#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:41:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179731 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/27/7002744.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002744
loop_
_publ_author_name
'Rubčić, Mirta'
'Milić, Dalibor'
'Horvat, Gordan'
'Đilović, Ivica'
'Galić, Nives'
'Tomišić, Vladislav'
'Cindrić, Marina'
_publ_section_title
;
 Vanadium-induced formation of thiadiazole and thiazoline compounds.
 Mononuclear and dinuclear oxovanadium(v) complexes with open-chain and
 cyclized thiosemicarbazone ligands
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9914
_journal_page_last               9923
_journal_paper_doi               10.1039/b913653c
_journal_year                    2009
_chemical_formula_moiety         'C17 H18 N3 O3 S V'
_chemical_formula_sum            'C17 H18 N3 O3 S V'
_chemical_formula_weight         395.34
_chemical_name_common
;Oxo-propoxo-(salicylaldehyde 4-phenylthiosemicarbazonato(2-
))vanadium(V)
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 114.404(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1837(4)
_cell_length_b                   8.0325(2)
_cell_length_c                   16.0582(5)
_cell_measurement_reflns_used    5529
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.9725
_cell_measurement_theta_min      3.7597
_cell_volume                     1783.52(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       'ω and φ 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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9284
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0299
_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/[σ²(Fo²)+(0.0504P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                2455
_reflns_number_total             3124
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b913653c.txt
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002744
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.30989(14) 0.2087(2) 0.01051(12) 0.0188(4) Uani 1 1 d . . .
C2 C 0.38969(14) 0.1990(2) -0.01160(12) 0.0185(4) Uani 1 1 d . . .
C3 C 0.38746(15) 0.0841(2) -0.07861(13) 0.0224(5) Uani 1 1 d . . .
H3 H 0.4409 0.0773 -0.0948 0.027 Uiso 1 1 calc R . .
C4 C 0.30900(16) -0.0185(3) -0.12093(14) 0.0258(5) Uani 1 1 d . . .
H4 H 0.3080 -0.0951 -0.1664 0.031 Uiso 1 1 calc R . .
C5 C 0.23128(16) -0.0093(3) -0.09667(14) 0.0275(5) Uani 1 1 d . . .
H5 H 0.1776 -0.0816 -0.1250 0.033 Uiso 1 1 calc R . .
C6 C 0.23096(14) 0.1039(2) -0.03177(13) 0.0230(5) Uani 1 1 d . . .
H6 H 0.1771 0.1099 -0.0162 0.028 Uiso 1 1 calc R . .
C7 C 0.47630(14) 0.2931(2) 0.03662(12) 0.0168(4) Uani 1 1 d . A .
H7 H 0.5311 0.2676 0.0247 0.020 Uiso 1 1 calc R . .
C8 C 0.59027(14) 0.5717(2) 0.20482(13) 0.0169(4) Uani 1 1 d . A .
C9 C 0.76590(14) 0.6333(2) 0.24702(13) 0.0199(4) Uani 1 1 d . . .
C10 C 0.78007(15) 0.5408(3) 0.18004(13) 0.0220(5) Uani 1 1 d . . .
H10 H 0.7288 0.4763 0.1374 0.026 Uiso 1 1 calc R . .
C11 C 0.86986(15) 0.5441(3) 0.17635(14) 0.0278(5) Uani 1 1 d . . .
H11 H 0.8794 0.4816 0.1305 0.033 Uiso 1 1 calc R . .
C12 C 0.94545(16) 0.6361(3) 0.23770(15) 0.0356(6) Uani 1 1 d . . .
H12 H 1.0064 0.6375 0.2343 0.043 Uiso 1 1 calc R . .
C13 C 0.93109(16) 0.7263(3) 0.30425(15) 0.0360(6) Uani 1 1 d . . .
H13 H 0.9828 0.7898 0.3470 0.043 Uiso 1 1 calc R . .
C14 C 0.84270(15) 0.7253(3) 0.30944(14) 0.0281(5) Uani 1 1 d . . .
