# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp49lt

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H20 F2 Fe N4 O2, C N S'
_chemical_formula_sum            'C33 H20 F2 Fe N5 O2 S'
_chemical_formula_weight         644.45

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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

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

_cell_length_a                   9.870(2)
_cell_length_b                   11.998(2)
_cell_length_c                   23.533(5)
_cell_angle_alpha                98.97(3)
_cell_angle_beta                 99.89(3)
_cell_angle_gamma                90.65(3)
_cell_volume                     2709.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11823
_cell_measurement_theta_min      0.89
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 201r'
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            87868
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         0.89
_diffrn_reflns_theta_max         27.50
_reflns_number_total             11823
_reflns_number_gt                11216
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.

The asymmetric unit contains two iron monomers and two thiocyanate anions. 
All the non-hydrogen atoms are refined anisotropically and all hydrogen
atoms are placed in calculated positions. One of the thiocyanate anions
is disordered over two positions and has been modelled in two parts, the
first part with a fixed occupancy of 0.6, N10-C66-S2, and the second with
a fixed occupancy of 0.4, N10'-C66'-S2'. No absorption correction has been
carried out due to the small size of the crystals and low absorption
coefficient value of 0.691.

The following restraints were used:
ISOR 0.001 C65
ISOR 0.001 N10 C66 N10' C66'

The crystal was run on the Australian synchrotron in which we were restricted
to one 360 degree phi scan and limited resolution hence the appearance of the
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low alert.     
;

_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)+(0.0526P)²+5.1097P] 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         11823
_refine_ls_number_parameters     821
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.053
_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 0.29676(3) 0.10035(3) 0.375502(13) 0.01628(9) Uani 1 1 d . . .
Fe2 Fe 0.92902(3) 0.70446(3) 0.124948(13) 0.01622(9) Uani 1 1 d . . .
F1 F 0.45170(18) -0.31489(15) 0.16641(7) 0.0367(4) Uani 1 1 d . . .
F2 F 0.14232(18) -0.17484(14) 0.58982(7) 0.0345(4) Uani 1 1 d . . .
F3 F 1.1678(3) 0.9073(2) -0.09616(8) 0.0646(7) Uani 1 1 d . . .
F4 F 1.3362(2) 0.48924(19) 0.34281(8) 0.0507(5) Uani 1 1 d . . .
O1 O 0.41540(17) -0.01912(14) 0.36461(7) 0.0208(3) Uani 1 1 d . . .
O2 O 0.16005(17) 0.00813(14) 0.39195(7) 0.0209(3) Uani 1 1 d . . .
O3 O 1.04173(18) 0.81933(14) 0.11034(7) 0.0213(3) Uani 1 1 d . . .
O4 O 1.06828(18) 0.60079(15) 0.13693(7) 0.0229(3) Uani 1 1 d . . .
N1 N 0.20252(19) 0.07822(16) 0.29456(8) 0.0178(4) Uani 1 1 d . . .
N2 N 0.1781(2) 0.23180(17) 0.38247(8) 0.0195(4) Uani 1 1 d . . .
N4 N 0.4406(2) 0.20460(17) 0.36281(8) 0.0188(4) Uani 1 1 d . . .
N5 N 0.8895(2) 0.63012(16) 0.04369(8) 0.0192(4) Uani 1 1 d . . .
N6 N 0.7965(2) 0.58731(16) 0.13505(8) 0.0180(4) Uani 1 1 d . . .
N7 N 0.9592(2) 0.77733(16) 0.20655(8) 0.0177(4) Uani 1 1 d . . .
N8 N 0.7728(2) 0.80617(16) 0.11824(8) 0.0183(4) Uani 1 1 d . . .
C1 C 0.4159(2) -0.08898(19) 0.31550(9) 0.0186(4) Uani 1 1 d . . .
C2 C 0.5150(3) -0.1727(2) 0.31636(10) 0.0230(5) Uani 1 1 d . . .
H2 H 0.5758 -0.1771 0.3519 0.028 Uiso 1 1 calc R . .
C3 C 0.5261(3) -0.2480(2) 0.26724(11) 0.0270(5) Uani 1 1 d . . .
H3 H 0.5932 -0.3040 0.2687 0.032 Uiso 1 1 calc R . .
C4 C 0.4373(3) -0.2410(2) 0.21510(10) 0.0255(5) Uani 1 1 d . . .
C5 C 0.3385(3) -0.1635(2) 0.21119(10) 0.0213(4) Uani 1 1 d . . .
H5 H 0.2788 -0.1615 0.1751 0.026 Uiso 1 1 calc R . .
C6 C 0.3256(2) -0.08539(19) 0.26180(9) 0.0176(4) Uani 1 1 d . . .
C7 C 0.2231(2) -0.00372(19) 0.25390(9) 0.0183(4) Uani 1 1 d . . .
H7 H 0.1661 -0.0093 0.2166 0.022 Uiso 1 1 calc R . .
C8 C 0.1069(2) 0.1621(2) 0.28162(10) 0.0201(4) Uani 1 1 d . . .
C9 C 0.0275(3) 0.1711(2) 0.22832(11) 0.0252(5) Uani 1 1 d . . .
H9 H 0.0311 0.1155 0.1952 0.030 Uiso 1 1 calc R . .
C10 C -0.0591(3) 0.2631(2) 0.22330(11) 0.0292(5) Uani 1 1 d . . .
H10 H -0.1134 0.2686 0.1865 0.035 Uiso 1 1 calc R . .
C11 C -0.0668(3) 0.3446(2) 0.27025(12) 0.0294(5) Uani 1 1 d . . .
H11 H -0.1246 0.4065 0.2656 0.035 Uiso 1 1 calc R . .
C12 C 0.0113(3) 0.3367(2) 0.32555(11) 0.0249(5) Uani 1 1 d . . .
C13 C 0.0077(3) 0.4153(2) 0.37673(12) 0.0292(5) Uani 1 1 d . . .
H13 H -0.0473 0.4796 0.3752 0.035 Uiso 1 1 calc R . .
C14 C 0.0847(3) 0.3973(2) 0.42850(11) 0.0277(5) Uani 1 1 d . . .
H14 H 0.0801 0.4475 0.4635 0.033 Uiso 1 1 calc R . .
C15 C 0.1701(2) 0.3051(2) 0.42997(10) 0.0233(5) Uani 1 1 d . . .
H15 H 0.2240 0.2948 0.4662 0.028 Uiso 1 1 calc R . .
C16 C 0.0978(2) 0.2453(2) 0.33055(10) 0.0205(4) Uani 1 1 d . . .
C17 C 0.1646(2) -0.0345(2) 0.44079(10) 0.0199(4) Uani 1 1 d . . .
C18 C 0.0603(3) -0.1152(2) 0.44170(10) 0.0238(5) Uani 1 1 d . . .
H18 H -0.0068 -0.1377 0.4076 0.029 Uiso 1 1 calc R . .
C19 C 0.0538(3) -0.1620(2) 0.49104(11) 0.0264(5) Uani 1 1 d . . .
H19 H -0.0167 -0.2167 0.4909 0.032 Uiso 1 1 calc R . .
C20 C 0.1520(3) -0.1282(2) 0.54126(10) 0.0253(5) Uani 1 1 d . . .
C21 C 0.2547(3) -0.0513(2) 0.54300(10) 0.0230(5) Uani 1 1 d . . .
H21 H 0.3204 -0.0303 0.5778 0.028 Uiso 1 1 calc R . .
C22 C 0.2638(2) -0.0023(2) 0.49254(10) 0.0198(4) Uani 1 1 d . . .
C23 C 0.3694(2) 0.0829(2) 0.49820(9) 0.0194(4) Uani 1 1 d . . .
H23 H 0.4281 0.1021 0.5350 0.023 Uiso 1 1 calc R . .
C24 C 0.4893(2) 0.2264(2) 0.46619(10) 0.0224(5) Uani 1 1 d . . .
C25 C 0.5566(3) 0.2831(3) 0.51912(11) 0.0316(6) Uani 1 1 d . . .
H25 H 0.5392 0.2621 0.5546 0.038 Uiso 1 1 calc R . .
C26 C 0.6512(4) 0.3724(3) 0.52034(13) 0.0473(9) Uani 1 1 d . . .
H26 H 0.6971 0.4116 0.5569 0.057 Uiso 1 1 calc R . .
C27 C 0.6787(4) 0.4043(3) 0.46978(13) 0.0495(9) Uani 1 1 d . . .
H27 H 0.7426 0.4652 0.4718 0.059 Uiso 1 1 calc R . .
C28 C 0.6126(3) 0.3472(3) 0.41484(11) 0.0319(6) Uani 1 1 d . . .
C29 C 0.6385(3) 0.3704(3) 0.36030(12) 0.0329(6) Uani 1 1 d . . .
H29 H 0.7031 0.4288 0.3589 0.040 Uiso 1 1 calc R . .
C30 C 0.5698(3) 0.3080(2) 0.30989(11) 0.0254(5) Uani 1 1 d . . .
H30 H 0.5904 0.3192 0.2732 0.031 Uiso 1 1 calc R . .
C31 C 0.4683(2) 0.2270(2) 0.31278(10) 0.0204(4) Uani 1 1 d . . .
H31 H 0.4177 0.1869 0.2774 0.025 Uiso 1 1 calc R . .
C32 C 0.5155(2) 0.2604(2) 0.41403(10) 0.0225(5) Uani 1 1 d . . .
C33 C 1.0704(2) 0.8340(2) 0.05923(10) 0.0227(5) Uani 1 1 d . . .
C34 C 1.1503(3) 0.9317(2) 0.05757(11) 0.0269(5) Uani 1 1 d . . .
H34 H 1.1816 0.9823 0.0928 0.032 Uiso 1 1 calc R . .
C35 C 1.1838(3) 0.9550(3) 0.00626(12) 0.0343(6) Uani 1 1 d . . .
H35 H 1.2382 1.0207 0.0060 0.041 Uiso 1 1 calc R . .
C36 C 1.1369(4) 0.8813(3) -0.04528(12) 0.0413(8) Uani 1 1 d . . .
C37 C 1.0605(4) 0.7859(3) -0.04655(12) 0.0407(7) Uani 1 1 d . . .
H37 H 1.0305 0.7369 -0.0824 0.049 Uiso 1 1 calc R . .
C38 C 1.0257(3) 0.7601(2) 0.00585(11) 0.0277(5) Uani 1 1 d . . .
C39 C 0.9408(3) 0.6610(2) 0.00103(10) 0.0269(5) Uani 1 1 d . . .
H39 H 0.9201 0.6142 -0.0361 0.032 Uiso 1 1 calc R . .
C40 C 0.7980(3) 0.53414(19) 0.03371(10) 0.0209(4) Uani 1 1 d . . .
C41 C 0.7518(3) 0.4640(2) -0.01842(11) 0.0291(5) Uani 1 1 d . . .
H41 H 0.7833 0.4766 -0.0529 0.035 Uiso 1 1 calc R . .
C42 C 0.6580(4) 0.3739(2) -0.02052(12) 0.0371(7) Uani 1 1 d . . .
H42 H 0.6273 0.3258 -0.0566 0.044 Uiso 1 1 calc R . .
C43 C 0.6096(3) 0.3539(2) 0.02843(12) 0.0345(6) Uani 1 1 d . . .
H43 H 0.5458 0.2926 0.0259 0.041 Uiso 1 1 calc R . .
C44 C 0.6547(3) 0.4244(2) 0.08262(11) 0.0254(5) Uani 1 1 d . . .
C45 C 0.6094(3) 0.4113(2) 0.13528(11) 0.0259(5) Uani 1 1 d . . .
H45 H 0.5459 0.3516 0.1360 0.031 Uiso 1 1 calc R . .
C46 C 0.6580(3) 0.4855(2) 0.18500(10) 0.0235(5) Uani 1 1 d . . .
H46 H 0.6283 0.4777 0.2206 0.028 Uiso 1 1 calc R . .
C47 C 0.7520(2) 0.5734(2) 0.18348(10) 0.0208(4) Uani 1 1 d . . .
H47 H 0.7847 0.6245 0.2184 0.025 Uiso 1 1 calc R . .
C48 C 0.7486(2) 0.51435(19) 0.08445(10) 0.0195(4) Uani 1 1 d . . .
C49 C 1.1316(2) 0.5801(2) 0.18810(10) 0.0219(5) Uani 1 1 d . . .
C50 C 1.2097(3) 0.4827(2) 0.18845(12) 0.0296(5) Uani 1 1 d . . .
H50 H 1.2153 0.4363 0.1524 0.035 Uiso 1 1 calc R . .
C51 C 1.2782(3) 0.4526(3) 0.23966(13) 0.0351(6) Uani 1 1 d . . .
H51 H 1.3295 0.3861 0.2390 0.042 Uiso 1 1 calc R . .
C52 C 1.2708(3) 0.5215(3) 0.29231(12) 0.0339(6) Uani 1 1 d . . .
C53 C 1.1986(3) 0.6171(2) 0.29490(11) 0.0282(5) Uani 1 1 d . . .
H53 H 1.1967 0.6630 0.3315 0.034 Uiso 1 1 calc R . .
C54 C 1.1258(2) 0.6480(2) 0.24264(10) 0.0213(5) Uani 1 1 d . . .
C55 C 1.0447(2) 0.7454(2) 0.24883(10) 0.0196(4) Uani 1 1 d . . .
H55 H 1.0538 0.7899 0.2865 0.023 Uiso 1 1 calc R . .
C56 C 0.8711(2) 0.86797(19) 0.21773(9) 0.0183(4) Uani 1 1 d . . .
C57 C 0.8734(3) 0.9404(2) 0.26968(10) 0.0234(5) Uani 1 1 d . . .
H57 H 0.9424 0.9350 0.3026 0.028 Uiso 1 1 calc R . .
C58 C 0.7726(3) 1.0223(2) 0.27355(11) 0.0284(5) Uani 1 1 d . . .
H58 H 0.7753 1.0724 0.3093 0.034 Uiso 1 1 calc R . .
C59 C 0.6708(3) 1.0315(2) 0.22696(12) 0.0281(5) Uani 1 1 d . . .
H59 H 0.6031 1.0865 0.2310 0.034 Uiso 1 1 calc R . .
C60 C 0.6665(3) 0.9592(2) 0.17303(11) 0.0223(5) Uani 1 1 d . . .
C61 C 0.5659(3) 0.9625(2) 0.12262(11) 0.0257(5) Uani 1 1 d . . .
H61 H 0.4948 1.0151 0.1236 0.031 Uiso 1 1 calc R . .
C62 C 0.5722(3) 0.8891(2) 0.07254(11) 0.0261(5) Uani 1 1 d . . .
H62 H 0.5054 0.8904 0.0384 0.031 Uiso 1 1 calc R . .
C63 C 0.6777(3) 0.8119(2) 0.07175(10) 0.0221(5) Uani 1 1 d . . .
H63 H 0.6811 0.7618 0.0366 0.027 Uiso 1 1 calc R . .
C64 C 0.7686(2) 0.87893(19) 0.16893(10) 0.0184(4) Uani 1 1 d . . .
N9 N 0.3112(2) 0.2456(2) 0.07032(9) 0.0265(4) Uani 1 1 d . . .
C65 C 0.3195(5) 0.2173(4) 0.1052(2) 0.0629(10) Uani 1 1 d U . .
N3 N 0.3905(2) 0.13582(17) 0.45612(8) 0.0188(4) Uani 1 1 d . . .
S1 S 0.32196(12) 0.17335(9) 0.16792(4) 0.0572(2) Uani 1 1 d . . .
S2 S 0.85102(16) 0.65301(14) 0.33234(7) 0.0284(3) Uani 0.60 1 d P A 1
N10 N 0.7303(5) 0.6920(4) 0.4310(2) 0.0280(13) Uani 0.60 1 d PU A 1
C66 C 0.7792(5) 0.6782(4) 0.3915(2) 0.0250(8) Uani 0.60 1 d PU A 1
C66' C 0.8064(6) 0.6659(4) 0.3622(3) 0.0132(9) Uani 0.40 1 d PU B 2
N10' N 0.8594(13) 0.6776(10) 0.3217(5) 0.052(4) Uani 0.40 1 d PU B 2
S2' S 0.7336(2) 0.65455(18) 0.41816(8) 0.0243(4) Uani 0.40 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.8637(18) . ?
Fe1 O1 1.8756(17) . ?
Fe1 N3 1.942(2) . ?
Fe1 N1 1.947(2) . ?
Fe1 N4 1.972(2) . ?
Fe1 N2 1.978(2) . ?
Fe2 O3 1.8707(18) . ?
Fe2 O4 1.8790(18) . ?
Fe2 N5 1.952(2) . ?
Fe2 N7 1.953(2) . ?
Fe2 N8 1.978(2) . ?
Fe2 N6 1.978(2) . ?
F1 C4 1.364(3) . ?
F2 C20 1.365(3) . ?
F3 C36 1.365(3) . ?
F4 C52 1.365(3) . ?
O1 C1 1.318(3) . ?
O2 C17 1.323(3) . ?
O3 C33 1.319(3) . ?
O4 C49 1.319(3) . ?
N1 C7 1.304(3) . ?
N1 C8 1.420(3) . ?
N2 C15 1.325(3) . ?
N2 C16 1.371(3) . ?
N4 C31 1.319(3) . ?
N4 C32 1.371(3) . ?
N5 C39 1.299(3) . ?
N5 C40 1.420(3) . ?
N6 C47 1.322(3) . ?
N6 C48 1.371(3) . ?
N7 C55 1.298(3) . ?
N7 C56 1.421(3) . ?
N8 C63 1.325(3) . ?
N8 C64 1.371(3) . ?
C1 C2 1.410(3) . ?
C1 C6 1.423(3) . ?
C2 C3 1.372(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.356(3) . ?
C5 C6 1.421(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(3) . ?
C8 C16 1.418(3) . ?
C9 C10 1.411(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.370(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.411(4) . ?
C11 H11 0.9500 . ?
C12 C16 1.404(3) . ?
C12 C13 1.415(4) . ?
C13 C14 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.411(3) . ?
C17 C22 1.423(3) . ?
C18 C19 1.377(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.354(4) . ?
C21 C22 1.420(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.426(3) . ?
C23 N3 1.301(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(3) . ?
C24 N3 1.416(3) . ?
C24 C32 1.415(3) . ?
C25 C26 1.407(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.373(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.411(4) . ?
C27 H27 0.9500 . ?
C28 C32 1.403(4) . ?
C28 C29 1.419(4) . ?
C29 C30 1.365(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.405(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C33 C34 1.414(4) . ?
C33 C38 1.419(3) . ?
C34 C35 1.373(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.356(4) . ?
C37 C38 1.413(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.425(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.378(3) . ?
C40 C48 1.416(3) . ?
C41 C42 1.405(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.415(3) . ?
C43 H43 0.9500 . ?
C44 C48 1.405(3) . ?
C44 C45 1.418(3) . ?
C45 C46 1.365(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.406(3) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C49 C50 1.408(3) . ?
C49 C54 1.419(3) . ?
C50 C51 1.379(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.392(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.356(4) . ?
C53 C54 1.418(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.427(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.382(3) . ?
C56 C64 1.418(3) . ?
C57 C58 1.410(4) . ?
C57 H57 0.9500 . ?
C58 C59 1.374(4) . ?
C58 H58 0.9500 . ?
C59 C60 1.415(3) . ?
C59 H59 0.9500 . ?
C60 C64 1.407(3) . ?
C60 C61 1.416(4) . ?
C61 C62 1.368(4) . ?
C61 H61 0.9500 . ?
C62 C63 1.402(3) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
N9 C65 0.927(5) . ?
C65 S1 1.641(5) . ?
S2 C66 1.656(6) . ?
N10 C66 1.110(7) . ?
C66' N10' 1.190(12) . ?
C66' S2' 1.627(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 93.21(8) . . ?
O2 Fe1 N3 94.56(8) . . ?
O1 Fe1 N3 88.48(8) . . ?
O2 Fe1 N1 88.36(8) . . ?
O1 Fe1 N1 95.12(8) . . ?
N3 Fe1 N1 175.24(8) . . ?
O2 Fe1 N4 176.29(8) . . ?
O1 Fe1 N4 89.10(8) . . ?
N3 Fe1 N4 82.59(9) . . ?
N1 Fe1 N4 94.33(8) . . ?
O2 Fe1 N2 90.67(8) . . ?
O1 Fe1 N2 175.50(8) . . ?
N3 Fe1 N2 93.49(9) . . ?
N1 Fe1 N2 82.70(9) . . ?
N4 Fe1 N2 87.14(8) . . ?
O3 Fe2 O4 96.34(8) . . ?
O3 Fe2 N5 94.44(8) . . ?
O4 Fe2 N5 87.16(8) . . ?
O3 Fe2 N7 87.71(8) . . ?
O4 Fe2 N7 94.36(8) . . ?
N5 Fe2 N7 177.21(8) . . ?
O3 Fe2 N8 88.95(8) . . ?
O4 Fe2 N8 173.88(8) . . ?
N5 Fe2 N8 95.52(9) . . ?
N7 Fe2 N8 82.74(8) . . ?
O3 Fe2 N6 174.79(8) . . ?
O4 Fe2 N6 87.90(8) . . ?
N5 Fe2 N6 82.71(8) . . ?
N7 Fe2 N6 95.00(8) . . ?
N8 Fe2 N6 86.99(8) . . ?
C1 O1 Fe1 126.07(15) . . ?
C17 O2 Fe1 125.58(15) . . ?
C33 O3 Fe2 126.83(16) . . ?
C49 O4 Fe2 125.79(15) . . ?
C7 N1 C8 120.66(19) . . ?
C7 N1 Fe1 125.27(16) . . ?
C8 N1 Fe1 114.06(15) . . ?
C15 N2 C16 118.9(2) . . ?
C15 N2 Fe1 127.81(17) . . ?
C16 N2 Fe1 113.32(15) . . ?
C31 N4 C32 119.0(2) . . ?
C31 N4 Fe1 128.26(17) . . ?
C32 N4 Fe1 112.76(15) . . ?
C39 N5 C40 120.6(2) . . ?
C39 N5 Fe2 125.41(17) . . ?
C40 N5 Fe2 113.96(15) . . ?
C47 N6 C48 119.1(2) . . ?
C47 N6 Fe2 127.71(16) . . ?
C48 N6 Fe2 113.20(15) . . ?
C55 N7 C56 120.82(19) . . ?
C55 N7 Fe2 125.43(16) . . ?
C56 N7 Fe2 113.64(15) . . ?
C63 N8 C64 118.9(2) . . ?
C63 N8 Fe2 127.98(16) . . ?
C64 N8 Fe2 113.15(16) . . ?
O1 C1 C2 117.2(2) . . ?
O1 C1 C6 125.1(2) . . ?
C2 C1 C6 117.7(2) . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 F1 119.3(2) . . ?
C5 C4 C3 122.5(2) . . ?
F1 C4 C3 118.3(2) . . ?
C4 C5 C6 119.0(2) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C1 120.0(2) . . ?
C5 C6 C7 115.9(2) . . ?
C1 C6 C7 124.0(2) . . ?
N1 C7 C6 124.3(2) . . ?
N1 C7 H7 117.9 . . ?
C6 C7 H7 117.9 . . ?
C9 C8 C16 118.9(2) . . ?
C9 C8 N1 127.7(2) . . ?
C16 C8 N1 113.4(2) . . ?
C8 C9 C10 119.7(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 121.6(2) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 120.0(2) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C16 C12 C11 118.4(2) . . ?
C16 C12 C13 117.6(2) . . ?
C11 C12 C13 124.0(2) . . ?
C14 C13 C12 119.0(2) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 120.2(2) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N2 C15 C14 122.1(2) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N2 C16 C12 122.2(2) . . ?
N2 C16 C8 116.4(2) . . ?
C12 C16 C8 121.3(2) . . ?
O2 C17 C18 117.0(2) . . ?
O2 C17 C22 124.9(2) . . ?
C18 C17 C22 118.1(2) . . ?
C19 C18 C17 121.4(2) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 119.2(2) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 F2 119.8(2) . . ?
C21 C20 C19 122.2(2) . . ?
F2 C20 C19 118.1(2) . . ?
C20 C21 C22 119.6(2) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C17 119.6(2) . . ?
C21 C22 C23 116.9(2) . . ?
C17 C22 C23 123.5(2) . . ?
N3 C23 C22 124.1(2) . . ?
N3 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
C25 C24 N3 127.8(2) . . ?
C25 C24 C32 119.1(2) . . ?
N3 C24 C32 113.1(2) . . ?
C24 C25 C26 119.6(2) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 121.5(3) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 120.4(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C32 C28 C27 117.7(2) . . ?
C32 C28 C29 117.6(2) . . ?
C27 C28 C29 124.7(3) . . ?
C30 C29 C28 119.4(2) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 119.4(2) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
N4 C31 C30 122.5(2) . . ?
N4 C31 H31 118.7 . . ?
C30 C31 H31 118.7 . . ?
N4 C32 C28 121.8(2) . . ?
N4 C32 C24 116.5(2) . . ?
C28 C32 C24 121.6(2) . . ?
O3 C33 C34 117.4(2) . . ?
O3 C33 C38 124.9(2) . . ?
C34 C33 C38 117.7(2) . . ?
C35 C34 C33 121.6(2) . . ?
C35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
C34 C35 C36 119.1(3) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C37 C36 F3 119.5(3) . . ?
C37 C36 C35 122.2(2) . . ?
F3 C36 C35 118.4(3) . . ?
C36 C37 C38 119.6(3) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C37 C38 C33 119.9(2) . . ?
C37 C38 C39 116.7(2) . . ?
C33 C38 C39 123.4(2) . . ?
N5 C39 C38 124.7(2) . . ?
N5 C39 H39 117.6 . . ?
C38 C39 H39 117.6 . . ?
C41 C40 C48 119.0(2) . . ?
C41 C40 N5 127.6(2) . . ?
C48 C40 N5 113.3(2) . . ?
C40 C41 C42 119.9(2) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 121.5(2) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C42 C43 C44 120.0(2) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C48 C44 C43 118.2(2) . . ?
C48 C44 C45 117.7(2) . . ?
C43 C44 C45 124.1(2) . . ?
C46 C45 C44 119.2(2) . . ?
C46 C45 H45 120.4 . . ?
C44 C45 H45 120.4 . . ?
C45 C46 C47 119.9(2) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
N6 C47 C46 122.2(2) . . ?
N6 C47 H47 118.9 . . ?
C46 C47 H47 118.9 . . ?
N6 C48 C44 122.0(2) . . ?
N6 C48 C40 116.7(2) . . ?
C44 C48 C40 121.3(2) . . ?
O4 C49 C50 117.3(2) . . ?
O4 C49 C54 125.0(2) . . ?
C50 C49 C54 117.7(2) . . ?
C51 C50 C49 121.9(2) . . ?
C51 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C50 C51 C52 118.8(3) . . ?
C50 C51 H51 120.6 . . ?
C52 C51 H51 120.6 . . ?
C53 C52 F4 119.5(2) . . ?
C53 C52 C51 122.2(2) . . ?
F4 C52 C51 118.2(2) . . ?
C52 C53 C54 119.5(2) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C53 C54 C49 119.8(2) . . ?
C53 C54 C55 116.6(2) . . ?
C49 C54 C55 123.5(2) . . ?
N7 C55 C54 124.5(2) . . ?
N7 C55 H55 117.7 . . ?
C54 C55 H55 117.7 . . ?
C57 C56 C64 119.2(2) . . ?
C57 C56 N7 127.4(2) . . ?
C64 C56 N7 113.34(19) . . ?
C56 C57 C58 119.6(2) . . ?
C56 C57 H57 120.2 . . ?
C58 C57 H57 120.2 . . ?
C59 C58 C57 121.6(2) . . ?
C59 C58 H58 119.2 . . ?
C57 C58 H58 119.2 . . ?
C58 C59 C60 120.1(2) . . ?
C58 C59 H59 119.9 . . ?
C60 C59 H59 119.9 . . ?
C64 C60 C59 118.2(2) . . ?
C64 C60 C61 117.6(2) . . ?
C59 C60 C61 124.2(2) . . ?
C62 C61 C60 119.3(2) . . ?
C62 C61 H61 120.4 . . ?
C60 C61 H61 120.4 . . ?
C61 C62 C63 119.8(2) . . ?
C61 C62 H62 120.1 . . ?
C63 C62 H62 120.1 . . ?
N8 C63 C62 122.4(2) . . ?
N8 C63 H63 118.8 . . ?
C62 C63 H63 118.8 . . ?
N8 C64 C60 122.0(2) . . ?
N8 C64 C56 116.7(2) . . ?
C60 C64 C56 121.3(2) . . ?
N9 C65 S1 174.9(5) . . ?
C23 N3 C24 121.1(2) . . ?
C23 N3 Fe1 125.19(17) . . ?
C24 N3 Fe1 113.72(15) . . ?
N10 C66 S2 178.1(5) . . ?
N10' C66' S2' 178.0(7) . . ?

