#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/28/1512801.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_1512801
loop_
_publ_author_name
'Tarlok S. Lobana'
'Poonam Kumari'
'Geeta Hundal'
'Ray J. Butcher'
'A. Castineiras'
'Takashiro Akitsu'
_publ_section_title
;
 Metal derivatives of N1-substituted thiosemicarbazones: Synthesis,
 structures and spectroscopy of nickel(II) and cobalt(III) complexes
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              605
_journal_page_last               615
_journal_paper_doi               10.1016/j.ica.2012.09.021
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C18 H20 N6 Ni S2'
_chemical_formula_sum            'C18 H20 N6 Ni S2'
_chemical_formula_weight         443.23
_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                90.00
_cell_angle_beta                 109.480(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.749(5)
_cell_length_b                   7.474(4)
_cell_length_c                   14.628(5)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     2035.6(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'SHELXTL-PC (Sheldrick, 1993)'
_computing_molecular_graphics
'ORTEP,Mercury(Farrugia,1997;Bruno et.al.,2002)'
_computing_publication_material  'WINGX,(Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altamore et. al., 1992)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1946
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         2.19
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et. al., 1968'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0463
_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)+(0.0716P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                1371
_reflns_number_total             1889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-605-615-1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1512801
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_calc_flag
_atom_site_refinement_flags
C1 C 0.4833(2) 0.2425(6) 0.4249(4) 0.0576(12) Uani 1 1 d .
H1 H 0.4455 0.2346 0.3666 0.069 Uiso 1 1 calc R
C2 C 0.5535(3) 0.2310(8) 0.4260(5) 0.0789(18) Uani 1 1 d .
H2 H 0.5621 0.2149 0.3678 0.095 Uiso 1 1 calc R
C3 C 0.6104(3) 0.2423(7) 0.5096(5) 0.0745(17) Uani 1 1 d .
H3 H 0.6570 0.2332 0.5084 0.089 Uiso 1 1 calc R
C4 C 0.5983(2) 0.2675(7) 0.5961(5) 0.0720(17) Uani 1 1 d .
H4 H 0.6367 0.2753 0.6538 0.086 Uiso 1 1 calc R
C5 C 0.5283(2) 0.2809(6) 0.5962(4) 0.0565(13) Uani 1 1 d .
H5 H 0.5204 0.3005 0.6546 0.068 Uiso 1 1 calc R
C6 C 0.4693(2) 0.2659(5) 0.5113(3) 0.0391(9) Uani 1 1 d .
C7 C 0.3991(2) 0.2787(5) 0.5241(3) 0.0373(9) Uani 1 1 d .
H7 H 0.4009 0.3152 0.5856 0.045 Uiso 1 1 calc R
C8 C 0.27328(18) 0.1004(5) 0.3305(3) 0.0326(8) Uani 1 1 d .
C9 C 0.3162(2) 0.0576(6) 0.1934(3) 0.0525(11) Uani 1 1 d .
H9A H 0.3002 -0.0016 0.1316 0.079 Uiso 1 1 calc R
H9B H 0.3616 0.0086 0.2324 0.079 Uiso 1 1 calc R
H9C H 0.3215 0.1833 0.1840 0.079 Uiso 1 1 calc R
N1 N 0.33472(16) 0.2482(4) 0.4651(2) 0.0325(7) Uani 1 1 d .
N2 N 0.33001(16) 0.1993(4) 0.3704(2) 0.0347(7) Uani 1 1 d .
N3 N 0.26366(17) 0.0310(5) 0.2420(2) 0.0429(8) Uani 1 1 d .
H31 H 0.2285 -0.0349 0.2197 0.051 Uiso 1 1 d .
S1 S 0.20990(5) 0.05016(15) 0.38593(8) 0.0422(3) Uani 1 1 d .
Ni Ni 0.2500 0.2500 0.5000 0.0301(2) Uani 1 2 d S
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C6 119.9(5) . .
C2 C1 H1 120.0 . .
C6 C1 H1 120.0 . .
C3 C2 C1 122.0(6) . .
C3 C2 H2 119.0 . .
C1 C2 H2 119.0 . .
C2 C3 C4 119.4(5) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C3 C4 C5 119.3(5) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C4 C5 C6 122.0(5) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
C1 C6 C5 117.3(4) . .
C1 C6 C7 127.4(4) . .
C5 C6 C7 115.3(4) . .
N1 C7 C6 131.7(4) . .
N1 C7 H7 114.2 . .
C6 C7 H7 114.2 . .
N2 C8 N3 118.1(3) . .
N2 C8 S1 123.8(3) . .
N3 C8 S1 118.1(3) . .
N3 C9 H9A 109.5 . .
N3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 N1 N2 115.4(3) . .
C7 N1 Ni 125.0(3) . .
N2 N1 Ni 119.4(2) . .
C8 N2 N1 110.6(3) . .
C8 N3 C9 121.5(3) . .
C8 N3 H31 116.1 . .
C9 N3 H31 122.2 . .
C8 S1 Ni 94.26(13) . .
N1 Ni N1 180.000(1) 7_556 .
N1 Ni S1 94.74(9) 7_556 .
N1 Ni S1 85.26(9) . .
N1 Ni S1 85.26(9) 7_556 7_556
N1 Ni S1 94.74(9) . 7_556
S1 Ni S1 180.0 . 7_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.384(6) .
C1 C6 1.391(6) .
C1 H1 0.9300 .
C2 C3 1.359(9) .
C2 H2 0.9300 .
C3 C4 1.375(9) .
C3 H3 0.9300 .
C4 C5 1.388(6) .
C4 H4 0.9300 .
C5 C6 1.394(6) .
C5 H5 0.9300 .
C6 C7 1.463(5) .
C7 N1 1.296(5) .
C7 H7 0.9300 .
C8 N2 1.306(4) .
C8 N3 1.348(5) .
C8 S1 1.744(4) .
C9 N3 1.454(5) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
N1 N2 1.405(4) .
N1 Ni 1.906(3) .
N3 H31 0.8248 .
S1 Ni 2.1819(13) .
Ni N1 1.906(3) 7_556
Ni S1 2.1819(13) 7_556
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
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 -0.2(8) .
C1 C2 C3 C4 -0.5(9) .
C2 C3 C4 C5 -0.1(8) .
C3 C4 C5 C6 1.4(8) .
C2 C1 C6 C5 1.4(7) .
C2 C1 C6 C7 -179.2(4) .
C4 C5 C6 C1 -2.1(7) .
C4 C5 C6 C7 178.5(4) .
C1 C6 C7 N1 10.8(7) .
C5 C6 C7 N1 -169.8(4) .
C6 C7 N1 N2 -2.3(6) .
C6 C7 N1 Ni 173.4(3) .
N3 C8 N2 N1 -175.2(3) .
S1 C8 N2 N1 3.8(4) .
C7 N1 N2 C8 152.5(3) .
Ni N1 N2 C8 -23.4(4) .
N2 C8 N3 C9 2.8(6) .
S1 C8 N3 C9 -176.3(3) .
N2 C8 S1 Ni 12.6(3) .
N3 C8 S1 Ni -168.3(3) .
C7 N1 Ni S1 -149.3(3) .
N2 N1 Ni S1 26.2(2) .
C7 N1 Ni S1 30.7(3) 7_556
N2 N1 Ni S1 -153.8(2) 7_556
C8 S1 Ni N1 162.45(15) 7_556
C8 S1 Ni N1 -17.55(15) .
