# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Ag4 O8 P2' _chemical_formula_weight 779.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 8.2461(11) _cell_length_b 28.040(4) _cell_length_c 8.1257(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.276(3) _cell_angle_gamma 90.00 _cell_volume 1859.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.360 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.774 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26236 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4425 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2(Bruker,2003) _computing_cell_refinement SAINT(Bruker,2001) _computing_data_reduction APEX2(Bruker,2003) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.9683P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4425 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.69369(4) 0.501480(13) 0.06409(4) 0.04097(11) Uani 1 1 d . . . Ag2 Ag 0.93552(4) 0.461294(12) -0.19897(4) 0.03694(10) Uani 1 1 d . . . Ag3 Ag 0.80289(4) 0.497728(12) 0.44356(4) 0.03850(11) Uani 1 1 d . . . Ag4 Ag 0.43172(4) 0.456884(12) 0.28376(4) 0.03631(10) Uani 1 1 d . . . P1 P 0.50929(10) 0.56769(3) 0.29632(10) 0.02407(19) Uani 1 1 d . . . P2 P 0.98059(10) 0.42972(3) 0.20853(10) 0.02460(19) Uani 1 1 d . . . O1 O 0.5700(3) 0.56523(11) 0.1284(3) 0.0375(6) Uani 1 1 d . . . O2 O 0.6505(3) 0.56160(9) 0.4391(3) 0.0296(5) Uani 1 1 d . . . O3 O 0.3688(3) 0.53353(10) 0.3116(4) 0.0348(6) Uani 1 1 d . . . O4 O 0.9379(4) 0.43561(11) 0.3834(3) 0.0401(7) Uani 1 1 d . . . O5 O 1.1230(3) 0.46151(9) 0.1764(4) 0.0348(6) Uani 1 1 d . . . O6 O 0.8323(3) 0.43564(10) 0.0736(3) 0.0332(6) Uani 1 1 d . . . OW1 O 1.0694(4) 0.39867(13) -0.2683(5) 0.0583(9) Uani 1 1 d . . . OW2 O 0.5390(4) 0.39247(13) 0.1934(4) 0.0521(8) Uani 1 1 d . . . C1 C 0.4309(4) 0.62756(13) 0.3135(4) 0.0279(7) Uani 1 1 d . . . C2 C 0.3106(4) 0.63709(15) 0.4123(5) 0.0367(9) Uani 1 1 d . . . H2 H 0.2693 0.6123 0.4698 0.044 Uiso 1 1 calc R . . C3 C 0.2511(6) 0.68269(17) 0.4269(6) 0.0524(12) Uani 1 1 d . . . H3 H 0.1707 0.6885 0.4937 0.063 Uiso 1 1 calc R . . C4 C 0.3120(6) 0.71979(16) 0.3413(7) 0.0576(13) Uani 1 1 d . . . H4 H 0.2720 0.7506 0.3500 0.069 Uiso 1 1 calc R . . C5 C 0.4299(6) 0.71118(17) 0.2450(7) 0.0543(12) Uani 1 1 d . . . H5 H 0.4708 0.7362 0.1882 0.065 Uiso 1 1 calc R . . C6 C 0.4901(5) 0.66576(15) 0.2302(5) 0.0424(10) Uani 1 1 d . . . H6 H 0.5713 0.6606 0.1637 0.051 Uiso 1 1 calc R . . C7 C 1.0468(4) 0.36847(14) 0.1951(4) 0.0272(7) Uani 1 1 d . . . C8 C 0.9756(5) 0.33809(14) 0.0694(5) 0.0377(9) Uani 1 1 d . . . H8 H 0.8885 0.3488 -0.0072 0.045 Uiso 1 1 calc R . . C9 C 1.0338(6) 0.29201(16) 0.0579(6) 0.0512(11) Uani 1 1 d . . . H9 H 0.9877 0.2723 -0.0284 0.061 Uiso 1 1 calc R . . C10 C 1.1593(6) 0.27523(17) 0.1735(7) 0.0560(12) Uani 1 1 d . . . H10 H 1.1970 0.2442 0.1659 0.067 Uiso 1 1 calc R . . C11 C 1.1750(4) 0.35103(14) 0.3115(5) 0.0361(8) Uani 1 1 d . . . H11 H 1.2240 0.3707 0.3964 0.043 Uiso 1 1 calc R . . C12 C 1.2288(5) 0.30451(16) 0.3004(6) 0.0493(11) Uani 1 1 d . . . H12 H 1.3126 0.2930 0.3793 0.059 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 0.03861(19) 0.0501(2) 0.03424(18) 0.00043(13) 0.00541(13) 0.01795(13) Ag2 0.03549(18) 0.0425(2) 0.03406(17) 0.00343(12) 0.00915(12) 0.01082(12) Ag3 0.03844(18) 0.0439(2) 0.03405(18) 0.00291(12) 0.00814(13) 0.01603(13) Ag4 0.03686(18) 0.0410(2) 0.03272(16) 0.00138(12) 0.01053(12) 0.01059(12) P1 0.0218(4) 0.0288(5) 0.0216(4) 0.0012(3) 0.0031(3) 0.0042(3) P2 0.0212(4) 0.0308(5) 0.0225(4) 0.0015(3) 0.0053(3) 0.0044(3) O1 0.0468(15) 0.0460(17) 0.0220(12) 0.0064(11) 0.0121(11) 0.0187(13) O2 0.0255(12) 0.0358(15) 0.0261(12) 0.0004(10) -0.0011(9) 0.0054(10) O3 0.0209(12) 0.0313(15) 0.0517(16) 0.0025(12) 0.0039(11) -0.0006(10) O4 0.0517(17) 0.0455(17) 0.0258(13) 0.0058(12) 0.0148(12) 0.0195(13) O5 0.0227(12) 0.0313(15) 0.0511(16) 0.0051(12) 0.0072(11) -0.0005(10) O6 0.0259(12) 0.0396(16) 0.0328(13) -0.0006(11) 0.0001(10) 0.0056(11) OW1 0.0480(18) 0.053(2) 0.079(2) 0.0086(18) 0.0253(17) 0.0109(15) OW2 0.0571(19) 0.051(2) 0.0507(19) 0.0000(15) 0.0156(15) 0.0073(15) C1 0.0257(16) 0.0274(19) 0.0295(17) 0.0006(14) 0.0003(13) 0.0022(14) C2 0.038(2) 0.032(2) 0.041(2) -0.0025(16) 0.0084(16) 0.0018(16) C3 0.050(3) 0.049(3) 0.061(3) -0.010(2) 0.016(2) 0.013(2) C4 0.061(3) 0.026(2) 0.082(4) -0.004(2) -0.001(3) 0.010(2) C5 0.053(3) 0.034(2) 0.075(3) 0.013(2) 0.004(2) -0.008(2) C6 0.039(2) 0.039(2) 0.050(2) 0.0057(19) 0.0074(18) -0.0053(18) C7 0.0247(16) 0.0293(19) 0.0297(17) -0.0009(14) 0.0106(13) -0.0012(14) C8 0.039(2) 0.036(2) 0.038(2) 0.0003(17) 0.0051(16) -0.0036(17) C9 0.062(3) 0.036(2) 0.056(3) -0.011(2) 0.008(2) -0.007(2) C10 0.070(3) 0.029(2) 0.071(3) -0.003(2) 0.016(3) 0.008(2) C11 0.0318(18) 0.038(2) 0.038(2) 0.0014(17) 0.0043(15) 0.0052(16) C12 0.050(2) 0.043(3) 0.054(3) 0.005(2) 0.003(2) 0.015(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 2.159(3) . ? Ag1 O6 2.167(3) . ? Ag1 Ag3 3.0871(6) . ? Ag1 Ag4 3.0952(5) 3_665 ? Ag1 Ag1 3.2152(7) 3_665 ? Ag1 Ag4 3.2444(5) . ? Ag1 Ag2 3.2673(6) 3_765 ? Ag1 Ag2 3.3231(5) . ? Ag2 OW1 2.191(3) . ? Ag2 O5 2.231(3) 3_765 ? Ag2 O3 2.548(2) 3_665 ? Ag2 O6 2.586(3) . ? Ag2 Ag3 3.1245(5) 1_554 ? Ag2 Ag1 3.2673(6) 3_765 ? Ag2 Ag3 3.3403(5) 3_765 ? Ag3 O4 2.161(3) . ? Ag3 O2 2.185(2) . ? Ag3 Ag2 3.1245(5) 1_556 ? Ag3 Ag3 3.2506(7) 3_766 ? Ag3 Ag2 3.3403(5) 3_765 ? Ag3 Ag4 3.3498(6) . ? Ag4 OW2 2.184(3) . ? Ag4 O3 2.230(3) . ? Ag4 O2 2.498(2) 3_666 ? Ag4 O5 2.573(3) 1_455 ? Ag4 Ag1 3.0952(5) 3_665 ? P1 O1 1.521(3) . ? P1 O3 1.522(3) . ? P1 O2 1.531(2) . ? P1 C1 1.812(4) . ? P2 O4 1.521(3) . ? P2 O5 1.527(3) . ? P2 O6 1.530(2) . ? P2 C7 1.810(4) . ? O2 Ag4 2.498(2) 3_666 ? O3 Ag2 2.548(2) 3_665 ? O5 Ag2 2.231(3) 3_765 ? O5 Ag4 2.573(3) 1_655 ? C1 C2 1.389(5) . ? C1 C6 1.392(5) . ? C2 C3 1.381(6) . ? C3 C4 1.385(7) . ? C4 C5 1.354(7) . ? C5 C6 1.379(6) . ? C7 C8 1.393(5) . ? C7 C11 1.401(5) . ? C8 C9 1.386(6) . ? C9 C10 1.376(7) . ? C10 C12 1.377(7) . ? C11 C12 1.385(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 O1 Ag1 O6 164.14(9) . . ? O1 Ag1 Ag3 82.34(7) . . ? O6 Ag1 Ag3 81.89(7) . . ? O1 Ag1 Ag4 78.54(7) . 3_665 ? O6 Ag1 Ag4 117.32(7) . 3_665 ? Ag3 Ag1 Ag4 159.399(17) . 3_665 ? O1 Ag1 Ag1 67.54(8) . 3_665 ? O6 Ag1 Ag1 118.93(7) . 3_665 ? Ag3 Ag1 Ag1 117.133(17) . 3_665 ? Ag4 Ag1 Ag1 61.845(11) 3_665 3_665 ? O1 Ag1 Ag4 79.10(8) . . ? O6 Ag1 Ag4 92.38(7) . . ? Ag3 Ag1 Ag4 63.829(13) . . ? Ag4 Ag1 Ag4 119.104(13) 3_665 . ? Ag1 Ag1 Ag4 57.259(14) 3_665 . ? O1 Ag1 Ag2 96.09(8) . 3_765 ? O6 Ag1 Ag2 78.29(7) . 3_765 ? Ag3 Ag1 Ag2 63.352(11) . 3_765 ? Ag4 Ag1 Ag2 111.061(15) 3_665 3_765 ? Ag1 Ag1 Ag2 162.758(19) 3_665 3_765 ? Ag4 Ag1 Ag2 127.131(14) . 3_765 ? O1 Ag1 Ag2 141.67(7) . . ? O6 Ag1 Ag2 51.07(7) . . ? Ag3 Ag1 Ag2 121.007(14) . . ? Ag4 Ag1 Ag2 72.123(13) 3_665 . ? Ag1 Ag1 Ag2 116.300(17) 3_665 . ? Ag4 Ag1 Ag2 137.048(16) . . ? Ag2 Ag1 Ag2 72.833(14) 3_765 . ? OW1 Ag2 O5 157.20(11) . 3_765 ? OW1 Ag2 O3 117.38(11) . 3_665 ? O5 Ag2 O3 76.15(9) 3_765 3_665 ? OW1 Ag2 O6 103.74(11) . . ? O5 Ag2 O6 95.61(10) 3_765 . ? O3 Ag2 O6 83.96(8) 3_665 . ? OW1 Ag2 Ag3 98.32(10) . 1_554 ? O5 Ag2 Ag3 73.04(8) 3_765 1_554 ? O3 Ag2 Ag3 56.82(7) 3_665 1_554 ? O6 Ag2 Ag3 140.59(5) . 1_554 ? OW1 Ag2 Ag1 81.98(9) . 3_765 ? O5 Ag2 Ag1 82.28(7) 3_765 3_765 ? O3 Ag2 Ag1 158.10(6) 3_665 3_765 ? O6 Ag2 Ag1 102.07(5) . 3_765 ? Ag3 Ag2 Ag1 113.131(14) 1_554 3_765 ? OW1 Ag2 Ag1 143.96(9) . . ? O5 Ag2 Ag1 57.40(7) 3_765 . ? O3 Ag2 Ag1 63.93(7) 3_665 . ? O6 Ag2 Ag1 40.67(6) . . ? Ag3 Ag2 Ag1 108.964(14) 1_554 . ? Ag1 Ag2 Ag1 107.167(14) 3_765 . ? OW1 Ag2 Ag3 74.35(9) . 3_765 ? O5 Ag2 Ag3 83.17(7) 3_765 3_765 ? O3 Ag2 Ag3 116.98(7) 3_665 3_765 ? O6 Ag2 Ag3 157.75(5) . 3_765 ? Ag3 Ag2 Ag3 60.264(13) 1_554 3_765 ? Ag1 Ag2 Ag3 55.694(12) 3_765 3_765 ? Ag1 Ag2 Ag3 139.890(16) . 3_765 ? O4 Ag3 O2 166.10(9) . . ? O4 Ag3 Ag1 83.52(7) . . ? O2 Ag3 Ag1 82.59(6) . . ? O4 Ag3 Ag2 79.86(7) . 1_556 ? O2 Ag3 Ag2 114.01(6) . 1_556 ? Ag1 Ag3 Ag2 162.257(16) . 1_556 ? O4 Ag3 Ag3 64.45(9) . 3_766 ? O2 Ag3 Ag3 121.46(7) . 3_766 ? Ag1 Ag3 Ag3 114.619(16) . 3_766 ? Ag2 Ag3 Ag3 63.160(11) 1_556 3_766 ? O4 Ag3 Ag2 75.22(8) . 3_765 ? O2 Ag3 Ag2 97.31(7) . 3_765 ? Ag1 Ag3 Ag2 60.955(13) . 3_765 ? Ag2 Ag3 Ag2 119.736(13) 1_556 3_765 ? Ag3 Ag3 Ag2 56.577(13) 3_766 3_765 ? O4 Ag3 Ag4 96.22(9) . . ? O2 Ag3 Ag4 77.45(6) . . ? Ag1 Ag3 Ag4 60.370(11) . . ? Ag2 Ag3 Ag4 115.251(14) 1_556 . ? Ag3 Ag3 Ag4 160.663(18) 3_766 . ? Ag2 Ag3 Ag4 121.281(14) 3_765 . ? OW2 Ag4 O3 160.47(11) . . ? OW2 Ag4 O2 107.88(10) . 3_666 ? O3 Ag4 O2 90.64(10) . 3_666 ? OW2 Ag4 O5 110.89(11) . 1_455 ? O3 Ag4 O5 75.66(9) . 1_455 ? O2 Ag4 O5 86.12(8) 3_666 1_455 ? OW2 Ag4 Ag1 95.92(9) . 3_665 ? O3 Ag4 Ag1 71.15(8) . 3_665 ? O2 Ag4 Ag1 143.43(5) 3_666 3_665 ? O5 Ag4 Ag1 59.15(6) 1_455 3_665 ? OW2 Ag4 Ag1 78.46(9) . . ? O3 Ag4 Ag1 82.38(7) . . ? O2 Ag4 Ag1 149.84(6) 3_666 . ? O5 Ag4 Ag1 119.92(6) 1_455 . ? Ag1 Ag4 Ag1 60.896(13) 3_665 . ? OW2 Ag4 Ag3 91.23(9) . . ? O3 Ag4 Ag3 81.04(6) . . ? O2 Ag4 Ag3 94.18(5) 3_666 . ? O5 Ag4 Ag3 156.70(6) 1_455 . ? Ag1 Ag4 Ag3 113.051(14) 3_665 . ? Ag1 Ag4 Ag3 55.801(12) . . ? O1 P1 O3 113.41(17) . . ? O1 P1 O2 111.23(15) . . ? O3 P1 O2 111.92(16) . . ? O1 P1 C1 106.16(16) . . ? O3 P1 C1 107.02(16) . . ? O2 P1 C1 106.61(15) . . ? O4 P2 O5 112.55(18) . . ? O4 P2 O6 112.90(16) . . ? O5 P2 O6 111.68(16) . . ? O4 P2 C7 105.76(16) . . ? O5 P2 C7 107.31(15) . . ? O6 P2 C7 106.07(16) . . ? P1 O1 Ag1 118.84(15) . . ? P1 O2 Ag3 118.49(14) . . ? P1 O2 Ag4 115.52(13) . 3_666 ? Ag3 O2 Ag4 92.58(9) . 3_666 ? P1 O3 Ag4 114.03(14) . . ? P1 O3 Ag2 131.05(15) . 3_665 ? Ag4 O3 Ag2 104.48(10) . 3_665 ? P2 O4 Ag3 119.67(15) . . ? P2 O5 Ag2 111.81(14) . 3_765 ? P2 O5 Ag4 131.35(15) . 1_655 ? Ag2 O5 Ag4 103.67(10) 3_765 1_655 ? P2 O6 Ag1 118.75(15) . . ? P2 O6 Ag2 108.44(13) . . ? Ag1 O6 Ag2 88.25(9) . . ? C2 C1 C6 117.6(4) . . ? C2 C1 P1 121.0(3) . . ? C6 C1 P1 121.4(3) . . ? C3 C2 C1 121.3(4) . . ? C2 C3 C4 119.6(4) . . ? C5 C4 C3 119.9(4) . . ? C4 C5 C6 120.8(4) . . ? C5 C6 C1 120.8(4) . . ? C8 C7 C11 118.6(4) . . ? C8 C7 P2 121.7(3) . . ? C11 C7 P2 119.7(3) . . ? C9 C8 C7 120.4(4) . . ? C10 C9 C8 120.4(4) . . ? C9 C10 C12 119.9(4) . . ? C12 C11 C7 120.2(4) . . ? C10 C12 C11 120.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ag1 Ag2 OW1 178.0(2) . . . . ? O6 Ag1 Ag2 OW1 11.52(18) . . . . ? Ag3 Ag1 Ag2 OW1 57.33(17) . . . . ? Ag4 Ag1 Ag2 OW1 -140.18(16) 3_665 . . . ? Ag1 Ag1 Ag2 OW1 -95.61(16) 3_665 . . . ? Ag4 Ag1 Ag2 OW1 -26.37(17) . . . . ? Ag2 Ag1 Ag2 OW1 100.16(16) 3_765 . . . ? O1 Ag1 Ag2 O5 9.17(15) . . . 3_765 ? O6 Ag1 Ag2 O5 -157.27(12) . . . 