# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPFetbpCl22rt
_database_code_depnum_ccdc_archive 'CCDC 1947251'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Cl2 Fe N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Cl4 Fe2 N8 P'
_chemical_formula_weight         1609.99

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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.8277(4)
_cell_length_b                   21.8277(4)
_cell_length_c                   7.61520(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3628.25(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    17759
_cell_measurement_theta_min      4.05
_cell_measurement_theta_max      68.025

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.231
_shelx_estimated_absorpt_T_min   0.421
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7381
_exptl_absorpt_correction_T_max  0.8938
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39231
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.051
_diffrn_reflns_theta_max         68.185
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3277
_reflns_number_gt                2200
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3277
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.2425
_refine_ls_wR_factor_gt          0.2040
_refine_ls_goodness_of_fit_ref   1.588
_refine_ls_restrained_S_all      1.588
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.000000 0.500000 0.0571(4) Uani 1 2 d S . P . .
N1 N 0.44334(17) -0.04465(17) 0.6777(5) 0.0509(10) Uani 1 1 d . . . . .
N2 N 0.48940(17) -0.07262(17) 0.3258(5) 0.0497(10) Uani 1 1 d . . . . .
Cl1 Cl 0.59017(6) -0.05240(6) 0.61202(19) 0.0690(5) Uani 1 1 d . . . . .
C1 C 0.4247(2) -0.0209(2) 0.8367(6) 0.0507(11) Uani 1 1 d . . . . .
C2 C 0.3824(2) -0.0642(2) 0.9197(6) 0.0501(11) Uani 1 1 d . . . . .
C3 C 0.3515(2) -0.0631(2) 1.0786(7) 0.0615(14) Uani 1 1 d . . . . .
H1 H 0.354995 -0.030009 1.155029 0.074 Uiso 1 1 calc R U . . .
C4 C 0.3152(2) -0.1132(3) 1.1189(7) 0.0662(15) Uani 1 1 d . . . . .
H2 H 0.293683 -0.113603 1.224276 0.079 Uiso 1 1 calc R U . . .
C5 C 0.3101(3) -0.1628(3) 1.0062(7) 0.0672(16) Uani 1 1 d . . . . .
H3 H 0.285939 -0.196055 1.038506 0.081 Uiso 1 1 calc R U . . .
C6 C 0.3403(2) -0.1638(2) 0.8466(7) 0.0601(13) Uani 1 1 d . . . . .
H4 H 0.335834 -0.196639 0.769872 0.072 Uiso 1 1 calc R U . . .
C7 C 0.3777(2) -0.1139(2) 0.8041(6) 0.0503(11) Uani 1 1 d . . . . .
C8 C 0.4235(2) -0.1368(2) 0.5076(6) 0.0559(13) Uani 1 1 d . . . . .
H5 H 0.402950 -0.174162 0.510041 0.067 Uiso 1 1 calc R U . . .
C9 C 0.4160(2) -0.1002(2) 0.6546(6) 0.0503(11) Uani 1 1 d . . . . .
C10 C 0.4575(2) -0.1253(2) 0.3575(6) 0.0500(11) Uani 1 1 d . . . . .
C11 C 0.4671(2) -0.1674(2) 0.2138(6) 0.0491(11) Uani 1 1 d . . . . .
C12 C 0.4473(2) -0.2278(2) 0.1836(7) 0.0588(13) Uani 1 1 d . . . . .
H6 H 0.421594 -0.247739 0.262603 0.071 Uiso 1 1 calc R U . . .
C13 C 0.4674(3) -0.2566(2) 0.0315(7) 0.0614(14) Uani 1 1 d . . . . .
H7 H 0.455839 -0.296941 0.009802 0.074 Uiso 1 1 calc R U . . .
C14 C 0.5038(3) -0.2267(2) -0.0868(7) 0.0648(14) Uani 1 1 d . . . . .
H8 H 0.515764 -0.247150 -0.188407 0.078 Uiso 1 1 calc R U . . .
C15 C 0.5235(2) -0.1673(2) -0.0608(7) 0.0582(13) Uani 1 1 d . . . . .
H9 H 0.548164 -0.147528 -0.142740 0.070 Uiso 1 1 calc R U . . .
C16 C 0.5050(2) -0.1380(2) 0.0939(6) 0.0502(11) Uani 1 1 d . . . . .
C17 C 0.5193(2) -0.0783(2) 0.1668(6) 0.0494(11) Uani 1 1 d . . . . .
C18 C 0.5579(2) -0.0349(2) 0.0951(7) 0.0522(12) Uani 1 1 d . . . . .
H10 H 0.574340 -0.044710 -0.014023 0.063 Uiso 1 1 calc R U . . .
P1 P 0.750000 -0.250000 0.750000 0.0556(7) Uani 1 4 d S T P . .
C19 C 0.6853(2) -0.2596(2) 0.6081(7) 0.0608(14) Uani 1 1 d . . . . .
C20 C 0.6856(3) -0.3089(3) 0.4907(8) 0.0733(17) Uani 1 1 d . . . . .
H11 H 0.717674 -0.336991 0.493733 0.088 Uiso 1 1 calc R U . . .
C21 C 0.6395(3) -0.3163(3) 0.3720(9) 0.0861(19) Uani 1 1 d . . . . .
H12 H 0.639919 -0.348960 0.293635 0.103 Uiso 1 1 calc R U . . .
C22 C 0.5920(3) -0.2743(4) 0.3699(9) 0.097(2) Uani 1 1 d . . . . .
H13 H 0.559762 -0.279711 0.291445 0.116 Uiso 1 1 calc R U . . .
C23 C 0.5914(3) -0.2249(4) 0.4808(9) 0.099(2) Uani 1 1 d . . . . .
H14 H 0.559211 -0.197018 0.477005 0.119 Uiso 1 1 calc R U . . .
C24 C 0.6391(3) -0.2168(3) 0.5987(8) 0.0749(17) Uani 1 1 d . . . . .
H15 H 0.639844 -0.182511 0.671242 0.090 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 2.076(4) 5_656 ?
Fe1 N1 2.076(4) . ?
Fe1 N2 2.080(4) 5_656 ?
Fe1 N2 2.080(4) . ?
Fe1 Cl1 2.4310(14) 5_656 ?
Fe1 Cl1 2.4310(14) . ?
N1 C9 1.362(5) . ?
N1 C1 1.379(5) . ?
N2 C10 1.366(6) . ?
N2 C17 1.381(6) . ?
C1 C18 1.379(6) 5_656 ?
C1 C2 1.464(6) . ?
C2 C3 1.385(7) . ?
C2 C7 1.402(6) . ?
C3 C4 1.386(7) . ?
C4 C5 1.386(7) . ?
C5 C6 1.382(7) . ?
C6 C7 1.399(6) . ?
C7 C9 1.444(6) . ?
C8 C9 1.385(6) . ?
C8 C10 1.386(6) . ?
C10 C11 1.443(6) . ?
C11 C16 1.389(6) . ?
C11 C12 1.407(6) . ?
C12 C13 1.389(7) . ?
C13 C14 1.368(7) . ?
C14 C15 1.381(7) . ?
C15 C16 1.401(7) . ?
C16 C17 1.451(6) . ?
C17 C18 1.379(6) . ?
P1 C19 1.790(5) 7_667 ?
P1 C19 1.790(5) 2_645 ?
P1 C19 1.790(5) 8_647 ?
P1 C19 1.790(5) . ?
C19 C24 1.379(7) . ?
C19 C20 1.399(8) . ?
C20 C21 1.363(8) . ?
C21 C22 1.384(10) . ?
C22 C23 1.369(10) . ?
C23 C24 1.386(8) . ?

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 5_656 . ?
N1 Fe1 N2 89.52(15) 5_656 5_656 ?
N1 Fe1 N2 90.48(15) . 5_656 ?
N1 Fe1 N2 90.48(15) 5_656 . ?
N1 Fe1 N2 89.52(15) . . ?
N2 Fe1 N2 180.0 5_656 . ?
N1 Fe1 Cl1 91.87(11) 5_656 5_656 ?
N1 Fe1 Cl1 88.12(11) . 5_656 ?
N2 Fe1 Cl1 87.44(11) 5_656 5_656 ?
N2 Fe1 Cl1 92.56(11) . 5_656 ?
N1 Fe1 Cl1 88.12(11) 5_656 . ?
N1 Fe1 Cl1 91.88(11) . . ?
N2 Fe1 Cl1 92.56(11) 5_656 . ?
N2 Fe1 Cl1 87.44(11) . . ?
Cl1 Fe1 Cl1 180.0 5_656 . ?
C9 N1 C1 108.6(4) . . ?
C9 N1 Fe1 126.5(3) . . ?
C1 N1 Fe1 124.9(3) . . ?
C10 N2 C17 108.7(4) . . ?
C10 N2 Fe1 125.9(3) . . ?
C17 N2 Fe1 125.1(3) . . ?
C18 C1 N1 125.6(4) 5_656 . ?
C18 C1 C2 125.6(4) 5_656 . ?
N1 C1 C2 108.8(4) . . ?
C3 C2 C7 121.8(4) . . ?
C3 C2 C1 132.3(4) . . ?
C7 C2 C1 106.0(4) . . ?
C2 C3 C4 117.2(5) . . ?
C5 C4 C3 121.7(5) . . ?
C6 C5 C4 121.2(5) . . ?
C5 C6 C7 118.0(5) . . ?
C6 C7 C2 120.0(4) . . ?
C6 C7 C9 133.0(5) . . ?
C2 C7 C9 106.9(4) . . ?
C9 C8 C10 128.6(5) . . ?
N1 C9 C8 124.5(4) . . ?
N1 C9 C7 109.7(4) . . ?
C8 C9 C7 125.8(4) . . ?
N2 C10 C8 124.8(4) . . ?
N2 C10 C11 109.1(4) . . ?
C8 C10 C11 126.0(4) . . ?
C16 C11 C12 120.6(4) . . ?
C16 C11 C10 106.9(4) . . ?
C12 C11 C10 132.5(4) . . ?
C13 C12 C11 117.6(5) . . ?
C14 C13 C12 121.1(5) . . ?
C13 C14 C15 122.3(5) . . ?
C14 C15 C16 117.4(5) . . ?
C11 C16 C15 120.9(4) . . ?
C11 C16 C17 107.0(4) . . ?
C15 C16 C17 132.0(5) . . ?
C18 C17 N2 125.1(4) . . ?
C18 C17 C16 126.6(5) . . ?
N2 C17 C16 108.3(4) . . ?
C1 C18 C17 128.7(5) 5_656 . ?
C19 P1 C19 111.38(18) 7_667 2_645 ?
C19 P1 C19 105.7(3) 7_667 8_647 ?
C19 P1 C19 111.38(18) 2_645 8_647 ?
C19 P1 C19 111.38(18) 7_667 . ?
C19 P1 C19 105.7(3) 2_645 . ?
C19 P1 C19 111.38(18) 8_647 . ?
C24 C19 C20 119.5(5) . . ?
C24 C19 P1 122.0(4) . . ?
C20 C19 P1 118.2(4) . . ?
C21 C20 C19 120.7(6) . . ?
C20 C21 C22 118.9(7) . . ?
C23 C22 C21 121.4(6) . . ?
C22 C23 C24 119.6(7) . . ?
C19 C24 C23 119.8(6) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C1 C18 -179.3(5) . . . 5_656 ?
Fe1 N1 C1 C18 -2.3(7) . . . 5_656 ?
C9 N1 C1 C2 -0.2(5) . . . . ?
Fe1 N1 C1 C2 176.8(3) . . . . ?
C18 C1 C2 C3 -1.8(9) 5_656 . . . ?
N1 C1 C2 C3 179.1(5) . . . . ?
C18 C1 C2 C7 179.5(5) 5_656 . . . ?
N1 C1 C2 C7 0.4(5) . . . . ?
C7 C2 C3 C4 -0.3(8) . . . . ?
C1 C2 C3 C4 -178.8(5) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C3 C4 C5 C6 -1.2(9) . . . . ?
C4 C5 C6 C7 1.8(8) . . . . ?
C5 C6 C7 C2 -1.7(7) . . . . ?
C5 C6 C7 C9 178.7(5) . . . . ?
C3 C2 C7 C6 1.0(7) . . . . ?
C1 C2 C7 C6 179.8(4) . . . . ?
C3 C2 C7 C9 -179.3(5) . . . . ?
C1 C2 C7 C9 -0.4(5) . . . . ?
C1 N1 C9 C8 178.9(5) . . . . ?
Fe1 N1 C9 C8 2.0(7) . . . . ?
C1 N1 C9 C7 -0.1(5) . . . . ?
Fe1 N1 C9 C7 -177.0(3) . . . . ?
C10 C8 C9 N1 -1.5(8) . . . . ?
C10 C8 C9 C7 177.3(5) . . . . ?
C6 C7 C9 N1 -180.0(5) . . . . ?
C2 C7 C9 N1 0.3(5) . . . . ?
C6 C7 C9 C8 1.1(9) . . . . ?
C2 C7 C9 C8 -178.6(5) . . . . ?
C17 N2 C10 C8 178.0(5) . . . . ?
Fe1 N2 C10 C8 4.7(7) . . . . ?
C17 N2 C10 C11 0.3(5) . . . . ?
Fe1 N2 C10 C11 -173.0(3) . . . . ?
C9 C8 C10 N2 -2.1(8) . . . . ?
C9 C8 C10 C11 175.2(5) . . . . ?
N2 C10 C11 C16 -0.8(5) . . . . ?
C8 C10 C11 C16 -178.5(5) . . . . ?
N2 C10 C11 C12 177.2(5) . . . . ?
C8 C10 C11 C12 -0.5(9) . . . . ?
C16 C11 C12 C13 0.6(7) . . . . ?
C10 C11 C12 C13 -177.2(5) . . . . ?
C11 C12 C13 C14 -1.7(8) . . . . ?
C12 C13 C14 C15 1.3(9) . . . . ?
C13 C14 C15 C16 0.3(8) . . . . ?
C12 C11 C16 C15 1.0(7) . . . . ?
C10 C11 C16 C15 179.3(4) . . . . ?
C12 C11 C16 C17 -177.3(4) . . . . ?
C10 C11 C16 C17 1.0(5) . . . . ?
C14 C15 C16 C11 -1.4(8) . . . . ?
C14 C15 C16 C17 176.4(5) . . . . ?
C10 N2 C17 C18 -177.3(5) . . . . ?
Fe1 N2 C17 C18 -4.0(7) . . . . ?
C10 N2 C17 C16 0.4(5) . . . . ?
Fe1 N2 C17 C16 173.7(3) . . . . ?
C11 C16 C17 C18 176.8(5) . . . . ?
C15 C16 C17 C18 -1.2(9) . . . . ?
C11 C16 C17 N2 -0.9(5) . . . . ?
C15 C16 C17 N2 -178.9(5) . . . . ?
N2 C17 C18 C1 0.9(9) . . . 5_656 ?
C16 C17 C18 C1 -176.3(5) . . . 5_656 ?
C19 P1 C19 C24 7.8(5) 7_667 . . . ?
C19 P1 C19 C24 -113.3(5) 2_645 . . . ?
C19 P1 C19 C24 125.6(6) 8_647 . . . ?
C19 P1 C19 C20 -179.1(5) 7_667 . . . ?
C19 P1 C19 C20 59.8(4) 2_645 . . . ?
C19 P1 C19 C20 -61.4(4) 8_647 . . . ?
C24 C19 C20 C21 -2.5(9) . . . . ?
P1 C19 C20 C21 -175.8(5) . . . . ?
C19 C20 C21 C22 -0.4(10) . . . . ?
C20 C21 C22 C23 1.9(11) . . . . ?
C21 C22 C23 C24 -0.4(11) . . . . ?
C20 C19 C24 C23 4.0(9) . . . . ?
P1 C19 C24 C23 177.0(5) . . . . ?
C22 C23 C24 C19 -2.5(11) . . . . ?

_refine_diff_density_max         0.440
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.077

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCoPcCl22rt
_database_code_depnum_ccdc_archive 'CCDC 1947259'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H16 Cl2 Co N8), C24 H20 P'
_chemical_formula_sum            'C88 H52 Cl4 Co2 N16 P'
_chemical_formula_weight         1624.08

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5677(4)
_cell_length_b                   21.5677(4)
_cell_length_c                   7.54110(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3507.86(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    24797
_cell_measurement_theta_min      4.105
_cell_measurement_theta_max      68.215

