#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4060240.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_4060240 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C20 H14 O10 W2' _chemical_formula_weight 782.01 _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 8.3085(7) _cell_length_b 8.5524(8) _cell_length_c 8.6499(8) _cell_angle_alpha 61.2290(10) _cell_angle_beta 69.9280(10) _cell_angle_gamma 79.162(2) _cell_volume 505.85(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1910 _cell_measurement_theta_min 5.436 _cell_measurement_theta_max 54.957 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.239 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.141 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 362 _exptl_absorpt_coefficient_mu 11.419 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.55897 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3110 _diffrn_reflns_av_R_equivalents 0.1508 _diffrn_reflns_av_sigmaI/netI 0.1072 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 28.31 _reflns_number_total 2247 _reflns_number_gt 2047 _reflns_threshold_expression >2sigma(I) _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^)+(0.0796P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.004(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2247 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.013 _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 W W 0.55688(4) 0.58392(5) 0.77968(5) 0.0217(2) Uani 1 1 d . . . O1 O 0.5342(13) 0.8926(13) 0.8818(13) 0.043(2) Uani 1 1 d . . . O2 O 0.1898(11) 0.4425(15) 0.9210(14) 0.047(2) Uani 1 1 d . . . O3 O 0.3606(13) 0.8780(13) 0.5135(14) 0.048(2) Uani 1 1 d . . . O4 O 0.8000(14) 0.8672(17) 0.2469(15) 0.055(3) Uani 1 1 d . . . O5 O 0.9642(11) 0.8814(12) 0.3933(13) 0.040(2) Uani 1 1 d . . . C1 C 0.5372(14) 0.7764(13) 0.8495(14) 0.023(2) Uani 1 1 d . . . C2 C 0.3221(14) 0.4933(16) 0.8781(14) 0.028(2) Uani 1 1 d . . . C3 C 0.4345(14) 0.7710(16) 0.6121(16) 0.030(2) Uani 1 1 d . . . C4 C 0.7025(15) 0.5061(17) 0.5457(17) 0.035(3) Uani 1 1 d . . . H4 H 0.6501 0.5267 0.4580 0.042 Uiso 1 1 calc R . . C5 C 0.6939(16) 0.3470(19) 0.7109(19) 0.040(3) Uani 1 1 d . . . H5 H 0.6357 0.2452 0.7508 0.048 Uiso 1 1 calc R . . C6 C 0.7902(15) 0.3708(16) 0.8045(17) 0.034(2) Uani 1 1 d . . . H6 H 0.8067 0.2859 0.9168 0.041 Uiso 1 1 calc R . . C7 C 0.8571(13) 0.5438(17) 0.7005(16) 0.032(2) Uani 1 1 d . . . H7 H 0.9232 0.5931 0.7329 0.038 Uiso 1 1 calc R . . C8 C 0.8045(14) 0.6303(16) 0.5347(15) 0.029(2) Uani 1 1 d . . . C9 C 0.8531(15) 0.8071(17) 0.3779(15) 0.034(3) Uani 1 1 d . . . C10 C 1.0280(19) 1.053(2) 0.240(2) 0.051(4) Uani 1 1 d . . . H10A H 1.1017 1.0360 0.1362 0.077 Uiso 1 1 calc R . . H10B H 1.0912 1.1061 0.2769 0.077 Uiso 1 1 calc R . . H10C H 0.9331 1.1310 0.2067 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.0171(3) 0.0264(3) 0.0175(3) -0.00830(18) -0.00342(16) 0.00066(15) O1 0.054(6) 0.035(5) 0.031(5) -0.008(4) -0.012(4) -0.003(4) O2 0.028(5) 0.070(7) 0.043(5) -0.025(5) -0.005(4) -0.013(4) O3 0.046(5) 0.043(5) 0.039(5) -0.004(4) -0.021(4) 0.007(4) O4 0.042(6) 0.068(7) 0.038(5) -0.007(5) -0.012(4) -0.010(5) O5 0.031(4) 0.040(5) 0.042(5) -0.013(4) -0.006(4) -0.009(4) C1 0.030(5) 0.021(5) 0.021(5) -0.009(4) -0.010(4) 0.001(4) C2 0.023(5) 0.040(6) 0.012(4) -0.006(4) -0.004(4) 0.001(4) C3 0.023(5) 0.036(6) 0.027(5) -0.012(5) -0.004(4) -0.003(4) C4 0.031(6) 0.047(7) 0.030(6) -0.023(6) -0.006(5) 0.001(5) C5 0.028(6) 0.049(8) 0.041(7) -0.028(6) 0.004(5) 0.000(5) C6 0.030(6) 0.033(6) 0.030(6) -0.012(5) -0.011(5) 0.014(4) C7 0.013(5) 0.043(6) 0.028(6) -0.013(5) -0.001(4) 0.009(4) C8 0.022(5) 0.039(6) 0.021(5) -0.015(5) 0.003(4) -0.003(4) C9 0.030(6) 0.044(7) 0.013(5) -0.007(5) 0.002(4) -0.001(5) C10 0.041(8) 0.049(8) 0.050(8) -0.016(7) -0.002(6) -0.008(6)