#------------------------------------------------------------------------------
#$Date: 2017-11-13 07:53:07 +0200 (Mon, 13 Nov 2017) $
#$Revision: 203106 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/67/7056743.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_7056743
loop_
_publ_author_name
'Bharty, M. K.'
'Paswan, Santosh'
'Bharati, P.'
'Sonkar, Piyush Kumar'
'Ganesan, Vellaichamy'
'Butcher, Raymond J.'
_publ_section_title
;
 Square planar Ni(II) complexes of acetone N4-phenyl-thiosemicarbazone and
 in situ generated benzoyl thiosemicarbazide ligand: Synthesis, spectral
 and structural characterizations, thermal behaviour and electrochemical
 studies
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C7NJ01030C
_journal_year                    2017
_chemical_formula_moiety         'C4 H6 N6 Ni S2'
_chemical_formula_sum            'C4 H6 N6 Ni S2'
_chemical_formula_weight         260.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.109(4)
_cell_length_b                   14.882(6)
_cell_length_c                   7.304(4)
_cell_measurement_reflns_used    2121
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.152
_cell_measurement_theta_min      4.012
_cell_volume                     881.4(7)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker Apex 2 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8833
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0255P)²+0.8703P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                850
_reflns_number_total             1282
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj01030c2.cif
_cod_data_source_block           shelx-2
_cod_original_cell_volume        881.3(7)
_cod_database_code               7056743
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;
TITL ups1956bztscnien_0ma in Pbcn
    shelx.res
    created by SHELXL-2016/6 at 12:52:26 on 05-Jul-2017
CELL 0.71073   8.1086  14.8816   7.3036  90.000  90.000  90.000
ZERR    4.00   0.0035   0.0063   0.0040   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, 0.5-Y, 0.5+Z
SYMM -X, Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C  H  N  S  Ni
UNIT 16 24 24 8 4
L.S. 15
ACTA
BOND $H
HTAB
EQIV $2 -x+2, -y+1, -z+1
HTAB N3 N2_$2
EQIV $3 x+1/2, -y+3/2, -z+1
HTAB N3 S1_$3
CONF
TEMP 23.000
WGHT    0.025500    0.870300
FVAR       1.00729
NI1   5    0.500000    0.596593    0.250000    10.50000    0.02995    0.03007 =
         0.04442    0.00000   -0.00373    0.00000
S1    4    0.690502    0.688145    0.338689    11.00000    0.04224    0.03203 =
         0.07481   -0.00218   -0.01415   -0.00156
N1    3    0.640793    0.504137    0.319767    11.00000    0.03129    0.03390 =
         0.04092   -0.00008    0.00033    0.00039
N2    3    0.793758    0.516165    0.396521    11.00000    0.02791    0.03944 =
         0.05302   -0.00142   -0.00697    0.00205
N3    3    0.967549    0.627519    0.491429    11.00000    0.04736    0.04412 =
         0.08812   -0.00431   -0.02440   -0.00213
AFIX  93
H3A   2    1.035979    0.587180    0.528002    11.00000   -1.20000
H3B   2    0.990870    0.683525    0.504553    11.00000   -1.20000
AFIX   0
C1    1    0.581956    0.423309    0.291406    11.00000    0.04245    0.03166 =
         0.05493    0.00296    0.00118    0.00260
H1C   2    0.639382    0.374981    0.319537    11.00000    0.02228
C2    1    0.825496    0.603262    0.414485    11.00000    0.03333    0.04486 =
         0.05019    0.00031   -0.00319    0.00466
 
HKLF 4
 
 
 
 
REM  ups1956bztscnien_0ma in Pbcn
REM R1 =  0.0435 for     850 Fo > 4sig(Fo)  and  0.0802 for all    1282 data
REM     64 parameters refined using      0 restraints
 
