#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/27/2012765.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012765
loop_
_publ_author_name
'Novaković, Sladjana B.'
'Tomić, Zoran D.'
'Jevtović, Violeta'
'Leovac, Vukadin M.'
_publ_section_title
;
 Transition metal complexes with thiosemicarbazide-based ligands.
 XLIII.
 Chlorobis(3-methylisothiosemicarbazide-κ²N¹,N⁴)zinc(II)
 chloride
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m358
_journal_page_last               m360
_journal_paper_doi               10.1107/S0108270102007564
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Zn (C2 H7 N3 S)2 Cl]Cl'
_chemical_formula_moiety         'C4 H14 Cl N6 S2 Zn + , Cl -'
_chemical_formula_sum            'C4 H14 Cl2 N6 S2 Zn'
_chemical_formula_weight         346.6
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.402(2)
_cell_length_b                   10.121(3)
_cell_length_c                   13.710(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.36
_cell_measurement_theta_min      12.78
_cell_volume                     1304.6(6)
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1988)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.095
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4392
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.592
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.63
_refine_ls_abs_structure_details 'Flack (1983); 1561 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0311P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.124
_reflns_number_gt                1913
_reflns_number_total             3730
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na1563.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P21 21 21'
_cod_database_code               2012765
_cod_database_fobs_code          2012765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn1 -0.47341(9) 0.05028(9) 0.18476(6) 0.0271(2) Uani d . 1 . . Zn
Cl2 -0.6464(2) -0.2407(2) 0.00274(14) 0.0350(5) Uani d . 1 . . Cl
Cl1 -0.2997(2) -0.0478(3) 0.27754(14) 0.0428(5) Uani d . 1 . . Cl
S5 -0.3392(3) 0.3251(2) -0.06148(17) 0.0533(7) Uani d . 1 . . S
S5A -0.9001(2) -0.0853(3) 0.30246(19) 0.0603(8) Uani d . 1 . . S
N1A -0.5795(6) 0.1589(5) 0.3075(5) 0.0317(15) Uani d . 1 . . N
H1A -0.5211 0.1648 0.3593 0.038 Uiso calc R 1 . . H
H2A -0.6044 0.2409 0.2888 0.038 Uiso calc R 1 . . H
N1 -0.3901(6) -0.0309(6) 0.0454(4) 0.0318(15) Uani d . 1 . . N
H1 -0.3144 -0.0832 0.0565 0.038 Uiso calc R 1 . . H
H2 -0.4575 -0.0786 0.0148 0.038 Uiso calc R 1 . . H
N2A -0.7008(7) 0.0836(7) 0.3306(4) 0.0429(19) Uani d . 1 . . N
H3A -0.7514 0.1015 0.3812 0.051 Uiso calc R 1 . . H
N4A -0.6539(6) -0.0504(6) 0.2006(4) 0.0288(13) Uani d . 1 . . N
H4A -0.6763 -0.1136 0.1617 0.035 Uiso calc R 1 . . H
N2 -0.3510(7) 0.0786(6) -0.0113(4) 0.0339(16) Uani d . 1 . . N
H3 -0.3054 0.0687 -0.0652 0.041 Uiso calc R 1 . . H
N4 -0.4465(7) 0.2119(6) 0.1043(4) 0.0327(17) Uani d . 1 . . N
H4 -0.4741 0.2879 0.1249 0.039 Uiso calc R 1 . . H
C3 -0.3868(8) 0.1993(7) 0.0211(5) 0.0276(18) Uani d . 1 . . C
C3A -0.7351(8) -0.0169(8) 0.2713(5) 0.031(2) Uani d . 1 . . C
C6A -0.9100(9) -0.2271(7) 0.2271(6) 0.059(3) Uani d . 1 . . C
H7A -0.9982 -0.2722 0.2389 0.089 Uiso calc R 1 . . H
H6A -0.8321 -0.2851 0.2418 0.089 Uiso calc R 1 . . H
H5A -0.9051 -0.2009 0.1599 0.089 Uiso calc R 1 . . H
C6 -0.4660(11) 0.4497(9) -0.0355(6) 0.073(3) Uani d . 1 . . C
