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_4076844
_publ_section_title
;
 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)
;
_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            'C33 H49 N2 O20 Sb W5'
_chemical_formula_weight         1834.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 112.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.606(8)
_cell_length_b                   11.595(2)
_cell_length_c                   24.166(5)
_cell_measurement_reflns_used    277
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.749
_cell_measurement_theta_min      4.555
_cell_volume                     10022(4)
_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      293(2)
_diffrn_detector_area_resol_mean 0.8957
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21336
_diffrn_reflns_theta_full        23.36
_diffrn_reflns_theta_max         23.36
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    12.031
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.235
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          '0.72 mm'
_exptl_crystal_size_mid          '0.17 mm'
_exptl_crystal_size_min          '0.07 mm'
_refine_diff_density_max         1.239
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          1.406
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5916
_reflns_number_total             7098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020129c.cif
_cod_data_source_block           '[Et4N]2[1a]'
_cod_original_cell_volume        10022(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076844