Polyoxometalates as advanced-performance anions for ∼<i>D</i><sub>5h</sub> Dy(III) single-ion magnets.
Lowe, Ethan; Wilson, Claire; Canaj, Angelos B.; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 54 (2025) 477–481; doi:10.1039/d4dt02877e

data_7718233
_publ_section_title
;
 Polyoxometalates as advanced-performance anions for
 &#x223c;<i>D</i><sub>5h</sub> Dy(III) single-ion magnets.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              477
_journal_page_last               481
_journal_paper_doi               10.1039/d4dt02877e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'O40 P W12, C36 H75 Dy O7 P2, 2(C18 H33 O P), 5(C4 H8 O), H2 O'
_chemical_formula_sum            'C92 H183 Dy O55 P5 W12'
_chemical_formula_weight         4692.92
_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   mixed
_audit_creation_date             2023-12-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-16 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.0650(10)
_cell_angle_beta                 91.0860(10)
_cell_angle_gamma                99.2480(10)
_cell_formula_units_Z            2
_cell_length_a                   14.8908(2)
_cell_length_b                   15.5061(2)
_cell_length_c                   28.8135(4)
_cell_measurement_reflns_used    34816
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      33.4390
_cell_measurement_theta_min      1.6360
_cell_volume                     6411.94(15)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -52.00   3.00   0.50   12.00    --  -16.37 104.00-140.00  110
  2  \w      3.00  55.00   0.50   12.00    --   19.34-104.00 117.00  104
  3  \w     21.00  64.00   0.50   12.00    --  -16.37  19.00   0.00   86
  4  \w     21.00  64.00   0.50   12.00    --  -16.37  19.00 150.00   86
  5  \w    -56.00  -2.00   0.50   12.00    --  -16.37 -57.00  90.00  108
  6  \w    -39.00  24.00   0.50   12.00    --  -16.37  77.00 120.00  126
  7  \w    -56.00  -2.00   0.50   12.00    --  -16.37 -57.00   0.00  108
  8  \w    -56.00  -2.00   0.50   12.00    --  -16.37 -57.00-180.00  108
  9  \w     21.00  64.00   0.50   12.00    --  -16.37  19.00 -60.00   86
 10  \w    -56.00  -2.00   0.50   12.00    --  -16.37 -57.00 -60.00  108
 11  \w     21.00  64.00   0.50   12.00    --  -16.37  19.00  30.00   86
 12  \w     -4.00  22.00   0.50   12.00    --   19.34  79.00 -30.39   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            84219
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.600
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_exptl_absorpt_coefficient_mu    11.435
_exptl_absorpt_correction_T_max  0.02287
_exptl_absorpt_correction_T_min  0.00802
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.431
_exptl_crystal_description       block
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         3.008
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1524
_refine_ls_number_reflns         26039
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0941P)^2^+69.0892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18639
_reflns_number_total             26039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02877e2.cif
_cod_data_source_block           2023ncs0520_2a
_cod_database_code               7718233
_shelx_shelxl_version_number     2018/3
