# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Craig MacKinnon' _publ_contact_author_email CRAIG.MACKINNON@LAKEHEADU.CA _publ_section_title ; 5,5'-Dicyano-2,2'-bithiophene and 3,3'-dicyanobiphenyl: off-axis rod-like ligands for silver(I) ; loop_ _publ_author_name 'Craig MacKinnon' 'Abdeljalil Assoud' 'Shawna L.M. Parent' 'Craig M Robertson' # Attachment 'B810479D_-_3AgBF4_tol__-_R.cif' data_cdm13_0m _database_code_depnum_ccdc_archive 'CCDC 692771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17.50 H16 Ag B F4 N2' _chemical_formula_weight 449.00 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/c 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 8.8779(14) _cell_length_b 14.465(2) _cell_length_c 13.422(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.114(3) _cell_angle_gamma 90.00 _cell_volume 1638.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6164 _exptl_absorpt_correction_T_max 0.8517 _exptl_absorpt_process_details 'APEX II' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18925 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 30.56 _reflns_number_total 5016 _reflns_number_gt 4475 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0356P)^2^+1.8329P] 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_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5016 _refine_ls_number_parameters 250 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.079 _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 Ag1 Ag 0.39423(3) 0.025797(12) 0.087112(19) 0.05377(10) Uani 1 1 d . . . B1 B 0.7538(3) 0.2295(2) 0.1789(2) 0.0433(6) Uani 1 1 d . . . F1 F 0.90222(18) 0.20891(13) 0.24302(17) 0.0664(5) Uani 1 1 d . A . F2 F 0.6729(2) 0.28122(14) 0.23116(17) 0.0672(5) Uani 1 1 d . A . F3 F 0.6731(2) 0.14594(17) 0.1490(2) 0.0848(7) Uani 1 1 d . A . F4A F 0.7775(13) 0.3164(10) 0.1171(8) 0.0785(12) Uani 0.287(8) 1 d PU A 1 F4B F 0.7624(5) 0.2664(4) 0.0889(3) 0.0785(12) Uani 0.713(8) 1 d PU A 2 N1 N 0.4980(2) -0.10637(12) 0.11314(16) 0.0356(4) Uani 1 1 d . . . N2 N 0.3192(2) -0.83543(12) 0.07039(16) 0.0358(4) Uani 1 1 d . . . C1 C 0.5286(2) -0.18300(14) 0.12452(16) 0.0301(4) Uani 1 1 d . . . C2 C 0.5679(2) -0.27926(13) 0.14083(15) 0.0278(3) Uani 1 1 d . . . C3 C 0.4465(2) -0.34426(13) 0.12187(16) 0.0279(3) Uani 1 1 d . . . H3A H 0.3390 -0.3250 0.0956 0.034 Uiso 1 1 calc R . . C4 C 0.4827(2) -0.43746(12) 0.14141(15) 0.0266(3) Uani 1 1 d . . . C5 C 0.6422(2) -0.46332(13) 0.17928(17) 0.0311(4) Uani 1 1 d . . . H5A H 0.6687 -0.5267 0.1933 0.037 Uiso 1 1 calc R . . C6 C 0.7623(2) -0.39829(14) 0.19679(18) 0.0341(4) Uani 1 1 d . . . H6A H 0.8698 -0.4176 0.2221 0.041 Uiso 1 1 calc R . . C7 C 0.7269(2) -0.30542(14) 0.17778(17) 0.0310(4) Uani 1 1 d . . . H7A H 0.8089 -0.2606 0.1896 0.037 Uiso 1 1 calc R . . C8 C 0.3539(2) -0.50691(13) 0.12406(15) 0.0264(3) Uani 1 1 d . . . C9 C 0.2053(3) -0.48304(14) 0.13177(18) 0.0341(4) Uani 1 1 d . . . H9A H 0.1854 -0.4208 0.1464 0.041 Uiso 1 1 calc R . . C10 C 0.0866(3) -0.54848(16) 0.1184(2) 0.0390(5) Uani 1 1 d . . . H10A H -0.0142 -0.5302 0.1224 0.047 Uiso 1 1 calc R . . C11 C 0.1133(3) -0.64025(15) 0.09937(18) 0.0355(4) Uani 1 1 d . . . H11A H 0.0326 -0.6855 0.0911 0.043 Uiso 1 1 calc R . . C12 C 0.2619(2) -0.66417(13) 0.09281(16) 0.0290(4) Uani 1 1 d . . . C13 C 0.3808(2) -0.59881(13) 0.10327(15) 0.0274(3) Uani 1 1 d . . . H13A H 0.4799 -0.6167 0.0963 0.033 Uiso 1 1 calc R . . C14 C 0.2942(2) -0.75954(14) 0.07879(17) 0.0312(4) Uani 1 1 d . . . C15 C 0.9150(3) 0.0545(2) 0.0245(2) 0.0479(6) Uani 1 1 d . . . C16 C 0.9075(6) -0.0005(5) 0.1086(5) 0.0507(12) Uani 0.50 1 d P . . C17 C 1.0056(4) 0.0876(3) -0.1281(3) 0.0670(9) Uani 1 1 d . . . C18 C 0.9223(6) 0.1074(4) -0.0595(5) 0.0531(14) Uani 0.50 1 d P . . C19 C 0.9955(6) 0.0329(4) -0.0419(4) 0.0455(11) Uani 0.50 1 d P . . 