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#$Date: 2018-02-09 06:37:38 +0200 (Fri, 09 Feb 2018) $
#$Revision: 206322 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045581.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_7045581
loop_
_publ_author_name
'Nishi, Miki'
'Ishii, Ryuta'
'Ikeda, Mitsuo'
'Hanasaki, Noriaki'
'Hoshino, Norihisa'
'Akutagawa, Tomoyuki'
'Sumimoto, Michinori'
'Matsuda, Masaki'
_publ_section_title
;
 An electrically conducting crystal composed of an octahedrally ligated
 porphyrin complex with high-spin iron(iii)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04649A
_journal_year                    2018
_chemical_formula_moiety         '2(C36 H20 Br2 Fe N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Br4 Fe2 N8 P'
_chemical_formula_weight         1787.83
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-01-22 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.6580(6)
_cell_length_b                   21.6580(6)
_cell_length_c                   7.6476(2)
_cell_measurement_reflns_used    26892
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      4.08
_cell_volume                     3587.25(17)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2015)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2015)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            39876
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         4.082
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    6.531
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5642
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       needle
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0734P)²+2.8702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2679
_reflns_number_total             3241
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04649a2.cif
_cod_data_source_block           TPPFetbpBrRT
_cod_original_cell_volume        3587.3(2)
_cod_database_code               7045581
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.355
_shelx_estimated_absorpt_t_max   0.780
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.500000 0.500000 0.000000 0.0458(2) Uani 1 2 d S . P
Br1 Br 0.59753(2) 0.55828(2) 0.10448(6) 0.05750(18) Uani 1 1 d . . .
P1 P 0.750000 0.750000 0.250000 0.0445(4) Uani 1 4 d S T P
N1 N 0.51167(13) 0.42787(13) 0.1736(4) 0.0441(7) Uani 1 1 d . . .
N2 N 0.44411(13) 0.54485(13) 0.1797(4) 0.0432(6) Uani 1 1 d . . .
C1 C 0.57638(17) 0.36189(17) -0.0107(5) 0.0485(9) Uani 1 1 d . . .
H1 H 0.596499 0.323981 -0.014236 0.058 Uiso 1 1 calc R U .
C2 C 0.54319(17) 0.37397(16) 0.1387(5) 0.0449(8) Uani 1 1 d . . .
C3 C 0.53396(16) 0.33144(16) 0.2835(5) 0.0455(8) Uani 1 1 d . . .
C4 C 0.55348(18) 0.27082(17) 0.3100(5) 0.0527(9) Uani 1 1 d . . .
H2 H 0.578866 0.250963 0.229669 0.063 Uiso 1 1 calc R U .
C5 C 0.5338(2) 0.24141(18) 0.4596(5) 0.0578(10) Uani 1 1 d . . .
H3 H 0.545332 0.200655 0.479456 0.069 Uiso 1 1 calc R U .
C6 C 0.4970(2) 0.27153(19) 0.5815(5) 0.0578(10) Uani 1 1 d . . .
H4 H 0.485125 0.250792 0.682549 0.069 Uiso 1 1 calc R U .
C7 C 0.47764(18) 0.33120(18) 0.5560(5) 0.0526(9) Uani 1 1 d . . .
H5 H 0.452971 0.351109 0.638002 0.063 Uiso 1 1 calc R U .
C8 C 0.49614(16) 0.36091(16) 0.4037(5) 0.0444(8) Uani 1 1 d . . .
C9 C 0.48223(16) 0.42147(16) 0.3306(5) 0.0435(8) Uani 1 1 d . . .
C10 C 0.44316(17) 0.46472(17) 0.4052(5) 0.0459(8) Uani 1 1 d . . .
H6 H 0.427039 0.454780 0.514367 0.055 Uiso 1 1 calc R U .
C11 C 0.42538(16) 0.52092(16) 0.3362(5) 0.0437(8) Uani 1 1 d . . .
C12 C 0.38287(16) 0.56444(17) 0.4195(5) 0.0442(8) Uani 1 1 d . . .
C13 C 0.35134(17) 0.56250(19) 0.5776(5) 0.0530(9) Uani 1 1 d . . .
H7 H 0.354166 0.528648 0.651955 0.064 Uiso 1 1 calc R U .
