# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_paper _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- dalton_dmitry.cif' _publ_contact_author ; Prof Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@unistra.fr _publ_contact_author_fax '33 3 68 85 13 23' _publ_contact_author_phone '33 3 68 85 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address 'Pogozhev, Dmitry' ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; "Baudron, St\'ephane A." ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; 'Hosseini, Mir Wais' ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_section_title ; Dipyrrin based silver [2+2] metallamacrocycles ; ###Material relevant to compound 2 at 173K ######## data_2 _database_code_depnum_ccdc_archive 'CCDC 791545' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H15 N3' _chemical_formula_sum 'C20 H15 N3' _chemical_formula_weight 297.35 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1131(3) _cell_length_b 7.2051(2) _cell_length_c 19.4251(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.5270(10) _cell_angle_gamma 90.00 _cell_volume 1498.62(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5119 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9843 _exptl_absorpt_correction_T_max 0.9921 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11268 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.74 _reflns_number_total 3465 _reflns_number_gt 2959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.6794P] 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 3465 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _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 0.41234(14) 0.6284(2) 0.41432(8) 0.0350(3) Uani 1 1 d . . . H1 H 0.4733 0.5390 0.4159 0.042 Uiso 1 1 calc R . . C2 C 0.41521(14) 0.7597(2) 0.46793(8) 0.0346(3) Uani 1 1 d . . . H2 H 0.4770 0.7724 0.5107 0.041 Uiso 1 1 calc R . . C3 C 0.30897(13) 0.8668(2) 0.44527(7) 0.0298(3) Uani 1 1 d . . . H3 H 0.2855 0.9650 0.4699 0.036 Uiso 1 1 calc R . . C4 C 0.24245(12) 0.79888(19) 0.37743(7) 0.0261(3) Uani 1 1 d . . . C5 C 0.13287(12) 0.86598(18) 0.32946(7) 0.0251(3) Uani 1 1 d . . . C6 C 0.07811(12) 0.78844(19) 0.26235(7) 0.0250(3) Uani 1 1 d . . . C7 C -0.03965(13) 0.8320(2) 0.21467(8) 0.0311(3) Uani 1 1 d . . . H7 H -0.0928 0.9277 0.2198 0.037 Uiso 1 1 calc R . . C8 C -0.06004(14) 0.7064(2) 0.15978(8) 0.0349(3) Uani 1 1 d . . . H8 H -0.1299 0.6995 0.1207 0.042 Uiso 1 1 calc R . . C9 C 0.04567(14) 0.5896(2) 0.17412(8) 0.0337(3) Uani 1 1 d . . . H9 H 0.0560 0.4920 0.1449 0.040 Uiso 1 1 calc R . . C10 C 0.06733(12) 1.02866(19) 0.35069(7) 0.0252(3) Uani 1 1 d . . . C11 C 0.06729(16) 1.1999(2) 0.31770(9) 0.0374(4) Uani 1 1 d . . . H11 H 0.1135 1.2158 0.2847 0.045 Uiso 1 1 calc R . . C12 C -0.00090(15) 1.3471(2) 0.33351(9) 0.0354(4) Uani 1 1 d . . . H12 H 0.0005 1.4609 0.3111 0.043 Uiso 1 1 calc R . . C13 C -0.07161(12) 1.32731(19) 0.38249(7) 0.0251(3) Uani 1 1 d . . . C14 C -0.07078(12) 1.15602(19) 0.41569(7) 0.0258(3) Uani 1 1 d . . . H14 H -0.1173 1.1399 0.4485 0.031 Uiso 1 1 calc R . . C15 C -0.00152(12) 1.00914(19) 0.40051(7) 0.0257(3) Uani 1 1 d . . . H15 H -0.0010 0.8963 0.4239 0.031 Uiso 1 1 calc R . . C16 C -0.14576(12) 1.48515(19) 0.39837(7) 0.0258(3) Uani 1 1 d . . . C17 C -0.19786(13) 1.6187(2) 0.34703(8) 0.0317(3) Uani 1 1 d . . . H17 H -0.1873 1.6103 0.3012 0.038 Uiso 1 1 calc R . . C18 C -0.26554(14) 1.7642(2) 0.36481(9) 0.0369(4) Uani 1 1 d . . . H18 H -0.3003 1.8505 0.3295 0.044 Uiso 1 1 calc R . . C19 C -0.23401(15) 1.6601(2) 0.47814(9) 0.0384(4) Uani 1 1 d . . . H19 H -0.2455 1.6734 0.5236 0.046 Uiso 1 1 calc R . . C20 C -0.16609(13) 1.5084(2) 0.46564(8) 0.0318(3) Uani 1 1 d . . . H20 H -0.1344 1.4228 0.5018 0.038 Uiso 1 1 calc R . . N1 N 0.30956(11) 0.65032(17) 0.36084(7) 0.0307(3) Uani 1 1 d . . . H1A H 0.2884 0.5841 0.3227 0.037 Uiso 1 1 calc R . . N2 N 0.12871(11) 0.63671(17) 0.23472(6) 0.0289(3) Uani 1 1 d . . . N3 N -0.28402(12) 1.78851(19) 0.42925(8) 0.0395(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 0.0343(7) 0.0314(8) 0.0391(8) 0.0074(6) 0.0097(6) 0.0087(6) C2 0.0355(7) 0.0382(9) 0.0284(7) 0.0049(6) 0.0058(6) 0.0022(6) C3 0.0354(7) 0.0271(7) 0.0291(7) 0.0003(6) 0.0125(6) -0.0009(6) C4 0.0292(6) 0.0219(7) 0.0293(7) 0.0005(5) 0.0115(5) 0.0003(5) C5 0.0298(6) 0.0192(6) 0.0299(7) 0.0008(5) 0.0141(5) -0.0006(5) C6 0.0280(6) 0.0213(7) 0.0279(6) 0.0003(5) 0.0115(5) 0.0004(5) C7 0.0315(7) 0.0298(8) 0.0329(7) 0.0029(6) 0.0102(6) 0.0028(6) C8 0.0340(7) 0.0410(9) 0.0284(7) -0.0019(6) 0.0061(6) -0.0026(6) C9 0.0401(8) 0.0346(8) 0.0298(7) -0.0074(6) 0.0149(6) -0.0028(6) C10 0.0265(6) 0.0213(7) 0.0287(6) -0.0021(5) 0.0089(5) 0.0006(5) C11 0.0512(9) 0.0251(8) 0.0472(9) 0.0039(7) 0.0327(8) 0.0028(7) C12 0.0474(8) 0.0204(7) 0.0467(9) 0.0044(6) 0.0268(7) 0.0018(6) C13 0.0257(6) 0.0213(7) 0.0283(6) -0.0035(5) 0.0075(5) -0.0003(5) C14 0.0267(6) 0.0264(7) 0.0258(6) -0.0002(5) 0.0095(5) 0.0002(5) C15 0.0281(6) 0.0221(7) 0.0271(6) 0.0030(5) 0.0074(5) 0.0013(5) C16 0.0226(6) 0.0203(7) 0.0346(7) -0.0048(5) 0.0078(5) -0.0030(5) C17 0.0323(7) 0.0255(7) 0.0374(8) -0.0030(6) 0.0093(6) -0.0008(6) C18 0.0336(7) 0.0253(8) 0.0494(9) -0.0011(7) 0.0069(7) 0.0030(6) C19 0.0374(8) 0.0370(9) 0.0450(9) -0.0111(7) 0.0184(7) -0.0006(7) C20 0.0304(7) 0.0294(8) 0.0365(7) -0.0037(6) 0.0106(6) 0.0005(6) N1 0.0338(6) 0.0251(6) 0.0327(6) -0.0016(5) 0.0080(5) 0.0047(5) N2 0.0333(6) 0.0268(6) 0.0293(6) -0.0043(5) 0.0132(5) 0.0001(5) N3 0.0328(6) 0.0305(7) 0.0571(8) -0.0081(6) 0.0151(6) 0.0039(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3316(19) . ? C1 C2 1.401(2) . ? C1 H1 0.9300 . ? C2 C3 1.380(2) . ? C2 H2 0.9300 . ? C3 C4 1.414(2) . ? C3 H3 0.9300 . ? C4 N1 1.3909(17) . ? C4 C5 1.4062(19) . ? C5 C6 1.3989(19) . ? C5 C10 1.4951(18) . ? C6 N2 1.4004(17) . ? C6 C7 1.4214(19) . ? C7 C8 1.371(2) . ? C7 H7 0.9300 . ? C8 C9 1.411(2) . ? C8 H8 0.9300 . ? C9 N2 1.3309(19) . ? C9 H9 0.9300 . ? C10 C11 1.390(2) . ? C10 C15 1.3924(18) . ? C11 C12 1.385(2) . ? C11 H11 0.9300 . ? C12 C13 1.3939(19) . ? C12 H12 0.9300 . ? C13 C14 1.3914(19) . ? C13 C16 1.4845(18) . ? C14 C15 1.3859(18) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.3945(19) . ? C16 C17 1.395(2) . ? C17 C18 1.387(2) . ? C17 H17 0.9300 . ? C18 N3 1.333(2) . ? C18 H18 0.9300 . ? C19 N3 1.336(2) . ? C19 C20 1.386(2) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N1 H1A 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.12(13) . . ? N1 C1 H1 124.9 . . ? C2 C1 H1 124.9 . . ? C3 C2 C1 107.03(13) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.05(13) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 122.27(12) . . ? N1 C4 C3 107.64(12) . . ? C5 C4 C3 129.97(13) . . ? C6 C5 C4 124.32(12) . . ? C6 C5 C10 116.59(12) . . ? C4 C5 C10 119.09(12) . . ? C5 C6 N2 123.35(12) . . ? C5 C6 C7 127.88(13) . . ? N2 C6 C7 108.48(12) . . ? C8 C7 C6 107.01(13) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 106.56(13) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C8 111.46(13) . . ? N2 C9 H9 124.3 . . ? C8 C9 H9 124.3 . . ? C11 C10 C15 118.53(12) . . ? C11 C10 C5 120.59(12) . . ? C15 C10 C5 120.76(12) . . ? C12 C11 C10 120.68(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.99(13) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 118.18(12) . . ? C14 C13 C16 121.22(12) . . ? C12 C13 C16 120.61(13) . . ? C15 C14 C13 120.92(12) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C10 120.70(13) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C20 C16 C17 116.53(13) . . ? C20 C16 C13 121.66(13) . . ? C17 C16 C13 121.81(12) . . ? C18 C17 C16 119.49(14) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? N3 C18 C17 124.29(15) . . ? N3 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? N3 C19 C20 124.34(15) . . ? N3 C19 H19 117.8 . . ? C20 C19 H19 117.8 . . ? C19 C20 C16 119.41(14) . . ? C19 C20 H20 120.3 . . ? C16 C20 H20 120.3 . . ? C1 N1 C4 108.15(12) . . ? C1 N1 H1A 125.9 . . ? C4 N1 H1A 125.9 . . ? C9 N2 C6 106.49(12) . . ? C18 N3 C19 115.93(13) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.74 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.372 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.043 #===END ###Material relevant to compound 3 at 173K ## data_3 _database_code_depnum_ccdc_archive 'CCDC 791546' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 N4' _chemical_formula_sum 'C18 H14 N4' _chemical_formula_weight 286.33 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' _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 12.8270(6) _cell_length_b 12.5383(5) _cell_length_c 18.6260(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.777(2) _cell_angle_gamma 90.00 _cell_volume 2836.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2896 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.09 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9836 _exptl_absorpt_correction_T_max 0.9934 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8513 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3261 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+1.9629P] 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 3261 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 1.07129(13) 1.33308(12) 0.35813(9) 0.0371(4) Uani 1 1 d . . . H1 H 1.0737 1.4057 0.3485 0.044 Uiso 1 1 calc R . . C2 C 1.15938(13) 1.27314(12) 0.40362(9) 0.0359(3) Uani 1 1 d . . . H2 H 1.2297 1.2981 0.4296 0.043 Uiso 1 1 calc R . . C3 C 1.12220(12) 1.16961(11) 0.40280(8) 0.0311(3) Uani 1 1 d . . . H3 H 1.1631 1.1118 0.4282 0.037 Uiso 1 1 calc R . . C4 C 1.01107(11) 1.16767(11) 0.35647(7) 0.0270(3) Uani 1 1 d . . . C5 C 0.93571(11) 1.08170(11) 0.33839(7) 0.0269(3) Uani 1 1 d . . . C6 C 0.82478(12) 1.09209(11) 0.29546(8) 0.0294(3) Uani 1 1 d . . . C7 C 0.74389(13) 1.01118(13) 0.26715(9) 0.0377(4) Uani 1 1 d . . . H7 H 0.7535 0.9382 0.2756 0.045 Uiso 1 1 calc R . . C8 C 0.64952(14) 1.06143(15) 0.22521(10) 0.0468(4) Uani 1 1 d . . . H8 H 0.5826 1.0293 0.1993 0.056 Uiso 1 1 calc R . . C9 C 0.67331(13) 1.17181(15) 0.22885(9) 0.0436(4) Uani 1 1 d . . . H9 H 0.6226 1.2242 0.2052 0.052 Uiso 1 1 calc R . . C10 C 0.98007(11) 0.97474(11) 0.36725(8) 0.0267(3) Uani 1 1 d . . . C11 C 0.93786(12) 0.91719(11) 0.41569(8) 0.0302(3) Uani 1 1 d . . . H11 H 0.8790 0.9446 0.4288 0.036 Uiso 1 1 calc R . . C12 C 0.98259(12) 0.81978(11) 0.44451(8) 0.0297(3) Uani 1 1 d . . . H12 H 0.9538 0.7822 0.4769 0.036 Uiso 1 1 calc R . . C13 C 1.07036(11) 0.77767(10) 0.42530(7) 0.0257(3) Uani 1 1 d . . . C14 C 1.11267(12) 0.83375(11) 0.37667(8) 0.0305(3) Uani 1 1 d . . . H14 H 1.1709 0.8057 0.3633 0.037 Uiso 1 1 calc R . . C15 C 1.06813(12) 0.93113(11) 0.34827(8) 0.0301(3) Uani 1 1 d . . . H15 H 1.0972 0.9685 0.3159 0.036 Uiso 1 1 calc R . . C16 C 1.18955(13) 0.61708(12) 0.43400(9) 0.0363(3) Uani 1 1 d . . . H16 H 1.2182 0.6371 0.3961 0.044 Uiso 1 1 calc R . . C17 C 1.09603(15) 0.62073(14) 0.51274(11) 0.0499(5) Uani 1 1 d . . . H17 H 1.0498 0.6405 0.5400 0.060 Uiso 1 1 calc R . . C18 C 1.15588(14) 0.53062(14) 0.52116(11) 0.0481(4) Uani 1 1 d . . . H18 H 1.1569 0.4772 0.5560 0.058 Uiso 1 1 calc R . . N1 N 0.98314(10) 1.27090(9) 0.33047(7) 0.0327(3) Uani 1 1 d . . . H1A H 0.9196 1.2913 0.3014 0.039 Uiso 1 1 calc R . . N2 N 0.77693(10) 1.19135(10) 0.27024(7) 0.0356(3) Uani 1 1 d . . . N3 N 1.11678(10) 0.67765(9) 0.45583(7) 0.0288(3) Uani 1 1 d . . . N4 N 1.21482(11) 0.52794(10) 0.47198(8) 0.0388(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 0.0408(9) 0.0299(7) 0.0418(8) 0.0043(6) 0.0151(7) -0.0042(6) C2 0.0303(7) 0.0371(8) 0.0397(8) -0.0007(6) 0.0107(7) -0.0048(6) C3 0.0296(7) 0.0320(7) 0.0327(7) 0.0017(6) 0.0115(6) 0.0020(6) C4 0.0287(7) 0.0283(7) 0.0263(7) 0.0013(5) 0.0121(6) 0.0015(5) C5 0.0298(7) 0.0300(7) 0.0243(6) -0.0016(5) 0.0136(6) 0.0022(6) C6 0.0292(7) 0.0342(7) 0.0270(7) -0.0014(5) 0.0123(6) 0.0015(6) C7 0.0343(8) 0.0411(9) 0.0399(8) -0.0067(7) 0.0150(7) -0.0032(7) C8 0.0303(8) 0.0619(11) 0.0430(9) -0.0064(8) 0.0047(7) -0.0066(8) C9 0.0309(8) 0.0575(10) 0.0374(8) 0.0061(7) 0.0038(7) 0.0057(7) C10 0.0256(7) 0.0277(7) 0.0278(6) -0.0035(5) 0.0099(5) -0.0006(5) C11 0.0280(7) 0.0308(7) 0.0370(7) -0.0031(6) 0.0178(6) 0.0014(6) C12 0.0313(7) 0.0304(7) 0.0332(7) -0.0009(5) 0.0182(6) -0.0011(6) C13 0.0239(6) 0.0254(6) 0.0275(6) -0.0041(5) 0.0078(5) -0.0004(5) C14 0.0282(7) 0.0312(7) 0.0376(7) -0.0044(6) 0.0183(6) 0.0010(6) C15 0.0308(7) 0.0315(7) 0.0330(7) -0.0006(6) 0.0173(6) -0.0008(6) C16 0.0422(8) 0.0320(7) 0.0390(8) -0.0022(6) 0.0188(7) 