Borohydride, Azide, and Chloride Anions As Terminal Ligands on Fe/Mo/S Clusters. Synthesis, Structure and Characterization of [(Cl4-cat)(PPr3) MoFe3S4(X)2]2(Bu4N)4and [(Cl4-cat)(PPr3)MoFe3S4(PPr3)(X)]2(Bu4N)2(X = N3-, BH4-, Cl-) Double-Fused Cubanes. NMR Reactivity Studies of [(Cl4-cat)(PPr3) MoFe3S4(BH4)2]2(Bu4N)4
Koutmos, Markos; Georgakaki, Irene P.; Coucouvanis, Dimitri; Inorganic Chemistry 45 (2006) 3648–3656; doi:10.1021/ic052156b

data_4332088
_publ_section_title
;
 Borohydride, Azide, and Chloride Anions As Terminal Ligands on Fe/Mo/S
 Clusters. Synthesis, Structure and Characterization of [(Cl4-cat)(PPr3)
 MoFe3S4(X)2]2(Bu4N)4and [(Cl4-cat)(PPr3)MoFe3S4(PPr3)(X)]2(Bu4N)2(X =
 N3-, BH4-, Cl-) Double-Fused Cubanes. NMR Reactivity Studies of
 [(Cl4-cat)(PPr3) MoFe3S4(BH4)2]2(Bu4N)4
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3648
_journal_page_last               3656
_journal_paper_doi               10.1021/ic052156b
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C47 H86 Cl4 Fe3 Mo N4 O2 P2 S4'
_chemical_formula_weight         1334.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.866(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9468(17)
_cell_length_b                   17.381(2)
_cell_length_c                   25.858(3)
_cell_measurement_reflns_used    52697
_cell_measurement_temperature    150(2)
_cell_volume                     6235.4(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            51727
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  25.64
_exptl_absorpt_correction_T_min  2.765
_exptl_absorpt_correction_type   'SADABS V2.10'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         12770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+7.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                8882
_reflns_number_total             12770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052156bsup2.cif
_cod_data_source_block           3106p
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6235.2(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332088
_ratio_trasmission_factors       0.762080