# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'James Crowley' _publ_contact_author_email JCROWLEY@CHEMISTRY.OTAGO.AC.NZ _publ_section_title ; A multicomponent CuAAC "click" approach to a library of hybrid polydentate 2-pyridyl-1,2,3-triazole ligands: New building blocks for the generation metallosupramolecular architectures. ; loop_ _publ_author_name 'James Crowley' 'Pauline H. Bandeen' # Attachment 'jc138DaltonNew10092009.cif' data_jc138 _database_code_depnum_ccdc_archive 'CCDC 734027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 N8, 0.22(CHCl3)' _chemical_formula_sum 'C22.22 H18.22 Cl0.66 N8' _chemical_formula_weight 420.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 31.6602(14) _cell_length_b 31.6602(14) _cell_length_c 5.4696(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4748.0(5) _cell_formula_units_Z 9 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9315 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.82 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1854.0 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9525 _exptl_absorpt_correction_T_max 0.9907 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21929 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.50 _reflns_number_total 1974 _reflns_number_gt 1832 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.023 177 41 ' ' 2 0.333 0.667 0.225 180 41 ' ' 3 0.667 0.333 0.892 180 41 ' ' _platon_squeeze_details ;The unit cell contains 2 chloroform molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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_coef 0.0021(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1974 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.1952 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.58509(6) 0.17464(6) 0.2230(3) 0.0340(5) Uani 1 1 d . . . H1 H 0.5861 0.1933 0.3567 0.041 Uiso 1 1 calc R . . C2 C 0.55212(6) 0.16711(6) 0.0389(3) 0.0354(5) Uani 1 1 d . . . H2 H 0.5314 0.1799 0.0495 0.042 Uiso 1 1 calc R . . C3 C 0.55092(6) 0.13984(7) -0.1616(3) 0.0360(5) Uani 1 1 d . . . H3 H 0.5293 0.1341 -0.2894 0.043 Uiso 1 1 calc R . . C4 C 0.58193(5) 0.12137(5) -0.1696(2) 0.0289(4) Uani 1 1 d . . . H4 H 0.5818 0.1031 -0.3028 0.035 Uiso 1 1 calc R . . C5 C 0.61359(5) 0.13060(5) 0.0260(2) 0.0214(4) Uani 1 1 d . . . C6 C 0.64734(5) 0.11137(4) 0.0288(2) 0.0205(4) Uani 1 1 d . . . C7 C 0.67391(5) 0.10843(5) 0.2204(2) 0.0219(4) Uani 1 1 d . . . H7 H 0.6742 0.1177 0.3820 0.026 Uiso 1 1 calc R . . C8 C 0.73687(5) 0.08160(5) 0.2386(3) 0.0255(4) Uani 1 1 d . . . H8A H 0.7360 0.0530 0.1687 0.031 Uiso 1 1 calc R . . H8B H 0.7300 0.0758 0.4120 0.031 Uiso 1 1 calc R . . C9 C 0.78706(5) 0.12545(5) 0.2032(2) 0.0230(4) Uani 1 1 d . . . C10 C 0.81454(5) 0.12947(5) -0.0042(3) 0.0261(4) Uani 1 1 d . . . H10 H 0.8019 0.1047 -0.1202 0.031 Uiso 1 1 calc R . . C11 C 0.80640(5) 0.16349(5) 0.3729(2) 0.0258(4) Uani 1 1 d . . . H11 H 0.7884 0.1617 0.5110 0.031 Uiso 1 1 calc R . . N1 N 0.61553(5) 0.15692(5) 0.2216(2) 0.0303(4) Uani 1 1 d . . . N2 N 0.65810(4) 0.09367(4) -0.1757(2) 0.0241(4) Uani 1 1 d . . . N4 N 0.69943(4) 0.08914(4) 0.12215(19) 0.0217(4) Uani 1 1 d . . . N3 N 0.69008(4) 0.08045(4) -0.1185(2) 0.0256(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0413(10) 0.0394(9) 0.0311(9) -0.0029(6) 0.0013(7) 0.0276(8) C2 0.0326(9) 0.0472(10) 0.0355(9) 0.0071(7) 0.0055(6) 0.0268(8) C3 0.0256(8) 0.0536(10) 0.0321(9) 0.0021(7) -0.0050(6) 0.0222(7) C4 0.0243(8) 0.0368(9) 0.0246(8) -0.0020(6) -0.0020(5) 0.0145(6) C5 0.0181(7) 0.0218(7) 0.0201(8) 0.0047(5) 0.0023(5) 0.0069(5) C6 0.0169(7) 0.0205(7) 0.0189(7) 0.0023(5) 0.0024(5) 0.0054(5) C7 0.0223(7) 0.0230(7) 0.0190(7) 0.0007(5) 0.0013(5) 0.0104(6) C8 0.0264(8) 0.0250(8) 0.0288(8) -0.0001(6) -0.0031(5) 0.0158(6) C9 0.0261(8) 0.0250(7) 0.0232(8) 0.0015(5) -0.0020(5) 0.0169(6) C10 0.0291(8) 0.0285(8) 0.0268(8) -0.0065(5) -0.0038(5) 0.0190(6) C11 0.0274(8) 0.0327(8) 0.0227(7) -0.0018(6) -0.0011(5) 0.0191(7) N1 0.0335(7) 0.0361(8) 0.0263(7) -0.0039(5) -0.0034(5) 0.0212(6) N2 0.0222(7) 0.0277(7) 0.0216(7) -0.0033(4) -0.0020(4) 0.0118(5) N4 0.0213(6) 0.0210(6) 0.0207(7) 0.0006(4) -0.0004(4) 0.0092(5) N3 0.0263(7) 0.0301(7) 0.0219(7) -0.0042(5) -0.0031(4) 0.0152(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.3357(19) . ? C1 C2 1.382(2) . ? C1 H1 0.9300 . ? C2 C3 1.384(2) . ? C2 H2 0.9300 . ? C3 C4 1.372(2) . ? C3 H3 0.9300 . ? C4 C5 1.3932(19) . ? C4 H4 0.9300 . ? C5 N1 1.3389(17) . ? C5 C6 1.471(2) . ? C6 C7 1.3760(19) . ? C6 N2 1.3682(17) . ? C7 N4 1.3446(19) . ? C7 H7 0.9300 . ? C8 N4 1.4663(17) . ? C8 C9 1.511(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.396(2) . ? C9 C11 1.3965(19) . ? C10 C11 1.385(2) 13_655 ? C10 H10 0.9300 . ? C11 C10 1.385(2) 13_655 ? C11 H11 0.9300 . ? N2 N3 1.3124(17) . ? N4 N3 1.3470(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.39(14) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 117.85(14) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 119.27(14) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.64(14) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 123.25(13) . . ? N1 C5 C6 115.64(11) . . ? C4 C5 C6 121.11(12) . . ? C7 C6 N2 108.00(12) . . ? C7 C6 C5 129.15(12) . . ? N2 C6 C5 122.84(12) . . ? N4 C7 C6 104.64(11) . . ? N4 C7 H7 127.7 . . ? C6 C7 H7 127.7 . . ? N4 C8 C9 111.05(11) . . ? N4 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N4 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C11 118.50(14) . . ? C10 C9 C8 120.59(12) . . ? C11 C9 C8 120.89(12) . . ? C11 C10 C9 120.94(13) 13_655 . ? C11 C10 H10 119.5 13_655 . ? C9 C10 H10 119.5 . . ? C10 C11 C9 120.56(13) 13_655 . ? C10 C11 H11 119.7 13_655 . ? C9 C11 H11 119.7 . . ? C1 N1 C5 116.60(12) . . ? N3 N2 C6 109.00(11) . . ? C7 N4 N3 111.28(11) . . ? C7 N4 C8 128.21(11) . . ? N3 N4 C8 120.26(10) . . ? N2 N3 N4 107.07(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.445 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.086 # Attachment 'jc275DaltonNew27082009.cif' data_jc275 _database_code_depnum_ccdc_archive 'CCDC 734028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C13 H11 Ag N5), C3 H6 O, 2(F6 Sb)' _chemical_formula_sum 'C29 H28 Ag2 F12 N10 O Sb2' _chemical_formula_weight 1219.8234 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.214(1) _cell_length_b 8.760(1) _cell_length_c 14.108(1) _cell_angle_alpha 74.161(4) _cell_angle_beta 86.982(4) _cell_angle_gamma 74.951(4) _cell_volume 942.92(17) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7978 _cell_measurement_theta_min 2.568 _cell_measurement_theta_max 46.924 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 2.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.370 _exptl_absorpt_correction_T_max 0.685 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16885 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3489 _reflns_number_gt 3460 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0286P)^2^+8.4679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3489 _refine_ls_number_parameters 267 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.251 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9544(8) 0.4240(8) 0.1982(5) 0.0196(13) Uani 1 1 d . . . H1A H 0.9950 0.3268 0.2469 0.023 Uiso 1 1 calc R . . C2 C 0.7826(8) 0.4968(8) 0.1923(5) 0.0221(13) Uani 1 1 d . . . H2B H 0.7103 0.4502 0.2372 0.027 Uiso 1 1 calc R . . C3 C 0.7198(8) 0.6394(8) 0.1191(5) 0.0201(13) Uani 1 1 d . . . H3A H 0.6045 0.6878 0.1120 0.024 Uiso 1 1 calc R . . C4 C 0.8321(8) 0.7084(8) 0.0567(5) 0.0170(12) Uani 1 1 d . . . H4A H 0.7938 0.8057 0.0078 0.020 Uiso 1 1 calc R . . C5 C 1.0035(7) 0.6304(7) 0.0680(4) 0.0143(11) Uani 1 1 d . . . C6 C 1.1290(7) 0.6998(7) 0.0049(4) 0.0141(11) Uani 1 1 d . . . C7 C 1.1085(8) 0.8391(8) -0.0711(5) 0.0181(12) Uani 1 1 d . . . H7 H 1.0080 0.9146 -0.0966 0.022 Uiso 1 1 calc R . . C8 C 1.6770(8) 0.0387(8) 0.1836(5) 0.0191(13) Uani 1 1 d . . . H8A H 1.7607 -0.0660 0.1970 0.023 Uiso 1 1 calc R . . H8B H 1.5725 0.0223 0.1645 0.023 Uiso 1 1 calc R . . C9 C 1.6497(7) 0.0952(7) 0.2760(4) 0.0156(12) Uani 1 1 d . . . C10 C 1.7598(9) 0.0231(10) 0.3558(5) 0.0322(17) Uani 1 1 d . . . H10A H 1.8572 -0.0575 0.3519 0.039 Uiso 1 1 calc R . . C11 C 1.7240(11) 0.0715(13) 0.4410(6) 0.046(2) Uani 1 1 d . . . H11A H 1.7962 0.0237 0.4956 0.056 Uiso 1 1 calc R . . C12 C 1.5792(10) 0.1921(11) 0.4441(5) 0.0323(17) Uani 1 1 d . . . H12A H 1.5519 0.2270 0.5009 0.039 Uiso 1 1 calc R . . C13 C 1.4761(9) 0.2599(9) 0.3616(5) 0.0236(14) Uani 1 1 d . . . H13A H 1.3783 0.3410 0.3640 0.028 Uiso 1 1 calc R . . N1 N 1.0641(6) 0.4874(6) 0.1370(4) 0.0165(10) Uani 1 1 d . . . N2 N 1.2974(6) 0.6266(7) 0.0179(4) 0.0185(11) Uani 1 1 d . . . N3 N 1.6196(6) 0.2862(7) 0.0466(4) 0.0178(11) Uani 1 1 d . . . N4 N 1.7338(6) 0.1571(6) 0.1011(4) 0.0154(10) Uani 1 1 d . . . N5 N 1.5097(6) 0.2146(6) 0.2779(4) 0.0175(11) Uani 1 1 d . . . F1 F 0.7758(6) 0.2911(7) 0.6071(3) 0.0451(13) Uani 1 1 d . . . F2 F 0.8267(6) -0.0209(6) 0.7081(5) 0.0529(15) Uani 1 1 d . . . F3 F 0.5175(5) 0.1772(5) 0.6899(3) 0.0280(9) Uani 1 1 d . . . F4 F 0.6840(5) 0.0670(6) 0.8616(3) 0.0365(11) Uani 1 1 d . . . F5 F 0.9374(5) 0.1837(5) 0.7800(3) 0.0268(9) Uani 1 1 d . . . F6 F 0.6287(5) 0.3794(5) 0.7623(3) 0.0310(9) Uani 1 1 d . . . Ag1 Ag 1.35421(6) 0.37667(6) 0.14510(3) 0.02029(16) Uani 1 1 d . . . Sb1 Sb 0.72760(5) 0.18018(5) 0.73389(3) 0.01627(15) Uani 1 1 d . . . O1 O 1.0767(15) 0.3398(15) 0.4443(9) 0.042(3) Uani 0.50 1 d P A -1 C14 C 1.019(2) 0.447(2) 0.4811(12) 0.038(4) Uani 0.50 1 d P A -1 C15 C 0.8771 0.5584 0.4349 0.065(4) Uani 0.50 1 d PU A -1 H15A H 0.9025 0.6079 0.3682 0.097 Uiso 0.50 1 calc PR A -1 H15B H 0.8397 0.6417 0.4691 0.097 Uiso 0.50 1 calc PR A -1 H15C H 0.7898 0.5037 0.4350 0.097 Uiso 0.50 1 calc PR A -1 C15A C 1.1210 0.4431 0.5646 0.065(4) Uani 0.50 1 d PU A -1 H15D H 1.0596 0.5218 0.5979 0.097 Uiso 0.50 1 calc PR A -1 H15E H 1.2246 0.4697 0.5408 0.097 Uiso 0.50 1 calc PR A -1 H15F H 1.1454 0.3354 0.6096 0.097 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.023(3) 