Synthesis of a Molecular Mo2Fe6S9 Cluster with the Topology of the PN Cluster of Nitrogenase by Rearrangement of an Edge-Bridged Mo2Fe6S8 Double Cubane
Yugen Zhang; R. H. Holm; Journal of the American Chemical Society 125 (2003) 3910–3920; doi:10.1021/ja0214633

data_4113598
_publ_section_title
;
 Synthesis of a Molecular Mo2Fe6S9 Cluster with the Topology of the PN
 Cluster of Nitrogenase by Rearrangement of an Edge-Bridged Mo2Fe6S8
 Double Cubane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3910
_journal_page_last               3920
_journal_paper_doi               10.1021/ja0214633
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         (Et4N)2[TpMoFe3S4(S-p-tol)3]
_chemical_formula_sum            'C92 H142 B2 Fe6 Mo2 N16 S14'
_chemical_formula_weight         2469.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 116.927(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.136(8)
_cell_length_b                   11.871(3)
_cell_length_c                   31.277(7)
_cell_measurement_temperature    293(2)
_cell_volume                     11300(5)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.1112
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40375
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       plate
_exptl_crystal_F_000             5049
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.352
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1226
_refine_ls_number_reflns         12114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.168
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+639.8959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2800
_refine_ls_wR_factor_ref         0.2954
_reflns_number_gt                8519
_reflns_number_total             12114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0214633_7.cif
_cod_data_source_block           (Et4N)2[TpMoFe3S4(S-p-tol)3]
_cod_original_cell_volume        11300(4)
_cod_database_code               4113598