# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Dr Christopher M. Fitchett' _publ_contact_author_address ;Department of Chemistry University of Canterbury Private Bag 4800 Christchurch 8140 New Zealand ; _publ_contact_author_email chris.fitchett@canterbury.ac.nz _publ_contact_author_phone '+64 3 3642460' _publ_contact_author_fax '+64 3 3642110' loop_ _publ_author_name _publ_author_address 'Dr Christopher M. Fitchett' ;Department of Chemistry University of Canterbury Privatge Bag 4800 Christchurch 8140 New Zealand ; J.L.Gulbransen ;Department of Chemistry University of Canterbury Privatge Bag 4800 Christchurch 8140 New Zealand ; data_1 _database_code_depnum_ccdc_archive 'CCDC 832767' #TrackingRef '- CMFJLGcecrevised.cif' _audit_creation_date 2012-06-10 _audit_creation_method ; Olex2 1.2-beta (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H16 Ag2 N8, 2(N O3)' _chemical_formula_sum 'C16 H16 Ag2 N10 O6' _chemical_formula_weight 660.13 _chemical_melting_point ? 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 13.4409(8) _cell_length_b 15.3904(8) _cell_length_c 19.3895(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.252(3) _cell_angle_gamma 90.00 _cell_volume 4010.0(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9962 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.80 _cell_measurement_theta_min 2.62 _exptl_absorpt_coefficient_mu 2.016 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0766 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.848091091762. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 2592 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 84288 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 1.69 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 6984 _reflns_number_total 9202 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.732 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.120 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 613 _refine_ls_number_reflns 9202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0308 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+3.7400P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0692 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.41488(2) 0.513954(16) 0.299352(13) 0.01946(7) Uani 1 1 d . . . Ag2 Ag 0.36670(2) 0.515715(16) 0.443981(13) 0.02016(7) Uani 1 1 d . . . Ag3 Ag 0.15217(2) 0.523775(16) 0.192752(13) 0.01860(7) Uani 1 1 d . . . Ag4 Ag 0.13057(2) 0.505975(15) 0.044076(13) 0.01799(7) Uani 1 1 d . . . O65 O -0.1722(2) 0.50548(15) 0.10112(13) 0.0243(6) Uani 1 1 d . . . O63 O -0.0480(2) 0.45938(16) 0.16503(14) 0.0330(7) Uani 1 1 d . . . O64 O -0.0919(2) 0.59448(16) 0.16825(13) 0.0313(7) Uani 1 1 d . . . O51 O 0.0438(2) 0.54811(16) 0.40426(15) 0.0307(7) Uani 1 1 d . . . O52 O 0.1588(2) 0.46182(17) 0.44384(14) 0.0335(7) Uani 1 1 d . . . O53 O 0.1888(2) 0.54606(18) 0.35768(14) 0.0350(7) Uani 1 1 d . . . O55 O 0.3189(2) 0.55095(16) 0.09358(14) 0.0291(6) Uani 1 1 d . . . O56 O 0.3858(2) 0.42604(18) 0.07309(14) 0.0400(8) Uani 1 1 d . . . O57 O 0.44994(19) 0.50815(16) 0.15281(12) 0.0227(6) Uani 1 1 d . . . O59 O 0.6152(2) 0.54700(19) 0.29691(16) 0.0443(8) Uani 1 1 d . . . O60 O 0.6152(3) 0.4689(2) 0.38694(16) 0.0659(12) Uani 1 1 d . . . O61 O 0.7411(2) 0.4661(2) 0.3214(2) 0.0591(11) Uani 1 1 d . . . N62 N -0.1044(2) 0.51984(18) 0.14510(14) 0.0191(6) Uani 1 1 d . . . N1 N 0.4120(2) 0.37356(17) 0.29619(14) 0.0154(6) Uani 1 1 d . . . N3 N 0.3889(2) 0.23248(17) 0.31275(14) 0.0151(6) Uani 1 1 d . . . N8 N 0.3986(2) 0.38306(17) 0.46039(14) 0.0166(6) Uani 1 1 d . . . N10 N 0.4019(2) 0.23996(17) 0.45357(14) 0.0164(6) Uani 1 1 d . . . N13 N 0.3806(2) 0.65084(17) 0.28835(14) 0.0154(6) Uani 1 1 d . . . N16 N 0.3478(2) 0.79131(17) 0.29747(14) 0.0162(6) Uani 1 1 d . . . N20 N 0.3561(2) 0.65256(18) 0.45179(14) 0.0180(6) Uani 1 1 d . . . N22 N 0.3513(2) 0.79485(17) 0.43830(15) 0.0165(6) Uani 1 1 d . . . N25 N 0.1698(2) 0.38828(17) 0.20915(14) 0.0159(6) Uani 1 1 d . . . N28 N 0.1455(2) 0.24651(18) 0.20839(14) 0.0160(6) Uani 1 1 d . . . N32 N 0.1420(2) 0.36769(17) 0.04510(14) 0.0158(6) Uani 1 1 d . . . N34 N 0.1545(2) 0.22768(17) 0.06928(14) 0.0154(6) Uani 1 1 d . . . N37 N 0.1075(2) 0.64294(17) 0.03049(14) 0.0159(6) Uani 1 1 d . . . N39 N 0.0994(2) 0.78585(17) 0.03512(14) 0.0160(6) Uani 1 1 d . . . N44 N 0.1318(2) 0.66006(18) 0.19518(14) 0.0166(6) Uani 1 1 d . . . N46 N 0.0907(2) 0.79667(17) 0.17522(14) 0.0159(6) Uani 1 1 d . . . N50 N 0.1295(2) 0.51852(18) 0.40176(15) 0.0199(7) Uani 1 1 d . . . N54 N 0.3855(2) 0.49493(18) 0.10591(14) 0.0194(7) Uani 1 1 d . . . N58 N 0.6581(3) 0.49393(18) 0.33502(15) 0.0236(7) Uani 1 1 d . . . C2 C 0.3996(3) 0.3115(2) 0.34317(17) 0.0144(7) Uani 1 1 d . . . C4 C 0.3938(3) 0.2441(2) 0.24270(17) 0.0171(7) Uani 1 1 d . . . H4 H 0.3886 0.2016 0.2087 0.021 Uiso 1 1 calc R . . C5 C 0.4078(3) 0.3312(2) 0.23325(17) 0.0169(7) Uani 1 1 d . . . H5 H 0.4137 0.3581 0.1906 0.020 Uiso 1 1 calc R . . C6 C 0.3644(3) 0.1527(2) 0.35037(17) 0.0182(8) Uani 1 1 d . . . H6A H 0.3865 0.1024 0.3247 0.022 Uiso 1 1 calc R . . H6B H 0.2929 0.1485 0.3553 0.022 Uiso 1 1 calc R . . C7 C 0.4152(3) 0.1542(2) 0.42099(17) 0.0206(8) Uani 1 1 d . . . H7A H 0.3869 0.1094 0.4498 0.025 Uiso 1 1 calc R . . H7B H 0.4856 0.1422 0.4165 0.025 Uiso 1 1 calc R . . C9 C 0.3991(3) 0.3153(2) 0.41751(17) 0.0143(7) Uani 1 1 d . . . C11 C 0.4053(3) 0.2600(2) 0.52237(18) 0.0199(8) Uani 1 1 d . . . H11 H 0.4084 0.2213 0.5592 0.024 Uiso 1 1 calc R . . C12 C 0.4030(3) 0.3486(2) 0.52583(17) 0.0181(7) Uani 1 1 d . . . H12 H 0.4043 0.3809 0.5664 0.022 Uiso 1 1 calc R . . C14 C 0.3744(3) 0.6878(2) 0.22345(18) 0.0171(7) Uani 1 1 d . . . H14 H 0.3830 0.6580 0.1823 0.021 Uiso 1 1 calc R . . C15 C 0.3539(3) 0.7735(2) 0.22865(17) 0.0187(8) Uani 1 1 d . . . H15 H 0.3457 0.8127 0.1925 0.022 Uiso 1 1 calc R . . C17 C 0.3631(3) 0.7155(2) 0.33195(17) 0.0144(7) Uani 1 1 d . . . C18 C 0.3157(3) 0.8718(2) 0.33089(18) 0.0213(8) Uani 1 1 d . . . H18A H 0.2437 0.8724 0.3337 0.026 Uiso 1 1 calc R . . H18B H 0.3357 0.9214 0.3036 0.026 Uiso 1 1 calc R . . C19 C 0.3617(3) 0.8786(2) 0.40262(18) 0.0211(8) Uani 1 1 d . . . H19A H 0.4316 0.8936 0.3997 0.025 Uiso 1 1 calc R . . H19B H 0.3287 0.9239 0.4283 0.025 Uiso 1 1 calc R . . C21 C 0.3579(3) 0.7166(2) 0.40651(17) 0.0159(7) Uani 1 1 d . . . C23 C 0.3464(3) 0.7795(2) 0.50793(18) 0.0199(8) Uani 1 1 d . . . H23 H 0.3416 0.8208 0.5427 0.024 Uiso 1 1 calc R . . C24 C 0.3501(3) 0.6915(2) 0.51571(18) 0.0204(8) Uani 1 1 d . . . H24 H 0.3489 0.6622 0.5576 0.024 Uiso 1 1 calc R . . C26 C 0.1704(3) 0.3578(2) 0.27610(17) 0.0176(7) Uani 1 1 d . . . H26 H 0.1801 0.3920 0.3152 0.021 Uiso 1 1 calc R . . C27 C 0.1547(3) 0.2704(2) 0.27645(17) 0.0168(7) Uani 1 1 d . . . H27 H 0.1510 0.2344 0.3148 0.020 Uiso 1 1 calc R . . C29 C 0.1545(2) 0.3185(2) 0.16979(17) 0.0142(7) Uani 1 1 d . . . C30 C 0.1223(3) 0.1597(2) 0.17961(17) 0.0187(8) Uani 1 1 d . . . H30A H 0.0509 0.1534 0.1732 0.022 Uiso 1 1 calc R . . H30B H 0.1455 0.1150 0.2113 0.022 Uiso 1 1 calc R . . C31 C 0.1731(3) 0.1498(2) 0.11097(17) 0.0184(7) Uani 1 1 d . . . H31A H 0.2441 0.1421 0.1186 0.022 Uiso 1 1 calc R . . H31B H 0.1473 0.0990 0.0869 0.022 Uiso 1 1 calc R . . C33 C 0.1501(3) 0.3090(2) 0.09523(17) 0.0135(7) Uani 1 1 d . . . C35 C 0.1512(3) 0.2344(2) -0.00162(17) 0.0175(8) Uani 1 1 d . . . H35 H 0.1541 0.1893 -0.0334 0.021 Uiso 1 1 calc R . . C36 C 0.1426(3) 0.3206(2) -0.01549(17) 0.0179(7) Uani 1 1 d . . . H36 H 0.1378 0.3445 -0.0595 0.022 Uiso 1 1 calc R . . C38 C 0.1070(3) 0.7115(2) 0.07191(17) 0.0139(7) Uani 1 1 d . . . C40 C 0.0958(3) 0.7644(2) -0.03326(18) 0.0181(7) Uani 1 1 d . . . H40 H 0.0916 0.8023 -0.0705 0.022 Uiso 1 1 calc R . . C41 C 0.0998(3) 0.6757(2) -0.03574(17) 0.0176(7) Uani 1 1 d . . . H41 H 0.0977 0.6426 -0.0758 0.021 Uiso 1 1 calc R . . C42 C 0.1046(3) 0.8735(2) 0.06564(18) 0.0195(8) Uani 1 1 d . . . H42A H 0.0708 0.9148 0.0355 0.023 Uiso 1 1 calc R . . H42B H 0.1735 0.8914 0.0711 0.023 Uiso 1 1 calc R . . C43 C 0.0555(3) 0.8718(2) 0.13538(17) 0.0180(7) Uani 1 1 d . . . H43A H 0.0712 0.9248 0.1604 0.022 Uiso 1 1 calc R . . H43B H -0.0162 0.8686 0.1289 0.022 Uiso 1 1 calc R . . C45 C 0.1111(3) 0.7181(2) 0.14679(17) 0.0145(7) Uani 1 1 d . . . C47 C 0.0964(3) 0.7869(2) 0.24529(17) 0.0181(7) Uani 1 1 d . . . H47 H 0.0847 0.8294 0.2782 0.022 Uiso 1 1 calc R . . C48 C 0.1226(3) 0.7029(2) 0.25731(18) 0.0183(8) Uani 1 1 d . . . H48 H 0.1328 0.6781 0.3006 0.022 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 0.02751(17) 0.01086(12) 0.02012(13) -0.00041(10) 0.00305(11) 0.00175(11) Ag2 0.02729(17) 0.01310(13) 0.02017(13) -0.00118(10) 0.00196(11) 0.00152(11) Ag3 0.02582(16) 0.01182(13) 0.01807(13) -0.00006(10) -0.00162(11) 0.00135(11) Ag4 0.02662(16) 0.01033(12) 0.01696(12) 0.00020(10) -0.00074(11) 0.00100(10) O65 0.0257(16) 0.0202(13) 0.0268(13) 0.0004(11) -0.0063(12) -0.0048(11) O63 0.0389(19) 0.0185(14) 0.0413(17) 0.0055(12) -0.0097(14) 0.0072(12) O64 0.053(2) 0.0165(13) 0.0240(14) -0.0068(11) -0.0064(13) 0.0026(12) O51 0.0202(16) 0.0226(14) 0.0489(18) -0.0104(12) -0.0098(13) 0.0046(11) O52 0.0388(18) 0.0227(14) 0.0387(16) 0.0127(12) -0.0088(14) 0.0055(12) O53 0.0358(19) 0.0331(16) 0.0362(16) 0.0072(13) 0.0035(14) -0.0083(13) O55 0.0257(16) 0.0169(13) 0.0443(17) 0.0047(12) -0.0065(13) 0.0030(11) O56 0.053(2) 0.0308(16) 0.0359(16) -0.0185(13) -0.0134(15) 0.0133(14) O57 0.0233(15) 0.0220(13) 0.0225(12) -0.0006(10) -0.0048(11) -0.0009(11) O59 0.041(2) 0.0343(17) 0.057(2) 0.0255(15) -0.0153(16) 0.0026(14) O60 0.119(4) 0.047(2) 0.0316(18) 0.0088(16) 0.009(2) -0.023(2) O61 0.032(2) 0.049(2) 0.096(3) -0.038(2) -0.0218(19) 0.0171(16) N62 0.0237(18) 0.0159(15) 0.0180(14) 0.0008(12) 0.0036(13) -0.0008(13) N1 0.0165(17) 0.0155(14) 0.0141(14) 0.0017(11) 0.0009(12) -0.0001(12) N3 0.0177(17) 0.0137(14) 0.0137(14) 0.0013(11) -0.0033(12) -0.0014(11) N8 0.0199(17) 0.0158(14) 0.0140(13) -0.0004(11) -0.0024(12) 0.0001(12) N10 0.0184(17) 0.0152(14) 0.0156(14) 0.0014(11) 0.0003(12) 0.0003(12) N13 0.0136(16) 0.0134(14) 0.0193(15) -0.0004(11) 0.0033(12) 0.0014(11) N16 0.0166(17) 0.0138(14) 0.0182(15) -0.0013(11) 0.0007(12) 0.0010(12) N20 0.0177(17) 0.0181(15) 0.0182(15) -0.0017(12) -0.0003(13) -0.0006(12) N22 0.0143(16) 0.0138(14) 0.0211(15) -0.0051(11) -0.0019(12) -0.0002(11) N25 0.0144(16) 0.0149(14) 0.0185(15) 0.0004(11) 0.0006(12) 0.0022(11) N28 0.0173(17) 0.0164(15) 0.0143(14) 0.0008(11) 0.0011(12) -0.0008(12) N32 0.0170(17) 0.0145(14) 0.0156(14) -0.0002(11) -0.0023(12) -0.0005(11) N34 0.0194(17) 0.0107(14) 0.0162(14) -0.0011(11) 0.0002(12) 0.0004(11) N37 0.0181(17) 0.0132(14) 0.0165(14) 0.0014(11) -0.0001(12) 0.0019(11) N39 0.0176(17) 0.0135(14) 0.0170(14) 0.0007(11) -0.0013(12) 0.0006(11) N44 0.0158(17) 0.0159(15) 0.0181(15) 0.0004(11) -0.0002(13) 0.0005(11) N46 0.0170(17) 0.0127(14) 0.0180(15) -0.0030(11) -0.0001(12) -0.0008(11) N50 0.0260(19) 0.0131(14) 0.0203(15) -0.0034(12) -0.0075(13) -0.0027(13) N54 0.0261(19) 0.0146(15) 0.0175(14) 0.0035(12) 0.0031(13) -0.0003(12) N58 0.035(2) 0.0133(15) 0.0225(16) -0.0013(12) -0.0074(14) 0.0007(13) C2 0.0121(18) 0.0122(16) 0.0190(17) 0.0002(13) -0.0012(14) 0.0008(13) C4 0.017(2) 0.0186(17) 0.0151(17) -0.0004(13) -0.0022(14) 0.0022(14) C5 0.015(2) 0.0184(17) 0.0175(17) 0.0008(14) 0.0018(14) 0.0021(14) C6 0.020(2) 0.0154(17) 0.0193(18) 0.0021(14) -0.0008(15) -0.0025(14) C7 0.033(2) 0.0094(16) 0.0195(18) 0.0021(13) -0.0018(16) 0.0004(14) C9 0.0115(18) 0.0132(16) 0.0181(17) 0.0025(13) -0.0018(14) 0.0002(13) C11 0.021(2) 0.0228(19) 0.0155(17) 0.0025(14) -0.0005(15) 0.0027(15) C12 0.020(2) 0.0207(18) 0.0138(17) 0.0014(14) 0.0006(15) 0.0002(14) C14 0.016(2) 0.0171(17) 0.0182(17) -0.0023(14) 0.0012(15) -0.0005(14) C15 0.019(2) 0.0188(18) 0.0182(18) 0.0019(14) -0.0007(15) -0.0029(14) C17 0.0099(18) 0.0131(16) 0.0201(17) -0.0004(13) -0.0003(14) 0.0006(13) C18 0.027(2) 0.0120(17) 0.0248(19) -0.0028(14) -0.0048(16) 0.0070(14) C19 0.024(2) 0.0131(17) 0.0264(19) -0.0053(14) -0.0016(16) 0.0007(14) C21 0.0139(19) 0.0142(17) 0.0194(17) -0.0036(13) -0.0020(14) 0.0008(13) C23 0.019(2) 0.0222(19) 0.0184(18) -0.0053(14) -0.0042(15) 0.0011(15) C24 0.019(2) 0.0233(19) 0.0187(18) -0.0013(15) -0.0017(16) 0.0013(15) C26 0.018(2) 0.0201(18) 0.0152(17) -0.0009(14) 0.0000(15) 0.0006(14) C27 0.018(2) 0.0183(17) 0.0139(17) 0.0026(13) 0.0029(14) 0.0026(14) C29 0.0109(18) 0.0118(16) 0.0197(17) -0.0003(13) -0.0002(14) 0.0019(12) C30 0.024(2) 0.0111(16) 0.0210(18) 0.0010(13) 0.0002(15) -0.0023(14) C31 0.024(2) 0.0135(17) 0.0178(17) 0.0044(13) -0.0007(15) 0.0010(14) C33 0.0117(18) 0.0129(16) 0.0158(16) -0.0019(13) -0.0009(14) -0.0008(13) C35 0.023(2) 0.0170(17) 0.0121(16) -0.0035(13) -0.0011(15) 0.0006(14) C36 0.021(2) 0.0182(18) 0.0147(17) 0.0008(13) 0.0012(15) -0.0014(14) C38 0.0118(18) 0.0130(16) 0.0169(16) 0.0033(13) -0.0003(14) 0.0026(13) C40 0.019(2) 0.0168(17) 0.0186(17) 0.0019(14) -0.0002(15) 0.0005(14) C41 0.021(2) 0.0160(17) 0.0155(17) 0.0004(13) 0.0006(15) 0.0000(14) C42 0.022(2) 0.0133(17) 0.0237(18) -0.0018(14) 0.0017(16) 0.0007(14) C43 0.017(2) 0.0135(17) 0.0233(18) -0.0012(14) -0.0001(15) 0.0032(13) C45 0.0125(19) 0.0113(16) 0.0196(17) -0.0007(13) 0.0009(14) 0.0000(13) C47 0.022(2) 0.0177(17) 0.0150(17) -0.0025(13) -0.0005(15) -0.0022(14) C48 0.017(2) 0.0224(19) 0.0157(17) -0.0021(14) 0.0001(15) 0.0008(14) _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 Ag2 2.8920(4) . ? Ag1 N1 2.162(3) . ? Ag1 N13 2.166(3) . ? Ag2 N8 2.109(3) . ? Ag2 N20 2.117(3) . ? Ag3 Ag4 2.9040(4) . ? Ag3 N25 2.122(3) . ? Ag3 N44 2.116(3) . ? Ag4 N32 2.134(3) . ? Ag4 N37 2.146(3) . ? O65 N62 1.254(4) . ? O63 N62 1.255(4) . ? O64 N62 1.243(4) . ? O51 N50 1.241(4) . ? O52 N50 1.253(4) . ? O53 N50 1.256(4) . ? O55 N54 1.261(4) . ? O56 N54 1.237(4) . ? O57 N54 1.259(4) . ? O59 N58 1.236(4) . ? O60 N58 1.233(4) . ? O61 N58 1.229(4) . ? N1 C2 1.333(4) . ? N1 C5 1.384(4) . ? N3 C2 1.358(4) . ? N3 C4 1.373(4) . ? N3 C6 1.469(4) . ? N8 C9 1.334(4) . ? N8 C12 1.375(4) . ? N10 C7 1.476(4) . ? N10 C9 1.354(4) . ? N10 C11 1.369(4) . ? N13 C14 1.382(4) . ? N13 C17 1.330(4) . ? N16 C15 1.366(4) . ? N16 C17 1.358(4) . ? N16 C18 1.467(4) . ? N20 C21 1.320(4) . ? N20 C24 1.380(4) . ? N22 C19 1.471(4) . ? N22 C21 1.357(4) . ? N22 C23 1.374(4) . ? N25 C26 1.380(4) . ? N25 C29 1.331(4) . ? N28 C27 1.373(4) . ? N28 C29 1.344(4) . ? N28 C30 1.478(4) . ? N32 C33 1.329(4) . ? N32 C36 1.380(4) . ? N34 C31 1.464(4) . ? N34 C33 1.351(4) . ? N34 C35 1.378(4) . ? N37 C38 1.326(4) . ? N37 C41 1.381(4) . ? N39 C38 1.352(4) . ? N39 C40 1.366(4) . ? N39 C42 1.474(4) . ? N44 C45 1.320(4) . ? N44 C48 1.381(4) . ? N46 C43 1.464(4) . ? N46 C45 1.360(4) . ? N46 C47 1.367(4) . ? C2 C9 1.443(5) . ? C4 H4 0.9300 . ? C4 C5 