0.013(3) -0.006(2) 0.002(2) -0.010(3) C2 0.023(3) 0.030(3) 0.018(3) -0.009(3) 0.009(2) -0.013(3) C3 0.014(3) 0.031(3) 0.018(3) -0.011(3) 0.003(2) -0.006(3) C4 0.013(3) 0.022(3) 0.016(3) -0.006(2) 0.002(2) -0.005(2) C5 0.014(3) 0.020(3) 0.012(3) -0.008(2) 0.003(2) -0.007(2) C6 0.011(3) 0.021(3) 0.011(3) -0.008(2) 0.002(2) -0.003(2) C7 0.014(3) 0.022(3) 0.019(3) -0.008(2) 0.004(2) -0.002(2) C8 0.017(3) 0.021(3) 0.020(3) -0.006(3) 0.006(2) -0.007(2) C9 0.016(3) 0.020(3) 0.010(3) 0.000(2) 0.005(2) -0.009(2) C10 0.022(4) 0.044(4) 0.024(4) -0.007(3) 0.002(3) 0.001(3) C11 0.034(4) 0.077(7) 0.019(4) -0.013(4) -0.006(3) 0.004(4) C12 0.031(4) 0.051(5) 0.014(3) -0.013(3) 0.002(3) -0.007(3) C13 0.024(3) 0.028(3) 0.015(3) -0.004(3) 0.006(3) -0.003(3) N1 0.015(2) 0.023(3) 0.012(2) -0.006(2) 0.0022(19) -0.006(2) N2 0.013(2) 0.027(3) 0.015(3) -0.007(2) 0.0010(19) -0.004(2) N3 0.014(2) 0.027(3) 0.009(2) -0.002(2) 0.0007(19) -0.004(2) N4 0.014(2) 0.020(3) 0.012(2) -0.005(2) 0.0030(19) -0.006(2) N5 0.017(3) 0.021(3) 0.011(2) 0.001(2) 0.0025(19) -0.005(2) F1 0.048(3) 0.086(4) 0.0104(19) -0.002(2) 0.0075(18) -0.044(3) F2 0.033(3) 0.039(3) 0.100(5) -0.046(3) 0.014(3) -0.007(2) F3 0.0212(19) 0.039(2) 0.026(2) -0.0025(17) -0.0020(16) -0.0167(17) F4 0.033(2) 0.047(3) 0.020(2) 0.0182(18) -0.0030(17) -0.020(2) F5 0.0155(18) 0.035(2) 0.032(2) -0.0095(18) -0.0016(15) -0.0091(16) F6 0.026(2) 0.026(2) 0.042(3) -0.0160(19) 0.0016(18) -0.0014(17) Ag1 0.0164(3) 0.0232(3) 0.0175(3) -0.00232(19) -0.00164(18) -0.00153(19) Sb1 0.0151(2) 0.0192(2) 0.0152(2) -0.00430(16) 0.00341(15) -0.00641(16) O1 0.034(6) 0.046(7) 0.037(6) -0.008(5) 0.009(5) 0.000(5) C14 0.044(9) 0.049(10) 0.024(8) -0.007(7) 0.014(7) -0.025(8) C15 0.092(10) 0.078(9) 0.039(7) -0.006(7) 0.004(7) -0.057(8) C15A 0.092(10) 0.079(9) 0.039(7) -0.006(7) 0.004(7) -0.057(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.336(8) . ? C1 C2 1.386(10) . ? C1 H1A 0.9300 . ? C2 C3 1.382(10) . ? C2 H2B 0.9300 . ? C3 C4 1.380(9) . ? C3 H3A 0.9300 . ? C4 C5 1.392(8) . ? C4 H4A 0.9300 . ? C5 N1 1.351(8) . ? C5 C6 1.469(8) . ? C6 N2 1.364(8) . ? C6 C7 1.367(9) . ? C7 N4 1.347(8) 2_865 ? C7 H7 0.9300 . ? C8 N4 1.478(8) . ? C8 C9 1.502(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N5 1.343(8) . ? C9 C10 1.380(10) . ? C10 C11 1.374(11) . ? C10 H10A 0.9300 . ? C11 C12 1.378(12) . ? C11 H11A 0.9300 . ? C12 C13 1.375(10) . ? C12 H12A 0.9300 . ? C13 N5 1.338(9) . ? C13 H13A 0.9300 . ? N1 Ag1 2.324(5) . ? N2 N3 1.305(8) 2_865 ? N2 Ag1 2.375(6) . ? N3 N2 1.305(8) 2_865 ? N3 N4 1.343(7) . ? N3 Ag1 2.587(5) . ? N4 C7 1.347(8) 2_865 ? N5 Ag1 2.239(5) . ? F1 Sb1 1.864(4) . ? F2 Sb1 1.863(5) . ? F3 Sb1 1.873(4) . ? F4 Sb1 1.871(4) . ? F5 Sb1 1.884(4) . ? F6 Sb1 1.865(4) . ? O1 C14 1.17(2) . ? C14 C15 1.372(19) . ? C14 C15A 1.470(18) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C15A H15D 0.9600 . ? C15A H15E 0.9600 . ? C15A H15F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.8(6) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 119.3(6) . . ? C3 C2 H2B 120.3 . . ? C1 C2 H2B 120.3 . . ? C4 C3 C2 118.5(6) . . ? C4 C3 H3A 120.8 . . ? C2 C3 H3A 120.8 . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 122.3(5) . . ? N1 C5 C6 116.2(5) . . ? C4 C5 C6 121.5(5) . . ? N2 C6 C7 108.0(5) . . ? N2 C6 C5 121.6(5) . . ? C7 C6 C5 130.3(5) . . ? N4 C7 C6 104.6(5) 2_865 . ? N4 C7 H7 127.7 2_865 . ? C6 C7 H7 127.7 . . ? N4 C8 C9 112.6(5) . . ? N4 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N5 C9 C10 122.1(6) . . ? N5 C9 C8 116.4(5) . . ? C10 C9 C8 121.4(6) . . ? C11 C10 C9 119.4(7) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C10 C11 C12 118.9(7) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 118.7(7) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? N5 C13 C12 123.1(6) . . ? N5 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C1 N1 C5 117.9(5) . . ? C1 N1 Ag1 124.8(4) . . ? C5 N1 Ag1 117.3(4) . . ? N3 N2 C6 109.2(5) 2_865 . ? N3 N2 Ag1 138.5(4) 2_865 . ? C6 N2 Ag1 112.2(4) . . ? N2 N3 N4 107.1(5) 2_865 . ? N2 N3 Ag1 130.5(4) 2_865 . ? N4 N3 Ag1 112.4(3) . . ? N3 N4 C7 111.0(5) . 2_865 ? N3 N4 C8 119.5(5) . . ? C7 N4 C8 129.4(5) 2_865 . ? C13 N5 C9 117.8(5) . . ? C13 N5 Ag1 116.3(4) . . ? C9 N5 Ag1 124.9(4) . . ? N5 Ag1 N1 127.07(18) . . ? N5 Ag1 N2 148.15(19) . . ? N1 Ag1 N2 72.57(18) . . ? N5 Ag1 N3 85.11(17) . . ? N1 Ag1 N3 145.35(17) . . ? N2 Ag1 N3 85.68(17) . . ? F2 Sb1 F1 90.6(3) . . ? F2 Sb1 F6 178.9(3) . . ? F1 Sb1 F6 90.5(2) . . ? F2 Sb1 F4 88.8(3) . . ? F1 Sb1 F4 178.8(2) . . ? F6 Sb1 F4 90.1(2) . . ? F2 Sb1 F3 90.7(2) . . ? F1 Sb1 F3 90.63(19) . . ? F6 Sb1 F3 89.62(19) . . ? F4 Sb1 F3 90.39(18) . . ? F2 Sb1 F5 89.8(2) . . ? F1 Sb1 F5 90.09(19) . . ? F6 Sb1 F5 89.84(19) . . ? F4 Sb1 F5 88.89(19) . . ? F3 Sb1 F5 179.10(18) . . ? O1 C14 C15 115.1(15) . . ? O1 C14 C15A 113.3(15) . . ? C15 C14 C15A 131.4(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.961 _refine_diff_density_min -2.605 _refine_diff_density_rms 0.184 # END of CIF # Attachment 'pbjdc12226052009.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-26 at 14:50:10 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\program files\wingx\files\archive.reqdat # CIF files read : pb122 pcf #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_pb122 _database_code_depnum_ccdc_archive 'CCDC 734029' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-05-26 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? # Insert blank lines between references _publ_section_references ; Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C38 H40 Ag2 N16, 2(F6 Sb)' _chemical_formula_sum 'C38 H40 Ag2 F12 N16 Sb2' _chemical_formula_weight 1408.1 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.719(3) _cell_length_b 23.253(6) _cell_length_c 12.871(6) _cell_angle_alpha 90.000 _cell_angle_beta 105.907(12) _cell_angle_gamma 90.000 _cell_volume 4812(3) _cell_formula_units_Z 4 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8810 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 30.83 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_type multi-scan #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_unetI/netI 0.0296 _diffrn_reflns_number 85713 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 8960 _reflns_number_gt 8109 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0318P)^2^+7.1141P] where P=(Fo^2^+2Fc^2^)/3' _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 0.00046(4) _refine_ls_number_reflns 8960 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.03 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.859 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # 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' 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' Sb Sb -0.5866 1.5461 '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 Sb1 Sb 0.562533(13) 0.786148(9) 0.051999(18) 0.02636(7) Uani 1 1 d . . . Ag2 Ag -0.162120(14) -0.016017(10) 0.89228(2) 0.02600(7) Uani 1 1 d . . . Ag1 Ag -0.322267(14) 0.007695(10) 0.60631(2) 0.02501(7) Uani 1 1 d . . . Sb2 Sb 0.893348(15) 0.172103(9) 0.37951(2) 0.03440(8) Uani 1 1 d . . . F7 F 0.90296(17) 0.21393(11) 0.5063(2) 0.0619(7) Uani 1 1 d . . . F5 F 0.47284(14) 0.80487(11) -0.06547(18) 0.0526(6) Uani 1 1 d . . . F2 F 0.51864(16) 0.71292(9) 0.0585(2) 0.0522(6) Uani 1 1 d . . . F8 F 0.89086(15) 0.10354(10) 0.4547(2) 0.0540(6) Uani 1 1 d . . . N5 N -0.05883(15) -0.07981(10) 0.9391(2) 0.0202(5) Uani 1 1 d . . . F4 F 0.60625(15) 0.85959(9) 0.0462(2) 0.0542(6) Uani 1 1 d . . . N6 N 0.00372(15) -0.07292(10) 1.0261(2) 0.0205(5) Uani 1 1 d . . . N12 N -0.17724(15) -0.00931(11) 0.6232(2) 0.0210(5) Uani 1 1 d . . . F11 F 0.89515(17) 0.24055(10) 0.3055(2) 0.0656(7) Uani 1 1 d . . . N15 N -0.48509(15) -0.09305(10) 0.36015(19) 0.0190(5) Uani 1 1 d . . . N4 N -0.27909(15) -0.07651(11) 0.8151(2) 0.0215(5) Uani 1 1 d . . . F6 F 0.61950(16) 0.75909(9) -0.0434(2) 0.0579(7) Uani 1 1 d . . . N7 N 0.04998(15) -0.12045(10) 1.0351(2) 0.0203(5) Uani 1 1 d . . . F1 F 0.50309(16) 0.81224(12) 0.1456(2) 0.0605(7) Uani 1 1 d . . . N9 N 0.14859(16) 0.05874(12) 0.8384(2) 0.0303(6) Uani 1 1 d . . . F3 F 0.65206(16) 0.76854(13) 0.1690(2) 0.0753(9) Uani 1 1 d . . . F9 F 0.77760(14) 0.17768(11) 0.3512(2) 0.0636(7) Uani 1 1 d . . . F12 F 1.00854(16) 0.16731(12) 0.4133(3) 0.0734(9) Uani 1 1 d . . . N2 N -0.40699(15) -0.09459(10) 0.7376(2) 0.0221(5) Uani 1 1 d . . . N16 N -0.32068(15) 0.10296(11) 0.6351(2) 0.0208(5) Uani 1 1 d . . . N10 N -0.04600(15) -0.01262(10) 0.6954(2) 0.0214(5) Uani 1 1 d . . . N13 N -0.38912(15) -0.05752(11) 0.4871(2) 0.0225(5) Uani 1 1 d . . . C35 C -0.3673(2) 0.18988(13) 0.6976(3) 0.0258(7) Uani 1 1 d . . . H35 H -0.4041 0.2082 0.7294 0.031 Uiso 1 1 calc R . . N14 N -0.46525(15) -0.04767(11) 0.4250(2) 0.0232(6) Uani 1 1 d . . . C100 C -0.2922(2) 0.05603(15) 0.9639(3) 0.0288(7) Uani 1 1 d . . . H100 H -0.31 0.0186 0.9703 0.035 Uiso 1 1 calc R . . C21 C 0.1483(3) 0.15751(17) 0.7898(3) 0.0452(10) Uani 1 1 d . . . H21 H 0.1764 0.1925 0.7975 0.054 Uiso 1 1 calc R . . N8 N -0.22592(15) 0.06387(11) 0.9270(2) 0.0222(5) Uani 1 1 d . . . C27 C -0.14241(19) -0.03425(13) 0.5510(2) 0.0220(6) Uani 1 1 d . . . N3 N -0.34898(15) -0.05314(11) 0.7554(2) 0.0240(6) Uani 1 1 d . . . C10 C -0.2255(2) -0.17269(14) 0.8936(3) 0.0297(8) Uani 1 1 d . . . H10A H -0.2503 -0.2044 0.9226 0.036 Uiso 1 1 calc R . . H10B H -0.1889 -0.1524 0.954 0.036 Uiso 1 1 calc R . . C33 C -0.43345(17) 0.09531(13) 0.7194(2) 0.0195(6) Uani 1 1 d . . . H33A H -0.412 0.0565 0.7342 0.023 Uiso 1 1 calc R . . H33B H -0.4398 0.1113 0.7863 0.023 Uiso 1 1 calc R . . N1 N -0.51627(19) -0.01588(12) 0.8022(3) 0.0369(7) Uani 1 1 d . . . C30 C -0.27686(19) -0.13216(13) 0.5168(3) 0.0269(7) Uani 1 1 d . . . H30A H -0.2809 -0.1732 0.5279 0.032 Uiso 1 1 calc R . . H30B H -0.2568 -0.1142 0.5871 0.032 Uiso 1 1 calc R . . N11 N -0.11838(15) 0.00394(11) 0.7120(2) 0.0217(5) Uani 1 1 d . . . C32 C -0.42336(18) -0.13199(13) 0.3795(2) 0.0214(6) Uani 1 1 d . . . H32 H -0.4228 -0.1669 0.3446 0.026 Uiso 1 1 calc R . . C13 