# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shim Sung Lee' _publ_contact_author_email SSLEE@GNU.AC.KR _publ_section_title ; Endo- and/or exocyclic silver(I) and mercury(II) complexes of an NO2S2-macrocycle: effect of ligand ratio and anion ; loop_ _publ_author_name 'Shim Sung Lee' 'Hyun Jee Kim' 'Jai Young Lee' 'Kaniz Fatima Sultana' # Attachment 'cifs.cif' data_Ligand _database_code_depnum_ccdc_archive 'CCDC 750352' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H23 N O2 S2' _chemical_formula_weight 409.54 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7460(8) _cell_length_b 7.1253(5) _cell_length_c 12.3756(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.5840(10) _cell_angle_gamma 90.00 _cell_volume 1028.93(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2979 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.74 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6083 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3860 _reflns_number_gt 3384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.2295P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(8) _refine_ls_number_reflns 3860 _refine_ls_number_parameters 272 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 S1 S 0.25512(6) 0.84582(11) 0.46139(6) 0.0377(2) Uani 1 1 d . . . S2 S 0.49938(7) 0.82506(12) 0.76189(6) 0.0414(2) Uani 1 1 d . . . O1 O 0.14889(17) 0.4072(3) 0.49841(14) 0.0388(5) Uani 1 1 d . . . O2 O 0.45177(15) 0.3686(3) 0.81893(14) 0.0357(5) Uani 1 1 d . . . N1 N 0.22651(18) 0.2565(3) 0.71556(17) 0.0253(5) Uani 1 1 d . . . C1 C 0.0893(2) 0.2666(4) 0.5533(2) 0.0287(6) Uani 1 1 d . . . H1A H 0.1138 0.1394 0.5335 0.034 Uiso 1 1 calc R . . H1B H 0.0055 0.2777 0.5333 0.034 Uiso 1 1 calc R . . C2 C 0.1239(2) 0.4252(4) 0.3881(2) 0.0277(6) Uani 1 1 d . A . C3 C 0.0292(2) 0.3482(5) 0.3275(2) 0.0320(6) Uani 1 1 d . . . H3A H -0.0228 0.2722 0.3615 0.038 Uiso 1 1 calc R . . C4 C 0.0106(2) 0.3829(4) 0.2162(2) 0.0355(7) Uani 1 1 d . . . H4A H -0.0551 0.3322 0.1744 0.043 Uiso 1 1 calc R . . C5 C 0.0868(3) 0.4904(4) 0.1665(2) 0.0326(7) Uani 1 1 d . . . H5A H 0.0737 0.5133 0.0905 0.039 Uiso 1 1 calc R . . C6 C 0.1829(2) 0.5655(4) 0.2270(2) 0.0301(6) Uani 1 1 d . A . H6A H 0.2358 0.6378 0.1919 0.036 Uiso 1 1 calc R . . C7 C 0.2023(2) 0.5355(4) 0.3389(2) 0.0274(6) Uani 1 1 d . . . C8 C 0.3025(2) 0.6264(4) 0.4059(2) 0.0301(6) Uani 1 1 d . A . H8A H 0.3645 0.6512 0.3599 0.036 Uiso 1 1 calc R . . H8B H 0.3327 0.5416 0.4658 0.036 Uiso 1 1 calc R . . C9 C 0.3788(3) 0.8956(6) 0.5598(3) 0.0344(13) Uani 0.770(9) 1 d P A 1 H9A H 0.4493 0.8501 0.5315 0.041 Uiso 0.770(9) 1 calc PR A 1 H9B H 0.3860 1.0328 0.5711 0.041 Uiso 0.770(9) 1 calc PR A 1 C10 C 0.3657(4) 0.8001(6) 0.6670(4) 0.0350(12) Uani 0.770(9) 1 d P A 1 H10A H 0.3485 0.6654 0.6543 0.042 Uiso 0.770(9) 1 calc PR A 1 H10B H 0.3009 0.8571 0.6998 0.042 Uiso 0.770(9) 1 calc PR A 1 C9' C 0.3163(11) 0.807(2) 0.6129(12) 0.031(4) Uani 0.230(9) 1 d P A 2 H9'A H 0.2660 0.8671 0.6618 0.038 Uiso 0.230(9) 1 calc PR A 2 H9'B H 0.3217 0.6716 0.6298 0.038 Uiso 0.230(9) 1 calc PR A 2 C10' C 0.4351(10) 0.8972(19) 0.6275(11) 0.030(4) Uani 0.230(9) 1 d P A 2 H10C H 0.4291 1.0356 0.6230 0.036 Uiso 0.230(9) 1 calc PR A 2 H10D H 0.4816 0.8526 0.5708 0.036 Uiso 0.230(9) 1 calc PR A 2 C11 C 0.5811(2) 0.6259(4) 0.7204(2) 0.0297(6) Uani 1 1 d . A . H11A H 0.5308 0.5437 0.6712 0.036 Uiso 1 1 calc R . . H11B H 0.6442 0.6708 0.6805 0.036 Uiso 1 1 calc R . . C12 C 0.6295(2) 0.5170(4) 0.8190(2) 0.0254(6) Uani 1 1 d . . . C13 C 0.7408(2) 0.5477(4) 0.8675(2) 0.0317(7) Uani 1 1 d . A . H13A H 0.7887 0.6332 0.8348 0.038 Uiso 1 1 calc R . . C14 C 0.7835(2) 0.4563(4) 0.9626(2) 0.0327(7) Uani 1 1 d . . . H14A H 0.8588 0.4823 0.9956 0.039 Uiso 1 1 calc R A . C15 C 0.7162(2) 0.3274(5) 1.0088(2) 0.0309(6) Uani 1 1 d . A . H15A H 0.7456 0.2640 1.0736 0.037 Uiso 1 1 calc R . . C16 C 0.6051(2) 0.2897(4) 0.9613(2) 0.0277(6) Uani 1 1 d . . . H16A H 0.5596 0.1983 0.9922 0.033 Uiso 1 1 calc R A . C17 C 0.5617(2) 0.3871(4) 0.8683(2) 0.0266(6) Uani 1 1 d . A . C18 C 0.3755(2) 0.2484(4) 0.8694(2) 0.0283(6) Uani 1 1 d . . . H18A H 0.3840 0.2696 0.9490 0.034 Uiso 1 1 calc R . . H18B H 0.3931 0.1152 0.8557 0.034 Uiso 1 1 calc R . . C19 C 0.2555(2) 0.2940(3) 0.8213(2) 0.0235(6) Uani 1 1 d . . . C20 C 0.1792(2) 0.3716(4) 0.8871(2) 0.0285(6) Uani 1 1 d . . . H20A H 0.2027 0.3955 0.9619 0.034 Uiso 1 1 calc R . . C21 C 0.0695(2) 0.4133(4) 0.8426(2) 0.0331(7) Uani 1 1 d . . . H21A H 0.0158 0.4649 0.8861 0.040 Uiso 1 1 calc R . . C22 C 0.0390(2) 0.3787(4) 0.7333(2) 0.0286(6) Uani 1 1 d . . . H22A H -0.0360 0.4072 0.7000 0.034 Uiso 1 1 calc R . . C23 C 0.1198(2) 0.3015(4) 0.6731(2) 0.0234(6) 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 0.0348(4) 0.0326(4) 0.0422(4) -0.0044(4) -0.0109(3) 0.0025(3) S2 0.0513(5) 0.0416(5) 0.0286(4) -0.0072(4) -0.0068(3) 0.0177(4) O1 0.0463(12) 0.0470(13) 0.0217(9) 0.0043(9) -0.0024(8) -0.0223(10) O2 0.0236(9) 0.0528(14) 0.0295(9) 0.0148(10) -0.0019(7) -0.0055(10) N1 0.0272(12) 0.0262(12) 0.0232(11) 0.0016(9) 0.0059(9) -0.0029(9) C1 0.0280(14) 0.0317(15) 0.0259(14) 0.0006(12) 0.0007(11) -0.0039(12) C2 0.0330(15) 0.0290(15) 0.0212(13) -0.0033(11) 0.0032(11) -0.0003(12) C3 0.0344(14) 0.0316(15) 0.0293(13) -0.0018(14) 0.0010(11) -0.0037(14) C4 0.0376(16) 0.0372(19) 0.0288(14) -0.0093(13) -0.0088(12) 0.0041(14) C5 0.0417(17) 0.0346(17) 0.0210(14) -0.0021(12) 0.0012(13) 0.0094(14) C6 0.0370(16) 0.0289(16) 0.0256(14) 0.0026(12) 0.0087(12) 0.0058(13) C7 0.0292(15) 0.0264(15) 0.0266(14) -0.0039(11) 0.0031(12) 0.0033(12) C8 0.0281(14) 0.0344(16) 0.0284(15) 0.0011(12) 0.0055(12) -0.0036(13) C9 0.032(2) 0.036(2) 0.034(3) 0.0027(18) -0.004(2) -0.0093(17) C10 0.029(2) 0.044(3) 0.031(2) 0.001(2) 0.0016(19) 0.002(2) C9' 0.015(7) 0.046(9) 0.030(7) -0.007(7) -0.011(6) 0.006(6) C10' 0.021(7) 0.036(7) 0.030(8) 0.010(6) -0.006(6) -0.005(5) C11 0.0321(15) 0.0321(16) 0.0264(15) 0.0007(12) 0.0102(12) 0.0036(13) C12 0.0256(14) 0.0281(15) 0.0229(13) -0.0025(11) 0.0043(11) 0.0044(11) C13 0.0279(15) 0.0313(16) 0.0369(16) -0.0054(13) 0.0080(13) -0.0010(12) C14 0.0239(14) 0.0388(18) 0.0344(16) -0.0135(13) -0.0007(12) 0.0039(12) C15 0.0300(13) 0.0367(17) 0.0250(12) -0.0050(13) -0.0015(10) 0.0093(14) C16 0.0279(14) 0.0316(16) 0.0244(13) 0.0010(11) 0.0063(11) 0.0007(12) C17 0.0219(13) 0.0326(16) 0.0254(13) -0.0028(12) 0.0027(10) 0.0017(11) C18 0.0260(14) 0.0327(16) 0.0262(14) 0.0045(12) 0.0025(11) -0.0016(12) C19 0.0252(13) 0.0182(14) 0.0274(13) 0.0064(11) 0.0050(10) -0.0029(11) C20 0.0339(14) 0.0288(17) 0.0235(12) -0.0014(12) 0.0061(11) -0.0033(13) C21 0.0309(15) 0.0368(17) 0.0331(15) 0.0003(14) 0.0105(12) 0.0039(13) C22 0.0234(13) 0.0267(16) 0.0355(14) 0.0048(12) 0.0021(11) 0.0005(11) C23 0.0235(12) 0.0192(14) 0.0270(13) 0.0045(11) 0.0005(10) -0.0048(10) _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 C9 1.820(4) . ? S1 C8 1.820(3) . ? S1 C9' 1.948(15) . ? S2 C10' 1.820(13) . ? S2 C11 1.820(3) . ? S2 C10 1.858(5) . ? O1 C2 1.369(3) . ? O1 C1 1.437(3) . ? O2 C17 1.370(3) . ? O2 C18 1.433(3) . ? N1 C19 1.341(3) . ? N1 C23 1.341(3) . ? C1 C23 1.506(3) . ? C2 C3 1.382(4) . ? C2 C7 1.403(4) . ? C3 C4 1.391(4) . ? C4 C5 1.376(4) . ? C5 C6 1.388(4) . ? C6 C7 1.393(4) . ? C7 C8 1.506(4) . ? C9 C10 1.514(6) . ? C9' C10' 1.527(18) . ? C11 C12 1.501(4) . ? C12 C13 1.393(4) . ? C12 C17 1.405(4) . ? C13 C14 1.387(4) . ? C14 C15 1.378(4) . ? C15 C16 1.395(4) . ? C16 C17 1.390(4) . ? C18 C19 1.501(4) . ? C19 C20 1.393(4) . ? C20 C21 1.374(4) . ? C21 C22 1.382(4) . ? C22 C23 1.386(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 C9 S1 C8 99.49(17) . . ? C9 S1 C9' 37.4(4) . . ? C8 S1 C9' 98.5(4) . . ? C10' S2 