Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'K.Molloy' 'D.Edwards' 'M.Mahon' 'Virginie Ogrodnik' _publ_contact_author_name 'Dr K Molloy' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email 'CHSKCM@BATH.AC.UK' _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Aerosol-assisted Chemical Vapour Deposition (AACVD) of Silver Films from Functionalised Silver Carboxylates and Some Representative Adducts ; data_96dae7 _database_code_CSD 195316 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H37 Ag O2 P2' _chemical_formula_weight 731.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.616(2) _cell_length_b 18.141(3) _cell_length_c 18.628(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.23(2) _cell_angle_gamma 90.00 _cell_volume 3492.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method ? _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5789 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 23.92 _reflns_number_total 5462 _reflns_number_observed 4305 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+2.2795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5459 _refine_ls_number_parameters 421 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_obs 0.0245 _refine_ls_wR_factor_all 0.0646 _refine_ls_wR_factor_obs 0.0548 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.020 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.020 _refine_ls_shift/esd_max -0.228 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.13803(2) 0.198173(10) 0.120959(11) 0.03750(8) Uani 1 d . . P1 P 0.07486(6) 0.32027(3) 0.07571(4) 0.0305(2) Uani 1 d . . P2 P 0.35211(6) 0.14523(4) 0.17381(4) 0.0314(2) Uani 1 d . . O1 O -0.0153(2) 0.10467(10) 0.06135(10) 0.0439(5) Uani 1 d . . O2 O 0.0010(2) 0.12331(11) 0.18002(10) 0.0516(5) Uani 1 d . . C1 C -0.0432(2) 0.36972(14) 0.11467(14) 0.0341(6) Uani 1 d . . C2 C -0.1387(3) 0.41428(15) 0.0729(2) 0.0422(7) Uani 1 d . . H2 H -0.1516(3) 0.41497(15) 0.0218(2) 0.051 Uiso 1 calc R . C3 C -0.2151(3) 0.4578(2) 0.1073(2) 0.0574(8) Uani 1 d . . H3 H -0.2793(3) 0.4874(2) 0.0791(2) 0.069 Uiso 1 calc R . C4 C -0.1963(3) 0.4574(2) 0.1825(2) 0.0660(10) Uani 1 d . . H4 H -0.2464(3) 0.4874(2) 0.2055(2) 0.079 Uiso 1 calc R . C5 C -0.1035(3) 0.4126(2) 0.2239(2) 0.0650(10) Uani 1 d . . H5 H -0.0913(3) 0.4120(2) 0.2750(2) 0.078 Uiso 1 calc R . C6 C -0.0283(3) 0.3684(2) 0.1905(2) 0.0496(7) Uani 1 d . . H6 H 0.0331(3) 0.3374(2) 0.2191(2) 0.060 Uiso 1 calc R . C7 C 0.2055(2) 0.38794(13) 0.08597(13) 0.0320(6) Uani 1 d . . C8 C 0.1929(3) 0.46060(14) 0.10568(15) 0.0402(6) Uani 1 d . . H8 H 0.1164(3) 0.47647(14) 0.11691(15) 0.048 Uiso 1 calc R . C9 C 0.2938(3) 0.5099(2) 0.1088(2) 0.0477(7) Uani 1 d . . H9 H 0.2843(3) 0.5586(2) 0.1221(2) 0.057 Uiso 1 calc R . C10 C 0.4072(3) 0.4876(2) 0.0925(2) 0.0534(8) Uani 1 d . . H10 H 0.4741(3) 0.5210(2) 0.0940(2) 0.064 Uiso 1 calc R . C11 C 0.4214(3) 0.4150(2) 0.0737(2) 0.0585(8) Uani 1 d . . H11 H 0.4983(3) 0.3995(2) 0.0627(2) 0.070 Uiso 1 calc R . C12 C 0.3218(3) 0.3654(2) 0.0711(2) 0.0471(7) Uani 1 d . . H12 H 0.3329(3) 0.3164(2) 0.0593(2) 0.057 Uiso 1 calc R . C13 C 0.3978(2) 0.16835(14) 0.27165(14) 0.0350(6) Uani 1 d . . C14 C 0.2986(3) 0.1818(2) 0.3067(2) 0.0546(8) Uani 1 d . . H14 H 0.2132(3) 0.1773(2) 0.2805(2) 0.066 Uiso 1 calc R . C15 C 0.3249(4) 0.2020(2) 0.3802(2) 0.0707(10) Uani 1 d . . H15 H 0.2573(4) 0.2107(2) 0.4032(2) 0.085 Uiso 1 calc R . C16 C 0.4502(4) 0.2091(2) 0.4193(2) 0.0641(9) Uani 1 d . . H16 H 0.4675(4) 0.2236(2) 0.4685(2) 0.077 Uiso 1 calc R . C17 C 0.5504(3) 0.1950(2) 0.3859(2) 0.0506(7) Uani 1 d . . H17 H 0.6354(3) 0.1991(2) 0.4128(2) 0.061 Uiso 1 calc R . C18 C 0.5253(3) 0.17473(15) 0.3128(2) 0.0426(7) Uani 1 d . . H18 H 0.5937(3) 0.16521(15) 0.2906(2) 0.051 Uiso 1 calc R . C19 C 0.4911(2) 0.17305(14) 0.13768(14) 0.0361(6) Uani 1 d . . C20 C 0.5527(3) 0.2400(2) 0.1573(2) 0.0492(7) Uani 1 d . . H20 H 0.5234(3) 0.2711(2) 0.1897(2) 0.059 Uiso 1 calc R . C21 C 0.6571(3) 0.2610(2) 0.1293(2) 0.0642(9) Uani 1 d . . H21 H 0.6982(3) 0.3057(2) 0.1435(2) 0.077 Uiso 1 calc R . C22 C 0.6998(3) 0.2167(2) 0.0812(2) 0.0672(10) Uani 1 d . . H22 H 0.7710(3) 0.2308(2) 0.0633(2) 0.081 Uiso 1 calc R . C23 C 0.6391(3) 0.1516(2) 0.0591(2) 0.0656(10) Uani 1 d . . H23 H 0.6674(3) 0.1220(2) 0.0252(2) 0.079 Uiso 1 calc R . C24 C 0.5344(3) 0.1294(2) 0.0875(2) 0.0493(7) Uani 1 d . . H24 H 0.4934(3) 0.0849(2) 0.0725(2) 0.059 Uiso 1 calc R . C25 C 0.3591(2) 0.04475(13) 0.16990(14) 0.0328(6) Uani 1 d . . C26 C 0.4615(3) 0.0049(2) 0.2115(2) 0.0451(7) Uani 1 d . . H26 H 0.5270(3) 0.0291(2) 0.2449(2) 0.054 Uiso 1 calc R . C27 C 0.4665(3) -0.0706(2) 0.2034(2) 0.0608(9) Uani 1 d . . H27 H 0.5349(3) -0.0973(2) 0.2317(2) 0.073 Uiso 1 calc R . C28 C 0.3700(3) -0.1065(2) 0.1533(2) 0.0632(9) Uani 1 d . . H28 H 0.3742(3) -0.1573(2) 0.1475(2) 0.076 Uiso 1 calc R . C29 C 0.2679(3) -0.0675(2) 0.1122(2) 0.0543(8) Uani 1 d . . H29 H 0.2028(3) -0.0919(2) 0.0788(2) 0.065 Uiso 1 calc R . C30 C 0.2620(3) 0.00818(15) 0.12052(15) 0.0397(6) Uani 1 d . . H30 H 0.1925(3) 0.03452(15) 0.09279(15) 0.048 Uiso 1 