#==============================================================================
data_global
#==============================================================================

_publ_contact_author_name         'Paul D. Beer' 
_publ_contact_author_address 
; 
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA, UK.
; 
 
_publ_contact_author_email        'paul.beer@chem.ox.ac.uk' 
_publ_requested_journal           'Beilstein J. Org. Chem.' 
 
_publ_section_title 
; 
A Ferrocene Redox-Active Triazolium Macrocycle that Binds and
Senses Chloride
; 
 
loop_ 
 _publ_author_name 
 _publ_author_address 
 'Nicholas G. White'
;    
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford, OX1 3TA, UK.
;
'Paul D. Beer'
; 
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA, UK.
; 


_publ_section_abstract 
; 
A ferrocene bis-triazole macrocycle has been synthesised in good yield by the
Eglinton coupling of an acyclic bis-alkyne precursor and characterised in the 
solid state by X-ray crystallography.  Alkylation gives the corresponding 
triazolium macrocycle, which binds chloride and benzoate strongly in CD3CN 
solution via favourable charge assisted C-H...anion interactions, as evidenced 
by 1H NMR titration experiments.  Preliminary electrochemical studies show 
reveal the redox-active macrocycle is capable of sensing chloride in CH3CN 
solution.
; 

#==============================================================================
data_3
#==============================================================================
 
_exptl_special_details 
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
; 
_refine_special_details 
; 
The crystal was twinned.  A twin law was found and included
using the ROTAX feature of CRYSTALS.
; 

_cell_length_a                    11.7117(2)
_cell_length_b                    11.9571(2)
_cell_length_c                    32.2561(6)
_cell_angle_alpha                 90
_cell_angle_beta                  92.6441(14)
_cell_angle_gamma                 90
_cell_volume                      4512.27(14)
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 21/c ' 
_symmetry_space_group_name_Hall   '-P 2ybc' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 'x,-y+1/2,z+1/2'
 '-x,y+1/2,-z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0020   0.0020   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0040   0.0030  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Fe      0.2960   0.8010  11.7695   4.7611   7.3573   0.3072   3.5222  15.3535
   2.3045  76.8805   1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    8

# Given Formula = C26 H26 Fe1 N6 
# Dc =      1.41 Fooo =   2000.00 Mu =      6.95 M =    956.76
# Found Formula = C26 H26 Fe1 N6 
# Dc =      1.41 FOOO =   2000.00 Mu =      6.95 M =    956.76

_chemical_formula_sum             'C26 H26 Fe1 N6'
_chemical_formula_moiety          'C26 H26 Fe1 N6'
_chemical_compound_source           synthesized
_chemical_formula_weight            478.38
 
 
_cell_measurement_reflns_used        18186
_cell_measurement_theta_min              2
_cell_measurement_theta_max             30
_cell_measurement_temperature          100
 
_exptl_crystal_description        'prism' 
_exptl_crystal_colour             'orange' 
_exptl_crystal_size_min           0.050 
_exptl_crystal_size_mid           0.070 
_exptl_crystal_size_max           0.250 
 
_exptl_crystal_density_diffrn     1.408 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              2000 
_exptl_absorpt_coefficient_mu     0.695 
 
# Sheldrick geometric approximatio 0.95 0.97 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'CrysAlis, (Oxford Diffraction, 2002)' 
_exptl_absorpt_correction_T_min   0.389 
_exptl_absorpt_correction_T_max   1.00 
_diffrn_measurement_device        'synchrotron' 
_diffrn_radiation_monochromator   'synchrotron' 
_diffrn_radiation_type            'Synchrotron'
_diffrn_radiation_wavelength          0.68890
_diffrn_measurement_method        ω/2θ 
 
_computing_data_collection        'CrystalClear (Rigaku, 1997--2002)' 
_computing_cell_refinement        'CrystalClear (Rigaku, 1997--2002)' 
_computing_data_reduction         'CrysAlis, (Oxford Diffraction, 2002)' 
_computing_structure_solution     'Superflip (Palatinus & Chapuis, 2007)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)'  
 
_diffrn_standards_interval_time   0 
_diffrn_standards_interval_count  0 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         0 
 
_diffrn_ambient_temperature        100
_diffrn_reflns_number             47035 
_reflns_number_total              13163 
_diffrn_reflns_av_R_equivalents   0.036 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 13163 
# Theoretical number of reflections is about 14933 
 
 
_diffrn_reflns_theta_min          1.687 
_diffrn_reflns_theta_max          30.241 
_diffrn_measured_fraction_theta_max 0.891 
 
_diffrn_reflns_theta_full         25.100 
_diffrn_measured_fraction_theta_full 0.979 
 
 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -44 
_diffrn_reflns_limit_l_max        46 
_reflns_limit_h_min               -16 
_reflns_limit_h_max               16 
_reflns_limit_k_min               0 
_reflns_limit_k_max               16 
_reflns_limit_l_min               0 
_reflns_limit_l_max               46 
 
_oxford_diffrn_Wilson_B_factor    1.54 
_oxford_diffrn_Wilson_scale       0.08 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.65 
_refine_diff_density_max          1.05 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-3.0\s(I)
_refine_ls_number_reflns          7393 
_refine_ls_number_restraints      52 
_refine_ls_number_parameters      605 
_oxford_refine_ls_R_factor_ref    0.0673 
_refine_ls_wR_factor_ref          0.1525 
_refine_ls_goodness_of_fit_ref    1.0444 
_refine_ls_shift/su_max           0.0008335 
_refine_ls_shift/su_mean          0.0000221 
 
 
# The values computed from all data 
_oxford_reflns_number_all         7393 
_refine_ls_R_factor_all           0.0673 
_refine_ls_wR_factor_all          0.1525 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 7068 
_refine_ls_R_factor_gt            0.0656 
_refine_ls_wR_factor_gt           0.1523 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment    constr         # none, undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.324E+04 0.469E+04 0.284E+04 0.119E+04 133. 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
CrystalClear: An Integrated Program for the Collection and Processing of 
Area Detector Data, Rigaku Corporation, 1997--2002. 

Oxford Diffraction, (2010). CrysAlisPro. 

Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 

Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 

Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.04621(6) 0.59746(6) 0.60010(2) 0.0251 1.0000 Uani . . . . . . 
C2 C 0.1508(5) 0.4877(5) 0.63223(17) 0.0346 1.0000 Uani . . . . . . 
C3 C 0.1195(5) 0.4438(4) 0.59274(17) 0.0335 1.0000 Uani . . . . . . 
C4 C -0.0024(4) 0.4349(4) 0.58939(16) 0.0270 1.0000 Uani . . . . . . 
C5 C -0.0459(4) 0.4760(4) 0.62698(15) 0.0252 1.0000 Uani . . . . . . 
C6 C 0.0488(4) 0.5068(4) 0.65358(16) 0.0301 1.0000 Uani . . . . . . 
C7 C -0.1689(4) 0.4817(4) 0.63734(15) 0.0253 1.0000 Uani . . . . . . 
N8 N -0.1980(3) 0.3868(3) 0.66399(12) 0.0215 1.0000 Uani . . . . . . 
N9 N -0.2448(4) 0.2935(4) 0.64753(13) 0.0316 1.0000 Uani . . . . . . 
N10 N -0.2502(4) 0.2207(4) 0.67812(14) 0.0323 1.0000 Uani . . . . . . 
C11 C -0.2071(4) 0.2664(4) 0.71360(16) 0.0265 1.0000 Uani . . . . . . 
C12 C -0.1734(4) 0.3741(4) 0.70468(15) 0.0247 1.0000 Uani . . . . . . 
C13 C -0.2045(5) 0.2057(5) 0.75401(17) 0.0370 1.0000 Uani . . . . . . 
C14 C -0.2843(5) 0.2544(6) 0.78499(17) 0.0456 1.0000 Uani . . . . . . 
C15 C -0.4073(5) 0.2595(6) 0.7696(2) 0.0496 1.0000 Uani . . . . . . 
C16 C -0.4364(5) 0.3442(5) 0.73758(16) 0.0359 1.0000 Uani . . . . . . 
C17 C -0.4613(4) 0.4135(5) 0.71219(15) 0.0295 1.0000 Uani . . . . . . 
C18 C -0.4841(4) 0.4930(4) 0.68188(14) 0.0262 1.0000 Uani . U . . . . 
C19 C -0.5007(5) 0.5615(4) 0.65560(15) 0.0294 1.0000 Uani . U . . . . 
C20 C -0.5134(5) 0.6497(5) 0.62338(16) 0.0363 1.0000 Uani . U . . . . 
C21 C -0.5598(4) 0.6081(5) 0.58158(16) 0.0329 1.0000 Uani . U . . . . 
C22 C -0.4916(5) 0.5135(5) 0.56290(16) 0.0324 1.0000 Uani . U . . . . 
C23 C -0.3755(5) 0.5412(5) 0.54840(14) 0.0306 1.0000 Uani . . . . . . 
N24 N -0.3134(4) 0.4598(4) 0.53021(14) 0.0413 1.0000 Uani . . . . . . 
N25 N -0.2156(4) 0.5017(5) 0.51952(14) 0.0468 1.0000 Uani . . . . . . 
N26 N -0.2128(4) 0.6098(4) 0.53029(14) 0.0398 1.0000 Uani . . . . . . 
C27 C -0.3110(5) 0.6369(5) 0.54811(17) 0.0360 1.0000 Uani . . . . . . 
C28 C -0.1135(5) 0.6763(7) 0.52060(19) 0.0554 1.0000 Uani . . . . . . 
C29 C -0.0286(5) 0.6993(5) 0.55566(18) 0.0376 1.0000 Uani . . . . . . 
C30 C 0.0916(5) 0.6977(4) 0.55244(17) 0.0359 1.0000 Uani . . . . . . 
C31 C 0.1428(5) 0.7362(4) 0.5908(2) 0.0399 1.0000 Uani . . . . . . 
C32 C 0.0543(5) 0.7617(4) 0.6178(2) 0.0417 1.0000 Uani . . . . . . 
C33 C -0.0509(5) 0.7396(4) 0.59627(18) 0.0382 1.0000 Uani . . . . . . 
Fe34 Fe 0.41462(6) 1.08922(6) 0.60312(2) 0.0262 1.0000 Uani . . . . . . 
C35 C 0.3207(5) 0.9681(5) 0.63058(17) 0.0354 1.0000 Uani . . . . . . 
C36 C 0.4232(4) 0.9903(4) 0.65482(16) 0.0292 1.0000 Uani . . . . . . 
C37 C 0.5172(4) 0.9699(4) 0.62956(15) 0.0272 1.0000 Uani . . . . . . 
C38 C 0.4736(5) 0.9329(4) 0.59005(15) 0.0304 1.0000 Uani . . . . . . 
C39 C 0.3522(5) 0.9331(4) 0.59050(17) 0.0358 1.0000 Uani . . . . . . 
C40 C 0.6419(4) 0.9819(4) 0.64208(16) 0.0284 1.0000 Uani . . . . . . 
N41 N 0.6799(3) 0.8855(3) 0.66783(12) 0.0228 1.0000 Uani . . . . . . 
N42 N 0.7263(4) 0.7953(4) 0.65039(14) 0.0328 1.0000 Uani . . . . . . 
N43 N 0.7413(4) 0.7199(4) 0.67966(14) 0.0335 1.0000 Uani . . . . . . 
C44 C 0.7038(4) 0.7610(4) 0.71574(16) 0.0289 1.0000 Uani . U . . . . 
C45 C 0.6648(4) 0.8678(4) 0.70815(15) 0.0251 1.0000 Uani . . . . . . 
C46 C 0.7111(5) 0.6955(5) 0.75510(18) 0.0405 1.0000 Uani D U . . . . 
C47 C 0.3455(5) 1.1928(4) 0.55837(16) 0.0331 1.0000 Uani . . . . . . 
C48 C 0.4670(5) 1.1946(4) 0.55806(15) 0.0299 1.0000 Uani . . . . . . 
C49 C 0.5099(5) 1.2313(4) 0.59767(16) 0.0318 1.0000 Uani . . . . . . 
C50 C 0.4150(5) 1.2516(4) 0.62256(17) 0.0366 1.0000 Uani . . . . . . 
C51 C 0.3135(5) 1.2267(4) 0.59830(18) 0.0383 1.0000 Uani . . . . . . 
C52 C 0.5321(5) 1.1713(5) 0.52002(16) 0.0402 1.0000 Uani . . . . . . 
N53 N 0.6472(4) 1.1270(4) 0.52700(13) 0.0327 1.0000 Uani . . . . . . 
N54 N 0.6679(4) 1.0167(4) 0.52141(14) 0.0397 1.0000 Uani . . . . . . 
N55 N 0.7794(4) 1.0029(4) 0.52653(14) 0.0404 1.0000 Uani . . . . . . 
C56 C 0.8296(5) 1.1044(5) 0.53525(14) 0.0328 1.0000 Uani . . . . . . 
C57 C 0.7452(5) 1.1829(5) 0.53551(16) 0.0362 1.0000 Uani . . . . . . 
C58 C 0.9567(5) 1.1153(5) 0.54233(16) 0.0350 1.0000 Uani . . . . . . 
C59 C 1.0007(5) 1.0531(5) 0.58089(16) 0.0353 1.0000 Uani . . . . . . 
C60 C 0.9648(5) 1.1125(5) 0.62032(16) 0.0337 1.0000 Uani . . . . . . 
C61 C 0.9697(5) 1.0411(5) 0.65731(16) 0.0315 1.0000 Uani . . . . . . 
C62 C 0.9624(4) 0.9811(5) 0.68690(16) 0.0310 1.0000 Uani . . . . . . 
C63 C 0.9487(4) 0.9112(5) 0.72036(16) 0.0326 1.0000 Uani . . . . . . 
C64 C 0.9286(5) 0.8482(5) 0.74804(17) 0.0372 1.0000 Uani . U . . . . 
C65 C 0.9048(5) 0.7712(5) 0.78199(19) 0.0449 1.0000 Uani D U . . . . 
C166 C 0.7860(8) 0.7538(9) 0.7908(3) 0.0440 0.6000 Uani D U . . 2 . 
C66 C 0.8317(9) 0.6701(10) 0.7687(4) 0.0330 0.4000 Uani D U . . 1 . 
H21 H 0.2280 0.5022 0.6425 0.0420 1.0000 Uiso R . . . . . 
H31 H 0.1730 0.4280 0.5700 0.0417 1.0000 Uiso R . . . . . 
H41 H -0.0493 0.4064 0.5650 0.0349 1.0000 Uiso R . . . . . 
H61 H 0.0483 0.5373 0.6820 0.0426 1.0000 Uiso R . . . . . 
H72 H -0.1786 0.5502 0.6538 0.0315 1.0000 Uiso R . . . . . 
H71 H -0.2171 0.4830 0.6117 0.0313 1.0000 Uiso R . . . . . 
H121 H -0.1409 0.4282 0.7240 0.0369 1.0000 Uiso R . . . . . 
H132 H -0.1280 0.2051 0.7668 0.0445 1.0000 Uiso R . . . . . 
H131 H -0.2292 0.1301 0.7481 0.0427 1.0000 Uiso R . . . . . 
H141 H -0.2787 0.2141 0.8115 0.0515 1.0000 Uiso R . . . . . 
H142 H -0.2615 0.3329 0.7901 0.0510 1.0000 Uiso R . . . . . 
H151 H -0.4577 0.2664 0.7925 0.0567 1.0000 Uiso R . . . . . 
H152 H -0.4244 0.1854 0.7551 0.0576 1.0000 Uiso R . . . . . 
H201 H -0.5642 0.7080 0.6330 0.0371 1.0000 Uiso R . . . . . 
H202 H -0.4372 0.6831 0.6198 0.0359 1.0000 Uiso R . . . . . 
H211 H -0.6347 0.5781 0.5863 0.0365 1.0000 Uiso R . . . . . 
H212 H -0.5670 0.6685 0.5608 0.0365 1.0000 Uiso R . . . . . 
H222 H -0.4831 0.4552 0.5835 0.0436 1.0000 Uiso R . . . . . 
H221 H -0.5358 0.4871 0.5385 0.0430 1.0000 Uiso R . . . . . 
H271 H -0.3293 0.7068 0.5584 0.0427 1.0000 Uiso R . . . . . 
H282 H -0.1423 0.7469 0.5088 0.0767 1.0000 Uiso R . . . . . 
H281 H -0.0736 0.6367 0.4989 0.0757 1.0000 Uiso R . . . . . 
H301 H 0.1305 0.6712 0.5282 0.0449 1.0000 Uiso R . . . . . 
H311 H 0.2256 0.7452 0.5978 0.0549 1.0000 Uiso R . . . . . 
H321 H 0.0621 0.7882 0.6472 0.0458 1.0000 Uiso R . . . . . 
H331 H -0.1277 0.7450 0.6066 0.0495 1.0000 Uiso R . . . . . 
H351 H 0.2413 0.9740 0.6402 0.0391 1.0000 Uiso R . . . . . 
H361 H 0.4270 1.0156 0.6838 0.0395 1.0000 Uiso R . . . . . 
H381 H 0.5211 0.9111 0.5673 0.0408 1.0000 Uiso R . . . . . 
H391 H 0.2981 0.9149 0.5672 0.0517 1.0000 Uiso R . . . . . 
H402 H 0.6521 1.0486 0.6589 0.0414 1.0000 Uiso R . . . . . 
H401 H 0.6895 0.9855 0.6184 0.0417 1.0000 Uiso R . . . . . 
H451 H 0.6353 0.9180 0.7264 0.0369 1.0000 Uiso R . . . . . 
H471 H 0.2944 1.1695 0.5352 0.0371 1.0000 Uiso R . . . . . 
H491 H 0.5902 1.2451 0.6061 0.0442 1.0000 Uiso R . . . . . 
H501 H 0.4166 1.2807 0.6521 0.0431 1.0000 Uiso R . . . . . 
H511 H 0.2360 1.2372 0.6079 0.0484 1.0000 Uiso R . . . . . 
H521 H 0.5378 1.2424 0.5056 0.0555 1.0000 Uiso R . . . . . 
H522 H 0.4888 1.1195 0.5023 0.0553 1.0000 Uiso R . . . . . 
H571 H 0.7568 1.2596 0.5417 0.0507 1.0000 Uiso R . . . . . 
H581 H 0.9765 1.1955 0.5459 0.0454 1.0000 Uiso R . . . . . 
H582 H 0.9941 1.0873 0.5187 0.0451 1.0000 Uiso R . . . . . 
H592 H 1.0822 1.0526 0.5817 0.0431 1.0000 Uiso R . . . . . 
H591 H 0.9703 0.9751 0.5811 0.0433 1.0000 Uiso R . . . . . 
H601 H 1.0166 1.1763 0.6253 0.0450 1.0000 Uiso R . . . . . 
H602 H 0.8877 1.1398 0.6158 0.0448 1.0000 Uiso R . . . . . 
H1661 H 0.7796 0.7171 0.8173 0.0418 0.6000 Uiso R . . . 2 . 
H1662 H 0.7557 0.8323 0.7947 0.0423 0.6000 Uiso R . . . 2 . 
H661 H 0.8298 0.6207 0.7931 0.0628 0.4000 Uiso R . . . 1 . 
H662 H 0.8688 0.6330 0.7467 0.0631 0.4000 Uiso R . . . 1 . 
H651 H 0.8657 0.8106 0.8026 0.0619 0.4000 Uiso R . . . 1 . 
H652 H 0.9764 0.7458 0.7934 0.0619 0.4000 Uiso R . . . 1 . 
H653 H 0.9442 0.7962 0.8075 0.0619 0.6000 Uiso . . . . 2 . 
H654 H 0.9361 0.6976 0.7762 0.0619 0.6000 Uiso . . . . 2 . 
H461 H 0.6355 0.6853 0.7653 0.0595 0.6000 Uiso . . . . 2 . 
H462 H 0.7437 0.6242 0.7509 0.0595 0.6000 Uiso . . . . 2 . 
H463 H 0.6789 0.7392 0.7762 0.0595 0.4000 Uiso R . . . 1 . 
H464 H 0.6687 0.6282 0.7514 0.0595 0.4000 Uiso R . . . 1 . 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 4.14(7) 