H14 H 0.8341 0.7877 0.3558 0.034 Uiso 1 1 calc R . .
O1 O 0.34183(10) 0.64576(16) 0.02440(9) 0.0226(3) Uani 1 1 d . . .
O2 O 0.30889(9) 0.31796(16) 0.07424(8) 0.0193(3) Uani 1 1 d . . .
O3 O 0.29124(9) 0.59627(16) 0.16236(9) 0.0212(3) Uani 1 1 d D . .
C15A C 0.2256(3) 0.7333(7) 0.1415(11) 0.030(3) Uani 0.557(5) 1 d PDU A 1
H15A H 0.2371 0.8101 0.0988 0.036 Uiso 0.557(5) 1 calc PR A 1
H15B H 0.2365 0.7953 0.1982 0.036 Uiso 0.557(5) 1 calc PR A 1
C16A C 0.1238(3) 0.6711(6) 0.0989(4) 0.0316(13) Uani 0.557(5) 1 d PDU A 1
H16A H 0.1129 0.5949 0.1422 0.038 Uiso 0.557(5) 1 calc PR A 1
H16B H 0.1142 0.6067 0.0432 0.038 Uiso 0.557(5) 1 calc PR A 1
C17A C 0.0504(3) 0.8109(5) 0.0737(3) 0.0384(13) Uani 0.557(5) 1 d PDU A 1
H17A H -0.0150 0.7640 0.0492 0.058 Uiso 0.557(5) 1 calc PR A 1
H17B H 0.0577 0.8820 0.0273 0.058 Uiso 0.557(5) 1 calc PR A 1
H17C H 0.0610 0.8773 0.1282 0.058 Uiso 0.557(5) 1 calc PR A 1
C15B C 0.2433(5) 0.7509(7) 0.1587(14) 0.018(2) Uani 0.443(5) 1 d PDU A 2
H15C H 0.2437 0.8187 0.1074 0.022 Uiso 0.443(5) 1 calc PR A 2
H15D H 0.2783 0.8134 0.2161 0.022 Uiso 0.443(5) 1 calc PR A 2
C16B C 0.1412(4) 0.7221(8) 0.1460(4) 0.0273(15) Uani 0.443(5) 1 d PDU A 2
H16C H 0.1144 0.8273 0.1579 0.033 Uiso 0.443(5) 1 calc PR A 2
H16D H 0.1406 0.6387 0.1911 0.033 Uiso 0.443(5) 1 calc PR A 2
C17B C 0.0776(5) 0.6618(9) 0.0509(4) 0.045(2) Uani 0.443(5) 1 d PDU A 2
H17D H 0.0115 0.6461 0.0455 0.068 Uiso 0.443(5) 1 calc PR A 2
H17E H 0.1026 0.5558 0.0394 0.068 Uiso 0.443(5) 1 calc PR A 2
H17F H 0.0775 0.7445 0.0059 0.068 Uiso 0.443(5) 1 calc PR A 2
N1 N 0.48573(11) 0.41090(19) 0.09552(10) 0.0165(4) Uani 1 1 d . . .
N2 N 0.58047(11) 0.46724(19) 0.14006(10) 0.0177(4) Uani 1 1 d . A .
N3 N 0.67811(11) 0.6414(2) 0.25654(11) 0.0200(4) Uani 1 1 d . . .
H3N H 0.6800 0.7009 0.3033 0.024 Uiso 1 1 calc R . .
S1 S 0.49597(4) 0.63256(6) 0.23461(3) 0.02130(14) Uani 1 1 d . . .
V1 V 0.36511(2) 0.52611(4) 0.10910(2) 0.01714(12) Uani 1 1 d . A .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 C6 119.03(17) . . ?
O2 C1 C2 120.66(17) . . ?
C6 C1 C2 120.30(18) . . ?
C1 C2 C3 118.76(18) . . ?
C1 C2 C7 122.04(17) . . ?
C3 C2 C7 119.03(17) . . ?
C4 C3 C2 120.86(19) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.50(19) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.91(19) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 119.65(19) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
N1 C7 C2 125.14(17) . . ?