_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.949
_refine_diff_density_max         1.896
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 994836'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp49200k

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H20 F2 Fe N4 O2, C N S'
_chemical_formula_sum            'C33 H20 F2 Fe N5 O2 S'
_chemical_formula_weight         644.45

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.849(2)
_cell_length_b                   12.100(2)
_cell_length_c                   23.856(5)
_cell_angle_alpha                99.39(3)
_cell_angle_beta                 99.45(3)
_cell_angle_gamma                90.81(3)
_cell_volume                     2764.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    15562
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      31.54

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 201r'
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            100614
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         31.54
_reflns_number_total             15562
_reflns_number_gt                14302
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.
 
The asymmetric unit contains two iron monomers and two thiocyanate anions.
All the non-hydrogen atoms are refined anisotropically and all hydrogen 
atoms are placed in calculated positions. One of the thiocyanate anions is
disordered over two positions as a free variable resulting in N10-C66-S2 
having an occupancy of 0.539 and N10'-C66'-S2' having an occupancy of 0.461.

The following restraints were applied:
ISOR 0.001 N10'

No absorption correction has been carried out due to the small size of the
crystals and low absorption coefficient value of 0.677.

The crystal was run on the Australian synchrotron in which we were restricted
to one 360 degree phi scan and limited resolution.
;

_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)+(0.0653P)²+1.9254P] 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         15562
_refine_ls_number_parameters     816
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1258
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.060
_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 0.79526(2) 0.60319(2) 0.375368(9) 0.02545(6) Uani 1 1 d . . .
O2 O 0.65938(13) 0.51132(11) 0.39229(5) 0.0336(3) Uani 1 1 d . . .
N4 N 0.93812(14) 0.70809(12) 0.36240(6) 0.0276(3) Uani 1 1 d . . .
N1 N 0.70171(14) 0.58143(12) 0.29567(6) 0.0265(3) Uani 1 1 d . . .
N3 N 0.88982(14) 0.63932(13) 0.45457(6) 0.0283(3) Uani 1 1 d . . .
O1 O 0.91405(13) 0.48529(11) 0.36362(5) 0.0325(3) Uani 1 1 d . . .
N2 N 0.67548(14) 0.73278(13) 0.38340(6) 0.0286(3) Uani 1 1 d . . .
C6 C 0.82320(17) 0.41839(14) 0.26239(7) 0.0286(3) Uani 1 1 d . . .
C21 C 0.7605(2) 0.44992(16) 0.53988(8) 0.0359(4) Uani 1 1 d . . .
H21 H 0.8265 0.4711 0.5739 0.043 Uiso 1 1 calc R . .
C17 C 0.66608(18) 0.46807(15) 0.43981(7) 0.0304(3) Uani 1 1 d . . .
C8 C 0.60663(17) 0.66497(15) 0.28370(7) 0.0291(3) Uani 1 1 d . . .
C22 C 0.76677(18) 0.49985(15) 0.49043(7) 0.0300(3) Uani 1 1 d . . .
C15 C 0.66638(19) 0.80485(16) 0.43063(8) 0.0346(4) Uani 1 1 d . . .
H15 H 0.7198 0.7944 0.4662 0.042 Uiso 1 1 calc R . .
C7 C 0.72314(17) 0.50087(14) 0.25519(7) 0.0283(3) Uani 1 1 d . . .
H7 H 0.6681 0.4968 0.2182 0.034 Uiso 1 1 calc R . .
C23 C 0.87044(17) 0.58621(15) 0.49594(7) 0.0301(3) Uani 1 1 d . . .
H23 H 0.9291 0.6062 0.5322 0.036 Uiso 1 1 calc R . .
C31 C 0.96498(18) 0.73093(15) 0.31300(8) 0.0315(3) Uani 1 1 d . . .
H31 H 0.9152 0.6902 0.2781 0.038 Uiso 1 1 calc R . .
C1 C 0.91254(17) 0.41455(14) 0.31550(7) 0.0293(3) Uani 1 1 d . . .
C30 C 1.0642(2) 0.81313(18) 0.31017(9) 0.0379(4) Uani 1 1 d . . .
H30 H 1.0844 0.8247 0.2739 0.046 Uiso 1 1 calc R . .
C20 C 0.6591(2) 0.37160(17) 0.53789(8) 0.0397(4) Uani 1 1 d . . .
C12 C 0.50862(19) 0.83684(17) 0.32832(9) 0.0361(4) Uani 1 1 d . . .
C5 C 0.8355(2) 0.34006(16) 0.21253(8) 0.0351(4) Uani 1 1 d . . .
H5 H 0.7770 0.3427 0.1769 0.042 Uiso 1 1 calc R . .
C32 C 1.01194(17) 0.76485(15) 0.41274(7) 0.0312(3) Uani 1 1 d . . .
C4 C 0.9314(2) 0.26157(18) 0.21619(9) 0.0415(4) Uani 1 1 d . . .
C16 C 0.59595(17) 0.74638(15) 0.33251(7) 0.0297(3) Uani 1 1 d . . .
C24 C 0.98674(17) 0.73073(16) 0.46425(7) 0.0324(3) Uani 1 1 d . . .
C13 C 0.5037(2) 0.91365(18) 0.37931(10) 0.0420(4) Uani 1 1 d . . .
H13 H 0.4476 0.9768 0.3784 0.050 Uiso 1 1 calc R . .
C29 C 1.1317(2) 0.87639(19) 0.35974(9) 0.0429(4) Uani 1 1 d . . .
H29 H 1.1946 0.9356 0.3582 0.051 Uiso 1 1 calc R . .
C19 C 0.5598(2) 0.33842(18) 0.48925(9) 0.0418(4) Uani 1 1 d . . .
H19 H 0.4901 0.2833 0.4892 0.050 Uiso 1 1 calc R . .
C9 C 0.5283(2) 0.67450(18) 0.23130(8) 0.0376(4) Uani 1 1 d . . .
H9 H 0.5332 0.6201 0.1982 0.045 Uiso 1 1 calc R . .
C14 C 0.5803(2) 0.89616(18) 0.42986(9) 0.0410(4) Uani 1 1 d . . .
H14 H 0.5755 0.9459 0.4646 0.049 Uiso 1 1 calc R . .
C2 C 1.0091(2) 0.32942(17) 0.31619(8) 0.0387(4) Uani 1 1 d . . .
H2 H 1.0688 0.3243 0.3512 0.046 Uiso 1 1 calc R . .
C28 C 1.1072(2) 0.85300(18) 0.41340(9) 0.0407(4) Uani 1 1 d . . .
C3 C 1.0187(2) 0.25383(19) 0.26759(9) 0.0444(5) Uani 1 1 d . . .
H3 H 1.0841 0.1969 0.2689 0.053 Uiso 1 1 calc R . .
C18 C 0.5637(2) 0.38654(17) 0.44107(8) 0.0376(4) Uani 1 1 d . . .
H18 H 0.4956 0.3642 0.4078 0.045 Uiso 1 1 calc R . .
C11 C 0.4317(2) 0.84507(19) 0.27374(9) 0.0435(4) Uani 1 1 d . . .
H11 H 0.3735 0.9062 0.2695 0.052 Uiso 1 1 calc R . .
C10 C 0.4412(2) 0.7651(2) 0.22702(9) 0.0442(5) Uani 1 1 d . . .
H10 H 0.3876 0.7709 0.1908 0.053 Uiso 1 1 calc R . .
C25 C 1.0534(2) 0.7882(2) 0.51631(8) 0.0448(5) Uani 1 1 d . . .
H25 H 1.0371 0.7673 0.5514 0.054 Uiso 1 1 calc R . .
C27 C 1.1726(3) 0.9107(2) 0.46757(10) 0.0578(7) Uani 1 1 d . . .
H27 H 1.2352 0.9722 0.4696 0.069 Uiso 1 1 calc R . .
C26 C 1.1460(3) 0.8783(2) 0.51715(10) 0.0598(7) Uani 1 1 d . . .
H26 H 1.1915 0.9177 0.5532 0.072 Uiso 1 1 calc R . .
Fe2 Fe 0.44476(3) 0.20765(2) 0.124644(9) 0.02739(7) Uani 1 1 d . . .
O3 O 0.55574(14) 0.31387(12) 0.10033(6) 0.0374(3) Uani 1 1 d . . .
N7 N 0.46335(15) 0.28121(12) 0.21232(6) 0.0284(3) Uani 1 1 d . . .
N6 N 0.29405(16) 0.08083(12) 0.12787(6) 0.0309(3) Uani 1 1 d . . .
O4 O 0.58693(15) 0.11103(12) 0.14672(6) 0.0393(3) Uani 1 1 d . . .
N8 N 0.27606(15) 0.31633(12) 0.12486(6) 0.0298(3) Uani 1 1 d . . .
C64 C 0.27336(18) 0.38493(14) 0.17630(7) 0.0296(3) Uani 1 1 d . . .
C54 C 0.62425(19) 0.14996(17) 0.24991(8) 0.0348(4) Uani 1 1 d . . .
C48 C 0.25093(19) 0.01015(15) 0.07710(7) 0.0316(3) Uani 1 1 d . . .
C63 C 0.1809(2) 0.32622(17) 0.08024(8) 0.0372(4) Uani 1 1 d . . .
H63 H 0.1834 0.2791 0.0445 0.045 Uiso 1 1 calc R . .
C56 C 0.37523(18) 0.37107(14) 0.22396(7) 0.0300(3) Uani 1 1 d . . .
C40 C 0.30137(19) 0.03342(15) 0.02754(7) 0.0316(3) Uani 1 1 d . . .
C55 C 0.54020(19) 0.24510(16) 0.25489(7) 0.0329(3) Uani 1 1 d . . .
H55 H 0.5403 0.2856 0.2925 0.040 Uiso 1 1 calc R . .
C33 C 0.57367(19) 0.33486(17) 0.04967(8) 0.0346(4) Uani 1 1 d . . .
C49 C 0.64073(19) 0.08482(17) 0.19667(8) 0.0349(4) Uani 1 1 d . . .
C57 C 0.3791(2) 0.44199(17) 0.27576(8) 0.0387(4) Uani 1 1 d . . .
H57 H 0.4488 0.4354 0.3076 0.046 Uiso 1 1 calc R . .
C60 C 0.1728(2) 0.46562(16) 0.18244(9) 0.0373(4) Uani 1 1 d . . .
C47 C 0.2473(2) 0.06292(17) 0.17462(8) 0.0387(4) Uani 1 1 d . . .
H47 H 0.2779 0.1124 0.2098 0.046 Uiso 1 1 calc R . .
C34 C 0.6587(2) 0.42761(19) 0.04705(9) 0.0422(4) Uani 1 1 d . . .
H34 H 0.7015 0.4734 0.0819 0.051 Uiso 1 1 calc R . .
C62 C 0.0760(2) 0.40334(19) 0.08332(10) 0.0441(4) Uani 1 1 d . . .
H62 H 0.0085 0.4071 0.0504 0.053 Uiso 1 1 calc R . .
F4 F 0.8218(2) -0.00931(18) 0.34992(7) 0.0791(6) Uani 1 1 d . . .
C41 C 0.2631(2) -0.03846(18) -0.02392(8) 0.0437(5) Uani 1 1 d . . .
H41 H 0.2971 -0.0248 -0.0573 0.052 Uiso 1 1 calc R . .
C53 C 0.6884(2) 0.1176(2) 0.30207(9) 0.0457(5) Uani 1 1 d . . .
H53 H 0.6795 0.1610 0.3381 0.055 Uiso 1 1 calc R . .
C38 C 0.5103(2) 0.26828(18) -0.00283(8) 0.0394(4) Uani 1 1 d . . .
C61 C 0.0721(2) 0.47243(19) 0.13380(11) 0.0451(5) Uani 1 1 d . . .
H61 H 0.0020 0.5252 0.1364 0.054 Uiso 1 1 calc R . .
C44 C 0.1601(2) -0.08287(17) 0.07351(9) 0.0417(4) Uani 1 1 d . . .
C58 C 0.2802(3) 0.52410(19) 0.28164(10) 0.0476(5) Uani 1 1 d . . .
H58 H 0.2839 0.5726 0.3175 0.057 Uiso 1 1 calc R . .
C46 C 0.1546(2) -0.02607(19) 0.17439(9) 0.0454(5) Uani 1 1 d . . .
H46 H 0.1220 -0.0356 0.2087 0.054 Uiso 1 1 calc R . .
C52 C 0.7626(3) 0.0237(2) 0.29989(10) 0.0528(6) Uani 1 1 d . . .
C45 C 0.1116(3) -0.09871(19) 0.12449(10) 0.0480(5) Uani 1 1 d . . .
H45 H 0.0493 -0.1598 0.1238 0.058 Uiso 1 1 calc R . .
C36 C 0.6165(3) 0.3876(2) -0.05525(10) 0.0568(7) Uani 1 1 d . . .
C51 C 0.7790(3) -0.0413(2) 0.24862(11) 0.0553(6) Uani 1 1 d . . .
H51 H 0.8314 -0.1067 0.2486 0.066 Uiso 1 1 calc R . .
C35 C 0.6814(3) 0.4535(2) -0.00468(10) 0.0510(6) Uani 1 1 d . . .
H35 H 0.7405 0.5155 -0.0058 0.061 Uiso 1 1 calc R . .
C59 C 0.1788(2) 0.53517(19) 0.23647(11) 0.0474(5) Uani 1 1 d . . .
H59 H 0.1119 0.5901 0.2415 0.057 Uiso 1 1 calc R . .
C50 C 0.7192(2) -0.0109(2) 0.19761(9) 0.0464(5) Uani 1 1 d . . .
H50 H 0.7311 -0.0556 0.1622 0.056 Uiso 1 1 calc R . .
C43 C 0.1222(3) -0.1537(2) 0.01968(10) 0.0552(6) Uani 1 1 d . . .
H43 H 0.0606 -0.2166 0.0162 0.066 Uiso 1 1 calc R . .
C42 C 0.1741(3) -0.1318(2) -0.02738(10) 0.0558(6) Uani 1 1 d . . .
H42 H 0.1493 -0.1808 -0.0632 0.067 Uiso 1 1 calc R . .
S1 S 0.81163(8) 0.69155(7) 0.16475(3) 0.06365(18) Uani 1 1 d . . .
N10' N 0.3381(6) 0.1464(5) 0.3323(3) 0.0135(9) Uani 0.461(5) 1 d PU A 2
N5 N 0.38903(15) 0.13139(12) 0.03743(6) 0.0293(3) Uani 1 1 d . . .
F3 F 0.6381(2) 0.41576(18) -0.10621(6) 0.0865(7) Uani 1 1 d . . .
C39 C 0.4225(2) 0.17135(18) -0.00607(8) 0.0390(4) Uani 1 1 d . . .
H39 H 0.3852 0.1326 -0.0435 0.047 Uiso 1 1 calc R . .
C37 C 0.5324(3) 0.2975(2) -0.05599(9) 0.0526(6) Uani 1 1 d . . .
H37 H 0.4890 0.2546 -0.0915 0.063 Uiso 1 1 calc R . .
C65 C 0.8413(3) 0.6923(2) 0.09999(12) 0.0593(7) Uani 1 1 d . . .
N9 N 0.8515(4) 0.7038(4) 0.05973(13) 0.140(2) Uani 1 1 d . . .
F2 F 0.65272(17) 0.32341(13) 0.58527(6) 0.0559(4) Uani 1 1 d . . .
F1 F 0.94512(17) 0.18705(13) 0.16839(6) 0.0613(4) Uani 1 1 d . . .
C66 C 0.2762(4) 0.1773(3) 0.38882(19) 0.0353(8) Uani 0.539(5) 1 d P A 1
S2' S 0.2428(3) 0.1709(3) 0.42113(14) 0.0630(8) Uiso 0.461(5) 1 d P A 2
N10 N 0.2463(8) 0.2008(6) 0.4266(2) 0.065(2) Uani 0.539(5) 1 d P A 1
C66' C 0.2950(5) 0.1549(4) 0.3575(3) 0.0427(11) Uani 0.461(5) 1 d P A 2
S2 S 0.3335(4) 0.1446(3) 0.32580(16) 0.0675(11) Uani 0.539(5) 1 d P A 1