loop_
    _oxford_twin_element_scale_factors
         0.924(2) 
         0.076(2) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Fe1 . C2 . 2.045(5)    yes
Fe1 . C3 . 2.046(5)    yes
Fe1 . C4 . 2.051(5)    yes
Fe1 . C5 . 2.027(5)    yes
Fe1 . C6 . 2.037(5)    yes
Fe1 . C29 . 2.047(5)    yes
Fe1 . C30 . 2.039(5)    yes
Fe1 . C31 . 2.038(5)    yes
Fe1 . C32 . 2.046(5)    yes
Fe1 . C33 . 2.046(5)    yes
C2 . C3 . 1.411(8)    yes
C2 . C6 . 1.425(7)    yes
C2 . H21 . 0.964    no
C3 . C4 . 1.431(7)    yes
C3 . H31 . 1.005    no
C4 . C5 . 1.424(7)    yes
C4 . H41 . 0.998    no
C5 . C6 . 1.419(7)    yes
C5 . C7 . 1.496(7)    yes
C6 . H61 . 0.986    no
C7 . N8 . 1.472(6)    yes
C7 . H72 . 0.985    no
C7 . H71 . 0.980    no
N8 . N9 . 1.342(6)    yes
N8 . C12 . 1.339(6)    yes
N9 . N10 . 1.319(6)    yes
N10 . C11 . 1.345(7)    yes
C11 . C12 . 1.380(7)    yes
C11 . C13 . 1.492(7)    yes
C12 . H121 . 0.965    no
C13 . C14 . 1.516(8)    yes
C13 . H132 . 0.970    no
C13 . H131 . 0.965    no
C14 . C15 . 1.503(8)    yes
C14 . H141 . 0.980    no
C14 . H142 . 0.987    no
C15 . C16 . 1.475(7)    yes
C15 . H151 . 0.969    no
C15 . H152 . 1.017    no
C16 . C17 . 1.192(7)    yes
C17 . C18 . 1.381(7)    yes
C18 . C19 . 1.189(7)    yes
C19 . C20 . 1.483(7)    yes
C20 . C21 . 1.514(7)    yes
C20 . H201 . 0.977    no
C20 . H202 . 0.989    no
C21 . C22 . 1.525(7)    yes
C21 . H211 . 0.967    no
C21 . H212 . 0.987    no
C22 . C23 . 1.494(7)    yes
C22 . H222 . 0.966    no
C22 . H221 . 0.975    no
C23 . N24 . 1.364(7)    yes
C23 . C27 . 1.372(8)    yes
N24 . N25 . 1.310(7)    yes
N25 . N26 . 1.339(7)    yes
N26 . C27 . 1.349(7)    yes
N26 . C28 . 1.454(8)    yes
C27 . H271 . 0.928    no
C28 . C29 . 1.496(9)    yes
C28 . H282 . 0.981    no
C28 . H281 . 0.982    no
C29 . C30 . 1.417(8)    yes
C29 . C33 . 1.431(8)    yes
C30 . C31 . 1.427(8)    yes
C30 . H301 . 0.975    no
C31 . C32 . 1.417(8)    yes
C31 . H311 . 0.991    no
C32 . C33 . 1.411(8)    yes
C32 . H321 . 1.000    no
C33 . H331 . 0.975    no
Fe34 . C35 . 2.046(5)    yes
Fe34 . C36 . 2.043(5)    yes
Fe34 . C37 . 2.027(5)    yes
Fe34 . C38 . 2.044(5)    yes
Fe34 . C39 . 2.039(5)    yes
Fe34 . C47 . 2.041(5)    yes
Fe34 . C48 . 2.039(5)    yes
Fe34 . C49 . 2.044(5)    yes
Fe34 . C50 . 2.041(5)    yes
Fe34 . C51 . 2.028(5)    yes
C35 . C36 . 1.428(7)    yes
C35 . C39 . 1.424(8)    yes
C35 . H351 . 0.996    no
C36 . C37 . 1.421(7)    yes
C36 . H361 . 0.980    no
C37 . C38 . 1.422(7)    yes
C37 . C40 . 1.504(7)    yes
C38 . C39 . 1.422(8)    yes
C38 . H381 . 0.976    no
C39 . H391 . 0.984    no
C40 . N41 . 1.477(6)    yes
C40 . H402 . 0.969    no
C40 . H401 . 0.966    no
N41 . N42 . 1.344(6)    yes
N41 . C45 . 1.337(6)    yes
N42 . N43 . 1.311(6)    yes
N43 . C44 . 1.355(7)    yes
C44 . C45 . 1.374(7)    yes
C44 . C46 . 1.491(7)    yes
C45 . H451 . 0.921    no
C46 . C66 . 1.491(11)    yes
C46 . H463 . 0.950    no
C46 . H464 . 0.950    no
C47 . C48 . 1.423(8)    yes
C47 . C51 . 1.417(8)    yes
C47 . H471 . 0.976    no
C48 . C49 . 1.421(7)    yes
C48 . C52 . 1.501(7)    yes
C49 . C50 . 1.421(8)    yes
C49 . H491 . 0.981    no
C50 . C51 . 1.424(8)    yes
C50 . H501 . 1.015    no
C51 . H511 . 0.981    no
C52 . N53 . 1.455(7)    yes
C52 . H521 . 0.974    no
C52 . H522 . 0.971    no
N53 . N54 . 1.354(6)    yes
N53 . C57 . 1.346(7)    yes
N54 . N55 . 1.319(7)    yes
N55 . C56 . 1.372(7)    yes
C56 . C57 . 1.363(8)    yes
C56 . C58 . 1.502(8)    yes
C57 . H571 . 0.947    no
C58 . C59 . 1.519(7)    yes
C58 . H581 . 0.992    no
C58 . H582 . 0.956    no
C59 . C60 . 1.532(7)    yes
C59 . H592 . 0.954    no
C59 . H591 . 0.998    no
C60 . C61 . 1.466(7)    yes
C60 . H601 . 0.983    no
C60 . H602 . 0.965    no
C61 . C62 . 1.200(7)    yes
C62 . C63 . 1.380(7)    yes
C63 . C64 . 1.200(8)    yes
C64 . C65 . 1.467(8)    yes
C65 . C66 . 1.532(12)    yes
C65 . H651 . 0.950    no
C65 . H652 . 0.950    no
C166 . H1661 . 0.966    no
C166 . H1662 . 1.014    no
C66 . H661 . 0.985    no
C66 . H662 . 0.959    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
C2 . Fe1 . C3 . 40.3(2)    yes
C2 . Fe1 . C4 . 68.4(2)    yes
C3 . Fe1 . C4 . 40.9(2)    yes
C2 . Fe1 . C5 . 69.0(2)    yes
C3 . Fe1 . C5 . 68.9(2)    yes
C4 . Fe1 . C5 . 40.88(19)    yes
C2 . Fe1 . C6 . 40.9(2)    yes
C3 . Fe1 . C6 . 68.3(2)    yes
C4 . Fe1 . C6 . 68.4(2)    yes
C5 . Fe1 . C6 . 40.9(2)    yes
C2 . Fe1 . C29 . 164.6(2)    yes
C3 . Fe1 . C29 . 128.4(2)    yes
C4 . Fe1 . C29 . 109.8(2)    yes
C5 . Fe1 . C29 . 120.4(2)    yes
C6 . Fe1 . C29 . 154.0(2)    yes
C2 . Fe1 . C30 . 126.0(2)    yes
C3 . Fe1 . C30 . 108.4(2)    yes
C4 . Fe1 . C30 . 120.7(2)    yes
C5 . Fe1 . C30 . 154.9(2)    yes
C6 . Fe1 . C30 . 163.2(2)    yes
C2 . Fe1 . C31 . 105.9(2)    yes
C3 . Fe1 . C31 . 118.4(2)    yes
C4 . Fe1 . C31 . 154.0(2)    yes
C5 . Fe1 . C31 . 162.9(2)    yes
C6 . Fe1 . C31 . 124.8(2)    yes
C2 . Fe1 . C32 . 117.1(2)    yes
C3 . Fe1 . C32 . 151.6(2)    yes
C4 . Fe1 . C32 . 165.0(2)    yes
C5 . Fe1 . C32 . 125.9(2)    yes
C6 . Fe1 . C32 . 106.0(2)    yes
C2 . Fe1 . C33 . 151.9(2)    yes
C3 . Fe1 . C33 . 166.9(2)    yes
C4 . Fe1 . C33 . 128.9(2)    yes
C5 . Fe1 . C33 . 108.4(2)    yes
C6 . Fe1 . C33 . 118.7(2)    yes
C29 . Fe1 . C30 . 40.6(2)    yes
C29 . Fe1 . C31 . 68.6(2)    yes
C30 . Fe1 . C31 . 41.0(2)    yes
C29 . Fe1 . C32 . 68.7(3)    yes
C30 . Fe1 . C32 . 68.7(2)    yes
C31 . Fe1 . C32 . 40.6(2)    yes
C29 . Fe1 . C33 . 40.9(2)    yes
C30 . Fe1 . C33 . 68.3(2)    yes
C31 . Fe1 . C33 . 68.0(2)    yes
C32 . Fe1 . C33 . 40.3(2)    yes
Fe1 . C2 . C3 . 69.9(3)    yes
Fe1 . C2 . C6 . 69.2(3)    yes
C3 . C2 . C6 . 107.9(5)    yes
Fe1 . C2 . H21 . 126.0    no
C3 . C2 . H21 . 125.3    no
C6 . C2 . H21 . 126.8    no
C2 . C3 . Fe1 . 69.8(3)    yes
C2 . C3 . C4 . 108.3(5)    yes
Fe1 . C3 . C4 . 69.7(3)    yes
C2 . C3 . H31 . 125.8    no
Fe1 . C3 . H31 . 122.2    no
C4 . C3 . H31 . 125.8    no
C3 . C4 . Fe1 . 69.4(3)    yes
C3 . C4 . C5 . 107.7(5)    yes
