# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1877 #============================================================================ data_cluster1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Cu4 N10 S8 W' _chemical_formula_weight 1431.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.69820(10) _cell_length_b 14.67930(10) _cell_length_c 28.3219(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6110.71(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 28.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 3.556 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2916 _exptl_absorpt_correction_T_max 0.3609 _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 26399 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3999 _reflns_number_gt 3892 _reflns_threshold_expression '> 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996a)' _computing_cell_refinement 'SAINT (Siemens, 1996b)' _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^)+(0.0251P)^2^+2.6830P] 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(6) _refine_ls_number_reflns 3999 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0524 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.570451(10) 0.570451(10) 0.0000 0.03362(8) Uani 1 2 d S . . Cu1 Cu 0.68920(4) 0.44620(4) 0.035482(18) 0.04870(15) Uani 1 1 d . . . Cu2 Cu 0.70188(3) 0.70188(3) 0.0000 0.04726(18) Uani 1 2 d S . . Cu3 Cu 0.43969(3) 0.43969(3) 0.0000 0.04763(18) Uani 1 2 d S . . S1 S 0.42802(8) 0.58722(7) 0.02680(3) 0.0441(2) Uani 1 1 d . . . S2 S 0.67071(8) 0.59592(7) 0.05805(4) 0.0453(3) Uani 1 1 d . . . S3 S 0.73537(19) 0.98258(13) 0.08042(8) 0.1200(8) Uani 1 1 d . . . S4A S 0.9544(11) 0.3014(11) -0.0232(4) 0.136(4) Uani 0.59(5) 1 d P A 1 S4B S 0.9743(17) 0.352(6) -0.0158(11) 0.204(18) Uani 0.41(5) 1 d P A 2 N1 N 0.6607(3) 0.3725(3) 0.09829(13) 0.0544(10) Uani 1 1 d . . . N2 N 0.4159(3) 0.3460(3) 0.05398(14) 0.0541(10) Uani 1 1 d . . . N3 N 0.6995(3) 0.8223(3) 0.03268(15) 0.0648(11) Uani 1 1 d . . . N4 N 0.8097(3) 0.4020(3) 0.01482(15) 0.0741(14) Uani 1 1 d . A . N5 N -0.0144(3) 0.7006(3) 0.09231(13) 0.0579(10) Uani 1 1 d . . . C1 C 0.6558(4) 0.4207(4) 0.13989(16) 0.0690(15) Uani 1 1 d . . . H1A H 0.6642 0.4834 0.1384 0.083 Uiso 1 1 calc R . . C2 C 0.6396(5) 0.3840(4) 0.1824(2) 0.0878(19) Uani 1 1 d . . . H2A H 0.6367 0.4194 0.2096 0.105 Uiso 1 1 calc R . . C3 C 0.6273(5) 0.2889(5) 0.1835(2) 0.091(2) Uani 1 1 d . . . H3A H 0.6152 0.2599 0.2120 0.109 Uiso 1 1 calc R . . C4 C 0.6331(4) 0.2400(4) 0.1436(2) 0.0792(18) Uani 1 1 d . . . H4A H 0.6258 0.1771 0.1444 0.095 Uiso 1 1 calc R . . C5 C 0.6503(3) 0.2839(4) 0.10080(19) 0.0603(13) Uani 1 1 d . . . C6 C 0.6585(5) 0.2310(4) 0.0565(2) 0.0778(17) Uani 1 1 d . . . H6A H 0.6211 0.2582 0.0326 0.117 Uiso 1 1 calc R . . H6B H 0.6389 0.1695 0.0620 0.117 Uiso 1 1 calc R . . H6C H 0.7208 0.2310 0.0463 0.117 Uiso 1 1 calc R . . C7 C 0.4077(3) 0.3786(4) 0.09837(17) 0.0673(15) Uani 1 1 d . . . H7A H 0.4124 0.4411 0.1032 0.081 Uiso 1 1 calc R . . C8 C 0.3930(4) 0.3237(5) 0.1362(2) 0.0854(18) Uani 1 1 d . . . H8A H 0.3869 0.3485 0.1662 0.103 Uiso 1 1 calc R . . C9 C 0.3874(5) 0.2338(5) 0.1298(3) 0.094(2) Uani 1 1 d . . . H9A H 0.3785 0.1955 0.1556 0.112 Uiso 1 1 calc R . . C10 C 0.3949(4) 0.1974(4) 0.0848(3) 0.0859(19) Uani 1 1 d . . . H10A H 0.3896 0.1350 0.0798 0.103 Uiso 1 1 calc R . . C11 C 0.4103(3) 0.2564(4) 0.0472(2) 0.0626(13) Uani 1 1 d . . . C12 C 0.4204(4) 0.2209(4) -0.0022(2) 0.0880(17) Uani 1 1 d . . . H12A H 0.4773 0.2412 -0.0152 0.132 Uiso 1 1 calc R . . H12B H 0.3713 0.2434 -0.0214 0.132 Uiso 1 1 calc R . . H12C H 0.4190 0.1556 -0.0018 