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_4117791
_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         '2(C29 H57 B1 Fe2 N7 S6 W)'
_chemical_formula_sum            'C58 H114 B2 Fe4 N14 S12 W2'
_chemical_formula_weight         2005.07
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.878(2)
_cell_angle_beta                 85.544(2)
_cell_angle_gamma                74.194(2)
_cell_formula_units_Z            2
_cell_length_a                   12.386(2)
_cell_length_b                   18.724(3)
_cell_length_c                   18.774(3)
_cell_measurement_reflns_used    12275
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.283
_cell_volume                     3981.4(11)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61993
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    3.947
_exptl_absorpt_correction_T_max  0.8271
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2008)'
_exptl_crystal_colour            black
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_exptl_crystal_description       needle
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         15198
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                12288
_reflns_number_total             15198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3010539_si_001_03.cif
_cod_data_source_block           compound4
_cod_database_code               4117791