Synthesis, Characterization, and Reactivity of Mononuclear O,N-Chelated Vanadium(IV) and -(III) Complexes of Methyl 2-Aminocyclopent-1-ene-1-dithiocarboxylate Based Ligand: Reporting an Example of Conformational Isomerism in the Solid State
Sudeep Bhattacharyya; Suman Mukhopadhyay; Satyabrata Samanta; Timothy J. R. Weakley; Muktimoy Chaudhury; Inorganic Chemistry 41 (2002) 2433–2440; doi:10.1021/ic0108639

data_4317914
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Synthesis, Characterization, and Reactivity of Mononuclear O,N-Chelated
 Vanadium(IV) and -(III) Complexes of Methyl
 2-Aminocyclopent-1-ene-1-dithiocarboxylate Based Ligand: Reporting an
 Example of Conformational Isomerism in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2433
_journal_page_last               2440
_journal_paper_doi               10.1021/ic0108639
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C32 H38 N4 O3 S4 V '
_chemical_formula_structural     'V O (C16 H19 N2 O S2)2'
_chemical_formula_sum            'C32 H38 N4 O3 S4 V'
_chemical_formula_weight         705.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.31(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.041(1)
_cell_length_b                   6.398(1)
_cell_length_c                   22.586(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      12.0
_cell_volume                     1686.0(4)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corp., 1997)'
_computing_publication_material  'TEXSAN (Molecular Structure Corp., 1997)'
_computing_structure_refinement  'TEXSAN (Molecular Structure Corp., 1997)'
_computing_structure_solution    'TEXSAN (Molecular Structure Corp., 1997)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.05889
_diffrn_orient_matrix_UB_12      -0.00450
_diffrn_orient_matrix_UB_13      -0.03990
_diffrn_orient_matrix_UB_21      -0.06226
_diffrn_orient_matrix_UB_22      0.00247
_diffrn_orient_matrix_UB_23      0.02222
_diffrn_orient_matrix_UB_31      -0.00070
_diffrn_orient_matrix_UB_32      0.15620
_diffrn_orient_matrix_UB_33      -0.00150
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_av_sigmaI/netI    0.110
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3425
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0.40
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews, 1968'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             738.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.56
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.38
_refine_ls_goodness_of_fit_ref   1.63
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2965
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.083
_refine_ls_R_factor_gt           0.064
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I) + (0.020I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.106
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                1681
_reflns_number_total             2965
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            ic0108639_3.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
;
_cod_original_cell_volume        1686.1(4)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C32 H38 N4 O3 S4 V '
_cod_database_code               4317914