# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_3_250_down
_database_code_depnum_ccdc_archive 'CCDC 867698'
_audit_update_record             
;
2012-02-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
#TrackingRef '9676_web_deposit_cif_file_3_RobertBronisz_1329662228.Cifs_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-[bis(μ₂-1,6-di(tetrazol-2-yl)hexane)-bis(propionitrile)]
-iron(II) diperchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H38 Fe N18, 2(Cl O4)'
_chemical_formula_sum            'C22 H38 Cl2 Fe N18 O8'
_chemical_formula_weight         809.45

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.495(3)
_cell_length_b                   9.667(2)
_cell_length_c                   11.668(4)
_cell_angle_alpha                89.51(3)
_cell_angle_beta                 68.43(4)
_cell_angle_gamma                65.88(3)
_cell_volume                     896.3(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    3067
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      28.68

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5543
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.84
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3261
_reflns_number_gt                2373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_structure_refinement  
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0452P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3261
_refine_ls_number_parameters     271
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.03119(14) Uani 1 2 d S . .
Cl1 Cl 0.29718(7) 0.93998(7) 0.24639(6) 0.04600(18) Uani 1 1 d . . .
O1 O 0.2192(12) 0.9707(14) 0.1548(8) 0.076(2) Uani 0.64(2) 1 d PU A 1
O2 O 0.4712(11) 0.9082(11) 0.1837(11) 0.0643(19) Uani 0.64(2) 1 d PU A 1
O3 O 0.2879(15) 0.8011(13) 0.2919(11) 0.079(2) Uani 0.64(2) 1 d PU A 1
O4 O 0.2060(14) 1.0688(10) 0.3421(11) 0.088(3) Uani 0.64(2) 1 d PU A 1
O11 O 0.249(2) 1.016(2) 0.1601(16) 0.076(3) Uani 0.36(2) 1 d PU A 2
O12 O 0.458(2) 0.933(2) 0.2351(16) 0.061(3) Uani 0.36(2) 1 d PU A 2
O13 O 0.308(3) 0.801(2) 0.243(2) 0.077(3) Uani 0.36(2) 1 d PU A 2
O14 O 0.181(2) 1.020(2) 0.3703(16) 0.081(4) Uani 0.36(2) 1 d PU A 2
N1 N 0.1387(3) 0.0265(2) -0.12889(19) 0.0489(5) Uani 1 1 d . . .
N2 N 0.1056(2) 0.1007(2) -0.21868(17) 0.0372(4) Uani 1 1 d . . .
N3 N 0.0527(2) 0.2491(2) -0.19516(17) 0.0377(4) Uani 1 1 d . . .
N4 N 0.0499(2) 0.2761(2) -0.08244(16) 0.0353(4) Uani 1 1 d . . .
C1 C 0.1371(3) 0.0203(3) -0.3380(2) 0.0474(6) Uani 1 1 d . . .
H1A H 0.0834 0.0940 -0.3833 0.057 Uiso 1 1 calc R . .
H1B H 0.0887 -0.0525 -0.3223 0.057 Uiso 1 1 calc R . .
C2 C 0.3246(3) -0.0639(3) -0.4164(2) 0.0468(6) Uani 1 1 d . . .
H2A H 0.3778 -0.1335 -0.3686 0.056 Uiso 1 1 calc R . .
H2B H 0.3426 -0.1254 -0.4902 0.056 Uiso 1 1 calc R . .
C3 C 0.4086(3) 0.0423(3) -0.4569(2) 0.0443(6) Uani 1 1 d . . .
H3A H 0.3499 0.1172 -0.4990 0.053 Uiso 1 1 calc R . .
H3B H 0.3990 0.0976 -0.3834 0.053 Uiso 1 1 calc R . .
C4 C 0.1019(3) 0.1403(3) -0.0457(2) 0.0454(6) Uani 1 1 d . . .
H4 H 0.1113 0.1272 0.0306 0.055 Uiso 1 1 calc R . .
N11 N -0.3646(2) 0.5453(2) 0.37062(17) 0.0426(5) Uani 1 1 d . . .
N12 N -0.2218(2) 0.43237(19) 0.36715(16) 0.0336(4) Uani 1 1 d . . .
N13 N -0.0959(2) 0.3917(2) 0.25779(16) 0.0379(5) Uani 1 1 d . . .
N14 N -0.1574(2) 0.4802(2) 0.18423(16) 0.0345(4) Uani 1 1 d . . .
C11 C -0.2028(3) 0.3702(3) 0.4776(2) 0.0382(5) Uani 1 1 d . . .
H11A H -0.0939 0.2824 0.4530 0.046 Uiso 1 1 calc R . .
H11B H -0.2890 0.3355 0.5178 0.046 Uiso 1 1 calc R . .
C12 C -0.2177(3) 0.4912(3) 0.5692(2) 0.0430(6) Uani 1 1 d . . .
H12A H -0.2049 0.4462 0.6415 0.052 Uiso 1 1 calc R . .
H12B H -0.3300 0.5748 0.5976 0.052 Uiso 1 1 calc R . .
C13 C -0.0904(3) 0.5575(2) 0.5174(2) 0.0406(6) Uani 1 1 d . . .
H13A H -0.1011 0.6004 0.4439 0.049 Uiso 1 1 calc R . .
H13B H -0.1179 0.6410 0.5794 0.049 Uiso 1 1 calc R . .
C14 C -0.3192(3) 0.5710(3) 0.2549(2) 0.0405(6) Uani 1 1 d . . .
H14 H -0.3915 0.6444 0.2253 0.049 Uiso 1 1 calc R . .
N20 N 0.2182(2) 0.3917(2) 0.04376(17) 0.0413(5) Uani 1 1 d . . .
C20 C 0.3273(3) 0.3265(3) 0.0725(2) 0.0369(5) Uani 1 1 d . . .
C21 C 0.4664(3) 0.2479(3) 0.1103(2) 0.0454(6) Uani 1 1 d . . .
H21A H 0.5351 0.1451 0.0620 0.054 Uiso 1 1 calc R . .
H21B H 0.4219 0.2385 0.1977 0.054 Uiso 1 1 calc R . .
C22 C 0.5758(3) 0.3318(3) 0.0918(3) 0.0664(8) Uani 1 1 d . . .
H22A H 0.6653 0.2760 0.1181 0.100 Uiso 1 1 calc R . .
H22B H 0.5089 0.4331 0.1405 0.100 Uiso 1 1 calc R . .
H22C H 0.6225 0.3392 0.0050 0.100 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N20 2.155(2) . ?
Fe1 N20 2.155(2) 2_565 ?
Fe1 N4 2.1677(19) 2_565 ?
Fe1 N4 2.1677(19) . ?
Fe1 N14 2.181(2) 2_565 ?
Fe1 N14 2.181(2) . ?
Cl1 O13 1.303(18) . ?
Cl1 O11 1.348(16) . ?
Cl1 O4 1.407(9) . ?
Cl1 O14 1.433(17) . ?
Cl1 O2 1.435(9) . ?
Cl1 O12 1.459(16) . ?
Cl1 O3 1.464(10) . ?
Cl1 O1 1.475(9) . ?
N1 C4 1.315(3) . ?
N1 N2 1.325(3) . ?
N2 N3 1.305(2) . ?
N2 C1 1.467(3) . ?
N3 N4 1.331(2) . ?
N4 C4 1.329(3) . ?
C1 C2 1.517(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.516(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C3 1.505(4) 2_654 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9300 . ?
N11 C14 1.314(3) . ?
N11 N12 1.335(2) . ?
N12 N13 1.309(2) . ?
N12 C11 1.457(3) . ?
N13 N14 1.325(2) . ?
N14 C14 1.338(3) . ?
C11 C12 1.518(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.526(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C13 1.511(4) 2_566 ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14 0.9300 . ?
N20 C20 1.141(3) . ?
C20 C21 1.455(3) . ?
C21 C22 1.518(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N20 Fe1 N20 180.00(9) . 2_565 ?
