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_4349633
_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         'C56 H42 Dy2 F12 O14'
_chemical_formula_sum            'C56 H42 Dy2 F12 O14'
_chemical_formula_weight         1491.90
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2015-07-09 deposited with the CCDC.
2016-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                113.112(6)
_cell_angle_beta                 105.241(5)
_cell_angle_gamma                99.434(5)
_cell_formula_units_Z            1
_cell_length_a                   9.7688(6)
_cell_length_b                   12.7894(8)
_cell_length_c                   13.0685(8)
_cell_measurement_reflns_used    4801
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2099
_cell_measurement_theta_min      2.8616
_cell_volume                     1381.69(18)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_details
;
  1 omega  -14.00   14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8540  -99.0000  -30.0000 28

  2 omega  -44.00   51.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   38.0000 -120.0000 95

  3 omega  -44.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   38.0000  120.0000 73

  4 omega  -23.00    6.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -99.0000 -120.0000 29

  5 omega  -17.00   23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -99.0000   90.0000 40

  6 omega  -89.00    9.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -77.0000  -30.0000 98

  7 omega   12.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   57.0000  120.0000 35
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0407155000
_diffrn_orient_matrix_UB_12      0.0377330000
_diffrn_orient_matrix_UB_13      0.0246504000
_diffrn_orient_matrix_UB_21      -0.0281635000
_diffrn_orient_matrix_UB_22      -0.0401317000
_diffrn_orient_matrix_UB_23      0.0199169000
_diffrn_orient_matrix_UB_31      0.0614549000
_diffrn_orient_matrix_UB_32      0.0310467000
_diffrn_orient_matrix_UB_33      0.0547601000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11173
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47330
_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_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             730
_refine_diff_density_max         3.504
_refine_diff_density_min         -2.948
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0943P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                5387
_reflns_number_total             6347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1381.69(14)
_cod_database_code               4349633
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H28 of C28, H3 of C3, H11 of C11, H5 of C5, H14 of C14, H26 of C26, H24 of
  C24, H18 of C18, H4 of C4, H25 of C25, H17 of C17, H21 of C21, H16 of C16,
  H15 of C15, H27 of C27
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H8A,H8B,H8C} of C8
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C3(H3), C11(H11), C5(H5), C14(H14), C26(H26), C24(H24), C18(H18),
 C4(H4), C25(H25), C21(H21), C16(H16), C15(H15), C17(H17), C27(H27)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;