# Copyright The Ryal Society of Chemistry, 1998 # 8/03468K data_manuscript loop_ _publ_author_name _publ_author_address 'Nicole Klaassen' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Deutschland ; 'Petra Seringer' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Deutschland ; 'Norbert Emig' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Deutschland ; 'Harald Krautscheid' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Deutschland ; 'Dr. Harald Krautscheid' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Deutschland ; _publ_contact_author_email 'harald@achibm6.chemie.uni-karlsruhe.de' _publ_contact_author_fax 'Int + 721 661921' _publ_contact_author_phone 'Int + 721 608 2970' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Thiocyanato Complexes of the Coinage Metals - Synthesis and Crystal Structures of the Polymeric Pyridine Complexes [AgxCuy(SCN)x+y(py)z] ; data_e7a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Cu(SCN)(NC5H5)] _chemical_formula_analytical ? _chemical_formula_sum 'C6 H5 Cu N2 S' _chemical_formula_weight 200.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 17.435(9) _cell_length_b 3.855(2) _cell_length_c 11.159(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.55(2) _cell_angle_gamma 90.00 _cell_volume 715.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 5 _cell_measurement_theta_max 12.5 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method ? _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 3.257 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 270(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'theta-omega scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% ? _diffrn_reflns_number 1559 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.00 _reflns_number_total 1551 _reflns_number_observed 1283 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE dif4' _computing_cell_refinement 'STOE dif4' _computing_data_reduction 'STOE redu4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL92' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.001(1) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 1551 _refine_ls_number_parameters 112 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.1123 _refine_ls_wR_factor_obs 0.1040 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.072 _refine_ls_restrained_S_all 1.045 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.4064 0.27206(15) 0.5438 0.0344(3) Uani 1 d . . S1 S 0.34513(8) 0.7692(3) 0.43219(10) 0.0269(3) Uani 1 d . . C1 C 0.3705(3) 0.7595(11) 0.3003(5) 0.0266(10) Uani 1 d . . N1 N 0.3861(4) 0.7489(11) 0.2068(5) 0.0375(12) Uani 1 d . . N2 N 0.5276(3) 0.2604(9) 0.5651(4) 0.0304(9) Uani 1 d . . C2 C 0.5783(4) 0.1425(16) 0.6724(6) 0.0388(11) Uani 1 d . . C3 C 0.6605(4) 0.1330(18) 0.6957(6) 0.0454(13) Uani 1 d . . C4 C 0.6933(4) 0.2506(14) 0.6058(6) 0.044(2) Uani 1 d . . C5 C 0.6415(5) 0.3669(19) 0.4945(7) 0.047(2) Uani 1 d . . C6 C 0.5601(4) 0.3717(17) 0.4763(5) 0.0378(12) Uani 1 d . . H1 H 0.5477(40) 0.0543(193) 0.7265(60) 0.054(18) Uiso 1 d . . H2 H 0.6931(45) 0.0608(178) 0.7697(67) 0.052(17) Uiso 1 d . . H3 H 0.7502(44) 0.2666(117) 0.6148(66) 0.031(17) Uiso 1 d . . H4 H 0.6544(33) 0.4371(155) 0.4517(56) 0.028(17) Uiso 1 d . . H5 H 0.5178(27) 0.4693(119) 0.3956(44) 0.017(11) Uiso 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 Cu1 0.0365(4) 0.0487(4) 0.0212(3) 0.0001(5) 0.0135(2) -0.0008(5) S1 0.0346(7) 0.0277(6) 0.0225(5) -0.0017(6) 0.0148(5) -0.0013(6) C1 0.029(3) 0.029(2) 0.023(2) 0.003(2) 0.010(2) 0.004(2) N1 0.051(3) 0.042(3) 0.023(2) 0.003(2) 0.016(2) 0.004(2) N2 0.026(2) 0.036(2) 0.030(2) -0.0005(14) 0.009(2) -0.001(2) C2 0.041(3) 0.043(3) 0.033(3) 0.007(2) 0.011(2) 0.005(2) C3 0.042(4) 0.054(3) 0.034(3) 0.003(3) 0.002(2) 0.010(3) C4 0.031(4) 0.047(4) 0.054(5) -0.005(2) 0.016(3) 0.004(2) C5 0.050(5) 0.051(3) 0.045(3) 0.011(3) 0.023(3) -0.001(3) C6 0.039(3) 0.048(3) 0.030(2) 0.006(2) 0.016(2) 0.006(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 Cu1 N1 1.957(5) 2_565 ? Cu1 N2 2.054(5) . ? Cu1 S1 2.358(2) . ? Cu1 S1 2.377(2) 1_545 ? S1 C1 1.660(6) . ? S1 Cu1 2.377(2) 1_565 ? C1 N1 1.156(8) . ? N1 Cu1 1.957(5) 2_564 ? N2 C2 1.336(7) . ? N2 C6 1.351(8) . ? C2 C3 1.378(8) . ? C3 C4 1.372(10) . ? C4 C5 1.371(10) . ? C5 C6 1.372(9) . ? 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 Cu1 N2 111.1(2) 2_565 . ? N1 Cu1 S1 110.14(15) 2_565 . ? N2 Cu1 S1 111.42(12) . . ? N1 Cu1 S1 105.94(14) 2_565 1_545 ? N2 Cu1 S1 109.08(12) . 1_545 ? S1 Cu1 S1 109.00(6) . 1_545 ? C1 S1 Cu1 104.5(2) . . ? C1 S1 Cu1 106.6(2) . 1_565 ? Cu1 S1 Cu1 109.00(6) . 1_565 ? N1 C1 S1 178.1(5) . . ? C1 N1 Cu1 177.0(5) . 2_564 ? C2 N2 C6 117.0(5) . . ? C2 N2 Cu1 119.4(4) . . ? C6 N2 Cu1 123.6(4) . . ? N2 C2 C3 123.2(5) . . ? C4 C3 C2 119.5(6) . . ? C5 C4 C3 117.7(6) . . ? C4 C5 C6 120.5(6) . . ? N2 C6 C5 122.1(5) . . ? _refine_diff_density_max 1.038 _refine_diff_density_min -.574 _refine_diff_density_rms .117 #=END data_petra6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Cu(SCN)(NC5H5)2] _chemical_formula_analytical ? _chemical_formula_sum 'C11 H10 Cu N3 S' _chemical_formula_weight 279.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 '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 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 5.850(3) _cell_length_b 14.076(6) _cell_length_c 14.792(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.80(4) _cell_angle_gamma 90.00 _cell_volume 1213.