#------------------------------------------------------------------------------
#$Date: 2020-09-12 04:09:14 +0300 (Sat, 12 Sep 2020) $
#$Revision: 256371 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559073.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_1559073
loop_
_publ_author_name
'Kobayashi, Yuka'
'Hirata, Kazuto'
'Hood, Samantha'
'Yang, Hui'
'Walsh, Aron'
'Matsushita, Yoshitaka'
'Ishioka, Kunie'
_publ_section_title
;
 Crystal structure and metallization mechanism of the π-radical metal TED
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03521A
_journal_year                    2020
_chemical_formula_sum            'C12 H2.5 O4 S8'
_chemical_formula_weight         467.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-04-29 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.506(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7464(2)
_cell_length_b                   11.8946(6)
_cell_length_c                   20.2094(11)
_cell_measurement_reflns_used    9455
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      39.44
_cell_measurement_theta_min      2.65
_cell_volume                     898.88(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11520
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.426
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.7764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             469
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.538
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0538
_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/[σ²(Fo²)+(0.0619P)²+5.3024P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1728
_reflns_number_total             1922
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03521a2.cif
_cod_data_source_block           kobayashi_y202001g_113k1_0m
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C12 H2.50 O4 S8'
_cod_database_code               1559073
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.983
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.3961(11) 0.6938(4) 0.7641(2) 0.0170(8) Uani 1 1 d . . . . .
H1 H -0.473362 0.652383 0.800763 0.020 Uiso 1 1 calc R U . . .
C2 C -0.1580(14) 0.750000 0.6520(3) 0.0110(10) Uani 1 2 d S T P . .
C3 C -0.0208(14) 0.750000 0.5909(3) 0.0104(10) Uani 1 2 d S T P . .
C4 C 0.2157(9) 0.6935(3) 0.47994(17) 0.0098(7) Uani 1 1 d . . . . .
C5 C 0.4546(14) 0.750000 0.3688(3) 0.0110(10) Uani 1 2 d S T P . .
C6 C 0.5916(14) 0.750000 0.3088(3) 0.0112(10) Uani 1 2 d S T P . .
C7 C 0.8426(10) 0.6931(3) 0.19732(19) 0.0145(8) Uani 1 1 d . . . . .
C8 C 0.9500(13) 0.6102(4) 0.1460(2) 0.0240(10) Uani 1 1 d . . . . .
O1 O 0.9086(10) 0.5099(3) 0.15819(17) 0.0309(8) Uani 1 1 d . . . . .
O2 O 1.0850(10) 0.6483(3) 0.09319(18) 0.0360(9) Uani 1 1 d . . . . .
H1O H 1.02(5) 0.750000 0.082(10) 0.054 Uiso 0.5 2 d S U P . .
S1 S -0.2491(3) 0.62625(8) 0.69431(5) 0.0126(3) Uani 1 1 d . . . . .
S2 S 0.0846(2) 0.62424(7) 0.55032(5) 0.0100(3) Uani 1 1 d . . . . .
S3 S 0.3547(2) 0.62399(7) 0.41031(5) 0.0104(3) Uani 1 1 d . . . . .
S4 S 0.6895(3) 0.62556(8) 0.26684(5) 0.0129(3) Uani 1 1 d . . . . .
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 Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 S1 117.49(14) 4_575 . ?
C1 C1 H1 121.3 4_575 . ?
S1 C1 H1 121.3 . . ?
C3 C2 S1 122.58(15) . 4_575 ?
C3 C2 S1 122.58(15) . . ?
S1 C2 S1 114.8(3) 4_575 . ?
C2 C3 S2 121.88(15) . . ?
C2 C3 S2 121.88(15) . 4_575 ?
S2 C3 S2 116.1(3) . 4_575 ?
C4 C4 S3 118.40(13) 4_575 . ?
C4 C4 S2 118.26(13) 4_575 . ?
S3 C4 S2 123.3(2) . . ?
C6 C5 S3 122.09(15) . . ?
C6 C5 S3 122.09(15) . 4_575 ?
S3 C5 S3 115.8(3) . 4_575 ?
C5 C6 S4 122.52(15) . . ?
C5 C6 S4 122.52(15) . 4_575 ?
S4 C6 S4 115.0(3) . 4_575 ?
C7 C7 C8 131.0(2) 4_575 . ?
C7 C7 S4 117.39(14) 4_575 . ?
C8 C7 S4 111.6(3) . . ?
O1 C8 O2 124.5(4) . . ?
O1 C8 C7 117.1(4) . . ?
O2 C8 C7 118.3(4) . . ?
C8 O2 H1O 114(9) . . ?
C1 S1 C2 95.1(2) . . ?
C4 S2 C3 93.5(2) . . ?
C4 S3 C5 93.6(2) . . ?
C7 S4 C6 95.1(2) . . ?
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
C1 C1 1.336(8) 4_575 ?
C1 S1 1.741(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.365(8) . ?
C2 S1 1.747(3) 4_575 ?
C2 S1 1.747(3) . ?
C3 S2 1.763(3) . ?
C3 S2 1.763(3) 4_575 ?
C4 C4 1.343(8) 4_575 ?
C4 S3 1.739(4) . ?
C4 S2 1.740(4) . ?
C5 C6 1.345(8) . ?
C5 S3 1.769(3) . ?
C5 S3 1.769(3) 4_575 ?
C6 S4 1.755(3) . ?
C6 S4 1.755(3) 4_575 ?
C7 C7 1.354(8) 4_575 ?
C7 C8 1.503(6) . ?
C7 S4 1.745(4) . ?
C8 O1 1.230(6) . ?
C8 O2 1.292(6) . ?
O2 H1O 1.25(5) . ?
