#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/05/2230527.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_2230527
loop_
_publ_author_name
'Wang, Yan-Li'
'Chang, Guang-Jun'
'Liu, Bing-Xin'
_publ_section_title
;
 Aqua(2,2'-diamino-4,4'-bi-1,3-thiazole-κ²N³,N^3'^)(thiodiacetato-κ³O,S,O')nickel(II)
 monohydrate
;
_journal_coeditor_code           XU5191
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m681
_journal_paper_doi               10.1107/S1600536811015157
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Ni (C4 H4 O4 S) (C6 H6 N4 S2) (H2 O)], H2 O'
_chemical_formula_moiety         'C10 H12 N4 Ni O5 S3, H2 O'
_chemical_formula_sum            'C10 H14 N4 Ni O6 S3'
_chemical_formula_weight         441.14
_chemical_name_systematic
;
Aqua(2,2'-diamino-4,4'-bi-1,3-thiazole-
κ²N³,N^3'^)(thiodiacetato-
κ³O,S,O')nickel(II) monohydrate
;
_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                 114.622(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.856(4)
_cell_length_b                   12.197(4)
_cell_length_c                   12.507(4)
_cell_measurement_reflns_used    2650
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1644.2(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8263
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.597
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0221
_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)+(0.0349P)²+0.4782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                2627
_reflns_number_total             2888
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5191.cif
_cod_data_source_block           I
_cod_original_cell_volume        1644.3(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230527
_cod_database_fobs_code          2230527
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_type_symbol
_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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.70472(2) 0.163736(19) 0.32141(2) 0.02339(9) Uani d . 1 1 . .
O O21 0.74187(13) 0.28151(11) 0.21850(12) 0.0346(3) Uani d . 1 1 . .
O O22 0.73617(12) 0.45346(12) 0.16017(12) 0.0365(3) Uani d . 1 1 . .
O O23 0.53565(12) 0.13917(11) 0.18614(12) 0.0328(3) Uani d . 1 1 . .
O O24 0.37049(13) 0.21909(12) 0.04991(12) 0.0422(4) Uani d . 1 1 . .
O O1 0.64613(13) 0.06045(11) 0.42019(12) 0.0353(3) Uani d . 1 1 . .
H H1A 0.5731 0.0782 0.4093 0.053 Uiso d R 1 1 . .
H H1B 0.6862 0.0612 0.4894 0.053 Uiso d R 1 1 . .
N N11 0.79168(13) 0.04751(12) 0.26220(13) 0.0244(3) Uani d . 1 1 . .
N N12 0.63575(15) -0.03738(15) 0.09932(14) 0.0364(4) Uani d . 1 1 . .
H H12A 0.6217 -0.0852 0.0508 0.044 Uiso d R 1 1 . .
H H12B 0.5822 0.0034 0.1111 0.044 Uiso d R 1 1 . .
N N13 0.88791(14) 0.17581(12) 0.45192(13) 0.0258(3) Uani d . 1 1 . .
N N14 0.88728(17) 0.30143(15) 0.59448(16) 0.0419(4) Uani d . 1 1 . .
H H14A 0.8266 0.2753 0.6018 0.050 Uiso d R 1 1 . .
H H14B 0.9332 0.3406 0.6512 0.050 Uiso d R 1 1 . .
S S11 0.87354(5) -0.09125(4) 0.15646(5) 0.03800(14) Uani d . 1 1 . .
S S12 1.10452(5) 0.24840(5) 0.58486(5) 0.03957(14) Uani d . 1 1 . .
S S21 0.60333(4) 0.32092(4) 0.36574(4) 0.02772(12) Uani d . 1 1 . .
O O1W 0.41649(16) 0.13394(15) 0.39419(16) 0.0567(5) Uani d . 1 1 . .
H H1WA 0.4000 0.1775 0.4391 0.085 Uiso d R 1 1 . .
H H1WB 0.3648 0.0823 0.3752 0.085 Uiso d R 1 1 . .
