# Copyright The Royal Society of Chemistry, 1998 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 1 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H38 Ag2 Cl2 N8 O8 P2' _chemical_formula_weight 1227.46 _chemical_melting_point ? _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting P-3c1 _symmetry_space_group_name_H-M trigonal loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 23.173(3) _cell_length_b 23.173(3) _cell_length_c 18.795(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8740.5(25) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.69 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method ? _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 1.118 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku RAXIS IIC' _diffrn_measurement_method IP _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22164 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.59 _reflns_number_total 5210 _reflns_number_observed 4550 _reflns_observed_criterion >2sigma(I) _computing_data_collection RASIX _computing_cell_refinement BIOTEX _computing_data_reduction BIOTEX _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SIEMENS SHELXTL PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5210 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_obs 0.0686 _refine_ls_wR_factor_all 0.1950 _refine_ls_wR_factor_obs 0.1825 _refine_ls_goodness_of_fit_all 1.391 _refine_ls_goodness_of_fit_obs 1.396 _refine_ls_restrained_S_all 1.391 _refine_ls_restrained_S_obs 1.396 _refine_ls_shift/esd_max -0.298 _refine_ls_shift/esd_mean 0.051 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 0.33435(2) 0.45896(2) 0.08523(2) 0.0817(2) Uani 1 d . . P1 P 0.25029(7) 0.42200(7) 0.17281(7) 0.0729(4) Uani 1 d . . C1 C 0.1615(4) 0.3136(4) 0.0961(4) 0.121(2) Uani 1 d . . H1A H 0.2014(4) 0.3184(4) 0.0750(4) 0.080 Uiso 1 d R . C2 C 0.0982(5) 0.2640(5) 0.0752(5) 0.171(4) Uani 1 d . . H2A H 0.0937(5) 0.2335(5) 0.0382(5) 0.080 Uiso 1 d R . C3 C 0.0429(4) 0.2587(5) 0.1078(6) 0.152(4) Uani 1 d . . H3A H -0.0006(4) 0.2244(5) 0.0933(6) 0.080 Uiso 1 d R . C4 C 0.0485(4) 0.3012(5) 0.1591(5) 0.133(3) Uani 1 d . . H4A H 0.0087(4) 0.2956(5) 0.1814(5) 0.080 Uiso 1 d R . C5 C 0.1098(3) 0.3504(4) 0.1803(4) 0.104(2) Uani 1 d . . H5A H 0.1142(3) 0.3815(4) 0.2165(4) 0.080 Uiso 1 d R . C6 C 0.1672(3) 0.3572(3) 