C -0.05188(18) -0.13113(13) 0.8916(2) 0.0219(6) Uani 1 1 d . . . C9 C -0.29293(19) -0.13270(13) 0.8349(3) 0.0227(6) Uani 1 1 d . . . C14 C 0.01804(19) -0.15705(13) 0.9538(3) 0.0256(7) Uani 1 1 d . . . H14 H 0.0392 -0.1927 0.9422 0.031 Uiso 1 1 calc R . . C19 C -0.3358(2) 0.10113(16) 0.9934(3) 0.0319(8) Uani 1 1 d . . . H19 H -0.3815 0.094 1.0195 0.038 Uiso 1 1 calc R . . C12 C -0.11521(19) -0.15263(14) 0.7943(3) 0.0279(7) Uani 1 1 d . . . H12A H -0.0873 -0.1704 0.7457 0.033 Uiso 1 1 calc R . . H12B H -0.1473 -0.1204 0.7568 0.033 Uiso 1 1 calc R . . C6 C -0.5481(2) -0.05774(13) 0.7329(3) 0.0269(7) Uani 1 1 d . . . C20 C 0.1854(2) 0.11023(16) 0.8437(3) 0.0374(9) Uani 1 1 d . . . H20 H 0.2397 0.1138 0.8871 0.045 Uiso 1 1 calc R . . C26 C -0.05797(19) -0.03607(13) 0.5975(3) 0.0231(6) Uani 1 1 d . . . H26 H -0.0176 -0.0506 0.5673 0.028 Uiso 1 1 calc R . . C24 C 0.07053(19) 0.05487(14) 0.7745(3) 0.0239(7) Uani 1 1 d . . . C34 C -0.37185(17) 0.13092(12) 0.6819(2) 0.0196(6) Uani 1 1 d . . . C31 C -0.36151(18) -0.10912(12) 0.4617(2) 0.0195(6) Uani 1 1 d . . . F10 F 0.8827(2) 0.12999(12) 0.2550(2) 0.0815(9) Uani 1 1 d . . . C8 C -0.37486(19) -0.14397(13) 0.7853(3) 0.0246(7) Uani 1 1 d . . . H8 H -0.4026 -0.1787 0.7848 0.03 Uiso 1 1 calc R . . C37 C -0.2555(2) 0.19317(15) 0.6188(3) 0.0328(8) Uani 1 1 d . . . H37 H -0.2146 0.2133 0.5972 0.039 Uiso 1 1 calc R . . C15 C 0.12641(18) -0.12562(13) 1.1238(2) 0.0225(6) Uani 1 1 d . . . H15A H 0.1282 -0.1631 1.1573 0.027 Uiso 1 1 calc R . . H15B H 0.1266 -0.0967 1.1781 0.027 Uiso 1 1 calc R . . C7 C -0.49190(18) -0.08386(14) 0.6718(3) 0.0265(7) Uani 1 1 d . . . H7A H -0.516 -0.1199 0.6403 0.032 Uiso 1 1 calc R . . H7B H -0.4899 -0.0583 0.613 0.032 Uiso 1 1 calc R . . C22 C 0.0683(3) 0.15294(17) 0.7233(3) 0.0478(10) Uani 1 1 d . . . H22 H 0.0418 0.1846 0.6847 0.057 Uiso 1 1 calc R . . C23 C 0.0283(2) 0.10007(15) 0.7154(3) 0.0312(7) Uani 1 1 d . . . H23 H -0.0256 0.0954 0.6713 0.037 Uiso 1 1 calc R . . C25 C 0.03247(19) -0.00362(13) 0.7794(3) 0.0250(7) Uani 1 1 d . . . H25A H 0.0719 -0.0329 0.7721 0.03 Uiso 1 1 calc R . . H25B H 0.0225 -0.0084 0.8496 0.03 Uiso 1 1 calc R . . C36 C -0.3082(2) 0.22117(14) 0.6660(3) 0.0311(8) Uani 1 1 d . . . H36 H -0.3043 0.2607 0.6765 0.037 Uiso 1 1 calc R . . C5 C -0.6307(2) -0.07393(18) 0.7070(3) 0.0398(9) Uani 1 1 d . . . H5 H -0.6499 -0.1048 0.6608 0.048 Uiso 1 1 calc R . . C29 C -0.2146(2) -0.12152(16) 0.4521(3) 0.0358(9) Uani 1 1 d . . . H29A H -0.1641 -0.1427 0.485 0.043 Uiso 1 1 calc R . . H29B H -0.2373 -0.1363 0.3795 0.043 Uiso 1 1 calc R . . C2 C -0.6533(3) 0.0007(2) 0.8189(4) 0.0579(14) Uani 1 1 d . . . H2 H -0.6884 0.0227 0.8479 0.069 Uiso 1 1 calc R . . C11 C -0.1743(2) -0.19655(14) 0.8233(3) 0.0333(8) Uani 1 1 d . . . H11A H -0.2117 -0.2111 0.757 0.04 Uiso 1 1 calc R . . H11B H -0.1418 -0.2287 0.8604 0.04 Uiso 1 1 calc R . . C3C4 C -0.6840(3) -0.0435(2) 0.7509(4) 0.0581(13) Uani 1 1 d . . . H3C4 H -0.7401 -0.053 0.7342 0.07 Uiso 1 1 calc R . . C38 C -0.2639(2) 0.13427(14) 0.6037(3) 0.0292(7) Uani 1 1 d . . . H38 H -0.2286 0.1155 0.5701 0.035 Uiso 1 1 calc R . . C28 C -0.1929(2) -0.05813(16) 0.4455(3) 0.0317(8) Uani 1 1 d . . . H28A H -0.1621 -0.0536 0.3922 0.038 Uiso 1 1 calc R . . H28B H -0.244 -0.0362 0.4212 0.038 Uiso 1 1 calc R . . C1 C -0.5690(3) 0.01252(17) 0.8446(4) 0.0480(11) Uani 1 1 d . . . H1 H -0.5481 0.0417 0.8939 0.058 Uiso 1 1 calc R . . C16 C -0.20135(18) 0.11811(13) 0.9170(2) 0.0219(6) Uani 1 1 d . . . C17 C -0.2419(2) 0.16527(14) 0.9442(3) 0.0290(7) Uani 1 1 d . . . H17 H -0.2235 0.2023 0.9364 0.035 Uiso 1 1 calc R . . C18 C -0.3103(2) 0.15647(15) 0.9831(3) 0.0331(8) Uani 1 1 d . . . H18 H -0.3385 0.1875 1.002 0.04 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 Sb1 0.02072(12) 0.02329(12) 0.03532(13) -0.00464(9) 0.00811(9) 0.00162(8) Ag2 0.02099(13) 0.01412(12) 0.03991(15) -0.00184(10) 0.00333(10) 0.00268(9) Ag1 0.02315(13) 0.01987(13) 0.03109(14) -0.00842(9) 0.00584(10) 0.00009(9) Sb2 0.03442(14) 0.01934(12) 0.05102(16) 0.00008(10) 0.01440(11) 0.00796(9) F7 0.0645(17) 0.0534(16) 0.0729(18) -0.0254(13) 0.0273(14) -0.0148(13) F5 0.0423(13) 0.0632(16) 0.0416(13) -0.0010(11) -0.0065(10) -0.0012(12) F2 0.0710(16) 0.0341(12) 0.0611(15) 0.0020(11) 0.0345(13) -0.0194(11) F8 0.0551(15) 0.0348(12) 0.0748(17) 0.0175(12) 0.0226(13) 0.0059(11) N5 0.0199(13) 0.0157(12) 0.0231(13) -0.0007(10) 0.0023(10) -0.0001(10) F4 0.0541(14) 0.0233(11) 0.0793(17) -0.0104(11) 0.0084(12) -0.0083(10) N6 0.0212(13) 0.0126(12) 0.0254(13) -0.0018(10) 0.0025(11) 0.0015(10) N12 0.0183(13) 0.0199(13) 0.0248(13) -0.0007(10) 0.0059(11) -0.0005(10) F11 0.0799(19) 0.0294(12) 0.092(2) 0.0200(13) 0.0315(16) 0.0136(12) N15 0.0192(12) 0.0176(12) 0.0191(12) -0.0008(10) 0.0034(10) 0.0010(10) N4 0.0198(13) 0.0180(13) 0.0257(13) 0.0002(10) 0.0045(11) -0.0026(10) F6 0.0721(17) 0.0306(12) 0.095(2) 0.0032(12) 0.0630(16) 0.0061(11) N7 0.0175(12) 0.0154(12) 0.0255(13) -0.0001(10) 0.0018(10) 0.0011(10) F1 0.0554(15) 0.0852(19) 0.0469(14) -0.0247(13) 0.0243(12) 0.0096(14) N9 0.0202(14) 0.0300(15) 0.0408(17) -0.0110(13) 0.0083(12) -0.0050(12) F3 0.0421(15) 0.079(2) 0.085(2) 0.0257(16) -0.0166(14) 0.0059(13) F9 0.0333(13) 0.0505(15) 0.097(2) 0.0072(14) 0.0009(13) 0.0044(11) F12 0.0404(14) 0.0615(17) 0.127(3) 0.0196(17) 0.0369(16) 0.0143(12) N2 0.0196(13) 0.0183(13) 0.0282(14) -0.0036(11) 0.0061(11) -0.0005(10) N16 0.0181(13) 0.0199(13) 0.0230(13) -0.0011(10) 0.0034(10) -0.0006(10) N10 0.0155(12) 0.0172(13) 0.0307(14) -0.0022(10) 0.0051(11) -0.0012(10) N13 0.0211(13) 0.0220(13) 0.0228(13) -0.0045(10) 0.0034(11) 0.0014(10) C35 0.0280(17) 0.0202(16) 0.0265(16) -0.0026(13) 0.0031(13) 0.0030(13) N14 0.0225(13) 0.0205(13) 0.0247(14) -0.0070(11) 0.0030(11) 0.0015(10) C100 0.0277(17) 0.0282(18) 0.0309(18) 0.0012(14) 0.0083(14) 0.0010(14) C21 0.051(2) 0.035(2) 0.051(2) -0.0031(18) 0.0156(19) -0.0249(19) N8 0.0212(13) 0.0178(13) 0.0252(13) -0.0006(10) 0.0021(11) 0.0031(10) C27 0.0229(16) 0.0202(15) 0.0249(16) 0.0010(12) 0.0099(13) 0.0010(12) N3 0.0200(13) 0.0183(13) 0.0328(15) -0.0015(11) 0.0057(11) -0.0033(10) C10 0.0232(17) 0.0242(17) 0.0377(19) 0.0095(14) 0.0014(14) -0.0061(13) C33 0.0187(15) 0.0187(15) 0.0184(14) -0.0006(11) 0.0006(12) 0.0029(12) N1 0.0412(18) 0.0265(16) 0.0504(19) -0.0034(14) 0.0250(15) -0.0012(13) C30 0.0247(16) 0.0166(15) 0.0325(17) -0.0016(13) -0.0040(13) 0.0024(12) N11 0.0172(13) 0.0215(13) 0.0267(14) -0.0039(11) 0.0063(11) -0.0014(10) C32 0.0222(15) 0.0154(15) 0.0244(16) -0.0009(12) 0.0029(12) 0.0031(12) C13 0.0178(15) 0.0195(15) 0.0281(16) -0.0011(12) 0.0058(12) 0.0001(12) C9 0.0217(16) 0.0171(15) 0.0298(17) 0.0001(12) 0.0080(13) -0.0005(12) C14 0.0213(16) 0.0169(15) 0.0355(18) -0.0081(13) 0.0022(13) 0.0016(12) C19 0.0234(17) 0.043(2) 0.0291(18) -0.0032(15) 0.0060(14) 0.0069(15) C12 0.0216(16) 0.0292(18) 0.0301(17) -0.0112(14) 0.0022(13) 0.0035(13) C6 0.0240(16) 0.0202(16) 0.0370(18) 0.0096(14) 0.0093(14) 0.0028(13) C20 0.0295(19) 0.040(2) 0.045(2) -0.0127(17) 0.0145(16) -0.0134(16) C26 0.0227(16) 0.0196(15) 0.0298(17) -0.0009(13) 0.0118(13) -0.0007(12) C24 0.0218(16) 0.0270(17) 0.0266(16) -0.0070(13) 0.0127(13) -0.0048(13) C34 0.0171(14) 0.0205(15) 0.0162(14) 0.0001(11) -0.0037(11) 0.0019(12) C31 0.0193(15) 0.0153(14) 0.0226(15) -0.0005(12) 0.0039(12) -0.0007(11) F10 0.137(3) 0.0485(16) 0.0645(18) -0.0153(14) 0.0365(18) 0.0088(17) C8 0.0236(16) 0.0163(15) 0.0342(17) 0.0002(13) 0.0086(13) -0.0041(12) C37 0.0291(18) 0.0284(18) 0.038(2) 0.0080(15) 0.0048(15) -0.0072(15) C15 0.0229(16) 0.0170(15) 0.0220(15) 0.0025(12) -0.0034(12) 0.0010(12) C7 0.0194(15) 0.0220(16) 0.0340(18) -0.0058(13) 0.0005(13) -0.0004(12) C22 0.057(3) 0.030(2) 0.053(2) 0.0109(18) 0.010(2) -0.0107(19) C23 0.0290(18) 0.0299(18) 0.0341(18) 0.0033(14) 0.0079(14) -0.0080(14) C25 0.0189(15) 0.0213(16) 0.0332(18) -0.0028(13) 0.0041(13) 0.0001(12) C36 0.039(2) 0.0188(16) 0.0318(18) 0.0000(14) 0.0024(15) -0.0020(14) C5 0.0256(18) 0.049(2) 0.044(2) 0.0163(18) 0.0086(16) 0.0010(16) C29 0.0211(17) 0.040(2) 0.042(2) -0.0227(17) 0.0006(15) 0.0060(15) C2 0.060(3) 0.063(3) 0.066(3) 0.035(3) 0.043(3) 0.039(2) C11 0.0236(17) 0.0178(16) 0.048(2) -0.0081(15) -0.0070(15) 0.0029(13) C3C4 0.030(2) 0.081(4) 0.068(3) 0.031(3) 0.022(2) 0.018(2) C38 0.0246(17) 0.0298(18) 0.0339(18) 0.0033(14) 0.0090(14) 0.0007(14) C28 0.0226(17) 0.050(2) 0.0248(17) -0.0007(15) 0.0099(14) 0.0016(15) C1 0.069(3) 0.029(2) 0.060(3) 0.0065(18) 0.040(2) 0.0111(19) C16 0.0189(15) 0.0187(15) 0.0211(15) -0.0011(12) -0.0063(12) 0.0017(12) C17 0.0246(17) 0.0191(16) 0.0368(19) -0.0066(14) -0.0026(14) 0.0034(13) C18 0.0262(18) 0.0316(19) 0.0357(19) -0.0129(15) -0.0012(14) 0.0096(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sb1 F5 1.866(2) . ? Sb1 F1 1.861(2) . ? Sb1 F4 1.867(2) . ? Sb1 F6 1.858(2) . ? Sb1 F2 1.865(2) . ? Sb1 F3 1.855(2) . ? Ag2 N5 2.231(2) . ? Ag2 N8 2.247(2) . ? Ag2 N4 2.393(2) . ? Ag1 N13 2.228(3) . ? Ag1 N16 2.245(3) . ? Ag1 N12 2.407(3) . ? Ag1 N3 2.521(3) . ? Sb2 F10 1.845(3) . ? Sb2 F11 1.859(2) . ? Sb2 F12 1.858(3) . ? Sb2 F7 1.868(3) . ? Sb2 F9 1.873(2) . ? Sb2 F8 1.871(2) . ? N5 N6 1.316(3) . ? N5 C13 1.360(4) . ? N6 N7 1.336(3) . ? N12 N11 1.324(4) . ? N12 C27 1.355(4) . ? N15 N14 1.330(3) . ? N15 C32 1.344(4) . ? N15 C33 1.464(4) 3_456 ? N4 N3 1.326(3) . ? N4 C9 1.363(4) . ? N7 C14 1.341(4) . ? N7 C15 1.466(4) . ? N9 C24 1.341(4) . ? N9 C20 1.339(4) . ? N2 N3 1.342(3) . ? N2 C8 1.343(4) . ? N2 C7 1.461(4) . ? N16 C34 1.341(4) . ? N16 C38 1.343(4) . ? N10 C26 1.336(4) . ? N10 N11 1.341(3) . ? N10 C25 1.468(4) . ? N13 N14 1.324(3) . ? N13 C31 1.357(4) . ? C35 C36 1.375(5) . ? C35 C34 1.385(4) . ? C35 H35 0.93 . ? C100 N8 1.333(4) . ? C100 C19 1.388(5) . ? C100 H100 0.93 . ? C21 C22 1.380(6) . ? C21 C20 1.356(6) . ? C21 H21 0.93 . ? N8 C16 1.343(4) . ? C27 C26 1.375(4) . ? C27 C28 1.495(4) . ? C10 C9 1.497(4) . ? C10 C11 1.511(5) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C33 N15 1.464(4) 3_456 ? C33 C34 1.501(4) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? N1 C6 1.329(4) . ? N1 C1 1.332(5) . ? C30 C31 1.498(4) . ? C30 C29 1.520(5) . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? C32 C31 1.368(4) . ? C32 H32 0.93 . ? C13 C14 1.363(4) . ? C13 C12 1.488(4) . ? C9 C8 1.369(4) . ? C14 H14 0.93 . ? C19 C18 1.374(5) . ? C19 H19 0.93 . ? C12 C11 1.537(5) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C6 C5 1.381(5) . ? C6 C7 1.509(5) . ? C20 H20 0.93 . ? C26 H26 0.93 . ? C24 C23 1.374(5) . ? C24 C25 1.510(4) . ? C8 H8 0.93 . ? C37 C38 1.385(5) . ? C37 C36 1.366(5) . ? C37 H37 0.93 . ? C15 C16 1.496(4) 3_557 ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C22 C23 1.390(5) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C36 H36 0.93 . ? C5 C3C4 1.375(6) . ? C5 H5 0.93 . ? C29 C28 1.526(5) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C2 C3C4 1.356(7) . ? C2 C1 1.385(7) . ? C2 H2 0.93 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C3C4 H3C4 0.93 . ? C38 H38 0.93 . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C1 H1 0.93 . ? C16 C17 1.384(4) . ? C16 C15 1.496(4) 3_557 ? C17 C18 1.383(5) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? 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 F5 Sb1 F1 89.73(12) . . ? F5 Sb1 F4 89.47(11) . . ? F1 Sb1 F4 90.68(12) . . ? F5 Sb1 F6 89.27(12) . . ? F1 Sb1 F6 178.55(12) . . ? F4 Sb1 F6 90.36(11) . . ? F5 Sb1 F2 90.61(12) . . ? F1 Sb1 F2 88.97(12) . . ? F4 Sb1 F2 179.64(11) . . ? F6 Sb1 F2 89.99(10) . . ? F5 Sb1 F3 179.26(12) . . ? F1 Sb1 F3 90.09(14) . . ? F4 Sb1 F3 89.81(12) . . ? F6 Sb1 F3 90.92(14) . . ? F2 Sb1 F3 90.10(12) . . ? N5 Ag2 N8 150.54(9) . . ? N5 Ag2 N4 101.85(9) . . ? N8 Ag2 N4 100.96(9) . . ? N13 Ag1 N16 140.03(9) . . ? N13 Ag1 N12 104.66(9) . . ? N16 Ag1 N12 100.44(9) . . ? N13 Ag1 N3 88.99(9) . . ? N16 Ag1 N3 115.13(9) . . ? N12 Ag1 N3 102.90(8) . . ? F10 Sb2 F11 91.18(13) . . ? F10 Sb2 F12 91.04(15) . . ? F11 Sb2 F12 90.57(12) . . ? F10 Sb2 F7 179.09(13) . . ? F11 Sb2 F7 89.54(13) . . ? F12 Sb2 F7 89.51(14) . . ? F10 Sb2 F9 91.12(15) . . ? F11 Sb2 F9 90.12(12) . . ? F12 Sb2 F9 177.72(15) . . ? F7 Sb2 F9 88.32(12) . . ? F10 Sb2 F8 89.22(13) . . ? F11 Sb2 F8 179.45(12) . . ? F12 Sb2 F8 89.80(11) . . ? F7 Sb2 F8 90.05(12) . . ? F9 Sb2 F8 89.50(11) . . ? N6 N5 C13 110.1(2) . . ? N6 N5 Ag2 121.66(18) . . ? C13 N5 Ag2 128.13(19) . . ? N5 N6 N7 106.2(2) . . ? N11 N12 C27 109.5(2) . . ? N11 N12 Ag1 122.15(19) . . ? C27 N12 Ag1 128.3(2) . . ? N14 N15 C32 111.8(2) . . ? N14 N15 C33 119.5(2) . 3_456 ? C32 N15 C33 128.7(2) . 3_456 ? N3 N4 C9 109.5(2) . . ? N3 N4 Ag2 119.32(18) . . ? C9 N4 Ag2 130.3(2) . . ? N6 N7 C14 111.1(2) . . ? N6 N7 C15 119.7(2) . . ? C14 N7 C15 129.1(3) . . ? C24 N9 C20 116.6(3) . . ? N3 N2 C8 110.9(2) . . ? N3 N2 C7 121.2(2) . . ? C8 N2 C7 127.9(3) . . ? C34 N16 C38 117.6(3) . . ? C34 N16 Ag1 124.9(2) . . ? C38 N16 Ag1 117.5(2) . . ? C26 N10 N11 111.0(2) . . ? C26 N10 C25 128.7(3) . . ? N11 N10 C25 120.3(2) . . ? N14 N13 C31 110.0(2) . . ? N14 N13 Ag1 121.04(19) . . ? C31 N13 Ag1 128.91(19) . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N13 N14 N15 105.9(2) . . ? N8 C100 C19 123.0(3) . . ? N8 C100 H100 118.5 . . ? C19 C100 H100 118.5 . . ? C22 C21 C20 119.0(3) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C100 N8 C16 117.9(3) . . ? C100 N8 Ag2 116.4(2) . . ? C16 N8 Ag2 125.7(2) . . ? N12 C27 C26 107.3(3) . . ? N12 C27 C28 122.7(3) . . ? C26 C27 C28 129.9(3) . . ? N4 N3 N2 106.6(2) . . ? N4 N3 Ag1 111.05(18) . . ? N2 N3 Ag1 122.95(19) . . ? C9 C10 C11 113.4(3) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N15 C33 C34 112.6(2) 3_456 . ? N15 C33 H33A 109.1 3_456 . ? C34 C33 H33A 109.1 . . ? N15 C33 H33B 109.1 3_456 . ? C34 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C6 N1 C1 116.7(3) . . ? C31 C30 C29 112.5(3) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? N12 N11 N10 106.6(2) . . ? N15 C32 C31 105.1(3) . . ? N15 C32 H32 127.4 . . ? C31 C32 H32 127.4 . . ? N5 C13 C14 106.8(3) . . ? N5 C13 C12 123.0(3) . . ? C14 C13 C12 130.1(3) . . ? N4 C9 C8 107.2(3) . . ? N4 C9 C10 123.2(3) . . ? C8 C9 C10 129.5(3) . . ? N7 C14 C13 105.8(3) . . ? N7 C14 H14 127.1 . . ? C13 C14 H14 127.1 . . ? C18 C19 C100 118.8(3) . . ? C18 C19 H19 120.6 . . ? C100 C19 H19 120.6 . . ? C13 C12 C11 112.1(3) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N1 C6 C5 123.5(3) . . ? N1 C6 C7 116.9(3) . . ? C5 C6 C7 119.2(3) . . ? N9 C20 C21 124.0(3) . . ? N9 C20 H20 118 . . ? C21 C20 H20 118 . . ? N10 C26 C27 105.6(3) . . ? N10 C26 H26 127.2 . . ? C27 C26 H26 127.2 . . ? N9 C24 C23 123.7(3) . . ? N9 C24 C25 112.7(3) . . ? C23 C24 C25 123.6(3) . . ? N16 C34 C35 122.0(3) . . ? N16 C34 C33 117.1(3) . . ? C35 C34 C33 120.9(3) . . ? N13 C31 C32 107.2(3) . . ? N13 C31 C30 122.8(3) . . ? C32 C31 C30 130.0(3) . . ? N2 C8 C9 105.9(3) . . ? N2 C8 H8 127.1 . . ? C9 C8 H8 127.1 . . ? C38 C37 C36 118.7(3) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? N7 C15 C16 110.6(2) . 3_557 ? N7 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 3_557 . ? N7 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 3_557 . ? H15A C15 H15B 108.1 . . ? N2 C7 C6 114.3(3) . . ? N2 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C21 C22 C23 118.6(4) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C22 C23 C24 118.1(3) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N10 C25 C24 113.6(3) . . ? N10 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N10 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C35 C36 C37 118.9(3) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C3C4 C5 C6 118.5(4) . . ? C3C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C28 C29 C30 113.4(3) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C3C4 C2 C1 119.0(4) . . ? C3C4 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C10 C11 C12 114.1(3) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C2 C3C4 C5 118.9(4) . . ? C2 C3C4 H3C4 120.6 . . ? C5 C3C4 H3C4 120.6 . . ? N16 C38 C37 123.1(3) . . ? N16 C38 H38 118.4 . . ? C37 C38 H38 118.4 . . ? C27 C28 C29 113.1(3) . . ? C27 C28 H28A 109 . . ? C29 C28 H28A 109 . . ? C27 C28 H28B 109 . . ? C29 C28 H28B 109 . . ? H28A C28 H28B 107.8 . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N8 C16 C17 122.4(3) . . ? N8 C16 C15 116.8(3) . 3_557 ? C17 C16 C15 120.8(3) . 3_557 ? C18 C17 C16 119.0(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C19 C18 C17 118.9(3) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? # END of CIF # Attachment 'jc276DaltonNEW28082009.cif' data_jc276 _database_code_depnum_ccdc_archive 'CCDC 734030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Ag2 N16, 2(F6 Sb)' _chemical_formula_sum 'C44 H36 Ag2 F12 N16 Sb2' _chemical_formula_weight 1476.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.495(7) _cell_length_b 14.440(14) _cell_length_c 22.888(3) _cell_angle_alpha 80.209(6) _cell_angle_beta 85.380(5) _cell_angle_gamma 84.307(5) _cell_volume 2423(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9436 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.57 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50393 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8764 _reflns_number_gt 7443 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.2000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8764 _refine_ls_number_parameters 735 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1105(5) 0.6113(3) 0.46209(18) 0.0317(9) Uani 1 1 d . . . H1 H 0.1105 0.5728 0.4334 0.038 Uiso 1 1 calc R . . C2 C 0.0304(5) 0.7026(3) 0.45090(18) 0.0297(9) Uani 1 1 d . . . H2 H -0.0231 0.7244 0.4153 0.036 Uiso 1 1 calc R . . C3 C 0.0300(5) 0.7605(3) 0.49215(17) 0.0263(9) Uani 1 1 d . . . H3 H -0.0203 0.8225 0.4848 0.032 Uiso 1 1 calc R . . C4 C 0.1069(4) 0.7243(3) 0.54557(17) 0.0228(8) Uani 1 1 d . . . H4 H 0.1054 0.7616 0.5750 0.027 Uiso 1 1 calc R . . C5 C 0.1856(4) 0.6328(3) 0.55457(16) 0.0172(7) Uani 1 1 d . . . C6 C 0.2706(4) 0.5929(3) 0.61014(17) 0.0190(7) Uani 1 1 d . . . C7 C 0.2921(4) 0.6341(3) 0.65864(16) 0.0217(8) Uani 1 1 d . . . H8 H 0.2501 0.6946 0.6650 0.026 Uiso 1 1 calc R . . C8 C 0.4493(7) 0.5720(3) 0.7544(2) 0.0458(13) Uani 1 1 d . . . H9A H 0.5677 0.5386 0.7582 0.055 Uiso 1 1 calc R . . H9B H 0.3682 0.5406 0.7849 0.055 Uiso 1 1 calc R . . C9 C 0.4573(6) 0.6724(3) 0.76411(17) 0.0291(9) Uani 1 1 d . . . C10 C 0.3137(5) 0.7115(3) 0.79809(17) 0.0303(9) Uani 1 1 d . . . H11 H 0.2177 0.6760 0.8124 0.036 Uiso 1 1 calc R . . C11 C 0.6868(5) 0.1982(3) 0.18944(17) 0.0282(9) Uani 1 1 d . . . H11A H 0.7833 0.1730 0.1672 0.034 Uiso 1 1 calc R . . C12 C 0.5444(5) 0.1454(3) 0.20995(17) 0.0307(9) Uani 1 1 d . . . H12A H 0.5439 0.0847 0.2014 0.037 Uiso 1 1 calc R . . C13 C 0.4015(5) 0.1835(3) 0.24350(18) 0.0312(9) Uani 1 1 d . . . H13A H 0.3053 0.1478 0.2571 0.037 Uiso 1 1 calc R . . C14 C 0.3996(5) 0.2736(3) 0.25707(17) 0.0272(9) Uani 1 1 d . . . C15 C 0.2393(6) 0.3106(4) 0.2936(2) 0.0498(15) Uani 1 1 d . . . H15C H 0.2029 0.3752 0.2764 0.060 Uiso 1 1 calc R . . H15D H 0.1395 0.2731 0.2927 0.060 Uiso 1 1 calc R . . C16 C 0.3577(5) 0.2355(3) 0.39338(18) 0.0274(9) Uani 1 1 d . . . H16A H 0.3929 0.1745 0.3865 0.033 Uiso 1 1 calc R . . C17 C 0.3719(4) 0.2722(3) 0.44440(16) 0.0205(8) Uani 1 1 d . . . C18 C 0.4492(4) 0.2279(3) 0.50086(17) 0.0212(8) Uani 1 1 d . . . C19 C 0.5112(5) 0.1334(3) 0.5115(2) 0.0344(10) Uani 1 1 d . . . H19A H 0.5012 0.0948 0.4835 0.041 Uiso 1 1 calc R . . C20 C 0.5886(6) 0.0974(4) 0.5645(2) 0.0501(14) Uani 1 1 d . . . H20A H 0.6291 0.0339 0.5731 0.060 Uiso 1 1 calc R . . C21 C 0.6046(6) 0.1563(4) 0.6041(2) 0.0510(15) Uani 1 1 d . . . H21A H 0.6601 0.1340 0.6393 0.061 Uiso 1 1 calc R . . C22 C 0.5384(5) 0.2482(4) 0.59144(19) 0.0396(12) Uani 1 1 d . . . H22A H 0.5465 0.2870 0.6195 0.048 Uiso 1 1 calc R . . C23 C 0.5726(5) 0.2559(4) 1.03105(19) 0.0357(10) Uani 1 1 d . . . H1B H 0.6315 0.2223 1.0634 0.043 Uiso 1 1 calc R . . C24 C 0.4993(5) 0.3464(3) 1.03439(19) 0.0344(10) Uani 1 1 d . . . H2B H 0.5070 0.3725 1.0684 0.041 Uiso 1 1 calc R . . C25 C 0.4138(5) 0.3979(3) 0.9860(2) 0.0349(10) Uani 1 1 d . . . H3B H 0.3607 