Designing a mononuclear DyIII single-molecule magnet (SMM) by using a N,O,N,O-based multichelating Schiff base ligand and a β-diketonate ligand
Zhang, Sheng; Mo, Wenjiao; Yin, Bing; Lü, Xingqiang; Zhang, Jiangwei; New Journal of Chemistry 43 (2019) 454–; doi:10.1039/C8NJ04019B

data_7057980
_publ_section_title
;
 Designing a mononuclear DyIII single-molecule magnet (SMM) by using a
 N,O,N,O-based multichelating Schiff base ligand and a \b-diketonate
 ligand
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              454
_journal_paper_doi               10.1039/C8NJ04019B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C43 H40 Dy F3 N4 O7'
_chemical_formula_sum            'C43 H40 Dy F3 N4 O7'
_chemical_formula_weight         944.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.602(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9674(8)
_cell_length_b                   11.0167(15)
_cell_length_c                   33.215(3)
_cell_measurement_reflns_used    771
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.6390
_cell_measurement_theta_min      4.1330
_cell_volume                     3994.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -81.00  -5.00   1.00    3.00    --  -56.18  61.00 -30.00   76
  2  \w    -30.00  -5.00   1.00    1.00    --    0.00  37.00-180.00   25
  3  \w      1.00  72.00   1.00    1.00    --    0.00  37.00-180.00   71
  4  \w     76.00 129.00   1.00    3.00    --   56.18  45.00 -90.00   53
  5  \w     87.00 173.00   1.00    3.00    --  112.35  77.00   0.00   86
  6  \w    152.00 177.00   1.00    3.00    --  112.35  50.00 -90.00   25
  7  \w    105.00 178.00   1.00    3.00    --  112.35 111.00-150.00   73
  8  \w     95.00 160.00   1.00    3.00    --  112.35  37.00 -60.00   65
  9  \w     87.00 116.00   1.00    3.00    --  112.35  50.00 -90.00   29
 10  \w     47.00  74.00   1.00    3.00    --   56.18 -61.00 120.00   27
 11  \w     18.00 116.00   1.00    3.00    --   56.18-125.00 120.00   98
 12  \w     88.00 115.00   1.00    3.00    --  112.35-111.00   0.00   27
 13  \w     77.00 153.00   1.00    3.00    --  112.35 -91.00-120.00   76
 14  \w     49.00  99.00   1.00    3.00    --  112.35-111.00  60.00   50
 15  \w     65.00 153.00   1.00    3.00    --  112.35 -91.00 120.00   88
 16  \w     43.00  68.00   1.00    3.00    --  112.35-111.00   0.00   25
 17  \w     -4.00  21.00   1.00    1.00    --    0.00 -99.00  60.00   25
 18  \w   -128.00 -80.00   1.00    3.00    --  -56.18 -94.00  30.00   48
 19  \w   -130.00 -80.00   1.00    3.00    --  -56.18 -94.00-120.00   50
 20  \w    -67.00 -42.00   1.00    1.00    --    0.00 178.00 120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457952000
_diffrn_orient_matrix_UB_12      -0.1322507000
_diffrn_orient_matrix_UB_13      -0.0004578000
_diffrn_orient_matrix_UB_21      -0.0375805000
_diffrn_orient_matrix_UB_22      0.0096112000
_diffrn_orient_matrix_UB_23      -0.0458139000
_diffrn_orient_matrix_UB_31      0.1281183000
_diffrn_orient_matrix_UB_32      -0.0443472000
_diffrn_orient_matrix_UB_33      -0.0085667000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.2686
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11737
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.639
_diffrn_reflns_theta_max         59.989
_diffrn_reflns_theta_min         2.673
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.607
_exptl_absorpt_correction_T_max  0.346
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ad
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         4845
_refine_ls_number_restraints     1888
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0094P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3245
_reflns_number_total             5941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04019b2.cif
_cod_data_source_block           exp_8720
_cod_depositor_comments
'Adding full bibliography for 7057980--7057981.cif.'
_cod_database_code               7057980
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.88
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C43
 1.48 with sigma of 0.01
 C8-O3
 1.42 with sigma of 0.01
 C35-C37 = C37-C39 = C39-C35 = C36-C38 = C38-C40 = C40-C36
 2.37 with sigma of 0.01
 C35-C36 = C36-C37 = C37-C38 = C38-C39 = C39-C40 = C40-C35
 1.38 with sigma of 0.01
 C14-C15 = C11-C12 = C37-C41 = C39-C42 = C1-C2
 1.52 with sigma of 0.01
 C12-C14 = C14-C16 = C16-C12 = C13-C15 = C15-C17 = C17-C13
 2.37 with sigma of 0.01
 C12-C13 = C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C12
 1.38 with sigma of 0.01
 C17-O6
 1.42 with sigma of 0.01
 F1-F2 = F2-F3 = F3-F1
 2.02 with sigma of 0.01
 C1-F1 = C1-F2 = C1-F3
 1.28 with sigma of 0.01
 C5-C7 = C7-C9 = C9-C5 = C6-C8 = C8-C10 = C10-C6
 2.37 with sigma of 0.01
 C4-C5 = C5-C6 = C6-C7 = C7-C8 = C8-C9 = C9-C10 = C10-C5
 1.38 with sigma of 0.01
 N1-C21 = C21-C22 = C22-C23 = C23-C24 = C24-C25 = C25-N1
 1.38 with sigma of 0.01
 N1-C22 = C22-C24 = C24-N1 = C21-C23 = C23-C25 = C25-C21
 2.37 with sigma of 0.01
 N4-C29 = C29-C30 = C30-C31 = C31-C32 = C32-C33 = C33-N4
 1.38 with sigma of 0.01
 N4-C32 = C32-C30 = C30-N4 = C29-C31 = C31-C33 = C33-C29
 2.37 with sigma of 0.01
 O3-C7 \\sim O3-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C34(H34A,H34B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C15(H15),
 C22(H22), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33),
  C36(H36), C38(H38), C42(H42)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;