#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/74/2217468.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_2217468
loop_
_publ_author_name
'Ping Liu'
'Dong-Sheng Deng'
_publ_section_title
;
 Tetraaquadiimidazolenickel(II) naphthalene-1,5-disulfonate
;
_journal_coeditor_code           CV2373
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m275
_journal_page_last               m275
_journal_paper_doi               10.1107/S1600536807067761
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C3 H4 N2)2 (H2 O)4] (C10 H6 O6 S2)'
_chemical_formula_moiety         'C6 H16 N4 Ni O4 2+, C10 H6 O6 S2 2-'
_chemical_formula_sum            'C16 H22 N4 Ni O10 S2'
_chemical_formula_weight         553.21
_chemical_name_systematic
;
Tetraaquadiimidazolenickel(II) naphthalene-1,5-disulfonate
;
_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                107.705(5)
_cell_angle_beta                 101.628(5)
_cell_angle_gamma                111.967(5)
_cell_formula_units_Z            1
_cell_length_a                   8.285(3)
_cell_length_b                   8.925(3)
_cell_length_c                   9.088(3)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.52
_cell_volume                     554.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1K 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  0.0111
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4834
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.7900
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2499
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0240
_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)+(0.0346P)²+0.1772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                2262
_reflns_number_total             2499
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2373.cif
_cod_data_source_block           I
_cod_database_code               2217468
_cod_database_fobs_code          2217468
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
Ni Ni1 0.5000 0.5000 0.5000 0.02611(9) Uani d S 1
N N1 0.28615(18) 0.55991(17) 0.43827(16) 0.0318(3) Uani d . 1
O O1W 0.31627(16) 0.23254(16) 0.43179(17) 0.0400(3) Uani d D 1
O O2W 0.50259(17) 0.42911(17) 0.25854(14) 0.0370(3) Uani d D 1
S S1 0.21612(5) 0.14229(5) 0.81936(4) 0.02708(10) Uani d . 1
C C1 0.41626(19) 0.11368(19) 0.88348(17) 0.0259(3) Uani d . 1
C C5 0.41915(19) 0.01134(18) 0.97747(17) 0.0248(3) Uani d . 1
O O3 0.06491(16) -0.03557(16) 0.71539(15) 0.0406(3) Uani d . 1
O O2 0.18864(17) 0.22940(17) 0.96754(15) 0.0407(3) Uani d . 1
O O1 0.25746(18) 0.25029(18) 0.72669(17) 0.0436(3) Uani d . 1
N N2 0.1179(2) 0.6991(2) 0.4648(2) 0.0478(4) Uani d . 1
H H7A 0.0826 0.7757 0.5081 0.057 Uiso calc R 1
C C2 0.5648(2) 0.1890(2) 0.8392(2) 0.0353(3) Uani d . 1
H H2A 0.5610 0.2560 0.7789 0.042 Uiso calc R 1
C C3 0.7231(2) 0.1653(2) 0.8846(2) 0.0390(4) Uani d . 1
H H3A 0.8235 0.2169 0.8541 0.047 Uiso calc R 1
C C7 0.0278(3) 0.5634(3) 0.3116(3) 0.0449(4) Uani d . 1
H H2B -0.0831 0.5350 0.2335 0.054 Uiso calc R 1
C C8 0.1323(2) 0.4782(2) 0.2957(2) 0.0384(4) Uani d . 1
H H8A 0.1045 0.3792 0.2025 0.046 Uiso calc R 1
C C6 0.2709(3) 0.6926(3) 0.5365(2) 0.0459(4) Uani d . 1
H H6A 0.3560 0.7719 0.6425 0.055 Uiso calc R 1
C C4 0.7313(2) 0.0678(2) 0.9726(2) 0.0317(3) Uani d . 1
H H4A 0.8366 0.0526 1.0006 0.038 Uiso calc R 1
H H2WA 0.570(3) 0.510(2) 0.241(3) 0.057(7) Uiso d D 1
H H2WB 0.402(3) 0.368(3) 0.176(3) 0.054(6) Uiso d D 1
