Unveiling new [1+1] Schiff-base macrocycles towards high energy-barrier hexagonal bipyramidal Dy(III) single-molecule magnets.
Armenis, Alexandros S.; Mondal, Arpan; Giblin, Sean R.; Raptopoulou, Catherine P.; Psycharis, Vassilis; Alexandropoulos, Dimitris I.; Tang, Jinkui; Layfield, Richard A.; Stamatatos, Theocharis C.; Chemical communications (Cambridge, England) 60 (2024) 12730–12733; doi:10.1039/d4cc04551c

data_7133835
_publ_section_title
;
 Unveiling new [1+1] Schiff-base macrocycles towards high energy-barrier
 hexagonal bipyramidal Dy(III) single-molecule magnets.
;
_journal_issue                   87
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12730
_journal_page_last               12733
_journal_paper_doi               10.1039/d4cc04551c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C53 H55 Dy N3 O5 Si2, F6 P'
_chemical_formula_sum            'C53 H55 Dy F6 N3 O5 P Si2'
_chemical_formula_weight         1177.65
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-13 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.425(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.895(3)
_cell_length_b                   14.733(3)
_cell_length_c                   20.760(4)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      66.633
_cell_measurement_theta_min      4.295
_cell_volume                     5124.1(17)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32297
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.628
_diffrn_reflns_theta_max         66.628
_diffrn_reflns_theta_min         2.637
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    9.160
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1021 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.6832.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.458
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0535P)^2^+0.7332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7878
_reflns_number_total             8909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04551c2.cif
_cod_data_source_block           cu_230210c_0m
_cod_depositor_comments
'Adding full bibliography for 7133834--7133835.cif.'
_cod_original_cell_volume        5124.3(15)
_cod_database_code               7133835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.711
_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-C15
 1.23 with sigma of 0.02
 C42-C16
 1.23 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C23(H23A,H23B), C29(H29A,H29B), C38(H38A,H38B), C41(H41A,H41B),
 C44(H44A,H44B), C46(H46A,H46B), C50(H50A,H50B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C14(H14),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C31(H31), C33(H33), C35(H35), C37(H37),
 C39(H39), C40(H40), C43(H43), C45(H45), C47(H47), C48(H48), C49(H49), C51(H51),
  C52(H52), C53(H53)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              65954
_shelx_hkl_checksum              36906
_olex2_submission_special_instructions 'No special instructions were received'