#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/84/2228482.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2228482
loop_
_publ_author_name
'Liu, Zhengming'
'Qu, Botao'
'Yu, Jianghua'
'Yuan, Limin'
'Liu, Wenlong'
_publ_section_title
;
 Bis(μ-2,2'-disulfanediyldibenzoato)bis[aqua(2,2'-bipyridine)nickel(II)]
;
_journal_coeditor_code           NG5064
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1563
_journal_paper_doi               10.1107/S1600536810045824
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni2 (C14 H8 O4 S2)2 (C10 H8 N2)2 (H2 O)2]'
_chemical_formula_moiety         'C48 H36 N4 Ni2 O10 S4'
_chemical_formula_sum            'C48 H36 N4 Ni2 O10 S4'
_chemical_formula_weight         1074.47
_chemical_name_systematic
;
Bis(μ-2,2'-disulfanediyldibenzoato)bis[aqua(2,2'-bipyridine)nickel(II)]
;
_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                 93.196(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.498(4)
_cell_length_b                   16.769(5)
_cell_length_c                   10.238(3)
_cell_measurement_reflns_used    7893
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.465
_cell_measurement_theta_min      2.333
_cell_volume                     2313.7(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19861
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.7559
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0291
_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)+(0.0369P)²+0.5543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                4428
_reflns_number_total             5302
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng5064.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228482
_cod_database_fobs_code          2228482
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_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.847531(15) 0.055670(13) 0.87112(2) 0.035 Uani d . 1 . .
C C1 0.71145(13) -0.16433(10) 0.72485(16) 0.0372(4) Uani d . 1 . .
C C2 0.61332(13) -0.15067(10) 0.75883(16) 0.0361(4) Uani d . 1 . .
C C3 0.54059(16) -0.20699(12) 0.7226(2) 0.0516(5) Uani d . 1 . .
H H3 0.4753 -0.1986 0.7440 0.062 Uiso calc R 1 . .
C C4 0.56481(19) -0.27532(13) 0.6549(2) 0.0630(6) Uani d . 1 . .
H H4 0.5157 -0.3124 0.6317 0.076 Uiso calc R 1 . .
C C5 0.66066(19) -0.28886(13) 0.6217(2) 0.0635(6) Uani d . 1 . .
H H5 0.6763 -0.3347 0.5760 0.076 Uiso calc R 1 . .
C C6 0.73315(17) -0.23407(12) 0.65659(19) 0.0514(5) Uani d . 1 . .
H H6 0.7980 -0.2435 0.6344 0.062 Uiso calc R 1 . .
C C7 0.79432(13) -0.10570(11) 0.75377(16) 0.0375(4) Uani d . 1 . .
C C8 0.26979(12) 0.00106(10) 0.79602(16) 0.0364(4) Uani d . 1 . .
C C9 0.37029(12) -0.01665(10) 0.77860(15) 0.0352(3) Uani d . 1 . .
C C10 0.41443(15) 0.01522(13) 0.67009(18) 0.0493(5) Uani d . 1 . .
H H10 0.4808 0.0044 0.6576 0.059 Uiso calc R 1 . .
C C11 0.36100(17) 0.06275(15) 0.5808(2) 0.0609(6) Uani d . 1 . .
H H11 0.3919 0.0836 0.5094 0.073 Uiso calc R 1 . .
C C12 0.26263(17) 0.07935(15) 0.5966(2) 0.0631(6) Uani d . 1 . .
H H12 0.2268 0.1108 0.5359 0.076 Uiso calc R 1 . .
C C13 0.21750(15) 0.04884(13) 0.70385(19) 0.0509(5) Uani d . 1 . .
H H13 0.1511 0.0603 0.7149 0.061 Uiso calc R 1 . .
C C14 0.21825(12) -0.02608(10) 0.91345(16) 0.0345(3) Uani d . 1 . .
O O1 0.76966(9) -0.04232(7) 0.81054(13) 0.0430(3) Uani d . 1 . .
O O2 0.87892(10) -0.12087(10) 0.71985(16) 0.0652(4) Uani d . 1 . .
O O3 0.26151(9) -0.07316(7) 0.99322(11) 0.0361(3) Uani d . 1 . .
O O4 0.13146(8) -0.00058(8) 0.93571(12) 0.0437(3) Uani d . 1 . .
S S1 0.58588(3) -0.06272(3) 0.85144(4) 0.03707(9) Uani d . 1 . .
S S2 0.44006(3) -0.07593(3) 0.89692(4) 0.03871(10) Uani d . 1 . .
C C15 0.71731(16) 0.10390(13) 0.6351(2) 0.0548(5) Uani d . 1 . .
H H15 0.7039 0.0497 0.6255 0.066 Uiso calc R 1 . .
C C16 0.66890(17) 0.15698(15) 0.5504(2) 0.0650(6) Uani d . 1 . .
H H16 0.6246 0.1389 0.4841 0.078 Uiso calc R 1 . .
C C17 0.68751(18) 0.23695(15) 0.5661(2) 0.0652(6) Uani d . 1 . .