N20 Fe1 N4 90.93(8) . 2_565 ?
N20 Fe1 N4 89.07(8) 2_565 2_565 ?
N20 Fe1 N4 89.07(8) . . ?
N20 Fe1 N4 90.93(8) 2_565 . ?
N4 Fe1 N4 180.00(4) 2_565 . ?
N20 Fe1 N14 90.19(8) . 2_565 ?
N20 Fe1 N14 89.81(8) 2_565 2_565 ?
N4 Fe1 N14 92.55(8) 2_565 2_565 ?
N4 Fe1 N14 87.45(8) . 2_565 ?
N20 Fe1 N14 89.81(8) . . ?
N20 Fe1 N14 90.19(8) 2_565 . ?
N4 Fe1 N14 87.45(8) 2_565 . ?
N4 Fe1 N14 92.55(8) . . ?
N14 Fe1 N14 180.0 2_565 . ?
O13 Cl1 O11 114.5(9) . . ?
O13 Cl1 O4 132.4(7) . . ?
O11 Cl1 O4 95.3(8) . . ?
O13 Cl1 O14 106.1(8) . . ?
O11 Cl1 O14 111.0(11) . . ?
O4 Cl1 O14 26.3(7) . . ?
O13 Cl1 O2 101.0(10) . . ?
O11 Cl1 O2 95.3(8) . . ?
O4 Cl1 O2 112.7(5) . . ?
O14 Cl1 O2 128.8(7) . . ?
O13 Cl1 O12 108.9(12) . . ?
O11 Cl1 O12 110.5(9) . . ?
O4 Cl1 O12 92.5(7) . . ?
O14 Cl1 O12 105.3(8) . . ?
O2 Cl1 O12 23.8(5) . . ?
O13 Cl1 O3 21.3(10) . . ?
O11 Cl1 O3 131.3(8) . . ?
O4 Cl1 O3 112.4(5) . . ?
O14 Cl1 O3 86.5(8) . . ?
O2 Cl1 O3 108.4(6) . . ?
O12 Cl1 O3 107.5(9) . . ?
O13 Cl1 O1 90.7(9) . . ?
O11 Cl1 O1 25.2(7) . . ?
O4 Cl1 O1 107.9(6) . . ?
O14 Cl1 O1 113.2(8) . . ?
O2 Cl1 O1 109.0(5) . . ?
O12 Cl1 O1 129.6(6) . . ?
O3 Cl1 O1 106.2(6) . . ?
C4 N1 N2 101.38(19) . . ?
N3 N2 N1 114.53(18) . . ?
N3 N2 C1 123.0(2) . . ?
N1 N2 C1 122.33(19) . . ?
N2 N3 N4 105.03(18) . . ?
C4 N4 N3 106.28(18) . . ?
C4 N4 Fe1 130.59(16) . . ?
N3 N4 Fe1 122.63(14) . . ?
N2 C1 C2 110.46(19) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C3 C2 C1 113.46(19) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 C3 C2 112.7(2) 2_654 . ?
C3 C3 H3A 109.1 2_654 . ?
C2 C3 H3A 109.1 . . ?
C3 C3 H3B 109.1 2_654 . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N1 C4 N4 112.8(2) . . ?
N1 C4 H4 123.6 . . ?
N4 C4 H4 123.6 . . ?
C14 N11 N12 101.62(18) . . ?
N13 N12 N11 113.91(18) . . ?
N13 N12 C11 122.75(18) . . ?
N11 N12 C11 123.08(18) . . ?
N12 N13 N14 105.49(16) . . ?
N13 N14 C14 106.43(18) . . ?
N13 N14 Fe1 123.27(14) . . ?
C14 N14 Fe1 128.88(15) . . ?
N12 C11 C12 110.69(18) . . ?
N12 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N12 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 115.04(19) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C13 C13 C12 114.3(2) 2_566 . ?
C13 C13 H13A 108.7 2_566 . ?
C12 C13 H13A 108.7 . . ?
C13 C13 H13B 108.7 2_566 . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
N11 C14 N14 112.6(2) . . ?
N11 C14 H14 123.7 . . ?
N14 C14 H14 123.7 . . ?
C20 N20 Fe1 173.94(19) . . ?
N20 C20 C21 178.2(2) . . ?
C20 C21 C22 112.5(2) . . ?
C20 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 N2 N3 0.2(3) . . . . ?
C4 N1 N2 C1 176.27(19) . . . . ?
N1 N2 N3 N4 -0.2(2) . . . . ?
C1 N2 N3 N4 -176.17(18) . . . . ?
N2 N3 N4 C4 0.0(2) . . . . ?
N2 N3 N4 Fe1 172.70(12) . . . . ?
N20 Fe1 N4 C4 39.7(2) . . . . ?
N20 Fe1 N4 C4 -140.3(2) 2_565 . . . ?
N4 Fe1 N4 C4 -74(100) 2_565 . . . ?
N14 Fe1 N4 C4 129.9(2) 2_565 . . . ?
N14 Fe1 N4 C4 -50.1(2) . . . . ?
N20 Fe1 N4 N3 -131.03(16) . . . . ?
N20 Fe1 N4 N3 48.97(16) 2_565 . . . ?
N4 Fe1 N4 N3 115(100) 2_565 . . . ?
N14 Fe1 N4 N3 -40.80(16) 2_565 . . . ?
N14 Fe1 N4 N3 139.20(16) . . . . ?
N3 N2 C1 C2 104.5(2) . . . . ?
N1 N2 C1 C2 -71.2(3) . . . . ?
N2 C1 C2 C3 -65.0(3) . . . . ?
C1 C2 C3 C3 -175.4(3) . . . 2_654 ?
N2 N1 C4 N4 -0.2(3) . . . . ?
N3 N4 C4 N1 0.1(3) . . . . ?
Fe1 N4 C4 N1 -171.75(15) . . . . ?
C14 N11 N12 N13 0.7(2) . . . . ?
C14 N11 N12 C11 175.0(2) . . . . ?
N11 N12 N13 N14 -0.6(2) . . . . ?
C11 N12 N13 N14 -174.98(18) . . . . ?
N12 N13 N14 C14 0.3(2) . . . . ?
N12 N13 N14 Fe1 167.79(12) . . . . ?
N20 Fe1 N14 N13 -14.12(16) . . . . ?
N20 Fe1 N14 N13 165.88(16) 2_565 . . . ?
N4 Fe1 N14 N13 -105.06(17) 2_565 . . . ?
N4 Fe1 N14 N13 74.94(17) . . . . ?
N14 Fe1 N14 N13 78(100) 2_565 . . . ?
N20 Fe1 N14 C14 150.34(19) . . . . ?
N20 Fe1 N14 C14 -29.66(19) 2_565 . . . ?
N4 Fe1 N14 C14 59.41(19) 2_565 . . . ?
N4 Fe1 N14 C14 -120.59(19) . . . . ?
N14 Fe1 N14 C14 -118(100) 2_565 . . . ?
N13 N12 C11 C12 108.6(2) . . . . ?
N11 N12 C11 C12 -65.2(3) . . . . ?
N12 C11 C12 C13 -58.5(3) . . . . ?
C11 C12 C13 C13 -64.7(3) . . . 2_566 ?
N12 N11 C14 N14 -0.4(3) . . . . ?
N13 N14 C14 N11 0.1(3) . . . . ?
Fe1 N14 C14 N11 -166.44(16) . . . . ?
N20 Fe1 N20 C20 -42(62) 2_565 . . . ?
N4 Fe1 N20 C20 123.6(17) 2_565 . . . ?
N4 Fe1 N20 C20 -56.4(17) . . . . ?
N14 Fe1 N20 C20 -143.8(17) 2_565 . . . ?
N14 Fe1 N20 C20 36.2(17) . . . . ?
Fe1 N20 C20 C21 -135(7) . . . . ?
