Synthesis, Structural and Magnetic Properties of Ternary Complexes of (Me4P+).{[Fe(I)Pc(-2)]-}.Triptycene and (Me4P+).{[Fe(I)Pc(-2)]-}.(N,N,N',N'-Tetrabenzyl-p-phenylenediamine)0.5 with Iron(I) Phthalocyanine Anions
Dmitri V. Konarev; Manabu Ishikawa; Salavat S. Khasanov; Akihiro Otsuka; Hideki Yamochi; Gunzi Saito; Rimma N. Lyubovskaya; Inorganic Chemistry 52 (2013) 3851–3859; doi:10.1021/ic3025364

data_4334301
_publ_contact_author_address
;
Institute of Problems of Chemical Physics, RAS,
Chernogolovka, 142432, Russia
;
_publ_contact_author_email       konarev@icp.ac.ru
_publ_contact_author_name        'Konarev, Dmitri V.'
_publ_section_title
;
 Synthesis, Structural and Magnetic Properties of Ternary Complexes of
 (Me4P+).{[Fe(I)Pc(-2)]-}.Triptycene and
 (Me4P+).{[Fe(I)Pc(-2)]-}.(N,N,N',N'-Tetrabenzyl-p-phenylenediamine)0.5
 with Iron(I) Phthalocyanine Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3851
_journal_page_last               3859
_journal_paper_doi               10.1021/ic3025364
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C53 H44 Fe N9 P'
_chemical_formula_weight         893.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.535(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.091(2)
_cell_length_b                   12.6449(19)
_cell_length_c                   25.604(4)
_cell_measurement_reflns_used    811
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.51
_cell_measurement_theta_min      2.65
_cell_volume                     4210.8(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    sir2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1380
_diffrn_reflns_av_sigmaI/netI    0.2295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19713
_diffrn_reflns_theta_full        24.83
_diffrn_reflns_theta_max         24.83
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_correction_T_min  0.7911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.754
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                3119
_reflns_number_total             7282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3025364_si_003_3.cif
_cod_data_source_block           FePc_Me4P_TBPDA_100K
_cod_original_cell_volume        4211.0(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4334301