An organic superconductor, (TEA)(HEDO-TTF-dc)<sub>2</sub>·2(H<sub>2</sub>C<sub>2</sub>O<sub>4</sub>), coupled with strong hydrogen-bonding interactions.
Morimachi, Yuto; Urai, Mizuki; Nakajima, Ryota; Kamebuchi, Hajime; Miyagawa, Kazuya; Kanoda, Kazushi; Zhou, Biao; Chemical communications (Cambridge, England) 59 (2023) 4162–4165; doi:10.1039/d3cc00080j

data_7131308
_publ_section_title
;
 An organic superconductor,
 (TEA)(HEDO-TTF-dc)<sub>2</sub>&#xb7;2(H<sub>2</sub>C<sub>2</sub>O<sub>4</sub>),
 coupled with strong hydrogen-bonding interactions.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4162
_journal_page_last               4165
_journal_paper_doi               10.1039/d3cc00080j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C10 H5 O6 S4, C4 H12 N'
_chemical_formula_sum            'C14 H17 N O6 S4'
_chemical_formula_weight         423.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.01.20 svn.r024a95a1 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-15 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8601(2)
_cell_length_b                   13.4801(4)
_cell_length_c                   19.2445(5)
_cell_measurement_reflns_used    15035
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.7130
_cell_measurement_theta_min      2.1590
_cell_volume                     1779.63(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.00
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -100.00  80.00   0.50    1.50    --  -10.00  45.00   0.00  360
  2  \w   -100.00  80.00   0.50    1.50    --  -10.00  45.00  90.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18774
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.153
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orangish
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.1896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3358
_reflns_number_total             3630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00080j2.cif
_cod_data_source_block           191001-eodc-tma-173k-
_cod_depositor_comments
'Adding full bibliography for 7131307--7131308.cif.'
_cod_database_code               7131308
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.946
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.77(9)
 0.23(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O5-C9 \\sim O5-C9A
 with sigma of 0.02
 O6-C10 \\sim O6-C10A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 O5-C10 \\sim O5-C10A
 with sigma of 0.04
 O6-C9 \\sim O6-C9A
 with sigma of 0.04
 O5-C9 \\sim O5-C9A \\sim O6-C10A \\sim O6-C10
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O3, H3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C9A(H9AA,H9AB), C10A(H10C,H10D)
;
_shelx_res_checksum              26465
_shelx_hkl_checksum              84927
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;