# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name W.Clegg _publ_contact_author_name W.Clegg _publ_contact_author_address ; ; _publ_contact_author_email w.clegg@ncl.ac.uk # Attachment 'dalton.cif' data_ab65_compound1 _database_code_depnum_ccdc_archive 'CCDC 804734' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H30 Cu3 I Mo N6 O S6,0.5 C2 H6 O' _chemical_formula_sum 'C16.5 H33 Cu3 I Mo N6 O1.5 S6' _chemical_formula_weight 945.31 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3 c' _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 13.019(2) _cell_length_b 13.019(2) _cell_length_c 63.286(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9290(2) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6500 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 3.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.354 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1761 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 74 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1761 _reflns_number_gt 1228 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 and local programs' _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^)+(0.1492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1761 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2274 _refine_ls_wR_factor_gt 0.2140 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 I I 0.0000 0.0000 0.14922(4) 0.0430(7) Uani 0.895(5) 3 d SP A 1 I' I 0.0000 0.0000 0.1365(4) 0.0430(7) Uani 0.105(5) 3 d SP . 2 Mo Mo 0.0000 0.0000 0.07677(3) 0.0265(5) Uani 1 3 d S . . Cu Cu 0.11341(12) -0.06332(12) 0.10376(2) 0.0374(5) Uani 1 1 d . . . S1 S 0.2107(2) -0.1321(3) 0.12171(5) 0.0361(7) Uani 1 1 d . A . S2 S -0.0673(2) -0.1844(2) 0.08975(5) 0.0326(7) Uani 1 1 d . . . O O 0.0000 0.0000 0.0495(2) 0.031(3) Uani 1 3 d S . . N1 N 0.1176(8) -0.3515(8) 0.13501(14) 0.029(2) Uani 1 1 d . A . H1N H 0.180(12) -0.347(11) 0.1298(18) 0.035 Uiso 1 1 d . . . N2 N -0.0014(9) -0.2699(9) 0.13928(16) 0.040(2) Uani 1 1 d . A . H2N H 0.027(12) -0.190(12) 0.1379(19) 0.049 Uiso 1 1 d . . . C1 C 0.0981(9) -0.2615(10) 0.13297(16) 0.030(2) Uani 1 1 d . . . C2 C 0.0471(12) -0.4542(10) 0.1485(2) 0.044(3) Uani 1 1 d . . . H2A H 0.0338 -0.4267 0.1623 0.053 Uiso 1 1 calc R A . H2B H 0.0922 -0.4956 0.1512 0.053 Uiso 1 1 calc R . . C3 C -0.0732(13) -0.5418(13) 0.1387(3) 0.063(4) Uani 1 1 d . A . H3A H -0.0614 -0.5854 0.1270 0.075 Uiso 1 1 calc R . . H3B H -0.1243 -0.6002 0.1494 0.075 Uiso 1 1 calc R . . C4 C -0.1318(15) -0.4778(14) 0.1305(3) 0.083(5) Uani 1 1 d . . . H4A H -0.1013 -0.4497 0.1161 0.099 Uiso 1 1 calc R A . H4B H -0.2176 -0.5357 0.1292 0.099 Uiso 1 1 calc R . . C5 C -0.1195(11) -0.3772(11) 0.1425(3) 0.075(5) Uani 1 1 d . A . H5A H -0.1309 -0.3977 0.1577 0.091 Uiso 1 1 calc R . . H5B H -0.1821 -0.3597 0.1380 0.091 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 I 0.0366(6) 0.0366(6) 0.0559(17) 0.000 0.000 0.0183(3) I' 0.0366(6) 0.0366(6) 0.0559(17) 0.000 0.000 0.0183(3) Mo 0.0205(6) 0.0205(6) 0.0385(10) 0.000 0.000 0.0103(3) Cu 0.0282(8) 0.0291(8) 0.0529(10) 0.0047(6) -0.0053(6) 0.0127(6) S1 0.0235(13) 0.0345(15) 0.0501(19) 0.0070(13) -0.0004(12) 0.0144(12) S2 0.0272(13) 0.0224(13) 0.0470(18) 0.0016(12) -0.0015(12) 0.0114(11) O 0.017(4) 0.017(4) 0.061(10) 0.000 0.000 0.0083(18) N1 0.031(5) 0.030(5) 0.033(5) 0.003(4) 0.005(4) 0.020(4) N2 0.036(5) 0.033(5) 0.051(6) 0.006(5) 0.011(5) 0.016(4) C1 0.026(5) 0.038(6) 0.025(6) -0.005(5) 0.006(4) 0.015(5) C2 0.047(7) 0.032(6) 0.049(8) -0.002(5) 0.003(6) 0.016(6) C3 0.052(9) 0.055(9) 0.077(11) 0.018(8) 0.018(8) 0.024(7) C4 0.059(10) 0.045(9) 0.141(16) -0.016(10) -0.002(11) 0.023(8) C5 0.033(7) 0.029(7) 0.160(17) -0.004(9) 0.027(9) 0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I' Cu 2.891(18) . ? I' Cu 2.891(18) 3 ? I' Cu 2.891(18) 2 ? Mo Cu 2.6448(18) . ? Mo Cu 2.6448(18) 3 ? Mo Cu 2.6449(18) 2 ? Mo S2 2.259(3) . ? Mo S2 2.259(3) 2 ? Mo S2 2.259(3) 3 ? Mo O 1.723(15) . ? Cu S1 2.198(3) . ? Cu S2 2.258(3) . ? Cu S2 2.233(3) 2 ? S1 C1 1.740(11) . ? S2 Cu 2.233(3) 3 ? N1 H1N 0.85(13) . ? N1 C1 1.323(14) . ? N1 C2 1.459(15) . ? N2 H2N 0.92(13) . ? N2 C1 1.307(14) . ? N2 C5 1.486(15) . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C2 C3 1.54(2) . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C3 C4 1.48(2) . ? C4 H4A 0.990 . ? C4 H4B 0.990 . ? C4 C5 1.45(2) . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? 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 Cu I' Cu 74.4(5) 3 2 ? Cu I' Cu 74.4(5) . 3 ? Cu I' Cu 74.4(5) . 2 ? S2 Mo S2 107.56(9) . 2 ? S2 Mo S2 107.56(9) . 3 ? S2 Mo S2 107.56(9) 2 3 ? S2 Mo O 111.32(8) . . ? S2 Mo O 111.32(8) 2 . ? S2 Mo O 111.32(8) 3 . ? I' Cu S1 103.1(4) . . ? I' Cu S2 88.7(2) . . ? I' Cu S2 89.2(2) . 2 ? S1 Cu S2 122.02(12) . . ? S1 Cu S2 127.87(12) . 2 ? S2 Cu S2 108.50(14) . 2 ? Cu S1 C1 103.2(4) . . ? Mo S2 Cu 71.67(9) . . ? Mo S2 Cu 72.14(9) . 3 ? Cu S2 Cu 102.27(13) . 3 ? H1N N1 C1 120(8) . . ? H1N N1 C2 116(8) . . ? C1 N1 C2 123.8(10) . . ? H2N N2 C1 93(8) . . ? H2N N2 C5 136(8) . . ? C1 N2 C5 129.5(11) . . ? S1 C1 N1 117.1(8) . . ? S1 C1 N2 121.7(9) . . ? N1 C1 N2 121.2(10) . . ? N1 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? N1 C2 C3 112.6(11) . . ? H2A C2 H2B 107.8 . . ? H2A C2 C3 109.1 . . ? H2B C2 C3 109.1 . . ? C2 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C2 C3 C4 110.2(13) . . ? H3A C3 H3B 108.1 . . ? H3A C3 C4 109.6 . . ? H3B C3 C4 109.6 . . ? C3 C4 H4A 107.7 . . ? C3 C4 H4B 107.7 . . ? C3 C4 C5 118.3(17) . . ? H4A C4 H4B 107.1 . . ? H4A C4 C5 107.7 . . ? H4B C4 C5 107.7 . . ? N2 C5 C4 111.9(12) . . ? N2 C5 H5A 109.2 . . ? N2 C5 H5B 109.2 . . ? C4 C5 H5A 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O 0.85(13) 2.07(13) 2.926(11) 180(14) 16_544 N2 H2N I' 0.92(13) 2.67(13) 3.509(10) 153(11) . N2 H2N I 0.92(13) 2.76(13) 3.561(10) 146(10) . _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.088 _refine_diff_density_min -3.762 _refine_diff_density_rms 0.222 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.001 0.000 0.000 23.5 1.6 2 0.000 0.000 0.250 131.0 27.2 3 -0.001 0.000 0.500 23.5 1.7 4 0.000 0.000 0.750 131.0 27.5 5 0.333 0.667 0.417 134.6 27.4 6 0.333 0.667 0.917 134.6 27.3 7 0.333 0.666 0.167 22.7 1.6 8 0.333 0.666 0.667 22.7 1.5 9 0.667 0.333 0.083 134.6 27.4 10 0.667 0.333 0.583 134.6 27.3 11 0.666 0.333 0.333 22.6 1.6 12 0.666 0.333 0.833 22.6 1.6 _platon_squeeze_details ; SQUEEZE used to remove a molecule of disordered solvent acetone which was lying on a three-fold axis. ; #===END data_ab69_compound2 _database_code_depnum_ccdc_archive 'CCDC 804735' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H30 Cu3 N6 O S6 W +, I -' _chemical_formula_sum 'C15 H30 Cu3 I N6 O S6 W' _chemical_formula_weight 1004.18 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-P 3*' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 12.8515(15) _cell_length_b 12.8515(15) _cell_length_c 12.8515(15) _cell_angle_alpha 61.399(17) _cell_angle_beta 61.399(17) _cell_angle_gamma 61.399(17) _cell_volume 1548.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16017 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 7.