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_7709121
_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         'C34 H26 Dy N7 O16'
_chemical_formula_sum            'C34 H26 Dy N7 O16'
_chemical_formula_weight         951.12
_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     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                74.093(3)
_cell_angle_beta                 88.444(3)
_cell_angle_gamma                87.655(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6525(3)
_cell_length_b                   13.5408(6)
_cell_length_c                   17.7030(6)
_cell_measurement_reflns_used    8408
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      71.6200
_cell_measurement_theta_min      4.8180
_cell_volume                     1762.44(12)
_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      296(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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   -104.00 -10.00   1.00    2.70    --  -36.42 -77.00 -60.00   94
  2  \w   -104.00 -20.00   1.00    2.70    --  -36.42 -57.00  30.00   84
  3  \w   -104.00 -20.00   1.00    2.70    --  -36.42 -57.00 -30.00   84
  4  \w    -53.00  31.00   1.00    2.70    --  -36.42  57.00 150.00   84
  5  \w   -106.00 -18.00   1.00    2.70    --  -36.42 -38.00-180.00   88
  6  \w     20.00 104.00   1.00    2.70    --   36.42  57.00 -90.00   84
  7  \w     23.00  90.00   1.00    2.70    --   36.42-125.00   0.00   67
  8  \w      1.00  75.00   1.00    2.70    --   36.42 -99.00 150.00   74
  9  \w    100.00 176.00   1.00   10.79    --  106.21 111.00-120.00   76
 10  \w     35.00 145.00   1.00   10.79    --  106.21 -15.00 -60.00  110
 11  \w     57.00 150.00   1.00   10.79    --  106.21 178.00 150.00   93
 12  \w     38.00 124.00   1.00   10.79    --  106.21 -45.00  30.00   86
 13  \w     36.00 113.00   1.00   10.79    --  106.21-111.00-120.00   77
 14  \w     38.00 124.00   1.00   10.79    --  106.21 -45.00  90.00   86
 15  \w     36.00 113.00   1.00   10.79    --  106.21-111.00-180.00   77
 16  \w     38.00 124.00   1.00   10.79    --  106.21 -45.00 150.00   86
 17  \w     36.00 128.00   1.00   10.79    --  106.21 -30.00 150.00   92
 18  \w     37.00 109.00   1.00   10.79    --  106.21 -94.00 -90.00   72
 19  \w     39.00 124.00   1.00   10.79    --  106.21 -61.00-120.00   85
 20  \w     37.00 109.00   1.00   10.79    --  106.21 -94.00  30.00   72
 21  \w     88.00 173.00   1.00   10.79    --  106.21  61.00   0.00   85
 22  \w     85.00 176.00   1.00   10.79    --  106.21  30.00 -30.00   91
 23  \w    -55.00  -4.00   1.00    2.70    --  -36.42  38.00 -90.00   51
;
_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      0.0423021000
_diffrn_orient_matrix_UB_12      -0.1162579000
_diffrn_orient_matrix_UB_13      0.0180274000
_diffrn_orient_matrix_UB_21      0.0692427000
_diffrn_orient_matrix_UB_22      0.0149034000
_diffrn_orient_matrix_UB_23      -0.0847741000
_diffrn_orient_matrix_UB_31      0.1844524000
_diffrn_orient_matrix_UB_32      0.0165648000
_diffrn_orient_matrix_UB_33      0.0260498000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.766
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09535
_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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       plate
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.471
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+0.0718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6229
_reflns_number_total             6762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03701c2.cif
_cod_data_source_block           yxq-yh-no2
_cod_database_code               7709121
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.98
_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 O(H,H) groups
2.a Rotating group:
 O2(H00a,H00b)
2.b Aromatic/amide H refined with riding coordinates:
 N00C(H00C), N00F(H00F), C00T(H00T), C00U(H00U), C00Z(H00Z), C011(H011),
 C012(H012), C013(H013), C015(H015), C016(H016), C017(H017), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G),
 C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M)
;
_shelx_res_checksum              94764
_shelx_hkl_checksum              69630
_olex2_date_sample_data_collection 2019-06-12
_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 6.642
_oxdiff_exptl_absorpt_empirical_full_min 0.544