#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/43/2204343.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_2204343
loop_
_publ_author_name
'Zhang, Xian-Ming'
_publ_section_title
catena-Poly[[bis[triaqua[2,5-bis(4-pyridyl)-1,3,4-thiadiazole]cobalt(II)]]-μ₄-tetravanadato]
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1411
_journal_page_last               m1413
_journal_paper_doi               10.1107/S1600536804022111
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C12 H8 N4 S) (V2 O6) 3(H2 O)]'
_chemical_formula_moiety         'Co (C12 H8 N4 S) (V2 O6) 3(H2 O)'
_chemical_formula_sum            'C12 H14 Co N4 O9 S V2'
_chemical_formula_weight         551.14
_chemical_name_systematic
;
catena-poly[bis[cobalt(II)-2,5-bis(4-pyridyl)
-1,3,4-thiadiazole](tetravanadate)(hexahydrate)]
;
_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   'difmap (O-H) and geom (C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.313(3)
_cell_angle_beta                 91.631(3)
_cell_angle_gamma                103.402(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0562(18)
_cell_length_b                   8.2506(18)
_cell_length_c                   14.253(3)
_cell_measurement_reflns_used    86
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.5
_cell_volume                     914.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT '
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL97 '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type  'Bruker SMART Apex CCD Diffractometer'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4126
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.398
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0485P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3035
_reflns_number_total             3483
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6090.cif
_cod_data_source_block           I
_cod_database_code               2204343
_cod_database_fobs_code          2204343
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_type_symbol
Co1 0.23745(6) 0.15653(5) 0.38131(3) 0.01374(14) Uani d . 1 Co
V1 0.09244(7) -0.25405(7) 0.46779(4) 0.01310(15) Uani d . 1 V
V2 0.19563(7) -0.43253(7) 0.64109(4) 0.01500(16) Uani d . 1 V
S1 0.68596(12) -0.41363(11) 0.12653(6) 0.0197(2) Uani d . 1 S
N1 0.4249(4) 0.0801(3) 0.29940(18) 0.0148(6) Uani d . 1 N
N2 0.6583(4) -0.1980(4) 0.0162(2) 0.0224(7) Uani d . 1 N
N3 0.7116(4) -0.3198(4) -0.0381(2) 0.0217(7) Uani d . 1 N
