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_7127571
_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 Dy N4 O4, C6 H6'
_chemical_formula_sum            'C66 H98 B3 Dy N4 O4'
_chemical_formula_weight         1206.41
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-16
_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                107.413(6)
_cell_angle_beta                 92.621(5)
_cell_angle_gamma                98.825(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7769(7)
_cell_length_b                   13.6689(7)
_cell_length_c                   19.8264(15)
_cell_measurement_reflns_used    8170
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3800
_cell_measurement_theta_min      2.9890
_cell_volume                     3249.4(4)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.998
_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    -33.00  50.00   1.00   15.00    --  -18.77  57.00 -30.00   83
  2  \w    -20.00  24.00   1.00   15.00    --  -18.77 -99.00 -30.00   44
  3  \w    -88.00 -22.00   1.00   15.00    --  -18.77 -57.00-180.00   66
  4  \w    -20.00   7.00   1.00   15.00    --  -18.77 -99.00-150.00   27
  5  \w     36.00  67.00   1.00   15.00    --   20.02 178.00 120.00   31
  6  \w     39.00  94.00   1.00   15.00    --   20.02 178.00-120.00   55
  7  \w    -52.00  45.00   1.00   15.00    --   20.02 -38.00-150.00   97
  8  \w     40.00  65.00   1.00   15.00    --   20.02 178.00  30.00   25
  9  \w    -24.00  49.00   1.00   15.00    --   20.02 -77.00  90.00   73
;
_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      -0.0558365000
_diffrn_orient_matrix_UB_12      -0.0038842000
_diffrn_orient_matrix_UB_13      0.0012246000
_diffrn_orient_matrix_UB_21      0.0076644000
_diffrn_orient_matrix_UB_22      0.0225338000
_diffrn_orient_matrix_UB_23      0.0374551000
_diffrn_orient_matrix_UB_31      0.0031226000
_diffrn_orient_matrix_UB_32      0.0502844000
_diffrn_orient_matrix_UB_33      -0.0038495000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1498
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11803
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.322
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.565
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.175
_refine_diff_density_max         4.601
_refine_diff_density_min         -4.057
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         11803
_refine_ls_number_restraints     1088
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+94.6784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3221
_refine_ls_wR_factor_ref         0.3354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9412
_reflns_number_total             11803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07446b2.cif
_cod_data_source_block           1Dy
_cod_depositor_comments
'Adding full bibliography for 7127568--7127571.cif.'
_cod_database_code               7127571
_manchester_internal_diff_code   ASTL483
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   15/08/2019
_manchester_internal_process_date 10/03/2020
_manchester_internal_process_user AW
_manchester_internal_solution_date 10/03/2020
_manchester_internal_solution_user AW
_manchester_internal_refinement_date 16/03/2020
_manchester_internal_refinement_user AW
_manchester_internal_validation_date 16/03/2020
_manchester_internal_validation_user AW
_manchester_internal_archive_date 16/03/2020
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy C70 H90 B3 O4 N4'
_chemical_oxdiff_usercomment     LTH/STL
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.686
_reflns_odcompleteness_completeness 88.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.773(4)
 0.227(4)
2. 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
3. Restrained distances
 B3-H3D = B3-H3B = B3-H3C = B3-H3A
 1.05 with sigma of 0.01
 H3B-H3C \\sim H3C-H3A \\sim H3B-H3A \\sim H3D-H3A \\sim H3B-H3D \\sim H3C-H3D
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C4 \\sim C10 \\sim C9 \\sim C3 \\sim C5: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24), C35(H35), C38(H38), C47(H47), C50(H50)
6.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)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19),
 C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C43(H43), C44(H44), C45(H45),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              44018
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   4414
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.944
_oxdiff_exptl_absorpt_empirical_full_min 0.614