#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/90/2009036.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_2009036
loop_
_publ_author_name
'Yu-Peng Tian'
'Jie-Ying Wu'
'Fu-Xin Xie'
'S. Shanmuga Sundara Raj'
'Ping Yang'
'Hoong-Kun Fun'
_publ_section_title
;
 Dichlorobis(dimethylformamide-O)bis(4-nitrobenzaldehyde
 thiosemicarbazone-S)cadmium(II)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1641
_journal_page_last               1644
_journal_paper_doi               10.1107/S010827019900815X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Cd Cl2 (C3 H7 N O)2 (C8 H8 N4 O2 S)2]'
_chemical_formula_sum            'C22 H30 Cd Cl2 N10 O6 S2'
_chemical_formula_weight         777.98
_chemical_name_systematic
;
Dichlorobis(dimethylformamide-O)bis(4-nitrobenzaldehyde thiosemicarbazone-S)
cadmium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.8100(10)
_cell_angle_beta                 111.1920(10)
_cell_angle_gamma                105.2500(10)
_cell_formula_units_Z            1
_cell_length_a                   8.8298(3)
_cell_length_b                   9.6918(3)
_cell_length_c                   10.5786(3)
_cell_measurement_reflns_used    6425
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.21
_cell_measurement_theta_min      2.63
_cell_volume                     787.04(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PARST (Nardelli, 1995)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5228
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.572
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.025
_refine_ls_R_factor_gt           0.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0393P)²+0.1231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                3352
_reflns_number_total             3530
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            na1428.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2009036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cd1 0 0 0.5 .02642(8) Uani d S 1 . . Cd
S1 .03084(6) -.26821(5) 0.51240(6) .03954(12) Uani d . 1 . . S
Cl1 .23244(6) .07938(5) 0.40594(5) .03887(11) Uani d . 1 . . Cl
O1 1.2195(2) -.5134(3) 0.8638(3) .0809(6) Uani d . 1 . . O
O2 1.1003(3) -.7067(3) 0.9188(2) .0734(6) Uani d . 1 . . O
O3 -.22520(18) -.09599(17) 0.27273(14) .0432(3) Uani d . 1 . . O
N1 1.0951(3) -.6008(2) 0.8681(2) .0521(5) Uani d . 1 . . N
N2 .43398(19) -.39246(17) 0.63636(16) .0333(3) Uani d . 1 . . N
N3 .2695(2) -.38761(17) 0.59393(18) .0370(3) Uani d . 1 . . N
H3B .1866 -.4628 0.5872 .044 Uiso calc R 1 . . H
N4 .3668(2) -.15181(19) 0.5750(2) .0406(4) Uani d . 1 . . N
H4A .4693 -.1564 0.6024 .049 Uiso calc R 1 . . H
H4B .3488 -.0727 0.5555 .049 Uiso calc R 1 . . H
N5 -.3113(2) -.0907(2) 0.04488(17) .0455(4) Uani d . 1 . . N
C1 .6171(2) -.5347(2) 0.70785(18) .0323(3) Uani d . 1 . . C
C2 .7665(3) -.4233(2) 0.7294(2) .0415(4) Uani d . 1 . . C
H2A .7606 -.3339 0.7093 .050 Uiso calc R 1 . . H
C3 .9239(3) -.4448(2) 0.7806(2) .0441(4) Uani d . 1 . . C
H3A 1.0247 -.3709 0.7951 .053 Uiso calc R 1 . . H
C4 .9275(2) -.5786(2) 0.8096(2) .0381(4) Uani d . 1 . . C
C5 .7816(3) -.6925(2) 0.7852(2) .0447(5) Uani d . 1 . . C
H5A .7882 -.7826 0.8031 .054 Uiso calc R 1 . . H
C6 .6251(3) -.6705(2) 0.7336(2) .0415(4) Uani d . 1 . . C
H6A .5244 -.7464 0.7159 .050 Uiso calc R 1 . . H
C7 .4483(2) -.5156(2) 0.6579(2) .0372(4) Uani d . 1 . . C
H7A .3505 -.5940 0.6418 .045 Uiso calc R 1 . . H
C8 .2382(2) -.26537(19) 0.56290(18) .0297(3) Uani d . 1 . . C
C9 -.2032(3) -.0441(2) 0.1780(2) .0419(4) Uani d . 1 . . C
H9A -.1019 .0344 0.2027 .050 Uiso calc R 1 . . H
C10 -.2674(5) -.0322(4) -0.0612(3) .0825(10) Uani d . 1 . . C
H10A -.1638 .0526 -0.0165 .124 Uiso calc R 1 . . H
H10B -.3599 -.0037 -0.1190 .124 Uiso calc R 1 . . H
H10C -.2494 -.1067 -0.1182 .124 Uiso calc R 1 . . H
C11 -.4654(3) -.2201(4) -0.0039(3) .0673(7) Uani d . 1 . . C
H11B -.4816 -.2478 0.0753 .101 Uiso calc R 1 . . H
H11C -.4527 -.3005 -0.0583 .101 Uiso calc R 1 . . H
H11D -.5637 -.1977 -0.0609 .101 Uiso calc R 1 . . H
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Cd1 O3 2_556 . 180.0 ?
O3 Cd1 Cl1 2_556 2_556 92.88(4) ?
O3 Cd1 Cl1 . 2_556 87.12(4) ?
O3 Cd1 Cl1 2_556 . 87.12(4) ?