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.359 _exptl_absorpt_correction_T_max 0.534 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26244 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1818 _reflns_number_gt 1633 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0684P)^2^+58.5626P] 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 1818 _refine_ls_number_parameters 101 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 W W 0.65425(3) 0.65425(3) -0.34575(3) 0.0199(3) Uani 1 3 d S . . I I 0.79770(6) 0.79770(6) -0.20230(6) 0.0299(4) Uani 1 3 d S . . S1 S 0.6077(5) 0.5349(5) 0.0895(5) 0.0376(11) Uani 1 1 d U . . S2 S 0.4952(4) 0.7773(14) -0.2333(15) 0.068(2) Uani 1 1 d . . . Cu Cu 0.6193(6) 0.6189(6) -0.11260(19) 0.0773(10) Uani 1 1 d . . . O O 0.5986(6) 0.5986(6) -0.4014(6) 0.026(3) Uani 1 3 d S . . N1 N 0.4133(15) 0.6537(16) 0.2491(14) 0.038(4) Uani 1 1 d D . . H1 H 0.4077 0.5790 0.2999 0.046 Uiso 1 1 calc R . . N2 N 0.5049(19) 0.7895(14) 0.0526(16) 0.056(5) Uani 1 1 d DU . . H2 H 0.5793 0.7979 0.0058 0.067 Uiso 1 1 calc R . . C1 C 0.5062(18) 0.6589(14) 0.1228(15) 0.0381(15) Uani 1 1 d DU . . C2 C 0.331(2) 0.7540(19) 0.300(3) 0.048(7) Uani 1 1 d . . . H2A H 0.3821 0.8003 0.2867 0.058 Uiso 1 1 calc R . . H2B H 0.2939 0.7177 0.3911 0.058 Uiso 1 1 calc R . . C3 C 0.226(3) 0.8473(17) 0.245(3) 0.044(5) Uani 1 1 d . . . H3A H 0.1829 0.9200 0.2756 0.052 Uiso 1 1 calc R . . H3B H 0.1634 0.8072 0.2727 0.052 Uiso 1 1 calc R . . C4 C 0.280(2) 0.891(2) 0.102(3) 0.076(9) Uani 1 1 d . . . H4A H 0.2835 0.8312 0.0721 0.091 Uiso 1 1 calc R . . H4B H 0.2202 0.9732 0.0697 0.091 Uiso 1 1 calc R . . C5 C 0.403(2) 0.905(2) 0.048(2) 0.064(6) Uani 1 1 d U . . H5A H 0.4156 0.9586 -0.0412 0.077 Uiso 1 1 calc R . . H5B H 0.4061 0.9483 0.0918 0.077 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 W 0.0160(3) 0.0160(3) 0.0160(3) -0.00234(16) -0.00234(16) -0.00234(16) I 0.0235(4) 0.0235(4) 0.0235(4) -0.0030(3) -0.0030(3) -0.0030(3) S1 0.038(3) 0.030(2) 0.026(2) -0.0017(18) -0.0098(18) -0.005(2) S2 0.0171(19) 0.106(6) 0.113(7) -0.095(4) -0.013(5) 0.010(5) Cu 0.125(4) 0.119(4) 0.0170(10) -0.003(3) -0.009(3) -0.093(2) O 0.021(4) 0.021(4) 0.021(4) -0.002(3) -0.002(3) -0.002(3) N1 0.034(9) 0.029(9) 0.036(9) 0.000(7) -0.011(7) -0.010(7) N2 0.047(9) 0.028(8) 0.034(9) 0.012(7) 0.006(7) -0.012(7) C1 0.038(3) 0.030(2) 0.027(3) -0.001(2) -0.010(2) -0.005(2) C2 0.037(13) 0.033(9) 0.07(2) -0.026(11) -0.006(15) -0.012(10) C3 0.035(15) 0.033(8) 0.027(14) -0.012(10) 0.011(10) -0.003(11) C4 0.043(14) 0.033(13) 0.08(2) -0.006(13) -0.020(14) 0.023(11) C5 0.057(11) 0.034(9) 0.039(9) 0.001(8) 0.004(8) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W S2 2.243(4) . ? W S2 2.243(4) 2_654 ? W S2 2.243(4) 3_564 ? W Cu 2.644(2) . ? W Cu 2.644(2) 3_564 ? W Cu 2.644(2) 2_654 ? W O 1.734(17) . ? S1 Cu 2.243(6) . ? S1 C1 1.598(18) . ? S2 Cu 2.309(16) . ? S2 Cu 2.195(17) 3_564 ? Cu S2 2.195(17) 2_654 ? N1 H1 0.880 . ? N1 C1 1.477(10) . ? N1 C2 1.43(3) . ? N2 H2 0.880 . ? N2 C1 1.472(10) . ? N2 C5 1.43(3) . ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C2 C3 1.52(3) . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C3 C4 1.53(4) . ? C4 H4A 0.990 . ? C4 H4B 0.990 . ? C4 C5 1.46(4) . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? 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 S2 W S2 108.19(12) . 2_654 ? S2 W S2 108.19(12) . 3_564 ? S2 W S2 108.19(12) 2_654 3_564 ? S2 W O 110.73(11) . . ? S2 W O 110.73(11) 2_654 . ? S2 W O 110.73(11) 3_564 . ? Cu S1 C1 94.1(7) . . ? W S2 Cu 71.0(3) . . ? W S2 Cu 73.1(3) . 3_564 ? Cu S2 Cu 102.8(2) . 3_564 ? S1 Cu S2 138.0(4) . . ? S1 Cu S2 112.7(4) . 2_654 ? S2 Cu S2 107.5(2) . 