C14 C 0.31521(19) 0.6138(2) 0.6195(6) 0.0603(11) Uani 1 1 d . . .
H8 H 0.294115 0.614436 0.725366 0.072 Uiso 1 1 calc R U .
C15 C 0.3099(2) 0.6640(2) 0.5069(6) 0.0614(11) Uani 1 1 d . . .
H9 H 0.285399 0.697372 0.538581 0.074 Uiso 1 1 calc R U .
C16 C 0.34052(18) 0.66477(18) 0.3496(6) 0.0558(10) Uani 1 1 d . . .
H10 H 0.336372 0.697960 0.273358 0.067 Uiso 1 1 calc R U .
C17 C 0.37802(16) 0.61446(16) 0.3070(5) 0.0457(8) Uani 1 1 d . . .
C18 C 0.41641(16) 0.60100(16) 0.1562(5) 0.0445(8) Uani 1 1 d . . .
C19 C 0.68638(17) 0.76640(17) 0.1078(5) 0.0482(8) Uani 1 1 d . . .
C20 C 0.6927(2) 0.8122(2) -0.0165(6) 0.0609(10) Uani 1 1 d . . .
H11 H 0.728516 0.835909 -0.019845 0.073 Uiso 1 1 calc R U .
C21 C 0.6463(2) 0.8228(2) -0.1354(6) 0.0718(13) Uani 1 1 d . . .
H12 H 0.650519 0.854150 -0.217676 0.086 Uiso 1 1 calc R U .
C22 C 0.5940(2) 0.7876(2) -0.1332(6) 0.0730(13) Uani 1 1 d . . .
H13 H 0.562546 0.795364 -0.212859 0.088 Uiso 1 1 calc R U .
C23 C 0.5880(2) 0.7416(3) -0.0161(7) 0.0788(15) Uani 1 1 d . . .
H14 H 0.552530 0.717364 -0.016803 0.095 Uiso 1 1 calc R U .
C24 C 0.63399(19) 0.7299(2) 0.1057(6) 0.0631(11) Uani 1 1 d . . .
H15 H 0.629646 0.697695 0.185300 0.076 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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
N1 Fe1 N1 180.0 . 5_665
N1 Fe1 N2 89.99(12) . .
N1 Fe1 N2 90.01(12) 5_665 .
N1 Fe1 N2 90.01(12) . 5_665
N1 Fe1 N2 89.99(12) 5_665 5_665
N2 Fe1 N2 180.0 . 5_665
N1 Fe1 Br1 94.05(8) . .
N1 Fe1 Br1 85.95(8) 5_665 .
N2 Fe1 Br1 92.49(8) . .
N2 Fe1 Br1 87.51(8) 5_665 .
N1 Fe1 Br1 85.95(8) . 5_665
N1 Fe1 Br1 94.05(8) 5_665 5_665
N2 Fe1 Br1 87.51(8) . 5_665
N2 Fe1 Br1 92.49(8) 5_665 5_665
Br1 Fe1 Br1 180.0 . 5_665
C19 P1 C19 111.64(13) . 7_576
C19 P1 C19 111.64(13) . 8_756
C19 P1 C19 105.2(2) 7_576 8_756
C19 P1 C19 105.2(2) . 2_665
C19 P1 C19 111.64(13) 7_576 2_665
C19 P1 C19 111.64(13) 8_756 2_665
C9 N1 C2 108.4(3) . .
C9 N1 Fe1 125.8(2) . .
C2 N1 Fe1 125.2(2) . .
C11 N2 C18 108.8(3) . .
C11 N2 Fe1 125.2(2) . .
C18 N2 Fe1 125.9(2) . .
C2 C1 C18 128.2(3) . 5_665
C2 C1 H1 115.9 . .
C18 C1 H1 115.9 5_665 .
C1 C2 N1 125.5(3) . .
C1 C2 C3 125.7(3) . .
N1 C2 C3 108.7(3) . .
C8 C3 C4 121.0(3) . .
C8 C3 C2 107.1(3) . .
C4 C3 C2 131.7(3) . .
C5 C4 C3 117.6(4) . .
C5 C4 H2 121.2 . .
C3 C4 H2 121.2 . .
C4 C5 C6 121.2(4) . .
C4 C5 H3 119.4 . .
C6 C5 H3 119.4 . .
C7 C6 C5 121.5(4) . .