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             1658
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    5.836
_shelx_estimated_absorpt_T_min   0.388
_shelx_estimated_absorpt_T_max   0.388
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7784
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36554
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.100
_diffrn_reflns_theta_max         68.217
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3184
_reflns_number_gt                2644
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3184
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1588
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_restrained_S_all      1.241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.000000 0.500000 0.0340(3) Uani 1 2 d S . P . .
Cl1 Cl 0.55024(3) -0.08616(3) 0.59719(11) 0.0477(3) Uani 1 1 d . . . . .
N1 N 0.43247(10) -0.01126(10) 0.6657(3) 0.0379(6) Uani 1 1 d . . . . .
N2 N 0.45761(10) -0.05237(10) 0.3312(3) 0.0388(6) Uani 1 1 d . . . . .
N3 N 0.36442(11) -0.07760(11) 0.4943(3) 0.0413(6) Uani 1 1 d . . . . .
N4 N 0.46567(10) 0.05667(11) 0.9030(3) 0.0399(6) Uani 1 1 d . . . . .
C1 C 0.42672(13) 0.01816(13) 0.8254(4) 0.0383(6) Uani 1 1 d . . . . .
C2 C 0.36589(13) 0.00381(13) 0.9022(4) 0.0376(7) Uani 1 1 d . . . . .
C3 C 0.33747(14) 0.02325(14) 1.0581(4) 0.0458(7) Uani 1 1 d . . . . .
H1 H 0.357826 0.048522 1.139296 0.055 Uiso 1 1 calc R U . . .
C4 C 0.27689(14) 0.00293(15) 1.0864(4) 0.0482(8) Uani 1 1 d . . . . .
H2 H 0.256149 0.015377 1.188489 0.058 Uiso 1 1 calc R U . . .
C5 C 0.24675(14) -0.03538(15) 0.9663(4) 0.0481(8) Uani 1 1 d . . . . .
H3 H 0.206354 -0.048104 0.989372 0.058 Uiso 1 1 calc R U . . .
C6 C 0.27608(13) -0.05504(13) 0.8118(4) 0.0438(7) Uani 1 1 d . . . . .
H4 H 0.256037 -0.080833 0.731276 0.053 Uiso 1 1 calc R U . . .
C7 C 0.33641(12) -0.03476(13) 0.7820(4) 0.0388(7) Uani 1 1 d . . . . .
C8 C 0.37914(12) -0.04338(13) 0.6352(4) 0.0388(7) Uani 1 1 d . . . . .
C9 C 0.40163(12) -0.08157(12) 0.3561(4) 0.0382(6) Uani 1 1 d . . . . .
C10 C 0.38813(12) -0.12069(12) 0.2044(4) 0.0391(7) Uani 1 1 d . . . . .
C11 C 0.33816(13) -0.15846(13) 0.1641(4) 0.0442(7) Uani 1 1 d . . . . .
H5 H 0.304780 -0.162493 0.241302 0.053 Uiso 1 1 calc R U . . .
C12 C 0.33989(15) -0.19016(16) 0.0034(4) 0.0491(9) Uani 1 1 d . . . . .
H6 H 0.306801 -0.215428 -0.028719 0.059 Uiso 1 1 calc R U . . .
C13 C 0.39038(15) -0.18454(15) -0.1096(4) 0.0500(8) Uani 1 1 d . . . . .
H7 H 0.390427 -0.206652 -0.215504 0.060 Uiso 1 1 calc R U . . .
C14 C 0.44023(14) -0.14746(13) -0.0705(4) 0.0447(7) Uani 1 1 d . . . . .
H8 H 0.473853 -0.143984 -0.147042 0.054 Uiso 1 1 calc R U . . .
C15 C 0.43804(13) -0.11536(12) 0.0892(4) 0.0382(7) Uani 1 1 d . . . . .
C16 C 0.48117(13) -0.07165(12) 0.1715(4) 0.0381(6) Uani 1 1 d . . . . .
P1 P 0.250000 0.250000 0.250000 0.0455(4) Uani 1 4 d S T P . .
C17 C 0.23907(15) 0.18461(14) 0.3928(4) 0.0508(8) Uani 1 1 d . . . . .
C18 C 0.28060(19) 0.13647(16) 0.4001(5) 0.0641(10) Uani 1 1 d . . . . .
H9 H 0.315058 0.136008 0.325984 0.077 Uiso 1 1 calc R U . . .
C19 C 0.2706(3) 0.0883(2) 0.5197(5) 0.0856(14) Uani 1 1 d . . . . .
H10 H 0.297835 0.054902 0.522393 0.103 Uiso 1 1 calc R U . . .
C20 C 0.2214(2) 0.0896(2) 0.6329(5) 0.0791(13) Uani 1 1 d . . . . .
H11 H 0.215292 0.057156 0.712102 0.095 Uiso 1 1 calc R U . . .
C21 C 0.18087(19) 0.13859(19) 0.6308(5) 0.0716(11) Uani 1 1 d . . . . .
H12 H 0.147612 0.139407 0.709223 0.086 Uiso 1 1 calc R U . . .
C22 C 0.18926(18) 0.18636(18) 0.5131(5) 0.0599(10) Uani 1 1 d . . . . .
H13 H 0.162071 0.219826 0.512855 0.072 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N2 1.932(2) 5_656 ?
Co1 N2 1.932(2) . ?
Co1 N1 1.934(2) . ?
Co1 N1 1.934(2) 5_656 ?
Co1 Cl1 2.2726(7) . ?
Co1 Cl1 2.2726(7) 5_656 ?
N1 C8 1.362(3) . ?
N1 C1 1.367(4) . ?
N2 C16 1.372(3) . ?
N2 C9 1.374(3) . ?
N3 C9 1.318(3) . ?
N3 C8 1.332(3) . ?
N4 C16 1.317(3) 5_656 ?
N4 C1 1.319(3) . ?
C1 C2 1.467(4) . ?
C2 C7 1.385(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.395(4) . ?
C4 C5 1.388(4) . ?
C5 C6 1.392(4) . ?
C6 C7 1.391(4) . ?
C7 C8 1.453(4) . ?
C9 C10 1.451(4) . ?
C10 C11 1.385(4) . ?
C10 C15 1.388(4) . ?
C11 C12 1.392(4) . ?
C12 C13 1.388(4) . ?
C13 C14 1.372(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.463(4) . ?
P1 C17 1.790(3) 2 ?
P1 C17 1.790(3) 7_566 ?
P1 C17 1.790(3) 8_656 ?
P1 C17 1.790(3) . ?
C17 C18 1.372(5) . ?
C17 C22 1.407(5) . ?
C18 C19 1.392(5) . ?
C19 C20 1.362(6) . ?
C20 C21 1.371(6) . ?
C21 C22 1.372(5) . ?

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
N2 Co1 N2 180.0 5_656 . ?
N2 Co1 N1 90.24(10) 5_656 . ?
N2 Co1 N1 89.76(10) . . ?
N2 Co1 N1 89.76(10) 5_656 5_656 ?
N2 Co1 N1 90.24(10) . 5_656 ?
N1 Co1 N1 180.00(13) . 5_656 ?
N2 Co1 Cl1 92.29(7) 5_656 . ?
N2 Co1 Cl1 87.71(7) . . ?
N1 Co1 Cl1 92.75(7) . . ?
N1 Co1 Cl1 87.25(7) 5_656 . ?
N2 Co1 Cl1 87.71(7) 5_656 5_656 ?
N2 Co1 Cl1 92.29(7) . 5_656 ?
N1 Co1 Cl1 87.25(7) . 5_656 ?
N1 Co1 Cl1 92.75(7) 5_656 5_656 ?
Cl1 Co1 Cl1 180.0 . 5_656 ?
C8 N1 C1 108.0(2) . . ?
C8 N1 Co1 126.18(19) . . ?
C1 N1 Co1 125.40(18) . . ?
C16 N2 C9 107.8(2) . . ?
C16 N2 Co1 125.48(18) . . ?
C9 N2 Co1 126.42(19) . . ?
C9 N3 C8 121.4(3) . . ?
C16 N4 C1 121.3(3) 5_656 . ?
N4 C1 N1 128.7(3) . . ?
N4 C1 C2 121.8(3) . . ?
N1 C1 C2 109.3(2) . . ?
C7 C2 C3 122.1(3) . . ?
C7 C2 C1 106.2(2) . . ?
C3 C2 C1 131.6(3) . . ?
C2 C3 C4 116.6(3) . . ?
C5 C4 C3 121.7(3) . . ?
C4 C5 C6 121.0(3) . . ?
C7 C6 C5 117.7(3) . . ?
C2 C7 C6 120.8(3) . . ?
C2 C7 C8 106.5(2) . . ?
C6 C7 C8 132.6(3) . . ?
N3 C8 N1 128.2(3) . . ?
N3 C8 C7 121.9(2) . . ?
N1 C8 C7 110.0(2) . . ?
N3 C9 N2 127.8(3) . . ?
N3 C9 C10 122.6(3) . . ?
N2 C9 C10 109.6(2) . . ?
C11 C10 C15 121.0(3) . . ?
C11 C10 C9 132.2(3) . . ?
C15 C10 C9 106.8(2) . . ?
C10 C11 C12 117.3(3) . . ?
C13 C12 C11 120.8(3) . . ?
C14 C13 C12 122.2(3) . . ?
C13 C14 C15 116.8(3) . . ?
C10 C15 C14 121.8(3) . . ?
C10 C15 C16 106.3(2) . . ?
C14 C15 C16 131.9(3) . . ?
N4 C16 N2 128.5(3) 5_656 . ?
N4 C16 C15 122.0(3) 5_656 . ?
N2 C16 C15 109.4(2) . . ?
C17 P1 C17 111.21(11) 2 7_566 ?
C17 P1 C17 111.21(11) 2 8_656 ?
C17 P1 C17 106.0(2) 7_566 8_656 ?
C17 P1 C17 106.0(2) 2 . ?
C17 P1 C17 111.21(11) 7_566 . ?
C17 P1 C17 111.21(11) 8_656 . ?
C18 C17 C22 119.5(3) . . ?
C18 C17 P1 122.3(3) . . ?
C22 C17 P1 117.9(3) . . ?
C17 C18 C19 119.3(4) . . ?
C20 C19 C18 120.7(4) . . ?
C19 C20 C21 120.4(4) . . ?
C20 C21 C22 120.1(4) . . ?
C21 C22 C17 119.9(4) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N4 C1 N1 -0.4(5) 5_656 . . . ?
C16 N4 C1 C2 -176.5(3) 5_656 . . . ?
C8 N1 C1 N4 -176.3(3) . . . . ?
Co1 N1 C1 N4 -3.7(4) . . . . ?
C8 N1 C1 C2 0.2(3) . . . . ?
Co1 N1 C1 C2 172.74(18) . . . . ?
N4 C1 C2 C7 176.6(3) . . . . ?
N1 C1 C2 C7 -0.1(3) . . . . ?
N4 C1 C2 C3 -1.5(5) . . . . ?
N1 C1 C2 C3 -178.2(3) . . . . ?
C7 C2 C3 C4 -1.3(4) . . . . ?
C1 C2 C3 C4 176.6(3) . . . . ?
C2 C3 C4 C5 0.8(5) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C4 C5 C6 C7 -0.2(5) . . . . ?
C3 C2 C7 C6 1.0(4) . . . . ?
C1 C2 C7 C6 -177.3(3) . . . . ?
C3 C2 C7 C8 178.3(3) . . . . ?
C1 C2 C7 C8 0.0(3) . . . . ?
C5 C6 C7 C2 -0.2(4) . . . . ?
C5 C6 C7 C8 -176.7(3) . . . . ?
C9 N3 C8 N1 -3.7(4) . . . . ?
C9 N3 C8 C7 175.1(3) . . . . ?
C1 N1 C8 N3 178.7(3) . . . . ?
Co1 N1 C8 N3 6.2(4) . . . . ?
C1 N1 C8 C7 -0.2(3) . . . . ?
Co1 N1 C8 C7 -172.66(18) . . . . ?
C2 C7 C8 N3 -178.9(3) . . . . ?
C6 C7 C8 N3 -2.0(5) . . . . ?
C2 C7 C8 N1 0.1(3) . . . . ?
C6 C7 C8 N1 177.0(3) . . . . ?
C8 N3 C9 N2 -1.5(4) . . . . ?
C8 N3 C9 C10 177.1(3) . . . . ?
C16 N2 C9 N3 177.9(3) . . . . ?
Co1 N2 C9 N3 3.6(4) . . . . ?
C16 N2 C9 C10 -0.9(3) . . . . ?
Co1 N2 C9 C10 -175.19(18) . . . . ?
N3 C9 C10 C11 2.1(5) . . . . ?
N2 C9 C10 C11 -179.1(3) . . . . ?
N3 C9 C10 C15 -177.6(3) . . . . ?
N2 C9 C10 C15 1.3(3) . . . . ?
C15 C10 C11 C12 -0.6(4) . . . . ?
C9 C10 C11 C12 179.8(3) . . . . ?
C10 C11 C12 C13 1.0(5) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C12 C13 C14 C15 0.0(5) . . . . ?
C11 C10 C15 C14 -0.1(4) . . . . ?
C9 C10 C15 C14 179.6(3) . . . . ?
C11 C10 C15 C16 179.2(3) . . . . ?
C9 C10 C15 C16 -1.1(3) . . . . ?
C13 C14 C15 C10 0.4(4) . . . . ?
C13 C14 C15 C16 -178.7(3) . . . . ?
C9 N2 C16 N4 -178.2(3) . . . 5_656 ?
Co1 N2 C16 N4 -3.8(4) . . . 5_656 ?
C9 N2 C16 C15 0.2(3) . . . . ?
Co1 N2 C16 C15 174.56(18) . . . . ?
C10 C15 C16 N4 179.1(3) . . . 5_656 ?
C14 C15 C16 N4 -1.7(5) . . . 5_656 ?
C10 C15 C16 N2 0.6(3) . . . . ?
C14 C15 C16 N2 179.8(3) . . . . ?
C17 P1 C17 C18 -114.6(3) 2 . . . ?
C17 P1 C17 C18 124.4(4) 7_566 . . . ?
C17 P1 C17 C18 6.4(3) 8_656 . . . ?
C17 P1 C17 C22 59.0(2) 2 . . . ?
C17 P1 C17 C22 -62.0(2) 7_566 . . . ?
C17 P1 C17 C22 -180.0(3) 8_656 . . . ?
C22 C17 C18 C19 3.7(5) . . . . ?
P1 C17 C18 C19 177.2(3) . . . . ?
C17 C18 C19 C20 -2.2(7) . . . . ?
C18 C19 C20 C21 0.0(7) . . . . ?
C19 C20 C21 C22 0.7(7) . . . . ?
C20 C21 C22 C17 0.9(6) . . . . ?
C18 C17 C22 C21 -3.1(5) . . . . ?
P1 C17 C22 C21 -176.9(3) . . . . ?

_refine_diff_density_max         0.223
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.075

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCoPcBr22rt
_database_code_depnum_ccdc_archive 'CCDC 1947260'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H16 Br2 Co N8), C24 H20 P'
_chemical_formula_sum            'C88 H52 Br4 Co2 N16 P'
_chemical_formula_weight         1801.92

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'
Co Co -2.3653 3.6143 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5347(4)
_cell_length_b                   21.5347(4)
_cell_length_c                   7.63450(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3540.45(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    14835
_cell_measurement_theta_min      4.105
_cell_measurement_theta_max      68.195

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_F_000             1802
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    7.038
_shelx_estimated_absorpt_T_min   0.333
_shelx_estimated_absorpt_T_max   0.540
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7442
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37608
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.106
_diffrn_reflns_theta_max         68.218
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3235
_reflns_number_gt                2795
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3235
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1627
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.000000 0.000000 0.0339(3) Uani 1 2 d S . P . .
Br1 Br 0.40716(2) 0.05478(2) 0.09528(6) 0.0470(2) Uani 1 1 d . . . . .
N1 N 0.51205(13) 0.06748(13) -0.1629(4) 0.0364(7) Uani 1 1 d . . . . .
N2 N 0.55161(14) 0.04238(13) 0.1677(4) 0.0366(7) Uani 1 1 d . . . . .
N3 N 0.57644(14) 0.13606(14) 0.0102(4) 0.0401(8) Uani 1 1 d . . . . .
N4 N 0.44425(14) 0.03452(14) -0.3986(4) 0.0388(7) Uani 1 1 d . . . . .
C1 C 0.48272(17) 0.07414(17) -0.3215(5) 0.0377(8) Uani 1 1 d . . . . .
C2 C 0.49653(17) 0.13481(17) -0.3958(5) 0.0380(8) Uani 1 1 d . . . . .
C3 C 0.47726(18) 0.16381(18) -0.5508(5) 0.0446(9) Uani 1 1 d . . . . .
H1 H 0.452054 0.143629 -0.631705 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4977(2) 0.22423(19) -0.5775(5) 0.0461(10) Uani 1 1 d . . . . .
H2 H 0.486301 0.245136 -0.679150 0.055 Uiso 1 1 calc R U . . .
C5 C 0.53566(19) 0.25448(18) -0.4527(5) 0.0463(9) Uani 1 1 d . . . . .
H3 H 0.547754 0.295348 -0.472325 0.056 Uiso 1 1 calc R U . . .
C6 C 0.55487(17) 0.22507(17) -0.3043(5) 0.0422(9) Uani 1 1 d . . . . .
H4 H 0.580570 0.244821 -0.223778 0.051 Uiso 1 1 calc R U . . .
C7 C 0.53473(16) 0.16459(16) -0.2775(5) 0.0367(8) Uani 1 1 d . . . . .
C8 C 0.54331(17) 0.12106(17) -0.1305(5) 0.0370(8) Uani 1 1 d . . . . .
C9 C 0.58081(16) 0.09872(16) 0.1431(5) 0.0367(8) Uani 1 1 d . . . . .
C10 C 0.61919(16) 0.11225(16) 0.2950(5) 0.0367(8) Uani 1 1 d . . . . .
C11 C 0.65755(17) 0.16236(17) 0.3365(5) 0.0433(9) Uani 1 1 d . . . . .
H5 H 0.662137 0.195808 0.260570 0.052 Uiso 1 1 calc R U . . .
C12 C 0.6887(2) 0.1603(2) 0.4965(5) 0.0490(11) Uani 1 1 d . . . . .
H6 H 0.713680 0.193506 0.529601 0.059 Uiso 1 1 calc R U . . .
C13 C 0.68322(19) 0.1098(2) 0.6063(6) 0.0520(11) Uani 1 1 d . . . . .
H7 H 0.705022 0.109676 0.711439 0.062 Uiso 1 1 calc R U . . .
C14 C 0.64613(18) 0.05922(18) 0.5648(5) 0.0431(9) Uani 1 1 d . . . . .
H8 H 0.643246 0.024939 0.638482 0.052 Uiso 1 1 calc R U . . .
C15 C 0.61392(17) 0.06217(17) 0.4100(5) 0.0387(8) Uani 1 1 d . . . . .
C16 C 0.57083(17) 0.01882(16) 0.3256(5) 0.0359(8) Uani 1 1 d . . . . .
P1 P 0.250000 0.250000 0.250000 0.0414(5) Uani 1 4 d S T P . .
C17 C 0.31417(18) 0.26582(18) 0.1082(5) 0.0444(9) Uani 1 1 d . . . . .
C18 C 0.3672(2) 0.2304(2) 0.1071(6) 0.0547(11) Uani 1 1 d . . . . .
H9 H 0.371524 0.198023 0.186917 0.066 Uiso 1 1 calc R U . . .
C19 C 0.4146(2) 0.2425(3) -0.0132(6) 0.0727(15) Uani 1 1 d . . . . .
H10 H 0.450986 0.219199 -0.012063 0.087 Uiso 1 1 calc R U . . .
C20 C 0.4068(2) 0.2888(3) -0.1316(7) 0.0707(14) Uani 1 1 d . . . . .
H11 H 0.438257 0.296984 -0.211597 0.085 Uiso 1 1 calc R U . . .
C21 C 0.3536(2) 0.3238(2) -0.1364(6) 0.0629(12) Uani 1 1 d . . . . .
H12 H 0.349423 0.355219 -0.219257 0.075 Uiso 1 1 calc R U . . .
C22 C 0.3074(2) 0.3128(2) -0.0212(6) 0.0578(12) Uani 1 1 d . . . . .
H13 H 0.270975 0.336018 -0.026418 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N2 1.926(3) 5_655 ?
Co1 N2 1.926(3) . ?
Co1 N1 1.930(3) . ?
Co1 N1 1.930(3) 5_655 ?
Co1 Br1 2.4328(4) . ?
Co1 Br1 2.4328(4) 5_655 ?
N1 C8 1.358(4) . ?
N1 C1 1.373(5) . ?
N2 C16 1.372(4) . ?
N2 C9 1.379(4) . ?
N3 C9 1.298(4) . ?
N3 C8 1.330(4) . ?
N4 C16 1.317(4) 5_655 ?
N4 C1 1.327(4) . ?
C1 C2 1.455(5) . ?
C2 C7 1.380(5) . ?
C2 C3 1.401(5) . ?
C3 C4 1.389(5) . ?
C4 C5 1.414(5) . ?
C5 C6 1.362(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.474(5) . ?
C9 C10 1.454(5) . ?
C10 C11 1.396(5) . ?
C10 C15 1.395(5) . ?
C11 C12 1.394(5) . ?
C12 C13 1.377(6) . ?
C13 C14 1.388(5) . ?
C14 C15 1.372(5) . ?
C15 C16 1.465(5) . ?
P1 C17 1.788(4) . ?
P1 C17 1.788(4) 2 ?
P1 C17 1.788(4) 8_656 ?
P1 C17 1.788(4) 7_566 ?
C17 C18 1.373(6) . ?
C17 C22 1.422(6) . ?
C18 C19 1.399(6) . ?
C19 C20 1.356(7) . ?
C20 C21 1.372(7) . ?
C21 C22 1.350(6) . ?

