# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1472618'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;

_chemical_name_common            'Complex [Fe(cis-5)][(BF4)2]'
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C32 H30 Fe N6), 0.217(C4 H6 N2), 4(B F4), 0.566(C2 H3 N)'

_chemical_formula_sum            'C66 H63 B4 F16 Fe2 N13'
_chemical_formula_weight         1497.23

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'
B B 0.0013 0.0007 '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'
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                   36.181(3)
_cell_length_b                   10.2086(6)
_cell_length_c                   19.477(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.983(10)
_cell_angle_gamma                90
_cell_volume                     6842.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    7279
_cell_measurement_theta_min      3.0841
_cell_measurement_theta_max      25.0047

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_F_000             3064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.519
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79441
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23852
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.090
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6002
_reflns_number_gt                4682
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1401P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6002
_refine_ls_number_parameters     523
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.2144
_refine_ls_wR_factor_gt          0.1970
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.069
_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 0.67567(10) 0.7690(3) 0.57120(18) 0.0587(8) Uani 1 1 d . . . . .
H1 H 0.7000 0.7941 0.5625 0.070 Uiso 1 1 calc R U . . .
C6 C 0.64440(10) 0.7557(3) 0.49855(18) 0.0570(8) Uani 1 1 d . . . . .
H6 H 0.6531 0.6892 0.4707 0.068 Uiso 1 1 calc R U . . .
C5 C 0.60630(11) 0.7086(4) 0.5077(2) 0.0708(10) Uani 1 1 d . . . . .
H5A H 0.5868 0.7001 0.4608 0.085 Uiso 1 1 calc R U . . .
H5B H 0.5970 0.7719 0.5357 0.085 Uiso 1 1 calc R U . . .
C4 C 0.61267(16) 0.5763(4) 0.5461(3) 0.0953(15) Uani 1 1 d . . . . .
H4A H 0.6193 0.5115 0.5154 0.114 Uiso 1 1 calc R U . . .
H4B H 0.5887 0.5488 0.5543 0.114 Uiso 1 1 calc R U . . .
C3 C 0.64506(16) 0.5821(4) 0.6185(3) 0.0918(14) Uani 1 1 d . . . . .
H3A H 0.6366 0.6359 0.6519 0.110 Uiso 1 1 calc R U . . .
H3B H 0.6500 0.4946 0.6386 0.110 Uiso 1 1 calc R U . . .
C2 C 0.68201(14) 0.6378(4) 0.6106(2) 0.0810(12) Uani 1 1 d . . . . .
H2A H 0.6929 0.5760 0.5842 0.097 Uiso 1 1 calc R U . . .
H2B H 0.7007 0.6491 0.6581 0.097 Uiso 1 1 calc R U . . .
C7 C 0.69771(11) 0.9186(4) 0.6763(2) 0.0656(9) Uani 1 1 d . . . . .
H7A H 0.6881 0.9429 0.7158 0.079 Uiso 1 1 calc R U . . .
H7B H 0.7158 0.8467 0.6924 0.079 Uiso 1 1 calc R U . . .
C8 C 0.71807(11) 1.0312(3) 0.65700(19) 0.0619(9) Uani 1 1 d . . . . .
C9 C 0.75625(12) 1.0666(5) 0.6967(2) 0.0774(12) Uani 1 1 d . . . . .
H9 H 0.7707 1.0157 0.7353 0.093 Uiso 1 1 calc R U . . .
C10 C 0.77152(12) 1.1757(5) 0.6776(3) 0.0844(13) Uani 1 1 d . . . . .
H10 H 0.7966 1.2006 0.7039 0.101 Uiso 1 1 calc R U . . .
C11 C 0.75055(12) 1.2525(4) 0.6190(3) 0.0773(13) Uani 1 1 d . . . . .
C12 C 0.71275(11) 1.2083(3) 0.5804(2) 0.0626(9) Uani 1 1 d . . . . .
C13 C 0.76372(17) 1.3681(5) 0.5920(4) 0.1053(19) Uani 1 1 d . . . . .
H13 H 0.7884 1.4004 0.6161 0.126 Uiso 1 1 calc R U . . .
C14 C 0.74142(19) 1.4321(4) 0.5326(4) 0.104(2) Uani 1 1 d . . . . .
H14 H 0.7507 1.5085 0.5177 0.125 Uiso 1 1 calc R U . . .
C15 C 0.70417(16) 1.3839(4) 0.4929(3) 0.0850(13) Uani 1 1 d . . . . .
C16 C 0.68941(12) 1.2725(3) 0.5165(2) 0.0674(10) Uani 1 1 d . . . . .
C17 C 0.6807(2) 1.4413(4) 0.4298(4) 0.102(2) Uani 1 1 d . . . . .
H17 H 0.6891 1.5167 0.4124 0.123 Uiso 1 1 calc R U . . .
C18 C 0.6459(2) 1.3890(5) 0.3934(3) 0.1063(19) Uani 1 1 d . . . . .
H18 H 0.6306 1.4275 0.3509 0.128 Uiso 1 1 calc R U . . .
C19 C 0.63274(14) 1.2750(4) 0.4206(2) 0.0782(11) Uani 1 1 d . . . . .
H19 H 0.6088 1.2389 0.3953 0.094 Uiso 1 1 calc R U . . .
C20 C 0.60798(10) 0.8953(4) 0.39278(18) 0.0632(9) Uani 1 1 d . . . . .
H20A H 0.5997 0.8086 0.3738 0.076 Uiso 1 1 calc R U . . .
H20B H 0.6158 0.9433 0.3566 0.076 Uiso 1 1 calc R U . . .
C21 C 0.57476(11) 0.9647(3) 0.40747(19) 0.0573(8) Uani 1 1 d . . . . .
C22 C 0.53667(12) 0.9666(4) 0.3604(2) 0.0742(11) Uani 1 1 d . . . . .
H22 H 0.5304 0.9180 0.3180 0.089 Uiso 1 1 calc R U . . .
C23 C 0.50878(13) 1.0391(4) 0.3763(3) 0.0821(12) Uani 1 1 d . . . . .
H23 H 0.4835 1.0404 0.3449 0.098 Uiso 1 1 calc R U . . .
C24 C 0.51850(11) 1.1122(4) 0.4410(2) 0.0725(10) Uani 1 1 d . . . . .
C25 C 0.55674(9) 1.1035(3) 0.48671(19) 0.0589(8) Uani 1 1 d . . . . .
C26 C 0.49219(12) 1.1904(5) 0.4650(3) 0.0980(15) Uani 1 1 d . . . . .
H26 H 0.4665 1.1974 0.4360 0.118 Uiso 1 1 calc R U . . .
C27 C 0.50364(13) 1.2539(6) 0.5281(3) 0.0998(15) Uani 1 1 d . . . . .
H27 H 0.4856 1.3036 0.5420 0.120 Uiso 1 1 calc R U . . .
C28 C 0.54292(12) 1.2475(5) 0.5750(2) 0.0783(11) Uani 1 1 d . . . . .
C29 C 0.56965(10) 1.1714(3) 0.55388(19) 0.0585(8) Uani 1 1 d . . . . .
C30 C 0.55690(14) 1.3080(5) 0.6429(3) 0.0942(14) Uani 1 1 d . . . . .
H30 H 0.5402 1.3586 0.6600 0.113 Uiso 1 1 calc R U . . .
C31 C 0.59392(15) 1.2934(5) 0.6833(3) 0.0899(13) Uani 1 1 d . . . . .
H31 H 0.6029 1.3327 0.7285 0.108 Uiso 1 1 calc R U . . .
C32 C 0.61934(11) 1.2183(4) 0.6571(2) 0.0694(10) Uani 1 1 d . . . . .
H32 H 0.6452 1.2105 0.6852 0.083 Uiso 1 1 calc R U . . .
N1 N 0.66480(8) 0.8753(3) 0.61403(14) 0.0530(6) Uani 1 1 d . . . . .
N4 N 0.64169(8) 0.8835(3) 0.45953(15) 0.0571(7) Uani 1 1 d . . . . .
N2 N 0.69756(7) 1.1003(3) 0.60038(15) 0.0553(7) Uani 1 1 d . . . . .
N3 N 0.65415(10) 1.2192(3) 0.48157(17) 0.0657(8) Uani 1 1 d . . . . .
N5 N 0.58406(8) 1.0310(2) 0.46935(15) 0.0529(7) Uani 1 1 d . . . . .
N6 N 0.60752(8) 1.1584(3) 0.59355(15) 0.0570(7) Uani 1 1 d . . . . .
C1S C 0.4836(13) 0.522(4) 0.718(2) 0.173(6) Uani 0.217(6) 1 d D U P A 1
C2S C 0.5020(17) 0.636(3) 0.763(2) 0.173(6) Uani 0.217(6) 1 d D U P A 1
H2S1 H 0.4832 0.6790 0.7809 0.259 Uiso 0.217(6) 1 calc R U P A 1
H2S2 H 0.5116 0.6958 0.7349 0.259 Uiso 0.217(6) 1 calc R U P A 1
H2S3 H 0.5232 0.6057 0.8034 0.259 Uiso 0.217(6) 1 calc R U P A 1
N1S N 0.4674(14) 0.446(3) 0.680(2) 0.173(6) Uani 0.217(6) 1 d D U P A 1
C1S' C 0.4667(15) 0.495(3) 0.678(2) 0.173(6) Uani 0.283(6) 1 d D U P A 2
C2S' C 0.4804(10) 0.629(2) 0.669(2) 0.173(6) Uani 0.283(6) 1 d D U P A 2
H2S4 H 0.5036 0.6475 0.7079 0.259 Uiso 0.283(6) 1 calc R U P A 2
H2S5 H 0.4606 0.6910 0.6694 0.259 Uiso 0.283(6) 1 calc R U P A 2
H2S6 H 0.4858 0.6336 0.6239 0.259 Uiso 0.283(6) 1 calc R U P A 2
N1S' N 0.4574(9) 0.3931(19) 0.6844(17) 0.173(6) Uani 0.283(6) 1 d D U P A 2
F5 F 0.90951(9) 1.3682(4) 0.84230(15) 0.1227(11) Uani 1 1 d D . . . .
F6 F 0.91946(16) 1.2038(5) 0.7828(4) 0.214(2) Uani 1 1 d D . . . .
F7 F 0.86526(8) 1.3236(4) 0.73948(19) 0.1328(12) Uani 1 1 d D . . . .
F8 F 0.92264(11) 1.3950(6) 0.7402(2) 0.206(3) Uani 1 1 d D . . . .
Fe1 Fe 0.64151(2) 1.04034(4) 0.53829(2) 0.0515(2) Uani 1 1 d . . . . .
B2 B 0.90341(14) 1.3304(6) 0.7740(3) 0.0844(15) Uani 1 1 d D . . . .
B1 B 0.6993(4) 1.2401(18) 0.8415(9) 0.127(15) Uani 0.435(12) 1 d D . P A 1
F1 F 0.6920(5) 1.1273(14) 0.8730(15) 0.217(11) Uani 0.435(12) 1 d D . P A 1
F2 F 0.6647(3) 1.2997(13) 0.8297(7) 0.101(4) Uani 0.435(12) 1 d D . P A 1
F3 F 0.7097(4) 1.203(2) 0.7855(8) 0.233(12) Uani 0.435(12) 1 d D . P A 1
F4 F 0.7282(2) 1.3030(13) 0.8879(8) 0.132(5) Uani 0.435(12) 1 d D . P A 1
B1' B 0.6985(3) 1.2288(10) 0.8407(4) 0.051(4) Uani 0.565(12) 1 d D . P A 2
F1' F 0.6834(3) 1.1102(7) 0.8242(6) 0.138(4) Uani 0.565(12) 1 d D . P A 2
F2' F 0.6709(4) 1.3210(10) 0.8178(7) 0.173(6) Uani 0.565(12) 1 d D . P A 2
F3' F 0.7202(4) 1.2463(15) 0.7993(7) 0.224(8) Uani 0.565(12) 1 d D . P A 2
F4' F 0.7168(3) 1.2355(12) 0.9099(4) 0.132(4) Uani 0.565(12) 1 d D . P A 2
H1N H 0.6478(9) 0.844(3) 0.6327(17) 0.039(8) Uiso 1 1 d . . . . .
H4N H 0.6649(11) 0.890(3) 0.447(2) 0.067(10) Uiso 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 1.493(4) . ?
C1 C6 1.520(5) . ?
C1 C2 1.525(5) . ?
C1 H1 0.9800 . ?
C6 N4 1.498(4) . ?
C6 C5 1.521(5) . ?
C6 H6 0.9800 . ?
C5 C4 1.527(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C4 C3 1.531(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 C2 1.504(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C7 C8 1.475(6) . ?
C7 N1 1.481(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.326(5) . ?
C8 C9 1.406(5) . ?
C9 C10 1.346(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.399(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.416(5) . ?
C11 C13 1.431(7) . ?
C12 N2 1.342(4) . ?
C12 C16 1.430(6) . ?
C13 C14 1.356(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.419(8) . ?
C14 H14 0.9300 . ?
C15 C17 1.390(8) . ?
C15 C16 1.393(5) . ?
C16 N3 1.360(5) . ?
C17 C18 1.350(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.419(6) . ?
C18 H18 0.9300 . ?
C19 N3 1.330(5) . ?
C19 H19 0.9300 . ?
C20 N4 1.488(4) . ?
C20 C21 1.497(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N5 1.332(4) . ?
C21 C22 1.399(5) . ?
C22 C23 1.362(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.412(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.398(5) . ?
C24 C26 1.427(6) . ?
C25 N5 1.359(4) . ?
C25 C29 1.426(5) . ?
C26 C27 1.338(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.434(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.398(5) . ?
C28 C30 1.405(6) . ?
C29 N6 1.356(4) . ?
C30 C31 1.336(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.408(5) . ?
C31 H31 0.9300 . ?
C32 N6 1.328(4) . ?
C32 H32 0.9300 . ?
N1 Fe1 2.227(3) . ?
N1 H1N 0.86(3) . ?
N4 Fe1 2.219(3) . ?
N4 H4N 0.95(4) . ?
N2 Fe1 2.106(3) . ?
N3 Fe1 2.253(3) . ?
N5 Fe1 2.100(3) . ?
N6 Fe1 2.223(3) . ?
C1S N1S 1.109(9) . ?
C1S C2S 1.482(9) . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
C1S' N1S' 1.115(8) . ?
C1S' C2S' 1.477(8) . ?
C2S' H2S4 0.9600 . ?
C2S' H2S5 0.9600 . ?
C2S' H2S6 0.9600 . ?
F5 B2 1.336(6) . ?
F6 B2 1.405(7) . ?
F7 B2 1.338(5) . ?
F8 B2 1.280(6) . ?
B1 F3 1.314(16) . ?
B1 F4 1.317(15) . ?
B1 F2 1.347(14) . ?
B1 F1 1.369(17) . ?
B1' F3' 1.302(9) . ?
B1' F4' 1.307(9) . ?
B1' F1' 1.327(11) . ?
B1' F2' 1.344(11) . ?