O3 Cd1 Cl1 . . 92.88(4) y
Cl1 Cd1 Cl1 2_556 . 180.0 ?
O3 Cd1 S1 2_556 . 87.90(4) ?
O3 Cd1 S1 . . 92.10(4) y
Cl1 Cd1 S1 2_556 . 85.155(15) ?
Cl1 Cd1 S1 . . 94.85(2) y
O3 Cd1 S1 2_556 2_556 92.10(4) ?
O3 Cd1 S1 . 2_556 87.90(4) ?
Cl1 Cd1 S1 2_556 2_556 94.845(15) ?
Cl1 Cd1 S1 . 2_556 85.155(15) ?
S1 Cd1 S1 . 2_556 180.0 ?
C8 S1 Cd1 . . 112.99(6) ?
C9 O3 Cd1 . . 117.69(13) ?
O1 N1 O2 . . 124.1(2) ?
O1 N1 C4 . . 118.5(2) ?
O2 N1 C4 . . 117.4(2) ?
C7 N2 N3 . . 114.79(16) ?
C8 N3 N2 . . 119.91(15) ?
C9 N5 C10 . . 121.4(2) ?
C9 N5 C11 . . 120.7(2) ?
C10 N5 C11 . . 117.1(2) ?
C2 C1 C6 . . 119.91(17) ?
C2 C1 C7 . . 122.25(17) ?
C6 C1 C7 . . 117.84(18) ?
C3 C2 C1 . . 120.22(18) ?
C4 C3 C2 . . 118.23(19) ?
C5 C4 C3 . . 122.91(18) ?
C5 C4 N1 . . 118.48(19) ?
C3 C4 N1 . . 118.61(19) ?
C4 C5 C6 . . 118.49(18) ?
C5 C6 C1 . . 120.17(19) ?
N2 C7 C1 . . 120.56(18) ?
N4 C8 N3 . . 118.90(16) ?
N4 C8 S1 . . 124.24(14) ?
N3 C8 S1 . . 116.85(13) ?
O3 C9 N5 . . 125.2(2) ?
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
Cd1 O3 2_556 2.3580(10) ?
Cd1 O3 . 2.3580(10) y
Cd1 Cl1 2_556 2.5784(4) ?
Cd1 Cl1 . 2.5784(4) y
Cd1 S1 . 2.6995(4) y
Cd1 S1 2_556 2.6995(4) ?
S1 C8 . 1.703(2) y
O1 N1 . 1.218(3) y
O2 N1 . 1.224(3) y
O3 C9 . 1.234(2) y
N1 C4 . 1.469(2) y
N2 C7 . 1.275(2) y
N2 N3 . 1.372(2) y
N3 C8 . 1.342(2) y
N4 C8 . 1.311(2) y
N5 C9 . 1.314(3) ?
N5 C10 . 1.450(3) ?
N5 C11 . 1.452(3) ?
C1 C2 . 1.387(3) ?
C1 C6 . 1.394(3) ?
C1 C7 . 1.462(2) ?
C2 C3 . 1.381(3) ?
C3 C4 . 1.379(3) ?
C4 C5 . 1.371(3) ?
C5 C6 . 1.376(3) ?
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
N3 H3B S1 2_546 0.86 2.60 3.405(2) 157 yes
N4 H4A Cl1 2_656 0.86 2.58 3.346(2) 149 yes
N4 H4B Cl1 1_555 0.86 2.45 3.253(2) 156 yes
N4 H4A N2 1_555 0.86 2.32 2.660(3) 104 yes
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_site_symmetry_1
_geom_torsion
O3 Cd1 S1 C8 2_556 -49.92(8)
O3 Cd1 S1 C8 . 130.08(8)
Cl1 Cd1 S1 C8 2_556 -143.00(7)
Cl1 Cd1 S1 C8 . 37.00(7)
S1 Cd1 S1 C8 2_556 6E1(10)
O3 Cd1 O3 C9 2_556 0E1(5)
Cl1 Cd1 O3 C9 2_556 154.23(15)
Cl1 Cd1 O3 C9 . -25.77(15)
S1 Cd1 O3 C9 . -120.73(15)
S1 Cd1 O3 C9 2_556 59.27(15)
C7 N2 N3 C8 . -177.40(18)
C6 C1 C2 C3 . -2.1(3)
C7 C1 C2 C3 . 178.11(19)
C1 C2 C3 C4 . -0.2(3)
C2 C3 C4 C5 . 2.4(3)
C2 C3 C4 N1 . -178.14(19)
O1 N1 C4 C5 . 165.5(2)
O2 N1 C4 C5 . -14.7(3)
O1 N1 C4 C3 . -14.0(3)
O2 N1 C4 C3 . 165.8(2)
C3 C4 C5 C6 . -2.1(3)
N1 C4 C5 C6 . 178.41(19)
C4 C5 C6 C1 . -0.3(3)
C2 C1 C6 C5 . 2.4(3)
C7 C1 C6 C5 . -177.82(19)
N3 N2 C7 C1 . -178.03(16)
C2 C1 C7 N2 . -2.1(3)
C6 C1 C7 N2 . 178.06(19)
N2 N3 C8 N4 . -0.5(3)
N2 N3 C8 S1 . -179.52(13)
Cd1 S1 C8 N4 . -9.49(19)
Cd1 S1 C8 N3 . 169.45(12)
Cd1 O3 C9 N5 . 176.01(17)
C10 N5 C9 O3 . -174.1(3)
C11 N5 C9 O3 . -5.0(4)