C11 0.8823(5) -0.8395(4) -0.0293(3) 0.0232(8) Uani d . 1 C
H11A 0.9049 -0.9247 0.0066 0.080 Uiso d R 1 H
O1 0.1785(3) -0.0811(3) 0.42268(15) 0.0190(5) Uani d . 1 O
O2 -0.0650(3) -0.2329(3) 0.53529(15) 0.0199(6) Uani d . 1 O
O3 0.2475(3) -0.3182(3) 0.53858(16) 0.0186(5) Uani d . 1 O
O4 0.3511(3) -0.5304(3) 0.65283(16) 0.0204(6) Uani d . 1 O
O5 0.1903(3) -0.3036(3) 0.73515(16) 0.0218(6) Uani d . 1 O
O6 -0.0145(3) -0.5768(3) 0.62458(15) 0.0177(5) Uani d . 1 O
C1 0.5054(5) -0.0304(4) 0.3291(2) 0.0195(8) Uani d . 1 C
H1A 0.5073 -0.0423 0.3953 0.080 Uiso d R 1 H
C2 0.5852(5) -0.1293(4) 0.2702(2) 0.0191(8) Uani d . 1 C
H2A 0.6435 -0.2061 0.2947 0.080 Uiso d R 1 H
C3 0.5805(4) -0.1132(4) 0.1739(2) 0.0167(7) Uani d . 1 C
C4 0.5083(5) 0.0112(4) 0.1437(2) 0.0189(8) Uani d . 1 C
H4A 0.5122 0.0322 0.0787 0.080 Uiso d R 1 H
C5 0.4323(4) 0.1039(4) 0.2075(2) 0.0181(8) Uani d . 1 C
H5A 0.3822 0.1889 0.1857 0.080 Uiso d R 1 H
C6 0.6413(4) -0.2272(4) 0.1041(2) 0.0178(8) Uani d . 1 C
C7 0.7318(4) -0.4413(4) 0.0088(2) 0.0179(8) Uani d . 1 C
C8 0.7913(5) -0.5854(4) -0.0348(2) 0.0187(8) Uani d . 1 C
C9 0.8209(5) -0.5973(4) -0.1313(2) 0.0213(8) Uani d . 1 C
H9A 0.8015 -0.5136 -0.1693 0.080 Uiso d R 1 H
C10 0.8787(5) -0.7333(5) -0.1701(3) 0.0241(9) Uani d . 1 C
H10A 0.8966 -0.7432 -0.2365 0.080 Uiso d R 1 H
N4 0.9109(4) -0.8529(4) -0.1214(2) 0.0228(7) Uani d . 1 N
C12 0.8231(5) -0.7097(4) 0.0169(2) 0.0204(8) Uani d . 1 C
H12A 0.8037 -0.7052 0.0832 0.080 Uiso d R 1 H
O1W 0.4151(3) 0.2473(3) 0.49621(16) 0.0200(5) Uani d . 1 O
O2W 0.0464(3) 0.0856(3) 0.27223(17) 0.0247(6) Uani d . 1 O
O3W 0.2934(3) 0.3962(3) 0.33170(16) 0.0215(6) Uani d . 1 O
H3WA 0.4075 0.4462 0.3431 0.050 Uiso d R 1 H
H1WA 0.5275 0.2806 0.4877 0.050 Uiso d R 1 H
H3WB 0.2439 0.4717 0.3557 0.050 Uiso d R 1 H
H2WA 0.0523 0.0354 0.2207 0.050 Uiso d R 1 H
H2WB -0.0256 0.1544 0.2674 0.050 Uiso d R 1 H
H1WB 0.3891 0.3240 0.5440 0.050 Uiso d R 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'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 O1 2_556 . 92.51(9) n
O2 Co1 O2W 2_556 . 88.19(10) n
O1 Co1 O2W . . 91.26(10) n
O2 Co1 O1W 2_556 . 86.38(10) n
O1 Co1 O1W . . 91.95(9) n
O2W Co1 O1W . . 173.81(9) n
O2 Co1 N1 2_556 . 177.54(10) n
O1 Co1 N1 . . 87.41(10) n
O2W Co1 N1 . . 94.27(10) n
O1W Co1 N1 . . 91.16(10) n
O2 Co1 O3W 2_556 . 88.71(9) n
O1 Co1 O3W . . 177.14(9) n
O2W Co1 O3W . . 86.19(10) n
O1W Co1 O3W . . 90.71(9) n
N1 Co1 O3W . . 91.48(10) n
O1 V1 O2 . . 112.63(12) no
O1 V1 O3 . . 111.07(12) no
O2 V1 O3 . . 107.25(11) no
