# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_LS_Fe5d
_database_code_depnum_ccdc_archive 'CCDC 1519517'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            LS-[Fe(5d)2](BF4)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H20 Br2 Fe N6, 2(BF4), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H26 B2 Br2 F8 Fe N8'
_chemical_formula_weight         983.96

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'
Br Br -0.2901 2.4595 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8218(4)
_cell_length_b                   11.8771(6)
_cell_length_c                   14.6612(7)
_cell_angle_alpha                92.953(4)
_cell_angle_beta                 97.763(3)
_cell_angle_gamma                114.772(4)
_cell_volume                     1838.58(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    110
_cell_measurement_reflns_used    6674
_cell_measurement_theta_min      3.5720
_cell_measurement_theta_max      28.1900

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.668
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.77095
_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_standards_number         1
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12559
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.239
_diffrn_reflns_theta_max         24.999
_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             6431
_reflns_number_gt                5596
_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 1.171.36.28 (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)+(0.0420P)²+0.8853P] 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         6431
_refine_ls_number_parameters     545
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0826
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5691(3) 0.5189(3) 0.78549(19) 0.0180(6) Uani 1 1 d . . . . .
H1 H 0.6284 0.5302 0.7469 0.022 Uiso 1 1 calc R U . . .
C2 C 0.5593(3) 0.6232(3) 0.8243(2) 0.0199(6) Uani 1 1 d . . . . .
H2 H 0.6114 0.7023 0.8111 0.024 Uiso 1 1 calc R U . . .
C3 C 0.4742(3) 0.6104(3) 0.8816(2) 0.0222(7) Uani 1 1 d . . . . .
H3 H 0.4671 0.6803 0.9065 0.027 Uiso 1 1 calc R U . . .
C4 C 0.3969(3) 0.4909(3) 0.9029(2) 0.0197(6) Uani 1 1 d . . . . .
C5 C 0.4144(2) 0.3916(3) 0.86230(19) 0.0159(6) Uani 1 1 d . . . . .
C6 C 0.3060(3) 0.4621(3) 0.9635(2) 0.0218(7) Uani 1 1 d . . . . .
H6 H 0.2928 0.5267 0.9912 0.026 Uiso 1 1 calc R U . . .
C7 C 0.2383(3) 0.3437(3) 0.9822(2) 0.0236(7) Uani 1 1 d . . . . .
H7 H 0.1802 0.3292 1.0222 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2549(3) 0.2414(3) 0.9413(2) 0.0195(6) Uani 1 1 d . . . . .
C9 C 0.3436(2) 0.2692(3) 0.88178(19) 0.0154(6) Uani 1 1 d . . . . .
C10 C 0.1914(3) 0.1145(3) 0.9536(2) 0.0242(7) Uani 1 1 d . . . . .
H10 H 0.1331 0.0906 0.9938 0.029 Uiso 1 1 calc R U . . .
C11 C 0.2151(3) 0.0262(3) 0.9067(2) 0.0223(7) Uani 1 1 d . . . . .
H11 H 0.1717 -0.0575 0.9145 0.027 Uiso 1 1 calc R U . . .
C12 C 0.3043(2) 0.0610(3) 0.8470(2) 0.0179(6) Uani 1 1 d . . . . .
C13 C 0.3425(3) -0.0165(3) 0.7908(2) 0.0191(6) Uani 1 1 d . . . . .
C14 C 0.2950(3) -0.1442(3) 0.7908(2) 0.0233(7) Uani 1 1 d . . . . .
H14 H 0.2316 -0.1854 0.8246 0.028 Uiso 1 1 calc R U . . .
C15 C 0.3425(3) -0.2104(3) 0.7401(2) 0.0268(7) Uani 1 1 d . . . . .
H15 H 0.3130 -0.2963 0.7403 0.032 Uiso 1 1 calc R U . . .
C16 C 0.4339(3) -0.1470(3) 0.6897(2) 0.0270(7) Uani 1 1 d . . . . .
H16 H 0.4679 -0.1893 0.6554 0.032 Uiso 1 1 calc R U . . .
C17 C 0.4753(3) -0.0191(3) 0.6903(2) 0.0211(7) Uani 1 1 d . . . . .
C18 C 0.2139(3) 0.1561(3) 0.6456(2) 0.0199(6) Uani 1 1 d . . . . .
H18 H 0.1812 0.1221 0.6972 0.024 Uiso 1 1 calc R U . . .
C19 C 0.1294(3) 0.1481(3) 0.5658(2) 0.0224(7) Uani 1 1 d . . . . .
H19 H 0.0427 0.1098 0.5655 0.027 Uiso 1 1 calc R U . . .
C20 C 0.1743(3) 0.1968(3) 0.4884(2) 0.0217(7) Uani 1 1 d . . . . .
H20 H 0.1185 0.1909 0.4352 0.026 Uiso 1 1 calc R U . . .
C21 C 0.3054(3) 0.2555(3) 0.4903(2) 0.0175(6) Uani 1 1 d . . . . .
C22 C 0.3823(2) 0.2581(3) 0.57263(19) 0.0151(6) Uani 1 1 d . . . . .
C23 C 0.3672(3) 0.3147(3) 0.4163(2) 0.0201(6) Uani 1 1 d . . . . .
H23 H 0.3181 0.3142 0.3610 0.024 Uiso 1 1 calc R U . . .
C24 C 0.4947(3) 0.3711(3) 0.4248(2) 0.0208(6) Uani 1 1 d . . . . .
H24 H 0.5309 0.4098 0.3757 0.025 Uiso 1 1 calc R U . . .
C25 C 0.5750(3) 0.3726(3) 0.5077(2) 0.0175(6) Uani 1 1 d . . . . .
C26 C 0.5150(2) 0.3137(3) 0.57895(19) 0.0148(6) Uani 1 1 d . . . . .
C27 C 0.7081(3) 0.4261(3) 0.5248(2) 0.0198(6) Uani 1 1 d . . . . .
H27 H 0.7528 0.4657 0.4793 0.024 Uiso 1 1 calc R U . . .
C28 C 0.7720(3) 0.4202(3) 0.6084(2) 0.0192(6) Uani 1 1 d . . . . .
H28 H 0.8599 0.4550 0.6194 0.023 Uiso 1 1 calc R U . . .
C29 C 0.7046(2) 0.3614(3) 0.6774(2) 0.0168(6) Uani 1 1 d . . . . .
C30 C 0.7546(2) 0.3471(3) 0.7704(2) 0.0167(6) Uani 1 1 d . . . . .
C31 C 0.8827(3) 0.3965(3) 0.8051(2) 0.0217(7) Uani 1 1 d . . . . .
H31 H 0.9415 0.4439 0.7700 0.026 Uiso 1 1 calc R U . . .
C32 C 0.9221(3) 0.3744(3) 0.8925(2) 0.0258(7) Uani 1 1 d . . . . .
H32 H 1.0078 0.4080 0.9173 0.031 Uiso 1 1 calc R U . . .
C33 C 0.8337(3) 0.3026(3) 0.9424(2) 0.0228(7) Uani 1 1 d . . . . .
H33 H 0.8579 0.2846 1.0008 0.027 Uiso 1 1 calc R U . . .
C34 C 0.7063(3) 0.2572(3) 0.9030(2) 0.0184(6) Uani 1 1 d . . . . .
C35 C 0.7826(4) 0.0079(3) 0.8087(3) 0.0415(9) Uani 1 1 d . . . . .
C36 C 0.8866(4) 0.0546(4) 0.7575(4) 0.0636(14) Uani 1 1 d . . . . .
H36A H 0.9397 0.0126 0.7710 0.095 Uiso 1 1 calc R U . . .
H36B H 0.9351 0.1428 0.7755 0.095 Uiso 1 1 calc R U . . .
H36C H 0.8538 0.0395 0.6923 0.095 Uiso 1 1 calc R U . . .
N1 N 0.4958(2) 0.4025(2) 0.80176(16) 0.0140(5) Uani 1 1 d . . . . .
N2 N 0.3693(2) 0.1821(2) 0.83812(16) 0.0154(5) Uani 1 1 d . . . . .
N3 N 0.4332(2) 0.0482(2) 0.73900(16) 0.0166(5) Uani 1 1 d . . . . .
N4 N 0.3386(2) 0.2100(2) 0.65048(16) 0.0148(5) Uani 1 1 d . . . . .
N5 N 0.57820(19) 0.3072(2) 0.66102(16) 0.0138(5) Uani 1 1 d . . . . .
N6 N 0.6635(2) 0.2796(2) 0.82067(16) 0.0150(5) Uani 1 1 d . . . . .
N8 N 0.6994(3) -0.0312(3) 0.8469(2) 0.0464(8) Uani 1 1 d . . . . .
F1 F 0.11916(18) 0.31656(17) 0.74631(14) 0.0355(5) Uani 1 1 d . . . . .
F2 F 0.16776(16) 0.51980(16) 0.78110(13) 0.0304(4) Uani 1 1 d . . . . .
F3 F 0.06555(17) 0.4229(2) 0.63745(14) 0.0428(5) Uani 1 1 d . . . . .
F4 F 0.27064(15) 0.46192(18) 0.68146(12) 0.0320(4) Uani 1 1 d . . . . .
F5 F 0.98870(16) 0.15844(17) 0.25830(12) 0.0298(4) Uani 1 1 d . U . . .
F6 F 1.1218(2) 0.1899(2) 0.15614(18) 0.0652(8) Uani 1 1 d . U . . .
F7 F 1.14961(18) 0.34842(19) 0.26050(15) 0.0486(6) Uani 1 1 d . U . . .
F8 F 0.98594(17) 0.27744(18) 0.14194(14) 0.0419(5) Uani 1 1 d . U . . .
Fe1 Fe 0.48166(3) 0.23591(4) 0.75282(3) 0.01189(10) Uani 1 1 d . . . . .
Br1 Br 0.59921(3) 0.05681(3) 0.61712(2) 0.02486(10) Uani 1 1 d . . . . .
Br2 Br 0.58888(3) 0.15603(3) 0.97369(2) 0.02054(9) Uani 1 1 d . . . . .
B1 B 0.1559(3) 0.4297(3) 0.7115(2) 0.0218(8) Uani 1 1 d . . . . .
B2 B 1.0616(3) 0.2432(3) 0.2038(3) 0.0248(8) Uani 1 1 d . U . . .
C37 C 0.8534(3) 0.1933(4) 0.4580(2) 0.0331(8) Uani 1 1 d . . . . .
C38 C 0.9304(4) 0.3112(4) 0.4286(3) 0.0327(8) Uani 1 1 d . . . . .
N9 N 0.7936(3) 0.0994(3) 0.4815(3) 0.0508(9) Uani 1 1 d . . . . .
8CII H 0.991(4) 0.361(4) 0.478(3) 0.051(12) Uiso 1 1 d . . . . .
8AII H 0.963(3) 0.300(4) 0.379(3) 0.048(12) Uiso 1 1 d . . . . .
8BII H 0.877(4) 0.351(4) 0.411(3) 0.057(12) 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 1.343(4) . ?
C1 C2 1.392(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.408(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(4) . ?
C4 C6 1.429(4) . ?
C5 N1 1.367(3) . ?
C5 C9 1.408(4) . ?
C6 C7 1.361(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.425(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(4) . ?
C8 C10 1.408(4) . ?
C9 N2 1.350(4) . ?
C10 C11 1.370(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.404(4) . ?
C11 H11 0.9300 . ?
C12 N2 1.340(4) . ?
C12 C13 1.449(4) . ?
C13 C14 1.380(4) . ?
C13 N3 1.381(4) . ?
C14 C15 1.381(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.368(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.386(4) . ?
C16 H16 0.9300 . ?
C17 N3 1.329(4) . ?
C17 Br1 1.879(3) . ?
C18 N4 1.329(3) . ?
C18 C19 1.403(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.370(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.404(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.401(4) . ?
C21 C23 1.437(4) . ?
C22 N4 1.369(3) . ?
C22 C26 1.411(4) . ?
C23 C24 1.353(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.432(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.394(4) . ?
C25 C27 1.407(4) . ?
C26 N5 1.352(3) . ?
C27 C28 1.372(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.403(4) . ?
C28 H28 0.9300 . ?
C29 N5 1.336(3) . ?
C29 C30 1.459(4) . ?
C30 N6 1.378(3) . ?
C30 C31 1.383(4) . ?
C31 C32 1.378(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.372(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.394(4) . ?
C33 H33 0.9300 . ?
C34 N6 1.329(4) . ?
C34 Br2 1.888(3) . ?
C35 N8 1.135(5) . ?
C35 C36 1.450(6) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 Fe1 2.001(2) . ?
N2 Fe1 1.886(2) . ?
N3 Fe1 2.047(2) . ?
N4 Fe1 2.009(2) . ?
N5 Fe1 1.885(2) . ?
N6 Fe1 2.077(2) . ?
F1 B1 1.377(4) . ?
F2 B1 1.389(4) . ?
F3 B1 1.390(4) . ?
F4 B1 1.387(4) . ?
F5 B2 1.392(4) . ?
F6 B2 1.365(4) . ?
F7 B2 1.380(4) . ?
F8 B2 1.382(4) . ?
C37 N9 1.143(5) . ?
C37 C38 1.440(5) . ?
C38 8CII 0.92(4) . ?
C38 8AII 0.90(4) . ?
C38 8BII 0.95(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.3(3) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 119.7(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 116.1(3) . . ?
C5 C4 C6 117.3(3) . . ?
C3 C4 C6 126.6(3) . . ?
N1 C5 C4 124.8(3) . . ?
N1 C5 C9 115.3(2) . . ?
C4 C5 C9 119.9(3) . . ?
C7 C6 C4 122.5(3) . . ?
C7 C6 H6 118.8 . . ?
C4 C6 H6 118.8 . . ?
C6 C7 C8 120.9(3) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C10 116.0(3) . . ?
C9 C8 C7 116.8(3) . . ?
C10 C8 C7 127.3(3) . . ?
N2 C9 C8 123.4(3) . . ?
N2 C9 C5 114.0(2) . . ?
C8 C9 C5 122.6(3) . . ?
C11 C10 C8 120.3(3) . . ?
C11 C10 H10 119.9 . . ?
C8 C10 H10 119.9 . . ?
C10 C11 C12 120.6(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
N2 C12 C11 119.5(3) . . ?
N2 C12 C13 111.0(2) . . ?
C11 C12 C13 129.5(3) . . ?
C14 C13 N3 122.4(3) . . ?
C14 C13 C12 122.9(3) . . ?
N3 C13 C12 114.6(2) . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 118.6(3) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
N3 C17 C16 123.9(3) . . ?
N3 C17 Br1 120.8(2) . . ?
C16 C17 Br1 115.3(2) . . ?
N4 C18 C19 122.8(3) . . ?
N4 C18 H18 118.6 . . ?
C19 C18 H18 118.6 . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 119.2(3) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C22 C21 C20 116.6(3) . . ?
C22 C21 C23 117.5(2) . . ?
C20 C21 C23 126.0(3) . . ?
N4 C22 C21 124.7(2) . . ?
N4 C22 C26 115.6(2) . . ?
C21 C22 C26 119.7(2) . . ?
C24 C23 C21 122.0(3) . . ?
C24 C23 H23 119.0 . . ?
C21 C23 H23 119.0 . . ?
C23 C24 C25 121.5(3) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C26 C25 C27 116.4(3) . . ?
C26 C25 C24 116.6(2) . . ?
C27 C25 C24 127.1(3) . . ?
N5 C26 C25 123.3(2) . . ?
N5 C26 C22 113.9(2) . . ?
C25 C26 C22 122.8(3) . . ?
C28 C27 C25 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C25 C27 H27 119.9 . . ?
C27 C28 C29 119.9(3) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
N5 C29 C28 120.4(3) . . ?
N5 C29 C30 111.4(2) . . ?
C28 C29 C30 128.2(2) . . ?
N6 C30 C31 122.7(3) . . ?
N6 C30 C29 114.4(2) . . ?
C31 C30 C29 122.9(3) . . ?
C32 C31 C30 119.2(3) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
C33 C32 C31 119.4(3) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 118.0(3) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
N6 C34 C33 124.9(3) . . ?
N6 C34 Br2 118.9(2) . . ?
C33 C34 Br2 116.2(2) . . ?
N8 C35 C36 178.1(4) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C1 N1 C5 116.5(2) . . ?
C1 N1 Fe1 131.74(19) . . ?
C5 N1 Fe1 111.74(18) . . ?
C12 N2 C9 120.2(2) . . ?
C12 N2 Fe1 122.2(2) . . ?
C9 N2 Fe1 117.04(18) . . ?
C17 N3 C13 116.3(2) . . ?
C17 N3 Fe1 131.0(2) . . ?
C13 N3 Fe1 112.78(18) . . ?
C18 N4 C22 116.5(2) . . ?
C18 N4 Fe1 132.1(2) . . ?
C22 N4 Fe1 111.40(17) . . ?
C29 N5 C26 119.7(2) . . ?
C29 N5 Fe1 122.64(19) . . ?
C26 N5 Fe1 117.28(17) . . ?
C34 N6 C30 115.7(2) . . ?
C34 N6 Fe1 131.91(19) . . ?
C30 N6 Fe1 112.38(18) . . ?
N5 Fe1 N2 169.61(10) . . ?
N5 Fe1 N1 91.20(9) . . ?
N2 Fe1 N1 81.59(10) . . ?
N5 Fe1 N4 81.74(9) . . ?
N2 Fe1 N4 91.07(9) . . ?
N1 Fe1 N4 92.59(9) . . ?
N5 Fe1 N3 108.39(9) . . ?
N2 Fe1 N3 79.01(10) . . ?
N1 Fe1 N3 160.41(9) . . ?
N4 Fe1 N3 90.47(9) . . ?
N5 Fe1 N6 78.61(9) . . ?
N2 Fe1 N6 108.82(9) . . ?
N1 Fe1 N6 90.96(9) . . ?
N4 Fe1 N6 160.10(9) . . ?
N3 Fe1 N6 92.71(9) . . ?
F1 B1 F4 110.1(3) . . ?
F1 B1 F2 108.6(3) . . ?
F4 B1 F2 109.9(2) . . ?
F1 B1 F3 110.2(3) . . ?
F4 B1 F3 109.1(3) . . ?
F2 B1 F3 109.0(3) . . ?
F6 B2 F7 109.8(3) . . ?
F6 B2 F8 109.5(3) . . ?
F7 B2 F8 108.9(3) . . ?
F6 B2 F5 109.4(3) . . ?
F7 B2 F5 109.0(3) . . ?
F8 B2 F5 110.3(3) . . ?
N9 C37 C38 179.1(4) . . ?
C37 C38 8CII 109(2) . . ?
C37 C38 8AII 111(3) . . ?
8CII C38 8AII 113(3) . . ?
C37 C38 8BII 108(2) . . ?
8CII C38 8BII 107(4) . . ?
8AII C38 8BII 108(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.4(4) . . . . ?
C1 C2 C3 C4 1.1(4) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C2 C3 C4 C6 178.0(3) . . . . ?
C3 C4 C5 N1 -2.9(4) . . . . ?
C6 C4 C5 N1 178.9(2) . . . . ?
C3 C4 C5 C9 178.3(2) . . . . ?
C6 C4 C5 C9 0.1(4) . . . . ?
C5 C4 C6 C7 0.1(4) . . . . ?
C3 C4 C6 C7 -177.9(3) . . . . ?
C4 C6 C7 C8 -0.1(4) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C6 C7 C8 C10 -179.6(3) . . . . ?
C10 C8 C9 N2 -0.3(4) . . . . ?
C7 C8 C9 N2 -179.9(3) . . . . ?
C10 C8 C9 C5 179.8(3) . . . . ?
C7 C8 C9 C5 0.2(4) . . . . ?
N1 C5 C9 N2 0.9(3) . . . . ?
C4 C5 C9 N2 179.9(2) . . . . ?
N1 C5 C9 C8 -179.2(2) . . . . ?
C4 C5 C9 C8 -0.3(4) . . . . ?
C9 C8 C10 C11 -1.8(4) . . . . ?
C7 C8 C10 C11 177.8(3) . . . . ?
C8 C10 C11 C12 1.0(4) . . . . ?
C10 C11 C12 N2 2.0(4) . . . . ?
C10 C11 C12 C13 -179.4(3) . . . . ?
N2 C12 C13 C14 176.6(3) . . . . ?
C11 C12 C13 C14 -2.1(5) . . . . ?
N2 C12 C13 N3 -1.6(3) . . . . ?
C11 C12 C13 N3 179.7(3) . . . . ?
N3 C13 C14 C15 2.5(4) . . . . ?
C12 C13 C14 C15 -175.6(3) . . . . ?
C13 C14 C15 C16 -1.4(4) . . . . ?
C14 C15 C16 C17 -0.5(4) . . . . ?
C15 C16 C17 N3 1.4(5) . . . . ?
C15 C16 C17 Br1 -179.2(2) . . . . ?
N4 C18 C19 C20 0.2(5) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
C19 C20 C21 C22 1.1(4) . . . . ?
C19 C20 C21 C23 -177.7(3) . . . . ?
C20 C21 C22 N4 -1.3(4) . . . . ?
C23 C21 C22 N4 177.6(3) . . . . ?
C20 C21 C22 C26 178.9(3) . . . . ?
C23 C21 C22 C26 -2.2(4) . . . . ?
C22 C21 C23 C24 0.1(4) . . . . ?
C20 C21 C23 C24 178.8(3) . . . . ?
C21 C23 C24 C25 1.3(4) . . . . ?
C23 C24 C25 C26 -0.4(4) . . . . ?
C23 C24 C25 C27 179.1(3) . . . . ?
C27 C25 C26 N5 0.3(4) . . . . ?
C24 C25 C26 N5 179.8(3) . . . . ?
C27 C25 C26 C22 178.7(3) . . . . ?
C24 C25 C26 C22 -1.8(4) . . . . ?
N4 C22 C26 N5 1.9(4) . . . . ?
C21 C22 C26 N5 -178.3(2) . . . . ?
N4 C22 C26 C25 -176.6(2) . . . . ?
C21 C22 C26 C25 3.2(4) . . . . ?
C26 C25 C27 C28 -0.8(4) . . . . ?
C24 C25 C27 C28 179.8(3) . . . . ?
C25 C27 C28 C29 -0.5(4) . . . . ?
C27 C28 C29 N5 2.4(4) . . . . ?
C27 C28 C29 C30 -179.0(3) . . . . ?
N5 C29 C30 N6 1.4(3) . . . . ?
C28 C29 C30 N6 -177.3(3) . . . . ?
N5 C29 C30 C31 -178.9(3) . . . . ?
C28 C29 C30 C31 2.4(5) . . . . ?
N6 C30 C31 C32 2.2(4) . . . . ?
C29 C30 C31 C32 -177.5(3) . . . . ?
C30 C31 C32 C33 1.0(5) . . . . ?
C31 C32 C33 C34 -1.6(5) . . . . ?
C32 C33 C34 N6 -0.9(5) . . . . ?
C32 C33 C34 Br2 178.8(2) . . . . ?
C2 C1 N1 C5 -3.0(4) . . . . ?
C2 C1 N1 Fe1 176.9(2) . . . . ?
C4 C5 N1 C1 4.3(4) . . . . ?
C9 C5 N1 C1 -176.8(2) . . . . ?
C4 C5 N1 Fe1 -175.6(2) . . . . ?
C9 C5 N1 Fe1 3.3(3) . . . . ?
C11 C12 N2 C9 -4.1(4) . . . . ?
C13 C12 N2 C9 177.0(2) . . . . ?
C11 C12 N2 Fe1 -175.28(19) . . . . ?
C13 C12 N2 Fe1 5.9(3) . . . . ?
C8 C9 N2 C12 3.3(4) . . . . ?
C5 C9 N2 C12 -176.8(2) . . . . ?
C8 C9 N2 Fe1 175.0(2) . . . . ?
C5 C9 N2 Fe1 -5.2(3) . . . . ?
C16 C17 N3 C13 -0.4(4) . . . . ?
Br1 C17 N3 C13 -179.76(19) . . . . ?
C16 C17 N3 Fe1 178.7(2) . . . . ?
Br1 C17 N3 Fe1 -0.7(4) . . . . ?
C14 C13 N3 C17 -1.6(4) . . . . ?
C12 C13 N3 C17 176.6(2) . . . . ?
C14 C13 N3 Fe1 179.2(2) . . . . ?
C12 C13 N3 Fe1 -2.6(3) . . . . ?
C19 C18 N4 C22 -0.3(4) . . . . ?
C19 C18 N4 Fe1 179.9(2) . . . . ?
C21 C22 N4 C18 0.9(4) . . . . ?
C26 C22 N4 C18 -179.3(2) . . . . ?
C21 C22 N4 Fe1 -179.3(2) . . . . ?
C26 C22 N4 Fe1 0.5(3) . . . . ?
C28 C29 N5 C26 -2.8(4) . . . . ?
C30 C29 N5 C26 178.3(2) . . . . ?
C28 C29 N5 Fe1 -175.9(2) . . . . ?
C30 C29 N5 Fe1 5.3(3) . . . . ?
C25 C26 N5 C29 1.5(4) . . . . ?
C22 C26 N5 C29 -177.0(2) . . . . ?
C25 C26 N5 Fe1 174.9(2) . . . . ?
C22 C26 N5 Fe1 -3.6(3) . . . . ?
C33 C34 N6 C30 3.8(4) . . . . ?
Br2 C34 N6 C30 -175.80(19) . . . . ?
C33 C34 N6 Fe1 -174.2(2) . . . . ?
Br2 C34 N6 Fe1 6.2(4) . . . . ?
C31 C30 N6 C34 -4.5(4) . . . . ?
C29 C30 N6 C34 175.3(2) . . . . ?
C31 C30 N6 Fe1 173.9(2) . . . . ?
C29 C30 N6 Fe1 -6.4(3) . . . . ?
C29 N5 Fe1 N2 129.6(5) . . . . ?
C26 N5 Fe1 N2 -43.6(6) . . . . ?
C29 N5 Fe1 N1 83.8(2) . . . . ?
C26 N5 Fe1 N1 -89.4(2) . . . . ?
C29 N5 Fe1 N4 176.2(2) . . . . ?
C26 N5 Fe1 N4 3.03(19) . . . . ?
C29 N5 Fe1 N3 -96.0(2) . . . . ?
C26 N5 Fe1 N3 90.8(2) . . . . ?
C29 N5 Fe1 N6 -7.0(2) . . . . ?
C26 N5 Fe1 N6 179.9(2) . . . . ?
C12 N2 Fe1 N5 130.5(5) . . . . ?
C9 N2 Fe1 N5 -41.0(6) . . . . ?
C12 N2 Fe1 N1 176.9(2) . . . . ?
C9 N2 Fe1 N1 5.49(19) . . . . ?
C12 N2 Fe1 N4 84.5(2) . . . . ?
C9 N2 Fe1 N4 -87.0(2) . . . . ?
C12 N2 Fe1 N3 -5.8(2) . . . . ?
C9 N2 Fe1 N3 -177.3(2) . . . . ?
C12 N2 Fe1 N6 -94.9(2) . . . . ?
C9 N2 Fe1 N6 93.6(2) . . . . ?

