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_4331880
_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 H83.5 B2 F2 Fe6 Mo2 N15.5 O9'
_chemical_formula_sum            'C43 H83.5 B2 F2 Fe6 Mo2 N15.5 O9'
_chemical_formula_weight         1708.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 109.696(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.902(2)
_cell_length_b                   17.331(3)
_cell_length_c                   16.724(3)
_cell_measurement_reflns_used    21212
_cell_measurement_temperature    193(2)
_cell_volume                     3793.7(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21212
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_correction_T_min  0.8071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1597
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.316
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       0.00012(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.198
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+15.6532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                5228
_reflns_number_total             6928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051770ksup1.cif
_cod_data_source_block           (Et4N)3(16)(MeCN)0.5(H2O)
_cod_original_cell_volume        3793.6(11)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4331880