#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208480.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_2208480
loop_
_publ_author_name
'Hong Lin'
'Hong Su'
'Yun-long Feng'
_publ_section_title
catena-Poly[[diaquabis[(4-tolylsulfanyl)acetato-κO]nickel(II)]-μ-4,4'-bipyridine-κ²N:N']
_journal_coeditor_code           AT2009
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m747
_journal_page_last               m749
_journal_paper_doi               10.1107/S1600536806007926
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (C9 H9 O2 S)2 (C8 H8 N2)]'
_chemical_formula_moiety         'C28 H30 N2 Ni O6 S2'
_chemical_formula_sum            'C28 H30 N2 Ni O6 S2'
_chemical_formula_weight         613.37
_chemical_name_systematic
;
catena-Poly[[dddiaquabis[(4-tolylsulfanyl)acetato-\kO]nickel(II)]-
μ-4,4'-bipyridine-κ²N:N']
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.649(4)
_cell_length_b                   11.271(2)
_cell_length_c                   11.050(2)
_cell_measurement_reflns_used    2318
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      1.88
_cell_volume                     2693.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8799
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  .895
_exptl_absorpt_correction_T_min  .838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .12
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3198
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_gt           0.0383
_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)+(0.0586P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                2417
_reflns_number_total             3198
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            at2009.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2208480
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Ni Ni1 0.0000 0.05002(3) 0.2500 0.02255(12) Uani d S 1
S S1 0.14634(3) 0.20241(6) -0.05321(6) 0.04796(19) Uani d . 1
N N1 0.0000 0.23474(19) 0.2500 0.0256(5) Uani d S 1
N N2 0.0000 0.86487(19) 0.2500 0.0253(5) Uani d S 1
O O1 0.15004(8) 0.1089(2) 0.27308(17) 0.0617(5) Uani d . 1
O O1W 0.05634(7) 0.05989(13) 0.40683(14) 0.0325(3) Uani d D 1
H H1WA 0.0636(11) 0.0061(19) 0.455(2) 0.049 Uiso d D 1
H H1WB 0.0912(9) 0.073(2) 0.377(2) 0.049 Uiso d D 1
O O2 0.07573(6) 0.05358(11) 0.13888(13) 0.0287(3) Uani d . 1
C C1 0.19654(15) 0.7095(3) 0.1132(3) 0.0719(9) Uani d . 1
H H1A 0.1815 0.7630 0.0510 0.108 Uiso calc R 1
H H1B 0.2402 0.7208 0.1274 0.108 Uiso calc R 1
H H1C 0.1758 0.7250 0.1865 0.108 Uiso calc R 1
C C2 0.18418(12) 0.5832(3) 0.0734(2) 0.0508(7) Uani d . 1
C C3 0.15479(12) 0.5561(3) -0.0373(3) 0.0515(7) Uani d . 1
H H3A 0.1423 0.6174 -0.0893 0.062 Uiso calc R 1
C C4 0.14359(11) 0.4399(2) -0.0721(2) 0.0463(6) Uani d . 1
H H4A 0.1241 0.4240 -0.1471 0.056 Uiso calc R 1
C C5 0.16121(10) 0.3467(2) 0.0043(2) 0.0404(6) Uani d . 1
C C6 0.18997(12) 0.3730(3) 0.1156(2) 0.0490(6) Uani d . 1
H H6A 0.2013 0.3121 0.1689 0.059 Uiso calc R 1
C C7 0.20176(12) 0.4891(3) 0.1475(2) 0.0555(7) Uani d . 1
H H7A 0.2223 0.5048 0.2215 0.067 Uiso calc R 1
C C8 0.17392(10) 0.1034(2) 0.0652(2) 0.0458(6) Uani d . 1
H H8A 0.1813 0.0262 0.0299 0.055 Uiso calc R 1
H H8B 0.2132 0.1329 0.0983 0.055 Uiso calc R 1
C C9 0.13020(10) 0.0880(2) 0.1690(2) 0.0351(5) Uani d . 1
C C10 0.01972(10) 0.29726(18) 0.15610(19) 0.0306(5) Uani d . 1
H H10A 0.0331 0.2560 0.0892 0.037 Uiso calc R 1
C C11 0.02130(10) 0.41928(17) 0.15342(19) 0.0313(5) Uani d . 1
H H11A 0.0366 0.4582 0.0869 0.038 Uiso calc R 1
C C12 0.0000 0.4846(2) 0.2500 0.0248(6) Uani d S 1
C C13 0.0000 0.6157(2) 0.2500 0.0236(6) Uani d S 1
C C14 -0.03052(11) 0.68065(18) 0.3350(2) 0.0363(5) Uani d . 1
H H14A -0.0518 0.6417 0.3945 0.044 Uiso calc R 1
C C15 -0.02947(11) 0.80322(19) 0.3318(2) 0.0373(5) Uani d . 1
H H15A -0.0505 0.8446 0.3900 0.045 Uiso calc R 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'
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
O1W Ni1 O1W 2 . 173.86(8) yes
O1W Ni1 N1 2 . 86.93(4) yes
O1W Ni1 N1 . . 86.93(4) ?
O1W Ni1 N2 2 1_545 93.07(4) yes
O1W Ni1 N2 . 1_545 93.07(4) ?
