#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:04:06 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229764 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/57/7045786.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_7045786
loop_
_publ_author_name
'Tarai, Arup'
'Baruah, Jubaraj B.'
_publ_section_title
;
 Four-coordinated see-saw
 N-(aryl)-2-(propan-2-ylidene)hydrazinecarbothioamide complexes of
 nickel(ii), copper(ii) and zinc(ii) and their propensity for catalytic
 cyclisation.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4921
_journal_page_last               4930
_journal_paper_doi               10.1039/C8DT00453F
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H22 N8 Ni O4 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C26 H36 N10 Ni O6 S2'
_chemical_formula_weight         707.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.580(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.826(3)
_cell_length_b                   7.8808(7)
_cell_length_c                   17.1929(15)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.63
_cell_measurement_theta_min      2.70
_cell_volume                     3310.8(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8506
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.667
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       Block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0100P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1616
_reflns_number_total             2907
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00453f2.cif
_cod_data_source_block           corr
_cod_depositor_comments
'Adding full bibliography for 7045785--7045793.cif.'
_cod_database_code               7045786
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.0000 -0.01388(7) 0.2500 0.0521(3) Uani 1 2 d S T P
S1 S 0.03598(4) -0.19753(10) 0.20006(8) 0.0612(4) Uani 1 1 d . . .
C4 C 0.05817(14) -0.0479(4) 0.1495(3) 0.0490(12) Uani 1 1 d . . .
C5 C 0.11292(16) -0.0187(5) 0.0696(3) 0.0530(12) Uani 1 1 d . . .
C3 C -0.02589(15) 0.2745(5) 0.1311(3) 0.0487(12) Uani 1 1 d . . .
C6 C 0.15365(17) -0.0980(5) 0.0574(3) 0.0645(14) Uani 1 1 d . . .
H6 H 0.1661 -0.2045 0.0822 0.077 Uiso 1 1 calc R U .
C8 C 0.15663(17) 0.1338(6) -0.0281(3) 0.0586(13) Uani 1 1 d . . .
C2 C -0.01909(14) 0.3827(4) 0.0649(3) 0.0649(13) Uani 1 1 d . . .
H2A H 0.0159 0.4378 0.0934 0.097 Uiso 1 1 calc R U .
H2B H -0.0475 0.4666 0.0413 0.097 Uiso 1 1 calc R U .
H2C H -0.0213 0.3124 0.0176 0.097 Uiso 1 1 calc R U .
C7 C 0.17575(16) -0.0228(5) 0.0098(3) 0.0695(14) Uani 1 1 d . . .
H7 H 0.2033 -0.0768 0.0032 0.083 Uiso 1 1 calc R U .
C10 C 0.09390(16) 0.1387(5) 0.0284(3) 0.0710(15) Uani 1 1 d . . .
H10 H 0.0662 0.1942 0.0340 0.085 Uiso 1 1 calc R U .
C13 C 0.22292(15) 0.3227(5) 0.2007(3) 0.0792(15) Uani 1 1 d . . .
H13A H 0.2152 0.4092 0.1570 0.119 Uiso 1 1 calc R U .
H13B H 0.2167 0.2131 0.1732 0.119 Uiso 1 1 calc R U .
H13C H 0.2604 0.3315 0.2459 0.119 Uiso 1 1 calc R U .
C9 C 0.11563(18) 0.2115(5) -0.0198(3) 0.0776(15) Uani 1 1 d . . .
H9 H 0.1023 0.3154 -0.0474 0.093 Uiso 1 1 calc R U .
C12 C 0.19128(15) 0.2221(5) 0.3054(3) 0.0948(18) Uani 1 1 d . . .
H12A H 0.1705 0.2617 0.3331 0.142 Uiso 1 1 calc R U .
H12B H 0.2289 0.2086 0.3494 0.142 Uiso 1 1 calc R U .
H12C H 0.1770 0.1150 0.2772 0.142 Uiso 1 1 calc R U .
C11 C 0.15068(17) 0.4678(5) 0.2125(3) 0.0769(16) Uani 1 1 d . . .
