# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Chi, Dae Yoon' 'Fun, H.' 'Hermann, W. A.' 'Song, Y.' 'Wang, Y.' 'Xin, X.' _publ_contact_author_name 'Prof Dae Yoon Chi' _publ_contact_author_address ; Department of Chemistry University of Kansas 5018 Malott Hall Lawrence KS 66045 UNITED STATES OF AMERICA ; _publ_contact_author_email 'CHIZHANG@KU.EDU' _publ_section_title ; Sign alteration of nonlinear refraction of the isomorphous cubane-shaped heterothiometallic clusters originating from a skeleton atomic effect ; data_cluster_1 _database_code_CSD 162907 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H21 Br Cu3 Mo N3 O S3' _chemical_formula_weight 758.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.1287(5) _cell_length_b 11.9739(5) _cell_length_c 18.9832(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2529.59(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6218 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 29.58 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.815 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2490 _exptl_absorpt_correction_T_max 0.2761 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18246 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.49 _reflns_number_total 6373 _reflns_number_gt 5111 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(8) _refine_ls_number_reflns 6373 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 Br1 Br 0.28631(4) -0.09913(4) -0.05677(3) 0.05215(13) Uani 1 1 d . . . Mo Mo -0.03682(3) -0.03676(3) -0.147015(18) 0.03297(8) Uani 1 1 d . . . Cu1 Cu 0.19256(5) -0.01642(4) -0.18874(3) 0.04831(14) Uani 1 1 d . . . Cu2 Cu 0.07282(6) -0.21695(4) -0.09491(3) 0.04659(14) Uani 1 1 d . . . Cu3 Cu 0.08095(6) 0.04063(5) -0.03449(3) 0.05265(15) Uani 1 1 d . . . S1 S 0.06931(10) -0.16406(8) -0.20996(5) 0.0388(2) Uani 1 1 d . . . S2 S -0.05449(9) -0.10237(9) -0.03496(5) 0.0394(2) Uani 1 1 d . . . S3 S 0.07535(11) 0.12183(8) -0.14277(6) 0.0424(2) Uani 1 1 d . . . O1 O -0.1752(3) -0.0130(3) -0.18455(18) 0.0589(9) Uani 1 1 d . . . N1 N 0.1298(4) 0.1307(3) 0.04813(19) 0.0472(9) Uani 1 1 d . . . N2 N 0.1023(3) -0.3774(3) -0.07726(18) 0.0370(8) Uani 1 1 d . . . N3 N 0.3411(3) 0.0132(3) -0.24289(18) 0.0406(8) Uani 1 1 d . . . C1 C 0.2459(5) 0.1338(4) 0.0669(2) 0.0498(12) Uani 1 1 d . . . H1A H 0.3003 0.0913 0.0412 0.060 Uiso 1 1 calc R . . C2 C 0.2886(5) 0.1960(5) 0.1220(3) 0.0617(14) Uani 1 1 d . . . H2A H 0.3702 0.1970 0.1325 0.074 Uiso 1 1 calc R . . C3 C 0.2091(5) 0.2563(4) 0.1609(3) 0.0604(14) Uani 1 1 d . . . H3A H 0.2351 0.2980 0.1993 0.072 Uiso 1 1 calc R . . C4 C 0.0901(5) 0.2544(4) 0.1425(3) 0.0580(13) Uani 1 1 d . . . H4A H 0.0348 0.2956 0.1685 0.070 Uiso 1 1 calc R . . C5 C 0.0516(5) 0.1919(4) 0.0857(2) 0.0479(11) Uani 1 1 d . . . C6 C -0.0779(5) 0.1886(5) 0.0641(3) 0.0810(18) Uani 1 1 d . . . H6A H -0.0866 0.1418 0.0233 0.122 Uiso 1 1 calc R . . H6B H -0.1047 0.2628 0.0531 0.122 Uiso 1 1 calc R . . H6C H -0.1253 0.1590 0.1020 0.122 Uiso 1 1 calc R . . C7 C 0.1001(4) -0.4479(3) -0.1330(2) 0.0462(11) Uani 1 1 d . . . H7A H 0.0905 -0.4181 -0.1779 0.055 Uiso 1 1 calc R . . C8 C 0.1113(5) -0.5611(3) -0.1261(3) 0.0515(12) Uani 1 1 d . . . H8A H 0.1082 -0.6074 -0.1654 0.062 Uiso 1 1 calc R . . C9 C 0.1273(5) -0.6048(4) -0.0603(3) 0.0630(15) Uani 1 1 d . . . H9A H 0.1349 -0.6816 -0.0543 0.076 Uiso 1 1 calc R . . C10 C 0.1322(5) -0.5344(4) -0.0027(3) 0.0534(12) Uani 1 1 d . . . H10A H 0.1439 -0.5635 0.0422 0.064 Uiso 1 1 calc R . . C11 C 0.1196(4) -0.4193(3) -0.0123(2) 0.0370(9) Uani 1 1 d . . . C12 C 0.1208(4) -0.3406(4) 0.0486(2) 0.0498(11) Uani 1 1 d . . . H12A H 0.1095 -0.2657 0.0319 0.075 Uiso 1 1 calc R . . H12B H 0.1966 -0.3459 0.0726 0.075 Uiso 1 1 calc R . . H12C H 0.0572 -0.3596 0.0806 0.075 Uiso 1 1 calc R . . C13 C 0.4463(4) -0.0295(4) -0.2194(3) 0.0568(12) Uani 1 1 d . . . H13A H 0.4459 -0.0728 -0.1787 0.068 Uiso 1 1 calc R . . C14 C 0.5536(5) -0.0113(5) -0.2531(3) 0.0726(16) Uani 1 1 d . . . H14A H 0.6247 -0.0411 -0.2355 0.087 Uiso 1 1 calc R . . C15 C 0.5538(5) 0.0516(5) -0.3134(3) 0.0761(17) Uani 1 1 d . . . H15A H 0.6249 0.0650 -0.3377 0.091 Uiso 1 1 calc R . . C16 C 0.4450(6) 0.0953(5) -0.3377(3) 0.0739(16) Uani 1 1 d . . . H16A H 0.4433 0.1381 -0.3786 0.089 Uiso 1 1 calc R . . C17 C 0.3413(4) 0.0754(4) -0.3014(3) 