Hard single-molecule magnet behavior and strong magnetic coupling in pyrazinyl radical-bridged lanthanide metallocenes
Bajaj, Neha; Mavragani, Niki; Kitos, Alexandros A.; Chartrand, Daniel; Maris, Thierry; Mansikkamäki, Akseli; Murugesu, Muralee; CHEM 10 (2024) 2484–2499; doi:10.1016/j.chempr.2024.04.006

data_1572659
_publ_section_title
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 Hard single-molecule magnet behavior and strong magnetic coupling in
 pyrazinyl radical-bridged lanthanide metallocenes
;
_journal_name_full               CHEM
_journal_page_first              2484
_journal_page_last               2499
_journal_paper_doi               10.1016/j.chempr.2024.04.006
_journal_volume                  10
_journal_year                    2024
_chemical_formula_moiety         'C96 H136 Dy4 N8, 10(C4 H8 O1)'
_chemical_formula_sum            'C136 H216 Dy4 N8 O10'
_chemical_formula_weight         2773.16
_chemical_name_systematic
;
tetrakis(\m-pyrazine radical anion)-octakis(pentamethylcyclopentadienyl)
-tetra-dysprosium(III) tetrahydrofuran solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                62.710(2)
_cell_angle_beta                 89.744(3)
_cell_angle_gamma                78.631(3)
_cell_formula_units_Z            1
_cell_length_a                   13.3406(8)
_cell_length_b                   16.5532(9)
_cell_length_c                   17.2872(9)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.708
_cell_measurement_theta_min      2.686
_cell_volume                     3309.8(3)
_citation_doi                    10.1016/j.chempr.2024.04.006
_computing_cell_refinement
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32559
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.174
_diffrn_reflns_theta_min         2.514
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    11.833
_exptl_absorpt_correction_T_max  0.5122
_exptl_absorpt_correction_T_min  0.2858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1636 before and 0.1004 after correction.
The Ratio of minimum to maximum transmission is 0.5580.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00061(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1372
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     1919
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0682
_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^)+(0.1005P)^2^+3.9387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7129
_reflns_number_total             12520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Dy4.cif
_cod_data_source_block           Dy4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
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_cod_database_code               1572659