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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ws100c_a
_database_code_depnum_ccdc_archive 'CCDC 1529176'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H20 Fe I N6 O2 S'
_chemical_formula_weight         663.29

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   8.5990(17)
_cell_length_b                   19.287(4)
_cell_length_c                   15.871(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.59(3)
_cell_angle_gamma                90.00
_cell_volume                     2535.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'Thin Plate'
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9624
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
; 
As the crystal is reall tiny, the Rint is a bit high. The refinement parameters are then high resulting in alert B.
However, the atoms in the structure well behave. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 315r CCD'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28290
_diffrn_reflns_av_R_equivalents  0.1207
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         30.13
_reflns_number_total             7304
_reflns_number_gt                5723
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BluIce (McPhillips, 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. 
;

_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)+(0.1294P)²+63.7917P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7304
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.1290
_refine_ls_wR_factor_ref         0.3791
_refine_ls_wR_factor_gt          0.3696
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_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
I1 I -0.19403(12) 0.50783(5) 0.23774(7) 0.0531(3) Uani 1 1 d . . .
Fe1 Fe 0.47469(19) 0.24501(8) 0.37723(10) 0.0292(4) Uani 1 1 d . . .
S1 S 0.6075(4) 0.33661(15) 0.44719(18) 0.0347(6) Uani 1 1 d . . .
O2 O 0.3756(10) 0.1636(4) 0.3148(5) 0.0348(16) Uani 1 1 d . . .
N2 N 0.6728(11) 0.2181(5) 0.3424(6) 0.0307(17) Uani 1 1 d . . .
O1 O 0.2779(9) 0.2694(4) 0.4035(5) 0.0340(16) Uani 1 1 d . . .
N1 N 0.4269(10) 0.2953(5) 0.2672(5) 0.0273(16) Uani 1 1 d . . .
N3 N 0.5337(11) 0.2006(5) 0.4906(6) 0.0322(18) Uani 1 1 d . . .
N4 N 0.6328(12) 0.2321(5) 0.5647(6) 0.0339(19) Uani 1 1 d . . .
C16 C 0.6734(13) 0.2435(5) 0.2640(7) 0.0290(19) Uani 1 1 d . . .
C7 C 0.3078(13) 0.3383(6) 0.2408(7) 0.0300(19) Uani 1 1 d . . .
H7 H 0.2993 0.3618 0.1871 0.036 Uiso 1 1 calc R . .
C8 C 0.5420(12) 0.2844(5) 0.2199(6) 0.0279(18) Uani 1 1 d . . .
C13 C 0.9291(14) 0.1872(6) 0.2729(8) 0.035(2) Uani 1 1 d . . .
H13 H 1.0182 0.1773 0.2502 0.041 Uiso 1 1 calc R . .
C23 C 0.4715(14) 0.1426(6) 0.5066(8) 0.034(2) Uani 1 1 d . . .
H23 H 0.4988 0.1276 0.5658 0.040 Uiso 1 1 calc R . .
C15 C 0.7909(14) 0.1783(6) 0.3867(8) 0.036(2) Uani 1 1 d . . .
H15 H 0.7879 0.1607 0.4422 0.043 Uiso 1 1 calc R . .
C6 C 0.1899(13) 0.3530(6) 0.2852(7) 0.032(2) Uani 1 1 d . . .
C3 C -0.0580(15) 0.3879(7) 0.3623(9) 0.041(3) Uani 1 1 d . . .
H3 H -0.1432 0.3991 0.3876 0.049 Uiso 1 1 calc R . .
C24 C 0.6693(14) 0.2975(7) 0.5491(7) 0.037(2) Uani 1 1 d . . .
C12 C 0.8022(13) 0.2285(6) 0.2250(7) 0.032(2) Uani 1 1 d . . .
C17 C 0.3245(13) 0.1099(6) 0.3528(8) 0.034(2) Uani 1 1 d . . .
C14 C 0.9252(14) 0.1610(6) 0.3520(8) 0.036(2) Uani 1 1 d . . .
H14 H 1.0095 0.1318 0.3840 0.044 Uiso 1 1 calc R . .
N5 N 0.7632(14) 0.3354(6) 0.6158(7) 0.042(2) Uani 1 1 d . . .
H5A H 0.7991 0.3169 0.6681 0.050 Uiso 1 1 calc R . .
H5B H 0.7883 0.3785 0.6066 0.050 Uiso 1 1 calc R . .
C11 C 0.7934(14) 0.2570(7) 0.1428(8) 0.039(2) Uani 1 1 d . . .
H11 H 0.8799 0.2497 0.1172 0.047 Uiso 1 1 calc R . .
C9 C 0.5370(14) 0.3108(6) 0.1375(7) 0.035(2) Uani 1 1 d . . .
H9 H 0.4491 0.3391 0.1076 0.042 Uiso 1 1 calc R . .
C1 C 0.1784(12) 0.3173(6) 0.3641(7) 0.031(2) Uani 1 1 d . . .
C2 C 0.0497(16) 0.3362(7) 0.3987(8) 0.041(3) Uani 1 1 d . . .
H2 H 0.0368 0.3126 0.4489 0.049 Uiso 1 1 calc R . .
C5 C 0.0769(13) 0.4069(6) 0.2512(8) 0.035(2) Uani 1 1 d . . .
H5 H 0.0863 0.4314 0.2009 0.041 Uiso 1 1 calc R . .
C22 C 0.3650(13) 0.0985(6) 0.4434(8) 0.034(2) Uani 1 1 d . . .
C21 C 0.2936(18) 0.0421(7) 0.4755(10) 0.045(3) Uani 1 1 d . . .
H21 H 0.3223 0.0338 0.5368 0.054 Uiso 1 1 calc R . .
C4 C -0.0430(15) 0.4248(6) 0.2872(8) 0.038(2) Uani 1 1 d . . .
C20 C 0.182(2) -0.0023(7) 0.4203(12) 0.052(3) Uani 1 1 d . . .
H20 H 0.1280 -0.0377 0.4433 0.063 Uiso 1 1 calc R . .
C10 C 0.6622(17) 0.2954(7) 0.0984(9) 0.042(3) Uani 1 1 d . . .
H10 H 0.6558 0.3117 0.0410 0.051 Uiso 1 1 calc R . .
C18 C 0.2227(15) 0.0615(6) 0.2971(8) 0.038(2) Uani 1 1 d . . .
H18 H 0.2019 0.0660 0.2355 0.046 Uiso 1 1 calc R . .
C19 C 0.1532(17) 0.0078(6) 0.3317(10) 0.044(3) Uani 1 1 d . . .
H19 H 0.0832 -0.0233 0.2929 0.053 Uiso 1 1 calc R . .
N6 N 0.755(4) 0.4856(10) 0.5661(15) 0.143(14) Uani 1 1 d . . .
C26 C 0.673(3) 0.5783(12) 0.4424(13) 0.081(6) Uani 1 1 d . . .
H26A H 0.5819 0.5620 0.3951 0.122 Uiso 1 1 calc R . .
H26B H 0.7672 0.5854 0.4196 0.122 Uiso 1 1 calc R . .
H26C H 0.6444 0.6222 0.4655 0.122 Uiso 1 1 calc R . .
C25 C 0.712(5) 0.5259(12) 0.513(2) 0.131(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C4 2.079(12) . ?
Fe1 O1 1.907(8) . ?
Fe1 O2 1.929(8) . ?
Fe1 N1 1.942(9) . ?
Fe1 N3 1.933(10) . ?
Fe1 N2 1.996(9) . ?
Fe1 S1 2.231(3) . ?
S1 C24 1.734(12) . ?
O2 C17 1.331(14) . ?
N2 C15 1.316(14) . ?
N2 C16 1.339(14) . ?
O1 C1 1.299(14) . ?
N1 C7 1.296(14) . ?
N1 C8 1.410(13) . ?
N3 C23 1.294(15) . ?
N3 N4 1.393(13) . ?
