#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:18:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179446 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/43/4334303.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4334303
loop_
_publ_author_name
'Dmitri V. Konarev'
'Manabu Ishikawa'
'Salavat S. Khasanov'
'Akihiro Otsuka'
'Hideki Yamochi'
'Gunzi Saito'
'Rimma N. Lyubovskaya'
_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            'C32 H16 Fe N8'
_chemical_formula_weight         568.38
_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                90.00
_cell_angle_beta                 120.7700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5276(15)
_cell_length_b                   4.7810(5)
_cell_length_c                   19.185(2)
_cell_measurement_reflns_used    4348
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.47
_cell_volume                     1144.9(2)
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13226
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       needle
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0350
_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/[σ²(Fo²)+(0.0651P)²+0.3093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1111
_reflns_number_gt                2396
_reflns_number_total             2951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3025364_si_003_5.cif
_cod_data_source_block           Beta_Fe(Pc)_100K
_cod_original_cell_volume        1145.0(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334303
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.0000 0.0000 0.01175(12) Uani 1 2 d S
N106 N 0.25360(12) 0.0287(3) 0.16165(10) 0.0135(3) Uani 1 1 d .
N105 N 0.07161(13) -0.5224(3) -0.07900(10) 0.0139(3) Uani 1 1 d .
C102 C 0.25603(15) -0.5007(4) 0.03284(11) 0.0138(4) Uani 1 1 d .
N101 N 0.13177(12) -0.1974(3) 0.03319(9) 0.0132(3) Uani 1 1 d .
N102 N 0.07349(12) 0.2201(3) 0.09761(9) 0.0130(3) Uani 1 1 d .
C104 C 0.23058(14) -0.1510(4) 0.10256(11) 0.0133(4) Uani 1 1 d .
C124 C 0.09894(15) 0.7487(4) 0.24599(11) 0.0155(4) Uani 1 1 d .
H124 H 0.0304 0.8517 0.2277 0.019 Uiso 1 1 calc R
C103 C 0.30972(15) -0.3383(4) 0.10264(11) 0.0147(4) Uani 1 1 d .
C107 C 0.10694(15) 0.5423(4) 0.19807(11) 0.0138(4) Uani 1 1 d .
C108 C 0.02819(15) 0.4297(4) 0.11964(11) 0.0136(4) Uani 1 1 d .
C118 C 0.41799(16) -0.7342(4) 0.06700(12) 0.0179(4) Uani 1 1 d .
H118 H 0.4586 -0.8764 0.0551 0.022 Uiso 1 1 calc R
C121 C 0.29389(15) 0.4541(4) 0.29755(12) 0.0163(4) Uani 1 1 d .
H121 H 0.3625 0.3513 0.3157 0.020 Uiso 1 1 calc R
C122 C 0.28614(15) 0.6597(4) 0.34565(11) 0.0177(4) Uani 1 1 d .
H122 H 0.3504 0.7045 0.3996 0.021 Uiso 1 1 calc R
C123 C 0.19051(15) 0.8055(4) 0.32042(11) 0.0173(4) Uani 1 1 d .
H123 H 0.1880 0.9526 0.3564 0.021 Uiso 1 1 calc R
C101 C 0.14499(15) -0.4101(4) -0.00934(11) 0.0138(4) Uani 1 1 d .
C117 C 0.30863(15) -0.7035(4) 0.01346(12) 0.0165(4) Uani 1 1 d .
H117 H 0.2695 -0.8208 -0.0365 0.020 Uiso 1 1 calc R
C119 C 0.47270(16) -0.5707(4) 0.13726(12) 0.0185(4) Uani 1 1 d .
H119 H 0.5515 -0.5982 0.1743 0.022 Uiso 1 1 calc R
C105 C 0.17968(15) 0.1988(4) 0.15883(11) 0.0136(4) Uani 1 1 d .
C106 C 0.20225(15) 0.3972(4) 0.22310(11) 0.0143(4) Uani 1 1 d .
C120 C 0.41950(15) -0.3701(4) 0.15660(11) 0.0169(4) Uani 1 1 d .
