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_7718534
_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 O5 Y, 3(C4 H8 O)'
_chemical_formula_sum            'C96 H114 Cl O8 Y'
_chemical_formula_weight         1520.23
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-28
_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                104.0730(10)
_cell_angle_beta                 91.5630(10)
_cell_angle_gamma                94.2090(10)
_cell_formula_units_Z            2
_cell_length_a                   12.06710(10)
_cell_length_b                   15.4384(2)
_cell_length_c                   23.3235(2)
_cell_measurement_reflns_used    38255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.4720
_cell_measurement_theta_min      1.9320
_cell_volume                     4198.74(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.960
_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    -71.00 -12.00   0.50    0.50    --  -45.10 -63.00-125.17  118
  2  \w   -100.00 -73.00   0.50    0.50    --  -45.10 -68.00 -29.41   54
  3  \w   -134.00-104.00   0.50    0.50    --  -45.10 -68.00 -29.41   60
  4  \w   -134.00  44.00   0.50    0.50    --  -45.10  13.00  97.53  356
  5  \w    -83.00  27.00   0.50    0.50    --  -45.10  73.00  64.64  220
  6  \w    -64.00 -37.00   0.50    0.50    --  -45.10 -68.00 -29.41   54
  7  \w    -67.00  32.00   0.50    0.50    --  -45.10  54.00 169.58  198
  8  \w   -103.00 -76.00   0.50    0.50    -- -110.00  76.00  90.00   54
  9  \w   -133.00-106.00   0.50    0.50    -- -110.00  76.00  90.00   54
 10  \w    -61.00 -34.00   0.50    0.50    -- -110.00  76.00 150.00   54
 11  \w   -136.00 -22.00   0.50    0.50    -- -110.00  76.00 120.00  228
 12  \w   -129.00-103.00   0.50    0.50    -- -110.00  76.00-150.00   52
 13  \w   -140.00 -94.00   0.50    0.50    -- -110.00 -76.00  90.00   92
 14  \w   -149.00 -21.00   0.50    0.50    -- -110.00  76.00   0.00  256
 15  \w   -150.00 -27.00   0.50    0.50    -- -110.00  76.00 -60.00  246
 16  \w    -83.00 -44.00   0.50    0.50    -- -110.00  57.00 -60.00   78
 17  \w   -148.00 -74.00   0.50    0.50    -- -110.00  76.00 -90.00  148
 18  \w    -53.00 -27.00   0.50    0.50    -- -110.00  76.00  60.00   52
 19  \w   -137.00-112.00   0.50    0.50    -- -110.00 -76.00 120.00   50
 20  \w   -145.00 -38.00   0.50    0.50    -- -110.00  76.00-120.00  214
 21  \w   -137.00-110.00   0.50    0.50    -- -110.00  38.00-180.00   54
 22  \w    -82.00 -22.00   0.50    0.50    -- -110.00  38.00-180.00  120
 23  \w   -144.00 -59.00   0.50    0.50    -- -110.00  76.00  60.00  170
 24  \w   -199.00 -48.00   0.50    0.50    -- -110.00   0.00-120.00  302
 25  \w   -101.00 -30.00   0.50    0.50    -- -110.00  19.00  90.00  142
 26  \w   -194.00-164.00   0.50    0.50    -- -110.00 -76.00  90.00   60
 27  \w    -64.00 -38.00   0.50    0.50    -- -110.00  38.00  30.00   52
 28  \w   -119.00 -94.00   0.50    0.50    -- -110.00  57.00 150.00   50
 29  \w    -69.00 -44.00   0.50    0.50    -- -110.00  57.00 150.00   50