N4 C24 1.339(16) . ?
C16 C8 1.402(14) . ?
C16 C12 1.436(15) . ?
C7 C6 1.410(15) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(14) . ?
C13 C14 1.362(16) . ?
C13 C12 1.400(15) . ?
C13 H13 0.9500 . ?
C23 C22 1.440(16) . ?
C23 H23 0.9500 . ?
C15 C14 1.445(17) . ?
C15 H15 0.9500 . ?
C6 C5 1.426(16) . ?
C6 C1 1.457(15) . ?
C3 C2 1.378(19) . ?
C3 C4 1.423(18) . ?
C3 H3 0.9500 . ?
C24 N5 1.359(15) . ?
C12 C11 1.399(17) . ?
C17 C22 1.404(16) . ?
C17 C18 1.415(17) . ?
C14 H14 0.9500 . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
C11 C10 1.375(18) . ?
C11 H11 0.9500 . ?
C9 C10 1.412(16) . ?
C9 H9 0.9500 . ?
C1 C2 1.409(16) . ?
C2 H2 0.9500 . ?
C5 C4 1.351(17) . ?
C5 H5 0.9500 . ?
C22 C21 1.410(17) . ?
C21 C20 1.40(2) . ?
C21 H21 0.9500 . ?
C20 C19 1.37(2) . ?
C20 H20 0.9500 . ?
C10 H10 0.9500 . ?
C18 C19 1.382(18) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
N6 C25 1.13(3) . ?
C26 C25 1.48(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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 91.0(4) . . ?
O1 Fe1 N1 95.0(4) . . ?
O2 Fe1 N1 89.2(4) . . ?
O1 Fe1 N3 86.1(4) . . ?
O2 Fe1 N3 95.0(4) . . ?
N1 Fe1 N3 175.6(4) . . ?
O1 Fe1 N2 176.5(4) . . ?
O2 Fe1 N2 86.4(4) . . ?
N1 Fe1 N2 82.6(4) . . ?
N3 Fe1 N2 96.4(4) . . ?
O1 Fe1 S1 93.5(3) . . ?
O2 Fe1 S1 175.5(3) . . ?
N1 Fe1 S1 90.5(3) . . ?
N3 Fe1 S1 85.2(3) . . ?
N2 Fe1 S1 89.1(3) . . ?
C24 S1 Fe1 96.2(4) . . ?
C17 O2 Fe1 123.7(7) . . ?
C15 N2 C16 121.0(10) . . ?
C15 N2 Fe1 126.7(8) . . ?
C16 N2 Fe1 112.3(7) . . ?
C1 O1 Fe1 125.4(7) . . ?
C7 N1 C8 122.0(9) . . ?
C7 N1 Fe1 124.6(7) . . ?
C8 N1 Fe1 113.3(7) . . ?
C23 N3 N4 113.7(10) . . ?
C23 N3 Fe1 123.2(8) . . ?
N4 N3 Fe1 122.7(7) . . ?
C24 N4 N3 112.0(9) . . ?
N2 C16 C8 117.8(9) . . ?
N2 C16 C12 121.6(10) . . ?
C8 C16 C12 120.7(9) . . ?
N1 C7 C6 125.3(10) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
C9 C8 C16 119.5(10) . . ?
C9 C8 N1 126.6(10) . . ?
C16 C8 N1 113.9(9) . . ?
C14 C13 C12 120.2(10) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
N3 C23 C22 126.3(10) . . ?
N3 C23 H23 116.8 . . ?
C22 C23 H23 116.8 . . ?
N2 C15 C14 120.8(11) . . ?
N2 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C7 C6 C5 117.8(10) . . ?
C7 C6 C1 124.0(10) . . ?
C5 C6 C1 118.2(10) . . ?
C2 C3 C4 120.7(11) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N4 C24 N5 118.9(10) . . ?
N4 C24 S1 123.6(9) . . ?
N5 C24 S1 117.5(10) . . ?
C11 C12 C13 124.7(10) . . ?
C11 C12 C16 117.9(10) . . ?
C13 C12 C16 117.4(10) . . ?
O2 C17 C22 124.4(11) . . ?
O2 C17 C18 117.0(10) . . ?
C22 C17 C18 118.6(11) . . ?
C13 C14 C15 119.1(10) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C10 C11 C12 121.5(11) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C8 C9 C10 120.1(11) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
O1 C1 C2 118.8(10) . . ?
O1 C1 C6 124.1(10) . . ?
C2 C1 C6 117.0(10) . . ?
C3 C2 C1 122.3(11) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C4 C5 C6 123.1(11) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C17 C22 C21 118.6(12) . . ?
C17 C22 C23 123.9(11) . . ?
C21 C22 C23 117.5(11) . . ?
C22 C21 C20 122.5(13) . . ?
C22 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
C5 C4 C3 118.6(11) . . ?
C5 C4 I1 120.5(9) . . ?
C3 C4 I1 120.9(9) . . ?
C19 C20 C21 117.1(13) . . ?
C19 C20 H20 121.4 . . ?
C21 C20 H20 121.4 . . ?
C11 C10 C9 120.3(11) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C19 C18 C17 120.5(12) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 122.4(13) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C25 C26 174(5) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         3.120
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.255
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_320K_a
_database_code_depnum_ccdc_archive 'CCDC 1529171'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(qsal-F)(thsa)]2.5MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H49 F2 Fe2 N15 O4 S2'
_chemical_formula_weight         1233.94

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.324(3)
_cell_length_b                   16.542(3)
_cell_length_c                   16.582(3)
_cell_angle_alpha                60.64(3)
_cell_angle_beta                 71.53(3)
_cell_angle_gamma                69.47(3)
_cell_volume                     2935.7(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    16589
_cell_measurement_theta_min      0.824
_cell_measurement_theta_max      31.849

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.631
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
;
This strcutures has been solved and refined by reasonable model.
The acetonitril molecules, N11 and N11', are disorder over two position and the total occupancy is one. 
Two molecules of MeCN are disorderd over 4 position (molecules of N15-N18). This has been treated the same as the structure at 100 K that shows no solvent loss after 
the warming after 320 K.
However, the anisotropy cannot applied on N11, N16, N17 and N18 molecules because of the thermal effect resulting in the weak diffractions and severly disorder of the solvents. 
;

_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1, Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61234
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_av_R_equivalents  0.1420
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.432
_diffrn_reflns_theta_max         31.849
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             16591
_reflns_number_gt                9261
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1153P)²]
 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         16591
_refine_ls_number_parameters     766
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.2132
_refine_ls_wR_factor_gt          0.1781
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.40633(3) 0.21298(3) 1.03065(3) 0.05191(13) Uani 1 1 d . . . . .
Fe2 Fe 0.47707(4) 0.75611(3) 0.42280(3) 0.05475(13) Uani 1 1 d . . . . .
S1 S 0.51064(7) 0.21232(5) 0.89541(5) 0.05891(19) Uani 1 1 d . . . . .
S2 S 0.35946(8) 0.75694(6) 0.56689(6) 0.0716(2) Uani 1 1 d . . . . .
O3 O 0.3688(2) 0.75110(17) 0.37037(17) 0.0747(6) Uani 1 1 d . . . . .
O4 O 0.5912(2) 0.72453(14) 0.33126(14) 0.0680(6) Uani 1 1 d . . . . .
O1 O 0.27924(18) 0.22112(14) 0.99741(14) 0.0643(5) Uani 1 1 d . . . . .
N9 N 0.5284(2) 0.61143(16) 0.51966(15) 0.0571(6) Uani 1 1 d . . . . .
O2 O 0.3261(2) 0.21401(16) 1.14816(14) 0.0696(6) Uani 1 1 d . . . . .
N1 N 0.4461(2) 0.07436(15) 1.09195(14) 0.0514(5) Uani 1 1 d . . . . .
N4 N 0.4273(2) 0.39599(16) 0.86779(15) 0.0584(6) Uani 1 1 d . . . . .
