#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:43:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179259 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317935.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_4317935
loop_
_publ_author_name
'Henning Nekola'
'Dongren Wang'
'Cerstin Grüning'
'Jessica Gätjens'
'Axel Behrens'
'Dieter Rehder'
_publ_contact_author
;
         'Wang Dongren'
         Institut für Anorganische und Angewandte Chemie
         Universität Hamburg
         Martin-Luther-King-Platz 6
         20146 Hamburg
         Bundesrepublik Deutschland
;
_publ_contact_author_email       wang@chemie.uni-hamburg.de
_publ_contact_author_fax         '+49 40 42838 2893'
_publ_contact_author_phone       '+49 40 42838 6084'
_publ_section_title
;
 Thiofunctional Vanadium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2379
_journal_page_last               2384
_journal_paper_doi               10.1021/ic011118z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C23 H23 Br N O S4 V'
_chemical_formula_weight         588.51
_chemical_name_systematic
;
  2,6-bis(2'-mercaptophenylthio)dimethylpyridine-vanadiumbromid(III)
;
_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                 96.8330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5001(4)
_cell_length_b                   13.9969(5)
_cell_length_c                   16.4615(5)
_cell_measurement_temperature    153(2)
_cell_volume                     2402.14(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64463
_diffrn_reflns_theta_full        32.54
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.441
_exptl_absorpt_correction_T_max  0.7924
_exptl_absorpt_correction_T_min  0.3221
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0498P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                6999
_reflns_number_total             8614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011118z_2.cif
_cod_data_source_block           vbrhn
_cod_database_code               4317935
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
Br1 Br 0.287448(14) 0.748280(10) 0.139528(8) 0.02515(5) Uani 1 1 d . . .
V1 V 0.41729(2) 0.815729(17) 0.263683(13) 0.01829(6) Uani 1 1 d . . .
S1 S 0.27261(3) 0.94192(3) 0.27652(2) 0.02339(8) Uani 1 1 d . . .
S2 S 0.29622(3) 0.72357(3) 0.35358(2) 0.02202(7) Uani 1 1 d . . .
S3 S 0.56962(3) 0.92851(3) 0.21388(2) 0.02508(8) Uani 1 1 d . . .
S4 S 0.58188(3) 0.70193(3) 0.26531(2) 0.02446(8) Uani 1 1 d . . .
N1 N 0.51392(11) 0.86276(8) 0.38020(7) 0.0192(2) Uani 1 1 d . . .
C1 C 0.17159(13) 0.89843(11) 0.34566(9) 0.0237(3) Uani 1 1 d . . .
C2 C 0.07267(15) 0.95884(13) 0.36601(10) 0.0315(3) Uani 1 1 d . . .
H2A H 0.0633 1.0210 0.3429 0.038 Uiso 1 1 calc R . .
C3 C -0.01065(16) 0.92802(15) 0.41947(12) 0.0429(5) Uani 1 1 d . . .
H3A H -0.0775 0.9691 0.4321 0.052 Uiso 1 1 calc R . .
C4 C 0.00154(17) 0.83890(16) 0.45471(12) 0.0449(5) Uani 1 1 d . . .
H4A H -0.0558 0.8192 0.4919 0.054 Uiso 1 1 calc R . .
C5 C 0.09742(16) 0.77811(14) 0.43585(11) 0.0350(4) Uani 1 1 d . . .
H5A H 0.1063 0.7164 0.4599 0.042 Uiso 1 1 calc R . .
C6 C 0.18123(13) 0.80806(11) 0.38112(9) 0.0240(3) Uani 1 1 d . . .
C7 C 0.41783(14) 0.72539(11) 0.44149(9) 0.0243(3) Uani 1 1 d . . .
H7A H 0.3753 0.7183 0.4917 0.029 Uiso 1 1 calc R . .
H7B H 0.4749 0.6696 0.4383 0.029 Uiso 1 1 calc R . .
C8 C 0.49809(13) 0.81402(10) 0.44902(8) 0.0210(3) Uani 1 1 d . . .
C9 C 0.55972(14) 0.84149(12) 0.52471(9) 0.0274(3) Uani 1 1 d . . .
