Syntheses, crystal structures and properties of a series of isostructural lanthanide organic frameworks
Guan, Ming-Xue; Li, Hui-Zi; Li, Shangda; Yang, Han-Jiang; Wang, Fei; Zhang, Jian; CrystEngComm 26 (2024) 2770–2774; doi:10.1039/D4CE00292J

data_7248527
_publ_section_title
;
 Syntheses, crystal structures and properties of a series of isostructural
 lanthanide organic frameworks
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              2770
_journal_page_last               2774
_journal_paper_doi               10.1039/D4CE00292J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C24 H22 O11 Tb, H2 O'
_chemical_formula_sum            'C24 H24 O12 Tb'
_chemical_formula_weight         663.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.661(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3235(7)
_cell_length_b                   9.2270(3)
_cell_length_c                   15.4275(6)
_cell_measurement_reflns_used    6595
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.8280
_cell_measurement_theta_min      2.5320
_cell_volume                     2275.62(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -55.00  -5.00   0.50    6.08    --   -6.67 -38.00  90.00  100
  2  \w     -8.00  27.00   0.50    6.08    --   -6.67 -99.00   0.00   70
  3  \w    -18.00  32.00   0.50    6.08    --    7.84 -99.00  30.00  100
  4  \w     -8.00  80.00   0.50    6.08    --    7.84  38.00  30.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210358000
_diffrn_orient_matrix_UB_12      0.0670552000
_diffrn_orient_matrix_UB_13      -0.0149602000
_diffrn_orient_matrix_UB_21      0.0384118000
_diffrn_orient_matrix_UB_22      0.0374279000
_diffrn_orient_matrix_UB_23      0.0216682000
_diffrn_orient_matrix_UB_31      0.0070073000
_diffrn_orient_matrix_UB_32      -0.0044680000
_diffrn_orient_matrix_UB_33      -0.0422778000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12389
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.548
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4025
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0241P)^2^+1.9688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3271
_reflns_number_total             4025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248527
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Tb C H O N '
_shelx_estimated_absorpt_t_max   0.569
_shelx_estimated_absorpt_t_min   0.569
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H6_$1-H9_$2
 2.1 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
5.a Free rotating group:
 O12(H12A,H12B)
5.b Rotating group:
 O10(H10A,H10B), O11(H11A,H11B)
5.c Ternary CH refined with riding coordinates:
 C15(H15), C24(H24), C16(H16)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5A), C12(H12), C19(H19), C10(H10), C21(H21), C13(H13), C6(H6A), C3(H3),
 C9(H9A), C22(H22), C18(H18), C2(H2)
5.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9), O5(H5)
;
_shelx_res_checksum              60849
_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 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.593