High-temperature magnetic blocking and magneto-structural correlations in a series of dysprosium(iii) metallocenium single-molecule magnets.
Randall McClain, K.; Gould, Colin A.; Chakarawet, Khetpakorn; Teat, Simon J.; Groshens, Thomas J.; Long, Jeffrey R.; Harvey, Benjamin G.; Chemical science 9 (2018) 8492–8503; doi:10.1039/c8sc03907k

data_1552914
_publ_section_title
;
 High-temperature magnetic blocking and magneto-structural correlations in
 a series of dysprosium(iii) metallocenium single-molecule magnets.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              8492
_journal_page_last               8503
_journal_paper_doi               10.1039/c8sc03907k
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         '1(C34 H58 Y), B C24 F20'
_chemical_formula_sum            'C58 H58 B F20 Y'
_chemical_formula_weight         1234.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-17 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.053(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.538(2)
_cell_length_b                   14.4952(18)
_cell_length_c                   22.753(3)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.377
_cell_measurement_theta_min      2.174
_cell_volume                     5454.4(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.405
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0942 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.7578. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.194
_refine_diff_density_max         1.299
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         24026
_refine_ls_number_restraints     600
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+9.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2386
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17173
_reflns_number_total             24026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k3.cif
_cod_data_source_block           tg_rm_3_75_1_0m
_cod_original_cell_volume        5454.3(12)
_cod_database_code               1552914
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.263(19)
 0.265(11) 0.237(11) 0.235(11)
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
3. Restrained distances
 F72B-C72B = F73B-C73B = F74B-C74B = F75B-C75B = F76B-C76B = F52B-C52B = F53B-
 C53B = F55B-C55B = F56B-C56B = F62B-C62B = F63B-C63B = F64B-C64B = F65B-C65B =
 F66B-C66B = F86B-C86B = F85B-C85B = F84B-C84B = F83B-C83B = F82B-C82B
 1.37 with sigma of 0.02
 F13B-C13B = F12B-C12B = F14B-C14B = F15B-C15B = F16B-C16B = F36B-C36B = F35B-
 C35B = F34B-C34B = F33B-C33B = F32B-C32B = F22B-C22B = F23B-C23B = F24B-C24B =
 F25B-C25B = F26B-C26B
 1.37 with sigma of 0.02
 C81B-B2B = C71B-B2B = C51B-B2B = C61B-B2B = B1B-C31B = B1B-C21B
 1.68 with sigma of 0.02
 C18-C26 = C20-C26 = C52-C66 = C55-C66
 2.6 with sigma of 0.03
 C13-C12 = C13A-C12 = C14A-C12 = C14-C12 = C58C-C57C = C59C-C57C = C63C-C65C
 1.54 with sigma of 0.02
 F42B-C42B = F43B-C43B = F44B-C44B = F45B-C45B = F46B-C46B
 1.37 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C39)
Uanis(B1A) = Uanis(B1B) = Uanis(C11A) = Uanis(C12A) = Uanis(C0AA) = Uanis(C1AA)
= Uanis(C15A) = Uanis(C16A) = Uanis(C24A) = Uanis(C23A) = Uanis(C22A) =
Uanis(C21A) = Uanis(C26A) = Uanis(C25A) = Uanis(C31A) = Uanis(C32A) =
Uanis(C33A) = Uanis(C34A) = Uanis(C35A) = Uanis(C36A) = Uanis(C41A) =
Uanis(C42A) = Uanis(C43A) = Uanis(C44A) = Uanis(C45A) = Uanis(C46A) =
Uanis(C11B) = Uanis(C12B) = Uanis(C13B) = Uanis(C14B) = Uanis(C15B) =
Uanis(C16B) = Uanis(C26B) = Uanis(C25B) = Uanis(C24B) = Uanis(C23B) =