3_765 ? Ag3 Ag1 Ag2 O5 -111.45(8) . . . 3_765 ? Ag4 Ag1 Ag2 O5 51.04(8) 3_665 . . 3_765 ? Ag1 Ag1 Ag2 O5 95.61(8) 3_665 . . 3_765 ? Ag4 Ag1 Ag2 O5 164.84(8) . . . 3_765 ? Ag2 Ag1 Ag2 O5 -68.62(8) 3_765 . . 3_765 ? O1 Ag1 Ag2 O3 -80.64(14) . . . 3_665 ? O6 Ag1 Ag2 O3 112.92(11) . . . 3_665 ? Ag3 Ag1 Ag2 O3 158.74(7) . . . 3_665 ? Ag4 Ag1 Ag2 O3 -38.77(7) 3_665 . . 3_665 ? Ag1 Ag1 Ag2 O3 5.80(7) 3_665 . . 3_665 ? Ag4 Ag1 Ag2 O3 75.03(7) . . . 3_665 ? Ag2 Ag1 Ag2 O3 -158.43(7) 3_765 . . 3_665 ? O1 Ag1 Ag2 O6 166.44(15) . . . . ? Ag3 Ag1 Ag2 O6 45.82(9) . . . . ? Ag4 Ag1 Ag2 O6 -151.69(9) 3_665 . . . ? Ag1 Ag1 Ag2 O6 -107.13(9) 3_665 . . . ? Ag4 Ag1 Ag2 O6 -37.89(9) . . . . ? Ag2 Ag1 Ag2 O6 88.65(9) 3_765 . . . ? O1 Ag1 Ag2 Ag3 -44.96(13) . . . 1_554 ? O6 Ag1 Ag2 Ag3 148.61(9) . . . 1_554 ? Ag3 Ag1 Ag2 Ag3 -165.58(2) . . . 1_554 ? Ag4 Ag1 Ag2 Ag3 -3.086(12) 3_665 . . 1_554 ? Ag1 Ag1 Ag2 Ag3 41.48(2) 3_665 . . 1_554 ? Ag4 Ag1 Ag2 Ag3 110.72(2) . . . 1_554 ? Ag2 Ag1 Ag2 Ag3 -122.745(18) 3_765 . . 1_554 ? O1 Ag1 Ag2 Ag1 77.79(13) . . . 3_765 ? O6 Ag1 Ag2 Ag1 -88.65(8) . . . 3_765 ? Ag3 Ag1 Ag2 Ag1 -42.831(18) . . . 3_765 ? Ag4 Ag1 Ag2 Ag1 119.659(17) 3_665 . . 3_765 ? Ag1 Ag1 Ag2 Ag1 164.22(2) 3_665 . . 3_765 ? Ag4 Ag1 Ag2 Ag1 -126.539(19) . . . 3_765 ? Ag2 Ag1 Ag2 Ag1 0.0 3_765 . . 3_765 ? O1 Ag1 Ag2 Ag3 21.08(13) . . . 3_765 ? O6 Ag1 Ag2 Ag3 -145.36(9) . . . 3_765 ? Ag3 Ag1 Ag2 Ag3 -99.54(2) . . . 3_765 ? Ag4 Ag1 Ag2 Ag3 62.95(2) 3_665 . . 3_765 ? Ag1 Ag1 Ag2 Ag3 107.52(2) 3_665 . . 3_765 ? Ag4 Ag1 Ag2 Ag3 176.753(14) . . . 3_765 ? Ag2 Ag1 Ag2 Ag3 -56.708(18) 3_765 . . 3_765 ? O1 Ag1 Ag3 O4 -177.46(10) . . . . ? O6 Ag1 Ag3 O4 4.25(11) . . . . ? Ag4 Ag1 Ag3 O4 -155.57(9) 3_665 . . . ? Ag1 Ag1 Ag3 O4 122.68(9) 3_665 . . . ? Ag4 Ag1 Ag3 O4 100.96(9) . . . . ? Ag2 Ag1 Ag3 O4 -76.66(9) 3_765 . . . ? Ag2 Ag1 Ag3 O4 -30.05(9) . . . . ? O1 Ag1 Ag3 O2 1.85(11) . . . . ? O6 Ag1 Ag3 O2 -176.44(9) . . . . ? Ag4 Ag1 Ag3 O2 23.73(8) 3_665 . . . ? Ag1 Ag1 Ag3 O2 -58.01(7) 3_665 . . . ? Ag4 Ag1 Ag3 O2 -79.73(7) . . . . ? Ag2 Ag1 Ag3 O2 102.65(7) 3_765 . . . ? Ag2 Ag1 Ag3 O2 149.26(7) . . . . ? O1 Ag1 Ag3 Ag2 161.95(9) . . . 1_556 ? O6 Ag1 Ag3 Ag2 -16.33(9) . . . 1_556 ? Ag4 Ag1 Ag3 Ag2 -176.16(3) 3_665 . . 1_556 ? Ag1 Ag1 Ag3 Ag2 102.10(5) 3_665 . . 1_556 ? Ag4 Ag1 Ag3 Ag2 80.37(5) . . . 1_556 ? Ag2 Ag1 Ag3 Ag2 -97.25(5) 3_765 . . 1_556 ? Ag2 Ag1 Ag3 Ag2 -50.63(6) . . . 1_556 ? O1 Ag1 Ag3 Ag3 -119.44(8) . . . 3_766 ? O6 Ag1 Ag3 Ag3 62.27(7) . . . 3_766 ? Ag4 Ag1 Ag3 Ag3 -97.55(4) 3_665 . . 3_766 ? Ag1 Ag1 Ag3 Ag3 -179.297(17) 3_665 . . 3_766 ? Ag4 Ag1 Ag3 Ag3 158.98(2) . . . 3_766 ? Ag2 Ag1 Ag3 Ag3 -18.641(18) 3_765 . . 3_766 ? Ag2 Ag1 Ag3 Ag3 27.97(3) . . . 3_766 ? O1 Ag1 Ag3 Ag2 -100.80(8) . . . 3_765 ? O6 Ag1 Ag3 Ag2 80.91(7) . . . 3_765 ? Ag4 Ag1 Ag3 Ag2 -78.91(4) 3_665 . . 3_765 ? Ag1 Ag1 Ag3 Ag2 -160.66(2) 3_665 . . 3_765 ? Ag4 Ag1 Ag3 Ag2 177.620(11) . . . 3_765 ? Ag2 Ag1 Ag3 Ag2 46.614(19) . . . 3_765 ? O1 Ag1 Ag3 Ag4 81.58(8) . . . . ? O6 Ag1 Ag3 Ag4 -96.71(7) . . . . ? Ag4 Ag1 Ag3 Ag4 103.47(4) 3_665 . . . ? Ag1 Ag1 Ag3 Ag4 21.724(19) 3_665 . . . ? Ag2 Ag1 Ag3 Ag4 -177.620(11) 3_765 . . . ? Ag2 Ag1 Ag3 Ag4 -131.01(2) . . . . ? O1 Ag1 Ag4 OW2 173.74(11) . . . . ? O6 Ag1 Ag4 OW2 -19.74(11) . . . . ? Ag3 Ag1 Ag4 OW2 -99.51(9) . . . . ? Ag4 Ag1 Ag4 OW2 103.55(9) 3_665 . . . ? Ag1 Ag1 Ag4 OW2 103.55(9) 3_665 . . . ? Ag2 Ag1 Ag4 OW2 -96.84(9) 3_765 . . . ? Ag2 Ag1 Ag4 OW2 8.82(9) . . . . ? O1 Ag1 Ag4 O3 -2.43(10) . . . . ? O6 Ag1 Ag4 O3 164.08(10) . . . . ? Ag3 Ag1 Ag4 O3 84.31(7) . . . . ? Ag4 Ag1 Ag4 O3 -72.63(7) 3_665 . . . ? Ag1 Ag1 Ag4 O3 -72.63(7) 3_665 . . . ? Ag2 Ag1 Ag4 O3 86.98(7) 3_765 . . . ? Ag2 Ag1 Ag4 O3 -167.36(7) . . . . ? O1 Ag1 Ag4 O2 -80.45(14) . . . 3_666 ? O6 Ag1 Ag4 O2 86.06(13) . . . 3_666 ? Ag3 Ag1 Ag4 O2 6.30(12) . . . 3_666 ? Ag4 Ag1 Ag4 O2 -150.65(12) 3_665 . . 3_666 ? Ag1 Ag1 Ag4 O2 -150.65(12) 3_665 . . 3_666 ? Ag2 Ag1 Ag4 O2 8.97(12) 3_765 . . 3_666 ? Ag2 Ag1 Ag4 O2 114.63(12) . . . 3_666 ? O1 Ag1 Ag4 O5 66.15(10) . . . 1_455 ? O6 Ag1 Ag4 O5 -127.34(10) . . . 1_455 ? Ag3 Ag1 Ag4 O5 152.90(7) . . . 1_455 ? Ag4 Ag1 Ag4 O5 -4.05(7) 3_665 . . 1_455 ? Ag1 Ag1 Ag4 O5 -4.05(7) 3_665 . . 1_455 ? Ag2 Ag1 Ag4 O5 155.57(7) 3_765 . . 1_455 ? Ag2 Ag1 Ag4 O5 -98.77(7) . . . 1_455 ? O1 Ag1 Ag4 Ag1 70.20(7) . . . 3_665 ? O6 Ag1 Ag4 Ag1 -123.29(7) . . . 3_665 ? Ag3 Ag1 Ag4 Ag1 156.944(19) . . . 3_665 ? Ag4 Ag1 Ag4 Ag1 0.0 3_665 . . 3_665 ? Ag2 Ag1 Ag4 Ag1 159.61(2) 3_765 . . 3_665 ? Ag2 Ag1 Ag4 Ag1 -94.72(2) . . . 3_665 ? O1 Ag1 Ag4 Ag3 -86.75(7) . . . . ? O6 Ag1 Ag4 Ag3 79.77(7) . . . . ? Ag4 Ag1 Ag4 Ag3 -156.944(19) 3_665 . . . ? Ag1 Ag1 Ag4 Ag3 -156.944(19) 3_665 . . . ? Ag2 Ag1 Ag4 Ag3 2.669(12) 3_765 . . . ? Ag2 Ag1 Ag4 Ag3 108.331(19) . . . . ? O4 Ag3 Ag4 OW2 -3.76(11) . . . . ? O2 Ag3 Ag4 OW2 163.69(11) . . . . ? Ag1 Ag3 Ag4 OW2 75.14(9) . . . . ? Ag2 Ag3 Ag4 OW2 -85.46(9) 1_556 . . . ? Ag3 Ag3 Ag4 OW2 -4.88(10) 3_766 . . . ? Ag2 Ag3 Ag4 OW2 72.70(9) 3_765 . . . ? O4 Ag3 Ag4 O3 -165.73(11) . . . . ? O2 Ag3 Ag4 O3 1.71(10) . . . . ? Ag1 Ag3 Ag4 O3 -86.84(8) . . . . ? Ag2 Ag3 Ag4 O3 112.56(8) 1_556 . . . ? Ag3 Ag3 Ag4 O3 -166.85(9) 3_766 . . . ? Ag2 Ag3 Ag4 O3 -89.28(8) 3_765 . . . ? O4 Ag3 Ag4 O2 104.27(9) . . . 3_666 ? O2 Ag3 Ag4 O2 -88.28(9) . . . 3_666 ? Ag1 Ag3 Ag4 O2 -176.83(6) . . . 3_666 ? Ag2 Ag3 Ag4 O2 22.57(6) 1_556 . . 3_666 ? Ag3 Ag3 Ag4 O2 103.16(8) 3_766 . . 3_666 ? Ag2 Ag3 Ag4 O2 -179.27(6) 3_765 . . 3_666 ? O4 Ag3 Ag4 O5 -165.82(18) . . . 1_455 ? O2 Ag3 Ag4 O5 1.62(18) . . . 1_455 ? Ag1 Ag3 Ag4 O5 -86.93(17) . . . 1_455 ? Ag2 Ag3 Ag4 O5 112.47(17) 1_556 . . 1_455 ? Ag3 Ag3 Ag4 O5 -166.94(17) 3_766 . . 1_455 ? Ag2 Ag3 Ag4 O5 -89.36(17) 3_765 . . 1_455 ? O4 Ag3 Ag4 Ag1 -100.73(7) . . . 3_665 ? O2 Ag3 Ag4 Ag1 66.72(7) . . . 3_665 ? Ag1 Ag3 Ag4 Ag1 -21.831(17) . . . 3_665 ? Ag2 Ag3 Ag4 Ag1 177.571(11) 1_556 . . 3_665 ? Ag3 Ag3 Ag4 Ag1 -101.84(5) 3_766 . . 3_665 ? Ag2 Ag3 Ag4 Ag1 -24.266(19) 3_765 . . 3_665 ? O4 Ag3 Ag4 Ag1 -78.89(7) . . . . ? O2 Ag3 Ag4 Ag1 88.55(7) . . . . ? Ag2 Ag3 Ag4 Ag1 -160.598(17) 1_556 . . . ? Ag3 Ag3 Ag4 Ag1 -80.01(5) 3_766 . . . ? Ag2 Ag3 Ag4 Ag1 -2.435(11) 3_765 . . . ? O3 P1 O1 Ag1 -68.0(2) . . . . ? O2 P1 O1 Ag1 59.2(2) . . . . ? C1 P1 O1 Ag1 174.79(16) . . . . ? O6 Ag1 O1 P1 -24.8(5) . . . . ? Ag3 Ag1 O1 P1 -31.06(17) . . . . ? Ag4 Ag1 O1 P1 156.64(19) 3_665 . . . ? Ag1 Ag1 O1 P1 92.56(19) 3_665 . . . ? Ag4 Ag1 O1 P1 33.65(17) . . . . ? Ag2 Ag1 O1 P1 -93.05(18) 3_765 . . . ? Ag2 Ag1 O1 P1 -162.96(9) . . . . ? O1 P1 O2 Ag3 -56.0(2) . . . . ? O3 P1 O2 Ag3 71.96(19) . . . . ? C1 P1 O2 Ag3 -171.34(15) . . . . ? O1 P1 O2 Ag4 -164.45(15) . . . 3_666 ? O3 P1 O2 Ag4 -36.5(2) . . . 3_666 ? C1 P1 O2 Ag4 80.24(18) . . . 3_666 ? O4 Ag3 O2 P1 29.3(5) . . . . ? Ag1 Ag3 O2 P1 26.47(14) . . . . ? Ag2 Ag3 O2 P1 -147.01(13) 1_556 . . . ? Ag3 Ag3 O2 P1 140.87(12) 3_766 . . . ? Ag2 Ag3 O2 P1 85.79(15) 3_765 . . . ? Ag4 Ag3 O2 P1 -34.72(14) . . . . ? O4 Ag3 O2 Ag4 150.3(4) . . . 3_666 ? Ag1 Ag3 O2 Ag4 147.48(7) . . . 3_666 ? Ag2 Ag3 O2 Ag4 -26.00(9) 1_556 . . 3_666 ? Ag3 Ag3 O2 Ag4 -98.13(7) 3_766 . . 3_666 ? Ag2 Ag3 O2 Ag4 -153.20(5) 3_765 . . 3_666 ? Ag4 Ag3 O2 Ag4 86.29(6) . . . 3_666 ? O1 P1 O3 Ag4 60.9(2) . . . . ? O2 P1 O3 Ag4 -65.94(19) . . . . ? C1 P1 O3 Ag4 177.61(15) . . . . ? O1 P1 O3 Ag2 -77.8(2) . . . 3_665 ? O2 P1 O3 Ag2 155.36(18) . . . 3_665 ? C1 P1 O3 Ag2 38.9(2) . . . 3_665 ? OW2 Ag4 O3 P1 -38.0(4) . . . . ? O2 Ag4 O3 P1 123.80(16) 3_666 . . . ? O5 Ag4 O3 P1 -150.4(2) 1_455 . . . ? Ag1 Ag4 O3 P1 -88.54(16) 3_665 . . . ? Ag1 Ag4 O3 P1 -26.76(15) . . . . ? Ag3 Ag4 O3 P1 29.66(15) . . . . ? OW2 Ag4 O3 Ag2 111.0(3) . . . 3_665 ? O2 Ag4 O3 Ag2 -87.13(10) 3_666 . . 3_665 ? O5 Ag4 O3 Ag2 -1.31(8) 1_455 . . 3_665 ? Ag1 Ag4 O3 Ag2 60.52(8) 3_665 . . 3_665 ? Ag1 Ag4 O3 Ag2 122.30(10) . . . 3_665 ? Ag3 Ag4 O3 Ag2 178.73(10) . . . 3_665 ? O5 P2 O4 Ag3 76.5(2) . . . . ? O6 P2 O4 Ag3 -51.1(2) . . . . ? C7 P2 O4 Ag3 -166.66(17) . . . . ? O2 Ag3 O4 P2 19.3(6) . . . . ? Ag1 Ag3 O4 P2 22.11(18) . . . . ? Ag2 Ag3 O4 P2 -164.1(2) 1_556 . . . ? Ag3 Ag3 O4 P2 -99.2(2) 3_766 . . . ? Ag2 Ag3 O4 P2 -39.50(18) 3_765 . . . ? Ag4 Ag3 O4 P2 81.3(2) . . . . ? O4 P2 O5 Ag2 -61.69(19) . . . 3_765 ? O6 P2 O5 Ag2 66.52(19) . . . 3_765 ? C7 P2 O5 Ag2 -177.64(14) . . . 3_765 ? O4 P2 O5 Ag4 72.0(2) . . . 1_655 ? O6 P2 O5 Ag4 -159.75(18) . . . 1_655 ? C7 P2 O5 Ag4 -43.9(2) . . . 1_655 ? O4 P2 O6 Ag1 57.1(2) . . . . ? O5 P2 O6 Ag1 -70.9(2) . . . . ? C7 P2 O6 Ag1 172.49(15) . . . . ? O4 P2 O6 Ag2 155.53(15) . . . . ? O5 P2 O6 Ag2 27.51(19) . . . . ? C7 P2 O6 Ag2 -89.09(16) . . . . ? O1 Ag1 O6 P2 -37.7(5) . . . . ? Ag3 Ag1 O6 P2 -31.49(15) . . . . ? Ag4 Ag1 O6 P2 140.66(13) 3_665 . . . ? Ag1 Ag1 O6 P2 -148.08(13) 3_665 . . . ? Ag4 Ag1 O6 P2 -94.63(16) . . . . ? Ag2 Ag1 O6 P2 32.84(15) 3_765 . . . ? Ag2 Ag1 O6 P2 110.13(18) . . . . ? O1 Ag1 O6 Ag2 -147.8(4) . . . . ? Ag3 Ag1 O6 Ag2 -141.62(6) . . . . ? Ag4 Ag1 O6 Ag2 30.53(9) 3_665 . . . ? Ag1 Ag1 O6 Ag2 101.79(6) 3_665 . . . ? Ag4 Ag1 O6 Ag2 155.24(5) . . . . ? Ag2 Ag1 O6 Ag2 -77.29(5) 3_765 . . . ? OW1 Ag2 O6 P2 67.14(17) . . . . ? O5 Ag2 O6 P2 -100.72(14) 3_765 . . . ? O3 Ag2 O6 P2 -176.11(15) 3_665 . . . ? Ag3 Ag2 O6 P2 -170.70(7) 1_554 . . . ? Ag1 Ag2 O6 P2 -17.44(15) 3_765 . . . ? Ag1 Ag2 O6 P2 -119.81(18) . . . . ? Ag3 Ag2 O6 P2 -15.1(3) 3_765 . . . ? OW1 Ag2 O6 Ag1 -173.06(11) . . . . ? O5 Ag2 O6 Ag1 19.09(10) 3_765 . . . ? O3 Ag2 O6 Ag1 -56.30(9) 3_665 . . . ? Ag3 Ag2 O6 Ag1 -50.89(13) 1_554 . . . ? Ag1 Ag2 O6 Ag1 102.37(6) 3_765 . . . ? Ag3 Ag2 O6 Ag1 104.76(14) 3_765 . . . ? O1 P1 C1 C2 153.8(3) . . . . ? O3 P1 C1 C2 32.4(3) . . . . ? O2 P1 C1 C2 -87.5(3) . . . . ? O1 P1 C1 C6 -27.0(3) . . . . ? O3 P1 C1 C6 -148.4(3) . . . . ? O2 P1 C1 C6 91.6(3) . . . . ? C6 C1 C2 C3 0.3(6) . . . . ? P1 C1 C2 C3 179.6(3) . . . . ? C1 C2 C3 C4 0.1(7) . . . . ? C2 C3 C4 C5 -0.4(8) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C4 C5 C6 C1 0.2(7) . . . . ? C2 C1 C6 C5 -0.5(6) . . . . ? P1 C1 C6 C5 -179.7(3) . . . . ? O4 P2 C7 C8 125.8(3) . . . . ? O5 P2 C7 C8 -113.9(3) . . . . ? O6 P2 C7 C8 5.6(3) . . . . ? O4 P2 C7 C11 -55.5(3) . . . . ? O5 P2 C7 C11 64.8(3) . . . . ? O6 P2 C7 C11 -175.6(3) . . . . ? C11 C7 C8 C9 -1.6(6) . . . . ? P2 C7 C8 C9 177.1(3) . . . . ? C7 C8 C9 C10 2.0(7) . . . . ? C8 C9 C10 C12 -0.7(8) . . . . ? C8 C7 C11 C12 0.1(6) . . . . ? P2 C7 C11 C12 -178.7(3) . . . . ? C9 C10 C12 C11 -0.9(8) . . . . ? C7 C11 C12 C10 1.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.942 _refine_diff_density_min -1.542 _refine_diff_density_rms 0.576 _database_code_depnum_ccdc_archive 'CCDC 936236' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Ag N4 O3 P' _chemical_formula_weight 457.