Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lyall R. Hanton' 'Paula L. Caradoc-Davies' _publ_contact_author_name 'Dr Lyall R Hanton' _publ_contact_author_address ; Department Chemistry University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email LHANTON@ALKALI.OTAGO.AC.NZ _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Molecular rectangles from metallomacrocycles: development of dibenzofuran ligands. ; data_Compound_1.3CH2Cl2 _database_code_CSD 186275 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ag2(L)2](ClO4)2.3CH2Cl2 _chemical_formula_sum 'C23.50 H17 Ag Cl4 N2 O5 S2' _chemical_formula_weight 721.18 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.666(5) _cell_length_b 10.113(5) _cell_length_c 14.921(5) _cell_angle_alpha 81.954(5) _cell_angle_beta 72.710(5) _cell_angle_gamma 81.553(5) _cell_volume 1370.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 6951 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.38 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10953 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5386 _reflns_number_gt 4618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+2.7779P] 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 5386 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.6249(6) -0.3456(6) 0.4862(4) 0.0471(12) Uani 1 1 d . . . H1 H 0.6495 -0.3248 0.5379 0.056 Uiso 1 1 calc R . . C2 C 0.6987(6) -0.4578(6) 0.4429(4) 0.0462(12) Uani 1 1 d . . . H2 H 0.7699 -0.5118 0.4657 0.055 Uiso 1 1 calc R . . C3 C 0.6648(5) -0.4885(4) 0.3650(3) 0.0357(10) Uani 1 1 d . . . C4 C 0.5586(6) -0.4055(5) 0.3338(4) 0.0398(10) Uani 1 1 d . . . H4 H 0.5343 -0.4227 0.2811 0.048 Uiso 1 1 calc R . . C5 C 0.4882(5) -0.2953(5) 0.3824(3) 0.0388(10) Uani 1 1 d . . . H5 H 0.4159 -0.2402 0.3613 0.047 Uiso 1 1 calc R . . C6 C 0.7162(5) -0.6152(5) 0.2055(3) 0.0389(10) Uani 1 1 d . . . C7 C 0.6252(6) -0.6939(5) 0.1848(4) 0.0455(12) Uani 1 1 d . . . H7 H 0.5815 -0.7594 0.2304 0.055 Uiso 1 1 calc R . . C8 C 0.5985(6) -0.6761(6) 0.0960(4) 0.0515(14) Uani 1 1 d . . . H8 H 0.5391 -0.7314 0.0835 0.062 Uiso 1 1 calc R . . C9 C 0.6588(6) -0.5779(5) 0.0267(4) 0.0442(12) Uani 1 1 d . . . H9 H 0.6400 -0.5669 -0.0316 0.053 Uiso 1 1 calc R . . C10 C 0.7481(5) -0.4956(5) 0.0461(3) 0.0363(10) Uani 1 1 d . . . C11 C 0.8296(5) -0.3838(5) -0.0044(3) 0.0369(10) Uani 1 1 d . . . C12 C 0.8483(6) -0.3104(5) -0.0931(4) 0.0445(12) Uani 1 1 d . . . H12 H 0.8028 -0.3303 -0.1357 0.053 Uiso 1 1 calc R . . C13 C 0.9368(6) -0.2069(5) -0.1158(4) 0.0479(13) Uani 1 1 d . . . H13 H 0.9514 -0.1579 -0.1748 0.057 Uiso 1 1 calc R . . C14 C 1.0037(6) -0.1749(5) -0.0530(3) 0.0434(12) Uani 1 1 d . . . H14 H 1.0617 -0.1046 -0.0706 0.052 Uiso 1 1 calc R . . C15 C 0.9863(5) -0.2457(4) 0.0367(3) 0.0351(10) Uani 1 1 d . . . C16 C 0.8980(5) -0.3495(4) 0.0581(3) 0.0319(9) Uani 1 1 d . . . C17 C 0.7761(5) -0.5171(4) 0.1340(3) 0.0341(9) Uani 1 1 d . . . C18 C 0.0527(5) 0.1401(4) 0.7942(3) 0.0343(9) Uani 1 1 d . . . C19 C 0.2002(5) 0.1118(4) 0.7901(3) 0.0352(10) Uani 1 1 d . . . H19 H 0.2346 0.1354 0.8370 0.042 Uiso 1 1 calc R . . C20 C 0.2935(5) 0.0490(4) 0.7161(3) 0.0365(10) Uani 1 1 d . . . H20 H 0.3915 0.0301 0.7139 0.044 Uiso 1 1 calc R . . C21 C 0.1075(6) 0.0431(5) 0.6501(4) 0.0438(11) Uani 1 1 d . . . H21 H 0.0759 0.0213 0.6014 0.053 Uiso 1 1 calc R . . C22 C 0.0072(6) 0.1040(5) 0.7223(4) 0.0438(11) Uani 1 1 d . . . H22 H -0.0904 0.1209 0.7231 0.053 Uiso 1 1 calc R . . C24 C 0.0984(10) -0.4912(8) 0.3249(6) 0.082(2) Uani 1 1 d . . . H24A H 0.0376 -0.4596 0.2832 0.099 Uiso 1 1 calc R . . H24B H 0.0671 -0.5756 0.3590 0.099 Uiso 1 1 calc R . . N1 N 0.5198(4) -0.2652(4) 0.4577(3) 0.0360(8) Uani 1 1 d . . . N2 N 0.2489(4) 0.0133(4) 0.6458(3) 0.0365(8) Uani 1 1 d . . . O12A O 0.3314(19) 0.019(3) 0.2627(14) 0.067(9) Uani 0.30(4) 1 d P . . O11A O 0.1385(13) 0.1757(11) 0.3429(15) 0.078(6) Uani 0.51(3) 1 d P . . O1 O 0.8672(3) -0.4297(3) 0.1428(2) 0.0338(7) Uani 1 1 d . . . O11 O 0.1397(11) 0.1865(10) 0.4142(15) 0.077(7) Uani 0.49(3) 1 d P . . O12 O 0.260(3) 0.099(2) 0.2652(9) 0.124(10) Uani 0.70(4) 1 d P . . O13 O 0.2123(5) -0.0381(5) 0.4102(4) 0.0702(13) Uani 1 1 d . . . O14 O 0.3787(5) 0.1200(5) 