_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 O2 1.8632(14) . ?
Fe1 O1 1.8726(14) . ?
Fe1 N3 1.9414(15) . ?
Fe1 N1 1.9461(14) . ?
Fe1 N4 1.9767(15) . ?
Fe1 N2 1.9788(16) . ?
O2 C17 1.316(2) . ?
N4 C31 1.320(2) . ?
N4 C32 1.368(2) . ?
N1 C7 1.301(2) . ?
N1 C8 1.419(2) . ?
N3 C23 1.300(2) . ?
N3 C24 1.415(2) . ?
O1 C1 1.313(2) . ?
N2 C15 1.324(2) . ?
N2 C16 1.368(2) . ?
C6 C5 1.418(2) . ?
C6 C7 1.423(2) . ?
C6 C1 1.427(2) . ?
C21 C20 1.357(3) . ?
C21 C22 1.420(2) . ?
C21 H21 0.9500 . ?
C17 C18 1.408(2) . ?
C17 C22 1.426(2) . ?
C8 C9 1.380(2) . ?
C8 C16 1.416(2) . ?
C22 C23 1.426(2) . ?
C15 C14 1.402(3) . ?
C15 H15 0.9500 . ?
C7 H7 0.9500 . ?
C23 H23 0.9500 . ?
C31 C30 1.402(3) . ?
C31 H31 0.9500 . ?
C1 C2 1.412(3) . ?
C30 C29 1.363(3) . ?
C30 H30 0.9500 . ?
C20 F2 1.363(2) . ?
C20 C19 1.389(3) . ?
C12 C16 1.408(3) . ?
C12 C13 1.413(3) . ?
C12 C11 1.414(3) . ?
C5 C4 1.351(3) . ?
C5 H5 0.9500 . ?
C32 C28 1.407(3) . ?
C32 C24 1.416(2) . ?
C4 F1 1.360(2) . ?
C4 C3 1.395(3) . ?
C24 C25 1.377(2) . ?
C13 C14 1.363(3) . ?
C13 H13 0.9500 . ?
C29 C28 1.412(3) . ?
C29 H29 0.9500 . ?
C19 C18 1.376(3) . ?
C19 H19 0.9500 . ?
C9 C10 1.409(3) . ?
C9 H9 0.9500 . ?
C14 H14 0.9500 . ?
C2 C3 1.372(3) . ?
C2 H2 0.9500 . ?
C28 C27 1.411(3) . ?
C3 H3 0.9500 . ?
C18 H18 0.9500 . ?
C11 C10 1.368(3) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
C25 C26 1.406(3) . ?
C25 H25 0.9500 . ?
C27 C26 1.368(4) . ?
C27 H27 0.9500 . ?
C26 H26 0.9500 . ?
Fe2 O3 1.8960(15) . ?
Fe2 O4 1.9000(15) . ?
Fe2 N7 2.1124(15) . ?
Fe2 N5 2.1133(16) . ?
Fe2 N8 2.1336(16) . ?
Fe2 N6 2.1391(16) . ?
O3 C33 1.313(2) . ?
N7 C55 1.303(2) . ?
N7 C56 1.421(2) . ?
N6 C47 1.322(2) . ?
N6 C48 1.364(2) . ?
O4 C49 1.312(2) . ?
N8 C63 1.320(2) . ?
N8 C64 1.369(2) . ?
C64 C60 1.409(3) . ?
C64 C56 1.421(2) . ?
C54 C49 1.416(3) . ?
C54 C53 1.417(3) . ?
C54 C55 1.428(3) . ?
C48 C44 1.410(3) . ?
C48 C40 1.422(2) . ?
C63 C62 1.404(3) . ?
C63 H63 0.9500 . ?
C56 C57 1.379(2) . ?
C40 C41 1.377(3) . ?
C40 N5 1.421(2) . ?
C55 H55 0.9500 . ?
C33 C34 1.407(3) . ?
C33 C38 1.417(3) . ?
C49 C50 1.403(3) . ?
C57 C58 1.408(3) . ?
C57 H57 0.9500 . ?
C60 C61 1.411(3) . ?
C60 C59 1.412(3) . ?
C47 C46 1.401(3) . ?
C47 H47 0.9500 . ?
C34 C35 1.373(3) . ?
C34 H34 0.9500 . ?
C62 C61 1.356(3) . ?
C62 H62 0.9500 . ?
F4 C52 1.363(2) . ?
C41 C42 1.403(3) . ?
C41 H41 0.9500 . ?
C53 C52 1.358(3) . ?
C53 H53 0.9500 . ?
C38 C37 1.420(3) . ?
C38 C39 1.431(3) . ?
C61 H61 0.9500 . ?
C44 C43 1.414(3) . ?
C44 C45 1.417(3) . ?
C58 C59 1.369(4) . ?
C58 H58 0.9500 . ?
C46 C45 1.361(3) . ?
C46 H46 0.9500 . ?
C52 C51 1.377(4) . ?
C45 H45 0.9500 . ?
C36 C37 1.355(3) . ?
C36 F3 1.363(2) . ?
C36 C35 1.385(3) . ?
C51 C50 1.371(3) . ?
C51 H51 0.9500 . ?
C35 H35 0.9500 . ?
C59 H59 0.9500 . ?
C50 H50 0.9500 . ?
C43 C42 1.369(3) . ?
C43 H43 0.9500 . ?
C42 H42 0.9500 . ?
S1 C65 1.620(3) . ?
N10' C66' 0.787(10) . ?
N5 C39 1.300(2) . ?
C39 H39 0.9500 . ?
C37 H37 0.9500 . ?
C65 N9 1.013(4) . ?
C66 N10 0.994(8) . ?
C66 S2 1.681(6) . ?
S2' C66' 1.663(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 93.25(6) . . ?
O2 Fe1 N3 94.43(6) . . ?
O1 Fe1 N3 88.62(6) . . ?
O2 Fe1 N1 89.14(6) . . ?
O1 Fe1 N1 94.96(6) . . ?
N3 Fe1 N1 174.80(6) . . ?
O2 Fe1 N4 175.95(6) . . ?
O1 Fe1 N4 89.38(6) . . ?
N3 Fe1 N4 82.56(7) . . ?
N1 Fe1 N4 93.69(6) . . ?
O2 Fe1 N2 90.37(6) . . ?
O1 Fe1 N2 175.73(6) . . ?
N3 Fe1 N2 93.35(7) . . ?
N1 Fe1 N2 82.82(7) . . ?
N4 Fe1 N2 87.12(6) . . ?
C17 O2 Fe1 125.57(11) . . ?
C31 N4 C32 118.87(15) . . ?
C31 N4 Fe1 128.42(12) . . ?
C32 N4 Fe1 112.66(11) . . ?
C7 N1 C8 120.89(14) . . ?
C7 N1 Fe1 125.27(12) . . ?
C8 N1 Fe1 113.82(11) . . ?
C23 N3 C24 121.28(14) . . ?
C23 N3 Fe1 125.12(12) . . ?
C24 N3 Fe1 113.59(11) . . ?
C1 O1 Fe1 126.22(11) . . ?
C15 N2 C16 118.88(16) . . ?
C15 N2 Fe1 127.95(13) . . ?
C16 N2 Fe1 113.16(12) . . ?
C5 C6 C7 116.43(15) . . ?
C5 C6 C1 119.97(16) . . ?
C7 C6 C1 123.55(15) . . ?
C20 C21 C22 119.20(17) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
O2 C17 C18 117.29(15) . . ?
O2 C17 C22 124.91(16) . . ?
C18 C17 C22 117.78(16) . . ?
C9 C8 C16 118.92(16) . . ?
C9 C8 N1 127.50(16) . . ?
C16 C8 N1 113.58(14) . . ?
C21 C22 C23 116.86(15) . . ?
C21 C22 C17 119.76(16) . . ?
C23 C22 C17 123.24(15) . . ?
N2 C15 C14 122.10(18) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N1 C7 C6 124.62(15) . . ?
N1 C7 H7 117.7 . . ?
C6 C7 H7 117.7 . . ?
N3 C23 C22 124.17(15) . . ?
N3 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
N4 C31 C30 122.42(17) . . ?
N4 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
O1 C1 C2 117.24(15) . . ?
O1 C1 C6 125.20(16) . . ?
C2 C1 C6 117.55(16) . . ?
C29 C30 C31 119.64(18) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C21 C20 F2 119.39(18) . . ?
C21 C20 C19 122.54(18) . . ?
F2 C20 C19 118.07(18) . . ?
C16 C12 C13 117.48(18) . . ?
C16 C12 C11 118.22(18) . . ?
C13 C12 C11 124.30(19) . . ?
C4 C5 C6 119.27(17) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
N4 C32 C28 121.85(17) . . ?
N4 C32 C24 116.47(15) . . ?
C28 C32 C24 121.67(16) . . ?
C5 C4 F1 119.64(18) . . ?
C5 C4 C3 122.41(18) . . ?
F1 C4 C3 117.95(19) . . ?
N2 C16 C12 122.14(16) . . ?
N2 C16 C8 116.53(15) . . ?
C12 C16 C8 121.33(16) . . ?
C25 C24 N3 127.80(17) . . ?
C25 C24 C32 118.97(17) . . ?
N3 C24 C32 113.21(15) . . ?
C14 C13 C12 119.27(19) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C30 C29 C28 119.36(18) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C18 C19 C20 119.05(18) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
C8 C9 C10 119.81(19) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C13 C14 C15 120.06(18) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C3 C2 C1 121.62(17) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C32 C28 C27 117.71(19) . . ?
C32 C28 C29 117.56(18) . . ?
C27 C28 C29 124.73(19) . . ?
C2 C3 C4 119.17(19) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C19 C18 C17 121.67(18) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C10 C11 C12 120.03(19) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C10 C9 121.68(18) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C24 C25 C26 119.5(2) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C26 C27 C28 120.2(2) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C26 C25 122.0(2) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
O3 Fe2 O4 97.45(7) . . ?
O3 Fe2 N7 98.60(6) . . ?
O4 Fe2 N7 88.16(6) . . ?
O3 Fe2 N5 88.35(6) . . ?
O4 Fe2 N5 98.14(7) . . ?
N7 Fe2 N5 169.98(6) . . ?
O3 Fe2 N8 92.20(6) . . ?
O4 Fe2 N8 163.36(6) . . ?
N7 Fe2 N8 76.98(6) . . ?
N5 Fe2 N8 95.65(6) . . ?
O3 Fe2 N6 164.34(6) . . ?
O4 Fe2 N6 89.73(7) . . ?
N7 Fe2 N6 95.51(6) . . ?
N5 Fe2 N6 76.83(6) . . ?
N8 Fe2 N6 84.37(6) . . ?
C33 O3 Fe2 133.83(12) . . ?
C55 N7 C56 119.69(15) . . ?
C55 N7 Fe2 124.96(13) . . ?
C56 N7 Fe2 115.15(11) . . ?
C47 N6 C48 119.13(16) . . ?
C47 N6 Fe2 125.61(13) . . ?
C48 N6 Fe2 115.14(11) . . ?
C49 O4 Fe2 132.68(12) . . ?
C63 N8 C64 118.64(16) . . ?
C63 N8 Fe2 126.31(13) . . ?
C64 N8 Fe2 114.97(11) . . ?
N8 C64 C60 121.70(17) . . ?
N8 C64 C56 117.55(15) . . ?
C60 C64 C56 120.74(17) . . ?
C49 C54 C53 119.36(18) . . ?
C49 C54 C55 123.85(16) . . ?
C53 C54 C55 116.72(17) . . ?
N6 C48 C44 121.67(16) . . ?
N6 C48 C40 117.47(15) . . ?
C44 C48 C40 120.86(16) . . ?
N8 C63 C62 122.89(19) . . ?
N8 C63 H63 118.6 . . ?
C62 C63 H63 118.6 . . ?
C57 C56 C64 119.04(17) . . ?
C57 C56 N7 126.61(17) . . ?
C64 C56 N7 114.34(15) . . ?
C41 C40 N5 126.72(17) . . ?
C41 C40 C48 118.76(17) . . ?
N5 C40 C48 114.52(15) . . ?
N7 C55 C54 125.69(17) . . ?
N7 C55 H55 117.2 . . ?
C54 C55 H55 117.2 . . ?
O3 C33 C34 118.95(17) . . ?
O3 C33 C38 122.81(17) . . ?
C34 C33 C38 118.24(17) . . ?
O4 C49 C50 118.87(18) . . ?
O4 C49 C54 122.73(17) . . ?
C50 C49 C54 118.40(17) . . ?
C56 C57 C58 120.19(19) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C64 C60 C61 117.74(18) . . ?
C64 C60 C59 118.41(19) . . ?
C61 C60 C59 123.85(19) . . ?
N6 C47 C46 122.69(18) . . ?
N6 C47 H47 118.7 . . ?
C46 C47 H47 118.7 . . ?
C35 C34 C33 121.49(19) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C61 C62 C63 119.32(19) . . ?
C61 C62 H62 120.3 . . ?
C63 C62 H62 120.3 . . ?
C40 C41 C42 120.41(19) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C52 C53 C54 119.2(2) . . ?
C52 C53 H53 120.4 . . ?
C54 C53 H53 120.4 . . ?
C33 C38 C37 119.56(18) . . ?
C33 C38 C39 123.73(17) . . ?
C37 C38 C39 116.71(18) . . ?
C62 C61 C60 119.69(19) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C48 C44 C43 118.50(19) . . ?
C48 C44 C45 117.47(18) . . ?
C43 C44 C45 124.03(19) . . ?
C59 C58 C57 121.0(2) . . ?
C59 C58 H58 119.5 . . ?
C57 C58 H58 119.5 . . ?
C45 C46 C47 119.32(19) . . ?
C45 C46 H46 120.3 . . ?
C47 C46 H46 120.3 . . ?
C53 C52 F4 119.5(2) . . ?
C53 C52 C51 122.4(2) . . ?
F4 C52 C51 118.1(2) . . ?
C46 C45 C44 119.70(19) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C37 C36 F3 119.1(2) . . ?
C37 C36 C35 122.8(2) . . ?
F3 C36 C35 118.1(2) . . ?
C50 C51 C52 119.4(2) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
C34 C35 C36 118.9(2) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C58 C59 C60 120.5(2) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C51 C50 C49 121.2(2) . . ?
C51 C50 H50 119.4 . . ?
C49 C50 H50 119.4 . . ?
C42 C43 C44 120.0(2) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C42 C41 121.4(2) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C39 N5 C40 119.79(15) . . ?
C39 N5 Fe2 124.77(12) . . ?
C40 N5 Fe2 115.31(11) . . ?
N5 C39 C38 126.07(17) . . ?
N5 C39 H39 117.0 . . ?
C38 C39 H39 117.0 . . ?
C36 C37 C38 119.0(2) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
N9 C65 S1 171.1(4) . . ?
N10 C66 S2 176.4(5) . . ?
N10' C66' S2' 165.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.843
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 994837'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp49270k

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C32 H20 F2 Fe N4 O2, (C N S)
;
_chemical_formula_sum            'C33 H20 F2 Fe N5 O2 S'
_chemical_formula_weight         644.45

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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

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

_cell_length_a                   9.919(2)
_cell_length_b                   12.084(2)
_cell_length_c                   23.951(5)
_cell_angle_alpha                99.55(3)
_cell_angle_beta                 99.39(3)
_cell_angle_gamma                90.62(3)
_cell_volume                     2791.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    15635
_cell_measurement_theta_min      0.87
_cell_measurement_theta_max      31.57

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'ADSC Quantum 201r'
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            102859
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         0.87
_diffrn_reflns_theta_max         31.57
_reflns_number_total             15635
_reflns_number_gt                13576
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.

The asymmetric unit contains two iron monomers and two thiocyanate anions.
All the non-hydrogen atoms are refined anisotropically and all hydrogen 
atoms are placed in calculated positions. One of the thiocyanate anions is
disordered over two positions with N10-C66-S2 having half occupancy and 
N10'-C66'-S2' having half occupancy.

The following restraints were used:
DFIX 1.17 0.001 C66 N10 C66' N10'
DFIX 1.65 0.001 S2 C66 S2' C66'
DANG 2.82 0.001 S2 N10 S2' N10'
ISOR 0.001 S2 C66 N10 S2' C66' N10'

No absorption correction has been carried out due to the small size of the
crystals and low absorption coefficient value of 0.671.

The crystal was run on the Australian synchrotron in which we were restricted
to one 360 degree phi scan and limited resolution.  
;

