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_1572713
_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         'C49 H53 Dy N2 O6'
_chemical_formula_sum            'C49 H53 Dy N2 O6'
_chemical_formula_weight         928.43
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-11
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.3790(7)
_cell_length_b                   12.3790(7)
_cell_length_c                   51.501(4)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.24
_cell_volume                     6834.7(8)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            59205
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.900
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0877 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.8921.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             2850
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3952 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         9181
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0175P)^2^+0.5903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0445
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                8671
_reflns_number_total             9181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02179g2.cif
_cod_data_source_block           qyy_1_pl
_cod_depositor_comments
'Adding full bibliography for 1572711--1572713.cif.'
_cod_original_cell_volume        6834.7(9)
_cod_database_code               1572713
_shelx_shelxl_version_number     2019/1
_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. Rigid bond restraints
 C10, C11, C12, C13, C11A, C12A, C13A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C23, C24, C25, C26, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12 \\sim C13 \\sim C11A \\sim C12A \\sim C13A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C24A \\sim C25A \\sim C26A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Same fragment restrains
{C9, C10, C11A, C12A, C13A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C9, C10, C11, C12, C13}
{C22, C23, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C22, C23, C24, C25, C26}
5. Others
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 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)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
6.a Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C24(H24A,H24B,H24C)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C34(H34), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47),
 C48(H48), C49(H49)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C11A(H11D,H11E,H11F), C12A(H12D,
 H12E,H12F), C13A(H13D,H13E,H13F), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              57032
_shelx_hkl_checksum              59685
_olex2_submission_special_instructions 'No special instructions were received'