_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 O(H,H) groups
2. Restrained distances
 C93-C83 \\sim C83-C82 \\sim C82-C81 \\sim C93-C81 \\sim C84-C83 \\sim C88-C87
\\sim C86-C85 \\sim C87-C86
 with sigma of 0.02
 O53-C84 \\sim O53-C81 \\sim O54-C85 \\sim O54-C88
 with sigma of 0.02
 C92-O91 \\sim C92-O91A
 with sigma of 0.02
 C90-O91 \\sim C90-O91A
 with sigma of 0.02
 O91-C90 \\sim O91A-C92 \\sim O91-C92 \\sim O91A-C90
 with sigma of 0.02
 C90-C89 \\sim C89-C55 \\sim C92-C55
 with sigma of 0.02
 C74-C73 \\sim C75-C74 \\sim C76-C75
 with sigma of 0.02
 O51-C76 \\sim O51-C73
 with sigma of 0.02
 Dy1-H5A \\sim Dy1-H5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C93 \\sim C83 \\sim C84: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
C85 \\sim O54 \\sim C88 \\sim C87 \\sim C86: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
C89 \\sim C90 \\sim C55 \\sim C92 \\sim O91A \\sim O91: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
O51 \\sim C76 \\sim C73 \\sim C75 \\sim H76A \\sim H76B \\sim H73A \\sim H73B
\\sim C74 \\sim H75A \\sim H75B \\sim H74A \\sim H74B: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
4. Others
 Sof(W12B)=1-FVAR(1)
 Sof(W12A)=FVAR(1)
 Fixed Sof: H83A(0.75) H83B(0.75) H83C(0.25) H83D(0.25) H81A(0.75) H81B(0.75)
 H81C(0.25) H81D(0.25) H92A(0.5) H92B(0.5) H92C(0.5) H92D(0.5) C82(0.75)
 H82A(0.75) H82B(0.75) H90A(0.5) H90B(0.5) H90C(0.5) H90D(0.5) O91(0.5)
 C93(0.25) H93A(0.25) H93B(0.25) O91A(0.5)
5.a Free rotating group:
 O5(H5A,H5B), O50(H50C,H50D)
5.b Rotating group:
 O4(H4A,H4B), O6(H6A,H6B), O7(H7A,H7B), O3(H3A,H3B)
5.c Ternary CH refined with riding coordinates:
 C31(H31), C1(H1), C13(H13), C43(H43), C25(H25), C7(H7), C49(H49), C37(H37),
 C67(H67), C61(H61), C94(H94)
5.d Secondary CH2 refined with riding coordinates:
 C3(H3C,H3D), C2(H2A,H2B), C36(H36A,H36B), C38(H38A,H38B), C30(H30A,H30B),
 C4(H4C,H4D), C33(H33A,H33B), C8(H8A,H8B), C39(H39A,H39B), C35(H35A,H35B),
 C17(H17A,H17B), C14(H14A,H14B), C16(H16A,H16B), C34(H34A,H34B), C32(H32A,H32B),
  C9(H9A,H9B), C6(H6C,H6D), C79(H79A,H79B), C24(H24A,H24B), C52(H52A,H52B),
 C41(H41A,H41B), C54(H54A,H54B), C78(H78A,H78B), C53(H53A,H53B), C77(H77A,H77B),
  C23(H23A,H23B), C44(H44A,H44B), C42(H42A,H42B), C55(H55A,H55B), C20(H20A,
 H20B), C80(H80A,H80B), C21(H21A,H21B), C70(H70A,H70B), C71(H71A,H71B),
 C47(H47A,H47B), C48(H48A,H48B), C29(H29A,H29B), C18(H18A,H18B), C72(H72A,H72B),
  C45(H45A,H45B), C83(H83A,H83B), C83(H83C,H83D), C5(H5C,H5D), C50(H50A,H50B),
 C81(H81A,H81B), C81(H81C,H81D), C15(H15A,H15B), C75(H75A,H75B), C89(H89A,H89B),
  C62(H62A,H62B), C51(H51A,H51B), C46(H46A,H46B), C65(H65A,H65B), C66(H66A,
 H66B), C12(H12A,H12B), C10(H10A,H10B), C68(H68A,H68B), C88(H88A,H88B),
 C22(H22A,H22B), C26(H26A,H26B), C11(H11A,H11B), C40(H40A,H40B), C85(H85A,H85B),
  C28(H28A,H28B), C92(H92A,H92B), C92(H92C,H92D), C63(H63A,H63B), C76(H76A,
 H76B), C60(H60A,H60B), C64(H64A,H64B), C56(H56A,H56B), C27(H27A,H27B),
 C69(H69A,H69B), C59(H59A,H59B), C86(H86A,H86B), C87(H87A,H87B), C84(H84A,H84B),
  C57(H57A,H57B), C73(H73A,H73B), C74(H74A,H74B), C58(H58A,H58B), C82(H82A,
 H82B), C90(H90A,H90B), C90(H90C,H90D), C93(H93A,H93B)
;
_shelx_res_checksum              14739
_shelx_hkl_checksum              1445
_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
;