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_7709124
_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         'C54 H45 Dy N6 O15, C2 H3 N'
_chemical_formula_sum            'C56 H48 Dy N7 O15'
_chemical_formula_weight         1221.51
_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     dual
_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                84.285(3)
_cell_angle_beta                 73.708(3)
_cell_angle_gamma                71.392(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8649(4)
_cell_length_b                   14.6451(5)
_cell_length_c                   14.8049(4)
_cell_measurement_reflns_used    11208
_cell_measurement_temperature    295.3(5)
_cell_measurement_theta_max      71.6400
_cell_measurement_theta_min      3.9720
_cell_volume                     2734.45(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      295.3(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.967
_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    -63.00  32.00   1.00    1.10    --  -36.04  77.00  90.00   95
  2  \w   -104.00  -9.00   1.00    1.10    --  -36.04 -77.00  30.00   95
  3  \w    -63.00  32.00   1.00    1.10    --  -36.04  77.00 150.00   95
  4  \w   -103.00 -19.00   1.00    1.10    --  -36.04 -57.00 -60.00   84
  5  \w     23.00  89.00   1.00    1.10    --   36.04-125.00 -60.00   66
  6  \w      7.00 107.00   1.00    1.10    --   36.04  19.00 -60.00  100
  7  \w     23.00  89.00   1.00    1.10    --   36.04-125.00-150.00   66
  8  \w    100.00 176.00   1.00    4.40    --  106.21 111.00-120.00   76
  9  \w     89.00 175.00   1.00    4.40    --  106.21  45.00 150.00   86
 10  \w    100.00 176.00   1.00    4.40    --  106.21 111.00 -30.00   76
 11  \w    100.00 176.00   1.00    4.40    --  106.21 111.00 150.00   76
 12  \w     38.00 124.00   1.00    4.40    --  106.21 -45.00  60.00   86
 13  \w     37.00 109.00   1.00    4.40    --  106.21 -94.00 -60.00   72
 14  \w     36.00 113.00   1.00    4.40    --  106.21-111.00  30.00   77
 15  \w     88.00 173.00   1.00    4.40    --  106.21  61.00-150.00   85
 16  \w    100.00 176.00   1.00    4.40    --  106.21 111.00-180.00   76
 17  \w     85.00 176.00   1.00    4.40    --  106.21  30.00 -30.00   91
 18  \w     37.00 109.00   1.00    4.40    --  106.21 -94.00  90.00   72
 19  \w     38.00 124.00   1.00    4.40    --  106.21 -45.00-180.00   86
 20  \w     37.00 109.00   1.00    4.40    --  106.21 -94.00-150.00   72
 21  \w     36.00 113.00   1.00    4.40    --  106.21-111.00-180.00   77
 22  \w    100.00 176.00   1.00    4.40    --  106.21 111.00  90.00   76
 23  \w     79.00 174.00   1.00    4.40    --  106.21  77.00-120.00   95
 24  \w   -104.00  -9.00   1.00    1.10    --  -36.04 -77.00 150.00   95
 25  \w   -104.00  -9.00   1.00    1.10    --  -36.04 -77.00-120.00   95
 26  \w      7.00 107.00   1.00    1.10    --   36.04  19.00 120.00  100
 27  \w     19.00 103.00   1.00    1.10    --   36.04  57.00 120.00   84
 28  \w    -31.00  53.00   1.00    1.10    --   36.04 -57.00 -30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007648000
_diffrn_orient_matrix_UB_12      -0.1007908000
_diffrn_orient_matrix_UB_13      0.0417755000
_diffrn_orient_matrix_UB_21      -0.0640132000
_diffrn_orient_matrix_UB_22      -0.0101898000
_diffrn_orient_matrix_UB_23      -0.0662286000
_diffrn_orient_matrix_UB_31      0.1033206000
_diffrn_orient_matrix_UB_32      -0.0453747000
_diffrn_orient_matrix_UB_33      -0.0749866000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28539
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.708
_diffrn_reflns_theta_min         3.487
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.484
_exptl_crystal_description       needle
_exptl_crystal_F_000             1238
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.136
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1217P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8933
_reflns_number_total             10356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03701c2.cif
_cod_data_source_block           yxq-yh-och3-dy_sq
_cod_original_cell_volume        2734.46(16)
_cod_database_code               7709124
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.199
_shelx_estimated_absorpt_t_min   0.072
_reflns_odcompleteness_completeness 98.79
_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
2.a Aromatic/amide H refined with riding coordinates:
 N5(H006), N6(H008), N1(H00D), C46(H00K), C52(H00S), C19(H00X), C11(H00Y),
 C13(H012), C28(H014), C48(H016), C51(H017), C42(H018), C49(H01A), C16(H01B),
 C5(H01C), C39(H01D), C34(H01E), C37(H01F), C36(H01G), C33(H01H), C20(H01J),
 C25(H01K), C40(H01L), C30(H01M), C17(H01P), C8(H01R), C14(H01S), C41(H01T),
 C3(H01U), C2(H01V), C7(H01W), C6(H01Y), C31(H01Z), C22(H020), C24(H021)
2.b Idealised Me refined as rotating group:
 C53(H01i,H01n,H01o), C54(H02a,H02b,H02c), C55(H02d,H02e,H02f), C57(H02g,H02h,
 H02i)
;
_shelx_res_checksum              30343
_shelx_hkl_checksum              3407
_shelx_fab_checksum              60198
_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 3.842
_oxdiff_exptl_absorpt_empirical_full_min 0.502