N2 N 0.5383(2) 0.19837(17) 1.07231(17) 0.0597(6) Uani 1 1 d . . . . .
N6 N 0.4137(2) 0.90897(17) 0.36197(16) 0.0629(6) Uani 1 1 d . . . . .
N3 N 0.3789(2) 0.35160(16) 0.96119(15) 0.0538(5) Uani 1 1 d . . . . .
N8 N 0.4852(2) 0.57684(17) 0.61544(16) 0.0664(7) Uani 1 1 d . . . . .
F1 F 0.0969(3) -0.0634(2) 1.0737(2) 0.1291(11) Uani 1 1 d . . . . .
N5 N 0.5380(2) 0.36924(17) 0.74192(16) 0.0651(7) Uani 1 1 d . . . . .
H5A H 0.5308 0.4297 0.7087 0.078 Uiso 1 1 calc R U . . .
H5B H 0.5776 0.3303 0.7175 0.078 Uiso 1 1 calc R U . . .
C7 C 0.3890(2) 0.01968(19) 1.10272(18) 0.0557(6) Uani 1 1 d . . . . .
H7 H 0.4149 -0.0458 1.1350 0.067 Uiso 1 1 calc R U . . .
C16 C 0.5947(2) 0.1052(2) 1.11265(18) 0.0544(6) Uani 1 1 d . . . . .
C9 C 0.6011(3) -0.0587(2) 1.16199(19) 0.0597(7) Uani 1 1 d . . . . .
H9 H 0.5720 -0.1057 1.1688 0.072 Uiso 1 1 calc R U . . .
C41 C 0.6585(3) 0.6466(2) 0.32591(19) 0.0572(6) Uani 1 1 d . . . . .
N7 N 0.5877(3) 0.8108(2) 0.44265(19) 0.0729(7) Uani 1 1 d . . . . .
C47 C 0.6009(3) 0.5456(2) 0.4968(2) 0.0616(7) Uani 1 1 d . . . . .
H47 H 0.6126 0.4842 0.5448 0.074 Uiso 1 1 calc R U . . .
N10 N 0.3656(3) 0.6118(2) 0.73291(18) 0.0837(9) Uani 1 1 d . . . . .
H10A H 0.3885 0.5543 0.7726 0.100 Uiso 1 1 calc R U . . .
H10B H 0.3152 0.6513 0.7520 0.100 Uiso 1 1 calc R U . . .
C12 C 0.6934(3) 0.0802(2) 1.1424(2) 0.0669(8) Uani 1 1 d . . . . .
C24 C 0.4874(3) 0.33568(19) 0.83159(18) 0.0543(6) Uani 1 1 d . . . . .
C10 C 0.7007(3) -0.0842(2) 1.1912(2) 0.0706(8) Uani 1 1 d . . . . .
H10 H 0.7367 -0.1483 1.2171 0.085 Uiso 1 1 calc R U . . .
C6 C 0.2891(3) 0.0514(2) 1.06922(19) 0.0584(7) Uani 1 1 d . . . . .
C22 C 0.2505(3) 0.3842(2) 1.0901(2) 0.0663(8) Uani 1 1 d . . . . .
C23 C 0.3117(3) 0.4103(2) 0.9951(2) 0.0617(7) Uani 1 1 d . . . . .
H23 H 0.3018 0.4751 0.9551 0.074 Uiso 1 1 calc R U . . .
C46 C 0.6646(3) 0.5575(2) 0.4056(2) 0.0629(7) Uani 1 1 d . . . . .
C2 C 0.1443(3) 0.1697(3) 0.9862(3) 0.0788(10) Uani 1 1 d . . . . .
H2 H 0.1121 0.2331 0.9512 0.095 Uiso 1 1 calc R U . . .
C32 C 0.4735(3) 0.9630(2) 0.36681(19) 0.0713(9) Uani 1 1 d . . . . .
C40 C 0.5661(4) 0.9073(3) 0.4111(2) 0.0757(10) Uani 1 1 d . . . . .
C8 C 0.5473(2) 0.03562(19) 1.12344(17) 0.0512(6) Uani 1 1 d . . . . .
C5 C 0.2383(3) -0.0186(2) 1.0865(3) 0.0736(9) Uani 1 1 d . . . . .
H5 H 0.2694 -0.0828 1.1196 0.088 Uiso 1 1 calc R U . . .
C31 C 0.3196(3) 0.9503(2) 0.3367(2) 0.0798(11) Uani 1 1 d . . . . .
H31 H 0.2962 1.0158 0.3190 0.096 Uiso 1 1 calc R U . . .
C17 C 0.2615(3) 0.2880(3) 1.1602(2) 0.0685(8) Uani 1 1 d . . . . .
C25 C 0.2743(3) 0.8092(3) 0.3516(2) 0.0765(10) Uani 1 1 d . . . . .
C1 C 0.2412(3) 0.1489(2) 1.0181(2) 0.0607(7) Uani 1 1 d . . . . .
C42 C 0.7237(3) 0.6497(3) 0.2409(2) 0.0719(9) Uani 1 1 d . . . . .
H42 H 0.7209 0.7079 0.1880 0.086 Uiso 1 1 calc R U . . .
F2 F -0.0252(3) 0.9838(4) 0.2814(3) 0.207(2) Uani 1 1 d . . . . .
C11 C 0.7453(3) -0.0177(3) 1.1824(2) 0.0739(9) Uani 1 1 d . . . . .
H11 H 0.8107 -0.0367 1.2030 0.089 Uiso 1 1 calc R U . . .
C48 C 0.4088(3) 0.6399(2) 0.6406(2) 0.0618(7) Uani 1 1 d . . . . .
C15 C 0.5761(3) 0.2667(2) 1.0649(3) 0.0767(9) Uani 1 1 d . . . . .
H15 H 0.5381 0.3299 1.0375 0.092 Uiso 1 1 calc R U . . .
C45 C 0.7354(3) 0.4755(3) 0.3957(3) 0.0831(10) Uani 1 1 d . . . . .
H45 H 0.7392 0.4165 0.4476 0.100 Uiso 1 1 calc R U . . .
C36 C 0.6334(5) 0.9515(4) 0.4201(3) 0.0966(14) Uani 1 1 d . . . . .
C21 C 0.1770(3) 0.4591(3) 1.1108(3) 0.0829(10) Uani 1 1 d . . . . .
H21 H 0.1708 0.5214 1.0642 0.099 Uiso 1 1 calc R U . . .
C30 C 0.2480(3) 0.9054(3) 0.3334(2) 0.0810(11) Uani 1 1 d . . . . .
C43 C 0.7923(3) 0.5684(3) 0.2332(3) 0.0867(11) Uani 1 1 d . . . . .
H43 H 0.8347 0.5722 0.1753 0.104 Uiso 1 1 calc R U . . .
C33 C 0.4520(5) 1.0598(3) 0.3330(3) 0.1025(16) Uani 1 1 d . . . . .
H33 H 0.3931 1.0984 0.3023 0.123 Uiso 1 1 calc R U . . .
C13 C 0.7308(3) 0.1550(3) 1.1337(3) 0.0872(11) Uani 1 1 d . . . . .
H13 H 0.7954 0.1417 1.1530 0.105 Uiso 1 1 calc R U . . .
C3 C 0.0966(3) 0.1005(3) 1.0049(3) 0.0868(11) Uani 1 1 d . . . . .
H3 H 0.0324 0.1161 0.9840 0.104 Uiso 1 1 calc R U . . .
C4 C 0.1456(3) 0.0069(3) 1.0557(3) 0.0852(11) Uani 1 1 d . . . . .
C20 C 0.1130(4) 0.4424(4) 1.1994(3) 0.1008(14) Uani 1 1 d . . . . .
H20 H 0.0649 0.4928 1.2124 0.121 Uiso 1 1 calc R U . . .
