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_7127569
_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         'C68 H104 B2 N4 O6 Y, C24 H20 B'
_chemical_formula_sum            'C92 H124 B3 N4 O6 Y'
_chemical_formula_weight         1503.28
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-19
_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                90
_cell_angle_beta                 93.672(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9871(5)
_cell_length_b                   27.1689(11)
_cell_length_c                   24.3048(11)
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.2180
_cell_measurement_theta_min      3.1060
_cell_volume                     8558.2(6)
_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 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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    -14.00  12.00   1.00   69.00    --  -18.77 -99.00-180.00   26
  2  \w    -65.00 -39.00   1.00   69.00    --  -18.77-178.00 -60.00   26
  3  \w    -13.00  24.00   1.00   69.00    --  -18.77 -99.00 120.00   37
  4  \w    -20.00  22.00   1.00   69.00    --  -18.77 -99.00 -30.00   42
  5  \w     35.00  77.00   1.00   69.00    --   20.02 178.00-150.00   42
  6  \w     34.00  96.00   1.00   69.00    --   20.02-178.00-180.00   62
  7  \w      9.00  44.00   1.00   69.00    --   20.02  57.00 -30.00   35
  8  \w     -6.00  84.00   1.00   69.00    --   20.02  38.00   0.00   90
  9  \w    -53.00  46.00   1.00   69.00    --   20.02 -38.00-180.00   99
;
_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      -0.0203533000
_diffrn_orient_matrix_UB_12      0.0213713000
_diffrn_orient_matrix_UB_13      -0.0134777000
_diffrn_orient_matrix_UB_21      -0.0033791000
_diffrn_orient_matrix_UB_22      -0.0128780000
_diffrn_orient_matrix_UB_23      -0.0254474000
_diffrn_orient_matrix_UB_31      -0.0506881000
_diffrn_orient_matrix_UB_32      -0.0077097000
_diffrn_orient_matrix_UB_33      0.0050572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74428
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.690
_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    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         18769
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0324P)^2^+2.6595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11827
_reflns_number_total             18769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07446b2.cif
_cod_data_source_block           2Y
_cod_depositor_comments
'Adding full bibliography for 7127568--7127571.cif.'
_cod_database_code               7127569
_manchester_internal_diff_code   astl459
_manchester_internal_stl_name    YLTH40
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   16/05/2019
_manchester_internal_process_date 17/05/2019
_manchester_internal_process_user LTH
_manchester_internal_solution_date 17/05/2019
_manchester_internal_solution_user LTH
_manchester_internal_refinement_date 19/08/2019
_manchester_internal_refinement_user LTH/AW
_manchester_internal_validation_date 19/08/2019
_manchester_internal_validation_user LTH/AW
_manchester_internal_archive_date 27/08/2019
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Y O6 B3 N4 C100 H100'
_chemical_oxdiff_usercomment     STL/LTH
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.831
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-C34 \\sim C33-C34A
 with sigma of 0.02
3. Others
 Sof(H24a)=Sof(C26A)=Sof(H26d)=Sof(H26e)=Sof(H26f)=1-FVAR(1)
 Sof(H24)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(H26c)=FVAR(1)
 Sof(H33a)=Sof(C34)=Sof(H34d)=Sof(H34e)=Sof(H34f)=1-FVAR(2)
 Sof(H33)=Sof(C34A)=Sof(H34a)=Sof(H34b)=Sof(H34c)=FVAR(2)
 Sof(H54c)=Sof(H54d)=Sof(C53A)=Sof(H53c)=Sof(H53d)=1-FVAR(3)
 Sof(H54a)=Sof(H54b)=Sof(C53)=Sof(H53a)=Sof(H53b)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C21(H21), C24(H24), C24(H24a), C33(H33), C33(H33a),
 C36(H36), C45(H45), C48(H48)
4.b Secondary CH2 refined with riding coordinates:
 C54(H54a,H54b), C54(H54c,H54d), C55(H55a,H55b), C56(H56a,H56b), C57(H57a,
 H57b), C58(H58a,H58b), C59(H59a,H59b), C60(H60a,H60b), C61(H61a,H61b),
 C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b), C65(H65a,H65b), C66(H66a,H66b),
  C67(H67a,H67b), C68(H68a,H68b), C53(H53a,H53b), C53A(H53c,H53d)
4.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), C41(H41), C42(H42), C43(H43), C51(H51), C52(H52),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C88(H88), C89(H89), C90(H90), C91(H91), C92(H92)
4.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), C35(H35a,H35b,
 H35c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C46(H46a,H46b,H46c), C47(H47a,
 H47b,H47c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C26(H26a,H26b,H26c),
 C34A(H34a,H34b,H34c), C26A(H26d,H26e,H26f), C34(H34d,H34e,H34f)
;
_shelx_res_checksum              17841
_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 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.754