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_7709123
_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         'C51 H36 Dy I3 N6 O12'
_chemical_formula_sum            'C51 H36 Dy I3 N6 O12'
_chemical_formula_weight         1468.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-15
_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                90
_cell_angle_beta                 116.048(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6705(5)
_cell_length_b                   19.3672(5)
_cell_length_c                   17.5330(7)
_cell_measurement_reflns_used    10237
_cell_measurement_temperature    285(16)
_cell_measurement_theta_max      71.6430
_cell_measurement_theta_min      5.0770
_cell_volume                     5085.7(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      285(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9767
_diffrn_measured_fraction_theta_max 0.9767
_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   -105.00 -17.00   1.00    4.22    --  -36.29 -38.00 -90.00   88
  2  \w   -104.00 -20.00   1.00    4.22    --  -36.29 -57.00   0.00   84
  3  \w    -53.00  31.00   1.00    4.22    --  -36.29  57.00 120.00   84
  4  \w    -35.00  63.00   1.00    4.22    --   36.29 -23.00 169.00   98
  5  \w    -31.00  53.00   1.00    4.22    --   36.29 -57.00  90.00   84
  6  \w     68.00 177.00   1.00   16.90    --  106.21  15.00  60.00  109
  7  \w     36.00 128.00   1.00   16.90    --  106.21 -30.00 150.00   92
  8  \w     89.00 175.00   1.00   16.90    --  106.21  45.00 -60.00   86
  9  \w     37.00 109.00   1.00   16.90    --  106.21 -94.00-180.00   72
 10  \w     37.00 109.00   1.00   16.90    --  106.21 -94.00  90.00   72
 11  \w     39.00 124.00   1.00   16.90    --  106.21 -61.00 -90.00   85
 12  \w     39.00 133.00   1.00   16.90    --  106.21 -77.00-120.00   94
 13  \w    -90.00  -2.00   1.00    4.22    --  -36.29 125.00 -60.00   88
 14  \w   -104.00 -20.00   1.00    4.22    --  -36.29 -57.00 150.00   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      0.0300851000
_diffrn_orient_matrix_UB_12      -0.0069415000
_diffrn_orient_matrix_UB_13      0.0961648000
_diffrn_orient_matrix_UB_21      -0.0949745000
_diffrn_orient_matrix_UB_22      -0.0229225000
_diffrn_orient_matrix_UB_23      -0.0171203000
_diffrn_orient_matrix_UB_31      0.0258613000
_diffrn_orient_matrix_UB_32      -0.0758846000
_diffrn_orient_matrix_UB_33      -0.0036033000
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27853
_diffrn_reflns_theta_full        72.1331
_diffrn_reflns_theta_max         72.13
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21267
_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    1.9172
_exptl_crystal_description       block
_exptl_crystal_F_000             2787.9989
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.9521
_refine_diff_density_min         -1.1835
_refine_diff_density_rms         0.1971
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             12.2204
_refine_ls_goodness_of_fit_ref   1.0368
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0368
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+6.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -20
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7564
_reflns_number_total             9800
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1dt03701c2.cif
_cod_data_source_block           yxq-yh-dyi
_cod_database_code               7709123
_reflns_odcompleteness_completeness 99.95
_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
2.a Aromatic/amide H refined with riding coordinates:
 N1(H00B), N3(H00F), N2(H00G), C7(H00Q), C10(H00U), C16(H00X), C41(H012),
 C44(H014), C4(H015), C5(H016), C24(H017), C50(H019), C45(H01A), C15(H01B),
 C39(H01C), C11(H01E), C18(H01F), C35(H01H), C28(H01J), C22(H01K), C47(H01M),
 C49(H01N), C36(H01O), C19(H01P), C21(H01Q), C13(H01R), C27(H01S), C38(H01T),
 C2(H01U), C30(H01V), C1(H01W), C12(H01X), C31(H01Y), C48(H01Z), C33(H020),
 C32(H021)
;
_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 2.645
_oxdiff_exptl_absorpt_empirical_full_min 0.498