C18 C 0.1951(3) 0.2740(3) 1.2495(3) 0.0924(12) Uani 1 1 d . . . . .
H18 H 0.2000 0.2124 1.2975 0.111 Uiso 1 1 calc R U . . .
C14 C 0.6710(4) 0.2463(3) 1.0969(3) 0.0926(12) Uani 1 1 d . . . . .
H14 H 0.6936 0.2955 1.0930 0.111 Uiso 1 1 calc R U . . .
C29 C 0.1453(5) 0.9635(4) 0.3088(4) 0.1173(19) Uani 1 1 d . . . . .
H29 H 0.1288 1.0281 0.2946 0.141 Uiso 1 1 calc R U . . .
C39 C 0.6742(4) 0.7569(4) 0.4832(3) 0.1000(13) Uani 1 1 d . . . . .
H39 H 0.6892 0.6911 0.5040 0.120 Uiso 1 1 calc R U . . .
C37 C 0.7224(5) 0.8902(6) 0.4653(4) 0.130(2) Uani 1 1 d . . . . .
H37 H 0.7677 0.9157 0.4745 0.156 Uiso 1 1 calc R U . . .
C35 C 0.6062(7) 1.0486(5) 0.3890(4) 0.133(3) Uani 1 1 d . . . . .
H35 H 0.6471 1.0778 0.3982 0.160 Uiso 1 1 calc R U . . .
C44 C 0.7987(4) 0.4809(3) 0.3111(3) 0.0971(13) Uani 1 1 d . . . . .
H44 H 0.8457 0.4262 0.3058 0.117 Uiso 1 1 calc R U . . .
C26 C 0.1952(4) 0.7728(4) 0.3482(3) 0.1095(15) Uani 1 1 d . . . . .
H26 H 0.2091 0.7089 0.3611 0.131 Uiso 1 1 calc R U . . .
C34 C 0.5202(7) 1.1019(4) 0.3450(3) 0.132(3) Uani 1 1 d . . . . .
H34 H 0.5047 1.1679 0.3217 0.158 Uiso 1 1 calc R U . . .
C28 C 0.0734(5) 0.9288(6) 0.3057(5) 0.135(2) Uani 1 1 d . . . . .
C19 C 0.1223(4) 0.3506(4) 1.2671(3) 0.1072(15) Uani 1 1 d . . . . .
H19 H 0.0792 0.3388 1.3263 0.129 Uiso 1 1 calc R U . . .
C27 C 0.0927(5) 0.8370(6) 0.3245(4) 0.138(2) Uani 1 1 d . . . . .
H27 H 0.0393 0.8144 0.3222 0.165 Uiso 1 1 calc R U . . .
C38 C 0.7432(5) 0.7945(6) 0.4958(5) 0.139(2) Uani 1 1 d . . . . .
H38 H 0.8030 0.7544 0.5249 0.166 Uiso 1 1 calc R U . . .
C51 C -0.0738(4) 0.3211(5) 1.1229(5) 0.1202(19) Uani 1 1 d D . . . .
N12 N -0.1542(5) 0.3074(6) 1.1587(5) 0.190(3) Uani 1 1 d D . . . .
C52 C 0.0265(5) 0.3520(9) 1.0671(9) 0.252(6) Uani 1 1 d . . . . .
H52A H 0.0253 0.3765 1.0015 0.378 Uiso 1 1 calc R U . . .
H52B H 0.0880 0.2987 1.0837 0.378 Uiso 1 1 calc R U . . .
H52C H 0.0322 0.4011 1.0794 0.378 Uiso 1 1 calc R U . . .
N11' N -0.1046(7) 0.9205(6) 0.5476(6) 0.102(2) Uiso 0.5 1 d . . P A 6
C50' C -0.0252(7) 0.8817(6) 0.5611(6) 0.089(2) Uiso 0.5 1 d D . P A 6
C49' C 0.0758(10) 0.8162(10) 0.5693(12) 0.152(5) Uiso 0.5 1 d D . P A 6
H49A H 0.1008 0.8068 0.6223 0.228 Uiso 0.5 1 calc R U P A 6
H49B H 0.1274 0.8402 0.5131 0.228 Uiso 0.5 1 calc R U P A 6
H49C H 0.0686 0.7564 0.5782 0.228 Uiso 0.5 1 calc R U P A 6
C55 C 0.1425(6) -0.3040(5) 1.1299(6) 0.162(3) Uani 1 1 d D . . . .
C56 C 0.2287(7) -0.2916(6) 1.1506(6) 0.186(3) Uani 1 1 d . . . . .
H56A H 0.2023 -0.2414 1.1709 0.279 Uiso 1 1 calc R U . . .
H56B H 0.2838 -0.2750 1.0953 0.279 Uiso 1 1 calc R U . . .
H56C H 0.2593 -0.3498 1.1996 0.279 Uiso 1 1 calc R U . . .
N13 N 0.0746(7) -0.3132(6) 1.1100(8) 0.281(6) Uani 1 1 d D . . . .
C62 C 0.633(2) 0.5620(18) 0.7593(15) 0.163(9) Uiso 0.529(3) 1 d D . P B 3
H62A H 0.6690 0.5746 0.7921 0.245 Uiso 0.529(3) 1 calc R U P B 3
H62B H 0.5955 0.5123 0.8033 0.245 Uiso 0.529(3) 1 calc R U P B 3
H62C H 0.5810 0.6189 0.7281 0.245 Uiso 0.529(3) 1 calc R U P B 3
N16 N 0.7711(13) 0.5103(10) 0.6385(10) 0.185(5) Uiso 0.529(3) 1 d D . P B 3
C63 C 0.7100(12) 0.5328(11) 0.6922(11) 0.155(5) Uiso 0.529(3) 1 d D . P B 3
N15 N 0.4703(13) 0.4913(8) 1.0558(9) 0.164(5) Uani 0.507(3) 1 d D . P C 2
C61 C 0.4348(12) 0.4604(9) 1.1317(11) 0.131(5) Uani 0.507(3) 1 d D . P C 2
C60 C 0.395(3) 0.417(2) 1.2279(12) 0.211(13) Uani 0.507(3) 1 d D . P C 2
H60A H 0.4430 0.3563 1.2562 0.317 Uiso 0.507(3) 1 calc R U P C 2
H60B H 0.3237 0.4084 1.2371 0.317 Uiso 0.507(3) 1 calc R U P C 2
H60C H 0.3899 0.4572 1.2563 0.317 Uiso 0.507(3) 1 calc R U P C 2
N11 N -0.1331(17) 0.9950(13) 0.5035(13) 0.242(8) Uiso 0.5 1 d D . P D 1
C49 C -0.0759(12) 1.1520(11) 0.4084(11) 0.144(5) Uiso 0.5 1 d D . P D 1
H49D H -0.0025 1.1349 0.4180 0.216 Uiso 0.5 1 calc R U P D 1
H49E H -0.1199 1.1982 0.4323 0.216 Uiso 0.5 1 calc R U P D 1
H49F H -0.0763 1.1788 0.3423 0.216 Uiso 0.5 1 calc R U P D 1
C50 C -0.1183(19) 1.0697(14) 0.4560(15) 0.220(8) Uiso 0.5 1 d D . P D 1
C64 C -0.0612(14) 0.5740(13) 1.3863(12) 0.147(5) Uiso 0.461(3) 1 d D . P E 4
H64A H -0.0723 0.6218 1.3243 0.221 Uiso 0.461(3) 1 calc R U P E 4
H64B H -0.1010 0.5999 1.4312 0.221 Uiso 0.461(3) 1 calc R U P E 4
H64C H -0.0865 0.5200 1.4007 0.221 Uiso 0.461(3) 1 calc R U P E 4
N17 N 0.1411(18) 0.525(2) 1.382(2) 0.320(14) Uiso 0.461(3) 1 d D . P E 4
C67 C 0.967(5) 0.637(4) 0.428(3) 0.41(2) Uiso 0.503(3) 1 d D . P F 5
C66 C 0.934(2) 0.6460(19) 0.3500(18) 0.267(13) Uiso 0.503(3) 1 d D . P F 5
H66A H 0.9009 0.5950 0.3693 0.400 Uiso 0.503(3) 1 calc R U P F 5
H66B H 0.9966 0.6434 0.3017 0.400 Uiso 0.503(3) 1 calc R U P F 5
H66C H 0.8829 0.7061 0.3260 0.400 Uiso 0.503(3) 1 calc R U P F 5
C65 C 0.0508(17) 0.545(2) 1.390(3) 0.271(12) Uiso 0.461(3) 1 d D . P E 4
N18 N 0.980(4) 0.647(3) 0.485(3) 0.46(2) Uiso 0.503(3) 1 d D . P F 5


_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 O1 1.884(2) . ?