1.365(5) . ? C5 H5 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.516(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 H11 0.9300 . ? C11 C12 1.366(5) . ? C12 H12 0.9300 . ? C14 H14 0.9300 . ? C14 C15 1.353(5) . ? C15 H15 0.9300 . ? C17 C21 1.449(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.513(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C23 H23 0.9300 . ? C23 C24 1.364(5) . ? C24 H24 0.9300 . ? C26 H26 0.9300 . ? C26 C27 1.362(5) . ? C27 H27 0.9300 . ? C29 C33 1.453(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.517(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C35 H35 0.9300 . ? C35 C36 1.359(5) . ? C36 H36 0.9300 . ? C38 C45 1.455(5) . ? C40 H40 0.9300 . ? C40 C41 1.366(4) . ? C41 H41 0.9300 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 C43 1.518(5) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C47 H47 0.9300 . ? C47 C48 1.360(5) . ? C48 H48 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 N1 Ag1 Ag2 91.87(7) . . ? N1 Ag1 N13 164.95(11) . . ? N13 Ag1 Ag2 91.99(7) . . ? N8 Ag2 Ag1 95.06(8) . . ? N8 Ag2 N20 165.10(11) . . ? N20 Ag2 Ag1 95.49(8) . . ? N25 Ag3 Ag4 93.70(7) . . ? N44 Ag3 Ag4 96.05(7) . . ? N44 Ag3 N25 170.04(11) . . ? N32 Ag4 Ag3 94.55(7) . . ? N32 Ag4 N37 172.30(11) . . ? N37 Ag4 Ag3 92.31(7) . . ? O65 N62 O63 120.2(3) . . ? O64 N62 O65 119.9(3) . . ? O64 N62 O63 119.9(3) . . ? C2 N1 Ag1 134.4(2) . . ? C2 N1 C5 105.2(3) . . ? C5 N1 Ag1 119.8(2) . . ? C2 N3 C4 107.8(3) . . ? C2 N3 C6 123.7(3) . . ? C4 N3 C6 128.1(3) . . ? C9 N8 Ag2 131.8(2) . . ? C9 N8 C12 105.8(3) . . ? C12 N8 Ag2 121.1(2) . . ? C9 N10 C7 123.2(3) . . ? C9 N10 C11 108.1(3) . . ? C11 N10 C7 128.1(3) . . ? C14 N13 Ag1 119.9(2) . . ? C17 N13 Ag1 134.9(2) . . ? C17 N13 C14 105.2(3) . . ? C15 N16 C18 128.7(3) . . ? C17 N16 C15 107.3(3) . . ? C17 N16 C18 123.4(3) . . ? C21 N20 Ag2 133.8(2) . . ? C21 N20 C24 106.0(3) . . ? C24 N20 Ag2 120.1(2) . . ? C21 N22 C19 123.8(3) . . ? C21 N22 C23 107.4(3) . . ? C23 N22 C19 128.3(3) . . ? C26 N25 Ag3 118.2(2) . . ? C29 N25 Ag3 133.8(2) . . ? C29 N25 C26 105.2(3) . . ? C27 N28 C30 128.2(3) . . ? C29 N28 C27 107.9(3) . . ? C29 N28 C30 123.7(3) . . ? C33 N32 Ag4 133.5(2) . . ? C33 N32 C36 105.3(3) . . ? C36 N32 Ag4 121.1(2) . . ? C33 N34 C31 124.1(3) . . ? C33 N34 C35 107.5(3) . . ? C35 N34 C31 127.9(3) . . ? C38 N37 Ag4 135.2(2) . . ? C38 N37 C41 105.7(3) . . ? C41 N37 Ag4 118.7(2) . . ? C38 N39 C40 107.9(3) . . ? C38 N39 C42 124.1(3) . . ? C40 N39 C42 127.7(3) . . ? C45 N44 Ag3 132.8(2) . . ? C45 N44 C48 106.0(3) . . ? C48 N44 Ag3 120.4(2) . . ? C45 N46 C43 123.7(3) . . ? C45 N46 C47 107.3(3) . . ? C47 N46 C43 128.4(3) . . ? O51 N50 O52 120.7(3) . . ? O51 N50 O53 120.5(3) . . ? O52 N50 O53 118.9(3) . . ? O56 N54 O55 119.9(3) . . ? O56 N54 O57 120.0(3) . . ? O57 N54 O55 120.0(3) . . ? O60 N58 O59 118.3(4) . . ? O61 N58 O59 121.1(4) . . ? O61 N58 O60 120.7(4) . . ? N1 C2 N3 111.0(3) . . ? N1 C2 C9 131.1(3) . . ? N3 C2 C9 117.9(3) . . ? N3 C4 H4 127.1 . . ? C5 C4 N3 105.7(3) . . ? C5 C4 H4 127.1 . . ? N1 C5 H5 124.8 . . ? C4 C5 N1 110.3(3) . . ? C4 C5 H5 124.8 . . ? N3 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? N3 C6 C7 109.5(3) . . ? H6A C6 H6B 108.2 . . ? C7 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? N10 C7 C6 110.1(3) . . ? N10 C7 H7A 109.6 . . ? N10 C7 H7B 109.6 . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N8 C9 N10 110.4(3) . . ? N8 C9 C2 130.9(3) . . ? N10 C9 C2 118.7(3) . . ? N10 C11 H11 127.1 . . ? C12 C11 N10 105.8(3) . . ? C12 C11 H11 127.1 . . ? N8 C12 H12 125.1 . . ? C11 C12 N8 109.9(3) . . ? C11 C12 H12 125.1 . . ? N13 C14 H14 125.0 . . ? C15 C14 N13 110.0(3) . . ? C15 C14 H14 125.0 . . ? N16 C15 H15 126.7 . . ? C14 C15 N16 106.6(3) . . ? C14 C15 H15 126.7 . . ? N13 C17 N16 110.9(3) . . ? N13 C17 C21 130.9(3) . . ? N16 C17 C21 118.1(3) . . ? N16 C18 H18A 109.6 . . ? N16 C18 H18B 109.6 . . ? N16 C18 C19 110.2(3) . . ? H18A C18 H18B 108.1 . . ? C19 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? N22 C19 C18 109.3(3) . . ? N22 C19 H19A 109.8 . . ? N22 C19 H19B 109.8 . . ? C18 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? N20 C21 N22 111.0(3) . . ? N20 C21 C17 131.1(3) . . ? N22 C21 C17 117.9(3) . . ? N22 C23 H23 127.0 . . ? C24 C23 N22 106.1(3) . . ? C24 C23 H23 127.0 . . ? N20 C24 H24 125.2 . . ? C23 C24 N20 109.5(3) . . ? C23 C24 H24 125.2 . . ? N25 C26 H26 125.0 . . ? C27 C26 N25 110.0(3) . . ? C27 C26 H26 125.0 . . ? N28 C27 H27 127.1 . . ? C26 C27 N28 105.7(3) . . ? C26 C27 H27 127.1 . . ? N25 C29 N28 111.1(3) . . ? N25 C29 C33 130.8(3) . . ? N28 C29 C33 118.0(3) . . ? N28 C30 H30A 109.9 . . ? N28 C30 H30B 109.9 . . ? N28 C30 C31 109.1(3) . . ? H30A C30 H30B 108.3 . . ? C31 C30 H30A 109.9 . . ? C31 C30 H30B 109.9 . . ? N34 C31 C30 109.1(3) . . ? N34 C31 H31A 109.9 . . ? N34 C31 H31B 109.9 . . ? C30 C31 H31A 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N32 C33 N34 111.1(3) . . ? N32 C33 C29 131.3(3) . . ? N34 C33 C29 117.5(3) . . ? N34 C35 H35 127.1 . . ? C36 C35 N34 105.8(3) . . ? C36 C35 H35 127.1 . . ? N32 C36 H36 124.9 . . ? C35 C36 N32 110.2(3) . . ? C35 C36 H36 124.9 . . ? N37 C38 N39 110.8(3) . . ? N37 C38 C45 131.3(3) . . ? N39 C38 C45 117.9(3) . . ? N39 C40 H40 127.0 . . ? N39 C40 C41 106.0(3) . . ? C41 C40 H40 127.0 . . ? N37 C41 H41 125.2 . . ? C40 C41 N37 109.5(3) . . ? C40 C41 H41 125.2 . . ? N39 C42 H42A 109.9 . . ? N39 C42 H42B 109.9 . . ? N39 C42 C43 108.9(3) . . ? H42A C42 H42B 108.3 . . ? C43 C42 H42A 109.9 . . ? C43 C42 H42B 109.9 . . ? N46 C43 C42 110.0(3) . . ? N46 C43 H43A 109.7 . . ? N46 C43 H43B 109.7 . . ? C42 C43 H43A 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? N44 C45 N46 110.8(3) . . ? N44 C45 C38 131.6(3) . . ? N46 C45 C38 117.6(3) . . ? N46 C47 H47 126.8 . . ? C48 C47 N46 106.5(3) . . ? C48 C47 H47 126.8 . . ? N44 C48 H48 125.3 . . ? C47 C48 N44 109.4(3) . . ? C47 C48 H48 125.3 . . ? #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 832768' #TrackingRef '- CMFJLGcecrevised.cif' _audit_creation_date 2012-06-10 _audit_creation_method ; Olex2 1.2-beta (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H32 Ag3 N16, C2 H3 N, 3(Cl O4)' _chemical_formula_sum 'C34 H35 Ag3 Cl3 N17 O12' _chemical_formula_weight 1303.75 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 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' _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_H-M_alt 'P 1 c 1' _space_group_name_Hall 'P -2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x, -y, z+1/2' _cell_length_a 11.8432(4) _cell_length_b 12.4409(4) _cell_length_c 15.8426(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.1470(10) _cell_angle_gamma 90.00 _cell_volume 2205.12(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9947 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 32.05 _cell_measurement_theta_min 2.45 _exptl_absorpt_coefficient_mu 1.583 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_correction_T_min 0.6112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0620 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.8183. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 1292 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0257 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 49118 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.49 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 9700 _reflns_number_total 10072 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.693 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.228(12) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 633 _refine_ls_number_reflns 10072 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0204 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.9761P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0485 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.662662(16) 0.444669(15) 0.737155(13) 0.02162(4) Uani 1 1 d . . . Ag2 Ag 0.500439(16) 0.629106(15) 0.643251(12) 0.02150(5) Uani 1 1 d . . . Ag3 Ag 0.607429(18) 0.751175(17) 0.517674(14) 0.02392(5) Uani 1 1 d . . . C2 C 0.8310(2) 0.6321(2) 0.72166(17) 0.0209(5) Uani 1 1 d . . . C4 C 0.9782(3) 0.5550(3) 0.68808(19) 0.0300(6) Uani 1 1 d . . . H4 H 1.0485 0.5436 0.6753 0.036 Uiso 1 1 calc R . . C5 C 0.8957(3) 0.4806(3) 0.68867(19) 0.0285(6) Uani 1 1 d . . . H5 H 0.9001 0.4080 0.6762 0.034 Uiso 1 1 calc R . . C6 C 0.9888(3) 0.7602(3) 0.7173(3) 0.0408(8) Uani 1 1 d . . . H6A H 0.9582 0.7965 0.6601 0.049 Uiso 1 1 calc R . . H6B H 1.0751 0.7559 0.7336 0.049 Uiso 1 1 calc R . . C7 C 0.9558(3) 0.8229(3) 0.7873(3) 0.0439(9) Uani 1 1 d . . . H7A H 0.9972 0.7938 0.8461 0.053 Uiso 1 1 calc R . . H7B H 0.9789 0.8976 0.7864 0.053 Uiso 1 1 calc R . . C9 C 0.7658(3) 0.7216(2) 0.74004(16) 0.0223(6) Uani 1 1 d . . . C11 C 0.7452(3) 0.8876(2) 0.7785(2) 0.0330(7) Uani 1 1 d . . . H11 H 0.7604 0.9586 0.7972 0.040 Uiso 1 1 calc R . . C12 C 0.6383(3) 0.8360(2) 0.75654(18) 0.0297(6) Uani 1 1 d . . . H12 H 0.5673 0.8665 0.7580 0.036 Uiso 1 1 calc R . . C14 C 0.4334(2) 0.3822(2) 0.78453(17) 0.0203(5) Uani 1 1 d . . . C16 C 0.4521(3) 0.2096(2) 0.81604(19) 0.0279(6) Uani 1 1 d . . . H16 H 0.4382 0.1401 0.8320 0.034 Uiso 1 1 calc R . . C17 C 0.5467(3) 0.2441(2) 0.7922(2) 0.0271(6) Uani 1 1 d . . . H17 H 0.6097 0.2011 0.7896 0.032 Uiso 1 1 calc R . . C18 C 0.2642(3) 0.3066(2) 0.82408(19) 0.0278(6) Uani 1 1 d . . . H18A H 0.2531 0.2476 0.8606 0.033 Uiso 1 1 calc R . . H18B H 0.2013 0.3032 0.7666 0.033 Uiso 1 1 calc R . . C19 C 0.2581(3) 0.4126(2) 0.86927(19) 0.0272(6) Uani 1 1 d . . . H19A H 0.1771 0.4253 0.8690 0.033 Uiso 1 1 calc R . . H19B H 0.3105 0.4107 0.9309 0.033 Uiso 1 1 calc R . . C21 C 0.3787(2) 0.4871(2) 0.78032(16) 0.0196(5) Uani 1 1 d . . . C23 C 0.2634(2) 0.6056(2) 0.81388(18) 0.0243(6) Uani 1 1 d . . . H23 H 0.2094 0.6387 0.8369 0.029 Uiso 1 1 calc R . . C24 C 0.3266(2) 0.6530(2) 0.76635(17) 0.0228(5) Uani 1 1 d . . . H24 H 0.3217 0.7252 0.7504 0.027 Uiso 1 1 calc R . . C26 C 0.5691(2) 0.4547(2) 0.50885(17) 0.0218(5) Uani 1 1 d . . . C28 C 0.4460(3) 0.3214(2) 0.50317(18) 0.0275(6) Uani 1 1 d . . . H28 H 0.4069 0.2554 0.4914 0.033 Uiso 1 1 calc R . . C29 C 0.4181(3) 0.4062(2) 0.54649(18) 0.0260(6) Uani 1 1 d . . . H29 H 0.3557 0.4075 0.5700 0.031 Uiso 1 1 calc R . . C30 C 0.6066(3) 0.2945(2) 0.42846(18) 0.0292(6) Uani 1 1 d . . . H30A H 0.5705 0.3105 0.3654 0.035 Uiso 1 1 calc R . . H30B H 0.6018 0.2176 0.4366 0.035 Uiso 1 1 calc R . . C31 C 0.7366(3) 0.3301(2) 0.46049(19) 0.0283(6) Uani 1 1 d . . . H31A H 0.7767 0.3023 0.5200 0.034 Uiso 1 1 calc R . . H31B H 0.7770 0.3021 0.4209 0.034 Uiso 1 1 calc R . . C33 C 0.6654(3) 0.5089(2) 0.48911(17) 0.0228(5) Uani 1 1 d . . . C35 C 0.8227(3) 0.5157(3) 0.44465(18) 0.0293(6) Uani 1 1 d . . . H35 H 0.8859 0.4968 0.4251 0.035 Uiso 1 1 calc R . . C36 C 0.7918(3) 0.6166(3) 0.46220(19) 0.0286(6) Uani 1 1 d . . . H36 H 0.8314 0.6792 0.4562 0.034 Uiso 1 1 calc R . . C38 C 0.3372(3) 0.8413(2) 0.55675(17) 0.0226(6) Uani 1 1 d . . . C40 C 0.1531(3) 0.8007(3) 0.54552(18) 0.0292(6) Uani 1 1 d . . . H40 H 0.0727 0.8052 0.5403 0.035 Uiso 1 1 calc R . . C41 C 0.2178(3) 0.7089(3) 0.54825(19) 0.0279(6) Uani 1 1 d . . . H41 H 0.1877 0.6394 0.5449 0.034 Uiso 1 1 calc R . . C42 C 0.2093(3) 1.0004(2) 0.5516(2) 0.0323(7) Uani 1 1 d . . . H42A H 0.1438 1.0152 0.5740 0.039 Uiso 1 1 calc R . . H42B H 0.1879 1.0278 0.4911 0.039 Uiso 1 1 calc R . . C43 C 0.3228(3) 1.0555(2) 0.6107(2) 0.0342(7) Uani 1 1 d . . . H43A H 0.3156 1.1326 0.6017 0.041 Uiso 1 1 calc R . . H43B H 0.3340 1.0407 0.6730 0.041 Uiso 1 1 calc R . . C45 C 0.4353(3) 0.9125(2) 0.56386(17) 0.0242(6) Uani 1 1 d . . . C47 C 0.5299(3) 1.0673(3) 0.5925(2) 0.0334(7) Uani 1 1 d . . . H47 H 0.5501 1.1384 0.6088 0.040 Uiso 1 1 calc R . . C48 C 0.5975(3) 0.9933(2) 0.5681(2) 0.0314(6) Uani 1 1 d . . . H48 H 0.6730 1.0060 0.5642 0.038 Uiso 1 1 calc R . . C51 C 0.8479(4) 0.1913(3) 0.7024(3) 0.0461(9) Uani 1 1 d . . . C52 C 0.9567(4) 0.1304(4) 0.7131(3) 0.0605(11) Uani 1 1 d . . . H52A H 1.0045 0.1674 0.6838 0.091 Uiso 1 1 calc R . . H52B H 0.9362 0.0604 0.6871 0.091 Uiso 1 1 calc R . . H52C H 1.0010 0.1231 0.7756 0.091 Uiso 1 1 calc R . . Cl60 Cl 0.27291(6) 0.05896(5) 0.32637(4) 0.02310(13) Uani 1 1 d . . . Cl65 Cl 0.10371(6) 0.35476(6) 0.54492(5) 0.03193(16) Uani 1 1 d . . . Cl70 Cl 0.84152(10) 0.95514(10) 0.47081(7) 0.0616(3) Uani 1 1 d . . . N1 N 0.8034(2) 0.52824(19) 0.71058(15) 0.0229(5) Uani 1 1 d . . . N3 N 0.9378(2) 0.6510(2) 0.71024(15) 0.0266(5) Uani 1 1 d . . . N8 N 0.6508(2) 0.73131(18) 0.73168(16) 0.0228(5) Uani 1 1 d . . . N10 N 0.8259(2) 0.8150(2) 0.76768(16) 0.0282(5) Uani 1 1 d . . . N13 N 0.5347(2) 0.35295(18) 0.77232(15) 0.0213(5) Uani 1 1 d . . . N15 N 0.3821(2) 0.29781(19) 0.81178(15) 0.0233(5) Uani 1 1 d . . . N20 N 0.3991(2) 0.57827(18) 0.74517(15) 0.0211(4) Uani 1 1 d . . . N22 N 0.2950(2) 0.49930(19) 0.82102(14) 0.0217(5) Uani 1 1 d . . . N25 N 0.4955(2) 0.48972(19) 0.55043(15) 0.0222(5) Uani 1 1 d . . . N27 N 0.5426(2) 0.35197(19) 0.48030(15) 0.0237(5) Uani 1 1 d . . . N32 N 0.6934(2) 0.6124(2) 0.49023(15) 0.0240(5) Uani 1 1 d . . . N34 N 0.7415(2) 0.4476(2) 0.46158(14) 0.0243(5) Uani 1 1 d . . . N37 N 0.3344(2) 0.73467(19) 0.55665(15) 0.0244(5) Uani 1 1 d . . . N39 N 0.2300(2) 0.8843(2) 0.55192(15) 0.0257(5) Uani 1 1 d . . . N44 N 0.5378(2) 0.89641(19) 0.55009(15) 0.0248(5) Uani 1 1 d . . . N46 N 0.4259(2) 1.0162(2) 0.58841(15) 0.0279(5) Uani 1 1 d . . . N50 N 0.7632(4) 0.2387(3) 0.6925(3) 0.0609(10) Uani 1 1 d . . . O61 O 0.2502(2) 0.14220(16) 0.38204(15) 0.0329(5) Uani 1 1 d . . . O62 O 0.2618(3) -0.04397(18) 0.36285(17) 0.0435(6) Uani 1 1 d . . . O63 O 0.1864(2) 0.0667(2) 0.23884(16) 0.0549(8) Uani 1 1 d . . . O64 O 0.3905(2) 0.0696(2) 0.3210(2) 0.0553(7) Uani 1 1 d . . . O66 O 0.1914(3) 0.2725(3) 0.5663(3) 0.0929(14) Uani 1 1 d . . . O67 O 0.0066(3) 0.3281(2) 0.5749(2) 0.0649(9) Uani 1 1 d . . . O68 O 0.0626(4) 0.3730(4) 0.4526(2) 0.1073(18) Uani 1 1 d . . . O69 O 0.1562(3) 0.4510(3) 0.5887(3) 0.0739(11) Uani 1 1 d . . . O71 O 0.7222(4) 0.9262(4) 0.4149(3) 0.1085(17) Uani 1 1 d . A . O72 O 0.8312(4) 1.0652(3) 0.4915(2) 0.0829(12) Uani 1 1 d . A . O73 O 0.9218(3) 0.9439(4) 0.4210(2) 0.1004(16) Uani 1 1 d . A . O74A O 0.9256(14) 0.9372(14) 0.5675(6) 0.070(5) Uani 0.38(2) 1 d PU A 2 O75B O 0.8503(13) 0.8717(10) 0.5364(7) 0.106(5) Uani 0.62(2) 1 d P A 1 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 0.01889(9) 0.01778(9) 0.02851(9) -0.00045(8) 0.00819(7) -0.00253(8) Ag2 0.02025(9) 0.01955(10) 0.02619(9) -0.00073(8) 0.00964(7) 0.00119(8) Ag3 0.02342(10) 0.02196(10) 0.02772(9) 0.00092(8) 0.01022(7) 0.00338(8) C2 0.0183(12) 0.0261(14) 0.0178(11) 0.0015(10) 0.0052(9) -0.0041(11) C4 0.0207(14) 0.0417(18) 0.0278(14) 