The First Example of a Seven-Coordinate Vanadium(III) Thiolate Complex Containing the Hydrazine Molecule, an Intermediate of Nitrogen Fixation
Hua-Fen Hsu; Wei-Cheng Chu; Chen-Hsiung Hung; Ju-Hsiou Liao; Inorganic Chemistry 42 (2003) 7369–7371; doi:10.1021/ic034992w

data_4312544
_publ_contact_author_address
;
Department of Chemistry
National Cheng Kung University
Tainan 701
Taiwan
;
_publ_contact_author_email       konopka@mail.ncku.edu.tw
_publ_contact_author_fax         '886-6-2757575 ext 65336'
_publ_contact_author_name        ' Professor Hua-Fen Hsu'
_publ_contact_author_phone       886-6-2740552
_publ_section_title
;
 The First Example of a Seven-Coordinate Vanadium(III) Thiolate Complex
 Containing the Hydrazine Molecule, an Intermediate of Nitrogen Fixation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7369
_journal_page_last               7371
_journal_paper_doi               10.1021/ic034992w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C39 H72 N6 O3 P S3 Si3 V'
_chemical_formula_weight         935.39
_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                86.032(2)
_cell_angle_beta                 88.291(2)
_cell_angle_gamma                75.138(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2441(10)
_cell_length_b                   11.2607(10)
_cell_length_c                   19.5312(17)
_cell_measurement_temperature    150(2)
_cell_volume                     2384.3(4)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.1891
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15187
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.8471
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                4909
_reflns_number_total             10574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034992wsi20030821_011943_1.cif
_cod_data_source_block           c:\xray\h739\work\h739m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4312544