# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Miguel N. Moreno-Carretero' _publ_contact_author_email mmoreno@ujaen.es _publ_author_name 'Miguel Moreno-Carretero' data_import _database_code_depnum_ccdc_archive 'CCDC 846884' #TrackingRef 'Ag_DLMAceMOx_nitrato.cif' _audit_creation_date 2009-09-22T13:36:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H24 Ag2 N12 O12' _chemical_formula_sum 'C22 H24 Ag2 N12 O12' _chemical_formula_weight 864.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 7.8901(10) _cell_length_b 17.736(2) _cell_length_c 20.584(4) _cell_angle_alpha 90.000(10) _cell_angle_beta 95.64(2) _cell_angle_gamma 90.000(10) _cell_volume 2866.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 77(2) _cell_measurement_reflns_used 119 _cell_measurement_theta_min 4 _cell_measurement_theta_max 21 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.18 -1 0 0 0.18 0 1 0 0.07 0 -1 0 0.07 0 3 -4 0.05 0 -3 4 0.07 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6011 _exptl_absorpt_correction_T_max 0.8224 _exptl_absorpt_process_details '(SADABS 2.10, 2003)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_unetI/netI 0.0642 _diffrn_reflns_number 42611 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6581 _reflns_number_gt 4553 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0462P)^2^+7.1390P] 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_number_reflns 6581 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.096 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.131 _refine_diff_density_min -0.787 _refine_diff_density_rms 0.16 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.77988(5) 0.19732(2) 0.10523(2) 0.01987(11) Uani 1 1 d . . . Ag2 Ag 0.44224(5) 0.28437(2) 0.095134(19) 0.01876(11) Uani 1 1 d . . . O4A O 0.9133(5) 0.2292(2) 0.21883(18) 0.0247(8) Uani 1 1 d . . . O6N O -0.0519(4) 0.22139(19) 0.00876(18) 0.0218(8) Uani 1 1 d . . . N5B N 0.5867(5) 0.1086(2) 0.14050(19) 0.0159(9) Uani 1 1 d . . . O4B O 0.8237(4) 0.06900(19) 0.05718(18) 0.0231(8) Uani 1 1 d . . . O2A O 1.2108(5) 0.4122(2) 0.33285(19) 0.0323(9) Uani 1 1 d . . . O2B O 0.5579(5) -0.1534(2) 0.01466(19) 0.0297(9) Uani 1 1 d . . . O2N O 0.4919(6) 0.5163(2) 0.1171(2) 0.0419(11) Uani 1 1 d . . . N1B N 0.4455(5) -0.0762(2) 0.0858(2) 0.0190(9) Uani 1 1 d . . . O61A O 0.4862(4) 0.30588(19) -0.05163(17) 0.0219(8) Uani 1 1 d . . . N3A N 1.0535(5) 0.3222(2) 0.2774(2) 0.0231(10) Uani 1 1 d . . . C61B C 0.4991(7) 0.1876(3) 0.2262(3) 0.0219(11) Uani 1 1 d . . . O3N O 0.3458(5) 0.4154(2) 0.1270(2) 0.0328(10) Uani 1 1 d . . . O61B O 0.5256(5) 0.3097(2) 0.24547(19) 0.0335(10) Uani 1 1 d . . . N8A N 0.9492(5) 0.4751(2) 0.1324(2) 0.0183(9) Uani 1 1 d . . . O4N O 0.1542(5) 0.2302(2) 0.0851(2) 0.0311(9) Uani 1 1 d . . . N61A N 0.5666(5) 0.3249(2) 0.0094(2) 0.0168(9) Uani 1 1 d . . . N8B N 0.3332(5) 0.0048(2) 0.1590(2) 0.0230(10) Uani 1 1 d . . . O1N O 0.5794(5) 0.4345(2) 0.1888(2) 0.0322(9) Uani 1 1 d . . . N3B N 0.6868(5) -0.0406(2) 0.0332(2) 0.0166(9) Uani 1 1 d . . . N61B N 0.4916(6) 0.2528(2) 0.1999(2) 0.0227(10) Uani 1 1 d . . . N1A N 1.0937(5) 0.4419(2) 0.2314(2) 0.0225(10) Uani 1 1 d . . . O5N O 0.1732(5) 0.2828(2) -0.0090(2) 0.0375(11) Uani 1 1 d . . . N5A N 0.8393(5) 0.3276(2) 0.1148(2) 0.0164(9) Uani 1 1 d . . . C8AB C 0.4521(6) -0.0088(3) 0.1190(2) 0.0173(10) Uani 1 1 d . . . N2N N 0.0927(5) 0.2446(2) 0.0288(2) 0.0230(10) Uani 1 1 d . . . C4AB C 0.5759(6) 0.0437(3) 0.1084(2) 0.0150(10) Uani 1 1 d . . . C71A C 0.7913(7) 0.5154(3) 0.0328(3) 0.0257(12) Uani 1 1 d . . . H71A H 0.8373 0.563 0.0482 0.039 Uiso 1 1 calc R . . H71B H 0.6692 0.5176 0.0294 0.039 Uiso 1 1 calc R . . H71C H 0.8282 0.5047 -0.0093 0.039 Uiso 1 1 calc R . . C1B C 0.3175(7) -0.1322(3) 0.0985(3) 0.0280(13) Uani 1 1 d . . . H1B1 H 0.3297 -0.1757 0.0715 0.042 Uiso 1 1 calc R . . H1B2 H 0.2059 -0.1111 0.0886 0.042 Uiso 1 1 calc R . . H1B3 H 0.3326 -0.1468 0.1436 0.042 Uiso 1 1 calc R . . C71B C 0.2091(8) 0.0842(3) 0.2353(3) 0.0399(17) Uani 1 1 d . . . H71D H 0.1326 0.042 0.2345 0.06 Uiso 1 1 calc R . . H71E H 0.1472 0.1285 0.2204 0.06 Uiso 1 1 calc R . . H71F H 0.26 0.092 0.2791 0.06 Uiso 1 1 calc R . . C2B C 0.5626(6) -0.0944(3) 0.0435(3) 0.0207(11) Uani 1 1 d . . . N1N N 0.4712(6) 0.4562(2) 0.1434(2) 0.0253(10) Uani 1 1 d . . . C61A C 0.7117(6) 0.3550(3) 0.0061(2) 0.0172(10) Uani 1 1 d . . . C4AA C 0.9288(6) 0.3493(3) 0.1699(3) 0.0178(10) Uani 1 1 d . . . C6A C 0.8037(6) 0.3789(3) 0.0687(2) 0.0156(10) Uani 1 1 d . . . C2A C 1.1248(7) 0.3937(3) 0.2834(3) 0.0264(13) Uani 1 1 d . . . C6B C 0.4746(6) 0.1215(3) 0.1837(2) 0.0190(11) Uani 1 1 d . . . C4A C 0.9624(6) 0.2940(3) 0.2220(3) 0.0192(11) Uani 1 1 d . . . C62A C 0.7899(6) 0.3674(3) -0.0556(2) 0.0205(11) Uani 1 1 d . . . H62A H 0.7147 0.3489 -0.0916 0.031 Uiso 1 1 calc R . . H62B H 0.8965 0.341 -0.054 0.031 Uiso 1 1 calc R . . H62C H 0.8091 0.4204 -0.0613 0.031 Uiso 1 1 calc R . . C8AA C 0.9900(6) 0.4223(3) 0.1765(3) 0.0196(11) Uani 1 1 d . . . C4B C 0.7064(6) 0.0269(3) 0.0657(2) 0.0162(10) Uani 1 1 d . . . C3A C 1.0863(8) 0.2732(3) 0.3346(3) 0.0331(14) Uani 1 1 d . . . H3A1 H 1.1504 0.3004 0.3691 0.05 Uiso 1 1 calc R . . H3A2 H 1.15 0.2299 0.3232 0.05 Uiso 1 1 calc R . . H3A3 H 0.98 0.2572 0.3491 0.05 Uiso 1 1 calc R . . C7A C 0.8516(6) 0.4552(3) 0.0791(3) 0.0190(11) Uani 1 1 d . . . C62B C 0.5460(9) 0.1764(3) 0.2976(3) 0.0375(15) Uani 1 1 d . . . H62D H 0.5575 0.2245 0.3188 0.056 Uiso 1 1 calc R . . H62E H 0.6521 0.1496 0.3042 0.056 Uiso 1 1 calc R . . H62F H 0.4586 0.1477 0.3156 0.056 Uiso 1 1 calc R . . C7B C 0.3446(7) 0.0686(3) 0.1918(3) 0.0231(12) Uani 1 1 d . . . C3B C 0.8193(6) -0.0636(3) -0.0074(3) 0.0219(12) Uani 1 1 d . . . H3B1 H 0.7901 -0.1115 -0.0271 0.033 Uiso 1 1 calc R . . H3B2 H 0.926 -0.0677 0.0191 0.033 Uiso 1 1 calc R . . H3B3 H 0.8291 -0.0266 -0.0409 0.033 Uiso 1 1 calc R . . C1A C 1.1883(7) 0.5130(3) 0.2362(3) 0.0290(13) Uani 1 1 d . . . H1A1 H 1.1578 0.5427 0.1978 0.044 Uiso 1 1 calc R . . H1A2 H 1.3083 0.5027 0.2397 0.044 Uiso 1 1 calc R . . H1A3 H 1.1608 0.5403 0.274 0.044 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 0.0223(2) 0.0169(2) 0.0206(2) -0.00139(16) 0.00319(15) -0.00339(15) Ag2 0.0206(2) 0.0211(2) 0.0147(2) 0.00097(16) 0.00193(15) -0.00145(15) O4A 0.033(2) 0.021(2) 0.019(2) -0.0006(16) -0.0045(16) -0.0019(16) O6N 0.0168(18) 0.0219(19) 0.026(2) -0.0030(16) -0.0003(15) -0.0064(14) N5B 0.021(2) 0.016(2) 0.012(2) 0.0012(17) 0.0023(17) -0.0001(17) O4B 0.0231(19) 0.0201(19) 0.027(2) -0.0040(16) 0.0090(16) -0.0056(15) O2A 0.034(2) 0.039(2) 0.021(2) -0.0101(19) -0.0091(17) -0.0008(18) O2B 0.041(2) 0.017(2) 0.032(2) -0.0052(17) 0.0077(18) -0.0090(17) O2N 0.056(3) 0.023(2) 0.048(3) 0.011(2) 0.014(2) 0.005(2) N1B 0.018(2) 0.020(2) 0.017(2) 0.0016(18) -0.0026(17) -0.0031(17) O61A 0.029(2) 0.0251(19) 0.0108(18) -0.0009(15) -0.0040(15) -0.0088(15) N3A 0.026(2) 0.027(2) 0.015(2) -0.0005(19) -0.0039(18) -0.0011(19) C61B 0.026(3) 0.025(3) 0.015(3) -0.001(2) 0.004(2) 0.005(2) O3N 0.027(2) 0.029(2) 0.043(3) -0.0095(19) 0.0034(18) 0.0022(17) O61B 0.057(3) 0.024(2) 0.018(2) -0.0061(17) -0.0015(19) 0.0055(19) N8A 0.019(2) 0.016(2) 0.020(2) -0.0034(18) 0.0008(18) -0.0002(17) O4N 0.027(2) 0.041(2) 0.025(2) -0.0078(19) -0.0022(17) 0.0051(18) N61A 0.018(2) 0.017(2) 0.015(2) -0.0015(17) -0.0013(17) -0.0040(17) N8B 0.018(2) 0.025(2) 0.026(3) 0.005(2) 0.0036(18) -0.0016(18) O1N 0.030(2) 0.030(2) 0.036(3) 0.0078(19) 0.0003(19) 0.0009(17) N3B 0.020(2) 0.014(2) 0.016(2) 0.0002(17) 0.0024(17) 0.0015(16) N61B 0.033(3) 0.023(2) 0.011(2) -0.0007(19) 0.0020(19) 0.002(2) N1A 0.022(2) 0.025(2) 0.020(3) -0.007(2) -0.0017(19) -0.0033(18) O5N 0.028(2) 0.031(2) 0.056(3) 0.010(2) 0.017(2) -0.0052(18) N5A 0.013(2) 0.020(2) 0.016(2) -0.0022(18) 0.0022(17) -0.0003(16) C8AB 0.017(2) 0.018(2) 0.017(3) 0.003(2) -0.001(2) 0.0004(19) N2N 0.021(2) 0.016(2) 0.033(3) -0.005(2) 0.005(2) -0.0007(18) C4AB 0.017(2) 0.015(2) 0.012(3) 0.002(2) 0.0012(19) 0.0017(19) C71A 0.023(3) 0.024(3) 0.030(3) -0.002(2) 0.004(2) 0.000(2) C1B 0.029(3) 0.019(3) 0.035(4) 0.006(3) 0.001(3) -0.008(2) C71B 0.032(3) 0.035(3) 0.058(5) 0.005(3) 0.029(3) 0.004(3) C2B 0.024(3) 0.017(3) 0.020(3) 0.004(2) -0.001(2) -0.001(2) N1N 0.031(3) 0.016(2) 0.031(3) -0.003(2) 0.011(2) 0.003(2) C61A 0.019(3) 0.018(3) 0.015(3) 0.002(2) 0.002(2) 0.001(2) C4AA 0.013(2) 0.023(3) 0.017(3) -0.006(2) -0.0011(19) -0.001(2) C6A 0.015(2) 0.017(2) 0.015(3) 0.000(2) 0.0031(19) 0.0008(19) C2A 0.021(3) 0.035(3) 0.023(3) -0.012(3) 0.001(2) 0.000(2) C6B 0.022(3) 0.021(3) 0.014(3) 0.003(2) 0.002(2) 0.005(2) C4A 0.014(2) 0.025(3) 0.018(3) -0.006(2) -0.0023(19) 0.000(2) C62A 0.019(3) 0.025(3) 0.018(3) 0.003(2) 0.000(2) -0.003(2) C8AA 0.012(2) 0.029(3) 0.018(3) -0.011(2) 0.002(2) -0.001(2) C4B 0.017(2) 0.016(2) 0.015(3) 0.000(2) -0.0027(19) 0.0034(19) C3A 0.039(3) 0.036(3) 0.022(3) 0.001(3) -0.007(3) 0.000(3) C7A 0.019(3) 0.020(3) 0.019(3) 0.000(2) 0.007(2) -0.001(2) C62B 0.066(4) 0.030(3) 0.017(3) 0.005(3) 0.007(3) 0.012(3) C7B 0.026(3) 0.018(3) 0.027(3) 0.002(2) 0.008(2) 0.005(2) C3B 0.021(3) 0.024(3) 0.020(3) -0.002(2) 0.002(2) 0.005(2) C1A 0.026(3) 0.029(3) 0.032(3) -0.014(3) 0.000(2) -0.009(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N5B 2.354(4) . ? Ag1 N5A 2.362(4) . ? Ag1 O4B 2.519(3) . ? Ag1 O6N 2.531(4) 1_655 ? Ag1 O4A 2.532(4) . ? Ag1 Ag2 3.0684(7) . ? Ag2 N61A 2.221(4) . ? Ag2 N61B 2.225(4) . ? Ag2 O4N 2.457(4) . ? Ag2 O3N 2.550(4) . ? O4A C4A 1.213(6) . ? O6N N2N 1.244(5) . ? O6N Ag1 2.531(4) 1_455 ? N5B C4AB 1.325(6) . ? N5B C6B 1.334(6) . ? O4B C4B 1.214(6) . ? O2A C2A 1.212(6) . ? O2B C2B 1.201(6) . ? O2N N1N 1.215(6) . ? N1B C2B 1.370(6) . ? N1B C8AB 1.374(6) . ? N1B C1B 1.459(6) . ? O61A N61A 1.393(5) . ? N3A C4A 1.382(6) . ? N3A C2A 1.389(7) . ? N3A C3A 1.465(7) . ? C61B N61B 1.276(7) . ? C61B C6B 1.463(7) . ? C61B C62B 1.493(7) . ? O3N N1N 1.245(6) . ? O61B N61B 1.386(6) . ? N8A C8AA 1.322(7) . ? N8A C7A 1.325(6) . ? O4N N2N 1.240(6) . ? N61A C61A 1.272(6) . ? N8B C7B 1.316(7) . ? N8B C8AB 1.331(6) . ? O1N N1N 1.261(6) . ? N3B C4B 1.373(6) . ? N3B C2B 1.399(6) . ? N3B C3B 1.459(6) . ? N1A C2A 1.372(7) . ? N1A C8AA 1.374(6) . ? N1A C1A 1.464(6) . ? O5N N2N 1.250(6) . ? N5A C6A 1.326(6) . ? N5A C4AA 1.332(6) . ? C8AB C4AB 1.382(6) . ? C4AB C4B 1.450(6) . ? C71A C7A 1.478(7) . ? C71A H71A 0.96 . ? C71A H71B 0.96 . ? C71A H71C 0.96 . ? C1B H1B1 0.96 . ? C1B H1B2 0.96 . ? C1B H1B3 0.96 . ? C71B C7B 1.486(7) . ? C71B H71D 0.96 . ? C71B H71E 0.96 . ? C71B H71F 0.96 . ? C61A C6A 1.476(7) . ? C61A C62A 1.483(7) . ? C4AA C8AA 1.382(7) . ? C4AA C4A 1.459(7) . ? C6A C7A 1.416(7) . ? C6B C7B 1.412(7) . ? C62A H62A 0.96 . ? C62A H62B 0.96 . ? C62A H62C 0.96 . ? C3A H3A1 0.96 . ? C3A H3A2 0.96 . ? C3A H3A3 0.96 . ? C62B H62D 0.96 . ? C62B H62E 0.96 . ? C62B H62F 0.96 . ? C3B H3B1 0.96 . ? C3B H3B2 0.96 . ? C3B H3B3 0.96 . ? C1A H1A1 0.96 . ? C1A H1A2 0.96 . ? C1A H1A3 0.96 . ? 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 N5B Ag1 N5A 139.21(13) . . ? N5B Ag1 O4B 68.62(12) . . ? N5A Ag1 O4B 151.99(12) . . ? N5B Ag1 O6N 139.47(12) . 1_655 ? N5A Ag1 O6N 77.60(12) . 1_655 ? O4B Ag1 O6N 75.02(11) . 1_655 ? N5B Ag1 O4A 95.01(13) . . ? N5A Ag1 O4A 69.12(13) . . ? O4B Ag1 O4A 120.24(12) . . ? O6N Ag1 O4A 118.98(12) 1_655 . ? N5B Ag1 Ag2 76.87(10) . . ? N5A Ag1 Ag2 71.18(9) . . ? O4B Ag1 Ag2 125.43(8) . . ? O6N Ag1 Ag2 112.38(8) 1_655 . ? O4A Ag1 Ag2 103.28(9) . . ? N61A Ag2 N61B 143.37(15) . . ? N61A Ag2 O4N 122.50(14) . . ? N61B Ag2 O4N 93.16(15) . . ? N61A Ag2 O3N 94.32(14) . . ? N61B Ag2 O3N 90.48(15) . . ? O4N Ag2 O3N 94.65(13) . . ? N61A Ag2 Ag1 76.61(11) . . ? N61B Ag2 Ag1 74.91(11) . . ? O4N Ag2 Ag1 126.76(9) . . ? O3N Ag2 Ag1 136.05(9) . . ? C4A O4A Ag1 111.3(3) . . ? N2N O6N Ag1 109.3(3) . 