Slow magnetic relaxation in distorted tetrahedral Dy(III) aryloxide complexes.
Parmar, Vijay S.; Gransbury, Gemma K.; Whitehead, George F. S.; Mills, David P.; Winpenny, Richard E. P.; Chemical communications (Cambridge, England) 57 (2021) 9208–9211; doi:10.1039/d1cc02707g

data_7128796
_publ_section_title
;
 Slow magnetic relaxation in distorted tetrahedral Dy(III) aryloxide
 complexes.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9208
_journal_page_last               9211
_journal_paper_doi               10.1039/d1cc02707g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C54 H87 Cl Dy O3, C24 H48 Na O6, 2(C4 H8 O)'
_chemical_formula_sum            'C86 H151 Cl Dy Na O11'
_chemical_formula_weight         1582.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.064(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7711(13)
_cell_length_b                   19.5922(14)
_cell_length_c                   28.944(2)
_cell_measurement_reflns_used    4810
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      53.6280
_cell_measurement_theta_min      2.6620
_cell_volume                     8937.6(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.107a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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    -72.05 123.95   1.00   30.00    --  -38.26  73.87-115.79  196
  2  \w     74.21 272.21   1.00   30.00    --  109.00  73.87  60.09  198
  3  \w     73.02 270.02   1.00   30.00    --  107.81  73.87   5.06  197
  4  \w     74.21 272.21   1.00   30.00    --  109.00  73.87 -43.27  198
  5  \w    -72.05 123.95   1.00   30.00    --  -38.26  73.87  64.21  196
  6  \w     73.48 271.48   1.00   30.00    --  108.27  73.87-123.43  198
  7  \f    -25.79 334.43   1.00   30.00  65.22 100.01  73.87    --   360
  8  \w      0.17 196.17   1.00   30.00    --   33.96  73.87 -25.79  196
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000666000
_diffrn_orient_matrix_UB_12      -0.0088255000
_diffrn_orient_matrix_UB_13      -0.0528786000
_diffrn_orient_matrix_UB_21      0.0716470000
_diffrn_orient_matrix_UB_22      -0.0530959000
_diffrn_orient_matrix_UB_23      0.0054843000
_diffrn_orient_matrix_UB_31      -0.0666260000
_diffrn_orient_matrix_UB_32      -0.0572766000
_diffrn_orient_matrix_UB_33      0.0031202000
_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  0.1112
_diffrn_reflns_av_unetI/netI     0.1124
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39211
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        54.252
_diffrn_reflns_theta_max         54.252
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
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    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             3396
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.815
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1196
_refine_ls_number_reflns         10658
_refine_ls_number_restraints     3201
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0770P)^2^+6.9576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7137
_reflns_number_total             10658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02707g2.cif
_cod_data_source_block           xdpm94_Complex-2
_cod_depositor_comments
'Adding full bibliography for 7128795--7128798.cif.'
