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_4326780
_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         'C36 H84 Fe6 Mo2 N6 Na2 S14, C4 H10 O'
_chemical_formula_sum            'C40 H94 Fe6 Mo2 N6 Na2 O S14'
_chemical_formula_weight         1697.15
_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                 91.349(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8665(14)
_cell_length_b                   20.871(3)
_cell_length_c                   17.322(2)
_cell_measurement_reflns_used    16089
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.27
_cell_volume                     3566.0(8)
_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(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55107
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  0.8584
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             1663
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.794
_refine_diff_density_min         -2.199
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0753P)^2^+28.6916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                6005
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2018117_si_002_14.cif
_cod_data_source_block           amit78
_cod_original_cell_volume        3566.0(9)
_cod_database_code               4326780