H120 H 0.4583 -0.2543 0.2069 0.020 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N102 Fe1 N102 180.0 3 .
N102 Fe1 N101 90.94(7) 3 .
N102 Fe1 N101 89.06(7) . .
N102 Fe1 N101 89.06(7) 3 3
N102 Fe1 N101 90.94(7) . 3
N101 Fe1 N101 180.0 . 3
C104 N106 C105 121.28(16) . .
C108 N105 C101 122.17(16) 3 .
C103 C102 C117 121.97(18) . .
C103 C102 C101 106.62(16) . .
C117 C102 C101 131.41(18) . .
C101 N101 C104 107.28(15) . .
C101 N101 Fe1 125.59(12) . .
C104 N101 Fe1 127.12(13) . .
C108 N102 C105 107.04(15) . .
C108 N102 Fe1 125.54(13) . .
C105 N102 Fe1 127.41(12) . .
N106 C104 N101 127.62(17) . .
N106 C104 C103 123.05(16) . .
N101 C104 C103 109.32(16) . .
C123 C124 C107 117.14(17) . .
C123 C124 H124 121.4 . .
C107 C124 H124 121.4 . .
C102 C103 C120 121.22(18) . .
C102 C103 C104 106.77(16) . .
C120 C103 C104 132.01(18) . .
C124 C107 C106 121.86(18) . .
C124 C107 C108 131.30(17) . .
C106 C107 C108 106.83(16) . .
N105 C108 N102 127.89(17) 3 .
N105 C108 C107 122.15(17) 3 .
N102 C108 C107 109.95(16) . .
C117 C118 C119 121.57(18) . .
C117 C118 H118 119.2 . .
C119 C118 H118 119.2 . .
C122 C121 C106 117.30(18) . .
C122 C121 H121 121.3 . .
C106 C121 H121 121.3 . .
C121 C122 C123 121.65(18) . .
C121 C122 H122 119.2 . .
C123 C122 H122 119.2 . .
C124 C123 C122 121.05(18) . .
C124 C123 H123 119.5 . .
C122 C123 H123 119.5 . .
N105 C101 N101 127.82(17) . .
N105 C101 C102 122.18(17) . .
N101 C101 C102 109.99(16) . .
C118 C117 C102 116.78(18) . .
C118 C117 H117 121.6 . .
C102 C117 H117 121.6 . .
C120 C119 C118 121.35(18) . .
C120 C119 H119 119.3 . .
C118 C119 H119 119.3 . .
N106 C105 N102 127.43(17) . .
N106 C105 C106 122.62(17) . .
N102 C105 C106 109.95(16) . .
C121 C106 C107 120.99(18) . .
C121 C106 C105 132.80(18) . .
C107 C106 C105 106.20(16) . .
C119 C120 C103 117.10(18) . .
C119 C120 H120 121.4 . .
C103 C120 H120 121.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N102 1.9258(15) 3
Fe1 N102 1.9258(15) .
Fe1 N101 1.9272(15) .
Fe1 N101 1.9272(15) 3
N106 C104 1.322(2) .
N106 C105 1.326(2) .
N105 C108 1.323(2) 3
N105 C101 1.324(2) .
C102 C103 1.391(3) .
C102 C117 1.398(3) .
C102 C101 1.452(2) .
N101 C101 1.377(2) .
N101 C104 1.388(2) .
N102 C108 1.378(2) .
N102 C105 1.384(2) .
C104 C103 1.457(3) .
C124 C123 1.392(3) .
C124 C107 1.394(3) .
C124 H124 1.0000 .
C103 C120 1.396(3) .
C107 C106 1.396(3) .
C107 C108 1.450(3) .
C108 N105 1.323(2) 3
C118 C117 1.390(3) .
C118 C119 1.401(3) .
C118 H118 1.0000 .
C121 C122 1.392(3) .
C121 C106 1.393(3) .
C121 H121 1.0000 .
C122 C123 1.401(3) .
C122 H122 1.0000 .
C123 H123 1.0000 .
C117 H117 1.0000 .
C119 C120 1.396(3) .
C119 H119 1.0000 .
