#------------------------------------------------------------------------------
#$Date: 2019-10-04 10:24:00 +0200 (vie 04 de oct de 2019) $
#$Revision: 219097 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/43/7234381.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_7234381
loop_
_publ_author_name
'Rie Suizu'
'Akito Iwasaki'
'Yoshiaki Shuku'
'Kunio Awaga'
_publ_section_title
;
 Spatially inhomogeneous, stepwise phase transitions in a thiazyl
 diradical: a structural mismatch induced by lattice transformation
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              7968
_journal_page_last               7977
_journal_paper_doi               10.1039/C5TC01410G
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C14 H8 N4 S4'
_chemical_formula_sum            'C14 H8 N4 S4'
_chemical_formula_weight         360.48
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   15.621(4)
_cell_length_b                   48.764(11)
_cell_length_c                   3.6313(8)
_cell_measurement_reflns_used    2229
_cell_measurement_temperature    380
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     2766.1(11)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      380
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            5208
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.49
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.280
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  623 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1528
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0388P)²+3.0204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                1442
_reflns_number_total             1528
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            J-Mater-Chem-C-2015-3-7968.cif
_cod_data_source_block           380K
_cod_original_cell_volume        2766.1(12)
_cod_database_code               7234381
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/4-X,1/4+Y,1/4+Z
3 1/4+X,1/4-Y,1/4+Z
4 1/2-X,-Y,1/2+Z
5 +X,1/2+Y,1/2+Z
6 1/4-X,3/4+Y,3/4+Z
7 1/4+X,3/4-Y,3/4+Z
8 1/2-X,1/2-Y,+Z
9 1/2+X,+Y,1/2+Z
10 3/4-X,1/4+Y,3/4+Z
11 3/4+X,1/4-Y,3/4+Z
12 -X,-Y,+Z
13 1/2+X,1/2+Y,+Z
14 3/4-X,3/4+Y,1/4+Z
15 3/4+X,3/4-Y,1/4+Z
16 -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
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.21377(3) 0.120064(10) 0.6676(3) 0.0672(3) Uani 1.0 16 d . . .
S2 S 0.12214(3) 0.089439(11) 0.6996(3) 0.0659(3) Uani 1.0 16 d . . .
N1 N 0.29435(10) 0.09902(3) 0.7037(8) 0.0543(6) Uani 1.0 16 d . . .
N2 N 0.19103(11) 0.06457(3) 0.7337(7) 0.0532(6) Uani 1.0 16 d . . .
C1 C 0.27300(11) 0.07255(4) 0.7305(6) 0.0399(5) Uani 1.0 16 d . . .
C2 C 0.34000(11) 0.05157(3) 0.7565(6) 0.0331(4) Uani 1.0 16 d . . .
C3 C 0.42436(11) 0.05749(3) 0.6571(6) 0.0365(4) Uani 1.0 16 d . . .
C4 C 0.32047(11) 0.02507(4) 0.8733(6) 0.0365(4) Uani 1.0 16 d . . .
C5 C 0.48639(11) 0.03749(3) 0.6730(6) 0.0348(4) Uani 1.0 16 d . . .
C6 C 0.38229(11) 0.00505(3) 0.8855(6) 0.0356(4) Uani 1.0 16 d . . .
C7 C 0.46661(10) 0.01071(3) 0.7867(5) 0.0303(4) Uani 1.0 16 d . . .
H3 H 0.4387 0.0751 0.5796 0.0438 Uiso 1.0 16 calc R . .
H4 H 0.2648 0.0209 0.9439 0.0438 Uiso 1.0 16 calc R . .
H5 H 0.5424 0.0418 0.6074 0.0417 Uiso 1.0 16 calc R . .
H6 H 0.3676 -0.0126 0.9610 0.0428 Uiso 1.0 16 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
S2 S1 N1 94.31(7) yes . . .
S1 S2 N2 94.86(7) yes . . .
S1 N1 C1 114.92(13) yes . . .
S2 N2 C1 114.56(13) yes . . .
N1 C1 N2 121.34(17) yes . . .
N1 C1 C2 120.02(16) yes . . .
N2 C1 C2 118.64(17) yes . . .
C1 C2 C3 120.83(15) yes . . .
C1 C2 C4 120.67(16) yes . . .
C3 C2 C4 118.48(15) yes . . .
C2 C3 C5 120.47(15) yes . . .
C2 C4 C6 120.99(17) yes . . .
C3 C5 C7 121.10(16) yes . . .
C4 C6 C7 121.03(15) yes . . .
C5 C7 C6 117.92(15) yes . . .
C5 C7 C7 120.17(15) yes . . 12_655
C6 C7 C7 121.87(14) yes . . 12_655
C2 C3 H3 119.761 no . . .
C5 C3 H3 119.765 no . . .
C2 C4 H4 119.497 no . . .
C6 C4 H4 119.517 no . . .
C3 C5 H5 119.431 no . . .
C7 C5 H5 119.464 no . . .
C4 C6 H6 119.482 no . . .
C7 C6 H6 119.486 no . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
S1 S2 2.0718(8) yes . .
S1 N1 1.6293(17) yes . .
S2 N2 1.6261(17) yes . .
N1 C1 1.337(3) yes . .
N2 C1 1.338(3) yes . .
C1 C2 1.467(3) yes . .
C2 C3 1.397(3) yes . .
C2 C4 1.394(3) yes . .
C3 C5 1.376(3) yes . .
C4 C6 1.374(3) yes . .
C5 C7 1.404(3) yes . .
C6 C7 1.393(3) yes . .
C7 C7 1.476(3) yes . 12_655
C3 H3 0.930 no . .