0.3745(4) 0.0710(13) Uani 1 1 d . . . S1 S 0.75783(15) -0.63641(12) 0.31455(9) 0.0431(3) Uani 1 1 d . . . S2 S -0.08417(13) 0.21425(12) 0.88654(9) 0.0400(3) Uani 1 1 d . . . C23 C 0.4784(17) -0.0360(14) 0.0519(8) 0.066(4) Uani 0.50 1 d P A -1 H23A H 0.4439 -0.0366 -0.0028 0.079 Uiso 0.50 1 calc PR A -1 H23B H 0.4180 0.0327 0.0899 0.079 Uiso 0.50 1 calc PR A -1 Cl1 Cl 0.6324(10) -0.0099(9) 0.0223(8) 0.172(3) Uani 0.50 1 d P A -1 Cl2 Cl 0.4712(7) -0.1986(7) 0.1200(6) 0.135(3) Uani 0.50 1 d P A -1 Cl3 Cl 0.2812(3) -0.5195(4) 0.2566(2) 0.1200(10) Uani 1 1 d . . . Cl4 Cl 0.0734(4) -0.3767(3) 0.4036(2) 0.1259(10) Uani 1 1 d . . . Cl5 Cl 0.25355(14) 0.08489(14) 0.35677(10) 0.0483(3) Uani 1 1 d . . . Ag1 Ag 0.39120(4) -0.11082(4) 0.54228(2) 0.04084(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(3) 0.053(3) 0.034(2) -0.010(2) -0.011(2) -0.003(2) C2 0.048(3) 0.050(3) 0.037(2) -0.004(2) -0.011(2) 0.007(2) C3 0.042(2) 0.027(2) 0.030(2) -0.0014(17) 0.0035(18) -0.0074(18) C4 0.044(3) 0.037(2) 0.039(2) -0.013(2) -0.008(2) -0.004(2) C5 0.041(3) 0.037(2) 0.037(2) -0.011(2) -0.006(2) -0.002(2) C6 0.042(3) 0.029(2) 0.037(2) -0.0099(19) 0.0028(19) 0.0006(19) C7 0.041(3) 0.035(2) 0.051(3) -0.012(2) 0.004(2) -0.006(2) C8 0.040(3) 0.047(3) 0.065(4) -0.027(3) 0.000(2) -0.008(2) C9 0.038(2) 0.049(3) 0.045(3) -0.022(2) -0.007(2) 0.004(2) C10 0.038(2) 0.031(2) 0.035(2) -0.0113(18) -0.0026(18) 0.0050(18) C11 0.036(2) 0.034(2) 0.033(2) -0.0100(19) -0.0004(18) 0.0085(18) C12 0.050(3) 0.044(3) 0.033(2) -0.007(2) -0.009(2) 0.010(2) C13 0.059(3) 0.039(3) 0.032(2) 0.003(2) 0.000(2) 0.007(2) C14 0.049(3) 0.033(2) 0.035(2) 0.000(2) 0.005(2) 0.001(2) C15 0.038(2) 0.028(2) 0.031(2) -0.0085(18) 0.0021(18) 0.0019(18) C16 0.037(2) 0.026(2) 0.0251(19) -0.0047(16) 0.0002(17) 0.0044(17) C17 0.035(2) 0.029(2) 0.033(2) -0.0105(18) 0.0017(18) -0.0004(17) C18 0.036(2) 0.024(2) 0.038(2) -0.0041(18) -0.0008(18) -0.0067(17) C19 0.041(2) 0.029(2) 0.033(2) -0.0077(18) -0.0043(19) -0.0061(18) C20 0.039(2) 0.029(2) 0.038(2) -0.0070(18) -0.0039(19) -0.0037(18) C21 0.047(3) 0.044(3) 0.042(3) -0.012(2) -0.009(2) -0.011(2) C22 0.036(2) 0.048(3) 0.047(3) -0.011(2) -0.007(2) -0.007(2) C24 0.096(6) 0.070(5) 0.085(5) -0.003(4) -0.037(5) -0.004(4) N1 0.044(2) 0.0325(19) 0.0279(18) -0.0059(15) -0.0021(16) -0.0062(16) N2 0.042(2) 0.0316(19) 0.0331(19) -0.0079(16) -0.0030(16) -0.0079(16) O12A 0.061(11) 0.101(19) 0.037(9) -0.031(10) -0.017(6) 0.023(9) O11A 0.075(7) 0.060(6) 0.102(15) -0.003(6) -0.043(7) 0.015(5) O1 0.0401(17) 0.0304(15) 0.0270(14) -0.0040(12) -0.0020(12) -0.0057(13) O11 0.047(6) 0.054(6) 0.105(15) -0.001(6) 0.007(6) 0.012(4) O12 0.21(2) 0.129(14) 0.075(7) 0.008(8) -0.095(11) -0.046(16) O13 0.074(3) 0.057(3) 0.085(3) 0.011(2) -0.034(3) -0.015(2) O14 0.059(3) 0.091(3) 0.078(3) -0.014(3) -0.033(2) -0.023(2) S1 0.0541(7) 0.0283(6) 0.0347(6) -0.0006(5) 0.0020(5) 0.0014(5) S2 0.0349(6) 0.0355(6) 0.0434(6) -0.0115(5) 0.0011(5) -0.0026(5) C23 0.092(10) 0.071(8) 0.041(6) -0.013(6) -0.009(6) -0.041(8) Cl1 0.150(7) 0.144(6) 0.215(9) -0.031(6) -0.040(6) -0.004(5) Cl2 0.118(4) 0.145(5) 0.178(6) -0.062(5) -0.095(5) 0.032(4) Cl3 0.0955(17) 0.160(3) 0.117(2) -0.0253(19) -0.0344(16) -0.0331(18) Cl4 0.141(3) 0.119(2) 0.113(2) 0.0072(17) -0.0494(18) 0.0113(19) Cl5 0.0408(6) 0.0494(7) 0.0592(8) 0.0014(6) -0.0243(6) -0.0052(5) Ag1 0.0486(3) 0.0376(2) 0.0332(2) -0.01409(15) -0.00171(16) -0.00577(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 C1 N1 1.338(7) . ? C1 C2 1.381(8) . ? C2 C3 1.382(7) . ? C3 C4 1.377(7) . ? C3 S1 1.769(5) . ? C4 C5 1.393(7) . ? C5 N1 1.332(6) . ? C6 C7 1.392(8) . ? C6 C17 1.401(7) . ? C6 S1 1.767(5) . ? C7 C8 1.406(9) . ? C8 C9 1.385(8) . ? C9 C10 1.395(7) . ? C10 C17 1.398(7) . ? C10 C11 1.462(7) . ? C11 C16 1.397(7) . ? C11 C12 1.399(7) . ? C12 C13 1.391(8) . ? C13 C14 1.381(8) . ? C14 C15 1.402(7) . ? C15 C16 1.394(7) . ? C15 S2 1.773(5) 2_656 ? C16 O1 1.379(5) . ? C17 O1 1.380(6) . ? C18 C22 1.384(7) . ? C18 C19 1.397(7) . ? C18 S2 1.768(5) . ? C19 C20 1.368(6) . ? C20 N2 1.356(6) . ? C21 N2 1.340(7) . ? C21 C22 1.368(7) . ? C24 Cl4 1.705(9) . ? C24 Cl3 1.762(10) . ? N1 Ag1 2.151(4) . ? N2 Ag1 2.150(4) . ? O12A O12 0.987(17) . ? O12A Cl5 1.572(14) . ? O11A O11 1.088(16) . ? O11A Cl5 1.381(10) . ? O11A O12 1.58(3) . ? O11 Cl5 1.535(12) . ? O12 Cl5 1.338(9) . ? O13 Cl5 1.422(5) . ? O14 Cl5 1.416(4) . ? S2 C15 1.773(5) 2_656 ? C23 Cl1 1.474(17) . ? C23 Cl2 1.806(16) . ? Ag1 Ag1 3.1711(13) 2_656 ? 