#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:57:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180457 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/26/7212680.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_7212680
loop_
_publ_author_name
'Janczak, Jan'
'Kubiak, Ryszard'
_publ_section_title
;
 Pyrazine control of the supramolecular chemistry of iron(ii) and
 cobalt(ii) phthalocyanines
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3599
_journal_paper_doi               10.1039/c003440a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C40 H24 Fe N12'
_chemical_formula_sum            'C40 H24 Fe N12'
_chemical_formula_weight         728.56
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.26(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5301(19)
_cell_length_b                   19.6721(37)
_cell_length_c                   9.1369(18)
_cell_measurement_reflns_used    1625
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.52
_cell_volume                     1596.4(5)
_computing_cell_refinement
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_data_collection
;
Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6
;
_computing_data_reduction
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17887
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_correction_T_min  0.8713
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      1.51
_exptl_crystal_density_method    floatation
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0230P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                2086
_reflns_number_total             3533
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c003440a.txt
_cod_data_source_block           Fe_Comp_I
_cod_original_cell_volume        1596.4(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7212680
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 0.5000 0.5000 0.5000 0.02685(12) Uani 1 2 d S
N1 N 0.44851(16) 0.55818(7) 0.64335(16) 0.0267(4) Uani 1 1 d .
N2 N 0.23044(17) 0.61613(7) 0.46211(18) 0.0297(4) Uani 1 1 d .
N3 N 0.33265(16) 0.53587(7) 0.32552(16) 0.0270(4) Uani 1 1 d .
N4 N 0.35854(18) 0.47308(8) 0.10856(17) 0.0320(4) Uani 1 1 d .
C1 C 0.5239(2) 0.56268(9) 0.8034(2) 0.0286(4) Uani 1 1 d .
C2 C 0.4544(2) 0.61481(9) 0.8672(2) 0.0308(5) Uani 1 1 d .
C3 C 0.4892(2) 0.64005(10) 1.0186(2) 0.0418(5) Uani 1 1 d .
H3 H 0.5698 0.6230 1.1027 0.050 Uiso 1 1 calc R
C4 C 0.3996(3) 0.69121(10) 1.0390(3) 0.0469(6) Uani 1 1 d .
H4 H 0.4201 0.7088 1.1390 0.056 Uiso 1 1 calc R
C5 C 0.2788(2) 0.71735(10) 0.9139(2) 0.0436(6) Uani 1 1 d .
H5 H 0.2210 0.7522 0.9318 0.052 Uiso 1 1 calc R
C6 C 0.2441(2) 0.69233(9) 0.7642(2) 0.0361(5) Uani 1 1 d .
H6 H 0.1635 0.7095 0.6803 0.043 Uiso 1 1 calc R
C7 C 0.3338(2) 0.64057(9) 0.7429(2) 0.0297(5) Uani 1 1 d .
C8 C 0.3313(2) 0.60399(9) 0.6037(2) 0.0274(4) Uani 1 1 d .
C9 C 0.23295(19) 0.58504(9) 0.3334(2) 0.0273(4) Uani 1 1 d .
C10 C 0.1264(2) 0.60057(9) 0.1772(2) 0.0295(5) Uani 1 1 d .
C11 C 0.0076(2) 0.64587(10) 0.1224(2) 0.0389(5) Uani 1 1 d .
H11 H -0.0181 0.6739 0.1908 0.047 Uiso 1 1 calc R
C12 C -0.0710(2) 0.64796(11) -0.0369(3) 0.0469(6) Uani 1 1 d .
H12 H -0.1514 0.6779 -0.0768 0.056 Uiso 1 1 calc R
C13 C -0.0329(2) 0.60633(11) -0.1390(2) 0.0460(6) Uani 1 1 d .
H13 H -0.0884 0.6089 -0.2461 0.055 Uiso 1 1 calc R
C14 C 0.0849(2) 0.56137(10) -0.0854(2) 0.0385(5) Uani 1 1 d .
H14 H 0.1100 0.5334 -0.1543 0.046 Uiso 1 1 calc R
C15 C 0.1648(2) 0.55903(9) 0.0742(2) 0.0300(5) Uani 1 1 d .
C16 C 0.2940(2) 0.51913(9) 0.1698(2) 0.0285(5) Uani 1 1 d .
N5 N 0.36760(17) 0.42625(7) 0.53246(16) 0.0280(4) Uani 1 1 d .
C17 C 0.2370(2) 0.43916(10) 0.5515(2) 0.0362(5) Uani 1 1 d .
H17 H 0.2058 0.4841 0.5495 0.043 Uiso 1 1 calc R
C18 C 0.1479(2) 0.38841(11) 0.5740(2) 0.0469(6) Uani 1 1 d .
H18 H 0.0592 0.4006 0.5877 0.056 Uiso 1 1 calc R
N6 N 0.1818(2) 0.32308(9) 0.5773(2) 0.0555(5) Uani 1 1 d .
C19 C 0.3106(3) 0.31084(11) 0.5581(2) 0.0537(6) Uani 1 1 d .