C C11 0.75308(18) -0.02181(15) 0.17266(16) 0.0271(4) Uani d . 1 1 . .
C C12 0.97924(18) -0.02114(17) 0.27670(17) 0.0340(5) Uani d . 1 1 . .
H H12 1.0649 -0.0297 0.3071 0.041 Uiso calc R 1 1 . .
C C13 0.91989(16) 0.04749(15) 0.31994(16) 0.0260(4) Uani d . 1 1 . .
C C14 0.97254(16) 0.12436(16) 0.41806(16) 0.0258(4) Uani d . 1 1 . .
C C15 1.09151(19) 0.15449(17) 0.47761(19) 0.0357(5) Uani d . 1 1 . .
H H15 1.1574 0.1284 0.4630 0.043 Uiso calc R 1 1 . .
C C16 0.94546(18) 0.24140(16) 0.54155(16) 0.0297(4) Uani d . 1 1 . .
C C21 0.72366(16) 0.38186(16) 0.22579(16) 0.0283(4) Uani d . 1 1 . .
C C22 0.68729(19) 0.42159(17) 0.32255(18) 0.0351(5) Uani d . 1 1 . .
H H22A 0.6365 0.4868 0.2955 0.042 Uiso calc R 1 1 . .
H H22B 0.7618 0.4418 0.3908 0.042 Uiso calc R 1 1 . .
C C23 0.45736(17) 0.21590(16) 0.14957(16) 0.0281(4) Uani d . 1 1 . .
C C24 0.46281(18) 0.31021(17) 0.23123(18) 0.0331(4) Uani d . 1 1 . .
H H24A 0.3931 0.3032 0.2522 0.040 Uiso calc R 1 1 . .
H H24B 0.4521 0.3782 0.1879 0.040 Uiso calc R 1 1 . .
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'
Ni Ni 0.3393 1.1124 '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'
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
O23 Ni N11 . . 93.83(6) ?
O23 Ni O1 . . 86.99(6) ?
N11 Ni O1 . . 97.92(6) ?
O23 Ni O21 . . 88.66(6) ?
N11 Ni O21 . . 89.21(6) ?
O1 Ni O21 . . 171.88(5) ?
O23 Ni N13 . . 173.36(6) ?
N11 Ni N13 . . 79.53(6) ?
O1 Ni N13 . . 94.23(6) ?
O21 Ni N13 . . 90.88(6) ?
O23 Ni S21 . . 84.09(4) ?
N11 Ni S21 . . 170.43(4) ?
O1 Ni S21 . . 91.31(4) ?
O21 Ni S21 . . 81.42(4) ?
N13 Ni S21 . . 102.40(5) ?
C21 O21 Ni . . 122.59(12) ?
C23 O23 Ni . . 120.86(12) ?
Ni O1 H1A . . 108.8 ?
Ni O1 H1B . . 116.4 ?
H1A O1 H1B . . 106.3 ?
C11 N11 C13 . . 111.02(15) ?
C11 N11 Ni . . 133.97(12) ?
C13 N11 Ni . . 114.65(12) ?
C11 N12 H12A . . 116.9 ?
C11 N12 H12B . . 115.7 ?
H12A N12 H12B . . 127.3 ?
C16 N13 C14 . . 110.52(16) ?
C16 N13 Ni . . 134.78(13) ?
C14 N13 Ni . . 111.95(12) ?
C16 N14 H14A . . 119.4 ?
C16 N14 H14B . . 115.9 ?
H14A N14 H14B . . 114.5 ?
C12 S11 C11 . . 89.46(9) ?
C15 S12 C16 . . 89.49(10) ?
C22 S21 C24 . . 100.37(10) ?
C22 S21 Ni . . 94.66(7) ?
C24 S21 Ni . . 94.68(7) ?
H1WA O1W H1WB . . 108.2 ?
N12 C11 N11 . . 124.86(17) ?
N12 C11 S11 . . 121.70(15) ?