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 C1 C2 123.5(5) . . ? C1 C2 C3 118.8(5) . . ? C4 C3 C2 118.4(4) . . ? C4 C3 S1 124.5(4) . . ? C2 C3 S1 117.1(4) . . ? C3 C4 C5 119.0(5) . . ? N1 C5 C4 123.0(5) . . ? C7 C6 C17 116.2(5) . . ? C7 C6 S1 123.0(4) . . ? C17 C6 S1 120.8(4) . . ? C6 C7 C8 121.0(5) . . ? C9 C8 C7 121.4(5) . . ? C8 C9 C10 118.8(5) . . ? C9 C10 C17 118.8(5) . . ? C9 C10 C11 136.3(5) . . ? C17 C10 C11 104.8(4) . . ? C16 C11 C12 119.2(5) . . ? C16 C11 C10 105.4(4) . . ? C12 C11 C10 135.4(5) . . ? C13 C12 C11 118.1(5) . . ? C14 C13 C12 121.7(5) . . ? C13 C14 C15 121.6(5) . . ? C16 C15 C14 115.9(5) . . ? C16 C15 S2 122.2(4) . 2_656 ? C14 C15 S2 121.6(4) . 2_656 ? O1 C16 C15 124.4(4) . . ? O1 C16 C11 112.2(4) . . ? C15 C16 C11 123.4(4) . . ? O1 C17 C10 112.5(4) . . ? O1 C17 C6 123.9(4) . . ? C10 C17 C6 123.6(5) . . ? C22 C18 C19 118.3(4) . . ? C22 C18 S2 116.4(4) . . ? C19 C18 S2 125.3(4) . . ? C20 C19 C18 119.1(5) . . ? N2 C20 C19 122.7(5) . . ? N2 C21 C22 123.4(5) . . ? C21 C22 C18 119.1(5) . . ? Cl4 C24 Cl3 112.9(5) . . ? C5 N1 C1 117.3(4) . . ? C5 N1 Ag1 122.2(3) . . ? C1 N1 Ag1 120.1(3) . . ? C21 N2 C20 117.4(4) . . ? C21 N2 Ag1 120.6(3) . . ? C20 N2 Ag1 121.4(3) . . ? O12 O12A Cl5 57.8(10) . . ? O11 O11A Cl5 75.8(9) . . ? O11 O11A O12 127.8(11) . . ? Cl5 O11A O12 53.2(8) . . ? C16 O1 C17 105.1(4) . . ? O11A O11 Cl5 60.8(8) . . ? O12A O12 Cl5 83.6(11) . . ? O12A O12 O11A 137.6(17) . . ? Cl5 O12 O11A 55.8(10) . . ? C6 S1 C3 101.6(2) . . ? C18 S2 C15 103.4(2) . 2_656 ? Cl1 C23 Cl2 106.4(11) . . ? O12 Cl5 O11A 71.0(16) . . ? O12 Cl5 O14 113.6(9) . . ? O11A Cl5 O14 124.5(6) . . ? O12 Cl5 O13 117.7(7) . . ? O11A Cl5 O13 114.5(6) . . ? O14 Cl5 O13 110.5(3) . . ? O12 Cl5 O11 113.5(15) . . ? O11A Cl5 O11 43.4(6) . . ? O14 Cl5 O11 98.2(8) . . ? O13 Cl5 O11 100.9(5) . . ? O12 Cl5 O12A 38.6(7) . . ? O11A Cl5 O12A 108.7(14) . . ? O14 Cl5 O12A 98.3(7) . . ? O13 Cl5 O12A 94.4(13) . . ? O11 Cl5 O12A 151.9(13) . . ? N2 Ag1 N1 169.43(14) . . ? N2 Ag1 Ag1 92.95(11) . 2_656 ? N1 Ag1 Ag1 96.24(11) . 2_656 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.117 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.134 #===END data_Compound_2.6CHCl3 _database_code_CSD 186276 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cu2(L)2Cl4].6CHCl3 _chemical_formula_sum 'C25 H17 Cl11 Cu N2 O S2' _chemical_formula_weight 879.02 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.050(4) _cell_length_b 12.715(5) _cell_length_c 13.400(5) _cell_angle_alpha 95.549(5) _cell_angle_beta 110.840(4) _cell_angle_gamma 106.598(5) _cell_volume 1644.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 6557 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 26.35 _exptl_crystal_description plate _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 1.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6616 _exptl_absorpt_correction_T_max 0.8143 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 20408 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 26.35 _reflns_number_total 6439 _reflns_number_gt 4506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6439 _refine_ls_number_parameters 453 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.212 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 C1 C 0.7914(6) 0.4644(5) 0.2118(5) 0.0311(13) Uani 1 1 d . . . H1 H 0.8137 0.5414 0.2430 0.037 Uiso 1 1 calc R . . C2 C 0.8948(6) 0.4199(5) 0.2406(5) 0.0299(13) Uani 1 1 d . . . H2 H 0.9848 0.4645 0.2925 0.036 Uiso 1 1 calc R . . C3 C 0.8662(6) 0.3073(5) 0.1924(4) 0.0259(12) Uani 1 1 d . . . C4 C 0.7324(6) 0.2484(5) 0.1177(5) 0.0315(13) Uani 1 1 d . . . H4 H 0.7082 0.1728 0.0813 0.038 Uiso 1 1 calc R . . C5 C 0.6331(6) 0.3004(5) 0.0959(5) 0.0308(13) Uani 1 1 d . . . H5 H 0.5417 0.2579 0.0454 0.037 Uiso 1 1 calc R . . C6 C 0.9216(6) 0.1146(5) 0.1508(5) 0.0292(13) Uani 1 1 d . . . C7 C 0.8912(6) 0.0222(5) 0.1956(5) 0.0327(14) Uani 1 1 d . . . H7 