calc R . C31 C 0.0102(2) 0.31846(13) -0.02388(13) 0.0307(6) Uani 1 d . . C32 C 0.0296(3) 0.37528(15) -0.07009(14) 0.0398(6) Uani 1 d . . H32 H 0.0721(3) 0.41790(15) -0.04996(14) 0.048 Uiso 1 calc R . C33 C -0.0136(3) 0.3692(2) -0.1457(2) 0.0458(7) Uani 1 d . . H33 H 0.0009(3) 0.4074(2) -0.1761(2) 0.055 Uiso 1 calc R . C34 C -0.0775(3) 0.3073(2) -0.1759(2) 0.0502(7) Uani 1 d . . H34 H -0.1068(3) 0.3033(2) -0.2268(2) 0.060 Uiso 1 calc R . C35 C -0.0984(3) 0.2510(2) -0.1310(2) 0.0572(8) Uani 1 d . . H35 H -0.1435(3) 0.2093(2) -0.1516(2) 0.069 Uiso 1 calc R . C36 C -0.0533(3) 0.2554(2) -0.05509(15) 0.0445(7) Uani 1 d . . H36 H -0.0656(3) 0.2162(2) -0.02525(15) 0.053 Uiso 1 calc R . C37 C -0.0416(2) 0.08784(14) 0.12181(14) 0.0355(6) Uani 1 d . . C38 C -0.1244(2) 0.0213(2) 0.12591(15) 0.0391(6) Uani 1 d . . C39 C -0.1299(3) -0.0319(2) 0.0771(2) 0.0527(8) Uani 1 d D . H39 H -0.0804(27) -0.0253(17) 0.0382(15) 0.063 Uiso 1 d D . C40 C -0.1913(3) 0.0189(2) 0.1889(2) 0.0588(8) Uani 1 d . . H40A H -0.2267(19) 0.0666(4) 0.1950(8) 0.088 Uiso 1 calc R . H40B H -0.1302(6) 0.0054(12) 0.2334(3) 0.088 Uiso 1 calc R . H40C H -0.2598(14) -0.0168(9) 0.1785(6) 0.088 Uiso 1 calc R . C41 C -0.2012(4) -0.1040(2) 0.0749(2) 0.0836(12) Uani 1 d . . H41A H -0.2048(24) -0.1280(8) 0.0285(7) 0.125 Uiso 1 calc R . H41B H -0.2875(10) -0.0949(2) 0.0806(16) 0.125 Uiso 1 calc R . H41C H -0.1566(16) -0.1351(6) 0.1143(10) 0.125 Uiso 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 0.03704(12) 0.03092(12) 0.04346(13) 0.00557(9) 0.00698(8) 0.00059(9) P1 0.0317(3) 0.0269(3) 0.0329(3) 0.0018(3) 0.0073(3) 0.0004(3) P2 0.0309(3) 0.0277(3) 0.0362(4) 0.0023(3) 0.0089(3) 0.0001(3) O1 0.0501(11) 0.0466(11) 0.0367(11) 0.0020(9) 0.0136(9) -0.0095(9) O2 0.0584(13) 0.0595(13) 0.0405(11) -0.0120(10) 0.0187(10) -0.0206(10) C1 0.0352(14) 0.0301(13) 0.0394(15) -0.0020(11) 0.0137(12) -0.0070(11) C2 0.040(2) 0.041(2) 0.049(2) 0.0056(13) 0.0166(13) 0.0038(13) C3 0.047(2) 0.046(2) 0.086(3) 0.004(2) 0.030(2) 0.0078(15) C4 0.064(2) 0.057(2) 0.092(3) -0.021(2) 0.049(2) -0.005(2) C5 0.069(2) 0.082(3) 0.053(2) -0.021(2) 0.033(2) -0.016(2) C6 0.049(2) 0.061(2) 0.041(2) -0.0017(15) 0.0149(14) -0.0019(15) C7 0.0299(13) 0.0323(14) 0.0320(13) 0.0001(11) 0.0033(11) 0.0000(11) C8 0.0365(14) 0.037(2) 0.047(2) -0.0038(12) 0.0096(12) 0.0001(12) C9 0.048(2) 0.034(2) 0.058(2) -0.0064(13) 0.0047(14) -0.0059(13) C10 0.041(2) 0.050(2) 0.067(2) -0.003(2) 0.0078(15) -0.0161(14) C11 0.037(2) 0.059(2) 0.084(2) -0.009(2) 0.021(2) -0.0051(15) C12 0.042(2) 0.038(2) 0.064(2) -0.0074(14) 0.0170(14) -0.0011(13) C13 0.0399(15) 0.0286(13) 0.0374(14) 0.0016(11) 0.0107(12) -0.0014(11) C14 0.048(2) 0.070(2) 0.048(2) -0.008(2) 0.0161(14) -0.012(2) C15 0.067(2) 0.100(3) 0.052(2) -0.019(2) 0.028(2) -0.017(2) C16 0.082(2) 0.072(2) 0.040(2) -0.012(2) 0.016(2) -0.025(2) C17 0.055(2) 0.045(2) 0.046(2) 0.0032(14) -0.0012(14) -0.0109(15) C18 0.041(2) 0.0381(15) 0.047(2) 0.0018(13) 0.0068(13) 0.0021(12) C19 0.0309(13) 0.0361(14) 0.0410(15) 0.0104(12) 0.0078(12) 0.0035(11) C20 0.050(2) 0.042(2) 0.057(2) 0.0053(14) 0.0156(15) -0.0074(14) C21 0.048(2) 0.067(2) 0.078(2) 0.017(2) 0.014(2) -0.017(2) C22 0.046(2) 0.079(3) 0.082(3) 0.034(2) 0.028(2) 0.002(2) C23 0.069(2) 0.073(2) 0.067(2) 0.017(2) 0.039(2) 0.019(2) C24 0.053(2) 0.048(2) 0.052(2) 0.0083(14) 0.0234(15) 0.0033(15) C25 0.0354(14) 0.0299(13) 0.0359(14) 0.0036(11) 0.0139(11) 0.0002(11) C26 0.043(2) 0.037(2) 0.053(2) 0.0046(13) 0.0076(14) 0.0021(13) C27 0.062(2) 0.041(2) 0.081(2) 0.018(2) 0.020(2) 0.015(2) C28 0.079(2) 0.030(2) 0.089(3) -0.007(2) 0.035(2) -0.002(2) C29 0.060(2) 0.041(2) 0.065(2) -0.015(2) 0.021(2) -0.010(2) C30 0.041(2) 0.037(2) 0.043(2) -0.0030(12) 0.0126(13) -0.0012(12) C31 0.0302(13) 0.0298(13) 0.0331(13) 0.0006(10) 0.0094(10) 0.0031(10) C32 0.045(2) 0.0324(14) 0.041(2) 0.0028(12) 0.0082(13) -0.0014(12) C33 0.051(2) 0.046(2) 0.040(2) 0.0101(13) 0.0117(13) 0.0026(14) C34 0.055(2) 0.061(2) 0.0338(15) -0.0025(14) 0.0076(13) -0.005(2) C35 0.070(2) 0.054(2) 0.046(2) -0.013(2) 0.011(2) -0.023(2) C36 0.053(2) 0.042(2) 0.040(2) -0.0008(13) 0.0137(13) -0.0140(14) C37 0.0294(13) 0.0388(15) 0.039(2) 0.0011(12) 0.0100(11) 0.0025(11) C38 0.0338(14) 0.045(2) 0.0374(14) 0.0032(13) 0.0059(12) -0.0043(12) C39 0.058(2) 0.051(2) 0.048(2) -0.003(2) 0.0088(15) -0.014(2) C40 0.056(2) 0.067(2) 0.059(2) 0.003(2) 0.024(2) -0.012(2) C41 0.104(3) 0.057(2) 0.089(3) -0.013(2) 0.021(2) -0.031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4099(7) . ? Ag1 O2 2.430(2) . ? Ag1 O1 2.436(2) . ? Ag1 P2 2.4562(8) . ? P1 C1 1.822(3) . ? P1 C31 1.825(2) . ? P1 C7 1.829(3) . ? P2 C13 1.824(3) . ? P2 C25 1.826(3) . ? P2 C19 1.827(3) . ? O1 C37 1.259(3) . ? O2 C37 1.253(3) . ? C1 C6 1.385(4) . ? C1 C2 1.388(4) . ? C2 C3 1.389(4) . ? C3 C4 1.370(5) . ? C4 C5 1.371(5) . ? C5 C6 1.377(4) . ? C7 C8 1.383(4) . ? C7 C12 1.387(4) . ? C8 C9 1.386(4) . ? C9 C10 1.369(4) . ? C10 C11 1.378(4) . ? C11 C12 1.381(4) . ? C13 C14 1.382(4) . ? C13 C18 1.400(4) . ? C14 C15 1.383(4) . ? C15 C16 1.368(5) . ? C16 C17 1.373(5) . ? C17 C18 