Thianaphtene in Pnma at 100 K
Thierry Maris; Personal communication to COD  (2020) –; doi:

data_3500113
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_publ_section_title
;
 Thianaphtene in Pnma at 100 K
;
_journal_name_full               'Personal communication to COD'
_journal_year                    2020
_chemical_formula_moiety         'C8 H6 S'
_chemical_formula_sum            'C8 H6 S'
_chemical_formula_weight         134.19
_chemical_name_common            Thianaphtene
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.72450(10)
_cell_length_b                   14.8852(2)
_cell_length_c                   5.78240(10)
_cell_measurement_reflns_used    6682
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.579
_cell_measurement_theta_min      2.969
_cell_volume                     664.865(17)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9454
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.854
_diffrn_reflns_theta_min         8.223
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.425
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.837916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0604 before and 0.0390 after correction.
The Ratio of minimum to maximum transmission is 0.8379.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       fragment
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_special_details
;
 ?
;
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.122
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         619
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1008
_refine_special_details
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S1A-C2A = S1A-C9A
 1.72 with sigma of 0.001
 C2A-C3A
 1.35 with sigma of 0.005
 C3A-C4A
 1.45 with sigma of 0.005
 C7A-C8A = C5A-C6A
 1.39 with sigma of 0.005
 C4A-C9A
 1.42 with sigma of 0.005
3. Restrained planarity
 S1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
5. Uiso/Uaniso restraints and constraints
Uanis(C9A) = Uanis(C9B)
Uanis(C8A) = Uanis(C8B)
Uanis(C7A) = Uanis(C7B)
Uanis(C6A) = Uanis(C6B)
Uanis(C5A) = Uanis(C5B)
Uanis(C4A) = Uanis(C4B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(S1A) = Uanis(S1B)
6. Same fragment restrains
{S1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A}
as
{S1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B}
7. Others
 Sof(S1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=0.5*(1-FVAR(2))
 Sof(S1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=0.5*FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C2B(H2B),
 C3B(H3B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B)
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                601
_reflns_number_total             619
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            thiana.cif
_cod_data_source_block           thiana
_cod_database_code               3500113
_cod_database_fobs_code          3500113
_vrf_plat088_thiana
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PROBLEM:  Poor Data / Parameter Ratio ....................       5.68
RESPONSE:
The structure is disordered with two molecules lying over a mirror plane.
The refinement involve both complete molecules and this situation generates
a large number of parameters. However, this is counterbalanced by the use of
numerous restraints applied on distances and atomic displacement parameters
that links many of these parameters.  See text for a more detailled description
of the disorder and the refinement procedure.
;
_shelxl_version_number           2014-3