H 0.9104 0.0328 0.2716 0.039 Uiso 1 1 calc R . . C8 C 0.8321(6) -0.0871(5) 0.1298(5) 0.0349(14) Uani 1 1 d . . . H8 H 0.8135 -0.1495 0.1625 0.042 Uiso 1 1 calc R . . C9 C 0.7999(6) -0.1067(5) 0.0169(5) 0.0313(13) Uani 1 1 d . . . H9 H 0.7579 -0.1810 -0.0269 0.038 Uiso 1 1 calc R . . C10 C 0.8307(6) -0.0154(5) -0.0288(5) 0.0282(13) Uani 1 1 d . . . C11 C 0.8154(6) 0.0027(5) -0.1401(5) 0.0297(13) Uani 1 1 d . . . C12 C 0.7644(6) -0.0656(5) -0.2436(5) 0.0344(14) Uani 1 1 d . . . H12 H 0.7295 -0.1451 -0.2540 0.041 Uiso 1 1 calc R . . C13 C 0.7649(7) -0.0162(5) -0.3322(5) 0.0367(14) Uani 1 1 d . . . H13 H 0.7287 -0.0625 -0.4035 0.044 Uiso 1 1 calc R . . C14 C 0.8187(7) 0.1017(5) -0.3169(5) 0.0367(15) Uani 1 1 d . . . H14 H 0.8192 0.1338 -0.3779 0.044 Uiso 1 1 calc R . . C15 C 0.8713(6) 0.1722(5) -0.2133(5) 0.0293(13) Uani 1 1 d . . . C16 C 0.8685(6) 0.1190(5) -0.1262(5) 0.0278(12) Uani 1 1 d . . . C17 C 0.8920(6) 0.0937(5) 0.0393(5) 0.0267(12) Uani 1 1 d . . . C18 C 0.8221(6) 0.3678(5) -0.1624(5) 0.0275(12) Uani 1 1 d . . . C19 C 0.6846(6) 0.2976(5) -0.1886(5) 0.0299(13) Uani 1 1 d . . . H19 H 0.6548 0.2191 -0.2178 0.036 Uiso 1 1 calc R . . C20 C 0.5957(6) 0.3460(5) -0.1705(5) 0.0310(13) Uani 1 1 d . . . H20 H 0.5040 0.2985 -0.1877 0.037 Uiso 1 1 calc R . . C21 C 0.7630(6) 0.5212(5) -0.1021(4) 0.0278(12) Uani 1 1 d . . . H21 H 0.7909 0.5990 -0.0708 0.033 Uiso 1 1 calc R . . C22 C 0.8592(6) 0.4806(5) -0.1165(5) 0.0275(12) Uani 1 1 d . . . H22 H 0.9513 0.5298 -0.0951 0.033 Uiso 1 1 calc R . . N1 N 0.6599(5) 0.4062(4) 0.1422(4) 0.0277(11) Uani 1 1 d . . . N2 N 0.6303(5) 0.4562(4) -0.1301(4) 0.0272(10) Uani 1 1 d . . . O1 O 0.9145(4) 0.1762(3) -0.0193(3) 0.0287(9) Uani 1 1 d . . . S1 S 1.00232(16) 0.25330(12) 0.23222(12) 0.0329(4) Uani 1 1 d . . . S2 S 0.94616(16) 0.31883(13) -0.18819(13) 0.0332(4) Uani 1 1 d . . . Cl1 Cl 0.63678(15) 0.62783(11) 0.08351(12) 0.0300(3) Uani 1 1 d . . . Cl2 Cl 0.43441(15) 0.34620(12) 0.22168(12) 0.0325(4) Uani 1 1 d . . . Cu1 Cu 0.50964(7) 0.47160(5) 0.12589(6) 0.0259(2) Uani 1 1 d . . . C23 C 1.3628(8) 0.6099(8) 0.5046(6) 0.063(2) Uani 1 1 d . . . H23 H 1.4303 0.5993 0.5724 0.076 Uiso 1 1 calc R . . Cl11 Cl 1.2064(3) 0.5921(4) 0.5203(3) 0.1467(17) Uani 1 1 d . . . Cl12 Cl 1.4279(4) 0.7454(2) 0.4901(2) 0.1051(11) Uani 1 1 d . . . Cl13 Cl 1.3379(3) 0.50982(18) 0.39272(16) 0.0713(7) Uani 1 1 d . . . C24A C 1.4190(10) -0.0725(8) 1.7285(6) 0.054(3) Uani 0.766(8) 1 d PDU A 1 H24A H 1.4743 -0.1218 1.7255 0.065 Uiso 0.766(8) 1 calc PR A 1 Cl21 Cl 1.2468(12) -0.1517(11) 1.6931(10) 0.422(8) Uani 0.766(8) 1 d PDU A 1 Cl22 Cl 1.4066(6) 0.0059(3) 1.6269(3) 0.1097(19) Uani 0.766(8) 1 d PDU A 1 Cl23 Cl 1.4869(3) 0.0163(2) 1.8602(2) 0.0498(10) Uani 0.766(8) 1 d PDU A 1 C24 C 1.388(6) -0.070(3) 1.743(2) 0.257(13) Uani 0.234(8) 1 d PDU A 2 H24 H 1.3073 -0.0978 1.7630 0.308 Uiso 0.234(8) 1 calc PR A 2 Cl24 Cl 1.419(3) -0.190(3) 1.7222(19) 0.278(12) Uani 0.234(8) 1 d PDU A 2 Cl25 Cl 1.317(3) -0.023(3) 1.6315(15) 0.244(12) Uani 0.234(8) 1 d PDU A 2 Cl26 Cl 1.500(3) 0.027(3) 1.8587(18) 0.253(12) Uani 0.234(8) 1 d PDU A 2 C25 C 0.8561(15) -0.2393(11) 0.396(2) 0.126(6) Uani 0.499(10) 1 d PDU B 3 H25 H 0.8443 -0.2485 0.3181 0.151 Uiso 0.499(10) 1 calc PR B 3 Cl31 Cl 0.9787(9) -0.2960(7) 0.4702(6) 0.108(3) Uani 0.499(10) 1 d PDU B 3 Cl32 Cl 0.7004(9) -0.3074(10) 0.4057(12) 0.147(4) Uani 0.499(10) 1 d PDU B 3 Cl33 Cl 0.9298(9) -0.0970(6) 0.4630(6) 0.121(3) Uani 0.499(10) 1 d PDU . 3 C25A C 0.8592(14) -0.2316(12) 0.482(2) 0.242(10) Uani 0.501(10) 1 d PDU B 4 H25A H 0.8847 -0.2116 0.5622 0.290 Uiso 0.501(10) 1 calc PR B 4 Cl34 Cl 0.9779(15) -0.2467(18) 0.4489(17) 0.301(9) Uani 0.501(10) 1 d PDU B 4 Cl35 Cl 0.6994(13) -0.3585(14) 0.4045(14) 0.231(7) Uani 0.501(10) 1 d PDU B 4 Cl36 Cl 0.7881(19) -0.1384(14) 0.4051(13) 0.293(8) Uani 0.501(10) 1 d PDU B 4 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 C1 0.037(3) 0.019(3) 0.039(3) 0.003(2) 0.019(3) 0.008(3) C2 0.029(3) 0.026(3) 0.032(3) 0.004(2) 0.012(3) 0.006(2) C3 0.029(3) 0.024(3) 0.026(3) 0.006(2) 0.013(2) 0.009(2) C4 0.037(3) 0.025(3) 0.034(3) 0.004(2) 0.014(3) 0.012(3) C5 0.028(3) 0.020(3) 0.040(3) 0.006(2) 0.010(3) 0.007(2) C6 0.025(3) 0.027(3) 