# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. #TrackingRef '- p1-3-r2.cif' _journal_coden_Cambridge 0182 _audit_update_record ; 2010-03-06 # Formatted by publCIF ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Huang, Rongbin State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; _publ_contact_author_phone 86-592-2185191 _publ_contact_author_fax 86-592-2183047 _publ_contact_author_email rbhuang@xmu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) # 3. TITLE AND AUTHOR LIST _publ_section_title ; Simultaneous self-Cassembly of a cage-Clike silver(I) complex encapsulating an Ag6 neutral cluster core and carbon dioxide fixation ; loop_ _publ_author_name _publ_author_address 'Di Sun' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; 'Geng-Geng Luo' ; Insitute of Materials Physical Chemistry, Huaqiao University, Quanzhou, Fujian 362021, China ; 'Na Zhang' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; 'Rong-Bin Huang' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; 'Lan-Sun Zheng' ; State Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, 361005, China ; _publ_section_exptl_refinement ; All H atoms were placed geometrically with C---H distances of 0.93 \%A, N---H distances of 0.86\%A and refined using a riding atom model with their isotropic displacement factors, J~iso~ fixed at 1.2 time the U~eq~ of the parent C and N atom. ; _publ_contact_author_name 'Huang, Rongbin' data_p1 _database_code_depnum_ccdc_archive 'CCDC 743742' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C312 H264 Ag34 Cl4 O36 P24' _chemical_formula_sum 'C312 H264 Ag34 Cl4 O36 P24' _chemical_formula_weight 9141.89 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting CUBIC _symmetry_space_group_name_H-M Fd-3 _symmetry_space_group_name_hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' '-x+1/4, y, -z+1/4' 'x, -y+1/4, -z+1/4' 'z, x, y' 'z, -x+1/4, -y+1/4' '-z+1/4, -x+1/4, y' '-z+1/4, x, -y+1/4' 'y, z, x' '-y+1/4, z, -x+1/4' 'y, -z+1/4, -x+1/4' '-y+1/4, -z+1/4, x' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' '-x+1/4, y+1/2, -z+3/4' 'x, -y+3/4, -z+3/4' 'z, x+1/2, y+1/2' 'z, -x+3/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+1/4, x+1/2, -y+3/4' 'y, z+1/2, x+1/2' '-y+1/4, z+1/2, -x+3/4' 'y, -z+3/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' '-x+3/4, y, -z+3/4' 'x+1/2, -y+1/4, -z+3/4' 'z+1/2, x, y+1/2' 'z+1/2, -x+1/4, -y+3/4' '-z+3/4, -x+1/4, y+1/2' '-z+3/4, x, -y+3/4' 'y+1/2, z, x+1/2' '-y+3/4, z, -x+3/4' 'y+1/2, -z+1/4, -x+3/4' '-y+3/4, -z+1/4, x+1/2' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+3/4, -z+1/4' 'z+1/2, x+1/2, y' 'z+1/2, -x+3/4, -y+1/4' '-z+3/4, -x+3/4, y' '-z+3/4, x+1/2, -y+1/4' 'y+1/2, z+1/2, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+3/4, -x+1/4' '-y+3/4, -z+3/4, x' '-x, -y, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y, z-1/4' '-x, y-1/4, z-1/4' '-z, -x, -y' '-z, x-1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-1/4, -x, y-1/4' '-y, -z, -x' 'y-1/4, -z, x-1/4' '-y, z-1/4, x-1/4' 'y-1/4, z-1/4, -x' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' 'x-1/4, -y+1/2, z+1/4' '-x, y+1/4, z+1/4' '-z, -x+1/2, -y+1/2' '-z, x+1/4, y+1/4' 'z-1/4, x+1/4, -y+1/2' 'z-1/4, -x+1/2, y+1/4' '-y, -z+1/2, -x+1/2' 'y-1/4, -z+1/2, x+1/4' '-y, z+1/4, x+1/4' 'y-1/4, z+1/4, -x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' 'x+1/4, -y, z+1/4' '-x+1/2, y-1/4, z+1/4' '-z+1/2, -x, -y+1/2' '-z+1/2, x-1/4, y+1/4' 'z+1/4, x-1/4, -y+1/2' 'z+1/4, -x, y+1/4' '-y+1/2, -z, -x+1/2' 'y+1/4, -z, x+1/4' '-y+1/2, z-1/4, x+1/4' 'y+1/4, z-1/4, -x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' 'x+1/4, -y+1/2, z-1/4' '-x+1/2, y+1/4, z-1/4' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/4, y-1/4' 'z+1/4, x+1/4, -y' 'z+1/4, -x+1/2, y-1/4' '-y+1/2, -z+1/2, -x' 'y+1/4, -z+1/2, x-1/4' '-y+1/2, z+1/4, x-1/4' 'y+1/4, z+1/4, -x' _cell_length_a 54.274(6) _cell_length_b 54.274(6) _cell_length_c 54.274(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 159876(32) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1897 _cell_measurement_theta_min 4.440 _cell_measurement_theta_max 34.053 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 35600 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7154 _exptl_absorpt_correction_T_max 0.7746 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ? _diffrn_ambient_temperature 173(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 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44892 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.1589 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -64 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 24.99 _reflns_number_total 11717 _reflns_number_gt 2790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal has a very weak high-angle diffraction, therefore not many high angle reflections have been detected. Complex 1 has unusually large voids. The solvent accessible volume is ca. 65.7 % calculated from PLATON software. The voids in the framework are filled with many disordered solvent molecules, which can not be located. Hence reflect on a high R(int) value. In the refinement we used SQEEZE procedure (Spek, A.L. (2008) Utrecht University, Utrecht, The Netherlands) to remove solvent electron density from voids which give a smaller final R(int) and R-value compared with the original R(int) and R-value. The following restrains were applied to the disordered parts: DELU 0.005 C23 C24 ISOR 0.005 C26 ; _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^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11717 _refine_ls_number_parameters 309 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1782 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2328 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.798 _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 0.6250 0.58859(3) 0.6250 0.1153(5) Uani 1 2 d S . . Ag2 Ag 0.62677(2) 0.530114(19) 0.65362(2) 0.1281(4) Uani 1 1 d . . . Ag3 Ag 0.66683(2) 0.52752(2) 0.68955(2) 0.1364(5) Uani 1 1 d . . . Ag4 Ag 0.58593(2) 0.58593(2) 0.66407(2) 0.1242(6) Uani 1 3 d S . . P1 P 0.65487(7) 0.48630(7) 0.69903(7) 0.1166(11) Uani 1 1 d . . . P2 P 0.61041(7) 0.49317(6) 0.66681(7) 0.1096(10) Uani 1 1 d . . . Cl1 Cl 0.70908(6) 0.54092(6) 0.70908(6) 0.1180(17) Uani 1 3 d S . . C1 C 0.7192(3) 0.4339(3) 0.7035(3) 0.141(6) Uani 1 1 d . . . H1A H 0.7331 0.4232 0.7045 0.169 Uiso 1 1 calc R . . C2 C 0.6977(4) 0.4230(3) 0.7012(3) 0.161(6) Uani 1 1 d . . . H2A H 0.6959 0.4057 0.6993 0.193 Uiso 1 1 calc R . . C3 C 0.6787(4) 0.4383(4) 0.7019(3) 0.161(6) Uani 1 1 d . . . H3A H 0.6628 0.4313 0.7035 0.193 Uiso 1 1 calc R . . C4 C 0.6803(3) 0.4627(3) 0.7004(2) 0.113(4) Uani 1 1 d . . . C5 C 0.7043(3) 0.4726(2) 0.7023(2) 0.109(4) Uani 1 1 d . . . H5A H 0.7067 0.4899 0.7021 0.131 Uiso 1 1 calc R . . C6 C 0.7240(3) 0.4572(3) 0.7044(3) 0.131(5) Uani 1 1 d . . . H6A H 0.7403 0.4632 0.7065 0.158 Uiso 1 1 calc R . . C7 C 0.5582(4) 0.4808(4) 0.7206(4) 0.161(7) Uani 1 1 d . . . H7A H 0.5472 0.4681 0.7255 0.193 Uiso 1 1 calc R . . C8 C 0.5587(3) 0.5028(5) 0.7322(3) 0.157(6) Uani 1 1 d . . . H8A H 0.5479 0.5050 0.7458 0.189 Uiso 1 1 calc R . . C9 C 0.5733(4) 0.5217(3) 0.7263(3) 0.149(6) Uani 1 1 d . . . H9A H 0.5736 0.5365 0.7356 0.179 Uiso 1 1 calc R . . C10 C 0.5879(3) 0.5183(3) 0.7055(3) 0.136(5) Uani 1 1 d . . . H10A H 0.5967 0.5320 0.6992 0.164 Uiso 1 1 calc R . . C11 