Improving the performance of β-diketonate-based Dy<sup>III</sup> single-molecule magnets displaying luminescence thermometry.
Bispo-Jr, Airton Germano; Yeh, Laurence; Errulat, Dylan; Gálico, Diogo Alves; Sigoli, Fernando Aparecido; Murugesu, Muralee; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc02148c

data_7131742
_publ_section_title
;
 Improving the performance of &#x3b2;-diketonate-based Dy<sup>III</sup>
 single-molecule magnets displaying luminescence thermometry.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc02148c
_journal_year                    2023
_chemical_formula_moiety         'C23 H27 Dy N4 O6, C H4 O'
_chemical_formula_sum            'C24 H31 Dy N4 O7'
_chemical_formula_weight         650.03
_chemical_name_systematic
'tris(acetylacetonato)(2,2'-bipyrimidine)dysprosium(III) methanol solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-23 deposited with the CCDC.	2023-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                94.788(2)
_cell_angle_beta                 105.748(2)
_cell_angle_gamma                94.997(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2135(4)
_cell_length_b                   9.3766(5)
_cell_length_c                   16.6513(8)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.19
_cell_volume                     1370.64(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40789
_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         27.999
_diffrn_reflns_theta_min         1.279
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0520 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.9431.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             650
_exptl_crystal_preparation
'Dy(acac)3 2H2O (627 mg, 1.26 mmol) is added to 30 mL of methanol and the mixture is sonicated for 20 minutes. The resulting colorless suspension is filtered through celite, and the filtrate is then mixed with a clear, 10-mL methanoic solution of bpm (200 mg, 1.26 mmol). The reaction mixture is then sonicated for 10 minutes,Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method
'The reaction mixture is left at zero degree Celsius to slowly evaporate. In two days, colourless blocks of single crystals were observed (10% yield).'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0225P)^2^+0.2547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5887
_reflns_number_total             6622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02148c2.cif
_cod_data_source_block           de_s1257_0m
_cod_database_code               7131742
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.581
_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, All O(H) groups
2. Restrained distances
 O7-H1
 0.86 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C16(H16), C8(H8), C18(H18), C17(H17), C13(H13), C22(H22), C23(H23),
 C3(H3)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,
 H15C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              83073
_shelx_hkl_checksum              86315
_olex2_exptl_crystal_mounting_method
'The crystal is covered with paraffin oil and mounted on a 200 um MiTeGen microloop.'
_olex2_submission_special_instructions 'No special instructions were received'