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_7248529
_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 Eu O11, H2 O'
_chemical_formula_sum            'C24 H24 Eu O12'
_chemical_formula_weight         656.39
_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             2023-06-08
_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                 111.900(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2995(3)
_cell_length_b                   9.31930(10)
_cell_length_c                   15.4902(2)
_cell_measurement_reflns_used    11447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.2200
_cell_measurement_theta_min      4.7730
_cell_volume                     2317.10(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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     20.00 108.00   0.50    0.71    --   76.59-125.00   0.00  176
  2  \w     42.00  68.00   0.50    0.71    --   76.59-108.00  19.00   52
  3  \w     -4.00  38.00   0.50    0.18    --   -0.78 -99.00 -90.00   84
  4  \w     -2.00  26.00   0.50    0.18    --   -0.78 -99.00 -60.00   56
  5  \w     10.00  36.00   0.50    0.18    --   -0.78 -99.00-150.00   52
  6  \w     10.00  36.00   0.50    0.18    --   -0.78 -99.00-180.00   52
  7  \w     -8.00  17.00   0.50    0.18    --   -0.78 -99.00 -30.00   50
  8  \w      5.00  36.00   0.50    0.18    --   -0.78 -99.00 120.00   62
  9  \w     88.00 140.00   0.50    0.71    --   76.59 108.00 116.00  104
 10  \w   -106.00  -8.00   0.50    0.71    --  -78.15 108.00 116.00  196
 11  \w    -82.00 -25.00   0.50    0.71    --  -78.15  57.00 120.00  114
 12  \w    -55.00 -12.00   0.50    0.71    --  -78.15  38.00 120.00   86
 13  \w    -36.00 -10.00   0.50    0.71    --  -78.15  38.00 -90.00   52
 14  \w    -70.00 -42.00   0.50    0.71    --  -78.15  38.00 -90.00   56
 15  \w    -71.00 -30.00   0.50    0.71    --  -78.15  38.00-120.00   82
 16  \w   -144.00 -91.00   0.50    0.71    --  -78.15 -99.00  90.00  106
 17  \w   -150.00 -88.00   0.50    0.71    --  -78.15 -99.00  60.00  124
 18  \w   -143.00-118.00   0.50    0.71    --  -78.15-108.00  19.00   50
 19  \w   -147.00 -89.00   0.50    0.71    --  -78.15-125.00 -90.00  116
;
_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      -0.0199007000
_diffrn_orient_matrix_UB_12      0.0504954000
_diffrn_orient_matrix_UB_13      0.0699777000
_diffrn_orient_matrix_UB_21      -0.0113979000
_diffrn_orient_matrix_UB_22      0.1308759000
_diffrn_orient_matrix_UB_23      -0.0384220000
_diffrn_orient_matrix_UB_31      -0.0802244000
_diffrn_orient_matrix_UB_32      -0.0311140000
_diffrn_orient_matrix_UB_33      -0.0480888000
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16036
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         55.832
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    14.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25029
_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    1.882
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0391P)^2^+5.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3952
_reflns_number_total             4553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           gm-36-4_auto
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248529
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Eu C H O N '
_shelx_estimated_absorpt_t_max   0.159
_shelx_estimated_absorpt_t_min   0.159
_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
 H12A-H11B_$1
 2.1 with sigma of 0.02
3.a Free rotating group:
 O12(H12A,H12B)
3.b Rotating group:
 O10(H10A,H10B), O11(H11A,H11B)
3.c Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C24(H24)
3.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C21(H21), C12(H12), C10(H10), C9(H9A), C19(H19), C5(H5A), C18(H18),
 C6(H6A), C3(H3), C2(H2), C22(H22)
3.e Idealised tetrahedral OH refined as rotating group:
 O9(H9), O6(H6), O5(H5)
;
_shelx_res_checksum              75254
_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 3.527
_oxdiff_exptl_absorpt_empirical_full_min 0.480