Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Blake, Alexander J.' 'Love, Jason B.' 'Schroder, Martin' 'Vere, Joanna M.' _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'M.SCHRODER@NOTTINGHAM.AC.UK' _publ_section_title ; Ditopic Azathioether Macrocycles as Hosts for Transition Metal Salts ; data_PDSNUR _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H50 Cl2 N6 O4 Pd S4' _chemical_formula_sum 'C26 H50 Cl2 N6 O4 Pd S4' _chemical_formula_weight 816.26 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' 'Pd' 'Pd' -0.9988 1.0072 '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 15.283(9) _cell_length_b 11.365(6) _cell_length_c 10.302(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.31(4) _cell_angle_gamma 90.00 _cell_volume 1782(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +-6.9' _diffrn_reflns_number 8508 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3501 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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^)+(0.0598P)^2^+2.5323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3501 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.0000 0.0000 0.5000 0.02276(17) Uani 1 2 d S . . Cl Cl -0.09440(9) 0.02343(11) 0.19295(12) 0.0341(3) Uani 1 1 d . . . S1 S -0.13213(8) 0.03546(11) 0.59069(12) 0.0263(3) Uani 1 1 d . . . S2 S -0.00452(8) -0.19660(10) 0.56271(12) 0.0248(3) Uani 1 1 d . . . N1 N -0.2030(3) -0.1960(4) 0.5039(4) 0.0284(9) Uani 1 1 d . . . N2 N -0.2780(3) -0.4978(4) 0.4939(4) 0.0309(9) Uani 1 1 d . . . H2A H -0.2352 -0.5149 0.5540 0.037 Uiso 1 1 calc R . . N3 N -0.3813(3) -0.5698(4) 0.3320(5) 0.0366(11) Uani 1 1 d . . . H3A H -0.3786 -0.4987 0.2990 0.044 Uiso 1 1 calc R . . O1 O -0.3426(3) -0.3423(4) 0.3808(4) 0.0436(10) Uani 1 1 d . . . O2 O -0.3097(3) -0.6929(4) 0.4821(4) 0.0487(11) Uani 1 1 d . . . C1 C -0.1311(3) 0.1956(4) 0.5936(5) 0.0293(11) Uani 1 1 d . . . H1A H -0.1904 0.2246 0.6086 0.035 Uiso 1 1 calc R . . H1B H -0.0896 0.2228 0.6671 0.035 Uiso 1 1 calc R . . C2 C -0.2220(3) 0.0159(4) 0.4615(5) 0.0303(11) Uani 1 1 d . . . H2B H -0.2652 0.0804 0.4651 0.036 Uiso 1 1 calc R . . H2C H -0.1985 0.0181 0.3751 0.036 Uiso 1 1 calc R . . C3 C -0.2666(3) -0.1021(5) 0.4802(6) 0.0349(12) Uani 1 1 d . . . H3B H -0.3028 -0.0965 0.5548 0.042 Uiso 1 1 calc R . . H3C H -0.3061 -0.1208 0.4013 0.042 Uiso 1 1 calc R . . C4 C -0.1525(3) -0.2240(4) 0.3935(5) 0.0286(11) Uani 1 1 d . . . H4A H -0.1406 -0.1506 0.3465 0.034 Uiso 1 1 calc R . . H4B H -0.1879 -0.2762 0.3322 0.034 Uiso 1 1 calc R . . C5 C -0.0667(3) -0.2837(4) 0.4373(5) 0.0268(10) Uani 1 1 d . . . H5A H -0.0317 -0.2936 0.3618 0.032 Uiso 1 1 calc R . . H5B H -0.0784 -0.3627 0.4722 0.032 Uiso 1 1 calc R . . C6 C 0.1045(3) -0.2467(4) 0.5309(5) 0.0304(11) Uani 1 1 d . . . H6A H 0.1476 -0.2231 0.6040 0.036 Uiso 1 1 calc R . . H6B H 0.1049 -0.3337 0.5252 0.036 Uiso 1 1 calc R . . C7 C -0.2368(3) -0.3000(4) 0.5627(5) 0.0289(11) Uani 1 1 d . . . H7A H -0.2732 -0.2751 0.6324 0.035 Uiso 1 1 calc R . . H7B H -0.1865 -0.3456 0.6044 0.035 Uiso 1 1 calc R . . C8 C -0.2917(3) -0.3813(5) 0.4693(5) 0.0305(11) Uani 1 1 d . . . C9 C -0.3241(4) -0.5952(5) 0.4349(5) 0.0338(12) Uani 1 1 d . . . C10 C -0.4481(4) -0.6494(5) 0.2693(5) 0.0336(12) Uani 1 1 d . . . C11 C -0.5251(5) -0.6541(8) 0.3515(7) 0.062(2) Uani 1 1 d . . . H11A H -0.5063 -0.6896 0.4362 0.093 Uiso 1 1 calc R . . H11B H -0.5723 -0.7016 0.3068 0.093 Uiso 1 1 calc R . . H11C H -0.5467 -0.5742 0.3646 0.093 Uiso 1 1 calc R . . C12 C -0.4771(4) -0.5942(6) 0.1375(6) 0.0489(16) Uani 1 1 d . . . H12A H -0.4271 -0.5911 0.0845 0.073 Uiso 1 1 calc R . . H12B H -0.4987 -0.5142 0.1505 0.073 Uiso 1 1 calc R . . H12C H -0.5241 -0.6416 0.0926 0.073 Uiso 1 1 calc R . . C13 C -0.4142(5) -0.7729(6) 0.2497(7) 0.0578(18) Uani 1 1 d . . . H13A H -0.3954 -0.8079 0.3347 0.087 Uiso 1 1 calc R . . H13B H -0.3642 -0.7697 0.1967 0.087 Uiso 1 1 calc R . . H13C H -0.4611 -0.8209 0.2052 0.087 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 Pd 0.0232(3) 0.0167(3) 0.0280(3) -0.0013(2) 0.00016(19) 0.0004(2) Cl 0.0418(7) 0.0282(7) 0.0310(6) 0.0022(5) -0.0041(5) -0.0103(5) S1 0.0253(6) 0.0214(6) 0.0321(6) -0.0017(5) 0.0020(5) 0.0003(5) S2 0.0278(6) 0.0176(6) 0.0283(6) 0.0002(5) -0.0007(5) -0.0008(4) N1 0.025(2) 0.023(2) 0.036(2) 0.0024(18) -0.0023(18) -0.0035(16) N2 0.028(2) 0.022(2) 0.040(2) 0.0052(19) -0.0125(18) -0.0044(18) N3 0.035(3) 0.025(2) 0.047(3) 0.009(2) -0.013(2) -0.0046(19) O1 0.040(2) 0.029(2) 