C7 C6 H4 119.3 . .
C5 C6 H4 119.3 . .
C6 C7 C8 117.9(4) . .
C6 C7 H5 121.1 . .
C8 C7 H5 121.1 . .
C3 C8 C7 120.8(3) . .
C3 C8 C9 106.4(3) . .
C7 C8 C9 132.8(3) . .
N1 C9 C10 125.3(3) . .
N1 C9 C8 109.4(3) . .
C10 C9 C8 125.2(3) . .
C11 C10 C9 127.5(3) . .
C11 C10 H6 116.3 . .
C9 C10 H6 116.3 . .
N2 C11 C10 125.9(3) . .
N2 C11 C12 108.9(3) . .
C10 C11 C12 125.2(3) . .
C17 C12 C13 121.7(3) . .
C17 C12 C11 106.3(3) . .
C13 C12 C11 132.0(3) . .
C12 C13 C14 116.8(4) . .
C12 C13 H7 121.6 . .
C14 C13 H7 121.6 . .
C15 C14 C13 121.7(4) . .
C15 C14 H8 119.1 . .
C13 C14 H8 119.1 . .
C16 C15 C14 120.8(4) . .
C16 C15 H9 119.6 . .
C14 C15 H9 119.6 . .
C15 C16 C17 118.3(4) . .
C15 C16 H10 120.8 . .
C17 C16 H10 120.8 . .
C12 C17 C16 120.5(3) . .
C12 C17 C18 107.0(3) . .
C16 C17 C18 132.5(3) . .
N2 C18 C1 125.0(3) . 5_665
N2 C18 C17 109.0(3) . .
C1 C18 C17 126.0(3) 5_665 .
C20 C19 C24 119.0(4) . .
C20 C19 P1 118.9(3) . .
C24 C19 P1 121.6(3) . .
C21 C20 C19 120.2(4) . .
C21 C20 H11 119.9 . .
C19 C20 H11 119.9 . .
C22 C21 C20 120.3(5) . .
C22 C21 H12 119.8 . .
C20 C21 H12 119.8 . .
C23 C22 C21 120.2(4) . .
C23 C22 H13 119.9 . .
C21 C22 H13 119.9 . .
C22 C23 C24 120.8(5) . .
C22 C23 H14 119.6 . .
C24 C23 H14 119.6 . .
C19 C24 C23 119.5(4) . .
C19 C24 H15 120.3 . .
C23 C24 H15 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.066(3) .
Fe1 N1 2.066(3) 5_665
Fe1 N2 2.073(3) .
Fe1 N2 2.073(3) 5_665
Fe1 Br1 2.5873(4) .
Fe1 Br1 2.5873(4) 5_665
P1 C19 1.791(4) .
P1 C19 1.791(4) 7_576
P1 C19 1.791(4) 8_756
P1 C19 1.791(4) 2_665
N1 C9 1.367(4) .
N1 C2 1.378(4) .
N2 C11 1.366(4) .
N2 C18 1.368(4) .
C1 C2 1.375(5) .
C1 C18 1.382(5) 5_665
C1 H1 0.9300 .
C2 C3 1.454(5) .
C3 C8 1.387(5) .
C3 C4 1.394(5) .
C4 C5 1.377(5) .
C4 H2 0.9300 .
C5 C6 1.389(6) .
C5 H3 0.9300 .
C6 C7 1.372(5) .
C6 H4 0.9300 .
C7 C8 1.389(5) .
C7 H5 0.9300 .
C8 C9 1.457(5) .
C9 C10 1.385(5) .
C10 C11 1.382(5) .
C10 H6 0.9300 .
C11 C12 1.464(5) .
C12 C17 1.388(5) .
C12 C13 1.389(5) .
C13 C14 1.396(6) .
C13 H7 0.9300 .
C14 C15 1.391(6) .
C14 H8 0.9300 .
C15 C16 1.373(5) .
C15 H9 0.9300 .
C16 C17 1.398(5) .
C16 H10 0.9300 .
C17 C18 1.451(5) .
C19 C20 1.381(6) .
C19 C24 1.383(6) .
C20 C21 1.375(6) .
C20 H11 0.9300 .
C21 C22 1.365(7) .
C21 H12 0.9300 .
C22 C23 1.346(7) .