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 0.07215(17) 0.02168(10) 0.07232(17) 0.00675(8) 0.02949(12) 0.01324(8) B1 0.0270(10) 0.0561(17) 0.0464(14) 0.0079(12) 0.0108(10) 0.0065(10) F1 0.0330(7) 0.0512(10) 0.0959(14) -0.0038(9) -0.0079(8) 0.0088(7) F2 0.0588(10) 0.0646(12) 0.0897(14) 0.0026(10) 0.0398(10) 0.0147(9) F3 0.0438(9) 0.0898(16) 0.1154(18) -0.0324(14) 0.0168(10) -0.0154(10) F4A 0.0902(18) 0.090(3) 0.062(2) 0.028(2) 0.0341(16) -0.004(2) F4B 0.0902(18) 0.090(3) 0.062(2) 0.028(2) 0.0341(16) -0.004(2) N1 0.0391(9) 0.0212(8) 0.0464(10) 0.0006(7) 0.0132(8) 0.0016(6) N2 0.0360(9) 0.0225(8) 0.0484(10) -0.0013(7) 0.0123(8) -0.0019(6) C1 0.0321(9) 0.0227(8) 0.0356(9) -0.0007(7) 0.0105(7) 0.0009(7) C2 0.0327(9) 0.0184(7) 0.0321(9) -0.0005(6) 0.0096(7) 0.0030(6) C3 0.0296(8) 0.0197(8) 0.0331(9) -0.0001(7) 0.0076(7) 0.0040(6) C4 0.0300(8) 0.0182(7) 0.0308(9) -0.0011(6) 0.0084(7) 0.0026(6) C5 0.0326(9) 0.0202(8) 0.0384(10) -0.0003(7) 0.0078(8) 0.0051(7) C6 0.0283(9) 0.0265(9) 0.0448(11) -0.0008(8) 0.0077(8) 0.0048(7) C7 0.0309(9) 0.0240(8) 0.0375(10) -0.0020(7) 0.0099(7) -0.0004(7) C8 0.0304(8) 0.0196(7) 0.0293(8) -0.0004(6) 0.0097(7) 0.0027(6) C9 0.0364(10) 0.0243(9) 0.0444(11) -0.0033(8) 0.0163(9) 0.0046(7) C10 0.0336(10) 0.0334(10) 0.0545(13) -0.0031(9) 0.0204(9) 0.0034(8) C11 0.0346(10) 0.0286(9) 0.0455(11) -0.0008(8) 0.0158(8) -0.0024(8) C12 0.0351(9) 0.0203(8) 0.0321(9) 0.0003(7) 0.0111(7) 0.0008(7) C13 0.0306(8) 0.0201(8) 0.0319(9) 0.0001(6) 0.0101(7) 0.0027(6) C14 0.0330(9) 0.0236(9) 0.0374(10) -0.0010(7) 0.0114(8) -0.0034(7) C15 0.0359(11) 0.0434(13) 0.0572(15) -0.0123(11) 0.0040(10) -0.0043(10) C16 0.040(2) 0.057(3) 0.054(3) -0.020(3) 0.013(2) -0.013(2) C17 0.0667(19) 0.070(2) 0.0516(16) 0.0054(15) 0.0005(14) -0.0275(17) C18 0.038(2) 0.032(2) 0.074(4) -0.006(2) -0.004(2) 0.0025(18) C19 0.042(2) 0.043(3) 0.041(2) -0.0021(19) -0.0011(19) -0.016(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 N1 2.1037(18) . ? Ag1 N2 2.1048(18) 1_565 ? B1 F4B 1.344(4) . ? B1 F1 1.364(3) . ? B1 F2 1.372(3) . ? B1 F3 1.398(4) . ? B1 F4A 1.556(11) . ? N1 C1 1.140(3) . ? N2 C14 1.132(3) . ? N2 Ag1 2.1048(18) 1_545 ? C1 C2 1.436(3) . ? C2 C3 1.393(3) . ? C2 C7 1.395(3) . ? C3 C4 1.392(2) . ? C4 C5 1.399(3) . ? C4 C8 1.485(3) . ? C5 C6 1.386(3) . ? C6 C7 1.385(3) . ? C8 C13 1.394(3) . ? C8 C9 1.398(3) . ? C9 C10 1.387(3) . ? C10 C11 1.386(3) . ? C11 C12 1.393(3) . ? C12 C13 1.391(3) . ? C12 C14 1.433(3) . ? C15 C19 1.340(7) . ? C15 C18 1.380(7) . ? C15 C16 1.400(7) . ? C15 C19 1.473(6) 3_755 ? C16 C17 1.458(8) 3_755 ? C16 C19 1.498(8) 3_755 ? C17 C18 1.379(8) . ? C17 C19 1.427(6) . ? C17 C16 1.458(8) 3_755 ? C18 C19 1.242(7) . ? C19 C19 1.456(10) 3_755 ? C19 C15 1.473(6) 3_755 ? C19 C16 1.498(8) 3_755 ? 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 172.79(7) . 1_565 ? F4B B1 F1 109.9(3) . . ? F4B B1 F2 115.3(3) . . ? F1 B1 F2 110.6(3) . . ? F4B B1 F3 104.7(4) . . ? F1 B1 F3 107.5(2) . . ? F2 B1 F3 108.4(2) . . ? F4B B1 F4A 31.3(4) . . ? F1 B1 F4A 104.4(5) . . ? F2 B1 F4A 90.6(5) . . ? F3 B1 F4A 133.4(5) . . ? C1 N1 Ag1 168.37(18) . . ? C14 N2 Ag1 168.25(19) . 