 30  \w   -106.00 -79.00   0.50    0.50    -- -110.00  76.00-180.00   54
 31  \w    -64.00 -30.00   0.50    0.50    -- -110.00  76.00-180.00   68
 32  \w   -194.00-132.00   0.50    0.50    -- -110.00  19.00  90.00  124
 33  \w   -131.00 -23.00   0.50    0.50    -- -110.00  57.00 120.00  216
 34  \w   -181.00-156.00   0.50    0.50    -- -110.00 -57.00  30.00   50
 35  \w   -144.00-101.00   0.50    0.50    -- -110.00 -57.00  30.00   86
 36  \w   -116.00 -90.00   0.50    0.50    -- -110.00  76.00  30.00   52
 37  \w   -194.00-169.00   0.50    0.50    -- -110.00 -76.00-150.00   50
 38  \w   -131.00-101.00   0.50    0.50    -- -110.00 -76.00-150.00   60
 39  \w   -105.00 -80.00   0.50    0.50    -- -110.00  76.00 150.00   50
 40  \w   -177.00-152.00   0.50    0.50    -- -110.00  19.00  60.00   50
 41  \w   -198.00 -33.00   0.50    0.50    -- -110.00 -19.00-180.00  330
;
_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      0.1032573000
_diffrn_orient_matrix_UB_12      0.0635662000
_diffrn_orient_matrix_UB_13      0.0260047000
_diffrn_orient_matrix_UB_21      -0.0429428000
_diffrn_orient_matrix_UB_22      0.0097473000
_diffrn_orient_matrix_UB_23      0.0626677000
_diffrn_orient_matrix_UB_31      0.0625828000
_diffrn_orient_matrix_UB_32      -0.0807476000
_diffrn_orient_matrix_UB_33      0.0066057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66418
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.316
_diffrn_reflns_theta_min         1.955
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         17120
_refine_ls_number_restraints     2132
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+1.8093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16071
_reflns_number_total             17120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00862j2.cif
_cod_data_source_block           rdpm94
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718533--7718536.cif.
;
_cod_database_code               7718534
_manchester_internal_diff_code   RDPM94
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   14/12/17
_manchester_internal_process_date 14/12/17
_manchester_internal_process_user FO
_manchester_internal_solution_date 15/12/17
_manchester_internal_solution_user VP
_manchester_internal_refinement_date 26/06/24
_manchester_internal_refinement_user VP/SCC
_manchester_internal_validation_date 26/06/24
_manchester_internal_validation_user SCC
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.724
_reflns_odcompleteness_completeness 98.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 C36A-C33 \\sim C36B-C33 \\sim C35A-C33 \\sim C35B-C33 \\sim C34A-C33 \\sim
C34B-C33
 with sigma of 0.02
 C78A-C77 \\sim C78B-C77 \\sim C79-C78A \\sim C79-C78B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. 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
5. Same fragment restrains
{O8A, C89A, C90A, C91A, C92A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O6A, C81A, C82A, C83A, C84A}
{O8A, C89A, C90A, C91A, C92A} sigma for 1-2: 0.01, 1-3: 0.04
