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_1567542
_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 Y'
_chemical_formula_sum            'C25 H37 Y'
_chemical_formula_weight         427.478
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-23
_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                 99.1673(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1312(3)
_cell_length_b                   21.6836(6)
_cell_length_c                   10.1764(3)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.63
_cell_volume                     2207.01(11)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8965
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.8965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41069
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.8965
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         33.06
_diffrn_reflns_theta_min         1.88
_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    2.677
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5914
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       plate
_exptl_crystal_F_000             893.068
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.3047
_refine_diff_density_min         -0.7787
_refine_diff_density_rms         0.1629
_refine_ls_d_res_high            0.6515
_refine_ls_d_res_low             10.8418
_refine_ls_goodness_of_fit_ref   1.0356
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7506
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.0316
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -15
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -9
_reflns_number_gt                5413
_reflns_number_total             7506
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc02560d2.cif
_cod_data_source_block           COTYCpttt_0m
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1567542
_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
 C2-H2 \\sim C5-H5
 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
;
_olex2_submission_special_instructions 'No special instructions were received'