_refine_diff_density_max         0.838
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.078

_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_Fe_5e
_database_code_depnum_ccdc_archive 'CCDC 1519519'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(5e)2](BF4)2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H26 Fe N10, 2(B F4), 3(C2 H3 N)'
_chemical_formula_sum            'C46 H35 B2 F8 Fe N13'
_chemical_formula_weight         999.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5860(5)
_cell_length_b                   12.6635(4)
_cell_length_c                   14.9829(5)
_cell_angle_alpha                96.447(3)
_cell_angle_beta                 100.639(3)
_cell_angle_gamma                110.225(4)
_cell_volume                     2161.73(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    109.8(3)
_cell_measurement_reflns_used    6084
_cell_measurement_theta_min      3.0200
_cell_measurement_theta_max      28.3400


_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             1020
_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    0.437
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.86187
_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            15107
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.921
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7558
_reflns_number_gt                6070
_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 1.171.36.28 (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)+(0.0700P)²+7.9584P] 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         7558
_refine_ls_number_parameters     632
_refine_ls_number_restraints     148
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.070
_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 0.2670(5) 0.1713(4) 0.6002(3) 0.0309(11) Uani 1 1 d . . . . .
H1 H 0.2367 0.1330 0.6447 0.037 Uiso 1 1 calc R U . . .
C1N C 0.0018(6) 0.0813(6) 0.6878(4) 0.0541(16) Uani 1 1 d . . . . .
C2 C 0.1870(5) 0.1638(5) 0.5175(4) 0.0398(13) Uani 1 1 d . . . . .
H2 H 0.1077 0.1215 0.5084 0.048 Uiso 1 1 calc R U . . .
C2N C -0.0011(7) 0.1910(6) 0.7082(5) 0.072(2) Uani 1 1 d . . . . .
H2N1 H 0.0067 0.2113 0.7735 0.107 Uiso 1 1 calc R U . . .
H2N2 H -0.0739 0.1911 0.6749 0.107 Uiso 1 1 calc R U . . .
H2N3 H 0.0620 0.2456 0.6903 0.107 Uiso 1 1 calc R U . . .
C3 C 0.2285(4) 0.2193(4) 0.4523(3) 0.0339(12) Uani 1 1 d . . . . .
H3 H 0.1783 0.2166 0.3974 0.041 Uiso 1 1 calc R U . . .
C3N C -0.2832(7) -0.0356(5) 0.8691(5) 0.0551(17) Uani 1 1 d . . . . .
C4 C 0.3515(4) 0.2826(4) 0.4691(3) 0.0319(11) Uani 1 1 d . . . . .
C4N C -0.1615(8) 0.0152(8) 0.8676(9) 0.112(4) Uani 1 1 d . . . . .
H4N1 H -0.1537 0.0604 0.8201 0.168 Uiso 1 1 calc R U . . .
H4N2 H -0.1324 -0.0444 0.8552 0.168 Uiso 1 1 calc R U . . .
H4N3 H -0.1176 0.0632 0.9265 0.168 Uiso 1 1 calc R U . . .
C5 C 0.4216(4) 0.2843(4) 0.5515(3) 0.0292(11) Uani 1 1 d . . . . .
C5N C -0.0941(5) 0.2128(6) 0.4682(4) 0.0513(16) Uani 1 1 d . . . . .
C6 C 0.4040(5) 0.3413(4) 0.4038(4) 0.0352(12) Uani 1 1 d . . . . .
H6 H 0.3564 0.3421 0.3486 0.042 Uiso 1 1 calc R U . . .
C6N C -0.0160(5) 0.3040(6) 0.4345(4) 0.0545(17) Uani 1 1 d . . . . .
H6N1 H 0.0555 0.3424 0.4811 0.082 Uiso 1 1 calc R U . . .
H6N2 H -0.0518 0.3578 0.4203 0.082 Uiso 1 1 calc R U . . .
H6N3 H 0.0003 0.2725 0.3796 0.082 Uiso 1 1 calc R U . . .
C7 C 0.5218(5) 0.3968(4) 0.4190(3) 0.0316(11) Uani 1 1 d . . . . .
H7 H 0.5531 0.4345 0.3746 0.038 Uiso 1 1 calc R U . . .
C8 C 0.5967(5) 0.3972(4) 0.5024(3) 0.0326(11) Uani 1 1 d . . . . .
C9 C 0.5447(5) 0.3404(4) 0.5708(3) 0.0300(11) Uani 1 1 d . . . . .
C10 C 0.7165(5) 0.4479(5) 0.5223(4) 0.0395(13) Uani 1 1 d . . . . .
H10 H 0.7530 0.4849 0.4797 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7830(5) 0.4439(5) 0.6057(4) 0.0383(13) Uani 1 1 d . . . . .
H11 H 0.8640 0.4776 0.6200 0.046 Uiso 1 1 calc R U . . .
C12 C 0.7248(4) 0.3882(4) 0.6672(3) 0.0228(10) Uani 1 1 d . . . . .
C13 C 0.7890(4) 0.3781(4) 0.7594(3) 0.0299(11) Uani 1 1 d . . . . .
C14 C 0.9086(5) 0.4237(4) 0.7898(4) 0.0362(12) Uani 1 1 d . . . . .
H14 H 0.9547 0.4652 0.7541 0.043 Uiso 1 1 calc R U . . .
C15 C 0.9596(4) 0.4066(4) 0.8751(4) 0.0331(12) Uani 1 1 d . . . . .
H15 H 1.0404 0.4366 0.8960 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8936(4) 0.3473(4) 0.9276(4) 0.0360(12) Uani 1 1 d . . . . .
H16 H 0.9263 0.3356 0.9847 0.043 Uiso 1 1 calc R U . . .
C17 C 0.7696(4) 0.3033(4) 0.8898(3) 0.0291(11) Uani 1 1 d . . . . .
C18 C 0.7176(5) 0.2150(4) 1.0235(3) 0.0326(12) Uani 1 1 d . . . . .
H18 H 0.7905 0.2359 1.0636 0.039 Uiso 1 1 calc R U . . .
C19 C 0.6115(4) 0.1528(4) 1.0383(4) 0.0346(12) Uani 1 1 d . . . . .
H19 H 0.5977 0.1220 1.0904 0.041 Uiso 1 1 calc R U . . .
C20 C 0.5285(5) 0.1449(4) 0.9597(3) 0.0336(12) Uani 1 1 d . . . . .
H20 H 0.4486 0.1075 0.9518 0.040 Uiso 1 1 calc R U . . .
C21 C 0.6018(4) 0.5215(4) 0.8007(3) 0.0266(10) Uani 1 1 d . . . . .
H21 H 0.6590 0.5198 0.7699 0.032 Uiso 1 1 calc R U . . .
C22 C 0.6029(4) 0.6284(4) 0.8367(3) 0.0283(11) Uani 1 1 d . . . . .
H22 H 0.6591 0.6953 0.8293 0.034 Uiso 1 1 calc R U . . .
C23 C 0.5214(4) 0.6339(4) 0.8824(3) 0.0256(10) Uani 1 1 d . . . . .
H23 H 0.5197 0.7044 0.9055 0.031 Uiso 1 1 calc R U . . .
C24 C 0.4397(4) 0.5325(4) 0.8946(3) 0.0250(10) Uani 1 1 d . . . . .
C25 C 0.4427(4) 0.4288(4) 0.8540(3) 0.0226(10) Uani 1 1 d . . . . .
C26 C 0.3564(4) 0.5302(4) 0.9491(3) 0.0271(10) Uani 1 1 d . . . . .
H26 H 0.3548 0.5991 0.9765 0.033 Uiso 1 1 calc R U . . .
C27 C 0.2803(4) 0.4306(4) 0.9614(3) 0.0268(10) Uani 1 1 d . . . . .
H27 H 0.2295 0.4319 0.9989 0.032 Uiso 1 1 calc R U . . .
C28 C 0.2774(4) 0.3239(4) 0.9175(3) 0.0241(10) Uani 1 1 d . . . . .
C29 C 0.3582(4) 0.3223(4) 0.8625(3) 0.0201(9) Uani 1 1 d . . . . .
C30 C 0.1997(4) 0.2180(4) 0.9251(3) 0.0274(10) Uani 1 1 d . . . . .
H30 H 0.1460 0.2148 0.9608 0.033 Uiso 1 1 calc R U . . .
C31 C 0.2015(4) 0.1185(4) 0.8805(3) 0.0258(10) Uani 1 1 d . . . . .
H31 H 0.1491 0.0478 0.8853 0.031 Uiso 1 1 calc R U . . .
C32 C 0.2842(4) 0.1250(4) 0.8270(3) 0.0208(9) Uani 1 1 d . . . . .
C33 C 0.2964(4) 0.0226(4) 0.7802(3) 0.0231(10) Uani 1 1 d . . . . .
C34 C 0.2245(4) -0.0890(4) 0.7797(3) 0.0261(10) Uani 1 1 d . . . . .
H34 H 0.1600 -0.1037 0.8051 0.031 Uiso 1 1 calc R U . . .
C35 C 0.2515(4) -0.1780(4) 0.7403(3) 0.0298(11) Uani 1 1 d . . . . .
H35 H 0.2060 -0.2534 0.7408 0.036 Uiso 1 1 calc R U . . .
C36 C 0.3447(4) -0.1557(4) 0.7005(3) 0.0291(11) Uani 1 1 d . . . . .
H36 H 0.3647 -0.2143 0.6747 0.035 Uiso 1 1 calc R U . . .
C37 C 0.4081(4) -0.0407(4) 0.7006(3) 0.0270(10) Uani 1 1 d . . . . .
C38 C 0.5429(5) -0.0773(4) 0.6088(4) 0.0378(13) Uani 1 1 d . . . . .
H38 H 0.5128 -0.1570 0.5954 0.045 Uiso 1 1 calc R U . . .
C39 C 0.6346(5) -0.0069(4) 0.5820(4) 0.0426(14) Uani 1 1 d . . . . .
H39 H 0.6803 -0.0279 0.5468 0.051 Uiso 1 1 calc R U . . .
C40 C 0.6460(5) 0.1041(5) 0.6185(4) 0.0407(13) Uani 1 1 d . . . . .
H40 H 0.7024 0.1702 0.6103 0.049 Uiso 1 1 calc R U . . .
N1 N 0.3786(4) 0.2271(3) 0.6191(3) 0.0304(9) Uani 1 1 d . . . . .
N1N N 0.0070(5) -0.0094(6) 0.6729(4) 0.0688(17) Uani 1 1 d . . . . .
N2 N 0.6106(4) 0.3376(3) 0.6513(3) 0.0285(9) Uani 1 1 d . . . . .
N2N N -0.3760(6) -0.0734(5) 0.8720(5) 0.0757(19) Uani 1 1 d . . . . .
N3 N 0.7217(3) 0.3201(3) 0.8088(3) 0.0254(9) Uani 1 1 d . . . . .
N3N N -0.1551(5) 0.1407(6) 0.4942(4) 0.078(2) Uani 1 1 d . . . . .
N4 N 0.6937(4) 0.2398(3) 0.9374(3) 0.0315(9) Uani 1 1 d . . . . .
N5 N 0.5769(3) 0.1969(3) 0.8981(3) 0.0284(9) Uani 1 1 d . . . . .
N6 N 0.5255(3) 0.4231(3) 0.8075(3) 0.0239(8) Uani 1 1 d . . . . .
N7 N 0.3606(3) 0.2255(3) 0.8196(2) 0.0209(8) Uani 1 1 d . . . . .
N8 N 0.3868(3) 0.0459(3) 0.7397(2) 0.0227(8) Uani 1 1 d . . . . .
N9 N 0.5031(4) -0.0098(3) 0.6588(3) 0.0300(9) Uani 1 1 d . . . . .
N10 N 0.5671(4) 0.1041(3) 0.6662(3) 0.0321(10) Uani 1 1 d . . . . .
F5 F 0.8557(3) 0.7267(4) 0.7729(3) 0.0836(14) Uani 1 1 d . . . . .
F6 F 0.8934(3) 0.6638(3) 0.9041(2) 0.0546(9) Uani 1 1 d . . . . .
F7 F 1.0250(3) 0.7013(3) 0.8171(3) 0.0599(10) Uani 1 1 d . . . . .
F8 F 0.9955(3) 0.8455(3) 0.8950(3) 0.0696(12) Uani 1 1 d . . . . .
B1 B 0.1903(18) 0.4914(18) 0.6967(14) 0.074(3) Uani 0.344(11) 1 d D U P A 1
F1 F 0.1135(13) 0.5177(12) 0.6341(10) 0.074(3) Uani 0.344(11) 1 d D U P A 1
F2 F 0.1706(10) 0.5231(14) 0.7816(8) 0.074(3) Uani 0.344(11) 1 d D U P A 1
F3 F 0.2296(11) 0.4045(10) 0.6821(11) 0.074(3) Uani 0.344(11) 1 d D U P A 1
F4 F 0.3016(12) 0.5823(12) 0.7191(10) 0.074(3) Uani 0.344(11) 1 d D U P A 1
B1' B 0.1854(10) 0.4828(10) 0.6884(8) 0.0485(12) Uani 0.656(11) 1 d D U P A 2
F1' F 0.0814(5) 0.4749(5) 0.6318(4) 0.0485(12) Uani 0.656(11) 1 d D U P A 2
F2' F 0.1638(5) 0.4555(6) 0.7704(3) 0.0485(12) Uani 0.656(11) 1 d D U P A 2
F3' F 0.2126(6) 0.4004(5) 0.6385(4) 0.0485(12) Uani 0.656(11) 1 d D U P A 2
F4' F 0.2715(6) 0.5879(5) 0.6930(4) 0.0485(12) Uani 0.656(11) 1 d D U P A 2
Fe1 Fe 0.51197(6) 0.23781(5) 0.74889(5) 0.0254(2) Uani 1 1 d . . . . .
B2 B 0.9413(5) 0.7350(5) 0.8468(4) 0.0374(14) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.294(6) . ?
C1 C2 1.416(7) . ?
C1N N1N 1.171(9) . ?
C1N C2N 1.403(10) . ?
C2 C3 1.344(8) . ?
C3 C4 1.434(7) . ?
C3N N2N 1.110(8) . ?
C3N C4N 1.447(11) . ?
C4 C5 1.372(7) . ?
C4 C6 1.418(7) . ?
C5 N1 1.393(6) . ?
C5 C9 1.419(7) . ?
C5N N3N 1.132(8) . ?
C5N C6N 1.444(8) . ?
C6 C7 1.365(7) . ?
C7 C8 1.417(7) . ?
C8 C10 1.377(8) . ?
C8 C9 1.445(7) . ?
C9 N2 1.343(6) . ?
C10 C11 1.386(8) . ?
C11 C12 1.386(7) . ?
C12 N2 1.317(6) . ?
C12 C13 1.508(7) . ?
C13 N3 1.316(6) . ?
C13 C14 1.376(7) . ?
C14 C15 1.395(8) . ?
C15 C16 1.347(7) . ?
C16 C17 1.439(7) . ?
C17 N3 1.325(6) . ?
C17 N4 1.384(6) . ?
C18 N4 1.367(6) . ?
C18 C19 1.369(7) . ?
C19 C20 1.391(7) . ?
C20 N5 1.312(6) . ?
C21 N6 1.313(6) . ?
C21 C22 1.394(7) . ?
C22 C23 1.351(7) . ?
C23 C24 1.396(7) . ?
C24 C25 1.400(6) . ?
C24 C26 1.437(6) . ?
C25 N6 1.372(6) . ?
C25 C29 1.436(6) . ?
C26 C27 1.350(7) . ?
C27 C28 1.420(6) . ?
C28 C30 1.392(7) . ?
C28 C29 1.425(6) . ?
C29 N7 1.331(6) . ?
C30 C31 1.367(7) . ?
C31 C32 1.413(6) . ?
C32 N7 1.335(6) . ?
C32 C33 1.473(6) . ?
C33 N8 1.346(6) . ?
C33 C34 1.388(6) . ?
C34 C35 1.387(7) . ?
C35 C36 1.370(7) . ?
C36 C37 1.398(7) . ?
C37 N8 1.318(6) . ?
C37 N9 1.407(6) . ?
C38 C39 1.352(7) . ?
C38 N9 1.355(6) . ?
C39 C40 1.398(7) . ?
C40 N10 1.326(6) . ?
N1 Fe1 2.279(4) . ?
N2 Fe1 2.297(4) . ?
N3 Fe1 2.424(4) . ?
N4 N5 1.363(5) . ?
N5 Fe1 2.411(4) . ?
N6 Fe1 2.348(4) . ?
N7 Fe1 2.314(4) . ?
N8 Fe1 2.367(4) . ?
N9 N10 1.367(5) . ?
N10 Fe1 2.355(4) . ?
F5 B2 1.361(8) . ?
F6 B2 1.380(7) . ?
F7 B2 1.390(7) . ?
F8 B2 1.370(7) . ?
B1 F3 1.365(17) . ?
B1 F1 1.373(16) . ?
B1 F2 1.383(18) . ?
B1 F4 1.423(18) . ?
B1' F2' 1.362(11) . ?
B1' F4' 1.381(11) . ?
B1' F1' 1.387(12) . ?
B1' F3' 1.390(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 C2 125.6(5) . . ?
N1N C1N C2N 178.0(8) . . ?
C3 C2 C1 118.3(5) . . ?
C2 C3 C4 118.8(5) . . ?
N2N C3N C4N 178.5(9) . . ?
C5 C4 C6 118.7(5) . . ?
C5 C4 C3 118.3(4) . . ?
C6 C4 C3 123.0(5) . . ?
C4 C5 N1 122.9(4) . . ?
C4 C5 C9 121.3(4) . . ?
N1 C5 C9 115.7(4) . . ?
N3N C5N C6N 179.5(9) . . ?
C7 C6 C4 122.3(5) . . ?
C6 C7 C8 120.3(4) . . ?
C10 C8 C7 124.2(5) . . ?
C10 C8 C9 117.6(5) . . ?
C7 C8 C9 118.2(5) . . ?
N2 C9 C5 119.6(4) . . ?
N2 C9 C8 121.3(5) . . ?
C5 C9 C8 119.1(4) . . ?
C8 C10 C11 120.3(5) . . ?
C10 C11 C12 117.8(5) . . ?
N2 C12 C11 124.4(5) . . ?
N2 C12 C13 113.6(4) . . ?
C11 C12 C13 122.0(4) . . ?
N3 C13 C14 121.9(5) . . ?
N3 C13 C12 114.7(4) . . ?
C14 C13 C12 123.4(5) . . ?
C13 C14 C15 118.9(5) . . ?
C16 C15 C14 121.0(5) . . ?
C15 C16 C17 115.9(5) . . ?
N3 C17 N4 116.5(4) . . ?
N3 C17 C16 122.8(4) . . ?
N4 C17 C16 120.7(5) . . ?
N4 C18 C19 105.4(5) . . ?
C18 C19 C20 106.3(5) . . ?
N5 C20 C19 111.7(5) . . ?
N6 C21 C22 124.5(4) . . ?
C23 C22 C21 119.2(4) . . ?
C22 C23 C24 119.3(4) . . ?
C23 C24 C25 117.7(4) . . ?
C23 C24 C26 123.2(4) . . ?
C25 C24 C26 119.1(4) . . ?
N6 C25 C24 123.0(4) . . ?
N6 C25 C29 117.4(4) . . ?
C24 C25 C29 119.6(4) . . ?
C27 C26 C24 121.7(4) . . ?
C26 C27 C28 120.6(4) . . ?
C30 C28 C27 123.8(4) . . ?
C30 C28 C29 116.6(4) . . ?
C27 C28 C29 119.6(4) . . ?
N7 C29 C28 122.8(4) . . ?
N7 C29 C25 117.9(4) . . ?
C28 C29 C25 119.3(4) . . ?
C31 C30 C28 120.7(4) . . ?
C30 C31 C32 118.9(4) . . ?
N7 C32 C31 121.6(4) . . ?
N7 C32 C33 115.6(4) . . ?
C31 C32 C33 122.7(4) . . ?
N8 C33 C34 122.0(4) . . ?
N8 C33 C32 114.1(4) . . ?
C34 C33 C32 123.8(4) . . ?
C35 C34 C33 118.2(4) . . ?
C36 C35 C34 120.5(4) . . ?
C35 C36 C37 116.8(4) . . ?
N8 C37 C36 124.2(4) . . ?
N8 C37 N9 115.0(4) . . ?
C36 C37 N9 120.8(4) . . ?
C39 C38 N9 107.1(4) . . ?
C38 C39 C40 105.2(4) . . ?
N10 C40 C39 112.2(5) . . ?
C1 N1 C5 116.1(4) . . ?
C1 N1 Fe1 127.1(3) . . ?
C5 N1 Fe1 116.8(3) . . ?
C12 N2 C9 118.7(4) . . ?
C12 N2 Fe1 125.3(3) . . ?
C9 N2 Fe1 116.0(3) . . ?
C13 N3 C17 119.6(4) . . ?
C13 N3 Fe1 120.0(3) . . ?
C17 N3 Fe1 120.4(3) . . ?
N5 N4 C18 111.8(4) . . ?
N5 N4 C17 119.0(4) . . ?
C18 N4 C17 129.1(5) . . ?
C20 N5 N4 104.9(4) . . ?
C20 N5 Fe1 137.0(3) . . ?
N4 N5 Fe1 118.1(3) . . ?
C21 N6 C25 116.3(4) . . ?
C21 N6 Fe1 128.0(3) . . ?
C25 N6 Fe1 115.8(3) . . ?
C29 N7 C32 119.4(4) . . ?
C29 N7 Fe1 118.1(3) . . ?
C32 N7 Fe1 122.0(3) . . ?
C37 N8 C33 118.2(4) . . ?
C37 N8 Fe1 121.1(3) . . ?
C33 N8 Fe1 120.6(3) . . ?
C38 N9 N10 111.8(4) . . ?
C38 N9 C37 129.6(4) . . ?
N10 N9 C37 118.5(4) . . ?
C40 N10 N9 103.7(4) . . ?
C40 N10 Fe1 138.5(3) . . ?
N9 N10 Fe1 117.8(3) . . ?
F3 B1 F1 126.9(16) . . ?
F3 B1 F2 120.8(16) . . ?
F1 B1 F2 104.6(14) . . ?
F3 B1 F4 96.4(14) . . ?
F1 B1 F4 109.4(15) . . ?
F2 B1 F4 91.4(14) . . ?
F2' B1' F4' 116.5(9) . . ?
F2' B1' F1' 108.0(8) . . ?
F4' B1' F1' 110.1(8) . . ?
F2' B1' F3' 112.0(9) . . ?
F4' B1' F3' 107.2(8) . . ?
F1' B1' F3' 102.1(8) . . ?
N1 Fe1 N2 71.92(15) . . ?
N1 Fe1 N7 83.42(14) . . ?
N2 Fe1 N7 141.26(14) . . ?
N1 Fe1 N6 90.89(14) . . ?
N2 Fe1 N6 80.22(13) . . ?
N7 Fe1 N6 70.56(13) . . ?
N1 Fe1 N10 90.00(15) . . ?
N2 Fe1 N10 75.81(14) . . ?
N7 Fe1 N10 134.84(13) . . ?
N6 Fe1 N10 154.46(13) . . ?
N1 Fe1 N8 83.42(14) . . ?
N2 Fe1 N8 135.34(13) . . ?
N7 Fe1 N8 67.50(13) . . ?
N6 Fe1 N8 138.05(13) . . ?
N10 Fe1 N8 67.37(13) . . ?
N1 Fe1 N5 155.59(14) . . ?
N2 Fe1 N5 132.44(14) . . ?
N7 Fe1 N5 76.27(13) . . ?
N6 Fe1 N5 94.92(13) . . ?
N10 Fe1 N5 94.75(14) . . ?
N8 Fe1 N5 76.43(13) . . ?
N1 Fe1 N3 138.28(14) . . ?
N2 Fe1 N3 66.37(14) . . ?
N7 Fe1 N3 131.56(13) . . ?
N6 Fe1 N3 83.11(13) . . ?
N10 Fe1 N3 79.33(14) . . ?
N8 Fe1 N3 126.85(13) . . ?
N5 Fe1 N3 66.07(13) . . ?
F5 B2 F8 111.1(6) . . ?
F5 B2 F6 109.2(5) . . ?
F8 B2 F6 109.8(5) . . ?
F5 B2 F7 110.0(5) . . ?
F8 B2 F7 108.0(5) . . ?
F6 B2 F7 108.7(5) . . ?