H7 -0.4494 0.5246 -0.0770 0.110 Uiso calc R 1 . . H
H5 -0.4574 0.4761 0.0315 0.110 Uiso calc R 1 . . H
H6 -0.5600 0.4160 -0.0470 0.110 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zn1 0.0301(4) 0.0274(4) 0.0236(4) -0.0014(5) 0.0034(4) 0.0023(5)
Cl2 0.0416(12) 0.0316(10) 0.0319(10) -0.0055(10) -0.0091(10) -0.0007(9)
Cl1 0.0499(13) 0.0415(12) 0.0370(11) 0.0050(13) -0.0206(9) -0.0001(12)
S5 0.0642(17) 0.0463(14) 0.0494(14) 0.0109(14) 0.0268(13) 0.0209(12)
S5A 0.0338(12) 0.0766(19) 0.0705(17) -0.0203(13) 0.0231(13) -0.0226(16)
N1A 0.040(4) 0.027(3) 0.028(3) -0.007(3) -0.001(3) -0.003(3)
N1 0.034(4) 0.024(4) 0.037(4) -0.001(3) 0.004(3) 0.000(3)
N2A 0.040(4) 0.058(5) 0.030(4) -0.014(4) 0.020(3) -0.021(4)
N4A 0.031(3) 0.027(3) 0.028(3) 0.001(3) 0.006(3) -0.005(3)
N2 0.044(4) 0.035(4) 0.023(3) 0.005(4) 0.011(3) 0.005(3)
N4 0.049(5) 0.025(3) 0.024(3) -0.002(3) 0.015(3) -0.001(3)
C3 0.028(4) 0.027(4) 0.028(4) -0.002(4) 0.000(4) 0.009(3)
C3A 0.030(4) 0.034(5) 0.028(4) 0.000(4) -0.004(4) 0.000(4)
C6A 0.065(7) 0.039(6) 0.073(7) -0.025(5) -0.003(6) 0.003(5)
C6 0.109(8) 0.055(6) 0.057(6) 0.036(8) 0.030(6) 0.019(6)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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_publ_flag
N4 Zn1 N4A 126.2(2) yes
N4 Zn1 N1 77.4(2) yes
N4A Zn1 N1 101.8(2) yes
N4 Zn1 N1A 94.0(2) yes
N4A Zn1 N1A 77.9(2) yes
N1 Zn1 N1A 169.3(2) yes
N4 Zn1 Cl1 124.9(2) yes
N4A Zn1 Cl1 108.9(2) yes
N1 Zn1 Cl1 93.8(2) yes
N1A Zn1 Cl1 96.5(2) yes
C3 S5 C6 102.4(4) no
C3A S5A C6A 103.0(4) no
N2A N1A Zn1 105.3(4) no
N2A N1A H1A 110.7 no
Zn1 N1A H1A 110.7 no
N2A N1A H2A 110.7 no
Zn1 N1A H2A 110.7 no
H1A N1A H2A 108.8 no
N2 N1 Zn1 106.1(4) no
N2 N1 H1 110.5 no
Zn1 N1 H1 110.5 no
N2 N1 H2 110.5 no
Zn1 N1 H2 110.5 no
H1 N1 H2 108.7 no
C3A N2A N1A 117.9(6) no
C3A N2A H3A 121.0 no
N1A N2A H3A 121.0 no
C3A N4A Zn1 117.1(5) no
C3A N4A H4A 121.4 no
Zn1 N4A H4A 121.4 no
C3 N2 N1 118.0(6) no
C3 N2 H3 121.0 no
N1 N2 H3 121.0 no
C3 N4 Zn1 118.0(5) no
C3 N4 H4 121.0 no
Zn1 N4 H4 121.0 no
N4 C3 N2 119.7(7) no
N4 C3 S5 127.8(6) no
N2 C3 S5 112.4(6) no
N4A C3A N2A 121.1(7) no
N4A C3A S5A 127.5(6) no
N2A C3A S5A 111.4(6) no
S5A C6A H7A 109.5 no
S5A C6A H6A 109.5 no
H7A C6A H6A 109.5 no
S5A C6A H5A 109.5 no
H7A C6A H5A 109.5 no
H6A C6A H5A 109.5 no
S5 C6 H7 109.5 no
S5 C6 H5 109.5 no
H7 C6 H5 109.5 no
S5 C6 H6 109.5 no
H7 C6 H6 109.5 no
H5 C6 H6 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N4 . 1.989(6) yes
Zn1 N4A . 1.991(6) yes
Zn1 N1 . 2.223(5) yes
Zn1 N1A . 2.244(6) yes
Zn1 Cl1 . 2.296(2) yes
S5 C3 . 1.761(8) no
S5 C6 . 1.772(9) no
S5A C3A . 1.752(8) no
S5A C6A . 1.771(8) no
N1A N2A . 1.407(7) no
N1A H1A . 0.9000 no
N1A H2A . 0.9000 no
N1 N2 . 1.403(8) no
N1 H1 . 0.9000 no
N1 H2 . 0.9000 no
N2A C3A . 1.342(9) no
N2A H3A . 0.8600 no
N4A C3A . 1.279(8) no
N4A H4A . 0.8600 no
N2 C3 . 1.343(9) no
N2 H3 . 0.8600 no
N4 C3 . 1.278(8) no
N4 H4 . 0.8600 no
C6A H7A . 0.9600 no
C6A H6A . 0.9600 no
C6A H5A . 0.9600 no
C6 H7 . 0.9600 no
C6 H5 . 0.9600 no
C6 H6 . 0.9600 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N4A H4A Cl2 . 0.86 2.55 3.328(6) 152 yes
N2 H3 Cl1 2_454 0.86 2.38 3.238(6) 174 yes
N2A H3A Cl2 2_355 0.86 2.38 3.188(7) 156 yes
N1 H1 Cl2 3_545 0.90 2.52 3.321(6) 149 yes
N1A H2A Cl1 4_455 0.90 2.49 3.385(6) 172 yes
N1 H2 Cl2 . 0.90 2.42 3.265(6) 156 yes
N1A H1A Cl2 4_455 0.90 2.64 3.509(6) 162 yes