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 C6 109.6(3) . . ?
N1 C1 C2 112.5(3) . . ?
C6 C1 C2 110.0(3) . . ?
N1 C1 H1 108.2 . . ?
C6 C1 H1 108.2 . . ?
C2 C1 H1 108.2 . . ?
N4 C6 C1 107.9(3) . . ?
N4 C6 C5 114.5(3) . . ?
C1 C6 C5 111.1(3) . . ?
N4 C6 H6 107.7 . . ?
C1 C6 H6 107.7 . . ?
C5 C6 H6 107.7 . . ?
C6 C5 C4 109.4(3) . . ?
C6 C5 H5A 109.8 . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5B 109.8 . . ?
C4 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
C5 C4 C3 111.9(4) . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C2 C3 C4 111.8(4) . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C3 C2 C1 112.5(3) . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C8 C7 N1 111.3(3) . . ?
C8 C7 H7A 109.4 . . ?
N1 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
N1 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C9 121.5(4) . . ?
N2 C8 C7 115.5(3) . . ?
C9 C8 C7 122.9(4) . . ?
C10 C9 C8 118.6(4) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C11 121.6(4) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C12 116.4(4) . . ?
C10 C11 C13 127.1(5) . . ?
C12 C11 C13 116.4(5) . . ?
N2 C12 C11 121.6(4) . . ?
N2 C12 C16 116.4(3) . . ?
C11 C12 C16 122.0(4) . . ?
C14 C13 C11 122.1(5) . . ?
C14 C13 H13 118.9 . . ?
C11 C13 H13 118.9 . . ?
C13 C14 C15 120.9(4) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C17 C15 C16 116.3(5) . . ?
C17 C15 C14 123.7(5) . . ?
C16 C15 C14 120.0(5) . . ?
N3 C16 C15 123.9(4) . . ?
N3 C16 C12 117.5(3) . . ?
C15 C16 C12 118.5(4) . . ?
C18 C17 C15 120.9(5) . . ?
C18 C17 H17 119.5 . . ?
C15 C17 H17 119.5 . . ?
C17 C18 C19 119.6(5) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
N3 C19 C18 121.0(5) . . ?
N3 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
N4 C20 C21 111.2(3) . . ?
N4 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
N4 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N5 C21 C22 120.5(3) . . ?
N5 C21 C20 114.8(3) . . ?
C22 C21 C20 124.6(3) . . ?
C23 C22 C21 120.5(4) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 119.5(4) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 117.4(3) . . ?
C25 C24 C26 117.1(4) . . ?
C23 C24 C26 125.4(4) . . ?
N5 C25 C24 122.0(3) . . ?
N5 C25 C29 115.8(3) . . ?
C24 C25 C29 122.2(3) . . ?
C27 C26 C24 121.5(4) . . ?
C27 C26 H26 119.2 . . ?
C24 C26 H26 119.2 . . ?
C26 C27 C28 121.9(4) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C29 C28 C30 116.1(4) . . ?
C29 C28 C27 118.5(4) . . ?
C30 C28 C27 125.3(4) . . ?
N6 C29 C28 123.8(3) . . ?
N6 C29 C25 117.5(3) . . ?
C28 C29 C25 118.7(3) . . ?
C31 C30 C28 120.6(4) . . ?
C31 C30 H30 119.7 . . ?
C28 C30 H30 119.7 . . ?
C30 C31 C32 119.7(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
N6 C32 C31 122.0(4) . . ?
N6 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C7 N1 C1 113.0(3) . . ?
C7 N1 Fe1 111.1(2) . . ?
C1 N1 Fe1 106.90(19) . . ?
C7 N1 H1N 105(2) . . ?
C1 N1 H1N 108.2(19) . . ?
Fe1 N1 H1N 113(2) . . ?
C20 N4 C6 114.9(3) . . ?
C20 N4 Fe1 111.7(2) . . ?
C6 N4 Fe1 106.95(19) . . ?
C20 N4 H4N 109(2) . . ?
C6 N4 H4N 105(2) . . ?
Fe1 N4 H4N 109(2) . . ?
C8 N2 C12 120.2(3) . . ?
C8 N2 Fe1 121.0(2) . . ?
C12 N2 Fe1 118.7(2) . . ?
C19 N3 C16 118.2(4) . . ?
C19 N3 Fe1 129.4(3) . . ?
C16 N3 Fe1 112.3(2) . . ?
C21 N5 C25 120.1(3) . . ?
C21 N5 Fe1 121.7(2) . . ?
C25 N5 Fe1 118.0(2) . . ?
C32 N6 C29 117.6(3) . . ?
C32 N6 Fe1 129.4(2) . . ?
C29 N6 Fe1 113.0(2) . . ?
N1S C1S C2S 173(5) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S' C1S' C2S' 178(4) . . ?
C1S' C2S' H2S4 109.5 . . ?
C1S' C2S' H2S5 109.5 . . ?
H2S4 C2S' H2S5 109.5 . . ?
C1S' C2S' H2S6 109.5 . . ?
H2S4 C2S' H2S6 109.5 . . ?
H2S5 C2S' H2S6 109.5 . . ?
N5 Fe1 N2 165.47(10) . . ?
N5 Fe1 N4 74.85(10) . . ?
N2 Fe1 N4 113.51(10) . . ?
N5 Fe1 N6 75.40(10) . . ?
N2 Fe1 N6 98.22(10) . . ?
N4 Fe1 N6 147.80(11) . . ?
N5 Fe1 N1 119.12(10) . . ?
N2 Fe1 N1 74.88(11) . . ?
N4 Fe1 N1 80.25(10) . . ?
N6 Fe1 N1 104.02(10) . . ?
N5 Fe1 N3 91.95(11) . . ?
N2 Fe1 N3 74.98(12) . . ?
N4 Fe1 N3 101.62(11) . . ?
N6 Fe1 N3 91.40(10) . . ?
N1 Fe1 N3 147.74(12) . . ?
F8 B2 F5 114.5(5) . . ?
F8 B2 F7 114.1(4) . . ?
F5 B2 F7 110.1(4) . . ?
F8 B2 F6 105.4(5) . . ?
F5 B2 F6 102.1(5) . . ?
F7 B2 F6 109.7(5) . . ?
F3 B1 F4 109.8(13) . . ?
F3 B1 F2 118.4(14) . . ?
F4 B1 F2 113.4(13) . . ?
F3 B1 F1 106.0(14) . . ?
F4 B1 F1 109.0(15) . . ?
F2 B1 F1 99.1(12) . . ?
F3' B1' F4' 114.9(10) . . ?
F3' B1' F1' 104.9(9) . . ?
F4' B1' F1' 109.7(8) . . ?
F3' B1' F2' 103.1(10) . . ?
F4' B1' F2' 113.2(8) . . ?
F1' B1' F2' 110.5(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C6 N4 60.6(3) . . . . ?
C2 C1 C6 N4 -175.2(3) . . . . ?
N1 C1 C6 C5 -65.7(4) . . . . ?
C2 C1 C6 C5 58.5(4) . . . . ?
N4 C6 C5 C4 178.4(3) . . . . ?
C1 C6 C5 C4 -59.0(4) . . . . ?
C6 C5 C4 C3 55.8(5) . . . . ?
C5 C4 C3 C2 -52.9(5) . . . . ?
C4 C3 C2 C1 52.3(5) . . . . ?
N1 C1 C2 C3 67.6(4) . . . . ?
C6 C1 C2 C3 -54.9(4) . . . . ?
N1 C7 C8 N2 21.8(4) . . . . ?
N1 C7 C8 C9 -160.0(3) . . . . ?
N2 C8 C9 C10 2.2(5) . . . . ?
C7 C8 C9 C10 -175.9(4) . . . . ?
C8 C9 C10 C11 -1.0(6) . . . . ?
C9 C10 C11 C12 -0.9(5) . . . . ?
C9 C10 C11 C13 -178.2(4) . . . . ?
C10 C11 C12 N2 1.8(5) . . . . ?
C13 C11 C12 N2 179.4(3) . . . . ?
C10 C11 C12 C16 -175.4(3) . . . . ?
C13 C11 C12 C16 2.1(5) . . . . ?
C10 C11 C13 C14 177.0(4) . . . . ?
C12 C11 C13 C14 -0.2(6) . . . . ?
C11 C13 C14 C15 -2.1(7) . . . . ?
C13 C14 C15 C17 -176.9(4) . . . . ?
C13 C14 C15 C16 2.6(6) . . . . ?
C17 C15 C16 N3 -0.1(5) . . . . ?
C14 C15 C16 N3 -179.6(3) . . . . ?
C17 C15 C16 C12 178.8(3) . . . . ?
C14 C15 C16 C12 -0.7(5) . . . . ?
N2 C12 C16 N3 -0.1(4) . . . . ?
C11 C12 C16 N3 177.3(3) . . . . ?
N2 C12 C16 C15 -179.0(3) . . . . ?
C11 C12 C16 C15 -1.7(5) . . . . ?
C16 C15 C17 C18 -1.1(6) . . . . ?
C14 C15 C17 C18 178.4(4) . . . . ?
C15 C17 C18 C19 1.0(7) . . . . ?
C17 C18 C19 N3 0.3(6) . . . . ?
N4 C20 C21 N5 16.5(4) . . . . ?
N4 C20 C21 C22 -165.7(3) . . . . ?
N5 C21 C22 C23 1.8(5) . . . . ?
C20 C21 C22 C23 -175.9(4) . . . . ?
C21 C22 C23 C24 -0.3(6) . . . . ?
C22 C23 C24 C25 -1.4(6) . . . . ?
C22 C23 C24 C26 -178.9(4) . . . . ?
C23 C24 C25 N5 1.9(5) . . . . ?
C26 C24 C25 N5 179.6(4) . . . . ?
C23 C24 C25 C29 -179.0(4) . . . . ?
C26 C24 C25 C29 -1.3(6) . . . . ?
C25 C24 C26 C27 0.7(7) . . . . ?
C23 C24 C26 C27 178.2(5) . . . . ?
C24 C26 C27 C28 0.3(9) . . . . ?
C26 C27 C28 C29 -0.7(8) . . . . ?
C26 C27 C28 C30 -178.0(5) . . . . ?
C30 C28 C29 N6 -2.7(6) . . . . ?
C27 C28 C29 N6 179.8(4) . . . . ?
C30 C28 C29 C25 177.6(4) . . . . ?
C27 C28 C29 C25 0.0(6) . . . . ?
N5 C25 C29 N6 0.4(4) . . . . ?
C24 C25 C29 N6 -178.8(3) . . . . ?
N5 C25 C29 C28 -179.8(3) . . . . ?
C24 C25 C29 C28 1.0(5) . . . . ?
C29 C28 C30 C31 1.0(7) . . . . ?
C27 C28 C30 C31 178.4(5) . . . . ?
C28 C30 C31 C32 0.9(8) . . . . ?
C30 C31 C32 N6 -1.4(7) . . . . ?
C8 C7 N1 C1 92.9(3) . . . . ?
C8 C7 N1 Fe1 -27.2(3) . . . . ?
C6 C1 N1 C7 -164.8(3) . . . . ?
C2 C1 N1 C7 72.4(4) . . . . ?
C6 C1 N1 Fe1 -42.2(3) . . . . ?
C2 C1 N1 Fe1 -165.0(3) . . . . ?
C21 C20 N4 C6 96.4(3) . . . . ?
C21 C20 N4 Fe1 -25.7(3) . . . . ?
C1 C6 N4 C20 -170.1(3) . . . . ?
C5 C6 N4 C20 -45.8(4) . . . . ?
C1 C6 N4 Fe1 -45.5(3) . . . . ?
C5 C6 N4 Fe1 78.8(3) . . . . ?
C9 C8 N2 C12 -1.4(5) . . . . ?
C7 C8 N2 C12 176.9(3) . . . . ?
C9 C8 N2 Fe1 176.7(2) . . . . ?
C7 C8 N2 Fe1 -5.0(4) . . . . ?
C11 C12 N2 C8 -0.7(5) . . . . ?
C16 C12 N2 C8 176.7(3) . . . . ?
C11 C12 N2 Fe1 -178.8(2) . . . . ?
C16 C12 N2 Fe1 -1.5(4) . . . . ?
C18 C19 N3 C16 -1.5(5) . . . . ?
C18 C19 N3 Fe1 179.8(3) . . . . ?
C15 C16 N3 C19 1.3(5) . . . . ?
C12 C16 N3 C19 -177.5(3) . . . . ?
C15 C16 N3 Fe1 -179.7(3) . . . . ?
C12 C16 N3 Fe1 1.4(4) . . . . ?
C22 C21 N5 C25 -1.4(5) . . . . ?
C20 C21 N5 C25 176.5(3) . . . . ?
C22 C21 N5 Fe1 -176.1(3) . . . . ?
C20 C21 N5 Fe1 1.8(4) . . . . ?
C24 C25 N5 C21 -0.5(5) . . . . ?
C29 C25 N5 C21 -179.6(3) . . . . ?
C24 C25 N5 Fe1 174.5(3) . . . . ?
C29 C25 N5 Fe1 -4.7(4) . . . . ?
C31 C32 N6 C29 -0.1(5) . . . . ?
C31 C32 N6 Fe1 177.9(3) . . . . ?
C28 C29 N6 C32 2.2(5) . . . . ?
C25 C29 N6 C32 -178.0(3) . . . . ?
C28 C29 N6 Fe1 -176.1(3) . . . . ?
C25 C29 N6 Fe1 3.7(4) . . . . ?

_refine_diff_density_max         0.510
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.071

_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
_database_code_depnum_ccdc_archive 'CCDC 1472619'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C34 H34 Fe N6), 4(B F4), C2 H3 N'
_chemical_formula_sum            'C70 H71 B4 F16 Fe2 N13'
_chemical_formula_weight         1553.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   14.2146(12)
_cell_length_b                   26.2737(19)
_cell_length_c                   22.698(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.469(10)
_cell_angle_gamma                90
_cell_volume                     8307.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    2599
_cell_measurement_theta_min      3.8120
_cell_measurement_theta_max      61.7580

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             3192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    3.501
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.38175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24177
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_standards_number         2
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  50
_diffrn_standards_decay_%        4
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.172
_diffrn_reflns_theta_max         61.996
_diffrn_reflns_theta_full        62.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             12715
_reflns_number_gt                6452
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.016 0.025 0.500 1019 272 ' '
2 0.009 0.480 0.000 1019 272 ' '
_platon_squeeze_details          ?