0.037(3) 0.008(2) 0.013(3) 0.011(2) C7 0.029(3) 0.036(3) 0.035(3) 0.014(3) 0.011(3) 0.014(3) C8 0.038(3) 0.026(3) 0.048(4) 0.016(3) 0.019(3) 0.016(3) C9 0.031(3) 0.027(3) 0.039(3) 0.010(2) 0.015(3) 0.012(3) C10 0.027(3) 0.024(3) 0.035(3) 0.007(2) 0.012(3) 0.012(2) C11 0.028(3) 0.026(3) 0.040(3) 0.008(2) 0.014(3) 0.015(3) C12 0.035(3) 0.032(3) 0.038(3) 0.006(3) 0.015(3) 0.016(3) C13 0.039(4) 0.038(4) 0.037(3) 0.006(3) 0.018(3) 0.018(3) C14 0.043(4) 0.045(4) 0.034(3) 0.016(3) 0.019(3) 0.026(3) C15 0.032(3) 0.027(3) 0.036(3) 0.008(2) 0.016(3) 0.015(3) C16 0.025(3) 0.031(3) 0.033(3) 0.008(2) 0.015(2) 0.015(2) C17 0.027(3) 0.023(3) 0.034(3) 0.009(2) 0.012(2) 0.014(2) C18 0.032(3) 0.029(3) 0.029(3) 0.012(2) 0.014(2) 0.016(3) C19 0.035(3) 0.026(3) 0.035(3) 0.010(2) 0.018(3) 0.013(3) C20 0.030(3) 0.027(3) 0.039(3) 0.010(3) 0.017(3) 0.011(3) C21 0.032(3) 0.022(3) 0.028(3) 0.005(2) 0.011(3) 0.009(2) C22 0.026(3) 0.027(3) 0.030(3) 0.012(2) 0.010(2) 0.009(2) N1 0.030(3) 0.021(2) 0.035(3) 0.007(2) 0.016(2) 0.009(2) N2 0.032(3) 0.020(2) 0.031(3) 0.0062(19) 0.014(2) 0.008(2) O1 0.034(2) 0.020(2) 0.033(2) 0.0076(16) 0.0144(18) 0.0106(17) S1 0.0307(8) 0.0283(8) 0.0354(8) 0.0038(6) 0.0065(6) 0.0136(6) S2 0.0344(8) 0.0294(8) 0.0487(9) 0.0160(7) 0.0261(7) 0.0152(7) Cl1 0.0326(8) 0.0212(7) 0.0390(8) 0.0081(6) 0.0182(6) 0.0081(6) Cl2 0.0381(8) 0.0290(8) 0.0329(8) 0.0110(6) 0.0163(6) 0.0110(6) Cu1 0.0282(4) 0.0205(4) 0.0333(4) 0.0079(3) 0.0154(3) 0.0102(3) C23 0.051(5) 0.087(6) 0.036(4) 0.006(4) 0.008(4) 0.015(4) Cl11 0.076(2) 0.261(5) 0.083(2) -0.003(2) 0.0347(16) 0.040(3) Cl12 0.157(3) 0.0643(16) 0.0675(16) 0.0033(12) 0.0329(17) 0.0193(17) Cl13 0.0977(17) 0.0597(13) 0.0374(10) 0.0060(9) 0.0130(11) 0.0190(12) C24A 0.068(6) 0.049(5) 0.046(5) 0.005(4) 0.023(5) 0.022(5) Cl21 0.366(12) 0.290(11) 0.363(12) -0.010(10) -0.027(10) 0.006(10) Cl22 0.134(4) 0.098(3) 0.058(2) 0.0287(19) 0.008(2) 0.019(3) Cl23 0.0395(15) 0.0507(16) 0.0471(17) -0.0003(11) 0.0180(12) 0.0011(11) C24 0.155(15) 0.53(4) 0.111(12) 0.035(16) 0.042(11) 0.183(19) Cl24 0.172(14) 0.54(4) 0.129(11) 0.036(15) 0.039(10) 0.171(19) Cl25 0.146(13) 0.53(4) 0.099(10) 0.032(14) 0.049(9) 0.195(18) Cl26 0.154(14) 0.53(4) 0.107(11) 0.034(15) 0.044(10) 0.186(19) C25 0.147(10) 0.131(10) 0.119(10) 0.031(9) 0.054(9) 0.073(9) Cl31 0.129(6) 0.128(6) 0.091(4) 0.021(4) 0.060(4) 0.058(4) Cl32 0.098(6) 0.180(9) 0.155(8) 0.083(7) 0.024(5) 0.056(6) Cl33 0.145(7) 0.132(6) 0.105(5) 0.035(4) 0.066(5) 0.052(5) C25A 0.185(15) 0.43(2) 0.237(15) 0.209(16) 0.165(13) 0.144(15) Cl34 0.206(12) 0.462(19) 0.291(13) 0.191(13) 0.167(10) 0.075(13) Cl35 0.204(10) 0.397(18) 0.231(11) 0.243(12) 0.154(9) 0.161(11) Cl36 0.245(13) 0.443(19) 0.241(11) 0.208(12) 0.121(10) 0.120(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.347(7) . ? C1 C2 1.368(8) . ? C2 C3 1.410(8) . ? C3 C4 1.385(8) . ? C3 S1 1.763(6) . ? C4 C5 1.397(8) . ? C5 N1 1.327(7) . ? C6 C7 1.381(8) . ? C6 C17 1.390(8) . ? C6 S1 1.770(6) . ? C7 C8 1.404(8) . ? C8 C9 1.403(9) . ? C9 C10 1.378(8) . ? C10 C17 1.412(7) . ? C10 C11 1.488(8) . ? C11 C12 1.388(8) . ? C11 C16 1.392(8) . ? C12 C13 1.397(9) . ? C13 C14 1.410(9) . ? C14 C15 1.399(8) . ? C15 C16 1.409(8) . ? C15 S2 1.753(6) . ? C16 O1 1.380(7) . ? C17 O1 1.389(7) . ? C18 C22 1.385(8) . ? C18 C19 1.419(8) . ? C18 S2 1.780(6) . ? C19 C20 1.375(8) . ? C20 N2 1.342(7) . ? C21 N2 1.353(7) . ? C21 C22 1.369(8) . ? N1 Cu1 2.016(5) . ? N2 Cu1 2.025(5) 2_665 ? Cl1 Cu1 2.3309(16) . ? Cl1 Cu1 2.6466(18) 2_665 ? Cl2 Cu1 2.2976(17) . ? Cu1 N2 2.025(5) 2_665 ? Cu1 Cl1 2.6466(18) 2_665 ? C23 Cl12 1.727(10) . ? C23 Cl13 1.755(8) . ? C23 Cl11 1.768(9) . ? C24A Cl21 1.741(12) . ? C24A Cl22 1.752(9) . ? C24A Cl23 1.773(8) . ? C24 Cl24 1.678(16) . ? C24 Cl26 1.682(17) . ? C24 Cl25 1.684(16) . ? C25 Cl32 1.746(15) . ? C25 Cl33 1.750(14) . ? C25 Cl31 1.754(15) . ? Cl33 Cl33 2.393(15) 2_756 ? C25A Cl34 1.576(18) . ? C25A Cl36 1.808(18) . ? C25A Cl35 1.882(18) . ? 