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2047(7) _cell_length_b 11.1686(7) _cell_length_c 14.7082(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.0820(10) _cell_angle_gamma 90.00 _cell_volume 1905.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19604 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.97 _reflns_number_total 4559 _reflns_number_gt 3768 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2(Bruker,2003) _computing_cell_refinement SAINT(Bruker,2001) _computing_data_reduction APEX2(Bruker,2003) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.2147P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4559 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.461676(18) 0.433627(18) 0.582006(13) 0.05003(8) Uani 1 1 d . . . P1 P 0.84053(5) 0.42803(5) 0.49792(4) 0.03488(13) Uani 1 1 d . . . O1 O 0.73687(16) 0.42237(16) 0.53182(14) 0.0526(5) Uani 1 1 d . . . O2 O 0.94957(17) 0.39360(17) 0.58401(11) 0.0451(4) Uani 1 1 d . . . O3 O 0.86150(14) 0.54612(14) 0.45559(12) 0.0417(4) Uani 1 1 d . . . N1 N 0.36664(16) 0.28580(16) 0.50818(13) 0.0375(4) Uani 1 1 d . . . N2 N 0.25440(16) 0.26688(16) 0.50156(13) 0.0378(4) Uani 1 1 d . . . H2 H 0.2131 0.3161 0.5219 0.045 Uiso 1 1 calc R . . N3 N 0.58554(16) 0.54295(17) 0.67716(13) 0.0382(4) Uani 1 1 d . . . N4 N 0.69754(17) 0.54325(18) 0.67815(13) 0.0403(4) Uani 1 1 d . . . H4 H 0.7244 0.4982 0.6427 0.048 Uiso 1 1 calc R . . C1 C 0.5184(2) 0.1802(3) 0.4624(2) 0.0591(7) Uani 1 1 d . . . H1A H 0.5619 0.2497 0.4909 0.089 Uiso 1 1 calc R . . H1B H 0.5152 0.1750 0.3965 0.089 Uiso 1 1 calc R . . H1C H 0.5548 0.1098 0.4958 0.089 Uiso 1 1 calc R . . C2 C 0.3992(2) 0.1898(2) 0.46879(16) 0.0397(5) Uani 1 1 d . . . C3 C 0.3065(2) 0.1110(2) 0.4376(2) 0.0500(6) Uani 1 1 d . . . H3 H 0.3061 0.0376 0.4076 0.060 Uiso 1 1 calc R . . C4 C 0.2162(2) 0.1626(2) 0.45962(17) 0.0426(5) Uani 1 1 d . . . C5 C 0.0954(2) 0.1214(3) 0.4451(3) 0.0695(9) Uani 1 1 d . . . H5A H 0.0549 0.1807 0.4695 0.104 Uiso 1 1 calc R . . H5B H 0.0967 0.0472 0.4784 0.104 Uiso 1 1 calc R . . H5C H 0.0570 0.1098 0.3781 0.104 Uiso 1 1 calc R . . C6 C 0.4691(2) 0.6471(3) 0.7628(2) 0.0537(6) Uani 1 1 d . . . H6A H 0.4096 0.5972 0.7224 0.081 Uiso 1 1 calc R . . H6B H 0.4482 0.7297 0.7501 0.081 Uiso 1 1 calc R . . H6C H 0.4782 0.6295 0.8286 0.081 Uiso 1 1 calc R . . C7 C 0.5794(2) 0.6236(2) 0.74302(16) 0.0381(5) Uani 1 1 d . . . C8 C 0.6877(2) 0.6750(2) 0.78426(16) 0.0426(5) Uani 1 1 d . . . H8 H 0.7069 0.7334 0.8316 0.051 Uiso 1 1 calc R . . C9 C 0.7602(2) 0.6221(2) 0.74100(16) 0.0418(5) Uani 1 1 d . . . C10 C 0.8855(2) 0.6396(3) 0.7537(2) 0.0670(8) Uani 1 1 d . . . H10A H 0.9086 0.5871 0.7114 0.101 Uiso 1 1 calc R . . H10B H 0.9296 0.6220 0.8187 0.101 Uiso 1 1 calc R . . H10C H 0.8988 0.7212 0.7394 0.101 Uiso 1 1 calc R . . C11 C 0.82699(18) 0.31448(19) 0.40802(15) 0.0349(4) Uani 1 1 d . . . C12 C 0.8488(2) 0.3410(2) 0.32305(16) 0.0429(5) Uani 1 1 d . . . H12 H 0.8748 0.4169 0.3137 0.051 Uiso 1 1 calc R . . C13 C 0.8319(2) 0.2549(3) 0.25189(18) 0.0537(7) Uani 1 1 d . . . H13 H 0.8467 0.2733 0.1952 0.064 Uiso 1 1 calc R . . C14 C 0.7936(2) 0.1430(3) 0.2651(2) 0.0579(7) Uani 1 1 d . . . H14 H 0.7809 0.0862 0.2167 0.070 Uiso 1 1 calc R . . C15 C 0.7738(2) 0.1142(2) 0.3494(2) 0.0560(7) Uani 1 1 d . . . H15 H 0.7493 0.0376 0.3585 0.067 Uiso 1 1 calc R . . C16 C 0.7904(2) 0.1996(2) 0.42127(18) 0.0453(5) Uani 1 1 d . . . H16 H 0.7770 0.1799 0.4783 0.054 Uiso 1 1 calc R . . H0 H 1.007(3) 0.407(3) 0.573(2) 0.051(9) 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 Ag 0.05668(13) 0.04919(12) 0.04505(12) -0.01181(8) 0.01700(9) -0.01928(9) P1 0.0366(3) 0.0351(3) 0.0365(3) -0.0061(2) 0.0166(2) 0.0018(2) O1 0.0480(10) 0.0585(11) 0.0622(11) -0.0208(9) 0.0329(9) -0.0063(8) O2 0.0480(11) 0.0510(10) 0.0358(8) 0.0036(7) 0.0121(8) -0.0045(8) O3 0.0433(9) 0.0356(8) 0.0489(9) -0.0015(7) 0.0182(7) 0.0058(7) N1 0.0364(10) 0.0340(9) 0.0407(9) -0.0032(7) 0.0101(8) -0.0004(7) N2 0.0352(10) 0.0349(9) 0.0437(10) -0.0037(8) 0.0127(8) 0.0044(8) N3 0.0364(10) 0.0400(10) 0.0389(10) -0.0059(8) 0.0126(8) -0.0034(8) N4 0.0394(10) 0.0473(11) 0.0372(9) -0.0060(8) 0.0164(8) 0.0006(8) C1 0.0510(15) 0.0552(16) 0.0783(19) 0.0048(14) 0.0305(14) 0.0123(13) C2 0.0384(12) 0.0365(11) 0.0436(12) 0.0009(9) 0.0122(9) 0.0058(9) C3 0.0504(14) 0.0322(11) 0.0636(16) -0.0100(11) 0.0122(12) 0.0049(10) C4 0.0375(12) 0.0335(11) 0.0513(13) -0.0017(9) 0.0060(10) 0.0001(9) C5 0.0416(15) 0.0571(18) 0.101(2) -0.0008(17) 0.0095(15) -0.0069(13) C6 0.0464(14) 0.0588(16) 0.0605(16) -0.0080(13) 0.0232(12) 0.0035(12) C7 0.0408(12) 0.0363(11) 0.0381(11) -0.0020(9) 0.0138(9) 0.0006(9) C8 0.0458(13) 0.0451(13) 0.0361(11) -0.0075(9) 0.0116(10) -0.0064(10) C9 0.0380(12) 0.0519(14) 0.0347(11) 0.0015(10) 0.0101(9) -0.0068(10) C10 0.0428(15) 0.102(3) 0.0557(16) -0.0080(16) 0.0146(12) -0.0154(16) C11 0.0301(10) 0.0379(11) 0.0370(10) -0.0057(8) 0.0109(8) 0.0068(8) C12 0.0422(12) 0.0467(13) 0.0408(12) -0.0048(10) 0.0144(10) 0.0048(10) C13 0.0485(14) 0.0737(19) 0.0395(12) -0.0142(12) 0.0144(11) 0.0069(13) C14 0.0492(15) 0.0614(17) 0.0582(16) -0.0297(13) 0.0095(12) 0.0015(13) C15 0.0515(15) 0.0427(14) 0.0709(18) -0.0172(13) 0.0147(13) -0.0044(12) C16 0.0447(13) 0.0422(13) 0.0503(13) -0.0059(10) 0.0166(11) 0.0007(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N3 2.1027(18) . ? Ag N1 2.1139(18) . ? Ag Ag 3.2083(4) 3_666 ? P1 O1 1.4982(18) . ? P1 O3 1.5138(17) . ? P1 O2 1.5736(18) . ? P1 C11 1.802(2) . ? O2 H0 0.78(3) . ? N1 C2 1.336(3) . ? N1 N2 1.359(3) . ? N2 C4 1.332(3) . ? N2 H2 0.8600 . ? N3 C7 1.342(3) . ? N3 N4 1.363(3) . ? N4 C9 1.333(3) . ? N4 H4 0.8600 . ? C1 C2 1.490(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.394(3) . ? C3 C4 1.368(4) . ? C3 H3 0.9300 . ? C4 C5 1.496(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.486(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.395(3) . ? C8 C9 1.374(3) . ? C8 H8 0.9300 . ? C9 C10 1.494(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.388(3) . ? C11 C16 1.392(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9300 . ? C13 C14 1.369(4) . ? C13 H13 0.9300 . ? C14 C15 1.374(4) . ? C14 H14 0.9300 . ? C15 C16 1.391(3) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag N1 164.14(7) . . ? N3 Ag Ag 85.12(5) . 3_666 ? N1 Ag Ag 102.49(5) . 3_666 ? O1 P1 O3 116.22(10) . . ? O1 P1 O2 108.21(11) . . ? O3 P1 O2 109.58(10) . . ? O1 P1 C11 108.65(10) . . ? O3 P1 C11 107.45(10) . . ? O2 P1 C11 106.29(10) . . ? P1 O2 H0 112(2) . . ? C2 N1 N2 105.82(18) . . ? C2 N1 Ag 131.29(16) . . ? N2 N1 Ag 122.57(14) . . ? C4 N2 N1 111.65(18) . . ? C4 N2 H2 124.2 . . ? N1 N2 H2 124.2 . . ? C7 N3 N4 105.75(18) . . ? C7 N3 Ag 132.88(16) . . ? N4 N3 Ag 121.35(14) . . ? C9 N4 N3 111.54(18) . . ? C9 N4 H4 124.2 . . ? N3 N4 H4 124.2 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.2(2) . . ? N1 C2 C1 120.8(2) . . ? C3 C2 C1 129.9(2) . . ? C4 C3 C2 106.6(2) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? N2 C4 C3 106.6(2) . . ? N2 C4 C5 121.5(2) . . ? C3 C4 C5 131.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 109.4(2) . . ? N3 C7 C6 121.1(2) . . ? C8 C7 C6 129.5(2) . . ? C9 C8 C7 106.4(2) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? N4 C9 C8 106.9(2) . . ? N4 C9 C10 121.2(2) . . ? C8 C9 C10 131.9(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 118.8(2) . . ? C12 C11 P1 120.71(18) . . ? C16 C11 P1 120.41(17) . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.3(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.2(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ag N1 C2 -51.0(4) . . . . ? Ag Ag N1 C2 66.4(2) 3_666 . . . ? N3 Ag N1 N2 121.5(3) . . . . ? Ag Ag N1 N2 -121.02(15) 3_666 . . . ? C2 N1 N2 C4 0.1(2) . . . . ? Ag N1 N2 C4 -174.10(15) . . . . ? N1 Ag N3 C7 -118.6(3) . . . . ? Ag Ag N3 C7 121.8(2) 3_666 . . . ? N1 Ag N3 N4 63.5(3) . . . . ? Ag Ag N3 N4 -56.10(16) 3_666 . . . ? C7 N3 N4 C9 -0.9(3) . . . . ? Ag N3 N4 C9 177.52(15) . . . . ? N2 N1 C2 C3 0.0(3) . . . . ? Ag N1 C2 C3 173.48(17) . . . . ? N2 N1 C2 C1 179.3(2) . . . . ? Ag N1 C2 C1 -7.2(3) . . . . ? N1 C2 C3 C4 -0.1(3) . . . . ? C1 C2 C3 C4 -179.3(3) . . . . ? N1 N2 C4 C3 -0.1(3) . . . . ? N1 N2 C4 C5 179.4(2) . . . . ? C2 C3 C4 N2 0.1(3) . . . . ? C2 C3 C4 C5 -179.3(3) . . . . ? N4 N3 C7 C8 0.6(3) . . . . ? Ag N3 C7 C8 -177.56(16) . . . . ? N4 N3 C7 C6 -179.4(2) . . . . ? Ag N3 C7 C6 2.4(3) . . . . ? N3 C7 C8 C9 -0.1(3) . . . . ? C6 C7 C8 C9 179.9(2) . . . . ? N3 N4 C9 C8 0.8(3) . . . . ? N3 N4 C9 C10 -179.1(2) . . . . ? C7 C8 C9 N4 -0.4(3) . . . . ? C7 C8 C9 C10 179.5(3) . . . . ? O1 P1 C11 C12 133.70(19) . . . . ? O3 P1 C11 C12 7.2(2) . . . . ? O2 P1 C11 C12 -110.06(19) . . . . ? O1 P1 C11 C16 -44.0(2) . . . . ? O3 P1 C11 C16 -170.47(18) . . . . ? O2 P1 C11 C16 72.3(2) . . . . ? C16 C11 C12 C13 1.3(3) . . . . ? P1 C11 C12 C13 -176.40(19) . . . . ? C11 C12 C13 C14 0.0(4) . . . . ? C12 C13 C14 C15 -1.4(4) . . . . ? C13 C14 C15 C16 1.3(4) . . . . ? C14 C15 C16 C11 0.0(4) . . . . ? C12 C11 C16 C15 -1.3(3) . . . . ? P1 C11 C16 C15 176.36(19) . . . . ? 