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
N2 Co1 N2 180.00(15) 5_655 . ?
N2 Co1 N1 90.34(13) 5_655 . ?
N2 Co1 N1 89.66(13) . . ?
N2 Co1 N1 89.66(13) 5_655 5_655 ?
N2 Co1 N1 90.34(13) . 5_655 ?
N1 Co1 N1 180.0 . 5_655 ?
N2 Co1 Br1 87.38(9) 5_655 . ?
N2 Co1 Br1 92.62(9) . . ?
N1 Co1 Br1 86.45(9) . . ?
N1 Co1 Br1 93.55(9) 5_655 . ?
N2 Co1 Br1 92.62(9) 5_655 5_655 ?
N2 Co1 Br1 87.38(9) . 5_655 ?
N1 Co1 Br1 93.55(9) . 5_655 ?
N1 Co1 Br1 86.45(9) 5_655 5_655 ?
Br1 Co1 Br1 180.0 . 5_655 ?
C8 N1 C1 107.4(3) . . ?
C8 N1 Co1 126.1(2) . . ?
C1 N1 Co1 125.8(2) . . ?
C16 N2 C9 107.9(3) . . ?
C16 N2 Co1 125.7(2) . . ?
C9 N2 Co1 126.1(2) . . ?
C9 N3 C8 121.3(3) . . ?
C16 N4 C1 121.8(3) 5_655 . ?
N4 C1 N1 127.7(3) . . ?
N4 C1 C2 122.2(3) . . ?
N1 C1 C2 110.1(3) . . ?
C7 C2 C3 121.5(3) . . ?
C7 C2 C1 106.5(3) . . ?
C3 C2 C1 132.0(3) . . ?
C4 C3 C2 116.6(4) . . ?
C3 C4 C5 121.0(4) . . ?
C6 C5 C4 121.5(4) . . ?
C5 C6 C7 117.6(3) . . ?
C2 C7 C6 121.7(3) . . ?
C2 C7 C8 106.1(3) . . ?
C6 C7 C8 132.1(3) . . ?
N3 C8 N1 128.3(3) . . ?
N3 C8 C7 121.9(3) . . ?
N1 C8 C7 109.9(3) . . ?
N3 C9 N2 128.2(3) . . ?
N3 C9 C10 122.7(3) . . ?
N2 C9 C10 109.1(3) . . ?
C11 C10 C15 120.2(3) . . ?
C11 C10 C9 132.3(3) . . ?
C15 C10 C9 107.5(3) . . ?
C12 C11 C10 117.3(4) . . ?
C13 C12 C11 121.1(4) . . ?
C12 C13 C14 122.0(4) . . ?
C15 C14 C13 116.8(4) . . ?
C14 C15 C10 122.5(3) . . ?
C14 C15 C16 132.0(3) . . ?
C10 C15 C16 105.5(3) . . ?
N4 C16 N2 128.3(3) 5_655 . ?
N4 C16 C15 121.7(3) 5_655 . ?
N2 C16 C15 110.0(3) . . ?
C17 P1 C17 105.5(3) . 2 ?
C17 P1 C17 111.51(14) . 8_656 ?
C17 P1 C17 111.50(14) 2 8_656 ?
C17 P1 C17 111.50(14) . 7_566 ?
C17 P1 C17 111.50(14) 2 7_566 ?
C17 P1 C17 105.5(3) 8_656 7_566 ?
C18 C17 C22 118.5(4) . . ?
C18 C17 P1 122.7(3) . . ?
C22 C17 P1 118.4(3) . . ?
C17 C18 C19 120.5(5) . . ?
C20 C19 C18 118.9(5) . . ?
C19 C20 C21 121.8(5) . . ?
C22 C21 C20 120.1(5) . . ?
C21 C22 C17 120.1(5) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N4 C1 N1 0.2(6) 5_655 . . . ?
C16 N4 C1 C2 -176.0(3) 5_655 . . . ?
C8 N1 C1 N4 -175.7(4) . . . . ?
Co1 N1 C1 N4 -4.9(5) . . . . ?
C8 N1 C1 C2 0.8(4) . . . . ?
Co1 N1 C1 C2 171.7(2) . . . . ?
N4 C1 C2 C7 176.5(3) . . . . ?
N1 C1 C2 C7 -0.2(4) . . . . ?
N4 C1 C2 C3 -1.9(7) . . . . ?
N1 C1 C2 C3 -178.7(4) . . . . ?
C7 C2 C3 C4 -1.0(6) . . . . ?
C1 C2 C3 C4 177.2(4) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
C3 C4 C5 C6 1.8(7) . . . . ?
C4 C5 C6 C7 -1.4(6) . . . . ?
C3 C2 C7 C6 1.4(6) . . . . ?
C1 C2 C7 C6 -177.3(3) . . . . ?
C3 C2 C7 C8 178.3(3) . . . . ?
C1 C2 C7 C8 -0.4(4) . . . . ?
C5 C6 C7 C2 -0.1(6) . . . . ?
C5 C6 C7 C8 -176.1(4) . . . . ?
C9 N3 C8 N1 -2.4(6) . . . . ?
C9 N3 C8 C7 176.1(3) . . . . ?
C1 N1 C8 N3 177.6(4) . . . . ?
Co1 N1 C8 N3 6.7(6) . . . . ?
C1 N1 C8 C7 -1.0(4) . . . . ?
Co1 N1 C8 C7 -171.9(2) . . . . ?
C2 C7 C8 N3 -177.9(3) . . . . ?
C6 C7 C8 N3 -1.4(6) . . . . ?
C2 C7 C8 N1 0.9(4) . . . . ?
C6 C7 C8 N1 177.4(4) . . . . ?
C8 N3 C9 N2 -3.9(6) . . . . ?
C8 N3 C9 C10 176.7(4) . . . . ?
C16 N2 C9 N3 179.0(4) . . . . ?
Co1 N2 C9 N3 5.0(6) . . . . ?
C16 N2 C9 C10 -1.5(4) . . . . ?
Co1 N2 C9 C10 -175.5(2) . . . . ?
N3 C9 C10 C11 -0.3(6) . . . . ?
N2 C9 C10 C11 -179.8(4) . . . . ?
N3 C9 C10 C15 -178.9(3) . . . . ?
N2 C9 C10 C15 1.6(4) . . . . ?
C15 C10 C11 C12 -1.0(6) . . . . ?
C9 C10 C11 C12 -179.6(4) . . . . ?
C10 C11 C12 C13 1.9(6) . . . . ?
C11 C12 C13 C14 -0.8(7) . . . . ?
C12 C13 C14 C15 -1.3(6) . . . . ?
C13 C14 C15 C10 2.2(6) . . . . ?
C13 C14 C15 C16 -179.4(4) . . . . ?
C11 C10 C15 C14 -1.0(6) . . . . ?
C9 C10 C15 C14 177.8(4) . . . . ?
C11 C10 C15 C16 -179.8(3) . . . . ?
C9 C10 C15 C16 -0.9(4) . . . . ?
C9 N2 C16 N4 -178.2(4) . . . 5_655 ?
Co1 N2 C16 N4 -4.2(6) . . . 5_655 ?
C9 N2 C16 C15 0.9(4) . . . . ?
Co1 N2 C16 C15 174.9(2) . . . . ?
C14 C15 C16 N4 0.7(7) . . . 5_655 ?
C10 C15 C16 N4 179.2(3) . . . 5_655 ?
C14 C15 C16 N2 -178.6(4) . . . . ?
C10 C15 C16 N2 0.0(4) . . . . ?
C17 P1 C17 C18 -118.6(4) 2 . . . ?
C17 P1 C17 C18 120.2(5) 8_656 . . . ?
C17 P1 C17 C18 2.6(4) 7_566 . . . ?
C17 P1 C17 C22 54.5(3) 2 . . . ?
C17 P1 C17 C22 -66.7(3) 8_656 . . . ?
C17 P1 C17 C22 175.7(4) 7_566 . . . ?
C22 C17 C18 C19 3.2(7) . . . . ?
P1 C17 C18 C19 176.4(4) . . . . ?
C17 C18 C19 C20 -1.7(8) . . . . ?
C18 C19 C20 C21 -0.1(8) . . . . ?
C19 C20 C21 C22 0.2(8) . . . . ?
C20 C21 C22 C17 1.4(7) . . . . ?
C18 C17 C22 C21 -3.1(7) . . . . ?
P1 C17 C22 C21 -176.6(4) . . . . ?

_refine_diff_density_max         0.402
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.096

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCotbpCl22rt
_database_code_depnum_ccdc_archive 'CCDC 1947253'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Cl2 Co N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Cl4 Co2 N8 P'
_chemical_formula_weight         1616.15

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.6858(4)
_cell_length_b                   21.6858(4)
_cell_length_c                   7.58710(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3568.01(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    15413
_cell_measurement_theta_min      4.075
_cell_measurement_theta_max      68.205

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             1658
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    5.700
_shelx_estimated_absorpt_T_min   0.395
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38337
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.077
_diffrn_reflns_theta_max         68.204
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3238
_reflns_number_gt                2604
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3238
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1816
_refine_ls_wR_factor_gt          0.1729
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_restrained_S_all      1.350
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.000000 0.000000 0.500000 0.0404(3) Uani 1 2 d S . P . .
Cl1 Cl 1.08436(4) 0.04864(4) 0.39014(12) 0.0539(3) Uani 1 1 d . . . . .
N1 N 0.94384(12) 0.04335(12) 0.3290(3) 0.0427(6) Uani 1 1 d . . . . .
N2 N 0.99034(12) 0.07068(12) 0.6703(4) 0.0429(6) Uani 1 1 d . . . . .
C1 C 0.94149(16) -0.03466(15) 0.0953(5) 0.0464(8) Uani 1 1 d . . . . .
H1 H 0.925133 -0.044355 -0.014587 0.056 Uiso 1 1 calc R U . . .
C2 C 0.92459(15) 0.02056(15) 0.1677(4) 0.0445(8) Uani 1 1 d . . . . .
C3 C 0.88230(15) 0.06379(15) 0.0851(4) 0.0442(7) Uani 1 1 d . . . . .
C4 C 0.85136(16) 0.06320(17) -0.0736(5) 0.0531(9) Uani 1 1 d . . . . .
H2 H 0.854992 0.030153 -0.150990 0.064 Uiso 1 1 calc R U . . .
C5 C 0.81486(17) 0.11332(18) -0.1135(5) 0.0573(9) Uani 1 1 d . . . . .
H3 H 0.793530 0.113941 -0.219771 0.069 Uiso 1 1 calc R U . . .
C6 C 0.80917(19) 0.16277(19) 0.0008(5) 0.0588(11) Uani 1 1 d . . . . .
H4 H 0.784334 0.195985 -0.030429 0.071 Uiso 1 1 calc R U . . .
C7 C 0.83985(16) 0.16352(16) 0.1606(5) 0.0518(9) Uani 1 1 d . . . . .
H5 H 0.835559 0.196424 0.238287 0.062 Uiso 1 1 calc R U . . .
C8 C 0.87735(14) 0.11345(14) 0.2015(4) 0.0433(7) Uani 1 1 d . . . . .
C9 C 0.91618(15) 0.09907(14) 0.3515(4) 0.0431(8) Uani 1 1 d . . . . .
C10 C 0.92273(17) 0.13679(16) 0.4961(4) 0.0497(9) Uani 1 1 d . . . . .
H6 H 0.901703 0.174167 0.494882 0.060 Uiso 1 1 calc R U . . .
C11 C 0.95779(15) 0.12375(14) 0.6422(4) 0.0427(7) Uani 1 1 d . . . . .
C12 C 0.96647(15) 0.16593(15) 0.7879(4) 0.0440(7) Uani 1 1 d . . . . .
C13 C 0.94578(17) 0.22611(16) 0.8178(5) 0.0512(8) Uani 1 1 d . . . . .
H7 H 0.919819 0.245945 0.738383 0.061 Uiso 1 1 calc R U . . .
C14 C 0.96564(19) 0.25504(17) 0.9711(5) 0.0570(10) Uani 1 1 d . . . . .
H8 H 0.953542 0.295431 0.993449 0.068 Uiso 1 1 calc R U . . .
C15 C 1.00317(18) 0.22482(17) 1.0912(5) 0.0562(9) Uani 1 1 d . . . . .
H9 H 1.015030 0.245145 1.193694 0.067 Uiso 1 1 calc R U . . .
C16 C 1.02342(17) 0.16507(17) 1.0623(5) 0.0539(9) Uani 1 1 d . . . . .
H10 H 1.048391 0.144871 1.143494 0.065 Uiso 1 1 calc R U . . .
C17 C 1.00494(15) 0.13656(15) 0.9071(4) 0.0437(8) Uani 1 1 d . . . . .
C18 C 1.01969(15) 0.07689(15) 0.8299(4) 0.0440(8) Uani 1 1 d . . . . .
P1 P 1.250000 0.250000 0.250000 0.0488(5) Uani 1 4 d S T P . .
C19 C 1.18465(16) 0.25816(17) 0.3929(5) 0.0533(9) Uani 1 1 d . . . . .
C20 C 1.1839(2) 0.3079(2) 0.5092(5) 0.0666(12) Uani 1 1 d . . . . .
H11 H 1.215571 0.336848 0.506162 0.080 Uiso 1 1 calc R U . . .
C21 C 1.1365(2) 0.3144(2) 0.6289(6) 0.0786(13) Uani 1 1 d . . . . .
H12 H 1.135659 0.347708 0.705973 0.094 Uiso 1 1 calc R U . . .
C22 C 1.0907(2) 0.2710(3) 0.6325(7) 0.0880(16) Uani 1 1 d . . . . .
H13 H 1.058117 0.275612 0.711304 0.106 Uiso 1 1 calc R U . . .
C23 C 1.0918(2) 0.2209(3) 0.5225(6) 0.0851(15) Uani 1 1 d . . . . .
H14 H 1.060452 0.191682 0.528603 0.102 Uiso 1 1 calc R U . . .
C24 C 1.13926(17) 0.2136(2) 0.4020(5) 0.0660(11) Uani 1 1 d . . . . .
H15 H 1.140548 0.179255 0.328671 0.079 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N1 2.013(3) . ?
Co1 N1 2.013(3) 5_756 ?
Co1 N2 2.016(3) . ?
Co1 N2 2.016(3) 5_756 ?
Co1 Cl1 2.2703(9) 5_756 ?
Co1 Cl1 2.2703(9) . ?
N1 C9 1.360(4) . ?
N1 C2 1.384(4) . ?
N2 C11 1.367(4) . ?
N2 C18 1.374(4) . ?
C1 C18 1.367(4) 5_756 ?
C1 C2 1.368(4) . ?
C2 C3 1.453(4) . ?
C3 C4 1.378(5) . ?
C3 C8 1.397(4) . ?
C4 C5 1.378(5) . ?
C5 C6 1.384(5) . ?
C6 C7 1.384(5) . ?
C7 C8 1.391(4) . ?
C8 C9 1.450(4) . ?
C9 C10 1.376(4) . ?
C10 C11 1.373(4) . ?
C11 C12 1.447(4) . ?
C12 C17 1.385(4) . ?
C12 C13 1.399(4) . ?
C13 C14 1.390(5) . ?
C14 C15 1.387(5) . ?
C15 C16 1.386(5) . ?
C16 C17 1.389(5) . ?
C17 C18 1.456(4) . ?
P1 C19 1.793(4) 8_746 ?
P1 C19 1.793(4) 2_755 ?
P1 C19 1.793(4) 7_676 ?
P1 C19 1.793(4) . ?
C19 C24 1.381(5) . ?
C19 C20 1.394(5) . ?
C20 C21 1.379(6) . ?
C21 C22 1.369(7) . ?
C22 C23 1.370(7) . ?
C23 C24 1.386(6) . ?

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 Co1 N1 180.0 . 5_756 ?
N1 Co1 N2 89.72(11) . . ?
N1 Co1 N2 90.28(11) 5_756 . ?
N1 Co1 N2 90.28(11) . 5_756 ?
N1 Co1 N2 89.72(11) 5_756 5_756 ?
N2 Co1 N2 180.0 . 5_756 ?
N1 Co1 Cl1 88.06(8) . 5_756 ?
N1 Co1 Cl1 91.95(8) 5_756 5_756 ?
N2 Co1 Cl1 91.96(8) . 5_756 ?
N2 Co1 Cl1 88.04(8) 5_756 5_756 ?
N1 Co1 Cl1 91.94(8) . . ?
N1 Co1 Cl1 88.05(8) 5_756 . ?
N2 Co1 Cl1 88.04(8) . . ?
N2 Co1 Cl1 91.96(8) 5_756 . ?
Cl1 Co1 Cl1 180.0 5_756 . ?
C9 N1 C2 107.2(3) . . ?
C9 N1 Co1 126.9(2) . . ?
C2 N1 Co1 125.9(2) . . ?
C11 N2 C18 107.1(3) . . ?
C11 N2 Co1 126.4(2) . . ?
C18 N2 Co1 126.2(2) . . ?
C18 C1 C2 125.8(3) 5_756 . ?
C1 C2 N1 125.9(3) . . ?
C1 C2 C3 124.1(3) . . ?
N1 C2 C3 109.9(3) . . ?
C4 C3 C8 121.5(3) . . ?
C4 C3 C2 132.7(3) . . ?
C8 C3 C2 105.9(3) . . ?
C5 C4 C3 117.6(3) . . ?
C4 C5 C6 121.7(3) . . ?
C7 C6 C5 121.0(4) . . ?
C6 C7 C8 117.8(3) . . ?
C7 C8 C3 120.4(3) . . ?
C7 C8 C9 133.0(3) . . ?
C3 C8 C9 106.6(3) . . ?
N1 C9 C10 125.7(3) . . ?
N1 C9 C8 110.4(3) . . ?
C10 C9 C8 123.9(3) . . ?
C11 C10 C9 125.3(3) . . ?
N2 C11 C10 125.8(3) . . ?
N2 C11 C12 110.2(3) . . ?
C10 C11 C12 123.9(3) . . ?
C17 C12 C13 121.1(3) . . ?
C17 C12 C11 106.6(3) . . ?
C13 C12 C11 132.2(3) . . ?
C14 C13 C12 117.2(3) . . ?
C15 C14 C13 121.2(3) . . ?
C16 C15 C14 121.6(3) . . ?
C15 C16 C17 117.3(4) . . ?
C12 C17 C16 121.5(3) . . ?
C12 C17 C18 106.1(3) . . ?
C16 C17 C18 132.3(3) . . ?
C1 C18 N2 125.8(3) 5_756 . ?
C1 C18 C17 124.3(3) 5_756 . ?
N2 C18 C17 109.9(3) . . ?
C19 P1 C19 111.44(12) 8_746 2_755 ?
C19 P1 C19 105.6(2) 8_746 7_676 ?
C19 P1 C19 111.44(12) 2_755 7_676 ?
C19 P1 C19 111.44(12) 8_746 . ?
C19 P1 C19 105.6(2) 2_755 . ?
C19 P1 C19 111.44(12) 7_676 . ?
C24 C19 C20 120.1(4) . . ?
C24 C19 P1 121.6(3) . . ?
C20 C19 P1 117.9(3) . . ?
C21 C20 C19 120.2(4) . . ?
C22 C21 C20 119.0(5) . . ?
C21 C22 C23 121.3(4) . . ?
C22 C23 C24 120.4(4) . . ?
C19 C24 C23 118.8(4) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C1 C2 N1 0.1(6) 5_756 . . . ?
C18 C1 C2 C3 -178.9(3) 5_756 . . . ?
C9 N1 C2 C1 -179.6(3) . . . . ?
Co1 N1 C2 C1 -1.5(5) . . . . ?
C9 N1 C2 C3 -0.5(4) . . . . ?
Co1 N1 C2 C3 177.6(2) . . . . ?
C1 C2 C3 C4 -1.7(6) . . . . ?
N1 C2 C3 C4 179.1(4) . . . . ?
C1 C2 C3 C8 179.7(3) . . . . ?
N1 C2 C3 C8 0.6(4) . . . . ?
C8 C3 C4 C5 -0.4(5) . . . . ?
C2 C3 C4 C5 -178.8(4) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C6 C7 C8 1.0(6) . . . . ?
C6 C7 C8 C3 -1.4(5) . . . . ?
C6 C7 C8 C9 179.0(4) . . . . ?
C4 C3 C8 C7 1.1(5) . . . . ?
C2 C3 C8 C7 179.9(3) . . . . ?
C4 C3 C8 C9 -179.2(3) . . . . ?
C2 C3 C8 C9 -0.4(4) . . . . ?
C2 N1 C9 C10 179.4(3) . . . . ?
Co1 N1 C9 C10 1.3(5) . . . . ?
C2 N1 C9 C8 0.3(4) . . . . ?
Co1 N1 C9 C8 -177.8(2) . . . . ?
C7 C8 C9 N1 179.8(4) . . . . ?
C3 C8 C9 N1 0.1(4) . . . . ?
C7 C8 C9 C10 0.7(6) . . . . ?
C3 C8 C9 C10 -179.0(3) . . . . ?
N1 C9 C10 C11 -0.8(6) . . . . ?
C8 C9 C10 C11 178.2(3) . . . . ?
C18 N2 C11 C10 178.9(3) . . . . ?
Co1 N2 C11 C10 4.1(5) . . . . ?
C18 N2 C11 C12 0.2(4) . . . . ?
Co1 N2 C11 C12 -174.5(2) . . . . ?
C9 C10 C11 N2 -2.1(6) . . . . ?
C9 C10 C11 C12 176.4(3) . . . . ?
N2 C11 C12 C17 -0.6(4) . . . . ?
C10 C11 C12 C17 -179.3(3) . . . . ?
N2 C11 C12 C13 176.6(3) . . . . ?
C10 C11 C12 C13 -2.0(6) . . . . ?
C17 C12 C13 C14 0.3(5) . . . . ?
C11 C12 C13 C14 -176.7(4) . . . . ?
C12 C13 C14 C15 -1.6(6) . . . . ?
C13 C14 C15 C16 1.3(6) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C13 C12 C17 C16 1.4(5) . . . . ?
C11 C12 C17 C16 179.0(3) . . . . ?
C13 C12 C17 C18 -176.9(3) . . . . ?
C11 C12 C17 C18 0.7(4) . . . . ?
C15 C16 C17 C12 -1.7(5) . . . . ?
C15 C16 C17 C18 176.1(4) . . . . ?
C11 N2 C18 C1 -178.0(3) . . . 5_756 ?
Co1 N2 C18 C1 -3.2(5) . . . 5_756 ?
C11 N2 C18 C17 0.2(4) . . . . ?
Co1 N2 C18 C17 175.0(2) . . . . ?
C12 C17 C18 C1 177.7(3) . . . 5_756 ?
C16 C17 C18 C1 -0.3(6) . . . 5_756 ?
C12 C17 C18 N2 -0.6(4) . . . . ?
C16 C17 C18 N2 -178.6(4) . . . . ?
C19 P1 C19 C24 8.0(3) 8_746 . . . ?
C19 P1 C19 C24 -113.2(4) 2_755 . . . ?
C19 P1 C19 C24 125.7(4) 7_676 . . . ?
C19 P1 C19 C20 -178.7(3) 8_746 . . . ?
C19 P1 C19 C20 60.2(3) 2_755 . . . ?
C19 P1 C19 C20 -61.0(2) 7_676 . . . ?
C24 C19 C20 C21 -2.9(6) . . . . ?
P1 C19 C20 C21 -176.3(3) . . . . ?
C19 C20 C21 C22 0.6(7) . . . . ?
C20 C21 C22 C23 1.3(8) . . . . ?
C21 C22 C23 C24 -1.0(8) . . . . ?
C20 C19 C24 C23 3.1(6) . . . . ?
P1 C19 C24 C23 176.3(3) . . . . ?
C22 C23 C24 C19 -1.2(7) . . . . ?

