C201 H20A 112.2 . . ? O201 C201 H20A 112.2 . . ? C202 C201 H20B 112.2 . . ? O201 C201 H20B 112.2 . . ? H20A C201 H20B 109.8 . . ? C201 C202 H20C 109.5 . . ? C201 C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C201 C202 H20E 109.5 . . ? H20C C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? #===END # Attachment 'gb1054b.cif' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_gb1054b _database_code_depnum_ccdc_archive 'CCDC 795574' #TrackingRef 'gb1054b.cif' _audit_creation_date 2010-08-26T22:06:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C37 H31 Ag O3 P2' _chemical_formula_moiety 'C37 H31 Ag O3 P2' _chemical_formula_weight 693.43 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2351(3) _cell_length_b 11.9944(3) _cell_length_c 13.8661(3) _cell_angle_alpha 85.949(2) _cell_angle_beta 87.989(2) _cell_angle_gamma 65.093(3) _cell_volume 1540.05(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21890 _cell_measurement_theta_min 3.6543 _cell_measurement_theta_max 37.5961 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic_rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0539 0 0 -1 0.0231 0 -1 0 0.0446 0 1 0 0.0417 4 17 0 0.0239 1 1 -1 0.0335 -2 -2 1 0.1631 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.95 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0044730295 _diffrn_orient_matrix_ub_12 -0.0025781413 _diffrn_orient_matrix_ub_13 -0.0507193977 _diffrn_orient_matrix_ub_21 -0.0317138927 _diffrn_orient_matrix_ub_22 0.0653300732 _diffrn_orient_matrix_ub_23 -0.0052509275 _diffrn_orient_matrix_ub_31 0.0694466579 _diffrn_orient_matrix_ub_32 -0.0006809766 _diffrn_orient_matrix_ub_33 -0.0059773891 _diffrn_measurement_device_type 'Oxford Diffraction Gemini diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_number 52522 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 37.73 _diffrn_reflns_theta_full 36.75 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 15737 _reflns_number_gt 12086 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0240P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 15737 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 0.92 _refine_ls_restrained_S_all 0.92 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.631 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.280597(8) 0.430052(8) 0.293457(6) 0.01348(2) Uani 1 1 d . . . P1 P 0.02688(3) 0.56564(2) 0.270623(19) 0.01191(5) Uani 1 1 d . . . C111 C -0.06693(11) 0.65140(10) 0.37399(7) 0.01505(19) Uani 1 1 d . . . C112 C 0.01772(12) 0.66107(11) 0.44674(8) 0.0202(2) Uani 1 1 d . . . H112 H 0.1195 0.6169 0.4443 