1.376(4) . ? C19 C24 1.381(4) . ? C19 C20 1.388(4) . ? C20 C21 1.381(4) . ? C21 C22 1.357(5) . ? C22 C23 1.363(5) . ? C23 C24 1.395(4) . ? C25 C30 1.383(4) . ? C25 C26 1.385(4) . ? C26 C27 1.380(4) . ? C27 C28 1.380(5) . ? C28 C29 1.371(5) . ? C29 C30 1.385(4) . ? C31 C36 1.385(4) . ? C31 C32 1.388(3) . ? C32 C33 1.382(4) . ? C33 C34 1.365(4) . ? C34 C35 1.370(4) . ? C35 C36 1.387(4) . ? C37 C38 1.505(4) . ? C38 C39 1.318(4) . ? C38 C40 1.504(4) . ? C39 C41 1.508(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 O2 121.64(5) . . ? P1 Ag1 O1 112.16(5) . . ? O2 Ag1 O1 53.86(6) . . ? P1 Ag1 P2 131.11(2) . . ? O2 Ag1 P2 101.24(5) . . ? O1 Ag1 P2 111.77(5) . . ? C1 P1 C31 106.30(11) . . ? C1 P1 C7 101.67(11) . . ? C31 P1 C7 102.61(11) . . ? C1 P1 Ag1 118.36(8) . . ? C31 P1 Ag1 110.42(8) . . ? C7 P1 Ag1 115.88(8) . . ? C13 P2 C25 105.39(12) . . ? C13 P2 C19 104.59(12) . . ? C25 P2 C19 102.57(12) . . ? C13 P2 Ag1 108.70(9) . . ? C25 P2 Ag1 114.61(9) . . ? C19 P2 Ag1 119.70(8) . . ? C37 O1 Ag1 91.3(2) . . ? C37 O2 Ag1 91.7(2) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 P1 118.0(2) . . ? C2 C1 P1 123.0(2) . . ? C1 C2 C3 120.1(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 119.7(3) . . ? C4 C5 C6 120.5(3) . . ? C5 C6 C1 120.5(3) . . ? C8 C7 C12 118.6(2) . . ? C8 C7 P1 123.4(2) . . ? C12 C7 P1 118.0(2) . . ? C7 C8 C9 120.4(3) . . ? C10 C9 C8 120.7(3) . . ? C9 C10 C11 119.4(3) . . ? C10 C11 C12 120.3(3) . . ? C11 C12 C7 120.6(3) . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P2 117.1(2) . . ? C18 C13 P2 124.7(2) . . ? C13 C14 C15 120.8(3) . . ? C16 C15 C14 120.2(3) . . ? C15 C16 C17 120.0(3) . . ? C16 C17 C18 120.3(3) . . ? C17 C18 C13 120.5(3) . . ? C24 C19 C20 118.0(3) . . ? C24 C19 P2 120.8(2) . . ? C20 C19 P2 121.1(2) . . ? C21 C20 C19 120.9(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C23 120.5(3) . . ? C22 C23 C24 119.9(3) . . ? C19 C24 C23 120.6(3) . . ? C30 C25 C26 119.4(2) . . ? C30 C25 P2 118.3(2) . . ? C26 C25 P2 122.1(2) . . ? C27 C26 C25 120.1(3) . . ? C28 C27 C26 120.1(3) . . ? C29 C28 C27 120.3(3) . . ? C28 C29 C30 119.9(3) . . ? C25 C30 C29 120.2(3) . . ? C36 C31 C32 118.6(2) . . ? C36 C31 P1 118.4(2) . . ? C32 C31 P1 122.8(2) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 120.2(3) . . ? C33 C34 C35 119.7(3) . . ? C34 C35 C36 120.9(3) . . ? C31 C36 C35 119.8(3) . . ? O2 C37 O1 122.6(2) . . ? O2 C37 C38 117.9(2) . . ? O1 C37 C38 119.5(2) . . ? C39 C38 C40 124.3(3) . . ? C39 C38 C37 119.1(3) . . ? C40 C38 C37 116.6(2) . . ? C38 C39 C41 126.6(3) . . ? _refine_diff_density_max 0.337 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.052 data_97vo1 _database_code_CSD 195317 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20.50 H18.50 Ag0.50 O P' _chemical_formula_weight 365.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.806(5) _cell_length_b 12.996(4) _cell_length_c 13.056(6) _cell_angle_alpha 66.26(3) _cell_angle_beta 62.40(3) _cell_angle_gamma 72.79(3) _cell_volume 1746.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method ? _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5758 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.93 _reflns_number_total 5477 _reflns_number_observed 4700 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.8933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5466 _refine_ls_number_parameters 435 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0325 _refine_ls_wR_factor_all 0.1109 _refine_ls_wR_factor_obs 0.0993 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.11684(2) 0.72224(2) 0.71726(3) 0.04215(13) Uani 1 d . . P1 P 0.28472(8) 0.82946(7) 0.62130(8) 0.0371(2) Uani 1 d . . P2 P -0.07053(8) 0.75098(8) 0.88396(8) 0.0382(2) Uani 1 d . . O1 O 0.1900(3) 0.5461(2) 0.6723(3) 0.0642(8) Uani 1 d . . O2 O 0.0911(4) 0.6715(3) 0.5685(4) 0.0846(12) Uani 1 d . . C1 C 0.2370(3) 0.9808(3) 0.5644(3) 0.0362(7) Uani 1 d . . C2 C 0.1629(4) 1.0131(3) 0.5029(4) 0.0489(9) Uani 1 d . . H2 H 0.1414(4) 0.9585(3) 0.4897(4) 0.059 Uiso 1 calc R . C3 C 0.1207(4) 1.1266(4) 0.4609(4) 0.0582(11) Uani 1 d . . H3 H 0.0710(4) 1.1478(4) 0.4198(4) 0.070 Uiso 1 calc R . C4 C 0.1516(4) 1.2075(4) 0.4795(4) 0.0565(11) Uani 1 d . . H4 H 0.1220(4) 1.2834(4) 0.4522(4) 0.068 Uiso 1 calc R . C5 C 0.2268(4) 1.1767(3) 0.5389(4) 0.0557(10) Uani 1 d . . H5 H 0.2492(4) 1.2318(3) 0.5503(4) 0.067 Uiso 1 calc R . C6 C 0.2689(3) 1.0632(3) 0.5816(4) 0.0462(9) Uani 1 d . . H6 H 0.3190(3) 1.0425(3) 0.6222(4) 0.055 Uiso 1 calc R . C7 C 0.4130(3) 0.8001(3) 0.4899(3) 0.0413(8) Uani 1 d . . C8 C 0.4742(3) 0.8837(3) 0.3922(4) 0.0486(9) Uani 1 d . . H8 H 0.4498(3) 0.9591(3) 0.3904(4) 0.058 Uiso 1 calc R . C9 C 0.5728(4) 0.8556(4) 0.2960(4) 0.0609(11) Uani 1 d . . H9 H 0.6142(4) 0.9124(4) 0.2300(4) 0.073 Uiso 1 calc R . C10 C 0.6092(4) 0.7462(5) 0.2976(5) 0.0715(13) Uani 1 d . . H10 H 0.6752(4) 0.7278(5) 0.2329(5) 0.086 Uiso 1 calc R . C11 C 0.5489(5) 0.6639(5) 0.3936(6) 0.086(2) Uani 1 d . . H11 H 0.5754(5) 0.5886(5) 0.3953(6) 0.103 Uiso 1 calc R . C12 C 0.4487(4) 0.6889(4) 0.4897(5) 0.0651(12) Uani 1 