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_7133834
_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_sum            'C54.25 H60.5 Cl2.5 Dy F6 N6 O2 P Si2'
_chemical_formula_weight         1280.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8869(6)
_cell_length_b                   11.3031(4)
_cell_length_c                   23.5314(8)
_cell_measurement_reflns_used    31062
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.025
_cell_volume                     5488.7(3)
_computing_cell_refinement       'CrystalClear, Rigaku MSC< 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC< 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC< 2005'
_computing_molecular_graphics    'Diamond ver.3.2'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23012
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.024
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       paralelepiped
_exptl_crystal_F_000             2598
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         4.689
_refine_diff_density_min         -4.070
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.539(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         23012
_refine_ls_number_restraints     2198
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+23.9876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                20201
_reflns_number_total             23012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04551c2.cif
_cod_data_source_block           compound
_cod_depositor_comments
'Adding full bibliography for 7133834--7133835.cif.'
_cod_original_sg_symbol_H-M      'P n'
_cod_original_formula_sum        'C54.25 H60.50 Cl2.50 Dy F6 N6 O2 P Si2'
_cod_database_code               7133834
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.868
_diffrn_reflns_v_r_equivalents   0.0593
_shelxl_version_number           2014/6
_shelx_res_checksum              88616
_shelx_hkl_checksum              75117
_shelx_fab_checksum              65672