Construction of a redox-active metal-organic framework with an octanuclear lithium one-dimensional building block.
Li, Shu-Fan; Meng, Ya-Ru; Xu, Min-Jie; Zhang, Gen; Su, Jian; Chemical communications (Cambridge, England) 60 (2024) 8047–8050; doi:10.1039/d4cc02111h

data_7133264
_publ_section_title
;
 Construction of a redox-active metal-organic framework with an
 octanuclear lithium one-dimensional building block.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8047
_journal_page_last               8050
_journal_paper_doi               10.1039/d4cc02111h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C77 H61 Li8 N7 O19'
_chemical_formula_sum            'C77 H61 Li8 N7 O19'
_chemical_formula_weight         1443.84
_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             2024-05-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_cell_angle_alpha                95.736(2)
_cell_angle_beta                 94.844(2)
_cell_angle_gamma                102.727(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8956(6)
_cell_length_b                   13.8451(9)
_cell_length_c                   14.4170(9)
_cell_measurement_reflns_used    6068
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.31
_cell_volume                     1905.5(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28945
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.420
_diffrn_reflns_theta_max         24.420
_diffrn_reflns_theta_min         1.954
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1238 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.9299.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       needle
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1327P)^2^+1.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4709
_reflns_number_total             6261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02111h2.cif
_cod_data_source_block           Li8-MOF
_cod_depositor_comments          'Adding full bibliography for 7133264.cif.'
_cod_database_code               7133264
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O10-C35
 1.257 with sigma of 0.02
 N4-O10
 2.27 with sigma of 0.02
 N4-C35
 1.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Li3 \\sim O10 \\sim C35 \\sim N4 \\sim C37 \\sim C36: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Li3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C38A)=Sof(H38A)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C38)=Sof(H38)=FVAR(1)
 Fixed Sof: N4(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C36(0.5) H36A(0.5)
 H36B(0.5) H36C(0.5) O10(0.5) C35(0.5) H35(0.5)
5.a Riding coordinates:
 C36(H36A,H36B,H36C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C27(H27),
  C31(H31), C30(H30), C34(H34), C33(H33), C38(H38), C35(H35), C38A(H38A)
5.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C37(H37A,H37B,H37C), C40A(H40D,H40E,
 H40F), C39A(H39D,H39E,H39F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22398
_shelx_hkl_checksum              89560
_shelx_fab_checksum              92774
_olex2_submission_special_instructions 'No special instructions were received'