#------------------------------------------------------------------------------
#$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $
#$Revision: 34330 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000693.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_4000693
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_volume                  12
_journal_year                    2000
_chemical_formula_sum            'C7 H14 I N5 S2'
_chemical_formula_weight         359.25
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.119(6)
_cell_length_b                   11.230(6)
_cell_length_c                   8.327(6)
_cell_measurement_temperature    295(2)
_cell_volume                     1413.8(14)
_diffrn_ambient_temperature      295(2)
_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  0.045
_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       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2163
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         2.2
_exptl_absorpt_coefficient_mu    2.54
_exptl_crystal_density_diffrn    1.612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         717
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0440
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_reflns_number_gt                695
_reflns_number_total             717
_reflns_threshold_expression     >3sigma(I)
_[local]_cod_data_source_file    deposit.cif
_[local]_cod_data_source_block   Iodo_1
_[local]_cod_cif_authors_sg_H-M  Cmcm
_[local]_cod_chemical_formula_sum_orig 'C7 H14 N5 S2 I'
_cod_original_cell_volume        1413.81
_cod_database_code               4000693
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
C2 C 0.0000 0.885(3) 0.013(7) 0.18(2) Uani
C3 C 0.073(2) 0.935(3) 0.015(6) 0.27(2) Uani
S1 S 0.2282(3) 0.7228(5) 0.250 0.0743(18) Uani
N1 N 0.3462(6) 0.8613(8) 0.1150(10) 0.054(3) Uani
C1 C 0.3145(9) 0.8220(10) 0.2500 0.040(4) Uani
I1 I 0.0000 0.59141(9) 0.2500 0.0274(3) 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
C2 0.18(4) 0.08(2) 0.28(6) 0.04(3) 0.00 0.00
C3 0.20(3) 0.22(3) 0.39(5) -0.19(4) -0.14(4) 0.14(2)
S1 0.087(3) 0.110(4) 0.026(2) 0.00 0.00 -0.075(3)
N1 0.058(5) 0.069(5) 0.035(5) 0.000(4) 0.006(4) -0.039(4)
C1 0.047(7) 0.049(7) 0.023(7) 0.000 0.000 -0.025(6)
I1 0.0226(5) 0.0255(5) 0.0341(7) 0.000 0.000 0.000
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
C3 C2 C3 126(4) 7_555 no
C2 C3 C3 116(3) 3_575 no
S1 C1 N1 120.1(6) . yes
S1 C1 N1 120.1(6) 6_555 yes
N1 C1 N1 119.8(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
S1 C1 1.716(14) . yes
N1 C1 1.299(11) . yes
C2 C3 1.24(3) . no
C2 C3 1.24(3) 7_555 no
C3 C3 1.48(5) 3_575 no