0.024 Uiso 1 1 calc R . . C113 C -0.04700(14) 0.73556(13) 0.52315(9) 0.0272(3) Uani 1 1 d . . . H113 H 0.0108 0.7439 0.5718 0.033 Uiso 1 1 calc R . . C114 C -0.19490(15) 0.79708(13) 0.52799(9) 0.0290(3) Uani 1 1 d . . . H114 H -0.2388 0.8479 0.58 0.035 Uiso 1 1 calc R . . C115 C -0.27984(13) 0.78523(13) 0.45730(9) 0.0263(3) Uani 1 1 d . . . H115 H -0.3818 0.8261 0.462 0.032 Uiso 1 1 calc R . . C116 C -0.21664(12) 0.71396(11) 0.37969(8) 0.0206(2) Uani 1 1 d . . . H116 H -0.2751 0.7077 0.3305 0.025 Uiso 1 1 calc R . . C121 C -0.00591(11) 0.68716(9) 0.17489(7) 0.01291(18) Uani 1 1 d . . . C122 C 0.10220(11) 0.72743(10) 0.15313(8) 0.01513(19) Uani 1 1 d . . . H122 H 0.1912 0.6902 0.1866 0.018 Uiso 1 1 calc R . . C123 C 0.07946(12) 0.82179(10) 0.08267(8) 0.0179(2) Uani 1 1 d . . . H123 H 0.1526 0.8498 0.0688 0.021 Uiso 1 1 calc R . . C124 C -0.04946(13) 0.87557(11) 0.03228(8) 0.0195(2) Uani 1 1 d . . . H124 H -0.0642 0.9396 -0.0163 0.023 Uiso 1 1 calc R . . C125 C -0.15723(12) 0.83503(10) 0.05330(8) 0.0175(2) Uani 1 1 d . . . H125 H -0.2453 0.8713 0.0187 0.021 Uiso 1 1 calc R . . C126 C -0.13621(11) 0.74226(10) 0.12434(8) 0.01537(19) Uani 1 1 d . . . H126 H -0.2104 0.7158 0.1389 0.018 Uiso 1 1 calc R . . C131 C -0.07750(11) 0.48736(10) 0.22979(8) 0.01521(19) Uani 1 1 d . . . C132 C -0.05312(12) 0.44990(11) 0.13510(8) 0.0187(2) Uani 1 1 d . . . H132 H 0.0101 0.4713 0.094 0.022 Uiso 1 1 calc R . . C133 C -0.12045(13) 0.38178(11) 0.10055(10) 0.0254(3) Uani 1 1 d . . . H133 H -0.1048 0.3581 0.0357 0.03 Uiso 1 1 calc R . . C134 C -0.21004(14) 0.34844(12) 0.16052(11) 0.0298(3) Uani 1 1 d . . . H134 H -0.2546 0.3003 0.1373 0.036 Uiso 1 1 calc R . . C135 C -0.23520(15) 0.38462(13) 0.25387(11) 0.0310(3) Uani 1 1 d . . . H135 H -0.2978 0.3619 0.2946 0.037 Uiso 1 1 calc R . . C136 C -0.16942(13) 0.45450(12) 0.28941(9) 0.0228(2) Uani 1 1 d . . . H136 H -0.1874 0.4794 0.3539 0.027 Uiso 1 1 calc R . . P2 P 0.43545(3) 0.23018(2) 0.233970(19) 0.01112(5) Uani 1 1 d . . . C211 C 0.46753(11) 0.24269(10) 0.10428(7) 0.01237(17) Uani 1 1 d . . . C212 C 0.43993(12) 0.35845(10) 0.06053(8) 0.0178(2) Uani 1 1 d . . . H212 H 0.4039 0.4284 0.0983 0.021 Uiso 1 1 calc R . . C213 C 0.46463(13) 0.37262(11) -0.03801(8) 0.0203(2) Uani 1 1 d . . . H213 H 0.4453 0.4521 -0.0671 0.024 Uiso 1 1 calc R . . C214 C 0.51743(12) 0.27096(11) -0.09382(8) 0.0186(2) Uani 1 1 d . . . H214 H 0.5355 0.2805 -0.1609 0.022 Uiso 1 1 calc R . . C215 C 0.54370(12) 0.15532(11) -0.05113(8) 0.0168(2) Uani 1 1 d . . . H215 H 0.5792 0.0857 -0.0893 0.02 Uiso 1 1 calc R . . C216 C 0.51846(11) 0.14061(10) 0.04712(7) 