O1 V1 O6 . 2_546 110.37(11) no
O2 V1 O6 . 2_546 108.94(12) no
O3 V1 O6 . 2_546 106.32(11) no
O5 V2 O4 . . 110.76(13) no
O5 V2 O6 . . 106.41(12) no
O4 V2 O6 . . 112.50(12) no
O5 V2 O3 . . 110.72(12) no
O4 V2 O3 . . 104.82(11) no
O6 V2 O3 . . 111.72(11) no
C6 S1 C7 . . 86.83(17) no
C1 N1 C5 . . 117.5(3) no
C1 N1 Co1 . . 119.8(2) no
C5 N1 Co1 . . 120.3(2) no
C6 N2 N3 . . 113.1(3) no
C7 N3 N2 . . 112.7(3) no
N4 C11 C12 . . 123.6(3) no
N4 C11 H11A . . 117.9 no
C12 C11 H11A . . 118.5 no
V1 O1 Co1 . . 165.77(15) y
V1 O2 Co1 . 2_556 168.36(15) y
V1 O3 V2 . . 123.74(13) y
V1 O6 V2 2_546 . 128.55(13) y
N1 C1 C2 . . 123.9(3) no
N1 C1 H1A . . 117.9 no
C2 C1 H1A . . 118.2 no
C1 C2 C3 . . 118.1(3) no
C1 C2 H2A . . 121.2 no
C3 C2 H2A . . 120.7 no
C4 C3 C2 . . 118.1(3) no
C4 C3 C6 . . 119.6(3) no
C2 C3 C6 . . 122.2(3) no
C5 C4 C3 . . 119.5(3) no
C5 C4 H4A . . 120.3 no
C3 C4 H4A . . 120.2 no
N1 C5 C4 . . 122.5(3) no
N1 C5 H5A . . 118.7 no
C4 C5 H5A . . 118.7 no
N2 C6 C3 . . 121.7(3) no
N2 C6 S1 . . 113.7(3) no
C3 C6 S1 . . 124.5(3) no
N3 C7 C8 . . 122.4(3) no
N3 C7 S1 . . 113.7(3) no
C8 C7 S1 . . 123.9(3) no
C12 C8 C9 . . 118.5(3) no
C12 C8 C7 . . 122.3(3) no
C9 C8 C7 . . 119.1(3) no
C10 C9 C8 . . 117.8(3) no
C10 C9 H9A . . 121.1 no
C8 C9 H9A . . 121.1 no
N4 C10 C9 . . 124.4(3) no
N4 C10 H10A . . 117.6 no
C9 C10 H10A . . 118.0 no
C10 N4 C11 . . 117.0(3) no
C11 C12 C8 . . 118.6(3) no
C11 C12 H12A . . 120.9 no
C8 C12 H12A . . 120.5 no
Co1 O1W H1WA . . 121.3 no
Co1 O1W H1WB . . 118.1 no
H1WA O1W H1WB . . 107.1 no
Co1 O2W H2WA . . 127.0 no
Co1 O2W H2WB . . 116.8 no
H2WA O2W H2WB . . 109.3 no
Co1 O3W H3WA . . 109.9 no
Co1 O3W H3WB . . 119.0 no
H3WA O3W H3WB . . 103.3 no
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
Co1 O2 2_556 2.019(2) yes
Co1 O1 . 2.063(2) yes
Co1 O2W . 2.092(2) yes
Co1 O1W . 2.096(2) yes
Co1 N1 . 2.102(3) yes
Co1 O3W . 2.127(2) yes
V1 O1 . 1.643(2) no
V1 O2 . 1.643(2) no
V1 O3 . 1.792(2) no
V1 O6 2_546 1.794(2) no
V2 O5 . 1.625(2) no
V2 O4 . 1.654(2) no
V2 O6 . 1.822(2) no
V2 O3 . 1.831(2) no
S1 C6 . 1.719(4) no
S1 C7 . 1.730(3) no
N1 C1 . 1.332(4) no
N1 C5 . 1.347(4) no
N2 C6 . 1.306(4) no
N2 N3 . 1.357(4) no
N3 C7 . 1.303(4) no
C11 N4 . 1.337(5) no
C11 C12 . 1.381(5) no
C11 H11A . 0.9600 no
O2 Co1 2_556 2.019(2) no
O6 V1 2_546 1.794(2) no
C1 C2 . 1.380(5) no
C1 H1A . 0.9600 no
C2 C3 . 1.395(5) no
C2 H2A . 0.9600 no
C3 C4 . 1.391(5) no
C3 C6 . 1.466(5) no
C4 C5 . 1.372(5) no
C4 H4A . 0.9599 no
C5 H5A . 0.9601 no
C7 C8 . 1.465(5) no
