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_7243060
_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         'C34 H20 O8 S4'
_chemical_formula_sum            'C34 H20 O8 S4'
_chemical_formula_weight         684.77
_chemical_name_systematic        PFC-78
_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   mixed
_audit_creation_date             2021-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2021-04-15 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                114.88(5)
_cell_angle_beta                 96.22(6)
_cell_angle_gamma                95.19(7)
_cell_formula_units_Z            2
_cell_length_a                   8.301(7)
_cell_length_b                   18.954(18)
_cell_length_c                   20.558(15)
_cell_measurement_reflns_used    4978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.719
_cell_measurement_theta_min      2.200
_cell_volume                     2884(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1408
_diffrn_reflns_av_unetI/netI     0.1413
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13491
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        18.960
_diffrn_reflns_theta_max         18.959
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    0.040
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1669 before and 0.1090 after correction.
The Ratio of minimum to maximum transmission is 0.6107.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.070
_exptl_crystal_description       block
_exptl_crystal_F_000             62
_exptl_crystal_preparation       'immersed in acetone'
_exptl_crystal_recrystallization_method 'immersed in acetone'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.606
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.897
_refine_ls_R_factor_all          0.2800
_refine_ls_R_factor_gt           0.1960
_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          0.4930
_refine_ls_wR_factor_ref         0.5540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2404
_reflns_number_total             4544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00519g2.cif
_cod_data_source_block           mo_gxy20210125pfc78_0m_a
_cod_depositor_comments
;
Adding full bibliography for 7243058--7243060.cif.

2024-10-30
Formula introduced (only elements indicated)
                 miguel
;
_cod_original_formula_sum            'C H O S'
_cod_original_formula_weight         61.08
_cod_database_code               7243060
_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
 O4-H4
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(S2) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(S4) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) = Uanis(S4)
Uanis(C9) = Uanis(C8)
Uanis(C19) = Uanis(C27)
Uanis(C9) = Uanis(C27)
Uanis(C28) = Uanis(C20)
Uanis(C7) = Uanis(C10)
Uanis(C21) = Uanis(C13)
Uanis(O5) = Uanis(O1)
Uanis(C26) = Uanis(C12)
Uanis(C33) = Uanis(C23)
Uanis(C16) = Uanis(C24)
Uanis(C11) = Uanis(C25)
Uanis(C23) = Uanis(C15)
Uanis(C2) = Uanis(C34)
Uanis(C26) = Uanis(C22)
Uanis(C12) = Uanis(C14)
Uanis(S4) = Uanis(S1)
Uanis(S3) = Uanis(S4)
Uanis(C34) = Uanis(C24)
Uanis(C31) = Uanis(C6)
Uanis(C33) = Uanis(C1)
Uanis(C5) = Uanis(C29)
Uanis(O4) = Uanis(O1)
Uanis(C22) = Uanis(C21) = Uanis(C20) = Uanis(C25) = Uanis(C26) = Uanis(C23)
Uanis(C12) = Uanis(C15) = Uanis(C14) = Uanis(C13) = Uanis(C10) = Uanis(C11)
4.a Riding coordinates:
 C1(H4)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C26(H26), C25(H25), C29(H29), C30(H30), C32(H32),
 C31(H31), C11(H11), C13(H13), C14(H14), C12(H12), C3(H3), C5(H5A), C6(H6),
 C4(H4A)
4.c Fitted hexagon refined as free rotating group:
 C21(C22,C23,C26,C25,C20), C28(C29,C30,C33,C32,C31), C11(C10,C13,C14,C15,C12),
 C3(C2,C5,C6,C7,C4)
4.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O5(H5), O8(H8)
;
_shelx_fab_checksum              10693
_shelx_shelxl_version_number     2016/6
_olex2_submission_original_sample_id PFC-78
_olex2_submission_special_instructions 'No special instructions were received'