Fe1 . C4 . C5 . 68.7(3)    yes
C3 . C4 . H41 . 126.6    no
Fe1 . C4 . H41 . 126.5    no
C5 . C4 . H41 . 125.7    no
C4 . C5 . Fe1 . 70.4(3)    yes
C4 . C5 . C6 . 107.7(4)    yes
Fe1 . C5 . C6 . 69.9(3)    yes
C4 . C5 . C7 . 126.3(4)    yes
Fe1 . C5 . C7 . 126.9(3)    yes
C6 . C5 . C7 . 126.0(4)    yes
C2 . C6 . C5 . 108.4(5)    yes
C2 . C6 . Fe1 . 69.9(3)    yes
C5 . C6 . Fe1 . 69.2(3)    yes
C2 . C6 . H61 . 123.3    no
C5 . C6 . H61 . 128.3    no
Fe1 . C6 . H61 . 126.1    no
C5 . C7 . N8 . 110.3(4)    yes
C5 . C7 . H72 . 107.1    no
N8 . C7 . H72 . 106.9    no
C5 . C7 . H71 . 109.6    no
N8 . C7 . H71 . 111.5    no
H72 . C7 . H71 . 111.5    no
C7 . N8 . N9 . 120.7(4)    yes
C7 . N8 . C12 . 127.9(4)    yes
N9 . N8 . C12 . 111.0(4)    yes
N8 . N9 . N10 . 106.6(4)    yes
N9 . N10 . C11 . 109.8(4)    yes
N10 . C11 . C12 . 107.6(4)    yes
N10 . C11 . C13 . 122.5(5)    yes
C12 . C11 . C13 . 129.9(5)    yes
C11 . C12 . N8 . 105.0(4)    yes
C11 . C12 . H121 . 126.8    no
N8 . C12 . H121 . 128.2    no
C11 . C13 . C14 . 113.6(5)    yes
C11 . C13 . H132 . 111.0    no
C14 . C13 . H132 . 107.9    no
C11 . C13 . H131 . 106.8    no
C14 . C13 . H131 . 107.6    no
H132 . C13 . H131 . 109.9    no
C13 . C14 . C15 . 114.1(5)    yes
C13 . C14 . H141 . 111.5    no
C15 . C14 . H141 . 109.4    no
C13 . C14 . H142 . 107.7    no
C15 . C14 . H142 . 105.3    no
H141 . C14 . H142 . 108.4    no
C14 . C15 . C16 . 116.5(5)    yes
C14 . C15 . H151 . 111.1    no
C16 . C15 . H151 . 110.2    no
C14 . C15 . H152 . 106.4    no
C16 . C15 . H152 . 104.0    no
H151 . C15 . H152 . 108.0    no
C15 . C16 . C17 . 178.8(6)    yes
C16 . C17 . C18 . 176.8(5)    yes
C17 . C18 . C19 . 178.3(5)    yes
C18 . C19 . C20 . 176.1(6)    yes
C19 . C20 . C21 . 114.2(5)    yes
C19 . C20 . H201 . 109.1    no
C21 . C20 . H201 . 108.6    no
C19 . C20 . H202 . 107.9    no
C21 . C20 . H202 . 108.5    no
H201 . C20 . H202 . 108.4    no
C20 . C21 . C22 . 115.0(4)    yes
C20 . C21 . H211 . 105.9    no
C22 . C21 . H211 . 106.4    no
C20 . C21 . H212 . 112.4    no
C22 . C21 . H212 . 107.7    no
H211 . C21 . H212 . 109.1    no
C21 . C22 . C23 . 117.4(5)    yes
C21 . C22 . H222 . 107.6    no
C23 . C22 . H222 . 108.0    no
C21 . C22 . H221 . 106.9    no
C23 . C22 . H221 . 106.0    no
H222 . C22 . H221 . 110.9    no
C22 . C23 . N24 . 119.2(5)    yes
C22 . C23 . C27 . 134.1(5)    yes
N24 . C23 . C27 . 106.7(5)    yes
C23 . N24 . N25 . 109.3(5)    yes
N24 . N25 . N26 . 108.2(5)    yes
N25 . N26 . C27 . 109.3(5)    yes
N25 . N26 . C28 . 118.9(5)    yes
C27 . N26 . C28 . 131.8(6)    yes
C23 . C27 . N26 . 106.5(5)    yes
C23 . C27 . H271 . 127.8    no
N26 . C27 . H271 . 125.8    no
N26 . C28 . C29 . 116.6(5)    yes
N26 . C28 . H282 . 106.9    no
C29 . C28 . H282 . 109.9    no
N26 . C28 . H281 . 107.6    no
C29 . C28 . H281 . 107.9    no
H282 . C28 . H281 . 107.7    no
C28 . C29 . Fe1 . 131.9(4)    yes
C28 . C29 . C30 . 124.8(5)    yes
Fe1 . C29 . C30 . 69.4(3)    yes
C28 . C29 . C33 . 127.6(5)    yes
Fe1 . C29 . C33 . 69.5(3)    yes
C30 . C29 . C33 . 107.2(5)    yes
C29 . C30 . Fe1 . 70.0(3)    yes
C29 . C30 . C31 . 108.2(5)    yes
Fe1 . C30 . C31 . 69.5(3)    yes
C29 . C30 . H301 . 124.4    no
Fe1 . C30 . H301 . 124.1    no
C31 . C30 . H301 . 127.3    no
C30 . C31 . Fe1 . 69.6(3)    yes
C30 . C31 . C32 . 108.2(5)    yes
Fe1 . C31 . C32 . 70.0(3)    yes
C30 . C31 . H311 . 126.8    no
Fe1 . C31 . H311 . 126.8    no
C32 . C31 . H311 . 125.0    no
C31 . C32 . Fe1 . 69.4(3)    yes
C31 . C32 . C33 . 107.7(5)    yes
Fe1 . C32 . C33 . 69.8(3)    yes
C31 . C32 . H321 . 127.8    no
Fe1 . C32 . H321 . 124.8    no
C33 . C32 . H321 . 124.5    no
C29 . C33 . C32 . 108.8(5)    yes
C29 . C33 . Fe1 . 69.6(3)    yes
C32 . C33 . Fe1 . 69.8(3)    yes
C29 . C33 . H331 . 123.1    no
C32 . C33 . H331 . 128.0    no
Fe1 . C33 . H331 . 123.5    no
C35 . Fe34 . C36 . 40.9(2)    yes
C35 . Fe34 . C37 . 68.9(2)    yes
C36 . Fe34 . C37 . 40.8(2)    yes
C35 . Fe34 . C38 . 68.6(2)    yes
C36 . Fe34 . C38 . 68.6(2)    yes
C37 . Fe34 . C38 . 40.88(19)    yes
C35 . Fe34 . C39 . 40.8(2)    yes
C36 . Fe34 . C39 . 68.7(2)    yes
C37 . Fe34 . C39 . 68.9(2)    yes
C38 . Fe34 . C39 . 40.8(2)    yes
C35 . Fe34 . C47 . 122.2(2)    yes
C36 . Fe34 . C47 . 158.7(2)    yes
C37 . Fe34 . C47 . 158.8(2)    yes
C38 . Fe34 . C47 . 122.4(2)    yes
C39 . Fe34 . C47 . 106.7(2)    yes
C35 . Fe34 . C48 . 158.7(2)    yes
C36 . Fe34 . C48 . 159.1(2)    yes
C37 . Fe34 . C48 . 122.9(2)    yes
C38 . Fe34 . C48 . 107.6(2)    yes
C39 . Fe34 . C48 . 122.7(2)    yes
C35 . Fe34 . C49 . 158.8(2)    yes
C36 . Fe34 . C49 . 123.0(2)    yes
C37 . Fe34 . C49 . 107.8(2)    yes
C38 . Fe34 . C49 . 123.5(2)    yes
C39 . Fe34 . C49 . 159.3(2)    yes
C35 . Fe34 . C50 . 122.3(2)    yes
C36 . Fe34 . C50 . 107.5(2)    yes
C37 . Fe34 . C50 . 123.2(2)    yes
C38 . Fe34 . C50 . 159.7(2)    yes
C39 . Fe34 . C50 . 158.2(2)    yes
C35 . Fe34 . C51 . 106.5(2)    yes
C36 . Fe34 . C51 . 122.6(2)    yes
C37 . Fe34 . C51 . 159.3(2)    yes
C38 . Fe34 . C51 . 158.0(2)    yes
C39 . Fe34 . C51 . 121.6(2)    yes
C47 . Fe34 . C48 . 40.8(2)    yes
C47 . Fe34 . C49 . 68.6(2)    yes
C48 . Fe34 . C49 . 40.7(2)    yes
C47 . Fe34 . C50 . 68.6(2)    yes
C48 . Fe34 . C50 . 68.6(2)    yes
C49 . Fe34 . C50 . 40.7(2)    yes
C47 . Fe34 . C51 . 40.8(2)    yes
C48 . Fe34 . C51 . 68.8(2)    yes
C49 . Fe34 . C51 . 68.8(2)    yes
C50 . Fe34 . C51 . 41.0(2)    yes
Fe34 . C35 . C36 . 69.5(3)    yes
Fe34 . C35 . C39 . 69.4(3)    yes
C36 . C35 . C39 . 107.8(5)    yes
Fe34 . C35 . H351 . 127.8    no
C36 . C35 . H351 . 126.2    no
C39 . C35 . H351 . 126.0    no
C35 . C36 . Fe34 . 69.7(3)    yes
C35 . C36 . C37 . 108.0(5)    yes
Fe34 . C36 . C37 . 69.0(3)    yes
C35 . C36 . H361 . 125.4    no
Fe34 . C36 . H361 . 126.6    no
C37 . C36 . H361 . 126.6    no
C36 . C37 . Fe34 . 70.2(3)    yes
C36 . C37 . C38 . 108.2(5)    yes
Fe34 . C37 . C38 . 70.2(3)    yes
C36 . C37 . C40 . 126.8(5)    yes
