# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1856804'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 B2 F8 Fe N10 O4'
_chemical_formula_weight         739.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.3370(10)
_cell_length_b                   16.5488(8)
_cell_length_c                   10.692(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.976(5)
_cell_angle_gamma                90
_cell_volume                     2963.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    5181
_cell_measurement_theta_min      2.8444
_cell_measurement_theta_max      27.4745

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.611
_shelx_estimated_absorpt_T_min   0.925
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_T_min  0.33100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      350.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            33269
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.850
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3412
_reflns_number_gt                2277
_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.1182P)²+7.2639P] 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         3412
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1839
_refine_ls_wR_factor_gt          0.1504
_refine_ls_goodness_of_fit_ref   0.806
_refine_ls_restrained_S_all      0.806
_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 0.1449(2) 0.2482(2) 1.0217(4) 0.0557(10) Uani 1 1 d . . . . .
H1 H 0.1541 0.1932 1.0363 0.067 Uiso 1 1 calc R U . . .
C2 C 0.1859(3) 0.3084(3) 1.1009(4) 0.0681(12) Uani 1 1 d . . . . .
H2 H 0.2263 0.3015 1.1765 0.082 Uiso 1 1 calc R U . . .
C3 C 0.1558(2) 0.3796(2) 1.0467(4) 0.0613(11) Uani 1 1 d . . . . .
H3 H 0.1720 0.4311 1.0770 0.074 Uiso 1 1 calc R U . . .
C4 C 0.04792(19) 0.41104(18) 0.8472(3) 0.0393(7) Uani 1 1 d . . . . .
C5 C 0.0487(2) 0.49376(19) 0.8540(3) 0.0442(8) Uani 1 1 d . . . . .
H5 H 0.0804 0.5209 0.9251 0.053 Uiso 1 1 calc R U . . .
C6 C 0.0000 0.5354(2) 0.7500 0.0406(10) Uani 1 2 d S T P . .
C7 C 0.0000 -0.0531(3) 0.7500 0.0404(10) Uani 1 2 d S T P . .
C8 C 0.0461(2) -0.01143(18) 0.6822(3) 0.0433(8) Uani 1 1 d . . . . .
H8 H 0.0762 -0.0385 0.6351 0.052 Uiso 1 1 calc R U . . .
C9 C 0.04518(19) 0.07174(18) 0.6881(3) 0.0408(7) Uani 1 1 d . . . . .
C10 C 0.1445(2) 0.1046(2) 0.5616(4) 0.0563(9) Uani 1 1 d . . . . .
H10 H 0.1590 0.0532 0.5407 0.068 Uiso 1 1 calc R U . . .
C11 C 0.1723(3) 0.1757(3) 0.5283(5) 0.0674(11) Uani 1 1 d . . . . .
H11 H 0.2090 0.1832 0.4795 0.081 Uiso 1 1 calc R U . . .
C12 C 0.1343(2) 0.2356(2) 0.5825(4) 0.0569(10) Uani 1 1 d . . . . .
H12 H 0.1430 0.2907 0.5759 0.068 Uiso 1 1 calc R U . . .
C13 C 0.0000 0.6255(3) 0.7500 0.0444(11) Uani 1 2 d S T P . .
C14 C 0.0000 -0.1432(3) 0.7500 0.0422(10) Uani 1 2 d S T P . .
N1 N 0.09062(17) 0.27879(16) 0.9220(3) 0.0457(7) Uani 1 1 d . . . . .
N2 N 0.09706(17) 0.36043(16) 0.9392(2) 0.0439(7) Uani 1 1 d . . . . .
N3 N 0.0000 0.3701(2) 0.7500 0.0354(8) Uani 1 2 d S T P . .
N4 N 0.0000 0.1127(2) 0.7500 0.0382(8) Uani 1 2 d S T P . .
N5 N 0.09170(17) 0.12232(16) 0.6308(3) 0.0449(7) Uani 1 1 d . . . . .
N6 N 0.08454(17) 0.20423(16) 0.6443(3) 0.0465(7) Uani 1 1 d . . . . .
O1 O 0.0126(2) 0.66063(15) 0.8568(3) 0.0705(9) Uani 1 1 d . . . . .
H1A H 0.0113 0.7097 0.8455 0.106 Uiso 0.5 1 calc R U P . .
O2 O 0.01701(19) -0.17786(14) 0.6564(3) 0.0636(8) Uani 1 1 d . . . . .
H2A H 0.0153 -0.2270 0.6657 0.095 Uiso 0.5 1 calc R U P . .
F1 F 0.1610(7) 0.4272(9) 0.6694(15) 0.128(5) Uani 0.5 1 d . . P A 1
F2 F 0.2755(7) 0.3564(8) 0.7254(12) 0.108(3) Uani 0.5 1 d . . P A 1
F3 F 0.2810(9) 0.4709(11) 0.6630(14) 0.133(6) Uani 0.5 1 d . . P A 1
F4 F 0.2575(8) 0.4428(7) 0.8600(9) 0.139(5) Uani 0.5 1 d . . P A 1
F5 F 0.1679(7) 0.4261(5) 0.6324(13) 0.122(5) Uani 0.5 1 d . . P A 2
F6 F 0.2194(7) 0.4898(8) 0.8129(11) 0.144(4) Uani 0.5 1 d . . P A 2
F7 F 0.2817(7) 0.4928(9) 0.6840(13) 0.113(5) Uani 0.5 1 d . . P A 2
F8 F 0.2604(15) 0.3694(11) 0.7745(17) 0.280(13) Uani 0.5 1 d . . P A 2
Fe Fe 0.0000 0.24223(3) 0.7500 0.0416(2) Uani 1 2 d S T P . .
B B 0.2378(4) 0.4325(4) 0.7281(6) 0.0751(15) 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 N1 1.326(4) . ?
C1 C2 1.380(5) . ?
C2 C3 1.356(5) . ?
C3 N2 1.361(4) . ?
C4 N3 1.335(3) . ?
C4 C5 1.371(4) . ?
C4 N2 1.400(4) . ?
C5 C6 1.393(4) . ?
C6 C5 1.393(4) 2_556 ?
C6 C13 1.491(6) . ?
C7 C8 1.393(4) . ?
C7 C8 1.393(4) 2_556 ?
C7 C14 1.490(6) . ?
C8 C9 1.378(4) . ?
C9 N4 1.334(4) . ?
C9 N5 1.408(4) . ?
C10 N5 1.349(5) . ?
C10 C11 1.355(5) . ?
C11 C12 1.395(6) . ?
C12 N6 1.321(5) . ?
C13 O1 1.249(3) . ?
C13 O1 1.250(3) 2_556 ?
C14 O2 1.254(3) . ?
C14 O2 1.254(3) 2_556 ?
N1 N2 1.364(4) . ?
N1 Fe 2.173(3) . ?
N3 C4 1.335(3) 2_556 ?
N3 Fe 2.116(3) . ?
N4 C9 1.334(4) 2_556 ?
N4 Fe 2.143(4) . ?
N5 N6 1.372(4) . ?
N6 Fe 2.163(3) . ?
F1 B 1.321(14) . ?
F2 B 1.422(12) . ?
F3 B 1.310(15) . ?
F4 B 1.373(11) . ?
F5 B 1.374(12) . ?
F6 B 1.406(13) . ?
F7 B 1.409(15) . ?
F8 B 1.178(15) . ?
Fe N6 2.163(3) 2_556 ?
Fe N1 2.173(3) 2_556 ?

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 C1 C2 111.3(3) . . ?
C3 C2 C1 106.5(3) . . ?
C2 C3 N2 106.3(3) . . ?
N3 C4 C5 122.9(3) . . ?
N3 C4 N2 112.7(3) . . ?
C5 C4 N2 124.3(3) . . ?
C4 C5 C6 117.2(3) . . ?
C5 C6 C5 120.6(4) . 2_556 ?
C5 C6 C13 119.68(19) . . ?
C5 C6 C13 119.68(19) 2_556 . ?
C8 C7 C8 120.6(4) . 2_556 ?
C8 C7 C14 119.7(2) . . ?
C8 C7 C14 119.7(2) 2_556 . ?
C9 C8 C7 117.1(3) . . ?
N4 C9 C8 123.1(3) . . ?
N4 C9 N5 112.9(3) . . ?
C8 C9 N5 124.0(3) . . ?
N5 C10 C11 107.0(4) . . ?
C10 C11 C12 105.7(4) . . ?
N6 C12 C11 111.6(3) . . ?
O1 C13 O1 124.6(4) . 2_556 ?
O1 C13 C6 117.7(2) . . ?
O1 C13 C6 117.7(2) 2_556 . ?
O2 C14 O2 125.5(4) . 2_556 ?
O2 C14 C7 117.3(2) . . ?
O2 C14 C7 117.3(2) 2_556 . ?
C1 N1 N2 104.7(3) . . ?
C1 N1 Fe 141.4(2) . . ?
N2 N1 Fe 113.94(18) . . ?
C3 N2 N1 111.2(3) . . ?
C3 N2 C4 129.8(3) . . ?
N1 N2 C4 119.0(2) . . ?
C4 N3 C4 119.0(3) 2_556 . ?
C4 N3 Fe 120.48(17) 2_556 . ?
C4 N3 Fe 120.48(17) . . ?
C9 N4 C9 118.9(4) 2_556 . ?
C9 N4 Fe 120.54(19) 2_556 . ?
C9 N4 Fe 120.55(19) . . ?
C10 N5 N6 111.4(3) . . ?
C10 N5 C9 130.9(3) . . ?
N6 N5 C9 117.6(3) . . ?
C12 N6 N5 104.3(3) . . ?
C12 N6 Fe 140.0(3) . . ?
N5 N6 Fe 115.7(2) . . ?
N3 Fe N4 180.0 . . ?
N3 Fe N6 106.90(7) . . ?
N4 Fe N6 73.10(7) . . ?
N3 Fe N6 106.90(7) . 2_556 ?
N4 Fe N6 73.10(7) . 2_556 ?
N6 Fe N6 146.20(14) . 2_556 ?
N3 Fe N1 73.83(7) . 2_556 ?
N4 Fe N1 106.17(7) . 2_556 ?
N6 Fe N1 94.47(11) . 2_556 ?
N6 Fe N1 94.81(11) 2_556 2_556 ?
N3 Fe N1 73.83(7) . . ?
N4 Fe N1 106.17(7) . . ?
N6 Fe N1 94.81(11) . . ?
N6 Fe N1 94.47(11) 2_556 . ?
N1 Fe N1 147.66(14) 2_556 . ?
F4 B F1 116.6(10) . . ?
F4 B F3 117.5(10) . . ?
F1 B F3 115.1(10) . . ?
F8 B F6 115.7(12) . . ?
F8 B F5 112.2(13) . . ?
F6 B F5 103.2(9) . . ?
F8 B F7 128.3(15) . . ?
F6 B F7 88.2(10) . . ?
F5 B F7 104.7(7) . . ?
F4 B F2 97.9(8) . . ?
F1 B F2 110.1(9) . . ?
F3 B F2 95.2(10) . . ?

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.060

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_ipc22b077
_database_code_depnum_ccdc_archive 'CCDC 1856805'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_audit_creation_date             2018-11-02
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H18 Fe N10 O4, 2(B F4)'
_chemical_formula_sum            'C24 H18 B2 F8 Fe N10 O4'
_chemical_formula_weight         739.95
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.1725(4)
_cell_length_b                   16.0377(4)
_cell_length_c                   10.6830(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.691(3)
_cell_angle_gamma                90
_cell_volume                     2818.22(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.4653
_cell_measurement_theta_min      2.9139
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.921
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            36207
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         2.920
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00    2.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -57.0000    0.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -88.00    5.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -69.0000  125.8234 93

#__ type_ start__ end____ width___ exp.time_
  3 omega  -88.00    1.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -59.0000 -149.1213 89

#__ type_ start__ end____ width___ exp.time_
  4 omega  -88.00    4.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -68.0000  -78.2451 92

#__ type_ start__ end____ width___ exp.time_
  5 omega  -18.00   45.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       20.8840  -68.0000  151.9306 63

#__ type_ start__ end____ width___ exp.time_
  6 omega  -46.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -68.0000  -87.9211 92

#__ type_ start__ end____ width___ exp.time_
  7 omega  -46.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -68.0000   72.4169 92

#__ type_ start__ end____ width___ exp.time_
  8 omega  -41.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -67.0000  -14.4210 87

#__ type_ start__ end____ width___ exp.time_
  9 omega  -46.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000 -149.1086 93

#__ type_ start__ end____ width___ exp.time_
 10 omega  -41.00   49.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340   57.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
 11 omega  -88.00    5.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.6340  -69.0000   45.3140 93

#__ type_ start__ end____ width___ exp.time_
 12 omega  -46.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000  106.3701 93

#__ type_ start__ end____ width___ exp.time_
 13 omega  -42.00   46.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -67.0000  -69.6662 88

#__ type_ start__ end____ width___ exp.time_
 14 omega  -25.00   -3.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -66.0000 -126.6387 22

#__ type_ start__ end____ width___ exp.time_
 15 omega  -43.00   47.00   1.0000   21.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000  -69.0000   19.2456 90
;
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0256229000
_diffrn_orient_matrix_UB_12      0.0351928000
_diffrn_orient_matrix_UB_13      -0.0040511000
_diffrn_orient_matrix_UB_21      -0.0341680000
_diffrn_orient_matrix_UB_22      -0.0245029000
_diffrn_orient_matrix_UB_23      -0.0327989000
_diffrn_orient_matrix_UB_31      -0.0060035000
_diffrn_orient_matrix_UB_32      -0.0108647000
_diffrn_orient_matrix_UB_33      0.0609032000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2778
_reflns_number_total             3248
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0413P)²+3.7461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0886
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1A(0.5) H2A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.62360(11) 0.24842(12) 0.58716(19) 0.0205(4) Uani 1 1 d . . . . .
H1 H 0.628930 0.307235 0.583006 0.025 Uiso 1 1 calc R . . . .
C2 C 0.66415(12) 0.19064(12) 0.52917(19) 0.0233(4) Uani 1 1 d . . . . .
H2 H 0.700566 0.202894 0.479455 0.028 Uiso 1 1 calc R . . . .
C3 C 0.64094(11) 0.11369(12) 0.55834(19) 0.0204(4) Uani 1 1 d . . . . .
H3 H 0.658324 0.061647 0.533377 0.024 Uiso 1 1 calc R . . . .
C4 C 0.54486(10) 0.07082(11) 0.68697(17) 0.0156(4) Uani 1 1 d . . . . .
C5 C 0.54592(10) -0.01545(11) 0.68176(17) 0.0161(4) Uani 1 1 d . . . . .
H5 H 0.576428 -0.044376 0.634068 0.019 Uiso 1 1 calc R . . . .
C6 C 0.500000 -0.05771(15) 0.750000 0.0152(5) Uani 1 2 d S T P . .
C7 C 0.500000 0.51870(15) 0.750000 0.0168(5) Uani 1 2 d S T P . .
C8 C 0.55074(11) 0.47690(11) 0.85699(18) 0.0176(4) Uani 1 1 d . . . . .
H8 H 0.583762 0.505848 0.930838 0.021 Uiso 1 1 calc R . . . .
C9 C 0.55018(10) 0.39075(11) 0.84929(17) 0.0154(3) Uani 1 1 d . . . . .
C10 C 0.65972(11) 0.34859(12) 1.05193(18) 0.0207(4) Uani 1 1 d . . . . .
H10 H 0.678176 0.400898 1.091017 0.025 Uiso 1 1 calc R . . . .
C11 C 0.68839(11) 0.27203(12) 1.09832(19) 0.0226(4) Uani 1 1 d . . . . .
H11 H 0.730333 0.260252 1.176201 0.027 Uiso 1 1 calc R . . . .
C12 C 0.64330(11) 0.21403(11) 1.00756(18) 0.0193(4) Uani 1 1 d . . . . .
H12 H 0.650882 0.155354 1.014686 0.023 Uiso 1 1 calc R . . . .
C13 C 0.500000 -0.15112(15) 0.750000 0.0161(5) Uani 1 2 d S T P . .
C14 C 0.500000 0.61229(15) 0.750000 0.0184(5) Uani 1 2 d S T P . .
N1 N 0.57712(9) 0.20992(9) 0.64816(15) 0.0162(3) Uani 1 1 d . . . . .
N2 N 0.58794(9) 0.12562(9) 0.63029(15) 0.0166(3) Uani 1 1 d . . . . .
N3 N 0.500000 0.11268(12) 0.750000 0.0143(4) Uani 1 2 d S T P . .
N4 N 0.58898(9) 0.25167(9) 0.91102(15) 0.0162(3) Uani 1 1 d . . . . .
N5 N 0.59965(9) 0.33579(9) 0.93896(15) 0.0167(3) Uani 1 1 d . . . . .
N6 N 0.500000 0.34895(12) 0.750000 0.0144(4) Uani 1 2 d S T P . .
O1 O 0.47802(8) -0.18721(8) 0.83900(13) 0.0236(3) Uani 1 1 d . . . . .
H1A H 0.480281 -0.239096 0.829840 0.035 Uiso 0.5 1 calc R . . . .
O2 O 0.50720(9) 0.64866(8) 0.85741(14) 0.0277(3) Uani 1 1 d . . . . .
H2A H 0.506427 0.700518 0.846074 0.042 Uiso 0.5 1 calc R . . . .
F1 F 0.75083(9) 0.05180(9) 0.14484(13) 0.0418(3) Uani 1 1 d . . . . .
F2 F 0.84292(7) 0.05125(8) 0.34755(12) 0.0316(3) Uani 1 1 d . . . . .
F3 F 0.72053(7) -0.01271(8) 0.31394(14) 0.0381(3) Uani 1 1 d . . . . .
F4 F 0.72697(8) 0.12837(8) 0.30667(14) 0.0403(3) Uani 1 1 d . . . . .
Fe Fe 0.500000 0.23049(2) 0.750000 0.01370(11) Uani 1 2 d S T P . .
B B 0.76040(13) 0.05468(14) 0.2782(2) 0.0236(5) 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 C2 1.405(3) . ?
C1 N1 1.320(2) . ?
C2 C3 1.360(3) . ?
C3 N2 1.363(2) . ?
C4 C5 1.385(2) . ?
C4 N2 1.394(2) . ?
C4 N3 1.340(2) . ?
C5 C6 1.394(2) . ?
C6 C13 1.498(3) . ?
C7 C8 1.394(2) 2_656 ?
C7 C8 1.394(2) . ?
C7 C14 1.501(3) . ?
C8 C9 1.384(2) . ?
C9 N5 1.396(2) . ?
C9 N6 1.339(2) . ?
C10 C11 1.362(3) . ?
C10 N5 1.359(2) . ?
C11 C12 1.405(3) . ?
C12 N4 1.321(2) . ?
C13 O1 1.2600(17) 2_656 ?
C13 O1 1.2601(17) . ?
C14 O2 1.2612(18) . ?
C14 O2 1.2612(18) 2_656 ?
N1 N2 1.385(2) . ?
N1 Fe 1.9683(15) . ?
N3 Fe 1.889(2) . ?
N4 N5 1.382(2) . ?
N4 Fe 1.9747(15) . ?
N6 Fe 1.900(2) . ?
F1 B 1.388(3) . ?
F2 B 1.399(2) . ?
F3 B 1.390(3) . ?
F4 B 1.385(3) . ?

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 C1 C2 110.84(17) . . ?
C3 C2 C1 106.40(17) . . ?
C2 C3 N2 106.79(17) . . ?
C5 C4 N2 126.70(16) . . ?
N3 C4 C5 122.47(17) . . ?
N3 C4 N2 110.84(16) . . ?
C4 C5 C6 116.66(17) . . ?
C5 C6 C5 121.8(2) . 2_656 ?
C5 C6 C13 119.09(11) . . ?
C5 C6 C13 119.09(11) 2_656 . ?
C8 C7 C8 122.5(2) . 2_656 ?
C8 C7 C14 118.74(11) 2_656 . ?
C8 C7 C14 118.74(11) . . ?
C9 C8 C7 116.06(17) . . ?
C8 C9 N5 126.67(16) . . ?
N6 C9 C8 122.61(16) . . ?
N6 C9 N5 110.72(15) . . ?
N5 C10 C11 106.84(16) . . ?
C10 C11 C12 106.01(16) . . ?
N4 C12 C11 111.21(16) . . ?
O1 C13 C6 117.35(12) 2_656 . ?
O1 C13 C6 117.35(11) . . ?
O1 C13 O1 125.3(2) 2_656 . ?
O2 C14 C7 117.55(12) . . ?
O2 C14 C7 117.55(12) 2_656 . ?
O2 C14 O2 124.9(2) 2_656 . ?
C1 N1 N2 105.33(15) . . ?
C1 N1 Fe 142.46(13) . . ?
N2 N1 Fe 112.20(11) . . ?
C3 N2 C4 132.84(16) . . ?
C3 N2 N1 110.64(14) . . ?
N1 N2 C4 116.52(14) . . ?
C4 N3 C4 119.9(2) . 2_656 ?
C4 N3 Fe 120.07(11) . . ?
C4 N3 Fe 120.07(11) 2_656 . ?
C12 N4 N5 104.91(14) . . ?
C12 N4 Fe 142.90(13) . . ?
N5 N4 Fe 112.17(11) . . ?
C10 N5 C9 132.13(16) . . ?
C10 N5 N4 111.03(14) . . ?
N4 N5 C9 116.82(14) . . ?
C9 N6 C9 119.9(2) 2_656 . ?
C9 N6 Fe 120.06(10) . . ?
C9 N6 Fe 120.05(10) 2_656 . ?
N1 Fe N1 160.71(9) 2_656 . ?
N1 Fe N4 92.01(6) . . ?
N1 Fe N4 92.01(6) 2_656 2_656 ?
N1 Fe N4 91.29(6) . 2_656 ?
N1 Fe N4 91.29(6) 2_656 . ?
N3 Fe N1 80.35(4) . 2_656 ?
N3 Fe N1 80.35(4) . . ?
N3 Fe N4 99.91(4) . . ?
N3 Fe N4 99.91(4) . 2_656 ?
N3 Fe N6 180.0 . . ?
N4 Fe N4 160.19(8) . 2_656 ?
N6 Fe N1 99.65(4) . 2_656 ?
N6 Fe N1 99.65(4) . . ?
N6 Fe N4 80.09(4) . 2_656 ?
N6 Fe N4 80.09(4) . . ?
F1 B F2 110.21(18) . . ?
F1 B F3 109.48(18) . . ?
F3 B F2 109.15(16) . . ?
F4 B F1 108.63(17) . . ?
F4 B F2 109.76(17) . . ?
F4 B F3 109.60(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1856809'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H42 F12 Fe2 N20 O21 S4'
_chemical_formula_weight         1787.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           ?
_space_group_name_H-M_alt        Pcab
_space_group_name_Hall           ?

_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, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'

_cell_length_a                   15.1365(3)
_cell_length_b                   21.8413(4)
_cell_length_c                   22.3085(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7375.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    10825
_cell_measurement_theta_min      3.5970
_cell_measurement_theta_max      27.3140

