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_1552913
_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         'C38 H66 Y, B C24 F20'
_chemical_formula_sum            'C62 H66 B F20 Y'
_chemical_formula_weight         1290.86
_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             2018-06-27
_audit_creation_method
; 
Olex2 1.2 
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) 
;
_audit_update_record
;
2018-10-17 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0163(5)
_cell_length_b                   23.1163(8)
_cell_length_c                   16.7813(6)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.712
_cell_measurement_theta_min      2.224
_cell_volume                     5824.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0245
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43460
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        21.036
_diffrn_reflns_theta_max         21.036
_diffrn_reflns_theta_min         1.500
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0608 before and 0.0437 after correction. 
The Ratio of minimum to maximum transmission is 0.9128. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.492
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0822P)^2^+16.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5070
_reflns_number_total             6283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k3.cif
_cod_data_source_block           tg_rm_7_56_1_0m
_cod_database_code               1552913
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.9705
_shelx_estimated_absorpt_t_min   0.8859
_olex2_refinement_description
;
1. 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 
2. Rigid bond restraints 
 C41B, C46B, C45B, C44B, C43B, C42B, F46B, F45B, F44B, F43B, F42B 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 
3. Rigid body (RIGU) restrains 
 C27, C28, C29, C29A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 C10, C8, C9 
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 
4. Others 
 Sof(H27A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1) 
 Sof(H27)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1) 
5.a Ternary CH refined with riding coordinates: 
 C8(H8), C11(H11), C14(H14), C17(H17), C27(H27), C27(H27A), C30(H30), C33(H33), 
  C36(H36) 
5.b Secondary CH2 refined with riding coordinates: 
 C6(H6A,H6B), C25(H25A,H25B) 
5.c Me refined with riding coordinates: 
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), 
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C28(H28A,H28B, 
 H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A, 
 H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C29(H29A,H29B,H29C), 
 C29A(H29D,H29E,H29F) 
5.d Idealised Me refined as rotating group: 
 C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C) 
;
_shelx_res_checksum              89049
_olex2_submission_special_instructions 'No special instructions were received'