Fe34 . C37 . C40 . 126.5(3)    yes
C38 . C37 . C40 . 125.1(5)    yes
C37 . C38 . Fe34 . 68.9(3)    yes
C37 . C38 . C39 . 108.0(5)    yes
Fe34 . C38 . C39 . 69.5(3)    yes
C37 . C38 . H381 . 124.3    no
Fe34 . C38 . H381 . 127.5    no
C39 . C38 . H381 . 127.8    no
C35 . C39 . C38 . 108.1(5)    yes
C35 . C39 . Fe34 . 69.8(3)    yes
C38 . C39 . Fe34 . 69.8(3)    yes
C35 . C39 . H391 . 124.9    no
C38 . C39 . H391 . 126.9    no
Fe34 . C39 . H391 . 124.5    no
C37 . C40 . N41 . 109.9(4)    yes
C37 . C40 . H402 . 108.8    no
N41 . C40 . H402 . 107.5    no
C37 . C40 . H401 . 112.4    no
N41 . C40 . H401 . 108.0    no
H402 . C40 . H401 . 110.1    no
C40 . N41 . N42 . 120.5(4)    yes
C40 . N41 . C45 . 128.4(4)    yes
N42 . N41 . C45 . 110.7(4)    yes
N41 . N42 . N43 . 107.1(4)    yes
N42 . N43 . C44 . 109.4(4)    yes
N43 . C44 . C45 . 107.6(5)    yes
N43 . C44 . C46 . 122.2(5)    yes
C45 . C44 . C46 . 130.2(5)    yes
C44 . C45 . N41 . 105.3(4)    yes
C44 . C45 . H451 . 128.6    no
N41 . C45 . H451 . 126.1    no
C44 . C46 . C66 . 112.0(6)    yes
C44 . C46 . H463 . 108.1    no
C66 . C46 . H463 . 107.6    no
C44 . C46 . H464 . 109.3    no
C66 . C46 . H464 . 110.3    no
H463 . C46 . H464 . 109.5    no
Fe34 . C47 . C48 . 69.5(3)    yes
Fe34 . C47 . C51 . 69.1(3)    yes
C48 . C47 . C51 . 108.0(5)    yes
Fe34 . C47 . H471 . 125.2    no
C48 . C47 . H471 . 125.3    no
C51 . C47 . H471 . 126.7    no
C47 . C48 . Fe34 . 69.7(3)    yes
C47 . C48 . C49 . 108.1(5)    yes
Fe34 . C48 . C49 . 69.8(3)    yes
C47 . C48 . C52 . 123.3(5)    yes
Fe34 . C48 . C52 . 130.5(4)    yes
C49 . C48 . C52 . 128.4(5)    yes
C48 . C49 . Fe34 . 69.5(3)    yes
C48 . C49 . C50 . 107.9(5)    yes
Fe34 . C49 . C50 . 69.5(3)    yes
C48 . C49 . H491 . 126.5    no
Fe34 . C49 . H491 . 129.5    no
C50 . C49 . H491 . 125.5    no
C49 . C50 . Fe34 . 69.8(3)    yes
C49 . C50 . C51 . 108.0(5)    yes
Fe34 . C50 . C51 . 69.0(3)    yes
C49 . C50 . H501 . 127.5    no
Fe34 . C50 . H501 . 127.9    no
C51 . C50 . H501 . 124.5    no
C50 . C51 . C47 . 108.0(5)    yes
C50 . C51 . Fe34 . 70.0(3)    yes
C47 . C51 . Fe34 . 70.1(3)    yes
C50 . C51 . H511 . 124.1    no
C47 . C51 . H511 . 127.7    no
Fe34 . C51 . H511 . 128.7    no
C48 . C52 . N53 . 116.3(4)    yes
C48 . C52 . H521 . 106.1    no
N53 . C52 . H521 . 108.0    no
C48 . C52 . H522 . 109.2    no
N53 . C52 . H522 . 108.4    no
H521 . C52 . H522 . 108.7    no
C52 . N53 . N54 . 120.2(5)    yes
C52 . N53 . C57 . 128.8(5)    yes
N54 . N53 . C57 . 110.7(5)    yes
N53 . N54 . N55 . 106.7(4)    yes
N54 . N55 . C56 . 109.1(5)    yes
N55 . C56 . C57 . 107.8(5)    yes
N55 . C56 . C58 . 121.4(5)    yes
C57 . C56 . C58 . 130.8(5)    yes
C56 . C57 . N53 . 105.6(5)    yes
C56 . C57 . H571 . 124.9    no
N53 . C57 . H571 . 129.5    no
C56 . C58 . C59 . 112.2(4)    yes
C56 . C58 . H581 . 109.1    no
C59 . C58 . H581 . 108.1    no
C56 . C58 . H582 . 109.6    no
C59 . C58 . H582 . 109.3    no
H581 . C58 . H582 . 108.5    no
C58 . C59 . C60 . 110.9(5)    yes
C58 . C59 . H592 . 109.1    no
C60 . C59 . H592 . 106.9    no
C58 . C59 . H591 . 110.9    no
C60 . C59 . H591 . 108.4    no
H592 . C59 . H591 . 110.6    no
C59 . C60 . C61 . 113.8(5)    yes
C59 . C60 . H601 . 107.8    no
C61 . C60 . H601 . 108.6    no
C59 . C60 . H602 . 108.8    no
C61 . C60 . H602 . 108.7    no
H601 . C60 . H602 . 109.1    no
C60 . C61 . C62 . 173.6(6)    yes
C61 . C62 . C63 . 177.3(6)    yes
C62 . C63 . C64 . 174.9(6)    yes
C63 . C64 . C65 . 179.6(6)    yes
C64 . C65 . C66 . 114.2(7)    yes
C64 . C65 . H651 . 109.1    no
C66 . C65 . H651 . 107.8    no
C64 . C65 . H652 . 107.2    no
C66 . C65 . H652 . 109.1    no
H651 . C65 . H652 . 109.5    no
C46 . C166 . C65 . 115.3(7)    yes
C46 . C166 . H1661 . 112.4    no
C65 . C166 . H1661 . 110.7    no
C46 . C166 . H1662 . 108.4    no
C65 . C166 . H1662 . 103.6    no
H1661 . C166 . H1662 . 105.5    no
C65 . C66 . C46 . 115.5(8)    yes
C65 . C66 . H661 . 106.4    no
C46 . C66 . H661 . 107.5    no
C65 . C66 . H662 . 107.8    no
C46 . C66 . H662 . 109.3    no
H661 . C66 . H662 . 110.1    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H72 . N43 1_455 161.09(16) 0.985 2.402 3.349(8)    yes
C20 . H202 . N42 1_455 148.05(16) 0.989 2.503 3.383(8)    yes
C33 . H331 . N42 1_455 158.77(19) 0.975 2.345 3.274(8)    yes
C40 . H402 . N10 1_665 152.60(16) 0.969 2.422 3.312(8)    yes
C49 . H491 . N9 1_665 160.59(17) 0.981 2.371 3.312(8)    yes
C52 . H522 . N54 2_676 159.35(17) 0.971 2.544 3.469(8)    yes
C57 . H571 . N24 1_665 146.69(16) 0.947 2.553 3.385(8)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 11/08/11 at 13:28:03
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 463,X'S) H   ( 464,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   ( 166,X'S) H   (1661,X'S) H   (1662,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 11/08/11 at 13:28:03
#
#LIST     16                                                                    
DIST 1.52, 0.02 = C(46) TO C(66), C(66) TO C(65) 
CONT C(46) TO C(166), C(166) TO C(65) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(19) TO C(20) 
VIBR .0, 0.00500 = C(20) TO C(18) 
VIBR .0, 0.00200 = C(20) TO C(21) 
VIBR .0, 0.00500 = C(22) TO C(20) 
VIBR .0, 0.00200 = C(46) TO C(66) 
VIBR .0, 0.00500 = C(66) TO C(44) 
VIBR .0, 0.00200 = C(65) TO C(66) 
VIBR .0, 0.00500 = C(66) TO C(64) 
VIBR .0, 0.00200 = C(46) TO C(166) 
VIBR .0, 0.00500 = C(166) TO C(44) 
VIBR .0, 0.00200 = C(65) TO C(166) 
VIBR .0, 0.00500 = C(166) TO C(64) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(19) TO C(20) 
U(IJ) .0, 0.04000 = C(20) TO C(21) 
U(IJ) .0, 0.04000 = C(46) TO C(66) 
U(IJ) .0, 0.04000 = C(65) TO C(66) 
U(IJ) .0, 0.04000 = C(46) TO C(166) 
U(IJ) .0, 0.04000 = C(65) TO C(166) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
   4   5   1  x   .
   0   6   0  x   .
   4   5  10  x   .
  -5   5  42  x   .
   0  11  33  x   .
   2   8   1  x   .
   7   3   1  x   .
  -7   3   1  x   .

