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_1550047
_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         'C40 H70 Dy1, B C24 F20'
_chemical_formula_sum            'C64 H70 B Dy F20'
_chemical_formula_weight         1392.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-09-03 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2173(4)
_cell_length_b                   22.8792(6)
_cell_length_c                   16.8807(5)
_cell_measurement_reflns_used    1382
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.027
_cell_measurement_theta_min      2.284
_cell_volume                     5876.9(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       APEX3
_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      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47155
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        21.594
_diffrn_reflns_theta_max         21.594
_diffrn_reflns_theta_min         0.913
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.462
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1076 before and 0.0646 after correction. The Ratio of minimum to maximum transmission is 0.9211. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.761
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         6341
_refine_ls_number_restraints     693
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0839P)^2^+28.9381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5565
_reflns_number_total             6341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k2.cif
_cod_data_source_block           cg045sc
_cod_depositor_comments
'Adding full bibliography for 1550047--1550050.cif.'
_cod_database_code               1550047
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9918(6)
 0.0082(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C7-C6 = C8-C6 = C7A-C6A = C8A-C6A = C9-C11 = C9A-C11A = C9A-C10A = C9-C10 =
 C13-C12 = C13A-C12A = C14A-C12A = C14-C12 = C16-C15 = C17-C15 = C16A-C15A =
 C17A-C15A = C19-C18 = C20-C18 = C19A-C18A = C20A-C18A
 1.54 with sigma of 0.02
 C30-C29 = C30A-C29A = C31-C29 = C31A-C29A = C33A-C32A = C34A-C32A = C34-C32 =
 C33-C32 = C27-C26 = C27A-C26A = C28-C26 = C28A-C26A = C39-C38A = C40A-C38A =
 C40-C38 = C37A-C35A = C35A-C36A = C37-C35 = C36-C35 = C38-C39 = C38A-C39A
 1.54 with sigma of 0.02
 C7-C8 = C7A-C8A = C10-C11 = C10A-C11A = C13-C14 = C13A-C14A = C16-C17 = C16A-
 C17A = C19-C20 = C19A-C20A = C27-C28 = C27A-C28A = C30-C31 = C30A-C31A = C33-
 C34 = C33A-C34A = C36-C37 = C36A-C37A = C39A-C40 = C39A-C40A
 2.5 with sigma of 0.04
 C2-C6 = C2-C6A = C5-C6 = C5-C6A = C1-C9 = C1-C9A = C3-C9 = C3-C9A = C3-C15 =
 C3-C15A = C5-C15 = C5-C15A = C1-C18 = C1-C18A = C4-C18 = C4-C18A
 2.5 with sigma of 0.04
 C22-C26 = C22-C26A = C25-C26 = C25-C26A = C21-C29 = C21-C29A = C23-C29 = C23-
 C29A = C22-C32 = C22-C32A = C24-C32 = C24-C32A = C23-C35 = C23-C35A = C25-C35 =
  C25-C35A = C21-C38 = C21-C38A = C24-C38 = C24-C38A
 2.5 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Dy1 \\sim Dy2 \\sim Dy3 \\sim Dy4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C21, C22, C23, C24, C25, C6, C7, C8, C9, C10, C11, C12,
 C13, C14, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C22, C23, C24, C25, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A,
  C35A, C36A, C37A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C2, C3, C4, C5, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A,
 C16A, C17A, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C22, C23, C24, C25, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16,
 C17, C18, C19, C20, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37,
  C38, C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 1*[Sof(Dy1)]+1*[Sof(Dy2)]+1*[Sof(Dy3)]+1*[Sof(Dy4)]=1 with esd of 0.0001
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=
 Sof(H8AB)=Sof(H8AC)=1-FVAR(1)
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(1)
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=FVAR(2)
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=FVAR(3)
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(4)
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(4)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(5)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=FVAR(5)
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(6)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(6)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(7)
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(7)
 Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(8)
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=FVAR(8)
7.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C12(H12), C15(H15), C18(H18), C26(H26), C29(H29), C32(H32),
 C35(H35), C38(H38), C6A(H6A), C9A(H9A), C12A(H12A), C15A(H15A), C18A(H18A),
 C26A(H26A), C29A(H29A), C32A(H32A), C35A(H35A), C38A(H38A)
7.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC),
 C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F), C14A(H14D,
 H14E,H14F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C19A(H19D,H19E,H19F),
 C20A(H20D,H20E,H20F), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C30A(H30D,
 H30E,H30F), C31A(H31D,H31E,H31F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F),
 C36A(H36D,H36E,H36F), C37A(H37D,H37E,H37F), C39A(H39D,H39E,H39F), C40A(H40D,
 H40E,H40F)
;
_olex2_submission_special_instructions 'No special instructions were received'