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_7248530
_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 Ho O11, H2 O'
_chemical_formula_sum            'C24 H24 Ho O12'
_chemical_formula_weight         669.36
_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             2023-05-17
_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                 112.636(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2512(4)
_cell_length_b                   9.2096(2)
_cell_length_c                   15.3351(4)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      60.1070
_cell_measurement_theta_min      2.4050
_cell_volume                     2248.71(10)
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_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    107.00 133.00   0.50    0.14    --   76.35 112.00 -62.00   52
  2  \w      1.00  71.00   0.50    0.14    --   76.35 -38.00-120.00  140
  3  \w      9.00  63.00   0.50    0.14    --   76.35 -38.00-180.00  108
  4  \w     35.00  60.00   0.50    0.14    --   76.35-112.00-155.00   50
  5  \w     77.00 103.00   0.50    0.14    --   76.35-125.00 -60.00   52
  6  \w    -71.00   0.00   0.50    0.05    --   -0.94 -57.00-180.00  142
  7  \w      4.00  38.00   0.50    0.05    --   -0.94 -99.00 -60.00   68
  8  \w     -8.00  25.00   0.50    0.05    --   -0.94 -99.00 150.00   66
  9  \w     -2.00  32.00   0.50    0.05    --   -0.94 -99.00  30.00   68
 10  \w   -135.00 -88.00   0.50    0.14    --  -78.22-112.00-155.00   94
 11  \w    -92.00 -40.00   0.50    0.14    --  -78.22  57.00 -60.00  104
 12  \w    -68.00  -1.00   0.50    0.14    --  -78.22  38.00-120.00  134
 13  \w    -63.00  -2.00   0.50    0.14    --  -78.22  38.00 -30.00  122
 14  \w    -69.00  -2.00   0.50    0.14    --  -78.22  38.00  90.00  134
 15  \w    -71.00  -1.00   0.50    0.14    --  -78.22  38.00 150.00  140
 16  \w    -50.00 -22.00   0.50    0.14    --  -78.22 125.00 120.00   56
 17  \w    -91.00 -64.00   0.50    0.14    --  -78.22 125.00 120.00   54
 18  \w   -104.00 -41.00   0.50    0.14    --  -78.22 112.00 -62.00  126
;
_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      0.0682186000
_diffrn_orient_matrix_UB_12      0.0471455000
_diffrn_orient_matrix_UB_13      0.0721027000
_diffrn_orient_matrix_UB_21      -0.0138776000
_diffrn_orient_matrix_UB_22      0.1346223000
_diffrn_orient_matrix_UB_23      -0.0357418000
_diffrn_orient_matrix_UB_31      -0.0472271000
_diffrn_orient_matrix_UB_32      0.0284307000
_diffrn_orient_matrix_UB_33      0.0497257000
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.929
_diffrn_reflns_theta_max         52.929
_diffrn_reflns_theta_min         2.413
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    16.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55626
_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    1.977
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.184
_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     342
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0846P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3391
_reflns_number_total             3961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00292j2.cif
_cod_data_source_block           ho_auto
_cod_depositor_comments
'Adding full bibliography for 7248523--7248531.cif.'
_cod_database_code               7248530
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Ho C H O N'
_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
 H008_$1-H00C_$2
 2.1 with sigma of 0.02
 H00H-H00D_$3
 2.1 with sigma of 0.02
 H00H-H00E_$3
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C00T) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C00F) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C00S) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
4.a Free rotating group:
 O00C(H00G,H00H)
4.b Rotating group:
 O005(H00A,H00B), O00D(H00D,H00E)
4.c Ternary CH refined with riding coordinates:
 C00O(H00O), C00R(H00R), C010(H010)
4.d Aromatic/amide H refined with riding coordinates:
 C00E(H00F), C00I(H00I), C00J(H00J), C00K(H00K), C00M(H00M), C00P(H00P),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C011(H011)
4.e Idealised tetrahedral OH refined as rotating group:
 O006(H006), O008(H008), O00B(H00C)
;
_shelx_res_checksum              32119
_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 5.262
_oxdiff_exptl_absorpt_empirical_full_min 0.401