#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/06/4000685.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_4000685
loop_
_publ_author_name
'Thierry Maris'
'Michael J. Henson'
'Stephen J. Heyes'
'Keith Prout'
_publ_section_title
;
 Investigations of the Phase Transitions in Thiourea Inclusion Compounds
 with Cycloheptane, Cyclooctane, and Cyclooctanone
;
_journal_name_full               'Chem. Mater.'
_journal_page_first              2483
_journal_page_last               2492
_journal_paper_doi               10.1021/cm991173u
_journal_volume                  13
_journal_year                    2001
_chemical_formula_sum            'C10 H26 N6 S3'
_chemical_formula_weight         52.07
_chemical_name_systematic
;                                                                               
?                                                                               
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-19-07
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.012(2)
_cell_length_b                   16.012(2)
_cell_length_c                   12.447(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      22
_cell_volume                     2763.7(7)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;                                                                               
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)                         
;
_computing_molecular_graphics
;                                                                               
 CAMERON (Watkin, Prout & Pearce,  1996)                                        
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_max 0.527
_diffrn_measurement_device_type  '  Enraf-nonius CAD4 '
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            743
_diffrn_reflns_theta_max         75.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.66
_exptl_absorpt_correction_T_max  0.48
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'ψ scan,(North et al, 1968)'
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.13
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             979.62
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8824
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     22
_refine_ls_number_reflns         524
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.000128
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
 12.1     9.42     9.15    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1078
_reflns_limit_h_max              0
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -5
_reflns_number_gt                524
_reflns_number_total             667
_reflns_threshold_expression     >3.00σ(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           TC7_RT
_cod_original_cell_volume        2763.8
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        ' C1.67 H2 N1 S0.50 '
_cod_database_code               4000685
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x+y,y,z+1/2
x-y,-y,-z+1/2
-x+y+1/3,y+2/3,z+7/6
x-y+1/3,-y+2/3,-z+7/6
-x+y+2/3,y+1/3,z+5/6
x-y+2/3,-y+1/3,-z+5/6
x,x-y,z+1/2
-x,-x+y,-z+1/2
x+1/3,x-y+2/3,z+7/6
-x+1/3,-x+y+2/3,-z+7/6
x+2/3,x-y+1/3,z+5/6
-x+2/3,-x+y+1/3,-z+5/6
-y,-x,z+1/2
y,x,-z+1/2
-y+1/3,-x+2/3,z+7/6
y+1/3,x+2/3,-z+7/6
-y+2/3,-x+1/3,z+5/6
y+2/3,x+1/3,-z+5/6
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
S1 0.69782(7) 0.0000 0.2500 0.0727 1.0000 Uani
C2 0.5908(3) 0.0000 0.2500 0.0695 1.0000 Uani
N3 0.5403(2) -0.0178(3) 0.1614(2) 0.0852 1.0000 Uani
C4 0.3333 0.6667 -0.0833 0.103(5) 7.0000 Uiso
H31 0.5612 -0.0334 0.0913 0.0944 1.0000 Uiso
H32 0.4746 -0.0191 0.1590 0.0944 1.0000 Uiso
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
S1 0.0798(7) 0.0940(9) 0.0490(8) -0.0044(4) -0.0022(2) 0.0470(4)
C2 0.0756(18) 0.079(2) 0.055(2) 0.0030(17) 0.0015(9) 0.0397(12)
N3 0.0877(18) 0.113(2) 0.0613(16) -0.0022(14) -0.0066(13) 0.0548(17)
C4 0.103(5) 1.676(11) 0.0000 0.0000 0.0000 0.0000
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 C2 N3 . 120.5(2) yes
S1 C2 N3 20_555 120.5(2) yes
N3 C2 N3 20_555 118.9(4) yes
C2 N3 H31 . 122.4(3) no
C2 N3 H32 . 122.3(3) no
H31 N3 H32 . 115.3(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C2 . 1.713(5) yes
C2 N3 . 1.313(4) yes
C2 N3 20_555 1.313(4) yes
N3 H31 . 1.009(3) no
N3 H32 . 1.042(3) no