1_455 ? C4AB N5B C6B 117.8(4) . . ? C4AB N5B Ag1 116.0(3) . . ? C6B N5B Ag1 125.7(3) . . ? C4B O4B Ag1 111.3(3) . . ? C2B N1B C8AB 121.8(4) . . ? C2B N1B C1B 118.3(4) . . ? C8AB N1B C1B 119.8(4) . . ? C4A N3A C2A 125.2(5) . . ? C4A N3A C3A 119.1(4) . . ? C2A N3A C3A 115.7(5) . . ? N61B C61B C6B 118.4(5) . . ? N61B C61B C62B 122.3(5) . . ? C6B C61B C62B 119.1(5) . . ? N1N O3N Ag2 110.5(3) . . ? C8AA N8A C7A 117.5(4) . . ? N2N O4N Ag2 105.7(3) . . ? C61A N61A O61A 112.8(4) . . ? C61A N61A Ag2 130.4(3) . . ? O61A N61A Ag2 116.1(3) . . ? C7B N8B C8AB 117.2(4) . . ? C4B N3B C2B 124.6(4) . . ? C4B N3B C3B 118.0(4) . . ? C2B N3B C3B 116.7(4) . . ? C61B N61B O61B 112.1(4) . . ? C61B N61B Ag2 129.4(4) . . ? O61B N61B Ag2 118.5(3) . . ? C2A N1A C8AA 122.0(4) . . ? C2A N1A C1A 115.7(4) . . ? C8AA N1A C1A 122.1(5) . . ? C6A N5A C4AA 117.9(4) . . ? C6A N5A Ag1 125.9(3) . . ? C4AA N5A Ag1 116.0(3) . . ? N8B C8AB N1B 118.1(4) . . ? N8B C8AB C4AB 121.8(5) . . ? N1B C8AB C4AB 120.1(4) . . ? O4N N2N O6N 120.2(4) . . ? O4N N2N O5N 121.2(5) . . ? O6N N2N O5N 118.6(5) . . ? N5B C4AB C8AB 121.3(4) . . ? N5B C4AB C4B 117.8(4) . . ? C8AB C4AB C4B 120.7(4) . . ? C7A C71A H71A 109.5 . . ? C7A C71A H71B 109.5 . . ? H71A C71A H71B 109.5 . . ? C7A C71A H71C 109.5 . . ? H71A C71A H71C 109.5 . . ? H71B C71A H71C 109.5 . . ? N1B C1B H1B1 109.5 . . ? N1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? N1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C7B C71B H71D 109.5 . . ? C7B C71B H71E 109.5 . . ? H71D C71B H71E 109.5 . . ? C7B C71B H71F 109.5 . . ? H71D C71B H71F 109.5 . . ? H71E C71B H71F 109.5 . . ? O2B C2B N1B 122.0(5) . . ? O2B C2B N3B 120.5(5) . . ? N1B C2B N3B 117.5(4) . . ? O2N N1N O3N 121.8(5) . . ? O2N N1N O1N 119.1(5) . . ? O3N N1N O1N 119.1(4) . . ? N61A C61A C6A 116.3(4) . . ? N61A C61A C62A 124.1(5) . . ? C6A C61A C62A 119.7(4) . . ? N5A C4AA C8AA 120.4(5) . . ? N5A C4AA C4A 118.2(4) . . ? C8AA C4AA C4A 121.4(5) . . ? N5A C6A C7A 120.9(5) . . ? N5A C6A C61A 118.6(4) . . ? C7A C6A C61A 120.5(4) . . ? O2A C2A N1A 122.0(5) . . ? O2A C2A N3A 120.6(5) . . ? N1A C2A N3A 117.4(5) . . ? N5B C6B C7B 120.1(5) . . ? N5B C6B C61B 118.5(4) . . ? C7B C6B C61B 121.1(4) . . ? O4A C4A N3A 121.7(5) . . ? O4A C4A C4AA 124.4(5) . . ? N3A C4A C4AA 114.0(4) . . ? C61A C62A H62A 109.5 . . ? C61A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C61A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? N8A C8AA N1A 118.0(5) . . ? N8A C8AA C4AA 122.5(5) . . ? N1A C8AA C4AA 119.5(5) . . ? O4B C4B N3B 121.2(4) . . ? O4B C4B C4AB 123.9(4) . . ? N3B C4B C4AB 115.0(4) . . ? N3A C3A H3A1 109.5 . . ? N3A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N3A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N8A C7A C6A 120.3(5) . . ? N8A C7A C71A 117.8(4) . . ? C6A C7A C71A 121.9(5) . . ? C61B C62B H62D 109.5 . . ? C61B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C61B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N8B C7B C6B 121.7(5) . . ? N8B C7B C71B 116.9(5) . . ? C6B C7B C71B 121.4(5) . . ? N3B C3B H3B1 109.5 . . ? N3B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N3B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N1A C1A H1A1 109.5 . . ? N1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? N1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5B Ag1 Ag2 N61A -143.21(15) . . . . ? N5A Ag1 Ag2 N61A 62.53(15) . . . . ? O4B Ag1 Ag2 N61A -91.92(15) . . . . ? O6N Ag1 Ag2 N61A -4.79(13) 1_655 . . . ? O4A Ag1 Ag2 N61A 124.67(13) . . . . ? N5B Ag1 Ag2 N61B 60.08(15) . . . . ? N5A Ag1 Ag2 N61B -94.19(16) . . . . ? O4B Ag1 Ag2 N61B 111.37(15) . . . . ? O6N Ag1 Ag2 N61B -161.50(14) 1_655 . . . ? O4A Ag1 Ag2 N61B -32.05(15) . . . . ? N5B Ag1 Ag2 O4N -22.44(16) . . . . ? N5A Ag1 Ag2 O4N -176.71(16) . . . . ? O4B Ag1 Ag2 O4N 28.85(16) . . . . ? O6N Ag1 Ag2 O4N 115.98(15) 1_655 . . . ? O4A Ag1 Ag2 O4N -114.57(15) . . . . ? N5B Ag1 Ag2 O3N 134.58(17) . . . . ? N5A Ag1 Ag2 O3N -19.69(18) . . . . ? O4B Ag1 Ag2 O3N -174.13(17) . . . . ? O6N Ag1 Ag2 O3N -87.00(16) 1_655 . . . ? O4A Ag1 Ag2 O3N 42.45(16) . . . . ? N5B Ag1 O4A C4A -149.3(3) . . . . ? N5A Ag1 O4A C4A -8.0(3) . . . . ? O4B Ag1 O4A C4A 142.6(3) . . . . ? O6N Ag1 O4A C4A 53.7(4) 1_655 . . . ? Ag2 Ag1 O4A C4A -71.6(3) . . . . ? N5A Ag1 N5B C4AB 163.0(3) . . . . ? O4B Ag1 N5B C4AB -12.9(3) . . . . ? O6N Ag1 N5B C4AB 14.9(4) 1_655 . . . ? O4A Ag1 N5B C4AB -133.5(3) . . . . ? Ag2 Ag1 N5B C4AB 124.0(3) . . . . ? N5A Ag1 N5B C6B -8.4(5) . . . . ? O4B Ag1 N5B C6B 175.7(4) . . . . ? O6N Ag1 N5B C6B -156.5(3) 1_655 . . . ? O4A Ag1 N5B C6B 55.1(4) . . . . ? Ag2 Ag1 N5B C6B -47.3(4) . . . . ? N5B Ag1 O4B C4B 12.2(3) . . . . ? N5A Ag1 O4B C4B -162.1(3) . . . . ? O6N Ag1 O4B C4B -149.5(4) 1_655 . . . ? O4A Ag1 O4B C4B 95.3(3) . . . . ? Ag2 Ag1 O4B C4B -42.5(4) . . . . ? N61A Ag2 O3N N1N -64.7(4) . . . . ? N61B Ag2 O3N N1N 78.9(4) . . . . ? O4N Ag2 O3N N1N 172.1(4) . . . . ? Ag1 Ag2 O3N N1N 10.4(4) . . . . ? N61A Ag2 O4N N2N -12.2(4) . . . . ? N61B Ag2 O4N N2N 176.6(3) . . . . ? O3N Ag2 O4N N2N 85.9(3) . . . . ? Ag1 Ag2 O4N N2N -109.9(3) . . . . ? N61B Ag2 N61A C61A -16.1(6) . . . . ? O4N Ag2 N61A C61A 178.8(4) . . . . ? O3N Ag2 N61A C61A 80.5(4) . . . . ? Ag1 Ag2 N61A C61A -55.9(4) . . . . ? N61B Ag2 N61A O61A 153.9(3) . . . . ? O4N Ag2 N61A O61A -11.2(4) . . . . ? O3N Ag2 N61A O61A -109.5(3) . . . . ? Ag1 Ag2 N61A O61A 114.1(3) . . . . ? C6B C61B N61B O61B -177.0(4) . . . . ? C62B C61B N61B O61B -2.2(7) . . . . ? C6B C61B N61B Ag2 0.8(7) . . . . ? C62B C61B N61B Ag2 175.6(4) . . . . ? N61A Ag2 N61B C61B -104.4(5) . . . . ? O4N Ag2 N61B C61B 63.0(5) . . . . ? O3N Ag2 N61B C61B 157.7(5) . . . . ? Ag1 Ag2 N61B C61B -64.3(5) . . . . ? N61A Ag2 N61B O61B 73.2(4) . . . . ? O4N Ag2 N61B O61B -119.4(3) . . . . ? O3N Ag2 N61B O61B -24.7(3) . . . . ? Ag1 Ag2 N61B O61B 113.3(3) . . . . ? N5B Ag1 N5A C6A -105.1(4) . . . . ? O4B Ag1 N5A C6A 66.8(5) . . . . ? O6N Ag1 N5A C6A 54.3(4) 1_655 . . . ? O4A Ag1 N5A C6A -177.7(4) . . . . ? Ag2 Ag1 N5A C6A -64.8(4) . . . . ? N5B Ag1 N5A C4AA 80.6(4) . . . . ? O4B Ag1 N5A C4AA -107.5(4) . . . . ? O6N Ag1 N5A C4AA -119.9(3) 1_655 . . . ? O4A Ag1 N5A C4AA 8.0(3) . . . . ? Ag2 Ag1 N5A C4AA 121.0(3) . . . . ? C7B N8B C8AB N1B 178.0(5) . . . . ? C7B N8B C8AB C4AB -4.4(7) . . . . ? C2B N1B C8AB N8B 179.8(5) . . . . ? C1B N1B C8AB N8B -4.1(7) . . . . ? C2B N1B C8AB C4AB 2.2(7) . . . . ? C1B N1B C8AB C4AB 178.3(5) . . . . ? Ag2 O4N N2N O6N 177.4(3) . . . . ? Ag2 O4N N2N O5N -3.0(5) . . . . ? Ag1 O6N N2N O4N 23.3(5) 1_455 . . . ? Ag1 O6N N2N O5N -156.2(3) 1_455 . . . ? C6B N5B C4AB C8AB 0.4(7) . . . . ? Ag1 N5B C4AB C8AB -171.7(4) . . . . ? C6B N5B C4AB C4B -174.8(4) . . . . ? Ag1 N5B C4AB C4B 13.1(5) . . . . ? N8B C8AB C4AB N5B 3.5(8) . . . . ? N1B C8AB C4AB N5B -179.0(4) . . . . ? N8B C8AB C4AB C4B 178.6(5) . . . . ? N1B C8AB C4AB C4B -3.9(7) . . . . ? C8AB N1B C2B O2B 179.6(5) . . . . ? C1B N1B C2B O2B 3.4(8) . . . . ? C8AB N1B C2B N3B -2.3(7) . . . . ? C1B N1B C2B N3B -178.5(4) . . . . ? C4B N3B C2B O2B -177.3(5) . . . . ? C3B N3B C2B O2B -7.2(7) . . . . ? C4B N3B C2B N1B 4.6(7) . . . . ? C3B N3B C2B N1B 174.7(4) . . . . ? Ag2 O3N N1N O2N 123.9(4) . . . . ? Ag2 O3N N1N O1N -56.2(5) . . . . ? O61A N61A C61A C6A 178.3(4) . . . . ? Ag2 N61A C61A C6A -11.4(7) . . . . ? O61A N61A C61A C62A -1.2(7) . . . . ? Ag2 N61A C61A C62A 169.1(4) . . . . ? C6A N5A C4AA C8AA -3.6(7) . . . . ? Ag1 N5A C4AA C8AA 171.1(3) . . . . ? C6A N5A C4AA C4A 177.4(4) . . . . ? Ag1 N5A C4AA C4A -7.8(5) . . . . ? C4AA N5A C6A C7A -3.3(7) . . . . ? Ag1 N5A C6A C7A -177.5(3) . . . . ? C4AA N5A C6A C61A 177.1(4) . . . . ? Ag1 N5A C6A C61A 3.0(6) . . . . ? N61A C61A C6A N5A 58.6(6) . . . . ? C62A C61A C6A N5A -121.8(5) . . . . ? N61A C61A C6A C7A -120.9(5) . . . . ? C62A C61A C6A C7A 58.6(6) . . . . ? C8AA N1A C2A O2A -177.1(5) . . . . ? C1A N1A C2A O2A 7.5(7) . . . . ? C8AA N1A C2A N3A 3.0(7) . . . . ? C1A N1A C2A N3A -172.5(4) . . . . ? C4A N3A C2A O2A -175.9(5) . . . . ? C3A N3A C2A O2A 1.5(7) . . . . ? C4A N3A C2A N1A 4.1(7) . . . . ? C3A N3A C2A N1A -178.6(5) . . . . ? C4AB N5B C6B C7B -3.1(7) . . . . ? Ag1 N5B C6B C7B 168.1(4) . . . . ? C4AB N5B C6B C61B 171.4(4) . . . . ? Ag1 N5B C6B C61B -17.3(6) . . . . ? N61B C61B C6B N5B 63.2(7) . . . . ? C62B C61B C6B N5B -111.8(6) . . . . ? N61B C61B C6B C7B -122.3(6) . . . . ? C62B C61B C6B C7B 62.7(7) . . . . ? Ag1 O4A C4A N3A -174.0(4) . . . . ? Ag1 O4A C4A C4AA 7.7(6) . . . . ? C2A N3A C4A O4A 175.1(5) . . . . ? C3A N3A C4A O4A -2.2(7) . . . . ? C2A N3A C4A C4AA -6.4(7) . . . . ? C3A N3A C4A C4AA 176.4(4) . . . . ? N5A C4AA C4A O4A -0.5(7) . . . . ? C8AA C4AA C4A O4A -179.4(5) . . . . ? N5A C4AA C4A N3A -179.0(4) . . . . ? C8AA C4AA C4A N3A 2.1(7) . . . . ? C7A N8A C8AA N1A 178.8(4) . . . . ? C7A N8A C8AA C4AA -2.9(7) . . . . ? C2A N1A C8AA N8A 171.4(4) . . . . ? C1A N1A C8AA N8A -13.5(7) . . . . ? C2A N1A C8AA C4AA -6.9(7) . . . . ? C1A N1A C8AA C4AA 168.2(4) . . . . ? N5A C4AA C8AA N8A 7.0(7) . . . . ? C4A C4AA C8AA N8A -174.0(4) . . . . ? N5A C4AA C8AA N1A -174.7(4) . . . . ? C4A C4AA C8AA N1A 4.2(7) . . . . ? Ag1 O4B C4B N3B 167.5(3) . . . . ? Ag1 O4B C4B C4AB -11.0(6) . . . . ? C2B N3B C4B O4B 175.4(5) . . . . ? C3B N3B C4B O4B 5.4(7) . . . . ? C2B N3B C4B C4AB -6.1(7) . . . . ? C3B N3B C4B C4AB -176.1(4) . . . . ? N5B C4AB C4B O4B -0.6(7) . . . . ? C8AB C4AB C4B O4B -175.9(5) . . . . ? N5B C4AB C4B N3B -179.2(4) . . . . ? C8AB C4AB C4B N3B 5.6(7) . . . . ? C8AA N8A C7A C6A -4.1(7) . . . . ? C8AA N8A C7A C71A 174.0(4) . . . . ? N5A C6A C7A N8A 7.4(7) . . . . ? C61A C6A C7A N8A -173.0(4) . . . . ? N5A C6A C7A C71A -170.6(4) . . . . ? C61A C6A C7A C71A 9.0(7) . . . . ? C8AB N8B C7B C6B 1.6(8) . . . . ? C8AB N8B C7B C71B 178.6(5) . . . . ? N5B C6B C7B N8B 2.2(8) . . . . ? C61B C6B C7B N8B -172.2(5) . . . . ? N5B C6B C7B C71B -174.7(5) . . . . ? C61B C6B C7B C71B 10.9(8) . . . . ? # Attachment 'Ag_DLMAceMOx_perchlorato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-10-05 at 13:01:56 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\archivos de programa\wingx\files\archive.dat # CIF files read : import dreduc struct data_Ag_DLMAceMOx_perchlorato _database_code_depnum_ccdc_archive 'CCDC 846885' #TrackingRef 'Ag_DLMAceMOx_perchlorato.cif' _audit_creation_date 2011-10-05T13:01:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H24 Ag2 Cl2 N10 O14' _chemical_formula_sum 'C22 H24 Ag2 Cl2 N10 O14' _chemical_formula_weight 939.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.2412(13) _cell_length_b 14.5295(15) _cell_length_c 16.661(3) _cell_angle_alpha 90 _cell_angle_beta 105.675(9) _cell_angle_gamma 90 _cell_volume 3086.