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_4349627
_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         'C72 H50 F12 O14 Tb2'
_chemical_formula_sum            'C72 H50 F12 O14 Tb2'
_chemical_formula_weight         1684.96
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-17
_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                90.00
_cell_angle_beta                 105.300(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.2874(7)
_cell_length_b                   14.2711(4)
_cell_length_c                   18.5381(6)
_cell_measurement_reflns_used    7964
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8845
_cell_measurement_theta_min      3.1071
_cell_volume                     6708.1(4)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_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 0.892
_diffrn_measurement_details
;
  1 omega  -49.00  -23.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6390  -77.0000 -150.0000 26

  2 omega   -3.00   28.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6390   57.0000  -30.0000 31

  3 omega   15.00   41.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       20.6390  -77.0000 -150.0000 26

  4 omega  -27.00   49.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890   57.0000 -150.0000 76

  5 omega  -25.00   23.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890  -99.0000  120.0000 48

  6 omega  -73.00  -37.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890 -178.0000   30.0000 36

  7 omega  -91.00    2.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890  -57.0000  -60.0000 93

  8 omega  -46.00   47.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.8890   57.0000   90.0000 93
;
_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      0.0071354000
_diffrn_orient_matrix_UB_12      -0.0466003000
_diffrn_orient_matrix_UB_13      -0.0063502000
_diffrn_orient_matrix_UB_21      -0.0222477000
_diffrn_orient_matrix_UB_22      -0.0170342000
_diffrn_orient_matrix_UB_23      0.0108434000
_diffrn_orient_matrix_UB_31      -0.0153773000
_diffrn_orient_matrix_UB_32      0.0029621000
_diffrn_orient_matrix_UB_33      -0.0376199000
_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     0.71000
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26117
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         3.11
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91345
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0480P)^2^+23.3160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                5657
_reflns_number_total             7929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j4.cif
_cod_data_source_block           thr138-4
_cod_original_cell_volume        6708.1(3)
_cod_database_code               4349627
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C6-H6AB
 1.7 with sigma of 0.02
3. Others
 Sof(C5A)=Sof(H5A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C1A)=Sof(H1A)=
 Sof(C0BB)=Sof(C4A)=Sof(C1BB)=Sof(H1BB)=Sof(C7AB)=Sof(C6AB)=Sof(H6AB)=Sof(C9AB)=
 Sof(H9AB)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C6)=Sof(H6)=Sof(C5)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C30(H30), C24(H24), C31(H31), C15(H15), C32(H32),
 C29(H29), C25(H25), C27(H27), C34(H34), C21(H21), C2(H2), C6(H6), C3(H3),
 C7(H7), C8(H8), C10(H10), C9(H9), C5A(H5A), C2A(H2A), C3A(H3A), C1A(H1A),
 C1BB(H1BB), C9AB(H9AB)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'