Insights into <i>D</i><sub>4h</sub>@metal-symmetry single-molecule magnetism: the case of a dysprosium-bis(boryloxide) complex.
Thomas-Hargreaves, Lewis R; Hunger, David; Kern, Michal; Wooles, Ashley J.; van Slageren, Joris; Chilton, Nicholas F.; Liddle, Stephen T.; Chemical communications (Cambridge, England) 57 (2021) 733–736; doi:10.1039/d0cc07446b

data_7127568
_publ_section_title
;
 Insights into <i>D</i><sub>4h</sub>@metal-symmetry single-molecule
 magnetism: the case of a dysprosium-bis(boryloxide) complex.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              733
_journal_page_last               736
_journal_paper_doi               10.1039/d0cc07446b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H92 B3 N4 O4 Y, C6 H6'
_chemical_formula_sum            'C66 H98 B3 N4 O4 Y'
_chemical_formula_weight         1132.82
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-11 deposited with the CCDC.	2020-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                79.924(3)
_cell_angle_beta                 82.227(4)
_cell_angle_gamma                81.650(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7081(5)
_cell_length_b                   13.6510(5)
_cell_length_c                   19.4888(8)
_cell_measurement_reflns_used    10347
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.5270
_cell_measurement_theta_min      3.1990
_cell_volume                     3272.4(2)
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.883
_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    -20.00  25.00   1.00   38.84    --  -18.77 -99.00  90.00   45
  2  \w    -88.00   3.00   1.00   38.84    --  -18.77 -57.00 -60.00   91
  3  \w    -93.00  31.00   1.00   38.84    --  -18.77 -19.00   0.00  124
  4  \w    -20.00  25.00   1.00   38.84    --  -18.77 -99.00 -60.00   45
  5  \w    -97.00 -34.00   1.00   38.84    --  -18.77 178.00  30.00   63
  6  \w     35.00  98.00   1.00   38.84    --   20.02 178.00 150.00   63
  7  \w    -51.00  52.00   1.00   38.84    --   20.02 -77.00-150.00  103
  8  \w    -20.00  64.00   1.00   38.84    --   20.02 -99.00-172.00   84
  9  \w     -2.00  89.00   1.00   38.84    --   20.02  57.00 -90.00   91
 10  \w     -2.00  23.00   1.00   38.84    --   20.02  57.00-180.00   25
 11  \w    -49.00  42.00   1.00   38.84    --   20.02 -57.00 -30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0206587000
_diffrn_orient_matrix_UB_12      0.0414425000
_diffrn_orient_matrix_UB_13      0.0173507000
_diffrn_orient_matrix_UB_21      -0.0174361000
_diffrn_orient_matrix_UB_22      -0.0332782000
_diffrn_orient_matrix_UB_23      0.0302445000
_diffrn_orient_matrix_UB_31      0.0499260000
_diffrn_orient_matrix_UB_32      -0.0020107000
_diffrn_orient_matrix_UB_33      0.0129718000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.177
_diffrn_reflns_theta_min         2.668
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.352
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         15633
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0750P)^2^+1.8665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10281
_reflns_number_total             15633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07446b2.cif
_cod_data_source_block           1Y
_cod_depositor_comments
'Adding full bibliography for 7127568--7127571.cif.'
_cod_database_code               7127568
_manchester_internal_diff_code   ASTL440
_manchester_internal_stl_name    YLTH26
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   28/02/2019
_manchester_internal_process_date 01/03/2019
_manchester_internal_process_user LTH
_manchester_internal_solution_date 01/05/2019
_manchester_internal_solution_user LTH
_manchester_internal_refinement_date 13/03/2020
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 01/05/2019
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 13/03/2020
_manchester_internal_archive_user aw
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         YCHNO4B3
_chemical_oxdiff_usercomment     STL/LTH
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.756
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H,H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-C64 = C66-C65 = C66-C61 = C62-C61 = C63-C62 = C64-C63
 1.39 with sigma of 0.01
 B3-H3C = B3-H3B = B3-H3D = B3-H3A
 1.05 with sigma of 0.01
 C62-C66 \\sim C64-C66 \\sim C61-C65 \\sim C61-C63 \\sim C64-C62 \\sim C63-C65
 with sigma of 0.02
 H3D-H3C \\sim H3D-H3B \\sim H3D-H3A \\sim H3C-H3B \\sim H3C-H3A \\sim H3B-H3A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C62 \\sim C61 \\sim C66 \\sim C63 \\sim C65 \\sim C64: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C63, C61, C62, C66, C65, C64
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C21(H21), C24(H24), C33(H33), C36(H36), C47(H47), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C29(H29), C30(H30), C31(H31), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              9177
_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 1.975
_oxdiff_exptl_absorpt_empirical_full_min 0.715