Vanadium Complexes of the N(CH2CH2S)33- and O(CH2CH2S)22- Ligands with Coligands Relevant to Nitrogen Fixation Processes
Sian C. Davies; David L. Hughes; Zofia Janas; Lucjan B. Jerzykiewicz; Raymond L. Richards; J. Roger Sanders; James E. Silverston; Piotr Sobota; Inorganic Chemistry 39 (2000) 3485–3498; doi:10.1021/ic9909476

data_4321222
_publ_section_title
;
 Vanadium Complexes of the N(CH2CH2S)33- and O(CH2CH2S)22- Ligands with
 Coligands Relevant to Nitrogen Fixation Processes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3485
_journal_page_last               3498
_journal_paper_doi               10.1021/ic9909476
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[V {N(CH2CH2S)3} (NNMePh)]'
_chemical_formula_sum            'C13 H20 N3 S3 V'
_chemical_formula_weight         365.44
_chemical_name_common            'Compound 2c'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.713(4)
_cell_length_b                   8.570(3)
_cell_length_c                   15.225(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      8.5
_cell_volume                     1624.4(8)
_computing_cell_refinement       'Kuma KM4 software 1996'
_computing_data_collection       'Kuma KM4 software 1996'
_computing_data_reduction        'Kuma KM4 software 1996'
_computing_molecular_graphics    'ORTEPII, 1976'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.775
_diffrn_measured_fraction_theta_max 0.775
_diffrn_measurement_device       'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta 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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2461
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_obs          0.0338
_refine_ls_shift/su_max          0.185
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.4775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0920
_refine_ls_wR_factor_obs         0.0884
_reflns_number_gt                2186
_reflns_number_total             2398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9909476_02.cif
_cod_data_source_block           C13H20N3S3V
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.4775P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.4775P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321222