Enhancing the magnetic properties of Dy(III) single-molecule magnets in octahedral coordination symmetry by tuning the equatorial ligands.
Peng, Xiao-Han; Shang, Tao; Zheng, Jieyu; Liu, Ming; Zheng, Qi; Guo, Fu-Sheng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16709–16715; doi:10.1039/d4dt02482f

data_7717075
_publ_section_title
;
 Enhancing the magnetic properties of Dy(III) single-molecule magnets in
 octahedral coordination symmetry by tuning the equatorial ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16709
_journal_page_last               16715
_journal_paper_doi               10.1039/d4dt02482f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H42 Cl2 Dy N3 O'
_chemical_formula_sum            'C28 H42 Cl2 Dy N3 O'
_chemical_formula_weight         670.04
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-12 deposited with the CCDC.	2024-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8925(7)
_cell_length_b                   18.1625(16)
_cell_length_c                   18.7460(17)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.445
_cell_measurement_theta_min      2.173
_cell_volume                     3027.7(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.243
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.6404.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 2242 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5765
_reflns_number_total             6610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02482f1.cif
_cod_data_source_block           '[dy(tritox)py3cl2]'
_cod_depositor_comments
'Adding full bibliography for 7717075--7717076.cif.'
_cod_database_code               7717075
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.386
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10A-C1 \\sim C10-C1
 with sigma of 0.02
 C13-C10 \\sim C12-C10 \\sim C11-C10 \\sim C13A-C10A \\sim C12A-C10A \\sim
C11A-C10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10A \\sim C10: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C11 \\sim C11A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C10A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C13A(H13D,H13E,H13F), C12A(H12D,H12E,H12F), C11A(H11D,H11E,H11F)
;
_shelx_res_checksum              21935
_shelx_hkl_checksum              82053
_olex2_submission_special_instructions 'No special instructions were received'