A fluorobenzene-bound dysprosium half-sandwich dication single-molecule magnet.
Corner, Sophie C.; Blackmore, William J. A.; Gransbury, Gemma K.; Mattioni, Andrea; Whitehead, George F. S.; Chilton, Nicholas F.; Mills, David P.; Chemical science 16 (2025) 610–620; doi:10.1039/d4sc06661h

data_1573412
_publ_section_title
;
 A fluorobenzene-bound dysprosium half-sandwich dication single-molecule
 magnet.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              610
_journal_page_last               620
_journal_paper_doi               10.1039/d4sc06661h
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C40 H92 B8 Y4'
_chemical_formula_sum            'C40 H92 B8 Y4'
_chemical_formula_weight         1015.25
_chemical_name_systematic        '[Y(Cp*)(BH4)2]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-26 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9654(2)
_cell_length_b                   21.7125(2)
_cell_length_c                   14.55590(10)
_cell_measurement_reflns_used    9618
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      75.7590
_cell_measurement_theta_min      4.4300
_cell_volume                     5361.39(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      99.97(12)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_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     95.00 132.00   1.00    1.00    --   44.80  60.00 -60.00   37
  2  \w    -44.00  79.00   1.00    1.00    --   44.80  60.00 -90.00  123
  3  \w     15.00 128.00   1.00    1.00    --   44.80  40.00 150.00  113
  4  \w    -45.00 -19.00   1.00    1.00    --   44.80  40.00 150.00   26
  5  \w    -28.00  -3.00   1.00    1.00    --   44.80  60.00 -60.00   25
  6  \w     20.00 197.00   1.00    2.00    --  108.20  20.00 150.00  177
  7  \w    155.00 198.00   1.00    2.00    --  108.20  50.00   0.00   43
  8  \w     64.00  91.00   1.00    2.00    --  108.20  50.00 -90.00   27
  9  \w    105.00 132.00   1.00    2.00    --  108.20  50.00   0.00   27
 10  \w     40.00 197.00   1.00    2.00    --  108.20  50.00 -30.00  157
 11  \w     78.00 124.00   1.00    2.00    --  108.20  50.00  30.00   46
 12  \w    116.00 195.00   1.00    2.00    --  108.20  50.00 -60.00   79
 13  \w     93.00 198.00   1.00    2.00    --  108.20  30.00   0.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0385609000
_diffrn_orient_matrix_UB_12      0.0050236000
_diffrn_orient_matrix_UB_13      -0.0949807000
_diffrn_orient_matrix_UB_21      0.0793468000
_diffrn_orient_matrix_UB_22      0.0161839000
_diffrn_orient_matrix_UB_23      0.0465233000
_diffrn_orient_matrix_UB_31      0.0213834000
_diffrn_orient_matrix_UB_32      -0.0689354000
_diffrn_orient_matrix_UB_33      0.0040042000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33940
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.174
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.759
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.258
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method 'Recrystallised from benzene at r.t.'
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     1624
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0393P)^2^+2.6355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8342
_reflns_number_total             10851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06661h2.cif
_cod_data_source_block           ldpm174
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1573408--1573414.cif.
;
_cod_database_code               1573412
_manchester_internal_diff_code   ldpm174
_manchester_internal_coll_client IV-Y
_manchester_internal_coll_date   27/11/20
_manchester_internal_process_date 04/01/21
_manchester_internal_process_user SCC
_manchester_internal_solution_date 04/01/21
_manchester_internal_solution_user SCC
_manchester_internal_refinement_date 04/01/21
_manchester_internal_refinement_user SCC
_manchester_internal_validation_date 06/06/24
_manchester_internal_validation_user SCC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Y C H B'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All B(H,H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 B1-H1B \\sim B1-H1C \\sim B1-H1A \\sim B1-H1D \\sim B2-H2A \\sim B2-H2B \\sim
B2-H2D \\sim B2-H2C \\sim B3-
 H3C \\sim B3-H3B \\sim B3-H3A \\sim B3-H3D \\sim B4-H4A \\sim B4-H4D \\sim
B4-H4C \\sim B4-H4B \\sim B5-H5C ~
 B5-H5B \\sim B5-H5A \\sim B5-H5D \\sim B6-H6E \\sim B6-H6D \\sim B6-H6F \\sim
B6-H6G \\sim B7-H7E \\sim B7-H7D
 \\sim B7-H7G \\sim B7-H7F \\sim B8-H8F \\sim B8-H8D \\sim B8-H8E \\sim B8-H8G
 with sigma of 0.02
 H1D-H1B \\sim H1D-H1C \\sim H1C-H1B \\sim H1C-H1A \\sim H1B-H1A \\sim H1D-H1A
\\sim H2D-H2A \\sim H2D-H2B
 \\sim H2D-H2C \\sim H2C-H2A \\sim H2C-H2B \\sim H2B-H2A \\sim H3D-H3A \\sim
H3D-H3B \\sim H3D-H3C \\sim H3B-
 H3A \\sim H3C-H3B \\sim H3C-H3A \\sim H4C-H4B \\sim H4D-H4B \\sim H4D-H4C
\\sim H4D-H4A \\sim H4B-H4A ~
 H4C-H4A \\sim H5D-H5C \\sim H5D-H5A \\sim H5D-H5B \\sim H5B-H5A \\sim H5C-H5B
\\sim H5C-H5A \\sim H6G-H6E
 \\sim H6G-H6D \\sim H6G-H6F \\sim H6F-H6D \\sim H6F-H6E \\sim H6E-H6D \\sim
H8G-H8D \\sim H8E-H8D \\sim H8F-
 H8D \\sim H8F-H8E \\sim H8G-H8E \\sim H8G-H8F \\sim H7F-H7E \\sim H7G-H7E
\\sim H7G-H7F \\sim H7G-H7D ~
 H7F-H7D \\sim H7E-H7D
 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              7986
_shelx_hkl_checksum              31050
_olex2_date_sample_submission    2020-11-27
_olex2_exptl_crystal_mounting_method 'Mounted in fomblin'
_olex2_submission_original_sample_id ldpm174
_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 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.807