Synthesis, Structures, and Photochemistry of Tricarbonyl Metal Polyoxoanion Complexes, [X2W20O70{M(CO)3}2]12- (X = Sb, Bi and M = Re, Mn)
Chongchao Zhao; Choon Sung Kambara; Ye Yang; Alexey L. Kaledin; Djamaladdin G. Musaev; Tianquan Lian; Craig L. Hill; Inorganic Chemistry 52 (2013) 671–678; doi:10.1021/ic301766b

data_4333540
_publ_section_title
;
 Synthesis, Structures, and Photochemistry of Tricarbonyl Metal
 Polyoxoanion Complexes, [X2W20O70{M(CO)3}2]12- (X = Sb, Bi and M = Re,
 Mn)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              671
_journal_page_last               678
_journal_paper_doi               10.1021/ic301766b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C6 K9 Mn2 Na3 O83 Sb2 W20'
_chemical_formula_sum            'C6 K9 Mn2 Na3 O83 Sb2 W20'
_chemical_formula_weight         5851.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.3750(10)
_cell_angle_beta                 74.3070(10)
_cell_angle_gamma                75.0430(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4433(10)
_cell_length_b                   13.0947(10)
_cell_length_c                   15.8076(13)
_cell_measurement_reflns_used    7746
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.46
_cell_volume                     2392.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37914
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.236
_exptl_absorpt_correction_T_max  0.6323
_exptl_absorpt_correction_T_min  0.1869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.282
_refine_diff_density_min         -2.620
_refine_diff_density_rms         0.427
_refine_ls_extinction_coef       0.00004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         10154
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+96.5540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                8131
_reflns_number_total             10154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301766b_si_002_3.cif
_cod_data_source_block           2a_SbMn
_cod_database_code               4333540