_refine_diff_density_max         1.735
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.088

_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_HS_Fe5d
_database_code_depnum_ccdc_archive 'CCDC 1519518'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            HS-[Fe(5d)2](BF4)2
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H20 Br2 Fe N6, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H26 B2 Br2 F8 Fe N8'
_chemical_formula_weight         983.96

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'
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'
Br Br -0.2901 2.4595 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.074(1)
_cell_length_b                   12.2201(8)
_cell_length_c                   14.8271(8)
_cell_angle_alpha                81.490(5)
_cell_angle_beta                 86.353(5)
_cell_angle_gamma                113.602(7)
_cell_volume                     1964.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298
_cell_measurement_reflns_used    3804
_cell_measurement_theta_min      3.3680
_cell_measurement_theta_max      25.6950

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.497
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.77095
_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      298
_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_standards_number         1
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  25
_diffrn_standards_decay_%        2

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11687
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.054
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.943
_reflns_number_total             6525
_reflns_number_gt                4185
_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 1.171.36.28 (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)+(0.1808P)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         6525
_refine_ls_number_parameters     580
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.2636
_refine_ls_wR_factor_gt          0.1866
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.048
_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 -0.0190(8) 0.9385(7) 0.2996(5) 0.0592(19) Uani 1 1 d . . . . .
H1 H -0.0298 0.8796 0.2638 0.071 Uiso 1 1 calc R U . . .
C2 C -0.1220(8) 0.9477(7) 0.3359(5) 0.067(2) Uani 1 1 d . . . . .
H2 H -0.1990 0.8975 0.3244 0.081 Uiso 1 1 calc R U . . .
C3 C -0.1068(9) 1.0348(8) 0.3906(6) 0.075(3) Uani 1 1 d . . . . .
H3 H -0.1743 1.0440 0.4160 0.090 Uiso 1 1 calc R U . . .
C4 C 0.0094(8) 1.1079(7) 0.4070(5) 0.0596(19) Uani 1 1 d . . . . .
C5 C 0.1074(8) 1.0910(6) 0.3650(4) 0.0548(19) Uani 1 1 d . . . . .
C6 C 0.0337(10) 1.1974(8) 0.4636(5) 0.074(2) Uani 1 1 d . . . . .
H6 H -0.0310 1.2092 0.4911 0.089 Uiso 1 1 calc R U . . .
C7 C 0.1498(13) 1.2665(8) 0.4784(5) 0.091(3) Uani 1 1 d . . . . .
H7 H 0.1628 1.3237 0.5162 0.109 Uiso 1 1 calc R U . . .
C8 C 0.2509(9) 1.2514(7) 0.4366(5) 0.066(2) Uani 1 1 d . . . . .
C9 C 0.2311(8) 1.1650(5) 0.3803(4) 0.0524(18) Uani 1 1 d . . . . .
C10 C 0.3727(11) 1.3155(8) 0.4507(6) 0.085(3) Uani 1 1 d . . . . .
H10 H 0.3911 1.3721 0.4893 0.102 Uiso 1 1 calc R U . . .
C11 C 0.4624(12) 1.2949(7) 0.4085(6) 0.089(3) Uani 1 1 d . . . . .
H11 H 0.5429 1.3379 0.4171 0.107 Uiso 1 1 calc R U . . .
C12 C 0.4337(8) 1.2064(6) 0.3499(5) 0.060(2) Uani 1 1 d . . . . .
C13 C 0.5203(8) 1.1738(6) 0.3003(5) 0.061(2) Uani 1 1 d . . . . .
C14 C 0.6489(9) 1.2273(8) 0.3068(6) 0.079(3) Uani 1 1 d . . . . .
H14 H 0.6816 1.2874 0.3415 0.095 Uiso 1 1 calc R U . . .
C15 C 0.7195(10) 1.1872(11) 0.2611(7) 0.095(3) Uani 1 1 d . . . . .
H15 H 0.8027 1.2198 0.2650 0.114 Uiso 1 1 calc R U . . .
C16 C 0.6744(9) 1.1013(9) 0.2095(7) 0.081(3) Uani 1 1 d . . . . .
H16 H 0.7251 1.0750 0.1778 0.098 Uiso 1 1 calc R U . . .
C17 C 0.5503(8) 1.0535(8) 0.2053(5) 0.068(2) Uani 1 1 d . . . . .
C18 C 0.3432(10) 1.2748(7) 0.1159(5) 0.075(2) Uani 1 1 d . . . . .
H18 H 0.3853 1.3121 0.1612 0.090 Uiso 1 1 calc R U . . .
C19 C 0.3358(10) 1.3466(7) 0.0351(6) 0.082(3) Uani 1 1 d . . . . .
H19 H 0.3661 1.4305 0.0307 0.098 Uiso 1 1 calc R U . . .
C20 C 0.2869(7) 1.2980(7) -0.0349(5) 0.064(2) Uani 1 1 d . . . . .
H20 H 0.2898 1.3472 -0.0900 0.077 Uiso 1 1 calc R U . . .
C21 C 0.2302(7) 1.1699(6) -0.0241(5) 0.0576(18) Uani 1 1 d . . . . .
C22 C 0.2362(7) 1.1029(6) 0.0601(4) 0.0481(16) Uani 1 1 d . . . . .
C23 C 0.1697(8) 1.1071(7) -0.0921(5) 0.068(2) Uani 1 1 d . . . . .
H23 H 0.1682 1.1517 -0.1481 0.082 Uiso 1 1 calc R U . . .
C24 C 0.1146(7) 0.9851(7) -0.0779(5) 0.0611(19) Uani 1 1 d . . . . .
H24 H 0.0726 0.9467 -0.1228 0.073 Uiso 1 1 calc R U . . .
C25 C 0.1203(7) 0.9142(6) 0.0060(4) 0.0536(17) Uani 1 1 d . . . . .
C26 C 0.1804(7) 0.9718(6) 0.0738(4) 0.0507(16) Uani 1 1 d . . . . .
C27 C 0.0678(7) 0.7858(7) 0.0272(5) 0.064(2) Uani 1 1 d . . . . .
H27 H 0.0278 0.7422 -0.0162 0.076 Uiso 1 1 calc R U . . .
C28 C 0.0745(7) 0.7246(6) 0.1093(6) 0.0598(19) Uani 1 1 d . . . . .
H28 H 0.0370 0.6401 0.1237 0.072 Uiso 1 1 calc R U . . .
C29 C 0.1403(7) 0.7934(6) 0.1729(5) 0.0559(18) Uani 1 1 d . . . . .
C30 C 0.1585(7) 0.7407(6) 0.2651(5) 0.0525(16) Uani 1 1 d . . . . .
C31 C 0.1084(9) 0.6157(7) 0.2984(6) 0.074(2) Uani 1 1 d . . . . .
H31 H 0.0612 0.5612 0.2638 0.088 Uiso 1 1 calc R U . . .
C32 C 0.1308(12) 0.5758(9) 0.3829(8) 0.108(4) Uani 1 1 d . . . . .
H32 H 0.0988 0.4927 0.4062 0.130 Uiso 1 1 calc R U . . .
C33 C 0.1988(10) 0.6547(8) 0.4339(6) 0.086(3) Uani 1 1 d . . . . .
H33 H 0.2156 0.6285 0.4915 0.103 Uiso 1 1 calc R U . . .
C34 C 0.2417(8) 0.7768(7) 0.3948(5) 0.066(2) Uani 1 1 d . . . . .
C35 C 0.3108(14) 0.6650(14) -0.0213(10) 0.113(4) Uani 1 1 d . . . . .
C36 C 0.2176(17) 0.5808(11) -0.0622(8) 0.135(5) Uani 1 1 d . . . . .
H36A H 0.2472 0.5869 -0.1252 0.202 Uiso 1 1 calc R U . . .
H36B H 0.1474 0.5993 -0.0597 0.202 Uiso 1 1 calc R U . . .
H36C H 0.1954 0.4997 -0.0291 0.202 Uiso 1 1 calc R U . . .
C37 C 0.500(2) 0.701(2) 0.3036(16) 0.180(9) Uani 1 1 d . . . . .
C38 C 0.4432(19) 0.6107(16) 0.2474(15) 0.187(8) Uani 1 1 d . . . . .
H38A H 0.4209 0.6478 0.1941 0.281 Uiso 1 1 calc R U . . .
H38B H 0.3717 0.5456 0.2827 0.281 Uiso 1 1 calc R U . . .
H38C H 0.5001 0.5790 0.2283 0.281 Uiso 1 1 calc R U . . .
B1 B -0.0740(9) 0.6533(8) -0.2011(6) 0.073(3) Uani 1 1 d D . . . .
N1 N 0.0972(6) 1.0084(4) 0.3118(3) 0.0502(14) Uani 1 1 d . . . . .
N2 N 0.3183(6) 1.1438(5) 0.3383(4) 0.0529(15) Uani 1 1 d . . . . .
N3 N 0.4739(5) 1.0882(5) 0.2493(4) 0.0542(14) Uani 1 1 d . . . . .
N4 N 0.2896(6) 1.1522(5) 0.1284(4) 0.0562(15) Uani 1 1 d . . . . .
N5 N 0.1882(5) 0.9126(4) 0.1552(4) 0.0479(13) Uani 1 1 d . . . . .
N6 N 0.2238(5) 0.8213(5) 0.3140(4) 0.0499(13) Uani 1 1 d . . . . .
N7 N 0.3902(19) 0.7266(15) 0.0096(13) 0.205(8) Uani 1 1 d . . . . .
N8 N 0.538(2) 0.779(2) 0.3452(12) 0.203(8) Uani 1 1 d . . . . .
F1 F -0.0480(7) 0.7640(5) -0.1795(4) 0.121(2) Uani 1 1 d D . . . .
F2 F -0.1905(6) 0.6086(8) -0.2206(7) 0.170(4) Uani 1 1 d D . . . .
F3 F -0.0588(10) 0.5788(6) -0.1320(5) 0.169(4) Uani 1 1 d D . . . .
F4 F -0.0057(6) 0.6591(5) -0.2788(4) 0.1066(19) Uani 1 1 d D . . . .
B2 B 0.251(2) 0.447(2) 0.7048(13) 0.054(7) Uani 0.314(17) 1 d D U P A 1
F5 F 0.277(3) 0.478(2) 0.6117(11) 0.099(10) Uani 0.314(17) 1 d D U P A 1
F6 F 0.1631(18) 0.483(2) 0.737(2) 0.130(11) Uani 0.314(17) 1 d D U P A 1
F7 F 0.209(3) 0.3235(14) 0.7264(16) 0.127(11) Uani 0.314(17) 1 d D U P A 1
F8 F 0.3373(15) 0.501(2) 0.7587(15) 0.060(5) Uani 0.314(17) 1 d D U P A 1
B2' B 0.2353(15) 0.4237(14) 0.6960(12) 0.084(7) Uani 0.686(17) 1 d D . P A 2
F5' F 0.3138(15) 0.396(3) 0.6476(17) 0.244(13) Uani 0.686(17) 1 d D . P A 2
F6' F 0.2095(18) 0.5012(12) 0.6374(13) 0.162(9) Uani 0.686(17) 1 d D . P A 2
F7' F 0.1382(12) 0.3278(14) 0.7310(15) 0.202(10) Uani 0.686(17) 1 d D . P A 2
F8' F 0.312(2) 0.4797(16) 0.7512(12) 0.191(11) Uani 0.686(17) 1 d D . P A 2
Fe1 Fe 0.27327(9) 1.01696(8) 0.25120(6) 0.0451(3) Uani 1 1 d . . . . .
Br1 Br 0.48265(10) 0.93900(9) 0.13020(6) 0.0852(4) Uani 1 1 d . . . . .
Br2 Br 0.34108(9) 0.89255(8) 0.46217(5) 0.0734(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.359(10) . ?
C1 C2 1.375(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.394(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(11) . ?
C4 C6 1.425(11) . ?
C5 N1 1.344(8) . ?
C5 C9 1.457(11) . ?
C6 C7 1.369(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.424(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.398(9) . ?
C8 C10 1.409(14) . ?
C9 N2 1.321(10) . ?
C10 C11 1.344(16) . ?
C10 H10 0.9300 . ?
C11 C12 1.435(11) . ?
C11 H11 0.9300 . ?
C12 N2 1.332(10) . ?
C12 C13 1.454(12) . ?
C13 N3 1.342(9) . ?
C13 C14 1.440(13) . ?
C14 C15 1.336(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.348(14) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(13) . ?
C16 H16 0.9300 . ?
C17 N3 1.331(10) . ?
C17 Br1 1.879(9) . ?
C18 N4 1.350(9) . ?
C18 C19 1.406(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.326(12) . ?
C19 H19 0.9300 . ?
C20 C21 1.413(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.410(9) . ?
C21 C23 1.419(10) . ?
C22 N4 1.325(9) . ?
C22 C26 1.443(9) . ?
C23 C24 1.343(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.429(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.389(9) . ?
C25 C27 1.413(10) . ?
C26 N5 1.341(8) . ?
C27 C28 1.356(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.422(10) . ?
C28 H28 0.9300 . ?
C29 N5 1.311(8) . ?
C29 C30 1.491(10) . ?
C30 N6 1.333(9) . ?
C30 C31 1.394(9) . ?
C31 C32 1.359(13) . ?
C31 H31 0.9300 . ?
C32 C33 1.355(14) . ?
C32 H32 0.9300 . ?
C33 C34 1.385(11) . ?
C33 H33 0.9300 . ?
C34 N6 1.308(9) . ?
C34 Br2 1.911(8) . ?
C35 N7 1.13(2) . ?
C35 C36 1.43(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N8 1.16(2) . ?
C37 C38 1.46(2) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
B1 F1 1.352(10) . ?
B1 F3 1.339(10) . ?
B1 F4 1.350(11) . ?
B1 F2 1.358(11) . ?
N1 Fe1 2.211(6) . ?
N2 Fe1 2.091(5) . ?
N3 Fe1 2.219(6) . ?
N4 Fe1 2.211(5) . ?
N5 Fe1 2.094(5) . ?
N6 Fe1 2.251(5) . ?
B2 F5 1.358(17) . ?
B2 F7 1.367(18) . ?
B2 F8 1.371(18) . ?
B2 F6 1.378(18) . ?
B2' F7' 1.288(15) . ?
B2' F8' 1.321(14) . ?
B2' F6' 1.333(15) . ?
B2' F5' 1.333(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
N1 C1 C2 125.5(7) . . ?
N1 C1 H1 117.3 . . ?
C2 C1 H1 117.3 . . ?
C1 C2 C3 117.7(8) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C2 C3 C4 119.8(8) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 117.1(7) . . ?
C3 C4 C6 123.9(8) . . ?
C5 C4 C6 119.0(8) . . ?
N1 C5 C4 125.1(8) . . ?
N1 C5 C9 115.5(7) . . ?
C4 C5 C9 119.3(6) . . ?
C7 C6 C4 121.7(9) . . ?
C7 C6 H6 119.2 . . ?
C4 C6 H6 119.1 . . ?
C6 C7 C8 120.5(8) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 119.6(9) . . ?
C9 C8 C10 116.2(8) . . ?
C7 C8 C10 124.2(8) . . ?
N2 C9 C8 124.4(8) . . ?
N2 C9 C5 115.7(6) . . ?
C8 C9 C5 119.9(8) . . ?
C11 C10 C8 120.0(8) . . ?
C11 C10 H10 120.0 . . ?
C8 C10 H10 120.0 . . ?
C10 C11 C12 120.0(10) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
N2 C12 C11 120.0(9) . . ?
N2 C12 C13 113.8(6) . . ?
C11 C12 C13 126.2(9) . . ?
N3 C13 C14 121.0(8) . . ?
N3 C13 C12 116.5(7) . . ?
C14 C13 C12 122.4(8) . . ?
C15 C14 C13 117.4(9) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C16 122.4(10) . . ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
C15 C16 C17 117.8(10) . . ?
C15 C16 H16 121.1 . . ?
C17 C16 H16 121.1 . . ?
N3 C17 C16 123.4(8) . . ?
N3 C17 Br1 116.5(6) . . ?
C16 C17 Br1 120.0(7) . . ?
N4 C18 C19 120.6(8) . . ?
N4 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 121.8(7) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C19 C20 C21 118.7(7) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.7 . . ?
C22 C21 C20 116.5(7) . . ?
C22 C21 C23 119.4(6) . . ?
C20 C21 C23 124.1(7) . . ?
N4 C22 C21 124.4(6) . . ?
N4 C22 C26 117.2(6) . . ?
C21 C22 C26 118.5(6) . . ?
C24 C23 C21 122.0(7) . . ?
C24 C23 H23 119.0 . . ?
C21 C23 H23 119.0 . . ?
C23 C24 C25 120.2(7) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C27 115.4(6) . . ?
C26 C25 C24 119.8(6) . . ?
C27 C25 C24 124.8(6) . . ?
N5 C26 C25 123.8(6) . . ?
N5 C26 C22 116.0(6) . . ?
C25 C26 C22 120.2(6) . . ?
C28 C27 C25 121.5(6) . . ?
C28 C27 H27 119.2 . . ?
C25 C27 H27 119.3 . . ?
C27 C28 C29 118.1(6) . . ?
C27 C28 H28 121.0 . . ?
C29 C28 H28 121.0 . . ?
N5 C29 C28 121.4(7) . . ?
N5 C29 C30 113.6(6) . . ?
C28 C29 C30 125.0(6) . . ?
N6 C30 C31 122.5(7) . . ?
N6 C30 C29 115.5(5) . . ?
C31 C30 C29 122.0(7) . . ?
C32 C31 C30 118.0(8) . . ?
C32 C31 H31 121.0 . . ?
C30 C31 H31 121.0 . . ?
C33 C32 C31 121.3(8) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 115.7(8) . . ?
C32 C33 H33 122.2 . . ?
C34 C33 H33 122.2 . . ?
N6 C34 C33 126.1(8) . . ?
N6 C34 Br2 116.1(5) . . ?
C33 C34 Br2 117.7(6) . . ?
N7 C35 C36 174.4(19) . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N8 C37 C38 173(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
F1 B1 F3 110.8(8) . . ?
F1 B1 F4 112.7(8) . . ?
F3 B1 F4 109.1(9) . . ?
F1 B1 F2 107.8(8) . . ?
F3 B1 F2 111.6(9) . . ?
F4 B1 F2 104.7(8) . . ?
C5 N1 C1 114.8(6) . . ?
C5 N1 Fe1 114.4(5) . . ?
C1 N1 Fe1 130.7(4) . . ?
C9 N2 C12 119.4(6) . . ?
C9 N2 Fe1 119.4(5) . . ?
C12 N2 Fe1 121.1(5) . . ?
C17 N3 C13 118.0(7) . . ?
C17 N3 Fe1 127.3(5) . . ?
C13 N3 Fe1 114.7(5) . . ?
C22 N4 C18 117.7(6) . . ?
C22 N4 Fe1 113.6(4) . . ?
C18 N4 Fe1 128.7(5) . . ?
C29 N5 C26 119.8(6) . . ?
C29 N5 Fe1 122.5(4) . . ?
C26 N5 Fe1 117.7(4) . . ?
C34 N6 C30 116.4(6) . . ?
C34 N6 Fe1 128.4(5) . . ?
C30 N6 Fe1 114.9(4) . . ?
F5 B2 F7 106.4(18) . . ?
F5 B2 F8 120(2) . . ?
F7 B2 F8 110(2) . . ?
F5 B2 F6 112(2) . . ?
F7 B2 F6 110(2) . . ?
F8 B2 F6 98.1(16) . . ?
F7' B2' F8' 118.9(18) . . ?
F7' B2' F6' 111.2(16) . . ?
F8' B2' F6' 111.8(15) . . ?
F7' B2' F5' 111.0(17) . . ?
F8' B2' F5' 96.2(16) . . ?
F6' B2' F5' 106.1(18) . . ?
N2 Fe1 N5 162.0(2) . . ?
N2 Fe1 N4 93.9(2) . . ?
N5 Fe1 N4 75.5(2) . . ?
N2 Fe1 N1 74.6(2) . . ?
N5 Fe1 N1 91.3(2) . . ?
N4 Fe1 N1 93.6(2) . . ?
N2 Fe1 N3 73.8(2) . . ?
N5 Fe1 N3 120.5(2) . . ?
N4 Fe1 N3 92.6(2) . . ?
N1 Fe1 N3 148.2(2) . . ?
N2 Fe1 N6 117.8(2) . . ?
N5 Fe1 N6 73.1(2) . . ?
N4 Fe1 N6 148.1(2) . . ?
N1 Fe1 N6 92.28(19) . . ?
N3 Fe1 N6 98.6(2) . . ?