0.0071(7) C17 0.0462(10) 0.0508(10) 0.0665(12) 0.0223(9) 0.0370(9) 0.0139(8) C18 0.0401(9) 0.0418(9) 0.0695(12) 0.0212(8) 0.0275(9) 0.0080(7) N1 0.0312(6) 0.0306(6) 0.0346(6) 0.0059(5) 0.0082(5) 0.0027(5) N2 0.0302(6) 0.0421(7) 0.0320(6) 0.0059(5) 0.0067(5) 0.0048(5) N3 0.0268(6) 0.0271(6) 0.0339(6) -0.0013(5) 0.0120(5) 0.0004(5) N4 0.0404(7) 0.0302(6) 0.0463(8) -0.0009(6) 0.0146(6) 0.0044(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.333(2) . ? C1 C2 1.394(2) . ? C1 H1 0.9300 . ? C2 C3 1.381(2) . ? C2 H2 0.9300 . ? C3 C4 1.409(2) . ? C3 H3 0.9300 . ? C4 N1 1.3879(17) . ? C4 C5 1.4143(19) . ? C5 C6 1.396(2) . ? C5 C10 1.4881(19) . ? C6 N2 1.4003(19) . ? C6 C7 1.425(2) . ? C7 C8 1.365(2) . ? C7 H7 0.9300 . ? C8 C9 1.414(3) . ? C8 H8 0.9300 . ? C9 N2 1.327(2) . ? C9 H9 0.9300 . ? C10 C11 1.3937(19) . ? C10 C15 1.3988(18) . ? C11 C12 1.382(2) . ? C11 H11 0.9300 . ? C12 C13 1.3906(18) . ? C12 H12 0.9300 . ? C13 C14 1.3878(19) . ? C13 N3 1.4257(17) . ? C14 C15 1.379(2) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N4 1.307(2) . ? C16 N3 1.3630(18) . ? C16 H16 0.9300 . ? C17 C18 1.346(2) . ? C17 N3 1.3730(19) . ? C17 H17 0.9300 . ? C18 N4 1.363(2) . ? C18 H18 0.9300 . ? N1 H1A 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.90(13) . . ? N1 C1 H1 125.1 . . ? C2 C1 H1 125.1 . . ? C3 C2 C1 106.89(14) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 107.49(13) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C3 107.11(12) . . ? N1 C4 C5 123.22(13) . . ? C3 C4 C5 129.65(13) . . ? C6 C5 C4 123.90(13) . . ? C6 C5 C10 119.46(12) . . ? C4 C5 C10 116.64(12) . . ? C5 C6 N2 122.07(13) . . ? C5 C6 C7 129.19(14) . . ? N2 C6 C7 108.68(13) . . ? C8 C7 C6 106.80(15) . . ? C8 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? C7 C8 C9 106.64(15) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C8 111.65(15) . . ? N2 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? C11 C10 C15 118.35(13) . . ? C11 C10 C5 121.15(12) . . ? C15 C10 C5 120.46(12) . . ? C12 C11 C10 120.65(12) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.31(12) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.64(13) . . ? C14 C13 N3 120.34(12) . . ? C12 C13 N3 120.01(12) . . ? C15 C14 C13 119.88(12) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 121.17(12) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? N4 C16 N3 112.92(13) . . ? N4 C16 H16 123.5 . . ? N3 C16 H16 123.5 . . ? C18 C17 N3 106.33(14) . . ? C18 C17 H17 126.8 . . ? N3 C17 H17 126.8 . . ? C17 C18 N4 111.18(14) . . ? C17 C18 H18 124.4 . . ? N4 C18 H18 124.4 . . ? C1 N1 C4 108.60(12) . . ? C1 N1 H1A 125.7 . . ? C4 N1 H1A 125.7 . . ? C9 N2 C6 106.24(13) . . ? C16 N3 C17 105.20(12) . . ? C16 N3 C13 127.54(12) . . ? C17 N3 C13 127.25(12) . . ? C16 N4 C18 104.37(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.255 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.039 #===END ###Material relevant to compound 6 at 173K ## data_6 _database_code_depnum_ccdc_archive 'CCDC 791547' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 Ag2 N6, 3(C6 H6), 2(C F3 O3 S)' _chemical_formula_sum 'C48 H40 Ag2 F6 N6 O6 S2' _chemical_formula_weight 1190.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 '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 9.2123(4) _cell_length_b 10.0695(5) _cell_length_c 13.2746(6) _cell_angle_alpha 102.508(3) _cell_angle_beta 93.810(3) _cell_angle_gamma 97.941(3) _cell_volume 1184.71(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1266 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.93 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8335 _exptl_absorpt_correction_T_max 0.9708 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9920 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.1199 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.06 _reflns_number_total 5061 _reflns_number_gt 3592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+1.6016P] 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 5061 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.000 _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 0.1647(9) 0.5555(8) 0.1157(6) 0.0339(18) Uani 1 1 d . . . H1 H 0.1143 0.5703 0.1746 0.041 Uiso 1 1 calc R . . C2 C 0.2477(9) 0.6634(8) 0.0792(6) 0.0356(18) Uani 1 1 d . . . H2 H 0.2589 0.7574 0.1079 0.043 Uiso 1 1 calc R . . C3 C 0.3057(8) 0.6014(8) -0.0045(6) 0.0313(17) Uani 1 1 d . . . H3 H 0.3658 0.6456 -0.0448 0.038 Uiso 1 1 calc R . . C4 C 0.2598(7) 0.4532(7) -0.0223(6) 0.0257(15) Uani 1 1 d . . . C5 C 0.2911(7) 0.3467(7) -0.0955(5) 0.0223(14) Uani 1 1 d . . . C6 C 0.3894(8) 0.3528(7) -0.1745(6) 0.0292(16) Uani 1 1 d . . . C7 C 0.4192(8) 0.2420(8) -0.2488(6) 0.0333(18) Uani 1 1 d . . . H7 H 0.3800 0.1500 -0.2552 0.040 Uiso 1 1 calc R . . C8 C 0.5175(9) 0.2922(9) -0.3119(7) 0.040(2) Uani 1 1 d . . . H8 H 0.5577 0.2406 -0.3669 0.048 Uiso 1 1 calc R . . C9 C 0.5439(9) 0.4341(8) -0.2767(7) 0.0374(19) Uani 1 1 d . . . H9 H 0.6036 0.4956 -0.3053 0.045 Uiso 1 1 calc R . . C10 C 0.2149(7) 0.2026(7) -0.1003(6) 0.0249(15) Uani 1 1 d . . . C11 C 0.0672(8) 0.1651(8) -0.1382(6) 0.0288(16) Uani 1 1 d . . . H11 H 0.0156 0.2280 -0.1609 0.035 Uiso 1 1 calc R . . C12 C -0.0021(8) 0.0327(7) -0.1417(6) 0.0271(16) Uani 1 1 d . . . H12 H -0.1014 0.0094 -0.1661 0.033 Uiso 1 1 calc R . . C13 C 0.2860(7) 0.1035(8) -0.0712(6) 0.0269(15) Uani 1 1 d . . . H13 H 0.3853 0.1242 -0.0466 0.032 Uiso 1 1 calc R . . C14 C 0.2099(8) -0.0263(7) -0.0785(6) 0.0291(16) Uani 1 1 d . . . H14 H 0.2608 -0.0921 -0.0594 0.035 Uiso 1 1 calc R . . N1 N 0.1676(6) 0.4330(6) 0.0567(5) 0.0269(13) Uani 1 1 d . . . N2 N 0.4688(7) 0.4676(6) -0.1945(5) 0.0304(14) Uani 1 1 d . . . H2A H 0.4703 0.5501 -0.1590 0.037 Uiso 1 1 calc R . . N3 N 0.0659(7) -0.0632(6) -0.1119(5) 0.0296(14) Uani 1 1 d . . . Ag1 Ag 0.06260(7) 0.25233(6) 0.09745(5) 0.0351(2) Uani 1 1 d . . . C15 C 0.5167(9) 0.1677(9) 0.3293(7) 0.0369(19) Uani 1 1 d . . . O1 O 0.5204(6) 0.2356(6) 0.1556(5) 0.0415(14) Uani 1 1 d . . . O2 O 0.2873(6) 0.2073(6) 0.2274(5) 0.0402(14) Uani 1 1 d . . . O3 O 0.3975(6) 0.0061(5) 0.1571(5) 0.0405(14) Uani 1 1 d . . . F1 F 0.5362(7) 0.2946(7) 0.3857(5) 0.0700(19) Uani 1 1 d . . . F2 F 0.4444(7) 0.0860(8) 0.3826(5) 0.0735(19) Uani 1 1 d . . . F3 F 0.6478(5) 0.1297(6) 0.3224(5) 0.0620(16) Uani 1 1 d . . . S1 S 0.41903(19) 0.15122(19) 0.20314(15) 0.0284(4) Uani 1 1 d . . . C16 C 1.0129(14) 0.6328(11) 0.6746(8) 0.061(3) Uani 1 1 d . . . H16 H 1.0277 0.7282 0.6971 0.073 Uiso 1 1 calc R . . C17 C 0.8845(11) 0.5649(12) 0.6135(7) 0.055(3) Uani 1 1 d . . . H17 H 0.8137 0.6152 0.5952 0.066 Uiso 1 1 calc R . . C18 C 0.8622(10) 0.4268(13) 0.5808(7) 0.059(3) Uani 1 1 d . . . H18 H 0.7760 0.3818 0.5400 0.070 Uiso 1 1 calc R . . C19 C 0.9675(12) 0.3517(9) 0.6077(7) 0.051(2) Uani 1 1 d . . . H19 H 0.9538 0.2563 0.5853 0.062 Uiso 1 1 calc R . . C20 C 1.0918(12) 0.4215(13) 0.6681(8) 0.061(3) Uani 1 1 d . . . H20 H 1.1626 0.3716 0.6872 0.073 Uiso 1 1 calc R . . C21 C 1.1165(11) 0.5599(13) 0.7014(8) 0.059(3) Uani 1 1 d . . . H21 H 1.2030 0.6043 0.7420 0.071 Uiso 1 1 calc R . . C22 C 0.1524(10) 0.0357(10) 0.5200(7) 0.047(2) Uani 1 1 d . . . H22 H 0.2541 0.0593 0.5336 0.056 Uiso 1 1 calc R . . C23 C 0.0816(10) 0.0462(9) 0.4271(7) 0.045(2) Uani 1 1 d . . . H23 H 0.1355 0.0773 0.3776 0.055 Uiso 1 1 calc R . . C24 C 0.0695(10) -0.0099(10) 0.5913(7) 0.046(2) Uani 1 1 d . . . H24 H 0.1164 -0.0167 0.6539 0.056 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 C1 0.039(4) 0.020(4) 0.041(5) 0.003(3) 0.008(4) 0.002(3) C2 0.047(5) 0.018(3) 0.041(5) 0.003(3) 0.013(4) 0.002(3) C3 0.037(4) 0.021(4) 0.037(4) 0.010(3) 0.009(3) -0.002(3) C4 0.025(3) 0.018(3) 0.032(4) 0.006(3) 0.002(3) -0.002(3) C5 0.022(3) 0.015(3) 0.030(4) 0.009(3) -0.003(3) 0.001(3) C6 0.025(4) 0.021(3) 0.038(4) 0.003(3) 0.003(3) -0.003(3) C7 0.033(4) 0.027(4) 0.035(4) 0.002(3) 0.010(3) -0.007(3) C8 0.049(5) 0.032(4) 0.039(5) 0.010(4) 0.017(4) 0.002(4) C9 0.037(4) 0.031(4) 0.045(5) 0.015(4) 0.013(4) -0.006(3) C10 0.020(3) 0.023(3) 0.030(4) 0.005(3) 0.002(3) 0.000(3) C11 0.024(4) 0.025(4) 0.037(4) 0.010(3) 0.000(3) -0.001(3) C12 0.023(3) 0.023(3) 0.032(4) 0.003(3) -0.002(3) -0.004(3) C13 0.019(3) 0.031(4) 0.031(4) 0.012(3) -0.003(3) -0.002(3) C14 0.034(4) 0.020(3) 0.035(4) 0.004(3) 0.012(3) 0.009(3) N1 0.034(3) 0.023(3) 0.026(3) 0.009(3) 0.010(3) 0.001(3) N2 0.036(3) 0.020(3) 0.035(4) 0.007(3) 0.012(3) 0.001(3) N3 0.030(3) 0.025(3) 0.032(3) 0.006(3) 0.009(3) -0.002(3) Ag1 0.0418(4) 0.0216(3) 0.0417(4) 0.0094(2) 0.0136(3) -0.0029(2) C15 0.034(4) 0.039(5) 0.040(5) 0.019(4) -0.001(4) 0.002(4) O1 0.044(3) 0.028(3) 0.052(4) 0.010(3) 0.014(3) -0.002(2) O2 0.031(3) 0.034(3) 0.056(4) 0.007(3) 0.002(3) 0.010(2) O3 0.045(3) 0.022(3) 0.054(4) 0.010(3) 0.001(3) 0.001(2) F1 0.078(4) 0.064(4) 0.052(4) -0.012(3) -0.018(3) 0.007(3) F2 0.067(4) 0.105(6) 0.058(4) 0.045(4) 0.005(3) 0.004(4) F3 0.037(3) 0.073(4) 0.079(4) 0.026(3) -0.012(3) 0.017(3) S1 0.0281(9) 0.0205(8) 0.0365(11) 0.0094(8) 0.0020(8) -0.0005(7) C16 0.095(8) 0.042(6) 0.041(6) 0.007(5) 0.025(6) -0.010(6) C17 0.059(6) 0.074(8) 0.043(6) 0.020(5) 0.015(5) 0.035(6) C18 0.042(5) 0.088(9) 0.033(5) -0.001(5) 0.008(4) -0.016(5) C19 0.080(7) 0.029(4) 0.047(6) 0.002(4) 0.021(5) 0.016(5) C20 0.062(7) 0.090(9) 0.045(6) 0.032(6) 0.009(5) 0.033(6) C21 0.051(6) 0.079(8) 0.038(5) 0.011(5) 0.003(4) -0.021(6) C22 0.034(4) 0.060(6) 0.044(5) 0.009(5) -0.003(4) 0.005(4) C23 0.047(5) 0.037(5) 0.053(6) 0.011(4) 0.017(4) 0.004(4) C24 0.043(5) 0.056(6) 0.040(5) 0.009(4) 0.000(4) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.315(9) . ? C1 C2 1.431(11) . ? C1 H1 0.9300 . ? C2 C3 1.334(11) . ? C2 H2 0.9300 . ? C3 C4 1.456(9) . ? C3 H3 0.9300 . ? C4 C5 1.360(9) . ? C4 N1 1.423(9) . ? C5 C6 1.436(10) . ? C5 C10 1.508(9) . ? C6 N2 1.366(9) . ? C6 C7 1.392(10) . ? C7 C8 1.391(10) . ? C7 H7 0.9300 . ? C8 C9 1.385(11) . ? C8 H8 0.9300 . ? C9 N2 1.338(10) . ? C9 H9 0.9300 . ? C10 C13 1.374(10) . ? C10 C11 1.389(9) . ? C11 C12 1.387(10) . ? C11 H11 0.9300 . ? C12 N3 1.334(10) . ? C12 H12 0.9300 . ? C13 C14 1.376(10) . ? C13 H13 0.9300 . ? C14 N3 1.345(9) . ? C14 H14 0.9300 . ? N1 Ag1 2.132(6) . ? N2 H2A 0.8600 . ? N3 Ag1 2.152(6) 2 ? Ag1 N3 2.152(6) 2 ? C15 F1 1.316(10) . ? C15 F3 1.319(10) . ? C15 F2 1.336(10) . ? C15 S1 1.811(8) . ? O1 S1 1.444(6) . ? O2 S1 1.435(6) . ? O3 S1 1.437(5) . ? C16 C21 1.356(16) . ? C16 C17 1.390(14) . ? C16 H16 0.9300 . ? C17 C18 1.347(15) . ? C17 H17 0.9300 . ? C18 C19 1.383(15) . ? C18 H18 0.9300 . ? C19 C20 1.364(14) . ? C19 H19 0.9300 . ? C20 C21 1.349(15) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C24 1.371(13) . ? C22 C23 1.387(13) . ? C22 H22 0.9300 . ? C23 C24 1.381(12) 2_556 ? C23 H23 0.9300 . ? C24 C23 1.381(12) 2_556 ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.4(7) . . ? N1 C1 H1 123.8 . . ? C2 C1 H1 123.8 . . ? C3 C2 C1 105.9(7) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? C2 C3 C4 108.8(7) . . ? C2 C3 H3 125.6 . . ? C4 C3 H3 125.6 . . ? C5 C4 N1 122.4(6) . . ? C5 C4 C3 131.5(7) . . ? N1 C4 C3 106.1(6) . . ? C4 C5 C6 127.7(6) . . ? C4 C5 C10 119.3(6) . . ? C6 C5 C10 112.9(6) . . ? N2 C6 C7 105.9(7) . . ? N2 C6 C5 127.5(7) . . ? C7 C6 C5 126.5(7) . . ? C8 C7 C6 108.4(7) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C9 C8 C7 106.6(7) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? N2 C9 C8 108.2(7) . . ? N2 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? C13 C10 C11 117.5(6) . . ? C13 C10 C5 122.9(6) . . ? C11 C10 C5 119.5(6) . . ? C12 C11 C10 119.1(7) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? N3 C12 C11 123.5(6) . . ? N3 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C10 C13 C14 119.8(6) . . ? C10 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N3 C14 C13 123.5(7) . . ? N3 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? C1 N1 C4 106.7(6) . . ? C1 N1 Ag1 120.4(5) . . ? C4 N1 Ag1 132.6(5) . . ? C9 N2 C6 110.8(6) . . ? C9 N2 H2A 124.6 . . ? C6 N2 H2A 124.6 . . ? C12 N3 C14 116.5(6) . . ? C12 N3 Ag1 119.3(5) . 2 ? C14 N3 Ag1 123.5(5) . 2 ? N1 Ag1 N3 169.7(2) . 