_cod_database_code               7128796
_manchester_internal_coll_name   XDPM94
_manchester_internal_coll_client VP
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 30
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w &\f scans'
_manchester_internal_coll_user   VP
_manchester_internal_coll_date   13/04/2019
_manchester_internal_process_user VP
_manchester_internal_process_date 13/04/2019
_manchester_internal_solution_user VP
_manchester_internal_solution_date 14/04/2019
_manchester_internal_refinement_user VP
_manchester_internal_refinement_date 15/04/2019
_manchester_internal_validation_date 10/05/21
_manchester_internal_validation_user GW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.624
_reflns_odcompleteness_completeness 97.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     54.18
_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. Uiso/Uaniso restraints and constraints
Na1 \\sim O4 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim O5 \\sim C59 \\sim
C60 \\sim C61 \\sim C62 \\sim O6 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim
O7 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim O8 \\sim C71 \\sim C72 \\sim
C73 \\sim C74 \\sim O9 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim O4A \\sim
C55A \\sim C56A \\sim C57A \\sim C58A \\sim O5A \\sim C59A \\sim C60A \\sim
C61A \\sim C62A \\sim O6A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim O7A
\\sim C67A \\sim C68A \\sim C69A \\sim C70A \\sim O8A \\sim C71A \\sim C72A
\\sim C73A \\sim C74A \\sim O9A \\sim C75A \\sim C76A \\sim C77A \\sim C78A
\\sim O10 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim O11 \\sim C84 \\sim C85
\\sim C86 \\sim C87 \\sim O10A \\sim C79A \\sim C80A \\sim C81A \\sim C82A
\\sim O11A \\sim C84A \\sim C85A \\sim C86A \\sim C87A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
3. 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
4. Same fragment restrains
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, C59, C60, C61, C62}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6, C63, C64, C65, C66}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, C67, C68, C69, C70}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O8, C71, C72, C73, C74}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, C75, C76, C77, C78}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O4A, C55A, C56A, C57A, C58A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, C59A, C60A, C61A, C62A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6A, C63A, C64A, C65A, C66A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, C67A, C68A, C69A, C70A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O8A, C71A, C72A, C73A, C74A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, C75A, C76A, C77A, C78A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, C79, C80, C81, C82}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, C84, C85, C86, C87}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, C79A, C80A, C81A, C82A}
{O4, C55, C56, C57, C58} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, C84A, C85A, C86A, C87A}
5. Others
 Sof(O4A)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=
 Sof(C57A)=Sof(H57C)=Sof(H57D)=Sof(C58A)=Sof(H58C)=Sof(H58D)=1-FVAR(1)
 Sof(O4)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=FVAR(1)
 Sof(O5A)=Sof(C59A)=Sof(H59C)=Sof(H59D)=Sof(C60A)=Sof(H60C)=Sof(H60D)=
 Sof(C61A)=Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=1-FVAR(2)
 Sof(O5)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=FVAR(2)
 Sof(O6A)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64C)=Sof(H64D)=
 Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=1-FVAR(3)
 Sof(O6)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=
 Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=FVAR(3)
 Sof(O7A)=Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=1-FVAR(4)
 Sof(O7)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=FVAR(4)
 Sof(O8A)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=
 Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=1-FVAR(5)
 Sof(O8)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(5)
 Sof(O9A)=Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=Sof(H76D)=
 Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=1-FVAR(6)
 Sof(O9)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=
 Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=FVAR(6)
 Sof(O10A)=Sof(C79A)=Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=
 Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=1-FVAR(7)
 Sof(O10)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C81)=
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=FVAR(7)
 Sof(O11A)=Sof(C84A)=Sof(H84C)=Sof(H84D)=Sof(C85A)=Sof(H85C)=Sof(H85D)=
 Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(C87A)=Sof(H87C)=Sof(H87D)=1-FVAR(8)
 Sof(O11)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=
 Sof(H86A)=Sof(H86B)=Sof(C87)=Sof(H87A)=Sof(H87B)=FVAR(8)
6.a Secondary CH2 refined with riding coordinates:
 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),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B), C55A(H55C,H55D), C56A(H56C,H56D), C57A(H57C,H57D), C58A(H58C,
 H58D), C59A(H59C,H59D), C60A(H60C,H60D), C61A(H61C,H61D), C62A(H62C,H62D),
 C63A(H63C,H63D), C64A(H64C,H64D), C65A(H65C,H65D), C66A(H66C,H66D), C67A(H67C,
 H67D), C68A(H68C,H68D), C69A(H69C,H69D), C70A(H70C,H70D), C71A(H71C,H71D),
 C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D), C75A(H75C,H75D), C76A(H76C,
 H76D), C77A(H77C,H77D), C78A(H78C,H78D), C79(H79A,H79B), C80(H80A,H80B),
 C81(H81A,H81B), C82(H82A,H82B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
  C87(H87A,H87B), C79A(H79C,H79D), C80A(H80C,H80D), C81A(H81C,H81D), C82A(H82C,
 H82D), C84A(H84C,H84D), C85A(H85C,H85D), C86A(H86C,H86D), C87A(H87C,H87D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C21(H21), C23(H23), C39(H39), C41(H41)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              12249
_shelx_hkl_checksum              92388
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.745
_oxdiff_exptl_absorpt_empirical_full_min 0.658