Uanis(C22B) = Uanis(C21B) = Uanis(C31B) = Uanis(C36B) = Uanis(C35B) =
Uanis(C34B) = Uanis(C33B) = Uanis(C32B) = Uanis(C41B) = Uanis(C42B) =
Uanis(C43B) = Uanis(C44B) = Uanis(C45B) = Uanis(C46B)
Uanis(B2A) = Uanis(B2B) = Uanis(C51A) = Uanis(C52A) = Uanis(C53A) = Uanis(C54A)
= Uanis(C55A) = Uanis(C56A) = Uanis(C61A) = Uanis(C62A) = Uanis(C63A) =
Uanis(C64A) = Uanis(C65A) = Uanis(C66A) = Uanis(C71A) = Uanis(C72A) =
Uanis(C73A) = Uanis(C74A) = Uanis(C75A) = Uanis(C76A) = Uanis(C81A) =
Uanis(C82A) = Uanis(C83A) = Uanis(C84A) = Uanis(C85A) = Uanis(C86A) =
Uanis(C51B) = Uanis(C52B) = Uanis(C53B) = Uanis(C54B) = Uanis(C55B) =
Uanis(C56B) = Uanis(C61B) = Uanis(C62B) = Uanis(C63B) = Uanis(C64B) =
Uanis(C65B) = Uanis(C66B) = Uanis(C71B) = Uanis(C72B) = Uanis(C73B) =
Uanis(C74B) = Uanis(C75B) = Uanis(C76B) = Uanis(C81B) = Uanis(C82B) =
Uanis(C83B) = Uanis(C84B) = Uanis(C85B) = Uanis(C86B)
Uanis(F12A) = Uanis(F13A) = Uanis(F14A) = Uanis(F15A) = Uanis(F16A) =
Uanis(F22A) = Uanis(F23A) = Uanis(F24A) = Uanis(F25A) = Uanis(F26A) =
Uanis(F32A) = Uanis(F33A) = Uanis(F34A) = Uanis(F35A) = Uanis(F36A) =
Uanis(F42A) = Uanis(F43A) = Uanis(F44A) = Uanis(F45A) = Uanis(F46A) =
Uanis(F12B) = Uanis(F13B) = Uanis(F14B) = Uanis(F15B) = Uanis(F16B) =
Uanis(F22B) = Uanis(F23B) = Uanis(F24B) = Uanis(F25B) = Uanis(F26B) =
Uanis(F32B) = Uanis(F33B) = Uanis(F34B) = Uanis(F35B) = Uanis(F36B) =
Uanis(F42B) = Uanis(F43B) = Uanis(F44B) = Uanis(F45B) = Uanis(F46B)
Uanis(F52A) = Uanis(F53A) = Uanis(F54A) = Uanis(F55A) = Uanis(F56A) =
Uanis(F62A) = Uanis(F63A) = Uanis(F64A) = Uanis(F65A) = Uanis(F66A) =
Uanis(F72A) = Uanis(F73A) = Uanis(F74A) = Uanis(F75A) = Uanis(F76A) =
Uanis(F82A) = Uanis(F83A) = Uanis(F84A) = Uanis(F85A) = Uanis(F86A) =
Uanis(F52B) = Uanis(F53B) = Uanis(F54B) = Uanis(F55B) = Uanis(F56B) =
Uanis(F62B) = Uanis(F63B) = Uanis(F64B) = Uanis(F65B) = Uanis(F66B) =
Uanis(F72B) = Uanis(F73B) = Uanis(F74B) = Uanis(F75B) = Uanis(F76B) =
Uanis(F82B) = Uanis(F83B) = Uanis(F84B) = Uanis(F85B) = Uanis(F86B)
Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C52C) =
Uanis(C53C) = Uanis(C54C) = Uanis(C55C) = Uanis(C56C)
Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60) = Uanis(C61C) = Uanis(C62) =
Uanis(C63) = Uanis(C64) = Uanis(C65) = Uanis(C66) = Uanis(C67) = Uanis(C68) =
Uanis(C57C) = Uanis(C58C) = Uanis(C59C) = Uanis(C60C) = Uanis(C61) =
Uanis(C62C) = Uanis(C63C) = Uanis(C64C) = Uanis(C65C) = Uanis(C66C) =
Uanis(C67C) = Uanis(C68C)
5. Rigid body (RIGU) restrains
 Y1, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C15, C16, C17, C18,
 C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34,
  C13, C14, C13A, C14A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Y2, Y2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49,
 C50, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C52C)=Sof(H52C)=Sof(C53C)=Sof(C54C)=Sof(C55C)=Sof(C56C)=Sof(C57C)=
 Sof(H57C)=Sof(C58C)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59C)=Sof(H59D)=
 Sof(H59E)=Sof(H59F)=Sof(C60C)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=
 Sof(C62C)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C63C)=Sof(H63C)=Sof(C64C)=
 Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C65C)=Sof(H65D)=Sof(H65E)=Sof(H65F)=
 Sof(C66C)=Sof(H66C)=Sof(C67C)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C68C)=
 Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(1)
 Sof(C52)=Sof(H52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=Sof(H57)=
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=