0.1490(3) 0.0808(14) Uani 1 d . . C7 C 0.2384(3) 0.5340(3) 0.1593(3) 0.094(2) Uani 1 d . . H7A H 0.2449(3) 0.5293(3) 0.1097(3) 0.080 Uiso 1 d R . C8 C 0.2294(3) 0.5846(3) 0.1822(5) 0.111(2) Uani 1 d . . H8A H 0.2289(3) 0.6155(3) 0.1486(5) 0.080 Uiso 1 d R . C9 C 0.2211(3) 0.5918(3) 0.2541(5) 0.112(2) Uani 1 d . . H9A H 0.2144(3) 0.6274(3) 0.2699(5) 0.080 Uiso 1 d R . C10 C 0.2218(4) 0.5478(3) 0.3017(4) 0.107(2) Uani 1 d . . H10A H 0.2157(4) 0.5529(3) 0.3513(4) 0.080 Uiso 1 d R . C11 C 0.2302(3) 0.4956(3) 0.2792(3) 0.088(2) Uani 1 d . . H11A H 0.2313(3) 0.4651(3) 0.3130(3) 0.080 Uiso 1 d R . C12 C 0.2390(2) 0.4884(3) 0.2083(3) 0.0728(12) Uani 1 d . . C13 C 0.2729(2) 0.3908(2) 0.2511(2) 0.0689(11) Uani 1 d . . C14 C 0.2297(3) 0.3322(3) 0.2857(3) 0.0848(14) Uani 1 d . . H14A H 0.1847(3) 0.3053(3) 0.2692(3) 0.080 Uiso 1 d R . Cl1 Cl 0.26602(7) 0.38609(8) -0.07115(7) 0.0882(4) Uani 1 d . . O1 O 0.2674(3) 0.4460(3) -0.0503(3) 0.131(2) Uani 1 d . . O2 O 0.2006(3) 0.3343(4) -0.0739(3) 0.164(2) Uani 1 d . . O3 O 0.3019(2) 0.3711(3) -0.0197(2) 0.1100(14) Uani 1 d . . O4 O 0.2949(3) 0.3937(3) -0.1390(2) 0.119(2) Uani 1 d . . N1 N 0.3369(2) 0.4301(2) 0.2713(2) 0.0699(10) Uani 1 d . . N2 N 0.4248(2) 0.4536(2) 0.3459(2) 0.0737(10) Uani 1 d . . N3 N 0.4566(2) 0.4351(2) 0.3926(2) 0.0720(10) Uani 1 d . . N4 N 0.5518(2) 0.4219(2) 0.4659(2) 0.0824(12) Uani 1 d . . C15 C 0.2536(3) 0.3137(3) 0.3440(3) 0.095(2) Uani 1 d . . H15A H 0.2250(3) 0.2732(3) 0.3691(3) 0.080 Uiso 1 d R . C16 C 0.3196(3) 0.3536(3) 0.3656(3) 0.0809(14) Uani 1 d . . H16A H 0.3377(3) 0.3427(3) 0.4060(3) 0.080 Uiso 1 d R . C17 C 0.3577(2) 0.4107(2) 0.3270(2) 0.0677(11) Uani 1 d . . C18 C 0.4652(3) 0.5178(3) 0.3252(4) 0.104(2) Uani 1 d . . H18A H 0.4531(3) 0.5421(3) 0.2929(4) 0.080 Uiso 1 d R . C19 C 0.5235(3) 0.5404(3) 0.3585(4) 0.107(2) Uani 1 d . . H19A H 0.5623(3) 0.5839(3) 0.3548(4) 0.080 Uiso 1 d R . C20 C 0.5172(3) 0.4877(3) 0.4004(3) 0.0773(13) Uani 1 d . . C21 C 0.5664(3) 0.4829(3) 0.4456(3) 0.0791(14) Uani 1 d . . C22 C 0.6256(3) 0.5395(3) 0.4661(3) 0.096(2) Uani 1 d . . H22A H 0.6352(3) 0.5826(3) 0.4497(3) 0.080 Uiso 1 d R . C23 C 0.6707(3) 0.5323(4) 0.5076(4) 0.109(2) Uani 1 d . . H23A H 0.7123(3) 0.5701(4) 0.5215(4) 0.080 Uiso 1 d R . C24 C 0.6541(3) 0.4700(5) 0.5302(3) 0.109(2) Uani 1 d . . H24A H 0.6837(3) 0.4645(5) 