#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/02/2230256.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_2230256
loop_
_publ_author_name
'Wang, Jing-Yi'
'Wang, Xiu-Guang'
'Zhao, Xiao-Jun'
_publ_section_title
;
 Tetraaquabis[2-(4-pyridylsulfanyl)acetato-κN]nickel(II)
;
_journal_coeditor_code           BT5549
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m795
_journal_paper_doi               10.1107/S1600536811019131
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C7 H6 N O2 S)2 (H2 O)4]'
_chemical_formula_moiety         'C14 H20 N2 Ni O8 S2'
_chemical_formula_sum            'C14 H20 N2 Ni O8 S2'
_chemical_formula_weight         467.15
_chemical_name_systematic
;
Tetraaquabis[2-(4-pyridylsulfanyl)acetato-κN]nickel(II)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.7130(10)
_cell_angle_beta                 103.4400(10)
_cell_angle_gamma                115.1200(10)
_cell_formula_units_Z            1
_cell_length_a                   6.3577(4)
_cell_length_b                   7.0330(5)
_cell_length_c                   11.7624(8)
_cell_measurement_reflns_used    2208
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      3.24
_cell_volume                     456.75(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Berndt,
1999)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD 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  0.0082
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2358
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.8349
_exptl_absorpt_correction_T_min  0.7575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             242
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0224
_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)+(0.0331P)²+0.2312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                1525
_reflns_number_total             1610
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt5549.cif
_cod_data_source_block           I
_cod_database_code               2230256
_cod_database_fobs_code          2230256
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 Ni1 0.0000 0.0000 0.0000 0.02365(11) Uani d S 1 2 . .
S S1 0.72786(9) 0.33945(8) 0.54727(4) 0.03489(14) Uani d . 1 1 . .
O O1 0.5787(3) 0.2690(3) 0.84929(12) 0.0430(4) Uani d . 1 1 . .
O O2 0.9194(3) 0.4387(2) 0.79704(12) 0.0423(4) Uani d . 1 1 . .
O O3 0.2259(2) 0.2716(2) -0.05684(11) 0.0347(3) Uani d . 1 1 . .
H H3A 0.1377 0.3317 -0.0833 0.052 Uiso d R 1 1 . .
H H3B 0.3544 0.3065 -0.0783 0.052 Uiso d R 1 1 . .
O O4 0.1770(2) -0.1742(2) -0.03636(11) 0.0302(3) Uani d . 1 1 . .
H H4A 0.2585 -0.1876 0.0284 0.045 Uiso d R 1 1 . .
H H4B 0.0891 -0.2861 -0.0878 0.045 Uiso d R 1 1 . .
N N1 0.2203(3) 0.1150(2) 0.17292(13) 0.0275(3) Uani d . 1 1 . .
C C1 0.5198(3) 0.2521(3) 0.40628(15) 0.0268(4) Uani d . 1 1 . .
C C2 0.2691(3) 0.1584(3) 0.38241(16) 0.0307(4) Uani d . 1 1 . .
H H2 0.1970 0.1401 0.4440 0.037 Uiso calc R 1 1 . .
C C3 0.1292(3) 0.0933(3) 0.26627(16) 0.0315(4) Uani d . 1 1 . .
H H3 -0.0381 0.0307 0.2517 0.038 Uiso calc R 1 1 . .
C C4 0.4625(3) 0.2085(3) 0.19676(16) 0.0313(4) Uani d . 1 1 . .
H H4 0.5298 0.2269 0.1334 0.038 Uiso calc R 1 1 . .
C C5 0.6160(3) 0.2784(3) 0.30962(16) 0.0312(4) Uani d . 1 1 . .
H H5 0.7827 0.3427 0.3216 0.037 Uiso calc R 1 1 . .
C C6 0.5391(3) 0.2753(3) 0.64667(15) 0.0301(4) Uani d . 1 1 . .
H H6A 0.4421 0.3520 0.6348 0.036 Uiso calc R 1 1 . .
H H6B 0.4304 0.1240 0.6296 0.036 Uiso calc R 1 1 . .
C C7 0.6951(3) 0.3354(3) 0.77521(16) 0.0306(4) Uani d . 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'
S S 0.1246 0.1234 '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'
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
O4 Ni1 O4 . 2 179.9990(10) .
O4 Ni1 N1 . . 92.68(5) .
O4 Ni1 N1 2 . 87.32(5) .
O4 Ni1 N1 . 2 87.32(5) .
O4 Ni1 N1 2 2 92.68(5) .
N1 Ni1 N1 . 2 180.0 .
O4 Ni1 O3 . 2 86.23(5) .
O4 Ni1 O3 2 2 93.77(5) .
N1 Ni1 O3 . 2 89.32(5) .
N1 Ni1 O3 2 2 90.69(5) .