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 C1 C2 124.3(5) . . ? C1 C2 C3 119.2(5) . . ? C4 C3 C2 116.7(5) . . ? C4 C3 S1 125.7(4) . . ? C2 C3 S1 117.6(4) . . ? C3 C4 C5 119.8(5) . . ? N1 C5 C4 123.4(5) . . ? C7 C6 C17 117.1(5) . . ? C7 C6 S1 121.7(5) . . ? C17 C6 S1 121.2(4) . . ? C6 C7 C8 120.4(6) . . ? C9 C8 C7 121.8(6) . . ? C10 C9 C8 118.4(5) . . ? C9 C10 C17 118.8(5) . . ? C9 C10 C11 136.3(5) . . ? C17 C10 C11 104.9(5) . . ? C12 C11 C16 119.4(6) . . ? C12 C11 C10 135.8(6) . . ? C16 C11 C10 104.7(5) . . ? C11 C12 C13 119.3(6) . . ? C12 C13 C14 120.6(6) . . ? C15 C14 C13 121.1(6) . . ? C14 C15 C16 116.5(5) . . ? C14 C15 S2 123.1(5) . . ? C16 C15 S2 120.3(4) . . ? O1 C16 C11 113.0(5) . . ? O1 C16 C15 123.9(5) . . ? C11 C16 C15 123.1(5) . . ? O1 C17 C6 124.8(5) . . ? O1 C17 C10 111.7(5) . . ? C6 C17 C10 123.5(5) . . ? C22 C18 C19 117.5(5) . . ? C22 C18 S2 119.0(4) . . ? C19 C18 S2 123.5(4) . . ? C20 C19 C18 118.3(5) . . ? N2 C20 C19 124.1(5) . . ? N2 C21 C22 123.3(5) . . ? C21 C22 C18 119.9(5) . . ? C5 N1 C1 116.6(5) . . ? C5 N1 Cu1 122.2(4) . . ? C1 N1 Cu1 120.7(4) . . ? C20 N2 C21 116.7(5) . . ? C20 N2 Cu1 123.0(4) . 2_665 ? C21 N2 Cu1 119.9(4) . 2_665 ? C16 O1 C17 105.6(4) . . ? C3 S1 C6 101.9(3) . . ? C15 S2 C18 103.1(3) . . ? Cu1 Cl1 Cu1 87.95(5) . 2_665 ? N1 Cu1 N2 172.84(18) . 2_665 ? N1 Cu1 Cl2 87.18(14) . . ? N2 Cu1 Cl2 89.68(14) 2_665 . ? N1 Cu1 Cl1 88.94(14) . . ? N2 Cu1 Cl1 92.10(14) 2_665 . ? Cl2 Cu1 Cl1 162.09(6) . . ? N1 Cu1 Cl1 94.82(14) . 2_665 ? N2 Cu1 Cl1 92.22(14) 2_665 2_665 ? Cl2 Cu1 Cl1 105.70(6) . 2_665 ? Cl1 Cu1 Cl1 92.05(5) . 2_665 ? Cl12 C23 Cl13 111.5(5) . . ? Cl12 C23 Cl11 108.9(5) . . ? Cl13 C23 Cl11 110.9(5) . . ? Cl21 C24A Cl22 101.9(7) . . ? Cl21 C24A Cl23 109.4(7) . . ? Cl22 C24A Cl23 111.2(5) . . ? Cl24 C24 Cl26 117.1(17) . . ? Cl24 C24 Cl25 116.6(17) . . ? Cl26 C24 Cl25 117.4(17) . . ? Cl32 C25 Cl33 113.2(12) . . ? Cl32 C25 Cl31 108.4(11) . . ? Cl33 C25 Cl31 102.7(10) . . ? C25 Cl33 Cl33 166.5(9) . 2_756 ? Cl34 C25A Cl36 108.6(14) . . ? Cl34 C25A Cl35 108.2(14) . . ? Cl36 C25A Cl35 93.4(10) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.121 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.134 #===END #===END data_Compound_3.2MeCN' _database_code_CSD 201745 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Cu4(L2)2I4.2MeCN _chemical_formula_sum 'C56 H50 Cu4 I4 N6 O2 S4' _chemical_formula_weight 1729.02 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.843(5) _cell_length_b 12.283(5) _cell_length_c 13.537(5) _cell_angle_alpha 79.209(5) _cell_angle_beta 88.332(5) _cell_angle_gamma 77.788(5) _cell_volume 1571.2(12) _cell_formula_units_Z 1 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 4352 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.13 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 3.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5873 _exptl_absorpt_correction_T_max 0.8700 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 19251 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.11 _reflns_number_total 5985 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5985 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1186 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.008 _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 C1 C 0.3274(8) 0.0390(7) 0.9185(7) 0.043(2) Uani 1 1 d . . . H1 H 0.2745 0.0947 0.9499 0.052 Uiso 1 1 calc R . . C2 C 0.3680(9) -0.0677(8) 0.9724(7) 0.053(3) Uani 1 1 d . . . H2 H 0.3472 -0.0858 1.0402 0.064 Uiso 1 1 calc R . . C3 C 0.4402(9) -0.1454(7) 0.9222(8) 0.051(3) Uani 1 1 d . . . H3 H 0.4697 -0.2193 0.9567 0.061 Uiso 1 1 calc R . . C4 C 0.4732(8) -0.1198(7) 0.8192(7) 0.045(2) Uani 1 1 d . . . H4 H 0.5205 -0.1767 0.7867 0.054 Uiso 1 1 calc R . . C5 C 0.4354(7) -0.0125(6) 0.7685(6) 0.033(2) Uani 1 1 d . . . C6 C 0.4725(7) 0.0252(6) 0.6541(6) 0.037(2) Uani 1 1 d . . . H6A H 0.4812 -0.0393 0.6208 0.045 Uiso 1 1 calc R . . H6B H 0.5623 0.0463 0.6512 0.045 Uiso 1 1 calc R . . C7 C 0.1836(7) 0.0896(6) 0.5938(5) 0.0270(18) Uani 1 1 d . . . H7A H 0.1713 0.0515 0.6620 0.032 Uiso 1 1 calc R . . H7B H 0.1056 0.1531 0.5767 0.032 Uiso 1 1 calc R . . C8 C 0.1879(7) 0.0099(6) 0.5235(5) 0.0236(17) Uani 1 1 d . . . C9 C 0.2326(7) -0.1043(6) 0.5567(5) 0.0266(18) Uani 1 1 d . . . H9 H 0.2611 -0.1321 0.6232 0.032 Uiso 1 1 calc R . . C10 C 0.2351(7) -0.1765(6) 0.4919(6) 0.0306(19) Uani 1 1 d . . . H10 H 0.2670 -0.2537 0.5152 0.037 Uiso 