_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1152P)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         12715
_refine_ls_number_parameters     1039
_refine_ls_number_restraints     1131
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.0851
_refine_ls_wR_factor_ref         0.2481
_refine_ls_wR_factor_gt          0.2101
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.921
_refine_ls_shift/su_max          0.002
_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
C10 C 0.9743(5) 0.5587(2) 0.3270(3) 0.0627(18) Uani 1 1 d . U . . .
H1 H 0.9700 0.5940 0.3280 0.075 Uiso 1 1 calc R U . . .
C11 C 0.8925(4) 0.5288(2) 0.3273(3) 0.0521(15) Uani 1 1 d . U . . .
C21 C 0.9598(5) 0.2813(3) 0.2734(4) 0.0636(16) Uani 1 1 d . U . . .
C20 C 0.9184(5) 0.3124(2) 0.2193(4) 0.0690(18) Uani 1 1 d . U . . .
H4A H 0.8491 0.3137 0.2146 0.083 Uiso 1 1 calc R U . . .
H4B H 0.9336 0.2968 0.1837 0.083 Uiso 1 1 calc R U . . .
C29 C 1.0398(4) 0.3243(3) 0.4227(4) 0.0616(15) Uani 1 1 d . U . . .
C69 C 0.1890(6) 0.7409(4) 0.5124(4) 0.099(3) Uani 1 1 d . U . . .
C32 C 1.0549(5) 0.4092(3) 0.4493(3) 0.0682(18) Uani 1 1 d . U . . .
H6 H 1.0522 0.4435 0.4392 0.082 Uiso 1 1 calc R U . . .
N13 N 0.2126(6) 0.7202(3) 0.5569(4) 0.122(3) Uani 1 1 d . U . . .
C16 C 0.8323(4) 0.4410(2) 0.3260(3) 0.0513(14) Uani 1 1 d . U . . .
C7 C 1.1558(4) 0.4504(2) 0.3271(3) 0.0608(17) Uani 1 1 d . U . . .
H8A H 1.2006 0.4665 0.3058 0.073 Uiso 1 1 calc R U . . .
H8B H 1.1868 0.4473 0.3691 0.073 Uiso 1 1 calc R U . . .
C56 C 0.3800(6) 0.5130(3) 0.1604(3) 0.0723(19) Uani 1 1 d . U . . .
H9 H 0.3197 0.4978 0.1542 0.087 Uiso 1 1 calc R U . . .
C57 C 0.4613(6) 0.4838(3) 0.1609(4) 0.078(2) Uani 1 1 d . U . . .
H10 H 0.4552 0.4487 0.1556 0.094 Uiso 1 1 calc R U . . .
C60 C 0.6438(6) 0.4821(3) 0.1655(3) 0.078(2) Uani 1 1 d . U . . .
H11 H 0.6464 0.4471 0.1597 0.093 Uiso 1 1 calc R U . . .
C62 C 0.7247(5) 0.5638(3) 0.1784(3) 0.0643(17) Uani 1 1 d . U . . .
C59 C 0.5540(5) 0.5587(2) 0.1778(3) 0.0573(15) Uani 1 1 d . U . . .
C6 C 1.0514(5) 0.3643(3) 0.2027(4) 0.0665(17) Uani 1 1 d . U . . .
H020 H 1.0812 0.3311 0.2141 0.080 Uiso 1 1 calc R U . . .
C61 C 0.7231(6) 0.5095(3) 0.1702(3) 0.079(2) Uani 1 1 d . U . . .
H021 H 0.7802 0.4930 0.1681 0.094 Uiso 1 1 calc R U . . .
C12 C 0.9046(4) 0.4759(2) 0.3228(3) 0.0490(14) Uani 1 1 d . U . . .
C36 C 0.4238(5) 0.6621(2) 0.3708(3) 0.0576(16) Uani 1 1 d . U . . .
H02A H 0.4712 0.6840 0.3952 0.069 Uiso 1 1 calc R U . . .
H02B H 0.4416 0.6271 0.3809 0.069 Uiso 1 1 calc R U . . .
C52 C 0.4166(5) 0.6733(3) 0.0009(3) 0.0627(17) Uani 1 1 d . U . . .
H030 H 0.3962 0.6532 -0.0330 0.075 Uiso 1 1 calc R U . . .
C58 C 0.5522(6) 0.5060(3) 0.1691(3) 0.0704(18) Uani 1 1 d . U . . .
C18 C 0.6949(5) 0.3711(3) 0.3340(3) 0.0649(19) Uani 1 1 d . U . . .
H035 H 0.6492 0.3461 0.3361 0.078 Uiso 1 1 calc R U . . .
C55 C 0.3892(5) 0.5652(2) 0.1694(3) 0.0576(16) Uani 1 1 d . U . . .
C25 C 1.0162(5) 0.2890(3) 0.3761(4) 0.0683(17) Uani 1 1 d . U . . .
C15 C 0.7398(4) 0.4586(2) 0.3319(3) 0.0556(16) Uani 1 1 d . U . . .
C8 C 1.0670(4) 0.4827(2) 0.3217(3) 0.0525(15) Uani 1 1 d . U . . .
C19 C 0.7878(5) 0.3567(2) 0.3285(3) 0.0593(17) Uani 1 1 d . U . . .
H40 H 0.8024 0.3222 0.3280 0.071 Uiso 1 1 calc R U . . .
C28 C 1.0639(5) 0.3078(3) 0.4834(4) 0.0697(18) Uani 1 1 d . U . . .
C17 C 0.6704(5) 0.4216(3) 0.3362(3) 0.0634(18) Uani 1 1 d . U . . .
H42 H 0.6091 0.4311 0.3404 0.076 Uiso 1 1 calc R U . . .
C67 C 0.5692(5) 0.6164(2) 0.3180(3) 0.0639(18) Uani 1 1 d . U . . .
H04A H 0.6289 0.6113 0.3052 0.096 Uiso 1 1 calc R U . . .
H04B H 0.5291 0.5870 0.3078 0.096 Uiso 1 1 calc R U . . .
H04C H 0.5814 0.6214 0.3608 0.096 Uiso 1 1 calc R U . . .
C53 C 0.4360(4) 0.6516(3) 0.0581(3) 0.0564(15) Uani 1 1 d . U . . .
H43 H 0.4296 0.6165 0.0611 0.068 Uiso 1 1 calc R U . . .
C35 C 0.4235(5) 0.6714(2) 0.3045(3) 0.0567(15) Uani 1 1 d . U . . .
H046 H 0.4078 0.7073 0.2963 0.068 Uiso 1 1 calc R U . . .
C64 C 0.8065(6) 0.5955(3) 0.1827(4) 0.080(2) Uani 1 1 d . U . . .
H047 H 0.8661 0.5815 0.1811 0.095 Uiso 1 1 calc R U . . .
C37 C 0.3250(5) 0.6729(3) 0.3848(3) 0.0623(17) Uani 1 1 d . U . . .
H04D H 0.3261 0.6661 0.4269 0.075 Uiso 1 1 calc R U . . .
H04E H 0.3088 0.7085 0.3771 0.075 Uiso 1 1 calc R U . . .
C54 C 0.3112(5) 0.6047(2) 0.1652(3) 0.0640(17) Uani 1 1 d . U . . .
H05A H 0.2874 0.6137 0.1235 0.077 Uiso 1 1 calc R U . . .
H05B H 0.2581 0.5911 0.1813 0.077 Uiso 1 1 calc R U . . .
C9 C 1.0612(5) 0.5358(2) 0.3252(3) 0.0589(16) Uani 1 1 d . U . . .
H052 H 1.1157 0.5557 0.3262 0.071 Uiso 1 1 calc R U . . .
C33 C 1.2021(4) 0.3603(2) 0.3287(3) 0.0666(19) Uani 1 1 d . U . . .
H05C H 1.1835 0.3274 0.3118 0.100 Uiso 1 1 calc R U . . .
H05D H 1.2059 0.3592 0.3714 0.100 Uiso 1 1 calc R U . . .
H05E H 1.2636 0.3693 0.3204 0.100 Uiso 1 1 calc R U . . .
C48 C 0.4760(4) 0.8094(2) 0.0478(3) 0.0582(16) Uani 1 1 d . U . . .
H055 H 0.4641 0.8276 0.0119 0.070 Uiso 1 1 calc R U . . .
C51 C 0.4283(4) 0.7258(3) -0.0048(3) 0.0586(16) Uani 1 1 d . U . . .
H057 H 0.4160 0.7409 -0.0426 0.070 Uiso 1 1 calc R U . . .
C31 C 1.0805(6) 0.3963(3) 0.5109(4) 0.082(2) Uani 1 1 d . U . . .
H70 H 1.0946 0.4214 0.5402 0.098 Uiso 1 1 calc R U . . .
C30 C 1.0840(6) 0.3440(3) 0.5267(4) 0.079(2) Uani 1 1 d . U . . .
H71 H 1.1002 0.3344 0.5669 0.095 Uiso 1 1 calc R U . . .
C27 C 1.0629(5) 0.2538(3) 0.4925(4) 0.082(2) Uani 1 1 d . U . . .
H72 H 1.0796 0.2414 0.5315 0.098 Uiso 1 1 calc R U . . .
C26 C 1.0390(5) 0.2202(3) 0.4472(5) 0.086(2) Uani 1 1 d . U . . .
H73 H 1.0389 0.1856 0.4558 0.104 Uiso 1 1 calc R U . . .
C22 C 0.9564(5) 0.2282(3) 0.2787(4) 0.0753(19) Uani 1 1 d . U . . .
H74 H 0.9355 0.2079 0.2450 0.090 Uiso 1 1 calc R U . . .
C66 C 0.7079(5) 0.6677(3) 0.1939(3) 0.0650(18) Uani 1 1 d . U . . .
H75 H 0.7042 0.7025 0.2004 0.078 Uiso 1 1 calc R U . . .
C65 C 0.7968(5) 0.6466(3) 0.1892(4) 0.080(2) Uani 1 1 d . U . . .
H76 H 0.8496 0.6678 0.1905 0.096 Uiso 1 1 calc R U . . .
C46 C 0.5055(4) 0.7566(2) 0.1555(3) 0.0451(13) Uani 1 1 d . U . . .
C45 C 0.5248(4) 0.8096(2) 0.1555(3) 0.0458(13) Uani 1 1 d . U . . .
C47 C 0.5085(4) 0.8343(2) 0.0986(3) 0.0528(14) Uani 1 1 d . U . . .
H79 H 0.5211 0.8689 0.0970 0.063 Uiso 1 1 calc R U . . .
C63 C 0.6407(5) 0.5877(2) 0.1831(3) 0.0526(14) Uani 1 1 d . U . . .
C50 C 0.4746(4) 0.7299(2) 0.1016(3) 0.0483(13) Uani 1 1 d . U . . .
C42 C 0.5572(4) 0.7472(2) 0.2577(3) 0.0516(14) Uani 1 1 d . U . . .
C41 C 0.5806(4) 0.7080(2) 0.3058(3) 0.0539(15) Uani 1 1 d . U . . .
H10A H 0.5680 0.7214 0.3433 0.065 Uiso 1 1 calc R U . . .
H10B H 0.6480 0.6991 0.3117 0.065 Uiso 1 1 calc R U . . .
C44 C 0.5610(4) 0.8304(2) 0.2131(3) 0.0525(14) Uani 1 1 d . U . . .
H103 H 0.5734 0.8652 0.2167 0.063 Uiso 1 1 calc R U . . .
C24 C 1.0140(5) 0.2366(2) 0.3863(4) 0.0698(18) Uani 1 1 d . U . . .
C23 C 0.9852(5) 0.2063(3) 0.3356(4) 0.078(2) Uani 1 1 d . U . . .
H105 H 0.9850 0.1710 0.3397 0.093 Uiso 1 1 calc R U . . .
C49 C 0.4581(4) 0.7549(2) 0.0460(3) 0.0530(14) Uani 1 1 d . U . . .
C43 C 0.5781(4) 0.8010(2) 0.2630(3) 0.0519(14) Uani 1 1 d . U . . .
H121 H 0.6030 0.8153 0.3003 0.062 Uiso 1 1 calc R U . . .
C1 C 1.1184(5) 0.4040(3) 0.2344(3) 0.0620(16) Uani 1 1 d . U . . .
H122 H 1.0892 0.4373 0.2230 0.074 Uiso 1 1 calc R U . . .
C2 C 1.2157(5) 0.4021(2) 0.2121(3) 0.0619(17) Uani 1 1 d . U . . .
H12A H 1.2566 0.4297 0.2305 0.074 Uiso 1 1 calc R U . . .
H12B H 1.2481 0.3703 0.2247 0.074 Uiso 1 1 calc R U . . .
C5 C 1.0382(5) 0.3686(3) 0.1349(4) 0.075(2) Uani 1 1 d . U . . .
H12C H 1.0071 0.4007 0.1217 0.090 Uiso 1 1 calc R U . . .
H12D H 0.9972 0.3413 0.1160 0.090 Uiso 1 1 calc R U . . .
C40 C 0.3479(5) 0.6407(3) 0.2645(3) 0.0570(15) Uani 1 1 d . U . . .
H140 H 0.3641 0.6047 0.2723 0.068 Uiso 1 1 calc R U . . .
C39 C 0.2484(5) 0.6494(2) 0.2805(3) 0.0585(16) Uani 1 1 d . U . . .
H14E H 0.2282 0.6842 0.2708 0.070 Uiso 1 1 calc R U . . .
H14F H 0.2019 0.6269 0.2566 0.070 Uiso 1 1 calc R U . . .
C38 C 0.2506(5) 0.6398(3) 0.3463(3) 0.0638(17) Uani 1 1 d . U . . .
H14G H 0.2654 0.6043 0.3554 0.077 Uiso 1 1 calc R U . . .
H14H H 0.1880 0.6469 0.3552 0.077 Uiso 1 1 calc R U . . .
C4 C 1.1348(5) 0.3659(3) 0.1156(4) 0.079(2) Uani 1 1 d . U . . .
H14C H 1.1639 0.3329 0.1263 0.095 Uiso 1 1 calc R U . . .
H14D H 1.1252 0.3694 0.0722 0.095 Uiso 1 1 calc R U . . .
C3 C 1.2002(5) 0.4066(3) 0.1448(3) 0.0701(19) Uani 1 1 d . U . . .
H14A H 1.1727 0.4396 0.1324 0.084 Uiso 1 1 calc R U . . .
H14B H 1.2613 0.4040 0.1323 0.084 Uiso 1 1 calc R U . . .
C68 C 0.2926(5) 0.6953(3) 0.1746(3) 0.0642(18) Uani 1 1 d . U . . .
H16A H 0.2974 0.6998 0.1334 0.096 Uiso 1 1 calc R U . . .
H16B H 0.3163 0.7251 0.1972 0.096 Uiso 1 1 calc R U . . .
H16C H 0.2266 0.6899 0.1770 0.096 Uiso 1 1 calc R U . . .
C13 C 0.7990(5) 0.5460(3) 0.3330(3) 0.0619(17) Uani 1 1 d . U . . .
H190 H 0.7873 0.5807 0.3358 0.074 Uiso 1 1 calc R U . . .
C14 C 0.7279(5) 0.5123(2) 0.3344(3) 0.0607(17) Uani 1 1 d . U . . .
H191 H 0.6678 0.5248 0.3371 0.073 Uiso 1 1 calc R U . . .
C34 C 0.8870(4) 0.4010(3) 0.1907(3) 0.0653(18) Uani 1 1 d . U . . .
H20A H 0.8313 0.4026 0.2086 0.098 Uiso 1 1 calc R U . . .
H20B H 0.8689 0.3889 0.1501 0.098 Uiso 1 1 calc R U . . .
H20C H 0.9147 0.4343 0.1906 0.098 Uiso 1 1 calc R U . . .
B1 B 0.8625(7) 0.7241(3) 0.3261(4) 0.080(2) Uani 1 1 d D U . . .
B2 B 0.3681(6) 0.8163(3) 0.3301(4) 0.070(2) Uani 1 1 d D U . . .
N1 N 1.1294(4) 0.3989(2) 0.3014(3) 0.0583(13) Uani 1 1 d . U . . .
N6 N 1.0347(3) 0.37583(19) 0.4052(3) 0.0585(13) Uani 1 1 d . U . . .
N5 N 0.9922(3) 0.3105(2) 0.3206(3) 0.0596(13) Uani 1 1 d . U . . .
N2 N 0.9892(3) 0.45346(19) 0.3186(2) 0.0522(12) Uani 1 1 d . U . . .
N3 N 0.8554(3) 0.39020(18) 0.3242(2) 0.0534(13) Uani 1 1 d . U . . .
N4 N 0.9584(3) 0.36575(18) 0.2259(3) 0.0571(13) Uani 1 1 d . U . . .
N11 N 0.4762(4) 0.58744(19) 0.1804(2) 0.0550(12) Uani 1 1 d . U . . .
N7 N 0.5202(3) 0.66185(18) 0.2876(2) 0.0464(11) Uani 1 1 d . U . . .
N10 N 0.3499(4) 0.65070(18) 0.1997(2) 0.0513(12) Uani 1 1 d . U . . .
N8 N 0.5187(3) 0.72766(18) 0.2048(2) 0.0474(11) Uani 1 1 d . U . . .
C70 C 0.1585(7) 0.7690(5) 0.4568(5) 0.145(5) Uani 1 1 d . U . . .
H70A H 0.1474 0.8039 0.4658 0.217 Uiso 1 1 calc R U . . .
H70B H 0.1003 0.7544 0.4344 0.217 Uiso 1 1 calc R U . . .
H70C H 0.2077 0.7672 0.4333 0.217 Uiso 1 1 calc R U . . .
N12 N 0.6288(4) 0.6398(2) 0.1895(2) 0.0565(13) Uani 1 1 d . U . . .
F1 F 0.8510(5) 0.67342(17) 0.3230(2) 0.124(2) Uani 1 1 d D U . . .
F2 F 0.7966(4) 0.7393(2) 0.3626(3) 0.1179(17) Uani 1 1 d D U . . .
F3 F 0.8379(3) 0.74744(15) 0.27162(19) 0.0812(12) Uani 1 1 d D U . . .
F4 F 0.9500(3) 0.74016(18) 0.3564(2) 0.1030(16) Uani 1 1 d D U . . .
F5 F 0.4452(3) 0.78822(14) 0.36035(17) 0.0660(10) Uani 1 1 d D U . . .
F6 F 0.3995(5) 0.86350(17) 0.3174(3) 0.1233(19) Uani 1 1 d D U . . .
F7 F 0.3006(3) 0.8206(2) 0.3648(2) 0.1181(19) Uani 1 1 d D U . . .
F8 F 0.3296(3) 0.79178(16) 0.27641(17) 0.0803(12) Uani 1 1 d D U . . .
B3 B 0.0650(13) 0.5399(7) 0.1621(9) 0.087(5) Uani 0.472(8) 1 d D U P A 1
F9 F 0.0818(12) 0.5280(8) 0.1058(7) 0.141(6) Uani 0.472(8) 1 d D U P A 1
F10 F 0.1450(6) 0.5255(3) 0.2031(5) 0.085(3) Uani 0.472(8) 1 d D U P A 1
F11 F 0.0493(14) 0.5902(5) 0.1688(8) 0.113(6) Uani 0.472(8) 1 d D U P A 1
F12 F -0.0149(17) 0.5124(10) 0.1698(13) 0.089(6) Uani 0.472(8) 1 d D U P A 1
B3' B 0.0435(10) 0.5521(6) 0.1440(7) 0.064(3) Uani 0.528(8) 1 d D U P A 2
F9' F -0.0028(7) 0.5808(3) 0.0957(4) 0.096(3) Uani 0.528(8) 1 d D U P A 2
F10' F 0.1233(7) 0.5317(4) 0.1292(6) 0.091(4) Uani 0.528(8) 1 d D U P A 2
F11' F 0.0591(14) 0.5835(4) 0.1938(5) 0.086(4) Uani 0.528(8) 1 d D U P A 2
F12' F -0.0159(16) 0.5124(9) 0.1547(11) 0.079(5) Uani 0.528(8) 1 d D U P A 2
N9 N 0.4631(3) 0.67792(19) 0.1084(2) 0.0481(11) Uani 1 1 d . U . . .
B4 B 0.5910(11) 0.9956(6) 0.1589(8) 0.082(5) Uani 0.504(10) 1 d D U P B 1
F13 F 0.6040(14) 0.9462(5) 0.1444(10) 0.077(5) Uani 0.504(10) 1 d D U P B 1
F14 F 0.5011(8) 1.0089(5) 0.1648(9) 0.146(6) Uani 0.504(10) 1 d D U P B 1
F15 F 0.6586(6) 1.0159(3) 0.2036(5) 0.084(3) Uani 0.504(10) 1 d D U P B 1
F16 F 0.5960(12) 1.0233(5) 0.1085(6) 0.147(5) Uani 0.504(10) 1 d D U P B 1
B4' B 0.5719(11) 0.9909(7) 0.1510(7) 0.070(4) Uani 0.496(10) 1 d D U P B 2
F13' F 0.6007(19) 0.9417(6) 0.1603(12) 0.100(6) Uani 0.496(10) 1 d D U P B 2
F14' F 0.5296(10) 0.9983(6) 0.2016(5) 0.110(4) Uani 0.496(10) 1 d D U P B 2
F15' F 0.6437(7) 1.0234(5) 0.1429(8) 0.124(5) Uani 0.496(10) 1 d D U P B 2
F16' F 0.4956(7) 0.9980(5) 0.1040(5) 0.120(5) Uani 0.496(10) 1 d D U P B 2
Fe2 Fe 0.49360(7) 0.65750(4) 0.19418(5) 0.0484(3) Uani 1 1 d . U . . .
Fe1 Fe 0.99281(7) 0.38229(4) 0.31668(5) 0.0546(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C10 C9 1.380(9) . ?
C10 C11 1.405(9) . ?
C11 C12 1.407(8) . ?
C11 C13 1.433(8) . ?
C21 N5 1.324(9) . ?
C21 C22 1.401(9) . ?
C21 C20 1.495(10) . ?
C20 N4 1.507(7) . ?
C29 C25 1.396(10) . ?
C29 N6 1.407(8) . ?
C29 C28 1.421(10) . ?
C69 N13 1.136(11) . ?
C69 C70 1.453(12) . ?
C32 N6 1.317(9) . ?
C32 C31 1.414(10) . ?
C16 N3 1.378(7) . ?
C16 C12 1.390(8) . ?
C16 C15 1.425(8) . ?
C7 N1 1.493(8) . ?
C7 C8 1.505(8) . ?
C56 C57 1.387(10) . ?
C56 C55 1.389(9) . ?
C57 C58 1.397(11) . ?
C60 C61 1.325(11) . ?
C60 C58 1.463(10) . ?
C62 C63 1.371(9) . ?
C62 C64 1.419(10) . ?
C62 C61 1.437(10) . ?
C59 N11 1.350(8) . ?
C59 C58 1.398(9) . ?
C59 C63 1.434(9) . ?
C6 C1 1.497(9) . ?
C6 N4 1.517(8) . ?
C6 C5 1.518(10) . ?
C12 N2 1.359(7) . ?
C36 C35 1.524(9) . ?
C36 C37 1.527(9) . ?
C52 C53 1.395(9) . ?
C52 C51 1.397(9) . ?
C18 C17 1.377(8) . ?
C18 C19 1.403(9) . ?
C55 N11 1.344(8) . ?
C55 C54 1.509(9) . ?
C25 N5 1.360(9) . ?
C25 C24 1.397(9) . ?
C15 C17 1.401(9) . ?
C15 C14 1.422(8) . ?
C8 N2 1.337(7) . ?
C8 C9 1.401(8) . ?
C19 N3 1.323(7) . ?
C28 C30 1.356(11) . ?
C28 C27 1.434(9) . ?
C67 N7 1.483(7) . ?
C53 N9 1.325(8) . ?
C35 C40 1.498(9) . ?
C35 N7 1.518(7) . ?
C64 C65 1.361(9) . ?
C37 C38 1.508(9) . ?
C54 N10 1.484(8) . ?
C33 N1 1.492(8) . ?
C48 C47 1.325(9) . ?
C48 C49 1.455(8) . ?
C51 C49 1.379(9) . ?
C31 C30 1.419(10) . ?
C27 C26 1.347(11) . ?
C26 C24 1.423(12) . ?
C22 C23 1.400(11) . ?
C66 N12 1.329(8) . ?
C66 C65 1.403(9) . ?
C46 N8 1.336(7) . ?
C46 C50 1.401(8) . ?
C46 C45 1.420(8) . ?
C45 C44 1.416(9) . ?
C45 C47 1.423(8) . ?
C63 N12 1.389(8) . ?
C50 N9 1.388(7) . ?
C50 C49 1.401(8) . ?
C42 N8 1.319(8) . ?
C42 C43 1.444(8) . ?
C42 C41 1.489(8) . ?
C41 N7 1.496(7) . ?
C44 C43 1.353(8) . ?
C24 C23 1.392(11) . ?
C1 N1 1.505(9) . ?
C1 C2 1.564(8) . ?
C2 C3 1.504(10) . ?
C5 C4 1.524(9) . ?
C40 N10 1.501(8) . ?
C40 C39 1.545(8) . ?
C39 C38 1.507(9) . ?
C4 C3 1.485(9) . ?
C68 N10 1.474(8) . ?
C13 C14 1.349(9) . ?
C34 N4 1.484(8) . ?
B1 F1 1.341(9) . ?
B1 F3 1.363(9) . ?
B1 F4 1.363(9) . ?
B1 F2 1.427(10) . ?
B2 F7 1.361(9) . ?
B2 F6 1.368(9) . ?
B2 F5 1.385(8) . ?
B2 F8 1.391(8) . ?
N1 Fe1 2.084(5) . ?
N6 Fe1 1.987(6) . ?
N5 Fe1 1.890(5) . ?
N2 Fe1 1.871(5) . ?
N3 Fe1 2.005(5) . ?
N4 Fe1 2.067(6) . ?
N11 Fe2 1.875(5) . ?
N7 Fe2 2.082(5) . ?
N10 Fe2 2.079(5) . ?
N8 Fe2 1.884(5) . ?
N12 Fe2 2.000(5) . ?
B3 F11 1.354(16) . ?
B3 F10 1.372(16) . ?
B3 F9 1.381(17) . ?
B3 F12 1.385(16) . ?
B3' F10' 1.357(14) . ?
B3' F11' 1.380(15) . ?
B3' F9' 1.385(15) . ?
B3' F12' 1.392(15) . ?
N9 Fe2 1.982(5) . ?
B4 F14 1.358(16) . ?
B4 F13 1.359(15) . ?
B4 F15 1.361(16) . ?
B4 F16 1.369(17) . ?
B4' F13' 1.362(16) . ?
B4' F15' 1.371(15) . ?
B4' F16' 1.374(16) . ?
B4' F14' 1.411(16) . ?

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
C9 C10 C11 120.3(6) . . ?
C10 C11 C12 115.9(6) . . ?
C10 C11 C13 127.5(6) . . ?
C12 C11 C13 116.6(6) . . ?
N5 C21 C22 121.3(8) . . ?
N5 C21 C20 111.3(6) . . ?
C22 C21 C20 126.9(7) . . ?
C21 C20 N4 110.4(6) . . ?
C25 C29 N6 115.8(7) . . ?
C25 C29 C28 120.4(7) . . ?
N6 C29 C28 123.7(7) . . ?
N13 C69 C70 177.9(13) . . ?
N6 C32 C31 124.4(7) . . ?
N3 C16 C12 116.9(5) . . ?
N3 C16 C15 123.2(6) . . ?
C12 C16 C15 119.9(6) . . ?
N1 C7 C8 109.7(5) . . ?
C57 C56 C55 119.5(7) . . ?
C56 C57 C58 121.1(7) . . ?
C61 C60 C58 120.9(7) . . ?
C63 C62 C64 116.1(7) . . ?
C63 C62 C61 118.3(7) . . ?
C64 C62 C61 125.6(7) . . ?
N11 C59 C58 124.6(7) . . ?
N11 C59 C63 113.4(6) . . ?
C58 C59 C63 121.9(6) . . ?
C1 C6 N4 109.4(5) . . ?
C1 C6 C5 111.8(6) . . ?
N4 C6 C5 114.2(6) . . ?
C60 C61 C62 122.8(7) . . ?
N2 C12 C16 113.1(5) . . ?
N2 C12 C11 123.8(5) . . ?
C16 C12 C11 122.9(5) . . ?
C35 C36 C37 110.7(6) . . ?
C53 C52 C51 118.9(7) . . ?
C57 C58 C59 115.1(7) . . ?
C57 C58 C60 128.5(7) . . ?
C59 C58 C60 116.3(7) . . ?
C17 C18 C19 120.8(6) . . ?
N11 C55 C56 120.8(7) . . ?
N11 C55 C54 110.6(5) . . ?
C56 C55 C54 128.5(7) . . ?
N5 C25 C29 113.8(6) . . ?
N5 C25 C24 123.5(8) . . ?
C29 C25 C24 122.7(8) . . ?
C17 C15 C14 126.5(6) . . ?
C17 C15 C16 117.2(6) . . ?
C14 C15 C16 116.3(6) . . ?
N2 C8 C9 121.2(6) . . ?
N2 C8 C7 110.6(5) . . ?
C9 C8 C7 127.9(6) . . ?
N3 C19 C18 122.5(6) . . ?
C30 C28 C29 117.7(7) . . ?
C30 C28 C27 126.5(8) . . ?
C29 C28 C27 115.7(8) . . ?
C18 C17 C15 118.7(6) . . ?
N9 C53 C52 124.0(7) . . ?
C40 C35 N7 109.6(5) . . ?
C40 C35 C36 111.9(5) . . ?
N7 C35 C36 113.4(5) . . ?
C65 C64 C62 119.1(7) . . ?
C38 C37 C36 109.9(5) . . ?
N10 C54 C55 109.6(5) . . ?
C10 C9 C8 119.8(6) . . ?
C47 C48 C49 122.6(6) . . ?
C49 C51 C52 119.5(6) . . ?
C32 C31 C30 118.2(8) . . ?
C28 C30 C31 120.1(8) . . ?
C26 C27 C28 123.2(9) . . ?
C27 C26 C24 121.3(8) . . ?
C23 C22 C21 118.7(8) . . ?
N12 C66 C65 122.6(7) . . ?
C64 C65 C66 120.6(7) . . ?
N8 C46 C50 114.5(5) . . ?
N8 C46 C45 124.2(6) . . ?
C50 C46 C45 121.2(6) . . ?
C44 C45 C46 114.5(6) . . ?
C44 C45 C47 128.7(6) . . ?
C46 C45 C47 116.7(6) . . ?
C48 C47 C45 122.1(6) . . ?
C62 C63 N12 125.8(6) . . ?
C62 C63 C59 119.8(6) . . ?
N12 C63 C59 114.3(5) . . ?
N9 C50 C46 114.7(6) . . ?
N9 C50 C49 124.0(6) . . ?
C46 C50 C49 121.3(6) . . ?
N8 C42 C43 119.9(6) . . ?
N8 C42 C41 112.9(6) . . ?
C43 C42 C41 127.1(6) . . ?
C42 C41 N7 109.1(5) . . ?
C43 C44 C45 121.5(6) . . ?
C23 C24 C25 116.1(8) . . ?
C23 C24 C26 127.2(7) . . ?
C25 C24 C26 116.7(8) . . ?
C24 C23 C22 120.7(7) . . ?
C51 C49 C50 117.5(6) . . ?
C51 C49 C48 126.4(6) . . ?
C50 C49 C48 116.0(6) . . ?
C44 C43 C42 119.3(6) . . ?
C6 C1 N1 110.5(5) . . ?
C6 C1 C2 110.0(5) . . ?
N1 C1 C2 113.8(6) . . ?
C3 C2 C1 111.4(6) . . ?
C6 C5 C4 110.6(6) . . ?
C35 C40 N10 110.4(5) . . ?
C35 C40 C39 110.9(5) . . ?
N10 C40 C39 113.7(6) . . ?
C38 C39 C40 111.6(6) . . ?
C39 C38 C37 110.6(5) . . ?
C3 C4 C5 110.9(6) . . ?
C4 C3 C2 110.5(6) . . ?
C14 C13 C11 120.4(6) . . ?
C13 C14 C15 123.7(6) . . ?
F1 B1 F3 113.2(7) . . ?
F1 B1 F4 115.1(8) . . ?
F3 B1 F4 111.3(6) . . ?
F1 B1 F2 102.8(7) . . ?
F3 B1 F2 108.7(7) . . ?
F4 B1 F2 104.9(7) . . ?
F7 B2 F6 110.1(7) . . ?
F7 B2 F5 109.6(6) . . ?
F6 B2 F5 109.2(7) . . ?
F7 B2 F8 110.2(7) . . ?
F6 B2 F8 108.9(6) . . ?
F5 B2 F8 108.8(6) . . ?
C33 N1 C7 110.8(5) . . ?
C33 N1 C1 113.8(5) . . ?
C7 N1 C1 106.4(5) . . ?
C33 N1 Fe1 112.3(4) . . ?
C7 N1 Fe1 107.2(4) . . ?
C1 N1 Fe1 105.9(4) . . ?
C32 N6 C29 115.8(6) . . ?
C32 N6 Fe1 133.4(5) . . ?
C29 N6 Fe1 110.8(5) . . ?
C21 N5 C25 119.5(6) . . ?
C21 N5 Fe1 123.0(5) . . ?
C25 N5 Fe1 117.1(5) . . ?
C8 N2 C12 118.8(5) . . ?
C8 N2 Fe1 123.3(4) . . ?
C12 N2 Fe1 117.6(4) . . ?
C19 N3 C16 117.5(5) . . ?
C19 N3 Fe1 132.2(4) . . ?
C16 N3 Fe1 110.2(4) . . ?
C34 N4 C20 108.8(5) . . ?
C34 N4 C6 112.3(5) . . ?
C20 N4 C6 106.2(5) . . ?
C34 N4 Fe1 114.0(4) . . ?
C20 N4 Fe1 107.7(4) . . ?
C6 N4 Fe1 107.5(4) . . ?
C55 N11 C59 118.7(6) . . ?
C55 N11 Fe2 122.9(5) . . ?
C59 N11 Fe2 118.3(4) . . ?
C67 N7 C41 109.5(5) . . ?
C67 N7 C35 112.4(5) . . ?
C41 N7 C35 107.2(4) . . ?
C67 N7 Fe2 113.8(4) . . ?
C41 N7 Fe2 107.6(4) . . ?
C35 N7 Fe2 106.0(4) . . ?
C68 N10 C54 108.9(5) . . ?
C68 N10 C40 113.6(5) . . ?
C54 N10 C40 107.2(5) . . ?
C68 N10 Fe2 112.5(4) . . ?
C54 N10 Fe2 107.7(4) . . ?
C40 N10 Fe2 106.5(4) . . ?
C42 N8 C46 120.3(5) . . ?
C42 N8 Fe2 122.1(4) . . ?
C46 N8 Fe2 117.2(4) . . ?
C66 N12 C63 115.6(6) . . ?
C66 N12 Fe2 132.4(5) . . ?
C63 N12 Fe2 111.9(4) . . ?
F11 B3 F10 108.9(16) . . ?
F11 B3 F9 112.8(17) . . ?
F10 B3 F9 107.1(15) . . ?
F11 B3 F12 109.6(18) . . ?
F10 B3 F12 111.1(17) . . ?
F9 B3 F12 107.3(18) . . ?
F10' B3' F11' 115.6(14) . . ?
F10' B3' F9' 107.9(13) . . ?
F11' B3' F9' 107.3(12) . . ?
F10' B3' F12' 108.3(15) . . ?
F11' B3' F12' 108.0(15) . . ?
F9' B3' F12' 109.6(15) . . ?
C53 N9 C50 116.0(6) . . ?
C53 N9 Fe2 132.4(5) . . ?
C50 N9 Fe2 111.6(4) . . ?
F14 B4 F13 116.5(15) . . ?
F14 B4 F15 111.3(14) . . ?
F13 B4 F15 116.4(15) . . ?
F14 B4 F16 98.7(15) . . ?
F13 B4 F16 105.9(16) . . ?
F15 B4 F16 105.5(15) . . ?
F13' B4' F15' 113.8(17) . . ?
F13' B4' F16' 114.6(17) . . ?
F15' B4' F16' 107.7(13) . . ?
F13' B4' F14' 99.7(15) . . ?
F15' B4' F14' 118.3(16) . . ?
F16' B4' F14' 102.4(13) . . ?
N11 Fe2 N8 175.7(2) . . ?
N11 Fe2 N9 96.1(2) . . ?
N8 Fe2 N9 82.0(2) . . ?
N11 Fe2 N12 81.9(2) . . ?
N8 Fe2 N12 94.3(2) . . ?
N9 Fe2 N12 92.1(2) . . ?
N11 Fe2 N10 80.0(2) . . ?
N8 Fe2 N10 103.88(19) . . ?
N9 Fe2 N10 93.2(2) . . ?
N12 Fe2 N10 161.6(2) . . ?
N11 Fe2 N7 102.4(2) . . ?
N8 Fe2 N7 79.9(2) . . ?
N9 Fe2 N7 161.0(2) . . ?
N12 Fe2 N7 94.9(2) . . ?
N10 Fe2 N7 85.70(19) . . ?
N2 Fe1 N5 175.2(2) . . ?
N2 Fe1 N6 93.8(2) . . ?
N5 Fe1 N6 82.5(2) . . ?
N2 Fe1 N3 82.1(2) . . ?
N5 Fe1 N3 94.9(2) . . ?
N6 Fe1 N3 91.4(2) . . ?
N2 Fe1 N4 103.4(2) . . ?
N5 Fe1 N4 80.5(2) . . ?
N6 Fe1 N4 162.6(2) . . ?
N3 Fe1 N4 93.7(2) . . ?
N2 Fe1 N1 79.9(2) . . ?
N5 Fe1 N1 103.3(2) . . ?
N6 Fe1 N1 94.8(2) . . ?
N3 Fe1 N1 161.3(2) . . ?
N4 Fe1 N1 85.5(2) . . ?

