#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/58/2015875.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_2015875
loop_
_publ_author_name
'M. Enriqueta Díaz de Vivar'
'Sergio Baggio'
'María Teresa Garland'
'Ricardo Baggio'
_publ_section_title
;
 An unusual P3₁2 framework for the
 Ni(4,4'-bipyridine)(H₂O)₄ chain
;
_journal_coeditor_code           AV3057
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m153
_journal_page_last               m156
_journal_paper_doi               10.1107/S0108270107007214
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C10 H8 N2) (H2 O)4] S2 O3 , 2H2 O'
_chemical_formula_moiety         'C10 H16 N2 Ni O4 2+ , O3 S2 2- , 2H2 O'
_chemical_formula_sum            'C10 H20 N2 Ni O9 S2'
_chemical_formula_weight         435.11
_chemical_name_systematic
;
catena-Poly[[[tetraaquanickel(II)]-μ-4,4'-bipyridine-κ²N:N'] thiosulfate
dihydrate]
;
_space_group_IT_number           152
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.3363(9)
_cell_length_b                   11.3363(9)
_cell_length_c                   11.1523(13)
_cell_measurement_temperature    274(2)
_cell_volume                     1241.2(2)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL-NT and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      274(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 0.970
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10484
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.309
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1907
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.0981
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0412P)²+0.57P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                1725
_reflns_number_total             1907
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            av3057.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'P 31 2" '
_cod_database_code               2015875
_cod_database_fobs_code          2015875
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'y, x, -z'
'-x+y, -x, z+2/3'
'-x, -x+y, -z+1/3'
'x-y, -y, -z+2/3'
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 1.0000 0.60675(4) 1.1667 0.02801(14) Uani d S 1 . .
O O1W 1.1959(2) 0.6991(2) 1.1020(2) 0.0395(5) Uani d D 1 . .
H H1WB 1.209(4) 0.649(3) 1.055(3) 0.066(13) Uiso d D 1 . .
H H1WA 1.269(2) 0.742(4) 1.142(3) 0.058(13) Uiso d D 1 . .
O O2W 1.0791(2) 0.6516(2) 1.33982(19) 0.0415(5) Uani d D 1 . .
H H2WB 1.153(2) 0.726(2) 1.346(3) 0.067(13) Uiso d D 1 . .
H H2WA 1.067(3) 0.613(3) 1.4072(17) 0.051(11) Uiso d D 1 . .
O O3W 0.6763(3) 0.4299(4) 0.7414(3) 0.0827(11) Uani d D 1 . .
H H3WB 0.649(4) 0.476(4) 0.781(4) 0.088(18) Uiso d D 1 . .
H H3WA 0.756(2) 0.488(4) 0.719(5) 0.107(19) Uiso d D 1 . .
N N1 1.0000 0.7946(3) 1.1667 0.0312(7) Uani d S 1 . .
N N2 1.0000 1.4214(3) 1.1667 0.0319(7) Uani d S 1 . .
C C1 0.8852(3) 0.8001(3) 1.1688(3) 0.0430(8) Uani d . 1 . .
H H1 0.8031 0.7182 1.1701 0.052 Uiso calc R 1 . .
C C2 0.8805(3) 0.9185(3) 1.1693(3) 0.0413(7) Uani d . 1 . .
H H2 0.7968 0.9150 1.1715 0.050 Uiso calc R 1 . .
C C3 1.0000 1.0435(3) 1.1667 0.0322(9) Uani d S 1 . .
C C4 1.0000 1.1750(4) 1.1667 0.0342(9) Uani d S 1 . .
C C5 0.8901(3) 1.1831(3) 1.1244(3) 0.0406(7) Uani d . 1 . .
H H5 0.8138 1.1061 1.0948 0.049 Uiso calc R 1 . .
C C6 0.8947(3) 1.3074(3) 1.1267(3) 0.0412(7) Uani d . 1 . .
H H6 0.8193 1.3110 1.0984 0.049 Uiso calc R 1 . .
S S1 0.98833(19) 0.44014(16) 0.69163(13) 0.0388(4) Uiso d PD 0.50 A -1
S S2 0.9882(2) 0.60284(18) 0.62674(14) 0.0477(4) Uani d P 0.50 A -1
O O1 0.9453(7) 0.4222(6) 0.8165(4) 0.078(2) Uani d PD 0.50 A -1
O O2 1.1256(9) 0.4590(16) 0.6800(11) 0.078(4) Uani d PD 0.50 A -1
O O3 0.8935(9) 0.3208(9) 0.6206(8) 0.044(2) Uani d PD 0.50 A -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
O1W Ni1 O1W 5_767 . 176.44(13) y
O2W Ni1 O2W . 5_767 176.68(14) y
N2 Ni1 N1 1_545 . 180.000 y
O1W Ni1 O2W 5_767 . 91.43(9) y
O1W Ni1 O2W . 5_767 91.42(9) ?
