(Z)-4,4′-Stilbene dicarboxylic acid, the overlooked metal–organic framework linker
Hunter, Lucy R.; Karlsson, Joshua K. G.; Sellars, Jonathan D.; Probert, Michael R.; CrystEngComm 25 (2023) 2353–2358; doi:10.1039/D3CE00138E

data_7246520
_publ_section_title
;
 (Z)-4,4&#x2032;-Stilbene dicarboxylic acid, the overlooked metal--organic
 framework linker
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2353
_journal_page_last               2358
_journal_paper_doi               10.1039/D3CE00138E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C51 H43 N O16 Tb2, 3(C3 H7 N O)'
_chemical_formula_sum            'C60 H64 N4 O19 Tb2'
_chemical_formula_weight         1462.99
_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             2023-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-10 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                83.589(4)
_cell_angle_beta                 78.689(4)
_cell_angle_gamma                84.942(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8353(10)
_cell_length_b                   13.8578(13)
_cell_length_c                   22.505(2)
_cell_measurement_reflns_used    8876
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.25
_cell_measurement_theta_min      4.60
_cell_volume                     2982.0(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100645
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.788
_diffrn_reflns_theta_min         3.216
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.160
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1620 before and 0.1135 after correction.
The Ratio of minimum to maximum transmission is 0.4392.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.00154(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11426
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1298P)^2^+5.0397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9809
_reflns_number_total             11426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00138e2.cif
_cod_data_source_block           mof8_tb_3d
_cod_depositor_comments
'Adding full bibliography for 7246512--7246521.cif.'
_cod_database_code               7246520
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.323
_olex2_refinement_description
;
1. Restrained distances
 Tb1-H1A \\sim Tb1-H1B
 with sigma of 0.02
 Tb2-H7A \\sim Tb2-H7B
 with sigma of 0.02
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O1(H1A,H1B), O7(H7A,H7B)
3.b Rotating group:
 O2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C01C(H01C), C02A(H02J), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C020(H020),
 C21(H21), C22(H22), C24(H24), C25(H25), C026(H026), C27(H27), C28(H28),
 C29(H29), C30(H30), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C43(H43), C44(H44), C45(H45), C46(H46)
3.d Idealised Me refined as rotating group:
 C01Y(H01A,H01B,H01D), C02B(H02D,H02E,H02F), C02C(H02K,H02L,H02M), C023(H02A,
 H02B,H02C), C027(H02N,H02O,H02P), C028(H02G,H02H,H02I), C029(H02Q,H02R,H02S),
 C49(H49A,H49B,H49C)
;
_shelx_res_checksum              8217
_shelx_hkl_checksum              23652
_olex2_submission_special_instructions 'No special instructions were received'