2 ? F1 C15 F3 107.3(7) . . ? F1 C15 F2 107.9(8) . . ? F3 C15 F2 105.5(7) . . ? F1 C15 S1 112.4(6) . . ? F3 C15 S1 112.2(6) . . ? F2 C15 S1 111.1(6) . . ? O2 S1 O3 115.2(3) . . ? O2 S1 O1 113.9(4) . . ? O3 S1 O1 115.3(4) . . ? O2 S1 C15 103.4(4) . . ? O3 S1 C15 104.4(4) . . ? O1 S1 C15 102.3(4) . . ? C21 C16 C17 120.0(10) . . ? C21 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.4(10) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.0(9) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 118.1(9) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C21 C20 C19 122.8(10) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C20 C21 C16 118.7(10) . . ? C20 C21 H21 120.6 . . ? C16 C21 H21 120.6 . . ? C24 C22 C23 118.7(8) . . ? C24 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 119.4(9) 2_556 . ? C24 C23 H23 120.3 2_556 . ? C22 C23 H23 120.3 . . ? C22 C24 C23 121.8(9) . 2_556 ? C22 C24 H24 119.1 . . ? C23 C24 H24 119.1 2_556 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.756 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.200 #===END ###Material relevant to compound 7 at 173K ## data_7 _database_code_depnum_ccdc_archive 'CCDC 791548' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 Ag2 N6, 2(F6 Sb)' _chemical_formula_sum 'C28 H22 Ag2 F12 N6 Sb2' _chemical_formula_weight 1129.76 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 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 17.3749(9) _cell_length_b 12.6487(6) _cell_length_c 17.0711(8) _cell_angle_alpha 90.00 _cell_angle_beta 118.616(2) _cell_angle_gamma 90.00 _cell_volume 3293.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3804 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.81 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 2.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9182 _exptl_absorpt_correction_T_max 0.9444 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13212 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3756 _reflns_number_gt 2826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0086P)^2^+57.9638P] 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 3756 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1289 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _refine_ls_shift/su_max 0.000 _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 0.4199(5) 0.0842(10) 0.4014(6) 0.064(3) Uani 1 1 d . . . H1 H 0.3951 0.1395 0.4175 0.077 Uiso 1 1 calc R . . C2 C 0.3733(6) -0.0077(10) 0.3578(6) 0.066(3) Uani 1 1 d . . . H2 H 0.3148 -0.0226 0.3398 0.079 Uiso 1 1 calc R . . C3 C 0.4316(6) -0.0704(10) 0.3475(6) 0.066(3) Uani 1 1 d . . . H3 H 0.4210 -0.1370 0.3212 0.079 Uiso 1 1 calc R . . C4 C 0.5137(5) -0.0122(10) 0.3856(6) 0.059(3) Uani 1 1 d . . . C5 C 0.5925(5) -0.0462(9) 0.3912(5) 0.058(3) Uani 1 1 d . . . C6 C 0.6114(6) -0.1505(9) 0.3754(7) 0.060(3) Uani 1 1 d . . . C7 C 0.5694(7) -0.2450(9) 0.3708(8) 0.079(4) Uani 1 1 d . . . H7 H 0.5213 -0.2529 0.3804 0.095 Uiso 1 1 calc R . . C8 C 0.6085(8) -0.3234(11) 0.3503(11) 0.112(6) Uani 1 1 d . . . H8 H 0.5917 -0.3940 0.3428 0.135 Uiso 1 1 calc R . . C9 C 0.6778(8) -0.2820(10) 0.3424(11) 0.105(5) Uani 1 1 d . . . H9 H 0.7157 -0.3190 0.3281 0.126 Uiso 1 1 calc R . . C10 C 0.6647(5) 0.0324(9) 0.4159(5) 0.052(2) Uani 1 1 d . . . C11 C 0.7427(6) 0.0231(10) 0.4959(6) 0.067(3) Uani 1 1 d . . . H11 H 0.7500 -0.0321 0.5348 0.080 Uiso 1 1 calc R . . C12 C 0.8087(5) 0.0954(10) 0.5173(6) 0.068(3) Uani 1 1 d . . . H12 H 0.8593 0.0880 0.5718 0.082 Uiso 1 1 calc R . . C13 C 0.7303(5) 0.1819(9) 0.3860(5) 0.054(2) Uani 1 1 d . . . H13 H 0.7260 0.2349 0.3464 0.064 Uiso 1 1 calc R . . C14 C 0.6602(5) 0.1146(8) 0.3604(5) 0.052(3) Uani 1 1 d . . . H14 H 0.6098 0.1243 0.3060 0.062 Uiso 1 1 calc R . . N1 N 0.5021(4) 0.0843(8) 0.4173(5) 0.061(2) Uani 1 1 d . . . N2 N 0.6804(5) -0.1755(9) 0.3595(7) 0.084(3) Uani 1 1 d . . . H2A H 0.7185 -0.1316 0.3603 0.100 Uiso 1 1 calc R . . N3 N 0.8048(4) 0.1763(7) 0.4644(5) 0.053(2) Uani 1 1 d . . . Ag1 Ag 0.59449(4) 0.20702(8) 0.48334(5) 0.0696(3) Uani 1 1 d . . . F1 F 0.3175(4) 0.4778(6) 0.3559(5) 0.096(2) Uani 1 1 d . . . F2 F 0.3529(4) 0.4587(6) 0.2239(4) 0.084(2) Uani 1 1 d . . . F3 F 0.3293(4) 0.2921(6) 0.2979(4) 0.089(2) Uani 1 1 d . . . F4 F 0.4894(4) 0.3330(8) 0.3223(4) 0.122(3) Uani 1 1 d . . . F5 F 0.4539(5) 0.3503(7) 0.4564(4) 0.113(3) Uani 1 1 d . . . F6 F 0.4751(5) 0.5279(8) 0.3829(5) 0.127(3) Uani 1 1 d . . . Sb1 Sb 0.40465(4) 0.40832(7) 0.34060(4) 0.0610(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(4) 0.115(10) 0.041(5) 0.019(6) 0.018(4) 0.024(6) C2 0.034(4) 0.116(10) 0.047(5) 0.012(6) 0.019(4) 0.001(6) C3 0.042(5) 0.106(10) 0.048(5) 0.018(6) 0.020(4) 0.006(5) C4 0.034(4) 0.104(9) 0.036(4) 0.025(5) 0.016(4) 0.010(5) C5 0.034(4) 0.105(9) 0.035(4) 0.023(5) 0.016(4) 0.014(5) C6 0.041(5) 0.070(7) 0.074(7) 0.039(6) 0.033(5) 0.017(5) C7 0.056(6) 0.075(8) 0.121(10) 0.058(7) 0.054(7) 0.027(6) C8 0.077(8) 0.075(10) 0.201(16) 0.076(10) 0.079(10) 0.026(7) C9 0.088(9) 0.066(9) 0.190(15) 0.071(9) 0.090(10) 0.051(7) C10 0.034(4) 0.090(8) 0.035(4) 0.016(5) 0.018(3) 0.019(5) C11 0.040(5) 0.118(10) 0.039(5) 0.030(6) 0.017(4) 0.023(6) C12 0.027(4) 0.130(10) 0.041(5) 0.009(6) 0.011(4) 0.011(5) C13 0.045(5) 0.082(8) 0.035(4) 0.002(4) 0.021(4) 0.019(5) C14 0.033(4) 0.093(8) 0.026(4) 0.008(4) 0.012(3) 0.015(5) N1 0.033(4) 0.113(8) 0.037(4) 0.015(4) 0.016(3) 0.012(4) N2 0.048(5) 0.097(8) 0.114(8) 0.057(6) 0.046(5) 0.024(5) N3 0.031(3) 0.091(6) 0.037(4) 0.002(4) 0.017(3) 0.008(4) Ag1 0.0336(3) 0.1260(8) 0.0449(4) -0.0120(4) 0.0153(3) 0.0073(4) F1 0.097(5) 0.089(5) 0.138(6) -0.041(5) 0.085(5) -0.005(4) F2 0.062(4) 0.119(6) 0.054(3) -0.006(4) 0.016(3) 0.011(4) F3 0.068(4) 0.095(5) 0.082(4) -0.042(4) 0.019(3) -0.007(4) F4 0.060(4) 0.247(10) 0.064(4) 0.028(5) 0.035(3) 0.053(5) F5 0.127(6) 0.165(8) 0.061(4) -0.026(5) 0.056(4) -0.021(6) F6 0.111(6) 0.177(9) 0.087(5) -0.033(5) 0.044(5) -0.092(6) Sb1 0.0328(3) 0.1083(6) 0.0456(3) -0.0291(4) 0.0218(3) -0.0132(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.320(10) . ? C1 C2 1.408(15) . ? C1 H1 0.9300 . ? C2 C3 1.363(14) . ? C2 H2 0.9300 . ? C3 C4 1.453(13) . ? C3 H3 0.9300 . ? C4 N1 1.389(14) . ? C4 C5 1.393(12) . ? C5 C6 1.416(15) . ? C5 C10 1.495(14) . ? C6 C7 1.383(15) . ? C6 N2 1.385(12) . ? C7 C8 1.340(17) . ? C7 H7 0.9300 . ? C8 C9 1.379(15) . ? C8 H8 0.9300 . ? C9 N2 1.375(16) . ? C9 H9 0.9300 . ? C10 C14 1.383(13) . ? C10 C11 1.393(11) . ? C11 C12 1.372(15) . ? C11 H11 0.9300 . ? C12 N3 1.345(13) . ? C12 H12 0.9300 . ? C13 N3 1.346(10) . ? C13 C14 1.375(13) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? N1 Ag1 2.127(9) . ? N2 H2A 0.8600 . ? N3 Ag1 2.131(8) 7_656 ? Ag1 N3 2.131(8) 7_656 ? F1 Sb1 1.875(6) . ? F2 Sb1 1.862(6) . ? F3 Sb1 1.869(6) . ? F4 Sb1 1.901(7) . ? F5 Sb1 1.887(7) . ? F6 Sb1 1.860(7) . ? 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 113.7(10) . . ? N1 C1 H1 123.2 . . ? C2 C1 H1 123.2 . . ? C3 C2 C1 105.9(9) . . ? C3 C2 H2 127.1 . . ? C1 C2 H2 127.1 . . ? C2 C3 C4 106.2(11) . . ? C2 C3 H3 126.9 . . ? C4 C3 H3 126.9 . . ? N1 C4 C5 124.5(10) . . ? N1 C4 C3 108.9(8) . . ? C5 C4 C3 126.6(11) . . ? C4 C5 C6 125.7(10) . . ? C4 C5 C10 118.6(10) . . ? C6 C5 C10 115.7(8) . . ? C7 C6 N2 105.9(10) . . ? C7 C6 C5 130.6(9) . . ? N2 C6 C5 123.4(9) . . ? C8 C7 C6 109.5(10) . . ? C8 C7 H7 125.2 . . ? C6 C7 H7 125.2 . . ? C7 C8 C9 108.7(12) . . ? C7 C8 H8 125.6 . . ? C9 C8 H8 125.6 . . ? N2 C9 C8 106.9(11) . . ? N2 C9 H9 126.5 . . ? C8 C9 H9 126.5 . . ? C14 C10 C11 116.4(9) . . ? C14 C10 C5 122.8(7) . . ? C11 C10 C5 120.8(9) . . ? C12 C11 C10 120.1(10) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? N3 C12 C11 124.1(8) . . ? N3 C12 H12 117.9 . . ? C11 C12 H12 117.9 . . ? N3 C13 C14 124.6(9) . . ? N3 C13 H13 117.7 . . ? C14 C13 H13 117.7 . . ? C13 C14 C10 119.8(8) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? C1 N1 C4 105.3(9) . . ? C1 N1 Ag1 125.3(8) . . ? C4 N1 Ag1 129.4(6) . . ? C9 N2 C6 108.8(9) . . ? C9 N2 H2A 125.6 . . ? C6 N2 H2A 125.6 . . ? C12 N3 C13 115.0(8) . . ? C12 N3 Ag1 118.6(6) . 7_656 ? C13 N3 Ag1 125.8(7) . 7_656 ? N1 Ag1 N3 170.8(3) . 7_656 ? F6 Sb1 F2 91.6(3) . . ? F6 Sb1 F3 177.2(4) . . ? F2 Sb1 F3 87.9(3) . . ? F6 Sb1 F1 89.4(4) . . ? F2 Sb1 F1 88.8(3) . . ? F3 Sb1 F1 87.8(3) . . ? F6 Sb1 F5 91.5(4) . . ? F2 Sb1 F5 176.9(3) . . ? F3 Sb1 F5 89.1(3) . . ? F1 Sb1 F5 91.6(3) . . ? F6 Sb1 F4 93.1(4) . . ? F2 Sb1 F4 90.6(3) . . ? F3 Sb1 F4 89.7(4) . . ? F1 Sb1 F4 177.4(4) . . ? F5 Sb1 F4 88.8(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.487 _refine_diff_density_min -2.135 _refine_diff_density_rms 0.127 #===END ###Material relevant to compound 8 at 173K ## data_8 _database_code_depnum_ccdc_archive 'CCDC 791549' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Ag2 N6 O2, 2(B F4)' _chemical_formula_sum 'C28 H26 Ag2 B2 F8 N6 O2' _chemical_formula_weight 867.91 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1379(2) _cell_length_b 9.5859(2) _cell_length_c 15.9091(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.4170(10) _cell_angle_gamma 90.00 _cell_volume 1503.86(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9879 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.43 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.392 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8508 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details sadabs _exptl_special_details ; No hydrogen atoms were introduced on the water molecule, although they are taken into account in the compound's formula. The BF4 anion is disordered over two positions, refined accordingly. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25736 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3415 _reflns_number_gt 3195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+2.1645P] 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 3415 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.003 _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 1.0131(2) 0.1949(3) 1.00935(15) 0.0273(5) Uani 1 1 d . . . H1 H 1.0393 0.2160 1.0679 0.033 Uiso 1 1 calc R . . C2 C 1.0938(2) 0.2244(3) 0.94850(16) 0.0285(5) Uani 1 1 d . . . H2 H 1.1784 0.2675 0.9600 0.034 Uiso 1 1 calc R . . C3 C 1.0226(2) 0.1772(3) 0.87084(16) 0.0261(5) Uani 1 1 d . . . H3 H 1.0493 0.1813 0.8188 0.031 Uiso 1 1 calc R . . C4 C 0.8972(2) 0.1194(2) 0.88410(14) 0.0230(4) Uani 1 1 d . . . C5 C 0.7882(2) 0.0634(2) 0.82547(15) 0.0225(4) Uani 1 1 d . . . C6 C 0.7818(2) 0.0329(2) 0.73678(15) 0.0234(5) Uani 1 1 d . . . C7 C 0.6658(2) 0.0075(3) 0.67148(16) 0.0284(5) Uani 1 1 d . . . H7 H 0.5774 0.0022 0.6785 0.034 Uiso 1 1 calc R . . C8 C 0.7062(3) -0.0084(3) 0.59355(16) 0.0325(6) Uani 1 1 d . . . H8 H 0.6499 -0.0254 0.5395 0.039 Uiso 1 1 calc R . . C9 C 0.8454(3) 0.0061(3) 0.61227(16) 0.0305(5) Uani 1 1 d . . . H9 H 0.8995 -0.0005 0.5725 0.037 Uiso 1 1 calc R . . C10 C 0.6590(2) 0.0329(2) 0.85247(14) 0.0230(5) Uani 1 1 d . . . C11 C 0.6178(3) -0.1019(3) 0.86334(17) 0.0310(5) Uani 1 1 d . . . H11 H 0.6708 -0.1772 0.8544 0.037 Uiso 1 1 calc R . . C12 C 0.4971(3) -0.1238(3) 0.88766(18) 0.0359(6) Uani 1 1 d . . . H12 H 0.4713 -0.2150 0.8957 0.043 Uiso 1 1 calc R . . C13 C 0.4542(3) 0.1099(3) 0.88699(17) 0.0335(6) Uani 1 1 d . . . H13 H 0.3972 0.1831 0.8935 0.040 Uiso 1 1 calc R . . C14 C 0.5745(2) 0.1410(3) 0.86413(17) 0.0315(5) Uani 1 1 d . . . H14 H 0.5982 0.2331 0.8567 0.038 Uiso 1 1 calc R . . N1 N 0.89756(19) 0.1345(2) 0.97253(12) 0.0238(4) Uani 1 1 d . . . N2 N 0.8904(2) 0.0313(2) 0.69754(13) 0.0276(4) Uani 1 1 d . . . H2A H 0.9738 0.0443 0.7236 0.033 Uiso 1 1 calc R . . N3 N 0.4159(2) -0.0197(3) 0.90011(13) 0.0308(5) Uani 1 1 d . . . Ag1 Ag 0.76069(2) 0.06290(3) 1.048007(13) 0.04132(9) Uani 1 1 d . . . O1 O 0.8892(3) 0.1631(3) 1.19724(16) 0.0673(7) Uani 1 1 d . . . B1 B 0.2663(4) 0.5147(5) 0.8495(2) 0.0523(10) Uani 1 1 d . . . F1 F 0.32436(19) 0.5939(2) 0.79458(15) 0.0590(5) Uani 1 1 d . A . F2 F 0.1620(6) 0.5737(5) 0.8790(4) 0.0665(16) Uani 0.587(8) 1 d P A 1 F3 F 0.3536(4) 0.4505(7) 0.9187(2) 0.0598(17) Uani 0.587(8) 1 d P A 1 F4 F 0.1979(5) 0.4035(6) 0.7994(2) 0.0724(19) Uani 0.587(8) 1 d P A 1 F2B F 0.1436(9) 0.5626(18) 0.8383(8) 0.163(8) Uani 0.413(8) 1 d P A 2 F3B F 0.3449(7) 0.5857(12) 0.9249(4) 0.093(4) Uani 0.413(8) 1 d P A 2 F4B F 0.2977(17) 0.3924(9) 0.8492(14) 0.203(11) Uani 0.413(8) 1 d P A 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 0.0227(11) 0.0334(13) 0.0261(11) -0.0039(10) 0.0060(9) -0.0051(10) C2 0.0226(11) 0.0310(13) 0.0332(12) -0.0024(10) 0.0094(9) -0.0065(9) C3 0.0231(11) 0.0284(12) 0.0298(12) 0.0011(10) 0.0122(9) -0.0031(9) C4 0.0212(10) 0.0244(11) 0.0245(11) 0.0007(9) 0.0076(8) -0.0012(9) C5 0.0194(10) 0.0222(11) 0.0273(11) 0.0029(9) 0.0085(9) -0.0001(8) C6 0.0210(11) 0.0253(12) 0.0252(11) 0.0005(9) 0.0080(9) -0.0015(9) C7 0.0229(11) 0.0329(13) 0.0288(12) -0.0004(10) 0.0051(9) -0.0004(10) C8 0.0357(13) 0.0344(14) 0.0252(12) -0.0004(10) 0.0023(10) 0.0009(11) C9 