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_4321229
_publ_section_title
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 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} (NH)]'
_chemical_formula_sum            'C6 H13 N2 S3 V'
_chemical_formula_weight         260.30
_chemical_name_common            'Compound 10'
_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
_cell_angle_alpha                86.359(9)
_cell_angle_beta                 74.676(9)
_cell_angle_gamma                65.116(9)
_cell_formula_units_Z            2
_cell_length_a                   7.4103(7)
_cell_length_b                   7.6618(9)
_cell_length_c                   10.5983(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8
_cell_volume                     525.68(11)
_computing_cell_refinement       'CAD4-Express (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4-Express (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1952
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        4.67
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            'Brownish red'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       'triangular plates'
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         1841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0308
_refine_ls_shift/esd_max         -0.079
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.1145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0825
_refine_ls_wR_factor_obs         0.0734
_reflns_number_observed          1451
_reflns_number_total             1841
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9909476_09.cif
_cod_data_source_block           roger20
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.1145P] 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^)+(0.0375P)^2^+0.1145P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        525.68(10)
_cod_database_code               4321229