Specific Incorporation of Chalcogenide Bridge Atoms in Molybdenum/Tungsten-Iron-Sulfur Single Cubane Clusters
Amit Majumdar; R. H. Holm; Inorganic Chemistry 50 (2011) 11242–11251; doi:10.1021/ic2018117

data_4326772
_publ_contact_author_address
;Department of Chemistry and Chemical Biology
Harvard University
12 Oxford Street
Cambridge, MA 02138
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_name        'Prof. Richard H. Holm'
_publ_contact_author_phone       617-496-3215
_publ_section_title
;
 Specific Incorporation of Chalcogenide Bridge Atoms in
 Molybdenum/Tungsten-Iron-Sulfur Single Cubane Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11242
_journal_page_last               11251
_journal_paper_doi               10.1021/ic2018117
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C33 H48 Fe3 Mo N3 S7, 2(C2 H3 N)'
_chemical_formula_sum            'C37 H54 Fe3 Mo N5 S7'
_chemical_formula_weight         1056.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 96.336(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.137(3)
_cell_length_b                   20.952(5)
_cell_length_c                   16.063(4)
_cell_measurement_reflns_used    4677
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.74
_cell_measurement_theta_min      2.32
_cell_volume                     4394.3(18)
_computing_cell_refinement       'Saint v7.46A (Bruker-AXS,2009'
_computing_data_collection       'APEX2 v2009.3.0(Bruker-AXS,2009)'
_computing_data_reduction        'Saint v7.46A (Bruker-AXS,2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39141
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.9382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            Black-brown
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       Block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.140
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+42.5079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                5374
_reflns_number_total             8340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2018117_si_002_06.cif
_cod_data_source_block           Am50
_cod_original_cell_volume        4394.4(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4326772