Complementation and joint contribution of appropriate intramolecular coupling and local ion symmetry to improve magnetic relaxation in a series of dinuclear Dy2 single-molecule magnets
Tu, Hao-Ran; Sun, Wen-Bin; Li, Hong-Feng; Chen, Peng; Tian, Yong-Mei; Zhang, Wan-Ying; Zhang, Yi-Quan; Yan, Peng-Fei; Inorganic Chemistry Frontiers 4 (2017) 499–; doi:10.1039/C6QI00508J

data_4349630
_publ_section_title
;
 Complementation and joint contribution of appropriate intramolecular
 coupling and local ion symmetry to improve magnetic relaxation in a
 series of dinuclear Dy2 single-molecule magnets
;
_journal_issue                   3
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              499
_journal_paper_doi               10.1039/C6QI00508J
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C74 H58 F12 O16 Tb2, 2(O)'
_chemical_formula_sum            'C74 H58 F12 O18 Tb2'
_chemical_formula_weight         1781.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                65.286(4)
_cell_angle_beta                 78.174(4)
_cell_angle_gamma                68.383(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4870(5)
_cell_length_b                   14.2174(7)
_cell_length_c                   14.5235(7)
_cell_measurement_reflns_used    7150
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.5199
_cell_measurement_theta_min      3.0875
_cell_volume                     1825.41(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -1.00   52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4268  -57.0000   30.0000 53

  2 omega  -35.00    1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -57.0000  150.0000 36

  3 omega -100.00  -16.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -38.0000  120.0000 84

  4 omega  -19.00   11.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -99.0000  -30.0000 30

  5 omega  -43.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768   38.0000  -60.0000 82

  6 omega  -55.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768   57.0000   30.0000 101

  7 omega  -20.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -99.0000   90.0000 43

  8 omega  -24.00    2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -99.0000  -90.0000 26
;
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       'omega rotation'
_diffrn_orient_matrix_UB_11      -0.0398483000
_diffrn_orient_matrix_UB_12      0.0560167000
_diffrn_orient_matrix_UB_13      -0.0153068000
_diffrn_orient_matrix_UB_21      0.0170912000
_diffrn_orient_matrix_UB_22      0.0063055000
_diffrn_orient_matrix_UB_23      -0.0516368000
_diffrn_orient_matrix_UB_31      -0.0585856000
_diffrn_orient_matrix_UB_32      -0.0133431000
_diffrn_orient_matrix_UB_33      -0.0006142000
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13362
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.09
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7443
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+2.1715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                6484
_reflns_number_total             7443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j4.cif
_cod_data_source_block           thr138-3
_cod_original_cell_volume        1825.41(15)
_cod_database_code               4349630
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C00X-H8
 1.847356 with sigma of 0.02
 Tb1-H8
 2.880939 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C0AA)=Sof(H0AA)=Sof(C01I)=Sof(H01I)=Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=
 Sof(H2AA)=Sof(C30)=Sof(C29)=Sof(H29)=Sof(C28)=Sof(H28)=Sof(C27)=Sof(C32)=
 Sof(H32)=Sof(C31)=1-FVAR(1)
 Sof(C00Z)=Sof(C010)=Sof(C015)=Sof(H015)=Sof(C37)=Sof(C36)=Sof(H36)=Sof(C01D)=
 Sof(H01D)=Sof(C01E)=Sof(H01E)=Sof(C33)=Sof(H33)=Sof(C35)=Sof(H35)=Sof(C34)=
 Sof(H34)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C19(H19), C9(H9), C18(H18), C25(H25), C6(H6), C015(H015),
 C14(H14), C7(H7), C13(H13), C11(H11), C12(H12), C36(H36), C01D(H01D),
 C01E(H01E), C33(H33), C35(H35), C34(H34), C0AA(H0AA), C01I(H01I), C1AA(H1AA),
 C2AA(H2AA), C29(H29), C28(H28), C32(H32)
5.b Idealised Me refined as rotating group:
 C00X(H00a,H00b,H00c), C15(H15a,H15b,H15c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'