#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:05:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179612 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/76/4507643.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_4507643
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 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.034(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5206(3)
_cell_length_b                   7.8048(3)
_cell_length_c                   18.6978(5)
_cell_measurement_reflns_used    10204
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8849
_cell_measurement_theta_min      2.1740
_cell_volume                     1243.43(7)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34910
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97504
_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    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0253
_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)+(0.0267P)²+0.4493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                2886
_reflns_number_total             3225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400005d_si_002.cif
_cod_data_source_block           ulme
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4507643
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.52269(3) 0.64556(4) 0.393343(14) 0.01613(7) Uani 1 1 d .
N1 N 0.45295(10) 0.78766(12) 0.51925(5) 0.01375(18) Uani 1 1 d .
N3 N 0.71586(11) 0.76390(13) 0.49400(5) 0.01649(19) Uani 1 1 d .
H03 H 0.7372(17) 0.807(2) 0.5344(8) 0.027(4) Uiso 1 1 d .
C2 C 0.56639(12) 0.73755(13) 0.47369(5) 0.01272(19) Uani 1 1 d .
C11 C 0.28793(12) 0.75246(15) 0.50338(6) 0.0194(2) Uani 1 1 d .
H11A H 0.2615 0.7990 0.4562 0.029 Uiso 1 1 calc R
H11B H 0.2216 0.8064 0.5398 0.029 Uiso 1 1 calc R
H11C H 0.2702 0.6284 0.5035 0.029 Uiso 1 1 calc R
C12 C 0.49148(13) 0.84768(15) 0.59112(6) 0.0174(2) Uani 1 1 d .
H12A H 0.5401 0.7543 0.6183 0.026 Uiso 1 1 calc R
H12B H 0.3954 0.8849 0.6154 0.026 Uiso 1 1 calc R
H12C H 0.5648 0.9441 0.5879 0.026 Uiso 1 1 calc R
C31 C 0.85139(13) 0.72254(17) 0.45017(6) 0.0216(2) Uani 1 1 d .
H31A H 0.8446 0.6029 0.4345 0.032 Uiso 1 1 calc R
H31B H 0.9475 0.7390 0.4782 0.032 Uiso 1 1 calc R
H31C H 0.8535 0.7978 0.4082 0.032 Uiso 1 1 calc R
S' S 0.92931(3) 0.58208(4) 0.132952(14) 0.01864(7) Uani 1 1 d .
N1' N 0.80740(11) 0.85625(12) 0.19998(5) 0.01546(18) Uani 1 1 d .
N3' N 0.75728(11) 0.59390(12) 0.25078(5) 0.01595(18) Uani 1 1 d .
H03' H 0.7170(17) 0.642(2) 0.2854(8) 0.027(4) Uiso 1 1 d .
C2' C 0.82644(11) 0.68484(14) 0.19845(5) 0.0132(2) Uani 1 1 d .
C11' C 0.88817(14) 0.97132(15) 0.15070(6) 0.0215(2) Uani 1 1 d .
H11D H 0.9625 0.9056 0.1216 0.032 Uiso 1 1 calc R
H11E H 0.9450 1.0588 0.1780 0.032 Uiso 1 1 calc R
H11F H 0.8112 1.0269 0.1194 0.032 Uiso 1 1 calc R
C12' C 0.70966(13) 0.94101(14) 0.25338(6) 0.0181(2) Uani 1 1 d .
H12D H 0.6171 0.8703 0.2632 0.027 Uiso 1 1 calc R
H12E H 0.6762 1.0530 0.2352 0.027 Uiso 1 1 calc R
H12F H 0.7700 0.9566 0.2975 0.027 Uiso 1 1 calc R
C31' C 0.75506(14) 0.40750(14) 0.25267(6) 0.0199(2) Uani 1 1 d .
H31D H 0.7004 0.3639 0.2103 0.030 Uiso 1 1 calc R
H31E H 0.7003 0.3689 0.2958 0.030 Uiso 1 1 calc R
H31F H 0.8630 0.3641 0.2532 0.030 Uiso 1 1 calc R
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 C12 120.94(9)
C2 N1 C11 120.49(9)
C12 N1 C11 117.54(9)
C2 N3 C31 124.05(9)
N3 C2 N1 117.20(9)
N3 C2 S 121.28(8)
N1 C2 S 121.52(8)
C2' N1' C12' 122.22(9)
C2' N1' C11' 122.73(10)
C12' N1' C11' 115.00(9)
C2' N3' C31' 123.43(10)
N3' C2' N1' 117.10(9)
N3' C2' S' 119.96(8)
N1' C2' S' 122.92(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S C2 1.7060(10)
N1 C2 1.3467(13)
N1 C12 1.4604(13)
N1 C11 1.4629(13)
N3 C2 1.3445(14)
N3 C31 1.4527(14)
S' C2' 1.7066(11)
N1' C2' 1.3479(14)
N1' C12' 1.4591(14)
N1' C11' 1.4594(14)
N3' C2' 1.3450(14)
N3' C31' 1.4554(14)
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 0.823(16) 2.612(16) 3.3571(10) 151.4(14) .
N3 H03 S' 0.848(15) 2.610(15) 3.3909(10) 153.6(13) 4_576
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 -177.88(10)
C31 N3 C2 S 1.76(15)
C12 N1 C2 N3 -7.55(15)
C11 N1 C2 N3 -175.64(9)
C12 N1 C2 S 172.81(8)
C11 N1 C2 S 4.72(14)
C31' N3' C2' N1' 174.16(10)
C31' N3' C2' S' -4.52(14)
C12' N1' C2' N3' -3.20(14)
C11' N1' C2' N3' 173.92(9)
C12' N1' C2' S' 175.44(8)
C11' N1' C2' S' -7.44(14)