2_654 ? H1 N1 C1 115.8 . . ? H1 N1 C2 115.8 . . ? C1 N1 C2 128.5(18) . . ? H2 N2 C1 114.5 . . ? H2 N2 C5 114.5 . . ? C1 N2 C5 131.0(18) . . ? S1 C1 N1 121.8(12) . . ? S1 C1 N2 128.5(13) . . ? N1 C1 N2 108.2(14) . . ? N1 C2 H2A 108.3 . . ? N1 C2 H2B 108.3 . . ? N1 C2 C3 116(2) . . ? H2A C2 H2B 107.4 . . ? H2A C2 C3 108.3 . . ? H2B C2 C3 108.3 . . ? C2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C2 C3 C4 109(3) . . ? H3A C3 H3B 108.3 . . ? H3A C3 C4 109.8 . . ? H3B C3 C4 109.8 . . ? C3 C4 H4A 108.1 . . ? C3 C4 H4B 108.1 . . ? C3 C4 C5 117(3) . . ? H4A C4 H4B 107.3 . . ? H4A C4 C5 108.1 . . ? H4B C4 C5 108.1 . . ? N2 C5 C4 115(2) . . ? N2 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? C4 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O 0.88 2.03 2.912(18) 174 4_665 N2 H2 I 0.88 2.80 3.627(18) 157 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.896 _refine_diff_density_min -3.209 _refine_diff_density_rms 0.323 #===END data_ab74_compound4 _database_code_depnum_ccdc_archive 'CCDC 804736' #TrackingRef 'dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 Ag5 I5 N8 S4' _chemical_formula_sum 'C36 H32 Ag5 I5 N8 S4' _chemical_formula_weight 1878.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4515(9) _cell_length_b 25.829(5) _cell_length_c 20.192(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.017(8) _cell_angle_gamma 90.00 _cell_volume 4917.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 125 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 5.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.231 _exptl_absorpt_correction_T_max 0.346 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91988 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11261 _reflns_number_gt 9734 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0239P)^2^+8.7387P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00029(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11261 _refine_ls_number_parameters 540 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.45936(3) 0.572172(13) 0.506156(15) 0.03310(7) Uani 1 1 d . . . Ag2 Ag 0.47599(3) 0.586801(13) 0.352682(16) 0.03582(8) Uani 1 1 d . . . Ag3 Ag 0.52886(3) 0.446748(13) 0.334580(14) 0.03213(7) Uani 1 1 d . . . Ag4 Ag 0.55286(3) 0.458391(13) 0.182057(14) 0.03257(7) Uani 1 1 d . . . Ag5 Ag 0.46941(3) 0.558830(12) -0.021388(14) 0.03067(7) Uani 1 1 d . . . I1 I 0.67339(2) 0.519123(9) 0.433851(11) 0.02299(6) Uani 1 1 d . . . I2 I 0.24304(2) 0.613948(9) 0.423222(12) 0.02694(6) Uani 1 1 d . . . I3 I 0.34798(2) 0.517435(9) 0.250991(11) 0.02524(6) Uani 1 1 d . . . I4 I 0.76508(2) 0.417385(9) 0.267845(11) 0.02398(6) Uani 1 1 d . . . I5 I 0.65819(2) 0.537370(9) 0.092212(11) 0.02363(6) Uani 1 1 d . . . S1 S 0.38247(9) 0.38399(3) 0.39936(4) 0.02301(17) Uani 1 1 d . . . S2 S 0.23599(9) 0.59790(3) 0.00418(4) 0.02376(17) Uani 1 1 d . . . S3 S 0.38620(9) 0.39898(3) 0.10876(4) 0.02162(17) Uani 1 1 d . . . S4 S 0.64009(9) 0.65130(4) 0.30665(5) 0.02800(19) Uani 1 1 d . . . N1 N 0.1893(3) 0.46435(13) 0.39370(15) 0.0257(6) Uani 1 1 d D . . H1 H 0.245(5) 0.4882(16) 0.378(2) 0.058(16) Uiso 1 1 d D . . N2 N 0.1102(3) 0.39505(12) 0.43688(14) 0.0241(6) Uani 1 1 d . . . N3 N 0.3671(4) 0.62495(13) 0.12557(16) 0.0278(7) Uani 1 1 d . . . H3 H 0.425(5) 0.6041(19) 0.124(2) 0.040(14) Uiso 1 1 d . . . N4 N 0.1806(3) 0.67009(11) 0.09809(14) 0.0208(6) Uani 1 1 d . . . N5 N 0.1987(3) 0.47931(11) 0.07714(14) 0.0215(6) Uani 1 1 d . . . H5 H 0.260(4) 0.4988(17) 0.055(2) 0.031(11) Uiso 1 1 d . . . N6 N 0.1084(3) 0.41793(11) 0.13242(13) 0.0199(6) Uani 1 1 d . . . N7 N 0.7985(3) 0.56565(12) 0.27597(15) 0.0272(7) Uani 1 1 d . . . H7 H 0.726(5) 0.540(2) 0.282(2) 0.049(14) Uiso 1 1 d . . . N8 N 0.9014(3) 0.63839(11) 0.26022(15) 0.0244(6) Uani 1 1 d . . . C1 C 0.2252(3) 0.41555(14) 0.41015(16) 0.0210(7) Uani 1 1 d . . . C2 C 0.0532(4) 0.47547(16) 0.41053(19) 0.0292(8) Uani 1 1 d . . . H2A H 0.0048 0.5076 0.4046 0.035 Uiso 1 1 calc R . . C3 C 0.0025(4) 0.43175(16) 0.43704(18) 0.0285(8) Uani 1 1 d . . . H3A H -0.0890 0.4270 0.4527 0.034 Uiso 1 1 calc R . . C4 C 0.0983(4) 0.34277(14) 0.46194(17) 0.0251(7) Uani 1 1 d . . . C5 C 0.0168(4) 0.30729(18) 