C 0.5901(3) 0.4953(3) 0.6934(3) 0.126(4) Uani 1 1 d . . . C12 C 0.5748(3) 0.4776(4) 0.7006(3) 0.163(7) Uani 1 1 d . . . H12A H 0.5750 0.4624 0.6920 0.196 Uiso 1 1 calc R . . C13 C 0.6196(3) 0.4792(4) 0.7762(4) 0.157(6) Uani 1 1 d . . . H13A H 0.6116 0.4786 0.7918 0.188 Uiso 1 1 calc R . . C14 C 0.6354(4) 0.4993(4) 0.7716(3) 0.184(8) Uani 1 1 d . . . H14A H 0.6396 0.5111 0.7838 0.221 Uiso 1 1 calc R . . C15 C 0.6446(3) 0.5003(3) 0.7469(4) 0.156(6) Uani 1 1 d . . . H15A H 0.6548 0.5138 0.7422 0.187 Uiso 1 1 calc R . . C16 C 0.6393(3) 0.4823(3) 0.7294(3) 0.126(5) Uani 1 1 d . . . C17 C 0.6254(3) 0.4627(3) 0.7361(4) 0.157(6) Uani 1 1 d . . . H17A H 0.6224 0.4500 0.7244 0.188 Uiso 1 1 calc R . . C18 C 0.6151(3) 0.4605(4) 0.7601(4) 0.164(7) Uani 1 1 d . . . H18A H 0.6054 0.4467 0.7647 0.196 Uiso 1 1 calc R . . C19 C 0.5638(3) 0.4795(3) 0.6130(3) 0.134(5) Uani 1 1 d . . . H19A H 0.5538 0.4892 0.6024 0.160 Uiso 1 1 calc R . . C20 C 0.5786(2) 0.4904(2) 0.6292(3) 0.113(4) Uani 1 1 d . . . H20A H 0.5798 0.5079 0.6300 0.136 Uiso 1 1 calc R . . C21 C 0.5921(2) 0.4757(3) 0.6447(2) 0.128(5) Uani 1 1 d . . . C22 C 0.5898(3) 0.4489(3) 0.6407(3) 0.143(5) Uani 1 1 d . . . H22A H 0.5993 0.4389 0.6515 0.172 Uiso 1 1 calc R . . C23 C 0.5774(3) 0.4378(3) 0.6256(3) 0.142(6) Uani 1 1 d U . . H23A H 0.5779 0.4204 0.6240 0.170 Uiso 1 1 calc R . . C24 C 0.5629(3) 0.4521(4) 0.6114(3) 0.157(6) Uani 1 1 d U . . H24A H 0.5519 0.4445 0.6001 0.189 Uiso 1 1 calc R . . C25 C 0.6337(2) 0.4714(2) 0.6774(2) 0.124(4) Uani 1 1 d . . . H25A H 0.6431 0.4650 0.6631 0.149 Uiso 1 1 calc R . . H25B H 0.6256 0.4573 0.6856 0.149 Uiso 1 1 calc R . . C26 C 0.6339(3) 0.5772(3) 0.6928(3) 0.109(4) Uani 1 1 d U . . O1 O 0.61958(14) 0.56486(13) 0.67792(16) 0.112(2) Uani 1 1 d . . . O2 O 0.65217(15) 0.56617(14) 0.70230(15) 0.112(2) Uani 1 1 d . . . O3 O 0.63120(13) 0.60043(15) 0.69509(14) 0.111(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1137(10) 0.1152(11) 0.1171(11) 0.000 0.0014(9) 0.000 Ag2 0.1326(9) 0.1194(8) 0.1321(9) 0.0068(7) -0.0026(7) -0.0023(7) Ag3 0.1383(9) 0.1217(9) 0.1492(10) 0.0063(7) -0.0082(8) 0.0008(7) Ag4 0.1242(6) 0.1242(6) 0.1242(6) 0.0000(6) 0.0000(6) 0.0000(6) P1 0.119(3) 0.107(3) 0.123(3) 0.009(2) -0.003(2) -0.005(2) P2 0.112(3) 0.097(2) 0.120(3) -0.004(2) 0.000(2) 0.006(2) Cl1 0.1180(17) 0.1180(17) 0.1180(17) 0.0024(19) -0.0024(19) 0.0024(19) C1 0.120(12) 0.138(15) 0.164(14) 0.048(11) -0.029(10) -0.033(11) C2 0.184(17) 0.081(10) 0.219(18) -0.009(11) 0.005(15) 0.024(12) C3 0.190(18) 0.121(14) 0.172(15) -0.019(12) 0.031(13) 0.011(14) C4 0.105(10) 0.137(12) 0.097(9) 0.001(8) -0.035(7) 0.017(9) C5 0.120(11) 0.092(9) 0.114(10) 0.005(7) -0.029(8) 0.014(9) C6 0.121(12) 0.116(11) 0.157(13) 0.007(10) -0.039(10) -0.032(11) C7 0.173(17) 0.116(13) 0.192(19) 0.030(13) 0.010(14) -0.025(12) C8 0.154(15) 0.171(17) 0.147(15) 0.047(15) 0.028(12) 0.041(14) C9 0.206(18) 0.120(12) 0.122(13) 0.013(10) 0.026(12) -0.028(13) C10 0.124(11) 0.121(13) 0.165(15) 0.013(11) 0.033(10) -0.031(9) C11 0.105(11) 0.126(12) 0.147(13) 0.006(11) -0.023(9) -0.004(9) C12 0.133(14) 0.193(18) 0.164(16) 0.006(13) 0.028(12) -0.042(13) C13 0.122(13) 0.167(18) 0.181(18) 0.016(16) 0.004(12) 0.017(12) C14 0.24(2) 0.160(17) 0.155(16) -0.002(13) 0.072(15) 0.000(16) C15 0.168(15) 0.108(12) 0.192(17) 0.019(12) 0.026(13) -0.046(10) C16 0.109(10) 0.089(9) 0.182(15) -0.011(10) -0.028(10) -0.019(8) C17 0.137(13) 0.162(15) 0.171(17) -0.004(13) -0.020(12) -0.039(12) C18 0.188(18) 0.172(18) 0.130(15) 0.035(13) 0.008(13) -0.014(14) C19 0.092(10) 0.168(15) 0.140(13) 0.023(11) -0.003(9) -0.003(10) C20 0.081(8) 0.106(9) 0.153(12) -0.011(9) -0.035(8) -0.002(7) C21 0.079(8) 0.187(16) 0.120(10) 0.027(11) -0.018(8) -0.006(9) C22 0.146(13) 0.082(10) 0.201(16) 0.007(10) -0.017(11) -0.020(9) C23 0.126(12) 0.105(11) 0.195(16) -0.028(10) -0.042(10) -0.041(9) C24 0.139(14) 0.21(2) 0.122(12) 0.010(12) -0.030(9) -0.050(12) C25 0.137(11) 0.091(9) 0.146(11) 0.000(8) -0.027(9) -0.030(8) C26 0.108(5) 0.108(5) 0.110(5) 0.002(4) 0.006(4) 0.003(4) O1 0.112(6) 0.074(5) 0.151(7) -0.005(5) 0.007(5) 0.003(4) O2 0.099(6) 0.103(6) 0.132(6) -0.020(5) 0.010(5) -0.003(5) O3 0.101(6) 0.102(6) 0.129(6) 0.005(5) -0.027(5) 0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O3 2.288(8) 11_566 y Ag1 O3 2.288(8) 12_665 y Ag1 Ag1 2.795(2) 10_656 y Ag1 Ag1 2.795(2) 6_566 y Ag1 Ag1 2.795(2) 5 y Ag1 Ag1 2.795(2) 9 y Ag1 Ag4 3.0027(16) 3_656 y Ag1 Ag4 3.0027(16) . y Ag2 O3 2.196(8) 12_665 y Ag2 P2 2.307(4) . y Ag2 O1 2.334(8) . y Ag2 Ag3 2.9243(16) . y Ag2 Ag2 3.113(2) 3_656 y Ag3 O2 2.348(8) . y Ag3 P1 2.386(4) . y Ag3 O2 2.483(8) 12_665 y Ag3 Cl1 2.629(3) . y Ag4 O1 2.282(8) 11_566 y Ag4 O1 2.282(8) . y Ag4 O1 2.282(8) 8_656 y Ag4 Ag1 3.0027(16) 6_566 y Ag4 Ag1 3.0027(16) 9 y P1 C25 1.829(11) . ? P1 C16 1.862(16) . ? P1 C4 1.883(14) . ? P2 C11 1.821(16) . ? P2 C21 1.825(14) . ? P2 C25 1.826(12) . ? Cl1 Ag3 2.629(3) 6_566 ? Cl1 Ag3 2.629(3) 12_665 ? C1 C6 1.293(17) . ? C1 C2 1.316(18) . ? C2 C3 1.323(19) . ? C3 C4 1.332(18) . ? C4 C5 1.414(16) . ? C5 C6 1.362(16) . ? C7 C8 1.35(2) . ? C7 C12 1.42(2) . ? C8 C9 1.33(2) . ? C9 C10 1.387(18) . ? C10 C11 1.413(18) . ? C11 C12 1.327(17) . ? C13 C18 1.36(2) . ? C13 C14 1.41(2) . ? C14 C15 1.434(19) . ? C15 C16 1.392(18) . ? C16 C17 1.358(18) . ? C17 C18 1.42(2) . ? C19 C20 1.329(17) . ? C19 C24 1.49(2) . ? C20 C21 1.375(16) . ? C21 C22 1.471(18) . ? C22 C23 1.220(17) . ? C23 C24 1.346(19) . ? C26 O2 1.268(14) . ? C26 O3 1.276(14) . ? C26 O1 1.305(14) . ? O2 Ag3 2.483(8) 6_566 ? O3 Ag2 2.196(8) 6_566 ? O3 Ag1 2.288(8) 6_566 ? 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 O3 Ag1 O3 73.9(4) 11_566 12_665 y O3 Ag1 Ag1 167.8(2) 11_566 10_656 y O3 Ag1 Ag1 98.8(2) 12_665 10_656 y O3 Ag1 Ag1 132.00(19) 11_566 6_566 y O3 Ag1 Ag1 117.46(18) 12_665 6_566 y Ag1 Ag1 Ag1 60.0 10_656 6_566 y O3 Ag1 Ag1 117.46(18) 11_566 5 y O3 Ag1 Ag1 132.00(19) 12_665 5 y Ag1 Ag1 Ag1 60.0 10_656 5 y Ag1 Ag1 Ag1 90.0 6_566 5 y O3 Ag1 Ag1 98.8(2) 11_566 9 y O3 Ag1 Ag1 167.8(2) 12_665 9 y Ag1 Ag1 Ag1 90.0 10_656 9 y Ag1 Ag1 Ag1 60.0 6_566 9 y Ag1 Ag1 Ag1 60.0 5 9 y O3 Ag1 Ag4 105.6(2) 11_566 3_656 y O3 Ag1 Ag4 69.74(19) 12_665 3_656 y Ag1 Ag1 Ag4 62.27(3) 10_656 3_656 y Ag1 Ag1 Ag4 122.24(3) 6_566 3_656 y Ag1 Ag1 Ag4 62.27(3) 5 3_656 y Ag1 Ag1 Ag4 122.24(3) 9 3_656 y O3 Ag1 Ag4 69.74(19) 11_566 . y O3 Ag1 Ag4 105.6(2) 12_665 . y Ag1 Ag1 Ag4 122.24(3) 10_656 . y Ag1 Ag1 Ag4 62.27(3) 6_566 . y Ag1 Ag1 Ag4 122.24(3) 5 . y Ag1 Ag1 Ag4 62.27(3) 9 . y Ag4 Ag1 Ag4 174.48(6) 3_656 . y O3 Ag2 P2 157.1(2) 12_665 . y O3 Ag2 O1 85.0(3) 12_665 . y P2 Ag2 O1 117.6(2) . . y O3 Ag2 Ag3 88.85(18) 12_665 . y P2 Ag2 Ag3 92.14(10) . . y O1 Ag2 Ag3 77.7(2) . . y O3 Ag2 Ag2 58.78(19) 12_665 3_656 y P2 Ag2 Ag2 106.62(10) . 3_656 y O1 Ag2 Ag2 123.6(2) . 3_656 y Ag3 Ag2 Ag2 135.35(6) . 3_656 y O2 Ag3 P1 133.0(2) . . y O2 Ag3 O2 88.4(4) . 12_665 y P1 Ag3 O2 133.7(2) . 12_665 y O2 Ag3 Cl1 86.0(2) . . y P1 Ag3 Cl1 114.21(14) . . y O2 Ag3 Cl1 83.3(2) 12_665 . y O2 Ag3 Ag2 84.3(2) . . y P1 Ag3 Ag2 89.23(10) . . y O2 Ag3 Ag2 73.15(19) 12_665 . y Cl1 Ag3 Ag2 154.71(11) . . y O1 Ag4 O1 119.971(11) 11_566 . y O1 Ag4 O1 119.970(12) 11_566 8_656 y O1 Ag4 O1 119.970(11) . 8_656 y O1 Ag4 Ag1 78.72(19) 11_566 . y O1 Ag4 Ag1 72.0(2) . . y O1 Ag4 Ag1 123.2(2) 8_656 . y O1 Ag4 Ag1 123.2(2) 11_566 6_566 y O1 Ag4 Ag1 78.72(19) . 6_566 y O1 Ag4 Ag1 72.0(2) 8_656 6_566 y Ag1 Ag4 Ag1 55.47(5) . 