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 -0.7(11) . . . . ?
C1 C2 C3 C4 -0.4(11) . . . . ?
C2 C3 C4 C5 1.3(10) . . . . ?
C2 C3 C4 C6 -178.5(7) . . . . ?
C3 C4 C5 N1 -1.3(10) . . . . ?
C6 C4 C5 N1 178.5(6) . . . . ?
C3 C4 C5 C9 -179.8(6) . . . . ?
C6 C4 C5 C9 0.1(9) . . . . ?
C3 C4 C6 C7 179.3(7) . . . . ?
C5 C4 C6 C7 -0.5(11) . . . . ?
C4 C6 C7 C8 0.6(12) . . . . ?
C6 C7 C8 C9 -0.3(11) . . . . ?
C6 C7 C8 C10 -177.7(8) . . . . ?
C7 C8 C9 N2 -180.0(6) . . . . ?
C10 C8 C9 N2 -2.3(10) . . . . ?
C7 C8 C9 C5 -0.2(10) . . . . ?
C10 C8 C9 C5 177.5(6) . . . . ?
N1 C5 C9 N2 1.5(8) . . . . ?
C4 C5 C9 N2 -179.9(6) . . . . ?
N1 C5 C9 C8 -178.4(5) . . . . ?
C4 C5 C9 C8 0.3(9) . . . . ?
C9 C8 C10 C11 2.2(12) . . . . ?
C7 C8 C10 C11 179.8(8) . . . . ?
C8 C10 C11 C12 -0.8(13) . . . . ?
C10 C11 C12 N2 -0.8(11) . . . . ?
C10 C11 C12 C13 -179.6(8) . . . . ?
N2 C12 C13 N3 1.0(9) . . . . ?
C11 C12 C13 N3 179.9(6) . . . . ?
N2 C12 C13 C14 -177.4(6) . . . . ?
C11 C12 C13 C14 1.5(11) . . . . ?
N3 C13 C14 C15 -0.8(11) . . . . ?
C12 C13 C14 C15 177.5(7) . . . . ?
C13 C14 C15 C16 0.8(13) . . . . ?
C14 C15 C16 C17 -0.5(14) . . . . ?
C15 C16 C17 N3 0.1(13) . . . . ?
C15 C16 C17 Br1 177.0(7) . . . . ?
N4 C18 C19 C20 -6.5(15) . . . . ?
C18 C19 C20 C21 6.2(14) . . . . ?
C19 C20 C21 C22 -3.4(12) . . . . ?
C19 C20 C21 C23 176.9(8) . . . . ?
C20 C21 C22 N4 0.8(11) . . . . ?
C23 C21 C22 N4 -179.5(7) . . . . ?
C20 C21 C22 C26 -179.5(7) . . . . ?
C23 C21 C22 C26 0.2(10) . . . . ?
C22 C21 C23 C24 1.9(12) . . . . ?
C20 C21 C23 C24 -178.4(8) . . . . ?
C21 C23 C24 C25 -2.8(12) . . . . ?
C23 C24 C25 C26 1.6(12) . . . . ?
C23 C24 C25 C27 -178.7(8) . . . . ?
C27 C25 C26 N5 -1.1(11) . . . . ?
C24 C25 C26 N5 178.6(7) . . . . ?
C27 C25 C26 C22 -179.2(7) . . . . ?
C24 C25 C26 C22 0.5(11) . . . . ?
N4 C22 C26 N5 0.1(10) . . . . ?
C21 C22 C26 N5 -179.6(6) . . . . ?
N4 C22 C26 C25 178.4(7) . . . . ?
C21 C22 C26 C25 -1.3(10) . . . . ?
C26 C25 C27 C28 1.3(11) . . . . ?
C24 C25 C27 C28 -178.4(8) . . . . ?
C25 C27 C28 C29 -2.5(12) . . . . ?
C27 C28 C29 N5 3.5(12) . . . . ?
C27 C28 C29 C30 -178.8(7) . . . . ?
N5 C29 C30 N6 -2.5(10) . . . . ?
C28 C29 C30 N6 179.6(7) . . . . ?
N5 C29 C30 C31 176.4(7) . . . . ?
C28 C29 C30 C31 -1.4(12) . . . . ?
N6 C30 C31 C32 -1.8(14) . . . . ?
C29 C30 C31 C32 179.3(9) . . . . ?
C30 C31 C32 C33 0.5(18) . . . . ?
C31 C32 C33 C34 0.8(18) . . . . ?
C32 C33 C34 N6 -1.0(16) . . . . ?
C32 C33 C34 Br2 -178.7(9) . . . . ?
C4 C5 N1 C1 0.2(9) . . . . ?
C9 C5 N1 C1 178.8(5) . . . . ?
C4 C5 N1 Fe1 176.5(5) . . . . ?
C9 C5 N1 Fe1 -5.0(7) . . . . ?
C2 C1 N1 C5 0.8(10) . . . . ?
C2 C1 N1 Fe1 -174.7(5) . . . . ?
C8 C9 N2 C12 0.8(10) . . . . ?
C5 C9 N2 C12 -179.0(5) . . . . ?
C8 C9 N2 Fe1 -177.0(5) . . . . ?
C5 C9 N2 Fe1 3.2(7) . . . . ?
C11 C12 N2 C9 0.8(9) . . . . ?
C13 C12 N2 C9 179.7(6) . . . . ?
C11 C12 N2 Fe1 178.6(5) . . . . ?
C13 C12 N2 Fe1 -2.5(8) . . . . ?
C16 C17 N3 C13 -0.1(11) . . . . ?
Br1 C17 N3 C13 -177.2(5) . . . . ?
C16 C17 N3 Fe1 -178.6(6) . . . . ?
Br1 C17 N3 Fe1 4.4(8) . . . . ?
C14 C13 N3 C17 0.5(10) . . . . ?
C12 C13 N3 C17 -177.9(6) . . . . ?
C14 C13 N3 Fe1 179.1(5) . . . . ?
C12 C13 N3 Fe1 0.7(7) . . . . ?
C21 C22 N4 C18 -0.9(11) . . . . ?
C26 C22 N4 C18 179.4(7) . . . . ?
C21 C22 N4 Fe1 177.6(6) . . . . ?
C26 C22 N4 Fe1 -2.1(8) . . . . ?
C19 C18 N4 C22 3.6(13) . . . . ?
C19 C18 N4 Fe1 -174.7(7) . . . . ?
C28 C29 N5 C26 -3.3(11) . . . . ?
C30 C29 N5 C26 178.8(6) . . . . ?
C28 C29 N5 Fe1 174.9(6) . . . . ?
C30 C29 N5 Fe1 -3.1(9) . . . . ?
C25 C26 N5 C29 2.2(11) . . . . ?
C22 C26 N5 C29 -179.6(6) . . . . ?
C25 C26 N5 Fe1 -176.1(6) . . . . ?
C22 C26 N5 Fe1 2.1(8) . . . . ?
C33 C34 N6 C30 -0.2(13) . . . . ?
Br2 C34 N6 C30 177.5(5) . . . . ?
C33 C34 N6 Fe1 173.2(7) . . . . ?
Br2 C34 N6 Fe1 -9.1(9) . . . . ?
C31 C30 N6 C34 1.7(11) . . . . ?
C29 C30 N6 C34 -179.4(7) . . . . ?
C31 C30 N6 Fe1 -172.6(6) . . . . ?
C29 C30 N6 Fe1 6.3(8) . . . . ?

_refine_diff_density_max         0.665
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.166

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.943       
RESPONSE: The crystal selected for measurement has been measured before
at 110 K. Measurement at 298 K has been performed in order to investigate
spin-cross over properties. During measurement a slight decay of intensities
of reference frames could be already recognized, attributed to a partial
loss of MeCN molecules as packing solvents. Suddenly, ca. at the end of
the data collection the crystal did rupture. An identical behaviour has
been observed when measuring other crystals, with data completeness at
ca. 95 % as well. This measurement has been choosen finally, as it directly
refers to the measurement performed before at 100 K.
;
# 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_Zn_5e
_database_code_depnum_ccdc_archive 'CCDC 1538100'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Zn(5e)2](ClO4)2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H26 N10 Zn, 2(Cl O4), 3(C2 H3 N)'
_chemical_formula_sum            'C46 H35 Cl2 N13 O8 Zn'
_chemical_formula_weight         1034.14

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           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                   14.7030(4)
_cell_length_b                   14.7863(3)
_cell_length_c                   21.1329(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.007(2)
_cell_angle_gamma                90
_cell_volume                     4476.48(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    6236
_cell_measurement_theta_min      3.1630
_cell_measurement_theta_max      28.0130


