Observation of magnetic interactions between localized 4f- and itinerant π-electrons in a single crystal of cationic bisphthalocyanine complexes containing diluted spin centres
Fukuda, Takamitsu; Onodera, Shun; Watanabe, Hirohito; Shirasaki, Kenji; Fuyuhiro, Akira; Yamamura, Tomoo; Ishikawa, Naoto; Dalton Trans.  (2017) –; doi:10.1039/C7DT02656K

data_7044009
_publ_section_title
;
 Observation of magnetic interactions between localized 4f- and itinerant
 \p-electrons in a single crystal of cationic bisphthalocyanine complexes
 containing diluted spin centres
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02656K
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C64 H32 B F4 N16 Tb0.05 Y0.95'
_chemical_formula_sum            'C64 H32 B F4 N16 Tb0.05 Y0.95'
_chemical_formula_weight         1204.27
_chemical_name_systematic        '[Pc2Y0.95Tb0.05]BF4'
_space_group_crystal_system      tetragonal
_space_group_IT_number           104
_space_group_name_Hall           'P 4 -2n'
_space_group_name_H-M_alt        'P 4 n c'
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   19.5834(7)
_cell_length_b                   19.5834(7)
_cell_length_c                   6.4890(2)
_cell_measurement_reflns_used    18839
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.12
_cell_volume                     2488.59(15)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            24703
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         3.290
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1218.60
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details
;
 Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2791
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2560
_reflns_number_total             2791
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7dt02656k2.cif
_cod_data_source_block           Y-Tb-Pc-BF4
_cod_original_cell_volume        2488.62(14)
_cod_database_code               7044009
_shelx_res_checksum              42182