Fe1 O2 1.908(2) . ?
Fe1 N1 1.943(2) . ?
Fe1 N3 1.951(2) . ?
Fe1 N2 1.984(3) . ?
Fe1 S1 2.2361(11) . ?
Fe2 O4 1.910(2) . ?
Fe2 O3 1.948(2) . ?
Fe2 N9 2.134(2) . ?
Fe2 N7 2.152(3) . ?
Fe2 N6 2.160(3) . ?
Fe2 S2 2.4103(13) . ?
S1 C24 1.740(3) . ?
S2 C48 1.724(3) . ?
O3 C25 1.309(4) . ?
O4 C41 1.313(4) . ?
O1 C1 1.310(4) . ?
N9 C47 1.303(4) . ?
N9 N8 1.394(3) . ?
O2 C17 1.293(4) . ?
N1 C7 1.292(4) . ?
N1 C8 1.419(4) . ?
N4 C24 1.311(4) . ?
N4 N3 1.392(3) . ?
N2 C15 1.331(4) . ?
N2 C16 1.371(4) . ?
N6 C31 1.291(5) . ?
N6 C32 1.430(4) . ?
N3 C23 1.292(4) . ?
N8 C48 1.308(4) . ?
F1 C4 1.388(4) . ?
N5 C24 1.338(3) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C7 C6 1.431(4) . ?
C7 H7 0.9300 . ?
C16 C12 1.405(4) . ?
C16 C8 1.412(4) . ?
C9 C8 1.373(4) . ?
C9 C10 1.410(4) . ?
C9 H9 0.9300 . ?
C41 C42 1.390(4) . ?
C41 C46 1.415(4) . ?
N7 C39 1.325(5) . ?
N7 C40 1.363(4) . ?
C47 C46 1.434(4) . ?
C47 H47 0.9300 . ?
N10 C48 1.350(4) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
C12 C11 1.412(5) . ?
C12 C13 1.418(5) . ?
C10 C11 1.352(5) . ?
C10 H10 0.9300 . ?
C6 C5 1.406(4) . ?
C6 C1 1.417(4) . ?
C22 C21 1.403(5) . ?
C22 C17 1.427(5) . ?
C22 C23 1.448(4) . ?
C23 H23 0.9300 . ?
C46 C45 1.407(5) . ?
C2 C3 1.359(5) . ?
C2 C1 1.417(5) . ?
C2 H2 0.9300 . ?
C32 C33 1.365(5) . ?
C32 C40 1.424(6) . ?
C40 C36 1.419(5) . ?
C5 C4 1.338(5) . ?
C5 H5 0.9300 . ?
C31 C30 1.426(6) . ?
C31 H31 0.9300 . ?
C17 C18 1.417(5) . ?
C25 C30 1.398(5) . ?
C25 C26 1.411(6) . ?
C42 C43 1.375(5) . ?
C42 H42 0.9300 . ?
F2 C28 1.362(6) . ?
C11 H11 0.9300 . ?
C15 C14 1.394(5) . ?
C15 H15 0.9300 . ?
C45 C44 1.366(6) . ?
C45 H45 0.9300 . ?
C36 C35 1.369(7) . ?
C36 C37 1.403(8) . ?
C21 C20 1.391(6) . ?
C21 H21 0.9300 . ?
C30 C29 1.418(6) . ?
C43 C44 1.387(6) . ?
C43 H43 0.9300 . ?
C33 C34 1.428(8) . ?
C33 H33 0.9300 . ?
C13 C14 1.360(6) . ?
C13 H13 0.9300 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C20 C19 1.366(6) . ?
C20 H20 0.9300 . ?
C18 C19 1.398(6) . ?
C18 H18 0.9300 . ?
C14 H14 0.9300 . ?
C29 C28 1.303(9) . ?
C29 H29 0.9300 . ?
C39 C38 1.389(7) . ?
C39 H39 0.9300 . ?
C37 C38 1.356(9) . ?
C37 H37 0.9300 . ?
C35 C34 1.347(9) . ?
C35 H35 0.9300 . ?
C44 H44 0.9300 . ?
C26 C27 1.435(8) . ?
C26 H26 0.9300 . ?
C34 H34 0.9300 . ?
C28 C27 1.335(9) . ?
C19 H19 0.9300 . ?
C27 H27 0.9300 . ?
C38 H38 0.9300 . ?
C51 N12 1.090(7) . ?
C51 C52 1.461(10) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N11' C50' 1.056(10) . ?
C50' C49' 1.398(9) . ?
C49' H49A 0.9600 . ?
C49' H49B 0.9600 . ?
C49' H49C 0.9600 . ?
C55 N13 1.133(7) . ?
C55 C56 1.401(10) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C62 C63 1.409(10) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
N16 C63 1.116(9) . ?
N15 C61 1.109(9) . ?
N15 N15 1.69(3) 2_667 ?
C61 C60 1.396(10) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N11 C50 1.142(10) . ?
C49 C50 1.414(9) . ?
C49 H49D 0.9600 . ?
C49 H49E 0.9600 . ?
C49 H49F 0.9600 . ?
C64 C65 1.411(10) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N17 C65 1.111(10) . ?
C67 N18 1.120(10) . ?
C67 C66 1.415(10) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O2 90.91(10) . . ?
O1 Fe1 N1 95.19(10) . . ?
O2 Fe1 N1 89.41(10) . . ?
O1 Fe1 N3 87.34(10) . . ?
O2 Fe1 N3 95.10(10) . . ?
N1 Fe1 N3 174.80(10) . . ?
O1 Fe1 N2 176.84(9) . . ?
O2 Fe1 N2 87.12(11) . . ?
N1 Fe1 N2 82.33(10) . . ?
N3 Fe1 N2 95.29(11) . . ?
O1 Fe1 S1 93.15(8) . . ?
O2 Fe1 S1 175.91(8) . . ?
N1 Fe1 S1 90.67(8) . . ?
N3 Fe1 S1 84.65(8) . . ?
N2 Fe1 S1 88.84(8) . . ?
O4 Fe2 O3 90.80(10) . . ?
O4 Fe2 N9 86.27(10) . . ?
O3 Fe2 N9 103.36(10) . . ?
O4 Fe2 N7 87.57(11) . . ?
O3 Fe2 N7 160.16(11) . . ?
N9 Fe2 N7 96.26(11) . . ?
O4 Fe2 N6 107.98(10) . . ?
O3 Fe2 N6 86.10(11) . . ?
N9 Fe2 N6 162.98(9) . . ?
N7 Fe2 N6 75.65(11) . . ?
O4 Fe2 S2 164.71(7) . . ?
O3 Fe2 S2 96.63(8) . . ?
N9 Fe2 S2 79.02(8) . . ?
N7 Fe2 S2 89.87(9) . . ?
N6 Fe2 S2 85.92(8) . . ?
C24 S1 Fe1 96.39(11) . . ?
C48 S2 Fe2 97.75(12) . . ?
C25 O3 Fe2 130.4(2) . . ?
C41 O4 Fe2 136.80(19) . . ?
C1 O1 Fe1 125.83(19) . . ?