H H17 0.6560 0.2739 0.5103 0.078 Uiso calc R 1 . .
C C18 0.75337(18) 0.26211(13) 0.6655(2) 0.0577(5) Uani d . 1 . .
H H18 0.7656 0.3162 0.6782 0.069 Uiso calc R 1 . .
C C19 0.80122(14) 0.20630(11) 0.74626(18) 0.0430(4) Uani d . 1 . .
C C20 0.87518(14) 0.22631(11) 0.85377(18) 0.0441(4) Uani d . 1 . .
C C21 0.90507(19) 0.30399(14) 0.8850(2) 0.0629(6) Uani d . 1 . .
H H21 0.8783 0.3471 0.8380 0.075 Uiso calc R 1 . .
C C22 0.9751(2) 0.31585(16) 0.9869(3) 0.0739(7) Uani d . 1 . .
H H22 0.9951 0.3673 1.0099 0.089 Uiso calc R 1 . .
C C23 1.01454(18) 0.25211(16) 1.0536(2) 0.0671(6) Uani d . 1 . .
H H23 1.0621 0.2593 1.1219 0.081 Uiso calc R 1 . .
C C24 0.98269(15) 0.17672(14) 1.0180(2) 0.0564(5) Uani d . 1 . .
H H24 1.0101 0.1332 1.0631 0.068 Uiso calc R 1 . .
N N1 0.78256(11) 0.12735(9) 0.73016(14) 0.0413(3) Uani d . 1 . .
N N2 0.91367(11) 0.16354(9) 0.92081(15) 0.0432(3) Uani d . 1 . .
O O5 0.96680(9) 0.01730(9) 0.77302(14) 0.0491(3) Uani d D 1 . .
H H5A 1.0177(12) 0.0183(13) 0.824(2) 0.074 Uiso d D 1 . .
H H5B 0.9511(17) -0.0306(7) 0.754(2) 0.074 Uiso d D 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
O1 Ni1 N1 . . 93.79(6) ?
O1 Ni1 O5 . . 90.21(6) ?
N1 Ni1 O5 . . 99.03(6) ?
O1 Ni1 N2 . . 173.06(6) ?
N1 Ni1 N2 . . 79.70(6) ?
O5 Ni1 N2 . . 93.16(6) ?
O1 Ni1 O3 . 3_657 86.85(5) ?
N1 Ni1 O3 . 3_657 95.52(6) ?
O5 Ni1 O3 . 3_657 165.32(5) ?
N2 Ni1 O3 . 3_657 91.37(5) ?
O1 Ni1 O4 . 3_657 88.47(5) ?
N1 Ni1 O4 . 3_657 156.68(6) ?
O5 Ni1 O4 . 3_657 104.18(5) ?
N2 Ni1 O4 . 3_657 96.58(6) ?
O3 Ni1 O4 3_657 3_657 61.39(5) ?
O1 Ni1 C14 . 3_657 84.52(5) ?
N1 Ni1 C14 . 3_657 126.01(6) ?
O5 Ni1 C14 . 3_657 134.86(6) ?
N2 Ni1 C14 . 3_657 97.33(6) ?
O3 Ni1 C14 3_657 3_657 30.51(5) ?
O4 Ni1 C14 3_657 3_657 31.10(5) ?
C6 C1 C2 . . 119.01(17) ?
C6 C1 C7 . . 117.97(17) ?
C2 C1 C7 . . 122.97(15) ?
C3 C2 C1 . . 118.77(17) ?
C3 C2 S1 . . 122.05(15) ?
C1 C2 S1 . . 119.15(13) ?
C4 C3 C2 . . 120.6(2) ?
C4 C3 H3 . . 119.7 ?
C2 C3 H3 . . 119.7 ?
C5 C4 C3 . . 120.7(2) ?
C5 C4 H4 . . 119.6 ?
C3 C4 H4 . . 119.6 ?
C4 C5 C6 . . 119.4(2) ?
C4 C5 H5 . . 120.3 ?
C6 C5 H5 . . 120.3 ?
C5 C6 C1 . . 121.4(2) ?
C5 C6 H6 . . 119.3 ?
C1 C6 H6 . . 119.3 ?
O2 C7 O1 . . 124.88(17) ?
O2 C7 C1 . . 119.81(17) ?
O1 C7 C1 . . 115.29(15) ?
C13 C8 C9 . . 119.23(16) ?
C13 C8 C14 . . 118.52(16) ?
C9 C8 C14 . . 122.18(15) ?
C10 C9 C8 . . 118.46(16) ?
C10 C9 S2 . . 121.23(14) ?
C8 C9 S2 . . 120.27(13) ?
C11 C10 C9 . . 121.06(18) ?
C11 C10 H10 . . 119.5 ?
C9 C10 H10 . . 119.5 ?
C12 C11 C10 . . 120.63(19) ?
C12 C11 H11 . . 119.7 ?
C10 C11 H11 . . 119.7 ?
C11 C12 C13 . . 119.32(19) ?
C11 C12 H12 . . 120.3 ?