_refine_diff_density_max         0.758
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.075


# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: During data collection measurement of standard frames
did indicate a slight decay of intensity. This is attributed to the
loss of packing solvents (diethyl ether and acetonitrile). Indeed,
a reliable refinement was possible only by using the SQUEEZE
procedure (cf. above), by which an electron count of 544 e/cell were
omitted.  That corresponds aproximately to three molecules diethyl
ether and one molecule acetonitrile. Therefore, very large VOIDS
are alerted as a level G alert. 
Finally, in order to avoid a full and/or further loss of intensity 
data collection has been restricted.
;
# end Validation Reply Form

_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
_database_code_depnum_ccdc_archive 'CCDC 1472620'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N6 Zn, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C36 H36 Cl2 N8 O8 Zn'
_chemical_formula_weight         845.00

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'
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'
Zn Zn 0.2839 1.4301 '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'

_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                   23.4625(1)
_cell_length_b                   10.3557(2)
_cell_length_c                   16.8781(4)
_cell_angle_alpha                90
_cell_angle_beta                 119.285(2)
_cell_angle_gamma                90
_cell_volume                     3576.78(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    8209
_cell_measurement_theta_min      2.9221
_cell_measurement_theta_max      24.9983


_exptl_crystal_description       block
_exptl_crystal_colour            colorless

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    0.902
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.89899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13625
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.134
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3132
_reflns_number_gt                2666
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0654P)²+1.9864P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3132
_refine_ls_number_parameters     273
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1023
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.097
_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
C2 C 0.4600(3) 0.6017(7) 0.6695(5) 0.0346(17) Uani 0.5 1 d D . P A 1
H2A H 0.4854 0.5969 0.6384 0.042 Uiso 0.5 1 calc R U P A 1
H2B H 0.4149 0.6167 0.6238 0.042 Uiso 0.5 1 calc R U P A 1
C3 C 0.4835(4) 0.7175(6) 0.7328(8) 0.040(4) Uani 0.5 1 d D . P A 1
H3A H 0.4615 0.7203 0.7687 0.048 Uiso 0.5 1 calc R U P A 1
H3B H 0.4735 0.7966 0.6976 0.048 Uiso 0.5 1 calc R U P A 1
C2' C 0.4290(3) 0.5877(7) 0.6460(5) 0.0315(17) Uani 0.5 1 d D . P A 2
H2'1 H 0.4466 0.5983 0.6051 0.038 Uiso 0.5 1 calc R U P A 2
H2'2 H 0.3823 0.5720 0.6102 0.038 Uiso 0.5 1 calc R U P A 2
C3' C 0.4420(3) 0.7064(6) 0.7041(6) 0.041(2) Uani 0.5 1 d D . P A 2
H3'1 H 0.4200 0.6994 0.7399 0.049 Uiso 0.5 1 calc R U P A 2
H3'2 H 0.4257 0.7826 0.6660 0.049 Uiso 0.5 1 calc R U P A 2
C4 C 0.37911(14) 0.3256(3) 0.6020(2) 0.0473(8) Uani 1 1 d . . . . .
H4A H 0.3701 0.2844 0.5454 0.057 Uiso 1 1 calc R U . . .
H4B H 0.3544 0.4055 0.5875 0.057 Uiso 1 1 calc R U . . .
C1 C 0.46400(16) 0.4707(2) 0.7139(2) 0.0492(8) Uani 1 1 d D . . . .
H1 H 0.4366 0.4711 0.7430 0.059 Uiso 0.5 1 calc R U P A 1
H1' H 0.4399 0.4587 0.7471 0.059 Uiso 0.5 1 calc R U P A 2
C5 C 0.35773(13) 0.2379(3) 0.65405(19) 0.0345(6) Uani 1 1 d . . . . .
C6 C 0.29205(13) 0.2212(3) 0.6315(2) 0.0432(7) Uani 1 1 d . . . . .
H6 H 0.2596 0.2722 0.5869 0.052 Uiso 1 1 calc R U . . .
C7 C 0.27647(13) 0.1292(3) 0.67597(19) 0.0416(7) Uani 1 1 d . . . . .
H7 H 0.2331 0.1169 0.6612 0.050 Uiso 1 1 calc R U . . .
C8 C 0.32571(12) 0.0534(3) 0.74383(18) 0.0319(6) Uani 1 1 d . . . . .
C9 C 0.39003(11) 0.0790(2) 0.76429(16) 0.0246(5) Uani 1 1 d . . . . .
C10 C 0.31496(14) -0.0493(3) 0.79268(19) 0.0390(7) Uani 1 1 d . . . . .
H10 H 0.2727 -0.0678 0.7805 0.047 Uiso 1 1 calc R U . . .
C11 C 0.36543(14) -0.1190(3) 0.85583(19) 0.0362(6) Uani 1 1 d . . . . .
H11 H 0.3570 -0.1864 0.8850 0.043 Uiso 1 1 calc R U . . .
C12 C 0.43155(13) -0.0917(2) 0.87898(16) 0.0291(6) Uani 1 1 d . . . . .
C13 C 0.44418(11) 0.0089(2) 0.83377(16) 0.0235(5) Uani 1 1 d . . . . .
C14 C 0.48606(14) -0.1590(2) 0.94584(18) 0.0341(6) Uani 1 1 d . . . . .
H14 H 0.4803 -0.2284 0.9762 0.041 Uiso 1 1 calc R U . . .
C15 C 0.54728(14) -0.1214(3) 0.96564(18) 0.0357(6) Uani 1 1 d . . . . .
H15 H 0.5837 -0.1634 1.0109 0.043 Uiso 1 1 calc R U . . .
C16 C 0.55494(13) -0.0185(2) 0.91694(17) 0.0307(6) Uani 1 1 d . . . . .
H16 H 0.5970 0.0061 0.9313 0.037 Uiso 1 1 calc R U . . .
C17 C 0.2770(2) 0.7055(4) 0.6345(3) 0.0922(16) Uani 1 1 d . . . . .
H17A H 0.3000 0.6695 0.6946 0.138 Uiso 1 1 calc R U . . .
H17C H 0.2445 0.7651 0.6311 0.138 Uiso 1 1 calc R U . . .
H17B H 0.3073 0.7500 0.6214 0.138 Uiso 1 1 calc R U . . .
C18 C 0.24580(17) 0.6033(4) 0.5694(2) 0.0620(10) Uani 1 1 d . . . . .
N1 N 0.44962(11) 0.3544(2) 0.65575(16) 0.0338(5) Uani 1 1 d D . . . .
N2 N 0.40451(9) 0.16903(19) 0.71903(14) 0.0258(5) Uani 1 1 d . . . . .
N3 N 0.50496(10) 0.04472(18) 0.85182(13) 0.0250(4) Uani 1 1 d . . . . .
N4 N 0.22148(15) 0.5225(4) 0.5189(2) 0.0766(10) Uani 1 1 d . . . . .
O1 O 0.55362(10) 0.3902(2) 0.59482(15) 0.0556(6) Uani 1 1 d . . . . .
O2 O 0.65135(13) 0.3711(3) 0.5931(2) 0.0897(10) Uani 1 1 d . . . . .
O3 O 0.64829(12) 0.4883(3) 0.70899(16) 0.0835(9) Uani 1 1 d . . . . .
O4 O 0.60184(14) 0.5664(2) 0.5630(2) 0.0824(9) Uani 1 1 d . . . . .
Cl1 Cl 0.61334(3) 0.45179(6) 0.61572(4) 0.02972(18) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.19574(4) 0.7500 0.02504(15) Uani 1 2 d S T P . .
H1N H 0.4669(13) 0.370(3) 0.6166(17) 0.039(8) Uiso 1 1 d 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
C2 C3 1.519(10) . ?
C2 C1 1.531(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C3' 1.543(11) 2_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2' C3' 1.508(10) . ?
C2' C1 1.593(8) . ?
C2' H2'1 0.9700 . ?
C2' H2'2 0.9700 . ?
C3' C3 1.543(11) 2_656 ?
C3' H3'1 0.9700 . ?
C3' H3'2 0.9700 . ?
C4 N1 1.477(4) . ?
C4 C5 1.510(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C1 N1 1.484(4) . ?
C1 C1 1.524(7) 2_656 ?
C1 H1 0.9800 . ?
C1 H1' 0.9800 . ?
C5 N2 1.318(3) . ?
C5 C6 1.406(4) . ?
C6 C7 1.369(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.403(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(3) . ?
C8 C10 1.442(4) . ?
C9 N2 1.350(3) . ?
C9 C13 1.435(3) . ?
C10 C11 1.351(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.430(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.406(3) . ?
C12 C14 1.408(4) . ?
C13 N3 1.356(3) . ?
C14 C15 1.362(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.410(4) . ?
C15 H15 0.9300 . ?
C16 N3 1.323(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.441(6) . ?
C17 H17A 0.9600 . ?
C17 H17C 0.9600 . ?
C17 H17B 0.9600 . ?
C18 N4 1.131(5) . ?
N1 Zn1 2.188(2) . ?
N1 H1N 0.941(17) . ?
N2 Zn1 2.0552(19) . ?
N3 Zn1 2.2841(19) . ?
O1 Cl1 1.4179(19) . ?
O2 Cl1 1.404(2) . ?
O3 Cl1 1.425(2) . ?
O4 Cl1 1.428(2) . ?
Zn1 N2 2.0552(19) 2_656 ?
Zn1 N1 2.188(2) 2_656 ?
Zn1 N3 2.2841(19) 2_656 ?

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
C3 C2 C1 116.2(7) . . ?
C3 C2 H2A 108.2 . . ?
C1 C2 H2A 108.2 . . ?
C3 C2 H2B 108.2 . . ?
C1 C2 H2B 108.2 . . ?
H2A C2 H2B 107.4 . . ?
C2 C3 H3A 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C3' C2' C1 106.5(6) . . ?
C3' C2' H2'1 110.4 . . ?
C1 C2' H2'1 110.4 . . ?
C3' C2' H2'2 110.4 . . ?
C1 C2' H2'2 110.4 . . ?
H2'1 C2' H2'2 108.6 . . ?
C2' C3' H3'1 110.1 . . ?
C2' C3' H3'2 110.1 . . ?
H3'1 C3' H3'2 108.4 . . ?
N1 C4 C5 110.8(2) . . ?
N1 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N1 C1 C1 109.43(19) . 2_656 ?
N1 C1 C2 117.1(4) . . ?
C1 C1 C2 99.8(3) 2_656 . ?
N1 C1 C2' 105.7(3) . . ?
C1 C1 C2' 123.7(3) 2_656 . ?
N1 C1 H1 110.0 . . ?
C1 C1 H1 110.0 2_656 . ?
C2 C1 H1 110.0 . . ?
N1 C1 H1' 105.6 . . ?
C1 C1 H1' 105.6 2_656 . ?
C2' C1 H1' 105.6 . . ?
N2 C5 C6 121.0(2) . . ?
N2 C5 C4 115.5(2) . . ?
C6 C5 C4 123.3(2) . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 120.2(2) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 117.0(2) . . ?
C9 C8 C10 117.9(2) . . ?
C7 C8 C10 125.1(2) . . ?
N2 C9 C8 122.1(2) . . ?
N2 C9 C13 116.4(2) . . ?
C8 C9 C13 121.5(2) . . ?
C11 C10 C8 121.0(2) . . ?
C11 C10 H10 119.5 . . ?
C8 C10 H10 119.5 . . ?
C10 C11 C12 121.7(2) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C13 C12 C14 116.8(2) . . ?
C13 C12 C11 119.1(2) . . ?
C14 C12 C11 124.0(2) . . ?
N3 C13 C12 124.0(2) . . ?
N3 C13 C9 117.3(2) . . ?
C12 C13 C9 118.8(2) . . ?
C15 C14 C12 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C12 C14 H14 120.3 . . ?
C14 C15 C16 119.5(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
N3 C16 C15 123.0(2) . . ?
N3 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
N4 C18 C17 179.4(5) . . ?
C4 N1 C1 113.2(2) . . ?
C4 N1 Zn1 109.81(15) . . ?
C1 N1 Zn1 105.12(17) . . ?
C4 N1 H1N 109.9(17) . . ?
C1 N1 H1N 106.9(17) . . ?
Zn1 N1 H1N 111.9(17) . . ?
C5 N2 C9 120.5(2) . . ?
C5 N2 Zn1 119.94(16) . . ?
C9 N2 Zn1 119.60(16) . . ?
C16 N3 C13 117.3(2) . . ?
C16 N3 Zn1 131.45(17) . . ?
C13 N3 Zn1 110.93(15) . . ?
O2 Cl1 O1 110.29(15) . . ?
O2 Cl1 O3 111.07(19) . . ?
O1 Cl1 O3 111.03(13) . . ?
O2 Cl1 O4 106.07(19) . . ?
O1 Cl1 O4 110.87(16) . . ?
O3 Cl1 O4 107.37(19) . . ?
N2 Zn1 N2 164.53(11) . 2_656 ?
N2 Zn1 N1 114.83(8) . 2_656 ?
N2 Zn1 N1 77.42(8) 2_656 2_656 ?
N2 Zn1 N1 77.42(8) . . ?
N2 Zn1 N1 114.83(8) 2_656 . ?
N1 Zn1 N1 82.65(13) 2_656 . ?
N2 Zn1 N3 93.93(8) . 2_656 ?
N2 Zn1 N3 75.36(7) 2_656 2_656 ?
N1 Zn1 N3 150.66(7) 2_656 2_656 ?
N1 Zn1 N3 99.01(8) . 2_656 ?
N2 Zn1 N3 75.36(7) . . ?
N2 Zn1 N3 93.93(8) 2_656 . ?
N1 Zn1 N3 99.01(8) 2_656 . ?
N1 Zn1 N3 150.66(7) . . ?
N3 Zn1 N3 93.58(9) 2_656 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C3' 67.4(11) . . . 2_656 ?
C1 C2' C3' C3 53.7(9) . . . 2_656 ?
C3 C2 C1 N1 -172.1(6) . . . . ?
C3 C2 C1 C1 -54.3(7) . . . 2_656 ?
C3 C2 C1 C2' 121.5(16) . . . . ?
C3' C2' C1 N1 179.0(4) . . . . ?
C3' C2' C1 C1 -54.0(7) . . . 2_656 ?
C3' C2' C1 C2 -59.0(12) . . . . ?
N1 C4 C5 N2 -22.1(4) . . . . ?
N1 C4 C5 C6 162.8(3) . . . . ?
N2 C5 C6 C7 -2.0(5) . . . . ?
C4 C5 C6 C7 172.8(3) . . . . ?
C5 C6 C7 C8 0.6(5) . . . . ?
C6 C7 C8 C9 1.5(4) . . . . ?
C6 C7 C8 C10 -177.5(3) . . . . ?
C7 C8 C9 N2 -2.4(4) . . . . ?
C10 C8 C9 N2 176.7(2) . . . . ?
C7 C8 C9 C13 178.8(2) . . . . ?
C10 C8 C9 C13 -2.1(4) . . . . ?
C9 C8 C10 C11 -0.4(4) . . . . ?
C7 C8 C10 C11 178.7(3) . . . . ?
C8 C10 C11 C12 1.9(4) . . . . ?
C10 C11 C12 C13 -1.0(4) . . . . ?
C10 C11 C12 C14 178.3(3) . . . . ?
C14 C12 C13 N3 -0.9(4) . . . . ?
C11 C12 C13 N3 178.4(2) . . . . ?
C14 C12 C13 C9 179.2(2) . . . . ?
C11 C12 C13 C9 -1.4(3) . . . . ?
N2 C9 C13 N3 4.2(3) . . . . ?
C8 C9 C13 N3 -176.9(2) . . . . ?
N2 C9 C13 C12 -175.9(2) . . . . ?
C8 C9 C13 C12 3.0(4) . . . . ?
C13 C12 C14 C15 2.4(4) . . . . ?
C11 C12 C14 C15 -177.0(2) . . . . ?
C12 C14 C15 C16 -1.9(4) . . . . ?
C14 C15 C16 N3 -0.1(4) . . . . ?
C5 C4 N1 C1 -89.7(3) . . . . ?
C5 C4 N1 Zn1 27.5(3) . . . . ?
C1 C1 N1 C4 163.3(2) 2_656 . . . ?
C2 C1 N1 C4 -84.2(4) . . . . ?
C2' C1 N1 C4 -61.4(4) . . . . ?
C1 C1 N1 Zn1 43.5(3) 2_656 . . . ?
C2 C1 N1 Zn1 155.9(4) . . . . ?
C2' C1 N1 Zn1 178.7(3) . . . . ?
C6 C5 N2 C9 1.2(4) . . . . ?
C4 C5 N2 C9 -174.0(2) . . . . ?
C6 C5 N2 Zn1 179.9(2) . . . . ?
C4 C5 N2 Zn1 4.7(3) . . . . ?
C8 C9 N2 C5 1.0(4) . . . . ?
C13 C9 N2 C5 179.9(2) . . . . ?
C8 C9 N2 Zn1 -177.63(18) . . . . ?
C13 C9 N2 Zn1 1.3(3) . . . . ?
C15 C16 N3 C13 1.5(3) . . . . ?
C15 C16 N3 Zn1 -171.37(18) . . . . ?
C12 C13 N3 C16 -1.0(3) . . . . ?
C9 C13 N3 C16 178.9(2) . . . . ?
C12 C13 N3 Zn1 173.31(18) . . . . ?
C9 C13 N3 Zn1 -6.9(2) . . . . ?

