Cluster Oxalate Complexes [M3(μ3-Q)(μ2-Q2)3(C2O4)3]2- and [Mo3(μ3-Q)(μ2-Q)3(C2O4)3(H2O)3]2- (M = Mo, W; Q = S, Se): Mechanochemical Synthesis and Crystal Structure
Maxim N. Sokolov; Artyom L. Gushchin; Dmitrii Yu. Naumov; Olga A. Gerasko; Vladimir P. Fedin; Inorganic Chemistry 44 (2005) 2431–2436; doi:10.1021/ic0488637

data_4309015
_publ_contact_author_address
;Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Academition Lavrentiev Avenue 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       d.y.naumov@ngs.ru
_publ_contact_author_fax         7(3832)344489
_publ_contact_author_name        'Dmitry Yu. Naumov'
_publ_contact_author_phone       7(3832)344466
_publ_section_title
;
Cluster Oxalate Complexes [M3(\m3-Q)(\m2-Q2)3(C2O4)3]2- and
[Mo3(\m3-Q)(\m2-Q)3(C2O4)3(H2O)3]2- (M = Mo, W; Q = S, Se):
Mechanochemical Synthesis and Crystal Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2431
_journal_page_last               2436
_journal_paper_doi               10.1021/ic0488637
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C6 O12 S7 Mo3, Br0.5, 3(H2O), K2.5'
_chemical_formula_sum            'C6 H6 Br0.5 K2.5 Mo3 O15 S7'
_chemical_formula_weight         968.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.154(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7810(8)
_cell_length_b                   13.1362(7)
_cell_length_c                   26.7804(14)
_cell_measurement_reflns_used    4994
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      3.59
_cell_volume                     5133.6(5)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.1270
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21374
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.258
_exptl_absorpt_correction_T_max  0.5342
_exptl_absorpt_correction_T_min  0.3951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.000052(13)
_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   0.814
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                5019
_reflns_number_total             8997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488637si20050204_024042.cif
_cod_data_source_block           ag78
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C6 H6 Br0.50 K2.50 Mo3 O15 S7'
_cod_database_code               4309015