C8 C12 . 1.392(5) no
C8 C9 . 1.400(5) no
C9 C10 . 1.379(5) no
C9 H9A . 0.9599 no
C10 N4 . 1.335(5) no
C10 H10A . 0.9600 no
C12 H12A . 0.9599 no
O1W H1WA . 0.8991 no
O1W H1WB . 0.9391 no
O2W H2WA . 0.8111 no
O2W H2WB . 0.9063 no
O3W H3WA . 0.9176 no
O3W H3WB . 0.8606 no
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
_geom_hbond_publ_flag
O3W H3WA O4 2_656 0.92 1.90 2.813(3) 171 yes
O1W H1WA O3 2_656 0.90 1.82 2.716(3) 172 yes
O3W H3WB O6 2_556 0.86 2.23 3.014(3) 152 yes
O2W H2WA N4 2_645 0.81 2.03 2.804(4) 160 yes
O2W H2WB O5 2_556 0.91 2.01 2.916(3) 176 yes
O1W H1WB O4 1_565 0.94 1.93 2.867(3) 173 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 Co1 N1 C1 . . -32.6(3) no
O2W Co1 N1 C1 . . -123.7(3) no
O1W Co1 N1 C1 . . 59.3(3) no
O3W Co1 N1 C1 . . 150.0(3) no
O1 Co1 N1 C5 . . 129.2(3) no
O2W Co1 N1 C5 . . 38.1(3) no
O1W Co1 N1 C5 . . -138.9(3) no
O3W Co1 N1 C5 . . -48.2(3) no
C6 N2 N3 C7 . . 1.0(4) no
O2 V1 O1 Co1 . . -6.3(6) no
O3 V1 O1 Co1 . . -126.6(6) no
O6 V1 O1 Co1 2_546 . 115.7(6) no
O2 Co1 O1 V1 2_556 . 9.7(6) no
O2W Co1 O1 V1 . . -78.5(6) no
O1W Co1 O1 V1 . . 96.2(6) no
N1 Co1 O1 V1 . . -172.7(6) no
O1 V1 O2 Co1 . 2_556 -18.0(8) no
O3 V1 O2 Co1 . 2_556 104.5(7) no
O6 V1 O2 Co1 2_546 2_556 -140.8(7) no
O1 V1 O3 V2 . . 149.75(14) no
O2 V1 O3 V2 . . 26.29(19) no
O6 V1 O3 V2 2_546 . -90.15(16) no
O5 V2 O3 V1 . . -84.03(18) no
O4 V2 O3 V1 . . 156.50(15) no
O6 V2 O3 V1 . . 34.39(19) no
O5 V2 O6 V1 . 2_546 178.61(16) no
O4 V2 O6 V1 . 2_546 -59.93(19) no
O3 V2 O6 V1 . 2_546 57.65(19) no
C5 N1 C1 C2 . . -4.6(5) no
Co1 N1 C1 C2 . . 157.7(3) no
N1 C1 C2 C3 . . -0.4(5) no
C1 C2 C3 C4 . . 5.3(5) no
C1 C2 C3 C6 . . -171.8(3) no
C2 C3 C4 C5 . . -5.3(5) no
C6 C3 C4 C5 . . 171.9(3) no
C1 N1 C5 C4 . . 4.6(5) no
Co1 N1 C5 C4 . . -157.6(3) no
C3 C4 C5 N1 . . 0.3(5) no
N3 N2 C6 C3 . . -178.3(3) no
N3 N2 C6 S1 . . -1.4(4) no
C4 C3 C6 N2 . . 12.4(5) no
C2 C3 C6 N2 . . -170.5(3) no
C4 C3 C6 S1 . . -164.1(3) no
C2 C3 C6 S1 . . 13.0(5) no
C7 S1 C6 N2 . . 1.1(3) no
C7 S1 C6 C3 . . 177.9(3) no
N2 N3 C7 C8 . . -179.0(3) no
N2 N3 C7 S1 . . -0.1(4) no
C6 S1 C7 N3 . . -0.5(3) no
C6 S1 C7 C8 . . 178.3(3) no
N3 C7 C8 C12 . . 175.9(3) no
S1 C7 C8 C12 . . -2.9(5) no
N3 C7 C8 C9 . . -2.7(5) no
S1 C7 C8 C9 . . 178.5(3) no
C12 C8 C9 C10 . . 0.6(5) no
C7 C8 C9 C10 . . 179.2(3) no
C8 C9 C10 N4 . . -1.1(6) no
C9 C10 N4 C11 . . 1.0(6) no
C12 C11 N4 C10 . . -0.4(5) no
N4 C11 C12 C8 . . -0.1(6) no
C9 C8 C12 C11 . . -0.1(5) no
C7 C8 C12 C11 . . -178.7(3) no