O4 Ni1 O3 . . 93.77(5) .
O4 Ni1 O3 2 . 86.23(5) .
N1 Ni1 O3 . . 90.69(5) .
N1 Ni1 O3 2 . 89.31(5) .
O3 Ni1 O3 2 . 180.0 .
C1 S1 C6 . . 103.65(9) ?
Ni1 O3 H3A . . 105.2 ?
Ni1 O3 H3B . . 134.1 ?
H3A O3 H3B . . 117.1 ?
Ni1 O4 H4A . . 109.3 ?
Ni1 O4 H4B . . 114.5 ?
H4A O4 H4B . . 117.0 ?
C3 N1 C4 . . 116.70(16) ?
C3 N1 Ni1 . . 122.04(12) ?
C4 N1 Ni1 . . 121.22(12) ?
C2 C1 C5 . . 117.45(16) ?
C2 C1 S1 . . 125.97(14) ?
C5 C1 S1 . . 116.57(14) ?
C3 C2 C1 . . 119.08(17) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
N1 C3 C2 . . 123.81(17) ?
N1 C3 H3 . . 118.1 ?
C2 C3 H3 . . 118.1 ?
N1 C4 C5 . . 123.50(17) ?
N1 C4 H4 . . 118.3 ?
C5 C4 H4 . . 118.3 ?
C4 C5 C1 . . 119.45(17) ?
C4 C5 H5 . . 120.3 ?
C1 C5 H5 . . 120.3 ?
C7 C6 S1 . . 110.25(13) ?
C7 C6 H6A . . 109.6 ?
S1 C6 H6A . . 109.6 ?
C7 C6 H6B . . 109.6 ?
S1 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
O2 C7 O1 . . 126.41(18) ?
O2 C7 C6 . . 119.17(17) ?
O1 C7 C6 . . 114.39(17) ?
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
Ni1 O4 . 2.0727(12) .
Ni1 O4 2 2.0727(12) .
Ni1 N1 . 2.0762(15) .
Ni1 N1 2 2.0762(15) .
Ni1 O3 2 2.0967(13) .
Ni1 O3 . 2.0967(13) .
S1 C1 . 1.7524(18) ?
S1 C6 . 1.8035(19) ?
O1 C7 . 1.253(2) ?
O2 C7 . 1.249(2) ?
O3 H3A . 0.8501 ?
O3 H3B . 0.8503 ?
O4 H4A . 0.8501 ?
O4 H4B . 0.8501 ?
N1 C3 . 1.342(2) ?
N1 C4 . 1.344(2) ?
C1 C2 . 1.392(3) ?
C1 C5 . 1.396(3) ?
C2 C3 . 1.377(3) ?
C2 H2 . 0.9300 ?
C3 H3 . 0.9300 ?
C4 C5 . 1.373(3) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
C6 C7 . 1.528(3) ?
C6 H6A . 0.9700 ?
C6 H6B . 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
O3 H3A O2 1_454 0.85 2.13 2.951(2) 161
O3 H3B O1 1_554 0.85 1.92 2.7265(18) 158
O4 H4A O1 2_656 0.85 1.83 2.6697(18) 168
O4 H4B O2 1_444 0.85 2.01 2.855(2) 172
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O4 Ni1 N1 C3 . . . . -125.81(15) ?
O4 Ni1 N1 C3 2 . . . 54.19(15) ?
O3 Ni1 N1 C3 2 . . . -39.62(15) ?
O3 Ni1 N1 C3 . . . . 140.38(15) ?
O4 Ni1 N1 C4 . . . . 51.79(15) ?
O4 Ni1 N1 C4 2 . . . -128.21(15) ?
O3 Ni1 N1 C4 2 . . . 137.98(15) ?
O3 Ni1 N1 C4 . . . . -42.02(15) ?
C6 S1 C1 C2 . . . . 0.69(19) ?
C6 S1 C1 C5 . . . . -178.92(14) ?
C5 C1 C2 C3 . . . . 1.2(3) ?
S1 C1 C2 C3 . . . . -178.44(14) ?
C4 N1 C3 C2 . . . . -0.8(3) ?
Ni1 N1 C3 C2 . . . . 176.86(15) ?
C1 C2 C3 N1 . . . . -0.1(3) ?
C3 N1 C4 C5 . . . . 0.8(3) ?
Ni1 N1 C4 C5 . . . . -176.94(14) ?
N1 C4 C5 C1 . . . . 0.2(3) ?
C2 C1 C5 C4 . . . . -1.2(3) ?
S1 C1 C5 C4 . . . . 178.42(14) ?
C1 S1 C6 C7 . . . . 178.07(12) ?
S1 C6 C7 O2 . . . . 8.2(2) ?
S1 C6 C7 O1 . . . . -170.33(14) ?
