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_4309011
_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 S7, Cl0.5, 3.5(H2 O), Cs2.5'
_chemical_formula_sum            'C6 H7 Cl0.5 Cs2.5 Mo3 O15.5 S7'
_chemical_formula_weight         1189.36
_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                 91.3310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0054(3)
_cell_length_b                   16.1190(4)
_cell_length_c                   23.8186(5)
_cell_measurement_reflns_used    8007
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.53
_cell_volume                     5375.7(2)
_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      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35905
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.371
_exptl_absorpt_correction_T_max  0.3768
_exptl_absorpt_correction_T_min  0.3124
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.226
_refine_diff_density_min         -2.564
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9753
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0543P)^2^+19.7096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                8446
_reflns_number_total             9753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0488637si20050204_023859.cif
_cod_data_source_block           ag131
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C6 H7 Cl0.50 Cs2.50 Mo3 O15.50 S7'
_cod_database_code               4309011