Rearrangement of Symmetrical Dicubane Clusters into Topological Analogues of the P Cluster of Nitrogenase: Nature's Choice?
Yugen Zhang; Jing-Lin Zuo; Hong-Cai Zhou; R. H. Holm; Journal of the American Chemical Society 124 (2002) 14292–14293; doi:10.1021/ja0279702

data_4115355
_publ_section_title
;
 Rearrangement of Symmetrical Dicubane Clusters into Topological Analogues
 of the P Cluster of Nitrogenase: Nature's Choice?
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14292
_journal_page_last               14293
_journal_paper_doi               10.1021/ja0279702
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '(Et4N)4[Tp2V2Fe6S9(SH)2] '
_chemical_formula_sum            'C62 H120 B2 Fe6 N22 S11 V2'
_chemical_formula_weight         1985.06
_chemical_name_systematic
;
  tetrakis(tetraethylammonium)bis(trispyrazoloylborate)
-bis(hydrogensulfido)-mu6-sulfido-hexakis-(mu3)-sulfido
-bis(mu2)-sulfido-hexa-iron-di-vanadium acetonitrile

solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 96.441(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.981(7)
_cell_length_b                   16.858(5)
_cell_length_c                   24.753(7)
_cell_measurement_reflns_used    1006
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      2.24
_cell_volume                     9529(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20028
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+101.6325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                5269
_reflns_number_total             6236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0279702_s1_4.cif
_cod_data_source_block           (Et4N)4[Tp2V2Fe6S9(SH)2]
_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 
;
_cod_database_code               4115355