C11 98.0(4) . . ? C10' S2 C10 38.5(4) . . ? C11 S2 C10 100.50(17) . . ? C2 O1 C1 118.4(2) . . ? C17 O2 C18 117.87(19) . . ? C19 N1 C23 117.1(2) . . ? O1 C1 C23 106.0(2) . . ? O1 C2 C3 124.8(2) . . ? O1 C2 C7 114.1(2) . . ? C3 C2 C7 121.0(2) . . ? C2 C3 C4 119.4(3) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C2 118.5(2) . . ? C6 C7 C8 120.7(3) . . ? C2 C7 C8 120.8(2) . . ? C7 C8 S1 108.91(19) . . ? C10 C9 S1 110.2(3) . . ? C9 C10 S2 110.3(3) . . ? C10' C9' S1 106.7(9) . . ? C9' C10' S2 105.6(9) . . ? C12 C11 S2 109.66(18) . . ? C13 C12 C17 117.8(2) . . ? C13 C12 C11 121.2(3) . . ? C17 C12 C11 120.9(2) . . ? C14 C13 C12 121.5(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 120.4(3) . . ? C17 C16 C15 119.3(3) . . ? O2 C17 C16 124.0(2) . . ? O2 C17 C12 114.9(2) . . ? C16 C17 C12 121.1(2) . . ? O2 C18 C19 107.7(2) . . ? N1 C19 C20 122.8(2) . . ? N1 C19 C18 117.8(2) . . ? C20 C19 C18 119.5(2) . . ? C21 C20 C19 119.2(2) . . ? C20 C21 C22 118.7(3) . . ? C21 C22 C23 118.7(2) . . ? N1 C23 C22 123.5(2) . . ? N1 C23 C1 116.9(2) . . ? C22 C23 C1 119.6(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.278 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.047 ######################################################################## data_Complex1a _database_code_depnum_ccdc_archive 'CCDC 750353' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Ag Cl2 F6 N O2 P S2' _chemical_formula_weight 747.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 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 16.9740(18) _cell_length_b 9.2667(10) _cell_length_c 22.0941(17) _cell_angle_alpha 90.00 _cell_angle_beta 126.589(5) _cell_angle_gamma 90.00 _cell_volume 2790.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4757 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.20 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6483 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16539 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6059 _reflns_number_gt 4507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+23.0382P] 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 6059 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.1993 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 Ag Ag -0.35214(4) -0.11691(7) -0.61299(3) 0.02758(19) Uani 1 1 d . . . S1 S -0.46063(15) -0.0633(2) -0.57116(11) 0.0301(5) Uani 1 1 d . . . S2 S -0.23603(15) -0.2408(2) -0.48522(12) 0.0321(5) Uani 1 1 d . . . O1 O -0.5206(4) -0.2256(6) -0.7369(3) 0.0270(12) Uani 1 1 d . . . O2 O -0.1869(4) 0.0076(6) -0.5751(3) 0.0275(12) Uani 1 1 d . . . N1 N -0.3599(4) -0.0797(6) -0.7170(4) 0.0223(13) Uani 1 1 d . . . C1 C -0.4916(5) -0.2593(9) -0.7840(4) 0.0285(17) Uani 1 1 d . . . H1A H -0.5512 -0.2689 -0.8365 0.034 Uiso 1 1 calc R . . H1B H -0.4579 -0.3540 -0.7684 0.034 Uiso 1 1 calc R . . C2 C -0.5973(5) -0.1321(8) -0.7624(4) 0.0241(16) Uani 1 1 d . . . C3 C -0.6490(6) -0.0624(8) -0.8321(4) 0.0273(17) Uani 1 1 d . . . H3A H -0.6310 -0.0758 -0.8650 0.033 Uiso 1 1 calc R . . C4 C -0.7266(6) 0.0264(10) -0.8526(5) 0.039(2) Uani 1 1 d . . . H4A H -0.7623 0.0733 -0.9002 0.047 Uiso 1 1 calc R . . C5 C -0.7529(6) 0.0480(11) -0.8057(6) 0.045(2) Uani 1 1 d . . . H5A H -0.8071 0.1084 -0.8210 0.055 Uiso 1 1 calc R . . C6 C -0.7008(6) -0.0178(10) -0.7364(6) 0.044(2) Uani 1 1 d . . . H6A H -0.7189 -0.0012 -0.7038 0.053 Uiso 1 1 calc R . . C7 C -0.6220(6) -0.1085(9) -0.7130(5) 0.0303(17) Uani 1 1 d . . . C8 C -0.5641(6) -0.1806(10) -0.6373(5) 0.037(2) Uani 1 1 d . . . H8A H -0.5401 -0.2758 -0.6402 0.044 Uiso 1 1 calc R . . H8B H -0.6059 -0.1956 -0.6203 0.044 Uiso 1 1 calc R . . C9 C -0.3963(6) -0.1768(11) -0.4867(5) 0.040(2) Uani 1 1 d . . . H9A H -0.4189 -0.1518 -0.4558 0.048 Uiso 1 1 calc R . . H9B H -0.4132 -0.2792 -0.5020 0.048 Uiso 1 1 calc R . . C10 C -0.2845(7) -0.1589(11) -0.4388(5) 0.043(2) Uani 1 1 d . . . H10A H -0.2539 -0.2047 -0.3890 0.052 Uiso 1 1 calc R . . H10B H -0.2677 -0.0549 -0.4305 0.052 Uiso 1 1 calc R . . C11 C -0.1242(6) -0.1382(10) -0.4455(5) 0.036(2) Uani 1 1 d . . . H11A H -0.1380 -0.0338 -0.4482 0.043 Uiso 1 1 calc R . . H11B H -0.0751 -0.1648 -0.3919 0.043 Uiso 1 1 calc R . . C12 C -0.0845(5) -0.1708(9) -0.4894(5) 0.0303(18) Uani 1 1 d . . . C13 C -0.0142(6) -0.2779(9) -0.4659(5) 0.037(2) Uani 1 1 d . . . H13A H 0.0071 -0.3331 -0.4224 0.045 Uiso 1 1 calc R . . C14 C 0.0254(6) -0.3059(10) -0.5042(5) 0.041(2) Uani 1 1 d . . . H14A H 0.0738 -0.3788 -0.4867 0.049 Uiso 1 1 calc R . . C15 C -0.0058(6) -0.2279(9) -0.5675(5) 0.035(2) Uani 1 1 d . . . H15A H 0.0220 -0.2456 -0.5935 0.042 Uiso 1 1 calc R . . C16 C -0.0781(5) -0.1226(9) -0.5940(5) 0.0315(18) Uani 1 1 d . . . H16A H -0.1006 -0.0702 -0.6385 0.038 Uiso 1 1 calc R . . C17 C -0.1168(5) -0.0951(8) -0.5552(4) 0.0258(17) Uani 1 1 d . . . C18 C -0.2242(6) 0.0908(8) -0.6410(5) 0.0318(18) Uani 1 1 d . . . H18A H -0.1685 0.1268 -0.6399 0.038 Uiso 1 1 calc R . . H18B H -0.2591 0.1757 -0.6403 0.038 Uiso 1 1 calc R . . C19 C -0.2942(5) 0.0079(8) -0.7144(4) 0.0270(17) Uani 1 1 d . . . C20 C -0.2906(6) 0.0259(9) -0.7744(5) 0.0328(19) Uani 1 1 d . . . H20A H -0.2419 0.0859 -0.7699 0.039 Uiso 1 1 calc R . . C21 C -0.3585(6) -0.0441(10) -0.8416(5) 0.036(2) Uani 1 1 d . . . H21A H -0.3582 -0.0315 -0.8841 0.043 Uiso 1 1 calc R . . C22 C -0.4269(6) -0.1330(9) -0.8454(5) 0.0348(19) Uani 1 1 d . . . H22A H -0.4746 -0.1818 -0.8910 0.042 Uiso 1 1 calc R . . C23 C -0.4252(5) -0.1504(8) -0.7821(4) 0.0241(16) Uani 1 1 d . . . P P 0.26822(18) -0.1985(3) -0.04180(14) 0.0405(6) Uani 1 1 d . . . F1 F 0.3423(7) -0.2875(11) -0.0478(5) 0.120(4) Uani 1 1 d . . . F2 F 0.2360(5) -0.1061(9) -0.1133(4) 0.091(3) Uani 1 1 d . . . F3 F 0.3502(5) -0.0809(9) 0.0107(4) 0.085(2) Uani 1 1 d . . . F4 F 0.1835(6) -0.3131(8) -0.0927(4) 0.079(2) Uani 1 1 d . . . F5 F 0.3030(5) -0.2921(7) 0.0311(3) 0.0599(16) Uani 1 1 d . . . F6 F 0.1945(4) -0.1128(6) -0.0339(4) 0.0571(15) Uani 1 1 d . . . Cl1 Cl -0.0775(3) -0.3503(6) -0.2605(2) 0.1099(15) Uani 1 1 d . . . Cl2 Cl 0.0754(3) -0.4369(7) -0.2713(3) 0.131(2) Uani 1 1 d . . . C24 C -0.0356(11) -0.473(2) -0.2948(10) 0.107(5) Uani 1 1 d . . . H24A H -0.0345 -0.5702 -0.2759 0.128 Uiso 1 1 calc R . . H24B H -0.0828 -0.4754 -0.3505 0.128 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 Ag 0.0226(3) 0.0337(3) 0.0240(3) 0.0006(3) 0.0126(2) -0.0029(3) S1 0.0284(10) 0.0331(11) 0.0315(10) 0.0023(9) 0.0193(9) 0.0009(8) S2 0.0306(10) 0.0282(11) 0.0314(11) 0.0038(9) 0.0152(9) 0.0027(8) O1 0.020(3) 0.026(3) 0.033(3) 0.000(2) 0.015(2) 0.002(2) O2 0.021(3) 0.026(3) 0.030(3) -0.003(2) 0.012(2) 0.001(2) N1 0.018(3) 0.014(3) 0.032(3) 0.004(2) 0.014(3) 0.006(2) C1 0.023(4) 0.029(4) 0.029(4) -0.005(3) 0.013(3) -0.001(3) C2 0.013(3) 0.017(4) 0.031(4) -0.001(3) 0.007(3) -0.010(3) C3 0.028(4) 0.019(4) 0.034(4) 0.001(3) 0.018(4) -0.004(3) C4 0.028(4) 0.032(5) 0.040(5) 0.010(4) 0.010(4) 0.000(4) C5 0.026(4) 0.039(5) 0.059(6) 0.009(5) 0.019(5) 0.013(4) C6 0.034(5) 0.045(6) 0.067(7) -0.007(5) 0.037(5) -0.002(4) C7 0.026(4) 0.030(4) 0.039(4) -0.004(4) 0.021(4) -0.010(3) C8 0.026(4) 0.043(5) 0.041(5) 0.001(4) 0.020(4) -0.009(4) C9 0.042(5) 0.050(6) 0.026(4) 0.011(4) 0.020(4) 0.007(4) C10 0.044(5) 0.056(6) 0.033(5) 0.007(4) 0.025(4) 0.006(4) C11 0.028(4) 0.035(5) 0.031(4) -0.004(4) 0.011(4) -0.003(4) C12 0.017(4) 0.026(4) 0.035(4) -0.004(3) 0.009(3) -0.003(3) C13 0.022(4) 0.030(5) 0.036(5) 0.005(4) 0.005(4) 0.000(3) C14 0.017(4) 0.033(5) 0.057(6) -0.007(4) 0.014(4) 0.002(3) C15 0.022(4) 0.033(5) 0.045(5) -0.012(4) 0.017(4) -0.003(3) C16 0.020(4) 0.025(4) 0.041(5) -0.005(4) 0.014(3) -0.005(3) C17 0.015(3) 0.018(4) 0.032(4) -0.006(3) 0.007(3) -0.006(3) C18 0.024(4) 