New mononuclear Dy(III) complex based on a calix[4]arene ligand with two appended salicylideneamine groups decorated with azophenyl fragments: synthesis, crystalline assembly and slow magnetic relaxation behavior.
Strelnikova, Iuliia V.; Iova, Angelina A.; Ovsyannikov, Alexander S.; Islamov, Daut R.; Litvonov, Igor A.; Lazarenko, Vladimir A.; Kulikova, Elizaveta S.; Bogomyakov, Artem S.; Lin, Meijin; Kiiamov, Airat G.; Solovieva, Svetlana E.; Antipin, Igor S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9584–9593; doi:10.1039/d5dt00936g

data_7718686
_publ_section_title
;
 New mononuclear Dy(III) complex based on a calix[4]arene ligand with two
 appended salicylideneamine groups decorated with azophenyl fragments:
 synthesis, crystalline assembly and slow magnetic relaxation behavior.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9584
_journal_page_last               9593
_journal_paper_doi               10.1039/d5dt00936g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C74 H79 Dy N6 O6, 2(H2 O), C H4 O'
_chemical_formula_sum            'C75 H87 Dy N6 O9'
_chemical_formula_weight         1379.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.127(4)
_cell_length_b                   13.967(3)
_cell_length_c                   26.635(5)
_cell_measurement_reflns_used    123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.809
_cell_measurement_theta_min      1.744
_cell_volume                     7065(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'MarCCD (Ross et al., 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7517
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1306
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11960
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         1.744
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.987
_refine_diff_density_min         -1.714
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.1127
_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^)+(0.0796P)^2^+200.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2708
_refine_ls_wR_factor_ref         0.3244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4505
_reflns_number_total             7014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00936g2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7718685--7718686.cif.'
_cod_original_cell_volume        7064(2)
_cod_database_code               7718686
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.699
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.02
 H8D-H4
 -2.4 with sigma of 0.02
 H8C-H4
 -2.4 with sigma of 0.02
 H1AB-O0AA
 1.96 with sigma of 0.001
 O0AA-H1AA
 -3.2 with sigma of 0.02
 H0AA-O1AA
 -3.2 with sigma of 0.02
 H0AB-O1AA
 -3.2 with sigma of 0.02
 C34-H0AA
 3.277 with sigma of 0.001
 H1AA-C32
 4.735 with sigma of 0.001
 C71-C25 \\sim C25-C67
 with sigma of 0.001
 C21-C16 \\sim C16-C17
 with sigma of 0.001
 C21-C20 \\sim C18-C17
 with sigma of 0.001
 C20-C19 \\sim C19-C18
 with sigma of 0.001
3. Rigid bond restraints
 N1, C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C53, C54, C55
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(O0AA) \\sim Ueq, Uanis(O1AA) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(C44) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C71) = Uanis(C67)
Uanis(C74) = Uanis(C73)
Uanis(C69) = Uanis(C68)
Uanis(C70) = Uanis(C72)
5. Rigid body (RIGU) restrains
 C21, C20, C19, C18, C17, C16, N3, N2, C14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C59, C61, C60, C62
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C63, C65, C66, C64
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C75, C78, C77, C76
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C71, C74, C69, C72, C25, C67, C68, C70, C73
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C38, N4, C37, C36, O3, C35
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C48, C47, C49, C50, C45, C46, N6, N5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C39, C44, C43
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C26, C27, C29, C28
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C4, C5, C6, O1, C7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C42, C43, C41, C44, N5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C71)=Sof(C73)=Sof(H73A)=Sof(H73B)=
 Sof(H73C)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=1-FVAR(1)
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C67)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(H69C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(1)
 Fixed Sof: O0AA(0.5) H0AA(0.5) H0AB(0.5) O1AA(0.5) H1AA(0.5) H1AB(0.5)
7.a Free rotating group:
 O8(H8C,H8D), C70(C67,C69,C68), C74(C71,C73,C72,H4), O0AA(H0AA,H0AB),
 O1AA(H1AA,H1AB)
7.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C29(H29A,H29B), C8(H8A,H8B), C22(H22A,H22B), C51(H51A,H51B),
 C7(H7A,H7B), C36(H36A,H36B), C37(H37A,H37B)
7.c Me refined with riding coordinates:
 C77(H77A,H77B,H77C), C66(H66A,H66B,H66C), C78(H78A,H78B,H78C), C65(H65A,H65B,
 H65C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C62(H62A,
 H62B,H62C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C),
 C74(H74A,H74B,H74C), C73(H73A,H73B,H73C), C72(H72A,H72B,H72C)
7.d Aromatic/amide H refined with riding coordinates:
 C38(H38), C4(H4A), C26(H26), C2(H2), C44(H44), C41(H41), C42(H42), C53(H53),
 C15(H15), C24(H24), C31(H31), C9(H9), C21(H21), C49(H49), C55(H55), C18(H18),
 C48(H48), C17(H17), C12(H12), C33(H33), C20(H20), C50(H50), C19(H19), C46(H46),
  C13(H13), C47(H47)
7.e Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C76(H76A,H76B,H76C)
7.f Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              8511
_shelx_hkl_checksum              42980
_olex2_submission_special_instructions 'No special instructions were received'