#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/21/8102141.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_8102141
loop_
_publ_author_name
'Li, Wen-Hui'
_publ_section_title
;
Crystal structure of bis(4-nitro-2-((3-dimethylamino-propylimino)methyl)-
phenolato)-diisothiocyanato-nickel(II), Ni(C₁₂H₁₇N₃O₃)₂
(NCS)₂
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              255
_journal_page_last               256
_journal_volume                  222
_journal_year                    2007
_chemical_formula_moiety         'C26 H34 N8 Ni O6 S2'
_chemical_formula_structural     Ni(C12H17N3O3)2(NCS)2
_chemical_formula_sum            'C26 H34 N8 Ni O6 S2'
_chemical_formula_weight         677.44
_chemical_name_systematic
; 
bis(4-nitro-2-((3-dimethylaminopropylimino)methyl)phenolato)-
diisothiocyanato-nickel(II) 
;
_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                96.668(5)
_cell_angle_beta                 105.805(5)
_cell_angle_gamma                98.427(5)
_cell_formula_units_Z            1
_cell_length_a                   7.247(2)
_cell_length_b                   10.045(3)
_cell_length_c                   11.324(4)
_cell_measurement_reflns_used    473
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.5
_cell_volume                     774.0(4)
_computing_structure_refinement  'SHELXL-97 [8]'
_computing_structure_solution    'SHELXS-97 [7]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       omega
_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  0.1153
_diffrn_reflns_av_sigmaI/netI    0.2363
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5047
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0699
_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)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                1249
_reflns_number_total             2742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2031.cff
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_database_code               8102141
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 1.0000 0.0000 0.0296(3) Uani 1 1 a d S . .
S1 S 0.2509(3) 1.31883(17) -0.22775(18) 0.0745(7) Uani 1 2 i d . . .
O1 O 0.1240(5) 1.0919(3) 0.1826(3) 0.0321(9) Uani 1 2 i d . . .
O2 O 0.4442(7) 0.6814(4) 0.5199(4) 0.0683(15) Uani 1 2 i d . . .
O3 O 0.3372(6) 0.8038(4) 0.6458(4) 0.0720(15) Uani 1 2 i d . . .
N1 N 0.2294(5) 0.8969(4) 0.0236(4) 0.0251(11) Uani 1 2 i d . . .
N2 N -0.1140(7) 0.6407(4) -0.2191(4) 0.0387(13) Uani 1 2 i d D . .
N3 N 0.3681(7) 0.7771(5) 0.5441(5) 0.0500(15) Uani 1 2 i d . . .
N4 N 0.1591(6) 1.1567(4) -0.0632(4) 0.0413(13) Uani 1 2 i d . . .
C1 C 0.2863(7) 0.9110(5) 0.2479(5) 0.0271(13) Uani 1 2 i d . . .
C2 C 0.1866(7) 1.0192(5) 0.2674(5) 0.0309(14) Uani 1 2 i d . . .
C3 C 0.1676(7) 1.0507(5) 0.3887(5) 0.0380(15) Uani 1 2 i d . . .
H3 H 0.1143 1.1263 0.4077 0.046 Uiso 1 2 i calc R . .
C4 C 0.2256(7) 0.9727(6) 0.4775(5) 0.0410(16) Uani 1 2 i d . . .
H4 H 0.2062 0.9929 0.5550 0.049 Uiso 1 2 i calc R . .
C5 C 0.3133(7) 0.8634(5) 0.4528(5) 0.0303(14) Uani 1 2 i d . . .
C6 C 0.3473(7) 0.8351(5) 0.3384(5) 0.0346(15) Uani 1 2 i d . . .
H6 H 0.4117 0.7643 0.3234 0.042 Uiso 1 2 i calc R . .
C7 C 0.3209(7) 0.8716(5) 0.1287(5) 0.0331(14) Uani 1 2 i d . . .
H7 H 0.4208 0.8227 0.1299 0.040 Uiso 1 2 i calc R . .
C8 C 0.2910(7) 0.8412(5) -0.0834(4) 0.0338(14) Uani 1 2 i d . . .
H8A H 0.4296 0.8743 -0.0673 0.041 Uiso 1 2 i calc R . .
H8B H 0.2223 0.8742 -0.1571 0.041 Uiso 1 2 i calc R . .
C9 C 0.2509(7) 0.6861(5) -0.1080(5) 0.0376(15) Uani 1 2 i d . . .
H9A H 0.2756 0.6565 -0.1860 0.045 Uiso 1 2 i calc R . .
H9B H 0.3439 0.6549 -0.0429 0.045 Uiso 1 2 i calc R . .
C10 C 0.0501(8) 0.6168(5) -0.1146(5) 0.0401(16) Uani 1 2 i d . . .
H10A H 0.0253 0.6464 -0.0367 0.048 Uiso 1 2 i calc R . .
