Synthesis of crown ether-capped highly symmetrical fluoride-centered lanthanide clusters [Ln<sub>6</sub>F<sub>13</sub>(12-crown-4)<sub>6</sub>]I<sub>3</sub>F<sub>2</sub> (Ln = Ho, Er).
Li, Yangjuan; He, Miao; Gong, Yu; Chemical communications (Cambridge, England) 62 (2026) 5433–5437; doi:10.1039/d6cc00045b

data_7135340
_publ_section_title
;
 Synthesis of crown ether-capped highly symmetrical fluoride-centered
 lanthanide clusters
 [Ln<sub>6</sub>F<sub>13</sub>(12-crown-4)<sub>6</sub>]I<sub>3</sub>F<sub>2</sub>
 (Ln = Ho, Er).
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5433
_journal_page_last               5437
_journal_paper_doi               10.1039/d6cc00045b
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C48 H96 Er6 F13 O24, 3(I), 2(F)'
_chemical_formula_sum            'C48 H96 Er6 F15 I3 O24'
_chemical_formula_weight         2726.50
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-10-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-10-11 deposited with the CCDC.	2026-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2915(4)
_cell_length_b                   18.2915(4)
_cell_length_c                   18.2915(4)
_cell_measurement_reflns_used    2802
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      34.5370
_cell_measurement_theta_min      2.2170
_cell_volume                     6120.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -24.00  30.00   0.50    7.00    --   14.35 -86.00  59.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0336530000
_diffrn_orient_matrix_UB_12      -0.0106916000
_diffrn_orient_matrix_UB_13      0.0160179000
_diffrn_orient_matrix_UB_21      -0.0162772000
_diffrn_orient_matrix_UB_22      0.0013133000
_diffrn_orient_matrix_UB_23      0.0351759000
_diffrn_orient_matrix_UB_31      -0.0102424000
_diffrn_orient_matrix_UB_32      -0.0372531000
_diffrn_orient_matrix_UB_33      -0.0033065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4004
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.304
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.891
_refine_diff_density_min         -2.072
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         581
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      24.762
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1028P)^2^+158.6583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                540
_reflns_number_total             581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00045b2.cif
_cod_data_source_block           yj-1267pingdi-3_auto
_cod_depositor_comments
'Adding full bibliography for 7135339--7135341.cif.'
_cod_original_cell_volume        6120.0(4)
_cod_database_code               7135340
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Er1C1N1O1I1F1B1
_shelx_estimated_absorpt_t_max   0.528
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C1_$1-C1_$2
 1.49 with sigma of 0.002
 H1a-H1a_$3
 2.11 with sigma of 0.002
 H1b-H1b_$3
 2.11 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(F2) = Uanis(F3)
4. Others
 Fixed Sof: F3(0.041667)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.854