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_4309012
_publ_contact_author_address
;Nikolaev 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)309489
_publ_contact_author_name        'Dr. Dmitry Yu. Naumov'
_publ_contact_author_phone       7(3832)309466
_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_sum            'C55 H66 Mo3 O24 P2 Se4'
_chemical_formula_weight         1776.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.2850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3693(10)
_cell_length_b                   14.6896(6)
_cell_length_c                   31.1011(19)
_cell_measurement_reflns_used    4592
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.09
_cell_measurement_theta_min      2.58
_cell_volume                     6860.9(7)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f 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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39670
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.14
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.4179
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         12432
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0769P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                7865
_reflns_number_total             12432
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0488637si20050204_023927.cif
_cod_data_source_block           ag138
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4309012