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_1567547
_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         'C29 H45 Nd O'
_chemical_formula_sum            'C29 H45 Nd O'
_chemical_formula_weight         553.916
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-04 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3040(4)
_cell_length_b                   15.4886(3)
_cell_length_c                   18.7216(4)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.44
_cell_volume                     5307.64(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_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 0.9994
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f 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  0.0877
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            309546
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9994
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         2.04
_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    1.973
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1282 before and 0.0721 after correction. The Ratio of minimum to maximum transmission is 0.7242. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear greenish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296.870
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.4424
_refine_diff_density_min         -1.3177
_refine_diff_density_rms         0.1653
_refine_ls_d_res_high            0.6700
_refine_ls_d_res_low             9.9969
_refine_ls_goodness_of_fit_ref   1.1344
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9241
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.1308
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0034P)^2^+7.4367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0399
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7173
_reflns_number_total             9241
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2sc02560d2.cif
_cod_data_source_block           COTNdCptttTHF
_cod_database_code               1567547
_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
;
_olex2_exptl_crystal_mounting_method Oil
_olex2_submission_special_instructions 'No special instructions were received'