1 1 calc R . . C11 C 0.1911(7) -0.1394(6) 0.3900(6) 0.0275(18) Uani 1 1 d . . . H11 H 0.1949 -0.1917 0.3479 0.033 Uiso 1 1 calc R . . C12 C 0.1433(6) -0.0271(6) 0.3544(5) 0.0201(16) Uani 1 1 d . . . C13 C 0.0897(7) 0.0426(6) 0.2573(5) 0.0235(17) Uani 1 1 d . . . C14 C 0.0634(8) 0.0236(6) 0.1609(5) 0.0319(19) Uani 1 1 d . . . H14 H 0.0794 -0.0502 0.1489 0.038 Uiso 1 1 calc R . . C15 C 0.0141(8) 0.1136(7) 0.0837(6) 0.040(2) Uani 1 1 d . . . H15 H -0.0020 0.1004 0.0200 0.049 Uiso 1 1 calc R . . C16 C -0.0107(8) 0.2210(7) 0.1016(6) 0.037(2) Uani 1 1 d . . . H16 H -0.0421 0.2816 0.0495 0.045 Uiso 1 1 calc R . . C17 C 0.0110(7) 0.2417(6) 0.1993(6) 0.0273(18) Uani 1 1 d . . . C18 C 0.0641(7) 0.1482(6) 0.2745(6) 0.0247(17) Uani 1 1 d . . . C19 C 0.1441(7) 0.0436(6) 0.4219(5) 0.0232(17) Uani 1 1 d . . . C20 C -0.0230(7) 0.3561(6) 0.2203(6) 0.0278(18) Uani 1 1 d . . . H20A H -0.0171 0.4094 0.1584 0.033 Uiso 1 1 calc R . . H20B H 0.0453 0.3641 0.2672 0.033 Uiso 1 1 calc R . . C21 C -0.3121(8) 0.3792(6) 0.1726(5) 0.0314(19) Uani 1 1 d . . . H21A H -0.2902 0.3007 0.1642 0.038 Uiso 1 1 calc R . . H21B H -0.4084 0.3959 0.1931 0.038 Uiso 1 1 calc R . . C22 C -0.2987(7) 0.4541(6) 0.0705(6) 0.0272(18) Uani 1 1 d . . . C23 C -0.3140(8) 0.4250(7) -0.0243(6) 0.037(2) Uani 1 1 d . . . H23 H -0.3282 0.3530 -0.0262 0.045 Uiso 1 1 calc R . . C24 C -0.3089(8) 0.4988(6) -0.1137(6) 0.038(2) Uani 1 1 d . . . H24 H -0.3221 0.4784 -0.1749 0.045 Uiso 1 1 calc R . . C25 C -0.2846(8) 0.5994(7) -0.1096(6) 0.038(2) Uani 1 1 d . . . H25 H -0.2816 0.6531 -0.1676 0.045 Uiso 1 1 calc R . . C26 C -0.2636(8) 0.6218(6) -0.0148(6) 0.036(2) Uani 1 1 d . . . H26 H -0.2420 0.6913 -0.0123 0.043 Uiso 1 1 calc R . . C27 C 0.2746(13) 0.4648(10) 0.4689(8) 0.101(4) Uani 1 1 d . . . H27A H 0.2104 0.4266 0.5088 0.151 Uiso 1 1 calc R . . H27B H 0.2245 0.5342 0.4295 0.151 Uiso 1 1 calc R . . H27C H 0.3399 0.4814 0.5123 0.151 Uiso 1 1 calc R . . C28 C 0.3496(14) 0.3916(10) 0.4016(9) 0.075(4) Uani 1 1 d . . . N1 N 0.3622(6) 0.0679(5) 0.8172(5) 0.0315(16) Uani 1 1 d . . . N2 N -0.2717(6) 0.5517(5) 0.0741(5) 0.0285(15) Uani 1 1 d . . . N3 N 0.4075(13) 0.3340(9) 0.3499(7) 0.103(4) Uani 1 1 d . . . O1 O 0.0974(5) 0.1516(4) 0.3739(3) 0.0232(11) Uani 1 1 d . . . S1 S 0.3478(2) 0.14142(16) 0.58567(15) 0.0309(5) Uani 1 1 d . . . S2 S -0.2026(2) 0.39365(16) 0.27480(15) 0.0314(5) Uani 1 1 d . . . Cu1 Cu 0.31045(10) 0.22584(7) 0.73170(7) 0.0354(3) Uani 1 1 d . . . Cu2 Cu -0.25344(10) 0.58658(7) 0.21914(7) 0.0355(3) Uani 1 1 d . . . I1 I 0.04403(6) 0.32070(4) 0.76534(5) 0.04095(19) Uani 1 1 d . . . I2 I 0.51949(6) 0.32336(5) 0.73938(5) 0.0456(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(5) 0.039(5) 0.050(6) -0.011(5) -0.009(5) -0.002(4) C2 0.056(7) 0.051(6) 0.053(7) 0.001(5) -0.017(5) -0.020(5) C3 0.048(6) 0.027(5) 0.069(8) 0.016(5) -0.015(5) -0.007(4) C4 0.044(6) 0.027(5) 0.065(7) -0.012(5) -0.006(5) -0.003(4) C5 0.019(4) 0.024(4) 0.052(6) -0.007(4) -0.014(4) 0.004(3) C6 0.021(4) 0.033(5) 0.065(6) -0.022(4) -0.006(4) -0.009(4) C7 0.023(4) 0.030(4) 0.030(5) -0.011(4) 0.004(4) -0.007(3) C8 0.019(4) 0.029(4) 0.027(5) -0.008(3) 0.010(3) -0.014(3) C9 0.026(5) 0.033(4) 0.020(4) -0.003(4) 0.000(3) -0.008(4) C10 0.039(5) 0.007(3) 0.043(5) 0.000(3) -0.005(4) -0.002(3) C11 0.027(4) 0.015(4) 0.043(5) -0.011(4) 0.007(4) -0.006(3) C12 0.008(4) 0.022(4) 0.031(5) -0.007(3) 0.004(3) -0.002(3) C13 0.024(4) 0.019(4) 0.032(5) -0.012(3) 0.003(4) -0.008(3) C14 0.041(5) 0.030(4) 0.027(5) -0.013(4) -0.003(4) -0.006(4) C15 0.048(6) 0.041(5) 0.036(5) -0.020(4) -0.008(4) -0.005(4) C16 0.039(5) 0.037(5) 0.032(5) -0.007(4) -0.005(4) 0.001(4) C17 0.032(5) 0.015(4) 0.037(5) -0.010(3) 0.004(4) -0.006(3) C18 0.019(4) 0.019(4) 0.037(5) -0.007(3) 0.008(4) -0.004(3) C19 0.024(4) 0.021(4) 0.027(5) -0.011(3) -0.004(3) -0.004(3) C20 0.024(4) 0.024(4) 0.031(5) -0.004(3) -0.001(4) 0.004(3) C21 0.032(5) 0.031(4) 0.035(5) -0.013(4) -0.002(4) -0.008(4) C22 0.028(5) 0.020(4) 0.033(5) -0.004(4) -0.002(4) -0.005(3) C23 0.036(5) 0.026(4) 0.055(6) -0.014(4) -0.004(4) -0.011(4) C24 0.045(5) 0.028(5) 0.043(6) -0.018(4) -0.016(4) 0.000(4) C25 0.039(5) 0.030(5) 0.039(6) -0.001(4) -0.004(4) 0.001(4) C26 0.043(5) 