C13 C12 H12 . . 120.3 ?
C12 C13 C8 . . 121.29(19) ?
C12 C13 H13 . . 119.4 ?
C8 C13 H13 . . 119.4 ?
O3 C14 O4 . . 119.43(15) ?
O3 C14 C8 . . 119.62(15) ?
O4 C14 C8 . . 120.92(15) ?
O3 C14 Ni1 . 3_657 58.08(9) ?
O4 C14 Ni1 . 3_657 62.00(9) ?
C8 C14 Ni1 . 3_657 170.27(12) ?
C7 O1 Ni1 . . 132.52(12) ?
C14 O3 Ni1 . 3_657 91.41(10) ?
C14 O4 Ni1 . 3_657 86.90(10) ?
C2 S1 S2 . . 104.94(6) ?
C9 S2 S1 . . 105.08(6) ?
N1 C15 C16 . . 122.5(2) ?
N1 C15 H15 . . 118.7 ?
C16 C15 H15 . . 118.7 ?
C17 C16 C15 . . 118.6(2) ?
C17 C16 H16 . . 120.7 ?
C15 C16 H16 . . 120.7 ?
C16 C17 C18 . . 119.46(19) ?
C16 C17 H17 . . 120.3 ?
C18 C17 H17 . . 120.3 ?
C17 C18 C19 . . 119.6(2) ?
C17 C18 H18 . . 120.2 ?
C19 C18 H18 . . 120.2 ?
N1 C19 C18 . . 120.67(19) ?
N1 C19 C20 . . 115.09(16) ?
C18 C19 C20 . . 124.23(19) ?
N2 C20 C21 . . 121.00(19) ?
N2 C20 C19 . . 115.26(16) ?
C21 C20 C19 . . 123.75(19) ?
C22 C21 C20 . . 118.9(2) ?
C22 C21 H21 . . 120.5 ?
C20 C21 H21 . . 120.5 ?
C23 C22 C21 . . 119.8(2) ?
C23 C22 H22 . . 120.1 ?
C21 C22 H22 . . 120.1 ?
C22 C23 C24 . . 118.7(2) ?
C22 C23 H23 . . 120.7 ?
C24 C23 H23 . . 120.7 ?
N2 C24 C23 . . 122.7(2) ?
N2 C24 H24 . . 118.6 ?
C23 C24 H24 . . 118.6 ?
C15 N1 C19 . . 119.12(16) ?
C15 N1 Ni1 . . 125.65(14) ?
C19 N1 Ni1 . . 114.83(12) ?
C24 N2 C20 . . 118.79(18) ?
C24 N2 Ni1 . . 126.75(14) ?
C20 N2 Ni1 . . 114.19(12) ?
Ni1 O5 H5A . . 108.9(17) ?
Ni1 O5 H5B . . 102.6(18) ?
H5A O5 H5B . . 110.3(14) ?
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 O1 . 2.0290(13) ?
Ni1 N1 . 2.0385(15) ?
Ni1 O5 . 2.0481(14) ?
Ni1 N2 . 2.0682(16) ?
Ni1 O3 3_657 2.0999(13) ?
Ni1 O4 3_657 2.1869(13) ?
Ni1 C14 3_657 2.4733(18) ?
C1 C6 . 1.402(3) ?
C1 C2 . 1.407(2) ?
C1 C7 . 1.506(2) ?
C2 C3 . 1.398(2) ?
C2 S1 . 1.8029(18) ?
C3 C4 . 1.387(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.375(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.375(3) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 O2 . 1.238(2) ?
C7 O1 . 1.265(2) ?
C8 C13 . 1.399(2) ?
C8 C9 . 1.410(2) ?
C8 C14 . 1.493(2) ?
C9 C10 . 1.396(2) ?
C9 S2 . 1.7932(17) ?
C10 C11 . 1.385(3) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.375(3) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.383(3) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
C14 O3 . 1.256(2) ?
C14 O4 . 1.279(2) ?
C14 Ni1 3_657 2.4734(18) ?
O3 Ni1 3_657 2.0999(13) ?
O4 Ni1 3_657 2.1870(13) ?
S1 S2 . 2.0596(8) ?
C15 N1 . 1.335(2) ?
C15 C16 . 1.381(3) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.372(3) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.379(3) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.385(3) ?
C18 H18 . 0.9300 ?
C19 N1 . 1.356(2) ?
C19 C20 . 1.483(3) ?
C20 N2 . 1.345(2) ?
C20 C21 . 1.395(3) ?
C21 C22 . 1.383(3) ?
C21 H21 . 0.9300 ?
C22 C23 . 1.361(4) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.378(3) ?
C23 H23 . 0.9300 ?
C24 N2 . 1.343(2) ?
C24 H24 . 0.9300 ?
O5 H5A . 0.841(9) ?
O5 H5B . 0.850(9) ?
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
O5 H5B O2 . 0.850(9) 1.824(11) 2.646(2) 162(2)
O5 H5A O4 1_655 0.841(9) 1.888(11) 2.7187(18) 169(2)