1_545 ? N1 C1 C2 179.0(2) . . ? C3 C2 C7 121.47(17) . . ? C3 C2 C1 119.30(17) . . ? C7 C2 C1 119.22(18) . . ? C4 C3 C2 119.93(17) . . ? C3 C4 C5 118.43(17) . . ? C3 C4 C8 120.27(17) . . ? C5 C4 C8 121.28(16) . . ? C6 C5 C4 121.25(18) . . ? C7 C6 C5 120.56(18) . . ? C6 C7 C2 118.36(18) . . ? C13 C8 C9 118.32(18) . . ? C13 C8 C4 120.34(17) . . ? C9 C8 C4 121.30(17) . . ? C10 C9 C8 121.26(19) . . ? C11 C10 C9 120.7(2) . . ? C10 C11 C12 117.98(19) . . ? C13 C12 C11 121.92(18) . . ? C13 C12 C14 119.36(18) . . ? C11 C12 C14 118.68(18) . . ? C12 C13 C8 119.76(18) . . ? N2 C14 C12 178.0(2) . . ? C19 C15 C18 54.3(3) . . ? C19 C15 C16 124.9(4) . . ? C18 C15 C16 179.0(4) . . ? C19 C15 C19 62.2(4) . 3_755 ? C18 C15 C19 116.5(4) . 3_755 ? C16 C15 C19 62.8(4) . 3_755 ? C15 C16 C17 118.7(4) . 3_755 ? C15 C16 C19 61.0(3) . 3_755 ? C17 C16 C19 57.7(3) 3_755 3_755 ? C18 C17 C19 52.5(4) . . ? C18 C17 C16 115.0(4) . 3_755 ? C19 C17 C16 62.5(4) . 3_755 ? C19 C18 C17 65.8(4) . . ? C19 C18 C15 61.2(4) . . ? C17 C18 C15 127.0(4) . . ? C18 C19 C15 64.5(5) . . ? C18 C19 C17 61.7(4) . . ? C15 C19 C17 126.2(5) . . ? C18 C19 C19 127.9(8) . 3_755 ? C15 C19 C19 63.4(4) . 3_755 ? C17 C19 C19 170.4(8) . 3_755 ? C18 C19 C15 177.7(6) . 3_755 ? C15 C19 C15 117.8(4) . 3_755 ? C17 C19 C15 115.9(5) . 3_755 ? C19 C19 C15 54.5(4) 3_755 3_755 ? C18 C19 C16 121.5(6) . 3_755 ? C15 C19 C16 174.0(5) . 3_755 ? C17 C19 C16 59.7(4) . 3_755 ? C19 C19 C16 110.7(7) 3_755 3_755 ? C15 C19 C16 56.2(4) 3_755 3_755 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.227 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.076 # Attachment 'B810479D_-_3AgClO4_benz__-_R.cif' data_cdm15a_0m _database_code_depnum_ccdc_archive 'CCDC 692772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 Ag Cl N2 O4' _chemical_formula_weight 489.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2_1/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4242(6) _cell_length_b 19.9968(17) _cell_length_c 12.8576(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.527(2) _cell_angle_gamma 90.00 _cell_volume 1907.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.226 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8186 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details 'APEX II' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18166 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 29.99 _reflns_number_total 5548 _reflns_number_gt 4476 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0155P)^2^+1.5553P] 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 5548 _refine_ls_number_parameters 257 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.279 _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 Ag1 Ag 0.22694(3) 0.515029(14) 0.505037(16) 0.04689(9) Uani 1 1 d . . . Cl1 Cl -0.06146(12) 0.62453(4) 0.66544(6) 0.04576(19) Uani 1 1 d . . . O1 O -0.0519(6) 0.69220(15) 0.6468(4) 0.1180(15) Uani 1 1 d . A . O2 O -0.0854(7) 0.6175(3) 0.7712(3) 0.157(2) Uani 1 1 d . A . O3 O 0.1102(4) 0.59112(17) 0.6573(3) 0.0919(10) Uani 1 1 d . A . O4A O -0.2191(9) 0.5897(2) 0.6250(6) 0.094(2) Uani 0.673(7) 1 d PU A 1 O4B O -0.1269(19) 0.6054(5) 0.5656(12) 0.094(2) Uani 0.327(7) 1 d PU A 2 N1 N 0.4190(3) 0.48449(13) 0.62505(18) 0.0415(6) Uani 1 1 d . . . N2 N 1.0703(4) 0.55650(13) 1.37651(18) 0.0410(6) Uani 1 1 d . . . C1 C 0.4908(4) 0.47104(14) 0.7024(2) 0.0337(6) Uani 1 1 d . . . C2 C 0.5788(3) 0.45413(14) 0.80040(18) 0.0296(5) Uani 1 1 d . . . C3 C 0.5941(4) 0.38758(15) 0.8291(2) 