_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)+(0.0853P)²+1.5502P] 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         15635
_refine_ls_number_parameters     812
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1589
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.093
_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 0.20450(3) 0.39820(2) 0.124480(11) 0.03524(8) Uani 1 1 d . . .
Fe2 Fe 0.55476(3) 0.79399(2) 0.375563(11) 0.03644(8) Uani 1 1 d . . .
S2 S 0.7459(2) 0.8228(2) 0.07858(8) 0.0720(4) Uani 0.50 1 d PDU A 1
S2' S 0.66409(18) 0.85112(15) 0.17108(8) 0.0596(3) Uani 0.50 1 d PDU B 2
F1 F 0.0542(2) 0.81315(18) 0.33248(8) 0.0889(7) Uani 1 1 d . . .
F2 F 0.3452(2) 0.67509(17) -0.08599(8) 0.0787(5) Uani 1 1 d . . .
F3 F 0.3619(3) 0.5867(3) 0.60503(9) 0.1238(12) Uani 1 1 d . . .
F4 F 0.1787(3) 1.0087(2) 0.15122(9) 0.1081(9) Uani 1 1 d . . .
O1 O 0.08661(17) 0.51599(14) 0.13747(7) 0.0471(3) Uani 1 1 d . . .
O2 O 0.33848(16) 0.48902(15) 0.10663(7) 0.0480(4) Uani 1 1 d . . .
O3 O 0.44459(18) 0.68815(15) 0.39981(7) 0.0498(4) Uani 1 1 d . . .
O4 O 0.41366(19) 0.89100(15) 0.35361(7) 0.0513(4) Uani 1 1 d . . .
N1 N 0.29695(16) 0.41887(14) 0.20494(7) 0.0363(3) Uani 1 1 d . . .
N2 N 0.32545(17) 0.26697(15) 0.11730(7) 0.0386(3) Uani 1 1 d . . .
N3 N 0.11081(17) 0.36003(15) 0.04456(7) 0.0377(3) Uani 1 1 d . . .
N4 N 0.06047(17) 0.29165(15) 0.13637(7) 0.0380(3) Uani 1 1 d . . .
N5 N 0.61080(18) 0.87020(15) 0.46247(7) 0.0390(3) Uani 1 1 d . . .
N6 N 0.70420(19) 0.92095(15) 0.37232(7) 0.0410(4) Uani 1 1 d . . .
N7 N 0.53709(18) 0.71980(14) 0.28814(7) 0.0375(3) Uani 1 1 d . . .
N8 N 0.72213(18) 0.68435(15) 0.37547(8) 0.0398(3) Uani 1 1 d . . .
N9 N 0.1592(5) 0.2883(4) 0.43722(16) 0.147(2) Uani 1 1 d . . .
N10 N 0.6862(12) 0.8743(10) 0.1908(2) 0.137(4) Uani 0.50 1 d PDU A 1
N10' N 0.7706(11) 0.7983(10) 0.0682(3) 0.122(4) Uani 0.50 1 d PDU B 2
C1 C 0.0873(2) 0.58643(19) 0.18538(10) 0.0422(4) Uani 1 1 d . . .
C2 C -0.0088(3) 0.6716(2) 0.18518(12) 0.0549(6) Uani 1 1 d . . .
H2 H -0.0669 0.6770 0.1512 0.066 Uiso 1 1 calc R . .
C3 C -0.0189(3) 0.7464(3) 0.23364(13) 0.0638(7) Uani 1 1 d . . .
H3 H -0.0831 0.8019 0.2326 0.077 Uiso 1 1 calc R . .
C4 C 0.0679(3) 0.7387(2) 0.28459(12) 0.0597(6) Uani 1 1 d . . .
C5 C 0.1633(2) 0.6601(2) 0.28822(10) 0.0493(5) Uani 1 1 d . . .
H5 H 0.2199 0.6573 0.3229 0.059 Uiso 1 1 calc R . .
C6 C 0.1757(2) 0.58186(18) 0.23837(9) 0.0397(4) Uani 1 1 d . . .
C7 C 0.2749(2) 0.49928(18) 0.24530(9) 0.0387(4) Uani 1 1 d . . .
H7 H 0.3279 0.5030 0.2814 0.046 Uiso 1 1 calc R . .
C9 C 0.4691(3) 0.3253(2) 0.26886(11) 0.0520(5) Uani 1 1 d . . .
H9 H 0.4631 0.3779 0.3014 0.062 Uiso 1 1 calc R . .
C10 C 0.5559(3) 0.2347(3) 0.27298(12) 0.0615(7) Uani 1 1 d . . .
H10 H 0.6078 0.2291 0.3083 0.074 Uiso 1 1 calc R . .
C11 C 0.5660(3) 0.1550(3) 0.22675(13) 0.0596(6) Uani 1 1 d . . .
H11 H 0.6229 0.0952 0.2310 0.072 Uiso 1 1 calc R . .
C12 C 0.4905(2) 0.1629(2) 0.17223(11) 0.0488(5) Uani 1 1 d . . .
C13 C 0.4961(3) 0.0860(2) 0.12132(13) 0.0573(6) Uani 1 1 d . . .
H13 H 0.5511 0.0242 0.1222 0.069 Uiso 1 1 calc R . .
C14 C 0.4207(3) 0.1033(2) 0.07126(12) 0.0558(6) Uani 1 1 d . . .
H14 H 0.4258 0.0543 0.0374 0.067 Uiso 1 1 calc R . .
C15 C 0.3352(2) 0.1946(2) 0.07032(10) 0.0467(5) Uani 1 1 d . . .
H15 H 0.2835 0.2047 0.0356 0.056 Uiso 1 1 calc R . .
C16 C 0.4030(2) 0.25379(18) 0.16798(9) 0.0399(4) Uani 1 1 d . . .
C17 C 0.3321(2) 0.53205(19) 0.05931(10) 0.0435(4) Uani 1 1 d . . .
C18 C 0.4331(3) 0.6138(2) 0.05803(12) 0.0539(6) Uani 1 1 d . . .
H18 H 0.4989 0.6363 0.0905 0.065 Uiso 1 1 calc R . .
C19 C 0.4366(3) 0.6612(2) 0.00993(13) 0.0600(6) Uani 1 1 d . . .
H19 H 0.5039 0.7154 0.0100 0.072 Uiso 1 1 calc R . .
C20 C 0.3390(3) 0.6277(2) -0.03867(12) 0.0566(6) Uani 1 1 d . . .
C21 C 0.2386(3) 0.5489(2) -0.04045(10) 0.0499(5) Uani 1 1 d . . .
H21 H 0.1746 0.5277 -0.0736 0.060 Uiso 1 1 calc R . .
C22 C 0.2327(2) 0.49952(19) 0.00869(9) 0.0419(4) Uani 1 1 d . . .
C23 C 0.12868(9) 0.41234(8) 0.00355(4) 0.0408(4) Uani 1 1 d . . .
H23 H 0.0710 0.3927 -0.0316 0.049 Uiso 1 1 calc R . .
C8 C 0.39367(9) 0.33600(8) 0.21716(4) 0.0398(4) Uani 1 1 d R . .
S1 S 0.18274(9) 0.30956(8) 0.33485(4) 0.0921(3) Uani 1 1 d R . .
C65 C 0.15754(9) 0.30816(8) 0.40115(4) 0.0862(11) Uani 1 1 d R . .
C24 C 0.0144(2) 0.26879(19) 0.03486(9) 0.0433(4) Uani 1 1 d . . .
C25 C -0.0508(3) 0.2114(3) -0.01686(11) 0.0604(7) Uani 1 1 d . . .
H25 H -0.0340 0.2314 -0.0510 0.072 Uiso 1 1 calc R . .
C26 C -0.1433(4) 0.1218(3) -0.01778(14) 0.0796(10) Uani 1 1 d . . .
H26 H -0.1878 0.0835 -0.0530 0.095 Uiso 1 1 calc R . .
C27 C -0.1697(3) 0.0893(3) 0.03125(14) 0.0754(9) Uani 1 1 d . . .
H27 H -0.2301 0.0286 0.0290 0.090 Uiso 1 1 calc R . .
C28 C -0.1064(3) 0.1468(2) 0.08515(11) 0.0535(6) Uani 1 1 d . . .
C29 C -0.1309(3) 0.1233(2) 0.13844(13) 0.0574(6) Uani 1 1 d . . .
H29 H -0.1919 0.0651 0.1397 0.069 Uiso 1 1 calc R . .
C30 C -0.0650(3) 0.1859(2) 0.18786(11) 0.0521(5) Uani 1 1 d . . .
H30 H -0.0850 0.1741 0.2231 0.063 Uiso 1 1 calc R . .
C31 C 0.0333(2) 0.26842(19) 0.18562(10) 0.0434(4) Uani 1 1 d . . .
H31 H 0.0810 0.3082 0.2198 0.052 Uiso 1 1 calc R . .
C32 C -0.0115(2) 0.23513(18) 0.08615(9) 0.0413(4) Uani 1 1 d . . .
C33 C 0.4260(2) 0.6678(2) 0.45006(10) 0.0458(5) Uani 1 1 d . . .
C34 C 0.3421(3) 0.5747(2) 0.45266(12) 0.0572(6) Uani 1 1 d . . .
H34 H 0.3013 0.5293 0.4187 0.069 Uiso 1 1 calc R . .
C35 C 0.3193(3) 0.5495(3) 0.50426(13) 0.0713(9) Uani 1 1 d . . .
H35 H 0.2615 0.4890 0.5053 0.086 Uiso 1 1 calc R . .
C36 C 0.3828(4) 0.6149(3) 0.55429(13) 0.0793(11) Uani 1 1 d . . .
C37 C 0.4655(4) 0.7058(3) 0.55507(12) 0.0753(10) Uani 1 1 d . . .
H37 H 0.5069 0.7482 0.5898 0.090 Uiso 1 1 calc R . .
C38 C 0.4877(3) 0.7349(2) 0.50233(10) 0.0538(6) Uani 1 1 d . . .
C39 C 0.5753(3) 0.8316(2) 0.50540(10) 0.0529(6) Uani 1 1 d . . .
H39 H 0.6100 0.8705 0.5419 0.063 Uiso 1 1 calc R . .
C40 C 0.6997(2) 0.96690(18) 0.47247(9) 0.0426(4) Uani 1 1 d . . .
C41 C 0.7408(3) 1.0371(2) 0.52409(11) 0.0608(7) Uani 1 1 d . . .
H41 H 0.7089 1.0234 0.5568 0.073 Uiso 1 1 calc R . .
C42 C 0.8308(4) 1.1293(3) 0.52756(13) 0.0788(10) Uani 1 1 d . . .
H42 H 0.8568 1.1766 0.5626 0.095 Uiso 1 1 calc R . .
C43 C 0.8808(4) 1.1512(3) 0.48065(14) 0.0765(10) Uani 1 1 d . . .
H43 H 0.9420 1.2118 0.4843 0.092 Uiso 1 1 calc R . .
C44 C 0.8404(3) 1.0824(2) 0.42661(12) 0.0564(6) Uani 1 1 d . . .
C45 C 0.8869(3) 1.0987(3) 0.37585(13) 0.0642(7) Uani 1 1 d . . .
H45 H 0.9483 1.1579 0.3766 0.077 Uiso 1 1 calc R . .
C46 C 0.8418(3) 1.0277(2) 0.32601(12) 0.0604(7) Uani 1 1 d . . .
H46 H 0.8719 1.0379 0.2923 0.073 Uiso 1 1 calc R . .
C47 C 0.7498(3) 0.9394(2) 0.32562(10) 0.0510(5) Uani 1 1 d . . .
H47 H 0.7193 0.8915 0.2911 0.061 Uiso 1 1 calc R . .
C48 C 0.7486(2) 0.99014(18) 0.42298(9) 0.0417(4) Uani 1 1 d . . .
C49 C 0.3593(2) 0.9161(2) 0.30376(10) 0.0458(5) Uani 1 1 d . . .
C50 C 0.2801(3) 1.0114(3) 0.30264(12) 0.0614(7) Uani 1 1 d . . .
H50 H 0.2679 1.0553 0.3371 0.074 Uiso 1 1 calc R . .
C51 C 0.2205(4) 1.0412(3) 0.25210(14) 0.0731(9) Uani 1 1 d . . .
H51 H 0.1688 1.1050 0.2522 0.088 Uiso 1 1 calc R . .
C52 C 0.2374(3) 0.9764(3) 0.20110(13) 0.0714(9) Uani 1 1 d . . .
C53 C 0.3124(3) 0.8830(3) 0.19909(11) 0.0616(7) Uani 1 1 d . . .
H53 H 0.3215 0.8404 0.1639 0.074 Uiso 1 1 calc R . .
C54 C 0.3766(2) 0.8509(2) 0.25085(9) 0.0458(5) Uani 1 1 d . . .
C55 C 0.4606(2) 0.75603(19) 0.24607(9) 0.0430(4) Uani 1 1 d . . .
H55 H 0.4607 0.7163 0.2093 0.052 Uiso 1 1 calc R . .
C56 C 0.6245(2) 0.62985(17) 0.27677(9) 0.0397(4) Uani 1 1 d . . .
C57 C 0.6213(3) 0.5585(2) 0.22514(11) 0.0525(5) Uani 1 1 d . . .
H57 H 0.5543 0.5652 0.1940 0.063 Uiso 1 1 calc R . .
C58 C 0.7190(4) 0.4760(2) 0.21964(14) 0.0664(7) Uani 1 1 d . . .
H58 H 0.7154 0.4283 0.1847 0.080 Uiso 1 1 calc R . .
C59 C 0.8190(3) 0.4643(2) 0.26443(14) 0.0652(7) Uani 1 1 d . . .
H59 H 0.8838 0.4100 0.2594 0.078 Uiso 1 1 calc R . .
C60 C 0.8248(3) 0.5340(2) 0.31846(12) 0.0511(5) Uani 1 1 d . . .
C61 C 0.9239(3) 0.5273(2) 0.36689(14) 0.0618(7) Uani 1 1 d . . .
H61 H 0.9922 0.4754 0.3644 0.074 Uiso 1 1 calc R . .
C62 C 0.9197(3) 0.5965(3) 0.41692(13) 0.0602(6) Uani 1 1 d . . .
H62 H 0.9849 0.5927 0.4491 0.072 Uiso 1 1 calc R . .
C63 C 0.8165(2) 0.6741(2) 0.41991(11) 0.0500(5) Uani 1 1 d . . .
H63 H 0.8141 0.7206 0.4548 0.060 Uiso 1 1 calc R . .
C64 C 0.7252(2) 0.61541(17) 0.32420(9) 0.0397(4) Uani 1 1 d . . .
C66 C 0.7050(5) 0.8455(4) 0.14357(12) 0.0525(10) Uani 0.50 1 d PDU A 1
C66' C 0.7207(5) 0.8220(4) 0.10941(13) 0.0512(10) Uani 0.50 1 d PDU B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 1.8610(17) . ?
Fe1 O1 1.8703(17) . ?
Fe1 N3 1.9640(17) . ?
Fe1 N1 1.9687(17) . ?
Fe1 N4 1.9986(18) . ?
Fe1 N2 2.0004(19) . ?
Fe2 O3 1.8948(17) . ?
Fe2 O4 1.8998(18) . ?
Fe2 N5 2.1130(18) . ?
Fe2 N7 2.1148(17) . ?
Fe2 N8 2.1352(19) . ?
Fe2 N6 2.1413(19) . ?
S2 C66 1.6520(10) . ?
S2' C66' 1.6503(10) . ?
F1 C4 1.362(3) . ?
F2 C20 1.362(3) . ?
F3 C36 1.362(3) . ?
F4 C52 1.361(3) . ?
O1 C1 1.310(3) . ?
O2 C17 1.316(3) . ?
O3 C33 1.309(3) . ?
O4 C49 1.312(3) . ?
N1 C7 1.299(3) . ?
N1 C8 1.4267(19) . ?
N2 C15 1.323(3) . ?
N2 C16 1.361(3) . ?
N3 C23 1.287(2) . ?
N3 C24 1.416(3) . ?
N4 C31 1.325(3) . ?
N4 C32 1.364(3) . ?
N5 C39 1.293(3) . ?
N5 C40 1.420(3) . ?
N6 C47 1.324(3) . ?
N6 C48 1.359(3) . ?
N7 C55 1.299(3) . ?
N7 C56 1.417(3) . ?
N8 C63 1.321(3) . ?
N8 C64 1.370(3) . ?
N9 C65 0.932(3) . ?
N10 C66 1.1725(10) . ?
N10' C66' 1.1711(10) . ?
C1 C2 1.411(3) . ?
C1 C6 1.430(3) . ?
C2 C3 1.366(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(4) . ?
C5 C6 1.418(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.419(3) . ?
C7 H7 0.9300 . ?
C9 C8 1.365(2) . ?
C9 C10 1.406(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.359(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.414(4) . ?
C11 H11 0.9300 . ?
C12 C16 1.414(3) . ?
C12 C13 1.414(4) . ?
C13 C14 1.354(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.401(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C8 1.426(2) . ?
C17 C18 1.407(3) . ?
C17 C22 1.429(3) . ?
C18 C19 1.374(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.387(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.361(4) . ?
C21 C22 1.414(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.443(2) . ?
C23 H23 0.9300 . ?
S1 C65 1.6501 . ?
C24 C25 1.370(3) . ?
C24 C32 1.416(3) . ?
C25 C26 1.406(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.361(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.405(4) . ?
C27 H27 0.9300 . ?
C28 C32 1.410(3) . ?
C28 C29 1.411(4) . ?
C29 C30 1.357(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.400(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C33 C34 1.408(3) . ?
C33 C38 1.415(3) . ?
C34 C35 1.373(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.373(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.360(4) . ?
C37 C38 1.416(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.433(3) . ?
C39 H39 0.9300 . ?
C40 C41 1.377(3) . ?
C40 C48 1.419(3) . ?
C41 C42 1.403(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.362(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.412(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.411(4) . ?
C44 C48 1.415(3) . ?
C45 C46 1.356(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.394(3) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C49 C50 1.404(4) . ?
C49 C54 1.413(3) . ?
C50 C51 1.364(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.373(5) . ?
C51 H51 0.9300 . ?
C52 C53 1.357(4) . ?
C53 C54 1.414(3) . ?
C53 H53 0.9300 . ?
C54 C55 1.425(3) . ?
C55 H55 0.9300 . ?
C56 C57 1.380(3) . ?
C56 C64 1.420(3) . ?
C57 C58 1.403(4) . ?
C57 H57 0.9300 . ?
C58 C59 1.365(5) . ?
C58 H58 0.9300 . ?
C59 C60 1.415(4) . ?
C59 H59 0.9300 . ?
C60 C61 1.407(4) . ?
C60 C64 1.408(3) . ?
C61 C62 1.350(4) . ?
C61 H61 0.9300 . ?
C62 C63 1.398(4) . ?
C62 H62 0.9300 . ?
C63 H63 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 93.89(8) . . ?
O2 Fe1 N3 93.75(8) . . ?
O1 Fe1 N3 89.99(8) . . ?
O2 Fe1 N1 90.51(7) . . ?
O1 Fe1 N1 94.28(8) . . ?
N3 Fe1 N1 173.76(7) . . ?
O2 Fe1 N4 174.57(7) . . ?
O1 Fe1 N4 89.11(8) . . ?
N3 Fe1 N4 81.71(8) . . ?
N1 Fe1 N4 93.79(8) . . ?
O2 Fe1 N2 90.37(8) . . ?
O1 Fe1 N2 174.38(7) . . ?
N3 Fe1 N2 93.39(8) . . ?
N1 Fe1 N2 82.01(8) . . ?
N4 Fe1 N2 86.94(7) . . ?
O3 Fe2 O4 97.44(8) . . ?
O3 Fe2 N5 88.38(7) . . ?
O4 Fe2 N5 98.41(8) . . ?
O3 Fe2 N7 98.69(7) . . ?
O4 Fe2 N7 88.29(7) . . ?
N5 Fe2 N7 169.59(7) . . ?
O3 Fe2 N8 92.05(8) . . ?
O4 Fe2 N8 163.51(7) . . ?
N5 Fe2 N8 95.30(8) . . ?
N7 Fe2 N8 76.92(7) . . ?
O3 Fe2 N6 164.36(7) . . ?
O4 Fe2 N6 89.61(8) . . ?
N5 Fe2 N6 76.75(7) . . ?
N7 Fe2 N6 95.44(7) . . ?
N8 Fe2 N6 84.64(7) . . ?
C1 O1 Fe1 127.04(14) . . ?
C17 O2 Fe1 126.29(14) . . ?
C33 O3 Fe2 133.93(15) . . ?
C49 O4 Fe2 132.63(15) . . ?
C7 N1 C8 120.48(15) . . ?
C7 N1 Fe1 125.05(14) . . ?
C8 N1 Fe1 114.47(11) . . ?
C15 N2 C16 119.1(2) . . ?
C15 N2 Fe1 127.48(16) . . ?
C16 N2 Fe1 113.40(14) . . ?
C23 N3 C24 120.75(16) . . ?
C23 N3 Fe1 125.37(12) . . ?
C24 N3 Fe1 113.85(14) . . ?
C31 N4 C32 119.04(18) . . ?
C31 N4 Fe1 127.93(15) . . ?
C32 N4 Fe1 112.97(14) . . ?
C39 N5 C40 119.90(18) . . ?
C39 N5 Fe2 124.59(15) . . ?
C40 N5 Fe2 115.42(13) . . ?
C47 N6 C48 119.12(19) . . ?
C47 N6 Fe2 125.69(16) . . ?
C48 N6 Fe2 115.11(14) . . ?
C55 N7 C56 120.19(18) . . ?
C55 N7 Fe2 124.56(15) . . ?
C56 N7 Fe2 115.07(13) . . ?
C63 N8 C64 118.5(2) . . ?
C63 N8 Fe2 126.49(16) . . ?
C64 N8 Fe2 114.96(14) . . ?
O1 C1 C2 117.6(2) . . ?
O1 C1 C6 124.95(19) . . ?
C2 C1 C6 117.4(2) . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 119.3(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 F1 119.3(3) . . ?
C5 C4 C3 122.6(2) . . ?
F1 C4 C3 118.1(2) . . ?
C4 C5 C6 119.1(2) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C7 116.41(19) . . ?
C5 C6 C1 119.9(2) . . ?
C7 C6 C1 123.61(19) . . ?
N1 C7 C6 124.84(18) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C8 C9 C10 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 121.9(2) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C16 C12 C11 118.0(2) . . ?
C16 C12 C13 117.4(2) . . ?
C11 C12 C13 124.6(2) . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.2(2) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
N2 C15 C14 122.0(2) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N2 C16 C12 121.9(2) . . ?
N2 C16 C8 117.40(17) . . ?
C12 C16 C8 120.72(19) . . ?
O2 C17 C18 117.5(2) . . ?
O2 C17 C22 124.8(2) . . ?
C18 C17 C22 117.7(2) . . ?
C19 C18 C17 121.5(2) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 119.5(2) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
F2 C20 C21 119.4(3) . . ?
F2 C20 C19 118.5(2) . . ?
C21 C20 C19 122.1(2) . . ?