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_F_000             3616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.621
_shelx_estimated_absorpt_T_min   0.812
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_T_min  0.85339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      300.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            29948
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.342
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7655
_reflns_number_gt                5884
_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0888P)²+6.5561P] 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         7655
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1654
_refine_ls_wR_factor_gt          0.1491
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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 0.2394(2) 0.34341(16) 0.11360(16) 0.0444(8) Uani 1 1 d . . . . .
H1 H 0.2373 0.3754 0.1411 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1879(3) 0.34010(19) 0.06150(18) 0.0551(10) Uani 1 1 d . . . . .
H2 H 0.1466 0.3687 0.0485 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2102(2) 0.28742(17) 0.03406(16) 0.0447(8) Uani 1 1 d . . . . .
H3 H 0.1869 0.2726 -0.0017 0.054 Uiso 1 1 calc R U . . .
C4 C 0.31981(19) 0.20540(14) 0.06277(13) 0.0278(6) Uani 1 1 d . . . . .
C5 C 0.3130(2) 0.16254(14) 0.01722(13) 0.0316(7) Uani 1 1 d . . . . .
H5 H 0.2747 0.1682 -0.0149 0.038 Uiso 1 1 calc R U . . .
C6 C 0.3659(2) 0.11086(14) 0.02170(13) 0.0308(7) Uani 1 1 d . . . . .
C7 C 0.4235(2) 0.10293(14) 0.06908(13) 0.0314(7) Uani 1 1 d . . . . .
H7 H 0.4594 0.0685 0.0718 0.038 Uiso 1 1 calc R U . . .
C8 C 0.42579(19) 0.14792(13) 0.11196(12) 0.0275(6) Uani 1 1 d . . . . .
C9 C 0.5409(2) 0.11052(16) 0.18530(15) 0.0386(8) Uani 1 1 d . . . . .
H9 H 0.5592 0.0739 0.1681 0.046 Uiso 1 1 calc R U . . .
C10 C 0.5716(2) 0.13550(18) 0.23690(15) 0.0461(9) Uani 1 1 d . . . . .
H10 H 0.6149 0.1196 0.2620 0.055 Uiso 1 1 calc R U . . .
C11 C 0.5247(2) 0.19001(16) 0.24477(14) 0.0384(8) Uani 1 1 d . . . . .
H11 H 0.5324 0.2166 0.2769 0.046 Uiso 1 1 calc R U . . .
C12 C 0.3599(2) 0.06075(15) -0.02473(13) 0.0338(7) Uani 1 1 d . . . . .
C13 C 0.2301(2) 0.18185(16) 0.23173(16) 0.0407(8) Uani 1 1 d . . . . .
H13 H 0.2208 0.1509 0.2038 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1833(2) 0.18756(17) 0.28551(17) 0.0453(8) Uani 1 1 d . . . . .
H14 H 0.1389 0.1619 0.2997 0.054 Uiso 1 1 calc R U . . .
C15 C 0.2160(2) 0.23826(15) 0.31275(15) 0.0367(7) Uani 1 1 d . . . . .
H15 H 0.1979 0.2544 0.3493 0.044 Uiso 1 1 calc R U . . .
C16 C 0.33932(19) 0.31024(13) 0.28246(13) 0.0278(6) Uani 1 1 d . . . . .
C17 C 0.3473(2) 0.34809(14) 0.33111(13) 0.0322(7) Uani 1 1 d . . . . .
H17 H 0.3112 0.3439 0.3646 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4123(2) 0.39317(14) 0.32796(13) 0.0309(7) Uani 1 1 d . . . . .
C19 C 0.4656(2) 0.39908(14) 0.27792(13) 0.0309(7) Uani 1 1 d . . . . .
H19 H 0.5093 0.4289 0.2757 0.037 Uiso 1 1 calc R U . . .
C20 C 0.4511(2) 0.35886(14) 0.23170(13) 0.0292(6) Uani 1 1 d . . . . .
C21 C 0.5628(2) 0.39087(16) 0.15340(15) 0.0405(8) Uani 1 1 d . . . . .
H21 H 0.5889 0.4251 0.1708 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5833(3) 0.36629(18) 0.09967(16) 0.0479(9) Uani 1 1 d . . . . .
H22 H 0.6260 0.3801 0.0730 0.057 Uiso 1 1 calc R U . . .
C23 C 0.5276(2) 0.31610(17) 0.09226(14) 0.0408(8) Uani 1 1 d . . . . .
H23 H 0.5276 0.2906 0.0588 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4280(2) 0.43719(15) 0.37821(14) 0.0366(7) Uani 1 1 d . . . . .
C25 C 0.4486(3) 0.1847(2) 0.41440(17) 0.0536(10) Uani 1 1 d . . . . .
C26 C 0.3389(3) 0.5357(2) 0.2113(3) 0.0704(13) Uani 1 1 d . . . . .
C27 C 0.6343(10) 0.0389(9) 0.5060(10) 0.158(9) Uani 0.5 1 d . . P . .
H27A H 0.6500 0.0110 0.5375 0.237 Uiso 0.5 1 calc R U P . .
H27B H 0.5712 0.0429 0.5043 0.237 Uiso 0.5 1 calc R U P . .
H27C H 0.6602 0.0782 0.5138 0.237 Uiso 0.5 1 calc R U P . .
C28 C 0.6636(5) 0.0179(4) 0.4547(5) 0.059(2) Uani 0.5 1 d . . P . .
C29 C 0.6451(7) 0.0534(4) 0.3990(5) 0.071(3) Uani 0.5 1 d . . P . .
H29A H 0.6697 0.0323 0.3651 0.106 Uiso 0.5 1 calc R U P . .
H29B H 0.6712 0.0933 0.4021 0.106 Uiso 0.5 1 calc R U P . .
H29C H 0.5824 0.0574 0.3938 0.106 Uiso 0.5 1 calc R U P . .
N1 N 0.29099(17) 0.29522(12) 0.11847(11) 0.0327(6) Uani 1 1 d . . . . .
N2 N 0.27304(18) 0.25979(12) 0.06836(11) 0.0316(6) Uani 1 1 d . . . . .
N3 N 0.37479(16) 0.19769(11) 0.10907(10) 0.0267(5) Uani 1 1 d . . . . .
N4 N 0.47853(17) 0.14907(12) 0.16348(11) 0.0305(6) Uani 1 1 d . . . . .
N5 N 0.46799(16) 0.19894(11) 0.20067(11) 0.0299(5) Uani 1 1 d . . . . .
N6 N 0.28919(17) 0.22600(12) 0.22553(11) 0.0312(6) Uani 1 1 d . . . . .
N7 N 0.28037(17) 0.26102(12) 0.27650(11) 0.0310(6) Uani 1 1 d . . . . .
N8 N 0.38933(16) 0.31527(11) 0.23399(10) 0.0264(5) Uani 1 1 d . . . . .
N9 N 0.49726(17) 0.35646(12) 0.17719(11) 0.0307(6) Uani 1 1 d . . . . .
N10 N 0.47470(17) 0.30939(12) 0.13901(11) 0.0318(6) Uani 1 1 d . . . . .
O1 O 0.38536(17) 0.00913(10) -0.01535(10) 0.0422(6) Uani 1 1 d . . . . .
O2 O 0.3252(2) 0.07980(11) -0.07452(10) 0.0508(7) Uani 1 1 d . . . . .
H2A H 0.3229 0.0514 -0.0985 0.076 Uiso 1 1 calc R U . . .
O3 O 0.48305(19) 0.47624(12) 0.37551(12) 0.0559(7) Uani 1 1 d . . . . .
O4 O 0.37522(19) 0.42865(13) 0.42407(11) 0.0573(8) Uani 1 1 d . . . . .
H4 H 0.3866 0.4538 0.4503 0.086 Uiso 1 1 calc R U . . .
O5 O 0.5264(2) 0.27871(14) 0.37179(12) 0.0636(8) Uani 1 1 d . . . . .
O6 O 0.6073(2) 0.21734(16) 0.44226(16) 0.0724(9) Uani 1 1 d . . . . .
O7 O 0.4855(2) 0.27854(14) 0.47698(13) 0.0699(9) Uani 1 1 d . . . . .
O8 O 0.25457(19) 0.43868(12) 0.24067(12) 0.0555(7) Uani 1 1 d . . . . .
O9 O 0.2084(2) 0.49073(12) 0.15220(12) 0.0612(8) Uani 1 1 d . . . . .
O10 O 0.1778(2) 0.53620(14) 0.24714(14) 0.0679(8) Uani 1 1 d . . . . .
O11 O 0.6995(4) -0.0280(2) 0.4567(4) 0.085(2) Uani 0.5 1 d . . P . .
F1 F 0.4771(2) 0.14815(14) 0.37101(12) 0.0881(9) Uani 1 1 d . . . . .
F2 F 0.4367(2) 0.15025(14) 0.46094(12) 0.0991(11) Uani 1 1 d . . . . .
F3 F 0.37029(19) 0.20616(18) 0.39874(18) 0.1059(12) Uani 1 1 d . . . . .
F4 F 0.3985(2) 0.50225(16) 0.1846(2) 0.1172(14) Uani 1 1 d . . . . .
F5 F 0.3677(3) 0.5467(2) 0.2655(2) 0.1384(16) Uani 1 1 d . . . . .
F6 F 0.3318(2) 0.58830(14) 0.18317(19) 0.1134(13) Uani 1 1 d . . . . .
S1 S 0.52572(6) 0.24733(4) 0.42803(4) 0.0434(2) Uani 1 1 d . . . . .
S2 S 0.23333(5) 0.49630(4) 0.21411(4) 0.0358(2) Uani 1 1 d . . . . .
Fe Fe 0.38035(3) 0.25739(2) 0.17088(2) 0.02601(14) 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 N1 1.315(4) . ?
C1 C2 1.401(5) . ?
C2 C3 1.346(5) . ?
C3 N2 1.362(4) . ?
C4 N3 1.337(4) . ?
C4 C5 1.385(4) . ?
C4 N2 1.389(4) . ?
C5 C6 1.388(4) . ?
C6 C7 1.381(4) . ?
C6 C12 1.510(4) . ?
C7 C8 1.372(4) . ?
C8 N3 1.335(4) . ?
C8 N4 1.400(4) . ?
C9 N4 1.355(4) . ?
C9 C10 1.356(5) . ?
C10 C11 1.397(5) . ?
C11 N5 1.320(4) . ?
C12 O1 1.210(4) . ?
C12 O2 1.297(4) . ?
C13 N6 1.323(4) . ?
C13 C14 1.399(5) . ?
C14 C15 1.357(5) . ?
C15 N7 1.360(4) . ?
C16 N8 1.325(4) . ?
C16 C17 1.370(4) . ?
C16 N7 1.403(4) . ?
C17 C18 1.394(5) . ?
C18 C19 1.384(4) . ?
C18 C24 1.496(4) . ?
C19 C20 1.372(4) . ?
C20 N8 1.335(4) . ?
C20 N9 1.404(4) . ?
C21 C22 1.349(5) . ?
C21 N9 1.353(4) . ?
C22 C23 1.393(5) . ?
C23 N10 1.323(4) . ?
C24 O3 1.194(4) . ?
C24 O4 1.311(4) . ?
C25 F2 1.294(5) . ?
C25 F3 1.322(5) . ?
C25 F1 1.326(5) . ?
C25 S1 1.825(4) . ?
C26 F4 1.304(6) . ?
C26 F5 1.308(7) . ?
C26 F6 1.314(5) . ?
C26 S2 1.816(4) . ?
C27 C28 1.31(2) . ?
C28 O11 1.141(10) . ?
C28 C29 1.490(14) . ?
N1 N2 1.386(3) . ?
N1 Fe 1.970(3) . ?
N3 Fe 1.900(2) . ?
N4 N5 1.379(3) . ?
N5 Fe 1.958(3) . ?
N6 N7 1.377(3) . ?
N6 Fe 1.965(3) . ?
N8 Fe 1.897(2) . ?
N9 N10 1.378(3) . ?
N10 Fe 1.958(3) . ?
O5 S1 1.430(3) . ?
O6 S1 1.433(3) . ?
O7 S1 1.424(3) . ?
O8 S2 1.428(2) . ?
O9 S2 1.437(3) . ?
O10 S2 1.417(3) . ?

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 C1 C2 110.9(3) . . ?
C3 C2 C1 106.4(3) . . ?
C2 C3 N2 107.3(3) . . ?
N3 C4 C5 121.9(3) . . ?
N3 C4 N2 110.8(2) . . ?
C5 C4 N2 127.3(3) . . ?
C4 C5 C6 117.0(3) . . ?
C7 C6 C5 121.5(3) . . ?
C7 C6 C12 118.2(3) . . ?
C5 C6 C12 120.4(3) . . ?
C8 C7 C6 117.3(3) . . ?
N3 C8 C7 122.4(3) . . ?
N3 C8 N4 110.8(2) . . ?
C7 C8 N4 126.8(3) . . ?
N4 C9 C10 107.1(3) . . ?
C9 C10 C11 106.0(3) . . ?
N5 C11 C10 111.2(3) . . ?
O1 C12 O2 125.2(3) . . ?
O1 C12 C6 122.5(3) . . ?
O2 C12 C6 112.3(3) . . ?
N6 C13 C14 111.5(3) . . ?
C15 C14 C13 105.8(3) . . ?
C14 C15 N7 107.1(3) . . ?
N8 C16 C17 123.1(3) . . ?
N8 C16 N7 110.5(2) . . ?
C17 C16 N7 126.4(3) . . ?
C16 C17 C18 116.7(3) . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 C24 116.9(3) . . ?
C17 C18 C24 121.9(3) . . ?
C20 C19 C18 116.9(3) . . ?
N8 C20 C19 122.7(3) . . ?
N8 C20 N9 110.8(2) . . ?
C19 C20 N9 126.5(3) . . ?
C22 C21 N9 107.2(3) . . ?
C21 C22 C23 106.2(3) . . ?
N10 C23 C22 111.1(3) . . ?
O3 C24 O4 124.5(3) . . ?
O3 C24 C18 122.1(3) . . ?
O4 C24 C18 113.4(3) . . ?
F2 C25 F3 107.1(4) . . ?
F2 C25 F1 106.3(4) . . ?
F3 C25 F1 108.2(4) . . ?
F2 C25 S1 113.0(3) . . ?
F3 C25 S1 110.6(3) . . ?
F1 C25 S1 111.4(3) . . ?
F4 C26 F5 107.1(5) . . ?
F4 C26 F6 109.2(4) . . ?
F5 C26 F6 107.9(5) . . ?
F4 C26 S2 111.1(4) . . ?
F5 C26 S2 110.4(4) . . ?
F6 C26 S2 111.0(3) . . ?
O11 C28 C27 115.7(13) . . ?
O11 C28 C29 125.3(11) . . ?
C27 C28 C29 118.9(11) . . ?
C1 N1 N2 105.3(3) . . ?
C1 N1 Fe 142.4(2) . . ?
N2 N1 Fe 112.28(18) . . ?
C3 N2 N1 110.0(3) . . ?
C3 N2 C4 133.2(3) . . ?
N1 N2 C4 116.7(2) . . ?
C8 N3 C4 120.0(2) . . ?
C8 N3 Fe 119.89(19) . . ?
C4 N3 Fe 120.1(2) . . ?
C9 N4 N5 110.8(2) . . ?
C9 N4 C8 132.9(3) . . ?
N5 N4 C8 116.3(2) . . ?
C11 N5 N4 104.9(2) . . ?
C11 N5 Fe 142.2(2) . . ?
N4 N5 Fe 112.92(17) . . ?
C13 N6 N7 104.7(3) . . ?
C13 N6 Fe 142.6(2) . . ?
N7 N6 Fe 112.75(18) . . ?
C15 N7 N6 111.0(3) . . ?
C15 N7 C16 132.8(3) . . ?
N6 N7 C16 116.2(2) . . ?
C16 N8 C20 119.4(2) . . ?
C16 N8 Fe 120.6(2) . . ?
C20 N8 Fe 119.80(19) . . ?
C21 N9 N10 110.7(2) . . ?
C21 N9 C20 133.2(3) . . ?
N10 N9 C20 116.1(2) . . ?
C23 N10 N9 104.8(3) . . ?
C23 N10 Fe 142.4(2) . . ?
N9 N10 Fe 112.89(18) . . ?
O7 S1 O5 116.5(2) . . ?
O7 S1 O6 114.7(2) . . ?
O5 S1 O6 114.0(2) . . ?
O7 S1 C25 102.31(19) . . ?
O5 S1 C25 102.61(19) . . ?
O6 S1 C25 104.2(2) . . ?
O10 S2 O8 117.38(19) . . ?
O10 S2 O9 113.34(19) . . ?
O8 S2 O9 112.54(17) . . ?
O10 S2 C26 104.4(2) . . ?
O8 S2 C26 103.5(2) . . ?
O9 S2 C26 103.8(2) . . ?
N8 Fe N3 177.84(11) . . ?
N8 Fe N5 97.70(10) . . ?
N3 Fe N5 80.14(10) . . ?
N8 Fe N10 80.26(10) . . ?
N3 Fe N10 99.61(10) . . ?
N5 Fe N10 90.42(11) . . ?
N8 Fe N6 79.76(10) . . ?
N3 Fe N6 100.35(10) . . ?
N5 Fe N6 92.15(11) . . ?
N10 Fe N6 160.02(10) . . ?
N8 Fe N1 102.14(10) . . ?
N3 Fe N1 80.02(10) . . ?
N5 Fe N1 160.15(10) . . ?
N10 Fe N1 92.41(11) . . ?
N6 Fe N1 91.87(11) . . ?

_refine_diff_density_max         0.846
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.089

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1856808'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H24 F12 Fe N10 O5 Sb2'
_chemical_formula_weight         1095.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y+1/2, x, z+1/4'
'-y+1/2, -x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1, x+1/2, z+3/4'
'-y+1, -x+1/2, z+3/4'

_cell_length_a                   23.6034(15)
_cell_length_b                   23.6034(15)
_cell_length_c                   14.9526(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8330.4(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    1704
_cell_measurement_theta_min      3.3930
_cell_measurement_theta_max      17.1230

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_F_000             4256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.732
_shelx_estimated_absorpt_T_min   0.769
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_T_min  0.40401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      299.9(3)
_diffrn_ambient_environment      air
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            19539
_diffrn_reflns_av_unetI/netI     0.1275
_diffrn_reflns_av_R_equivalents  0.1398
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.226
_diffrn_reflns_theta_max         27.604
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4802
_reflns_number_gt                2000
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.998

_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0588P)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_abs_structure_details 
;
 Flack x determined using 640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4802
_refine_ls_number_parameters     276
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1756
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1825
_refine_ls_wR_factor_gt          0.1328
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_restrained_S_all      0.957
_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 0.5917(8) 0.4541(9) 1.0257(13) 0.091(6) Uani 1 1 d . . . . .
H1 H 0.6168 0.4844 1.0285 0.109 Uiso 1 1 calc R U . . .
C2 C 0.6001(9) 0.4017(10) 1.0698(13) 0.095(7) Uani 1 1 d . . . . .
H2 H 0.6304 0.3921 1.1066 0.114 Uiso 1 1 calc R U . . .
C3 C 0.5560(9) 0.3689(10) 1.0484(13) 0.092(6) Uani 1 1 d . . . . .
H3 H 0.5500 0.3316 1.0663 0.110 Uiso 1 1 calc R U . . .
C4 C 0.4709(7) 0.3877(7) 0.9486(12) 0.070(5) Uani 1 1 d . . . . .
C5 C 0.4426(7) 0.3380(8) 0.9554(11) 0.071(5) Uani 1 1 d . . . . .
H5 H 0.4540 0.3094 0.9943 0.085 Uiso 1 1 calc R U . . .
C6 C 0.3961(8) 0.3328(6) 0.9010(13) 0.069(4) Uani 1 1 d . . . . .
C7 C 0.3757(6) 0.3758(7) 0.8466(12) 0.071(5) Uani 1 1 d . . . . .
H7 H 0.3423 0.3725 0.8139 0.086 Uiso 1 1 calc R U . . .
C8 C 0.4091(7) 0.4245(6) 0.8447(11) 0.058(4) Uani 1 1 d . . . . .
C9 C 0.3566(8) 0.4892(9) 0.7391(16) 0.090(5) Uani 1 1 d . . . . .
H9 H 0.3240 0.4685 0.7269 0.109 Uiso 1 1 calc R U . . .
C10 C 0.3710(10) 0.5421(8) 0.7047(15) 0.099(7) Uani 1 1 d . . . . .
H10 H 0.3500 0.5636 0.6645 0.119 Uiso 1 1 calc R U . . .
C11 C 0.4232(10) 0.5564(8) 0.7428(14) 0.090(6) Uani 1 1 d . . . . .
H11 H 0.4435 0.5893 0.7305 0.108 Uiso 1 1 calc R U . . .
C12 C 0.3635(10) 0.2764(8) 0.9034(19) 0.098(7) Uani 1 1 d . . . . .
C13 C 0.194(2) 0.236(3) 0.881(4) 0.16(3) Uani 0.5 1 d . . P . .
H13A H 0.2231 0.2651 0.8862 0.244 Uiso 0.5 1 calc R U P . .
H13B H 0.1727 0.2347 0.9350 0.244 Uiso 0.5 1 calc R U P . .
H13C H 0.1698 0.2455 0.8316 0.244 Uiso 0.5 1 calc R U P . .
C14 C 0.2204(19) 0.183(2) 0.865(3) 0.091(14) Uani 0.5 1 d . . P . .
C15 C 0.1865(17) 0.1321(16) 0.871(4) 0.133(19) Uani 0.5 1 d . . P . .
H15A H 0.2100 0.0996 0.8609 0.199 Uiso 0.5 1 calc R U P . .
H15B H 0.1570 0.1333 0.8268 0.199 Uiso 0.5 1 calc R U P . .
H15C H 0.1698 0.1296 0.9295 0.199 Uiso 0.5 1 calc R U P . .
N1 N 0.5444(6) 0.4546(5) 0.9804(9) 0.066(4) Uani 1 1 d . . . . .
N2 N 0.5215(5) 0.4007(6) 0.9950(11) 0.072(4) Uani 1 1 d . . . . .
N3 N 0.4564(5) 0.4306(5) 0.8948(10) 0.059(3) Uani 1 1 d . . . . .
N4 N 0.3998(6) 0.4740(6) 0.7940(10) 0.067(4) Uani 1 1 d . . . . .
N5 N 0.4395(6) 0.5162(6) 0.7989(9) 0.066(4) Uani 1 1 d . . . . .
O1 O 0.3782(7) 0.2384(7) 0.9481(12) 0.124(6) Uani 1 1 d . . . . .
O2 O 0.3223(8) 0.2762(6) 0.8500(15) 0.153(8) Uani 1 1 d . . . . .
H2A H 0.3061 0.2455 0.8527 0.229 Uiso 1 1 calc R U . . .
O3 O 0.2697(14) 0.1775(10) 0.848(2) 0.115(11) Uani 0.5 1 d . . P . .
F1 F 0.8293(4) 0.4909(7) 0.9897(13) 0.154(5) Uani 1 1 d . . . . .
F2 F 0.7997(7) 0.5929(7) 0.9511(13) 0.189(8) Uani 1 1 d . . . . .
F3 F 0.7464(7) 0.5102(10) 0.8787(12) 0.181(8) Uani 1 1 d . . . . .
F4 F 0.7815(10) 0.5512(8) 1.1097(13) 0.185(8) Uani 1 1 d . . . . .
F5 F 0.7283(6) 0.4692(7) 1.0404(13) 0.175(8) Uani 1 1 d . . . . .
F6 F 0.6954(6) 0.5679(8) 1.0021(14) 0.195(9) Uani 1 1 d . . . . .
Fe Fe 0.5000 0.5000 0.8895(3) 0.0564(7) Uani 1 2 d S T P . .
Sb Sb 0.76307(6) 0.53228(7) 0.99542(11) 0.0960(5) 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 N1 1.31(2) . ?
C1 C2 1.41(3) . ?
C2 C3 1.34(3) . ?
C3 N2 1.37(2) . ?
C4 N3 1.34(2) . ?
C4 C5 1.35(2) . ?
C4 N2 1.41(2) . ?
C5 C6 1.37(2) . ?
C6 C7 1.39(2) . ?
C6 C12 1.54(2) . ?
C7 C8 1.39(2) . ?
C8 N3 1.351(19) . ?
C8 N4 1.410(19) . ?
C9 N4 1.36(2) . ?
C9 C10 1.39(3) . ?
C10 C11 1.40(3) . ?
C11 N5 1.32(2) . ?
C12 O1 1.17(2) . ?
C12 O2 1.26(3) . ?
C13 C14 1.42(6) . ?
C14 O3 1.20(5) . ?
C14 C15 1.45(5) . ?
N1 N2 1.400(16) . ?
N1 Fe 2.023(14) . ?
N3 Fe 1.937(12) . ?
N4 N5 1.371(17) . ?
N5 Fe 2.006(14) . ?
F1 Sb 1.846(11) . ?
F2 Sb 1.798(14) . ?
F3 Sb 1.863(17) . ?
F4 Sb 1.819(17) . ?
F5 Sb 1.829(15) . ?
F6 Sb 1.808(13) . ?
Fe N3 1.937(12) 2_665 ?
Fe N5 2.006(14) 2_665 ?
Fe N1 2.023(14) 2_665 ?

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 C1 C2 111.7(18) . . ?
C3 C2 C1 106.7(18) . . ?
C2 C3 N2 106.5(19) . . ?
N3 C4 C5 125.0(17) . . ?
N3 C4 N2 110.3(14) . . ?
C5 C4 N2 124.6(17) . . ?
C4 C5 C6 115.4(17) . . ?
C5 C6 C7 124.0(15) . . ?
C5 C6 C12 117.7(18) . . ?
C7 C6 C12 118.3(18) . . ?
C8 C7 C6 114.8(15) . . ?
N3 C8 C7 123.0(15) . . ?
N3 C8 N4 109.8(12) . . ?
C7 C8 N4 127.3(16) . . ?
N4 C9 C10 106.2(18) . . ?
C9 C10 C11 106.3(18) . . ?
N5 C11 C10 109.8(18) . . ?
O1 C12 O2 126(2) . . ?
O1 C12 C6 122(2) . . ?
O2 C12 C6 112(2) . . ?
O3 C14 C13 123(4) . . ?
O3 C14 C15 117(5) . . ?
C13 C14 C15 119(4) . . ?
C1 N1 N2 103.9(15) . . ?
C1 N1 Fe 142.8(13) . . ?
N2 N1 Fe 112.6(10) . . ?
C3 N2 N1 111.1(15) . . ?
C3 N2 C4 132.0(17) . . ?
N1 N2 C4 116.6(14) . . ?
C4 N3 C8 117.7(13) . . ?
C4 N3 Fe 121.8(11) . . ?
C8 N3 Fe 120.5(11) . . ?
C9 N4 N5 110.6(15) . . ?
C9 N4 C8 131.5(16) . . ?
N5 N4 C8 117.9(13) . . ?
C11 N5 N4 106.9(15) . . ?
C11 N5 Fe 140.5(14) . . ?
N4 N5 Fe 112.6(10) . . ?
N3 Fe N3 175.4(9) . 2_665 ?
N3 Fe N5 104.2(6) . 2_665 ?
N3 Fe N5 79.1(6) 2_665 2_665 ?
N3 Fe N5 79.1(6) . . ?
N3 Fe N5 104.1(6) 2_665 . ?
N5 Fe N5 95.0(8) 2_665 . ?
N3 Fe N1 78.5(5) . . ?
N3 Fe N1 98.3(5) 2_665 . ?
N5 Fe N1 89.0(5) 2_665 . ?
N5 Fe N1 157.5(5) . . ?
N3 Fe N1 98.3(5) . 2_665 ?
N3 Fe N1 78.5(5) 2_665 2_665 ?
N5 Fe N1 157.5(5) 2_665 2_665 ?
N5 Fe N1 89.0(5) . 2_665 ?
N1 Fe N1 95.6(8) . 2_665 ?
F2 Sb F6 94.3(8) . . ?
F2 Sb F4 92.1(11) . . ?
F6 Sb F4 92.6(9) . . ?
F2 Sb F5 177.9(8) . . ?
F6 Sb F5 87.8(8) . . ?
F4 Sb F5 87.8(11) . . ?
F2 Sb F1 89.8(8) . . ?
F6 Sb F1 175.7(9) . . ?
F4 Sb F1 88.3(9) . . ?
F5 Sb F1 88.1(7) . . ?
F2 Sb F3 88.8(9) . . ?
F6 Sb F3 89.7(9) . . ?
F4 Sb F3 177.5(9) . . ?
F5 Sb F3 91.3(10) . . ?
F1 Sb F3 89.3(8) . . ?

_refine_diff_density_max         0.418
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1856806'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 As2 F12 Fe N10 O6'
_chemical_formula_weight         1060.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y+1/2, x, z+1/4'
'-y+1/2, -x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1, x+1/2, z+3/4'
'-y+1, -x+1/2, z+3/4'

_cell_length_a                   23.3533(3)
_cell_length_b                   23.3533(3)
_cell_length_c                   14.3811(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7843.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5184
_cell_measurement_theta_min      3.4430
_cell_measurement_theta_max      26.6850

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             4224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.173
_shelx_estimated_absorpt_T_min   0.571
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_T_min  0.86484
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120.05(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            15144
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.327
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4151
_reflns_number_gt                3530
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_max     0.875
_reflns_Friedel_fraction_full    0.998

_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0359P)²+4.7591P] 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_abs_structure_details 
;
 Flack x determined using 1431 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4151
_refine_ls_number_parameters     276
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0771
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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 0.4055(2) 0.0424(3) -0.0774(4) 0.0245(13) Uani 1 1 d . . . . .
H1 H 0.3805 0.0104 -0.0794 0.029 Uiso 1 1 calc R U . . .
C2 C 0.3952(3) 0.0941(3) -0.1222(4) 0.0284(14) Uani 1 1 d . . . . .
H2 H 0.3632 0.1032 -0.1600 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4400(3) 0.1291(3) -0.1014(4) 0.0255(14) Uani 1 1 d . . . . .
H3 H 0.4452 0.1676 -0.1209 0.031 Uiso 1 1 calc R U . . .
C4 C 0.5261(2) 0.1119(2) 0.0015(4) 0.0163(12) Uani 1 1 d . . . . .
C5 C 0.5551(2) 0.1631(2) -0.0034(4) 0.0199(12) Uani 1 1 d . . . . .
H5 H 0.5430 0.1930 -0.0438 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6025(2) 0.1690(2) 0.0531(4) 0.0181(12) Uani 1 1 d . . . . .
C7 C 0.6217(2) 0.1243(2) 0.1092(4) 0.0187(11) Uani 1 1 d . . . . .
H7 H 0.6549 0.1281 0.1469 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5904(2) 0.0747(2) 0.1074(4) 0.0172(12) Uani 1 1 d . . . . .
C9 C 0.6454(2) 0.0077(2) 0.2119(4) 0.0210(12) Uani 1 1 d . . . . .
H9 H 0.6791 0.0289 0.2249 0.025 Uiso 1 1 calc R U . . .
C10 C 0.6319(3) -0.0460(3) 0.2443(4) 0.0267(14) Uani 1 1 d . . . . .
H10 H 0.6545 -0.0692 0.2843 0.032 Uiso 1 1 calc R U . . .
C11 C 0.5791(3) -0.0595(2) 0.2071(4) 0.0242(13) Uani 1 1 d . . . . .
H11 H 0.5593 -0.0944 0.2185 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6317(2) 0.2262(2) 0.0535(4) 0.0240(13) Uani 1 1 d . . . . .
C13 C 0.3071(4) 0.2487(4) 0.1079(8) 0.076(3) Uani 1 1 d . . . . .
H13A H 0.2766 0.2753 0.1258 0.114 Uiso 1 1 calc R U . . .
H13B H 0.3237 0.2608 0.0485 0.114 Uiso 1 1 calc R U . . .
H13C H 0.3369 0.2486 0.1559 0.114 Uiso 1 1 calc R U . . .
C14 C 0.2827(3) 0.1895(4) 0.0979(5) 0.048(2) Uani 1 1 d . . . . .
C15 C 0.3212(4) 0.1418(4) 0.0722(7) 0.075(3) Uani 1 1 d . . . . .
H15A H 0.2993 0.1061 0.0693 0.113 Uiso 1 1 calc R U . . .
H15B H 0.3516 0.1382 0.1189 0.113 Uiso 1 1 calc R U . . .
H15C H 0.3384 0.1496 0.0112 0.113 Uiso 1 1 calc R U . . .
N1 N 0.45440(19) 0.04355(19) -0.0317(3) 0.0192(11) Uani 1 1 d . . . . .
N2 N 0.47612(18) 0.0975(2) -0.0465(3) 0.0193(10) Uani 1 1 d . . . . .
N3 N 0.54283(18) 0.06876(19) 0.0565(3) 0.0149(9) Uani 1 1 d . . . . .
N4 N 0.6009(2) 0.02413(19) 0.1578(3) 0.0174(10) Uani 1 1 d . . . . .
N5 N 0.5594(2) -0.01764(19) 0.1535(3) 0.0182(10) Uani 1 1 d . . . . .
O1 O 0.61888(18) 0.26480(16) 0.0028(3) 0.0254(9) Uani 1 1 d . . . . .
O2 O 0.6714(2) 0.22891(19) 0.1182(3) 0.0451(13) Uani 1 1 d . . . . .
H2A H 0.6870 0.2613 0.1170 0.068 Uiso 1 1 calc R U . . .
O3 O 0.2322(2) 0.1791(2) 0.1129(4) 0.0549(15) Uani 1 1 d . . . . .
F1 F 0.43630(17) 0.30146(15) 0.2084(3) 0.0494(11) Uani 1 1 d . . . . .
F2 F 0.44813(17) 0.22305(17) 0.0985(3) 0.0449(11) Uani 1 1 d . . . . .
F3 F 0.41238(17) 0.20369(16) 0.2549(3) 0.0465(11) Uani 1 1 d . . . . .
F4 F 0.50755(15) 0.17282(13) 0.2100(3) 0.0337(8) Uani 1 1 d . . . . .
F5 F 0.4958(2) 0.25087(15) 0.3193(3) 0.0476(11) Uani 1 1 d . . . . .
F6 F 0.53105(17) 0.27002(16) 0.1637(3) 0.0399(10) Uani 1 1 d . . . . .
Fe Fe 0.5000 0.0000 0.06002(9) 0.0159(2) Uani 1 2 d S T P . .
As As 0.47192(3) 0.23700(3) 0.20885(5) 0.02768(17) 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 N1 1.317(7) . ?
C1 C2 1.388(8) . ?
C2 C3 1.361(8) . ?
C3 N2 1.369(7) . ?
C4 N3 1.339(7) . ?
C4 C5 1.375(7) . ?
C4 N2 1.398(7) . ?
C5 C6 1.381(7) . ?
C6 C7 1.393(7) . ?
C6 C12 1.499(7) . ?
C7 C8 1.372(7) . ?
C8 N3 1.338(7) . ?
C8 N4 1.406(7) . ?
C9 N4 1.353(7) . ?
C9 C10 1.372(8) . ?
C10 C11 1.382(8) . ?
C11 N5 1.327(7) . ?
C12 O1 1.197(6) . ?
C12 O2 1.316(7) . ?
C13 C14 1.502(12) . ?
C14 O3 1.223(9) . ?
C14 C15 1.478(11) . ?
N1 N2 1.375(6) . ?
N1 Fe 1.977(5) . ?
N3 Fe 1.892(4) . ?
N4 N5 1.377(6) . ?
N5 Fe 1.975(5) . ?
F1 As 1.720(3) . ?
F2 As 1.713(4) . ?
F3 As 1.725(4) . ?
F4 As 1.714(3) . ?
F5 As 1.715(4) . ?
F6 As 1.710(4) . ?
Fe N3 1.892(4) 2_655 ?
Fe N5 1.975(5) 2_655 ?
Fe N1 1.977(5) 2_655 ?

