Construction of a stable radical hydrogen-bonded metal-organic framework with functionalized tetrathiafulvalene linkers.
Su, Jian; Han, Xiao; Ke, Si-Wen; Zhou, Xiao-Cheng; Yuan, Shuai; Ding, Mengning; Zuo, Jing-Lin; Chemical communications (Cambridge, England) 60 (2024) 5812–5815; doi:10.1039/d4cc01152j

data_7133024
_publ_section_title
;
 Construction of a stable radical hydrogen-bonded metal-organic framework
 with functionalized tetrathiafulvalene linkers.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5812
_journal_page_last               5815
_journal_paper_doi               10.1039/d4cc01152j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C38 H32 Cd O11 S4, 4(H2 O) 0.5(N O3) C2 H6 O'
_chemical_formula_sum            'C40 H46 Cd N0.5 O17.5 S4'
_chemical_formula_weight         1054.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-05-07 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.000(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.722(3)
_cell_length_b                   39.433(11)
_cell_length_c                   14.317(4)
_cell_measurement_reflns_used    3775
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.491
_cell_measurement_theta_min      2.305
_cell_volume                     6008(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  multi-scan
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.1064
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14330
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        22.722
_diffrn_reflns_theta_max         22.722
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear blackish black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7902
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0755
_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^)+(0.0940P)^2^+7.5226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4660
_reflns_number_total             7902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01152j2.cif
_cod_data_source_block           Cd-2-Me-H2TTFTB
_cod_depositor_comments          'Adding full bibliography for 7133024.cif.'
_cod_original_formula_sum        'C40 H46 Cd O17.5 N0.5 S4'
_cod_database_code               7133024
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.875
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H8 of O8
 At 1.5 times of:
  All C(H,H,H) groups, H3 of O3, All O(H,H) groups
2. Restrained distances
 H11A-H13B_$3
 2.4 with sigma of 0.02
 H11B-H13B_$3
 2.4 with sigma of 0.02
3. Rigid bond restraints
 O10, O11, O12, O13, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3A
5. Rigid body (RIGU) restrains
 O11, O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(H35)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=1-FVAR(1)
 Sof(H33)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
7.a Riding coordinates:
 O8(H8), O9(H9A,H9B), O10(H10A,H10B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,
 H14B)
7.b Rotating group:
 O11(H11A,H11B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6), C12(H12), C13(H13), C16(H16), C24(H24), C27(H27),
 C28(H28), C32(H32), C33(H33), C35(H35), C36(H36)
7.d Tetrahedral OH refined with riding coordinates:
 O3(H3)
7.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_smtbx_masks_special_details
;
The solvent masking procedure, as implemented in Olex2, was employed to eliminate
 the electronic contribution of solvent molecules during the refinement process. It's 
postulated that each asymmetric unit (ASU) contains one water molecule (H2O), half
 of a nitrate molecule (NO3), and one ethanol molecule, totaling 52 electrons per ASU.
 Due to the heavy-atom effect of sulfur (S) and cadmium (Cd) atoms, the electron 
density in the voids was slightly altered. Nevertheless, the results obtained from 
thermogravimetric analysis (TGA) can provide support for our analytical conclusions.
;
_shelx_res_checksum              91826
_shelx_hkl_checksum              10097
_shelx_fab_checksum              51951
_olex2_submission_original_sample_id Cd-2-Me-H2TTFTB
_olex2_submission_special_instructions 'No special instructions were received'