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description rod _exptl_crystal_colour 'yellow-green' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method ? _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 1.946 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE IPDS' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8267 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2111 _reflns_number_observed 1796 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL92 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0370P)^2^+0.7261P] 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 refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2110 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_obs 0.0328 _refine_ls_wR_factor_all 0.0768 _refine_ls_wR_factor_obs 0.0708 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.050 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.050 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.61220(5) 0.61239(2) 0.27997(2) 0.03594(13) Uani 1 d . . S1 S 0.38936(10) 0.60240(5) 0.40088(4) 0.0381(2) Uani 1 d . . N1 N -0.0604(4) 0.6145(2) 0.3184(2) 0.0394(5) Uani 1 d . . C1 C 0.1257(4) 0.6099(2) 0.3512(2) 0.0301(5) Uani 1 d . . N2 N 0.5349(4) 0.4969(2) 0.1926(2) 0.0371(5) Uani 1 d . . C2 C 0.6770(6) 0.4754(3) 0.1298(2) 0.0591(9) Uani 1 d . . C3 C 0.6410(7) 0.4004(3) 0.0705(3) 0.0757(12) Uani 1 d . . C4 C 0.4483(6) 0.3446(3) 0.0747(2) 0.0580(8) Uani 1 d . . C5 C 0.3018(6) 0.3659(2) 0.1385(2) 0.0485(7) Uani 1 d . . C6 C 0.3495(5) 0.4417(2) 0.1964(2) 0.0423(6) Uani 1 d . . H1 H 0.8146(76) 0.5193(32) 0.1278(29) 0.092(13) Uiso 1 d . . H2 H 0.7394(78) 0.3844(29) 0.0280(31) 0.083(13) Uiso 1 d . . H3 H 0.4214(59) 0.2906(27) 0.0358(23) 0.063(10) Uiso 1 d . . H4 H 0.1783(68) 0.3303(28) 0.1437(25) 0.069(11) Uiso 1 d . . H5 H 0.2489(57) 0.4609(23) 0.2380(23) 0.052(9) Uiso 1 d . . N3 N 0.5205(4) 0.7258(2) 0.19602(14) 0.0333(5) Uani 1 d . . C7 C 0.6686(5) 0.7960(2) 0.1820(2) 0.0397(6) Uani 1 d . . C8 C 0.6180(6) 0.8701(2) 0.1228(2) 0.0468(7) Uani 1 d . . C9 C 0.4060(6) 0.8721(2) 0.0745(2) 0.0478(7) Uani 1 d . . C10 C 0.2513(5) 0.8010(2) 0.0885(2) 0.0465(7) Uani 1 d . . C11 C 0.3135(5) 0.7298(2) 0.1492(2) 0.0400(6) Uani 1 d . . H6 H 0.8054(53) 0.7944(20) 0.2154(19) 0.038(7) Uiso 1 d . . H7 H 0.7217(62) 0.9155(26) 0.1165(23) 0.060(10) Uiso 1 d . . H8 H 0.3695(56) 0.9217(25) 0.0337(23) 0.056(9) Uiso 1 d . . H9 H 0.0979(58) 0.7984(24) 0.0550(21) 0.055(9) Uiso 1 d . . H10 H 0.2122(55) 0.6758(23) 0.1587(21) 0.050(8) Uiso 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 Cu1 0.0253(2) 0.0384(2) 0.0431(2) 0.00282(14) -0.00281(13) 0.00119(13) S1 0.0246(3) 0.0558(4) 0.0331(3) -0.0005(3) -0.0031(3) 0.0005(3) N1 0.0264(12) 0.0437(13) 0.0479(13) 0.0013(10) 0.0017(10) -0.0005(9) C1 0.0261(13) 0.0328(13) 0.0317(12) -0.0006(10) 0.0045(10) -0.0015(10) N2 0.0345(11) 0.0366(12) 0.0400(12) -0.0017(9) 0.0011(9) 0.0007(9) C2 0.054(2) 0.064(2) 0.062(2) -0.018(2) 0.020(2) -0.014(2) C3 0.073(3) 0.086(3) 0.072(2) -0.034(2) 0.031(2) -0.011(2) C4 0.073(2) 0.048(2) 0.053(2) -0.017(2) 0.006(2) -0.005(2) C5 0.053(2) 0.039(2) 0.054(2) -0.0044(13) 0.0044(15) -0.0079(14) C6 0.045(2) 0.039(2) 0.043(2) -0.0040(12) 0.0077(13) -0.0023(12) N3 0.0285(11) 0.0358(11) 0.0351(11) 0.0019(9) -0.0006(9) 0.0015(8) C7 0.0370(14) 0.0401(15) 0.0415(15) -0.0024(12) 0.0003(12) -0.0034(12) C8 0.059(2) 0.0352(15) 0.047(2) -0.0004(12) 0.0142(14) -0.0044(13) C9 0.068(2) 0.039(2) 0.0371(15) 0.0051(12) 0.0100(14) 0.0158(14) C10 0.043(2) 0.059(2) 0.0359(14) 0.0044(13) -0.0012(12) 0.0144(14) C11 0.0331(14) 0.047(2) 0.0395(14) 0.0030(12) -0.0007(11) 0.0012(12) _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 Cu1 N1 1.952(2) 1_655 ? Cu1 N3 2.065(2) . ? Cu1 N2 2.103(2) . ? Cu1 S1 2.3039(14) . ? S1 C1 1.656(3) . ? N1 C1 1.156(3) . ? N1 Cu1 1.952(2) 1_455 ? N2 C2 1.331(4) . ? N2 C6 1.339(4) . ? C2 C3 1.378(5) . ? C3 C4 1.379(5) . ? C4 C5 1.360(5) . ? C5 C6 1.383(4) . ? N3 C7 1.343(4) . ? N3 C11 1.345(3) . ? C7 C8 1.377(4) . ? C8 C9 1.379(5) . ? C9 C10 1.376(5) . ? C10 C11 1.374(4) . ? 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 Cu1 N3 111.24(9) 1_655 . ? N1 Cu1 N2 110.26(9) 1_655 . ? N3 Cu1 N2 101.31(10) . . ? N1 Cu1 S1 112.34(8) 1_655 . ? N3 Cu1 S1 112.24(7) . . ? N2 Cu1 S1 108.89(7) . . ? C1 S1 Cu1 102.61(10) . . ? C1 N1 Cu1 171.1(2) . 1_455 ? N1 C1 S1 178.4(2) . . ? C2 N2 C6 116.9(3) . . ? C2 N2 Cu1 119.3(2) . . ? C6 N2 Cu1 123.7(2) . . ? N2 C2 C3 123.2(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 118.1(3) . . ? C4 C5 C6 119.6(3) . . ? N2 C6 C5 122.9(3) . . ? C7 N3 C11 117.0(2) . . ? C7 N3 Cu1 121.6(2) . . ? C11 N3 Cu1 121.3(2) . . ? N3 C7 C8 123.3(3) . . ? C7 C8 C9 118.8(3) . . ? C10 C9 C8 118.8(3) . . ? C11 C10 C9 119.1(3) . . ? N3 C11 C10 123.0(3) . . ? _refine_diff_density_max .298 _refine_diff_density_min -.341 _refine_diff_density_rms .065 #=END data_ch33 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Ag(SCN)(NC5H5)] _chemical_formula_analytical ? _chemical_formula_sum 'C6 H5 Ag N2 S' _chemical_formula_weight 245.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 4.0221(5) _cell_length_b 10.9748(12) _cell_length_c 17.809(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 786.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 78 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method ? _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 2.749 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'theta/omega scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '<1%' _diffrn_reflns_number 2892 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1387 _reflns_number_observed 1052 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL92 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0366P)^2^+0.4019P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(12) _refine_ls_number_reflns 1386 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_obs 0.0322 _refine_ls_wR_factor_all 0.0880 _refine_ls_wR_factor_obs 0.0713 _refine_ls_goodness_of_fit_all 1.144 _refine_ls_goodness_of_fit_obs 1.079 _refine_ls_restrained_S_all 1.147 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.2688(2) 0.29715(4) 0.27196(3) 0.0570(2) Uani 1 d . . S1 S 0.7646(7) 0.34650(13) 0.18503(9) 0.0449(4) Uani 1 d . . C1 C 0.7674(23) 0.4973(5) 0.1922(3) 0.0367(13) Uani 1 d . . N1 N 0.7743(23) 0.6022(5) 0.1942(3) 0.0543(15) Uani 1 d . . N2 N 0.2537(20) 0.4152(4) 0.3795(2) 0.0447(12) Uani 1 d . . C2 C 0.3754(22) 0.5292(6) 