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 C1 C2 111.4(5) . . ?
C3 C2 C1 106.6(5) . . ?
C2 C3 N2 106.1(5) . . ?
N3 C4 C5 122.8(5) . . ?
N3 C4 N2 110.7(4) . . ?
C5 C4 N2 126.5(5) . . ?
C4 C5 C6 116.8(5) . . ?
C5 C6 C7 121.7(5) . . ?
C5 C6 C12 117.1(5) . . ?
C7 C6 C12 121.3(5) . . ?
C8 C7 C6 116.8(5) . . ?
N3 C8 C7 122.7(5) . . ?
N3 C8 N4 109.9(5) . . ?
C7 C8 N4 127.4(5) . . ?
N4 C9 C10 106.2(5) . . ?
C9 C10 C11 106.4(5) . . ?
N5 C11 C10 111.4(5) . . ?
O1 C12 O2 124.8(5) . . ?
O1 C12 C6 123.7(5) . . ?
O2 C12 C6 111.4(5) . . ?
O3 C14 C15 118.8(8) . . ?
O3 C14 C13 122.1(8) . . ?
C15 C14 C13 119.1(8) . . ?
C1 N1 N2 105.1(5) . . ?
C1 N1 Fe 142.1(4) . . ?
N2 N1 Fe 112.1(3) . . ?
C3 N2 N1 110.8(5) . . ?
C3 N2 C4 132.0(5) . . ?
N1 N2 C4 116.9(4) . . ?
C8 N3 C4 119.2(4) . . ?
C8 N3 Fe 120.8(4) . . ?
C4 N3 Fe 120.1(4) . . ?
C9 N4 N5 111.4(4) . . ?
C9 N4 C8 131.9(5) . . ?
N5 N4 C8 116.7(4) . . ?
C11 N5 N4 104.6(4) . . ?
C11 N5 Fe 142.4(4) . . ?
N4 N5 Fe 112.1(3) . . ?
N3 Fe N3 176.9(3) 2_655 . ?
N3 Fe N5 102.26(19) 2_655 . ?
N3 Fe N5 79.88(18) . . ?
N3 Fe N5 79.87(18) 2_655 2_655 ?
N3 Fe N5 102.27(19) . 2_655 ?
N5 Fe N5 94.2(3) . 2_655 ?
N3 Fe N1 80.23(18) 2_655 2_655 ?
N3 Fe N1 97.69(18) . 2_655 ?
N5 Fe N1 88.22(18) . 2_655 ?
N5 Fe N1 160.01(18) 2_655 2_655 ?
N3 Fe N1 97.69(18) 2_655 . ?
N3 Fe N1 80.23(18) . . ?
N5 Fe N1 160.02(18) . . ?
N5 Fe N1 88.22(18) 2_655 . ?
N1 Fe N1 96.3(3) 2_655 . ?
F6 As F2 89.8(2) . . ?
F6 As F4 90.35(17) . . ?
F2 As F4 90.01(18) . . ?
F6 As F5 90.2(2) . . ?
F2 As F5 179.9(2) . . ?
F4 As F5 89.89(18) . . ?
F6 As F1 89.68(18) . . ?
F2 As F1 90.4(2) . . ?
F4 As F1 179.6(2) . . ?
F5 As F1 89.7(2) . . ?
F6 As F3 179.8(2) . . ?
F2 As F3 90.5(2) . . ?
F4 As F3 89.61(18) . . ?
F5 As F3 89.6(2) . . ?
F1 As F3 90.36(18) . . ?

_refine_diff_density_max         0.520
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1856811'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 F12 Fe N10 O6 Sb2'
_chemical_formula_weight         1153.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y+1/2, x, z+1/4'
'-y+1/2, -x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1, x+1/2, z+3/4'
'-y+1, -x+1/2, z+3/4'

_cell_length_a                   23.4653(2)
_cell_length_b                   23.4653(2)
_cell_length_c                   14.6485(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8065.8(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    19254
_cell_measurement_theta_min      3.8180
_cell_measurement_theta_max      27.2540

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             4512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.796
_shelx_estimated_absorpt_T_min   0.615
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_T_min  0.57492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            65363
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.279
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4631
_reflns_number_gt                4302
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0322P)²+20.5844P] 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_abs_structure_details 
;
 Flack x determined using 1968 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.030(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4631
_refine_ls_number_parameters     276
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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
C1 C 0.9419(2) 0.9214(2) 0.0839(4) 0.0251(11) Uani 1 1 d . . . . .
H1 H 0.9071 0.9408 0.0956 0.030 Uiso 1 1 calc R U . . .
C2 C 0.9565(3) 0.8687(3) 0.1210(4) 0.0289(13) Uani 1 1 d . . . . .
H2 H 0.9339 0.8463 0.1611 0.035 Uiso 1 1 calc R U . . .
C3 C 1.0097(2) 0.8553(2) 0.0887(5) 0.0228(10) Uani 1 1 d . . . . .
H3 H 1.0311 0.8219 0.1016 0.027 Uiso 1 1 calc R U . . .
C4 C 1.0751(2) 0.9106(2) -0.0155(4) 0.0178(10) Uani 1 1 d . . . . .
C5 C 1.1253(2) 0.8793(2) -0.0141(4) 0.0203(10) Uani 1 1 d . . . . .
H5 H 1.1295 0.8463 0.0228 0.024 Uiso 1 1 calc R U . . .
C6 C 1.1693(2) 0.8990(2) -0.0697(4) 0.0207(11) Uani 1 1 d . . . . .
C7 C 1.1632(2) 0.9464(2) -0.1250(4) 0.0214(11) Uani 1 1 d . . . . .
H7 H 1.1929 0.9588 -0.1644 0.026 Uiso 1 1 calc R U . . .
C8 C 1.1116(2) 0.9747(2) -0.1197(4) 0.0209(11) Uani 1 1 d . . . . .
C9 C 1.1279(3) 1.0605(3) -0.2207(4) 0.0264(12) Uani 1 1 d . . . . .
H9 H 1.1662 1.0554 -0.2400 0.032 Uiso 1 1 calc R U . . .
C10 C 1.0932(3) 1.1049(3) -0.2426(4) 0.0296(13) Uani 1 1 d . . . . .
H10 H 1.1022 1.1367 -0.2800 0.035 Uiso 1 1 calc R U . . .
C11 C 1.0410(3) 1.0939(2) -0.1984(4) 0.0256(12) Uani 1 1 d . . . . .
H11 H 1.0087 1.1183 -0.2011 0.031 Uiso 1 1 calc R U . . .
C12 C 1.2264(2) 0.8696(2) -0.0709(4) 0.0257(12) Uani 1 1 d . . . . .
C13 C 1.2445(4) 1.1961(4) -0.0272(8) 0.069(3) Uani 1 1 d . . . . .
H13A H 1.2724 1.2262 -0.0144 0.104 Uiso 1 1 calc R U . . .
H13B H 1.2532 1.1784 -0.0861 0.104 Uiso 1 1 calc R U . . .
H13C H 1.2462 1.1672 0.0211 0.104 Uiso 1 1 calc R U . . .
C14 C 1.1859(4) 1.2214(4) -0.0303(6) 0.0486(19) Uani 1 1 d . . . . .
C15 C 1.1370(4) 1.1828(4) -0.0485(8) 0.071(3) Uani 1 1 d . . . . .
H15A H 1.1015 1.2049 -0.0484 0.107 Uiso 1 1 calc R U . . .
H15B H 1.1352 1.1535 -0.0010 0.107 Uiso 1 1 calc R U . . .
H15C H 1.1420 1.1647 -0.1082 0.107 Uiso 1 1 calc R U . . .
N1 N 0.98319(19) 0.9410(2) 0.0298(3) 0.0210(9) Uani 1 1 d . . . . .
N2 N 1.02530(19) 0.8995(2) 0.0346(3) 0.0210(9) Uani 1 1 d . . . . .
N3 N 1.06925(19) 0.95824(19) -0.0651(4) 0.0188(9) Uani 1 1 d . . . . .
N5 N 1.09730(19) 1.02481(18) -0.1658(4) 0.0229(9) Uani 1 1 d . . . . .
N6 N 1.04269(19) 1.0457(2) -0.1529(3) 0.0214(10) Uani 1 1 d . . . . .
O1 O 1.22980(19) 0.8304(2) -0.0067(4) 0.0436(13) Uani 1 1 d . . . . .
H1A H 1.2619 0.8146 -0.0089 0.065 Uiso 1 1 calc R U . . .
O2 O 1.26386(17) 0.88225(19) -0.1227(3) 0.0295(9) Uani 1 1 d . . . . .
O3 O 1.1773(2) 1.2719(2) -0.0140(5) 0.0532(15) Uani 1 1 d . . . . .
F1 F 1.16657(13) 0.99246(16) 0.0896(3) 0.0360(8) Uani 1 1 d . . . . .
F2 F 1.27171(16) 0.96558(19) 0.0384(3) 0.0423(10) Uani 1 1 d . . . . .
F3 F 1.25113(17) 1.0067(2) 0.2047(3) 0.0508(12) Uani 1 1 d . . . . .
F4 F 1.30697(16) 1.06888(19) 0.0817(4) 0.0528(12) Uani 1 1 d . . . . .
F5 F 1.20064(19) 1.09674(19) 0.1304(3) 0.0495(11) Uani 1 1 d . . . . .
F6 F 1.2204(2) 1.05489(19) -0.0345(3) 0.0501(11) Uani 1 1 d . . . . .
Fe Fe 1.0000 1.0000 -0.06205(9) 0.0177(2) Uani 1 2 d S T P . .
Sb Sb 1.23652(2) 1.03112(2) 0.08504(3) 0.02979(11) 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 N1 1.335(7) . ?
C1 C2 1.394(8) . ?
C2 C3 1.370(8) . ?
C3 N2 1.357(7) . ?
C4 N3 1.341(7) . ?
C4 C5 1.388(7) . ?
C4 N2 1.404(7) . ?
C5 C6 1.393(8) . ?
C6 C7 1.384(8) . ?
C6 C12 1.509(7) . ?
C7 C8 1.383(8) . ?
C8 N3 1.334(7) . ?
C8 N5 1.397(7) . ?
C9 C10 1.360(8) . ?
C9 N5 1.366(7) . ?
C10 C11 1.409(8) . ?
C11 N6 1.314(7) . ?
C12 O2 1.198(7) . ?
C12 O1 1.318(7) . ?
C13 C14 1.499(13) . ?
C14 O3 1.225(10) . ?
C14 C15 1.485(11) . ?
N1 N2 1.389(6) . ?
N1 Fe 1.970(5) . ?
N3 Fe 1.898(4) . ?
N5 N6 1.385(6) . ?
N6 Fe 1.981(5) . ?
F1 Sb 1.877(3) . ?
F2 Sb 1.874(4) . ?
F3 Sb 1.876(5) . ?
F4 Sb 1.876(4) . ?
F5 Sb 1.876(4) . ?
F6 Sb 1.876(5) . ?
Fe N3 1.898(4) 2_775 ?
Fe N1 1.970(5) 2_775 ?
Fe N6 1.981(5) 2_775 ?

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 C1 C2 111.0(5) . . ?
C3 C2 C1 107.0(5) . . ?
N2 C3 C2 105.9(5) . . ?
N3 C4 C5 122.4(5) . . ?
N3 C4 N2 110.6(5) . . ?
C5 C4 N2 127.0(5) . . ?
C4 C5 C6 116.4(5) . . ?
C7 C6 C5 122.2(5) . . ?
C7 C6 C12 116.8(5) . . ?
C5 C6 C12 120.9(5) . . ?
C8 C7 C6 116.3(5) . . ?
N3 C8 C7 123.1(5) . . ?
N3 C8 N5 110.8(5) . . ?
C7 C8 N5 126.0(5) . . ?
C10 C9 N5 107.1(5) . . ?
C9 C10 C11 105.8(5) . . ?
N6 C11 C10 111.4(5) . . ?
O2 C12 O1 125.5(5) . . ?
O2 C12 C6 123.1(5) . . ?
O1 C12 C6 111.3(5) . . ?
O3 C14 C15 119.8(8) . . ?
O3 C14 C13 121.9(8) . . ?
C15 C14 C13 118.2(8) . . ?
C1 N1 N2 104.2(4) . . ?
C1 N1 Fe 142.5(4) . . ?
N2 N1 Fe 112.6(3) . . ?
C3 N2 N1 111.9(4) . . ?
C3 N2 C4 132.2(5) . . ?
N1 N2 C4 115.9(4) . . ?
C8 N3 C4 119.4(5) . . ?
C8 N3 Fe 120.2(4) . . ?
C4 N3 Fe 120.4(4) . . ?
C9 N5 N6 110.5(5) . . ?
C9 N5 C8 132.4(5) . . ?
N6 N5 C8 117.0(5) . . ?
C11 N6 N5 105.3(5) . . ?
C11 N6 Fe 142.4(4) . . ?
N5 N6 Fe 111.6(3) . . ?
N3 Fe N3 177.3(3) 2_775 . ?
N3 Fe N1 101.97(19) 2_775 . ?
N3 Fe N1 79.9(2) . . ?
N3 Fe N1 79.9(2) 2_775 2_775 ?
N3 Fe N1 101.97(19) . 2_775 ?
N1 Fe N1 93.9(3) . 2_775 ?
N3 Fe N6 80.26(19) 2_775 2_775 ?
N3 Fe N6 97.91(19) . 2_775 ?
N1 Fe N6 88.68(19) . 2_775 ?
N1 Fe N6 160.09(18) 2_775 2_775 ?
N3 Fe N6 97.92(19) 2_775 . ?
N3 Fe N6 80.26(19) . . ?
N1 Fe N6 160.09(18) . . ?
N1 Fe N6 88.68(19) 2_775 . ?
N6 Fe N6 95.6(3) 2_775 . ?
F2 Sb F5 179.3(2) . . ?
F2 Sb F4 89.42(18) . . ?
F5 Sb F4 90.98(19) . . ?
F2 Sb F1 90.08(17) . . ?
F5 Sb F1 89.53(19) . . ?
F4 Sb F1 179.1(2) . . ?
F2 Sb F3 90.5(2) . . ?
F5 Sb F3 90.1(2) . . ?
F4 Sb F3 90.4(2) . . ?
F1 Sb F3 88.8(2) . . ?
F2 Sb F6 89.6(2) . . ?
F5 Sb F6 89.8(2) . . ?
F4 Sb F6 90.7(2) . . ?
F1 Sb F6 90.04(19) . . ?
F3 Sb F6 178.9(2) . . ?

_refine_diff_density_max         0.991
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.087

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1856812'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H24 F6 Fe N10 O11 S2'
_chemical_formula_weight         922.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           ?
_space_group_name_H-M_alt        Pcab
_space_group_name_Hall           ?

_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, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'

_cell_length_a                   14.8997(4)
_cell_length_b                   21.7329(5)
_cell_length_c                   22.2566(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7207.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5158
_cell_measurement_theta_min      3.5760
_cell_measurement_theta_max      25.5850

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_F_000             3744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.640
_shelx_estimated_absorpt_T_min   0.812
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_T_min  0.70907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            30229
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.258
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7672
_reflns_number_gt                5185
_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0291P)²+4.2117P] 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         7672
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.5271(2) 0.19180(14) 0.24458(13) 0.0161(7) Uani 1 1 d . . . . .
H1 H 0.5348 0.2194 0.2773 0.019 Uiso 1 1 calc R U . . .
C2 C 0.5746(2) 0.13670(15) 0.23727(13) 0.0201(8) Uani 1 1 d . . . . .
H2 H 0.6190 0.1203 0.2634 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5443(2) 0.11123(14) 0.18505(13) 0.0165(7) Uani 1 1 d . . . . .
H3 H 0.5635 0.0735 0.1678 0.020 Uiso 1 1 calc R U . . .
C4 C 0.4276(2) 0.14825(14) 0.11101(13) 0.0138(7) Uani 1 1 d . . . . .
C5 C 0.4256(2) 0.10256(14) 0.06787(12) 0.0138(7) Uani 1 1 d . . . . .
H5 H 0.4633 0.0674 0.0705 0.017 Uiso 1 1 calc R U . . .
C6 C 0.3661(2) 0.11036(14) 0.02058(12) 0.0123(7) Uani 1 1 d . . . . .
C7 C 0.3124(2) 0.16248(14) 0.01611(13) 0.0142(7) Uani 1 1 d . . . . .
H7 H 0.2727 0.1682 -0.0168 0.017 Uiso 1 1 calc R U . . .
C8 C 0.3191(2) 0.20543(14) 0.06130(13) 0.0122(7) Uani 1 1 d . . . . .
C9 C 0.2085(2) 0.28831(15) 0.03185(14) 0.0203(8) Uani 1 1 d . . . . .
H9 H 0.1850 0.2729 -0.0049 0.024 Uiso 1 1 calc R U . . .
C10 C 0.1855(2) 0.34197(15) 0.05888(14) 0.0230(8) Uani 1 1 d . . . . .
H10 H 0.1430 0.3714 0.0452 0.028 Uiso 1 1 calc R U . . .
C11 C 0.2380(2) 0.34493(14) 0.11168(14) 0.0194(8) Uani 1 1 d . . . . .
H11 H 0.2362 0.3779 0.1397 0.023 Uiso 1 1 calc R U . . .
C12 C 0.3603(2) 0.06011(14) -0.02544(13) 0.0146(7) Uani 1 1 d . . . . .
C13 C 0.2298(2) 0.18058(14) 0.23048(13) 0.0171(7) Uani 1 1 d . . . . .
H13 H 0.2207 0.1488 0.2018 0.020 Uiso 1 1 calc R U . . .
C14 C 0.1826(2) 0.18561(14) 0.28478(13) 0.0182(7) Uani 1 1 d . . . . .
H14 H 0.1367 0.1590 0.2991 0.022 Uiso 1 1 calc R U . . .
C15 C 0.2160(2) 0.23651(14) 0.31266(13) 0.0151(7) Uani 1 1 d . . . . .
H15 H 0.1980 0.2522 0.3506 0.018 Uiso 1 1 calc R U . . .
C16 C 0.3390(2) 0.31004(13) 0.28197(13) 0.0134(7) Uani 1 1 d . . . . .
C17 C 0.3479(2) 0.34809(13) 0.33137(13) 0.0131(7) Uani 1 1 d . . . . .
H17 H 0.3113 0.3433 0.3660 0.016 Uiso 1 1 calc R U . . .
C18 C 0.4131(2) 0.39381(14) 0.32776(13) 0.0138(7) Uani 1 1 d . . . . .
C19 C 0.4662(2) 0.40088(14) 0.27691(12) 0.0138(7) Uani 1 1 d . . . . .
H19 H 0.5107 0.4321 0.2744 0.017 Uiso 1 1 calc R U . . .
C20 C 0.4512(2) 0.36070(13) 0.23054(12) 0.0122(7) Uani 1 1 d . . . . .
C21 C 0.5636(2) 0.39386(14) 0.15126(13) 0.0173(7) Uani 1 1 d . . . . .
H21 H 0.5899 0.4293 0.1689 0.021 Uiso 1 1 calc R U . . .
C22 C 0.5850(2) 0.36891(14) 0.09714(13) 0.0184(8) Uani 1 1 d . . . . .
H22 H 0.6286 0.3835 0.0695 0.022 Uiso 1 1 calc R U . . .
C23 C 0.5294(2) 0.31722(14) 0.09040(13) 0.0166(7) Uani 1 1 d . . . . .
H23 H 0.5301 0.2905 0.0566 0.020 Uiso 1 1 calc R U . . .
C24 C 0.4295(2) 0.43843(14) 0.37815(13) 0.0165(7) Uani 1 1 d . . . . .
C25 C 0.4515(3) 0.18413(16) 0.41317(14) 0.0230(8) Uani 1 1 d . . . . .
C26 C 0.3410(3) 0.53737(17) 0.21150(18) 0.0311(9) Uani 1 1 d . . . . .
C27 C 0.6442(3) 0.0547(2) 0.3989(2) 0.0550(13) Uani 1 1 d . . . . .
H27A H 0.6721 0.0321 0.3657 0.082 Uiso 1 1 calc R U . . .
H27B H 0.6693 0.0963 0.4008 0.082 Uiso 1 1 calc R U . . .
H27C H 0.5793 0.0572 0.3923 0.082 Uiso 1 1 calc R U . . .
C28 C 0.6623(3) 0.0218(2) 0.4568(2) 0.0493(13) Uani 1 1 d . . . . .
C29 C 0.6245(4) 0.0500(3) 0.5124(2) 0.0839(19) Uani 1 1 d . . . . .
H29A H 0.6398 0.0244 0.5471 0.126 Uiso 1 1 calc R U . . .
H29B H 0.5590 0.0528 0.5088 0.126 Uiso 1 1 calc R U . . .
H29C H 0.6496 0.0913 0.5178 0.126 Uiso 1 1 calc R U . . .
N1 N 0.47011(18) 0.20027(11) 0.19980(10) 0.0133(6) Uani 1 1 d . . . . .
N2 N 0.48134(18) 0.15004(11) 0.16238(10) 0.0130(6) Uani 1 1 d . . . . .
N3 N 0.37541(18) 0.19828(11) 0.10800(10) 0.0119(6) Uani 1 1 d . . . . .
N4 N 0.27123(18) 0.26071(11) 0.06682(10) 0.0129(6) Uani 1 1 d . . . . .
N5 N 0.29004(18) 0.29598(11) 0.11697(10) 0.0130(6) Uani 1 1 d . . . . .
N6 N 0.28857(18) 0.22559(11) 0.22439(10) 0.0131(6) Uani 1 1 d . . . . .
N7 N 0.28010(18) 0.26060(11) 0.27588(10) 0.0131(6) Uani 1 1 d . . . . .
N8 N 0.38957(18) 0.31621(11) 0.23268(10) 0.0116(6) Uani 1 1 d . . . . .
N9 N 0.49767(18) 0.35862(11) 0.17545(10) 0.0132(6) Uani 1 1 d . . . . .
N10 N 0.47608(18) 0.31074(11) 0.13743(10) 0.0141(6) Uani 1 1 d . . . . .
O1 O 0.38707(16) 0.00810(9) -0.01619(8) 0.0169(5) Uani 1 1 d . . . . .
O2 O 0.32472(17) 0.07901(9) -0.07601(9) 0.0223(6) Uani 1 1 d . . . . .
H2A H 0.3226 0.0496 -0.1005 0.034 Uiso 1 1 calc R U . . .
O3 O 0.48553(16) 0.47783(10) 0.37530(9) 0.0230(6) Uani 1 1 d . . . . .
O4 O 0.37421(17) 0.42947(10) 0.42424(9) 0.0246(6) Uani 1 1 d . . . . .
H4 H 0.3855 0.4552 0.4514 0.037 Uiso 1 1 calc R U . . .
O5 O 0.61274(16) 0.21660(10) 0.44042(10) 0.0250(6) Uani 1 1 d . . . . .
O6 O 0.52671(16) 0.28027(10) 0.37149(9) 0.0244(6) Uani 1 1 d . . . . .
O7 O 0.48770(17) 0.27785(10) 0.47788(9) 0.0247(6) Uani 1 1 d . . . . .
O8 O 0.21040(17) 0.48914(10) 0.15212(9) 0.0241(6) Uani 1 1 d . . . . .
O9 O 0.25744(16) 0.43887(10) 0.24283(9) 0.0229(6) Uani 1 1 d . . . . .
O10 O 0.17719(16) 0.53648(10) 0.24780(10) 0.0264(6) Uani 1 1 d . . . . .
O11 O 0.7033(2) -0.02525(13) 0.45793(17) 0.0718(11) Uani 1 1 d . . . . .
F1 F 0.44245(17) 0.14677(9) 0.46049(8) 0.0383(6) Uani 1 1 d . . . . .
F2 F 0.47901(15) 0.14915(9) 0.36738(8) 0.0323(5) Uani 1 1 d . . . . .
F3 F 0.36941(15) 0.20487(10) 0.39977(10) 0.0402(6) Uani 1 1 d . . . . .
F4 F 0.40345(15) 0.50404(10) 0.18307(11) 0.0478(7) Uani 1 1 d . . . . .
F5 F 0.37140(17) 0.54942(12) 0.26593(12) 0.0601(8) Uani 1 1 d . . . . .
F6 F 0.33174(16) 0.58972(9) 0.18172(11) 0.0496(7) Uani 1 1 d . . . . .
S1 S 0.52884(6) 0.24710(4) 0.42751(3) 0.01748(19) Uani 1 1 d . . . . .
S2 S 0.23469(6) 0.49594(4) 0.21471(3) 0.01523(19) Uani 1 1 d . . . . .
Fe Fe 0.38058(3) 0.25820(2) 0.16954(2) 0.01186(12) 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 N1 1.322(4) . ?
C1 C2 1.400(4) . ?
C2 C3 1.364(4) . ?
C3 N2 1.358(4) . ?
C4 N3 1.338(4) . ?
C4 C5 1.381(4) . ?
C4 N2 1.397(4) . ?
C5 C6 1.387(4) . ?
C6 C7 1.390(4) . ?
C6 C12 1.500(4) . ?
C7 C8 1.376(4) . ?
C8 N3 1.345(4) . ?
C8 N4 1.402(4) . ?
C9 N4 1.356(4) . ?
C9 C10 1.356(4) . ?
C10 C11 1.414(4) . ?
C11 N5 1.321(4) . ?
C12 O1 1.216(3) . ?
C12 O2 1.310(3) . ?
C13 N6 1.319(4) . ?
C13 C14 1.403(4) . ?
C14 C15 1.363(4) . ?
C15 N7 1.362(4) . ?
C16 N8 1.337(4) . ?
C16 C17 1.382(4) . ?
C16 N7 1.394(4) . ?
C17 C18 1.392(4) . ?
C18 C19 1.389(4) . ?
C18 C24 1.503(4) . ?
C19 C20 1.370(4) . ?
C20 N8 1.335(4) . ?
C20 N9 1.409(4) . ?
C21 N9 1.357(4) . ?
C21 C22 1.359(4) . ?
C22 C23 1.403(4) . ?
C23 N10 1.322(4) . ?
C24 O3 1.197(4) . ?
C24 O4 1.330(4) . ?
C25 F2 1.336(4) . ?
C25 F1 1.337(4) . ?
C25 F3 1.338(4) . ?
C25 S1 1.817(4) . ?
C26 F5 1.319(4) . ?
C26 F6 1.324(4) . ?
C26 F4 1.338(4) . ?
C26 S2 1.824(4) . ?
C27 C28 1.498(6) . ?
C28 O11 1.192(5) . ?
C28 C29 1.492(6) . ?
N1 N2 1.383(3) . ?
N1 Fe 1.954(3) . ?
N3 Fe 1.892(2) . ?
N4 N5 1.383(3) . ?
N5 Fe 1.965(3) . ?
N6 N7 1.381(3) . ?
N6 Fe 1.968(3) . ?
N8 Fe 1.893(2) . ?
N9 N10 1.379(3) . ?
N10 Fe 1.959(3) . ?
O5 S1 1.444(2) . ?
O6 S1 1.441(2) . ?
O7 S1 1.442(2) . ?
O8 S2 1.447(2) . ?
O9 S2 1.430(2) . ?
O10 S2 1.433(2) . ?