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.066

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCotbpCl22LT
_database_code_depnum_ccdc_archive 'CCDC 1947254'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Cl2 Co N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Cl4 Co2 N8 P'
_chemical_formula_weight         1616.15

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'
Cl Cl 0.3639 0.7018 '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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5443(4)
_cell_length_b                   21.5443(4)
_cell_length_c                   7.52580(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3493.15(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    15170
_cell_measurement_theta_min      4.105
_cell_measurement_theta_max      68.15

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_F_000             1658
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    5.822
_shelx_estimated_absorpt_T_min   0.389
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8588
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36216
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.104
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3190
_reflns_number_gt                2737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3190
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1651
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_restrained_S_all      1.285
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.000000 0.000000 0.500000 0.0260(2) Uani 1 2 d S . P . .
Cl1 Cl 0.95056(3) -0.08486(3) 0.39272(10) 0.0324(2) Uani 1 1 d . . . . .
N1 N 0.95645(11) 0.05607(10) 0.3276(3) 0.0274(6) Uani 1 1 d . . . . .
N2 N 0.92905(10) 0.01023(11) 0.6722(3) 0.0274(5) Uani 1 1 d . . . . .
C1 C 1.03491(13) 0.05862(13) 0.0909(4) 0.0291(6) Uani 1 1 d . . . . .
H1 H 1.044747 0.075362 -0.022451 0.035 Uiso 1 1 calc R U . . .
C2 C 0.97940(14) 0.07573(13) 0.1653(4) 0.0293(6) Uani 1 1 d . . . . .
C3 C 0.93565(13) 0.11814(13) 0.0814(4) 0.0295(6) Uani 1 1 d . . . . .
C4 C 0.93665(14) 0.14936(14) -0.0785(4) 0.0332(7) Uani 1 1 d . . . . .
H2 H 0.970858 0.145812 -0.157542 0.040 Uiso 1 1 calc R U . . .
C5 C 0.88580(14) 0.18616(14) -0.1196(4) 0.0351(7) Uani 1 1 d . . . . .
H3 H 0.885064 0.207813 -0.229548 0.042 Uiso 1 1 calc R U . . .
C6 C 0.83587(16) 0.19211(16) -0.0037(4) 0.0370(8) Uani 1 1 d . . . . .
H4 H 0.801793 0.217773 -0.035674 0.044 Uiso 1 1 calc R U . . .
C7 C 0.83511(13) 0.16112(14) 0.1579(4) 0.0327(7) Uani 1 1 d . . . . .
H5 H 0.801258 0.165444 0.237786 0.039 Uiso 1 1 calc R U . . .
C8 C 0.88565(13) 0.12345(13) 0.1990(4) 0.0294(6) Uani 1 1 d . . . . .
C9 C 0.90038(13) 0.08442(13) 0.3501(4) 0.0283(6) Uani 1 1 d . . . . .
C10 C 0.86215(14) 0.07839(15) 0.4964(4) 0.0326(7) Uani 1 1 d . . . . .
H6 H 0.823783 0.100111 0.495090 0.039 Uiso 1 1 calc R U . . .
C11 C 0.87563(13) 0.04319(13) 0.6440(4) 0.0275(6) Uani 1 1 d . . . . .
C12 C 0.83306(13) 0.03470(13) 0.7910(4) 0.0301(6) Uani 1 1 d . . . . .
C13 C 0.77279(13) 0.05539(14) 0.8211(4) 0.0310(6) Uani 1 1 d . . . . .
H7 H 0.752533 0.082326 0.739681 0.037 Uiso 1 1 calc R U . . .
C14 C 0.74323(14) 0.03503(15) 0.9756(4) 0.0338(7) Uani 1 1 d . . . . .
H8 H 0.701640 0.047339 0.998379 0.041 Uiso 1 1 calc R U . . .
C15 C 0.77376(14) -0.00300(14) 1.0968(4) 0.0329(7) Uani 1 1 d . . . . .
H9 H 0.752777 -0.015382 1.201989 0.040 Uiso 1 1 calc R U . . .
C16 C 0.83410(14) -0.02336(14) 1.0680(4) 0.0342(7) Uani 1 1 d . . . . .
H10 H 0.854926 -0.049035 1.151512 0.041 Uiso 1 1 calc R U . . .
C17 C 0.86274(13) -0.00441(13) 0.9109(4) 0.0275(6) Uani 1 1 d . . . . .
C18 C 0.92259(13) -0.01929(13) 0.8332(4) 0.0292(6) Uani 1 1 d . . . . .
P1 P 0.750000 -0.250000 0.250000 0.0277(4) Uani 1 4 d S T P . .
C19 C 0.74150(13) -0.18448(14) 0.3947(4) 0.0309(7) Uani 1 1 d . . . . .
C20 C 0.78715(16) -0.13885(14) 0.4049(4) 0.0362(7) Uani 1 1 d . . . . .
H11 H 0.822495 -0.140410 0.329537 0.043 Uiso 1 1 calc R U . . .
C21 C 0.78016(18) -0.09102(16) 0.5271(5) 0.0450(9) Uani 1 1 d . . . . .
H12 H 0.810520 -0.059124 0.533648 0.054 Uiso 1 1 calc R U . . .
C22 C 0.72936(17) -0.08950(16) 0.6391(5) 0.0456(9) Uani 1 1 d . . . . .
H13 H 0.725024 -0.056455 0.721742 0.055 Uiso 1 1 calc R U . . .
C23 C 0.68464(17) -0.13578(16) 0.6321(5) 0.0430(8) Uani 1 1 d . . . . .
H14 H 0.650054 -0.134715 0.710304 0.052 Uiso 1 1 calc R U . . .
C24 C 0.69080(16) -0.18353(15) 0.5101(4) 0.0361(8) Uani 1 1 d . . . . .
H15 H 0.660566 -0.215582 0.505004 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N1 2.006(2) . ?
Co1 N1 2.006(2) 5_756 ?
Co1 N2 2.016(2) . ?
Co1 N2 2.016(2) 5_756 ?
Co1 Cl1 2.2647(7) . ?
Co1 Cl1 2.2647(7) 5_756 ?
N1 C9 1.364(3) . ?
N1 C2 1.384(4) . ?
N2 C11 1.369(3) . ?
N2 C18 1.375(4) . ?
C1 C2 1.371(4) . ?
C1 C18 1.372(4) 5_756 ?
C2 C3 1.457(4) . ?
C3 C4 1.379(4) . ?
C3 C8 1.399(4) . ?
C4 C5 1.387(4) . ?
C5 C6 1.391(4) . ?
C6 C7 1.388(4) . ?
C7 C8 1.393(4) . ?
C8 C9 1.450(4) . ?
C9 C10 1.381(4) . ?
C10 C11 1.376(4) . ?
C11 C12 1.449(4) . ?
C12 C17 1.390(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.397(4) . ?
C14 C15 1.391(4) . ?
C15 C16 1.389(4) . ?
C16 C17 1.395(4) . ?
C17 C18 1.452(4) . ?
P1 C19 1.792(3) 8_646 ?
P1 C19 1.792(3) 7_666 ?
P1 C19 1.792(3) 2_645 ?
P1 C19 1.792(3) . ?
C19 C20 1.393(4) . ?
C19 C24 1.396(4) . ?
C20 C21 1.389(4) . ?
C21 C22 1.382(5) . ?
C22 C23 1.387(5) . ?
C23 C24 1.385(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 Co1 N1 180.0 . 5_756 ?
N1 Co1 N2 89.73(10) . . ?
N1 Co1 N2 90.27(10) 5_756 . ?
N1 Co1 N2 90.26(10) . 5_756 ?
N1 Co1 N2 89.74(10) 5_756 5_756 ?
N2 Co1 N2 180.0 . 5_756 ?
N1 Co1 Cl1 92.04(7) . . ?
N1 Co1 Cl1 87.96(7) 5_756 . ?
N2 Co1 Cl1 87.75(7) . . ?
N2 Co1 Cl1 92.25(7) 5_756 . ?
N1 Co1 Cl1 87.96(7) . 5_756 ?
N1 Co1 Cl1 92.04(7) 5_756 5_756 ?
N2 Co1 Cl1 92.25(7) . 5_756 ?
N2 Co1 Cl1 87.75(7) 5_756 5_756 ?
Cl1 Co1 Cl1 180.0 . 5_756 ?
C9 N1 C2 106.8(2) . . ?
C9 N1 Co1 127.12(19) . . ?
C2 N1 Co1 126.02(18) . . ?
C11 N2 C18 106.9(2) . . ?
C11 N2 Co1 126.47(19) . . ?
C18 N2 Co1 126.33(19) . . ?
C2 C1 C18 125.3(3) . 5_756 ?
C1 C2 N1 126.2(3) . . ?
C1 C2 C3 123.8(3) . . ?
N1 C2 C3 110.1(2) . . ?
C4 C3 C8 121.6(3) . . ?
C4 C3 C2 132.4(3) . . ?
C8 C3 C2 106.0(3) . . ?
C3 C4 C5 117.4(3) . . ?
C4 C5 C6 121.6(3) . . ?
C7 C6 C5 121.0(3) . . ?
C6 C7 C8 117.8(3) . . ?
C7 C8 C3 120.6(3) . . ?
C7 C8 C9 133.1(3) . . ?
C3 C8 C9 106.3(2) . . ?
N1 C9 C10 125.8(3) . . ?
N1 C9 C8 110.9(2) . . ?
C10 C9 C8 123.3(3) . . ?
C11 C10 C9 124.7(3) . . ?
N2 C11 C10 126.1(3) . . ?
N2 C11 C12 110.4(2) . . ?
C10 C11 C12 123.5(3) . . ?
C17 C12 C13 121.2(3) . . ?
C17 C12 C11 106.3(2) . . ?
C13 C12 C11 132.4(3) . . ?
C12 C13 C14 117.4(3) . . ?
C15 C14 C13 121.0(3) . . ?
C16 C15 C14 121.8(3) . . ?
C15 C16 C17 117.0(3) . . ?
C12 C17 C16 121.6(3) . . ?
C12 C17 C18 106.3(3) . . ?
C16 C17 C18 132.0(3) . . ?
C1 C18 N2 125.8(3) 5_756 . ?
C1 C18 C17 124.2(3) 5_756 . ?
N2 C18 C17 110.0(2) . . ?
C19 P1 C19 105.17(19) 8_646 7_666 ?
C19 P1 C19 111.66(10) 8_646 2_645 ?
C19 P1 C19 111.66(10) 7_666 2_645 ?
C19 P1 C19 111.66(10) 8_646 . ?
C19 P1 C19 111.66(10) 7_666 . ?
C19 P1 C19 105.18(19) 2_645 . ?
C20 C19 C24 120.5(3) . . ?
C20 C19 P1 121.2(2) . . ?
C24 C19 P1 118.0(2) . . ?
C21 C20 C19 118.9(3) . . ?
C22 C21 C20 120.5(3) . . ?
C21 C22 C23 120.6(3) . . ?
C24 C23 C22 119.5(3) . . ?
C23 C24 C19 119.9(3) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C1 C2 N1 -0.7(5) 5_756 . . . ?
C18 C1 C2 C3 179.4(3) 5_756 . . . ?
C9 N1 C2 C1 179.7(3) . . . . ?
Co1 N1 C2 C1 2.5(4) . . . . ?
C9 N1 C2 C3 -0.3(3) . . . . ?
Co1 N1 C2 C3 -177.53(18) . . . . ?
C1 C2 C3 C4 0.6(5) . . . . ?
N1 C2 C3 C4 -179.4(3) . . . . ?
C1 C2 C3 C8 -179.9(3) . . . . ?
N1 C2 C3 C8 0.2(3) . . . . ?
C8 C3 C4 C5 -0.4(5) . . . . ?
C2 C3 C4 C5 179.0(3) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C4 C5 C6 C7 -0.2(5) . . . . ?
C5 C6 C7 C8 -0.7(5) . . . . ?
C6 C7 C8 C3 0.9(4) . . . . ?
C6 C7 C8 C9 -179.1(3) . . . . ?
C4 C3 C8 C7 -0.4(5) . . . . ?
C2 C3 C8 C7 -180.0(3) . . . . ?
C4 C3 C8 C9 179.6(3) . . . . ?
C2 C3 C8 C9 0.1(3) . . . . ?
C2 N1 C9 C10 -178.8(3) . . . . ?
Co1 N1 C9 C10 -1.7(4) . . . . ?
C2 N1 C9 C8 0.4(3) . . . . ?
Co1 N1 C9 C8 177.54(18) . . . . ?
C7 C8 C9 N1 179.8(3) . . . . ?
C3 C8 C9 N1 -0.3(3) . . . . ?
C7 C8 C9 C10 -1.0(5) . . . . ?
C3 C8 C9 C10 178.9(3) . . . . ?
N1 C9 C10 C11 1.1(5) . . . . ?
C8 C9 C10 C11 -178.0(3) . . . . ?
C18 N2 C11 C10 -178.5(3) . . . . ?
Co1 N2 C11 C10 -4.0(4) . . . . ?
C18 N2 C11 C12 -0.2(3) . . . . ?
Co1 N2 C11 C12 174.31(18) . . . . ?
C9 C10 C11 N2 2.0(5) . . . . ?
C9 C10 C11 C12 -176.2(3) . . . . ?
N2 C11 C12 C17 0.4(3) . . . . ?
C10 C11 C12 C17 178.8(3) . . . . ?
N2 C11 C12 C13 -176.4(3) . . . . ?
C10 C11 C12 C13 2.0(5) . . . . ?
C17 C12 C13 C14 -0.4(4) . . . . ?
C11 C12 C13 C14 176.0(3) . . . . ?
C12 C13 C14 C15 1.8(4) . . . . ?
C13 C14 C15 C16 -1.4(5) . . . . ?
C14 C15 C16 C17 -0.6(5) . . . . ?
C13 C12 C17 C16 -1.5(5) . . . . ?
C11 C12 C17 C16 -178.8(3) . . . . ?
C13 C12 C17 C18 176.8(3) . . . . ?
C11 C12 C17 C18 -0.5(3) . . . . ?
C15 C16 C17 C12 2.0(4) . . . . ?
C15 C16 C17 C18 -175.8(3) . . . . ?
C11 N2 C18 C1 178.1(3) . . . 5_756 ?
Co1 N2 C18 C1 3.6(4) . . . 5_756 ?
C11 N2 C18 C17 -0.2(3) . . . . ?
Co1 N2 C18 C17 -174.63(18) . . . . ?
C12 C17 C18 C1 -177.8(3) . . . 5_756 ?
C16 C17 C18 C1 0.2(5) . . . 5_756 ?
C12 C17 C18 N2 0.4(3) . . . . ?
C16 C17 C18 N2 178.5(3) . . . . ?
C19 P1 C19 C20 -126.3(3) 8_646 . . . ?
C19 P1 C19 C20 -8.9(2) 7_666 . . . ?
C19 P1 C19 C20 112.4(3) 2_645 . . . ?
C19 P1 C19 C24 60.01(19) 8_646 . . . ?
C19 P1 C19 C24 177.4(3) 7_666 . . . ?
C19 P1 C19 C24 -61.3(2) 2_645 . . . ?
C24 C19 C20 C21 -2.5(5) . . . . ?
P1 C19 C20 C21 -176.0(3) . . . . ?
C19 C20 C21 C22 1.3(5) . . . . ?
C20 C21 C22 C23 0.3(6) . . . . ?
C21 C22 C23 C24 -0.7(5) . . . . ?
C22 C23 C24 C19 -0.5(5) . . . . ?
C20 C19 C24 C23 2.1(5) . . . . ?
P1 C19 C24 C23 175.8(2) . . . . ?