0.0365(13) 0.0311(13) 0.0266(12) 0.0002(10) 0.0126(10) 0.0014(11) C10 0.0191(10) 0.0282(12) 0.0221(10) -0.0001(9) 0.0055(8) -0.0040(9) C11 0.0310(13) 0.0259(13) 0.0401(14) -0.0050(10) 0.0160(11) -0.0047(10) C12 0.0367(14) 0.0353(14) 0.0395(14) -0.0065(12) 0.0165(11) -0.0149(12) C13 0.0268(12) 0.0399(15) 0.0363(14) 0.0060(11) 0.0122(10) 0.0058(11) C14 0.0284(12) 0.0289(13) 0.0404(14) 0.0072(11) 0.0146(10) 0.0016(10) N1 0.0219(9) 0.0268(10) 0.0241(9) -0.0017(8) 0.0084(7) -0.0027(8) N2 0.0214(9) 0.0347(12) 0.0281(10) -0.0025(8) 0.0090(8) -0.0005(8) N3 0.0200(9) 0.0482(14) 0.0251(10) -0.0007(9) 0.0068(8) -0.0075(9) Ag1 0.03109(12) 0.06721(17) 0.02948(12) -0.00845(10) 0.01484(8) -0.02208(10) O1 0.0593(15) 0.0799(19) 0.0555(15) -0.0160(13) -0.0015(12) 0.0146(14) B1 0.0372(18) 0.079(3) 0.0420(19) 0.0076(19) 0.0122(15) -0.0007(18) F1 0.0431(10) 0.0597(13) 0.0803(14) 0.0048(10) 0.0267(10) -0.0104(9) F2 0.056(3) 0.082(3) 0.076(4) 0.031(3) 0.045(3) 0.024(2) F3 0.0401(18) 0.100(5) 0.0372(18) 0.0091(19) 0.0045(14) 0.005(2) F4 0.076(3) 0.099(4) 0.045(2) -0.007(2) 0.020(2) -0.055(3) F2B 0.029(3) 0.36(2) 0.106(8) 0.121(10) 0.028(5) 0.008(6) F3B 0.078(4) 0.157(10) 0.044(3) 0.018(4) 0.013(3) -0.038(5) F4B 0.224(17) 0.049(5) 0.42(3) 0.089(10) 0.25(2) 0.058(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.316(3) . ? C1 C2 1.433(3) . ? C1 H1 0.9300 . ? C2 C3 1.356(3) . ? C2 H2 0.9300 . ? C3 C4 1.446(3) . ? C3 H3 0.9300 . ? C4 C5 1.379(3) . ? C4 N1 1.414(3) . ? C5 C6 1.428(3) . ? C5 C10 1.499(3) . ? C6 N2 1.385(3) . ? C6 C7 1.398(3) . ? C7 C8 1.401(4) . ? C7 H7 0.9300 . ? C8 C9 1.380(4) . ? C8 H8 0.9300 . ? C9 N2 1.349(3) . ? C9 H9 0.9300 . ? C10 C11 1.381(3) . ? C10 C14 1.384(3) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 N3 1.338(4) . ? C12 H12 0.9300 . ? C13 N3 1.333(4) . ? C13 C14 1.384(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? N1 Ag1 2.1475(19) . ? N2 H2A 0.8600 . ? N3 Ag1 2.178(2) 3_657 ? Ag1 N3 2.178(2) 3_657 ? B1 F4B 1.215(9) . ? B1 F2B 1.299(11) . ? B1 F2 1.374(6) . ? B1 F3 1.387(6) . ? B1 F1 1.388(4) . ? B1 F4 1.413(6) . ? B1 F3B 1.447(8) . ? 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 112.0(2) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 106.4(2) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.2(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 122.0(2) . . ? C5 C4 C3 130.1(2) . . ? N1 C4 C3 107.85(19) . . ? C4 C5 C6 126.4(2) . . ? C4 C5 C10 119.9(2) . . ? C6 C5 C10 113.6(2) . . ? N2 C6 C7 106.4(2) . . ? N2 C6 C5 126.1(2) . . ? C7 C6 C5 127.4(2) . . ? C6 C7 C8 107.9(2) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? C9 C8 C7 107.0(2) . . ? C9 C8 H8 126.5 . . ? C7 C8 H8 126.5 . . ? N2 C9 C8 109.0(2) . . ? N2 C9 H9 125.5 . . ? C8 C9 H9 125.5 . . ? C11 C10 C14 118.0(2) . . ? C11 C10 C5 121.9(2) . . ? C14 C10 C5 120.1(2) . . ? C10 C11 C12 119.4(2) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N3 C12 C11 122.9(3) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N3 C13 C14 123.2(3) . . ? N3 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C10 119.0(2) . . ? C13 C14 H14 120.5 . . ? C10 C14 H14 120.5 . . ? C1 N1 C4 106.51(19) . . ? C1 N1 Ag1 121.05(16) . . ? C4 N1 Ag1 132.15(15) . . ? C9 N2 C6 109.7(2) . . ? C9 N2 H2A 125.1 . . ? C6 N2 H2A 125.1 . . ? C13 N3 C12 117.4(2) . . ? C13 N3 Ag1 122.08(18) . 3_657 ? C12 N3 Ag1 120.20(18) . 3_657 ? N1 Ag1 N3 165.30(8) . 3_657 ? F4B B1 F2B 125.7(11) . . ? F4B B1 F2 128.4(6) . . ? F2B B1 F2 27.5(6) . . ? F4B B1 F3 57.0(10) . . ? F2B B1 F3 132.8(6) . . ? F2 B1 F3 108.1(4) . . ? F4B B1 F1 112.1(6) . . ? F2B B1 F1 104.7(6) . . ? F2 B1 F1 117.6(4) . . ? F3 B1 F1 117.2(3) . . ? F4B B1 F4 50.5(10) . . ? F2B B1 F4 82.0(8) . . ? F2 B1 F4 100.8(4) . . ? F3 B1 F4 104.6(4) . . ? F1 B1 F4 106.4(3) . . ? F4B B1 F3B 111.3(11) . . ? F2B B1 F3B 105.8(9) . . ? F2 B1 F3B 80.9(5) . . ? F3 B1 F3B 54.8(4) . . ? F1 B1 F3B 91.8(4) . . ? F4 B1 F3B 157.9(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.619 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.070 #===END ###Material relevant to compound 9 at 173K ## data_9 _database_code_depnum_ccdc_archive 'CCDC 791550' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Ag2 N6, 2(C F3 O3 S)' _chemical_formula_sum 'C42 H30 Ag2 F6 N6 O6 S2' _chemical_formula_weight 1108.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.8577(4) _cell_length_b 11.1300(4) _cell_length_c 11.5098(5) _cell_angle_alpha 118.0560(10) _cell_angle_beta 92.695(2) _cell_angle_gamma 107.9120(10) _cell_volume 1032.41(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4506 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.42 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8394 _exptl_absorpt_correction_T_max 0.9560 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12472 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4690 _reflns_number_gt 3991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.9682P] 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 4690 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _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 0.3091(3) 0.4136(3) 0.2081(3) 0.0240(6) Uani 1 1 d . . . H1 H 0.4062 0.4755 0.2294 0.029 Uiso 1 1 calc R . . C2 C 0.1906(3) 0.4170(3) 0.1352(3) 0.0255(6) Uani 1 1 d . . . H2A H 0.1967 0.4790 0.1012 0.031 Uiso 1 1 calc R . . C3 C 0.0675(3) 0.3123(3) 0.1252(3) 0.0233(6) Uani 1 1 d . . . H3 H -0.0275 0.2898 0.0842 0.028 Uiso 1 1 calc R . . C4 C 0.1118(3) 0.2421(3) 0.1904(3) 0.0199(5) Uani 1 1 d . . . C5 C 0.0272(3) 0.1216(3) 0.1959(3) 0.0196(5) Uani 1 1 d . . . C6 C -0.1296(3) 0.0710(3) 0.1685(3) 0.0212(6) Uani 1 1 d . . . C7 C -0.2320(3) -0.0706(3) 0.1127(3) 0.0240(6) Uani 1 1 d . . . H7 H -0.2119 -0.1543 0.0900 0.029 Uiso 1 1 calc R . . C8 C -0.3717(3) -0.0649(3) 0.0966(3) 0.0300(7) Uani 1 1 d . . . H8 H -0.4607 -0.1442 0.0593 0.036 Uiso 1 1 calc R . . C9 C -0.3525(3) 0.0798(3) 0.1463(3) 0.0302(7) Uani 1 1 d . . . H9 H -0.4269 0.1158 0.1506 0.036 Uiso 1 1 calc R . . C10 C 0.0935(3) 0.0354(3) 0.2289(3) 0.0189(5) Uani 1 1 d . . . C11 C 0.2093(3) -0.0003(3) 0.1752(3) 0.0219(6) Uani 1 1 d . . . H11 H 0.2434 0.0264 0.1135 0.026 Uiso 1 1 calc R . . C12 C 0.2735(3) -0.0748(3) 0.2128(3) 0.0213(6) Uani 1 1 d . . . H12 H 0.3494 -0.0988 0.1749 0.026 Uiso 1 1 calc R . . C13 C 0.2266(3) -0.1148(3) 0.3067(3) 0.0194(5) Uani 1 1 d . . . C14 C 0.1072(3) -0.0842(3) 0.3554(3) 0.0231(6) Uani 1 1 d . . . H14 H 0.0714 -0.1131 0.4153 0.028 Uiso 1 1 calc R . . C15 C 0.0410(3) -0.0120(3) 0.3168(3) 0.0227(6) Uani 1 1 d . . . H15 H -0.0396 0.0053 0.3495 0.027 Uiso 1 1 calc R . . C16 C 0.3062(3) -0.1779(3) 0.3605(3) 0.0206(5) Uani 1 1 d . . . C17 C 0.4517(3) -0.1599(3) 0.3550(3) 0.0235(6) Uani 1 1 d . . . H17 H 0.4981 -0.1158 0.3087 0.028 Uiso 1 1 calc R . . C18 C 0.5268(3) -0.2069(3) 0.4176(3) 0.0249(6) Uani 1 1 d . . . H18 H 0.6235 -0.1940 0.4117 0.030 Uiso 1 1 calc R . . C19 C 0.3261(3) -0.2930(3) 0.4892(3) 0.0262(6) Uani 1 1 d . . . H19 H 0.2823 -0.3393 0.5347 0.031 Uiso 1 1 calc R . . C20 C 0.2425(3) -0.2509(3) 0.4273(3) 0.0238(6) Uani 1 1 d . . . H20 H 0.1442 -0.2709 0.4298 0.029 Uiso 1 1 calc R . . N1 N 0.2647(2) 0.3124(2) 0.2419(2) 0.0216(5) Uani 1 1 d . . . N2 N -0.2072(3) 0.1610(3) 0.1879(2) 0.0260(5) Uani 1 1 d . . . H2 H -0.1689 0.2544 0.2214 0.031 Uiso 1 1 calc R . . N3 N 0.4675(3) -0.2706(2) 0.4870(2) 0.0241(5) Uani 1 1 d . . . Ag1 Ag 0.39694(2) 0.30506(2) 0.38864(2) 0.02859(8) Uani 1 1 d . . . C21 C 0.2314(4) 0.4761(4) 0.8273(3) 0.0404(8) Uani 1 1 d . . . O1 O 0.3625(3) 0.5333(3) 0.6621(3) 0.0558(7) Uani 1 1 d . . . O2 O 0.1155(3) 0.5250(2) 0.6583(2) 0.0406(5) Uani 1 1 d . . . O3 O 0.1616(3) 0.3005(2) 0.5701(2) 0.0492(7) Uani 1 1 d . . . F1 F 0.2839(3) 0.6154(2) 0.9241(2) 0.0717(7) Uani 1 1 d . . . F2 F 0.3194(3) 0.4147(3) 0.8462(3) 0.0780(8) Uani 1 1 d . . . F3 F 0.1018(3) 0.4149(3) 0.8451(2) 0.0641(7) Uani 1 1 d . . . S1 S 0.21572(8) 0.45562(8) 0.65993(8) 0.02813(17) 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 0.0239(15) 0.0191(13) 0.0230(14) 0.0087(12) 0.0033(11) 0.0044(11) C2 0.0314(16) 0.0239(14) 0.0242(15) 0.0137(12) 0.0069(12) 0.0117(12) C3 0.0238(15) 0.0241(14) 0.0233(14) 0.0118(12) 0.0033(11) 0.0114(12) C4 0.0191(13) 0.0223(13) 0.0196(13) 0.0104(11) 0.0048(11) 0.0101(11) C5 0.0187(13) 0.0238(13) 0.0165(13) 0.0092(11) 0.0053(10) 0.0099(11) C6 0.0217(14) 0.0263(14) 0.0222(14) 0.0144(12) 0.0078(11) 0.0135(12) C7 0.0232(15) 0.0264(14) 0.0226(14) 0.0132(12) 0.0067(11) 0.0082(12) C8 0.0178(14) 0.0396(17) 0.0290(16) 0.0169(14) 0.0068(12) 0.0072(13) C9 0.0193(15) 0.0428(18) 0.0333(17) 0.0206(15) 0.0084(12) 0.0152(13) C10 0.0181(13) 0.0184(12) 0.0192(13) 0.0090(11) 0.0023(10) 0.0067(10) C11 0.0211(14) 0.0254(14) 0.0212(14) 0.0132(12) 0.0076(11) 0.0086(11) C12 0.0186(13) 0.0249(14) 0.0236(14) 0.0131(12) 0.0072(11) 0.0106(11) C13 0.0188(13) 0.0158(12) 0.0208(14) 0.0082(11) 0.0019(11) 0.0054(10) C14 0.0246(15) 0.0260(14) 0.0237(14) 0.0165(12) 0.0076(12) 0.0090(12) C15 0.0219(14) 0.0256(14) 0.0238(14) 0.0133(12) 0.0087(11) 0.0111(12) C16 0.0237(14) 0.0169(12) 0.0187(13) 0.0076(11) 0.0011(11) 0.0077(11) C17 0.0223(14) 0.0243(14) 0.0250(14) 0.0133(12) 0.0055(11) 0.0090(12) C18 0.0205(14) 0.0241(14) 0.0283(15) 0.0117(13) 0.0040(12) 0.0090(12) C19 0.0278(16) 0.0263(14) 0.0267(15) 0.0157(13) 0.0049(12) 0.0095(12) C20 0.0194(14) 0.0254(14) 0.0286(15) 0.0155(13) 0.0047(11) 0.0082(11) N1 0.0189(12) 0.0240(11) 0.0219(12) 0.0122(10) 0.0031(9) 0.0074(10) N2 0.0237(13) 0.0280(12) 0.0317(14) 0.0169(11) 0.0081(10) 0.0132(10) N3 0.0235(12) 0.0242(12) 0.0247(12) 0.0121(11) 0.0018(10) 0.0104(10) Ag1 0.02507(13) 0.03352(13) 0.02987(14) 0.01857(11) 0.00046(9) 0.01116(10) C21 0.041(2) 0.0394(19) 0.0394(19) 0.0217(17) 0.0081(16) 0.0113(16) O1 0.0268(13) 0.0846(19) 0.085(2) 0.0669(17) 0.0203(13) 0.0166(13) O2 0.0359(13) 0.0398(13) 0.0477(14) 0.0188(12) 0.0075(11) 0.0223(11) O3 0.078(2) 0.0301(12) 0.0372(13) 0.0127(11) 0.0203(13) 0.0238(13) F1 0.0808(18) 0.0502(14) 0.0400(13) 0.0048(11) -0.0076(12) 0.0032(13) F2 0.101(2) 0.110(2) 0.0735(17) 0.0684(17) 0.0274(15) 0.0652(18) F3 0.0586(15) 0.0756(16) 0.0460(13) 0.0347(12) 0.0207(11) 0.0029(12) S1 0.0261(4) 0.0284(4) 0.0368(4) 0.0202(3) 0.0123(3) 0.0121(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.318(3) . ? C1 C2 1.426(4) . ? C1 H1 0.9300 . ? C2 C3 1.355(4) . ? C2 H2A 0.9300 . ? C3 C4 1.448(3) . ? C3 H3 0.9300 . ? C4 C5 1.376(3) . ? C4 N1 1.410(3) . ? C5 C6 1.434(4) . ? C5 C10 1.482(4) . ? C6 N2 1.384(3) . ? C6 C7 1.387(4) . ? C7 C8 1.406(4) . ? C7 H7 0.9300 . ? C8 C9 1.375(4) . ? C8 H8 0.9300 . ? C9 N2 1.353(4) . ? C9 H9 0.9300 . ? C10 C15 1.398(3) . ? C10 C11 1.399(4) . ? C11 C12 1.383(4) . ? C11 H11 0.9300 . ? C12 C13 1.398(3) . ? C12 H12 0.9300 . ? C13 C14 1.395(4) . ? C13 C16 1.481(4) . ? C14 C15 1.378(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.394(4) . ? C16 C20 1.402(4) . ? C17 C18 1.372(4) . ? C17 H17 0.9300 . ? C18 N3 1.343(3) . ? C18 H18 0.9300 . ? C19 N3 1.342(4) . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N1 Ag1 2.132(2) . ? N2 H2 0.8600 . ? N3 Ag1 2.153(2) 2_656 ? Ag1 N3 2.153(2) 2_656 ? C21 F1 1.319(4) . ? C21 F2 1.324(4) . ? C21 F3 1.326(4) . ? C21 S1 1.824(3) . ? O1 S1 1.431(2) . ? O2 S1 1.433(2) . ? O3 S1 1.427(2) . ? 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 112.0(2) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 106.6(2) . . ? C3 C2 H2A 126.7 . . ? C1 C2 H2A 126.7 . . ? C2 C3 C4 107.0(2) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 123.7(2) . . ? C5 C4 C3 128.3(2) . . ? N1 C4 C3 107.8(2) . . ? C4 C5 C6 122.2(2) . . ? C4 C5 C10 121.6(2) . . ? C6 C5 C10 116.1(2) . . ? N2 C6 C7 106.7(2) . . ? N2 C6 C5 123.8(2) . . ? C7 C6 C5 129.4(3) . . ? C6 C7 C8 107.7(3) . . ? C6 C7 H7 126.1 . . ? C8 C7 H7 126.1 . . ? C9 C8 C7 107.3(3) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? N2 C9 C8 108.5(3) . . ? N2 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? C15 C10 C11 118.0(2) . . ? C15 C10 C5 120.0(2) . . ? C11 C10 C5 122.0(2) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 121.3(2) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 117.5(2) . . ? C14 C13 C16 120.7(2) . . ? C12 C13 C16 121.6(2) . . ? C15 C14 C13 121.5(2) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 C20 116.3(2) . . ? C17 C16 C13 121.8(2) . . ? C20 C16 C13 121.8(2) . . ? C18 C17 C16 120.4(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? N3 C18 C17 123.2(3) . . ? N3 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? N3 C19 C20 123.3(3) . . ? N3 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C16 119.7(3) . . ? C19 C20 H20 120.1 . . ? C16 C20 H20 120.1 . . ? C1 N1 C4 106.5(2) . . ? C1 N1 Ag1 123.23(19) . . ? C4 N1 Ag1 128.46(16) . . ? C9 N2 C6 109.7(2) . . ? C9 N2 H2 125.1 . . ? C6 N2 H2 125.1 . . ? C19 N3 C18 117.0(2) . . ? C19 N3 Ag1 121.92(18) . 