C20 C21 C22 119.3(2) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C17 119.9(2) . . ?
C21 C22 C23 117.05(18) . . ?
C17 C22 C23 122.98(18) . . ?
N3 C23 C22 124.04(13) . . ?
N3 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?
C9 C8 C16 119.19(16) . . ?
C9 C8 N1 128.10(14) . . ?
C16 C8 N1 112.64(12) . . ?
N9 C65 S1 162.6(4) . . ?
C25 C24 N3 127.7(2) . . ?
C25 C24 C32 119.1(2) . . ?
N3 C24 C32 113.27(18) . . ?
C24 C25 C26 119.4(3) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C27 C26 C25 122.1(3) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C26 C27 C28 120.3(3) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C32 117.6(2) . . ?
C27 C28 C29 124.9(2) . . ?
C32 C28 C29 117.5(2) . . ?
C30 C29 C28 119.6(2) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 119.7(2) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
N4 C31 C30 122.2(2) . . ?
N4 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
N4 C32 C28 121.7(2) . . ?
N4 C32 C24 116.81(18) . . ?
C28 C32 C24 121.5(2) . . ?
O3 C33 C34 119.0(2) . . ?
O3 C33 C38 122.9(2) . . ?
C34 C33 C38 118.1(2) . . ?
C35 C34 C33 121.4(2) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C36 C35 C34 119.1(3) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C37 C36 F3 119.0(3) . . ?
C37 C36 C35 122.7(3) . . ?
F3 C36 C35 118.3(3) . . ?
C36 C37 C38 119.1(3) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C33 C38 C37 119.6(2) . . ?
C33 C38 C39 123.5(2) . . ?
C37 C38 C39 117.0(2) . . ?
N5 C39 C38 126.5(2) . . ?
N5 C39 H39 116.8 . . ?
C38 C39 H39 116.8 . . ?
C41 C40 C48 118.9(2) . . ?
C41 C40 N5 126.7(2) . . ?
C48 C40 N5 114.43(18) . . ?
C40 C41 C42 120.3(2) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 121.4(3) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C44 120.5(3) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C45 C44 C43 124.3(2) . . ?
C45 C44 C48 117.5(2) . . ?
C43 C44 C48 118.1(2) . . ?
C46 C45 C44 119.7(2) . . ?
C46 C45 H45 120.1 . . ?
C44 C45 H45 120.1 . . ?
C45 C46 C47 119.5(2) . . ?
C45 C46 H46 120.3 . . ?
C47 C46 H46 120.3 . . ?
N6 C47 C46 122.7(2) . . ?
N6 C47 H47 118.6 . . ?
C46 C47 H47 118.6 . . ?
N6 C48 C44 121.4(2) . . ?
N6 C48 C40 117.77(19) . . ?
C44 C48 C40 120.8(2) . . ?
O4 C49 C50 118.8(2) . . ?
O4 C49 C54 122.9(2) . . ?
C50 C49 C54 118.3(2) . . ?
C51 C50 C49 121.4(3) . . ?
C51 C50 H50 119.3 . . ?
C49 C50 H50 119.3 . . ?
C50 C51 C52 119.5(3) . . ?
C50 C51 H51 120.2 . . ?
C52 C51 H51 120.2 . . ?
C53 C52 F4 119.4(3) . . ?
C53 C52 C51 122.1(3) . . ?
F4 C52 C51 118.5(3) . . ?
C52 C53 C54 119.5(3) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C49 C54 C53 119.2(2) . . ?
C49 C54 C55 123.7(2) . . ?
C53 C54 C55 117.0(2) . . ?
N7 C55 C54 126.2(2) . . ?
N7 C55 H55 116.9 . . ?
C54 C55 H55 116.9 . . ?
C57 C56 N7 126.6(2) . . ?
C57 C56 C64 118.8(2) . . ?
N7 C56 C64 114.67(18) . . ?
C56 C57 C58 120.1(3) . . ?
C56 C57 H57 120.0 . . ?
C58 C57 H57 120.0 . . ?
C59 C58 C57 121.5(3) . . ?
C59 C58 H58 119.3 . . ?
C57 C58 H58 119.3 . . ?
C58 C59 C60 120.4(3) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C61 C60 C64 117.9(2) . . ?
C61 C60 C59 124.1(2) . . ?
C64 C60 C59 118.0(3) . . ?
C62 C61 C60 119.8(2) . . ?
C62 C61 H61 120.1 . . ?
C60 C61 H61 120.1 . . ?
C61 C62 C63 119.4(3) . . ?
C61 C62 H62 120.3 . . ?
C63 C62 H62 120.3 . . ?
N8 C63 C62 123.0(2) . . ?
N8 C63 H63 118.5 . . ?
C62 C63 H63 118.5 . . ?
N8 C64 C60 121.4(2) . . ?
N8 C64 C56 117.38(19) . . ?
C60 C64 C56 121.2(2) . . ?
N10 C66 S2 171.2(6) . . ?
N10' C66' S2' 174.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.836
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 994838'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp48_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H20 Cl2 Fe N4 O2, C N S, C H4 O '

_chemical_formula_sum            'C34 H24 Cl2 Fe N5 O3 S'
_chemical_formula_weight         709.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.0244(12)
_cell_length_b                   12.1032(14)
_cell_length_c                   13.0961(16)
_cell_angle_alpha                105.652(7)
_cell_angle_beta                 97.910(8)
_cell_angle_gamma                98.813(7)
_cell_volume                     1485.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2326
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      20.12

_exptl_crystal_description       Plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             726
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8427
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_process_details   sadabs

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23398
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.1760
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6678
_reflns_number_gt                3319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.

The asymmetric unit contains  the iron monomer, one thiocyanate anion and 
one methanol solvent molecule. All the non-hydrogen atoms are refined 
anisotropically and all hydrogen  atoms are placed in calculated positions.  
;

_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)+(0.0858P)²+1.8671P] 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         6678
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1829
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2156
_refine_ls_wR_factor_gt          0.1755
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.52462(9) 0.29045(7) 0.13610(7) 0.0209(3) Uani 1 1 d . . .
Cl1 Cl 0.95362(17) 0.53645(14) -0.17901(14) 0.0364(5) Uani 1 1 d . . .
Cl2 Cl -0.05425(16) -0.15446(14) -0.18792(14) 0.0334(4) Uani 1 1 d . . .
S1 S 0.17454(19) 0.28514(16) 0.63944(16) 0.0392(5) Uani 1 1 d . . .
O1 O 0.6295(4) 0.2455(3) 0.0295(3) 0.0237(10) Uani 1 1 d . . .
O2 O 0.3642(4) 0.2699(3) 0.0353(3) 0.0226(10) Uani 1 1 d . . .
N1 N 0.4289(5) 0.3467(4) 0.2571(4) 0.0245(12) Uani 1 1 d . . .
N2 N 0.5582(5) 0.4568(4) 0.1439(4) 0.0199(11) Uani 1 1 d . . .
N3 N 0.6871(5) 0.3061(4) 0.2463(4) 0.0188(11) Uani 1 1 d . . .
N4 N 0.4933(5) 0.1293(4) 0.1395(4) 0.0213(12) Uani 1 1 d . . .
N5 N -0.0828(7) 0.1501(7) 0.6373(5) 0.071(2) Uani 1 1 d . . .
C1 C 0.3679(6) 0.2862(6) 0.3133(5) 0.0294(16) Uani 1 1 d . . .
H1 H 0.3671 0.2046 0.2954 0.035 Uiso 1 1 calc R . .
C2 C 0.3046(7) 0.3356(7) 0.3974(6) 0.0369(18) Uani 1 1 d . . .
H2 H 0.2618 0.2887 0.4361 0.044 Uiso 1 1 calc R . .
C3 C 0.3048(7) 0.4531(6) 0.4238(6) 0.0368(18) Uani 1 1 d . . .
H3 H 0.2630 0.4886 0.4818 0.044 Uiso 1 1 calc R . .
C4 C 0.3669(6) 0.5213(6) 0.3652(6) 0.0334(17) Uani 1 1 d . . .
C5 C 0.3721(7) 0.6433(6) 0.3847(6) 0.0413(19) Uani 1 1 d . . .
H5 H 0.3311 0.6837 0.4410 0.050 Uiso 1 1 calc R . .
C6 C 0.4347(7) 0.7036(6) 0.3245(6) 0.0384(19) Uani 1 1 d . . .
H6 H 0.4341 0.7846 0.3373 0.046 Uiso 1 1 calc R . .
C7 C 0.5010(6) 0.6456(5) 0.2423(5) 0.0286(16) Uani 1 1 d . . .
H7 H 0.5474 0.6888 0.2025 0.034 Uiso 1 1 calc R . .
C8 C 0.4987(6) 0.5270(5) 0.2201(5) 0.0234(14) Uani 1 1 d . . .
C9 C 0.4303(6) 0.4652(5) 0.2816(5) 0.0252(15) Uani 1 1 d . . .
C10 C 0.6308(6) 0.5008(5) 0.0834(5) 0.0223(14) Uani 1 1 d . . .
H10 H 0.6369 0.5818 0.0912 0.027 Uiso 1 1 calc R . .
C11 C 0.7016(6) 0.4386(5) 0.0069(5) 0.0220(14) Uani 1 1 d . . .
C12 C 0.7819(6) 0.5034(5) -0.0460(5) 0.0228(14) Uani 1 1 d . . .
H12 H 0.7837 0.5849 -0.0317 0.027 Uiso 1 1 calc R . .
C13 C 0.8559(7) 0.4514(6) -0.1165(5) 0.0291(16) Uani 1 1 d . . .
C14 C 0.8602(8) 0.3339(5) -0.1386(5) 0.0316(17) Uani 1 1 d . . .
H14 H 0.9174 0.2997 -0.1850 0.038 Uiso 1 1 calc R . .
C15 C 0.7787(7) 0.2677(5) -0.0912(5) 0.0262(15) Uani 1 1 d . . .
H15 H 0.7749 0.1856 -0.1106 0.031 Uiso 1 1 calc R . .
C16 C 0.7010(6) 0.3163(5) -0.0152(5) 0.0190(13) Uani 1 1 d . . .
C17 C 0.7865(6) 0.3996(5) 0.2952(5) 0.0253(15) Uani 1 1 d . . .
H17 H 0.7831 0.4706 0.2778 0.030 Uiso 1 1 calc R . .
C18 C 0.8942(6) 0.3953(5) 0.3708(5) 0.0216(14) Uani 1 1 d . . .
H18 H 0.9627 0.4641 0.4042 0.026 Uiso 1 1 calc R . .
C19 C 0.9070(7) 0.2972(6) 0.3997(5) 0.0315(16) Uani 1 1 d . . .
H19 H 0.9818 0.2977 0.4530 0.038 Uiso 1 1 calc R . .
C20 C 0.8055(7) 0.1938(6) 0.3481(5) 0.0285(16) Uani 1 1 d . . .
C21 C 0.8065(7) 0.0858(6) 0.3670(5) 0.0332(17) Uani 1 1 d . . .
H21 H 0.8780 0.0779 0.4187 0.040 Uiso 1 1 calc R . .
C22 C 0.7043(6) -0.0093(6) 0.3109(5) 0.0311(16) Uani 1 1 d . . .
H22 H 0.7062 -0.0827 0.3238 0.037 Uiso 1 1 calc R . .
C23 C 0.5976(7) 0.0004(6) 0.2352(5) 0.0311(16) Uani 1 1 d . . .
H23 H 0.5284 -0.0667 0.1972 0.037 Uiso 1 1 calc R . .
C24 C 0.5907(7) 0.1049(5) 0.2144(5) 0.0243(15) Uani 1 1 d . . .
C25 C 0.6979(6) 0.2034(5) 0.2725(5) 0.0228(14) Uani 1 1 d . . .
C26 C 0.3942(6) 0.0458(5) 0.0768(5) 0.0226(14) Uani 1 1 d . . .
H26 H 0.3940 -0.0312 0.0812 0.027 Uiso 1 1 calc R . .
C27 C 0.2868(6) 0.0612(5) 0.0023(5) 0.0221(14) Uani 1 1 d . . .
C28 C 0.1825(6) -0.0378(5) -0.0530(5) 0.0248(15) Uani 1 1 d . . .
H28 H 0.1890 -0.1111 -0.0414 0.030 Uiso 1 1 calc R . .
C29 C 0.0739(7) -0.0302(5) -0.1221(5) 0.0278(16) Uani 1 1 d . . .
C30 C 0.0581(8) 0.0750(5) -0.1423(5) 0.0341(17) Uani 1 1 d . . .
H30 H -0.0198 0.0794 -0.1901 0.041 Uiso 1 1 calc R . .
C31 C 0.1622(7) 0.1743(5) -0.0890(5) 0.0299(16) Uani 1 1 d . . .
H31 H 0.1557 0.2462 -0.1037 0.036 Uiso 1 1 calc R . .
C32 C 0.2741(6) 0.1701(5) -0.0156(5) 0.0237(15) Uani 1 1 d . . .
C33 C 0.0246(9) 0.2074(7) 0.6379(6) 0.051(2) Uani 1 1 d . . .
C1S C 0.6343(11) 0.9506(8) 0.5775(8) 0.082(3) Uani 1 1 d . . .
H1S1 H 0.6197 1.0010 0.5314 0.122 Uiso 1 1 calc R . .
H1S2 H 0.5462 0.9023 0.5770 0.122 Uiso 1 1 calc R . .
H1S3 H 0.6969 0.8998 0.5502 0.122 Uiso 1 1 calc R . .
O1S O 0.6876(7) 1.0150(7) 0.6755(5) 0.084(2) Uani 1 1 d . . .
H1S H 0.7692 1.0466 0.6781 0.126 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 O2 1.872(4) . ?
Fe1 O1 1.876(4) . ?
Fe1 N4 1.941(5) . ?
Fe1 N2 1.962(5) . ?
Fe1 N3 1.970(5) . ?
Fe1 N1 1.982(5) . ?
Cl1 C13 1.748(6) . ?
Cl2 C29 1.749(6) . ?
S1 C33 1.640(9) . ?
O1 C16 1.337(7) . ?
O2 C32 1.336(7) . ?
N1 C1 1.315(8) . ?
N1 C9 1.380(8) . ?
N2 C10 1.308(7) . ?
N2 C8 1.391(8) . ?
N3 C17 1.331(7) . ?
N3 C25 1.392(7) . ?
N4 C26 1.305(7) . ?
N4 C24 1.408(8) . ?
N5 C33 1.186(10) . ?
C1 C2 1.389(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.369(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(9) . ?
C3 H3 0.9500 . ?
C4 C9 1.410(9) . ?
C4 C5 1.420(10) . ?
C5 C6 1.362(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.423(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.381(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.413(9) . ?
C10 C11 1.423(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.413(8) . ?
C11 C16 1.429(8) . ?
C12 C13 1.348(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(8) . ?
C14 C15 1.379(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.407(8) . ?
C15 H15 0.9500 . ?
C17 C18 1.379(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.357(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.422(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.397(9) . ?
C20 C25 1.401(9) . ?
C21 C22 1.375(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.431(8) . ?
C26 C27 1.419(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.411(8) . ?
C27 C32 1.422(8) . ?
C28 C29 1.348(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.395(9) . ?
C30 C31 1.408(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.390(9) . ?
C31 H31 0.9500 . ?
C1S O1S 1.297(10) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O1S H1S 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 93.46(18) . . ?
O2 Fe1 N4 94.75(19) . . ?
O1 Fe1 N4 87.47(19) . . ?
O2 Fe1 N2 87.82(18) . . ?
O1 Fe1 N2 95.57(18) . . ?
N4 Fe1 N2 175.9(2) . . ?
O2 Fe1 N3 176.60(18) . . ?
O1 Fe1 N3 88.65(19) . . ?
N4 Fe1 N3 82.7(2) . . ?
N2 Fe1 N3 94.63(19) . . ?
O2 Fe1 N1 90.97(19) . . ?
O1 Fe1 N1 174.94(19) . . ?
N4 Fe1 N1 94.6(2) . . ?
N2 Fe1 N1 82.1(2) . . ?
N3 Fe1 N1 87.0(2) . . ?
C16 O1 Fe1 126.3(4) . . ?
C32 O2 Fe1 127.3(4) . . ?
C1 N1 C9 119.1(6) . . ?
C1 N1 Fe1 128.4(5) . . ?
C9 N1 Fe1 112.5(4) . . ?
C10 N2 C8 121.3(5) . . ?
C10 N2 Fe1 123.8(4) . . ?
C8 N2 Fe1 114.9(4) . . ?
C17 N3 C25 117.5(5) . . ?
C17 N3 Fe1 128.6(4) . . ?
C25 N3 Fe1 113.9(4) . . ?
C26 N4 C24 120.3(5) . . ?
C26 N4 Fe1 124.9(4) . . ?
C24 N4 Fe1 114.8(4) . . ?
N1 C1 C2 123.3(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.9(7) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C9 117.9(6) . . ?
C3 C4 C5 124.9(6) . . ?
C9 C4 C5 117.3(6) . . ?
C6 C5 C4 121.4(7) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 120.2(6) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 N2 128.4(6) . . ?
C7 C8 C9 118.4(6) . . ?
N2 C8 C9 113.2(5) . . ?
N1 C9 C4 120.8(6) . . ?
N1 C9 C8 117.2(6) . . ?
C4 C9 C8 122.0(6) . . ?
N2 C10 C11 126.1(5) . . ?
N2 C10 H10 117.0 . . ?
C11 C10 H10 117.0 . . ?
C12 C11 C10 117.6(5) . . ?
C12 C11 C16 118.6(6) . . ?
C10 C11 C16 123.7(5) . . ?
C13 C12 C11 121.1(6) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 122.1(6) . . ?
C12 C13 Cl1 118.9(5) . . ?
C14 C13 Cl1 118.9(5) . . ?
C15 C14 C13 117.9(6) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
C14 C15 C16 122.9(6) . . ?
C14 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
O1 C16 C15 118.5(5) . . ?
O1 C16 C11 124.3(5) . . ?
C15 C16 C11 117.2(5) . . ?
N3 C17 C18 121.1(6) . . ?
N3 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 123.1(6) . . ?
C19 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
C18 C19 C20 118.3(6) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
C21 C20 C25 118.8(6) . . ?
C21 C20 C19 125.0(6) . . ?
C25 C20 C19 116.2(6) . . ?
C22 C21 C20 120.1(6) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.9(6) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 121.4(6) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 N4 128.7(6) . . ?
C23 C24 C25 117.4(6) . . ?
N4 C24 C25 113.8(5) . . ?
N3 C25 C20 123.8(5) . . ?
N3 C25 C24 114.8(6) . . ?
C20 C25 C24 121.3(6) . . ?
N4 C26 C27 125.1(6) . . ?
N4 C26 H26 117.4 . . ?
C27 C26 H26 117.4 . . ?
C28 C27 C26 117.2(6) . . ?
C28 C27 C32 118.3(6) . . ?
C26 C27 C32 124.3(5) . . ?
C29 C28 C27 121.2(6) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 122.2(6) . . ?
C28 C29 Cl2 119.8(5) . . ?
C30 C29 Cl2 118.0(5) . . ?
C29 C30 C31 117.5(6) . . ?
C29 C30 H30 121.3 . . ?
C31 C30 H30 121.3 . . ?
C32 C31 C30 121.9(6) . . ?
C32 C31 H31 119.1 . . ?
C30 C31 H31 119.1 . . ?
O2 C32 C31 117.8(5) . . ?
O2 C32 C27 123.3(6) . . ?
C31 C32 C27 118.9(5) . . ?
N5 C33 S1 179.0(9) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S O1S H1S 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.591
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.125
_database_code_depnum_ccdc_archive 'CCDC 994839'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp42lt

