#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/68/2226891.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_2226891
loop_
_publ_author_name
'Monim-ul-Mehboob, Muhammad'
'Akkurt, Mehmet'
'Khan, Islam Ullah'
'Sharif, Shahzad'
'Asif, Iram'
'Ahmad, Saeed'
_publ_section_title
;
 Hexakis(thiourea-κS)nickel(II) nitrate: a redetermination
;
_journal_coeditor_code           HB5527
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i57
_journal_page_last               i58
_journal_paper_doi               10.1107/S1600536810026668
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C H4 N2 S)6] (N O3)2'
_chemical_formula_moiety         'C6 H24 N12 Ni S6 2+, 2(N O3 -)'
_chemical_formula_sum            'C6 H24 N14 Ni O6 S6'
_chemical_formula_weight         639.50
_chemical_name_common
;
Hexakis(thiourea-κS)nickel(II) nitrate
;
_chemical_name_systematic
;
Hexakis(thiourea-κS)nickel(II) dinitrate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 129.7240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4433(6)
_cell_length_b                   9.2398(3)
_cell_length_c                   16.3136(5)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.51
_cell_volume                     2601.96(14)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11568
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0299
_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)+(0.0256P)²+1.7568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                2542
_reflns_number_total             3129
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb5527.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2226891
_cod_database_fobs_code          2226891
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+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_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ni Ni1 0.25000 0.25000 0.00000 0.02460(10) Uani . . 1.000
S S1 0.38321(3) 0.34540(6) 0.10478(4) 0.0362(2) Uani . . 1.000
S S2 0.28084(3) -0.01160(5) 0.01164(4) 0.03310(10) Uani . . 1.000
S S3 0.28343(3) 0.27376(5) 0.17786(4) 0.03110(10) Uani . . 1.000
N N1 0.49791(11) 0.3572(3) 0.10299(17) 0.0630(8) Uani . . 1.000
N N2 0.42272(13) 0.1592(2) 0.02330(19) 0.0630(9) Uani . . 1.000
N N3 0.40567(10) 0.00546(19) 0.21644(13) 0.0475(6) Uani . . 1.000
N N4 0.36277(12) -0.2195(2) 0.14917(16) 0.0621(7) Uani . . 1.000
N N5 0.20704(11) 0.0325(2) 0.14718(15) 0.0516(7) Uani . . 1.000
N N6 0.29045(13) 0.1162(2) 0.31643(15) 0.0687(8) Uani . . 1.000
C C1 0.43826(11) 0.2808(2) 0.07398(16) 0.0341(6) Uani . . 1.000
C C2 0.35527(11) -0.0788(2) 0.13536(15) 0.0324(6) Uani . . 1.000
C C3 0.25769(12) 0.1293(2) 0.21517(16) 0.0363(7) Uani . . 1.000
O O1 0.41450(9) 0.6847(2) -0.02032(13) 0.0604(6) Uani . . 1.000
O O2 0.50573(11) 0.6706(2) 0.14802(14) 0.0786(7) Uani . . 1.000
O O3 0.48990(11) 0.86552(19) 0.06598(15) 0.0676(7) Uani . . 1.000
N N7 0.46952(10) 0.7413(2) 0.06486(15) 0.0429(6) Uani . . 1.000
H H1A 0.52660 0.32720 0.08860 0.0940 Uiso calc R 1.000
H H1B 0.50850 0.43750 0.13650 0.0940 Uiso calc R 1.000
H H2A 0.45170 0.12990 0.00920 0.0940 Uiso calc R 1.000
H H2B 0.38350 0.10840 0.00400 0.0940 Uiso calc R 1.000
H H3A 0.44270 -0.03180 0.27720 0.0570 Uiso calc R 1.000
H H3B 0.40160 0.09790 0.20880 0.0570 Uiso calc R 1.000
H H4A 0.40020 -0.25490 0.21050 0.0930 Uiso calc R 1.000
H H4B 0.33030 -0.27630 0.09690 0.0930 Uiso calc R 1.000
H H5A 0.19560 -0.03860 0.16890 0.0620 Uiso calc R 1.000
H H5B 0.18520 0.03990 0.08080 0.0620 Uiso calc R 1.000
H H6A 0.27850 0.04460 0.33710 0.0820 Uiso calc R 1.000