d . . H12 H 0.4060(4) 0.6317(4) 0.5533(5) 0.078 Uiso 1 calc R . C13 C -0.0508(3) 0.7589(3) 1.0104(3) 0.0418(8) Uani 1 d . . C14 C -0.0922(4) 0.8542(4) 1.0476(4) 0.0545(10) Uani 1 d . . H14 H -0.1378(4) 0.9154(4) 1.0123(4) 0.065 Uiso 1 calc R . C15 C -0.0659(5) 0.8591(5) 1.1374(5) 0.0737(14) Uani 1 d . . H15 H -0.0941(5) 0.9235(5) 1.1619(5) 0.088 Uiso 1 calc R . C16 C 0.0013(5) 0.7697(5) 1.1900(4) 0.0721(14) Uani 1 d . . H16 H 0.0198(5) 0.7736(5) 1.2493(4) 0.087 Uiso 1 calc R . C17 C 0.0410(4) 0.6742(5) 1.1543(4) 0.0666(12) Uani 1 d . . H17 H 0.0845(4) 0.6122(5) 1.1915(4) 0.080 Uiso 1 calc R . C18 C 0.0168(4) 0.6696(4) 1.0642(4) 0.0562(10) Uani 1 d . . H18 H 0.0465(4) 0.6054(4) 1.0391(4) 0.067 Uiso 1 calc R . C19 C -0.1642(3) 0.8842(3) 0.8434(3) 0.0443(8) Uani 1 d . . C20 C -0.2873(4) 0.8938(4) 0.8901(5) 0.0614(11) Uani 1 d . . H20 H -0.3256(4) 0.8309(4) 0.9453(5) 0.074 Uiso 1 calc R . C21 C -0.3528(4) 0.9965(4) 0.8549(6) 0.0759(14) Uani 1 d . . H21 H -0.4352(4) 1.0022(4) 0.8865(6) 0.091 Uiso 1 calc R . C22 C -0.2980(5) 1.0909(4) 0.7737(5) 0.0713(13) Uani 1 d . . H22 H -0.3430(5) 1.1598(4) 0.7504(5) 0.086 Uiso 1 calc R . C23 C -0.1771(5) 1.0824(4) 0.7277(5) 0.0642(12) Uani 1 d . . H23 H -0.1395(5) 1.1461(4) 0.6736(5) 0.077 Uiso 1 calc R . C24 C -0.1100(4) 0.9793(3) 0.7611(4) 0.0518(9) Uani 1 d . . H24 H -0.0275(4) 0.9741(3) 0.7279(4) 0.062 Uiso 1 calc R . C25 C -0.1688(3) 0.6443(3) 0.9510(3) 0.0421(8) Uani 1 d . . C26 C -0.2118(3) 0.5806(3) 1.0723(3) 0.0452(9) Uani 1 d . . H26 H -0.1892(3) 0.5896(3) 1.1260(3) 0.054 Uiso 1 calc R . C27 C -0.2889(4) 0.5027(4) 1.1146(4) 0.0594(11) Uani 1 d . . H27 H -0.3165(4) 0.4591(4) 1.1962(4) 0.071 Uiso 1 calc R . C28 C -0.3244(4) 0.4900(4) 1.0360(5) 0.0673(13) Uani 1 d . . H28 H -0.3782(4) 0.4400(4) 1.0653(5) 0.081 Uiso 1 calc R . C29 C -0.2805(5) 0.5512(4) 0.9145(5) 0.0658(12) Uani 1 d . . H29 H -0.3035(5) 0.5417(4) 0.8613(5) 0.079 Uiso 1 calc R . C30 C -0.2025(4) 0.6265(4) 0.8720(4) 0.0577(11) Uani 1 d . . H30 H -0.1714(4) 0.6663(4) 0.7893(4) 0.069 Uiso 1 calc R . C31 C 0.3477(3) 0.8198(3) 0.7252(3) 0.0427(8) Uani 1 d . . C32 C 0.4691(4) 0.8037(4) 0.6963(4) 0.0576(11) Uani 1 d . . H32 H 0.5230(4) 0.7972(4) 0.6204(4) 0.069 Uiso 1 calc R . C33 C 0.5103(5) 0.7970(5) 0.7810(5) 0.0727(14) Uani 1 d . . H33 H 0.5917(5) 0.7845(5) 0.7617(5) 0.087 Uiso 1 calc R . C34 C 0.4329(5) 0.8086(5) 0.8911(5) 0.0734(14) Uani 1 d . . H34 H 0.4613(5) 0.8054(5) 0.9464(5) 0.088 Uiso 1 calc R . C35 C 0.3129(5) 0.8251(4) 0.9212(4) 0.0688(13) Uani 1 d . . H35 H 0.2601(5) 0.8332(4) 0.9967(4) 0.083 Uiso 1 calc R . C36 C 0.2701(4) 0.8298(4) 0.8394(4) 0.0550(10) Uani 1 d . . H36 H 0.1884(4) 0.8397(4) 0.8610(4) 0.066 Uiso 1 calc R . C37 C 0.1456(4) 0.5763(3) 0.5968(4) 0.0493(9) Uani 1 d . . C38 C 0.1596(6) 0.4917(4) 0.5365(5) 0.0747(14) Uani 1 d . . H38A H 0.2259(6) 0.4337(4) 0.5448(5) 0.090 Uiso 1 calc R . H38B H 0.0885(6) 0.4549(4) 0.5798(5) 0.090 Uiso 1 calc R . C39 C 0.1800(7) 0.5411(6) 0.4061(6) 0.094(2) Uani 1 d D . H39A H 0.1301(7) 0.6133(6) 0.3911(6) 0.112 Uiso 1 calc R 1 H39B H 0.1626(7) 0.4904(6) 0.3799(6) 0.112 Uiso 1 calc R 1 C40 C 0.3150(20) 0.5573(28) 0.3370(19) 0.140(10) Uani 0.55 d PD 1 H40 H 0.3553(20) 0.5228(28) 0.3886(19) 0.168 Uiso 0.55 calc PR 1 C41 C 0.3778(27) 0.6011(24) 0.2383(24) 0.147(11) Uani 0.55 d P 1 H41A H 0.3481(27) 0.6388(24) 0.1778(24) 0.176 Uiso 0.55 calc PR 1 H41B H 0.4577(27) 0.5985(24) 0.2198(24) 0.176 Uiso 0.55 calc PR 1 C40A C 0.2857(19) 0.5995(14) 0.3122(24) 0.107(8) Uani 0.45 d PD 2 H40A H 0.2694(19) 0.6761(14) 0.2728(24) 0.128 Uiso 0.45 calc PR 2 C41A C 0.3773(35) 0.5649(65) 0.2842(67) 0.294(43) Uani 0.45 d P 2 H41C H 0.3997(35) 0.4886(65) 0.3200(67) 0.353 Uiso 0.45 calc PR 2 H41D H 0.4349(35) 0.6109(65) 0.2241(67) 0.353 Uiso 0.45 calc PR 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 0.0410(2) 0.0413(2) 0.0447(2) -0.01738(12) -0.01354(13) -0.00645(11) P1 0.0351(5) 0.0334(5) 0.0428(5) -0.0134(4) -0.0147(4) -0.0039(4) P2 0.0395(5) 0.0383(5) 0.0362(5) -0.0125(4) -0.0134(4) -0.0058(4) O1 0.095(2) 0.047(2) 0.067(2) -0.0161(14) -0.051(2) -0.003(2) O2 0.103(3) 0.074(2) 0.114(3) -0.053(2) -0.079(3) 0.032(2) C1 0.032(2) 0.035(2) 0.039(2) -0.0140(14) -0.0108(14) -0.0024(14) C2 0.056(2) 0.048(2) 0.051(2) -0.014(2) -0.027(2) -0.009(2) C3 0.063(3) 0.060(3) 0.052(2) -0.009(2) -0.034(2) 0.001(2) C4 0.057(2) 0.040(2) 0.054(2) -0.009(2) -0.018(2) 0.004(2) C5 0.064(3) 0.039(2) 0.065(3) -0.024(2) -0.023(2) -0.002(2) C6 0.045(2) 0.040(2) 0.057(2) -0.015(2) -0.025(2) -0.002(2) C7 0.037(2) 0.042(2) 0.047(2) -0.019(2) -0.016(2) -0.0014(15) C8 0.044(2) 0.047(2) 0.052(2) -0.021(2) -0.013(2) -0.004(2) C9 0.049(2) 0.071(3) 0.055(2) -0.026(2) -0.007(2) -0.012(2) C10 0.053(3) 0.083(4) 0.077(3) -0.051(3) -0.006(2) -0.003(2) C11 0.079(4) 0.058(3) 0.104(4) -0.051(3) -0.009(3) 0.004(3) C12 0.067(3) 0.041(2) 0.071(3) -0.029(2) -0.006(2) -0.007(2) C13 0.037(2) 0.048(2) 0.038(2) -0.014(2) -0.010(2) -0.011(2) C14 0.067(3) 0.048(2) 0.051(2) -0.022(2) -0.024(2) 0.000(2) C15 0.105(4) 0.070(3) 0.061(3) -0.037(3) -0.031(3) -0.013(3) C16 