0.0373(6) Uani 1 1 d . . . H3A H 0.5530 0.3537 0.7845 0.045 Uiso 1 1 calc R . . C4 C 0.6723(5) 0.37313(15) 0.9261(2) 0.0431(7) Uani 1 1 d . . . H4A H 0.6839 0.3288 0.9473 0.052 Uiso 1 1 calc R . . C5 C 0.7337(4) 0.42377(14) 0.99186(19) 0.0364(6) Uani 1 1 d . . . H5A H 0.7850 0.4127 1.0569 0.044 Uiso 1 1 calc R . . C6 C 0.7206(3) 0.49076(13) 0.96329(18) 0.0257(5) Uani 1 1 d . . . C7 C 0.6408(3) 0.50559(13) 0.86578(18) 0.0279(5) Uani 1 1 d . . . H7A H 0.6289 0.5499 0.8444 0.033 Uiso 1 1 calc R . . C8 C 0.7870(3) 0.54557(12) 1.03361(18) 0.0260(5) Uani 1 1 d . . . C9 C 0.7748(4) 0.61257(14) 1.0040(2) 0.0412(7) Uani 1 1 d . . . H9A H 0.7255 0.6230 0.9382 0.049 Uiso 1 1 calc R . . C10 C 0.8331(5) 0.66402(15) 1.0687(2) 0.0484(8) Uani 1 1 d . . . H10A H 0.8214 0.7081 1.0464 0.058 Uiso 1 1 calc R . . C11 C 0.9087(4) 0.65025(14) 1.1663(2) 0.0388(7) Uani 1 1 d . . . H11A H 0.9494 0.6845 1.2102 0.047 Uiso 1 1 calc R . . C12 C 0.9224(3) 0.58417(13) 1.19722(18) 0.0293(5) Uani 1 1 d . . . C13 C 0.8629(3) 0.53205(13) 1.13258(18) 0.0268(5) Uani 1 1 d . . . H13A H 0.8739 0.4881 1.1555 0.032 Uiso 1 1 calc R . . C14 C 1.0048(4) 0.56834(13) 1.2976(2) 0.0321(5) Uani 1 1 d . . . C15 C 0.5692(11) 0.7564(4) 0.3297(6) 0.113(3) Uani 1 1 d . . . H15A H 0.6660 0.7729 0.2939 0.169 Uiso 1 1 calc R . . C16 C 0.3931(13) 0.7782(2) 0.3065(4) 0.101(2) Uani 1 1 d . . . H16A H 0.3695 0.8096 0.2543 0.121 Uiso 1 1 calc R . . C17 C 0.2589(8) 0.7531(3) 0.3609(5) 0.0861(16) Uani 1 1 d . . . H17A H 0.1410 0.7669 0.3458 0.103 Uiso 1 1 calc R . . C18 C 0.2924(10) 0.7087(3) 0.4359(5) 0.0954(18) Uani 1 1 d . . . H18A H 0.1978 0.6923 0.4735 0.143 Uiso 1 1 calc R . . C19 C 0.4580(14) 0.6875(3) 0.4578(4) 0.104(2) Uani 1 1 d . . . H19A H 0.4783 0.6561 0.5104 0.156 Uiso 1 1 calc R . . C20 C 0.5938(9) 0.7098(4) 0.4069(7) 0.109(3) Uani 1 1 d . . . H20A H 0.7092 0.6938 0.4233 0.164 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04803(15) 0.06138(17) 0.02979(12) 0.00798(10) -0.01505(9) 0.00278(11) Cl1 0.0682(5) 0.0259(3) 0.0432(4) -0.0025(3) 0.0020(3) 0.0033(3) O1 0.137(3) 0.0344(16) 0.178(4) 0.036(2) -0.042(3) -0.0024(18) O2 0.169(5) 0.211(6) 0.096(3) 0.044(3) 0.056(3) 0.006(4) O3 0.081(2) 0.073(2) 0.121(3) -0.0262(19) -0.0035(19) 0.0213(17) O4A 0.096(4) 0.047(3) 0.133(5) -0.013(3) -0.054(4) -0.007(2) O4B 0.096(4) 0.047(3) 0.133(5) -0.013(3) -0.054(4) -0.007(2) N1 0.0427(14) 0.0504(15) 0.0304(11) -0.0015(10) -0.0103(10) 0.0005(12) N2 0.0526(15) 0.0365(13) 0.0324(12) 0.0024(10) -0.0140(11) -0.0047(11) C1 0.0331(14) 0.0399(15) 0.0275(12) -0.0044(10) -0.0060(10) -0.0001(11) C2 0.0281(12) 0.0373(14) 0.0227(11) -0.0024(10) -0.0052(9) 0.0023(10) C3 0.0449(16) 0.0352(15) 0.0309(13) -0.0057(11) -0.0077(11) -0.0027(12) C4 0.063(2) 0.0275(14) 0.0376(15) 0.0018(11) -0.0123(14) -0.0009(13) C5 0.0496(17) 0.0326(14) 0.0260(12) 0.0032(10) -0.0105(11) -0.0002(12) C6 0.0277(12) 0.0285(12) 0.0207(10) 0.0010(9) -0.0023(9) -0.0001(9) C7 0.0290(12) 0.0312(13) 0.0229(11) 0.0004(9) -0.0055(9) 0.0017(10) C8 0.0298(12) 0.0262(12) 0.0214(10) 0.0012(9) -0.0047(9) 0.0005(9) C9 0.0615(19) 0.0295(14) 0.0306(13) 0.0041(11) -0.0186(13) 0.0002(13) C10 0.075(2) 0.0250(14) 0.0428(16) 0.0035(12) -0.0232(15) -0.0005(14) C11 0.0528(18) 0.0282(13) 0.0339(13) -0.0024(11) -0.0147(12) -0.0008(12) C12 0.0317(13) 0.0329(13) 0.0228(11) 0.0012(9) -0.0055(9) 0.0002(10) C13 0.0289(12) 0.0277(12) 0.0232(10) 0.0025(9) -0.0044(9) 0.0012(9) C14 0.0374(14) 0.0296(13) 0.0286(12) 0.0001(10) -0.0079(10) -0.0034(11) C15 