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_4317913
_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_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           96
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      96
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.259(1)
_cell_length_b                   9.259(1)
_cell_length_c                   39.194(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      12.0
_cell_volume                     3360.1(7)
_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      297
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.06825
_diffrn_orient_matrix_UB_12      0.07883
_diffrn_orient_matrix_UB_13      -0.00664
_diffrn_orient_matrix_UB_21      -0.08269
_diffrn_orient_matrix_UB_22      0.06919
_diffrn_orient_matrix_UB_23      -0.00151
_diffrn_orient_matrix_UB_31      0.01334
_diffrn_orient_matrix_UB_32      0.02564
_diffrn_orient_matrix_UB_33      0.02459
_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  0.00
_diffrn_reflns_av_sigmaI/netI    0.090
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1812
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1476.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_details 'see above'
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.53
_refine_ls_goodness_of_fit_ref   1.56
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1812
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.008
_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         0.052
_reflns_number_gt                1537
_reflns_number_total             1812
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            ic0108639_2.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
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        3360(1)
_cod_original_sg_symbol_H-M      'P 43 21 2 '
_cod_original_formula_sum        'C32 H38 N4 O3 S4 V '
_cod_database_code               4317913