_refine_diff_density_max         0.803
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.059

# start Validation Reply Form
_vrf_PLAT410_shelx               
;
PROBLEM: Short Intra H...H Contact  H2'2   ..  H4B     ..       1.82 Ang.  
RESPONSE: Alerted are hydrogen atoms, of which one (H2'2) originates from
a disordered cyclohexyl ring. Likely, the model choosen for this 
disorder is 'wrong' - however, no better model could be refined reliably. 
Additionally, the use of further SHELXL constraints/restraints as DANG etc. 
did not help to bring the corresponding carbon atoms farer away to each other.   
;
# end Validation Reply Form

_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
_database_code_depnum_ccdc_archive 'CCDC 1472621'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C32 H28 N6 Zn), 2(C32 H28 Fe N6), C4 H6 N2, 8(Cl O4)'
_chemical_formula_sum            'C132 H126 Cl8 Fe2 N26 O32 Zn2'
_chemical_formula_weight         3114.62


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'
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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 2'
_space_group_name_Hall           'I 2y'

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

_cell_length_a                   14.5861(3)
_cell_length_b                   13.0946(3)
_cell_length_c                   17.1156(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.518(2)
_cell_angle_gamma                90
_cell_volume                     3224.06(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    110
_cell_measurement_reflns_used    6481
_cell_measurement_theta_min      3.9920
_cell_measurement_theta_max      28.2430


_exptl_crystal_description       irregular
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_F_000             1604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.846
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.93858
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14257
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.020
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        25.000
_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 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.917
_reflns_number_total             5241
_reflns_number_gt                4802
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_max     0.829
_reflns_Friedel_fraction_full    0.829

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+2.3431P] 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 1941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.021(7)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         5241
_refine_ls_number_parameters     499
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0809
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002

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 0.4643(4) 0.3129(5) 0.4614(3) 0.0309(13) Uani 1 1 d . . . . .
H1A H 0.4019 0.3114 0.4757 0.037 Uiso 1 1 calc R U . . .
C2 C 0.4761(4) 0.2177(5) 0.4141(4) 0.0348(14) Uani 1 1 d . . . . .
H2A H 0.4297 0.2171 0.3664 0.042 Uiso 1 1 calc R U . . .
H2B H 0.5370 0.2183 0.3984 0.042 Uiso 1 1 calc R U . . .
C3 C 0.4660(5) 0.1229(5) 0.4618(4) 0.0455(16) Uani 1 1 d . . . . .
H3A H 0.4032 0.1191 0.4733 0.055 Uiso 1 1 calc R U . . .
H3B H 0.4766 0.0631 0.4309 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3873(4) 0.4303(5) 0.3588(3) 0.0389(14) Uani 1 1 d . . . . .
H4A H 0.3576 0.3665 0.3402 0.047 Uiso 1 1 calc R U . . .
H4B H 0.4025 0.4671 0.3135 0.047 Uiso 1 1 calc R U . . .
C5 C 0.3220(4) 0.4932(5) 0.3991(4) 0.0387(14) Uani 1 1 d . . . . .
C6 C 0.2255(5) 0.5007(6) 0.3723(4) 0.054(2) Uani 1 1 d . . . . .
H6 H 0.1977 0.4652 0.3276 0.065 Uiso 1 1 calc R U . . .
C7 C 0.1729(5) 0.5619(6) 0.4140(4) 0.054(2) Uani 1 1 d . . . . .
H7 H 0.1093 0.5677 0.3966 0.065 Uiso 1 1 calc R U . . .
C8 C 0.2142(4) 0.6154(5) 0.4820(4) 0.0462(16) Uani 1 1 d . . . . .
C9 C 0.3096(4) 0.6053(5) 0.5027(4) 0.0355(14) Uani 1 1 d . . . . .
C10 C 0.1663(5) 0.6786(6) 0.5311(4) 0.055(2) Uani 1 1 d . . . . .
H10 H 0.1021 0.6856 0.5193 0.066 Uiso 1 1 calc R U . . .
C11 C 0.2147(5) 0.7282(6) 0.5947(4) 0.054(2) Uani 1 1 d . . . . .
H11 H 0.1826 0.7678 0.6263 0.065 Uiso 1 1 calc R U . . .
C12 C 0.3118(5) 0.7212(5) 0.6139(4) 0.0447(18) Uani 1 1 d . . . . .
C13 C 0.3614(4) 0.6592(5) 0.5688(3) 0.0354(14) Uani 1 1 d . . . . .
C14 C 0.3661(5) 0.7770(5) 0.6757(3) 0.0489(18) Uani 1 1 d . . . . .
H14 H 0.3375 0.8217 0.7064 0.059 Uiso 1 1 calc R U . . .
C15 C 0.4599(5) 0.7653(5) 0.6900(3) 0.0494(18) Uani 1 1 d . . . . .
H15 H 0.4959 0.8012 0.7309 0.059 Uiso 1 1 calc R U . . .
C16 C 0.5016(4) 0.6990(5) 0.6430(3) 0.0375(14) Uani 1 1 d . . . . .
H16 H 0.5657 0.6905 0.6540 0.045 Uiso 1 1 calc R U . . .
C17 C 0.9689(4) 1.2488(4) 0.4607(3) 0.0257(11) Uani 1 1 d . . . . .
H17 H 0.9044 1.2484 0.4702 0.031 Uiso 1 1 calc R U . . .
C18 C 0.9828(4) 1.3453(4) 0.4127(3) 0.0306(13) Uani 1 1 d . . . . .
H18A H 1.0455 1.3462 0.4007 0.037 Uiso 1 1 calc R U . . .
H18B H 0.9397 1.3446 0.3631 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9666(4) 1.4413(5) 0.4601(3) 0.0312(13) Uani 1 1 d . . . . .
H19A H 0.9028 1.4426 0.4694 0.037 Uiso 1 1 calc R U . . .
H19B H 0.9770 1.5018 0.4301 0.037 Uiso 1 1 calc R U . . .
C20 C 0.9025(4) 1.1305(4) 0.3561(3) 0.0272(12) Uani 1 1 d . . . . .
H20A H 0.9209 1.0875 0.3153 0.033 Uiso 1 1 calc R U . . .
H20B H 0.8768 1.1933 0.3317 0.033 Uiso 1 1 calc R U . . .
C21 C 0.8313(4) 1.0769(5) 0.3947(3) 0.0272(12) Uani 1 1 d . . . . .
C22 C 0.7357(4) 1.0684(4) 0.3676(3) 0.0326(13) Uani 1 1 d . . . . .
H22 H 0.7085 1.1021 0.3217 0.039 Uiso 1 1 calc R U . . .
C23 C 0.6824(4) 1.0099(5) 0.4093(3) 0.0353(14) Uani 1 1 d . . . . .
H23 H 0.6189 1.0041 0.3913 0.042 Uiso 1 1 calc R U . . .
C24 C 0.7226(4) 0.9588(5) 0.4787(3) 0.0293(12) Uani 1 1 d . . . . .
C25 C 0.8180(3) 0.9723(4) 0.5013(3) 0.0242(11) Uani 1 1 d . . . . .
C26 C 0.6771(4) 0.8927(5) 0.5282(3) 0.0351(14) Uani 1 1 d . . . . .
H26 H 0.6131 0.8830 0.5162 0.042 Uiso 1 1 calc R U . . .
C27 C 0.7257(4) 0.8454(5) 0.5914(3) 0.0350(14) Uani 1 1 d . . . . .
H27 H 0.6938 0.8048 0.6226 0.042 Uiso 1 1 calc R U . . .
C28 C 0.8241(4) 0.8545(5) 0.6128(3) 0.0300(13) Uani 1 1 d . . . . .
C29 C 0.8699(4) 0.9192(4) 0.5668(3) 0.0236(11) Uani 1 1 d . . . . .
C30 C 0.8811(4) 0.8019(5) 0.6751(3) 0.0350(13) Uani 1 1 d . . . . .
H30 H 0.8550 0.7572 0.7075 0.042 Uiso 1 1 calc R U . . .
C31 C 0.9747(4) 0.8179(5) 0.6868(3) 0.0342(13) Uani 1 1 d . . . . .
H31 H 1.0127 0.7839 0.7276 0.041 Uiso 1 1 calc R U . . .
C32 C 1.0136(4) 0.8845(5) 0.6383(3) 0.0276(11) Uani 1 1 d . . . . .
H32 H 1.0777 0.8940 0.6484 0.033 Uiso 1 1 calc R U . . .
N1 N 0.4728(3) 0.4092(4) 0.4153(3) 0.0326(11) Uani 1 1 d . . . . .
H1 H 0.5251 0.4026 0.3863 0.039 Uiso 1 1 calc R U . . .
N1N N 0.087(2) 0.459(2) 0.1967(12) 0.083(10) Uani 0.25 1 d D U P A 1
C1N C 0.042(6) 0.487(9) 0.233(6) 0.25(3) Uani 0.25 1 d D U P A 1
C2N C -0.034(5) 0.539(8) 0.270(4) 0.23(3) Uani 0.25 1 d D U P A 1
H2N1 H -0.0323 0.5134 0.3230 0.349 Uiso 0.25 1 calc R U P A 1
H2N2 H -0.0935 0.5256 0.2392 0.349 Uiso 0.25 1 calc R U P A 1
H2N3 H -0.0229 0.6116 0.2725 0.349 Uiso 0.25 1 calc R U P A 1
N1N' N -0.0707(19) 0.610(3) 0.2961(17) 0.084(9) Uani 0.25 1 d D U P B 2
C1N' C -0.022(2) 0.563(2) 0.271(2) 0.077(12) Uani 0.25 1 d D U P B 2
C2N' C 0.040(2) 0.511(3) 0.225(2) 0.083(10) Uani 0.25 1 d D U P B 2
H2N4 H 0.0035 0.4791 0.1796 0.125 Uiso 0.25 1 calc R U P B 2
H2N5 H 0.0754 0.4600 0.2570 0.125 Uiso 0.25 1 calc R U P B 2
H2N6 H 0.0815 0.5598 0.2076 0.125 Uiso 0.25 1 calc R U P B 2
N2 N 0.3606(3) 0.5461(4) 0.4611(2) 0.0305(11) Uani 1 1 d . . . . .
N3 N 0.4532(3) 0.6468(4) 0.5825(2) 0.0315(11) Uani 1 1 d . . . . .
N4 N 0.9843(3) 1.1534(4) 0.4177(2) 0.0243(9) Uani 1 1 d . . . . .
H4 H 1.0404 1.1597 0.3934 0.029 Uiso 1 1 calc R U . . .
N5 N 0.8703(3) 1.0309(4) 0.4618(2) 0.0239(9) Uani 1 1 d . . . . .
N6 N 0.9649(3) 0.9355(3) 0.5784(2) 0.0249(10) Uani 1 1 d . . . . .
O1 O 0.7233(3) 0.1058(6) 0.6903(4) 0.099(2) Uani 1 1 d . . . . .
O2 O 0.7906(4) 0.1975(5) 0.5979(2) 0.0639(16) Uani 1 1 d . . . . .
O3 O 0.8845(3) 0.1084(4) 0.6978(2) 0.0439(11) Uani 1 1 d . . . . .
O4 O 0.8060(4) 0.2542(5) 0.7273(3) 0.0816(19) Uani 1 1 d . . . . .
O5 O 0.7800(3) 0.4586(5) 0.3130(3) 0.0673(16) Uani 1 1 d . . . . .
O6 O 0.7152(3) 0.3765(5) 0.4123(2) 0.0572(14) Uani 1 1 d . . . . .
O7 O 0.6937(3) 0.3089(4) 0.2829(3) 0.0553(12) Uani 1 1 d . . . . .
O8 O 0.6183(3) 0.4605(4) 0.3099(2) 0.0426(10) Uani 1 1 d . . . . .
Cl1 Cl 0.80065(9) 0.16587(13) 0.67938(7) 0.0364(4) Uani 1 1 d . . . . .
Cl2 Cl 0.70259(8) 0.40118(12) 0.32985(6) 0.0321(3) Uani 1 1 d . . . . .
Fe1 Fe 1.0000 1.03657(7) 0.5000 0.0206(2) Uani 1 2 d S T P . .
Zn1 Zn 0.5000 0.53404(5) 0.5000 0.0274(2) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.503(7) . ?
C1 C2 1.512(8) . ?
C1 C1 1.542(11) 2_656 ?
C1 H1A 0.9800 . ?
C2 C3 1.506(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C3 1.505(13) 2_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.471(8) . ?
C4 C5 1.510(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.314(8) . ?
C5 C6 1.409(9) . ?
C6 C7 1.385(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.406(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.385(9) . ?
C8 C10 1.440(10) . ?
C9 N2 1.355(7) . ?
C9 C13 1.438(9) . ?
C10 C11 1.360(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.402(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.401(9) . ?
C12 C14 1.415(10) . ?
C13 N3 1.331(7) . ?
C14 C15 1.359(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.390(8) . ?
C15 H15 0.9300 . ?
C16 N3 1.339(8) . ?
C16 H16 0.9300 . ?
C17 N4 1.485(7) . ?
C17 C17 1.493(10) 2_756 ?
C17 C18 1.540(8) . ?
C17 H17 0.9800 . ?
C18 C19 1.536(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C19 1.542(11) 2_756 ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.486(7) . ?
C20 C21 1.494(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N5 1.337(6) . ?
C21 C22 1.399(8) . ?
C22 C23 1.373(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(7) . ?
C24 C26 1.447(8) . ?
C25 N5 1.341(7) . ?
C25 C29 1.425(7) . ?
C26 C27 1.343(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.426(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.399(8) . ?
C28 C30 1.417(8) . ?
C29 N6 1.383(7) . ?
C30 C31 1.363(8) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(8) . ?
C31 H31 0.9300 . ?
C32 N6 1.327(6) . ?
C32 H32 0.9300 . ?
N1 Zn1 2.178(5) . ?
N1 H1 0.9800 . ?
N1N C1N 1.04(3) . ?
C1N C2N 1.53(2) . ?
C2N H2N1 0.9882 . ?
C2N H2N2 0.9872 . ?
C2N H2N3 0.9884 . ?
N1N' C1N' 1.09(2) . ?
C1N' C2N' 1.46(2) . ?
C2N' H2N4 0.9618 . ?
C2N' H2N5 0.9618 . ?
C2N' H2N6 0.9618 . ?
N2 Zn1 2.038(4) . ?
N3 Zn1 2.227(5) . ?
N4 Fe1 2.067(4) . ?
N4 H4 0.9800 . ?
N5 Fe1 1.899(4) . ?
N6 Fe1 2.010(4) . ?
O1 Cl1 1.413(5) . ?
O2 Cl1 1.439(5) . ?
O3 Cl1 1.426(4) . ?
O4 Cl1 1.412(6) . ?
O5 Cl2 1.425(5) . ?
O6 Cl2 1.430(4) . ?
O7 Cl2 1.445(5) . ?
O8 Cl2 1.446(4) . ?
Fe1 N5 1.899(4) 2_756 ?
Fe1 N6 2.010(4) 2_756 ?
Fe1 N4 2.067(4) 2_756 ?
Zn1 N2 2.038(4) 2_656 ?
Zn1 N1 2.178(5) 2_656 ?
Zn1 N3 2.227(5) 2_656 ?

