#------------------------------------------------------------------------------
#$Date: 2016-03-21 00:21:50 +0100 (lun 21 de mar de 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000695.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_4000695
loop_
_publ_author_name
'Keith Prout'
'Stephen J. Heyes'
'Christopher M. Dobson'
'Andrew McDaid'
'Thierry Maris'
'Matthias Muller'
'Matthew J. Seaman'
_publ_section_title
;
 Variable-Temperature Studies of Order/Disorder Transitions in the
 Thiourea Pyridinium Halide Crystals by XRD and Solid-State 2H NMR
;
_journal_name_full               'Chemistry of Material'
_journal_page_first              3561
_journal_page_last               3569
_journal_paper_doi               10.1021/cm0001612
_journal_volume                  12
_journal_year                    2000
_chemical_formula_sum            'C7 H14 Cl N5 S2'
_chemical_formula_weight         267.80
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.563(8)
_cell_length_b                   10.561(4)
_cell_length_c                   8.398(2)
_cell_measurement_temperature    265(2)
_cell_volume                     1291.6(9)
_diffrn_ambient_temperature      265(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1478
_diffrn_reflns_theta_max         74.4
_diffrn_reflns_theta_min         5.2
_exptl_absorpt_coefficient_mu    5.49
_exptl_crystal_density_diffrn    1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         733
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0817
_refine_ls_weighting_scheme      calc
_reflns_number_gt                672
_reflns_number_total             733
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           Chloro_1
_cod_original_cell_volume        1291.61
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               4000695
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,1/2+z
3 x,-y,-z
4 -x,y,1/2-z
5 -x,-y,-z
6 x,y,1/2-z
7 -x,y,z
8 x,-y,1/2+z
9 1/2+x,1/2+y,z
10 1/2-x,1/2-y,1/2+z
11 1/2+x,1/2-y,-z
12 1/2-x,1/2+y,1/2-z
13 1/2-x,1/2-y,-z
14 1/2+x,1/2+y,1/2-z
15 1/2-x,1/2+y,z
16 1/2+x,1/2-y,1/2+z
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
C5 C 0.5000 0.3760(3) -0.0520(7) 0.1133(18) Uani
C6 C 0.5781(2) 0.4373(2) -0.0249(5) 0.1217(14) Uani
S2 S 0.76697(2) 0.28785(4) 0.250 0.0510(3) Uani
N3 N 0.64716(8) 0.13180(10) 0.11320(10) 0.0490(4) Uani
C4 C 0.68260(10) 0.17680(10) 0.2500 0.0365(5) Uani
Cl1 Cl 0.50000 -0.08330(4) 0.2500 0.0491(4) Uani
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
C5 0.133(3) 0.083(2) 0.124(4) 0.037(2) 0.00 0.00
C6 0.092(2) 0.122(2) 0.151(3) 0.062(2) 0.043(2) 0.0410(10)
S2 0.0575(6) 0.0599(6) 0.0357(6) 0.00 0.00 -0.0283(2)
N3 0.0566(7) 0.0560(7) 0.0343(7) -0.0051(4) 0.0006(4) -0.0180(4)
C4 0.0430(8) 0.0335(7) 0.0330(10) 0.000 0.000 -0.0067(4)
Cl1 0.0379(6) 0.0355(6) 0.0740(7) 0.000 0.000 0.0000
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C5 C6 117.8(3) 7_655 no
C5 C6 C6 121.1(3) 3_565 no
S2 C4 N3 121.41(6) . yes
S2 C4 N3 121.41(6) 6_555 yes
N3 C4 N3 117.18(11) 6_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S2 C4 1.6986(16) . yes
N3 C4 1.3461(14) . yes
C5 C6 1.328(3) . no
C5 C6 1.328(3) 7_655 no
C6 C6 1.389(3) 3_565 no