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H20 Br2 Fe N4 O2, C N S, C H4 O'
_chemical_formula_sum            'C34 H24 Br2 Fe N5 O3 S'
_chemical_formula_weight         798.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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

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

_cell_length_a                   10.1777(6)
_cell_length_b                   12.7832(8)
_cell_length_c                   25.5491(18)
_cell_angle_alpha                76.095(2)
_cell_angle_beta                 79.175(3)
_cell_angle_gamma                77.517(2)
_cell_volume                     3117.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3543
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      25.51

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    3.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20532
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         0.83
_diffrn_reflns_theta_max         27.55
_reflns_number_total             13875
_reflns_number_gt                7987
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.

The asymmetric unit contains two iron monomers, two thiocyanate anions and 
two methanol solvent molecules. All the non-hydrogen atoms are refined 
anisotropically and all hydrogen  atoms are placed in calculated positions.    
;

_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)+(0.0672P)²+4.3097P] 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         13875
_refine_ls_number_parameters     833
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1639
_refine_ls_wR_factor_gt          0.1381
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
Br1 Br 0.89279(7) 0.64081(6) 0.41802(3) 0.03246(18) Uani 1 1 d . . .
Br2 Br 0.67192(7) 1.07989(6) 0.79860(3) 0.03429(19) Uani 1 1 d . . .
Br3 Br 0.13708(8) 0.14972(6) 0.31903(3) 0.0430(2) Uani 1 1 d . . .
Br4 Br 1.03886(7) 0.37006(6) -0.09084(3) 0.0376(2) Uani 1 1 d . . .
Fe1 Fe 0.36000(8) 0.85575(7) 0.62293(3) 0.0175(2) Uani 1 1 d . . .
Fe2 Fe 0.49780(9) 0.56595(8) 0.12207(4) 0.0236(2) Uani 1 1 d . . .
S1 S 0.13804(19) 0.93901(15) 0.81764(7) 0.0348(4) Uani 1 1 d . . .
S2 S 0.1382(3) 0.6176(2) 0.30104(10) 0.0700(8) Uani 1 1 d . . .
O1 O 0.5139(4) 0.7467(3) 0.61754(15) 0.0215(9) Uani 1 1 d . . .
O2 O 0.4569(4) 0.9672(3) 0.62040(15) 0.0205(9) Uani 1 1 d . . .
O3 O 0.6715(4) 0.4765(3) 0.11015(17) 0.0276(10) Uani 1 1 d . . .
O4 O 0.3977(4) 0.4514(4) 0.12957(18) 0.0303(11) Uani 1 1 d . . .
O5 O 0.3288(7) 0.7089(6) 0.4641(3) 0.079(2) Uani 1 1 d . . .
H5A H 0.2963 0.7006 0.4378 0.095 Uiso 1 1 calc R . .
O6 O -0.3233(6) 0.8213(5) 0.9548(2) 0.0597(16) Uani 1 1 d . . .
H6 H -0.2480 0.8230 0.9346 0.072 Uiso 1 1 calc R . .
N1 N 0.3629(5) 0.9066(4) 0.54472(18) 0.0186(11) Uani 1 1 d . . .
N2 N 0.1919(5) 0.9660(4) 0.62639(18) 0.0194(11) Uani 1 1 d . . .
N3 N 0.3456(5) 0.8042(4) 0.70125(18) 0.0161(10) Uani 1 1 d . . .
N4 N 0.2462(5) 0.7458(4) 0.62819(19) 0.0202(11) Uani 1 1 d . . .
N5 N 0.4874(5) 0.5328(5) 0.2061(2) 0.0307(13) Uani 1 1 d . . .
N6 N 0.5886(5) 0.6908(5) 0.1328(3) 0.0386(16) Uani 1 1 d . . .
N7 N 0.5022(5) 0.6210(4) 0.03898(19) 0.0204(11) Uani 1 1 d . . .
N8 N 0.3208(5) 0.6877(4) 0.1179(2) 0.0247(12) Uani 1 1 d . . .
N9 N -0.0839(6) 0.8595(5) 0.8851(3) 0.0480(17) Uani 1 1 d . . .
N10 N 0.2927(8) 0.6462(6) 0.3736(3) 0.068(2) Uani 1 1 d . . .
C1 C 0.5937(6) 0.7290(5) 0.5725(2) 0.0221(14) Uani 1 1 d . . .
C2 C 0.7027(6) 0.6393(5) 0.5767(3) 0.0267(15) Uani 1 1 d . . .
H2 H 0.7162 0.5957 0.6117 0.032 Uiso 1 1 calc R . .
C3 C 0.7896(6) 0.6133(5) 0.5320(3) 0.0278(15) Uani 1 1 d . . .
H3 H 0.8618 0.5523 0.5362 0.033 Uiso 1 1 calc R . .
C4 C 0.7720(6) 0.6765(5) 0.4805(2) 0.0234(14) Uani 1 1 d . . .
C5 C 0.6678(6) 0.7631(5) 0.4735(2) 0.0249(14) Uani 1 1 d . . .
H5 H 0.6569 0.8049 0.4379 0.030 Uiso 1 1 calc R . .
C6 C 0.5748(6) 0.7913(5) 0.5193(2) 0.0195(13) Uani 1 1 d . . .
C7 C 0.4620(6) 0.8762(5) 0.5084(2) 0.0211(14) Uani 1 1 d . . .
H7 H 0.4589 0.9139 0.4717 0.025 Uiso 1 1 calc R . .
C8 C 0.2483(6) 0.9874(5) 0.5305(2) 0.0203(13) Uani 1 1 d . . .
C9 C 0.2176(7) 1.0353(5) 0.4786(2) 0.0251(14) Uani 1 1 d . . .
H9 H 0.2747 1.0140 0.4476 0.030 Uiso 1 1 calc R . .
C10 C 0.1004(7) 1.1161(5) 0.4727(3) 0.0296(16) Uani 1 1 d . . .
H10 H 0.0808 1.1504 0.4370 0.036 Uiso 1 1 calc R . .
C11 C 0.0135(7) 1.1474(5) 0.5160(2) 0.0266(15) Uani 1 1 d . . .
H11 H -0.0639 1.2031 0.5099 0.032 Uiso 1 1 calc R . .
C12 C 0.0376(7) 1.0972(5) 0.5704(2) 0.0239(14) Uani 1 1 d . . .
C13 C -0.0400(6) 1.1261(5) 0.6166(3) 0.0264(15) Uani 1 1 d . . .
H13 H -0.1200 1.1803 0.6137 0.032 Uiso 1 1 calc R . .
C14 C -0.0030(6) 1.0774(5) 0.6667(3) 0.0280(15) Uani 1 1 d . . .
H14 H -0.0557 1.0981 0.6987 0.034 Uiso 1 1 calc R . .
C15 C 0.1149(6) 0.9959(5) 0.6701(2) 0.0239(14) Uani 1 1 d . . .
H15 H 0.1401 0.9613 0.7050 0.029 Uiso 1 1 calc R . .
C16 C 0.1575(6) 1.0182(5) 0.5758(2) 0.0192(13) Uani 1 1 d . . .
C17 C 0.4942(6) 0.9904(5) 0.6610(2) 0.0184(13) Uani 1 1 d . . .
C18 C 0.5581(6) 1.0814(5) 0.6516(2) 0.0246(14) Uani 1 1 d . . .
H18 H 0.5672 1.1254 0.6158 0.030 Uiso 1 1 calc R . .
C19 C 0.6082(6) 1.1102(5) 0.6915(3) 0.0238(14) Uani 1 1 d . . .
H19 H 0.6517 1.1720 0.6835 0.029 Uiso 1 1 calc R . .
C20 C 0.5930(6) 1.0454(5) 0.7444(3) 0.0252(14) Uani 1 1 d . . .
C21 C 0.5260(6) 0.9584(5) 0.7572(2) 0.0213(13) Uani 1 1 d . . .
H21 H 0.5142 0.9178 0.7936 0.026 Uiso 1 1 calc R . .
C22 C 0.4747(6) 0.9296(5) 0.7161(2) 0.0183(13) Uani 1 1 d . . .
C23 C 0.4035(6) 0.8396(5) 0.7323(2) 0.0212(14) Uani 1 1 d . . .
H23 H 0.3984 0.8027 0.7695 0.025 Uiso 1 1 calc R . .
C24 C 0.2646(6) 0.7206(5) 0.7214(2) 0.0182(13) Uani 1 1 d . . .
C25 C 0.2339(6) 0.6704(5) 0.7749(2) 0.0225(14) Uani 1 1 d . . .
H25 H 0.2687 0.6891 0.8028 0.027 Uiso 1 1 calc R . .
C26 C 0.1498(6) 0.5906(5) 0.7880(2) 0.0258(15) Uani 1 1 d . . .
H26 H 0.1297 0.5557 0.8251 0.031 Uiso 1 1 calc R . .
C27 C 0.0960(6) 0.5612(5) 0.7495(3) 0.0263(15) Uani 1 1 d . . .
H27 H 0.0386 0.5080 0.7596 0.032 Uiso 1 1 calc R . .
C28 C 0.1282(6) 0.6123(5) 0.6940(3) 0.0227(14) Uani 1 1 d . . .
C29 C 0.0818(7) 0.5881(5) 0.6505(3) 0.0297(15) Uani 1 1 d . . .
H29 H 0.0236 0.5359 0.6574 0.036 Uiso 1 1 calc R . .
C30 C 0.1206(7) 0.6397(5) 0.5984(3) 0.0327(16) Uani 1 1 d . . .
H30 H 0.0925 0.6216 0.5688 0.039 Uiso 1 1 calc R . .
C31 C 0.2022(7) 0.7197(5) 0.5888(3) 0.0294(15) Uani 1 1 d . . .
H31 H 0.2265 0.7565 0.5524 0.035 Uiso 1 1 calc R . .
C32 C 0.2124(6) 0.6922(5) 0.6809(2) 0.0189(13) Uani 1 1 d . . .
C33 C 0.3432(7) 0.3889(5) 0.1720(3) 0.0287(15) Uani 1 1 d . . .
C34 C 0.2684(7) 0.3106(5) 0.1643(3) 0.0306(16) Uani 1 1 d . . .
H34 H 0.2616 0.3058 0.1284 0.037 Uiso 1 1 calc R . .
C35 C 0.2077(7) 0.2436(6) 0.2077(3) 0.0338(17) Uani 1 1 d . . .
H35 H 0.1586 0.1933 0.2016 0.041 Uiso 1 1 calc R . .
C36 C 0.2168(7) 0.2484(5) 0.2601(3) 0.0298(16) Uani 1 1 d . . .
C37 C 0.2874(7) 0.3179(6) 0.2697(3) 0.0354(17) Uani 1 1 d . . .
H37 H 0.2943 0.3186 0.3062 0.042 Uiso 1 1 calc R . .
C38 C 0.3514(7) 0.3897(5) 0.2263(3) 0.0284(15) Uani 1 1 d . . .
C39 C 0.4236(7) 0.4621(6) 0.2399(3) 0.0328(17) Uani 1 1 d . . .
H39 H 0.4243 0.4573 0.2775 0.039 Uiso 1 1 calc R . .
C40 C 0.5576(7) 0.5992(6) 0.2257(3) 0.040(2) Uani 1 1 d . . .
C41 C 0.5756(8) 0.5866(8) 0.2788(4) 0.060(3) Uani 1 1 d . . .
H41 H 0.5412 0.5307 0.3064 0.073 Uiso 1 1 calc R . .
C42 C 0.6473(9) 0.6596(11) 0.2918(5) 0.083(4) Uani 1 1 d . . .
H42 H 0.6595 0.6518 0.3286 0.100 Uiso 1 1 calc R . .
C43 C 0.6975(9) 0.7381(10) 0.2540(6) 0.086(4) Uani 1 1 d . . .
H43 H 0.7476 0.7830 0.2640 0.103 Uiso 1 1 calc R . .
C44 C 0.6767(8) 0.7557(8) 0.1982(5) 0.065(3) Uani 1 1 d . . .
C45 C 0.7179(9) 0.8379(9) 0.1572(6) 0.081(4) Uani 1 1 d . . .
H45 H 0.7633 0.8887 0.1651 0.097 Uiso 1 1 calc R . .
C46 C 0.6950(8) 0.8476(7) 0.1063(6) 0.075(4) Uani 1 1 d . . .
H46 H 0.7215 0.9063 0.0784 0.090 Uiso 1 1 calc R . .
C47 C 0.6310(7) 0.7701(6) 0.0940(4) 0.053(2) Uani 1 1 d . . .
H47 H 0.6186 0.7752 0.0575 0.063 Uiso 1 1 calc R . .
C48 C 0.6077(7) 0.6826(6) 0.1847(4) 0.044(2) Uani 1 1 d . . .
C49 C 0.7484(6) 0.4548(5) 0.0653(2) 0.0217(14) Uani 1 1 d . . .
C50 C 0.8703(7) 0.3795(5) 0.0690(3) 0.0297(16) Uani 1 1 d . . .
H50 H 0.8943 0.3446 0.1040 0.036 Uiso 1 1 calc R . .
C51 C 0.9568(6) 0.3544(5) 0.0234(3) 0.0287(15) Uani 1 1 d . . .
H51 H 1.0388 0.3028 0.0271 0.034 Uiso 1 1 calc R . .
C52 C 0.9223(6) 0.4057(5) -0.0283(3) 0.0255(14) Uani 1 1 d . . .
C53 C 0.8061(6) 0.4792(5) -0.0334(2) 0.0247(14) Uani 1 1 d . . .
H53 H 0.7836 0.5130 -0.0687 0.030 Uiso 1 1 calc R . .
C54 C 0.7168(6) 0.5069(5) 0.0127(2) 0.0209(14) Uani 1 1 d . . .
C55 C 0.5972(6) 0.5855(5) 0.0026(2) 0.0243(14) Uani 1 1 d . . .
H55 H 0.5859 0.6150 -0.0345 0.029 Uiso 1 1 calc R . .
C56 C 0.3919(6) 0.7049(5) 0.0226(3) 0.0240(14) Uani 1 1 d . . .
C57 C 0.3673(7) 0.7530(5) -0.0303(3) 0.0298(16) Uani 1 1 d . . .
H57 H 0.4274 0.7288 -0.0600 0.036 Uiso 1 1 calc R . .
C58 C 0.2563(7) 0.8358(6) -0.0405(3) 0.0407(19) Uani 1 1 d . . .
H58 H 0.2406 0.8663 -0.0770 0.049 Uiso 1 1 calc R . .
C59 C 0.1697(8) 0.8740(6) 0.0008(3) 0.0389(18) Uani 1 1 d . . .
H59 H 0.0969 0.9331 -0.0073 0.047 Uiso 1 1 calc R . .
C60 C 0.1867(7) 0.8267(5) 0.0558(3) 0.0319(16) Uani 1 1 d . . .
C61 C 0.1029(7) 0.8588(6) 0.1005(3) 0.0365(18) Uani 1 1 d . . .
H61 H 0.0303 0.9193 0.0953 0.044 Uiso 1 1 calc R . .
C62 C 0.1232(7) 0.8045(6) 0.1522(3) 0.0338(17) Uani 1 1 d . . .
H62 H 0.0632 0.8246 0.1829 0.041 Uiso 1 1 calc R . .
C63 C 0.2365(6) 0.7171(6) 0.1591(3) 0.0314(16) Uani 1 1 d . . .
H63 H 0.2509 0.6790 0.1950 0.038 Uiso 1 1 calc R . .
C64 C 0.2989(6) 0.7400(5) 0.0661(3) 0.0217(14) Uani 1 1 d . . .
C65 C 0.4047(13) 0.6139(11) 0.4856(5) 0.110(4) Uani 1 1 d . . .
H65A H 0.4880 0.5985 0.4602 0.164 Uiso 1 1 calc R . .
H65B H 0.3530 0.5545 0.4921 0.164 Uiso 1 1 calc R . .
H65C H 0.4285 0.6195 0.5201 0.164 Uiso 1 1 calc R . .
C66 C -0.4009(10) 0.9221(8) 0.9471(5) 0.089(4) Uani 1 1 d . . .
H66A H -0.4669 0.9295 0.9798 0.133 Uiso 1 1 calc R . .
H66B H -0.4493 0.9324 0.9159 0.133 Uiso 1 1 calc R . .
H66C H -0.3429 0.9774 0.9398 0.133 Uiso 1 1 calc R . .
C67 C 0.0088(7) 0.8928(5) 0.8564(3) 0.0302(16) Uani 1 1 d . . .
C68 C 0.2273(8) 0.6328(6) 0.3418(3) 0.041(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.906(6) . ?
Br2 C20 1.902(6) . ?
Br3 C36 1.894(7) . ?
Br4 C52 1.891(6) . ?
Fe1 O1 1.866(4) . ?
Fe1 O2 1.882(4) . ?
Fe1 N3 1.939(4) . ?
Fe1 N1 1.944(5) . ?
Fe1 N2 1.970(5) . ?
Fe1 N4 1.973(5) . ?
Fe2 O3 1.902(4) . ?
Fe2 O4 1.912(4) . ?
Fe2 N7 2.065(5) . ?
Fe2 N5 2.072(6) . ?
Fe2 N6 2.102(6) . ?
Fe2 N8 2.112(5) . ?
S1 C67 1.620(8) . ?
S2 C68 1.573(10) . ?
O1 C1 1.316(7) . ?
O2 C17 1.286(7) . ?
O3 C49 1.313(7) . ?
O4 C33 1.292(8) . ?
O5 C65 1.345(13) . ?
O5 H5A 0.8400 . ?
O6 C66 1.348(10) . ?
O6 H6 0.8400 . ?
N1 C7 1.296(7) . ?
N1 C8 1.421(7) . ?
N2 C15 1.324(7) . ?
N2 C16 1.377(7) . ?
N3 C23 1.284(7) . ?
N3 C24 1.429(7) . ?
N4 C31 1.311(8) . ?
N4 C32 1.374(7) . ?
N5 C39 1.285(9) . ?
N5 C40 1.443(8) . ?
N6 C47 1.320(10) . ?
N6 C48 1.352(10) . ?
N7 C55 1.297(7) . ?
N7 C56 1.423(7) . ?
N8 C63 1.302(8) . ?
N8 C64 1.369(8) . ?
N9 C67 1.173(8) . ?
N10 C68 1.206(11) . ?
C1 C2 1.412(8) . ?
C1 C6 1.426(8) . ?
C2 C3 1.369(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.361(8) . ?
C5 C6 1.426(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.417(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(8) . ?
C8 C16 1.416(8) . ?
C9 C10 1.405(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.363(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.426(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.374(9) . ?
C12 C16 1.411(8) . ?
C13 C14 1.365(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.410(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.403(8) . ?
C17 C22 1.436(8) . ?
C18 C19 1.375(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.370(9) . ?
C21 C22 1.409(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.429(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.372(8) . ?
C24 C32 1.399(8) . ?
C25 C26 1.411(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.370(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.420(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.407(9) . ?
C28 C32 1.412(8) . ?
C29 C30 1.361(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.402(9) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C33 C38 1.409(9) . ?
C33 C34 1.449(9) . ?
C34 C35 1.363(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.377(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.347(10) . ?
C37 C38 1.412(10) . ?
C37 H37 0.9500 . ?
C38 C39 1.436(10) . ?
C39 H39 0.9500 . ?
C40 C41 1.369(11) . ?
C40 C48 1.412(11) . ?
C41 C42 1.432(13) . ?
C41 H41 0.9500 . ?
C42 C43 1.330(16) . ?
C42 H42 0.9500 . ?
C43 C44 1.439(16) . ?
C43 H43 0.9500 . ?
C44 C45 1.368(15) . ?
C44 C48 1.418(11) . ?
C45 C46 1.337(15) . ?
C45 H45 0.9500 . ?
C46 C47 1.417(12) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C49 C50 1.399(9) . ?
C49 C54 1.412(8) . ?
C50 C51 1.382(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.399(9) . ?
C51 H51 0.9500 . ?
C52 C53 1.347(9) . ?
C53 C54 1.413(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.422(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.389(8) . ?
C56 C64 1.412(9) . ?
C57 C58 1.388(9) . ?
C57 H57 0.9500 . ?
C58 C59 1.356(10) . ?
C58 H58 0.9500 . ?
C59 C60 1.416(10) . ?
C59 H59 0.9500 . ?
C60 C61 1.383(10) . ?
C60 C64 1.424(9) . ?
C61 C62 1.366(10) . ?
C61 H61 0.9500 . ?
C62 C63 1.426(9) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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
O1 Fe1 O2 95.15(18) . . ?
O1 Fe1 N3 87.16(18) . . ?
O2 Fe1 N3 95.21(18) . . ?
O1 Fe1 N1 94.97(18) . . ?
O2 Fe1 N1 87.39(19) . . ?
N3 Fe1 N1 176.5(2) . . ?
O1 Fe1 N2 176.5(2) . . ?
O2 Fe1 N2 87.96(19) . . ?
N3 Fe1 N2 94.27(19) . . ?
N1 Fe1 N2 83.4(2) . . ?
O1 Fe1 N4 88.90(19) . . ?
O2 Fe1 N4 175.65(19) . . ?
N3 Fe1 N4 83.4(2) . . ?
N1 Fe1 N4 93.8(2) . . ?
N2 Fe1 N4 88.0(2) . . ?
O3 Fe2 O4 95.02(19) . . ?
O3 Fe2 N7 89.96(19) . . ?
O4 Fe2 N7 96.76(19) . . ?
O3 Fe2 N5 94.84(19) . . ?
O4 Fe2 N5 88.9(2) . . ?
N7 Fe2 N5 172.3(2) . . ?
O3 Fe2 N6 90.7(2) . . ?
O4 Fe2 N6 166.7(2) . . ?
N7 Fe2 N6 95.3(2) . . ?
N5 Fe2 N6 78.6(2) . . ?
O3 Fe2 N8 166.75(19) . . ?
O4 Fe2 N8 92.44(19) . . ?
N7 Fe2 N8 78.3(2) . . ?
N5 Fe2 N8 96.3(2) . . ?
N6 Fe2 N8 84.4(2) . . ?
C1 O1 Fe1 126.4(4) . . ?
C17 O2 Fe1 126.7(4) . . ?
C49 O3 Fe2 131.7(4) . . ?
C33 O4 Fe2 131.9(4) . . ?
C65 O5 H5A 109.5 . . ?
C66 O6 H6 109.5 . . ?
C7 N1 C8 122.2(5) . . ?
C7 N1 Fe1 124.5(4) . . ?
C8 N1 Fe1 113.2(4) . . ?
C15 N2 C16 118.8(5) . . ?
C15 N2 Fe1 128.2(4) . . ?
C16 N2 Fe1 112.9(4) . . ?
C23 N3 C24 122.7(5) . . ?
C23 N3 Fe1 124.2(4) . . ?
C24 N3 Fe1 113.1(4) . . ?
C31 N4 C32 119.0(5) . . ?
C31 N4 Fe1 128.4(4) . . ?
C32 N4 Fe1 112.6(4) . . ?
C39 N5 C40 120.2(6) . . ?
C39 N5 Fe2 125.6(5) . . ?
C40 N5 Fe2 114.1(5) . . ?
C47 N6 C48 119.7(7) . . ?
C47 N6 Fe2 126.0(6) . . ?
C48 N6 Fe2 114.2(5) . . ?
C55 N7 C56 119.9(5) . . ?
C55 N7 Fe2 124.6(4) . . ?
C56 N7 Fe2 115.4(4) . . ?
C63 N8 C64 119.5(6) . . ?
C63 N8 Fe2 126.3(5) . . ?
C64 N8 Fe2 114.2(4) . . ?
O1 C1 C2 117.9(5) . . ?
O1 C1 C6 124.6(5) . . ?
C2 C1 C6 117.5(6) . . ?
C3 C2 C1 122.0(6) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C2 C3 C4 119.9(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.9(6) . . ?
C5 C4 Br1 118.9(5) . . ?
C3 C4 Br1 120.1(5) . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C1 123.5(5) . . ?
C7 C6 C5 117.1(5) . . ?
C1 C6 C5 119.2(5) . . ?
N1 C7 C6 125.2(5) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
C9 C8 C16 118.9(6) . . ?
C9 C8 N1 127.0(6) . . ?
C16 C8 N1 114.1(5) . . ?
C8 C9 C10 118.7(6) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 122.8(6) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C10 C11 C12 120.7(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C13 C12 C16 118.7(5) . . ?
C13 C12 C11 125.2(6) . . ?
C16 C12 C11 116.0(6) . . ?
C14 C13 C12 120.4(6) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 118.8(6) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
N2 C15 C14 122.3(6) . . ?
N2 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N2 C16 C12 120.8(5) . . ?
N2 C16 C8 116.2(5) . . ?
C12 C16 C8 123.0(5) . . ?
O2 C17 C18 118.5(5) . . ?
O2 C17 C22 124.6(5) . . ?
C18 C17 C22 116.9(5) . . ?
C19 C18 C17 123.3(6) . . ?
C19 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C18 C19 C20 118.1(6) . . ?
C18 C19 H19 121.0 . . ?
C20 C19 H19 121.0 . . ?
C21 C20 C19 121.9(6) . . ?
C21 C20 Br2 120.1(5) . . ?
C19 C20 Br2 118.0(5) . . ?
C20 C21 C22 119.7(5) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C21 C22 C23 116.9(5) . . ?
C21 C22 C17 120.1(5) . . ?
C23 C22 C17 123.0(5) . . ?
N3 C23 C22 125.9(5) . . ?
N3 C23 H23 117.1 . . ?
C22 C23 H23 117.1 . . ?
C25 C24 C32 119.7(5) . . ?
C25 C24 N3 126.4(5) . . ?
C32 C24 N3 113.9(5) . . ?
C24 C25 C26 119.1(6) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 122.8(6) . . ?
C27 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C26 C27 C28 118.4(6) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C29 C28 C32 117.2(6) . . ?
C29 C28 C27 124.0(6) . . ?
C32 C28 C27 118.7(6) . . ?
C30 C29 C28 119.8(6) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 119.6(6) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
N4 C31 C30 122.5(6) . . ?
N4 C31 H31 118.7 . . ?
C30 C31 H31 118.7 . . ?
N4 C32 C24 117.0(5) . . ?
N4 C32 C28 121.8(5) . . ?
C24 C32 C28 121.2(5) . . ?
O4 C33 C38 124.9(6) . . ?
O4 C33 C34 118.9(6) . . ?
C38 C33 C34 116.2(6) . . ?
C35 C34 C33 121.2(6) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 C36 120.5(7) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C37 C36 C35 120.9(7) . . ?
C37 C36 Br3 119.9(5) . . ?
C35 C36 Br3 119.1(5) . . ?
C36 C37 C38 120.9(6) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C33 C38 C37 120.3(6) . . ?
C33 C38 C39 122.1(7) . . ?
C37 C38 C39 117.6(6) . . ?
N5 C39 C38 126.4(6) . . ?
N5 C39 H39 116.8 . . ?
C38 C39 H39 116.8 . . ?
C41 C40 C48 120.9(7) . . ?
C41 C40 N5 125.3(8) . . ?
C48 C40 N5 113.9(7) . . ?
C40 C41 C42 118.5(11) . . ?
C40 C41 H41 120.7 . . ?
C42 C41 H41 120.7 . . ?
C43 C42 C41 122.0(11) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C42 C43 C44 120.9(10) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C45 C44 C48 117.7(10) . . ?
C45 C44 C43 124.9(10) . . ?
C48 C44 C43 117.4(11) . . ?
C46 C45 C44 120.8(9) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 119.8(10) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
N6 C47 C46 120.7(10) . . ?
N6 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
N6 C48 C40 118.5(6) . . ?
N6 C48 C44 121.2(9) . . ?
C40 C48 C44 120.2(9) . . ?
O3 C49 C50 119.3(6) . . ?
O3 C49 C54 123.1(5) . . ?
C50 C49 C54 117.6(6) . . ?
C51 C50 C49 122.1(6) . . ?
C51 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
C50 C51 C52 119.3(6) . . ?
C50 C51 H51 120.4 . . ?
C52 C51 H51 120.4 . . ?
C53 C52 C51 120.2(6) . . ?
C53 C52 Br4 120.3(5) . . ?
C51 C52 Br4 119.5(5) . . ?
C52 C53 C54 121.5(6) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
C49 C54 C53 119.4(6) . . ?
C49 C54 C55 123.9(6) . . ?
C53 C54 C55 116.7(5) . . ?
N7 C55 C54 126.4(6) . . ?
N7 C55 H55 116.8 . . ?
C54 C55 H55 116.8 . . ?
C57 C56 C64 118.4(6) . . ?
C57 C56 N7 127.2(6) . . ?
C64 C56 N7 114.4(5) . . ?
C58 C57 C56 121.0(7) . . ?
C58 C57 H57 119.5 . . ?
C56 C57 H57 119.5 . . ?
C59 C58 C57 121.3(7) . . ?
C59 C58 H58 119.4 . . ?
C57 C58 H58 119.4 . . ?
C58 C59 C60 120.7(6) . . ?
C58 C59 H59 119.7 . . ?
C60 C59 H59 119.7 . . ?
C61 C60 C59 125.0(7) . . ?
C61 C60 C64 117.1(7) . . ?
C59 C60 C64 117.9(6) . . ?
C62 C61 C60 120.8(7) . . ?
C62 C61 H61 119.6 . . ?
C60 C61 H61 119.6 . . ?
C61 C62 C63 118.6(6) . . ?
C61 C62 H62 120.7 . . ?
C63 C62 H62 120.7 . . ?
N8 C63 C62 122.1(7) . . ?
N8 C63 H63 118.9 . . ?
C62 C63 H63 118.9 . . ?
N8 C64 C56 117.6(5) . . ?
N8 C64 C60 121.7(6) . . ?
C56 C64 C60 120.6(6) . . ?
O5 C65 H65A 109.5 . . ?
O5 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
O5 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O6 C66 H66A 109.5 . . ?
O6 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
O6 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N9 C67 S1 178.9(7) . . ?
N10 C68 S2 178.3(8) . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         1.591
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.130
_database_code_depnum_ccdc_archive 'CCDC 994840'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp42RT