C105 C106 1.454(3) .
C120 H120 1.0000 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N102 Fe1 N101 C101 -0.24(15) 3 .
N102 Fe1 N101 C101 179.76(15) . .
N101 Fe1 N101 C101 -53.0(19) 3 .
N102 Fe1 N101 C104 178.53(15) 3 .
N102 Fe1 N101 C104 -1.47(15) . .
N101 Fe1 N101 C104 125.7(19) 3 .
N102 Fe1 N102 C108 -44.1(3) 3 .
N101 Fe1 N102 C108 179.65(15) . .
N101 Fe1 N102 C108 -0.35(15) 3 .
N102 Fe1 N102 C105 135.22(18) 3 .
N101 Fe1 N102 C105 -1.03(15) . .
N101 Fe1 N102 C105 178.97(15) 3 .
C105 N106 C104 N101 -2.0(3) . .
C105 N106 C104 C103 179.01(17) . .
C101 N101 C104 N106 -177.80(18) . .
Fe1 N101 C104 N106 3.3(3) . .
C101 N101 C104 C103 1.3(2) . .
Fe1 N101 C104 C103 -177.64(12) . .
C117 C102 C103 C120 0.3(3) . .
C101 C102 C103 C120 -178.97(17) . .
C117 C102 C103 C104 179.62(17) . .
C101 C102 C103 C104 0.31(19) . .
N106 C104 C103 C102 178.15(17) . .
N101 C104 C103 C102 -1.0(2) . .
N106 C104 C103 C120 -2.7(3) . .
N101 C104 C103 C120 178.16(19) . .
C123 C124 C107 C106 0.1(3) . .
C123 C124 C107 C108 178.64(19) . .
C105 N102 C108 N105 179.59(18) . 3
Fe1 N102 C108 N105 -1.0(3) . 3
C105 N102 C108 C107 -1.2(2) . .
Fe1 N102 C108 C107 178.21(12) . .
C124 C107 C108 N105 1.1(3) . 3
C106 C107 C108 N105 179.82(17) . 3
C124 C107 C108 N102 -178.15(18) . .
C106 C107 C108 N102 0.6(2) . .
C106 C121 C122 C123 -0.4(3) . .
C107 C124 C123 C122 -0.2(3) . .
C121 C122 C123 C124 0.3(3) . .
C108 N105 C101 N101 2.8(3) 3 .
C108 N105 C101 C102 -176.23(17) 3 .
C104 N101 C101 N105 179.79(18) . .
Fe1 N101 C101 N105 -1.2(3) . .
C104 N101 C101 C102 -1.1(2) . .
Fe1 N101 C101 C102 177.85(12) . .
C103 C102 C101 N105 179.64(17) . .
C117 C102 C101 N105 0.4(3) . .
C103 C102 C101 N101 0.5(2) . .
C117 C102 C101 N101 -178.73(18) . .
C119 C118 C117 C102 0.3(3) . .
C103 C102 C117 C118 -0.6(3) . .
C101 C102 C117 C118 178.52(19) . .
C117 C118 C119 C120 0.2(3) . .
C104 N106 C105 N102 -0.9(3) . .
C104 N106 C105 C106 179.53(17) . .
C108 N102 C105 N106 -178.16(17) . .
Fe1 N102 C105 N106 2.4(3) . .
C108 N102 C105 C106 1.4(2) . .
Fe1 N102 C105 C106 -178.01(12) . .
C122 C121 C106 C107 0.3(3) . .
C122 C121 C106 C105 -178.80(19) . .
C124 C107 C106 C121 -0.1(3) . .
C108 C107 C106 C121 -178.99(17) . .
C124 C107 C106 C105 179.16(17) . .
C108 C107 C106 C105 0.3(2) . .
N106 C105 C106 C121 -2.3(3) . .
N102 C105 C106 C121 178.1(2) . .
N106 C105 C106 C107 178.54(17) . .
N102 C105 C106 C107 -1.1(2) . .
C118 C119 C120 C103 -0.5(3) . .
C102 C103 C120 C119 0.2(3) . .
C104 C103 C120 C119 -178.87(19) . .
