Precursors to Clusters with the Topology of the PNCluster of Nitrogenase: Edge-Bridged Double Cubane Clusters [(Tp)2Mo2Fe6S8L4]z: Synthesis, Structures, and Electron Transfer Series
Berlinguette, Curtis P.; Miyaji, Taichi; Zhang, Yugen; Holm, R. H.; Inorganic Chemistry 45 (2006) 1997–2007; doi:10.1021/ic051770k

data_4331875
_publ_section_title
;
 Precursors to Clusters with the Topology of the PNCluster of
 Nitrogenase:&#x00A0; Edge-Bridged Double Cubane Clusters
 [(Tp)2Mo2Fe6S8L4]z:&#x00A0; Synthesis, Structures, and Electron Transfer
 Series
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1997
_journal_page_last               2007
_journal_paper_doi               10.1021/ic051770k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C96 H189 B2 F4 Fe6 Mo2 N23 O2 S8'
_chemical_formula_sum            'C96 H189 B2 F4 Fe6 Mo2 N23 O2 S8'
_chemical_formula_weight         2578.8
_chemical_name_common            EBDC-F4-
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.526(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.081(13)
_cell_length_b                   15.937(13)
_cell_length_c                   25.45(2)
_cell_measurement_temperature    273(2)
_cell_volume                     6492(9)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0898
_diffrn_reflns_av_sigmaI/netI    0.1848
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27212
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2698
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1205
_refine_ls_number_reflns         17230
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.235
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+14.6637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                9513
_reflns_number_total             17230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051770ksup1.cif
_cod_data_source_block           (TBA)3(8).7MeCN.2H2O
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4331875