Selenium as a Structural Surrogate of Sulfur: Template-Assisted Assembly of Five Types of Tungsten-Iron-Sulfur/Selenium Clusters and the Structural Fate of Chalcogenide Reactants
Bo Zheng; Xu-Dong Chen; Shao-Liang Zheng; R. H. Holm; Journal of the American Chemical Society 134 (2012) 6479–6490; doi:10.1021/ja3010539

data_4117793
_publ_section_title
;
 Selenium as a Structural Surrogate of Sulfur: Template-Assisted Assembly
 of Five Types of Tungsten-Iron-Sulfur/Selenium Clusters and the
 Structural Fate of Chalcogenide Reactants
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6479
_journal_page_last               6490
_journal_paper_doi               10.1021/ja3010539
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'(C21 H37 B Fe3 N6 S6 Se W), (C8 H20 N), 0.5(C4 H8 O)'
_chemical_formula_sum            'C31 H61 B Fe3 N7 O0.5 S6 Se W'
_chemical_formula_weight         1173.40
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.973(2)
_cell_angle_beta                 91.723(2)
_cell_angle_gamma                110.001(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7035(15)
_cell_length_b                   11.7457(16)
_cell_length_c                   20.309(3)
_cell_measurement_reflns_used    11016
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.718
_cell_measurement_theta_min      2.2245
_cell_volume                     2397.2(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEx2 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      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker D8 goniometer with 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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27077
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.8810
_exptl_absorpt_correction_T_min  0.4932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.775
_refine_diff_density_min         -2.446
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9127
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0513P)^2^+15.3147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                8214
_reflns_number_total             9127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3010539_si_001_05.cif
_cod_data_source_block           compound6b
_cod_database_code               4117793