0.140(6) 0.079(4) 0.125(5) -0.068(4) 0.059(5) -0.064(4) C16 0.211(8) 0.040(2) 0.050(2) -0.0103(18) -0.015(4) 0.004(4) C17 0.090(4) 0.070(3) 0.096(4) -0.044(3) -0.032(3) 0.015(3) C18 0.136(5) 0.057(3) 0.095(4) -0.033(3) 0.024(4) -0.036(3) C19 0.194(7) 0.046(3) 0.068(3) -0.018(2) -0.041(4) 0.013(4) C20 0.091(4) 0.087(5) 0.145(6) -0.075(4) -0.053(4) 0.014(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 N1 2.143(2) . ? Ag1 N2 2.145(2) 1_454 ? Cl1 O1 1.377(3) . ? Cl1 O2 1.386(4) . ? Cl1 O4B 1.405(12) . ? Cl1 O4A 1.439(5) . ? Cl1 O3 1.447(3) . ? N1 C1 1.139(3) . ? N2 C14 1.131(3) . ? N2 Ag1 2.145(2) 1_656 ? C1 C2 1.434(3) . ? C2 C3 1.384(4) . ? C2 C7 1.394(3) . ? C3 C4 1.383(4) . ? C4 C5 1.384(4) . ? C5 C6 1.391(4) . ? C6 C7 1.395(3) . ? C6 C8 1.491(3) . ? C8 C9 1.395(4) . ? C8 C13 1.395(3) . ? C9 C10 1.381(4) . ? C10 C11 1.380(4) . ? C11 C12 1.382(4) . ? C12 C13 1.393(3) . ? C12 C14 1.439(3) . ? C15 C20 1.367(10) . ? C15 C16 1.398(9) . ? C16 C17 1.340(8) . ? C17 C18 1.327(8) . ? C18 C19 1.319(9) . ? C19 C20 1.305(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 Ag1 N2 170.30(10) . 1_454 ? O1 Cl1 O2 106.3(3) . . ? O1 Cl1 O4B 97.4(5) . . ? O2 Cl1 O4B 144.5(7) . . ? O1 Cl1 O4A 117.4(3) . . ? O2 Cl1 O4A 99.6(4) . . ? O4B Cl1 O4A 45.2(6) . . ? O1 Cl1 O3 112.9(2) . . ? O2 Cl1 O3 100.1(3) . . ? O4B Cl1 O3 94.5(6) . . ? O4A Cl1 O3 117.1(3) . . ? C1 N1 Ag1 165.1(3) . . ? C14 N2 Ag1 165.8(3) . 1_656 ? N1 C1 C2 179.3(3) . . ? C3 C2 C7 121.9(2) . . ? C3 C2 C1 119.3(2) . . ? C7 C2 C1 118.8(2) . . ? C4 C3 C2 117.9(2) . . ? C3 C4 C5 120.8(3) . . ? C4 C5 C6 121.7(2) . . ? C5 C6 C7 117.6(2) . . ? C5 C6 C8 122.0(2) . . ? C7 C6 C8 120.3(2) . . ? C2 C7 C6 120.1(2) . . ? C9 C8 C13 117.0(2) . . ? C9 C8 C6 121.7(2) . . ? C13 C8 C6 121.3(2) . . ? C10 C9 C8 122.4(2) . . ? C11 C10 C9 120.2(3) . . ? C10 C11 C12 118.3(2) . . ? C11 C12 C13 121.8(2) . . ? C11 C12 C14 119.4(2) . . ? C13 C12 C14 118.8(2) . . ? C12 C13 C8 120.3(2) . . ? N2 C14 C12 179.3(3) . . ? C20 C15 C16 117.5(6) . . ? C17 C16 C15 118.8(5) . . ? C18 C17 C16 120.7(6) . . ? C19 C18 C17 120.9(6) . . ? C20 C19 C18 121.1(6) . . ? C19 C20 C15 121.1(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.918 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.085 # Attachment 'B810479D_-_4_-_R.cif' data_cdm5_0m _database_code_depnum_ccdc_archive 'CCDC 692773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common T2CN2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H4 N2 S2' _chemical_formula_weight 216.27 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 3.8090(2) _cell_length_b 7.4518(4) _cell_length_c 8.2086(5) _cell_angle_alpha 87.9360(10) _cell_angle_beta 85.4850(10) _cell_angle_gamma 82.1260(10) _cell_volume 230.00(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 110 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.932997 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'APEX II' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2744 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.67 _diffrn_reflns_theta_max 26.46 _reflns_number_total 947 _reflns_number_gt 889 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0266P)^2^+0.1080P] 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 947 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 S1 S 0.70875(9) 0.21636(4) 0.45877(4) 0.02063(13) Uani 1 1 d . . . N1 N 0.8497(4) -0.15045(18) 0.15240(16) 0.0319(3) Uani 1 1 d . . . C1 C 0.6413(4) 0.16932(19) 0.26015(16) 