0.5614(3) 0.080 Uiso 1 d R . C25 C 0.5953(3) 0.4165(4) 0.5082(3) 0.098(2) Uani 1 d . . H25A H 0.5848(3) 0.3727(4) 0.5232(3) 0.080 Uiso 1 d 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 0.0754(3) 0.0902(3) 0.0763(3) 0.0083(2) 0.0083(2) 0.0389(2) P1 0.0680(8) 0.0766(8) 0.0703(7) 0.0054(6) 0.0033(6) 0.0333(6) C1 0.094(5) 0.117(5) 0.117(5) -0.029(4) 0.008(4) 0.026(4) C2 0.131(8) 0.156(8) 0.153(8) -0.068(6) -0.018(6) 0.018(7) C3 0.085(5) 0.147(8) 0.159(8) -0.004(7) -0.019(5) 0.008(5) C4 0.080(5) 0.157(8) 0.144(7) -0.012(6) -0.009(4) 0.046(5) C5 0.072(4) 0.118(5) 0.112(5) -0.007(4) -0.004(3) 0.040(4) C6 0.069(3) 0.082(3) 0.081(3) 0.006(3) -0.002(2) 0.030(3) C7 0.091(4) 0.084(4) 0.098(4) 0.011(3) -0.012(3) 0.038(3) C8 0.108(5) 0.085(4) 0.145(6) 0.014(4) -0.024(4) 0.052(4) C9 0.097(5) 0.086(4) 0.166(7) -0.004(4) -0.006(4) 0.056(4) C10 0.124(5) 0.107(5) 0.108(4) 0.005(4) 0.020(4) 0.073(4) C11 0.097(4) 0.092(4) 0.090(3) 0.016(3) 0.019(3) 0.058(3) C12 0.065(3) 0.071(3) 0.081(3) 0.007(2) 0.001(2) 0.034(3) C13 0.070(3) 0.072(3) 0.068(2) 0.003(2) 0.009(2) 0.038(2) C14 0.067(3) 0.085(4) 0.097(4) 0.013(3) 0.000(3) 0.034(3) Cl1 0.0880(9) 0.1119(11) 0.0770(7) -0.0011(7) -0.0039(6) 0.0591(8) O1 0.186(5) 0.148(4) 0.112(3) -0.007(3) 0.003(3) 0.125(4) O2 0.085(3) 0.200(6) 0.156(5) 0.006(4) -0.019(3) 0.034(4) O3 0.128(4) 0.145(4) 0.092(3) -0.016(3) -0.026(2) 0.095(3) O4 0.151(4) 0.154(4) 0.086(3) 0.003(3) 0.014(3) 0.100(4) N1 0.069(2) 0.069(2) 0.076(2) 0.001(2) 0.007(2) 0.037(2) N2 0.069(2) 0.065(2) 0.090(3) -0.002(2) 0.000(2) 0.036(2) N3 0.073(3) 0.070(2) 0.075(2) -0.007(2) -0.003(2) 0.037(2) N4 0.077(3) 0.098(3) 0.066(2) -0.010(2) -0.010(2) 0.039(3) C15 0.088(4) 0.090(4) 0.093(4) 0.025(3) 0.006(3) 0.036(3) C16 0.075(3) 0.088(4) 0.084(3) 0.012(3) 0.001(3) 0.045(3) C17 0.065(3) 0.070(3) 0.074(3) -0.003(2) 0.000(2) 0.038(2) C18 0.098(4) 0.074(4) 0.149(6) 0.014(4) -0.008(4) 0.048(3) C19 0.077(4) 0.068(4) 0.161(6) 0.001(4) -0.013(4) 0.026(3) C20 0.073(3) 0.068(3) 0.091(3) -0.017(3) 0.001(3) 0.035(3) C21 0.074(3) 0.085(4) 0.078(3) -0.023(3) -0.003(2) 0.039(3) C22 0.083(4) 0.091(4) 0.111(4) -0.032(3) -0.005(3) 0.041(3) C23 0.076(4) 0.130(6) 0.113(5) -0.052(5) -0.018(3) 0.044(4) C24 0.088(4) 0.154(7) 0.083(4) -0.025(4) -0.024(3) 0.058(5) C25 0.096(4) 0.116(5) 0.080(3) -0.002(3) -0.011(3) 