N20 C20 C21 C22 -30(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.048
####################################################################### 
# 
# 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_3_200_down
_database_code_depnum_ccdc_archive 'CCDC 867699'
_audit_update_record             
;
2012-02-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
#TrackingRef '9676_web_deposit_cif_file_3_RobertBronisz_1329662228.Cifs_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-[bis(μ₂-1,6-di(tetrazol-2-yl)hexane)-bis(propionitrile)]
-iron(II) diperchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H38 Fe N18, 2(Cl O4)'
_chemical_formula_sum            'C22 H38 Cl2 Fe N18 O8'
_chemical_formula_weight         809.45

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.454(2)
_cell_length_b                   9.637(2)
_cell_length_c                   11.621(4)
_cell_angle_alpha                89.74(3)
_cell_angle_beta                 68.55(4)
_cell_angle_gamma                66.06(3)
_cell_volume                     887.7(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4604
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      28.63

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7719
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3839
_reflns_number_gt                2908
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_structure_refinement  
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0502P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3839
_refine_ls_number_parameters     271
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.010
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.02441(11) Uani 1 2 d S . .
Cl1 Cl 0.29809(6) 0.93965(5) 0.24549(4) 0.03570(13) Uani 1 1 d . . .
O1 O 0.2233(7) 0.9723(10) 0.1524(4) 0.0601(17) Uani 0.73(2) 1 d P A 1
O2 O 0.4705(6) 0.9108(7) 0.1863(10) 0.0532(16) Uani 0.73(2) 1 d P A 1
O3 O 0.2901(10) 0.8035(10) 0.2892(9) 0.0575(15) Uani 0.73(2) 1 d P A 1
O4 O 0.2047(10) 1.0658(7) 0.3437(9) 0.0653(17) Uani 0.73(2) 1 d P A 1
O11 O 0.254(2) 1.017(2) 0.1573(14) 0.063(3) Uani 0.27(2) 1 d PU A 2
O12 O 0.4645(17) 0.9307(17) 0.2352(19) 0.045(3) Uani 0.27(2) 1 d PU A 2
O13 O 0.307(3) 0.792(2) 0.243(2) 0.059(4) Uani 0.27(2) 1 d PU A 2
O14 O 0.1805(18) 1.022(3) 0.3729(13) 0.058(4) Uani 0.27(2) 1 d PU A 2
N1 N 0.1364(2) 0.02712(18) -0.12949(16) 0.0400(4) Uani 1 1 d . . .
N2 N 0.10291(18) 0.10154(17) -0.21951(14) 0.0306(3) Uani 1 1 d . . .
N3 N 0.05032(18) 0.25037(17) -0.19584(14) 0.0311(3) Uani 1 1 d . . .
N4 N 0.04813(18) 0.27771(17) -0.08298(13) 0.0291(3) Uani 1 1 d . . .
C1 C 0.1343(2) 0.0212(2) -0.33939(18) 0.0382(5) Uani 1 1 d . . .
H1A H 0.0797 0.0966 -0.3857 0.046 Uiso 1 1 calc R . .
H1B H 0.0845 -0.0532 -0.3236 0.046 Uiso 1 1 calc R . .
C2 C 0.3226(2) -0.0635(2) -0.41795(18) 0.0375(5) Uani 1 1 d . . .
H2A H 0.3766 -0.1356 -0.3694 0.045 Uiso 1 1 calc R . .
H2B H 0.3409 -0.1253 -0.4943 0.045 Uiso 1 1 calc R . .
C3 C 0.4074(2) 0.0430(2) -0.45674(19) 0.0365(4) Uani 1 1 d . . .
H3A H 0.3974 0.0988 -0.3807 0.044 Uiso 1 1 calc R . .
H3B H 0.3483 0.1202 -0.4998 0.044 Uiso 1 1 calc R . .
C4 C 0.0998(2) 0.1414(2) -0.04534(18) 0.0368(4) Uani 1 1 d . . .
H4 H 0.1092 0.1282 0.0330 0.044 Uiso 1 1 calc R . .
N11 N -0.36529(18) 0.54628(18) 0.37029(15) 0.0354(4) Uani 1 1 d . . .
N12 N -0.22275(17) 0.43301(16) 0.36713(13) 0.0260(3) Uani 1 1 d . . .
N13 N -0.09615(18) 0.39187(16) 0.25734(13) 0.0300(3) Uani 1 1 d . . .
N14 N -0.15672(18) 0.48059(16) 0.18318(13) 0.0283(3) Uani 1 1 d . . .
C11 C -0.2045(2) 0.3707(2) 0.47852(17) 0.0311(4) Uani 1 1 d . . .
H11A H -0.0933 0.2808 0.4535 0.037 Uiso 1 1 calc R . .
H11B H -0.2930 0.3355 0.5194 0.037 Uiso 1 1 calc R . .
C12 C -0.2191(2) 0.4922(2) 0.57072(17) 0.0340(4) Uani 1 1 d . . .
H12A H -0.2054 0.4464 0.6446 0.041 Uiso 1 1 calc R . .
H12B H -0.3341 0.5776 0.6001 0.041 Uiso 1 1 calc R . .
C13 C -0.0909(2) 0.5587(2) 0.51764(18) 0.0321(4) Uani 1 1 d . . .
H13A H -0.1021 0.6020 0.4423 0.039 Uiso 1 1 calc R . .
H13B H -0.1179 0.6443 0.5807 0.039 Uiso 1 1 calc R . .
C14 C -0.3191(2) 0.5724(2) 0.25410(17) 0.0329(4) Uani 1 1 d . . .
H14 H -0.3927 0.6479 0.2238 0.039 Uiso 1 1 calc R . .
N20 N 0.21721(19) 0.39146(18) 0.04355(14) 0.0335(4) Uani 1 1 d . . .
C20 C 0.3265(2) 0.3267(2) 0.07280(17) 0.0311(4) Uani 1 1 d . . .
C21 C 0.4661(2) 0.2475(2) 0.11060(19) 0.0374(4) Uani 1 1 d . . .
H21A H 0.5357 0.1421 0.0614 0.045 Uiso 1 1 calc R . .
H21B H 0.4207 0.2386 0.2003 0.045 Uiso 1 1 calc R . .
C22 C 0.5765(3) 0.3316(3) 0.0910(2) 0.0521(6) Uani 1 1 d . . .
H22A H 0.6684 0.2750 0.1178 0.078 Uiso 1 1 calc R . .
H22B H 0.5085 0.4355 0.1406 0.078 Uiso 1 1 calc R . .
H22C H 0.6239 0.3385 0.0019 0.078 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N20 2.1399(17) . ?
Fe1 N20 2.1399(17) 2_565 ?
Fe1 N4 2.1523(16) 2_565 ?
Fe1 N4 2.1523(16) . ?
Fe1 N14 2.1625(18) . ?
Fe1 N14 2.1625(18) 2_565 ?
Cl1 O11 1.354(14) . ?
Cl1 O13 1.39(2) . ?
Cl1 O4 1.401(5) . ?
Cl1 O2 1.422(5) . ?
Cl1 O3 1.426(8) . ?
Cl1 O1 1.465(6) . ?
Cl1 O14 1.467(13) . ?
Cl1 O12 1.500(13) . ?
N1 C4 1.320(2) . ?
N1 N2 1.327(2) . ?
N2 N3 1.306(2) . ?
N2 C1 1.466(2) . ?
N3 N4 1.330(2) . ?
N4 C4 1.337(2) . ?
C1 C2 1.519(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.516(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.518(4) 2_654 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 0.9500 . ?
N11 C14 1.316(2) . ?
N11 N12 1.334(2) . ?
N12 N13 1.311(2) . ?
N12 C11 1.462(2) . ?
N13 N14 1.326(2) . ?
N14 C14 1.341(2) . ?
C11 C12 1.520(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.530(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C13 1.521(4) 2_566 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14 0.9500 . ?
N20 C20 1.142(2) . ?
C20 C21 1.456(3) . ?
C21 C22 1.519(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
N20 Fe1 N20 180.00(13) . 2_565 ?
