Direct characterisation of <i>m</i><sub><i>J</i></sub> = ±15/2 ground state in octahedral Dy(III) single-molecule magnets.
Parmar, Vijay S.; Gransbury, Gemma K.; Corner, Sophie C.; Chou, Wei-Hao; Hill, Stephen; Winpenny, Richard E. P.; Chilton, Nicholas F.; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7616–7620; doi:10.1039/d5dt00862j

data_7718536
_publ_section_title
;
 Direct characterisation of <i>m</i><sub><i>J</i></sub> = &#xb1;15/2
 ground state in octahedral Dy(III) single-molecule magnets.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7616
_journal_page_last               7620
_journal_paper_doi               10.1039/d5dt00862j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C84 H90 Cl Dy0.05 O5 Y0.95'
_chemical_formula_sum            'C84 H90 Cl Dy0.05 O5 Y0.95'
_chemical_formula_weight         1307.59
_chemical_name_systematic        '[5%Dy@Y(PH*O)2(THF)3Cl]'
_chemical_properties_physical    Air-sensitive,Moisture-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   geom
_audit_creation_date             2024-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2025-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                118.073(2)
_cell_angle_beta                 96.087(2)
_cell_angle_gamma                93.434(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6646(3)
_cell_length_b                   18.2180(5)
_cell_length_c                   18.4204(4)
_cell_measurement_reflns_used    25720
_cell_measurement_temperature    100.02(13)
_cell_measurement_theta_max      75.5810
_cell_measurement_theta_min      2.7280
_cell_volume                     3991.66(18)
_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      100.02(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.957
_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    -29.00  -3.00   1.00    1.00    --    5.00 -57.00 120.00   26
  2  \w    -82.00   3.00   1.00    1.00    --  -43.98  76.00 -30.00   85
  3  \w    -76.00  37.00   1.00    1.00    --  -43.98  57.00-180.00  113
  4  \w      9.00  44.00   1.00    1.00    --  -43.98  76.00 -30.00   35
  5  \w    -76.00   6.00   1.00    1.00    --  -46.22  57.00 -90.00   82
  6  \w    -85.00  13.00   1.00    1.00    --  -46.22  38.00-180.00   98
  7  \w    -85.00  12.00   1.00    1.00    --  -46.22  76.00  60.00   97
  8  \w    -99.00 -18.00   1.00    2.00    -- -107.20 -19.00-120.00   81
  9  \w   -197.00-132.00   1.00    2.00    -- -107.20 -76.00  30.00   65
 10  \w   -126.00 -99.00   1.00    2.00    -- -107.20  76.00 120.00   27
 11  \w    -68.00 -36.00   1.00    2.00    -- -107.20  76.00 -90.00   32
 12  \w   -136.00 -31.00   1.00    2.00    -- -107.20  76.00  60.00  105
 13  \w   -118.00 -82.00   1.00    2.00    -- -107.20  76.00 -30.00   36
 14  \w   -128.00 -88.00   1.00    2.00    -- -107.20  76.00-120.00   40
 15  \w    -56.00 -18.00   1.00    2.00    -- -107.20  76.00 150.00   38
 16  \w   -122.00 -63.00   1.00    2.00    -- -107.20  76.00 150.00   59
 17  \w   -117.00 -18.00   1.00    2.00    -- -107.20   0.00-180.00   99
 18  \w   -148.00 -18.00   1.00    2.00    -- -107.20  76.00  30.00  130
 19  \w   -166.00-127.00   1.00    2.00    -- -107.20   0.00-180.00   39
 20  \w    -74.00 -20.00   1.00    2.00    -- -107.20  76.00-120.00   54
 21  \w   -147.00 -18.00   1.00    2.00    -- -107.20  76.00-150.00  129
 22  \w   -124.00 -88.00   1.00    2.00    -- -107.20  76.00 -90.00   36
 23  \w    -68.00 -43.00   1.00    2.00    -- -107.20  76.00 120.00   25
 24  \w   -117.00 -89.00   1.00    2.00    -- -107.20  76.00  90.00   28
 25  \w   -182.00 -18.00   1.00    2.00    -- -107.20  19.00 150.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0592206000
_diffrn_orient_matrix_UB_12      -0.0641861000
_diffrn_orient_matrix_UB_13      -0.0851435000
_diffrn_orient_matrix_UB_21      -0.0647372000
_diffrn_orient_matrix_UB_22      -0.0344066000
_diffrn_orient_matrix_UB_23      0.0434811000
_diffrn_orient_matrix_UB_31      -0.0732232000
_diffrn_orient_matrix_UB_32      0.0634631000
_diffrn_orient_matrix_UB_33      0.0076085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45707
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.828
_diffrn_reflns_theta_min         2.751
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_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    1.088
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1383
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         15922
_refine_ls_number_restraints     909
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0402P)^2^+1.9442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14793
_reflns_number_total             15922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00862j2.cif
_cod_data_source_block           rdpm266
_cod_depositor_comments
'Adding full bibliography for 7718533--7718536.cif.'
_cod_database_code               7718536
_manchester_internal_diff_code   rdpm266
_manchester_internal_coll_user   VP
_manchester_internal_coll_date   03/02/21
_manchester_internal_process_date 26/06/24
_manchester_internal_process_user SCC
_manchester_internal_solution_date 26/06/24
_manchester_internal_solution_user SCC
_manchester_internal_refinement_date 26/06/24
_manchester_internal_refinement_user SCC
_manchester_internal_validation_date 26/06/24
_manchester_internal_validation_user SCC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C84H90ClDy0.05O5Y0.95
_chemical_oxdiff_usercomment     119_VP
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Shared sites
{Y1, Dy1}
3. Restrained distances
 C59A-C58A \\sim C59-C57 \\sim C59A-C57A \\sim C58-C57 \\sim C58A-C57A \\sim
C59-C58
 with sigma of 0.02
 C57A-C56 \\sim C57-C56 \\sim C59A-C56 \\sim C59-C56 \\sim C58-C56 \\sim
C58A-C56
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C56 \\sim C57 \\sim C57A \\sim C58 \\sim C58A \\sim C59 \\sim C59A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Y1) = Uanis(Dy1)
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
 Sof(C57A)=Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(C58A)=Sof(H58D)=Sof(H58E)=
 Sof(H58F)=Sof(C59A)=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(1)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Fixed Sof: Dy1(0.05) Y1(0.95)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C24(H24), C43(H43), C60(H60)
7.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39),
 C41(H41), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
7.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C57(H57A,H57B,
 H57C), C57A(H57D,H57E,H57F), C58(H58A,H58B,H58C), C58A(H58D,H58E,H58F),
 C59(H59A,H59B,H59C), C59A(H59D,H59E,H59F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63722
_shelx_hkl_checksum              88379
_shelx_fab_checksum              11994
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.824