Hybrid Metal Carbonyl−Oxide Clusters: Synthesis and Structure of [Et4N]2[(OC)5WSbW3(CO)9(μ3-OMe)2(μ3-O)WO2(OR)] (R = Me, H)
Xu, Li; Whitmire, Kenton H.; Organometallics 21 (2002) 2581–; doi:10.1021/om020129c

data_4076845
_publ_section_title
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 Hybrid Metal Carbonyl&#x2212;Oxide Clusters:&#x00A0; Synthesis and
 Structure of [Et4N]2[(OC)5WSbW3(CO)9(\m3-OMe)2(\m3-O)WO2(OR)] (R = Me, H)
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2581
_journal_paper_doi               10.1021/om020129c
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C32 H47 N2 O20 Sb W5'
_chemical_formula_weight         1820.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.352(2)
_cell_length_b                   44.091(9)
_cell_length_c                   19.876(4)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    570(2)
_cell_measurement_theta_max      44.649
_cell_measurement_theta_min      4.326
_cell_volume                     9648(3)
_computing_cell_refinement       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_collection       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_reduction        'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      570(2)
_diffrn_detector_area_resol_mean 0.9400
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker AXS Smart 1000 CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2678
_diffrn_reflns_av_sigmaI/netI    0.2013
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            44691
_diffrn_reflns_theta_full        23.41
_diffrn_reflns_theta_max         23.41
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    12.496
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6672
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.184
_refine_diff_density_min         -3.521
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         13951
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          1.121
_refine_ls_shift/su_mean         0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                7441
_reflns_number_total             13951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020129c.cif
_cod_data_source_block           '[Et4N]2[1b]'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4076845