New Oxovanadium Bis(1,2-dithiolate) Compounds That Mimic the Hydrogen-Bonding Interactions at the Active Sites of Mononuclear Molybdenum Enzymes
J. Jon A. Cooney; Michael D. Carducci; Anne E. McElhaney; Hugh D. Selby; John H. Enemark; Inorganic Chemistry 41 (2002) 7086–7093; doi:10.1021/ic025856e

data_4319089
_publ_contact_author_address
;
     University of Arizona
     Department of Chemistry
     1306 E. University
     Tucson, AZ 85721-0041
     USA
;
_publ_contact_author_email       jenemark@u.arizona.edu
_publ_contact_author_fax         520-621-8407
_publ_contact_author_name        'John H. Enemark'
_publ_contact_author_phone       520-621-2245
_publ_section_title
;
 New Oxovanadium Bis(1,2-dithiolate) Compounds That Mimic the
 Hydrogen-Bonding Interactions at the Active Sites of Mononuclear
 Molybdenum Enzymes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7086
_journal_page_last               7093
_journal_paper_doi               10.1021/ic025856e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C14 H12 O S4 V, 2(C6 H16 N)'
_chemical_formula_sum            'C26 H44 N2 O S4 V'
_chemical_formula_weight         579.81
_chemical_name_common
'bis-triethyl ammonium salt of oxovanadium bis-4-methyl-1,2-benzenedithiolate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.480(9)
_cell_length_b                   27.749(9)
_cell_length_c                   7.847(2)
_cell_measurement_reflns_used    5652
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.3415
_cell_measurement_theta_min      2.7975
_cell_volume                     5984(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      110(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11522
_diffrn_reflns_theta_full        27.23
_diffrn_reflns_theta_max         27.23
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0.13
_diffrn_standards_interval_count 2727
_diffrn_standards_number         103
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.635038
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Bruker, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3079
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                2621
_reflns_number_total             3079
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic025856e-3_s1_2.cif
_cod_data_source_block           '[HNEt3]2[VO(tdt)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:
'_symmetry_space_group_number' data item was removed -- it should
have been renamed to '_space_group_IT_number' as specified in the
replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst',
but the replacement data item was already present in the data block
and had the same value as the '_symmetry_space_group_number' data
item.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4319089