6_566 y O1 Ag4 Ag1 72.0(2) 11_566 9 y O1 Ag4 Ag1 123.2(2) . 9 y O1 Ag4 Ag1 78.72(19) 8_656 9 y Ag1 Ag4 Ag1 55.47(5) . 9 y Ag1 Ag4 Ag1 55.47(5) 6_566 9 y C25 P1 C16 103.4(6) . . ? C25 P1 C4 100.6(6) . . ? C16 P1 C4 102.6(6) . . ? C25 P1 Ag3 116.6(4) . . ? C16 P1 Ag3 115.0(5) . . ? C4 P1 Ag3 116.5(5) . . ? C11 P2 C21 103.1(7) . . ? C11 P2 C25 102.2(6) . . ? C21 P2 C25 104.4(7) . . ? C11 P2 Ag2 115.0(6) . . ? C21 P2 Ag2 117.3(5) . . ? C25 P2 Ag2 113.2(4) . . ? Ag3 Cl1 Ag3 90.07(15) 6_566 12_665 ? Ag3 Cl1 Ag3 90.07(15) 6_566 . ? Ag3 Cl1 Ag3 90.07(15) 12_665 . ? C6 C1 C2 128.4(17) . . ? C1 C2 C3 114.1(16) . . ? C2 C3 C4 124.9(18) . . ? C3 C4 C5 115.6(14) . . ? C3 C4 P1 129.2(14) . . ? C5 C4 P1 115.0(12) . . ? C6 C5 C4 120.0(12) . . ? C1 C6 C5 115.9(14) . . ? C8 C7 C12 116.8(17) . . ? C9 C8 C7 125.3(18) . . ? C8 C9 C10 115.6(16) . . ? C9 C10 C11 123.0(14) . . ? C12 C11 C10 116.6(16) . . ? C12 C11 P2 124.2(15) . . ? C10 C11 P2 118.6(13) . . ? C11 C12 C7 122.1(18) . . ? C18 C13 C14 125(2) . . ? C13 C14 C15 114.3(18) . . ? C16 C15 C14 122.5(15) . . ? C17 C16 C15 118.9(16) . . ? C17 C16 P1 125.6(14) . . ? C15 C16 P1 115.3(12) . . ? C16 C17 C18 122.0(17) . . ? C13 C18 C17 117.3(19) . . ? C20 C19 C24 120.2(14) . . ? C19 C20 C21 117.8(14) . . ? C20 C21 C22 116.1(13) . . ? C20 C21 P2 112.9(13) . . ? C22 C21 P2 130.9(12) . . ? C23 C22 C21 129.3(16) . . ? C22 C23 C24 114.9(17) . . ? C23 C24 C19 121.5(15) . . ? P2 C25 P1 110.5(6) . . ? O2 C26 O3 121.1(14) . . ? O2 C26 O1 118.4(14) . . ? O3 C26 O1 120.0(14) . . ? C26 O1 Ag4 115.0(9) . . ? C26 O1 Ag2 131.6(9) . . ? Ag4 O1 Ag2 110.6(4) . . ? C26 O2 Ag3 124.5(9) . . ? C26 O2 Ag3 130.0(9) . 6_566 ? Ag3 O2 Ag3 100.7(3) . 6_566 ? C26 O3 Ag2 123.6(9) . 6_566 ? C26 O3 Ag1 120.9(8) . 6_566 ? Ag2 O3 Ag1 104.0(3) 6_566 6_566 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.441 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.068 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.002 -0.001 -0.007 105099 52682 ' ' 2 0.000 0.500 0.000 53 1 ' ' 3 0.250 0.750 0.000 53 1 ' ' 4 0.500 0.000 0.000 53 1 ' ' 5 0.750 0.250 0.000 53 1 ' ' 6 0.000 0.750 0.250 53 1 ' ' 7 0.250 0.500 0.250 53 1 ' ' 8 0.500 0.250 0.250 53 1 ' ' 9 0.750 0.000 0.250 53 1 ' ' 10 0.000 1.000 0.500 53 1 ' ' 11 0.250 0.250 0.500 53 1 ' ' 12 0.500 0.500 0.500 53 1 ' ' 13 0.750 0.750 0.500 53 1 ' ' 14 0.000 0.250 0.750 53 1 ' ' 15 0.250 0.000 0.750 53 1 ' ' 16 0.500 0.750 0.750 53 1 ' ' 17 0.750 0.500 0.750 53 1 ' ' _platon_squeeze_details ; A. L. Spek, J. Appl. Crystallogr., 2003, 36, 7-13. ; # start Validation Reply Form _vrf_PLAT026_p1 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 24 Perc. RESPONSE: Crystal have week diffraction intensities, hence only small amount of reflections have I>2sigma(I) ; ############################################# data_p3 _database_code_depnum_ccdc_archive 'CCDC 743743' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H60 Ag4 N6 P4, 2(C31 H30 Ag2 N3 P2), 4(Cl O4) ' _chemical_formula_sum 'C124 H120 Ag8 Cl4 N12 O16 P8' _chemical_formula_weight 3286.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_HALL '-P 2ybc' 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 12.670(3) _cell_length_b 16.694(3) _cell_length_c 30.990(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.75(3) _cell_angle_gamma 90.00 _cell_volume 6552(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 46461 _cell_measurement_theta_min 6.01 _cell_measurement_theta_max 54.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7651 _exptl_absorpt_correction_T_max 0.8159 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 298(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 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88354 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12870 _reflns_number_gt 8957 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+7.6475P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11501 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.58867(4) 0.95923(4) 0.557351(14) 0.07093(17) Uani 1 1 d . . . Ag2 Ag 0.38215(3) 0.91877(3) 0.526499(13) 0.05574(13) Uani 1 1 d . . . Ag3 Ag -0.07060(4) 0.46270(3) 0.446936(14) 0.06013(14) Uani 1 1 d . . . Ag4 Ag 0.05997(3) 0.60447(3) 0.448993(13) 0.05591(13) Uani 1 1 d . . . Cl1 Cl 0.26356(18) 0.40688(11) 0.24592(5) 0.0840(5) Uani 1 1 d . . . Cl2 Cl 0.16431(14) 0.79701(10) 0.48308(5) 0.0720(4) Uani 1 1 d . . . P1 P 0.14326(11) 0.56759(9) 0.38485(4) 0.0504(3) Uani 1 1 d . . . P2 P -0.00801(11) 0.42255(9) 0.37826(4) 0.0504(3) Uani 1 1 d . . . P3 P 0.54147(10) 0.99403(9) 0.62839(4) 0.0481(3) Uani 1 1 d . . . P4 P 0.31955(10) 0.94685(9) 0.59590(4) 0.0466(3) Uani 1 1 d . . . C1 C 0.5725(4) 0.8647(3) 0.47173(16) 0.0511(13) Uani 1 1 d . . . C2 C 0.7421(5) 0.8614(4) 0.50269(19) 0.0611(15) Uani 1 1 d . . . C3 C 0.7748(5) 0.8142(4) 0.4696(2) 0.0666(16) Uani 1 1 d . . . H3A H 0.8436 0.7948 0.4694 0.080 Uiso 1 1 calc R . . C4 C 0.7042(5) 0.7963(4) 0.4369(2) 0.0645(16) Uani 1 1 d . . . C5 C 0.8140(5) 0.8863(6) 0.5395(2) 0.096(3) Uani 1 1 d . . . H5A H 0.7759 0.9194 0.5590 0.144 Uiso 1 1 calc R . . H5B H 0.8725 0.9159 0.5286 0.144 Uiso 1 1 calc R . . H5C H 0.8398 0.8396 0.5545 0.144 Uiso 1 1 calc R . . C6 C 0.7362(6) 0.7500(6) 0.3978(3) 0.104(3) Uani 1 1 d . . . H6A H 0.6761 0.7433 0.3785 0.156 Uiso 1 1 calc R . . H6B H 0.7624 0.6983 0.4065 0.156 Uiso 1 1 calc R . . H6C H 0.7905 0.7787 0.3833 0.156 Uiso 1 1 calc R . . C7 C 0.6043(4) 1.0835(3) 0.64995(17) 0.0513(13) Uani 1 1 d . . . C8 C 0.7014(5) 1.1043(5) 0.6352(2) 0.077(2) Uani 1 1 d . . . H8A H 0.7328 1.0728 0.6144 0.093 Uiso 1 1 calc R . . C9 C 0.7530(6) 1.1713(5) 0.6509(3) 0.094(3) Uani 1 1 d . . . H9A H 0.8188 1.1850 0.6406 0.112 Uiso 1 1 calc R . . C10 C 0.7088(6) 1.2172(5) 0.6811(2) 0.084(2) Uani 1 1 d . . . H10A H 0.7448 1.2617 0.6921 0.101 Uiso 1 1 calc R . . C11 C 0.6132(6) 1.1990(5) 0.6953(3) 0.101(3) Uani 1 1 d . . . H11A H 0.5822 1.2318 0.7156 0.121 Uiso 1 1 calc R . . C12 C 0.5603(6) 1.1325(5) 0.6803(3) 0.090(2) Uani 1 1 d . . . H12A H 0.4941 1.1204 0.6907 0.107 Uiso 1 1 calc R . . C13 C 0.3151(4) 0.8551(3) 0.62697(17) 0.0502(12) Uani 1 1 d . . . C14 C 0.3435(6) 0.7847(4) 0.6076(2) 0.0746(18) Uani 1 1 d . . . H14A H 0.3639 0.7850 0.5790 0.089 Uiso 1 1 calc R . . C15 C 0.3418(7) 0.7132(5) 0.6302(3) 0.100(3) Uani 1 1 d . . . H15A H 0.3615 0.6659 0.6167 0.120 Uiso 1 1 calc R . . C16 C 0.3116(7) 0.7117(5) 0.6721(3) 0.095(2) Uani 1 1 d . . . H16A H 0.3096 0.6635 0.6871 0.114 Uiso 1 1 calc R . . C17 C 0.2847(7) 0.7805(5) 0.6916(3) 0.090(2) Uani 1 1 d . . . H17A H 0.2657 0.7799 0.7204 0.107 Uiso 1 1 calc R . . C18 C 0.2850(6) 0.8517(4) 0.6694(2) 0.0741(18) Uani 1 1 d . . . H18A H 0.2646 0.8984 0.6831 0.089 Uiso 1 1 calc R . . C19 C 0.1903(4) 0.9946(3) 0.59725(17) 0.0470(12) Uani 1 1 d . . . C20 C 0.1512(5) 1.0269(4) 0.6345(2) 0.0639(15) Uani 1 1 d . . . H20A H 0.1909 1.0238 0.6602 0.077 Uiso 1 1 calc R . . C21 C 0.0535(5) 1.0638(4) 0.6339(2) 0.0713(18) Uani 1 1 d . . . H21A H 0.0272 1.0850 0.6591 0.086 Uiso 1 1 calc R . . C22 C -0.0044(5) 1.0691(4) 0.5959(2) 0.0693(17) Uani 1 1 d . . . H22A H -0.0697 1.0945 0.5954 0.083 Uiso 1 1 calc R . . C23 C 0.0331(5) 1.0374(4) 0.5591(2) 0.0701(17) Uani 1 1 d . . . H23A H -0.0069 1.0407 0.5335 0.084 Uiso 1 1 calc R . . C24 C 0.1305(4) 1.0001(3) 0.55949(18) 0.0541(13) Uani 1 1 d . . . H24A H 0.1558 0.9787 0.5341 0.065 Uiso 1 1 calc R . . C25 C 0.5608(4) 0.9190(4) 