#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/25/2222527.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_2222527
loop_
_publ_author_name
'Du, Zhong-Xiang'
'Ji, Su-Ning'
_publ_section_title
catena-Poly[[diaquanickel(II)]-bis(μ-pyridine-4-sulfinato)-κ²N,O;κ²O,N]
_journal_coeditor_code           AT2818
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m846
_journal_paper_doi               10.1107/S1600536809024258
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C5 H4 N O2 S)2 (H2 O)2]'
_chemical_formula_moiety         'C10 H12 N2 Ni O6 S2'
_chemical_formula_sum            'C10 H12 N2 Ni O6 S2'
_chemical_formula_weight         379.05
_chemical_name_systematic
;
catena-Poly[[diaquanickel(II)]-bis(μ-pyridine-4-sulfinato)-
κ²N,O;κ²O,N]
;
_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                96.784(8)
_cell_angle_beta                 95.140(8)
_cell_angle_gamma                107.709(8)
_cell_formula_units_Z            1
_cell_length_a                   6.403(5)
_cell_length_b                   7.309(5)
_cell_length_c                   7.602(5)
_cell_measurement_reflns_used    1414
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.72
_cell_volume                     333.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.9493
_diffrn_measured_fraction_theta_max 0.9493
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2417
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.7871
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             194
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0311
_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)+(0.0581P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                1043
_reflns_number_total             1180
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2818.cif
_cod_data_source_block           I
_cod_database_code               2222527
_cod_database_fobs_code          2222527
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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.5000 0.0000 1.0000 0.02196(18) Uani d S 1 . .
S S1 0.37032(11) 0.32818(9) 0.81172(8) 0.0282(2) Uani d . 1 . .
O O1 0.1697(3) -0.2599(3) 0.9900(3) 0.0432(5) Uani d . 1 . .
H H1W 0.1594 -0.3595 0.9190 0.065 Uiso d R 1 . .
H H2W 0.0660 -0.2844 1.0522 0.065 Uiso d R 1 . .
O O2 0.1653(3) 0.3862(3) 0.7920(3) 0.0374(5) Uani d . 1 . .
O O3 0.3059(3) 0.1287(3) 0.8709(2) 0.0330(4) Uani d . 1 . .
N N1 0.4591(3) 0.1289(3) 0.2369(3) 0.0257(5) Uani d . 1 . .
C C1 0.2579(4) 0.1289(4) 0.2770(4) 0.0306(6) Uani d . 1 . .
H H1 0.1377 0.0841 0.1873 0.037 Uiso calc R 1 . .
C C2 0.2257(5) 0.1933(4) 0.4472(4) 0.0320(6) Uani d . 1 . .
H H2 0.0857 0.1920 0.4721 0.038 Uiso calc R 1 . .
C C3 0.4053(4) 0.2601(3) 0.5805(3) 0.0250(5) Uani d . 1 . .
C C4 0.6131(4) 0.2690(4) 0.5387(3) 0.0271(6) Uani d . 1 . .
H H4 0.7370 0.3191 0.6247 0.033 Uiso calc R 1 . .
C C5 0.6316(4) 0.2014(4) 0.3656(4) 0.0304(6) Uani d . 1 . .
H H5 0.7713 0.2066 0.3369 0.036 Uiso calc R 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 0.0291(3) 0.0292(3) 0.0131(2) 0.0168(2) 0.00585(17) 0.00249(17)
S1 0.0353(4) 0.0309(4) 0.0215(4) 0.0151(3) 0.0082(3) 0.0004(3)
O1 0.0457(12) 0.0320(11) 0.0528(13) 0.0108(9) 0.0236(10) 0.0015(9)
O2 0.0473(12) 0.0441(11) 0.0339(11) 0.0299(10) 0.0164(9) 0.0075(9)
O3 0.0414(11) 0.0401(10) 0.0251(9) 0.0212(9) 0.0098(8) 0.0081(8)
N1 0.0288(11) 0.0309(11) 0.0210(11) 0.0141(9) 0.0055(8) 0.0047(9)
C1 0.0284(13) 0.0412(15) 0.0254(14) 0.0162(11) 0.0033(11) 0.0040(11)
C2 0.0277(13) 0.0435(15) 0.0299(15) 0.0176(12) 0.0089(11) 0.0047(12)
C3 0.0328(13) 0.0246(12) 0.0217(13) 0.0134(10) 0.0079(10) 0.0047(10)
C4 0.0271(13) 0.0327(13) 0.0217(13) 0.0106(11) 0.0036(10) 0.0015(10)
C5 0.0304(14) 0.0377(15) 0.0275(15) 0.0160(12) 0.0084(11) 0.0053(11)
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'
Ni Ni 0.3393 1.1124 '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'
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
N1 Ni1 N1 2_656 1_556 180.0000(10) yes
N1 Ni1 O3 2_656 2_657 90.55(9) ?