N11 C11 S11 . . 113.42(14) ?
C13 C12 S11 . . 110.28(15) ?
C13 C12 H12 . . 124.9 ?
S11 C12 H12 . . 124.9 ?
C12 C13 N11 . . 115.81(17) ?
C12 C13 C14 . . 128.72(17) ?
N11 C13 C14 . . 115.46(15) ?
C15 C14 N13 . . 115.59(18) ?
C15 C14 C13 . . 128.58(18) ?
N13 C14 C13 . . 115.80(15) ?
C14 C15 S12 . . 110.29(16) ?
C14 C15 H15 . . 124.9 ?
S12 C15 H15 . . 124.9 ?
N13 C16 N14 . . 123.90(18) ?
N13 C16 S12 . . 114.04(14) ?
N14 C16 S12 . . 122.03(15) ?
O22 C21 O21 . . 124.33(18) ?
O22 C21 C22 . . 116.75(18) ?
O21 C21 C22 . . 118.89(17) ?
C21 C22 S21 . . 113.36(14) ?
C21 C22 H22A . . 108.9 ?
S21 C22 H22A . . 108.9 ?
C21 C22 H22B . . 108.9 ?
S21 C22 H22B . . 108.9 ?
H22A C22 H22B . . 107.7 ?
O24 C23 O23 . . 124.30(18) ?
O24 C23 C24 . . 115.78(17) ?
O23 C23 C24 . . 119.87(16) ?
C23 C24 S21 . . 116.29(13) ?
C23 C24 H24A . . 108.2 ?
S21 C24 H24A . . 108.2 ?
C23 C24 H24B . . 108.2 ?
S21 C24 H24B . . 108.2 ?
H24A C24 H24B . . 107.4 ?
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
Ni O1 . 2.0763(14) y
Ni O21 . 2.0944(14) y
Ni O23 . 2.0357(14) y
Ni N11 . 2.0634(15) y
Ni N13 . 2.1094(16) y
Ni S21 . 2.4461(7) y
O21 C21 . 1.253(2) ?
O22 C21 . 1.249(2) ?
O23 C23 . 1.262(2) ?
O24 C23 . 1.244(2) ?
O1 H1A . 0.8465 ?
O1 H1B . 0.7947 ?
N11 C11 . 1.323(2) ?
N11 C13 . 1.385(2) ?
N12 C11 . 1.323(2) ?
N12 H12A . 0.8078 ?
N12 H12B . 0.8657 ?
N13 C16 . 1.313(2) ?
N13 C14 . 1.391(2) ?
N14 C16 . 1.353(3) ?
N14 H14A . 0.8259 ?
N14 H14B . 0.8401 ?
S11 C12 . 1.730(2) ?
S11 C11 . 1.7434(19) ?
S12 C15 . 1.721(2) ?
S12 C16 . 1.734(2) ?
S21 C22 . 1.800(2) ?
S21 C24 . 1.813(2) ?
O1W H1WA . 0.8530 ?
O1W H1WB . 0.8413 ?
C12 C13 . 1.344(3) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.462(3) ?
C14 C15 . 1.343(3) ?
C15 H15 . 0.9300 ?
C21 C22 . 1.523(3) ?
C22 H22A . 0.9700 ?
C22 H22B . 0.9700 ?
C23 C24 . 1.522(3) ?
C24 H24A . 0.9700 ?
C24 H24B . 0.9700 ?
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
O1 H1A O1W . 0.85 1.91 2.7540 173 y
O1 H1B O22 4_566 0.79 1.97 2.7399 162 y
N12 H12A O24 3_655 0.81 2.09 2.8785 166 y
N12 H12B O23 . 0.87 2.09 2.8807 152 y
N14 H14A O21 4_566 0.83 2.20 2.9378 149 y
O1W H1WA O24 4_566 0.85 2.01 2.8616 177 y
O1W H1WB O22 2_645 0.84 1.91 2.7493 173 y