0.0034(12) 0.0084(11) 0.0042(13) C5 0.0226(14) 0.0333(16) 0.0301(14) -0.0042(12) 0.0091(11) 0.0008(12) C6 0.0233(15) 0.0336(18) 0.065(2) 0.0192(16) 0.0136(15) -0.0062(13) C7 0.0334(18) 0.0267(17) 0.059(2) 0.0052(15) -0.0018(15) -0.0139(14) C9 0.0288(15) 0.0195(13) 0.0179(12) 0.0010(10) 0.0068(10) -0.0062(11) C11 0.050(2) 0.0164(14) 0.0291(14) -0.0035(11) 0.0081(13) -0.0033(13) C12 0.0429(18) 0.0243(15) 0.0247(14) -0.0015(11) 0.0149(12) -0.0013(13) C14 0.0231(13) 0.0162(13) 0.0209(12) -0.0016(9) 0.0063(10) -0.0050(10) C16 0.0366(16) 0.0170(14) 0.0315(14) -0.0022(11) 0.0129(12) -0.0082(12) C17 0.0310(16) 0.0194(14) 0.0310(15) -0.0013(11) 0.0105(12) 0.0017(12) C18 0.0253(14) 0.0296(16) 0.0303(14) 0.0007(12) 0.0116(11) -0.0110(12) C19 0.0268(14) 0.0287(15) 0.0314(14) 0.0032(12) 0.0165(12) -0.0085(12) C21 0.0176(12) 0.0205(13) 0.0208(11) 0.0002(10) 0.0066(10) -0.0027(10) C23 0.0211(13) 0.0271(15) 0.0262(13) -0.0028(11) 0.0099(10) 0.0006(11) C24 0.0229(14) 0.0204(13) 0.0252(12) 0.0005(10) 0.0081(10) 0.0017(11) C26 0.0226(13) 0.0229(14) 0.0189(11) -0.0010(10) 0.0052(10) 0.0031(10) C28 0.0306(15) 0.0245(15) 0.0251(13) -0.0011(11) 0.0062(11) -0.0022(12) C29 0.0225(14) 0.0304(15) 0.0249(13) 0.0000(11) 0.0077(11) -0.0013(12) C30 0.0346(16) 0.0269(15) 0.0241(13) -0.0058(11) 0.0068(11) 0.0113(13) C31 0.0295(15) 0.0326(16) 0.0232(13) -0.0034(11) 0.0094(11) 0.0113(13) C33 0.0231(13) 0.0271(14) 0.0181(11) 0.0011(10) 0.0067(10) 0.0075(11) C35 0.0228(14) 0.0423(18) 0.0258(13) 0.0042(12) 0.0120(11) 0.0078(13) C36 0.0243(14) 0.0364(17) 0.0276(14) 0.0086(12) 0.0119(11) 0.0061(13) C38 0.0266(14) 0.0225(14) 0.0188(12) 0.0029(10) 0.0074(10) 0.0079(11) C40 0.0244(14) 0.0384(17) 0.0271(13) 0.0003(12) 0.0116(11) 0.0071(13) C41 0.0254(14) 0.0295(15) 0.0287(13) -0.0019(12) 0.0086(11) 0.0036(12) C42 0.0416(18) 0.0281(16) 0.0346(15) 0.0104(12) 0.0225(13) 0.0177(14) C43 0.051(2) 0.0216(15) 0.0399(16) 0.0017(12) 0.0276(15) 0.0085(14) C45 0.0369(16) 0.0191(13) 0.0178(11) 0.0033(10) 0.0105(11) 0.0042(12) C47 0.0465(19) 0.0221(15) 0.0355(16) 0.0042(12) 0.0188(14) 0.0003(14) C48 0.0396(17) 0.0247(15) 0.0308(14) 0.0020(12) 0.0129(13) 0.0003(13) C51 0.052(2) 0.0346(19) 0.055(2) -0.0004(16) 0.0216(18) -0.0121(18) C52 0.055(3) 0.054(3) 0.069(3) 0.020(2) 0.015(2) 0.003(2) Cl60 0.0257(3) 0.0188(3) 0.0269(3) 0.0012(2) 0.0115(3) 0.0052(2) Cl65 0.0212(3) 0.0234(3) 0.0506(4) -0.0039(3) 0.0109(3) 0.0042(3) Cl70 0.0674(7) 0.0758(8) 0.0547(5) 0.0376(5) 0.0379(5) 0.0403(6) N1 0.0205(11) 0.0231(12) 0.0254(11) -0.0040(9) 0.0079(9) -0.0042(9) N3 0.0190(11) 0.0329(14) 0.0260(11) 0.0064(10) 0.0049(9) -0.0054(10) N8 0.0274(13) 0.0193(11) 0.0246(11) -0.0041(9) 0.0124(9) -0.0023(10) N10 0.0305(13) 0.0214(13) 0.0276(12) 0.0017(10) 0.0026(10) -0.0114(11) N13 0.0234(12) 0.0158(11) 0.0258(11) -0.0005(9) 0.0096(9) -0.0015(9) N15 0.0275(12) 0.0193(11) 0.0244(11) 0.0005(9) 0.0101(9) -0.0068(10) N20 0.0210(11) 0.0190(11) 0.0249(11) -0.0017(9) 0.0097(9) -0.0024(9) N22 0.0213(11) 0.0220(12) 0.0233(11) -0.0002(9) 0.0095(9) -0.0034(9) N25 0.0196(11) 0.0232(12) 0.0243(11) -0.0016(9) 0.0076(9) 0.0024(9) N27 0.0265(12) 0.0208(12) 0.0228(11) -0.0040(9) 0.0069(9) 0.0030(10) N32 0.0226(12) 0.0264(13) 0.0244(11) 0.0040(9) 0.0093(9) 0.0034(10) N34 0.0254(12) 0.0286(13) 0.0199(10) 0.0012(9) 0.0087(9) 0.0099(10) N37 0.0258(12) 0.0200(12) 0.0266(11) -0.0020(9) 0.0073(10) 0.0047(10) N39 0.0305(13) 0.0269(13) 0.0231(11) 0.0054(9) 0.0135(10) 0.0127(10) N44 0.0275(12) 0.0227(12) 0.0239(11) 0.0019(9) 0.0081(9) 0.0011(10) N46 0.0421(15) 0.0169(12) 0.0282(12) 0.0034(9) 0.0164(11) 0.0066(11) N50 0.054(2) 0.048(2) 0.091(3) -0.0036(19) 0.038(2) -0.0063(18) O61 0.0426(13) 0.0200(10) 0.0401(11) -0.0081(9) 0.0189(10) 0.0000(9) O62 0.0715(18) 0.0180(11) 0.0518(14) 0.0054(10) 0.0350(13) 0.0069(11) O63 0.0572(18) 0.0755(19) 0.0284(11) -0.0022(12) 0.0091(11) 0.0370(15) O64 0.0376(14) 0.0468(16) 0.094(2) -0.0078(14) 0.0393(14) -0.0013(12) O66 0.0458(18) 0.0383(17) 0.199(5) 0.019(2) 0.046(2) 0.0262(14) O67 0.0447(16) 0.0411(16) 0.124(3) 0.0030(16) 0.0482(18) -0.0043(13) O68 0.097(3) 0.177(5) 0.0492(18) 0.000(2) 0.0258(19) 0.065(3) O69 0.0559(18) 0.059(2) 0.123(3) -0.0491(19) 0.052(2) -0.0263(15) O71 0.103(3) 0.129(4) 0.113(3) -0.051(3) 0.062(3) -0.079(3) O72 0.110(3) 0.078(3) 0.068(2) -0.0293(18) 0.039(2) -0.048(2) O73 0.067(2) 0.188(5) 0.0586(19) 0.051(2) 0.0363(17) 0.071(3) O74A 0.085(8) 0.086(8) 0.048(5) 0.043(4) 0.035(4) 0.057(6) O75B 0.138(10) 0.111(8) 0.093(6) 0.075(6) 0.070(7) 0.052(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 Ag2 3.0487(3) . ? Ag1 N1 2.120(2) . ? Ag1 N13 2.112(2) . ? Ag2 Ag3 3.0860(3) . ? Ag2 N8 2.261(2) . ? Ag2 N20 2.392(2) . ? Ag2 N25 2.262(2) . ? Ag2 N37 2.388(2) . ? Ag3 N32 2.120(2) . ? Ag3 N44 2.118(2) . ? C2 C9 1.439(4) . ? C2 N1 1.330(4) . ? C2 N3 1.356(3) . ? C4 H4 0.9300 . ? C4 C5 1.349(4) . ? C4 N3 1.374(4) . ? C5 H5 0.9300 . ? C5 N1 1.384(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.508(6) . ? C6 N3 1.476(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 N10 1.469(4) . ? C9 N8 1.330(4) . ? C9 N10 1.358(4) . ? C11 H11 0.9300 . ? C11 C12 1.359(5) . ? C11 N10 1.367(4) . ? C12 H12 0.9300 . ? C12 N8 1.382(4) . ? C14 C21 1.449(4) . ? C14 N13 1.328(4) . ? C14 N15 1.352(3) . ? C16 H16 0.9300 . ? C16 C17 1.363(4) . ? C16 N15 1.364(4) . ? C17 H17 0.9300 . ? C17 N13 1.387(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.514(4) . ? C18 N15 1.476(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 N22 1.469(3) . ? C21 N20 1.320(3) . ? C21 N22 1.357(3) . ? C23 H23 0.9300 . ? C23 C24 1.358(4) . ? C23 N22 1.369(4) . ? C24 H24 0.9300 . ? C24 N20 1.380(3) . ? C26 C33 1.446(4) . ? C26 N25 1.327(3) . ? C26 N27 1.357(4) . ? C28 H28 0.9300 . ? C28 C29 1.357(4) . ? C28 N27 1.363(4) . ? C29 H29 0.9300 . ? C29 N25 1.374(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 C31 1.520(4) . ? C30 N27 1.473(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 N34 1.464(4) . ? C33 N32 1.328(4) . ? C33 N34 1.357(4) . ? C35 H35 0.9300 . ? C35 C36 1.361(5) . ? C35 N34 1.372(4) . ? C36 H36 0.9300 . ? C36 N32 1.378(4) . ? C38 C45 1.436(4) . ? C38 N37 1.327(4) . ? C38 N39 1.357(4) . ? C40 H40 0.9300 . ? C40 C41 1.368(4) . ? C40 N39 1.364(4) . ? C41 H41 0.9300 . ? C41 N37 1.381(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 C43 1.526(5) . ? C42 N39 1.464(4) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 N46 1.462(4) . ? C45 N44 1.317(4) . ? C45 N46 1.362(4) . ? C47 H47 0.9300 . ? C47 C48 1.358(4) . ? C47 N46 1.368(4) . ? C48 H48 0.9300 . ? C48 N44 1.379(4) . ? C51 C52 1.455(6) . ? C51 N50 1.130(5) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? Cl60 O61 1.442(2) . ? Cl60 O62 1.429(2) . ? Cl60 O63 1.432(3) . ? Cl60 O64 1.430(3) . ? Cl65 O66 1.418(3) . ? Cl65 O67 1.420(3) . ? Cl65 O68 1.401(4) . ? Cl65 O69 1.421(3) . ? Cl70 O71 1.446(4) . ? Cl70 O72 1.422(4) . ? Cl70 O73 1.428(3) . ? Cl70 O74A 1.546(10) . ? Cl70 O75B 1.448(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 N1 Ag1 Ag2 86.82(6) . . ? N13 Ag1 Ag2 98.26(6) . . ? N13 Ag1 N1 174.71(9) . . ? Ag1 Ag2 Ag3 111.019(8) . . ? N8 Ag2 Ag1 83.03(6) . . ? N8 Ag2 Ag3 73.52(6) . . ? N8 Ag2 N20 101.43(8) . . ? N8 Ag2 N25 132.93(8) . . ? N8 Ag2 N37 112.30(8) . . ? N20 Ag2 Ag1 81.20(6) . . ? N20 Ag2 Ag3 165.59(6) . . ? N25 Ag2 Ag1 67.55(6) . . ? N25 Ag2 Ag3 83.50(6) . . ? N25 Ag2 