N20 Fe1 N4 90.85(7) . 2_565 ?
N20 Fe1 N4 89.15(7) 2_565 2_565 ?
N20 Fe1 N4 89.15(7) . . ?
N20 Fe1 N4 90.85(7) 2_565 . ?
N4 Fe1 N4 180.00(4) 2_565 . ?
N20 Fe1 N14 89.79(7) . . ?
N20 Fe1 N14 90.21(7) 2_565 . ?
N4 Fe1 N14 87.34(7) 2_565 . ?
N4 Fe1 N14 92.66(7) . . ?
N20 Fe1 N14 90.21(7) . 2_565 ?
N20 Fe1 N14 89.79(7) 2_565 2_565 ?
N4 Fe1 N14 92.66(7) 2_565 2_565 ?
N4 Fe1 N14 87.34(7) . 2_565 ?
N14 Fe1 N14 180.00(8) . 2_565 ?
O11 Cl1 O13 115.6(8) . . ?
O11 Cl1 O4 96.5(6) . . ?
O13 Cl1 O4 129.9(7) . . ?
O11 Cl1 O2 94.5(7) . . ?
O13 Cl1 O2 102.7(9) . . ?
O4 Cl1 O2 112.5(3) . . ?
O11 Cl1 O3 132.6(9) . . ?
O13 Cl1 O3 20.5(8) . . ?
O4 Cl1 O3 111.0(3) . . ?
O2 Cl1 O3 108.5(4) . . ?
O11 Cl1 O1 25.0(8) . . ?
O13 Cl1 O1 92.0(8) . . ?
O4 Cl1 O1 108.1(3) . . ?
O2 Cl1 O1 108.9(3) . . ?
O3 Cl1 O1 107.7(4) . . ?
O11 Cl1 O14 111.9(10) . . ?
O13 Cl1 O14 105.8(7) . . ?
O4 Cl1 O14 24.2(7) . . ?
O2 Cl1 O14 126.6(6) . . ?
O3 Cl1 O14 87.1(8) . . ?
O1 Cl1 O14 114.2(7) . . ?
O11 Cl1 O12 109.6(8) . . ?
O13 Cl1 O12 108.9(11) . . ?
O4 Cl1 O12 93.5(6) . . ?
O2 Cl1 O12 22.6(4) . . ?
O3 Cl1 O12 106.5(6) . . ?
O1 Cl1 O12 128.8(5) . . ?
O14 Cl1 O12 104.4(8) . . ?
C4 N1 N2 101.49(15) . . ?
N3 N2 N1 114.63(15) . . ?
N3 N2 C1 122.88(16) . . ?
N1 N2 C1 122.35(15) . . ?
N2 N3 N4 105.09(15) . . ?
N3 N4 C4 106.48(15) . . ?
N3 N4 Fe1 123.03(12) . . ?
C4 N4 Fe1 130.02(13) . . ?
N2 C1 C2 110.41(16) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C3 C2 C1 113.37(16) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 C3 112.47(19) . 2_654 ?
C2 C3 H3A 109.1 . . ?
C3 C3 H3A 109.1 2_654 . ?
C2 C3 H3B 109.1 . . ?
C3 C3 H3B 109.1 2_654 . ?
H3A C3 H3B 107.8 . . ?
N1 C4 N4 112.30(17) . . ?
N1 C4 H4 123.8 . . ?
N4 C4 H4 123.8 . . ?
C14 N11 N12 101.74(15) . . ?
N13 N12 N11 113.84(15) . . ?
N13 N12 C11 122.80(14) . . ?
N11 N12 C11 123.10(14) . . ?
N12 N13 N14 105.65(14) . . ?
N13 N14 C14 106.27(15) . . ?
N13 N14 Fe1 123.59(11) . . ?
C14 N14 Fe1 128.73(13) . . ?
N12 C11 C12 110.61(15) . . ?
N12 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N12 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.57(15) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C13 C13 C12 113.69(19) 2_566 . ?
C13 C13 H13A 108.8 2_566 . ?
C12 C13 H13A 108.8 . . ?
C13 C13 H13B 108.8 2_566 . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
N11 C14 N14 112.49(17) . . ?
N11 C14 H14 123.8 . . ?
N14 C14 H14 123.8 . . ?
C20 N20 Fe1 174.22(15) . . ?
N20 C20 C21 178.64(19) . . ?
C20 C21 C22 112.03(16) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 N2 N3 0.3(2) . . . . ?
C4 N1 N2 C1 176.14(16) . . . . ?
N1 N2 N3 N4 -0.1(2) . . . . ?
C1 N2 N3 N4 -175.86(14) . . . . ?
N2 N3 N4 C4 -0.22(18) . . . . ?
N2 N3 N4 Fe1 172.62(10) . . . . ?
N20 Fe1 N4 N3 -131.23(13) . . . . ?
N20 Fe1 N4 N3 48.77(13) 2_565 . . . ?
N4 Fe1 N4 N3 128(100) 2_565 . . . ?
N14 Fe1 N4 N3 139.02(13) . . . . ?
N14 Fe1 N4 N3 -40.98(13) 2_565 . . . ?
N20 Fe1 N4 C4 39.78(16) . . . . ?
N20 Fe1 N4 C4 -140.22(16) 2_565 . . . ?
N4 Fe1 N4 C4 -61(100) 2_565 . . . ?
N14 Fe1 N4 C4 -49.97(16) . . . . ?
N14 Fe1 N4 C4 130.03(16) 2_565 . . . ?
N3 N2 C1 C2 104.6(2) . . . . ?
N1 N2 C1 C2 -70.9(2) . . . . ?
N2 C1 C2 C3 -64.4(2) . . . . ?
C1 C2 C3 C3 -175.6(2) . . . 2_654 ?
N2 N1 C4 N4 -0.4(2) . . . . ?
N3 N4 C4 N1 0.4(2) . . . . ?
Fe1 N4 C4 N1 -171.72(12) . . . . ?
C14 N11 N12 N13 0.45(19) . . . . ?
C14 N11 N12 C11 174.74(15) . . . . ?
N11 N12 N13 N14 -0.53(19) . . . . ?
C11 N12 N13 N14 -174.84(14) . . . . ?
N12 N13 N14 C14 0.37(18) . . . . ?
N12 N13 N14 Fe1 167.86(10) . . . . ?
N20 Fe1 N14 N13 -14.15(13) . . . . ?
N20 Fe1 N14 N13 165.85(13) 2_565 . . . ?
N4 Fe1 N14 N13 -105.01(14) 2_565 . . . ?
N4 Fe1 N14 N13 74.99(14) . . . . ?
N14 Fe1 N14 N13 113(100) 2_565 . . . ?
N20 Fe1 N14 C14 150.39(15) . . . . ?
N20 Fe1 N14 C14 -29.61(15) 2_565 . . . ?
N4 Fe1 N14 C14 59.53(15) 2_565 . . . ?
N4 Fe1 N14 C14 -120.47(15) . . . . ?
N14 Fe1 N14 C14 -82(100) 2_565 . . . ?
N13 N12 C11 C12 108.64(18) . . . . ?
N11 N12 C11 C12 -65.1(2) . . . . ?
N12 C11 C12 C13 -57.9(2) . . . . ?
C11 C12 C13 C13 -64.7(3) . . . 2_566 ?
N12 N11 C14 N14 -0.2(2) . . . . ?
N13 N14 C14 N11 -0.1(2) . . . . ?
Fe1 N14 C14 N11 -166.73(13) . . . . ?
N20 Fe1 N20 C20 -42(5) 2_565 . . . ?
N4 Fe1 N20 C20 119.3(15) 2_565 . . . ?
N4 Fe1 N20 C20 -60.7(15) . . . . ?
N14 Fe1 N20 C20 32.0(15) . . . . ?
N14 Fe1 N20 C20 -148.0(15) 2_565 . . . ?
Fe1 N20 C20 C21 -136(8) . . . . ?
