#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/65/2206532.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_2206532
loop_
_publ_author_name
'Fa-Qian Liu'
'Fang-Fang Jian'
'Guang-Ye Liu'
'Lu-De Lu'
'Xu-Jie Yang'
'Xin Wang'
_publ_section_title
Diisothiocyanatotetrakis(1-methyl-1H-imidazole-κN³)nickel(II)
_journal_coeditor_code           RZ6101
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1568
_journal_page_last               m1570
_journal_paper_doi               10.1107/S1600536805021987
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ni (N C S)2 (C4 H6 N2)4]'
_chemical_formula_moiety         'C18 H24 N10 Ni S2'
_chemical_formula_sum            'C18 H24 N10 Ni S2'
_chemical_formula_weight         503.30
_chemical_name_systematic
;
Diisothiocyanatotetrakis(1-methyl-1H-imidazole-\kN³)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                 94.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.002(2)
_cell_length_b                   15.300(3)
_cell_length_c                   14.309(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      4
_cell_volume                     2401.9(8)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'NRCVAX (Gabe et al., 1989)'
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick, 1990)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5451
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.479
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0515
_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)+(0.051P)²+3.586P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                2901
_reflns_number_total             5188
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rz6101.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      'P 21/c'
_cod_database_code               2206532
_cod_database_fobs_code          2206532
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_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_type_symbol
Ni1 0.24111(5) 0.12729(4) 0.24373(4) 0.03989(19) Uani d . 1 Ni
S1 -0.10041(18) 0.12590(15) 0.43860(17) 0.1146(8) Uani d . 1 S
S2 0.54720(15) 0.15052(11) 0.01688(11) 0.0750(5) Uani d . 1 S
N1 0.2354(4) -0.1493(3) 0.2771(4) 0.0649(13) Uani d . 1 N
N2 0.2524(4) -0.0108(3) 0.2457(3) 0.0506(10) Uani d . 1 N
N3 0.4667(3) 0.1190(3) 0.4974(3) 0.0533(10) Uani d . 1 N
N4 0.3764(3) 0.1302(2) 0.3556(3) 0.0464(9) Uani d . 1 N
N5 0.2726(4) 0.4047(3) 0.2754(3) 0.0565(11) Uani d . 1 N
N6 0.2328(3) 0.2663(2) 0.2396(3) 0.0474(9) Uani d . 1 N
N7 0.0160(3) 0.1258(3) -0.0106(3) 0.0506(10) Uani d . 1 N
N8 0.1062(3) 0.1191(3) 0.1311(3) 0.0482(9) Uani d . 1 N
N9 0.1053(4) 0.1245(3) 0.3384(3) 0.0560(10) Uani d . 1 N
N10 0.3747(4) 0.1329(3) 0.1481(3) 0.0587(11) Uani d . 1 N
C1 0.1933(7) -0.2271(5) 0.3221(5) 0.105(2) Uani d . 1 C
H1A 0.2620 -0.2628 0.3424 0.158 Uiso calc R 1 H
H1B 0.1400 -0.2592 0.2784 0.158 Uiso calc R 1 H
H1C 0.1501 -0.2108 0.3752 0.158 Uiso calc R 1 H
