Four mononuclear dysprosium complexes with neutral Schiff-base ligands: syntheses, crystal structures and slow magnetic relaxation behavior
Yang, Hui; Liu, Shan-Shan; Meng, Yin-Shan; Zhang, Yi-Quan; Pu, Lin; Wang, Xincheng; Lin, Shijing; Dalton Transactions  (2022) –; doi:10.1039/D1DT03701C

data_7709122
_publ_section_title
;
 Four mononuclear dysprosium complexes with neutral Schiff-base ligands:
 syntheses, crystal structures and slow magnetic relaxation behavior
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03701C
_journal_year                    2022
_chemical_formula_moiety         'C35 H28 Cl2 Dy N5 O12'
_chemical_formula_sum            'C35 H28 Cl2 Dy N5 O12'
_chemical_formula_weight         944.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-17 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                74.391(3)
_cell_angle_beta                 75.603(3)
_cell_angle_gamma                88.261(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1590(3)
_cell_length_b                   13.0834(4)
_cell_length_c                   16.2171(4)
_cell_measurement_reflns_used    10960
_cell_measurement_temperature    294.3(7)
_cell_measurement_theta_max      72.8550
_cell_measurement_theta_min      3.8960
_cell_volume                     1811.47(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.3(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9804
_diffrn_measured_fraction_theta_max 0.9795
_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   -108.00  -7.00   1.00    3.56    --  -36.54 -19.00 150.00  101
  2  \w    -55.00  33.00   1.00    3.56    --  -36.54  38.00 -30.00   88
  3  \w   -106.00 -18.00   1.00    3.56    --  -36.54 -38.00 150.00   88
  4  \w     23.00  90.00   1.00    3.56    --   36.54-125.00  30.00   67
  5  \w     23.00  90.00   1.00    3.56    --   36.54-125.00 120.00   67
  6  \w    -31.00  53.00   1.00    3.56    --   36.54 -57.00  90.00   84
  7  \w     23.00  90.00   1.00    3.56    --   36.54-125.00-120.00   67
  8  \w     20.00 104.00   1.00    3.56    --   36.54  57.00  30.00   84
  9  \w     39.00 109.00   1.00   14.25    --  108.71 -94.00 120.00   70
 10  \w     39.00 130.00   1.00   14.25    --  108.71 -30.00 -30.00   91
 11  \w     39.00 109.00   1.00   14.25    --  108.71 -94.00-150.00   70
 12  \w     40.00 126.00   1.00   14.25    --  108.71 -45.00 120.00   86
 13  \w    100.00 178.00   1.00   14.25    --  108.71 111.00-150.00   78
 14  \w     39.00 115.00   1.00   14.25    --  108.71-111.00  60.00   76
 15  \w     39.00 130.00   1.00   14.25    --  108.71 -30.00  90.00   91
 16  \w     87.00 178.00   1.00   14.25    --  108.71  30.00-180.00   91
 17  \w     40.00 126.00   1.00   14.25    --  108.71 -45.00-150.00   86
 18  \w     37.00 147.00   1.00   14.25    --  108.71 -15.00-180.00  110
 19  \w     39.00 115.00   1.00   14.25    --  108.71-111.00 -60.00   76
 20  \w    100.00 178.00   1.00   14.25    --  108.71 111.00-180.00   78
 21  \w     91.00 176.00   1.00   14.25    --  108.71  61.00 -90.00   85
 22  \w     57.00 151.00   1.00   14.25    --  108.71 178.00  90.00   94
 23  \w     20.00 104.00   1.00    3.56    --   36.54  57.00 120.00   84
 24  \w    -33.00  55.00   1.00    3.56    --   36.54 -38.00 150.00   88
 25  \w     10.00 104.00   1.00    3.56    --   36.54  77.00-180.00   94
 26  \w     10.00 104.00   1.00    3.56    --   36.54  77.00 -60.00   94
 27  \w     20.00 104.00   1.00    3.56    --   36.54  57.00  60.00   84
 28  \w     20.00 104.00   1.00    3.56    --   36.54  57.00 -60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1524919000
_diffrn_orient_matrix_UB_12      -0.0518041000
_diffrn_orient_matrix_UB_13      0.0592651000
_diffrn_orient_matrix_UB_21      0.0562644000
_diffrn_orient_matrix_UB_22      -0.1099100000
_diffrn_orient_matrix_UB_23      -0.0080859000
_diffrn_orient_matrix_UB_31      0.0615042000
_diffrn_orient_matrix_UB_32      -0.0143444000
_diffrn_orient_matrix_UB_33      0.0824443000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20040
_diffrn_reflns_theta_full        73.1665
_diffrn_reflns_theta_max         73.17
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.7306
_exptl_crystal_description       block
_exptl_crystal_F_000             922.8529
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.2080
_refine_diff_density_min         -0.9305
_refine_diff_density_rms         0.1225
_refine_ls_d_res_high            0.8054
_refine_ls_d_res_low             12.5912
_refine_ls_goodness_of_fit_ref   1.0401
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7120
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0399
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.0011
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.2556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6738
_reflns_number_total             7120
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03701c2.cif
_cod_data_source_block           yxq-yh-c3-dy
_cod_original_cell_volume        1811.46(10)
_cod_database_code               7709122
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.01
 C18-H2
 1.911461 with sigma of 0.02
 Dy01-H2
 2.882467 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1), C7(H7), C25(H25), C28(H28), C22(H22), C15(H15), C23(H23),
 C16(H16), C29(H29), C1(H1a), C12(H12), C13(H13), C5(H5a), C10(H10), C31(H31),
 C11(H11), C34(H34), C33(H33), C4(H4), C32(H32), C2(H2a), C19(H19), C20(H20)
3.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c)
;
_olex2_date_sample_data_collection 2018-11-09
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.797