C47 N9 N8 112.5(2) . . ?
C47 N9 Fe2 124.68(19) . . ?
N8 N9 Fe2 122.78(19) . . ?
C17 O2 Fe1 125.7(2) . . ?
C7 N1 C8 121.1(2) . . ?
C7 N1 Fe1 124.7(2) . . ?
C8 N1 Fe1 114.13(18) . . ?
C24 N4 N3 113.2(2) . . ?
C15 N2 C16 118.8(3) . . ?
C15 N2 Fe1 127.9(2) . . ?
C16 N2 Fe1 113.31(19) . . ?
C31 N6 C32 119.8(3) . . ?
C31 N6 Fe2 123.8(3) . . ?
C32 N6 Fe2 115.5(2) . . ?
C23 N3 N4 113.9(2) . . ?
C23 N3 Fe1 124.0(2) . . ?
N4 N3 Fe1 122.12(18) . . ?
C48 N8 N9 114.4(2) . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N1 C7 C6 125.5(3) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
N2 C16 C12 122.1(3) . . ?
N2 C16 C8 116.2(3) . . ?
C12 C16 C8 121.8(3) . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
O4 C41 C42 120.5(3) . . ?
O4 C41 C46 121.0(3) . . ?
C42 C41 C46 118.4(3) . . ?
C39 N7 C40 118.7(4) . . ?
C39 N7 Fe2 124.3(3) . . ?
C40 N7 Fe2 117.0(3) . . ?
N9 C47 C46 127.1(3) . . ?
N9 C47 H47 116.4 . . ?
C46 C47 H47 116.4 . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C16 C12 C11 117.6(3) . . ?
C16 C12 C13 117.4(3) . . ?
C11 C12 C13 125.0(3) . . ?
N4 C24 N5 119.2(2) . . ?
N4 C24 S1 123.5(2) . . ?
N5 C24 S1 117.2(2) . . ?
C11 C10 C9 121.6(3) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 117.7(3) . . ?
C1 C6 C7 123.1(3) . . ?
C21 C22 C17 120.4(3) . . ?
C21 C22 C23 116.4(3) . . ?
C17 C22 C23 123.2(3) . . ?
N3 C23 C22 125.7(3) . . ?
N3 C23 H23 117.1 . . ?
C22 C23 H23 117.1 . . ?
C45 C46 C41 119.0(3) . . ?
C45 C46 C47 117.7(3) . . ?
C41 C46 C47 123.4(3) . . ?
C3 C2 C1 122.4(3) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C33 C32 C40 117.9(4) . . ?
C33 C32 N6 127.4(4) . . ?
C40 C32 N6 114.7(3) . . ?
N7 C40 C36 122.1(4) . . ?
N7 C40 C32 117.1(3) . . ?
C36 C40 C32 120.7(4) . . ?
C9 C8 C16 118.7(3) . . ?
C9 C8 N1 127.8(3) . . ?
C16 C8 N1 113.6(2) . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
N6 C31 C30 126.4(3) . . ?
N6 C31 H31 116.8 . . ?
C30 C31 H31 116.8 . . ?
O2 C17 C18 118.4(3) . . ?
O2 C17 C22 125.2(3) . . ?
C18 C17 C22 116.4(3) . . ?
O3 C25 C30 123.6(4) . . ?
O3 C25 C26 118.1(4) . . ?
C30 C25 C26 118.3(4) . . ?
O1 C1 C2 117.4(3) . . ?
O1 C1 C6 125.6(3) . . ?
C2 C1 C6 117.0(3) . . ?
C43 C42 C41 121.4(3) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C10 C11 C12 120.6(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
N8 C48 N10 117.4(3) . . ?
N8 C48 S2 126.0(2) . . ?
N10 C48 S2 116.5(2) . . ?
N2 C15 C14 121.9(3) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C44 C45 C46 121.2(3) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C35 C36 C37 124.3(5) . . ?
C35 C36 C40 119.4(6) . . ?
C37 C36 C40 116.3(5) . . ?
C20 C21 C22 121.5(4) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C25 C30 C29 119.1(5) . . ?
C25 C30 C31 123.8(3) . . ?
C29 C30 C31 117.1(4) . . ?
C42 C43 C44 120.4(4) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C32 C33 C34 119.8(5) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 122.7(3) . . ?
C5 C4 F1 119.3(4) . . ?
C3 C4 F1 118.0(3) . . ?
C19 C20 C21 118.7(4) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
C19 C18 C17 121.4(4) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C28 C29 C30 121.7(6) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
N7 C39 C38 122.8(5) . . ?
N7 C39 H39 118.6 . . ?
C38 C39 H39 118.6 . . ?
C38 C37 C36 121.0(5) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C34 C35 C36 120.1(5) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C45 C44 C43 119.6(4) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C25 C26 C27 118.3(5) . . ?
C25 C26 H26 120.8 . . ?
C27 C26 H26 120.8 . . ?
C35 C34 C33 121.9(5) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C29 C28 C27 122.0(6) . . ?
C29 C28 F2 122.4(7) . . ?
C27 C28 F2 115.7(7) . . ?
C20 C19 C18 121.6(4) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C28 C27 C26 120.6(6) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C37 C38 C39 119.1(6) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N12 C51 C52 172.5(10) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N11' C50' C49' 164.8(13) . . ?
C50' C49' H49A 109.5 . . ?
C50' C49' H49B 109.5 . . ?
H49A C49' H49B 109.5 . . ?
C50' C49' H49C 109.5 . . ?
H49A C49' H49C 109.5 . . ?
H49B C49' H49C 109.5 . . ?
N13 C55 C56 177.6(12) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N16 C63 C62 179(2) . . ?
C61 N15 N15 164.8(15) . 2_667 ?
N15 C61 C60 177(2) . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C50 C49 H49D 109.5 . . ?
C50 C49 H49E 109.5 . . ?
H49D C49 H49E 109.5 . . ?
C50 C49 H49F 109.5 . . ?
H49D C49 H49F 109.5 . . ?
H49E C49 H49F 109.5 . . ?
N11 C50 C49 165(3) . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N18 C67 C66 166(7) . . ?
C67 C66 H66A 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C67 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N17 C65 C64 171(5) . . ?

_refine_diff_density_max         0.664
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ws101a
_database_code_depnum_ccdc_archive 'CCDC 1529168'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H17 Br Fe N5 O2 S, 0.5(C2 H3 N)'
_chemical_formula_sum            'C25 H18.50 Br Fe N5.50 O2 S'
_chemical_formula_weight         595.77

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                   12.456(3)
_cell_length_b                   13.824(3)
_cell_length_c                   16.723(3)
_cell_angle_alpha                102.95(3)
_cell_angle_beta                 98.81(3)
_cell_angle_gamma                109.24(3)
_cell_volume                     2567.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'Thin plate'
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    2.258
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9562
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
; 
The crystal is really tiny and the structure was obtained from MX2 at the Asustralian Synchrotron. The second run was attempted to get high% completeness of the data.
However, the single crystal decomposed and did not diffract well as it was. We then could not get enough completeness data.
Regarding to the accescible void, there is no trace of any significant electron density left to define as a solvent in the void.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 315r CCD'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29040
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_sigmaI/netI    0.1754
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         30.09
_reflns_number_total             13474
_reflns_number_gt                8160
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BluIce (McPhillips, 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. 
;

_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)+(0.1101P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13474
_refine_ls_number_parameters     641
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2500
_refine_ls_wR_factor_gt          0.2200
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_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 0.85411(6) 0.23922(5) 1.01353(4) 0.02716(17) Uani 1 1 d . . .
Br1 Br 0.59371(6) 0.59328(5) 0.86540(4) 0.04517(18) Uani 1 1 d . . .
Fe2 Fe 0.94003(8) 0.29863(6) 0.61237(5) 0.0357(2) Uani 1 1 d . . .
Br2 Br 0.38818(8) 0.25853(9) 0.73249(6) 0.0873(4) Uani 1 1 d . . .
