#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/51/2015185.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2015185
loop_
_publ_author_name
'Zhi-Yong Wu'
'Yan-Tuan Li'
'Duan-Jun Xu'
_publ_section_title
;
 Diaqua(2,2'-diamino-4,4'-bi-1,3-thiazole)oxosulfatovanadium(IV)
 tetrahydrate
;
_journal_coeditor_code           SF1012
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m463
_journal_page_last               m465
_journal_paper_doi               10.1107/S0108270105028982
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V O (S O4) (C6 H6 N4 S2) (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C6 H10 N4 O7 S3 V, 4H2 O'
_chemical_formula_sum            'C6 H18 N4 O11 S3 V'
_chemical_formula_weight         469.36
_chemical_name_systematic
;
Diaqua(2,2'-diamino-4,4'-bi-1,3-thiazole)oxosulfatovanadium tetrahydrate
;
_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
_cell_angle_alpha                102.32(3)
_cell_angle_beta                 102.61(3)
_cell_angle_gamma                110.50(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9043(16)
_cell_length_b                   10.230(2)
_cell_length_c                   12.597(3)
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.24
_cell_volume                     883.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8440
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.8286
_exptl_absorpt_correction_T_min  0.7716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.401
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0307
_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)+(0.0472P)²+0.4813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                3573
_reflns_number_total             4015
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            sf1012.cif
_cod_data_source_block           I
_cod_original_cell_volume        883.1(3)
_cod_database_code               2015185
_cod_database_fobs_code          2015185
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
V1 0.93524(4) 0.08832(3) 0.24812(3) 0.02433(9) Uani d . 1 . . V
O1 1.0989(2) 0.03140(18) 0.25991(14) 0.0380(3) Uani d . 1 . . O
O1W 0.6844(2) 0.14440(16) 0.21230(13) 0.0323(3) Uani d . 1 . . O
H1WA 0.6916 0.2060 0.1722 0.080 Uiso d . 1 . . H
H1WB 0.5802 0.0791 0.1770 0.080 Uiso d . 1 . . H
O2W 0.7848(2) -0.04916(16) 0.08169(12) 0.0328(3) Uani d . 1 . . O
H2WA 0.7393 -0.0187 0.0260 0.080 Uiso d . 1 . . H
H2WB 0.8472 -0.0976 0.0503 0.080 Uiso d . 1 . . H
S2 1.17296(7) 0.31067(5) 0.12801(4) 0.02631(11) Uani d . 1 . . S
O2 1.0403(2) 0.26338(16) 0.19537(12) 0.0319(3) Uani d . 1 . . O
O3 1.0705(2) 0.22654(19) 0.00590(13) 0.0410(4) Uani d . 1 . . O
O4 1.3387(2) 0.2814(2) 0.16737(16) 0.0494(4) Uani d . 1 . . O
O5 1.2233(3) 0.46667(18) 0.14634(17) 0.0498(4) Uani d . 1 . . O