_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_F_000             2120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.740
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.91594
_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     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            24690
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.927
_diffrn_reflns_theta_max         24.998
_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             7873
_reflns_number_gt                6363
_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 1.171.37.31 (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)+(0.0319P)²+2.4409P] 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         7873
_refine_ls_number_parameters     634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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 0.73557(17) 0.31771(14) 0.37526(11) 0.0195(5) Uani 1 1 d . . . . .
H1 H 0.6711 0.3239 0.3680 0.023 Uiso 1 1 calc R U . . .
C2 C 0.79037(18) 0.34505(14) 0.43494(11) 0.0225(6) Uani 1 1 d . . . . .
H2 H 0.7624 0.3676 0.4670 0.027 Uiso 1 1 calc R U . . .
C3 C 0.88542(18) 0.33850(14) 0.44612(11) 0.0202(5) Uani 1 1 d . . . . .
H3 H 0.9223 0.3568 0.4858 0.024 Uiso 1 1 calc R U . . .
C4 C 0.92727(17) 0.30405(14) 0.39743(11) 0.0176(5) Uani 1 1 d . . . . .
C5 C 0.86617(16) 0.27552(13) 0.33958(10) 0.0150(5) Uani 1 1 d . . . . .
C6 C 1.02538(16) 0.29562(14) 0.40309(11) 0.0188(5) Uani 1 1 d . . . . .
H6 H 1.0658 0.3134 0.4415 0.023 Uiso 1 1 calc R U . . .
C7 C 1.06156(17) 0.26264(14) 0.35438(11) 0.0186(5) Uani 1 1 d . . . . .
H7 H 1.1259 0.2610 0.3588 0.022 Uiso 1 1 calc R U . . .
C8 C 1.00100(16) 0.23006(14) 0.29580(10) 0.0156(5) Uani 1 1 d . . . . .
C9 C 0.90439(16) 0.23391(13) 0.28992(10) 0.0134(5) Uani 1 1 d . . . . .
C10 C 1.03244(16) 0.19143(14) 0.24360(11) 0.0173(5) Uani 1 1 d . . . . .
H10 H 1.0959 0.1903 0.2442 0.021 Uiso 1 1 calc R U . . .
C11 C 0.96913(16) 0.15538(14) 0.19178(11) 0.0175(5) Uani 1 1 d . . . . .
H11 H 0.9895 0.1296 0.1573 0.021 Uiso 1 1 calc R U . . .
C12 C 0.87424(16) 0.15777(13) 0.19136(10) 0.0141(5) Uani 1 1 d . . . . .
C13 C 0.80023(16) 0.11839(14) 0.13924(10) 0.0151(5) Uani 1 1 d . . . . .
C14 C 0.81037(17) 0.11237(15) 0.07568(10) 0.0189(5) Uani 1 1 d . . . . .
H14 H 0.8670 0.1259 0.0652 0.023 Uiso 1 1 calc R U . . .
C15 C 0.73387(17) 0.08573(15) 0.02824(11) 0.0210(5) Uani 1 1 d . . . . .
H15 H 0.7379 0.0835 -0.0150 0.025 Uiso 1 1 calc R U . . .
C16 C 0.65214(16) 0.06260(14) 0.04523(10) 0.0173(5) Uani 1 1 d . . . . .
H16 H 0.6002 0.0442 0.0141 0.021 Uiso 1 1 calc R U . . .
C17 C 0.64951(16) 0.06755(13) 0.11042(10) 0.0149(5) Uani 1 1 d . . . . .
C18 C 0.56222(16) 0.00503(14) 0.18926(10) 0.0173(5) Uani 1 1 d . . . . .
H18 H 0.6114 -0.0085 0.2241 0.021 Uiso 1 1 calc R U . . .
C19 C 0.47026(17) -0.00787(14) 0.18652(11) 0.0200(5) Uani 1 1 d . . . . .
H19 H 0.4434 -0.0321 0.2186 0.024 Uiso 1 1 calc R U . . .
C20 C 0.42419(17) 0.02303(15) 0.12496(11) 0.0223(5) Uani 1 1 d . . . . .
H20 H 0.3596 0.0230 0.1101 0.027 Uiso 1 1 calc R U . . .
C21 C 0.67603(17) 0.30980(13) 0.10925(11) 0.0176(5) Uani 1 1 d . . . . .
H21 H 0.7406 0.3124 0.1151 0.021 Uiso 1 1 calc R U . . .
C22 C 0.62040(17) 0.34109(14) 0.05082(11) 0.0201(5) Uani 1 1 d . . . . .
H22 H 0.6478 0.3626 0.0182 0.024 Uiso 1 1 calc R U . . .
C23 C 0.52571(18) 0.33983(14) 0.04193(11) 0.0207(5) Uani 1 1 d . . . . .
H23 H 0.4883 0.3610 0.0033 0.025 Uiso 1 1 calc R U . . .
C24 C 0.48471(17) 0.30652(14) 0.09124(11) 0.0178(5) Uani 1 1 d . . . . .
C25 C 0.54585(16) 0.27438(13) 0.14757(10) 0.0137(5) Uani 1 1 d . . . . .
C26 C 0.38632(17) 0.30447(15) 0.08782(11) 0.0220(5) Uani 1 1 d . . . . .
H26 H 0.3455 0.3254 0.0505 0.026 Uiso 1 1 calc R U . . .
C27 C 0.35129(17) 0.27310(15) 0.13717(11) 0.0217(5) Uani 1 1 d . . . . .
H27 H 0.2872 0.2748 0.1340 0.026 Uiso 1 1 calc R U . . .
C28 C 0.41138(16) 0.23719(14) 0.19450(11) 0.0176(5) Uani 1 1 d . . . . .
C29 C 0.50799(15) 0.23685(14) 0.19891(10) 0.0141(5) Uani 1 1 d . . . . .
C30 C 0.38047(17) 0.20034(14) 0.24753(11) 0.0196(5) Uani 1 1 d . . . . .
H30 H 0.3172 0.2007 0.2476 0.023 Uiso 1 1 calc R U . . .
C31 C 0.44350(16) 0.16406(15) 0.29887(11) 0.0188(5) Uani 1 1 d . . . . .
H31 H 0.4231 0.1395 0.3338 0.023 Uiso 1 1 calc R U . . .
C32 C 0.53845(16) 0.16388(14) 0.29880(10) 0.0156(5) Uani 1 1 d . . . . .
C33 C 0.61204(16) 0.12421(14) 0.35049(10) 0.0152(5) Uani 1 1 d . . . . .
C34 C 0.60030(17) 0.11405(14) 0.41371(11) 0.0195(5) Uani 1 1 d . . . . .
H34 H 0.5441 0.1290 0.4242 0.023 Uiso 1 1 calc R U . . .
C35 C 0.67429(17) 0.08116(15) 0.46044(11) 0.0213(5) Uani 1 1 d . . . . .
H35 H 0.6688 0.0749 0.5032 0.026 Uiso 1 1 calc R U . . .
C36 C 0.75597(17) 0.05777(14) 0.44331(11) 0.0196(5) Uani 1 1 d . . . . .
H36 H 0.8062 0.0345 0.4738 0.023 Uiso 1 1 calc R U . . .
C37 C 0.76123(16) 0.07001(14) 0.37892(10) 0.0153(5) Uani 1 1 d . . . . .
C38 C 0.85003(17) 0.00413(14) 0.30275(11) 0.0179(5) Uani 1 1 d . . . . .
H38 H 0.8011 -0.0124 0.2686 0.021 Uiso 1 1 calc R U . . .
C39 C 0.94294(17) -0.00838(14) 0.30626(11) 0.0214(5) Uani 1 1 d . . . . .
H39 H 0.9705 -0.0351 0.2754 0.026 Uiso 1 1 calc R U . . .
C40 C 0.98767(17) 0.02775(14) 0.36639(11) 0.0212(5) Uani 1 1 d . . . . .
H40 H 1.0521 0.0291 0.3816 0.025 Uiso 1 1 calc R U . . .
C41 C 1.1967(2) -0.0034(2) 0.26053(16) 0.0501(8) Uani 1 1 d . . . . .
H41A H 1.2237 0.0313 0.2985 0.075 Uiso 1 1 calc R U . . .
H41B H 1.1363 -0.0249 0.2637 0.075 Uiso 1 1 calc R U . . .
H41C H 1.1906 0.0340 0.2226 0.075 Uiso 1 1 calc R U . . .
C42 C 1.2564(2) -0.0796(2) 0.25563(13) 0.0353(7) Uani 1 1 d . . . . .
C43 C 1.0886(2) -0.13632(18) 0.08442(14) 0.0396(7) Uani 1 1 d . . . . .
H43A H 1.1438 -0.1682 0.1060 0.059 Uiso 1 1 calc R U . . .
H43B H 1.1061 -0.0806 0.0671 0.059 Uiso 1 1 calc R U . . .
H43C H 1.0539 -0.1729 0.0497 0.059 Uiso 1 1 calc R U . . .
C44 C 1.0316(2) -0.11721(17) 0.13037(13) 0.0309(6) Uani 1 1 d . . . . .
C45 C 0.4887(2) -0.12868(19) 0.40253(14) 0.0407(7) Uani 1 1 d . . . . .
H45A H 0.4434 -0.1733 0.3835 0.061 Uiso 1 1 calc R U . . .
H45B H 0.4578 -0.0726 0.4067 0.061 Uiso 1 1 calc R U . . .
H45C H 0.5218 -0.1488 0.4446 0.061 Uiso 1 1 calc R U . . .
C46 C 0.55460(19) -0.11551(16) 0.36099(12) 0.0269(6) Uani 1 1 d . . . . .
N1 N 0.77205(13) 0.28301(11) 0.32823(8) 0.0150(4) Uani 1 1 d . . . . .
N2 N 0.84304(13) 0.19744(11) 0.23944(8) 0.0125(4) Uani 1 1 d . . . . .
N3 N 0.72035(13) 0.09668(11) 0.15694(8) 0.0140(4) Uani 1 1 d . . . . .
N4 N 0.56895(13) 0.04173(11) 0.13112(8) 0.0151(4) Uani 1 1 d . . . . .
N5 N 0.48285(13) 0.05227(12) 0.09025(9) 0.0195(4) Uani 1 1 d . . . . .
N6 N 0.64008(13) 0.27621(11) 0.15708(8) 0.0144(4) Uani 1 1 d . . . . .
N7 N 0.56946(13) 0.20067(11) 0.24961(8) 0.0136(4) Uani 1 1 d . . . . .
N8 N 0.69205(13) 0.10340(11) 0.33301(8) 0.0133(4) Uani 1 1 d . . . . .
N9 N 0.84274(13) 0.04545(11) 0.35899(9) 0.0160(4) Uani 1 1 d . . . . .
N10 N 0.92818(13) 0.05979(12) 0.39915(9) 0.0191(4) Uani 1 1 d . . . . .
N11 N 1.3034(2) -0.13937(18) 0.25220(14) 0.0567(8) Uani 1 1 d . . . . .
N12 N 0.98750(19) -0.10322(17) 0.16713(12) 0.0459(7) Uani 1 1 d . . . . .
N13 N 0.60626(16) -0.10537(13) 0.32862(11) 0.0310(5) Uani 1 1 d . . . . .
O1 O 1.15990(14) 0.15966(15) 0.13769(9) 0.0474(6) Uani 1 1 d . . . . .
O2 O 1.04038(12) 0.09394(13) 0.05933(9) 0.0364(5) Uani 1 1 d . . . . .
O3 O 1.13399(15) 0.20933(12) 0.03007(10) 0.0469(5) Uani 1 1 d . . . . .
O4 O 1.19682(13) 0.06646(12) 0.05760(9) 0.0368(5) Uani 1 1 d . . . . .
O5 O 0.79902(15) 0.31207(13) -0.01889(9) 0.0466(5) Uani 1 1 d . . . . .
O6 O 0.72025(12) 0.43851(11) -0.07127(8) 0.0295(4) Uani 1 1 d . . . . .
O7 O 0.77425(12) 0.32621(11) -0.13204(8) 0.0314(4) Uani 1 1 d . . . . .
O8 O 0.88110(12) 0.42085(12) -0.06404(9) 0.0357(5) Uani 1 1 d . . . . .
Cl1 Cl 1.13254(4) 0.13254(4) 0.07092(3) 0.02442(14) Uani 1 1 d . . . . .
Cl2 Cl 0.79348(4) 0.37420(4) -0.07142(3) 0.02262(14) Uani 1 1 d . . . . .
Zn1 Zn 0.70621(2) 0.20467(2) 0.24404(2) 0.01469(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.334(3) . ?
C1 C2 1.395(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.367(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.408(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.409(3) . ?
C4 C6 1.426(3) . ?
C5 N1 1.355(3) . ?
C5 C9 1.436(3) . ?
C6 C7 1.352(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.436(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(3) . ?
C8 C10 1.409(3) . ?
C9 N2 1.345(3) . ?
C10 C11 1.375(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9300 . ?
C12 N2 1.340(3) . ?
C12 C13 1.482(3) . ?
C13 N3 1.349(3) . ?
C13 C14 1.387(3) . ?
C14 C15 1.385(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(3) . ?
C16 H16 0.9300 . ?
C17 N3 1.333(3) . ?
C17 N4 1.405(3) . ?
C18 C19 1.354(3) . ?
C18 N4 1.367(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.401(3) . ?
C19 H19 0.9300 . ?
C20 N5 1.324(3) . ?
C20 H20 0.9300 . ?
C21 N6 1.337(3) . ?
C21 C22 1.398(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.362(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.405(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.403(3) . ?
C24 C26 1.432(3) . ?
C25 N6 1.355(3) . ?
C25 C29 1.437(3) . ?
C26 C27 1.345(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.431(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.402(3) . ?
C28 C30 1.410(3) . ?
C29 N7 1.347(3) . ?
C30 C31 1.368(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.396(3) . ?
C31 H31 0.9300 . ?
C32 N7 1.341(3) . ?
C32 C33 1.475(3) . ?
C33 N8 1.346(3) . ?
C33 C34 1.393(3) . ?
C34 C35 1.383(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.374(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.392(3) . ?
C36 H36 0.9300 . ?
C37 N8 1.332(3) . ?
C37 N9 1.404(3) . ?
C38 N9 1.362(3) . ?
C38 C39 1.364(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.399(3) . ?
C39 H39 0.9300 . ?
C40 N10 1.320(3) . ?
C40 H40 0.9300 . ?
C41 C42 1.446(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 N11 1.134(4) . ?
C43 C44 1.446(4) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 N12 1.138(3) . ?
C45 C46 1.459(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 N13 1.141(3) . ?
N1 Zn1 2.1608(17) . ?
N2 Zn1 2.0387(18) . ?
N3 Zn1 2.4806(17) . ?
N4 N5 1.371(2) . ?
N6 Zn1 2.1534(18) . ?
N7 Zn1 2.0413(18) . ?
N8 Zn1 2.4489(17) . ?
N9 N10 1.365(2) . ?
O1 Cl1 1.4347(18) . ?
O2 Cl1 1.4395(18) . ?
O3 Cl1 1.4294(18) . ?
O4 Cl1 1.4307(18) . ?
O5 Cl2 1.4291(19) . ?
O6 Cl2 1.4371(17) . ?
O7 Cl2 1.4359(17) . ?
O8 Cl2 1.4385(18) . ?

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 122.5(2) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.7(2) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.8(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 116.4(2) . . ?
C3 C4 C6 124.8(2) . . ?
C5 C4 C6 118.8(2) . . ?
N1 C5 C4 123.7(2) . . ?
N1 C5 C9 117.25(19) . . ?
C4 C5 C9 119.0(2) . . ?
C7 C6 C4 122.1(2) . . ?
C7 C6 H6 118.9 . . ?
C4 C6 H6 118.9 . . ?
C6 C7 C8 120.2(2) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C10 116.9(2) . . ?
C9 C8 C7 118.9(2) . . ?
C10 C8 C7 124.2(2) . . ?
N2 C9 C8 122.71(19) . . ?
N2 C9 C5 116.7(2) . . ?
C8 C9 C5 120.6(2) . . ?
C11 C10 C8 119.9(2) . . ?
C11 C10 H10 120.1 . . ?
C8 C10 H10 120.1 . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N2 C12 C11 121.3(2) . . ?
N2 C12 C13 114.6(2) . . ?
C11 C12 C13 124.15(19) . . ?
N3 C13 C14 122.9(2) . . ?
N3 C13 C12 115.26(18) . . ?
C14 C13 C12 121.6(2) . . ?
C15 C14 C13 118.2(2) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C16 C15 C14 119.9(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 117.9(2) . . ?
C15 C16 H16 121.1 . . ?
C17 C16 H16 121.1 . . ?
N3 C17 C16 123.9(2) . . ?
N3 C17 N4 115.58(18) . . ?
C16 C17 N4 120.56(19) . . ?
C19 C18 N4 106.9(2) . . ?
C19 C18 H18 126.5 . . ?
N4 C18 H18 126.5 . . ?
C18 C19 C20 105.3(2) . . ?
C18 C19 H19 127.4 . . ?
C20 C19 H19 127.4 . . ?
N5 C20 C19 112.4(2) . . ?
N5 C20 H20 123.8 . . ?
C19 C20 H20 123.8 . . ?
N6 C21 C22 122.6(2) . . ?
N6 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 119.6(2) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 119.9(2) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 116.6(2) . . ?
C25 C24 C26 118.8(2) . . ?
C23 C24 C26 124.5(2) . . ?
N6 C25 C24 123.9(2) . . ?
N6 C25 C29 116.90(19) . . ?
C24 C25 C29 119.2(2) . . ?
C27 C26 C24 121.8(2) . . ?
C27 C26 H26 119.1 . . ?
C24 C26 H26 119.1 . . ?
C26 C27 C28 120.9(2) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C29 C28 C30 116.7(2) . . ?
C29 C28 C27 118.7(2) . . ?
C30 C28 C27 124.6(2) . . ?
N7 C29 C28 122.8(2) . . ?
N7 C29 C25 116.7(2) . . ?
C28 C29 C25 120.5(2) . . ?
C31 C30 C28 120.0(2) . . ?
C31 C30 H30 120.0 . . ?
C28 C30 H30 120.0 . . ?
C30 C31 C32 119.9(2) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
N7 C32 C31 121.0(2) . . ?
N7 C32 C33 114.5(2) . . ?
C31 C32 C33 124.5(2) . . ?
N8 C33 C34 122.9(2) . . ?
N8 C33 C32 115.38(18) . . ?
C34 C33 C32 121.6(2) . . ?
C35 C34 C33 118.4(2) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C36 C35 C34 119.6(2) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C37 118.0(2) . . ?
C35 C36 H36 121.0 . . ?
C37 C36 H36 121.0 . . ?
N8 C37 C36 124.0(2) . . ?
N8 C37 N9 116.14(18) . . ?
C36 C37 N9 119.9(2) . . ?
N9 C38 C39 106.7(2) . . ?
N9 C38 H38 126.6 . . ?
C39 C38 H38 126.6 . . ?
C38 C39 C40 104.9(2) . . ?
C38 C39 H39 127.5 . . ?
C40 C39 H39 127.5 . . ?
N10 C40 C39 112.5(2) . . ?
N10 C40 H40 123.8 . . ?
C39 C40 H40 123.8 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N11 C42 C41 179.6(4) . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N12 C44 C43 178.9(3) . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N13 C46 C45 179.8(3) . . ?
C1 N1 C5 117.8(2) . . ?
C1 N1 Zn1 129.72(16) . . ?
C5 N1 Zn1 110.63(13) . . ?
C12 N2 C9 119.59(19) . . ?
C12 N2 Zn1 124.67(15) . . ?
C9 N2 Zn1 115.72(14) . . ?
C17 N3 C13 117.19(18) . . ?
C17 N3 Zn1 124.99(14) . . ?
C13 N3 Zn1 106.03(13) . . ?
C18 N4 N5 111.58(19) . . ?
C18 N4 C17 128.65(19) . . ?
N5 N4 C17 119.76(17) . . ?
C20 N5 N4 103.76(18) . . ?
C21 N6 C25 117.41(19) . . ?
C21 N6 Zn1 130.40(16) . . ?
C25 N6 Zn1 111.54(13) . . ?
C32 N7 C29 119.57(19) . . ?
C32 N7 Zn1 124.59(15) . . ?
C29 N7 Zn1 115.84(14) . . ?
C37 N8 C33 117.14(18) . . ?
C37 N8 Zn1 127.06(15) . . ?
C33 N8 Zn1 107.55(13) . . ?
C38 N9 N10 111.72(19) . . ?
C38 N9 C37 128.16(19) . . ?
N10 N9 C37 120.09(17) . . ?
C40 N10 N9 104.13(18) . . ?
O3 Cl1 O4 108.87(11) . . ?
O3 Cl1 O1 109.45(13) . . ?
O4 Cl1 O1 109.45(13) . . ?
O3 Cl1 O2 110.71(12) . . ?
O4 Cl1 O2 109.51(11) . . ?
O1 Cl1 O2 108.84(11) . . ?
O5 Cl2 O7 109.92(12) . . ?
O5 Cl2 O6 109.60(11) . . ?
O7 Cl2 O6 109.38(11) . . ?
O5 Cl2 O8 109.33(12) . . ?
O7 Cl2 O8 108.99(10) . . ?
O6 Cl2 O8 109.61(11) . . ?
N2 Zn1 N7 175.30(7) . . ?
N2 Zn1 N6 104.24(7) . . ?
N7 Zn1 N6 78.58(7) . . ?
N2 Zn1 N1 78.66(7) . . ?
N7 Zn1 N1 103.45(7) . . ?
N6 Zn1 N1 118.16(6) . . ?
N2 Zn1 N8 105.06(6) . . ?
N7 Zn1 N8 71.52(6) . . ?
N6 Zn1 N8 148.81(6) . . ?
N1 Zn1 N8 78.19(6) . . ?
N2 Zn1 N3 71.49(6) . . ?
N7 Zn1 N3 105.80(6) . . ?
N6 Zn1 N3 77.30(6) . . ?
N1 Zn1 N3 149.24(6) . . ?
N8 Zn1 N3 102.23(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.5(3) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C2 C3 C4 C6 178.8(2) . . . . ?
C3 C4 C5 N1 2.7(3) . . . . ?
C6 C4 C5 N1 -177.88(19) . . . . ?
C3 C4 C5 C9 -175.67(18) . . . . ?
C6 C4 C5 C9 3.8(3) . . . . ?
C3 C4 C6 C7 -179.5(2) . . . . ?
C5 C4 C6 C7 1.2(3) . . . . ?
C4 C6 C7 C8 -3.4(3) . . . . ?
C6 C7 C8 C9 0.6(3) . . . . ?
C6 C7 C8 C10 -177.5(2) . . . . ?
C10 C8 C9 N2 4.5(3) . . . . ?
C7 C8 C9 N2 -173.76(18) . . . . ?
C10 C8 C9 C5 -177.41(18) . . . . ?
C7 C8 C9 C5 4.4(3) . . . . ?
N1 C5 C9 N2 -6.8(3) . . . . ?
C4 C5 C9 N2 171.69(18) . . . . ?
N1 C5 C9 C8 175.00(18) . . . . ?
C4 C5 C9 C8 -6.5(3) . . . . ?
C9 C8 C10 C11 -3.5(3) . . . . ?
C7 C8 C10 C11 174.6(2) . . . . ?
C8 C10 C11 C12 0.2(3) . . . . ?
C10 C11 C12 N2 2.4(3) . . . . ?
C10 C11 C12 C13 -177.91(19) . . . . ?
N2 C12 C13 N3 -24.0(3) . . . . ?
C11 C12 C13 N3 156.3(2) . . . . ?
N2 C12 C13 C14 150.4(2) . . . . ?
C11 C12 C13 C14 -29.3(3) . . . . ?
N3 C13 C14 C15 2.2(3) . . . . ?
C12 C13 C14 C15 -171.80(19) . . . . ?
C13 C14 C15 C16 -2.7(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C15 C16 C17 N3 2.7(3) . . . . ?
C15 C16 C17 N4 -177.76(19) . . . . ?
N4 C18 C19 C20 -0.3(2) . . . . ?
C18 C19 C20 N5 1.0(3) . . . . ?
N6 C21 C22 C23 1.6(3) . . . . ?
C21 C22 C23 C24 -0.5(3) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C22 C23 C24 C26 178.1(2) . . . . ?
C23 C24 C25 N6 1.8(3) . . . . ?
C26 C24 C25 N6 -177.43(19) . . . . ?
C23 C24 C25 C29 -178.07(18) . . . . ?
C26 C24 C25 C29 2.7(3) . . . . ?
C25 C24 C26 C27 0.3(3) . . . . ?
C23 C24 C26 C27 -178.9(2) . . . . ?
C24 C26 C27 C28 -2.3(3) . . . . ?
C26 C27 C28 C29 1.2(3) . . . . ?
C26 C27 C28 C30 -177.9(2) . . . . ?
C30 C28 C29 N7 2.3(3) . . . . ?
C27 C28 C29 N7 -176.84(19) . . . . ?
C30 C28 C29 C25 -178.99(19) . . . . ?
C27 C28 C29 C25 1.8(3) . . . . ?
N6 C25 C29 N7 -4.9(3) . . . . ?
C24 C25 C29 N7 175.00(18) . . . . ?
N6 C25 C29 C28 176.33(19) . . . . ?
C24 C25 C29 C28 -3.8(3) . . . . ?
C29 C28 C30 C31 -2.0(3) . . . . ?
C27 C28 C30 C31 177.1(2) . . . . ?
C28 C30 C31 C32 0.3(3) . . . . ?
C30 C31 C32 N7 1.5(3) . . . . ?
C30 C31 C32 C33 -178.1(2) . . . . ?
N7 C32 C33 N8 -20.8(3) . . . . ?
C31 C32 C33 N8 158.8(2) . . . . ?
N7 C32 C33 C34 155.8(2) . . . . ?
C31 C32 C33 C34 -24.6(3) . . . . ?
N8 C33 C34 C35 0.0(3) . . . . ?
C32 C33 C34 C35 -176.33(19) . . . . ?
C33 C34 C35 C36 -1.3(3) . . . . ?
C34 C35 C36 C37 1.2(3) . . . . ?
C35 C36 C37 N8 0.3(3) . . . . ?
C35 C36 C37 N9 -178.81(19) . . . . ?
N9 C38 C39 C40 -0.3(2) . . . . ?
C38 C39 C40 N10 0.8(3) . . . . ?
C2 C1 N1 C5 -0.7(3) . . . . ?
C2 C1 N1 Zn1 161.99(16) . . . . ?
C4 C5 N1 C1 -1.4(3) . . . . ?
C9 C5 N1 C1 176.94(18) . . . . ?
C4 C5 N1 Zn1 -167.31(16) . . . . ?
C9 C5 N1 Zn1 11.1(2) . . . . ?
C11 C12 N2 C9 -1.6(3) . . . . ?
C13 C12 N2 C9 178.73(17) . . . . ?
C11 C12 N2 Zn1 -179.82(15) . . . . ?
C13 C12 N2 Zn1 0.5(2) . . . . ?
C8 C9 N2 C12 -2.0(3) . . . . ?
C5 C9 N2 C12 179.82(18) . . . . ?
C8 C9 N2 Zn1 176.42(15) . . . . ?
C5 C9 N2 Zn1 -1.8(2) . . . . ?
C16 C17 N3 C13 -3.2(3) . . . . ?
N4 C17 N3 C13 177.25(17) . . . . ?
C16 C17 N3 Zn1 134.42(18) . . . . ?
N4 C17 N3 Zn1 -45.2(2) . . . . ?
C14 C13 N3 C17 0.7(3) . . . . ?
C12 C13 N3 C17 175.01(17) . . . . ?
C14 C13 N3 Zn1 -144.26(18) . . . . ?
C12 C13 N3 Zn1 30.1(2) . . . . ?
C19 C18 N4 N5 -0.5(2) . . . . ?
C19 C18 N4 C17 179.75(19) . . . . ?
N3 C17 N4 C18 -31.3(3) . . . . ?
C16 C17 N4 C18 149.1(2) . . . . ?
N3 C17 N4 N5 148.97(18) . . . . ?
C16 C17 N4 N5 -30.6(3) . . . . ?
C19 C20 N5 N4 -1.3(2) . . . . ?
C18 N4 N5 C20 1.1(2) . . . . ?
C17 N4 N5 C20 -179.13(18) . . . . ?
C22 C21 N6 C25 -0.9(3) . . . . ?
C22 C21 N6 Zn1 168.89(15) . . . . ?
C24 C25 N6 C21 -0.8(3) . . . . ?
C29 C25 N6 C21 179.07(17) . . . . ?
C24 C25 N6 Zn1 -172.51(16) . . . . ?
C29 C25 N6 Zn1 7.4(2) . . . . ?
C31 C32 N7 C29 -1.3(3) . . . . ?
C33 C32 N7 C29 178.33(18) . . . . ?
C31 C32 N7 Zn1 179.93(15) . . . . ?
C33 C32 N7 Zn1 -0.5(2) . . . . ?
C28 C29 N7 C32 -0.7(3) . . . . ?
C25 C29 N7 C32 -179.43(18) . . . . ?
C28 C29 N7 Zn1 178.21(16) . . . . ?
C25 C29 N7 Zn1 -0.5(2) . . . . ?
C36 C37 N8 C33 -1.6(3) . . . . ?
N9 C37 N8 C33 177.57(17) . . . . ?
C36 C37 N8 Zn1 142.68(18) . . . . ?
N9 C37 N8 Zn1 -38.2(2) . . . . ?
C34 C33 N8 C37 1.4(3) . . . . ?
C32 C33 N8 C37 177.97(18) . . . . ?
C34 C33 N8 Zn1 -149.35(18) . . . . ?
C32 C33 N8 Zn1 27.2(2) . . . . ?
C39 C38 N9 N10 -0.3(2) . . . . ?
C39 C38 N9 C37 -178.06(19) . . . . ?
N8 C37 N9 C38 -39.6(3) . . . . ?
C36 C37 N9 C38 139.6(2) . . . . ?
N8 C37 N9 N10 142.85(19) . . . . ?
C36 C37 N9 N10 -37.9(3) . . . . ?
C39 C40 N10 N9 -0.9(2) . . . . ?
C38 N9 N10 C40 0.7(2) . . . . ?
C37 N9 N10 C40 178.71(18) . . . . ?