2_656 ? C18 N3 Ag1 120.48(19) . 2_656 ? N1 Ag1 N3 171.89(8) . 2_656 ? F1 C21 F2 107.5(3) . . ? F1 C21 F3 106.7(3) . . ? F2 C21 F3 108.1(3) . . ? F1 C21 S1 111.7(2) . . ? F2 C21 S1 111.5(2) . . ? F3 C21 S1 111.2(2) . . ? O3 S1 O1 115.17(17) . . ? O3 S1 O2 115.28(16) . . ? O1 S1 O2 114.22(15) . . ? O3 S1 C21 103.71(15) . . ? O1 S1 C21 103.10(16) . . ? O2 S1 C21 103.02(16) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.995 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.088 #===END ###Material relevant to compound 10 at 173K ## data_10 _database_code_depnum_ccdc_archive 'CCDC 791551' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Ag2 N6, 2(F6 P)' _chemical_formula_sum 'C40 H30 Ag2 F12 N6 P2' _chemical_formula_weight 1100.38 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3668(3) _cell_length_b 13.6996(4) _cell_length_c 13.8058(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.6260(10) _cell_angle_gamma 90.00 _cell_volume 1951.27(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7234 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.10 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8808 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22705 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4497 _reflns_number_gt 3647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+3.6182P] 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 4497 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _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 0.3227(4) 0.6344(3) 0.5584(3) 0.0377(8) Uani 1 1 d . . . H1 H 0.3475 0.6952 0.5838 0.045 Uiso 1 1 calc R . . C2 C 0.3705(4) 0.5934(3) 0.4737(3) 0.0384(8) Uani 1 1 d . . . H2 H 0.4305 0.6212 0.4361 0.046 Uiso 1 1 calc R . . C3 C 0.3112(3) 0.5062(3) 0.4593(2) 0.0324(7) Uani 1 1 d . . . H3 H 0.3223 0.4625 0.4092 0.039 Uiso 1 1 calc R . . C4 C 0.2272(3) 0.4931(2) 0.5359(2) 0.0274(7) Uani 1 1 d . . . C5 C 0.1474(3) 0.4166(2) 0.5540(2) 0.0264(6) Uani 1 1 d . . . C6 C 0.1074(3) 0.3437(2) 0.4825(2) 0.0286(7) Uani 1 1 d . . . C7 C 0.1154(4) 0.3377(3) 0.3820(2) 0.0332(7) Uani 1 1 d . . . H7 H 0.1495 0.3849 0.3433 0.040 Uiso 1 1 calc R . . C8 C 0.0630(4) 0.2478(3) 0.3502(3) 0.0372(8) Uani 1 1 d . . . H8 H 0.0571 0.2241 0.2868 0.045 Uiso 1 1 calc R . . C9 C 0.0216(4) 0.2009(3) 0.4296(3) 0.0375(8) Uani 1 1 d . . . H9 H -0.0180 0.1400 0.4291 0.045 Uiso 1 1 calc R . . C10 C 0.1044(3) 0.4042(2) 0.6527(2) 0.0265(7) Uani 1 1 d . . . C11 C 0.1972(3) 0.3985(3) 0.7334(2) 0.0326(7) Uani 1 1 d . . . H11 H 0.2849 0.4026 0.7247 0.039 Uiso 1 1 calc R . . C12 C 0.1592(3) 0.3868(3) 0.8263(2) 0.0317(7) Uani 1 1 d . . . H12 H 0.2221 0.3830 0.8790 0.038 Uiso 1 1 calc R . . C13 C 0.0285(3) 0.3807(2) 0.8425(2) 0.0246(6) Uani 1 1 d . . . C14 C -0.0632(3) 0.3848(2) 0.7612(2) 0.0284(7) Uani 1 1 d . . . H14 H -0.1508 0.3802 0.7699 0.034 Uiso 1 1 calc R . . C15 C -0.0261(3) 0.3956(2) 0.6687(2) 0.0288(7) Uani 1 1 d . . . H15 H -0.0891 0.3971 0.6159 0.035 Uiso 1 1 calc R . . C16 C -0.0123(3) 0.3734(2) 0.9423(2) 0.0257(6) Uani 1 1 d . . . C17 C 0.0762(4) 0.3651(3) 1.0237(2) 0.0362(8) Uani 1 1 d . . . H17 H 0.1643 0.3616 1.0164 0.043 Uiso 1 1 calc R . . C18 C 0.0349(4) 0.3619(3) 1.1156(3) 0.0395(8) Uani 1 1 d . . . H18 H 0.0971 0.3554 1.1686 0.047 Uiso 1 1 calc R . . C19 C -0.1746(4) 0.3769(4) 1.0548(3) 0.0502(11) Uani 1 1 d . . . H19 H -0.2618 0.3821 1.0646 0.060 Uiso 1 1 calc R . . C20 C -0.1410(4) 0.3794(4) 0.9609(3) 0.0476(11) Uani 1 1 d . . . H20 H -0.2054 0.3851 0.9093 0.057 Uiso 1 1 calc R . . N1 N 0.2401(3) 0.5769(2) 0.5963(2) 0.0307(6) Uani 1 1 d . . . N2 N 0.0481(3) 0.2582(2) 0.5082(2) 0.0335(6) Uani 1 1 d . . . H2A H 0.0307 0.2438 0.5662 0.040 Uiso 1 1 calc R . . N3 N -0.0883(3) 0.3675(2) 1.1328(2) 0.0321(6) Uani 1 1 d . . . Ag1 Ag 0.14938(3) 0.61087(2) 0.723779(19) 0.03695(11) Uani 1 1 d . . . F1 F 0.4349(2) 0.6417(2) 0.8095(2) 0.0673(8) Uani 1 1 d . . . F2 F 0.5587(5) 0.5341(3) 0.9042(3) 0.1190(17) Uani 1 1 d . . . F3 F 0.6398(3) 0.6731(2) 0.8602(2) 0.0691(8) Uani 1 1 d . . . F4 F 0.7026(3) 0.5318(2) 0.7934(2) 0.0763(9) Uani 1 1 d . . . F5 F 0.5807(4) 0.6385(2) 0.7043(2) 0.0800(10) Uani 1 1 d . . . F6 F 0.4972(3) 0.4976(2) 0.7441(3) 0.0887(12) Uani 1 1 d . . . P1 P 0.56645(10) 0.58269(8) 0.80336(7) 0.0376(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(2) 0.0338(18) 0.036(2) -0.0040(15) 0.0107(16) -0.0086(15) C2 0.040(2) 0.045(2) 0.0322(19) 0.0013(15) 0.0143(16) -0.0054(16) C3 0.0338(18) 0.0397(19) 0.0250(16) -0.0018(14) 0.0096(14) -0.0001(14) C4 0.0289(16) 0.0343(17) 0.0194(14) 0.0001(12) 0.0046(12) 0.0024(13) C5 0.0294(16) 0.0312(16) 0.0188(14) 0.0019(12) 0.0037(12) 0.0031(13) C6 0.0328(17) 0.0310(16) 0.0225(15) 0.0010(13) 0.0053(13) -0.0004(13) C7 0.0393(19) 0.0383(19) 0.0223(16) 0.0036(14) 0.0051(14) -0.0001(15) C8 0.043(2) 0.043(2) 0.0255(17) -0.0062(14) 0.0024(15) 0.0026(16) C9 0.044(2) 0.0323(18) 0.0356(19) -0.0036(15) 0.0026(16) -0.0039(15) C10 0.0329(17) 0.0270(16) 0.0202(15) 0.0005(12) 0.0056(12) -0.0011(12) C11 0.0257(16) 0.047(2) 0.0250(17) 0.0044(14) 0.0043(12) -0.0026(14) C12 0.0274(16) 0.046(2) 0.0213(16) 0.0057(14) -0.0001(12) -0.0043(14) C13 0.0295(16) 0.0239(14) 0.0209(15) 0.0008(11) 0.0048(12) -0.0003(12) C14 0.0264(16) 0.0349(17) 0.0241(16) -0.0014(13) 0.0042(12) 0.0007(13) C15 0.0278(16) 0.0367(17) 0.0212(15) -0.0018(13) -0.0003(12) 0.0023(13) C16 0.0322(17) 0.0243(15) 0.0210(15) -0.0005(11) 0.0056(12) -0.0019(12) C17 0.0288(18) 0.057(2) 0.0229(17) 0.0005(15) 0.0037(13) 0.0074(16) C18 0.040(2) 0.057(2) 0.0217(17) 0.0009(15) 0.0011(14) 0.0072(17) C19 0.032(2) 0.089(3) 0.030(2) -0.004(2) 0.0100(16) -0.014(2) C20 0.0309(19) 0.089(3) 0.0229(18) -0.0017(19) 0.0024(14) -0.014(2) N1 0.0348(15) 0.0353(15) 0.0226(14) -0.0026(12) 0.0066(11) -0.0034(12) N2 0.0433(17) 0.0348(15) 0.0229(14) 0.0023(11) 0.0064(12) -0.0060(13) N3 0.0395(16) 0.0370(16) 0.0207(13) -0.0026(11) 0.0073(12) -0.0062(12) Ag1 0.04619(19) 0.04300(18) 0.02369(15) -0.00748(11) 0.01365(11) -0.00696(12) F1 0.0371(13) 0.091(2) 0.0746(19) -0.0380(16) 0.0080(12) 0.0123(13) F2 0.228(5) 0.076(2) 0.064(2) 0.0248(18) 0.068(3) 0.024(3) F3 0.0554(17) 0.0666(18) 0.082(2) -0.0273(16) -0.0121(14) 0.0136(14) F4 0.0643(18) 0.084(2) 0.078(2) -0.0230(17) -0.0079(15) 0.0409(16) F5 0.113(3) 0.078(2) 0.0551(18) 0.0080(15) 0.0408(18) 0.033(2) F6 0.0625(19) 0.080(2) 0.125(3) -0.058(2) 0.0203(19) -0.0184(16) P1 0.0375(5) 0.0452(5) 0.0309(5) -0.0047(4) 0.0081(4) 0.0082(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.309(5) . ? C1 C2 1.430(5) . ? C1 H1 0.9300 . ? C2 C3 1.350(5) . ? C2 H2 0.9300 . ? C3 C4 1.447(4) . ? C3 H3 0.9300 . ? C4 C5 1.373(5) . ? C4 N1 1.418(4) . ? C5 C6 1.436(5) . ? C5 C10 1.485(4) . ? C6 N2 1.384(4) . ? C6 C7 1.401(4) . ? C7 C8 1.399(5) . ? C7 H7 0.9300 . ? C8 C9 1.374(5) . ? C8 H8 0.9300 . ? C9 N2 1.346(5) . ? C9 H9 0.9300 . ? C10 C15 1.397(5) . ? C10 C11 1.401(5) . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 C13 1.397(5) . ? C12 H12 0.9300 . ? C13 C14 1.398(5) . ? C13 C16 1.484(4) . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.384(5) . ? C16 C20 1.386(5) . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 N3 1.324(5) . ? C18 H18 0.9300 . ? C19 N3 1.337(5) . ? C19 C20 1.376(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N1 Ag1 2.127(3) . ? N2 H2A 0.8600 . ? N3 Ag1 2.157(3) 3_567 ? Ag1 N3 2.157(3) 3_567 ? F1 P1 1.594(3) . ? F2 P1 1.553(3) . ? F3 P1 1.616(3) . ? F4 P1 1.592(3) . ? F5 P1 1.586(3) . ? F6 P1 1.558(3) . ? 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 112.5(3) . . ? N1 C1 H1 123.7 . . ? C2 C1 H1 123.7 . . ? C3 C2 C1 106.2(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 107.5(3) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? C5 C4 N1 122.4(3) . . ? C5 C4 C3 130.1(3) . . ? N1 C4 C3 107.5(3) . . ? C4 C5 C6 123.0(3) . . ? C4 C5 C10 119.6(3) . . ? C6 C5 C10 117.3(3) . . ? N2 C6 C7 106.0(3) . . ? N2 C6 C5 121.2(3) . . ? C7 C6 C5 132.9(3) . . ? C8 C7 C6 107.6(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C9 C8 C7 107.7(3) . . ? C9 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? N2 C9 C8 108.4(3) . . ? N2 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? C15 C10 C11 118.1(3) . . ? C15 C10 C5 122.5(3) . . ? C11 C10 C5 119.4(3) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 121.6(3) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 117.6(3) . . ? C12 C13 C16 121.5(3) . . ? C14 C13 C16 121.0(3) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 121.1(3) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? C17 C16 C20 115.4(3) . . ? C17 C16 C13 122.2(3) . . ? C20 C16 C13 122.3(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? N3 C18 C17 123.7(3) . . ? N3 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N3 C19 C20 123.4(4) . . ? N3 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C16 120.6(4) . . ? C19 C20 H20 119.7 . . ? C16 C20 H20 119.7 . . ? C1 N1 C4 106.3(3) . . ? C1 N1 Ag1 123.9(2) . . ? C4 N1 Ag1 129.7(2) . . ? C9 N2 C6 110.3(3) . . ? C9 N2 H2A 124.9 . . ? C6 N2 H2A 124.9 . . ? C18 N3 C19 116.2(3) . . ? C18 N3 Ag1 123.2(2) . 3_567 ? C19 N3 Ag1 119.5(3) . 3_567 ? N1 Ag1 N3 169.37(11) . 3_567 ? F2 P1 F6 95.1(2) . . ? F2 P1 F5 175.8(3) . . ? F6 P1 F5 89.1(2) . . ? F2 P1 F4 90.8(2) . . ? F6 P1 F4 89.67(18) . . ? F5 P1 F4 88.76(19) . . ? F2 P1 F1 92.9(2) . . ? F6 P1 F1 93.12(17) . . ? F5 P1 F1 87.34(18) . . ? F4 P1 F1 175.2(2) . . ? F2 P1 F3 87.5(2) . . ? F6 P1 F3 177.4(2) . . ? F5 P1 F3 88.3(2) . . ? F4 P1 F3 89.92(17) . . ? F1 P1 F3 87.12(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.267 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.100 #===END ###Material relevant to compound alpha11 at 173K ## data_alpha11 _database_code_depnum_ccdc_archive 'CCDC 791552' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Ag2 N6, 2(C2 H3 N), 2(B F4)' _chemical_formula_sum 'C44 H36 Ag2 B2 F8 N8' _chemical_formula_weight 1066.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 '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 9.3120(3) _cell_length_b 10.4615(3) _cell_length_c 12.4452(4) _cell_angle_alpha 112.286(2) _cell_angle_beta 94.953(2) _cell_angle_gamma 101.894(2) _cell_volume 1079.46(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8463 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.51 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9166 _exptl_absorpt_correction_T_max 0.9617 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16820 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4916 _reflns_number_gt 4506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.9944P] 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 4916 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _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 -0.0645(4) 0.1425(4) -0.0650(3) 0.0348(7) Uani 1 1 d . . . H1 H 0.0009 0.1729 -0.1081 0.042 Uiso 1 1 calc R . . C2 C -0.2185(4) 0.0725(4) -0.1100(3) 0.0374(8) Uani 1 1 d . . . H2A H -0.2708 0.0513 -0.1843 0.045 Uiso 1 1 calc R . . C3 C -0.2739(4) 0.0428(4) -0.0214(3) 0.0336(7) Uani 1 1 d . . . H3 H -0.3717 -0.0038 -0.0245 0.040 Uiso 1 1 calc R . . C4 C -0.1532(4) 0.0969(3) 0.0774(3) 0.0283(6) Uani 1 1 d . . . C5 C -0.1529(4) 0.0937(3) 0.1880(3) 0.0276(6) Uani 1 1 d . . . C6 C -0.2689(4) 0.0018(4) 0.2113(3) 0.0306(7) Uani 1 1 d . . . C7 C -0.3780(4) -0.1234(4) 0.1371(4) 0.0385(8) Uani 1 1 d . . . H7 H -0.3897 -0.1681 0.0554 0.046 Uiso 1 1 calc R . . C8 C -0.4652(5) -0.1689(5) 0.2069(4) 0.0491(10) Uani 1 1 d . . . H8 H -0.5461 -0.2489 0.1806 0.059 Uiso 1 1 calc R . . C9 C -0.4103(5) -0.0740(4) 0.3221(4) 0.0444(9) Uani 1 1 d . . . H9 H -0.4488 -0.0789 0.3874 0.053 Uiso 1 1 calc R . . C10 C -0.0287(4) 0.1890(3) 0.2874(3) 0.0257(6) Uani 1 1 d . . . C11 C 0.0111(4) 0.3366(3) 0.3186(3) 0.0299(7) Uani 1 1 d . . . H11 H -0.0392 0.3746 0.2752 0.036 Uiso 1 1 calc R . . C12 C 0.1237(4) 0.4266(3) 0.4127(3) 0.0321(7) Uani 1 1 d . . . H12 H 0.1463 0.5247 0.4334 0.038 Uiso 1 1 calc R . . C13 C 0.2045(4) 0.3718(3) 0.4774(3) 0.0263(6) Uani 1 1 d . . . C14 C 0.0497(4) 0.1343(4) 0.3534(3) 0.0318(7) Uani 1 1 d . . . H14 H 0.0240 0.0367 0.3350 0.038 Uiso 1 1 calc R . . C15 C 0.1652(4) 0.2246(4) 0.4460(3) 0.0315(7) Uani 1 1 d . . . H15 H 0.2175 0.1863 