#------------------------------------------------------------------------------
#$Date: 2017-10-13 13:42:48 +0200 (vie 13 de oct de 2017) $
#$Revision: 201982 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/76/4507644.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_4507644
loop_
_publ_author_name
'Näther, Christian'
'Jess, Inke'
'Jones, Peter G.'
'Taouss, Christina'
'Teschmit, Nicole'
_publ_section_title
;
 Structural, Thermodynamic, and Kinetic Aspects of the Polymorphism of
 Trimethylthiourea: The Influence of Kinetics on the Transformations
 between Polymorphs
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1676
_journal_paper_doi               10.1021/cg400005d
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C4 H10 N2 S'
_chemical_formula_weight         118.20
_chemical_name_systematic
;
 ?
;
_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                 101.202(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.9388(2)
_cell_length_b                   11.6530(4)
_cell_length_c                   11.0955(5)
_cell_measurement_reflns_used    8708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9281
_cell_measurement_theta_min      2.5555
_cell_volume                     626.40(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31347
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0249
_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)+(0.0259P)²+0.2231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1678
_reflns_number_total             1887
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details
;
TITL Tanne in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073   4.938828  11.652999  11.095465  90.0000 101.2021  90.0000
ZERR    4.00   0.0002   0.0004   0.0005   0.0000   0.004   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N S
UNIT 16.00 40.00 8.00 4.00
TEMP -173
SIZE 0.3 0.2 0.05
ACTA 61
CONF
L.S. 4
FMAP 2
PLAN 8
EQIV $1 x+1/2, -y+1/2, z+1/2
HTAB N3 S_$1
WGHT    0.025900    0.223100
FVAR       8.53359
S     4    0.535688    0.159204    0.634458    11.00000    0.01647    0.01656 =
         0.01374   -0.00273    0.00128   -0.00009
N1    3    0.409749    0.334243    0.770800    11.00000    0.01445    0.01561 =
         0.01342   -0.00112    0.00059    0.00162
N3    3    0.777835    0.222024    0.859311    11.00000    0.01607    0.01809 =
         0.01345   -0.00185    0.00052    0.00345
H03   2    0.790924    0.262011    0.922032    11.00000    0.02399
C2    1    0.574924    0.243806    0.761845    11.00000    0.01252    0.01432 =
         0.01317    0.00072    0.00315   -0.00237
C11   1    0.180246    0.363093    0.670856    11.00000    0.01501    0.02007 =
         0.01810    0.00153   -0.00046    0.00275
AFIX 137
H11A  2    0.252884    0.390442    0.599870    11.00000   -1.50000
H11B  2    0.067647    0.423412    0.698142    11.00000   -1.50000
H11C  2    0.066428    0.294755    0.647587    11.00000   -1.50000
AFIX   0
C12   1    0.454351    0.405277    0.881661    11.00000    0.02316    0.01765 =
         0.01594   -0.00309    0.00218    0.00430
AFIX 137
H12A  2    0.437131    0.357735    0.952641    11.00000   -1.50000
H12B  2    0.316247    0.466686    0.872016    11.00000   -1.50000
H12C  2    0.639542    0.438979    0.894569    11.00000   -1.50000
AFIX   0
C31   1    0.971244    0.127318    0.863620    11.00000    0.01587    0.02009 =
         0.01884    0.00088    0.00086    0.00418
AFIX 137
H31A  2    0.871489    0.054408    0.861362    11.00000   -1.50000
H31B  2    1.110259    0.131844    0.939627    11.00000   -1.50000
H31C  2    1.062317    0.131881    0.792775    11.00000   -1.50000
HKLF 4
;
_cod_data_source_file            cg400005d_si_003.cif
_cod_data_source_block           tanne
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4507644
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_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S S 0.53569(5) 0.159204(19) 0.63446(2) 0.01581(7) Uani 1 1 d .
N1 N 0.40975(16) 0.33424(7) 0.77080(7) 0.01478(16) Uani 1 1 d .
N3 N 0.77783(17) 0.22202(7) 0.85931(7) 0.01618(16) Uani 1 1 d .
H03 H 0.791(3) 0.2620(12) 0.9220(13) 0.024(3) Uiso 1 1 d .
C2 C 0.57492(18) 0.24381(8) 0.76185(8) 0.01325(17) Uani 1 1 d .
C11 C 0.1802(2) 0.36309(8) 0.67086(9) 0.01822(19) Uani 1 1 d .
H11A H 0.2529 0.3904 0.5999 0.027 Uiso 1 1 calc R
H11B H 0.0676 0.4234 0.6981 0.027 Uiso 1 1 calc R
H11C H 0.0664 0.2948 0.6476 0.027 Uiso 1 1 calc R
C12 C 0.4544(2) 0.40528(8) 0.88166(9) 0.01913(19) Uani 1 1 d .
H12A H 0.4371 0.3577 0.9526 0.029 Uiso 1 1 calc R
H12B H 0.3162 0.4667 0.8720 0.029 Uiso 1 1 calc R
H12C H 0.6395 0.4390 0.8946 0.029 Uiso 1 1 calc R
C31 C 0.97124(19) 0.12732(9) 0.86362(9) 0.01860(19) Uani 1 1 d .
H31A H 0.8715 0.0544 0.8614 0.028 Uiso 1 1 calc R
H31B H 1.1103 0.1318 0.9396 0.028 Uiso 1 1 calc R
H31C H 1.0623 0.1319 0.7928 0.028 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S 0.01647(12) 0.01656(12) 0.01374(11) -0.00273(8) 0.00128(8) -0.00009(8)
N1 0.0145(4) 0.0156(4) 0.0134(3) -0.0011(3) 0.0006(3) 0.0016(3)
N3 0.0161(4) 0.0181(4) 0.0134(3) -0.0018(3) 0.0005(3) 0.0034(3)
C2 0.0125(4) 0.0143(4) 0.0132(4) 0.0007(3) 0.0032(3) -0.0024(3)
C11 0.0150(4) 0.0201(4) 0.0181(4) 0.0015(3) -0.0005(3) 0.0028(3)
C12 0.0232(5) 0.0176(4) 0.0159(4) -0.0031(3) 0.0022(4) 0.0043(4)
C31 0.0159(4) 0.0201(4) 0.0188(4) 0.0009(3) 0.0009(3) 0.0042(3)
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
C2 N1 C11 120.98(8)
C2 N1 C12 120.64(8)
C11 N1 C12 118.37(8)
C2 N3 C31 123.40(8)
N3 C2 N1 117.02(8)
N3 C2 S 120.25(7)
N1 C2 S 122.73(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S C2 1.7032(9)
N1 C2 1.3481(12)
N1 C11 1.4626(12)
N1 C12 1.4634(11)
N3 C2 1.3480(11)
N3 C31 1.4543(12)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H03 S 0.830(14) 2.599(14) 3.3685(8) 155.0(12) 4_666
C12 H12B S 0.98 2.83 3.8049(10) 173.0 2_556
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
C31 N3 C2 N1 179.68(8)
C31 N3 C2 S -0.48(13)
C11 N1 C2 N3 -178.65(8)
C12 N1 C2 N3 0.69(13)
C11 N1 C2 S 1.51(12)
C12 N1 C2 S -179.16(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 2060159
