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_7128797
_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 O2 Y, C24 H48 Na O6, 3(C4 H8 O)'
_chemical_formula_sum            'C96 H154 Cl2 Na O11 Y'
_chemical_formula_weight         1666.98
_chemical_name_systematic        '[Y(OAr)2Cl2][Na(THF)6].3THF'
_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                 94.260(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3031(4)
_cell_length_b                   46.2765(15)
_cell_length_c                   16.8926(7)
_cell_measurement_reflns_used    15655
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.0860
_cell_measurement_theta_min      1.4990
_cell_volume                     8811.6(6)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -63.00 -33.00   1.00   15.00    --    7.20  40.00   0.00   30
  2  \w      2.00  40.00   1.00   15.00    --    7.20  40.00   0.00   38
  3  \w    -81.00  95.00   1.00   15.00    --    7.20  40.00 -90.00  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      0.0008408000
_diffrn_orient_matrix_UB_12      0.0139165000
_diffrn_orient_matrix_UB_13      -0.0175432000
_diffrn_orient_matrix_UB_21      0.0047123000
_diffrn_orient_matrix_UB_22      0.0063950000
_diffrn_orient_matrix_UB_23      0.0382894000
_diffrn_orient_matrix_UB_31      0.0627045000
_diffrn_orient_matrix_UB_32      -0.0007206000
_diffrn_orient_matrix_UB_33      0.0005196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            61122
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.495
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_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    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         17943
_refine_ls_number_restraints     2777
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0874
_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^)+(0.0615P)^2^+20.9248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11942
_reflns_number_total             17943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02707g2.cif
_cod_data_source_block           ldpm161_Comple(1-Y)
_cod_depositor_comments
'Adding full bibliography for 7128795--7128798.cif.'
_cod_database_code               7128797
_manchester_internal_diff_code   LDPM161
_manchester_internal_coll_client VP/DPM
_manchester_internal_coll_user   AW
_manchester_internal_coll_date   27/08/2020
_manchester_internal_process_date 15/09/2020
_manchester_internal_process_user VP
_manchester_internal_solution_date 16/09/2020
_manchester_internal_solution_user VP
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 15
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_refinement_date 16/09/2020
_manchester_internal_refinement_user VP
_manchester_internal_validation_date 10/05/21
_manchester_internal_validation_user GW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H98ClO4Y
_chemical_oxdiff_usercomment     113_VP
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.793
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{C70A, C71}
2. Restrained distances
 C84-C83 = C83-C82 = C83-C82A = C82-C81 = C82A-C81A = C70-C69 = C72A-C71A =
 C71A-C70A = C71-C70 = C72-C70A = C71-C69A
 1.49 with sigma of 0.02
 C94-C93 = C95-C94 = C95A-C94 = C96A-C95A = C96-C95
 1.49 with sigma of 0.02
 Na1-O5 \\sim Na1-O6 \\sim Na1-O6A \\sim Na1-O7 \\sim Na1-O7A \\sim Na1-O8
\\sim Na1-O3 \\sim Na1-O3A ~
 Na1-O4 \\sim Na1-O4A
 with sigma of 0.02
 C70-C69A \\sim C72-C71A \\sim C72A-C70A \\sim C71-C69 \\sim C84-C82A \\sim
C83-C81A \\sim C83-C81 ~
 C84-C82
 with sigma of 0.02
 O8-C84 \\sim O8-C81 \\sim O8-C81A \\sim O5-C69 \\sim O5-C72A \\sim O5-C69A
\\sim O5-C72
 with sigma of 0.02
 O11-C96A \\sim O11-C96 \\sim O11-C93
 with sigma of 0.02
 C95A-C93 \\sim C95-C93 \\sim C96A-C94 \\sim C96-C94
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C69A \\sim C69 \\sim C70 \\sim C71 \\sim C70A \\sim C71A \\sim C72A \\sim C72:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O6 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim O6A \\sim C73A \\sim C74A
\\sim C75A \\sim C76A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O7 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim O7A \\sim C77A \\sim C78A
\\sim C79A \\sim C80A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O4 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim O4A \\sim C65A \\sim C66A
\\sim C67A \\sim C68A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O9 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim O9A \\sim C85A \\sim C86A
\\sim C87A \\sim C88A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C83 \\sim C84 \\sim C81 \\sim C82 \\sim C81A \\sim C82A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
O11 \\sim C93 \\sim C96 \\sim C96A \\sim C94 \\sim C95 \\sim C95A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C70A) = Uanis(C71)
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
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3, C61, C62, C63, C64}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O4, C65, C66, C67, C68}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6, C73, C74, C75, C76}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7, C77, C78, C79, C80}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9, C85, C86, C87, C88}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O3A, C61A, C62A, C63A, C64A}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O4A, C65A, C66A, C67A, C68A}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6A, C73A, C74A, C75A, C76A}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O7A, C77A, C78A, C79A, C80A}
{O10, C89, C90, C91, C92} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O9A, C85A, C86A, C87A, C88A}
6. Others
 Sof(C69A)=Sof(H69A)=Sof(H69B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C71A)=
 Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72A)=Sof(H72B)=1-FVAR(1)
 Sof(C69)=Sof(H69C)=Sof(H69D)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C70A)=Sof(H70C)=
 Sof(H70D)=Sof(C72)=Sof(H72C)=Sof(H72D)=FVAR(1)
 Sof(H83C)=Sof(H83D)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=
 Sof(H82D)=1-FVAR(2)
 Sof(H83A)=Sof(H83B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 FVAR(2)
 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)=1-FVAR(3)
 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)=FVAR(3)
 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(4)
 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)=FVAR(4)
 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(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(5)
 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)=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)=FVAR(5)
 Sof(O9A)=Sof(C85A)=Sof(H85C)=Sof(H85D)=Sof(C86A)=Sof(H86C)=Sof(H86D)=
 Sof(C87A)=Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=1-FVAR(6)
 Sof(O9)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C87)=
 Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=FVAR(6)
 Sof(H94C)=Sof(H94D)=Sof(C96A)=Sof(H96C)=Sof(H96D)=Sof(C95A)=Sof(H95C)=
 Sof(H95D)=1-FVAR(7)
 Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=
 FVAR(7)
7.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)
7.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),
  C69A(H69A,H69B), C69(H69C,H69D), C70(H70A,H70B), C71(H71A,H71B), C70A(H70C,
 H70D), C71A(H71C,H71D), C72A(H72A,H72B), C72(H72C,H72D), C83(H83A,H83B),
 C83(H83C,H83D), C84(H84A,H84B), C81(H81A,H81B), C82(H82A,H82B), C81A(H81C,
 H81D), C82A(H82C,H82D), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C94(H94C,H94D), C95(H95A,H95B),
  C96(H96A,H96B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C85(H85A,H85B), C86(H86A,
 H86B), C87(H87A,H87B), C88(H88A,H88B), C61A(H61C,H61D), C62A(H62C,H62D),
 C63A(H63C,H63D), C64A(H64C,H64D), C65A(H65C,H65D), C66A(H66C,H66D), C67A(H67C,
 H67D), C68A(H68C,H68D), C73A(H73C,H73D), C74A(H74C,H74D), C75A(H75C,H75D),
 C76A(H76C,H76D), C77A(H77C,H77D), C78A(H78C,H78D), C79A(H79C,H79D), C80A(H80C,
 H80D), C85A(H85C,H85D), C86A(H86C,H86D), C87A(H87C,H87D), C88A(H88C,H88D),
 C96A(H96C,H96D), C95A(H95C,H95D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C33(H33), C35(H35)
7.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              87721
_shelx_hkl_checksum              49404
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.679