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_4334299
_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_moiety         'C32 H16 N8 FE1, C4 H12 P1, C20 H14'
_chemical_formula_sum            'C56 H42 Fe N8 P'
_chemical_formula_weight         913.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 93.022(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   18.086(5)
_cell_length_b                   25.771(5)
_cell_length_c                   19.180(5)
_cell_measurement_reflns_used    2300
_cell_measurement_temperature    280(1)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     8927(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      280(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3294
_diffrn_reflns_av_sigmaI/netI    0.5437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22738
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9958
_exptl_absorpt_correction_T_min  0.9015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         10771
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.3704
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.2941
_reflns_number_gt                2339
_reflns_number_total             10771
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3025364_si_003_1.cif
_cod_data_source_block           FePc_Me4P_TPC
_cod_original_formula_sum        'C56 H42 Fe1 N8 P1'
_cod_database_code               4334299