0.01432(18) Uani 1 1 d . . . H216 H 0.5357 0.0613 0.0756 0.017 Uiso 1 1 calc R . . C221 C 0.61187(11) 0.15379(10) 0.29040(7) 0.01260(17) Uani 1 1 d . . . C222 C 0.62459(12) 0.18158(11) 0.38467(8) 0.0165(2) Uani 1 1 d . . . H222 H 0.5445 0.2428 0.4152 0.02 Uiso 1 1 calc R . . C223 C 0.75334(13) 0.12036(12) 0.43416(8) 0.0224(2) Uani 1 1 d . . . H223 H 0.7614 0.1397 0.4983 0.027 Uiso 1 1 calc R . . C224 C 0.87088(12) 0.03037(12) 0.38946(9) 0.0235(2) Uani 1 1 d . . . H224 H 0.9592 -0.0117 0.4232 0.028 Uiso 1 1 calc R . . C225 C 0.85910(11) 0.00241(11) 0.29627(9) 0.0197(2) Uani 1 1 d . . . H225 H 0.9392 -0.0593 0.2662 0.024 Uiso 1 1 calc R . . C226 C 0.73083(11) 0.06401(10) 0.24631(8) 0.0163(2) Uani 1 1 d . . . H226 H 0.7238 0.0451 0.1818 0.02 Uiso 1 1 calc R . . C231 C 0.36636(10) 0.11196(9) 0.24625(7) 0.01135(17) Uani 1 1 d . . . C232 C 0.22455(11) 0.14537(10) 0.21659(8) 0.01516(19) Uani 1 1 d . . . H232 H 0.1704 0.2254 0.1876 0.018 Uiso 1 1 calc R . . C233 C 0.16305(12) 0.06218(11) 0.22930(8) 0.0179(2) Uani 1 1 d . . . H233 H 0.0671 0.0852 0.2086 0.021 Uiso 1 1 calc R . . C234 C 0.24130(12) -0.05493(11) 0.27224(8) 0.0171(2) Uani 1 1 d . . . H234 H 0.1986 -0.1116 0.2813 0.021 Uiso 1 1 calc R . . C235 C 0.38203(12) -0.08889(10) 0.30181(8) 0.01565(19) Uani 1 1 d . . . H235 H 0.4356 -0.1688 0.3311 0.019 Uiso 1 1 calc R . . C236 C 0.44439(11) -0.00568(10) 0.28852(7) 0.01391(18) Uani 1 1 d . . . H236 H 0.5408 -0.0293 0.3084 0.017 Uiso 1 1 calc R . . C1 C 0.42920(11) 0.55884(11) 0.36689(8) 0.0163(2) Uani 1 1 d . . . O1 O 0.40223(9) 0.47896(7) 0.41872(6) 0.01677(15) Uani 1 1 d . . . O2 O 0.39096(10) 0.58970(9) 0.28149(6) 0.02648(19) Uani 1 1 d . . . O3 O 0.50356(10) 0.61329(8) 0.40695(7) 0.02301(18) Uani 1 1 d . . . H3 H 0.5292(18) 0.5771(16) 0.4655(13) 0.043(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01149(3) 0.01122(3) 0.01591(4) -0.00273(2) -0.00104(2) -0.00264(3) P1 0.01082(11) 0.01100(12) 0.01250(11) -0.00085(9) -0.00066(9) -0.00315(9) C111 0.0153(4) 0.0140(5) 0.0128(4) 0.0004(4) 0.0010(4) -0.0034(4) C112 0.0177(5) 0.0221(6) 0.0164(5) -0.0040(4) -0.0012(4) -0.0035(4) C113 0.0312(6) 0.0283(7) 0.0152(5) -0.0061(5) -0.0028(5) -0.0049(5) C114 0.0324(7) 0.0286(7) 0.0141(5) -0.0042(5) 0.0059(5) -0.0012(5) C115 0.0189(5) 0.0286(7) 0.0204(6) -0.0010(5) 0.0066(4) 0.0000(5) C116 0.0163(5) 0.0237(6) 0.0165(5) -0.0008(4) 0.0012(4) -0.0033(4) C121 0.0137(4) 0.0110(4) 0.0122(4) -0.0013(3) -0.0010(3) -0.0033(4) C122 0.0155(4) 0.0138(5) 0.0161(5) -0.0010(4) -0.0035(4) -0.0060(4) C123 0.0209(5) 0.0159(5) 0.0202(5) 0.0007(4) -0.0029(4) -0.0110(4) C124 