_refine_diff_density_max         0.399
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCoTBPBr22LT
_database_code_depnum_ccdc_archive 'CCDC 1947256'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Br2 Co N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Br4 Co2 N8 P'
_chemical_formula_weight         1793.99

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'
Co Co -2.3653 3.6143 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.4211(4)
_cell_length_b                   21.4211(4)
_cell_length_c                   7.61460(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3494.06(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    111(2)
_cell_measurement_reflns_used    21358
_cell_measurement_theta_min      4.13
_cell_measurement_theta_max      68.21

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_F_000             1802
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.094
_shelx_estimated_absorpt_T_min   0.126
_shelx_estimated_absorpt_T_max   0.815
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5261
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      111(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37529
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.128
_diffrn_reflns_theta_max         68.229
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3184
_reflns_number_gt                2679
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2019 (Burla, 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3184
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1770
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_restrained_S_all      1.339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 1.000000 0.000000 0.0379(3) Uani 1 2 d S . P . .
Br1 Br 0.55472(2) 0.90799(2) 0.10148(6) 0.0446(2) Uani 1 1 d . . . . .
N1 N 0.57122(15) 1.01158(15) -0.1691(5) 0.0387(8) Uani 1 1 d . . . . .
N2 N 0.45580(15) 0.94491(15) -0.1742(4) 0.0361(7) Uani 1 1 d . . . . .
C1 C 0.62522(19) 1.0440(2) -0.1381(5) 0.0394(10) Uani 1 1 d . . . . .
C2 C 0.66833(18) 1.03513(18) -0.2844(6) 0.0401(9) Uani 1 1 d . . . . .
C3 C 0.72921(19) 1.0556(2) -0.3115(6) 0.0459(10) Uani 1 1 d . . . . .
H1 H 0.749650 1.081853 -0.229145 0.055 Uiso 1 1 calc R U . . .
C4 C 0.7590(2) 1.0359(2) -0.4644(6) 0.0458(10) Uani 1 1 d . . . . .
H2 H 0.800902 1.048284 -0.485321 0.055 Uiso 1 1 calc R U . . .
C5 C 0.7286(2) 0.9983(2) -0.5880(5) 0.0453(11) Uani 1 1 d . . . . .
H3 H 0.749965 0.986143 -0.691828 0.054 Uiso 1 1 calc R U . . .
C6 C 0.6673(2) 0.9784(2) -0.5608(6) 0.0451(10) Uani 1 1 d . . . . .
H4 H 0.646091 0.953388 -0.644829 0.054 Uiso 1 1 calc R U . . .
C7 C 0.6383(2) 0.9969(2) -0.4045(5) 0.0408(10) Uani 1 1 d . . . . .
C8 C 0.57769(19) 0.98240(19) -0.3283(5) 0.0388(9) Uani 1 1 d . . . . .
C9 C 0.5350(2) 0.9430(2) -0.4043(6) 0.0424(10) Uani 1 1 d . . . . .
H5 H 0.545147 0.926665 -0.516693 0.051 Uiso 1 1 calc R U . . .
C10 C 0.47941(19) 0.92527(18) -0.3336(5) 0.0386(9) Uani 1 1 d . . . . .
C11 C 0.4357(2) 0.8832(2) -0.4178(5) 0.0423(10) Uani 1 1 d . . . . .
C12 C 0.4371(2) 0.8513(2) -0.5765(6) 0.0465(11) Uani 1 1 d . . . . .
H6 H 0.472061 0.854172 -0.652689 0.056 Uiso 1 1 calc R U . . .
C13 C 0.3859(2) 0.8151(2) -0.6200(6) 0.0516(12) Uani 1 1 d . . . . .
H7 H 0.385463 0.793782 -0.729431 0.062 Uiso 1 1 calc R U . . .
C14 C 0.3330(2) 0.8088(2) -0.5025(6) 0.0529(13) Uani 1 1 d . . . . .
H8 H 0.298266 0.783402 -0.533249 0.063 Uiso 1 1 calc R U . . .
C15 C 0.3343(2) 0.8401(2) -0.3477(6) 0.0485(11) Uani 1 1 d . . . . .
H9 H 0.300193 0.836309 -0.268502 0.058 Uiso 1 1 calc R U . . .
C16 C 0.3847(2) 0.87769(19) -0.3033(6) 0.0433(10) Uani 1 1 d . . . . .
C17 C 0.39966(19) 0.9164(2) -0.1524(5) 0.0405(10) Uani 1 1 d . . . . .
C18 C 0.3612(2) 0.9223(2) -0.0071(5) 0.0434(10) Uani 1 1 d . . . . .
H10 H 0.322362 0.900951 -0.009587 0.052 Uiso 1 1 calc R U . . .
P1 P 0.750000 0.750000 -0.750000 0.0375(5) Uani 1 4 d S T P . .
C19 C 0.6856(2) 0.7658(2) -0.6080(5) 0.0392(10) Uani 1 1 d . . . . .
C20 C 0.6919(2) 0.8133(2) -0.4820(6) 0.0503(12) Uani 1 1 d . . . . .
H11 H 0.728639 0.838077 -0.479052 0.060 Uiso 1 1 calc R U . . .
C21 C 0.6448(2) 0.8239(2) -0.3630(6) 0.0524(12) Uani 1 1 d . . . . .
H12 H 0.648194 0.857264 -0.281518 0.063 Uiso 1 1 calc R U . . .
C22 C 0.5925(2) 0.7861(2) -0.3615(6) 0.0551(12) Uani 1 1 d . . . . .
H13 H 0.560728 0.793100 -0.276722 0.066 Uiso 1 1 calc R U . . .
C23 C 0.5859(2) 0.7390(3) -0.4794(6) 0.0573(13) Uani 1 1 d . . . . .
H14 H 0.549554 0.713628 -0.477690 0.069 Uiso 1 1 calc R U . . .
C24 C 0.6336(2) 0.7278(2) -0.6054(6) 0.0498(12) Uani 1 1 d . . . . .
H15 H 0.629674 0.694475 -0.686970 0.060 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N1 2.012(3) 5_675 ?
Co1 N1 2.012(3) . ?
Co1 N2 2.012(3) . ?
Co1 N2 2.012(3) 5_675 ?
Co1 Br1 2.4198(5) . ?
Co1 Br1 2.4199(5) 5_675 ?
N1 C1 1.370(5) . ?
N1 C8 1.371(5) . ?
N2 C17 1.359(5) . ?
N2 C10 1.381(5) . ?
C1 C18 1.352(5) 5_675 ?
C1 C2 1.460(5) . ?
C2 C7 1.385(6) . ?
C2 C3 1.391(5) . ?
C3 C4 1.393(6) . ?
C4 C5 1.399(6) . ?
C5 C6 1.397(6) . ?
C6 C7 1.400(6) . ?
C7 C8 1.455(5) . ?
C8 C9 1.372(6) . ?
C9 C10 1.361(6) . ?
C10 C11 1.448(6) . ?
C11 C12 1.389(6) . ?
C11 C16 1.403(6) . ?
C12 C13 1.382(6) . ?
C13 C14 1.451(7) . ?
C14 C15 1.357(6) . ?
C15 C16 1.389(6) . ?
C16 C17 1.453(6) . ?
C17 C18 1.385(5) . ?
P1 C19 1.785(4) 8_754 ?
P1 C19 1.785(4) 2_665 ?
P1 C19 1.785(4) 7_574 ?
P1 C19 1.785(4) . ?
C19 C24 1.380(6) . ?
C19 C20 1.404(6) . ?
C20 C21 1.375(6) . ?
C21 C22 1.382(7) . ?
C22 C23 1.357(7) . ?
C23 C24 1.422(6) . ?

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 Co1 N1 180.0 5_675 . ?
N1 Co1 N2 89.59(14) 5_675 . ?
N1 Co1 N2 90.42(14) . . ?
N1 Co1 N2 90.41(14) 5_675 5_675 ?
N1 Co1 N2 89.58(14) . 5_675 ?
N2 Co1 N2 180.0 . 5_675 ?
N1 Co1 Br1 93.58(9) 5_675 . ?
N1 Co1 Br1 86.42(9) . . ?
N2 Co1 Br1 87.75(9) . . ?
N2 Co1 Br1 92.25(9) 5_675 . ?
N1 Co1 Br1 86.42(9) 5_675 5_675 ?
N1 Co1 Br1 93.58(9) . 5_675 ?
N2 Co1 Br1 92.25(9) . 5_675 ?
N2 Co1 Br1 87.75(9) 5_675 5_675 ?
Br1 Co1 Br1 180.0 . 5_675 ?
C1 N1 C8 107.4(3) . . ?
C1 N1 Co1 126.3(3) . . ?
C8 N1 Co1 125.9(3) . . ?
C17 N2 C10 107.1(3) . . ?
C17 N2 Co1 126.9(3) . . ?
C10 N2 Co1 125.9(3) . . ?
C18 C1 N1 126.4(4) 5_675 . ?
C18 C1 C2 123.9(4) 5_675 . ?
N1 C1 C2 109.6(4) . . ?
C7 C2 C3 121.6(4) . . ?
C7 C2 C1 106.7(4) . . ?
C3 C2 C1 131.7(4) . . ?
C2 C3 C4 117.3(4) . . ?
C3 C4 C5 121.6(4) . . ?
C6 C5 C4 120.9(4) . . ?
C5 C6 C7 117.2(4) . . ?
C2 C7 C6 121.5(4) . . ?
C2 C7 C8 106.1(3) . . ?
C6 C7 C8 132.3(4) . . ?
N1 C8 C9 125.8(4) . . ?
N1 C8 C7 110.2(3) . . ?
C9 C8 C7 123.9(4) . . ?
C10 C9 C8 126.0(4) . . ?
C9 C10 N2 125.7(4) . . ?
C9 C10 C11 124.3(4) . . ?
N2 C10 C11 110.0(3) . . ?
C12 C11 C16 121.0(4) . . ?
C12 C11 C10 132.7(4) . . ?
C16 C11 C10 106.3(3) . . ?
C13 C12 C11 117.9(4) . . ?
C12 C13 C14 121.6(4) . . ?
C15 C14 C13 118.3(4) . . ?
C14 C15 C16 120.9(4) . . ?
C15 C16 C11 120.3(4) . . ?
C15 C16 C17 134.0(4) . . ?
C11 C16 C17 105.7(4) . . ?
N2 C17 C18 125.6(4) . . ?
N2 C17 C16 110.8(4) . . ?
C18 C17 C16 123.6(4) . . ?
C1 C18 C17 125.1(4) 5_675 . ?
C19 P1 C19 111.51(13) 8_754 2_665 ?
C19 P1 C19 105.5(3) 8_754 7_574 ?
C19 P1 C19 111.51(13) 2_665 7_574 ?
C19 P1 C19 111.51(13) 8_754 . ?
C19 P1 C19 105.5(3) 2_665 . ?
C19 P1 C19 111.51(13) 7_574 . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 P1 121.4(3) . . ?
C20 C19 P1 118.5(3) . . ?
C21 C20 C19 119.9(5) . . ?
C20 C21 C22 120.2(5) . . ?
C23 C22 C21 120.9(5) . . ?
C22 C23 C24 119.8(5) . . ?
C19 C24 C23 119.3(4) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 C18 -177.9(4) . . . 5_675 ?
Co1 N1 C1 C18 -4.9(6) . . . 5_675 ?
C8 N1 C1 C2 -0.1(5) . . . . ?
Co1 N1 C1 C2 173.0(3) . . . . ?
C18 C1 C2 C7 178.5(4) 5_675 . . . ?
N1 C1 C2 C7 0.6(5) . . . . ?
C18 C1 C2 C3 1.3(8) 5_675 . . . ?
N1 C1 C2 C3 -176.7(4) . . . . ?
C7 C2 C3 C4 -0.2(6) . . . . ?
C1 C2 C3 C4 176.7(4) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 C6 -0.9(7) . . . . ?
C4 C5 C6 C7 -0.9(7) . . . . ?
C3 C2 C7 C6 -1.6(7) . . . . ?
C1 C2 C7 C6 -179.2(4) . . . . ?
C3 C2 C7 C8 176.8(4) . . . . ?
C1 C2 C7 C8 -0.8(5) . . . . ?
C5 C6 C7 C2 2.1(7) . . . . ?
C5 C6 C7 C8 -175.8(4) . . . . ?
C1 N1 C8 C9 177.1(4) . . . . ?
Co1 N1 C8 C9 4.0(6) . . . . ?
C1 N1 C8 C7 -0.5(4) . . . . ?
Co1 N1 C8 C7 -173.6(3) . . . . ?
C2 C7 C8 N1 0.8(5) . . . . ?
C6 C7 C8 N1 179.0(5) . . . . ?
C2 C7 C8 C9 -176.8(4) . . . . ?
C6 C7 C8 C9 1.3(8) . . . . ?
N1 C8 C9 C10 -1.3(8) . . . . ?
C7 C8 C9 C10 176.0(4) . . . . ?
C8 C9 C10 N2 1.4(7) . . . . ?
C8 C9 C10 C11 -179.6(4) . . . . ?
C17 N2 C10 C9 -179.9(4) . . . . ?
Co1 N2 C10 C9 -4.3(6) . . . . ?
C17 N2 C10 C11 1.0(5) . . . . ?
Co1 N2 C10 C11 176.6(3) . . . . ?
C9 C10 C11 C12 0.9(8) . . . . ?
N2 C10 C11 C12 180.0(5) . . . . ?
C9 C10 C11 C16 -179.4(4) . . . . ?
N2 C10 C11 C16 -0.3(5) . . . . ?
C16 C11 C12 C13 1.6(7) . . . . ?
C10 C11 C12 C13 -178.7(4) . . . . ?
C11 C12 C13 C14 -1.8(7) . . . . ?
C12 C13 C14 C15 0.7(7) . . . . ?
C13 C14 C15 C16 0.6(7) . . . . ?
C14 C15 C16 C11 -0.8(7) . . . . ?
C14 C15 C16 C17 179.7(5) . . . . ?
C12 C11 C16 C15 -0.4(7) . . . . ?
C10 C11 C16 C15 179.9(4) . . . . ?
C12 C11 C16 C17 179.3(4) . . . . ?
C10 C11 C16 C17 -0.5(5) . . . . ?
C10 N2 C17 C18 178.3(4) . . . . ?
Co1 N2 C17 C18 2.8(6) . . . . ?
C10 N2 C17 C16 -1.3(5) . . . . ?
Co1 N2 C17 C16 -176.8(3) . . . . ?
C15 C16 C17 N2 -179.3(5) . . . . ?
C11 C16 C17 N2 1.1(5) . . . . ?
C15 C16 C17 C18 1.1(8) . . . . ?
C11 C16 C17 C18 -178.5(4) . . . . ?
N2 C17 C18 C1 -2.1(7) . . . 5_675 ?
C16 C17 C18 C1 177.4(4) . . . 5_675 ?
C19 P1 C19 C24 4.9(4) 8_754 . . . ?
C19 P1 C19 C24 -116.2(4) 2_665 . . . ?
C19 P1 C19 C24 122.6(5) 7_574 . . . ?
C19 P1 C19 C20 176.9(4) 8_754 . . . ?
C19 P1 C19 C20 55.7(3) 2_665 . . . ?
C19 P1 C19 C20 -65.5(3) 7_574 . . . ?
C24 C19 C20 C21 -3.6(7) . . . . ?
P1 C19 C20 C21 -175.6(4) . . . . ?
C19 C20 C21 C22 3.0(7) . . . . ?
C20 C21 C22 C23 -1.6(7) . . . . ?
C21 C22 C23 C24 0.6(8) . . . . ?
C20 C19 C24 C23 2.6(7) . . . . ?
P1 C19 C24 C23 174.4(4) . . . . ?
C22 C23 C24 C19 -1.2(7) . . . . ?

_refine_diff_density_max         0.921
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.090

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPFetbpCl22LT
_database_code_depnum_ccdc_archive 'CCDC 1947252'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Cl2 Fe N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Cl4 Fe2 N8 P'
_chemical_formula_weight         1609.99

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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.6659(4)
_cell_length_b                   21.6659(4)
_cell_length_c                   7.55230(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3545.13(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    21830
_cell_measurement_theta_min      4.08
_cell_measurement_theta_max      68.105