0.3821(4) 0.050(2) Uani 1 d . . H2 H 0.4589(22) 0.5640(6) 0.3377(4) 0.060 Uiso 1 calc R . C3 C 0.3826(23) 0.5965(7) 0.4467(5) 0.063(3) Uani 1 d . . H3 H 0.4678(23) 0.6763(7) 0.4467(5) 0.076 Uiso 1 calc R . C4 C 0.2618(28) 0.5448(7) 0.5122(3) 0.062(2) Uani 1 d . . H4 H 0.2615(28) 0.5892(7) 0.5573(3) 0.074 Uiso 1 calc R . C5 C 0.1434(21) 0.4285(8) 0.5100(4) 0.060(3) Uani 1 d . . H5 H 0.0612(21) 0.3911(8) 0.5537(4) 0.071 Uiso 1 calc R . C6 C 0.1464(19) 0.3665(7) 0.4426(4) 0.051(2) Uani 1 d . . H6 H 0.0681(19) 0.2858(7) 0.4417(4) 0.061 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0903(4) 0.0331(3) 0.0476(3) -0.0001(2) -0.0004(5) 0.0007(5) S1 0.0488(10) 0.0301(7) 0.0558(9) -0.0057(6) -0.0021(15) 0.0000(12) C1 0.038(3) 0.044(3) 0.029(3) -0.002(2) -0.002(4) -0.003(5) N1 0.075(4) 0.031(3) 0.057(3) -0.005(2) 0.008(5) 0.001(5) N2 0.060(3) 0.037(3) 0.037(3) 0.000(2) 0.007(5) 0.006(5) C2 0.074(6) 0.039(4) 0.036(4) 0.004(3) 0.000(3) 0.001(4) C3 0.085(7) 0.040(4) 0.065(5) -0.011(4) -0.005(5) -0.003(4) C4 0.070(6) 0.076(5) 0.039(4) -0.016(3) -0.015(6) 0.033(8) C5 0.064(6) 0.072(5) 0.042(4) 0.008(4) 0.019(4) 0.016(4) C6 0.055(6) 0.047(4) 0.052(4) 0.007(3) 0.003(4) 0.009(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 Ag1 N1 2.230(5) 4_645 ? Ag1 N2 2.313(4) . ? Ag1 S1 2.582(3) . ? Ag1 S1 2.608(3) 1_455 ? S1 C1 1.660(6) . ? S1 Ag1 2.608(3) 1_655 ? C1 N1 1.152(7) . ? N1 Ag1 2.230(5) 4_655 ? N2 C6 1.317(8) . ? N2 C2 1.344(8) . ? C2 C3 1.368(9) . ? C3 C4 1.385(11) . ? C4 C5 1.363(12) . ? C5 C6 1.380(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 108.1(2) 4_645 . ? N1 Ag1 S1 115.0(2) 4_645 . ? N2 Ag1 S1 113.5(2) . . ? N1 Ag1 S1 107.4(2) 4_645 1_455 ? N2 Ag1 S1 110.8(2) . 1_455 ? S1 Ag1 S1 101.60(6) . 1_455 ? C1 S1 Ag1 99.7(3) . . ? C1 S1 Ag1 99.0(3) . 1_655 ? Ag1 S1 Ag1 101.60(6) . 1_655 ? N1 C1 S1 177.2(6) . . ? C1 N1 Ag1 164.9(6) . 4_655 ? C6 N2 C2 117.9(6) . . ? C6 N2 Ag1 119.2(4) . . ? C2 N2 Ag1 122.7(4) . . ? N2 C2 C3 122.6(7) . . ? C2 C3 C4 118.7(7) . . ? C5 C4 C3 118.9(6) . . ? C4 C5 C6 118.9(7) . . ? N2 C6 C5 123.1(7) . . ? _refine_diff_density_max .422 _refine_diff_density_min -.353 _refine_diff_density_rms .090 #=END data_ag5m1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Ag(SCN)(NC5H5)2] _chemical_formula_analytical ? _chemical_formula_sum 'C11 H10 Ag N3 S' _chemical_formula_weight 324.15 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 7.772(2) _cell_length_b 17.084(4) _cell_length_c 18.495(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2455.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 428 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.0 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method ? _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.786 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE IPDS' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12217 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.98 _reflns_number_total 5221 _reflns_number_observed 4953 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0512P)^2^+0.5334P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(3) _refine_ls_number_reflns 5221 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_obs 0.0306 _refine_ls_wR_factor_all 0.0772 _refine_ls_wR_factor_obs 0.0758 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max 0.012 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.21778(4) 0.55543(2) 0.18145(2) 0.04360(9) Uani 1 d . . S1 S -0.00139(12) 0.48036(5) 0.10834(5) 0.0355(2) Uani 1 d . . C1 C 0.1116(5) 0.3978(2) 0.1096(2) 0.0382(8) Uani 1 d . . N1 N 0.1920(6) 0.3406(3) 0.1092(3) 0.0582(11) Uani 1 d . . N2 N 0.2296(4) 0.6786(2) 0.2261(2) 0.0403(7) Uani 1 d . . C2 C 0.1093(5) 0.7340(2) 0.2179(2) 0.0428(8) Uani 1 d . . H2 H 0.0168(5) 0.7240(2) 0.1864(2) 0.051 Uiso 1 calc R . C3 C 0.1145(7) 0.8043(3) 0.2530(3) 0.0536(11) Uani 1 d . . H3 H 0.0277(7) 0.8418(3) 0.2453(3) 0.064 Uiso 1 calc R . C4 C 0.2481(8) 0.8198(3) 0.2995(3) 0.0594(13) Uani 1 d . . H4 H 0.2533(8) 0.8674(3) 0.3248(3) 0.071 Uiso 1 calc R . C5 C 0.3743(7) 0.7638(3) 0.3083(2) 0.0554(12) Uani 1 d . . H5 H 0.4683(7) 0.7730(3) 0.3392(2) 0.066 Uiso 1 calc R . C6 C 0.3605(6) 0.6943(3) 0.2714(3) 0.0494(10) Uani 1 d . . H6 H 0.4462(6) 0.6562(3) 0.2780(3) 0.059 Uiso 1 calc R . N3 N 0.2568(5) 0.4843(2) 0.2920(2) 0.0428(8) Uani 1 d . . C7 C 0.2177(7) 0.5128(3) 0.3580(2) 0.0513(11) Uani 1 d . . H7 H 0.1857(7) 0.5657(3) 0.3622(2) 0.062 Uiso 1 calc R . C8 C 0.2231(8) 0.4669(4) 0.4200(3) 0.0616(13) Uani 1 d . . H8 H 0.1954(8) 0.4888(4) 0.4652(3) 0.074 Uiso 1 calc R . C9 C 0.2689(7) 0.3901(4) 0.4150(3) 0.0622(14) Uani 1 d . . H9 H 0.2728(7) 0.3584(4) 0.4565(3) 0.075 Uiso 1 calc R . C10 C 0.3095(7) 0.3596(3) 0.3475(3) 0.0574(12) Uani 1 d . . H10 H 0.3409(7) 0.3068(3) 0.3423(3) 0.069 Uiso 1 calc R . C11 C 0.3028(6) 0.4083(3) 0.2888(2) 0.0465(10) Uani 1 d . . H11 H 0.3321(6) 0.3874(3) 0.2434(2) 0.056 Uiso 1 calc R . Ag2 Ag 0.17034(4) 0.95816(2) 0.47264(2) 0.04281(9) Uani 1 d . . S2 S 0.43279(12) 1.01405(6) 0.38654(5) 0.0375(2) Uani 1 d . . C12 C 0.3346(5) 1.1008(3) 0.3853(2) 0.0369(8) Uani 1 d . . N4 N 0.2641(5) 1.1602(3) 0.3839(2) 0.0543(9) Uani 1 d . . N5 N 0.2420(5) 0.8294(2) 0.4956(2) 0.0435(8) Uani 1 d . . C13 C 0.1396(6) 0.7671(2) 0.4878(3) 0.0488(10) Uani 1 d . . H13 H 0.0235(6) 0.7755(2) 0.4758(3) 0.059 Uiso 1 calc R . C14 C 0.1964(7) 0.6911(3) 0.4965(3) 0.0592(13) Uani 1 d . . H14 H 0.1205(7) 0.6487(3) 0.4903(3) 0.071 Uiso 1 calc R . C15 C 0.3658(8) 0.6784(3) 0.5144(3) 0.0625(14) Uani 1 d . . H15 H 0.4083(8) 0.6274(3) 0.5207(3) 0.075 Uiso 1 calc R . C16 C 0.4720(7) 0.7428(4) 0.5229(3) 0.0661(14) Uani 1 d . . H16 H 0.5880(7) 0.7361(4) 0.5358(3) 0.079 Uiso 1 calc R . C17 C 0.4068(6) 0.8161(3) 0.5125(3) 0.0566(11) Uani 1 d . . H17 H 0.4810(6) 0.8592(3) 0.5174(3) 0.068 Uiso 1 calc R . N6 N 0.2541(4) 1.0220(2) 0.5773(2) 0.0363(7) Uani 1 d . . C18 C 0.2522(6) 0.9847(3) 0.6407(2) 0.0458(9) Uani 1 d . . H18 H 0.2180(6) 0.9319(3) 0.6414(2) 0.055 