Quantum Tunnelling of the Magnetisation in Single-Molecule Magnet Isotopologue Dimers
Moreno-Pineda, Eufemio; Taran, Gheorghe; Wernsdorfer, Wolfgang; Ruben, Mario; Chemical Science  (2019) –; doi:10.1039/C9SC01062A

data_1550884
_publ_section_title
;
 Quantum Tunnelling of the Magnetisation in Single-Molecule Magnet
 Isotopologue Dimers
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01062A
_journal_year                    2019
_chemical_formula_moiety         'C74 H120 Dy2 N4 O12, C4 H10 O2'
_chemical_formula_sum            'C78 H130 Dy2 N4 O14'
_chemical_formula_weight         1672.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-02-20 deposited with the CCDC.    2019-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.039(2)
_cell_angle_beta                 93.333(2)
_cell_angle_gamma                107.553(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8743(2)
_cell_length_b                   13.8790(3)
_cell_length_c                   14.8618(4)
_cell_measurement_reflns_used    21010
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.2550
_cell_measurement_theta_min      1.9900
_cell_volume                     2131.63(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -90.00 90.00 1.00 180.60 -- 0.00 180.00 252.00 180 2 \w -90.00 20.00 1.00 180.60 -- 0.00 180.00 64.00 110'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0032390000
_diffrn_orient_matrix_UB_12      -0.0277168000
_diffrn_orient_matrix_UB_13      0.0394425000
_diffrn_orient_matrix_UB_21      0.0507811000
_diffrn_orient_matrix_UB_22      -0.0180126000
_diffrn_orient_matrix_UB_23      -0.0139204000
_diffrn_orient_matrix_UB_31      0.0459961000
_diffrn_orient_matrix_UB_32      0.0423019000
_diffrn_orient_matrix_UB_33      0.0233063000
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25289
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         4.080
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             870
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane and ethanol'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8697
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0297P)^2^+2.3589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8350
_reflns_number_total             8697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01062a2.cif
_cod_data_source_block           em1-118
_cod_database_code               1550884
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Dy2 N4 O12 C30'
_reflns_odcompleteness_completeness 86.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.43
_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. Restrained distances
 C1AA-C5
 1.54 with sigma of 0.02
 C5-O0AA
 1.1 with sigma of 0.02
 C2C-C4C \\sim C4C-C3C \\sim C3C-C4C \\sim C4C-C1C \\sim C1C-C4C \\sim C4C-C2C
 with sigma of 0.02
 C2C-C3C \\sim C3C-C1C \\sim C3C-C1C \\sim C1C-C2C \\sim C1C-C2C \\sim C2C-C3C
 with sigma of 0.02
 C2CA-C4C \\sim C4C-C3CA \\sim C3CA-C4C \\sim C4C-C1CA \\sim C1CA-C4C \\sim
C4C-C2CA
 with sigma of 0.02
 C2CA-C3CA \\sim C3CA-C1CA \\sim C3CA-C1CA \\sim C1CA-C2CA \\sim C1CA-C2CA
\\sim C2CA-C3CA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1CA) = Uanis(C2CA) = Uanis(C3CA)
Uanis(C9B) = Uanis(C11B) = Uanis(C10B)
4. Rigid body (RIGU) restrains
 C1C, C1CA, C2C, C3C, C3CA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C1AA, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11B, C9B, C10B, C8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1CA)=Sof(H1CD)=Sof(H1CE)=Sof(H1CF)=Sof(C2CA)=Sof(H2CD)=Sof(H2CE)=
 Sof(H2CF)=Sof(C3CA)=Sof(H3CD)=Sof(H3CE)=Sof(H3CF)=1-FVAR(1)
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(H2CC)=
 Sof(C3C)=Sof(H3CA)=Sof(H3CB)=Sof(H3CC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
6.b Me refined with riding coordinates:
 C1AA(H1AD,H1AE,H1AF)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6A(H6A), C6B(H6B), C6C(H6C)
6.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1CA(H1CD,H1CE,
 H1CF), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC),
 C2CA(H2CD,H2CE,H2CF), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C3C(H3CA,H3CB,
 H3CC), C3CA(H3CD,H3CE,H3CF), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC),
 C9C(H9CA,H9CB,H9CC), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G,
 H10H,H10I), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11C(H11G,H11H,H11I)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling'
_oxdiff_exptl_absorpt_empirical_full_max 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.873