0.024(4) 0.040(6) -0.005(4) 0.000(4) -0.007(4) C27 0.142(13) 0.092(10) 0.061(8) -0.008(7) 0.000(8) -0.014(9) C28 0.123(11) 0.062(8) 0.035(7) 0.020(6) -0.005(7) -0.037(8) N1 0.029(4) 0.032(4) 0.038(4) -0.014(3) 0.000(3) -0.009(3) N2 0.027(4) 0.021(3) 0.037(4) -0.008(3) -0.003(3) 0.001(3) N3 0.180(12) 0.074(8) 0.051(7) 0.005(6) -0.001(7) -0.031(8) O1 0.033(3) 0.015(2) 0.022(3) -0.004(2) -0.004(2) -0.003(2) S1 0.0370(12) 0.0262(10) 0.0350(13) -0.0110(9) 0.0039(10) -0.0149(9) S2 0.0415(13) 0.0222(10) 0.0290(12) -0.0048(9) 0.0003(10) -0.0031(9) Cu1 0.0445(7) 0.0199(5) 0.0441(7) -0.0123(5) -0.0043(5) -0.0058(4) Cu2 0.0451(7) 0.0204(5) 0.0419(7) -0.0128(5) -0.0017(5) -0.0024(4) I1 0.0328(3) 0.0339(3) 0.0590(4) -0.0175(3) -0.0027(3) -0.0050(2) I2 0.0336(4) 0.0379(3) 0.0757(5) -0.0333(3) 0.0071(3) -0.0115(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 C1 C2 1.359(11) . ? C1 N1 1.402(10) . ? C2 C3 1.344(12) . ? C3 C4 1.414(12) . ? C4 C5 1.348(10) . ? C5 N1 1.358(9) . ? C5 C6 1.587(11) . ? C6 S1 1.798(8) . ? C7 C8 1.482(9) . ? C7 S1 1.851(7) . ? C8 C9 1.371(9) . ? C8 C19 1.412(9) . ? C9 C10 1.355(9) . ? C10 C11 1.419(10) . ? C11 C12 1.358(9) . ? C12 C19 1.374(9) . ? C12 C13 1.472(10) . ? C13 C18 1.331(9) . ? C13 C14 1.409(9) . ? C14 C15 1.386(10) . ? C15 C16 1.356(10) . ? C16 C17 1.423(10) . ? C17 C18 1.403(10) . ? C17 C20 1.454(9) . ? C18 O1 1.403(8) . ? C19 O1 1.353(8) . ? C20 S2 1.895(7) . ? C21 C22 1.529(10) . ? C21 S2 1.834(7) . ? C22 N2 1.292(9) . ? C22 C23 1.415(10) . ? C23 C24 1.376(11) . ? C24 C25 1.318(10) . ? C25 C26 1.392(10) . ? C26 N2 1.353(9) . ? C27 C28 1.474(16) . ? C28 N3 1.143(14) . ? N1 Cu1 2.034(6) . ? N2 Cu2 2.106(6) . ? S1 Cu1 2.384(2) . ? S2 Cu2 2.299(2) . ? Cu1 Cu2 2.4641(15) 2_566 ? Cu1 I2 2.6040(15) . ? Cu1 I1 2.6978(16) . ? Cu2 Cu1 2.4641(15) 2_566 ? Cu2 I1 2.5880(15) 2_566 ? Cu2 I2 2.7052(16) 2_566 ? I1 Cu2 2.5880(15) 2_566 ? I2 Cu2 2.7052(16) 2_566 ? 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 C2 C1 N1 122.3(8) . . ? C3 C2 C1 116.1(9) . . ? C2 C3 C4 123.0(8) . . ? C5 C4 C3 119.5(8) . . ? C4 C5 N1 118.8(8) . . ? C4 C5 C6 123.2(7) . . ? N1 C5 C6 118.0(6) . . ? C5 C6 S1 114.6(5) . . ? C8 C7 S1 109.5(5) . . ? C9 C8 C19 116.0(6) . . ? C9 C8 C7 120.0(7) . . ? C19 C8 C7 123.9(6) . . ? C10 C9 C8 119.5(7) . . ? C9 C10 C11 122.9(6) . . ? C12 C11 C10 119.6(6) . . ? C11 C12 C19 115.9(7) . . ? C11 C12 C13 135.7(7) . . ? C19 C12 C13 108.4(6) . . ? C18 C13 C14 119.3(7) . . ? C18 C13 C12 103.9(6) . . ? C14 C13 C12 136.7(6) . . ? C15 C14 C13 120.7(7) . . ? C16 C15 C14 119.6(7) . . ? C15 C16 C17 120.5(7) . . ? C18 C17 C16 117.9(6) . . ? C18 C17 C20 121.4(7) . . ? C16 C17 C20 120.7(7) . . ? C13 C18 C17 121.9(7) . . ? C13 C18 O1 111.8(6) . . ? C17 C18 O1 126.3(6) . . ? O1 C19 C12 108.3(6) . . ? O1 C19 C8 125.6(6) . . ? C12 C19 C8 126.1(6) . . ? C17 C20 S2 113.3(5) . . ? C22 C21 S2 116.2(5) . . ? N2 C22 C23 119.1(7) . . ? N2 C22 C21 115.3(6) . . ? C23 C22 C21 125.6(7) . . ? C24 C23 C22 122.9(7) . . ? C25 C24 C23 117.8(8) . . ? C24 C25 C26 117.1(8) . . ? N2 C26 C25 126.1(7) . . ? N3 C28 C27 179.4(13) . . ? C5 N1 C1 120.2(7) . . ? C5 N1 Cu1 114.8(5) . . ? C1 N1 Cu1 125.1(5) . . ? C22 N2 C26 116.9(7) . . ? C22 N2 Cu2 115.8(5) . . ? C26 N2 Cu2 127.2(5) . . ? C19 O1 C18 107.6(5) . . ? C6 S1 C7 104.5(3) . . ? C6 S1 Cu1 90.1(3) . . ? C7 S1 Cu1 96.0(2) . . ? C21 S2 C20 101.1(3) . . ? C21 S2 Cu2 88.7(2) . . ? C20 S2 Cu2 100.3(2) . . ? N1 Cu1 S1 88.53(19) . . ? N1 Cu1 Cu2 130.54(18) . 2_566 ? S1 Cu1 Cu2 140.79(7) . 2_566 ? N1 Cu1 I2 107.33(17) . . ? S1 Cu1 I2 105.23(6) . . ? Cu2 Cu1 I2 64.45(4) 2_566 . ? N1 Cu1 I1 109.83(18) . . ? S1 Cu1 I1 115.51(6) . . ? Cu2 Cu1 I1 59.98(3) 2_566 . ? I2 Cu1 I1 124.37(5) . . ? N2 Cu2 S2 86.82(17) . . ? N2 Cu2 Cu1 126.67(16) . 2_566 ? S2 Cu2 Cu1 145.83(7) . 2_566 ? N2 Cu2 I1 112.13(17) . 2_566 ? S2 Cu2 I1 112.81(7) . 2_566 ? Cu1 Cu2 I1 64.50(4) 2_566 2_566 ? N2 Cu2 I2 102.32(16) . 2_566 ? S2 Cu2 I2 110.92(7) . 2_566 ? Cu1 Cu2 I2 60.28(3) 2_566 2_566 ? I1 Cu2 I2 124.72(5) 2_566 2_566 ? Cu2 I1 Cu1 55.53(4) 2_566 . ? Cu1 I2 Cu2 55.27(4) . 2_566 ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 0.920 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.140 #===END