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 77(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.12 -1 0 0 0.17 0 1 0 0.16 0 -1 0 0.16 0 0 1 0.18 0 0 -1 0.2 -5 6 0 0.146 5 -6 0 0.136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS 2.10, 2003)' _exptl_absorpt_correction_T_min 0.5527 _exptl_absorpt_correction_T_max 0.657 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1998 _diffrn_reflns_av_unetI/netI 0.1234 _diffrn_reflns_number 74990 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7099 _reflns_number_gt 3313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Despite the crystals are not of quality enough to reach good results in the refinement, XRD experiments for compound 3 allowed to know the main features of the structure. The reported results correspond to the best of three measurements on different crystals (even one at the liquid nitrogen temperature). The structure was refined taking into account no solvent molecules; however, the final parameters clearly indicate the presence of at least five important unassigned peaks. A peak (Q2) at 2.853 from the O22 atom could be assigned to the oxygen of a really disordered water molecule, because during the refinement a too high isotropic thermal parameter for this atom was reached. On the other hand, two couples of unassigned peaks are placed in a quasi-centrosymmetric pattern through the middle point of the Ag-Ag segment; Q3 and Q4 are placed at ca. 1.33 from Ag1 (Q3-Ag1-Q4, 177\%), whereas Q1 and Q5 are placed at ca. 1.42 from Ag2 (Q1-Ag2-Q5, 176\%). ; _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0000(2) _refine_ls_number_reflns 7099 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2139 _refine_ls_R_factor_gt 0.1069 _refine_ls_wR_factor_ref 0.3489 _refine_ls_wR_factor_gt 0.2694 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.09 _refine_ls_shift/su_mean 0 _refine_diff_density_max 5.293 _refine_diff_density_min -2.908 _refine_diff_density_rms 0.477 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 Ag2 Ag 0.24288(7) 0.94686(7) 0.25373(6) 0.0325(4) Uani 1 1 d . . . Ag1 Ag 0.19194(8) 1.15820(7) 0.28493(7) 0.0358(4) Uani 1 1 d . . . Cl2 Cl 0.4872(2) 0.8668(2) 0.2901(2) 0.0313(8) Uani 1 1 d . . . Cl1 Cl 0.0232(3) 0.7899(2) 0.1694(2) 0.0332(8) Uani 1 1 d . . . O8P O 0.5689(7) 0.8111(6) 0.3361(6) 0.035(2) Uani 1 1 d . . . O1P O 0.0903(8) 0.8368(6) 0.2400(6) 0.041(3) Uani 1 1 d . . . O5P O 0.3887(7) 0.8295(5) 0.2944(6) 0.035(2) Uani 1 1 d . . . O2B O 0.7000(7) 1.2155(6) 0.4648(6) 0.035(2) Uani 1 1 d . . . O4A O 0.0263(7) 1.1514(6) 0.1765(6) 0.034(2) Uani 1 1 d . . . O4B O 0.3465(7) 1.2152(6) 0.3944(6) 0.037(2) Uani 1 1 d . . . O61B O 0.0957(7) 1.0014(7) 0.0705(6) 0.040(2) Uani 1 1 d . . . O6P O 0.4906(7) 0.8756(6) 0.2068(6) 0.036(2) Uani 1 1 d . . . O4P O 0.0520(8) 0.6963(6) 0.1695(7) 0.043(3) Uani 1 1 d . . . O61A O 0.3911(6) 0.9879(6) 0.4427(6) 0.035(2) Uani 1 1 d . . . O2A O -0.2918(7) 1.0141(7) 0.1006(6) 0.049(3) Uani 1 1 d . . . O3P O -0.0824(7) 0.7953(7) 0.1719(7) 0.046(3) Uani 1 1 d . . . O7P O 0.4955(8) 0.9569(6) 0.3271(6) 0.040(2) Uani 1 1 d . . . N3B N 0.5240(7) 1.2130(7) 0.4299(7) 0.026(2) Uani 1 1 d . . . C61A C 0.2206(9) 0.9952(8) 0.4343(8) 0.028(3) Uani 1 1 d . . . N8B N 0.5305(8) 1.1069(7) 0.2089(7) 0.030(3) Uani 1 1 d . . . N61A N 0.2879(8) 0.9747(7) 0.3933(7) 0.032(3) Uani 1 1 d . . . N3A N -0.1312(8) 1.0827(8) 0.1385(7) 0.034(3) Uani 1 1 d . . . N1A N -0.1794(8) 0.9737(8) 0.2239(7) 0.034(3) Uani 1 1 d . . . N61B N 0.1924(8) 1.0156(8) 0.1287(7) 0.036(3) Uani 1 1 d . . . C8AB C 0.5257(9) 1.1450(8) 0.2789(8) 0.024(3) Uani 1 1 d . . . N5A N 0.0867(7) 1.0412(7) 0.3140(7) 0.027(2) Uani 1 1 d . . . O2P O 0.0341(8) 0.8329(7) 0.0954(7) 0.050(3) Uani 1 1 d . . . N8A N -0.0630(8) 0.9285(7) 0.3476(7) 0.030(3) Uani 1 1 d . . . N1B N 0.6158(8) 1.1657(7) 0.3347(7) 0.030(3) Uani 1 1 d . . . N5B N 0.3375(8) 1.1439(6) 0.2396(7) 0.028(3) Uani 1 1 d . . . C1A C -0.2565(9) 0.9085(11) 0.2382(9) 0.038(3) Uani 1 1 d . . . H1A1 H -0.2769 0.867 0.1917 0.056 Uiso 1 1 calc R . . H1A2 H -0.3169 0.9413 0.2441 0.056 Uiso 1 1 calc R . . H1A3 H -0.2263 0.8741 0.2881 0.056 Uiso 1 1 calc R . . C61B C 0.2414(9) 1.0834(9) 0.1087(8) 0.025(3) Uani 1 1 d . . . C71A C 0.0534(11) 0.8751(10) 0.4750(10) 0.044(4) Uani 1 1 d . . . H71A H 0.0305 0.9078 0.517 0.066 Uiso 1 1 calc R . . H71B H 0.1271 0.8622 0.4951 0.066 Uiso 1 1 calc R . . H71C H 0.0153 0.8184 0.4624 0.066 Uiso 1 1 calc R . . C2A C -0.2065(11) 1.0230(10) 0.1517(8) 0.035(3) Uani 1 1 d . . . C71B C 0.4440(10) 1.0397(8) 0.0768(9) 0.031(3) Uani 1 1 d . . . H71D H 0.5132 1.0454 0.0694 0.047 Uiso 1 1 calc R . . H71E H 0.394 1.0671 0.0303 0.047 Uiso 1 1 calc R . . H71F H 0.4275 0.9757 0.0804 0.047 Uiso 1 1 calc R . . C4B C 0.4282(9) 1.1981(8) 0.3773(8) 0.026(3) Uani 1 1 d . . . C6B C 0.3443(10) 1.1016(8) 0.1723(8) 0.028(3) Uani 1 1 d . . . C62A C 0.2475(11) 1.0287(9) 0.5191(9) 0.037(3) Uani 1 1 d . . . H62A H 0.2975 0.9879 0.5541 0.056 Uiso 1 1 calc R . . H62B H 0.1855 1.0314 0.5384 0.056 Uiso 1 1 calc R . . H62C H 0.2774 1.0891 0.5212 0.056 Uiso 1 1 calc R . . C7A C 0.0338(9) 0.9329(8) 0.3978(9) 0.030(3) Uani 1 1 d . . . C4AA C -0.0104(11) 1.0347(9) 0.2610(9) 0.035(3) Uani 1 1 d . . . C4A C -0.0309(9) 1.0936(9) 0.1890(8) 0.026(3) Uani 1 1 d . . . C6A C 0.1096(9) 0.9891(8) 0.3815(8) 0.025(3) Uani 1 1 d . . . C8AA C -0.0810(9) 0.9775(9) 0.2781(8) 0.027(3) Uani 1 1 d . . . C2B C 0.6171(10) 1.1991(8) 0.4130(8) 0.028(3) Uani 1 1 d . . . C62B C 0.2045(11) 1.1415(10) 0.0350(10) 0.045(4) Uani 1 1 d . . . H62D H 0.1798 1.1035 -0.0134 0.068 Uiso 1 1 calc R . . H62E H 0.2612 1.1793 0.0284 0.068 Uiso 1 1 calc R . . H62F H 0.1484 1.1801 0.0417 0.068 Uiso 1 1 calc R . . C1B C 0.7178(10) 1.1576(9) 0.3169(9) 0.035(3) Uani 1 1 d . . . H1B1 H 0.7466 1.0977 0.3333 0.052 Uiso 1 1 calc R . . H1B2 H 0.7645 1.2038 0.3475 0.052 Uiso 1 1 calc R . . H1B3 H 0.7091 1.166 0.2583 0.052 Uiso 1 1 calc R . . C3A C -0.1617(12) 1.1422(10) 0.0661(9) 0.043(4) Uani 1 1 d . . . H3A1 H -0.1808 1.2016 0.0826 0.065 Uiso 1 1 calc R . . H3A2 H -0.2205 1.1157 0.0258 0.065 Uiso 1 1 calc R . . H3A3 H -0.104 1.1487 0.0419 0.065 Uiso 1 1 calc R . . C3B C 0.5316(11) 1.2470(10) 0.5129(9) 0.042(4) Uani 1 1 d . . . H3B1 H 0.5838 1.2125 0.5527 0.063 Uiso 1 1 calc R . . H3B2 H 0.465 1.2402 0.5249 0.063 Uiso 1 1 calc R . . H3B3 H 0.5509 1.3109 0.5162 0.063 Uiso 1 1 calc R . . C7B C 0.4401(9) 1.0860(8) 0.1530(9) 0.030(3) Uani 1 1 d . . . C4AB C 0.4314(11) 1.1606(8) 0.2977(9) 0.032(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 Ag2 0.0266(6) 0.0279(6) 0.0427(7) -0.0002(4) 0.0086(5) -0.0017(4) Ag1 0.0231(6) 0.0315(6) 0.0535(8) 0.0018(5) 0.0115(5) -0.0032(4) Cl2 0.0255(17) 0.0232(16) 0.047(2) -0.0018(14) 0.0121(15) -0.0003(13) Cl1 0.0298(18) 0.0259(17) 0.045(2) 0.0000(14) 0.0124(15) -0.0037(14) O8P 0.028(5) 0.028(5) 0.049(6) -0.004(4) 0.010(4) 0.005(4) O1P 0.039(6) 0.037(6) 0.046(6) -0.009(5) 0.008(5) -0.015(4) O5P 0.035(5) 0.017(4) 0.056(7) -0.008(4) 0.017(5) -0.008(4) O2B 0.024(5) 0.039(5) 0.040(6) -0.013(4) 0.004(4) -0.001(4) O4A 0.028(5) 0.038(5) 0.040(6) 0.004(4) 0.014(4) 0.007(4) O4B 0.021(5) 0.035(5) 0.055(7) -0.001(5) 0.013(4) 0.000(4) O61B 0.018(5) 0.053(6) 0.043(6) 0.000(5) -0.004(4) -0.005(5) O6P 0.036(6) 0.043(6) 0.037(6) 0.004(5) 0.021(4) 0.001(5) O4P 0.039(6) 0.034(5) 0.064(7) 0.004(5) 0.026(5) 0.003(5) O61A 0.015(4) 0.039(5) 0.046(6) -0.014(4) -0.003(4) 0.001(4) O2A 0.028(5) 0.061(7) 0.048(7) -0.008(5) -0.005(5) -0.004(5) O3P 0.026(5) 0.039(6) 0.074(8) -0.016(5) 0.015(5) 0.000(4) O7P 0.052(6) 0.029(5) 0.043(6) -0.001(4) 0.023(5) -0.006(4) N3B 0.016(5) 0.025(5) 0.040(7) -0.006(5) 0.010(5) 0.004(4) C61A 0.024(7) 0.027(7) 0.034(8) 0.009(6) 0.011(6) -0.004(5) N8B 0.037(7) 0.017(5) 0.039(7) 0.002(5) 0.015(5) -0.009(5) N61A 0.018(5) 0.029(6) 0.046(7) -0.004(5) 0.006(5) 0.002(5) N3A 0.030(6) 0.028(6) 0.044(7) 0.005(5) 0.010(5) 0.010(5) N1A 0.018(6) 0.038(6) 0.047(8) 0.007(5) 0.010(5) -0.001(5) N61B 0.010(5) 0.043(7) 0.051(8) -0.011(6) -0.001(5) -0.005(5) C8AB 0.006(5) 0.024(6) 0.043(8) 0.005(6) 0.012(5) -0.003(5) N5A 0.010(5) 0.035(6) 0.034(6) 0.010(5) 0.002(4) 0.003(4) O2P 0.050(7) 0.044(6) 0.055(7) 0.005(5) 0.013(5) -0.004(5) N8A 0.023(6) 0.026(6) 0.042(7) 0.003(5) 0.008(5) 0.003(5) N1B 0.015(5) 0.028(6) 0.048(8) 0.000(5) 0.009(5) -0.002(4) N5B 0.027(6) 0.013(5) 0.055(7) -0.016(5) 0.029(5) -0.011(4) C1A 0.011(6) 0.054(9) 0.053(10) 0.01 0.017(6) 0.01 C61B 0.011(6) 0.029(7) 0.033(7) 0.002(6) 0.003(5) -0.001(5) C71A 0.025(7) 0.046(9) 0.065(11) 0.014(8) 0.016(7) 0.008(7) C2A 0.027(7) 0.048(8) 0.030(8) -0.008(7) 0.009(6) 0.003(7) C71B 0.027(7) 0.025(7) 0.048(9) -0.009(6) 0.020(6) -0.007(6) C4B 0.019(6) 0.015(6) 0.044(8) 0.008(5) 0.010(6) 0.004(5) C6B 0.027(7) 0.017(6) 0.044(8) 0.000(6) 0.019(6) -0.005(5) C62A 0.050(9) 0.027(7) 0.042(9) -0.002(6) 0.024(7) 0.009(6) C7A 0.016(6) 0.025(7) 0.056(9) -0.008(6) 0.021(6) -0.004(5) C4AA 0.033(8) 0.037(8) 0.037(8) 0.005(6) 0.014(6) 0.015(6) C4A 0.012(6) 0.038(7) 0.030(7) -0.004(6) 0.008(5) -0.006(6) C6A 0.022(6) 0.020(6) 0.030(7) 0.003(5) 0.000(5) 0.002(5) C8AA 0.018(6) 0.034(7) 0.028(7) -0.006(6) 0.005(5) 0.011(5) C2B 0.026(7) 0.013(6) 0.040(8) 0.001(5) 0.002(6) -0.004(5) C62B 0.029(8) 0.057(10) 0.046(10) 0.010(8) 0.004(7) -0.001(7) C1B 0.027(7) 0.036(8) 0.045(9) 0.01 0.018(6) 0.01 C3A 0.041(9) 0.056(10) 0.035(9) 0.008(7) 0.013(7) 0.007(7) C3B 0.031(8) 0.056(10) 0.042(9) -0.016(7) 0.015(7) -0.003(7) C7B 0.018(6) 0.021(6) 0.050(9) 0.024(6) 0.005(6) 0.005(5) C4AB 0.030(8) 0.024(7) 0.049(9) 0.014(6) 0.020(7) 0.007(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ag2 N61B 2.243(12) . ? Ag2 N61A 2.275(11) . ? Ag2 O5P 2.528(9) . ? Ag2 O1P 2.538(9) . ? Ag2 Ag1 3.2161(14) . ? Ag1 N5B 2.262(10) . ? Ag1 N5A 2.331(10) . ? Ag1 O4A 2.439(9) . ? Ag1 O4B 2.487(9) . ? Cl2 O8P 1.402(9) . ? Cl2 O6P 1.407(9) . ? Cl2 O5P 1.432(9) . ? Cl2 O7P 1.438(9) . ? Cl1 O3P 1.413(9) . ? Cl1 O4P 1.413(10) . ? Cl1 O2P 1.424(11) . ? Cl1 O1P 1.440(10) . ? O2B C2B 1.223(14) . ? O4A C4A 1.186(14) . ? O4B C4B 1.217(14) . ? O61B N61B 1.398(13) . ? O61A N61A 1.404(13) . ? O2A C2A 1.224(16) . ? N3B C4B 1.351(15) . ? N3B C2B 1.352(15) . ? N3B C3B 1.446(16) . ? C61A N61A 1.295(16) . ? C61A C62A 1.446(18) . ? C61A C6A 1.498(17) . ? N8B C8AB 1.309(16) . ? N8B C7B 1.338(16) . ? N3A C4A 1.375(15) . ? N3A C2A 1.384(18) . ? N3A C3A 1.450(17) . ? N1A C2A 1.363(17) . ? N1A C8AA 1.371(15) . ? N1A C1A 1.458(17) . ? N61B C61B 1.271(16) . ? C8AB N1B 1.333(16) . ? C8AB C4AB 1.386(17) . ? N5A C6A 1.321(15) . ? N5A C4AA 1.352(17) . ? N8A C8AA 1.326(16) . ? N8A C7A 1.329(16) . ? N1B C2B 1.387(17) . ? N1B C1B 1.464(16) . ? N5B C6B 1.302(15) . ? N5B C4AB 1.376(18) . ? C1A H1A1 0.96 . ? C1A H1A2 0.96 . ? C1A H1A3 0.96 . ? C61B C62B 1.462(18) . ? C61B C6B 1.507(17) . ? C71A C7A 1.50(2) . ? C71A H71A 0.96 . ? C71A H71B 0.96 . ? C71A H71C 0.96 . ? C71B C7B 1.450(19) . ? C71B H71D 0.96 . ? C71B H71E 0.96 . ? C71B H71F 0.96 . ? C4B C4AB 1.445(19) . ? C6B C7B 1.409(17) . ? C62A H62A 0.96 . ? C62A H62B 0.96 . ? C62A H62C 0.96 . ? C7A C6A 1.377(16) . ? C4AA C8AA 1.337(19) . ? C4AA C4A 1.440(19) . ? C62B H62D 0.96 . ? C62B H62E 0.96 . ? C62B H62F 0.96 . ? C1B H1B1 0.96 . ? C1B H1B2 0.96 . ? C1B H1B3 0.96 . ? C3A H3A1 0.96 . ? C3A H3A2 0.96 . ? C3A H3A3 0.96 . ? C3B H3B1 0.96 . ? C3B H3B2 0.96 . ? C3B H3B3 0.96 . ? 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 N61B Ag2 N61A 143.1(4) . . ? N61B Ag2 O5P 124.3(4) . . ? N61A Ag2 O5P 82.8(3) . . ? N61B Ag2 O1P 99.6(3) . . ? N61A Ag2 O1P 100.7(4) . . ? O5P Ag2 O1P 97.5(3) . . ? N61B Ag2 Ag1 72.7(3) . . ? N61A Ag2 Ag1 71.0(3) . . ? O5P Ag2 Ag1 141.2(2) . . ? O1P Ag2 Ag1 114.8(2) . . ? N5B Ag1 N5A 127.9(3) . . ? N5B Ag1 O4A 115.2(4) . . ? N5A Ag1 O4A 69.9(3) . . ? N5B Ag1 O4B 70.7(4) . . ? N5A Ag1 O4B 120.7(3) . . ? O4A Ag1 O4B 162.6(3) . . ? N5B Ag1 Ag2 67.9(2) . . ? N5A Ag1 Ag2 60.0(2) . . ? O4A Ag1 Ag2 91.6(2) . . ? O4B Ag1 Ag2 105.6(2) . . ? O8P Cl2 O6P 111.5(6) . . ? O8P Cl2 O5P 109.4(6) . . ? O6P Cl2 O5P 110.9(6) . . ? O8P Cl2 O7P 109.4(6) . . ? O6P Cl2 O7P 108.8(6) . . ? O5P Cl2 O7P 106.7(5) . . ? O3P Cl1 O4P 108.7(6) . . ? O3P Cl1 O2P 109.6(7) . . ? O4P Cl1 O2P 109.5(6) . . ? O3P Cl1 O1P 110.2(6) . . ? O4P Cl1 O1P 110.4(6) . . ? O2P Cl1 O1P 108.4(6) . . ? Cl1 O1P Ag2 132.2(6) . . ? Cl2 O5P Ag2 111.8(5) . . ? C4A O4A Ag1 112.8(8) . . ? C4B O4B Ag1 111.5(8) . . ? C4B N3B C2B 126.1(11) . . ? C4B N3B C3B 119.1(10) . . ? C2B N3B C3B 114.8(10) . . ? N61A C61A C62A 124.7(12) . . ? N61A C61A C6A 112.5(12) . . ? C62A C61A C6A 122.5(12) . . ? C8AB N8B C7B 117.8(11) . . ? C61A N61A O61A 111.1(11) . . ? C61A N61A Ag2 123.5(9) . . ? O61A N61A Ag2 124.6(8) . . ? C4A N3A C2A 126.4(12) . . ? C4A N3A C3A 116.5(12) . . ? C2A N3A C3A 117.1(11) . . ? C2A N1A C8AA 122.5(11) . . ? C2A N1A C1A 117.2(11) . . ? C8AA N1A C1A 120.1(11) . . ? C61B N61B O61B 111.7(11) . . ? C61B N61B Ag2 122.9(8) . . ? O61B N61B Ag2 124.5(8) . . ? N8B C8AB N1B 117.9(11) . . ? N8B C8AB C4AB 122.3(12) . . ? N1B C8AB C4AB 119.8(13) . . ? C6A N5A C4AA 118.3(11) . . ? C6A N5A Ag1 125.6(8) . . ? C4AA N5A Ag1 115.6(8) . . ? C8AA N8A C7A 116.1(11) . . ? C8AB N1B C2B 121.1(11) . . ? C8AB N1B C1B 122.7(12) . . ? C2B N1B C1B 116.1(11) . . ? C6B N5B C4AB 115.4(11) . . ? C6B N5B Ag1 126.5(8) . . ? C4AB N5B Ag1 116.0(8) . . ? N1A C1A H1A1 109.5 . . ? N1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? N1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? N61B C61B C62B 126.2(11) . . ? N61B C61B C6B 112.4(11) . . ? C62B C61B C6B 121.5(11) . . ? C7A C71A H71A 109.5 . . ? C7A C71A H71B 109.5 . . ? H71A C71A H71B 109.5 . . ? C7A C71A H71C 109.5 . . ? H71A C71A H71C 109.5 . . ? H71B C71A H71C 109.5 . . ? O2A C2A N1A 122.1(13) . . ? O2A C2A N3A 121.7(13) . . ? N1A C2A N3A 116.2(12) . . ? C7B C71B H71D 109.5 . . ? C7B C71B H71E 109.5 . . ? H71D C71B H71E 109.5 . . ? C7B C71B H71F 109.5 . . ? H71D C71B H71F 109.5 . . ? H71E C71B H71F 109.5 . . ? O4B C4B N3B 123.6(12) . . ? O4B C4B C4AB 122.7(12) . . ? N3B C4B C4AB 113.7(11) . . ? N5B C6B C7B 123.3(12) . . ? N5B C6B C61B 115.4(11) . . ? C7B C6B C61B 120.6(12) . . ? C61A C62A H62A 109.5 . . ? C61A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C61A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? N8A C7A C6A 122.2(13) . . ? N8A C7A C71A 115.3(11) . . ? C6A C7A C71A 122.4(12) . . ? C8AA C4AA N5A 120.0(12) . . ? C8AA C4AA C4A 124.2(13) . . ? N5A C4AA C4A 115.8(12) . . ? O4A C4A N3A 122.1(12) . . ? O4A C4A C4AA 125.6(12) . . ? N3A C4A C4AA 112.0(11) . . ? N5A C6A C7A 119.8(11) . . ? N5A C6A C61A 115.4(10) . . ? C7A C6A C61A 124.8(11) . . ? N8A C8AA C4AA 123.3(12) . . ? N8A C8AA N1A 117.9(12) . . ? C4AA C8AA N1A 118.7(12) . . ? O2B C2B N3B 121.2(12) . . ? O2B C2B N1B 120.9(12) . . ? N3B C2B N1B 117.9(11) . . ? C61B C62B H62D 109.5 . . ? C61B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C61B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N1B C1B H1B1 109.5 . . ? N1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? N1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? N3A C3A H3A1 109.5 . . ? N3A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N3A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N3B C3B H3B1 109.5 . . ? N3B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N3B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N8B C7B C6B 119.8(13) . . ? N8B C7B C71B 118.5(11) . . ? C6B C7B C71B 121.5(12) . . ? N5B C4AB C8AB 120.7(13) . . ? N5B C4AB C4B 117.9(11) . . ? C8AB C4AB C4B 121.3(13) . . ? 