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 112.6(4) . . ?
N1 C1 C1 110.3(4) . 2_656 ?
C2 C1 C1 109.8(4) . 2_656 ?
N1 C1 H1A 108.0 . . ?
C2 C1 H1A 108.0 . . ?
C1 C1 H1A 108.0 2_656 . ?
C3 C2 C1 111.1(5) . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C3 C3 C2 111.2(4) 2_656 . ?
C3 C3 H3A 109.4 2_656 . ?
C2 C3 H3A 109.4 . . ?
C3 C3 H3B 109.4 2_656 . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N1 C4 C5 109.4(4) . . ?
N1 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 119.9(6) . . ?
N2 C5 C4 115.9(5) . . ?
C6 C5 C4 124.1(6) . . ?
C7 C6 C5 118.7(7) . . ?
C7 C6 H6 120.6 . . ?
C5 C6 H6 120.6 . . ?
C6 C7 C8 121.1(6) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 116.0(6) . . ?
C9 C8 C10 118.0(7) . . ?
C7 C8 C10 126.0(7) . . ?
N2 C9 C8 122.5(6) . . ?
N2 C9 C13 115.5(5) . . ?
C8 C9 C13 122.0(6) . . ?
C11 C10 C8 120.2(6) . . ?
C11 C10 H10 119.9 . . ?
C8 C10 H10 119.9 . . ?
C10 C11 C12 121.8(7) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 120.2(7) . . ?
C13 C12 C14 115.8(6) . . ?
C11 C12 C14 124.0(6) . . ?
N3 C13 C12 124.7(6) . . ?
N3 C13 C9 117.5(5) . . ?
C12 C13 C9 117.7(6) . . ?
C15 C14 C12 119.9(6) . . ?
C15 C14 H14 120.0 . . ?
C12 C14 H14 120.0 . . ?
C14 C15 C16 119.3(7) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.4 . . ?
N3 C16 C15 122.8(6) . . ?
N3 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
N4 C17 C17 109.1(4) . 2_756 ?
N4 C17 C18 112.4(4) . . ?
C17 C17 C18 111.5(4) 2_756 . ?
N4 C17 H17 107.9 . . ?
C17 C17 H17 107.9 2_756 . ?
C18 C17 H17 107.9 . . ?
C19 C18 C17 110.2(4) . . ?
C19 C18 H18A 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 C19 109.7(4) . 2_756 ?
C18 C19 H19A 109.7 . . ?
C19 C19 H19A 109.7 2_756 . ?
C18 C19 H19B 109.7 . . ?
C19 C19 H19B 109.7 2_756 . ?
H19A C19 H19B 108.2 . . ?
N4 C20 C21 108.5(4) . . ?
N4 C20 H20A 110.0 . . ?
C21 C20 H20A 110.0 . . ?
N4 C20 H20B 110.0 . . ?
C21 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
N5 C21 C22 120.6(5) . . ?
N5 C21 C20 111.3(4) . . ?
C22 C21 C20 128.1(5) . . ?
C23 C22 C21 119.4(5) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 120.9(5) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 115.6(5) . . ?
C25 C24 C26 116.5(5) . . ?
C23 C24 C26 127.8(5) . . ?
N5 C25 C24 123.9(5) . . ?
N5 C25 C29 113.8(4) . . ?
C24 C25 C29 122.2(5) . . ?
C27 C26 C24 121.0(5) . . ?
C27 C26 H26 119.5 . . ?
C24 C26 H26 119.5 . . ?
C26 C27 C28 122.9(5) . . ?
C26 C27 H27 118.6 . . ?
C28 C27 H27 118.5 . . ?
C29 C28 C30 116.2(5) . . ?
C29 C28 C27 117.4(5) . . ?
C30 C28 C27 126.4(5) . . ?
N6 C29 C28 125.0(5) . . ?
N6 C29 C25 115.2(4) . . ?
C28 C29 C25 119.8(5) . . ?
C31 C30 C28 119.0(5) . . ?
C31 C30 H30 120.5 . . ?
C28 C30 H30 120.5 . . ?
C30 C31 C32 120.5(5) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
N6 C32 C31 123.9(5) . . ?
N6 C32 H32 118.1 . . ?
C31 C32 H32 118.1 . . ?
C4 N1 C1 111.6(5) . . ?
C4 N1 Zn1 109.7(4) . . ?
C1 N1 Zn1 107.6(3) . . ?
C4 N1 H1 109.3 . . ?
C1 N1 H1 109.3 . . ?
Zn1 N1 H1 109.3 . . ?
N1N C1N C2N 168(10) . . ?
C1N C2N H2N1 112.3 . . ?
C1N C2N H2N2 111.9 . . ?
H2N1 C2N H2N2 106.5 . . ?
C1N C2N H2N3 112.4 . . ?
H2N1 C2N H2N3 106.6 . . ?
H2N2 C2N H2N3 106.7 . . ?
N1N' C1N' C2N' 169(3) . . ?
C1N' C2N' H2N4 109.7 . . ?
C1N' C2N' H2N5 109.7 . . ?
H2N4 C2N' H2N5 109.3 . . ?
C1N' C2N' H2N6 109.5 . . ?
H2N4 C2N' H2N6 109.3 . . ?
H2N5 C2N' H2N6 109.3 . . ?
C5 N2 C9 121.7(5) . . ?
C5 N2 Zn1 119.7(4) . . ?
C9 N2 Zn1 118.6(4) . . ?
C13 N3 C16 117.4(5) . . ?
C13 N3 Zn1 111.9(4) . . ?
C16 N3 Zn1 130.6(4) . . ?
C17 N4 C20 110.6(4) . . ?
C17 N4 Fe1 107.0(3) . . ?
C20 N4 Fe1 108.6(3) . . ?
C17 N4 H4 110.2 . . ?
C20 N4 H4 110.2 . . ?
Fe1 N4 H4 110.2 . . ?
C21 N5 C25 119.6(4) . . ?
C21 N5 Fe1 122.4(4) . . ?
C25 N5 Fe1 117.8(3) . . ?
C32 N6 C29 115.4(4) . . ?
C32 N6 Fe1 133.1(4) . . ?
C29 N6 Fe1 111.5(3) . . ?
O4 Cl1 O1 110.4(4) . . ?
O4 Cl1 O3 109.9(3) . . ?
O1 Cl1 O3 110.6(4) . . ?
O4 Cl1 O2 108.3(4) . . ?
O1 Cl1 O2 109.4(4) . . ?
O3 Cl1 O2 108.1(3) . . ?
O5 Cl2 O6 110.0(3) . . ?
O5 Cl2 O7 109.3(3) . . ?
O6 Cl2 O7 110.1(3) . . ?
O5 Cl2 O8 109.9(3) . . ?
O6 Cl2 O8 108.7(3) . . ?
O7 Cl2 O8 108.9(3) . . ?
N5 Fe1 N5 175.5(3) 2_756 . ?
N5 Fe1 N6 95.37(18) 2_756 . ?
N5 Fe1 N6 81.64(18) . . ?
N5 Fe1 N6 81.64(18) 2_756 2_756 ?
N5 Fe1 N6 95.37(18) . 2_756 ?
N6 Fe1 N6 97.6(2) . 2_756 ?
N5 Fe1 N4 78.62(19) 2_756 2_756 ?
N5 Fe1 N4 104.82(19) . 2_756 ?
N6 Fe1 N4 92.54(16) . 2_756 ?
N6 Fe1 N4 158.53(16) 2_756 2_756 ?
N5 Fe1 N4 104.82(19) 2_756 . ?
N5 Fe1 N4 78.62(19) . . ?
N6 Fe1 N4 158.53(16) . . ?
N6 Fe1 N4 92.54(16) 2_756 . ?
N4 Fe1 N4 84.5(2) 2_756 . ?
N2 Zn1 N2 171.1(3) . 2_656 ?
N2 Zn1 N1 109.77(19) . 2_656 ?
N2 Zn1 N1 77.2(2) 2_656 2_656 ?
N2 Zn1 N1 77.2(2) . . ?
N2 Zn1 N1 109.77(19) 2_656 . ?
N1 Zn1 N1 82.7(3) 2_656 . ?
N2 Zn1 N3 76.24(19) . . ?
N2 Zn1 N3 97.74(18) 2_656 . ?
N1 Zn1 N3 96.70(16) 2_656 . ?
N1 Zn1 N3 151.50(17) . . ?
N2 Zn1 N3 97.74(18) . 2_656 ?
N2 Zn1 N3 76.24(19) 2_656 2_656 ?
N1 Zn1 N3 151.50(17) 2_656 2_656 ?
N1 Zn1 N3 96.69(16) . 2_656 ?
N3 Zn1 N3 96.9(2) . 2_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -179.3(5) . . . . ?
C1 C1 C2 C3 57.4(7) 2_656 . . . ?
C1 C2 C3 C3 -56.6(8) . . . 2_656 ?
N1 C4 C5 N2 23.0(7) . . . . ?
N1 C4 C5 C6 -159.6(6) . . . . ?
N2 C5 C6 C7 -2.0(9) . . . . ?
C4 C5 C6 C7 -179.3(6) . . . . ?
C5 C6 C7 C8 -0.4(10) . . . . ?
C6 C7 C8 C9 1.9(9) . . . . ?
C6 C7 C8 C10 -178.1(6) . . . . ?
C7 C8 C9 N2 -1.2(9) . . . . ?
C10 C8 C9 N2 178.8(5) . . . . ?
C7 C8 C9 C13 177.3(6) . . . . ?
C10 C8 C9 C13 -2.7(8) . . . . ?
C9 C8 C10 C11 1.3(9) . . . . ?
C7 C8 C10 C11 -178.6(7) . . . . ?
C8 C10 C11 C12 1.1(10) . . . . ?
C10 C11 C12 C13 -2.2(10) . . . . ?
C10 C11 C12 C14 175.1(6) . . . . ?
C11 C12 C13 N3 -179.5(5) . . . . ?
C14 C12 C13 N3 3.0(9) . . . . ?
C11 C12 C13 C9 0.9(9) . . . . ?
C14 C12 C13 C9 -176.7(5) . . . . ?
N2 C9 C13 N3 0.5(8) . . . . ?
C8 C9 C13 N3 -178.1(5) . . . . ?
N2 C9 C13 C12 -179.8(5) . . . . ?
C8 C9 C13 C12 1.6(8) . . . . ?
C13 C12 C14 C15 -2.6(9) . . . . ?
C11 C12 C14 C15 180.0(6) . . . . ?
C12 C14 C15 C16 0.7(9) . . . . ?
C14 C15 C16 N3 1.3(9) . . . . ?
N4 C17 C18 C19 -179.7(5) . . . . ?
C17 C17 C18 C19 -56.9(6) 2_756 . . . ?
C17 C18 C19 C19 57.9(6) . . . 2_756 ?
N4 C20 C21 N5 -23.6(6) . . . . ?
N4 C20 C21 C22 158.7(6) . . . . ?
N5 C21 C22 C23 -1.8(9) . . . . ?
C20 C21 C22 C23 175.7(5) . . . . ?
C21 C22 C23 C24 0.1(9) . . . . ?
C22 C23 C24 C25 0.3(8) . . . . ?
C22 C23 C24 C26 -178.5(5) . . . . ?
C23 C24 C25 N5 0.9(8) . . . . ?
C26 C24 C25 N5 179.9(5) . . . . ?
C23 C24 C25 C29 -175.0(5) . . . . ?
C26 C24 C25 C29 3.9(8) . . . . ?
C25 C24 C26 C27 -1.7(8) . . . . ?
C23 C24 C26 C27 177.1(6) . . . . ?
C24 C26 C27 C28 -1.5(9) . . . . ?
C26 C27 C28 C29 2.5(9) . . . . ?
C26 C27 C28 C30 -175.5(6) . . . . ?
C30 C28 C29 N6 -0.6(8) . . . . ?
C27 C28 C29 N6 -178.8(5) . . . . ?
C30 C28 C29 C25 177.9(5) . . . . ?
C27 C28 C29 C25 -0.3(8) . . . . ?
N5 C25 C29 N6 -0.7(7) . . . . ?
C24 C25 C29 N6 175.7(4) . . . . ?
N5 C25 C29 C28 -179.3(5) . . . . ?
C24 C25 C29 C28 -3.0(8) . . . . ?
C29 C28 C30 C31 0.7(8) . . . . ?
C27 C28 C30 C31 178.7(5) . . . . ?
C28 C30 C31 C32 -0.1(9) . . . . ?
C30 C31 C32 N6 -0.6(9) . . . . ?
C5 C4 N1 C1 88.9(5) . . . . ?
C5 C4 N1 Zn1 -30.2(5) . . . . ?
C2 C1 N1 C4 78.0(6) . . . . ?
C1 C1 N1 C4 -159.0(5) 2_656 . . . ?
C2 C1 N1 Zn1 -161.6(4) . . . . ?
C1 C1 N1 Zn1 -38.6(6) 2_656 . . . ?
C6 C5 N2 C9 2.7(9) . . . . ?
C4 C5 N2 C9 -179.7(5) . . . . ?
C6 C5 N2 Zn1 179.5(4) . . . . ?
C4 C5 N2 Zn1 -2.9(7) . . . . ?
C8 C9 N2 C5 -1.1(9) . . . . ?
C13 C9 N2 C5 -179.7(5) . . . . ?
C8 C9 N2 Zn1 -177.9(4) . . . . ?
C13 C9 N2 Zn1 3.5(7) . . . . ?
C12 C13 N3 C16 -1.3(8) . . . . ?
C9 C13 N3 C16 178.4(5) . . . . ?
C12 C13 N3 Zn1 176.6(5) . . . . ?
C9 C13 N3 Zn1 -3.7(6) . . . . ?
C15 C16 N3 C13 -1.0(8) . . . . ?
C15 C16 N3 Zn1 -178.3(4) . . . . ?
C17 C17 N4 C20 158.1(5) 2_756 . . . ?
C18 C17 N4 C20 -77.7(5) . . . . ?
C17 C17 N4 Fe1 40.0(5) 2_756 . . . ?
C18 C17 N4 Fe1 164.2(4) . . . . ?
C21 C20 N4 C17 -82.9(5) . . . . ?
C21 C20 N4 Fe1 34.2(5) . . . . ?
C22 C21 N5 C25 3.0(8) . . . . ?
C20 C21 N5 C25 -174.9(5) . . . . ?
C22 C21 N5 Fe1 178.2(4) . . . . ?
C20 C21 N5 Fe1 0.4(7) . . . . ?
C24 C25 N5 C21 -2.6(8) . . . . ?
C29 C25 N5 C21 173.6(5) . . . . ?
C24 C25 N5 Fe1 -178.1(4) . . . . ?
C29 C25 N5 Fe1 -1.8(6) . . . . ?
C31 C32 N6 C29 0.7(8) . . . . ?
C31 C32 N6 Fe1 179.1(4) . . . . ?
C28 C29 N6 C32 -0.1(7) . . . . ?
C25 C29 N6 C32 -178.7(5) . . . . ?
C28 C29 N6 Fe1 -178.8(4) . . . . ?
C25 C29 N6 Fe1 2.6(6) . . . . ?
C21 N5 Fe1 N6 -172.7(5) . . . . ?
C25 N5 Fe1 N6 2.6(4) . . . . ?
C21 N5 Fe1 N6 -75.8(5) . . . 2_756 ?
C25 N5 Fe1 N6 99.5(4) . . . 2_756 ?
C21 N5 Fe1 N4 96.8(5) . . . 2_756 ?
C25 N5 Fe1 N4 -87.8(4) . . . 2_756 ?
C21 N5 Fe1 N4 15.7(5) . . . . ?
C25 N5 Fe1 N4 -168.9(5) . . . . ?

_refine_diff_density_max         0.387
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.051

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT113_shelx               
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space group.       I2/a Check 
RESPONSE: The cocrystallized Fe(II) and Zn(II) complex
have been made from commercially available enantiopure starting materials.
Consequently, a centre of symmetry cannot be observed.
;
_vrf_PLAT415_shelx               
;
PROBLEM: Short Inter D-H..H-X       H19B   ..  H2N1    ..       1.82 Ang.  
RESPONSE: Hydrogen atom H2N1 corresponds to a partially occupated and
disordered MeCN molecule as packing solvent. Obviously, it interacts with
additional hydrogen atoms and its refinement is questionable. However, all
trials to refine this MeCN molecule in other orientations and/or with a 
different model of its disorder lead to non-reliable results only.
;
_vrf_PLAT090_shelx               
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.99 Note  
RESPONSE: ...
;
_vrf_PLAT111_shelx               
;
PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry .....        100 %Fit  
RESPONSE: The cocrystallized Fe(II) and Zn(II) complex
have been made from commercially available enantiopure starting materials.
Consequently, a centre of symmetry cannot be observed.
;
_vrf_PLAT987_shelx               
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The Flack x is within 3sigma standard deviation almost 0,
cf. above and below

_refine_ls_abs_structure_Flack    0.021(7)

By doing a BASF/TWIN refinement no significantly different data have
been obtained.
;
# end Validation Reply Form
####################################################################### 
# 
# 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 1472622'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2016-07-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H34 Fe N6, 2(B F4)'
_chemical_formula_sum            'C30 H34 B2 F8 Fe N6'
_chemical_formula_weight         708.10

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'
N N 0.0061 0.0033 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.0747(5)
_cell_length_b                   9.8281(3)
_cell_length_c                   36.0100(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.327(3)
_cell_angle_gamma                90
_cell_volume                     5979.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    115
_cell_measurement_reflns_used    12470
_cell_measurement_theta_min      3.2700
_cell_measurement_theta_max      27.7770