N20 C20 C21 C22 -25(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.053
####################################################################### 
# 
# 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_3_160_down
_database_code_depnum_ccdc_archive 'CCDC 867700'
_audit_update_record             
;
2012-02-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
#TrackingRef '9676_web_deposit_cif_file_3_RobertBronisz_1329662228.Cifs_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-[bis(μ₂-1,6-di(tetrazol-2-yl)hexane)-bis(propionitrile)]
-iron(II) diperchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H38 Fe N18, 2(Cl O4)'
_chemical_formula_sum            'C22 H38 Cl2 Fe N18 O8'
_chemical_formula_weight         809.45

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.403(3)
_cell_length_b                   9.602(2)
_cell_length_c                   11.546(4)
_cell_angle_alpha                90.08(3)
_cell_angle_beta                 68.46(4)
_cell_angle_gamma                66.12(3)
_cell_volume                     872.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    4671
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      28.55

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-pink
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7396
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3754
_reflns_number_gt                2933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_structure_refinement  
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0445P)²+0.0776P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3754
_refine_ls_number_parameters     271
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.01909(10) Uani 1 2 d S . .
Cl1 Cl 0.30030(5) 0.93878(5) 0.24461(4) 0.02853(12) Uani 1 1 d . . .
O1 O 0.2269(6) 0.9698(8) 0.1495(4) 0.0462(12) Uani 0.726(19) 1 d PU A 1
O2 O 0.4750(5) 0.9101(6) 0.1847(8) 0.0401(12) Uani 0.726(19) 1 d PU A 1
O3 O 0.2918(7) 0.8007(7) 0.2889(7) 0.0418(11) Uani 0.726(19) 1 d PU A 1
O4 O 0.2058(8) 1.0669(6) 0.3449(6) 0.0502(13) Uani 0.726(19) 1 d PU A 1
O11 O 0.2524(17) 1.0133(17) 0.1556(12) 0.045(2) Uani 0.274(19) 1 d PU A 2
O12 O 0.4661(15) 0.9317(15) 0.2308(15) 0.035(2) Uani 0.274(19) 1 d PU A 2
O13 O 0.3092(19) 0.7914(18) 0.2450(16) 0.041(2) Uani 0.274(19) 1 d PU A 2
O14 O 0.1807(17) 1.0312(18) 0.3703(13) 0.041(2) Uani 0.274(19) 1 d PU A 2
N1 N 0.1318(2) 0.03326(19) -0.12588(16) 0.0347(4) Uani 1 1 d . . .
N2 N 0.09846(18) 0.10740(17) -0.21669(14) 0.0266(3) Uani 1 1 d . . .
N3 N 0.04760(18) 0.25693(17) -0.19351(14) 0.0263(3) Uani 1 1 d . . .
N4 N 0.04639(17) 0.28510(17) -0.07982(13) 0.0246(3) Uani 1 1 d . . .
C1 C 0.1301(2) 0.0255(2) -0.33734(18) 0.0322(4) Uani 1 1 d . . .
H1A H 0.0757 0.1007 -0.3841 0.039 Uiso 1 1 calc R . .
H1B H 0.0790 -0.0485 -0.3210 0.039 Uiso 1 1 calc R . .
C2 C 0.3194(2) -0.0612(2) -0.41696(18) 0.0320(4) Uani 1 1 d . . .
H2A H 0.3372 -0.1231 -0.4940 0.038 Uiso 1 1 calc R . .
H2B H 0.3730 -0.1339 -0.3684 0.038 Uiso 1 1 calc R . .
C3 C 0.4069(2) 0.0444(2) -0.45615(18) 0.0307(4) Uani 1 1 d . . .
H3A H 0.3482 0.1223 -0.4993 0.037 Uiso 1 1 calc R . .
H3B H 0.3975 0.1003 -0.3796 0.037 Uiso 1 1 calc R . .
C4 C 0.0976(2) 0.1480(2) -0.04174(18) 0.0313(4) Uani 1 1 d . . .
H4 H 0.1081 0.1351 0.0368 0.038 Uiso 1 1 calc R . .
N11 N -0.36443(19) 0.54565(18) 0.36453(15) 0.0304(4) Uani 1 1 d . . .
N12 N -0.22090(17) 0.43225(16) 0.36206(14) 0.0233(3) Uani 1 1 d . . .
N13 N -0.09130(18) 0.39220(16) 0.25211(14) 0.0257(3) Uani 1 1 d . . .
N14 N -0.15139(18) 0.48187(16) 0.17769(14) 0.0244(3) Uani 1 1 d . . .
C11 C -0.2041(2) 0.3701(2) 0.47422(17) 0.0262(4) Uani 1 1 d . . .
H11A H -0.0922 0.2799 0.4491 0.031 Uiso 1 1 calc R . .
H11B H -0.2933 0.3347 0.5145 0.031 Uiso 1 1 calc R . .
C12 C -0.2206(2) 0.4928(2) 0.56858(17) 0.0285(4) Uani 1 1 d . . .
H12A H -0.2083 0.4470 0.6431 0.034 Uiso 1 1 calc R . .
H12B H -0.3363 0.5787 0.5978 0.034 Uiso 1 1 calc R . .
C13 C -0.0913(2) 0.5593(2) 0.51667(17) 0.0265(4) Uani 1 1 d . . .
H13A H -0.1000 0.6014 0.4400 0.032 Uiso 1 1 calc R . .
H13B H -0.1201 0.6461 0.5805 0.032 Uiso 1 1 calc R . .
C14 C -0.3166(2) 0.5729(2) 0.24828(17) 0.0283(4) Uani 1 1 d . . .
H14 H -0.3902 0.6482 0.2176 0.034 Uiso 1 1 calc R . .
N20 N 0.2079(2) 0.39721(17) 0.04208(14) 0.0278(3) Uani 1 1 d . . .
C20 C 0.3179(2) 0.3325(2) 0.07167(16) 0.0278(4) Uani 1 1 d . . .
C21 C 0.4568(2) 0.2519(2) 0.11083(18) 0.0323(4) Uani 1 1 d . . .
H21A H 0.5253 0.1451 0.0621 0.039 Uiso 1 1 calc R . .
H21B H 0.4092 0.2453 0.2015 0.039 Uiso 1 1 calc R . .
C22 C 0.5717(3) 0.3332(3) 0.0905(2) 0.0430(5) Uani 1 1 d . . .
H22A H 0.6632 0.2752 0.1178 0.064 Uiso 1 1 calc R . .
H22B H 0.5050 0.4382 0.1401 0.064 Uiso 1 1 calc R . .
H22C H 0.6208 0.3385 0.0006 0.064 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N20 2.0413(18) 2_565 ?
Fe1 N20 2.0414(18) . ?
Fe1 N4 2.0660(16) 2_565 ?
Fe1 N4 2.0660(16) . ?
Fe1 N14 2.0792(18) 2_565 ?
Fe1 N14 2.0792(18) . ?
Cl1 O11 1.362(12) . ?
Cl1 O13 1.384(17) . ?
Cl1 O4 1.414(5) . ?
Cl1 O2 1.433(4) . ?
Cl1 O3 1.443(6) . ?
Cl1 O14 1.465(13) . ?
Cl1 O1 1.470(5) . ?
Cl1 O12 1.481(12) . ?
N1 C4 1.320(2) . ?
N1 N2 1.329(2) . ?
N2 N3 1.308(2) . ?
N2 C1 1.467(2) . ?
N3 N4 1.335(2) . ?
N4 C4 1.342(2) . ?
C1 C2 1.517(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.519(4) 2_654 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 0.9500 . ?
N11 C14 1.313(2) . ?
N11 N12 1.338(2) . ?
N12 N13 1.314(2) . ?
N12 C11 1.461(2) . ?
N13 N14 1.328(2) . ?
N14 C14 1.345(2) . ?
C11 C12 1.524(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.530(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C13 1.524(3) 2_566 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14 0.9500 . ?
N20 C20 1.146(2) . ?
C20 C21 1.458(3) . ?
