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_7715119
_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         '1.988(C85 H66 Cl2 Dy2 N6 O6 P)'
_chemical_formula_sum            'C169 H131 Cl4 Dy4 N12 O12 P2'
_chemical_formula_weight         3375.59
_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             2023-05-31
_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                83.682(4)
_cell_angle_beta                 84.689(5)
_cell_angle_gamma                78.406(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2499(16)
_cell_length_b                   18.894(2)
_cell_length_c                   36.404(5)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.02
_cell_volume                     7514.2(17)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            97170
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.822
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             3374
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1894
_refine_ls_number_reflns         28941
_refine_ls_number_restraints     547
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0548
_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^)+31.8713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20157
_reflns_number_total             28941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04257j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715118--7715122.cif.'
_cod_original_cell_volume        7514.3(17)
_cod_database_code               7715119
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 P2-C158 = P2-C1A
 1.8 with sigma of 0.01
 P2-C165 = P2-C8A
 1.8 with sigma of 0.01
 O12-H12B
 0.85 with sigma of 0.01
 Dy1-H12B
 2.885928 with sigma of 0.02
 C170-H12B
 1.877342 with sigma of 0.02
3. Rigid bond restraints
 C7A, C8A, C9A, C10A, C11A, C12A, C164, C165, C166, C167, C168, C169
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C75, C76, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C158, C159, C160, C161, C162, C163, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C69, C70, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C164 \\sim C165
\\sim C166 \\sim C167 \\sim C168 \\sim C169: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C158 \\sim C159 \\sim C160 \\sim C161 \\sim C162 \\sim C163 \\sim C1A \\sim C2A
\\sim C3A \\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
Uanis(C158) \\sim Ueq, Uanis(C159) \\sim Ueq, Uanis(C160) \\sim Ueq,
Uanis(C161) \\sim Ueq, Uanis(C162) \\sim Ueq, Uanis(C163) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C158)=Sof(C159)=Sof(H159)=Sof(C160)=Sof(H160)=Sof(C161)=Sof(H161)=
 Sof(C162)=Sof(H162)=Sof(C163)=Sof(H163)=FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10C)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=1-FVAR(2)
 Sof(C164)=Sof(H164)=Sof(C165)=Sof(C166)=Sof(H166)=Sof(C167)=Sof(H167)=
 Sof(C168)=Sof(H168)=Sof(C169)=Sof(H169)=FVAR(2)
6.a Riding coordinates:
 O10(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N8(H8), N11(H11), C1(H1), C2(H2B), C3(H3), C4(H4), C5(H5), C10(H10),
 C11(H11B), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52),
  C53(H53), C54(H54), C56(H56), C59(H59), C60(H60), C61(H61), C64(H64),
 C65(H65), C66(H66), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C89(H89), C90(H90), C91(H91), C95(H95), C96(H96),
  C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102), C103(H103),
 C104(H104), C105(H105), C106(H106), C108(H108), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C119(H119),
 C120(H120), C121(H121), C123(H123), C127(H127), C128(H128), C129(H129),
 C130(H130), C131(H131), C132(H132), C133(H133), C134(H134), C135(H135),
 C136(H136), C137(H137), C140(H140), C143(H143), C144(H144), C145(H145),
 C148(H148), C149(H149), C150(H150), C151(H151), C153(H153), C154(H154),
 C155(H155), C156(H156), C157(H157), C159(H159), C160(H160), C161(H161),
 C162(H162), C163(H163), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
 C164(H164), C166(H166), C167(H167), C168(H168), C169(H169), C7A(H7A), C9A(H9A),
  C10A(H10C), C11A(H11A), C12A(H12A)
6.c Fitted hexagon refined as free rotating group:
 C158(C159,C160,C161,C162,C163), C1A(C2A,C3A,C4A,C5A,C6A), C164(C165,C166,C167,
 C168,C169), C7A(C8A,C9A,C10A,C11A,C12A)
6.d Idealised Me refined as rotating group:
 C170(H17A,H17B,H17C)
;
_shelx_res_checksum              76447
_olex2_submission_special_instructions 'No special instructions were received'