Enhancing the single-molecule magnetic performance of β-diketonate Dy(III) complexes by modulating the coordination microenvironment and magnetic interaction: from a mononuclear to a dinuclear structure.
Wang, Yafu; Zeng, Zhaopeng; Luo, Shuchang; Guo, Yan; Liu, Xiangyu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17272–17280; doi:10.1039/d4dt02179g

data_1572711
_publ_section_title
;
 Enhancing the single-molecule magnetic performance of &#x3b2;-diketonate
 Dy(III) complexes by modulating the coordination microenvironment and
 magnetic interaction: from a mononuclear to a dinuclear structure.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17272
_journal_page_last               17280
_journal_paper_doi               10.1039/d4dt02179g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C43 H48 Dy N2 O6'
_chemical_formula_sum            'C43 H48 Dy N2 O6'
_chemical_formula_weight         851.33
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2024-04-01 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                104.710(4)
_cell_angle_beta                 90.508(4)
_cell_angle_gamma                116.886(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4689(18)
_cell_length_b                   12.5848(17)
_cell_length_c                   15.1880(18)
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      51.316
_cell_measurement_theta_min      6.245
_cell_volume                     2034.7(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32561
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.728
_diffrn_reflns_theta_min         2.155
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6924
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.7927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6979
_reflns_number_total             7586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02179g2.cif
_cod_data_source_block           qyy19-1
_cod_depositor_comments
'Adding full bibliography for 1572711--1572713.cif.'
_cod_database_code               1572711
_shelx_shelxl_version_number     2018/3
_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
 C30-C28 \\sim C30A-C28 \\sim C29A-C28 \\sim C29-C28 \\sim C28-C27A \\sim
C28-C27
 with sigma of 0.02
 C30A-C29A \\sim C30A-C27A \\sim C29A-C27A
 with sigma of 0.02
 C16A-C15 \\sim C16-C15 \\sim C15-C14A \\sim C15-C14 \\sim C17A-C15 \\sim
C17-C15
 with sigma of 0.02
 C16A-C14A \\sim C17A-C14A \\sim C17A-C16A
 with sigma of 0.02
3. Rigid bond restraints
 C28, C30A, C27, C27A, C29, C29A, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16, C14A, C14, C17A, C17, C16A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C5, C1, C2, C3, C4, C2A, C3A, C4A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C28 \\sim C30A \\sim C27 \\sim C27A \\sim C29 \\sim C29A \\sim C30: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C16 \\sim C16A \\sim C17 \\sim C17A \\sim C14 \\sim C14A \\sim C15: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C5 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C2A \\sim C3A \\sim C4A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
5. Same fragment restrains
{C5, C1, C2A, C3A, C4A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C5, C1, C2, C3, C4}
6. Others
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(3)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C46(H46), C6(H6), C8(H8), C10(H10), C11(H11), C45(H45), C12(H12),
 C13(H13), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C34(H34), C35(H35),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41)
7.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C2A(H2AA,H2AB,H2AC),
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C30A(H30D,H30E,H30F), C27A(H27D,H27E,H27F), C29A(H29D,H29E,H29F),
 C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C14A(H14D,H14E,H14F)
;
_shelx_res_checksum              78159
_shelx_hkl_checksum              56029
_olex2_submission_special_instructions 'No special instructions were received'