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_4110856
_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_sum            'C48 H93 B2 Fe6 Mo2 N16 O0 S10 Se'
_chemical_formula_weight         1846.85
_chemical_name_common            (Et4N)3.Cluster.1MeCN
_chemical_name_systematic
; 
 ? 
;
_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                91.50(16)
_cell_angle_beta                 101.83(17)
_cell_angle_gamma                115.15(9)
_cell_formula_units_Z            2
_cell_length_a                   14.98(5)
_cell_length_b                   17.10(6)
_cell_length_c                   18.49(7)
_cell_measurement_reflns_used    8692
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.638
_cell_measurement_theta_min      2.42
_cell_volume                     4162(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19515
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    2.052
_exptl_absorpt_correction_T_max  0.6497
_exptl_absorpt_correction_T_min  0.5596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00015(11)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.166
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+6.4566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2186
_refine_ls_wR_factor_ref         0.2593
_reflns_number_gt                5070
_reflns_number_total             8692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063604xsi20060523_110500_3.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        4160.(25)
_cod_database_code               4110856