0.051(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.302(4) 4 ? Ag1 P1 2.3600(14) . ? Ag1 N3 2.399(4) 4 ? P1 C12 1.812(5) . ? P1 C6 1.809(5) . ? P1 C13 1.828(5) . ? C1 C6 1.375(8) . ? C1 C2 1.393(11) . ? C2 C3 1.367(13) . ? C3 C4 1.338(13) . ? C4 C5 1.363(10) . ? C5 C6 1.389(8) . ? C7 C8 1.358(10) . ? C7 C12 1.407(7) . ? C8 C9 1.387(10) . ? C9 C10 1.361(10) . ? C10 C11 1.384(8) . ? C11 C12 1.371(7) . ? C13 N1 1.350(6) . ? C13 C14 1.381(7) . ? C14 C15 1.389(8) . ? Cl1 O2 1.386(6) . ? Cl1 O4 1.410(5) . ? Cl1 O3 1.427(4) . ? Cl1 O1 1.428(5) . ? N1 C17 1.323(6) . ? N2 C18 1.360(7) . ? N2 N3 1.346(6) . ? N2 C17 1.410(6) . ? N3 C20 1.330(7) . ? N3 Ag1 2.399(4) 4 ? N4 C21 1.335(7) . ? N4 C25 1.338(7) . ? N4 Ag1 2.302(4) 4 ? C15 C16 1.396(8) . ? C16 C17 1.373(7) . ? C18 C19 1.335(9) . ? C19 C20 1.398(8) . ? C20 C21 1.469(8) . ? C21 C22 1.397(8) . ? C22 C23 1.378(10) . ? C23 C24 1.363(10) . ? C24 C25 1.370(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 N4 Ag1 P1 144.27(11) 4 . ? N4 Ag1 N3 71.4(2) 4 4 ? P1 Ag1 N3 120.43(10) . 4 ? C12 P1 C6 104.6(3) . . ? C12 P1 C13 103.4(2) . . ? C6 P1 C13 105.5(2) . . ? C12 P1 Ag1 113.1(2) . . ? C6 P1 Ag1 118.1(2) . . ? C13 P1 Ag1 110.9(2) . . ? C6 C1 C2 119.0(8) . . ? C1 C2 C3 120.0(8) . . ? C4 C3 C2 121.0(8) . . ? C5 C4 C3 120.1(8) . . ? C4 C5 C6 120.7(7) . . ? C1 C6 C5 119.1(6) . . ? C1 C6 P1 117.5(5) . . ? C5 C6 P1 123.4(5) . . ? C8 C7 C12 120.3(7) . . ? C9 C8 C7 120.2(6) . . ? C8 C9 C10 119.7(7) . . ? C11 C10 C9 120.9(7) . . ? C12 C11 C10 119.8(5) . . ? C11 C12 C7 119.1(5) . . ? C11 C12 P1 123.7(4) . . ? C7 C12 P1 117.2(4) . . ? N1 C13 C14 122.9(5) . . ? N1 C13 P1 113.2(3) . . ? C14 C13 P1 123.8(4) . . ? C13 C14 C15 117.9(5) . . ? O2 Cl1 O4 108.6(4) . . ? O2 Cl1 O3 109.4(4) . . ? O4 Cl1 O3 110.2(3) . . ? O2 Cl1 O1 109.7(4) . . ? O4 Cl1 O1 110.4(3) . . ? O3 Cl1 O1 108.5(3) . . ? C17 N1 C13 117.2(4) . . ? C18 N2 N3 110.4(4) . . ? C18 N2 C17 127.8(5) . . ? N3 N2 C17 121.7(4) . . ? C20 N3 N2 106.0(4) . . ? C20 N3 Ag1 110.2(3) . 4 ? N2 N3 Ag1 134.9(3) . 4 ? C21 N4 C25 117.7(5) . . ? C21 N4 Ag1 116.4(3) . 4 ? C25 N4 Ag1 125.5(4) . 