High magnetization reversal barriers in luminescent dysprosium octahedral and pentagonal bipyramidal single-molecule magnets based on fluorinated alkoxide ligands.
Long, Jérôme; Tolpygin, Aleksei O.; Lyubov, Dmitry M.; Rad'kova, Natalia Yu; Cherkasov, Anton V.; Nelyubina, Yulia V.; Guari, Yannick; Larionova, Joulia; Trifonov, Alexander A.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8487–8496; doi:10.1039/d1dt01319j

data_7707393
_publ_section_title
;
 High magnetization reversal barriers in luminescent dysprosium octahedral
 and pentagonal bipyramidal single-molecule magnets based on fluorinated
 alkoxide ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8487
_journal_page_last               8496
_journal_paper_doi               10.1039/d1dt01319j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H40 Dy F18 O7, 2.5(C4 H8 O), C24 H19 B'
_chemical_formula_sum            'C78 H79 B Dy F18 O9.5'
_chemical_formula_weight         1683.72
_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             2021-03-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-03-19 deposited with the CCDC.	2021-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.820(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9539(13)
_cell_length_b                   24.207(2)
_cell_length_c                   23.410(2)
_cell_measurement_reflns_used    2717
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.29
_cell_measurement_theta_min      2.29
_cell_volume                     7331.9(11)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1365
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47737
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.574
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0837 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.8303.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       plate
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00048(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         14392
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7855
_reflns_number_total             14392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01319j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7707391--7707393.cif.'
_cod_original_cell_volume        7331.8(12)
_cod_original_formula_sum        'C78 H79 B Dy F18 O9.50'
_cod_database_code               7707393
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.729
_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
2. Restrained distances
 C53-C54_$1
 2.4 with sigma of 0.02
 C11S-C9S
 2.2 with sigma of 0.02
 C27S-C25S
 2.2 with sigma of 0.02
 C26S-C25S
 1.4 with sigma of 0.02
 C25S-C28S
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5S) \\sim Ueq, Uanis(C5S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4S) \\sim Ueq, Uanis(C4S') \\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(C2S')
\\sim Ueq, Uanis(C1S') \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C3S') \\sim Ueq, Uanis(C3S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26X) \\sim Ueq, Uanis(C28X) \\sim Ueq, Uanis(C25X) \\sim Ueq,
Uanis(C27X) \\sim Ueq, Uanis(O6X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6S) \\sim Ueq, Uanis(C6S') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16S) \\sim Ueq, Uanis(C16X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18X) \\sim Ueq, Uanis(C18S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20X) \\sim Ueq, Uanis(C20S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C19S) \\sim Ueq, Uanis(C19X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9S') \\sim Ueq, Uanis(C9S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11S) \\sim Ueq, Uanis(C11X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10X) \\sim Ueq, Uanis(C10S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17X) \\sim Ueq, Uanis(C17S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14X) \\sim Ueq, Uanis(C15X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C6S) = Uanis(C6S')