0.0256(5) 0.0136(5) 0.0193(5) 0.0027(4) -0.0056(4) -0.0083(4) C125 0.0165(5) 0.0137(5) 0.0195(5) 0.0005(4) -0.0046(4) -0.0033(4) C126 0.0128(4) 0.0139(5) 0.0176(5) -0.0006(4) -0.0005(4) -0.0040(4) C131 0.0128(4) 0.0117(5) 0.0201(5) 0.0018(4) -0.0041(4) -0.0042(4) C132 0.0174(5) 0.0155(5) 0.0220(5) -0.0028(4) -0.0035(4) -0.0052(4) C133 0.0256(6) 0.0164(5) 0.0329(7) -0.0035(5) -0.0121(5) -0.0063(5) C134 0.0269(6) 0.0169(6) 0.0485(8) 0.0033(5) -0.0169(6) -0.0116(5) C135 0.0274(6) 0.0265(7) 0.0456(8) 0.0090(6) -0.0055(6) -0.0190(6) C136 0.0227(5) 0.0208(6) 0.0265(6) 0.0053(5) -0.0019(5) -0.0117(5) P2 0.01036(11) 0.00979(11) 0.01247(11) -0.00109(9) -0.00001(9) -0.00345(9) C211 0.0114(4) 0.0125(4) 0.0134(4) 0.0008(3) -0.0005(3) -0.0054(4) C212 0.0188(5) 0.0131(5) 0.0198(5) 0.0009(4) 0.0010(4) -0.0053(4) C213 0.0222(5) 0.0160(5) 0.0213(5) 0.0058(4) 0.0004(4) -0.0079(4) C214 0.0192(5) 0.0233(6) 0.0143(5) 0.0029(4) -0.0001(4) -0.0108(4) C215 0.0198(5) 0.0193(5) 0.0139(5) -0.0024(4) 0.0018(4) -0.0106(4) C216 0.0159(4) 0.0129(5) 0.0150(4) -0.0002(4) 0.0002(4) -0.0071(4) C221 0.0116(4) 0.0119(4) 0.0147(4) -0.0002(3) -0.0003(3) -0.0054(4) C222 0.0159(5) 0.0178(5) 0.0141(5) -0.0016(4) 0.0008(4) -0.0055(4) C223 0.0210(5) 0.0281(6) 0.0156(5) -0.0008(4) -0.0046(4) -0.0077(5) C224 0.0147(5) 0.0274(6) 0.0246(6) 0.0024(5) -0.0059(4) -0.0052(5) C225 0.0110(4) 0.0195(5) 0.0264(6) -0.0036(4) -0.0002(4) -0.0040(4) C226 0.0129(4) 0.0173(5) 0.0185(5) -0.0044(4) 0.0005(4) -0.0057(4) C231 0.0116(4) 0.0127(4) 0.0098(4) -0.0018(3) 0.0013(3) -0.0051(3) C232 0.0137(4) 0.0154(5) 0.0156(5) 0.0020(4) -0.0028(4) -0.0056(4) C233 0.0141(5) 0.0219(6) 0.0200(5) 0.0009(4) -0.0028(4) -0.0099(4) C234 0.0192(5) 0.0197(5) 0.0164(5) -0.0005(4) 0.0008(4) -0.0123(4) C235 0.0177(5) 0.0137(5) 0.0153(5) 0.0009(4) 0.0004(4) -0.0067(4) C236 0.0120(4) 0.0132(5) 0.0152(4) -0.0004(4) 0.0002(3) -0.0041(4) C1 0.0150(4) 0.0172(5) 0.0169(5) 0.0003(4) -0.0029(4) -0.0069(4) O1 0.0214(4) 0.0159(4) 0.0160(4) 0.0013(3) -0.0043(3) -0.0108(3) O2 0.0282(4) 0.0381(6) 0.0183(4) 0.0100(4) -0.0100(3) -0.0200(4) O3 0.0305(5) 0.0243(5) 0.0220(4) 0.0080(3) -0.0108(4) -0.0197(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.4128(7) . ? Ag1 P1 2.4323(3) . ? Ag1 P2 2.4345(3) . ? Ag1 O2 2.5951(9) . ? P1 C131 1.8182(11) . ? P1 C111 1.8205(10) . ? P1 C121 1.8289(11) . ? C111 C112 1.3944(15) . ? C111 C116 1.3959(15) . ? C112 C113 1.3949(16) . ? C112 H112 0.95 . ? C113 C114 1.3782(18) . ? C113 H113 0.95 . ? C114 C115 1.3858(19) . ? C114 H114 0.95 . ? C115 C116 1.3867(16) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.3982(15) . ? C121 