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_4326781
_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         'C21 H48 Fe3 N3 S6 Se W'
_chemical_formula_sum            'C21 H48 Fe3 N3 S6 Se W'
_chemical_formula_weight         965.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.982(3)
_cell_length_b                   16.568(2)
_cell_length_c                   9.7591(12)
_cell_measurement_reflns_used    19213
_cell_measurement_temperature    15(1)
_cell_measurement_theta_max      16.20
_cell_measurement_theta_min      2.21
_cell_volume                     3230.9(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX II v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      15(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46168
_diffrn_reflns_theta_full        16.23
_diffrn_reflns_theta_max         16.23
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.8761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       needle
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.204
_refine_diff_density_min         -3.746
_refine_diff_density_rms         0.351
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         7624
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+153.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                7342
_reflns_number_total             7624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2018117_si_002_15.cif
_cod_data_source_block           dataatAPS
_cod_original_cell_volume        3230.8(7)
_cod_database_code               4326781