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H20 Br2 Fe N4 O2, C N S, C H4 O'
_chemical_formula_sum            'C34 H24 Br2 Cl0 Fe N5 O3 S'
_chemical_formula_weight         798.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'

_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                   10.3118(6)
_cell_length_b                   12.8729(8)
_cell_length_c                   25.6592(16)
_cell_angle_alpha                76.441(2)
_cell_angle_beta                 79.516(2)
_cell_angle_gamma                77.756(2)
_cell_volume                     3204.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3404
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      22.59

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    3.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.414
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(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  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21439
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         27.50
_reflns_number_total             14503
_reflns_number_gt                6829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.

The asymmetric unit contains two iron monomers, two thiocyanate anions and 
two methanol solvent molecules. All the non-hydrogen atoms are refined 
anisotropically and all hydrogen  atoms are placed in calculated positions.   
;

_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)+(0.0940P)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         14503
_refine_ls_number_parameters     826
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1624
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1907
_refine_ls_wR_factor_gt          0.1476
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      0.930
_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 0.63827(8) 0.64333(6) 0.37709(3) 0.0328(2) Uani 1 1 d . . .
Br1 Br 0.11578(8) 0.85956(7) 0.58009(3) 0.0716(3) Uani 1 1 d . . .
Fe2 Fe 0.49556(8) 1.05927(7) 0.12395(3) 0.0416(2) Uani 1 1 d . . .
Br4 Br 1.03279(8) 0.87834(7) -0.09113(3) 0.0698(3) Uani 1 1 d . . .
Br3 Br 0.13297(8) 0.64805(7) 0.31855(3) 0.0811(3) Uani 1 1 d . . .
Br2 Br 0.32920(9) 0.41756(7) 0.20256(3) 0.0766(3) Uani 1 1 d . . .
O4 O 0.3942(4) 0.9461(3) 0.13239(16) 0.0520(11) Uani 1 1 d . . .
O2 O 0.5422(4) 0.5337(3) 0.37956(15) 0.0392(10) Uani 1 1 d . . .
O3 O 0.6654(4) 0.9704(3) 0.10895(16) 0.0522(11) Uani 1 1 d . . .
N7 N 0.5024(5) 1.1215(4) 0.03935(19) 0.0397(12) Uani 1 1 d . . .
N3 N 0.6513(5) 0.6926(4) 0.29921(17) 0.0349(11) Uani 1 1 d . . .
N2 N 0.8033(5) 0.5338(4) 0.37383(18) 0.0358(11) Uani 1 1 d . . .
N5 N 0.4822(5) 1.0273(4) 0.2094(2) 0.0479(13) Uani 1 1 d . . .
C53 C 0.8033(6) 0.9847(5) -0.0335(2) 0.0444(15) Uani 1 1 d . . .
H53 H 0.7842 1.0213 -0.0678 0.053 Uiso 1 1 calc R . .
N4 N 0.7515(4) 0.7523(4) 0.37162(18) 0.0368(11) Uani 1 1 d . . .
N8 N 0.3208(5) 1.1848(4) 0.1173(2) 0.0483(13) Uani 1 1 d . . .
N1 N 0.6345(5) 0.5930(4) 0.45475(17) 0.0350(11) Uani 1 1 d . . .
C1 C 0.4096(6) 0.7701(5) 0.4274(2) 0.0392(14) Uani 1 1 d . . .
C3 C 0.2171(6) 0.8855(6) 0.4670(3) 0.0542(18) Uani 1 1 d . . .
H3 H 0.1471 0.9443 0.4629 0.065 Uiso 1 1 calc R . .
N6 N 0.5894(5) 1.1827(5) 0.1388(3) 0.0583(15) Uani 1 1 d . . .
C7 C 0.5384(6) 0.6240(5) 0.4910(2) 0.0397(14) Uani 1 1 d . . .
H7 H 0.5423 0.5881 0.5268 0.048 Uiso 1 1 calc R . .
C6 C 0.4266(6) 0.7095(5) 0.4802(2) 0.0374(14) Uani 1 1 d . . .
C21 C 0.4732(6) 0.5384(5) 0.2435(2) 0.0462(16) Uani 1 1 d . . .
H21 H 0.4857 0.5764 0.2078 0.055 Uiso 1 1 calc R . .
C25 C 0.7614(6) 0.8255(5) 0.2259(2) 0.0446(15) Uani 1 1 d . . .
H25 H 0.7280 0.8068 0.1987 0.054 Uiso 1 1 calc R . .
C23 C 0.5945(5) 0.6574(5) 0.2682(2) 0.0376(14) Uani 1 1 d . . .
H23 H 0.6004 0.6922 0.2319 0.045 Uiso 1 1 calc R . .
C55 C 0.5965(6) 1.0891(5) 0.0035(2) 0.0444(15) Uani 1 1 d . . .
H55 H 0.5873 1.1219 -0.0323 0.053 Uiso 1 1 calc R . .
C54 C 0.7148(6) 1.0081(5) 0.0120(2) 0.0423(15) Uani 1 1 d . . .
C5 C 0.3359(6) 0.7373(5) 0.5250(2) 0.0451(15) Uani 1 1 d . . .
H5 H 0.3456 0.6958 0.5595 0.054 Uiso 1 1 calc R . .
C33 C 0.3383(6) 0.8831(5) 0.1740(2) 0.0414(14) Uani 1 1 d . . .
C24 C 0.7303(5) 0.7761(4) 0.2788(2) 0.0354(13) Uani 1 1 d . . .
C15 C 0.8808(6) 0.5023(5) 0.3307(2) 0.0430(15) Uani 1 1 d . . .
H15 H 0.8569 0.5347 0.2965 0.052 Uiso 1 1 calc R . .
C18 C 0.4403(6) 0.4201(5) 0.3482(3) 0.0450(15) Uani 1 1 d . . .
H18 H 0.4308 0.3776 0.3829 0.054 Uiso 1 1 calc R . .
C31 C 0.7954(7) 0.7790(5) 0.4107(3) 0.0504(17) Uani 1 1 d . . .
H31 H 0.7712 0.7449 0.4463 0.060 Uiso 1 1 calc R . .
C17 C 0.5039(5) 0.5098(5) 0.3391(2) 0.0367(14) Uani 1 1 d . . .
C37 C 0.2831(7) 0.8142(5) 0.2711(3) 0.0532(17) Uani 1 1 d . . .
H37 H 0.2905 0.8144 0.3066 0.064 Uiso 1 1 calc R . .
C8 C 0.7489(6) 0.5143(4) 0.4689(2) 0.0373(14) Uani 1 1 d . . .
C32 C 0.7829(5) 0.8050(4) 0.3193(2) 0.0363(13) Uani 1 1 d . . .
C20 C 0.4072(6) 0.4535(5) 0.2563(3) 0.0479(16) Uani 1 1 d . . .
C22 C 0.5233(6) 0.5697(5) 0.2845(2) 0.0388(14) Uani 1 1 d . . .
C51 C 0.9474(6) 0.8555(5) 0.0225(3) 0.0520(17) Uani 1 1 d . . .
H51 H 1.0257 0.8044 0.0257 0.062 Uiso 1 1 calc R . .
C38 C 0.3458(6) 0.8858(5) 0.2281(2) 0.0425(15) Uani 1 1 d . . .
C36 C 0.2141(7) 0.7469(5) 0.2613(3) 0.0526(18) Uani 1 1 d . . .
C49 C 0.7446(6) 0.9532(5) 0.0647(2) 0.0415(15) Uani 1 1 d . . .
C4 C 0.2355(6) 0.8231(6) 0.5186(3) 0.0523(17) Uani 1 1 d . . .
C9 C 0.7781(6) 0.4674(5) 0.5203(2) 0.0479(16) Uani 1 1 d . . .
H9 H 0.7226 0.4885 0.5503 0.057 Uiso 1 1 calc R . .
C63 C 0.2361(6) 1.2141(6) 0.1582(3) 0.0582(19) Uani 1 1 d . . .
H63 H 0.2493 1.1757 0.1929 0.070 Uiso 1 1 calc R . .
C2 C 0.3028(6) 0.8594(5) 0.4226(3) 0.0525(17) Uani 1 1 d . . .
H2 H 0.2904 0.9016 0.3885 0.063 Uiso 1 1 calc R . .
C48 C 0.6045(6) 1.1731(6) 0.1908(3) 0.0585(19) Uani 1 1 d . . .
C16 C 0.8371(6) 0.4830(4) 0.4242(2) 0.0343(13) Uani 1 1 d . . .
C56 C 0.3945(6) 1.2050(5) 0.0231(3) 0.0428(15) Uani 1 1 d . . .
C52 C 0.9166(6) 0.9097(5) -0.0285(3) 0.0461(16) Uani 1 1 d . . .
C39 C 0.4172(6) 0.9565(6) 0.2419(2) 0.0507(17) Uani 1 1 d . . .
H39 H 0.4172 0.9512 0.2786 0.061 Uiso 1 1 calc R . .
C35 C 0.2043(7) 0.7411(5) 0.2084(3) 0.0573(18) Uani 1 1 d . . .
H35 H 0.1580 0.6918 0.2020 0.069 Uiso 1 1 calc R . .
C47 C 0.6355(7) 1.2605(6) 0.1025(4) 0.073(2) Uani 1 1 d . . .
H47 H 0.6254 1.2662 0.0666 0.087 Uiso 1 1 calc R . .
C64 C 0.3018(6) 1.2380(5) 0.0657(3) 0.0451(15) Uani 1 1 d . . .
C19 C 0.3919(6) 0.3924(5) 0.3087(3) 0.0500(17) Uani 1 1 d . . .
H19 H 0.3488 0.3329 0.3166 0.060 Uiso 1 1 calc R . .
C34 C 0.2646(7) 0.8100(5) 0.1664(3) 0.0585(19) Uani 1 1 d . . .
H34 H 0.2561 0.8079 0.1312 0.070 Uiso 1 1 calc R . .
C40 C 0.5507(6) 1.0915(6) 0.2299(3) 0.0556(18) Uani 1 1 d . . .
C41 C 0.5663(8) 1.0784(8) 0.2832(3) 0.081(3) Uani 1 1 d . . .
H41 H 0.5298 1.0251 0.3094 0.097 Uiso 1 1 calc R . .
C12 C 0.9535(6) 0.4039(5) 0.4303(3) 0.0435(15) Uani 1 1 d . . .
C28 C 0.8654(6) 0.8845(5) 0.3057(3) 0.0459(15) Uani 1 1 d . . .
C30 C 0.8774(7) 0.8571(5) 0.4006(3) 0.0606(19) Uani 1 1 d . . .
H30 H 0.9075 0.8734 0.4292 0.073 Uiso 1 1 calc R . .
C50 C 0.8635(7) 0.8767(5) 0.0682(3) 0.0519(17) Uani 1 1 d . . .
H50 H 0.8857 0.8398 0.1020 0.062 Uiso 1 1 calc R . .
C29 C 0.9129(7) 0.9087(5) 0.3498(3) 0.0574(18) Uani 1 1 d . . .
H29 H 0.9682 0.9602 0.3433 0.069 Uiso 1 1 calc R . .
C13 C 1.0320(6) 0.3757(5) 0.3850(3) 0.0527(17) Uani 1 1 d . . .
H13 H 1.1100 0.3243 0.3883 0.063 Uiso 1 1 calc R . .
C26 C 0.8443(7) 0.9050(5) 0.2127(3) 0.0576(19) Uani 1 1 d . . .
H26 H 0.8637 0.9383 0.1766 0.069 Uiso 1 1 calc R . .
C11 C 0.9791(7) 0.3564(5) 0.4837(3) 0.0574(18) Uani 1 1 d . . .
H11 H 1.0550 0.3037 0.4895 0.069 Uiso 1 1 calc R . .
C10 C 0.8939(7) 0.3866(6) 0.5270(3) 0.0604(19) Uani 1 1 d . . .
H10 H 0.9124 0.3533 0.5618 0.072 Uiso 1 1 calc R . .
C14 C 0.9962(7) 0.4229(5) 0.3344(3) 0.0550(18) Uani 1 1 d . . .
H14 H 1.0476 0.4024 0.3036 0.066 Uiso 1 1 calc R . .
C27 C 0.8965(7) 0.9344(5) 0.2507(3) 0.0515(17) Uani 1 1 d . . .
H27 H 0.9517 0.9863 0.2408 0.062 Uiso 1 1 calc R . .
C46 C 0.6989(8) 1.3356(7) 0.1144(5) 0.096(3) Uani 1 1 d . . .
H46 H 0.7257 1.3922 0.0874 0.115 Uiso 1 1 calc R . .
C42 C 0.6383(9) 1.1464(9) 0.2982(5) 0.100(3) Uani 1 1 d . . .
H42 H 0.6506 1.1365 0.3341 0.120 Uiso 1 1 calc R . .
C45 C 0.7205(9) 1.3247(9) 0.1649(5) 0.096(3) Uani 1 1 d . . .
H45 H 0.7662 1.3721 0.1734 0.116 Uiso 1 1 calc R . .
C43 C 0.6898(8) 1.2264(9) 0.2602(5) 0.100(4) Uani 1 1 d . . .
H43 H 0.7355 1.2709 0.2711 0.120 Uiso 1 1 calc R . .
C44 C 0.6754(8) 1.2437(8) 0.2045(4) 0.078(3) Uani 1 1 d . . .
O1 O 0.4869(4) 0.7522(3) 0.38260(15) 0.0438(10) Uani 1 1 d . . .
S1 S 0.8577(2) 0.55763(18) 0.18183(9) 0.0793(6) Uani 1 1 d . . .
C67 C 0.9834(9) 0.6058(6) 0.1436(3) 0.068(2) Uani 1 1 d . . .
N9 N 1.0721(8) 0.6387(7) 0.1149(4) 0.109(3) Uani 1 1 d . . .
O6 O 1.3084(8) 0.6775(7) 0.0454(4) 0.136(3) Uani 1 1 d . . .
H6 H 1.2284 0.6746 0.0498 0.163 Uiso 1 1 calc R . .
C66 C 1.3784(14) 0.5796(10) 0.0486(6) 0.181(7) Uani 1 1 d . . .
H66A H 1.4297 0.5727 0.0140 0.271 Uiso 1 1 calc R . .
H66B H 1.3190 0.5277 0.0590 0.271 Uiso 1 1 calc R . .
H66C H 1.4378 0.5663 0.0751 0.271 Uiso 1 1 calc R . .
O5 O 0.6849(9) 0.7966(7) 0.5391(4) 0.145(3) Uani 1 1 d . . .
H5A H 0.7498 0.8128 0.5476 0.174 Uiso 1 1 calc R . .
C65 C 0.6047(11) 0.8846(9) 0.5202(6) 0.141(5) Uani 1 1 d . . .
H65A H 0.5400 0.9070 0.5493 0.212 Uiso 1 1 calc R . .
H65B H 0.5593 0.8707 0.4937 0.212 Uiso 1 1 calc R . .
H65C H 0.6557 0.9411 0.5037 0.212 Uiso 1 1 calc R . .
C59 C 0.1778(8) 1.3736(6) 0.0013(4) 0.076(2) Uani 1 1 d . . .
H59 H 0.1078 1.4310 -0.0064 0.092 Uiso 1 1 calc R . .
C57 C 0.3726(7) 1.2542(6) -0.0294(3) 0.0598(19) Uani 1 1 d . . .
H57 H 0.4308 1.2308 -0.0582 0.072 Uiso 1 1 calc R . .
C61 C 0.1078(7) 1.3540(6) 0.1011(4) 0.073(2) Uani 1 1 d . . .
H61 H 0.0371 1.4120 0.0959 0.088 Uiso 1 1 calc R . .
C60 C 0.1917(7) 1.3248(6) 0.0556(4) 0.062(2) Uani 1 1 d . . .
C58 C 0.2642(8) 1.3386(6) -0.0397(4) 0.077(2) Uani 1 1 d . . .
H58 H 0.2517 1.3709 -0.0753 0.092 Uiso 1 1 calc R . .
C62 C 0.1248(3) 1.3015(2) 0.15253(12) 0.072(2) Uani 1 1 d . . .
H62 H 0.0673 1.3213 0.1824 0.087 Uiso 1 1 calc R . .
S2 S 1.1212(3) 1.1171(2) 0.29904(12) 0.1627(18) Uani 1 1 d R . .
C68 C 1.2184(3) 1.1386(2) 0.34164(12) 0.124(6) Uani 1 1 d R . .
N10 N 1.2702(3) 1.1521(2) 0.36898(12) 0.194(7) Uani 1 1 d 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 O2 1.872(4) . ?
Fe1 O1 1.873(4) . ?
Fe1 N3 1.938(4) . ?
Fe1 N1 1.942(4) . ?
Fe1 N2 1.969(5) . ?
Fe1 N4 1.974(5) . ?
Br1 C4 1.903(6) . ?
Fe2 O3 1.907(4) . ?
Fe2 O4 1.917(4) . ?
Fe2 N5 2.118(5) . ?
Fe2 N7 2.124(5) . ?
Fe2 N8 2.153(5) . ?
Fe2 N6 2.162(5) . ?
Br4 C52 1.893(6) . ?
Br3 C36 1.899(6) . ?
Br2 C20 1.902(6) . ?
O4 C33 1.303(6) . ?
O2 C17 1.296(7) . ?
O3 C49 1.307(7) . ?
N7 C55 1.283(7) . ?
N7 C56 1.421(7) . ?
N3 C23 1.278(7) . ?
N3 C24 1.431(7) . ?
N2 C15 1.335(7) . ?
N2 C16 1.376(7) . ?
N5 C39 1.294(8) . ?
N5 C40 1.430(8) . ?
C53 C52 1.354(8) . ?
C53 C54 1.396(8) . ?
C53 H53 0.9300 . ?
N4 C31 1.313(7) . ?
N4 C32 1.370(7) . ?
N8 C63 1.311(8) . ?
N8 C64 1.369(8) . ?
N1 C7 1.296(7) . ?
N1 C8 1.424(7) . ?
C1 O1 1.313(6) . ?
C1 C2 1.413(8) . ?
C1 C6 1.415(8) . ?
C3 C2 1.370(8) . ?
C3 C4 1.401(9) . ?
C3 H3 0.9300 . ?
N6 C47 1.304(9) . ?
N6 C48 1.346(9) . ?
C7 C6 1.433(8) . ?
C7 H7 0.9300 . ?
C6 C5 1.410(8) . ?
C21 C20 1.353(8) . ?
C21 C22 1.422(8) . ?
C21 H21 0.9300 . ?
C25 C24 1.369(7) . ?
C25 C26 1.412(8) . ?
C25 H25 0.9300 . ?
C23 C22 1.417(8) . ?
C23 H23 0.9300 . ?
C55 C54 1.439(8) . ?
C55 H55 0.9300 . ?
C54 C49 1.426(8) . ?
C5 C4 1.345(9) . ?
C5 H5 0.9300 . ?
C33 C34 1.393(9) . ?
C33 C38 1.414(8) . ?
C24 C32 1.407(8) . ?
C15 C14 1.396(8) . ?
C15 H15 0.9300 . ?
C18 C19 1.353(8) . ?
C18 C17 1.399(8) . ?
C18 H18 0.9300 . ?
C31 C30 1.397(9) . ?
C31 H31 0.9300 . ?
C17 C22 1.433(8) . ?
C37 C36 1.322(9) . ?
C37 C38 1.415(8) . ?
C37 H37 0.9300 . ?
C8 C9 1.374(8) . ?
C8 C16 1.409(8) . ?
C32 C28 1.410(8) . ?
C20 C19 1.391(9) . ?
C51 C50 1.370(9) . ?
C51 C52 1.389(9) . ?
C51 H51 0.9300 . ?
C38 C39 1.424(9) . ?
C36 C35 1.399(9) . ?
C49 C50 1.402(8) . ?
C9 C10 1.414(9) . ?
C9 H9 0.9300 . ?
C63 C62 1.429(8) . ?
C63 H63 0.9300 . ?
C2 H2 0.9300 . ?
C48 C40 1.404(10) . ?
C48 C44 1.417(10) . ?
C16 C12 1.406(8) . ?
C56 C57 1.383(9) . ?
C56 C64 1.398(9) . ?
C39 H39 0.9300 . ?
C35 C34 1.371(8) . ?
C35 H35 0.9300 . ?
C47 C46 1.390(11) . ?
C47 H47 0.9300 . ?
C64 C60 1.428(9) . ?
C19 H19 0.9300 . ?
C34 H34 0.9300 . ?
C40 C41 1.373(10) . ?
C41 C42 1.414(11) . ?
C41 H41 0.9300 . ?
C12 C13 1.367(9) . ?
C12 C11 1.411(9) . ?
C28 C27 1.416(8) . ?
C28 C29 1.432(9) . ?
C30 C29 1.340(9) . ?
C30 H30 0.9300 . ?
C50 H50 0.9300 . ?
C29 H29 0.9300 . ?
C13 C14 1.377(9) . ?
C13 H13 0.9300 . ?
C26 C27 1.354(9) . ?
C26 H26 0.9300 . ?
C11 C10 1.364(9) . ?
C11 H11 0.9300 . ?
C10 H10 0.9300 . ?
C14 H14 0.9300 . ?
C27 H27 0.9300 . ?
C46 C45 1.325(13) . ?
C46 H46 0.9300 . ?
C42 C43 1.366(14) . ?
C42 H42 0.9300 . ?
C45 C44 1.368(13) . ?
C45 H45 0.9300 . ?
C43 C44 1.426(13) . ?
C43 H43 0.9300 . ?
S1 C67 1.618(9) . ?
C67 N9 1.154(10) . ?
O6 C66 1.305(12) . ?
O6 H6 0.8200 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
O5 C65 1.302(11) . ?
O5 H5A 0.8200 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C59 C58 1.347(11) . ?
C59 C60 1.406(11) . ?
C59 H59 0.9300 . ?
C57 C58 1.399(10) . ?
C57 H57 0.9300 . ?
C61 C62 1.358(9) . ?
C61 C60 1.398(11) . ?
C61 H61 0.9300 . ?
C58 H58 0.9300 . ?
C62 H62 0.9300 . ?
S2 C68 1.7130 . ?
C68 N10 1.0197 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 95.22(18) . . ?
O2 Fe1 N3 94.69(18) . . ?
O1 Fe1 N3 87.43(18) . . ?
O2 Fe1 N1 86.87(18) . . ?
O1 Fe1 N1 94.69(18) . . ?
N3 Fe1 N1 177.3(2) . . ?
O2 Fe1 N2 88.04(18) . . ?
O1 Fe1 N2 176.20(19) . . ?
N3 Fe1 N2 94.26(19) . . ?
N1 Fe1 N2 83.52(19) . . ?
O2 Fe1 N4 175.60(18) . . ?
O1 Fe1 N4 88.82(19) . . ?
N3 Fe1 N4 83.72(19) . . ?
N1 Fe1 N4 94.56(19) . . ?
N2 Fe1 N4 87.99(19) . . ?
O3 Fe2 O4 95.0(2) . . ?
O3 Fe2 N5 98.21(18) . . ?
O4 Fe2 N5 87.75(19) . . ?
O3 Fe2 N7 88.08(18) . . ?
O4 Fe2 N7 100.07(17) . . ?
N5 Fe2 N7 169.5(2) . . ?
O3 Fe2 N8 163.2(2) . . ?
O4 Fe2 N8 92.88(19) . . ?
N5 Fe2 N8 96.9(2) . . ?
N7 Fe2 N8 75.9(2) . . ?
O3 Fe2 N6 91.5(2) . . ?
O4 Fe2 N6 163.6(2) . . ?
N5 Fe2 N6 76.4(2) . . ?
N7 Fe2 N6 95.2(2) . . ?
N8 Fe2 N6 85.0(2) . . ?
C33 O4 Fe2 134.2(4) . . ?
C17 O2 Fe1 127.1(3) . . ?
C49 O3 Fe2 134.5(4) . . ?
C55 N7 C56 119.7(5) . . ?
C55 N7 Fe2 124.3(4) . . ?
C56 N7 Fe2 116.1(4) . . ?
C23 N3 C24 121.9(5) . . ?
C23 N3 Fe1 125.0(4) . . ?
C24 N3 Fe1 113.1(4) . . ?
C15 N2 C16 118.1(5) . . ?
C15 N2 Fe1 129.1(4) . . ?
C16 N2 Fe1 112.7(4) . . ?
C39 N5 C40 120.8(6) . . ?
C39 N5 Fe2 124.3(4) . . ?
C40 N5 Fe2 114.9(4) . . ?
C52 C53 C54 121.0(6) . . ?
C52 C53 H53 119.5 . . ?
C54 C53 H53 119.5 . . ?
C31 N4 C32 119.3(5) . . ?
C31 N4 Fe1 128.4(4) . . ?
C32 N4 Fe1 112.2(4) . . ?
C63 N8 C64 119.3(6) . . ?
C63 N8 Fe2 125.2(5) . . ?
C64 N8 Fe2 115.5(4) . . ?
C7 N1 C8 121.9(5) . . ?
C7 N1 Fe1 125.1(4) . . ?
C8 N1 Fe1 113.0(3) . . ?
O1 C1 C2 117.0(5) . . ?
O1 C1 C6 125.5(5) . . ?
C2 C1 C6 117.4(5) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C47 N6 C48 118.7(7) . . ?
C47 N6 Fe2 126.5(6) . . ?
C48 N6 Fe2 114.8(5) . . ?
N1 C7 C6 124.9(5) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C5 C6 C1 119.8(6) . . ?
C5 C6 C7 117.2(5) . . ?
C1 C6 C7 122.8(5) . . ?
C20 C21 C22 120.0(6) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C24 C25 C26 119.9(6) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
N3 C23 C22 125.3(5) . . ?
N3 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
N7 C55 C54 127.8(6) . . ?
N7 C55 H55 116.1 . . ?
C54 C55 H55 116.1 . . ?
C53 C54 C49 119.6(6) . . ?
C53 C54 C55 117.8(6) . . ?
C49 C54 C55 122.5(5) . . ?
C4 C5 C6 120.9(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
O4 C33 C34 120.2(6) . . ?
O4 C33 C38 123.0(5) . . ?
C34 C33 C38 116.7(6) . . ?
C25 C24 C32 119.2(5) . . ?
C25 C24 N3 127.3(5) . . ?
C32 C24 N3 113.5(4) . . ?
N2 C15 C14 122.9(6) . . ?
N2 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
C19 C18 C17 122.9(6) . . ?
C19 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
N4 C31 C30 122.1(6) . . ?
N4 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
O2 C17 C18 119.1(5) . . ?
O2 C17 C22 124.0(5) . . ?
C18 C17 C22 116.9(5) . . ?
C36 C37 C38 120.8(6) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C9 C8 C16 119.2(6) . . ?
C9 C8 N1 126.7(5) . . ?
C16 C8 N1 114.1(5) . . ?
N4 C32 C24 117.4(5) . . ?
N4 C32 C28 122.0(5) . . ?
C24 C32 C28 120.5(5) . . ?
C21 C20 C19 121.3(6) . . ?
C21 C20 Br2 120.2(5) . . ?
C19 C20 Br2 118.5(5) . . ?
C23 C22 C21 117.2(5) . . ?
C23 C22 C17 123.5(5) . . ?
C21 C22 C17 119.3(5) . . ?
C50 C51 C52 120.6(6) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 H51 119.7 . . ?
C33 C38 C37 119.6(6) . . ?
C33 C38 C39 122.8(5) . . ?
C37 C38 C39 117.5(6) . . ?
C37 C36 C35 121.5(6) . . ?
C37 C36 Br3 121.2(6) . . ?
C35 C36 Br3 117.2(5) . . ?
O3 C49 C50 119.7(6) . . ?
O3 C49 C54 122.7(6) . . ?
C50 C49 C54 117.6(5) . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 Br1 119.9(5) . . ?
C3 C4 Br1 119.5(5) . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N8 C63 C62 123.8(7) . . ?
N8 C63 H63 118.1 . . ?
C62 C63 H63 118.1 . . ?
C3 C2 C1 121.5(6) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
N6 C48 C40 118.4(6) . . ?
N6 C48 C44 119.6(8) . . ?
C40 C48 C44 122.0(8) . . ?
N2 C16 C12 121.2(5) . . ?
N2 C16 C8 116.5(5) . . ?
C12 C16 C8 122.3(5) . . ?
C57 C56 C64 118.3(6) . . ?
C57 C56 N7 127.0(6) . . ?
C64 C56 N7 114.7(6) . . ?
C53 C52 C51 120.2(6) . . ?
C53 C52 Br4 119.8(5) . . ?
C51 C52 Br4 120.0(5) . . ?
N5 C39 C38 127.8(6) . . ?
N5 C39 H39 116.1 . . ?
C38 C39 H39 116.1 . . ?
C34 C35 C36 118.3(6) . . ?
C34 C35 H35 120.9 . . ?
C36 C35 H35 120.9 . . ?
N6 C47 C46 123.8(9) . . ?
N6 C47 H47 118.1 . . ?
C46 C47 H47 118.1 . . ?
N8 C64 C56 117.7(6) . . ?
N8 C64 C60 121.2(6) . . ?
C56 C64 C60 121.0(7) . . ?
C18 C19 C20 119.6(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C35 C34 C33 123.0(6) . . ?
C35 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C41 C40 C48 119.8(7) . . ?
C41 C40 N5 125.3(7) . . ?
C48 C40 N5 114.9(6) . . ?
C40 C41 C42 119.7(9) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C13 C12 C16 118.8(6) . . ?
C13 C12 C11 124.3(6) . . ?
C16 C12 C11 116.9(6) . . ?
C32 C28 C27 119.3(6) . . ?
C32 C28 C29 116.3(5) . . ?
C27 C28 C29 124.4(6) . . ?
C29 C30 C31 120.5(6) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C51 C50 C49 121.0(6) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C30 C29 C28 119.8(6) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C12 C13 C14 120.4(6) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C27 C26 C25 122.3(6) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C10 C11 C12 120.9(6) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C10 C9 121.7(6) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C13 C14 C15 118.4(6) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C26 C27 C28 118.7(6) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
C45 C46 C47 118.6(10) . . ?
C45 C46 H46 120.7 . . ?
C47 C46 H46 120.7 . . ?
C43 C42 C41 120.5(9) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C46 C45 C44 120.0(9) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C42 C43 C44 121.9(9) . . ?
C42 C43 H43 119.0 . . ?
C44 C43 H43 119.0 . . ?
C45 C44 C48 119.2(9) . . ?
C45 C44 C43 124.7(9) . . ?
C48 C44 C43 116.0(9) . . ?
C1 O1 Fe1 126.3(4) . . ?
N9 C67 S1 177.6(9) . . ?
C66 O6 H6 109.5 . . ?
O6 C66 H66A 109.5 . . ?
O6 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
O6 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 O5 H5A 109.5 . . ?
O5 C65 H65A 109.5 . . ?
O5 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
O5 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C58 C59 C60 121.2(7) . . ?
C58 C59 H59 119.4 . . ?
C60 C59 H59 119.4 . . ?
C56 C57 C58 121.0(7) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 H57 119.5 . . ?
C62 C61 C60 123.0(7) . . ?
C62 C61 H61 118.5 . . ?
C60 C61 H61 118.5 . . ?
C61 C60 C59 126.0(8) . . ?
C61 C60 C64 116.4(8) . . ?
C59 C60 C64 117.6(7) . . ?
C59 C58 C57 120.7(8) . . ?
C59 C58 H58 119.6 . . ?
C57 C58 H58 119.6 . . ?
C61 C62 C63 116.2(5) . . ?
C61 C62 H62 121.9 . . ?
C63 C62 H62 121.9 . . ?
N10 C68 S2 175.9 . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.090
_database_code_depnum_ccdc_archive 'CCDC 994841'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wp57lt

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C32 H20 Fe I2 N4 O2), 2(C N S), 0.5(C H2 Cl2), (C H4 O)
;
_chemical_formula_sum            'C67.50 H42.40 Cl Fe2 I4 N10 O5 S2'
_chemical_formula_weight         1792.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   20.8247(10)
_cell_length_b                   23.9937(11)
_cell_length_c                   12.6558(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.1070(10)
_cell_angle_gamma                90.00
_cell_volume                     6322.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7040
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      27.32

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3482
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3896
_exptl_absorpt_correction_T_max  0.6981
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(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  'APEX X8'
_diffrn_measurement_method       'Scans in phi  and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            43766
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.54
_reflns_number_total             14538
_reflns_number_gt                9770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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.

The asymmetric unit contains two iron monomers, two thiocyanate anions,
a half occupied dichloromethane solvate molecule and a methanol solvate
molecule. All the non-hydrogen atoms are refined anisotropically and all
hydrogen atoms are placed in calculated positions. One thiocyanate is 
disordered over two positions, the first, S1-C65-N9, with a fixed
occupancy of 0.65 and the second, S1'-C65'N9', with a fixed occupancy
of 0.35. The second thiocyanate has been modelled over two positions, 
S2-C66-N10 and S2'-C66'-N10' each with half occupancy. The dichloromethane
solvate molecule, Cl1-C68-Cl2 has been modelled with half occupancy and
sits over the same position as S2-C66-N10. There is a methanol solvate molecule
which is disordered over two positions, O5-C67 (0.35 occupancy) and O5'-C67'
(0.65 occupancy).

The following restraints have been applied:

DFIX 1.72 0.001 C68 CL1 C68 CL2
DFIX 1.42 0.001 C67 O5 C67' O5'
DFIX 1.65 0.001 S2 C66 S2' C66' S1' C65'
DFIX 1.17 0.001 C66 N10 C66' N10' N9 C65'
ISOR 0.001 N10 C66 CL1 C67 O5' S2' C66'
ISOR 0.001 N10' C68 C67' S1'

Response to PLAT431 ALERT 2 A
The short I4-S1' contact of 3.24 Angstroms (14% less than van der Waals radius)
is comparable to values reported by Pennignton et al (Chem Comm 2010 46 1854) of 
around 3.28 angstroms and Kato et al (J Chem Soc Chem Commun 1995 1097) of 
around 3.31 angstroms.

The cif check has reported discrepancies between the chemical formula sum and moeity.
This happens when there are fractional occupancies present and the cif check seems to
multiply to integer numbers making the calculated Z and formula incorrect. Z is clearly four
when examining the unit cell in a X-Seed and so the reported formula and z is correct.
 
;