0.0532(12) Uani 1 1 d . . . C18 C 0.2241(5) 0.1221(6) -0.3261(3) 0.085(2) Uani 1 1 d . . . H18A H 0.1613 0.0989 -0.2947 0.127 Uiso 1 1 calc R . . H18B H 0.2074 0.0952 -0.3727 0.127 Uiso 1 1 calc R . . H18C H 0.2285 0.2021 -0.3268 0.127 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 Br1 0.0364(2) 0.0680(3) 0.0521(3) 0.0047(2) -0.0077(2) 0.0030(2) Mo 0.02918(16) 0.03463(16) 0.03512(17) 0.00006(16) -0.00701(14) 0.00203(14) Cu1 0.0397(3) 0.0461(3) 0.0591(3) -0.0008(3) 0.0120(3) -0.0049(2) Cu2 0.0630(4) 0.0350(2) 0.0417(3) 0.0056(2) 0.0028(3) 0.0105(3) Cu3 0.0645(4) 0.0552(3) 0.0383(3) -0.0055(3) -0.0093(3) -0.0182(3) S1 0.0460(6) 0.0371(5) 0.0334(5) -0.0042(4) -0.0006(4) 0.0004(5) S2 0.0359(6) 0.0439(5) 0.0384(5) 0.0011(5) 0.0038(4) -0.0033(5) S3 0.0515(6) 0.0302(5) 0.0456(6) 0.0010(5) -0.0021(5) -0.0006(4) O1 0.0436(18) 0.070(2) 0.063(2) -0.0014(18) -0.0206(16) 0.0111(16) N1 0.054(2) 0.049(2) 0.039(2) -0.0010(18) -0.0058(18) -0.0121(18) N2 0.0358(19) 0.0344(16) 0.041(2) 0.0010(15) -0.0043(15) -0.0004(15) N3 0.0377(19) 0.0444(19) 0.040(2) 0.0013(17) 0.0012(15) -0.0059(16) C1 0.049(3) 0.055(3) 0.045(3) -0.003(2) -0.004(2) -0.005(2) C2 0.058(3) 0.072(3) 0.055(3) 0.000(3) -0.016(3) -0.023(3) C3 0.086(4) 0.049(3) 0.047(3) -0.002(2) -0.020(3) -0.016(3) C4 0.080(4) 0.049(2) 0.046(3) -0.013(2) 0.002(3) -0.002(3) C5 0.054(3) 0.047(2) 0.042(3) 0.002(2) -0.006(2) -0.006(2) C6 0.058(4) 0.095(4) 0.091(5) -0.015(4) -0.014(3) 0.011(3) C7 0.050(3) 0.045(2) 0.044(3) -0.006(2) -0.009(2) 0.001(2) C8 0.059(3) 0.036(2) 0.060(3) -0.008(2) -0.016(2) 0.000(2) C9 0.069(4) 0.031(2) 0.089(4) 0.001(3) -0.017(3) -0.006(2) C10 0.064(3) 0.037(2) 0.059(3) 0.013(2) -0.008(2) -0.006(2) C11 0.031(2) 0.0335(19) 0.046(3) 0.0028(19) -0.0049(18) -0.0053(17) C12 0.048(3) 0.059(3) 0.042(3) 0.010(2) -0.006(2) -0.005(2) C13 0.044(3) 0.074(3) 0.052(3) 0.000(3) 0.000(2) 0.000(3) C14 0.038(3) 0.107(4) 0.073(4) -0.014(4) -0.002(3) 0.004(3) C15 0.051(3) 0.095(4) 0.082(4) -0.015(4) 0.027(3) -0.017(3) C16 0.074(4) 0.084(4) 0.064(4) 0.019(3) 0.023(3) 0.005(3) C17 0.050(3) 0.054(3) 0.056(3) 0.006(2) 0.009(2) -0.003(2) C18 0.068(4) 0.113(5) 0.072(4) 0.042(4) 0.005(3) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu2 2.8564(8) . ? Br1 Cu3 2.8640(8) . ? Br1 Cu1 2.8888(8) . ? Mo O1 1.720(3) . ? Mo S1 2.2685(11) . ? Mo S3 2.2739(10) . ? Mo S2 2.2762(11) . ? Mo Cu2 2.6687(6) . ? Mo Cu3 2.6719(6) . ? Mo Cu1 2.6838(6) . ? Cu1 N3 1.978(3) . ? Cu1 S1 2.2735(12) . ? Cu1 S3 2.2809(12) . ? Cu2 N2 1.978(3) . ? Cu2 S1 2.2743(12) . ? Cu2 S2 2.2771(12) . ? Cu3 N1 1.980(4) . ? Cu3 S3 2.2747(12) . ? Cu3 S2 2.2812(11) . ? N1 C1 1.341(6) . ? N1 C5 1.343(6) . ? N2 C11 1.346(5) . ? N2 C7 1.354(5) . ? N3 C17 1.338(6) . ? N3 C13 1.353(6) . ? C1 C2 1.369(6) . ? C2 C3 1.360(8) . ? C3 C4 1.370(7) . ? C4 C5 1.381(6) . ? C5 C6 1.499(7) . ? C7 C8 1.368(6) . ? C8 C9 1.366(7) . ? C9 C10 1.382(7) . ? C10 C11 1.397(6) . ? C11 C12 1.491(6) . ? C13 C14 1.373(7) . ? C14 C15 1.371(8) . ? C15 C16 1.397(8) . ? C16 C17 1.364(7) . ? C17 C18 1.494(7) . ? 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 Cu2 Br1 Cu3 70.261(19) . . ? Cu2 Br1 Cu1 69.457(18) . . ? Cu3 Br1 Cu1 68.870(19) . . ? O1 Mo S1 111.03(12) . . ? O1 Mo S3 111.60(12) . . ? S1 Mo S3 107.09(4) . . ? O1 Mo S2 111.52(12) . . ? S1 Mo S2 107.78(4) . . ? S3 Mo S2 107.61(4) . . ? O1 Mo Cu2 134.13(11) . . ? S1 Mo Cu2 54.12(3) . . ? S3 Mo Cu2 114.27(3) . . ? S2 Mo Cu2 54.13(3) . . ? O1 Mo Cu3 135.47(11) . . ? S1 Mo Cu3 113.50(3) . . ? S3 Mo Cu3 54.04(3) . . ? S2 Mo Cu3 54.19(3) . . ? Cu2 Mo Cu3 76.10(2) . . ? O1 Mo Cu1 135.57(12) . . ? S1 Mo Cu1 53.87(3) . . ? S3 Mo Cu1 54.02(3) . . ? S2 Mo Cu1 112.91(3) . . ? Cu2 Mo Cu1 75.40(2) . . ? Cu3 Mo Cu1 74.80(2) . . ? N3 Cu1 S1 123.44(10) . . ? N3 Cu1 S3 123.13(10) . . ? S1 Cu1 S3 106.68(4) . . ? N3 Cu1 Mo 164.62(11) . . ? S1 Cu1 Mo 53.69(3) . . ? S3 Cu1 Mo 53.78(3) . . ? N3 Cu1 Br1 102.14(10) . . ? S1 Cu1 Br1 96.03(3) . . ? S3 Cu1 Br1 97.10(4) . . ? Mo Cu1 Br1 93.24(2) . . ? N2 Cu2 S1 115.85(10) . . ? N2 Cu2 S2 127.14(11) . . ? S1 Cu2 S2 107.55(4) . . ? N2 Cu2 Mo 157.51(10) . . ? S1 Cu2 Mo 53.92(3) . . ? S2 Cu2 Mo 54.10(3) . . ? N2 Cu2 Br1 107.40(10) . . ? S1 Cu2 Br1 96.90(4) . . ? S2 Cu2 Br1 95.35(3) . . ? Mo Cu2 Br1 94.30(2) . . ? N1 Cu3 S3 119.38(11) . . ? N1 Cu3 S2 126.40(11) . . ? S3 Cu3 S2 