Edge-Bridged Mo2Fe6S8 to PN-Type Mo2Fe6S9 Cluster Conversion: Structural Fate of the Attacking Sulfide/Selenide Nucleophile
Curtis P. Berlinguette; R. H. Holm; Journal of the American Chemical Society 128 (2006) 11993–12000; doi:10.1021/ja063604x

data_4110854
_publ_contact_author_address
;
      Department of Chemistry and Chemical Biology
      Harvard University
      12 Oxford Street
      Cambridge, MA 02138
      USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '617 496-9289'
_publ_contact_author_name        'Richard H. Holm'
_publ_contact_author_phone       '617 495-0853'
_publ_section_title
;
 Edge-Bridged Mo2Fe6S8 to PN-Type Mo2Fe6S9 Cluster Conversion: Structural
 Fate of the Attacking Sulfide/Selenide Nucleophile
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11993
_journal_page_last               12000
_journal_paper_doi               10.1021/ja063604x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         C47.50H90.25B2Fe6Mo2N17.50S10.09Se0.92
_chemical_formula_sum            'C47.5 H90.25 B2 Fe6 Mo2 N17.5 S10.09 Se0.92'
_chemical_formula_weight         1858.3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 115.456(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.048(2)
_cell_length_b                   17.736(3)
_cell_length_c                   18.142(3)
_cell_measurement_reflns_used    15909
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.747
_cell_measurement_theta_min      2.615
_cell_volume                     4662.4(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15909
_diffrn_reflns_theta_full        18.85
_diffrn_reflns_theta_max         18.85
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.8418
_exptl_absorpt_correction_T_min  0.7396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             1777
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00061(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         3818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.770
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+110.6985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2527
_refine_ls_wR_factor_ref         0.2587
_reflns_number_gt                3412
_reflns_number_total             3818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063604xsi20060523_110500_1.cif
_cod_data_source_block           (TEA)3[(Tp)2Mo2Fe6S8Se(SH)2](4).2.75MeCN
_cod_original_cell_volume        4662.6(13)
_cod_original_formula_sum
'C47.50 H90.25 B2 Fe6 Mo2 N17.50 S10.09 Se0.92'
_cod_database_code               4110854