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_4349626
_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         'C48 H38 F12 O14 S4 Y2'
_chemical_formula_sum            'C48 H38 F12 O14 S4 Y2'
_chemical_formula_weight         1372.84
_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             2015-03-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2015-07-15 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                71.071(8)
_cell_angle_beta                 76.611(7)
_cell_angle_gamma                67.152(7)
_cell_formula_units_Z            1
_cell_length_a                   10.9144(7)
_cell_length_b                   11.0520(9)
_cell_length_c                   13.0251(12)
_cell_measurement_reflns_used    2806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1503
_cell_measurement_theta_min      2.9729
_cell_volume                     1359.5(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details
;
  1 omega   24.00   50.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   57.0000  -90.0000 26

  2 omega  -17.00   22.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -99.0000   30.0000 39

  3 omega  -41.00   36.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   57.0000   30.0000 77

  4 omega  -21.00   17.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -99.0000  -90.0000 38

  5 omega  -64.00  -38.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  178.0000 -120.0000 26

  6 omega  -44.00   47.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   38.0000  -90.0000 91

  7 omega  -88.00   -2.00   1.0000   10.0600
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -57.0000  120.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0061900000
_diffrn_orient_matrix_UB_12      0.0304338000
_diffrn_orient_matrix_UB_13      0.0420910000
_diffrn_orient_matrix_UB_21      0.0527188000
_diffrn_orient_matrix_UB_22      -0.0574879000
_diffrn_orient_matrix_UB_23      0.0240139000
_diffrn_orient_matrix_UB_31      0.0472190000
_diffrn_orient_matrix_UB_32      0.0312281000
_diffrn_orient_matrix_UB_33      -0.0318644000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10797
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82708
_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    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_refine_diff_density_max         1.486
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+2.8272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                4673
_reflns_number_total             6189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j3.cif
_cod_data_source_block           1
_cod_original_cell_volume        1359.50(19)
_cod_database_code               4349626
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B} of C1, H3 of C3, H15 of C15, H16 of C16, H19 of C19, H24 of C24,
  H11 of C11, {H22A,H22B} of C22, H4 of C4, H5 of C5, H23 of C23
 At 1.5 times of:
  {H9A,H9B,H9C} of C9, {H6A,H6B,H6C} of C6
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C23(H23), C5(H5), C4(H4), C11(H11), C24(H24), C19(H19), C16(H16),
 C15(H15)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;