#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:52:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179516 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/13/4341388.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_4341388
loop_
_publ_author_name
'Hunter, Seth C.'
'Smith, Brenda A.'
'Hoffmann, Christina M.'
'Wang, Xiaoping'
'Chen, Yu-Sheng'
'McIntyre, Garry J.'
'Xue, Zi-Ling'
_publ_section_title
;
 Intermolecular interactions in solid-state metalloporphyrins and their
 impacts on crystal and molecular structures.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11552
_journal_page_last               11562
_journal_paper_doi               10.1021/ic5015835
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C44 H28 Cl Fe N4'
_chemical_formula_sum            'C44 H28 Cl Fe N4'
_chemical_formula_weight         704.03
_chemical_name_common            Fe(TPP)Cl
_chemical_name_systematic
; 
Chloro(meso-tetraphenylporphyrinato)iron(Ill) 
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4761(6)
_cell_length_b                   13.4761(6)
_cell_length_c                   9.6889(6)
_cell_measurement_reflns_used    1045
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      21.0
_cell_measurement_theta_min      2.5
_cell_volume                     1759.56(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'image plate detector'
_diffrn_measurement_method       Laue
_diffrn_radiation_monochromator  'Gd2O3 doped BaFBr:Eu2+'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.83880
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1893
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         35.41
_diffrn_reflns_theta_min         3.57
_diffrn_refln_wavelength_id      neut
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal bipyramidal'
_exptl_crystal_F_000             488
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         0.543
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         1263
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0232P)²+5.9811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                1045
_reflns_number_total             1263
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic5015835_si_002.cif
_cod_data_source_block           neutron20K
_cod_depositor_comments
'Adding full bibliography for 4341385--4341388.cif.'
_cod_original_sg_symbol_H-M      I4
_cod_database_code               4341388
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+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
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.0435(10) 0.0052(5) Uani 0.613(15) 4 d SPD 1
Cl1 Cl 0.0000 0.0000 0.2713(9) 0.0082(5) Uani 0.613(15) 4 d SPD 1
Fe2 Fe 0.0000 0.0000 -0.0373(14) 0.0052(5) Uani 0.387(15) 4 d SPD 2
Cl2 Cl 0.0000 0.0000 -0.2631(13) 0.0082(5) Uani 0.387(15) 4 d SPD 2
N1 N 0.14554(7) 0.03659(7) 0.0000 0.0104(2) Uani 1 1 d . .
C1 C 0.22526(11) -0.02776(11) 0.0020(7) 0.0105(3) Uani 1 1 d . .
C2 C 0.31703(11) 0.02739(11) 0.0020(9) 0.0116(3) Uani 1 1 d . .
H2 H 0.3904(2) -0.0053(3) 0.0017(18) 0.0282(8) Uani 1 1 d . .
C3 C 0.29236(11) 0.12554(11) -0.0016(8) 0.0118(3) Uani 1 1 d . .
H3 H 0.3419(3) 0.1885(3) -0.0095(17) 0.0256(13) Uani 1 1 d . .
C4 C 0.18544(10) 0.13105(11) -0.0013(7) 0.0095(3) Uani 1 1 d . .
C5 C 0.13140(11) 0.21980(11) -0.0026(8) 0.0098(3) Uani 1 1 d U .
C6 C 0.18817(10) 0.31549(8) 0.0011(6) 0.0095(3) Uani 0.700(14) 1 d PGDU 1
C7 C 0.2242(4) 0.3547(3) 0.1252(5) 0.0129(11) Uani 0.700(14) 1 d PGDU 1
C8 C 0.2779(4) 0.4436(3) 0.1249(6) 0.0155(12) Uani 0.700(14) 1 d PGDU 1
C9 C 0.29560(10) 0.49328(9) 0.0004(6) 0.0131(3) Uani 0.700(14) 1 d PGDU 1
C10 C 0.2596(3) 0.4541(2) -0.1236(6) 0.0101(12) Uani 0.700(14) 1 d PGDU 1
C11 C 0.2059(3) 0.3652(2) -0.1233(5) 0.0066(10) Uani 0.700(14) 1 d PGDU 1
H7 H 0.2089(12) 0.3172(8) 0.2228(12) 0.036(3) Uani 0.700(14) 1 d PD 1
H8 H 0.3085(11) 0.4768(14) 0.219(2) 0.040(3) Uani 0.700(14) 1 d PD 1
H9 H 0.3398(3) 0.5608(3) 0.0021(16) 0.0299(9) Uani 0.700(14) 1 d PD 1
H10 H 0.2731(10) 0.4903(13) -0.2205(16) 0.036(3) Uani 0.700(14) 1 d PD 1
H11 H 0.1775(10) 0.3377(11) -0.2208(14) 0.027(2) Uani 0.700(14) 1 d PD 1
C6B C 0.18817(10) 0.31549(8) 0.0011(6) 0.0095(3) Uani 0.300(14) 1 d PD 2
C7B C 0.1985(12) 0.3702(8) 0.1231(7) 0.0129(11) Uani 0.300(14) 1 d PD 2
C8B C 0.2540(13) 0.4580(8) 0.1233(7) 0.0155(12) Uani 0.300(14) 1 d PD 2
C9B C 0.29560(10) 0.49328(9) 0.0004(6) 0.0131(3) Uani 0.300(14) 1 d PD 2
C10B C 0.2798(11) 0.4421(7) -0.1232(6) 0.0101(12) Uani 0.300(14) 1 d PD 2
C11B C 0.2293(11) 0.3513(7) -0.1218(7) 0.0066(10) Uani 0.300(14) 1 d PD 2
H7B H 0.175(3) 0.339(3) 0.222(3) 0.036(3) Uani 0.300(14) 1 d PD 2
H8B H 0.271(4) 0.486(4) 0.230(5) 0.040(3) Uani 0.300(14) 1 d P 2
H9B H 0.3398(3) 0.5608(3) 0.0021(16) 0.0299(9) Uani 0.300(14) 1 d P 2
H10B H 0.304(3) 0.482(4) -0.215(4) 0.036(3) Uani 0.300(14) 1 d PD 2
H11B H 0.209(3) 0.306(2) -0.210(2) 0.027(2) Uani 0.300(14) 1 d PD 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.0000 0.0000 '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 156.5(5) 2 . y
N1 Fe1 N1 87.62(10) 2 4 ?