H H6B 0.32380 0.17910 0.36190 0.0820 Uiso calc R 1.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Ni1 S2 . . . 98.00(2) no
S1 Ni1 S3 . . . 80.37(2) no
S1 Ni1 S1 . . 7_555 180.00 no
S1 Ni1 S2 . . 7_555 82.00(2) no
S1 Ni1 S3 . . 7_555 99.63(2) no
S2 Ni1 S3 . . . 97.72(2) no
S1 Ni1 S2 7_555 . . 82.00(2) no
S2 Ni1 S2 . . 7_555 180.00 no
S2 Ni1 S3 . . 7_555 82.28(2) no
S1 Ni1 S3 7_555 . . 99.63(2) no
S2 Ni1 S3 7_555 . . 82.28(2) no
S3 Ni1 S3 . . 7_555 180.00 no
S1 Ni1 S2 7_555 . 7_555 98.00(2) no
S1 Ni1 S3 7_555 . 7_555 80.37(2) no
S2 Ni1 S3 7_555 . 7_555 97.72(2) no
Ni1 S1 C1 . . . 116.99(8) no
Ni1 S2 C2 . . . 117.12(7) no
Ni1 S3 C3 . . . 115.14(7) no
C1 N1 H1B . . . 120.00 no
H1A N1 H1B . . . 120.00 no
C1 N1 H1A . . . 120.00 no
H2A N2 H2B . . . 120.00 no
C1 N2 H2A . . . 120.00 no
C1 N2 H2B . . . 120.00 no
C2 N3 H3B . . . 120.00 no
C2 N3 H3A . . . 120.00 no
H3A N3 H3B . . . 120.00 no
C2 N4 H4B . . . 120.00 no
C2 N4 H4A . . . 120.00 no
H4A N4 H4B . . . 120.00 no
H5A N5 H5B . . . 120.00 no
C3 N5 H5A . . . 120.00 no
C3 N5 H5B . . . 120.00 no
C3 N6 H6B . . . 120.00 no
H6A N6 H6B . . . 120.00 no
C3 N6 H6A . . . 120.00 no
O2 N7 O3 . . . 120.0(2) no
O1 N7 O2 . . . 119.6(2) no
O1 N7 O3 . . . 120.29(19) no
S1 C1 N2 . . . 122.4(2) no
S1 C1 N1 . . . 118.06(18) no
N1 C1 N2 . . . 119.5(3) no
S2 C2 N4 . . . 118.85(16) no
S2 C2 N3 . . . 122.36(15) no
N3 C2 N4 . . . 118.78(19) no
N5 C3 N6 . . . 119.2(2) no
S3 C3 N5 . . . 122.62(17) no
S3 C3 N6 . . . 118.22(17) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 S1 . . 2.4708(7) y
Ni1 S2 . . 2.4879(5) y
Ni1 S3 . . 2.4995(6) y
Ni1 S1 . 7_555 2.4708(7) no
Ni1 S2 . 7_555 2.4879(5) no
Ni1 S3 . 7_555 2.4995(6) no
S1 C1 . . 1.711(3) no
S2 C2 . . 1.715(2) no
S3 C3 . . 1.713(2) no
O1 N7 . . 1.239(3) no
O2 N7 . . 1.232(3) no
O3 N7 . . 1.231(3) no
N1 C1 . . 1.306(4) no
N2 C1 . . 1.304(3) no
N3 C2 . . 1.313(3) no
N4 C2 . . 1.312(3) no
N5 C3 . . 1.308(3) no
N6 C3 . . 1.316(3) no
N1 H1B . . 0.8600 no
N1 H1A . . 0.8600 no
N2 H2A . . 0.8600 no
N2 H2B . . 0.8600 no
N3 H3A . . 0.8600 no
N3 H3B . . 0.8600 no
N4 H4B . . 0.8600 no
N4 H4A . . 0.8600 no
N5 H5A . . 0.8600 no
N5 H5B . . 0.8600 no
N6 H6A . . 0.8600 no
N6 H6B . . 0.8600 no
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
N1 H1A O1 3_665 0.86 2.21 3.037(4) 161 yes
N1 H1B O2 . 0.86 2.17 2.965(3) 154 yes
N2 H2A O3 1_545 0.86 2.56 2.963(3) 110 yes
N2 H2A O3 3_665 0.86 2.30 3.110(4) 157 yes
N2 H2B S2 . 0.86 2.63 3.449(3) 159 yes
N3 H3A O3 2_645 0.86 2.19 3.022(2) 163 yes
N3 H3B S1 . 0.86 2.72 3.5021(19) 152 yes
N3 H3B S3 . 0.86 2.87 3.444(2) 126 yes
N4 H4A O2 2_645 0.86 2.01 2.865(3) 175 yes
N4 H4B S2 7_545 0.86 2.75 3.555(2) 157 yes
N5 H5A S3 6_545 0.86 2.82 3.623(2) 155 yes
N5 H5A O1 7_555 0.86 2.48 2.922(3) 113 yes
N5 H5B S1 7_555 0.86 2.59 3.410(2) 160 yes
N6 H6A S2 4_555 0.86 2.83 3.464(3) 132 yes
N6 H6A S3 6_545 0.86 2.80 3.601(2) 156 yes
N6 H6B O1 4_565 0.86 2.10 2.958(3) 174 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
S2 Ni1 S1 C1 . . . . 47.38(8) no
S3 Ni1 S1 C1 . . . . 143.91(8) no
S2 Ni1 S1 C1 7_555 . . . -132.62(8) no
S3 Ni1 S1 C1 7_555 . . . -36.09(8) no
S1 Ni1 S2 C2 . . . . 48.29(12) no
S3 Ni1 S2 C2 . . . . -33.00(12) no
S1 Ni1 S2 C2 7_555 . . . -131.71(12) no
S3 Ni1 S2 C2 7_555 . . . 147.00(12) no
S1 Ni1 S3 C3 . . . . -135.52(11) no
S2 Ni1 S3 C3 . . . . -38.66(11) no
S1 Ni1 S3 C3 7_555 . . . 44.48(11) no
S2 Ni1 S3 C3 7_555 . . . 141.34(11) no
Ni1 S1 C1 N1 . . . . 159.63(16) no
Ni1 S1 C1 N2 . . . . -20.5(2) no
Ni1 S2 C2 N3 . . . . -15.4(3) no
Ni1 S2 C2 N4 . . . . 165.6(2) no
Ni1 S3 C3 N5 . . . . -17.6(3) no
Ni1 S3 C3 N6 . . . . 162.5(2) no
