Slow magnetic relaxation and strong magnetic coupling in the nitroxyl radical complexes of lanthanide(iii) with diamagnetic ground state (Ln = Lu, Eu).
Sorace, Lorenzo; Dmitriev, Alexey A.; Perfetti, Mauro; Vostrikova, Kira E.; Chemical science 16 (2024) 218–232; doi:10.1039/d4sc05035e

data_1573299
_publ_section_title
;
 Slow magnetic relaxation and strong magnetic coupling in the nitroxyl
 radical complexes of lanthanide(iii) with diamagnetic ground state (Ln =
 Lu, Eu).
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              218
_journal_page_last               232
_journal_paper_doi               10.1039/d4sc05035e
_journal_volume                  16
_journal_year                    2024
_chemical_formula_moiety         'C15 H16 Lu N6 O11'
_chemical_formula_sum            'C15 H16 Lu N6 O11'
_chemical_formula_weight         631.31
_chemical_properties_physical    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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-26 deposited with the CCDC.	2024-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9511(2)
_cell_length_b                   16.4632(4)
_cell_length_c                   12.8156(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.45
_cell_volume                     2036.39(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26385
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.053
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.922
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.7663.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0149
_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^)+1.7579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3835
_reflns_number_total             4001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05035e2.cif
_cod_data_source_block           kv954_Lu
_cod_depositor_comments
'Adding full bibliography for 1573298--1573299.cif.'
_cod_database_code               1573299
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.526
_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.a Secondary CH2 refined with riding coordinates:
 C00R(H00D,H00E)
2.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00N(H00N), C00Q(H00Q), C00S(H00S), C00V(H00V),
 C00W(H00W), C00X(H00X)
2.c Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00U(H00F,H00G,H00H)
;
_shelx_res_checksum              11623
_shelx_hkl_checksum              31627
_olex2_submission_special_instructions 'No special instructions were received'