 

#==============================================================================
data_4
#==============================================================================
 
_exptl_special_details 
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
; 
_refine_special_details 
; 
? 
; 

_cell_length_a                    21.1393(8)
_cell_length_b                    11.1627(2)
_cell_length_c                    9.8316(2)
_cell_angle_alpha                 90
_cell_angle_beta                  101.439(3)
_cell_angle_gamma                 90
_cell_volume                      2273.90(11)
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 21/c ' 
_symmetry_space_group_name_Hall   '-P 2ybc' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 'x,-y+1/2,z+1/2'
 '-x,y+1/2,-z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0020   0.0020   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0040   0.0030  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Fe      0.2960   0.8010  11.7695   4.7611   7.3573   0.3072   3.5222  15.3535
   2.3045  76.8805   1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C52 H52 Fe2 N12 
# Dc =      1.40 Fooo =   1000.00 Mu =      6.90 M =    478.38
# Found Formula = C52 H52 Fe2 N12 
# Dc =      1.40 FOOO =   1000.00 Mu =      6.90 M =    478.38

_chemical_formula_sum             'C52 H52 Fe2 N12'
_chemical_formula_moiety          'C52 H52 Fe2 N12'
_chemical_compound_source              synthesised
_chemical_formula_weight            956.76
 
 
_cell_measurement_reflns_used         5565
_cell_measurement_theta_min            1.7683
_cell_measurement_theta_max            31.9808
_cell_measurement_temperature          120
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'orange' 
_exptl_crystal_size_min           0.01 
_exptl_crystal_size_mid           0.06 
_exptl_crystal_size_max           0.20 
 
_exptl_crystal_density_diffrn     1.397 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1000 
_exptl_absorpt_coefficient_mu     0.690 
 
# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'CrysAlis, (Oxford Diffraction, 2002)' 
_exptl_absorpt_correction_T_min   0.76 
_exptl_absorpt_correction_T_max   1.00 
_diffrn_measurement_device_type   'synchrotron'  
_diffrn_radiation_monochromator   'synchrotron' 
_diffrn_radiation_type            'Synchrotron'
_diffrn_radiation_wavelength           0.68890
_diffrn_measurement_method        ω/2θ  
 
 
_computing_data_collection        'Crystal Clear (Rigaku, 1997--2002)' 
_computing_cell_refinement        'CrystalClear (Rigaku, 1997--2002)' 
_computing_data_reduction         'CrysAlis, (Oxford Diffraction, 2002)' 
_computing_structure_solution     'Superflip (Palatinus & Chapuis, 2007)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)'  
 
_diffrn_standards_interval_time   0 
_diffrn_standards_interval_count  0 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         0 
 
_diffrn_ambient_temperature        120
_diffrn_reflns_number             29726 
_reflns_number_total              7996 
_diffrn_reflns_av_R_equivalents   0.0681 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7996 
# Theoretical number of reflections is about 10703 
 
 
_diffrn_reflns_theta_min          1.905 
_diffrn_reflns_theta_max          31.981 
_diffrn_measured_fraction_theta_max 0.924 
 
_diffrn_reflns_theta_full         27.184 
_diffrn_measured_fraction_theta_full 0.996 
 
 
_diffrn_reflns_limit_h_min        -32 
_diffrn_reflns_limit_h_max        32 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_reflns_limit_h_min               -32 
_reflns_limit_h_max               31 
_reflns_limit_k_min               0 
_reflns_limit_k_max               16 
_reflns_limit_l_min               0 
_reflns_limit_l_max               14 
 
_oxford_diffrn_Wilson_B_factor    1.95 
_oxford_diffrn_Wilson_scale       0.07 
 
_atom_sites_solution_primary      Other  #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.66 
_refine_diff_density_max          1.18 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>-3.0\s(I)
_refine_ls_number_reflns          5334 
_refine_ls_number_restraints      0 
_refine_ls_number_parameters      298 
_oxford_refine_ls_R_factor_ref    0.0645 
_refine_ls_wR_factor_ref          0.0980 
_refine_ls_goodness_of_fit_ref    0.9278 
_refine_ls_shift/su_max           0.0007642 
_refine_ls_shift/su_mean          0.0000192 
 
 
# The values computed from all data 
_oxford_reflns_number_all         5334 
_refine_ls_R_factor_all           0.0645 
_refine_ls_wR_factor_all          0.0980 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 4310 
_refine_ls_R_factor_gt            0.0495 
_refine_ls_wR_factor_gt           0.0914 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         # none, undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.124E+04 0.183E+04 0.109E+04 416. 62.6 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 

 
CrystalClear: An Integrated Program for the Collection and Processing of 
Area Detector Data, Rigaku Corporation, 1997--2002. 
 
Oxford Diffraction, (2010). CrysAlisPro. 
 
 
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.

Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982.  
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.219354(18) 0.50036(3) 0.73434(4) 0.0255 1.0000 Uani . . . . . . 
C2 C 0.23619(13) 0.3668(2) 0.6043(3) 0.0295 1.0000 Uani . . . . . . 
C3 C 0.28573(13) 0.3678(2) 0.7264(3) 0.0281 1.0000 Uani . . . . . . 
C4 C 0.25543(13) 0.3495(2) 0.8429(3) 0.0306 1.0000 Uani . . . . . . 
C5 C 0.18765(14) 0.3387(2) 0.7923(3) 0.0328 1.0000 Uani . . . . . . 
C6 C 0.17566(13) 0.3488(2) 0.6445(3) 0.0324 1.0000 Uani . . . . . . 
C7 C 0.35659(13) 0.3863(2) 0.7313(3) 0.0311 1.0000 Uani . . . . . . 
N8 N 0.38794(10) 0.2785(2) 0.6895(2) 0.0289 1.0000 Uani . . . . . . 
N9 N 0.41178(13) 0.2807(2) 0.5726(2) 0.0406 1.0000 Uani . . . . . . 
N10 N 0.43852(13) 0.1747(2) 0.5619(2) 0.0397 1.0000 Uani . . . . . . 
C11 C 0.43209(12) 0.1058(2) 0.6719(3) 0.0303 1.0000 Uani . . . . . . 
C12 C 0.39939(13) 0.1715(2) 0.7533(3) 0.0312 1.0000 Uani . . . . . . 
C13 C 0.45754(13) -0.0199(2) 0.6886(3) 0.0329 1.0000 Uani . . . . . . 
C14 C 0.41386(13) -0.1082(2) 0.5956(3) 0.0322 1.0000 Uani . . . . . . 
C15 C 0.43838(13) -0.2377(2) 0.6148(3) 0.0340 1.0000 Uani . . . . . . 
C16 C 0.39526(13) -0.3193(2) 0.5231(3) 0.0330 1.0000 Uani . . . . . . 
C17 C 0.35653(13) -0.3765(2) 0.4436(3) 0.0315 1.0000 Uani . . . . . . 
C18 C 0.30862(13) -0.4361(2) 0.3517(3) 0.0326 1.0000 Uani . . . . . . 
C19 C 0.26599(13) -0.4817(2) 0.2694(3) 0.0311 1.0000 Uani . . . . . . 
C20 C 0.20932(13) -0.5311(2) 0.1751(3) 0.0338 1.0000 Uani . . . . . . 
C21 C 0.14820(13) -0.5105(3) 0.2327(3) 0.0340 1.0000 Uani . . . . . . 
C22 C 0.08586(14) -0.5544(3) 0.1369(3) 0.0356 1.0000 Uani . . . . . . 
C23 C 0.03059(13) -0.5482(2) 0.2105(3) 0.0327 1.0000 Uani . . . . . . 
N24 N 0.00766(12) -0.4408(2) 0.2477(3) 0.0370 1.0000 Uani . . . . . . 
N25 N -0.03690(11) -0.4607(2) 0.3223(3) 0.0372 1.0000 Uani . . . . . . 
N26 N -0.04211(11) -0.5801(2) 0.3337(2) 0.0328 1.0000 Uani . . . . . . 
C27 C -0.00120(14) -0.6377(2) 0.2657(3) 0.0341 1.0000 Uani . . . . . . 
C28 C -0.08810(14) -0.6331(3) 0.4100(3) 0.0373 1.0000 Uani . . . . . . 
C29 C -0.15595(13) -0.6384(2) 0.3248(3) 0.0310 1.0000 Uani . . . . . . 
C30 C -0.17452(13) -0.6353(2) 0.1772(3) 0.0293 1.0000 Uani . . . . . . 
C31 C -0.24270(13) -0.6479(2) 0.1413(3) 0.0309 1.0000 Uani . . . . . . 
C32 C -0.26671(13) -0.6606(2) 0.2660(3) 0.0327 1.0000 Uani . . . . . . 
C33 C -0.21321(14) -0.6546(2) 0.3796(3) 0.0330 1.0000 Uani . . . . . . 
H21 H 0.2422 0.3787 0.5098 0.0349 1.0000 Uiso R . . . . . 
H41 H 0.2770 0.3459 0.9410 0.0358 1.0000 Uiso R . . . . . 
H51 H 0.1555 0.3289 0.8482 0.0380 1.0000 Uiso R . . . . . 
H61 H 0.1329 0.3476 0.5825 0.0378 1.0000 Uiso R . . . . . 
H72 H 0.3777 0.4079 0.8260 0.0365 1.0000 Uiso R . . . . . 
H71 H 0.3613 0.4508 0.6687 0.0364 1.0000 Uiso R . . . . . 
H121 H 0.3872 0.1501 0.8371 0.0362 1.0000 Uiso R . . . . . 
H132 H 0.5005 -0.0220 0.6647 0.0388 1.0000 Uiso R . . . . . 
H131 H 0.4627 -0.0435 0.7858 0.0387 1.0000 Uiso R . . . . . 
H141 H 0.4113 -0.0855 0.4982 0.0386 1.0000 Uiso R . . . . . 
H142 H 0.3702 -0.1043 0.6153 0.0381 1.0000 Uiso R . . . . . 
H151 H 0.4818 -0.2419 0.5943 0.0403 1.0000 Uiso R . . . . . 
H152 H 0.4391 -0.2620 0.7121 0.0397 1.0000 Uiso R . . . . . 
H201 H 0.2149 -0.6168 0.1634 0.0393 1.0000 Uiso R . . . . . 
H202 H 0.2042 -0.4917 0.0860 0.0394 1.0000 Uiso R . . . . . 
H211 H 0.1533 -0.5529 0.3214 0.0411 1.0000 Uiso R . . . . . 
H212 H 0.1436 -0.4257 0.2502 0.0407 1.0000 Uiso R . . . . . 
H222 H 0.0905 -0.6381 0.1088 0.0418 1.0000 Uiso R . . . . . 
H221 H 0.0773 -0.5052 0.0530 0.0422 1.0000 Uiso R . . . . . 
H271 H 0.0039 -0.7216 0.2581 0.0404 1.0000 Uiso R . . . . . 
H282 H -0.0724 -0.7124 0.4370 0.0463 1.0000 Uiso R . . . . . 
H281 H -0.0877 -0.5841 0.4944 0.0458 1.0000 Uiso R . . . . . 
H301 H -0.1451 -0.6244 0.1141 0.0328 1.0000 Uiso R . . . . . 
H311 H -0.2684 -0.6443 0.0464 0.0375 1.0000 Uiso R . . . . . 
H321 H -0.3118 -0.6725 0.2725 0.0386 1.0000 Uiso R . . . . . 
H331 H -0.2153 -0.6585 0.4792 0.0395 1.0000 Uiso R . . . . . 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 4.01(4) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Fe1 . C30 2_556 2.062(2)    yes
Fe1 . C31 2_556 2.052(3)    yes
Fe1 . C32 2_556 2.050(3)    yes
Fe1 . C29 2_556 2.050(3)    yes
Fe1 . C33 2_556 2.044(3)    yes
Fe1 . C2 . 2.041(2)    yes
Fe1 . C3 . 2.051(3)    yes
Fe1 . C4 . 2.058(3)    yes
Fe1 . C5 . 2.045(3)    yes
Fe1 . C6 . 2.042(3)    yes
C2 . C3 . 1.428(4)    yes
C2 . C6 . 1.426(4)    yes
C2 . H21 . 0.972    no
C3 . C4 . 1.433(4)    yes
C3 . C7 . 1.503(4)    yes
C4 . C5 . 1.426(4)    yes
C4 . H41 . 0.982    no
C5 . C6 . 1.429(4)    yes
C5 . H51 . 0.962    no
C6 . H61 . 0.985    no
C7 . N8 . 1.471(3)    yes
C7 . H72 . 0.980    no
C7 . H71 . 0.964    no
N8 . N9 . 1.344(3)    yes
N8 . C12 . 1.349(3)    yes
N9 . N10 . 1.325(3)    yes
N10 . C11 . 1.355(3)    yes
C11 . C12 . 1.369(4)    yes
C11 . C13 . 1.501(4)    yes
C12 . H121 . 0.942    no
C13 . C14 . 1.525(4)    yes
C13 . H132 . 0.982    no
C13 . H131 . 0.977    no
C14 . C15 . 1.534(4)    yes
C14 . H141 . 0.981    no
C14 . H142 . 0.982    no
C15 . C16 . 1.466(4)    yes
C15 . H151 . 0.980    no
C15 . H152 . 0.991    no
C16 . C17 . 1.197(4)    yes
C17 . C18 . 1.387(4)    yes
C18 . C19 . 1.199(4)    yes
C19 . C20 . 1.469(4)    yes
C20 . C21 . 1.528(4)    yes
C20 . H201 . 0.974    no
C20 . H202 . 0.967    no
C21 . C22 . 1.540(4)    yes
C21 . H211 . 0.979    no
C21 . H212 . 0.971    no
C22 . C23 . 1.493(4)    yes
C22 . H222 . 0.985    no
C22 . H221 . 0.978    no
C23 . N24 . 1.370(3)    yes
C23 . C27 . 1.374(4)    yes
N24 . N25 . 1.322(3)    yes
N25 . N26 . 1.343(3)    yes
N26 . C27 . 1.355(4)    yes
N26 . C28 . 1.466(4)    yes
C27 . H271 . 0.948    no
C28 . C29 . 1.512(4)    yes
C28 . H282 . 0.964    no
C28 . H281 . 0.992    no
C29 . C30 . 1.427(4)    yes
C29 . C33 . 1.430(4)    yes
C30 . C31 . 1.421(4)    yes
C30 . H301 . 0.969    no
C31 . C32 . 1.424(4)    yes
C31 . H311 . 0.983    no
C32 . C33 . 1.425(4)    yes
C32 . H321 . 0.977    no
C33 . H331 . 0.990    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
C30 2_556 Fe1 . C31 2_556 40.41(10)    yes
C30 2_556 Fe1 . C32 2_556 68.21(10)    yes
C31 2_556 Fe1 . C32 2_556 40.62(11)    yes
C30 2_556 Fe1 . C29 2_556 40.62(10)    yes
C31 2_556 Fe1 . C29 2_556 68.41(11)    yes