107.41(4) . . ? N1 Cu3 Mo 163.15(12) . . ? S3 Cu3 Mo 54.01(3) . . ? S2 Cu3 Mo 54.02(3) . . ? N1 Cu3 Br1 102.48(12) . . ? S3 Cu3 Br1 97.94(4) . . ? S2 Cu3 Br1 95.06(3) . . ? Mo Cu3 Br1 94.06(2) . . ? Mo S1 Cu1 72.44(3) . . ? Mo S1 Cu2 71.95(3) . . ? Cu1 S1 Cu2 92.06(4) . . ? Mo S2 Cu2 71.76(3) . . ? Mo S2 Cu3 71.79(3) . . ? Cu2 S2 Cu3 92.46(4) . . ? Mo S3 Cu3 71.95(3) . . ? Mo S3 Cu1 72.20(3) . . ? Cu3 S3 Cu1 91.14(4) . . ? C1 N1 C5 117.9(4) . . ? C1 N1 Cu3 119.4(3) . . ? C5 N1 Cu3 122.7(3) . . ? C11 N2 C7 119.1(3) . . ? C11 N2 Cu2 122.8(3) . . ? C7 N2 Cu2 118.1(3) . . ? C17 N3 C13 118.8(4) . . ? C17 N3 Cu1 122.2(3) . . ? C13 N3 Cu1 119.0(3) . . ? N1 C1 C2 123.6(5) . . ? C3 C2 C1 118.5(5) . . ? C2 C3 C4 118.8(5) . . ? C3 C4 C5 120.5(5) . . ? N1 C5 C4 120.6(5) . . ? N1 C5 C6 117.6(4) . . ? C4 C5 C6 121.8(5) . . ? N2 C7 C8 122.8(4) . . ? C9 C8 C7 118.6(4) . . ? C8 C9 C10 119.7(4) . . ? C9 C10 C11 119.7(4) . . ? N2 C11 C10 120.1(4) . . ? N2 C11 C12 118.5(3) . . ? C10 C11 C12 121.4(4) . . ? N3 C13 C14 122.7(5) . . ? C15 C14 C13 118.5(5) . . ? C14 C15 C16 118.7(5) . . ? C17 C16 C15 120.1(5) . . ? N3 C17 C16 121.2(5) . . ? N3 C17 C18 117.8(4) . . ? C16 C17 C18 121.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo Cu1 N3 1.0(4) . . . . ? S1 Mo Cu1 N3 84.7(4) . . . . ? S3 Mo Cu1 N3 -83.8(4) . . . . ? S2 Mo Cu1 N3 -179.5(4) . . . . ? Cu2 Mo Cu1 N3 140.7(4) . . . . ? Cu3 Mo Cu1 N3 -140.1(4) . . . . ? O1 Mo Cu1 S1 -83.68(16) . . . . ? S3 Mo Cu1 S1 -168.47(5) . . . . ? S2 Mo Cu1 S1 95.85(5) . . . . ? Cu2 Mo Cu1 S1 55.97(4) . . . . ? Cu3 Mo Cu1 S1 135.23(4) . . . . ? O1 Mo Cu1 S3 84.79(16) . . . . ? S1 Mo Cu1 S3 168.47(5) . . . . ? S2 Mo Cu1 S3 -95.69(5) . . . . ? Cu2 Mo Cu1 S3 -135.56(4) . . . . ? Cu3 Mo Cu1 S3 -56.31(4) . . . . ? O1 Mo Cu1 Br1 -178.78(16) . . . . ? S1 Mo Cu1 Br1 -95.10(4) . . . . ? S3 Mo Cu1 Br1 96.43(4) . . . . ? S2 Mo Cu1 Br1 0.75(4) . . . . ? Cu2 Mo Cu1 Br1 -39.13(2) . . . . ? Cu3 Mo Cu1 Br1 40.13(2) . . . . ? Cu2 Br1 Cu1 N3 -142.40(10) . . . . ? Cu3 Br1 Cu1 N3 141.59(10) . . . . ? Cu2 Br1 Cu1 S1 -16.28(3) . . . . ? Cu3 Br1 Cu1 S1 -92.28(3) . . . . ? Cu2 Br1 Cu1 S3 91.43(3) . . . . ? Cu3 Br1 Cu1 S3 15.42(3) . . . . ? Cu2 Br1 Cu1 Mo 37.539(18) . . . . ? Cu3 Br1 Cu1 Mo -38.466(18) . . . . ? O1 Mo Cu2 N2 15.6(3) . . . . ? S1 Mo Cu2 N2 -69.5(3) . . . . ? S3 Mo Cu2 N2 -163.7(3) . . . . ? S2 Mo Cu2 N2 101.5(3) . . . . ? Cu3 Mo Cu2 N2 157.2(3) . . . . ? Cu1 Mo Cu2 N2 -125.2(3) . . . . ? O1 Mo Cu2 S1 85.14(17) . . . . ? S3 Mo Cu2 S1 -94.12(5) . . . . ? S2 Mo Cu2 S1 171.08(5) . . . . ? Cu3 Mo Cu2 S1 -133.31(4) . . . . ? Cu1 Mo Cu2 S1 -55.70(4) . . . . ? O1 Mo Cu2 S2 -85.94(17) . . . . ? S1 Mo Cu2 S2 -171.08(5) . . . . ? S3 Mo Cu2 S2 94.80(5) . . . . ? Cu3 Mo Cu2 S2 55.61(4) . . . . ? Cu1 Mo Cu2 S2 133.22(4) . . . . ? O1 Mo Cu2 Br1 -179.44(17) . . . . ? S1 Mo Cu2 Br1 95.41(4) . . . . ? S3 Mo Cu2 Br1 1.29(4) . . . . ? S2 Mo Cu2 Br1 -93.50(4) . . . . ? Cu3 Mo Cu2 Br1 -37.89(2) . . . . ? Cu1 Mo Cu2 Br1 39.72(2) . . . . ? Cu3 Br1 Cu2 N2 -149.75(11) . . . . ? Cu1 Br1 Cu2 N2 136.19(11) . . . . ? Cu3 Br1 Cu2 S1 90.37(3) . . . . ? Cu1 Br1 Cu2 S1 16.30(3) . . . . ? Cu3 Br1 Cu2 S2 -18.08(3) . . . . ? Cu1 Br1 Cu2 S2 -92.15(3) . . . . ? Cu3 Br1 Cu2 Mo 36.223(18) . . . . ? Cu1 Br1 Cu2 Mo -37.843(19) . . . . ? O1 Mo Cu3 N1 -12.7(4) . . . . ? S1 Mo Cu3 N1 166.8(4) . . . . ? S3 Mo Cu3 N1 72.2(4) . . . . ? S2 Mo Cu3 N1 -97.6(4) . . . . ? Cu2 Mo Cu3 N1 -153.2(4) . . . . ? Cu1 Mo Cu3 N1 128.5(4) . . . . ? O1 Mo Cu3 S3 -84.89(17) . . . . ? S1 Mo Cu3 S3 94.62(5) . . . . ? S2 Mo Cu3 S3 -169.82(5) . . . . ? Cu2 Mo Cu3 S3 134.63(4) . . . . ? Cu1 Mo Cu3 S3 56.28(4) . . . . ? O1 Mo Cu3 S2 84.93(17) . . . . ? S1 Mo Cu3 S2 -95.56(5) . . . . ? S3 Mo Cu3 S2 169.82(5) . . . . ? Cu2 Mo Cu3 S2 -55.55(4) . . . . ? Cu1 Mo Cu3 S2 -133.90(4) . . . . ? O1 Mo Cu3 Br1 178.23(17) . . . . ? S1 Mo Cu3 Br1 -2.25(4) . . . . ? S3 Mo Cu3 Br1 -96.87(4) . . . . ? S2 Mo Cu3 Br1 93.31(4) . . . . ? Cu2 Mo Cu3 Br1 37.76(2) . . . . ? Cu1 Mo Cu3 Br1 -40.590(19) . . . . ? Cu2 Br1 Cu3 N1 147.07(11) . . . . ? Cu1 Br1 Cu3 N1 -138.06(11) . . . . ? Cu2 Br1 Cu3 S3 -90.36(3) . . . . ? Cu1 Br1 Cu3 S3 -15.49(3) . . . . ? Cu2 Br1 Cu3 S2 18.04(3) . . . . ? Cu1 Br1 Cu3 S2 92.91(3) . . . . ? Cu2 Br1 Cu3 Mo -36.160(18) . . . . ? Cu1 Br1 Cu3 Mo 38.710(18) . . . . ? O1 Mo S1 Cu1 