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_4331874
_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         'C43 H80 B2 F3 Fe6 Mo2 N12 O3 P4 S9'
_chemical_formula_sum            'C43 H80 B2 F3 Fe6 Mo2 N12 O3 P4 S9'
_chemical_formula_weight         1831.23
_chemical_name_common            EBDC-PEt3+
_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                72.162(17)
_cell_angle_beta                 79.29(2)
_cell_angle_gamma                65.66(2)
_cell_formula_units_Z            1
_cell_length_a                   11.690(4)
_cell_length_b                   12.858(4)
_cell_length_c                   14.298(5)
_cell_measurement_reflns_used    8779
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.890
_cell_measurement_theta_min      2.613
_cell_volume                     1859.6(11)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13107
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  27.89
_exptl_absorpt_correction_T_min  2.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             907
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+0.1614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                7233
_reflns_number_total             8779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051770ksup1.cif
_cod_data_source_block           (7).(CF3SO3)
_cod_original_cell_volume        1859.6(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331874