C22 H13 0.9300 .
C23 C24 1.387(6) .
C23 H14 0.9300 .
C24 H15 0.9300 .
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
C18 C1 C2 N1 -2.2(6) 5_665 .
C18 C1 C2 C3 175.8(4) 5_665 .
C9 N1 C2 C1 177.3(4) . .
Fe1 N1 C2 C1 6.1(5) . .
C9 N1 C2 C3 -1.0(4) . .
Fe1 N1 C2 C3 -172.2(2) . .
C1 C2 C3 C8 -177.9(4) . .
N1 C2 C3 C8 0.4(4) . .
C1 C2 C3 C4 -1.1(7) . .
N1 C2 C3 C4 177.2(4) . .
C8 C3 C4 C5 0.1(6) . .
C2 C3 C4 C5 -176.3(4) . .
C3 C4 C5 C6 -1.4(6) . .
C4 C5 C6 C7 1.4(7) . .
C5 C6 C7 C8 0.0(6) . .
C4 C3 C8 C7 1.3(6) . .
C2 C3 C8 C7 178.5(3) . .
C4 C3 C8 C9 -176.9(3) . .
C2 C3 C8 C9 0.3(4) . .
C6 C7 C8 C3 -1.3(6) . .
C6 C7 C8 C9 176.4(4) . .
C2 N1 C9 C10 -176.3(4) . .
Fe1 N1 C9 C10 -5.2(5) . .
C2 N1 C9 C8 1.2(4) . .
Fe1 N1 C9 C8 172.3(2) . .
C3 C8 C9 N1 -0.9(4) . .
C7 C8 C9 N1 -178.8(4) . .
C3 C8 C9 C10 176.6(4) . .
C7 C8 C9 C10 -1.3(7) . .
N1 C9 C10 C11 1.6(6) . .
C8 C9 C10 C11 -175.5(4) . .
C18 N2 C11 C10 179.6(4) . .
Fe1 N2 C11 C10 3.9(5) . .
C18 N2 C11 C12 -0.1(4) . .
Fe1 N2 C11 C12 -175.8(2) . .
C9 C10 C11 N2 -0.9(6) . .
C9 C10 C11 C12 178.7(4) . .
N2 C11 C12 C17 -0.5(4) . .
C10 C11 C12 C17 179.8(3) . .
N2 C11 C12 C13 -179.8(4) . .
C10 C11 C12 C13 0.5(7) . .
C17 C12 C13 C14 -1.0(6) . .
C11 C12 C13 C14 178.2(4) . .
C12 C13 C14 C15 1.3(6) . .
C13 C14 C15 C16 -0.2(7) . .
C14 C15 C16 C17 -1.2(6) . .
C13 C12 C17 C16 -0.4(6) . .
C11 C12 C17 C16 -179.8(3) . .
C13 C12 C17 C18 -179.8(3) . .
C11 C12 C17 C18 0.8(4) . .
C15 C16 C17 C12 1.5(6) . .
C15 C16 C17 C18 -179.2(4) . .
C11 N2 C18 C1 -178.7(3) . 5_665
Fe1 N2 C18 C1 -3.0(5) . 5_665
C11 N2 C18 C17 0.6(4) . .
Fe1 N2 C18 C17 176.3(2) . .
C12 C17 C18 N2 -0.9(4) . .
C16 C17 C18 N2 179.8(4) . .
C12 C17 C18 C1 178.4(4) . 5_665
C16 C17 C18 C1 -1.0(7) . 5_665
C19 P1 C19 C20 65.9(3) 7_576 .
C19 P1 C19 C20 -176.7(3) 8_756 .
C19 P1 C19 C20 -55.4(3) 2_665 .
C19 P1 C19 C24 -121.7(4) 7_576 .
C19 P1 C19 C24 -4.3(3) 8_756 .
C19 P1 C19 C24 117.0(4) 2_665 .
C24 C19 C20 C21 2.8(6) . .
P1 C19 C20 C21 175.4(3) . .
C19 C20 C21 C22 -1.0(7) . .
C20 C21 C22 C23 -0.9(7) . .
C21 C22 C23 C24 1.1(8) . .
C20 C19 C24 C23 -2.6(6) . .
P1 C19 C24 C23 -175.0(4) . .
C22 C23 C24 C19 0.7(8) . .