0.4241(2) 0.0379(10) Uani 1 1 d . . . H5A H -0.0299 0.3170 0.3828 0.045 Uiso 1 1 calc R . . C6 C 0.0055(5) 0.25722(19) 0.4484(3) 0.0502(13) Uani 1 1 d . . . H6A H -0.0474 0.2321 0.4228 0.060 Uiso 1 1 calc R . . C7 C 0.0702(5) 0.24361(18) 0.5092(3) 0.0468(12) Uani 1 1 d . . . H7A H 0.0604 0.2094 0.5254 0.056 Uiso 1 1 calc R . . C8 C 0.1497(5) 0.27970(18) 0.5470(2) 0.0415(10) Uani 1 1 d . . . H8A H 0.1936 0.2702 0.5890 0.050 Uiso 1 1 calc R . . C9 C 0.1649(4) 0.32990(16) 0.5230(2) 0.0326(8) Uani 1 1 d . . . H9A H 0.2198 0.3548 0.5480 0.039 Uiso 1 1 calc R . . C10 C 0.2630(4) 0.63103(13) 0.07708(16) 0.0208(7) Uani 1 1 d . . . C11 C 0.3529(4) 0.65942(15) 0.17668(18) 0.0311(8) Uani 1 1 d . . . H11A H 0.4132 0.6623 0.2162 0.037 Uiso 1 1 calc R . . C12 C 0.2373(4) 0.68821(14) 0.15988(17) 0.0274(8) Uani 1 1 d . . . H12A H 0.2009 0.7156 0.1851 0.033 Uiso 1 1 calc R . . C13 C 0.0586(4) 0.69194(14) 0.06167(17) 0.0230(7) Uani 1 1 d . . . C14 C 0.0643(4) 0.74300(15) 0.0430(2) 0.0324(8) Uani 1 1 d . . . H14A H 0.1465 0.7632 0.0542 0.039 Uiso 1 1 calc R . . C15 C -0.0536(5) 0.76476(18) 0.0070(2) 0.0445(11) Uani 1 1 d . . . H15A H -0.0514 0.8000 -0.0064 0.053 Uiso 1 1 calc R . . C16 C -0.1718(5) 0.7352(2) -0.0088(2) 0.0466(12) Uani 1 1 d . . . H16A H -0.2504 0.7499 -0.0340 0.056 Uiso 1 1 calc R . . C17 C -0.1774(4) 0.68410(18) 0.0117(2) 0.0415(10) Uani 1 1 d . . . H17A H -0.2607 0.6643 0.0015 0.050 Uiso 1 1 calc R . . C18 C -0.0623(4) 0.66170(15) 0.0471(2) 0.0324(9) Uani 1 1 d . . . H18A H -0.0653 0.6266 0.0610 0.039 Uiso 1 1 calc R . . C19 C 0.2295(3) 0.43332(13) 0.10561(16) 0.0198(6) Uani 1 1 d . . . C20 C 0.0599(4) 0.49333(14) 0.08545(17) 0.0255(7) Uani 1 1 d . . . H20A H 0.0135 0.5241 0.0698 0.031 Uiso 1 1 calc R . . C21 C 0.0031(4) 0.45488(14) 0.12001(17) 0.0232(7) Uani 1 1 d . . . H21A H -0.0912 0.4533 0.1334 0.028 Uiso 1 1 calc R . . C22 C 0.0881(3) 0.37064(13) 0.16870(16) 0.0198(6) Uani 1 1 d . . . C23 C -0.0105(4) 0.33514(15) 0.1429(2) 0.0315(8) Uani 1 1 d . . . H23A H -0.0595 0.3406 0.1008 0.038 Uiso 1 1 calc R . . C24 C -0.0364(5) 0.29118(16) 0.1801(2) 0.0393(10) Uani 1 1 d . . . H24A H -0.1044 0.2665 0.1636 0.047 Uiso 1 1 calc R . . C25 C 0.0364(4) 0.28341(16) 0.2409(2) 0.0345(9) Uani 1 1 d . . . H25A H 0.0181 0.2533 0.2659 0.041 Uiso 1 1 calc R . . C26 C 0.1359(4) 0.31898(15) 0.26580(18) 0.0294(8) Uani 1 1 d . . . H26A H 0.1862 0.3130 0.3075 0.035 Uiso 1 1 calc R . . C27 C 0.1624(4) 0.36333(14) 0.22984(17) 0.0247(7) Uani 1 1 d . . . H27A H 0.2299 0.3881 0.2467 0.030 Uiso 1 1 calc R . . C28 C 0.7804(4) 0.61735(13) 0.28006(16) 0.0222(7) Uani 1 1 d . . . C29 C 0.9307(4) 0.55412(15) 0.2547(2) 0.0316(8) Uani 1 1 d . . . H29A H 0.9684 0.5205 0.2481 0.038 Uiso 1 1 calc R . . C30 C 0.9958(4) 0.59938(15) 0.2450(2) 0.0323(8) Uani 1 1 d . . . H30A H 1.0884 0.6040 0.2305 0.039 Uiso 1 1 calc R . . C31 C 0.9304(4) 0.69310(13) 0.25684(18) 0.0248(7) Uani 1 1 d . . . C32 C 1.0279(4) 0.71441(15) 0.3031(2) 0.0316(8) Uani 1 1 d . . . H32A H 1.0735 0.6936 0.3370 0.038 Uiso 1 1 calc R . . C33 C 1.0584(5) 0.76731(16) 0.2993(2) 0.0382(9) Uani 1 1 d . . . H33A H 1.1262 0.7826 0.3303 0.046 Uiso 1 1 calc R . . C34 C 0.9896(5) 0.79730(16) 0.2502(2) 0.0401(10) Uani 1 1 d . . . H34A H 1.0096 0.8333 0.2480 0.048 Uiso 1 1 calc R . . C35 C 0.8923(5) 0.77540(17) 0.2045(2) 0.0423(10) Uani 1 1 d . . . H35A H 0.8454 0.7964 0.1712 0.051 Uiso 1 1 calc R . . C36 C 0.8619(4) 0.72229(16) 0.2069(2) 0.0333(9) Uani 1 1 d . . . H36A H 0.7962 0.7068 0.1750 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02621(15) 0.04206(18) 0.03063(15) 0.00101(13) -0.00083(11) 0.00521(12) Ag2 0.02717(15) 0.04422(18) 0.03671(16) 0.00695(13) 0.00680(12) -0.00296(13) Ag3 0.02611(14) 0.04023(17) 0.03121(15) 0.00198(12) 0.01026(12) -0.00125(12) Ag4 