0.4880 0.038 Uiso 1 1 calc R . . C16 C 0.6695(4) 0.5320(4) 0.4256(3) 0.0379(6) Uani 1 1 d . . . C17 C 0.6316(4) 0.3859(4) 0.3869(3) 0.0379(6) Uani 1 1 d . . . H17 H 0.6902 0.3430 0.4195 0.046 Uiso 1 1 calc R . . C18 C 0.5084(5) 0.3016(4) 0.3005(4) 0.0489(10) Uani 1 1 d . . . H18 H 0.4869 0.2032 0.2777 0.059 Uiso 1 1 calc R . . C19 C 0.4530(7) 0.4926(5) 0.2860(6) 0.082(2) Uani 1 1 d . . . H19 H 0.3917 0.5321 0.2518 0.098 Uiso 1 1 calc R . . C20 C 0.5736(7) 0.5846(5) 0.3729(5) 0.080(2) Uani 1 1 d . . . H20 H 0.5903 0.6828 0.3960 0.096 Uiso 1 1 calc R . . N1 N -0.0251(3) 0.1593(3) 0.0454(2) 0.0290(6) Uani 1 1 d . . . N2 N -0.2923(3) 0.0268(3) 0.3256(3) 0.0350(6) Uani 1 1 d . . . H2 H -0.2393 0.0961 0.3887 0.042 Uiso 1 1 calc R . . N3 N 0.4197(3) 0.3518(3) 0.2486(3) 0.0360(7) Uani 1 1 d . . . Ag1 Ag 0.20107(3) 0.23978(3) 0.13908(2) 0.03690(10) Uani 1 1 d . . . B1 B 0.1652(7) 0.7841(5) 0.3533(5) 0.0492(12) Uani 1 1 d . . . F1 F 0.1558(4) 0.7545(3) 0.4519(2) 0.0686(8) Uani 1 1 d . . . F2 F 0.2069(6) 0.6846(4) 0.2658(4) 0.1089(15) Uani 1 1 d . . . F3 F 0.0197(4) 0.7866(4) 0.3112(4) 0.0964(12) Uani 1 1 d . . . F4 F 0.2559(4) 0.9210(3) 0.3862(3) 0.0678(8) Uani 1 1 d . . . C21 C 0.1900(13) 0.5306(8) 0.8879(8) 0.146(4) Uani 1 1 d . . . H21A H 0.1859 0.4665 0.8077 0.218 Uiso 1 1 calc R . . H21B H 0.2597 0.6204 0.9054 0.218 Uiso 1 1 calc R . . H21C H 0.0929 0.5455 0.8982 0.218 Uiso 1 1 calc R . . C22 C 0.2370(6) 0.4697(5) 0.9661(4) 0.0556(11) Uani 1 1 d . . . N4 N 0.2673(8) 0.4189(6) 1.0225(5) 0.0928(18) 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 0.0367(19) 0.0388(18) 0.0280(16) 0.0148(14) 0.0021(14) 0.0073(15) C2 0.038(2) 0.0429(19) 0.0277(17) 0.0135(15) -0.0053(14) 0.0089(15) C3 0.0272(17) 0.0364(18) 0.0333(18) 0.0133(14) -0.0047(14) 0.0058(13) C4 0.0254(16) 0.0297(15) 0.0279(16) 0.0110(13) -0.0009(13) 0.0069(12) C5 0.0250(15) 0.0259(15) 0.0299(16) 0.0098(13) -0.0006(13) 0.0081(12) C6 0.0277(16) 0.0306(16) 0.0342(17) 0.0148(14) 0.0011(13) 0.0078(13) C7 0.0337(19) 0.0366(18) 0.040(2) 0.0161(16) -0.0033(15) 0.0021(15) C8 0.036(2) 0.046(2) 0.063(3) 0.029(2) 0.0002(19) -0.0030(17) C9 0.040(2) 0.050(2) 0.055(2) 0.034(2) 0.0158(18) 0.0118(17) C10 0.0248(15) 0.0280(15) 0.0237(14) 0.0101(12) 0.0015(12) 0.0076(12) C11 0.0322(17) 0.0298(16) 0.0306(16) 0.0155(13) -0.0009(13) 0.0107(13) C12 0.0378(19) 0.0245(15) 0.0299(16) 0.0104(13) -0.0035(14) 0.0052(13) C13 0.0265(15) 0.0264(15) 0.0241(15) 0.0096(12) 0.0007(12) 0.0062(12) C14 0.0356(18) 0.0255(15) 0.0330(17) 0.0132(13) -0.0015(14) 0.0059(13) C15 0.0329(17) 0.0297(16) 0.0324(17) 0.0151(14) -0.0046(14) 0.0083(13) C16 0.0368(14) 0.0297(12) 0.0403(14) 0.0119(11) -0.0101(11) 0.0059(10) C17 0.0368(14) 0.0297(12) 0.0403(14) 0.0119(11) -0.0101(11) 0.0059(10) C18 0.048(2) 0.0277(18) 0.056(3) 0.0100(17) -0.017(2) 0.0042(16) C19 0.085(4) 0.042(2) 0.096(4) 0.035(3) -0.062(3) -0.010(2) C20 0.085(4) 0.037(2) 0.094(4) 0.033(3) -0.058(3) -0.012(2) N1 0.0259(14) 0.0313(14) 0.0278(14) 0.0120(11) -0.0010(11) 0.0054(11) N2 0.0367(16) 0.0356(15) 0.0346(15) 0.0167(13) 0.0060(13) 0.0087(12) N3 0.0299(15) 0.0343(15) 0.0361(16) 0.0125(13) -0.0060(12) 0.0008(12) Ag1 0.02551(15) 0.04475(17) 0.03172(15) 0.01198(12) -0.00302(10) 0.00129(11) B1 0.070(3) 0.042(2) 0.045(3) 0.024(2) 0.020(2) 0.019(2) F1 0.115(3) 0.0445(14) 0.0447(14) 0.0228(12) 0.0100(15) 0.0109(15) F2 0.168(4) 0.078(2) 0.094(3) 0.026(2) 0.076(3) 0.055(3) F3 0.088(3) 0.089(3) 0.111(3) 0.049(2) -0.013(2) 0.017(2) F4 0.080(2) 0.0519(16) 0.084(2) 0.0396(16) 0.0241(17) 0.0172(14) C21 0.241(12) 0.072(5) 0.112(7) 0.049(5) -0.047(7) 0.028(6) C22 0.075(3) 0.040(2) 0.048(2) 0.019(2) 0.003(2) 0.009(2) N4 0.143(6) 0.073(3) 0.061(3) 0.037(3) -0.006(3) 0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.326(4) . ? C1 C2 1.422(5) . ? C1 H1 0.9300 . ? C2 C3 1.368(5) . ? C2 H2A 0.9300 . ? C3 C4 1.438(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(5) . ? C4 N1 1.401(4) . ? C5 C6 1.419(5) . ? C5 C10 1.484(4) . ? C6 N2 1.391(5) . ? C6 C7 1.404(5) . ? C7 C8 1.384(6) . ? C7 H7 0.9300 . ? C8 C9 1.374(6) . ? C8 H8 0.9300 . ? C9 N2 1.342(5) . ? C9 H9 0.9300 . ? C10 C11 1.399(4) . ? C10 C14 1.400(4) . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C12 C13 1.402(4) . ? C12 H12 0.9300 . ? C13 C15 1.395(4) . ? C13 C16 1.481(5) 2_666 ? C14 C15 1.385(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.372(5) . ? C16 C20 1.380(6) . ? C16 C13 1.481(5) 2_666 ? C17 C18 1.379(5) . ? C17 H17 0.9300 . ? C18 N3 1.312(5) . ? C18 H18 0.9300 . ? C19 N3 1.323(5) . ? C19 C20 1.383(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N1 Ag1 2.146(3) . ? N2 H2 0.8600 . ? N3 Ag1 2.168(3) . ? B1 F2 1.342(6) . ? B1 F1 1.379(5) . ? B1 F4 1.389(6) . ? B1 F3 1.419(7) . ? C21 C22 1.434(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.080(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.1(3) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 105.9(3) . . ? C3 C2 H2A 127.0 . . ? C1 C2 H2A 127.0 . . ? C2 C3 C4 107.4(3) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? C5 C4 N1 122.5(3) . . ? C5 C4 C3 129.5(3) . . ? N1 C4 C3 108.1(3) . . ? C4 C5 C6 122.3(3) . . ? C4 C5 C10 120.2(3) . . ? C6 C5 C10 117.5(3) . . ? N2 C6 C7 105.8(3) . . ? N2 C6 C5 121.8(3) . . ? C7 C6 C5 132.4(3) . . ? C8 C7 C6 108.1(4) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C9 C8 C7 107.4(3) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? N2 C9 C8 109.2(4) . . ? N2 C9 H9 125.4 . . ? C8 C9 H9 125.4 . . ? C11 C10 C14 118.3(3) . . ? C11 C10 C5 120.5(3) . . ? C14 C10 C5 121.1(3) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C15 C13 C12 118.2(3) . . ? C15 C13 C16 121.2(3) . 2_666 ? C12 C13 C16 120.6(3) . 2_666 ? C15 C14 C10 120.5(3) . . ? C15 C14 H14 119.8 . . ? C10 C14 H14 119.8 . . ? C14 C15 C13 121.1(3) . . ? C14 C15 H15 119.4 . . ? C13 C15 H15 119.4 . . ? C17 C16 C20 114.6(4) . . ? C17 C16 C13 123.5(3) . 2_666 ? C20 C16 C13 121.8(3) . 2_666 ? C16 C17 C18 121.2(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? N3 C18 C17 124.0(4) . . ? N3 C18 H18 118.0 . . ? C17 C18 H18 118.0 . . ? N3 C19 C20 123.8(4) . . ? N3 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C16 C20 C19 120.6(4) . . ? C16 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C1 N1 C4 106.6(3) . . ? C1 N1 Ag1 123.7(2) . . ? C4 N1 Ag1 129.1(2) . . ? C9 N2 C6 109.4(3) . . ? C9 N2 H2 125.3 . . ? C6 N2 H2 125.3 . . ? C18 N3 C19 115.7(3) . . ? C18 N3 Ag1 127.8(3) . . ? C19 N3 Ag1 115.0(3) . . ? N1 Ag1 N3 170.97(11) . . ? F2 B1 F1 113.4(4) . . ? F2 B1 F4 112.8(4) . . ? F1 B1 F4 109.5(4) . . ? F2 B1 F3 107.8(5) . . ? F1 B1 F3 106.4(4) . . ? F4 B1 F3 106.5(4) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C21 176.9(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.137 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.093 #===END ###Material relevant to compound beta11 at 173K ## data_beta11 _database_code_depnum_ccdc_archive 'CCDC 791553' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Ag2 N6, 2(C2 H3 N), 2(B F4) ' _chemical_formula_sum 'C44 H36 Ag2 B2 F8 N8' _chemical_formula_weight 1066.17 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5431(4) _cell_length_b 7.2584(3) _cell_length_c 27.3348(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.822(2) _cell_angle_gamma 90.00 _cell_volume 2087.17(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4973 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.32 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8875 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15348 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4798 _reflns_number_gt 3669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2.3299P] 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 4798 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.6638(3) 0.9494(4) 0.27219(11) 0.0305(7) Uani 1 1 d . . . H1 H 0.7136 1.0553 0.2729 0.037 Uiso 1 1 calc R . . C2 C 0.6304(3) 0.8523(5) 0.31488(11) 0.0332(7) Uani 1 1 d . . . H2 H 0.6530 0.8837 0.3473 0.040 Uiso 1 1 calc R . . C3 C 0.5595(3) 0.7061(4) 0.29928(11) 0.0275(6) Uani 1 1 d . . . H3 H 0.5243 0.6176 0.3189 0.033 Uiso 1 1 calc R . . C4 C 0.5488(3) 0.7130(4) 0.24626(10) 0.0232(6) Uani 1 1 d . . . C5 C 0.4864(3) 0.5958(4) 0.21333(10) 0.0237(6) Uani 1 1 d . . . C6 C 0.4341(3) 0.4215(4) 0.22624(11) 0.0252(6) Uani 1 1 d . . . C7 C 0.4561(3) 0.3150(4) 0.26825(11) 0.0292(7) Uani 1 1 d . . . H7 H 0.5120 0.3429 0.2950 0.035 Uiso 1 1 calc R . . C8 C 0.3796(4) 0.1597(5) 0.26306(14) 0.0432(9) Uani 1 1 d . . . H8 H 0.3752 0.0646 0.2857 0.052 Uiso 1 1 calc R . . C9 C 0.3115(3) 0.1714(5) 0.21857(15) 0.0428(9) Uani 1 1 d . . . H9 H 0.2519 0.0860 0.2062 0.051 Uiso 1 1 calc R . . C10 C 0.4718(3) 0.6431(4) 0.15993(10) 0.0237(6) Uani 1 1 d . . . C11 C 0.3658(3) 0.7389(4) 0.14072(11) 0.0273(6) Uani 1 1 d . . . H11 H 0.3051 0.7803 0.1613 0.033 Uiso 1 1 calc R . . C12 C 0.3508(3) 0.7724(4) 0.09080(11) 0.0257(6) Uani 1 1 d . . . H12 H 0.2788 0.8346 0.0781 0.031 Uiso 1 1 calc R . . C13 C 0.4411(3) 0.7154(4) 0.05921(10) 0.0204(6) Uani 1 1 d . . . C14 C 0.5471(3) 0.6222(4) 0.07905(10) 0.0246(6) Uani 1 1 d . . . H14 H 0.6095 0.5848 0.0587 0.029 Uiso 1 1 calc R . . C15 C 0.5618(3) 0.5839(4) 0.12857(11) 0.0263(6) Uani 1 1 d . . . H15 H 0.6325 0.5181 0.1410 0.032 Uiso 1 1 calc R . . C16 C 0.4255(3) 0.7582(4) 0.00624(10) 0.0216(6) Uani 1 1 d . . . C17 C 0.3059(3) 0.7860(4) -0.01764(11) 0.0265(6) Uani 1 1 d . . . H17 H 0.2332 0.7683 -0.0007 0.032 Uiso 1 1 calc R . . C18 C 0.2949(3) 0.8394(4) -0.06606(11) 0.0262(6) Uani 1 1 d . . . H18 H 0.2141 0.8585 -0.0810 0.031 Uiso 1 1 calc R . . C19 C 0.5108(3) 0.8307(4) -0.07072(11) 0.0248(6) Uani 1 1 d . . . H19 H 0.5817 0.8426 -0.0890 0.030 Uiso 1 1 calc R . . C20 C 0.5295(3) 0.7783(4) -0.02222(11) 0.0240(6) Uani 1 1 d . . . H20 H 0.6113 0.7565 -0.0086 0.029 Uiso 1 1 calc R . . N1 N 0.6155(2) 0.8708(3) 0.23174(9) 0.0258(5) Uani 1 1 d . . . N2 N 0.3453(3) 0.3280(4) 0.19570(10) 0.0353(6) Uani 1 1 d . . . H2A H 0.3166 0.3635 0.1671 0.042 Uiso 1 1 calc R . . N3 N 0.3965(2) 0.8653(3) -0.09274(9) 0.0258(5) Uani 1 1 d . . . Ag1 Ag 0.62239(2) 0.99093(3) 0.161228(8) 0.03318(10) Uani 1 1 d . . . B1 B 0.1225(4) 0.2104(7) 0.08277(17) 0.0479(11) Uani 1 1 d . . . F1 F 0.1341(3) 0.0720(4) 0.11756(9) 0.0661(7) Uani 1 1 d . . . F2 F 0.1841(3) 0.3618(5) 0.10281(15) 0.1164(14) Uani 1 1 d . . . F3 F 0.1768(3) 0.1461(5) 0.04190(10) 0.0943(11) Uani 1 1 d . . . F4 F -0.0034(2) 0.2531(4) 0.07163(10) 0.0624(7) Uani 1 1 d . . . C21 C 0.9770(5) 0.7160(7) 0.05809(16) 0.0644(12) Uani 1 1 d . . . H21A H 0.9215 0.6863 0.0299 0.097 Uiso 1 1 calc R . . H21B H 1.0299 0.6118 0.0667 0.097 Uiso 1 1 calc R . . H21C H 1.0295 0.8190 0.0506 0.097 Uiso 1 1 calc R . . C22 C 0.9018(4) 0.7629(5) 0.09895(14) 0.0389(8) Uani 1 1 d . . . N4 N 0.8429(4) 0.8013(5) 0.13038(13) 0.0562(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0301(17) 0.0332(15) 0.0279(16) -0.0002(13) -0.0014(13) -0.0085(13) C2 0.0387(19) 0.0388(17) 0.0213(15) 0.0014(14) -0.0043(13) -0.0065(14) C3 0.0295(16) 0.0310(15) 0.0216(15) 0.0026(12) 0.0002(12) -0.0036(13) C4 0.0232(15) 0.0266(14) 0.0197(14) 0.0013(12) 0.0015(11) -0.0014(11) C5 0.0231(15) 0.0270(14) 0.0210(14) -0.0006(12) 0.0027(11) 0.0018(12) C6 0.0250(15) 0.0278(14) 0.0231(15) -0.0030(12) 0.0030(12) -0.0027(12) C7 0.0345(17) 0.0291(15) 0.0241(15) 0.0052(13) 0.0020(13) 0.0033(13) C8 0.049(2) 0.0291(17) 0.054(2) 0.0127(16) 0.0224(19) 0.0042(15) C9 0.037(2) 0.0317(17) 0.062(2) -0.0103(17) 0.0161(18) -0.0096(15) C10 0.0266(15) 0.0232(14) 0.0213(14) -0.0024(12) 0.0015(12) -0.0038(11) C11 0.0263(16) 0.0322(15) 0.0241(15) -0.0016(13) 0.0074(12) 0.0020(13) C12 0.0214(14) 0.0303(15) 0.0256(15) 0.0015(12) 0.0021(12) 0.0027(12) C13 0.0225(14) 0.0189(12) 0.0200(14) -0.0028(11) 0.0023(11) -0.0031(11) C14 0.0260(15) 0.0276(14) 0.0202(14) -0.0042(12) 0.0026(12) 0.0034(12) C15 0.0278(16) 0.0280(15) 0.0228(14) -0.0011(12) -0.0012(12) 0.0061(12) C16 0.0243(15) 0.0184(12) 0.0221(14) -0.0033(11) 0.0023(12) -0.0023(11) C17 0.0240(15) 0.0305(15) 0.0255(15) -0.0023(13) 0.0049(12) -0.0020(12) C18 0.0250(15) 0.0287(15) 0.0243(15) -0.0010(12) -0.0021(12) 0.0005(12) C19 0.0257(15) 0.0250(14) 0.0242(15) -0.0020(12) 0.0057(12) -0.0037(12) C20 0.0226(14) 0.0240(14) 0.0251(15) -0.0019(12) 0.0002(12) -0.0011(11) N1 0.0260(13) 0.0293(12) 0.0221(12) 0.0020(11) 0.0021(10) -0.0036(10) N2 0.0342(16) 0.0363(15) 0.0358(15) -0.0052(12) 0.0042(12) -0.0052(12) N3 0.0310(14) 0.0243(12) 0.0221(12) 0.0013(10) 0.0021(10) -0.0005(10) Ag1 0.04336(16) 0.03323(14) 0.02255(13) 0.00650(10) -0.00080(10) -0.00813(11) B1 0.032(2) 0.066(3) 0.046(3) -0.001(2) 0.0028(19) 0.001(2) F1 0.0796(18) 0.0671(16) 0.0528(15) -0.0017(13) 0.0121(13) 0.0210(14) F2 0.100(3) 0.073(2) 0.167(4) 0.026(2) -0.060(2) -0.0314(18) F3 0.0675(18) 0.163(3) 0.0547(16) 0.0261(19) 0.0239(14) 0.039(2) F4 0.0277(11) 0.0792(17) 0.0802(17) -0.0036(14) 0.0021(11) 0.0068(11) C21 0.069(3) 0.074(3) 0.051(3) -0.004(2) 0.011(2) 0.009(2) C22 0.042(2) 0.0350(18) 0.039(2) 0.0048(16) -0.0059(16) -0.0004(15) N4 0.061(2) 0.054(2) 0.056(2) 0.0001(18) 0.0152(18) -0.0032(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.316(4) . ? C1 C2 1.427(4) . ? C1 H1 0.9300 . ? C2 C3 1.350(4) . ? C2 H2 0.9300 . ? C3 C4 1.447(4) . ? C3 H3 0.9300 . ? C4 C5 1.374(4) . ? C4 N1 1.415(4) . ? C5 C6 1.434(4) . ? C5 C10 1.497(4) . ? C6 N2 1.389(4) . ? C6 C7 1.391(4) . ? C7 C8 1.388(5) . ? C7 H7 0.9300 . ? C8 C9 1.373(5) . ? C8 H8 0.9300 . ? C9 N2 1.357(4) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 C15 1.389(4) . ? C11 C12 1.385(4) . ? C11 H11 0.9300 . ? C12 C13 1.390(4) . ? C12 H12 0.9300 . ? C13 C14 1.386(4) . ? C13 C16 1.480(4) . ? C14 C15 1.380(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.394(4) . ? C16 C17 1.395(4) . ? C17 C18 1.377(4) . ? C17 H17 0.9300 . ? C18 N3 1.349(4) . ? C18 H18 0.9300 . ? C19 N3 1.335(4) . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? N1 Ag1 2.121(2) . ? N2 H2A 0.8600 . ? N3 Ag1 2.141(2) 3_675 ? Ag1 N3 2.141(2) 3_675 ? B1 F3 1.371(5) . ? B1 F2 1.372(6) . ? B1 F4 1.377(5) . ? B1 F1 1.383(5) . ? C21 C22 1.453(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.128(5) . ? 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 111.7(3) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.9(3) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 107.1(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 122.9(3) . . ? C5 C4 C3 129.6(3) . . ? N1 C4 C3 107.6(2) . . ? C4 C5 C6 124.1(3) . . ? C4 C5 C10 120.7(3) . . ? C6 C5 C10 115.2(2) . . ? N2 C6 C7 107.1(3) . . ? N2 C6 C5 122.6(3) . . ? C7 C6 C5 130.4(3) . . ? C8 C7 C6 107.7(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C9 C8 C7 107.8(3) . . ? C9 C8 H8 126.1 . . ? C7 C8 H8 126.1 . . ? N2 C9 C8 108.8(3) . . ? N2 C9 H9 125.6 . . ? C8 C9 H9 125.6 . . ? C11 C10 C15 119.1(3) . . ? C11 C10 C5 120.8(3) . . ? C15 C10 C5 120.0(3) . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.5(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 118.0(3) . . ? C14 C13 C16 121.3(2) . . ? C12 C13 C16 120.6(3) . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 120.4(3) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C20 C16 C17 116.4(3) . . ? C20 C16 C13 121.9(3) . . ? C17 C16 C13 121.8(3) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? N3 C18 C17 122.7(3) . . ? N3 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? N3 C19 C20 123.5(3) . . ? N3 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C16 119.8(3) . . ? C19 C20 H20 120.1 . . ? C16 C20 H20 120.1 . . ? C1 N1 C4 106.7(2) . . ? C1 N1 Ag1 123.4(2) . . ? C4 N1 Ag1 129.46(19) . . ? C9 N2 C6 108.7(3) . . ? C9 N2 H2A 125.7 . . ? C6 N2 H2A 125.7 . . ? C19 N3 C18 117.1(2) . . ? C19 N3 Ag1 120.98(19) . 3_675 ? C18 N3 Ag1 120.6(2) . 3_675 ? N1 Ag1 N3 171.15(9) . 3_675 ? F3 B1 F2 112.7(4) . . ? F3 B1 F4 110.2(4) . . ? F2 B1 F4 109.3(4) . . ? F3 B1 F1 106.9(4) . . ? F2 B1 F1 106.8(4) . . ? F4 B1 F1 110.8(4) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C21 179.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.116 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.082 #===END ###Material relevant to compound 12 at 173K ## data_12 _database_code_depnum_ccdc_archive 'CCDC 791554' #TrackingRef '- dalton_dmitry.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 Ag2 N8, 2(C F3 O3 S), 3(C2 H3 N) ' _chemical_formula_sum 'C44 H37 Ag2 F6 N11 O6 S2' _chemical_formula_weight 1209.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7000(3) _cell_length_b 20.4863(5) _cell_length_c 18.5461(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.8480(10) _cell_angle_gamma 90.00 _cell_volume 4685.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9861 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9146 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details sadabs _exptl_special_details ; One triflate anion is disordered over two positions. These two positions have been modeled accordingly. Owing to the vicinity of an inversion center, an alert is generated regarding the proximity of this anion and its symmetry equivalent. An acetonitrile is also disordered over two positions, modeled accordingly. The hydrogen atoms on this molecule have not been introduced but are taken into account in the molecular formula. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49682 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10775 _reflns_number_gt 9305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+5.5992P] 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 10775 _refine_ls_number_parameters 724 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.197 _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 0.8755(2) 0.71499(15) 0.63665(16) 0.0248(6) Uani 1 1 d . . . H1 H 0.8327 0.6849 0.6541 0.030 Uiso 1 1 calc R . . C2 C 0.9703(2) 0.74345(15) 0.68106(16) 0.0263(6) Uani 1 1 d . . . H2A H 1.0006 0.7351 0.7310 0.032 Uiso 1 1 calc R . . C3 C 1.0086(2) 0.78543(14) 0.63663(16) 0.0239(6) Uani 1 1 d . . . H3 H 1.0696 0.8119 0.6506 0.029 Uiso 1 1 calc R . . C4 C 0.9371(2) 0.78121(14) 0.56399(16) 0.0219(6) Uani 1 1 d . . . C5 C 0.9467(2) 0.80977(13) 0.49789(16) 0.0210(6) Uani 1 1 d . . . C6 C 1.0130(2) 0.86537(14) 0.49510(17) 0.0252(6) Uani 1 1 d . . . C7 C 1.0601(3) 0.88628(16) 0.4382(2) 0.0334(7) Uani 1 1 d . . . H7 H 1.0511 0.8669 0.3918 0.040 Uiso 1 1 calc R . . C8 C 1.1223(3) 0.94090(18) 0.4631(2) 0.0450(9) Uani 1 1 d . . . H8 H 1.1634 0.9645 0.4369 0.054 Uiso 1 1 calc R . . C9 C 1.1121(3) 0.95390(16) 0.5341(2) 0.0422(9) Uani 1 1 d . . . H9 H 1.1445 0.9884 0.5638 0.051 Uiso 1 1 calc R . . C10 C 0.8905(2) 0.78068(14) 0.42536(16) 0.0200(6) Uani 1 1 d . . . C11 C 0.8331(2) 0.81975(14) 0.36747(16) 0.0231(6) Uani 1 1 d . . . H11 H 0.8295 0.8646 0.3743 0.028 Uiso 1 1 calc R . . C12 C 0.7815(2) 0.79228(14) 0.29981(16) 0.0235(6) Uani 1 1 d . . . H12 H 0.7425 0.8186 0.2618 0.028 Uiso 1 1 calc R . . C13 C 0.7881(2) 0.72533(14) 0.28893(15) 0.0201(6) Uani 1 1 d . . . C14 C 0.8459(2) 0.68581(14) 0.34570(16) 0.0214(6) Uani 1 1 d . . . H14 H 0.8512 0.6412 0.3383 0.026 Uiso 1 1 calc R . . C15 C 0.8957(2) 0.71353(14) 0.41353(16) 0.0215(6) Uani 1 1 d . . . H15 H 0.9331 0.6870 0.4518 0.026 Uiso 1 1 calc R . . C16 C 0.7721(3) 0.64458(14) 0.18491(17) 0.0268(7) Uani 1 1 d . . . H16 H 0.8336 0.6195 0.2037 0.032 Uiso 1 1 calc R . . C17 C 0.7004(2) 0.63662(15) 0.11879(17) 0.0271(7) Uani 1 1 d . . . H17 H 0.7042 0.6047 0.0839 0.033 Uiso 1 1 calc R . . C18 C 0.6450(2) 0.71904(15) 0.17199(16) 0.0238(6) Uani 1 1 d . . . H18 H 0.6047 0.7546 0.1813 0.029 Uiso 1 1 calc R . . C19 C 0.3161(2) 0.68741(15) -0.12619(16) 0.0253(6) Uani 1 1 d . . . H19 H 0.3613 0.6581 -0.1424 0.030 Uiso 1 1 calc R . . C20 C 0.2203(2) 0.71515(16) -0.17283(17) 0.0282(7) Uani 1 1 d . . . H20 H 0.1925 0.7068 -0.2231 0.034 Uiso 1 1 calc R . . C21 C 0.1781(2) 0.75573(15) -0.12976(16) 0.0244(6) Uani 1 1 d . . . H21 H 0.1160 0.7811 -0.1450 0.029 Uiso 1 1 calc R . . C22 C 0.2471(2) 0.75239(14) -0.05567(16) 0.0205(6) Uani 1 1 d . . . C23 C 0.2359(2) 0.78240(14) 0.00832(15) 0.0206(6) Uani 1 1 d . . . C24 C 0.1648(2) 0.83589(13) 0.01099(16) 0.0209(6) Uani 1 1 d . . . C25 C 0.0587(3) 0.92251(15) -0.02413(18) 0.0298(7) Uani 1 1 d . . . H25 H 0.0224 0.9566 -0.0527 0.036 Uiso 1 1 calc R . . C26 C 0.0558(3) 0.90893(15) 0.04809(19) 0.0308(7) Uani 1 1 d . . . H26 H 0.0166 0.9314 0.0766 0.037 Uiso 1 1 calc R . . C27 C 0.1229(2) 0.85509(14) 0.07048(17) 0.0246(6) Uani 1 1 d . . . H27 H 0.1371 0.8355 0.1170 0.029 Uiso 1 1 calc R . . C28 C 0.2973(2) 0.75952(14) 0.08249(16) 0.0207(6) Uani 1 1 d . . . C29 C 0.2907(2) 0.69489(14) 0.10475(16) 0.0234(6) Uani 1 1 d . . . H29 H 0.2535 0.6644 0.0709 0.028 Uiso 1 1 calc R . . C30 C 0.3388(2) 0.67569(14) 0.17667(16) 0.0244(6) Uani 1 1 d . . . H30 H 0.3338 0.6326 0.1912 0.029 Uiso 1 1 calc R . . C31 C 0.3947(2) 0.72115(14) 0.22699(16) 0.0206(6) Uani 1 1 d . . . C32 C 0.4040(2) 0.78565(14) 0.20539(16) 0.0221(6) Uani 1 1 d . . . H32 H 0.4427 0.8158 0.2390 0.027 Uiso 1 1 calc R . . C33 C 0.3554(2) 0.80450(14) 0.13357(16) 0.0227(6) Uani 1 1 d . . . H33 H 0.3614 0.8475 0.1191 0.027 Uiso 1 1 calc R . . C34 C 0.4075(2) 0.65588(14) 0.34343(17) 0.0248(6) Uani 1 1 d . . . H34 H 0.3469 0.6293 0.3284 0.030 Uiso 1 1 calc R . . C35 C 0.4785(2) 0.65639(15) 0.41084(17) 0.0261(6) Uani 1 1 d . . . H35 H 0.4746 0.6296 0.4506 0.031 Uiso 1 1 calc R . . C36 C 0.5339(2) 0.72980(14) 0.34496(16) 0.0228(6) Uani 1 1 d . . . H36 H 0.5740 0.7629 0.3299 0.027 Uiso 1 1 calc R . . N1 N 0.85461(19) 0.73636(11) 0.56704(13) 0.0207(5) Uani 1 1 d . . . N2 N 1.0477(2) 0.90849(12) 0.55311(15) 0.0301(6) Uani 1 1 d . . . H2 H 1.0305 0.9065 0.5952 0.036 Uiso 1 1 calc R . . N3 N 0.6205(2) 0.68355(12) 0.11133(14) 0.0252(5) Uani 1 1 d . . . N4 N 0.33217(19) 0.70863(12) -0.05737(13) 0.0224(5) Uani 1 1 d . . . N5 N 0.1227(2) 0.87814(11) -0.04672(14) 0.0232(5) Uani 1 1 d . . . H5 H 0.1353 0.8765 -0.0902 0.028 Uiso 1 1 calc R . . N6 N 0.5577(2) 0.70307(12) 0.41123(13) 0.0235(5) Uani 1 1 d . . . N7 N 0.73658(19) 0.69726(12) 0.21927(13) 0.0216(5) Uani 1 1 d . . . N8 N 0.44366(19) 0.70285(12) 0.30154(13) 0.0207(5) Uani 1 1 d . . . Ag1 Ag 0.479591(19) 0.693213(12) 0.023918(13) 0.02743(7) Uani 1 1 d . . . Ag2 Ag 0.700367(19) 0.724281(11) 0.493378(13) 0.02659(7) Uani 1 1 d . . . C37 C 0.0942(3) 0.46390(17) 0.2751(2) 0.0386(8) Uani 1 1 d . . . O1 O 0.1430(2) 0.58423(14) 0.30007(17) 0.0567(8) Uani 1 1 d . . . O2 O 0.0033(3) 0.55558(13) 0.18911(14) 0.0534(8) Uani 1 1 d . . . O3 O -0.0339(2) 0.54701(14) 0.30999(15) 0.0492(7) Uani 1 1 d . . . F1 F 0.1403(2) 0.44947(13) 0.34572(14) 0.0667(8) Uani 1 1 d . . . F2 F 0.1659(2) 0.45289(13) 0.23567(16) 0.0711(8) Uani 1 1 d . . . F3 F 0.0132(2) 0.42234(11) 0.25236(16) 0.0676(7) Uani 1 1 d . . . S3 S 0.04762(8) 0.54754(4) 0.26737(5) 0.03370(19) Uani 1 1 d . . . S2 S 0.59670(7) 0.91929(4) 0.38843(6) 0.0402(2) Uani 1 1 d D . . C43 C 0.2796(5) -0.0267(4) 0.2486(4) 0.094(2) Uani 1 1 d D . . C38 C 0.5912(7) 1.0050(4) 0.3726(5) 0.049(2) Uani 0.492(3) 1 d PD A 1 C44 C 0.3393(7) 0.0341(4) 0.2262(5) 0.051(2) Uani 0.492(3) 1 d PD A 1 N11 N 0.3807(7) 0.0749(4) 0.2107(4) 0.067(2) Uani 0.492(3) 1 d PD A 1 O4 O 0.5788(6) 0.8865(3) 0.3247(3) 0.0491(16) Uani 0.492(3) 1 d PD A 1 O5 O 0.5105(5) 0.9102(3) 0.4335(3) 0.0549(17) Uani 0.492(3) 1 d PD A 1 O6 O 0.7046(5) 0.9133(3) 0.4455(3) 0.0582(17) Uani 0.492(3) 1 d PD A 1 F4 F 0.6078(7) 1.0438(3) 0.4295(4) 0.077(2) Uani 0.492(3) 1 d PD A 1 F5 F 0.4972(5) 1.0207(3) 0.3280(5) 0.093(2) Uani 0.492(3) 1 d PD A 1 F6 F 0.6667(5) 1.0176(3) 0.3350(3) 0.0711(17) Uani 0.492(3) 1 d PD A 1 C38A C 0.5411(6) 0.9856(4) 0.4255(4) 0.047(2) Uani 0.508(3) 1 d PD A 2 C45 C 0.2458(10) -0.0326(5) 0.3178(6) 0.083(3) Uani 0.508(3) 1 d PD A 2 N12 N 0.3020(11) -0.0413(8) 0.1962(7) 0.138(5) Uani 0.508(3) 1 d PD A 2 F4A F 0.4443(4) 0.9689(3) 0.4369(3) 0.087(2) Uani 0.508(3) 1 d PD . 2 F5A F 0.6099(4) 0.9985(3) 0.4920(3) 0.082(2) Uani 0.508(3) 1 d PD . 