_refine_diff_density_max         0.329
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.056

_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_Fe_5c
_database_code_depnum_ccdc_archive 'CCDC 1519516'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(5c)2](BF4)2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H26 Fe N6 O2, 2(B F4) [+ solvent]'
_chemical_formula_sum            'C36 H26 B2 F8 Fe N6 O2'
_chemical_formula_weight         804.10

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/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                   15.7622(6)
_cell_length_b                   12.2746(3)
_cell_length_c                   24.0938(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.441(4)
_cell_angle_gamma                90
_cell_volume                     4447.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    10685
_cell_measurement_theta_min      3.0740
_cell_measurement_theta_max      27.8260


_exptl_crystal_description       irregular
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             1632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.407
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.86451
_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            36979
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.028
_diffrn_reflns_theta_max         25.000
_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             7815
_reflns_number_gt                6235
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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)+(0.0526P)²+4.0793P] 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         7815
_refine_ls_number_parameters     543
_refine_ls_number_restraints     569
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.037
_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
C18 C 0.3919(2) 0.4264(2) 0.66462(13) 0.0437(8) Uani 1 1 d . U . . .
H1A H 0.3774 0.5011 0.6541 0.066 Uiso 1 1 calc R U . . .
H1B H 0.4553 0.4178 0.6778 0.066 Uiso 1 1 calc R U . . .
H1C H 0.3675 0.4059 0.6952 0.066 Uiso 1 1 calc R U . . .
C17 C 0.36737(18) 0.2501(2) 0.62086(12) 0.0291(6) Uani 1 1 d . U . . .
C16 C 0.41957(19) 0.1997(2) 0.67167(12) 0.0332(6) Uani 1 1 d . U . . .
H3 H 0.4481 0.2406 0.7044 0.040 Uiso 1 1 calc R U . . .
C15 C 0.42776(19) 0.0888(2) 0.67212(12) 0.0362(7) Uani 1 1 d . U . . .
H4 H 0.4621 0.0538 0.7056 0.043 Uiso 1 1 calc R U . . .
C14 C 0.38575(18) 0.0284(2) 0.62361(12) 0.0313(6) Uani 1 1 d . U . . .
H5 H 0.3914 -0.0470 0.6237 0.038 Uiso 1 1 calc R U . . .
C13 C 0.33493(17) 0.08276(19) 0.57482(11) 0.0254(5) Uani 1 1 d . U . . .
C12 C 0.28510(17) 0.0287(2) 0.52059(11) 0.0254(5) Uani 1 1 d . U . . .
C11 C 0.28004(18) -0.0828(2) 0.50752(12) 0.0306(6) Uani 1 1 d . U . . .
H8 H 0.3119 -0.1327 0.5350 0.037 Uiso 1 1 calc R U . . .
C10 C 0.22809(19) -0.1184(2) 0.45417(12) 0.0318(6) Uani 1 1 d . U . . .
H9 H 0.2253 -0.1923 0.4454 0.038 Uiso 1 1 calc R U . . .
C8 C 0.17858(18) -0.0428(2) 0.41235(12) 0.0300(6) Uani 1 1 d . U . . .
C9 C 0.18796(17) 0.0661(2) 0.42912(11) 0.0257(5) Uani 1 1 d . U . . .
C7 C 0.1205(2) -0.0656(2) 0.35568(12) 0.0359(7) Uani 1 1 d . U . . .
H12 H 0.1128 -0.1373 0.3426 0.043 Uiso 1 1 calc R U . . .
C6 C 0.0765(2) 0.0149(2) 0.32062(13) 0.0383(7) Uani 1 1 d . U . . .
H13 H 0.0375 -0.0031 0.2844 0.046 Uiso 1 1 calc R U . . .
C4 C 0.08782(19) 0.1278(2) 0.33741(12) 0.0325(6) Uani 1 1 d . U . . .
C5 C 0.14371(17) 0.1512(2) 0.39267(11) 0.0264(6) Uani 1 1 d . U . . .
C3 C 0.0475(2) 0.2167(2) 0.30287(13) 0.0410(7) Uani 1 1 d . U . . .
H16 H 0.0088 0.2059 0.2657 0.049 Uiso 1 1 calc R U . . .
C2 C 0.0663(2) 0.3195(2) 0.32509(13) 0.0406(7) Uani 1 1 d . U . . .
H17 H 0.0408 0.3793 0.3025 0.049 Uiso 1 1 calc R U . . .
C1 C 0.12308(19) 0.3356(2) 0.38100(12) 0.0332(6) Uani 1 1 d . U . . .
H18 H 0.1350 0.4065 0.3947 0.040 Uiso 1 1 calc R U . . .
C36 C 0.4509(2) 0.0863(3) 0.43034(17) 0.0545(9) Uani 1 1 d . U . . .
H19A H 0.4379 0.0106 0.4336 0.082 Uiso 1 1 calc R U . . .
H19B H 0.5104 0.1015 0.4543 0.082 Uiso 1 1 calc R U . . .
H19C H 0.4458 0.1031 0.3906 0.082 Uiso 1 1 calc R U . . .
C35 C 0.39738(19) 0.2602(2) 0.44742(12) 0.0332(6) Uani 1 1 d . U . . .
C34 C 0.4571(2) 0.3137(2) 0.42457(13) 0.0397(7) Uani 1 1 d . U . . .
H21 H 0.4952 0.2742 0.4093 0.048 Uiso 1 1 calc R U . . .
C33 C 0.4591(2) 0.4250(3) 0.42487(14) 0.0435(7) Uani 1 1 d . U . . .
H22 H 0.4979 0.4618 0.4090 0.052 Uiso 1 1 calc R U . . .
C32 C 0.4033(2) 0.4830(2) 0.44889(13) 0.0399(7) Uani 1 1 d . U . . .
H23 H 0.4046 0.5587 0.4500 0.048 Uiso 1 1 calc R U . . .
C31 C 0.34519(18) 0.4248(2) 0.47129(11) 0.0306(6) Uani 1 1 d . U . . .
C30 C 0.28278(19) 0.4757(2) 0.49762(11) 0.0306(6) Uani 1 1 d . U . . .
C29 C 0.2736(2) 0.5857(2) 0.51072(13) 0.0384(7) Uani 1 1 d . U . . .
H26 H 0.3112 0.6377 0.5027 0.046 Uiso 1 1 calc R U . . .
C28 C 0.2099(2) 0.6165(2) 0.53510(14) 0.0476(8) Uani 1 1 d . U . . .
H27 H 0.2047 0.6893 0.5442 0.057 Uiso 1 1 calc R U . . .
C26 C 0.1510(2) 0.5376(2) 0.54686(13) 0.0427(7) Uani 1 1 d . U . . .
C27 C 0.16636(19) 0.4304(2) 0.53366(12) 0.0327(6) Uani 1 1 d . U . . .
C25 C 0.0803(3) 0.5559(3) 0.57076(17) 0.0608(10) Uani 1 1 d . U . . .
H30 H 0.0678 0.6266 0.5797 0.073 Uiso 1 1 calc R U . . .
C24 C 0.0308(3) 0.4731(3) 0.58080(17) 0.0610(10) Uani 1 1 d . U . . .
H31 H -0.0150 0.4885 0.5965 0.073 Uiso 1 1 calc R U . . .
C22 C 0.0463(2) 0.3612(2) 0.56809(14) 0.0429(7) Uani 1 1 d . U . . .
C23 C 0.11538(19) 0.3419(2) 0.54413(12) 0.0327(6) Uani 1 1 d . U . . .
C21 C -0.0008(2) 0.2709(3) 0.57784(15) 0.0484(8) Uani 1 1 d . U . . .
H34 H -0.0472 0.2791 0.5939 0.058 Uiso 1 1 calc R U . . .
C20 C 0.0226(2) 0.1694(3) 0.56332(14) 0.0418(7) Uani 1 1 d . U . . .
H35 H -0.0082 0.1083 0.5696 0.050 Uiso 1 1 calc R U . . .
C19 C 0.09216(18) 0.1574(2) 0.53923(12) 0.0330(6) Uani 1 1 d . U . . .
H36 H 0.1065 0.0877 0.5298 0.040 Uiso 1 1 calc R U . . .
N3 N 0.32467(14) 0.19413(16) 0.57285(9) 0.0260(5) Uani 1 1 d . U . . .
N2 N 0.24049(14) 0.10056(16) 0.48151(9) 0.0245(5) Uani 1 1 d . U . . .
N1 N 0.16079(14) 0.25396(16) 0.41544(9) 0.0271(5) Uani 1 1 d . U . . .
N6 N 0.34108(14) 0.31349(17) 0.46975(9) 0.0282(5) Uani 1 1 d . U . . .
N5 N 0.23031(15) 0.40051(17) 0.51030(9) 0.0289(5) Uani 1 1 d . U . . .
N4 N 0.13896(15) 0.24123(17) 0.52916(10) 0.0293(5) Uani 1 1 d . U . . .
O1 O 0.38869(13) 0.15203(15) 0.44929(9) 0.0391(5) Uani 1 1 d . U . . .
O2 O 0.35490(13) 0.35779(14) 0.61464(8) 0.0358(5) Uani 1 1 d . U . . .
F1 F -0.18242(14) 0.14055(18) 0.11587(8) 0.0676(6) Uani 1 1 d . U . . .
F2 F -0.06146(12) 0.07757(15) 0.18332(8) 0.0533(5) Uani 1 1 d . U . . .
F3 F -0.19820(15) 0.03104(16) 0.18703(10) 0.0687(6) Uani 1 1 d . U . . .
F4 F -0.14835(12) 0.20387(14) 0.20775(9) 0.0547(5) Uani 1 1 d . U . . .
B2 B 0.4174(11) 0.7432(13) 0.1845(8) 0.054(4) Uani 0.343(6) 1 d D U P A 1
F5 F 0.4921(5) 0.6792(5) 0.1945(3) 0.054(2) Uani 0.343(6) 1 d D U P A 1
F6 F 0.3617(8) 0.6941(9) 0.2115(4) 0.122(4) Uani 0.343(6) 1 d D U P A 1
F7 F 0.3682(16) 0.750(2) 0.1263(7) 0.060(6) Uani 0.343(6) 1 d D U P A 1
F8 F 0.4342(7) 0.8437(6) 0.2097(3) 0.078(3) Uani 0.343(6) 1 d D U P A 1
B2' B 0.4064(6) 0.7638(6) 0.1816(4) 0.0429(19) Uani 0.657(6) 1 d D U P A 2
F5' F 0.4339(3) 0.6703(2) 0.21356(13) 0.0665(16) Uani 0.657(6) 1 d D U P A 2
F6' F 0.3375(3) 0.8125(3) 0.19569(19) 0.0931(17) Uani 0.657(6) 1 d D U P A 2
F7' F 0.3811(7) 0.7380(9) 0.1225(3) 0.0377(14) Uani 0.657(6) 1 d D U P A 2
F8' F 0.4772(3) 0.8389(3) 0.19071(16) 0.0517(10) Uani 0.657(6) 1 d D U P A 2
Fe1 Fe 0.24140(2) 0.25073(3) 0.49690(2) 0.02392(11) Uani 1 1 d . U . . .
B1 B -0.1486(2) 0.1121(3) 0.17335(15) 0.0385(8) 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
C18 O2 1.441(3) . ?
C18 H1A 0.9600 . ?
C18 H1B 0.9600 . ?
C18 H1C 0.9600 . ?
C17 O2 1.338(3) . ?
C17 N3 1.340(3) . ?
C17 C16 1.398(4) . ?
C16 C15 1.367(4) . ?
C16 H3 0.9300 . ?
C15 C14 1.374(4) . ?
C15 H4 0.9300 . ?
C14 C13 1.380(4) . ?
C14 H5 0.9300 . ?
C13 N3 1.376(3) . ?
C13 C12 1.466(4) . ?
C12 N2 1.327(3) . ?
C12 C11 1.402(4) . ?
C11 C10 1.372(4) . ?
C11 H8 0.9300 . ?
C10 C8 1.419(4) . ?
C10 H9 0.9300 . ?
C8 C9 1.391(4) . ?
C8 C7 1.425(4) . ?
C9 N2 1.353(3) . ?
C9 C5 1.408(4) . ?
C7 C6 1.349(4) . ?
C7 H12 0.9300 . ?
C6 C4 1.440(4) . ?
C6 H13 0.9300 . ?
C4 C5 1.389(4) . ?
C4 C3 1.403(4) . ?
C5 N1 1.370(3) . ?
C3 C2 1.369(4) . ?
C3 H16 0.9300 . ?
C2 C1 1.390(4) . ?
C2 H17 0.9300 . ?
C1 N1 1.323(3) . ?
C1 H18 0.9300 . ?
C36 O1 1.446(3) . ?
C36 H19A 0.9600 . ?
C36 H19B 0.9600 . ?
C36 H19C 0.9600 . ?
C35 O1 1.337(3) . ?
C35 N6 1.338(3) . ?
C35 C34 1.389(4) . ?
C34 C33 1.367(4) . ?
C34 H21 0.9300 . ?
C33 C32 1.387(4) . ?
C33 H22 0.9300 . ?
C32 C31 1.391(4) . ?
C32 H23 0.9300 . ?
C31 N6 1.368(3) . ?
C31 C30 1.461(4) . ?
C30 N5 1.334(3) . ?
C30 C29 1.404(4) . ?
C29 C28 1.360(4) . ?
C29 H26 0.9300 . ?
C28 C26 1.427(4) . ?
C28 H27 0.9300 . ?
C26 C27 1.393(4) . ?
C26 C25 1.417(5) . ?
C27 N5 1.344(4) . ?
C27 C23 1.418(4) . ?
C25 C24 1.347(5) . ?
C25 H30 0.9300 . ?
C24 C22 1.444(4) . ?
C24 H31 0.9300 . ?
C22 C21 1.392(4) . ?
C22 C23 1.397(4) . ?
C23 N4 1.370(3) . ?
C21 C20 1.374(4) . ?
C21 H34 0.9300 . ?
C20 C19 1.393(4) . ?
C20 H35 0.9300 . ?
C19 N4 1.330(3) . ?
C19 H36 0.9300 . ?
N3 Fe1 2.028(2) . ?
N2 Fe1 1.879(2) . ?
N1 Fe1 1.993(2) . ?
N6 Fe1 2.026(2) . ?
N5 Fe1 1.884(2) . ?
N4 Fe1 1.994(2) . ?
F1 B1 1.372(4) . ?
F2 B1 1.388(4) . ?
F3 B1 1.365(4) . ?
F4 B1 1.398(4) . ?
B2 F8 1.366(16) . ?
B2 F5 1.376(15) . ?
B2 F6 1.378(17) . ?
B2 F7 1.385(17) . ?
B2' F6' 1.369(9) . ?
B2' F5' 1.378(8) . ?
B2' F7' 1.395(10) . ?
B2' F8' 1.413(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C18 H1A 109.5 . . ?
O2 C18 H1B 109.5 . . ?
H1A C18 H1B 109.5 . . ?
O2 C18 H1C 109.5 . . ?
H1A C18 H1C 109.5 . . ?
H1B C18 H1C 109.5 . . ?
O2 C17 N3 113.0(2) . . ?
O2 C17 C16 124.3(2) . . ?
N3 C17 C16 122.7(2) . . ?
C15 C16 C17 118.5(3) . . ?
C15 C16 H3 120.7 . . ?
C17 C16 H3 120.7 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H4 119.7 . . ?
C14 C15 H4 119.7 . . ?
C15 C14 C13 118.2(2) . . ?
C15 C14 H5 120.9 . . ?
C13 C14 H5 120.9 . . ?
N3 C13 C14 122.8(2) . . ?
N3 C13 C12 113.1(2) . . ?
C14 C13 C12 124.1(2) . . ?
N2 C12 C11 120.5(2) . . ?
N2 C12 C13 111.1(2) . . ?
C11 C12 C13 128.4(2) . . ?
C10 C11 C12 119.9(2) . . ?
C10 C11 H8 120.0 . . ?
C12 C11 H8 120.0 . . ?
C11 C10 C8 120.3(2) . . ?
C11 C10 H9 119.9 . . ?
C8 C10 H9 119.9 . . ?
C9 C8 C10 115.7(2) . . ?
C9 C8 C7 116.7(2) . . ?
C10 C8 C7 127.6(2) . . ?
N2 C9 C8 123.6(2) . . ?
N2 C9 C5 113.6(2) . . ?
C8 C9 C5 122.8(2) . . ?
C6 C7 C8 121.2(3) . . ?
C6 C7 H12 119.4 . . ?
C8 C7 H12 119.4 . . ?
C7 C6 C4 122.1(3) . . ?
C7 C6 H13 118.9 . . ?
C4 C6 H13 118.9 . . ?
C5 C4 C3 116.9(2) . . ?
C5 C4 C6 117.3(2) . . ?
C3 C4 C6 125.8(3) . . ?
N1 C5 C4 124.5(2) . . ?
N1 C5 C9 115.6(2) . . ?
C4 C5 C9 119.9(2) . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 H16 120.7 . . ?
C4 C3 H16 120.7 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H17 119.6 . . ?
C1 C2 H17 119.6 . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H18 118.7 . . ?
C2 C1 H18 118.7 . . ?
O1 C36 H19A 109.5 . . ?
O1 C36 H19B 109.5 . . ?
H19A C36 H19B 109.5 . . ?
O1 C36 H19C 109.5 . . ?
H19A C36 H19C 109.5 . . ?
H19B C36 H19C 109.5 . . ?
O1 C35 N6 112.6(2) . . ?
O1 C35 C34 124.8(3) . . ?
N6 C35 C34 122.6(3) . . ?
C33 C34 C35 119.2(3) . . ?
C33 C34 H21 120.4 . . ?
C35 C34 H21 120.4 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H22 120.0 . . ?
C32 C33 H22 120.0 . . ?
C33 C32 C31 118.2(3) . . ?
C33 C32 H23 120.9 . . ?
C31 C32 H23 120.9 . . ?
N6 C31 C32 122.2(3) . . ?
N6 C31 C30 114.0(2) . . ?
C32 C31 C30 123.8(3) . . ?
N5 C30 C29 120.0(3) . . ?
N5 C30 C31 110.4(2) . . ?
C29 C30 C31 129.6(3) . . ?
C28 C29 C30 120.3(3) . . ?
C28 C29 H26 119.9 . . ?
C30 C29 H26 119.9 . . ?
C29 C28 C26 120.3(3) . . ?
C29 C28 H27 119.8 . . ?
C26 C28 H27 119.8 . . ?
C27 C26 C25 117.0(3) . . ?
C27 C26 C28 115.4(3) . . ?
C25 C26 C28 127.7(3) . . ?
N5 C27 C26 123.8(3) . . ?
N5 C27 C23 113.7(2) . . ?
C26 C27 C23 122.5(3) . . ?
C24 C25 C26 121.5(3) . . ?
C24 C25 H30 119.3 . . ?
C26 C25 H30 119.3 . . ?
C25 C24 C22 122.5(3) . . ?
C25 C24 H31 118.8 . . ?
C22 C24 H31 118.8 . . ?
C21 C22 C23 117.1(3) . . ?
C21 C22 C24 126.1(3) . . ?
C23 C22 C24 116.8(3) . . ?
N4 C23 C22 124.6(3) . . ?
N4 C23 C27 115.5(2) . . ?
C22 C23 C27 119.8(2) . . ?
C20 C21 C22 118.8(3) . . ?
C20 C21 H34 120.6 . . ?
C22 C21 H34 120.6 . . ?
C21 C20 C19 120.4(3) . . ?
C21 C20 H35 119.8 . . ?
C19 C20 H35 119.8 . . ?
N4 C19 C20 122.9(3) . . ?
N4 C19 H36 118.6 . . ?
C20 C19 H36 118.6 . . ?
C17 N3 C13 117.1(2) . . ?
C17 N3 Fe1 128.67(17) . . ?
C13 N3 Fe1 114.15(17) . . ?
C12 N2 C9 120.0(2) . . ?
C12 N2 Fe1 122.72(18) . . ?
C9 N2 Fe1 117.21(17) . . ?
C1 N1 C5 116.7(2) . . ?
C1 N1 Fe1 131.82(18) . . ?
C5 N1 Fe1 111.52(16) . . ?
C35 N6 C31 117.9(2) . . ?
C35 N6 Fe1 128.01(18) . . ?
C31 N6 Fe1 113.96(18) . . ?
C30 N5 C27 120.1(2) . . ?
C30 N5 Fe1 122.68(19) . . ?
C27 N5 Fe1 117.22(18) . . ?
C19 N4 C23 116.2(2) . . ?
C19 N4 Fe1 132.40(18) . . ?
C23 N4 Fe1 111.43(18) . . ?
C35 O1 C36 117.2(2) . . ?
C17 O2 C18 118.3(2) . . ?
F8 B2 F5 113.3(13) . . ?
F8 B2 F6 104.5(13) . . ?
F5 B2 F6 107.5(14) . . ?
F8 B2 F7 111.7(16) . . ?
F5 B2 F7 113.7(16) . . ?
F6 B2 F7 105.2(16) . . ?
F6' B2' F5' 111.4(7) . . ?
F6' B2' F7' 110.3(8) . . ?
F5' B2' F7' 109.1(7) . . ?
F6' B2' F8' 108.9(6) . . ?
F5' B2' F8' 110.8(6) . . ?
F7' B2' F8' 106.1(7) . . ?
N2 Fe1 N5 174.50(10) . . ?
N2 Fe1 N1 81.97(9) . . ?
N5 Fe1 N1 94.86(9) . . ?
N2 Fe1 N4 93.46(9) . . ?
N5 Fe1 N4 82.11(9) . . ?
N1 Fe1 N4 91.91(9) . . ?
N2 Fe1 N6 105.67(9) . . ?
N5 Fe1 N6 78.75(9) . . ?
N1 Fe1 N6 90.09(9) . . ?
N4 Fe1 N6 160.86(9) . . ?
N2 Fe1 N3 78.85(9) . . ?
N5 Fe1 N3 104.35(9) . . ?
N1 Fe1 N3 160.79(8) . . ?
N4 Fe1 N3 90.51(9) . . ?
N6 Fe1 N3 93.83(9) . . ?
F3 B1 F1 110.6(3) . . ?
F3 B1 F2 110.1(3) . . ?
F1 B1 F2 108.5(3) . . ?
F3 B1 F4 110.1(3) . . ?
F1 B1 F4 109.0(3) . . ?
F2 B1 F4 108.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C17 C16 C15 -179.2(3) . . . . ?
N3 C17 C16 C15 0.5(4) . . . . ?
C17 C16 C15 C14 0.2(4) . . . . ?
C16 C15 C14 C13 -0.4(4) . . . . ?
C15 C14 C13 N3 -0.1(4) . . . . ?
C15 C14 C13 C12 -178.7(3) . . . . ?
N3 C13 C12 N2 -0.3(3) . . . . ?
C14 C13 C12 N2 178.4(2) . . . . ?
N3 C13 C12 C11 -179.7(3) . . . . ?
C14 C13 C12 C11 -0.9(4) . . . . ?
N2 C12 C11 C10 -0.5(4) . . . . ?
C13 C12 C11 C10 178.8(3) . . . . ?
C12 C11 C10 C8 -0.7(4) . . . . ?
C11 C10 C8 C9 0.9(4) . . . . ?
C11 C10 C8 C7 -178.8(3) . . . . ?
C10 C8 C9 N2 0.2(4) . . . . ?
C7 C8 C9 N2 179.9(2) . . . . ?
C10 C8 C9 C5 179.8(2) . . . . ?
C7 C8 C9 C5 -0.5(4) . . . . ?
C9 C8 C7 C6 -0.6(4) . . . . ?
C10 C8 C7 C6 179.1(3) . . . . ?
C8 C7 C6 C4 2.2(5) . . . . ?
C7 C6 C4 C5 -2.6(4) . . . . ?
C7 C6 C4 C3 177.4(3) . . . . ?
C3 C4 C5 N1 0.8(4) . . . . ?
C6 C4 C5 N1 -179.3(3) . . . . ?
C3 C4 C5 C9 -178.5(3) . . . . ?
C6 C4 C5 C9 1.4(4) . . . . ?
N2 C9 C5 N1 0.3(3) . . . . ?
C8 C9 C5 N1 -179.3(2) . . . . ?
N2 C9 C5 C4 179.7(2) . . . . ?
C8 C9 C5 C4 0.1(4) . . . . ?
C5 C4 C3 C2 0.9(4) . . . . ?
C6 C4 C3 C2 -179.1(3) . . . . ?
C4 C3 C2 C1 -1.0(5) . . . . ?
C3 C2 C1 N1 -0.6(5) . . . . ?
O1 C35 C34 C33 179.6(3) . . . . ?
N6 C35 C34 C33 0.2(5) . . . . ?
C35 C34 C33 C32 1.3(5) . . . . ?
C34 C33 C32 C31 -1.1(5) . . . . ?
C33 C32 C31 N6 -0.7(4) . . . . ?
C33 C32 C31 C30 -179.8(3) . . . . ?
N6 C31 C30 N5 -4.9(3) . . . . ?
C32 C31 C30 N5 174.3(3) . . . . ?
N6 C31 C30 C29 174.2(3) . . . . ?
C32 C31 C30 C29 -6.6(5) . . . . ?
N5 C30 C29 C28 -1.5(4) . . . . ?
C31 C30 C29 C28 179.5(3) . . . . ?
C30 C29 C28 C26 -0.9(5) . . . . ?
C29 C28 C26 C27 2.2(5) . . . . ?
C29 C28 C26 C25 -178.5(3) . . . . ?
C25 C26 C27 N5 179.3(3) . . . . ?
C28 C26 C27 N5 -1.4(4) . . . . ?
C25 C26 C27 C23 -1.0(5) . . . . ?
C28 C26 C27 C23 178.3(3) . . . . ?
C27 C26 C25 C24 0.7(6) . . . . ?
C28 C26 C25 C24 -178.5(4) . . . . ?
C26 C25 C24 C22 0.0(6) . . . . ?
C25 C24 C22 C21 179.1(4) . . . . ?
C25 C24 C22 C23 -0.5(6) . . . . ?
C21 C22 C23 N4 0.8(5) . . . . ?
C24 C22 C23 N4 -179.7(3) . . . . ?
C21 C22 C23 C27 -179.4(3) . . . . ?
C24 C22 C23 C27 0.2(5) . . . . ?
N5 C27 C23 N4 0.1(4) . . . . ?
C26 C27 C23 N4 -179.6(3) . . . . ?
N5 C27 C23 C22 -179.7(3) . . . . ?
C26 C27 C23 C22 0.6(5) . . . . ?
C23 C22 C21 C20 -0.3(5) . . . . ?
C24 C22 C21 C20 -179.9(3) . . . . ?
C22 C21 C20 C19 -0.1(5) . . . . ?
C21 C20 C19 N4 0.1(5) . . . . ?
O2 C17 N3 C13 178.9(2) . . . . ?
C16 C17 N3 C13 -0.9(4) . . . . ?
O2 C17 N3 Fe1 -3.7(3) . . . . ?
C16 C17 N3 Fe1 176.5(2) . . . . ?
C14 C13 N3 C17 0.7(4) . . . . ?
C12 C13 N3 C17 179.4(2) . . . . ?
C14 C13 N3 Fe1 -177.1(2) . . . . ?
C12 C13 N3 Fe1 1.6(3) . . . . ?
C11 C12 N2 C9 1.6(4) . . . . ?
C13 C12 N2 C9 -177.8(2) . . . . ?
C11 C12 N2 Fe1 178.04(19) . . . . ?
C13 C12 N2 Fe1 -1.4(3) . . . . ?
C8 C9 N2 C12 -1.4(4) . . . . ?
C5 C9 N2 C12 178.9(2) . . . . ?
C8 C9 N2 Fe1 -178.1(2) . . . . ?
C5 C9 N2 Fe1 2.3(3) . . . . ?
C2 C1 N1 C5 2.2(4) . . . . ?
C2 C1 N1 Fe1 -178.4(2) . . . . ?
C4 C5 N1 C1 -2.3(4) . . . . ?
C9 C5 N1 C1 177.1(2) . . . . ?
C4 C5 N1 Fe1 178.1(2) . . . . ?
C9 C5 N1 Fe1 -2.5(3) . . . . ?
O1 C35 N6 C31 178.7(2) . . . . ?
C34 C35 N6 C31 -1.9(4) . . . . ?
O1 C35 N6 Fe1 -6.5(3) . . . . ?
C34 C35 N6 Fe1 172.9(2) . . . . ?
C32 C31 N6 C35 2.1(4) . . . . ?
C30 C31 N6 C35 -178.6(2) . . . . ?
C32 C31 N6 Fe1 -173.4(2) . . . . ?
C30 C31 N6 Fe1 5.8(3) . . . . ?
C29 C30 N5 C27 2.4(4) . . . . ?
C31 C30 N5 C27 -178.4(2) . . . . ?
C29 C30 N5 Fe1 -177.5(2) . . . . ?
C31 C30 N5 Fe1 1.7(3) . . . . ?
C26 C27 N5 C30 -1.0(4) . . . . ?
C23 C27 N5 C30 179.3(2) . . . . ?
C26 C27 N5 Fe1 179.0(2) . . . . ?
C23 C27 N5 Fe1 -0.7(3) . . . . ?
C20 C19 N4 C23 0.3(4) . . . . ?
C20 C19 N4 Fe1 179.0(2) . . . . ?
C22 C23 N4 C19 -0.7(4) . . . . ?
C27 C23 N4 C19 179.4(2) . . . . ?
C22 C23 N4 Fe1 -179.7(2) . . . . ?
C27 C23 N4 Fe1 0.5(3) . . . . ?
N6 C35 O1 C36 -175.4(3) . . . . ?
C34 C35 O1 C36 5.2(4) . . . . ?
N3 C17 O2 C18 175.4(2) . . . . ?
C16 C17 O2 C18 -4.9(4) . . . . ?
C12 N2 Fe1 N1 -179.5(2) . . . . ?
C9 N2 Fe1 N1 -2.92(18) . . . . ?
C12 N2 Fe1 N4 -88.0(2) . . . . ?
C9 N2 Fe1 N4 88.53(19) . . . . ?
C12 N2 Fe1 N6 92.7(2) . . . . ?
C9 N2 Fe1 N6 -90.75(19) . . . . ?
C12 N2 Fe1 N3 1.8(2) . . . . ?
C9 N2 Fe1 N3 178.4(2) . . . . ?
C30 N5 Fe1 N1 -88.0(2) . . . . ?
C27 N5 Fe1 N1 92.0(2) . . . . ?
C30 N5 Fe1 N4 -179.3(2) . . . . ?
C27 N5 Fe1 N4 0.8(2) . . . . ?
C30 N5 Fe1 N6 1.1(2) . . . . ?
C27 N5 Fe1 N6 -178.8(2) . . . . ?
C30 N5 Fe1 N3 92.2(2) . . . . ?
C27 N5 Fe1 N3 -87.7(2) . . . . ?