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.353
_shelx_estimated_absorpt_T_min   0.414
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7344
_exptl_absorpt_correction_T_max  0.8913
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38200
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.081
_diffrn_reflns_theta_max         68.205
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3204
_reflns_number_gt                2521
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3204
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1984
_refine_ls_wR_factor_gt          0.1854
_refine_ls_goodness_of_fit_ref   1.433
_refine_ls_restrained_S_all      1.433
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 0.000000 0.500000 0.0384(3) Uani 1 2 d S . P . .
N1 N 0.44312(14) -0.04479(14) 0.6798(4) 0.0333(7) Uani 1 1 d . . . . .
N2 N 0.48901(14) -0.07298(14) 0.3240(4) 0.0340(7) Uani 1 1 d . . . . .
Cl1 Cl 0.59069(5) -0.05343(5) 0.60899(14) 0.0432(3) Uani 1 1 d . . . . .
C1 C 0.42424(17) -0.02124(17) 0.8399(5) 0.0323(8) Uani 1 1 d . . . . .
C2 C 0.38202(17) -0.06471(17) 0.9241(5) 0.0328(8) Uani 1 1 d . . . . .
C3 C 0.35080(17) -0.06341(19) 1.0840(6) 0.0383(9) Uani 1 1 d . . . . .
H1 H 0.354333 -0.029255 1.162205 0.046 Uiso 1 1 calc R U . . .
C4 C 0.31416(19) -0.11386(19) 1.1256(6) 0.0430(10) Uani 1 1 d . . . . .
H2 H 0.292279 -0.114125 1.234646 0.052 Uiso 1 1 calc R U . . .
C5 C 0.3086(2) -0.16419(19) 1.0118(5) 0.0421(10) Uani 1 1 d . . . . .
H3 H 0.283513 -0.198221 1.045056 0.050 Uiso 1 1 calc R U . . .
C6 C 0.33925(18) -0.16527(17) 0.8504(5) 0.0380(9) Uani 1 1 d . . . . .
H4 H 0.334806 -0.199131 0.771489 0.046 Uiso 1 1 calc R U . . .
C7 C 0.37690(17) -0.11491(17) 0.8074(5) 0.0323(8) Uani 1 1 d . . . . .
C8 C 0.41538(16) -0.10084(16) 0.6550(5) 0.0326(8) Uani 1 1 d . . . . .
C9 C 0.42230(18) -0.13819(18) 0.5074(5) 0.0366(9) Uani 1 1 d . . . . .
H5 H 0.401045 -0.176530 0.509839 0.044 Uiso 1 1 calc R U . . .
C10 C 0.45670(17) -0.12603(17) 0.3565(5) 0.0330(8) Uani 1 1 d . . . . .
C11 C 0.46583(17) -0.16858(17) 0.2106(5) 0.0334(8) Uani 1 1 d . . . . .
C12 C 0.44618(18) -0.22941(17) 0.1816(5) 0.0373(9) Uani 1 1 d . . . . .
H6 H 0.419934 -0.249906 0.263478 0.045 Uiso 1 1 calc R U . . .
C13 C 0.46664(19) -0.25863(18) 0.0282(5) 0.0388(9) Uani 1 1 d . . . . .
H7 H 0.454667 -0.300111 0.006335 0.047 Uiso 1 1 calc R U . . .
C14 C 0.50388(18) -0.22878(18) -0.0927(5) 0.0399(9) Uani 1 1 d . . . . .
H8 H 0.516476 -0.250023 -0.196662 0.048 Uiso 1 1 calc R U . . .
C15 C 0.52338(18) -0.16845(17) -0.0662(6) 0.0360(9) Uani 1 1 d . . . . .
H9 H 0.548617 -0.148077 -0.150841 0.043 Uiso 1 1 calc R U . . .
C16 C 0.50469(17) -0.13861(17) 0.0890(5) 0.0346(8) Uani 1 1 d . . . . .
C17 C 0.51899(17) -0.07876(17) 0.1639(5) 0.0330(8) Uani 1 1 d . . . . .
C18 C 0.55804(17) -0.03538(17) 0.0897(5) 0.0341(9) Uani 1 1 d . . . . .
H10 H 0.574777 -0.045484 -0.022892 0.041 Uiso 1 1 calc R U . . .
P1 P 0.750000 -0.250000 0.750000 0.0329(5) Uani 1 4 d S T P . .
C19 C 0.68498(17) -0.26029(17) 0.6067(5) 0.0347(9) Uani 1 1 d . . . . .
C20 C 0.6857(2) -0.31033(19) 0.4890(5) 0.0413(10) Uani 1 1 d . . . . .
H11 H 0.718873 -0.339029 0.492676 0.050 Uiso 1 1 calc R U . . .
C21 C 0.6389(2) -0.3182(2) 0.3682(6) 0.0476(11) Uani 1 1 d . . . . .
H12 H 0.639299 -0.352256 0.289103 0.057 Uiso 1 1 calc R U . . .
C22 C 0.5912(2) -0.2756(2) 0.3633(6) 0.0540(12) Uani 1 1 d . . . . .
H13 H 0.558360 -0.281228 0.281516 0.065 Uiso 1 1 calc R U . . .
C23 C 0.5904(2) -0.2252(2) 0.4750(6) 0.0533(12) Uani 1 1 d . . . . .
H14 H 0.557548 -0.196321 0.469175 0.064 Uiso 1 1 calc R U . . .
C24 C 0.63824(19) -0.2170(2) 0.5967(6) 0.0453(10) Uani 1 1 d . . . . .
H15 H 0.638654 -0.181872 0.672034 0.054 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 2.075(3) 5_656 ?
Fe1 N1 2.075(3) . ?
Fe1 N2 2.079(3) . ?
Fe1 N2 2.079(3) 5_656 ?
Fe1 Cl1 2.4245(10) 5_656 ?
Fe1 Cl1 2.4246(10) . ?
N1 C8 1.368(4) . ?
N1 C1 1.375(5) . ?
N2 C10 1.368(5) . ?
N2 C17 1.378(5) . ?
C1 C18 1.391(5) 5_656 ?
C1 C2 1.459(5) . ?
C2 C3 1.384(5) . ?
C2 C7 1.404(5) . ?
C3 C4 1.387(5) . ?
C4 C5 1.394(6) . ?
C5 C6 1.388(5) . ?
C6 C7 1.401(5) . ?
C7 C8 1.454(5) . ?
C8 C9 1.385(5) . ?
C9 C10 1.387(5) . ?
C10 C11 1.450(5) . ?
C11 C12 1.402(5) . ?
C11 C16 1.405(5) . ?
C12 C13 1.393(5) . ?
C13 C14 1.380(5) . ?
C14 C15 1.388(5) . ?
C15 C16 1.399(5) . ?
C16 C17 1.448(5) . ?
C17 C18 1.383(5) . ?
P1 C19 1.790(4) . ?
P1 C19 1.790(4) 7_667 ?
P1 C19 1.790(4) 8_647 ?
P1 C19 1.790(4) 2_645 ?
C19 C24 1.382(5) . ?
C19 C20 1.402(5) . ?
C20 C21 1.375(6) . ?
C21 C22 1.386(7) . ?
C22 C23 1.379(7) . ?
C23 C24 1.396(6) . ?

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 5_656 . ?
N1 Fe1 N2 90.30(12) 5_656 . ?
N1 Fe1 N2 89.70(12) . . ?
N1 Fe1 N2 89.70(12) 5_656 5_656 ?
N1 Fe1 N2 90.30(12) . 5_656 ?
N2 Fe1 N2 180.0 . 5_656 ?
N1 Fe1 Cl1 92.06(9) 5_656 5_656 ?
N1 Fe1 Cl1 87.94(9) . 5_656 ?
N2 Fe1 Cl1 93.05(9) . 5_656 ?
N2 Fe1 Cl1 86.94(9) 5_656 5_656 ?
N1 Fe1 Cl1 87.94(9) 5_656 . ?
N1 Fe1 Cl1 92.06(9) . . ?
N2 Fe1 Cl1 86.95(9) . . ?
N2 Fe1 Cl1 93.06(9) 5_656 . ?
Cl1 Fe1 Cl1 180.0 5_656 . ?
C8 N1 C1 108.6(3) . . ?
C8 N1 Fe1 125.9(3) . . ?
C1 N1 Fe1 125.4(2) . . ?
C10 N2 C17 108.8(3) . . ?
C10 N2 Fe1 125.6(3) . . ?
C17 N2 Fe1 125.2(2) . . ?
N1 C1 C18 125.5(3) . 5_656 ?
N1 C1 C2 109.3(3) . . ?
C18 C1 C2 125.2(3) 5_656 . ?
C3 C2 C7 121.6(3) . . ?
C3 C2 C1 132.3(3) . . ?
C7 C2 C1 106.0(3) . . ?
C2 C3 C4 117.5(4) . . ?
C3 C4 C5 121.7(4) . . ?
C6 C5 C4 120.9(4) . . ?
C5 C6 C7 118.0(4) . . ?
C6 C7 C2 120.3(3) . . ?
C6 C7 C8 132.9(4) . . ?
C2 C7 C8 106.8(3) . . ?
N1 C8 C9 125.5(3) . . ?
N1 C8 C7 109.2(3) . . ?
C9 C8 C7 125.2(3) . . ?
C8 C9 C10 127.5(4) . . ?
N2 C10 C9 125.6(3) . . ?
N2 C10 C11 109.1(3) . . ?
C9 C10 C11 125.2(3) . . ?
C12 C11 C16 121.0(3) . . ?
C12 C11 C10 132.4(4) . . ?
C16 C11 C10 106.5(3) . . ?
C13 C12 C11 117.4(4) . . ?
C14 C13 C12 121.6(4) . . ?
C13 C14 C15 121.6(4) . . ?
C14 C15 C16 117.9(4) . . ?
C15 C16 C11 120.5(3) . . ?
C15 C16 C17 132.8(4) . . ?
C11 C16 C17 106.7(3) . . ?
N2 C17 C18 125.6(3) . . ?
N2 C17 C16 108.9(3) . . ?
C18 C17 C16 125.5(3) . . ?
C17 C18 C1 127.8(4) . 5_656 ?
C19 P1 C19 111.42(12) . 7_667 ?
C19 P1 C19 111.42(12) . 8_647 ?
C19 P1 C19 105.6(2) 7_667 8_647 ?
C19 P1 C19 105.6(2) . 2_645 ?
C19 P1 C19 111.42(12) 7_667 2_645 ?
C19 P1 C19 111.42(12) 8_647 2_645 ?
C24 C19 C20 119.9(4) . . ?
C24 C19 P1 121.7(3) . . ?
C20 C19 P1 118.0(3) . . ?
C21 C20 C19 120.5(4) . . ?
C20 C21 C22 119.1(4) . . ?
C23 C22 C21 121.3(4) . . ?
C22 C23 C24 119.7(4) . . ?
C19 C24 C23 119.5(4) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 C18 -179.1(4) . . . 5_656 ?
Fe1 N1 C1 C18 -2.5(5) . . . 5_656 ?
C8 N1 C1 C2 0.3(4) . . . . ?
Fe1 N1 C1 C2 176.9(2) . . . . ?
N1 C1 C2 C3 179.6(4) . . . . ?
C18 C1 C2 C3 -1.1(7) 5_656 . . . ?
N1 C1 C2 C7 0.2(4) . . . . ?
C18 C1 C2 C7 179.5(4) 5_656 . . . ?
C7 C2 C3 C4 0.2(6) . . . . ?
C1 C2 C3 C4 -179.1(4) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C3 C4 C5 C6 -0.8(7) . . . . ?
C4 C5 C6 C7 1.4(6) . . . . ?
C5 C6 C7 C2 -1.2(6) . . . . ?
C5 C6 C7 C8 179.3(4) . . . . ?
C3 C2 C7 C6 0.4(6) . . . . ?
C1 C2 C7 C6 179.9(3) . . . . ?
C3 C2 C7 C8 -180.0(4) . . . . ?
C1 C2 C7 C8 -0.5(4) . . . . ?
C1 N1 C8 C9 178.9(4) . . . . ?
Fe1 N1 C8 C9 2.3(5) . . . . ?
C1 N1 C8 C7 -0.6(4) . . . . ?
Fe1 N1 C8 C7 -177.2(2) . . . . ?
C6 C7 C8 N1 -179.8(4) . . . . ?
C2 C7 C8 N1 0.7(4) . . . . ?
C6 C7 C8 C9 0.7(7) . . . . ?
C2 C7 C8 C9 -178.8(4) . . . . ?
N1 C8 C9 C10 -1.7(6) . . . . ?
C7 C8 C9 C10 177.7(4) . . . . ?
C17 N2 C10 C9 177.9(4) . . . . ?
Fe1 N2 C10 C9 4.8(5) . . . . ?
C17 N2 C10 C11 -0.1(4) . . . . ?
Fe1 N2 C10 C11 -173.3(2) . . . . ?
C8 C9 C10 N2 -2.2(6) . . . . ?
C8 C9 C10 C11 175.5(4) . . . . ?
N2 C10 C11 C12 176.3(4) . . . . ?
C9 C10 C11 C12 -1.8(7) . . . . ?
N2 C10 C11 C16 -0.3(4) . . . . ?
C9 C10 C11 C16 -178.4(4) . . . . ?
C16 C11 C12 C13 -0.1(6) . . . . ?
C10 C11 C12 C13 -176.2(4) . . . . ?
C11 C12 C13 C14 -1.2(6) . . . . ?
C12 C13 C14 C15 0.8(6) . . . . ?
C13 C14 C15 C16 0.7(6) . . . . ?
C14 C15 C16 C11 -2.0(6) . . . . ?
C14 C15 C16 C17 175.6(4) . . . . ?
C12 C11 C16 C15 1.6(6) . . . . ?
C10 C11 C16 C15 178.7(3) . . . . ?
C12 C11 C16 C17 -176.5(4) . . . . ?
C10 C11 C16 C17 0.6(4) . . . . ?
C10 N2 C17 C18 -177.5(4) . . . . ?
Fe1 N2 C17 C18 -4.3(5) . . . . ?
C10 N2 C17 C16 0.5(4) . . . . ?
Fe1 N2 C17 C16 173.7(2) . . . . ?
C15 C16 C17 N2 -178.4(4) . . . . ?
C11 C16 C17 N2 -0.7(4) . . . . ?
C15 C16 C17 C18 -0.5(7) . . . . ?
C11 C16 C17 C18 177.3(4) . . . . ?
N2 C17 C18 C1 1.2(7) . . . 5_656 ?
C16 C17 C18 C1 -176.4(4) . . . 5_656 ?
C19 P1 C19 C24 8.4(3) 7_667 . . . ?
C19 P1 C19 C24 126.1(4) 8_647 . . . ?
C19 P1 C19 C24 -112.8(4) 2_645 . . . ?
C19 P1 C19 C20 -178.7(3) 7_667 . . . ?
C19 P1 C19 C20 -61.0(2) 8_647 . . . ?
C19 P1 C19 C20 60.1(3) 2_645 . . . ?
C24 C19 C20 C21 -2.8(6) . . . . ?
P1 C19 C20 C21 -175.8(3) . . . . ?
C19 C20 C21 C22 0.5(6) . . . . ?
C20 C21 C22 C23 1.1(7) . . . . ?
C21 C22 C23 C24 -0.6(7) . . . . ?
C20 C19 C24 C23 3.3(6) . . . . ?
P1 C19 C24 C23 176.1(3) . . . . ?
C22 C23 C24 C19 -1.6(7) . . . . ?

_refine_diff_density_max         0.731
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.078

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPCoTBPBr22rt
_database_code_depnum_ccdc_archive 'CCDC 1947255'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H20 Br2 Co N4), C24 H20 P'
_chemical_formula_sum            'C96 H60 Br4 Co2 N8 P'
_chemical_formula_weight         1793.99

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'
Co Co -2.3653 3.6143 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5389(4)
_cell_length_b                   21.5389(4)
_cell_length_c                   7.66860(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3557.65(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    20328
_cell_measurement_theta_min      4.105
_cell_measurement_theta_max      68.16

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_F_000             1802
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    6.967
_shelx_estimated_absorpt_T_min   0.128
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8276
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37919
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.105
_diffrn_reflns_theta_max         68.209
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3219
_reflns_number_gt                2446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2019 (Burla, 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3219
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1642
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_restrained_S_all      1.227
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.000000 0.500000 0.500000 0.0488(3) Uani 1 2 d S . P . .
Br1 Br 0.05362(2) 0.40846(2) 0.39570(7) 0.0614(3) Uani 1 1 d . . . . .
N1 N 0.07101(16) 0.51090(16) 0.6686(5) 0.0507(9) Uani 1 1 d . . . . .
N2 N -0.04395(16) 0.44492(16) 0.6731(5) 0.0491(8) Uani 1 1 d . . . . .
C1 C 0.1245(2) 0.5433(2) 0.6385(6) 0.0524(11) Uani 1 1 d . . . . .
C2 C 0.16707(19) 0.53448(19) 0.7831(6) 0.0514(10) Uani 1 1 d . . . . .
C3 C 0.2277(2) 0.5549(2) 0.8110(6) 0.0614(12) Uani 1 1 d . . . . .
H1 H 0.247693 0.580468 0.731098 0.074 Uiso 1 1 calc R U . . .
C4 C 0.2568(2) 0.5355(2) 0.9626(6) 0.0644(13) Uani 1 1 d . . . . .
H2 H 0.297473 0.547912 0.983879 0.077 Uiso 1 1 calc R U . . .
C5 C 0.2267(2) 0.4980(3) 1.0838(6) 0.0622(13) Uani 1 1 d . . . . .
H3 H 0.247298 0.486190 1.185045 0.075 Uiso 1 1 calc R U . . .
C6 C 0.1671(2) 0.4782(2) 1.0557(7) 0.0629(13) Uani 1 1 d . . . . .
H4 H 0.146675 0.453593 1.137051 0.075 Uiso 1 1 calc R U . . .
C7 C 0.1380(2) 0.4963(2) 0.9009(6) 0.0511(11) Uani 1 1 d . . . . .
C8 C 0.0771(2) 0.4819(2) 0.8268(6) 0.0513(10) Uani 1 1 d . . . . .
C9 C 0.0351(2) 0.4429(2) 0.8999(6) 0.0564(12) Uani 1 1 d . . . . .
H5 H 0.045191 0.426392 1.008322 0.068 Uiso 1 1 calc R U . . .
C10 C -0.0206(2) 0.4254(2) 0.8301(6) 0.0493(10) Uani 1 1 d . . . . .
C11 C -0.0641(2) 0.3838(2) 0.9139(6) 0.0536(11) Uani 1 1 d . . . . .
C12 C -0.0633(2) 0.3514(2) 1.0715(6) 0.0605(12) Uani 1 1 d . . . . .
H6 H -0.029461 0.354090 1.146415 0.073 Uiso 1 1 calc R U . . .
C13 C -0.1131(3) 0.3160(2) 1.1126(6) 0.0668(14) Uani 1 1 d . . . . .
H7 H -0.113365 0.294993 1.218551 0.080 Uiso 1 1 calc R U . . .
C14 C -0.1660(3) 0.3096(2) 0.9975(6) 0.0709(15) Uani 1 1 d . . . . .
H8 H -0.199755 0.284957 1.027710 0.085 Uiso 1 1 calc R U . . .
C15 C -0.1644(2) 0.3406(2) 0.8448(7) 0.0635(13) Uani 1 1 d . . . . .
H9 H -0.197620 0.336974 0.768097 0.076 Uiso 1 1 calc R U . . .
C16 C -0.1144(2) 0.3779(2) 0.7995(6) 0.0547(11) Uani 1 1 d . . . . .
C17 C -0.0997(2) 0.4166(2) 0.6489(6) 0.0538(11) Uani 1 1 d . . . . .
C18 C -0.1379(2) 0.4231(2) 0.5079(6) 0.0580(12) Uani 1 1 d . . . . .
H10 H -0.176031 0.402952 0.511739 0.070 Uiso 1 1 calc R U . . .
P1 P 0.250000 0.250000 1.250000 0.0542(6) Uani 1 4 d S T P . .
C19 C 0.1857(2) 0.2651(2) 1.1092(6) 0.0558(11) Uani 1 1 d . . . . .
C24 C 0.1908(3) 0.3119(3) 0.9830(7) 0.0722(15) Uani 1 1 d . . . . .
H15 H 0.226022 0.336853 0.980428 0.087 Uiso 1 1 calc R U . . .
C23 C 0.1446(3) 0.3215(3) 0.8639(7) 0.0799(16) Uani 1 1 d . . . . .
H14 H 0.148107 0.353136 0.781893 0.096 Uiso 1 1 calc R U . . .
C22 C 0.0933(3) 0.2843(3) 0.8663(8) 0.0862(17) Uani 1 1 d . . . . .
H13 H 0.061767 0.291295 0.785930 0.103 Uiso 1 1 calc R U . . .
C21 C 0.0874(3) 0.2379(3) 0.9819(8) 0.0866(19) Uani 1 1 d . . . . .
H12 H 0.052142 0.212916 0.979550 0.104 Uiso 1 1 calc R U . . .
C20 C 0.1342(3) 0.2267(3) 1.1069(7) 0.0761(16) Uani 1 1 d . . . . .
H11 H 0.130440 0.194257 1.186133 0.091 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Co1 N2 2.016(3) 5_566 ?
Co1 N2 2.016(3) . ?
Co1 N1 2.016(3) . ?
Co1 N1 2.016(3) 5_566 ?
Co1 Br1 2.4210(5) . ?
Co1 Br1 2.4210(5) 5_566 ?
N1 C1 1.366(5) . ?
N1 C8 1.371(5) . ?
N2 C17 1.359(5) . ?
N2 C10 1.371(5) . ?
C1 C18 1.366(6) 5_566 ?
C1 C2 1.452(6) . ?
C2 C7 1.373(6) . ?
C2 C3 1.394(6) . ?
C3 C4 1.386(6) . ?
C4 C5 1.392(6) . ?
C5 C6 1.369(7) . ?
C6 C7 1.398(6) . ?
C7 C8 1.462(6) . ?
C8 C9 1.357(6) . ?
C9 C10 1.366(6) . ?
C10 C11 1.446(6) . ?
C11 C12 1.396(6) . ?
C11 C16 1.401(6) . ?
C12 C13 1.353(7) . ?
C13 C14 1.447(7) . ?
C14 C15 1.349(6) . ?
C15 C16 1.387(6) . ?
C16 C17 1.459(6) . ?
C17 C18 1.365(6) . ?
P1 C19 1.785(5) 7_568 ?
P1 C19 1.785(5) 8_658 ?
P1 C19 1.785(5) 2 ?
P1 C19 1.785(5) . ?
C19 C20 1.384(7) . ?
C19 C24 1.403(7) . ?
C24 C23 1.365(7) . ?
C23 C22 1.365(9) . ?
C22 C21 1.342(9) . ?
C21 C20 1.412(7) . ?