H11 H 0.1286 0.4767 0.2393 0.092 Uiso 1 1 calc R U .
C1 C -0.07000(14) 0.3233(4) 0.1525(3) 0.0706(14) Uani 1 1 d . . .
H1A H -0.0775 0.2299 0.1809 0.106 Uiso 1 1 calc R U .
H1B H -0.1025 0.3520 0.0989 0.106 Uiso 1 1 calc R U .
H1C H -0.0583 0.4195 0.1916 0.106 Uiso 1 1 calc R U .
N2 N 0.04320(12) 0.1107(3) 0.1373(2) 0.0538(10) Uani 1 1 d . . .
N1 N 0.00502(12) 0.1420(3) 0.1681(2) 0.0460(9) Uani 1 1 d . . .
N3 N 0.09348(13) -0.1037(4) 0.1202(2) 0.0560(10) Uani 1 1 d . . .
H3 H 0.1053 -0.2056 0.1353 0.067 Uiso 1 1 calc R U .
N5 N 0.18749(14) 0.3443(4) 0.2399(2) 0.0619(11) Uani 1 1 d . . .
N4 N 0.18047(16) 0.2162(6) -0.0775(3) 0.0809(14) Uani 1 1 d . . .
O3 O 0.14333(12) 0.5718(3) 0.1543(2) 0.0895(12) Uani 1 1 d . . .
O1 O 0.16884(12) 0.3669(4) -0.0980(2) 0.1038(13) Uani 1 1 d . . .
O2 O 0.21223(14) 0.1389(4) -0.0939(3) 0.1065(13) Uani 1 1 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'
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'
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 100.63(18) 2 .
N1 Ni1 S1 158.37(9) 2 .
N1 Ni1 S1 85.81(10) . .
N1 Ni1 S1 85.81(10) 2 2
N1 Ni1 S1 158.37(9) . 2
S1 Ni1 S1 95.76(6) . 2
C4 S1 Ni1 95.00(14) . .
N2 C4 N3 118.6(4) . .
N2 C4 S1 124.5(4) . .
N3 C4 S1 116.9(3) . .
C6 C5 N3 117.6(4) . .
C6 C5 C10 117.3(5) . .
N3 C5 C10 125.1(4) . .
N1 C3 C1 120.9(4) . .
N1 C3 C2 121.9(4) . .
C1 C3 C2 117.2(3) . .
C7 C6 C5 121.6(4) . .
C9 C8 C7 120.4(5) . .
C9 C8 N4 119.9(4) . .
C7 C8 N4 119.6(5) . .
C6 C7 C8 119.2(4) . .
C9 C10 C5 120.6(4) . .
C8 C9 C10 120.8(4) . .
O3 C11 N5 125.2(5) . .
C4 N2 N1 110.2(3) . .
C3 N1 N2 113.2(3) . .
C3 N1 Ni1 127.2(3) . .
N2 N1 Ni1 119.5(2) . .
C4 N3 C5 129.3(3) . .
C11 N5 C13 120.3(4) . .
C11 N5 C12 121.4(4) . .
C13 N5 C12 118.2(3) . .
O2 N4 O1 122.5(5) . .
O2 N4 C8 119.8(4) . .
O1 N4 C8 117.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.923(3) 2
Ni1 N1 1.923(3) .
Ni1 S1 2.1579(11) .
Ni1 S1 2.1580(11) 2
S1 C4 1.744(4) .
C4 N2 1.302(4) .
C4 N3 1.373(5) .
C5 C6 1.396(5) .
C5 N3 1.396(5) .
C5 C10 1.401(5) .
C3 N1 1.308(4) .
C3 C1 1.491(5) .
C3 C2 1.505(5) .
C6 C7 1.371(5) .
C8 C9 1.361(5) .
C8 C7 1.378(5) .
C8 N4 1.457(6) .
C10 C9 1.364(5) .
C13 N5 1.445(5) .
C12 N5 1.448(5) .
C11 O3 1.232(5) .
C11 N5 1.325(4) .
N2 N1 1.417(4) .
N4 O2 1.212(4) .
N4 O1 1.237(4) .
