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_4310379
_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)3[Tp2Mo2Fe6S9(SPh)2]5.5MeCN
_chemical_formula_sum            'C65 H106.5 B2 Fe6 Mo2 N20.5 S11'
_chemical_formula_weight         2076.47
_chemical_melting_point          ?
_chemical_name_systematic
;
  ?
;
_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                 91.602(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.114(3)
_cell_length_b                   17.997(3)
_cell_length_c                   27.898(4)
_cell_measurement_temperature    193(2)
_cell_volume                     9091(3)
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.1891
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark black '
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         15216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          7.135
_refine_ls_shift/su_mean         0.160
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                6591
_reflns_number_total             15216
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic030259t_04.cif
_cod_data_source_block           (Et4N)3[Tp2Mo2Fe6S9(SPh)2]5.5MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        9091(2)
_cod_original_formula_sum        'C65 H106.50 B2 Fe6 Mo2 N20.50 S11'
_cod_database_code               4310379