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
N2 Co1 N2 180.00(17) 5_566 . ?
N2 Co1 N1 89.86(15) 5_566 . ?
N2 Co1 N1 90.14(15) . . ?
N2 Co1 N1 90.14(15) 5_566 5_566 ?
N2 Co1 N1 89.85(15) . 5_566 ?
N1 Co1 N1 180.00(12) . 5_566 ?
N2 Co1 Br1 92.16(10) 5_566 . ?
N2 Co1 Br1 87.84(10) . . ?
N1 Co1 Br1 86.83(10) . . ?
N1 Co1 Br1 93.16(10) 5_566 . ?
N2 Co1 Br1 87.84(10) 5_566 5_566 ?
N2 Co1 Br1 92.16(10) . 5_566 ?
N1 Co1 Br1 93.17(10) . 5_566 ?
N1 Co1 Br1 86.83(10) 5_566 5_566 ?
Br1 Co1 Br1 180.0 . 5_566 ?
C1 N1 C8 107.5(4) . . ?
C1 N1 Co1 126.2(3) . . ?
C8 N1 Co1 126.0(3) . . ?
C17 N2 C10 107.9(4) . . ?
C17 N2 Co1 126.1(3) . . ?
C10 N2 Co1 125.9(3) . . ?
C18 C1 N1 126.0(4) 5_566 . ?
C18 C1 C2 124.3(4) 5_566 . ?
N1 C1 C2 109.7(4) . . ?
C7 C2 C3 121.0(4) . . ?
C7 C2 C1 107.0(4) . . ?
C3 C2 C1 131.9(4) . . ?
C4 C3 C2 117.3(4) . . ?
C3 C4 C5 121.6(5) . . ?
C6 C5 C4 120.8(4) . . ?
C5 C6 C7 117.9(5) . . ?
C2 C7 C6 121.4(4) . . ?
C2 C7 C8 106.3(4) . . ?
C6 C7 C8 132.4(4) . . ?
C9 C8 N1 125.7(4) . . ?
C9 C8 C7 124.7(4) . . ?
N1 C8 C7 109.5(4) . . ?
C8 C9 C10 126.5(4) . . ?
C9 C10 N2 125.6(4) . . ?
C9 C10 C11 124.4(4) . . ?
N2 C10 C11 110.0(4) . . ?
C12 C11 C16 120.4(4) . . ?
C12 C11 C10 133.4(4) . . ?
C16 C11 C10 106.2(4) . . ?
C13 C12 C11 118.3(5) . . ?
C12 C13 C14 122.4(4) . . ?
C15 C14 C13 117.5(5) . . ?
C14 C15 C16 121.6(5) . . ?
C15 C16 C11 119.8(4) . . ?
C15 C16 C17 134.3(4) . . ?
C11 C16 C17 106.0(4) . . ?
N2 C17 C18 126.5(4) . . ?
N2 C17 C16 109.9(4) . . ?
C18 C17 C16 123.6(4) . . ?
C17 C18 C1 125.3(5) . 5_566 ?
C19 P1 C19 105.6(3) 7_568 8_658 ?
C19 P1 C19 111.45(16) 7_568 2 ?
C19 P1 C19 111.45(15) 8_658 2 ?
C19 P1 C19 111.45(15) 7_568 . ?
C19 P1 C19 111.45(16) 8_658 . ?
C19 P1 C19 105.6(3) 2 . ?
C20 C19 C24 118.9(5) . . ?
C20 C19 P1 121.4(4) . . ?
C24 C19 P1 119.2(4) . . ?
C23 C24 C19 120.9(6) . . ?
C22 C23 C24 119.4(6) . . ?
C21 C22 C23 121.6(6) . . ?
C22 C21 C20 120.4(6) . . ?
C19 C20 C21 118.7(6) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N1 C1 C18 177.6(5) . . . 5_566 ?
Co1 N1 C1 C18 3.7(7) . . . 5_566 ?
C8 N1 C1 C2 0.4(5) . . . . ?
Co1 N1 C1 C2 -173.5(3) . . . . ?
C18 C1 C2 C7 -177.5(5) 5_566 . . . ?
N1 C1 C2 C7 -0.3(5) . . . . ?
C18 C1 C2 C3 -0.7(8) 5_566 . . . ?
N1 C1 C2 C3 176.6(5) . . . . ?
C7 C2 C3 C4 -0.6(7) . . . . ?
C1 C2 C3 C4 -177.1(5) . . . . ?
C2 C3 C4 C5 -1.0(8) . . . . ?
C3 C4 C5 C6 0.8(8) . . . . ?
C4 C5 C6 C7 0.8(8) . . . . ?
C3 C2 C7 C6 2.3(7) . . . . ?
C1 C2 C7 C6 179.6(4) . . . . ?
C3 C2 C7 C8 -177.3(4) . . . . ?
C1 C2 C7 C8 0.0(5) . . . . ?
C5 C6 C7 C2 -2.4(7) . . . . ?
C5 C6 C7 C8 177.1(5) . . . . ?
C1 N1 C8 C9 -176.9(5) . . . . ?
Co1 N1 C8 C9 -2.9(7) . . . . ?
C1 N1 C8 C7 -0.4(5) . . . . ?
Co1 N1 C8 C7 173.5(3) . . . . ?
C2 C7 C8 C9 176.8(5) . . . . ?
C6 C7 C8 C9 -2.7(9) . . . . ?
C2 C7 C8 N1 0.3(5) . . . . ?
C6 C7 C8 N1 -179.2(5) . . . . ?
N1 C8 C9 C10 0.0(9) . . . . ?
C7 C8 C9 C10 -175.9(5) . . . . ?
C8 C9 C10 N2 -0.5(8) . . . . ?
C8 C9 C10 C11 -179.6(5) . . . . ?
C17 N2 C10 C9 179.1(5) . . . . ?
Co1 N2 C10 C9 3.9(7) . . . . ?
C17 N2 C10 C11 -1.7(5) . . . . ?
Co1 N2 C10 C11 -176.9(3) . . . . ?
C9 C10 C11 C12 -1.0(9) . . . . ?
N2 C10 C11 C12 179.8(5) . . . . ?
C9 C10 C11 C16 -179.6(5) . . . . ?
N2 C10 C11 C16 1.1(5) . . . . ?
C16 C11 C12 C13 -2.1(8) . . . . ?
C10 C11 C12 C13 179.4(5) . . . . ?
C11 C12 C13 C14 1.4(8) . . . . ?
C12 C13 C14 C15 -0.1(8) . . . . ?
C13 C14 C15 C16 -0.6(8) . . . . ?
C14 C15 C16 C11 0.0(8) . . . . ?
C14 C15 C16 C17 -179.4(5) . . . . ?
C12 C11 C16 C15 1.4(7) . . . . ?
C10 C11 C16 C15 -179.7(4) . . . . ?
C12 C11 C16 C17 -179.1(4) . . . . ?
C10 C11 C16 C17 -0.2(5) . . . . ?
C10 N2 C17 C18 -179.3(5) . . . . ?
Co1 N2 C17 C18 -4.1(7) . . . . ?
C10 N2 C17 C16 1.5(5) . . . . ?
Co1 N2 C17 C16 176.8(3) . . . . ?
C15 C16 C17 N2 178.6(5) . . . . ?
C11 C16 C17 N2 -0.8(5) . . . . ?
C15 C16 C17 C18 -0.6(9) . . . . ?
C11 C16 C17 C18 180.0(4) . . . . ?
N2 C17 C18 C1 4.0(8) . . . 5_566 ?
C16 C17 C18 C1 -176.9(5) . . . 5_566 ?
C19 P1 C19 C20 -122.4(5) 7_568 . . . ?
C19 P1 C19 C20 -4.7(4) 8_658 . . . ?
C19 P1 C19 C20 116.4(5) 2 . . . ?
C19 P1 C19 C24 65.8(3) 7_568 . . . ?
C19 P1 C19 C24 -176.6(4) 8_658 . . . ?
C19 P1 C19 C24 -55.4(4) 2 . . . ?
C20 C19 C24 C23 2.6(8) . . . . ?
P1 C19 C24 C23 174.7(4) . . . . ?
C19 C24 C23 C22 -1.0(9) . . . . ?
C24 C23 C22 C21 -0.8(10) . . . . ?
C23 C22 C21 C20 0.8(10) . . . . ?
C24 C19 C20 C21 -2.5(8) . . . . ?
P1 C19 C20 C21 -174.4(4) . . . . ?
C22 C21 C20 C19 0.9(10) . . . . ?

_refine_diff_density_max         0.647
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.077

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPFePcCl22rt
_database_code_depnum_ccdc_archive 'CCDC 1947257'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H16 Cl2 Fe N8), C24 H20 P'
_chemical_formula_sum            'C88 H52 Cl4 Fe2 N16 P'
_chemical_formula_weight         1617.92

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'
Cl Cl 0.3639 0.7018 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5815(4)
_cell_length_b                   21.5815(4)
_cell_length_c                   7.53300(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3508.58(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    25577
_cell_measurement_theta_min      4.095
_cell_measurement_theta_max      68.170

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_F_000             1684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.668
_shelx_estimated_absorpt_T_min   0.601
_shelx_estimated_absorpt_T_max   0.601
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8597
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38163
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.097
_diffrn_reflns_theta_max         68.173
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3210
_reflns_number_gt                2846
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3210
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_restrained_S_all      1.261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.48195(10) 0.07366(10) 0.1735(3) 0.0337(5) Uani 1 1 d . . . . .
C2 C 0.49624(10) 0.13446(10) 0.0966(3) 0.0339(5) Uani 1 1 d . . . . .
C3 C 0.47685(11) 0.16309(11) -0.0593(3) 0.0406(5) Uani 1 1 d . . . . .
H1 H 0.451792 0.142773 -0.141134 0.049 Uiso 1 1 calc R U . . .
C4 C 0.49679(12) 0.22351(11) -0.0865(3) 0.0436(6) Uani 1 1 d . . . . .
H2 H 0.484208 0.244374 -0.188286 0.052 Uiso 1 1 calc R U . . .
C5 C 0.53500(12) 0.25367(11) 0.0341(3) 0.0442(6) Uani 1 1 d . . . . .
H3 H 0.547398 0.294179 0.011515 0.053 Uiso 1 1 calc R U . . .
C6 C 0.55505(11) 0.22418(11) 0.1882(3) 0.0402(5) Uani 1 1 d . . . . .
H4 H 0.580988 0.244062 0.268722 0.048 Uiso 1 1 calc R U . . .
C7 C 0.53482(10) 0.16407(10) 0.2170(3) 0.0352(5) Uani 1 1 d . . . . .
C8 C 0.54339(10) 0.12115(10) 0.3647(3) 0.0342(5) Uani 1 1 d . . . . .
C9 C 0.58135(10) 0.09846(10) 0.6448(3) 0.0347(5) Uani 1 1 d . . . . .
C10 C 0.62085(10) 0.11235(10) 0.7970(3) 0.0349(5) Uani 1 1 d . . . . .
C11 C 0.65857(11) 0.16201(10) 0.8374(3) 0.0386(5) Uani 1 1 d . . . . .
H5 H 0.662593 0.195389 0.760186 0.046 Uiso 1 1 calc R U . . .
C12 C 0.69038(13) 0.16027(12) 0.9980(3) 0.0458(7) Uani 1 1 d . . . . .
H6 H 0.715726 0.193298 1.029858 0.055 Uiso 1 1 calc R U . . .
C13 C 0.68475(12) 0.10978(12) 1.1116(3) 0.0462(6) Uani 1 1 d . . . . .
H7 H 0.706864 0.109748 1.217567 0.055 Uiso 1 1 calc R U . . .
C14 C 0.64758(11) 0.05996(11) 1.0724(3) 0.0401(5) Uani 1 1 d . . . . .
H8 H 0.644131 0.026374 1.149095 0.048 Uiso 1 1 calc R U . . .
C15 C 0.61534(10) 0.06206(10) 0.9127(3) 0.0341(5) Uani 1 1 d . . . . .
C16 C 0.57183(10) 0.01909(10) 0.8295(3) 0.0342(5) Uani 1 1 d . . . . .
C17 C 0.31538(11) 0.26107(12) 0.6058(3) 0.0446(6) Uani 1 1 d . . . . .
C18 C 0.31325(15) 0.31131(14) 0.4869(3) 0.0554(8) Uani 1 1 d . . . . .
H9 H 0.279858 0.338542 0.488399 0.066 Uiso 1 1 calc R U . . .
C19 C 0.36105(16) 0.31975(16) 0.3685(4) 0.0684(9) Uani 1 1 d . . . . .
H10 H 0.360066 0.352824 0.289385 0.082 Uiso 1 1 calc R U . . .
C20 C 0.41024(15) 0.27934(18) 0.3671(4) 0.0748(10) Uani 1 1 d . . . . .
H11 H 0.442992 0.285911 0.289081 0.090 Uiso 1 1 calc R U . . .
C21 C 0.41150(15) 0.2295(2) 0.4794(4) 0.0771(10) Uani 1 1 d . . . . .
H12 H 0.444608 0.201941 0.475149 0.093 Uiso 1 1 calc R U . . .
C22 C 0.36382(13) 0.21973(16) 0.5996(4) 0.0583(7) Uani 1 1 d . . . . .
H13 H 0.364586 0.185632 0.675028 0.070 Uiso 1 1 calc R U . . .
N1 N 0.55230(8) 0.04265(8) 0.6700(2) 0.0337(4) Uani 1 1 d . . . . .
N2 N 0.57733(9) 0.13599(9) 0.5061(2) 0.0370(5) Uani 1 1 d . . . . .
N3 N 0.51168(8) 0.06784(8) 0.3333(2) 0.0336(4) Uani 1 1 d . . . . .
N4 N 0.44347(9) 0.03437(8) 0.0961(2) 0.0361(4) Uani 1 1 d . . . . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0308(2) Uani 1 2 d S . P . .
Cl1 Cl 0.41299(3) 0.05077(3) 0.59653(8) 0.0454(2) Uani 1 1 d . . . . .
P1 P 0.250000 0.250000 0.750000 0.0398(3) Uani 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N4 1.322(3) . ?
C1 N3 1.370(3) . ?
C1 C2 1.467(3) . ?
C2 C7 1.387(3) . ?
C2 C3 1.391(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.388(3) . ?
C5 C6 1.393(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.460(3) . ?
C8 N2 1.332(3) . ?
C8 N3 1.359(3) . ?
C9 N2 1.325(3) . ?
C9 N1 1.371(3) . ?
C9 C10 1.460(3) . ?
C10 C11 1.380(3) . ?
C10 C15 1.397(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.391(3) . ?
C13 C14 1.374(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.461(3) . ?
C16 N4 1.324(3) 5_656 ?
C16 N1 1.371(3) . ?
C17 C22 1.375(4) . ?
C17 C18 1.407(4) . ?
C17 P1 1.797(2) . ?
C18 C19 1.376(4) . ?
C19 C20 1.374(5) . ?
C20 C21 1.369(5) . ?
C21 C22 1.386(4) . ?
N1 Fe1 1.9392(17) . ?
N3 Fe1 1.9455(17) . ?
Fe1 Cl1 2.2924(6) 5_656 ?
Fe1 Cl1 2.2924(6) . ?

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
N4 C1 N3 128.52(19) . . ?
N4 C1 C2 122.12(19) . . ?
N3 C1 C2 109.28(18) . . ?
C7 C2 C3 121.8(2) . . ?
C7 C2 C1 106.29(18) . . ?
C3 C2 C1 131.8(2) . . ?
C4 C3 C2 116.6(2) . . ?
C5 C4 C3 121.9(2) . . ?
C4 C5 C6 121.0(2) . . ?
C7 C6 C5 117.4(2) . . ?
C6 C7 C2 121.2(2) . . ?
C6 C7 C8 132.3(2) . . ?
C2 C7 C8 106.37(18) . . ?
N2 C8 N3 128.31(19) . . ?
N2 C8 C7 121.8(2) . . ?
N3 C8 C7 109.91(18) . . ?
N2 C9 N1 128.02(19) . . ?
N2 C9 C10 122.2(2) . . ?
N1 C9 C10 109.80(18) . . ?
C11 C10 C15 121.1(2) . . ?
C11 C10 C9 132.6(2) . . ?
C15 C10 C9 106.30(19) . . ?
C10 C11 C12 117.5(2) . . ?
C13 C12 C11 120.9(2) . . ?
C14 C13 C12 122.1(2) . . ?
C13 C14 C15 116.9(2) . . ?
C14 C15 C10 121.5(2) . . ?
C14 C15 C16 132.2(2) . . ?
C10 C15 C16 106.28(18) . . ?
N4 C16 N1 128.1(2) 5_656 . ?
N4 C16 C15 122.11(19) 5_656 . ?
N1 C16 C15 109.77(18) . . ?
C22 C17 C18 120.2(3) . . ?
C22 C17 P1 122.1(2) . . ?
C18 C17 P1 117.5(2) . . ?
C19 C18 C17 119.4(3) . . ?
C20 C19 C18 120.0(3) . . ?
C21 C20 C19 120.6(3) . . ?
C20 C21 C22 120.5(3) . . ?
C17 C22 C21 119.2(3) . . ?
C16 N1 C9 107.83(17) . . ?
C16 N1 Fe1 125.56(14) . . ?
C9 N1 Fe1 126.29(14) . . ?
C9 N2 C8 121.3(2) . . ?
C8 N3 C1 108.14(17) . . ?
C8 N3 Fe1 126.13(14) . . ?
C1 N3 Fe1 125.14(14) . . ?
C1 N4 C16 121.9(2) . 5_656 ?
N1 Fe1 N1 180.0 . 5_656 ?
N1 Fe1 N3 89.63(8) . . ?
N1 Fe1 N3 90.37(8) 5_656 . ?
N1 Fe1 N3 90.36(8) . 5_656 ?
N1 Fe1 N3 89.63(8) 5_656 5_656 ?
N3 Fe1 N3 180.0 . 5_656 ?
N1 Fe1 Cl1 87.68(6) . 5_656 ?
N1 Fe1 Cl1 92.32(5) 5_656 5_656 ?
N3 Fe1 Cl1 92.80(6) . 5_656 ?
N3 Fe1 Cl1 87.20(6) 5_656 5_656 ?
N1 Fe1 Cl1 92.32(6) . . ?
N1 Fe1 Cl1 87.68(6) 5_656 . ?
N3 Fe1 Cl1 87.20(6) . . ?
N3 Fe1 Cl1 92.80(6) 5_656 . ?
Cl1 Fe1 Cl1 180.0 5_656 . ?
C17 P1 C17 105.60(16) . 2 ?
C17 P1 C17 111.44(8) . 8_657 ?
C17 P1 C17 111.44(8) 2 8_657 ?
C17 P1 C17 111.44(8) . 7_567 ?
C17 P1 C17 111.44(8) 2 7_567 ?
C17 P1 C17 105.60(16) 8_657 7_567 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C1 C2 C7 176.7(2) . . . . ?
N3 C1 C2 C7 -0.4(2) . . . . ?
N4 C1 C2 C3 -1.3(4) . . . . ?
N3 C1 C2 C3 -178.4(2) . . . . ?
C7 C2 C3 C4 -1.6(3) . . . . ?
C1 C2 C3 C4 176.1(2) . . . . ?
C2 C3 C4 C5 1.0(4) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C4 C5 C6 C7 -0.7(4) . . . . ?
C5 C6 C7 C2 0.1(3) . . . . ?
C5 C6 C7 C8 -176.1(2) . . . . ?
C3 C2 C7 C6 1.0(3) . . . . ?
C1 C2 C7 C6 -177.2(2) . . . . ?
C3 C2 C7 C8 178.2(2) . . . . ?
C1 C2 C7 C8 -0.1(2) . . . . ?
C6 C7 C8 N2 -1.9(4) . . . . ?
C2 C7 C8 N2 -178.6(2) . . . . ?
C6 C7 C8 N3 177.2(2) . . . . ?
C2 C7 C8 N3 0.5(2) . . . . ?
N2 C9 C10 C11 1.9(4) . . . . ?
N1 C9 C10 C11 -179.2(2) . . . . ?
N2 C9 C10 C15 -177.7(2) . . . . ?
N1 C9 C10 C15 1.2(2) . . . . ?
C15 C10 C11 C12 -0.5(3) . . . . ?
C9 C10 C11 C12 179.9(2) . . . . ?
C10 C11 C12 C13 0.9(4) . . . . ?
C11 C12 C13 C14 -0.6(4) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C13 C14 C15 C10 0.4(3) . . . . ?
C13 C14 C15 C16 -179.0(2) . . . . ?
C11 C10 C15 C14 -0.1(3) . . . . ?
C9 C10 C15 C14 179.6(2) . . . . ?
C11 C10 C15 C16 179.5(2) . . . . ?
C9 C10 C15 C16 -0.9(2) . . . . ?
C14 C15 C16 N4 -1.2(4) . . . 5_656 ?
C10 C15 C16 N4 179.2(2) . . . 5_656 ?
C14 C15 C16 N1 179.8(2) . . . . ?
C10 C15 C16 N1 0.2(2) . . . . ?
C22 C17 C18 C19 -2.1(4) . . . . ?
P1 C17 C18 C19 -177.0(2) . . . . ?
C17 C18 C19 C20 0.0(5) . . . . ?
C18 C19 C20 C21 1.8(5) . . . . ?
C19 C20 C21 C22 -1.5(5) . . . . ?
C18 C17 C22 C21 2.4(4) . . . . ?
P1 C17 C22 C21 177.0(2) . . . . ?
C20 C21 C22 C17 -0.6(5) . . . . ?
N4 C16 N1 C9 -178.4(2) 5_656 . . . ?
C15 C16 N1 C9 0.5(2) . . . . ?
N4 C16 N1 Fe1 -4.5(3) 5_656 . . . ?
C15 C16 N1 Fe1 174.41(14) . . . . ?
N2 C9 N1 C16 177.8(2) . . . . ?
C10 C9 N1 C16 -1.1(2) . . . . ?
N2 C9 N1 Fe1 4.0(3) . . . . ?
C10 C9 N1 Fe1 -174.90(14) . . . . ?
N1 C9 N2 C8 -2.0(4) . . . . ?
C10 C9 N2 C8 176.7(2) . . . . ?
N3 C8 N2 C9 -3.7(3) . . . . ?
C7 C8 N2 C9 175.3(2) . . . . ?
N2 C8 N3 C1 178.3(2) . . . . ?
C7 C8 N3 C1 -0.8(2) . . . . ?
N2 C8 N3 Fe1 6.7(3) . . . . ?
C7 C8 N3 Fe1 -172.35(14) . . . . ?
N4 C1 N3 C8 -176.1(2) . . . . ?
C2 C1 N3 C8 0.7(2) . . . . ?
N4 C1 N3 Fe1 -4.4(3) . . . . ?
C2 C1 N3 Fe1 172.40(14) . . . . ?
N3 C1 N4 C16 0.1(4) . . . 5_656 ?
C2 C1 N4 C16 -176.4(2) . . . 5_656 ?
C22 C17 P1 C17 -115.2(3) . . . 2 ?
C18 C17 P1 C17 59.62(19) . . . 2 ?
C22 C17 P1 C17 123.7(3) . . . 8_657 ?
C18 C17 P1 C17 -61.54(17) . . . 8_657 ?
C22 C17 P1 C17 6.0(2) . . . 7_567 ?
C18 C17 P1 C17 -179.2(2) . . . 7_567 ?

