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_7717076
_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 Dy I2 N3 O'
_chemical_formula_sum            'C28 H42 Dy I2 N3 O'
_chemical_formula_weight         852.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-12
_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                   9.1597(6)
_cell_length_b                   18.4547(12)
_cell_length_c                   19.0883(10)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.434
_cell_measurement_theta_min      2.402
_cell_volume                     3226.7(3)
_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
_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  0.0675
_diffrn_reflns_av_unetI/netI     0.0543
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31180
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.496
_diffrn_reflns_theta_min         2.134
_exptl_absorpt_coefficient_mu    4.252
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0763 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8609.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1954 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6688
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0096P)^2^+6.4088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5300
_reflns_number_total             6688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02482f1.cif
_cod_data_source_block           '[dy(tritox)py3i2]'
_cod_depositor_comments
'Adding full bibliography for 7717075--7717076.cif.'
_cod_database_code               7717076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.727
_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
 C5-C2 = C11-C10
 1.55 with sigma of 0.01
 C8-C6
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) \\sim Ueq, Uanis(C28A) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.05
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C25) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C5) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.015
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=
 Sof(C24A)=Sof(H24A)=1-FVAR(1)
 Sof(H26)=Sof(C28)=Sof(H28)=Sof(C27)=Sof(H27)=Sof(C25)=Sof(H25)=Sof(C24)=
 Sof(H24)=FVAR(1)
5.a Riding coordinates:
 C8(H8A,H8B,H8C), C5(H5A,H5B,H5C)
5.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C28A(H28A), C27A(H27A), C26(H26A), C26(H26), C25A(H25A), C24A(H24A),
  C28(H28), C27(H27), C25(H25), C24(H24), C18(H18), C23(H23), C22(H22),
 C14(H14), C15(H15), C21(H21), C20(H20), C17(H17), C16(H16)
5.c Fitted hexagon refined as free rotating group:
 N3(C28A,C27A,C26,C25A,C24A)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C), C11(H11A,
 H11B,H11C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              83795
_shelx_hkl_checksum              34203
_olex2_submission_special_instructions 'No special instructions were received'