N1 Fe1 N1 87.62(10) . 4 y
N1 Fe1 N1 87.62(10) 2 3 ?
N1 Fe1 N1 87.62(10) . 3 ?
N1 Fe1 N1 156.5(5) 4 3 ?
N1 Fe1 Cl1 101.8(3) 2 . ?
N1 Fe1 Cl1 101.8(3) . . y
N1 Fe1 Cl1 101.8(3) 4 . ?
N1 Fe1 Cl1 101.8(3) 3 . ?
N1 Fe2 N1 159.7(7) . 2 y
Fe1 Fe2 N1 79.9(4) . 3 ?
N1 Fe2 N1 88.23(13) . 3 ?
N1 Fe2 N1 88.23(13) 2 3 ?
N1 Fe2 N1 88.23(13) . 4 y
N1 Fe2 N1 88.23(13) 2 4 ?
N1 Fe2 N1 159.7(7) 3 4 ?
Fe1 Fe2 Cl2 180.0 . . ?
N1 Fe2 Cl2 100.1(4) . . ?
N1 Fe2 Cl2 100.1(4) 2 . ?
N1 Fe2 Cl2 100.1(4) 3 . ?
N1 Fe2 Cl2 100.1(4) 4 . ?
C1 N1 C4 106.02(11) . . ?
C1 N1 Fe2 126.48(11) . . ?
C4 N1 Fe2 126.23(13) . . ?
C1 N1 Fe1 125.87(14) . . ?
C4 N1 Fe1 126.24(12) . . ?
N1 C1 C5 125.84(13) . 4 ?
N1 C1 C2 110.08(12) . . ?
C5 C1 C2 124.00(14) 4 . ?
C3 C2 C1 106.89(13) . . ?
C3 C2 H2 128.1(2) . . ?
C1 C2 H2 125.0(2) . . ?
C2 C3 C4 107.05(13) . . ?
C2 C3 H3 127.7(3) . . ?
C4 C3 H3 125.1(3) . . ?
N1 C4 C5 125.76(13) . . ?
N1 C4 C3 109.95(12) . . ?
C5 C4 C3 124.28(13) . . ?
C1 C5 C4 124.31(13) 3 . ?
C1 C5 C6 117.59(13) 3 . ?
C4 C5 C6 117.96(13) . . ?
C7 C6 C11 120.0 . . ?
C7 C6 C5 121.5(3) . . ?
C11 C6 C5 118.5(3) . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.2(8) . . ?
C8 C7 H7 119.8(8) . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8 122.9(12) . . ?
C9 C8 H8 117.1(12) . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 121.2(8) . . ?
C8 C9 H9 118.8(8) . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 121.4(9) . . ?
C11 C10 H10 118.6(9) . . ?
C10 C11 C6 120.0 . . ?
C10 C11 H11 118.2(8) . . ?
C6 C11 H11 121.7(8) . . ?
C8B C7B H7B 119(2) . . ?
C7B C8B H8B 113(2) . . ?
C11B C10B H10B 126(3) . . ?
C10B C11B H11 114.1(10) . . ?
C10B C11B H11B 127.2(16) . . ?
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 Fe2 0.782(7) . y
Fe1 N1 2.066(2) 2 ?
Fe1 N1 2.066(2) . y
Fe1 N1 2.066(2) 4 ?
Fe1 N1 2.066(2) 3 ?
Fe1 Cl1 2.208(8) . y
Fe2 N1 2.054(3) . y
Fe2 N1 2.054(3) 2 ?
Fe2 N1 2.054(3) 3 ?
Fe2 N1 2.054(3) 4 ?
Fe2 Cl2 2.188(12) . y
N1 C1 1.3807(17) . ?
N1 C4 1.3820(17) . ?
C1 C5 1.399(2) 4 ?
C1 C2 1.443(2) . ?
C2 C3 1.364(2) . ?
C2 H2 1.083(3) . ?
C3 C4 1.443(2) . ?
C3 H3 1.082(4) . ?
C4 C5 1.400(2) . ?
C5 C1 1.399(2) 3 ?
C5 C6 1.4998(18) . ?
C6 C7 1.3997 . ?
C6 C11 1.3998 . ?
C7 C8 1.3997 . ?
C7 H7 1.092(9) . ?
C8 C9 1.3997 . ?
C8 H8 1.095(19) . ?
C9 C10 1.3997 . ?
C9 H9 1.087(3) . ?
C10 C11 1.3997 . ?
C10 H10 1.073(14) . ?
C11 H11 1.085(12) . ?
C11 H11B 1.161(17) . ?
C7B C8B 1.400(2) . ?
C7B H7B 1.089(12) . ?
C8B H8B 1.12(5) . ?
C10B C11B 1.400(2) . ?
C10B H10B 1.088(12) . ?
C11B H11B 1.086(11) . ?