N1 Ni1 O3 1_556 2_657 89.45(9) ?
N1 Ni1 O3 2_656 . 89.45(9) yes
N1 Ni1 O3 1_556 . 90.55(9) yes
O3 Ni1 O3 2_657 . 180.0000(10) yes
N1 Ni1 O1 2_656 2_657 92.01(8) ?
N1 Ni1 O1 1_556 2_657 87.99(8) ?
O3 Ni1 O1 2_657 2_657 85.24(9) ?
O3 Ni1 O1 . 2_657 94.76(9) ?
N1 Ni1 O1 2_656 . 87.99(8) yes
N1 Ni1 O1 1_556 . 92.01(8) ?
O3 Ni1 O1 2_657 . 94.76(9) ?
O3 Ni1 O1 . . 85.24(9) yes
O1 Ni1 O1 2_657 . 180.0 yes
O2 S1 O3 . . 107.19(12) ?
O2 S1 C3 . . 102.55(12) ?
O3 S1 C3 . . 99.77(11) ?
Ni1 O1 H1W . . 114.8 ?
Ni1 O1 H2W . . 135.0 ?
H1W O1 H2W . . 109.3 ?
S1 O3 Ni1 . . 128.93(12) ?
C5 N1 C1 . . 118.2(2) ?
C5 N1 Ni1 . 1_554 119.50(18) ?
C1 N1 Ni1 . 1_554 121.99(18) ?
N1 C1 C2 . . 121.9(2) ?
N1 C1 H1 . . 119.1 ?
C2 C1 H1 . . 119.1 ?
C1 C2 C3 . . 118.9(2) ?
C1 C2 H2 . . 120.5 ?
C3 C2 H2 . . 120.5 ?
C4 C3 C2 . . 119.5(2) ?
C4 C3 S1 . . 119.35(19) ?
C2 C3 S1 . . 121.1(2) ?
C3 C4 C5 . . 118.0(2) ?
C3 C4 H4 . . 121.0 ?
C5 C4 H4 . . 121.0 ?
N1 C5 C4 . . 123.3(2) ?
N1 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
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 N1 2_656 2.008(2) ?
Ni1 N1 1_556 2.008(2) yes
Ni1 O3 2_657 2.026(2) ?
Ni1 O3 . 2.026(2) yes
Ni1 O1 2_657 2.362(2) ?
Ni1 O1 . 2.362(2) yes
S1 O2 . 1.498(2) ?
S1 O3 . 1.523(2) ?
S1 C3 . 1.821(3) ?
O1 H1W . 0.8350 ?
O1 H2W . 0.8371 ?
N1 C5 . 1.336(4) ?
N1 C1 . 1.350(3) ?
N1 Ni1 1_554 2.008(2) ?
C1 C2 . 1.379(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.386(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.380(4) ?
C4 C5 . 1.378(4) ?
C4 H4 . 0.9300 ?
C5 H5 . 0.9300 ?
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 H1W O2 1_545 0.84 2.00 2.826(3) 168.2 yes
O1 H2W O2 2_557 0.84 2.00 2.827(3) 169.4 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 S1 O3 Ni1 . . . . -157.49(13) ?
C3 S1 O3 Ni1 . . . . 96.00(15) ?
N1 Ni1 O3 S1 2_656 . . . -93.25(15) ?
N1 Ni1 O3 S1 1_556 . . . 86.75(15) ?
O1 Ni1 O3 S1 2_657 . . . -1.28(15) ?
O1 Ni1 O3 S1 . . . . 178.72(15) ?
C5 N1 C1 C2 . . . . -2.8(4) ?
Ni1 N1 C1 C2 1_554 . . . 170.9(2) ?
N1 C1 C2 C3 . . . . 0.1(4) ?
C1 C2 C3 C4 . . . . 2.9(4) ?
C1 C2 C3 S1 . . . . -174.8(2) ?
O2 S1 C3 C4 . . . . 155.44(19) ?
O3 S1 C3 C4 . . . . -94.3(2) ?
O2 S1 C3 C2 . . . . -26.8(2) ?
O3 S1 C3 C2 . . . . 83.4(2) ?
C2 C3 C4 C5 . . . . -3.1(4) ?
S1 C3 C4 C5 . . . . 174.71(19) ?
C1 N1 C5 C4 . . . . 2.7(4) ?
Ni1 N1 C5 C4 1_554 . . . -171.20(19) ?
C3 C4 C5 N1 . . . . 0.3(4) ?
