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_4117795
_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         'C67 H135 B2 Fe6 N19 O3.5 S9 Se2 W2'
_chemical_formula_sum            'C67 H135 B2 Fe6 N19 O3.5 S9 Se2 W2'
_chemical_formula_weight         2433.82
_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                 94.2900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5402(13)
_cell_length_b                   18.5500(10)
_cell_length_c                   25.5168(13)
_cell_measurement_reflns_used    13056
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.594
_cell_measurement_theta_min      2.174
_cell_volume                     11111.2(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93060
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.6455
_exptl_absorpt_correction_T_min  0.5112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2008)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       Block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         21162
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+30.9707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                15758
_reflns_number_total             21162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3010539_si_001_07.cif
_cod_data_source_block           compound9
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4117795