0.67011(19) 0.0573(14) Uani 1 1 d . . . C26 C 0.6068(6) 0.8479(5) 0.6598(3) 0.088(2) Uani 1 1 d . . . H26A H 0.6276 0.8384 0.6318 0.106 Uiso 1 1 calc R . . C27 C 0.6227(8) 0.7892(6) 0.6917(4) 0.124(3) Uani 1 1 d . . . H27A H 0.6567 0.7416 0.6850 0.148 Uiso 1 1 calc R . . C28 C 0.5891(7) 0.8012(6) 0.7318(3) 0.101(3) Uani 1 1 d . . . H28A H 0.5976 0.7612 0.7525 0.121 Uiso 1 1 calc R . . C29 C 0.5436(7) 0.8702(6) 0.7421(2) 0.089(2) Uani 1 1 d . . . H29A H 0.5219 0.8785 0.7701 0.107 Uiso 1 1 calc R . . C30 C 0.5282(6) 0.9296(5) 0.7116(2) 0.0751(18) Uani 1 1 d . . . H30A H 0.4955 0.9772 0.7192 0.090 Uiso 1 1 calc R . . C31 C -0.1396(5) 0.6030(3) 0.50670(16) 0.0527(13) Uani 1 1 d . . . C32 C -0.2982(6) 0.6275(5) 0.5372(2) 0.080(2) Uani 1 1 d . . . C33 C -0.3408(6) 0.5599(5) 0.5167(3) 0.090(2) Uani 1 1 d . . . H33A H -0.4111 0.5457 0.5200 0.108 Uiso 1 1 calc R . . C34 C -0.2760(5) 0.5153(4) 0.4918(2) 0.0712(17) Uani 1 1 d . . . C35 C -0.3150(6) 0.4417(5) 0.4683(3) 0.104(3) Uani 1 1 d . . . H35A H -0.2584 0.4186 0.4526 0.157 Uiso 1 1 calc R . . H35B H -0.3717 0.4561 0.4486 0.157 Uiso 1 1 calc R . . H35C H -0.3398 0.4035 0.4888 0.157 Uiso 1 1 calc R . . C36 C -0.3633(7) 0.6791(6) 0.5658(3) 0.118(3) Uani 1 1 d . . . H36A H -0.3208 0.7225 0.5770 0.178 Uiso 1 1 calc R . . H36B H -0.3881 0.6476 0.5894 0.178 Uiso 1 1 calc R . . H36C H -0.4226 0.7002 0.5495 0.178 Uiso 1 1 calc R . . C37 C 0.2864(5) 0.5785(4) 0.38396(19) 0.0616(15) Uani 1 1 d . . . C38 C 0.3487(5) 0.5308(5) 0.3591(3) 0.088(2) Uani 1 1 d . . . H38A H 0.3171 0.4925 0.3412 0.105 Uiso 1 1 calc R . . C39 C 0.4575(6) 0.5385(6) 0.3602(3) 0.112(3) Uani 1 1 d . . . H39A H 0.4990 0.5058 0.3434 0.134 Uiso 1 1 calc R . . C40 C 0.5026(7) 0.5956(7) 0.3866(4) 0.122(3) Uani 1 1 d . . . H40A H 0.5757 0.6014 0.3876 0.146 Uiso 1 1 calc R . . C41 C 0.4437(7) 0.6434(6) 0.4113(4) 0.125(4) Uani 1 1 d . . . H41A H 0.4758 0.6813 0.4293 0.150 Uiso 1 1 calc R . . C42 C 0.3347(6) 0.6357(5) 0.4095(3) 0.088(2) Uani 1 1 d . . . H42A H 0.2938 0.6697 0.4259 0.105 Uiso 1 1 calc R . . C43 C 0.0863(4) 0.6230(3) 0.33950(17) 0.0535(13) Uani 1 1 d . . . C44 C 0.0197(5) 0.6856(4) 0.3476(2) 0.0665(16) Uani 1 1 d . . . H44A H 0.0075 0.6998 0.3760 0.080 Uiso 1 1 calc R . . C45 C -0.0299(6) 0.7284(5) 0.3143(2) 0.088(2) Uani 1 1 d . . . H45A H -0.0755 0.7703 0.3203 0.105 Uiso 1 1 calc R . . C46 C -0.0103(7) 0.7075(5) 0.2722(2) 0.091(2) Uani 1 1 d . . . H46A H -0.0424 0.7356 0.2494 0.110 Uiso 1 1 calc R . . C47 C 0.0562(7) 0.6458(5) 0.2641(2) 0.090(2) Uani 1 1 d . . . H47A H 0.0689 0.6318 0.2357 0.108 Uiso 1 1 calc R . . C48 C 0.1050(6) 0.6036(4) 0.29739(19) 0.0730(18) Uani 1 1 d . . . H48A H 0.1507 0.5618 0.2913 0.088 Uiso 1 1 calc R . . C49 C -0.0870(4) 0.4541(4) 0.33173(18) 0.0563(14) Uani 1 1 d . . . C50 C -0.1628(6) 0.5124(5) 0.3368(3) 0.092(2) Uani 1 1 d . . . H50A H -0.1741 0.5337 0.3640 0.110 Uiso 1 1 calc R . . C51 C -0.2221(8) 0.5393(7) 0.3013(4) 0.132(4) Uani 1 1 d . . . H51A H -0.2715 0.5798 0.3046 0.158 Uiso 1 1 calc R . . C52 C -0.2089(8) 0.5073(8) 0.2622(3) 0.118(3) Uani 1 1 d . . . H52A H -0.2497 0.5255 0.2388 0.142 Uiso 1 1 calc R . . C53 C -0.1375(8) 0.4495(7) 0.2565(3) 0.107(3) Uani 1 1 d . . . H53A H -0.1298 0.4271 0.2293 0.128 Uiso 1 1 calc R . . C54 C -0.0750(6) 0.4228(5) 0.2912(2) 0.084(2) Uani 1 1 d . . . H54A H -0.0244 0.3835 0.2869 0.100 Uiso 1 1 calc R . . C55 C 0.0127(4) 0.3156(3) 0.37147(17) 0.0535(13) Uani 1 1 d . . . C56 C 0.0880(5) 0.2837(4) 0.3450(2) 0.0683(16) Uani 1 1 d . . . H56A H 0.1316 0.3178 0.3298 0.082 Uiso 1 1 calc R . . C57 C 0.0994(6) 0.2024(4) 0.3408(2) 0.081(2) Uani 1 1 d . . . H57A H 0.1505 0.1816 0.3230 0.097 Uiso 1 1 calc R . . C58 C 0.0350(7) 0.1520(4) 0.3629(3) 0.089(2) Uani 1 1 d . . . H58A H 0.0410 0.0968 0.3595 0.107 Uiso 1 1 calc R . . C59 C -0.0389(7) 0.1831(5) 0.3900(3) 0.089(2) Uani 1 1 d . . . H59A H -0.0812 0.1487 0.4056 0.107 Uiso 1 1 calc R . . C60 C -0.0502(5) 0.2640(4) 0.3942(2) 0.0659(16) Uani 1 1 d . . . H60A H -0.1004 0.2845 0.4125 0.079 Uiso 1 1 calc R . . C61 C 0.4002(4) 1.0167(3) 0.62850(16) 0.0471(12) Uani 1 1 d . . . H61A H 0.3890 1.0706 0.6176 0.056 Uiso 1 1 calc R . . H61B H 0.3768 1.0154 0.6580 0.056 Uiso 1 1 calc R . . C62 C 0.1244(4) 0.4620(3) 0.36985(17) 0.0497(12) Uani 1 1 d . . . H62A H 0.1403 0.4558 0.3396 0.060 Uiso 1 1 calc R . . H62B H 0.1749 0.4299 0.3865 0.060 Uiso 1 1 calc R . . N1 N 0.4716(4) 0.8877(3) 0.47291(14) 0.0583(12) Uani 1 1 d . . . H1A H 0.4386 0.8902 0.4483 0.070 Uiso 1 1 calc R . . N2 N 0.6414(3) 0.8884(3) 0.50393(14) 0.0525(11) Uani 1 1 d . . . N3 N 0.6044(4) 0.8205(3) 0.43742(15) 0.0640(13) Uani 1 1 d . . . N4 N -0.1756(4) 0.5353(3) 0.48632(15) 0.0571(12) Uani 1 1 d . . . N5 N -0.0383(4) 0.6246(3) 0.50151(14) 0.0596(12) Uani 1 1 d . . . H5D H -0.0095 0.6504 0.5228 0.072 Uiso 1 1 calc R . . N6 N -0.1986(4) 0.6480(3) 0.53282(16) 0.0666(13) Uani 1 1 d . . . O1 O 0.1504(9) 0.4020(10) 0.2438(5) 0.281(8) Uani 1 1 d . . . O2 O 0.2808(10) 0.3869(4) 0.2860(2) 0.189(5) Uani 1 1 d . . . O3 O 0.2827(7) 0.4863(4) 0.2358(2) 0.143(3) Uani 1 1 d . . . O4 O 0.2952(6) 0.3581(5) 0.21348(19) 0.141(3) Uani 1 1 d . . . O5 O 0.1296(5) 0.7616(3) 0.44390(17) 0.1115(19) Uani 1 1 d . . . O6 O 0.2122(4) 0.8737(3) 0.47303(18) 0.0982(16) Uani 1 1 d . . . O7 O 0.0747(6) 0.8138(5) 0.5077(2) 0.139(3) Uani 1 1 d . . . O8 O 0.2318(9) 0.7467(6) 0.5047(3) 0.191(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0521(3) 0.1068(4) 0.0543(3) -0.0244(3) 0.0080(2) -0.0190(3) Ag2 0.0480(2) 0.0670(3) 0.0521(2) -0.0074(2) 0.00101(18) -0.0014(2) Ag3 0.0584(3) 0.0647(3) 0.0580(3) -0.0112(2) 0.0134(2) -0.0109(2) Ag4 0.0587(3) 0.0595(3) 0.0498(2) -0.00453(19) 0.00600(19) -0.0085(2) Cl1 0.1247(16) 0.0684(11) 0.0605(9) 0.0090(8) 0.0290(10) 0.0128(10) Cl2 0.0826(11) 0.0701(10) 0.0629(9) -0.0078(8) -0.0046(8) 0.0022(9) P1 0.0504(8) 0.0514(8) 0.0496(7) -0.0036(6) 0.0056(6) -0.0105(6) P2 0.0518(8) 0.0525(8) 0.0472(7) -0.0019(6) 0.0057(6) -0.0097(6) P3 0.0413(7) 0.0572(8) 0.0459(7) -0.0065(6) 0.0013(6) -0.0061(6) P4 0.0386(7) 0.0511(8) 0.0502(7) -0.0043(6) 0.0010(6) -0.0028(6) C1 0.058(3) 0.053(3) 0.042(3) 0.000(2) 0.003(2) -0.008(3) C2 0.053(3) 0.073(4) 0.057(3) 0.006(3) 0.004(3) -0.003(3) C3 0.057(3) 0.067(4) 0.076(4) 0.001(3) 0.013(3) 0.007(3) C4 0.067(4) 0.049(3) 0.078(4) -0.005(3) 0.022(3) -0.003(3) C5 0.053(4) 0.160(8) 0.074(4) -0.007(5) -0.005(3) 0.003(5) C6 0.088(5) 0.116(7) 0.110(6) -0.047(5) 0.034(5) -0.006(5) C7 0.048(3) 0.059(3) 0.047(3) -0.005(2) 0.002(2) -0.012(3) C8 0.066(4) 0.095(5) 0.072(4) -0.021(4) 0.016(3) -0.031(4) C9 0.076(5) 0.105(6) 0.102(6) -0.031(5) 0.031(4) -0.043(4) C10 0.093(5) 0.076(5) 0.084(5) -0.014(4) 0.008(4) -0.034(4) C11 0.087(5) 0.088(6) 0.129(7) -0.051(5) 0.027(5) -0.020(4) C12 0.064(4) 0.094(5) 0.112(6) -0.041(5) 0.028(4) -0.029(4) C13 0.041(3) 0.054(3) 0.056(3) -0.006(2) -0.002(2) -0.003(2) C14 0.090(5) 0.057(4) 0.077(4) 0.000(3) 0.008(4) 0.009(3) C15 0.137(8) 0.060(5) 0.104(6) -0.001(4) 0.010(5) 0.010(5) C16 0.115(7) 0.068(5) 0.101(6) 0.022(4) -0.005(5) -0.003(4) C17 0.110(6) 0.084(5) 0.075(5) 0.020(4) 0.011(4) 0.000(5) C18 0.090(5) 0.067(4) 0.067(4) 0.001(3) 0.012(3) -0.003(4) C19 0.038(3) 0.045(3) 0.058(3) -0.005(2) -0.002(2) -0.006(2) C20 0.052(3) 0.074(4) 0.065(4) -0.013(3) 0.001(3) 0.004(3) C21 0.058(4) 0.073(4) 0.083(4) -0.019(3) 0.016(3) 0.007(3) C22 0.044(3) 0.067(4) 0.097(5) -0.001(4) 0.004(3) 0.010(3) C23 0.050(3) 0.073(4) 0.086(5) 