C32 2_556 Fe1 . C29 2_556 68.62(11)    yes
C30 2_556 Fe1 . C33 2_556 68.35(10)    yes
C31 2_556 Fe1 . C33 2_556 68.41(11)    yes
C32 2_556 Fe1 . C33 2_556 40.73(11)    yes
C29 2_556 Fe1 . C33 2_556 40.89(10)    yes
C30 2_556 Fe1 . C2 . 161.80(11)    yes
C31 2_556 Fe1 . C2 . 155.29(11)    yes
C32 2_556 Fe1 . C2 . 119.38(11)    yes
C29 2_556 Fe1 . C2 . 123.85(11)    yes
C33 2_556 Fe1 . C2 . 105.81(11)    yes
C30 2_556 Fe1 . C3 . 156.66(10)    yes
C31 2_556 Fe1 . C3 . 121.07(11)    yes
C32 2_556 Fe1 . C3 . 106.94(11)    yes
C29 2_556 Fe1 . C3 . 160.97(10)    yes
C33 2_556 Fe1 . C3 . 123.82(11)    yes
C30 2_556 Fe1 . C4 . 122.23(10)    yes
C31 2_556 Fe1 . C4 . 109.11(10)    yes
C32 2_556 Fe1 . C4 . 125.74(11)    yes
C29 2_556 Fe1 . C4 . 156.48(11)    yes
C33 2_556 Fe1 . C4 . 161.87(11)    yes
C30 2_556 Fe1 . C5 . 108.90(11)    yes
C31 2_556 Fe1 . C5 . 126.57(11)    yes
C32 2_556 Fe1 . C5 . 163.25(12)    yes
C29 2_556 Fe1 . C5 . 120.71(11)    yes
C33 2_556 Fe1 . C5 . 155.13(12)    yes
C30 2_556 Fe1 . C6 . 125.54(11)    yes
C31 2_556 Fe1 . C6 . 163.15(11)    yes
C32 2_556 Fe1 . C6 . 154.29(11)    yes
C29 2_556 Fe1 . C6 . 106.61(11)    yes
C33 2_556 Fe1 . C6 . 119.11(11)    yes
C2 . Fe1 . C3 . 40.85(10)    yes
C2 . Fe1 . C4 . 68.53(10)    yes
C3 . Fe1 . C4 . 40.82(10)    yes
C2 . Fe1 . C5 . 68.72(11)    yes
C3 . Fe1 . C5 . 68.80(10)    yes
C4 . Fe1 . C5 . 40.66(11)    yes
C2 . Fe1 . C6 . 40.89(10)    yes
C3 . Fe1 . C6 . 68.92(10)    yes
C4 . Fe1 . C6 . 68.64(11)    yes
C5 . Fe1 . C6 . 40.93(11)    yes
Fe1 . C2 . C3 . 69.97(14)    yes
Fe1 . C2 . C6 . 69.60(14)    yes
C3 . C2 . C6 . 108.5(2)    yes
Fe1 . C2 . H21 . 124.8    no
C3 . C2 . H21 . 126.2    no
C6 . C2 . H21 . 125.3    no
C2 . C3 . Fe1 . 69.18(14)    yes
C2 . C3 . C4 . 107.5(2)    yes
Fe1 . C3 . C4 . 69.84(14)    yes
C2 . C3 . C7 . 126.0(2)    yes
Fe1 . C3 . C7 . 125.76(17)    yes
C4 . C3 . C7 . 126.5(2)    yes
C3 . C4 . Fe1 . 69.34(14)    yes
C3 . C4 . C5 . 108.1(2)    yes
Fe1 . C4 . C5 . 69.20(15)    yes
C3 . C4 . H41 . 126.6    no
Fe1 . C4 . H41 . 126.5    no
C5 . C4 . H41 . 125.3    no
C4 . C5 . Fe1 . 70.14(14)    yes
C4 . C5 . C6 . 108.1(2)    yes
Fe1 . C5 . C6 . 69.41(14)    yes
C4 . C5 . H51 . 125.9    no
Fe1 . C5 . H51 . 124.6    no
C6 . C5 . H51 . 125.9    no
C5 . C6 . C2 . 107.8(2)    yes
C5 . C6 . Fe1 . 69.66(15)    yes
C2 . C6 . Fe1 . 69.51(14)    yes
C5 . C6 . H61 . 125.7    no
C2 . C6 . H61 . 126.4    no
Fe1 . C6 . H61 . 124.1    no
C3 . C7 . N8 . 112.3(2)    yes
C3 . C7 . H72 . 109.0    no
N8 . C7 . H72 . 108.8    no
C3 . C7 . H71 . 108.1    no
N8 . C7 . H71 . 108.9    no
H72 . C7 . H71 . 109.7    no
C7 . N8 . N9 . 119.3(2)    yes
C7 . N8 . C12 . 130.1(2)    yes
N9 . N8 . C12 . 110.5(2)    yes
N8 . N9 . N10 . 106.9(2)    yes
N9 . N10 . C11 . 109.3(2)    yes
N10 . C11 . C12 . 107.8(2)    yes
N10 . C11 . C13 . 121.8(2)    yes
C12 . C11 . C13 . 130.4(3)    yes
C11 . C12 . N8 . 105.5(2)    yes
C11 . C12 . H121 . 129.3    no
N8 . C12 . H121 . 125.2    no
C11 . C13 . C14 . 112.2(2)    yes
C11 . C13 . H132 . 108.9    no
C14 . C13 . H132 . 108.7    no
C11 . C13 . H131 . 109.2    no
C14 . C13 . H131 . 110.4    no
H132 . C13 . H131 . 107.3    no
C13 . C14 . C15 . 112.7(2)    yes
C13 . C14 . H141 . 109.1    no
C15 . C14 . H141 . 108.4    no
C13 . C14 . H142 . 109.6    no
C15 . C14 . H142 . 109.0    no
H141 . C14 . H142 . 107.9    no
C14 . C15 . C16 . 110.9(2)    yes
C14 . C15 . H151 . 109.1    no
C16 . C15 . H151 . 109.7    no
C14 . C15 . H152 . 108.5    no
C16 . C15 . H152 . 108.2    no
H151 . C15 . H152 . 110.4    no
C15 . C16 . C17 . 173.7(3)    yes
C16 . C17 . C18 . 176.0(3)    yes
C17 . C18 . C19 . 176.5(3)    yes
C18 . C19 . C20 . 174.4(3)    yes
C19 . C20 . C21 . 110.7(2)    yes
C19 . C20 . H201 . 109.9    no
C21 . C20 . H201 . 108.9    no
C19 . C20 . H202 . 109.4    no
C21 . C20 . H202 . 108.5    no
H201 . C20 . H202 . 109.5    no
C20 . C21 . C22 . 114.1(2)    yes
C20 . C21 . H211 . 107.8    no
C22 . C21 . H211 . 108.6    no
C20 . C21 . H212 . 109.6    no
C22 . C21 . H212 . 108.4    no
H211 . C21 . H212 . 108.2    no
C21 . C22 . C23 . 110.2(2)    yes
C21 . C22 . H222 . 110.6    no
C23 . C22 . H222 . 108.2    no
C21 . C22 . H221 . 109.3    no
C23 . C22 . H221 . 110.6    no
H222 . C22 . H221 . 108.0    no
C22 . C23 . N24 . 121.5(2)    yes
C22 . C23 . C27 . 130.5(3)    yes
N24 . C23 . C27 . 107.7(2)    yes
C23 . N24 . N25 . 109.2(2)    yes
N24 . N25 . N26 . 107.0(2)    yes
N25 . N26 . C27 . 111.0(2)    yes
N25 . N26 . C28 . 121.1(2)    yes
C27 . N26 . C28 . 127.9(2)    yes
C23 . C27 . N26 . 105.1(2)    yes
C23 . C27 . H271 . 128.0    no
N26 . C27 . H271 . 126.9    no
N26 . C28 . C29 . 112.6(2)    yes
N26 . C28 . H282 . 106.6    no
C29 . C28 . H282 . 110.7    no
N26 . C28 . H281 . 108.0    no
C29 . C28 . H281 . 109.5    no
H282 . C28 . H281 . 109.3    no
C28 . C29 . Fe1 2_556 128.52(19)    yes
C28 . C29 . C30 . 127.0(2)    yes
Fe1 2_556 C29 . C30 . 70.15(15)    yes
C28 . C29 . C33 . 125.3(2)    yes
Fe1 2_556 C29 . C33 . 69.34(15)    yes
C30 . C29 . C33 . 107.7(2)    yes
C29 . C30 . Fe1 2_556 69.22(14)    yes
C29 . C30 . C31 . 108.1(2)    yes
Fe1 2_556 C30 . C31 . 69.43(14)    yes
C29 . C30 . H301 . 124.9    no
Fe1 2_556 C30 . H301 . 125.8    no
C31 . C30 . H301 . 127.0    no
C30 . C31 . Fe1 2_556 70.16(14)    yes
C30 . C31 . C32 . 108.3(2)    yes
Fe1 2_556 C31 . C32 . 69.59(14)    yes
C30 . C31 . H311 . 125.0    no
Fe1 2_556 C31 . H311 . 123.7    no
C32 . C31 . H311 . 126.7    no
C31 . C32 . Fe1 2_556 69.78(14)    yes
C31 . C32 . C33 . 107.9(2)    yes
Fe1 2_556 C32 . C33 . 69.42(15)    yes
C31 . C32 . H321 . 126.1    no
Fe1 2_556 C32 . H321 . 127.0    no
C33 . C32 . H321 . 126.1    no
C29 . C33 . C32 . 108.1(2)    yes
C29 . C33 . Fe1 2_556 69.77(15)    yes
C32 . C33 . Fe1 2_556 69.85(15)    yes
C29 . C33 . H331 . 125.8    no
C32 . C33 . H331 . 126.1    no
Fe1 2_556 C33 . H331 . 124.7    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C7 . H72 . N10 3_555 144.64(8) 0.980 2.588 3.435(4)    yes
C12 . H121 . N9 3_555 136.02(9) 0.942 2.398 3.144(4)    yes
C27 . H271 . N24 4_545 166.78(9) 0.948 2.459 3.388(4)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/12/11 at 11:43:47
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/12/11 at 11:43:47
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
   8   1   5  x   .