C21 C22 1.527(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
N20 Fe1 N20 180.00(13) 2_565 . ?
N20 Fe1 N4 89.31(7) 2_565 2_565 ?
N20 Fe1 N4 90.69(7) . 2_565 ?
N20 Fe1 N4 90.69(7) 2_565 . ?
N20 Fe1 N4 89.31(7) . . ?
N4 Fe1 N4 180.0 2_565 . ?
N20 Fe1 N14 89.48(7) 2_565 2_565 ?
N20 Fe1 N14 90.52(7) . 2_565 ?
N4 Fe1 N14 92.38(7) 2_565 2_565 ?
N4 Fe1 N14 87.62(7) . 2_565 ?
N20 Fe1 N14 90.52(7) 2_565 . ?
N20 Fe1 N14 89.48(7) . . ?
N4 Fe1 N14 87.62(7) 2_565 . ?
N4 Fe1 N14 92.38(7) . . ?
N14 Fe1 N14 180.00(8) 2_565 . ?
O11 Cl1 O13 115.4(7) . . ?
O11 Cl1 O4 97.4(5) . . ?
O13 Cl1 O4 128.7(5) . . ?
O11 Cl1 O2 96.0(5) . . ?
O13 Cl1 O2 103.0(6) . . ?
O4 Cl1 O2 111.9(3) . . ?
O11 Cl1 O3 130.5(6) . . ?
O13 Cl1 O3 18.9(6) . . ?
O4 Cl1 O3 111.0(2) . . ?
O2 Cl1 O3 108.8(3) . . ?
O11 Cl1 O14 109.1(7) . . ?
O13 Cl1 O14 107.9(6) . . ?
O4 Cl1 O14 20.9(5) . . ?
O2 Cl1 O14 125.5(5) . . ?
O3 Cl1 O14 90.6(5) . . ?
O11 Cl1 O1 23.0(6) . . ?
O13 Cl1 O1 93.3(6) . . ?
O4 Cl1 O1 109.0(3) . . ?
O2 Cl1 O1 108.5(3) . . ?
O3 Cl1 O1 107.6(3) . . ?
O14 Cl1 O1 113.2(6) . . ?
O11 Cl1 O12 109.9(6) . . ?
O13 Cl1 O12 109.2(8) . . ?
O4 Cl1 O12 93.7(5) . . ?
O2 Cl1 O12 21.1(4) . . ?
O3 Cl1 O12 107.8(5) . . ?
O14 Cl1 O12 104.9(7) . . ?
O1 Cl1 O12 126.7(5) . . ?
C4 N1 N2 101.61(15) . . ?
N3 N2 N1 114.70(15) . . ?
N3 N2 C1 122.91(15) . . ?
N1 N2 C1 122.21(15) . . ?
N2 N3 N4 104.99(14) . . ?
N3 N4 C4 106.44(15) . . ?
N3 N4 Fe1 122.88(11) . . ?
C4 N4 Fe1 130.28(13) . . ?
N2 C1 C2 110.63(15) . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 113.42(15) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 C3 C2 112.20(19) 2_654 . ?
C3 C3 H3A 109.2 2_654 . ?
C2 C3 H3A 109.2 . . ?
C3 C3 H3B 109.2 2_654 . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 N4 112.25(17) . . ?
N1 C4 H4 123.9 . . ?
N4 C4 H4 123.9 . . ?
C14 N11 N12 102.05(15) . . ?
N13 N12 N11 113.76(15) . . ?
N13 N12 C11 122.65(14) . . ?
N11 N12 C11 123.27(15) . . ?
N12 N13 N14 105.41(14) . . ?
N13 N14 C14 106.58(15) . . ?
N13 N14 Fe1 124.00(11) . . ?
C14 N14 Fe1 128.42(13) . . ?
N12 C11 C12 110.64(14) . . ?
N12 C11 H11A 109.5 . . ?
C12 C11 H11A 109.5 . . ?
N12 C11 H11B 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.60(15) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C13 C13 C12 113.37(18) 2_566 . ?
C13 C13 H13A 108.9 2_566 . ?
C12 C13 H13A 108.9 . . ?
C13 C13 H13B 108.9 2_566 . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
N11 C14 N14 112.20(17) . . ?
N11 C14 H14 123.9 . . ?
N14 C14 H14 123.9 . . ?
C20 N20 Fe1 174.20(14) . . ?
N20 C20 C21 179.19(19) . . ?
C20 C21 C22 112.23(16) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 N2 N3 0.2(2) . . . . ?
C4 N1 N2 C1 175.34(15) . . . . ?
N1 N2 N3 N4 -0.13(19) . . . . ?
C1 N2 N3 N4 -175.27(14) . . . . ?
N2 N3 N4 C4 0.03(18) . . . . ?
N2 N3 N4 Fe1 173.52(10) . . . . ?
N20 Fe1 N4 N3 48.15(13) 2_565 . . . ?
N20 Fe1 N4 N3 -131.85(13) . . . . ?
N4 Fe1 N4 N3 173(85) 2_565 . . . ?
N14 Fe1 N4 N3 -41.30(13) 2_565 . . . ?
N14 Fe1 N4 N3 138.70(13) . . . . ?
N20 Fe1 N4 C4 -140.05(16) 2_565 . . . ?
N20 Fe1 N4 C4 39.95(16) . . . . ?
N4 Fe1 N4 C4 -15(85) 2_565 . . . ?
N14 Fe1 N4 C4 130.50(16) 2_565 . . . ?
N14 Fe1 N4 C4 -49.50(16) . . . . ?
N3 N2 C1 C2 104.04(19) . . . . ?
N1 N2 C1 C2 -70.7(2) . . . . ?
N2 C1 C2 C3 -63.9(2) . . . . ?
C1 C2 C3 C3 -175.6(2) . . . 2_654 ?
N2 N1 C4 N4 -0.1(2) . . . . ?
N3 N4 C4 N1 0.1(2) . . . . ?
Fe1 N4 C4 N1 -172.76(12) . . . . ?
C14 N11 N12 N13 0.67(19) . . . . ?
C14 N11 N12 C11 174.28(15) . . . . ?
N11 N12 N13 N14 -0.56(18) . . . . ?
C11 N12 N13 N14 -174.21(14) . . . . ?
N12 N13 N14 C14 0.20(17) . . . . ?
N12 N13 N14 Fe1 169.58(10) . . . . ?
N20 Fe1 N14 N13 164.93(13) 2_565 . . . ?
N20 Fe1 N14 N13 -15.07(13) . . . . ?
N4 Fe1 N14 N13 -105.79(14) 2_565 . . . ?
N4 Fe1 N14 N13 74.21(14) . . . . ?
N14 Fe1 N14 N13 -45(100) 2_565 . . . ?
N20 Fe1 N14 C14 -28.10(15) 2_565 . . . ?
N20 Fe1 N14 C14 151.90(15) . . . . ?
N4 Fe1 N14 C14 61.18(15) 2_565 . . . ?
N4 Fe1 N14 C14 -118.82(15) . . . . ?
N14 Fe1 N14 C14 122(100) 2_565 . . . ?
N13 N12 C11 C12 107.57(17) . . . . ?
N11 N12 C11 C12 -65.5(2) . . . . ?
N12 C11 C12 C13 -58.1(2) . . . . ?
C11 C12 C13 C13 -65.3(3) . . . 2_566 ?
N12 N11 C14 N14 -0.52(19) . . . . ?
N13 N14 C14 N11 0.2(2) . . . . ?
Fe1 N14 C14 N11 -168.54(12) . . . . ?
N20 Fe1 N20 C20 60(100) 2_565 . . . ?
N4 Fe1 N20 C20 120.4(14) 2_565 . . . ?
N4 Fe1 N20 C20 -59.6(14) . . . . ?
N14 Fe1 N20 C20 -147.3(14) 2_565 . . . ?
N14 Fe1 N20 C20 32.7(14) . . . . ?
Fe1 N20 C20 C21 -93(15) . . . . ?
