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_7248523
_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 Ce O11, H2 O'
_chemical_formula_sum            'C24 H24 Ce O12'
_chemical_formula_weight         644.55
_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             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-02 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.316(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3426(3)
_cell_length_b                   9.36730(10)
_cell_length_c                   15.5652(3)
_cell_measurement_reflns_used    11920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.1630
_cell_measurement_theta_min      2.3500
_cell_volume                     2371.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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   -107.00 -42.00   0.50    0.12    --  -78.15  77.00   0.00  130
  2  \w    -96.00 -18.00   0.50    0.12    --  -78.15  57.00  30.00  156
  3  \w    -29.00  -4.00   0.50    0.12    --  -78.15  77.00   0.00   50
  4  \w    -26.00  -1.00   0.50    0.12    --  -78.15  38.00-120.00   50
  5  \w    -71.00 -31.00   0.50    0.12    --  -78.15  38.00-120.00   80
  6  \w   -143.00-118.00   0.50    0.12    --  -78.15-109.00 -75.00   50
  7  \w   -117.00 -88.00   0.50    0.12    --  -78.15 -99.00 -60.00   58
  8  \w   -150.00 -88.00   0.50    0.12    --  -78.15 -99.00   0.00  124
  9  \w     -7.00  35.00   0.50    0.05    --   -0.78 -99.00-180.00   84
 10  \w     -8.00  35.00   0.50    0.05    --   -0.78 -99.00-150.00   86
 11  \w   -138.00 -88.00   0.50    0.12    --  -78.15 -77.00 -30.00  100
 12  \w   -105.00  -8.00   0.50    0.12    --  -78.15 109.00  21.00  194
 13  \w      1.00  38.00   0.50    0.05    --   -0.78 -99.00  30.00   74
 14  \w     -4.00  22.00   0.50    0.05    --   -0.78 -99.00  90.00   52
 15  \w      3.00  33.00   0.50    0.05    --   -0.78 -99.00 120.00   60
 16  \w      0.00  71.00   0.50    0.12    --   76.59 -38.00 -30.00  142
 17  \w     37.00  66.00   0.50    0.12    --   76.59-109.00 -75.00   58
 18  \w     87.00 133.00   0.50    0.12    --   76.59 109.00  21.00   92
 19  \w     80.00 147.00   0.50    0.12    --   76.59 125.00 -30.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0173072000
_diffrn_orient_matrix_UB_12      0.1255697000
_diffrn_orient_matrix_UB_13      -0.0435950000
_diffrn_orient_matrix_UB_21      0.0100706000
_diffrn_orient_matrix_UB_22      -0.0589122000
_diffrn_orient_matrix_UB_23      -0.0738205000
_diffrn_orient_matrix_UB_31      -0.0798780000
_diffrn_orient_matrix_UB_32      -0.0345166000
_diffrn_orient_matrix_UB_33      -0.0326908000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18636
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.293
_diffrn_reflns_theta_min         2.362
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    10.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    1.805
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.559
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5280
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0375P)^2^+0.9934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4522
_reflns_number_total             5280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           gm-36-15_auto
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248523
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Ce C H O N'
_shelx_estimated_absorpt_t_max   0.076
_shelx_estimated_absorpt_t_min   0.076
_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
 H00A-H00G
 2.1 with sigma of 0.02
 H00G-H00A
 2.3 with sigma of 0.02
3.a Free rotating group:
 O00C(H00F,H00G)
3.b Rotating group:
 O008(H00A,H00B), O00R(H00C,H00D)
3.c Ternary CH refined with riding coordinates:
 C00I(H00I), C00W(H00W), C00Z(H00Z)
3.d Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q),
 C00T(H00T), C00V(H00V), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011)
3.e Idealised tetrahedral OH refined as rotating group:
 O002(H002), O003(H003), O005(H005)
;
_shelx_res_checksum              36946
_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 2.012
_oxdiff_exptl_absorpt_empirical_full_min 0.665