C2 0.3058(5) -0.1481(4) 0.2065(5) 0.0788(18) Uani d . 1 C
H2A 0.3405 -0.1950 0.1770 0.095 Uiso calc R 1 H
C3 0.3151(5) -0.0617(4) 0.1872(4) 0.0651(15) Uani d . 1 C
H3A 0.3593 -0.0395 0.1396 0.078 Uiso calc R 1 H
C4 0.2028(5) -0.0665(4) 0.3017(4) 0.0640(15) Uani d . 1 C
H4A 0.1540 -0.0521 0.3498 0.077 Uiso calc R 1 H
C5 0.4829(5) 0.1170(4) 0.5995(4) 0.0793(18) Uani d . 1 C
H5A 0.4050 0.1098 0.6247 0.119 Uiso calc R 1 H
H5B 0.5192 0.1708 0.6219 0.119 Uiso calc R 1 H
H5C 0.5350 0.0691 0.6190 0.119 Uiso calc R 1 H
C6 0.5561(5) 0.1212(4) 0.4380(4) 0.0700(16) Uani d . 1 C
H6A 0.6395 0.1177 0.4538 0.084 Uiso calc R 1 H
C7 0.5002(4) 0.1293(4) 0.3502(4) 0.0605(14) Uani d . 1 C
H7A 0.5399 0.1337 0.2953 0.073 Uiso calc R 1 H
C8 0.3608(4) 0.1248(3) 0.4456(3) 0.0536(12) Uani d . 1 C
H8A 0.2850 0.1249 0.4703 0.064 Uiso calc R 1 H
C9 0.3274(5) 0.4809(4) 0.3255(5) 0.0831(19) Uani d . 1 C
H9A 0.3462 0.4660 0.3902 0.125 Uiso calc R 1 H
H9B 0.2709 0.5288 0.3212 0.125 Uiso calc R 1 H
H9C 0.4008 0.4974 0.2978 0.125 Uiso calc R 1 H
C10 0.1875(5) 0.4043(4) 0.2007(4) 0.0625(14) Uani d . 1 C
H10A 0.1526 0.4529 0.1703 0.075 Uiso calc R 1 H
C11 0.1639(5) 0.3192(3) 0.1794(4) 0.0570(13) Uani d . 1 C
H11A 0.1092 0.2998 0.1312 0.068 Uiso calc R 1 H
C12 0.2969(4) 0.3207(3) 0.2962(4) 0.0517(12) Uani d . 1 C
H12A 0.3524 0.3027 0.3446 0.062 Uiso calc R 1 H
C13 0.0000(5) 0.1386(4) -0.1124(3) 0.0739(17) Uani d . 1 C
H13A -0.0654 0.1791 -0.1270 0.111 Uiso calc R 1 H
H13B -0.0189 0.0837 -0.1425 0.111 Uiso calc R 1 H
H13C 0.0740 0.1615 -0.1345 0.111 Uiso calc R 1 H
C14 -0.0706(5) 0.1064(4) 0.0466(4) 0.0709(17) Uani d . 1 C
H14A -0.1532 0.0983 0.0301 0.085 Uiso calc R 1 H
C15 -0.0136(5) 0.1009(4) 0.1334(4) 0.0677(16) Uani d . 1 C
H15A -0.0516 0.0865 0.1872 0.081 Uiso calc R 1 H
C16 0.1205(4) 0.1331(4) 0.0426(3) 0.0562(13) Uani d . 1 C
H16A 0.1949 0.1466 0.0193 0.067 Uiso calc R 1 H
C17 0.0218(4) 0.1250(3) 0.3801(3) 0.0525(12) Uani d . 1 C
C18 0.4460(4) 0.1399(3) 0.0939(3) 0.0449(11) Uani d . 1 C
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'
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
_geom_angle_publ_flag
N10 Ni1 N9 178.63(17) y
N10 Ni1 N4 90.26(15) y
N9 Ni1 N4 90.40(15) y
N10 Ni1 N8 89.51(15) y
N9 Ni1 N8 89.87(15) y
N4 Ni1 N8 177.80(15) y
N10 Ni1 N2 90.35(17) y
N9 Ni1 N2 90.87(17) y
N4 Ni1 N2 88.48(14) y
N8 Ni1 N2 89.33(15) y
N10 Ni1 N6 88.39(16) y
N9 Ni1 N6 90.39(16) y
N4 Ni1 N6 91.51(15) y
N8 Ni1 N6 90.68(15) y
N2 Ni1 N6 178.74(15) y
C2 N1 C4 111.3(5) ?
C2 N1 C1 125.3(6) ?
C4 N1 C1 123.3(6) ?
C4 N2 C3 104.7(5) ?
C4 N2 Ni1 128.9(4) ?
C3 N2 Ni1 126.3(4) ?
C8 N3 C6 107.2(4) ?
C8 N3 C5 126.4(5) ?
C6 N3 C5 126.3(4) ?
C8 N4 C7 104.9(4) ?
C8 N4 Ni1 127.4(3) ?
C7 N4 Ni1 127.4(3) ?
C12 N5 C10 106.4(4) ?
C12 N5 C9 125.6(5) ?
C10 N5 C9 128.0(5) ?
C12 N6 C11 104.9(4) ?
C12 N6 Ni1 126.2(3) ?
C11 N6 Ni1 128.9(3) ?
C14 N7 C16 107.0(4) ?
C14 N7 C13 126.9(4) ?
C16 N7 C13 126.1(4) ?
C16 N8 C15 104.3(4) ?
C16 N8 Ni1 127.0(3) ?
C15 N8 Ni1 128.7(3) ?
C17 N9 Ni1 171.3(4) ?
