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_7127570
_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 Dy N4 O6, C24 H20 B, C6 H6'
_chemical_formula_sum            'C98 H130 B3 Dy N4 O6'
_chemical_formula_weight         1654.98
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-24
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5114(3)
_cell_length_b                   19.5012(3)
_cell_length_c                   19.8810(3)
_cell_measurement_reflns_used    30984
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.3570
_cell_measurement_theta_min      2.0380
_cell_volume                     9115.4(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -78.00  96.00   1.00   15.00    --    7.50  57.00 -58.00  174
  2  \w    -49.00   1.00   1.00   15.00    --    7.50  60.00   0.00   50
  3  \w     26.00  53.00   1.00   15.00    --    7.50  60.00   0.00   27
  4  \w    -78.00 -51.00   1.00   15.00    --    7.50  30.00-180.00   27
  5  \w    -80.00  96.00   1.00   15.00    --    7.50  30.00-120.00  176
;
_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      -0.0217227000
_diffrn_orient_matrix_UB_12      0.0251064000
_diffrn_orient_matrix_UB_13      -0.0027543000
_diffrn_orient_matrix_UB_21      -0.0131808000
_diffrn_orient_matrix_UB_22      -0.0195185000
_diffrn_orient_matrix_UB_23      -0.0257881000
_diffrn_orient_matrix_UB_31      -0.0162434000
_diffrn_orient_matrix_UB_32      -0.0176853000
_diffrn_orient_matrix_UB_33      0.0244963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54368
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.700
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.553
_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    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.185
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     536
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0214P)^2^+105.1352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3872
_reflns_number_total             4264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07446b2.cif
_cod_data_source_block           2Dy
_cod_depositor_comments
'Adding full bibliography for 7127568--7127571.cif.'
_cod_original_cell_volume        9115.5(2)
_cod_database_code               7127570
_manchester_internal_diff_code   astl478
_manchester_internal_stl_name    DYLTH9
_manchester_internal_coll_client LTH
_manchester_internal_coll_date   19/07/2019
_manchester_internal_process_date 22/07/2019
_manchester_internal_process_user AW/LTH
_manchester_internal_solution_date 22/07/2019
_manchester_internal_solution_user LTH/AW
_manchester_internal_refinement_date 24/07/2019
_manchester_internal_refinement_user AW/LTH
_manchester_internal_validation_date 24/07/2019
_manchester_internal_validation_user AW/LTH
_manchester_internal_archive_date 24/07/2019
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Dy B3 O6 N4 C60 H80'
_chemical_oxdiff_usercomment     LTH
_reflns_odcompleteness_completeness 99.92
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-C29 = C29-C28 = C25-C24 = C26-C25 = C27-C26 = C1F-C1E = C1E-C1D = C1D-C1C
 = C1C-C1B = C1B-C1A = C1F-C1A = C29-C28 = C30-C29 = C31-C30 = C31-C30_$1 =
 C30_$1-C29_$1 = C29_$1-C28
 1.39 with sigma of 0.01
 C23-C22 = C23-C22A = C23A-C22A = C17-C16 = C16-C15 = C15-C14 = C19-C20 = C20-
 C21 = C18-C19
 1.55 with sigma of 0.01
 O2-C14 = O2-C17 = O4-C23A = O4-C22
 1.45 with sigma of 0.01
 C20-O3 \\sim O3-C19
 with sigma of 0.02
 C1A-C1D \\sim C1C-C1F \\sim C1E-C1B
 with sigma of 0.02
 C1F-C1D \\sim C1E-C1C \\sim C1E-C1A \\sim C1F-C1B \\sim C1C-C1A \\sim C1D-C1B
 with sigma of 0.01
 C14-C16 \\sim C15-C17
 with sigma of 0.02
 C29_$1-C30 \\sim C29-C30_$1 \\sim C28-C31
 with sigma of 0.01
3. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma of 0.1
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
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. Others
 Fixed Sof: O4(0.25) C23(0.25) H23A(0.25) H23B(0.25) O2(0.25) O3(0.5)
 C14(0.25) H14A(0.25) H14B(0.25) C15(0.25) H15A(0.25) H15B(0.25) C16(0.25)
 H16A(0.25) H16B(0.25) C17(0.25) H17A(0.25) H17B(0.25) C18(0.5) H18A(0.5)
 H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) C22(0.25) H22A(0.25) H22B(0.25) C1A(0.25) H1A(0.25)
 C1B(0.25) H1B(0.25) C1C(0.25) H1C(0.25) C1D(0.25) H1D(0.25) C1E(0.25)
 H1E(0.25) C1F(0.25) H1F(0.25) C23A(0.25) H23C(0.25) H23D(0.25) C22A(0.25)
 H22C(0.25) H22D(0.25)
7.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11)
7.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23A(H23C,H23D), C22A(H22C,H22D)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C25(H25), C26(H26), C27(H27), C29(H29),
 C30(H30), C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F), C31(H31)
7.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              28911
_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 1.154
_oxdiff_exptl_absorpt_empirical_full_min 0.820