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_4317912
_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 (C16 H19 N2 O S2 )2 (C5 H7 O2)'
_chemical_formula_sum            'C37 H45 N4 O4 S4 V'
_chemical_formula_weight         788.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                107.67(1)
_cell_angle_beta                 95.85(1)
_cell_angle_gamma                95.64(1)
_cell_formula_units_Z            2
_cell_length_a                   8.366(2)
_cell_length_b                   12.958(2)
_cell_length_c                   18.767(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.0
_cell_measurement_theta_min      12.0
_cell_volume                     1910.4(6)
_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-2\q
_diffrn_orient_matrix_UB_11      -0.01357
_diffrn_orient_matrix_UB_12      -0.07319
_diffrn_orient_matrix_UB_13      -0.03968
_diffrn_orient_matrix_UB_21      0.01462
_diffrn_orient_matrix_UB_22      0.03639
_diffrn_orient_matrix_UB_23      -0.03931
_diffrn_orient_matrix_UB_31      0.11959
_diffrn_orient_matrix_UB_32      -0.00147
_diffrn_orient_matrix_UB_33      0.00825
_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  0.028
_diffrn_reflns_av_sigmaI/netI    0.120
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7212
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.2
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             828.00
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.73
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.19
_refine_ls_goodness_of_fit_ref   1.36
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.089
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_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         0.103
_refine_ls_wR_factor_ref         0.048
_reflns_number_gt                4132
_reflns_number_total             6698
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            ic0108639_1.cif
_cod_data_source_block           3
_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        1910.4(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C37 H45 N4 O4 S4 V '
_cod_database_code               4317912