4 ? C16 C15 C14 120.0(5) . . ? C17 C16 C15 116.6(5) . . ? N1 C17 C16 125.3(5) . . ? N1 C17 N2 114.9(4) . . ? C16 C17 N2 119.8(4) . . ? N2 C18 C19 107.6(6) . . ? C18 C19 C20 106.1(6) . . ? N3 C20 C19 109.8(5) . . ? N3 C20 C21 119.9(5) . . ? C19 C20 C21 130.2(5) . . ? N4 C21 C22 121.7(5) . . ? N4 C21 C20 116.8(5) . . ? C22 C21 C20 121.6(6) . . ? C21 C22 C23 119.4(7) . . ? C24 C23 C22 118.3(6) . . ? C23 C24 C25 119.5(7) . . ? N4 C25 C24 123.3(7) . . ? _refine_diff_density_max 0.837 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.216 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H38 Ag2 Cl2 N8 O8 P2' _chemical_formula_weight 1155.40 _chemical_melting_point ? _chemical_compound_source Synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting P2(1)/c _symmetry_space_group_name_H-M monoclinic 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 9.6630(10) _cell_length_b 11.5570(10) _cell_length_c 21.344(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.88 _cell_angle_gamma 90.00 _cell_volume 2348.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 52 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method ? _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type PSI _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.835 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 38min. _diffrn_standards_decay_% 0 _diffrn_reflns_number 6979 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5409 _reflns_number_observed 3726 _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 'SIEMENS SHELXTL PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 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^)+(0.0738P)^2^+11.1106P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5401 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_obs 0.0550 _refine_ls_wR_factor_all 0.1614 _refine_ls_wR_factor_obs 0.1281 _refine_ls_goodness_of_fit_all 1.114 _refine_ls_goodness_of_fit_obs 1.363 _refine_ls_restrained_S_all 1.170 _refine_ls_restrained_S_obs 1.363 _refine_ls_shift/esd_max -0.003 _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 0.41485(6) 0.09646(5) 0.01892(3) 0.0438(2) Uani 1 d . . P1 P 0.4794(2) -0.18211(14) 0.06236(7) 0.0317(4) Uani 1 d . . Cl1 Cl 0.2050(3) 0.6279(3) 0.28412(11) 0.0739(7) Uani 1 d . . O1 O 0.3162(13) 0.6962(13) 0.3177(7) 0.183(6) Uani 1 d . . O2 O 0.0792(12) 0.6714(14) 0.2976(6) 0.184(6) Uani 1 d . . O3 O 0.2123(18) 0.6337(11) 0.2229(5) 0.184(6) Uani 1 d . . O4 O 0.2296(17) 0.5195(12) 0.3104(9) 0.242(9) Uani 1 d . . N1 N 0.3625(7) 0.2408(5) 0.0926(3) 0.0475(15) Uani 1 d . . N2 