0.056(3) 0.0122(18) -0.0251(19) -0.0085(17) O2 0.052(3) 0.028(2) 0.061(3) 0.003(2) -0.021(2) 0.0043(19) C1 0.030(3) 0.020(3) 0.038(3) -0.003(2) 0.003(2) 0.005(2) C2 0.025(2) 0.024(3) 0.040(3) 0.000(2) -0.009(2) -0.002(2) C3 0.025(3) 0.029(3) 0.050(3) 0.000(2) -0.003(2) -0.002(2) C4 0.034(3) 0.022(2) 0.027(2) 0.000(2) -0.006(2) -0.002(2) C5 0.029(3) 0.020(2) 0.030(2) -0.004(2) -0.002(2) -0.0035(19) C6 0.027(3) 0.019(2) 0.044(3) -0.001(2) -0.005(2) 0.0071(19) C7 0.028(3) 0.024(3) 0.032(3) 0.001(2) -0.008(2) -0.002(2) C8 0.025(3) 0.025(3) 0.040(3) 0.005(2) -0.005(2) -0.005(2) C9 0.031(3) 0.027(3) 0.041(3) 0.001(2) -0.007(2) -0.006(2) C10 0.037(3) 0.027(3) 0.034(3) 0.000(2) -0.011(2) -0.008(2) C11 0.056(4) 0.082(6) 0.047(4) -0.011(4) 0.002(3) -0.025(4) C12 0.046(4) 0.051(4) 0.046(4) 0.001(3) -0.014(3) -0.008(3) C13 0.066(5) 0.036(4) 0.067(4) -0.013(3) -0.018(4) -0.002(3) _geom_special_details ; Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.47 3.332(5) 165 N2-H2A...Cl(x, -y-1/2, z+1/2) 0.88 2.02 2.690(6) 132 N3-H3A...O1 ; 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 Pd S1 2.337(2) . Yes Pd S2 2.329(2) . Yes Pd S2 2.329(2) 3_556 ? Pd S1 2.337(2) 3_556 ? S1 C1 1.820(5) . ? S1 C2 1.836(5) . ? S2 C6 1.820(5) . ? S2 C5 1.823(5) . ? N1 C7 1.446(6) . ? N1 C3 1.449(7) . ? N1 C4 1.467(6) . ? N2 C8 1.361(7) . ? N2 C9 1.418(7) . ? N3 C9 1.341(7) . ? N3 C10 1.467(7) . ? O1 C8 1.226(6) . ? O2 C9 1.224(7) . ? C1 C6 1.498(7) 3_556 ? C2 C3 1.525(7) . ? C4 C5 1.509(7) . ? C6 C1 1.498(7) 3_556 ? C7 C8 1.528(7) . ? C10 C11 1.513(9) . ? C10 C13 1.516(9) . ? C10 C12 1.524(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 S1 Pd S2 90.32(4) . . Yes S2 Pd S2 180.0 . 3_556 ? S2 Pd S1 89.68(4) . 3_556 ? S2 Pd S1 90.32(4) 3_556 3_556 ? S2 Pd S1 89.68(4) 3_556 . ? S1 Pd S1 180.0 3_556 . ? C1 S1 C2 97.9(2) . . ? C1 S1 Pd 99.93(17) . . ? C2 S1 Pd 107.77(19) . . ? C6 S2 C5 97.4(2) . . ? C6 S2 Pd 101.49(17) . . ? C5 S2 Pd 110.55(17) . . ? C7 N1 C3 114.4(4) . . ? C7 N1 C4 112.4(4) . . ? C3 N1 C4 114.9(4) . . ? C8 N2 C9 128.1(4) . . ? C9 N3 C10 126.3(5) . . ? C6 C1 S1 112.1(3) 3_556 . ? C3 C2 S1 109.1(4) . . ? N1 C3 C2 111.6(4) . . ? N1 C4 C5 111.8(4) . . ? C4 C5 S2 110.5(3) . . ? C1 C6 S2 111.0(3) 3_556 . ? N1 C7 C8 115.3(4) . . ? O1 C8 N2 124.5(5) . . ? O1 C8 C7 121.6(5) . . ? N2 C8 C7 113.9(4) . . ? O2 C9 N3 126.1(5) . . ? O2 C9 N2 118.2(5) . . ? N3 C9 N2 115.7(5) . . ? N3 C10 C11 108.7(5) . . ? N3 C10 C13 113.4(5) . . ? C11 C10 C13 109.5(6) . . ? N3 C10 C12 105.8(4) . . ? C11 C10 C12 109.6(5) . . ? C13 C10 C12 109.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S1 C1 C6 -65.4(4) . . . 3_556 Yes C1 S1 C2 C3 -153.2(4) . . . . Yes C7 N1 C3 C2 161.2(4) . . . . Yes C4 N1 C3 C2 -66.6(6) . . . . Yes S1 C2 C3 N1 -47.0(5) . . . . Yes C7 N1 C4 C5 -69.6(5) . . . . Yes C3 N1 C4 C5 157.3(4) . . . . Yes N1 C4 C5 S2 -53.2(5) . . . . Yes C6 S2 C5 C4 -153.0(4) . . . . Yes C5 S2 C6 C1 72.5(4) . . . 3_556 Yes C3 N1 C7 C8 78.8(6) . . . . Yes C4 N1 C7 C8 -54.6(6) . . . . Yes C9 N2 C8 O1 -7.2(9) . . . . Yes C9 N2 C8 C7 173.1(5) . . . . Yes N1 C7 C8 O1 -38.2(7) . . . . Yes N1 C7 C8 N2 141.5(5) . . . . Yes C10 N3 C9 O2 10.8(10) . . . . Yes C10 N3 C9 N2 -168.0(5) . . . . Yes C8 N2 C9 O2 -170.6(6) . . . . Yes C8 N2 C9 N3 8.4(8) . . . . Yes C9 N3 C10 C11 78.3(7) . . . . Yes C9 N3 C10 C13 -43.8(8) . . . . Yes C9 N3 C10 C12 -164.1(6) . . . . Yes _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.79 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.12 #===END data_cusnur _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H58 Cl2 Cu2 N6 O4 S6 2+, Cu Cl4 2-, H2 O, 2(C2 H3 N)' _chemical_formula_sum 'C34 H66 Cl6 Cu3 N8 O5 S6' _chemical_formula_weight 1262.63 _exptl_special_details ; The best available crystal diffracted poorly, with the result that only 2953/4926 reflections had I > 2sigma(I). One consequence of this was that it proved impossible to refine the lighter (C,N,O) atoms other than isotropically. The resulting residuals and other quality indicators reflect the limited quality of the crystal but there is no doubt as to the chemical identity and connectivity of the product. ; 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.419(6) _cell_length_b 17.06(2) _cell_length_c 33.09(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.20(5) _cell_angle_gamma 90.00 _cell_volume 5308(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2604 _exptl_absorpt_coefficient_mu 1.774 