Uiso 1 calc R . C19 C 0.2979(7) 1.0196(4) 0.7052(3) 0.0555(12) Uani 1 d . . H19 H 0.2983(7) 0.9906(4) 0.7484(3) 0.067 Uiso 1 calc R . C20 C 0.3431(6) 1.0977(3) 0.7050(3) 0.0543(11) Uani 1 d . . H20 H 0.3719(6) 1.1235(3) 0.7482(3) 0.065 Uiso 1 calc R . C21 C 0.3449(6) 1.1371(3) 0.6397(3) 0.0489(10) Uani 1 d . . H21 H 0.3761(6) 1.1903(3) 0.6375(3) 0.059 Uiso 1 calc R . C22 C 0.3002(6) 1.0972(3) 0.5780(2) 0.0425(9) Uani 1 d . . H22 H 0.3022(6) 1.1244(3) 0.5338(2) 0.051 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0565(2) 0.03197(12) 0.0424(2) -0.00575(12) -0.0013(2) -0.00140(12) S1 0.0334(4) 0.0342(4) 0.0388(4) 0.0015(3) -0.0015(3) 0.0002(3) C1 0.039(2) 0.041(2) 0.035(2) -0.007(2) 0.002(2) -0.002(2) N1 0.059(2) 0.048(2) 0.068(3) -0.013(2) 0.003(2) 0.016(2) N2 0.040(2) 0.0317(15) 0.049(2) -0.0081(15) -0.0025(15) 0.0005(13) C2 0.042(2) 0.038(2) 0.048(2) 0.000(2) 0.003(2) 0.002(2) C3 0.066(3) 0.034(2) 0.061(3) -0.001(2) 0.009(2) 0.008(2) C4 0.090(4) 0.040(2) 0.049(2) -0.009(2) 0.007(2) -0.011(2) C5 0.067(3) 0.053(3) 0.047(2) -0.008(2) -0.006(2) -0.024(2) C6 0.045(2) 0.044(2) 0.059(3) -0.002(2) -0.008(2) -0.005(2) N3 0.047(2) 0.048(2) 0.034(2) 0.0018(14) 0.0011(14) 0.007(2) C7 0.060(3) 0.057(3) 0.037(2) -0.004(2) 0.006(2) 0.012(2) C8 0.065(3) 0.084(4) 0.036(2) 0.002(2) 0.008(2) 0.010(3) C9 0.057(3) 0.081(4) 0.048(3) 0.029(2) -0.001(2) -0.002(3) C10 0.061(3) 0.050(3) 0.061(3) 0.012(2) -0.008(2) 0.001(2) C11 0.056(2) 0.043(2) 0.041(2) -0.001(2) -0.004(2) 0.007(2) Ag2 0.0493(2) 0.03462(14) 0.0445(2) 0.00199(13) -0.01416(14) -0.00529(11) S2 0.0328(4) 0.0415(5) 0.0383(4) -0.0043(4) -0.0037(4) -0.0014(4) C12 0.035(2) 0.046(2) 0.029(2) 0.006(2) -0.0052(14) 0.000(2) N4 0.058(2) 0.050(2) 0.055(2) 0.009(2) -0.005(2) 0.008(2) N5 0.045(2) 0.034(2) 0.051(2) 0.0023(14) -0.0074(15) 0.0027(14) C13 0.041(2) 0.037(2) 0.068(3) 0.005(2) 0.007(2) 0.000(2) C14 0.066(3) 0.035(2) 0.076(3) 0.009(2) 0.026(2) 0.000(2) C15 0.083(4) 0.047(3) 0.058(3) 0.017(2) 0.014(3) 0.030(3) C16 0.059(3) 0.072(3) 0.067(3) 0.005(3) -0.015(3) 0.027(3) C17 0.050(2) 0.050(2) 0.070(3) -0.005(2) -0.020(2) 0.008(2) N6 0.035(2) 0.042(2) 0.0318(15) -0.0025(13) -0.0015(12) -0.0046(13) C18 0.053(2) 0.042(2) 0.042(2) 0.003(2) 0.004(2) -0.011(2) C19 0.066(3) 0.071(3) 0.030(2) 0.005(2) 0.006(2) -0.006(2) C20 0.060(3) 0.067(3) 0.036(2) -0.014(2) -0.003(2) -0.009(2) C21 0.053(2) 0.040(2) 0.054(2) -0.012(2) 0.003(2) -0.006(2) C22 0.050(2) 0.039(2) 0.039(2) 0.003(2) -0.005(2) -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 Ag1 N2 2.262(3) . ? Ag1 N3 2.397(4) . ? Ag1 S1 2.5248(10) . ? Ag1 S1 2.6393(11) 4_565 ? S1 C1 1.662(4) . ? S1 Ag1 2.6393(11) 4_465 ? C1 N1 1.161(6) . ? N2 C2 1.339(5) . ? N2 C6 1.344(6) . ? C2 C3 1.367(6) . ? C3 C4 1.374(8) . ? C4 C5 1.380(9) . ? C5 C6 1.374(7) . ? N3 C7 1.350(6) . ? N3 C11 1.349(6) . ? C7 C8 1.389(7) . ? C8 C9 1.362(9) . ? C9 C10 1.390(8) . ? C10 C11 1.369(7) . ? Ag2 N5 2.308(3) . ? Ag2 N6 2.315(3) . ? Ag2 S2 2.4839(10) 4_475 ? Ag2 S2 2.7583(11) . ? S2 C12 1.667(4) . ? S2 Ag2 2.4839(10) 4_575 ? C12 N4 1.154(6) . ? N5 C13 1.337(6) . ? N5 C17 1.338(6) . ? C13 C14 1.382(6) . ? C14 C15 1.375(8) . ? C15 C16 1.384(9) . ? C16 C17 1.365(7) . ? N6 C22 1.333(6) . ? N6 C18 1.334(6) . ? C18 C19 1.380(7) . ? C19 C20 1.380(9) . ? C20 C21 1.383(7) . ? C21 C22 1.374(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 N2 Ag1 N3 98.89(13) . . ? N2 Ag1 S1 134.06(9) . . ? N3 Ag1 S1 106.53(10) . . ? N2 Ag1 S1 111.67(9) . 4_565 ? N3 Ag1 S1 102.41(9) . 4_565 ? S1 Ag1 S1 99.55(3) . 4_565 ? C1 S1 Ag1 93.86(14) . . ? C1 S1 Ag1 103.50(14) . 4_465 ? Ag1 S1 Ag1 113.65(4) . 4_465 ? N1 C1 S1 178.7(4) . . ? C2 N2 C6 117.3(4) . . ? C2 N2 Ag1 126.0(3) . . ? C6 N2 Ag1 116.4(3) . . ? N2 C2 C3 123.1(4) . . ? C2 C3 C4 119.2(5) . . ? C3 C4 C5 118.6(4) . . ? C6 C5 C4 119.0(5) . . ? N2 C6 C5 122.8(4) . . ? C7 N3 C11 116.5(4) . . ? C7 N3 Ag1 124.1(3) . . ? C11 N3 Ag1 119.0(3) . . ? N3 C7 C8 122.5(5) . . ? C9 C8 C7 119.7(5) . . ? C8 C9 C10 118.8(5) . . ? C11 C10 C9 118.5(5) . . ? N3 C11 C10 124.1(4) . . ? N5 Ag2 N6 103.14(13) . . ? N5 Ag2 S2 118.64(9) . 4_475 ? N6 Ag2 S2 130.92(9) . 4_475 ? N5 Ag2 S2 104.93(10) . . ? N6 Ag2 S2 96.41(9) . . ? S2 Ag2 S2 96.51(4) 4_475 . ? C12 S2 Ag2 100.33(14) . 4_575 ? C12 S2 Ag2 88.68(14) . . ? Ag2 S2 Ag2 104.22(4) 4_575 . ? N4 C12 S2 178.8(4) . . ? C13 N5 C17 117.4(4) . . ? C13 N5 Ag2 126.5(3) . . ? C17 N5 Ag2 115.9(3) . . ? N5 C13 C14 123.1(4) . . ? C15 C14 C13 118.8(5) . . ? C14 C15 C16 118.3(4) . . ? C17 C16 C15 119.5(5) . . ? N5 C17 C16 123.0(5) . . ? C22 N6 C18 117.0(4) . . ? C22 N6 Ag2 122.5(3) . . ? C18 N6 Ag2 120.4(3) . . ? N6 C18 C19 123.4(4) . . ? C20 C19 C18 118.7(4) . . ? C19 C20 C21 118.4(4) . . ? C22 C21 C20 118.7(4) . . ? N6 C22 C21 123.7(4) . . ? _refine_diff_density_max .576 _refine_diff_density_min -.732 _refine_diff_density_rms .073 #=END data_ag7p _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [AgCu(SCN)2(NC5H5)4] _chemical_formula_analytical ? _chemical_formula_sum 'C22 H20 Ag Cu N6 S2' _chemical_formula_weight 603.97 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -.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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3250(7) _cell_length_b 10.9567(5) _cell_length_c 17.1474(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.686(4) _cell_angle_gamma 90.00 _cell_volume 2517.