0.132 Uiso 1 1 calc R . . C13 C 0.7143(4) 0.8884(4) 0.05261(18) 0.0626(14) Uani 1 1 d . . . C14 C 0.8732(4) 0.3680(5) 0.0004(2) 0.090(2) Uani 1 1 d . . . C15 C -0.0329(5) 0.7824(5) 0.0598(2) 0.097(2) Uani 1 1 d . . . H15A H -0.0077 0.7689 0.0289 0.116 Uiso 1 1 calc R . . H15B H -0.0982 0.7885 0.0561 0.116 Uiso 1 1 calc R . . C16 C 0.0044(7) 0.8723(5) 0.0759(3) 0.131(3) Uani 1 1 d . . . H16A H -0.0021 0.9163 0.0510 0.197 Uiso 1 1 calc R . . H16B H 0.0677 0.8657 0.0836 0.197 Uiso 1 1 calc R . . H16C H -0.0284 0.8926 0.1032 0.197 Uiso 1 1 calc R . . C17 C -0.0537(4) 0.7177(4) 0.14085(18) 0.0790(17) Uani 1 1 d . . . H17A H -0.0227 0.7693 0.1550 0.095 Uiso 1 1 calc R . . H17B H -0.0422 0.6649 0.1606 0.095 Uiso 1 1 calc R . . C18 C -0.1578(4) 0.7370(5) 0.1400(2) 0.097(2) Uani 1 1 d . . . H18A H -0.1793 0.7453 0.1717 0.145 Uiso 1 1 calc R . . H18B H -0.1889 0.6864 0.1259 0.145 Uiso 1 1 calc R . . H18C H -0.1694 0.7911 0.1220 0.145 Uiso 1 1 calc R . . C19 C 0.0856(4) 0.6884(6) 0.0994(2) 0.098(2) Uani 1 1 d . . . H19A H 0.0953 0.6387 0.1214 0.117 Uiso 1 1 calc R . . H19B H 0.1101 0.7433 0.1137 0.117 Uiso 1 1 calc R . . C20 C 0.1378(5) 0.6687(8) 0.0546(3) 0.145(4) Uani 1 1 d . . . H20A H 0.1956 0.6422 0.0623 0.217 Uiso 1 1 calc R . . H20B H 0.1471 0.7243 0.0375 0.217 Uiso 1 1 calc R . . H20C H 0.1037 0.6269 0.0354 0.217 Uiso 1 1 calc R . . C21 C -0.0580(5) 0.6189(5) 0.0689(2) 0.0906(19) Uani 1 1 d . . . H21A H -0.0303 0.6097 0.0382 0.109 Uiso 1 1 calc R . . H21B H -0.1221 0.6312 0.0640 0.109 Uiso 1 1 calc R . . C22 C -0.0481(6) 0.5312(5) 0.0981(3) 0.135(3) Uani 1 1 d . . . H22A H -0.0879 0.4852 0.0857 0.203 Uiso 1 1 calc R . . H22B H -0.0639 0.5434 0.1304 0.203 Uiso 1 1 calc R . . H22C H 0.0137 0.5102 0.0965 0.203 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 0.03541(9) 0.03541(9) 0.03006(12) 0.00217(8) -0.00217(8) -0.00360(10) Cu1 0.0503(3) 0.0507(3) 0.0450(3) 0.0025(2) -0.0042(2) 0.0073(3) Cu2 0.0481(3) 0.0481(3) 0.0455(4) 0.0044(3) -0.0044(3) -0.0115(3) Cu3 0.0478(3) 0.0478(3) 0.0473(4) -0.0007(3) 0.0007(3) -0.0125(3) S1 0.0440(6) 0.0456(6) 0.0427(5) 0.0012(5) 0.0072(5) -0.0008(5) S2 0.0561(7) 0.0416(6) 0.0380(5) 0.0051(5) -0.0119(5) -0.0080(5) S3 0.193(2) 0.0583(10) 0.1082(14) -0.0225(10) 0.0031(15) -0.0206(12) S4A 0.101(6) 0.209(9) 0.096(3) -0.014(5) 0.005(4) 0.092(5) S4B 0.068(7) 0.42(4) 0.124(11) 0.082(17) 0.042(6) 0.105(16) N1 0.060(3) 0.050(3) 0.053(2) 0.0090(18) -0.0007(18) 0.0077(19) N2 0.047(2) 0.058(3) 0.058(2) 0.0136(19) -0.0007(19) -0.0109(19) N3 0.089(3) 0.049(3) 0.056(2) 0.003(2) -0.002(2) -0.010(2) N4 0.061(3) 0.102(4) 0.060(3) 0.009(2) -0.002(2) 0.018(3) N5 0.056(3) 0.071(3) 0.047(2) -0.007(2) -0.0124(18) -0.005(2) C1 0.106(4) 0.052(3) 0.049(3) 0.008(3) 0.006(3) 0.006(3) C2 0.125(6) 0.081(4) 0.057(3) 0.013(3) 0.005(3) 0.011(4) C3 0.114(5) 0.084(5) 0.075(4) 0.030(4) 0.018(4) 0.001(4) C4 0.097(5) 0.057(3) 0.084(4) 0.028(3) -0.001(4) -0.003(3) C5 0.058(3) 0.050(3) 0.073(3) 0.006(3) -0.008(3) 0.007(2) C6 0.101(5) 0.052(3) 0.080(4) -0.005(3) -0.016(3) 0.006(3) C7 0.069(4) 0.078(4) 0.055(3) 0.010(3) 0.009(2) -0.005(3) C8 0.089(5) 0.103(5) 0.065(4) 0.009(4) 0.013(3) 0.009(4) C9 0.088(5) 0.094(5) 0.099(5) 0.051(4) 0.021(4) 0.009(4) C10 0.078(4) 0.070(4) 0.109(5) 0.033(4) 0.004(4) -0.002(3) C11 0.052(3) 0.056(3) 0.080(4) 0.013(3) -0.005(3) -0.007(2) C12 0.107(5) 0.064(3) 0.094(4) -0.007(3) -0.018(5) -0.008(3) C13 0.087(4) 0.045(3) 0.056(3) 0.009(3) 0.002(3) -0.002(3) C14 0.059(3) 0.156(6) 0.054(3) 0.029(4) 0.000(3) 0.034(4) C15 0.113(6) 0.110(5) 0.068(4) 0.012(4) -0.016(4) -0.007(4) C16 0.162(8) 0.090(5) 0.142(8) 0.015(5) -0.015(6) -0.024(6) C17 