0.000(4) -0.009(3) 0.009(3) C24 0.046(3) 0.055(3) 0.061(3) -0.001(3) -0.003(2) -0.003(3) C25 0.041(3) 0.067(4) 0.064(4) 0.001(3) -0.005(3) -0.008(3) C26 0.091(5) 0.074(5) 0.101(5) 0.012(4) 0.029(4) 0.025(4) C27 0.128(8) 0.089(7) 0.156(9) 0.031(6) 0.036(7) 0.033(6) C28 0.077(5) 0.105(7) 0.121(7) 0.047(6) 0.001(5) 0.005(5) C29 0.098(6) 0.105(6) 0.064(4) 0.023(4) -0.005(4) -0.015(5) C30 0.084(5) 0.082(5) 0.059(4) 0.002(3) -0.005(3) 0.005(4) C31 0.061(3) 0.055(3) 0.042(3) 0.000(2) -0.001(2) 0.005(3) C32 0.078(5) 0.076(5) 0.086(5) 0.000(4) 0.022(4) 0.016(4) C33 0.056(4) 0.093(6) 0.122(6) -0.015(5) 0.026(4) 0.001(4) C34 0.061(4) 0.070(4) 0.083(4) -0.006(3) 0.007(3) 0.000(3) C35 0.057(4) 0.108(6) 0.150(8) -0.032(6) 0.020(5) -0.014(4) C36 0.098(6) 0.107(7) 0.155(9) -0.028(6) 0.060(6) 0.016(5) C37 0.058(3) 0.063(4) 0.063(3) -0.004(3) 0.006(3) -0.012(3) C38 0.062(4) 0.104(6) 0.099(5) -0.025(5) 0.015(4) -0.017(4) C39 0.057(4) 0.134(8) 0.147(8) -0.020(7) 0.022(5) -0.009(5) C40 0.059(5) 0.123(8) 0.184(11) -0.013(7) -0.003(6) -0.013(5) C41 0.082(6) 0.115(8) 0.176(10) -0.038(7) -0.024(6) -0.032(6) C42 0.067(4) 0.079(5) 0.116(6) -0.025(4) -0.004(4) -0.017(4) C43 0.056(3) 0.051(3) 0.054(3) 0.002(2) 0.004(3) -0.010(3) C44 0.075(4) 0.061(4) 0.064(4) 0.001(3) -0.001(3) -0.005(3) C45 0.103(6) 0.071(5) 0.088(5) 0.002(4) -0.017(4) 0.004(4) C46 0.114(6) 0.082(5) 0.077(5) 0.015(4) -0.022(4) -0.005(5) C47 0.122(7) 0.093(6) 0.055(4) 0.009(4) -0.006(4) -0.015(5) C48 0.095(5) 0.072(4) 0.052(3) -0.001(3) 0.010(3) -0.008(4) C49 0.052(3) 0.059(3) 0.058(3) 0.001(3) 0.002(3) -0.012(3) C50 0.080(5) 0.108(6) 0.086(5) -0.010(4) -0.004(4) 0.027(5) C51 0.109(7) 0.162(11) 0.123(8) -0.002(7) -0.030(6) 0.048(7) C52 0.097(7) 0.162(10) 0.093(6) 0.024(7) -0.030(5) 0.014(7) C53 0.109(7) 0.148(9) 0.062(4) 0.009(5) -0.014(4) 0.000(6) C54 0.082(5) 0.109(6) 0.060(4) 0.000(4) -0.005(3) 0.008(4) C55 0.060(3) 0.054(3) 0.046(3) 0.003(2) -0.004(3) -0.011(3) C56 0.080(4) 0.055(4) 0.071(4) 0.000(3) 0.014(3) -0.003(3) C57 0.097(5) 0.055(4) 0.090(5) -0.012(4) -0.002(4) 0.003(4) C58 0.115(6) 0.049(4) 0.101(6) 0.004(4) -0.034(5) -0.008(4) C59 0.098(6) 0.063(5) 0.105(6) 0.023(4) -0.024(5) -0.042(4) C60 0.062(4) 0.070(4) 0.066(4) 0.010(3) -0.002(3) -0.022(3) C61 0.041(3) 0.055(3) 0.045(3) -0.002(2) -0.003(2) -0.002(2) C62 0.047(3) 0.050(3) 0.053(3) 0.001(2) 0.004(2) -0.005(2) N1 0.051(3) 0.080(3) 0.043(2) -0.007(2) -0.002(2) 0.000(2) N2 0.048(2) 0.060(3) 0.050(2) -0.002(2) 0.008(2) -0.003(2) N3 0.070(3) 0.065(3) 0.058(3) -0.016(2) 0.007(2) -0.008(3) N4 0.050(3) 0.066(3) 0.056(3) 0.002(2) 0.008(2) 0.001(2) N5 0.069(3) 0.062(3) 0.048(3) -0.007(2) -0.004(2) -0.003(2) N6 0.074(3) 0.067(3) 0.059(3) -0.002(2) 0.015(3) 0.008(3) O1 0.155(9) 0.37(2) 0.325(17) -0.041(14) 0.126(11) -0.050(11) O2 0.391(15) 0.104(5) 0.073(4) 0.011(4) -0.006(6) 0.002(7) O3 0.244(9) 0.080(4) 0.105(5) 0.021(3) 0.017(5) -0.030(5) O4 0.186(7) 0.147(6) 0.091(4) -0.006(4) 0.038(4) 0.068(5) O5 0.162(5) 0.087(4) 0.084(3) -0.021(3) -0.017(4) -0.029(4) O6 0.094(4) 0.096(4) 0.104(4) -0.013(3) -0.003(3) -0.034(3) O7 0.156(6) 0.138(6) 0.128(5) -0.001(4) 0.074(5) 0.001(5) O8 0.261(10) 0.164(8) 0.144(6) 0.005(5) -0.060(7) 0.110(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 N2 2.157(4) . y Ag1 P3 2.3710(15) . y Ag1 Ag2 2.8397(9) . y Ag1 Ag2 3.3311(9) 3_676 y Ag2 N1 2.104(4) . y Ag2 P4 2.3619(15) . y Ag2 Ag1 3.3311(9) 3_676 y Ag3 N4 2.197(5) . y Ag3 P2 2.3897(15) . y Ag3 N5 2.539(5) 3_566 y Ag3 Ag4 2.8871(7) . y Ag4 N5 2.106(5) . y Ag4 P1 2.3604(16) . y Cl1 O2 1.298(7) . ? Cl1 O4 1.363(6) . ? Cl1 O3 1.385(6) . ? Cl1 O1 1.436(12) . ? Cl2 O8 1.361(7) . ? Cl2 O5 1.409(5) . ? Cl2 O7 1.415(6) . ? Cl2 O6 1.454(6) . ? P1 C43 1.814(6) . ? P1 C37 1.823(6) . ? P1 C62 1.836(5) . ? P2 C49 1.808(6) . ? P2 C55 1.817(6) . ? P2 C62 1.829(5) . ? P3 C25 1.811(6) . ? P3 C7 1.811(5) . ? P3 C61 1.829(5) . ? P4 C13 1.811(6) . ? P4 C19 1.823(5) . ? P4 C61 1.834(5) . ? C1 N1 1.336(7) . ? C1 N2 1.364(7) . ? C1 N3 1.365(7) . ? C2 N2 1.355(7) . ? C2 C3 1.368(9) . ? C2 C5 1.498(9) . ? C3 C4 1.364(9) . ? C3 H3A 0.9300 . ? C4 N3 1.329(8) . ? C4 C6 1.504(9) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.370(8) . ? C7 C12 1.378(9) . ? C8 C9 1.378(9) . ? C8 H8A 0.9300 . ? C9 C10 1.345(10) . ? C9 H9A 0.9300 . ? C10 C11 1.337(10) . ? C10 H10A 0.9300 . ? C11 C12 1.371(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.373(8) . ? C13 C18 1.380(8) . ? C14 C15 1.384(10) . ? C14 H14A 0.9300 . ? C15 C16 1.367(11) . ? C15 H15A 0.9300 . ? C16 C17 1.346(11) . ? C16 H16A 0.9300 . ? C17 C18 1.373(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C24 1.378(7) . ? C19 C20 1.380(8) . ? C20 C21 1.382(8) . ? C20 H20A 0.9300 . ? C21 C22 1.370(9) . ? C21 H21A 0.9300 . ? C22 C23 1.358(9) . ? C22 H22A 0.9300 . ? C23 C24 1.381(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.366(9) . ? C25 C30 1.375(9) . ? C26 C27 1.401(11) . ? C26 H26A 0.9300 . ? C27 C28 1.341(12) . ? C27 H27A 0.9300 . ? C28 C29 1.332(12) . ? C28 H28A 0.9300 . ? C29 C30 1.378(10) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 N5 1.347(7) . ? C31 N6 1.347(7) . ? C31 N4 1.367(7) . ? C32 N6 1.318(9) . ? C32 C33 1.395(11) . ? C32 C36 1.502(9) . ? C33 C34 1.367(9) . ? C33 H33A 0.9300 . ? C34 N4 1.331(8) . ? C34 C35 1.501(10) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C42 1.374(9) . ? C37 C38 1.374(9) . ? C38 C39 1.384(10) . ? C38 H38A 0.9300 . ? C39 C40 1.369(13) . ? C39 H39A 0.9300 . ? C40 C41 1.346(13) . ? C40 H40A 0.9300 . ? C41 C42 1.386(11) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.371(8) . ? C43 C48 1.372(8) . ? C44 C45 1.389(9) . ? C44 H44A 0.9300 . ? C45 C46 1.382(11) . ? C45 H45A 0.9300 . ? C46 C47 1.359(11) . ? C46 H46A 0.9300 . ? C47 C48 1.379(10) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 C54 1.373(9) . ? C49 C50 1.380(9) . ? C50 C51 1.389(12) . ? C50 H50A 0.9300 . ? C51 C52 1.337(13) . ? C51 H51A 0.9300 . ? C52 C53 1.338(13) . ? C52 H52A 0.9300 . ? C53 C54 1.389(10) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C55 C60 1.382(8) . ? C55 C56 1.385(8) . ? C56 C57 1.371(9) . ? C56 H56A 0.9300 . ? C57 C58 1.370(11) . ? C57 H57A 0.9300 . ? C58 C59 1.379(11) . ? C58 H58A 0.9300 . ? C59 C60 1.365(10) . ? C59 H59A 0.9300 . ? C60 H60A 0.9300 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? N1 H1A 0.8600 . ? N5 Ag3 2.539(5) 3_566 ? N5 H5D 0.8600 . ? 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 N2 Ag1 P3 160.02(13) . . y N2 Ag1 Ag2 85.11(12) . . y P3 Ag1 Ag2 96.60(4) . . y N2 Ag1 Ag2 72.06(12) . 3_676 y P3 Ag1 Ag2 127.71(5) . 3_676 y Ag2 Ag1 Ag2 90.33(3) . 3_676 y N1 Ag2 P4 166.33(13) . . y N1 Ag2 Ag1 79.13(13) . . y P4 Ag2 Ag1 88.72(4) . . y N1 Ag2 Ag1 57.29(14) . 3_676 y P4 Ag2 Ag1 129.59(4) . 3_676 y Ag1 Ag2 Ag1 89.67(3) . 3_676 y N4 Ag3 P2 150.76(13) . . y N4 Ag3 N5 107.07(16) . 3_566 y P2 Ag3 N5 102.16(11) . 