131.80(13) . . . . ? S3 Mo S1 Cu1 9.75(4) . . . . ? S2 Mo S1 Cu1 -105.79(4) . . . . ? Cu2 Mo S1 Cu1 -98.21(4) . . . . ? Cu3 Mo S1 Cu1 -47.83(4) . . . . ? O1 Mo S1 Cu2 -129.99(13) . . . . ? S3 Mo S1 Cu2 107.96(4) . . . . ? S2 Mo S1 Cu2 -7.58(4) . . . . ? Cu3 Mo S1 Cu2 50.38(4) . . . . ? Cu1 Mo S1 Cu2 98.21(4) . . . . ? N3 Cu1 S1 Mo -161.55(13) . . . . ? S3 Cu1 S1 Mo -9.69(4) . . . . ? Br1 Cu1 S1 Mo 89.59(3) . . . . ? N3 Cu1 S1 Cu2 128.12(13) . . . . ? S3 Cu1 S1 Cu2 -80.03(5) . . . . ? Mo Cu1 S1 Cu2 -70.33(3) . . . . ? Br1 Cu1 S1 Cu2 19.26(4) . . . . ? N2 Cu2 S1 Mo 156.53(12) . . . . ? S2 Cu2 S1 Mo 7.57(4) . . . . ? Br1 Cu2 S1 Mo -90.30(3) . . . . ? N2 Cu2 S1 Cu1 -132.69(12) . . . . ? S2 Cu2 S1 Cu1 78.34(5) . . . . ? Mo Cu2 S1 Cu1 70.78(3) . . . . ? Br1 Cu2 S1 Cu1 -19.52(4) . . . . ? O1 Mo S2 Cu2 129.68(12) . . . . ? S1 Mo S2 Cu2 7.58(4) . . . . ? S3 Mo S2 Cu2 -107.61(4) . . . . ? Cu3 Mo S2 Cu2 -98.98(4) . . . . ? Cu1 Mo S2 Cu2 -49.96(4) . . . . ? O1 Mo S2 Cu3 -131.34(12) . . . . ? S1 Mo S2 Cu3 106.56(4) . . . . ? S3 Mo S2 Cu3 -8.63(5) . . . . ? Cu2 Mo S2 Cu3 98.98(4) . . . . ? Cu1 Mo S2 Cu3 49.02(4) . . . . ? N2 Cu2 S2 Mo -151.96(13) . . . . ? S1 Cu2 S2 Mo -7.55(4) . . . . ? Br1 Cu2 S2 Mo 91.44(3) . . . . ? N2 Cu2 S2 Cu3 138.14(13) . . . . ? S1 Cu2 S2 Cu3 -77.45(5) . . . . ? Mo Cu2 S2 Cu3 -69.90(3) . . . . ? Br1 Cu2 S2 Cu3 21.53(4) . . . . ? N1 Cu3 S2 Mo 159.09(15) . . . . ? S3 Cu3 S2 Mo 8.62(4) . . . . ? Br1 Cu3 S2 Mo -91.35(3) . . . . ? N1 Cu3 S2 Cu2 -131.03(15) . . . . ? S3 Cu3 S2 Cu2 78.50(5) . . . . ? Mo Cu3 S2 Cu2 69.88(3) . . . . ? Br1 Cu3 S2 Cu2 -21.46(4) . . . . ? O1 Mo S3 Cu3 131.30(13) . . . . ? S1 Mo S3 Cu3 -107.00(4) . . . . ? S2 Mo S3 Cu3 8.65(5) . . . . ? Cu2 Mo S3 Cu3 -49.27(4) . . . . ? Cu1 Mo S3 Cu3 -97.27(4) . . . . ? O1 Mo S3 Cu1 -131.43(13) . . . . ? S1 Mo S3 Cu1 -9.73(4) . . . . ? S2 Mo S3 Cu1 105.92(4) . . . . ? Cu2 Mo S3 Cu1 48.00(4) . . . . ? Cu3 Mo S3 Cu1 97.27(4) . . . . ? N1 Cu3 S3 Mo -161.54(14) . . . . ? S2 Cu3 S3 Mo -8.62(5) . . . . ? Br1 Cu3 S3 Mo 89.25(3) . . . . ? N1 Cu3 S3 Cu1 127.61(14) . . . . ? S2 Cu3 S3 Cu1 -79.47(5) . . . . ? Mo Cu3 S3 Cu1 -70.85(3) . . . . ? Br1 Cu3 S3 Cu1 18.40(4) . . . . ? N3 Cu1 S3 Mo 161.65(12) . . . . ? S1 Cu1 S3 Mo 9.68(4) . . . . ? Br1 Cu1 S3 Mo -88.82(3) . . . . ? N3 Cu1 S3 Cu3 -127.74(13) . . . . ? S1 Cu1 S3 Cu3 80.30(5) . . . . ? Mo Cu1 S3 Cu3 70.61(3) . . . . ? Br1 Cu1 S3 Cu3 -18.20(4) . . . . ? S3 Cu3 N1 C1 -91.1(3) . . . . ? S2 Cu3 N1 C1 121.6(3) . . . . ? Mo Cu3 N1 C1 -153.2(3) . . . . ? Br1 Cu3 N1 C1 15.6(4) . . . . ? S3 Cu3 N1 C5 87.2(3) . . . . ? S2 Cu3 N1 C5 -60.2(4) . . . . ? Mo Cu3 N1 C5 25.0(6) . . . . ? Br1 Cu3 N1 C5 -166.2(3) . . . . ? S1 Cu2 N2 C11 172.7(3) . . . . ? S2 Cu2 N2 C11 -45.3(4) . . . . ? Mo Cu2 N2 C11 -130.0(3) . . . . ? Br1 Cu2 N2 C11 65.8(3) . . . . ? S1 Cu2 N2 C7 -9.9(3) . . . . ? S2 Cu2 N2 C7 132.1(3) . . . . ? Mo Cu2 N2 C7 47.4(5) . . . . ? Br1 Cu2 N2 C7 -116.8(3) . . . . ? S1 Cu1 N3 C17 89.5(3) . . . . ? S3 Cu1 N3 C17 -57.9(4) . . . . ? Mo Cu1 N3 C17 15.4(6) . . . . ? Br1 Cu1 N3 C17 -164.8(3) . . . . ? S1 Cu1 N3 C13 -91.6(3) . . . . ? S3 Cu1 N3 C13 121.0(3) . . . . ? Mo Cu1 N3 C13 -165.7(3) . . . . ? Br1 Cu1 N3 C13 14.1(3) . . . . ? C5 N1 C1 C2 -0.2(7) . . . . ? Cu3 N1 C1 C2 178.1(4) . . . . ? N1 C1 C2 C3 1.5(8) . . . . ? C1 C2 C3 C4 -1.5(7) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C1 N1 C5 C4 -1.0(6) . . . . ? Cu3 N1 C5 C4 -179.3(3) . . . . ? C1 N1 C5 C6 179.7(4) . . . . ? Cu3 N1 C5 C6 1.4(6) . . . . ? C3 C4 C5 N1 0.9(7) . . . . ? C3 C4 C5 C6 -179.8(5) . . . . ? C11 N2 C7 C8 1.9(7) . . . . ? Cu2 N2 C7 C8 -175.5(4) . . . . ? N2 C7 C8 C9 -1.1(8) . . . . ? C7 C8 C9 C10 -0.3(8) . . . . ? C8 C9 C10 C11 0.7(8) . . . . ? C7 N2 C11 C10 -1.5(6) . . . . ? Cu2 N2 C11 C10 175.9(3) . . . . ? C7 N2 C11 C12 -179.6(4) . . . . ? Cu2 N2 C11 C12 -2.2(5) . . . . ? C9 C10 C11 N2 0.2(7) . . . . ? C9 C10 C11 C12 178.2(5) . . . . ? C17 N3 C13 C14 0.1(7) . . . . ? Cu1 N3 C13 C14 -178.9(4) . . . . ? N3 C13 C14 C15 -0.7(8) . . . . ? C13 C14 C15 C16 0.5(9) . . . . ? C14 C15 C16 C17 0.2(9) . . . . ? C13 N3 C17 C16 0.6(7) . . . . ? Cu1 N3 C17 C16 179.5(4) . . . . ? C13 N3 C17 C18 -179.7(5) . . . . ? Cu1 N3 C17 C18 -0.8(6) . . . . ? C15 C16 C17 N3 -0.8(9) . . . . ? C15 C16 C17 C18 179.