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'X-red (Stoe & Cie, 1997b)' _diffrn_ambient_temperature 150(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 Stadi-4 _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +-8' _diffrn_reflns_number 4926 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1524 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 19.99 _reflns_number_total 4926 _reflns_number_gt 2953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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^)+(0.0001P)^2^+ 465.4P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4926 _refine_ls_number_parameters 324 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.218 _refine_ls_R_factor_gt 0.128 _refine_ls_wR_factor_ref 0.303 _refine_ls_wR_factor_gt 0.257 _refine_ls_goodness_of_fit_ref 1.49 _refine_ls_restrained_S_all 1.49 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.2083(3) 0.02587(18) 0.11923(8) 0.0158(9) Uani 1 1 d U . . Cu2 Cu 0.8421(3) 0.47414(19) 0.12339(9) 0.0188(9) Uani 1 1 d U . . Cu3 Cu 0.4996(3) 0.25464(19) -0.01771(9) 0.0159(9) Uani 1 1 d U . . Cl1 Cl 0.1877(7) -0.0121(4) 0.18354(19) 0.0243(17) Uani 1 1 d U . . Cl2 Cl 0.8887(7) 0.5072(4) 0.18829(19) 0.0291(18) Uani 1 1 d U . . Cl3 Cl 0.6737(7) 0.3274(4) -0.04205(19) 0.0225(17) Uani 1 1 d U . . Cl4 Cl 0.3161(7) 0.1831(4) -0.04214(19) 0.0200(16) Uani 1 1 d U . . Cl5 Cl 0.6370(7) 0.1594(4) 0.01351(18) 0.0179(16) Uani 1 1 d U . . Cl6 Cl 0.3763(6) 0.3472(4) 0.01529(18) 0.0154(15) Uani 1 1 d U . . S1 S -0.0275(7) 0.0718(4) 0.1126(2) 0.0221(17) Uani 1 1 d U . . S2 S 0.0889(8) -0.1076(4) 0.0816(2) 0.0254(18) Uani 1 1 d U . . S3 S 0.4227(7) -0.0428(4) 0.11468(19) 0.0171(16) Uani 1 1 d U . . S4 S 1.0761(7) 0.4289(4) 0.1153(2) 0.0220(18) Uani 1 1 d U . . S5 S 0.9491(7) 0.6131(4) 0.0891(2) 0.029(2) Uani 1 1 d U . . S6 S 0.6262(7) 0.5425(4) 0.12148(19) 0.0190(17) Uani 1 1 d U . . N1 N 0.2396(18) 0.0751(10) 0.0636(5) 0.001(4) Uiso 1 1 d U . . N2 N 0.348(2) 0.2661(12) 0.1047(6) 0.020(5) Uiso 1 1 d U . . N3 N 0.345(2) 0.2935(12) 0.1756(6) 0.018(5) Uiso 1 1 d U . . N4 N 0.788(2) 0.4306(11) 0.0649(6) 0.012(5) Uiso 1 1 d U . . N5 N 0.7015(19) 0.2312(11) 0.1043(5) 0.008(5) Uiso 1 1 d U . . N6 N 0.733(2) 0.1953(12) 0.1729(6) 0.019(5) Uiso 1 1 d U . . N7 N 0.730(3) -0.1719(19) 0.1729(10) 0.077(10) Uiso 1 1 d U . . N8 N 0.394(3) -0.2895(18) 0.1736(9) 0.068(9) Uiso 1 1 d U . . O1 O 0.2677(17) 0.1555(10) 0.1363(5) 0.020(4) Uiso 1 1 d U . . O2 O 0.4287(18) 0.3844(10) 0.1304(5) 0.024(5) Uiso 1 1 d U . . O3 O 0.7940(16) 0.3402(9) 0.1374(5) 0.015(4) Uiso 1 1 d U . . O4 O 0.6197(16) 0.1139(9) 0.1248(4) 0.013(4) Uiso 1 1 d U . . O5 O 1.005(2) 0.2571(12) 0.0000(5) 0.038(5) Uiso 1 1 d . . . C1 C 0.101(3) 0.0813(15) 0.0388(7) 0.015(7) Uiso 1 1 d U . . C2 C -0.011(2) 0.1222(14) 0.0628(7) 0.010(6) Uiso 1 1 d U . . C3 C -0.135(3) -0.0146(16) 0.0977(8) 0.029(7) Uiso 1 1 d U . . C4 C -0.063(3) -0.0916(16) 0.1138(8) 0.027(7) Uiso 1 1 d U . . C5 C 0.216(3) -0.1662(16) 0.1157(8) 0.029(7) Uiso 1 1 d U . . C6 C 0.369(3) -0.1441(16) 0.1035(8) 0.027(7) Uiso 1 1 d U . . C7 C 0.466(3) -0.0056(14) 0.0669(7) 0.014(6) Uiso 1 1 d U . . C8 C 0.334(3) 0.0183(15) 0.0394(7) 0.020(7) Uiso 1 1 d U . . C9 C 0.313(3) 0.1531(16) 0.0645(8) 0.029(7) Uiso 1 1 d U . . C10 C 0.303(2) 0.1908(14) 0.1063(7) 0.009(6) Uiso 1 1 d U . . C11 C 0.376(3) 0.3216(16) 0.1386(8) 0.022(7) Uiso 1 1 d U . . C12 C 0.355(2) 0.3457(14) 0.2114(7) 0.011(6) Uiso 1 1 d U . . C13 C 0.247(3) 0.4121(16) 0.2094(8) 0.031(8) Uiso 1 1 d U . . C14 C 0.503(3) 0.3757(18) 0.2220(9) 0.040(8) Uiso 1 1 d U . . C15 C 0.318(3) 0.2878(18) 0.2468(9) 0.046(9) Uiso 1 1 d U . . C16 C 0.920(2) 0.4278(14) 0.0403(7) 0.010(6) Uiso 1 1 d U . . C17 C 1.034(3) 0.3846(15) 0.0654(8) 0.019(7) Uiso 1 1 d U . . C18 C 1.190(3) 0.5146(16) 0.1053(8) 0.027(7) Uiso 1 1 d U . . C19 C 1.113(3) 0.5952(17) 0.1180(9) 0.037(8) Uiso 1 1 d U . . C20 C 0.836(3) 0.6654(16) 0.1222(8) 0.028(7) Uiso 1 1 d U . . C21 C 0.678(3) 0.6469(16) 0.1090(8) 0.029(8) Uiso 1 1 d U . . C22 C 0.564(3) 0.5068(16) 0.0710(8) 0.027(7) Uiso 1 1 d U . . C23 C 0.682(3) 0.4886(15) 0.0446(8) 0.023(7) Uiso 1 1 d U . . C24 C 0.721(3) 0.3538(15) 0.0669(8) 0.019(7) Uiso 1 1 d U . . C25 C 0.743(3) 0.3080(15) 0.1079(8) 0.018(7) Uiso 1 1 d U . . C26 C 0.684(2) 0.1779(13) 0.1349(7) 0.006(6) Uiso 1 1 d U . . C27 C 0.718(3) 0.1390(16) 0.2089(8) 0.024(7) Uiso 1 1 d U . . C28 C 0.556(3) 0.1233(17) 0.2147(9) 0.033(8) Uiso 1 1 d U . . C29 C 0.801(3) 0.0608(16) 0.2038(8) 