 Sof(C60)=Sof(H60)=Sof(C61C)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62)=Sof(H62A)=
 Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(1)
 Sof(F12B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=Sof(F16B)=Sof(F22B)=Sof(F23B)=
 Sof(F24B)=Sof(F25B)=Sof(F26B)=Sof(F32B)=Sof(F33B)=Sof(F34B)=Sof(F35B)=
 Sof(F36B)=Sof(F42B)=Sof(F43B)=Sof(F44B)=Sof(F45B)=Sof(F46B)=Sof(C11B)=
 Sof(C12B)=Sof(C13B)=Sof(C14B)=Sof(C15B)=Sof(C16B)=Sof(C26B)=Sof(C25B)=
 Sof(C24B)=Sof(C23B)=Sof(C22B)=Sof(C21B)=Sof(C31B)=Sof(C36B)=Sof(C35B)=
 Sof(C34B)=Sof(C33B)=Sof(C32B)=Sof(C41B)=Sof(C42B)=Sof(C43B)=Sof(C44B)=
 Sof(C45B)=Sof(C46B)=Sof(B1B)=1-FVAR(2)
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F22A)=Sof(F23A)=
 Sof(F24A)=Sof(F25A)=Sof(F26A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=Sof(F35A)=
 Sof(F36A)=Sof(F42A)=Sof(F43A)=Sof(F44A)=Sof(F45A)=Sof(F46A)=Sof(C11A)=
 Sof(C12A)=Sof(C0AA)=Sof(C1AA)=Sof(C15A)=Sof(C16A)=Sof(C24A)=Sof(C23A)=
 Sof(C22A)=Sof(C21A)=Sof(C26A)=Sof(C25A)=Sof(C31A)=Sof(C32A)=Sof(C33A)=
 Sof(C34A)=Sof(C35A)=Sof(C36A)=Sof(C41A)=Sof(C42A)=Sof(C43A)=Sof(C44A)=
 Sof(C45A)=Sof(C46A)=Sof(B1A)=FVAR(2)
 Sof(F52B)=Sof(F53B)=Sof(F54B)=Sof(F55B)=Sof(F56B)=Sof(F62B)=Sof(F63B)=
 Sof(F64B)=Sof(F65B)=Sof(F66B)=Sof(F72B)=Sof(F73B)=Sof(F74B)=Sof(F75B)=
 Sof(F76B)=Sof(F82B)=Sof(F83B)=Sof(F84B)=Sof(F85B)=Sof(F86B)=Sof(C51B)=
 Sof(C52B)=Sof(C53B)=Sof(C54B)=Sof(C55B)=Sof(C56B)=Sof(C61B)=Sof(C62B)=
 Sof(C63B)=Sof(C64B)=Sof(C65B)=Sof(C66B)=Sof(C71B)=Sof(C72B)=Sof(C73B)=
 Sof(C74B)=Sof(C75B)=Sof(C76B)=Sof(C81B)=Sof(C82B)=Sof(C83B)=Sof(C84B)=
 Sof(C85B)=Sof(C86B)=Sof(B2B)=1-FVAR(3)
 Sof(F52A)=Sof(F53A)=Sof(F54A)=Sof(F55A)=Sof(F56A)=Sof(F62A)=Sof(F63A)=
 Sof(F64A)=Sof(F65A)=Sof(F66A)=Sof(F72A)=Sof(F73A)=Sof(F74A)=Sof(F75A)=
 Sof(F76A)=Sof(F82A)=Sof(F83A)=Sof(F84A)=Sof(F85A)=Sof(F86A)=Sof(C51A)=
 Sof(C52A)=Sof(C53A)=Sof(C54A)=Sof(C55A)=Sof(C56A)=Sof(C61A)=Sof(C62A)=
 Sof(C63A)=Sof(C64A)=Sof(C65A)=Sof(C66A)=Sof(C71A)=Sof(C72A)=Sof(C73A)=
 Sof(C74A)=Sof(C75A)=Sof(C76A)=Sof(C81A)=Sof(C82A)=Sof(C83A)=Sof(C84A)=
 Sof(C85A)=Sof(C86A)=Sof(B2A)=FVAR(3)
 Sof(Y2A)=1-FVAR(4)
 Sof(Y2)=FVAR(4)
 Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=1-FVAR(5)
 Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C12(H12), C12(H12A), C15(H15), C23(H23), C26(H26), C29(H29),
 C32(H32), C40(H40), C43(H43), C46(H46), C49(H49), C57(H57), C60(H60), C63(H63),
  C66(H66), C57C(H57C), C60C(H60C), C63C(H63C), C66C(H66C)
7.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C41(H41A,H41B,
 H41C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C61C(H61D,H61E,H61F), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C58C(H58D,H58E,H58F), C59C(H59D,H59E,H59F), C61(H61A,H61B,H61C), C62C(H62D,
 H62E,H62F), C64C(H64D,H64E,H64F), C65C(H65D,H65E,H65F), C67C(H67D,H67E,H67F),
 C68C(H68D,H68E,H68F)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C35(H35), C52(H52), C52C(H52C)
7.d Fitted pentagon refined as free rotating group:
 C52(C53,C54,C55,C56), C52C(C53C,C54C,C55C,C56C)
7.e Fitted hexagon refined as free rotating group:
 C11A(C12A,C0AA,C1AA,C15A,C16A), C24A(C23A,C22A,C21A,C26A,C25A), C31A(C32A,
 C33A,C34A,C35A,C36A), C41A(C42A,C43A,C44A,C45A,C46A), C51A(C52A,C53A,C54A,C55A,
 C56A), C61A(C62A,C63A,C64A,C65A,C66A), C71A(C72A,C73A,C74A,C75A,C76A),
 C81A(C82A,C83A,C84A,C85A,C86A), C11B(C12B,C13B,C14B,C15B,C16B), C26B(C25B,C24B,
 C23B,C22B,C21B), C31B(C36B,C35B,C34B,C33B,C32B), C51B(C52B,C53B,C54B,C55B,
 C56B), C61B(C62B,C63B,C64B,C65B,C66B), C71B(C72B,C73B,C74B,C75B,C76B),
 C81B(C82B,C83B,C84B,C85B,C86B)
7.f Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'