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 C1 C2 110.9(3) . . ?
C3 C2 C1 106.2(3) . . ?
N2 C3 C2 107.0(3) . . ?
N3 C4 C5 122.5(3) . . ?
N3 C4 N2 110.6(3) . . ?
C5 C4 N2 127.0(3) . . ?
C4 C5 C6 117.0(3) . . ?
C5 C6 C7 121.5(3) . . ?
C5 C6 C12 117.8(3) . . ?
C7 C6 C12 120.8(3) . . ?
C8 C7 C6 117.3(3) . . ?
N3 C8 C7 122.1(3) . . ?
N3 C8 N4 110.4(2) . . ?
C7 C8 N4 127.5(3) . . ?
N4 C9 C10 107.5(3) . . ?
C9 C10 C11 105.5(3) . . ?
N5 C11 C10 111.2(3) . . ?
O1 C12 O2 124.7(3) . . ?
O1 C12 C6 122.8(3) . . ?
O2 C12 C6 112.4(3) . . ?
N6 C13 C14 111.3(3) . . ?
C15 C14 C13 105.8(3) . . ?
N7 C15 C14 107.1(3) . . ?
N8 C16 C17 122.6(3) . . ?
N8 C16 N7 110.6(2) . . ?
C17 C16 N7 126.8(3) . . ?
C16 C17 C18 116.6(3) . . ?
C19 C18 C17 121.6(3) . . ?
C19 C18 C24 116.4(3) . . ?
C17 C18 C24 122.1(3) . . ?
C20 C19 C18 116.8(3) . . ?
N8 C20 C19 123.2(3) . . ?
N8 C20 N9 110.2(2) . . ?
C19 C20 N9 126.6(3) . . ?
N9 C21 C22 107.2(3) . . ?
C21 C22 C23 106.0(3) . . ?
N10 C23 C22 110.8(3) . . ?
O3 C24 O4 125.3(3) . . ?
O3 C24 C18 122.4(3) . . ?
O4 C24 C18 112.4(3) . . ?
F2 C25 F1 106.7(3) . . ?
F2 C25 F3 107.6(3) . . ?
F1 C25 F3 106.7(3) . . ?
F2 C25 S1 111.6(2) . . ?
F1 C25 S1 112.5(2) . . ?
F3 C25 S1 111.4(2) . . ?
F5 C26 F6 109.0(3) . . ?
F5 C26 F4 107.7(3) . . ?
F6 C26 F4 107.5(3) . . ?
F5 C26 S2 111.1(3) . . ?
F6 C26 S2 110.7(3) . . ?
F4 C26 S2 110.8(3) . . ?
O11 C28 C29 121.9(5) . . ?
O11 C28 C27 121.4(5) . . ?
C29 C28 C27 116.7(4) . . ?
C1 N1 N2 105.4(2) . . ?
C1 N1 Fe 142.0(2) . . ?
N2 N1 Fe 112.55(18) . . ?
C3 N2 N1 110.5(2) . . ?
C3 N2 C4 133.0(3) . . ?
N1 N2 C4 116.5(2) . . ?
C4 N3 C8 119.7(3) . . ?
C4 N3 Fe 120.0(2) . . ?
C8 N3 Fe 120.4(2) . . ?
C9 N4 N5 111.0(2) . . ?
C9 N4 C8 132.8(3) . . ?
N5 N4 C8 116.3(2) . . ?
C11 N5 N4 104.8(2) . . ?
C11 N5 Fe 142.4(2) . . ?
N4 N5 Fe 112.83(18) . . ?
C13 N6 N7 105.2(2) . . ?
C13 N6 Fe 142.4(2) . . ?
N7 N6 Fe 112.33(18) . . ?
C15 N7 N6 110.5(2) . . ?
C15 N7 C16 132.8(3) . . ?
N6 N7 C16 116.6(2) . . ?
C20 N8 C16 119.3(2) . . ?
C20 N8 Fe 120.3(2) . . ?
C16 N8 Fe 120.2(2) . . ?
C21 N9 N10 110.6(2) . . ?
C21 N9 C20 133.1(3) . . ?
N10 N9 C20 116.3(2) . . ?
C23 N10 N9 105.4(2) . . ?
C23 N10 Fe 142.0(2) . . ?
N9 N10 Fe 112.66(18) . . ?
O6 S1 O7 115.57(14) . . ?
O6 S1 O5 114.90(14) . . ?
O7 S1 O5 115.22(14) . . ?
O6 S1 C25 102.18(14) . . ?
O7 S1 C25 102.48(15) . . ?
O5 S1 C25 103.77(15) . . ?
O9 S2 O10 116.76(14) . . ?
O9 S2 O8 113.07(13) . . ?
O10 S2 O8 114.09(14) . . ?
O9 S2 C26 103.85(16) . . ?
O10 S2 C26 103.66(16) . . ?
O8 S2 C26 103.29(16) . . ?
N3 Fe N8 177.61(11) . . ?
N3 Fe N1 80.43(10) . . ?
N8 Fe N1 97.17(10) . . ?
N3 Fe N10 99.60(10) . . ?
N8 Fe N10 80.28(10) . . ?
N1 Fe N10 90.31(11) . . ?
N3 Fe N5 80.13(10) . . ?
N8 Fe N5 102.26(10) . . ?
N1 Fe N5 160.55(10) . . ?
N10 Fe N5 92.17(10) . . ?
N3 Fe N6 99.96(10) . . ?
N8 Fe N6 80.13(10) . . ?
N1 Fe N6 91.71(10) . . ?
N10 Fe N6 160.41(10) . . ?
N5 Fe N6 92.39(11) . . ?

_refine_diff_density_max         0.458
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1856807'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H24 As2 F12 Fe N10 O5'
_chemical_formula_weight         1002.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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, y, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, -x, z+3/4'
'-y, x+1/2, z+1/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'-x+1, -y+1, z+1'
'x+1, -y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, -x+1/2, z+5/4'
'-y+1/2, x+1, z+3/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   23.4197(9)
_cell_length_b                   23.4197(9)
_cell_length_c                   14.6422(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8031.0(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    4045
_cell_measurement_theta_min      3.8180
_cell_measurement_theta_max      18.4380

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.65
_exptl_crystal_F_000             3968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.115
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.920
_exptl_absorpt_correction_T_min  0.44802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      300.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            21855
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.282
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4345
_reflns_number_gt                2221
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_max     0.909
_reflns_Friedel_fraction_full    0.999

_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.0920P)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_abs_structure_details 
;
 Flack x determined using 781 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4345
_refine_ls_number_parameters     330
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1421
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.962
_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 0.9541(6) 0.9078(6) 0.0364(10) 0.085(4) Uani 1 1 d . . . . .
H1 H 0.9845 0.8824 0.0337 0.102 Uiso 1 1 calc R U . . .
C2 C 0.9013(7) 0.8987(6) -0.0070(11) 0.099(5) Uani 1 1 d . . . . .
H2 H 0.8906 0.8673 -0.0421 0.119 Uiso 1 1 calc R U . . .
C3 C 0.8701(6) 0.9440(6) 0.0125(10) 0.083(4) Uani 1 1 d . . . . .
H3 H 0.8330 0.9507 -0.0075 0.100 Uiso 1 1 calc R U . . .
C4 C 0.8884(5) 1.0296(5) 0.1146(8) 0.062(3) Uani 1 1 d . . . . .
C5 C 0.8390(5) 1.0593(5) 0.1093(8) 0.066(3) Uani 1 1 d . . . . .
H5 H 0.8099 1.0482 0.0700 0.080 Uiso 1 1 calc R U . . .
C6 C 0.8334(4) 1.1070(5) 0.1644(9) 0.068(3) Uani 1 1 d . . . . .
C7 C 0.8774(5) 1.1247(5) 0.2185(9) 0.070(3) Uani 1 1 d . . . . .
H7 H 0.8743 1.1577 0.2536 0.085 Uiso 1 1 calc R U . . .
C8 C 0.9268(4) 1.0923(5) 0.2196(8) 0.058(3) Uani 1 1 d . . . . .
C9 C 0.9936(6) 1.1437(6) 0.3269(11) 0.086(4) Uani 1 1 d . . . . .
H9 H 0.9734 1.1767 0.3412 0.103 Uiso 1 1 calc R U . . .
C10 C 1.0454(6) 1.1284(7) 0.3583(11) 0.099(5) Uani 1 1 d . . . . .
H10 H 1.0677 1.1496 0.3984 0.119 Uiso 1 1 calc R U . . .
C11 C 1.0600(5) 1.0763(7) 0.3215(11) 0.085(4) Uani 1 1 d . . . . .
H11 H 1.0934 1.0562 0.3335 0.102 Uiso 1 1 calc R U . . .
C12 C 0.7773(6) 1.1374(7) 0.1632(13) 0.100(5) Uani 1 1 d . . . . .
C13 C 0.6340(16) 0.3151(15) 0.184(3) 0.154(15) Uani 0.5 1 d . . P . .
H13A H 0.5996 0.2930 0.1892 0.230 Uiso 0.5 1 calc R U P . .
H13B H 0.6372 0.3294 0.1225 0.230 Uiso 0.5 1 calc R U P . .
H13C H 0.6327 0.3465 0.2258 0.230 Uiso 0.5 1 calc R U P . .
C14 C 0.6820(16) 0.280(2) 0.204(2) 0.106(12) Uani 0.5 1 d . . P . .
C15 C 0.739(3) 0.306(2) 0.190(5) 0.22(3) Uani 0.5 1 d . . P . .
H15A H 0.7677 0.2783 0.2041 0.324 Uiso 0.5 1 calc R U P . .
H15B H 0.7426 0.3384 0.2288 0.324 Uiso 0.5 1 calc R U P . .
H15C H 0.7424 0.3174 0.1272 0.324 Uiso 0.5 1 calc R U P . .
As As 0.46994(9) 0.23809(7) 0.06778(12) 0.0940(6) Uani 1 1 d . . . . .
F1 F 0.424(2) 0.1973(15) 0.131(2) 0.134(14) Uani 0.5 1 d . . P A 1
F2 F 0.4458(19) 0.205(2) -0.026(3) 0.18(2) Uani 0.5 1 d . . P A 1
F3 F 0.4986(18) 0.1776(15) 0.080(4) 0.146(18) Uani 0.5 1 d . . P A 1
F4 F 0.522(2) 0.2723(13) 0.011(4) 0.24(3) Uani 0.5 1 d . . P A 1
F5 F 0.418(3) 0.288(2) 0.054(5) 0.21(3) Uani 0.5 1 d . . P A 1
F6 F 0.485(2) 0.263(2) 0.163(2) 0.20(2) Uani 0.5 1 d . . P A 1
F7 F 0.497(2) 0.2523(14) 0.183(3) 0.151(18) Uani 0.5 1 d . . P A 2
F8 F 0.444(2) 0.3030(17) 0.066(3) 0.120(12) Uani 0.5 1 d . . P A 2
F9 F 0.5293(13) 0.2663(14) 0.027(2) 0.138(15) Uani 0.5 1 d . . P A 2
F10 F 0.454(2) 0.228(2) -0.041(2) 0.142(18) Uani 0.5 1 d . . P A 2
F11 F 0.5199(17) 0.1801(17) 0.070(2) 0.108(12) Uani 0.5 1 d . . P A 2
F12 F 0.4090(16) 0.209(2) 0.098(3) 0.142(13) Uani 0.5 1 d . . P A 2
Fe Fe 1.0000 1.0000 0.1725(2) 0.0536(5) Uani 1 2 d S T P . .
N1 N 0.9554(4) 0.9563(4) 0.0812(7) 0.066(3) Uani 1 1 d . . . . .
N2 N 0.9015(4) 0.9796(4) 0.0671(7) 0.068(2) Uani 1 1 d . . . . .
N3 N 0.9316(3) 1.0449(3) 0.1685(7) 0.053(2) Uani 1 1 d . . . . .
N4 N 0.9769(4) 1.1009(4) 0.2699(7) 0.064(2) Uani 1 1 d . . . . .
N5 N 1.0184(4) 1.0594(4) 0.2659(7) 0.065(2) Uani 1 1 d . . . . .
O1 O 0.7776(5) 1.1803(6) 0.2173(12) 0.162(6) Uani 1 1 d . . . . .
H1A H 0.7464 1.1962 0.2157 0.242 Uiso 1 1 calc R U . . .
O2 O 0.7379(5) 1.1233(5) 0.1185(9) 0.118(4) Uani 1 1 d . . . . .
O3 O 0.6799(9) 0.2330(11) 0.218(2) 0.131(10) Uani 0.5 1 d . . 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 N1 1.311(15) . ?
C1 C2 1.406(18) . ?
C2 C3 1.321(17) . ?
C3 N2 1.369(16) . ?
C4 N3 1.332(14) . ?
C4 C5 1.353(14) . ?
C4 N2 1.395(14) . ?
C5 C6 1.385(15) . ?
C6 C7 1.364(16) . ?
C6 C12 1.494(16) . ?
C7 C8 1.384(15) . ?
C8 N3 1.343(14) . ?
C8 N4 1.401(14) . ?
C9 C10 1.35(2) . ?
C9 N4 1.363(16) . ?
C10 C11 1.378(19) . ?
C11 N5 1.330(16) . ?
C12 O2 1.179(17) . ?
C12 O1 1.279(18) . ?
C13 C14 1.42(4) . ?
C14 O3 1.12(5) . ?
C14 C15 1.47(6) . ?
As F6 1.55(4) . ?
As F3 1.58(4) . ?
As F12 1.64(4) . ?
As F8 1.64(5) . ?
As F9 1.65(3) . ?
As F10 1.65(3) . ?
As F2 1.68(4) . ?
As F4 1.68(3) . ?
As F5 1.70(6) . ?
As F1 1.71(4) . ?
As F11 1.79(4) . ?
As F7 1.83(4) . ?
Fe N3 1.917(8) . ?
Fe N3 1.917(8) 11_664 ?
Fe N1 1.982(10) 11_664 ?
Fe N1 1.982(10) . ?
Fe N5 1.997(10) 11_664 ?
Fe N5 1.997(10) . ?
N1 N2 1.391(12) . ?
N4 N5 1.376(12) . ?

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 C1 C2 112.3(12) . . ?
C3 C2 C1 105.4(12) . . ?
C2 C3 N2 108.6(12) . . ?
N3 C4 C5 122.9(11) . . ?
N3 C4 N2 110.9(9) . . ?
C5 C4 N2 126.2(11) . . ?
C4 C5 C6 117.6(11) . . ?
C7 C6 C5 120.8(9) . . ?
C7 C6 C12 121.8(12) . . ?
C5 C6 C12 117.4(12) . . ?
C6 C7 C8 118.1(11) . . ?
N3 C8 C7 121.2(10) . . ?
N3 C8 N4 110.0(9) . . ?
C7 C8 N4 128.9(11) . . ?
C10 C9 N4 105.7(12) . . ?
C9 C10 C11 109.1(13) . . ?
N5 C11 C10 108.7(12) . . ?
O2 C12 O1 124.6(13) . . ?
O2 C12 C6 124.2(15) . . ?
O1 C12 C6 111.2(14) . . ?
O3 C14 C13 125(4) . . ?
O3 C14 C15 118(3) . . ?
C13 C14 C15 116(4) . . ?
F6 As F3 98(3) . . ?
F12 As F8 94(2) . . ?
F12 As F9 174.3(17) . . ?
F8 As F9 86.1(18) . . ?
F12 As F10 90(2) . . ?
F8 As F10 92(2) . . ?
F9 As F10 84(2) . . ?
F6 As F2 171(3) . . ?
F3 As F2 80(3) . . ?
F6 As F4 95(3) . . ?
F3 As F4 100(2) . . ?
F2 As F4 94(3) . . ?
F6 As F5 90(3) . . ?
F3 As F5 160(2) . . ?
F2 As F5 89(3) . . ?
F4 As F5 97(2) . . ?
F6 As F1 83(2) . . ?
F3 As F1 73(2) . . ?
F2 As F1 88(2) . . ?
F4 As F1 172(2) . . ?
F5 As F1 90(2) . . ?
F12 As F11 104.2(19) . . ?
F8 As F11 161(2) . . ?
F9 As F11 76.2(18) . . ?
F10 As F11 93.3(18) . . ?
F12 As F7 97.5(19) . . ?
F8 As F7 89(2) . . ?
F9 As F7 88.1(17) . . ?
F10 As F7 172(2) . . ?
F11 As F7 83.8(19) . . ?
N3 Fe N3 176.5(6) . 11_664 ?
N3 Fe N1 97.8(4) . 11_664 ?
N3 Fe N1 79.8(4) 11_664 11_664 ?
N3 Fe N1 79.8(4) . . ?
N3 Fe N1 97.8(4) 11_664 . ?
N1 Fe N1 95.2(6) 11_664 . ?
N3 Fe N5 102.9(4) . 11_664 ?
N3 Fe N5 79.6(4) 11_664 11_664 ?
N1 Fe N5 159.3(4) 11_664 11_664 ?
N1 Fe N5 89.3(4) . 11_664 ?
N3 Fe N5 79.6(4) . . ?
N3 Fe N5 102.9(4) 11_664 . ?
N1 Fe N5 89.3(4) 11_664 . ?
N1 Fe N5 159.3(4) . . ?
N5 Fe N5 93.5(6) 11_664 . ?
C1 N1 N2 104.2(10) . . ?
C1 N1 Fe 142.9(9) . . ?
N2 N1 Fe 112.0(7) . . ?
C3 N2 N1 109.6(10) . . ?
C3 N2 C4 133.2(11) . . ?
N1 N2 C4 117.0(9) . . ?
C4 N3 C8 119.3(9) . . ?
C4 N3 Fe 120.3(7) . . ?
C8 N3 Fe 120.4(7) . . ?
C9 N4 N5 110.2(10) . . ?
C9 N4 C8 131.9(11) . . ?
N5 N4 C8 117.9(9) . . ?
C11 N5 N4 106.3(10) . . ?
C11 N5 Fe 141.6(9) . . ?
N4 N5 Fe 111.7(7) . . ?

_refine_diff_density_max         0.262
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.059

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 1856814'
_audit_update_record             
;
2018-10-01 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H18 Cl2 Fe N10 O12'
_chemical_formula_weight         765.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.574(3)
_cell_length_b                   16.554(2)
_cell_length_c                   10.8254(15)
_cell_angle_alpha                90
_cell_angle_beta                 104.686(15)
_cell_angle_gamma                90
_cell_volume                     3046.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    400.00(10)
_cell_measurement_reflns_used    2229
_cell_measurement_theta_min      2.9398
_cell_measurement_theta_max      27.6640

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.751
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.04679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      400.00(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_reflns_number            23217
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_av_R_equivalents  0.1780
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.137
_diffrn_reflns_theta_max         27.725
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3513
_reflns_number_gt                1589
_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_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (A. Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'WinGX (L. J. Farrugia, 2012)'
_computing_publication_material  'WinGX (L. J. Farrugia, 2012)'

_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)+(0.1558P)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         3513
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.2628
_refine_ls_wR_factor_gt          0.1936
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_restrained_S_all      0.846
_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 -0.1317(4) 0.2353(4) 0.4163(6) 0.0805(18) Uani 1 1 d . . . . .
H1 H -0.1402 0.2904 0.4227 0.097 Uiso 1 1 calc R U . . .
C2 C -0.1693(4) 0.1752(4) 0.4685(7) 0.092(2) Uani 1 1 d . . . . .
H2 H -0.2067 0.1828 0.5148 0.111 Uiso 1 1 calc R U . . .
C3 C -0.1411(3) 0.1037(4) 0.4390(6) 0.0766(16) Uani 1 1 d . . . . .
H3 H -0.1549 0.0526 0.4616 0.092 Uiso 1 1 calc R U . . .
C4 C -0.0435(3) 0.0708(3) 0.3117(5) 0.0550(12) Uani 1 1 d . . . . .
C5 C -0.0444(3) -0.0124(3) 0.3190(5) 0.0610(13) Uani 1 1 d . . . . .
H5 H -0.0732 -0.0392 0.3676 0.073 Uiso 1 1 calc R U . . .
C6 C 0.0000 -0.0542(4) 0.2500 0.0549(16) Uani 1 2 d S T P . .
C7 C 0.0000 -0.1437(4) 0.2500 0.0636(19) Uani 1 2 d S T P . .
C8 C 0.1428(4) 0.2456(4) 0.5154(6) 0.0774(17) Uani 1 1 d . . . . .
H8 H 0.1527 0.1908 0.5296 0.093 Uiso 1 1 calc R U . . .
C9 C 0.1826(4) 0.3068(4) 0.5944(6) 0.091(2) Uani 1 1 d . . . . .
H9 H 0.2228 0.3004 0.6685 0.109 Uiso 1 1 calc R U . . .
C10 C 0.1517(4) 0.3765(4) 0.5428(5) 0.0839(18) Uani 1 1 d . . . . .
H10 H 0.1662 0.4280 0.5742 0.101 Uiso 1 1 calc R U . . .
C11 C 0.0466(3) 0.4089(3) 0.3450(4) 0.0519(11) Uani 1 1 d . . . . .
C12 C 0.0470(3) 0.4909(3) 0.3516(5) 0.0579(12) Uani 1 1 d . . . . .
H12 H 0.0779 0.5179 0.4220 0.070 Uiso 1 1 calc R U . . .
C13 C 0.0000 0.5329(4) 0.2500 0.0556(17) Uani 1 2 d S T P . .
C14 C 0.0000 0.6243(4) 0.2500 0.0602(18) Uani 1 2 d S T P . .
N1 N -0.0819(3) 0.2031(3) 0.3560(4) 0.0653(11) Uani 1 1 d . . . . .
N2 N -0.0887(2) 0.1214(2) 0.3698(4) 0.0618(11) Uani 1 1 d . . . . .
N3 N 0.0000 0.1116(3) 0.2500 0.0526(13) Uani 1 2 d S T P . .
N4 N 0.0892(3) 0.2755(3) 0.4181(4) 0.0660(12) Uani 1 1 d . . . . .
N5 N 0.0951(2) 0.3579(2) 0.4358(4) 0.0558(10) Uani 1 1 d . . . . .
N6 N 0.0000 0.3677(3) 0.2500 0.0492(12) Uani 1 2 d S T P . .
O1 O -0.0167(3) -0.1793(2) 0.3426(4) 0.0851(12) Uani 1 1 d . . . . .
H1A H -0.0149 -0.2283 0.3326 0.128 Uiso 0.5 1 calc R U P . .
O2 O 0.0136(3) 0.6586(2) 0.3552(4) 0.0955(14) Uani 1 1 d . . . . .
H2A H 0.0122 0.7077 0.3446 0.143 Uiso 0.5 1 calc R U P . .
Fe1 Fe 0.0000 0.24023(5) 0.2500 0.0581(4) Uani 1 2 d S T P . .
Cl1 Cl 0.26202(11) 0.06589(13) 0.77266(19) 0.0961(6) Uani 1 1 d . . . . .
O3 O 0.2178(14) 0.0213(19) 0.836(2) 0.166(11) Uani 0.5 1 d . . P A 1
O4 O 0.3396(8) 0.0706(14) 0.834(2) 0.117(7) Uani 0.5 1 d . . P A 1
O5 O 0.2243(11) 0.1424(11) 0.7855(14) 0.130(6) Uani 0.5 1 d . . P A 1
O6 O 0.2449(16) 0.0569(13) 0.6396(16) 0.158(9) Uani 0.5 1 d . . P A 1
O7 O 0.2194(10) 0.0020(14) 0.8138(19) 0.130(9) Uani 0.5 1 d . . P A 2
O8 O 0.3323(14) 0.0735(15) 0.868(2) 0.186(12) Uani 0.5 1 d . . P A 2
O9 O 0.2817(14) 0.0085(15) 0.683(2) 0.192(11) Uani 0.5 1 d . . P A 2
O10 O 0.235(2) 0.127(2) 0.717(3) 0.316(19) Uani 0.5 1 d . . P A 2


_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 N1 1.328(7) . ?
C1 C2 1.391(9) . ?
C2 C3 1.353(8) . ?
C3 N2 1.359(7) . ?
C4 N3 1.322(5) . ?
C4 C5 1.380(7) . ?
C4 N2 1.407(6) . ?
C5 C6 1.394(6) . ?
C6 C5 1.394(6) 2 ?
C6 C7 1.482(9) . ?
C7 O1 1.259(5) 2 ?
C7 O1 1.259(5) . ?
C8 N4 1.318(7) . ?
C8 C9 1.395(9) . ?
C9 C10 1.335(9) . ?
C10 N5 1.357(7) . ?
C11 N6 1.329(5) . ?
C11 C12 1.358(7) . ?
C11 N5 1.408(6) . ?
C12 C13 1.384(6) . ?
C13 C12 1.384(6) 2 ?
C13 C14 1.512(9) . ?
C14 O2 1.241(5) 2 ?
C14 O2 1.241(5) . ?
N1 N2 1.370(6) . ?
N1 Fe1 2.146(4) . ?
N3 C4 1.322(5) 2 ?
N3 Fe1 2.129(5) . ?
N4 N5 1.378(6) . ?
N4 Fe1 2.159(5) . ?
N6 C11 1.329(5) 2 ?
N6 Fe1 2.110(5) . ?
Fe1 N1 2.146(4) 2 ?
Fe1 N4 2.159(5) 2 ?
Cl1 O10 1.21(2) . ?
Cl1 O4 1.359(16) . ?
Cl1 O3 1.38(2) . ?
Cl1 O8 1.40(2) . ?
Cl1 O6 1.403(17) . ?
Cl1 O9 1.46(2) . ?
Cl1 O5 1.453(13) . ?
Cl1 O7 1.431(19) . ?