0.092(5) 0.090(4) 0.054(3) -0.014(3) -0.005(3) -0.003(4) C18 0.074(4) 0.127(6) 0.090(5) -0.017(4) 0.009(4) 0.012(4) C19 0.069(4) 0.133(6) 0.091(4) -0.033(4) -0.020(3) -0.001(4) C20 0.082(5) 0.249(12) 0.104(6) -0.047(7) 0.013(4) 0.019(6) C21 0.090(5) 0.105(5) 0.077(4) -0.031(4) -0.019(4) -0.017(4) C22 0.180(9) 0.077(5) 0.150(8) -0.014(5) -0.031(7) -0.025(5) _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 S1 2.2379(11) 7 ? W1 S2 2.2380(11) 7 ? W1 S2 2.2392(11) . ? W1 S1 2.2404(11) . ? W1 Cu3 2.7163(7) . ? W1 Cu1 2.7172(5) . ? W1 Cu1 2.7173(5) 7 ? W1 Cu2 2.7302(7) . ? Cu1 N4 1.975(5) . ? Cu1 N1 2.124(4) . ? Cu1 S2 2.3049(12) . ? Cu1 S1 2.3301(11) 7 ? Cu2 N3 1.996(4) . ? Cu2 N3 1.998(4) 7 ? Cu2 S2 2.3091(11) . ? Cu2 S2 2.3104(11) 7 ? Cu3 N2 2.086(4) . ? Cu3 N2 2.087(4) 7 ? Cu3 S1 2.3011(11) . ? Cu3 S1 2.3037(11) 7 ? S1 Cu1 2.3289(11) 7 ? S3 C13 1.621(6) . ? S4A C14 1.681(10) . ? S4B C14 1.572(13) . ? N1 C5 1.311(6) . ? N1 C1 1.377(6) . ? N2 C11 1.332(6) . ? N2 C7 1.350(6) . ? N3 C13 1.143(6) . ? N4 C14 1.134(7) . ? N5 C19 1.496(7) . ? N5 C17 1.512(6) . ? N5 C21 1.513(7) . ? N5 C15 1.537(7) . ? C1 C2 1.339(7) . ? C2 C3 1.408(9) . ? C3 C4 1.344(9) . ? C4 C5 1.395(7) . ? C5 C6 1.480(7) . ? C7 C8 1.357(8) . ? C8 C9 1.335(9) . ? C9 C10 1.387(10) . ? C10 C11 1.391(8) . ? C11 C12 1.500(8) . ? C15 C16 1.501(10) . ? C17 C18 1.556(8) . ? C19 C20 1.513(9) . ? C21 C22 1.537(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 W1 S2 110.29(4) 7 7 ? S1 W1 S2 109.42(4) 7 . ? S2 W1 S2 108.63(6) 7 . ? S1 W1 S1 108.69(5) 7 . ? S2 W1 S1 109.45(4) 7 . ? S2 W1 S1 110.36(4) . . ? S1 W1 Cu3 54.39(3) 7 . ? S2 W1 Cu3 125.66(3) 7 . ? S2 W1 Cu3 125.71(3) . . ? S1 W1 Cu3 54.30(3) . . ? S1 W1 Cu1 55.08(3) 7 . ? S2 W1 Cu1 127.28(3) 7 . ? S2 W1 Cu1 54.40(3) . . ? S1 W1 Cu1 123.28(3) . . ? Cu3 W1 Cu1 88.863(12) . . ? S1 W1 Cu1 123.22(3) 7 7 ? S2 W1 Cu1 54.47(3) 7 7 ? S2 W1 Cu1 127.35(3) . 7 ? S1 W1 Cu1 55.02(3) . 7 ? Cu3 W1 Cu1 88.726(12) . 7 ? Cu1 W1 Cu1 177.59(2) . 7 ? S1 W1 Cu2 125.61(3) 7 . ? S2 W1 Cu2 54.34(3) 7 . ? S2 W1 Cu2 54.29(3) . . ? S1 W1 Cu2 125.70(3) . . ? Cu3 W1 Cu2 180.000(9) . . ? Cu1 W1 Cu2 91.137(12) . . ? Cu1 W1 Cu2 91.274(12) 7 . ? N4 Cu1 N1 104.93(16) . . ? N4 Cu1 S2 120.07(15) . . ? N1 Cu1 S2 103.32(11) . . ? N4 Cu1 S1 108.37(13) . 7 ? N1 Cu1 S1 116.67(11) . 7 ? S2 Cu1 S1 104.08(4) . 7 ? N4 Cu1 W1 133.39(13) . . ? N1 Cu1 W1 121.68(11) . . ? S2 Cu1 W1 52.17(3) . . ? S1 Cu1 W1 51.95(3) 7 . ? N3 Cu2 N3 104.2(3) . 7 ? N3 Cu2 S2 105.26(12) . . ? N3 Cu2 S2 119.60(13) 7 . ? N3 Cu2 S2 119.58(13) . 7 ? N3 Cu2 S2 105.33(12) 7 7 ? S2 Cu2 S2 103.85(6) . 7 ? N3 Cu2 W1 127.86(13) . . ? N3 Cu2 W1 127.93(13) 7 . ? S2 Cu2 W1 51.95(3) . . ? S2 Cu2 W1 51.91(3) 7 . ? N2 Cu3 N2 108.4(2) . 7 ? N2 Cu3 S1 111.48(12) . . ? N2 Cu3 S1 110.49(11) 7 . ? N2 Cu3 S1 110.51(11) . 7 ? N2 Cu3 S1 111.54(12) 7 7 ? S1 Cu3 S1 104.41(6) . 7 ? N2 Cu3 W1 125.78(11) . . ? N2 Cu3 W1 125.82(11) 7 . ? S1 Cu3 W1 52.25(3) . . ? S1 Cu3 W1 52.16(3) 7 . ? W1 S1 Cu3 73.45(3) . . ? W1 S1 Cu1 72.95(3) . 7 ? Cu3 S1 Cu1 110.28(4) . 7 ? W1 S2 Cu1 73.43(3) . . ? W1 S2 Cu2 73.76(3) . . ? Cu1 S2 Cu2 114.93(5) . . ? C5 N1 C1 117.2(4) . . ? C5 N1 Cu1 125.0(3) . . ? C1 N1 Cu1 117.7(3) . . ? C11 N2 C7 118.6(4) . . ? C11 N2 Cu3 123.7(4) . . ? C7 N2 Cu3 117.6(3) . . ? C13 N3 Cu2 167.8(5) . . ? C14 N4 Cu1 171.4(6) . . ? C19 N5 C17 105.8(4) . . ? C19 N5 C21 112.4(5) . . ? C17 N5 C21 111.6(4) . . ? C19 N5 C15 110.4(5) . . ? C17 N5 C15 110.3(5) . . ? C21 N5 C15 106.4(4) . . ? C2 C1 N1 124.9(5) . . ? C1 C2 C3 116.2(6) . . ? C4 C3 C2 120.2(6) . . ? C3 C4 C5 119.7(6) . . ? N1 C5 C4 121.8(5) . . ? N1 C5 C6 