as
{O6B, C81B, C82B, C83B, C84B}
{O7A, C85A, C86A, C87A, C88A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7B, C85B, C86B, C87B, C88B}
{O8A, C89A, C90A, C91A, C92A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O8B, C89B, C90B, C91B, C92B}
6. Others
 Sof(C34B)=Sof(H34d)=Sof(H34e)=Sof(H34f)=Sof(C35B)=Sof(H35d)=Sof(H35e)=
 Sof(H35f)=Sof(C36B)=Sof(H36d)=Sof(H36e)=Sof(H36f)=Sof(H77c)=Sof(H77d)=
 Sof(C78B)=Sof(H78c)=Sof(H78d)=Sof(H79c)=Sof(H79d)=Sof(O6B)=Sof(C81B)=Sof(H81e)=
 Sof(H81f)=Sof(C82B)=Sof(H82e)=Sof(H82f)=Sof(C83B)=Sof(H83e)=Sof(H83f)=
 Sof(C84B)=Sof(H84e)=Sof(H84f)=Sof(O7B)=Sof(C85B)=Sof(H85c)=Sof(H85d)=Sof(C86B)=
 Sof(H86c)=Sof(H86d)=Sof(C87B)=Sof(H87c)=Sof(H87d)=Sof(C88B)=Sof(H88c)=
 Sof(H88d)=Sof(O8B)=Sof(C89B)=Sof(H89c)=Sof(H89d)=Sof(C90B)=Sof(H90c)=Sof(H90d)=
 Sof(C91B)=Sof(H91c)=Sof(H91d)=Sof(C92B)=Sof(H92c)=Sof(H92d)=1-FVAR(1)
 Sof(C34A)=Sof(H34a)=Sof(H34b)=Sof(H34c)=Sof(C35A)=Sof(H35a)=Sof(H35b)=
 Sof(H35c)=Sof(C36A)=Sof(H36a)=Sof(H36b)=Sof(H36c)=Sof(H77a)=Sof(H77b)=
 Sof(C78A)=Sof(H78a)=Sof(H78b)=Sof(H79a)=Sof(H79b)=Sof(O6A)=Sof(C81A)=Sof(H81c)=
 Sof(H81d)=Sof(C82A)=Sof(H82c)=Sof(H82d)=Sof(C83A)=Sof(H83c)=Sof(H83d)=
 Sof(C84A)=Sof(H84c)=Sof(H84d)=Sof(O7A)=Sof(C85A)=Sof(H85a)=Sof(H85b)=Sof(C86A)=
 Sof(H86a)=Sof(H86b)=Sof(C87A)=Sof(H87a)=Sof(H87b)=Sof(C88A)=Sof(H88a)=
 Sof(H88b)=Sof(O8A)=Sof(C89A)=Sof(H89a)=Sof(H89b)=Sof(C90A)=Sof(H90a)=Sof(H90b)=
 Sof(C91A)=Sof(H91a)=Sof(H91b)=Sof(C92A)=Sof(H92a)=Sof(H92b)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C20(H20), C43(H43), C56(H56)
7.b Secondary CH2 refined with riding coordinates:
 C73(H73a,H73b), C74(H74a,H74b), C75(H75a,H75b), C76(H76a,H76b), C77(H77a,
 H77b), C77(H77c,H77d), C78A(H78a,H78b), C78B(H78c,H78d), C79(H79a,H79b),
 C79(H79c,H79d), C80(H80a,H80b), C81(H81a,H81b), C82(H82a,H82b), C83(H83a,H83b),
  C84(H84a,H84b), C81A(H81c,H81d), C82A(H82c,H82d), C83A(H83c,H83d), C84A(H84c,
 H84d), C81B(H81e,H81f), C82B(H82e,H82f), C83B(H83e,H83f), C84B(H84e,H84f),
 C85A(H85a,H85b), C86A(H86a,H86b), C87A(H87a,H87b), C88A(H88a,H88b), C85B(H85c,
 H85d), C86B(H86c,H86d), C87B(H87c,H87d), C88B(H88c,H88d), C89A(H89a,H89b),
 C90A(H90a,H90b), C91A(H91a,H91b), C92A(H92a,H92b), C89B(H89c,H89d), C90B(H90c,
 H90d), C91B(H91c,H91d), C92B(H92c,H92d)
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), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C39(H39),
 C41(H41), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52),
  C53(H53), C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61),
 C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
7.d Idealised Me refined as rotating group:
 C34A(H34a,H34b,H34c), C34B(H34d,H34e,H34f), C35A(H35a,H35b,H35c), C35B(H35d,
 H35e,H35f), C36A(H36a,H36b,H36c), C36B(H36d,H36e,H36f), C70(H70a,H70b,H70c),
 C71(H71a,H71b,H71c), C72(H72a,H72b,H72c)
;
_shelx_res_checksum              25279
_shelx_hkl_checksum              28056
_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 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.807