C126 1.4017(15) . ? C122 C123 1.3883(16) . ? C122 H122 0.95 . ? C123 C124 1.3891(16) . ? C123 H123 0.95 . ? C124 C125 1.3955(16) . ? C124 H124 0.95 . ? C125 C126 1.3832(16) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.3913(16) . ? C131 C132 1.3978(15) . ? C132 C133 1.3874(16) . ? C132 H132 0.95 . ? C133 C134 1.379(2) . ? C133 H133 0.95 . ? C134 C135 1.375(2) . ? C134 H134 0.95 . ? C135 C136 1.3984(18) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C221 1.8212(10) . ? P2 C211 1.8238(10) . ? P2 C231 1.8280(10) . ? C211 C212 1.3922(15) . ? C211 C216 1.4035(14) . ? C212 C213 1.3923(16) . ? C212 H212 0.95 . ? C213 C214 1.3881(16) . ? C213 H213 0.95 . ? C214 C215 1.3884(16) . ? C214 H214 0.95 . ? C215 C216 1.3905(15) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.3952(14) . ? C221 C226 1.3973(14) . ? C222 C223 1.3871(16) . ? C222 H222 0.95 . ? C223 C224 1.3946(17) . ? C223 H223 0.95 . ? C224 C225 1.3796(17) . ? C224 H224 0.95 . ? C225 C226 1.3870(15) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C236 1.3926(15) . ? C231 C232 1.4018(14) . ? C232 C233 1.3854(15) . ? C232 H232 0.95 . ? C233 C234 1.3917(16) . ? C233 H233 0.95 . ? C234 C235 1.3901(16) . ? C234 H234 0.95 . ? C235 C236 1.3927(15) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C1 O2 1.2414(13) . ? C1 O1 1.2737(14) . ? C1 O3 1.3468(13) . ? O3 H3 0.886(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 P1 116.33(2) . . ? O1 Ag1 P2 109.90(2) . . ? P1 Ag1 P2 132.882(9) . . ? O1 Ag1 O2 52.47(3) . . ? P1 Ag1 O2 100.47(2) . . ? P2 Ag1 O2 114.81(2) . . ? C131 P1 C111 107.69(5) . . ? C131 P1 C121 102.07(5) . . ? C111 P1 C121 102.78(5) . . ? C131 P1 Ag1 113.19(4) . . ? C111 P1 Ag1 116.15(4) . . ? C121 P1 Ag1 113.56(3) . . ? C112 C111 C116 119.54(10) . . ? C112 C111 P1 117.10(8) . . ? C116 C111 P1 123.19(8) . . ? C111 C112 C113 120.03(11) . . ? C111 C112 H112 120 . . ? C113 C112 H112 120 . . ? C114 C113 C112 119.94(12) . . ? C114 C113 H113 120 . . ? C112 C113 H113 120 . . ? C113 C114 C115 120.31(11) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C114 C115 C116 120.28(11) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C111 119.86(11) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C122 C121 C126 119.31(10) . . ? C122 C121 P1 118.49(8) . . ? C126 C121 P1 122.19(8) . . ? C123 C122 C121 120.02(10) . . ? C123 C122 H122 120 . . ? C121 C122 H122 120 . . ? C122 C123 C124 120.48(10) . . ? C122 C123 H123 119.8 . . ? C124 C123 H123 119.8 . . ? C123 C124 C125 119.67(11) . . ? C123 C124 H124 120.2 . . ? C125 C124 H124 120.2 . . ? C126 C125 C124 