117.7(5) . . ? C4 C5 C6 120.5(5) . . ? N2 C7 C8 122.6(6) . . ? C9 C8 C7 119.4(6) . . ? C8 C9 C10 120.0(6) . . ? C9 C10 C11 118.6(6) . . ? N2 C11 C10 120.9(6) . . ? N2 C11 C12 118.1(5) . . ? C10 C11 C12 121.0(5) . . ? N3 C13 S3 179.5(5) . . ? N4 C14 S4B 161(3) . . ? N4 C14 S4A 169.5(10) . . ? S4B C14 S4A 29(3) . . ? C16 C15 N5 116.2(5) . . ? N5 C17 C18 113.1(4) . . ? N5 C19 C20 114.1(5) . . ? N5 C21 C22 112.8(5) . . ? _diffrn_measured_fraction_theta_max 1.002 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.562 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.068 #============================================================================ # END OF CIF #============================================================================ data_cluster2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Cu4 Mo N10 S8' _chemical_formula_weight 1343.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.6884(3) _cell_length_b 14.6881(2) _cell_length_c 28.3778(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6122.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8824 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5679 _exptl_absorpt_correction_T_max 0.6830 _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 26338 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4000 _reflns_number_gt 3122 _reflns_threshold_expression '> 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996a)' _computing_cell_refinement 'SAINT (Siemens, 1996b)' _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^)+(0.0380P)^2^+3.5379P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4000 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Mo1 Mo 0.57047(4) 0.57047(4) 0.0000 0.0341(2) Uani 1 2 d S . . Cu1 Cu 0.68871(7) 0.44694(6) 0.03507(3) 0.0495(3) Uani 1 1 d . . . Cu2 Cu 0.70100(6) 0.70100(6) 0.0000 0.0478(3) Uani 1 2 d S . . Cu3 Cu 0.44041(5) 0.44041(5) 0.0000 0.0479(3) Uani 1 2 d S . . S1 S 0.42762(13) 0.58712(12) 0.02649(6) 0.0446(5) Uani 1 1 d . . . S2 S 0.67109(14) 0.59564(13) 0.05771(7) 0.0466(5) Uani 1 1 d . . . S3 S 0.7347(3) 0.9816(2) 0.08002(12) 0.1227(13) Uani 1 1 d . . . S4A S 0.9549(14) 0.3026(13) -0.0231(5) 0.129(6) Uani 0.60(8) 1 d P A 1 S4B S 0.975(3) 0.357(10) -0.0133(19) 0.23(3) Uani 0.40(8) 1 d P A 2 N1 N 0.6603(5) 0.3731(5) 0.0981(2) 0.0589(19) Uani 1 1 d . . . N2 N 0.4165(4) 0.3469(5) 0.0539(3) 0.0561(18) Uani 1 1 d . . . N3 N 0.6990(5) 0.8216(5) 0.0327(2) 0.065(2) Uani 1 1 d . . . N4 N 0.8095(5) 0.4034(5) 0.0151(2) 0.069(2) Uani 1 1 d . A . N5 N -0.0157(4) 0.7004(5) 0.0930(2) 0.0572(18) Uani 1 1 d . . . C1 C 0.6552(6) 0.4210(6) 0.1392(3) 0.070(3) Uani 1 1 d . . . H1A H 0.6630 0.4838 0.1378 0.084 Uiso 1 1 calc R . . C2 C 0.6399(7) 0.3836(7) 0.1813(3) 0.086(3) Uani 1 1 d . . . H2A H 0.6383 0.4193 0.2084 0.103 Uiso 1 1 calc R . . C3 C 0.6261(8) 0.2893(8) 0.1837(4) 0.102(4) Uani 1 1 d . . . H3A H 0.6125 0.2612 0.2122 0.122 Uiso 1 1 calc R . . C4 C 0.6331(7) 0.2393(7) 0.1431(4) 0.075(3) Uani 1 1 d . . . H4A H 0.6257 0.1764 0.1436 0.090 Uiso 1 1 calc R . . C5 C 0.6516(6) 0.2848(6) 0.1004(3) 0.062(3) Uani 1 1 d . . . C6 C 0.6590(6) 0.2314(6) 0.0564(3) 0.076(3) Uani 1 1 d . . . H6A H 0.6717 0.2716 0.0305 0.114 Uiso 1 1 calc R . . H6B H 0.6027 0.2000 0.0507 0.114 Uiso 1 1 calc R . . H6C H 0.7074 0.1878 0.0594 0.114 Uiso 1 1 calc R . . C7 C 0.4081(6) 0.3797(7) 0.0985(3) 0.066(3) Uani 1 1 d . . . H7A H 0.4127 0.4421 0.1036 0.079 Uiso 1 1 calc R . . C8 C 0.3930(7) 0.3236(9) 0.1361(4) 0.089(3) Uani 1 1 d . . . H8A H 0.3869 0.3474 0.1663 0.107 Uiso 1 1 calc R . . C9 C 0.3872(7) 0.2340(9) 0.1288(5) 0.097(4) Uani 1 1 d . . . H9A H 0.3767 0.1960 