0.4586 0.9872 0.042 Uiso 1 1 calc R . . C26 C 0.4099(5) 0.3561(3) 0.93599(19) 0.0280(9) Uani 1 1 d . . . H4B H 0.3586 0.3900 0.9023 0.034 Uiso 1 1 calc R . . C27 C 0.4821(4) 0.2642(3) 0.93613(17) 0.0235(8) Uani 1 1 d . . . C28 C 0.4678(4) 0.2162(3) 0.88490(17) 0.0213(8) Uani 1 1 d . . . C29 C 0.3692(4) 0.2433(3) 0.83618(17) 0.0242(8) Uani 1 1 d . . . H7B H 0.3008 0.3002 0.8256 0.029 Uiso 1 1 calc R . . C30 C 0.6767(5) -0.1583(3) 1.25005(17) 0.0280(9) Uani 1 1 d . . . H15A H 0.5885 -0.1768 1.2823 0.034 Uiso 1 1 calc R . . H15B H 0.6938 -0.0924 1.2493 0.034 Uiso 1 1 calc R . . C31 C 0.8529(4) -0.2171(3) 1.26181(16) 0.0201(8) Uani 1 1 d . . . C32 C 0.8482(5) -0.3078(3) 1.29394(16) 0.0249(8) Uani 1 1 d . . . H13C H 0.7377 -0.3302 1.3076 0.030 Uiso 1 1 calc R . . C33 C 1.0039(6) -0.3653(3) 1.30606(17) 0.0293(9) Uani 1 1 d . . . H12C H 0.9978 -0.4255 1.3279 0.035 Uiso 1 1 calc R . . C34 C 1.1675(5) -0.3333(3) 1.28571(17) 0.0295(9) Uani 1 1 d . . . H11C H 1.2726 -0.3720 1.2935 0.035 Uiso 1 1 calc R . . C35 C 1.1761(5) -0.2427(3) 1.25344(18) 0.0266(9) Uani 1 1 d . . . H10C H 1.2874 -0.2210 1.2402 0.032 Uiso 1 1 calc R . . C36 C 1.0192(4) -0.1840(3) 1.24060(15) 0.0178(7) Uani 1 1 d . . . C37 C 1.0342(5) -0.0863(3) 1.20473(16) 0.0224(8) Uani 1 1 d . . . H8C1 H 0.9632 -0.0402 1.2252 0.027 Uiso 1 1 calc R . . H8C2 H 1.1585 -0.0716 1.2017 0.027 Uiso 1 1 calc R . . C38 C 1.0028(4) -0.1422(3) 1.10668(16) 0.0211(8) Uani 1 1 d . . . H7C H 1.0719 -0.1997 1.1123 0.025 Uiso 1 1 calc R . . C39 C 0.9097(5) -0.1020(3) 1.05783(16) 0.0212(8) Uani 1 1 d . . . C40 C 0.8852(4) -0.1362(3) 1.00205(16) 0.0221(8) Uani 1 1 d . . . C41 C 0.9650(5) -0.2232(3) 0.99180(17) 0.0242(8) Uani 1 1 d . . . H4C H 1.0346 -0.2610 1.0200 0.029 Uiso 1 1 calc R . . C42 C 0.9394(5) -0.2535(3) 0.93836(18) 0.0291(9) Uani 1 1 d . . . H3C H 0.9903 -0.3118 0.9304 0.035 Uiso 1 1 calc R . . C43 C 0.8364(5) -0.1940(3) 0.89796(18) 0.0321(9) Uani 1 1 d . . . H2C H 0.8183 -0.2114 0.8617 0.039 Uiso 1 1 calc R . . C44 C 0.7597(5) -0.1079(3) 0.91162(17) 0.0290(9) Uani 1 1 d . . . H1C H 0.6896 -0.0687 0.8842 0.035 Uiso 1 1 calc R . . N1 N 0.1884(4) 0.5766(2) 0.51317(15) 0.0252(7) Uani 1 1 d . . . N2 N 0.3528(4) 0.5028(2) 0.61963(15) 0.0246(7) Uani 1 1 d . . . N3 N 0.4231(4) 0.4882(2) 0.67175(16) 0.0309(8) Uani 1 1 d . . . N4 N 0.3870(4) 0.5678(2) 0.69483(15) 0.0292(8) Uani 1 1 d . . . N5 N 0.2817(4) 0.3074(3) 0.35597(15) 0.0323(8) Uani 1 1 d . . . N6 N 0.2486(4) 0.3866(3) 0.38088(14) 0.0305(8) Uani 1 1 d . . . N7 N 0.3029(4) 0.3641(2) 0.43500(14) 0.0229(7) Uani 1 1 d . . . N8 N 0.4620(4) 0.2858(3) 0.54070(15) 0.0267(7) Uani 1 1 d . . . N9 N 0.5636(4) 0.2135(3) 0.98346(14) 0.0259(7) Uani 1 1 d . . . N10 N 0.5482(4) 0.1271(2) 0.88255(15) 0.0266(7) Uani 1 1 d . . . N11 N 0.5017(4) 0.0993(2) 0.83460(15) 0.0273(7) Uani 1 1 d . . . N12 N 0.3932(3) 0.1693(2) 0.80691(14) 0.0220(7) Uani 1 1 d . . . N13 N 0.9713(4) -0.0796(2) 1.14431(13) 0.0197(6) Uani 1 1 d . . . N14 N 0.8666(4) -0.0028(2) 1.12190(14) 0.0234(7) Uani 1 1 d . . . N15 N 0.8289(4) -0.0164(2) 1.06847(14) 0.0239(7) Uani 1 1 d . . . N16 N 0.7834(4) -0.0796(2) 0.96280(14) 0.0247(7) Uani 1 1 d . . . Ag1 Ag 0.33959(4) 0.43458(2) 0.524919(16) 0.03469(12) Uani 1 1 d . . . Ag2 Ag 0.66579(4) 0.06330(2) 0.986027(14) 0.03051(12) Uani 1 1 d . . . Sb1 Sb 0.91274(3) 0.483082(18) 0.861650(11) 0.02492(11) Uani 1 1 d . . . Sb2 Sb 0.08956(3) 0.960742(19) 0.641128(11) 0.02669(11) Uani 1 1 d . . . F7 F -0.0831(6) 0.9197(4) 0.6003(3) 0.0453(13) Uani 0.648(4) 1 d P A 1 F8 F 0.0683(6) 0.8318(3) 0.6790(2) 0.0541(13) Uani 0.648(4) 1 d P A 1 F9 F 0.2885(6) 0.9155(4) 0.5995(2) 0.0573(14) Uani 0.648(4) 1 d P A 1 F10 F -0.1280(5) 0.9937(3) 0.68588(18) 0.0436(11) Uani 0.648(4) 1 d P A 1 F11 F 0.0924(7) 1.0814(3) 0.6046(2) 0.0593(14) Uani 0.648(4) 1 d P A 1 F12 F 0.2710(9) 1.0030(5) 0.6820(4) 0.079(2) Uani 0.648(4) 1 d P A 1 F7' F 0.1893(9) 1.0155(6) 0.5636(3) 0.0396(19) Uiso 0.352(4) 1 d P A 2 F8' F 0.0142(9) 0.9142(6) 0.7158(3) 0.0395(19) Uiso 0.352(4) 1 d P A 2 F9' F 0.2502(9) 0.8538(5) 0.6346(3) 0.0339(18) Uiso 0.352(4) 1 d P A 2 F10' F -0.0416(13) 0.9432(8) 0.5777(4) 0.044(3) Uiso 0.352(4) 1 d P A 2 F11' F -0.0364(10) 1.0802(6) 0.6459(4) 0.044(2) Uiso 0.352(4) 1 d P A 2 F12' F 0.2080(10) 0.9735(6) 0.7037(4) 0.0262(19) Uiso 0.352(4) 1 d P A 2 F1 F 1.0312(4) 0.3608(2) 0.86446(15) 0.0337(8) Uani 0.807(4) 1 d P B 1 F2 F 0.7112(4) 0.4365(3) 0.83498(16) 0.0508(10) Uani 0.807(4) 1 d P B 1 F3 F 0.9998(6) 0.5153(3) 0.78341(14) 0.0555(11) Uani 0.807(4) 1 d P B 1 F4 F 0.7895(6) 0.6014(3) 0.85896(17) 0.0577(12) Uani 0.807(4) 1 d P B 1 F5 F 1.1122(4) 0.5251(2) 0.88885(15) 0.0369(8) Uani 0.807(4) 1 d P B 1 F6 F 0.8236(4) 0.4460(3) 0.94077(13) 0.0412(9) Uani 0.807(4) 1 d P B 1 F1' F 0.9291(15) 0.6171(9) 0.8310(6) 0.031(3) Uiso 0.193(4) 1 d P B 2 F2' F 0.825(2) 0.4732(12) 0.7909(7) 0.052(4) Uiso 0.193(4) 1 d P B 2 F3' F 1.155(2) 0.4596(12) 0.8246(7) 0.056(4) Uiso 0.193(4) 1 d P B 2 F4' F 0.686(2) 0.5163(14) 0.8921(8) 0.067(5) Uiso 0.193(4) 1 d P B 2 F5' F 0.920(3) 0.3577(15) 0.8881(8) 0.067(5) Uiso 0.193(4) 1 d P B 2 F6' F 1.027(3) 0.5060(18) 0.9285(10) 0.089(7) Uiso 0.193(4) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(2) 0.031(2) 0.022(2) -0.0115(19) -0.0046(17) -0.0080(19) C2 0.0341(19) 0.032(2) 0.023(2) -0.0021(19) -0.0115(16) -0.0022(17) C3 0.0253(18) 0.025(2) 0.027(2) -0.0011(18) -0.0043(15) 0.0003(16) C4 0.0216(16) 0.026(2) 0.023(2) -0.0093(17) -0.0013(14) -0.0029(15) C5 0.0178(15) 0.0152(18) 0.0199(19) -0.0063(15) 0.0015(13) -0.0044(13) C6 0.0172(15) 0.0147(18) 0.027(2) -0.0065(16) -0.0006(14) -0.0043(13) C7 0.0229(16) 0.0144(18) 0.028(2) -0.0052(16) -0.0057(14) 0.0026(14) C8 0.082(3) 0.025(2) 0.037(3) -0.014(2) -0.035(2) 0.008(2) C9 0.047(2) 0.023(2) 0.017(2) -0.0008(17) -0.0184(17) 0.0066(18) C10 0.039(2) 0.035(2) 0.016(2) 0.0008(18) -0.0050(16) -0.0054(19) C11 0.039(2) 0.029(2) 0.015(2) -0.0072(17) -0.0027(16) 0.0066(18) C12 0.050(2) 0.020(2) 0.024(2) -0.0081(17) -0.0147(18) 0.0055(18) C13 0.036(2) 0.039(3) 0.020(2) -0.0038(19) -0.0112(16) -0.0065(19) C14 0.0306(18) 0.033(2) 0.017(2) -0.0052(17) -0.0129(15) 0.0101(17) C15 0.037(2) 0.087(4) 0.027(2) -0.023(3) -0.0149(19) 0.021(3) C16 0.0233(17) 0.029(2) 0.032(2) -0.0142(19) -0.0003(16) 0.0017(16) C17 0.0224(16) 0.0134(18) 0.025(2) -0.0013(15) 0.0015(14) -0.0034(14) C18 0.0195(16) 0.0170(19) 0.026(2) -0.0019(16) 0.0046(14) -0.0015(14) C19 0.037(2) 0.018(2) 0.045(3) 0.0006(19) 0.0010(19) -0.0029(17) C20 0.040(2) 0.042(3) 0.056(3) 0.018(3) 0.006(2) 0.006(2) C21 0.032(2) 0.078(4) 0.031(3) 0.015(3) 0.0014(19) 0.011(2) C22 0.031(2) 0.065(4) 0.022(2) -0.010(2) 0.0005(17) 0.003(2) C23 0.0296(19) 0.050(3) 0.028(2) -0.008(2) 0.0009(17) -0.0064(19) C24 0.0282(19) 0.047(3) 0.033(2) -0.021(2) 0.0026(17) -0.0074(19) C25 0.0261(19) 0.033(2) 0.049(3) -0.015(2) -0.0018(18) -0.0056(17) C26 0.0225(17) 0.027(2) 0.036(2) -0.0059(19) -0.0069(16) -0.0047(15) C27 0.0153(15) 0.028(2) 0.027(2) -0.0011(17) -0.0018(14) -0.0043(14) C28 0.0124(14) 0.022(2) 0.029(2) -0.0037(17) -0.0006(13) -0.0015(13) C29 0.0212(16) 0.023(2) 0.028(2) -0.0038(17) -0.0027(14) 0.0001(15) C30 0.0211(17) 0.042(3) 0.023(2) -0.0122(19) -0.0016(14) 0.0015(16) C31 0.0231(16) 0.022(2) 0.0167(18) -0.0071(16) -0.0032(14) -0.0001(14) C32 0.0303(18) 0.027(2) 0.0183(19) -0.0035(16) 0.0027(14) -0.0086(16) C33 0.048(2) 0.021(2) 0.018(2) -0.0028(17) -0.0044(17) 0.0038(18) C34 0.0327(19) 0.033(2) 0.021(2) -0.0056(18) -0.0109(16) 0.0133(17) C35 0.0210(17) 0.035(2) 0.026(2) -0.0128(18) -0.0039(15) 0.0003(16) C36 0.0224(16) 0.0203(19) 0.0121(17) -0.0062(15) -0.0037(13) -0.0007(14) C37 0.0291(17) 0.0195(19) 0.021(2) -0.0063(16) -0.0012(14) -0.0061(15) C38 0.0228(16) 0.0165(18) 0.023(2) -0.0031(16) 0.0020(14) -0.0017(14) C39 0.0248(17) 0.0189(19) 0.0203(19) -0.0024(16) -0.0003(14) -0.0063(14) C40 0.0216(16) 0.023(2) 0.021(2) 0.0012(16) -0.0001(14) -0.0062(14) C41 0.0296(18) 0.024(2) 0.019(2) -0.0028(17) -0.0008(15) -0.0058(16) C42 0.041(2) 0.021(2) 0.027(2) -0.0094(18) 0.0007(17) -0.0050(17) C43 0.042(2) 0.035(2) 0.023(2) -0.0106(19) -0.0043(17) -0.0114(19) C44 0.034(2) 0.034(2) 0.018(2) 0.0026(18) -0.0045(15) -0.0090(18) N1 0.0300(16) 0.0210(17) 0.0257(18) -0.0075(15) 0.0007(13) -0.0028(13) N2 0.0297(15) 0.0134(16) 0.0316(19) -0.0062(14) -0.0052(13) -0.0001(13) N3 0.0389(18) 0.0169(17) 0.039(2) -0.0115(16) -0.0105(15) 0.0047(14) N4 0.0412(18) 0.0192(17) 0.0283(19) -0.0073(15) -0.0105(14) 0.0041(14) N5 0.0301(16) 0.042(2) 0.0265(19) -0.0186(17) -0.0043(14) 0.0122(16) N6 0.0324(16) 0.035(2) 0.0214(18) -0.0031(16) -0.0024(13) 0.0099(15) N7 0.0279(15) 0.0183(17) 0.0221(17) -0.0054(14) 0.0020(12) 0.0000(13) N8 0.0232(14) 0.0313(19) 0.0237(18) -0.0037(15) 0.0043(13) 0.0012(14) N9 0.0199(14) 0.0317(19) 0.0237(18) 0.0004(15) -0.0002(12) -0.0003(13) N10 0.0246(15) 0.0217(17) 0.0342(19) -0.0033(15) -0.0102(13) -0.0013(13) N11 0.0247(15) 0.0257(18) 0.0316(19) -0.0035(15) -0.0057(13) -0.0023(13) N12 0.0148(13) 0.0264(18) 0.0243(17) -0.0016(14) -0.0021(11) -0.0029(12) N13 0.0238(14) 0.0174(16) 0.0179(16) -0.0012(13) -0.0024(12) -0.0042(12) N14 0.0283(15) 0.0215(17) 0.0211(17) -0.0073(14) 0.0010(13) -0.0016(13) N15 0.0271(15) 0.0238(18) 0.0201(17) -0.0027(14) -0.0002(12) -0.0004(13) N16 0.0286(15) 0.0258(18) 0.0209(18) -0.0024(15) -0.0025(13) -0.0101(14) Ag1 0.0398(2) 0.0233(2) 0.0439(2) -0.01895(16) 0.00745(15) -0.00185(14) Ag2 0.03045(18) 0.0252(2) 0.0319(2) 0.00518(15) -0.00396(13) 0.00121(14) Sb1 0.03298(17) 0.02092(18) 0.01937(18) -0.00491(12) -0.00517(11) 0.01061(12) Sb2 0.03607(17) 0.02286(18) 0.02137(18) -0.00917(13) -0.00800(12) 0.01089(12) F7 0.030(2) 0.035(3) 0.076(4) -0.016(3) -0.014(2) -0.009(2) F8 0.066(3) 0.017(2) 0.076(3) -0.001(2) -0.012(2) 0.0048(19) F9 0.049(2) 0.068(4) 0.055(3) -0.029(3) 0.008(2) 0.017(2) F10 0.041(2) 0.041(3) 0.046(3) -0.013(2) 0.0035(18) 0.0083(18) F11 0.079(3) 0.031(2) 0.058(3) 0.015(2) 0.000(2) 0.003(2) F12 0.083(4) 0.063(4) 0.110(6) -0.059(4) -0.075(4) 0.034(4) F1 0.0321(15) 0.0204(16) 0.046(2) -0.0005(14) -0.0051(14) 0.0055(12) F2 