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 N61B Ag2 Ag1 N5B -69.2(4) . . . . ? N61A Ag2 Ag1 N5B 104.8(4) . . . . ? O5P Ag2 Ag1 N5B 54.5(5) . . . . ? O1P Ag2 Ag1 N5B -161.9(4) . . . . ? N61B Ag2 Ag1 N5A 113.1(4) . . . . ? N61A Ag2 Ag1 N5A -73.0(4) . . . . ? O5P Ag2 Ag1 N5A -123.3(5) . . . . ? O1P Ag2 Ag1 N5A 20.3(4) . . . . ? N61B Ag2 Ag1 O4A 47.5(3) . . . . ? N61A Ag2 Ag1 O4A -138.6(4) . . . . ? O5P Ag2 Ag1 O4A 171.2(4) . . . . ? O1P Ag2 Ag1 O4A -45.3(3) . . . . ? N61B Ag2 Ag1 O4B -130.2(4) . . . . ? N61A Ag2 Ag1 O4B 43.8(3) . . . . ? O5P Ag2 Ag1 O4B -6.5(4) . . . . ? O1P Ag2 Ag1 O4B 137.1(3) . . . . ? O3P Cl1 O1P Ag2 -136.1(7) . . . . ? O4P Cl1 O1P Ag2 103.7(8) . . . . ? O2P Cl1 O1P Ag2 -16.2(10) . . . . ? N61B Ag2 O1P Cl1 31.4(8) . . . . ? N61A Ag2 O1P Cl1 -179.5(8) . . . . ? O5P Ag2 O1P Cl1 -95.4(8) . . . . ? Ag1 Ag2 O1P Cl1 106.6(7) . . . . ? O8P Cl2 O5P Ag2 162.2(5) . . . . ? O6P Cl2 O5P Ag2 -74.5(6) . . . . ? O7P Cl2 O5P Ag2 43.8(7) . . . . ? N61B Ag2 O5P Cl2 60.5(7) . . . . ? N61A Ag2 O5P Cl2 -92.5(6) . . . . ? O1P Ag2 O5P Cl2 167.6(5) . . . . ? Ag1 Ag2 O5P Cl2 -45.4(7) . . . . ? N5B Ag1 O4A C4A 124.3(9) . . . . ? N5A Ag1 O4A C4A 1.0(8) . . . . ? O4B Ag1 O4A C4A -129.5(11) . . . . ? Ag2 Ag1 O4A C4A 58.1(9) . . . . ? N5B Ag1 O4B C4B -8.7(8) . . . . ? N5A Ag1 O4B C4B 114.5(8) . . . . ? O4A Ag1 O4B C4B -121.7(11) . . . . ? Ag2 Ag1 O4B C4B 50.4(8) . . . . ? C62A C61A N61A O61A 1.0(17) . . . . ? C6A C61A N61A O61A 175.5(10) . . . . ? C62A C61A N61A Ag2 -168.7(9) . . . . ? C6A C61A N61A Ag2 5.8(15) . . . . ? N61B Ag2 N61A C61A 75.0(12) . . . . ? O5P Ag2 N61A C61A -143.7(10) . . . . ? O1P Ag2 N61A C61A -47.4(10) . . . . ? Ag1 Ag2 N61A C61A 65.3(10) . . . . ? N61B Ag2 N61A O61A -93.2(10) . . . . ? O5P Ag2 N61A O61A 48.0(9) . . . . ? O1P Ag2 N61A O61A 144.4(9) . . . . ? Ag1 Ag2 N61A O61A -102.9(9) . . . . ? N61A Ag2 N61B C61B 51.2(13) . . . . ? O5P Ag2 N61B C61B -80.0(11) . . . . ? O1P Ag2 N61B C61B 173.9(10) . . . . ? Ag1 Ag2 N61B C61B 60.8(10) . . . . ? N61A Ag2 N61B O61B -116.5(9) . . . . ? O5P Ag2 N61B O61B 112.3(9) . . . . ? O1P Ag2 N61B O61B 6.2(10) . . . . ? Ag1 Ag2 N61B O61B -106.9(9) . . . . ? C7B N8B C8AB N1B 179.8(10) . . . . ? C7B N8B C8AB C4AB 2.6(17) . . . . ? N5B Ag1 N5A C6A 76.9(12) . . . . ? O4A Ag1 N5A C6A -176.3(11) . . . . ? O4B Ag1 N5A C6A -11.6(12) . . . . ? Ag2 Ag1 N5A C6A 79.5(10) . . . . ? N5B Ag1 N5A C4AA -111.1(9) . . . . ? O4A Ag1 N5A C4AA -4.3(8) . . . . ? O4B Ag1 N5A C4AA 160.4(8) . . . . ? Ag2 Ag1 N5A C4AA -108.5(9) . . . . ? N8B C8AB N1B C2B -174.6(11) . . . . ? C4AB C8AB N1B C2B 2.8(17) . . . . ? N8B C8AB N1B C1B 7.4(17) . . . . ? C4AB C8AB N1B C1B -175.3(11) . . . . ? N5A Ag1 N5B C6B 57.0(12) . . . . ? O4A Ag1 N5B C6B -26.3(11) . . . . ? O4B Ag1 N5B C6B 171.3(11) . . . . ? Ag2 Ag1 N5B C6B 54.6(10) . . . . ? N5A Ag1 N5B C4AB -105.7(8) . . . . ? O4A Ag1 N5B C4AB 171.0(8) . . . . ? O4B Ag1 N5B C4AB 8.7(8) . . . . ? Ag2 Ag1 N5B C4AB -108.1(9) . . . . ? O61B N61B C61B C62B 0.2(19) . . . . ? Ag2 N61B C61B C62B -168.9(11) . . . . ? O61B N61B C61B C6B 178.1(10) . . . . ? Ag2 N61B C61B C6B 9.0(15) . . . . ? C8AA N1A C2A O2A 174.4(12) . . . . ? C1A N1A C2A O2A 0(2) . . . . ? C8AA N1A C2A N3A -4.4(19) . . . . ? C1A N1A C2A N3A -178.4(11) . . . . ? C4A N3A C2A O2A -175.6(13) . . . . ? C3A N3A C2A O2A 7(2) . . . . ? C4A N3A C2A N1A 3.2(19) . . . . ? C3A N3A C2A N1A -174.3(12) . . . . ? Ag1 O4B C4B N3B -173.0(9) . . . . ? Ag1 O4B C4B C4AB 7.8(14) . . . . ? C2B N3B C4B O4B -177.0(12) . . . . ? C3B N3B C4B O4B 3.1(19) . . . . ? C2B N3B C4B C4AB 2.2(17) . . . . ? C3B N3B C4B C4AB -177.6(11) . . . . ? C4AB N5B C6B C7B -9.5(17) . . . . ? Ag1 N5B C6B C7B -172.2(9) . . . . ? C4AB N5B C6B C61B -180.0(10) . . . . ? Ag1 N5B C6B C61B 17.3(16) . . . . ? N61B C61B C6B N5B -77.4(14) . . . . ? C62B C61B C6B N5B 100.6(15) . . . . ? N61B C61B C6B C7B 111.8(13) . . . . ? C62B C61B C6B C7B -70.2(17) . . . . ? C8AA N8A C7A C6A 3.7(18) . . . . ? C8AA N8A C7A C71A -178.5(12) . . . . ? C6A N5A C4AA C8AA 0.8(19) . . . . ? Ag1 N5A C4AA C8AA -171.8(9) . . . . ? C6A N5A C4AA C4A 179.6(11) . . . . ? Ag1 N5A C4AA C4A 7.0(15) . . . . ? Ag1 O4A C4A N3A 175.3(9) . . . . ? Ag1 O4A C4A C4AA 2.5(16) . . . . ? C2A N3A C4A O4A -174.1(12) . . . . ? C3A N3A C4A O4A 3.4(19) . . . . ? C2A N3A C4A C4AA -0.4(18) . . . . ? C3A N3A C4A C4AA 177.1(12) . . . . ? C8AA C4AA C4A O4A 172.0(13) . . . . ? N5A C4AA C4A O4A -7(2) . . . . ? C8AA C4AA C4A N3A -1.4(19) . . . . ? N5A C4AA C4A N3A 179.9(11) . . . . ? C4AA N5A C6A C7A -2.5(18) . . . . ? Ag1 N5A C6A C7A 169.3(8) . . . . ? C4AA N5A C6A C61A 176.1(11) . . . . ? Ag1 N5A C6A C61A -12.2(16) . . . . ? N8A C7A C6A N5A 0.2(19) . . . . ? C71A C7A C6A N5A -177.4(12) . . . . ? N8A C7A C6A C61A -178.2(12) . . . . ? C71A C7A C6A C61A 4(2) . . . . ? N61A C61A C6A N5A -57.4(15) . . . . ? C62A C61A C6A N5A 117.2(14) . . . . ? N61A C61A C6A C7A 121.1(14) . . . . ? C62A C61A C6A C7A -64.3(18) . . . . ? C7A N8A C8AA C4AA -5.6(19) . . . . ? C7A N8A C8AA N1A 179.0(11) . . . . ? N5A C4AA C8AA N8A 3(2) . . . . ? C4A C4AA C8AA N8A -175.2(12) . . . . ? N5A C4AA C8AA N1A 178.9(12) . . . . ? C4A C4AA C8AA N1A 0(2) . . . . ? C2A N1A C8AA N8A 178.6(12) . . . . ? C1A N1A C8AA N8A -7.7(18) . . . . ? C2A N1A C8AA C4AA 2.9(19) . . . . ? C1A N1A C8AA C4AA 176.7(12) . . . . ? C4B N3B C2B O2B 179.4(11) . . . . ? C3B N3B C2B O2B -0.8(17) . . . . ? C4B N3B C2B N1B -0.4(18) . . . . ? C3B N3B C2B N1B 179.4(11) . . . . ? C8AB N1B C2B O2B 177.9(11) . . . . ? C1B N1B C2B O2B -3.9(17) . . . . ? C8AB N1B C2B N3B -2.3(17) . . . . ? C1B N1B C2B N3B 175.9(11) . . . . ? C8AB N8B C7B C6B -2.8(17) . . . . ? C8AB N8B C7B C71B -177.0(11) . . . . ? N5B C6B C7B N8B 6.7(18) . . . . ? C61B C6B C7B N8B 176.8(11) . . . . ? N5B C6B C7B C71B -179.2(12) . . . . ? C61B C6B C7B C71B -9.2(18) . . . . ? C6B N5B C4AB C8AB 9.0(17) . . . . ? Ag1 N5B C4AB C8AB 173.6(9) . . . . ? C6B N5B C4AB C4B -173.3(11) . . . . ? Ag1 N5B C4AB C4B -8.7(14) . . . . ? N8B C8AB C4AB N5B -5.9(18) . . . . ? N1B C8AB C4AB N5B 176.9(11) . . . . ? N8B C8AB C4AB C4B 176.5(11) . . . . ? N1B C8AB C4AB C4B -0.7(18) . . . . ? O4B C4B C4AB N5B -0.1(18) . . . . ? N3B C4B C4AB N5B -179.4(10) . . . . ? O4B C4B C4AB C8AB 177.6(12) . . . . ? N3B C4B C4AB C8AB -1.7(17) . . . . ? # Attachment 'DLMAceMOx.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-06-10 at 12:17:42 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\archivos de programa\wingx\files\archive.dat # CIF files read : import dreduc struct data_DLMAceMOx _database_code_depnum_ccdc_archive 'CCDC 846886' #TrackingRef 'DLMAceMOx.cif' _audit_creation_date 2009-06-10T12:17:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C11 H13 N5 O3' _chemical_formula_sum 'C11 H13 N5 O3' _chemical_formula_weight 263.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.140(3) _cell_length_b 8.3040(15) _cell_length_c 9.365(5) _cell_angle_alpha 94.10(2) _cell_angle_beta 106.43(3) _cell_angle_gamma 110.59(2) _cell_volume 558.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 4 _cell_measurement_theta_max 19 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.08 -1 0 0 0.06 0 1 0 0.2 0 -1 0 0.16 0 0 1 0.05 0 0 -1 0.05 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9443 _exptl_absorpt_correction_T_max 0.9883 _exptl_absorpt_process_details '(SADABS 2.10, 2003)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 77(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0911 _diffrn_reflns_av_unetI/netI 0.0862 _diffrn_reflns_number 14733 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 5.15 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2554 _reflns_number_gt 1200 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1394P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2554 _refine_ls_number_parameters 180 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.175 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2482 _refine_ls_wR_factor_gt 0.183 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.702 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 O 0.4238(3) 0.0571(3) 0.8424(3) 0.0282(6) Uani 1 1 d . . . N1 N 0.3456(4) -0.1425(3) 0.6329(3) 0.0225(7) Uani 1 1 d . . . N5 N 0.6411(4) -0.2712(3) 0.4658(3) 0.0226(7) Uani 1 1 d . . . C4A C 0.5870(5) -0.1940(4) 0.5631(4) 0.0227(8) Uani 1 1 d . . . N8 N 0.2681(4) -0.3387(3) 0.4138(3) 0.0245(7) Uani 1 1 d . . . O4 O 0.8906(3) -0.0455(3) 0.7344(3) 0.0330(7) Uani 1 1 d . . . N3 N 0.6583(4) 0.0065(3) 0.7878(3) 0.0247(7) Uani 1 1 d . . . C4 C 0.7264(5) -0.0757(4) 0.6988(4) 0.0228(8) Uani 1 1 d . . . O61 O 0.5839(4) -0.6600(4) 0.0769(3) 0.0355(7) Uani 1 1 d . . . C8A C 0.4007(5) -0.2267(4) 0.5359(4) 0.0222(8) Uani 1 1 d . . . C6 C 0.5134(5) -0.3821(4) 0.3441(4) 0.0231(8) Uani 1 1 d . . . C2 C 0.4735(5) -0.0216(4) 0.7602(4) 0.0230(8) Uani 1 1 d . . . C7 C 0.3231(5) -0.4185(4) 0.3178(4) 0.0242(8) Uani 1 1 d . . . N61 N 0.4887(4) -0.6081(4) 0.1631(3) 0.0292(8) Uani 1 1 d . . . C61 C 0.5894(5) -0.4554(4) 0.2422(4) 0.0244(8) Uani 1 1 d . . . C3 C 0.7947(5) 0.1265(5) 0.9263(4) 0.0314(9) Uani 1 1 d . . . H3A H 0.8311 0.0604 1.0003 0.047 Uiso 1 1 calc R . . H3B H 0.7408 0.1979 0.9655 0.047 Uiso 1 1 calc R . . H3C H 0.9018 0.2 0.9042 0.047 Uiso 1 1 calc R . . C71 C 0.1696(5) -0.5428(5) 0.1832(4) 0.0318(9) Uani 1 1 d . . . H71A H 0.1535 -0.6609 0.194 0.048 Uiso 1 1 calc R . . H71B H 0.2004 -0.5202 0.0929 0.048 Uiso 1 1 calc R . . H71C H 0.0564 -0.5271 0.176 0.048 Uiso 1 1 calc R . . C1 C 0.1488(5) -0.1795(5) 0.6044(4) 0.0327(9) Uani 1 1 d . . . H1A H 0.1058 -0.1237 0.5237 0.049 Uiso 1 1 calc R . . H1B H 0.1324 -0.1352 0.6946 0.049 Uiso 1 1 calc R . . H1C H 0.0789 -0.3037 0.576 0.049 Uiso 1 1 calc R . . C62 C 0.7754(5) -0.3476(5) 0.2368(4) 0.0365(10) Uani 1 1 d . . . H62A H 0.8627 -0.3971 0.2837 0.055 Uiso 1 1 calc R . . H62B H 0.8147 -0.2303 0.2902 0.055 Uiso 1 1 calc R . . H62C H 0.7694 -0.3455 0.1331 0.055 Uiso 1 1 calc R . . H61 H 0.495(9) -0.777(9) 0.004(8) 0.14(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0297(15) 0.0309(13) 0.0243(13) -0.0028(10) 0.0091(11) 0.0134(11) N1 0.0201(16) 0.0283(16) 0.0203(15) 0.0011(12) 0.0073(13) 0.0109(13) N5 0.0266(17) 0.0209(15) 0.0203(15) 0.0036(12) 0.0090(13) 0.0084(13) C4A 0.025(2) 0.0246(18) 0.0214(18) 0.0055(14) 0.0114(15) 0.0106(15) N8 0.0267(17) 0.0237(15) 0.0209(16) 0.0016(12) 0.0065(14) 0.0088(13) O4 0.0273(16) 0.0383(15) 0.0321(15) 0.0007(11) 0.0109(12) 0.0116(12) N3 0.0254(17) 0.0251(15) 0.0213(15) 0.0001(12) 0.0074(13) 0.0082(13) C4 0.024(2) 0.0252(18) 0.0227(19) 0.0028(14) 0.0101(16) 0.0120(16) O61 0.0417(17) 0.0418(16) 0.0264(14) 0.0003(12) 0.0151(13) 0.0183(14) C8A 0.027(2) 0.0250(18) 0.0168(17) 0.0069(14) 0.0073(15) 0.0115(15) C6 0.032(2) 0.0189(17) 0.0196(18) 0.0050(14) 0.0098(16) 0.0092(15) C2 0.0242(19) 0.0267(18) 0.0235(18) 0.0081(15) 0.0117(16) 0.0125(16) C7 0.026(2) 0.0231(18) 0.0222(19) 0.0049(14) 0.0073(16) 0.0083(15) N61 0.043(2) 0.0262(17) 0.0219(16) 0.0012(13) 0.0150(15) 0.0142(15) C61 0.031(2) 0.0282(19) 0.0182(17) 0.0067(15) 0.0096(16) 0.0144(17) C3 0.031(2) 0.036(2) 0.024(2) -0.0032(16) 0.0098(17) 0.0100(17) C71 0.028(2) 0.036(2) 0.025(2) -0.0005(16) 0.0067(17) 0.0093(17) C1 0.025(2) 0.043(2) 0.033(2) 0.0029(17) 0.0114(17) 0.0163(18) C62 0.032(2) 0.044(2) 0.030(2) -0.0064(17) 0.0108(18) 0.0130(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 C2 1.215(4) . ? N1 C8A 1.369(4) . ? N1 C2 1.380(4) . ? N1 C1 1.460(4) . ? N5 C6 1.316(4) . ? N5 C4A 1.333(4) . ? C4A C8A 1.386(5) . ? C4A C4 1.446(5) . ? N8 C8A 1.334(4) . ? N8 C7 1.341(4) . ? O4 C4 1.208(4) . ? N3 C2 1.381(4) . ? N3 C4 1.383(4) . ? N3 C3 1.459(4) . ? O61 N61 1.406(4) . ? O61 H61 1.03(7) . ? C6 C7 1.413(5) . ? C6 C61 1.477(5) . ? C7 C71 1.494(5) . ? N61 C61 1.273(4) . ? C61 C62 1.481(5) . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C71 H71A 0.96 . ? C71 H71B 0.96 . ? C71 H71C 0.96 . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C62 H62A 0.96 . ? C62 H62B 0.96 . ? C62 H62C 0.96 . ? 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 C8A N1 C2 121.2(3) . . ? C8A N1 C1 120.6(3) . . ? C2 N1 C1 118.2(3) . . ? C6 N5 C4A 118.6(3) . . ? N5 C4A C8A 121.0(3) . . ? N5 C4A C4 118.8(3) . . ? C8A C4A C4 120.2(3) . . ? C8A N8 C7 117.0(3) . . ? C2 N3 C4 125.7(3) . . ? C2 N3 C3 118.0(3) . . ? C4 N3 C3 116.2(3) . . ? O4 C4 N3 120.9(3) . . ? O4 C4 C4A 124.5(3) . . ? N3 C4 C4A 114.6(3) . . ? N61 O61 H61 109(4) . . ? N8 C8A N1 117.2(3) . . ? N8 C8A C4A 121.8(3) . . ? N1 C8A C4A 121.0(3) . . ? N5 C6 C7 120.5(3) . . ? N5 C6 C61 113.9(3) . . ? C7 C6 C61 125.5(3) . . ? O2 C2 N1 120.7(3) . . ? O2 C2 N3 122.2(3) . . ? N1 C2 N3 117.2(3) . . ? N8 C7 C6 121.1(3) . . ? N8 C7 C71 115.0(3) . . ? C6 C7 C71 123.9(3) . . ? C61 N61 O61 110.0(3) . . ? N61 C61 C6 117.3(3) . . ? N61 C61 C62 124.1(3) . . ? C6 C61 C62 118.6(3) . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N5 C4A C8A -1.2(4) . . . . ? C6 N5 C4A C4 178.4(3) . . . . ? C2 N3 C4 O4 -178.2(3) . . . . ? C3 N3 C4 O4 -1.3(5) . . . . ? C2 N3 C4 C4A 2.9(5) . . . . ? C3 N3 C4 C4A 179.8(3) . . . . ? N5 C4A C4 O4 -2.8(5) . . . . ? C8A C4A C4 O4 176.8(3) . . . . ? N5 C4A C4 N3 176.1(3) . . . . ? C8A C4A C4 N3 -4.3(4) . . . . ? C7 N8 C8A N1 178.9(3) . . . . ? C7 N8 C8A C4A -0.2(5) . . . . ? C2 N1 C8A N8 -178.6(3) . . . . ? C1 N1 C8A N8 1.7(4) . . . . ? C2 N1 C8A C4A 0.5(5) . . . . ? C1 N1 C8A C4A -179.2(3) . . . . ? N5 C4A C8A N8 1.5(5) . . . . ? C4 C4A C8A N8 -178.1(3) . . . . ? N5 C4A C8A N1 -177.5(3) . . . . ? C4 C4A C8A N1 2.8(5) . . . . ? C4A N5 C6 C7 -0.2(4) . . . . ? C4A N5 C6 C61 178.2(3) . . . . ? C8A N1 C2 O2 177.3(3) . . . . ? C1 N1 C2 O2 -3.0(4) . . . . ? C8A N1 C2 N3 -2.0(4) . . . . ? C1 N1 C2 N3 177.7(3) . . . . ? C4 N3 C2 O2 -179.1(3) . . . . ? C3 N3 C2 O2 4.1(5) . . . . ? C4 N3 C2 N1 0.2(5) . . . . ? C3 N3 C2 N1 -176.6(3) . . . . ? C8A N8 C7 C6 -1.2(4) . . . . ? C8A N8 C7 C71 179.9(3) . . . . ? N5 C6 C7 N8 1.4(5) . . . . ? C61 C6 C7 N8 -176.8(3) . . . . ? N5 C6 C7 C71 -179.8(3) . . . . ? C61 C6 C7 C71 2.0(5) . . . . ? O61 N61 C61 C6 -178.0(3) . . . . ? O61 N61 C61 C62 2.6(5) . . . . ? N5 C6 C61 N61 150.9(3) . . . . ? C7 C6 C61 N61 -30.8(5) . . . . ? N5 C6 C61 C62 -29.7(4) . . . . ? C7 C6 C61 C62 148.6(3) . . . . ? # Attachment 'Ag_DLMAceMOx_trifluoromethylsulphonato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-02-15 at 08:57:44 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\archivos de programa\wingx\files\archive.dat # CIF files read : import ag_dmlacemox_trifluoromethylsulp dreduc struct data_Ag_DLMAceMOx_trifluoromethylsulphonato _database_code_depnum_ccdc_archive 'CCDC 849559' #TrackingRef 'Ag_DLMAceMOx_trifluoromethylsulphonato.cif' _audit_creation_date 2012-02-15T08:57:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H29 Ag2 F6 N10 O13 S2, C2 H5 O' _chemical_formula_sum 'C28 H34 Ag2 F6 N10 O14 S2' _chemical_formula_weight 1128.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.6665(19) _cell_length_b 15.0893(9) _cell_length_c 19.703(3) _cell_angle_alpha 90 _cell_angle_beta 105.714(10) _cell_angle_gamma 90 _cell_volume 4197.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 239 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -3 3 0.1 -8 3 -1 0.106 -6 7 -2 0.119 -1 8 5 0.128 1 -4 -5 0.058 0 0 -1 0.095 5 6 -1 0.123 -5 1 7 0.096 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6728 _exptl_absorpt_correction_T_max 0.7572 _exptl_absorpt_process_details '(SADABS 2.10, 2003)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_unetI/netI 0.0564 _diffrn_reflns_number 57571 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 9642 _reflns_number_gt 6313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0799P)^2^+10.1684P] 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_number_reflns 9642 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.131 _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 _refine_diff_density_max 1.539 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.165 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' S S 0.1246 0.1234 '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' 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 0.54756(3) 0.48853(3) 0.23244(2) 0.02676(12) Uani 1 1 d . . . Ag2 Ag 0.49866(3) 0.66466(3) 0.27636(2) 0.02671(12) Uani 1 1 d . . . S1Y S 0.29507(10) 0.71151(10) 0.32342(8) 0.0318(3) Uani 1 1 d . . . S1X S 0.65626(11) 0.83468(10) 0.22089(9) 0.0399(4) Uani 1 1 d . . . O61A O 0.4517(3) 0.6918(2) 0.10923(19) 0.0268(8) Uani 1 1 d . . . O1R O 0.5857(3) 0.3556(3) 0.1792(2) 0.0341(9) Uani 1 1 d . . . O2A O 0.2868(3) 0.2864(3) 0.4198(2) 0.0357(9) Uani 1 1 d . . . O2Y O 0.3151(3) 0.6208(3) 0.3456(2) 0.0408(10) Uani 1 1 d . . . O1X O 0.5710(3) 0.7831(3) 0.2150(2) 0.0422(10) Uani 1 1 d . . . F2Y F 0.2504(3) 0.8494(2) 0.3887(2) 0.0538(10) Uani 1 1 d . . . O3Y O 0.2099(3) 0.7253(3) 0.2680(2) 0.0407(10) Uani 1 1 d . . . O1Y O 0.3782(3) 0.7584(3) 0.3162(2) 0.0407(10) Uani 1 1 d . . . F3Y F 0.1948(3) 0.7258(3) 0.4147(2) 0.0572(11) Uani 1 1 d . . . O3X O 0.6564(4) 0.9213(3) 0.2502(3) 0.0508(12) Uani 1 1 d . . . F1Y F 0.3428(3) 0.7564(3) 0.45641(19) 0.0548(11) Uani 1 1 d . . . O4B O 0.6319(3) 0.5614(3) 0.15349(19) 0.0334(9) Uani 1 1 d . . . O61B O 0.4881(3) 0.5673(3) 0.41717(19) 0.0300(9) Uani 1 1 d . . . O4A O 0.5200(3) 0.3875(2) 0.32769(19) 0.0286(8) Uani 1 1 d . . . N3A N 0.4030(3) 0.3383(3) 0.3748(2) 0.0246(9) Uani 1 1 d . . . N5A N 0.3875(3) 0.4881(3) 0.2283(2) 0.0213(9) Uani 1 1 d . . . O2B O 0.9325(3) 0.6329(3) 0.1521(2) 0.0449(11) Uani 1 1 d . . . N1B N 0.9013(3) 0.6286(3) 0.2589(2) 0.0263(10) Uani 1 1 d . . . N1A N 0.2429(3) 0.3819(3) 0.3278(2) 0.0233(9) Uani 1 1 d . . . N3B N 0.7806(3) 0.6018(3) 0.1525(2) 0.0276(10) Uani 1 1 d . . . N8B N 0.8655(3) 0.6258(3) 0.3672(2) 0.0259(10) Uani 1 1 d . . . N5B N 0.6817(3) 0.5723(3) 0.2995(2) 0.0221(9) Uani 1 1 d . . . N8A N 0.1996(3) 0.4813(3) 0.2335(2) 0.0254(10) Uani 1 1 d . . . N61B N 0.5534(3) 0.5936(3) 0.3807(2) 0.0232(9) Uani 1 1 d . . . N61A N 0.4216(3) 0.6444(3) 0.1593(2) 0.0226(9) Uani 1 1 d . . . F3X F 0.6387(4) 0.7791(3) 0.0921(3) 0.0776(15) Uani 1 1 d . . . O2X O 0.7417(3) 0.7846(3) 0.2462(3) 0.0694(17) Uani 1 1 d . . . F1X F 0.5810(5) 0.9075(3) 0.0990(3) 0.0991(19) Uani 1 1 d . . . C8AB C 0.8380(4) 0.6143(3) 0.2974(3) 0.0228(11) Uani 1 1 d . . . C62B C 0.6595(4) 0.5028(4) 0.4721(3) 0.0311(13) Uani 1 1 d . . . H62A H 0.6049 0.497 0.4897 0.047 Uiso 1 1 calc R . . H62B H 0.7107 0.5281 0.508 0.047 Uiso 1 1 calc R . . H62C H 0.6779 0.4455 0.4593 0.047 Uiso 1 1 calc R . . C61B C 0.6364(4) 0.5618(4) 0.4087(3) 0.0258(11) Uani 1 1 d . . . C61A C 0.3514(4) 0.5922(3) 0.1327(3) 0.0230(11) Uani 1 1 d . . . C62A C 0.3065(4) 0.5857(4) 0.0558(3) 0.0274(12) Uani 1 1 d . . . H62D H 0.3358 0.6272 0.0314 0.041 Uiso 1 1 calc R . . H62E H 0.2402 0.5989 0.0463 0.041 Uiso 1 1 calc R . . H62F H 0.3143 0.5267 0.0401 0.041 Uiso 1 1 calc R . . C7A C 0.2257(4) 0.5311(3) 0.1863(3) 0.0254(11) Uani 1 1 d . . . C2A C 0.3087(4) 0.3331(3) 0.3763(3) 0.0273(12) Uani 1 1 d . . . C6B C 0.7093(4) 0.5833(3) 0.3699(3) 0.0226(11) Uani 1 1 d . . . C8AA C 0.2685(4) 0.4344(3) 0.2785(3) 0.0243(11) Uani 1 1 d . . . F2X F 0.7302(5) 0.8917(4) 0.1225(3) 0.113(2) Uani 1 1 d . . . C4A C 0.4359(4) 0.3867(3) 0.3266(3) 0.0256(11) Uani 1 1 d . . . C7B C 0.8021(4) 0.6113(3) 0.4039(3) 0.0262(11) Uani 1 1 d . . . C1A C 0.1432(4) 0.3793(4) 0.3278(3) 0.0324(13) Uani 1 1 d . . . H1A1 H 0.1069 0.4169 0.2911 0.049 Uiso 1 1 calc R . . H1A2 H 0.1371 0.3996 0.3726 0.049 Uiso 1 1 calc R . . H1A3 H 0.1201 0.3196 0.3199 0.049 Uiso 1 1 calc R . . C71A C 0.1491(4) 0.5846(4) 0.1384(3) 0.0335(13) Uani 1 1 d . . . H71A H 0.0898 0.5722 0.1484 0.05 Uiso 1 1 calc R . . H71B H 0.1447 0.5694 0.0903 0.05 Uiso 1 1 calc R . . H71C H 0.1635 0.6465 0.1457 0.05 Uiso 1 1 calc R . . C3A C 0.4739(4) 0.2900(4) 0.4297(3) 0.0298(12) Uani 1 1 d . . . H3A1 H 0.4427 0.259 0.4596 0.045 Uiso 1 1 calc R . . H3A2 H 0.5186 0.3313 0.4573 0.045 Uiso 1 1 calc R . . H3A3 H 0.5065 0.2483 0.4078 0.045 Uiso 1 1 calc R . . C6A C 0.3201(4) 0.5351(3) 0.1838(3) 0.0221(11) Uani 1 1 d . . . C4AA C 0.3621(4) 0.4365(3) 0.2764(3) 0.0238(11) Uani 1 1 d . . . C2B C 0.8762(4) 0.6219(4) 0.1866(3) 0.0289(12) Uani 1 1 d . . . C4B C 0.7123(4) 0.5828(3) 0.1863(3) 0.0233(11) Uani 1 1 d . . . C2R C 0.4933(5) 0.3962(5) 0.0635(3) 0.0482(17) Uani 1 1 d . . . H2R1 H 0.4925 0.3961 0.0146 0.072 Uiso 1 1 calc R . . H2R2 H 0.4889 0.4561 0.0788 0.072 Uiso 1 1 calc R . . H2R3 H 0.4405 0.3626 0.0696 0.072 Uiso 1 1 calc R . . C71B C 0.8374(4) 0.6282(5) 0.4810(3) 0.0375(14) Uani 1 1 d . . . H71D H 0.9024 0.6467 0.4922 0.056 Uiso 1 1 calc R . . H71E H 0.8325 0.5748 0.5064 0.056 Uiso 1 1 calc R . . H71F H 0.8 0.6739 0.4942 0.056 Uiso 1 1 calc R . . C1R C 0.5829(5) 0.3559(4) 0.1060(3) 0.0416(15) Uani 1 1 d . . . H1R1 H 0.5878 0.2956 0.0902 0.05 Uiso 1 1 calc R . . H1R2 H 0.6363 0.3893 0.0993 0.05 Uiso 1 1 calc R . . C4AB C 0.7441(4) 0.5901(3) 0.2628(3) 0.0223(11) Uani 1 1 d . . . C1B C 1.0017(4) 0.6502(5) 0.2935(3) 0.0402(15) Uani 1 1 d . . . H05A H 1.0351 0.6581 0.2583 0.06 Uiso 1 1 calc R . . H05B H 1.03 0.6027 0.3244 0.06 Uiso 1 1 calc R . . H05C H 1.0049 0.7039 0.3202 0.06 Uiso 1 1 calc R . . O1S O 0.5655(5) 0.9779(6) 0.4615(3) 0.105(3) Uani 1 1 d . . . C3B C 0.7564(5) 0.5997(5) 0.0754(3) 0.0419(15) Uani 1 1 d . . . H05D H 0.8113 0.6144 0.06 0.063 Uiso 1 1 calc R . . H05E H 0.7071 0.642 0.0565 0.063 Uiso 1 1 calc R . . H05F H 0.7348 0.5415 0.059 0.063 Uiso 1 1 calc R . . C1Y C 0.2693(4) 0.7640(4) 0.3993(3) 0.0368(14) Uani 1 1 d . . . C1S C 0.5319(7) 0.9064(6) 0.4108(5) 0.087(3) Uani 1 1 d . . . H1S1 H 0.5062 0.9324 0.3645 0.105 Uiso 1 1 calc R . . H1S2 H 0.4806 0.8759 0.4234 0.105 Uiso 1 1 calc R . . C1X C 0.6500(6) 0.8549(5) 0.1284(5) 0.061(2) Uani 1 1 d . . . C2S C 0.6054(7) 0.8399(6) 0.4063(5) 0.078(3) Uani 1 1 d . . . H2S1 H 0.5773 0.7952 0.3724 0.118 Uiso 1 1 calc R . . H2S2 H 0.6307 0.8128 0.4516 0.118 Uiso 1 1 calc R . . H2S3 H 0.6555 0.8688 0.392 0.118 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 0.0227(2) 0.0295(2) 0.0287(2) 0.00044(17) 0.00805(16) -0.00199(17) Ag2 0.0263(2) 0.0302(2) 0.0230(2) 0.00009(17) 0.00543(16) -0.00014(17) S1Y 0.0289(7) 0.0335(8) 0.0317(7) -0.0015(6) 0.0057(6) -0.0023(6) S1X 0.0335(8) 0.0259(7) 0.0541(10) 0.0046(7) 0.0012(7) -0.0063(6) O61A 0.028(2) 0.0286(19) 0.0257(19) 0.0080(16) 0.0102(15) -0.0033(16) O1R 0.034(2) 0.036(2) 0.031(2) 0.0007(17) 0.0061(17) 0.0072(18) O2A 0.043(2) 0.034(2) 0.036(2) 0.0080(18) 0.0207(19) 0.0023(19) O2Y 0.039(3) 0.036(2) 0.047(3) -0.007(2) 0.012(2) 0.0000(19) O1X 0.041(3) 0.038(2) 