0.1545 0.116 Uiso 1 1 calc R . . C10 C 0.3961(7) 0.1952(8) 0.0843(4) 0.090(3) Uani 1 1 d . . . H10A H 0.3928 0.1327 0.0794 0.108 Uiso 1 1 calc R . . C11 C 0.4107(6) 0.2569(6) 0.0470(3) 0.060(2) Uani 1 1 d . . . C12 C 0.4210(7) 0.2217(6) -0.0019(4) 0.090(3) Uani 1 1 d . . . H12A H 0.4304 0.2718 -0.0231 0.134 Uiso 1 1 calc R . . H12B H 0.3670 0.1893 -0.0109 0.134 Uiso 1 1 calc R . . H12C H 0.4724 0.1814 -0.0034 0.134 Uiso 1 1 calc R . . C13 C 0.7138(6) 0.8887(6) 0.0525(3) 0.061(2) Uani 1 1 d . . . C14 C 0.8722(7) 0.3691(8) 0.0003(4) 0.091(4) Uani 1 1 d . . . C15 C -0.0320(9) 0.7823(8) 0.0604(4) 0.111(4) Uani 1 1 d . . . H15A H -0.0062 0.7682 0.0298 0.133 Uiso 1 1 calc R . . H15B H -0.0971 0.7893 0.0562 0.133 Uiso 1 1 calc R . . C16 C 0.0056(10) 0.8712(8) 0.0760(5) 0.147(6) Uani 1 1 d . . . H16A H -0.0086 0.9170 0.0530 0.220 Uiso 1 1 calc R . . H16B H 0.0705 0.8664 0.0793 0.220 Uiso 1 1 calc R . . H16C H -0.0208 0.8876 0.1058 0.220 Uiso 1 1 calc R . . C17 C -0.0527(7) 0.7168(7) 0.1409(3) 0.084(3) Uani 1 1 d . . . H17A H -0.0218 0.7686 0.1548 0.101 Uiso 1 1 calc R . . H17B H -0.0404 0.6640 0.1605 0.101 Uiso 1 1 calc R . . C18 C -0.1569(7) 0.7352(8) 0.1403(3) 0.099(4) Uani 1 1 d . . . H18A H -0.1779 0.7454 0.1719 0.149 Uiso 1 1 calc R . . H18B H -0.1879 0.6836 0.1272 0.149 Uiso 1 1 calc R . . H18C H -0.1692 0.7881 0.1215 0.149 Uiso 1 1 calc R . . C19 C 0.0851(6) 0.6878(8) 0.0996(4) 0.104(4) Uani 1 1 d . . . H19A H 0.1099 0.7423 0.1139 0.125 Uiso 1 1 calc R . . H19B H 0.0950 0.6378 0.1213 0.125 Uiso 1 1 calc R . . C20 C 0.1363(7) 0.6687(10) 0.0550(4) 0.141(6) Uani 1 1 d . . . H20A H 0.1998 0.6615 0.0620 0.212 Uiso 1 1 calc R . . H20B H 0.1284 0.7185 0.0335 0.212 Uiso 1 1 calc R . . H20C H 0.1134 0.6138 0.0409 0.212 Uiso 1 1 calc R . . C21 C -0.0561(8) 0.6189(7) 0.0691(4) 0.094(4) Uani 1 1 d . . . H21A H -0.0259 0.6099 0.0391 0.113 Uiso 1 1 calc R . . H21B H -0.1200 0.6306 0.0628 0.113 Uiso 1 1 calc R . . C22 C -0.0476(9) 0.5304(8) 0.0988(4) 0.138(5) Uani 1 1 d . . . H22A H -0.0745 0.4806 0.0820 0.208 Uiso 1 1 calc R . . H22B H -0.0786 0.5384 0.1283 0.208 Uiso 1 1 calc R . . H22C H 0.0155 0.5177 0.1046 0.208 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 Mo1 0.0353(3) 0.0353(3) 0.0318(5) 0.0027(3) -0.0027(3) -0.0035(4) Cu1 0.0514(6) 0.0500(6) 0.0472(5) 0.0033(5) -0.0049(5) 0.0069(5) Cu2 0.0479(5) 0.0479(5) 0.0477(8) 0.0043(6) -0.0043(6) -0.0121(7) Cu3 0.0472(5) 0.0472(5) 0.0492(8) -0.0002(6) 0.0002(6) -0.0136(7) S1 0.0444(12) 0.0445(12) 0.0450(10) 0.0016(9) 0.0062(10) -0.0011(10) S2 0.0560(14) 0.0426(12) 0.0412(11) 0.0044(10) -0.0114(11) -0.0073(10) S3 0.200(4) 0.0570(18) 0.111(2) -0.0228(18) 0.003(3) -0.023(2) S4A 0.096(8) 0.197(17) 0.093(6) -0.010(7) 0.000(6) 0.089(6) S4B 0.068(12) 0.49(9) 0.126(18) 0.07(3) 0.046(12) 0.11(3) N1 0.064(5) 0.056(5) 0.056(5) 0.009(4) -0.007(4) 0.017(4) N2 0.042(4) 0.064(5) 0.063(5) 0.009(4) -0.003(4) -0.012(4) N3 0.086(6) 0.048(5) 0.062(5) 0.013(4) -0.001(4) -0.010(4) N4 0.054(5) 0.092(6) 0.062(5) 0.004(4) -0.003(4) 0.021(5) N5 0.059(5) 0.071(5) 0.041(4) -0.006(4) -0.014(3) -0.003(4) C1 0.103(8) 0.059(6) 0.048(6) 0.008(5) 0.013(5) 0.008(5) C2 0.123(9) 0.076(8) 0.058(6) 0.007(6) 0.004(6) 0.005(6) C3 0.117(9) 0.101(10) 0.087(9) 0.045(8) 0.022(7) 0.000(8) C4 0.096(8) 0.060(7) 0.070(7) 0.011(6) -0.002(6) 0.003(6) C5 0.054(6) 0.060(7) 0.071(7) 0.012(6) -0.004(5) 0.010(5) C6 0.085(7) 0.059(6) 0.083(7) -0.009(5) -0.020(6) 0.011(5) C7 0.063(6) 0.084(7) 0.049(6) 0.013(5) 0.012(5) 0.005(5) C8 0.089(8) 0.112(10) 0.066(7) -0.005(7) 0.009(6) -0.001(7) C9 0.087(8) 0.089(10) 0.115(10) 0.061(8) 0.028(8) 0.007(7) C10 0.087(8) 