0.02711(15) 0.04079(17) 0.02937(15) -0.00252(12) -0.00105(11) 0.00290(12) Ag5 0.02594(14) 0.03929(17) 0.02777(14) 0.00143(12) 0.00879(11) 0.00428(12) I1 0.02327(11) 0.02400(11) 0.02185(11) -0.00041(8) 0.00263(8) 0.00331(9) I2 0.02349(12) 0.02904(12) 0.02821(12) 0.00225(9) 0.00122(9) 0.00379(9) I3 0.02940(12) 0.02431(12) 0.02261(11) 0.00039(9) 0.00609(9) 0.00423(9) I4 0.02068(11) 0.02609(12) 0.02563(11) 0.00124(9) 0.00491(8) 0.00157(9) I5 0.02380(11) 0.02366(11) 0.02356(11) 0.00201(8) 0.00247(8) 0.00303(9) S1 0.0204(4) 0.0242(4) 0.0250(4) -0.0007(3) 0.0052(3) 0.0004(3) S2 0.0242(4) 0.0236(4) 0.0233(4) -0.0033(3) 0.0004(3) 0.0049(3) S3 0.0198(4) 0.0213(4) 0.0241(4) 0.0015(3) 0.0040(3) 0.0011(3) S4 0.0215(4) 0.0256(4) 0.0373(5) 0.0023(4) 0.0045(4) 0.0008(3) N1 0.0222(15) 0.0300(17) 0.0252(15) 0.0039(13) 0.0040(12) 0.0016(13) N2 0.0205(14) 0.0287(16) 0.0233(14) 0.0018(12) 0.0044(12) -0.0014(12) N3 0.0292(17) 0.0249(16) 0.0286(16) -0.0008(13) -0.0032(13) 0.0089(14) N4 0.0215(14) 0.0197(14) 0.0213(14) -0.0023(11) 0.0021(11) 0.0008(11) N5 0.0238(15) 0.0211(14) 0.0198(14) 0.0037(11) 0.0038(12) -0.0010(12) N6 0.0188(13) 0.0209(14) 0.0205(13) 0.0027(11) 0.0039(11) -0.0014(11) N7 0.0336(17) 0.0201(15) 0.0283(16) -0.0012(12) 0.0039(13) -0.0041(13) N8 0.0252(15) 0.0170(14) 0.0316(16) 0.0008(12) 0.0073(13) -0.0001(12) C1 0.0184(16) 0.0278(18) 0.0171(15) 0.0001(13) 0.0029(12) -0.0026(13) C2 0.0219(18) 0.035(2) 0.0307(19) 0.0039(16) 0.0027(15) 0.0059(15) C3 0.0200(17) 0.039(2) 0.0266(18) 0.0013(16) 0.0051(14) 0.0027(15) C4 0.0242(17) 0.0260(18) 0.0263(17) -0.0003(14) 0.0108(14) -0.0026(14) C5 0.036(2) 0.046(3) 0.033(2) -0.0033(18) 0.0070(17) -0.0169(19) C6 0.057(3) 0.041(3) 0.055(3) -0.014(2) 0.022(2) -0.026(2) C7 0.051(3) 0.028(2) 0.065(3) 0.006(2) 0.026(2) -0.0068(19) C8 0.042(2) 0.040(2) 0.044(2) 0.0127(19) 0.0102(19) 0.0057(19) C9 0.031(2) 0.035(2) 0.033(2) 0.0005(17) 0.0056(16) 0.0007(17) C10 0.0255(17) 0.0166(15) 0.0203(16) 0.0016(12) 0.0018(13) -0.0019(13) C11 0.041(2) 0.027(2) 0.0244(18) -0.0018(15) -0.0045(16) -0.0005(16) C12 0.036(2) 0.0233(18) 0.0228(17) -0.0040(14) 0.0009(15) -0.0042(15) C13 0.0202(16) 0.0250(18) 0.0242(17) -0.0045(14) 0.0047(13) 0.0038(13) C14 0.0264(19) 0.0245(19) 0.046(2) 0.0018(17) 0.0026(17) 0.0015(15) C15 0.042(2) 0.033(2) 0.057(3) 0.009(2) -0.003(2) 0.0106(19) C16 0.032(2) 0.057(3) 0.048(3) -0.007(2) -0.0105(19) 0.019(2) C17 0.026(2) 0.045(3) 0.052(3) -0.018(2) -0.0048(18) 0.0034(18) C18 0.0270(19) 0.0244(19) 0.046(2) -0.0093(17) 0.0024(17) 0.0011(15) C19 0.0202(16) 0.0212(16) 0.0182(15) -0.0025(12) 0.0035(12) -0.0016(13) C20 0.0272(18) 0.0242(18) 0.0248(17) 0.0010(14) 0.0002(14) 0.0037(14) C21 0.0195(16) 0.0270(18) 0.0232(17) 0.0022(14) 0.0029(13) 0.0036(14) C22 0.0175(15) 0.0189(16) 0.0233(16) 0.0060(13) 0.0033(13) 0.0011(12) C23 0.034(2) 0.028(2) 0.0314(19) 0.0053(16) -0.0077(16) -0.0065(16) C24 0.044(2) 0.027(2) 0.046(2) 0.0066(18) -0.0042(19) -0.0158(18) C25 0.039(2) 0.027(2) 0.039(2) 0.0098(17) 0.0034(17) -0.0017(17) C26 0.033(2) 0.030(2) 0.0258(18) 0.0087(15) 0.0025(15) 0.0030(16) C27 0.0248(18) 0.0250(18) 0.0245(17) 0.0014(14) 0.0030(14) -0.0044(14) C28 0.0251(17) 0.0209(17) 0.0202(16) 0.0028(13) -0.0010(13) -0.0031(13) C29 0.037(2) 0.0221(18) 0.037(2) -0.0029(16) 0.0093(17) 0.0046(16) C30 0.029(2) 0.0251(19) 0.044(2) 0.0003(17) 0.0122(17) 0.0018(15) C31 0.0254(18) 0.0174(16) 0.0327(19) 0.0022(14) 0.0096(15) 0.0007(13) C32 0.036(2) 0.0233(19) 0.035(2) 0.0037(16) 0.0044(17) -0.0017(16) C33 0.042(2) 0.026(2) 0.046(2) -0.0033(18) 0.0031(19) -0.0076(17) C34 0.043(2) 0.0190(19) 0.060(3) 0.0035(18) 0.015(2) 0.0000(17) C35 0.042(2) 0.033(2) 0.052(3) 0.016(2) 0.004(2) 0.0102(19) C36 0.031(2) 0.030(2) 0.039(2) 0.0063(17) 