0.030(8) Uiso 1 1 d U . . C30 C 0.781(3) 0.1871(17) 0.2446(8) 0.034(8) Uiso 1 1 d U . . C31 C 0.348(4) -0.400(3) 0.2277(13) 0.087(14) Uiso 1 1 d U . . C32 C 0.376(4) -0.336(2) 0.1986(11) 0.056(10) Uiso 1 1 d U . . C33 C 0.540(3) -0.1112(16) 0.2191(8) 0.026(7) Uiso 1 1 d U . . C34 C 0.644(3) -0.1404(17) 0.1940(9) 0.032(8) Uiso 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.021(2) 0.0174(19) 0.0085(18) 0.0043(15) -0.0002(14) 0.0008(16) Cu2 0.021(2) 0.026(2) 0.0092(18) -0.0014(16) -0.0018(14) 0.0007(16) Cu3 0.0169(19) 0.0181(19) 0.0127(17) 0.0007(16) 0.0003(14) 0.0019(15) Cl1 0.031(4) 0.031(4) 0.012(3) 0.003(3) 0.008(3) 0.000(3) Cl2 0.036(5) 0.038(5) 0.014(4) 0.001(3) 0.003(3) -0.005(4) Cl3 0.027(4) 0.019(4) 0.022(4) 0.004(3) 0.000(3) -0.003(3) Cl4 0.021(4) 0.023(4) 0.016(4) 0.001(3) 0.000(3) -0.002(3) Cl5 0.020(4) 0.021(4) 0.012(4) -0.004(3) -0.002(3) 0.005(3) Cl6 0.015(4) 0.020(4) 0.011(4) 0.000(3) -0.002(3) 0.005(3) S1 0.014(4) 0.036(5) 0.017(4) -0.001(3) 0.008(3) -0.006(3) S2 0.025(4) 0.028(4) 0.023(4) -0.001(3) 0.006(3) -0.007(3) S3 0.023(4) 0.013(4) 0.015(4) 0.000(3) -0.003(3) 0.006(3) S4 0.015(4) 0.030(5) 0.022(4) -0.007(3) -0.003(3) -0.002(3) S5 0.021(5) 0.037(5) 0.029(5) 0.011(4) -0.002(4) 0.003(4) S6 0.018(4) 0.019(4) 0.020(4) -0.001(3) 0.002(3) 0.002(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 Cu1 N1 2.06(2) . Yes Cu1 Cl1 2.243(7) . Yes Cu1 O1 2.34(2) . Yes Cu1 S3 2.346(7) . Yes Cu1 S1 2.354(7) . Yes Cu1 S2 2.801(8) . Yes Cu2 N4 2.11(2) . Yes Cu2 Cl2 2.240(7) . Yes Cu2 S6 2.343(7) . Yes Cu2 S4 2.364(8) . Yes Cu2 O3 2.38(2) . Yes Cu3 Cl4 2.230(7) . Yes Cu3 Cl3 2.242(7) . Yes Cu3 Cl6 2.276(7) . Yes Cu3 Cl5 2.287(7) . Yes S1 C3 1.84(3) . ? S1 C2 1.87(2) . ? S2 C4 1.85(3) . ? S2 C5 1.88(3) . ? S3 C7 1.77(2) . ? S3 C6 1.83(3) . ? S4 C17 1.84(3) . ? S4 C18 1.85(3) . ? S5 C19 1.80(3) . ? S5 C20 1.81(3) . ? S6 C22 1.84(3) . ? S6 C21 1.90(3) . ? N1 C9 1.50(3) . ? N1 C1 1.51(3) . ? N1 C8 1.57(3) . ? N2 C10 1.35(3) . ? N2 C11 1.48(3) . ? N3 C11 1.36(3) . ? N3 C12 1.48(3) . ? N4 C24 1.46(3) . ? N4 C16 1.53(3) . ? N4 C23 1.53(3) . ? N5 C25 1.37(3) . ? N5 C26 1.38(3) . ? N6 C26 1.35(3) . ? N6 C27 1.54(3) . ? N7 C34 1.22(4) . ? N8 C32 1.17(4) . ? O1 C10 1.23(3) . ? O2 C11 1.22(3) . ? O3 C25 1.20(3) . ? O4 C26 1.28(3) . ? C1 C2 1.53(3) . ? C3 C4 1.56(4) . ? C5 C6 1.57(4) . ? C7 C8 1.55(3) . ? C9 C10 1.53(4) . ? C12 C14 1.51(4) . ? C12 C13 1.52(4) . ? C12 C15 1.59(4) . ? C16 C17 1.52(3) . ? C18 C19 1.62(4) . ? C20 C21 1.56(4) . ? C22 C23 1.49(4) . ? C24 C25 1.57(4) . ? C27 C30 1.53(4) . ? C27 C29 1.56(4) . ? C27 C28 1.57(4) . ? C31 C32 1.48(5) . ? C33 C34 1.41(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 Cl1 171.9(5) . . Yes N1 Cu1 O1 77.7(6) . . Yes Cl1 Cu1 O1 94.3(4) . . Yes N1 Cu1 S3 88.9(5) . . Yes Cl1 Cu1 S3 92.1(3) . . Yes O1 Cu1 S3 107.0(4) . . Yes N1 Cu1 S1 87.8(5) . . Yes Cl1 Cu1 S1 93.1(3) . . Yes O1 Cu1 S1 85.4(4) . . Yes S3 Cu1 S1 166.2(3) . . Yes N1 Cu1 S2 90.5(5) . . Yes Cl1 Cu1 S2 97.7(3) . . Yes O1 Cu1 S2 163.6(4) . . Yes S3 Cu1 S2 83.8(2) . . Yes S1 Cu1 S2 82.8(2) . . Yes N4 Cu2 Cl2 173.2(6) . . Yes N4 Cu2 S6 89.1(5) . . Yes Cl2 Cu2 S6 91.3(3) . . Yes N4 Cu2 S4 87.8(5) . . Yes Cl2 Cu2 S4 93.3(3) . . Yes S6 Cu2 S4 166.6(3) . . Yes N4 Cu2 O3 78.6(6) . . Yes Cl2 Cu2 O3 94.8(4) . . Yes S6 Cu2 O3 108.0(4) . . Yes S4 Cu2 O3 84.1(4) . . Yes Cl4 Cu3 Cl3 137.8(3) . . Yes Cl4 Cu3 Cl6 98.5(3) . . Yes Cl3 Cu3 Cl6 101.0(3) . . Yes Cl4 Cu3 Cl5 100.5(3) . . Yes Cl3 Cu3 Cl5 98.5(3) . . Yes Cl6 Cu3 Cl5 124.6(2) . . Yes C3 S1 C2 101.8(11) . . ? C3 S1 Cu1 105.1(9) . . ? C2 S1 Cu1 96.4(8) . . ? C4 S2 C5 102.6(12) . . ? C4 S2 Cu1 85.9(9) . . ? C5 S2 Cu1 86.5(9) . . ? C7 S3 C6 103.4(12) . . ? C7 S3 Cu1 96.8(8) . . ? C6 S3 Cu1 104.8(9) . . ? C17 S4 C18 105.1(12) . . ? C17 S4 Cu2 94.7(8) . . ? C18 S4 Cu2 108.3(9) . . ? C19 S5 C20 106.2(13) . . ? C22 S6 C21 100.7(12) . . ? C22 S6 Cu2 95.3(9) . . ? C21 S6 Cu2 103.9(9) . . ? C9 N1 C1 110(2) . . ? C9 N1 C8 107(2) . . ? C1 N1 C8 106(2) . . ? C9 N1 Cu1 116(2) . . ? C1 N1 Cu1 110.7(13) . . ? C8 N1 Cu1 108.6(13) . . ? C10 N2 C11 128(2) . . ? C11 N3 C12 120(2) . . ? C24 N4 C16 112(2) . . ? C24 N4 C23 110(2) . . ? C16 N4 C23 109(2) . . ? C24 N4 Cu2 111(2) . . ? C16 N4 Cu2 109.7(14) . . ? C23 N4 Cu2 107.1(14) . . ? C25 N5 C26 128(2) . . ? C26 N6 C27 123(2) . . ? C10 O1 Cu1 110(2) . . ? C25 O3 Cu2 111(2) . . ? N1 C1 C2 111(2) . . ? C1 C2 S1 110(2) . . ? C4 C3 S1 111(2) . . ? C3 C4 S2 105(2) . . ? C6 C5 S2 106(2) . . ? C5 