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#$Date: 2022-07-01 09:45:35 +0300 (Fri, 01 Jul 2022) $
#$Revision: 276468 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/55/8105597.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_8105597
loop_
_publ_author_name
'Machálková, Aneta'
'Charamzová, Iva'
'Honzíček, Jan'
'Vinklárek, Jaromír'
'Císařová, Ivana'
_publ_section_title
;
 Crystal structure of oxidobis(piperidine-1-carbodithioato-κ2
 S,S′)vanadium(IV), C12H20N2OS4V
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              223
_journal_page_last               225
_journal_paper_doi               10.1515/ncrs-2018-0265
_journal_volume                  234
_journal_year                    2019
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C12 H20 N2 O S4 V'
_chemical_formula_sum            'C12 H20 N2 O S4 V'
_chemical_formula_weight         387.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                87.1010(10)
_cell_angle_beta                 82.3160(10)
_cell_angle_gamma                71.4110(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0892(2)
_cell_length_b                   8.8797(2)
_cell_length_c                   13.8486(3)
_cell_measurement_reflns_used    8541
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5583
_cell_measurement_theta_min      2.8284
_cell_volume                     818.84(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v2016.1.0.1'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'NoniusKappa+Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3755
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.578
_diffrn_reflns_theta_min         2.420
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       prism
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0324P)²+0.1903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3414
_reflns_number_total             3755
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0265_suppl.cif
_cod_data_source_block           jv
_cod_database_code               8105597
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.840
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2290(3) 0.4588(2) 0.16031(12) 0.0136(3) Uani 1 1 d . . . . .
C2 C 0.3778(3) 0.2406(2) 0.04422(13) 0.0167(4) Uani 1 1 d . . . . .
H2A H 0.439807 0.135674 0.074027 0.020 Uiso 1 1 calc R U . . .
H2B H 0.482136 0.293318 0.028912 0.020 Uiso 1 1 calc R U . . .
C3 C 0.2993(3) 0.2179(2) -0.04903(14) 0.0188(4) Uani 1 1 d . . . . .
H3A H 0.409628 0.147035 -0.093244 0.023 Uiso 1 1 calc R U . . .
H3B H 0.250277 0.321801 -0.082363 0.023 Uiso 1 1 calc R U . . .
C4 C 0.1292(3) 0.1461(2) -0.02727(15) 0.0218(4) Uani 1 1 d . . . . .
H4A H 0.076247 0.136277 -0.088477 0.026 Uiso 1 1 calc R U . . .
H4B H 0.180111 0.038559 0.001403 0.026 Uiso 1 1 calc R U . . .
C5 C -0.0379(3) 0.2519(2) 0.04369(15) 0.0208(4) Uani 1 1 d . . . . .
H5A H -0.097162 0.355873 0.012231 0.025 Uiso 1 1 calc R U . . .
H5B H -0.144755 0.202010 0.060365 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0409(3) 0.2774(2) 0.13628(14) 0.0183(4) Uani 1 1 d . . . . .
H6A H -0.067455 0.354145 0.178302 0.022 Uiso 1 1 calc R U . . .
H6B H 0.082610 0.175593 0.172544 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3656(3) 0.7371(2) 0.45494(13) 0.0157(4) Uani 1 1 d . . . . .
C8 C 0.2620(3) 0.7993(3) 0.62803(14) 0.0227(4) Uani 1 1 d . . . . .
H8A H 0.272599 0.709082 0.674268 0.027 Uiso 1 1 calc R U . . .
H8B H 0.125969 0.832947 0.607555 0.027 Uiso 1 1 calc R U . . .
C9 C 0.2928(3) 0.9358(2) 0.67804(15) 0.0228(4) Uani 1 1 d . . . . .
H9A H 0.195490 0.964245 0.737718 0.027 Uiso 1 1 calc R U . . .
H9B H 0.267610 1.029794 0.634146 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5052(3) 0.8920(2) 0.70500(14) 0.0222(4) Uani 1 1 d . . . . .
H10A H 0.524606 0.985406 0.733312 0.027 Uiso 1 1 calc R U . . .
H10B H 0.525708 0.806007 0.754635 0.027 Uiso 1 1 calc R U . . .
C11 C 0.6575(3) 0.8374(2) 0.61538(15) 0.0226(4) Uani 1 1 d . . . . .
H11A H 0.794238 0.800834 0.634988 0.027 Uiso 1 1 calc R U . . .
H11B H 0.648512 0.928064 0.569658 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6222(3) 0.7032(2) 0.56407(15) 0.0205(4) Uani 1 1 d . . . . .
H12A H 0.714844 0.677803 0.502713 0.025 Uiso 1 1 calc R U . . .