0.0208(3) Uani 1 1 d . . . C2 C 0.4761(4) 0.3172(2) 0.17862(17) 0.0240(3) Uani 1 1 d . . . H2 H 0.4174 0.3165 0.0683 0.029 Uiso 1 1 calc R . . C3 C 0.4038(4) 0.47018(19) 0.27763(17) 0.0231(3) Uani 1 1 d . . . H3 H 0.2899 0.5843 0.2410 0.028 Uiso 1 1 calc R . . C4 C 0.5146(4) 0.43794(18) 0.43267(17) 0.0188(3) Uani 1 1 d . . . C5 C 0.7562(4) -0.0077(2) 0.19903(17) 0.0233(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 S1 0.0240(2) 0.01785(19) 0.01964(19) -0.00246(12) -0.00401(13) 0.00052(13) N1 0.0424(8) 0.0258(7) 0.0263(7) -0.0050(5) -0.0053(6) 0.0020(6) C1 0.0222(7) 0.0216(7) 0.0188(7) -0.0044(5) -0.0009(5) -0.0033(5) C2 0.0276(8) 0.0246(7) 0.0203(7) -0.0013(6) -0.0041(6) -0.0034(6) C3 0.0259(7) 0.0201(7) 0.0228(7) 0.0005(5) -0.0036(6) -0.0008(6) C4 0.0175(7) 0.0161(6) 0.0227(7) -0.0016(5) -0.0007(5) -0.0022(5) C5 0.0256(8) 0.0248(7) 0.0193(7) -0.0011(6) -0.0024(5) -0.0027(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 S1 C1 1.7259(14) . ? S1 C4 1.7274(14) . ? N1 C5 1.144(2) . ? C1 C2 1.372(2) . ? C1 C5 1.4274(19) . ? C2 C3 1.408(2) . ? C3 C4 1.375(2) . ? C4 C4 1.455(3) 2_666 ? 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 C1 S1 C4 91.10(7) . . ? C2 C1 C5 127.78(13) . . ? C2 C1 S1 112.24(11) . . ? C5 C1 S1 119.98(11) . . ? C1 C2 C3 112.05(13) . . ? C4 C3 C2 113.25(13) . . ? C3 C4 C4 128.80(16) . 2_666 ? C3 C4 S1 111.37(10) . . ? C4 C4 S1 119.83(14) 2_666 . ? N1 C5 C1 178.94(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.271 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.046 # Attachment 'B810479D_-__4_2AgBF4.cif' data_cdm12_0m _database_code_depnum_ccdc_archive 'CCDC 692774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H8 Ag B F4 N4 S4' _chemical_formula_weight 627.22 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' 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 Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 13.6376(19) _cell_length_b 13.6376(19) _cell_length_c 6.2054(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1154.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7832 _exptl_absorpt_correction_T_max 0.9042 _exptl_absorpt_process_details 'APEX II' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10648 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1398 _reflns_number_gt 1233 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0125P)^2^+1.6840P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1398 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.348 _refine_ls_restrained_S_all 1.348 _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 Ag1 Ag 0.2500 0.7500 0.5000 0.04420(19) Uani 1 4 d S . . S1 S 0.47262(7) 0.60431(6) 1.24374(14) 0.0419(2) Uani 1 1 d . . . B1 B 0.2500 0.2500 0.774(2) 0.064(3) Uani 1 4 d S . . N1 N 0.3263(2) 0.6527(2) 0.7498(5) 0.0460(7) Uani 1 1 d . . . C1 C 0.3803(2) 0.5584(2) 1.0844(5) 0.0384(7) Uani 1 1 d . . . C2 C 0.3474(3) 0.4691(3) 1.1546(6) 0.0496(9) Uani 1 1 d . . . H2A H 0.2974 0.4323 1.0852 0.059 Uiso 1 1 calc R . . C3 C 0.3966(3) 0.4387(3) 1.3417(6) 0.0473(8) Uani 1 1 d . . . H3A H 0.3824 0.3793 1.4150 0.057 Uiso 1 1 calc R . . C4 C 0.4671(2) 0.5033(2) 1.4078(5) 0.0362(7) Uani 1 1 d . . . C5 C 0.3497(2) 0.6103(3) 0.8984(6) 0.0398(7) Uani 1 1 d . . . F6 F 0.2500 0.2500 1.0033(12) 0.110(2) Uani 1 4 d S . . F7A F 0.2557(6) 0.3467(4) 0.7236(9) 0.129(2) Uani 0.70 1 d P . . F7B F 0.2500 0.2500 0.526(5) 0.102(11) Uani 0.20 4 d SP . . 