O1W Ni1 O2 2 2 92.43(6) yes
O1W Ni1 O2 . 2 87.45(6) ?
N1 Ni1 O2 . 2 88.90(4) yes
N2 Ni1 O2 1_545 2 91.10(4) yes
O1W Ni1 O2 2 . 87.45(6) yes
O1W Ni1 O2 . . 92.43(6) ?
N1 Ni1 O2 . . 88.90(4) yes
N2 Ni1 O2 1_545 . 91.10(4) yes
O2 Ni1 O2 2 . 177.80(7) yes
C5 S1 C8 . . 105.03(13) ?
C10 N1 C10 . 2 116.5(2) ?
C10 N1 Ni1 . . 121.73(12) ?
C10 N1 Ni1 2 . 121.73(12) ?
C15 N2 C15 2 . 116.8(2) ?
C15 N2 Ni1 2 1_565 121.59(12) ?
C15 N2 Ni1 . 1_565 121.59(12) ?
Ni1 O1W H1WA . . 126.3(19) ?
Ni1 O1W H1WB . . 100.7(18) ?
H1WA O1W H1WB . . 103.5(18) ?
C9 O2 Ni1 . . 126.46(14) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
C7 C2 C3 . . 117.1(3) ?
C7 C2 C1 . . 120.7(3) ?
C3 C2 C1 . . 122.2(3) ?
C4 C3 C2 . . 121.4(3) ?
C4 C3 H3A . . 119.3 ?
C2 C3 H3A . . 119.3 ?
C3 C4 C5 . . 120.5(2) ?
C3 C4 H4A . . 119.8 ?
C5 C4 H4A . . 119.8 ?
C6 C5 C4 . . 118.5(2) ?
C6 C5 S1 . . 125.6(2) ?
C4 C5 S1 . . 115.81(19) ?
C7 C6 C5 . . 120.1(3) ?
C7 C6 H6A . . 119.9 ?
C5 C6 H6A . . 119.9 ?
C6 C7 C2 . . 122.3(3) ?
C6 C7 H7A . . 118.8 ?
C2 C7 H7A . . 118.8 ?
C9 C8 S1 . . 114.77(16) ?
C9 C8 H8A . . 108.6 ?
S1 C8 H8A . . 108.6 ?
C9 C8 H8B . . 108.6 ?
S1 C8 H8B . . 108.6 ?
H8A C8 H8B . . 107.6 ?
O1 C9 O2 . . 125.6(2) ?
O1 C9 C8 . . 118.5(2) ?
O2 C9 C8 . . 115.9(2) ?
N1 C10 C11 . . 123.46(19) ?
N1 C10 H10A . . 118.3 ?
C11 C10 H10A . . 118.3 ?
C10 C11 C12 . . 120.16(19) ?
C10 C11 H11A . . 119.9 ?
C12 C11 H11A . . 119.9 ?
C11 C12 C11 . 2 116.2(3) ?
C11 C12 C13 . . 121.91(13) ?
C14 C13 C14 . 2 116.1(2) ?
C14 C13 C12 . . 121.96(12) ?
C14 C13 C12 2 . 121.96(12) ?
C13 C14 C15 . . 120.21(19) ?
C13 C14 H14A . . 119.9 ?
C15 C14 H14A . . 119.9 ?
N2 C15 C14 . . 123.3(2) ?
N2 C15 H15A . . 118.3 ?
C14 C15 H15A . . 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 O1W 2 2.0766(17) yes
Ni1 O1W . 2.0766(17) ?
Ni1 N1 . 2.082(2) yes
Ni1 N2 1_545 2.087(2) yes
Ni1 O2 2 2.0927(14) yes
Ni1 O2 . 2.0927(14) ?
S1 C5 . 1.771(3) ?
S1 C8 . 1.801(3) ?
N1 C10 . 1.340(2) ?
N1 C10 2 1.340(2) ?
N2 C15 2 1.327(2) ?
N2 C15 . 1.327(2) ?
N2 Ni1 1_565 2.087(2) ?
O1 C9 . 1.232(3) ?
O1W H1WA . 0.817(15) ?
O1W H1WB . 0.850(15) ?
O2 C9 . 1.271(3) ?
C1 C2 . 1.510(4) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 C7 . 1.383(4) ?
C2 C3 . 1.388(4) ?
C3 C4 . 1.384(3) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.390(3) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.385(3) ?
C6 C7 . 1.375(4) ?
C6 H6A . 0.9300 ?
C7 H7A . 0.9300 ?
C8 C9 . 1.530(3) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C10 C11 . 1.376(3) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.392(2) ?
C11 H11A . 0.9300 ?
C12 C11 2 1.392(2) ?
C12 C13 . 1.479(4) ?
C13 C14 . 1.382(2) ?
C13 C14 2 1.382(2) ?
C14 C15 . 1.382(3) ?
C14 H14A . 0.9300 ?
C15 H15A . 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
O1W H1WA O2 6_556 0.817(15) 2.146(19) 2.879(2) 149(3)
O1W H1WA S1 6_556 0.817(15) 2.96(2) 3.5572(17) 132(2)
O1W H1WB O1 . 0.850(15) 1.800(16) 2.622(2) 162(3)
