#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:04:06 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229764 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/57/7045793.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_7045793
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         'C11 H13 N3 O S'
_chemical_formula_sum            'C11 H13 N3 O S'
_chemical_formula_weight         235.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-01 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                99.804(8)
_cell_angle_beta                 91.409(7)
_cell_angle_gamma                109.424(8)
_cell_formula_units_Z            2
_cell_length_a                   5.9381(5)
_cell_length_b                   6.2676(6)
_cell_length_c                   17.4543(17)
_cell_measurement_reflns_used    1378
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.15
_cell_measurement_theta_min      3.48
_cell_volume                     601.38(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0200
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.486
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       Needle
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0456
_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)+(0.0800P)²+0.0100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1577
_reflns_number_total             2129
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00453f2.cif
_cod_data_source_block           Lmethoxy
_cod_depositor_comments
'Adding full bibliography for 7045785--7045793.cif.'
_cod_database_code               7045793
_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'
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
S1 S -0.27539(13) -0.45581(11) 0.24810(4) 0.0635(3) Uani 1 1 d . .
O1 O 0.3194(3) 0.2130(3) 0.02549(10) 0.0621(5) Uani 1 1 d . .
N1 N 0.1237(3) -0.0922(3) 0.30508(11) 0.0438(5) Uani 1 1 d . .
N3 N -0.0454(4) -0.2997(4) 0.39426(14) 0.0606(6) Uani 1 1 d . .
N2 N 0.1306(4) -0.1396(4) 0.43091(13) 0.0617(6) Uani 1 1 d . .
C7 C -0.0610(4) -0.2783(4) 0.31213(14) 0.0478(6) Uani 1 1 d . .
C1 C 0.1755(4) -0.0073(4) 0.23407(13) 0.0413(6) Uani 1 1 d . .
C4 C 0.2667(4) 0.1502(4) 0.09556(13) 0.0435(6) Uani 1 1 d . .
C3 C 0.3833(4) 0.0103(4) 0.11895(14) 0.0473(6) Uani 1 1 d . .
H3 H 0.4940 -0.0294 0.0881 0.057 Uiso 1 1 calc R U
C5 C 0.1071(5) 0.2139(4) 0.14292(15) 0.0516(7) Uani 1 1 d . .
H5 H 0.0307 0.3103 0.1283 0.062 Uiso 1 1 calc R U
C6 C 0.0620(4) 0.1338(4) 0.21176(15) 0.0504(7) Uani 1 1 d . .
H6 H -0.0460 0.1756 0.2434 0.060 Uiso 1 1 calc R U
C8 C 0.2619(4) 0.0169(4) 0.38024(14) 0.0511(7) Uani 1 1 d . .
C2 C 0.3365(4) -0.0696(4) 0.18706(14) 0.0459(6) Uani 1 1 d . .
H2 H 0.4128 -0.1658 0.2018 0.055 Uiso 1 1 calc R U
C9 C 0.2498(5) 0.2557(5) 0.40915(16) 0.0705(9) Uani 1 1 d . .
H9A H 0.3338 0.3583 0.3761 0.106 Uiso 1 1 calc R U
H9B H 0.3226 0.3122 0.4617 0.106 Uiso 1 1 calc R U
H9C H 0.0852 0.2472 0.4079 0.106 Uiso 1 1 calc R U
C10 C 0.5173(5) 0.0180(6) 0.37997(16) 0.0719(9) Uani 1 1 d . .
H10A H 0.5162 -0.1372 0.3659 0.108 Uiso 1 1 calc R U
H10B H 0.5988 0.0856 0.4310 0.108 Uiso 1 1 calc R U
H10C H 0.5986 0.1064 0.3428 0.108 Uiso 1 1 calc R U
C11 C 0.1967(6) 0.3498(5) -0.00218(18) 0.0689(8) Uani 1 1 d . .
H11A H 0.0268 0.2738 -0.0031 0.103 Uiso 1 1 calc R U
H11B H 0.2379 0.3701 -0.0539 0.103 Uiso 1 1 calc R U
H11C H 0.2428 0.4976 0.0319 0.103 Uiso 1 1 calc R U
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C4 O1 C11 117.6(2)
C7 N1 C1 124.7(2)
C7 N1 C8 110.72(19)
C1 N1 C8 124.53(18)
N2 N3 C7 110.0(2)
N3 N2 C8 111.9(2)
N1 C7 N3 106.1(2)
N1 C7 S1 131.0(2)
N3 C7 S1 122.85(18)
C6 C1 C2 119.8(2)
C6 C1 N1 119.9(2)
C2 C1 N1 120.4(2)
O1 C4 C5 124.8(2)
O1 C4 C3 115.7(2)
C5 C4 C3 119.5(2)
C2 C3 C4 120.4(2)
C6 C5 C4 119.7(2)
C1 C6 C5 120.5(2)
N1 C8 N2 101.21(19)
N1 C8 C10 112.5(2)
N2 C8 C10 109.1(2)
N1 C8 C9 112.0(2)
N2 C8 C9 109.0(2)
C10 C8 C9 112.3(2)
C3 C2 C1 120.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C7 1.635(3)
O1 C4 1.360(3)
O1 C11 1.428(3)
N1 C7 1.335(3)
N1 C1 1.431(3)
N1 C8 1.460(3)
N3 N2 1.249(3)
N3 C7 1.466(3)
N2 C8 1.474(3)
C1 C6 1.375(3)
C1 C2 1.384(3)
C4 C5 1.385(3)
C4 C3 1.388(3)
C3 C2 1.367(3)
C5 C6 1.378(3)
C8 C10 1.514(4)
C8 C9 1.522(4)
