Dy<sup>III</sup> single-molecule magnets from ligands incorporating both amine and acylhydrazine Schiff base groups: the centrosymmetric {Dy<sub>2</sub>} displaying dual magnetic relaxation behaviors.
Su, Sen-Da; Li, Jia-Xin; Xu, Fan; Wang, Chen-Xiao; Wang, Kai; Li, Yan; Zhang, Shu-Hua; Zhang, Xiu-Qing; Zhang, Yi-Quan; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15739–15749; doi:10.1039/c9dt04434e

data_7705723
_publ_section_title
;
 Dy<sup>III</sup> single-molecule magnets from ligands incorporating both
 amine and acylhydrazine Schiff base groups: the centrosymmetric
 {Dy<sub>2</sub>} displaying dual magnetic relaxation behaviors.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15739
_journal_page_last               15749
_journal_paper_doi               10.1039/c9dt04434e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C38 H46 Dy2 N8 O12'
_chemical_formula_sum            'C38 H46 Dy2 N8 O12'
_chemical_formula_weight         1131.83
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-10-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                109.174(3)
_cell_angle_beta                 100.065(3)
_cell_angle_gamma                90.167(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4259(4)
_cell_length_b                   10.7569(3)
_cell_length_c                   11.1938(3)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    302.13(10)
_cell_measurement_theta_max      31.1270
_cell_measurement_theta_min      1.9460
_cell_volume                     1053.30(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      302.13(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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      0.00  33.00   0.50    0.32    --    8.30 -83.00 -62.00   66
  2  \w    -31.00  10.00   0.50    0.32    --   -8.54  83.00  58.00   82
  3  \w    -37.00  17.00   0.50    0.32    --   -8.54 -83.00 -62.00  108
  4  \w    -67.00   4.00   0.50    0.32    --    8.30 -19.00  30.00  142
  5  \w    -66.00  20.00   0.50    0.32    --    8.30 -37.00 -30.00  172
  6  \w    -14.00  42.00   0.50    0.32    --    8.30 -99.00  90.00  112
  7  \w     -7.00  48.00   0.50    0.32    --    8.30  57.00-180.00  110
  8  \w    -69.00  12.00   0.50    0.32    --   -8.54 -77.00-150.00  162
  9  \w     29.00  72.00   0.50    0.32    --    8.30  77.00 -30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0014304000
_diffrn_orient_matrix_UB_12      0.0087188000
_diffrn_orient_matrix_UB_13      -0.0599053000
_diffrn_orient_matrix_UB_21      -0.0674357000
_diffrn_orient_matrix_UB_22      0.0289666000
_diffrn_orient_matrix_UB_23      0.0018971000
_diffrn_orient_matrix_UB_31      0.0362780000
_diffrn_orient_matrix_UB_32      0.0630806000
_diffrn_orient_matrix_UB_33      0.0327075000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14369
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.960
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3691
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3313
_reflns_number_total             3691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04434e2.cif
_cod_data_source_block           hzb201014_1_rt
_cod_depositor_comments
'Adding full bibliography for 7705722--7705724.cif.'
_cod_database_code               7705723
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.762
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 Dy1-H6
 2.992158 with sigma of 0.02
 C18-H6
 1.935441 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13)
4.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              42242
_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 2.248
_oxdiff_exptl_absorpt_empirical_full_min 0.646