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_4349625
_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 Gd2 O14 S4'
_chemical_formula_sum            'C48 H38 F12 Gd2 O14 S4'
_chemical_formula_weight         1509.52
_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             2016-12-6
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2016-12-06 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                71.247(4)
_cell_angle_beta                 76.901(4)
_cell_angle_gamma                67.048(5)
_cell_formula_units_Z            1
_cell_length_a                   10.9212(6)
_cell_length_b                   11.0906(6)
_cell_length_c                   13.0365(5)
_cell_measurement_reflns_used    5143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0966
_cell_measurement_theta_min      2.9623
_cell_volume                     1367.50(13)
_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 0.983
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details
;
  1 omega   35.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277  178.0000 -180.0000 61

  2 omega    9.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277  -99.0000    0.0000 50

  3 omega  -85.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215  -38.0000 -150.0000 75

  4 omega  -24.00   13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215  -99.0000  120.0000 37

  5 omega  -12.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215  -99.0000  150.0000 29

  6 omega  -15.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215  -99.0000 -150.0000 31

  7 omega  -73.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215    0.0000   60.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0029072000
_diffrn_orient_matrix_UB_12      0.0589227000
_diffrn_orient_matrix_UB_13      0.0083169000
_diffrn_orient_matrix_UB_21      -0.0708180000
_diffrn_orient_matrix_UB_22      0.0290209000
_diffrn_orient_matrix_UB_23      0.0035601000
_diffrn_orient_matrix_UB_31      -0.0043598000
_diffrn_orient_matrix_UB_32      -0.0293130000
_diffrn_orient_matrix_UB_33      0.0571389000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11433
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76358
_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    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0783P)^2^+0.8253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                5730
_reflns_number_total             6742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j3.cif
_cod_data_source_block           1
_cod_original_cell_volume        1367.49(12)
_cod_database_code               4349625
_reflns_odcompleteness_completeness 97.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H11 of C11, H19 of C19, {H14A,H14B} of C14, H5 of C5, H16 of C16, H3 of C3,
  {H22A,H22B} of C22, H4 of C4, H15 of C15, H24 of C24, H23 of C23
 At 1.5 times of:
  {H8A,H8B,H8C} of C8, {H1A,H1B,H1C} of C1
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C5(H5), C16(H16), C3(H3), C23(H23), C24(H24), C19(H19),
 C11(H11)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;