0.021(4) 0.045(5) 0.003(4) 0.018(4) 0.000(3) C19 0.021(4) 0.019(4) 0.035(4) 0.006(3) 0.014(3) 0.009(3) C20 0.027(4) 0.034(5) 0.040(5) 0.003(4) 0.021(4) 0.002(4) C21 0.037(5) 0.045(5) 0.033(4) 0.003(4) 0.025(4) 0.005(4) C22 0.031(4) 0.033(5) 0.034(4) -0.003(4) 0.016(4) 0.005(4) C23 0.023(4) 0.016(4) 0.027(4) -0.001(3) 0.012(3) 0.006(3) P 0.0429(13) 0.0474(15) 0.0394(13) 0.0102(11) 0.0291(12) 0.0051(11) F1 0.144(8) 0.155(9) 0.135(7) 0.056(7) 0.124(7) 0.084(7) F2 0.076(5) 0.139(7) 0.065(4) 0.057(5) 0.046(4) 0.011(5) F3 0.044(4) 0.093(6) 0.091(5) 0.013(4) 0.026(4) -0.022(4) F4 0.101(5) 0.062(4) 0.056(4) -0.015(3) 0.037(4) -0.019(4) F5 0.082(4) 0.054(4) 0.049(3) 0.020(3) 0.042(3) 0.017(3) F6 0.051(3) 0.050(3) 0.084(4) 0.010(3) 0.048(3) 0.004(3) Cl1 0.085(3) 0.159(4) 0.083(3) -0.024(3) 0.049(2) -0.007(3) Cl2 0.068(2) 0.226(6) 0.092(3) -0.003(3) 0.044(2) -0.004(3) C24 0.085(11) 0.117(14) 0.132(14) -0.021(12) 0.072(11) -0.001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.250(6) . ? Ag S1 2.554(2) . ? Ag S2 2.557(2) . ? S1 C8 1.829(9) . ? S1 C9 1.830(8) . ? S2 C11 1.815(8) . ? S2 C10 1.820(9) . ? O1 C2 1.373(9) . ? O1 C1 1.427(9) . ? O2 C17 1.374(9) . ? O2 C18 1.419(10) . ? N1 C23 1.351(10) . ? N1 C19 1.352(10) . ? C1 C23 1.495(11) . ? C2 C3 1.395(11) . ? C2 C7 1.401(11) . ? C3 C4 1.380(12) . ? C4 C5 1.366(13) . ? C5 C6 1.372(14) . ? C6 C7 1.392(12) . ? C7 C8 1.500(12) . ? C9 C10 1.535(13) . ? C11 C12 1.505(12) . ? C12 C13 1.393(11) . ? C12 C17 1.397(11) . ? C13 C14 1.382(13) . ? C14 C15 1.371(13) . ? C15 C16 1.394(11) . ? C16 C17 1.380(11) . ? C18 C19 1.528(11) . ? C19 C20 1.375(11) . ? C20 C21 1.382(12) . ? C21 C22 1.384(12) . ? C22 C23 1.391(11) . ? P F1 1.574(7) . ? P F6 1.576(6) . ? P F2 1.580(6) . ? P F4 1.592(7) . ? P F3 1.595(7) . ? P F5 1.600(6) . ? Cl1 C24 1.737(16) . ? Cl2 C24 1.662(15) . ? 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 Ag S1 136.43(15) . . ? N1 Ag S2 137.23(15) . . ? S1 Ag S2 86.29(7) . . ? C8 S1 C9 100.3(4) . . ? C8 S1 Ag 98.7(3) . . ? C9 S1 Ag 97.8(3) . . ? C11 S2 C10 101.7(4) . . ? C11 S2 Ag 101.2(3) . . ? C10 S2 Ag 97.2(3) . . ? C2 O1 C1 119.5(6) . . ? C17 O2 C18 118.5(6) . . ? C23 N1 C19 118.0(7) . . ? C23 N1 Ag 121.6(5) . . ? C19 N1 Ag 120.2(5) . . ? O1 C1 C23 114.6(6) . . ? O1 C2 C3 124.4(7) . . ? O1 C2 C7 115.3(7) . . ? C3 C2 C7 120.2(7) . . ? C4 C3 C2 119.3(8) . . ? C5 C4 C3 121.1(8) . . ? C4 C5 C6 119.8(8) . . ? C5 C6 C7 121.4(9) . . ? C6 C7 C2 118.2(8) . . ? C6 C7 C8 121.9(8) . . ? C2 C7 C8 119.9(7) . . ? C7 C8 S1 107.7(6) . . ? C10 C9 S1 112.5(6) . . ? C9 C10 S2 110.8(6) . . ? C12 C11 S2 109.0(6) . . ? C13 C12 C17 117.6(8) . . ? C13 C12 C11 121.0(8) . . ? C17 C12 C11 121.3(7) . . ? C14 C13 C12 121.8(8) . . ? C15 C14 C13 119.5(8) . . ? C14 C15 C16 120.3(8) . . ? C17 C16 C15 119.7(8) . . ? O2 C17 C16 124.8(7) . . ? O2 C17 C12 114.2(7) . . ? C16 C17 C12 121.0(7) . . ? O2 C18 C19 113.8(6) . . ? N1 C19 C20 122.7(7) . . ? N1 C19 C18 116.6(7) . . ? C20 C19 C18 120.7(7) . . ? C19 C20 C21 119.4(8) . . ? C20 C21 C22 118.5(8) . . ? C21 C22 C23 119.6(8) . . ? N1 C23 C22 121.7(7) . . ? N1 C23 C1 118.9(7) . . ? C22 C23 C1 119.2(7) . . ? F1 P F6 178.3(4) . . ? F1 P F2 91.0(4) . . ? F6 P F2 90.7(4) . . ? F1 P F4 91.2(5) . . ? F6 P F4 88.4(4) . . ? F2 P F4 91.5(4) . . ? F1 P F3 91.4(5) . . ? F6 P F3 88.9(4) . . ? F2 P F3 89.3(4) . . ? F4 P F3 177.2(4) . . ? F1 P F5 88.1(4) . . ? F6 P F5 90.2(3) . . ? F2 P F5 178.9(4) . . ? F4 P F5 89.2(4) . . ? F3 P F5 90.0(4) . . ? Cl2 C24 Cl1 114.6(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.303 _refine_diff_density_min -1.394 _refine_diff_density_rms 0.159 ######################################################################## data_Complex1b _database_code_depnum_ccdc_archive 'CCDC 750354' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H23 Ag Cl N O6 S2' _chemical_formula_weight 616.86 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.6205(6) _cell_length_b 19.9138(12) _cell_length_c 12.7424(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.0350(10) _cell_angle_gamma 90.00 _cell_volume 2357.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9317 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7172 _exptl_absorpt_correction_T_max 0.7972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14237 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5116 _reflns_number_gt 4433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+3.0537P] 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 5116 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Ag Ag 0.44598(3) 0.257914(11) 0.02866(2) 0.05453(9) Uani 1 1 d . . . Cl Cl 0.11869(8) 0.61761(4) 0.19627(6) 0.04794(17) Uani 1 1 d . . . S1 S 0.50351(8) 0.17995(4) -0.10640(6) 0.04572(17) Uani 1 1 d . . . S2 S 0.71017(8) 0.28446(4) 0.09885(6) 0.04645(17) Uani 1 1 d . . . O1 O 0.3726(2) 0.15567(9) 0.12724(15) 0.0415(4) Uani 1 1 d . . . O2 O 0.40337(19) 0.38892(9) 0.00063(15) 0.0386(4) Uani 1 1 d . . . O3 O 0.2651(3) 0.6265(2) 0.2526(2) 0.0969(10) Uani 1 1 d . . . O4 O 0.0721(3) 0.67307(13) 0.1249(2) 0.0672(6) Uani 1 1 d . . . O5 O 0.1028(3) 0.55726(14) 0.1343(2) 0.0833(8) Uani 1 1 d . . . O6 O 0.0306(3) 0.61475(14) 0.2711(2) 0.0781(8) Uani 1 1 d . . . N1 N 0.2728(2) 0.28907(11) 0.10357(17) 0.0357(5) Uani 1 1 d . . . C1 C 0.3139(3) 0.18452(14) 0.2093(2) 0.0457(6) Uani 1 1 d . . . H1A H 0.3932 0.1922 0.2752 0.055 Uiso 1 1 calc R . . H1B H 0.2469 0.1518 0.2283 0.055 Uiso 1 1 calc R . . C2 C 0.2826(3) 0.11910(12) 0.0451(2) 0.0382(6) Uani 1 1 d . . . C3 C 0.1366(3) 0.11134(14) 0.0336(2) 0.0450(6) Uani 1 1 d . . . H3B H 0.0909 0.1342 0.0809 0.054 Uiso 1 1 calc R . . C4 C 0.0578(4) 0.07003(16) -0.0474(3) 0.0538(8) Uani 1 1 d . . . H4B H -0.0426 0.0647 -0.0557 0.065 Uiso 1 1 calc R . . C5 C 0.1233(4) 0.03667(16) -0.1160(3) 0.0594(8) Uani 1 1 d . . . H5B H 0.0693 0.0068 -0.1694 0.071 Uiso 1 1 calc R . . C6 C 0.2678(4) 0.04667(15) -0.1072(2) 0.0524(7) Uani 1 1 d . . . H6B H 0.3115 0.0245 -0.1564 0.063 Uiso 1 1 calc R . . C7 C 0.3511(3) 0.08847(13) -0.0278(2) 0.0418(6) Uani 1 1 d . . . C8 C 0.5061(3) 0.10376(15) -0.0248(2) 0.0476(7) Uani 1 1 d . . . H8A H 0.5492 0.0659 -0.0558 0.057 Uiso 1 1 calc R . . H8B H 0.5632 0.1113 0.0509 0.057 Uiso 1 1 calc R . . C9 C 0.6905(3) 0.20473(18) -0.0901(3) 0.0541(8) Uani 1 1 d . . . H9A H 0.7397 0.1670 -0.1162 0.065 Uiso 1 1 calc R . . H9B H 0.6906 0.2431 -0.1395 0.065 Uiso 1 1 calc R . . C10 C 0.7806(3) 0.22424(16) 0.0198(3) 0.0531(7) Uani 1 1 d . . . H10A H 0.8726 0.2423 0.0106 0.064 Uiso 1 1 calc R . . H10B H 0.8037 0.1827 0.0636 0.064 Uiso 1 1 calc R . . C11 C 0.6974(3) 0.36479(14) 0.0252(2) 0.0423(6) Uani 1 1 d . . . H11A H 0.7930 0.3783 0.0170 0.051 Uiso 1 1 calc R . . H11B H 0.6304 0.3607 -0.0480 0.051 Uiso 1 1 calc R . . C12 C 0.6422(3) 0.41587(13) 0.0919(2) 0.0371(5) Uani 1 1 d . . . C13 C 0.7397(3) 0.45329(15) 0.1696(3) 0.0490(7) Uani 1 1 d . . . H13A H 0.8400 0.4470 0.1782 0.059 Uiso 1 1 calc R . . C14 C 0.6942(4) 0.49948(16) 0.2345(3) 0.0550(8) Uani 1 1 d . . . H14A H 0.7626 0.5243 0.2874 0.066 Uiso 1 1 calc R . . C15 C 0.5488(3) 0.50928(15) 0.2219(3) 0.0510(7) Uani 1 1 d . . . H15A H 0.5172 0.5411 0.2662 0.061 Uiso 1 1 calc R . . C16 C 0.4488(3) 0.47304(14) 0.1452(2) 0.0431(6) Uani 1 1 d . . . H16A H 0.3489 0.4800 0.1368 0.052 Uiso 1 1 calc R . . C17 C 0.4951(3) 0.42636(12) 0.0806(2) 0.0354(5) Uani 1 1 d . . . C18 C 0.2521(3) 0.39059(15) -0.0063(2) 0.0420(6) Uani 1 1 d . . . H18A H 0.1985 0.3728 -0.0779 0.050 Uiso 1 1 calc R . . H18B H 0.2221 0.4378 -0.0016 0.050 Uiso 1 1 calc R . . C19 C 0.2124(3) 0.35032(13) 0.0821(2) 0.0361(5) Uani 1 1 d . . . C20 C 0.1141(3) 0.37418(15) 0.1352(2) 0.0442(6) Uani 1 1 d . . . H20A H 