_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             2912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.589
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.75173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41l (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.870
_oxdiff_exptl_absorpt_empirical_full_max 1.455
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      115
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46925
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10500
_reflns_number_gt                8887
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²+10.3855P] 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         10500
_refine_ls_number_parameters     847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.1224
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.002
_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 1.04165(19) 0.4063(4) 0.12108(9) 0.0308(7) Uani 1 1 d . . . . .
H1 H 1.0321 0.3545 0.1432 0.037 Uiso 1 1 calc R U . . .
C2 C 0.96167(19) 0.4564(3) 0.10315(10) 0.0338(8) Uani 1 1 d . . . . .
H2A H 0.9260 0.3796 0.0984 0.041 Uiso 1 1 calc R U . . .
H2B H 0.9667 0.4983 0.0792 0.041 Uiso 1 1 calc R U . . .
C3 C 0.9263(2) 0.5592(4) 0.12770(11) 0.0371(8) Uani 1 1 d . . . . .
H3A H 0.8773 0.5945 0.1141 0.045 Uiso 1 1 calc R U . . .
H3B H 0.9141 0.5141 0.1501 0.045 Uiso 1 1 calc R U . . .
C4 C 0.9819(2) 0.6744(4) 0.13869(11) 0.0404(9) Uani 1 1 d . . . . .
H4A H 0.9584 0.7375 0.1546 0.049 Uiso 1 1 calc R U . . .
H4B H 0.9922 0.7230 0.1165 0.049 Uiso 1 1 calc R U . . .
C5 C 1.06025(19) 0.6183(3) 0.16000(10) 0.0327(8) Uani 1 1 d . . . . .
H5A H 1.0967 0.6928 0.1669 0.039 Uiso 1 1 calc R U . . .
H5B H 1.0501 0.5736 0.1828 0.039 Uiso 1 1 calc R U . . .
C6 C 1.09737(19) 0.5168(4) 0.13544(10) 0.0323(8) Uani 1 1 d . . . . .
H6 H 1.1093 0.5675 0.1135 0.039 Uiso 1 1 calc R U . . .
C7 C 1.04422(18) 0.1732(3) 0.10026(9) 0.0264(7) Uani 1 1 d . . . . .
H7A H 1.0550 0.1154 0.0798 0.032 Uiso 1 1 calc R U . . .
H7B H 0.9873 0.1838 0.0986 0.032 Uiso 1 1 calc R U . . .
C8 C 1.07680(17) 0.1095(3) 0.13701(9) 0.0244(7) Uani 1 1 d . . . . .
C9 C 1.04017(19) 0.0161(3) 0.15729(9) 0.0297(7) Uani 1 1 d . . . . .
H9 H 0.9879 -0.0093 0.1495 0.036 Uiso 1 1 calc R U . . .
C10 C 1.0827(2) -0.0395(3) 0.18950(10) 0.0321(8) Uani 1 1 d . . . . .
H10 H 1.0581 -0.0995 0.2041 0.038 Uiso 1 1 calc R U . . .
C11 C 1.1612(2) -0.0061(3) 0.19987(9) 0.0305(7) Uani 1 1 d . . . . .
H11 H 1.1908 -0.0473 0.2205 0.037 Uiso 1 1 calc R U . . .
C12 C 1.19519(18) 0.0900(3) 0.17894(8) 0.0240(7) Uani 1 1 d . . . . .
C13 C 1.27628(18) 0.1424(3) 0.18528(8) 0.0249(7) Uani 1 1 d . . . . .
C14 C 1.3339(2) 0.0999(4) 0.21395(9) 0.0310(7) Uani 1 1 d . . . . .
H14 H 1.3231 0.0298 0.2298 0.037 Uiso 1 1 calc R U . . .
C15 C 1.4072(2) 0.1612(4) 0.21909(10) 0.0357(8) Uani 1 1 d . . . . .
H15 H 1.4461 0.1339 0.2384 0.043 Uiso 1 1 calc R U . . .
C16 C 1.42166(19) 0.2641(3) 0.19490(9) 0.0315(8) Uani 1 1 d . . . . .
H16 H 1.4699 0.3097 0.1983 0.038 Uiso 1 1 calc R U . . .
C17 C 1.36363(18) 0.2982(3) 0.16572(9) 0.0257(7) Uani 1 1 d . . . . .
H17 H 1.3750 0.3643 0.1488 0.031 Uiso 1 1 calc R U . . .
C18 C 1.2374(2) 0.5579(4) 0.15122(10) 0.0337(8) Uani 1 1 d . . . . .
H18A H 1.2811 0.5432 0.1712 0.040 Uiso 1 1 calc R U . . .
H18B H 1.2170 0.6490 0.1539 0.040 Uiso 1 1 calc R U . . .
C19 C 1.26644(17) 0.5451(3) 0.11378(9) 0.0251(7) Uani 1 1 d . . . . .
C20 C 1.31211(19) 0.6387(3) 0.09783(10) 0.0307(7) Uani 1 1 d . . . . .
H20 H 1.3206 0.7251 0.1082 0.037 Uiso 1 1 calc R U . . .
C21 C 1.3450(2) 0.6024(3) 0.06638(10) 0.0330(8) Uani 1 1 d . . . . .
H21 H 1.3752 0.6649 0.0552 0.040 Uiso 1 1 calc R U . . .
C22 C 1.33290(19) 0.4721(3) 0.05147(9) 0.0300(7) Uani 1 1 d . . . . .
H22 H 1.3558 0.4455 0.0307 0.036 Uiso 1 1 calc R U . . .
C23 C 1.28581(17) 0.3827(3) 0.06839(8) 0.0225(6) Uani 1 1 d . . . . .
C24 C 1.26926(17) 0.2393(3) 0.05870(8) 0.0229(6) Uani 1 1 d . . . . .
C25 C 1.29418(19) 0.1738(4) 0.02839(9) 0.0290(7) Uani 1 1 d . . . . .
H25 H 1.3222 0.2210 0.0122 0.035 Uiso 1 1 calc R U . . .
C26 C 1.2769(2) 0.0378(4) 0.02255(9) 0.0328(8) Uani 1 1 d . . . . .
H26 H 1.2935 -0.0083 0.0025 0.039 Uiso 1 1 calc R U . . .
C27 C 1.2344(2) -0.0292(3) 0.04691(9) 0.0316(8) Uani 1 1 d . . . . .
H27 H 1.2212 -0.1205 0.0431 0.038 Uiso 1 1 calc R U . . .
C28 C 1.21171(18) 0.0405(3) 0.07679(9) 0.0255(7) Uani 1 1 d . . . . .
H28 H 1.1840 -0.0059 0.0933 0.031 Uiso 1 1 calc R U . . .
C29 C 1.07281(19) 0.3500(3) 0.05724(8) 0.0269(7) Uani 1 1 d . . . . .
H29A H 1.0970 0.4372 0.0551 0.040 Uiso 1 1 calc R U . . .
H29B H 1.0175 0.3554 0.0474 0.040 Uiso 1 1 calc R U . . .
H29C H 1.0979 0.2838 0.0433 0.040 Uiso 1 1 calc R U . . .
C30 C 1.1719(2) 0.4291(4) 0.19471(9) 0.0410(9) Uani 1 1 d . . . . .
H30A H 1.1313 0.3634 0.1970 0.062 Uiso 1 1 calc R U . . .
H30B H 1.1606 0.5119 0.2070 0.062 Uiso 1 1 calc R U . . .
H30C H 1.2222 0.3941 0.2061 0.062 Uiso 1 1 calc R U . . .
C31 C 0.59315(19) 0.0255(4) 0.13036(9) 0.0307(7) Uani 1 1 d . . . . .
H31 H 0.6092 -0.0278 0.1097 0.037 Uiso 1 1 calc R U . . .
C32 C 0.5475(2) -0.0700(4) 0.15294(10) 0.0340(8) Uani 1 1 d . . . . .
H32A H 0.5816 -0.1449 0.1625 0.041 Uiso 1 1 calc R U . . .
H32B H 0.5326 -0.0211 0.1742 0.041 Uiso 1 1 calc R U . . .
C33 C 0.4739(2) -0.1262(4) 0.12949(11) 0.0407(9) Uani 1 1 d . . . . .
H33A H 0.4885 -0.1800 0.1090 0.049 Uiso 1 1 calc R U . . .
H33B H 0.4457 -0.1847 0.1448 0.049 Uiso 1 1 calc R U . . .
C34 C 0.4215(2) -0.0102(4) 0.11421(13) 0.0482(11) Uani 1 1 d . . . . .
H34A H 0.4046 0.0398 0.1349 0.058 Uiso 1 1 calc R U . . .
H34B H 0.3746 -0.0460 0.0989 0.058 Uiso 1 1 calc R U . . .
C35 C 0.46448(19) 0.0866(4) 0.09055(11) 0.0388(9) Uani 1 1 d . . . . .
H35A H 0.4761 0.0395 0.0683 0.047 Uiso 1 1 calc R U . . .
H35B H 0.4305 0.1634 0.0825 0.047 Uiso 1 1 calc R U . . .
C36 C 0.54132(19) 0.1377(4) 0.11317(10) 0.0342(8) Uani 1 1 d . . . . .
H36 H 0.5263 0.1914 0.1340 0.041 Uiso 1 1 calc R U . . .
C37 C 0.73085(19) -0.0205(3) 0.15338(9) 0.0298(7) Uani 1 1 d . . . . .
H37A H 0.7092 -0.1103 0.1566 0.036 Uiso 1 1 calc R U . . .
H37B H 0.7717 -0.0027 0.1745 0.036 Uiso 1 1 calc R U . . .
C38 C 0.76554(17) -0.0151(3) 0.11734(9) 0.0240(7) Uani 1 1 d . . . . .
C39 C 0.81116(18) -0.1151(3) 0.10410(9) 0.0278(7) Uani 1 1 d . . . . .
H39 H 0.8159 -0.2003 0.1155 0.033 Uiso 1 1 calc R U . . .
C40 C 0.84968(19) -0.0872(3) 0.07385(9) 0.0298(7) Uani 1 1 d . . . . .
H40 H 0.8799 -0.1541 0.0644 0.036 Uiso 1 1 calc R U . . .
C41 C 0.84320(18) 0.0412(3) 0.05742(9) 0.0288(7) Uani 1 1 d . . . . .
H41 H 0.8701 0.0621 0.0375 0.035 Uiso 1 1 calc R U . . .
C42 C 0.79573(17) 0.1375(3) 0.07149(8) 0.0222(6) Uani 1 1 d . . . . .
C43 C 0.78507(18) 0.2802(3) 0.06027(8) 0.0244(7) Uani 1 1 d . . . . .
C44 C 0.8164(2) 0.3387(4) 0.03071(9) 0.0326(8) Uani 1 1 d . . . . .
H44 H 0.8437 0.2859 0.0154 0.039 Uiso 1 1 calc R U . . .
C45 C 0.8066(2) 0.4762(4) 0.02433(10) 0.0403(9) Uani 1 1 d . . . . .
H45 H 0.8279 0.5178 0.0049 0.048 Uiso 1 1 calc R U . . .
C46 C 0.7647(2) 0.5515(4) 0.04714(10) 0.0389(9) Uani 1 1 d . . . . .
H46 H 0.7572 0.6444 0.0431 0.047 Uiso 1 1 calc R U . . .
C47 C 0.7342(2) 0.4878(3) 0.07591(9) 0.0302(7) Uani 1 1 d . . . . .
H47 H 0.7062 0.5396 0.0911 0.036 Uiso 1 1 calc R U . . .
C48 C 0.55318(19) 0.3710(3) 0.09220(9) 0.0307(7) Uani 1 1 d . . . . .
H48A H 0.4959 0.3645 0.0877 0.037 Uiso 1 1 calc R U . . .
H48B H 0.5700 0.4276 0.0728 0.037 Uiso 1 1 calc R U . . .
C49 C 0.57951(18) 0.4329(3) 0.12996(9) 0.0269(7) Uani 1 1 d . . . . .
C50 C 0.53974(19) 0.5266(3) 0.14885(10) 0.0301(7) Uani 1 1 d . . . . .
H50 H 0.4887 0.5539 0.1391 0.036 Uiso 1 1 calc R U . . .
C51 C 0.5770(2) 0.5797(3) 0.18269(10) 0.0329(8) Uani 1 1 d . . . . .
H51 H 0.5500 0.6395 0.1963 0.039 Uiso 1 1 calc R U . . .
C52 C 0.65415(19) 0.5433(3) 0.19602(9) 0.0299(7) Uani 1 1 d . . . . .
H52 H 0.6806 0.5822 0.2178 0.036 Uiso 1 1 calc R U . . .
C53 C 0.69151(18) 0.4479(3) 0.17627(8) 0.0230(6) Uani 1 1 d . . . . .
C54 C 0.77141(17) 0.3920(3) 0.18581(8) 0.0230(6) Uani 1 1 d . . . . .
C55 C 0.82446(19) 0.4334(3) 0.21649(9) 0.0280(7) Uani 1 1 d . . . . .
H55 H 0.8113 0.5034 0.2318 0.034 Uiso 1 1 calc R U . . .
C56 C 0.89721(19) 0.3695(4) 0.22405(9) 0.0327(8) Uani 1 1 d . . . . .
H56 H 0.9333 0.3947 0.2448 0.039 Uiso 1 1 calc R U . . .
C57 C 0.91541(19) 0.2670(3) 0.20020(9) 0.0307(7) Uani 1 1 d . . . . .
H57 H 0.9637 0.2217 0.2048 0.037 Uiso 1 1 calc R U . . .
C58 C 0.86094(18) 0.2337(3) 0.16968(9) 0.0250(7) Uani 1 1 d . . . . .
H58 H 0.8742 0.1667 0.1535 0.030 Uiso 1 1 calc R U . . .
C59 C 0.6577(2) 0.1167(4) 0.19164(9) 0.0337(8) Uani 1 1 d . . . . .
H59A H 0.6170 0.1840 0.1919 0.051 Uiso 1 1 calc R U . . .
H59B H 0.7068 0.1514 0.2045 0.051 Uiso 1 1 calc R U . . .
H59C H 0.6434 0.0357 0.2040 0.051 Uiso 1 1 calc R U . . .
C60 C 0.5866(2) 0.1911(4) 0.05144(9) 0.0360(8) Uani 1 1 d . . . . .
H60A H 0.6095 0.1022 0.0504 0.054 Uiso 1 1 calc R U . . .
H60B H 0.6162 0.2552 0.0389 0.054 Uiso 1 1 calc R U . . .
H60C H 0.5327 0.1893 0.0393 0.054 Uiso 1 1 calc R U . . .
N1 N 1.08210(14) 0.3088(3) 0.09749(7) 0.0227(5) Uani 1 1 d . . . . .
N2 N 1.15190(14) 0.1491(3) 0.14886(7) 0.0218(5) Uani 1 1 d . . . . .
N3 N 1.29126(15) 0.2405(3) 0.16046(7) 0.0228(6) Uani 1 1 d . . . . .
N4 N 1.17447(15) 0.4571(3) 0.15413(7) 0.0229(6) Uani 1 1 d . . . . .
N5 N 1.25239(14) 0.4211(2) 0.09858(7) 0.0209(5) Uani 1 1 d . . . . .
N6 N 1.22822(14) 0.1732(2) 0.08304(7) 0.0211(5) Uani 1 1 d . . . . .
N7 N 0.66685(14) 0.0843(3) 0.15206(7) 0.0211(5) Uani 1 1 d . . . . .
N8 N 0.75697(14) 0.1074(2) 0.10071(7) 0.0194(5) Uani 1 1 d . . . . .
N9 N 0.74318(15) 0.3537(3) 0.08295(7) 0.0230(6) Uani 1 1 d . . . . .
N10 N 0.58888(15) 0.2324(3) 0.09118(7) 0.0269(6) Uani 1 1 d . . . . .
N11 N 0.65268(14) 0.3915(2) 0.14462(7) 0.0225(5) Uani 1 1 d . . . . .
N12 N 0.78917(14) 0.2930(2) 0.16196(7) 0.0214(5) Uani 1 1 d . . . . .
F1 F 1.05476(13) -0.1578(2) 0.00704(6) 0.0457(5) Uani 1 1 d . . . . .
F2 F 0.97729(12) -0.2970(2) 0.03654(6) 0.0446(5) Uani 1 1 d . . . . .
F3 F 1.11180(13) -0.3107(2) 0.04959(6) 0.0454(5) Uani 1 1 d . . . . .
F4 F 1.04675(15) -0.1281(2) 0.06882(7) 0.0593(7) Uani 1 1 d . . . . .
F5 F 0.82673(12) 0.7235(2) 0.18529(6) 0.0427(5) Uani 1 1 d . . . . .
F6 F 0.92008(14) 0.7210(2) 0.23741(7) 0.0573(7) Uani 1 1 d . . . . .
F7 F 0.80450(14) 0.8332(3) 0.23727(6) 0.0593(7) Uani 1 1 d . . . . .
F8 F 0.89650(13) 0.9130(2) 0.20291(7) 0.0523(6) Uani 1 1 d . . . . .
F9 F 1.39698(15) 0.6172(3) 0.20649(11) 0.1021(13) Uani 1 1 d . . . . .
F10 F 1.30380(15) 0.7193(3) 0.23534(7) 0.0660(7) Uani 1 1 d . . . . .
F11 F 1.33647(16) 0.8064(3) 0.18364(7) 0.0650(7) Uani 1 1 d . . . . .
F12 F 1.42434(15) 0.8157(3) 0.23697(9) 0.0769(9) Uani 1 1 d . . . . .
F13 F 1.37847(16) 0.1488(2) -0.04354(7) 0.0627(7) Uani 1 1 d . . . . .
F14 F 1.50713(14) 0.2037(3) -0.03809(7) 0.0633(7) Uani 1 1 d . . . . .
F15 F 1.4160(2) 0.3132(3) -0.07893(8) 0.0990(13) Uani 1 1 d . . . . .
F16 F 1.41826(16) 0.3472(2) -0.01679(7) 0.0667(8) Uani 1 1 d . . . . .
Fe1 Fe 1.19806(2) 0.28951(4) 0.12334(2) 0.01876(12) Uani 1 1 d . . . . .
Fe2 Fe 0.70123(2) 0.24641(4) 0.12177(2) 0.01881(12) Uani 1 1 d . . . . .
B1 B 1.0471(3) -0.2227(4) 0.04065(12) 0.0349(9) Uani 1 1 d . . . . .
B2 B 0.8626(2) 0.7985(4) 0.21605(11) 0.0323(9) Uani 1 1 d . . . . .
B3 B 1.3671(3) 0.7372(4) 0.21652(13) 0.0394(10) Uani 1 1 d . . . . .
B4 B 1.4305(3) 0.2547(4) -0.04421(12) 0.0351(9) 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 C6 1.486(5) . ?
C1 C2 1.506(4) . ?
C1 N1 1.512(4) . ?
C1 H1 0.9800 . ?
C2 C3 1.523(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.494(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.544(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.530(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N4 1.508(4) . ?
C6 H6 0.9800 . ?
C7 N1 1.491(4) . ?
C7 C8 1.496(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.349(4) . ?
C8 C9 1.379(4) . ?
C9 C10 1.388(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9300 . ?
C12 N2 1.351(4) . ?
C12 C13 1.464(4) . ?
C13 N3 1.364(4) . ?
C13 C14 1.383(4) . ?
C14 C15 1.377(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.380(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(4) . ?
C16 H16 0.9300 . ?
C17 N3 1.348(4) . ?
C17 H17 0.9300 . ?
C18 N4 1.477(4) . ?
C18 C19 1.507(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N5 1.344(4) . ?
C19 C20 1.383(4) . ?
C20 C21 1.382(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.393(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.390(4) . ?
C22 H22 0.9300 . ?
C23 N5 1.353(4) . ?
C23 C24 1.469(4) . ?
C24 N6 1.364(4) . ?
C24 C25 1.386(4) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.384(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.377(4) . ?
C27 H27 0.9300 . ?
C28 N6 1.346(4) . ?
C28 H28 0.9300 . ?
C29 N1 1.491(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N4 1.494(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C36 1.492(5) . ?
C31 N7 1.498(4) . ?
C31 C32 1.527(5) . ?
C31 H31 0.9800 . ?
C32 C33 1.514(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.503(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.534(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.526(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N10 1.529(4) . ?
C36 H36 0.9800 . ?
C37 N7 1.497(4) . ?
C37 C38 1.504(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 N8 1.344(4) . ?
C38 C39 1.381(4) . ?
C39 C40 1.379(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.391(5) . ?
C40 H40 0.9300 . ?
C41 C42 1.389(4) . ?
C41 H41 0.9300 . ?
C42 N8 1.354(4) . ?
C42 C43 1.464(4) . ?
C43 N9 1.367(4) . ?
C43 C44 1.384(4) . ?
C44 C45 1.377(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.380(5) . ?
C45 H45 0.9300 . ?
C46 C47 1.376(5) . ?
C46 H46 0.9300 . ?
C47 N9 1.347(4) . ?
C47 H47 0.9300 . ?
C48 N10 1.495(4) . ?
C48 C49 1.498(4) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 N11 1.347(4) . ?
C49 C50 1.381(4) . ?
C50 C51 1.392(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.382(5) . ?
C51 H51 0.9300 . ?
C52 C53 1.387(4) . ?
C52 H52 0.9300 . ?
C53 N11 1.351(4) . ?
C53 C54 1.464(4) . ?
C54 N12 1.361(4) . ?
C54 C55 1.384(4) . ?
C55 C56 1.383(5) . ?
C55 H55 0.9300 . ?
C56 C57 1.388(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.373(4) . ?
C57 H57 0.9300 . ?
C58 N12 1.349(4) . ?
C58 H58 0.9300 . ?
C59 N7 1.491(4) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 N10 1.483(4) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N1 Fe1 2.071(2) . ?
N2 Fe1 1.892(3) . ?
N3 Fe1 1.984(3) . ?
N4 Fe1 2.057(2) . ?
N5 Fe1 1.889(2) . ?
N6 Fe1 1.974(2) . ?
N7 Fe2 2.064(2) . ?
N8 Fe2 1.886(2) . ?
N9 Fe2 1.967(3) . ?
N10 Fe2 2.074(3) . ?
N11 Fe2 1.896(2) . ?
N12 Fe2 1.982(2) . ?
F1 B1 1.391(4) . ?
F2 B1 1.388(5) . ?
F3 B1 1.403(5) . ?
F4 B1 1.377(4) . ?
F5 B2 1.396(5) . ?
F6 B2 1.384(4) . ?
F7 B2 1.380(4) . ?
F8 B2 1.379(4) . ?
F9 B3 1.354(5) . ?
F10 B3 1.367(5) . ?
F11 B3 1.399(5) . ?
F12 B3 1.373(5) . ?
F13 B4 1.371(5) . ?
F14 B4 1.389(5) . ?
F15 B4 1.366(5) . ?
F16 B4 1.379(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 113.9(3) . . ?
C6 C1 N1 109.7(3) . . ?
C2 C1 N1 115.2(3) . . ?
C6 C1 H1 105.7 . . ?
C2 C1 H1 105.7 . . ?
N1 C1 H1 105.7 . . ?
C1 C2 C3 112.3(3) . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 111.5(3) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 C5 109.4(3) . . ?
