Tuning slow magnetic relaxation behaviour in a {Dy2}-based one-dimensional chain via crystal field perturbation
Yu, Shui; Zhang, Qinhua; Hu, Huancheng; Chen, Zilu; Liu, Dongcheng; Liang, Yuning; Liang, Fupei; RSC Advances 10 (2020) 11831–11835; doi:10.1039/D0RA01604G

data_7240189
_publ_section_title
;
 Tuning slow magnetic relaxation behaviour in a {Dy2}-based
 one-dimensional chain via crystal field perturbation
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              11831
_journal_page_last               11835
_journal_paper_doi               10.1039/D0RA01604G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C60 H56 Dy2 N6 O14 S2, 2(C H4 O)'
_chemical_formula_sum            'C62 H64 Dy2 N6 O16 S2'
_chemical_formula_weight         1538.31
_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             2020-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-15 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                73.569(3)
_cell_angle_beta                 88.693(4)
_cell_angle_gamma                65.351(5)
_cell_formula_units_Z            1
_cell_length_a                   9.9101(6)
_cell_length_b                   11.7555(5)
_cell_length_c                   15.8011(5)
_cell_measurement_reflns_used    11063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6680
_cell_measurement_theta_min      3.6460
_cell_volume                     1595.15(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  52.00   1.00   25.00    --   10.68 -19.00-150.00  121
  2  \w    -20.00  52.00   1.00   25.00    --   10.68 -99.00  60.00   72
  3  \w    -77.00  99.00   1.00   25.00    --   10.68   0.00-120.00  176
  4  \w    -20.00  29.00   1.00   25.00    --  -11.93 -99.00 -90.00   49
  5  \w    -99.00 -34.00   1.00   25.00    --  -11.93 178.00  90.00   65
  6  \w    -20.00  29.00   1.00   25.00    --  -11.93 -99.00  90.00   49
  7  \w    -88.00 -42.00   1.00   25.00    --  -11.93 -77.00 -60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0755252000
_diffrn_orient_matrix_UB_12      -0.0094362000
_diffrn_orient_matrix_UB_13      0.0014016000
_diffrn_orient_matrix_UB_21      0.0066949000
_diffrn_orient_matrix_UB_22      -0.0215029000
_diffrn_orient_matrix_UB_23      0.0470572000
_diffrn_orient_matrix_UB_31      0.0229639000
_diffrn_orient_matrix_UB_32      -0.0655312000
_diffrn_orient_matrix_UB_33      -0.0005973000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22939
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.730
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0910P)^2^+0.3919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                4923
_reflns_number_total             5598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ra01604g2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7240189--7240190.cif.'
_cod_original_cell_volume        1595.15(12)
_cod_database_code               7240189
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(Dy1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) = Uanis(C30)
3.a Ternary CH refined with riding coordinates:
 C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2A), C2(H2B), C3(H3), C5(H5), C6(H6), C7(H7), C0AA(H0AA),
 C11(H11), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24)
3.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C8(H8A,H8B,H8C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O31(H31)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.575