0.045(2) 0.001(2) 0.007(2) -0.011(2) F2Y 0.073(3) 0.041(2) 0.051(2) -0.0026(18) 0.023(2) 0.017(2) O3Y 0.034(2) 0.050(3) 0.033(2) 0.001(2) 0.0005(18) -0.001(2) O1Y 0.036(2) 0.040(2) 0.047(3) -0.004(2) 0.014(2) -0.0056(19) F3Y 0.055(3) 0.072(3) 0.051(2) 0.000(2) 0.026(2) -0.009(2) O3X 0.063(3) 0.024(2) 0.061(3) 0.000(2) 0.009(2) -0.008(2) F1Y 0.055(3) 0.070(3) 0.033(2) -0.0091(19) 0.0019(17) 0.018(2) O4B 0.035(2) 0.040(2) 0.025(2) -0.0033(17) 0.0074(17) -0.0116(18) O61B 0.028(2) 0.040(2) 0.0261(19) 0.0033(17) 0.0142(16) -0.0030(17) O4A 0.024(2) 0.034(2) 0.0265(19) 0.0019(16) 0.0043(15) -0.0028(16) N3A 0.025(2) 0.023(2) 0.026(2) 0.0034(18) 0.0072(18) -0.0008(18) N5A 0.021(2) 0.021(2) 0.021(2) -0.0017(17) 0.0054(17) -0.0024(17) O2B 0.033(2) 0.072(3) 0.035(2) 0.012(2) 0.0197(19) 0.006(2) N1B 0.018(2) 0.029(2) 0.034(2) 0.001(2) 0.0090(18) -0.0018(18) N1A 0.021(2) 0.024(2) 0.027(2) 0.0022(18) 0.0115(18) -0.0040(18) N3B 0.031(3) 0.030(2) 0.023(2) -0.0015(19) 0.0100(19) -0.004(2) N8B 0.020(2) 0.027(2) 0.030(2) -0.001(2) 0.0063(18) -0.0016(18) N5B 0.020(2) 0.023(2) 0.024(2) 0.0023(18) 0.0064(17) 0.0010(17) N8A 0.023(2) 0.028(2) 0.027(2) -0.0011(19) 0.0095(18) 0.0007(19) N61B 0.024(2) 0.025(2) 0.024(2) 0.0010(18) 0.0128(18) -0.0001(18) N61A 0.024(2) 0.023(2) 0.022(2) 0.0042(18) 0.0085(17) 0.0010(18) F3X 0.108(4) 0.062(3) 0.075(3) -0.021(3) 0.046(3) -0.035(3) O2X 0.037(3) 0.035(3) 0.115(5) -0.002(3) -0.015(3) -0.004(2) F1X 0.147(6) 0.065(3) 0.069(3) 0.027(3) 0.002(3) 0.010(3) C8AB 0.022(3) 0.018(2) 0.028(3) 0.001(2) 0.006(2) 0.001(2) C62B 0.032(3) 0.035(3) 0.028(3) 0.005(2) 0.010(2) 0.001(2) C61B 0.028(3) 0.027(3) 0.023(3) -0.005(2) 0.008(2) -0.004(2) C61A 0.022(3) 0.024(3) 0.023(3) 0.000(2) 0.007(2) 0.002(2) C62A 0.024(3) 0.030(3) 0.027(3) 0.001(2) 0.005(2) -0.005(2) C7A 0.022(3) 0.023(3) 0.030(3) 0.000(2) 0.005(2) -0.002(2) C2A 0.032(3) 0.025(3) 0.026(3) -0.001(2) 0.010(2) -0.003(2) C6B 0.023(3) 0.019(2) 0.025(3) 0.002(2) 0.005(2) 0.001(2) C8AA 0.028(3) 0.023(3) 0.023(3) -0.001(2) 0.008(2) -0.001(2) F2X 0.150(6) 0.086(4) 0.136(5) -0.036(4) 0.095(5) -0.078(4) C4A 0.032(3) 0.018(2) 0.025(3) -0.004(2) 0.005(2) 0.000(2) C7B 0.030(3) 0.024(3) 0.025(3) 0.000(2) 0.009(2) 0.003(2) C1A 0.030(3) 0.041(3) 0.029(3) 0.007(3) 0.013(2) -0.002(3) C71A 0.025(3) 0.043(3) 0.034(3) 0.005(3) 0.010(2) 0.003(3) C3A 0.036(3) 0.028(3) 0.024(3) 0.005(2) 0.006(2) 0.000(2) C6A 0.023(3) 0.022(3) 0.021(2) -0.002(2) 0.006(2) -0.004(2) C4AA 0.033(3) 0.019(3) 0.020(2) -0.001(2) 0.008(2) -0.006(2) C2B 0.030(3) 0.032(3) 0.029(3) 0.004(2) 0.014(2) 0.002(2) C4B 0.027(3) 0.019(2) 0.025(3) -0.001(2) 0.008(2) -0.002(2) C2R 0.045(4) 0.059(4) 0.038(4) 0.004(3) 0.005(3) -0.005(3) C71B 0.032(3) 0.052(4) 0.028(3) -0.004(3) 0.007(2) -0.008(3) C1R 0.048(4) 0.036(3) 0.043(4) -0.003(3) 0.015(3) 0.006(3) C4AB 0.028(3) 0.013(2) 0.027(3) -0.002(2) 0.011(2) -0.002(2) C1B 0.022(3) 0.057(4) 0.042(3) -0.002(3) 0.011(3) -0.012(3) O1S 0.064(4) 0.180(8) 0.076(4) -0.057(5) 0.027(3) -0.045(5) C3B 0.050(4) 0.055(4) 0.024(3) 0.005(3) 0.015(3) -0.005(3) C1Y 0.036(3) 0.037(3) 0.036(3) 0.005(3) 0.006(3) 0.008(3) C1S 0.085(7) 0.064(6) 0.083(6) 0.004(5) -0.028(5) -0.019(5) C1X 0.071(6) 0.046(4) 0.069(5) -0.004(4) 0.027(4) -0.028(4) C2S 0.091(7) 0.066(6) 0.057(5) 0.006(4) -0.015(5) -0.015(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N5A 2.327(4) . ? Ag1 O1R 2.399(4) . ? Ag1 N5B 2.409(4) . ? Ag1 O4B 2.490(4) . ? Ag1 O4A 2.534(4) . ? Ag1 Ag2 2.9432(6) . ? Ag2 N61B 2.264(4) . ? Ag2 N61A 2.297(4) . ? Ag2 O1X 2.545(4) . ? Ag2 O1Y 2.548(4) . ? S1Y O3Y 1.434(4) . ? S1Y O2Y 1.442(4) . ? S1Y O1Y 1.449(4) . ? S1Y C1Y 1.819(6) . ? S1X O3X 1.429(5) . ? S1X O2X 1.432(5) . ? S1X O1X 1.450(4) . ? S1X C1X 1.826(9) . ? O61A N61A 1.385(5) . ? O1R C1R 1.432(7) . ? O2A C2A 1.218(6) . ? F2Y C1Y 1.323(7) . ? F3Y C1Y 1.341(7) . ? F1Y C1Y 1.337(7) . ? O4B C4B 1.225(6) . ? O61B N61B 1.402(5) . ? O4A C4A 1.227(6) . ? N3A C4A 1.384(7) . ? N3A C2A 1.394(7) . ? N3A C3A 1.474(7) . ? N5A C6A 1.334(6) . ? N5A C4AA 1.354(6) . ? O2B C2B 1.214(6) . ? N1B C8AB 1.367(7) . ? N1B C2B 1.376(7) . ? N1B C1B 1.481(7) . ? N1A C2A 1.374(7) . ? N1A C8AA 1.381(6) . ? N1A C1A 1.463(7) . ? N3B C4B 1.374(6) . ? N3B C2B 1.414(7) . ? N3B C3B 1.465(7) . ? N8B C8AB 1.336(7) . ? N8B C7B 1.340(7) . ? N5B C4AB 1.339(6) . ? N5B C6B 1.345(6) . ? N8A C7A 1.330(7) . ? N8A C8AA 1.350(7) . ? N61B C61B 1.286(7) . ? N61A C61A 1.290(7) . ? F3X C1X 1.334(9) . ? F1X C1X 1.294(10) . ? C8AB C4AB 1.409(7) . ? C62B C61B 1.496(8) . ? C62B H62A 0.96 . ? C62B H62B 0.96 . ? C62B H62C 0.96 . ? C61B C6B 1.508(7) . ? C61A C62A 1.482(7) . ? C61A C6A 1.488(7) . ? C62A H62D 0.96 . ? C62A H62E 0.96 . ? C62A H62F 0.96 . ? C7A C6A 1.401(7) . ? C7A C71A 1.494(7) . ? C6B C7B 1.409(7) . ? C8AA C4AA 1.385(7) . ? F2X C1X 1.333(9) . ? C4A C4AA 1.461(7) . ? C7B C71B 1.488(7) . ? C1A H1A1 0.96 . ? C1A H1A2 0.96 . ? C1A H1A3 0.96 . ? C71A H71A 0.96 . ? C71A H71B 0.96 . ? C71A H71C 0.96 . ? C3A H3A1 0.96 . ? C3A H3A2 0.96 . ? C3A H3A3 0.96 . ? C4B C4AB 1.457(7) . ? C2R C1R 1.484(9) . ? C2R H2R1 0.96 . ? C2R H2R2 0.96 . ? C2R H2R3 0.96 . ? C71B H71D 0.96 . ? C71B H71E 0.96 . ? C71B H71F 0.96 . ? C1R H1R1 0.97 . ? C1R H1R2 0.97 . ? C1B H05A 0.96 . ? C1B H05B 0.96 . ? C1B H05C 0.96 . ? O1S C1S 1.462(10) . ? C3B H05D 0.96 . ? C3B H05E 0.96 . ? C3B H05F 0.96 . ? C1S C2S 1.494(13) . ? C1S H1S1 0.97 . ? C1S H1S2 0.97 . ? C2S H2S1 0.96 . ? C2S H2S2 0.96 . ? C2S H2S3 0.96 . ? 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 N5A Ag1 O1R 109.58(14) . . ? N5A Ag1 N5B 133.35(14) . . ? O1R Ag1 N5B 115.22(14) . . ? N5A Ag1 O4B 130.28(14) . . ? O1R Ag1 O4B 83.22(13) . . ? N5B Ag1 O4B 68.99(13) . . ? N5A Ag1 O4A 70.26(13) . . ? O1R Ag1 O4A 85.62(13) . . ? N5B Ag1 O4A 100.33(13) . . ? O4B Ag1 O4A 159.11(13) . . ? N5A Ag1 Ag2 71.86(10) . . ? O1R Ag1 Ag2 171.07(9) . . ? N5B Ag1 Ag2 65.97(10) . . ? O4B Ag1 Ag2 89.24(10) . . ? O4A Ag1 Ag2 103.00(9) . . ? N61B Ag2 N61A 143.65(15) . . ? N61B Ag2 O1X 132.29(15) . . ? N61A Ag2 O1X 76.82(14) . . ? N61B Ag2 O1Y 95.05(14) . . ? N61A Ag2 O1Y 100.94(15) . . ? O1X Ag2 O1Y 99.76(14) . . ? N61B Ag2 Ag1 77.56(11) . . ? N61A Ag2 Ag1 71.17(11) . . ? O1X Ag2 Ag1 109.18(10) . . ? O1Y Ag2 Ag1 146.77(10) . . ? O3Y S1Y O2Y 115.6(3) . . ? O3Y S1Y O1Y 115.9(3) . . ? O2Y S1Y O1Y 112.7(3) . . ? O3Y S1Y C1Y 103.3(3) . . ? O2Y S1Y C1Y 103.6(3) . . ? O1Y S1Y C1Y 103.6(3) . . ? O3X S1X O2X 115.9(3) . . ? O3X S1X O1X 115.4(3) . . ? O2X S1X O1X 113.5(3) . . ? O3X S1X C1X 104.2(3) . . ? O2X S1X C1X 103.8(4) . . ? O1X S1X C1X 101.6(3) . . ? C1R O1R Ag1 119.4(3) . . ? S1X O1X Ag2 143.1(3) . . ? S1Y O1Y Ag2 115.5(2) . . ? C4B O4B Ag1 111.0(3) . . ? C4A O4A Ag1 110.7(3) . . ? C4A N3A C2A 125.2(4) . . ? C4A N3A C3A 117.2(4) . . ? C2A N3A C3A 117.6(4) . . ? C6A N5A C4AA 118.1(4) . . ? C6A N5A Ag1 125.6(3) . . ? C4AA N5A Ag1 116.3(3) . . ? C8AB N1B C2B 122.1(5) . . ? C8AB N1B C1B 121.3(5) . . ? C2B N1B C1B 116.5(4) . . ? C2A N1A C8AA 121.5(4) . . ? C2A N1A C1A 119.9(4) . . ? C8AA N1A C1A 118.6(4) . . ? C4B N3B C2B 125.0(4) . . ? C4B N3B C3B 119.6(5) . . ? C2B N3B C3B 115.4(5) . . ? C8AB N8B C7B 118.3(5) . . ? C4AB N5B C6B 118.2(4) . . ? C4AB N5B Ag1 112.6(3) . . ? C6B N5B Ag1 127.1(3) . . ? C7A N8A C8AA 116.7(4) . . ? C61B N61B O61B 111.9(4) . . ? C61B N61B Ag2 128.9(3) . . ? O61B N61B Ag2 118.4(3) . . ? C61A N61A O61A 113.5(4) . . ? C61A N61A Ag2 127.7(3) . . ? O61A N61A Ag2 118.8(3) . . ? N8B C8AB N1B 119.4(5) . . ? N8B C8AB C4AB 121.0(5) . . ? N1B C8AB C4AB 119.6(5) . . ? C61B C62B H62A 109.5 . . ? C61B C62B H62B 109.5 . . ? H62A C62B H62B 109.5 . . ? C61B C62B H62C 109.5 . . ? H62A C62B H62C 109.5 . . ? H62B C62B H62C 109.5 . . ? N61B C61B C62B 123.7(5) . . ? N61B C61B C6B 114.9(5) . . ? C62B C61B C6B 121.3(5) . . ? N61A C61A C62A 122.8(5) . . ? N61A C61A C6A 115.9(4) . . ? C62A C61A C6A 121.3(4) . . ? C61A C62A H62D 109.5 . . ? C61A C62A H62E 109.5 . . ? H62D C62A H62E 109.5 . . ? C61A C62A H62F 109.5 . . ? H62D C62A H62F 109.5 . . ? H62E C62A H62F 109.5 . . ? N8A C7A C6A 121.6(5) . . ? N8A C7A C71A 116.0(5) . . ? C6A C7A C71A 122.4(5) . . ? O2A C2A N1A 122.0(5) . . ? O2A C2A N3A 120.0(5) . . ? N1A C2A N3A 118.0(4) . . ? N5B C6B C7B 120.6(5) . . ? N5B C6B C61B 116.0(4) . . ? C7B C6B C61B 123.3(4) . . ? N8A C8AA N1A 117.7(5) . . ? N8A C8AA C4AA 122.7(5) . . ? N1A C8AA C4AA 119.6(5) . . ? O4A C4A N3A 121.9(5) . . ? O4A C4A C4AA 124.4(5) . . ? N3A C4A C4AA 113.8(5) . . ? N8B C7B C6B 121.0(5) . . ? N8B C7B C71B 115.0(5) . . ? C6B C7B C71B 124.1(5) . . ? N1A C1A H1A1 109.5 . . ? N1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? N1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C7A C71A H71A 109.5 . . ? C7A C71A H71B 109.5 . . ? H71A C71A H71B 109.5 . . ? C7A C71A H71C 109.5 . . ? H71A C71A H71C 109.5 . . ? H71B C71A H71C 109.5 . . ? N3A C3A H3A1 109.5 . . ? N3A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N3A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N5A C6A C7A 121.1(5) . . ? N5A C6A C61A 116.4(4) . . ? C7A C6A C61A 122.6(5) . . ? N5A C4AA C8AA 119.8(5) . . ? N5A C4AA C4A 118.4(5) . . ? C8AA C4AA C4A 121.8(5) . . ? O2B C2B N1B 122.6(5) . . ? O2B C2B N3B 120.0(5) . . ? N1B C2B N3B 117.4(4) . . ? O4B C4B N3B 121.6(5) . . ? O4B C4B C4AB 123.9(5) . . ? N3B C4B C4AB 114.5(5) . . ? C1R C2R H2R1 109.5 . . ? C1R C2R H2R2 109.5 . . ? H2R1 C2R H2R2 109.5 . . ? C1R C2R H2R3 109.5 . . ? H2R1 C2R H2R3 109.5 . . ? H2R2 C2R H2R3 109.5 . . ? C7B C71B H71D 109.5 . . ? C7B C71B H71E 109.5 . . ? H71D C71B H71E 109.5 . . ? C7B C71B H71F 109.5 . . ? H71D C71B H71F 109.5 . . ? H71E C71B H71F 109.5 . . ? O1R C1R C2R 110.4(5) . . ? O1R C1R H1R1 109.6 . . ? C2R C1R H1R1 109.6 . . ? O1R C1R H1R2 109.6 . . ? C2R C1R H1R2 109.6 . . ? H1R1 C1R H1R2 108.1 . . ? N5B C4AB C8AB 120.8(5) . . ? N5B C4AB C4B 118.1(5) . . ? C8AB C4AB C4B 121.1(5) . . ? N1B C1B H05A 109.5 . . ? N1B C1B H05B 109.5 . . ? H05A C1B H05B 109.5 . . ? N1B C1B H05C 109.5 . . ? H05A C1B H05C 109.5 . . ? H05B C1B H05C 109.5 . . ? N3B C3B H05D 109.5 . . ? N3B C3B H05E 109.5 . . ? H05D C3B H05E 109.5 . . ? N3B C3B H05F 109.5 . . ? H05D C3B H05F 109.5 . . ? H05E C3B H05F 109.5 . . ? F2Y C1Y F1Y 107.6(5) . . ? F2Y C1Y F3Y 107.8(5) . . ? F1Y C1Y F3Y 107.0(5) . . ? F2Y C1Y S1Y 112.1(4) . . ? F1Y C1Y S1Y 110.8(4) . . ? F3Y C1Y S1Y 111.3(4) . . ? O1S C1S C2S 114.9(8) . . ? O1S C1S H1S1 108.5 . . ? C2S C1S H1S1 108.5 . . ? O1S C1S H1S2 108.5 . . ? C2S C1S H1S2 108.5 . . ? H1S1 C1S H1S2 107.5 . . ? F1X C1X F2X 107.8(7) . . ? F1X C1X F3X 108.5(7) . . ? F2X C1X F3X 107.2(7) . . ? F1X C1X S1X 111.7(6) . . ? F2X C1X S1X 110.4(6) . . ? F3X C1X S1X 110.9(5) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5A Ag1 Ag2 N61B 94.30(15) . . . . ? O1R Ag1 Ag2 N61B -164.9(6) . . . . ? N5B Ag1 Ag2 N61B -65.23(15) . . . . ? O4B Ag1 Ag2 N61B -132.49(14) . . . . ? O4A Ag1 Ag2 N61B 30.43(14) . . . . ? N5A Ag1 Ag2 N61A -66.89(15) . . . . ? O1R Ag1 Ag2 N61A 33.9(6) . . . . ? N5B Ag1 Ag2 N61A 133.58(15) . . . . ? O4B Ag1 Ag2 N61A 66.33(14) . . . . ? O4A Ag1 Ag2 N61A -130.76(14) . . . . ? N5A Ag1 Ag2 O1X -134.94(15) . . . . ? O1R Ag1 Ag2 O1X -34.1(6) . . . . ? N5B Ag1 Ag2 O1X 65.52(15) . . . . ? O4B Ag1 Ag2 O1X -1.73(13) . . . . ? O4A Ag1 Ag2 O1X 161.18(13) . . . . ? N5A Ag1 Ag2 O1Y 14.2(2) . . . . ? O1R Ag1 Ag2 O1Y 115.0(7) . . . . ? N5B Ag1 Ag2 O1Y -145.3(2) . . . . ? O4B Ag1 Ag2 O1Y 147.4(2) . . . . ? O4A Ag1 Ag2 O1Y -49.7(2) . . . . ? N5A Ag1 O1R C1R 93.3(4) . . . . ? N5B Ag1 O1R C1R -100.1(4) . . . . ? O4B Ag1 O1R C1R -37.2(4) . . . . ? O4A Ag1 O1R C1R 160.5(4) . . . . ? Ag2 Ag1 O1R C1R -4.5(9) . . . . ? O3X S1X O1X Ag2 -96.6(5) . . . . ? O2X S1X O1X Ag2 40.6(6) . . . . ? C1X S1X O1X Ag2 151.4(5) . . . . ? N61B Ag2 O1X S1X 3.4(6) . . . . ? N61A Ag2 O1X S1X -151.5(5) . . . . ? O1Y Ag2 O1X S1X 109.5(5) . . . . ? Ag1 Ag2 O1X S1X -87.1(5) . . . . ? O3Y S1Y O1Y Ag2 -103.6(3) . . . . ? O2Y S1Y O1Y Ag2 32.7(3) . . . . ? C1Y S1Y O1Y Ag2 144.0(3) . . . . ? N61B Ag2 O1Y S1Y -73.4(3) . . . . ? N61A Ag2 O1Y S1Y 73.8(3) . . . . ? O1X Ag2 O1Y S1Y 152.1(3) . . . . ? Ag1 Ag2 O1Y S1Y 1.6(4) . . . . ? N5A Ag1 O4B C4B 148.3(3) . . . . ? O1R