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_7248531
_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 Sm, H2 O'
_chemical_formula_sum            'C24 H23 O12 Sm'
_chemical_formula_weight         653.77
_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
_audit_creation_date             2023-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.620(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3836(3)
_cell_length_b                   9.24400(10)
_cell_length_c                   15.4813(3)
_cell_measurement_reflns_used    12094
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      60.1020
_cell_measurement_theta_min      2.3950
_cell_volume                     2296.38(7)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     58.00  83.00   0.50    0.29    --   75.32  77.00   0.00   50
  2  \w     80.00 149.00   0.50    0.29    --   75.32 125.00 150.00  138
  3  \w    113.00 149.00   0.50    0.29    --   75.32  77.00   0.00   72
  4  \w     80.00 139.00   0.50    0.29    --   75.32 125.00-150.00  118
  5  \w     64.00 103.00   0.50    0.29    --   75.32  41.00 -75.00   78
  6  \w   -144.00 -55.00   0.50    0.29    --  -78.14 -57.00 120.00  178
  7  \w   -136.00-104.00   0.50    0.29    --  -78.14 -41.00 131.00   64
  8  \w    -77.00 -16.00   0.50    0.07    --   -1.41 -41.00 131.00  122
  9  \w    -11.00  20.00   0.50    0.07    --   -1.41 -41.00 131.00   62
 10  \w    -70.00  -2.00   0.50    0.29    --  -78.14  38.00  30.00  136
 11  \w   -107.00 -81.00   0.50    0.29    --  -78.14  77.00 150.00   52
 12  \w    -67.00 -25.00   0.50    0.29    --  -78.14  38.00 120.00   84
 13  \w    -59.00  -2.00   0.50    0.29    --  -78.14  41.00 -75.00  114
 14  \w    -71.00 -13.00   0.50    0.29    --  -78.14  38.00-120.00  116
 15  \w      6.00  58.00   0.50    0.07    --   -1.41  41.00 -75.00  104
 16  \w      1.00  73.00   0.50    0.29    --   75.32 -41.00 131.00  144
 17  \w     -7.00  38.00   0.50    0.07    --   -1.41 -99.00   0.00   90
 18  \w   -152.00 -85.00   0.50    0.29    --  -78.14-125.00 -90.00  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      0.0589628000
_diffrn_orient_matrix_UB_12      0.0663984000
_diffrn_orient_matrix_UB_13      -0.0212540000
_diffrn_orient_matrix_UB_21      -0.0571410000
_diffrn_orient_matrix_UB_22      0.0357694000
_diffrn_orient_matrix_UB_23      -0.0840642000
_diffrn_orient_matrix_UB_31      -0.0151296000
_diffrn_orient_matrix_UB_32      0.1235928000
_diffrn_orient_matrix_UB_33      0.0356161000
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.917
_diffrn_reflns_theta_max         52.917
_diffrn_reflns_theta_min         2.394
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    13.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27649
_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    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4049
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0383P)^2^+2.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3501
_reflns_number_total             4049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248531
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sm C H O N'
_shelx_estimated_absorpt_t_max   0.168
_shelx_estimated_absorpt_t_min   0.168
_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
 Sm1-H11A \\sim Sm1-H11B
 with sigma of 0.02
3.a Free rotating group:
 O12(H12A,H12B), O11(H11A,H11B)
3.b Rotating group:
 O10(H10A,H10B)
3.c Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C24(H24)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5A), C10(H10), C9(H9A), C13(H13), C21(H21), C12(H12), C6(H6A), C19(H19),
 C18(H18), C2(H2), C3(H3), C22(H22)
3.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O5(H5), O9(H9)
;
_shelx_res_checksum              45180
_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 2.715
_oxdiff_exptl_absorpt_empirical_full_min 0.602