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 29.49 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.413 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.100 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag # D H A symm D-H H...A D...A D-H...A flag example O7 H7 N10 . . 1_555 0.94(4) 1.74(3) 2.617(3) 154(3) yes #============================================================================END # CLUSTER 2 data_cluster_2 _database_code_CSD 162908 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H21 Cu3 I N3 O S3 W' _chemical_formula_weight 892.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.968(5) _cell_length_b 19.102(4) _cell_length_c 11.209(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2562.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 4.59 _cell_measurement_theta_max 12.49 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 8.395 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.023 _exptl_absorpt_correction_T_max 0.008 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.7 _diffrn_reflns_number 3315 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3116 _reflns_number_gt 2771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0510P)^2^+2.0645P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(13) _refine_ls_number_reflns 3116 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 W1 W 0.53551(4) 0.85314(2) 0.52387(4) 0.06146(14) Uani 1 1 d . . . I1 I 0.59837(9) 0.94436(5) 0.18991(8) 0.0794(3) Uani 1 1 d . . . Cu1 Cu 0.71626(12) 0.90530(8) 0.41502(18) 0.0773(4) Uani 1 1 d . . . Cu2 Cu 0.51713(15) 0.81073(9) 0.29439(15) 0.0802(4) Uani 1 1 d . . . Cu3 Cu 0.45500(15) 0.96482(8) 0.40628(17) 0.0823(4) Uani 1 1 d . . . S1 S 0.6632(3) 0.79000(15) 0.4222(3) 0.0682(7) Uani 1 1 d . . . S2 S 0.5991(3) 0.96395(15) 0.5413(3) 0.0669(7) Uani 1 1 d . . . S3 S 0.3766(2) 0.85487(17) 0.4154(3) 0.0720(7) Uani 1 1 d . . . O1 O 0.5125(8) 0.8154(5) 0.6666(7) 0.079(2) Uani 1 1 d . . . N1 N 0.8777(8) 0.9216(5) 0.3898(9) 0.064(2) Uani 1 1 d . . . N2 N 0.4860(9) 0.7520(5) 0.1509(9) 0.071(3) Uani 1 1 d . . . N3 N 0.3642(9) 1.0487(5) 0.3656(11) 0.077(3) Uani 1 1 d . . . C11 C 0.9444(10) 0.8674(8) 0.4008(13) 0.079(4) Uani 1 1 d . . . H11A H 0.9131 0.8243 0.4197 0.095 Uiso 1 1 calc R . . C12 C 1.0605(11) 0.8713(8) 0.3855(15) 0.088(4) Uani 1 1 d . . . H12A H 1.1058 0.8318 0.3890 0.105 Uiso 1 1 calc R . . C13 C 1.1040(11) 0.9376(7) 0.3648(14) 0.082(4) Uani 1 1 d . . . H13A H 1.1809 0.9438 0.3590 0.098 Uiso 1 1 calc R . . C14 C 1.0354(12) 0.9931(7) 0.3531(14) 0.084(4) Uani 1 1 d . . . H14A H 1.0643 1.0373 0.3372 0.100 Uiso 1 1 calc R . . C15 C 0.9226(10) 0.9835(6) 0.3650(11) 0.066(3) Uani 1 1 d . . . C16 C 0.8444(12) 1.0452(6) 0.3572(12) 0.075(3) Uani 1 1 d . . . H16A H 0.7840 1.0343 0.3039 0.112 Uiso 1 1 calc R . . H16B H 0.8843 1.0852 0.3277 0.112 Uiso 1 1 calc R . . H16C H 0.8150 1.0554 0.4349 0.112 Uiso 1 1 calc R . . C21 C 0.5272(14) 0.7719(8) 0.0427(12) 0.092(4) Uani 1 1 d . . . H21A H 0.5715 0.8118 0.0372 0.110 Uiso 1 1 calc R . . C22 C 0.5050(17) 0.7354(8) -0.0543(15) 0.105(6) Uani 1 1 d . . . H22A H 0.5351 0.7498 -0.1268 0.126 Uiso 1 1 calc R . . C23 C 0.4410(16) 0.6788(10) -0.0514(17) 0.111(6) Uani 1 1 d . . . H23A H 0.4236 0.6550 -0.1213 0.134 Uiso 1 1 calc R . . C24 C 0.4020(18) 0.6564(9) 0.0531(19) 0.116(6) Uani 1 1 d . . . H24A H 0.3594 0.6158 0.0569 0.139 Uiso 1 1 calc R . . C25 C 0.4253(13) 0.6943(7) 0.1575(14) 0.085(4) Uani 1 1 d . . . C26 C 0.3789(19) 0.6744(9) 0.2732(17) 0.122(7) Uani 1 1 d . . . H26A H 0.4376 0.6732 0.3315 0.182 Uiso 1 1 calc R . . H26B H 0.3451 0.6290 0.2671 0.182 Uiso 1 1 calc R . . H26C H 0.3236 0.7081 0.2968 0.182 Uiso 1 1 calc R . . C31 C 0.3581(13) 1.0670(8) 0.2488(14) 0.088(4) Uani 1 1 d . . . H31A H 0.3964 1.0415 0.1911 0.106 Uiso 1 1 calc R . . C32 C 0.2942(15) 1.1240(8) 0.2171(14) 0.090(4) Uani 1 1 d . . . H32A H 0.2918 1.1374 0.1373 0.108 Uiso 1 1 calc R . . C33 C 0.2354(13) 1.1610(8) 0.2973(17) 0.093(4) Uani 1 1 d . . . H33A H 0.1930 1.1994 0.2737 0.111 Uiso 1 1 calc R . . C34 C 0.2391(12) 1.1410(7) 0.4146(19) 0.097(5) Uani 1 1 d . . . H34A H 0.1978 1.1654 0.4714 0.116 Uiso 1 1 calc R . . C35 C 0.3058(12) 1.0833(7) 0.4495(13) 0.082(4) Uani 1 1 d . . . C36 C 0.3107(19) 1.0575(9) 0.5694(16) 0.120(6) Uani 1 1 d . . . H36A H 0.2825 1.0105 0.5717 0.180 Uiso 1 1 calc R . . H36B H 0.2661 1.0868 0.6202 