N20 C20 C21 C22 -70(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_3_100_down
_database_code_depnum_ccdc_archive 'CCDC 867701'
_audit_update_record             
;
2012-02-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
#TrackingRef '9676_web_deposit_cif_file_3_RobertBronisz_1329662228.Cifs_3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena-[bis(μ₂-1,6-di(tetrazol-2-yl)hexane)-bis(propionitrile)]
-iron(II) diperchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H38 Fe N18, 2(Cl O4)'
_chemical_formula_sum            'C22 H38 Cl2 Fe N18 O8'
_chemical_formula_weight         809.45

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.341(3)
_cell_length_b                   9.555(2)
_cell_length_c                   11.409(4)
_cell_angle_alpha                90.68(3)
_cell_angle_beta                 68.74(4)
_cell_angle_gamma                66.37(3)
_cell_volume                     854.6(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5183
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      28.73

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Kuma KM4CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7328
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3667
_reflns_number_gt                3020
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_structure_refinement  
;
SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0492P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3667
_refine_ls_number_parameters     271
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0804
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.078
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.01141(10) Uani 1 2 d S . .
Cl1 Cl 0.30208(5) 0.93647(4) 0.24186(4) 0.01713(11) Uani 1 1 d . . .
O1 O 0.2276(9) 0.9641(11) 0.1462(7) 0.0242(12) Uani 0.74(4) 1 d PU A 1
O2 O 0.4787(8) 0.9088(9) 0.1803(11) 0.0215(11) Uani 0.74(4) 1 d PU A 1
O3 O 0.2935(14) 0.7959(12) 0.2893(11) 0.0231(11) Uani 0.74(4) 1 d PU A 1
O4 O 0.2095(13) 1.0679(9) 0.3442(9) 0.0277(13) Uani 0.74(4) 1 d PU A 1
O11 O 0.246(3) 0.995(3) 0.148(2) 0.028(3) Uani 0.26(4) 1 d PU A 2
O12 O 0.471(2) 0.927(2) 0.215(2) 0.020(2) Uani 0.26(4) 1 d PU A 2
O13 O 0.307(4) 0.798(4) 0.262(3) 0.027(3) Uani 0.26(4) 1 d PU A 2
O14 O 0.185(3) 1.047(3) 0.362(2) 0.023(3) Uani 0.26(4) 1 d PU A 2
N1 N 0.12659(18) 0.03947(16) -0.12343(13) 0.0190(3) Uani 1 1 d . . .
N2 N 0.09435(17) 0.11337(16) -0.21565(13) 0.0151(3) Uani 1 1 d . . .
N3 N 0.04503(17) 0.26410(15) -0.19264(13) 0.0148(3) Uani 1 1 d . . .
N4 N 0.04472(16) 0.29219(15) -0.07778(13) 0.0138(3) Uani 1 1 d . . .
C1 C 0.1259(2) 0.0299(2) -0.33784(16) 0.0182(3) Uani 1 1 d . . .
H1A H 0.0724 0.1049 -0.3856 0.022 Uiso 1 1 calc R . .
H1B H 0.0735 -0.0437 -0.3214 0.022 Uiso 1 1 calc R . .
C2 C 0.3165(2) -0.05888(19) -0.41774(16) 0.0180(3) Uani 1 1 d . . .
H2A H 0.3343 -0.1203 -0.4965 0.022 Uiso 1 1 calc R . .
H2B H 0.3689 -0.1326 -0.3687 0.022 Uiso 1 1 calc R . .
C3 C 0.4067(2) 0.04581(19) -0.45515(16) 0.0181(3) Uani 1 1 d . . .
H3A H 0.3485 0.1257 -0.4976 0.022 Uiso 1 1 calc R . .
H3B H 0.3992 0.0998 -0.3770 0.022 Uiso 1 1 calc R . .
C4 C 0.0935(2) 0.15517(19) -0.03791(16) 0.0177(3) Uani 1 1 d . . .
H4 H 0.1029 0.1431 0.0419 0.021 Uiso 1 1 calc R . .
N11 N -0.36291(17) 0.54521(16) 0.35841(13) 0.0173(3) Uani 1 1 d . . .
N12 N -0.21932(16) 0.43172(15) 0.35620(12) 0.0133(3) Uani 1 1 d . . .
N13 N -0.08714(17) 0.39248(15) 0.24618(13) 0.0148(3) Uani 1 1 d . . .
N14 N -0.14647(16) 0.48376(15) 0.17130(13) 0.0136(3) Uani 1 1 d . . .
C11 C -0.2051(2) 0.36966(18) 0.47019(15) 0.0151(3) Uani 1 1 d . . .
H11A H -0.0931 0.2787 0.4456 0.018 Uiso 1 1 calc R . .
H11B H -0.2954 0.3348 0.5096 0.018 Uiso 1 1 calc R . .
C12 C -0.2224(2) 0.49348(19) 0.56679(15) 0.0167(3) Uani 1 1 d . . .
H12A H -0.2114 0.4481 0.6424 0.020 Uiso 1 1 calc R . .
H12B H -0.3382 0.5799 0.5957 0.020 Uiso 1 1 calc R . .
C13 C -0.0916(2) 0.55962(18) 0.51597(16) 0.0162(3) Uani 1 1 d . . .
H13A H -0.0985 0.6008 0.4380 0.019 Uiso 1 1 calc R . .
H13B H -0.1213 0.6475 0.5809 0.019 Uiso 1 1 calc R . .
C14 C -0.3131(2) 0.57488(19) 0.24144(15) 0.0159(3) Uani 1 1 d . . .
H14 H -0.3860 0.6512 0.2105 0.019 Uiso 1 1 calc R . .
N20 N 0.19715(17) 0.40287(15) 0.04184(12) 0.0139(3) Uani 1 1 d . . .
C20 C 0.3071(2) 0.33860(18) 0.07230(15) 0.0144(3) Uani 1 1 d . . .
C21 C 0.4464(2) 0.25640(19) 0.11273(16) 0.0176(3) Uani 1 1 d . . .
H21A H 0.5137 0.1487 0.0637 0.021 Uiso 1 1 calc R . .
H21B H 0.3977 0.2510 0.2045 0.021 Uiso 1 1 calc R . .
C22 C 0.5649(2) 0.3355(2) 0.09264(19) 0.0247(4) Uani 1 1 d . . .
H22A H 0.6562 0.2761 0.1204 0.037 Uiso 1 1 calc R . .
H22B H 0.4997 0.4413 0.1429 0.037 Uiso 1 1 calc R . .
H22C H 0.6149 0.3399 0.0017 0.037 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N20 1.9387(15) . ?
Fe1 N20 1.9387(15) 2_565 ?
Fe1 N4 1.9822(15) 2_565 ?
Fe1 N4 1.9822(15) . ?
Fe1 N14 1.9884(17) 2_565 ?
Fe1 N14 1.9884(17) . ?
Cl1 O13 1.33(3) . ?
Cl1 O11 1.38(2) . ?
Cl1 O4 1.432(8) . ?
Cl1 O2 1.446(7) . ?
Cl1 O12 1.46(2) . ?
Cl1 O14 1.46(2) . ?
Cl1 O1 1.468(8) . ?
Cl1 O3 1.475(11) . ?
N1 C4 1.323(2) . ?
N1 N2 1.332(2) . ?
N2 N3 1.3141(19) . ?
N2 C1 1.468(2) . ?
N3 N4 1.3333(19) . ?
N4 C4 1.347(2) . ?
C1 C2 1.521(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.523(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.521(3) 2_654 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 0.9500 . ?
N11 C14 1.320(2) . ?
N11 N12 1.3358(19) . ?
N12 N13 1.3170(19) . ?
N12 C11 1.463(2) . ?
N13 N14 1.3309(19) . ?
N14 C14 1.347(2) . ?
C11 C12 1.525(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.531(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C13 1.528(3) 2_566 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14 0.9500 . ?
N20 C20 1.145(2) . ?
C20 C21 1.466(2) . ?