N20 108.93(8) . . ? N25 Ag2 N37 101.95(8) . . ? N37 Ag2 Ag1 164.26(6) . . ? N37 Ag2 Ag3 78.10(6) . . ? N37 Ag2 N20 91.84(8) . . ? N32 Ag3 Ag2 93.31(6) . . ? N44 Ag3 Ag2 89.34(6) . . ? N44 Ag3 N32 174.61(10) . . ? N1 C2 C9 130.8(2) . . ? N1 C2 N3 110.5(2) . . ? N3 C2 C9 118.6(3) . . ? C5 C4 H4 126.9 . . ? C5 C4 N3 106.3(3) . . ? N3 C4 H4 126.9 . . ? C4 C5 H5 125.0 . . ? C4 C5 N1 110.0(3) . . ? N1 C5 H5 125.0 . . ? H6A C6 H6B 108.2 . . ? C7 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? N3 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? N3 C6 C7 109.5(3) . . ? C6 C7 H7A 110.0 . . ? C6 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? N10 C7 C6 108.4(3) . . ? N10 C7 H7A 110.0 . . ? N10 C7 H7B 110.0 . . ? N8 C9 C2 130.6(3) . . ? N8 C9 N10 111.5(3) . . ? N10 C9 C2 117.9(3) . . ? C12 C11 H11 126.7 . . ? C12 C11 N10 106.7(3) . . ? N10 C11 H11 126.7 . . ? C11 C12 H12 125.1 . . ? C11 C12 N8 109.9(3) . . ? N8 C12 H12 125.1 . . ? N13 C14 C21 130.6(2) . . ? N13 C14 N15 110.9(2) . . ? N15 C14 C21 118.3(2) . . ? C17 C16 H16 127.0 . . ? C17 C16 N15 106.0(3) . . ? N15 C16 H16 127.0 . . ? C16 C17 H17 125.1 . . ? C16 C17 N13 109.8(3) . . ? N13 C17 H17 125.1 . . ? H18A C18 H18B 108.3 . . ? C19 C18 H18A 109.9 . . ? C19 C18 H18B 109.9 . . ? N15 C18 H18A 109.9 . . ? N15 C18 H18B 109.9 . . ? N15 C18 C19 108.7(2) . . ? C18 C19 H19A 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N22 C19 C18 109.0(2) . . ? N22 C19 H19A 109.9 . . ? N22 C19 H19B 109.9 . . ? N20 C21 C14 130.8(2) . . ? N20 C21 N22 111.5(2) . . ? N22 C21 C14 117.7(2) . . ? C24 C23 H23 126.9 . . ? C24 C23 N22 106.2(2) . . ? N22 C23 H23 126.9 . . ? C23 C24 H24 125.0 . . ? C23 C24 N20 110.0(2) . . ? N20 C24 H24 125.0 . . ? N25 C26 C33 130.4(3) . . ? N25 C26 N27 110.9(3) . . ? N27 C26 C33 118.7(2) . . ? C29 C28 H28 126.8 . . ? C29 C28 N27 106.4(3) . . ? N27 C28 H28 126.8 . . ? C28 C29 H29 125.0 . . ? C28 C29 N25 110.0(3) . . ? N25 C29 H29 125.0 . . ? H30A C30 H30B 108.3 . . ? C31 C30 H30A 109.9 . . ? C31 C30 H30B 109.9 . . ? N27 C30 H30A 109.9 . . ? N27 C30 H30B 109.9 . . ? N27 C30 C31 108.8(2) . . ? C30 C31 H31A 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? N34 C31 C30 109.1(2) . . ? N34 C31 H31A 109.9 . . ? N34 C31 H31B 109.9 . . ? N32 C33 C26 131.3(3) . . ? N32 C33 N34 111.1(3) . . ? N34 C33 C26 117.5(3) . . ? C36 C35 H35 126.9 . . ? C36 C35 N34 106.1(3) . . ? N34 C35 H35 126.9 . . ? C35 C36 H36 125.0 . . ? C35 C36 N32 110.0(3) . . ? N32 C36 H36 125.0 . . ? N37 C38 C45 129.5(3) . . ? N37 C38 N39 111.8(3) . . ? N39 C38 C45 118.6(3) . . ? C41 C40 H40 126.9 . . ? N39 C40 H40 126.9 . . ? N39 C40 C41 106.3(3) . . ? C40 C41 H41 125.0 . . ? C40 C41 N37 110.0(3) . . ? N37 C41 H41 125.0 . . ? H42A C42 H42B 108.3 . . ? C43 C42 H42A 109.8 . . ? C43 C42 H42B 109.8 . . ? N39 C42 H42A 109.8 . . ? N39 C42 H42B 109.8 . . ? N39 C42 C43 109.2(2) . . ? C42 C43 H43A 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? N46 C43 C42 109.9(2) . . ? N46 C43 H43A 109.7 . . ? N46 C43 H43B 109.7 . . ? N44 C45 C38 131.2(3) . . ? N44 C45 N46 110.9(3) . . ? N46 C45 C38 117.8(3) . . ? C48 C47 H47 127.0 . . ? C48 C47 N46 106.1(3) . . ? N46 C47 H47 127.0 . . ? C47 C48 H48 125.0 . . ? C47 C48 N44 109.9(3) . . ? N44 C48 H48 125.0 . . ? N50 C51 C52 178.7(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O62 Cl60 O61 109.61(13) . . ? O62 Cl60 O63 108.66(18) . . ? O62 Cl60 O64 109.17(17) . . ? O63 Cl60 O61 109.06(14) . . ? O64 Cl60 O61 110.56(15) . . ? O64 Cl60 O63 109.75(18) . . ? O66 Cl65 O67 111.2(2) . . ? O66 Cl65 O69 108.8(2) . . ? O67 Cl65 O69 107.89(19) . . ? O68 Cl65 O66 110.0(3) . . ? O68 Cl65 O67 110.2(2) . . ? O68 Cl65 O69 108.6(3) . . ? O71 Cl70 O74A 138.9(8) . . ? O71 Cl70 O75B 95.0(7) . . ? O72 Cl70 O71 103.9(3) . . ? O72 Cl70 O73 110.2(3) . . ? O72 Cl70 O74A 89.2(6) . . ? O72 Cl70 O75B 121.1(5) . . ? O73 Cl70 O71 109.3(3) . . ? O73 Cl70 O74A 101.8(5) . . ? O73 Cl70 O75B 115.0(3) . . ? O75B Cl70 O74A 46.7(5) . . ? C2 N1 Ag1 128.71(19) . . ? C2 N1 C5 105.6(2) . . ? C5 N1 Ag1 125.2(2) . . ? C2 N3 C4 107.6(2) . . ? C2 N3 C6 121.7(3) . . ? C4 N3 C6 130.6(3) . . ? C9 N8 Ag2 125.68(18) . . ? C9 N8 C12 105.0(2) . . ? C12 N8 Ag2 124.8(2) . . ? C9 N10 C7 121.9(3) . . ? C9 N10 C11 106.9(3) . . ? C11 N10 C7 131.0(3) . . ? C14 N13 Ag1 130.67(19) . . ? C14 N13 C17 105.3(2) . . ? C17 N13 Ag1 124.0(2) . . ? C14 N15 C16 108.1(2) . . ? C14 N15 C18 121.9(2) . . ? C16 N15 C18 129.8(2) . . ? C21 N20 Ag2 135.51(18) . . ? C21 N20 C24 105.2(2) . . ? C24 N20 Ag2 118.44(17) . . ? C21 N22 C19 123.6(2) . . ? C21 N22 C23 107.0(2) . . ? C23 N22 C19 129.2(2) . . ? C26 N25 Ag2 133.91(19) . . ? C26 N25 C29 105.4(2) . . ? C29 N25 Ag2 118.97(18) . . ? C26 N27 C28 107.3(2) . . ? C26 N27 C30 122.5(3) . . ? C28 N27 C30 130.0(3) . . ? C33 N32 Ag3 131.15(19) . . ? C33 N32 C36 105.4(2) . . ? C36 N32 Ag3 123.3(2) . . ? C33 N34 C31 122.5(3) . . ? C33 N34 C35 107.3(3) . . ? C35 N34 C31 130.0(2) . . ? C38 N37 Ag2 122.24(19) . . ? C38 N37 C41 104.8(2) . . ? C41 N37 Ag2 122.47(19) . . ? C38 N39 C40 107.0(2) . . ? C38 N39 C42 122.8(3) . . ? C40 N39 C42 130.1(3) . . ? C45 N44 Ag3 128.6(2) . . ? C45 N44 C48 105.7(2) . . ? C48 N44 Ag3 125.5(2) . . ? C45 N46 C43 122.6(3) . . ? C45 N46 C47 107.3(3) . . ? C47 N46 C43 130.0(3) . . ? 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 Ag1 Ag2 Ag3 N32 30.68(6) . . . . ? Ag1 Ag2 Ag3 N44 -144.62(6) . . . . ? Ag1 Ag2 N8 C9 51.0(2) . . . . ? Ag1 Ag2 N8 C12 -156.6(2) . . . . ? Ag1 Ag2 N20 C21 -34.5(2) . . . . ? Ag1 Ag2 N20 C24 157.74(19) . . . . ? Ag1 Ag2 N25 C26 -76.8(2) . . . . ? Ag1 Ag2 N25 C29 85.9(2) . . . . ? Ag1 Ag2 N37 C38 171.47(15) . . . . ? Ag1 Ag2 N37 C41 32.0(4) . . . . ? Ag2 Ag1 N1 C2 45.7(2) . . . . ? Ag2 Ag1 N1 C5 -143.4(2) . . . . ? Ag2 Ag1 N13 C14 -24.4(2) . . . . ? Ag2 Ag1 N13 C17 159.0(2) . . . . ? Ag2 Ag3 N32 C33 28.7(2) . . . . ? Ag2 Ag3 N32 C36 -156.4(2) . . . . ? Ag2 Ag3 N44 C45 -37.5(2) . . . . ? Ag2 Ag3 N44 C48 136.9(2) . . . . ? Ag3 Ag2 N8 C9 -63.4(2) . . . . ? Ag3 Ag2 N8 C12 89.0(2) . . . . ? Ag3 Ag2 N20 C21 176.59(16) . . . . ? Ag3 Ag2 N20 C24 8.9(4) . . . . ? Ag3 Ag2 N25 C26 39.1(2) . . . . ? Ag3 Ag2 N25 C29 -158.2(2) . . . . ? Ag3 Ag2 N37 C38 -61.4(2) . . . . ? Ag3 Ag2 N37 C41 159.2(2) . . . . ? C2 C9 N8 Ag2 -21.5(4) . . . . ? C2 C9 N8 C12 -178.3(3) . . . . ? C2 C9 N10 C7 -6.1(4) . . . . ? C2 C9 N10 C11 178.5(2) . . . . ? C4 C5 N1 Ag1 -171.64(19) . . . . ? C4 C5 N1 C2 0.9(3) . . . . ? C5 C4 N3 C2 -1.3(3) . . . . ? C5 C4 N3 C6 -177.9(3) . . . . ? C6 C7 N10 C9 40.7(4) . . . . ? C6 C7 N10 C11 -145.1(3) . . . . ? C7 C6 N3 C2 34.3(4) . . . . ? C7 C6 N3 C4 -149.4(3) . . . . ? C9 C2 N1 Ag1 -11.6(4) . . . . ? C9 C2 N1 C5 176.1(3) . . . . ? C9 C2 N3 C4 -176.2(2) . . . . ? C9 C2 N3 C6 0.8(4) . . . . ? C11 C12 N8 Ag2 -156.5(2) . . . . ? C11 C12 N8 C9 0.6(3) . . . . ? C12 C11 N10 C7 -175.1(3) . . . . ? C12 C11 N10 C9 -0.3(3) . . . . ? C14 C21 N20 Ag2 15.2(4) . . . . ? C14 C21 N20 C24 -176.0(3) . . . . ? C14 C21 N22 C19 0.5(4) . . . . ? C14 C21 N22 C23 175.6(2) . . . . ? C16 C17 N13 Ag1 177.31(19) . . . . ? C16 C17 N13 C14 0.0(3) . . . . ? C17 C16 N15 C14 1.0(3) . . . . ? C17 C16 N15 C18 175.0(3) . . . . ? C18 C19 N22 C21 -33.3(3) . . . . ? C18 C19 N22 C23 152.7(3) . . . . ? C19 C18 N15 C14 -41.9(3) . . . . ? C19 C18 N15 C16 144.8(3) . . . . ? C21 C14 N13 Ag1 -2.1(4) . . . . ? C21 C14 N13 C17 175.0(3) . . . . ? C21 