Ag1 O4B C4B -101.7(4) . . . . ? N5B Ag1 O4B C4B 18.6(3) . . . . ? O4A Ag1 O4B C4B -43.5(6) . . . . ? Ag2 Ag1 O4B C4B 83.1(4) . . . . ? N5A Ag1 O4A C4A -0.3(3) . . . . ? O1R Ag1 O4A C4A -112.9(3) . . . . ? N5B Ag1 O4A C4A 132.2(3) . . . . ? O4B Ag1 O4A C4A -170.7(4) . . . . ? Ag2 Ag1 O4A C4A 64.7(3) . . . . ? O1R Ag1 N5A C6A -103.6(4) . . . . ? N5B Ag1 N5A C6A 93.1(4) . . . . ? O4B Ag1 N5A C6A -5.7(5) . . . . ? O4A Ag1 N5A C6A 178.7(4) . . . . ? Ag2 Ag1 N5A C6A 67.1(4) . . . . ? O1R Ag1 N5A C4AA 77.5(4) . . . . ? N5B Ag1 N5A C4AA -85.7(4) . . . . ? O4B Ag1 N5A C4AA 175.4(3) . . . . ? O4A Ag1 N5A C4AA -0.1(3) . . . . ? Ag2 Ag1 N5A C4AA -111.8(3) . . . . ? N5A Ag1 N5B C4AB -144.8(3) . . . . ? O1R Ag1 N5B C4AB 52.6(4) . . . . ? O4B Ag1 N5B C4AB -18.7(3) . . . . ? O4A Ag1 N5B C4AB 142.6(3) . . . . ? Ag2 Ag1 N5B C4AB -117.6(3) . . . . ? N5A Ag1 N5B C6B 51.7(5) . . . . ? O1R Ag1 N5B C6B -110.8(4) . . . . ? O4B Ag1 N5B C6B 177.9(4) . . . . ? O4A Ag1 N5B C6B -20.8(4) . . . . ? Ag2 Ag1 N5B C6B 78.9(4) . . . . ? N61A Ag2 N61B C61B 93.3(5) . . . . ? O1X Ag2 N61B C61B -42.4(5) . . . . ? O1Y Ag2 N61B C61B -150.5(4) . . . . ? Ag1 Ag2 N61B C61B 62.3(4) . . . . ? N61A Ag2 N61B O61B -76.1(4) . . . . ? O1X Ag2 N61B O61B 148.2(3) . . . . ? O1Y Ag2 N61B O61B 40.1(3) . . . . ? Ag1 Ag2 N61B O61B -107.1(3) . . . . ? N61B Ag2 N61A C61A 39.1(6) . . . . ? O1X Ag2 N61A C61A -173.0(5) . . . . ? O1Y Ag2 N61A C61A -75.4(4) . . . . ? Ag1 Ag2 N61A C61A 71.1(4) . . . . ? N61B Ag2 N61A O61A -140.6(3) . . . . ? O1X Ag2 N61A O61A 7.4(3) . . . . ? O1Y Ag2 N61A O61A 105.0(3) . . . . ? Ag1 Ag2 N61A O61A -108.5(3) . . . . ? C7B N8B C8AB N1B -179.9(5) . . . . ? C7B N8B C8AB C4AB 1.8(7) . . . . ? C2B N1B C8AB N8B -176.9(5) . . . . ? C1B N1B C8AB N8B 4.5(7) . . . . ? C2B N1B C8AB C4AB 1.4(7) . . . . ? C1B N1B C8AB C4AB -177.2(5) . . . . ? O61B N61B C61B C62B 0.8(7) . . . . ? Ag2 N61B C61B C62B -169.2(4) . . . . ? O61B N61B C61B C6B 176.9(4) . . . . ? Ag2 N61B C61B C6B 6.9(7) . . . . ? O61A N61A C61A C62A -1.2(7) . . . . ? Ag2 N61A C61A C62A 179.2(4) . . . . ? O61A N61A C61A C6A 176.1(4) . . . . ? Ag2 N61A C61A C6A -3.5(7) . . . . ? C8AA N8A C7A C6A -0.5(7) . . . . ? C8AA N8A C7A C71A -178.2(5) . . . . ? C8AA N1A C2A O2A -179.8(5) . . . . ? C1A N1A C2A O2A 0.5(8) . . . . ? C8AA N1A C2A N3A 0.4(7) . . . . ? C1A N1A C2A N3A -179.3(5) . . . . ? C4A N3A C2A O2A 177.8(5) . . . . ? C3A N3A C2A O2A -3.4(7) . . . . ? C4A N3A C2A N1A -2.3(7) . . . . ? C3A N3A C2A N1A 176.4(4) . . . . ? C4AB N5B C6B C7B -1.2(7) . . . . ? Ag1 N5B C6B C7B 161.4(4) . . . . ? C4AB N5B C6B C61B -179.7(4) . . . . ? Ag1 N5B C6B C61B -17.0(6) . . . . ? N61B C61B C6B N5B -46.0(6) . . . . ? C62B C61B C6B N5B 130.2(5) . . . . ? N61B C61B C6B C7B 135.6(5) . . . . ? C62B C61B C6B C7B -48.2(7) . . . . ? C7A N8A C8AA N1A -179.6(5) . . . . ? C7A N8A C8AA C4AA -0.3(7) . . . . ? C2A N1A C8AA N8A -179.0(5) . . . . ? C1A N1A C8AA N8A 0.8(7) . . . . ? C2A N1A C8AA C4AA 1.7(7) . . . . ? C1A N1A C8AA C4AA -178.6(5) . . . . ? Ag1 O4A C4A N3A -178.2(4) . . . . ? Ag1 O4A C4A C4AA 0.7(6) . . . . ? C2A N3A C4A O4A -179.0(5) . . . . ? C3A N3A C4A O4A 2.3(7) . . . . ? C2A N3A C4A C4AA 2.0(7) . . . . ? C3A N3A C4A C4AA -176.8(4) . . . . ? C8AB N8B C7B C6B 0.9(7) . . . . ? C8AB N8B C7B C71B -178.2(5) . . . . ? N5B C6B C7B N8B -1.3(8) . . . . ? C61B C6B C7B N8B 177.1(5) . . . . ? N5B C6B C7B C71B 177.7(5) . . . . ? C61B C6B C7B C71B -3.9(8) . . . . ? C4AA N5A C6A C7A -0.3(7) . . . . ? Ag1 N5A C6A C7A -179.1(4) . . . . ? C4AA N5A C6A C61A 178.9(4) . . . . ? Ag1 N5A C6A C61A 0.1(6) . . . . ? N8A C7A C6A N5A 0.8(8) . . . . ? C71A C7A C6A N5A 178.4(5) . . . . ? N8A C7A C6A C61A -178.3(5) . . . . ? C71A C7A C6A C61A -0.7(8) . . . . ? N61A C61A C6A N5A -51.3(6) . . . . ? C62A C61A C6A N5A 126.1(5) . . . . ? N61A C61A C6A C7A 127.9(5) . . . . ? C62A C61A C6A C7A -54.7(7) . . . . ? C6A N5A C4AA C8AA -0.5(7) . . . . ? Ag1 N5A C4AA C8AA 178.4(4) . . . . ? C6A N5A C4AA C4A -178.4(4) . . . . ? Ag1 N5A C4AA C4A 0.5(6) . . . . ? N8A C8AA C4AA N5A 0.8(8) . . . . ? N1A C8AA C4AA N5A -179.8(4) . . . . ? N8A C8AA C4AA C4A 178.7(5) . . . . ? N1A C8AA C4AA C4A -2.0(8) . . . . ? O4A C4A C4AA N5A -0.9(8) . . . . ? N3A C4A C4AA N5A 178.1(4) . . . . ? O4A C4A C4AA C8AA -178.8(5) . . . . ? N3A C4A C4AA C8AA 0.2(7) . . . . ? C8AB N1B C2B O2B -178.7(5) . . . . ? C1B N1B C2B O2B -0.1(8) . . . . ? C8AB N1B C2B N3B 1.7(7) . . . . ? C1B N1B C2B N3B -179.6(5) . . . . ? C4B N3B C2B O2B 175.9(5) . . . . ? C3B N3B C2B O2B -2.5(8) . . . . ? C4B N3B C2B N1B -4.5(8) . . . . ? C3B N3B C2B N1B 177.1(5) . . . . ? Ag1 O4B C4B N3B 162.2(4) . . . . ? Ag1 O4B C4B C4AB -17.5(6) . . . . ? C2B N3B C4B O4B -176.1(5) . . . . ? C3B N3B C4B O4B 2.3(8) . . . . ? C2B N3B C4B C4AB 3.6(7) . . . . ? C3B N3B C4B C4AB -178.0(5) . . . . ? Ag1 O1R C1R C2R -48.3(6) . . . . ? C6B N5B C4AB C8AB 3.9(7) . . . . ? Ag1 N5B C4AB C8AB -161.1(4) . . . . ? C6B N5B C4AB C4B -176.6(4) . . . . ? Ag1 N5B C4AB C4B 18.4(5) . . . . ? N8B C8AB C4AB N5B -4.4(7) . . . . ? N1B C8AB C4AB N5B 177.3(4) . . . . ? N8B C8AB C4AB C4B 176.2(5) . . . . ? N1B C8AB C4AB C4B -2.2(7) . . . . ? O4B C4B C4AB N5B -0.1(8) . . . . ? N3B C4B C4AB N5B -179.7(4) . . . . ? O4B C4B C4AB C8AB 179.4(5) . . . . ? N3B C4B C4AB C8AB -0.3(7) . . . . ? O3Y S1Y C1Y F2Y -60.1(5) . . . . ? O2Y S1Y C1Y F2Y 179.0(4) . . . . ? O1Y S1Y C1Y F2Y 61.2(5) . . . . ? O3Y S1Y C1Y F1Y 179.7(4) . . . . ? O2Y S1Y C1Y F1Y 58.8(5) . . . . ? O1Y S1Y C1Y F1Y -59.0(5) . . . . ? O3Y S1Y C1Y F3Y 60.7(5) . . . . ? O2Y S1Y C1Y F3Y -60.2(5) . . . . ? O1Y S1Y C1Y F3Y -178.0(4) . . . . ? O3X S1X C1X F1X -51.8(6) . . . . ? O2X S1X C1X F1X -173.5(5) . . . . ? O1X S1X C1X F1X 68.5(6) . . . . ? O3X S1X C1X F2X 68.2(7) . . . . ? O2X S1X C1X F2X -53.5(7) . . . . ? O1X S1X C1X F2X -171.5(6) . . . . ? O3X S1X C1X F3X -173.0(6) . . . . ? O2X S1X C1X F3X 65.2(6) . . . . ? O1X S1X C1X F3X -52.8(7) . . . . ? # Attachment 'Ag_DLMAceMOx_tetrafluoroborato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-12-14 at 12:46:59 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\archivos de programa\wingx\files\archive.dat # CIF files read : import archivebbbbbbbbbbb dreduc struct data_Ag_DLMAceMOx_tetrafluoroborato _database_code_depnum_ccdc_archive 'CCDC 861991' #TrackingRef 'Ag_DLMAceMOx_tetrafluoroborato.cif' _audit_creation_date 2011-12-14T12:46:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C22 H24 Ag N10 O6, B F4' _chemical_formula_sum 'C22 H24 Ag B F4 N10 O6' _chemical_formula_weight 719.19 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.493(3) _cell_length_b 9.5635(6) _cell_length_c 17.306(3) _cell_angle_alpha 90 _cell_angle_beta 97.588(15) _cell_angle_gamma 90 _cell_volume 2705.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 77(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.1 -1 0 0 0.08 0 1 0 0.08 -2 -1 -6 0.09 2 1 6 0.045 0 -1 1 0.106 4 3 -3 0.1 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS 2.10, 2003)' _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 0.8646 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 77(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1099 _diffrn_reflns_av_unetI/netI 0.1022 _diffrn_reflns_number 37829 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6225 _reflns_number_gt 3097 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. There are a few unassigned important density peaks. The largest one (Q1, 3.097) is placed at 2.062 from the Ag atom (Ag-Q1-N61A, 87.9\%; Ag-Q1-N61A-O61A, 117.4\%). ; _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^)+(0.1435P)^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_number_reflns 6225 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1642 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2468 _refine_ls_wR_factor_gt 0.1816 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.097 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.195 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.76187(3) 0.24707(6) 0.02803(3) 0.0265(2) Uani 1 1 d . . . F3 F 0.7448(3) 0.7438(4) 0.0244(3) 0.0384(12) Uani 1 1 d . . . F1 F 0.8299(3) 0.9273(5) 0.0188(3) 0.0394(12) Uani 1 1 d . . . O61A O 0.7253(4) 0.0076(5) -0.1080(3) 0.0364(14) Uani 1 1 d . . . F2 F 0.8392(3) 0.7914(6) 0.1282(3) 0.0507(13) Uani 1 1 d . . . F4 F 0.7298(3) 0.9337(5) 0.0985(3) 0.0432(12) Uani 1 1 d . . . O61B O 0.7862(3) 0.1291(5) 0.2025(3) 0.0321(13) Uani 1 1 d . . . O4B O 0.7813(3) 0.4688(6) -0.0889(3) 0.0320(13) Uani 1 1 d . . . O2B O 0.9406(3) 0.8508(5) -0.1168(3) 0.0335(13) Uani 1 1 d . . . O2A O 0.5437(3) 0.8485(6) 0.0894(3) 0.0342(13) Uani 1 1 d . . . O4A O 0.6716(3) 0.4283(5) 0.1317(3) 0.0317(13) Uani 1 1 d . . . N8B N 0.9914(3) 0.5996(6) 0.1123(3) 0.0238(14) Uani 1 1 d . . . N61A N 0.7064(4) 0.1423(6) -0.0846(3) 0.0259(14) Uani 1 1 d . . . N5A N 0.6348(4) 0.3609(6) -0.0253(3) 0.0255(14) Uani 1 1 d . . . N3B N 0.8593(4) 0.6607(6) -0.1021(3) 0.0264(14) Uani 1 1 d . . . N3A N 0.6103(4) 0.6416(6) 0.1104(3) 0.0239(14) Uani 1 1 d . . . N5B N 0.8548(3) 0.4366(6) 0.0655(3) 0.0240(13) Uani 1 1 d . . . N1A N 0.5539(4) 0.7124(7) -0.0161(4) 0.0287(15) Uani 1 1 d . . . N8A N 0.5711(4) 0.5729(6) -0.1257(3) 0.0257(14) Uani 1 1 d . . . N1B N 0.9708(4) 0.7218(6) -0.0058(3) 0.0229(14) Uani 1 1 d . . . N61B N 0.8237(4) 0.2194(7) 0.1537(4) 0.0294(16) Uani 1 1 d . . . C7B C 0.9659(4) 0.5031(7) 0.1602(4) 0.0241(16) Uani 1 1 d . . . C61A C 0.6462(5) 0.1981(8) -0.1280(4) 0.0254(16) Uani 1 1 d . . . C4AB C 0.8811(4) 0.5308(7) 0.0166(4) 0.0219(16) Uani 1 1 d . . . C4AA C 0.6148(4) 0.4865(8) 0.0026(4) 0.0269(17) Uani 1 1 d . . . C8AB C 0.9478(4) 0.6150(7) 0.0421(4) 0.0234(16) Uani 1 1 d . . . C2B C 0.9242(4) 0.7489(7) -0.0773(4) 0.0227(15) Uani 1 1 d . . . C4B C 0.8355(4) 0.5465(8) -0.0614(4) 0.0231(16) Uani 1 1 d . . . C71B C 1.0210(4) 0.4854(8) 0.2356(4) 0.0283(17) Uani 1 1 d . . . H71A H 1.0666 0.5514 0.2376 0.042 Uiso 1 1 calc R . . H71B H 1.0422 0.3896 0.2392 0.042 Uiso 1 1 calc R . . H71C H 0.99 0.5035 0.2791 0.042 Uiso 1 1 calc R . . C1B C 1.0382(5) 0.8180(8) 0.0225(4) 0.0310(18) Uani 1 1 d . . . H1B1 H 1.0652 0.7856 0.0733 0.046 Uiso 1 1 calc R . . H1B2 H 1.0163 0.9122 0.028 0.046 Uiso 1 1 calc R . . H1B3 H 1.078 0.82 -0.0148 0.046 Uiso 1 1 calc R . . C3B C 0.8077(5) 0.6975(9) -0.1766(4) 0.0308(18) Uani 1 1 d . . . H3B1 H 0.8309 0.7794 -0.1997 0.046 Uiso 1 1 calc R . . H3B2 H 0.752 0.7188 -0.1663 0.046 Uiso 1 1 calc R . . H3B3 H 0.8063 0.6184 -0.2127 0.046 Uiso 1 1 calc R . . C6A C 0.6222(4) 0.3396(8) -0.1019(4) 0.0252(17) Uani 1 1 d . . . C62B C 0.8596(5) 0.3490(9) 0.2755(4) 0.0352(19) Uani 1 1 d . . . H62A H 0.8344 0.2691 0.2986 0.053 Uiso 1 1 calc R . . H62B H 0.8282 0.4339 0.2828 0.053 Uiso 1 1 calc R . . H62C H 0.9159 0.3607 0.3008 0.053 Uiso 1 1 calc R . . C6B C 0.8937(4) 0.4257(7) 0.1370(4) 0.0243(16) Uani 1 1 d . . . C3A C 0.6348(5) 0.6832(8) 0.1912(4) 0.0309(18) Uani 1 1 d . . . H3A1 H 0.6131 0.7766 0.1997 0.046 Uiso 1 1 calc R . . H3A2 H 0.6946 0.685 0.202 0.046 Uiso 1 1 calc R . . H3A3 H 0.613 0.6161 0.226 0.046 Uiso 1 1 calc R . . C7A C 0.5936(4) 0.4490(8) -0.1529(4) 0.0254(16) Uani 1 1 d . . . C61B C 0.8599(4) 0.3235(8) 0.1897(4) 0.0251(16) Uani 1 1 d . . . C4A C 0.6352(4) 0.5107(8) 0.0866(4) 0.0259(17) Uani 1 1 d . . . C8AA C 0.5801(4) 0.5893(8) -0.0468(4) 0.0298(18) Uani 1 1 d . . . C71A C 0.5932(5) 0.4406(9) -0.2388(4) 0.037(2) Uani 1 1 d . . . H71D H 0.5709 0.5274 -0.263 0.055 Uiso 1 1 calc R . . H71E H 0.5592 0.3615 -0.2594 0.055 Uiso 1 1 calc R . . H71F H 0.6492 0.4272 -0.2504 0.055 Uiso 1 1 calc R . . C62A C 0.6000(5) 0.1256(7) -0.1967(4) 0.0280(17) Uani 1 1 d . . . H62D H 0.6253 0.0347 -0.2041 0.042 Uiso 1 1 calc R . . H62E H 0.6011 0.183 -0.2434 0.042 Uiso 1 1 calc R . . H62F H 0.5431 0.1115 -0.1875 0.042 Uiso 1 1 calc R . . C2A C 0.5670(4) 0.7415(7) 0.0608(4) 0.0193(15) Uani 1 1 d . . . C1A C 0.5096(5) 0.8176(9) -0.0694(4) 0.039(2) Uani 1 1 d . . . H1A1 H 0.5046 0.783 -0.1231 0.058 Uiso 1 1 calc R . . H1A2 H 0.5401 0.9058 -0.0655 0.058 Uiso 1 1 calc R . . H1A3 H 0.455 0.8331 -0.0546 0.058 Uiso 1 1 calc R . . B1 B 0.7867(6) 0.8486(10) 0.0689(6) 