C18 N10 Ni1 176.5(4) ?
N1 C1 H1A 109.5 ?
N1 C1 H1B 109.5 ?
H1A C1 H1B 109.5 ?
N1 C1 H1C 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
N1 C2 C3 103.1(5) ?
N1 C2 H2A 128.4 ?
C3 C2 H2A 128.4 ?
C2 C3 N2 112.5(6) ?
C2 C3 H3A 123.8 ?
N2 C3 H3A 123.8 ?
N2 C4 N1 108.3(5) ?
N2 C4 H4A 125.8 ?
N1 C4 H4A 125.8 ?
N3 C5 H5A 109.5 ?
N3 C5 H5B 109.5 ?
H5A C5 H5B 109.5 ?
N3 C5 H5C 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
N3 C6 C7 106.5(4) ?
N3 C6 H6A 126.8 ?
C7 C6 H6A 126.8 ?
C6 C7 N4 109.4(5) ?
C6 C7 H7A 125.3 ?
N4 C7 H7A 125.3 ?
N4 C8 N3 112.1(4) ?
N4 C8 H8A 124.0 ?
N3 C8 H8A 124.0 ?
N5 C9 H9A 109.5 ?
N5 C9 H9B 109.5 ?
H9A C9 H9B 109.5 ?
N5 C9 H9C 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
C11 C10 N5 106.7(5) ?
C11 C10 H10A 126.6 ?
N5 C10 H10A 126.6 ?
C10 C11 N6 109.8(5) ?
C10 C11 H11A 125.1 ?
N6 C11 H11A 125.1 ?
N6 C12 N5 112.2(4) ?
N6 C12 H12A 123.9 ?
N5 C12 H12A 123.9 ?
N7 C13 H13A 109.5 ?
N7 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
N7 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
N7 C14 C15 105.9(4) ?
N7 C14 H14A 127.0 ?
C15 C14 H14A 127.0 ?
N8 C15 C14 110.6(5) ?
N8 C15 H15A 124.7 ?
C14 C15 H15A 124.7 ?
N8 C16 N7 112.2(4) ?
N8 C16 H16A 123.9 ?
N7 C16 H16A 123.9 ?
N9 C17 S1 178.9(5) y
N10 C18 S2 179.7(5) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N10 2.083(4) y
Ni1 N9 2.091(4) y
Ni1 N4 2.103(4) y
Ni1 N8 2.112(4) y
Ni1 N2 2.116(4) y
Ni1 N6 2.129(4) y
S1 C17 1.635(5) y
S2 C18 1.632(5) y
N1 C2 1.319(8) ?
N1 C4 1.370(7) ?
N1 C1 1.445(8) ?
N2 C4 1.316(7) ?
N2 C3 1.367(6) ?
N3 C8 1.336(5) ?
N3 C6 1.348(6) ?
N3 C5 1.459(6) ?
N4 C8 1.314(6) ?
N4 C7 1.370(6) ?
N5 C12 1.342(6) ?
N5 C10 1.368(7) ?
N5 C9 1.473(7) ?
N6 C12 1.327(6) ?
N6 C11 1.370(6) ?
N7 C14 1.334(6) ?
N7 C16 1.336(6) ?
N7 C13 1.468(6) ?
N8 C16 1.305(6) ?
N8 C15 1.350(6) ?
N9 C17 1.133(6) y
N10 C18 1.148(6) y
C1 H1A 0.9600 ?
C1 H1B 0.9600 ?
C1 H1C 0.9600 ?
C2 C3 1.355(8) ?
C2 H2A 0.9300 ?
C3 H3A 0.9300 ?
C4 H4A 0.9300 ?
C5 H5A 0.9600 ?
C5 H5B 0.9600 ?
C5 H5C 0.9600 ?
C6 C7 1.362(7) ?
C6 H6A 0.9300 ?
C7 H7A 0.9300 ?
C8 H8A 0.9300 ?
C9 H9A 0.9600 ?
C9 H9B 0.9600 ?
C9 H9C 0.9600 ?
C10 C11 1.358(7) ?
C10 H10A 0.9300 ?
C11 H11A 0.9300 ?
C12 H12A 0.9300 ?
C13 H13A 0.9600 ?
C13 H13B 0.9600 ?
C13 H13C 0.9600 ?
C14 C15 1.351(7) ?
C14 H14A 0.9300 ?
C15 H15A 0.9300 ?
C16 H16A 0.9300 ?