C14 N15 C16 -176.2(2) . . . . ? C21 C14 N15 C18 9.2(4) . . . . ? C23 C24 N20 Ag2 170.99(17) . . . . ? C23 C24 N20 C21 -0.1(3) . . . . ? C24 C23 N22 C19 176.7(3) . . . . ? C24 C23 N22 C21 2.0(3) . . . . ? C26 C33 N32 Ag3 -2.2(4) . . . . ? C26 C33 N32 C36 -177.8(3) . . . . ? C26 C33 N34 C31 -6.5(4) . . . . ? C26 C33 N34 C35 178.4(2) . . . . ? C28 C29 N25 Ag2 -166.79(18) . . . . ? C28 C29 N25 C26 0.4(3) . . . . ? C29 C28 N27 C26 -1.1(3) . . . . ? C29 C28 N27 C30 -176.5(3) . . . . ? C30 C31 N34 C33 39.9(3) . . . . ? C30 C31 N34 C35 -146.2(3) . . . . ? C31 C30 N27 C26 34.6(3) . . . . ? C31 C30 N27 C28 -150.6(3) . . . . ? C33 C26 N25 Ag2 -18.5(5) . . . . ? C33 C26 N25 C29 177.1(3) . . . . ? C33 C26 N27 C28 -177.1(2) . . . . ? C33 C26 N27 C30 -1.3(4) . . . . ? C35 C36 N32 Ag3 -176.24(18) . . . . ? C35 C36 N32 C33 -0.2(3) . . . . ? C36 C35 N34 C31 -174.9(3) . . . . ? C36 C35 N34 C33 -0.4(3) . . . . ? C38 C45 N44 Ag3 -4.0(4) . . . . ? C38 C45 N44 C48 -179.3(3) . . . . ? C38 C45 N46 C43 2.4(4) . . . . ? C38 C45 N46 C47 178.7(2) . . . . ? C40 C41 N37 Ag2 143.93(19) . . . . ? C40 C41 N37 C38 -1.4(3) . . . . ? C41 C40 N39 C38 1.0(3) . . . . ? C41 C40 N39 C42 179.3(3) . . . . ? C42 C43 N46 C45 -35.5(4) . . . . ? C42 C43 N46 C47 149.1(3) . . . . ? C43 C42 N39 C38 -34.4(3) . . . . ? C43 C42 N39 C40 147.5(3) . . . . ? C45 C38 N37 Ag2 34.5(4) . . . . ? C45 C38 N37 C41 179.9(3) . . . . ? C45 C38 N39 C40 179.9(2) . . . . ? C45 C38 N39 C42 1.4(4) . . . . ? C47 C48 N44 Ag3 -175.6(2) . . . . ? C47 C48 N44 C45 -0.2(3) . . . . ? C48 C47 N46 C43 177.4(3) . . . . ? C48 C47 N46 C45 1.5(3) . . . . ? N1 Ag1 Ag2 Ag3 21.85(6) . . . . ? N1 Ag1 Ag2 N8 -47.47(8) . . . . ? N1 Ag1 Ag2 N20 -150.23(8) . . . . ? N1 Ag1 Ag2 N25 94.99(9) . . . . ? N1 Ag1 Ag2 N37 145.2(2) . . . . ? N1 Ag1 N13 C14 139.2(9) . . . . ? N1 Ag1 N13 C17 -37.3(11) . . . . ? N1 C2 C9 N8 -17.1(5) . . . . ? N1 C2 C9 N10 165.6(3) . . . . ? N1 C2 N3 C4 1.9(3) . . . . ? N1 C2 N3 C6 179.0(3) . . . . ? N3 C2 C9 N8 160.7(3) . . . . ? N3 C2 C9 N10 -16.7(4) . . . . ? N3 C2 N1 Ag1 170.47(17) . . . . ? N3 C2 N1 C5 -1.8(3) . . . . ? N3 C4 C5 N1 0.2(3) . . . . ? N3 C6 C7 N10 -51.5(3) . . . . ? N8 Ag2 Ag3 N32 106.25(9) . . . . ? N8 Ag2 Ag3 N44 -69.05(9) . . . . ? N8 Ag2 N20 C21 -115.5(3) . . . . ? N8 Ag2 N20 C24 76.7(2) . . . . ? N8 Ag2 N25 C26 -21.1(3) . . . . ? N8 Ag2 N25 C29 141.58(19) . . . . ? N8 Ag2 N37 C38 5.1(2) . . . . ? N8 Ag2 N37 C41 -134.4(2) . . . . ? N8 C9 N10 C7 176.1(3) . . . . ? N8 C9 N10 C11 0.7(3) . . . . ? N10 C9 N8 Ag2 155.98(18) . . . . ? N10 C9 N8 C12 -0.8(3) . . . . ? N10 C11 C12 N8 -0.2(3) . . . . ? N13 Ag1 Ag2 Ag3 -159.64(6) . . . . ? N13 Ag1 Ag2 N8 131.04(9) . . . . ? N13 Ag1 Ag2 N20 28.28(8) . . . . ? N13 Ag1 Ag2 N25 -86.50(9) . . . . ? N13 Ag1 Ag2 N37 -36.3(2) . . . . ? N13 Ag1 N1 C2 -118.1(10) . . . . ? N13 Ag1 N1 C5 52.8(11) . . . . ? N13 C14 C21 N20 16.6(5) . . . . ? N13 C14 C21 N22 -160.6(3) . . . . ? N13 C14 N15 C16 -1.0(3) . . . . ? N13 C14 N15 C18 -175.6(2) . . . . ? N15 C14 C21 N20 -169.3(3) . . . . ? N15 C14 C21 N22 13.4(3) . . . . ? N15 C14 N13 Ag1 -176.42(18) . . . . ? N15 C14 N13 C17 0.6(3) . . . . ? N15 C16 C17 N13 -0.6(3) . . . . ? N15 C18 C19 N22 50.1(3) . . . . ? N20 Ag2 Ag3 N32 177.5(2) . . . . ? N20 Ag2 Ag3 N44 2.2(2) . . . . ? N20 Ag2 N8 C9 130.6(2) . . . . ? N20 Ag2 N8 C12 -77.0(2) . . . . ? N20 Ag2 N25 C26 -148.4(2) . . . . ? N20 Ag2 N25 C29 14.3(2) . . . . ? N20 Ag2 N37 C38 108.2(2) . . . . ? N20 Ag2 N37 C41 -31.2(2) . . . . ? N20 C21 N22 C19 -177.3(2) . . . . ? N20 C21 N22 C23 -2.2(3) . . . . ? N22 C21 N20 Ag2 -167.41(18) . . . . ? N22 C21 N20 C24 1.4(3) . . . . ? N22 C23 C24 N20 -1.2(3) . . . . ? N25 Ag2 Ag3 N32 -32.22(9) . . . . ? N25 Ag2 Ag3 N44 152.48(9) . . . . ? N25 Ag2 N8 C9 0.8(3) . . . . ? N25 Ag2 N8 C12 153.2(2) . . . . ? N25 Ag2 N20 C21 28.0(3) . . . . ? N25 Ag2 N20 C24 -139.75(19) . . . . ? N25 Ag2 N37 C38 -142.0(2) . . . . ? N25 Ag2 N37 C41 78.6(2) . . . . ? N25 C26 C33 N32 -15.3(5) . . . . ? N25 C26 C33 N34 167.1(3) . . . . ? N25 C26 N27 C28 1.4(3) . . . . ? N25 C26 N27 C30 177.2(2) . . . . ? N27 C26 C33 N32 162.8(3) . . . . ? N27 C26 C33 N34 -14.8(4) . . . . ? N27 C26 N25 Ag2 163.28(18) . . . . ? N27 C26 N25 C29 -1.1(3) . . . . ? N27 C28 C29 N25 0.4(3) . . . . ? N27 C30 C31 N34 -50.3(3) . . . . ? N32 Ag3 N44 C45 -157.0(9) . . . . ? N32 Ag3 N44 C48 17.4(11) . . . . ? N32 C33 N34 C31 175.4(2) . . . . ? N32 C33 N34 C35 0.3(3) . . . . ? N34 C33 N32 Ag3 175.56(18) . . . . ? N34 C33 N32 C36 -0.1(3) . . . . ? N34 C35 C36 N32 0.3(3) . . . . ? N37 Ag2 Ag3 N32 -135.93(9) . . . . ? N37 Ag2 Ag3 N44 48.77(9) . . . . ? N37 Ag2 N8 C9 -132.6(2) . . . . ? N37 Ag2 N8 C12 19.8(2) . . . . ? N37 Ag2 N20 C21 131.3(3) . . . . ? N37 Ag2 N20 C24 -36.4(2) . . . . ? N37 Ag2 N25 C26 115.5(3) . . . . ? N37 Ag2 N25 C29 -81.8(2) . . . . ? N37 C38 C45 N44 19.3(5) . . . . ? N37 C38 C45 N46 -161.1(3) . . . . ? N37 C38 N39 C40 -2.0(3) . . . . ? N37 C38 N39 C42 179.5(2) . . . . ? N39 C38 C45 N44 -162.9(3) . . . . ? N39 C38 C45 N46 16.6(4) . . . . ? N39 C38 N37 Ag2 -143.35(19) . . . . ? N39 C38 N37 C41 2.1(3) . . . . ? N39 C40 C41 N37 0.2(3) . . . . ? N39 C42 C43 N46 48.2(3) . . . . ? N44 Ag3 N32 C33 148.0(9) . . . . ? N44 Ag3 N32 C36 -37.0(11) . . . . ? N44 C45 N46 C43 -178.0(2) . . . . ? N44 C45 N46 C47 -1.7(3) . . . . ? N46 C45 N44 Ag3 176.40(17) . . . . ? N46 C45 N44 C48 1.1(3) . . . . ? N46 C47 C48 N44 -0.8(3) . . . . ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 832769' #TrackingRef '- CMFJLGcecrevised.cif' _audit_creation_date 2012-06-10 _audit_creation_method ; Olex2 1.2-beta (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H12 Ag N6, F6 P' _chemical_formula_sum 'C12 H12 Ag F6 N6 P' _chemical_formula_weight 493.12 _chemical_melting_point ? 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y+1/2, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-x, y, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y-1/2, -z-1/2' 7 '-x-1/2, y-1/2, z' 8 'x, -y, z-1/2' _cell_length_a 21.9927(5) _cell_length_b 12.7858(3) _cell_length_c 11.2203(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3155.08(13) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9881 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 31.34 _cell_measurement_theta_min 2.59 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.6256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0617 before and 0.0533 after correction. The Ratio of minimum to maximum transmission is 0.83268792711. The \l/2 correction factor is 0.0015 ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1936 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_unetI/netI 0.0149 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 68125 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 3.04 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 3109 _reflns_number_total 3617 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.878 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 3617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0203 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+3.2256P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0516 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.535851(6) 1.038482(11) 0.607366(13) 0.02025(5) Uani 1 1 d . . . N10 N 0.32168(7) 1.05075(13) 0.65289(14) 0.0183(3) Uani 1 1 d . . . N13 N 0.56573(7) 