Synthesis and Crystal Structure of a Sulfur-bridged Incomplete Cubane-type Molybdenum Cluster with a Tris(pyrazolyl)methanesulfonate Ligand
MORIWAKI, Kazuhiro; YOSHIDA, Ryouichi; AKASHI, Haruo; X-ray Structure Analysis Online 30 (2014) 11–; doi:10.2116/xraystruct.30.11

data_1551652
_publ_section_title
;
 Synthesis and Crystal Structure of a Sulfur-bridged Incomplete
 Cubane-type Molybdenum Cluster with a Tris(pyrazolyl)methanesulfonate
 Ligand
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              11
_journal_paper_doi               10.2116/xraystruct.30.11
_journal_volume                  30
_journal_year                    2014
_chemical_formula_moiety         'C45 H46 Cl12 Mo6 N24 O13 S12'
_chemical_formula_sum            'C45 H46 Cl12 Mo6 N24 O13 S12'
_chemical_formula_weight         2516.81
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 132.942(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.509(7)
_cell_length_b                   29.273(6)
_cell_length_c                   16.490(5)
_cell_measurement_reflns_used    6158
_cell_measurement_temperature    93
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.25
_cell_volume                     8661(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16204
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4944.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7989
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0286P)^2^+183.6587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                6688
_reflns_number_total             7991
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            30_11_1.txt
_cod_data_source_block           120730b
_cod_database_code               1551652