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_1550050
_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         '1(C36 H62 Dy), B C24 F20'
_chemical_formula_sum            'C60 H62 B Dy F20'
_chemical_formula_weight         1336.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-25
_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                 90.027(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.50(2)
_cell_length_b                   16.63(3)
_cell_length_c                   46.59(8)
_cell_measurement_reflns_used    675
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10.424
_cell_measurement_theta_min      2.511
_cell_volume                     11234(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 0.999
_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  0.1408
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            163480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         0.896
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1325 before and 0.1020 after correction. 
The Ratio of minimum to maximum transmission is 0.8925. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5384
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.562
_refine_diff_density_min         -3.785
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         20570
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0605P)^2^+47.0657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16474
_reflns_number_total             20570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03907k2.cif
_cod_data_source_block           cg042sa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1550047--1550050.cif.
;
_cod_original_cell_volume        11236(33)
_cod_database_code               1550050
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.854
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8197(7)
 0.1803(7)
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
 C65A-C66A
 2.54 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C65) = Uanis(C59) = Uanis(C55) = Uanis(C57) = Uanis(C69) = Uanis(C58) =
Uanis(C63) = Uanis(C70) = Uanis(C66) = Uanis(C56) = Uanis(C60) = Uanis(C68) =
Uanis(C67) = Uanis(C64) = Uanis(C72) = Uanis(C61) = Uanis(C71) = Uanis(C62)
Uanis(C65A) = Uanis(C70A) = Uanis(C61A) = Uanis(C67A) = Uanis(C60A) =
Uanis(C64A) = Uanis(C56A) = Uanis(C59A) = Uanis(C58A) = Uanis(C55A) =
Uanis(C57A) = Uanis(C68A) = Uanis(C71A) = Uanis(C66A) = Uanis(C72A) =
Uanis(C69A) = Uanis(C62A) = Uanis(C63A)
Uanis(C19A) = Uanis(C28A) = Uanis(C25A) = Uanis(C31A) = Uanis(C24A) =
Uanis(C34A) = Uanis(C21A) = Uanis(C22A) = Uanis(C23A) = Uanis(C20A) =
Uanis(C35A) = Uanis(C36A) = Uanis(C29A) = Uanis(C32A) = Uanis(C26A) =
Uanis(C33A) = Uanis(C30A) = Uanis(C27A)
Uanis(C19) = Uanis(C32) = Uanis(C22) = Uanis(C35) = Uanis(C29) = Uanis(C23) =
Uanis(C21) = Uanis(C36) = Uanis(C24) = Uanis(C33) = Uanis(C30) = Uanis(C26) =
Uanis(C25) = Uanis(C28) = Uanis(C31) = Uanis(C34) = Uanis(C20) = Uanis(C27)
5. Others
 Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28A)=
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34A)=Sof(C35A)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=
 Sof(H34)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
 Sof(C55A)=Sof(C56A)=Sof(C57A)=Sof(C58A)=Sof(C59A)=Sof(C60A)=Sof(H60D)=
 Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C66A)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=
 Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70A)=Sof(C71A)=
 Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(2)
 Sof(C55)=Sof(C56)=Sof(C57)=Sof(C58)=Sof(C59)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67)=Sof(C68)=
 Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=
 Sof(H70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)=
 Sof(H72C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C16(H16), C25(H25), C28(H28), C31(H31), C34(H34),
 C25A(H25A), C28A(H28A), C31A(H31A), C34A(H34A), C43(H43), C46(H46), C49(H49),
 C52(H52), C61(H61), C64(H64), C67(H67), C70(H70), C61A(H61A), C64A(H64A),
 C67A(H67A), C70A(H70A)
6.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F),
 C27A(H27D,H27E,H27F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C32A(H32D,
 H32E,H32F), C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F),
 C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C60A(H60D,H60E,H60F), C62A(H62D,H62E,H62F),
 C63A(H63D,H63E,H63F), C65A(H65D,H65E,H65F), C66A(H66D,H66E,H66F), C68A(H68D,
 H68E,H68F), C69A(H69D,H69E,H69F), C71A(H71D,H71E,H71F), C72A(H72D,H72E,H72F)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), 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), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              54128
_olex2_submission_special_instructions 'No special instructions were received'