0.0425(18) 0.059(3) 0.056(2) -0.022(2) -0.0284(17) 0.0134(17) F3 0.103(3) 0.034(2) 0.0263(18) 0.0001(15) 0.0105(18) -0.007(2) F4 0.081(3) 0.037(2) 0.054(2) -0.0156(18) -0.025(2) 0.033(2) F5 0.0370(15) 0.0240(16) 0.050(2) -0.0028(15) -0.0057(14) -0.0075(13) F6 0.0426(17) 0.054(2) 0.0256(17) -0.0075(16) 0.0053(13) -0.0027(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.346(5) . ? C1 C2 1.384(6) . ? C1 H1 0.9300 . ? C2 C3 1.363(6) . ? C2 H2 0.9300 . ? C3 C4 1.392(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 N1 1.346(5) . ? C5 C6 1.471(5) . ? C6 C7 1.373(5) . ? C6 N2 1.374(5) . ? C7 N4 1.342(5) . ? C7 H8 0.9300 . ? C8 N4 1.489(5) . ? C8 C9 1.511(6) . ? C8 H9A 0.9700 . ? C8 H9B 0.9700 . ? C9 C10 1.405(6) . ? C9 C14 1.396(6) 2_666 ? C10 C11 1.381(6) 2_666 ? C10 H11 0.9300 . ? C11 C10 1.381(6) 2_666 ? C11 C12 1.378(6) . ? C11 H11A 0.9300 . ? C12 C13 1.391(6) . ? C12 H12A 0.9300 . ? C13 C14 1.386(6) . ? C13 H13A 0.9300 . ? C14 C9 1.396(6) 2_666 ? C14 C15 1.514(6) . ? C15 N5 1.478(5) . ? C15 H15C 0.9700 . ? C15 H15D 0.9700 . ? C16 C17 1.378(5) . ? C16 N5 1.339(5) . ? C16 H16A 0.9300 . ? C17 N7 1.363(5) . ? C17 C18 1.477(5) . ? C18 N8 1.353(5) . ? C18 C19 1.384(6) . ? C19 C20 1.385(7) . ? C19 H19A 0.9300 . ? C20 C21 1.362(8) . ? C20 H20A 0.9300 . ? C21 C22 1.361(8) . ? C21 H21A 0.9300 . ? C22 N8 1.342(5) . ? C22 H22A 0.9300 . ? C23 C24 1.378(7) . ? C23 N9 1.346(6) . ? C23 H1B 0.9300 . ? C24 C25 1.389(6) . ? C24 H2B 0.9300 . ? C25 C26 1.386(6) . ? C25 H3B 0.9300 . ? C26 C27 1.382(6) . ? C26 H4B 0.9300 . ? C27 N9 1.353(5) . ? C27 C28 1.476(5) . ? C28 N10 1.374(5) . ? C28 C29 1.368(5) . ? C29 N12 1.346(5) . ? C29 H7B 0.9300 . ? C30 N12 1.482(5) 2_657 ? C30 C31 1.515(5) . ? C30 H15A 0.9700 . ? C30 H15B 0.9700 . ? C31 C32 1.391(5) . ? C31 C36 1.400(5) . ? C32 C33 1.382(6) . ? C32 H13C 0.9300 . ? C33 C34 1.372(6) . ? C33 H12C 0.9300 . ? C34 C35 1.393(6) . ? C34 H11C 0.9300 . ? C35 C36 1.400(5) . ? C35 H10C 0.9300 . ? C36 C37 1.517(5) . ? C37 N13 1.482(5) . ? C37 H8C1 0.9700 . ? C37 H8C2 0.9700 . ? C38 N13 1.343(5) . ? C38 C39 1.378(5) . ? C38 H7C 0.9300 . ? C39 N15 1.372(5) . ? C39 C40 1.476(5) . ? C40 C41 1.385(6) . ? C40 N16 1.340(5) . ? C41 C42 1.400(6) . ? C41 H4C 0.9300 . ? C42 C43 1.379(6) . ? C42 H3C 0.9300 . ? C43 C44 1.392(6) . ? C43 H2C 0.9300 . ? C44 N16 1.335(5) . ? C44 H1C 0.9300 . ? N1 Ag1 2.228(3) . ? N2 N3 1.319(5) . ? N2 Ag1 2.541(3) . ? N3 N4 1.340(5) . ? N5 N6 1.356(5) . ? N6 N7 1.313(5) . ? N7 Ag1 2.491(3) . ? N8 Ag1 2.233(4) . ? N9 Ag2 2.220(4) . ? N10 N11 1.314(5) . ? N10 Ag2 2.582(3) . ? N11 N12 1.337(4) . ? N12 C30 1.482(5) 2_657 ? N13 N14 1.344(4) . ? N14 N15 1.328(4) . ? N15 Ag2 2.394(3) . ? N16 Ag2 2.292(4) . ? Ag1 Ag1 3.2217(14) 2_666 ? Ag2 Ag2 3.1897(15) 2_657 ? Sb1 F5' 1.81(2) . ? Sb1 F4' 1.832(17) . ? Sb1 F2' 1.830(16) . ? Sb1 F5 1.857(3) . ? Sb1 F3 1.854(3) . ? Sb1 F4 1.853(4) . ? Sb1 F6' 1.90(2) . ? Sb1 F6 1.886(3) . ? Sb1 F1 1.889(3) . ? Sb1 F2 1.896(3) . ? Sb1 F3' 1.967(16) . ? Sb1 F1' 1.956(13) . ? Sb2 F12' 1.788(9) . ? Sb2 F11 1.800(5) . ? Sb2 F8' 1.795(7) . ? Sb2 F7 1.854(4) . ? Sb2 F9 1.830(4) . ? Sb2 F9' 1.881(7) . ? Sb2 F11' 1.899(9) . ? Sb2 F12 1.913(5) . ? Sb2 F10 1.918(4) . ? Sb2 F10' 1.882(10) . ? Sb2 F8 1.931(4) . ? Sb2 F7' 1.938(7) . ? F8' F12' 1.738(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.1(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 119.9(4) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 118.2(4) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 N1 121.8(3) . . ? C4 C5 C6 121.0(3) . . ? N1 C5 C6 117.2(3) . . ? C7 C6 N2 108.0(3) . . ? C7 C6 C5 129.9(3) . . ? N2 C6 C5 122.0(3) . . ? N4 C7 C6 104.7(3) . . ? N4 C7 H8 127.6 . . ? C6 C7 H8 127.6 . . ? N4 C8 C9 111.9(4) . . ? N4 C8 H9A 109.2 . . ? C9 C8 H9A 109.2 . . ? N4 C8 H9B 109.2 . . ? C9 C8 H9B 109.2 . . ? H9A C8 H9B 107.9 . . ? C10 C9 C14 118.9(4) . 2_666 ? C10 C9 C8 117.2(4) . . ? C14 C9 C8 123.8(4) 2_666 . ? C9 C10 C11 120.9(4) . 2_666 ? C9 C10 H11 119.5 . . ? C11 C10 H11 119.5 2_666 . ? C10 C11 C12 120.0(4) 2_666 . ? C10 C11 H11A 120.0 2_666 . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 121.3(4) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C13 C14 C9 119.3(4) . 2_666 ? C13 C14 C15 118.4(4) . . ? C9 C14 C15 122.2(4) 2_666 . ? N5 C15 C14 111.4(3) . . ? N5 C15 H15C 109.4 . . ? C14 C15 H15C 109.4 . . ? N5 C15 H15D 109.4 . . ? C14 C15 H15D 109.4 . . ? H15C C15 H15D 108.0 . . ? C17 C16 N5 104.5(4) . . ? C17 C16 H16A 127.8 . . ? N5 C16 H16A 127.8 . . ? C16 C17 N7 107.9(3) . . ? C16 C17 C18 130.1(4) . . ? N7 C17 C18 122.0(3) . . ? N8 C18 C19 121.9(4) . . ? N8 C18 C17 116.0(3) . . ? C19 C18 C17 122.0(4) . . ? C20 C19 C18 118.9(5) . . ? C20 C19 H19A 120.6 . . ? C18 C19 H19A 120.6 . . ? C21 C20 C19 119.1(5) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 N8 123.5(5) . . ? C21 C22 H22A 118.2 . . ? N8 C22 H22A 118.2 . . ? C24 C23 N9 123.5(4) . . ? C24 C23 H1B 118.3 . . ? N9 C23 H1B 118.3 . . ? C25 C24 C23 118.9(4) . . ? C25 C24 H2B 120.5 . . ? C23 C24 H2B 120.5 . . ? C24 C25 C26 118.0(4) . . ? C24 C25 H3B 121.0 . . ? C26 C25 H3B 121.0 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H4B 119.9 . . ? C25 C26 H4B 119.9 . . ? C26 C27 N9 121.9(4) . . ? C26 C27 C28 120.9(4) . . ? N9 C27 C28 117.1(4) . . ? N10 C28 C29 108.1(3) . . ? N10 C28 C27 121.8(3) . . ? C29 C28 C27 129.9(3) . . ? N12 C29 C28 104.6(3) . . ? N12 C29 H7B 127.7 . . ? C28 C29 H7B 127.7 . . ? N12 C30 C31 112.4(3) 2_657 . ? N12 C30 H15A 109.1 2_657 . ? C31 C30 H15A 109.1 . . ? N12 C30 H15B 109.1 2_657 . ? C31 C30 H15B 109.1 . . ? H15A C30 H15B 107.9 . . ? C32 C31 C36 119.1(3) . . ? C32 C31 C30 118.5(3) . . ? C36 C31 C30 122.4(3) . . ? C31 C32 C33 121.5(3) . . ? C31 C32 H13C 119.2 . . ? C33 C32 H13C 119.2 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H12C 120.1 . . ? C32 C33 H12C 120.1 . . ? C33 C34 C35 119.9(4) . . ? C33 C34 H11C 120.1 . . ? C35 C34 H11C 120.1 . . ? C36 C35 C34 120.8(3) . . ? C36 C35 H10C 119.6 . . ? C34 C35 H10C 119.6 . . ? C35 C36 C31 118.9(4) . . ? C35 C36 C37 119.2(3) . . ? C31 C36 C37 121.9(3) . . ? N13 C37 C36 111.6(3) . . ? N13 C37 H8C1 109.3 . . ? C36 C37 H8C1 109.3 . . ? N13 C37 H8C2 109.3 . . ? C36 C37 H8C2 109.3 . . ? H8C1 C37 H8C2 108.0 . . ? N13 C38 C39 104.5(3) . . ? N13 C38 H7C 127.7 . . ? C39 C38 H7C 127.7 . . ? N15 C39 C38 107.8(3) . . ? N15 C39 C40 120.7(3) . . ? C38 C39 C40 131.5(4) . . ? C41 C40 N16 122.6(4) . . ? C41 C40 C39 120.5(3) . . ? N16 C40 C39 116.9(3) . . ? C40 C41 C42 119.1(4) . . ? C40 C41 H4C 120.5 . . ? C42 C41 H4C 120.5 . . ? C41 C42 C43 117.8(4) . . ? C41 C42 H3C 121.1 . . ? C43 C42 H3C 121.1 . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H2C 120.1 . . ? C42 C43 H2C 120.1 . . ? N16 C44 C43 122.2(4) . . ? N16 C44 H1C 118.9 . . ? C43 C44 H1C 118.9 . . ? C1 N1 C5 118.3(3) . . ? C1 N1 Ag1 120.4(3) . . ? C5 N1 Ag1 121.0(3) . . ? N3 N2 C6 108.4(3) . . ? N3 N2 Ag1 143.8(2) . . ? C6 N2 Ag1 107.3(2) . . ? N2 N3 N4 107.2(3) . . ? N3 N4 C7 111.6(3) . . ? N3 N4 C8 119.4(3) . . ? C7 N4 C8 129.0(3) . . ? C16 N5 N6 111.8(3) . . ? C16 N5 C15 129.0(4) . . ? N6 N5 C15 119.2(4) . . ? N7 N6 N5 106.0(3) . . ? N6 N7 C17 109.8(3) . . ? N6 N7 Ag1 141.4(3) . . ? C17 N7 Ag1 108.7(2) . . ? C18 N8 C22 117.3(4) . . ? C18 N8 Ag1 120.6(3) . . ? C22 N8 Ag1 121.9(3) . . ? C27 N9 C23 117.5(4) . . ? C27 N9 Ag2 122.1(3) . . ? C23 N9 Ag2 120.3(3) . . ? N11 N10 C28 108.7(3) . . ? N11 N10 Ag2 142.0(3) . . ? C28 N10 Ag2 106.8(2) . . ? N10 N11 N12 107.1(3) . . ? N11 N12 C29 111.7(3) . . ? N11 N12 C30 118.9(3) . 2_657 ? C29 N12 C30 129.4(3) . 2_657 ? N14 N13 C38 112.4(3) . . ? N14 N13 C37 119.0(3) . . ? C38 N13 C37 128.6(3) . . ? N15 N14 N13 105.9(3) . . ? N14 N15 C39 109.3(3) . . ? N14 N15 Ag2 139.2(3) . . ? C39 N15 Ag2 111.5(2) . . ? C44 N16 C40 118.5(4) . . ? C44 N16 Ag2 123.4(3) . . ? C40 N16 Ag2 118.1(3) . . ? N8 Ag1 N1 173.58(11) . . ? N8 Ag1 N7 72.35(11) . . ? N1 Ag1 N7 107.20(11) . . ? N8 Ag1 N2 107.87(11) . . ? N1 Ag1 N2 72.05(11) . . ? N7 Ag1 N2 175.54(10) . . ? N8 Ag1 Ag1 106.86(9) . 2_666 ? N1 Ag1 Ag1 79.56(9) . 2_666 ? N7 Ag1 Ag1 99.81(7) . 2_666 ? N2 Ag1 Ag1 84.43(7) . 2_666 ? N9 Ag2 N16 165.19(11) . . ? N9 Ag2 N15 119.37(12) . . ? N16 Ag2 N15 72.82(11) . . ? N9 Ag2 N10 71.50(11) . . ? N16 Ag2 N10 95.23(11) . . ? N15 Ag2 N10 166.11(11) . . ? N9 Ag2 Ag2 108.69(9) . 2_657 ? N16 Ag2 Ag2 76.70(8) . 2_657 ? N15 Ag2 Ag2 95.20(8) . 2_657 ? N10 Ag2 Ag2 88.68(7) . 2_657 ? F5' Sb1 F4' 98.2(9) . . ? F5' Sb1 F2' 93.4(8) . . ? F4' Sb1 F2' 90.9(7) . . ? F5' Sb1 F5 106.7(6) . . ? F4' Sb1 F5 120.4(6) . . ? F2' Sb1 F5 138.7(5) . . ? F5' Sb1 F3 114.4(6) . . ? F4' Sb1 F3 125.8(6) . . ? F2' Sb1 F3 47.6(5) . . ? F5 Sb1 F3 91.11(17) . . ? F5' Sb1 F4 148.5(6) . . ? F4' Sb1 F4 50.3(6) . . ? F2' Sb1 F4 89.7(5) . . ? F5 Sb1 F4 91.06(17) . . ? F3 Sb1 F4 90.41(17) . . ? F5' Sb1 F6' 92.8(10) . . ? F4' Sb1 F6' 93.9(9) . . ? F2' Sb1 F6' 171.6(9) . . ? F5 Sb1 F6' 33.3(7) . . ? F3 Sb1 F6' 124.3(7) . . ? F4 Sb1 F6' 88.1(7) . . ? F5' Sb1 F6 63.6(6) . . ? F4' Sb1 F6 54.8(6) . . ? F2' Sb1 F6 131.3(5) . . ? F5 Sb1 F6 90.03(15) . . ? F3 Sb1 F6 178.00(15) . . ? F4 Sb1 F6 91.21(17) . . ? F6' Sb1 F6 56.9(7) . . ? F5' Sb1 F1 30.0(6) . . ? F4' Sb1 F1 128.0(6) . . ? F2' Sb1 F1 89.5(5) . . ? F5 Sb1 F1 90.66(14) . . ? F3 Sb1 F1 90.21(15) . . ? F4 Sb1 F1 178.16(16) . . ? F6' Sb1 F1 93.0(7) . . ? F6 Sb1 F1 88.14(15) . . ? F5' Sb1 F2 71.6(6) . . ? F4' Sb1 F2 60.2(6) . . ? F2' Sb1 F2 42.1(5) . . ? F5 Sb1 F2 178.31(14) . . ? F3 Sb1 F2 89.62(18) . . ? F4 Sb1 F2 90.46(18) . . ? F6' Sb1 F2 146.0(7) . . ? F6 Sb1 F2 89.20(16) . . ? F1 Sb1 F2 87.81(15) . . ? F5' Sb1 F3' 87.2(8) . . ? F4' Sb1 F3' 174.5(7) . . ? F2' Sb1 F3' 87.8(7) . . ? F5 Sb1 F3' 58.5(5) . . ? F3 Sb1 F3' 50.1(5) . . ? F4 Sb1 F3' 124.3(5) . . ? F6' Sb1 F3' 86.8(8) . . ? F6 Sb1 F3' 129.5(5) . . ? F1 Sb1 F3' 57.2(5) . . ? F2 Sb1 F3' 121.1(5) . . ? F5' Sb1 F1' 174.7(7) . . ? F4' Sb1 F1' 87.0(7) . . ? F2' Sb1 F1' 87.5(6) . . ? F5 Sb1 F1' 69.5(4) . . ? F3 Sb1 F1' 62.6(4) . . ? F4 Sb1 F1' 36.7(4) . . ? F6' Sb1 F1' 85.8(8) . . ? F6 Sb1 F1' 119.3(4) . . ? F1 Sb1 F1' 