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 C1 C2 110.7(5) . . ?
C3 C2 C1 106.8(6) . . ?
C2 C3 N2 106.3(6) . . ?
N3 C4 C5 123.7(5) . . ?
N3 C4 N2 112.7(4) . . ?
C5 C4 N2 123.5(4) . . ?
C4 C5 C6 116.7(5) . . ?
C5 C6 C5 120.5(6) 2 . ?
C5 C6 C7 119.8(3) 2 . ?
C5 C6 C7 119.8(3) . . ?
O1 C7 O1 124.2(7) 2 . ?
O1 C7 C6 117.9(3) 2 . ?
O1 C7 C6 117.9(3) . . ?
N4 C8 C9 111.3(5) . . ?
C10 C9 C8 106.4(6) . . ?
C9 C10 N5 107.1(6) . . ?
N6 C11 C12 123.2(4) . . ?
N6 C11 N5 112.2(4) . . ?
C12 C11 N5 124.6(4) . . ?
C11 C12 C13 117.8(5) . . ?
C12 C13 C12 119.7(6) 2 . ?
C12 C13 C14 120.2(3) 2 . ?
C12 C13 C14 120.2(3) . . ?
O2 C14 O2 125.5(7) 2 . ?
O2 C14 C13 117.2(3) 2 . ?
O2 C14 C13 117.2(3) . . ?
C1 N1 N2 104.9(4) . . ?
C1 N1 Fe1 139.7(4) . . ?
N2 N1 Fe1 115.4(3) . . ?
N1 N2 C3 111.3(4) . . ?
N1 N2 C4 117.7(4) . . ?
C3 N2 C4 131.0(5) . . ?
C4 N3 C4 118.6(6) . 2 ?
C4 N3 Fe1 120.7(3) . . ?
C4 N3 Fe1 120.7(3) 2 . ?
C8 N4 N5 104.3(5) . . ?
C8 N4 Fe1 142.3(4) . . ?
N5 N4 Fe1 113.4(3) . . ?
C10 N5 N4 110.9(4) . . ?
C10 N5 C11 130.0(5) . . ?
N4 N5 C11 119.1(4) . . ?
C11 N6 C11 118.2(5) . 2 ?
C11 N6 Fe1 120.9(3) . . ?
C11 N6 Fe1 120.9(3) 2 . ?
N6 Fe1 N3 180.0 . . ?
N6 Fe1 N1 106.62(11) . . ?
N3 Fe1 N1 73.38(11) . . ?
N6 Fe1 N1 106.62(11) . 2 ?
N3 Fe1 N1 73.38(11) . 2 ?
N1 Fe1 N1 146.8(2) . 2 ?
N6 Fe1 N4 74.33(12) . . ?
N3 Fe1 N4 105.67(12) . . ?
N1 Fe1 N4 93.94(16) . . ?
N1 Fe1 N4 94.93(17) 2 . ?
N6 Fe1 N4 74.32(12) . 2 ?
N3 Fe1 N4 105.68(12) . 2 ?
N1 Fe1 N4 94.93(17) . 2 ?
N1 Fe1 N4 93.94(16) 2 2 ?
N4 Fe1 N4 148.6(2) . 2 ?
O4 Cl1 O3 114.2(14) . . ?
O10 Cl1 O8 117(2) . . ?
O4 Cl1 O6 115.9(14) . . ?
O3 Cl1 O6 117.0(15) . . ?
O10 Cl1 O9 110.0(18) . . ?
O8 Cl1 O9 103.5(16) . . ?
O4 Cl1 O5 109.1(12) . . ?
O3 Cl1 O5 95.2(15) . . ?
O6 Cl1 O5 101.9(11) . . ?
O10 Cl1 O7 127.3(19) . . ?
O8 Cl1 O7 105.8(12) . . ?
O9 Cl1 O7 87.5(14) . . ?

_refine_diff_density_max         0.441
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_vg77_5
_database_code_depnum_ccdc_archive 'CCDC 1856810'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_audit_creation_date             2018-11-02
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C28 H26 Fe N10 O4), 4(Cl O4), 3(C3 H6 O)'
_chemical_formula_sum            'C65 H70 Cl4 Fe2 N20 O27'
_chemical_formula_weight         1816.91
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4649(3)
_cell_length_b                   21.2806(5)
_cell_length_c                   23.1689(8)
_cell_angle_alpha                110.978(3)
_cell_angle_beta                 95.650(3)
_cell_angle_gamma                91.629(3)
_cell_volume                     3868.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6544
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      25.2460
_cell_measurement_theta_min      3.5250
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.221
_diffrn_reflns_theta_min         3.238
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00  11.00   1.00   12.00    --  -17.68 -68.00-123.09   99
  2  ω    -88.00  11.00   1.00   12.00    --  -17.68 -68.00 -32.90   99
  3  ω    -89.00  11.00   1.00   12.00    --  -17.68 -69.00  85.76  100
  4  ω    -87.00   8.00   1.00   12.00    --  -17.68 -63.00 164.74   95
  5  ω    -51.00  48.00   1.00   12.00    --   20.00 -67.00-138.90   99
  6  ω    -51.00  48.00   1.00   12.00    --   20.00 -68.00  27.26   99
  7  ω    -51.00  48.00   1.00   12.00    --   20.00 -68.00 102.20   99
  8  ω    -51.00  49.00   1.00   12.00    --   20.00 -69.00 -46.77  100
  9  ω    -51.00  26.00   1.00   12.00    --   20.00 -69.00-166.60   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0070554000
_diffrn_orient_matrix_UB_12      -0.0078110000
_diffrn_orient_matrix_UB_13      0.0274079000
_diffrn_orient_matrix_UB_21      0.0808859000
_diffrn_orient_matrix_UB_22      -0.0065336000
_diffrn_orient_matrix_UB_23      -0.0035272000
_diffrn_orient_matrix_UB_31      0.0230471000
_diffrn_orient_matrix_UB_32      0.0343013000
_diffrn_orient_matrix_UB_33      0.0180597000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8370
_reflns_number_total             16847
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         16847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0682
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+2.9907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.2041
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O13(0.5) O14(0.5) O15(0.5) O16(0.5) O17(0.5) O18(0.5) O19(0.5)
 O20(0.5) O21A(0.6) O21B(0.4) O22A(0.6) O22B(0.4) O23A(0.6) O23B(0.4) O24A(0.6)
 O24B(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C27(H27A,H27B), C41(H41A,H41B), C55(H55A,H55B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C24(H24), C25(H25), C29(H29),
  C30(H30), C31(H31), C33(H33), C35(H35), C37(H37), C38(H38), C39(H39),
 C43(H43), C44(H44), C45(H45), C47(H47), C49(H49), C51(H51), C52(H52), C53(H53)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 1.15595(8) 0.75927(3) 0.98556(3) 0.01781(18) Uani 1 1 d . . . . .
O1 O 1.0014(4) 1.08985(16) 1.11899(17) 0.0420(10) Uani 1 1 d . . . . .
O2 O 1.2321(4) 1.08760(15) 1.17564(15) 0.0305(8) Uani 1 1 d . . . . .
O3 O 1.2912(4) 0.43685(14) 0.80300(15) 0.0262(8) Uani 1 1 d . . . . .
O4 O 1.2814(4) 0.43000(14) 0.89782(14) 0.0258(8) Uani 1 1 d . . . . .
N1 N 0.9335(4) 0.76989(17) 0.95777(16) 0.0204(9) Uani 1 1 d . . . . .
N2 N 0.8948(4) 0.83644(17) 0.98119(16) 0.0198(9) Uani 1 1 d . . . . .
N3 N 1.1437(4) 0.85229(17) 1.03038(16) 0.0176(8) Uani 1 1 d . . . . .
N4 N 1.3963(4) 0.84780(17) 1.06959(17) 0.0204(9) Uani 1 1 d . . . . .
N5 N 1.3727(4) 0.78152(16) 1.02831(16) 0.0171(8) Uani 1 1 d . . . . .
N6 N 1.2212(4) 0.76060(17) 0.90673(16) 0.0184(8) Uani 1 1 d . . . . .
N7 N 1.2400(4) 0.69663(17) 0.86523(16) 0.0187(9) Uani 1 1 d . . . . .
N8 N 1.1754(4) 0.66596(17) 0.94357(16) 0.0164(8) Uani 1 1 d . . . . .
N9 N 1.1102(4) 0.65699(17) 1.03261(16) 0.0186(8) Uani 1 1 d . . . . .
N10 N 1.0997(4) 0.72569(17) 1.04999(17) 0.0198(9) Uani 1 1 d . . . . .
C1 C 0.8087(6) 0.7372(2) 0.9183(2) 0.0273(12) Uani 1 1 d . . . . .
H1 H 0.800854 0.691254 0.894983 0.033 Uiso 1 1 calc R . . . .
C2 C 0.6903(6) 0.7809(3) 0.9163(2) 0.0318(12) Uani 1 1 d . . . . .
H2 H 0.591536 0.769490 0.892387 0.038 Uiso 1 1 calc R . . . .
C3 C 0.7477(6) 0.8434(2) 0.9561(2) 0.0263(11) Uani 1 1 d . . . . .
H3 H 0.695990 0.883174 0.964526 0.032 Uiso 1 1 calc R . . . .
C4 C 1.0105(5) 0.8829(2) 1.0237(2) 0.0192(10) Uani 1 1 d . . . . .
C5 C 0.9954(6) 0.9503(2) 1.0550(2) 0.0234(11) Uani 1 1 d . . . . .
H5 H 0.903290 0.970845 1.048652 0.028 Uiso 1 1 calc R . . . .
C6 C 1.1247(6) 0.9863(2) 1.0969(2) 0.0237(11) Uani 1 1 d . . . . .
C7 C 1.2630(6) 0.9555(2) 1.1055(2) 0.0226(11) Uani 1 1 d . . . . .
H7 H 1.348602 0.979468 1.133968 0.027 Uiso 1 1 calc R . . . .
C8 C 1.2685(5) 0.8882(2) 1.0702(2) 0.0190(10) Uani 1 1 d . . . . .
C9 C 1.5448(6) 0.8603(2) 1.0997(2) 0.0257(11) Uani 1 1 d . . . . .
H9 H 1.587699 0.901080 1.129447 0.031 Uiso 1 1 calc R . . . .
C10 C 1.6209(6) 0.8021(2) 1.0784(2) 0.0281(12) Uani 1 1 d . . . . .
H10 H 1.724755 0.795336 1.090893 0.034 Uiso 1 1 calc R . . . .
C11 C 1.5110(5) 0.7545(2) 1.0338(2) 0.0243(11) Uani 1 1 d . . . . .
H11 H 1.531639 0.710292 1.011299 0.029 Uiso 1 1 calc R . . . .
C12 C 1.1095(6) 1.0604(2) 1.1315(2) 0.0267(12) Uani 1 1 d . . . . .
C13 C 1.2257(7) 1.1598(2) 1.2125(2) 0.0386(14) Uani 1 1 d . . . . .
H13A H 1.179186 1.182585 1.186019 0.046 Uiso 1 1 calc R . . . .
H13B H 1.332702 1.179921 1.228868 0.046 Uiso 1 1 calc R . . . .
C14 C 1.1288(7) 1.1687(3) 1.2647(3) 0.0531(17) Uani 1 1 d . . . . .
H14A H 1.020781 1.152165 1.248324 0.080 Uiso 1 1 calc GR . . . .
H14B H 1.131666 1.215662 1.290172 0.080 Uiso 1 1 calc GR . . . .
H14C H 1.171421 1.143894 1.289428 0.080 Uiso 1 1 calc GR . . . .
C15 C 1.2485(5) 0.8016(2) 0.8768(2) 0.0210(10) Uani 1 1 d . . . . .
H15 H 1.242285 0.848109 0.893220 0.025 Uiso 1 1 calc R . . . .
C16 C 1.2881(5) 0.7655(2) 0.8167(2) 0.0230(11) Uani 1 1 d . . . . .
H16 H 1.313752 0.782934 0.787023 0.028 Uiso 1 1 calc R . . . .
C17 C 1.2808(5) 0.6995(2) 0.8112(2) 0.0232(11) Uani 1 1 d . . . . .
H17 H 1.300460 0.662988 0.776537 0.028 Uiso 1 1 calc R . . . .
C18 C 1.2200(5) 0.6433(2) 0.8865(2) 0.0161(10) Uani 1 1 d . . . . .
C19 C 1.2468(5) 0.5762(2) 0.8552(2) 0.0201(10) Uani 1 1 d . . . . .
H19 H 1.273252 0.560774 0.814645 0.024 Uiso 1 1 calc R . . . .
C20 C 1.2316(5) 0.5331(2) 0.8885(2) 0.0177(10) Uani 1 1 d . . . . .
C21 C 1.1870(5) 0.5560(2) 0.9481(2) 0.0186(10) Uani 1 1 d . . . . .
H21 H 1.177435 0.527399 0.970116 0.022 Uiso 1 1 calc R . . . .
C22 C 1.1573(5) 0.6233(2) 0.9732(2) 0.0172(10) Uani 1 1 d . . . . .
C23 C 1.0818(5) 0.6360(2) 1.0802(2) 0.0223(11) Uani 1 1 d . . . . .
H23 H 1.083682 0.592217 1.079813 0.027 Uiso 1 1 calc R . . . .
C24 C 1.0501(6) 0.6923(2) 1.1284(2) 0.0271(12) Uani 1 1 d . . . . .
H24 H 1.025043 0.694172 1.167120 0.032 Uiso 1 1 calc R . . . .
C25 C 1.0625(5) 0.7460(2) 1.1080(2) 0.0201(10) Uani 1 1 d . . . . .
H25 H 1.046893 0.790403 1.131818 0.024 Uiso 1 1 calc R . . . .
C26 C 1.2711(5) 0.4616(2) 0.8573(2) 0.0204(10) Uani 1 1 d . . . . .
C27 C 1.3418(6) 0.3629(2) 0.8782(2) 0.0281(12) Uani 1 1 d . . . . .
H27A H 1.320487 0.341080 0.833372 0.034 Uiso 1 1 calc R . . . .
H27B H 1.288427 0.335514 0.897103 0.034 Uiso 1 1 calc R . . . .
C28 C 1.5176(6) 0.3687(2) 0.8976(2) 0.0332(13) Uani 1 1 d . . . . .
H28A H 1.570347 0.394560 0.877764 0.050 Uiso 1 1 calc GR . . . .
H28B H 1.556809 0.324448 0.885511 0.050 Uiso 1 1 calc GR . . . .
H28C H 1.538298 0.390747 0.941968 0.050 Uiso 1 1 calc GR . . . .
Fe2 Fe 0.67298(8) 0.76607(3) 0.48934(3) 0.01779(18) Uani 1 1 d . . . . .
O5 O 0.8128(4) 0.44552(15) 0.30262(15) 0.0284(8) Uani 1 1 d . . . . .
O6 O 0.7900(4) 0.43518(14) 0.39539(14) 0.0272(8) Uani 1 1 d . . . . .
O7 O 0.4911(5) 1.09354(16) 0.60971(18) 0.0477(11) Uani 1 1 d . . . . .
O8 O 0.7038(5) 1.09514(16) 0.67581(16) 0.0384(10) Uani 1 1 d . . . . .
N11 N 0.6105(4) 0.72967(17) 0.55121(17) 0.0198(9) Uani 1 1 d . . . . .
N12 N 0.6236(4) 0.66074(17) 0.53267(16) 0.0183(8) Uani 1 1 d . . . . .
N13 N 0.6984(4) 0.67328(17) 0.44633(16) 0.0161(8) Uani 1 1 d . . . . .
N14 N 0.7634(4) 0.70622(17) 0.36920(16) 0.0186(8) Uani 1 1 d . . . . .
N15 N 0.7444(4) 0.76993(17) 0.41223(17) 0.0208(9) Uani 1 1 d . . . . .
N16 N 0.8876(4) 0.79293(17) 0.53596(16) 0.0183(8) Uani 1 1 d . . . . .
N17 N 0.9004(5) 0.85874(17) 0.57732(16) 0.0211(9) Uani 1 1 d . . . . .
N18 N 0.6504(4) 0.85863(17) 0.53377(16) 0.0178(8) Uani 1 1 d . . . . .
N19 N 0.4036(4) 0.83720(18) 0.48145(17) 0.0218(9) Uani 1 1 d . . . . .
N20 N 0.4509(4) 0.77265(17) 0.45810(16) 0.0206(9) Uani 1 1 d . . . . .
C29 C 0.5633(5) 0.7477(2) 0.6073(2) 0.0240(11) Uani 1 1 d . . . . .
H29 H 0.544076 0.791672 0.631379 0.029 Uiso 1 1 calc R . . . .
C30 C 0.5460(5) 0.6921(2) 0.6258(2) 0.0239(11) Uani 1 1 d . . . . .
H30 H 0.514652 0.692269 0.663197 0.029 Uiso 1 1 calc R . . . .
C31 C 0.5848(5) 0.6378(2) 0.5775(2) 0.0213(11) Uani 1 1 d . . . . .
H31 H 0.584752 0.593383 0.575624 0.026 Uiso 1 1 calc R . . . .
C32 C 0.6754(5) 0.6288(2) 0.4743(2) 0.0176(10) Uani 1 1 d . . . . .
C33 C 0.7034(5) 0.5618(2) 0.4477(2) 0.0198(10) Uani 1 1 d . . . . .
H33 H 0.691073 0.532004 0.468378 0.024 Uiso 1 1 calc R . . . .
C34 C 0.7509(5) 0.5407(2) 0.3888(2) 0.0171(10) Uani 1 1 d . . . . .
C35 C 0.7696(5) 0.5853(2) 0.3573(2) 0.0185(10) Uani 1 1 d . . . . .
H35 H 0.798408 0.570804 0.317115 0.022 Uiso 1 1 calc R . . . .
C36 C 0.7429(5) 0.6518(2) 0.3894(2) 0.0186(10) Uani 1 1 d . . . . .
C37 C 0.8057(5) 0.7107(2) 0.3156(2) 0.0242(11) Uani 1 1 d . . . . .
H37 H 0.826417 0.675031 0.280366 0.029 Uiso 1 1 calc R . . . .
C38 C 0.8121(6) 0.7775(2) 0.3230(2) 0.0256(11) Uani 1 1 d . . . . .
H38 H 0.836560 0.796157 0.293977 0.031 Uiso 1 1 calc R . . . .
C39 C 0.7745(5) 0.8120(2) 0.3831(2) 0.0217(11) Uani 1 1 d . . . . .
H39 H 0.770853 0.858622 0.400696 0.026 Uiso 1 1 calc R . . . .
C40 C 0.7894(5) 0.4687(2) 0.3563(2) 0.0241(11) Uani 1 1 d . . . . .
C41 C 0.8432(6) 0.3670(2) 0.3749(2) 0.0271(12) Uani 1 1 d . . . . .
H41A H 0.828708 0.347271 0.329851 0.032 Uiso 1 1 calc R . . . .
H41B H 0.780408 0.339330 0.390800 0.032 Uiso 1 1 calc R . . . .
C42 C 1.0156(6) 0.3691(2) 0.3984(3) 0.0356(13) Uani 1 1 d . . . . .
H42A H 1.078267 0.393131 0.379613 0.053 Uiso 1 1 calc GR . . . .
H42B H 1.048344 0.323896 0.387752 0.053 Uiso 1 1 calc GR . . . .
H42C H 1.030498 0.391559 0.442784 0.053 Uiso 1 1 calc GR . . . .
C43 C 1.0282(6) 0.7696(2) 0.5452(2) 0.0246(11) Uani 1 1 d . . . . .
H43 H 1.055327 0.725982 0.523749 0.030 Uiso 1 1 calc R . . . .
C44 C 1.1293(6) 0.8189(2) 0.5912(2) 0.0301(12) Uani 1 1 d . . . . .
H44 H 1.232934 0.814399 0.605970 0.036 Uiso 1 1 calc R . . . .
C45 C 1.0466(6) 0.8747(2) 0.6100(2) 0.0256(11) Uani 1 1 d . . . . .
H45 H 1.083386 0.916300 0.639889 0.031 Uiso 1 1 calc R . . . .
C46 C 0.7687(5) 0.8966(2) 0.5751(2) 0.0193(10) Uani 1 1 d . . . . .
C47 C 0.7571(6) 0.9641(2) 0.6097(2) 0.0225(11) Uani 1 1 d . . . . .
H47 H 0.838479 0.989509 0.639703 0.027 Uiso 1 1 calc R . . . .
C48 C 0.6162(6) 0.9923(2) 0.5971(2) 0.0221(11) Uani 1 1 d . . . . .
C49 C 0.4924(6) 0.9534(2) 0.5542(2) 0.0255(11) Uani 1 1 d . . . . .
H49 H 0.398819 0.972131 0.546081 0.031 Uiso 1 1 calc R . . . .
C50 C 0.5135(5) 0.8860(2) 0.5242(2) 0.0186(10) Uani 1 1 d . . . . .
C51 C 0.2536(6) 0.8410(2) 0.4564(2) 0.0275(12) Uani 1 1 d . . . . .
H51 H 0.196402 0.879361 0.465176 0.033 Uiso 1 1 calc R . . . .
C52 C 0.2030(6) 0.7776(2) 0.4159(2) 0.0298(12) Uani 1 1 d . . . . .
H52 H 0.105399 0.764274 0.391423 0.036 Uiso 1 1 calc R . . . .
C53 C 0.3280(6) 0.7369(2) 0.4188(2) 0.0255(11) Uani 1 1 d . . . . .
H53 H 0.325372 0.690812 0.396175 0.031 Uiso 1 1 calc R . . . .
C54 C 0.5950(7) 1.0656(2) 0.6282(2) 0.0314(13) Uani 1 1 d . . . . .
C55 C 0.6953(7) 1.1671(2) 0.7113(2) 0.0432(15) Uani 1 1 d . . . . .
H55A H 0.652394 1.189195 0.683689 0.052 Uiso 1 1 calc R . . . .
H55B H 0.801402 1.187414 0.729027 0.052 Uiso 1 1 calc R . . . .
C56 C 0.5929(8) 1.1771(3) 0.7618(3) 0.0576(18) Uani 1 1 d . . . . .
H56A H 0.486411 1.159257 0.744071 0.086 Uiso 1 1 calc GR . . . .
H56B H 0.592301 1.224421 0.785670 0.086 Uiso 1 1 calc GR . . . .
H56C H 0.633706 1.154134 0.788412 0.086 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.26411(15) 0.43917(6) 0.07465(6) 0.0300(3) Uani 1 1 d . . . . .
O9 O 0.3995(5) 0.4782(3) 0.1136(3) 0.0950(19) Uani 1 1 d . . . . .
O10 O 0.1768(4) 0.48013(17) 0.04673(17) 0.0412(10) Uani 1 1 d . . . . .
O11 O 0.1652(4) 0.42082(16) 0.11429(16) 0.0375(9) Uani 1 1 d . . . . .
O12 O 0.3024(7) 0.3808(2) 0.0281(2) 0.095(2) Uani 1 1 d . . . . .
Cl2 Cl 0.500000 1.000000 1.000000 0.0343(5) Uani 1 2 d S T P . .
O13 O 0.5529(10) 1.0636(3) 1.0122(4) 0.045(2) Uani 0.5 1 d . . . . .
O14 O 0.5647(8) 0.9675(3) 1.0413(3) 0.0280(16) Uani 0.5 1 d . . . . .
O15 O 0.3267(8) 0.9886(3) 0.9902(3) 0.0367(18) Uani 0.5 1 d . . . . .
O16 O 0.5480(9) 0.9544(3) 0.9352(3) 0.0373(19) Uani 0.5 1 d . . . . .
Cl3 Cl 1.000000 1.000000 0.500000 0.0375(5) Uani 1 2 d S T P . .
O17 O 0.9562(9) 0.9373(3) 0.4960(3) 0.0365(18) Uani 0.5 1 d . . . . .
O18 O 1.0436(8) 0.9515(3) 0.4325(3) 0.0343(18) Uani 0.5 1 d . . . . .
O19 O 1.1732(8) 1.0140(3) 0.5097(3) 0.0304(16) Uani 0.5 1 d . . . . .
O20 O 1.0728(8) 0.9720(3) 0.5402(3) 0.0336(17) Uani 0.5 1 d . . . . .
Cl4 Cl 1.0494(2) 1.07575(8) 0.77643(7) 0.0558(5) Uani 1 1 d . . . . .
O21A O 1.0297(11) 1.0133(4) 0.7332(4) 0.068(2) Uiso 0.6 1 d . . . A 1
O21B O 1.0966(15) 1.0326(6) 0.7192(6) 0.071(4) Uiso 0.4 1 d . . . A 2
O22A O 1.0368(11) 1.1350(4) 0.7614(4) 0.069(3) Uiso 0.6 1 d . . . A 1
O22B O 1.127(2) 1.1342(9) 0.7753(8) 0.116(6) Uiso 0.4 1 d . . . A 2
O23A O 1.1136(10) 1.0866(4) 0.8350(4) 0.053(2) Uiso 0.6 1 d . . . A 1
O23B O 1.1595(16) 1.0659(7) 0.8265(6) 0.062(4) Uiso 0.4 1 d . . . A 2
O24A O 0.8814(8) 1.0869(3) 0.7957(3) 0.0529(19) Uiso 0.6 1 d . . . A 1
O24B O 0.893(3) 1.0303(12) 0.7623(11) 0.187(9) Uiso 0.4 1 d . . . A 2
Cl5 Cl 0.25048(15) 0.56280(6) 0.43090(6) 0.0285(3) Uani 1 1 d . . . . .
O25 O 0.2059(6) 0.6228(2) 0.4755(2) 0.0788(16) Uani 1 1 d . . . . .
O26 O 0.1176(5) 0.5208(2) 0.3923(2) 0.0733(15) Uani 1 1 d . . . . .
O27 O 0.3495(4) 0.58018(16) 0.39105(15) 0.0344(9) Uani 1 1 d . . . . .
O28 O 0.3407(4) 0.52529(17) 0.46219(16) 0.0387(9) Uani 1 1 d . . . . .
O29 O 0.6292(5) 0.68125(18) 0.76097(17) 0.0449(10) Uani 1 1 d . . . . .
C57 C 0.8714(6) 0.6285(3) 0.7626(3) 0.0452(15) Uani 1 1 d . . . . .
H57A H 0.918322 0.672685 0.769806 0.068 Uiso 1 1 calc GR . . . .
H57B H 0.905076 0.596770 0.725411 0.068 Uiso 1 1 calc GR . . . .
H57C H 0.904525 0.615556 0.797282 0.068 Uiso 1 1 calc GR . . . .
C58 C 0.6947(7) 0.6294(3) 0.7550(2) 0.0324(13) Uani 1 1 d . . . . .
C59 C 0.6024(7) 0.5641(3) 0.7412(3) 0.0493(16) Uani 1 1 d . . . . .
H59A H 0.620177 0.549953 0.776180 0.074 Uiso 1 1 calc GR . . . .
H59B H 0.636477 0.530565 0.705174 0.074 Uiso 1 1 calc GR . . . .
H59C H 0.491132 0.569542 0.733408 0.074 Uiso 1 1 calc GR . . . .
O30 O 0.1442(5) 0.67534(18) 0.26129(17) 0.0459(10) Uani 1 1 d . . . . .
C60 C 0.3844(6) 0.6218(3) 0.2633(3) 0.0414(14) Uani 1 1 d . . . . .
H60A H 0.415538 0.591522 0.224839 0.062 Uiso 1 1 calc GR . . . .
H60B H 0.418314 0.606141 0.296243 0.062 Uiso 1 1 calc GR . . . .
H60C H 0.432970 0.666103 0.272408 0.062 Uiso 1 1 calc GR . . . .
C61 C 0.2091(6) 0.6242(3) 0.2575(2) 0.0316(12) Uani 1 1 d . . . . .
C62 C 0.1139(6) 0.5593(2) 0.2468(2) 0.0346(13) Uani 1 1 d . . . . .
H62A H 0.130719 0.547726 0.283303 0.052 Uiso 1 1 calc GR . . . .
H62B H 0.147539 0.523853 0.211992 0.052 Uiso 1 1 calc GR . . . .
H62C H 0.002968 0.564821 0.238367 0.052 Uiso 1 1 calc GR . . . .
O31 O 0.3922(5) 0.8507(2) 0.71675(19) 0.0629(13) Uani 1 1 d . . . . .
C63 C 0.3249(8) 0.9351(3) 0.8067(3) 0.0550(18) Uani 1 1 d . . . . .
H63A H 0.236420 0.904627 0.804299 0.083 Uiso 1 1 calc GR . . . .
H63B H 0.289002 0.979504 0.814770 0.083 Uiso 1 1 calc GR . . . .
H63C H 0.403874 0.936143 0.839830 0.083 Uiso 1 1 calc GR . . . .
C64 C 0.3945(7) 0.9120(3) 0.7472(3) 0.0430(15) Uani 1 1 d . . . . .
C65 C 0.4649(8) 0.9598(4) 0.7262(3) 0.076(2) Uani 1 1 d . . . . .
H65A H 0.569517 0.974627 0.748049 0.115 Uiso 1 1 calc GR . . . .
H65B H 0.400680 0.997790 0.733834 0.115 Uiso 1 1 calc GR . . . .
H65C H 0.472306 0.939432 0.682341 0.115 Uiso 1 1 calc GR . . . .


