Observation of Magnetodielectric Effect in a Dysprosium-Based Single-Molecule Magnet.
Wang, Yu-Xia; Ma, Yinina; Chai, Yisheng; Shi, Wei; Sun, Young; Cheng, Peng; Journal of the American Chemical Society 140 (2018) 7795–7798; doi:10.1021/jacs.8b04818

data_4132550
_publ_section_title
;
 Observation of Magnetodielectric Effect in a Dysprosium-Based
 Single-Molecule Magnet.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7795
_journal_page_last               7798
_journal_paper_doi               10.1021/jacs.8b04818
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C38 H72 Cl3 Dy O3 P2, C2 H6 O'
_chemical_formula_sum            'C40 H78 Cl3 Dy O4 P2'
_chemical_formula_weight         953.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4000(5)
_cell_length_b                   15.3943(5)
_cell_length_c                   19.6252(13)
_cell_measurement_reflns_used    5040
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.9742
_cell_measurement_theta_min      2.3740
_cell_volume                     4652.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15242
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.842
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1988
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 1457 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.078(14)
_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     459
_refine_ls_number_reflns         7796
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5823
_reflns_number_total             7796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04818_si_002.cif
_cod_data_source_block           a
_cod_database_code               4132550
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7065(14)
 0.2935(14)
2. 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, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C21-C5
 1.45 with sigma of 0.02
 C6-C2
 1.45 with sigma of 0.02
 H6A_$1-H13B_$2
 2.15 with sigma of 0.02
 H6C-H13B_$3
 2.15 with sigma of 0.02
 O1AA-H1AB
 0.85 with sigma of 0.01
 O1AA-H1AA
 0.85 with sigma of 0.01
 C2-O1AA
 1.45 with sigma of 0.02
 C21-O1AA
 1.45 with sigma of 0.02
 C11-C8
 1.45 with sigma of 0.02
 O2AA-C11
 1.4 with sigma of 0.02
 Dy1-H1AB
 2.974488 with sigma of 0.02
 Dy1-H1AA
 2.923229 with sigma of 0.02
 C2-H1AB
 1.886394 with sigma of 0.02
 C21-H1AA
 1.912694 with sigma of 0.02
 C8CA-C20 \\sim C20-C9
 with sigma of 0.02
 C1-C0BA \\sim C0BA-C8CA
 with sigma of 0.02
 C7-C4 \\sim C4-C6DA
 with sigma of 0.02
 C4-C6DA \\sim C6DA-C15
 with sigma of 0.02
 C6DA-C15 \\sim C15-C3CA
 with sigma of 0.02
 C9-C20 \\sim C20-C8CA
 with sigma of 0.02
 C13-C1 \\sim C1-C0BA
 with sigma of 0.02
 C8CA-C13 \\sim C1-C20
 with sigma of 0.02
 C1-C13 \\sim C13-C9
 with sigma of 0.02
 C13-C9 \\sim C9-C20
 with sigma of 0.02
 C8CA-C13 \\sim C20-C1
 with sigma of 0.02
 C8CA-C1 \\sim C13-C20
 with sigma of 0.02
 C8CA-C0BA \\sim C0BA-C1
 with sigma of 0.02
 C20-C9 \\sim C9-C13
 with sigma of 0.02
 C9-C13 \\sim C13-C1
 with sigma of 0.02
 C0BA-C8CA \\sim C8CA-C20
 with sigma of 0.02
 C0BA-C1 \\sim C1-C13
 with sigma of 0.02
 C15-C3CA \\sim C3CA-C4CA
 with sigma of 0.02
 C3CA-C4CA \\sim C4CA-C7
 with sigma of 0.02
 C4CA-C7 \\sim C7-C4
 with sigma of 0.02
 C6DA-C4CA \\sim C4-C3CA
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C0BA \\sim C8CA \\sim C20 \\sim C1 \\sim C9 \\sim C13: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.005
C4CA \\sim C4 \\sim C6DA \\sim C15 \\sim C3CA \\sim C7: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.005
C6CA \\sim P6AA \\sim C15 \\sim C0BA: within 3.8A with sigma of 0.003 and sigma
for terminal atoms of 0.003
Uanis(C15) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4CA) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C8CA) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C3CA) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C2) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O2AA) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C2) = Uanis(C21)
Uanis(C6) = Uanis(C5)
5. Others
 Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=1-
 FVAR(1)
 Sof(H1AA)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=
 FVAR(1)
6.a Riding coordinates:
 O1AA(H1AB), O1AA(H1AA), O2AA(H2AA), C3AA(H3AA,H3AB), C4AA(H4AA,H4AB),
 C5CA(H5CA,H5CB), C7CA(H7CA,H7CB), C7BA(H7BA,H7BB), C9BA(H9BA,H9BB), C3CA(H3CA,
 H3CB), C6DA(H6DA,H6DB), C8DA(H8DA,H8DB), C9DA(H9DA,H9DB), C0EA(H0EA,H0EB),
 C3BA(H3BA,H3BB), C4CA(H4CA,H4CB), C8CA(H8CA,H8CB), C0DA(H0DA,H0DB), C1DA(H1DA,
 H1DB), C2(H2A,H2B), C3DA(H3DA,H3DB), C5DA(H5DA,H5DB), C0CA(H0CA,H0CB),
 C5AA(H5AA,H5AB), C0AA(H0AA,H0AB), C11(H11A,H11B), C12(H12A,H12B), C20(H20A,
 H20B), C4(H4A,H4B), C7(H7A,H7B), C1(H1A,H1B), C3(H3A,H3B), C9(H9A,H9B),
 C13(H13A,H13B), C6(H6A,H6B,H6C), C21(H21A,H21B), C5(H5A,H5B,H5C), C8(H8A,H8B,
 H8C)
6.b Ternary CH refined with riding coordinates:
 C6CA(H6CA), C5BA(H5BA), C1CA(H1CA), C0BA(H0BA), C7DA(H7DA), C15(H15)
6.c Secondary CH2 refined with riding coordinates:
 C9CA(H9CA,H9CB)
;
_shelx_res_checksum              51007
_shelx_hkl_checksum              76693
_olex2_submission_special_instructions 'No special instructions were received'