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_4113599
_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)5[Tp4Mo4Fe12S14Se6]8CH3CN
_chemical_formula_sum            'C46 H82 B2 Fe6 Mo2 N18.5 S7 Se3'
_chemical_formula_weight         1904.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.883(10)
_cell_length_b                   26.168(6)
_cell_length_c                   16.194(6)
_cell_measurement_temperature    293(2)
_cell_volume                     15630(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0912
_diffrn_reflns_av_sigmaI/netI    0.1974
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55706
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.070(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         18937
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                8681
_reflns_number_total             18937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0214633_8.cif
_cod_data_source_block           (Et4N)5[Tp4Mo4Fe12S14Se6]8CH3CN
_cod_original_cell_volume        15631(7)
_cod_original_formula_sum        'C46 H82 B2 Fe6 Mo2 N18.50 S7 Se3'
_cod_database_code               4113599