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_4500898
_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         'C16 H16 N3 O4 S V'
_chemical_formula_sum            'C16 H16 N3 O4 S V'
_chemical_formula_weight         397.32
_chemical_melting_point          441
_chemical_name_systematic
;
methoxo-(4-methoxysalicylaldehyde-4-phenylthiosemicarbazonato(2-))-
oxo-vanadium(V)

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.598(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2897(5)
_cell_length_b                   10.3757(4)
_cell_length_c                   16.3811(9)
_cell_measurement_reflns_used    3647
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.4930
_cell_measurement_theta_min      4.0712
_cell_volume                     1698.47(15)
_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_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12518
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.8793
_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            black
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.043
_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     231
_refine_ls_number_reflns         3688
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                2358
_reflns_number_total             3688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg200466b_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        1698.46(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4500898