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_4331877
_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         'C82 H164 B2 Fe6 Mo2 N28 S8'
_chemical_formula_sum            'C82 H148 B2 Fe6 Mo2 N28 S8'
_chemical_formula_weight         2347.47
_chemical_name_common            'EBDC-Cl 3-'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.7(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.38(4)
_cell_length_b                   19.10(6)
_cell_length_c                   33.68(8)
_cell_measurement_reflns_used    38419
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15.593
_cell_measurement_theta_min      2.212
_cell_volume                     10948(5)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            38419
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7226
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.176
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13187
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          1.935
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                8046
_reflns_number_total             13187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051770ksup1.cif
_cod_data_source_block           (TBA)4(10)
_cod_original_cell_volume        10950(50)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4331877