0.037(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 Ag 0.0291(3) 0.0242(4) 0.0247(3) 0.0001(2) -0.0014(2) -0.0003(3) F3 0.041(3) 0.029(3) 0.047(3) -0.009(2) 0.012(2) -0.007(2) F1 0.034(3) 0.034(3) 0.051(3) 0.009(2) 0.008(2) 0.002(2) O61A 0.053(4) 0.020(3) 0.038(3) -0.011(2) 0.011(3) 0.007(3) F2 0.054(3) 0.065(3) 0.032(3) 0.007(2) 0.004(2) 0.012(3) F4 0.042(3) 0.036(3) 0.053(3) -0.009(2) 0.014(2) 0.001(2) O61B 0.030(3) 0.034(3) 0.033(3) 0.012(2) 0.006(2) -0.003(2) O4B 0.035(3) 0.034(3) 0.026(3) -0.004(2) 0.000(2) -0.012(3) O2B 0.040(3) 0.030(3) 0.032(3) 0.002(3) 0.009(2) -0.006(3) O2A 0.035(3) 0.029(3) 0.039(3) -0.003(3) 0.006(2) 0.002(3) O4A 0.046(3) 0.024(3) 0.026(3) 0.001(2) 0.007(2) 0.009(3) N8B 0.025(3) 0.022(3) 0.024(3) 0.001(3) 0.003(3) 0.006(3) N61A 0.027(3) 0.028(4) 0.022(3) -0.002(3) 0.003(3) 0.001(3) N5A 0.030(4) 0.021(3) 0.026(3) -0.003(3) 0.005(3) 0.003(3) N3B 0.030(4) 0.030(4) 0.018(3) 0.001(3) 0.001(3) -0.001(3) N3A 0.031(4) 0.016(3) 0.025(3) 0.005(3) 0.005(3) 0.004(3) N5B 0.023(3) 0.022(3) 0.026(3) 0.002(3) 0.002(3) 0.002(3) N1A 0.025(3) 0.029(4) 0.030(4) 0.005(3) 0.001(3) -0.002(3) N8A 0.028(3) 0.025(4) 0.025(3) -0.006(3) 0.004(3) -0.001(3) N1B 0.026(3) 0.021(4) 0.022(3) 0.004(2) 0.003(3) -0.004(3) N61B 0.025(3) 0.037(4) 0.026(3) 0.013(3) 0.004(3) 0.004(3) C7B 0.020(4) 0.021(4) 0.032(4) -0.005(3) 0.007(3) 0.004(3) C61A 0.037(4) 0.020(4) 0.019(4) 0.000(3) 0.004(3) -0.002(4) C4AB 0.032(4) 0.016(4) 0.018(3) -0.006(3) 0.005(3) 0.005(3) C4AA 0.030(4) 0.022(4) 0.028(4) 0.005(3) 0.000(3) 0.001(3) C8AB 0.029(4) 0.021(4) 0.020(4) 0.000(3) 0.001(3) 0.010(3) C2B 0.023(4) 0.018(4) 0.028(4) -0.002(3) 0.005(3) -0.001(3) C4B 0.025(4) 0.023(4) 0.021(4) 0.000(3) 0.002(3) 0.001(3) C71B 0.028(4) 0.028(4) 0.027(4) -0.005(3) -0.002(3) -0.003(3) C1B 0.028(4) 0.031(5) 0.032(4) 0.002(4) 0.002(3) -0.006(4) C3B 0.034(5) 0.037(4) 0.020(4) 0.003(3) 0.000(3) -0.001(4) C6A 0.027(4) 0.025(4) 0.021(4) 0.002(3) -0.003(3) -0.008(3) C62B 0.041(5) 0.035(5) 0.031(4) 0.005(4) 0.010(4) -0.005(4) C6B 0.028(4) 0.022(4) 0.022(4) -0.006(3) 0.003(3) 0.000(3) C3A 0.043(5) 0.025(4) 0.025(4) 0.000(3) 0.006(3) -0.005(4) C7A 0.023(4) 0.019(4) 0.034(4) -0.001(3) 0.000(3) -0.002(3) C61B 0.026(4) 0.023(4) 0.027(4) 0.002(3) 0.009(3) 0.005(3) C4A 0.027(4) 0.028(4) 0.022(4) 0.001(3) -0.002(3) -0.002(3) C8AA 0.025(4) 0.033(5) 0.032(4) 0.003(4) 0.006(3) 0.000(4) C71A 0.031(5) 0.049(5) 0.029(4) 0.002(4) 0.001(3) 0.006(4) C62A 0.039(5) 0.016(4) 0.029(4) -0.010(3) 0.005(3) -0.001(3) C2A 0.016(3) 0.017(4) 0.026(4) -0.001(3) 0.005(3) -0.001(3) C1A 0.047(5) 0.032(5) 0.036(5) -0.003(4) 0.003(4) 0.010(4) B1 0.036(5) 0.036(6) 0.040(5) 0.008(5) 0.011(4) 0.005(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N61A 2.274(6) . ? Ag N61B 2.293(6) . ? Ag N5B 2.407(6) . ? Ag N5A 2.433(6) . ? F3 B1 1.391(11) . ? F1 B1 1.411(10) . ? O61A N61A 1.398(7) . ? F2 B1 1.367(10) . ? F4 B1 1.389(10) . ? O61B N61B 1.407(7) . ? O4B C4B 1.210(8) . ? O2B C2B 1.240(8) . ? O2A C2A 1.221(8) . ? O4A C4A 1.211(8) . ? N8B C8AB 1.336(8) . ? N8B C7B 1.343(9) . ? N61A C61A 1.279(9) . ? N5A C6A 1.330(8) . ? N5A C4AA 1.351(9) . ? N3B C4B 1.384(9) . ? N3B C2B 1.386(9) . ? N3B C3B 1.490(9) . ? N3A C4A 1.397(9) . ? N3A C2A 1.413(9) . ? N3A C3A 1.457(9) . ? N5B C6B 1.322(8) . ? N5B C4AB 1.346(9) . ? N1A C2A 1.349(9) . ? N1A C8AA 1.383(10) . ? N1A C1A 1.490(10) . ? N8A C7A 1.345(9) . ? N8A C8AA 1.363(9) . ? N1B C2B 1.391(10) . ? N1B C8AB 1.399(9) . ? N1B C1B 1.476(9) . ? N61B C61B 1.279(10) . ? C7B C6B 1.415(10) . ? C7B C71B 1.497(9) . ? C61A C62A 1.495(10) . ? C61A C6A 1.497(11) . ? C4AB C8AB 1.388(10) . ? C4AB C4B 1.464(9) . ? C4AA C8AA 1.377(10) . ? C4AA C4A 1.466(10) . ? C71B H71A 0.98 . ? C71B H71B 0.98 . ? C71B H71C 0.98 . ? C1B H1B1 0.98 . ? C1B H1B2 0.98 . ? C1B H1B3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C6A C7A 1.410(10) . ? C62B C61B 1.504(10) . ? C62B H62A 0.98 . ? C62B H62B 0.98 . ? C62B H62C 0.98 . ? C6B C61B 1.494(10) . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C7A C71A 1.487(10) . ? C71A H71D 0.98 . ? C71A H71E 0.98 . ? C71A H71F 0.98 . ? C62A H62D 0.98 . ? C62A H62E 0.98 . ? C62A H62F 0.98 . ? C1A H1A1 0.98 . ? C1A H1A2 0.98 . ? C1A H1A3 0.98 . ? 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 N61A Ag N61B 147.2(2) . . ? N61A Ag N5B 137.1(2) . . ? N61B Ag N5B 69.1(2) . . ? N61A Ag N5A 69.1(2) . . ? N61B Ag N5A 131.6(2) . . ? N5B Ag N5A 104.54(19) . . ? C8AB N8B C7B 117.6(6) . . ? C61A N61A O61A 113.6(6) . . ? C61A N61A Ag 120.9(5) . . ? O61A N61A Ag 125.0(4) . . ? C6A N5A C4AA 118.6(6) . . ? C6A N5A Ag 108.8(5) . . ? C4AA N5A Ag 120.0(5) . . ? C4B N3B C2B 125.6(6) . . ? C4B N3B C3B 117.3(6) . . ? C2B N3B C3B 117.0(6) . . ? C4A N3A C2A 124.8(6) . . ? C4A N3A C3A 118.3(6) . . ? C2A N3A C3A 116.9(6) . . ? C6B N5B C4AB 119.0(6) . . ? C6B N5B Ag 113.9(5) . . ? C4AB N5B Ag 125.6(4) . . ? C2A N1A C8AA 122.5(6) . . ? C2A N1A C1A 118.3(6) . . ? C8AA N1A C1A 119.3(6) . . ? C7A N8A C8AA 117.0(6) . . ? C2B N1B C8AB 120.1(6) . . ? C2B N1B C1B 118.9(6) . . ? C8AB N1B C1B 120.6(6) . . ? C61B N61B O61B 113.5(6) . . ? C61B N61B Ag 119.5(5) . . ? O61B N61B Ag 117.7(4) . . ? N8B C7B C6B 120.3(6) . . ? N8B C7B C71B 114.3(6) . . ? C6B C7B C71B 125.3(6) . . ? N61A C61A C62A 123.2(7) . . ? N61A C61A C6A 114.5(6) . . ? C62A C61A C6A 122.2(6) . . ? N5B C4AB C8AB 119.8(6) . . ? N5B C4AB C4B 118.6(6) . . ? C8AB C4AB C4B 121.5(6) . . ? N5A C4AA C8AA 121.0(7) . . ? N5A C4AA C4A 117.4(6) . . ? C8AA C4AA C4A 121.6(7) . . ? N8B C8AB C4AB 122.2(6) . . ? N8B C8AB N1B 117.7(6) . . ? C4AB C8AB N1B 120.0(6) . . ? O2B C2B N3B 121.6(7) . . ? O2B C2B N1B 120.1(6) . . ? N3B C2B N1B 118.4(6) . . ? O4B C4B N3B 122.0(6) . . ? O4B C4B C4AB 124.2(7) . . ? N3B C4B C4AB 113.8(6) . . ? C7B C71B H71A 109.5 . . ? C7B C71B H71B 109.5 . . ? H71A C71B H71B 109.5 . . ? C7B C71B H71C 109.5 . . ? H71A C71B H71C 109.5 . . ? H71B C71B H71C 109.5 . . ? N1B C1B H1B1 109.5 . . ? N1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? N1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? N3B C3B H3B1 109.5 . . ? N3B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N3B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N5A C6A C7A 120.4(7) . . ? N5A C6A C61A 115.3(6) . . ? C7A C6A C61A 124.2(6) . . ? C61B C62B H62A 109.5 . . ? C61B C62B H62B 109.5 . . ? H62A C62B H62B 109.5 . . ? C61B C62B H62C 109.5 . . ? H62A C62B H62C 109.5 . . ? H62B C62B H62C 109.5 . . ? N5B C6B C7B 120.7(7) . . ? N5B C6B C61B 116.7(6) . . ? C7B C6B C61B 122.5(6) . . ? N3A C3A H3A1 109.5 . . ? N3A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N3A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N8A C7A C6A 121.3(7) . . ? N8A C7A C71A 115.6(7) . . ? C6A C7A C71A 122.8(7) . . ? N61B C61B C6B 113.5(6) . . ? N61B C61B C62B 123.0(7) . . ? C6B C61B C62B 123.1(7) . . ? O4A C4A N3A 122.1(6) . . ? O4A C4A C4AA 124.5(7) . . ? N3A C4A C4AA 113.4(6) . . ? N8A C8AA C4AA 121.3(7) . . ? N8A C8AA N1A 119.0(7) . . ? C4AA C8AA N1A 119.6(7) . . ? C7A C71A H71D 109.5 . . ? C7A C71A H71E 109.5 . . ? H71D C71A H71E 109.5 . . ? C7A C71A H71F 109.5 . . ? H71D C71A H71F 109.5 . . ? H71E C71A H71F 109.5 . . ? C61A C62A H62D 109.5 . . ? C61A C62A H62E 109.5 . . ? H62D C62A H62E 109.5 . . ? C61A C62A H62F 109.5 . . ? H62D C62A H62F 109.5 . . ? H62E C62A H62F 109.5 . . ? O2A C2A N1A 123.7(7) . . ? O2A C2A N3A 118.8(6) . . ? N1A C2A N3A 117.6(6) . . ? N1A C1A H1A1 109.5 . . ? N1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? N1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? F2 B1 F4 110.4(7) . . ? F2 B1 F3 110.3(7) . . ? F4 B1 F3 108.5(7) . . ? F2 B1 F1 110.7(7) . . ? F4 B1 F1 109.5(7) . . ? F3 B1 F1 107.3(7) . . ? 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 N61B Ag N61A C61A 146.4(5) . . . . ? N5B Ag N61A C61A -78.7(6) . . . . ? N5A Ag N61A C61A 10.3(5) . . . . ? N61B Ag N61A O61A -24.6(7) . . . . ? N5B Ag N61A O61A 110.2(5) . . . . ? N5A Ag N61A O61A -160.7(6) . . . . ? N61A Ag N5A C6A -25.4(4) . . . . ? N61B Ag N5A C6A -175.2(4) . . . . ? N5B Ag N5A C6A 109.9(5) . . . . ? N61A Ag N5A C4AA -166.7(6) . . . . ? N61B Ag N5A C4AA 43.4(6) . . . . ? N5B Ag N5A C4AA -31.4(5) . . . . ? N61A Ag N5B C6B -154.6(5) . . . . ? N61B Ag N5B C6B 1.2(5) . . . . ? N5A Ag N5B C6B 130.6(5) . . . . ? N61A Ag N5B C4AB 11.2(7) . . . . ? N61B Ag N5B C4AB 167.0(6) . . . . ? N5A Ag N5B C4AB -63.6(6) . . . . ? N61A Ag N61B C61B 165.0(5) . . . . ? N5B Ag N61B C61B 16.1(5) . . . . ? N5A Ag N61B C61B -75.1(6) . . . . ? N61A Ag N61B O61B -50.4(7) . . . . ? N5B Ag N61B O61B 160.7(5) . . . . ? N5A Ag N61B O61B 69.6(5) . . . . ? C8AB N8B C7B C6B -2.4(9) . . . . ? C8AB N8B C7B C71B 176.0(6) . . . . ? O61A N61A C61A C62A 0.6(10) . . . . ? Ag N61A C61A C62A -171.4(5) . . . . ? O61A N61A C61A C6A 177.2(6) . . . . ? Ag N61A C61A C6A 5.2(9) . . . . ? C6B N5B C4AB C8AB -0.4(10) . . . . ? Ag N5B C4AB C8AB -165.6(5) . . . . ? C6B N5B C4AB C4B -177.3(6) . . . . ? Ag N5B C4AB C4B 17.6(9) . . . . ? C6A N5A C4AA C8AA 1.8(11) . . . . ? Ag N5A C4AA C8AA 139.5(6) . . . . ? C6A N5A C4AA C4A -175.4(6) . . . . ? Ag N5A C4AA C4A -37.7(8) . . . . ? C7B N8B C8AB C4AB -3.3(10) . . . . ? C7B N8B C8AB N1B 175.7(6) . . . . ? N5B C4AB C8AB N8B 4.9(10) . . . . ? C4B C4AB C8AB N8B -178.3(6) . . . . ? N5B C4AB C8AB N1B -174.0(6) . . . . ? C4B C4AB C8AB N1B 2.8(10) . . . . ? C2B N1B C8AB N8B -175.5(6) . . . . ? C1B N1B C8AB N8B -3.0(10) . . . . ? C2B N1B C8AB C4AB 3.5(10) . . . . ? C1B N1B C8AB C4AB 176.0(7) . . . . ? C4B N3B C2B O2B -178.7(7) . . . . ? C3B N3B C2B O2B -2.6(10) . . . . ? C4B N3B C2B N1B 0.4(10) . . . . ? C3B N3B C2B N1B 176.5(6) . . . . ? C8AB N1B C2B O2B 174.0(6) . . . . ? C1B N1B C2B O2B 1.4(10) . . . . ? C8AB N1B C2B N3B -5.1(10) . . . . ? C1B N1B C2B N3B -177.8(6) . . . . ? C2B N3B C4B O4B -175.1(7) . . . . ? C3B N3B C4B O4B 8.8(10) . . . . ? C2B N3B C4B C4AB 5.3(10) . . . . ? C3B N3B C4B C4AB -170.7(6) . . . . ? N5B C4AB C4B O4B -9.6(11) . . . . ? C8AB C4AB C4B O4B 173.6(7) . . . . ? N5B C4AB C4B N3B 169.9(6) . . . . ? C8AB C4AB C4B N3B -6.9(10) . . . . ? C4AA N5A C6A C7A 4.0(10) . . . . ? Ag N5A C6A C7A -138.0(6) . . . . ? C4AA N5A C6A C61A 179.8(6) . . . . ? Ag N5A C6A C61A 37.8(7) . . . . ? N61A C61A C6A N5A -31.0(10) . . . . ? C62A C61A C6A N5A 145.7(7) . . . . ? N61A C61A C6A C7A 144.6(7) . . . . ? C62A C61A C6A C7A -38.7(11) . . . . ? C4AB N5B C6B C7B -5.2(10) . . . . ? Ag N5B C6B C7B 161.6(5) . . . . ? C4AB N5B C6B C61B 177.7(6) . . . . ? Ag N5B C6B C61B -15.5(8) . . . . ? N8B C7B C6B N5B 6.9(10) . . . . ? C71B C7B C6B N5B -171.4(7) . . . . ? N8B C7B C6B C61B -176.2(6) . . . . ? C71B C7B C6B C61B 5.5(11) . . . . ? C8AA N8A C7A C6A 2.2(10) . . . . ? C8AA N8A C7A C71A -172.5(6) . . . . ? N5A C6A C7A N8A -6.2(11) . . . . ? C61A C6A C7A N8A 178.4(7) . . . . ? N5A C6A C7A C71A 168.1(7) . . . . ? C61A C6A C7A C71A -7.3(11) . . . . ? O61B N61B C61B C6B -175.2(6) . . . . ? Ag N61B C61B C6B -29.2(8) . . . . ? O61B N61B C61B C62B -2.1(10) . . . . ? Ag N61B C61B C62B 143.9(6) . . . . ? N5B C6B C61B N61B 29.6(9) . . . . ? C7B C6B C61B N61B -147.5(7) . . . . ? N5B C6B C61B C62B -143.5(7) . . . . ? C7B C6B C61B C62B 39.5(10) . . . . ? C2A N3A C4A O4A -179.3(7) . . . . ? C3A N3A C4A O4A 4.7(11) . . . . ? C2A N3A C4A C4AA 2.3(10) . . . . ? C3A N3A C4A C4AA -173.6(6) . . . . ? N5A C4AA C4A O4A 3.3(11) . . . . ? C8AA C4AA C4A O4A -173.9(7) . . . . ? N5A C4AA C4A N3A -178.3(6) . . . . ? C8AA C4AA C4A N3A 4.5(10) . . . . ? C7A N8A C8AA C4AA 3.6(11) . . . . ? C7A N8A C8AA N1A -176.8(6) . . . . ? N5A C4AA C8AA N8A -5.8(11) . . . . ? C4A C4AA C8AA N8A 171.3(7) . . . . ? N5A C4AA C8AA N1A 174.6(7) . . . . ? C4A C4AA C8AA N1A -8.3(11) . . . . ? C2A N1A C8AA N8A -174.2(6) . . . . ? C1A N1A C8AA N8A 5.9(10) . . . . ? C2A N1A C8AA C4AA 5.5(11) . . . . ? C1A N1A C8AA C4AA -174.5(7) . . . . ? C8AA N1A C2A O2A -179.1(7) . . . . ? C1A N1A C2A O2A 0.8(11) . . . . ? C8AA N1A C2A N3A 1.0(10) . . . . ? C1A N1A C2A N3A -179.0(6) . . . . ? C4A N3A C2A O2A 175.1(7) . . . . ? C3A N3A C2A O2A -8.9(9) . . . . ? C4A N3A C2A N1A -5.0(10) . . . . ? C3A N3A C2A N1A 170.9(6) . . . . ?