H H1WA 0.215(2) 0.179(3) 0.357(2) 0.062(7) Uiso d D 1
H H1WB 0.302(3) 0.211(4) 0.511(2) 0.075(9) 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
N1 Ni1 N1 2_666 . 180.0
N1 Ni1 O2W 2_666 2_666 91.34(5)
N1 Ni1 O2W . 2_666 88.66(5)
N1 Ni1 O2W 2_666 . 88.66(5)
N1 Ni1 O2W . . 91.34(5)
O2W Ni1 O2W 2_666 . 180.0
N1 Ni1 O1W 2_666 . 87.22(6)
N1 Ni1 O1W . . 92.78(6)
O2W Ni1 O1W 2_666 . 91.48(5)
O2W Ni1 O1W . . 88.52(5)
N1 Ni1 O1W 2_666 2_666 92.78(6)
N1 Ni1 O1W . 2_666 87.22(6)
O2W Ni1 O1W 2_666 2_666 88.52(5)
O2W Ni1 O1W . 2_666 91.48(5)
O1W Ni1 O1W . 2_666 180.0
C6 N1 C8 . . 104.96(14)
C6 N1 Ni1 . . 124.39(12)
C8 N1 Ni1 . . 130.65(11)
Ni1 O1W H1WA . . 122.5(16)
Ni1 O1W H1WB . . 113.1(19)
H1WA O1W H1WB . . 107.7(19)
Ni1 O2W H2WA . . 115.4(16)
Ni1 O2W H2WB . . 121.1(15)
H2WA O2W H2WB . . 106.8(18)
O2 S1 O3 . . 113.08(8)
O2 S1 O1 . . 112.57(8)
O3 S1 O1 . . 111.83(8)
O2 S1 C1 . . 106.98(7)
O3 S1 C1 . . 105.41(7)
O1 S1 C1 . . 106.33(7)
C2 C1 C5 . . 121.07(13)
C2 C1 S1 . . 118.79(12)
C5 C1 S1 . . 120.14(10)
C4 C5 C5 2_657 2_657 119.05(17)
C4 C5 C1 2_657 . 122.89(13)
C5 C5 C1 2_657 . 118.05(16)
C6 N2 C7 . . 107.87(15)
C6 N2 H7A . . 126.1
C7 N2 H7A . . 126.1
C1 C2 C3 . . 120.14(15)
C1 C2 H2A . . 119.9
C3 C2 H2A . . 119.9
C4 C3 C2 . . 120.80(14)
C4 C3 H3A . . 119.6
C2 C3 H3A . . 119.6
C8 C7 N2 . . 105.88(16)
C8 C7 H2B . . 127.1
N2 C7 H2B . . 127.1
C7 C8 N1 . . 109.81(16)
C7 C8 H8A . . 125.1
N1 C8 H8A . . 125.1
N1 C6 N2 . . 111.48(16)
N1 C6 H6A . . 124.3
N2 C6 H6A . . 124.3
C3 C4 C5 . 2_657 120.88(14)
C3 C4 H4A . . 119.6
C5 C4 H4A 2_657 . 119.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 N1 2_666 2.0568(14)
Ni1 N1 . 2.0568(14)
Ni1 O2W 2_666 2.0979(13)
Ni1 O2W . 2.0979(13)
Ni1 O1W . 2.0978(13)
Ni1 O1W 2_666 2.0978(13)
N1 C6 . 1.315(2)
N1 C8 . 1.378(2)
O1W H1WA . 0.82(2)
O1W H1WB . 0.82(2)
O2W H2WA . 0.81(2)
O2W H2WB . 0.81(2)
S1 O2 . 1.4453(12)
S1 O3 . 1.4508(13)
S1 O1 . 1.4556(13)
S1 C1 . 1.7811(15)
C1 C2 . 1.369(2)
C1 C5 . 1.431(2)
C5 C4 2_657 1.422(2)
C5 C5 2_657 1.427(3)
N2 C6 . 1.334(2)
N2 C7 . 1.357(3)
N2 H7A . 0.8600
C2 C3 . 1.407(2)
C2 H2A . 0.9300
C3 C4 . 1.359(2)
C3 H3A . 0.9300
C7 C8 . 1.351(2)
C7 H2B . 0.9300
C8 H8A . 0.9300
C6 H6A . 0.9300
C4 C5 2_657 1.422(2)
C4 H4A . 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 O3 2_556 0.82(2) 2.022(15) 2.7507(18) 148(2)
O1W H1WB O1 . 0.82(2) 2.018(14) 2.788(2) 156(3)
O2W H2WA O1 2_666 0.81(2) 1.962(10) 2.7496(19) 161(2)
O2W H2WB O2 1_554 0.81(2) 1.96(2) 2.7979(18) 173(2)
N2 H7A O3 1_565 0.86 2.19 2.981(2) 153.8
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_4
_geom_torsion
O2W Ni1 N1 C6 2_666 . 37.27(15)
O2W Ni1 N1 C6 . . -142.73(15)
O1W Ni1 N1 C6 . . 128.69(15)
O1W Ni1 N1 C6 2_666 . -51.31(15)
O2W Ni1 N1 C8 2_666 . -142.13(15)
O2W Ni1 N1 C8 . . 37.87(15)
O1W Ni1 N1 C8 . . -50.71(15)
O1W Ni1 N1 C8 2_666 . 129.29(15)
O2 S1 C1 C2 . . -121.03(14)
O3 S1 C1 C2 . . 118.35(14)
O1 S1 C1 C2 . . -0.52(15)
O2 S1 C1 C5 . . 59.89(13)
O3 S1 C1 C5 . . -60.73(13)
O1 S1 C1 C5 . . -179.60(12)
C2 C1 C5 C4 . 2_657 179.40(15)
S1 C1 C5 C4 . 2_657 -1.5(2)
C2 C1 C5 C5 . 2_657 -0.5(2)
S1 C1 C5 C5 . 2_657 178.52(13)
C5 C1 C2 C3 . . 0.6(2)
S1 C1 C2 C3 . . -178.51(14)
C1 C2 C3 C4 . . 0.0(3)
C6 N2 C7 C8 . . -0.1(2)
N2 C7 C8 N1 . . 0.2(2)
C6 N1 C8 C7 . . -0.1(2)
Ni1 N1 C8 C7 . . 179.38(12)
C8 N1 C6 N2 . . 0.0(2)
Ni1 N1 C6 N2 . . -179.51(12)
C7 N2 C6 N1 . . 0.1(2)
C2 C3 C4 C5 . 2_657 -0.6(3)
