Cyclooctatetraenide-based single-ion magnets featuring bulky cyclopentadienyl ligand
Korzyński, Maciej Damian; Bernhardt, Moritz; Romankov, Vladyslav; Dreiser, Jan; Matmon, Guy; Pointillart, Fabrice; Le Guennic, Boris; Cador, Olivier; Copéret, Christophe; Chemical Science  (2022) –; doi:10.1039/D2SC02560D

data_1567545
_publ_section_title
;
 Cyclooctatetraenide-based single-ion magnets featuring bulky
 cyclopentadienyl ligand
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC02560D
_journal_year                    2022
_chemical_formula_moiety         'C25 H37 Dy'
_chemical_formula_sum            'C25 H37 Dy'
_chemical_formula_weight         500.04
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-04 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.224(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1186(8)
_cell_length_b                   21.6751(17)
_cell_length_c                   10.1771(8)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.23
_cell_volume                     2203.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            113975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.197
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.397
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SAFABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1661 before and 0.0944 after correction. The Ratio of minimum to maximum transmission is 0.7449. The \I/2 correction factor is NOT present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             1012
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+0.6130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5601
_reflns_number_total             6739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02560d2.cif
_cod_data_source_block           cotdycpttt_0m
_cod_database_code               1567545
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Restrained distances
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C1
 with sigma of 0.02
 C6-C7 \\sim C7-C8 \\sim C8-C9 \\sim C9-C10 \\sim C10-C11 \\sim C11-C12 \\sim
C12-C13 \\sim C13-C6
 with sigma of 0.02
 C5-H5 \\sim C2-H2
 with sigma of 0.02
 C6-H6 \\sim C7-H7 \\sim C8-H8 \\sim C9-H9 \\sim C10-H10 \\sim C11-H11 \\sim
C12-H12 \\sim C13-H13
 with sigma of 0.02
2. Restrained planarity
 C1, C2, C3, C4, C5
 with sigma of 0.1
 C6, C7, C8, C9, C10, C11, C12, C13
 with sigma of 0.1
3. Rigid bond restraints
 C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7, C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
;
_shelx_res_checksum              3702
_olex2_submission_special_instructions 'No special instructions were received'