Deferasirox HOF and its in situ metallization affording a new family of lanthanide coordination polymer-based MHOFs
Cao, Yue-Mei; He, Ying; Pei, Xin-Yue; Liang, Jia-Xing; Feng, Jing; Wang, Hong-Yan; Bo, Qi-Bing; CrystEngComm 27 (2025) 2175–2189; doi:10.1039/D4CE01245C

data_7250024
_publ_section_title
;
 Deferasirox HOF and its in situ metallization affording a new family of
 lanthanide coordination polymer-based MHOFs
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2175
_journal_page_last               2189
_journal_paper_doi               10.1039/D4CE01245C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C252 H174 N36 O51 Tb4'
_chemical_formula_sum            'C252 H174 N36 O51 Tb4'
_chemical_formula_weight         5157.94
_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             2023-02-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-02-25 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                82.461(2)
_cell_angle_beta                 77.237(2)
_cell_angle_gamma                88.009(2)
_cell_formula_units_Z            2
_cell_length_a                   18.0208(4)
_cell_length_b                   18.1390(4)
_cell_length_c                   35.2150(9)
_cell_measurement_reflns_used    25198
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6550
_cell_measurement_theta_min      3.4590
_cell_volume                     11129.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  55.00   1.00  139.32    --   16.17 -99.00 120.00   80
  2  \w     -3.00  85.00   1.00  139.32    --   16.17  37.00 -60.00   88
  3  \w    -13.00  88.00   1.00  139.32    --   16.17  19.00  60.00  101
  4  \w    -25.00  55.00   1.00  139.32    --   16.17 -99.00-150.00   80
  5  \w    -25.00  22.00   1.00  139.32    --  -16.64 -99.00 -30.00   47
  6  \w    -25.00  55.00   1.00  139.32    --   16.17 -99.00   0.00   80
  7  \w    -13.00  88.00   1.00  139.32    --   16.17  19.00-180.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120195000
_diffrn_orient_matrix_UB_12      0.0374524000
_diffrn_orient_matrix_UB_13      -0.0054998000
_diffrn_orient_matrix_UB_21      -0.0366280000
_diffrn_orient_matrix_UB_22      0.0123665000
_diffrn_orient_matrix_UB_23      0.0090507000
_diffrn_orient_matrix_UB_31      0.0119452000
_diffrn_orient_matrix_UB_32      -0.0005592000
_diffrn_orient_matrix_UB_33      0.0179253000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            39241
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             5212
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.477
_refine_diff_density_min         -4.493
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3127
_refine_ls_number_reflns         39241
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      2.357
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+53.2199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29942
_reflns_number_total             39241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01245c2.cif
_cod_data_source_block           DFX-Tb
_cod_depositor_comments
'Adding full bibliography for 7250020--7250024.cif.'
_cod_database_code               7250024
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.844
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.497(13)
 0.503(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H50A,H50B} of O50, {H49A,H49B} of O49
 At 1.5 times of:
  All O(H) groups, {H51A,H51B} of O51, {H51C,H51D} of O51A
3. Restrained distances
 Tb5-O51A
 2.117 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O51) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.001
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O51) = Uanis(O51A)
5. Others
 Fixed Sof: Tb4(0.9) Tb5(0.1) O51(0.9) H51A(0.9) H51B(0.9) O51A(0.1) H51C(0.1)
 H51D(0.1)
6.a Rotating group:
 O51(H51A,H51B), O51A(H51C,H51D)
6.b Secondary CH2 refined with riding coordinates:
 O49(H49A,H49B), O50(H50A,H50B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C6(H6), C7(H7A), C11(H11A), C12(H12A), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19A), C20(H20A), C24(H24A), C25(H25), C27(H27A),
 C28(H28A), C30(H30), C31(H31A), C32(H32A), C33(H33), C39(H39A), C40(H40A),
 C41(H41), C42(H42), C45(H45), C46(H46), C48(H48A), C53(H53), C54(H54),
 C55(H55), C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C66(H66), C67(H67),
  C69(H69), C70(H70), C73(H73), C74(H74), C75(H75), C76(H76), C80(H80),
 C81(H81), C82(H82), C83(H83), C87(H87), C88(H88), C90(H90), C91(H91), C94(H94),
  C95(H95), C96(H96), C97(H97), C101(H101), C102(H102), C103(H103), C104(H104),
 C108(H108), C109(H109), C111(H111), C112(H112), C115(H115), C116(H116),
 C117(H117), C118(H118), C122(H122), C123(H123), C124(H124), C125(H125),
 C129(H129), C130(H130), C132(H132), C133(H133), C136(H136), C137(H137),
 C138(H138), C139(H139), C144(H144), C145(H145), C146(H146), C147(H147),
 C150(H150), C151(H151), C153(H153), C154(H154), C157(H157), C158(H158),
 C159(H159), C160(H160), C165(H165), C166(H166), C167(H167), C168(H168),
 C171(H171), C172(H172), C174(H174), C175(H175), C179(H179), C180(H180),
 C181(H181), C182(H182), C185(H185), C186(H186), C187(H187), C188(H188),
 C192(H192), C193(H193), C195(H195), C196(H196), C200(H200), C201(H201),
 C202(H202), C203(H203), C206(H206), C207(H207), C208(H208), C209(H209),
 C213(H213), C214(H214), C216(H216), C217(H217), C220(H220), C221(H221),
 C222(H222), C223(H223), C227(H227), C228(H228), C229(H229), C230(H230),
 C234(H234), C235(H235), C237(H237), C238(H238), C241(H241), C242(H242),
 C243(H243), C244(H244), C248(H248), C249(H249), C250(H250), C251(H251),
 C254(H254)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O7(H7), O8(H8), O11(H11), O12(H12), O15(H15), O16(H16),
 O19(H19), O20(H20), O23(H23), O24(H24), O27(H27), O28(H28), O31(H31), O32(H32),
  O35(H35), O36(H36), O39(H39), O40(H40), O43(H43), O44(H44), O47(H47), O48(H48)
;
_shelx_res_checksum              91632
_shelx_fab_checksum              63311
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.673