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 70 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.809 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'omega scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '<2%' _diffrn_reflns_number 6953 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4920 _reflns_number_observed 4182 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL92 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 27 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0153P)^2^+1.6730P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_number_reflns 4893 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_obs 0.0253 _refine_ls_wR_factor_all 0.0624 _refine_ls_wR_factor_obs 0.0535 _refine_ls_goodness_of_fit_all 1.092 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.307964(15) 0.54826(2) 0.699735(14) 0.04422(7) Uani 1 d . . Cu1 Cu 0.65880(2) 0.28054(3) 0.71899(2) 0.04424(10) Uani 1 d . . S1 S 0.43335(5) 0.60800(6) 0.62897(4) 0.0420(2) Uani 1 d . . C1 C 0.5182(2) 0.5005(2) 0.6660(2) 0.0360(5) Uani 1 d . . N1 N 0.5788(2) 0.4270(2) 0.6910(2) 0.0440(5) Uani 1 d . . S2 S 0.38157(6) 0.45381(7) 0.84153(5) 0.0586(2) Uani 1 d . . C2 C 0.3200(2) 0.3236(2) 0.8256(2) 0.0366(5) Uani 1 d . . N2 N 0.2785(2) 0.2317(2) 0.81594(15) 0.0491(6) Uani 1 d . . N3 N 0.1854(2) 0.4381(2) 0.59513(15) 0.0476(5) Uani 1 d . . C3 C 0.1471(2) 0.4929(3) 0.5218(2) 0.0657(9) Uani 1 d . . H3 H 0.1623(2) 0.5757(3) 0.5182(2) 0.079 Uiso 1 calc R . C4 C 0.0863(3) 0.4354(4) 0.4503(2) 0.0762(10) Uani 1 d . . H4 H 0.0609(3) 0.4778(4) 0.3995(2) 0.091 Uiso 1 calc R . C5 C 0.0641(3) 0.3146(4) 0.4556(2) 0.0732(10) Uani 1 d . . H5 H 0.0234(3) 0.2723(4) 0.4081(2) 0.088 Uiso 1 calc R . C6 C 0.1016(3) 0.2572(3) 0.5301(2) 0.0705(10) Uani 1 d . . H6 H 0.0867(3) 0.1747(3) 0.5352(2) 0.085 Uiso 1 calc R . C7 C 0.1622(2) 0.3218(3) 0.5987(2) 0.0586(8) Uani 1 d . . H7 H 0.1881(2) 0.2812(3) 0.6502(2) 0.070 Uiso 1 calc R . N4 N 0.7438(2) 0.2577(2) 0.84270(14) 0.0421(5) Uani 1 d . . C8 C 0.7592(2) 0.3469(3) 0.8983(2) 0.0551(7) Uani 1 d . . H8 H 0.7288(2) 0.4230(3) 0.8806(2) 0.066 Uiso 1 calc R . C9 C 0.8183(3) 0.3324(4) 0.9814(2) 0.0778(11) Uani 1 d . . H9 H 0.8277(3) 0.3975(4) 1.0191(2) 0.093 Uiso 1 calc R . C10 C 0.8630(3) 0.2218(4) 1.0078(2) 0.0758(10) Uani 1 d . . H10 H 0.9038(3) 0.2101(4) 1.0638(2) 0.091 Uiso 1 calc R . C11 C 0.8477(2) 0.1297(3) 0.9523(2) 0.0641(9) Uani 1 d . . H11 H 0.8773(2) 0.0529(3) 0.9690(2) 0.077 Uiso 1 calc R . C12 C 0.7882(2) 0.1504(3) 0.8709(2) 0.0544(7) Uani 1 d . . H12 H 0.7779(2) 0.0858(3) 0.8327(2) 0.065 Uiso 1 calc R . N5 N 0.74295(15) 0.2367(2) 0.64810(13) 0.0391(5) Uani 1 d . . C13 C 0.7017(2) 0.2275(3) 0.5654(2) 0.0537(7) Uani 1 d . . H13 H 0.6341(2) 0.2488(3) 0.5399(2) 0.064 Uiso 1 calc R . C14 C 0.7522(2) 0.1888(3) 0.5155(2) 0.0628(9) Uani 1 d . . H14 H 0.7196(2) 0.1836(3) 0.4575(2) 0.075 Uiso 1 calc R . C15 C 0.8504(3) 0.1576(3) 0.5510(2) 0.0627(8) Uani 1 d . . H15 H 0.8865(3) 0.1303(3) 0.5181(2) 0.075 Uiso 1 calc R . C16 C 0.8949(2) 0.1671(3) 0.6355(2) 0.0639(9) Uani 1 d . . H16 H 0.9626(2) 0.1473(3) 0.6617(2) 0.077 Uiso 1 calc R . C17 C 0.8390(2) 0.2063(3) 0.6817(2) 0.0513(7) Uani 1 d . . H17 H 0.8702(2) 0.2119(3) 0.7399(2) 0.062 Uiso 1 calc R . N6 N 0.5549(2) 0.1376(2) 0.69718(15) 0.0436(5) Uani 1 d . . C18 C 0.4770(2) 0.1477(3) 0.7219(2) 0.0484(7) Uani 1 d . . H18 H 0.4636(2) 0.2237(3) 0.7411(2) 0.058 Uiso 1 calc R . C19 C 0.4151(2) 0.0505(3) 0.7202(2) 0.0631(9) Uani 1 d . . H19 H 0.3611(2) 0.0608(3) 0.7386(2) 0.076 Uiso 1 calc R . C20 C 0.4322(2) -0.0600(3) 0.6920(2) 0.0627(9) Uani 1 d . . H20 H 0.3914(2) -0.1274(3) 0.6916(2) 0.075 Uiso 1 calc R . C21 C 0.5107(3) -0.0710(3) 0.6640(3) 0.0702(10) Uani 1 d . . H21 H 0.5238(3) -0.1455(3) 0.6426(3) 0.084 Uiso 1 calc R . C22 C 0.5692(2) 0.0294(3) 0.6681(2) 0.0621(9) Uani 1 d . . H22 H 0.6230(2) 0.0212(3) 0.6492(2) 0.075 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04160(12) 0.03892(11) 0.05022(13) -0.00091(9) 0.01383(9) -0.00005(9) Cu1 0.0385(2) 0.0390(2) 0.0549(2) 0.0047(2) 0.01598(15) 0.00761(14) S1 0.0365(3) 0.0357(3) 0.0523(4) 0.0089(3) 0.0138(3) 0.0051(3) C1 0.0342(12) 0.0310(12) 0.0417(14) -0.0034(11) 0.0121(11) -0.0062(11) N1 0.0397(12) 0.0356(11) 0.0559(14) 0.0042(10) 0.0159(11) 0.0046(10) S2 0.0660(5) 0.0433(4) 0.0508(4) 0.0066(3) 0.0012(4) -0.0194(4) C2 0.0368(13) 0.0377(13) 0.0360(13) 0.0030(11) 0.0138(10) 0.0029(11) N2 0.0555(14) 0.0399(12) 0.0523(14) 0.0013(11) 0.0193(12) -0.0084(11) N3 0.0441(12) 0.0472(13) 0.0476(14) -0.0045(11) 0.0112(11) -0.0080(11) C3 0.066(2) 0.058(2) 0.061(2) 0.007(2) 0.007(2) -0.010(2) C4 0.069(2) 0.090(3) 0.053(2) 0.006(2) 0.002(2) -0.011(2) C5 0.058(2) 0.097(3) 0.055(2) -0.021(2) 0.009(2) -0.028(2) C6 0.077(2) 0.062(2) 0.068(2) -0.015(2) 0.019(2) -0.032(2) C7 0.065(2) 0.057(2) 0.049(2) 0.0002(15) 0.0142(15) -0.017(2) N4 0.0425(12) 0.0428(12) 0.0438(12) 0.0055(10) 0.0189(10) 0.0048(10) C8 0.066(2) 0.044(2) 0.060(2) 0.0014(14) 0.028(2) -0.0026(14) C9 0.103(3) 0.070(2) 0.052(2) -0.013(2) 0.016(2) -0.013(2) C10 0.080(2) 0.088(3) 0.049(2) 0.016(2) 0.009(2) 0.002(2) C11 0.066(2) 0.070(2) 0.056(2) 0.021(2) 0.021(2) 0.020(2) C12 0.060(2) 0.051(2) 0.053(2) 0.0082(14) 0.0213(15) 0.0160(14) N5 0.0348(11) 0.0432(12) 0.0376(11) 0.0068(10) 0.0108(9) 0.0055(9) C13 0.0381(14) 0.077(2) 0.041(2) 0.0155(15) 0.0080(12) 0.0056(14) C14 0.063(2) 0.089(2) 0.0327(14) 0.005(2) 0.0127(14) -0.002(2) C15 0.073(2) 0.075(2) 0.052(2) 0.007(2) 0.036(2) 0.012(2) C16 0.042(2) 0.097(3) 0.055(2) 0.009(2) 0.0194(14) 0.023(2) C17 0.0368(14) 0.074(2) 0.0377(14) 0.0018(14) 0.0063(11) 0.0115(14) N6 0.0379(11) 0.0369(11) 0.0568(14) -0.0008(10) 0.0178(10) 0.0016(9) C18 0.0443(15) 0.057(2) 0.046(2) -0.0079(14) 0.0183(12) -0.0003(13) C19 0.048(2) 0.086(2) 0.061(2) -0.011(2) 0.0261(15) -0.016(2) C20 0.055(2) 0.064(2) 0.065(2) -0.001(2) 0.016(2) -0.025(2) C21 0.068(2) 0.039(2) 0.107(3) -0.008(2) 0.036(2) -0.007(2) C22 0.054(2) 0.040(2) 0.104(3) -0.006(2) 0.042(2) 0.0003(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.326(2) 2_556 ? Ag1 N3 2.352(2) . ? Ag1 S2 2.5066(8) . ? Ag1 S1 2.5821(7) . ? Cu1 N1 1.932(2) . ? Cu1 N5 2.049(2) . ? Cu1 N4 2.054(2) . ? Cu1 N6 2.101(2) . ? S1 C1 1.650(3) . ? C1 N1 1.150(3) . ? S2 C2 1.648(3) . ? C2 N2 1.151(3) . ? N2 Ag1 2.326(2) 2_546 ? N3 C7 1.324(4) . ? N3 C3 1.325(4) . ? C3 C4 1.379(5) . ? C4 C5 1.372(5) . ? C5 C6 1.353(5) . ? C6 C7 1.386(4) . ? N4 C8 1.329(4) . ? N4 C12 1.342(4) . ? C8 C9 1.385(5) . ? C9 C10 1.371(5) . ? C10 C11 1.351(5) . ? C11 C12 1.373(4) . ? N5 C17 1.332(3) . ? N5 C13 1.333(3) . ? C13 C14 1.368(4) . ? C14 C15 1.364(5) . ? C15 C16 1.364(4) . ? C16 C17 1.380(4) . ? N6 C22 1.330(4) . ? N6 C18 1.332(3) . ? C18 C19 1.379(4) . ? C19 C20 1.359(5) . ? C20 C21 1.373(5) . ? C21 C22 1.370(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N3 97.58(8) 2_556 . ? N2 Ag1 S2 119.55(6) 2_556 . ? N3 Ag1 S2 118.22(6) . . ? N2 Ag1 S1 99.03(6) 2_556 . ? N3 Ag1 S1 103.14(6) . . ? S2 Ag1 S1 115.87(3) . . ? N1 Cu1 N5 117.98(9) . . ? N1 Cu1 N4 116.16(10) . . ? N5 Cu1 N4 109.02(8) . . ? N1 Cu1 N6 104.75(9) . . ? N5 Cu1 N6 104.35(9) . . ? N4 Cu1 N6 102.53(9) . . ? C1 S1 Ag1 100.24(9) . . ? N1 C1 S1 178.3(2) . . ? C1 N1 Cu1 167.9(2) . . ? C2 S2 Ag1 100.31(9) . . ? N2 C2 S2 178.5(2) . . ? C2 N2 Ag1 177.8(2) . 