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#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000697.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_4000697
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 Br N5 S2'
_chemical_formula_weight         312.25
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.771(7)
_cell_length_b                   10.897(4)
_cell_length_c                   8.368(2)
_cell_measurement_temperature    295(2)
_cell_volume                     1346.9(9)
_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_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            2385
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         1.0
_exptl_absorpt_coefficient_mu    3.34
_exptl_crystal_density_diffrn    1.461
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         853
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0408
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_reflns_number_gt                580
_reflns_number_total             853
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           Bromo_1
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               4000697
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 0.0772(6) 0.0610(10) -0.021(2) 0.154(5) Uani
C3 C 0.0000 0.1180(10) -0.039(2) 0.145(8) Uani
S1 S 0.26920(10) 0.2174(2) 0.250 0.0584(5) Uani
N1 N 0.1500(3) 0.3656(4) 0.1139(4) 0.0530(12) Uani
C1 C 0.1840(4) 0.3225(5) 0.2500 0.0400(16) Uani
Br1 Br 0.5000 0.08751(7) 0.2500 0.0413(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 0.112(6) 0.141(8) 0.210(10) -0.080(10) 0.048(8) -0.050(6)
C3 0.20(2) 0.064(6) 0.170(10) -0.016(8) 0.000 0.000
S1 0.0680(10) 0.0770(10) 0.0301(7) 0.00 0.00 0.0406(9)
N1 0.064(2) 0.063(2) 0.032(2) 0.005(2) -0.004(2) 0.026(2)
C1 0.049(3) 0.041(3) 0.030(2) 0.000 0.000 0.011(2)
Br1 0.0333(4) 0.0345(4) 0.0562(5) 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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C2 C3 119.3(9) 3_555 . no
C2 C3 C2 121.5(11) . 7_555 no
S1 C1 N1 121.1(3) . . yes
S1 C1 N1 121.1(3) . 6_555 yes
N1 C1 N1 117.8(5) . 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 1.702(6) . yes
N1 C1 1.330(5) . yes
C2 C2 1.375(16) 3_555 no
C2 C3 1.307(11) . no