H12B H 0.650772 0.606990 0.606072 0.025 Uiso 1 1 calc R U . . .
N1 N 0.2133(2) 0.33817(18) 0.11385(11) 0.0143(3) Uani 1 1 d . . . . .
N2 N 0.4131(2) 0.74806(19) 0.54210(11) 0.0172(3) Uani 1 1 d . . . . .
O1 O 0.2133(2) 0.88143(15) 0.20516(11) 0.0251(3) Uani 1 1 d . . . . .
S1 S 0.44321(7) 0.51475(5) 0.14671(3) 0.01716(11) Uani 1 1 d . . . . .
S2 S 0.03816(7) 0.57162(5) 0.24339(3) 0.01768(11) Uani 1 1 d . . . . .
S3 S 0.54246(7) 0.67672(6) 0.35371(3) 0.01816(11) Uani 1 1 d . . . . .
S4 S 0.12117(7) 0.77960(6) 0.43065(4) 0.02207(12) Uani 1 1 d . . . . .
V1 V 0.26244(5) 0.71744(3) 0.26431(2) 0.01483(8) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 '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'
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'
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
N1 C1 S1 123.31(14) . .
N1 C1 S2 122.67(14) . .
S1 C1 S2 113.99(10) . .
N1 C2 C3 110.51(15) . .
N1 C2 H2A 109.5 . .
C3 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C3 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C2 C3 C4 110.87(16) . .
C2 C3 H3A 109.5 . .
C4 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 108.1 . .
C5 C4 C3 109.64(16) . .
C5 C4 H4A 109.7 . .
C3 C4 H4A 109.7 . .
C5 C4 H4B 109.7 . .
C3 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
C6 C5 C4 111.15(16) . .
C6 C5 H5A 109.4 . .
C4 C5 H5A 109.4 . .
C6 C5 H5B 109.4 . .
C4 C5 H5B 109.4 . .
H5A C5 H5B 108.0 . .
N1 C6 C5 111.11(15) . .
N1 C6 H6A 109.4 . .
C5 C6 H6A 109.4 . .
N1 C6 H6B 109.4 . .
C5 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
N2 C7 S4 123.15(14) . .
N2 C7 S3 123.09(14) . .
S4 C7 S3 113.75(10) . .
N2 C8 C9 110.56(16) . .
N2 C8 H8A 109.5 . .
C9 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
C8 C9 C10 111.11(17) . .
C8 C9 H9A 109.4 . .
C10 C9 H9A 109.4 . .
C8 C9 H9B 109.4 . .
C10 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
C11 C10 C9 110.31(16) . .
C11 C10 H10A 109.6 . .
C9 C10 H10A 109.6 . .
C11 C10 H10B 109.6 . .
C9 C10 H10B 109.6 . .
H10A C10 H10B 108.1 . .
C10 C11 C12 111.59(17) . .
C10 C11 H11A 109.3 . .
C12 C11 H11A 109.3 . .
C10 C11 H11B 109.3 . .
C12 C11 H11B 109.3 . .
H11A C11 H11B 108.0 . .
N2 C12 C11 110.85(16) . .
N2 C12 H12A 109.5 . .
C11 C12 H12A 109.5 . .
N2 C12 H12B 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 108.1 . .
C1 N1 C2 122.47(15) . .
C1 N1 C6 122.69(15) . .
C2 N1 C6 114.41(14) . .
C7 N2 C8 122.87(16) . .
C7 N2 C12 123.20(16) . .
C8 N2 C12 113.86(15) . .
C1 S1 V1 85.83(6) . .
C1 S2 V1 86.01(6) . .
C7 S3 V1 85.98(6) . .
C7 S4 V1 86.00(6) . .
O1 V1 S3 112.09(6) . .
O1 V1 S2 112.55(6) . .
S3 V1 S2 135.360(18) . .
O1 V1 S4 106.85(6) . .
S3 V1 S4 74.231(19) . .
S2 V1 S4 92.64(2) . .
O1 V1 S1 105.83(6) . .
S3 V1 S1 94.08(2) . .
S2 V1 S1 74.168(18) . .
S4 V1 S1 147.307(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.318(2) .
C1 S1 1.7272(18) .
C1 S2 1.7306(18) .
C2 N1 1.477(2) .
C2 C3 1.519(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.525(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.524(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.520(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 N1 1.478(2) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 N2 1.312(2) .
C7 S4 1.7274(19) .
C7 S3 1.7328(19) .
C8 N2 1.474(2) .
C8 C9 1.514(3) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.523(3) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.520(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.520(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 N2 1.477(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
O1 V1 1.5954(12) .
S1 V1 2.4086(6) .
S2 V1 2.4005(6) .
S3 V1 2.3997(6) .
S4 V1 2.4027(6) .