3_566 y N4 Ag3 Ag4 83.80(13) . . y P2 Ag3 Ag4 92.53(4) . . y N5 Ag3 Ag4 99.02(11) 3_566 . y N5 Ag4 P1 169.24(14) . . y N5 Ag4 Ag3 78.23(14) . . y P1 Ag4 Ag3 92.19(4) . . y O2 Cl1 O4 120.5(5) . . ? O2 Cl1 O3 115.9(5) . . ? O4 Cl1 O3 110.3(5) . . ? O2 Cl1 O1 99.6(8) . . ? O4 Cl1 O1 104.4(7) . . ? O3 Cl1 O1 103.1(8) . . ? O8 Cl2 O5 109.9(5) . . ? O8 Cl2 O7 111.0(6) . . ? O5 Cl2 O7 108.3(5) . . ? O8 Cl2 O6 112.9(6) . . ? O5 Cl2 O6 107.8(3) . . ? O7 Cl2 O6 106.8(4) . . ? C43 P1 C37 108.1(3) . . ? C43 P1 C62 104.3(3) . . ? C37 P1 C62 102.3(3) . . ? C43 P1 Ag4 109.99(19) . . ? C37 P1 Ag4 117.2(2) . . ? C62 P1 Ag4 113.92(18) . . ? C49 P2 C55 105.8(3) . . ? C49 P2 C62 105.6(3) . . ? C55 P2 C62 101.6(3) . . ? C49 P2 Ag3 116.0(2) . . ? C55 P2 Ag3 115.57(18) . . ? C62 P2 Ag3 110.90(18) . . ? C25 P3 C7 105.0(3) . . ? C25 P3 C61 104.6(3) . . ? C7 P3 C61 104.4(3) . . ? C25 P3 Ag1 117.5(2) . . ? C7 P3 Ag1 115.09(18) . . ? C61 P3 Ag1 109.08(17) . . ? C13 P4 C19 108.4(2) . . ? C13 P4 C61 105.7(2) . . ? C19 P4 C61 101.3(2) . . ? C13 P4 Ag2 109.45(18) . . ? C19 P4 Ag2 115.75(18) . . ? C61 P4 Ag2 115.53(17) . . ? N1 C1 N2 119.2(5) . . ? N1 C1 N3 118.9(5) . . ? N2 C1 N3 121.9(5) . . ? N2 C2 C3 121.3(6) . . ? N2 C2 C5 115.9(6) . . ? C3 C2 C5 122.7(6) . . ? C4 C3 C2 118.5(6) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? N3 C4 C3 121.8(6) . . ? N3 C4 C6 116.5(6) . . ? C3 C4 C6 121.7(6) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 117.7(6) . . ? C8 C7 P3 118.3(5) . . ? C12 C7 P3 124.0(4) . . ? C7 C8 C9 120.6(6) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C10 C9 C8 120.4(7) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 120.0(7) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.7(7) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 120.6(6) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? C14 C13 C18 117.7(6) . . ? C14 C13 P4 118.6(4) . . ? C18 C13 P4 123.7(5) . . ? C13 C14 C15 120.5(7) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 120.4(8) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C18 120.5(7) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C17 C18 C13 121.2(7) . . ? C17 C18 H18A 119.4 . . ? C13 C18 H18A 119.4 . . ? C24 C19 C20 118.9(5) . . ? C24 C19 P4 118.8(4) . . ? C20 C19 P4 122.3(4) . . ? C19 C20 C21 120.4(6) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C22 C21 C20 119.8(6) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C23 C22 C21 120.3(6) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C19 C24 C23 120.4(6) . . ? C19 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C26 C25 C30 118.2(6) . . ? C26 C25 P3 119.0(5) . . ? C30 C25 P3 122.8(5) . . ? C25 C26 C27 119.8(8) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 120.4(9) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C29 C28 C27 120.2(8) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C28 C29 C30 120.8(8) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C25 C30 C29 120.5(7) . . ? C25 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? N5 C31 N6 118.1(5) . . ? N5 C31 N4 118.1(5) . . ? N6 C31 N4 123.7(5) . . ? N6 C32 C33 121.5(6) . . ? N6 C32 C36 117.2(7) . . ? C33 C32 C36 121.4(7) . . ? C34 C33 C32 117.9(7) . . ? C34 C33 H33A 121.0 . . ? C32 C33 H33A 121.0 . . ? N4 C34 C33 121.8(7) . . ? N4 C34 C35 116.5(6) . . ? C33 C34 C35 121.7(6) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 118.2(6) . . ? C42 C37 P1 119.1(5) . . ? C38 C37 P1 122.7(5) . . ? C37 C38 C39 121.4(8) . . ? C37 C38 H38A 119.3 . . ? C39 C38 H38A 119.3 . . ? C40 C39 C38 118.5(9) . . ? C40 C39 H39A 120.7 . . ? C38 C39 H39A 120.7 . . ? C41 C40 C39 121.5(8) . . ? C41 C40 H40A 119.3 . . ? C39 C40 H40A 119.3 . . ? C40 C41 C42 119.5(8) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C37 C42 C41 120.9(8) . . ? C37 C42 H42A 119.6 . . ? C41 C42 H42A 119.6 . . ? C44 C43 C48 118.6(6) . . ? C44 C43 P1 118.6(4) . . ? C48 C43 P1 122.7(5) . . ? C43 C44 C45 121.5(6) . . ? C43 C44 H44A 119.2 . . ? C45 C44 H44A 119.2 . . ? C46 C45 C44 118.8(8) . . ? C46 C45 H45A 120.6 . . ? C44 C45 H45A 120.6 . . ? C47 C46 C45 119.7(7) . . ? C47 C46 H46A 120.2 . . ? C45 C46 H46A 120.2 . . ? C46 C47 C48 121.1(7) . . ? C46 C47 H47A 119.4 . . ? C48 C47 H47A 119.4 . . ? C43 C48 C47 120.2(7) . . ? C43 C48 H48A 119.9 . . ? C47 C48 H48A 119.9 . . ? C54 C49 C50 118.0(6) . . ? C54 C49 P2 123.0(5) . . ? C50 C49 P2 119.0(5) . . ? C49 C50 C51 120.0(8) . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C52 C51 C50 120.5(10) . . ? C52 C51 H51A 119.7 . . ? C50 C51 H51A 119.7 . . ? C51 C52 C53 120.9(9) . . ? C51 C52 H52A 119.6 . . ? C53 C52 H52A 119.6 . . ? C52 C53 C54 119.9(9) . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C49 C54 C53 120.7(8) . . ? C49 C54 H54A 119.7 . . ? C53 C54 H54A 119.7 . . ? C60 C55 C56 118.7(6) . . ? C60 C55 P2 117.8(5) . . ? C56 C55 P2 123.5(4) . . ? C57 C56 C55 121.0(6) . . ? C57 C56 H56A 119.5 . . ? C55 C56 H56A 119.5 . . ? C58 C57 C56 119.6(7) . . ? C58 C57 H57A 120.2 . . ? C56 C57 H57A 120.2 . . ? C57 C58 C59 120.0(7) . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C60 C59 C58 120.4(7) . . ? C60 C59 H59A 119.8 . . ? C58 C59 H59A 119.8 . . ? C59 C60 C55 120.3(7) . . ? C59 C60 H60A 119.8 . . ? C55 C60 H60A 119.8 . . ? P3 C61 P4 113.3(3) . . ? P3 C61 H61A 108.9 . . ? P4 C61 H61A 108.9 . . ? P3 C61 H61B 108.9 . . ? P4 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? P2 C62 P1 115.0(3) . . ? P2 C62 H62A 108.5 . . ? P1 C62 H62A 108.5 . . ? P2 C62 H62B 108.5 . . ? P1 C62 H62B 108.5 . . ? H62A C62 H62B 107.5 . . ? C1 N1 Ag2 129.1(4) . . ? C1 N1 H1A 115.4 . . ? Ag2 N1 H1A 115.4 . . ? C2 N2 C1 117.7(5) . . ? C2 N2 Ag1 121.2(4) . . ? C1 N2 Ag1 121.0(4) . . ? C4 N3 C1 118.6(5) . . ? C34 N4 C31 117.1(5) . . ? C34 N4 Ag3 122.0(4) . . ? C31 N4 Ag3 120.9(4) . . ? C31 N5 Ag4 129.6(4) . . ? C31 N5 Ag3 105.8(3) . 3_566 ? Ag4 N5 Ag3 94.13(18) . 3_566 ? C31 N5 H5D 115.2 . . ? Ag4 N5 H5D 115.2 . . ? Ag3 N5 H5D 66.1 3_566 . ? C32 N6 C31 117.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.271 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.088 ########################################### # end Validation Reply Form ################################################ data_p2 _database_code_depnum_ccdc_archive 'CCDC 743901' #TrackingRef '- p1-3-r2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H64 Ag4 Cl2 O12 P6, 2(C3 H7 N O) ' _chemical_formula_sum 'C80 H78 Ag4 Cl2 N2 O14 P6' _chemical_formula_weight 1979.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_HALL '-P 2yn' 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 11.453(2) _cell_length_b 15.193(3) _cell_length_c 23.416(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.14(3) _cell_angle_gamma 90.00 _cell_volume 4043.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 18666 _cell_measurement_theta_min 5.99 _cell_measurement_theta_max 54.98 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7949 _exptl_absorpt_correction_T_max 0.8892 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31261 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7115 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Positional parameters for the DMF molecule (C38 C39 C40 N1 O7) which is most likely also disordered, were refined with isotropic thermal parameters. The following restrains were applied to the disordered DMF: dfix 1.44 0.01 n1 c38 n1 c39 dfix 1.35 0.01 n1 c40 dfix 1.25 0.01 c40 o7 dfix 2.50 0.01 c38 c39 ; _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^)+(0.1370P)^2^+9.8827P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7115 _refine_ls_number_parameters 463 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2748 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.146 _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 0.96320(8) 1.07860(5) -0.08914(4) 0.0567(3) Uani 1 1 d . . . Ag2 Ag 0.83361(8) 1.08068(5) 0.02523(4) 0.0559(3) Uani 1 1 d . . . P1 P 0.8699(2) 1.21392(16) -0.11654(11) 0.0464(7) Uani 1 1 d . . . P2 P 