_refine_diff_density_max         0.206
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.075

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TPPFePcBr22rt
_database_code_depnum_ccdc_archive 'CCDC 1947258'
loop_
_audit_author_name
_audit_author_address
'Masaki Matsuda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H16 Br2 Fe N8), C24 H20 P'
_chemical_formula_sum            'C88 H52 Br4 Fe2 N16 P'
_chemical_formula_weight         1795.76

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

_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.
;

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'

_cell_length_a                   21.5372(4)
_cell_length_b                   21.5372(4)
_cell_length_c                   7.62570(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3537.19(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    18014
_cell_measurement_theta_min      4.105
_cell_measurement_theta_max      68.21

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_F_000             1798
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.660
_shelx_estimated_absorpt_T_min   0.556
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7562
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 2010)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37512
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.105
_diffrn_reflns_theta_max         68.210
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3234
_reflns_number_gt                2816
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3234
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1472
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.48311(14) 0.07415(14) 0.1763(4) 0.0302(7) Uani 1 1 d . . . . .
C2 C 0.49687(15) 0.13532(15) 0.1032(4) 0.0310(7) Uani 1 1 d . . . . .
C3 C 0.47745(16) 0.16424(16) -0.0500(5) 0.0361(7) Uani 1 1 d . . . . .
H1 H 0.452293 0.143976 -0.130960 0.043 Uiso 1 1 calc R U . . .
C4 C 0.49733(19) 0.22475(17) -0.0767(5) 0.0422(9) Uani 1 1 d . . . . .
H2 H 0.485346 0.245604 -0.178006 0.051 Uiso 1 1 calc R U . . .
C5 C 0.53526(17) 0.25524(16) 0.0464(5) 0.0392(8) Uani 1 1 d . . . . .
H3 H 0.547381 0.296045 0.025970 0.047 Uiso 1 1 calc R U . . .
C6 C 0.55478(15) 0.22552(14) 0.1972(4) 0.0361(7) Uani 1 1 d . . . . .
H4 H 0.580471 0.245299 0.277740 0.043 Uiso 1 1 calc R U . . .
C7 C 0.53461(14) 0.16504(14) 0.2240(4) 0.0318(7) Uani 1 1 d . . . . .
C8 C 0.54363(15) 0.12200(15) 0.3691(4) 0.0304(7) Uani 1 1 d . . . . .
C9 C 0.58058(14) 0.09858(15) 0.6464(4) 0.0312(7) Uani 1 1 d . . . . .
C10 C 0.61943(14) 0.11248(14) 0.7983(4) 0.0312(7) Uani 1 1 d . . . . .
C11 C 0.65719(14) 0.16277(15) 0.8403(5) 0.0352(7) Uani 1 1 d . . . . .
H5 H 0.661214 0.196484 0.764930 0.042 Uiso 1 1 calc R U . . .
C12 C 0.68854(17) 0.16063(17) 0.9988(5) 0.0416(9) Uani 1 1 d . . . . .
H6 H 0.713592 0.193864 1.031283 0.050 Uiso 1 1 calc R U . . .
C13 C 0.68327(17) 0.10949(18) 1.1110(5) 0.0420(9) Uani 1 1 d . . . . .
H7 H 0.705288 0.109184 1.215904 0.050 Uiso 1 1 calc R U . . .
C14 C 0.64611(16) 0.05958(16) 1.0691(4) 0.0370(8) Uani 1 1 d . . . . .
H8 H 0.642856 0.025435 1.143138 0.044 Uiso 1 1 calc R U . . .
C15 C 0.61366(15) 0.06229(15) 0.9115(4) 0.0307(7) Uani 1 1 d . . . . .
C16 C 0.57063(14) 0.01914(14) 0.8287(4) 0.0301(7) Uani 1 1 d . . . . .
C17 C 0.31436(16) 0.26620(16) 0.6077(5) 0.0381(8) Uani 1 1 d . . . . .
C18 C 0.3067(2) 0.31350(19) 0.4802(5) 0.0497(10) Uani 1 1 d . . . . .
H9 H 0.270355 0.336751 0.476649 0.060 Uiso 1 1 calc R U . . .
C19 C 0.3534(2) 0.3246(2) 0.3624(6) 0.0570(11) Uani 1 1 d . . . . .
H10 H 0.348854 0.355804 0.278986 0.068 Uiso 1 1 calc R U . . .
C20 C 0.4071(2) 0.2898(2) 0.3670(6) 0.0623(12) Uani 1 1 d . . . . .
H11 H 0.438595 0.297812 0.286694 0.075 Uiso 1 1 calc R U . . .
C21 C 0.4145(2) 0.2440(3) 0.4875(6) 0.0634(12) Uani 1 1 d . . . . .
H12 H 0.451020 0.220855 0.489325 0.076 Uiso 1 1 calc R U . . .
C22 C 0.36763(19) 0.2314(2) 0.6085(5) 0.0491(10) Uani 1 1 d . . . . .
H13 H 0.372494 0.199563 0.689591 0.059 Uiso 1 1 calc R U . . .
N1 N 0.55157(12) 0.04309(12) 0.6698(3) 0.0303(6) Uani 1 1 d . . . . .
N2 N 0.57657(13) 0.13641(13) 0.5094(3) 0.0340(7) Uani 1 1 d . . . . .
N3 N 0.51249(11) 0.06799(12) 0.3355(4) 0.0305(6) Uani 1 1 d . . . . .
N4 N 0.44479(13) 0.03472(13) 0.1000(4) 0.0323(6) Uani 1 1 d . . . . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0287(2) Uani 1 2 d S . P . .
P1 P 0.250000 0.250000 0.750000 0.0345(4) Uani 1 4 d S T P . .
Br1 Br 0.40608(2) 0.05573(2) 0.59390(6) 0.0419(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N4 1.319(4) . ?
C1 N3 1.376(4) . ?
C1 C2 1.461(4) . ?
C2 C7 1.386(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.387(5) . ?
C4 C5 1.407(5) . ?
C5 C6 1.381(4) . ?
C6 C7 1.388(4) . ?
C7 C8 1.456(4) . ?
C8 N2 1.321(4) . ?
C8 N3 1.367(4) . ?
C9 N2 1.328(4) . ?
C9 N1 1.360(4) . ?
C9 C10 1.460(4) . ?
C10 C15 1.389(4) . ?
C10 C11 1.392(4) . ?
C11 C12 1.385(5) . ?
C12 C13 1.399(5) . ?
C13 C14 1.378(5) . ?
C14 C15 1.391(4) . ?
C15 C16 1.457(4) . ?
C16 N4 1.323(4) 5_656 ?
C16 N1 1.379(4) . ?
C17 C22 1.370(5) . ?
C17 C18 1.418(5) . ?
C17 P1 1.795(4) . ?
C18 C19 1.369(5) . ?
C19 C20 1.379(6) . ?
C20 C21 1.358(7) . ?
C21 C22 1.395(6) . ?
N1 Fe1 1.942(3) . ?
N3 Fe1 1.947(3) . ?
Fe1 Br1 2.4586(4) 5_656 ?
Fe1 Br1 2.4587(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
N4 C1 N3 127.9(3) . . ?
N4 C1 C2 122.6(3) . . ?
N3 C1 C2 109.3(3) . . ?
C7 C2 C3 122.0(3) . . ?
C7 C2 C1 106.4(3) . . ?
C3 C2 C1 131.6(3) . . ?
C4 C3 C2 116.9(3) . . ?
C3 C4 C5 121.3(3) . . ?
C6 C5 C4 121.1(3) . . ?
C5 C6 C7 117.5(3) . . ?
C2 C7 C6 121.3(3) . . ?
C2 C7 C8 106.8(3) . . ?
C6 C7 C8 131.9(3) . . ?
N2 C8 N3 128.0(3) . . ?
N2 C8 C7 122.5(3) . . ?
N3 C8 C7 109.5(3) . . ?
N2 C9 N1 127.8(3) . . ?
N2 C9 C10 122.4(3) . . ?
N1 C9 C10 109.8(3) . . ?
C15 C10 C11 121.0(3) . . ?
C15 C10 C9 106.4(3) . . ?
C11 C10 C9 132.6(3) . . ?
C12 C11 C10 117.4(3) . . ?
C11 C12 C13 121.3(3) . . ?
C14 C13 C12 121.3(3) . . ?
C13 C14 C15 117.4(3) . . ?
C10 C15 C14 121.6(3) . . ?
C10 C15 C16 106.5(3) . . ?
C14 C15 C16 131.9(3) . . ?
N4 C16 N1 127.9(3) 5_656 . ?
N4 C16 C15 122.7(3) 5_656 . ?
N1 C16 C15 109.4(3) . . ?
C22 C17 C18 119.5(4) . . ?
C22 C17 P1 122.5(3) . . ?
C18 C17 P1 117.7(3) . . ?
C19 C18 C17 119.4(4) . . ?
C18 C19 C20 120.3(4) . . ?
C21 C20 C19 120.8(4) . . ?
C20 C21 C22 120.2(4) . . ?
C17 C22 C21 119.9(4) . . ?
C9 N1 C16 107.9(3) . . ?
C9 N1 Fe1 126.5(2) . . ?
C16 N1 Fe1 125.2(2) . . ?
C8 N2 C9 121.9(3) . . ?
C8 N3 C1 108.0(3) . . ?
C8 N3 Fe1 126.0(2) . . ?
C1 N3 Fe1 125.3(2) . . ?
C1 N4 C16 122.7(3) . 5_656 ?
N1 Fe1 N1 180.0 . 5_656 ?
N1 Fe1 N3 89.49(11) . . ?
N1 Fe1 N3 90.51(11) 5_656 . ?
N1 Fe1 N3 90.51(11) . 5_656 ?
N1 Fe1 N3 89.49(11) 5_656 5_656 ?
N3 Fe1 N3 180.0 . 5_656 ?
N1 Fe1 Br1 87.53(8) . 5_656 ?
N1 Fe1 Br1 92.47(8) 5_656 5_656 ?
N3 Fe1 Br1 93.78(8) . 5_656 ?
N3 Fe1 Br1 86.22(8) 5_656 5_656 ?
N1 Fe1 Br1 92.47(8) . . ?
N1 Fe1 Br1 87.53(8) 5_656 . ?
N3 Fe1 Br1 86.22(8) . . ?
N3 Fe1 Br1 93.78(8) 5_656 . ?
Br1 Fe1 Br1 180.0 5_656 . ?
C17 P1 C17 111.45(12) 2 8_657 ?
C17 P1 C17 111.45(12) 2 7_567 ?
C17 P1 C17 105.6(2) 8_657 7_567 ?
C17 P1 C17 105.6(2) 2 . ?
C17 P1 C17 111.46(12) 8_657 . ?
C17 P1 C17 111.45(12) 7_567 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C1 C2 C7 175.6(3) . . . . ?
N3 C1 C2 C7 -0.4(4) . . . . ?
N4 C1 C2 C3 -2.2(6) . . . . ?
N3 C1 C2 C3 -178.2(3) . . . . ?
C7 C2 C3 C4 -0.4(5) . . . . ?
C1 C2 C3 C4 177.1(4) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C3 C4 C5 C6 1.0(6) . . . . ?
C4 C5 C6 C7 -1.2(5) . . . . ?
C3 C2 C7 C6 0.1(5) . . . . ?
C1 C2 C7 C6 -177.9(3) . . . . ?
C3 C2 C7 C8 178.1(3) . . . . ?
C1 C2 C7 C8 0.1(4) . . . . ?
C5 C6 C7 C2 0.7(5) . . . . ?
C5 C6 C7 C8 -176.7(3) . . . . ?
C2 C7 C8 N2 -178.5(3) . . . . ?
C6 C7 C8 N2 -0.8(6) . . . . ?
C2 C7 C8 N3 0.3(4) . . . . ?
C6 C7 C8 N3 178.0(3) . . . . ?
N2 C9 C10 C15 -178.2(3) . . . . ?
N1 C9 C10 C15 1.4(4) . . . . ?
N2 C9 C10 C11 1.5(6) . . . . ?
N1 C9 C10 C11 -178.9(3) . . . . ?
C15 C10 C11 C12 0.0(5) . . . . ?
C9 C10 C11 C12 -179.6(3) . . . . ?
C10 C11 C12 C13 1.0(5) . . . . ?
C11 C12 C13 C14 -0.8(6) . . . . ?
C12 C13 C14 C15 -0.5(6) . . . . ?
C11 C10 C15 C14 -1.3(5) . . . . ?
C9 C10 C15 C14 178.4(3) . . . . ?
C11 C10 C15 C16 179.3(3) . . . . ?
C9 C10 C15 C16 -1.0(3) . . . . ?
C13 C14 C15 C10 1.5(5) . . . . ?
C13 C14 C15 C16 -179.3(3) . . . . ?
C10 C15 C16 N4 178.8(3) . . . 5_656 ?
C14 C15 C16 N4 -0.5(6) . . . 5_656 ?
C10 C15 C16 N1 0.2(4) . . . . ?
C14 C15 C16 N1 -179.0(3) . . . . ?
C22 C17 C18 C19 -1.5(6) . . . . ?
P1 C17 C18 C19 -176.1(3) . . . . ?
C17 C18 C19 C20 0.5(7) . . . . ?
C18 C19 C20 C21 0.2(7) . . . . ?
C19 C20 C21 C22 0.1(7) . . . . ?
C18 C17 C22 C21 1.8(6) . . . . ?
P1 C17 C22 C21 176.1(3) . . . . ?
C20 C21 C22 C17 -1.1(7) . . . . ?
N2 C9 N1 C16 178.3(3) . . . . ?
C10 C9 N1 C16 -1.3(3) . . . . ?
N2 C9 N1 Fe1 4.8(5) . . . . ?
C10 C9 N1 Fe1 -174.8(2) . . . . ?
N4 C16 N1 C9 -177.8(3) 5_656 . . . ?
C15 C16 N1 C9 0.7(3) . . . . ?
N4 C16 N1 Fe1 -4.2(5) 5_656 . . . ?
C15 C16 N1 Fe1 174.2(2) . . . . ?
N3 C8 N2 C9 -3.8(5) . . . . ?
C7 C8 N2 C9 174.8(3) . . . . ?
N1 C9 N2 C8 -2.9(5) . . . . ?
C10 C9 N2 C8 176.7(3) . . . . ?
N2 C8 N3 C1 178.2(3) . . . . ?
C7 C8 N3 C1 -0.6(3) . . . . ?
N2 C8 N3 Fe1 7.7(5) . . . . ?
C7 C8 N3 Fe1 -171.1(2) . . . . ?
N4 C1 N3 C8 -175.1(3) . . . . ?
C2 C1 N3 C8 0.7(3) . . . . ?
N4 C1 N3 Fe1 -4.5(5) . . . . ?
C2 C1 N3 Fe1 171.2(2) . . . . ?
N3 C1 N4 C16 -0.6(5) . . . 5_656 ?
C2 C1 N4 C16 -175.8(3) . . . 5_656 ?
C22 C17 P1 C17 -119.4(4) . . . 2 ?
C18 C17 P1 C17 55.0(3) . . . 2 ?
C22 C17 P1 C17 119.4(4) . . . 8_657 ?
C18 C17 P1 C17 -66.2(2) . . . 8_657 ?
C22 C17 P1 C17 1.7(3) . . . 7_567 ?
C18 C17 P1 C17 176.2(3) . . . 7_567 ?

_refine_diff_density_max         0.584
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.100