0.080(3) 0.097(4) 0.058(3) -0.031(3) -0.033(3) -0.017(3) C17 0.064(3) 0.083(3) 0.059(3) -0.026(2) -0.034(2) 0.003(2) C18 0.056(2) 0.064(3) 0.055(2) -0.029(2) -0.026(2) 0.006(2) C19 0.048(2) 0.040(2) 0.048(2) -0.015(2) -0.021(2) -0.003(2) C20 0.050(2) 0.054(2) 0.072(3) -0.013(2) -0.024(2) -0.005(2) C21 0.050(3) 0.064(3) 0.105(4) -0.022(3) -0.035(3) 0.006(2) C22 0.081(3) 0.048(3) 0.095(4) -0.025(3) -0.053(3) 0.012(2) C23 0.083(3) 0.040(2) 0.076(3) -0.011(2) -0.043(3) -0.007(2) C24 0.057(2) 0.044(2) 0.058(2) -0.016(2) -0.028(2) -0.006(2) C25 0.043(2) 0.038(2) 0.043(2) -0.012(2) -0.018(2) -0.003(2) C26 0.048(2) 0.041(2) 0.046(2) -0.017(2) -0.018(2) -0.001(2) C27 0.056(2) 0.049(2) 0.060(3) -0.006(2) -0.017(2) -0.015(2) C28 0.060(3) 0.046(2) 0.092(4) -0.012(2) -0.027(3) -0.019(2) C29 0.079(3) 0.062(3) 0.078(3) -0.024(2) -0.043(3) -0.017(2) C30 0.076(3) 0.056(2) 0.050(2) -0.011(2) -0.031(2) -0.019(2) C31 0.044(2) 0.033(2) 0.046(2) -0.0029(15) -0.021(2) -0.0065(15) C32 0.046(2) 0.063(3) 0.059(3) -0.009(2) -0.024(2) -0.011(2) C33 0.068(3) 0.076(3) 0.083(4) -0.007(3) -0.048(3) -0.015(2) C34 0.089(4) 0.083(3) 0.064(3) -0.005(3) -0.044(3) -0.033(3) C35 0.088(4) 0.075(3) 0.051(3) -0.014(2) -0.030(2) -0.026(3) C36 0.052(2) 0.063(3) 0.050(2) -0.014(2) -0.019(2) -0.016(2) C37 0.052(2) 0.044(2) 0.056(2) -0.018(2) -0.023(2) -0.005(2) C38 0.107(4) 0.063(3) 0.069(3) -0.030(2) -0.036(3) -0.018(3) C39 0.130(6) 0.097(4) 0.082(4) -0.039(3) -0.050(4) -0.024(4) C40 0.121(21) 0.169(25) 0.075(10) 0.017(14) -0.047(12) -0.011(17) C41 0.156(22) 0.181(19) 0.116(13) -0.103(15) 0.016(13) -0.078(16) C40A 0.097(14) 0.052(9) 0.103(19) -0.003(9) -0.016(14) 0.012(8) C41A 0.076(22) 0.398(85) 0.319(76) -0.064(62) -0.025(28) -0.071(34) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.401(3) . ? Ag1 P2 2.433(2) . ? Ag1 P1 2.4504(15) . ? Ag1 O2 2.464(4) . ? P1 C31 1.823(4) . ? P1 C1 1.824(4) . ? P1 C7 1.826(4) . ? P2 C25 1.819(4) . ? P2 C13 1.827(4) . ? P2 C19 1.828(4) . ? O1 C37 1.235(5) . ? O2 C37 1.230(5) . ? C1 C6 1.378(5) . ? C1 C2 1.387(5) . ? C2 C3 1.385(6) . ? C3 C4 1.365(7) . ? C4 C5 1.379(7) . ? C5 C6 1.387(6) . ? C7 C8 1.373(6) . ? C7 C12 1.380(6) . ? C8 C9 1.390(6) . ? C9 C10 1.354(7) . ? C10 C11 1.351(8) . ? C11 C12 1.385(7) . ? C13 C18 1.379(6) . ? C13 C14 1.381(6) . ? C14 C15 1.389(7) . ? C15 C16 1.370(8) . ? C16 C17 1.374(7) . ? C17 C18 1.375(6) . ? C19 C24 1.383(6) . ? C19 C20 1.387(6) . ? C20 C21 1.377(7) . ? C21 C22 1.375(8) . ? C22 C23 1.365(7) . ? C23 C24 1.385(6) . ? C25 C26 1.379(5) . ? C25 C30 1.403(6) . ? C26 C27 1.392(6) . ? C27 C28 1.378(7) . ? C28 C29 1.373(7) . ? C29 C30 1.376(7) . ? C31 C32 1.390(6) . ? C31 C36 1.390(6) . ? C32 C33 1.394(7) . ? C33 C34 1.356(8) . ? C34 C35 1.369(8) . ? C35 C36 1.384(6) . ? C37 C38 1.520(6) . ? C38 C39 1.478(8) . ? C39 C40A 1.49(2) . ? C39 C40 1.57(2) . ? C40 C41 1.16(3) . ? C40A C41A 1.07(5) . ? 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 P2 122.61(10) . . ? O1 Ag1 P1 107.95(10) . . ? P2 Ag1 P1 126.23(4) . . ? O1 Ag1 O2 52.84(11) . . ? P2 Ag1 O2 112.50(11) . . ? P1 Ag1 O2 111.88(12) . . ? C31 P1 C1 104.0(2) . . ? C31 P1 C7 104.6(2) . . ? C1 P1 C7 103.5(2) . . ? C31 P1 Ag1 114.04(12) . . ? C1 P1 Ag1 110.48(12) . . ? C7 P1 Ag1 118.74(13) . . ? C25 P2 C13 105.8(2) . . ? C25 P2 C19 103.5(2) . . ? C13 P2 C19 103.1(2) . . ? C25 P2 Ag1 115.83(13) . . ? C13 P2 Ag1 113.01(12) . . ? C19 P2 Ag1 114.26(14) . . ? C37 O1 Ag1 93.5(2) . . ? C37 O2 Ag1 90.7(3) . . ? C6 C1 C2 119.0(3) . . ? C6 C1 P1 123.5(3) . . ? C2 C1 P1 117.5(3) . . ? C3 C2 C1 120.1(4) . . ? C4 C3 C2 120.5(4) . . ? C3 C4 C5 120.0(4) . . ? C4 C5 C6 119.8(4) . . ? C1 C6 C5 120.6(4) . . ? C8 C7 C12 119.3(4) . . ? C8 C7 P1 122.7(3) . . ? C12 C7 P1 118.1(3) . . ? C7 C8 C9 119.9(4) . . ? C10 C9 C8 120.6(4) . . ? C11 C10 C9 119.5(4) . . ? C10 C11 C12 121.5(5) . . ? C7 C12 C11 119.1(4) . . ? C18 C13 C14 118.6(4) . . ? C18 C13 P2 118.4(3) . . ? C14 C13 P2 122.8(3) . . ? C13 C14 C15 120.2(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C17 119.2(4) . . ? C16 C17 C18 120.5(4) . . ? C17 C18 C13 120.9(4) . . ? C24 C19 C20 118.5(4) . . ? C24 C19 P2 118.5(3) . . ? C20 C19 P2 122.9(3) . . ? C21 C20 C19 120.1(4) . . ? C22 C21 C20 121.0(5) . . ? C23 C22 C21 119.4(4) . . ? C22 C23 C24 120.3(4) . . ? C19 C24 C23 120.8(4) . . ? C26 C25 C30 118.3(4) . . ? C26 C25 P2 125.0(3) . . ? C30 C25 P2 116.7(3) . . ? C25 C26 C27 120.3(4) . . ? C28 C27 C26 120.3(4) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 119.7(4) . . ? C29 C30 C25 121.2(4) . . ? C32 C31 C36 118.1(4) . . ? C32 C31 P1 123.6(3) . . ? C36 C31 P1 118.3(3) . . ? C31 C32 C33 120.2(5) . . ? C34 C33 C32 120.6(5) . . ? C33 C34 C35 120.1(5) . . ? C34 C35 C36 120.2(5) . . ? C35 C36 C31 120.7(4) . . ? O2 C37 O1 122.9(4) . . ? O2 C37 C38 119.0(4) . . ? O1 C37 C38 118.2(4) . . ? C39 C38 C37 114.8(5) . . ? C38 C39 C40A 122.6(14) . . ? C38 C39 C40 105.4(9) . . ? C41 C40 C39 136.8(24) . . ? C41A C40A C39 128.6(46) . . ? _refine_diff_density_max 0.442 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.070 data_96dae1 _database_code_CSD 195318 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H32 Ag N O2 P2' _chemical_formula_weight 716.