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_1550049
_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         'C34 H58 Dy, B C24 F20'
_chemical_formula_sum            'C58 H58 B Dy F20'
_chemical_formula_weight         1308.35
_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     direct
_audit_creation_date             2018-06-11
_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                 90.0586(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5863(17)
_cell_length_b                   14.4989(15)
_cell_length_c                   22.708(2)
_cell_measurement_reflns_used    9251
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.271
_cell_measurement_theta_min      2.456
_cell_volume                     5460.9(9)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.66
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.228
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0820 before and 0.0593 after correction. The Ratio of minimum to maximum transmission is 0.8433. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.044
_refine_diff_density_max         5.009
_refine_diff_density_min         -4.052
_refine_diff_density_rms         0.190
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         19909
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0779P)^2^+64.4005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                19061
_reflns_number_total             19909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k2.cif
_cod_data_source_block           tg_rm_6_31
_cod_depositor_comments
'Adding full bibliography for 1550047--1550050.cif.'
_cod_original_cell_volume        5461.0(9)
_cod_database_code               1550049
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.635
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.29(3)
 0.289(19) 0.212(19) 0.209(19)
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
 C41-C40 = C40-C42
 1.54 with sigma of 0.02
4. Rigid bond restraints
 C36, C37, C40, C41, C42, C43, C44, C45, C35, C39, C49, C51, C50, C38, C46,
 C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(B1) \\sim Ueq, Uanis(B2) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C41B) = Uanis(C42B) = Uanis(C43B) = Uanis(C44B) = Uanis(C45B) =
Uanis(C46B)
Uanis(C81B) = Uanis(C82B) = Uanis(C83B) = Uanis(C84B) = Uanis(C85B) =
Uanis(C86B)
Uanis(C61B) = Uanis(C62B) = Uanis(C63B) = Uanis(C64B) = Uanis(C65B) =
Uanis(C66B)
Uanis(C11B) = Uanis(C12B) = Uanis(C13B) = Uanis(C14B) = Uanis(C15B) =
Uanis(C16B)
Uanis(C21B) = Uanis(C22B) = Uanis(C23B) = Uanis(C24B) = Uanis(C25B) =
Uanis(C26B)
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(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(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5)
Uanis(C7) = Uanis(C8) = Uanis(C10) = Uanis(C11) = Uanis(C13) = Uanis(C14) =
Uanis(C16) = Uanis(C17)
Uanis(C27) = Uanis(C28) = Uanis(C30) = Uanis(C31) = Uanis(C33) = Uanis(C34) =
Uanis(C24) = Uanis(C25)
Uanis(C9) = Uanis(C12) = Uanis(C15) = Uanis(C6)
Uanis(C26) = Uanis(C29) = Uanis(C32) = Uanis(C23)
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22)
Uanis(C61) = Uanis(C62) = Uanis(C64) = Uanis(C65) = Uanis(C58) = Uanis(C59) =
Uanis(C67) = Uanis(C68)
Uanis(C63) = Uanis(C60) = Uanis(C57) = Uanis(C66)
Uanis(C49) = Uanis(C46) = Uanis(C43) = Uanis(C40)
Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56)
Uanis(C42) = Uanis(C41) = Uanis(C45) = Uanis(C44) = Uanis(C47) = Uanis(C48) =
Uanis(C51) = Uanis(C50)
Uanis(C51B) = Uanis(C52B) = Uanis(C53B) = Uanis(C54B) = Uanis(C55B) =
Uanis(C56B)
Uanis(C71B) = Uanis(C72B) = Uanis(C73B) = Uanis(C74B) = Uanis(C75B) =
Uanis(C76B)
6. Rigid body (RIGU) restrains
 C31B, C32B, C33B, C34B, C35B, C36B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C12(H12), 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)
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), 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), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), 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),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C35(H35), C52(H52)
7.d Fitted hexagon refined as free rotating group:
 C11B(C12B,C13B,C14B,C15B,C16B), C21B(C22B,C23B,C24B,C25B,C26B), C31B(C32B,
 C33B,C34B,C35B,C36B), C41B(C42B,C43B,C44B,C45B,C46B), C51B(C52B,C53B,C54B,C55B,
 C56B), C61B(C62B,C63B,C64B,C65B,C66B), C71B(C72B,C73B,C74B,C75B,C76B),
 C81B(C82B,C83B,C84B,C85B,C86B)
;
_shelx_res_checksum              31827
_olex2_submission_special_instructions 'No special instructions were received'