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_4309013
_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 Mo3 O12 Se7, Br0.5, 4(H2 O), K2.5'
_chemical_formula_sum            'C6 H8 Br0.5 K2.5 Mo3 O16 Se7'
_chemical_formula_weight         1314.37
_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                 100.8780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0725(8)
_cell_length_b                   13.5246(8)
_cell_length_c                   27.3192(15)
_cell_measurement_reflns_used    5421
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.56
_cell_measurement_theta_min      2.98
_cell_volume                     5468.9(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23210
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.847
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.947
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0458P)^2^+34.9416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                6536
_reflns_number_total             7869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488637si20050204_023951.cif
_cod_data_source_block           ag64
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C6 H8 Br0.50 K2.50 Mo3 O16 Se7'
_cod_database_code               4309013