0.0754 0.4181 0.1210 0.053 Uiso 1 1 calc R . . C21 C 0.0729(3) 0.33300(15) 0.2092(3) 0.0477(7) Uani 1 1 d . . . H21A H 0.0038 0.3481 0.2453 0.057 Uiso 1 1 calc R . . C22 C 0.1325(3) 0.27015(15) 0.2302(2) 0.0446(6) Uani 1 1 d . . . H22A H 0.1045 0.2410 0.2801 0.053 Uiso 1 1 calc R . . C23 C 0.2346(3) 0.25005(13) 0.1770(2) 0.0368(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 Ag 0.05466(15) 0.03709(12) 0.0859(2) -0.00030(11) 0.04348(14) 0.00171(9) Cl 0.0487(4) 0.0550(4) 0.0434(4) 0.0025(3) 0.0178(3) 0.0103(3) S1 0.0457(4) 0.0513(4) 0.0412(4) -0.0012(3) 0.0132(3) 0.0015(3) S2 0.0450(4) 0.0425(4) 0.0513(4) -0.0015(3) 0.0117(3) 0.0037(3) O1 0.0507(11) 0.0368(9) 0.0375(10) -0.0026(8) 0.0125(8) 0.0025(8) O2 0.0348(9) 0.0409(10) 0.0413(10) 0.0000(8) 0.0122(8) -0.0006(8) O3 0.0549(16) 0.149(3) 0.0757(19) -0.0115(19) -0.0030(14) 0.0183(17) O4 0.0745(16) 0.0663(15) 0.0649(15) 0.0186(12) 0.0254(13) 0.0120(12) O5 0.108(2) 0.0608(16) 0.092(2) -0.0189(14) 0.0451(17) 0.0023(15) O6 0.099(2) 0.0759(17) 0.0809(18) 0.0159(14) 0.0615(16) 0.0197(15) N1 0.0352(11) 0.0374(11) 0.0355(11) -0.0040(9) 0.0110(9) -0.0007(9) C1 0.0642(18) 0.0401(14) 0.0346(13) -0.0026(11) 0.0162(13) 0.0028(13) C2 0.0531(16) 0.0282(12) 0.0343(13) 0.0039(10) 0.0134(11) 0.0026(11) C3 0.0566(17) 0.0379(14) 0.0450(15) 0.0048(12) 0.0211(13) -0.0024(12) C4 0.0567(18) 0.0467(17) 0.0567(18) 0.0068(14) 0.0121(15) -0.0118(14) C5 0.080(2) 0.0441(17) 0.0504(18) -0.0047(14) 0.0106(16) -0.0139(16) C6 0.076(2) 0.0402(15) 0.0423(16) -0.0045(12) 0.0181(15) 0.0036(15) C7 0.0562(16) 0.0312(12) 0.0388(14) 0.0032(11) 0.0138(12) 0.0073(12) C8 0.0563(17) 0.0433(15) 0.0453(16) 0.0026(12) 0.0171(13) 0.0157(13) C9 0.0529(18) 0.063(2) 0.0548(18) -0.0040(15) 0.0287(15) 0.0044(15) C10 0.0434(16) 0.0485(17) 0.071(2) -0.0041(15) 0.0218(15) 0.0063(13) C11 0.0396(14) 0.0437(14) 0.0479(15) -0.0015(12) 0.0190(12) 0.0002(11) C12 0.0383(13) 0.0332(12) 0.0420(14) 0.0022(11) 0.0142(11) -0.0001(10) C13 0.0400(15) 0.0418(15) 0.0631(18) -0.0053(14) 0.0097(13) -0.0021(12) C14 0.0570(19) 0.0431(16) 0.0610(19) -0.0119(14) 0.0084(15) -0.0066(14) C15 0.0629(19) 0.0389(15) 0.0564(18) -0.0078(13) 0.0245(15) -0.0016(13) C16 0.0443(15) 0.0365(13) 0.0537(16) 0.0011(12) 0.0220(13) 0.0013(11) C17 0.0398(13) 0.0308(12) 0.0378(13) 0.0056(10) 0.0137(11) -0.0020(10) C18 0.0323(13) 0.0459(15) 0.0468(15) 0.0047(12) 0.0083(11) 0.0022(11) C19 0.0285(12) 0.0376(13) 0.0407(13) -0.0027(11) 0.0064(10) -0.0023(10) C20 0.0357(14) 0.0419(14) 0.0568(17) -0.0067(13) 0.0153(12) 0.0010(11) C21 0.0388(14) 0.0515(16) 0.0592(18) -0.0130(14) 0.0242(13) -0.0047(12) C22 0.0476(16) 0.0461(15) 0.0447(15) -0.0083(12) 0.0204(13) -0.0106(12) C23 0.0399(14) 0.0361(13) 0.0341(13) -0.0070(10) 0.0093(10) -0.0052(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.213(2) . ? Ag S1 2.4845(8) . ? Ag S2 2.5219(8) . ? Ag O1 2.5851(19) . ? Cl O3 1.416(3) . ? Cl O5 1.425(3) . ? Cl O4 1.427(2) . ? Cl O6 1.431(2) . ? S1 C9 1.824(3) . ? S1 C8 1.836(3) . ? S2 C10 1.807(3) . ? S2 C11 1.843(3) . ? O1 C2 1.380(3) . ? O1 C1 1.431(3) . ? O2 C17 1.381(3) . ? O2 C18 1.436(3) . ? N1 C23 1.339(3) . ? N1 C19 1.348(3) . ? C1 C23 1.513(4) . ? C2 C3 1.382(4) . ? C2 C7 1.410(4) . ? C3 C4 1.382(4) . ? C4 C5 1.374(5) . ? C5 C6 1.380(5) . ? C6 C7 1.392(4) . ? C7 C8 1.513(4) . ? C9 C10 1.495(5) . ? C11 C12 1.508(4) . ? C12 C13 1.391(4) . ? C12 C17 1.400(4) . ? C13 C14 1.382(4) . ? C14 C15 1.380(4) . ? C15 C16 1.383(4) . ? C16 C17 1.389(4) . ? C18 C19 1.510(4) . ? C19 C20 1.381(4) . ? C20 C21 1.384(4) . ? C21 C22 1.374(4) . ? C22 C23 1.389(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 Ag S1 143.32(6) . . ? N1 Ag S2 126.19(6) . . ? S1 Ag S2 89.51(3) . . ? N1 Ag O1 71.34(7) . . ? S1 Ag O1 88.99(4) . . ? S2 Ag O1 111.71(5) . . ? O3 Cl O5 109.7(2) . . ? O3 Cl O4 109.4(2) . . ? O5 Cl O4 109.17(17) . . ? O3 Cl O6 110.50(19) . . ? O5 Cl O6 109.81(18) . . ? O4 Cl O6 108.27(16) . . ? C9 S1 C8 106.91(15) . . ? C9 S1 Ag 98.18(10) . . ? C8 S1 Ag 95.57(9) . . ? C10 S2 C11 106.10(14) . . ? C10 S2 Ag 98.77(11) . . ? C11 S2 Ag 94.21(9) . . ? C2 O1 C1 118.5(2) . . ? C2 O1 Ag 104.12(14) . . ? C1 O1 Ag 104.35(15) . . ? C17 O2 C18 118.4(2) . . ? C23 N1 C19 119.0(2) . . ? C23 N1 Ag 120.84(17) . . ? C19 N1 Ag 119.96(17) . . ? O1 C1 C23 114.5(2) . . ? O1 C2 C3 124.1(2) . . ? O1 C2 C7 114.8(2) . . ? C3 C2 C7 121.2(3) . . ? C2 C3 C4 119.5(3) . . ? C5 C4 C3 120.6(3) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C7 121.6(3) . . ? C6 C7 C2 117.2(3) . . ? C6 C7 C8 121.1(3) . . ? C2 C7 C8 121.6(3) . . ? C7 C8 S1 106.48(19) . . ? C10 C9 S1 119.5(2) . . ? C9 C10 S2 119.0(2) . . ? C12 C11 S2 106.56(18) . . ? C13 C12 C17 118.1(2) . . ? C13 C12 C11 119.4(2) . . ? C17 C12 C11 122.5(2) . . ? C14 C13 C12 121.5(3) . . ? C15 C14 C13 119.6(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C17 119.8(3) . . ? O2 C17 C16 123.9(2) . . ? O2 C17 C12 115.5(2) . . ? C16 C17 C12 120.6(2) . . ? O2 C18 C19 113.0(2) . . ? N1 C19 C20 121.7(2) . . ? N1 C19 C18 116.9(2) . . ? C20 C19 C18 121.3(2) . . ? C19 C20 C21 118.9(3) . . ? C22 C21 C20 119.6(3) . . ? C21 C22 C23 118.7(3) . . ? N1 C23 C22 122.0(2) . . ? N1 C23 C1 118.7(2) . . ? C22 C23 C1 119.1(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.019 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.069 ######################################################################## data_Complex2 _database_code_depnum_ccdc_archive 'CCDC 750355' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Ag F6 N2 O4 P S4' _chemical_formula_weight 1071.93 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' P P 0.1023 0.0942 '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' F F 0.0171 0.0103 '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 13.5110(12) _cell_length_b 13.8785(12) _cell_length_c 13.9628(12) _cell_angle_alpha 69.590(2) _cell_angle_beta 66.2200(10) _cell_angle_gamma 77.622(2) _cell_volume 2237.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5620 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7548 _exptl_absorpt_correction_T_max 0.8653 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18014 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8699 _reflns_number_gt 7716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+3.8484P] 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 8699 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _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 Ag Ag 0.51146(2) 0.18538(2) 0.10365(2) 0.02884(9) Uani 1 1 d . . . P P 0.13336(8) -0.35481(7) 0.68531(7) 0.0270(2) Uani 1 1 d . . . F1 F 0.2337(2) -0.4337(3) 0.6987(3) 0.0828(11) Uani 1 1 d . . . F2 F 0.0341(3) -0.2748(3) 0.6735(3) 0.0914(13) Uani 1 1 d . . . F3 F 0.0892(3) -0.4341(3) 0.6586(2) 0.0860(12) Uani 1 1 d . . . F4 F 0.0666(2) -0.4029(2) 0.81299(19) 0.0551(7) Uani 1 1 d . . . F5 F 0.1774(3) -0.2746(3) 0.7132(3) 0.0863(12) Uani 1 1 d . . . F6 F 0.2006(2) -0.3082(2) 0.55927(18) 0.0468(6) Uani 1 1 d . . . S1 S 0.52505(7) 0.21223(6) 0.27327(7) 0.02353(18) Uani 1 1 d . . . S2 S 0.66617(9) 0.35030(7) 0.00747(7) 0.0336(2) Uani 1 1 d . . . S3 S 0.47143(7) -0.02523(6) 0.20072(7) 0.02335(18) Uani 1 1 d . . . S4 S 0.67313(7) 0.09167(6) -0.03247(7) 0.02393(18) Uani 1 1 d . . . O1 O 0.28878(19) 0.19376(18) 0.25205(19) 0.0250(5) Uani 1 1 d . . . O2 O 0.5534(2) 0.42632(19) -0.1603(2) 0.0305(6) Uani 1 1 d . . . O3 O 0.73779(18) -0.15202(18) 0.27687(19) 0.0248(5) Uani 1 1 d . . . O4 O 0.92082(18) -0.05898(19) -0.1343(2) 0.0284(5) Uani 1 1 d . . . N1 N 0.3784(2) 0.2638(2) 0.0158(2) 0.0201(6) Uani 1 1 d . . . N2 N 0.9352(2) -0.1515(2) 0.0836(2) 0.0248(6) Uani 1 1 d . . . C1 C 0.2411(3) 0.1753(3) 0.1861(3) 0.0243(7) Uani 