S1 1.14155(9) 0.41820(6) 0.61634(4) 0.04024(14) Uani d . 1 . . S
N1 1.2495(3) 0.4547(2) 0.43399(17) 0.0451(5) Uani d . 1 . . N
H1A 1.2462 0.4257 0.3640 0.054 Uiso calc R 1 . . H
H1B 1.3267 0.5425 0.4775 0.054 Uiso calc R 1 . . H
N2 1.0110(2) 0.22656(18) 0.41594(14) 0.0279(3) Uani d . 1 . . N
C1 1.1357(3) 0.3641(2) 0.47481(17) 0.0314(4) Uani d . 1 . . C
C2 0.9173(3) 0.1605(2) 0.48555(17) 0.0304(4) Uani d . 1 . . C
C3 0.9702(3) 0.2461(3) 0.59469(19) 0.0395(5) Uani d . 1 . . C
H3 0.9213 0.2166 0.6506 0.047 Uiso calc R 1 . . H
S3 0.51609(9) -0.24520(6) 0.37459(5) 0.04363(15) Uani d . 1 . . S
N3 0.5707(3) -0.2831(2) 0.17027(18) 0.0478(5) Uani d . 1 . . N
H3A 0.6258 -0.2554 0.1221 0.057 Uiso calc R 1 . . H
H3B 0.4824 -0.3704 0.1505 0.057 Uiso calc R 1 . . H
N4 0.7554(2) -0.05404(18) 0.31591(14) 0.0294(3) Uani d . 1 . . N
C4 0.6221(3) -0.1906(2) 0.27541(19) 0.0334(4) Uani d . 1 . . C
C5 0.7767(3) 0.0105(2) 0.43067(17) 0.0309(4) Uani d . 1 . . C
C6 0.6616(3) -0.0762(3) 0.4755(2) 0.0398(5) Uani d . 1 . . C
H6 0.6608 -0.0486 0.5506 0.048 Uiso calc R 1 . . H
O3W 0.5463(2) 0.26994(19) 0.38688(14) 0.0441(4) Uani d . 1 . . O
H3WA 0.4670 0.2822 0.3334 0.080 Uiso d . 1 . . H
H3WB 0.6065 0.2272 0.3447 0.080 Uiso d . 1 . . H
O4W 0.3382(3) -0.0817(2) 0.07216(18) 0.0562(5) Uani d . 1 . . O
H4WA 0.3581 -0.1533 0.0361 0.080 Uiso d . 1 . . H
H4WB 0.2172 -0.1228 0.0807 0.080 Uiso d . 1 . . H
O5W 0.6417(2) 0.3216(2) 0.08582(16) 0.0461(4) Uani d . 1 . . O
H5WA 0.7380 0.4034 0.1030 0.080 Uiso d . 1 . . H
H5WB 0.5496 0.3377 0.1085 0.080 Uiso d . 1 . . H
O6W 0.9489(3) 0.5826(2) 0.14037(16) 0.0532(5) Uani d . 1 . . O
H6WA 1.0515 0.5579 0.1397 0.080 Uiso d . 1 . . H
H6WB 0.9454 0.6409 0.0958 0.080 Uiso d . 1 . . H
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_publ_flag
O1 V1 O2 102.46(8) yes
O1 V1 O2W 93.86(8) yes
O2 V1 O2W 92.05(7) ?
O1 V1 N2 101.30(8) yes
O2 V1 N2 90.89(7) ?
O2W V1 N2 163.55(6) ?
O1 V1 N4 99.21(8) yes
O2 V1 N4 157.53(6) ?
O2W V1 N4 92.40(7) ?
N2 V1 N4 79.00(7) yes
O1 V1 O1W 172.97(7) yes
O2 V1 O1W 79.66(6) yes
O2W V1 O1W 79.31(6) yes
N2 V1 O1W 85.31(7) yes
N4 V1 O1W 79.54(6) yes
V1 O1W H1WA 114.33 ?
V1 O1W H1WB 118.84 ?
H1WA O1W H1WB 101.83 ?
V1 O2W H2WA 123.03 ?
V1 O2W H2WB 113.97 ?
H2WA O2W H2WB 102.59 ?
O4 S2 O5 112.14(12) ?
O4 S2 O3 110.15(11) ?
O5 S2 O3 110.16(11) ?
O4 S2 O2 109.26(9) ?
O5 S2 O2 106.62(10) ?
O3 S2 O2 108.39(10) ?
S2 O2 V1 136.69(9) yes
C3 S1 C1 89.99(11) ?
N1 C1 N2 125.38(19) ?
N1 C1 S1 121.14(17) ?
N2 C1 S1 113.47(16) ?
C1 N1 H1A 120.0 ?
C1 N1 H1B 120.0 ?
H1A N1 H1B 120.0 ?
C1 N2 C2 110.70(17) ?
C1 N2 V1 134.48(14) ?
C2 N2 V1 114.75(13) ?
C3 C2 N2 115.33(19) ?
C3 C2 C5 128.8(2) ?
N2 C2 C5 115.84(18) ?
C2 C3 S1 110.50(17) ?
C2 C3 H3 124.8 ?
S1 C3 H3 124.8 ?
C6 S3 C4 90.01(11) ?