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.689(3) _cell_length_b 12.850(2) _cell_length_c 13.351(3) _cell_angle_alpha 65.160(10) _cell_angle_beta 61.89(2) _cell_angle_gamma 72.21(2) _cell_volume 1726.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method ? _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5692 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.93 _reflns_number_total 5418 _reflns_number_observed 4589 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+1.1845P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0075(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5415 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_obs 0.0249 _refine_ls_wR_factor_all 0.0724 _refine_ls_wR_factor_obs 0.0639 _refine_ls_goodness_of_fit_all 0.920 _refine_ls_goodness_of_fit_obs 0.892 _refine_ls_restrained_S_all 0.924 _refine_ls_restrained_S_obs 0.892 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.10815(2) 0.22284(2) 0.22616(2) 0.04659(9) Uani 1 d . . P1 P -0.08409(6) 0.25554(6) 0.38425(6) 0.0432(2) Uani 1 d . . P2 P 0.28109(6) 0.32857(5) 0.12668(6) 0.0413(2) Uani 1 d . . N1 N 0.1743(9) 0.0696(6) -0.1605(7) 0.262(5) Uani 1 d . . O1 O 0.1000(3) 0.1712(2) 0.0697(3) 0.0936(9) Uani 1 d . . O2 O 0.1899(2) 0.0415(2) 0.1843(2) 0.0709(6) Uani 1 d . . C1 C -0.1875(2) 0.1499(2) 0.4510(2) 0.0460(6) Uani 1 d . . C2 C -0.2133(3) 0.1263(3) 0.3739(3) 0.0613(8) Uani 1 d . . H2 H -0.1757(3) 0.1616(3) 0.2913(3) 0.074 Uiso 1 calc R . C3 C -0.2947(3) 0.0505(3) 0.4179(3) 0.0721(9) Uani 1 d . . H3 H -0.3137(3) 0.0373(3) 0.3653(3) 0.087 Uiso 1 calc R . C4 C -0.3468(3) -0.0046(3) 0.5387(4) 0.0782(10) Uani 1 d . . H4 H -0.4037(3) -0.0534(3) 0.5689(4) 0.094 Uiso 1 calc R . C5 C -0.3153(3) 0.0120(3) 0.6153(3) 0.0796(10) Uani 1 d . . H5 H -0.3473(3) -0.0291(3) 0.6971(3) 0.095 Uiso 1 calc R . C6 C -0.2362(3) 0.0895(3) 0.5724(3) 0.0624(8) Uani 1 d . . H6 H -0.2159(3) 0.1008(3) 0.6252(3) 0.075 Uiso 1 calc R . C7 C -0.1728(2) 0.3946(2) 0.3402(2) 0.0467(6) Uani 1 d . . C8 C -0.2971(3) 0.4103(3) 0.3856(3) 0.0688(8) Uani 1 d . . H8 H -0.3391(3) 0.3478(3) 0.4404(3) 0.083 Uiso 1 calc R . C9 C -0.3594(3) 0.5183(3) 0.3501(4) 0.0850(11) Uani 1 d . . H9 H -0.4432(3) 0.5280(3) 0.3808(4) 0.102 Uiso 1 calc R . C10 C -0.2985(4) 0.6118(3) 0.2696(3) 0.0789(10) Uani 1 d . . H10 H -0.3408(4) 0.6845(3) 0.2461(3) 0.095 Uiso 1 calc R . C11 C -0.1750(3) 0.5972(3) 0.2242(3) 0.0704(9) Uani 1 d . . H11 H -0.1335(3) 0.6602(3) 0.1701(3) 0.084 Uiso 1 calc R . C12 C -0.1125(3) 0.4901(2) 0.2583(3) 0.0577(7) Uani 1 d . . H12 H -0.0287(3) 0.4809(2) 0.2263(3) 0.069 Uiso 1 calc R . C13 C -0.0624(2) 0.2596(2) 0.5076(2) 0.0457(6) Uani 1 d . . C14 C -0.1025(3) 0.3560(3) 0.5441(3) 0.0595(7) Uani 1 d . . H14 H -0.1490(3) 0.4194(3) 0.5102(3) 0.071 Uiso 1 calc R . C15 C -0.0735(4) 0.3579(3) 0.6311(3) 0.0767(10) Uani 1 d . . H15 H -0.0996(4) 0.4233(3) 0.6542(3) 0.092 Uiso 1 calc R . C16 C -0.0073(3) 0.2654(3) 0.6830(3) 0.0745(10) Uani 1 d . . H16 H 0.0110(3) 0.2674(3) 0.7418(3) 0.089 Uiso 1 calc R . C17 C 0.0323(3) 0.1696(3) 0.6486(3) 0.0776(10) Uani 1 d . . H17 H 0.0771(3) 0.1061(3) 0.6846(3) 0.093 Uiso 1 calc R . C18 C 0.0061(3) 0.1663(3) 0.5603(3) 0.0647(8) Uani 1 d . . H18 H 0.0346(3) 0.1012(3) 0.5364(3) 0.078 Uiso 1 calc R . C19 C 0.4094(2) 0.2975(2) -0.0031(2) 0.0462(6) Uani 1 d . . C20 C 0.4403(3) 0.1861(3) -0.0048(3) 0.0766(10) Uani 1 d . . H20 H 0.3953(3) 0.1283(3) 0.0581(3) 0.092 Uiso 1 calc R . C21 C 0.5393(4) 0.1602(3) -0.1011(4) 0.1042(15) Uani 1 d . . H21 H 0.5615(4) 0.0843(3) -0.1013(4) 0.125 Uiso 1 calc R . C22 C 0.6043(3) 0.2436(3) -0.1947(3) 0.0848(11) Uani 1 d . . H22 H 0.6710(3) 0.2247(3) -0.2582(3) 0.102 Uiso 1 calc R . C23 C 0.5719(3) 0.3545(3) -0.1958(3) 0.0642(8) Uani 1 d . . H23 H 0.6152(3) 0.4123(3) -0.2609(3) 0.077 Uiso 1 calc R . C24 C 0.4745(2) 0.3816(2) -0.0999(2) 0.0531(7) Uani 1 d . . H24 H 0.4527(2) 0.4579(2) -0.1009(2) 0.064 Uiso 1 calc R . C25 C 0.3453(2) 0.3199(2) 0.2272(2) 0.0457(6) Uani 1 d . . C26 C 0.2667(3) 0.3260(3) 0.3408(3) 0.0591(7) Uani 1 d . . H26 H 0.1841(3) 0.3333(3) 0.3636(3) 0.071 Uiso 1 calc R . C27 C 0.3099(3) 0.3213(3) 0.4205(3) 0.0729(9) Uani 1 d . . H27 H 0.2563(3) 0.3269(3) 0.4957(3) 0.088 Uiso 1 calc R . C28 C 0.4314(4) 0.3082(3) 0.3885(3) 0.0784(10) Uani 1 d . . H28 H 0.4606(4) 0.3040(3) 0.4425(3) 0.094 Uiso 1 calc R . C29 C 0.5100(3) 0.3014(3) 0.2772(3) 0.0756(10) Uani 1 d . . H29 H 0.5925(3) 0.2927(3) 0.2558(3) 0.091 Uiso 1 calc R . C30 C 0.4679(3) 0.3074(3) 0.1962(3) 0.0598(7) Uani 1 d . . H30 H 0.5221(3) 0.3029(3) 0.1206(3) 0.072 Uiso 1 calc R . C31 C 0.2340(2) 0.4820(2) 0.0658(2) 0.0397(5) Uani 1 d . . C32 C 0.1652(3) 0.5152(3) -0.0015(3) 0.0554(7) Uani 1 d . . H32 H 0.1473(3) 0.4594(3) -0.0163(3) 0.066 Uiso 1 calc R . C33 C 0.1235(3) 0.6296(3) -0.0463(3) 0.0641(8) Uani 1 d . . H33 H 0.0777(3) 0.6507(3) -0.0911(3) 0.077 Uiso 1 calc R . C34 C 0.1491(3) 0.7132(3) -0.0255(3) 0.0639(8) Uani 1 d . . H34 H 0.1196(3) 0.7906(3) -0.0550(3) 