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 N2 H2 O3 0.86 1.87 2.704(2) 163.4 3_666 C14 H14 O3 0.93 2.63 3.387(3) 139.2 2_645 N4 H4 O1 0.86 1.88 2.707(2) 159.4 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.538 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 936237' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114.75 H127.34 Ag8 Cl3.25 N0.75 O29.25 P10' _chemical_formula_weight 3272.89 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 '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 16.358(2) _cell_length_b 37.807(4) _cell_length_c 22.401(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.382(2) _cell_angle_gamma 90.00 _cell_volume 13069(3) _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 block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6545 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 230128 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 28.16 _reflns_number_total 31725 _reflns_number_gt 28109 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2(Bruker,2003) _computing_cell_refinement SAINT(Bruker,2001) _computing_data_reduction APEX2(Bruker,2003) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+210.4782P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31725 _refine_ls_number_parameters 1591 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.1665 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.273 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.15170(3) 0.680591(13) -0.24893(2) 0.01853(11) Uani 1 1 d . . . Ag2 Ag -0.14577(3) 0.571729(13) -0.25346(2) 0.01802(10) Uani 1 1 d . . . Ag3 Ag 0.19236(3) 0.676746(14) -0.10681(3) 0.01982(11) Uani 1 1 d . . . Ag4 Ag 0.19741(3) 0.580519(14) -0.10955(3) 0.01959(11) Uani 1 1 d . . . Ag5 Ag 0.05032(3) 0.567848(14) -0.23391(2) 0.01955(11) Uani 1 1 d . A . Ag6 Ag 0.04112(3) 0.688375(14) -0.22727(3) 0.02003(11) Uani 1 1 d . A . Ag7 Ag -0.24314(4) 0.575986(14) -0.39893(3) 0.02458(12) Uani 1 1 d . A . Ag8 Ag -0.25009(4) 0.678255(15) -0.39267(3) 0.02739(13) Uani 1 1 d . A . P9 P -0.18820(11) 0.74124(4) -0.24998(8) 0.0144(3) Uani 1 1 d . A . P10 P 0.01720(10) 0.62566(4) -0.13608(7) 0.0126(3) Uani 1 1 d . . . P11 P 0.23012(11) 0.73694(5) -0.09320(8) 0.0155(3) Uani 1 1 d . A . P12 P -0.27950(12) 0.73877(5) -0.39323(8) 0.0169(3) Uani 1 1 d . . . P13 P 0.14267(12) 0.52188(5) -0.24035(8) 0.0174(3) Uani 1 1 d . . . P14 P -0.08459(11) 0.62838(5) -0.34982(8) 0.0163(3) Uani 1 1 d . . . P15 P 0.12394(11) 0.73803(5) -0.23115(8) 0.0162(3) Uani 1 1 d . . . P16 P 0.24726(11) 0.52180(5) -0.10120(8) 0.0158(3) Uani 1 1 d . A . P17 P -0.17344(11) 0.51013(4) -0.25938(8) 0.0143(3) Uani 1 1 d . A . P18 P -0.26372(11) 0.51486(5) -0.40338(8) 0.0164(3) Uani 1 1 d . . . O1 O 0.1166(3) 0.62768(12) -0.1238(2) 0.0168(9) Uani 1 1 d . A . O2 O -0.0190(3) 0.59171(13) -0.1718(2) 0.0194(10) Uani 1 1 d . A . O3 O -0.0255(3) 0.65961(13) -0.1683(2) 0.0192(10) Uani 1 1 d . A . O4 O -0.0607(3) 0.66190(15) -0.3101(2) 0.0241(11) Uani 1 1 d . A . O5 O -0.1844(3) 0.62786(14) -0.3841(2) 0.0232(11) Uani 1 1 d . A . O6 O -0.0576(3) 0.59381(15) -0.3143(2) 0.0236(11) Uani 1 1 d . A . O1W O 0.3050(4) 0.63085(15) -0.0770(3) 0.0383(15) Uani 1 1 d . A . C1 C -0.1067(5) 0.7683(2) -0.1928(3) 0.0210(14) Uani 1 1 d . . . C2 C -0.0663(5) 0.7534(2) -0.1335(4) 0.0258(16) Uani 1 1 d . A . H2 H -0.0758 0.7298 -0.1264 0.031 Uiso 1 1 calc R . . C3 C -0.0117(5) 0.7738(3) -0.0849(4) 0.041(2) Uani 1 1 d . . . H3 H 0.0141 0.7641 -0.0449 0.049 Uiso 1 1 calc R A . C4 C 0.0038(6) 0.8088(3) -0.0965(5) 0.043(2) Uani 1 1 d . A . H4 H 0.0394 0.8226 -0.0638 0.052 Uiso 1 1 calc R . . C5 C -0.0327(6) 0.8233(3) -0.1557(5) 0.045(3) Uani 1 1 d . . . H5 H -0.0196 0.8464 -0.1634 0.054 Uiso 1 1 calc R A . C6 C -0.0895(6) 0.8032(2) -0.2041(4) 0.0326(18) Uani 1 1 d . A . H6 H -0.1159 0.8132 -0.2438 0.039 Uiso 1 1 calc R . . C7 C -0.2848(4) 0.7528(2) -0.2310(3) 0.0186(13) Uani 1 1 d . . . C8 C -0.3043(5) 0.7882(2) -0.2244(4) 0.0266(16) Uani 1 1 d . A . H8 H -0.2685 0.8060 -0.2303 0.032 Uiso 1 1 calc R . . C9 C -0.3780(6) 0.7968(3) -0.2090(4) 0.035(2) Uani 1 1 d . . . H9 H -0.3922 0.8204 -0.2057 0.042 Uiso 1 1 calc R A . C10 C -0.4293(5) 0.7704(3) -0.1989(4) 0.037(2) Uani 1 1 d . A . H10 H -0.4776 0.7761 -0.1878 0.045 Uiso 1 1 calc R . . C11 C -0.4097(5) 0.7350(3) -0.2052(4) 0.035(2) Uani 1 1 d . . . H11 H -0.4450 0.7172 -0.1984 0.042 Uiso 1 1 calc R A . C12 C -0.3374(5) 0.7261(2) -0.2216(4) 0.0260(16) Uani 1 1 d . A . H12 H -0.3245 0.7025 -0.2262 0.031 Uiso 1 1 calc R . . C13 C -0.2037(4) 0.76301(18) -0.3260(3) 0.0164(12) Uani 1 1 d . A . C14 C -0.2648(4) 0.76136(18) -0.4609(3) 0.0175(13) Uani 1 1 d . A . C15 C -0.2482(5) 0.7410(2) -0.5071(3) 0.0221(14) Uani 1 1 d . . . H15 H -0.2463 0.7165 -0.5036 0.027 Uiso 1 1 calc R A . C16 C -0.2343(5) 0.7572(2) -0.5588(4) 0.0310(18) Uani 1 1 d . A . H16 H -0.2233 0.7435 -0.5898 0.037 Uiso 1 1 calc R . . C17 C -0.2369(6) 0.7939(3) -0.5641(4) 0.037(2) Uani 1 1 d . . . H17 H -0.2279 0.8047 -0.5987 0.044 Uiso 1 1 calc R A . C18 C -0.2529(6) 0.8141(2) -0.5181(4) 0.035(2) Uani 1 1 d . A . H18 H -0.2538 0.8386 -0.5215 0.042 Uiso 1 1 calc R . . C19 C -0.2677(5) 0.7983(2) -0.4668(3) 0.0254(15) Uani 1 1 d . . . H19 H -0.2795 0.8122 -0.4363 0.031 Uiso 1 1 calc R A . C20 C -0.3881(4) 0.7492(2) -0.3941(3) 0.0224(15) Uani 1 1 d . A . C21 C -0.4130(6) 0.7833(3) -0.3829(4) 0.0348(19) Uani 1 1 d . . . H21 H -0.3730 0.8017 -0.3728 0.042 Uiso 1 1 calc R A . C22 C -0.4989(7) 0.7892(4) -0.3873(5) 0.057(3) Uani 1 1 d . A . H22 H -0.5156 0.8117 -0.3793 0.068 Uiso 1 1 calc R . . C23 C -0.5586(6) 0.7628(5) -0.4030(5) 0.064(4) Uani 1 1 d . . . H23 H -0.6159 0.7676 -0.4068 0.076 Uiso 1 1 calc R A . C24 C -0.5343(6) 0.7288(4) -0.4133(5) 0.056(3) Uani 1 1 d . A . H24 H -0.5753 0.7107 -0.4234 0.067 Uiso 1 1 calc R . . C25 C -0.4489(6) 0.7216(3) -0.4086(4) 0.040(2) Uani 1 1 d . . . H25 H -0.4323 0.6987 -0.4150 0.048 Uiso 1 1 calc R A . C26 C 0.0623(5) 0.7685(2) -0.2925(3) 0.0230(15) Uani 1 1 d . A . C27 C 0.0538(7) 0.8041(3) -0.2826(5) 0.051(3) Uani 1 1 d . . . H27 H 0.0818 0.8141 -0.2432 0.061 Uiso 1 1 calc R A . C28 C 0.0027(8) 0.8250(3) -0.3325(6) 0.057(3) Uani 1 1 d . A . H28 H -0.0020 0.8492 -0.3263 0.069 Uiso 1 1 calc R . . C29 C -0.0401(6) 0.8106(3) -0.3901(5) 0.047(3) Uani 1 1 d . . . H29 H -0.0741 0.8249 -0.4226 0.056 Uiso 1 1 calc R A . C30 C -0.0334(6) 0.7752(3) -0.4004(4) 0.042(2) Uani 1 1 d . A . H30 H -0.0629 0.7655 -0.4399 0.050 Uiso 1 1 calc R . . C31 C 0.0179(5) 0.7538(3) -0.3514(4) 0.0339(19) Uani 1 1 d . . . H31 H 0.0225 0.7297 -0.3581 0.041 Uiso 1 1 calc R A . C32 C 0.2233(4) 0.7293(2) -0.2480(3) 0.0218(15) Uani 1 1 d . A . C33 C 0.2538(6) 0.6958(2) -0.2467(4) 0.0317(18) Uani 1 1 d . . . H33 H 0.2242 0.6770 -0.2364 0.038 Uiso 1 1 calc R A . C34 C 0.3297(6) 0.6896(3) -0.2607(5) 0.046(2) Uani 1 1 d . A . H34 H 0.3504 0.6666 -0.2603 0.055 Uiso 1 1 calc R . . C35 C 0.3737(6) 0.7177(3) -0.2753(5) 0.047(3) Uani 1 1 d . . . H35 H 0.4237 0.7134 -0.2853 0.057 Uiso 1 1 calc R A . C36 C 0.3452(6) 0.7514(3) -0.2754(4) 0.045(3) Uani 1 1 d . A . H36 H 0.3759 0.7699 -0.2853 0.054 Uiso 1 1 calc R . . C37 C 0.2703(5) 0.7585(2) -0.2608(4) 0.0294(17) Uani 1 1 d . . . H37 H 0.2515 0.7816 -0.2595 0.035 Uiso 1 1 calc R A . C38 C 0.1589(4) 0.76405(18) -0.1579(3) 0.0176(13) Uani 1 1 d . A . C39 C 0.2151(4) 0.75594(19) -0.0233(3) 0.0176(13) Uani 1 1 d . . . C40 C 0.1988(5) 0.7331(2) 0.0209(3) 0.0224(14) Uani 1 1 d . A . H40 H 0.1980 0.7088 0.0146 0.027 Uiso 1 1 calc R . . C41 C 0.1838(5) 0.7466(2) 0.0736(4) 0.0314(18) Uani 1 1 d . . . H41 H 0.1722 0.7313 0.1024 0.038 Uiso 1 1 calc R A . C42 C 0.1860(6) 0.7824(3) 0.0837(4) 0.0352(19) Uani 1 1 d . A . H42 H 0.1758 0.7913 0.1194 0.042 Uiso 1 1 calc R . . C43 C 0.2033(6) 0.8056(2) 0.0412(4) 0.0319(18) Uani 1 1 d . . . H43 H 0.2056 0.8298 0.0488 0.038 Uiso 1 1 calc R A . C44 C 0.2173(6) 0.7924(2) -0.0127(4) 0.0272(16) Uani 1 1 d . A . H44 H 0.2280 0.8078 -0.0415 0.033 Uiso 1 1 calc R . . C45 C 0.3407(4) 0.7483(2) -0.0872(3) 0.0222(15) Uani 1 1 d . . . C46 C 0.3669(6) 0.7836(3) -0.0885(4) 0.0316(18) Uani 1 1 d . A . H46 H 0.3268 0.8019 -0.0957 0.038 Uiso 1 1 calc R . . C47 C 0.4546(6) 0.7908(3) -0.0788(4) 0.042(2) Uani 1 1 d . . . H47 H 0.4727 0.8141 -0.0799 0.051 Uiso 1 1 calc R A . C48 C 0.5133(6) 0.7642(3) -0.0679(4) 0.047(3) Uani 1 1 d . A . H48 H 0.5715 0.7694 -0.0602 0.056 Uiso 1 1 calc R . . C49 C 0.4872(6) 0.7292(4) -0.0681(5) 0.049(3) Uani 1 1 d . . . H49 H 0.5277 0.7112 -0.0619 0.059 Uiso 1 1 calc R A . C50 C 0.4005(6) 0.7209(3) -0.0776(4) 0.036(2) Uani 1 1 d . A . H50 H 0.3831 0.6975 -0.0774 0.043 Uiso 1 1 calc R . . C51 C -0.0871(4) 0.4841(2) -0.2043(4) 0.0222(14) Uani 1 1 d . . . C52 C -0.0494(5) 0.4979(2) -0.1430(4) 0.0283(17) Uani 1 1 d . A . H52 H -0.0635 0.5205 -0.1331 0.034 Uiso 1 1 calc R . . C53 C 0.0095(6) 0.4770(3) -0.0974(4) 0.044(3) Uani 1 1 d . . . H53 H 0.0333 0.4854 -0.0562 0.053 Uiso 1 1 calc R A . C54 C 0.0330(6) 0.4440(3) -0.1128(5) 0.052(3) Uani 1 1 d . A . H54 H 0.0714 0.4302 -0.0816 0.062 Uiso 1 1 calc R . . C55 C 0.0002(6) 0.4315(3) -0.1738(6) 0.049(3) Uani 1 1 d . . . H55 H 0.0185 0.4098 -0.1841 0.059 Uiso 1 1 calc R A . C56 C -0.0604(5) 0.4514(2) -0.2206(5) 0.037(2) Uani 1 1 d . A . H56 H -0.0827 0.4431 -0.2619 0.044 Uiso 1 1 calc R . . C57 C -0.2815(5) 0.45812(19) -0.2347(3) 0.0226(15) Uani 1 1 d . A . H57 H -0.2409 0.4417 -0.2380 0.027 Uiso 1 1 calc R . . C58 C -0.3546(5) 0.4468(2) -0.2223(4) 0.0293(17) Uani 1 1 d . . . H58 H -0.3630 0.4228 -0.2173 0.035 Uiso 1 1 calc R . . C59 C -0.4153(5) 0.4710(2) -0.2174(4) 0.0322(18) Uani 1 1 d . . . H59 H -0.4646 0.4633 -0.2094 0.039 Uiso 1 1 calc R . . C60 C -0.4024(5) 0.5069(2) -0.2245(4) 0.0282(16) Uani 1 1 d . . . H60 H -0.4428 0.5232 -0.2204 0.034 Uiso 1 1 calc R . . C61 C -0.3300(5) 0.5185(2) -0.2375(3) 0.0213(14) Uani 1 1 d . A . H61 H -0.3225 0.5425 -0.2430 0.026 Uiso 1 1 calc R . . C62 C -0.2682(4) 0.49439(19) -0.2423(3) 0.0173(13) Uani 1 1 d . . . C63 C -0.1861(4) 0.49108(18) -0.3372(3) 0.0171(13) Uani 1 1 d . A . C64 C -0.3709(4) 0.5014(2) -0.4054(3) 0.0186(13) Uani 1 1 d . A . C65 C -0.4358(5) 0.5273(2) -0.4197(4) 0.0288(17) Uani 1 1 d . . . H65 H -0.4228 0.5505 -0.4274 0.035 Uiso 1 1 calc R A . C66 C -0.5187(5) 0.5186(3) -0.4225(4) 0.036(2) Uani 1 1 d . A . H66 H -0.5614 0.5360 -0.4316 0.043 Uiso 1 1 calc R . . C67 C -0.5387(5) 0.4841(3) -0.4116(4) 0.041(2) Uani 1 1 d . . . H67 H -0.5950 0.4783 -0.4142 0.050 Uiso 1 1 calc R A . C68 C -0.4755(5) 0.4584(3) -0.3971(4) 0.035(2) Uani 1 1 d . A . H68 H -0.4891 0.4353 -0.3891 0.043 Uiso 1 1 calc R . . C69 C -0.3920(5) 0.4666(2) -0.3943(4) 0.0245(15) Uani 1 1 d . . . H69 H -0.3498 0.4490 -0.3852 0.029 Uiso 1 1 calc R A . C70 C 0.0875(4) 0.4910(2) -0.3032(3) 0.0198(14) Uani 1 1 d . A . C71 C 0.0956(7) 0.4549(2) -0.2975(5) 0.045(3) Uani 1 1 d . . . H71 H 0.1316 0.4448 -0.2601 0.054 Uiso 1 1 calc R A . C72 C 0.0494(8) 0.4332(3) -0.3483(6) 0.060(3) Uani 1 1 d . A . H72 H 0.0544 0.4087 -0.3442 0.072 Uiso 1 1 calc R . . C73 C -0.0029(6) 0.4476(3) -0.4036(5) 0.047(3) Uani 1 1 d . . . H73 H -0.0344 0.4331 -0.4368 0.057 Uiso 1 1 calc R A . C74 C -0.0086(5) 0.4834(3) -0.4101(4) 0.039(2) Uani 1 1 d . A . H74 H -0.0423 0.4932 -0.4485 0.047 Uiso 1 1 calc R . . C75 C 0.0353(5) 0.5056(3) -0.3600(4) 0.0304(17) Uani 1 1 d . . . H75 H 0.0297 0.5300 -0.3646 0.036 Uiso 1 1 calc R A . C76 C 0.2939(5) 0.5086(2) -0.2692(4) 0.0301(17) Uani 1 1 d . . . H76 H 0.2804 0.4848 -0.2675 0.036 Uiso 1 1 calc R A . C77 C 0.3663(6) 0.5178(3) -0.2833(4) 0.038(2) Uani 1 1 d . A . H77 H 0.4022 0.5005 -0.2907 0.046 Uiso 1 1 calc R . . C78 C 0.3854(7) 0.5534(3) -0.2865(6) 0.055(3) Uani 1 1 d . . . H78 H 0.4344 0.5598 -0.2963 0.066 Uiso 1 1 calc R A . C79 C 0.3343(7) 0.5789(3) -0.2757(7) 0.058(3) Uani 1 1 d . A . H79 H 0.3479 0.6026 -0.2787 0.070 Uiso 1 1 calc R . . C80 C 0.2402(5) 0.5343(2) -0.2574(3) 0.0214(14) Uani 1 1 d . A . C81 C 0.2616(6) 0.5700(3) -0.2602(5) 0.045(2) Uani 1 1 d . . . H81 H 0.2272 0.5876 -0.2518 0.054 Uiso 1 1 calc R A . C82 C 0.1819(5) 0.49464(19) -0.1683(3) 0.0200(14) Uani 1 1 d . A . C83 C 0.3586(5) 0.5161(2) -0.0976(3) 0.0218(14) Uani 1 1 d . . . C84 C 0.3930(6) 0.4825(2) -0.0995(5) 0.042(2) Uani 1 1 d . A . H84 H 