0.7415(2) 1.21460(16) -0.00759(12) 0.0471(7) Uani 1 1 d . . . P3 P 0.8699(2) 0.89353(17) -0.04004(12) 0.0456(6) Uani 1 1 d . . . C1 C 0.5957(10) 1.2025(6) -0.0458(5) 0.056(3) Uani 1 1 d . . . C2 C 0.5282(13) 1.2728(9) -0.0688(8) 0.098(5) Uani 1 1 d . . . H2A H 0.5563 1.3298 -0.0626 0.117 Uiso 1 1 calc R . . C3 C 0.4201(13) 1.2594(11) -0.1007(8) 0.100(5) Uani 1 1 d . . . H3A H 0.3778 1.3075 -0.1167 0.120 Uiso 1 1 calc R . . C4 C 0.3750(13) 1.1784(11) -0.1090(6) 0.084(4) Uani 1 1 d . . . H4A H 0.3008 1.1707 -0.1295 0.101 Uiso 1 1 calc R . . C5 C 0.4361(14) 1.1100(11) -0.0880(9) 0.110(6) Uani 1 1 d . . . H5A H 0.4051 1.0538 -0.0943 0.132 Uiso 1 1 calc R . . C6 C 0.5472(12) 1.1206(9) -0.0562(7) 0.080(4) Uani 1 1 d . . . H6A H 0.5889 1.0711 -0.0420 0.096 Uiso 1 1 calc R . . C7 C 0.7342(10) 0.8982(7) -0.0861(5) 0.051(3) Uani 1 1 d . . . C8 C 0.7299(14) 0.8994(8) -0.1458(5) 0.073(3) Uani 1 1 d . . . H8A H 0.7989 0.9026 -0.1629 0.087 Uiso 1 1 calc R . . C9 C 0.6212(16) 0.8958(10) -0.1796(7) 0.090(5) Uani 1 1 d . . . H9A H 0.6190 0.8974 -0.2194 0.108 Uiso 1 1 calc R . . C10 C 0.5199(17) 0.8900(10) -0.1572(8) 0.097(5) Uani 1 1 d . . . H10A H 0.4489 0.8886 -0.1812 0.117 Uiso 1 1 calc R . . C11 C 0.5206(12) 0.8863(9) -0.0990(8) 0.084(4) Uani 1 1 d . . . H11A H 0.4506 0.8804 -0.0831 0.101 Uiso 1 1 calc R . . C12 C 0.6273(12) 0.8914(8) -0.0638(6) 0.071(3) Uani 1 1 d . . . H12A H 0.6273 0.8904 -0.0241 0.085 Uiso 1 1 calc R . . C13 C 0.8959(9) 0.7771(6) -0.0329(5) 0.052(3) Uani 1 1 d . . . C14 C 0.9510(12) 0.7337(8) -0.0750(6) 0.075(4) Uani 1 1 d . . . H14A H 0.9805 0.7647 -0.1043 0.090 Uiso 1 1 calc R . . C15 C 0.9602(16) 0.6415(10) -0.0713(9) 0.107(6) Uani 1 1 d . . . H15A H 0.9972 0.6116 -0.0988 0.128 Uiso 1 1 calc R . . C16 C 0.9180(18) 0.5951(10) -0.0300(10) 0.116(8) Uani 1 1 d . . . H16A H 0.9253 0.5341 -0.0291 0.139 Uiso 1 1 calc R . . C17 C 0.8634(16) 0.6382(10) 0.0114(8) 0.098(5) Uani 1 1 d . . . H17A H 0.8342 0.6057 0.0401 0.118 Uiso 1 1 calc R . . C18 C 0.8513(13) 0.7307(8) 0.0111(6) 0.078(4) Uani 1 1 d . . . H18A H 0.8149 0.7596 0.0391 0.094 Uiso 1 1 calc R . . C19 C 0.9667(10) 1.2903(7) -0.1476(4) 0.051(3) Uani 1 1 d . . . C20 C 1.0581(11) 1.2542(8) -0.1750(5) 0.063(3) Uani 1 1 d . . . H20A H 1.0662 1.1934 -0.1772 0.075 Uiso 1 1 calc R . . C21 C 1.1369(13) 1.3093(11) -0.1987(6) 0.085(4) Uani 1 1 d . . . H21A H 1.1967 1.2847 -0.2170 0.103 Uiso 1 1 calc R . . C22 C 1.1279(14) 1.3968(10) -0.1956(6) 0.078(4) Uani 1 1 d . . . H22A H 1.1805 1.4327 -0.2119 0.094 Uiso 1 1 calc R . . C23 C 1.0382(15) 1.4339(8) -0.1675(7) 0.086(5) Uani 1 1 d . . . H23A H 1.0321 1.4948 -0.1648 0.104 Uiso 1 1 calc R . . C24 C 0.9602(12) 1.3815(8) -0.1443(5) 0.067(3) Uani 1 1 d . . . H24A H 0.9014 1.4071 -0.1258 0.081 Uiso 1 1 calc R . . C25 C 0.7415(11) 1.2087(7) -0.1706(5) 0.060(3) Uani 1 1 d . . . C26 C 0.6890(19) 1.1300(10) -0.1836(8) 0.122(7) Uani 1 1 d . . . H26A H 0.7227 1.0785 -0.1676 0.146 Uiso 1 1 calc R . . C27 C 0.584(2) 1.1263(16) -0.2210(10) 0.142(8) Uani 1 1 d U . . H27A H 0.5425 1.0736 -0.2264 0.170 Uiso 1 1 calc R . . C28 C 0.5436(16) 1.1984(13) -0.2489(7) 0.105(5) Uani 1 1 d . . . H28A H 0.4779 1.1946 -0.2765 0.126 Uiso 1 1 calc R . . C29 C 0.5937(15) 1.2732(13) -0.2385(7) 0.103(5) Uani 1 1 d . . . H29A H 0.5639 1.3229 -0.2585 0.124 Uiso 1 1 calc R . . C30 C 0.6908(16) 1.2808(10) -0.1980(8) 0.111(6) Uani 1 1 d . . . H30A H 0.7226 1.3362 -0.1892 0.133 Uiso 1 1 calc R . . C31 C 0.7268(10) 1.2931(7) 0.0506(5) 0.056(3) Uani 1 1 d . . . C32 C 0.7387(11) 1.2625(9) 0.1054(5) 0.070(3) Uani 1 1 d . . . H32A H 0.7559 1.2034 0.1127 0.084 Uiso 1 1 calc R . . C33 C 0.7253(14) 1.3186(12) 0.1501(6) 0.090(5) Uani 1 1 d . . . H33A H 0.7335 1.2977 0.1877 0.107 Uiso 1 1 calc R . . C34 C 0.6990(17) 1.4079(11) 0.1388(7) 0.106(6) Uani 1 1 d . . . H34A H 0.6867 1.4454 0.1689 0.127 Uiso 1 1 calc R . . C35 C 0.6915(15) 1.4401(10) 0.0837(7) 0.090(4) Uani 1 1 d U . . H35A H 0.6781 1.4997 0.0764 0.108 Uiso 1 1 calc R . . C36 C 0.7044(13) 1.3819(8) 0.0393(5) 0.074(4) Uani 1 1 d . . . H36A H 0.6980 1.4024 0.0016 0.089 Uiso 1 1 calc R . . C37 C 0.8195(9) 1.2783(6) -0.0558(4) 0.043(2) Uani 1 1 d . . . H37A H 0.8877 1.3051 -0.0338 0.052 Uiso 1 1 calc R . . H37B H 0.7686 1.3256 -0.0719 0.052 Uiso 1 1 calc R . . C38 C 0.594(4) 1.644(2) -0.1980(9) 0.30(2) Uiso 1 1 d D . . H38A H 0.6033 1.6076 -0.2308 0.453 Uiso 1 1 calc R . . H38B H 0.6461 1.6935 -0.1975 0.453 Uiso 1 1 calc R . . H38C H 0.5144 1.6638 -0.2003 0.453 Uiso 1 1 calc R . . C39 C 0.612(4) 1.636(2) -0.0914(9) 0.274(18) Uiso 1 1 d D . . H39A H 0.6371 1.5969 -0.0602 0.411 Uiso 1 1 calc R . . H39B H 0.5308 1.6518 -0.0901 0.411 Uiso 1 1 calc R . . H39C H 0.6593 1.6882 -0.0880 0.411 Uiso 1 1 calc R . . C40 C 0.665(4) 1.5102(17) -0.1464(10) 0.35(3) Uiso 1 1 d D . . H40A H 0.6832 1.4851 -0.1804 0.426 Uiso 1 1 calc R . . N1 N 0.6232(16) 1.5928(10) -0.1457(8) 0.126(5) Uiso 1 1 d D . . O1 O 1.0361(15) 1.0109(11) -0.1856(6) 0.164(7) Uani 1 1 d . . . O2 O 1.1581(15) 0.8975(8) -0.2112(7) 0.148(6) Uani 1 1 d . . . O3 O 1.2151(14) 1.0412(9) -0.2171(5) 0.135(5) Uani 1 1 d . . . O4 O 1.2094(12) 0.9726(9) -0.1289(5) 0.125(4) Uani 1 1 d U . . O5 O 0.9663(6) 0.9336(4) -0.0704(3) 0.0510(17) Uani 1 1 d . . . O6 O 0.8545(6) 0.9317(4) 0.0181(3) 0.0473(16) Uani 1 1 d . . . O7 O 0.6783(13) 1.4675(9) -0.1002(6) 0.129(4) Uiso 1 1 d D . . Cl1 Cl 1.1516(3) 0.9804(2) -0.18635(14) 0.0743(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0614(6) 0.0522(5) 0.0569(6) 0.0072(4) 0.0086(4) 0.0090(4) Ag2 0.0517(6) 0.0538(5) 0.0626(6) 0.0066(4) 0.0087(4) 0.0077(4) P1 0.0467(16) 0.0457(13) 0.0469(15) 0.0024(11) 0.0060(13) 0.0015(11) P2 0.0438(16) 0.0466(14) 0.0512(15) 0.0019(11) 0.0067(13) 0.0010(11) P3 0.0408(15) 0.0447(13) 0.0501(15) -0.0002(11) 0.0010(12) -0.0023(11) C1 0.048(7) 0.045(5) 0.076(8) -0.004(5) 0.006(6) 0.003(5) C2 0.064(9) 0.059(7) 0.160(16) 0.004(9) -0.026(10) -0.002(7) C3 0.052(9) 0.100(11) 0.140(15) 0.020(10) -0.020(9) 0.013(8) C4 0.059(9) 0.113(11) 0.077(9) -0.020(8) -0.007(7) -0.002(8) C5 0.054(9) 0.093(10) 0.170(18) -0.026(11) -0.036(11) -0.003(8) C6 0.061(9) 0.069(8) 0.106(11) -0.017(7) -0.004(8) -0.001(6) C7 0.045(6) 0.052(6) 0.056(6) -0.003(5) 0.005(5) -0.006(5) C8 0.083(10) 0.073(8) 0.060(7) 0.008(6) 0.001(7) -0.001(7) C9 0.086(12) 0.105(11) 0.068(9) 0.019(8) -0.032(9) -0.009(9) C10 0.095(14) 0.092(10) 0.092(12) -0.006(9) -0.041(10) -0.006(9) C11 0.040(7) 0.088(9) 0.122(13) -0.016(9) 0.000(8) -0.015(6) C12 0.070(9) 0.070(7) 0.067(8) -0.012(6) -0.012(7) -0.012(6) C13 0.038(6) 0.041(5) 0.073(7) -0.001(5) -0.008(5) -0.002(4) C14 0.071(9) 0.068(7) 0.087(9) -0.015(7) 0.017(8) 0.012(6) C15 0.107(14) 0.065(9) 0.139(15) -0.036(10) -0.022(12) 0.035(9) C16 0.118(16) 0.053(8) 0.156(19) 0.006(10) -0.066(15) 0.002(9) C17 0.105(13) 0.072(9) 0.108(12) 0.029(9) -0.028(11) -0.016(9) C18 0.083(10) 0.063(7) 0.086(9) 0.016(7) 0.003(8) -0.014(7) C19 0.054(7) 0.057(6) 0.043(5) 0.006(5) 0.007(5) 0.001(5) C20 0.061(8) 0.071(7) 0.058(7) -0.005(6) 0.014(6) -0.003(6) C21 0.066(9) 0.128(13) 0.065(8) 0.001(8) 0.016(7) -0.006(9) C22 0.075(10) 0.097(10) 0.064(8) 0.003(7) 0.018(7) -0.027(8) C23 0.105(13) 0.054(7) 0.091(10) -0.008(7) -0.024(10) -0.023(7) C24 0.079(9) 0.075(8) 0.048(6) -0.001(6) 0.011(6) 0.006(7) C25 0.062(8) 0.058(6) 0.060(7) -0.003(5) 0.009(6) -0.002(5) C26 0.147(18) 0.069(9) 0.129(14) 0.003(9) -0.067(13) -0.022(10) C27 0.142(9) 0.139(9) 0.140(9) 0.000(5) 