The effect of magnetic coupling along the magnetic axis on slow magnetic relaxation in Dy<sup>III</sup> complexes with <i>D</i><sub>5h</sub> configuration based on an aggregation-induced-emission-active ligand.
Yao, Min-Xia; Gao, Yu-Qi; An, Zhong-Wu; Zhu, Dong-Mei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5133–5146; doi:10.1039/d3dt04257j

data_7715118
_publ_section_title
;
 The effect of magnetic coupling along the magnetic axis on slow magnetic
 relaxation in Dy<sup>III</sup> complexes with <i>D</i><sub>5h</sub>
 configuration based on an aggregation-induced-emission-active ligand.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5133
_journal_page_last               5146
_journal_paper_doi               10.1039/d3dt04257j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C90 H98.852 Cl2 Dy2 N6 O6 P2, 1.148(H), 2(C2 H3 N), 2(O)'
_chemical_formula_sum            'C94 H106 Cl2 Dy2 N8 O8 P2'
_chemical_formula_weight         1933.70
_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
_audit_creation_date             2023-06-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2024-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                65.090(2)
_cell_angle_beta                 82.000(2)
_cell_angle_gamma                74.102(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7971(5)
_cell_length_b                   13.9098(7)
_cell_length_c                   16.1086(7)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.30
_cell_volume                     2304.88(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.00
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43370
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.121
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6135
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1213 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.8228.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.121
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9052
_refine_ls_number_restraints     1306
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0999P)^2^+2.4436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7282
_reflns_number_total             9052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04257j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715118--7715122.cif.'
_cod_database_code               7715118
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.766
_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
 C10-O4
 2.43 with sigma of 0.001
 C39-C41 = C39A-C41A
 2.5636 with sigma of 0.01
 C40-C41 = C40A-C41A
 1.5334 with sigma of 0.005
 N4-C48
 1.1624 with sigma of 0.005
 C34-C35 = C34A-C35A
 1.5334 with sigma of 0.005
 N4-C47
 2.6158 with sigma of 0.005
 C47-C48
 1.4534 with sigma of 0.005
 C38-C39 = C38A-C39A
 1.5334 with sigma of 0.005
 C34-C36 = C34A-C36A
 2.5636 with sigma of 0.005
 C38-C40 = C38A-C40A
 2.5636 with sigma of 0.005
 C35-C36 = C35A-C36A
 1.5348 with sigma of 0.005
 C39-C40 = C39A-C40A
 1.5348 with sigma of 0.005
 C35-C37 = C35A-C37A
 2.5636 with sigma of 0.005
 C36-C37 = C36A-C37A
 1.5334 with sigma of 0.005
3. Rigid bond restraints
 O4, O4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C47, C48, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 P1, C42
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C35A \\sim C36 \\sim C36A \\sim C37 \\sim C37A \\sim
C38 \\sim C38A \\sim C39 \\sim C39A \\sim C40 \\sim C40A \\sim C41 \\sim C41A
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C34A \\sim C47 \\sim C48: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
O4 \\sim O4A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C47 \\sim C48 \\sim N4: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=
 Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41D)=
 Sof(H41E)=Sof(H41F)=Sof(C34A)=Sof(H34C)=Sof(H)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=FVAR(1)
 Sof(O4A)=1-FVAR(2)
 Sof(O4)=FVAR(2)
6.a Riding coordinates:
 C41(H41A,H41B,H41C), C41A(H41D,H41E,H41F), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C)
6.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C35A(H35C,H35D), C36(H36A,H36B), C36A(H36C,
 H36D), C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D),
 C40(H40A,H40B), C40A(H40C,H40D), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C34A(H34C,H)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
6.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C37A(H37D,H37E,H37F)
;
_shelx_res_checksum              31414
_olex2_submission_special_instructions 'No special instructions were received'