1 1 d . . . H1A H 0.1611 0.1784 0.2224 0.029 Uiso 1 1 calc R . . H1B H 0.2673 0.1058 0.1764 0.029 Uiso 1 1 calc R . . C2 C 0.2807(3) 0.1193(3) 0.3500(3) 0.0233(7) Uani 1 1 d . . . C3 C 0.2298(3) 0.0293(3) 0.3879(3) 0.0268(7) Uani 1 1 d . . . H3A H 0.1953 0.0170 0.3464 0.032 Uiso 1 1 calc R . . C4 C 0.2293(3) -0.0426(3) 0.4863(3) 0.0294(8) Uani 1 1 d . . . H4A H 0.1952 -0.1045 0.5118 0.035 Uiso 1 1 calc R . . C5 C 0.2787(3) -0.0240(3) 0.5475(3) 0.0325(8) Uani 1 1 d . . . H5A H 0.2780 -0.0730 0.6152 0.039 Uiso 1 1 calc R . . C6 C 0.3288(3) 0.0659(3) 0.5097(3) 0.0294(8) Uani 1 1 d . . . H6A H 0.3629 0.0778 0.5517 0.035 Uiso 1 1 calc R . . C7 C 0.3303(3) 0.1395(3) 0.4113(3) 0.0245(7) Uani 1 1 d . . . C8 C 0.3880(3) 0.2352(3) 0.3681(3) 0.0249(7) Uani 1 1 d . . . H8A H 0.3919 0.2528 0.4293 0.030 Uiso 1 1 calc R . . H8B H 0.3480 0.2937 0.3298 0.030 Uiso 1 1 calc R . . C9 C 0.5741(3) 0.3382(3) 0.2293(3) 0.0302(8) Uani 1 1 d . . . H9A H 0.5192 0.3925 0.2089 0.036 Uiso 1 1 calc R . . H9B H 0.5858 0.3492 0.2901 0.036 Uiso 1 1 calc R . . C10 C 0.6789(3) 0.3453(3) 0.1326(3) 0.0310(8) Uani 1 1 d . . . H10A H 0.7294 0.2849 0.1511 0.037 Uiso 1 1 calc R . . H10B H 0.7120 0.4079 0.1198 0.037 Uiso 1 1 calc R . . C11 C 0.6668(3) 0.4878(3) -0.0696(3) 0.0281(8) Uani 1 1 d . . . H11A H 0.5922 0.5220 -0.0490 0.034 Uiso 1 1 calc R . . H11B H 0.7129 0.5221 -0.0535 0.034 Uiso 1 1 calc R . . C12 C 0.7113(3) 0.4951(3) -0.1897(3) 0.0264(7) Uani 1 1 d . . . C13 C 0.8100(3) 0.5354(3) -0.2599(3) 0.0354(9) Uani 1 1 d . . . H13A H 0.8488 0.5628 -0.2331 0.042 Uiso 1 1 calc R . . C14 C 0.8524(3) 0.5361(3) -0.3685(3) 0.0420(10) Uani 1 1 d . . . H14A H 0.9194 0.5647 -0.4159 0.050 Uiso 1 1 calc R . . C15 C 0.7975(3) 0.4954(3) -0.4076(3) 0.0410(10) Uani 1 1 d . . . H15A H 0.8278 0.4943 -0.4816 0.049 Uiso 1 1 calc R . . C16 C 0.6982(3) 0.4559(3) -0.3397(3) 0.0367(9) Uani 1 1 d . . . H16A H 0.6600 0.4284 -0.3670 0.044 Uiso 1 1 calc R . . C17 C 0.6553(3) 0.4572(3) -0.2320(3) 0.0261(7) Uani 1 1 d . . . C18 C 0.5230(3) 0.3337(3) -0.1585(3) 0.0290(8) Uani 1 1 d . . . H18A H 0.5674 0.2734 -0.1283 0.035 Uiso 1 1 calc R . . H18B H 0.5340 0.3352 -0.2335 0.035 Uiso 1 1 calc R . . C19 C 0.4048(3) 0.3270(2) -0.0870(3) 0.0229(7) Uani 1 1 d . . . C20 C 0.3275(3) 0.3853(3) -0.1312(3) 0.0300(8) Uani 1 1 d . . . H20A H 0.3492 0.4282 -0.2048 0.036 Uiso 1 1 calc R . . C21 C 0.2191(3) 0.3801(3) -0.0669(3) 0.0342(9) Uani 1 1 d . . . H21A H 0.1652 0.4209 -0.0949 0.041 Uiso 1 1 calc R . . C22 C 0.1899(3) 0.3147(3) 0.0388(3) 0.0288(8) Uani 1 1 d . . . H22A H 0.1157 0.3098 0.0848 0.035 Uiso 1 1 calc R . . C23 C 0.2720(3) 0.2558(3) 0.0769(3) 0.0223(7) Uani 1 1 d . . . C24 C 0.8462(3) -0.1880(3) 0.2784(3) 0.0284(8) Uani 1 1 d . . . H24A H 0.8420 -0.2454 0.3459 0.034 Uiso 1 1 calc R . . H24B H 0.8793 -0.1313 0.2791 0.034 Uiso 1 1 calc R . . C25 C 0.6574(3) -0.2184(3) 0.3342(3) 0.0230(7) Uani 1 1 d . . . C26 C 0.6757(3) -0.3246(3) 0.3741(3) 0.0311(8) Uani 1 1 d . . . H26A H 0.7477 -0.3565 0.3588 0.037 Uiso 1 1 calc R . . C27 C 0.5877(4) -0.3838(3) 0.4368(3) 0.0374(9) Uani 1 1 d . . . H27A H 0.6001 -0.4564 0.4644 0.045 Uiso 1 1 calc R . . C28 C 0.4825(3) -0.3384(3) 0.4594(3) 0.0388(9) Uani 1 1 d . . . H28A H 0.4229 -0.3791 0.5045 0.047 Uiso 1 1 calc R . . C29 C 0.4651(3) -0.2334(3) 0.4158(3) 0.0320(8) Uani 1 1 d . . . H29A H 0.3928 -0.2025 0.4291 0.038 Uiso 1 1 calc R . . C30 C 0.5511(3) -0.1719(3) 0.3530(3) 0.0228(7) Uani 1 1 d . . . C31 C 0.5284(3) -0.0573(3) 0.3074(3) 0.0231(7) Uani 1 1 d . . . H31A H 0.5968 -0.0238 0.2769 0.028 Uiso 1 1 calc R . . H31B H 0.4770 -0.0293 0.3676 0.028 Uiso 1 1 calc R . . C32 C 0.5767(3) -0.0865(3) 0.1054(3) 0.0249(7) Uani 1 1 d . . . H32A H 0.5880 -0.1602 0.1448 0.030 Uiso 1 1 calc R . . H32B H 0.5504 -0.0836 0.0476 0.030 Uiso 1 1 calc R . . C33 C 0.6856(3) -0.0410(3) 0.0505(3) 0.0239(7) Uani 1 1 d . . . H33A H 0.7383 -0.0827 0.0037 0.029 Uiso 1 1 calc R . . H33B H 0.7134 -0.0435 0.1070 0.029 Uiso 1 1 calc R . . C34 C 0.8129(3) 0.1257(3) -0.0814(3) 0.0264(7) Uani 1 1 d . . . H34A H 0.8114 0.1958 -0.0773 0.032 Uiso 1 1 calc R . . H34B H 0.8505 0.0768 -0.0331 0.032 Uiso 1 1 calc R . . C35 C 0.8750(3) 0.1226(3) -0.1969(3) 0.0253(7) Uani 1 1 d . . . C36 C 0.8801(3) 0.2118(3) -0.2839(3) 0.0357(9) Uani 1 1 d . . . H36A H 0.8443 0.2748 -0.2695 0.043 Uiso 1 1 calc R . . C37 C 0.9365(3) 0.2104(4) -0.3911(3) 0.0431(11) Uani 1 1 d . . . H37A H 0.9392 0.2721 -0.4495 0.052 Uiso 1 1 calc R . . C38 C 0.9886(3) 0.1193(4) -0.4129(3) 0.0412(10) Uani 1 1 d . . . H38A H 1.0270 0.1181 -0.4865 0.049 Uiso 1 1 calc R . . C39 C 0.9849(3) 0.0293(3) -0.3274(3) 0.0335(8) Uani 1 1 d . . . H39A H 1.0213 -0.0334 -0.3424 0.040 Uiso 1 1 calc R . . C40 C 0.9282(3) 0.0310(3) -0.2205(3) 0.0255(7) Uani 1 1 d . . . C41 C 1.0198(3) -0.0955(3) -0.1137(3) 0.0332(8) Uani 1 1 d . . . H41A H 1.0497 -0.0383 -0.1100 0.040 Uiso 1 1 calc R . . H41B H 1.0739 -0.1222 -0.1737 0.040 Uiso 1 1 calc R . . C42 C 0.9965(3) -0.1799(3) -0.0069(3) 0.0256(7) Uani 1 1 d . . . C43 C 1.0399(3) -0.2809(3) -0.0037(3) 0.0317(8) Uani 1 1 d . . . H43A H 1.0806 -0.2990 -0.0694 0.038 Uiso 1 1 calc R . . C44 C 1.0226(3) -0.3543(3) 0.0970(3) 0.0348(9) Uani 1 1 d . . . H44A H 1.0531 -0.4234 0.1016 0.042 Uiso 1 1 calc R . . C45 C 0.9606(3) -0.3262(3) 0.1904(3) 0.0324(8) Uani 1 1 d . . . H45A H 0.9481 -0.3753 0.2605 0.039 Uiso 1 1 calc R . . C46 C 0.9166(3) -0.2243(3) 0.1802(3) 0.0255(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02434(15) 0.03750(17) 0.02970(15) -0.01562(12) -0.01293(11) 0.00361(11) P 0.0297(5) 0.0263(5) 0.0243(5) -0.0041(4) -0.0115(4) -0.0031(4) F1 0.0524(18) 0.087(2) 0.0620(19) 0.0074(17) -0.0169(15) 0.0293(16) F2 0.058(2) 0.105(3) 0.070(2) -0.0073(19) -0.0215(17) 0.0398(19) F3 0.122(3) 0.097(3) 0.0532(18) -0.0232(17) -0.0104(18) -0.076(2) F4 0.0679(18) 0.0510(16) 0.0281(12) -0.0071(11) -0.0017(12) -0.0075(13) F5 0.146(3) 0.077(2) 0.0604(19) -0.0105(17) -0.045(2) -0.059(2) F6 0.0493(15) 0.0544(15) 0.0273(12) 0.0027(11) -0.0109(11) -0.0164(12) S1 0.0251(4) 0.0239(4) 0.0233(4) -0.0065(3) -0.0096(3) -0.0043(3) S2 0.0501(6) 0.0250(5) 0.0261(5) -0.0066(4) -0.0111(4) -0.0107(4) S3 0.0201(4) 0.0258(4) 0.0247(4) -0.0086(3) -0.0087(3) 0.0004(3) S4 0.0190(4) 0.0234(4) 0.0262(4) -0.0058(3) -0.0078(3) 0.0015(3) O1 0.0278(13) 0.0268(13) 0.0239(12) -0.0041(10) -0.0138(10) -0.0057(10) O2 0.0244(13) 0.0329(14) 0.0366(14) -0.0175(11) -0.0061(11) -0.0050(10) O3 0.0205(12) 0.0251(12) 0.0253(12) -0.0046(10) -0.0079(10) -0.0003(9) O4 0.0177(12) 0.0304(13) 0.0331(13) -0.0061(11) -0.0080(10) -0.0013(10) N1 0.0221(14) 0.0179(13) 0.0255(14) -0.0095(11) -0.0118(11) 0.0001(10) N2 0.0199(14) 0.0257(15) 0.0291(15) -0.0063(12) -0.0116(12) 0.0001(11) C1 0.0210(17) 0.0297(18) 0.0276(17) -0.0085(15) -0.0134(14) -0.0034(13) C2 0.0182(16) 0.0269(18) 0.0231(16) -0.0085(14) -0.0061(13) 0.0007(13) C3 0.0209(17) 0.035(2) 0.0258(17) -0.0114(15) -0.0069(14) -0.0046(14) C4 0.0244(18) 0.0271(18) 0.0273(18) -0.0043(15) -0.0016(14) -0.0055(14) C5 0.032(2) 0.037(2) 0.0193(17) -0.0042(15) -0.0038(15) -0.0021(16) C6 0.0299(19) 0.038(2) 0.0204(17) -0.0102(15) -0.0074(14) -0.0031(15) C7 0.0235(17) 0.0260(17) 0.0231(17) -0.0106(14) -0.0056(14) 0.0002(13) C8 0.0259(18) 0.0299(18) 0.0208(16) -0.0132(14) -0.0055(14) -0.0023(14) C9 0.034(2) 0.0292(19) 0.0305(19) -0.0116(15) -0.0101(16) -0.0077(15) C10 0.033(2) 0.032(2) 0.0318(19) -0.0059(16) -0.0139(16) -0.0105(15) C11 0.0281(19) 0.0230(18) 0.0351(19) -0.0096(15) -0.0113(15) -0.0044(14) C12 0.0239(17) 0.0193(16) 0.0312(18) -0.0031(14) -0.0099(14) 0.0006(13) C13 0.028(2) 0.034(2) 0.041(2) -0.0023(17) -0.0144(17) -0.0056(15) C14 0.031(2) 0.046(2) 0.035(2) 