H19 H 0.3405 0.2658 0.5591 0.064 Uiso 1 1 calc R
C20 C 0.4028(2) 0.36044(10) 0.5367(2) 0.0381(5) Uani 1 1 d .
H20 H 0.4921 0.3478 0.5248 0.046 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
_geom_angle_publ_flag
N1 Fe1 N1 180.0 . 3_666 y
N1 Fe1 N3 89.63(6) . 3_666 y
N1 Fe1 N3 90.37(6) 3_666 3_666 y
N1 Fe1 N3 90.37(6) . . y
N1 Fe1 N3 89.63(6) 3_666 . y
N3 Fe1 N3 180.0 3_666 . y
N1 Fe1 N5 89.99(6) . 3_666 y
N1 Fe1 N5 90.01(6) 3_666 3_666 y
N3 Fe1 N5 90.62(6) 3_666 3_666 y
N3 Fe1 N5 89.38(6) . 3_666 y
N1 Fe1 N5 90.01(6) . . y
N1 Fe1 N5 89.99(6) 3_666 . y
N3 Fe1 N5 89.38(6) 3_666 . y
N3 Fe1 N5 90.62(6) . . y
N5 Fe1 N5 180.0 3_666 . y
C8 N1 C1 107.35(14) . . ?
C8 N1 Fe1 126.18(12) . . ?
C1 N1 Fe1 126.46(12) . . ?
C8 N2 C9 122.69(16) . . ?
C16 N3 C9 106.96(15) . . ?
C16 N3 Fe1 126.68(12) . . ?
C9 N3 Fe1 126.32(12) . . ?
C1 N4 C16 121.82(16) 3_666 . ?
N4 C1 N1 127.81(16) 3_666 . ?
N4 C1 C2 122.76(17) 3_666 . ?
N1 C1 C2 109.43(16) . . ?
C7 C2 C3 120.79(18) . . ?
C7 C2 C1 107.02(16) . . ?
C3 C2 C1 132.19(18) . . ?
C4 C3 C2 117.3(2) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
C3 C4 C5 121.86(19) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
C6 C5 C4 120.84(19) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 117.61(19) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
C2 C7 C6 121.55(17) . . ?
C2 C7 C8 106.33(16) . . ?
C6 C7 C8 132.10(18) . . ?
N2 C8 N1 127.40(16) . . ?
N2 C8 C7 122.74(17) . . ?
N1 C8 C7 109.84(16) . . ?
N2 C9 N3 127.01(17) . . ?
N2 C9 C10 122.71(16) . . ?
N3 C9 C10 110.28(15) . . ?
C11 C10 C15 120.95(18) . . ?
C11 C10 C9 132.81(18) . . ?
C15 C10 C9 106.23(16) . . ?
C12 C11 C10 117.56(19) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C11 C12 C13 121.33(19) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 121.38(19) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C15 117.74(19) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C14 C15 C10 121.03(17) . . ?
C14 C15 C16 132.50(18) . . ?
C10 C15 C16 106.47(16) . . ?
N4 C16 N3 127.51(17) . . ?
N4 C16 C15 122.42(16) . . ?
N3 C16 C15 110.06(16) . . ?
C20 N5 C17 114.53(16) . . ?
C20 N5 Fe1 122.61(13) . . ?
C17 N5 Fe1 122.87(12) . . ?
N5 C17 C18 122.31(18) . . ?
N5 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
N6 C18 C17 123.4(2) . . ?
N6 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C18 N6 C19 113.86(19) . . ?
N6 C19 C20 124.2(2) . . ?
N6 C19 H19 117.9 . . ?
C20 C19 H19 117.9 . . ?
N5 C20 C19 121.75(19) . . ?
N5 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.9318(14) . y
Fe1 N1 1.9318(14) 3_666 y
Fe1 N3 1.9337(16) 3_666 y
Fe1 N3 1.9337(16) . y
Fe1 N5 2.0141(15) 3_666 y
Fe1 N5 2.0141(15) . y
N1 C8 1.377(2) . ?
N1 C1 1.379(2) . ?
N2 C8 1.324(2) . ?
N2 C9 1.334(2) . ?
N3 C16 1.374(2) . ?
N3 C9 1.376(2) . ?
N4 C1 1.320(2) 3_666 ?
N4 C16 1.327(2) . ?
C1 N4 1.320(2) 3_666 ?
C1 C2 1.453(2) . ?
C2 C7 1.386(2) . ?
C2 C3 1.392(2) . ?
C3 C4 1.375(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.387(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.454(2) . ?
C9 C10 1.452(2) . ?
C10 C11 1.384(2) . ?
C10 C15 1.392(2) . ?
C11 C12 1.375(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.385(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.373(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.379(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.454(2) . ?
N5 C20 1.334(2) . ?
N5 C17 1.342(2) . ?
C17 C18 1.374(3) . ?
C17 H17 0.9300 . ?
C18 N6 1.323(3) . ?
C18 H18 0.9300 . ?
N6 C19 1.323(3) . ?
C19 C20 1.374(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
