Dramatic impact of the lattice solvent on the dynamic magnetic relaxation of dinuclear dysprosium single-molecule magnets
Zhang, Wan-Ying; Zhang, Yi-Quan; Jiang, Shang-Da; Sun, Wen-Bin; Li, Hong-Feng; Wang, Bing-Wu; Chen, Peng; Yan, Peng-Fei; Gao, Song; Inorganic Chemistry Frontiers 5 (2018) 1575–; doi:10.1039/C8QI00266E

data_4349860
_publ_section_title
;
 Dramatic impact of the lattice solvent on the dynamic magnetic relaxation
 of dinuclear dysprosium single-molecule magnets
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1575
_journal_paper_doi               10.1039/C8QI00266E
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C76 H62 Dy2 O14, 4(C H Cl3)'
_chemical_formula_sum            'C80 H66 Cl12 Dy2 O14'
_chemical_formula_weight         2001.73
_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_block_doi                 10.5517/cc1jd3hj
_audit_creation_date             2015-02-02
_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.
2018-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.801(6)
_cell_angle_beta                 91.679(5)
_cell_angle_gamma                108.946(7)
_cell_formula_units_Z            1
_cell_length_a                   11.7531(9)
_cell_length_b                   13.8438(10)
_cell_length_c                   13.9872(7)
_cell_measurement_reflns_used    6200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.9270
_cell_measurement_theta_min      2.9016
_cell_volume                     2086.3(3)
_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 0.864
_diffrn_measurement_details
;
  1 omega  -10.00   90.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000  120.0000 100

  2 omega   31.00   58.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000 -150.0000 27

  3 omega    4.00   64.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000  -30.0000 60

  4 omega  -10.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277   77.0000 -120.0000 96

  5 omega   23.00   49.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215   77.0000 -120.0000 26

  6 omega   11.00   38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215   77.0000  150.0000 27

  7 omega  -48.00   49.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215   77.0000    0.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0099563000
_diffrn_orient_matrix_UB_12      -0.0090455000
_diffrn_orient_matrix_UB_13      0.0470034000
_diffrn_orient_matrix_UB_21      0.0549557000
_diffrn_orient_matrix_UB_22      0.0433928000
_diffrn_orient_matrix_UB_23      0.0100829000
_diffrn_orient_matrix_UB_31      -0.0316540000
_diffrn_orient_matrix_UB_32      0.0339997000
_diffrn_orient_matrix_UB_33      0.0206460000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19528
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78558
_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    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             994
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         10517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                7914
_reflns_number_total             10517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi00266e2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2086.3(2)
_cod_database_code               4349860
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H25 of C25, H26 of C26, H11 of C11, H5 of C5, H38 of C38, H13 of C13, H21
  of C21, H27 of C27, H16 of C16, H3 of C3, H40 of C40, H24 of C24, H28 of C28,
  H37 of C37, H23 of C23, H4 of C4, H34 of C34, H31 of C31, H10 of C10, H22 of
  C22, H9 of C9, H36 of C36, H39 of C39, H12 of C12, H35 of C35, H20 of C20,
  H19 of C19
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H8A,H8B,H8C} of C8
2.a Ternary CH refined with riding coordinates:
 C40(H40), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C5(H5), C12(H12), C35(H35), C20(H20), C19(H19), C11(H11), C26(H26),
 C25(H25), C13(H13), C21(H21), C27(H27), C16(H16), C3(H3), C24(H24), C28(H28),
 C37(H37), C23(H23), C4(H4), C34(H34), C31(H31), C10(H10), C22(H22), C9(H9),
 C36(H36)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;