0.007(5) -0.003(5) C28 0.082(12) 0.135(15) 0.088(11) 0.006(11) -0.036(9) -0.005(11) C29 0.086(12) 0.119(13) 0.092(11) 0.005(10) -0.036(10) 0.017(10) C30 0.094(13) 0.083(10) 0.140(15) 0.001(10) -0.045(11) 0.027(9) C31 0.056(7) 0.052(6) 0.059(7) -0.013(5) 0.004(6) -0.002(5) C32 0.064(8) 0.085(8) 0.063(8) -0.010(7) 0.014(7) -0.016(7) C33 0.090(11) 0.130(13) 0.050(7) -0.014(8) 0.018(7) -0.042(10) C34 0.133(16) 0.108(12) 0.086(11) -0.045(9) 0.050(11) -0.038(11) C35 0.096(6) 0.085(5) 0.089(6) -0.010(4) 0.017(5) -0.003(4) C36 0.097(11) 0.073(8) 0.056(7) -0.013(6) 0.018(7) -0.001(7) C37 0.048(6) 0.035(4) 0.046(5) 0.001(4) 0.004(5) -0.005(4) O1 0.159(14) 0.209(16) 0.134(11) 0.027(10) 0.059(11) 0.101(12) O2 0.161(14) 0.112(9) 0.179(13) -0.077(9) 0.051(11) 0.002(9) O3 0.195(15) 0.130(9) 0.089(8) 0.020(7) 0.055(9) -0.034(10) O4 0.125(6) 0.135(6) 0.114(5) 0.005(4) 0.011(4) -0.019(4) O5 0.030(4) 0.055(4) 0.066(4) 0.008(3) -0.006(3) 0.000(3) O6 0.044(4) 0.048(4) 0.048(4) -0.006(3) -0.001(3) 0.001(3) Cl1 0.088(3) 0.0757(19) 0.0611(18) -0.0071(15) 0.0193(18) 0.0017(17) _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 O5 2.246(7) . y Ag1 P1 2.369(3) . y Ag1 O6 2.508(7) 3_775 y Ag1 Ag2 3.2192(14) . y Ag2 O6 2.284(6) . y Ag2 P2 2.375(3) . y Ag2 O5 2.412(7) 3_775 y P1 C19 1.819(10) . ? P1 C25 1.819(13) . ? P1 C37 1.875(9) . ? P2 C1 1.804(12) . ? P2 C37 1.807(9) . ? P2 C31 1.835(10) . ? P3 O6 1.510(7) . ? P3 O5 1.513(7) . ? P3 C7 1.780(12) . ? P3 C13 1.799(10) . ? C1 C6 1.373(16) . ? C1 C2 1.387(17) . ? C2 C3 1.38(2) . ? C2 H2A 0.9300 . ? C3 C4 1.34(2) . ? C3 H3A 0.9300 . ? C4 C5 1.31(2) . ? C4 H4A 0.9300 . ? C5 C6 1.40(2) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.393(16) . ? C7 C12 1.394(17) . ? C8 C9 1.39(2) . ? C8 H8A 0.9300 . ? C9 C10 1.33(2) . ? C9 H9A 0.9300 . ? C10 C11 1.36(2) . ? C10 H10A 0.9300 . ? C11 C12 1.389(19) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.396(16) . ? C13 C14 1.400(16) . ? C14 C15 1.41(2) . ? C14 H14A 0.9300 . ? C15 C16 1.33(3) . ? C15 H15A 0.9300 . ? C16 C17 1.38(3) . ? C16 H16A 0.9300 . ? C17 C18 1.41(2) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C24 1.389(15) . ? C19 C20 1.405(15) . ? C20 C21 1.396(18) . ? C20 H20A 0.9300 . ? C21 C22 1.34(2) . ? C21 H21A 0.9300 . ? C22 C23 1.41(2) . ? C22 H22A 0.9300 . ? C23 C24 1.360(19) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.356(18) . ? C25 C30 1.363(18) . ? C26 C27 1.40(3) . ? C26 H26A 0.9300 . ? C27 C28 1.33(3) . ? C27 H27A 0.9300 . ? C28 C29 1.28(2) . ? C28 H28A 0.9300 . ? C29 C30 1.37(2) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.355(16) . ? C31 C36 1.392(16) . ? C32 C33 1.374(18) . ? C32 H32A 0.9300 . ? C33 C34 1.41(2) . ? C33 H33A 0.9300 . ? C34 C35 1.37(2) . ? C34 H34A 0.9300 . ? C35 C36 1.388(18) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N1 1.451(10) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N1 1.452(10) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 O7 1.254(10) . ? C40 N1 1.343(10) . ? C40 H40A 0.9300 . ? O1 Cl1 1.404(14) . ? O2 Cl1 1.394(11) . ? O3 Cl1 1.424(11) . ? O4 Cl1 1.428(13) . ? O5 Ag2 2.412(7) 3_775 ? O6 Ag1 2.508(7) 3_775 ? 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 O5 Ag1 P1 154.16(19) . . y O5 Ag1 O6 79.5(2) . 3_775 y P1 Ag1 O6 122.99(16) . 3_775 y O5 Ag1 Ag2 81.08(19) . . y P1 Ag1 Ag2 88.72(7) . . y O6 Ag1 Ag2 83.15(16) 3_775 . y O6 Ag2 P2 150.62(19) . . y O6 Ag2 O5 80.8(2) . 3_775 y P2 Ag2 O5 125.34(17) . 3_775 y O6 Ag2 Ag1 82.31(18) . . y P2 Ag2 Ag1 88.36(7) . . y O5 Ag2 Ag1 81.54(18) 3_775 . y C19 P1 C25 103.3(5) . . ? C19 P1 C37 103.3(4) . . ? C25 P1 C37 104.6(5) . . ? C19 P1 Ag1 112.7(4) . . ? C25 P1 Ag1 116.7(4) . . ? C37 P1 Ag1 114.8(3) . . ? C1 P2 C37 104.1(5) . . ? C1 P2 C31 105.7(5) . . ? C37 P2 C31 102.4(5) . . ? C1 P2 Ag2 114.8(3) . . ? C37 P2 Ag2 115.3(3) . . ? C31 P2 Ag2 113.2(4) . . ? O6 P3 O5 116.3(4) . . ? O6 P3 C7 109.9(5) . . ? O5 P3 C7 109.4(5) . . ? O6 P3 C13 109.3(5) . . ? O5 P3 C13 108.5(5) . . ? C7 P3 C13 102.5(5) . . ? C6 C1 C2 115.8(12) . . ? C6 C1 P2 120.6(9) . . ? C2 C1 P2 123.4(9) . . ? C3 C2 C1 121.1(13) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C4 C3 C2 121.2(14) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C5 C4 C3 119.6(15) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.0(15) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C1 C6 C5 121.2(14) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C12 117.0(12) . . ? C8 C7 P3 121.8(10) . . ? C12 C7 P3 120.8(9) . . ? C9 C8 C7 119.1(14) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C10 C9 C8 122.8(15) . . ? C10 C9 H9A 118.6 . . ? C8 C9 H9A 118.6 . . ? C9 C10 C11 119.8(16) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C10 C11 C12 119.2(15) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C11 C12 C7 122.0(13) . . ? C11 C12 H12A 119.0 . . ? C7 C12 H12A 119.0 . . ? C18 C13 C14 121.3(11) . . ? C18 C13 P3 119.6(9) . . ? C14 C13 P3 118.8(9) . . ? C13 C14 C15 117.6(15) . . ? C13 C14 H14A 121.2 . . ? C15 C14 H14A 121.2 . . ? C16 C15 C14 122.6(17) . . ? C16 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C15 C16 C17 119.6(15) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C18 121.3(16) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C13 C18 C17 117.5(14) . . ? C13 C18 H18A 121.2 . . ? C17 C18 H18A 121.2 . . ? C24 C19 C20 117.6(10) . . ? C24 C19 P1 125.0(9) . . ? C20 C19 P1 117.3(8) . . ? C21 C20 C19 120.1(12) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C22 C21 C20 121.2(13) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C23 119.4(12) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 120.4(12) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C19 121.3(12) . . ? C23 C24 H24A 119.4 . . ? C19 C24 H24A 119.4 . . ? C26 C25 C30 116.9(14) . . ? C26 C25 P1 119.5(11) . . ? C30 C25 P1 123.6(10) . . ? C25 C26 C27 119.9(17) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 120(2) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C29 C28 C27 121.1(19) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C30 120.7(17) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C25 C30 C29 121.3(16) . . ? C25 C30 H30A 119.4 . . ? C29 C30 H30A 119.4 . . ? C32 C31 C36 120.5(11) . . ? C32 C31 P2 118.2(9) . . ? C36 C31 P2 121.3(9) . . ? C31 C32 C33 120.0(14) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C33 C34 119.8(14) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 120.5(13) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 118.5(15) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? C35 C36 C31 120.6(13) . . ? C35 C36 H36A 119.7 . . ? C31 C36 H36A 119.7 . . ? P2 C37 P1 114.7(5) . . ? P2 C37 H37A 108.6 . . ? P1 C37 H37A 108.6 . . ? P2 C37 H37B 108.6 . . ? P1 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? N1 C38 H38A 109.5 . . ? N1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 N1 119(2) . . ? O7 C40 H40A 120.7 . . ? N1 C40 H40A 120.7 . . ? C40 N1 C38 122(2) . . ? C40 N1 C39 120(2) . . ? C38 N1 C39 117.4(11) . . ? P3 O5 Ag1 119.4(4) . . ? P3 O5 Ag2 117.8(4) . 3_775 ? Ag1 O5 Ag2 99.5(3) . 3_775 ? P3 O6 Ag2 118.1(4) . . ? P3 O6 Ag1 113.1(4) . 3_775 ? Ag2 O6 Ag1 95.7(2) . 3_775 ? O2 Cl1 O1 113.8(11) . . ? O2 Cl1 O3 108.6(8) . . ? O1 Cl1 O3 109.5(9) . . ? O2 Cl1 O4 105.9(9) . . ? O1 Cl1 O4 110.0(8) . . ? O3 Cl1 O4 108.9(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.852 _refine_diff_density_min -1.323 _refine_diff_density_rms 0.181