END
 
WGHT      0.0251      0.8720
 
REM Instructions for potential hydrogen bonds
HTAB N3 N2_$2
HTAB N3 S1_$3
 
REM Highest difference peak  0.654,  deepest hole -0.343,  1-sigma level  0.092
Q1    1   0.5000  0.3786  0.2500  10.50000  0.05    0.65
Q2    1   1.0604  0.5081  0.5063  11.00000  0.05    0.42
Q3    1   0.7182  0.4527  0.3146  11.00000  0.05    0.37
Q4    1   0.6230  0.6626  0.4050  11.00000  0.05    0.35
Q5    1   0.8482  0.6709  0.4232  11.00000  0.05    0.35
Q6    1   0.5801  0.6689  0.2547  11.00000  0.05    0.34
Q7    1   0.5000  0.6874  0.2500  10.50000  0.05    0.31
Q8    1   0.7944  0.6331  0.3567  11.00000  0.05    0.30
Q9    1   0.5000  0.5465  0.2500  10.50000  0.05    0.30
Q10   1   0.8990  0.4765  0.3837  11.00000  0.05    0.29
Q11   1   0.6341  0.3985  0.3791  11.00000  0.05    0.29
Q12   1   0.5828  0.3288  0.3162  11.00000  0.05    0.28
Q13   1   0.6765  0.7507  0.4170  11.00000  0.05    0.28
Q14   1   0.5986  0.7216  0.3102  11.00000  0.05    0.28
Q15   1   0.7164  0.3855  0.3099  11.00000  0.05    0.27
Q16   1   0.8606  0.5243  0.4180  11.00000  0.05    0.27
Q17   1   0.5387  0.6059  0.4163  11.00000  0.05    0.26
Q18   1   0.8873  0.6098  0.4443  11.00000  0.05    0.26
Q19   1   0.6415  0.4783  0.2415  11.00000  0.05    0.26
Q20   1   0.5103  0.3584  0.3873  11.00000  0.05    0.26
;
_shelx_res_checksum              53513
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.500000 0.59659(3) 0.250000 0.03482(19) Uani 1 2 d S T P
S1 S 0.69050(11) 0.68815(5) 0.33869(14) 0.0497(3) Uani 1 1 d . . .
N1 N 0.6408(3) 0.50414(16) 0.3198(4) 0.0354(6) Uani 1 1 d . . .
N2 N 0.7938(3) 0.51616(17) 0.3965(4) 0.0401(7) Uani 1 1 d . . .
N3 N 0.9675(3) 0.6275(2) 0.4914(5) 0.0599(9) Uani 1 1 d . . .
H3A H 1.035979 0.587180 0.528002 0.072 Uiso 1 1 calc R U .
H3B H 0.990870 0.683525 0.504553 0.072 Uiso 1 1 calc R U .
C1 C 0.5820(4) 0.4233(2) 0.2914(5) 0.0430(8) Uani 1 1 d . . .
H1C H 0.639(3) 0.3750(18) 0.320(4) 0.022(7) Uiso 1 1 d . . .
C2 C 0.8255(4) 0.6033(2) 0.4145(5) 0.0428(8) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0300(3) 0.0301(3) 0.0444(3) 0.000 -0.0037(3) 0.000
S1 0.0422(5) 0.0320(4) 0.0748(7) -0.0022(4) -0.0141(4) -0.0016(4)
N1 0.0313(13) 0.0339(14) 0.0409(14) -0.0001(11) 0.0003(11) 0.0004(11)
N2 0.0279(13) 0.0394(16) 0.0530(18) -0.0014(12) -0.0070(12) 0.0021(12)
N3 0.0474(19) 0.0441(16) 0.088(2) -0.0043(16) -0.0244(16) -0.0021(14)
C1 0.0425(19) 0.0317(18) 0.055(2) 0.0030(14) 0.0012(15) 0.0026(15)
C2 0.0333(17) 0.045(2) 0.050(2) 0.0003(16) -0.0032(15) 0.0047(15)
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
N1 Ni1 N1 84.52(15) . 3_655
N1 Ni1 S1 86.87(8) . .
N1 Ni1 S1 171.33(8) 3_655 .
N1 Ni1 S1 171.33(8) . 3_655
N1 Ni1 S1 86.87(8) 3_655 3_655
S1 Ni1 S1 101.75(6) . 3_655
C2 S1 Ni1 94.96(12) . .
C1 N1 N2 120.9(3) . .
C1 N1 Ni1 114.4(2) . .
N2 N1 Ni1 124.77(19) . .
C2 N2 N1 110.0(2) . .
C2 N3 H3A 120.0 . .
C2 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
N1 C1 C1 113.38(18) . 3_655
N1 C1 H1C 121.3(18) . .
C1 C1 H1C 125.3(17) 3_655 .
N2 C2 N3 118.3(3) . .
N2 C2 S1 123.3(2) . .
N3 C2 S1 118.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.859(2) .
Ni1 N1 1.859(2) 3_655
Ni1 S1 2.1592(11) .
Ni1 S1 2.1592(10) 3_655
S1 C2 1.761(3) .
N1 C1 1.310(4) .
N1 N2 1.373(3) .
N2 C2 1.328(4) .
N3 C2 1.331(4) .
N3 H3A 0.8600 .
N3 H3B 0.8600 .
C1 C1 1.460(7) 3_655
C1 H1C 0.88(3) .
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
N3 H3A N2 0.86 2.14 2.998(4) 176.7 5_766
N3 H3B S1 0.86 2.75 3.512(3) 148.0 4_566
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_1
_geom_torsion_site_symmetry_4
N1 Ni1 N1 C1 -0.25(18) 3_655 .
S1 Ni1 N1 C1 -179.2(2) . .
N1 Ni1 N1 N2 -179.7(3) 3_655 .
S1 Ni1 N1 N2 1.3(2) . .
C1 N1 N2 C2 -179.0(3) . .
Ni1 N1 N2 C2 0.4(4) . .
N2 N1 C1 C1 -179.9(3) . 3_655
Ni1 N1 C1 C1 0.7(5) . 3_655
N1 N2 C2 N3 178.3(3) . .
N1 N2 C2 S1 -2.7(4) . .
Ni1 S1 C2 N2 3.2(3) . .
Ni1 S1 C2 N3 -177.7(3) . .