0.0010(19) -0.0053(17) -0.0101(18) C15 0.041(2) 0.045(2) 0.0237(19) -0.0004(17) -0.0070(17) -0.0010(18) C16 0.037(2) 0.042(2) 0.030(2) -0.0058(17) -0.0146(17) -0.0029(17) C17 0.0227(17) 0.0240(17) 0.0290(18) -0.0053(14) -0.0106(14) 0.0021(13) C18 0.035(2) 0.0213(17) 0.0260(18) -0.0042(14) -0.0084(15) -0.0019(14) C19 0.0305(18) 0.0163(16) 0.0264(17) -0.0083(13) -0.0121(14) -0.0036(13) C20 0.043(2) 0.0210(17) 0.0319(19) -0.0025(15) -0.0231(17) -0.0044(15) C21 0.040(2) 0.0267(19) 0.047(2) -0.0044(17) -0.0319(19) -0.0025(16) C22 0.0239(18) 0.0291(19) 0.041(2) -0.0096(16) -0.0201(16) -0.0027(14) C23 0.0252(17) 0.0217(16) 0.0284(17) -0.0118(14) -0.0144(14) -0.0013(13) C24 0.0254(18) 0.0324(19) 0.0306(19) -0.0084(15) -0.0154(15) 0.0006(14) C25 0.0284(18) 0.0225(17) 0.0173(15) -0.0047(13) -0.0075(13) -0.0039(13) C26 0.037(2) 0.0241(18) 0.034(2) -0.0090(15) -0.0167(17) 0.0026(15) C27 0.052(3) 0.0195(18) 0.041(2) -0.0012(16) -0.0217(19) -0.0075(16) C28 0.042(2) 0.034(2) 0.042(2) -0.0094(18) -0.0127(19) -0.0142(17) C29 0.0279(19) 0.032(2) 0.036(2) -0.0101(16) -0.0103(16) -0.0052(15) C30 0.0267(18) 0.0228(17) 0.0223(16) -0.0082(13) -0.0113(14) -0.0012(13) C31 0.0259(17) 0.0242(17) 0.0224(16) -0.0107(14) -0.0098(14) 0.0005(13) C32 0.0301(18) 0.0202(16) 0.0265(17) -0.0114(14) -0.0093(14) -0.0005(13) C33 0.0222(17) 0.0226(17) 0.0235(17) -0.0061(14) -0.0083(14) 0.0041(13) C34 0.0207(17) 0.0279(18) 0.0326(19) -0.0120(15) -0.0076(14) -0.0043(13) C35 0.0203(17) 0.0293(18) 0.0272(18) -0.0086(14) -0.0092(14) -0.0018(13) C36 0.0268(19) 0.036(2) 0.036(2) -0.0011(17) -0.0123(16) -0.0009(15) C37 0.033(2) 0.052(3) 0.032(2) 0.0076(19) -0.0157(18) -0.0067(19) C38 0.028(2) 0.069(3) 0.0256(19) -0.011(2) -0.0063(16) -0.0130(19) C39 0.0235(18) 0.048(2) 0.032(2) -0.0198(18) -0.0047(15) -0.0055(16) C40 0.0143(16) 0.0332(19) 0.0300(18) -0.0090(15) -0.0078(14) -0.0047(13) C41 0.0182(17) 0.046(2) 0.033(2) -0.0116(17) -0.0096(15) 0.0017(15) C42 0.0135(15) 0.0345(19) 0.0321(18) -0.0118(15) -0.0103(14) -0.0012(13) C43 0.0187(17) 0.039(2) 0.042(2) -0.0211(18) -0.0100(16) 0.0001(15) C44 0.0240(19) 0.0258(19) 0.058(3) -0.0168(18) -0.0171(18) 0.0042(14) C45 0.0259(19) 0.0285(19) 0.041(2) -0.0031(16) -0.0169(17) -0.0019(14) C46 0.0177(16) 0.0288(18) 0.0339(19) -0.0078(15) -0.0146(14) -0.0011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.435(3) . ? Ag S1 2.6033(9) . ? Ag S4 2.6894(9) . ? Ag S3 2.8277(9) . ? P F3 1.568(3) . ? P F2 1.572(3) . ? P F1 1.580(3) . ? P F6 1.584(2) . ? P F5 1.588(3) . ? P F4 1.603(2) . ? S1 C9 1.814(4) . ? S1 C8 1.830(3) . ? S2 C10 1.800(4) . ? S2 C11 1.835(4) . ? S3 C32 1.806(3) . ? S3 C31 1.823(3) . ? S4 C33 1.816(3) . ? S4 C34 1.837(3) . ? O1 C2 1.375(4) . ? O1 C1 1.430(4) . ? O2 C17 1.387(4) . ? O2 C18 1.420(4) . ? O3 C25 1.372(4) . ? O3 C24 1.449(4) . ? O4 C40 1.388(4) . ? O4 C41 1.430(4) . ? N1 C19 1.342(4) . ? N1 C23 1.350(4) . ? N2 C46 1.337(4) . ? N2 C42 1.343(5) . ? C1 C23 1.499(5) . ? C2 C3 1.388(5) . ? C2 C7 1.404(5) . ? C3 C4 1.386(5) . ? C4 C5 1.389(5) . ? C5 C6 1.382(5) . ? C6 C7 1.392(5) . ? C7 C8 1.497(5) . ? C9 C10 1.504(5) . ? C11 C12 1.509(5) . ? C12 C13 1.391(5) . ? C12 C17 1.395(5) . ? C13 C14 1.385(6) . ? C14 C15 1.374(6) . ? C15 C16 1.389(6) . ? C16 C17 1.382(5) . ? C18 C19 1.507(5) . ? C19 C20 1.391(5) . ? C20 C21 1.376(6) . ? C21 C22 1.381(5) . ? C22 C23 1.401(5) . ? C24 C46 1.504(5) . ? C25 C26 1.387(5) . ? C25 C30 1.402(5) . ? C26 C27 1.390(6) . ? C27 C28 1.382(6) . ? C28 C29 1.378(5) . ? C29 C30 1.390(5) . ? C30 C31 1.508(5) . ? C32 C33 1.517(5) . ? C34 C35 1.499(5) . ? C35 C36 1.390(5) . ? C35 C40 1.398(5) . ? C36 C37 1.384(6) . ? C37 C38 1.379(7) . ? C38 C39 1.388(6) . ? C39 C40 1.382(5) . ? C41 C42 1.502(5) . ? C42 C43 1.391(5) . ? C43 C44 1.381(6) . ? C44 C45 1.374(6) . ? C45 C46 1.394(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag S1 129.10(7) . . ? N1 Ag S4 106.57(7) . . ? S1 Ag S4 123.24(3) . . ? N1 Ag S3 105.35(7) . . ? S1 Ag S3 96.17(3) . . ? S4 Ag S3 76.64(3) . . ? F3 P F2 90.6(2) . . ? F3 P F1 90.7(2) . . ? F2 P F1 178.6(2) . . ? F3 P F6 90.37(15) . . ? F2 P F6 90.18(16) . . ? F1 P F6 90.21(15) . . ? F3 P F5 179.6(2) . . ? F2 P F5 89.3(2) . . ? F1 P F5 89.4(2) . . ? F6 P F5 90.02(16) . . ? F3 P F4 89.64(16) . . ? F2 P F4 90.53(17) . . ? F1 P F4 89.08(16) . . ? F6 P F4 179.29(16) . . ? F5 P F4 89.97(17) . . ? C9 S1 C8 100.05(17) . . ? C9 S1 Ag 107.12(12) . . ? C8 S1 Ag 108.94(11) . . ? C10 S2 C11 104.36(17) . . ? C32 S3 C31 100.13(16) . . ? C32 S3 Ag 102.92(11) . . ? C31 S3 Ag 99.37(11) . . ? C33 S4 C34 100.47(16) . . ? C33 S4 Ag 104.69(11) . . ? C34 S4 Ag 119.75(12) . . ? C2 O1 C1 116.6(3) . . ? C17 O2 C18 118.0(3) . . ? C25 O3 C24 119.2(3) . . ? C40 O4 C41 113.7(3) . . ? C19 N1 C23 117.7(3) . . ? C19 N1 Ag 122.7(2) . . ? C23 N1 Ag 118.9(2) . . ? C46 N2 C42 117.7(3) . . ? O1 C1 C23 108.8(3) . . ? O1 C2 C3 124.5(3) . . ? O1 C2 C7 114.8(3) . . ? C3 C2 C7 120.7(3) . . ? C4 C3 C2 120.0(3) . . ? C3 C4 C5 120.0(3) . . ? C6 C5 C4 119.8(3) . . ? C5 C6 C7 121.4(3) . . ? C6 C7 C2 118.1(3) . . ? C6 C7 C8 121.6(3) . . ? C2 C7 C8 120.3(3) . . ? C7 C8 S1 108.7(2) . . ? C10 C9 S1 109.9(3) . . ? C9 C10 S2 114.9(3) . . ? C12 C11 S2 107.4(2) . . ? C13 C12 C17 118.2(3) . . ? C13 C12 C11 121.7(3) . . ? C17 C12 C11 120.0(3) . . ? C14 C13 C12 120.8(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 120.4(4) . . ? C17 C16 C15 119.3(4) . . ? C16 C17 O2 123.4(3) . . ? C16 C17 C12 121.2(3) . . ? O2 C17 C12 115.3(3) . . ? O2 C18 C19 106.8(3) . . ? N1 C19 C20 122.8(3) . . ? N1 C19 C18 118.7(3) . . ? C20 C19 C18 118.5(3) . . ? C21 C20 C19 119.3(3) . . ? C20 C21 C22 119.0(3) . . ? C21 C22 C23 118.7(3) . . ? N1 C23 C22 122.5(3) . . ? N1 C23 C1 118.3(3) . . ? C22 C23 C1 119.1(3) . . ? O3 C24 C46 111.2(3) . . ? O3 C25 C26 124.4(3) . . ? O3 C25 C30 115.4(3) . . ? C26 C25 C30 120.2(3) . . ? C25 C26 C27 119.4(3) . . ? C28 C27 C26 120.9(3) . . ? C29 C28 C27 119.2(4) . . ? C28 C29 C30 121.3(4) . . ? C29 C30 C25 118.8(3) . . ? C29 C30 C31 119.6(3) . . ? C25 C30 C31 121.6(3) . . ? C30 C31 S3 112.6(2) . . ? C33 C32 S3 116.1(2) . . ? C32 C33 S4 110.8(2) . . ? C35 C34 S4 111.7(2) . . ? C36 C35 C40 118.1(3) . . ? C36 C35 C34 120.4(3) . . ? C40 C35 C34 121.5(3) . . ? C37 C36 C35 121.2(4) . . ? C38 C37 C36 119.9(4) . . ? C37 C38 C39 120.0(4) . . ? C40 C39 C38 119.9(4) . . ? C39 C40 O4 120.6(3) . . ? C39 C40 C35 120.9(3) . . ? O4 C40 C35 118.5(3) . . ? O4 C41 C42 108.7(3) . . ? N2 C42 C43 122.8(3) . . ? N2 C42 C41 116.3(3) . . ? C43 C42 C41 120.9(3) . . ? C44 C43 C42 118.6(4) . . ? C45 C44 C43 119.2(3) . . ? C44 C45 C46 118.7(3) . . ? N2 C46 C45 122.9(3) . . ? N2 C46 C24 115.2(3) . . ? C45 C46 C24 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.249 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.089 ######################################################################## data_Complex3 _database_code_depnum_ccdc_archive 'CCDC 750356' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H23 Cl2 Hg N O10 S2' _chemical_formula_weight 809.03 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' Hg Hg -2.3894 9.2266 '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, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, 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, z+1/2' '-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+1/2, y+1/2, z' '-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' _cell_length_a 30.1951(15) _cell_length_b 12.3606(6) _cell_length_c 13.9210(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5195.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5177 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 6.