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_7128795
_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
'C60 H82 Cl2 Dy O2, C24 H48 Na O6, 3(C4 H8 O)'
_chemical_formula_sum            'C96 H154 Cl2 Dy Na O11'
_chemical_formula_weight         1740.57
_chemical_name_systematic        '[Dy(OAd*)2Cl2]'
_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             2021-05-11
_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                 94.0073(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.39679(13)
_cell_length_b                   46.8821(5)
_cell_length_c                   16.9513(2)
_cell_measurement_reflns_used    17095
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.8050
_cell_measurement_theta_min      2.7680
_cell_volume                     9035.03(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_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)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.966
_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      0.00  68.00   1.00    1.00    --    5.00  57.00  30.00   68
  2  \w    -76.00  40.00   1.00    1.00    --  -45.60  57.00  90.00  116
  3  \w    -61.00  44.00   1.00    1.00    --  -45.60  57.00 150.00  105
  4  \w   -158.00-115.00   1.00    4.00    -- -107.20 -57.00-150.00   43
  5  \w   -196.00-163.00   1.00    4.00    -- -107.20 -57.00-150.00   33
  6  \w   -114.00 -62.00   1.00    4.00    -- -107.20  57.00 150.00   52
  7  \w   -136.00-108.00   1.00    4.00    -- -107.20  57.00 120.00   28
  8  \w   -144.00 -19.00   1.00    4.00    -- -107.20  76.00 150.00  125
  9  \w   -139.00 -25.00   1.00    4.00    -- -107.20  57.00 -30.00  114
 10  \w   -132.00 -63.00   1.00    4.00    -- -107.20  76.00-150.00   69
 11  \w   -146.00 -33.00   1.00    4.00    -- -107.20  38.00 -30.00  113
;
_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      0.0043958000
_diffrn_orient_matrix_UB_12      0.0006842000
_diffrn_orient_matrix_UB_13      0.0910308000
_diffrn_orient_matrix_UB_21      -0.0263257000
_diffrn_orient_matrix_UB_22      0.0322253000
_diffrn_orient_matrix_UB_23      -0.0024943000
_diffrn_orient_matrix_UB_31      -0.1328672000
_diffrn_orient_matrix_UB_32      -0.0063589000
_diffrn_orient_matrix_UB_33      -0.0030209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50657
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.106
_diffrn_reflns_theta_min         2.778
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.7b (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             3716
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         18249
_refine_ls_number_restraints     3979
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0762P)^2^+2.4280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14786
_reflns_number_total             18249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02707g2.cif
_cod_data_source_block           rdpm232_Complex1
_cod_depositor_comments
'Adding full bibliography for 7128795--7128798.cif.'
_cod_original_cell_volume        9035.02(18)
_cod_database_code               7128795
_manchester_internal_diff_code   FRX(right)
_manchester_internal_coll_name   RDPM232
_manchester_internal_coll_client VP/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time '1 & 4'
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   Ash
_manchester_internal_coll_date   08/09/2020
_manchester_internal_process_user VP
_manchester_internal_process_date 08/09/2020
_manchester_internal_solution_user VP
_manchester_internal_solution_date 15/09/2020
_manchester_internal_refinement_user VP
_manchester_internal_refinement_date 16/09/2020
_manchester_internal_validation_date 10/05/21
_manchester_internal_validation_user GW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H98ClDyO4
_chemical_oxdiff_usercomment     115_VP
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.245
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Restrained distances
 C88-C87
 1.49 with sigma of 0.02
 Na1-O8 \\sim Na1-O8A \\sim Na1-O3 \\sim Na1-O3A \\sim Na1-O7A \\sim Na1-O7
\\sim Na1-O4A \\sim Na1-O4 ~
 Na1-O6 \\sim Na1-O6A \\sim Na1-O5A \\sim Na1-O5
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O3 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim O4 \\sim C65 \\sim C66 \\sim
C67 \\sim C68 \\sim O5 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim O6 \\sim
C73 \\sim C74 \\sim C75 \\sim C76 \\sim O7 \\sim C77 \\sim C78 \\sim C79 \\sim
C80 \\sim O8 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim O9 \\sim C85 \\sim
C86 \\sim C87 \\sim C88 \\sim O10 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim
O11 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim O3A \\sim C61A \\sim C62A
\\sim C63A \\sim C64A \\sim O4A \\sim C65A \\sim C66A \\sim C67A \\sim C68A
