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_4349862
_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, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C80 H70 Cl4 Dy2 O14'
_chemical_formula_weight         1722.16
_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/cc1jd3jk
_audit_creation_date             2015-06-25
_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                70.393(3)
_cell_angle_beta                 71.631(3)
_cell_angle_gamma                75.913(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4039(3)
_cell_length_b                   13.0199(5)
_cell_length_c                   13.9897(5)
_cell_measurement_reflns_used    8873
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      29.4220
_cell_measurement_theta_min      3.2720
_cell_volume                     1834.87(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.5830
_diffrn_measurement_details
;
  1 omega  -59.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191    0.0000   90.0000 143

  2 omega    7.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -99.0000  120.0000 49

  3 omega  -16.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -38.0000   30.0000 49

  4 omega -104.00  -78.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566 -178.0000  150.0000 26

  5 omega  -62.00   16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -77.0000 -150.0000 78

  6 omega -102.00  -67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000  -90.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120398000
_diffrn_orient_matrix_UB_12      0.0402733000
_diffrn_orient_matrix_UB_13      -0.0460704000
_diffrn_orient_matrix_UB_21      -0.0371209000
_diffrn_orient_matrix_UB_22      0.0358776000
_diffrn_orient_matrix_UB_23      0.0304984000
_diffrn_orient_matrix_UB_31      0.0536338000
_diffrn_orient_matrix_UB_32      0.0227275000
_diffrn_orient_matrix_UB_33      -0.0068253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18982
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         3.09
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             862
_refine_diff_density_max         2.047
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                7971
_reflns_number_total             9451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi00266e2.cif
_cod_data_source_block           3
_cod_original_cell_volume        1834.87(11)
_cod_database_code               4349862
_chemical_oxdiff_formula         'Dy2 C76 H62 O14'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H81A,H81B} of C81, {H80A,H80B} of C80, H45 of C45, H44 of C44, H43 of C43,
  H42 of C42, H41 of C41, H1AA of C1A, H1BA of C1B, H1CA of C1C, H5 of C5, H6
  of C6, H7 of C7, H18 of C18, H19 of C19, H20 of C20, H21 of C21, H24 of C24,
  H27 of C27, H28 of C28, H29 of C29, H31 of C31, H32 of C32, H33 of C33, H34
  of C34, H35 of C35, H38 of C38
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H8A,H8B,H8C} of C8
2.a Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C81(H81A,H81B)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C1C(H1CA), C5(H5), C6(H6), C7(H7), C18(H18), C19(H19),
 C20(H20), C21(H21), C24(H24), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;