0.3583 0.4625 -0.1048 0.050 Uiso 1 1 calc R . . C85 C 0.4805(6) 0.4795(3) -0.0932(5) 0.047(3) Uani 1 1 d . . . H85 H 0.5046 0.4572 -0.0930 0.056 Uiso 1 1 calc R A . C86 C 0.5315(6) 0.5090(3) -0.0873(4) 0.039(2) Uani 1 1 d . A . H86 H 0.5898 0.5064 -0.0826 0.047 Uiso 1 1 calc R . . C87 C 0.4969(6) 0.5421(3) -0.0884(5) 0.047(3) Uani 1 1 d . . . H87 H 0.5310 0.5621 -0.0862 0.057 Uiso 1 1 calc R A . C88 C 0.4097(5) 0.5456(2) -0.0927(5) 0.036(2) Uani 1 1 d . A . H88 H 0.3863 0.5680 -0.0922 0.043 Uiso 1 1 calc R . . C89 C 0.2395(4) 0.49812(19) -0.0327(3) 0.0168(13) Uani 1 1 d . . . C90 C 0.2452(5) 0.4612(2) -0.0281(3) 0.0247(15) Uani 1 1 d . A . H90 H 0.2519 0.4479 -0.0611 0.030 Uiso 1 1 calc R . . C91 C 0.2406(6) 0.4446(2) 0.0259(4) 0.0338(19) Uani 1 1 d . . . H91 H 0.2456 0.4201 0.0294 0.041 Uiso 1 1 calc R A . C92 C 0.2287(6) 0.4642(3) 0.0746(4) 0.036(2) Uani 1 1 d . A . H92 H 0.2253 0.4528 0.1106 0.043 Uiso 1 1 calc R . . C93 C 0.2217(5) 0.5006(2) 0.0700(4) 0.0299(17) Uani 1 1 d . . . H93 H 0.2138 0.5136 0.1029 0.036 Uiso 1 1 calc R A . C94 C 0.2265(5) 0.5178(2) 0.0162(3) 0.0222(14) Uani 1 1 d . A . H94 H 0.2211 0.5423 0.0128 0.027 Uiso 1 1 calc R . . C95 C -0.2424(5) 0.4941(2) -0.4707(3) 0.0209(14) Uani 1 1 d . A . C96 C -0.2237(5) 0.5160(2) -0.5146(4) 0.0266(16) Uani 1 1 d . . . H96 H -0.2248 0.5404 -0.5104 0.032 Uiso 1 1 calc R A . C97 C -0.2033(6) 0.5011(3) -0.5645(4) 0.0342(19) Uani 1 1 d . A . H97 H -0.1921 0.5156 -0.5944 0.041 Uiso 1 1 calc R . . C98 C -0.1997(6) 0.4647(3) -0.5697(4) 0.0351(19) Uani 1 1 d . . . H98 H -0.1845 0.4549 -0.6026 0.042 Uiso 1 1 calc R A . C99 C -0.2187(6) 0.4427(2) -0.5264(4) 0.0319(18) Uani 1 1 d . A . H99 H -0.2170 0.4182 -0.5307 0.038 Uiso 1 1 calc R . . C100 C -0.2403(5) 0.4575(2) -0.4764(4) 0.0246(15) Uani 1 1 d . . . H100 H -0.2531 0.4429 -0.4472 0.030 Uiso 1 1 calc R A . C101 C 0.0404(7) 0.6564(2) -0.0205(4) 0.0339(19) Uani 1 1 d . . . H10A H 0.1017 0.6570 -0.0129 0.051 Uiso 1 1 calc R A . H10B H 0.0300 0.6555 0.0193 0.051 Uiso 1 1 calc R . . H10C H 0.0139 0.6772 -0.0433 0.051 Uiso 1 1 calc R . . C102 C -0.0962(6) 0.6222(3) -0.0713(4) 0.037(2) Uani 1 1 d . . . H10D H -0.1229 0.6431 -0.0936 0.056 Uiso 1 1 calc R A . H10E H -0.1064 0.6210 -0.0315 0.056 Uiso 1 1 calc R . . H10F H -0.1205 0.6017 -0.0961 0.056 Uiso 1 1 calc R . . C103 C 0.0443(7) 0.5902(2) -0.0237(4) 0.038(2) Uani 1 1 d . . . H10G H 0.1056 0.5912 -0.0162 0.057 Uiso 1 1 calc R A . H10H H 0.0204 0.5697 -0.0485 0.057 Uiso 1 1 calc R . . H10I H 0.0340 0.5890 0.0160 0.057 Uiso 1 1 calc R . . C104 C 0.0014(5) 0.62342(19) -0.0595(3) 0.0194(13) Uani 1 1 d . A . C105 C -0.0346(6) 0.6306(2) -0.4113(4) 0.0294(17) Uani 1 1 d . A . C106 C 0.0640(6) 0.6306(3) -0.3795(5) 0.047(3) Uani 1 1 d . . . H10J H 0.0815 0.6094 -0.3549 0.070 Uiso 1 1 calc R A . H10K H 0.0809 0.6509 -0.3524 0.070 Uiso 1 1 calc R . . H10L H 0.0913 0.6315 -0.4114 0.070 Uiso 1 1 calc R . . C107 C -0.0631(7) 0.5985(3) -0.4555(4) 0.041(2) Uani 1 1 d . . . H10M H -0.0448 0.5771 -0.4316 0.062 Uiso 1 1 calc R A . H10N H -0.0373 0.5998 -0.4882 0.062 Uiso 1 1 calc R . . H10O H -0.1251 0.5985 -0.4743 0.062 Uiso 1 1 calc R . . C108 C -0.0648(8) 0.6638(3) -0.4513(4) 0.045(2) Uani 1 1 d . . . H10P H -0.0478 0.6844 -0.4249 0.067 Uiso 1 1 calc R A . H10Q H -0.1267 0.6634 -0.4703 0.067 Uiso 1 1 calc R . . H10R H -0.0388 0.6646 -0.4839 0.067 Uiso 1 1 calc R . . Cl1 Cl -0.81033(19) 0.87515(6) -0.14899(13) 0.0500(6) Uani 1 1 d D . . O9 O -0.7639(5) 0.90538(16) -0.1563(4) 0.054(2) Uani 1 1 d D . . O10 O -0.8134(10) 0.8727(3) -0.0875(4) 0.152(7) Uani 1 1 d D . . O11 O -0.8982(5) 0.8788(2) -0.1928(5) 0.076(3) Uani 1 1 d D . . O12 O -0.7756(5) 0.84411(17) -0.1665(5) 0.087(4) Uani 1 1 d D . . Cl2 Cl -0.3710(2) 0.62644(8) -0.52064(18) 0.0398(10) Uani 0.672(6) 1 d PD A 1 O13 O -0.3329(7) 0.6599(2) -0.5196(5) 0.048(3) Uiso 0.672(6) 1 d PD A 1 O14 O -0.3279(8) 0.5960(3) -0.5270(6) 0.050(3) Uiso 0.672(6) 1 d PD A 1 O15 O -0.4571(7) 0.6258(4) -0.5636(6) 0.068(4) Uiso 0.672(6) 1 d PD A 1 O16 O -0.3754(7) 0.6231(3) -0.4563(4) 0.049(3) Uiso 0.672(6) 1 d PD A 1 N1 N -0.2876(7) 0.6253(2) -0.2881(5) 0.0252(10) Uani 0.672(6) 1 d P A 1 O25 O -0.3308(6) 0.6543(2) -0.3074(4) 0.0252(10) Uani 0.672(6) 1 d P A 1 O26 O -0.3313(6) 0.5969(2) -0.3124(4) 0.0252(10) Uani 0.672(6) 1 d P A 1 O27 O -0.2223(6) 0.6252(2) -0.2542(4) 0.0252(10) Uani 0.672(6) 1 d P A 1 C6A C -0.4597(11) 0.6308(6) -0.1773(8) 0.050(5) Uani 0.672(6) 1 d P A 1 O6A O -0.387(2) 0.6199(9) -0.1693(17) 0.168(14) Uiso 0.672(6) 1 d P A 1 Cl2' Cl -0.3447(7) 0.6320(3) -0.5429(5) 0.066(3) Uiso 0.328(6) 1 d PD A 2 O13' O -0.4207(10) 0.6291(5) -0.5965(8) 0.041(5) Uiso 0.328(6) 1 d PD A 2 O14' O -0.282(2) 0.6553(10) -0.554(2) 0.19(3) Uiso 0.328(6) 1 d PD A 2 O15' O -0.2981(17) 0.6003(5) -0.5285(13) 0.062(8) Uiso 0.328(6) 1 d PD A 2 O16' O -0.367(3) 0.6471(13) -0.4919(15) 0.19(3) Uiso 0.328(6) 1 d PD A 2 Cl4 Cl -0.3992(5) 0.62292(17) -0.1796(4) 0.0293(16) Uani 0.328(6) 1 d PD A 2 O21 O -0.404(2) 0.6143(11) -0.1188(9) 0.123(17) Uani 0.328(6) 1 d PD A 2 O22 O -0.4653(14) 0.6472(6) -0.2105(15) 0.095(13) Uani 0.328(6) 1 d PD A 2 O23 O -0.4153(15) 0.5919(6) -0.2175(15) 0.111(16) Uani 0.328(6) 1 d PD A 2 O24 O -0.3153(9) 0.6358(6) -0.1710(10) 0.052(7) Uani 0.328(6) 1 d PD A 2 O2W O -0.3644(13) 0.6276(8) -0.3696(11) 0.060(7) Uani 0.328(6) 1 d P A 2 Cl3 Cl -0.2308(6) 0.88086(16) -0.3417(3) 0.0557(19) Uani 0.695(15) 1 d PD B 1 O17 O -0.2682(9) 0.9139(2) -0.3345(7) 0.053(3) Uani 0.695(15) 1 d PD B 1 O18 O -0.2853(12) 0.8521(4) -0.3393(10) 0.091(7) Uani 0.695(15) 1 d PD B 1 O19 O -0.1514(8) 0.8763(4) -0.2899(6) 0.086(5) Uani 0.695(15) 1 d PD B 1 O20 O -0.2102(16) 0.8804(5) -0.3980(7) 0.090(8) Uani 0.695(15) 1 d PD B 1 Cl3' Cl -0.2665(10) 0.8817(3) -0.3578(6) 0.045(3) Uani 0.305(15) 1 d PD B 2 O17' O -0.2302(18) 0.9134(6) -0.3267(14) 0.056(10) Uiso 0.305(15) 1 d PD B 2 O18' O -0.3585(11) 0.8806(7) -0.3725(16) 0.089(13) Uani 0.305(15) 1 d PD B 2 O19' O -0.232(2) 0.8518(6) -0.3199(16) 0.064(11) Uani 0.305(15) 1 d PD B 2 O20' O -0.250(3) 0.8806(11) -0.4162(12) 0.079(18) Uani 0.305(15) 1 d PD B 2 C3A C -0.5331(6) 0.6356(3) -0.0802(6) 0.048(3) Uani 1 1 d . . . O3A O -0.4736(14) 0.6334(4) -0.0234(14) 0.209(12) Uani 1 1 d . . . O4A O -0.7367(8) 0.6524(3) -0.8736(5) 0.083(3) Uani 1 1 d . . . C4A C -0.7985(10) 0.6362(5) -0.8504(7) 0.087(5) Uani 1 1 d . . . O5A O -0.4143(7) 0.3507(3) -0.2211(5) 0.083(3) Uani 1 1 d . . . C5A C -0.4149(9) 0.3516(4) -0.2851(6) 0.066(3) Uani 1 1 d . . . O7A O -0.5070(9) 0.6482(4) -0.3036(7) 0.034(4) Uani 0.408(16) 1 d PD C 1 C7A C -0.532(6) 0.631(2) -0.364(3) 0.23(4) Uiso 0.408(16) 1 d PD C 1 C8A C -0.5311(12) 0.6163(6) -0.4152(11) 0.059(6) Uani 0.592(16) 1 d PD C 2 O8A O -0.592(2) 0.6234(9) -0.4771(13) 0.170(13) Uiso 0.592(16) 1 d PD C 2 C9A C -0.394(5) 0.597(2) -0.729(2) 0.24(4) Uiso 0.512(17) 1 d PD D 1 O9A O -0.4470(10) 0.6106(5) -0.7880(11) 0.083(8) Uani 0.512(17) 1 d PD D 1 O2A O -0.3286(17) 0.5901(6) -0.6633(11) 0.086(8) Uani 0.488(17) 1 d P D 2 C2A C -0.253(3) 0.6070(12) -0.6534(17) 0.117(18) Uani 0.488(17) 1 d P D 2 O1A O 0.2988(7) 0.6159(3) 0.0341(4) 0.081(3) Uani 1 1 d . E 2 C1A C 0.3707(11) 0.5952(4) 0.0677(7) 0.077(4) Uani 1 1 d . E 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 0.0193(2) 0.0163(2) 0.0192(2) 0.00265(18) 0.00522(19) 0.00220(18) Ag2 0.0186(2) 0.0170(2) 0.0187(2) -0.00271(19) 0.00661(19) -0.00285(18) Ag3 0.0208(2) 0.0176(2) 0.0195(2) -0.00235(19) 0.0046(2) -0.00106(19) Ag4 0.0202(2) 0.0182(2) 0.0187(2) -0.00248(19) 0.00410(19) 0.00485(19) Ag5 0.0175(2) 0.0220(3) 0.0178(2) -0.00312(19) 0.00398(19) 0.00505(19) Ag6 0.0179(2) 0.0211(3) 0.0191(2) 0.00064(19) 0.00356(19) -0.00626(19) Ag7 0.0331(3) 0.0175(3) 0.0198(3) -0.0008(2) 0.0042(2) -0.0044(2) Ag8 0.0413(3) 0.0179(3) 0.0184(3) 0.0007(2) 0.0038(2) 0.0036(2) P9 0.0140(7) 0.0159(8) 0.0134(7) 0.0024(6) 0.0047(6) 0.0013(6) P10 0.0137(7) 0.0136(7) 0.0107(7) -0.0005(6) 0.0043(6) 0.0007(6) P11 0.0143(8) 0.0196(8) 0.0127(8) -0.0011(6) 0.0045(6) -0.0015(6) P12 0.0186(8) 0.0178(8) 0.0138(8) 0.0022(6) 0.0046(6) 0.0009(6) P13 0.0185(8) 0.0201(8) 0.0120(8) -0.0017(6) 0.0032(6) 0.0043(7) P14 0.0171(8) 0.0211(8) 0.0096(7) -0.0002(6) 0.0029(6) -0.0023(6) P15 0.0148(8) 0.0212(8) 0.0116(7) -0.0011(6) 0.0030(6) -0.0055(6) P16 0.0158(8) 0.0190(8) 0.0123(7) -0.0014(6) 0.0045(6) 0.0028(6) P17 0.0150(7) 0.0143(8) 0.0131(7) -0.0019(6) 0.0040(6) -0.0005(6) P18 0.0173(8) 0.0169(8) 0.0145(8) -0.0022(6) 0.0046(6) -0.0015(6) O1 0.015(2) 0.014(2) 0.023(2) 0.0002(18) 0.0079(18) 0.0036(17) O2 0.020(2) 0.022(2) 0.017(2) -0.0057(19) 0.0066(19) -0.0026(19) O3 0.019(2) 0.022(2) 0.016(2) 0.0050(19) 0.0049(19) 0.0037(19) O4 0.023(3) 0.028(3) 0.021(3) -0.010(2) 0.008(2) -0.007(2) O5 0.025(3) 0.020(2) 0.019(2) 0.001(2) -0.001(2) -0.002(2) O6 0.021(3) 0.030(3) 0.019(2) 0.008(2) 0.006(2) 0.003(2) O1W 0.024(3) 0.017(3) 0.068(5) -0.009(3) 0.007(3) 0.003(2) C1 0.017(3) 0.026(4) 0.019(3) -0.005(3) 0.005(3) 0.001(3) C2 0.023(4) 0.035(4) 0.020(4) 0.004(3) 0.009(3) 0.006(3) C3 0.021(4) 0.083(8) 0.020(4) -0.008(4) 0.009(3) 0.007(4) C4 0.024(4) 0.061(6) 0.037(5) -0.030(5) 0.001(4) 0.000(4) C5 0.028(4) 0.027(4) 0.068(7) -0.017(4) -0.001(4) -0.001(4) C6 0.034(4) 0.020(4) 0.036(5) 0.002(3) 0.002(4) 0.000(3) C7 0.016(3) 0.028(4) 0.010(3) 0.004(3) 0.002(2) 0.001(3) C8 0.025(4) 0.028(4) 0.027(4) 0.004(3) 0.010(3) 0.008(3) C9 0.037(5) 0.038(5) 0.032(4) 0.000(4) 0.014(4) 0.017(4) C10 0.018(4) 0.068(7) 0.027(4) -0.007(4) 0.009(3) 0.003(4) C11 0.018(4) 0.060(6) 0.026(4) 0.001(4) 0.007(3) -0.004(4) C12 0.022(4) 0.035(4) 0.020(4) -0.004(3) 0.006(3) -0.007(3) C13 0.019(3) 0.017(3) 0.013(3) 0.000(2) 0.004(2) -0.002(2) C14 0.016(3) 0.020(3) 0.016(3) 0.002(2) 0.005(3) 0.003(2) C15 0.020(3) 0.027(4) 0.017(3) -0.004(3) 0.004(3) 0.000(3) C16 0.030(4) 0.047(5) 0.019(4) -0.003(3) 0.012(3) -0.008(4) C17 0.049(5) 0.042(5) 0.021(4) 0.005(3) 0.013(4) -0.016(4) C18 0.046(5) 0.031(4) 0.025(4) 0.011(3) 0.007(4) -0.008(4) C19 0.033(4) 0.028(4) 0.015(3) 0.005(3) 0.007(3) 0.003(3) C20 0.014(3) 0.041(4) 0.010(3) 0.002(3) 0.001(2) -0.002(3) C21 0.025(4) 0.052(6) 0.028(4) 0.004(4) 0.010(3) 0.007(4) C22 0.033(5) 0.103(10) 0.031(5) 0.002(6) 0.008(4) 0.027(6) C23 0.015(4) 0.149(14) 0.030(5) 0.007(7) 0.010(4) 0.009(6) C24 0.025(5) 0.112(11) 0.032(5) 0.001(6) 0.012(4) -0.032(6) C25 0.030(4) 0.066(7) 0.025(4) 0.001(4) 0.011(4) -0.015(4) C26 0.017(3) 0.035(4) 0.017(3) 0.010(3) 0.005(3) -0.004(3) C27 0.060(7) 0.038(5) 0.036(5) 0.011(4) -0.009(5) -0.010(5) C28 0.056(7) 0.032(5) 0.068(8) 0.024(5) 0.000(6) -0.001(5) C29 0.027(4) 0.064(7) 0.040(5) 0.034(5) -0.001(4) -0.004(4) C30 0.026(4) 0.078(8) 0.019(4) 0.011(4) 0.004(3) -0.005(4) C31 0.024(4) 