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_7250023
_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         'C126 H86 Gd2 N18 O25'
_chemical_formula_sum            'C126 H86 Gd2 N18 O25'
_chemical_formula_weight         2566.62
_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             2023-02-23
_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                87.998(5)
_cell_angle_beta                 83.599(5)
_cell_angle_gamma                77.479(5)
_cell_formula_units_Z            2
_cell_length_a                   17.1488(9)
_cell_length_b                   18.0395(12)
_cell_length_c                   18.1496(11)
_cell_measurement_reflns_used    6684
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0320
_cell_measurement_theta_min      3.3600
_cell_volume                     5446.6(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.994
_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    -53.00  85.00   1.00  131.80    --   16.01   0.00  30.00  138
  2  \w    -53.00  35.00   1.00  131.80    --   16.01 -37.00-180.00   88
  3  \w    -77.00 -27.00   1.00  131.80    --  -16.33 138.00-106.13   50
  4  \w    -72.00 -21.00   1.00  131.80    --  -16.33 128.00  28.85   51
  5  \w    -25.00  23.00   1.00  131.80    --  -16.33 -99.00-180.00   48
  6  \w    -13.00  87.00   1.00  131.80    --   16.01  19.00-180.00  100
  7  \w    -51.00 -26.00   1.00  131.80    --   16.01 -57.00   0.00   25
;
_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      0.0000981000
_diffrn_orient_matrix_UB_12      -0.0390750000
_diffrn_orient_matrix_UB_13      -0.0034297000
_diffrn_orient_matrix_UB_21      -0.0199360000
_diffrn_orient_matrix_UB_22      0.0082643000
_diffrn_orient_matrix_UB_23      -0.0324668000
_diffrn_orient_matrix_UB_31      0.0376515000
_diffrn_orient_matrix_UB_32      -0.0053082000
_diffrn_orient_matrix_UB_33      -0.0219233000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.1621
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55809
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96033
_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            'clear light yellow'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       needle
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1560
_refine_ls_number_reflns         22172
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13043
_reflns_number_total             22172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01245c2.cif
_cod_data_source_block           DFX-Gd
_cod_depositor_comments
'Adding full bibliography for 7250020--7250024.cif.'
_cod_database_code               7250023
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Gd'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.697
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 H25A-O25
 0.95 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C6(H6), C7(H7A), C10(H10), C11(H11A), C12(H12A), C13(H13),
 C17(H17), C18(H18), C19(H19A), C20(H20A), C24(H24A), C25(H25), C27(H27),
 C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40),
  C41(H41), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C53(H53),
 C54(H54), C55(H55), 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)
3.b 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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88993
_shelx_fab_checksum              18593
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.775