_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 1.975(4) . ?
Fe1 N3 1.889(3) . ?
Fe1 N5 1.956(4) . ?
Fe1 N6 1.969(4) . ?
Fe1 N8 1.893(3) . ?
Fe1 N10 1.962(4) . ?
O1 C12 1.194(6) . ?
O2 C12 1.338(6) . ?
O2 C13 1.473(5) . ?
O3 C26 1.208(5) . ?
O4 C26 1.335(5) . ?
O4 C27 1.460(5) . ?
N1 N2 1.385(5) . ?
N1 C1 1.323(6) . ?
N2 C3 1.357(5) . ?
N2 C4 1.402(5) . ?
N3 C4 1.342(5) . ?
N3 C8 1.345(5) . ?
N4 N5 1.387(5) . ?
N4 C8 1.399(5) . ?
N4 C9 1.346(6) . ?
N5 C11 1.334(5) . ?
N6 N7 1.381(4) . ?
N6 C15 1.323(5) . ?
N7 C17 1.352(5) . ?
N7 C18 1.401(5) . ?
N8 C18 1.333(5) . ?
N8 C22 1.335(5) . ?
N9 N10 1.378(5) . ?
N9 C22 1.408(5) . ?
N9 C23 1.367(5) . ?
N10 C25 1.328(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.394(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.362(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(6) . ?
C6 C7 1.389(6) . ?
C6 C12 1.508(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.376(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.365(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.401(6) . ?
C11 H11 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.489(7) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9300 . ?
C15 C16 1.407(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.363(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.387(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.405(6) . ?
C20 C21 1.386(6) . ?
C20 C26 1.496(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.379(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.368(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.389(6) . ?
C25 H25 0.9300 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.500(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Fe2 N11 1.964(4) . ?
Fe2 N13 1.896(3) . ?
Fe2 N15 1.969(4) . ?
Fe2 N16 1.977(4) . ?
Fe2 N18 1.893(3) . ?
Fe2 N20 1.974(4) . ?
O5 C40 1.202(5) . ?
O6 C40 1.338(5) . ?
O6 C41 1.455(5) . ?
O7 C54 1.203(6) . ?
O8 C54 1.315(6) . ?
O8 C55 1.464(5) . ?
N11 N12 1.384(4) . ?
N11 C29 1.322(6) . ?
N12 C31 1.359(5) . ?
N12 C32 1.399(5) . ?
N13 C32 1.345(5) . ?
N13 C36 1.330(5) . ?
N14 N15 1.391(5) . ?
N14 C36 1.407(5) . ?
N14 C37 1.362(5) . ?
N15 C39 1.333(5) . ?
N16 N17 1.379(5) . ?
N16 C43 1.329(5) . ?
N17 C45 1.351(5) . ?
N17 C46 1.401(5) . ?
N18 C46 1.336(5) . ?
N18 C50 1.346(5) . ?
N19 N20 1.372(5) . ?
N19 C50 1.396(5) . ?
N19 C51 1.360(6) . ?
N20 C53 1.328(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.405(6) . ?
C30 H30 0.9300 . ?
C30 C31 1.366(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.375(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.380(6) . ?
C34 C35 1.401(6) . ?
C34 C40 1.507(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.381(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.368(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.396(6) . ?
C39 H39 0.9300 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.500(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43 0.9300 . ?
C43 C44 1.393(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.351(6) . ?
C45 H45 0.9300 . ?
C46 C47 1.384(6) . ?
C47 H47 0.9300 . ?
C47 C48 1.401(6) . ?
C48 C49 1.388(6) . ?
C48 C54 1.492(6) . ?
C49 H49 0.9300 . ?
C49 C50 1.378(6) . ?
C51 H51 0.9300 . ?
C51 C52 1.365(6) . ?
C52 H52 0.9300 . ?
C52 C53 1.398(6) . ?
C53 H53 0.9300 . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55 C56 1.483(8) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
Cl1 O9 1.422(4) . ?
Cl1 O10 1.439(3) . ?
Cl1 O11 1.444(4) . ?
Cl1 O12 1.394(4) . ?
Cl2 O13 1.333(6) 2_677 ?
Cl2 O13 1.333(6) . ?
Cl2 O14 1.444(6) . ?
Cl2 O14 1.444(6) 2_677 ?
Cl2 O15 1.462(7) 2_677 ?
Cl2 O15 1.462(7) . ?
Cl2 O16 1.569(6) 2_677 ?
Cl2 O16 1.569(6) . ?
O13 O14 1.448(10) 2_677 ?
O13 O15 1.518(9) 2_677 ?
O13 O16 1.698(9) 2_677 ?
O14 O15 1.680(9) 2_677 ?
Cl3 O17 1.343(6) 2_776 ?
Cl3 O17 1.344(6) . ?
Cl3 O18 1.621(6) 2_776 ?
Cl3 O18 1.621(6) . ?
Cl3 O19 1.467(6) . ?
Cl3 O19 1.467(6) 2_776 ?
Cl3 O20 1.382(6) . ?
Cl3 O20 1.382(6) 2_776 ?
O17 O19 1.557(9) 2_776 ?
O17 O20 1.336(9) . ?
O19 O20 1.598(9) . ?
Cl4 O21A 1.341(8) . ?
Cl4 O21B 1.420(13) . ?
Cl4 O22A 1.427(8) . ?
Cl4 O22B 1.400(17) . ?
Cl4 O23A 1.346(8) . ?
Cl4 O23B 1.493(13) . ?
Cl4 O24A 1.532(7) . ?
Cl4 O24B 1.55(2) . ?
Cl5 O25 1.414(4) . ?
Cl5 O26 1.426(4) . ?
Cl5 O27 1.439(3) . ?
Cl5 O28 1.444(3) . ?
O29 C58 1.218(6) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C57 C58 1.490(7) . ?
C58 C59 1.489(7) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
O30 C61 1.213(6) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C60 C61 1.481(7) . ?
C61 C62 1.507(7) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
O31 C64 1.240(6) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C63 C64 1.477(8) . ?
C64 C65 1.417(8) . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?

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
N3 Fe1 N1 80.14(15) . . ?
N3 Fe1 N5 80.36(15) . . ?
N3 Fe1 N6 101.16(14) . . ?
N3 Fe1 N8 177.36(15) . . ?
N3 Fe1 N10 98.05(15) . . ?
N5 Fe1 N1 160.50(15) . . ?
N5 Fe1 N6 93.21(15) . . ?
N5 Fe1 N10 88.69(15) . . ?
N6 Fe1 N1 90.12(15) . . ?
N8 Fe1 N1 102.19(15) . . ?
N8 Fe1 N5 97.31(15) . . ?
N8 Fe1 N6 80.16(14) . . ?
N8 Fe1 N10 80.60(15) . . ?
N10 Fe1 N1 94.45(15) . . ?
N10 Fe1 N6 160.75(14) . . ?
C12 O2 C13 115.3(4) . . ?
C26 O4 C27 118.1(4) . . ?
N2 N1 Fe1 112.1(3) . . ?
C1 N1 Fe1 142.4(3) . . ?
C1 N1 N2 104.9(4) . . ?
N1 N2 C4 116.7(3) . . ?
C3 N2 N1 110.8(4) . . ?
C3 N2 C4 132.5(4) . . ?
C4 N3 Fe1 120.7(3) . . ?
C4 N3 C8 119.4(4) . . ?
C8 N3 Fe1 120.0(3) . . ?
N5 N4 C8 115.9(3) . . ?
C9 N4 N5 110.9(4) . . ?
C9 N4 C8 133.1(4) . . ?
N4 N5 Fe1 112.8(3) . . ?
C11 N5 Fe1 142.2(3) . . ?
C11 N5 N4 105.0(4) . . ?
N7 N6 Fe1 112.2(3) . . ?
C15 N6 Fe1 142.4(3) . . ?
C15 N6 N7 105.3(4) . . ?
N6 N7 C18 116.7(4) . . ?
C17 N7 N6 110.4(3) . . ?
C17 N7 C18 132.9(4) . . ?
C18 N8 Fe1 120.5(3) . . ?
C18 N8 C22 119.6(4) . . ?
C22 N8 Fe1 119.7(3) . . ?
N10 N9 C22 116.4(3) . . ?
C23 N9 N10 110.9(3) . . ?
C23 N9 C22 132.6(4) . . ?
N9 N10 Fe1 112.4(3) . . ?
C25 N10 Fe1 142.5(3) . . ?
C25 N10 N9 105.0(3) . . ?
N1 C1 H1 124.5 . . ?
N1 C1 C2 111.1(4) . . ?
C2 C1 H1 124.5 . . ?
C1 C2 H2 126.7 . . ?
C3 C2 C1 106.5(4) . . ?
C3 C2 H2 126.7 . . ?
N2 C3 C2 106.7(4) . . ?
N2 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
N3 C4 N2 110.2(4) . . ?
N3 C4 C5 123.0(4) . . ?
C5 C4 N2 126.8(4) . . ?
C4 C5 H5 121.6 . . ?
C4 C5 C6 116.7(4) . . ?
C6 C5 H5 121.6 . . ?
C5 C6 C12 117.1(4) . . ?
C7 C6 C5 121.4(4) . . ?
C7 C6 C12 121.5(4) . . ?
C6 C7 H7 121.3 . . ?
C8 C7 C6 117.5(4) . . ?
C8 C7 H7 121.3 . . ?
N3 C8 N4 110.7(4) . . ?
N3 C8 C7 122.0(4) . . ?
C7 C8 N4 127.3(4) . . ?
N4 C9 H9 126.3 . . ?
N4 C9 C10 107.4(4) . . ?
C10 C9 H9 126.3 . . ?
C9 C10 H10 126.9 . . ?
C9 C10 C11 106.2(4) . . ?
C11 C10 H10 126.9 . . ?
N5 C11 C10 110.6(4) . . ?
N5 C11 H11 124.7 . . ?
C10 C11 H11 124.7 . . ?
O1 C12 O2 125.8(4) . . ?
O1 C12 C6 122.6(5) . . ?
O2 C12 C6 111.6(4) . . ?
O2 C13 H13A 109.6 . . ?
O2 C13 H13B 109.6 . . ?
O2 C13 C14 110.1(4) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15 124.5 . . ?
N6 C15 C16 111.0(4) . . ?
C16 C15 H15 124.5 . . ?
C15 C16 H16 127.3 . . ?
C17 C16 C15 105.3(4) . . ?
C17 C16 H16 127.3 . . ?
N7 C17 C16 107.9(4) . . ?
N7 C17 H17 126.1 . . ?
C16 C17 H17 126.1 . . ?
N8 C18 N7 110.4(4) . . ?
N8 C18 C19 123.0(4) . . ?
C19 C18 N7 126.6(4) . . ?
C18 C19 H19 122.0 . . ?
C18 C19 C20 115.9(4) . . ?
C20 C19 H19 122.0 . . ?
C19 C20 C26 116.8(4) . . ?
C21 C20 C19 121.8(4) . . ?
C21 C20 C26 121.4(4) . . ?
C20 C21 H21 121.6 . . ?
C22 C21 C20 116.8(4) . . ?
C22 C21 H21 121.6 . . ?
N8 C22 N9 110.7(4) . . ?
N8 C22 C21 122.8(4) . . ?
C21 C22 N9 126.4(4) . . ?
N9 C23 H23 126.8 . . ?
N9 C23 C24 106.4(4) . . ?
C24 C23 H23 126.8 . . ?
C23 C24 H24 126.8 . . ?
C23 C24 C25 106.4(4) . . ?
C25 C24 H24 126.8 . . ?
N10 C25 C24 111.3(4) . . ?
N10 C25 H25 124.3 . . ?
C24 C25 H25 124.3 . . ?
O3 C26 O4 125.6(4) . . ?
O3 C26 C20 124.1(4) . . ?
O4 C26 C20 110.4(4) . . ?
O4 C27 H27A 109.8 . . ?
O4 C27 H27B 109.8 . . ?
O4 C27 C28 109.6(4) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N11 Fe2 N15 160.52(14) . . ?
N11 Fe2 N16 90.02(15) . . ?
N11 Fe2 N20 93.47(15) . . ?
N13 Fe2 N11 80.46(14) . . ?
N13 Fe2 N15 80.06(14) . . ?
N13 Fe2 N16 99.11(15) . . ?
N13 Fe2 N20 100.72(15) . . ?
N15 Fe2 N16 93.08(15) . . ?
N15 Fe2 N20 90.10(15) . . ?
N18 Fe2 N11 98.79(15) . . ?
N18 Fe2 N13 178.77(15) . . ?
N18 Fe2 N15 100.69(15) . . ?
N18 Fe2 N16 79.90(15) . . ?
N18 Fe2 N20 80.27(15) . . ?
N20 Fe2 N16 160.17(15) . . ?
C40 O6 C41 118.4(4) . . ?
C54 O8 C55 118.1(4) . . ?
N12 N11 Fe2 112.4(3) . . ?
C29 N11 Fe2 142.5(3) . . ?
C29 N11 N12 105.0(4) . . ?
N11 N12 C32 116.6(3) . . ?
C31 N12 N11 110.8(3) . . ?
C31 N12 C32 132.6(4) . . ?
C32 N13 Fe2 119.7(3) . . ?
C36 N13 Fe2 120.8(3) . . ?
C36 N13 C32 119.4(4) . . ?
N15 N14 C36 116.2(3) . . ?
C37 N14 N15 110.6(3) . . ?
C37 N14 C36 133.2(4) . . ?
N14 N15 Fe2 112.3(3) . . ?
C39 N15 Fe2 142.9(3) . . ?
C39 N15 N14 104.6(4) . . ?
N17 N16 Fe2 112.4(3) . . ?
C43 N16 Fe2 143.0(3) . . ?
C43 N16 N17 104.5(4) . . ?
N16 N17 C46 116.3(4) . . ?
C45 N17 N16 110.8(4) . . ?
C45 N17 C46 132.7(4) . . ?
C46 N18 Fe2 120.4(3) . . ?
C46 N18 C50 120.0(4) . . ?
C50 N18 Fe2 119.7(3) . . ?
N20 N19 C50 116.9(4) . . ?
C51 N19 N20 111.1(4) . . ?
C51 N19 C50 132.1(4) . . ?
N19 N20 Fe2 112.3(3) . . ?
C53 N20 Fe2 142.4(3) . . ?
C53 N20 N19 105.1(4) . . ?
N11 C29 H29 124.3 . . ?
N11 C29 C30 111.3(4) . . ?
C30 C29 H29 124.3 . . ?
C29 C30 H30 127.1 . . ?
C31 C30 C29 105.7(4) . . ?
C31 C30 H30 127.1 . . ?
N12 C31 C30 107.1(4) . . ?
N12 C31 H31 126.4 . . ?
C30 C31 H31 126.4 . . ?
N13 C32 N12 110.7(4) . . ?
N13 C32 C33 122.7(4) . . ?
C33 C32 N12 126.6(4) . . ?
C32 C33 H33 121.6 . . ?
C32 C33 C34 116.8(4) . . ?
C34 C33 H33 121.6 . . ?
C33 C34 C35 121.9(4) . . ?
C33 C34 C40 120.9(4) . . ?
C35 C34 C40 117.2(4) . . ?
C34 C35 H35 121.9 . . ?
C36 C35 C34 116.2(4) . . ?
C36 C35 H35 121.9 . . ?
N13 C36 N14 110.4(4) . . ?
N13 C36 C35 122.9(4) . . ?
C35 C36 N14 126.7(4) . . ?
N14 C37 H37 126.3 . . ?
N14 C37 C38 107.3(4) . . ?
C38 C37 H37 126.3 . . ?
C37 C38 H38 127.1 . . ?
C37 C38 C39 105.8(4) . . ?
C39 C38 H38 127.1 . . ?
N15 C39 C38 111.6(4) . . ?
N15 C39 H39 124.2 . . ?
C38 C39 H39 124.2 . . ?
O5 C40 O6 125.9(4) . . ?
O5 C40 C34 123.8(4) . . ?
O6 C40 C34 110.3(4) . . ?
O6 C41 H41A 109.8 . . ?
O6 C41 H41B 109.8 . . ?
O6 C41 C42 109.5(4) . . ?
H41A C41 H41B 108.2 . . ?
C42 C41 H41A 109.8 . . ?
C42 C41 H41B 109.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N16 C43 H43 124.4 . . ?
N16 C43 C44 111.1(4) . . ?
C44 C43 H43 124.4 . . ?
C43 C44 H44 126.9 . . ?
C45 C44 C43 106.1(4) . . ?
C45 C44 H44 126.9 . . ?
N17 C45 H45 126.3 . . ?
C44 C45 N17 107.4(4) . . ?
C44 C45 H45 126.3 . . ?
N18 C46 N17 110.7(4) . . ?
N18 C46 C47 122.6(4) . . ?
C47 C46 N17 126.6(4) . . ?
C46 C47 H47 121.8 . . ?
C46 C47 C48 116.4(4) . . ?
C48 C47 H47 121.8 . . ?
C47 C48 C54 121.2(4) . . ?
C49 C48 C47 121.4(4) . . ?
C49 C48 C54 117.4(4) . . ?
C48 C49 H49 121.3 . . ?
C50 C49 C48 117.5(4) . . ?
C50 C49 H49 121.3 . . ?
N18 C50 N19 110.8(4) . . ?
N18 C50 C49 121.9(4) . . ?
C49 C50 N19 127.3(4) . . ?
N19 C51 H51 126.6 . . ?
N19 C51 C52 106.8(4) . . ?
C52 C51 H51 126.6 . . ?
C51 C52 H52 127.0 . . ?
C51 C52 C53 106.0(4) . . ?
C53 C52 H52 127.0 . . ?
N20 C53 C52 111.0(4) . . ?
N20 C53 H53 124.5 . . ?
C52 C53 H53 124.5 . . ?
O7 C54 O8 125.3(4) . . ?
O7 C54 C48 122.3(5) . . ?
O8 C54 C48 112.4(4) . . ?
O8 C55 H55A 109.5 . . ?
O8 C55 H55B 109.5 . . ?
O8 C55 C56 110.6(4) . . ?
H55A C55 H55B 108.1 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O9 Cl1 O10 109.1(3) . . ?
O9 Cl1 O11 106.9(3) . . ?
O10 Cl1 O11 108.7(2) . . ?
O12 Cl1 O9 113.3(4) . . ?
O12 Cl1 O10 109.4(3) . . ?
O12 Cl1 O11 109.3(2) . . ?
O13 Cl2 O13 180.0 . 2_677 ?
O13 Cl2 O14 117.3(4) 2_677 2_677 ?
O13 Cl2 O14 62.7(4) 2_677 . ?
O13 Cl2 O14 117.3(4) . . ?
O13 Cl2 O14 62.7(4) . 2_677 ?
O13 Cl2 O15 65.6(4) 2_677 . ?
O13 Cl2 O15 114.4(4) 2_677 2_677 ?
O13 Cl2 O15 65.6(4) . 2_677 ?
O13 Cl2 O15 114.4(4) . . ?
O13 Cl2 O16 108.9(4) . . ?
O13 Cl2 O16 71.1(4) . 2_677 ?
O13 Cl2 O16 108.9(4) 2_677 2_677 ?
O13 Cl2 O16 71.1(4) 2_677 . ?
O14 Cl2 O14 180.0(4) . 2_677 ?
O14 Cl2 O15 70.6(4) 2_677 . ?
O14 Cl2 O15 109.4(4) 2_677 2_677 ?
O14 Cl2 O15 109.4(4) . . ?
O14 Cl2 O15 70.6(4) . 2_677 ?
O14 Cl2 O16 76.9(3) 2_677 . ?
O14 Cl2 O16 103.1(3) . . ?
O14 Cl2 O16 76.9(3) . 2_677 ?
O14 Cl2 O16 103.1(3) 2_677 2_677 ?
O15 Cl2 O15 180.0 . 2_677 ?
O15 Cl2 O16 78.0(4) . 2_677 ?
O15 Cl2 O16 102.0(4) . . ?
O15 Cl2 O16 78.0(4) 2_677 . ?
O15 Cl2 O16 102.0(4) 2_677 2_677 ?
O16 Cl2 O16 180.0 . 2_677 ?
Cl2 O13 O14 62.4(4) . 2_677 ?
Cl2 O13 O15 61.3(4) . 2_677 ?
Cl2 O13 O16 60.9(3) . 2_677 ?
O14 O13 O15 106.2(6) 2_677 2_677 ?
O14 O13 O16 97.0(5) 2_677 2_677 ?
O15 O13 O16 94.0(5) 2_677 2_677 ?
Cl2 O14 O13 54.9(3) . 2_677 ?
Cl2 O14 O15 55.2(3) . 2_677 ?
O13 O14 O15 97.1(5) 2_677 2_677 ?
Cl2 O15 O13 53.1(4) . 2_677 ?
Cl2 O15 O14 54.2(3) . 2_677 ?
O13 O15 O14 95.7(5) 2_677 2_677 ?
Cl2 O16 O13 48.0(3) . 2_677 ?
O17 Cl3 O17 180.0 2_776 . ?
O17 Cl3 O18 75.3(4) 2_776 2_776 ?
O17 Cl3 O18 75.3(4) . . ?
O17 Cl3 O18 104.7(4) 2_776 . ?
O17 Cl3 O18 104.7(4) . 2_776 ?
O17 Cl3 O19 67.1(4) 2_776 . ?
O17 Cl3 O19 112.9(4) 2_776 2_776 ?
O17 Cl3 O19 112.9(4) . . ?
O17 Cl3 O19 67.1(4) . 2_776 ?
O17 Cl3 O20 58.7(4) 2_776 2_776 ?
O17 Cl3 O20 121.3(4) 2_776 . ?
O17 Cl3 O20 58.7(4) . . ?
O17 Cl3 O20 121.3(4) . 2_776 ?
O18 Cl3 O18 180.0 2_776 . ?
O19 Cl3 O18 99.4(4) 2_776 . ?
O19 Cl3 O18 80.6(4) 2_776 2_776 ?
O19 Cl3 O18 80.6(4) . . ?
O19 Cl3 O18 99.4(4) . 2_776 ?
O19 Cl3 O19 180.00(8) . 2_776 ?
O20 Cl3 O18 103.4(4) . . ?
O20 Cl3 O18 103.4(4) 2_776 2_776 ?
O20 Cl3 O18 76.6(4) . 2_776 ?
O20 Cl3 O18 76.6(4) 2_776 . ?
O20 Cl3 O19 111.8(4) 2_776 . ?
O20 Cl3 O19 111.8(4) . 2_776 ?
O20 Cl3 O19 68.2(4) . . ?
O20 Cl3 O19 68.2(4) 2_776 2_776 ?
O20 Cl3 O20 180.0(4) 2_776 . ?
Cl3 O17 O19 60.2(3) . 2_776 ?
O20 O17 Cl3 62.1(4) . . ?
O20 O17 O19 109.0(6) . 2_776 ?
Cl3 O19 O17 52.6(3) . 2_776 ?
Cl3 O19 O20 53.4(3) . . ?
O17 O19 O20 97.7(5) 2_776 . ?
Cl3 O20 O19 58.4(3) . . ?
O17 O20 Cl3 59.2(4) . . ?
O17 O20 O19 105.6(6) . . ?
O21A Cl4 O22A 122.7(5) . . ?
O21A Cl4 O23A 121.0(5) . . ?
O21A Cl4 O24A 101.6(5) . . ?
O21B Cl4 O23B 106.1(7) . . ?
O21B Cl4 O24B 88.9(10) . . ?
O22A Cl4 O24A 86.6(5) . . ?
O22B Cl4 O21B 95.0(9) . . ?
O22B Cl4 O23B 98.3(9) . . ?
O22B Cl4 O24B 148.0(12) . . ?
O23A Cl4 O22A 114.9(5) . . ?
O23A Cl4 O24A 92.6(5) . . ?
O23B Cl4 O24B 111.1(10) . . ?
O25 Cl5 O26 113.0(3) . . ?
O25 Cl5 O27 108.9(2) . . ?
O25 Cl5 O28 109.5(3) . . ?
O26 Cl5 O27 107.6(3) . . ?
O26 Cl5 O28 109.2(2) . . ?
O27 Cl5 O28 108.6(2) . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
C58 C57 H57C 109.5 . . ?
O29 C58 C57 121.7(5) . . ?
O29 C58 C59 121.7(5) . . ?
C59 C58 C57 116.6(5) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
O30 C61 C60 122.4(5) . . ?
O30 C61 C62 121.2(5) . . ?
C60 C61 C62 116.4(4) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
C64 C63 H63C 109.5 . . ?
O31 C64 C63 119.2(6) . . ?
O31 C64 C65 120.9(6) . . ?
C65 C64 C63 119.8(5) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.483
####################################################################### 
# 
# 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_vg77_4300k77
_database_code_depnum_ccdc_archive 'CCDC 1856813'
_audit_update_record             
;
2018-11-05 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_audit_creation_date             2018-11-02
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C28 H28 Fe N10 O4), 2(C28 H26 Fe N10 O4), 3(C3 H6 O), 4(Cl2 O8)'
_chemical_formula_sum            'C121 H126 Cl8 Fe4 N40 O51'
_chemical_formula_weight         3463.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5561(4)
_cell_length_b                   21.3922(9)
_cell_length_c                   23.5484(11)
_cell_angle_alpha                69.009(4)
_cell_angle_beta                 83.330(4)
_cell_angle_gamma                89.892(4)
_cell_volume                     3993.2(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      22.6340
_cell_measurement_theta_min      3.3640
_shelx_estimated_absorpt_T_max   0.983
_shelx_estimated_absorpt_T_min   0.804
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1780
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60459
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         3.309
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -88.00   10.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -67.0000   27.2844 98

#__ type_ start__ end____ width___ exp.time_
  2 omega  -88.00    6.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -57.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -88.00   11.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -68.0000  -83.9700 99

#__ type_ start__ end____ width___ exp.time_
  4 omega  -89.00   11.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.6840  -69.0000  124.1873 100

#__ type_ start__ end____ width___ exp.time_
  5 omega  -52.00   47.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5434  -69.0000 -104.3589 99

#__ type_ start__ end____ width___ exp.time_
  6 omega  -51.00   49.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -69.0000   69.9356 100

#__ type_ start__ end____ width___ exp.time_
  7 omega  -51.00   48.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -68.0000   -6.4472 99

#__ type_ start__ end____ width___ exp.time_
  8 omega  -51.00   49.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -69.0000  175.2479 100