0.058(6) 0.018(4) 0.002(4) 0.004(3) 0.005(4) C32 0.016(3) 0.036(4) 0.017(3) -0.007(3) 0.009(3) -0.007(3) C33 0.037(5) 0.030(4) 0.026(4) -0.013(3) 0.007(3) 0.000(3) C34 0.036(5) 0.060(7) 0.038(5) -0.015(5) 0.008(4) 0.014(5) C35 0.025(4) 0.085(8) 0.036(5) -0.011(5) 0.014(4) -0.003(5) C36 0.025(4) 0.082(8) 0.034(5) -0.013(5) 0.018(4) -0.022(5) C37 0.021(4) 0.045(5) 0.023(4) -0.007(3) 0.007(3) -0.009(3) C38 0.020(3) 0.017(3) 0.014(3) 0.002(2) 0.002(3) 0.000(2) C39 0.014(3) 0.026(4) 0.012(3) -0.001(3) 0.004(2) -0.002(3) C40 0.025(4) 0.022(3) 0.021(3) 0.003(3) 0.008(3) -0.003(3) C41 0.032(4) 0.046(5) 0.018(4) 0.002(3) 0.010(3) -0.005(4) C42 0.042(5) 0.044(5) 0.020(4) -0.005(3) 0.012(4) 0.006(4) C43 0.036(4) 0.032(4) 0.028(4) -0.012(3) 0.010(3) -0.001(3) C44 0.037(4) 0.023(4) 0.021(4) -0.002(3) 0.009(3) -0.002(3) C45 0.014(3) 0.039(4) 0.012(3) 0.000(3) 0.002(2) -0.007(3) C46 0.029(4) 0.044(5) 0.022(4) 0.000(3) 0.008(3) -0.011(4) C47 0.030(5) 0.067(7) 0.027(4) 0.005(4) 0.005(4) -0.022(4) C48 0.021(4) 0.094(9) 0.025(4) 0.011(5) 0.007(3) -0.013(5) C49 0.021(4) 0.088(9) 0.036(5) 0.000(5) 0.007(4) 0.005(5) C50 0.025(4) 0.046(5) 0.037(5) 0.002(4) 0.010(4) 0.007(4) C51 0.013(3) 0.026(4) 0.025(4) 0.008(3) 0.004(3) -0.002(3) C52 0.022(4) 0.046(5) 0.016(3) -0.001(3) 0.006(3) -0.002(3) C53 0.028(4) 0.081(8) 0.021(4) 0.016(4) 0.006(3) -0.013(5) C54 0.029(5) 0.060(7) 0.056(6) 0.041(6) -0.001(4) -0.009(4) C55 0.028(4) 0.028(5) 0.073(7) 0.016(5) -0.010(5) -0.003(4) C56 0.023(4) 0.031(4) 0.046(5) 0.000(4) -0.003(4) -0.002(3) C57 0.031(4) 0.018(3) 0.022(4) -0.005(3) 0.014(3) -0.005(3) C58 0.034(4) 0.026(4) 0.032(4) 0.001(3) 0.016(3) -0.013(3) C59 0.023(4) 0.047(5) 0.027(4) 0.001(4) 0.010(3) -0.009(3) C60 0.023(4) 0.036(4) 0.028(4) 0.001(3) 0.011(3) 0.002(3) C61 0.018(3) 0.026(4) 0.015(3) 0.003(3) -0.001(3) 0.002(3) C62 0.017(3) 0.023(3) 0.014(3) -0.002(2) 0.007(2) -0.004(3) C63 0.020(3) 0.020(3) 0.011(3) -0.005(2) 0.005(2) 0.001(3) C64 0.016(3) 0.028(4) 0.012(3) -0.003(3) 0.005(2) -0.002(3) C65 0.032(4) 0.029(4) 0.023(4) -0.003(3) 0.006(3) 0.009(3) C66 0.022(4) 0.049(5) 0.035(5) -0.003(4) 0.007(3) 0.012(4) C67 0.015(4) 0.082(8) 0.027(4) 0.002(4) 0.006(3) -0.001(4) C68 0.025(4) 0.049(5) 0.032(4) 0.003(4) 0.008(3) -0.014(4) C69 0.019(3) 0.029(4) 0.024(4) -0.007(3) 0.005(3) -0.004(3) C70 0.016(3) 0.030(4) 0.012(3) -0.009(3) 0.004(2) 0.000(3) C71 0.069(7) 0.023(4) 0.030(5) -0.010(3) -0.002(5) 0.001(4) C72 0.077(8) 0.035(5) 0.051(7) -0.021(5) -0.002(6) -0.007(5) C73 0.032(5) 0.073(7) 0.036(5) -0.034(5) 0.010(4) -0.008(5) C74 0.021(4) 0.067(7) 0.026(4) -0.014(4) 0.002(3) 0.000(4) C75 0.024(4) 0.043(5) 0.021(4) -0.005(3) 0.003(3) -0.003(3) C76 0.028(4) 0.040(5) 0.022(4) 0.000(3) 0.008(3) 0.011(3) C77 0.024(4) 0.060(6) 0.033(5) 0.006(4) 0.012(4) 0.013(4) C78 0.031(5) 0.065(7) 0.075(8) 0.003(6) 0.023(5) -0.006(5) C79 0.039(6) 0.039(6) 0.099(10) 0.002(6) 0.026(6) -0.011(4) C80 0.017(3) 0.033(4) 0.013(3) 0.000(3) 0.003(3) 0.001(3) C81 0.036(5) 0.034(5) 0.057(6) -0.006(4) 0.007(5) 0.002(4) C82 0.026(4) 0.022(3) 0.010(3) -0.004(2) 0.002(3) 0.002(3) C83 0.019(3) 0.032(4) 0.015(3) 0.000(3) 0.006(3) 0.006(3) C84 0.034(5) 0.030(5) 0.072(7) 0.016(4) 0.032(5) 0.013(4) C85 0.037(5) 0.049(6) 0.063(7) 0.018(5) 0.028(5) 0.025(4) C86 0.024(4) 0.060(6) 0.033(5) -0.007(4) 0.007(4) 0.007(4) C87 0.018(4) 0.059(7) 0.065(7) -0.014(5) 0.015(4) -0.006(4) C88 0.018(4) 0.037(5) 0.052(6) -0.017(4) 0.012(4) -0.001(3) C89 0.014(3) 0.023(3) 0.011(3) -0.002(2) 0.002(2) 0.001(2) C90 0.028(4) 0.028(4) 0.015(3) 0.000(3) 0.005(3) -0.001(3) C91 0.048(5) 0.029(4) 0.023(4) 0.000(3) 0.010(4) -0.009(4) C92 0.036(5) 0.051(5) 0.020(4) 0.002(4) 0.010(3) -0.016(4) C93 0.030(4) 0.041(5) 0.019(4) -0.005(3) 0.009(3) -0.004(3) C94 0.019(3) 0.032(4) 0.015(3) -0.004(3) 0.004(3) 0.002(3) C95 0.018(3) 0.029(4) 0.016(3) -0.003(3) 0.007(3) -0.003(3) C96 0.016(3) 0.041(5) 0.020(4) -0.002(3) 0.004(3) -0.002(3) C97 0.031(4) 0.053(6) 0.018(4) 0.001(4) 0.007(3) -0.004(4) C98 0.034(4) 0.052(6) 0.021(4) -0.005(4) 0.011(3) 0.008(4) C99 0.038(5) 0.034(4) 0.022(4) -0.011(3) 0.007(3) 0.005(4) C100 0.030(4) 0.026(4) 0.018(3) -0.007(3) 0.008(3) -0.003(3) C101 0.058(6) 0.027(4) 0.021(4) -0.009(3) 0.018(4) -0.009(4) C102 0.037(5) 0.045(5) 0.039(5) 0.002(4) 0.026(4) -0.002(4) C103 0.059(6) 0.035(5) 0.026(4) 0.015(4) 0.023(4) 0.013(4) C104 0.025(3) 0.019(3) 0.017(3) 0.001(3) 0.010(3) 0.002(3) C105 0.042(5) 0.029(4) 0.022(4) 0.002(3) 0.016(3) -0.001(3) C106 0.029(4) 0.077(8) 0.045(6) 0.008(5) 0.027(4) -0.002(5) C107 0.062(6) 0.043(5) 0.024(4) -0.010(4) 0.020(4) 0.002(5) C108 0.067(7) 0.046(6) 0.028(5) 0.008(4) 0.025(5) -0.009(5) Cl1 0.0656(16) 0.0229(10) 0.0545(15) 0.0074(10) 0.0103(12) -0.0105(10) O9 0.069(5) 0.023(3) 0.070(5) 0.001(3) 0.022(4) -0.010(3) O10 0.32(2) 0.059(7) 0.067(7) 0.008(6) 0.053(11) -0.058(10) O11 0.050(5) 0.055(5) 0.116(8) 0.014(5) 0.017(5) 0.000(4) O12 0.050(5) 0.019(3) 0.166(11) -0.003(5) 0.002(6) -0.001(3) Cl2 0.0376(18) 0.0230(14) 0.0385(19) 0.0020(13) -0.0143(15) 0.0002(13) N1 0.038(2) 0.0150(19) 0.029(2) -0.0018(16) 0.0188(18) -0.0003(17) O25 0.038(2) 0.0150(19) 0.029(2) -0.0018(16) 0.0188(18) -0.0003(17) O26 0.038(2) 0.0150(19) 0.029(2) -0.0018(16) 0.0188(18) -0.0003(17) O27 0.038(2) 0.0150(19) 0.029(2) -0.0018(16) 0.0188(18) -0.0003(17) C6A 0.036(8) 0.088(14) 0.037(8) 0.027(8) 0.024(7) 0.023(9) Cl4 0.037(4) 0.021(3) 0.043(4) -0.011(2) 0.032(3) -0.013(2) O21 0.10(3) 0.21(5) 0.07(2) 0.05(3) 0.05(2) -0.01(3) O22 0.036(14) 0.06(2) 0.17(4) -0.03(2) 0.01(2) 0.022(14) O23 0.044(15) 0.042(15) 0.23(4) -0.08(2) 0.02(2) -0.018(12) O24 0.024(10) 0.091(18) 0.047(12) -0.028(12) 0.019(9) -0.030(11) O2W 0.025(10) 0.11(2) 0.042(12) 0.025(13) 0.002(9) -0.015(12) Cl3 0.099(5) 0.0158(17) 0.039(3) 0.0006(18) 0.005(3) -0.014(3) O17 0.049(8) 0.016(5) 0.090(10) -0.004(5) 0.017(7) 0.000(4) O18 0.16(2) 0.026(7) 0.097(15) -0.003(7) 0.053(15) -0.038(11) O19 0.095(12) 0.074(10) 0.079(10) 0.035(8) 0.015(8) 0.040(9) O20 0.17(2) 0.033(8) 0.057(11) -0.004(8) 0.028(13) -0.025(11) Cl3' 0.078(9) 0.019(4) 0.029(6) -0.001(4) 0.004(5) -0.012(5) O18' 0.051(18) 0.053(19) 0.13(3) -0.012(18) -0.017(18) -0.021(14) O19' 0.10(3) 0.016(12) 0.08(2) 0.013(13) 0.03(2) -0.003(17) O20' 0.18(5) 0.040(18) 0.015(13) -0.014(13) 0.03(2) -0.05(3) C3A 0.015(4) 0.039(5) 0.084(8) -0.019(5) 0.009(4) -0.002(4) O3A 0.20(2) 0.083(11) 0.43(4) -0.045(17) 0.22(2) -0.009(12) O4A 0.110(8) 0.078(7) 0.060(6) 0.011(5) 0.029(6) 0.039(6) C4A 0.063(9) 0.145(16) 0.055(8) 0.013(9) 0.024(7) 0.025(10) O5A 0.087(7) 0.088(7) 0.085(7) -0.027(6) 0.043(6) -0.030(6) C5A 0.074(9) 0.061(8) 0.060(8) -0.021(6) 0.019(7) -0.014(7) O7A 0.020(7) 0.053(10) 0.034(8) 0.013(7) 0.014(6) 0.005(6) C8A 0.037(9) 0.059(12) 0.088(16) -0.033(11) 0.028(10) 0.003(8) O9A 0.028(8) 0.088(14) 0.113(17) -0.065(12) -0.004(9) 0.002(8) O2A 0.12(2) 0.071(14) 0.096(17) 0.019(12) 0.079(16) 0.021(13) C2A 0.11(3) 0.18(4) 0.10(3) 0.09(3) 0.07(2) 0.11(3) O1A 0.093(7) 0.097(8) 0.048(5) 0.014(5) 0.018(5) 0.061(6) C1A 0.100(11) 0.065(9) 0.054(8) 0.008(6) 0.008(7) 0.036(8) _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 P9 2.3676(18) . ? Ag1 O27 2.376(8) . ? Ag1 O3 2.382(5) . ? Ag1 O4 2.439(5) . ? Ag1 Ag6 3.0422(8) . ? Ag1 Ag8 3.0865(9) . ? Ag2 P17 2.3679(18) . ? Ag2 O27 2.374(8) . ? Ag2 O2 2.388(5) . ? Ag2 O6 2.436(5) . ? Ag2 Ag5 3.0935(8) . ? Ag2 Ag7 3.1204(8) . ? Ag3 O1 2.193(5) . ? Ag3 P11 2.3512(18) . ? Ag3 O1W 2.457(6) . ? Ag3 Ag6 3.0272(8) . ? Ag4 O1 2.179(5) . ? Ag4 P16 2.3511(18) . ? Ag4 O1W 2.530(6) . ? Ag4 Ag5 3.0547(8) . ? Ag5 O2 2.254(5) . ? Ag5 O6 2.283(5) . ? Ag5 P13 2.3384(18) . ? Ag6 O3 2.252(5) . ? Ag6 O4 2.273(5) . ? Ag6 P15 2.3334(18) . ? Ag7 O5 2.161(5) . ? Ag7 P18 2.3328(18) . ? Ag8 O5 2.165(5) . ? Ag8 P12 2.3373(19) . ? P9 C7 1.820(7) . ? P9 C1 1.825(7) . ? P9 C13 1.832(7) . ? P10 O2 1.524(5) . ? P10 O3 1.524(5) . ? P10 O1 1.558(5) . ? P10 C104 1.821(7) . ? P11 C39 1.812(7) . ? P11 C45 1.821(7) . ? P11 C38 1.841(7) . ? P12 C20 1.814(7) . ? P12 C14 1.825(7) . ? P12 C13 1.845(7) . ? P13 C80 1.821(7) . ? P13 C70 1.822(7) . ? P13 C82 1.841(7) . ? P14 O6 1.518(5) . ? P14 O4 1.523(5) . ? P14 O5 1.556(5) . ? P14 C105 1.822(8) . ? P15 C32 1.816(7) . ? P15 C26 1.821(7) . ? P15 C38 1.833(7) . ? P16 C83 1.808(7) . ? P16 C89 1.817(7) . ? P16 C82 1.841(7) . ? P17 C62 1.817(7) . ? P17 C51 1.825(7) . ? P17 C63 1.832(7) . ? P18 C64 1.811(7) . ? P18 C95 1.833(7) . ? P18 C63 1.836(7) . ? C1 C6 1.389(11) . ? C1 C2 1.393(10) . ? C2 C3 1.389(12) . ? C3 C4 1.387(16) . ? C4 C5 1.375(15) . ? C5 C6 1.395(12) . ? C7 C12 1.388(10) . ? C7 C8 1.396(11) . ? C8 C9 1.397(11) . ? C9 C10 1.371(14) . ? C10 C11 1.395(14) . ? C11 C12 1.390(11) . ? C14 C15 1.387(10) . ? C14 C19 1.402(10) . ? C15 C16 1.392(11) . ? C16 C17 1.391(13) . ? C17 C18 1.376(13) . ? C18 C19 1.387(11) . ? C20 C21 1.398(12) . ? C20 C25 1.404(12) . ? C21 C22 1.393(13) . ? C22 C23 1.357(19) . ? C23 C24 1.390(19) . ? C24 C25 1.393(14) . ? C26 C27 1.377(13) . ? C26 C31 1.394(11) . ? C27 C28 1.398(13) . ? C28 C29 1.360(16) . ? C29 C30 1.368(16) . ? C30 C31 1.400(12) . ? C32 C33 1.358(11) . ? C32 C37 1.428(11) . ? C33 C34 1.398(13) . ? C34 C35 1.383(16) . ? C35 C36 1.356(16) . ? C36 C37 1.395(12) . ? C39 C44 1.397(10) . ? C39 C40 1.403(10) . ? C40 C41 1.380(11) . ? C41 C42 1.370(13) . ? C42 C43 1.390(13) . ? C43 C44 1.394(11) . ? C45 C50 1.391(12) . ? C45 C46 1.406(12) . ? C46 C47 1.405(12) . ? C47 C48 1.356(16) . ? C48 C49 1.389(17) . ? C49 C50 1.398(13) . ? C51 C56 1.396(12) . ? C51 C52 1.408(11) . ? C52 C53 1.393(13) . ? C53 C54 1.382(17) . ? C54 C55 1.377(17) . ? C55 C56 1.399(12) . ? C57 C58 1.382(10) . ? C57 C62 1.407(10) . ? C58 C59 1.382(12) . ? C59 C60 1.390(12) . ? C60 C61 1.381(11) . ? C61 C62 1.391(10) . ? C64 C65 1.401(10) . ? C64 C69 1.404(11) . ? C65 C66 1.378(12) . ? C66 C67 1.385(15) . ? C67 C68 1.379(14) . ? C68 C69 1.381(11) . ? C70 C71 1.374(12) . ? C70 C75 1.390(11) . ? C71 C72 1.402(13) . ? C72 C73 1.366(16) . ? C73 C74 1.360(16) . ? C74 C75 1.393(12) . ? C76 C77 1.368(12) . ? C76 C80 1.393(11) . ? C77 C78 1.387(16) . ? C78 C79 1.351(16) . ? C79 C81 1.387(15) . ? C80 C81 1.401(12) . ? C83 C88 1.376(12) . ? C83 C84 1.395(11) . ? C84 C85 1.396(12) . ? C85 C86 1.370(15) . ? C86 C87 1.372(15) . ? C87 C88 1.404(11) . ? C89 C94 1.396(9) . ? C89 C90 1.399(10) . ? C90 C91 1.388(11) . ? C91 C92 1.385(12) . ? C92 C93 1.383(13) . ? C93 C94 1.396(11) . ? C95 C100 1.392(11) . ? C95 C96 1.395(11) . ? C96 C97 1.387(11) . ? C97 C98 1.382(13) . ? C98 C99 1.390(13) . ? C99 C100 1.398(10) . ? C101 C104 1.533(10) . ? C102 C104 1.529(11) . ? C103 C104 1.528(10) . ? C105 C108 1.528(12) . ? C105 C106 1.531(13) . ? C105 C107 1.537(12) . ? Cl1 O10 1.398(8) . ? Cl1 O9 1.412(6) . ? Cl1 O12 1.414(7) . ? Cl1 O11 1.453(7) . ? Cl2 O14 1.380(9) . ? Cl2 O13 1.406(9) . ? Cl2 O15 1.418(10) . ? Cl2 O16 1.472(9) . ? N1 O27 1.087(13) . ? N1 O25 1.297(12) . ? N1 O26 1.305(12) . ? C6A O6A 1.22(4) . ? Cl2' O15' 1.398(13) . ? Cl2' O13' 1.416(12) . ? Cl2' O16' 1.426(13) . ? Cl2' O14' 1.434(14) . ? Cl4 O24 1.409(11) . ? Cl4 O22 1.413(12) . ? Cl4 O23 1.419(12) . ? Cl4 O21 1.426(12) . ? Cl3 O20 1.408(11) . ? Cl3 O18 1.419(10) . ? Cl3 O17 1.424(9) . ? Cl3 O19 1.437(11) . ? Cl3' O17' 1.414(13) . ? Cl3' O19' 1.415(13) . ? Cl3' O20' 1.422(13) . ? Cl3' O18' 1.431(13) . ? C3A O3A 1.32(3) . ? O4A C4A 1.420(19) . ? O5A C5A 1.433(16) . ? O7A C7A 1.43(2) . ? C8A O8A 1.435(18) . ? C9A O9A 1.41(2) . ? O2A C2A 1.34(5) . ? O1A C1A 1.406(15) . ? 