0.078(7) 0.104(9) 0.045(8) 0.006(7) 0.004(6) C11 0.045(6) 0.055(6) 0.079(7) 0.005(6) -0.007(5) -0.002(4) C12 0.115(8) 0.057(6) 0.096(8) -0.005(6) -0.022(8) -0.010(6) C13 0.080(7) 0.046(5) 0.056(6) 0.013(5) -0.001(5) -0.002(5) C14 0.061(6) 0.150(10) 0.064(6) 0.041(7) 0.003(6) 0.036(7) C15 0.135(11) 0.127(10) 0.070(7) 0.013(8) -0.012(7) -0.007(9) C16 0.177(14) 0.105(10) 0.158(14) -0.018(10) 0.002(11) -0.028(10) C17 0.096(8) 0.092(8) 0.064(7) -0.016(6) 0.002(6) -0.015(7) C18 0.078(8) 0.139(11) 0.082(8) -0.019(7) 0.012(6) 0.016(7) C19 0.066(7) 0.137(10) 0.108(9) -0.032(8) -0.024(7) 0.008(7) C20 0.073(8) 0.249(18) 0.102(10) -0.049(11) 0.026(7) 0.009(9) C21 0.090(8) 0.110(9) 0.082(8) -0.033(7) -0.022(7) -0.024(7) C22 0.197(16) 0.081(8) 0.138(13) -0.021(9) -0.013(11) -0.015(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S2 2.237(2) 7 ? Mo1 S2 2.237(2) . ? Mo1 S1 2.242(2) 7 ? Mo1 S1 2.242(2) . ? Mo1 Cu3 2.7016(14) . ? Mo1 Cu1 2.7017(9) . ? Mo1 Cu1 2.7017(9) 7 ? Mo1 Cu2 2.7114(14) . ? Cu1 N4 1.969(8) . ? Cu1 N1 2.133(7) . ? Cu1 S2 2.291(2) . ? Cu1 S1 2.315(2) 7 ? Cu2 N3 2.000(8) . ? Cu2 N3 2.000(8) 7 ? Cu2 S2 2.295(2) . ? Cu2 S2 2.296(2) 7 ? Cu3 N2 2.086(7) . ? Cu3 N2 2.086(7) 7 ? Cu3 S1 2.2900(19) . ? Cu3 S1 2.2900(19) 7 ? S1 Cu1 2.315(2) 7 ? S3 C13 1.602(10) . ? S4A C14 1.696(16) . ? S4B C14 1.58(2) . ? N1 C5 1.305(10) . ? N1 C1 1.363(10) . ? N2 C11 1.340(10) . ? N2 C7 1.361(10) . ? N3 C13 1.155(9) . ? N4 C14 1.130(11) . ? N5 C17 1.484(10) . ? N5 C21 1.499(10) . ? N5 C19 1.504(11) . ? N5 C15 1.536(11) . ? C1 C2 1.336(11) . ? C2 C3 1.402(13) . ? C3 C4 1.371(14) . ? C4 C5 1.409(11) . ? C5 C6 1.480(11) . ? C7 C8 1.365(12) . ? C8 C9 1.335(14) . ? C9 C10 1.393(15) . ? C10 C11 1.409(12) . ? C11 C12 1.489(12) . ? C15 C16 1.484(14) . ? C17 C18 1.555(13) . ? C19 C20 1.499(13) . ? C21 C22 1.555(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Mo1 S2 108.52(10) 7 . ? S2 Mo1 S1 110.78(7) 7 7 ? S2 Mo1 S1 109.15(7) . 7 ? S2 Mo1 S1 109.15(7) 7 . ? S2 Mo1 S1 110.78(7) . . ? S1 Mo1 S1 108.46(10) 7 . ? S2 Mo1 Cu3 125.74(5) 7 . ? S2 Mo1 Cu3 125.74(5) . . ? S1 Mo1 Cu3 54.23(5) 7 . ? S1 Mo1 Cu3 54.23(5) . . ? S2 Mo1 Cu1 127.39(6) 7 . ? S2 Mo1 Cu1 54.31(5) . . ? S1 Mo1 Cu1 54.89(5) 7 . ? S1 Mo1 Cu1 123.46(5) . . ? Cu3 Mo1 Cu1 88.84(3) . . ? S2 Mo1 Cu1 54.31(5) 7 7 ? S2 Mo1 Cu1 127.39(6) . 7 ? S1 Mo1 Cu1 123.46(5) 7 7 ? S1 Mo1 Cu1 54.89(5) . 7 ? Cu3 Mo1 Cu1 88.83(3) . 7 ? Cu1 Mo1 Cu1 177.67(6) . 7 ? S2 Mo1 Cu2 54.26(5) 7 . ? S2 Mo1 Cu2 54.26(5) . . ? S1 Mo1 Cu2 125.77(5) 7 . ? S1 Mo1 Cu2 125.77(5) . . ? Cu3 Mo1 Cu2 180.0 . . ? Cu1 Mo1 Cu2 91.16(3) . . ? Cu1 Mo1 Cu2 91.17(3) 7 . ? N4 Cu1 N1 104.6(3) . . ? N4 Cu1 S2 119.5(2) . . ? N1 Cu1 S2 103.1(2) . . ? N4 Cu1 S1 108.9(2) . 7 ? N1 Cu1 S1 116.4(2) . 7 ? S2 Cu1 S1 104.81(8) . 7 ? N4 Cu1 Mo1 133.8(2) . . ? N1 Cu1 Mo1 121.62(18) . . ? S2 Cu1 Mo1 52.44(5) . . ? S1 Cu1 Mo1 52.41(5) 7 . ? N3 Cu2 N3 103.9(4) . 7 ? N3 Cu2 S2 105.28(19) . . ? N3 Cu2 S2 119.4(2) 7 . ? N3 Cu2 S2 119.4(2) . 7 ? N3 Cu2 S2 105.28(19) 7 7 ? S2 Cu2 S2 104.53(11) . 7 ? N3 Cu2 Mo1 128.0(2) . . ? N3 Cu2 Mo1 128.0(2) 7 . ? S2 Cu2 Mo1 52.27(5) . . ? S2 Cu2 Mo1 52.26(5) 7 . ? N2 Cu3 N2 108.4(4) . 7 ? N2 Cu3 S1 111.4(2) . . ? N2 Cu3 S1 110.20(18) 7 . ? N2 Cu3 S1 110.20(18) . 7 ? N2 Cu3 S1 111.4(2) 7 7 ? S1 Cu3 S1 105.20(11) . 7 ? N2 Cu3 Mo1 125.78(19) . . ? N2 Cu3 Mo1 125.78(19) 7 . ? S1 Cu3 Mo1 52.60(5) . . ? S1 Cu3 Mo1 52.60(5) 7 . ? Mo1 S1 Cu3 73.17(6) . . ? Mo1 S1 Cu1 72.70(6) . 7 ? Cu3 S1 Cu1 110.41(8) . 