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_1550885
_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                91.995(2)
_cell_angle_beta                 93.347(2)
_cell_angle_gamma                107.530(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8671(2)
_cell_length_b                   13.8736(3)
_cell_length_c                   14.8582(3)
_cell_measurement_reflns_used    20815
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.0580
_cell_measurement_theta_min      2.0120
_cell_volume                     2129.20(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 0.993
_diffrn_measured_fraction_theta_max 0.994
_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 -- 0.00 180.00 250.00 180 2 \w -10.00 90.00 1.00 180.60 -- 0.00 180.00 64.00 100'
_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      -0.0350774000
_diffrn_orient_matrix_UB_12      -0.0473788000
_diffrn_orient_matrix_UB_13      -0.0219213000
_diffrn_orient_matrix_UB_21      -0.0182383000
_diffrn_orient_matrix_UB_22      0.0252296000
_diffrn_orient_matrix_UB_23      -0.0367919000
_diffrn_orient_matrix_UB_31      0.0560970000
_diffrn_orient_matrix_UB_32      -0.0014560000
_diffrn_orient_matrix_UB_33      -0.0214353000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_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            24512
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.970
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (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    1.305
_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          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8663
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0241
_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^)+(0.0326P)^2^+2.5740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8201
_reflns_number_total             8663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01062a2.cif
_cod_data_source_block           em1-119
_cod_database_code               1550885
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C76H125Dy2N4O13
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.800
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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
 C1S-O0AA = C1S-C2S
 1.54 with sigma of 0.02
 O0AA-C1S
 1.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O0AA) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(C2A) = Uanis(C1A) = Uanis(C3A)
4. Rigid body (RIGU) restrains
 C3A, C4A, C1A, C2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C1S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6D)=Sof(H6E)=Sof(H6F)=
 Sof(C9CA)=Sof(H9CD)=Sof(H9CE)=Sof(H9CF)=1-FVAR(1)
 Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=Sof(C10C)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=Sof(C11C)=Sof(H11G)=Sof(H11H)=Sof(H11I)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6A(H6A), C6B(H6B), C6C(H6C)
6.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C2A(H2AA,H2AB,
 H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,
 H3BB,H3BC), C3C(H3CA,H3CB,H3CC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC),
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C11A(H11A,H11B,H11C), C11B(H11D,
 H11E,H11F), C9C(H9CA,H9CB,H9CC), C10C(H10G,H10H,H10I), C11C(H11G,H11H,H11I),
 C5(H5A,H5B,H5C), C6(H6D,H6E,H6F), C9CA(H9CD,H9CE,H9CF), C2S(H2SA,H2SB,H2SC)
;
_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 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.848