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 P9 Ag1 O27 137.4(2) . . ? P9 Ag1 O3 118.83(13) . . ? O27 Ag1 O3 91.6(2) . . ? P9 Ag1 O4 118.30(14) . . ? O27 Ag1 O4 95.4(2) . . ? O3 Ag1 O4 78.03(17) . . ? P9 Ag1 Ag6 98.78(5) . . ? O27 Ag1 Ag6 123.7(2) . . ? O3 Ag1 Ag6 47.14(12) . . ? O4 Ag1 Ag6 47.44(12) . . ? P9 Ag1 Ag8 88.56(4) . . ? O27 Ag1 Ag8 81.2(2) . . ? O3 Ag1 Ag8 143.30(12) . . ? O4 Ag1 Ag8 67.03(13) . . ? Ag6 Ag1 Ag8 108.86(2) . . ? P17 Ag2 O27 138.3(2) . . ? P17 Ag2 O2 117.09(13) . . ? O27 Ag2 O2 93.3(2) . . ? P17 Ag2 O6 116.32(14) . . ? O27 Ag2 O6 96.5(2) . . ? O2 Ag2 O6 78.17(17) . . ? P17 Ag2 Ag5 97.54(5) . . ? O27 Ag2 Ag5 124.1(2) . . ? O2 Ag2 Ag5 46.38(12) . . ? O6 Ag2 Ag5 46.93(12) . . ? P17 Ag2 Ag7 88.30(4) . . ? O27 Ag2 Ag7 82.2(2) . . ? O2 Ag2 Ag7 142.78(12) . . ? O6 Ag2 Ag7 65.80(12) . . ? Ag5 Ag2 Ag7 107.23(2) . . ? O1 Ag3 P11 161.85(13) . . ? O1 Ag3 O1W 77.25(18) . . ? P11 Ag3 O1W 120.48(14) . . ? O1 Ag3 Ag6 73.79(12) . . ? P11 Ag3 Ag6 94.41(5) . . ? O1W Ag3 Ag6 131.46(16) . . ? O1 Ag4 P16 164.12(13) . . ? O1 Ag4 O1W 75.93(18) . . ? P16 Ag4 O1W 119.84(14) . . ? O1 Ag4 Ag5 74.88(13) . . ? P16 Ag4 Ag5 94.12(5) . . ? O1W Ag4 Ag5 130.00(16) . . ? O2 Ag5 O6 84.19(18) . . ? O2 Ag5 P13 143.41(14) . . ? O6 Ag5 P13 128.13(15) . . ? O2 Ag5 Ag4 77.26(13) . . ? O6 Ag5 Ag4 145.15(14) . . ? P13 Ag5 Ag4 80.99(5) . . ? O2 Ag5 Ag2 50.08(12) . . ? O6 Ag5 Ag2 51.22(13) . . ? P13 Ag5 Ag2 133.41(5) . . ? Ag4 Ag5 Ag2 125.99(2) . . ? O3 Ag6 O4 84.24(19) . . ? O3 Ag6 P15 144.15(14) . . ? O4 Ag6 P15 126.94(15) . . ? O3 Ag6 Ag3 79.56(12) . . ? O4 Ag6 Ag3 145.52(15) . . ? P15 Ag6 Ag3 80.63(5) . . ? O3 Ag6 Ag1 50.85(12) . . ? O4 Ag6 Ag1 52.21(13) . . ? P15 Ag6 Ag1 130.99(5) . . ? Ag3 Ag6 Ag1 128.72(2) . . ? O5 Ag7 P18 162.99(15) . . ? O5 Ag7 Ag2 80.77(13) . . ? P18 Ag7 Ag2 90.57(5) . . ? O5 Ag8 P12 163.21(15) . . ? O5 Ag8 Ag1 82.01(13) . . ? P12 Ag8 Ag1 90.73(5) . . ? C7 P9 C1 100.9(3) . . ? C7 P9 C13 104.3(3) . . ? C1 P9 C13 104.1(3) . . ? C7 P9 Ag1 117.8(2) . . ? C1 P9 Ag1 114.4(2) . . ? C13 P9 Ag1 113.6(2) . . ? O2 P10 O3 115.0(3) . . ? O2 P10 O1 109.6(3) . . ? O3 P10 O1 109.3(3) . . ? O2 P10 C104 107.7(3) . . ? O3 P10 C104 107.4(3) . . ? O1 P10 C104 107.6(3) . . ? C39 P11 C45 105.0(3) . . ? C39 P11 C38 103.2(3) . . ? C45 P11 C38 106.3(3) . . ? C39 P11 Ag3 113.0(2) . . ? C45 P11 Ag3 116.7(3) . . ? C38 P11 Ag3 111.5(2) . . ? C20 P12 C14 106.8(3) . . ? C20 P12 C13 106.9(3) . . ? C14 P12 C13 102.0(3) . . ? C20 P12 Ag8 114.3(3) . . ? C14 P12 Ag8 112.3(2) . . ? C13 P12 Ag8 113.6(2) . . ? C80 P13 C70 104.3(3) . . ? C80 P13 C82 104.7(3) . . ? C70 P13 C82 105.0(3) . . ? C80 P13 Ag5 116.8(3) . . ? C70 P13 Ag5 111.1(2) . . ? C82 P13 Ag5 114.0(2) . . ? O6 P14 O4 115.9(3) . . ? O6 P14 O5 108.8(3) . . ? O4 P14 O5 108.8(3) . . ? O6 P14 C105 108.1(4) . . ? O4 P14 C105 108.1(3) . . ? O5 P14 C105 106.7(4) . . ? C32 P15 C26 105.5(3) . . ? C32 P15 C38 104.4(3) . . ? C26 P15 C38 105.4(3) . . ? C32 P15 Ag6 115.6(3) . . ? C26 P15 Ag6 110.8(2) . . ? C38 P15 Ag6 114.3(2) . . ? C83 P16 C89 104.8(3) . . ? C83 P16 C82 105.8(3) . . ? C89 P16 C82 103.3(3) . . ? C83 P16 Ag4 115.7(3) . . ? C89 P16 Ag4 114.4(2) . . ? C82 P16 Ag4 111.7(2) . . ? C62 P17 C51 101.8(3) . . ? C62 P17 C63 103.7(3) . . ? C51 P17 C63 104.4(3) . . ? C62 P17 Ag2 118.1(2) . . ? C51 P17 Ag2 113.7(2) . . ? C63 P17 Ag2 113.5(2) . . ? C64 P18 C95 107.8(3) . . ? C64 P18 C63 106.7(3) . . ? C95 P18 C63 100.7(3) . . ? C64 P18 Ag7 113.8(2) . . ? C95 P18 Ag7 113.3(3) . . ? C63 P18 Ag7 113.5(2) . . ? P10 O1 Ag4 122.2(3) . . ? P10 O1 Ag3 124.7(3) . . ? Ag4 O1 Ag3 112.7(2) . . ? P10 O2 Ag5 118.3(3) . . ? P10 O2 Ag2 139.1(3) . . ? Ag5 O2 Ag2 83.53(16) . . ? P10 O3 Ag6 116.7(3) . . ? P10 O3 Ag1 141.8(3) . . ? Ag6 O3 Ag1 82.01(15) . . ? P14 O4 Ag6 145.1(3) . . ? P14 O4 Ag1 118.9(3) . . ? Ag6 O4 Ag1 80.34(16) . . ? P14 O5 Ag7 115.3(3) . . ? P14 O5 Ag8 116.2(3) . . ? Ag7 O5 Ag8 127.1(2) . . ? P14 O6 Ag5 142.9(3) . . ? P14 O6 Ag2 117.8(3) . . ? Ag5 O6 Ag2 81.85(16) . . ? Ag3 O1W Ag4 93.8(2) . . ? C6 C1 C2 119.8(7) . . ? C6 C1 P9 123.4(6) . . ? C2 C1 P9 116.6(6) . . ? C3 C2 C1 120.1(8) . . ? C4 C3 C2 119.4(9) . . ? C5 C4 C3 120.9(8) . . ? C4 C5 C6 119.8(9) . . ? C1 C6 C5 119.9(8) . . ? C12 C7 C8 120.4(7) . . ? C12 C7 P9 119.4(6) . . ? C8 C7 P9 120.1(6) . . ? C7 C8 C9 119.7(8) . . ? C10 C9 C8 119.8(8) . . ? C9 C10 C11 120.6(8) . . ? C12 C11 C10 120.1(8) . . ? C7 C12 C11 119.3(8) . . ? P9 C13 P12 112.6(3) . . ? C15 C14 C19 119.5(7) . . ? C15 C14 P12 118.3(5) . . ? C19 C14 P12 122.3(5) . . ? C14 C15 C16 120.2(7) . . ? C17 C16 C15 120.0(8) . . ? C18 C17 C16 119.8(8) . . ? C17 C18 C19 120.8(8) . . ? C18 C19 C14 119.7(8) . . ? C21 C20 C25 120.1(8) . . ? C21 C20 P12 122.7(6) . . ? C25 C20 P12 117.1(7) . . ? C22 C21 C20 118.8(10) . . ? C23 C22 C21 121.6(12) . . ? C22 C23 C24 120.1(9) . . ? C23 C24 C25 120.3(10) . . ? C24 C25 C20 119.1(11) . . ? C27 C26 C31 119.6(8) . . ? C27 C26 P15 123.9(6) . . ? C31 C26 P15 116.4(7) . . ? C26 C27 C28 119.3(10) . . ? C29 C28 C27 120.9(11) . . ? C28 C29 C30 120.6(9) . . ? C29 C30 C31 119.6(9) . . ? C26 C31 C30 120.0(9) . . ? C33 C32 C37 120.4(7) . . ? C33 C32 P15 120.8(6) . . ? C37 C32 P15 118.7(6) . . ? C32 C33 C34 120.0(9) . . ? C35 C34 C33 119.6(10) . . ? C36 C35 C34 121.1(9) . . ? C35 C36 C37 120.6(9) . . ? C36 C37 C32 118.2(9) . . ? P15 C38 P11 109.5(4) . . ? C44 C39 C40 119.1(7) . . ? C44 C39 P11 122.3(5) . . ? C40 C39 P11 118.6(6) . . ? C41 C40 C39 120.4(7) . . ? C42 C41 C40 120.3(8) . . ? C41 C42 C43 120.6(8) . . ? C42 C43 C44 119.8(8) . . ? C43 C44 C39 119.9(7) . . ? C50 C45 C46 120.5(7) . . ? C50 C45 P11 117.7(6) . . ? C46 C45 P11 121.6(6) . . ? C47 C46 C45 118.9(9) . . ? C48 C47 C46 120.6(10) . . ? C47 C48 C49 120.5(9) . . ? C48 C49 C50 120.6(10) . . ? C45 C50 C49 118.8(10) . . ? C56 C51 C52 120.7(7) . . ? C56 C51 P17 122.7(6) . . ? C52 C51 P17 116.7(6) . . ? C53 C52 C51 118.4(9) . . ? C54 C53 C52 120.8(9) . . ? C55 C54 C53 120.5(9) . . ? C54 C55 C56 120.3(10) . . ? C51 C56 C55 119.0(9) . . ? C58 C57 C62 120.4(7) . . ? C59 C58 C57 120.1(8) . . ? C58 C59 C60 120.0(7) . . ? C61 C60 C59 120.3(8) . . ? C60 C61 C62 120.4(7) . . ? C61 C62 C57 118.9(6) . . ? C61 C62 P17 119.7(5) . . ? C57 C62 P17 121.4(5) . . ? P17 C63 P18 113.9(4) . . ? C65 C64 C69 118.9(7) . . ? C65 C64 P18 117.6(6) . . ? C69 C64 P18 123.5(6) . . ? C66 C65 C64 120.2(8) . . ? C65 C66 C67 120.2(8) . . ? C68 C67 C66 120.3(8) . . ? C67 C68 C69 120.2(9) . . ? C68 C69 C64 120.1(8) . . ? C71 C70 C75 119.4(7) . . ? C71 C70 P13 123.9(6) . . ? C75 C70 P13 116.7(6) . . ? C70 C71 C72 119.8(9) . . ? C73 C72 C71 120.6(10) . . ? C74 C73 C72 119.7(9) . . ? C73 C74 C75 120.9(9) . . ? C70 C75 C74 119.6(9) . . ? C77 C76 C80 121.0(9) . . ? C76 C77 C78 119.1(9) . . ? C79 C78 C77 121.4(10) . . ? C78 C79 C81 120.2(10) . . ? C76 C80 C81 118.7(8) . . ? C76 C80 P13 120.8(6) . . ? C81 C80 P13 120.5(6) . . ? C79 C81 C80 119.6(9) . . ? P16 C82 P13 110.0(4) . . ? C88 C83 C84 119.9(7) . . ? C88 C83 P16 118.9(6) . . ? C84 C83 P16 121.2(6) . . ? C83 C84 C85 118.9(9) . . ? C86 C85 C84 120.9(9) . . ? C85 C86 C87 120.5(8) . . ? C86 C87 C88 119.3(10) . . ? C83 C88 C87 120.4(9) . . ? C94 C89 C90 119.9(7) . . ? C94 C89 P16 118.1(6) . . ? C90 C89 P16 122.0(5) . . ? C91 C90 C89 119.5(7) . . ? C92 C91 C90 120.6(8) . . ? C93 C92 C91 120.1(8) . . ? C92 C93 C94 120.2(8) . . ? C93 C94 C89 119.7(7) . . ? C100 C95 C96 120.5(7) . . ? C100 C95 P18 121.3(6) . . ? C96 C95 P18 118.1(6) . . ? C97 C96 C95 119.6(8) . . ? C98 C97 C96 120.1(8) . . ? C97 C98 C99 120.8(8) . . ? C98 C99 C100 119.6(8) . . ? C95 C100 C99 119.5(8) . . ? C103 C104 C102 109.7(7) . . ? C103 C104 C101 109.6(7) . . ? C102 C104 C101 109.7(7) . . ? C103 C104 P10 110.3(5) . . ? C102 C104 P10 107.8(5) . . ? C101 C104 P10 109.7(5) . . ? C108 C105 C106 111.0(8) . . ? C108 C105 C107 107.5(7) . . ? C106 C105 C107 110.4(8) . . ? C108 C105 P14 110.0(6) . . ? C106 C105 P14 108.4(6) . . ? C107 C105 P14 109.5(6) . . ? O10 Cl1 O9 111.3(5) . . ? O10 Cl1 O12 111.6(6) . . ? O9 Cl1 O12 111.0(5) . . ? O10 Cl1 O11 108.7(7) . . ? O9 Cl1 O11 107.2(5) . . ? O12 Cl1 O11 106.8(5) . . ? O14 Cl2 O13 120.7(8) . . ? O14 Cl2 O15 110.0(8) . . ? O13 Cl2 O15 111.2(7) . . ? O14 Cl2 O16 102.8(7) . . ? O13 Cl2 O16 103.1(7) . . ? O15 Cl2 O16 107.7(7) . . ? O27 N1 O25 122.6(10) . . ? O27 N1 O26 124.2(10) . . ? O25 N1 O26 113.2(9) . . ? N1 O27 Ag2 113.8(7) . . ? N1 O27 Ag1 112.2(7) . . ? Ag2 O27 Ag1 120.2(4) . . ? O15' Cl2' O13' 112.8(14) . . ? O15' Cl2' O16' 114.8(19) . . ? O13' Cl2' O16' 109.0(18) . . ? O15' Cl2' O14' 101.6(17) . . ? O13' Cl2' O14' 112.2(18) . . ? O16' Cl2' O14' 106.1(19) . . ? O24 Cl4 O22 113.3(15) . . ? O24 Cl4 O23 110.2(13) . . ? O22 Cl4 O23 106.5(15) . . ? O24 Cl4 O21 107.8(14) . . ? O22 Cl4 O21 110.0(17) . . ? O23 Cl4 O21 109.0(17) . . ? O20 Cl3 O18 111.3(11) . . ? O20 Cl3 O17 110.7(10) . . ? O18 Cl3 O17 111.6(11) . . ? O20 Cl3 O19 107.5(11) . . ? O18 Cl3 O19 106.8(10) . . ? O17 Cl3 O19 108.7(9) . . ? O17' Cl3' O19' 111.2(17) . . ? O17' Cl3' O20' 107.6(16) . . ? O19' Cl3' O20' 111.5(19) . . ? O17' Cl3' O18' 112.0(16) . . ? O19' Cl3' O18' 107.3(16) . . ? O20' Cl3' O18' 107.2(17) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.963 _refine_diff_density_min -2.389 _refine_diff_density_rms 0.185 _database_code_depnum_ccdc_archive 'CCDC 936238' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Ag2 N O5 P2' _chemical_formula_weight 552.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' 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' 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' _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 6.0537(9) _cell_length_b 11.2351(16) _cell_length_c 12.7177(18) _cell_angle_alpha 80.978(3) _cell_angle_beta 88.194(2) _cell_angle_gamma 85.894(2) _cell_volume 851.