7 ? Mo1 S2 Cu1 73.25(6) . . ? Mo1 S2 Cu2 73.48(6) . . ? Cu1 S2 Cu2 114.90(9) . . ? C5 N1 C1 117.7(8) . . ? C5 N1 Cu1 124.5(6) . . ? C1 N1 Cu1 117.7(6) . . ? C11 N2 C7 118.7(8) . . ? C11 N2 Cu3 123.6(6) . . ? C7 N2 Cu3 117.7(6) . . ? C13 N3 Cu2 168.1(8) . . ? C14 N4 Cu1 170.3(9) . . ? C17 N5 C21 113.5(7) . . ? C17 N5 C19 105.4(7) . . ? C21 N5 C19 110.4(8) . . ? C17 N5 C15 111.6(8) . . ? C21 N5 C15 107.0(7) . . ? C19 N5 C15 109.0(8) . . ? C2 C1 N1 124.2(9) . . ? C1 C2 C3 118.3(10) . . ? C4 C3 C2 118.6(10) . . ? C3 C4 C5 118.9(9) . . ? N1 C5 C4 122.3(9) . . ? N1 C5 C6 118.5(9) . . ? C4 C5 C6 119.2(9) . . ? N2 C7 C8 121.9(9) . . ? C9 C8 C7 119.0(10) . . ? C8 C9 C10 122.5(11) . . ? C9 C10 C11 115.7(10) . . ? N2 C11 C10 122.2(9) . . ? N2 C11 C12 118.2(8) . . ? C10 C11 C12 119.5(9) . . ? N3 C13 S3 179.8(11) . . ? N4 C14 S4B 158(6) . . ? N4 C14 S4A 170.5(15) . . ? S4B C14 S4A 31(5) . . ? C16 C15 N5 116.8(9) . . ? N5 C17 C18 112.3(7) . . ? C20 C19 N5 114.3(8) . . ? N5 C21 C22 112.9(8) . . ? 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 S2 Mo1 Cu1 N4 -10.3(3) 7 . . . ? S2 Mo1 Cu1 N4 -97.1(3) . . . . ? S1 Mo1 Cu1 N4 80.2(3) 7 . . . ? S1 Mo1 Cu1 N4 170.1(3) . . . . ? Cu3 Mo1 Cu1 N4 125.7(3) . . . . ? Cu1 Mo1 Cu1 N4 125.7(3) 7 . . . ? Cu2 Mo1 Cu1 N4 -54.3(3) . . . . ? S2 Mo1 Cu1 N1 168.9(2) 7 . . . ? S2 Mo1 Cu1 N1 82.1(2) . . . . ? S1 Mo1 Cu1 N1 -100.6(2) 7 . . . ? S1 Mo1 Cu1 N1 -10.7(2) . . . . ? Cu3 Mo1 Cu1 N1 -55.1(2) . . . . ? Cu1 Mo1 Cu1 N1 -55.1(2) 7 . . . ? Cu2 Mo1 Cu1 N1 124.9(2) . . . . ? S2 Mo1 Cu1 S2 86.74(14) 7 . . . ? S1 Mo1 Cu1 S2 177.23(9) 7 . . . ? S1 Mo1 Cu1 S2 -92.81(9) . . . . ? Cu3 Mo1 Cu1 S2 -137.22(7) . . . . ? Cu1 Mo1 Cu1 S2 -137.22(7) 7 . . . ? Cu2 Mo1 Cu1 S2 42.78(7) . . . . ? S2 Mo1 Cu1 S1 -90.50(9) 7 . . 7 ? S2 Mo1 Cu1 S1 -177.23(9) . . . 7 ? S1 Mo1 Cu1 S1 89.96(12) . . . 7 ? Cu3 Mo1 Cu1 S1 45.54(6) . . . 7 ? Cu1 Mo1 Cu1 S1 45.54(6) 7 . . 7 ? Cu2 Mo1 Cu1 S1 -134.46(6) . . . 7 ? S2 Mo1 Cu2 N3 100.5(3) 7 . . . ? S2 Mo1 Cu2 N3 -79.5(3) . . . . ? S1 Mo1 Cu2 N3 -168.3(2) 7 . . . ? S1 Mo1 Cu2 N3 11.7(2) . . . . ? Cu3 Mo1 Cu2 N3 -143.9(2) . . . . ? Cu1 Mo1 Cu2 N3 -122.3(2) . . . . ? Cu1 Mo1 Cu2 N3 57.7(2) 7 . . . ? S2 Mo1 Cu2 N3 -79.5(3) 7 . . 7 ? S2 Mo1 Cu2 N3 100.5(3) . . . 7 ? S1 Mo1 Cu2 N3 11.7(2) 7 . . 7 ? S1 Mo1 Cu2 N3 -168.3(2) . . . 7 ? Cu3 Mo1 Cu2 N3 36.1(2) . . . 7 ? Cu1 Mo1 Cu2 N3 57.7(2) . . . 7 ? Cu1 Mo1 Cu2 N3 -122.3(2) 7 . . 7 ? S2 Mo1 Cu2 S2 180.0 7 . . . ? S1 Mo1 Cu2 S2 -88.84(9) 7 . . . ? S1 Mo1 Cu2 S2 91.16(9) . . . . ? Cu3 Mo1 Cu2 S2 -64.43(6) . . . . ? Cu1 Mo1 Cu2 S2 -42.81(7) . . . . ? Cu1 Mo1 Cu2 S2 137.19(7) 7 . . . ? S2 Mo1 Cu2 S2 180.0 . . . 7 ? S1 Mo1 Cu2 S2 91.16(9) 7 . . 7 ? S1 Mo1 Cu2 S2 -88.84(9) . . . 7 ? Cu3 Mo1 Cu2 S2 115.57(6) . . . 7 ? Cu1 Mo1 Cu2 S2 137.19(7) . . . 7 ? Cu1 Mo1 Cu2 S2 -42.81(7) 7 . . 7 ? S2 Mo1 Cu3 N2 -179.7(3) 7 . . . ? S2 Mo1 Cu3 N2 0.3(3) . . . . ? S1 Mo1 Cu3 N2 89.1(2) 7 . . . ? S1 Mo1 Cu3 N2 -90.9(2) . . . . ? Cu1 Mo1 Cu3 N2 43.1(2) . . . . ? Cu1 Mo1 Cu3 N2 -136.9(2) 7 . . . ? Cu2 Mo1 Cu3 N2 64.7(2) . . . . ? S2 Mo1 Cu3 N2 0.3(3) 7 . . 7 ? S2 Mo1 Cu3 N2 -179.7(3) . . . 7 ? S1 Mo1 Cu3 N2 -90.9(2) 7 . . 7 ? S1 Mo1 Cu3 N2 89.1(2) . . . 7 ? Cu1 Mo1 Cu3 N2 -136.9(2) . . . 7 ? Cu1 Mo1 Cu3 N2 43.1(2) 7 . . 7 ? Cu2 Mo1 Cu3 N2 -115.3(2) . . . 7 ? S2 Mo1 Cu3 S1 -88.84(9) 7 . . . ? S2 Mo1 Cu3 S1 91.16(9) . . . . ? S1 Mo1 Cu3 S1 180.0 7 . . . ? Cu1 Mo1 Cu3 S1 133.97(6) . . . . ? Cu1 Mo1 Cu3 S1 -46.03(6) 7 . . . ? Cu2 Mo1 Cu3 S1 155.59(6) . . . . ? S2 Mo1 Cu3 S1 91.16(9) 7 . . 7 ? S2 Mo1 Cu3 S1 -88.84(9) . . . 7 ? S1 Mo1 Cu3 S1 180.0 . . . 7 ? Cu1 Mo1 Cu3 S1 -46.03(6) . . . 7 ? Cu1 Mo1 Cu3 S1 133.97(6) 7 . . 7 ? Cu2 Mo1 Cu3 S1 -24.41(6) . . . 