N 0.3410(6) 0.1944(5) 0.1482(3) 0.0417(13) Uani 1 d . . N3 N 0.4135(5) 0.0131(4) 0.1179(2) 0.0318(11) Uani 1 d . . N4 N 0.1712(8) 0.0634(8) -0.0253(4) 0.076(2) Uani 1 d . . C1 C 0.3165(9) 0.3476(7) 0.0934(4) 0.056(2) Uani 1 d . . H1B H 0.3187(9) 0.4022(7) 0.0598(4) 0.080 Uiso 1 d R . C2 C 0.2660(11) 0.3720(8) 0.1481(4) 0.069(3) Uani 1 d . . H2B H 0.2269(11) 0.4438(8) 0.1595(4) 0.080 Uiso 1 d R . C3 C 0.2815(10) 0.2737(8) 0.1822(4) 0.066(2) Uani 1 d . . H3A H 0.2556(10) 0.2611(8) 0.2231(4) 0.080 Uiso 1 d R . C4 C 0.3785(7) 0.0788(6) 0.1641(3) 0.040(2) Uani 1 d . . C5 C 0.3771(10) 0.0382(7) 0.2250(4) 0.055(2) Uani 1 d . . H5A H 0.3526(10) 0.0887(7) 0.2571(4) 0.080 Uiso 1 d R . C6 C 0.4101(10) -0.0760(7) 0.2377(3) 0.059(2) Uani 1 d . . H6A H 0.4086(10) -0.1079(7) 0.2791(3) 0.080 Uiso 1 d R . C7 C 0.4447(8) -0.1460(7) 0.1901(3) 0.047(2) Uani 1 d . . H7A H 0.4679(8) -0.2260(7) 0.1978(3) 0.080 Uiso 1 d R . C8 C 0.4466(7) -0.0978(6) 0.1312(3) 0.0343(13) Uani 1 d . . C9 C 0.7234(8) -0.2655(7) 0.1355(3) 0.048(2) Uani 1 d . . H9A H 0.7417(8) -0.1861(7) 0.1472(3) 0.080 Uiso 1 d R . C10 C 0.8229(9) -0.3504(9) 0.1571(4) 0.064(2) Uani 1 d . . H10A H 0.9098(9) -0.3295(9) 0.1837(4) 0.080 Uiso 1 d R . C11 C 0.7969(11) -0.4644(9) 0.1404(5) 0.072(3) Uani 1 d . . H11A H 0.8654(11) -0.5228(9) 0.1552(5) 0.080 Uiso 1 d R . C12 C 0.6740(11) -0.4950(8) 0.1027(5) 0.069(3) Uani 1 d . . H12A H 0.6558(11) -0.5747(8) 0.0917(5) 0.080 Uiso 1 d R . C13 C 0.5747(9) -0.4117(7) 0.0805(4) 0.053(2) Uani 1 d . . H13A H 0.4891(9) -0.4341(7) 0.0535(4) 0.080 Uiso 1 d R . C14 C 0.5977(7) -0.2960(6) 0.0970(3) 0.0384(15) Uani 1 d . . C15 C 0.2433(8) -0.3156(7) 0.0766(4) 0.049(2) Uani 1 d . . H15A H 0.2893(8) -0.3291(7) 0.1196(4) 0.080 Uiso 1 d R . C16 C 0.1115(9) -0.3600(8) 0.0557(5) 0.065(2) Uani 1 d . . H16A H 0.0655(9) -0.4047(8) 0.0840(5) 0.080 Uiso 1 d R . C17 C 0.0457(9) -0.3396(9) -0.0059(5) 0.072(3) Uani 1 d . . H17A H -0.0461(9) -0.3712(9) -0.0202(5) 0.080 Uiso 1 d R . C18 C 0.1094(10) -0.2753(8) -0.0467(5) 0.067(2) Uani 1 d . . H18A H 0.0621(10) -0.2610(8) -0.0893(5) 0.080 Uiso 1 d R . C19 C 0.2433(8) -0.2311(6) -0.0256(4) 0.048(2) Uani 1 d . . H19A H 0.2893(8) -0.1871(6) -0.0542(4) 0.080 Uiso 1 d R . C20 C 0.3098(7) -0.2498(6) 0.0355(3) 0.0375(14) Uani 1 d . . C21 C 0.0761(9) 0.0586(8) -0.0639(5) 0.063(2) Uani 1 d . . C22 C -0.0468(11) 0.0496(12) -0.1126(6) 0.096(4) 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 0.0510(3) 0.0434(3) 0.0423(3) 0.0093(2) 0.0227(2) 0.0038(3) P1 0.0373(9) 0.0295(8) 0.0300(8) 0.0013(6) 0.0105(6) -0.0008(7) Cl1 0.077(2) 0.090(2) 0.0564(13) 0.0086(12) 0.0158(11) 0.0090(14) O1 0.137(10) 0.201(14) 0.192(13) 0.009(11) -0.028(9) -0.046(10) O2 0.140(10) 0.275(17) 0.135(9) -0.031(10) 0.020(8) 0.095(11) O3 0.323(19) 0.164(11) 0.085(7) 0.001(7) 0.093(9) 0.007(11) O4 0.251(17) 0.159(12) 0.356(22) 0.164(14) 0.166(16) 0.066(12) N1 0.060(4) 0.034(3) 0.052(4) 0.002(3) 0.019(3) -0.002(3) N2 0.051(3) 0.036(3) 0.039(3) -0.009(2) 0.009(3) 0.002(3) N3 0.035(3) 0.031(3) 0.030(3) -0.003(2) 0.007(2) -0.004(2) N4 0.049(4) 0.078(6) 0.100(7) 0.003(5) 0.011(4) -0.007(4) C1 0.068(5) 0.035(4) 0.063(5) 0.001(4) 0.009(4) 0.002(4) C2 0.095(7) 0.046(5) 0.063(5) -0.012(4) 0.004(5) 0.019(5) C3 0.092(7) 0.058(5) 0.047(4) -0.017(4) 0.016(4) 0.022(5) C4 0.045(4) 0.040(4) 0.037(3) -0.002(3) 0.008(3) 0.001(3) C5 0.081(6) 0.047(4) 0.039(4) -0.009(3) 0.021(4) 0.004(4) C6 0.090(6) 0.059(5) 0.030(3) 0.007(3) 0.018(4) 0.002(5) C7 0.065(5) 0.041(4) 0.036(3) 0.002(3) 0.012(3) 0.000(4) C8 0.039(3) 0.034(3) 0.031(3) -0.002(3) 0.009(3) 0.000(3) C9 0.047(4) 0.056(5) 0.043(4) 0.011(3) 0.010(3) -0.001(4) C10 0.038(4) 0.096(7) 0.058(5) 0.020(5) 0.010(4) 0.011(5) C11 0.070(6) 0.073(7) 0.081(6) 0.026(5) 0.030(5) 0.037(5) C12 0.081(7) 0.045(5) 0.084(7) 0.004(4) 0.026(6) 0.024(5) C13 0.062(5) 0.040(4) 0.060(5) -0.002(4) 0.017(4) 0.005(4) C14 0.040(4) 0.039(4) 0.040(3) 0.006(3) 0.018(3) 0.001(3) C15 0.047(4) 0.050(4) 0.054(4) 0.000(4) 0.015(3) -0.007(4) C16 0.049(5) 0.060(5) 0.088(7) 0.001(5) 0.020(5) -0.015(4) C17 0.043(5) 0.068(6) 0.099(8) -0.013(6) -0.007(5) -0.014(4) C18 0.065(6) 0.060(5) 0.065(6) -0.010(4) -0.017(5) 0.001(5) C19 0.055(5) 0.041(4) 0.046(4) -0.004(3) 0.006(3) -0.001(3) C20 0.038(3) 0.034(3) 0.042(4) -0.004(3) 0.012(3) 0.002(3) C21 0.034(4) 0.069(6) 0.086(6) -0.005(5) 0.012(4) -0.001(4) C22 0.051(6) 0.129(11) 0.102(9) -0.033(8) -0.002(5) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.324(5) . ? Ag1 P1 2.375(2) 3_655 ? Ag1 N1 2.405(6) . ? Ag1 N4 2.412(8) . ? Ag1 Ag1 2.9643(11) 3_655 ? P1 C14 1.816(7) . ? P1 C20 1.817(7) . ? P1 C8 1.836(6) . ? P1 Ag1 2.375(2) 3_655 ? Cl1 O3 1.323(10) . ? Cl1 O4 