Synthesis, structure and chemistry of vanadium(iv) and vanadium(v) compounds with substituted hydrazido(1‒) and hydrazido(2‒) ligands
Davies, Sian C.; Hughes, David L.; Konkol, Martin; Richards, Raymond L.; Sanders, J. Roger; Sobota, Piotr; Journal of the Chemical Society, Dalton Transactions  (2002) 2811–; doi:10.1039/b202098j

data_7011601
_publ_section_title
;
 Synthesis, structure and chemistry of vanadium(iv) and vanadium(v)
 compounds with substituted hydrazido(1--) and hydrazido(2--) ligands
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2811
_journal_paper_doi               10.1039/b202098j
_journal_year                    2002
_chemical_formula_moiety         'C7 H17 N3 S3 V'
_chemical_formula_structural     '[V(NMeNH2)(NS3)]'
_chemical_formula_sum            'C7 H17 N3 S3 V'
_chemical_formula_weight         290.36
_chemical_name_common            'complex 1'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
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_symmetry_space_group_name_H-M   'P 21 21 21'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7299(11)
_cell_length_b                   9.736(2)
_cell_length_c                   16.638(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1252.1(4)
_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       '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           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.035
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_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1771
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            brownish-orange
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       'flat needles'
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.787
_refine_diff_density_min         -1.172
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(8)
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.163
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_refine_ls_number_parameters     132
_refine_ls_number_reflns         1288
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_obs          0.0549
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0928P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1358
_refine_ls_wR_factor_obs         0.1301
_reflns_number_observed          1136
_reflns_number_total             1288
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b202098j.txt
_cod_data_source_block           roger32
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0928P)^2^] 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^)+(0.0928P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1252.2(4)
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               7011601