C21 C22 1.530(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
N20 Fe1 N20 180.00(12) . 2_565 ?
N20 Fe1 N4 90.72(6) . 2_565 ?
N20 Fe1 N4 89.28(6) 2_565 2_565 ?
N20 Fe1 N4 89.28(6) . . ?
N20 Fe1 N4 90.72(6) 2_565 . ?
N4 Fe1 N4 180.00(3) 2_565 . ?
N20 Fe1 N14 90.63(7) . 2_565 ?
N20 Fe1 N14 89.37(7) 2_565 2_565 ?
N4 Fe1 N14 92.24(7) 2_565 2_565 ?
N4 Fe1 N14 87.76(7) . 2_565 ?
N20 Fe1 N14 89.37(7) . . ?
N20 Fe1 N14 90.63(7) 2_565 . ?
N4 Fe1 N14 87.76(7) 2_565 . ?
N4 Fe1 N14 92.24(7) . . ?
N14 Fe1 N14 180.00(8) 2_565 . ?
O13 Cl1 O11 115.9(16) . . ?
O13 Cl1 O4 121.2(10) . . ?
O11 Cl1 O4 102.6(9) . . ?
O13 Cl1 O2 105.0(14) . . ?
O11 Cl1 O2 99.6(9) . . ?
O4 Cl1 O2 110.5(4) . . ?
O13 Cl1 O12 107.7(16) . . ?
O11 Cl1 O12 111.2(10) . . ?
O4 Cl1 O12 96.6(8) . . ?
O2 Cl1 O12 15.9(7) . . ?
O13 Cl1 O14 107.6(12) . . ?
O11 Cl1 O14 107.2(12) . . ?
O4 Cl1 O14 14.5(9) . . ?
O2 Cl1 O14 121.9(8) . . ?
O12 Cl1 O14 106.9(11) . . ?
O13 Cl1 O1 100.5(14) . . ?
O11 Cl1 O1 15.8(10) . . ?
O4 Cl1 O1 110.1(5) . . ?
O2 Cl1 O1 108.7(4) . . ?
O12 Cl1 O1 122.4(8) . . ?
O14 Cl1 O1 110.9(10) . . ?
O13 Cl1 O3 10.5(13) . . ?
O11 Cl1 O3 123.2(11) . . ?
O4 Cl1 O3 110.9(4) . . ?
O2 Cl1 O3 109.2(5) . . ?
O12 Cl1 O3 109.0(9) . . ?
O14 Cl1 O3 97.5(9) . . ?
O1 Cl1 O3 107.4(5) . . ?
C4 N1 N2 101.68(13) . . ?
N3 N2 N1 114.95(13) . . ?
N3 N2 C1 122.85(14) . . ?
N1 N2 C1 122.01(14) . . ?
N2 N3 N4 104.49(13) . . ?
N3 N4 C4 107.11(13) . . ?
N3 N4 Fe1 122.42(11) . . ?
C4 N4 Fe1 130.21(11) . . ?
N2 C1 C2 110.52(14) . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 113.43(14) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 C3 C2 111.76(17) 2_654 . ?
C3 C3 H3A 109.3 2_654 . ?
C2 C3 H3A 109.3 . . ?
C3 C3 H3B 109.3 2_654 . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 N4 111.77(15) . . ?
N1 C4 H4 124.1 . . ?
N4 C4 H4 124.1 . . ?
C14 N11 N12 102.12(14) . . ?
N13 N12 N11 114.09(14) . . ?
N13 N12 C11 122.68(13) . . ?
N11 N12 C11 122.84(13) . . ?
N12 N13 N14 105.04(13) . . ?
N13 N14 C14 106.95(13) . . ?
N13 N14 Fe1 124.04(11) . . ?
C14 N14 Fe1 128.27(12) . . ?
N12 C11 C12 110.40(13) . . ?
N12 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N12 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.58(14) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C13 C13 C12 113.47(17) 2_566 . ?
C13 C13 H13A 108.9 2_566 . ?
C12 C13 H13A 108.9 . . ?
C13 C13 H13B 108.9 2_566 . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
N11 C14 N14 111.80(15) . . ?
N11 C14 H14 124.1 . . ?
N14 C14 H14 124.1 . . ?
C20 N20 Fe1 174.34(13) . . ?
N20 C20 C21 179.35(17) . . ?
C20 C21 C22 112.49(14) . . ?
C20 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 N2 N3 0.21(17) . . . . ?
C4 N1 N2 C1 175.27(14) . . . . ?
N1 N2 N3 N4 0.10(17) . . . . ?
C1 N2 N3 N4 -174.92(13) . . . . ?
N2 N3 N4 C4 -0.37(16) . . . . ?
N2 N3 N4 Fe1 174.36(9) . . . . ?
N20 Fe1 N4 N3 -132.55(12) . . . . ?
N20 Fe1 N4 N3 47.45(12) 2_565 . . . ?
N4 Fe1 N4 N3 92(100) 2_565 . . . ?
N14 Fe1 N4 N3 -41.89(12) 2_565 . . . ?
N14 Fe1 N4 N3 138.11(12) . . . . ?
N20 Fe1 N4 C4 40.85(15) . . . . ?
N20 Fe1 N4 C4 -139.15(14) 2_565 . . . ?
N4 Fe1 N4 C4 -94(100) 2_565 . . . ?
N14 Fe1 N4 C4 131.51(14) 2_565 . . . ?
N14 Fe1 N4 C4 -48.49(14) . . . . ?
N3 N2 C1 C2 103.85(17) . . . . ?
N1 N2 C1 C2 -70.82(19) . . . . ?
N2 C1 C2 C3 -62.84(19) . . . . ?
C1 C2 C3 C3 -174.76(17) . . . 2_654 ?
N2 N1 C4 N4 -0.44(17) . . . . ?
N3 N4 C4 N1 0.53(18) . . . . ?
Fe1 N4 C4 N1 -173.64(11) . . . . ?
C14 N11 N12 N13 0.43(17) . . . . ?
C14 N11 N12 C11 173.42(14) . . . . ?
N11 N12 N13 N14 -0.51(17) . . . . ?
C11 N12 N13 N14 -173.51(13) . . . . ?
N12 N13 N14 C14 0.36(16) . . . . ?
N12 N13 N14 Fe1 171.19(9) . . . . ?
N20 Fe1 N14 N13 -16.23(12) . . . . ?
N20 Fe1 N14 N13 163.77(12) 2_565 . . . ?
N4 Fe1 N14 N13 -106.98(13) 2_565 . . . ?
N4 Fe1 N14 N13 73.02(13) . . . . ?
N14 Fe1 N14 N13 -147(100) 2_565 . . . ?
N20 Fe1 N14 C14 152.57(14) . . . . ?
N20 Fe1 N14 C14 -27.43(14) 2_565 . . . ?
N4 Fe1 N14 C14 61.82(14) 2_565 . . . ?
N4 Fe1 N14 C14 -118.18(14) . . . . ?
N14 Fe1 N14 C14 22(100) 2_565 . . . ?
N13 N12 C11 C12 106.48(16) . . . . ?
N11 N12 C11 C12 -65.91(19) . . . . ?
N12 C11 C12 C13 -57.94(18) . . . . ?
C11 C12 C13 C13 -65.6(2) . . . 2_566 ?
N12 N11 C14 N14 -0.18(17) . . . . ?
N13 N14 C14 N11 -0.12(18) . . . . ?
Fe1 N14 C14 N11 -170.43(11) . . . . ?
N20 Fe1 N20 C20 -4(100) 2_565 . . . ?
N4 Fe1 N20 C20 121.0(13) 2_565 . . . ?
N4 Fe1 N20 C20 -59.0(13) . . . . ?
N14 Fe1 N20 C20 -146.8(13) 2_565 . . . ?
N14 Fe1 N20 C20 33.2(13) . . . . ?
Fe1 N20 C20 C21 -38(16) . . . . ?
N20 C20 C21 C22 -126(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.063


#====== end of cif