S1 S 0.95349(13) 0.37826(9) 1.12751(8) 0.0350(3) Uani 1 1 d . . .
S2 S 0.76163(14) 0.17580(12) 0.50524(9) 0.0423(3) Uani 1 1 d . . .
O2 O 0.7799(3) 0.1164(3) 0.9164(2) 0.0346(8) Uani 1 1 d . . .
N1 N 0.9181(4) 0.3235(3) 0.9421(2) 0.0267(8) Uani 1 1 d . . .
N3 N 0.7981(4) 0.1622(3) 1.0936(3) 0.0304(9) Uani 1 1 d . . .
O1 O 0.7155(3) 0.2676(3) 1.0047(2) 0.0348(8) Uani 1 1 d . . .
N2 N 0.9969(4) 0.2058(3) 1.0155(3) 0.0304(8) Uani 1 1 d . . .
O3 O 0.8665(4) 0.3938(3) 0.6630(3) 0.0462(10) Uani 1 1 d . . .
C7 C 0.8753(4) 0.3896(4) 0.9161(3) 0.0282(9) Uani 1 1 d . . .
H7 H 0.9170 0.4317 0.8849 0.034 Uiso 1 1 calc R . .
N7 N 1.0210(4) 0.1806(4) 0.5966(3) 0.0371(10) Uani 1 1 d . . .
O4 O 1.0901(4) 0.4053(3) 0.6745(2) 0.0455(10) Uani 1 1 d . . .
C1 C 0.6949(5) 0.3389(4) 0.9713(3) 0.0320(10) Uani 1 1 d . . .
C8 C 1.0210(4) 0.3138(3) 0.9224(3) 0.0266(9) Uani 1 1 d . . .
N4 N 0.8415(4) 0.2101(3) 1.1809(3) 0.0359(10) Uani 1 1 d . . .
C22 C 0.6535(5) 0.0051(4) 0.9847(3) 0.0316(10) Uani 1 1 d . . .
C40 C 1.0075(5) 0.1209(4) 0.6514(3) 0.0370(12) Uani 1 1 d . . .
N6 N 0.8796(4) 0.2076(3) 0.6943(3) 0.0366(10) Uani 1 1 d . . .
C9 C 1.0827(5) 0.3576(4) 0.8691(3) 0.0337(11) Uani 1 1 d . . .
H9 H 1.0571 0.4018 0.8412 0.040 Uiso 1 1 calc R . .
C23 C 0.7150(5) 0.0693(4) 1.0709(3) 0.0312(10) Uani 1 1 d . . .
H23 H 0.6918 0.0401 1.1146 0.037 Uiso 1 1 calc R . .
C3 C 0.5556(5) 0.4236(4) 0.9407(4) 0.0401(12) Uani 1 1 d . . .
H3 H 0.4815 0.4287 0.9409 0.048 Uiso 1 1 calc R . .
C5 C 0.7399(5) 0.4802(4) 0.9005(3) 0.0331(10) Uani 1 1 d . . .
H5 H 0.7917 0.5250 0.8758 0.040 Uiso 1 1 calc R . .
C17 C 0.6869(5) 0.0316(4) 0.9126(3) 0.0324(10) Uani 1 1 d . . .
C21 C 0.5553(5) -0.0895(4) 0.9730(3) 0.0329(10) Uani 1 1 d . . .
H21 H 0.5342 -0.1084 1.0212 0.040 Uiso 1 1 calc R . .
C48 C 0.8062(6) 0.2098(4) 0.4186(3) 0.0407(12) Uani 1 1 d . . .
N9 N 0.9779(5) 0.3394(4) 0.5026(3) 0.0396(10) Uani 1 1 d . . .
C10 C 1.1832(5) 0.3377(4) 0.8553(4) 0.0377(11) Uani 1 1 d . . .
H10 H 1.2239 0.3680 0.8178 0.045 Uiso 1 1 calc R . .
C24 C 0.9141(5) 0.3110(4) 1.2010(3) 0.0363(11) Uani 1 1 d . . .
C6 C 0.7709(4) 0.4020(4) 0.9317(3) 0.0295(9) Uani 1 1 d . . .
N10 N 0.7340(5) 0.1512(4) 0.3407(3) 0.0465(12) Uani 1 1 d . . .
H10A H 0.7547 0.1644 0.2951 0.056 Uiso 1 1 calc R . .
H10B H 0.6666 0.1000 0.3360 0.056 Uiso 1 1 calc R . .
C32 C 0.9337(6) 0.1332(4) 0.7061(3) 0.0394(12) Uani 1 1 d . . .
C4 C 0.6360(5) 0.4902(4) 0.9066(3) 0.0348(11) Uani 1 1 d . . .
C18 C 0.6190(6) -0.0361(4) 0.8326(4) 0.0413(12) Uani 1 1 d . . .
H18 H 0.6400 -0.0193 0.7836 0.050 Uiso 1 1 calc R . .
N5 N 0.9635(5) 0.3670(4) 1.2830(3) 0.0477(13) Uani 1 1 d . . .
H5A H 0.9473 0.3363 1.3228 0.057 Uiso 1 1 calc R . .
H5B H 1.0120 0.4343 1.2969 0.057 Uiso 1 1 calc R . .
C31 C 0.7858(6) 0.2038(4) 0.7209(3) 0.0432(14) Uani 1 1 d . . .
H31 H 0.7576 0.1528 0.7501 0.052 Uiso 1 1 calc R . .
N8 N 0.9060(5) 0.2854(4) 0.4222(3) 0.0439(11) Uani 1 1 d . . .
C13 C 1.1951(6) 0.1629(4) 0.9956(4) 0.0438(13) Uani 1 1 d . . .
H13 H 1.2626 0.1473 0.9892 0.053 Uiso 1 1 calc R . .
C12 C 1.1629(5) 0.2293(4) 0.9514(4) 0.0374(12) Uani 1 1 d . . .
C16 C 1.0613(4) 0.2480(3) 0.9635(3) 0.0279(9) Uani 1 1 d . . .
C2 C 0.5864(5) 0.3503(4) 0.9741(4) 0.0395(12) Uani 1 1 d . . .
H2 H 0.5338 0.3071 0.9993 0.047 Uiso 1 1 calc R . .
C39 C 1.0877(6) 0.1675(5) 0.5437(4) 0.0439(13) Uani 1 1 d . . .
H39 H 1.0962 0.2083 0.5046 0.053 Uiso 1 1 calc R . .
C41 C 1.1784(6) 0.4721(4) 0.6553(4) 0.0447(14) Uani 1 1 d . . .
C11 C 1.2230(5) 0.2757(4) 0.8952(4) 0.0402(12) Uani 1 1 d . . .
H11 H 1.2913 0.2635 0.8854 0.048 Uiso 1 1 calc R . .
C46 C 1.1704(6) 0.4840(5) 0.5729(4) 0.0453(14) Uani 1 1 d . . .
C30 C 0.7209(6) 0.2726(5) 0.7091(4) 0.0462(14) Uani 1 1 d . . .
C19 C 0.5221(6) -0.1269(5) 0.8228(4) 0.0447(13) Uani 1 1 d . . .
H19 H 0.4771 -0.1709 0.7676 0.054 Uiso 1 1 calc R . .
C15 C 1.0303(5) 0.1443(4) 1.0549(4) 0.0397(12) Uani 1 1 d . . .
H15 H 0.9848 0.1140 1.0902 0.048 Uiso 1 1 calc R . .
C20 C 0.4895(5) -0.1547(4) 0.8934(4) 0.0403(12) Uani 1 1 d . . .
H20 H 0.4232 -0.2175 0.8866 0.048 Uiso 1 1 calc R . .
C35 C 1.0457(7) -0.0102(5) 0.7145(5) 0.0587(19) Uani 1 1 d . . .
H35 H 1.0831 -0.0594 0.7180 0.070 Uiso 1 1 calc R . .
