Exchange-bias quantum tunnelling in a CO2-based Dy4-single molecule magnet.
Pineda, Eufemio Moreno; Lan, Yanhua; Fuhr, Olaf; Wernsdorfer, Wolfgang; Ruben, Mario; Chemical science 8 (2017) 1178–1185; doi:10.1039/c6sc03184f

data_1544182
_publ_section_title
;
 Exchange-bias quantum tunnelling in a CO2-based Dy4-single molecule
 magnet.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              1178
_journal_page_last               1185
_journal_paper_doi               10.1039/c6sc03184f
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C84 H168 Dy4 N12 O24, 3(C7 H8)'
_chemical_formula_sum            'C105 H192 Dy4 N12 O24'
_chemical_formula_weight         2656.69
_chemical_properties_physical    ', Moisture-sensitive'
_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
_audit_creation_date             2015-12-24
_audit_creation_method
;
Olex2 1.2
(compiled Sep 16 2015 11:44:03 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-06-07 deposited with the CCDC.
2016-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.985(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.1117(11)
_cell_length_b                   20.1279(6)
_cell_length_c                   22.8674(10)
_cell_measurement_reflns_used    59399
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.23
_cell_volume                     12438.7(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41630
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.782
_diffrn_reflns_theta_min         2.226
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_T_max  0.7085
_exptl_absorpt_correction_T_min  0.4286
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             5448
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.855
_refine_diff_density_min         -3.850
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         11718
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1490P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8356
_reflns_number_total             11718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc03184f2.cif
_cod_data_source_block           Dy4
_cod_depositor_comments
;Adding full bibliography for 1544182.cif.

 Adding full bibliography for 1544182.cif.
;
_cod_database_code               1544182
_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
 C14S, C9S, C8S, C11S, C10S, C13S, C12S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C8S(0.5) H8SA(0.5) H8SB(0.5) H8SC(0.5) C9S(0.5) C14S(0.5)
 H14S(0.5) C13S(0.5) H13S(0.5) C12S(0.5) H12S(0.5) C11S(0.5) H11S(0.5)
 C10S(0.5) H10S(0.5)
4.a Ternary CH refined with riding coordinates:
 C37(H37), C23(H23), C33(H33), C40(H40), C2(H2), C16(H16), C26(H26), C19(H19),
 C12(H12), C5(H5), C30(H30), C9(H9)
4.b Aromatic/amide H refined with riding coordinates:
 C6S(H6S), C3S(H3S), C4S(H4S), C7S(H7S), C5S(H5S), C14S(H14S), C13S(H13S),
 C12S(H12S), C11S(H11S), C10S(H10S)
4.c Fitted hexagon refined as free rotating group:
 C9S(C14S,C13S,C12S,C11S,C10S)
4.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C39(H39A,H39B,H39C), C18(H18A,H18B,H18C), C35(H35A,H35B,
 H35C), C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C34(H34A,
 H34B,H34C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C),
 C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
  C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C42(H42A,H42B,H42C),
  C31(H31A,H31B,H31C), C1S(H1SA,H1SB,H1SC), C8S(H8SA,H8SB,H8SC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method Toluene