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_7248524
_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 Gd O11, H2 O'
_chemical_formula_sum            'C24 H24 Gd O12'
_chemical_formula_weight         661.68
_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     iterative
_audit_creation_date             2023-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.988(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2951(5)
_cell_length_b                   9.2984(2)
_cell_length_c                   15.4981(4)
_cell_measurement_reflns_used    7158
_cell_measurement_temperature    297.03(10)
_cell_measurement_theta_max      28.4960
_cell_measurement_theta_min      2.5280
_cell_volume                     2311.07(11)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.03(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 0.867
_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    -12.00  30.00   0.50    0.98    --  -20.01 -99.00 -90.00   84
  2  \w   -102.00   7.00   0.50    0.98    --  -20.01 -40.00  -8.00  218
  3  \w    -21.00  54.00   0.50    0.98    --  -20.01  40.00 145.00  150
  4  \w     65.00 102.00   0.50    0.98    --   21.26 178.00  60.00   74
  5  \w     50.00  99.00   0.50    0.98    --   21.26 178.00  30.00   98
;
_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      0.0330972000
_diffrn_orient_matrix_UB_12      0.0136548000
_diffrn_orient_matrix_UB_13      0.0430107000
_diffrn_orient_matrix_UB_21      -0.0281731000
_diffrn_orient_matrix_UB_22      0.0351480000
_diffrn_orient_matrix_UB_23      0.0165296000
_diffrn_orient_matrix_UB_31      -0.0081250000
_diffrn_orient_matrix_UB_32      -0.0662783000
_diffrn_orient_matrix_UB_33      0.0176935000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13294
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.849
_diffrn_reflns_theta_min         2.532
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75855
_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    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5258
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0265P)^2^+1.0381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4141
_reflns_number_total             5258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248524
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Gd C H O N'
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.591
_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
 H5-H9_$1
 2 with sigma of 0.02
3.a Free rotating group:
 O12(H12A,H12B)
3.b Rotating group:
 O11(H11A), O10(H10A,H10B)
3.c Ternary CH refined with riding coordinates:
 C16(H16), C15(H15), C24(H24)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C21(H21), C19(H19), C5(H5A), C2(H2), C13(H13), C22(H22),
 C6(H6A), C10(H10), C18(H18), C9(H9A)
3.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9), O5(H5)
;
_shelx_res_checksum              63765
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.629