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 0.0545(2) 0.0545(2) 0.0236(2) 0.000 0.000 0.000 S1 0.0473(5) 0.0412(5) 0.0371(4) 0.0106(4) -0.0066(4) 0.0018(3) B1 0.063(4) 0.063(4) 0.067(7) 0.000 0.000 0.000 N1 0.0470(17) 0.0542(18) 0.0369(15) 0.0047(14) -0.0059(13) 0.0044(13) C1 0.0378(17) 0.0444(18) 0.0330(16) 0.0035(14) 0.0009(13) 0.0101(14) C2 0.052(2) 0.052(2) 0.045(2) 0.0047(17) -0.0092(17) -0.0019(17) C3 0.055(2) 0.045(2) 0.0416(19) 0.0119(16) -0.0040(16) -0.0020(16) C4 0.0416(17) 0.0382(16) 0.0287(15) 0.0067(13) 0.0036(13) 0.0087(14) C5 0.0394(17) 0.0432(18) 0.0369(17) 0.0008(15) -0.0016(14) 0.0062(14) F6 0.128(4) 0.128(4) 0.076(4) 0.000 0.000 0.000 F7A 0.194(6) 0.089(3) 0.104(4) 0.028(3) -0.012(4) 0.003(4) F7B 0.128(17) 0.128(17) 0.049(17) 0.000 0.000 0.000 _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 2.291(3) . ? Ag1 N1 2.291(3) 7_566 ? Ag1 N1 2.291(3) 2_565 ? Ag1 N1 2.291(3) 8_666 ? S1 C4 1.715(3) . ? S1 C1 1.719(4) . ? B1 F7A 1.358(6) . ? B1 F7A 1.358(6) 2 ? B1 F7A 1.358(6) 3 ? B1 F7A 1.358(6) 4 ? B1 F6 1.421(13) . ? B1 F7B 1.54(3) . ? N1 C5 1.135(4) . ? C1 C2 1.368(5) . ? C1 C5 1.417(5) . ? C2 C3 1.404(5) . ? C3 C4 1.366(5) . ? C4 C4 1.457(6) 5_668 ? 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 N1 117.25(9) . 7_566 ? N1 Ag1 N1 94.84(16) . 2_565 ? N1 Ag1 N1 117.25(9) 7_566 2_565 ? N1 Ag1 N1 117.25(9) . 8_666 ? N1 Ag1 N1 94.84(16) 7_566 8_666 ? N1 Ag1 N1 117.25(9) 2_565 8_666 ? C4 S1 C1 90.94(17) . . ? F7A B1 F7A 153.2(11) . 2 ? F7A B1 F7A 86.9(3) . 3 ? F7A B1 F7A 86.9(3) 2 3 ? F7A B1 F7A 86.9(3) . 4 ? F7A B1 F7A 86.9(3) 2 4 ? F7A B1 F7A 153.2(11) 3 4 ? F7A B1 F6 103.4(6) . . ? F7A B1 F6 103.4(6) 2 . ? F7A B1 F6 103.4(6) 3 . ? F7A B1 F6 103.4(6) 4 . ? F7A B1 F7B 76.6(6) . . ? F7A B1 F7B 76.6(6) 2 . ? F7A B1 F7B 76.6(6) 3 . ? F7A B1 F7B 76.6(6) 4 . ? F6 B1 F7B 180.000(12) . . ? C5 N1 Ag1 166.7(3) . . ? C2 C1 C5 127.4(3) . . ? C2 C1 S1 112.4(3) . . ? C5 C1 S1 120.1(3) . . ? C1 C2 C3 111.6(3) . . ? C4 C3 C2 113.2(3) . . ? C3 C4 C4 129.0(4) . 5_668 ? C3 C4 S1 111.7(3) . . ? C4 C4 S1 119.3(3) 5_668 . ? N1 C5 C1 179.1(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.771 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.078 # Attachment 'B810479D_-__4_2AgClO4_-_R.cif' data_cdm-8_0m _database_code_depnum_ccdc_archive 'CCDC 692775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H8 Ag Cl N4 O4 S4' _chemical_formula_weight 639.86 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 13.834(5) _cell_length_b 13.834(5) _cell_length_c 6.162(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1179.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7023 _exptl_absorpt_correction_T_max 0.8991 _exptl_absorpt_process_details 'APEX II' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10613 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 29.99 _reflns_number_total 1699 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0149P)^2^+0.5349P] 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 1699 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.342 _refine_ls_restrained_S_all 1.342 _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 Ag1 Ag 0.2500 0.7500 0.5000 0.04622(12) Uani 1 4 d S . . Cl1 Cl 0.2500 0.2500 0.8058(2) 0.0553(3) Uani 1 4 d S . . S1 S 0.47298(4) 0.60196(4) 1.23856(9) 0.04199(15) Uani 1 1 d . . . O6 O 0.2500 0.2500 1.0400(7) 0.0757(12) Uani 1 4 d S A . O7A O 0.284(2) 0.3348(18) 0.722(2) 0.147(8) Uani 0.40 1 d P A 1 O7B O 0.3525(8) 0.2590(15) 0.7440(15) 0.079(4) Uani 0.35 1 d P A 2 N1 N 