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.051

_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_Fe_5a
_database_code_depnum_ccdc_archive 'CCDC 1519515'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            '[Fe(5a)2](BF4)2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H22 Fe N6, 2(C2 H3 N), 2(B F4)'
_chemical_formula_sum            'C38 H28 B2 F8 Fe N8'
_chemical_formula_weight         826.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5432(5)
_cell_length_b                   11.9637(9)
_cell_length_c                   14.2066(10)
_cell_angle_alpha                90.196(6)
_cell_angle_beta                 95.816(5)
_cell_angle_gamma                113.065(6)
_cell_volume                     1793.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    101(2)
_cell_measurement_reflns_used    5094
_cell_measurement_theta_min      2.8798
_cell_measurement_theta_max      28.5155

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.505
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76563
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      101(2)
_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            14152
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.886
_diffrn_reflns_theta_max         28.578
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.834
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7643
_reflns_number_gt                6297
_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-2014/6 (Sheldrick, 2014)'
_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)+(0.0839P)²+3.0835P] 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         7643
_refine_ls_number_parameters     606
_refine_ls_number_restraints     493
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.1883
_refine_ls_wR_factor_gt          0.1780
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.098
_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 0.6757(4) 0.0772(3) 0.3263(3) 0.0354(8) Uani 1 1 d . . . . .
H1 H 0.6256 0.0792 0.2713 0.042 Uiso 1 1 calc R U . . .
C2 C 0.6170(4) 0.0159(4) 0.4034(3) 0.0422(9) Uani 1 1 d . . . . .
H2 H 0.5290 -0.0208 0.3990 0.051 Uiso 1 1 calc R U . . .
C3 C 0.6867(4) 0.0091(4) 0.4847(3) 0.0414(9) Uani 1 1 d . . . . .
H3 H 0.6471 -0.0335 0.5349 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8193(4) 0.0674(3) 0.4917(3) 0.0344(8) Uani 1 1 d . . . . .
C5 C 0.8702(3) 0.1269(3) 0.4117(2) 0.0294(7) Uani 1 1 d . . . . .
C6 C 0.9075(4) 0.0730(4) 0.5725(3) 0.0409(9) Uani 1 1 d . . . . .
H6 H 0.8758 0.0338 0.6264 0.049 Uiso 1 1 calc R U . . .
C7 C 1.0344(4) 0.1328(4) 0.5737(3) 0.0400(9) Uani 1 1 d . . . . .
H7 H 1.0874 0.1332 0.6277 0.048 Uiso 1 1 calc R U . . .
C8 C 1.0883(4) 0.1955(3) 0.4927(2) 0.0325(7) Uani 1 1 d . . . . .
C9 C 1.0031(3) 0.1902(3) 0.4144(2) 0.0286(7) Uani 1 1 d . . . . .
C10 C 1.2179(4) 0.2631(4) 0.4838(3) 0.0393(9) Uani 1 1 d . . . . .
H10 H 1.2792 0.2688 0.5335 0.047 Uiso 1 1 calc R U . . .
C11 C 1.2531(4) 0.3206(4) 0.4011(3) 0.0388(8) Uani 1 1 d . . . . .
H11 H 1.3382 0.3658 0.3953 0.047 Uiso 1 1 calc R U . . .
C12 C 1.1611(3) 0.3111(3) 0.3258(3) 0.0310(7) Uani 1 1 d . . . . .
C13 C 1.1768(3) 0.3648(3) 0.2332(3) 0.0328(7) Uani 1 1 d . . . . .
C14 C 1.2910(4) 0.4404(4) 0.2035(3) 0.0423(9) Uani 1 1 d . . . . .
H14 H 1.3662 0.4615 0.2434 0.051 Uiso 1 1 calc R U . . .
C15 C 1.2912(4) 0.4835(4) 0.1139(3) 0.0477(10) Uani 1 1 d . . . . .
H15 H 1.3668 0.5351 0.0927 0.057 Uiso 1 1 calc R U . . .
C16 C 1.1791(4) 0.4502(4) 0.0558(3) 0.0419(9) Uani 1 1 d . . . . .
H16 H 1.1785 0.4782 -0.0052 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0680(4) 0.3750(3) 0.0887(3) 0.0336(8) Uani 1 1 d . . . . .
H17 H 0.9926 0.3529 0.0490 0.040 Uiso 1 1 calc R U . . .
C18 C 0.9356(4) 0.4633(3) 0.3344(2) 0.0334(8) Uani 1 1 d . . . . .
H18 H 1.0022 0.4601 0.3756 0.040 Uiso 1 1 calc R U . . .
C19 C 0.8987(4) 0.5607(4) 0.3451(3) 0.0439(9) Uani 1 1 d . . . . .
H19 H 0.9420 0.6214 0.3919 0.053 Uiso 1 1 calc R U . . .
C20 C 0.8002(4) 0.5671(4) 0.2878(3) 0.0479(10) Uani 1 1 d . . . . .
H20 H 0.7750 0.6311 0.2960 0.057 Uiso 1 1 calc R U . . .
C21 C 0.7372(4) 0.4774(4) 0.2168(3) 0.0401(9) Uani 1 1 d . . . . .
C22 C 0.7806(3) 0.3836(3) 0.2091(2) 0.0300(7) Uani 1 1 d . . . . .
C23 C 0.6290(4) 0.4671(5) 0.1487(4) 0.0560(12) Uani 1 1 d . . . . .
H23 H 0.5941 0.5247 0.1532 0.067 Uiso 1 1 calc R U . . .
C24 C 0.5778(4) 0.3790(5) 0.0801(3) 0.0559(13) Uani 1 1 d . . . . .
H24 H 0.5087 0.3771 0.0393 0.067 Uiso 1 1 calc R U . . .
C25 C 0.6283(3) 0.2859(4) 0.0682(3) 0.0401(9) Uani 1 1 d . . . . .
C26 C 0.7271(3) 0.2921(3) 0.1352(2) 0.0308(7) Uani 1 1 d . . . . .
C27 C 0.5900(4) 0.1940(4) -0.0029(3) 0.0470(10) Uani 1 1 d . U . . .
H27 H 0.5257 0.1879 -0.0503 0.056 Uiso 1 1 calc R U . . .
C28 C 0.6476(4) 0.1120(4) -0.0029(3) 0.0483(10) Uani 1 1 d . U . . .
H28 H 0.6231 0.0513 -0.0508 0.058 Uiso 1 1 calc R U . . .
C29 C 0.7439(4) 0.1209(4) 0.0701(3) 0.0387(9) Uani 1 1 d . . . . .
C30 C 0.8142(4) 0.0443(3) 0.0868(3) 0.0412(9) Uani 1 1 d . . . . .
C31 C 0.7945(5) -0.0571(4) 0.0292(3) 0.0551(12) Uani 1 1 d . . . . .
H31 H 0.7343 -0.0797 -0.0236 0.066 Uiso 1 1 calc R U . . .
C32 C 0.8663(5) -0.1224(4) 0.0526(4) 0.0624(14) Uani 1 1 d . . . . .
H32 H 0.8531 -0.1922 0.0165 0.075 Uiso 1 1 calc R U . . .
C33 C 0.9578(5) -0.0861(4) 0.1290(4) 0.0597(13) Uani 1 1 d . . . . .
H33 H 1.0079 -0.1298 0.1437 0.072 Uiso 1 1 calc R U . . .
C34 C 0.9750(4) 0.0178(4) 0.1848(3) 0.0449(10) Uani 1 1 d . . . . .
H34 H 1.0369 0.0428 0.2365 0.054 Uiso 1 1 calc R U . . .
C35 C 0.1309(5) 0.6988(4) 0.1817(3) 0.0484(10) Uani 1 1 d . . . . .
C36 C 0.2415(6) 0.7652(7) 0.2464(4) 0.0864(19) Uani 1 1 d . . . . .
H36A H 0.2238 0.7440 0.3101 0.130 Uiso 1 1 calc R U . . .
H36B H 0.2640 0.8509 0.2407 0.130 Uiso 1 1 calc R U . . .
H36C H 0.3105 0.7449 0.2317 0.130 Uiso 1 1 calc R U . . .
C37 C 0.2831(5) 0.6479(5) 0.4934(3) 0.0601(13) Uani 1 1 d . . . . .
C38 C 0.4039(6) 0.6379(7) 0.5228(5) 0.099(2) Uani 1 1 d . . . . .
H38A H 0.3880 0.5596 0.5481 0.149 Uiso 1 1 calc R U . . .
H38B H 0.4522 0.7003 0.5705 0.149 Uiso 1 1 calc R U . . .
H38C H 0.4506 0.6472 0.4692 0.149 Uiso 1 1 calc R U . . .
N1 N 0.8009(3) 0.1327(3) 0.3295(2) 0.0287(6) Uani 1 1 d . . . . .
N2 N 1.0390(3) 0.2457(3) 0.3334(2) 0.0295(6) Uani 1 1 d . . . . .
N3 N 1.0647(3) 0.3325(3) 0.1757(2) 0.0298(6) Uani 1 1 d . . . . .
N4 N 0.8792(3) 0.3757(3) 0.26778(19) 0.0277(6) Uani 1 1 d . . . . .
N5 N 0.7829(3) 0.2122(3) 0.1364(2) 0.0303(6) Uani 1 1 d . . . . .
N6 N 0.9030(3) 0.0811(3) 0.1641(2) 0.0362(7) Uani 1 1 d . . . . .
N7 N 0.0458(5) 0.6471(4) 0.1304(3) 0.0642(11) Uani 1 1 d . . . . .
N8 N 0.1868(5) 0.6502(4) 0.4759(3) 0.0612(11) Uani 1 1 d . . . . .
Fe1 Fe 0.91217(4) 0.22932(4) 0.23435(3) 0.02634(16) Uani 1 1 d . . . . .
B1 B 0.6284(9) 0.8590(9) 0.7648(6) 0.0511(17) Uani 0.591(7) 1 d D U P A 1
F1 F 0.5776(8) 0.9218(9) 0.8174(6) 0.067(2) Uani 0.591(7) 1 d D U P A 1
F2 F 0.5391(6) 0.7567(7) 0.7213(5) 0.106(2) Uani 0.591(7) 1 d D U P A 1
F3 F 0.7029(8) 0.8181(8) 0.8256(6) 0.099(2) Uani 0.591(7) 1 d D U P A 1
F4 F 0.7005(9) 0.9302(8) 0.7026(5) 0.139(3) Uani 0.591(7) 1 d D U P A 1
B1' B 0.6390(12) 0.8753(13) 0.7621(9) 0.065(2) Uani 0.409(7) 1 d D U P A 2
F1' F 0.5676(14) 0.9089(15) 0.8144(10) 0.087(3) Uani 0.409(7) 1 d D U P A 2
F2' F 0.5866(8) 0.8561(11) 0.6736(6) 0.096(3) Uani 0.409(7) 1 d D U P A 2
F3' F 0.6560(14) 0.7820(12) 0.7979(11) 0.128(3) Uani 0.409(7) 1 d D U P A 2
F4' F 0.7554(7) 0.9645(10) 0.7609(8) 0.105(3) Uani 0.409(7) 1 d D U P A 2
B2 B 0.5985(7) 0.7587(7) 0.2428(6) 0.0475(17) Uani 0.648(7) 1 d D U P B 3
F5 F 0.5905(5) 0.6993(5) 0.1581(4) 0.0774(16) Uani 0.648(7) 1 d D U P B 3
F6 F 0.5300(6) 0.8291(6) 0.2280(5) 0.108(3) Uani 0.648(7) 1 d D U P B 3
F7 F 0.5500(7) 0.6749(7) 0.3087(5) 0.109(3) Uani 0.648(7) 1 d D U P B 3
F8 F 0.7221(5) 0.8283(7) 0.2744(5) 0.0606(18) Uani 0.648(7) 1 d D U P B 3
B2' B 0.5675(11) 0.7213(11) 0.2865(9) 0.049(3) Uani 0.352(7) 1 d D U P B 4
F5' F 0.5534(7) 0.6116(8) 0.3274(5) 0.0439(19) Uani 0.352(7) 1 d D U P B 4
F6' F 0.4919(7) 0.7659(8) 0.3307(7) 0.077(3) Uani 0.352(7) 1 d D U P B 4
F7' F 0.5270(9) 0.6988(7) 0.1906(6) 0.060(3) Uani 0.352(7) 1 d D U P B 4
F8' F 0.6930(9) 0.8011(10) 0.3014(8) 0.046(2) Uani 0.352(7) 1 d D U P B 4