0.180 Uiso 1 1 calc R . . H36C H 0.3867 1.0580 0.5966 0.180 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 W1 0.0585(2) 0.0620(2) 0.0639(2) 0.0073(2) 0.0027(2) 0.0000(2) I1 0.0926(6) 0.0801(5) 0.0655(4) 0.0073(4) 0.0015(5) -0.0078(5) Cu1 0.0583(7) 0.0729(9) 0.1005(11) -0.0027(9) 0.0106(9) -0.0055(7) Cu2 0.0752(10) 0.0873(10) 0.0781(9) -0.0142(8) -0.0055(9) 0.0007(9) Cu3 0.0785(9) 0.0664(8) 0.1019(11) 0.0085(8) -0.0178(10) 0.0042(8) S1 0.0605(15) 0.0613(15) 0.0826(19) 0.0003(15) -0.0027(16) 0.0050(13) S2 0.0666(15) 0.0662(15) 0.0677(17) -0.0049(14) -0.0016(15) 0.0000(13) S3 0.0505(13) 0.0710(16) 0.095(2) 0.0001(18) -0.0031(15) -0.0036(14) O1 0.084(6) 0.085(5) 0.069(5) 0.007(4) 0.016(5) -0.003(5) N1 0.058(5) 0.062(5) 0.070(6) 0.005(5) -0.002(5) -0.002(4) N2 0.071(6) 0.065(5) 0.077(6) -0.005(5) -0.012(6) 0.005(5) N3 0.072(6) 0.067(6) 0.092(7) 0.004(6) -0.009(6) -0.004(5) C11 0.054(6) 0.097(9) 0.087(9) 0.014(7) 0.000(6) -0.008(6) C12 0.072(8) 0.090(9) 0.101(10) 0.003(8) 0.009(8) 0.029(7) C13 0.064(7) 0.080(8) 0.101(10) 0.017(8) -0.007(8) -0.007(7) C14 0.069(7) 0.083(8) 0.099(10) -0.001(8) -0.001(9) -0.025(8) C15 0.076(7) 0.067(6) 0.057(6) 0.016(5) -0.014(6) -0.013(6) C16 0.082(8) 0.066(7) 0.076(7) -0.004(6) -0.002(7) -0.001(6) C21 0.109(10) 0.083(8) 0.083(9) -0.001(7) 0.007(10) -0.006(9) C22 0.140(16) 0.086(9) 0.089(10) -0.020(8) 0.003(10) 0.021(11) C23 0.118(14) 0.114(13) 0.102(13) -0.023(11) -0.005(11) 0.002(11) C24 0.123(13) 0.080(9) 0.144(17) -0.029(11) -0.011(14) -0.005(10) C25 0.092(10) 0.074(8) 0.090(9) -0.004(7) 0.006(8) -0.008(8) C26 0.153(18) 0.091(10) 0.121(14) -0.013(10) 0.022(14) -0.035(12) C31 0.088(9) 0.092(9) 0.084(9) 0.014(8) -0.017(8) -0.003(8) C32 0.106(11) 0.088(9) 0.077(9) 0.017(8) -0.012(9) 0.004(9) C33 0.084(9) 0.079(9) 0.115(12) 0.011(9) -0.013(10) 0.014(8) C34 0.080(8) 0.061(7) 0.149(15) 0.012(9) 0.007(10) -0.003(7) C35 0.075(7) 0.083(8) 0.088(10) 0.015(7) 0.001(7) 0.003(7) C36 0.144(16) 0.114(12) 0.103(12) 0.016(11) 0.026(12) 0.002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.776(8) . ? W1 S2 2.258(3) . ? W1 S1 2.255(3) . ? W1 S3 2.257(3) . ? W1 Cu1 2.6758(18) . ? W1 Cu3 2.6863(17) . ? W1 Cu2 2.7056(17) . ? I1 Cu2 2.972(2) . ? I1 Cu1 2.986(2) . ? I1 Cu3 2.996(2) . ? Cu1 N1 1.977(9) . ? Cu1 S2 2.286(4) . ? Cu1 S1 2.294(3) . ? Cu2 N2 1.996(10) . ? Cu2 S1 2.294(4) . ? Cu2 S3 2.320(4) . ? Cu3 N3 1.989(11) . ? Cu3 S2 2.294(4) . ? Cu3 S3 2.303(4) . ? N1 C11 1.313(16) . ? N1 C15 1.329(14) . ? N2 C25 1.321(16) . ? N2 C21 1.364(17) . ? N3 C35 1.345(18) . ? N3 C31 1.358(19) . ? C11 C12 1.402(18) . ? C12 C13 1.389(19) . ? C13 C14 1.35(2) . ? C14 C15 1.369(18) . ? C15 C16 1.508(17) . ? C21 C22 1.32(2) . ? C22 C23 1.33(2) . ? C23 C24 1.33(2) . ? C24 C25 1.40(2) . ? C25 C26 1.46(2) . ? C31 C32 1.378(19) . ? C32 C33 1.34(2) . ? C33 C34 1.37(2) . ? C34 C35 1.416(19) . ? C35 C36 1.43(2) . ? 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 O1 W1 S2 110.8(3) . . ? O1 W1 S1 110.1(3) . . ? S2 W1 S1 108.48(11) . . ? O1 W1 S3 111.1(3) . . ? S2 W1 S3 108.47(12) . . ? S1 W1 S3 107.85(12) . . ? O1 W1 Cu1 133.4(3) . . ? S2 W1 Cu1 54.41(9) . . ? S1 W1 Cu1 54.64(9) . . ? S3 W1 Cu1 115.48(10) . . ? O1 W1 Cu3 135.1(3) . . ? S2 W1 Cu3 54.47(9) . . ? S1 W1 Cu3 114.82(10) . . ? S3 W1 Cu3 54.69(9) . . ? Cu1 W1 Cu3 76.74(6) . . ? O1 W1 Cu2 136.2(3) . . ? S2 W1 Cu2 112.99(9) . . ? S1 W1 Cu2 54.18(9) . . ? S3 W1 Cu2 54.84(10) . . ? Cu1 W1 Cu2 75.15(6) . . ? Cu3 W1 Cu2 75.06(6) . . ? Cu2 I1 Cu1 66.85(5) . . ? Cu2 I1 Cu3 66.78(5) . . ? Cu1 I1 Cu3 67.61(5) . . ? N1 Cu1 S2 127.7(3) . . ? N1 Cu1 S1 115.3(3) . . ? S2 Cu1 S1 106.19(13) . . ? N1 Cu1 W1 156.0(3) . . ? S2 Cu1 W1 53.43(8) . . ? S1 Cu1 W1 53.31(9) . . ? N1 Cu1 I1 107.5(3) . . ? S2 Cu1 I1 96.37(10) . . ? S1 Cu1 I1 97.98(10) . . ? W1 Cu1 I1 95.53(6) . . ? N2 Cu2 S1 123.3(3) . . ? N2 Cu2 S3 122.7(3) . . ? S1 Cu2 S3 104.47(13) . . ? N2 Cu2 W1 161.7(3) . . ? S1 Cu2 W1 52.85(9) . . ? S3 Cu2 W1 52.71(9) . . ? N2 Cu2 I1 103.1(3) . . ? S1 Cu2 I1 98.35(10) . . ? S3 Cu2 I1 98.94(10) . . ? W1 Cu2 I1 95.21(5) . . ? N3 Cu3 S2 124.6(3) . . ? N3 Cu3 S3 121.5(3) . . ? S2 Cu3 S3 105.68(12) . . ? N3 Cu3 W1 161.5(4) . . ? S2 Cu3 W1 53.20(8) . . ? S3 Cu3 W1 53.13(9) . . ? N3 Cu3 I1 103.4(4) . . ? S2 Cu3 I1 95.89(10) . . ? S3 Cu3 I1 98.65(10) . . ? W1 Cu3 I1 95.06(6) . . ? W1 