N4 C4 N3 125.7(2) ?
N4 C4 S3 113.51(17) ?
N3 C4 S3 120.76(16) ?
C4 N3 H3A 120.0 ?
C4 N3 H3B 120.0 ?
H3A N3 H3B 120.0 ?
C4 N4 C5 110.77(18) ?
C4 N4 V1 135.47(15) ?
C5 N4 V1 113.74(13) ?
C6 C5 N4 115.2(2) ?
C6 C5 C2 128.2(2) ?
N4 C5 C2 116.60(18) ?
C5 C6 S3 110.54(17) ?
C5 C6 H6 124.7 ?
S3 C6 H6 124.7 ?
H3WA O3W H3WB 101.60 ?
H4WA O4W H4WB 107.0 ?
H5WA O5W H5WB 109.7 ?
H6WA O6W H6WB 108.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O1 . 1.5858(16) yes
V1 O2 . 2.0113(15) yes
V1 O1W . 2.2319(15) yes
V1 O2W . 2.0662(18) yes
V1 N2 . 2.0990(19) yes
V1 N4 . 2.1170(18) yes
O1W H1WA . 0.8824 ?
O1W H1WB . 0.8062 ?
O2W H2WA . 0.8834 ?
O2W H2WB . 0.9044 ?
S2 O2 . 1.5041(14) yes
S2 O3 . 1.4716(17) yes
S2 O4 . 1.4513(17) yes
S2 O5 . 1.4548(17) yes
S1 C3 . 1.724(3) ?
S1 C1 . 1.736(2) ?
C1 N1 . 1.324(3) ?
C1 N2 . 1.329(3) ?
N1 H1A . 0.8600 ?
N1 H1B . 0.8600 ?
N2 C2 . 1.400(2) ?
C2 C3 . 1.346(3) ?
C2 C5 . 1.444(3) ?
C3 H3 . 0.9300 ?
S3 C6 . 1.720(3) ?
S3 C4 . 1.733(2) ?
C4 N4 . 1.324(3) ?
C4 N3 . 1.332(3) ?
N3 H3A . 0.8600 ?
N3 H3B . 0.8600 ?
N4 C5 . 1.401(3) ?
C5 C6 . 1.344(3) ?
C6 H6 . 0.9300 ?
O3W H3WA . 0.8769 ?
O3W H3WB . 0.9259 ?
O4W H4WA . 0.858 ?
O4W H4WB . 0.9409 ?
O5W H5WA . 0.8554 ?
O5W H5WB . 0.8905 ?
O6W H6WA . 0.931 ?
O6W H6WB . 0.9052 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A O2 . 0.86 2.24 2.942(3) 139
N1 H1B O3W 2_766 0.86 2.03 2.854(3) 161
N3 H3A O2W . 0.86 2.27 2.994(3) 141
N3 H3B O5 1_445 0.86 2.12 2.928(3) 156
O1W H1WA O5W . 0.8824 1.8510 2.714(2) 165.21
O1W H1WB O4W . 0.8062 1.969 2.769(3) 172.05
O2W H2WA O4W 2_655 0.8834 1.900 2.773(3) 169.25
O2W H2WB O3 2_755 0.9044 1.7515 2.640(2) 166.68
O3W H3WA O4 1_455 0.8769 2.1127 2.940(3) 157.02
O3W H3WB O1W . 0.9259 2.0221 2.916(2) 161.77
O4W H4WA O5W 2_655 0.858 2.049 2.887(3) 165.10
O4W H4WB O3 2_655 0.9409 2.0543 2.870(3) 144.08
O5W H5WA O6W . 0.8554 1.873 2.729(3) 179.93
O5W H5WB O4 1_455 0.8905 1.9261 2.743(2) 151.69
O6W H6WA O5 . 0.931 1.8957 2.808(3) 165.90
O6W H6WB O3 2_765 0.9052 2.0704 2.975(3) 178.28
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
O3 S2 O2 V1 75.40(15) yes
O4 S2 O2 V1 -44.64(17) yes
O5 S2 O2 V1 -166.03(14) yes