0.0015(17) -0.0006(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 I1 2.9180(5) . ? Ag1 I1 2.9690(6) 3_666 ? Ag1 I2 2.7693(5) . ? Ag1 S1 2.5995(10) 3_666 ? Ag2 I1 2.9655(5) . ? Ag2 I2 2.7942(5) . ? Ag2 I3 2.9227(7) . ? Ag2 S4 2.4994(10) . ? Ag3 I1 2.9992(6) . ? Ag3 I3 2.9497(5) . ? Ag3 I4 2.7924(5) . ? Ag3 S1 2.5507(10) . ? Ag4 I3 2.8966(5) . ? Ag4 I4 2.7675(5) . ? Ag4 I5 2.9490(6) . ? Ag4 S3 2.5885(10) . ? Ag5 I5 2.8599(7) . ? Ag5 I5 3.0711(6) 3_665 ? Ag5 S2 2.5124(9) . ? Ag5 S3 2.5495(10) 3_665 ? I1 Ag1 2.9690(6) 3_666 ? I5 Ag5 3.0711(6) 3_665 ? S1 Ag1 2.5995(10) 3_666 ? S1 C1 1.723(3) . ? S2 C10 1.706(3) . ? S3 Ag5 2.5495(10) 3_665 ? S3 C19 1.724(3) . ? S4 C28 1.707(4) . ? N1 H1 0.884(19) . ? N1 C1 1.341(5) . ? N1 C2 1.384(5) . ? N2 C1 1.354(4) . ? N2 C3 1.391(5) . ? N2 C4 1.449(5) . ? N3 H3 0.77(5) . ? N3 C10 1.348(5) . ? N3 C11 1.377(5) . ? N4 C10 1.360(4) . ? N4 C12 1.403(4) . ? N4 C13 1.439(4) . ? N5 H5 0.90(4) . ? N5 C19 1.343(4) . ? N5 C20 1.383(5) . ? N6 C19 1.359(4) . ? N6 C21 1.389(4) . ? N6 C22 1.444(4) . ? N7 H7 0.98(5) . ? N7 C28 1.349(5) . ? N7 C29 1.382(5) . ? N8 C28 1.352(4) . ? N8 C30 1.394(5) . ? N8 C31 1.442(4) . ? C2 H2A 0.950 . ? C2 C3 1.352(5) . ? C3 H3A 0.950 . ? C4 C5 1.391(5) . ? C4 C9 1.384(5) . ? C5 H5A 0.950 . ? C5 C6 1.390(7) . ? C6 H6A 0.950 . ? C6 C7 1.377(7) . ? C7 H7A 0.950 . ? C7 C8 1.391(7) . ? C8 H8A 0.950 . ? C8 C9 1.395(6) . ? C9 H9A 0.950 . ? C11 H11A 0.950 . ? C11 C12 1.346(5) . ? C12 H12A 0.950 . ? C13 C14 1.374(5) . ? C13 C18 1.398(5) . ? C14 H14A 0.950 . ? C14 C15 1.404(6) . ? C15 H15A 0.950 . ? C15 C16 1.372(7) . ? C16 H16A 0.950 . ? C16 C17 1.387(7) . ? C17 H17A 0.950 . ? C17 C18 1.385(6) . ? C18 H18A 0.950 . ? C20 H20A 0.950 . ? C20 C21 1.347(5) . ? C21 H21A 0.950 . ? C22 C23 1.383(5) . ? C22 C27 1.390(5) . ? C23 H23A 0.950 . ? C23 C24 1.392(5) . ? C24 H24A 0.950 . ? C24 C25 1.378(6) . ? C25 H25A 0.950 . ? C25 C26 1.384(6) . ? C26 H26A 0.950 . ? C26 C27 1.388(5) . ? C27 H27A 0.950 . ? C29 H29A 0.950 . ? C29 C30 1.342(5) . ? C30 H30A 0.950 . ? C31 C32 1.380(5) . ? C31 C36 1.384(5) . ? C32 H32A 0.950 . ? C32 C33 1.399(5) . ? C33 H33A 0.950 . ? C33 C34 1.384(6) . ? C34 H34A 0.950 . ? C34 C35 1.378(7) . ? C35 H35A 0.950 . ? C35 C36 1.403(6) . ? C36 H36A 0.950 . ? 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 I1 Ag1 I1 99.135(17) . 3_666 ? I1 Ag1 I2 112.88(2) . . ? I1 Ag1 I2 103.944(15) 3_666 . ? I1 Ag1 S1 100.87(2) . 3_666 ? I1 Ag1 S1 106.51(3) 3_666 3_666 ? I2 Ag1 S1 129.52(3) . 3_666 ? I1 Ag2 I2 110.73(2) . . ? I1 Ag2 I3 103.908(19) . . ? I1 Ag2 S4 102.46(3) . . ? I2 Ag2 I3 102.108(17) . . ? I2 Ag2 S4 123.64(3) . . ? I3 Ag2 S4 112.61(3) . . ? I1 Ag3 I3 102.427(19) . . ? I1 Ag3 I4 98.608(16) . . ? I1 Ag3 S1 106.94(3) . . ? I3 Ag3 I4 110.06(2) . . ? I3 Ag3 S1 111.92(2) . . ? I4 Ag3 S1 123.75(3) . . ? I3 Ag4 I4 112.35(2) . . ? I3 Ag4 I5 101.376(18) . . ? I3 Ag4 S3 100.74(2) . . ? I4 Ag4 I5 112.872(16) . . ? I4 Ag4 S3 121.09(3) . . ? I5 Ag4 S3 106.05(3) . . ? I5 Ag5 I5 114.786(15) . 3_665 ? I5 Ag5 S2 114.87(3) . . ? I5 Ag5 S2 95.67(2) 3_665 . ? I5 Ag5 S3 107.68(3) . 3_665 ? I5 Ag5 S3 103.62(3) 3_665 3_665 ? S2 Ag5 S3 119.39(3) . 3_665 ? Ag1 I1 Ag1 80.865(17) . 3_666 ? Ag1 I1 Ag2 64.43(2) . . ? Ag1 I1 Ag2 115.225(14) 3_666 . ? Ag1 I1 Ag3 109.137(16) . . ? Ag1 I1 Ag3 65.92(2) 3_666 . ? Ag2 I1 Ag3 76.030(18) . . ? Ag1 I2 Ag2 68.64(2) . . ? Ag2 I3 Ag3 77.446(19) . . ? Ag2 I3 Ag4 113.739(16) . . ? Ag3 I3 Ag4 64.46(2) . . ? Ag3 I4 Ag4 68.23(2) . . ? Ag4 I5 Ag5 114.139(17) . . ? Ag4 I5 Ag5 65.69(2) . 3_665 ? Ag5 I5 Ag5 65.214(15) . 3_665 ? Ag1 S1 Ag3 78.16(3) 3_666 . ? Ag1 S1 C1 99.09(12) 3_666 . ? Ag3 S1 C1 105.55(12) . . ? Ag5 S2 C10 107.34(12) . . ? Ag4 S3 Ag5 78.95(3) . 