Constructing high axiality mononuclear dysprosium molecular magnets <i>via</i> a regulation-of-co-ligands strategy.
Wang, Jia-Ling; Chen, Ji-Tun; Yan, Han; Wang, Tian-Tian; Zhang, Yi-Quan; Sun, Wen-Bin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10982–10990; doi:10.1039/d4dt00040d

data_7716266
_publ_section_title
;
 Constructing high axiality mononuclear dysprosium molecular magnets
 <i>via</i> a regulation-of-co-ligands strategy.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10982
_journal_page_last               10990
_journal_paper_doi               10.1039/d4dt00040d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H31 Dy F4 N5 O2, C24 H20 B'
_chemical_formula_sum            'C52 H51 B Dy F4 N5 O2'
_chemical_formula_weight         1027.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2351(6)
_cell_length_b                   17.8266(13)
_cell_length_c                   27.2325(16)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.4520
_cell_measurement_theta_min      3.2360
_cell_volume                     4968.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -27.00  27.00   1.00    0.30    --  -48.42  19.00  60.00   54
  2  \w   -104.00 -29.00   1.00    0.30    --  -48.42 154.00-155.00   75
  3  \w    -66.00 -22.00   1.00    5.00    --  -91.75  57.00 -60.00   44
  4  \w   -118.00 -73.00   1.00    0.30    --  -48.42-125.00  90.00   45
  5  \w   -163.00-101.00   1.00    5.00    --  -91.75-121.00 -36.00   62
  6  \w     43.00 106.00   1.00    5.00    --  106.65 -99.00   0.00   63
  7  \w     94.00 140.00   1.00    5.00    --  106.65  31.00 -20.00   46
  8  \w    108.00 176.00   1.00    5.00    --  106.65  92.00 153.00   68
  9  \w    141.00 167.00   1.00    5.00    --  106.65  19.00 150.00   26
 10  \w     97.00 130.00   1.00    5.00    --  106.65  19.00 150.00   33
 11  \w   -163.00-123.00   1.00    5.00    --  -91.75 -92.00  41.00   40
 12  \w     37.00  94.00   1.00    0.30    --   48.42-125.00 -90.00   57
 13  \w    -65.00 -21.00   1.00    5.00    --  -91.75  57.00   0.00   44
 14  \w    -85.00 -55.00   1.00    5.00    --  -91.75 125.00   0.00   30
 15  \w    -48.00 -22.00   1.00    5.00    --  -91.75 125.00   0.00   26
 16  \w     94.00 158.00   1.00    5.00    --  106.65  57.00  60.00   64
 17  \w     36.00  66.00   1.00    5.00    --  106.65 -57.00  30.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0117889000
_diffrn_orient_matrix_UB_12      -0.0104520000
_diffrn_orient_matrix_UB_13      -0.0560111000
_diffrn_orient_matrix_UB_21      0.0599532000
_diffrn_orient_matrix_UB_22      0.0790479000
_diffrn_orient_matrix_UB_23      -0.0043901000
_diffrn_orient_matrix_UB_31      0.1375543000
_diffrn_orient_matrix_UB_32      -0.0332504000
_diffrn_orient_matrix_UB_33      0.0068361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9071
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.034(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0755
_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^)+(0.1731P)^2^+0.2622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2308
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                7169
_reflns_number_total             9071
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.8114\% 
around [1.00 -0.00 -0.02] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            d4dt00040d2.cif
_cod_data_source_block           Dy1
_cod_depositor_comments
'Adding full bibliography for 7716265--7716266.cif.'
_cod_database_code               7716266
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyBNO
_shelx_estimated_absorpt_t_max   0.483
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.956(8)
 0.044(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C38 = N5-C26 = N4-C23
 1.5 with sigma of 0.01
 N3-C51
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim C8 \\sim C9 \\sim C10 \\sim C12
\\sim C13 \\sim C14 \\sim C16 \\sim C23 \\sim C25 \\sim C26 \\sim C38 \\sim C42
\\sim C43 \\sim C45 \\sim C50 \\sim C51: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 2A
F2 \\sim F3 \\sim O1 \\sim C2 \\sim C15 \\sim C21 \\sim C28 \\sim C29 \\sim
C33: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within
2A
5.a Ternary CH refined with riding coordinates:
 N3(H3), N4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C23(H23A,H23B), C38(H38A,H38B), C42(H42A,H42B),
 C50(H50A,H50B), C51(H51A,H51B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C14(H14), C2(H2), C21(H21), C32(H32), C33(H33), C34(H34),
 C52(H52), C1(H1), C3(H3A), C4(H4A), C5(H5), C11(H11), C19(H19), C20(H20),
 C22(H22), C31(H31), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
  C44(H44), C46(H46), C47(H47), C48(H48), C49(H49)
5.d Fitted hexagon refined as free rotating group:
 N1(C8,C10,C12,C14,C16)
5.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C43(H43A,H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13257
_shelx_hkl_checksum              1400
_shelx_fab_checksum              2575
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.665
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2