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_7240190
_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         'C62 H60 Dy2 N4 O18, 2(C H4 O)'
_chemical_formula_sum            'C64 H68 Dy2 N4 O20'
_chemical_formula_weight         1538.22
_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                83.259(3)
_cell_angle_beta                 82.471(2)
_cell_angle_gamma                76.012(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9272(2)
_cell_length_b                   11.8458(4)
_cell_length_c                   15.0341(4)
_cell_measurement_reflns_used    15441
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8070
_cell_measurement_theta_min      3.9290
_cell_volume                     1693.96(8)
_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 15.9784
_diffrn_detector_type            Eos
_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    -51.00  38.00   1.00    5.00    --   17.61 -57.00 120.00   89
  2  \w    -73.00   4.00   1.00    5.00    --  -19.96 118.00 143.00   77
  3  \w    -90.00  10.00   1.00    5.00    --  -19.96 -77.00 -90.00  100
  4  \w    -50.00  50.00   1.00    5.00    --  -19.96  77.00  30.00  100
  5  \w    -89.00   1.00   1.00    5.00    --  -19.96 -57.00  30.00   90
  6  \w    -64.00  53.00   1.00    5.00    --  -19.96  19.00-150.00  117
  7  \w     35.00  94.00   1.00    5.00    --   17.61 178.00  30.00   59
  8  \w    -20.00  60.00   1.00    5.00    --   17.61 -99.00 -60.00   80
  9  \w    -89.00 -35.00   1.00    5.00    --  -19.96 -57.00 150.00   54
 10  \w    -89.00   1.00   1.00    5.00    --  -19.96 -57.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0682382000
_diffrn_orient_matrix_UB_12      0.0011016000
_diffrn_orient_matrix_UB_13      0.0085553000
_diffrn_orient_matrix_UB_21      0.0179000000
_diffrn_orient_matrix_UB_22      0.0130630000
_diffrn_orient_matrix_UB_23      -0.0466776000
_diffrn_orient_matrix_UB_31      -0.0225228000
_diffrn_orient_matrix_UB_32      0.0605515000
_diffrn_orient_matrix_UB_33      0.0055584000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25041
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48175
_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    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0701P)^2^+0.9644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                5647
_reflns_number_total             5943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ra01604g2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7240189--7240190.cif.'
_cod_original_cell_volume        1693.97(8)
_cod_database_code               7240190
_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:
  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. Restrained distances
 C32-O10
 1.4 with sigma of 0.001
 C30-C31
 1.5 with sigma of 0.0001
 H31C-H6_$1
 2.1 with sigma of 0.005
3. Others
 1*[Sof(O2A)+Sof(H2AA)]+1*[Sof(O2)]=1 with esd of 0.0001
 1*[Sof(O2A)+Sof(H2AA)]+1*[Sof(H2B)]=1 with esd of 0.0001
 Sof(O2A)=Sof(H2AA)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C11(H11), C2(H2), C3(H3), C8(H8), C5(H5), C7(H7), C6(H6), N2(H2A),
 C15(H15), C24(H24), C18(H18), C23(H23), C19(H19), C21(H21), C20(H20)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C32(H32A,H32B,
 H32C)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2B), O10(H10), O2A(H2AA)
;
_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 1.728
_oxdiff_exptl_absorpt_empirical_full_min 0.677