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 2.510 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7039 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.01 _reflns_number_total 4001 _reflns_number_gt 3124 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2(Bruker,2003) _computing_cell_refinement SAINT(Bruker,2001) _computing_data_reduction APEX2(Bruker,2003) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+0.9484P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4001 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.21137(5) 0.47476(3) 0.41188(2) 0.04183(9) Uani 1 1 d . . . Ag2 Ag 0.28175(5) 0.71889(3) 0.47857(2) 0.04578(10) Uani 1 1 d . . . P1 P 0.22185(14) 0.33410(7) 0.66276(6) 0.02840(18) Uani 1 1 d . . . P2 P 0.28513(14) 0.57100(8) 0.71801(6) 0.02901(18) Uani 1 1 d . . . O1 O 0.2706(4) 0.4251(2) 0.74325(17) 0.0344(5) Uani 1 1 d . . . O2 O -0.0234(4) 0.3381(2) 0.6462(2) 0.0423(6) Uani 1 1 d . . . O3 O 0.3657(4) 0.3610(2) 0.56496(19) 0.0453(6) Uani 1 1 d . . . O4 O 0.5206(4) 0.5988(2) 0.6975(2) 0.0416(6) Uani 1 1 d . . . O5 O 0.1222(4) 0.6197(2) 0.63241(18) 0.0383(6) Uani 1 1 d . . . N N 0.2631(7) 0.9215(3) 0.4545(3) 0.0610(10) Uani 1 1 d . . . C1 C 0.3114(6) 0.1919(3) 0.7380(3) 0.0319(7) Uani 1 1 d . . . C2 C 0.5182(7) 0.1734(4) 0.7850(3) 0.0459(9) Uani 1 1 d . . . H2 H 0.6128 0.2360 0.7772 0.055 Uiso 1 1 calc R . . C3 C 0.5842(8) 0.0629(4) 0.8431(4) 0.0632(13) Uani 1 1 d . . . H3 H 0.7210 0.0522 0.8758 0.076 Uiso 1 1 calc R . . C4 C 0.4496(10) -0.0309(4) 0.8527(4) 0.0766(16) Uani 1 1 d . . . H4 H 0.4956 -0.1053 0.8914 0.092 Uiso 1 1 calc R . . C5 C 0.2468(10) -0.0158(4) 0.8055(5) 0.0839(17) Uani 1 1 d . . . H5 H 0.1556 -0.0799 0.8118 0.101 Uiso 1 1 calc R . . C6 C 0.1784(8) 0.0953(4) 0.7484(4) 0.0595(12) Uani 1 1 d . . . H6 H 0.0408 0.1052 0.7164 0.071 Uiso 1 1 calc R . . C7 C 0.1952(5) 0.6160(3) 0.8427(3) 0.0316(7) Uani 1 1 d . . . C8 C -0.0230(6) 0.6493(4) 0.8648(3) 0.0497(10) Uani 1 1 d . . . H8 H -0.1310 0.6466 0.8149 0.060 Uiso 1 1 calc R . . C9 C -0.0814(7) 0.6870(4) 0.9616(4) 0.0607(12) Uani 1 1 d . . . H9 H -0.2280 0.7118 0.9753 0.073 Uiso 1 1 calc R . . C10 C 0.0747(8) 0.6879(4) 1.0367(3) 0.0596(12) Uani 1 1 d . . . H10 H 0.0339 0.7115 1.1018 0.071 Uiso 1 1 calc R . . C11 C 0.3510(7) 0.6188(4) 0.9193(3) 0.0563(11) Uani 1 1 d . . . H11 H 0.4987 0.5966 0.9054 0.068 Uiso 1 1 calc R . . C12 C 0.2910(9) 0.6540(5) 1.0158(4) 0.0734(15) Uani 1 1 d . . . H12 H 0.3976 0.6547 1.0668 0.088 Uiso 1 1 calc R . . C13 C 0.2591(7) 1.0210(4) 0.4263(4) 0.0525(10) Uani 1 1 d . . . C14 C 0.2535(10) 1.1502(4) 0.3906(5) 0.0751(15) Uani 1 1 d . . . H14A H 0.2286 1.1919 0.4508 0.113 Uiso 1 1 calc R . . H14B H 0.1360 1.1735 0.3411 0.113 Uiso 1 1 calc R . . H14C H 0.3923 1.1708 0.3565 0.113 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 0.03744(15) 0.04086(17) 0.04578(17) -0.00530(12) -0.00458(12) 0.00553(12) Ag2 0.04640(17) 0.04258(18) 0.04705(18) -0.00138(13) 0.00183(13) -0.00755(13) P1 0.0309(4) 0.0271(4) 0.0272(4) -0.0060(3) -0.0020(3) 0.0024(3) P2 0.0304(4) 0.0276(4) 0.0291(4) -0.0039(3) 0.0013(3) -0.0044(3) O1 0.0462(14) 0.0264(12) 0.0308(12) -0.0041(9) -0.0056(10) -0.0030(10) O2 0.0346(13) 0.0362(14) 0.0570(16) -0.0097(12) -0.0112(12) 0.0020(11) O3 0.0523(15) 0.0473(15) 0.0310(12) 0.0011(11) 0.0074(11) 0.0134(13) O4 0.0336(13) 0.0496(15) 0.0449(14) -0.0155(12) 0.0067(11) -0.0102(11) O5 0.0391(13) 0.0378(13) 0.0354(12) 0.0033(10) -0.0032(10) -0.0042(11) N 0.067(2) 0.039(2) 0.079(3) -0.0125(19) -0.003(2) -0.0058(18) C1 0.0361(17) 0.0290(17) 0.0301(16) -0.0051(13) 0.0000(14) 0.0018(14) C2 0.048(2) 0.043(2) 0.045(2) -0.0015(17) -0.0099(18) -0.0012(18) C3 0.059(3) 0.061(3) 0.062(3) 0.010(2) -0.015(2) 0.013(2) C4 0.087(4) 0.043(3) 0.089(4) 0.020(2) -0.004(3) 0.009(3) C5 0.084(4) 0.040(3) 0.122(5) 0.012(3) -0.014(4) -0.016(3) C6 0.055(3) 0.039(2) 0.082(3) 0.002(2) -0.014(2) -0.007(2) C7 0.0355(17) 0.0261(16) 0.0339(17) -0.0062(13) 0.0032(14) -0.0051(14) C8 0.039(2) 0.064(3) 0.048(2) -0.016(2) 0.0008(17) -0.0005(19) C9 0.045(2) 0.080(3) 0.061(3) -0.027(2) 0.018(2) 0.000(2) C10 0.067(3) 0.072(3) 0.049(2) -0.031(2) 0.018(2) -0.021(2) C11 0.042(2) 0.085(3) 0.047(2) -0.030(2) -0.0010(18) -0.002(2) C12 0.063(3) 0.117(5) 0.051(3) -0.043(3) -0.001(2) -0.015(3) C13 0.052(2) 0.039(2) 0.069(3) -0.015(2) -0.005(2) -0.0026(19) C14 0.086(4) 0.037(2) 0.100(4) -0.006(3) -0.009(3) 0.001(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 O4 2.297(2) 2_666 ? Ag1 O3 2.336(2) . ? Ag1 O2 2.342(2) 2_566 ? Ag1 O5 2.467(2) 2_566 ? Ag1 Ag2 3.0568(6) . ? Ag2 N 2.244(4) . ? Ag2 O5 2.314(2) . ? Ag2 O3 2.340(3) 2_666 ? Ag2 O2 2.448(2) 2_566 ? P1 O3 1.500(3) . ? P1 O2 1.502(2) . ? P1 O1 1.603(2) . ? P1 C1 1.786(3) . ? P2 O4 1.487(2) . ? P2 O5 1.504(2) . ? P2 O1 1.628(2) . ? P2 C7 1.795(3) . ? O2 Ag1 2.342(2) 2_566 ? O2 Ag2 2.448(2) 2_566 ? O3 Ag2 2.340(3) 2_666 ? O4 Ag1 2.297(2) 2_666 ? O5 Ag1 2.467(2) 2_566 ? N C13 1.118(5) . ? C1 C6 1.385(5) . ? C1 C2 1.392(5) . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.365(7) . ? C3 H3 0.9300 . ? C4 C5 1.372(7) . ? C4 H4 0.9300 . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.379(5) . ? C7 C11 1.383(5) . ? C8 C9 1.391(6) . ? C8 H8 0.9300 . ? C9 C10 1.366(6) . ? C9 H9 0.9300 . ? C10 C12 1.367(7) . ? C10 H10 0.9300 . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.449(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 O4 Ag1 O3 92.71(9) 2_666 . ? O4 Ag1 O2 118.85(9) 2_666 2_566 ? O3 Ag1 O2 140.88(9) . 2_566 ? O4 Ag1 O5 102.81(8) 2_666 2_566 ? O3 Ag1 O5 108.88(9) . 2_566 ? O2 Ag1 O5 87.32(8) 2_566 2_566 ? O4 Ag1 Ag2 116.60(6) 2_666 . ? O3 Ag1 Ag2 94.76(7) . . ? O2 Ag1 Ag2 51.89(6) 2_566 . ? O5 Ag1 Ag2 132.78(6) 2_566 . ? N Ag2 O5 117.81(12) . . ? N Ag2 O3 111.61(12) . 2_666 ? O5 Ag2 O3 114.93(9) . 2_666 ? N Ag2 O2 106.48(12) . 2_566 ? O5 Ag2 O2 96.87(9) . 2_566 ? O3 Ag2 O2 107.09(9) 2_666 2_566 ? N Ag2 Ag1 153.65(10) . . ? O5 Ag2 Ag1 79.08(6) . . ? O3 Ag2 Ag1 74.27(7) 2_666 . ? O2 Ag2 Ag1 48.83(6) 2_566 . ? O3 P1 O2 116.72(15) . . ? O3 P1 O1 108.72(15) . . ? O2 P1 O1 109.18(14) . . ? O3 P1 C1 110.23(15) . . ? O2 P1 C1 109.49(15) . . ? O1 P1 C1 101.39(13) . . ? O4 P2 O5 117.53(15) . . ? O4 P2 O1 109.10(14) . . ? O5 P2 O1 107.73(13) . . ? O4 P2 C7 108.81(15) . . ? O5 P2 C7 110.61(15) . . ? O1 P2 C7 101.90(13) . . ? P1 O1 P2 128.53(14) . . ? P1 O2 Ag1 118.51(14) . 2_566 ? P1 O2 Ag2 139.22(15) . 2_566 ? Ag1 O2 Ag2 79.27(7) 2_566 2_566 ? P1 O3 Ag1 118.94(15) . . ? P1 O3 Ag2 131.30(14) . 2_666 ? Ag1 O3 Ag2 108.78(9) . 2_666 ? P2 O4 Ag1 131.43(15) . 2_666 ? P2 O5 Ag2 113.99(13) . . ? P2 O5 Ag1 127.17(13) . 2_566 ? Ag2 O5 Ag1 109.78(9) . 2_566 ? C13 N Ag2 169.2(4) . . ? C6 C1 C2 118.0(3) . . ? C6 C1 P1 120.5(3) . . ? C2 C1 P1 121.5(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 119.7(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 121.1(4) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C11 118.5(3) . . ? C8 C7 P2 122.7(3) . . ? C11 C7 P2 118.8(3) . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C12 C10 C9 119.9(4) . . ? C12 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C12 C11 C7 121.1(4) . . ? C12 C11 H11 119.5 . . ? C7 C11 H11 119.5 . . ? C10 C12 C11 120.0(4) . . ? C10 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N C13 C14 179.5(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ag1 Ag2 N 83.4(2) 2_666 . . . ? O3 Ag1 Ag2 N 178.9(2) . . . . ? O2 Ag1 Ag2 N -23.6(2) 2_566 . . . ? O5 Ag1 Ag2 N -59.8(2) 2_566 . . . ? O4 Ag1 Ag2 O5 -143.65(10) 2_666 . . . ? O3 Ag1 Ag2 O5 -48.21(9) . . . . ? O2 Ag1 Ag2 O5 109.31(10) 2_566 . . . ? O5 Ag1 Ag2 O5 73.09(10) 2_566 . . . ? O4 Ag1 Ag2 O3 -23.63(10) 2_666 . . 2_666 ? O3 Ag1 Ag2 O3 71.81(10) . . . 2_666 ? O2 Ag1 Ag2 O3 -130.67(10) 2_566 . . 2_666 ? O5 Ag1 Ag2 O3 -166.89(9) 2_566 . . 2_666 ? O4 Ag1 Ag2 O2 107.04(11) 2_666 . . 2_566 ? O3 Ag1 Ag2 O2 -157.52(11) . . . 2_566 ? O5 Ag1 Ag2 O2 -36.22(11) 2_566 . . 2_566 ? O3 P1 O1 P2 47.7(2) . . . . ? O2 P1 O1 P2 -80.6(2) . . . . ? C1 P1 O1 P2 163.9(2) . . . . ? O4 P2 O1 P1 -94.8(2) . . . . ? O5 P2 O1 P1 33.8(2) . . . . ? C7 P2 O1 P1 150.2(2) . . . . ? O3 P1 O2 Ag1 -68.7(2) . . . 2_566 ? O1 P1 O2 Ag1 55.08(18) . . . 2_566 ? C1 P1 O2 Ag1 165.26(15) . . . 2_566 ? O3 P1 O2 Ag2 39.1(3) . . . 2_566 ? O1 P1 O2 Ag2 162.86(19) . . . 2_566 ? C1 P1 O2 Ag2 -87.0(2) . . . 2_566 ? O2 P1 O3 Ag1 23.3(2) . . . . ? O1 P1 O3 Ag1 -100.70(17) . . . . ? C1 P1 O3 Ag1 148.99(16) . . . . ? O2 P1 O3 Ag2 -144.03(18) . . . 2_666 ? O1 P1 O3 Ag2 92.0(2) . . . 2_666 ? C1 P1 O3 Ag2 -18.3(3) . . . 2_666 ? O4 Ag1 O3 P1 -157.99(17) 2_666 . . . ? O2 Ag1 O3 P1 56.5(2) 2_566 . . . ? O5 Ag1 O3 P1 -53.46(19) 2_566 . . . ? Ag2 Ag1 O3 P1 85.03(17) . . . . ? O4 Ag1 O3 Ag2 11.98(12) 2_666 . . 2_666 ? O2 Ag1 O3 Ag2 -133.49(12) 2_566 . . 2_666 ? O5 Ag1 O3 Ag2 116.50(11) 2_566 . . 2_666 ? Ag2 Ag1 O3 Ag2 -105.01(10) . . . 2_666 ? O5 P2 O4 Ag1 -73.6(2) . . . 2_666 ? O1 P2 O4 Ag1 49.4(2) . . . 2_666 ? C7 P2 O4 Ag1 159.76(18) . . . 2_666 ? O4 P2 O5 Ag2 4.0(2) . . . . ? O1 P2 O5 Ag2 -119.61(14) . . . . ? C7 P2 O5 Ag2 129.81(15) . . . . ? O4 P2 O5 Ag1 147.37(16) . . . 2_566 ? O1 P2 O5 Ag1 23.7(2) . . . 2_566 ? C7 P2 O5 Ag1 -86.86(19) . . . 2_566 ? N Ag2 O5 P2 -100.20(18) . . . . ? O3 Ag2 O5 P2 34.57(18) 2_666 . . . ? O2 Ag2 O5 P2 147.05(15) 2_566 . . . ? Ag1 Ag2 O5 P2 101.36(14) . . . . ? N Ag2 O5 Ag1 110.18(14) . . . 2_566 ? O3 Ag2 O5 Ag1 -115.05(11) 2_666 . . 2_566 ? O2 Ag2 O5 Ag1 -2.57(11) 2_566 . . 2_566 ? Ag1 Ag2 O5 Ag1 -48.26(8) . . . 2_566 ? O5 Ag2 N C13 -159(2) . . . . ? O3 Ag2 N C13 65(2) 2_666 . . . ? O2 Ag2 N C13 -51(2) 2_566 . . . ? Ag1 Ag2 N C13 -33(2) . . . . ? O3 P1 C1 C6 -113.2(3) . . . . ? O2 P1 C1 C6 16.5(4) . . . . ? O1 P1 C1 C6 131.8(3) . . . . ? O3 P1 C1 C2 64.8(3) . . . . ? O2 P1 C1 C2 -165.5(3) . . . . ? O1 P1 C1 C2 -50.2(3) . . . . ? C6 C1 C2 C3 -2.1(6) . . . . ? P1 C1 C2 C3 179.8(3) . . . . ? C1 C2 C3 C4 1.8(7) . . . . ? C2 C3 C4 C5 -0.5(9) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? C2 C1 C6 C5 1.2(7) . . . . ? P1 C1 C6 C5 179.3(4) . . . . ? C4 C5 C6 C1 0.0(9) . . . . ? O4 P2 C7 C8 152.6(3) . . . . ? O5 P2 C7 C8 22.1(4) . . . . ? O1 P2 C7 C8 -92.2(3) . . . . ? O4 P2 C7 C11 -26.6(4) . . . . ? O5 P2 C7 C11 -157.1(3) . . . . ? O1 P2 C7 C11 88.6(3) . . . . ? C11 C7 C8 C9 1.3(6) . . . . ? P2 C7 C8 C9 -177.9(3) . . . . ? C7 C8 C9 C10 -2.0(7) . . . . ? C8 C9 C10 C12 1.4(8) . . . . ? C8 C7 C11 C12 0.0(7) . . . . ? P2 C7 C11 C12 179.2(4) . . . . ? C9 C10 C12 C11 -0.1(8) . . . . ? C7 C11 C12 C10 -0.6(8) . . . . ? Ag2 N C13 C14 178(100) . . . . ? 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 C14 H14C O4 0.96 2.66 3.247(5) 120.0 2_676 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.720 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 936239'