0.077 Uiso 1 calc R . C35 C 0.2179(3) 0.6821(2) 0.0387(3) 0.0627(8) Uani 1 d . . H35 H 0.2367(3) 0.7387(2) 0.0515(3) 0.075 Uiso 1 calc R . C36 C 0.2601(2) 0.5671(2) 0.0848(3) 0.0508(6) Uani 1 d . . H36 H 0.3064(2) 0.5469(2) 0.1289(3) 0.061 Uiso 1 calc R . C37 C 0.1536(3) 0.0759(3) 0.1038(3) 0.0602(7) Uani 1 d . . C38 C 0.1803(5) -0.0111(3) 0.0411(4) 0.109(2) Uani 1 d . . H38A H 0.2594(5) -0.0544(3) 0.0343(4) 0.131 Uiso 1 calc R . H38B H 0.1222(5) -0.0656(3) 0.0924(4) 0.131 Uiso 1 calc R . C39 C 0.1778(6) 0.0342(4) -0.0710(5) 0.124(2) Uani 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 0.04577(13) 0.04738(13) 0.04740(13) -0.02145(9) -0.01089(9) -0.01142(8) P1 0.0434(4) 0.0458(4) 0.0396(3) -0.0166(3) -0.0109(3) -0.0105(3) P2 0.0382(3) 0.0378(3) 0.0470(4) -0.0161(3) -0.0134(3) -0.0069(3) N1 0.483(14) 0.209(7) 0.212(7) -0.117(6) -0.256(9) 0.068(8) O1 0.125(2) 0.073(2) 0.127(2) -0.060(2) -0.091(2) 0.0376(15) O2 0.107(2) 0.0523(12) 0.0645(13) -0.0196(10) -0.0485(13) -0.0009(11) C1 0.0495(14) 0.0436(14) 0.0408(14) -0.0132(11) -0.0131(12) -0.0101(11) C2 0.077(2) 0.064(2) 0.051(2) -0.0109(14) -0.029(2) -0.026(2) C3 0.087(2) 0.068(2) 0.085(2) -0.021(2) -0.047(2) -0.023(2) C4 0.078(2) 0.062(2) 0.094(3) -0.013(2) -0.031(2) -0.031(2) C5 0.094(3) 0.070(2) 0.059(2) -0.009(2) -0.013(2) -0.037(2) C6 0.076(2) 0.060(2) 0.049(2) -0.0169(14) -0.0181(15) -0.021(2) C7 0.0481(15) 0.0512(15) 0.0432(14) -0.0172(12) -0.0172(12) -0.0088(12) C8 0.051(2) 0.069(2) 0.074(2) -0.015(2) -0.022(2) -0.0099(15) C9 0.058(2) 0.083(3) 0.099(3) -0.024(2) -0.034(2) 0.006(2) C10 0.088(3) 0.063(2) 0.085(2) -0.022(2) -0.048(2) 0.010(2) C11 0.086(2) 0.053(2) 0.071(2) -0.013(2) -0.034(2) -0.013(2) C12 0.057(2) 0.052(2) 0.060(2) -0.0147(14) -0.0211(14) -0.0108(13) C13 0.0414(13) 0.054(2) 0.0419(14) -0.0204(12) -0.0100(11) -0.0107(11) C14 0.067(2) 0.060(2) 0.057(2) -0.0283(14) -0.0226(15) -0.0056(14) C15 0.099(3) 0.079(2) 0.073(2) -0.044(2) -0.035(2) -0.011(2) C16 0.075(2) 0.106(3) 0.060(2) -0.038(2) -0.027(2) -0.019(2) C17 0.081(2) 0.093(3) 0.069(2) -0.032(2) -0.044(2) 0.006(2) C18 0.074(2) 0.063(2) 0.065(2) -0.031(2) -0.035(2) 0.007(2) C19 0.0388(13) 0.0444(14) 0.057(2) -0.0231(12) -0.0149(12) -0.0046(11) C20 0.069(2) 0.046(2) 0.086(2) -0.030(2) -0.003(2) -0.0067(15) C21 0.095(3) 0.063(2) 0.120(3) -0.057(2) 0.004(3) -0.004(2) C22 0.066(2) 0.090(3) 0.084(2) -0.055(2) 0.003(2) -0.010(2) C23 0.056(2) 0.077(2) 0.055(2) -0.026(2) -0.0095(14) -0.017(2) C24 0.049(2) 0.051(2) 0.056(2) -0.0233(13) -0.0116(13) -0.0093(12) C25 0.0469(14) 0.0368(13) 0.053(2) -0.0102(11) -0.0223(12) -0.0084(11) C26 0.055(2) 0.066(2) 0.062(2) -0.0242(15) -0.0224(15) -0.0119(14) C27 0.087(2) 0.081(2) 0.062(2) -0.022(2) -0.031(2) -0.024(2) C28 0.096(3) 0.082(2) 0.076(2) -0.008(2) -0.053(2) -0.030(2) C29 0.062(2) 0.084(2) 0.085(3) -0.009(2) -0.042(2) -0.021(2) C30 0.052(2) 0.062(2) 0.062(2) -0.0110(14) -0.0253(14) -0.0119(13) C31 0.0353(12) 0.0418(13) 0.0391(13) -0.0165(11) -0.0099(10) -0.0049(10) C32 0.062(2) 0.057(2) 0.055(2) -0.0195(14) -0.0285(14) -0.0091(14) C33 0.069(2) 0.064(2) 0.059(2) -0.013(2) -0.037(2) 0.001(2) C34 0.071(2) 0.047(2) 0.057(2) -0.0130(14) -0.024(2) 0.0062(14) C35 0.077(2) 0.042(2) 0.075(2) -0.0272(15) -0.032(2) -0.0001(14) C36 0.054(2) 0.0439(15) 0.063(2) -0.0218(13) -0.0279(14) -0.0026(12) C37 0.078(2) 0.048(2) 0.066(2) -0.0281(15) -0.034(2) -0.0014(15) C38 0.181(5) 0.074(2) 0.103(3) -0.051(2) -0.080(3) 0.013(3) C39 0.208(6) 0.105(3) 0.120(4) -0.063(3) -0.110(4) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4185(10) . ? Ag1 O2 2.427(2) . ? Ag1 P2 2.4464(10) . ? Ag1 O1 2.495(2) . ? P1 C13 1.816(3) . ? P1 C7 1.821(3) . ? P1 C1 1.824(3) . ? P2 C31 1.815(2) . ? P2 C25 1.825(3) . ? P2 C19 1.827(3) . ? N1 C39 1.103(6) . ? O1 C37 1.219(4) . ? O2 C37 1.226(4) . ? C1 C6 1.380(4) . ? C1 C2 1.380(4) . ? C2 C3 1.386(4) . ? C3 C4 1.364(5) . ? C4 C5 1.370(5) . ? C5 C6 1.384(5) . ? C7 C8 1.379(4) . ? C7 C12 1.394(4) . ? C8 C9 1.381(5) . ? C9 C10 1.377(5) . ? C10 C11 1.370(5) . ? C11 C12 1.370(4) . ? C13 C18 1.385(4) . ? C13 C14 1.385(4) . ? C14 C15 1.384(4) . ? C15 C16 1.358(5) . ? C16 C17 1.362(5) . ? C17 C18 1.386(4) . ? C19 C20 1.371(4) . ? C19 C24 1.374(4) . ? C20 C21 1.387(5) . ? C21 C22 1.354(5) . ? C22 C23 1.354(5) . ? C23 C24 1.381(4) . ? C25 C30 1.382(4) . ? C25 C26 1.388(4) . ? C26 C27 1.381(4) . ? C27 C28 1.368(5) . ? C28 C29 1.367(5) . ? C29 C30 1.383(4) . ? C31 C36 1.379(4) . ? C31 C32 1.394(4) . ? C32 C33 1.372(4) . ? C33 C34 1.373(5) . ? C34 C35 1.365(4) . ? C35 C36 1.383(4) . ? C37 C38 1.535(4) . ? C38 C39 1.372(6) . ? 