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3632 _exptl_absorpt_correction_T_max 0.5692 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6730 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2179 _reflns_number_gt 1990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(8) _refine_ls_number_reflns 2179 _refine_ls_number_parameters 178 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.110 _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 Hg Hg 0.5000 0.0000 0.49989(3) 0.03188(10) Uani 1 2 d S . . Cl Cl 0.56575(5) 0.26372(10) 0.43315(13) 0.0357(3) Uani 1 1 d . . . S1 S 0.49617(4) 0.13938(12) 0.63135(10) 0.0319(3) Uani 1 1 d . . . O1 O 0.42897(11) 0.0884(3) 0.4399(3) 0.0275(8) Uani 1 1 d . . . O2 O 0.5495(4) 0.2343(5) 0.3370(6) 0.103(3) Uani 1 1 d . . . O3 O 0.6047(2) 0.3180(6) 0.4146(9) 0.134(4) Uani 1 1 d . . . O4 O 0.5317(3) 0.3185(6) 0.4729(6) 0.135(4) Uani 1 1 d . . . O5 O 0.57364(15) 0.1638(3) 0.4820(3) 0.0431(11) Uani 1 1 d . . . N N 0.5000 0.0000 0.3437(5) 0.0258(14) Uani 1 2 d S . . C1 C 0.41988(19) 0.0374(4) 0.3498(4) 0.0281(12) Uani 1 1 d . . . H1A H 0.3991 0.0825 0.3120 0.034 Uiso 1 1 calc R . . H1B H 0.4059 -0.0339 0.3608 0.034 Uiso 1 1 calc R . . C2 C 0.39423(16) 0.0959(4) 0.5062(4) 0.0253(10) Uani 1 1 d . . . C3 C 0.35355(17) 0.0498(4) 0.4903(5) 0.0291(11) Uani 1 1 d . . . H3B H 0.3479 0.0116 0.4324 0.035 Uiso 1 1 calc R . . C4 C 0.3204(2) 0.0597(5) 0.5602(5) 0.0346(13) Uani 1 1 d . . . H4B H 0.2925 0.0254 0.5511 0.042 Uiso 1 1 calc R . . C5 C 0.3284(2) 0.1200(5) 0.6433(5) 0.0372(14) Uani 1 1 d . . . H5B H 0.3058 0.1296 0.6900 0.045 Uiso 1 1 calc R . . C6 C 0.3700(2) 0.1658(4) 0.6568(4) 0.0351(13) Uani 1 1 d . . . H6A H 0.3757 0.2051 0.7140 0.042 Uiso 1 1 calc R . . C7 C 0.40335(19) 0.1554(4) 0.5883(4) 0.0282(12) Uani 1 1 d . . . C8 C 0.4462(2) 0.2144(5) 0.6031(5) 0.0370(14) Uani 1 1 d . . . H8A H 0.4415 0.2674 0.6554 0.044 Uiso 1 1 calc R . . H8B H 0.4522 0.2565 0.5439 0.044 Uiso 1 1 calc R . . C9 C 0.48264(19) 0.0461(4) 0.7277(4) 0.0270(12) Uani 1 1 d . . . H9A H 0.4831 0.0843 0.7902 0.032 Uiso 1 1 calc R . . H9B H 0.4526 0.0158 0.7178 0.032 Uiso 1 1 calc R . . C10 C 0.5000 0.0000 0.1453(7) 0.037(2) Uani 1 2 d S . . H10A H 0.5000 0.0000 0.0771 0.045 Uiso 1 2 calc SR . . C11 C 0.4617(2) 0.0239(4) 0.1951(5) 0.0335(13) Uani 1 1 d . . . H11A H 0.4352 0.0408 0.1617 0.040 Uiso 1 1 calc R . . C12 C 0.46256(19) 0.0230(4) 0.2951(4) 0.0259(12) 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 Hg 0.02481(14) 0.05349(16) 0.01734(13) 0.000 0.000 0.00091(17) Cl 0.0288(8) 0.0325(7) 0.0460(10) 0.0062(6) 0.0000(7) 0.0003(5) S1 0.0353(8) 0.0375(7) 0.0228(7) 0.0030(5) -0.0033(6) -0.0127(6) O1 0.0246(19) 0.0371(18) 0.0207(19) -0.0036(15) -0.0031(15) -0.0040(15) O2 0.169(9) 0.080(5) 0.059(5) -0.001(3) -0.022(5) 0.038(4) O3 0.081(5) 0.078(5) 0.243(12) 0.073(6) 0.024(6) -0.008(4) O4 0.166(8) 0.112(6) 0.127(8) 0.061(5) 0.091(6) 0.094(6) O5 0.045(3) 0.040(2) 0.044(3) 0.006(2) -0.007(2) 0.0067(18) N 0.030(4) 0.028(3) 0.019(3) 0.000 0.000 -0.008(3) C1 0.030(3) 0.034(3) 0.021(3) -0.003(2) -0.001(2) -0.006(2) C2 0.028(3) 0.027(2) 0.021(3) 0.002(2) 0.001(2) 0.0084(19) C3 0.030(3) 0.030(2) 0.028(3) 0.005(2) 0.005(2) 0.003(2) C4 0.031(3) 0.033(3) 0.040(3) 0.012(2) -0.007(3) 0.003(2) C5 0.038(4) 0.043(3) 0.030(3) 0.013(3) 0.011(3) 0.018(3) C6 0.047(4) 0.036(3) 0.023(3) 0.001(2) -0.003(3) 0.005(3) C7 0.036(3) 0.022(2) 0.026(3) 0.000(2) -0.007(2) 0.001(2) C8 0.049(4) 0.030(3) 0.032(4) -0.007(3) 0.000(3) 0.000(3) C9 0.027(3) 0.034(3) 0.020(3) 0.005(2) -0.001(2) -0.004(2) C10 0.050(6) 0.040(4) 0.021(4) 0.000 0.000 0.009(4) C11 0.038(4) 0.040(3) 0.022(3) 0.002(2) -0.003(3) -0.003(2) C12 0.028(3) 0.027(3) 0.023(3) -0.003(2) -0.003(2) -0.001(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 Hg N 2.174(7) . ? Hg S1 2.5161(15) . ? Hg S1 2.5161(15) 2_655 ? Hg O1 2.548(4) . ? Hg O1 2.548(4) 2_655 ? Cl O4 1.349(6) . ? Cl O3 1.378(6) . ? Cl O5 1.430(4) . ? Cl O2 1.471(9) . ? S1 C8 1.814(7) . ? S1 C9 1.816(5) . ? O1 C2 1.401(6) . ? O1 C1 1.430(6) . ? N C12 1.348(7) 2_655 ? N C12 1.348(7) . ? C1 C12 1.507(8) . ? C2 C3 1.372(7) . ? C2 C7 1.385(7) . ? C3 C4 1.401(9) . ? C4 C5 1.398(10) . ? C5 C6 1.388(9) . ? C6 C7 1.394(8) . ? C7 C8 1.501(9) . ? C9 C9 1.548(11) 2_655 ? C10 C11 1.381(8) 2_655 ? C10 C11 1.381(8) . ? C11 C12 1.392(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Hg S1 136.67(3) . . ? N Hg S1 136.67(3) . 2_655 ? S1 Hg S1 86.67(6) . 2_655 ? N Hg O1 70.87(9) . . ? S1 Hg O1 84.61(9) . . ? S1 Hg O1 124.81(9) 2_655 . ? N Hg O1 70.87(9) . 2_655 ? S1 Hg O1 124.81(9) . 2_655 ? S1 Hg O1 84.61(9) 2_655 2_655 ? O1 Hg O1 141.73(18) . 2_655 ? O4 Cl O3 118.8(6) . . ? O4 Cl O5 111.5(4) . . ? O3 Cl O5 111.5(4) . . ? O4 Cl O2 104.1(6) . . ? O3 Cl O2 103.6(7) . . ? O5 Cl O2 105.9(3) . . ? C8 S1 C9 107.4(3) . . ? C8 S1 Hg 103.3(2) . . ? C9 S1 Hg 96.47(19) . . ? C2 O1 C1 117.6(4) . . ? C2 O1 Hg 116.3(3) . . ? C1 O1 Hg 105.0(3) . . ? C12 N C12 119.7(7) 2_655 . ? C12 N Hg 120.1(4) 2_655 . ? C12 N Hg 120.1(4) . . ? O1 C1 C12 109.3(4) . . ? C3 C2 C7 122.1(5) . . ? C3 C2 O1 122.4(5) . . ? C7 C2 O1 115.5(5) . . ? C2 C3 C4 119.4(6) . . ? C5 C4 C3 119.8(6) . . ? C6 C5 C4 119.1(6) . . ? C5 C6 C7 121.6(6) . . ? C2 C7 C6 118.0(5) . . ? C2 C7 C8 122.9(5) . . ? C6 C7 C8 119.1(5) . . ? C7 C8 S1 119.9(4) . . ? C9 C9 S1 108.4(4) 2_655 . ? C11 C10 C11 119.7(9) 2_655 . ? C10 C11 C12 119.0(6) . . ? N C12 C11 121.3(6) . . ? N C12 C1 119.2(5) . . ? C11 C12 C1 119.2(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.150 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.095 ######################################################################## data_Complex4 _database_code_depnum_ccdc_archive 'CCDC 750357' #TrackingRef 'cifs.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 Cl2 Hg N O3 S2' _chemical_formula_weight 699.05 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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' _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 10.2253(7) _cell_length_b 8.3445(6) _cell_length_c 29.2722(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.355(3) _cell_angle_gamma 90.00 _cell_volume 2448.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4631 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.22 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 6.700 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2026 _exptl_absorpt_correction_T_max 0.6162 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17374 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.00 _reflns_number_total 5900 _reflns_number_gt 3945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.7491P] 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 5900 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Hg Hg 0.38459(4) -0.07414(4) -0.075774(12) 0.04998(15) Uani 1 1 d . A . Cl1 Cl 0.1419(3) -0.0476(3) -0.11411(9) 0.0620(7) Uani 1 1 d . . . Cl2 Cl 0.5230(4) 0.1508(4) -0.05738(9) 0.0969(13) Uani 1 1 d . . . S1 S 0.4560(2) -0.2439(3) -0.14938(7) 0.0440(5) Uani 1 1 d . . . S2 S 0.3744(2) -0.3546(2) -0.04585(7) 0.0385(4) Uani 1 1 d . . . O1 O 0.1468(5) -0.3858(6) -0.23737(18) 0.0366(12) Uani 1 1 d . . . O2 O 0.0422(6) -0.5642(6) -0.0795(2) 0.0464(14) Uani 1 1 d . . . N N -0.0216(6) -0.5632(7) -0.1844(2) 0.0348(14) Uani 1 1 d . . . C1 C 0.0303(7) -0.4763(9) -0.2573(3) 0.0342(16) Uani 1 1 d . . . H1A H 0.0547 -0.5855 -0.2634 0.041 Uiso 1 1 calc R . . H1B H -0.0141 -0.4284 -0.2864 0.041 Uiso 1 1 calc R . . C2 C 0.2429(7) -0.3627(8) -0.2635(2) 0.0282(14) Uani 1 1 d . A . C3 C 0.2409(8) -0.4365(8) -0.3062(3) 0.0349(17) Uani 1 1 d . . . H3A H 0.1729 -0.5073 -0.3187 0.042 Uiso 1 1 calc R . . C4 C 0.3430(8) -0.4020(9) -0.3298(3) 