0.89032(13) 0.68617(13) 0.0167(3) Uani 1 1 d . . . N15 N 0.56077(8) 0.72087(13) 0.72575(14) 0.0194(3) Uani 1 1 d . . . N1 N 0.47154(7) 1.16602(13) 0.59964(13) 0.0172(3) Uani 1 1 d . . . N3 N 0.38202(7) 1.23832(12) 0.63547(13) 0.0174(3) Uani 1 1 d . . . N8 N 0.39250(8) 0.96324(12) 0.55318(14) 0.0183(3) Uani 1 1 d . . . C11 C 0.29738(10) 0.95501(16) 0.62663(18) 0.0235(4) Uani 1 1 d . . . H11 H 0.2588 0.9309 0.6464 0.028 Uiso 1 1 calc R . . C12 C 0.34128(9) 0.90215(16) 0.56566(17) 0.0220(4) Uani 1 1 d . . . H12 H 0.3372 0.8344 0.5366 0.026 Uiso 1 1 calc R . . C9 C 0.37895(8) 1.05206(14) 0.60792(15) 0.0156(4) Uani 1 1 d . . . C7 C 0.29516(9) 1.14147(16) 0.71326(18) 0.0235(4) Uani 1 1 d . . . H7A H 0.3084 1.1433 0.7957 0.028 Uiso 1 1 calc R . . H7B H 0.2512 1.1367 0.7120 0.028 Uiso 1 1 calc R . . C18 C 0.53340(9) 0.62273(16) 0.76747(18) 0.0246(4) Uani 1 1 d . . . H18A H 0.5373 0.6172 0.8533 0.030 Uiso 1 1 calc R . . H18B H 0.5540 0.5635 0.7314 0.030 Uiso 1 1 calc R . . C17 C 0.62040(8) 0.84300(16) 0.65756(16) 0.0192(4) Uani 1 1 d . . . H17 H 0.6541 0.8776 0.6268 0.023 Uiso 1 1 calc R . . C16 C 0.61784(9) 0.73882(16) 0.68071(17) 0.0215(4) Uani 1 1 d . . . H16 H 0.6484 0.6898 0.6686 0.026 Uiso 1 1 calc R . . C14 C 0.53119(8) 0.81399(15) 0.72868(15) 0.0167(4) Uani 1 1 d . . . C6 C 0.31563(9) 1.24032(16) 0.64944(18) 0.0226(4) Uani 1 1 d . . . H6A H 0.2964 1.2445 0.5718 0.027 Uiso 1 1 calc R . . H6B H 0.3037 1.3013 0.6952 0.027 Uiso 1 1 calc R . . C4 C 0.42289(10) 1.31861(15) 0.62702(17) 0.0218(4) Uani 1 1 d . . . H4 H 0.4147 1.3897 0.6342 0.026 Uiso 1 1 calc R . . C5 C 0.47797(9) 1.27345(16) 0.60592(16) 0.0204(4) Uani 1 1 d . . . H5 H 0.5144 1.3095 0.5971 0.025 Uiso 1 1 calc R . . C2 C 0.41274(8) 1.14827(14) 0.61613(15) 0.0157(4) Uani 1 1 d . . . P20 P 0.33982(2) 0.57101(4) 0.43846(4) 0.01873(10) Uani 1 1 d . . . F24 F 0.27065(6) 0.60784(11) 0.42475(12) 0.0363(3) Uani 1 1 d . . . F25 F 0.34043(6) 0.53474(9) 0.30140(10) 0.0285(3) Uani 1 1 d . . . F26 F 0.31832(6) 0.45642(10) 0.47624(12) 0.0341(3) Uani 1 1 d . . . F21 F 0.40949(5) 0.53528(10) 0.45150(12) 0.0300(3) Uani 1 1 d . . . F22 F 0.36236(6) 0.68540(10) 0.39928(11) 0.0298(3) Uani 1 1 d . . . F23 F 0.33928(7) 0.60726(11) 0.57495(11) 0.0362(3) 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 0.01584(8) 0.01766(8) 0.02726(8) -0.00569(6) -0.00372(6) 0.00226(5) N10 0.0149(8) 0.0213(9) 0.0187(7) -0.0008(6) -0.0004(6) -0.0001(6) N13 0.0157(8) 0.0208(8) 0.0138(7) -0.0008(6) -0.0004(6) 0.0007(6) N15 0.0210(8) 0.0185(8) 0.0187(8) 0.0004(6) 0.0001(6) 0.0032(7) N1 0.0166(8) 0.0167(8) 0.0183(7) -0.0003(6) 0.0010(6) -0.0006(6) N3 0.0172(8) 0.0160(8) 0.0190(7) -0.0030(6) -0.0026(6) 0.0035(6) N8 0.0231(8) 0.0147(7) 0.0170(7) 0.0004(6) 0.0005(6) 0.0004(6) C11 0.0207(10) 0.0244(10) 0.0254(10) 0.0023(8) -0.0033(8) -0.0067(8) C12 0.0291(11) 0.0180(9) 0.0188(9) 0.0015(7) -0.0040(8) -0.0055(8) C9 0.0150(9) 0.0167(9) 0.0151(8) 0.0007(7) 0.0000(6) 0.0012(7) C7 0.0155(9) 0.0308(11) 0.0242(9) -0.0072(8) 0.0020(7) 0.0029(8) C18 0.0313(12) 0.0170(10) 0.0256(10) 0.0027(8) 0.0024(8) 0.0031(8) C17 0.0147(9) 0.0280(10) 0.0147(8) -0.0018(7) -0.0002(7) 0.0013(8) C16 0.0195(10) 0.0264(11) 0.0186(9) -0.0027(8) -0.0008(7) 0.0067(8) C14 0.0185(10) 0.0190(9) 0.0127(8) -0.0012(7) -0.0021(7) 0.0021(7) C6 0.0173(10) 0.0239(10) 0.0265(10) -0.0077(8) -0.0041(8) 0.0078(8) C4 0.0288(11) 0.0138(9) 0.0227(9) -0.0014(7) -0.0050(8) 0.0006(8) C5 0.0222(10) 0.0182(9) 0.0209(9) 0.0005(7) -0.0020(7) -0.0041(8) C2 0.0177(9) 0.0158(9) 0.0137(8) -0.0013(7) -0.0012(6) 0.0026(7) P20 0.0193(2) 0.0187(2) 0.0182(2) 0.00074(18) 0.00185(18) 0.0029(2) F24 0.0225(7) 0.0400(8) 0.0465(8) -0.0016(6) -0.0004(6) 0.0107(6) F25 0.0366(7) 0.0286(7) 0.0205(6) -0.0051(5) -0.0002(5) -0.0004(5) F26 0.0347(7) 0.0252(7) 0.0422(7) 0.0089(6) 0.0122(6) -0.0017(6) F21 0.0200(6) 0.0342(7) 0.0357(7) 0.0020(5) -0.0008(5) 0.0056(5) F22 0.0407(8) 0.0184(6) 0.0303(6) 0.0004(5) 0.0020(5) -0.0013(5) F23 0.0452(8) 0.0454(8) 0.0179(6) -0.0033(5) 0.0042(5) 0.0070(7) _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 Ag1 3.0430(3) 5_676 ? Ag1 N13 2.1914(16) . ? Ag1 N1 2.1604(16) . ? Ag1 N8 2.3934(16) 5_676 ? N10 C11 1.368(3) . ? N10 C9 1.357(2) . ? N10 C7 1.464(2) . ? N13 C17 1.384(2) . ? N13 C14 1.326(2) . ? N15 C18 1.468(2) . ? N15 C16 1.372(3) . ? N15 C14 1.357(2) . ? N1 C5 1.383(3) . ? N1 C2 1.326(2) . ? N3 C6 1.469(2) . ? N3 C4 1.368(3) . ? N3 C2 1.353(2) . ? N8 Ag1 2.3934(16) 5_676 ? N8 C12 1.378(3) . ? N8 C9 1.325(2) . ? C11 H11 0.9300 . ? C11 C12 1.363(3) . ? C12 H12 0.9300 . ? C9 C2 1.440(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C6 1.521(3) . ? C18 C18 1.520(4) 4_656 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 H17 0.9300 . ? C17 C16 1.358(3) . ? C16 H16 0.9300 . ? C14 C14 1.453(4) 4_656 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C4 H4 0.9300 . ? C4 C5 1.363(3) . ? C5 H5 0.9300 . ? P20 F24 1.5999(13) . ? P20 F25 1.6063(12) . ? P20 F26 1.5969(13) . ? P20 F21 1.6054(13) . ? P20 F22 1.6056(13) . ? P20 F23 1.6001(13) . ? 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 N13 Ag1 Ag1 101.26(4) . 5_676 ? N13 Ag1 N8 95.64(5) . 5_676 ? N1 Ag1 Ag1 82.71(4) . 5_676 ? N1 Ag1 N13 149.88(6) . . ? N1 Ag1 N8 114.07(6) . 5_676 ? N8 Ag1 Ag1 75.07(4) 5_676 5_676 ? C11 N10 C7 130.77(17) . . ? C9 N10 C11 107.07(16) . . ? C9 N10 C7 122.13(16) . . ? C17 N13 Ag1 123.02(12) . . ? C14 N13 Ag1 127.58(12) . . ? C14 N13 C17 105.04(16) . . ? C16 N15 C18 129.44(17) . . ? C14 N15 C18 123.05(16) . . ? C14 N15 C16 107.50(16) . . ? C5 N1 Ag1 132.90(13) . . ? C2 N1 Ag1 120.24(13) . . ? C2 N1 C5 105.24(16) . . ? C4 N3 C6 130.36(17) . . ? C2 N3 C6 121.92(16) . . ? C2 N3 C4 107.43(16) . . ? C12 N8 Ag1 127.56(12) . 5_676 ? C9 N8 Ag1 120.32(12) . 5_676 ? C9 N8 C12 104.77(16) . . ? N10 C11 H11 127.0 . . ? C12 C11 N10 105.98(18) . . ? C12 C11 H11 127.0 . . ? N8 C12 H12 124.8 . . ? C11 C12 N8 110.44(17) . . ? C11 C12 H12 124.8 . . ? N10 C9 C2 117.76(16) . . ? N8 C9 N10 111.74(17) . . ? N8 C9 C2 130.22(17) . . ? N10 C7 H7A 109.9 . . ? N10 C7 H7B 109.9 . . ? N10 C7 C6 108.82(15) . . ? H7A C7 H7B 108.3 . . ? C6 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? N15 C18 C18 108.30(13) . 4_656 ? N15 C18 H18A 110.0 . . ? N15 C18 H18B 110.0 . . ? C18 C18 H18A 110.0 4_656 . ? C18 C18 H18B 110.0 4_656 . ? H18A C18 H18B 108.4 . . ? N13 C17 H17 124.8 . . ? C16 C17 N13 110.38(17) . . ? C16 C17 H17 124.8 . . ? N15 C16 H16 127.1 . . ? C17 C16 N15 105.81(17) . . ? C17 C16 H16 127.1 . . ? N13 C14 N15 111.25(16) . . ? N13 C14 C14 131.27(11) . 4_656 ? N15 C14 C14 117.43(11) . 4_656 ? N3 C6 C7 109.26(16) . . ? N3 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C7 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N3 C4 H4 126.9 . . ? C5 C4 N3 106.16(17) . . ? C5 C4 H4 126.9 . . ? N1 C5 H5 125.1 . . ? C4 C5 N1 109.80(18) . . ? C4 C5 H5 125.1 . . ? N1 C2 N3 111.34(17) . . ? N1 C2 C9 129.84(17) . . ? N3 C2 C9 118.66(16) . . ? F24 P20 F25 90.05(7) . . ? F24 P20 F21 179.34(8) . . ? F24 P20 F22 89.95(8) . . ? F24 P20 F23 89.98(7) . . ? F26 P20 F24 90.80(8) . . ? F26 P20 F25 89.53(7) . . ? F26 P20 F21 89.84(7) . . ? F26 P20 F22 179.06(8) . . ? F26 P20 F23 90.54(8) . . ? F21 P20 F25 89.84(7) . . ? F21 P20 F22 89.41(7) . . ? F22 P20 F25 89.90(7) . . ? F23 P20 F25 179.93(10) . . ? F23 P20 F21 90.13(7) . . ? F23 P20 F22 90.03(7) . . ? #===END