C3 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 C4 110.3(3) . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C4 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C1 C6 N4 110.1(3) . . ?
C1 C6 C5 112.3(3) . . ?
N4 C6 C5 113.8(3) . . ?
C1 C6 H6 106.7 . . ?
N4 C6 H6 106.7 . . ?
C5 C6 H6 106.7 . . ?
N1 C7 C8 108.9(2) . . ?
N1 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N2 C8 C9 120.5(3) . . ?
N2 C8 C7 112.0(3) . . ?
C9 C8 C7 127.5(3) . . ?
C8 C9 C10 118.8(3) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 118.8(3) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
N2 C12 C11 120.3(3) . . ?
N2 C12 C13 111.6(3) . . ?
C11 C12 C13 128.0(3) . . ?
N3 C13 C14 121.5(3) . . ?
N3 C13 C12 114.2(3) . . ?
C14 C13 C12 124.3(3) . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 118.6(3) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C17 C16 C15 119.0(3) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N3 C17 C16 123.3(3) . . ?
N3 C17 H17 118.4 . . ?
C16 C17 H17 118.4 . . ?
N4 C18 C19 110.1(3) . . ?
N4 C18 H18A 109.6 . . ?
C19 C18 H18A 109.6 . . ?
N4 C18 H18B 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N5 C19 C20 120.8(3) . . ?
N5 C19 C18 112.2(3) . . ?
C20 C19 C18 126.4(3) . . ?
C21 C20 C19 119.3(3) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 119.9(3) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 118.4(3) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
N5 C23 C22 121.0(3) . . ?
N5 C23 C24 111.7(3) . . ?
C22 C23 C24 127.3(3) . . ?
N6 C24 C25 122.0(3) . . ?
N6 C24 C23 113.8(3) . . ?
C25 C24 C23 124.2(3) . . ?
C26 C25 C24 119.1(3) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 119.1(3) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C28 C27 C26 119.4(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
N6 C28 C27 122.5(3) . . ?
N6 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
N1 C29 H29A 109.5 . . ?
N1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N4 C30 H30A 109.5 . . ?
N4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C36 C31 N7 109.5(3) . . ?
C36 C31 C32 111.0(3) . . ?
N7 C31 C32 114.5(3) . . ?
C36 C31 H31 107.2 . . ?
N7 C31 H31 107.2 . . ?
C32 C31 H31 107.2 . . ?
C33 C32 C31 112.0(3) . . ?
C33 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
C31 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 109.2(3) . . ?
C34 C33 H33A 109.8 . . ?
C32 C33 H33A 109.8 . . ?
C34 C33 H33B 109.8 . . ?
C32 C33 H33B 109.8 . . ?
H33A C33 H33B 108.3 . . ?
C33 C34 C35 111.5(3) . . ?
C33 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 110.6(3) . . ?
C36 C35 H35A 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C31 C36 C35 113.0(3) . . ?
C31 C36 N10 109.7(3) . . ?
C35 C36 N10 113.8(3) . . ?
C31 C36 H36 106.6 . . ?
C35 C36 H36 106.6 . . ?
N10 C36 H36 106.6 . . ?
N7 C37 C38 109.0(2) . . ?
N7 C37 H37A 109.9 . . ?
C38 C37 H37A 109.9 . . ?
N7 C37 H37B 109.9 . . ?
C38 C37 H37B 109.9 . . ?
H37A C37 H37B 108.3 . . ?
N8 C38 C39 121.0(3) . . ?
N8 C38 C37 112.6(3) . . ?
C39 C38 C37 125.8(3) . . ?
C40 C39 C38 119.3(3) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
C39 C40 C41 119.9(3) . . ?
C39 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
C42 C41 C40 118.5(3) . . ?
C42 C41 H41 120.7 . . ?
C40 C41 H41 120.7 . . ?
N8 C42 C41 120.8(3) . . ?
N8 C42 C43 111.6(3) . . ?
C41 C42 C43 127.4(3) . . ?
N9 C43 C44 122.3(3) . . ?
N9 C43 C42 113.3(3) . . ?
C44 C43 C42 124.3(3) . . ?
C45 C44 C43 118.9(3) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C44 C45 C46 119.3(3) . . ?
C44 C45 H45 120.4 . . ?
C46 C45 H45 120.4 . . ?
C47 C46 C45 119.3(3) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
N9 C47 C46 122.8(3) . . ?
N9 C47 H47 118.6 . . ?
C46 C47 H47 118.6 . . ?
N10 C48 C49 108.8(3) . . ?
N10 C48 H48A 109.9 . . ?
C49 C48 H48A 109.9 . . ?
N10 C48 H48B 109.9 . . ?
C49 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
N11 C49 C50 120.2(3) . . ?
N11 C49 C48 111.9(3) . . ?
C50 C49 C48 127.9(3) . . ?
C49 C50 C51 119.1(3) . . ?
C49 C50 H50 120.5 . . ?
C51 C50 H50 120.5 . . ?
C52 C51 C50 120.0(3) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 118.9(3) . . ?
C51 C52 H52 120.6 . . ?
C53 C52 H52 120.6 . . ?
N11 C53 C52 120.2(3) . . ?
N11 C53 C54 111.8(3) . . ?
C52 C53 C54 128.0(3) . . ?
N12 C54 C55 122.3(3) . . ?
N12 C54 C53 113.9(3) . . ?
C55 C54 C53 123.8(3) . . ?
C56 C55 C54 119.3(3) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C55 C56 C57 118.9(3) . . ?
C55 C56 H56 120.6 . . ?
C57 C56 H56 120.6 . . ?
C58 C57 C56 118.8(3) . . ?
C58 C57 H57 120.6 . . ?
C56 C57 H57 120.6 . . ?
N12 C58 C57 123.5(3) . . ?
N12 C58 H58 118.2 . . ?
C57 C58 H58 118.2 . . ?
N7 C59 H59A 109.5 . . ?
N7 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N7 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N10 C60 H60A 109.5 . . ?
N10 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N10 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C7 N1 C29 108.7(2) . . ?
C7 N1 C1 106.9(2) . . ?
C29 N1 C1 112.4(2) . . ?
C7 N1 Fe1 106.49(18) . . ?
C29 N1 Fe1 114.96(18) . . ?
C1 N1 Fe1 106.87(18) . . ?
C8 N2 C12 121.0(3) . . ?
C8 N2 Fe1 120.0(2) . . ?
C12 N2 Fe1 119.0(2) . . ?
C17 N3 C13 117.4(3) . . ?
C17 N3 Fe1 128.5(2) . . ?
C13 N3 Fe1 113.9(2) . . ?
C18 N4 C30 108.5(3) . . ?
C18 N4 C6 107.7(3) . . ?
C30 N4 C6 111.1(3) . . ?
C18 N4 Fe1 107.31(18) . . ?
C30 N4 Fe1 114.6(2) . . ?
C6 N4 Fe1 107.31(18) . . ?
C19 N5 C23 120.6(3) . . ?
C19 N5 Fe1 120.0(2) . . ?
C23 N5 Fe1 118.8(2) . . ?
C28 N6 C24 117.9(3) . . ?
C28 N6 Fe1 127.9(2) . . ?
C24 N6 Fe1 114.2(2) . . ?
C59 N7 C37 107.1(2) . . ?
C59 N7 C31 112.6(2) . . ?
C37 N7 C31 107.8(2) . . ?
C59 N7 Fe2 114.67(19) . . ?
C37 N7 Fe2 106.60(18) . . ?
C31 N7 Fe2 107.69(18) . . ?
C38 N8 C42 120.5(3) . . ?
C38 N8 Fe2 119.9(2) . . ?
C42 N8 Fe2 119.1(2) . . ?
C47 N9 C43 117.3(3) . . ?
C47 N9 Fe2 128.0(2) . . ?
C43 N9 Fe2 114.7(2) . . ?
C60 N10 C48 108.6(3) . . ?
C60 N10 C36 113.1(3) . . ?
C48 N10 C36 107.0(3) . . ?
C60 N10 Fe2 115.1(2) . . ?
C48 N10 Fe2 105.98(18) . . ?
C36 N10 Fe2 106.57(18) . . ?
C49 N11 C53 121.4(3) . . ?
C49 N11 Fe2 119.7(2) . . ?
C53 N11 Fe2 118.8(2) . . ?
C58 N12 C54 117.2(3) . . ?
C58 N12 Fe2 128.3(2) . . ?
C54 N12 Fe2 114.29(19) . . ?
N5 Fe1 N2 175.05(10) . . ?
N5 Fe1 N6 81.44(10) . . ?
N2 Fe1 N6 96.08(10) . . ?
N5 Fe1 N3 94.77(10) . . ?
N2 Fe1 N3 81.13(10) . . ?
N6 Fe1 N3 94.90(10) . . ?
N5 Fe1 N4 81.62(10) . . ?
N2 Fe1 N4 101.21(10) . . ?
N6 Fe1 N4 162.23(10) . . ?
N3 Fe1 N4 91.82(10) . . ?
N5 Fe1 N1 103.18(10) . . ?
N2 Fe1 N1 81.18(10) . . ?
N6 Fe1 N1 93.26(10) . . ?
N3 Fe1 N1 161.19(10) . . ?
N4 Fe1 N1 85.41(10) . . ?
N8 Fe2 N11 175.66(11) . . ?
N8 Fe2 N9 81.11(10) . . ?
N11 Fe2 N9 97.61(11) . . ?
N8 Fe2 N12 95.03(10) . . ?
N11 Fe2 N12 80.92(10) . . ?
N9 Fe2 N12 94.57(10) . . ?
N8 Fe2 N7 81.49(10) . . ?
N11 Fe2 N7 100.11(10) . . ?
N9 Fe2 N7 161.85(10) . . ?
N12 Fe2 N7 92.05(10) . . ?
N8 Fe2 N10 102.72(10) . . ?
N11 Fe2 N10 81.47(10) . . ?
N9 Fe2 N10 93.57(10) . . ?
N12 Fe2 N10 161.42(10) . . ?
N7 Fe2 N10 85.26(10) . . ?
F4 B1 F2 109.8(3) . . ?
F4 B1 F1 110.0(3) . . ?
F2 B1 F1 109.6(3) . . ?
F4 B1 F3 109.5(3) . . ?
F2 B1 F3 109.6(3) . . ?
F1 B1 F3 108.2(3) . . ?
F8 B2 F7 111.1(3) . . ?
F8 B2 F6 110.0(3) . . ?
F7 B2 F6 109.7(3) . . ?
F8 B2 F5 108.4(3) . . ?
F7 B2 F5 107.5(3) . . ?
F6 B2 F5 110.1(3) . . ?
F9 B3 F10 112.1(4) . . ?
F9 B3 F12 111.5(4) . . ?
F10 B3 F12 111.0(4) . . ?
F9 B3 F11 107.9(4) . . ?
F10 B3 F11 104.9(3) . . ?
F12 B3 F11 109.3(3) . . ?
F15 B4 F13 107.7(4) . . ?
F15 B4 F16 110.6(3) . . ?
F13 B4 F16 108.8(3) . . ?
F15 B4 F14 109.8(3) . . ?
F13 B4 F14 108.7(3) . . ?
F16 B4 F14 111.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -49.3(4) . . . . ?
N1 C1 C2 C3 -177.3(3) . . . . ?
C1 C2 C3 C4 54.0(4) . . . . ?
C2 C3 C4 C5 -58.6(4) . . . . ?
C3 C4 C5 C6 58.5(4) . . . . ?
C2 C1 C6 N4 177.9(3) . . . . ?
N1 C1 C6 N4 -51.3(4) . . . . ?
C2 C1 C6 C5 49.9(4) . . . . ?
N1 C1 C6 C5 -179.3(3) . . . . ?
C4 C5 C6 C1 -54.2(4) . . . . ?
C4 C5 C6 N4 179.9(3) . . . . ?
N1 C7 C8 N2 -30.1(3) . . . . ?
N1 C7 C8 C9 152.9(3) . . . . ?
N2 C8 C9 C10 -1.9(5) . . . . ?
C7 C8 C9 C10 174.9(3) . . . . ?
C8 C9 C10 C11 -3.0(5) . . . . ?
C9 C10 C11 C12 4.0(5) . . . . ?
C10 C11 C12 N2 -0.3(5) . . . . ?
C10 C11 C12 C13 178.6(3) . . . . ?
N2 C12 C13 N3 1.2(4) . . . . ?
C11 C12 C13 N3 -177.8(3) . . . . ?
N2 C12 C13 C14 -179.7(3) . . . . ?
C11 C12 C13 C14 1.3(5) . . . . ?
N3 C13 C14 C15 3.1(5) . . . . ?
C12 C13 C14 C15 -176.0(3) . . . . ?
C13 C14 C15 C16 -0.6(5) . . . . ?
C14 C15 C16 C17 -2.5(5) . . . . ?
C15 C16 C17 N3 3.4(5) . . . . ?
N4 C18 C19 N5 -23.2(4) . . . . ?
N4 C18 C19 C20 165.4(3) . . . . ?
N5 C19 C20 C21 -1.5(5) . . . . ?
C18 C19 C20 C21 169.2(3) . . . . ?
C19 C20 C21 C22 -0.9(5) . . . . ?
C20 C21 C22 C23 1.6(5) . . . . ?
C21 C22 C23 N5 0.1(5) . . . . ?
C21 C22 C23 C24 -176.1(3) . . . . ?
N5 C23 C24 N6 -3.6(4) . . . . ?
C22 C23 C24 N6 172.9(3) . . . . ?
N5 C23 C24 C25 178.1(3) . . . . ?
C22 C23 C24 C25 -5.5(5) . . . . ?
N6 C24 C25 C26 0.2(5) . . . . ?
C23 C24 C25 C26 178.4(3) . . . . ?
C24 C25 C26 C27 0.7(5) . . . . ?
C25 C26 C27 C28 -1.3(5) . . . . ?
C26 C27 C28 N6 1.1(5) . . . . ?
C36 C31 C32 C33 55.5(4) . . . . ?
N7 C31 C32 C33 -179.9(3) . . . . ?
C31 C32 C33 C34 -58.2(4) . . . . ?
C32 C33 C34 C35 58.2(4) . . . . ?
C33 C34 C35 C36 -55.4(4) . . . . ?
N7 C31 C36 C35 -179.8(3) . . . . ?
C32 C31 C36 C35 -52.5(4) . . . . ?
N7 C31 C36 N10 52.0(4) . . . . ?
C32 C31 C36 N10 179.3(3) . . . . ?
C34 C35 C36 C31 52.6(4) . . . . ?
C34 C35 C36 N10 178.6(3) . . . . ?
N7 C37 C38 N8 25.5(4) . . . . ?
N7 C37 C38 C39 -163.1(3) . . . . ?
N8 C38 C39 C40 1.4(5) . . . . ?
C37 C38 C39 C40 -169.4(3) . . . . ?
C38 C39 C40 C41 1.0(5) . . . . ?
C39 C40 C41 C42 -1.8(5) . . . . ?
C40 C41 C42 N8 0.4(5) . . . . ?
C40 C41 C42 C43 175.3(3) . . . . ?
N8 C42 C43 N9 4.0(4) . . . . ?
C41 C42 C43 N9 -171.3(3) . . . . ?
N8 C42 C43 C44 -178.5(3) . . . . ?
C41 C42 C43 C44 6.2(5) . . . . ?
N9 C43 C44 C45 1.4(5) . . . . ?
C42 C43 C44 C45 -175.9(3) . . . . ?
C43 C44 C45 C46 -1.0(5) . . . . ?
C44 C45 C46 C47 0.4(5) . . . . ?
C45 C46 C47 N9 -0.1(5) . . . . ?
N10 C48 C49 N11 32.1(4) . . . . ?
N10 C48 C49 C50 -151.0(3) . . . . ?
N11 C49 C50 C51 1.5(5) . . . . ?
C48 C49 C50 C51 -175.2(3) . . . . ?
C49 C50 C51 C52 3.1(5) . . . . ?
C50 C51 C52 C53 -3.7(5) . . . . ?
C51 C52 C53 N11 -0.2(5) . . . . ?
C51 C52 C53 C54 -178.0(3) . . . . ?
N11 C53 C54 N12 -2.1(4) . . . . ?
C52 C53 C54 N12 175.9(3) . . . . ?
N11 C53 C54 C55 178.9(3) . . . . ?
C52 C53 C54 C55 -3.1(5) . . . . ?
N12 C54 C55 C56 -2.1(5) . . . . ?
C53 C54 C55 C56 176.9(3) . . . . ?
C54 C55 C56 C57 1.1(5) . . . . ?
C55 C56 C57 C58 0.7(5) . . . . ?
C56 C57 C58 N12 -1.8(5) . . . . ?
C8 C7 N1 C29 160.1(2) . . . . ?
C8 C7 N1 C1 -78.3(3) . . . . ?
C8 C7 N1 Fe1 35.7(3) . . . . ?
C6 C1 N1 C7 151.8(3) . . . . ?
C2 C1 N1 C7 -78.1(3) . . . . ?
C6 C1 N1 C29 -88.9(3) . . . . ?
C2 C1 N1 C29 41.1(4) . . . . ?
C6 C1 N1 Fe1 38.1(3) . . . . ?
C2 C1 N1 Fe1 168.2(2) . . . . ?
C9 C8 N2 C12 5.7(4) . . . . ?
C7 C8 N2 C12 -171.6(3) . . . . ?
C9 C8 N2 Fe1 -174.2(2) . . . . ?
C7 C8 N2 Fe1 8.6(3) . . . . ?
C11 C12 N2 C8 -4.6(4) . . . . ?
C13 C12 N2 C8 176.3(3) . . . . ?
C11 C12 N2 Fe1 175.2(2) . . . . ?
C13 C12 N2 Fe1 -3.8(3) . . . . ?
C16 C17 N3 C13 -1.0(4) . . . . ?
C16 C17 N3 Fe1 173.4(2) . . . . ?
C14 C13 N3 C17 -2.3(4) . . . . ?
C12 C13 N3 C17 176.8(3) . . . . ?
C14 C13 N3 Fe1 -177.5(2) . . . . ?
C12 C13 N3 Fe1 1.7(3) . . . . ?
C19 C18 N4 C30 155.5(3) . . . . ?
C19 C18 N4 C6 -84.0(3) . . . . ?
C19 C18 N4 Fe1 31.2(3) . . . . ?
C1 C6 N4 C18 153.0(3) . . . . ?
C5 C6 N4 C18 -79.9(3) . . . . ?
C1 C6 N4 C30 -88.3(3) . . . . ?
C5 C6 N4 C30 38.8(4) . . . . ?
C1 C6 N4 Fe1 37.7(3) . . . . ?
C5 C6 N4 Fe1 164.8(2) . . . . ?
C20 C19 N5 C23 3.2(4) . . . . ?
C18 C19 N5 C23 -168.7(3) . . . . ?
C20 C19 N5 Fe1 174.3(2) . . . . ?
C18 C19 N5 Fe1 2.4(3) . . . . ?
C22 C23 N5 C19 -2.5(4) . . . . ?
C24 C23 N5 C19 174.2(3) . . . . ?
C22 C23 N5 Fe1 -173.6(2) . . . . ?
C24 C23 N5 Fe1 3.1(3) . . . . ?
C27 C28 N6 C24 -0.3(4) . . . . ?
C27 C28 N6 Fe1 178.2(2) . . . . ?
C25 C24 N6 C28 -0.3(4) . . . . ?
C23 C24 N6 C28 -178.7(3) . . . . ?
C25 C24 N6 Fe1 -179.1(2) . . . . ?
C23 C24 N6 Fe1 2.6(3) . . . . ?
C38 C37 N7 C59 -156.9(3) . . . . ?
C38 C37 N7 C31 81.7(3) . . . . ?
C38 C37 N7 Fe2 -33.7(3) . . . . ?
C36 C31 N7 C59 88.1(3) . . . . ?
C32 C31 N7 C59 -37.2(4) . . . . ?
C36 C31 N7 C37 -153.9(3) . . . . ?
C32 C31 N7 C37 80.7(3) . . . . ?
C36 C31 N7 Fe2 -39.3(3) . . . . ?
C32 C31 N7 Fe2 -164.6(2) . . . . ?
C39 C38 N8 C42 -2.8(4) . . . . ?
C37 C38 N8 C42 169.1(3) . . . . ?
C39 C38 N8 Fe2 -175.0(2) . . . . ?
C37 C38 N8 Fe2 -3.1(3) . . . . ?
C41 C42 N8 C38 1.9(4) . . . . ?
C43 C42 N8 C38 -173.8(3) . . . . ?
C41 C42 N8 Fe2 174.2(2) . . . . ?
C43 C42 N8 Fe2 -1.5(3) . . . . ?
C46 C47 N9 C43 0.4(5) . . . . ?
C46 C47 N9 Fe2 -178.2(3) . . . . ?
C44 C43 N9 C47 -1.1(4) . . . . ?
C42 C43 N9 C47 176.5(3) . . . . ?
C44 C43 N9 Fe2 177.7(2) . . . . ?
C42 C43 N9 Fe2 -4.7(3) . . . . ?
C49 C48 N10 C60 -160.7(3) . . . . ?
C49 C48 N10 C36 76.9(3) . . . . ?
C49 C48 N10 Fe2 -36.6(3) . . . . ?
C31 C36 N10 C60 89.8(3) . . . . ?
C35 C36 N10 C60 -37.9(4) . . . . ?
C31 C36 N10 C48 -150.6(3) . . . . ?
C35 C36 N10 C48 81.6(3) . . . . ?
C31 C36 N10 Fe2 -37.6(3) . . . . ?
C35 C36 N10 Fe2 -165.3(2) . . . . ?
C50 C49 N11 C53 -5.5(5) . . . . ?
C48 C49 N11 C53 171.7(3) . . . . ?
C50 C49 N11 Fe2 172.0(2) . . . . ?
C48 C49 N11 Fe2 -10.8(4) . . . . ?
C52 C53 N11 C49 4.8(5) . . . . ?
C54 C53 N11 C49 -177.0(3) . . . . ?
C52 C53 N11 Fe2 -172.7(2) . . . . ?
C54 C53 N11 Fe2 5.5(3) . . . . ?
C57 C58 N12 C54 0.8(5) . . . . ?
C57 C58 N12 Fe2 -174.5(2) . . . . ?
C55 C54 N12 C58 1.1(4) . . . . ?
C53 C54 N12 C58 -177.9(3) . . . . ?
C55 C54 N12 Fe2 177.1(2) . . . . ?
C53 C54 N12 Fe2 -1.9(3) . . . . ?
C19 N5 Fe1 N6 -172.6(2) . . . . ?
C23 N5 Fe1 N6 -1.4(2) . . . . ?
C19 N5 Fe1 N3 -78.3(2) . . . . ?
C23 N5 Fe1 N3 92.8(2) . . . . ?
C19 N5 Fe1 N4 12.8(2) . . . . ?
C23 N5 Fe1 N4 -176.0(2) . . . . ?
C19 N5 Fe1 N1 96.0(2) . . . . ?
C23 N5 Fe1 N1 -92.8(2) . . . . ?
C8 N2 Fe1 N6 -82.3(2) . . . . ?
C12 N2 Fe1 N6 97.8(2) . . . . ?
C8 N2 Fe1 N3 -176.3(2) . . . . ?
C12 N2 Fe1 N3 3.8(2) . . . . ?
C8 N2 Fe1 N4 93.6(2) . . . . ?
C12 N2 Fe1 N4 -86.3(2) . . . . ?
C8 N2 Fe1 N1 10.1(2) . . . . ?
C12 N2 Fe1 N1 -169.8(2) . . . . ?
C38 N8 Fe2 N9 171.5(2) . . . . ?
C42 N8 Fe2 N9 -0.8(2) . . . . ?
C38 N8 Fe2 N12 77.7(2) . . . . ?
C42 N8 Fe2 N12 -94.6(2) . . . . ?
C38 N8 Fe2 N7 -13.6(2) . . . . ?
C42 N8 Fe2 N7 174.0(2) . . . . ?
C38 N8 Fe2 N10 -96.8(2) . . . . ?
C42 N8 Fe2 N10 90.9(2) . . . . ?
C49 N11 Fe2 N9 83.8(2) . . . . ?
C53 N11 Fe2 N9 -98.7(2) . . . . ?
C49 N11 Fe2 N12 177.2(2) . . . . ?
C53 N11 Fe2 N12 -5.2(2) . . . . ?
C49 N11 Fe2 N7 -92.3(2) . . . . ?
C53 N11 Fe2 N7 85.2(2) . . . . ?
C49 N11 Fe2 N10 -8.7(2) . . . . ?
C53 N11 Fe2 N10 168.8(2) . . . . ?

_refine_diff_density_max         0.693
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT112_shelx               
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.      c/2         92 %Fit  
RESPONSE: The search for an appropiate C centered unit cell together with
accompanied data integration gave non-reliable results only.
The selected crystal was twinned, whereby reflections belonging to the
major domain comprise ca. 82 % of all reflections, whith at least three
further domains with ca. 5 % each of all reflections. Trials to perform
a twin integration failed, as reflections were not separated well from each 
other.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          19 Note  
RESPONSE: ...
;
# end Validation Reply Form