O1W Ni1 O2W . . 88.68(9) y
O1W Ni1 O2W 5_767 5_767 88.68(9) ?
O1W Ni1 N2 . 1_545 88.22(6) y
O1W Ni1 N2 5_767 1_545 88.22(6) ?
O2W Ni1 N2 . 1_545 91.66(7) y
O2W Ni1 N2 5_767 1_545 91.66(7) ?
O1W Ni1 N1 . . 91.78(6) y
O1W Ni1 N1 5_767 . 91.78(6) ?
O2W Ni1 N1 . . 88.34(7) y
O2W Ni1 N1 5_767 . 88.34(7) ?
Ni1 O1W H1WB . . 113(3) ?
Ni1 O1W H1WA . . 127(3) ?
H1WB O1W H1WA . . 106(2) ?
Ni1 O2W H2WB . . 115(2) ?
Ni1 O2W H2WA . . 139(2) ?
H2WB O2W H2WA . . 105(2) ?
H3WB O3W H3WA . . 104(2) ?
C1 N1 C1 5_767 . 115.4(4) ?
C1 N1 Ni1 5_767 . 122.31(19) ?
C1 N1 Ni1 . . 122.3(2) ?
C6 N2 C6 5_767 . 116.6(4) ?
C6 N2 Ni1 5_767 1_565 121.69(19) ?
C6 N2 Ni1 . 1_565 121.69(19) ?
N1 C1 C2 . . 124.3(3) ?
N1 C1 H1 . . 117.9 ?
C2 C1 H1 . . 117.9 ?
C1 C2 C3 . . 120.3(3) ?
C1 C2 H2 . . 119.9 ?
C3 C2 H2 . . 119.9 ?
C2 C3 C2 . 5_767 115.5(4) ?
C2 C3 C4 . . 122.2(2) ?
C2 C3 C4 5_767 . 122.2(2) ?
C5 C4 C5 5_767 . 117.4(4) ?
C5 C4 C3 5_767 . 121.28(19) ?
C5 C4 C3 . . 121.28(19) ?
C4 C5 C6 . . 119.2(3) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
N2 C6 C5 . . 123.8(3) ?
N2 C6 H6 . . 118.1 ?
C5 C6 H6 . . 118.1 ?
O1 S1 O2 . . 111.2(5) ?
O1 S1 O3 . . 110.3(4) ?
O2 S1 O3 . . 108.7(4) ?
O1 S1 S2 . . 108.8(2) ?
O2 S1 S2 . . 109.0(5) ?
O3 S1 S2 . . 108.6(6) ?
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 5_767 2.055(2) ?
Ni1 O1W . 2.055(2) y
Ni1 O2W . 2.082(2) y
Ni1 O2W 5_767 2.082(2) ?
Ni1 N2 1_545 2.101(3) y
Ni1 N1 . 2.129(3) y
O1W H1WA . 0.85(4) ?
O1W H1WB . 0.85(4) ?
O2W H2WA . 0.85(2) ?
O2W H2WB . 0.85(2) ?
O3W H3WA . 0.85(5) ?
O3W H3WB . 0.85(5) ?
N1 C1 5_767 1.334(4) ?
N1 C1 . 1.334(4) ?
N2 C6 5_767 1.324(4) ?
N2 C6 . 1.324(4) ?
N2 Ni1 1_565 2.101(3) ?
C1 C2 . 1.370(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.388(4) ?
C2 H2 . 0.9300 ?
C3 C2 5_767 1.388(4) ?
C3 C4 . 1.490(5) ?
C4 C5 5_767 1.377(4) ?
C4 C5 . 1.377(4) ?
C5 C6 . 1.384(4) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
S1 O1 . 1.456(5) ?
S1 O2 . 1.466(6) ?
S1 O3 . 1.470(6) ?
S1 S2 . 1.982(2) ?
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 O1 3_657 0.85(4) 2.13(2) 2.835(7) 140(4)
O1W H1WB O3W 6_666 0.85(4) 1.85(2) 2.681(4) 167(4)
O2W H2WA O1 5_767 0.85(2) 1.91(2) 2.710(5) 156(3)
O2W H2WA S2 1_556 0.85(2) 2.59(2) 3.322(3) 146(3)
O2W H2WB O2 4_775 0.85(2) 1.88(2) 2.723(7) 169(4)
O2W H2WB O3 3_657 0.85(2) 1.93(2) 2.776(7) 174(3)
O3W H3WA S2 . 0.85(5) 2.50(2) 3.324(4) 164(4)
O3W H3WA S2 5_766 0.85(5) 2.51(2) 3.322(4) 160(5)
O3W H3WB O3 2_655 0.85(5) 2.16(2) 2.862(13) 140(5)
O3W H3WB O2 6_566 0.85(5) 2.39(2) 3.037(14) 134(5)
O3W H3WB O1 6_566 0.85(5) 2.37(2) 3.196(8) 164(5)