0.0399(19) Uani 1 1 d . . . H4A H 0.3428 -0.4511 -0.3583 0.048 Uiso 1 1 calc R . . C5 C 0.4442(8) -0.2972(9) -0.3122(3) 0.0387(18) Uani 1 1 d . . . H5A H 0.5117 -0.2766 -0.3285 0.046 Uiso 1 1 calc R . . C6 C 0.4446(7) -0.2232(9) -0.2701(3) 0.0360(17) Uani 1 1 d . A . H6A H 0.5122 -0.1510 -0.2583 0.043 Uiso 1 1 calc R . . C7 C 0.3448(7) -0.2547(8) -0.2447(2) 0.0287(15) Uani 1 1 d . . . C8 C 0.3415(7) -0.1677(7) -0.1995(2) 0.0342(17) Uani 1 1 d . A . H8A H 0.2518 -0.1740 -0.1934 0.041 Uiso 1 1 calc R . . H8B H 0.3614 -0.0554 -0.2034 0.041 Uiso 1 1 calc R . . C9 C 0.4029(7) -0.4322(7) -0.1371(2) 0.027(3) Uani 0.67(2) 1 d PR A 1 H9A H 0.3647 -0.4844 -0.1663 0.033 Uiso 0.67(2) 1 d PR A 1 H9B H 0.4803 -0.4941 -0.1226 0.033 Uiso 0.67(2) 1 d PR A 1 C10 C 0.3007(16) -0.4386(16) -0.1055(5) 0.039(4) Uani 0.67(2) 1 d P A 1 H10A H 0.2733 -0.5487 -0.1024 0.047 Uiso 0.67(2) 1 calc PR A 1 H10B H 0.2225 -0.3770 -0.1194 0.047 Uiso 0.67(2) 1 calc PR A 1 C9' C 0.318(2) -0.416(2) -0.1390(8) 0.026(6) Uani 0.33(2) 1 d P A 2 H9'A H 0.2313 -0.3682 -0.1401 0.031 Uiso 0.33(2) 1 calc PR A 2 H9'B H 0.3098 -0.4985 -0.1629 0.031 Uiso 0.33(2) 1 calc PR A 2 C10' C 0.372(3) -0.490(3) -0.0901(9) 0.037(7) Uani 0.33(2) 1 d P A 2 H10C H 0.4621 -0.5295 -0.0891 0.044 Uiso 0.33(2) 1 calc PR A 2 H10D H 0.3169 -0.5806 -0.0854 0.044 Uiso 0.33(2) 1 calc PR A 2 C11 C 0.2184(7) -0.3600(9) -0.0252(3) 0.0375(17) Uani 1 1 d . A . H11A H 0.2225 -0.2840 0.0002 0.045 Uiso 1 1 calc R . . H11B H 0.1461 -0.3279 -0.0502 0.045 Uiso 1 1 calc R . . C12 C 0.1905(7) -0.5235(9) -0.0086(3) 0.0334(16) Uani 1 1 d . . . C13 C 0.2555(9) -0.5793(10) 0.0342(3) 0.047(2) Uani 1 1 d . A . H13A H 0.3144 -0.5117 0.0534 0.057 Uiso 1 1 calc R . . C14 C 0.2359(10) -0.7325(12) 0.0494(3) 0.059(3) Uani 1 1 d . . . H14A H 0.2807 -0.7682 0.0783 0.071 Uiso 1 1 calc R A . C15 C 0.1486(10) -0.8306(12) 0.0206(3) 0.058(3) Uani 1 1 d . A . H15A H 0.1341 -0.9337 0.0306 0.070 Uiso 1 1 calc R . . C16 C 0.0823(9) -0.7818(10) -0.0222(3) 0.049(2) Uani 1 1 d . . . H16A H 0.0253 -0.8517 -0.0413 0.059 Uiso 1 1 calc R A . C17 C 0.1009(8) -0.6264(9) -0.0369(3) 0.0368(17) Uani 1 1 d . A . C18 C -0.0512(8) -0.6624(10) -0.1101(3) 0.0430(19) Uani 1 1 d . . . H18A H -0.1251 -0.6920 -0.0956 0.052 Uiso 1 1 calc R . . H18B H -0.0083 -0.7594 -0.1181 0.052 Uiso 1 1 calc R . . C19 C -0.0986(7) -0.5639(8) -0.1524(3) 0.0358(17) Uani 1 1 d . . . C20 C -0.2150(8) -0.4784(11) -0.1582(3) 0.0408(18) Uani 1 1 d . . . H20A H -0.2681 -0.4831 -0.1359 0.049 Uiso 1 1 calc R . . C21 C -0.2529(8) -0.3854(10) -0.1975(3) 0.043(2) Uani 1 1 d . . . H21A H -0.3313 -0.3258 -0.2019 0.052 Uiso 1 1 calc R . . C22 C -0.1740(8) -0.3821(9) -0.2296(3) 0.0395(19) Uani 1 1 d . . . H22A H -0.1965 -0.3184 -0.2560 0.047 Uiso 1 1 calc R . . C23 C -0.0598(7) -0.4745(9) -0.2226(3) 0.0348(17) Uani 1 1 d . . . O1W O 0.2246(7) -0.7408(9) -0.1672(3) 0.074(2) Uani 1 1 d . . . H1WA H 0.1389 -0.6862 -0.1767 0.111 Uiso 1 1 d R . . H1WB H 0.2261 -0.8473 -0.1542 0.111 Uiso 1 1 d 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 Hg 0.0606(3) 0.04026(19) 0.0448(2) -0.00412(14) 0.00010(16) -0.01179(15) Cl1 0.0651(15) 0.0619(14) 0.0573(15) -0.0016(11) 0.0081(12) 0.0224(12) Cl2 0.166(3) 0.0801(19) 0.0421(14) -0.0113(13) 0.0129(18) -0.078(2) S1 0.0402(11) 0.0671(14) 0.0259(10) 0.0093(9) 0.0095(8) 0.0146(10) S2 0.0451(12) 0.0418(10) 0.0325(10) 0.0014(8) 0.0170(9) 0.0011(9) O1 0.032(3) 0.045(3) 0.032(3) -0.005(2) 0.007(2) -0.008(2) O2 0.048(3) 0.051(3) 0.034(3) 0.002(3) -0.006(3) -0.013(3) N 0.026(3) 0.034(3) 0.042(4) -0.008(3) 0.000(3) -0.002(2) C1 0.032(4) 0.036(4) 0.034(4) -0.004(3) 0.005(3) 0.000(3) C2 0.027(4) 0.032(3) 0.024(4) 0.004(3) 0.002(3) 0.005(3) C3 0.042(4) 0.025(3) 0.039(4) 0.001(3) 0.010(3) 0.008(3) C4 0.042(5) 0.036(4) 0.044(5) -0.003(3) 0.014(4) 0.016(3) C5 0.036(4) 0.040(4) 0.042(5) 0.008(3) 0.013(4) 0.008(3) C6 0.027(4) 0.038(4) 0.043(5) 0.011(3) 0.007(3) 0.008(3) C7 0.023(4) 0.030(3) 0.032(4) 0.001(3) 0.001(3) 0.005(3) C8 0.039(4) 0.028(3) 0.033(4) 0.005(3) 0.000(3) -0.001(3) C9 0.031(8) 0.022(5) 0.029(6) 0.002(4) 0.005(5) 0.010(5) C10 0.051(9) 0.030(6) 0.036(8) -0.005(6) 0.009(7) -0.003(6) C9' 0.022(12) 0.035(11) 0.020(12) -0.001(9) 0.003(9) 0.018(9) C10' 0.057(18) 0.029(12) 0.022(12) 0.000(9) 0.003(12) 0.012(12) C11 0.032(4) 0.041(4) 0.037(4) -0.007(3) 0.003(3) 0.003(3) C12 0.030(4) 0.043(4) 0.029(4) -0.005(3) 0.010(3) -0.002(3) C13 0.049(5) 0.064(5) 0.029(4) -0.004(4) 0.007(4) -0.017(4) C14 0.060(6) 0.076(7) 0.037(5) 0.019(5) -0.001(4) -0.008(5) C15 0.063(6) 0.058(6) 0.054(6) 0.016(5) 0.010(5) -0.011(5) C16 0.049(5) 0.052(5) 0.045(5) 0.002(4) 0.007(4) -0.010(4) C17 0.040(4) 0.040(4) 0.032(4) 0.003(3) 0.010(3) 0.002(3) C18 0.044(5) 0.047(5) 0.038(5) -0.006(4) 0.009(4) -0.011(4) C19 0.029(4) 0.036(4) 0.039(4) -0.007(3) -0.001(3) -0.013(3) C20 0.029(4) 0.059(5) 0.035(4) -0.009(4) 0.008(3) 0.002(4) C21 0.027(4) 0.052(5) 0.051(5) -0.001(4) 0.005(4) 0.007(3) C22 0.032(4) 0.036(4) 0.045(5) -0.004(3) -0.006(4) -0.002(3) C23 0.023(4) 0.038(4) 0.041(4) -0.008(3) 0.002(3) -0.008(3) O1W 0.072(5) 0.076(5) 0.073(5) -0.007(4) 0.009(4) 0.007(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 Hg Cl2 2.348(2) . ? Hg S2 2.508(2) . ? Hg Cl1 2.524(3) . ? Hg S1 2.793(2) . ? S1 C9 1.724(6) . ? S1 C8 1.802(6) . ? S1 C9' 2.08(2) . ? S2 C10' 1.72(2) . ? S2 C11 1.815(8) . ? S2 C10 1.895(13) . ? O1 C2 1.373(9) . ? O1 C1 1.434(9) . ? O2 C17 1.374(9) . ? O2 C18 1.432(9) . ? N C23 1.332(10) . ? N C19 1.338(11) . ? C1 C23 1.501(11) . ? C2 C3 1.390(10) . ? C2 C7 1.405(9) . ? C3 C4 1.391(12) . ? C4 C5 1.375(11) . ? C5 C6 1.378(11) . ? C6 C7 1.400(10) . ? C7 C8 1.517(9) . ? C9 C10 1.526(16) . ? C9' C10' 1.56(3) . ? C11 C12 1.494(11) . ? C12 C13 1.378(11) . ? C12 C17 1.402(11) . ? C13 C14 1.381(12) . ? C14 C15 1.371(13) . ? C15 C16 1.364(12) . ? C16 C17 1.391(11) . ? C18 C19 1.485(11) . ? C19 C20 1.369(11) . ? C20 C21 1.378(12) . ? C21 C22 1.353(12) . ? C22 C23 1.381(11) . ? 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 Cl2 Hg S2 136.90(10) . . ? Cl2 Hg Cl1 121.81(12) . . ? S2 Hg Cl1 97.61(8) . . ? Cl2 Hg S1 110.17(10) . . ? S2 Hg S1 80.29(6) . . ? Cl1 Hg S1 94.88(7) . . ? C9 S1 C8 108.1(3) . . ? C9 S1 C9' 24.1(6) . . ? C8 S1 C9' 90.7(7) . . ? C9 S1 Hg 99.2(2) . . ? C8 S1 Hg 102.8(2) . . ? C9' S1 Hg 87.2(6) . . ? C10' S2 C11 110.7(11) . . ? C10' S2 C10 28.0(9) . . ? C11 S2 C10 94.7(5) . . ? C10' S2 Hg 110.2(9) . . ? C11 S2 Hg 103.8(3) . . ? C10 S2 Hg 93.4(4) . . ? C2 O1 C1 118.4(5) . . ? C17 O2 C18 118.1(6) . . ? C23 N C19 118.3(7) . . ? O1 C1 C23 106.9(6) . . ? O1 C2 C3 123.6(6) . . ? O1 C2 C7 115.4(6) . . ? C3 C2 C7 120.9(7) . . ? C2 C3 C4 118.4(7) . . ? C5 C4 C3 121.9(8) . . ? C4 C5 C6 119.3(8) . . ? C5 C6 C7 121.1(7) . . ? C6 C7 C2 118.4(7) . . ? C6 C7 C8 121.1(6) . . ? C2 C7 C8 120.4(6) . . ? C7 C8 S1 114.8(4) . . ? C10 C9 S1 116.1(6) . . ? C9 C10 S2 110.5(8) . . ? C10' C9' S1 106.2(17) . . ? C9' C10' S2 112.6(18) . . ? C12 C11 S2 111.6(5) . . ? C13 C12 C17 118.2(7) . . ? C13 C12 C11 121.0(7) . . ? C17 C12 C11 120.8(7) . . ? C12 C13 C14 122.1(8) . . ? C15 C14 C13 118.2(8) . . ? C16 C15 C14 122.1(9) . . ? C15 C16 C17 119.3(8) . . ? O2 C17 C16 124.8(7) . . ? O2 C17 C12 115.0(7) . . ? C16 C17 C12 120.0(7) . . ? O2 C18 C19 105.9(6) . . ? N C19 C20 121.8(7) . . ? N C19 C18 116.4(7) . . ? C20 C19 C18 121.8(8) . . ? C19 C20 C21 119.5(8) . . ? C22 C21 C20 118.8(8) . . ? C21 C22 C23 119.2(8) . . ? N C23 C22 122.3(8) . . ? N C23 C1 116.4(7) . . ? C22 C23 C1 121.3(8) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.229 _refine_diff_density_min -1.438 _refine_diff_density_rms 0.223 ########################################################################