Single-crystal-to-single-crystal transformation of tetrathiafulvalene-based hydrogen-bonded organic frameworks
Gao, Xiang-Yu; Li, Yu-Lin; Liu, Tian-Fu; Huang, Xin-Song; Cao, Rong; CrystEngComm 23 (2021) 4743–4747; doi:10.1039/D1CE00519G

data_7243058
_publ_section_title
;
 Single-crystal-to-single-crystal transformation of
 tetrathiafulvalene-based hydrogen-bonded organic frameworks
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              4743
_journal_page_last               4747
_journal_paper_doi               10.1039/D1CE00519G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C17 H10 O4 S2'
_chemical_formula_sum            'C17 H10 O4 S2'
_chemical_formula_weight         342.37
_chemical_name_systematic        PFC-77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-15 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                81.532(19)
_cell_angle_beta                 81.28(2)
_cell_angle_gamma                86.70(2)
_cell_formula_units_Z            2
_cell_length_a                   5.778(3)
_cell_length_b                   13.713(7)
_cell_length_c                   16.811(8)
_cell_measurement_reflns_used    3602
_cell_measurement_temperature    140.15
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.48
_cell_volume                     1301.4(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      140.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8974
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.723
_diffrn_reflns_theta_max         22.723
_diffrn_reflns_theta_min         3.006
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1370 before and 0.0928 after correction.
The Ratio of minimum to maximum transmission is 0.4449.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.874
_exptl_crystal_description       needle
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.395
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.395
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.1420
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4046
_refine_ls_wR_factor_ref         0.4283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1953
_reflns_number_total             3487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00519g2.cif
_cod_data_source_block           mo_h4ttftbgxy20200826_0ma_a_sqd_pl_sq
_cod_depositor_comments
'Adding full bibliography for 7243058--7243060.cif.'
_cod_database_code               7243058
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H4a-O3_$1
 1.775 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C12) = Uanis(C14) = Uanis(C13) = Uanis(C15) = Uanis(C16)
Uanis(S1) = Uanis(S2) = Uanis(C10) = Uanis(C8) = Uanis(C9)
Uanis(C2) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C3) = Uanis(C4)
Uanis(O3) = Uanis(O4) = Uanis(C17)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C12(H12), C3(H3), C4(H4), C14(H14), C13(H13), C15(H15)
4.b Tetrahedral OH refined with riding coordinates:
 O4(H4a)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              7100
_shelx_hkl_checksum              50402
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id HOF-H4TTFTB
_olex2_submission_special_instructions 'No special instructions were received'