Synthesis and Crystal Structure of a Sulfur-bridged Cubane-type Molybdenum-Palladium Cluster with a Hydrotris(methimazolyl)borate Ligand
YOSHIDA, Ryouichi; SATO, Hiroyasu; AKASHI, Haruo; X-ray Structure Analysis Online 29 (2013) 3–; doi:10.2116/xraystruct.29.3

data_1551692
_publ_section_title
;
 Synthesis and Crystal Structure of a Sulfur-bridged Cubane-type
 Molybdenum-Palladium Cluster with a Hydrotris(methimazolyl)borate Ligand
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              3
_journal_paper_doi               10.2116/xraystruct.29.3
_journal_volume                  29
_journal_year                    2013
_chemical_formula_moiety         'C54.50 H71 B3 F6 Mo3 N18 O3.50 P2 Pd S13'
_chemical_formula_sum            'C54.5 H71 B3 F6 Mo3 N18 O3.5 P2 Pd S13'
_chemical_formula_weight         2053.65
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                109.806(8)
_cell_angle_beta                 96.546(7)
_cell_angle_gamma                101.774(7)
_cell_formula_units_Z            2
_cell_length_a                   14.8578(3)
_cell_length_b                   14.9415(3)
_cell_length_c                   20.3082(14)
_cell_measurement_temperature    93
_cell_volume                     4069.5(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_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 10.000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48637
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.501
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2062.00
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.610
_refine_diff_density_min         -0.910
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         14608
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0894P)^2^+5.5878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                12575
_reflns_number_total             14608
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            29_3_1.txt
_cod_data_source_block           shelxl_
_cod_original_cell_volume        4069.5(5)
_cod_original_formula_sum        'C54.50 H71 B3 F6 Mo3 N18 O3.50 P2 Pd S13'
_cod_database_code               1551692