H10B H 0.0479 0.5193 -0.1216 0.048 Uiso 1 2 i calc R . .
C12 C -0.0935(8) 0.5906(5) -0.3442(5) 0.0519(18) Uani 1 2 i d . . .
H12A H -0.0837 0.4960 -0.3502 0.078 Uiso 1 2 i calc R . .
H12B H 0.0219 0.6424 -0.3543 0.078 Uiso 1 2 i calc R . .
H12C H -0.2057 0.6015 -0.4082 0.078 Uiso 1 2 i calc R . .
C11 C -0.3041(7) 0.5764(5) -0.2081(5) 0.0578(19) Uani 1 2 i d . . .
H11A H -0.4069 0.5882 -0.2779 0.087 Uiso 1 2 i calc R . .
H11B H -0.3223 0.6184 -0.1325 0.087 Uiso 1 2 i calc R . .
H11C H -0.3065 0.4808 -0.2067 0.087 Uiso 1 2 i calc R . .
C13 C 0.1984(7) 1.2260(5) -0.1341(5) 0.0346(15) Uani 1 2 i d . . .
H2 H -0.096(8) 0.7313(15) -0.221(5) 0.080 Uiso 1 2 i d D . .
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.000(1) 2_575 . ?
N1 Ni1 O1 92.98(14) 2_575 . ?
N1 Ni1 O1 87.02(14) . . ?
N1 Ni1 O1 87.02(14) 2_575 2_575 ?
N1 Ni1 O1 92.98(14) . 2_575 ?
O1 Ni1 O1 180.00(17) . 2_575 ?
N1 Ni1 N4 90.11(15) 2_575 2_575 ?
N1 Ni1 N4 89.89(15) . 2_575 ?
O1 Ni1 N4 88.31(15) . 2_575 ?
O1 Ni1 N4 91.69(15) 2_575 2_575 ?
N1 Ni1 N4 89.89(15) 2_575 . ?
N1 Ni1 N4 90.11(15) . . ?
O1 Ni1 N4 91.69(15) . . ?
O1 Ni1 N4 88.31(15) 2_575 . ?
N4 Ni1 N4 180.0(2) 2_575 . ?
C2 O1 Ni1 120.0(3) . . ?
C7 N1 C8 115.8(4) . . ?
C7 N1 Ni1 122.7(3) . . ?
C8 N1 Ni1 121.5(3) . . ?
C11 N2 C10 110.5(4) . . ?
C11 N2 C12 110.6(4) . . ?
C10 N2 C12 112.0(4) . . ?
C11 N2 H2 117(4) . . ?
C10 N2 H2 108(4) . . ?
C12 N2 H2 99(4) . . ?
O2 N3 O3 122.2(5) . . ?
O2 N3 C5 119.4(6) . . ?
O3 N3 C5 118.4(6) . . ?
C13 N4 Ni1 157.7(5) . . ?
C6 C1 C2 121.4(5) . . ?
C6 C1 C7 116.7(5) . . ?
C2 C1 C7 121.9(5) . . ?
O1 C2 C1 122.8(5) . . ?
O1 C2 C3 120.5(5) . . ?
C1 C2 C3 116.5(5) . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 N3 120.6(5) . . ?
C6 C5 N3 119.2(5) . . ?
C1 C6 C5 120.1(5) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N1 C7 C1 127.0(5) . . ?
N1 C7 H7 116.5 . . ?
C1 C7 H7 116.5 . . ?
N1 C8 C9 112.4(4) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 116.5(4) . . ?
C10 C9 H9A 108.2 . . ?
C8 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
C8 C9 H9B 108.2 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 N2 116.3(4) . . ?
C9 C10 H10A 108.2 . . ?
N2 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
N2 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C13 S1 179.7(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.058(4) 2_575 ?
Ni1 N1 2.058(4) . ?
Ni1 O1 2.058(3) . ?
Ni1 O1 2.058(3) 2_575 ?
Ni1 N4 2.121(4) 2_575 ?
Ni1 N4 2.121(4) . ?
S1 C13 1.577(6) . ?
O1 C2 1.298(5) . ?
O2 N3 1.217(6) . ?
O3 N3 1.240(6) . ?
N1 C7 1.269(5) . ?
N1 C8 1.480(5) . ?
N2 C11 1.477(6) . ?
N2 C10 1.501(6) . ?
N2 C12 1.502(6) . ?
N2 H2 0.905(10) . ?
N3 C5 1.436(6) . ?
N4 C13 1.186(6) . ?
C1 C6 1.364(6) . ?
C1 C2 1.418(6) . ?
C1 C7 1.460(6) . ?
C2 C3 1.421(6) . ?
C3 C4 1.360(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.521(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.497(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O1 0.905(10) 1.83(3) 2.684(5) 156(5) 2_575
