Synthesis of a Molecular Mo2Fe6S9 Cluster with the Topology of the PN Cluster of Nitrogenase by Rearrangement of an Edge-Bridged Mo2Fe6S8 Double Cubane
Yugen Zhang; R. H. Holm; Journal of the American Chemical Society 125 (2003) 3910–3920; doi:10.1021/ja0214633

data_4113595
_publ_section_title
;
 Synthesis of a Molecular Mo2Fe6S9 Cluster with the Topology of the PN
 Cluster of Nitrogenase by Rearrangement of an Edge-Bridged Mo2Fe6S8
 Double Cubane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3910
_journal_page_last               3920
_journal_paper_doi               10.1021/ja0214633
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '(Et4N)4[ Tp2Mo2Fe6S8Cl4]2MeCN '
_chemical_formula_sum            'C54 H106 B2 Cl4 Fe6 Mo2 N18 S8'
_chemical_formula_weight         1954.44
_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                 94.503(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5127(14)
_cell_length_b                   14.1623(13)
_cell_length_c                   19.4281(18)
_cell_measurement_temperature    293(2)
_cell_volume                     3980.8(6)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_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      213(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26545
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         9713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+13.9980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                8308
_reflns_number_total             9713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0214633_4.cif
_cod_data_source_block           (Et4N)4[Tp2Mo2Fe6S8Cl4]2MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4113595