1.376(11) . ? Cl1 O2 1.390(11) . ? Cl1 O1 1.424(12) . ? N1 C1 1.313(10) . ? N1 N2 1.350(8) . ? N2 C3 1.357(9) . ? N2 C4 1.410(9) . ? N3 C4 1.333(8) . ? N3 C8 1.340(8) . ? N4 C21 1.126(11) . ? C1 C2 1.369(12) . ? C2 C3 1.343(12) . ? C4 C5 1.385(10) . ? C5 C6 1.373(11) . ? C6 C7 1.384(11) . ? C7 C8 1.376(9) . ? C9 C14 1.390(10) . ? C9 C10 1.396(11) . ? C10 C11 1.376(15) . ? C11 C12 1.362(14) . ? C12 C13 1.384(11) . ? C13 C14 1.390(10) . ? C15 C16 1.375(11) . ? C15 C20 1.398(10) . ? C16 C17 1.378(14) . ? C17 C18 1.369(14) . ? C18 C19 1.392(11) . ? C19 C20 1.369(10) . ? C21 C22 1.441(14) . ? 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 N3 Ag1 P1 155.08(14) . 3_655 ? N3 Ag1 N1 70.0(2) . . ? P1 Ag1 N1 110.72(15) 3_655 . ? N3 Ag1 N4 97.6(3) . . ? P1 Ag1 N4 107.1(2) 3_655 . ? N1 Ag1 N4 93.7(3) . . ? N3 Ag1 Ag1 91.49(13) . 3_655 ? P1 Ag1 Ag1 77.64(5) 3_655 3_655 ? N1 Ag1 Ag1 152.7(2) . 3_655 ? N4 Ag1 Ag1 108.9(2) . 3_655 ? C14 P1 C20 106.7(3) . . ? C14 P1 C8 104.0(3) . . ? C20 P1 C8 102.2(3) . . ? C14 P1 Ag1 106.2(2) . 3_655 ? C20 P1 Ag1 115.3(2) . 3_655 ? C8 P1 Ag1 121.2(2) . 3_655 ? O3 Cl1 O4 114.4(10) . . ? O3 Cl1 O2 112.6(9) . . ? O4 Cl1 O2 109.9(9) . . ? O3 Cl1 O1 107.8(9) . . ? O4 Cl1 O1 103.7(11) . . ? O2 Cl1 O1 107.8(9) . . ? C1 N1 N2 105.0(6) . . ? C1 N1 Ag1 140.4(6) . . ? N2 N1 Ag1 112.4(4) . . ? N1 N2 C3 110.1(6) . . ? N1 N2 C4 121.1(5) . . ? C3 N2 C4 128.8(7) . . ? C4 N3 C8 118.0(5) . . ? C4 N3 Ag1 118.6(4) . . ? C8 N3 Ag1 123.4(4) . . ? C21 N4 Ag1 156.0(8) . . ? N1 C1 C2 112.1(8) . . ? C3 C2 C1 105.3(8) . . ? C2 C3 N2 107.5(8) . . ? N3 C4 C5 123.1(7) . . ? N3 C4 N2 116.6(6) . . ? C5 C4 N2 120.3(6) . . ? C6 C5 C4 118.1(7) . . ? C5 C6 C7 119.6(7) . . ? C8 C7 C6 118.5(7) . . ? N3 C8 C7 122.7(6) . . ? N3 C8 P1 113.9(4) . . ? C7 C8 P1 123.2(5) . . ? C14 C9 C10 120.0(8) . . ? C11 C10 C9 120.2(9) . . ? C12 C11 C10 120.2(8) . . ? C11 C12 C13 120.3(9) . . ? C12 C13 C14 120.7(8) . . ? C13 C14 C9 118.6(7) . . ? C13 C14 P1 122.1(6) . . ? C9 C14 P1 118.8(6) . . ? C16 C15 C20 119.9(8) . . ? C15 C16 C17 119.8(9) . . ? C18 C17 C16 121.0(8) . . ? C17 C18 C19 119.2(8) . . ? C20 C19 C18 120.5(8) . . ? C19 C20 C15 119.5(7) . . ? C19 C20 P1 118.9(5) . . ? C15 C20 P1 121.5(6) . . ? N4 C21 C22 178.4(12) . . ? _refine_diff_density_max 0.721 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.109