S1 Cu1 72.05(10) . . ? W1 S1 Cu2 72.97(10) . . ? Cu1 S1 Cu2 91.34(12) . . ? W1 S2 Cu1 72.16(10) . . ? W1 S2 Cu3 72.33(10) . . ? Cu1 S2 Cu3 93.22(13) . . ? W1 S3 Cu3 72.18(10) . . ? W1 S3 Cu2 72.46(10) . . ? Cu3 S3 Cu2 90.57(12) . . ? C11 N1 C15 118.4(10) . . ? C11 N1 Cu1 117.2(8) . . ? C15 N1 Cu1 124.4(8) . . ? C25 N2 C21 118.8(12) . . ? C25 N2 Cu2 121.7(10) . . ? C21 N2 Cu2 119.5(9) . . ? C35 N3 C31 121.4(13) . . ? C35 N3 Cu3 121.3(10) . . ? C31 N3 Cu3 117.2(10) . . ? N1 C11 C12 123.3(13) . . ? C13 C12 C11 116.1(13) . . ? C14 C13 C12 120.3(12) . . ? C13 C14 C15 119.2(13) . . ? N1 C15 C14 122.5(13) . . ? N1 C15 C16 117.2(11) . . ? C14 C15 C16 120.2(12) . . ? C22 C21 N2 120.9(14) . . ? C21 C22 C23 121.8(18) . . ? C22 C23 C24 119.1(17) . . ? C23 C24 C25 119.9(16) . . ? N2 C25 C24 119.5(15) . . ? N2 C25 C26 118.4(14) . . ? C24 C25 C26 122.0(14) . . ? N3 C31 C32 118.8(15) . . ? C33 C32 C31 122.3(15) . . ? C34 C33 C32 118.6(14) . . ? C33 C34 C35 120.0(16) . . ? N3 C35 C36 117.8(14) . . ? N3 C35 C34 118.8(14) . . ? C36 C35 C34 123.4(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 W1 Cu1 N1 16.2(8) . . . . ? S2 W1 Cu1 N1 101.8(8) . . . . ? S1 W1 Cu1 N1 -68.5(7) . . . . ? S3 W1 Cu1 N1 -163.0(8) . . . . ? Cu3 W1 Cu1 N1 157.3(8) . . . . ? Cu2 W1 Cu1 N1 -124.9(7) . . . . ? O1 W1 Cu1 S2 -85.6(4) . . . . ? S1 W1 Cu1 S2 -170.32(15) . . . . ? S3 W1 Cu1 S2 95.19(14) . . . . ? Cu3 W1 Cu1 S2 55.56(11) . . . . ? Cu2 W1 Cu1 S2 133.35(11) . . . . ? O1 W1 Cu1 S1 84.7(4) . . . . ? S2 W1 Cu1 S1 170.32(15) . . . . ? S3 W1 Cu1 S1 -94.49(14) . . . . ? Cu3 W1 Cu1 S1 -134.12(12) . . . . ? Cu2 W1 Cu1 S1 -56.33(11) . . . . ? O1 W1 Cu1 I1 -179.4(4) . . . . ? S2 W1 Cu1 I1 -93.84(11) . . . . ? S1 W1 Cu1 I1 95.84(12) . . . . ? S3 W1 Cu1 I1 1.35(11) . . . . ? Cu3 W1 Cu1 I1 -38.28(5) . . . . ? Cu2 W1 Cu1 I1 39.51(5) . . . . ? Cu2 I1 Cu1 N1 135.9(3) . . . . ? Cu3 I1 Cu1 N1 -150.8(3) . . . . ? Cu2 I1 Cu1 S2 -91.24(10) . . . . ? Cu3 I1 Cu1 S2 -17.96(9) . . . . ? Cu2 I1 Cu1 S1 16.15(9) . . . . ? Cu3 I1 Cu1 S1 89.44(10) . . . . ? Cu2 I1 Cu1 W1 -37.51(5) . . . . ? Cu3 I1 Cu1 W1 35.78(5) . . . . ? O1 W1 Cu2 N2 2.5(11) . . . . ? S2 W1 Cu2 N2 -178.9(10) . . . . ? S1 W1 Cu2 N2 84.3(10) . . . . ? S3 W1 Cu2 N2 -81.9(10) . . . . ? Cu1 W1 Cu2 N2 141.1(10) . . . . ? Cu3 W1 Cu2 N2 -138.9(10) . . . . ? O1 W1 Cu2 S1 -81.8(5) . . . . ? S2 W1 Cu2 S1 96.80(13) . . . . ? S3 W1 Cu2 S1 -166.19(15) . . . . ? Cu1 W1 Cu2 S1 56.83(11) . . . . ? Cu3 W1 Cu2 S1 136.76(11) . . . . ? O1 W1 Cu2 S3 84.3(5) . . . . ? S2 W1 Cu2 S3 -97.01(14) . . . . ? S1 W1 Cu2 S3 166.19(15) . . . . ? Cu1 W1 Cu2 S3 -136.98(12) . . . . ? Cu3 W1 Cu2 S3 -57.06(11) . . . . ? O1 W1 Cu2 I1 -178.4(4) . . . . ? S2 W1 Cu2 I1 0.27(10) . . . . ? S1 W1 Cu2 I1 -96.53(11) . . . . ? S3 W1 Cu2 I1 97.28(11) . . . . ? Cu1 W1 Cu2 I1 -39.70(5) . . . . ? Cu3 W1 Cu2 I1 40.23(6) . . . . ? Cu1 I1 Cu2 N2 -143.3(3) . . . . ? Cu3 I1 Cu2 N2 142.2(3) . . . . ? Cu1 I1 Cu2 S1 -16.16(9) . . . . ? Cu3 I1 Cu2 S1 -90.66(10) . . . . ? Cu1 I1 Cu2 S3 90.02(10) . . . . ? Cu3 I1 Cu2 S3 15.53(9) . . . . ? Cu1 I1 Cu2 W1 37.00(5) . . . . ? Cu3 I1 Cu2 W1 -37.49(5) . . . . ? O1 W1 Cu3 N3 -5.6(11) . . . . ? S2 W1 Cu3 N3 -89.9(10) . . . . ? S1 W1 Cu3 N3 174.4(10) . . . . ? S3 W1 Cu3 N3 79.5(10) . . . . ? Cu1 W1 Cu3 N3 -145.4(10) . . . . ? Cu2 W1 Cu3 N3 136.7(10) . . . . ? O1 W1 Cu3 S2 84.3(5) . . . . ? S1 W1 Cu3 S2 -95.67(14) . . . . ? S3 W1 Cu3 S2 169.38(16) . . . . ? Cu1 W1 Cu3 S2 -55.50(11) . . . . ? Cu2 W1 Cu3 S2 -133.40(11) . . . . ? O1 W1 Cu3 S3 -85.1(5) . . . . ? S2 W1 Cu3 S3 -169.38(16) . . . . ? S1 W1 Cu3 S3 94.95(14) . . . . ? Cu1 W1 Cu3 S3 135.12(12) . . . . ? Cu2 W1 Cu3 S3 57.22(12) . . . . ? O1 W1 Cu3 I1 177.9(4) . . . . ? S2 W1 Cu3 I1 93.59(11) . . . . ? S1 W1 Cu3 I1 -2.08(11) . . . . ? S3 W1 Cu3 I1 -97.03(12) . . . . ? Cu1 W1 Cu3 I1 38.08(6) . . . . ? Cu2 W1 Cu3 I1 -39.82(6) . . . . ? Cu2 I1 Cu3 N3 -141.1(3) . . . . ? Cu1 I1 Cu3 N3 145.6(3) . . . . ? Cu2 I1 Cu3 S2 91.26(9) . . . . ? Cu1 I1 Cu3 S2 17.88(8) . . . . ? Cu2 I1 Cu3 S3 -15.63(9) . . . . ? Cu1 I1 Cu3 S3 -89.02(10) . . . . ? Cu2 I1 Cu3 W1 37.80(5) . . . . ? Cu1 I1 Cu3 W1 -35.59(5) . . . . ? O1 W1 S1 Cu1 -129.6(3) . . . . ? S2 W1 S1 Cu1 -8.29(13) . . . . ? S3 W1 S1 Cu1 109.00(12) . . . . ? Cu3 W1 S1 Cu1 50.34(11) . . . . ? Cu2 W1 S1 Cu1 97.17(11) . . . . ? O1 W1 S1 Cu2 