N1 C7 H7 117.4 . . ?
C2 C7 H7 117.4 . . ?
N2 C8 N3 120.83(17) . . ?
N2 C8 S1 124.23(15) . . ?
N3 C8 S1 114.93(14) . . ?
C14 C9 C10 119.14(19) . . ?
C14 C9 N3 116.50(17) . . ?
C10 C9 N3 124.36(18) . . ?
C11 C10 C9 119.3(2) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C10 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 118.9(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 120.9(2) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.34(19) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
C15A O3 V1 130.9(7) . . ?
C15B O3 V1 132.4(7) . . ?
O3 C15A C16A 109.8(4) . . ?
O3 C15A H15A 109.7 . . ?
C16A C15A H15A 109.7 . . ?
O3 C15A H15B 109.7 . . ?
C16A C15A H15B 109.7 . . ?
H15A C15A H15B 108.2 . . ?
C15A C16A C17A 112.5(4) . . ?
C15A C16A H16A 109.1 . . ?
C17A C16A H16A 109.1 . . ?
C15A C16A H16B 109.1 . . ?
C17A C16A H16B 109.1 . . ?
H16A C16A H16B 107.8 . . ?
C16A C17A H17A 109.5 . . ?
C16A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
C16A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
O3 C15B C16B 110.7(5) . . ?
O3 C15B H15C 109.5 . . ?
C16B C15B H15C 109.5 . . ?
O3 C15B H15D 109.5 . . ?
C16B C15B H15D 109.5 . . ?
H15C C15B H15D 108.1 . . ?
C15B C16B C17B 112.4(8) . . ?
C15B C16B H16C 109.1 . . ?
C17B C16B H16C 109.1 . . ?
C15B C16B H16D 109.1 . . ?
C17B C16B H16D 109.1 . . ?
H16C C16B H16D 107.9 . . ?
C16B C17B H17D 109.5 . . ?
C16B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
C16B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C7 N1 N2 112.92(15) . . ?
C7 N1 V1 123.05(13) . . ?
N2 N1 V1 123.58(12) . . ?
C8 N2 N1 112.00(15) . . ?
C8 N3 C9 130.29(16) . . ?
C8 N3 H3N 114.9 . . ?
C9 N3 H3N 114.9 . . ?
C8 S1 V1 99.33(7) . . ?
O1 V1 O3 105.21(6) . . ?
O1 V1 O2 112.12(6) . . ?
O3 V1 O2 97.41(6) . . ?
O1 V1 N1 94.11(6) . . ?
O3 V1 N1 158.57(6) . . ?
O2 V1 N1 83.46(6) . . ?
O1 V1 S1 109.18(5) . . ?
O3 V1 S1 87.08(5) . . ?
O2 V1 S1 135.49(4) . . ?
N1 V1 S1 77.72(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.353(2) . ?
C1 C6 1.390(3) . ?
C1 C2 1.398(2) . ?
C2 C3 1.407(3) . ?
C2 C7 1.435(3) . ?
C3 C4 1.375(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N1 1.303(2) . ?
C7 H7 0.9500 . ?
C8 N2 1.296(2) . ?
C8 N3 1.366(2) . ?
C8 S1 1.7561(18) . ?
C9 C14 1.395(3) . ?
C9 C10 1.395(3) . ?
C9 N3 1.405(2) . ?
C10 C11 1.389(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
O1 V1 1.5816(13) . ?
O2 V1 1.8555(13) . ?
O3 C15A 1.428(4) . ?
O3 C15B 1.429(4) . ?
O3 V1 1.7606(12) . ?
C15A C16A 1.494(4) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A C17A 1.515(4) . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C15B C16B 1.494(5) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C16B C17B 1.510(4) . ?
C16B H16C 0.9900 . ?
C16B H16D 0.9900 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
N1 N2 1.391(2) . ?
N1 V1 2.1420(15) . ?
N3 H3N 0.8800 . ?
S1 V1 2.3306(6) . ?