3_665 ? Ag4 S3 C19 101.71(11) . . ? Ag5 S3 C19 104.75(12) 3_665 . ? Ag2 S4 C28 106.88(12) . . ? H1 N1 C1 127(4) . . ? H1 N1 C2 122(4) . . ? C1 N1 C2 110.9(3) . . ? C1 N2 C3 110.0(3) . . ? C1 N2 C4 126.0(3) . . ? C3 N2 C4 124.0(3) . . ? H3 N3 C10 122(4) . . ? H3 N3 C11 127(4) . . ? C10 N3 C11 111.4(3) . . ? C10 N4 C12 109.5(3) . . ? C10 N4 C13 126.0(3) . . ? C12 N4 C13 124.4(3) . . ? H5 N5 C19 125(3) . . ? H5 N5 C20 124(3) . . ? C19 N5 C20 111.0(3) . . ? C19 N6 C21 109.9(3) . . ? C19 N6 C22 126.5(3) . . ? C21 N6 C22 123.6(3) . . ? H7 N7 C28 125(3) . . ? H7 N7 C29 124(3) . . ? C28 N7 C29 110.7(3) . . ? C28 N8 C30 110.0(3) . . ? C28 N8 C31 125.1(3) . . ? C30 N8 C31 124.8(3) . . ? S1 C1 N1 128.2(3) . . ? S1 C1 N2 126.1(3) . . ? N1 C1 N2 105.7(3) . . ? N1 C2 H2A 126.7 . . ? N1 C2 C3 106.6(3) . . ? H2A C2 C3 126.7 . . ? N2 C3 C2 106.8(3) . . ? N2 C3 H3A 126.6 . . ? C2 C3 H3A 126.6 . . ? N2 C4 C5 118.4(3) . . ? N2 C4 C9 119.5(3) . . ? C5 C4 C9 122.0(4) . . ? C4 C5 H5A 120.9 . . ? C4 C5 C6 118.2(4) . . ? H5A C5 C6 120.9 . . ? C5 C6 H6A 119.6 . . ? C5 C6 C7 120.8(4) . . ? H6A C6 C7 119.6 . . ? C6 C7 H7A 119.8 . . ? C6 C7 C8 120.4(4) . . ? H7A C7 C8 119.8 . . ? C7 C8 H8A 120.1 . . ? C7 C8 C9 119.8(4) . . ? H8A C8 C9 120.1 . . ? C4 C9 C8 118.8(4) . . ? C4 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? S2 C10 N3 128.7(3) . . ? S2 C10 N4 125.9(3) . . ? N3 C10 N4 105.4(3) . . ? N3 C11 H11A 126.6 . . ? N3 C11 C12 106.8(3) . . ? H11A C11 C12 126.6 . . ? N4 C12 C11 107.0(3) . . ? N4 C12 H12A 126.5 . . ? C11 C12 H12A 126.5 . . ? N4 C13 C14 118.1(3) . . ? N4 C13 C18 120.2(3) . . ? C14 C13 C18 121.7(4) . . ? C13 C14 H14A 120.6 . . ? C13 C14 C15 118.7(4) . . ? H14A C14 C15 120.6 . . ? C14 C15 H15A 119.9 . . ? C14 C15 C16 120.1(4) . . ? H15A C15 C16 119.9 . . ? C15 C16 H16A 119.8 . . ? C15 C16 C17 120.5(4) . . ? H16A C16 C17 119.8 . . ? C16 C17 H17A 119.8 . . ? C16 C17 C18 120.5(4) . . ? H17A C17 C18 119.8 . . ? C13 C18 C17 118.4(4) . . ? C13 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? S3 C19 N5 129.1(3) . . ? S3 C19 N6 125.5(3) . . ? N5 C19 N6 105.4(3) . . ? N5 C20 H20A 126.7 . . ? N5 C20 C21 106.6(3) . . ? H20A C20 C21 126.7 . . ? N6 C21 C20 107.1(3) . . ? N6 C21 H21A 126.5 . . ? C20 C21 H21A 126.5 . . ? N6 C22 C23 118.7(3) . . ? N6 C22 C27 119.3(3) . . ? C23 C22 C27 122.0(3) . . ? C22 C23 H23A 120.8 . . ? C22 C23 C24 118.5(4) . . ? H23A C23 C24 120.8 . . ? C23 C24 H24A 119.9 . . ? C23 C24 C25 120.2(4) . . ? H24A C24 C25 119.9 . . ? C24 C25 H25A 119.6 . . ? C24 C25 C26 120.7(4) . . ? H25A C25 C26 119.6 . . ? C25 C26 H26A 120.0 . . ? C25 C26 C27 120.0(4) . . ? H26A C26 C27 120.0 . . ? C22 C27 C26 118.6(3) . . ? C22 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? S4 C28 N7 129.2(3) . . ? S4 C28 N8 125.3(3) . . ? N7 C28 N8 105.4(3) . . ? N7 C29 H29A 126.5 . . ? N7 C29 C30 106.9(3) . . ? H29A C29 C30 126.5 . . ? N8 C30 C29 106.9(3) . . ? N8 C30 H30A 126.5 . . ? C29 C30 H30A 126.5 . . ? N8 C31 C32 118.6(3) . . ? N8 C31 C36 119.2(3) . . ? C32 C31 C36 122.2(3) . . ? C31 C32 H32A 120.6 . . ? C31 C32 C33 118.8(4) . . ? H32A C32 C33 120.6 . . ? C32 C33 H33A 120.1 . . ? C32 C33 C34 119.9(4) . . ? H33A C33 C34 120.1 . . ? C33 C34 H34A 119.7 . . ? C33 C34 C35 120.5(4) . . ? H34A C34 C35 119.7 . . ? C34 C35 H35A 119.8 . . ? C34 C35 C36 120.5(4) . . ? H35A C35 C36 119.8 . . ? C31 C36 C35 118.1(4) . . ? C31 C36 H36A 120.9 . . ? C35 C36 H36A 120.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 I3 0.884(19) 2.91(4) 3.611(3) 138(4) . N3 H3 I5 0.77(5) 2.90(5) 3.660(3) 168(5) . N5 H5 S2 0.90(4) 2.76(4) 3.428(3) 131(3) . N5 H5 I5 0.90(4) 3.27(4) 3.789(3) 119(3) 3_665 N7 H7 I1 0.98(5) 3.18(5) 3.679(3) 114(3) . N7 H7 I4 0.98(5) 3.20(5) 3.845(3) 125(3) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.759 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.134 #===END