H9A H 0.5466 0.8068 0.5726 0.033 Uiso 1 1 calc R . .
C10 C 0.63995(14) 0.91955(12) 0.52967(9) 0.0296(3) Uani 1 1 d . . .
H10A H 0.6836 0.9387 0.5810 0.036 Uiso 1 1 calc R . .
C11 C 0.65657(14) 0.96980(11) 0.45958(10) 0.0266(3) Uani 1 1 d . . .
H11A H 0.7115 1.0239 0.4620 0.032 Uiso 1 1 calc R . .
C12 C 0.59119(13) 0.93984(10) 0.38488(9) 0.0219(3) Uani 1 1 d . . .
C13 C 0.59902(15) 0.99666(11) 0.30852(9) 0.0273(3) Uani 1 1 d . . .
H13A H 0.6854 1.0258 0.3115 0.033 Uiso 1 1 calc R . .
H13B H 0.5358 1.0494 0.3066 0.033 Uiso 1 1 calc R . .
C14 C 0.71380(14) 0.86038(12) 0.21606(9) 0.0255(3) Uani 1 1 d . . .
C15 C 0.82220(15) 0.90585(14) 0.19315(10) 0.0341(4) Uani 1 1 d . . .
H15A H 0.8190 0.9717 0.1790 0.041 Uiso 1 1 calc R . .
C16 C 0.93451(15) 0.85448(16) 0.19115(10) 0.0403(4) Uani 1 1 d . . .
H16A H 1.0090 0.8851 0.1762 0.048 Uiso 1 1 calc R . .
C17 C 0.93781(17) 0.75871(15) 0.21094(12) 0.0409(5) Uani 1 1 d . . .
H17A H 1.0147 0.7235 0.2091 0.049 Uiso 1 1 calc R . .
C18 C 0.83041(15) 0.71343(14) 0.23347(11) 0.0350(4) Uani 1 1 d . . .
H18A H 0.8344 0.6474 0.2469 0.042 Uiso 1 1 calc R . .
C19 C 0.71530(14) 0.76399(11) 0.23672(9) 0.0252(3) Uani 1 1 d . . .
C30 C -0.3293(2) 0.50672(16) 0.4828(2) 0.0841(10) Uani 1 1 d . . .
H30A H -0.3839 0.4902 0.4315 0.101 Uiso 1 1 calc R . .
H30B H -0.3557 0.4665 0.5273 0.101 Uiso 1 1 calc R . .
C31 C -0.1936(2) 0.48829(15) 0.47328(14) 0.0511(5) Uani 1 1 d . . .
H31A H -0.1457 0.4653 0.5250 0.061 Uiso 1 1 calc R . .
H31B H -0.1853 0.4409 0.4295 0.061 Uiso 1 1 calc R . .
C32 C -0.1487(3) 0.58277(18) 0.4510(2) 0.0926(12) Uani 1 1 d . . .
H32A H -0.1490 0.5874 0.3910 0.111 Uiso 1 1 calc R . .
H32B H -0.0602 0.5939 0.4773 0.111 Uiso 1 1 calc R . .
C33 C -0.23773(18) 0.65477(13) 0.47976(12) 0.0413(4) Uani 1 1 d . . .
H33A H -0.1954 0.6898 0.5278 0.050 Uiso 1 1 calc R . .
H33B H -0.2648 0.7014 0.4358 0.050 Uiso 1 1 calc R . .
O1 O -0.34522(12) 0.60274(10) 0.50106(9) 0.0459(3) 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'
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'
Br Br -0.2901 2.4595 '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'
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
N1 V1 S4 85.95(3) . . ?
N1 V1 S1 86.09(3) . . ?
S4 V1 S1 171.605(17) . . ?
N1 V1 S2 81.13(3) . . ?
S4 V1 S2 94.043(15) . . ?
S1 V1 S2 87.350(15) . . ?
N1 V1 S3 81.09(3) . . ?
S4 V1 S3 86.111(15) . . ?
S1 V1 S3 90.033(15) . . ?
S2 V1 S3 162.164(16) . . ?
