Conformational Diversity of Thiosemicarbazonatovanadium(V) Complexes in the Solid State: From Polymorphism to Isostructurality
Rubčić, Mirta; Milić, Dalibor; Pavlović, Gordana; Cindrić, Marina; Crystal Growth & Design 11 (2011) 5227–; doi:10.1021/cg200466b

data_4500899
_publ_section_title
;
 Conformational Diversity of Thiosemicarbazonatovanadium(V) Complexes in
 the Solid State: From Polymorphism to Isostructurality
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5227
_journal_paper_doi               10.1021/cg200466b
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C17 H18 N3 O4 S V'
_chemical_formula_sum            'C17 H18 N3 O4 S V'
_chemical_formula_weight         411.34
_chemical_melting_point          415
_chemical_name_systematic
;
ethoxo-(4-methoxysalicylaldehyde-4-phenylthiosemicarbazonato(2-))-
oxo-vanadium(V)
;
_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-97
_cell_angle_alpha                87.323(18)
_cell_angle_beta                 86.732(15)
_cell_angle_gamma                71.447(17)
_cell_formula_units_Z            2
_cell_length_a                   7.2239(11)
_cell_length_b                   9.693(2)
_cell_length_c                   13.592(3)
_cell_measurement_reflns_used    2056
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.8248
_cell_measurement_theta_min      4.2027
_cell_volume                     900.4(3)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.Version 1.171.33.41.'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.Version 1.171.33.41.'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.Version 1.171.33.41.'
_computing_molecular_graphics
;
 ORTEP-3 for Windows, Ver. 1.08 (Farrugia, 2005), 
 MERCURY 1.4.2 (CCDC, 2006)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9134
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41. 
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5152
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2864
_reflns_number_total             5152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200466b_si_002.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_Hall     ' -P 1'
_cod_database_code               4500899