Leveraging anion selection to modulate crystallographic symmetry in Yb(III) single-molecule magnets.
Lowe, Ethan; Hourston, Hamish; Sharma, Tanu; Dugmore, Sarah K.; Wilson, Claire; Rajaraman, Gopalan; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14070–14078; doi:10.1039/d5dt01565k

data_7719554
_publ_section_title
;
 Leveraging anion selection to modulate crystallographic symmetry in
 Yb(III) single-molecule magnets.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14070
_journal_page_last               14078
_journal_paper_doi               10.1039/d5dt01565k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C72 H60 As4 Cl2 O4 Yb, C24 H20 B'
_chemical_formula_sum            'C96 H80 As4 B Cl2 O4 Yb'
_chemical_formula_weight         1852.03
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-07-03 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0581(2)
_cell_length_b                   15.0581(2)
_cell_length_c                   35.8664(9)
_cell_measurement_reflns_used    10477
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      32.9660
_cell_measurement_theta_min      2.7030
_cell_volume                     8132.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.135a 64-bit (release 19-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.930
_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     16.00  43.00   0.50    5.00    --   -0.17  57.00 120.00   54
  2  \w      8.00  40.00   0.50    5.00    --   -0.17  77.00   0.00   64
  3  \w      1.00  34.00   0.50    5.00    --   -0.17  57.00-120.00   66
  4  \w     24.00  52.00   0.50    5.00    --   -0.17  37.00-120.00   56
  5  \w    -42.00   6.00   0.50    5.00    --   -0.17 -77.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061837000
_diffrn_orient_matrix_UB_12      0.0001922000
_diffrn_orient_matrix_UB_13      0.0196020000
_diffrn_orient_matrix_UB_21      -0.0141864000
_diffrn_orient_matrix_UB_22      0.0448932000
_diffrn_orient_matrix_UB_23      0.0007270000
_diffrn_orient_matrix_UB_31      -0.0444881000
_diffrn_orient_matrix_UB_32      -0.0142747000
_diffrn_orient_matrix_UB_33      0.0025083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            36459
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.954
_diffrn_reflns_theta_min         2.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.135a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             3716
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.094
_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     244
_refine_ls_number_reflns         7698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0125P)^2^+14.7932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5752
_reflns_number_total             7698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01565k2.cif
_cod_data_source_block           el-2_auto
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7719554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Yb As C H  O Cl B'
_chemical_oxdiff_usercomment     'EL_2 150K'
_diffrn_oxdiff_digest_frames
;
015bc9d9c5e5c13d5aa0dfc4d5fe61f97000336a859
;
_diffrn_oxdiff_digest_hkl
;
4354d3bfcaf333074502cd2a1b15688f3fea8e
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              33637
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.070
_oxdiff_exptl_absorpt_empirical_full_min 0.897