C4 H4 0.930 no . .
C5 H5 0.930 no . .
C6 H6 0.930 no . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
N1 C3 2.873(3) no . .
N2 C4 2.838(3) no . .
C2 C7 2.810(3) no . .
C3 C6 2.767(3) no . .
C4 C5 2.759(3) no . .
C5 C6 3.018(3) no . 12_655
S1 S2 3.3270(10) no . 3_555
S1 N1 3.1433(19) no . 11_454
S2 S1 3.3270(10) no . 11_454
S2 N1 3.3586(19) no . 11_454
N1 S1 3.1433(19) no . 3_555
N1 S2 3.3586(19) no . 3_555
C2 C3 3.538(3) no . 1_556
C2 C4 3.471(3) no . 1_554
C3 C2 3.538(3) no . 1_554
C4 C2 3.471(3) no . 1_556
C5 C7 3.487(3) no . 1_554
C6 C7 3.538(3) no . 1_556
C7 C5 3.487(3) no . 1_556
C7 C6 3.538(3) no . 1_554
N1 H3 2.5791 no . .
N2 H4 2.5393 no . .
C1 H3 2.6489 no . .
C1 H4 2.6392 no . .
C2 H5 3.2424 no . .
C2 H6 3.2425 no . .
C3 H4 3.2383 no . .
C4 H3 3.2398 no . .
C5 H6 3.2390 no . .
C5 H6 2.7883 no . 12_655
C6 H5 3.2377 no . .
C6 H5 2.7610 no . 12_655
C7 H3 3.2570 no . .
C7 H4 3.2425 no . .
C7 H5 2.6453 no . 12_655
C7 H6 2.6675 no . 12_655
H3 H5 2.2949 no . .
H4 H6 2.2897 no . .
H5 H6 2.3792 no . 12_655
S1 H3 2.9690 no . 11_454
S2 H3 3.2564 no . 9_455
S2 H5 3.4025 no . 9_454
S2 H5 3.0240 no . 9_455
N2 H5 3.4352 no . 9_454
N2 H5 2.9100 no . 9_455
N2 H6 2.8730 no . 4_554
C2 H3 3.5533 no . 1_556
C2 H4 3.5114 no . 1_554
C3 H3 3.4652 no . 1_556
C4 H4 3.4913 no . 1_554
C4 H4 3.0372 no . 4_554
C4 H4 3.3297 no . 4_555
C4 H6 3.3534 no . 4_554
C5 H5 3.5100 no . 1_556
C6 H4 3.0737 no . 4_554
C6 H4 3.3145 no . 4_555
C6 H6 3.4726 no . 1_554
C7 H5 3.5466 no . 1_556
C7 H6 3.5590 no . 1_554
H3 S1 2.9690 no . 3_555
H3 S2 3.2564 no . 9_554
H3 C2 3.5533 no . 1_554
H3 C3 3.4652 no . 1_554
H4 C2 3.5114 no . 1_556
H4 C4 3.4913 no . 1_556
H4 C4 3.3297 no . 4_554
H4 C4 3.0372 no . 4_555
H4 C6 3.3145 no . 4_554
H4 C6 3.0737 no . 4_555
H4 H4 2.7670 no . 4_554
H4 H4 2.7670 no . 4_555
H4 H6 2.7413 no . 4_554
H4 H6 2.8227 no . 4_555
H5 S2 3.0240 no . 9_554
H5 S2 3.4025 no . 9_555
H5 N2 2.9100 no . 9_554
H5 N2 3.4352 no . 9_555
H5 C5 3.5100 no . 1_554
H5 C7 3.5466 no . 1_554
H5 H6 3.0853 no . 12_654
H6 N2 2.8730 no . 4_555
H6 C4 3.3534 no . 4_555
H6 C6 3.4726 no . 1_556
H6 C7 3.5590 no . 1_556
H6 H4 2.8227 no . 4_554
H6 H4 2.7413 no . 4_555
H6 H5 3.0853 no . 12_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
S2 S1 N1 C1 1.1(2) no . . . .
N1 S1 S2 N2 -0.75(12) no . . . .
S1 S2 N2 C1 0.31(18) no . . . .
S1 N1 C1 N2 -1.2(4) no . . . .
S1 N1 C1 C2 178.71(16) no . . . .
S2 N2 C1 N1 0.4(3) no . . . .
S2 N2 C1 C2 -179.45(15) no . . . .
N1 C1 C2 C3 -17.2(3) no . . . .
N1 C1 C2 C4 164.3(2) no . . . .
N2 C1 C2 C3 162.70(19) no . . . .
N2 C1 C2 C4 -15.8(3) no . . . .
C1 C2 C3 C5 -178.26(17) no . . . .
C1 C2 C4 C6 177.61(17) no . . . .
C3 C2 C4 C6 -0.9(3) no . . . .
C4 C2 C3 C5 0.3(3) no . . . .
C2 C3 C5 C7 0.4(3) no . . . .
C2 C4 C6 C7 0.9(3) no . . . .
C3 C5 C7 C6 -0.5(3) no . . . .
C3 C5 C7 C7 177.42(16) no . . . 12_655
C4 C6 C7 C5 -0.2(3) no . . . .
C4 C6 C7 C7 -178.03(17) no . . . 12_655
C5 C7 C7 C5 -140.24(16) no . . 12_655 12_655
C5 C7 C7 C6 37.5(3) no . . 12_655 12_655
C6 C7 C7 C5 37.5(3) no . . 12_655 12_655
C6 C7 C7 C6 -144.66(17) no . . 12_655 12_655
