#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003267.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_2003267
loop_
_publ_author_name
'Heinemann, F. W.'
'Hartung, H.'
'Dehne, H.'
'Scheunemann, A.'
_publ_section_title
;
 Thiooxalic Acid 2-Amide-1-hydrazide-2-hydrazone
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              442
_journal_page_last               445
_journal_paper_doi               10.1107/S0108270194005494
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'recrystallized from water'
_chemical_formula_moiety         'C2 H7 N5 S1'
_chemical_formula_sum            'C2 H7 N5 S'
_chemical_formula_weight         133.19
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_type_scat_source           IntTabC
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   8.411(2)
_cell_length_b                   7.094(1)
_cell_length_c                   19.349(4)
_cell_measurement_reflns_used    82
_cell_measurement_temperature    293
_cell_measurement_theta_max      15.5
_cell_measurement_theta_min      10.0
_cell_volume                     1154.5(4)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       ω/θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2792
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        +-5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.180
_refine_ls_extinction_coef       \c=0.021(2)
_refine_ls_extinction_method
; empirical, Fcorr = kFc(1 +
0.001\cFc²λ³/sin(2θ)]^-1/4^
;
_refine_ls_goodness_of_fit_obs   1.004
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1017
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; w = 1/[\s^2^(F~o~^2^) + (0.0431P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_obs         0.0804
_reflns_number_observed          701
_reflns_number_total             1017
_reflns_observed_criterion       F~o~^2^>2\s(F~o~^2^)
_cod_data_source_file            ka1069.cif
_cod_data_source_block           ka1069_structure_1_of_1
_cod_original_formula_sum        'C2 H7 N5 S1'
_cod_database_code               2003267
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,y,1/2-z
x,1/2-y,1/2+z
1/2-x,1/2+y,z
-x,-y,-z
1/2-x,-y,1/2+z
-x,1/2+y,1/2-z
1/2+x,1/2-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
S1 .08589(6) .16190(10) .61326(3) .0369(2)
N1 -.1396(2) .0218(3) .69960(9) .0303(5)
N2 -.0152(3) -.0282(3) .74147(11) .0374(5)
N3 -.3853(2) .1269(3) .62573(9) .0277(5)
N4 -.5220(2) .1600(4) .58554(11) .0350(5)
N5 -.2255(2) .2178(3) .53745(9) .0342(5)
C1 -.1027(2) .1079(3) .64297(11) .0242(5)
C2 -.2444(2) .1540(3) .60010(10) .0244(5)
H21 .0770(27) -.0414(37) .7184(13) .034(7)
H22 -.0454(33) -.1172(43) .7664(15) .045(8)
H31 -.3976(25) .0896(35) .6631(14) .030(7)
H41 -.5629(36) .2583(48) .6033(15) .055(9)
H42 -.5862(32) .0657(42) .5913(16) .055(10)
H51 -.3015(35) .2404(37) .5063(14) .052(8)
H52 -.1388(36) .2380(42) .5215(13) .054(8)
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
C1 N1 N2 116.1(2) yes
C2 N3 N4 120.6(2) yes
N1 C1 C2 112.6(2) yes
N1 C1 S1 127.3(2) yes
C2 C1 S1 120.0(2) yes
N3 C2 N5 121.2(2) yes
N3 C2 C1 119.0(2) yes
N5 C2 C1 119.8(2) yes
N1 N2 H22 107.8(19) no
N1 N2 H21 113.1(16) no
C2 N3 H31 121.8(17) no
N4 N3 H31 117.5(16) no
N3 N4 H42 108.(2) no
N3 N4 H41 104.(2) no
C2 N5 H52 122.(2) no
C2 N5 H51 127.0(19) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C1 1.730(2) yes
N1 C1 1.292(3) yes
N1 N2 1.370(3) yes
N3 C2 1.299(3) yes
N3 N4 1.408(3) yes
N5 C2 1.304(3) yes
C1 C2 1.488(3) yes
N2 H21 0.90(2) no
N3 H31 0.78(3) no
N5 H51 0.89(3) no
N5 H52 0.80(3) no
N3 H31 0.78(3) no
N4 H42 0.87(3) no
N5 H52 0.80(3) no
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_publ_flag
N2 N1 C1 C2 179.0(2) yes
N2 N1 C1 S1 1.7(3) yes
N4 N3 C2 N5 2.1(3) yes
N4 N3 C2 C1 -176.8(2) yes
N1 C1 C2 N3 8.2(3) yes
S1 C1 C2 N3 -174.3(2) yes
N1 C1 C2 N5 -170.8(2) yes
S1 C1 C2 N5 6.8(3) yes