Uanis(C5S) = Uanis(C5S')
Uanis(C1S') = Uanis(C1S)
Uanis(C2S) = Uanis(C2S')
Uanis(C4S) = Uanis(C4S')
Uanis(C3S) = Uanis(C3S')
Uanis(C15X) = Uanis(C15S)
Uanis(C14X) = Uanis(C14S)
Uanis(C13S) = Uanis(C13X)
Uanis(C16S) = Uanis(C16X)
Uanis(C18S) = Uanis(C18X)
Uanis(C17S) = Uanis(C17X)
Uanis(C19S) = Uanis(C19X)
Uanis(C20S) = Uanis(C20X)
Uanis(C11X) = Uanis(C11S)
Uanis(C12X) = Uanis(C12S)
Uanis(C10X) = Uanis(C10S)
Uanis(C9S') = Uanis(C9S)
Uanis(O6X) = Uanis(O6S')
Uanis(C25X) = Uanis(C25S)
Uanis(C26S) = Uanis(C26X)
Uanis(C27X) = Uanis(C27S)
Uanis(C28S) = Uanis(C28X)
4. Others
 Sof(H7SC)=Sof(H7SD)=Sof(C5S')=Sof(H5SC)=Sof(H5SD)=Sof(C6S')=Sof(H6SC)=
 Sof(H6SD)=1-FVAR(1)
 Sof(H7SA)=Sof(H7SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=
 FVAR(1)
 Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(C2S')=Sof(H2SA)=Sof(H2SB)=Sof(C3S')=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S')=Sof(H4SA)=Sof(H4SB)=1-FVAR(2)
 Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(C2S)=Sof(H2SC)=Sof(H2SD)=Sof(C3S)=Sof(H3SC)=
 Sof(H3SD)=Sof(C4S)=Sof(H4SC)=Sof(H4SD)=FVAR(2)
 Sof(C13X)=Sof(H13C)=Sof(H13D)=Sof(C14X)=Sof(H14C)=Sof(H14D)=Sof(C15X)=
 Sof(H15C)=Sof(H15D)=Sof(C16X)=Sof(H16C)=Sof(H16D)=1-FVAR(3)
 Sof(C13S)=Sof(H13A)=Sof(H13B)=Sof(C14S)=Sof(H14A)=Sof(H14B)=Sof(C15S)=
 Sof(H15A)=Sof(H15B)=Sof(C16S)=Sof(H16A)=Sof(H16B)=FVAR(3)
 Sof(C17X)=Sof(H17C)=Sof(H17D)=Sof(C18X)=Sof(H18C)=Sof(H18D)=Sof(C19X)=
 Sof(H19C)=Sof(H19D)=Sof(C20X)=Sof(H20C)=Sof(H20D)=1-FVAR(4)
 Sof(C17S)=Sof(H17A)=Sof(H17B)=Sof(C18S)=Sof(H18A)=Sof(H18B)=Sof(C19S)=
 Sof(H19A)=Sof(H19B)=Sof(C20S)=Sof(H20A)=Sof(H20B)=FVAR(4)
 Sof(C9S')=Sof(H9SC)=Sof(H9SD)=Sof(C10X)=Sof(H10C)=Sof(H10D)=Sof(C11X)=
 Sof(H11C)=Sof(H11D)=Sof(C12X)=Sof(H12C)=Sof(H12D)=1-FVAR(5)
 Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(C10S)=Sof(H10A)=Sof(H10B)=Sof(C11S)=
 Sof(H11A)=Sof(H11B)=Sof(C12S)=Sof(H12A)=Sof(H12B)=FVAR(5)
 Sof(O6S')=Sof(C25S)=Sof(H25C)=Sof(H25D)=Sof(C26S)=Sof(H26C)=Sof(H26D)=
 Sof(C27S)=Sof(H27C)=Sof(H27D)=Sof(C28S)=Sof(H28C)=Sof(H28D)=1-FVAR(6)
 Sof(O6X)=Sof(C25X)=Sof(H25A)=Sof(H25B)=Sof(C26X)=Sof(H26A)=Sof(H26B)=
 Sof(C27X)=Sof(H27A)=Sof(H27B)=Sof(C28X)=Sof(H28A)=Sof(H28B)=FVAR(6)
 Fixed Sof: O7S(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7S(H7SA,H7SB), C7S(H7SC,H7SD), C8S(H8SA,H8SB), C1S'(H1SA,H1SB), C2S'(H2SA,
 H2SB), C3S'(H3SA,H3SB), C4S'(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB),
 C9S(H9SA,H9SB), C10S(H10A,H10B), C11S(H11A,H11B), C12S(H12A,H12B), C13S(H13A,
 H13B), C14S(H14A,H14B), C15S(H15A,H15B), C16S(H16A,H16B), C17S(H17A,H17B),
 C18S(H18A,H18B), C19S(H19A,H19B), C20S(H20A,H20B), C1S(H1SC,H1SD), C2S(H2SC,
 H2SD), C3S(H3SC,H3SD), C4S(H4SC,H4SD), C5S'(H5SC,H5SD), C6S'(H6SC,H6SD),
 C9S'(H9SC,H9SD), C10X(H10C,H10D), C11X(H11C,H11D), C12X(H12C,H12D), C13X(H13C,
 H13D), C14X(H14C,H14D), C15X(H15C,H15D), C16X(H16C,H16D), C17X(H17C,H17D),
 C18X(H18C,H18D), C19X(H19C,H19D), C20X(H20C,H20D), C21S(H21A,H21B), C22S(H22A,
 H22B), C23S(H23A,H23B), C24S(H24A,H24B), C25X(H25A,H25B), C26X(H26A,H26B),
 C27X(H27A,H27B), C28X(H28A,H28B), C53(H53A,H53B), C54(H54A,H54B), C25S(H25C,
 H25D), C26S(H26C,H26D), C27S(H27C,H27D), C28S(H28C,H28D)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47)
;
_shelx_res_checksum              17502
_shelx_hkl_checksum              93795
_olex2_submission_special_instructions 'No special instructions were received'