2 F6A F 0.5269(5) 1.0392(2) 0.3855(4) 0.0714(18) Uani 0.508(3) 1 d PD A 2 O4A O 0.6150(5) 0.8686(3) 0.4368(3) 0.0566(17) Uani 0.508(3) 1 d PD A 2 O5A O 0.5120(5) 0.9051(3) 0.3163(3) 0.0405(13) Uani 0.508(3) 1 d PD A 2 O6A O 0.6922(4) 0.9485(2) 0.3657(3) 0.0396(13) Uani 0.508(3) 1 d PD A 2 C39 C 0.3964(3) 0.4110(2) 0.3743(2) 0.0433(9) Uani 1 1 d . . . C40 C 0.4212(4) 0.4708(2) 0.3396(3) 0.0673(14) Uani 1 1 d . . . H40A H 0.3710 0.4762 0.2923 0.101 Uiso 1 1 calc R . . H40B H 0.4937 0.4685 0.3327 0.101 Uiso 1 1 calc R . . H40C H 0.4155 0.5074 0.3708 0.101 Uiso 1 1 calc R . . N9 N 0.3754(3) 0.36488(17) 0.4016(2) 0.0561(9) Uani 1 1 d . . . C42 C 0.3123(3) -0.0004(2) 0.0193(2) 0.0470(10) Uani 1 1 d . . . C41 C 0.2515(4) 0.0552(2) 0.0342(3) 0.0657(13) Uani 1 1 d . . . H41A H 0.2991 0.0846 0.0670 0.099 Uiso 1 1 calc R . . H41B H 0.1953 0.0409 0.0571 0.099 Uiso 1 1 calc R . . H41C H 0.2196 0.0771 -0.0115 0.099 Uiso 1 1 calc R . . N10 N 0.3594(3) -0.0434(2) 0.0066(3) 0.0803(14) 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 0.0213(15) 0.0317(16) 0.0213(15) 0.0016(12) 0.0050(12) 0.0020(12) C2 0.0259(16) 0.0351(16) 0.0161(14) -0.0002(12) 0.0016(12) 0.0048(13) C3 0.0197(15) 0.0283(15) 0.0213(15) -0.0047(12) 0.0005(11) 0.0002(12) C4 0.0194(14) 0.0225(14) 0.0228(15) -0.0036(11) 0.0032(11) 0.0007(11) C5 0.0173(14) 0.0214(13) 0.0234(15) -0.0007(11) 0.0030(11) 0.0036(11) C6 0.0262(16) 0.0226(14) 0.0266(16) -0.0009(12) 0.0058(12) 0.0017(12) C7 0.0347(18) 0.0317(17) 0.0372(19) 0.0015(15) 0.0151(15) -0.0040(14) C8 0.042(2) 0.0342(19) 0.063(3) 0.0065(18) 0.0195(19) -0.0099(16) C9 0.039(2) 0.0239(16) 0.062(3) -0.0039(16) 0.0076(18) -0.0095(14) C10 0.0193(14) 0.0223(14) 0.0187(14) 0.0002(11) 0.0050(11) -0.0005(11) C11 0.0283(16) 0.0203(13) 0.0215(15) -0.0001(11) 0.0077(12) 0.0018(11) C12 0.0288(16) 0.0249(14) 0.0166(14) 0.0044(11) 0.0049(11) 0.0056(12) C13 0.0177(14) 0.0248(14) 0.0180(14) -0.0021(11) 0.0045(11) 0.0002(11) C14 0.0224(14) 0.0201(13) 0.0210(14) -0.0005(11) 0.0038(11) 0.0020(11) C15 0.0206(14) 0.0235(14) 0.0195(14) 0.0028(11) 0.0032(11) 0.0017(11) C16 0.0246(16) 0.0227(14) 0.0301(17) -0.0030(12) 0.0009(13) 0.0042(12) C17 0.0276(16) 0.0251(15) 0.0261(16) -0.0040(12) 0.0015(12) 0.0047(12) C18 0.0200(15) 0.0291(15) 0.0220(15) 0.0017(12) 0.0047(11) 0.0031(12) C19 0.0247(15) 0.0299(15) 0.0211(15) -0.0047(12) 0.0048(12) 0.0021(12) C20 0.0240(16) 0.0391(17) 0.0198(15) -0.0028(13) 0.0016(12) 0.0012(13) C21 0.0201(15) 0.0306(15) 0.0201(15) 0.0022(12) 0.0001(11) 0.0014(12) C22 0.0190(14) 0.0221(13) 0.0201(14) 0.0006(11) 0.0039(11) -0.0005(11) C23 0.0178(14) 0.0242(14) 0.0182(14) 0.0009(11) 0.0012(11) -0.0009(11) C24 0.0212(14) 0.0187(13) 0.0214(14) 0.0009(11) 0.0025(11) -0.0011(11) C25 0.0302(17) 0.0209(14) 0.0366(18) 0.0033(13) 0.0043(14) 0.0042(12) C26 0.0343(18) 0.0250(15) 0.0346(18) -0.0051(13) 0.0110(14) 0.0048(13) C27 0.0268(16) 0.0259(15) 0.0216(15) 0.0013(12) 0.0070(12) 0.0003(12) C28 0.0174(14) 0.0245(14) 0.0199(14) -0.0014(11) 0.0041(11) 0.0019(11) C29 0.0215(15) 0.0249(14) 0.0223(15) -0.0032(12) 0.0027(11) -0.0030(11) C30 0.0234(15) 0.0229(14) 0.0251(15) 0.0005(12) 0.0021(12) -0.0022(11) C31 0.0160(13) 0.0265(14) 0.0183(14) 0.0005(11) 0.0023(11) 0.0014(11) C32 0.0189(14) 0.0257(14) 0.0203(14) -0.0038(11) 0.0018(11) -0.0015(11) C33 0.0243(15) 0.0198(13) 0.0220(15) 0.0003(11) 0.0015(12) 0.0003(11) C34 0.0221(15) 0.0247(14) 0.0266(16) 0.0034(12) 0.0036(12) -0.0030(11) C35 0.0285(16) 0.0249(15) 0.0243(15) 0.0043(12) 0.0052(12) -0.0011(12) C36 0.0188(14) 0.0276(15) 0.0209(14) 0.0013(12) 0.0025(11) -0.0033(11) N1 0.0202(12) 0.0234(12) 0.0173(12) -0.0004(9) 0.0021(9) -0.0002(9) N2 0.0332(15) 0.0246(13) 0.0320(15) -0.0041(11) 0.0064(12) -0.0028(11) N3 0.0221(13) 0.0303(13) 0.0207(13) -0.0007(10) 0.0003(10) 0.0014(10) N4 0.0195(12) 0.0269(12) 0.0200(12) -0.0001(10) 0.0028(10) 0.0021(10) N5 0.0249(13) 0.0222(12) 0.0216(13) 0.0010(10) 0.0040(10) 0.0021(10) N6 0.0196(12) 0.0286(13) 0.0202(12) 0.0018(10) 0.0006(10) -0.0010(10) N7 0.0199(12) 0.0239(12) 0.0194(12) 0.0001(10) 0.0017(10) 0.0023(9) N8 0.0186(12) 0.0246(12) 0.0180(12) 0.0017(10) 0.0025(9) -0.0001(9) Ag1 0.02137(12) 0.03418(13) 0.02303(12) 0.00010(9) -0.00201(9) 0.00430(9) Ag2 0.02216(12) 0.03190(13) 0.02209(12) -0.00084(9) -0.00181(9) -0.00213(9) C37 0.043(2) 0.0318(18) 0.039(2) -0.0001(15) 0.0066(16) 0.0094(15) O1 0.0583(19) 0.0477(16) 0.0634(19) -0.0165(14) 0.0130(15) -0.0147(14) O2 0.074(2) 0.0496(16) 0.0314(14) 0.0159(12) 0.0014(13) 0.0029(14) O3 0.0435(16) 0.0614(18) 0.0423(16) -0.0122(13) 0.0095(12) 0.0146(13) F1 0.0724(18) 0.0700(17) 0.0518(15) 0.0258(13) 0.0031(13) 0.0288(14) F2 0.0789(19) 0.0661(17) 0.080(2) -0.0175(15) 0.0414(16) 0.0228(15) F3 0.082(2) 0.0340(12) 0.0825(19) -0.0043(12) 0.0123(15) -0.0111(12) S3 0.0432(5) 0.0246(4) 0.0290(4) -0.0029(3) 0.0001(4) 0.0061(3) S2 0.0323(5) 0.0269(4) 0.0613(6) -0.0068(4) 0.0113(4) -0.0034(3) C43 0.065(4) 0.125(6) 0.084(5) -0.015(4) 0.001(3) 0.020(4) C38 0.057(6) 0.037(4) 0.052(5) -0.008(4) 0.014(4) -0.017(4) C44 0.044(5) 0.051(5) 0.062(6) 0.007(4) 0.021(4) 0.026(4) N11 0.083(6) 0.077(6) 0.053(5) 0.012(4) 0.042(5) 0.030(5) O4 0.078(5) 0.031(3) 0.038(3) -0.014(2) 0.013(3) -0.009(3) O5 0.067(4) 0.037(3) 0.070(4) 0.001(3) 0.035(3) -0.012(3) O6 0.053(4) 0.075(4) 0.045(3) 0.003(3) 0.008(3) 0.012(3) F4 0.129(6) 0.035(3) 0.081(5) -0.027(3) 0.056(4) -0.018(3) F5 0.065(4) 0.052(4) 0.140(7) -0.005(4) -0.017(4) 0.017(3) F6 0.093(4) 0.059(3) 0.073(4) -0.007(3) 0.045(3) -0.029(3) C38A 0.039(4) 0.051(5) 0.055(5) -0.019(4) 0.018(4) -0.002(4) C45 0.089(8) 0.068(7) 0.090(8) -0.011(6) 0.016(7) 0.014(6) N12 0.106(10) 0.175(14) 0.121(11) -0.036(10) 0.001(9) -0.003(9) F4A 0.059(4) 0.116(5) 0.105(5) -0.041(4) 0.053(3) -0.007(3) F5A 0.087(4) 0.094(5) 0.056(3) -0.045(3) 0.001(3) 0.006(3) F6A 0.074(4) 0.032(3) 0.106(6) -0.006(3) 0.019(4) 0.019(3) O4A 0.080(5) 0.045(3) 0.043(3) 0.017(3) 0.011(3) -0.010(3) O5A 0.044(3) 0.041(3) 0.037(3) -0.010(2) 0.011(3) -0.010(3) O6A 0.027(2) 0.034(3) 0.063(3) -0.004(2) 0.020(2) -0.003(2) C39 0.038(2) 0.045(2) 0.046(2) -0.0128(18) 0.0085(17) -0.0050(17) C40 0.087(4) 0.062(3) 0.054(3) 0.002(2) 0.020(3) -0.028(3) N9 0.051(2) 0.0394(19) 0.074(3) -0.0006(18) 0.0062(19) -0.0051(16) C42 0.041(2) 0.041(2) 0.056(3) -0.0007(19) 0.0044(19) -0.0063(17) C41 0.055(3) 0.047(2) 0.094(4) -0.017(2) 0.016(3) -0.003(2) N10 0.055(3) 0.058(3) 0.126(4) -0.019(3) 0.018(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.328(4) . ? C1 C2 1.412(4) . ? C1 H1 0.9300 . ? C2 C3 1.359(4) . ? C2 H2A 0.9300 . ? C3 C4 1.436(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 N1 1.404(4) . ? C5 C6 1.425(4) . ? C5 C10 1.488(4) . ? C6 N2 1.380(4) . ? C6 C7 1.398(4) . ? C7 C8 1.384(5) . ? C7 H7 0.9300 . ? C8 C9 1.380(6) . ? C8 H8 0.9300 . ? C9 N2 1.340(4) . ? C9 H9 0.9300 . ? C10 C11 1.396(4) . ? C10 C15 1.397(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9300 . ? C12 C13 1.392(4) . ? C12 H12 0.9300 . ? C13 C14 1.390(4) . ? C13 N7 1.422(3) . ? C14 C15 1.387(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.351(4) . ? C16 N7 1.383(4) . ? C16 H16 0.9300 . ? C17 N3 1.380(4) . ? C17 H17 0.9300 . ? C18 N3 1.313(4) . ? C18 N7 1.354(4) . ? C18 H18 0.9300 . ? C19 N4 1.317(4) . ? C19 C20 1.431(4) . ? C19 H19 0.9300 . ? C20 C21 1.350(4) . ? C20 H20 0.9300 . ? C21 C22 1.444(4) . ? C21 H21 0.9300 . ? C22 C23 1.374(4) . ? C22 N4 1.411(4) . ? C23 C24 1.428(4) . ? C23 C28 1.486(4) . ? C24 N5 1.381(4) . ? C24 C27 1.392(4) . ? C25 N5 1.351(4) . ? C25 C26 1.377(5) . ? C25 H25 0.9300 . ? C26 C27 1.395(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.395(4) . ? C28 C33 1.399(4) . ? C29 C30 1.385(4) . ? C29 H29 0.9300 . ? C30 C31 1.387(4) . ? C30 H30 0.9300 . ? C31 C32 1.394(4) . ? C31 N8 1.424(3) . ? C32 C33 1.382(4) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.355(4) . ? C34 N8 1.382(4) . ? C34 H34 0.9300 . ? C35 N6 1.387(4) . ? C35 H35 0.9300 . ? C36 N6 1.313(4) . ? C36 N8 1.351(4) . ? C36 H36 0.9300 . ? N1 Ag2 2.117(2) . ? N2 H2 0.8600 . ? N3 Ag1 2.117(2) . ? N4 Ag1 2.128(2) . ? N5 H5 0.8600 . ? N6 Ag2 2.115(2) . ? C37 F2 1.316(4) . ? C37 F3 1.323(4) . ? C37 F1 1.334(4) . ? C37 S3 1.807(3) . ? O1 S3 1.431(3) . ? O2 S3 1.435(3) . ? O3 S3 1.445(3) . ? S2 O4 1.331(5) . ? S2 O4A 1.356(5) . ? S2 O6A 1.501(4) . ? S2 O6 1.522(5) . ? S2 O5A 1.531(5) . ? S2 O5 1.539(5) . ? S2 C38A 1.746(7) . ? S2 C38 1.779(8) . ? C43 N12 1.117(12) . ? C43 C45 1.453(11) . ? C43 C44 1.565(10) . ? C38 F4 1.296(9) . ? C38 F5 1.320(10) . ? C38 F6 1.339(9) . ? C44 N11 1.063(10) . ? C38A F6A 1.313(9) . ? C38A F4A 1.341(8) . ? C38A F5A 1.355(8) . ? F4A F5A 1.760(7) 3_676 ? F5A F4A 1.760(7) 3_676 ? C39 N9 1.134(5) . ? C39 C40 1.454(6) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C42 N10 1.121(5) . ? C42 C41 1.440(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 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 112.0(3) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 106.7(3) . . ? C3 C2 H2A 126.7 . . ? C1 C2 H2A 126.7 . . ? C2 C3 C4 107.0(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 122.3(3) . . ? C5 C4 C3 129.2(3) . . ? N1 C4 C3 108.2(2) . . ? C4 C5 C6 123.1(3) . . ? C4 C5 C10 120.3(3) . . ? C6 C5 C10 116.6(3) . . ? N2 C6 C7 106.1(3) . . ? N2 C6 C5 124.4(3) . . ? C7 C6 C5 129.4(3) . . ? C8 C7 C6 108.0(3) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C9 C8 C7 107.3(3) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? N2 C9 C8 108.6(3) . . ? N2 C9 H9 125.7 . . ? C8 C9 H9 125.7 . . ? C11 C10 C15 118.6(3) . . ? C11 C10 C5 121.0(3) . . ? C15 C10 C5 120.4(2) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 N7 119.8(2) . . ? C12 C13 N7 120.0(3) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C10 121.1(3) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? C17 C16 N7 106.8(3) . . ? C17 C16 H16 126.6 . . ? N7 C16 H16 126.6 . . ? C16 C17 N3 109.1(3) . . ? C16 C17 H17 125.5 . . ? N3 C17 H17 125.5 . . ? N3 C18 N7 111.3(3) . . ? N3 C18 H18 124.4 . . ? N7 C18 H18 124.4 . . ? N4 C19 C20 111.5(3) . . ? N4 C19 H19 124.2 . . ? C20 C19 H19 124.2 . . ? C21 C20 C19 106.7(3) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? C20 C21 C22 107.3(3) . . ? C20 C21 H21 126.3 . . ? C22 C21 H21 126.3 . . ? C23 C22 N4 122.8(3) . . ? C23 C22 C21 129.5(3) . . ? N4 C22 C21 107.6(2) . . ? C22 C23 C24 124.8(3) . . ? C22 C23 C28 121.2(3) . . ? C24 C23 C28 114.0(2) . . ? N5 C24 C27 106.7(3) . . ? N5 C24 C23 125.8(3) . . ? C27 C24 C23 127.6(3) . . ? N5 C25 C26 108.9(3) . . ? N5 C25 H25 125.6 . . ? C26 C25 H25 125.6 . . ? C25 C26 C27 107.0(3) . . ? C25 C26 H26 126.5 . . ? C27 C26 H26 126.5 . . ? C24 C27 C26 108.0(3) . . ? C24 C27 H27 126.0 . . ? C26 C27 H27 126.0 . . ? C29 C28 C33 119.0(3) . . ? C29 C28 C23 121.2(3) . . ? C33 C28 C23 119.6(3) . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.6(3) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 N8 120.7(3) . . ? C32 C31 N8 118.8(2) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C28 120.7(3) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C35 C34 N8 106.0(3) . . ? C35 C34 H34 127.0 . . ? N8 C34 H34 127.0 . . ? C34 C35 N6 109.4(3) . . ? C34 C35 H35 125.3 . . ? N6 C35 H35 125.3 . . ? N6 C36 N8 111.1(3) . . ? N6 C36 H36 124.5 . . ? N8 C36 H36 124.5 . . ? C1 N1 C4 106.1(2) . . ? C1 N1 Ag2 121.8(2) . . ? C4 N1 Ag2 129.35(19) . . ? C9 N2 C6 109.9(3) . . ? C9 N2 H2 125.1 . . ? C6 N2 H2 125.1 . . ? C18 N3 C17 106.4(2) . . ? C18 N3 Ag1 126.0(2) . . ? C17 N3 Ag1 127.5(2) . . ? C19 N4 C22 106.8(2) . . ? C19 N4 Ag1 122.9(2) . . ? C22 N4 Ag1 128.87(19) . . ? C25 N5 C24 109.4(3) . . ? C25 N5 H5 125.3 . . ? C24 N5 H5 125.3 . . ? C36 N6 C35 106.2(2) . . ? C36 N6 Ag2 123.6(2) . . ? C35 N6 Ag2 129.9(2) . . ? C18 N7 C16 106.5(2) . . ? C18 N7 C13 126.3(2) . . ? C16 N7 C13 127.2(2) . . ? C36 N8 C34 107.3(2) . . ? C36 N8 C31 125.6(2) . . ? C34 N8 C31 127.0(2) . . ? N3 Ag1 N4 174.74(10) . . ? N6 Ag2 N1 171.76(10) . . ? F2 C37 F3 107.5(3) . . ? F2 C37 F1 107.9(3) . . ? F3 C37 F1 107.2(3) . . ? F2 C37 S3 112.0(3) . . ? F3 C37 S3 111.7(3) . . ? F1 C37 S3 110.3(3) . . ? O1 S3 O2 117.10(19) . . ? O1 S3 O3 114.62(17) . . ? O2 S3 O3 113.27(18) . . ? O1 S3 C37 103.71(18) . . ? O2 S3 C37 103.33(17) . . ? O3 S3 C37 102.32(18) . . ? O4 S2 O4A 99.6(4) . . ? O4 S2 O6A 86.0(4) . . ? O4A S2 O6A 118.0(3) . . ? O4 S2 O6 120.7(4) . . ? O4A S2 O6 59.6(3) . . ? O6A S2 O6 64.8(3) . . ? O4 S2 O5A 36.2(3) . . ? O4A S2 O5A 114.0(3) . . ? O6A S2 O5A 106.1(3) . . ? O6 S2 O5A 156.8(3) . . ? O4 S2 O5 115.4(4) . . ? O4A S2 O5 65.2(3) . . ? O6A S2 O5 158.2(3) . . ? O6 S2 O5 104.6(3) . . ? O5A S2 O5 90.5(3) . . ? O4 S2 C38A 138.0(4) . . ? O4A S2 C38A 110.9(4) . . ? O6A S2 C38A 103.3(3) . . ? O6 S2 C38A 99.9(3) . . ? O5A S2 C38A 103.1(3) . . ? O5 S2 C38A 58.2(3) . . ? O4 S2 C38 111.1(4) . . ? O4A S2 C38 149.2(4) . . ? O6A S2 C38 64.1(3) . . ? O6 S2 C38 100.8(4) . . ? O5A S2 C38 93.0(3) . . ? O5 S2 C38 101.7(4) . . ? C38A S2 C38 45.0(4) . . ? N12 C43 C45 159.6(12) . . ? N12 C43 C44 75.1(10) . . ? C45 C43 C44 124.4(8) . . ? F4 C38 F5 107.9(8) . . ? F4 C38 F6 107.9(6) . . ? F5 C38 F6 106.2(7) . . ? F4 C38 S2 118.6(6) . . ? F5 C38 S2 109.8(5) . . ? F6 C38 S2 105.7(6) . . ? N11 C44 C43 179.1(9) . . ? F6A C38A F4A 107.2(7) . . ? F6A C38A F5A 108.8(6) . . ? F4A C38A F5A 108.7(6) . . ? F6A C38A S2 116.2(6) . . ? F4A C38A S2 109.6(5) . . ? F5A C38A S2 106.0(5) . . ? C38A F4A F5A 124.0(5) . 3_676 ? C38A F5A F4A 118.2(5) . 3_676 ? N9 C39 C40 178.8(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N10 C42 C41 178.9(6) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.641 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.096 #===END