#__ type_ start__ end____ width___ exp.time_
  9 omega  -51.00   15.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5434  -63.0000  134.7372 66
;
_diffrn_measurement_device_type  
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0090108000
_diffrn_orient_matrix_UB_12      0.0080759000
_diffrn_orient_matrix_UB_13      0.0268699000
_diffrn_orient_matrix_UB_21      -0.0799916000
_diffrn_orient_matrix_UB_22      0.0069718000
_diffrn_orient_matrix_UB_23      -0.0038265000
_diffrn_orient_matrix_UB_31      -0.0223452000
_diffrn_orient_matrix_UB_32      -0.0339079000
_diffrn_orient_matrix_UB_33      0.0178981000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7004
_reflns_number_total             17045
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         17045
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.2250
_refine_ls_R_factor_gt           0.1136
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3075
_refine_ls_wR_factor_ref         0.4051
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4-O22A = Cl4-O23A = Cl4-O22B = Cl4-O24B = Cl4-O24A = Cl4-O21A = Cl4-O23B =
 Cl4-O21B
 1.4 with sigma of 0.02
 Cl5-O26B = Cl5-O28A = Cl5-O27B = Cl5-O25A = Cl5-O26A = Cl5-O28B = Cl5-O25B =
 Cl5-O27A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O19A \\sim O19B \\sim O18A \\sim O18B \\sim O20A \\sim O20B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O28B \\sim O25B \\sim O26A \\sim O26B \\sim O27A \\sim O27B \\sim O28A \\sim
O25A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O23B \\sim O22A \\sim O22B \\sim O21A \\sim O24B \\sim O23A \\sim O21B \\sim
O24A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: C13A(0.5) H13A(0.5) H13B(0.5) C13B(0.5) H13C(0.5) H13D(0.5)
 C14A(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C14B(0.5) H14D(0.5) H14E(0.5)
 H14F(0.5) C56A(0.5) H56A(0.5) H56B(0.5) C56B(0.5) H56C(0.5) H56D(0.5)
 C57A(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C57B(0.5) H57D(0.5) H57E(0.5)
 H57F(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5) O29(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) O30(0.5) C64(0.5) H64A(0.5) H64B(0.5)
 H64C(0.5) C65(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) O31(0.5) O9(0.5)
 O10(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) O15(0.5) O16(0.5) O18A(0.6)
 O18B(0.4) O19A(0.6) O19B(0.4) O20A(0.6) O20B(0.4) O21A(0.6) O21B(0.4)
 O22A(0.6) O22B(0.4) O23A(0.6) O23B(0.4) O24A(0.6) O24B(0.4) O25A(0.6)
 O25B(0.4) O26A(0.6) O26B(0.4) O27A(0.6) O27B(0.4) O28A(0.6) O28B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C16(H16A,H16B), C24(H24A,H24B), C27(H27A,
 H27B), C42(H42A,H42B), C56A(H56A,H56B), C56B(H56C,H56D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C15(H15),
 C17(H17), C19(H19), C21(H21), C23(H23), C25(H25), C29(H29), C30(H30), C31(H31),
  C34(H34), C36(H36), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45),
 C46(H46), C48(H48), C50(H50), C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C28(H28A,H28B,H28C), C43(H43A,
 H43B,H43C), C57A(H57A,H57B,H57C), C57B(H57D,H57E,H57F), C58(H58A,H58B,H58C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C66(H66A,H66B,H66C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.4805(9) 0.2445(4) 0.5348(3) 0.0555(19) Uani 1 1 d . . . . .
H1 H 0.456792 0.288621 0.513821 0.067 Uiso 1 1 calc R . . . .
C2 C 0.3763(9) 0.1965(4) 0.5772(4) 0.062(2) Uani 1 1 d . . . . .
H2 H 0.271664 0.202423 0.589343 0.075 Uiso 1 1 calc R . . . .
C3 C 0.4531(9) 0.1406(4) 0.5974(4) 0.062(2) Uani 1 1 d . . . . .
H3 H 0.411932 0.100202 0.626810 0.074 Uiso 1 1 calc R . . . .
C4 C 0.7323(8) 0.1130(3) 0.5682(3) 0.0468(16) Uani 1 1 d . . . . .
C5 C 0.7445(9) 0.0468(3) 0.6024(3) 0.0528(18) Uani 1 1 d . . . . .
H5 H 0.661016 0.022684 0.630666 0.063 Uiso 1 1 calc R . . . .
C6 C 0.8846(9) 0.0162(3) 0.5941(3) 0.0501(17) Uani 1 1 d . . . . .
C7 C 1.0110(9) 0.0531(3) 0.5531(3) 0.0540(19) Uani 1 1 d . . . . .
H7 H 1.105650 0.033500 0.547242 0.065 Uiso 1 1 calc R . . . .
C8 C 0.9895(8) 0.1203(3) 0.5215(3) 0.0465(16) Uani 1 1 d . . . . .
C9 C 1.2479(9) 0.1608(4) 0.4563(4) 0.066(2) Uani 1 1 d . . . . .
H9 H 1.301221 0.121339 0.463502 0.080 Uiso 1 1 calc R . . . .
C10 C 1.3018(9) 0.2236(4) 0.4181(4) 0.069(2) Uani 1 1 d . . . . .
H10 H 1.400131 0.235597 0.394942 0.082 Uiso 1 1 calc R . . . .
C11 C 1.1828(9) 0.2651(4) 0.4209(3) 0.0578(19) Uani 1 1 d . . . . .
H11 H 1.188603 0.310936 0.398401 0.069 Uiso 1 1 calc R . . . .
C12 C 0.9057(12) -0.0569(4) 0.6271(4) 0.067(2) Uani 1 1 d . . . . .
C13A C 0.778(3) -0.1601(11) 0.6991(10) 0.080(7) Uiso 0.5 1 d . . . A 1
H13A H 0.829331 -0.181211 0.672045 0.095 Uiso 0.5 1 calc R . . A 1
H13B H 0.670916 -0.178248 0.713258 0.095 Uiso 0.5 1 calc R . . A 1
C13B C 0.806(3) -0.1518(10) 0.7131(9) 0.063(5) Uiso 0.5 1 d . . . A 2
H13C H 0.865832 -0.177329 0.691938 0.076 Uiso 0.5 1 calc R . . A 2
H13D H 0.703814 -0.174485 0.729596 0.076 Uiso 0.5 1 calc R . . A 2
C14A C 0.878(2) -0.1661(10) 0.7556(10) 0.072(5) Uiso 0.5 1 d . . . A 1
H14A H 0.983431 -0.148350 0.739572 0.108 Uiso 0.5 1 calc GR . . A 1
H14B H 0.880421 -0.212268 0.781562 0.108 Uiso 0.5 1 calc GR . . A 1
H14C H 0.828430 -0.141057 0.778883 0.108 Uiso 0.5 1 calc GR . . A 1
C14B C 0.899(3) -0.1487(14) 0.7696(12) 0.121(10) Uiso 0.5 1 d . . . A 2
H14D H 0.986358 -0.116703 0.753304 0.181 Uiso 0.5 1 calc GR . . A 2
H14E H 0.936954 -0.192129 0.790851 0.181 Uiso 0.5 1 calc GR . . A 2
H14F H 0.827926 -0.135551 0.797518 0.181 Uiso 0.5 1 calc GR . . A 2
C15 C 0.9216(9) 0.2551(4) 0.6077(3) 0.0543(18) Uani 1 1 d . . . . .
H15 H 0.935710 0.210654 0.631477 0.065 Uiso 1 1 calc R . . . .
C16 C 0.9332(10) 0.3084(4) 0.6271(3) 0.069(2) Uani 1 1 d . . . . .
H16A H 1.038919 0.313244 0.636487 0.083 Uiso 1 1 calc R . . . .
H16B H 0.859496 0.301763 0.663515 0.083 Uiso 1 1 calc R . . . .
C17 C 0.8975(10) 0.3651(4) 0.5787(3) 0.065(2) Uani 1 1 d . . . . .
H17 H 0.891819 0.408718 0.578095 0.077 Uiso 1 1 calc R . . . .
C18 C 0.8337(7) 0.3780(3) 0.4740(3) 0.0395(14) Uani 1 1 d . . . . .
C19 C 0.8063(8) 0.4453(3) 0.4476(3) 0.0464(16) Uani 1 1 d . . . . .
H19 H 0.814674 0.474311 0.468641 0.056 Uiso 1 1 calc R . . . .
C20 C 0.7662(8) 0.4679(3) 0.3891(3) 0.0461(16) Uani 1 1 d . . . . .
C21 C 0.7558(8) 0.4249(3) 0.3566(3) 0.0458(16) Uani 1 1 d . . . . .
H21 H 0.735469 0.440407 0.315997 0.055 Uiso 1 1 calc R . . . .
C22 C 0.7776(8) 0.3580(3) 0.3884(3) 0.0444(16) Uani 1 1 d . . . . .
C23 C 0.7177(10) 0.3034(4) 0.3155(3) 0.062(2) Uani 1 1 d . . . . .
H23 H 0.696594 0.340218 0.281909 0.075 Uiso 1 1 calc R . . . .
C24 C 0.7136(11) 0.2383(4) 0.3200(4) 0.073(2) Uani 1 1 d . . . . .
H24A H 0.789985 0.231606 0.289123 0.088 Uiso 1 1 calc R . . . .
H24B H 0.609699 0.224661 0.314862 0.088 Uiso 1 1 calc R . . . .
C25 C 0.7512(9) 0.2012(3) 0.3798(3) 0.0556(19) Uani 1 1 d . . . . .
H25 H 0.757619 0.154886 0.396044 0.067 Uiso 1 1 calc R . . . .
C26 C 0.7334(8) 0.5415(3) 0.3564(4) 0.0525(18) Uani 1 1 d . . . . .
C27 C 0.6771(11) 0.6417(4) 0.3749(4) 0.075(3) Uani 1 1 d . . . . .
H27A H 0.704357 0.663526 0.330972 0.090 Uiso 1 1 calc R . . . .
H27B H 0.727177 0.667261 0.394996 0.090 Uiso 1 1 calc R . . . .
C28 C 0.5067(12) 0.6391(5) 0.3905(5) 0.096(3) Uani 1 1 d . . . . .
H28A H 0.456823 0.621305 0.364780 0.144 Uiso 1 1 calc GR . . . .
H28B H 0.471904 0.683507 0.384442 0.144 Uiso 1 1 calc GR . . . .
H28C H 0.479123 0.610912 0.432668 0.144 Uiso 1 1 calc GR . . . .
Fe1 Fe 0.83591(11) 0.24228(4) 0.48677(4) 0.0436(3) Uani 1 1 d . . . . .
N1 N 0.6191(7) 0.2185(3) 0.5284(2) 0.0496(14) Uani 1 1 d . . . . .
N2 N 0.6030(7) 0.1523(3) 0.5678(2) 0.0467(14) Uani 1 1 d . . . . .
N3 N 0.8543(7) 0.1493(3) 0.5299(2) 0.0454(13) Uani 1 1 d . . . . .
N4 N 1.1019(6) 0.1675(3) 0.4814(3) 0.0490(14) Uani 1 1 d . . . . .
N5 N 1.0582(7) 0.2335(2) 0.4587(2) 0.0485(14) Uani 1 1 d . . . . .
N6 N 0.8872(7) 0.2761(3) 0.5501(2) 0.0497(14) Uani 1 1 d . . . . .
N7 N 0.8728(7) 0.3437(3) 0.5329(2) 0.0480(14) Uani 1 1 d . . . . .
N8 N 0.8145(6) 0.3349(2) 0.4454(2) 0.0400(12) Uani 1 1 d . . . . .
N9 N 0.7572(7) 0.3046(2) 0.3677(2) 0.0472(14) Uani 1 1 d . . . . .
N10 N 0.7753(7) 0.2417(3) 0.4084(3) 0.0492(14) Uani 1 1 d . . . . .
O1 O 1.0145(8) -0.0851(3) 0.6137(3) 0.102(2) Uani 1 1 d . . . . .
O2 O 0.7860(8) -0.0850(2) 0.6700(3) 0.0773(17) Uani 1 1 d . . . . .
O3 O 0.7153(7) 0.5638(2) 0.3039(2) 0.0679(15) Uani 1 1 d . . . . .
O4 O 0.7319(6) 0.5741(2) 0.3946(2) 0.0662(15) Uani 1 1 d . . . . .
C29 C 0.7813(8) -0.1880(3) 1.1141(3) 0.0526(18) Uani 1 1 d . . . . .
H29 H 0.772770 -0.141863 1.097046 0.063 Uiso 1 1 calc R . . . .
C30 C 0.8234(10) -0.2221(4) 1.1731(4) 0.067(2) Uani 1 1 d . . . . .
H30 H 0.850921 -0.203516 1.200825 0.081 Uiso 1 1 calc R . . . .
C31 C 0.8150(9) -0.2898(4) 1.1809(3) 0.060(2) Uani 1 1 d . . . . .
H31 H 0.833279 -0.325831 1.215654 0.072 Uiso 1 1 calc R . . . .
C32 C 0.7549(8) -0.3477(3) 1.1089(3) 0.0437(16) Uani 1 1 d . . . . .
C34 C 0.7759(8) -0.4142(3) 1.1418(3) 0.0502(17) Uani 1 1 d . . . . .
H34 H 0.799376 -0.428269 1.181941 0.060 Uiso 1 1 calc R . . . .
C35 C 0.7606(8) -0.4581(3) 1.1129(3) 0.0438(16) Uani 1 1 d . . . . .
C36 C 0.7167(8) -0.4382(3) 1.0547(3) 0.0492(17) Uani 1 1 d . . . . .
H36 H 0.704249 -0.468440 1.035232 0.059 Uiso 1 1 calc R . . . .
C37 C 0.6921(8) -0.3705(3) 1.0270(3) 0.0466(16) Uani 1 1 d . . . . .
C38 C 0.6091(10) -0.3640(4) 0.9256(4) 0.067(2) Uani 1 1 d . . . . .
H38 H 0.611939 -0.408244 0.927895 0.080 Uiso 1 1 calc R . . . .
C39 C 0.5666(11) -0.3088(4) 0.8777(3) 0.074(2) Uani 1 1 d . . . . .
H39 H 0.532622 -0.309129 0.841752 0.088 Uiso 1 1 calc R . . . .
C40 C 0.5845(9) -0.2535(4) 0.8939(3) 0.0578(19) Uani 1 1 d . . . . .
H40 H 0.568451 -0.209769 0.868881 0.069 Uiso 1 1 calc R . . . .
C41 C 0.7906(9) -0.5315(4) 1.1465(4) 0.058(2) Uani 1 1 d . . . . .
C42 C 0.8272(12) -0.6362(4) 1.1310(5) 0.096(3) Uani 1 1 d . . . . .
H42A H 0.813149 -0.655320 1.175421 0.115 Uiso 1 1 calc R . . . .
H42B H 0.759337 -0.661488 1.115964 0.115 Uiso 1 1 calc R . . . .
C43 C 0.9840(14) -0.6400(6) 1.1088(6) 0.122(4) Uani 1 1 d . . . . .
H43A H 1.007842 -0.606543 1.068517 0.183 Uiso 1 1 calc GR . . . .
H43B H 1.000505 -0.683609 1.106842 0.183 Uiso 1 1 calc GR . . . .
H43C H 1.051619 -0.632374 1.135678 0.183 Uiso 1 1 calc GR . . . .
C44 C 0.3432(9) -0.2646(4) 1.0795(3) 0.059(2) Uani 1 1 d . . . . .
H44 H 0.343087 -0.310428 1.101616 0.070 Uiso 1 1 calc R . . . .
C45 C 0.2160(9) -0.2256(4) 1.0820(4) 0.070(2) Uani 1 1 d . . . . .
H45 H 0.118367 -0.239883 1.105175 0.084 Uiso 1 1 calc R . . . .
C46 C 0.2619(9) -0.1612(4) 1.0436(3) 0.060(2) Uani 1 1 d . . . . .
H46 H 0.202046 -0.123352 1.035704 0.072 Uiso 1 1 calc R . . . .
C47 C 0.5176(8) -0.1146(3) 0.9773(3) 0.0436(16) Uani 1 1 d . . . . .
C48 C 0.4915(8) -0.0493(3) 0.9477(3) 0.0515(18) Uani 1 1 d . . . . .
H48 H 0.396572 -0.030951 0.955735 0.062 Uiso 1 1 calc R . . . .
C49 C 0.6127(9) -0.0103(3) 0.9045(3) 0.0493(17) Uani 1 1 d . . . . .
C50 C 0.7549(8) -0.0370(3) 0.8918(3) 0.0475(17) Uani 1 1 d . . . . .
H50 H 0.834683 -0.011454 0.862388 0.057 Uiso 1 1 calc R . . . .
C51 C 0.7699(8) -0.1037(3) 0.9258(3) 0.0452(16) Uani 1 1 d . . . . .
C52 C 1.0506(10) -0.1246(4) 0.8919(4) 0.072(2) Uani 1 1 d . . . . .
H52 H 1.084159 -0.083478 0.861898 0.087 Uiso 1 1 calc R . . . .
C53 C 1.1382(9) -0.1782(4) 0.9105(4) 0.073(2) Uani 1 1 d . . . . .
H53 H 1.242921 -0.181460 0.896426 0.088 Uiso 1 1 calc R . . . .
C54 C 1.0412(9) -0.2278(4) 0.9549(3) 0.0563(19) Uani 1 1 d . . . . .
H54 H 1.071378 -0.270953 0.975910 0.068 Uiso 1 1 calc R . . . .
C55 C 0.5889(11) 0.0630(4) 0.8732(4) 0.064(2) Uani 1 1 d . . . . .
C56A C 0.658(3) 0.1628(11) 0.7886(11) 0.075(7) Uiso 0.5 1 d . . . B 1
H56A H 0.756248 0.188980 0.771521 0.090 Uiso 0.5 1 calc R . . B 1
H56B H 0.597113 0.183544 0.813957 0.090 Uiso 0.5 1 calc R . . B 1
C56B C 0.707(3) 0.1663(12) 0.7979(11) 0.087(8) Uiso 0.5 1 d . . . B 2
H56C H 0.814469 0.181998 0.780070 0.104 Uiso 0.5 1 calc R . . B 2
H56D H 0.670292 0.188271 0.826226 0.104 Uiso 0.5 1 calc R . . B 2
C57A C 0.558(3) 0.1624(15) 0.7321(12) 0.125(11) Uiso 0.5 1 d . . . B 1
H57A H 0.456449 0.140595 0.749085 0.188 Uiso 0.5 1 calc GR . . B 1
H57B H 0.614914 0.138725 0.709076 0.188 Uiso 0.5 1 calc GR . . B 1
H57C H 0.545397 0.207678 0.705590 0.188 Uiso 0.5 1 calc GR . . B 1
C57B C 0.594(3) 0.1763(11) 0.7471(11) 0.083(6) Uiso 0.5 1 d . . . B 2
H57D H 0.490397 0.158170 0.766382 0.125 Uiso 0.5 1 calc GR . . B 2
H57E H 0.633626 0.153570 0.720269 0.125 Uiso 0.5 1 calc GR . . B 2
H57F H 0.588650 0.223248 0.723860 0.125 Uiso 0.5 1 calc GR . . B 2
Fe2 Fe 0.68657(11) -0.23404(4) 1.01015(4) 0.0430(3) Uani 1 1 d . . . . .
N11 N 0.7557(6) -0.2298(2) 1.0862(2) 0.0468(14) Uani 1 1 d . . . . .
N12 N 0.7756(7) -0.2927(3) 1.1289(2) 0.0473(14) Uani 1 1 d . . . . .
N13 N 0.7158(6) -0.3254(2) 1.0526(2) 0.0384(12) Uani 1 1 d . . . . .
N14 N 0.6455(7) -0.3393(3) 0.9683(2) 0.0480(14) Uani 1 1 d . . . . .
N15 N 0.6281(7) -0.2711(3) 0.9504(2) 0.0513(15) Uani 1 1 d . . . . .
N16 N 0.4651(7) -0.2295(3) 1.0420(3) 0.0504(14) Uani 1 1 d . . . . .
N17 N 0.4133(7) -0.1644(3) 1.0194(3) 0.0514(14) Uani 1 1 d . . . . .
N18 N 0.6571(6) -0.1419(3) 0.9669(2) 0.0424(13) Uani 1 1 d . . . . .
N19 N 0.9062(7) -0.1398(3) 0.9234(2) 0.0468(14) Uani 1 1 d . . . . .
N20 N 0.8989(7) -0.2051(3) 0.9635(2) 0.0476(14) Uani 1 1 d . . . . .
O5 O 0.8126(7) -0.5530(3) 1.1986(3) 0.0779(17) Uani 1 1 d . . . . .
O6 O 0.7852(7) -0.5663(2) 1.1105(3) 0.0763(17) Uani 1 1 d . . . . .
O7 O 0.4824(8) 0.0903(3) 0.8927(3) 0.100(2) Uani 1 1 d . . . . .
O8 O 0.6929(8) 0.0921(3) 0.8275(3) 0.090(2) Uani 1 1 d . . . . .
C58 C 0.6078(17) 0.3849(8) 0.7646(6) 0.067(4) Uani 0.5 1 d . . . . .
H58A H 0.551624 0.344770 0.767794 0.100 Uiso 0.5 1 calc GR . . . .
H58B H 0.581950 0.421428 0.729494 0.100 Uiso 0.5 1 calc GR . . . .
H58C H 0.578576 0.394957 0.800930 0.100 Uiso 0.5 1 calc GR . . . .
C59 C 0.7810(16) 0.3750(7) 0.7578(5) 0.041(3) Uani 0.5 1 d . . . . .
C60 C 0.8712(18) 0.4358(7) 0.7443(7) 0.070(5) Uani 0.5 1 d . . . . .
H60A H 0.980821 0.428441 0.735941 0.105 Uiso 0.5 1 calc GR . . . .
H60B H 0.855695 0.450065 0.778743 0.105 Uiso 0.5 1 calc GR . . . .
H60C H 0.837790 0.469846 0.709035 0.105 Uiso 0.5 1 calc GR . . . .
O29 O 0.8388(14) 0.3231(5) 0.7636(4) 0.073(3) Uani 0.5 1 d . . . . .
C61 C 0.4696(17) -0.0450(11) 0.7728(6) 0.082(7) Uani 0.5 1 d . . . . .
H61A H 0.496370 -0.066346 0.813673 0.123 Uiso 0.5 1 calc GR . . . .
H61B H 0.397220 -0.010448 0.772125 0.123 Uiso 0.5 1 calc GR . . . .
H61C H 0.563247 -0.025637 0.745367 0.123 Uiso 0.5 1 calc GR . . . .
C62 C 0.4045(15) -0.0890(6) 0.7558(6) 0.043(4) Uani 0.5 1 d . . . . .
C63 C 0.3423(16) -0.0688(6) 0.6969(6) 0.052(4) Uani 0.5 1 d . . . . .
H63A H 0.427766 -0.054422 0.664232 0.078 Uiso 0.5 1 calc GR . . . .
H63B H 0.272904 -0.032660 0.693341 0.078 Uiso 0.5 1 calc GR . . . .
H63C H 0.285222 -0.106169 0.694353 0.078 Uiso 0.5 1 calc GR . . . .
O30 O 0.4120(14) -0.1468(7) 0.7842(5) 0.092(4) Uani 0.5 1 d . . . . .
C64 C 1.4013(17) 0.4294(8) 0.2342(8) 0.078(6) Uani 0.5 1 d . . . . .
H64A H 1.400419 0.452404 0.190968 0.118 Uiso 0.5 1 calc GR . . . .
H64B H 1.507402 0.418986 0.242541 0.118 Uiso 0.5 1 calc GR . . . .
H64C H 1.359754 0.457411 0.255810 0.118 Uiso 0.5 1 calc GR . . . .
C65 C 1.3045(18) 0.3675(7) 0.2544(5) 0.048(4) Uani 0.5 1 d . . . . .
C66 C 1.1357(18) 0.3725(9) 0.2656(8) 0.080(5) Uani 0.5 1 d . . . . .
H66A H 1.104617 0.414123 0.237397 0.120 Uiso 0.5 1 calc GR . . . .
H66B H 1.107744 0.370830 0.306840 0.120 Uiso 0.5 1 calc GR . . . .
H66C H 1.083004 0.335896 0.260118 0.120 Uiso 0.5 1 calc GR . . . .
O31 O 1.3736(14) 0.3165(5) 0.2612(4) 0.068(3) Uani 0.5 1 d . . . . .
Cl1 Cl 0.500000 0.000000 0.500000 0.0782(9) Uani 1 2 d S T P . .
O9 O 0.4295(17) 0.0307(7) 0.5399(6) 0.089(4) Uani 0.5 1 d . . . . .
O10 O 0.6610(16) 0.0069(11) 0.4948(10) 0.143(7) Uani 0.5 1 d . . . . .
O11 O 0.547(2) 0.0638(8) 0.4862(9) 0.122(5) Uani 0.5 1 d . . . . .
O12 O 0.456(2) 0.0457(7) 0.4389(6) 0.115(5) Uani 0.5 1 d . . . . .
Cl2 Cl 1.000000 0.000000 1.000000 0.0739(9) Uani 1 2 d S T P . .
O13 O 1.083(2) -0.0260(10) 0.9599(8) 0.119(5) Uani 0.5 1 d . . . . .
O14 O 1.048(2) -0.0486(6) 1.0639(7) 0.113(5) Uani 0.5 1 d . . . . .
O15 O 1.029(2) 0.0643(6) 0.9966(8) 0.104(5) Uani 0.5 1 d . . . . .
O16 O 1.1628(15) 0.0105(8) 0.9950(8) 0.114(5) Uani 0.5 1 d . . . . .
Cl3 Cl 1.2395(3) 0.56284(12) 0.06789(12) 0.0826(7) Uani 1 1 d . . . . .
O17 O 1.3426(12) 0.5761(4) 0.1066(4) 0.143(3) Uani 1 1 d . . . . .
O18A O 1.3431(14) 0.5327(6) 0.0318(5) 0.095(3) Uiso 0.6 1 d . U . C 1
O18B O 1.339(5) 0.605(2) 0.0102(18) 0.265(17) Uiso 0.4 1 d . U . C 2
O19A O 1.1294(18) 0.5123(7) 0.1092(7) 0.132(5) Uiso 0.6 1 d . U . C 1
O19B O 1.193(5) 0.5097(19) 0.0645(19) 0.236(15) Uiso 0.4 1 d . U . C 2
O20A O 1.207(3) 0.6226(9) 0.0228(10) 0.168(7) Uiso 0.6 1 d . U . C 1
O20B O 1.115(3) 0.6120(10) 0.0542(10) 0.121(7) Uiso 0.4 1 d . U . C 2
Cl4 Cl 1.0515(4) 0.07477(16) 0.72386(13) 0.1133(11) Uani 1 1 d D . . . .
O21A O 0.8920(14) 0.0864(6) 0.7023(5) 0.122(4) Uiso 0.6 1 d D U . D 1
O21B O 1.225(2) 0.0895(14) 0.7136(13) 0.207(11) Uiso 0.4 1 d D U . D 2
O22A O 1.0659(18) 0.0176(7) 0.7749(6) 0.128(5) Uiso 0.6 1 d D U . D 1
O22B O 0.956(3) 0.0129(10) 0.7568(12) 0.184(10) Uiso 0.4 1 d D U . D 2
O23A O 1.1560(17) 0.0651(7) 0.6750(6) 0.123(5) Uiso 0.6 1 d D U . D 1
O23B O 1.042(5) 0.061(2) 0.7888(9) 0.278(16) Uiso 0.4 1 d D U . D 2
O24A O 1.0381(19) 0.1391(7) 0.7317(7) 0.158(6) Uiso 0.6 1 d D U . D 1
O24B O 1.082(4) 0.0906(18) 0.6591(9) 0.235(16) Uiso 0.4 1 d D U . D 2
Cl5 Cl 1.2774(3) 0.43824(12) 0.42801(12) 0.0813(7) Uani 1 1 d D . . . .
O25A O 1.1650(12) 0.4255(5) 0.3900(4) 0.075(3) Uiso 0.6 1 d D U . E 1
O25B O 1.198(4) 0.3913(13) 0.4843(10) 0.170(11) Uiso 0.4 1 d D U . E 2
O26A O 1.1738(16) 0.4723(7) 0.4576(6) 0.116(4) Uiso 0.6 1 d D U . E 1
O26B O 1.288(5) 0.5040(10) 0.4259(17) 0.213(13) Uiso 0.4 1 d D U . E 2
O27A O 1.397(2) 0.4891(9) 0.3879(8) 0.189(7) Uiso 0.6 1 d D U . E 1
O27B O 1.266(4) 0.4264(16) 0.3734(11) 0.225(14) Uiso 0.4 1 d D U . E 2
O28A O 1.410(2) 0.4010(10) 0.4409(9) 0.195(8) Uiso 0.6 1 d D U . E 1
O28B O 1.283(3) 0.3752(9) 0.4758(9) 0.122(7) Uiso 0.4 1 d D U . E 2


