Structural Conversions of Molybdenum-Iron-Sulfur Edge-Bridged Double Cubanes and PN-Type Clusters Topologically Related to the Nitrogenase P-Cluster
Yugen Zhang; R. H. Holm; Inorganic Chemistry 43 (2004) 674–682; doi:10.1021/ic030259t

data_4310380
_publ_section_title
;
 Structural Conversions of Molybdenum-Iron-Sulfur Edge-Bridged Double
 Cubanes and PN-Type Clusters Topologically Related to the Nitrogenase
 P-Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              674
_journal_page_last               682
_journal_paper_doi               10.1021/ic030259t
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         (Et4N)2.75[Tp2Mo2Fe6S8.75(SEt)2.25]2.5MeCN
_chemical_formula_sum            'C48.5 H93.75 B2 Fe6 Mo2 N18 S11'
_chemical_formula_weight         1812.97
_chemical_melting_point          ?
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.331(5)
_cell_angle_beta                 78.884(5)
_cell_angle_gamma                64.905(5)
_cell_formula_units_Z            2
_cell_length_a                   14.938(4)
_cell_length_b                   17.094(4)
_cell_length_c                   18.600(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4191.8(19)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23553
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    1.614
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'Dark green '
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1926
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         14667
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.818
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                8652
_reflns_number_total             14667
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic030259t_05.cif
_cod_data_source_block           (Et4N)2.75[Tp2Mo2Fe6S8.75(SEt)2.25]2.5MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value ' not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4191.6(18)
_cod_original_formula_sum        'C48.50 H93.75 B2 Fe6 Mo2 N18 S11'
_cod_database_code               4310380