_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 1.329(5) . ?
C1 C2 1.402(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.360(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.404(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(5) . ?
C4 C6 1.438(6) . ?
C5 N1 1.365(4) . ?
C5 C9 1.417(5) . ?
C6 C7 1.354(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.434(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(5) . ?
C8 C10 1.414(5) . ?
C9 N2 1.350(4) . ?
C10 C11 1.379(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.399(5) . ?
C11 H11 0.9300 . ?
C12 N2 1.334(4) . ?
C12 C13 1.463(5) . ?
C13 N3 1.372(5) . ?
C13 C14 1.384(5) . ?
C14 C15 1.375(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.376(5) . ?
C16 H16 0.9300 . ?
C17 N3 1.336(4) . ?
C17 H17 0.9300 . ?
C18 N4 1.324(5) . ?
C18 C19 1.402(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.358(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.389(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.404(5) . ?
C21 C23 1.465(6) . ?
C22 N4 1.375(4) . ?
C22 C26 1.418(5) . ?
C23 C24 1.341(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.462(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.388(5) . ?
C25 C27 1.394(6) . ?
C26 N5 1.345(5) . ?
C27 C28 1.385(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.413(6) . ?
C28 H28 0.9300 . ?
C29 N5 1.343(5) . ?
C29 C30 1.449(6) . ?
C30 N6 1.365(5) . ?
C30 C31 1.390(5) . ?
C31 C32 1.364(8) . ?
C31 H31 0.9300 . ?
C32 C33 1.374(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.408(6) . ?
C33 H33 0.9300 . ?
C34 N6 1.340(5) . ?
C34 H34 0.9300 . ?
C35 N7 1.120(6) . ?
C35 C36 1.438(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N8 1.125(7) . ?
C37 C38 1.465(9) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N1 Fe1 2.004(3) . ?
N2 Fe1 1.875(3) . ?
N3 Fe1 1.980(3) . ?
N4 Fe1 1.998(3) . ?
N5 Fe1 1.882(3) . ?
N6 Fe1 1.993(3) . ?
B1 F4 1.341(10) . ?
B1 F2 1.349(10) . ?
B1 F1 1.376(9) . ?
B1 F3 1.382(10) . ?
B1' F3' 1.303(13) . ?
B1' F2' 1.317(13) . ?
B1' F1' 1.332(13) . ?
B1' F4' 1.351(13) . ?
B2 F7 1.366(8) . ?
B2 F8 1.366(8) . ?
B2 F6 1.367(8) . ?
B2 F5 1.372(8) . ?
B2' F8' 1.382(12) . ?
B2' F6' 1.383(12) . ?
B2' F7' 1.385(12) . ?
B2' F5' 1.394(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 121.8(4) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 121.0(4) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 116.3(3) . . ?
C5 C4 C6 116.9(3) . . ?
C3 C4 C6 126.8(3) . . ?
N1 C5 C4 124.9(3) . . ?
N1 C5 C9 115.6(3) . . ?
C4 C5 C9 119.5(3) . . ?
C7 C6 C4 123.0(4) . . ?
C7 C6 H6 118.5 . . ?
C4 C6 H6 118.5 . . ?
C6 C7 C8 120.8(4) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C10 116.3(3) . . ?
C9 C8 C7 116.3(3) . . ?
C10 C8 C7 127.4(3) . . ?
N2 C9 C8 123.3(3) . . ?
N2 C9 C5 113.2(3) . . ?
C8 C9 C5 123.5(3) . . ?
C11 C10 C8 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C8 C10 H10 120.1 . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N2 C12 C11 120.2(3) . . ?
N2 C12 C13 110.5(3) . . ?
C11 C12 C13 129.3(3) . . ?
N3 C13 C14 121.7(3) . . ?
N3 C13 C12 113.1(3) . . ?
C14 C13 C12 125.2(3) . . ?
C15 C14 C13 118.7(4) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 119.7(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 119.4(4) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
N3 C17 C16 122.3(4) . . ?
N3 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
N4 C18 C19 122.3(4) . . ?
N4 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C20 C21 C22 116.9(4) . . ?
C20 C21 C23 128.0(4) . . ?
C22 C21 C23 115.1(4) . . ?
N4 C22 C21 123.9(3) . . ?
N4 C22 C26 115.3(3) . . ?
C21 C22 C26 120.8(3) . . ?
C24 C23 C21 123.4(4) . . ?
C24 C23 H23 118.3 . . ?
C21 C23 H23 118.3 . . ?
C23 C24 C25 121.4(4) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C26 C25 C27 117.1(4) . . ?
C26 C25 C24 115.3(4) . . ?
C27 C25 C24 127.6(4) . . ?
N5 C26 C25 123.3(4) . . ?
N5 C26 C22 112.9(3) . . ?
C25 C26 C22 123.8(3) . . ?
C28 C27 C25 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C25 C27 H27 120.0 . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
N5 C29 C28 119.8(4) . . ?
N5 C29 C30 110.6(3) . . ?
C28 C29 C30 129.7(4) . . ?
N6 C30 C31 122.7(4) . . ?
N6 C30 C29 114.0(3) . . ?
C31 C30 C29 123.3(4) . . ?
C32 C31 C30 117.9(5) . . ?
C32 C31 H31 121.0 . . ?
C30 C31 H31 121.0 . . ?
C31 C32 C33 120.6(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C34 119.4(5) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
N6 C34 C33 120.6(5) . . ?
N6 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
N7 C35 C36 179.1(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N8 C37 C38 175.0(7) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C1 N1 C5 116.8(3) . . ?
C1 N1 Fe1 131.6(3) . . ?
C5 N1 Fe1 111.6(2) . . ?
C12 N2 C9 120.2(3) . . ?
C12 N2 Fe1 121.9(2) . . ?
C9 N2 Fe1 117.9(2) . . ?
C17 N3 C13 118.3(3) . . ?
C17 N3 Fe1 126.8(3) . . ?
C13 N3 Fe1 114.9(2) . . ?
C18 N4 C22 116.9(3) . . ?
C18 N4 Fe1 131.2(2) . . ?
C22 N4 Fe1 111.9(2) . . ?
C29 N5 C26 120.1(3) . . ?
C29 N5 Fe1 121.5(3) . . ?
C26 N5 Fe1 118.4(2) . . ?
C34 N6 C30 118.8(3) . . ?
C34 N6 Fe1 126.6(3) . . ?
C30 N6 Fe1 114.6(3) . . ?
N2 Fe1 N5 179.07(12) . . ?
N2 Fe1 N3 79.59(12) . . ?
N5 Fe1 N3 101.29(12) . . ?
N2 Fe1 N6 100.93(13) . . ?
N5 Fe1 N6 79.38(14) . . ?
N3 Fe1 N6 91.47(12) . . ?
N2 Fe1 N4 98.40(12) . . ?
N5 Fe1 N4 81.31(12) . . ?
N3 Fe1 N4 90.61(11) . . ?
N6 Fe1 N4 160.61(13) . . ?
N2 Fe1 N1 81.65(12) . . ?
N5 Fe1 N1 97.46(12) . . ?
N3 Fe1 N1 161.22(12) . . ?
N6 Fe1 N1 93.08(11) . . ?
N4 Fe1 N1 91.11(11) . . ?
F4 B1 F2 111.2(8) . . ?
F4 B1 F1 111.4(8) . . ?
F2 B1 F1 112.4(8) . . ?
F4 B1 F3 108.6(8) . . ?
F2 B1 F3 104.3(7) . . ?
F1 B1 F3 108.6(7) . . ?
F3' B1' F2' 113.9(12) . . ?
F3' B1' F1' 110.0(11) . . ?
F2' B1' F1' 108.7(11) . . ?
F3' B1' F4' 106.6(11) . . ?
F2' B1' F4' 105.9(10) . . ?
F1' B1' F4' 111.6(11) . . ?
F7 B2 F8 108.2(6) . . ?
F7 B2 F6 110.9(7) . . ?
F8 B2 F6 110.9(7) . . ?
F7 B2 F5 109.2(7) . . ?
F8 B2 F5 110.4(6) . . ?
F6 B2 F5 107.3(6) . . ?
F8' B2' F6' 110.7(9) . . ?
F8' B2' F7' 110.8(10) . . ?
F6' B2' F7' 110.6(9) . . ?
F8' B2' F5' 109.5(9) . . ?
F6' B2' F5' 106.4(9) . . ?
F7' B2' F5' 108.7(9) . . ?

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 -1.0(6) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
C2 C3 C4 C5 -1.4(5) . . . . ?
C2 C3 C4 C6 178.0(4) . . . . ?
C3 C4 C5 N1 0.6(5) . . . . ?
C6 C4 C5 N1 -178.9(3) . . . . ?
C3 C4 C5 C9 178.5(3) . . . . ?
C6 C4 C5 C9 -1.0(5) . . . . ?
C5 C4 C6 C7 0.3(5) . . . . ?
C3 C4 C6 C7 -179.1(4) . . . . ?
C4 C6 C7 C8 0.4(6) . . . . ?
C6 C7 C8 C9 -0.4(5) . . . . ?
C6 C7 C8 C10 178.9(4) . . . . ?
C10 C8 C9 N2 -0.2(5) . . . . ?
C7 C8 C9 N2 179.2(3) . . . . ?
C10 C8 C9 C5 -179.7(3) . . . . ?
C7 C8 C9 C5 -0.4(5) . . . . ?
N1 C5 C9 N2 -0.4(4) . . . . ?
C4 C5 C9 N2 -178.5(3) . . . . ?
N1 C5 C9 C8 179.2(3) . . . . ?
C4 C5 C9 C8 1.1(5) . . . . ?
C9 C8 C10 C11 1.0(5) . . . . ?
C7 C8 C10 C11 -178.3(3) . . . . ?
C8 C10 C11 C12 -0.7(6) . . . . ?
C10 C11 C12 N2 -0.5(5) . . . . ?
C10 C11 C12 C13 179.3(4) . . . . ?
N2 C12 C13 N3 -2.0(4) . . . . ?
C11 C12 C13 N3 178.1(3) . . . . ?
N2 C12 C13 C14 178.3(3) . . . . ?
C11 C12 C13 C14 -1.6(6) . . . . ?
N3 C13 C14 C15 -0.1(6) . . . . ?
C12 C13 C14 C15 179.6(4) . . . . ?
C13 C14 C15 C16 -0.6(6) . . . . ?
C14 C15 C16 C17 0.7(6) . . . . ?
C15 C16 C17 N3 -0.1(6) . . . . ?
N4 C18 C19 C20 1.5(6) . . . . ?
C18 C19 C20 C21 -1.2(6) . . . . ?
C19 C20 C21 C22 0.1(6) . . . . ?
C19 C20 C21 C23 179.4(4) . . . . ?
C20 C21 C22 N4 0.9(5) . . . . ?
C23 C21 C22 N4 -178.5(3) . . . . ?
C20 C21 C22 C26 -176.2(3) . . . . ?
C23 C21 C22 C26 4.3(5) . . . . ?
C20 C21 C23 C24 177.3(4) . . . . ?
C22 C21 C23 C24 -3.3(6) . . . . ?
C21 C23 C24 C25 -0.5(7) . . . . ?
C23 C24 C25 C26 3.3(6) . . . . ?
C23 C24 C25 C27 -175.7(4) . . . . ?
C27 C25 C26 N5 -2.5(5) . . . . ?
C24 C25 C26 N5 178.4(3) . . . . ?
C27 C25 C26 C22 176.9(3) . . . . ?
C24 C25 C26 C22 -2.2(5) . . . . ?
N4 C22 C26 N5 0.4(4) . . . . ?
C21 C22 C26 N5 177.7(3) . . . . ?
N4 C22 C26 C25 -179.0(3) . . . . ?
C21 C22 C26 C25 -1.7(5) . . . . ?
C26 C25 C27 C28 1.7(5) . . . . ?
C24 C25 C27 C28 -179.2(4) . . . . ?
C25 C27 C28 C29 0.9(6) . . . . ?
C27 C28 C29 N5 -3.2(5) . . . . ?
C27 C28 C29 C30 177.7(4) . . . . ?
N5 C29 C30 N6 -0.3(4) . . . . ?
C28 C29 C30 N6 178.9(3) . . . . ?
N5 C29 C30 C31 -179.7(3) . . . . ?
C28 C29 C30 C31 -0.6(6) . . . . ?
N6 C30 C31 C32 1.0(6) . . . . ?
C29 C30 C31 C32 -179.7(4) . . . . ?
C30 C31 C32 C33 -2.1(7) . . . . ?
C31 C32 C33 C34 1.6(7) . . . . ?
C32 C33 C34 N6 0.1(6) . . . . ?
C2 C1 N1 C5 0.2(5) . . . . ?
C2 C1 N1 Fe1 -178.6(3) . . . . ?
C4 C5 N1 C1 0.0(5) . . . . ?
C9 C5 N1 C1 -177.9(3) . . . . ?
C4 C5 N1 Fe1 179.0(3) . . . . ?
C9 C5 N1 Fe1 1.1(3) . . . . ?
C11 C12 N2 C9 1.4(5) . . . . ?
C13 C12 N2 C9 -178.5(3) . . . . ?
C11 C12 N2 Fe1 -179.6(3) . . . . ?
C13 C12 N2 Fe1 0.5(4) . . . . ?
C8 C9 N2 C12 -1.0(5) . . . . ?
C5 C9 N2 C12 178.6(3) . . . . ?
C8 C9 N2 Fe1 179.9(2) . . . . ?
C5 C9 N2 Fe1 -0.5(4) . . . . ?
C16 C17 N3 C13 -0.6(5) . . . . ?
C16 C17 N3 Fe1 177.5(3) . . . . ?
C14 C13 N3 C17 0.7(5) . . . . ?
C12 C13 N3 C17 -179.0(3) . . . . ?
C14 C13 N3 Fe1 -177.6(3) . . . . ?
C12 C13 N3 Fe1 2.7(4) . . . . ?
C19 C18 N4 C22 -0.5(5) . . . . ?
C19 C18 N4 Fe1 178.9(3) . . . . ?
C21 C22 N4 C18 -0.7(5) . . . . ?
C26 C22 N4 C18 176.6(3) . . . . ?
C21 C22 N4 Fe1 179.8(3) . . . . ?
C26 C22 N4 Fe1 -2.9(4) . . . . ?
C28 C29 N5 C26 2.6(5) . . . . ?
C30 C29 N5 C26 -178.2(3) . . . . ?
C28 C29 N5 Fe1 -179.3(3) . . . . ?
C30 C29 N5 Fe1 0.0(4) . . . . ?
C25 C26 N5 C29 0.3(5) . . . . ?
C22 C26 N5 C29 -179.1(3) . . . . ?
C25 C26 N5 Fe1 -178.0(3) . . . . ?
C22 C26 N5 Fe1 2.6(4) . . . . ?
C33 C34 N6 C30 -1.2(5) . . . . ?
C33 C34 N6 Fe1 179.7(3) . . . . ?
C31 C30 N6 C34 0.7(5) . . . . ?
C29 C30 N6 C34 -178.7(3) . . . . ?
C31 C30 N6 Fe1 179.9(3) . . . . ?
C29 C30 N6 Fe1 0.5(4) . . . . ?
C12 N2 Fe1 N3 0.8(3) . . . . ?
C9 N2 Fe1 N3 179.8(3) . . . . ?
C12 N2 Fe1 N6 90.2(3) . . . . ?
C9 N2 Fe1 N6 -90.7(2) . . . . ?
C12 N2 Fe1 N4 -88.3(3) . . . . ?
C9 N2 Fe1 N4 90.7(2) . . . . ?
C12 N2 Fe1 N1 -178.2(3) . . . . ?
C9 N2 Fe1 N1 0.8(2) . . . . ?
C29 N5 Fe1 N3 89.6(3) . . . . ?
C26 N5 Fe1 N3 -92.2(2) . . . . ?
C29 N5 Fe1 N6 0.2(3) . . . . ?
C26 N5 Fe1 N6 178.4(3) . . . . ?
C29 N5 Fe1 N4 178.5(3) . . . . ?
C26 N5 Fe1 N4 -3.3(2) . . . . ?
C29 N5 Fe1 N1 -91.6(3) . . . . ?
C26 N5 Fe1 N1 86.7(2) . . . . ?

_refine_diff_density_max         1.170
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.079

_shelxl_version_number           2014/6

