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_7135341
_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         'C18 H35 Ho N O8, 3(B F4)'
_chemical_formula_sum            'C18 H35 B3 F12 Ho N O8'
_chemical_formula_weight         818.83
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2026-01-19 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            4
_cell_length_a                   10.3911(3)
_cell_length_b                   10.7144(3)
_cell_length_c                   26.1234(7)
_cell_measurement_reflns_used    11454
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      34.4770
_cell_measurement_theta_min      2.1040
_cell_volume                     2908.43(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.124a 64-bit (release 23-05-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_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      180.00(10)
_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    -80.00 -16.00   0.50    1.00    --  -16.23 -69.00 -50.00  128
  2  \w    -24.00   2.00   0.50    1.00    --  -16.23 -87.00  70.00   52
  3  \w    -56.00  -3.00   0.50    1.00    --  -16.23 -67.00 176.00  106
  4  \w    -86.00 -57.00   0.50    1.00    --  -16.23-178.00 -60.00   58
;
_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      -0.0236473000
_diffrn_orient_matrix_UB_12      -0.0372553000
_diffrn_orient_matrix_UB_13      0.0203690000
_diffrn_orient_matrix_UB_21      -0.0465065000
_diffrn_orient_matrix_UB_22      0.0463279000
_diffrn_orient_matrix_UB_23      0.0057346000
_diffrn_orient_matrix_UB_31      -0.0441082000
_diffrn_orient_matrix_UB_32      -0.0290412000
_diffrn_orient_matrix_UB_33      -0.0169976000
_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  0.0181
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13042
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.054
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024)
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    1.870
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 2189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5821
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+8.2185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_full    0.957
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                5401
_reflns_number_total             5821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00045b2.cif
_cod_data_source_block           yj-1337_auto
_cod_depositor_comments
'Adding full bibliography for 7135339--7135341.cif.'
_cod_database_code               7135341
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ho1C1N1O1I1F1B1Ag1
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.601
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F11-B3 = F10-B3 = F9-B3 = F12-B3
 1.381 with sigma of 0.002
 B3-F12 \\sim B3-F12A
 with sigma of 0.02
 C18-C17 \\sim C18A-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10) = Uanis(F11)
4. Others
 Sof(F12A)=1-FVAR(1)
 Sof(F12)=FVAR(1)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C13(H13A,H13B), C1(H1A,H1B), C16(H16A,H16B), C10(H10A,H10B),
 C7(H7A,H7B), C6(H6A,H6B), C9(H9A,H9B), C3(H3A,H3B), C4(H4A,H4B), C8(H8A,H8B),
 C2(H2A,H2B), C14(H14A,H14B), C15(H15A,H15B), C12(H12A,H12B), C11(H11A,H11B)
5.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F)
;
_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 15.994
_oxdiff_exptl_absorpt_empirical_full_min 0.580