144.9(4) . . ? F2 Sb1 F1' 112.2(4) . . ? F3' Sb1 F1' 87.7(6) . . ? F12' Sb2 F11 96.4(3) . . ? F12' Sb2 F8' 58.0(3) . . ? F11 Sb2 F8' 129.7(3) . . ? F12' Sb2 F7 157.5(3) . . ? F11 Sb2 F7 100.6(2) . . ? F8' Sb2 F7 99.5(3) . . ? F12' Sb2 F9 94.9(3) . . ? F11 Sb2 F9 96.0(2) . . ? F8' Sb2 F9 126.0(3) . . ? F7 Sb2 F9 97.9(2) . . ? F12' Sb2 F9' 86.5(4) . . ? F11 Sb2 F9' 131.4(3) . . ? F8' Sb2 F9' 92.6(3) . . ? F7 Sb2 F9' 93.1(3) . . ? F9 Sb2 F9' 35.7(3) . . ? F12' Sb2 F11' 88.4(4) . . ? F11 Sb2 F11' 40.9(3) . . ? F8' Sb2 F11' 92.0(3) . . ? F7 Sb2 F11' 94.8(3) . . ? F9 Sb2 F11' 136.7(3) . . ? F9' Sb2 F11' 170.1(3) . . ? F12' Sb2 F12 23.4(3) . . ? F11 Sb2 F12 79.2(3) . . ? F8' Sb2 F12 81.4(4) . . ? F7 Sb2 F12 178.9(3) . . ? F9 Sb2 F12 81.1(3) . . ? F9' Sb2 F12 86.3(3) . . ? F11' Sb2 F12 85.7(3) . . ? F12' Sb2 F10 87.5(3) . . ? F11 Sb2 F10 89.9(2) . . ? F8' Sb2 F10 50.6(3) . . ? F7 Sb2 F10 77.9(2) . . ? F9 Sb2 F10 173.3(2) . . ? F9' Sb2 F10 138.6(3) . . ? F11' Sb2 F10 49.4(3) . . ? F12 Sb2 F10 103.1(3) . . ? F12' Sb2 F10' 177.3(4) . . ? F11 Sb2 F10' 85.7(4) . . ? F8' Sb2 F10' 119.3(4) . . ? F7 Sb2 F10' 19.9(3) . . ? F9 Sb2 F10' 86.4(3) . . ? F9' Sb2 F10' 93.2(4) . . ? F11' Sb2 F10' 92.3(4) . . ? F12 Sb2 F10' 159.2(4) . . ? F10 Sb2 F10' 91.0(3) . . ? F12' Sb2 F8 86.6(3) . . ? F11 Sb2 F8 175.8(2) . . ? F8' Sb2 F8 49.9(3) . . ? F7 Sb2 F8 75.8(2) . . ? F9 Sb2 F8 86.6(2) . . ? F9' Sb2 F8 51.5(3) . . ? F11' Sb2 F8 136.7(3) . . ? F12 Sb2 F8 104.5(3) . . ? F10 Sb2 F8 87.3(2) . . ? F10' Sb2 F8 91.1(4) . . ? F12' Sb2 F7' 116.6(3) . . ? F11 Sb2 F7' 48.4(3) . . ? F8' Sb2 F7' 174.6(3) . . ? F7 Sb2 F7' 85.9(3) . . ? F9 Sb2 F7' 52.6(3) . . ? F9' Sb2 F7' 87.1(3) . . ? F11' Sb2 F7' 87.6(3) . . ? F12 Sb2 F7' 93.2(4) . . ? F10 Sb2 F7' 131.5(3) . . ? F10' Sb2 F7' 66.1(4) . . ? F8 Sb2 F7' 132.4(3) . . ? F12' F8' Sb2 60.8(4) . . ? F8' F12' Sb2 61.2(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.254 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.098 # Attachment 'jc324b.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-25 at 14:52:52 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\program files\wingx\files\archive.reqdat # CIF files read : jc324b pcf #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_jc324b _database_code_depnum_ccdc_archive 'CCDC 734031' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-05-25 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? # Insert blank lines between references _publ_section_references ; Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H34 Ag3 N18, 3(F6 Sb), 2(C2 H3 N)' _chemical_formula_sum 'C40 H40 Ag3 F18 N20 Sb3 ' _chemical_formula_weight 1831.81 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.779(1) _cell_length_b 13.727(2) _cell_length_c 14.166(2) _cell_angle_alpha 62.945(5) _cell_angle_beta 78.556(6) _cell_angle_gamma 73.474(6) _cell_volume 1452.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7441 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 26.4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.08 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.474 _exptl_absorpt_correction_type multi-scan #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_number 24028 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.94 _diffrn_measured_fraction_theta_max 0.94 _reflns_number_total 5084 _reflns_number_gt 4867 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _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 0.011(2) _refine_ls_number_reflns 5084 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.3021 _refine_ls_wR_factor_gt 0.2931 _refine_ls_goodness_of_fit_ref 1.47 _refine_ls_restrained_S_all 1.47 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.577 _refine_diff_density_min -4.249 _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' 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' Sb Sb -0.5866 1.5461 '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 C1 C 0.3741(8) 0.3177(7) -0.1367(6) 0.0252(17) Uani 1 1 d . . . H1 H 0.3395 0.3878 -0.1355 0.03 Uiso 1 1 calc R . . C2 C 0.2961(8) 0.2349(7) -0.0691(6) 0.0242(16) Uani 1 1 d . . . H2 H 0.2115 0.2486 -0.0223 0.029 Uiso 1 1 calc R . . C3 C 0.3450(9) 0.1290(8) -0.0710(6) 0.0308(19) Uani 1 1 d . . . H3 H 0.2925 0.0718 -0.0269 0.037 Uiso 1 1 calc R . . C4 C 0.4747(8) 0.1123(7) -0.1411(6) 0.0245(16) Uani 1 1 d . . . H4 H 0.5121 0.0432 -0.1442 0.029 Uiso 1 1 calc R . . C5 C 0.5467(7) 0.2019(6) -0.2064(5) 0.0165(14) Uani 1 1 d . . . C6 C 0.6876(8) 0.1880(6) -0.2836(6) 0.0233(16) Uani 1 1 d . . . H6A H 0.7681 0.2222 -0.2805 0.028 Uiso 1 1 calc R . . H6B H 0.7339 0.1087 -0.2629 0.028 Uiso 1 1 calc R . . C7 C 0.6404(8) 0.1916(6) -0.4562(6) 0.0206(15) Uani 1 1 d . . . H7 H 0.6687 0.1156 -0.4405 0.025 Uiso 1 1 calc R . . C8 C 0.4120(8) 0.7198(7) -0.4495(5) 0.0192(15) Uani 1 1 d . . . C9 C 0.4447(8) 0.7149(6) -0.3497(6) 0.0188(15) Uani 1 1 d . . . C10 C 0.4244(8) 0.7949(6) -0.3139(5) 0.0160(14) Uani 1 1 d . . . H10 H 0.3818 0.8714 -0.3484 0.019 Uiso 1 1 calc R . . C11 C 0.4911(9) 0.7787(7) -0.1398(6) 0.0210(15) Uani 1 1 d . . . H11A H 0.4912 0.858 -0.1779 0.025 Uiso 1 1 calc R . . H11B H 0.5912 0.7403 -0.107 0.025 Uiso 1 1 calc R . . C12 C 0.3549(9) 0.7631(7) -0.0532(6) 0.0266(17) Uani 1 1 d . . . C13 C 0.2476(10) 0.8552(6) -0.0453(6) 0.0256(17) Uani 1 1 d . . . H13 H 0.2535 0.927 -0.0965 0.031 Uiso 1 1 calc R . . C14 C 0.1302(9) 0.8405(7) 0.0395(6) 0.0252(17) Uani 1 1 d . . . H14 H 0.0579 0.9016 0.0465 0.03 Uiso 1 1 calc R . . C15 C 0.1251(9) 0.7335(8) 0.1116(6) 0.0306(19) Uani 1 1 d . . . H15 H 0.0505 0.7201 0.1702 0.037 Uiso 1 1 calc R . . C16 C 0.2326(8) 0.6452(6) 0.0965(6) 0.0199(14) Uani 1 1 d . . . H16 H 0.2249 0.5726 0.1447 0.024 Uiso 1 1 calc R . . C100 C 0.9790(10) 0.4872(6) -0.3730(5) 0.0247(17) Uani 1 1 d . . . C101 C 1.1351(9) 0.5060(8) -0.3810(7) 0.0292(18) Uani 1 1 d . . . H10A H 1.2137 0.4514 -0.3997 0.044 Uiso 1 1 calc R . . H10B H 1.1553 0.4993 -0.3139 0.044 Uiso 1 1 calc R . . H10C H 1.1403 0.58 -0.4348 0.044 Uiso 1 1 calc R . . C102 C -0.1340(12) 0.8624(8) -0.2781(10) 0.050(3) Uani 1 1 d . . . C103 C -0.2273(11) 0.9143(9) -0.2438(11) 0.052(3) Uani 1 1 d . . . H10D H -0.3115 0.8756 -0.2063 0.079 Uiso 1 1 calc R . . H10E H -0.2695 0.9849 -0.3 0.079 Uiso 1 1 calc R . . H10F H -0.1814 0.9271 -0.1954 0.079 Uiso 1 1 calc R . . N1 N 0.4988(7) 0.3021(5) -0.2048(5) 0.0228(14) Uani 1 1 d . . . N2 N 0.6414(7) 0.2397(6) -0.3929(5) 0.0223(13) Uani 1 1 d . . . N3 N 0.5889(7) 0.3521(5) -0.4419(5) 0.0210(13) Uani 1 1 d . . . N4 N 0.4426(7) 0.6247(5) -0.4625(5) 0.0206(13) Uani 1 1 d . . . N5 N 0.5064(8) 0.6134(6) -0.2731(5) 0.0309(16) Uani 1 1 d . . . N6 N 0.5309(8) 0.6281(6) -0.1928(5) 0.0307(16) Uani 1 1 d . . . N7 N 0.4814(7) 0.7364(5) -0.2155(5) 0.0194(12) Uani 1 1 d . . . N8 N 0.3472(7) 0.6579(5) 0.0165(4) 0.0195(13) Uani 1 1 d . . . N100 N 0.8543(8) 0.4715(6) -0.3666(5) 0.0292(15) Uani 1 1 d . . . N101 N -0.0119(13) 0.7929(11) -0.3227(9) 0.071(3) Uani 1 1 d . . . F1 F 1.0041(6) 0.7637(5) -0.5653(4) 0.0418(13) Uani 1 1 d . . . F2 F 0.9193(6) 0.8855(5) -0.7611(4) 0.0463(15) Uani 1 1 d . . . F3 F 0.7128(7) 0.8355(6) -0.4906(4) 0.0517(17) Uani 1 1 d . . . F4 F 0.8801(7) 0.9790(5) -0.6295(6) 0.0528(16) Uani 1 1 d . . . F5 F 0.6304(6) 0.9585(4) -0.6871(4) 0.0352(12) Uani 1 1 d . . . F6 F 0.7483(6) 0.7420(5) -0.6227(5) 0.0507(15) Uani 1 1 d . . . F7 F 0.0381(6) 0.6454(4) -0.0649(4) 0.0355(11) Uani 1 1 d . . . F8 F 0.2166(6) 0.4368(5) 0.0198(4) 0.0379(13) Uani 1 1 d . . . F9 F 0.0336(6) 0.4953(5) -0.1330(4) 0.0359(12) Uani 1 1 d . . . Ag1 Ag 0.59216(7) 0.45729(5) -0.33296(4) 0.0235(4) Uani 1 1 d . . . Ag2 Ag 0.5 0.5 0 0.0219(4) Uani 1 2 d S . . Sb1 Sb 0.81623(5) 0.85869(4) -0.62536(4) 0.0247(4) Uani 1 1 d . . . Sb2 Sb 0 0.5 0 0.0231(4) Uani 1 2 d S . . 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 C1 0.016(3) 0.036(4) 0.018(3) -0.014(3) -0.002(3) 0.007(3) C2 0.019(3) 0.033(4) 0.021(4) -0.016(3) -0.004(3) 0.004(3) C3 0.022(4) 0.046(5) 0.014(3) -0.007(4) 0.003(3) -0.003(3) C4 0.019(4) 0.037(4) 0.015(3) -0.012(3) -0.004(3) 0.001(3) C5 0.014(3) 0.023(3) 0.007(3) -0.005(3) -0.007(2) 0.004(3) C6 0.017(3) 0.023(4) 0.022(4) -0.010(3) -0.005(3) 0.011(3) C7 0.014(3) 0.024(4) 0.018(3) -0.011(3) 0.000(3) 0.007(3) C8 0.009(3) 0.026(4) 0.014(3) -0.006(3) 0.000(2) 0.004(3) C9 0.020(3) 0.020(4) 0.017(3) -0.014(3) -0.004(3) 0.007(3) C10 0.020(3) 0.018(3) 0.013(3) -0.010(3) -0.003(3) -0.004(3) C11 0.024(4) 0.030(4) 0.011(3) -0.012(3) -0.002(3) -0.002(3) C12 0.019(3) 0.039(5) 0.018(4) -0.013(3) -0.010(3) 0.007(3) C13 0.034(4) 0.016(4) 0.018(3) -0.005(3) 0.002(3) 0.002(3) C14 0.022(3) 0.023(4) 0.018(4) -0.008(3) -0.002(3) 0.011(3) C15 0.018(4) 0.042(5) 0.017(4) -0.011(4) -0.003(3) 0.013(3) C16 0.017(3) 0.021(4) 0.020(4) -0.008(3) -0.003(3) -0.003(3) C100 0.028(4) 0.021(4) 0.009(3) 0.000(3) -0.003(3) 0.008(3) C101 0.015(4) 0.045(5) 0.021(4) -0.014(4) -0.003(3) 0.003(3) C102 0.031(5) 0.025(5) 0.069(7) -0.003(5) 0.006(5) -0.007(4) C103 0.028(5) 0.030(5) 0.103(9) -0.037(6) 0.020(5) -0.013(4) N1 0.021(3) 0.023(3) 0.016(3) -0.009(3) -0.008(2) 0.012(2) N2 0.019(3) 0.029(3) 0.016(3) -0.011(3) -0.001(2) 0.003(2) N3 0.021(3) 0.025(3) 0.013(3) -0.007(3) -0.005(2) 0.001(2) N4 0.020(3) 0.022(3) 0.011(3) -0.006(3) -0.003(2) 0.006(2) N5 0.038(4) 0.031(4) 0.012(3) -0.006(3) -0.006(3) 0.006(3) N6 0.043(4) 0.030(4) 0.021(3) -0.018(3) -0.018(3) 0.012(3) N7 0.016(3) 0.022(3) 0.011(3) -0.005(2) 0.001(2) 0.006(2) N8 0.017(3) 0.027(3) 0.012(3) -0.010(2) -0.005(2) 0.006(2) N100 0.025(4) 0.035(4) 0.018(3) -0.008(3) 0.002(3) -0.002(3) N101 0.052(6) 0.096(9) 0.055(6) -0.039(6) -0.009(5) 0.017(6) F1 0.025(2) 0.050(3) 0.036(3) -0.012(3) -0.006(2) 0.007(2) F2 0.037(3) 0.058(4) 0.024(2) -0.015(3) 0.003(2) 0.011(3) F3 0.034(3) 0.091(5) 0.032(3) -0.031(3) 0.002(2) -0.011(3) F4 0.035(3) 0.044(3) 0.079(4) -0.027(3) -0.007(3) -0.004(2) F5 0.026(2) 0.028(3) 0.043(3) -0.015(2) -0.011(2) 0.012(2) F6 0.037(3) 0.035(3) 0.067(4) -0.017(3) -0.011(3) 0.009(2) F7 0.036(3) 0.040(3) 0.035(3) -0.018(2) -0.008(2) -0.008(2) F8 0.020(2) 