Borohydride Anions as Terminal Ligands on a Fe/Mo/S Cluster. Synthesis, Structure, and Characterization of the [(Cl4-cat)(PPr3)MoFe3S4(BH4)2]2(Bu4N)4 Double-Fused Cubane
Markos Koutmos; Dimitri Coucouvanis; Inorganic Chemistry 43 (2004) 6508–6510; doi:10.1021/ic049275w

data_4311759
_publ_section_title
;
 Borohydride Anions as Terminal Ligands on a Fe/Mo/S Cluster. Synthesis,
 Structure, and Characterization of the
 [(Cl4-cat)(PPr3)MoFe3S4(BH4)2]2(Bu4N)4 Double-Fused Cubane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6508
_journal_page_last               6510
_journal_paper_doi               10.1021/ic049275w
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C94 H202 B4 Cl8 Fe6 Mo2 N4 O4 P2 S8'
_chemical_formula_weight         2624.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.387(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.1420(19)
_cell_length_b                   22.604(3)
_cell_length_c                   17.2955(18)
_cell_measurement_reflns_used    83965
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.993
_cell_measurement_theta_min      2.986
_cell_volume                     6281.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82811
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_type   'SADABS V2.10'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         15651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.345
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+4.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                12463
_reflns_number_total             15651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049275wsi20040816_025315.cif
_cod_data_source_block           4164p
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6282.0(12)
_cod_database_code               4311759
_ratio_trasmission_factors       0.883698