133.2(3) . . . . ? S2 W1 S1 Cu2 -105.46(11) . . . . ? S3 W1 S1 Cu2 11.83(13) . . . . ? Cu1 W1 S1 Cu2 -97.17(11) . . . . ? Cu3 W1 S1 Cu2 -46.83(10) . . . . ? N1 Cu1 S1 W1 155.3(4) . . . . ? S2 Cu1 S1 W1 8.08(12) . . . . ? I1 Cu1 S1 W1 -90.97(8) . . . . ? N1 Cu1 S1 Cu2 -133.1(4) . . . . ? S2 Cu1 S1 Cu2 79.70(15) . . . . ? W1 Cu1 S1 Cu2 71.61(10) . . . . ? I1 Cu1 S1 Cu2 -19.35(11) . . . . ? N2 Cu2 S1 W1 -158.1(4) . . . . ? S3 Cu2 S1 W1 -11.31(12) . . . . ? I1 Cu2 S1 W1 90.23(8) . . . . ? N2 Cu2 S1 Cu1 131.2(4) . . . . ? S3 Cu2 S1 Cu1 -82.08(14) . . . . ? W1 Cu2 S1 Cu1 -70.76(9) . . . . ? I1 Cu2 S1 Cu1 19.47(11) . . . . ? O1 W1 S2 Cu1 129.2(3) . . . . ? S1 W1 S2 Cu1 8.31(13) . . . . ? S3 W1 S2 Cu1 -108.59(12) . . . . ? Cu3 W1 S2 Cu1 -99.46(12) . . . . ? Cu2 W1 S2 Cu1 -49.78(10) . . . . ? O1 W1 S2 Cu3 -131.3(3) . . . . ? S1 W1 S2 Cu3 107.78(12) . . . . ? S3 W1 S2 Cu3 -9.12(13) . . . . ? Cu1 W1 S2 Cu3 99.46(12) . . . . ? Cu2 W1 S2 Cu3 49.69(11) . . . . ? N1 Cu1 S2 W1 -149.8(4) . . . . ? S1 Cu1 S2 W1 -8.07(12) . . . . ? I1 Cu1 S2 W1 92.17(7) . . . . ? N1 Cu1 S2 Cu3 139.9(4) . . . . ? S1 Cu1 S2 Cu3 -78.35(14) . . . . ? W1 Cu1 S2 Cu3 -70.28(9) . . . . ? I1 Cu1 S2 Cu3 21.90(10) . . . . ? N3 Cu3 S2 W1 157.3(4) . . . . ? S3 Cu3 S2 W1 8.81(13) . . . . ? I1 Cu3 S2 W1 -91.92(7) . . . . ? N3 Cu3 S2 Cu1 -132.6(4) . . . . ? S3 Cu3 S2 Cu1 78.93(15) . . . . ? W1 Cu3 S2 Cu1 70.12(9) . . . . ? I1 Cu3 S2 Cu1 -21.79(10) . . . . ? O1 W1 S3 Cu3 131.1(3) . . . . ? S2 W1 S3 Cu3 9.10(13) . . . . ? S1 W1 S3 Cu3 -108.20(12) . . . . ? Cu1 W1 S3 Cu3 -49.54(11) . . . . ? Cu2 W1 S3 Cu3 -96.47(11) . . . . ? O1 W1 S3 Cu2 -132.5(3) . . . . ? S2 W1 S3 Cu2 105.56(11) . . . . ? S1 W1 S3 Cu2 -11.74(13) . . . . ? Cu1 W1 S3 Cu2 46.93(11) . . . . ? Cu3 W1 S3 Cu2 96.47(11) . . . . ? N3 Cu3 S3 W1 -158.5(4) . . . . ? S2 Cu3 S3 W1 -8.82(13) . . . . ? I1 Cu3 S3 W1 89.84(9) . . . . ? N3 Cu3 S3 Cu2 130.2(4) . . . . ? S2 Cu3 S3 Cu2 -80.17(15) . . . . ? W1 Cu3 S3 Cu2 -71.35(9) . . . . ? I1 Cu3 S3 Cu2 18.50(11) . . . . ? N2 Cu2 S3 W1 158.3(4) . . . . ? S1 Cu2 S3 W1 11.34(12) . . . . ? I1 Cu2 S3 W1 -89.75(8) . . . . ? N2 Cu2 S3 Cu3 -130.6(4) . . . . ? S1 Cu2 S3 Cu3 82.42(14) . . . . ? W1 Cu2 S3 Cu3 71.08(9) . . . . ? I1 Cu2 S3 Cu3 -18.67(11) . . . . ? S2 Cu1 N1 C11 126.8(9) . . . . ? S1 Cu1 N1 C11 -12.1(11) . . . . ? W1 Cu1 N1 C11 43.5(15) . . . . ? I1 Cu1 N1 C11 -120.2(10) . . . . ? S2 Cu1 N1 C15 -51.8(12) . . . . ? S1 Cu1 N1 C15 169.3(9) . . . . ? W1 Cu1 N1 C15 -135.1(8) . . . . ? I1 Cu1 N1 C15 61.2(11) . . . . ? S1 Cu2 N2 C25 86.1(11) . . . . ? S3 Cu2 N2 C25 -54.8(11) . . . . ? W1 Cu2 N2 C25 14.5(17) . . . . ? I1 Cu2 N2 C25 -164.6(10) . . . . ? S1 Cu2 N2 C21 -94.6(11) . . . . ? S3 Cu2 N2 C21 124.5(10) . . . . ? W1 Cu2 N2 C21 -166.1(9) . . . . ? I1 Cu2 N2 C21 14.7(11) . . . . ? S2 Cu3 N3 C35 -59.1(11) . . . . ? S3 Cu3 N3 C35 84.8(11) . . . . ? W1 Cu3 N3 C35 17.5(18) . . . . ? I1 Cu3 N3 C35 -166.1(10) . . . . ? S2 Cu3 N3 C31 124.9(10) . . . . ? S3 Cu3 N3 C31 -91.3(11) . . . . ? W1 Cu3 N3 C31 -158.6(8) . . . . ? I1 Cu3 N3 C31 17.9(11) . . . . ? C15 N1 C11 C12 -1(2) . . . . ? Cu1 N1 C11 C12 -179.9(13) . . . . ? N1 C11 C12 C13 4(3) . . . . ? C11 C12 C13 C14 -4(3) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C11 N1 C15 C14 -1(2) . . . . ? Cu1 N1 C15 C14 177.1(11) . . . . ? C11 N1 C15 C16 -177.9(12) . . . . ? Cu1 N1 C15 C16 0.7(16) . . . . ? C13 C14 C15 N1 1(2) . . . . ? C13 C14 C15 C16 177.5(13) . . . . ? C25 N2 C21 C22 2(2) . . . . ? Cu2 N2 C21 C22 -177.8(13) . . . . ? N2 C21 C22 C23 1(3) . . . . ? C21 C22 C23 C24 -3(3) . . . . ? C22 C23 C24 C25 2(3) . . . . ? C21 N2 C25 C24 -2(2) . . . . ? Cu2 N2 C25 C24 177.4(12) . . . . ? C21 N2 C25 C26 -178.3(16) . . . . ? Cu2 N2 C25 C26 1(2) . . . . ? C23 C24 C25 N2 0(3) . . . . ? C23 C24 C25 C26 176(2) . . . . ? C35 N3 C31 C32 3(2) . . . . ? Cu3 N3 C31 C32 178.8(10) . . . . ? N3 C31 C32 C33 -2(2) . . . . ? C31 C32 C33 C34 0(3) . . . . ? C32 C33 C34 C35 1(2) . . . . ? C31 N3 C35 C36 175.6(16) . . . . ? Cu3 N3 C35 C36 0(2) . . . . ? C31 N3 C35 C34 -2(2) . . . . ? Cu3 N3 C35 C34 -177.5(10) . . . . ? C33 C34 C35 N3 0(2) . . . . ? C33 C34 C35 C36 -177.5(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.706 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.141 #==============================================================END