7 ? S2 Mo1 S1 Cu3 120.79(7) 7 . . . ? S2 Mo1 S1 Cu3 -119.78(6) . . . . ? S1 Mo1 S1 Cu3 0.0 7 . . . ? Cu1 Mo1 S1 Cu3 -59.59(7) . . . . ? Cu1 Mo1 S1 Cu3 118.41(6) 7 . . . ? Cu2 Mo1 S1 Cu3 180.0 . . . . ? S2 Mo1 S1 Cu1 2.38(8) 7 . . 7 ? S2 Mo1 S1 Cu1 121.81(7) . . . 7 ? S1 Mo1 S1 Cu1 -118.41(6) 7 . . 7 ? Cu3 Mo1 S1 Cu1 -118.41(6) . . . 7 ? Cu1 Mo1 S1 Cu1 -178.01(5) . . . 7 ? Cu2 Mo1 S1 Cu1 61.59(6) . . . 7 ? N2 Cu3 S1 Mo1 119.39(19) . . . . ? N2 Cu3 S1 Mo1 -120.2(2) 7 . . . ? S1 Cu3 S1 Mo1 0.0 7 . . . ? N2 Cu3 S1 Cu1 -176.97(19) . . . 7 ? N2 Cu3 S1 Cu1 -56.6(2) 7 . . 7 ? S1 Cu3 S1 Cu1 63.64(7) 7 . . 7 ? Mo1 Cu3 S1 Cu1 63.64(7) . . . 7 ? S2 Mo1 S2 Cu1 -123.22(7) 7 . . . ? S1 Mo1 S2 Cu1 -2.39(8) 7 . . . ? S1 Mo1 S2 Cu1 116.96(7) . . . . ? Cu3 Mo1 S2 Cu1 56.78(7) . . . . ? Cu1 Mo1 S2 Cu1 178.01(5) 7 . . . ? Cu2 Mo1 S2 Cu1 -123.22(7) . . . . ? S2 Mo1 S2 Cu2 0.0 7 . . . ? S1 Mo1 S2 Cu2 120.83(6) 7 . . . ? S1 Mo1 S2 Cu2 -119.81(6) . . . . ? Cu3 Mo1 S2 Cu2 180.0 . . . . ? Cu1 Mo1 S2 Cu2 123.22(7) . . . . ? Cu1 Mo1 S2 Cu2 -58.77(8) 7 . . . ? N4 Cu1 S2 Mo1 124.6(2) . . . . ? N1 Cu1 S2 Mo1 -119.98(19) . . . . ? S1 Cu1 S2 Mo1 2.27(7) 7 . . . ? N4 Cu1 S2 Cu2 62.4(2) . . . . ? N1 Cu1 S2 Cu2 177.9(2) . . . . ? S1 Cu1 S2 Cu2 -59.89(11) 7 . . . ? Mo1 Cu1 S2 Cu2 -62.15(7) . . . . ? N3 Cu2 S2 Mo1 126.6(2) . . . . ? N3 Cu2 S2 Mo1 -117.3(2) 7 . . . ? S2 Cu2 S2 Mo1 0.0 7 . . . ? N3 Cu2 S2 Cu1 -171.4(2) . . . . ? N3 Cu2 S2 Cu1 -55.3(2) 7 . . . ? S2 Cu2 S2 Cu1 62.03(7) 7 . . . ? Mo1 Cu2 S2 Cu1 62.03(7) . . . . ? N4 Cu1 N1 C5 -62.8(7) . . . . ? S2 Cu1 N1 C5 171.5(6) . . . . ? S1 Cu1 N1 C5 57.4(7) 7 . . . ? Mo1 Cu1 N1 C5 117.7(6) . . . . ? N4 Cu1 N1 C1 113.7(6) . . . . ? S2 Cu1 N1 C1 -11.9(6) . . . . ? S1 Cu1 N1 C1 -126.1(6) 7 . . . ? Mo1 Cu1 N1 C1 -65.7(7) . . . . ? N2 Cu3 N2 C11 51.6(6) 7 . . . ? S1 Cu3 N2 C11 173.0(6) . . . . ? S1 Cu3 N2 C11 -70.6(7) 7 . . . ? Mo1 Cu3 N2 C11 -128.4(6) . . . . ? N2 Cu3 N2 C7 -129.6(7) 7 . . . ? S1 Cu3 N2 C7 -8.2(6) . . . . ? S1 Cu3 N2 C7 108.2(6) 7 . . . ? Mo1 Cu3 N2 C7 50.4(7) . . . . ? N3 Cu2 N3 C13 -35(3) 7 . . . ? S2 Cu2 N3 C13 92(3) . . . . ? S2 Cu2 N3 C13 -151(3) 7 . . . ? Mo1 Cu2 N3 C13 145(3) . . . . ? N1 Cu1 N4 C14 89(5) . . . . ? S2 Cu1 N4 C14 -156(5) . . . . ? S1 Cu1 N4 C14 -36(5) 7 . . . ? Mo1 Cu1 N4 C14 -92(5) . . . . ? C5 N1 C1 C2 -1.7(14) . . . . ? Cu1 N1 C1 C2 -178.5(8) . . . . ? N1 C1 C2 C3 -1.3(16) . . . . ? C1 C2 C3 C4 2.9(17) . . . . ? C2 C3 C4 C5 -1.5(17) . . . . ? C1 N1 C5 C4 3.2(13) . . . . ? Cu1 N1 C5 C4 179.8(7) . . . . ? C1 N1 C5 C6 -178.6(8) . . . . ? Cu1 N1 C5 C6 -2.0(11) . . . . ? C3 C4 C5 N1 -1.7(15) . . . . ? C3 C4 C5 C6 -179.8(10) . . . . ? C11 N2 C7 C8 -0.7(13) . . . . ? Cu3 N2 C7 C8 -179.5(7) . . . . ? N2 C7 C8 C9 0.6(16) . . . . ? C7 C8 C9 C10 0.2(18) . . . . ? C8 C9 C10 C11 -0.8(17) . . . . ? C7 N2 C11 C10 0.0(13) . . . . ? Cu3 N2 C11 C10 178.8(7) . . . . ? C7 N2 C11 C12 -179.3(8) . . . . ? Cu3 N2 C11 C12 -0.5(11) . . . . ? C9 C10 C11 N2 0.7(15) . . . . ? C9 C10 C11 C12 -180.0(9) . . . . ? Cu2 N3 C13 S3 -6(100) . . . . ? Cu1 N4 C14 S4B 166(4) . . . . ? Cu1 N4 C14 S4A -20(11) . . . . ? C17 N5 C15 C16 57.5(13) . . . . ? C21 N5 C15 C16 -177.8(11) . . . . ? C19 N5 C15 C16 -58.5(13) . . . . ? C21 N5 C17 C18 -61.4(11) . . . . ? C19 N5 C17 C18 177.7(9) . . . . ? C15 N5 C17 C18 59.6(11) . . . . ? C17 N5 C19 C20 179.1(10) . . . . ? C21 N5 C19 C20 56.1(13) . . . . ? C15 N5 C19 C20 -61.0(13) . . . . ? C17 N5 C21 C22 -54.6(12) . . . . ? C19 N5 C21 C22 63.4(12) . . . . ? C15 N5 C21 C22 -178.2(10) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.348 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.075 #============================================================================ # END OF CIF