_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)+(0.0451P)²+14.8471P] 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         14538
_refine_ls_number_parameters     905
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.051948(18) 0.373987(17) 0.24000(3) 0.02289(10) Uani 1 1 d . . .
I2 I 0.591903(18) 0.357603(18) 0.69352(3) 0.02370(10) Uani 1 1 d . . .
I3 I 0.556091(18) 0.133353(18) 0.69405(3) 0.02477(10) Uani 1 1 d . . .
I4 I 1.093140(17) 0.140894(17) 0.24924(3) 0.02086(10) Uani 1 1 d . . .
Fe1 Fe 0.31573(4) 0.18856(3) 0.46353(6) 0.01494(17) Uani 1 1 d . . .
Fe2 Fe 0.82358(4) 0.31216(3) 0.47838(6) 0.01693(18) Uani 1 1 d . . .
Cl1 Cl 0.7115(6) 0.4336(6) 0.8026(11) 0.165(5) Uani 0.50 1 d PDU A 2
Cl2 Cl 0.6350(2) 0.4843(2) 0.9389(3) 0.0566(11) Uani 0.50 1 d PD A 2
S1 S 0.95443(19) 0.4523(2) 0.0918(3) 0.0405(9) Uani 0.65 1 d P B 1
S1' S 0.8111(3) 0.5584(3) 0.3757(7) 0.0547(18) Uani 0.35 1 d PDU C 2
S2 S 0.7141(2) 0.43464(17) 0.8035(4) 0.0299(11) Uani 0.50 1 d PD D 1
S2' S 0.4588(3) 0.0179(3) 0.9058(5) 0.0944(19) Uani 0.50 1 d PDU E 2
O1 O 0.24966(18) 0.23577(16) 0.5063(3) 0.0174(8) Uani 1 1 d . . .
O2 O 0.37328(18) 0.24532(16) 0.4273(3) 0.0202(9) Uani 1 1 d . . .
O3 O 0.76006(19) 0.26128(16) 0.4348(3) 0.0203(9) Uani 1 1 d . . .
O4 O 0.88461(18) 0.25784(16) 0.5164(3) 0.0199(9) Uani 1 1 d . . .
O5 O 0.9358(8) 0.4211(6) 0.1215(14) 0.047(4) Uani 0.35 1 d PD F 2
H5A H 0.9174 0.4363 0.1725 0.056 Uiso 0.35 1 calc PR F 2
O5' O 0.8206(7) 0.5500(6) 0.4446(8) 0.107(4) Uani 0.65 1 d PDU G 1
H5' H 0.8430 0.5209 0.4495 0.128 Uiso 0.65 1 calc PR G 1
N1 N 0.3789(2) 0.13437(19) 0.4161(3) 0.0160(10) Uani 1 1 d . . .
N2 N 0.2897(2) 0.19003(19) 0.3153(3) 0.0155(10) Uani 1 1 d . . .
N3 N 0.3424(2) 0.18653(19) 0.6115(3) 0.0167(10) Uani 1 1 d . . .
N4 N 0.2618(2) 0.12497(19) 0.5024(3) 0.0168(10) Uani 1 1 d . . .
N5 N 0.7998(2) 0.3108(2) 0.6265(3) 0.0187(10) Uani 1 1 d . . .
N6 N 0.8853(2) 0.36854(19) 0.5277(3) 0.0171(10) Uani 1 1 d . . .
N7 N 0.8480(2) 0.31494(19) 0.3306(3) 0.0161(10) Uani 1 1 d . . .
N8 N 0.7655(2) 0.3732(2) 0.4364(4) 0.0191(10) Uani 1 1 d . . .
N9 N 0.8901(3) 0.4779(2) 0.2813(5) 0.0401(15) Uani 1 1 d D . .
N10 N 0.6153(6) 0.5082(6) 0.8579(14) 0.085(5) Uani 0.50 1 d PDU D 1
N10' N 0.4339(9) 0.0928(6) 0.7389(10) 0.094(6) Uani 0.50 1 d PDU E 2
C1 C 0.2072(3) 0.2611(2) 0.4447(4) 0.0166(12) Uani 1 1 d . . .
C2 C 0.1600(3) 0.2935(3) 0.4933(4) 0.0219(13) Uani 1 1 d . . .
H2 H 0.1588 0.2944 0.5683 0.026 Uiso 1 1 calc R . .
C3 C 0.1154(3) 0.3241(3) 0.4364(4) 0.0223(13) Uani 1 1 d . . .
H3 H 0.0840 0.3453 0.4720 0.027 Uiso 1 1 calc R . .
C4 C 0.1165(3) 0.3238(2) 0.3262(4) 0.0169(12) Uani 1 1 d . . .
C5 C 0.1608(3) 0.2911(2) 0.2750(4) 0.0174(12) Uani 1 1 d . . .
H5 H 0.1607 0.2901 0.2000 0.021 Uiso 1 1 calc R . .
C6 C 0.2062(3) 0.2593(2) 0.3325(4) 0.0164(12) Uani 1 1 d . . .
C7 C 0.2481(3) 0.2239(2) 0.2745(4) 0.0173(12) Uani 1 1 d . . .
H7 H 0.2450 0.2255 0.1995 0.021 Uiso 1 1 calc R . .
C8 C 0.3275(3) 0.1545(2) 0.2513(4) 0.0180(12) Uani 1 1 d . . .
C9 C 0.3222(3) 0.1464(3) 0.1439(4) 0.0205(13) Uani 1 1 d . . .
H9 H 0.2899 0.1653 0.1037 0.025 Uiso 1 1 calc R . .
C10 C 0.3644(3) 0.1103(3) 0.0944(5) 0.0246(14) Uani 1 1 d . . .
H10 H 0.3607 0.1056 0.0200 0.029 Uiso 1 1 calc R . .
C11 C 0.4104(3) 0.0817(3) 0.1479(4) 0.0220(13) Uani 1 1 d . . .
H11 H 0.4381 0.0571 0.1114 0.026 Uiso 1 1 calc R . .
C12 C 0.4172(3) 0.0883(2) 0.2587(4) 0.0210(13) Uani 1 1 d . . .
C13 C 0.4639(3) 0.0606(3) 0.3227(5) 0.0257(14) Uani 1 1 d . . .
H13 H 0.4933 0.0354 0.2916 0.031 Uiso 1 1 calc R . .
C14 C 0.4665(3) 0.0702(3) 0.4298(5) 0.0293(15) Uani 1 1 d . . .
H14 H 0.4975 0.0518 0.4735 0.035 Uiso 1 1 calc R . .
C15 C 0.4227(3) 0.1074(2) 0.4732(4) 0.0207(13) Uani 1 1 d . . .
H15 H 0.4245 0.1137 0.5473 0.025 Uiso 1 1 calc R . .
C16 C 0.3755(3) 0.1250(2) 0.3094(4) 0.0163(12) Uani 1 1 d . . .
C17 C 0.4204(3) 0.2651(2) 0.4888(4) 0.0181(12) Uani 1 1 d . . .
C18 C 0.4649(3) 0.3001(3) 0.4413(4) 0.0239(14) Uani 1 1 d . . .
H18 H 0.4615 0.3067 0.3674 0.029 Uiso 1 1 calc R . .
C19 C 0.5139(3) 0.3254(3) 0.4989(4) 0.0246(14) Uani 1 1 d . . .
H19 H 0.5435 0.3492 0.4650 0.030 Uiso 1 1 calc R . .
C20 C 0.5195(3) 0.3155(2) 0.6086(4) 0.0188(12) Uani 1 1 d . . .
C21 C 0.4775(3) 0.2804(2) 0.6564(4) 0.0184(12) Uani 1 1 d . . .
H21 H 0.4819 0.2736 0.7302 0.022 Uiso 1 1 calc R . .
C22 C 0.4276(3) 0.2539(2) 0.5982(4) 0.0163(12) Uani 1 1 d . . .
C23 C 0.3866(3) 0.2173(2) 0.6544(4) 0.0156(11) Uani 1 1 d . . .
H23 H 0.3922 0.2153 0.7290 0.019 Uiso 1 1 calc R . .
C24 C 0.3050(3) 0.1485(2) 0.6712(4) 0.0167(12) Uani 1 1 d . . .
C25 C 0.3066(3) 0.1415(3) 0.7802(4) 0.0231(13) Uani 1 1 d . . .
H25 H 0.3343 0.1636 0.8235 0.028 Uiso 1 1 calc R . .
C26 C 0.2667(3) 0.1012(3) 0.8254(5) 0.0271(14) Uani 1 1 d . . .
H26 H 0.2680 0.0965 0.8999 0.033 Uiso 1 1 calc R . .
C27 C 0.2265(3) 0.0687(3) 0.7668(5) 0.0277(15) Uani 1 1 d . . .
H27 H 0.2003 0.0419 0.8004 0.033 Uiso 1 1 calc R . .
C28 C 0.2233(3) 0.0746(2) 0.6554(5) 0.0222(13) Uani 1 1 d . . .
C29 C 0.1841(3) 0.0424(3) 0.5860(5) 0.0287(15) Uani 1 1 d . . .
H29 H 0.1570 0.0144 0.6136 0.034 Uiso 1 1 calc R . .
C30 C 0.1852(3) 0.0515(3) 0.4799(5) 0.0251(14) Uani 1 1 d . . .
H30 H 0.1592 0.0299 0.4331 0.030 Uiso 1 1 calc R . .
C31 C 0.2249(3) 0.0931(2) 0.4412(5) 0.0225(13) Uani 1 1 d . . .
H31 H 0.2257 0.0989 0.3669 0.027 Uiso 1 1 calc R . .
C32 C 0.2628(3) 0.1156(2) 0.6099(4) 0.0161(12) Uani 1 1 d . . .
C33 C 0.7175(3) 0.2370(2) 0.4954(4) 0.0201(12) Uani 1 1 d . . .
C34 C 0.6717(3) 0.2025(3) 0.4461(5) 0.0272(14) Uani 1 1 d . . .
H34 H 0.6718 0.1991 0.3714 0.033 Uiso 1 1 calc R . .
C35 C 0.6268(3) 0.1736(3) 0.5014(5) 0.0287(15) Uani 1 1 d . . .
H35 H 0.5968 0.1503 0.4651 0.034 Uiso 1 1 calc R . .
C36 C 0.6252(3) 0.1785(2) 0.6120(4) 0.0207(13) Uani 1 1 d . . .
C37 C 0.6690(3) 0.2124(2) 0.6633(4) 0.0205(13) Uani 1 1 d . . .
H37 H 0.6677 0.2158 0.7380 0.025 Uiso 1 1 calc R . .
C38 C 0.7157(3) 0.2423(2) 0.6072(4) 0.0191(12) Uani 1 1 d . . .
C39 C 0.7574(3) 0.2781(2) 0.6664(4) 0.0187(12) Uani 1 1 d . . .
H39 H 0.7536 0.2780 0.7411 0.022 Uiso 1 1 calc R . .
C40 C 0.8378(3) 0.3473(2) 0.6910(4) 0.0181(12) Uani 1 1 d . . .
C41 C 0.8348(3) 0.3543(3) 0.7987(4) 0.0235(13) Uani 1 1 d . . .
H41 H 0.8043 0.3338 0.8379 0.028 Uiso 1 1 calc R . .
C42 C 0.8762(3) 0.3915(3) 0.8506(4) 0.0227(13) Uani 1 1 d . . .
H42 H 0.8731 0.3961 0.9248 0.027 Uiso 1 1 calc R . .
C43 C 0.9205(3) 0.4209(3) 0.7979(4) 0.0244(14) Uani 1 1 d . . .
H43 H 0.9486 0.4454 0.8354 0.029 Uiso 1 1 calc R . .
C44 C 0.9255(3) 0.4153(2) 0.6851(4) 0.0203(12) Uani 1 1 d . . .
C45 C 0.9711(3) 0.4429(3) 0.6232(4) 0.0232(13) Uani 1 1 d . . .
H45 H 1.0006 0.4683 0.6550 0.028 Uiso 1 1 calc R . .
C46 C 0.9724(3) 0.4327(3) 0.5173(5) 0.0240(13) Uani 1 1 d . . .
H46 H 1.0030 0.4510 0.4747 0.029 Uiso 1 1 calc R . .
C47 C 0.9288(3) 0.3955(3) 0.4717(4) 0.0216(13) Uani 1 1 d . . .
H47 H 0.9302 0.3890 0.3977 0.026 Uiso 1 1 calc R . .
C48 C 0.8834(3) 0.3779(2) 0.6342(4) 0.0172(12) Uani 1 1 d . . .
C49 C 0.9297(3) 0.2373(2) 0.4552(4) 0.0188(12) Uani 1 1 d . . .
C50 C 0.9756(3) 0.2019(3) 0.5019(4) 0.0226(13) Uani 1 1 d . . .
H50 H 0.9743 0.1954 0.5758 0.027 Uiso 1 1 calc R . .
C51 C 1.0226(3) 0.1763(3) 0.4443(4) 0.0218(13) Uani 1 1 d . . .
H51 H 1.0528 0.1523 0.4786 0.026 Uiso 1 1 calc R . .
C52 C 1.0260(3) 0.1854(2) 0.3356(4) 0.0178(12) Uani 1 1 d . . .
C53 C 0.9829(3) 0.2208(2) 0.2873(4) 0.0198(12) Uani 1 1 d . . .
H53 H 0.9855 0.2272 0.2134 0.024 Uiso 1 1 calc R . .
C54 C 0.9346(3) 0.2480(2) 0.3453(4) 0.0159(12) Uani 1 1 d . . .
C55 C 0.8921(3) 0.2848(2) 0.2885(4) 0.0179(12) Uani 1 1 d . . .
H55 H 0.8968 0.2872 0.2141 0.022 Uiso 1 1 calc R . .
C56 C 0.8101(3) 0.3526(2) 0.2692(4) 0.0196(12) Uani 1 1 d . . .
C57 C 0.8125(3) 0.3616(2) 0.1610(4) 0.0203(12) Uani 1 1 d . . .
H57 H 0.8414 0.3409 0.1192 0.024 Uiso 1 1 calc R . .
C58 C 0.7722(3) 0.4013(3) 0.1141(5) 0.0257(14) Uani 1 1 d . . .
H58 H 0.7738 0.4067 0.0399 0.031 Uiso 1 1 calc R . .
C59 C 0.7305(3) 0.4326(3) 0.1708(5) 0.0255(14) Uani 1 1 d . . .
H59 H 0.7041 0.4596 0.1363 0.031 Uiso 1 1 calc R . .
C60 C 0.7269(3) 0.4246(2) 0.2820(5) 0.0216(13) Uani 1 1 d . . .
C61 C 0.6847(3) 0.4541(3) 0.3477(5) 0.0297(15) Uani 1 1 d . . .
H61 H 0.6570 0.4820 0.3191 0.036 Uiso 1 1 calc R . .
C62 C 0.6844(3) 0.4419(3) 0.4530(5) 0.0298(15) Uani 1 1 d . . .
H62 H 0.6555 0.4609 0.4978 0.036 Uiso 1 1 calc R . .
C63 C 0.7260(3) 0.4017(3) 0.4958(5) 0.0227(13) Uani 1 1 d . . .
H63 H 0.7259 0.3948 0.5697 0.027 Uiso 1 1 calc R . .
C64 C 0.7665(3) 0.3845(2) 0.3287(4) 0.0173(12) Uani 1 1 d . . .
C65 C 0.9181(4) 0.4659(4) 0.2002(7) 0.0198(19) Uani 0.65 1 d P B 1
C65' C 0.8575(6) 0.5104(5) 0.3234(12) 0.029(4) Uani 0.35 1 d PD C 2
C66 C 0.6554(6) 0.4749(7) 0.8449(15) 0.048(4) Uani 0.50 1 d PDU D 1
C66' C 0.4417(5) 0.0621(4) 0.8097(7) 0.020(2) Uani 0.50 1 d PDU E 2
C67 C 0.9694(12) 0.4620(10) 0.0632(19) 0.029(7) Uani 0.35 1 d PDU F 2
H67A H 0.9960 0.4845 0.1117 0.044 Uiso 0.35 1 calc PR F 2
H67B H 0.9384 0.4862 0.0260 0.044 Uiso 0.35 1 calc PR F 2
H67C H 0.9968 0.4436 0.0118 0.044 Uiso 0.35 1 calc PR F 2
C67' C 0.8014(5) 0.5582(5) 0.3374(8) 0.026(3) Uani 0.65 1 d PDU G 1
H67D H 0.7547 0.5540 0.3305 0.039 Uiso 0.65 1 calc PR G 1
H67E H 0.8224 0.5306 0.2929 0.039 Uiso 0.65 1 calc PR G 1
H67F H 0.8137 0.5958 0.3151 0.039 Uiso 0.65 1 calc PR G 1
C68 C 0.6542(9) 0.4851(8) 0.8074(5) 0.061(6) Uani 0.50 1 d PDU A 2
H69A H 0.6165 0.4760 0.7618 0.074 Uiso 0.50 1 calc PR A 2
H69B H 0.6718 0.5216 0.7862 0.074 Uiso 0.50 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C4 2.094(5) . ?
I2 C20 2.094(5) . ?
I3 C36 2.093(6) . ?
I4 C52 2.086(6) . ?
Fe1 O1 1.870(4) . ?
Fe1 O2 1.877(4) . ?
Fe1 N3 1.944(4) . ?
Fe1 N2 1.944(4) . ?
Fe1 N1 1.953(5) . ?
Fe1 N4 1.963(5) . ?
Fe2 O3 1.875(4) . ?
Fe2 O4 1.877(4) . ?
Fe2 N5 1.948(5) . ?
Fe2 N7 1.948(4) . ?
Fe2 N6 1.959(5) . ?
Fe2 N8 1.967(5) . ?
Cl1 C68 1.7197(10) . ?
Cl2 C68 1.7199(10) . ?
S1 C65 1.612(10) . ?
S1' C65' 1.6502(10) . ?
S2 C66 1.6500(10) . ?
S2' C66' 1.6485(10) . ?
O1 C1 1.316(6) . ?
O2 C17 1.328(6) . ?
O3 C33 1.319(7) . ?
O4 C49 1.323(7) . ?
O5 C67 1.4201(10) . ?
O5 H5A 0.8400 . ?
O5' C67' 1.4203(10) . ?
O5' H5' 0.8400 . ?
N1 C15 1.321(7) . ?
N1 C16 1.370(6) . ?
N2 C7 1.287(7) . ?
N2 C8 1.424(7) . ?
N3 C23 1.291(7) . ?
N3 C24 1.425(7) . ?
N4 C31 1.324(7) . ?
N4 C32 1.378(6) . ?
N5 C39 1.293(7) . ?
N5 C40 1.426(7) . ?
N6 C47 1.330(7) . ?
N6 C48 1.367(7) . ?
N7 C55 1.293(7) . ?
N7 C56 1.420(7) . ?
N8 C63 1.316(7) . ?
N8 C64 1.389(7) . ?
N9 C65' 1.1704(10) . ?
N9 C65 1.224(10) . ?
N10 C66 1.1704(10) . ?
N10' C66' 1.1683(10) . ?
C1 C2 1.405(8) . ?
C1 C6 1.421(7) . ?
C2 C3 1.375(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(8) . ?
C5 C6 1.406(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.431(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(7) . ?
C8 C16 1.419(8) . ?
C9 C10 1.392(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.349(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.415(7) . ?
C11 H11 0.9500 . ?
C12 C16 1.401(8) . ?
C12 C13 1.419(8) . ?
C13 C14 1.375(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.397(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.396(8) . ?
C17 C22 1.416(7) . ?
C18 C19 1.382(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.411(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.364(8) . ?
C21 C22 1.413(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.426(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(8) . ?
C24 C32 1.404(7) . ?
C25 C26 1.404(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.355(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.416(8) . ?
C27 H27 0.9500 . ?
C28 C32 1.412(8) . ?
C28 C29 1.417(8) . ?
C29 C30 1.361(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(8) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C33 C34 1.400(8) . ?
C33 C38 1.423(7) . ?
C34 C35 1.367(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.407(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.376(8) . ?
C37 C38 1.411(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.423(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.376(7) . ?
C40 C48 1.409(8) . ?
C41 C42 1.396(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.349(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.440(8) . ?
C43 H43 0.9500 . ?
C44 C48 1.403(8) . ?
C44 C45 1.407(8) . ?
C45 C46 1.364(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.391(8) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C49 C50 1.401(8) . ?
C49 C54 1.420(7) . ?
C50 C51 1.376(8) . ?
C50 H50 0.9500 . ?
C51 C52 1.397(7) . ?
C51 H51 0.9500 . ?
C52 C53 1.371(8) . ?
C53 C54 1.417(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.432(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.388(7) . ?
C56 C64 1.417(8) . ?
C57 C58 1.394(8) . ?
C57 H57 0.9500 . ?
C58 C59 1.362(9) . ?
C58 H58 0.9500 . ?
C59 C60 1.425(8) . ?
C59 H59 0.9500 . ?
C60 C64 1.390(8) . ?
C60 C61 1.413(8) . ?
C61 C62 1.365(8) . ?
C61 H61 0.9500 . ?
C62 C63 1.399(8) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C67' H67D 0.9800 . ?
C67' H67E 0.9800 . ?
C67' H67F 0.9800 . ?
C68 H69A 0.9900 . ?
C68 H69B 0.9900 . ?

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
O1 Fe1 O2 96.20(18) . . ?
O1 Fe1 N3 86.24(17) . . ?
O2 Fe1 N3 94.67(17) . . ?
O1 Fe1 N2 94.30(17) . . ?
O2 Fe1 N2 85.35(17) . . ?
N3 Fe1 N2 179.5(2) . . ?
O1 Fe1 N1 174.97(18) . . ?
O2 Fe1 N1 88.33(18) . . ?
N3 Fe1 N1 95.60(19) . . ?
N2 Fe1 N1 83.85(19) . . ?
O1 Fe1 N4 88.31(18) . . ?
O2 Fe1 N4 175.17(18) . . ?
N3 Fe1 N4 83.86(18) . . ?
N2 Fe1 N4 96.07(18) . . ?
N1 Fe1 N4 87.24(19) . . ?
O3 Fe2 O4 95.37(18) . . ?
O3 Fe2 N5 94.67(18) . . ?
O4 Fe2 N5 85.72(18) . . ?
O3 Fe2 N7 86.30(17) . . ?
O4 Fe2 N7 94.70(18) . . ?
N5 Fe2 N7 178.9(2) . . ?
O3 Fe2 N6 176.07(19) . . ?
O4 Fe2 N6 87.79(18) . . ?
N5 Fe2 N6 83.22(19) . . ?
N7 Fe2 N6 95.79(19) . . ?
O3 Fe2 N8 88.77(18) . . ?
O4 Fe2 N8 175.34(19) . . ?
N5 Fe2 N8 96.1(2) . . ?
N7 Fe2 N8 83.42(19) . . ?
N6 Fe2 N8 88.17(19) . . ?
C1 O1 Fe1 126.7(3) . . ?
C17 O2 Fe1 125.8(3) . . ?
C33 O3 Fe2 126.5(3) . . ?
C49 O4 Fe2 126.4(3) . . ?
C67 O5 H5A 109.5 . . ?
C15 N1 C16 118.7(5) . . ?
C15 N1 Fe1 128.3(4) . . ?
C16 N1 Fe1 112.9(3) . . ?
C7 N2 C8 121.7(5) . . ?
C7 N2 Fe1 124.9(4) . . ?
C8 N2 Fe1 113.0(3) . . ?
C23 N3 C24 122.3(4) . . ?
C23 N3 Fe1 125.4(4) . . ?
C24 N3 Fe1 112.2(3) . . ?
C31 N4 C32 118.8(5) . . ?
C31 N4 Fe1 129.1(4) . . ?
C32 N4 Fe1 112.1(3) . . ?
C39 N5 C40 121.7(5) . . ?
C39 N5 Fe2 125.1(4) . . ?
C40 N5 Fe2 113.1(4) . . ?
C47 N6 C48 118.6(5) . . ?
C47 N6 Fe2 128.0(4) . . ?
C48 N6 Fe2 113.4(4) . . ?
C55 N7 C56 121.5(5) . . ?
C55 N7 Fe2 125.2(4) . . ?
C56 N7 Fe2 113.3(4) . . ?
C63 N8 C64 118.7(5) . . ?
C63 N8 Fe2 128.3(4) . . ?
C64 N8 Fe2 112.9(4) . . ?
C65' N9 C65 145.9(11) . . ?
O1 C1 C2 117.7(5) . . ?
O1 C1 C6 125.1(5) . . ?
C2 C1 C6 117.2(5) . . ?
C3 C2 C1 122.5(5) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C2 C3 C4 119.9(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 I1 120.7(4) . . ?
C3 C4 I1 119.7(4) . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 C7 117.8(5) . . ?
C1 C6 C7 122.3(5) . . ?
N2 C7 C6 125.5(5) . . ?
N2 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
C9 C8 C16 118.9(5) . . ?
C9 C8 N2 127.7(5) . . ?
C16 C8 N2 113.4(5) . . ?
C8 C9 C10 119.6(5) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 122.6(5) . . ?
C11 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C16 C12 C11 118.2(5) . . ?
C16 C12 C13 117.2(5) . . ?
C11 C12 C13 124.6(6) . . ?
C14 C13 C12 119.8(6) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C13 C14 C15 118.8(6) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
N1 C15 C14 123.2(5) . . ?
N1 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N1 C16 C12 122.3(5) . . ?
N1 C16 C8 116.8(5) . . ?
C12 C16 C8 120.9(5) . . ?
O2 C17 C18 116.9(5) . . ?
O2 C17 C22 124.7(5) . . ?
C18 C17 C22 118.4(5) . . ?
C19 C18 C17 121.7(5) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 119.5(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C21 C20 C19 119.9(5) . . ?
C21 C20 I2 122.1(4) . . ?
C19 C20 I2 118.0(4) . . ?
C20 C21 C22 121.2(5) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C17 119.2(5) . . ?
C21 C22 C23 117.3(5) . . ?
C17 C22 C23 123.4(5) . . ?
N3 C23 C22 124.9(5) . . ?
N3 C23 H23 117.6 . . ?
C22 C23 H23 117.6 . . ?
C25 C24 C32 118.9(5) . . ?
C25 C24 N3 127.0(5) . . ?
C32 C24 N3 114.1(5) . . ?
C24 C25 C26 119.0(5) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 122.5(6) . . ?
C27 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C26 C27 C28 120.2(6) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C32 C28 C27 117.4(5) . . ?
C32 C28 C29 117.4(5) . . ?
C27 C28 C29 125.2(5) . . ?
C30 C29 C28 120.3(6) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 118.9(5) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
N4 C31 C30 123.3(5) . . ?
N4 C31 H31 118.3 . . ?
C30 C31 H31 118.3 . . ?
N4 C32 C24 116.9(5) . . ?
N4 C32 C28 121.2(5) . . ?
C24 C32 C28 122.0(5) . . ?
O3 C33 C34 117.5(5) . . ?
O3 C33 C38 124.7(5) . . ?
C34 C33 C38 117.8(5) . . ?
C35 C34 C33 122.6(5) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C34 C35 C36 119.8(6) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 119.4(5) . . ?
C37 C36 I3 121.9(4) . . ?
C35 C36 I3 118.7(4) . . ?
C36 C37 C38 121.4(5) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
C37 C38 C33 119.1(5) . . ?
C37 C38 C39 117.5(5) . . ?
C33 C38 C39 123.4(5) . . ?
N5 C39 C38 125.1(5) . . ?
N5 C39 H39 117.4 . . ?
C38 C39 H39 117.4 . . ?
C41 C40 C48 119.1(5) . . ?
C41 C40 N5 127.4(5) . . ?
C48 C40 N5 113.6(5) . . ?
C40 C41 C42 120.3(6) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C43 C42 C41 121.6(5) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C42 C43 C44 120.3(6) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C48 C44 C45 117.9(5) . . ?
C48 C44 C43 117.3(5) . . ?
C45 C44 C43 124.7(5) . . ?
C46 C45 C44 119.3(6) . . ?
C46 C45 H45 120.4 . . ?
C44 C45 H45 120.4 . . ?
C45 C46 C47 119.8(6) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
N6 C47 C46 122.5(5) . . ?
N6 C47 H47 118.8 . . ?
C46 C47 H47 118.8 . . ?
N6 C48 C44 121.9(5) . . ?
N6 C48 C40 116.7(5) . . ?
C44 C48 C40 121.4(5) . . ?
O4 C49 C50 117.7(5) . . ?
O4 C49 C54 124.8(5) . . ?
C50 C49 C54 117.5(5) . . ?
C51 C50 C49 122.3(5) . . ?
C51 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C50 C51 C52 120.1(5) . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C53 C52 C51 119.5(5) . . ?
C53 C52 I4 121.6(4) . . ?
C51 C52 I4 118.9(4) . . ?
C52 C53 C54 121.3(5) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
C53 C54 C49 119.3(5) . . ?
C53 C54 C55 117.4(5) . . ?
C49 C54 C55 123.2(5) . . ?
N7 C55 C54 125.1(5) . . ?
N7 C55 H55 117.5 . . ?
C54 C55 H55 117.5 . . ?
C57 C56 C64 118.4(5) . . ?
C57 C56 N7 127.5(5) . . ?
C64 C56 N7 114.1(5) . . ?
C56 C57 C58 119.6(6) . . ?
C56 C57 H57 120.2 . . ?
C58 C57 H57 120.2 . . ?
C59 C58 C57 122.5(6) . . ?
C59 C58 H58 118.8 . . ?
C57 C58 H58 118.8 . . ?
C58 C59 C60 119.5(6) . . ?
C58 C59 H59 120.3 . . ?
C60 C59 H59 120.3 . . ?
C64 C60 C61 117.8(5) . . ?
C64 C60 C59 118.1(5) . . ?
C61 C60 C59 124.0(6) . . ?
C62 C61 C60 118.8(6) . . ?
C62 C61 H61 120.6 . . ?
C60 C61 H61 120.6 . . ?
C61 C62 C63 120.7(6) . . ?
C61 C62 H62 119.6 . . ?
C63 C62 H62 119.6 . . ?
N8 C63 C62 121.7(6) . . ?
N8 C63 H63 119.1 . . ?
C62 C63 H63 119.1 . . ?
N8 C64 C60 122.1(5) . . ?
N8 C64 C56 116.0(5) . . ?
C60 C64 C56 121.9(5) . . ?
N9 C65 S1 177.9(8) . . ?
N9 C65' S1' 176.4(15) . . ?
N10 C66 S2 168(2) . . ?
N10' C66' S2' 175.2(14) . . ?
O5 C67 H67A 109.5 . . ?
O5 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
O5 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
Cl1 C68 Cl2 101.6(8) . . ?
Cl1 C68 H69A 111.4 . . ?
Cl2 C68 H69A 111.4 . . ?
Cl1 C68 H69B 111.4 . . ?
Cl2 C68 H69B 111.4 . . ?
H69A C68 H69B 109.3 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.349
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.156
_database_code_depnum_ccdc_archive 'CCDC 994842'