2_546 ? C7 N3 C3 117.0(3) . . ? C7 N3 Ag1 126.2(2) . . ? C3 N3 Ag1 116.0(2) . . ? N3 C3 C4 123.8(3) . . ? C5 C4 C3 118.1(4) . . ? C6 C5 C4 119.1(3) . . ? C5 C6 C7 119.0(3) . . ? N3 C7 C6 123.0(3) . . ? C8 N4 C12 116.6(3) . . ? C8 N4 Cu1 122.6(2) . . ? C12 N4 Cu1 120.7(2) . . ? N4 C8 C9 122.6(3) . . ? C10 C9 C8 119.1(3) . . ? C11 C10 C9 119.2(3) . . ? C10 C11 C12 118.7(3) . . ? N4 C12 C11 123.8(3) . . ? C17 N5 C13 116.3(2) . . ? C17 N5 Cu1 122.4(2) . . ? C13 N5 Cu1 121.1(2) . . ? N5 C13 C14 123.7(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 118.5(3) . . ? C15 C16 C17 119.0(3) . . ? N5 C17 C16 123.3(3) . . ? C22 N6 C18 116.8(2) . . ? C22 N6 Cu1 122.6(2) . . ? C18 N6 Cu1 120.1(2) . . ? N6 C18 C19 122.3(3) . . ? C20 C19 C18 120.0(3) . . ? C19 C20 C21 118.4(3) . . ? C22 C21 C20 118.2(3) . . ? N6 C22 C21 124.2(3) . . ? _refine_diff_density_max .298 _refine_diff_density_min -.384 _refine_diff_density_rms .053 #=END data_ag2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [AgCu(SCN)2(NC5H5)3] _chemical_formula_analytical ? _chemical_formula_sum 'C17 H15 Ag Cu N5 S2' _chemical_formula_weight 524.87 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' '-x+1/2, -y+1/2, z+1' 'x+1/2, y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' '-x+1, -y, z+1' 'x+1/2, y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' '-x+1, -y+1/2, z+1/2' _cell_length_a 52.305(4) _cell_length_b 12.088(1) _cell_length_c 12.785(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8083.5(14) _cell_formula_units_Z 16 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 3 _cell_measurement_theta_max 12.5 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method ? _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 2.238 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '<2%' _diffrn_reflns_number 4195 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3580 _reflns_number_observed 2925 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL92 _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0206P)^2^+15.7407P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 3567 _refine_ls_number_parameters 235 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_obs 0.0349 _refine_ls_wR_factor_all 0.0739 _refine_ls_wR_factor_obs 0.0594 _refine_ls_goodness_of_fit_all 1.153 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.179 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.103042(10) 0.38759(4) 0.19784(4) 0.04491(14) Uani 1 d . . Cu1 Cu 0.19627(2) 0.54944(7) 0.03850(6) 0.0443(2) Uani 1 d . . S1 S 0.12669(3) 0.5583(2) 0.27899(14) 0.0485(5) Uani 1 d . . C1 C 0.15200(11) 0.5603(5) 0.2007(5) 0.0362(14) Uani 1 d . . N1 N 0.16913(11) 0.5637(5) 0.1446(4) 0.0442(14) Uani 1 d . . S2 S 0.05549(4) 0.4266(2) 0.1691(2) 0.0549(5) Uani 1 d . . C2 C 0.05526(12) 0.5585(6) 0.2035(5) 0.040(2) Uani 1 d . . N2 N 0.05481(12) 0.6502(5) 0.2239(4) 0.051(2) Uani 1 d . . N3 N 0.10292(11) 0.2604(5) 0.3331(4) 0.0448(14) Uani 1 d . . C3 C 0.0864(2) 0.1770(7) 0.3329(6) 0.063(2) Uani 1 d . . H3 H 0.0758(2) 0.1676(7) 0.2741(6) 0.076 Uiso 1 calc R . C4 C 0.0840(2) 0.1031(7) 0.4153(8) 0.076(3) Uani 1 d . . H4 H 0.0721(2) 0.0451(7) 0.4130(8) 0.092 Uiso 1 calc R . C5 C 0.0996(2) 0.1175(8) 0.4997(8) 0.081(3) Uani 1 d . . H5 H 0.0985(2) 0.0695(8) 0.5574(8) 0.097 Uiso 1 calc R . C6 C 0.1166(2) 0.2011(8) 0.4996(6) 0.080(3) Uani 1 d . . H6 H 0.1275(2) 0.2115(8) 0.5573(6) 0.096 Uiso 1 calc R . C7 C 0.1181(2) 0.2710(6) 0.4159(6) 0.060(2) Uani 1 d . . H7 H 0.1302(2) 0.3284(6) 0.4169(6) 0.072 Uiso 1 calc R . N4 N 0.19627(10) 0.6742(5) -0.0701(5) 0.0456(14) Uani 1 d . . C8 C 0.1799(2) 0.6746(7) -0.1482(7) 0.067(2) Uani 1 d . . H8 H 0.1675(2) 0.6184(7) -0.1496(7) 0.080 Uiso 1 calc R . C9 C 0.1795(2) 0.7510(10) -0.2281(8) 0.095(3) Uani 1 d . . H9 H 0.1676(2) 0.7458(10) -0.2828(8) 0.114 Uiso 1 calc R . C10 C 0.1970(2) 0.8342(10) -0.2251(9) 0.100(4) Uani 1 d . . H10 H 0.1971(2) 0.8892(10) -0.2770(9) 0.120 Uiso 1 calc R . C11 C 0.2139(2) 0.8362(9) -0.1464(10) 0.103(4) Uani 1 d . . H11 H 0.2263(2) 0.8924(9) -0.1436(10) 0.123 Uiso 1 calc R . C12 C 0.2132(2) 0.7555(7) -0.0693(8) 0.073(3) Uani 1 d . . H12 H 0.2252(2) 0.7587(7) -0.0145(8) 0.088 Uiso 1 calc R . N5 N 0.23167(10) 0.5484(5) 0.1145(4) 0.0426(14) Uani 1 d . . C13 C 0.23508(12) 0.6071(6) 0.2022(7) 0.049(2) Uani 1 d . . H13 H 0.22224(12) 0.6572(6) 0.2222(7) 0.059 Uiso 1 calc R . C14 C 0.25629(14) 0.5980(6) 0.2642(5) 0.050(2) Uani 1 d . . H14 H 0.25781(14) 0.6424(6) 0.3242(5) 0.061 Uiso 1 calc R . C15 C 0.2751(2) 0.5257(8) 0.2398(6) 0.066(2) Uani 1 d . . H15 H 0.2896(2) 0.5176(8) 0.2822(6) 0.079 Uiso 1 calc R . C16 C 0.27186(15) 0.4638(8) 0.1492(7) 0.078(3) Uani 1 d . . H16 H 0.28453(15) 0.4132(8) 0.1285(7) 0.094 Uiso 1 calc R . C17 C 0.25015(15) 0.4766(7) 0.0898(6) 0.062(2) Uani 1 d . . H17 H 0.24821(15) 0.4330(7) 0.0294(6) 0.074 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0501(3) 0.0476(3) 0.0370(2) 0.0103(3) -0.0011(2) -0.0003(3) Cu1 0.0429(5) 0.0484(5) 0.0417(5) 0.0063(4) 0.0022(4) -0.0046(4) S1 0.0440(10) 0.0615(12) 0.0400(9) -0.0110(9) 0.0082(8) -0.0158(9) C1 0.039(4) 0.035(3) 0.035(3) 0.004(3) -0.005(3) 0.000(3) N1 0.042(3) 0.046(3) 0.045(3) 0.004(3) 0.000(3) 0.004(3) S2 0.0434(11) 0.0514(11) 0.0698(13) -0.0052(10) -0.0054(9) -0.0023(9) C2 