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 O2 124.33(6) . . ? P1 Ag1 P2 127.93(3) . . ? O2 Ag1 P2 104.89(7) . . ? P1 Ag1 O1 115.66(7) . . ? O2 Ag1 O1 52.61(7) . . ? P2 Ag1 O1 106.75(8) . . ? C13 P1 C7 103.63(12) . . ? C13 P1 C1 106.12(12) . . ? C7 P1 C1 104.42(12) . . ? C13 P1 Ag1 110.55(9) . . ? C7 P1 Ag1 114.34(9) . . ? C1 P1 Ag1 116.65(9) . . ? C31 P2 C25 104.44(11) . . ? C31 P2 C19 102.78(11) . . ? C25 P2 C19 105.49(12) . . ? C31 P2 Ag1 109.60(8) . . ? C25 P2 Ag1 114.13(9) . . ? C19 P2 Ag1 118.92(8) . . ? C37 O1 Ag1 89.0(2) . . ? C37 O2 Ag1 92.0(2) . . ? C6 C1 C2 118.8(3) . . ? C6 C1 P1 123.8(2) . . ? C2 C1 P1 117.3(2) . . ? C1 C2 C3 120.8(3) . . ? C4 C3 C2 119.8(3) . . ? C3 C4 C5 119.8(3) . . ? C4 C5 C6 120.7(3) . . ? C1 C6 C5 119.9(3) . . ? C8 C7 C12 118.4(3) . . ? C8 C7 P1 123.0(2) . . ? C12 C7 P1 118.6(2) . . ? C7 C8 C9 120.3(3) . . ? C10 C9 C8 120.5(3) . . ? C11 C10 C9 119.6(3) . . ? C10 C11 C12 120.2(3) . . ? C11 C12 C7 120.9(3) . . ? C18 C13 C14 118.6(3) . . ? C18 C13 P1 118.5(2) . . ? C14 C13 P1 122.7(2) . . ? C15 C14 C13 120.0(3) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 119.9(3) . . ? C16 C17 C18 120.4(3) . . ? C13 C18 C17 120.3(3) . . ? C20 C19 C24 118.7(3) . . ? C20 C19 P2 118.6(2) . . ? C24 C19 P2 122.7(2) . . ? C19 C20 C21 119.4(3) . . ? C22 C21 C20 121.1(3) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 119.7(3) . . ? C19 C24 C23 121.0(3) . . ? C30 C25 C26 118.5(3) . . ? C30 C25 P2 123.4(2) . . ? C26 C25 P2 118.1(2) . . ? C27 C26 C25 120.8(3) . . ? C28 C27 C26 119.9(3) . . ? C29 C28 C27 119.9(3) . . ? C28 C29 C30 120.7(3) . . ? C25 C30 C29 120.1(3) . . ? C36 C31 C32 118.3(2) . . ? C36 C31 P2 123.7(2) . . ? C32 C31 P2 118.0(2) . . ? C33 C32 C31 120.6(3) . . ? C32 C33 C34 120.5(3) . . ? C35 C34 C33 119.5(3) . . ? C34 C35 C36 120.6(3) . . ? C31 C36 C35 120.5(3) . . ? O1 C37 O2 126.4(3) . . ? O1 C37 C38 118.1(3) . . ? O2 C37 C38 115.5(3) . . ? C39 C38 C37 116.4(4) . . ? N1 C39 C38 178.9(8) . . ? _refine_diff_density_max 0.405 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.050 data_96dae2 _database_code_CSD 195319 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H7 Ag O2' _chemical_formula_weight 206.98 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 5.9650(10) _cell_length_b 8.956(2) _cell_length_c 10.292(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.51(2) _cell_angle_gamma 90.00 _cell_volume 549.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.501 _exptl_crystal_density_method ? _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 3.556 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.228 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 676 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 21.97 _reflns_number_total 676 _reflns_number_observed 613 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+1.0654P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(20) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 674 _refine_ls_number_parameters 69 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_obs 0.0357 _refine_ls_wR_factor_all 0.1024 _refine_ls_wR_factor_obs 0.0947 _refine_ls_goodness_of_fit_all 1.154 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_restrained_S_all 1.186 _refine_ls_restrained_S_obs 1.158 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.08128(9) 0.63239(5) 0.44021(5) 0.0233(4) Uani 1 d . . O1 O -0.2630(8) 0.6291(4) 0.3571(4) 0.0171(11) Uani 1 d . . O2 O -0.3542(8) 0.3961(5) 0.4129(5) 0.0178(10) Uani 1 d . . C1 C -0.3882(9) 0.5135(6) 0.3505(6) 0.0137(14) Uiso 1 d . . C2 C -0.5748(9) 0.5191(6) 0.2508(6) 0.0143(14) Uiso 1 d . . C3 C -0.7433(11) 0.4211(7) 0.2596(6) 0.0168(14) Uani 1 d D . H3 H -0.7622(130) 0.3577(61) 0.3247(52) 0.020 Uiso 1 d D . C4 C -0.9362(11) 0.3998(8) 0.1654(7) 0.0196(15) Uani 1 d . . H4A H -1.0649(21) 0.3661(43) 0.2112(8) 0.029 Uiso 1 calc R . H4B H -0.8971(26) 0.3267(33) 0.1017(23) 0.029 Uiso 1 calc R . H4C H -0.9703(44) 0.4928(12) 0.1230(29) 0.029 Uiso 1 calc R . C5 C -0.5548(12) 0.6296(6) 0.1421(7) 0.018(2) Uani 1 d . . H5A H -0.4193(34) 0.6108(27) 0.0965(23) 0.027 Uiso 1 calc R . H5B H -0.5508(64) 0.7290(6) 0.1771(8) 0.027 Uiso 1 calc R . H5C H -0.6814(34) 0.6198(29) 0.0832(21) 0.027 Uiso 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 0.0227(5) 0.0240(5) 0.0233(6) 0.0069(2) -0.0007(3) -0.0039(2) O1 0.019(3) 0.019(3) 0.013(3) -0.003(2) 0.004(2) 0.003(2) O2 0.017(2) 0.025(2) 0.011(2) -0.002(2) 0.007(2) 0.005(2) C3 0.028(4) 0.014(3) 0.009(4) 0.002(3) 0.012(3) 0.006(3) C4 0.017(3) 0.023(3) 0.019(4) 0.000(3) 0.006(3) -0.002(3) C5 0.021(4) 0.021(4) 0.013(4) -0.001(2) 0.009(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.204(5) . ? Ag1 O2 2.207(5) 3_566 ? Ag1 O1 2.490(4) 4_675 ? Ag1 Ag1 2.8532(10) 3_566 ? O1 C1 1.277(7) . ? O1 Ag1 2.490(4) 4_575 ? O2 C1 1.246(8) . ? O2 Ag1 2.207(5) 3_566 ? C1 C2 1.495(9) . ? C2 C3 1.339(9) . ? C2 C5 1.501(9) . ? C3 C4 1.497(10) . ? 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 O2 158.0(2) . 3_566 ? O1 Ag1 O1 103.33(14) . 4_675 ? O2 Ag1 O1 93.4(2) 3_566 4_675 ? O1 Ag1 Ag1 80.35(11) . 3_566 ? O2 Ag1 Ag1 82.03(13) 3_566 3_566 ? O1 Ag1 Ag1 174.44(11) 4_675 3_566 ? C1 O1 Ag1 124.7(4) . . ? C1 O1 Ag1 119.4(4) . 4_575 ? Ag1 O1 Ag1 102.0(2) . 4_575 ? C1 O2 Ag1 123.9(4) . 3_566 ? O2 C1 O1 124.7(6) . . ? O2 C1 C2 119.4(5) . . ? O1 C1 C2 115.7(5) . . ? C3 C2 C1 118.6(6) . . ? C3 C2 C5 123.9(6) . . ? C1 C2 C5 117.5(5) . . ? C2 C3 C4 127.3(6) . . ? _refine_diff_density_max 0.812 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.178