#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100966.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100966 _chemical_formula_sum 'C31 H66 Cu4 N8 S8 W2' _chemical_formula_moiety 'C31 H66 Cu4 N8 S8 W2' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '1/2-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '1/2+X,1/2-Y,1/2+Z' _cell_length_a 10.078(4) _cell_length_b 18.958(7) _cell_length_c 13.535(5) _cell_angle_alpha 90 _cell_angle_beta 101.785(4) _cell_angle_gamma 90 _cell_volume 2531.4(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6635 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.1 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400.00 _exptl_absorpt_coefficient_mu 6.542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.264 _exptl_absorpt_correction_T_max 0.375 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 25541 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9962 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9962 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_number_total 5781 _reflns_number_gt 4715 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0500 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4715 _refine_ls_number_parameters 239 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0008Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.63 _refine_diff_density_min -1.25 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'W' 'W' -0.849 6.872 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W(1) W 0.56225(2) 0.18717(10) 0.78849(2) 0.0207(7) Uani 1.00 1 d . . . Cu(1) Cu 0.67694(9) 0.24783(5) 0.65121(6) 0.0306(2) Uani 1.00 1 d . . . Cu(2) Cu 0.45556(8) 0.12537(4) 0.93730(6) 0.0268(2) Uani 1.00 1 d . . . S(1) S 0.5376(2) 0.29912(10) 0.7385(2) 0.0396(5) Uani 1.00 1 d . . . S(2) S 0.6945(2) 0.13471(10) 0.69766(13) 0.0322(4) Uani 1.00 1 d . . . S(3) S 0.6590(2) 0.18431(9) 0.94908(12) 0.0287(4) Uani 1.00 1 d . . . S(4) S 0.3660(2) 0.13219(11) 0.76660(13) 0.0343(5) Uani 1.00 1 d . . . N(1) N 0.3391(2) 0.1795(2) 1.0146(2) 0.0246(12) Uiso 0.50 1 d P . . N(1a) N 0.2748(3) 0.2082(3) 1.0633(3) 0.038(2) Uiso 0.50 1 d P . . N(2) N 0.4781(3) 0.0309(3) 0.9853(3) 0.0306(13) Uiso 0.50 1 d P . . N(3) N 0.0983(6) 0.3770(3) 0.8289(4) 0.031(2) Uani 1.00 1 d . . . N(4) N -0.0073(12) 0.0289(6) 0.6290(9) 0.092(4) Uani 1.00 1 d . . . N(5) N 0.5000 0.5000 0.5000 0.023(2) Uani 1.00 2 d S . . C(1) C 0.2749(3) 0.2082(3) 1.0634(3) 0.038(2) Uiso 0.50 1 d P . . C(1a) C 0.3391(2) 0.1795(2) 1.0146(2) 0.0246(12) Uiso 0.50 1 d P . . C(2) C 0.4781(3) 0.0309(3) 0.9853(3) 0.0306(13) Uiso 0.50 1 d P . . C(3) C 0.0972(7) 0.4199(4) 0.7329(5) 0.036(2) Uani 1.00 1 d . . . C(4) C 0.2356(8) 0.4274(6) 0.7060(6) 0.051(3) Uani 1.00 1 d . . . C(5) C 0.1898(8) 0.4124(5) 0.9176(6) 0.044(2) Uani 1.00 1 d . . . C(6) C 0.1557(11) 0.4884(6) 0.9386(8) 0.065(3) Uani 1.00 1 d . . . C(7) C -0.0477(7) 0.3743(4) 0.8400(6) 0.036(2) Uani 1.00 1 d . . . C(8) C -0.0729(10) 0.3346(6) 0.9322(7) 0.057(3) Uani 1.00 1 d . . . C(9) C 0.1558(9) 0.3048(4) 0.8208(7) 0.048(2) Uani 1.00 1 d . . . C(10) C 0.0818(12) 0.2589(5) 0.7343(8) 0.067(3) Uani 1.00 1 d . . . C(11) C 0.0228(10) 0.0766(6) 0.5859(8) 0.061(3) Uani 1.00 1 d . . . C(12) C 0.0601(12) 0.1364(6) 0.5295(9) 0.068(3) Uani 1.00 1 d . . . C(13) C 0.433(2) 0.5386(8) 0.5763(11) 0.035(3) Uiso 0.50 1 d P . . C(14) C 0.479(2) 0.6113(10) 0.607(2) 0.044(5) Uiso 0.50 1 d P . . C(15) C 0.6570(13) 0.5027(7) 0.5346(10) 0.026(3) Uiso 0.50 1 d P . . C(16) C 0.713(2) 0.4748(10) 0.639(2) 0.038(5) Uiso 0.50 1 d P . . C(17) C 0.451(2) 0.4250(9) 0.4955(12) 0.043(4) Uiso 0.50 1 d P . . C(18) C 0.498(2) 0.3795(9) 0.4195(13) 0.031(3) Uiso 0.50 1 d P . . C(19) C 0.468(2) 0.5377(9) 0.3984(12) 0.040(4) Uiso 0.50 1 d P . . C(20) C 0.317(2) 0.5356(10) 0.349(1) 0.033(4) Uiso 0.50 1 d P . . H(1) H 0.0383 0.3972 0.6784 0.043 Uiso 1.00 1 c R . . H(2) H 0.0637 0.4657 0.7421 0.043 Uiso 1.00 1 c R . . H(3) H 0.2705 0.3819 0.6962 0.063 Uiso 1.00 1 c R . . H(4) H 0.2276 0.4542 0.6458 0.063 Uiso 1.00 1 c R . . H(5) H 0.2954 0.4507 0.7593 0.063 Uiso 1.00 1 c R . . H(6) H 0.1864 0.3855 0.9763 0.051 Uiso 1.00 1 c R . . H(7) H 0.2795 0.4116 0.9057 0.051 Uiso 1.00 1 c R . . H(8) H 0.2182 0.5061 0.9955 0.080 Uiso 1.00 1 c R . . H(9) H 0.1613 0.5157 0.8808 0.080 Uiso 1.00 1 c R . . H(10) H 0.0668 0.4905 0.9520 0.080 Uiso 1.00 1 c R . . H(11) H -0.0784 0.4214 0.8439 0.045 Uiso 1.00 1 c R . . H(12) H -0.0991 0.3521 0.7816 0.045 Uiso 1.00 1 c R . . H(13) H -0.1664 0.3356 0.9347 0.071 Uiso 1.00 1 c R . . H(14) H -0.0447 0.2871 0.9275 0.071 Uiso 1.00 1 c R . . H(15) H -0.0226 0.3560 0.9916 0.071 Uiso 1.00 1 c R . . H(16) H 0.2467 0.3102 0.8128 0.056 Uiso 1.00 1 c R . . H(17) H 0.1550 0.2806 0.8822 0.056 Uiso 1.00 1 c R . . H(18) H -0.0099 0.2536 0.7405 0.078 Uiso 1.00 1 c R . . H(19) H 0.0847 0.2815 0.6721 0.078 Uiso 1.00 1 c R . . H(20) H 0.1242 0.2139 0.7373 0.078 Uiso 1.00 1 c R . . H(21) H 0.1317 0.1233 0.4973 0.081 Uiso 1.00 1 c R . . H(22) H 0.0889 0.1745 0.5745 0.081 Uiso 1.00 1 c R . . H(23) H -0.0163 0.1506 0.4801 0.081 Uiso 1.00 1 c R . .