0.032(4) 0.052(4) 0.035(3) 0.007(4) -0.004(3) -0.001(3) N2 0.053(4) 0.056(4) 0.043(3) 0.001(3) -0.007(3) 0.006(3) N3 0.051(4) 0.047(3) 0.037(3) 0.011(3) -0.002(3) -0.005(3) C3 0.064(6) 0.054(5) 0.070(6) 0.017(4) -0.010(4) -0.004(4) C4 0.068(6) 0.049(5) 0.111(8) 0.034(5) 0.016(6) -0.004(5) C5 0.098(8) 0.075(7) 0.071(6) 0.048(6) 0.033(6) 0.029(6) C6 0.104(8) 0.083(7) 0.053(5) 0.027(5) -0.005(5) 0.010(6) C7 0.065(5) 0.061(5) 0.054(5) 0.016(4) -0.018(4) -0.006(4) N4 0.044(3) 0.048(3) 0.045(4) 0.006(3) 0.009(3) -0.001(3) C8 0.065(6) 0.076(6) 0.058(5) 0.012(5) -0.003(4) -0.004(5) C9 0.082(7) 0.123(9) 0.080(7) 0.045(7) -0.020(6) 0.021(7) C10 0.106(9) 0.098(8) 0.095(8) 0.067(7) 0.030(7) 0.028(7) C11 0.095(8) 0.084(8) 0.129(10) 0.047(8) 0.015(8) -0.027(7) C12 0.064(5) 0.072(6) 0.083(6) 0.017(6) -0.009(5) -0.019(5) N5 0.038(3) 0.046(3) 0.044(3) -0.011(3) 0.003(3) -0.006(3) C13 0.046(4) 0.050(4) 0.051(4) -0.004(4) 0.005(4) 0.004(4) C14 0.053(5) 0.053(5) 0.045(4) -0.006(4) -0.005(4) -0.001(4) C15 0.057(5) 0.085(7) 0.055(5) 0.001(5) -0.013(4) -0.001(5) C16 0.043(5) 0.096(8) 0.095(7) -0.014(6) -0.006(5) 0.026(5) C17 0.044(4) 0.087(6) 0.055(4) -0.024(5) -0.001(4) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.314(5) . ? Ag1 S2 2.558(2) . ? Ag1 S1 2.589(2) 6_544 ? Ag1 S1 2.620(2) . ? Cu1 N1 1.971(6) . ? Cu1 N2 1.985(7) 6_544 ? Cu1 N4 2.050(6) . ? Cu1 N5 2.091(5) . ? S1 C1 1.659(7) . ? S1 Ag1 2.589(2) 2 ? C1 N1 1.149(8) . ? S2 C2 1.653(8) . ? C2 N2 1.140(8) . ? N2 Cu1 1.985(7) 2 ? N3 C3 1.327(9) . ? N3 C7 1.330(8) . ? C3 C4 1.387(11) . ? C4 C5 1.364(12) . ? C5 C6 1.345(13) . ? C6 C7 1.365(10) . ? N4 C8 1.314(10) . ? N4 C12 1.323(9) . ? C8 C9 1.377(12) . ? C9 C10 1.358(14) . ? C10 C11 1.342(15) . ? C11 C12 1.388(12) . ? N5 C17 1.338(9) . ? N5 C13 1.338(9) . ? C13 C14 1.368(9) . ? C14 C15 1.351(11) . ? C15 C16 1.390(11) . ? C16 C17 1.375(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 S2 103.1(2) . . ? N3 Ag1 S1 112.2(2) . 6_544 ? S2 Ag1 S1 110.28(6) . 6_544 ? N3 Ag1 S1 103.2(2) . . ? S2 Ag1 S1 111.75(7) . . ? S1 Ag1 S1 115.37(5) 6_544 . ? N1 Cu1 N2 110.2(2) . 6_544 ? N1 Cu1 N4 113.7(2) . . ? N2 Cu1 N4 112.8(2) 6_544 . ? N1 Cu1 N5 108.6(2) . . ? N2 Cu1 N5 102.3(2) 6_544 . ? N4 Cu1 N5 108.6(2) . . ? C1 S1 Ag1 99.8(2) . 2 ? C1 S1 Ag1 98.6(2) . . ? Ag1 S1 Ag1 144.58(9) 2 . ? N1 C1 S1 178.0(6) . . ? C1 N1 Cu1 171.3(6) . . ? C2 S2 Ag1 98.4(2) . . ? N2 C2 S2 177.7(7) . . ? C2 N2 Cu1 168.7(6) . 2 ? C3 N3 C7 117.6(6) . . ? C3 N3 Ag1 120.3(5) . . ? C7 N3 Ag1 122.0(5) . . ? N3 C3 C4 123.1(8) . . ? C5 C4 C3 117.7(8) . . ? C6 C5 C4 119.3(8) . . ? C5 C6 C7 120.3(9) . . ? N3 C7 C6 122.0(8) . . ? C8 N4 C12 116.0(7) . . ? C8 N4 Cu1 121.2(5) . . ? C12 N4 Cu1 122.8(6) . . ? N4 C8 C9 125.2(9) . . ? C10 C9 C8 117.7(9) . . ? C11 C10 C9 118.6(9) . . ? C10 C11 C12 120.1(10) . . ? N4 C12 C11 122.4(9) . . ? C17 N5 C13 116.5(6) . . ? C17 N5 Cu1 122.3(5) . . ? C13 N5 Cu1 120.3(4) . . ? N5 C13 C14 123.4(7) . . ? C15 C14 C13 120.6(7) . . ? C14 C15 C16 116.9(8) . . ? C17 C16 C15 120.0(8) . . ? N5 C17 C16 122.7(7) . . ? _refine_diff_density_max .437 _refine_diff_density_min -.356 _refine_diff_density_rms .081 #=END data_ag3x _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Ag2Cu(SCN)3(NC5H5)3] _chemical_formula_analytical ? _chemical_formula_sum 'C18 H15 Ag2 Cu N6 S3' _chemical_formula_weight 690.82 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.9808(6) _cell_length_b 15.0009(10) _cell_length_c 8.4219(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.288(6) _cell_angle_gamma 90.00 _cell_volume 1133.69(13) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.024 _exptl_crystal_density_method ? _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 2.934 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'theta/omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '<2%' _diffrn_reflns_number 5650 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.96 _reflns_number_total 5448 _reflns_number_observed 4403 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE XRED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SCHAKAL92 _computing_publication_material ? _refine_special_details ; The Ag2Cu(SCN)3 framework can be described in space group Am ( Cm, No. 8), but the orientation of the pyridine rings destroys this symmetry. Refinement without disorder is possible in space group Pc. The reflections hkl with k+l=2n+1 are weak, but not systematically absent. Refinement on F^2^ for ALL reflections except for 18 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0472P)^2^+0.8744P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 5430 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_obs 0.0356 _refine_ls_wR_factor_all 0.1082 _refine_ls_wR_factor_obs 0.0861 _refine_ls_goodness_of_fit_all 1.152 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.187 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.64075(4) 0.07903(3) 0.37506(5) 0.0457(2) Uani 1 d . . Ag2 Ag 0.65911(4) 0.41470(3) 0.37508(5) 0.0465(2) Uani 1 d . . Cu1 Cu 0.32533(10) 0.25206(5) 0.86025(10) 0.0418(2) Uani 1 d . . S1 S 0.5369(2) -0.00296(10) 0.6140(2) 0.0430(4) Uani 1 d . . C1 C 0.4523(6) 0.0835(4) 0.6955(7) 0.0383(13) Uani 1 d . . N1 N 0.3887(7) 0.1414(4) 0.7508(7) 0.0482(13) Uani 1 d . . S2 S 0.5692(3) 0.24926(10) 0.3747(2) 0.0509(4) Uani 1 d . . C2 C 0.4762(7) 0.2507(4) 0.2001(8) 0.0391(12) Uani 1 d . . N2 N 0.4091(7) 0.2505(3) 0.0820(7) 0.0465(12) Uani 1 d . . S3 S 0.5661(2) 0.49909(11) 0.6194(2) 0.0507(5) Uani 1 d . . C3 C 0.4797(6) 0.4143(4) 0.7046(7) 0.0369(12) Uani 1 d . . N3 N 0.4151(6) 0.3568(4) 0.7592(7) 0.0458(12) Uani 1 d . . N4 N 0.8976(6) 0.0821(3) 0.3666(7) 0.0430(12) Uani 1 d . . C5 C 0.9611(8) 0.1430(5) 0.2772(10) 0.055(2) Uani 1 d . . H5 H 0.9011(8) 0.1848(5) 0.2240(10) 0.066 Uiso 1 calc R . C6 C 1.1127(8) 0.1464(6) 0.2604(11) 0.062(2) Uani 1 d . . H6 H 1.1539(8) 0.1895(6) 0.1960(11) 0.074 Uiso 1 calc R . C7 C 1.2019(9) 0.0861(6) 0.3391(11) 0.063(2) Uani 