120.21(10) . . ? C126 C125 H125 119.9 . . ? C124 C125 H125 119.9 . . ? C125 C126 C121 120.30(10) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C136 C131 C132 119.09(10) . . ? C136 C131 P1 123.74(9) . . ? C132 C131 P1 116.94(8) . . ? C133 C132 C131 120.60(12) . . ? C133 C132 H132 119.7 . . ? C131 C132 H132 119.7 . . ? C134 C133 C132 119.88(12) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C135 C134 C133 120.22(12) . . ? C135 C134 H134 119.9 . . ? C133 C134 H134 119.9 . . ? C134 C135 C136 120.57(13) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C131 C136 C135 119.63(12) . . ? C131 C136 H136 120.2 . . ? C135 C136 H136 120.2 . . ? C221 P2 C211 106.52(5) . . ? C221 P2 C231 102.98(5) . . ? C211 P2 C231 103.24(4) . . ? C221 P2 Ag1 115.24(3) . . ? C211 P2 Ag1 111.11(3) . . ? C231 P2 Ag1 116.55(3) . . ? C212 C211 C216 118.91(10) . . ? C212 C211 P2 118.43(8) . . ? C216 C211 P2 122.66(8) . . ? C211 C212 C213 120.64(10) . . ? C211 C212 H212 119.7 . . ? C213 C212 H212 119.7 . . ? C214 C213 C212 120.17(11) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C215 119.65(10) . . ? C213 C214 H214 120.2 . . ? C215 C214 H214 120.2 . . ? C214 C215 C216 120.49(10) . . ? C214 C215 H215 119.8 . . ? C216 C215 H215 119.8 . . ? C215 C216 C211 120.13(10) . . ? C215 C216 H216 119.9 . . ? C211 C216 H216 119.9 . . ? C222 C221 C226 119.12(10) . . ? C222 C221 P2 117.57(8) . . ? C226 C221 P2 123.19(8) . . ? C223 C222 C221 120.44(10) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C222 C223 C224 119.81(11) . . ? C222 C223 H223 120.1 . . ? C224 C223 H223 120.1 . . ? C225 C224 C223 120.07(11) . . ? C225 C224 H224 120 . . ? C223 C224 H224 120 . . ? C224 C225 C226 120.29(10) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C225 C226 C221 120.27(10) . . ? C225 C226 H226 119.9 . . ? C221 C226 H226 119.9 . . ? C236 C231 C232 119.20(9) . . ? C236 C231 P2 123.20(8) . . ? C232 C231 P2 117.49(8) . . ? C233 C232 C231 120.27(10) . . ? C233 C232 H232 119.9 . . ? C231 C232 H232 119.9 . . ? C232 C233 C234 120.22(10) . . ? C232 C233 H233 119.9 . . ? C234 C233 H233 119.9 . . ? C235 C234 C233 119.89(10) . . ? C235 C234 H234 120.1 . . ? C233 C234 H234 120.1 . . ? C234 C235 C236 119.98(10) . . ? C234 C235 H235 120 . . ? C236 C235 H235 120 . . ? C231 C236 C235 120.43(10) . . ? C231 C236 H236 119.8 . . ? C235 C236 H236 119.8 . . ? O2 C1 O1 123.92(10) . . ? O2 C1 O3 117.90(11) . . ? O1 C1 O3 118.19(10) . . ? C1 O1 Ag1 95.62(6) . . ? C1 O2 Ag1 87.96(7) . . ? C1 O3 H3 106.9(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 0.886(18) 1.747(18) 2.6238(12) 169.8(17) 2_666 #===END