#------------------------------------------------------------------------------
#$Date: 2017-10-13 11:03:29 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201974 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/58/2215826.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_2215826
loop_
_publ_author_name
'Thomas M. Klapötke'
'Stefan M. Sproll'
_publ_section_title
;
 2-Methylthiosemicarbazide
;
_journal_coeditor_code           BV2072
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4270
_journal_page_last               o4270
_journal_paper_doi               10.1107/S1600536807048398
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C2 H7 N3 S'
_chemical_formula_moiety         'C2 H7 N3 S'
_chemical_formula_sum            'C2 H7 N3 S'
_chemical_formula_weight         105.17
_chemical_melting_point          173
_chemical_name_systematic
;
2-methylthiosemicarbazide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.508(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6071(9)
_cell_length_b                   5.9337(6)
_cell_length_c                   9.7415(10)
_cell_measurement_reflns_used    913
_cell_measurement_temperature    200(2)
_cell_volume                     492.04(9)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'PLATON (Spek, 2003), SHELXL97 (Sheldrick, 1997) and publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Xcalibur 3CCD'
_diffrn_measurement_method       ω
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4506
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+0.3245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                900
_reflns_number_total             913
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bv2072.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2215826
_cod_database_fobs_code          2215826
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_occupancy
H H3B 0.776(3) 0.157(4) 1.033(3) 0.049(7) Uiso d 1
H H1B 0.366(3) 0.151(4) 0.798(2) 0.033(6) Uiso d 1
H H1A 0.504(2) 0.043(4) 0.862(2) 0.025(5) Uiso d 1
H H2B 0.809(3) 0.572(4) 1.027(3) 0.046(7) Uiso d 1
H H2A 0.875(3) 0.546(4) 0.885(2) 0.040(6) Uiso d 1
H H2C 0.732(3) 0.688(5) 0.891(3) 0.057(8) Uiso d 1
H H3A 0.837(3) 0.130(4) 0.911(3) 0.041(7) Uiso d 1
S S1 0.44036(5) 0.59448(8) 0.76678(5) 0.02764(19) Uani d 1
C C1 0.5343(2) 0.3573(3) 0.83652(18) 0.0213(4) Uani d 1
N N2 0.68539(17) 0.3589(2) 0.89476(16) 0.0228(4) Uani d 1
N N3 0.7511(2) 0.1490(3) 0.9432(2) 0.0300(4) Uani d 1
N N1 0.4598(2) 0.1604(3) 0.83089(19) 0.0292(4) Uani d 1
C C2 0.7809(2) 0.5601(4) 0.9259(2) 0.0291(4) Uani d 1
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
S1 0.0213(3) 0.0227(3) 0.0375(3) 0.00257(18) -0.00012(19) 0.00346(19)
C1 0.0196(9) 0.0221(9) 0.0225(9) 0.0003(7) 0.0044(7) -0.0016(7)
N2 0.0191(8) 0.0189(8) 0.0293(8) 0.0015(6) -0.0005(6) 0.0016(6)
N3 0.0254(9) 0.0276(9) 0.0359(10) 0.0059(7) 0.0012(7) 0.0062(7)
N1 0.0204(9) 0.0208(9) 0.0452(10) -0.0025(7) 0.0003(7) 0.0010(7)
C2 0.0217(10) 0.0277(11) 0.0363(11) -0.0046(8) -0.0004(8) 0.0009(9)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 C1 N2 117.09(16)
N1 C1 S1 120.63(14)
N2 C1 S1 122.25(13)
C1 N2 N3 116.65(15)
C1 N2 C2 125.24(15)
N3 N2 C2 117.73(14)
N2 N3 H3B 108.3(17)
N2 N3 H3A 108.5(16)
H3B N3 H3A 106(2)
C1 N1 H1B 120.8(16)
C1 N1 H1A 122.2(15)
H1B N1 H1A 117(2)
N2 C2 H2B 108.5(14)
N2 C2 H2A 109.2(15)
H2B C2 H2A 109(2)
N2 C2 H2C 112.9(17)
H2B C2 H2C 110(2)
H2A C2 H2C 107(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C1 1.7128(18)
C1 N1 1.330(2)
C1 N2 1.340(2)
N2 N3 1.420(2)
N2 C2 1.456(2)
N3 H3B 0.87(3)
N3 H3A 0.85(3)
N1 H1B 0.82(2)
N1 H1A 0.83(2)
C2 H2B 0.98(3)
C2 H2A 0.95(2)
C2 H2C 0.91(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
N1 H1A S1 1_545 0.83(2) 2.84(2) 3.4150(18) 127.6(17)
N1 H1A N3 . 0.83(2) 2.25(2) 2.584(3) 104.5(17)
N1 H1B S1 2_546 0.82(2) 2.64(3) 3.4573(19) 170(2)
N3 H3A S1 2_646 0.85(3) 2.77(3) 3.598(2) 163(2)
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
N1 C1 N2 N3 0.7(2)
S1 C1 N2 N3 -177.29(13)
N1 C1 N2 C2 -172.04(18)
S1 C1 N2 C2 10.0(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 2298697