1 d . . H7 H 1.3046(9) 0.0872(6) 0.3284(11) 0.076 Uiso 1 calc R . C8 C 1.1384(9) 0.0241(6) 0.4338(11) 0.064(2) Uani 1 d . . H8 H 1.1969(9) -0.0170(6) 0.4907(11) 0.076 Uiso 1 calc R . C9 C 0.9849(8) 0.0238(5) 0.4431(10) 0.057(2) Uani 1 d . . H9 H 0.9412(8) -0.0192(5) 0.5057(10) 0.068 Uiso 1 calc R . N5 N 0.9159(6) 0.4129(3) 0.3650(7) 0.0410(12) Uani 1 d . . C10 C 0.9979(8) 0.3559(5) 0.4492(10) 0.058(2) Uani 1 d . . H10 H 0.9497(8) 0.3156(5) 0.5135(10) 0.069 Uiso 1 calc R . C11 C 1.1501(9) 0.3526(6) 0.4475(12) 0.066(2) Uani 1 d . . H11 H 1.2036(9) 0.3116(6) 0.5096(12) 0.079 Uiso 1 calc R . C12 C 1.2214(8) 0.4110(7) 0.3526(12) 0.069(2) Uani 1 d . . H12 H 1.3247(8) 0.4104(7) 0.3486(12) 0.083 Uiso 1 calc R . C13 C 1.1387(9) 0.4704(6) 0.2633(12) 0.072(3) Uani 1 d . . H13 H 1.1845(9) 0.5105(6) 0.1966(12) 0.086 Uiso 1 calc R . C14 C 0.9871(8) 0.4697(5) 0.2740(10) 0.057(2) Uani 1 d . . H14 H 0.9312(8) 0.5110(5) 0.2146(10) 0.068 Uiso 1 calc R . N6 N 0.0936(6) 0.2516(3) 0.8534(7) 0.0393(12) Uani 1 d . . C15 C 0.0142(7) 0.1905(5) 0.7719(10) 0.052(2) Uani 1 d . . H15 H 0.0649(7) 0.1481(5) 0.7143(10) 0.063 Uiso 1 calc R . C16 C -0.1382(9) 0.1873(6) 0.7689(12) 0.069(2) Uani 1 d . . H16 H -0.1881(9) 0.1430(6) 0.7108(12) 0.083 Uiso 1 calc R . C17 C -0.2176(10) 0.2486(6) 0.8504(15) 0.074(3) Uani 1 d . . H17 H -0.3212(10) 0.2479(6) 0.8485(15) 0.089 Uiso 1 calc R . C18 C -0.1372(11) 0.3108(7) 0.9348(14) 0.086(3) Uani 1 d . . H18 H -0.1866(11) 0.3533(7) 0.9934(14) 0.103 Uiso 1 calc R . C19 C 0.0145(8) 0.3115(6) 0.9345(11) 0.062(2) Uani 1 d . . H19 H 0.0657(8) 0.3553(6) 0.9928(11) 0.075 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0371(5) 0.0496(3) 0.0503(4) 0.0009(3) 0.0034(3) -0.0036(2) Ag2 0.0381(5) 0.0477(3) 0.0541(4) 0.0003(3) 0.0078(4) -0.0008(2) Cu1 0.0408(4) 0.0401(4) 0.0444(4) 0.0014(4) 0.0011(3) -0.0034(3) S1 0.0584(10) 0.0361(7) 0.0351(9) 0.0049(6) 0.0076(7) 0.0083(6) C1 0.038(3) 0.036(3) 0.041(3) 0.003(2) 0.003(2) -0.004(2) N1 0.059(3) 0.040(3) 0.047(3) 0.000(2) 0.009(3) 0.006(2) S2 0.0731(12) 0.0301(6) 0.0478(8) 0.0003(7) -0.0182(8) -0.0032(6) C2 0.042(3) 0.031(3) 0.044(3) 0.002(3) 0.006(3) -0.004(2) N2 0.054(3) 0.046(3) 0.040(3) 0.004(3) -0.003(2) -0.002(2) S3 0.0754(13) 0.0393(8) 0.0386(10) -0.0070(7) 0.0171(9) -0.0197(8) C3 0.032(2) 0.042(3) 0.036(3) -0.006(2) 0.002(2) 0.001(2) N3 0.043(3) 0.040(3) 0.055(3) 0.004(2) 0.010(2) -0.006(2) N4 0.035(2) 0.047(3) 0.047(3) -0.002(2) 0.004(2) -0.003(2) C5 0.048(4) 0.048(4) 0.071(5) 0.005(3) 0.008(3) -0.002(3) C6 0.046(4) 0.072(5) 0.068(5) 0.003(4) 0.016(4) -0.012(4) C7 0.046(4) 0.083(6) 0.062(5) -0.020(4) 0.012(3) -0.006(4) C8 0.045(4) 0.077(5) 0.068(5) -0.004(4) -0.007(4) 0.014(4) C9 0.051(4) 0.059(4) 0.061(5) 0.008(4) 0.007(3) 0.005(3) N5 0.033(2) 0.043(3) 0.048(3) -0.001(2) 0.007(2) 0.000(2) C10 0.050(4) 0.056(4) 0.067(5) 0.013(4) 0.002(3) -0.003(3) C11 0.054(5) 0.064(5) 0.080(6) -0.003(4) -0.017(4) 0.010(4) C12 0.030(3) 0.093(6) 0.084(7) -0.019(5) 0.001(3) -0.006(4) C13 0.047(4) 0.088(6) 0.080(6) 0.018(5) 0.005(4) -0.016(4) C14 0.049(4) 0.055(4) 0.067(5) 0.012(4) 0.001(3) -0.008(3) N6 0.032(2) 0.037(3) 0.049(3) 0.004(2) 0.003(2) 0.004(2) C15 0.045(3) 0.051(4) 0.061(4) -0.012(3) -0.002(3) -0.004(3) C16 0.051(4) 0.076(5) 0.079(6) -0.011(5) -0.007(4) -0.013(4) C17 0.036(4) 0.097(7) 0.090(7) 0.013(5) 0.001(4) 0.002(4) C18 0.072(6) 0.077(6) 0.111(9) -0.021(6) 0.025(5) 0.019(5) C19 0.050(4) 0.059(5) 0.078(6) -0.020(4) 0.010(4) 0.003(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 Ag1 N4 2.311(5) . ? Ag1 S1 2.566(2) . ? Ag1 S1 2.615(2) 2_554 ? Ag1 S2 2.633(2) . ? Ag2 N5 2.312(5) . ? Ag2 S3 2.583(2) . ? Ag2 S2 2.610(2) . ? Ag2 S3 2.620(2) 2_564 ? Cu1 N3 1.974(5) . ? Cu1 N2 1.985(6) 1_556 ? Cu1 N1 1.992(5) . ? Cu1 N6 2.080(6) . ? S1 C1 1.665(6) . ? S1 Ag1 2.615(2) 2 ? C1 N1 1.149(8) . ? S2 C2 1.662(7) . ? C2 N2 1.143(9) . ? N2 Cu1 1.985(6) 1_554 ? S3 C3 1.667(6) . ? S3 Ag2 2.620(2) 2_565 ? C3 N3 1.146(8) . ? N4 C9 1.325(9) . ? N4 C5 1.327(9) . ? C5 C6 1.375(10) . ? C6 C7 1.363(12) . ? C7 C8 1.366(13) . ? C8 C9 1.383(10) . ? N5 C10 1.318(9) . ? N5 C14 1.327(9) . ? C10 C11 1.368(10) . ? C11 C12 1.362(13) . ? C12 C13 1.367(13) . ? C13 C14 1.368(10) . ? N6 C15 1.334(9) . ? N6 C19 1.348(9) . ? C15 C16 1.369(10) . ? C16 C17 1.366(13) . ? C17 C18 1.361(14) . ? C18 C19 1.363(12) . ? 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 N4 Ag1 S1 115.4(2) . . ? N4 Ag1 S1 107.8(2) . 2_554 ? S1 Ag1 S1 108.76(4) . 2_554 ? N4 Ag1 S2 102.96(14) . . ? S1 Ag1 S2 111.68(6) . . ? S1 Ag1 S2 110.09(5) 2_554 . ? N5 Ag2 S3 113.0(2) . . ? N5 Ag2 S2 107.34(14) . . ? S3 Ag2 S2 110.92(6) . . ? N5 Ag2 S3 105.1(2) . 2_564 ? S3 Ag2 S3 108.07(4) . 2_564 ? S2 Ag2 S3 112.34(6) . 2_564 ? N3 Cu1 N2 105.6(2) . 1_556 ? N3 Cu1 N1 109.5(2) . . ? N2 Cu1 N1 108.7(2) 1_556 . ? N3 Cu1 N6 114.6(2) . . ? N2 Cu1 N6 111.6(3) 1_556 . ? N1 Cu1 N6 106.8(2) . . ? C1 S1 Ag1 97.8(2) . . ? C1 S1 Ag1 98.4(2) . 2 ? Ag1 S1 Ag1 137.73(7) . 2 ? N1 C1 S1 177.3(6) . . ? C1 N1 Cu1 166.8(6) . . ? C2 S2 Ag2 97.6(2) . . ? C2 S2 Ag1 97.3(2) . . ? Ag2 S2 Ag1 147.87(10) . . ? N2 C2 S2 178.1(6) . . ? C2 N2 Cu1 170.4(6) . 1_554 ? C3 S3 Ag2 98.1(2) . . ? C3 S3 Ag2 99.3(2) . 2_565 ? Ag2 S3 Ag2 142.57(9) . 2_565 ? N3 C3 S3 177.2(6) . . ? C3 N3 Cu1 173.7(5) . . ? C9 N4 C5 118.1(6) . . ? C9 N4 Ag1 122.9(5) . . ? C5 N4 Ag1 118.9(5) . . ? N4 C5 C6 122.3(7) . . ? C7 C6 C5 119.4(8) . . ? C6 C7 C8 119.0(8) . . ? C7 C8 C9 118.4(8) . . ? N4 C9 C8 122.8(7) . . ? C10 N5 C14 117.2(6) . . ? C10 N5 Ag2 121.6(5) . . ? C14 N5 Ag2 121.2(5) . . ? N5 C10 C11 123.6(7) . . ? C12 C11 C10 118.5(8) . . ? C11 C12 C13 119.0(7) . . ? C12 C13 C14 118.6(8) . . ? N5 C14 C13 123.1(7) . . ? C15 N6 C19 115.9(6) . . ? C15 N6 Cu1 122.0(5) . . ? C19 N6 Cu1 122.0(5) . . ? N6 C15 C16 123.2(7) . . ? C17 C16 C15 120.6(8) . . ? C18 C17 C16 116.5(8) . . ? C17 C18 C19 121.0(8) . . ? N6 C19 C18 122.8(8) . . ? _refine_diff_density_max 0.671 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.096 #=END