0.055(3) 0.041(3) -0.032(3) -0.012(2) 0.016(2) F9 0.029(3) 0.053(3) 0.027(2) -0.024(2) -0.0030(19) 0.001(2) Ag1 0.0221(5) 0.0231(5) 0.0188(5) -0.0068(4) -0.0060(3) 0.0042(3) Ag2 0.0188(5) 0.0222(6) 0.0172(5) -0.0084(4) -0.0047(3) 0.0088(4) Sb1 0.0162(5) 0.0291(5) 0.0202(5) -0.0096(3) -0.0009(3) 0.0058(3) Sb2 0.0127(5) 0.0328(6) 0.0209(5) -0.0155(4) -0.0045(3) 0.0082(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.346(9) . ? C1 C2 1.367(12) . ? C1 H1 0.93 . ? C2 C3 1.405(13) . ? C2 H2 0.93 . ? C3 C4 1.394(10) . ? C3 H3 0.93 . ? C4 C5 1.394(11) . ? C4 H4 0.93 . ? C5 N1 1.328(10) . ? C5 C6 1.510(9) . ? C6 N2 1.467(9) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 N2 1.336(10) . ? C7 C8 1.386(10) 2_664 ? C7 H7 0.93 . ? C8 N4 1.345(11) . ? C8 C7 1.386(10) 2_664 ? C8 C9 1.466(10) . ? C9 C10 1.362(10) . ? C9 N5 1.357(10) . ? C10 N7 1.367(9) . ? C10 H10 0.93 . ? C11 N7 1.458(9) . ? C11 C12 1.519(10) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 N8 1.340(11) . ? C12 C13 1.381(11) . ? C13 C14 1.398(11) . ? C13 H13 0.93 . ? C14 C15 1.362(12) . ? C14 H14 0.93 . ? C15 C16 1.383(11) . ? C15 H15 0.93 . ? C16 N8 1.339(9) . ? C16 H16 0.93 . ? C100 N100 1.154(11) . ? C100 C101 1.438(12) . ? C101 H10A 0.96 . ? C101 H10B 0.96 . ? C101 H10C 0.96 . ? C102 C103 1.113(14) . ? C102 N101 1.468(15) . ? C103 H10D 0.96 . ? C103 H10E 0.96 . ? C103 H10F 0.96 . ? N1 Ag1 2.322(7) . ? N2 N3 1.350(9) . ? N3 N4 1.312(8) 2_664 ? N3 Ag1 2.556(6) . ? N4 N3 1.312(8) 2_664 ? N4 Ag1 2.403(6) . ? N5 N6 1.308(9) . ? N5 Ag1 2.522(7) . ? N6 N7 1.324(9) . ? N6 Ag2 2.497(7) . ? N8 Ag2 2.288(6) . ? N100 Ag1 2.301(7) . ? F1 Sb1 1.863(5) . ? F2 Sb1 1.872(5) . ? F3 Sb1 1.870(5) . ? F4 Sb1 1.864(6) . ? F5 Sb1 1.873(5) . ? F6 Sb1 1.845(6) . ? F7 Sb2 1.879(5) . ? F8 Sb2 1.871(5) . ? F9 Sb2 1.876(5) . ? Ag2 N8 2.288(6) 2_665 ? Ag2 N6 2.497(7) 2_665 ? Sb2 F8 1.871(5) 2_565 ? Sb2 F9 1.876(5) 2_565 ? Sb2 F7 1.879(5) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.8(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.4(7) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 118.0(8) . . ? C4 C3 H3 121 . . ? C2 C3 H3 121 . . ? C3 C4 C5 118.3(7) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 123.4(6) . . ? N1 C5 C6 116.3(7) . . ? C4 C5 C6 120.3(6) . . ? N2 C6 C5 111.6(5) . . ? N2 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108 . . ? N2 C7 C8 104.8(7) . 2_664 ? N2 C7 H7 127.6 . . ? C8 C7 H7 127.6 2_664 . ? N4 C8 C7 107.6(6) . 2_664 ? N4 C8 C9 119.6(6) . . ? C7 C8 C9 132.6(7) 2_664 . ? C10 C9 N5 108.9(6) . . ? C10 C9 C8 132.7(7) . . ? N5 C9 C8 118.3(7) . . ? N7 C10 C9 103.8(6) . . ? N7 C10 H10 128.1 . . ? C9 C10 H10 128.1 . . ? N7 C11 C12 113.2(6) . . ? N7 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N7 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? N8 C12 C13 122.0(7) . . ? N8 C12 C11 117.6(7) . . ? C13 C12 C11 120.3(8) . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C15 C14 C13 117.8(7) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? C14 C15 C16 119.0(7) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N8 C16 C15 123.9(8) . . ? N8 C16 H16 118 . . ? C15 C16 H16 118 . . ? N100 C100 C101 179.6(9) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 N101 179.3(13) . . ? C102 C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C102 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C1 N1 C5 118.2(7) . . ? C1 N1 Ag1 118.6(5) . . ? C5 N1 Ag1 122.4(5) . . ? C7 N2 N3 111.0(6) . . ? C7 N2 C6 129.6(7) . . ? N3 N2 C6 119.4(6) . . ? N4 N3 N2 106.6(6) 2_664 . ? N4 N3 Ag1 138.5(5) 2_664 . ? N2 N3 Ag1 114.8(4) . . ? N3 N4 C8 110.0(6) 2_664 . ? N3 N4 Ag1 130.6(5) 2_664 . ? C8 N4 Ag1 117.7(4) . . ? N6 N5 C9 108.5(7) . . ? N6 N5 Ag1 136.1(5) . . ? C9 N5 Ag1 114.1(5) . . ? N5 N6 N7 108.0(6) . . ? N5 N6 Ag2 127.0(6) . . ? N7 N6 Ag2 114.8(4) . . ? N6 N7 C10 110.7(6) . . ? N6 N7 C11 120.8(6) . . ? C10 N7 C11 128.5(6) . . ? C16 N8 C12 117.2(6) . . ? C16 N8 Ag2 117.9(5) . . ? C12 N8 Ag2 124.7(5) . . ? C100 N100 Ag1 169.1(6) . . ? N100 Ag1 N1 125.2(2) . . ? N100 Ag1 N4 107.3(2) . . ? N1 Ag1 N4 127.4(2) . . ? N100 Ag1 N5 92.9(2) . . ? N1 Ag1 N5 109.1(2) . . ? N4 Ag1 N5 68.6(2) . . ? N100 Ag1 N3 100.6(2) . . ? N1 Ag1 N3 78.4(2) . . ? N4 Ag1 N3 89.3(2) . . ? N5 Ag1 N3 156.8(2) . . ? N8 Ag2 N8 180.0(3) 2_665 . ? N8 Ag2 N6 95.4(2) 2_665 . ? N8 Ag2 N6 84.6(2) . . ? N8 Ag2 N6 84.6(2) 2_665 2_665 ? N8 Ag2 N6 95.4(2) . 2_665 ? N6 Ag2 N6 180.0(5) . 2_665 ? F6 Sb1 F1 92.1(3) . . ? F6 Sb1 F3 90.6(3) . . ? F1 Sb1 F3 90.9(2) . . ? F6 Sb1 F4 178.6(2) . . ? F1 Sb1 F4 89.4(3) . . ? F3 Sb1 F4 89.3(3) . . ? F6 Sb1 F2 90.6(3) . . ? F1 Sb1 F2 89.7(2) . . ? F3 Sb1 F2 178.6(3) . . ? F4 Sb1 F2 89.5(3) . . ? F6 Sb1 F5 89.9(2) . . ? F1 Sb1 F5 178.0(3) . . ? F3 Sb1 F5 89.6(2) . . ? F4 Sb1 F5 88.7(2) . . ? F2 Sb1 F5 89.8(2) . . ? F8 Sb2 F8 180.0(4) 2_565 . ? F8 Sb2 F9 89.7(2) 2_565 2_565 ? F8 Sb2 F9 90.3(2) . 2_565 ? F8 Sb2 F9 90.3(2) 2_565 . ? F8 Sb2 F9 89.7(2) . . ? F9 Sb2 F9 180.0(4) 2_565 . ? F8 Sb2 F7 88.9(2) 2_565 . ? F8 Sb2 F7 91.1(2) . . ? F9 Sb2 F7 90.0(2) 2_565 . ? F9 Sb2 F7 90.0(2) . . ? F8 Sb2 F7 91.1(2) 2_565 2_565 ? F8 Sb2 F7 88.9(2) . 2_565 ? F9 Sb2 F7 90.0(2) 2_565 2_565 ? F9 Sb2 F7 90.0(2) . 2_565 ? F7 Sb2 F7 180.0(3) . 2_565 ? # Attachment 'jc328revisedDalton.cif' data_pcf _database_code_depnum_ccdc_archive 'CCDC 734032' _audit_creation_date 2009-08-05T09:33:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H16 N8' _chemical_formula_sum 'C17 H16 N8' _chemical_formula_weight 332.38 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.377(6) _cell_length_b 4.4451(8) _cell_length_c 11.1901(19) _cell_angle_alpha 90.000(0) _cell_angle_beta 105.681(6) _cell_angle_gamma 90.000(0) _cell_volume 1550.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 4412 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 33.87 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type multi-scan #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_unetI/netI 0.0193 _diffrn_reflns_number 6260 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.48 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 1428 _reflns_number_gt 1275 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.0644P)^2^+1.0338P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1428 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.213 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' 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 C1 C 0.30395(5) 0.3848(4) 0.47363(14) 0.0217(4) Uani 1 1 d . . . H1 H 0.2887 0.3393 0.5309 0.026 Uiso 1 1 calc R . . C2 C 0.29182(5) 0.2434(3) 0.35948(14) 0.0208(4) Uani 1 1 d . . . H2 H 0.269 0.1088 0.3404 0.025 Uiso 1 1 calc R . . C3 C 0.31470(5) 0.3083(3) 0.27429(13) 0.0193(4) Uani 1 1 d . . . H3 H 0.3076 0.2165 0.1967 0.023 Uiso 1 1 calc R . . C4 C 0.34806(4) 0.5105(3) 0.30635(13) 0.0177(3) Uani 1 1 d . . . H4 H 0.3639 0.5575 0.2507 0.021 Uiso 1 1 calc R . . C5 C 0.35782(4) 0.6438(3) 0.42335(13) 0.0157(3) Uani 1 1 d . . . C6 C 0.39287(4) 0.8602(3) 0.46314(12) 0.0154(3) Uani 1 1 d . . . C7 C 0.40726(4) 1.0048(3) 0.57523(13) 0.0162(3) Uani 1 1 d . . . H7 H 0.3968 0.9869 0.6446 0.019 Uiso 1 1 calc R . . C8 C 0.46886(5) 1.3634(3) 0.65578(13) 0.0183(4) Uani 1 1 d . . . H8A H 0.4524 1.4864 0.6978 0.022 Uiso 1 1 calc R . . H8B H 0.4847 1.4965 0.6156 0.022 Uiso 1 1 calc R . . C9 C 0.5 1.1691(4) 0.75 0.0159(4) Uani 1 2 d S . . H9A H 0.4842 1.0409 0.7923 0.019 Uiso 0.5 1 calc PR . . H9B H 0.5158 1.0409 0.7077 0.019 Uiso 0.5 1 calc PR . . N1 N 0.33598(4) 0.5820(3) 0.50702(11) 0.0194(3) Uani 1 1 d . . . N2 N 0.41737(4) 0.9513(3) 0.38800(11) 0.0183(3) Uani 1 1 d . . . N3 N 0.44594(4) 1.1446(3) 0.44850(11) 0.0189(3) Uani 1 1 d . . . N4 N 0.43975(4) 1.1775(3) 0.56227(11) 0.0163(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 C1 0.0195(8) 0.0280(8) 0.0193(8) 0.0011(6) 0.0080(6) -0.0030(6) C2 0.0154(7) 0.0226(8) 0.0224(8) 0.0000(6) 0.0016(6) -0.0024(6) C3 0.0209(8) 0.0200(7) 0.0145(7) -0.0013(6) 0.0006(6) 0.0023(6) C4 0.0178(8) 0.0206(7) 0.0149(7) 0.0021(6) 0.0045(6) 0.0025(6) C5 0.0140(7) 0.0175(7) 0.0146(7) 0.0029(5) 0.0022(6) 0.0038(5) C6 0.0150(7) 0.0176(7) 0.0132(7) 0.0024(5) 0.0030(6) 0.0037(5) C7 0.0153(7) 0.0180(7) 0.0151(7) 0.0018(5) 0.0039(6) 0.0015(5) C8 0.0180(8) 0.0171(7) 0.0178(8) -0.0021(5) 0.0013(6) -0.0012(5) C9 0.0158(10) 0.0166(10) 0.0154(9) 0 0.0045(8) 0 N1 0.0185(7) 0.0242(7) 0.0159(6) 0.0006(5) 0.0053(5) -0.0011(5) N2 0.0166(7) 0.0224(7) 0.0160(6) 0.0002(5) 0.0043(5) -0.0006(5) N3 0.0181(7) 0.0227(7) 0.0155(6) 0.0003(5) 0.0040(5) -0.0007(5) N4 0.0149(6) 0.0187(6) 0.0138(6) 0.0008(4) 0.0015(5) 0.0011(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.332(2) . ? C1 C2 1.382(2) . ? C1 H1 0.93 . ? C2 C3 1.386(2) . ? C2 H2 0.93 . ? C3 C4 1.376(2) . ? C3 H3 0.93 . ? C4 C5 1.393(2) . ? C4 H4 0.93 . ? C5 N1 1.3453(18) . ? C5 C6 1.462(2) . ? C6 N2 1.3643(18) . ? C6 C7 1.374(2) . ? C7 N4 1.3415(19) . ? C7 H7 0.93 . ? C8 N4 1.4603(19) . ? C8 C9 1.5164(19) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C8 1.5164(19) 2_656 ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? N2 N3 1.3092(19) . ? N3 N4 1.3491(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.32(13) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 118.02(14) . . ? C1 C2 H2 121 . . ? C3 C2 H2 121 . . ? C4 C3 C2 118.95(13) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.04(13) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.59(14) . . ? N1 C5 C6 115.66(12) . . ? C4 C5 C6 121.75(13) . . ? N2 C6 C7 108.27(13) . . ? N2 C6 C5 122.70(12) . . ? C7 C6 C5 129.02(13) . . ? N4 C7 C6 104.56(12) . . ? N4 C7 H7 127.7 . . ? C6 C7 H7 127.7 . . ? N4 C8 C9 110.80(13) . . ? N4 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C8 110.57(17) 2_656 . ? C8 C9 H9A 109.5 2_656 . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 2_656 . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C1 N1 C5 117.07(13) . . ? N3 N2 C6 108.87(12) . . ? N2 N3 N4 107.14(11) . . ? C7 N4 N3 111.15(12) . . ? C7 N4 C8 128.27(12) . . ? N3 N4 C8 120.38(12) . . ? # END of CIF