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_7243059
_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         684.74
_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   mixed
_atom_sites_solution_primary     iterative
_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                106.291(9)
_cell_angle_beta                 97.991(9)
_cell_angle_gamma                103.267(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4537(17)
_cell_length_b                   14.128(3)
_cell_length_c                   18.021(4)
_cell_measurement_reflns_used    3650
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.41
_cell_volume                     1962.5(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1757
_diffrn_reflns_av_unetI/netI     0.1751
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_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            12077
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        20.816
_diffrn_reflns_theta_max         20.816
_diffrn_reflns_theta_min         2.413
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2832
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1847 before and 0.0897 after correction.
The Ratio of minimum to maximum transmission is 0.3798.
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    1.159
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_preparation       'immersed in CHCl3'
_exptl_crystal_recrystallization_method 'immersed in CHCl3'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.442
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         4074
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.439
_refine_ls_R_factor_all          0.2914
_refine_ls_R_factor_gt           0.1694
_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          0.4085
_refine_ls_wR_factor_ref         0.4897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1794
_reflns_number_total             4074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00519g2.cif
_cod_data_source_block           mo_h4ttftb10_0m
_cod_depositor_comments
'Adding full bibliography for 7243058--7243060.cif.'
_cod_database_code               7243059
_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. Rigid bond restraints
 C00X, C012, C00R, C00W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00J \\sim C00E \\sim C00H \\sim C00L \\sim C00N \\sim C00D: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C00F) \\sim Ueq, Uanis(C00Q) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Everything fixed:
 H007
4.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00E(H00E), C00J(H00J), C00K(H00K), C00L(H00L),
 C00N(H00N), C00P(H00P), C00Z(H00Z), C010(H010), C011(H011), C013(H013),
 C014(H014), C017(H017), C018(H018), C019(H019)
4.c Tetrahedral OH refined with riding coordinates:
 O00M(H00M), O00U(H00U)
4.d Idealised tetrahedral OH refined as rotating group:
 O008(H008)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_fab_checksum              34451
_shelx_shelxl_version_number     2016/6
_olex2_submission_original_sample_id PFC-77
_olex2_submission_special_instructions 'No special instructions were received'