C6 S3 115(2) . . ? C8 C7 S3 114(2) . . ? C7 C8 N1 109(2) . . ? N1 C9 C10 110(2) . . ? O1 C10 N2 127(2) . . ? O1 C10 C9 124(2) . . ? N2 C10 C9 109(2) . . ? O2 C11 N3 128(2) . . ? O2 C11 N2 117(2) . . ? N3 C11 N2 115(2) . . ? N3 C12 C14 114(2) . . ? N3 C12 C13 114(2) . . ? C14 C12 C13 112(2) . . ? N3 C12 C15 102(2) . . ? C14 C12 C15 106(2) . . ? C13 C12 C15 109(2) . . ? C17 C16 N4 107(2) . . ? C16 C17 S4 114(2) . . ? C19 C18 S4 111(2) . . ? C18 C19 S5 113(2) . . ? C21 C20 S5 108(2) . . ? C20 C21 S6 112(2) . . ? C23 C22 S6 113(2) . . ? C22 C23 N4 112(2) . . ? N4 C24 C25 117(2) . . ? O3 C25 N5 127(2) . . ? O3 C25 C24 120(2) . . ? N5 C25 C24 112(2) . . ? O4 C26 N6 124(2) . . ? O4 C26 N5 117(2) . . ? N6 C26 N5 119(2) . . ? C30 C27 N6 102(2) . . ? C30 C27 C29 112(2) . . ? N6 C27 C29 113(2) . . ? C30 C27 C28 110(2) . . ? N6 C27 C28 109(2) . . ? C29 C27 C28 111(2) . . ? N8 C32 C31 175(4) . . ? N7 C34 C33 175(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 S1 C3 102.1(10) . . . . ? Cl1 Cu1 S1 C3 -86.0(9) . . . . ? O1 Cu1 S1 C3 179.9(10) . . . . ? S3 Cu1 S1 C3 26.0(16) . . . . ? S2 Cu1 S1 C3 11.3(9) . . . . ? N1 Cu1 S1 C2 -2.0(9) . . . . ? Cl1 Cu1 S1 C2 169.9(8) . . . . ? O1 Cu1 S1 C2 75.8(9) . . . . ? S3 Cu1 S1 C2 -78.1(14) . . . . ? S2 Cu1 S1 C2 -92.8(8) . . . . ? N1 Cu1 S2 C4 -127.6(10) . . . . ? Cl1 Cu1 S2 C4 52.3(9) . . . . ? O1 Cu1 S2 C4 -84.3(18) . . . . ? S3 Cu1 S2 C4 143.6(9) . . . . ? S1 Cu1 S2 C4 -39.8(9) . . . . ? N1 Cu1 S2 C5 129.5(10) . . . . ? Cl1 Cu1 S2 C5 -50.6(9) . . . . ? O1 Cu1 S2 C5 172.8(17) . . . . ? S3 Cu1 S2 C5 40.7(9) . . . . ? S1 Cu1 S2 C5 -142.7(9) . . . . ? N1 Cu1 S3 C7 0.1(9) . . . . ? Cl1 Cu1 S3 C7 -171.8(8) . . . . ? O1 Cu1 S3 C7 -76.6(9) . . . . ? S1 Cu1 S3 C7 76.1(14) . . . . ? S2 Cu1 S3 C7 90.7(8) . . . . ? N1 Cu1 S3 C6 -105.7(10) . . . . ? Cl1 Cu1 S3 C6 82.4(9) . . . . ? O1 Cu1 S3 C6 177.6(10) . . . . ? S1 Cu1 S3 C6 -29.7(16) . . . . ? S2 Cu1 S3 C6 -15.1(9) . . . . ? N4 Cu2 S4 C17 -3.1(10) . . . . ? Cl2 Cu2 S4 C17 170.2(8) . . . . ? S6 Cu2 S4 C17 -79.8(15) . . . . ? O3 Cu2 S4 C17 75.7(9) . . . . ? N4 Cu2 S4 C18 104.6(11) . . . . ? Cl2 Cu2 S4 C18 -82.2(9) . . . . ? S6 Cu2 S4 C18 27.8(16) . . . . ? O3 Cu2 S4 C18 -176.7(10) . . . . ? N4 Cu2 S6 C22 1.3(10) . . . . ? Cl2 Cu2 S6 C22 -171.9(9) . . . . ? S4 Cu2 S6 C22 77.9(15) . . . . ? O3 Cu2 S6 C22 -76.3(10) . . . . ? N4 Cu2 S6 C21 -101.1(10) . . . . ? Cl2 Cu2 S6 C21 85.7(9) . . . . ? S4 Cu2 S6 C21 -24.5(16) . . . . ? O3 Cu2 S6 C21 -178.8(10) . . . . ? Cl1 Cu1 N1 C9 4(5) . . . . ? O1 Cu1 N1 C9 14.3(15) . . . . ? S3 Cu1 N1 C9 -93.4(15) . . . . ? S1 Cu1 N1 C9 100.1(15) . . . . ? S2 Cu1 N1 C9 -177.1(15) . . . . ? Cl1 Cu1 N1 C1 -122(3) . . . . ? O1 Cu1 N1 C1 -111.1(14) . . . . ? S3 Cu1 N1 C1 141.2(14) . . . . ? S1 Cu1 N1 C1 -25.4(14) . . . . ? S2 Cu1 N1 C1 57.5(14) . . . . ? Cl1 Cu1 N1 C8 123(3) . . . . ? O1 Cu1 N1 C8 133.7(14) . . . . ? S3 Cu1 N1 C8 26.0(13) . . . . ? S1 Cu1 N1 C8 -140.5(13) . . . . ? S2 Cu1 N1 C8 -57.7(13) . . . . ? Cl2 Cu2 N4 C24 -1(6) . . . . ? S6 Cu2 N4 C24 -94.8(15) . . . . ? S4 Cu2 N4 C24 98.3(15) . . . . ? O3 Cu2 N4 C24 13.8(14) . . . . ? Cl2 Cu2 N4 C16 -125(4) . . . . ? S6 Cu2 N4 C16 141.8(14) . . . . ? S4 Cu2 N4 C16 -25.2(14) . . . . ? O3 Cu2 N4 C16 -109.7(14) . . . . ? Cl2 Cu2 N4 C23 118(5) . . . . ? S6 Cu2 N4 C23 24.5(14) . . . . ? S4 Cu2 N4 C23 -142.5(14) . . . . ? O3 Cu2 N4 C23 133.0(14) . . . . ? N1 Cu1 O1 C10 -6.5(15) . . . . ? Cl1 Cu1 O1 C10 172.0(14) . . . . ? S3 Cu1 O1 C10 78.5(15) . . . . ? S1 Cu1 O1 C10 -95.2(15) . . . . ? S2 Cu1 O1 C10 -51(2) . . . . ? N4 Cu2 O3 C25 -8.9(16) . . . . ? Cl2 Cu2 O3 C25 169.3(16) . . . . ? S6 Cu2 O3 C25 76.3(16) . . . . ? S4 Cu2 O3 C25 -97.9(16) . . . . ? C9 N1 C1 C2 -77(2) . . . . ? C8 N1 C1 C2 169.1(18) . . . . ? Cu1 N1 C1 C2 52(2) . . . . ? N1 C1 C2 S1 -54(2) . . . . ? C3 S1 C2 C1 -78.1(18) . . . . ? Cu1 S1 C2 C1 28.8(16) . . . . ? C2 S1 C3 C4 127.8(18) . . . . ? Cu1 S1 C3 C4 27.8(19) . . . . ? S1 C3 C4 S2 -73.6(19) . . . . ? C5 S2 C4 C3 153.6(17) . . . . ? Cu1 S2 C4 C3 68.1(16) . . . . ? C4 S2 C5 C6 -149.2(18) . . . . ? Cu1 S2 C5 C6 -64.2(16) . . . . ? S2 C5 C6 S3 67(2) . . . . ? C7 S3 C6 C5 -122.8(19) . . . . ? Cu1 S3 C6 C5 -22(2) . . . . ? C6 S3 C7 C8 79(2) . . . . ? Cu1 S3 C7 C8 -27.8(18) . . . . ? S3 C7 C8 N1 52(2) . . . . ? C9 N1 C8 C7 76(2) . . . . ? C1 N1 C8 C7 -167.9(19) . . . . ? Cu1 N1 C8 C7 -49(2) . . . . ? C1 N1 C9 C10 107(2) . . . . ? C8 N1 C9 C10 -140.0(19) . . . . ? Cu1 N1 C9 C10 -19(2) . . . . ? Cu1 O1 C10 N2 -178.1(19) . . . . ? Cu1 O1 C10 C9 -3(3) . . . . ? C11 N2 C10 O1 5(4) . . . . ? C11 N2 C10 C9 -171(2) . . . . ? N1 C9 C10 O1 14(3) . . . . ? N1 C9 C10 N2 -169.7(19) . . . . ? C12 N3 C11 O2 10(4) . . . . ? C12 N3 C11 N2 -174.2(19) . . . . ? C10 N2 C11 O2 173(2) . . . . ? C10 N2 C11 N3 -3(4) . . . . ? C11 N3 C12 C14 -64(3) . . . . ? C11 N3 C12 C13 66(3) . . . . ? C11 N3 C12 C15 -178(2) . . . . ? C24 N4 C16 C17 -72(2) . . . . ? C23 N4 C16 C17 167.8(19) . . . . ? Cu2 N4 C16 C17 51(2) . . . . ? N4 C16 C17 S4 -57(2) . . . . ? C18 S4 C17 C16 -78(2) . . . . ? Cu2 S4 C17 C16 32.6(17) . . . . ? C17 S4 C18 C19 117.4(19) . . . . ? Cu2 S4 C18 C19 17(2) . . . . ? S4 C18 C19 S5 -63(2) . . . . ? C20 S5 C19 C18 148.6(19) . . . . ? C19 S5 C20 C21 -152.1(19) . . . . ? S5 C20 C21 S6 71(2) . . . . ? C22 S6 C21 C20 -123.5(19) . . . . ? Cu2 S6 C21 C20 -25(2) . . . . ? C21 S6 C22 C23 76(2) . . . . ? Cu2 S6 C22 C23 -28.9(19) . . . . ? S6 C22 C23 N4 55(3) . . . . ? C24 N4 C23 C22 70(3) . . . . ? C16 N4 C23 C22 -169(2) . . . . ? Cu2 N4 C23 C22 -50(2) . . . . ? C16 N4 C24 C25 104(2) . . . . ? C23 N4 C24 C25 -136(2) . . . . ? Cu2 N4 C24 C25 -18(2) . . . . ? Cu2 O3 C25 N5 180(2) . . . . ? Cu2 O3 C25 C24 2(3) . . . . ? C26 N5 C25 O3 13(4) . . . . ? C26 N5 C25 C24 -168(2) . . . . ? N4 C24 C25 O3 11(3) . . . . ? N4 C24 C25 N5 -167.6(19) . . . . ? C27 N6 C26 O4 1(3) . . . . ? C27 N6 C26 N5 -180(2) . . . . ? C25 N5 C26 O4 168(2) . . . . ? C25 N5 C26 N6 -12(3) . . . . ? C26 N6 C27 C30 -177(2) . . . . ? C26 N6 C27 C29 63(3) . . . . ? C26 N6 C27 C28 -61(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 19.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.207 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.232 #===END data_agbuns _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Ag N3 O2 S3 +, N O3 -, C2 H3 N' _chemical_formula_sum 'C17 H27 Ag N5 O5 S3' _chemical_formula_weight 585.49 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 34.987(11) _cell_length_b 8.892(3) _cell_length_c 16.046(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4992(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description 'triangular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'random variation +-4.6' _diffrn_reflns_number 7196 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4902 _reflns_number_gt 3688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _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^)+(0.0397P)^2^+92.0P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.47(9) _refine_ls_number_reflns 4902 _refine_ls_number_parameters 275 _refine_ls_number_restraints 131 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.165 _refine_ls_wR_factor_gt 0.135 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.13 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.713668(16) -0.84139(6) 0.2021(3) 0.03143(18) Uani 1 1 d U . . S1 S 0.68967(19) -0.9189(6) 0.0585(4) 0.0626(15) Uani 1 1 d U . . C2 C 0.7008(7) -1.1309(17) 0.0599(13) 0.087(5) Uani 1 1 d U . . H2A H 0.6817 -1.1814 0.0239 0.105 Uiso 1 1 calc R . . H2B H 0.7260 -1.1452 0.0333 0.105 Uiso 1 1 calc R . . C3 C 0.7013(5) -1.2046(15) 0.1341(12) 0.077(5) Uani 1 1 d U . . H3A H 0.7055 -1.3130 0.1232 0.092 Uiso 1 1 calc R . . H3B H 0.6760 -1.1938 0.1607 0.092 Uiso 1 1 calc R . . S4 S 0.73567(5) -1.1437(2) 0.2030(6) 0.0371(5) Uani 1 1 d U . . C5 C 0.7133(5) -1.186(2) 0.3164(12) 0.064(3) Uani 1 1 d U . . H5A H 0.7079 -1.2949 0.3203 0.077 Uiso 1 1 calc R . . H5B H 0.7329 -1.1620 0.3589 0.077 Uiso 1 1 calc R . . C6 C 0.6787(5) -1.1050(18) 0.3374(11) 0.067(4) Uani 1 1 d U . . H6A H 0.6679 -1.1442 0.3901 0.080 Uiso 1 1 calc R . . H6B H 0.6594 -1.1179 0.2928 0.080 Uiso 1 1 calc R . . S7 S 0.69024(17) -0.9173(7) 0.3482(4) 0.0602(13) Uani 1 1 d U . . C8 C 0.6399(5) -0.831(2) 0.3400(13) 0.084(4) Uani 1 1 d U . . H8A H 0.6227 -0.8887 0.3768 0.101 Uiso 1 1 calc R . . H8B H 0.6412 -0.7270 0.3624 0.101 Uiso 1 1 calc R . . C9 C 0.6217(4) -0.8233(17) 0.2546(13) 0.081(4) Uani 1 1 d U . . H9A H 0.6172 -0.9269 0.2342 0.097 Uiso 1 1 calc R . . H9B H 0.5966 -0.7728 0.2592 0.097 Uiso 1 1 calc R . . N10 N 0.6440(2) -0.7465(8) 0.1969(15) 0.0579(17) Uani 1 1 d U . . C11 C 0.6308(5) -0.775(2) 0.1041(14) 0.085(3) Uani 1 1 d U . . H11A H 0.6028 -0.7616 0.1007 0.102 Uiso 1 1 calc R . . H11B H 0.6428 -0.6987 0.0676 0.102 Uiso 1 1 calc R . . C12 C 0.6405(5) -0.9241(19) 0.0730(12) 0.085(4) Uani 1 1 d U . . H12A H 0.6272 -0.9449 0.0198 0.102 Uiso 1 1 calc R . . H12B H 0.6335 -1.0026 0.1140 0.102 Uiso 1 1 calc R . . C13 C 0.6509(3) -0.5871(10) 0.2086(19) 0.054(3) Uani 1 1 d U . . H13A H 0.6597 -0.5427 0.1553 0.065 Uiso 1 1 calc R . . H13B H 0.6715 -0.5732 0.2502 0.065 Uiso 1 1 calc R . . C14 C 0.6139(4) -0.5024(14) 0.2389(9) 0.057(3) Uani 1 1 d U . . O14 O 0.5854(2) -0.5071(9) 0.2057(15) 0.077(3) Uani 1 1 d U . . N15 N 0.6175(3) -0.4191(12) 0.3155(8) 0.058(2) Uani 1 1 d U . . C16 C 0.5889(5) -0.3218(19) 0.3450(14) 0.080(4) Uani 1 1 d U . . O16 O 0.5973(5) -0.2507(14) 0.4055(9) 0.108(4) Uani 1 1 d U . . N17 N 0.5562(4) -0.3138(17) 0.3004(14) 0.102(5) Uani 1 1 d U A . C18 C 0.5237(5) -0.2050(16) 0.3258(8) 0.109(7) Uani 1 1 d DU . . C19 C 0.5172(9) -0.224(3) 0.4205(11) 0.064(8) Uiso 0.50 1 d PDU A 1 H19A H 0.5410 -0.2022 0.4504 0.096 Uiso 0.50 1 calc PR A 1 H19B H 0.5092 -0.3272 0.4323 0.096 Uiso 0.50 1 calc PR A 1 H19C H 0.4973 -0.1538 0.4389 0.096 Uiso 0.50 1 calc PR A 1 C20 C 0.5383(12) -0.046(3) 0.304(2) 0.095(14) Uiso 0.50 1 d PDU A 1 H20A H 0.5547 -0.0088 0.3491 0.142 Uiso 0.50 1 calc PR A 1 H20B H 0.5164 0.0221 0.2971 0.142 Uiso 0.50 1 calc PR A 1 H20C H 0.5529 -0.0495 0.2520 0.142 Uiso 0.50 1 calc PR A 1 C21 C 0.4873(10) -0.244(5) 0.277(2) 0.134(19) Uiso 0.50 1 d PDU A 1 H21A H 0.4675 -0.2792 0.3154 0.201 Uiso 0.50 1 calc PR A 1 H21B H 0.4930 -0.3242 0.2364 0.201 Uiso 0.50 1 calc PR A 1 H21C H 0.4782 -0.1550 0.2470 0.201 Uiso 0.50 1 calc PR A 1 C19' C 0.4979(13) -0.250(5) 0.3995(16) 0.17(3) Uiso 0.50 1 d PDU A 2 H19D H 0.5123 -0.2411 0.4517 0.260 Uiso 0.50 1 calc PR A 2 H19E H 0.4893 -0.3541 0.3923 0.260 Uiso 0.50 1 calc PR A 2 H19F H 0.4756 -0.1833 0.4014 0.260 Uiso 0.50 1 calc PR A 2 C20' C 0.5403(10) -0.045(2) 0.337(2) 0.072(10) Uiso 0.50 1 d PDU A 2 H20D H 0.5547 -0.0406 0.3895 0.108 Uiso 0.50 1 calc PR A 2 H20E H 0.5193 0.0279 0.3387 0.108 Uiso 0.50 1 calc PR A 2 H20F H 0.5573 -0.0219 0.2905 0.108 Uiso 0.50 1 calc PR A 2 C21' C 0.5010(10) -0.219(4) 0.2432(16) 0.098(12) Uiso 0.50 1 d PDU A 2 H21D H 0.5178 -0.1953 0.1961 0.148 Uiso 0.50 1 calc PR A 2 H21E H 0.4795 -0.1485 0.2439 0.148 Uiso 0.50 1 calc PR A 2 H21F H 0.4914 -0.3219 0.2373 0.148 Uiso 0.50 1 calc PR A 2 N N 0.6927(2) -0.5048(12) 0.4665(7) 0.091(7) Uani 1 1 d DU . . O1 O 0.6607(4) -0.545(3) 0.4928(14) 0.095(9) Uiso 0.62(3) 1 d PDU B 1 O2 O 0.7014(7) -0.507(3) 0.3920(10) 0.111(12) Uiso 0.62(3) 1 d PDU B 1 O3 O 0.7153(4) -0.4622(16) 0.5218(7) 0.042(4) Uiso 0.62(3) 1 d PDU B 1 O1' O 0.6956(10) -0.519(6) 0.5425(10) 0.16(2) Uiso 0.38(3) 1 d PDU B 2 O2' O 0.6614(5) -0.484(4) 0.4316(18) 0.080(13) Uiso 0.38(3) 1 d PDU B 2 O3' O 0.7213(6) -0.510(5) 0.4198(17) 0.125(17) Uiso 0.38(3) 1 d PDU B 2 C1S C 0.5730(5) -1.411(2) 0.0127(13) 0.093(6) Uani 1 1 d DU . . C2S C 0.572(2) -1.277(3) 0.068(3) 0.10(3) Uiso 0.40 1 d PDU C 1 C2S' C 0.5779(12) -1.260(3) 0.042(3) 0.076(10) Uiso 0.60 1 d PDU C 2 N3S N 0.5759(5) -1.145(2) 0.0765(14) 0.130(7) Uani 1 1 d DU . . 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 0.0245(3) 0.0269(3) 0.0428(3) 0.0003(9) -0.0001(8) -0.0036(2) S1 0.088(4) 0.039(2) 0.061(2) -0.006(2) -0.040(3) -0.003(3) C2 0.118(13) 0.040(5) 0.104(8) -0.022(5) -0.073(9) 0.003(7) C3 0.085(11) 0.028(3) 0.117(9) -0.013(5) -0.078(10) 0.021(7) S4 0.0235(8) 0.0218(9) 0.0660(13) 0.003(3) -0.005(3) -0.0001(8) C5 0.055(7) 0.050(5) 0.087(7) 0.035(5) 0.012(7) 0.003(6) C6 0.061(8) 0.059(5) 0.080(10) 0.020(5) 0.030(7) -0.006(5) S7 0.066(3) 0.059(3) 0.055(2) 0.006(3) 0.024(2) 0.003(3) C8 0.053(6) 0.074(9) 0.126(7) 0.021(10) 0.053(5) 0.001(7) C9 0.026(4) 0.045(7) 0.173(10) 0.032(9) 0.016(4) -0.007(6) N10 0.029(3) 0.027(3) 0.118(5) 0.012(4) -0.001(5) 0.001(2) C11 0.054(7) 0.056(8) 0.146(7) 0.011(7) -0.057(6) -0.003(6) C12 0.084(5) 0.059(8) 0.111(11) 0.008(7) -0.071(6) -0.001(7) C13 0.031(4) 0.029(3) 0.102(9) 0.012(6) 0.018(7) -0.001(3) C14 0.039(5) 0.034(5) 0.097(8) -0.001(5) -0.003(5) 0.008(5) O14 0.038(3) 0.054(4) 0.140(8) -0.035(11) -0.012(7) 0.017(3) N15 0.045(5) 0.041(6) 0.088(7) 0.002(5) 0.014(5) -0.002(4) C16 0.073(7) 0.045(8) 0.121(12) -0.003(7) 0.045(6) -0.004(6) O16 0.157(12) 0.052(7) 0.115(9) -0.009(6) 0.058(8) -0.002(7) N17 0.040(5) 0.068(9) 0.198(15) 0.009(9) 0.048(6) 0.009(6) C18 0.101(11) 0.057(10) 0.17(2) 0.010(12) 0.061(12) 0.033(9) N 0.014(4) 0.016(4) 0.24(2) -0.005(7) -0.006(10) 0.000(7) C1S 0.055(9) 0.095(11) 0.129(16) -0.033(12) -0.029(11) 0.026(9) N3S 0.089(12) 0.105(12) 0.20(2) -0.052(13) -0.038(13) -0.013(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 