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_1552912
_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 Y, B C24 F20'
_chemical_formula_sum            'C64 H70 B F20 Y'
_chemical_formula_weight         1318.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 106.0490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.336(2)
_cell_length_b                   11.5772(10)
_cell_length_c                   19.4333(17)
_cell_measurement_reflns_used    8212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.30
_cell_volume                     5910.4(8)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 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 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33243
_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         25.349
_diffrn_reflns_theta_min         1.550
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0518 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9501. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+12.6660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4102
_reflns_number_total             5416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k3.cif
_cod_data_source_block           tg_rm_6_15_1_0m
_cod_original_cell_volume        5910.4(9)
_cod_database_code               1552912
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C11A, C12A, C13A, C14A, C15A, C16A, C21A, C22A, C23A, C24A, C25A, C26A, F12A,
 F13A, F14A, F15A, F16A, F22A, F23A, F24A, F25A, F26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11B, C12B, C13B, C14B, C15B, C16B, C21B, C22B, C23B, C24B, C25B, C26B, F12B,
 F13B, F14B, F15B, F16B, F22B, F23B, F24B, F25B, F26B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F12B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=Sof(F16B)=Sof(F22B)=Sof(F23B)=
 Sof(F24B)=Sof(F25B)=Sof(F26B)=Sof(C11B)=Sof(C12B)=Sof(C13B)=Sof(C14B)=
 Sof(C15B)=Sof(C16B)=Sof(C21B)=Sof(C22B)=Sof(C23B)=Sof(C24B)=Sof(C25B)=
 Sof(C26B)=1-FVAR(1)
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F22A)=Sof(F23A)=
 Sof(F24A)=Sof(F25A)=Sof(F26A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(C16A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=
 Sof(C26A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C12(H12), C15(H15), C18(H18)
4.b Idealised Me refined as rotating group:
 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)
;
_olex2_submission_special_instructions 'No special instructions were received'