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_1550048
_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 Dy, B C24 F20'
_chemical_formula_sum            'C62 H66 B Dy F20'
_chemical_formula_weight         1364.45
_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             2018-05-07
_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                 90.789(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9801(4)
_cell_length_b                   23.0586(7)
_cell_length_c                   16.7069(5)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.892
_cell_measurement_theta_min      2.501
_cell_volume                     5770.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker 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
_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 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  0.0868
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.880
_diffrn_reflns_theta_max         23.880
_diffrn_reflns_theta_min         1.544
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.9067.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.884
_refine_diff_density_min         -2.414
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0623P)^2^+40.8794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6586
_reflns_number_total             8291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k2.cif
_cod_data_source_block           cg046s
_cod_depositor_comments
'Adding full bibliography for 1550047--1550050.cif.'
_cod_database_code               1550048
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.830
_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
 C10, C8, C9, C36, C37, C38A, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(H36A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(1)
 Sof(H36)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C27(H27), C30(H30), C33(H33), C36(H36),
 C36(H36A)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C25(H25A,H25B)
4.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C38A(H38D,H38E,
 H38F)
;
_shelx_res_checksum              60800
_olex2_submission_special_instructions 'No special instructions were received'