S1 2.546(6) . Yes Ag S4 2.797(2) . Yes Ag S4 2.496(2) 4_655 Yes Ag S7 2.575(6) . Yes Ag N10 2.580(7) . Yes S1 C12 1.736(19) . ? S1 C2 1.925(17) . ? C2 C3 1.36(2) . ? C3 S4 1.721(14) . ? S4 C5 2.015(19) . ? S4 Ag 2.496(2) 4_645 ? C5 C6 1.45(2) . ? C6 S7 1.726(17) . ? S7 C8 1.927(18) . ? C8 C9 1.51(3) . ? C9 N10 1.39(2) . ? N10 C13 1.449(12) . ? N10 C11 1.58(3) . ? C11 C12 1.46(2) . ? C13 C14 1.575(16) . ? C14 O14 1.132(17) . ? C14 N15 1.441(18) . ? N15 C16 1.41(2) . ? C16 O16 1.19(2) . ? C16 N17 1.35(3) . ? N17 C18 1.55(2) . ? C18 C21 1.539(14) . ? C18 C19' 1.543(15) . ? C18 C20' 1.544(14) . ? C18 C20 1.544(14) . ? C18 C19 1.547(14) . ? C18 C21' 1.550(14) . ? N O1' 1.232(11) . ? N O2 1.233(10) . ? N O2' 1.243(10) . ? N O1 1.248(10) . ? N O3 1.248(10) . ? N O3' 1.252(11) . ? C1S C2S' 1.432(17) . ? C1S C2S 1.485(19) . ? C2S N3S 1.193(19) . ? C2S' N3S 1.165(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag S4 115.5(3) 4_655 . Yes S1 Ag S4 80.5(2) . . Yes S1 Ag S7 130.39(11) . . Yes S1 Ag N10 75.4(5) . . Yes S4 Ag S4 118.78(4) 4_655 . Yes S4 Ag S7 113.9(3) 4_655 . Yes S7 Ag N10 79.3(5) . . Yes S4 Ag S7 80.2(2) . . Yes S4 Ag N10 125.08(17) . . Yes S4 Ag N10 116.13(17) 4_655 . Yes C12 S1 C2 99.9(10) . . ? C12 S1 Ag 102.3(7) . . ? C2 S1 Ag 100.9(6) . . ? C3 C2 S1 119.0(14) . . ? C2 C3 S4 114.9(14) . . ? C3 S4 C5 104.5(10) . . ? C3 S4 Ag 105.7(6) . 4_645 ? C5 S4 Ag 98.6(5) . 4_645 ? C3 S4 Ag 96.1(5) . . ? C5 S4 Ag 94.4(5) . . ? Ag S4 Ag 150.73(8) 4_645 . ? C6 C5 S4 116.3(11) . . ? C5 C6 S7 107.9(12) . . ? C6 S7 C8 99.6(8) . . ? C6 S7 Ag 103.7(6) . . ? C8 S7 Ag 97.1(6) . . ? C9 C8 S7 117.7(12) . . ? N10 C9 C8 112.8(14) . . ? C9 N10 C13 119.2(18) . . ? C9 N10 C11 112.5(14) . . ? C13 N10 C11 109.1(17) . . ? C9 N10 Ag 110.4(9) . . ? C13 N10 Ag 99.1(5) . . ? C11 N10 Ag 104.7(11) . . ? C12 C11 N10 113.6(13) . . ? C11 C12 S1 104.7(12) . . ? N10 C13 C14 111.8(9) . . ? O14 C14 N15 119.9(14) . . ? O14 C14 C13 124.2(16) . . ? N15 C14 C13 115.9(13) . . ? C16 N15 C14 122.8(14) . . ? O16 C16 N17 127.5(19) . . ? O16 C16 N15 115(2) . . ? N17 C16 N15 117.2(18) . . ? C16 N17 C18 121.1(18) . . ? C21 C18 C19' 81.2(19) . . ? C21 C18 C20' 126(3) . . ? C19' C18 C20' 111.6(12) . . ? C21 C18 C20 111.5(12) . . ? C19' C18 C20 127(3) . . ? C20' C18 C20 20.0(17) . . ? C21 C18 N17 109(2) . . ? C19' C18 N17 118(2) . . ? C20' C18 N17 109.3(18) . . ? C20 C18 N17 105.8(19) . . ? C21 C18 C19 110.8(12) . . ? C19' C18 C19 29.6(17) . . ? C20' C18 C19 92.2(17) . . ? C20 C18 C19 111.7(12) . . ? N17 C18 C19 107.4(17) . . ? C21 C18 C21' 28.3(17) . . ? C19' C18 C21' 109.5(12) . . ? C20' C18 C21' 111.6(12) . . ? C20 C18 C21' 92.8(18) . . ? N17 C18 C21' 96(2) . . ? C19 C18 C21' 139.0(18) . . ? O1' N O2 159.7(17) . . ? O1' N O2' 122.3(12) . . ? O2 N O2' 77.6(14) . . ? O1' N O1 73.0(16) . . ? O2 N O1 123.2(11) . . ? O2' N O1 53.5(13) . . ? O1' N O3 43(2) . . ? O2 N O3 122.4(11) . . ? O2' N O3 146.6(16) . . ? O1 N O3 114.5(10) . . ? O1' N O3' 121.5(12) . . ? O2 N O3' 38.9(15) . . ? O2' N O3' 116.2(11) . . ? O1 N O3' 156(2) . . ? O3 N O3' 85.9(17) . . ? C2S' C1S C2S 19(3) . . ? N3S C2S C1S 149(4) . . ? N3S C2S' C1S 166(4) . . ? C2S' N3S C2S 24(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 S1 C2 C3 -76.7(19) . . . . ? S1 C2 C3 S4 -63(2) . . . . ? C2 C3 S4 C5 151.1(18) . . . . ? C3 S4 C5 C6 -63.4(14) . . . . ? S4 C5 C6 S7 -68.3(16) . . . . ? C5 C6 S7 C8 162.7(13) . . . . ? C6 S7 C8 C9 -75.1(15) . . . . ? S7 C8 C9 N10 -56.4(19) . . . . ? C8 C9 N10 C13 -65.5(18) . . . . ? C8 C9 N10 C11 164.8(15) . . . . ? C9 N10 C11 C12 -73.4(17) . . . . ? C13 N10 C11 C12 151.9(15) . . . . ? N10 C11 C12 S1 -72.3(18) . . . . ? C2 S1 C12 C11 159.2(13) . . . . ? C9 N10 C13 C14 -41(2) . . . . ? C11 N10 C13 C14 90(2) . . . . ? N10 C13 C14 O14 -54(3) . . . . ? N10 C13 C14 N15 123.8(18) . . . . ? O14 C14 N15 C16 -11(2) . . . . ? C13 C14 N15 C16 171.3(13) . . . . ? C14 N15 C16 O16 -173.8(14) . . . . ? C14 N15 C16 N17 3(2) . . . . ? O16 C16 N17 C18 -1(3) . . . . ? N15 C16 N17 C18 -177.4(12) . . . . ? C16 N17 C18 C21 -167.6(18) . . . . ? C16 N17 C18 C19' -77(2) . . . . ? C16 N17 C18 C20' 52(2) . . . . ? C16 N17 C18 C20 72(2) . . . . ? C16 N17 C18 C19 -47(2) . . . . ? C16 N17 C18 C21' 166.9(18) . . . . ? C2S' C1S C2S N3S 11(5) . . . . ? C2S C1S C2S' N3S -26(13) . . . . ? C1S C2S' N3S C2S 26(13) . . . . ? C1S C2S N3S C2S' -11(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.99 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.14 #===END