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_7248528
_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 Nd O11, H2 O'
_chemical_formula_sum            'C24 H24 Nd O12'
_chemical_formula_weight         648.67
_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             2023-10-24
_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                 112.308(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4259(3)
_cell_length_b                   9.27290(10)
_cell_length_c                   15.4800(3)
_cell_measurement_reflns_used    11282
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      60.0240
_cell_measurement_theta_min      2.3990
_cell_volume                     2314.18(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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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    -68.00   0.00   0.50    0.06    --  -79.29  30.00 150.00  136
  2  \w    -69.00  -5.00   0.50    0.06    --  -79.29  30.00  90.00  128
  3  \w    -91.00 -40.00   0.50    0.06    --  -79.29  77.00 -60.00  102
  4  \w    -24.00  70.00   0.50    0.05    --   -1.48  57.00-150.00  188
  5  \w     12.00  65.00   0.50    0.05    --   -1.48  57.00-120.00  106
  6  \w   -124.00 -67.00   0.50    0.06    --  -79.29 145.00 -78.00  114
  7  \w   -153.00-127.00   0.50    0.06    --  -79.29-126.00  36.00   52
  8  \w   -123.00 -81.00   0.50    0.06    --  -79.29-126.00  36.00   84
  9  \w   -134.00-109.00   0.50    0.06    --  -79.29-145.00-131.00   50
 10  \w     -5.00  23.00   0.50    0.05    --   -1.48 -99.00   0.00   56
 11  \w   -106.00 -75.00   0.50    0.06    --  -79.29 126.00 112.00   62
 12  \w     -3.00  67.00   0.50    0.06    --   76.33 -30.00 -90.00  140
 13  \w     73.00 109.00   0.50    0.06    --   76.33-125.00 -90.00   72
 14  \w      9.00 102.00   0.50    0.06    --   76.33 -61.00-180.00  186
 15  \w     80.00 107.00   0.50    0.06    --   76.33 125.00-150.00   54
 16  \w     83.00 108.00   0.50    0.06    --   76.33 145.00 -78.00   50
 17  \w     85.00 121.00   0.50    0.06    --   76.33 126.00 112.00   72
;
_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      0.0791302000
_diffrn_orient_matrix_UB_12      -0.0376720000
_diffrn_orient_matrix_UB_13      0.0202889000
_diffrn_orient_matrix_UB_21      -0.0223165000
_diffrn_orient_matrix_UB_22      -0.1390668000
_diffrn_orient_matrix_UB_23      -0.0116588000
_diffrn_orient_matrix_UB_31      -0.0119974000
_diffrn_orient_matrix_UB_32      0.0095231000
_diffrn_orient_matrix_UB_33      -0.0905441000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13311
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         4.770
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    12.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43420
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.806
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0818P)^2^+1.7890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3567
_reflns_number_total             3969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248528
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Nd C H O N'
_shelx_estimated_absorpt_t_max   0.374
_shelx_estimated_absorpt_t_min   0.374
_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
 O12-H12B
 0.87 with sigma of 0.02
3.a Free rotating group:
 O12(H12A)
3.b Rotating group:
 O10(H10A,H10B), O11(H11A)
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), C21(H21), C10(H10), C13(H13), C12(H12), C18(H18), C6(H6A), C19(H19),
 C9(H9A), C3(H3), C2(H2), C22(H22)
3.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O5(H5)
;
_shelx_res_checksum              3404
_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 3.817
_oxdiff_exptl_absorpt_empirical_full_min 0.382