0.32319(14) 0.65123(15) 0.7473(3) 0.0471(5) Uani 1 1 d . . . C1 C 0.37797(15) 0.55880(16) 1.0862(4) 0.0395(4) Uani 1 1 d . . . C2 C 0.34311(19) 0.47269(18) 1.1639(4) 0.0506(6) Uani 1 1 d . . . H2A H 0.2921 0.4388 1.1017 0.061 Uiso 1 1 calc R . . C3 C 0.39397(18) 0.44188(18) 1.3491(4) 0.0491(5) Uani 1 1 d . . . H3A H 0.3798 0.3851 1.4232 0.059 Uiso 1 1 calc R . . C4 C 0.46636(15) 0.50366(14) 1.4093(3) 0.0370(4) Uani 1 1 d . . . C5 C 0.34690(16) 0.60950(16) 0.8986(4) 0.0409(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.05514(16) 0.05514(16) 0.02839(17) 0.000 0.000 0.000 Cl1 0.0569(5) 0.0569(5) 0.0520(7) 0.000 0.000 0.000 S1 0.0433(3) 0.0384(3) 0.0442(3) 0.0109(2) -0.0052(2) 0.0007(2) O6 0.088(2) 0.088(2) 0.051(2) 0.000 0.000 0.000 O7A 0.148(13) 0.175(16) 0.119(8) 0.047(10) 0.013(10) -0.112(13) O7B 0.052(5) 0.116(10) 0.070(5) 0.026(6) 0.007(4) -0.044(7) N1 0.0456(11) 0.0508(11) 0.0450(11) 0.0049(9) -0.0060(8) 0.0042(9) C1 0.0394(11) 0.0420(11) 0.0372(10) 0.0025(8) -0.0016(8) 0.0074(8) C2 0.0508(14) 0.0481(13) 0.0531(14) 0.0058(10) -0.0092(11) -0.0054(10) C3 0.0545(14) 0.0436(12) 0.0493(13) 0.0137(10) -0.0032(10) -0.0044(10) C4 0.0409(11) 0.0342(10) 0.0359(10) 0.0051(8) 0.0050(8) 0.0060(8) C5 0.0392(11) 0.0420(11) 0.0414(11) -0.0005(9) -0.0013(9) 0.0059(9) _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 2.284(2) 7_566 ? Ag1 N1 2.284(2) 8_666 ? Ag1 N1 2.284(2) 2_565 ? Ag1 N1 2.284(2) . ? Cl1 O7A 1.368(14) 2 ? Cl1 O7A 1.368(14) 3 ? Cl1 O7A 1.368(14) 4 ? Cl1 O7A 1.368(14) . ? Cl1 O6 1.443(4) . ? Cl1 O7B 1.474(10) 2 ? Cl1 O7B 1.474(10) 4 ? Cl1 O7B 1.474(10) . ? Cl1 O7B 1.474(10) 3 ? S1 C4 1.722(2) . ? S1 C1 1.722(2) . ? O7A O7A 1.79(2) 3 ? O7A O7A 1.79(2) 4 ? N1 C5 1.144(3) . ? C1 C2 1.371(3) . ? C1 C5 1.419(3) . ? C2 C3 1.407(3) . ? C3 C4 1.368(3) . ? C4 C4 1.458(4) 5_668 ? 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 N1 96.27(11) 7_566 8_666 ? N1 Ag1 N1 116.45(6) 7_566 2_565 ? N1 Ag1 N1 116.45(6) 8_666 2_565 ? N1 Ag1 N1 116.45(6) 7_566 . ? N1 Ag1 N1 116.45(6) 8_666 . ? N1 Ag1 N1 96.27(11) 2_565 . ? O7A Cl1 O7A 81.7(4) 2 3 ? O7A Cl1 O7A 81.7(4) 2 4 ? O7A Cl1 O7A 135.4(12) 3 4 ? O7A Cl1 O7A 135.4(12) 2 . ? O7A Cl1 O7A 81.7(4) 3 . ? O7A Cl1 O7A 81.7(4) 4 . ? O7A Cl1 O6 112.3(6) 2 . ? O7A Cl1 O6 112.3(6) 3 . ? O7A Cl1 O6 112.3(6) 4 . ? O7A Cl1 O6 112.3(6) . . ? O7A Cl1 O7B 59.7(9) 2 2 ? O7A Cl1 O7B 26.6(9) 3 2 ? O7A Cl1 O7B 134.3(7) 4 2 ? O7A Cl1 O7B 108.0(8) . 2 ? O6 Cl1 O7B 105.0(4) . 2 ? O7A Cl1 O7B 26.6(9) 2 4 ? O7A Cl1 O7B 108.0(8) 3 4 ? O7A Cl1 O7B 59.7(9) 4 4 ? O7A Cl1 O7B 134.3(7) . 4 ? O6 Cl1 O7B 105.0(4) . 4 ? O7B Cl1 O7B 86.17(19) 2 4 ? O7A Cl1 O7B 108.0(8) 2 . ? O7A Cl1 O7B 134.3(7) 3 . ? O7A Cl1 O7B 26.6(9) 4 . ? O7A Cl1 O7B 59.7(9) . . ? O6 Cl1 O7B 105.0(4) . . ? O7B Cl1 O7B 150.1(8) 2 . ? O7B Cl1 O7B 86.17(19) 4 . ? O7A Cl1 O7B 134.3(7) 2 3 ? O7A Cl1 O7B 59.7(9) 3 3 ? O7A Cl1 O7B 108.0(8) 4 3 ? O7A Cl1 O7B 26.6(9) . 3 ? O6 Cl1 O7B 105.0(4) . 3 ? O7B Cl1 O7B 86.17(19) 2 3 ? O7B Cl1 O7B 150.1(8) 4 3 ? O7B Cl1 O7B 86.17(19) . 3 ? C4 S1 C1 91.08(11) . . ? Cl1 O7A O7A 49.1(2) . 3 ? Cl1 O7A O7A 49.1(2) . 4 ? O7A O7A O7A 90.000(4) 3 4 ? C5 N1 Ag1 166.5(2) . . ? C2 C1 C5 127.4(2) . . ? C2 C1 S1 112.29(17) . . ? C5 C1 S1 120.27(17) . . ? C1 C2 C3 111.7(2) . . ? C4 C3 C2 113.4(2) . . ? C3 C4 C4 129.2(2) . 5_668 ? C3 C4 S1 111.50(17) . . ? C4 C4 S1 119.3(2) 5_668 . ? N1 C5 C1 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.503 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.073