Structural Conversions of Molybdenum-Iron-Sulfur Edge-Bridged Double Cubanes and PN-Type Clusters Topologically Related to the Nitrogenase P-Cluster
Yugen Zhang; R. H. Holm; Inorganic Chemistry 43 (2004) 674–682; doi:10.1021/ic030259t

data_4310378
_publ_section_title
;
 Structural Conversions of Molybdenum-Iron-Sulfur Edge-Bridged Double
 Cubanes and PN-Type Clusters Topologically Related to the Nitrogenase
 P-Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              674
_journal_page_last               682
_journal_paper_doi               10.1021/ic030259t
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         (Et4N)3[Tp2Mo2Fe6S8(SPh)4]MeCN
_chemical_formula_sum            'C68 H103 B2 Fe6 Mo2 N16 S12'
_chemical_formula_weight         2077.98
_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                84.84(3)
_cell_angle_beta                 72.41(3)
_cell_angle_gamma                70.77(3)
_cell_formula_units_Z            1
_cell_length_a                   12.333(3)
_cell_length_b                   13.935(3)
_cell_length_c                   15.016(3)
_cell_measurement_temperature    193(2)
_cell_volume                     2322.6(11)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.1790
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14160
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark green '
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1065
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9083
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          3.593
_refine_ls_shift/su_mean         0.368
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4135
_reflns_number_total             9083
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic030259t_03.cif
_cod_data_source_block           (Et4N)3[Tp2Mo2Fe6S8(SPh)4]MeCN
_cod_original_cell_volume        2322.6(8)
_cod_database_code               4310378