\\sim O5A \\sim C69A \\sim C70A \\sim C71A \\sim C72A \\sim O6A \\sim C73A
\\sim C74A \\sim C75A \\sim C76A \\sim O7A \\sim C77A \\sim C78A \\sim C79A
\\sim C80A \\sim O8A \\sim C81A \\sim C82A \\sim C83A \\sim C84A \\sim O10A
\\sim C89A \\sim C90A \\sim C91A \\sim C92A \\sim O11A \\sim C93A \\sim C94A
\\sim C95A \\sim C96A: 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
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O4, C65, C66, C67, C68}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5, C69, C70, C71, C72}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6, C73, C74, C75, C76}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, C77, C78, C79, C80}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O8, C81, C82, C83, C84}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, C85, C86, C87, C88}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10, C89, C90, C91, C92}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11, C93, C94, C95, C96}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, C61A, C62A, C63A, C64A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O4A, C65A, C66A, C67A, C68A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O5A, C69A, C70A, C71A, C72A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6A, C73A, C74A, C75A, C76A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, C77A, C78A, C79A, C80A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O8A, C81A, C82A, C83A, C84A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O10A, C89A, C90A, C91A, C92A}
{O3, C61, C62, C63, C64} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O11A, C93A, C94A, C95A, C96A}
5. Others
 Sof(O5)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=
 Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(O6)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=
 Sof(H76A)=Sof(H76B)=Sof(O8)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=
 Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(O7A)=
 Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=Sof(H78C)=Sof(H78D)=Sof(C79A)=
 Sof(H79C)=Sof(H79D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=1-FVAR(1)
 Sof(O7)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(O5A)=Sof(C69A)=Sof(H69C)=
 Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=Sof(H71C)=Sof(H71D)=
 Sof(C72A)=Sof(H72C)=Sof(H72D)=Sof(O6A)=Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=
 Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C76A)=Sof(H76C)=
 Sof(H76D)=Sof(O8A)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=FVAR(1)
 Sof(O3A)=Sof(C61A)=Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=
 Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64C)=Sof(H64D)=Sof(O4A)=Sof(C65A)=
 Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=Sof(H67C)=
 Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=1-FVAR(2)
 Sof(O3)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(O4)=Sof(C65)=Sof(H65A)=
 Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=
 Sof(H68A)=Sof(H68B)=FVAR(2)
 Sof(O10A)=Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=Sof(H90D)=
 Sof(C91A)=Sof(H91C)=Sof(H91D)=Sof(C92A)=Sof(H92C)=Sof(H92D)=1-FVAR(3)
 Sof(O10)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=
 Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=Sof(H92B)=FVAR(3)
 Sof(O11A)=Sof(C93A)=Sof(H93C)=Sof(H93D)=Sof(C94A)=Sof(H94C)=Sof(H94D)=
 Sof(C95A)=Sof(H95C)=Sof(H95D)=Sof(C96A)=Sof(H96C)=Sof(H96D)=1-FVAR(4)
 Sof(O11)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C95)=
 Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C13(H13), C15(H15), C25(H25), C27(H27), C29(H29), C41(H41),
 C43(H43), C45(H45), C55(H55), C57(H57), C59(H59)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
  C28(H28A,H28B), C30(H30A,H30B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C42(H42A,H42B), C44(H44A,H44B), C46(H46A,H46B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C56(H56A,H56B), C58(H58A,H58B), 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), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
  C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,
 H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B), 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), C79A(H79C,H79D),
 C80A(H80C,H80D), C81A(H81C,H81D), C82A(H82C,H82D), C83A(H83C,H83D), C84A(H84C,
 H84D), C89A(H89C,H89D), C90A(H90C,H90D), C91A(H91C,H91D), C92A(H92C,H92D),
 C93A(H93C,H93D), C94A(H94C,H94D), C95A(H95C,H95D), C96A(H96C,H96D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C33(H33), C35(H35)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              59133
_shelx_hkl_checksum              50092
_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 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.820