_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 H1 0.9300 . ?
C1 C2 1.382(10) . ?
C1 N1 1.325(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.323(10) . ?
C3 H3 0.9300 . ?
C3 N2 1.366(9) . ?
C4 C5 1.367(8) . ?
C4 N2 1.387(8) . ?
C4 N3 1.337(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(9) . ?
C6 C7 1.392(9) . ?
C6 C12 1.497(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.386(8) . ?
C8 N3 1.339(8) . ?
C8 N4 1.394(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.366(10) . ?
C9 N4 1.349(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.361(10) . ?
C11 H11 0.9300 . ?
C11 N5 1.319(8) . ?
C12 O1 1.182(9) . ?
C12 O2 1.325(10) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C13A C14A 1.63(3) . ?
C13A O2 1.50(2) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C13B C14B 1.65(3) . ?
C13B O2 1.45(2) . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15 H15 0.9300 . ?
C15 C16 1.379(10) . ?
C15 N6 1.336(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.398(10) . ?
C17 H17 0.9300 . ?
C17 N7 1.351(9) . ?
C18 C19 1.381(8) . ?
C18 N7 1.396(8) . ?
C18 N8 1.341(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.370(9) . ?
C20 C21 1.401(9) . ?
C20 C26 1.527(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.380(8) . ?
C22 N8 1.330(8) . ?
C22 N9 1.412(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.358(10) . ?
C23 N9 1.322(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.420(10) . ?
C25 H25 0.9300 . ?
C25 N10 1.305(8) . ?
C26 O3 1.182(8) . ?
C26 O4 1.321(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.458(12) . ?
C27 O4 1.447(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Fe1 N1 1.971(6) . ?
Fe1 N3 1.898(5) . ?
Fe1 N5 1.971(6) . ?
Fe1 N6 1.967(6) . ?
Fe1 N8 1.889(5) . ?
Fe1 N10 1.977(6) . ?
N1 N2 1.384(7) . ?
N4 N5 1.385(7) . ?
N6 N7 1.364(7) . ?
N9 N10 1.365(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.406(10) . ?
C29 N11 1.317(8) . ?
C30 H30 0.9300 . ?
C30 C31 1.393(10) . ?
C31 H31 0.9300 . ?
C31 N12 1.330(8) . ?
C32 C34 1.377(8) . ?
C32 N12 1.434(8) . ?
C32 N13 1.321(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.356(9) . ?
C35 C36 1.379(9) . ?
C35 C41 1.522(9) . ?
C36 H36 0.9300 . ?
C36 C37 1.386(9) . ?
C37 N13 1.336(8) . ?
C37 N14 1.406(8) . ?
C38 H38 0.9300 . ?
C38 C39 1.392(10) . ?
C38 N14 1.356(9) . ?
C39 H39 0.9300 . ?
C39 C40 1.378(11) . ?
C40 H40 0.9300 . ?
C40 N15 1.344(8) . ?
C41 O5 1.184(9) . ?
C41 O6 1.319(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.396(13) . ?
C42 O6 1.455(9) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44 0.9300 . ?
C44 C45 1.380(10) . ?
C44 N16 1.321(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.377(10) . ?
C46 H46 0.9300 . ?
C46 N17 1.365(8) . ?
C47 C48 1.350(8) . ?
C47 N17 1.400(8) . ?
C47 N18 1.363(8) . ?
C48 H48 0.9300 . ?
C48 C49 1.399(9) . ?
C49 C50 1.389(9) . ?
C49 C55 1.500(9) . ?
C50 H50 0.9300 . ?
C50 C51 1.378(8) . ?
C51 N18 1.325(8) . ?
C51 N19 1.405(8) . ?
C52 H52 0.9300 . ?
C52 C53 1.333(11) . ?
C52 N19 1.341(9) . ?
C53 H53 0.9300 . ?
C53 C54 1.385(10) . ?
C54 H54 0.9300 . ?
C54 N20 1.330(8) . ?
C55 O7 1.214(9) . ?
C55 O8 1.280(9) . ?
C56A H56A 0.9700 . ?
C56A H56B 0.9700 . ?
C56A C57A 1.67(3) . ?
C56A O8 1.51(2) . ?
C56B H56C 0.9700 . ?
C56B H56D 0.9700 . ?
C56B C57B 1.58(3) . ?
C56B O8 1.49(2) . ?
C57A H57A 0.9600 . ?
C57A H57B 0.9600 . ?
C57A H57C 0.9600 . ?
C57B H57D 0.9600 . ?
C57B H57E 0.9600 . ?
C57B H57F 0.9600 . ?
Fe2 N11 1.981(6) . ?
Fe2 N13 1.880(5) . ?
Fe2 N15 1.956(6) . ?
Fe2 N16 1.971(6) . ?
Fe2 N18 1.899(5) . ?
Fe2 N20 1.987(6) . ?
N11 N12 1.387(7) . ?
N14 N15 1.379(7) . ?
N16 N17 1.393(7) . ?
N19 N20 1.373(7) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C58 C59 1.495(19) . ?
C59 C60 1.43(2) . ?
C59 O29 1.184(15) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C61 C62 1.30(2) . ?
C62 C63 1.462(18) . ?
C62 O30 1.181(15) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C64 C65 1.46(2) . ?
C65 C66 1.45(2) . ?
C65 O31 1.207(15) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
Cl1 O9 1.411(12) . ?
Cl1 O9 1.411(12) 2_656 ?
Cl1 O10 1.372(14) 2_656 ?
Cl1 O10 1.372(14) . ?
Cl1 O11 1.335(16) . ?
Cl1 O11 1.335(16) 2_656 ?
Cl1 O12 1.510(13) 2_656 ?
Cl1 O12 1.510(13) . ?
O9 O10 1.593(19) 2_656 ?
O9 O11 1.47(2) . ?
O10 O11 1.53(2) . ?
O10 O12 1.76(2) 2_656 ?
O11 O12 1.58(2) . ?
Cl2 O13 1.387(15) 2_757 ?
Cl2 O13 1.387(15) . ?
Cl2 O14 1.593(13) . ?
Cl2 O14 1.593(13) 2_757 ?
Cl2 O15 1.371(12) 2_757 ?
Cl2 O15 1.371(12) . ?
Cl2 O16 1.396(13) 2_757 ?
Cl2 O16 1.396(13) . ?
O13 O15 1.348(19) 2_757 ?
O13 O16 1.53(2) . ?
O14 O15 1.775(19) 2_757 ?
O15 O16 1.626(19) . ?
Cl3 O17 1.436(8) . ?
Cl3 O18A 1.462(11) . ?
Cl3 O18B 1.50(4) . ?
Cl3 O19A 1.428(15) . ?
Cl3 O19B 1.24(4) . ?
Cl3 O20A 1.390(19) . ?
Cl3 O20B 1.47(2) . ?
Cl4 O21A 1.500(11) . ?
Cl4 O21B 1.496(18) . ?
Cl4 O22A 1.391(11) . ?
Cl4 O22B 1.462(17) . ?
Cl4 O23A 1.449(11) . ?
Cl4 O23B 1.444(19) . ?
Cl4 O24A 1.455(13) . ?
Cl4 O24B 1.431(18) . ?
O22B O23B 1.69(4) . ?
Cl5 O25A 1.476(9) . ?
Cl5 O25B 1.436(17) . ?
Cl5 O26A 1.422(11) . ?
Cl5 O26B 1.391(18) . ?
Cl5 O27A 1.473(15) . ?
Cl5 O27B 1.411(18) . ?
Cl5 O28A 1.382(15) . ?
Cl5 O28B 1.418(15) . ?
O25B O28B 0.84(3) . ?

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
C2 C1 H1 124.9 . . ?
N1 C1 H1 124.9 . . ?
N1 C1 C2 110.1(6) . . ?
C1 C2 H2 126.4 . . ?
C3 C2 C1 107.3(7) . . ?
C3 C2 H2 126.4 . . ?
C2 C3 H3 125.9 . . ?
C2 C3 N2 108.3(7) . . ?
N2 C3 H3 125.9 . . ?
C5 C4 N2 128.0(6) . . ?
N3 C4 C5 121.4(6) . . ?
N3 C4 N2 110.6(6) . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.6(7) . . ?
C6 C5 H5 120.7 . . ?
C5 C6 C12 122.3(7) . . ?
C7 C6 C5 120.4(6) . . ?
C7 C6 C12 117.3(7) . . ?
C6 C7 H7 121.5 . . ?
C8 C7 C6 117.0(6) . . ?
C8 C7 H7 121.5 . . ?
C7 C8 N4 126.9(6) . . ?
N3 C8 C7 122.1(6) . . ?
N3 C8 N4 110.8(6) . . ?
C10 C9 H9 126.8 . . ?
N4 C9 H9 126.8 . . ?
N4 C9 C10 106.4(7) . . ?
C9 C10 H10 126.9 . . ?
C11 C10 C9 106.2(7) . . ?
C11 C10 H10 126.9 . . ?
C10 C11 H11 123.6 . . ?
N5 C11 C10 112.8(7) . . ?
N5 C11 H11 123.6 . . ?
O1 C12 C6 122.4(8) . . ?
O1 C12 O2 125.7(7) . . ?
O2 C12 C6 111.9(7) . . ?
H13A C13A H13B 109.9 . . ?
C14A C13A H13A 112.3 . . ?
C14A C13A H13B 112.3 . . ?
O2 C13A H13A 112.3 . . ?
O2 C13A H13B 112.3 . . ?
O2 C13A C14A 97.5(15) . . ?
H13C C13B H13D 108.0 . . ?
C14B C13B H13C 109.4 . . ?
C14B C13B H13D 109.4 . . ?
O2 C13B H13C 109.4 . . ?
O2 C13B H13D 109.4 . . ?
O2 C13B C14B 111.0(15) . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C16 C15 H15 124.7 . . ?
N6 C15 H15 124.7 . . ?
N6 C15 C16 110.6(7) . . ?
C15 C16 H16A 110.5 . . ?
C15 C16 H16B 110.5 . . ?
C15 C16 C17 106.1(7) . . ?
H16A C16 H16B 108.7 . . ?
C17 C16 H16A 110.5 . . ?
C17 C16 H16B 110.5 . . ?
C16 C17 H17 126.9 . . ?
N7 C17 C16 106.1(7) . . ?
N7 C17 H17 126.9 . . ?
C19 C18 N7 127.8(6) . . ?
N8 C18 C19 122.0(6) . . ?
N8 C18 N7 110.1(5) . . ?
C18 C19 H19 121.2 . . ?
C20 C19 C18 117.6(6) . . ?
C20 C19 H19 121.2 . . ?
C19 C20 C21 121.7(6) . . ?
C19 C20 C26 121.1(6) . . ?
C21 C20 C26 117.2(6) . . ?
C20 C21 H21 122.0 . . ?
C22 C21 C20 115.9(6) . . ?
C22 C21 H21 122.0 . . ?
C21 C22 N9 126.3(6) . . ?
N8 C22 C21 123.3(6) . . ?
N8 C22 N9 110.4(5) . . ?
C24 C23 H23 126.4 . . ?
N9 C23 H23 126.4 . . ?
N9 C23 C24 107.2(7) . . ?
C23 C24 H24A 110.7 . . ?
C23 C24 H24B 110.7 . . ?
C23 C24 C25 105.3(7) . . ?
H24A C24 H24B 108.8 . . ?
C25 C24 H24A 110.7 . . ?
C25 C24 H24B 110.7 . . ?
C24 C25 H25 125.0 . . ?
N10 C25 C24 110.0(6) . . ?
N10 C25 H25 125.0 . . ?
O3 C26 C20 122.6(7) . . ?
O3 C26 O4 127.3(7) . . ?
O4 C26 C20 110.1(6) . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
O4 C27 H27A 109.9 . . ?
O4 C27 H27B 109.9 . . ?
O4 C27 C28 109.1(7) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 Fe1 N5 160.8(2) . . ?
N1 Fe1 N10 92.5(2) . . ?
N3 Fe1 N1 80.2(2) . . ?
N3 Fe1 N5 80.6(2) . . ?
N3 Fe1 N6 98.9(2) . . ?
N3 Fe1 N10 101.0(2) . . ?
N5 Fe1 N10 90.1(2) . . ?
N6 Fe1 N1 90.2(2) . . ?
N6 Fe1 N5 93.8(2) . . ?
N6 Fe1 N10 160.1(2) . . ?
N8 Fe1 N1 98.7(2) . . ?
N8 Fe1 N3 178.7(2) . . ?
N8 Fe1 N5 100.5(2) . . ?
N8 Fe1 N6 80.2(2) . . ?
N8 Fe1 N10 79.9(2) . . ?
C1 N1 Fe1 142.3(5) . . ?
C1 N1 N2 105.9(6) . . ?
N2 N1 Fe1 111.7(4) . . ?
C3 N2 C4 134.3(6) . . ?
C3 N2 N1 108.4(6) . . ?
N1 N2 C4 117.3(5) . . ?
C4 N3 C8 120.4(6) . . ?
C4 N3 Fe1 120.0(5) . . ?
C8 N3 Fe1 119.7(5) . . ?
C9 N4 C8 131.6(6) . . ?
C9 N4 N5 111.1(6) . . ?
N5 N4 C8 117.2(5) . . ?
C11 N5 Fe1 144.3(5) . . ?
C11 N5 N4 103.6(5) . . ?
N4 N5 Fe1 111.6(4) . . ?
C15 N6 Fe1 141.6(5) . . ?
C15 N6 N7 106.0(6) . . ?
N7 N6 Fe1 112.2(4) . . ?
C17 N7 C18 131.5(6) . . ?
C17 N7 N6 111.1(6) . . ?
N6 N7 C18 117.4(5) . . ?
C18 N8 Fe1 120.0(4) . . ?
C22 N8 C18 119.3(5) . . ?
C22 N8 Fe1 120.7(4) . . ?
C23 N9 C22 131.7(6) . . ?
C23 N9 N10 111.9(5) . . ?
N10 N9 C22 116.4(5) . . ?
C25 N10 Fe1 141.7(5) . . ?
C25 N10 N9 105.6(5) . . ?
N9 N10 Fe1 112.6(4) . . ?
C12 O2 C13A 117.3(10) . . ?
C12 O2 C13B 117.0(10) . . ?
C26 O4 C27 118.0(6) . . ?
C30 C29 H29 124.3 . . ?
N11 C29 H29 124.3 . . ?
N11 C29 C30 111.4(6) . . ?
C29 C30 H30 127.4 . . ?
C31 C30 C29 105.2(7) . . ?
C31 C30 H30 127.4 . . ?
C30 C31 H31 126.8 . . ?
N12 C31 C30 106.4(7) . . ?
N12 C31 H31 126.8 . . ?
C34 C32 N12 126.1(6) . . ?
N13 C32 C34 124.0(6) . . ?
N13 C32 N12 110.0(5) . . ?
C32 C34 H34 121.6 . . ?
C35 C34 C32 116.9(6) . . ?
C35 C34 H34 121.6 . . ?
C34 C35 C36 122.0(6) . . ?
C34 C35 C41 118.6(6) . . ?
C36 C35 C41 119.4(6) . . ?
C35 C36 H36 122.0 . . ?
C35 C36 C37 116.1(6) . . ?
C37 C36 H36 122.0 . . ?
C36 C37 N14 125.9(6) . . ?
N13 C37 C36 123.4(6) . . ?
N13 C37 N14 110.7(5) . . ?
C39 C38 H38 127.4 . . ?
N14 C38 H38 127.4 . . ?
N14 C38 C39 105.2(7) . . ?
C38 C39 H39 126.5 . . ?
C40 C39 C38 106.9(7) . . ?
C40 C39 H39 126.5 . . ?
C39 C40 H40 124.4 . . ?
N15 C40 C39 111.2(7) . . ?
N15 C40 H40 124.4 . . ?
O5 C41 C35 122.7(7) . . ?
O5 C41 O6 126.2(7) . . ?
O6 C41 C35 111.1(6) . . ?
H42A C42 H42B 108.3 . . ?
C43 C42 H42A 109.9 . . ?
C43 C42 H42B 109.9 . . ?
C43 C42 O6 109.1(8) . . ?
O6 C42 H42A 109.9 . . ?
O6 C42 H42B 109.9 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 H44 123.9 . . ?
N16 C44 H44 123.9 . . ?
N16 C44 C45 112.2(7) . . ?
C44 C45 H45 126.7 . . ?
C46 C45 C44 106.6(7) . . ?
C46 C45 H45 126.7 . . ?
C45 C46 H46 127.1 . . ?
N17 C46 C45 105.8(7) . . ?
N17 C46 H46 127.1 . . ?
C48 C47 N17 128.4(6) . . ?
C48 C47 N18 122.0(6) . . ?
N18 C47 N17 109.5(5) . . ?
C47 C48 H48 121.3 . . ?
C47 C48 C49 117.4(6) . . ?
C49 C48 H48 121.3 . . ?
C48 C49 C55 118.2(7) . . ?
C50 C49 C48 122.0(6) . . ?
C50 C49 C55 119.7(7) . . ?
C49 C50 H50 122.2 . . ?
C51 C50 C49 115.6(6) . . ?
C51 C50 H50 122.2 . . ?
C50 C51 N19 125.4(6) . . ?
N18 C51 C50 123.8(6) . . ?
N18 C51 N19 110.8(5) . . ?
C53 C52 H52 125.5 . . ?
C53 C52 N19 108.9(7) . . ?
N19 C52 H52 125.5 . . ?
C52 C53 H53 127.1 . . ?
C52 C53 C54 105.9(7) . . ?
C54 C53 H53 127.1 . . ?
C53 C54 H54 124.8 . . ?
N20 C54 C53 110.5(6) . . ?
N20 C54 H54 124.8 . . ?
O7 C55 C49 120.7(8) . . ?
O7 C55 O8 125.6(7) . . ?
O8 C55 C49 113.6(7) . . ?
H56A C56A H56B 108.1 . . ?
C57A C56A H56A 109.6 . . ?
C57A C56A H56B 109.6 . . ?
O8 C56A H56A 109.6 . . ?
O8 C56A H56B 109.6 . . ?
O8 C56A C57A 110.3(16) . . ?
H56C C56B H56D 109.6 . . ?
C57B C56B H56C 111.9 . . ?
C57B C56B H56D 111.9 . . ?
O8 C56B H56C 111.9 . . ?
O8 C56B H56D 111.9 . . ?
O8 C56B C57B 99.3(16) . . ?
C56A C57A H57A 109.5 . . ?
C56A C57A H57B 109.5 . . ?
C56A C57A H57C 109.5 . . ?
H57A C57A H57B 109.5 . . ?
H57A C57A H57C 109.5 . . ?
H57B C57A H57C 109.5 . . ?
C56B C57B H57D 109.5 . . ?
C56B C57B H57E 109.5 . . ?
C56B C57B H57F 109.5 . . ?
H57D C57B H57E 109.5 . . ?
H57D C57B H57F 109.5 . . ?
H57E C57B H57F 109.5 . . ?
N11 Fe2 N20 92.5(2) . . ?
N13 Fe2 N11 79.8(2) . . ?
N13 Fe2 N15 80.3(2) . . ?
N13 Fe2 N16 99.2(2) . . ?
N13 Fe2 N18 179.7(2) . . ?
N13 Fe2 N20 100.6(2) . . ?
N15 Fe2 N11 160.1(2) . . ?
N15 Fe2 N16 92.6(2) . . ?
N15 Fe2 N20 91.3(2) . . ?
N16 Fe2 N11 90.4(2) . . ?
N16 Fe2 N20 160.1(2) . . ?
N18 Fe2 N11 100.4(2) . . ?
N18 Fe2 N15 99.4(2) . . ?
N18 Fe2 N16 80.9(2) . . ?
N18 Fe2 N20 79.3(2) . . ?
C29 N11 Fe2 142.7(5) . . ?
C29 N11 N12 104.5(6) . . ?
N12 N11 Fe2 112.5(4) . . ?
C31 N12 C32 132.2(6) . . ?
C31 N12 N11 112.4(6) . . ?
N11 N12 C32 115.4(5) . . ?
C32 N13 C37 117.5(5) . . ?
C32 N13 Fe2 122.1(4) . . ?
C37 N13 Fe2 120.3(4) . . ?
C38 N14 C37 132.0(6) . . ?
C38 N14 N15 112.4(6) . . ?
N15 N14 C37 115.6(5) . . ?
C40 N15 Fe2 142.6(5) . . ?
C40 N15 N14 104.2(6) . . ?
N14 N15 Fe2 113.0(4) . . ?
C44 N16 Fe2 144.2(5) . . ?
C44 N16 N17 104.2(6) . . ?
N17 N16 Fe2 111.5(4) . . ?
C46 N17 C47 130.8(6) . . ?
C46 N17 N16 111.1(6) . . ?
N16 N17 C47 118.0(5) . . ?
C47 N18 Fe2 120.0(4) . . ?
C51 N18 C47 119.2(6) . . ?
C51 N18 Fe2 120.8(5) . . ?
C52 N19 C51 134.5(6) . . ?
C52 N19 N20 109.4(6) . . ?
N20 N19 C51 116.0(5) . . ?
C54 N20 Fe2 142.0(5) . . ?
C54 N20 N19 105.3(6) . . ?
N19 N20 Fe2 112.7(4) . . ?
C41 O6 C42 120.5(7) . . ?
C55 O8 C56A 115.1(10) . . ?
C55 O8 C56B 121.5(12) . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
C59 C58 H58C 109.5 . . ?
C60 C59 C58 112.1(13) . . ?
O29 C59 C58 124.8(15) . . ?
O29 C59 C60 123.1(14) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
C61 C62 C63 120.7(12) . . ?
O30 C62 C61 120.0(16) . . ?
O30 C62 C63 118.7(15) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
C66 C65 C64 117.4(13) . . ?
O31 C65 C64 116.5(14) . . ?
O31 C65 C66 126.1(15) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O9 Cl1 O9 180.0 2_656 . ?
O9 Cl1 O12 101.8(7) 2_656 2_656 ?
O9 Cl1 O12 78.2(7) 2_656 . ?
O9 Cl1 O12 101.8(7) . . ?
O9 Cl1 O12 78.2(7) . 2_656 ?
O10 Cl1 O9 69.8(8) 2_656 . ?
O10 Cl1 O9 110.2(8) 2_656 2_656 ?
O10 Cl1 O9 69.8(8) . 2_656 ?
O10 Cl1 O9 110.2(8) . . ?
O10 Cl1 O10 180.0 . 2_656 ?
O10 Cl1 O12 105.0(11) 2_656 2_656 ?
O10 Cl1 O12 75.0(11) . 2_656 ?
O10 Cl1 O12 105.0(11) . . ?
O10 Cl1 O12 75.0(11) 2_656 . ?
O11 Cl1 O9 64.9(9) . . ?
O11 Cl1 O9 64.9(9) 2_656 2_656 ?
O11 Cl1 O9 115.1(9) 2_656 . ?
O11 Cl1 O9 115.1(9) . 2_656 ?
O11 Cl1 O10 68.8(10) . . ?
O11 Cl1 O10 111.2(10) . 2_656 ?
O11 Cl1 O10 111.2(10) 2_656 . ?
O11 Cl1 O10 68.8(10) 2_656 2_656 ?
O11 Cl1 O11 180.0 2_656 . ?
O11 Cl1 O12 67.2(9) . . ?
O11 Cl1 O12 112.8(9) . 2_656 ?
O11 Cl1 O12 67.2(9) 2_656 2_656 ?
O11 Cl1 O12 112.8(9) 2_656 . ?
O12 Cl1 O12 180.0(14) . 2_656 ?
Cl1 O9 O10 54.0(7) . 2_656 ?
Cl1 O9 O11 55.1(8) . . ?
O11 O9 O10 93.4(12) . 2_656 ?
Cl1 O10 O9 56.2(7) . 2_656 ?
Cl1 O10 O11 54.5(8) . . ?
Cl1 O10 O12 56.0(8) . 2_656 ?
O9 O10 O12 85.0(11) 2_656 2_656 ?
O11 O10 O9 95.8(12) . 2_656 ?
O11 O10 O12 92.1(11) . 2_656 ?
Cl1 O11 O9 60.0(8) . . ?
Cl1 O11 O10 56.8(9) . . ?
Cl1 O11 O12 61.7(9) . . ?
O9 O11 O10 98.9(13) . . ?
O9 O11 O12 95.7(12) . . ?
O10 O11 O12 94.7(13) . . ?
Cl1 O12 O10 48.9(7) . 2_656 ?
Cl1 O12 O11 51.1(7) . . ?
O11 O12 O10 83.8(10) . 2_656 ?
O13 Cl2 O13 180.0(13) 2_757 . ?
O13 Cl2 O14 101.0(9) 2_757 2_757 ?
O13 Cl2 O14 79.0(9) . 2_757 ?
O13 Cl2 O14 79.0(9) 2_757 . ?
O13 Cl2 O14 101.0(9) . . ?
O13 Cl2 O16 66.9(8) . . ?
O13 Cl2 O16 66.9(8) 2_757 2_757 ?
O13 Cl2 O16 113.1(8) 2_757 . ?
O13 Cl2 O16 113.1(8) . 2_757 ?
O14 Cl2 O14 180.0 2_757 . ?
O15 Cl2 O13 58.5(9) . 2_757 ?
O15 Cl2 O13 121.5(9) 2_757 2_757 ?
O15 Cl2 O13 121.5(9) . . ?
O15 Cl2 O13 58.5(9) 2_757 . ?
O15 Cl2 O14 106.9(7) 2_757 2_757 ?
O15 Cl2 O14 73.1(7) 2_757 . ?
O15 Cl2 O14 73.1(7) . 2_757 ?
O15 Cl2 O14 106.9(7) . . ?
O15 Cl2 O15 180.0(14) 2_757 . ?
O15 Cl2 O16 72.0(9) 2_757 2_757 ?
O15 Cl2 O16 108.0(9) . 2_757 ?
O15 Cl2 O16 108.0(9) 2_757 . ?
O15 Cl2 O16 72.0(9) . . ?
O16 Cl2 O14 104.7(9) 2_757 . ?
O16 Cl2 O14 75.3(9) 2_757 2_757 ?
O16 Cl2 O14 104.7(9) . 2_757 ?
O16 Cl2 O14 75.3(9) . . ?
O16 Cl2 O16 180.0 2_757 . ?
Cl2 O13 O16 56.8(8) . . ?
O15 O13 Cl2 60.1(9) 2_757 . ?
O15 O13 O16 101.7(13) 2_757 . ?
Cl2 O14 O15 47.7(5) . 2_757 ?
Cl2 O15 O14 59.2(7) . 2_757 ?
Cl2 O15 O16 54.7(7) . . ?
O13 O15 Cl2 61.3(9) 2_757 . ?
O13 O15 O14 94.1(12) 2_757 2_757 ?
O13 O15 O16 102.2(12) 2_757 . ?
O16 O15 O14 88.2(10) . 2_757 ?
Cl2 O16 O13 56.2(8) . . ?
Cl2 O16 O15 53.3(7) . . ?
O13 O16 O15 99.1(11) . . ?
O17 Cl3 O18A 102.8(6) . . ?
O17 Cl3 O18B 93.3(16) . . ?
O17 Cl3 O20B 111.2(9) . . ?
O19A Cl3 O17 104.4(7) . . ?
O19A Cl3 O18A 108.6(8) . . ?
O19B Cl3 O17 131.7(18) . . ?
O19B Cl3 O18B 111(3) . . ?
O19B Cl3 O20B 110(2) . . ?
O20A Cl3 O17 109.8(9) . . ?
O20A Cl3 O18A 101.2(11) . . ?
O20A Cl3 O19A 127.6(12) . . ?
O20B Cl3 O18B 90.2(18) . . ?
O22A Cl4 O21A 117.0(8) . . ?
O22A Cl4 O23A 104.3(9) . . ?
O22A Cl4 O24A 118.8(9) . . ?
O22B Cl4 O21B 131.9(16) . . ?
O23A Cl4 O21A 106.6(8) . . ?
O23A Cl4 O24A 122.9(9) . . ?
O23B Cl4 O21B 93(2) . . ?
O23B Cl4 O22B 71.2(18) . . ?
O24A Cl4 O21A 86.2(8) . . ?
O24B Cl4 O21B 79.3(18) . . ?
O24B Cl4 O22B 114.4(19) . . ?
O24B Cl4 O23B 172(2) . . ?
Cl4 O22B O23B 53.9(11) . . ?
Cl4 O23B O22B 54.9(12) . . ?
O26A Cl5 O25A 97.0(7) . . ?
O26A Cl5 O27A 105.8(10) . . ?
O26B Cl5 O25B 115(2) . . ?
O26B Cl5 O27B 119(2) . . ?
O26B Cl5 O28B 133.1(17) . . ?
O27A Cl5 O25A 108.8(9) . . ?
O27B Cl5 O25B 118.1(19) . . ?
O27B Cl5 O28B 107.7(16) . . ?
O28A Cl5 O25A 121.6(9) . . ?
O28A Cl5 O26A 136.6(10) . . ?
O28A Cl5 O27A 81.3(11) . . ?
O28B Cl5 O25B 34.0(13) . . ?
O28B O25B Cl5 71.8(17) . . ?
O25B O28B Cl5 74.2(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