N1 V1 Br1 172.48(3) . . ?
S4 V1 Br1 94.712(12) . . ?
S1 V1 Br1 93.531(12) . . ?
S2 V1 Br1 91.341(12) . . ?
S3 V1 Br1 106.434(13) . . ?
C1 S1 V1 104.13(5) . . ?
C6 S2 C7 102.78(7) . . ?
C6 S2 V1 102.78(5) . . ?
C7 S2 V1 96.24(5) . . ?
C14 S3 C13 101.86(7) . . ?
C14 S3 V1 103.55(5) . . ?
C13 S3 V1 95.85(5) . . ?
C19 S4 V1 105.69(5) . . ?
C12 N1 C8 119.37(12) . . ?
C12 N1 V1 120.69(9) . . ?
C8 N1 V1 119.93(9) . . ?
C6 C1 C2 117.66(14) . . ?
C6 C1 S1 124.60(11) . . ?
C2 C1 S1 117.73(12) . . ?
C3 C2 C1 120.27(17) . . ?
C4 C3 C2 121.18(17) . . ?
C3 C4 C5 119.84(16) . . ?
C4 C5 C6 119.48(18) . . ?
C1 C6 C5 121.56(15) . . ?
C1 C6 S2 120.86(11) . . ?
C5 C6 S2 117.50(13) . . ?
C8 C7 S2 114.46(10) . . ?
N1 C8 C9 121.51(13) . . ?
N1 C8 C7 118.29(12) . . ?
C9 C8 C7 120.11(13) . . ?
C10 C9 C8 119.33(15) . . ?
C9 C10 C11 119.51(14) . . ?
C10 C11 C12 118.97(14) . . ?
N1 C12 C11 121.30(14) . . ?
N1 C12 C13 118.05(12) . . ?
C11 C12 C13 120.54(13) . . ?
C12 C13 S3 114.77(10) . . ?
C19 C14 C15 121.53(15) . . ?
C19 C14 S3 120.51(11) . . ?
C15 C14 S3 117.90(13) . . ?
C16 C15 C14 119.61(18) . . ?
C17 C16 C15 119.78(16) . . ?
C16 C17 C18 120.71(17) . . ?
C17 C18 C19 120.76(18) . . ?
C14 C19 C18 117.60(15) . . ?
C14 C19 S4 123.92(11) . . ?
C18 C19 S4 118.47(13) . . ?
O1 C30 C31 109.54(18) . . ?
C32 C31 C30 102.24(19) . . ?
C31 C32 C33 107.38(18) . . ?
O1 C33 C32 106.16(16) . . ?
C30 O1 C33 108.78(16) . . ?
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
Br1 V1 2.5028(3) . ?
V1 N1 2.1629(11) . ?
V1 S4 2.3480(4) . ?
V1 S1 2.3555(4) . ?
V1 S2 2.4326(4) . ?
V1 S3 2.4565(4) . ?
S1 C1 1.7546(15) . ?
S2 C6 1.7867(15) . ?
S2 C7 1.8126(15) . ?
S3 C14 1.7859(16) . ?
S3 C13 1.8217(15) . ?
S4 C19 1.7595(16) . ?
N1 C12 1.3466(18) . ?
N1 C8 1.3495(18) . ?
C1 C6 1.392(2) . ?
C1 C2 1.410(2) . ?
C2 C3 1.382(2) . ?
C3 C4 1.375(3) . ?
C4 C5 1.381(3) . ?
C5 C6 1.397(2) . ?
C7 C8 1.497(2) . ?
C8 C9 1.388(2) . ?
C9 C10 1.376(2) . ?
C10 C11 1.380(2) . ?
C11 C12 1.400(2) . ?
C12 C13 1.498(2) . ?
C14 C19 1.391(2) . ?
C14 C15 1.395(2) . ?
C15 C16 1.385(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.382(3) . ?
C18 C19 1.407(2) . ?
C30 O1 1.392(3) . ?
C30 C31 1.475(3) . ?
C31 C32 1.465(3) . ?
C32 C33 1.489(3) . ?
C33 O1 1.422(2) . ?