C36 C 1.0635(6) 0.0467(5) 0.6553(4) 0.0459(14) Uani 1 1 d . . .
C14 C 1.1312(6) 0.1219(5) 1.0466(4) 0.0447(13) Uani 1 1 d . . .
H14 H 1.1539 0.0782 1.0767 0.054 Uiso 1 1 calc R . .
C25 C 0.7661(6) 0.3638(5) 0.6813(4) 0.0476(15) Uani 1 1 d . . .
C33 C 0.9188(7) 0.0767(5) 0.7638(4) 0.0528(17) Uani 1 1 d . . .
H33 H 0.8706 0.0867 0.8013 0.063 Uiso 1 1 calc R . .
C26 C 0.6893(7) 0.4225(6) 0.6711(4) 0.0578(18) Uani 1 1 d . . .
H26 H 0.7162 0.4842 0.6523 0.069 Uiso 1 1 calc R . .
C47 C 1.0723(6) 0.4180(5) 0.5028(4) 0.0441(13) Uani 1 1 d . . .
H47 H 1.0760 0.4328 0.4503 0.053 Uiso 1 1 calc R . .
C38 C 1.1467(6) 0.0960(5) 0.5427(4) 0.0489(15) Uani 1 1 d . . .
H38 H 1.1947 0.0899 0.5044 0.059 Uiso 1 1 calc R . .
C28 C 0.5415(6) 0.3032(7) 0.7140(4) 0.062(2) Uani 1 1 d . . .
C29 C 0.6091(6) 0.2429(6) 0.7283(4) 0.0577(18) Uani 1 1 d . . .
H29 H 0.5814 0.1840 0.7501 0.069 Uiso 1 1 calc R . .
C43 C 1.3753(7) 0.6068(5) 0.6997(5) 0.064(2) Uani 1 1 d . . .
H43 H 1.4461 0.6469 0.7424 0.077 Uiso 1 1 calc R . .
C45 C 1.2663(7) 0.5597(5) 0.5566(5) 0.0565(17) Uani 1 1 d . . .
H45 H 1.2605 0.5682 0.5015 0.068 Uiso 1 1 calc R . .
C27 C 0.5829(8) 0.3936(7) 0.6868(4) 0.063(2) Uani 1 1 d . . .
H27 H 0.5360 0.4345 0.6794 0.075 Uiso 1 1 calc R . .
C42 C 1.2836(7) 0.5370(5) 0.7178(5) 0.0600(19) Uani 1 1 d . . .
H42 H 1.2903 0.5316 0.7738 0.072 Uiso 1 1 calc R . .
C37 C 1.1340(6) 0.0369(5) 0.5964(4) 0.0515(16) Uani 1 1 d . . .
H37 H 1.1725 -0.0122 0.5955 0.062 Uiso 1 1 calc R . .
C44 C 1.3671(8) 0.6209(6) 0.6184(5) 0.065(2) Uani 1 1 d . . .
H44 H 1.4306 0.6720 0.6067 0.078 Uiso 1 1 calc R . .
C34 C 0.9747(9) 0.0040(6) 0.7678(5) 0.064(2) Uani 1 1 d . . .
H34 H 0.9634 -0.0356 0.8076 0.077 Uiso 1 1 calc R . .
N11 N 0.4584(12) 0.0294(8) 0.3666(6) 0.123(4) Uani 1 1 d . . .
C49 C 0.4540(12) 0.0762(9) 0.4325(6) 0.097(4) Uani 1 1 d . . .
C50 C 0.4575(14) 0.1384(14) 0.5169(7) 0.138(6) Uani 1 1 d . . .
H50A H 0.5392 0.1817 0.5478 0.207 Uiso 1 1 calc R . .
H50B H 0.4209 0.0895 0.5479 0.207 Uiso 1 1 calc R . .
H50C H 0.4147 0.1856 0.5114 0.207 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 O1 1.884(4) . ?
Fe1 O2 1.910(4) . ?
Fe1 N1 1.931(4) . ?
Fe1 N3 1.962(4) . ?
Fe1 N2 1.977(4) . ?
Fe1 S1 2.2197(18) . ?
Br1 C4 1.899(5) . ?
Fe2 O4 1.910(5) . ?
Fe2 O3 1.954(4) . ?
Fe2 N9 2.112(5) . ?
Fe2 N6 2.120(5) . ?
Fe2 N7 2.173(5) . ?
Fe2 S2 2.442(2) . ?
Br2 C28 1.901(8) . ?
S1 C24 1.734(6) . ?
S2 C48 1.734(6) . ?
O2 C17 1.330(6) . ?
N1 C7 1.316(6) . ?
N1 C8 1.411(6) . ?
N3 C23 1.284(7) . ?
N3 N4 1.397(6) . ?
O1 C1 1.312(6) . ?
N2 C15 1.316(7) . ?
N2 C16 1.368(6) . ?
O3 C25 1.289(8) . ?
C7 C6 1.421(6) . ?
C7 H7 0.9500 . ?
N7 C39 1.326(7) . ?
N7 C40 1.358(7) . ?
O4 C41 1.318(8) . ?
C1 C6 1.415(7) . ?
C1 C2 1.417(7) . ?
C8 C9 1.378(7) . ?
C8 C16 1.424(7) . ?
N4 C24 1.320(7) . ?
C22 C21 1.415(7) . ?
C22 C17 1.418(7) . ?
C22 C23 1.447(7) . ?
C40 C32 1.415(8) . ?
C40 C36 1.426(8) . ?
N6 C31 1.301(8) . ?
N6 C32 1.434(8) . ?
C9 C10 1.408(7) . ?
C9 H9 0.9500 . ?
C23 H23 0.9500 . ?
C3 C2 1.389(8) . ?
C3 C4 1.406(8) . ?
C3 H3 0.9500 . ?
C5 C4 1.363(7) . ?
C5 C6 1.435(7) . ?
C5 H5 0.9500 . ?
C17 C18 1.398(8) . ?
C21 C20 1.377(8) . ?
C21 H21 0.9500 . ?
C48 N8 1.316(8) . ?
C48 N10 1.360(7) . ?
N9 C47 1.311(8) . ?
N9 N8 1.381(7) . ?
C10 C11 1.364(8) . ?
C10 H10 0.9500 . ?
C24 N5 1.346(7) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
C32 C33 1.369(9) . ?
C18 C19 1.382(8) . ?
C18 H18 0.9500 . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
C31 C30 1.463(9) . ?
C31 H31 0.9500 . ?
C13 C14 1.345(9) . ?
C13 C12 1.416(8) . ?
C13 H13 0.9500 . ?
C12 C16 1.406(7) . ?
C12 C11 1.423(8) . ?
C2 H2 0.9500 . ?
C39 C38 1.412(9) . ?
C39 H39 0.9500 . ?
C41 C42 1.414(9) . ?
C41 C46 1.416(9) . ?
C11 H11 0.9500 . ?
C46 C45 1.414(9) . ?
C46 C47 1.431(9) . ?
C30 C25 1.413(10) . ?
C30 C29 1.425(9) . ?
C19 C20 1.397(9) . ?
C19 H19 0.9500 . ?
C15 C14 1.410(8) . ?
C15 H15 0.9500 . ?
C20 H20 0.9500 . ?
C35 C34 1.376(11) . ?
C35 C36 1.396(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.429(9) . ?
C14 H14 0.9500 . ?
C25 C26 1.458(10) . ?
C33 C34 1.407(11) . ?
C33 H33 0.9500 . ?
C26 C27 1.339(11) . ?
C26 H26 0.9500 . ?
C47 H47 0.9500 . ?
C38 C37 1.337(10) . ?
C38 H38 0.9500 . ?
C28 C27 1.391(12) . ?
C28 C29 1.397(11) . ?
C29 H29 0.9500 . ?
C43 C42 1.355(12) . ?
C43 C44 1.408(12) . ?
C43 H43 0.9500 . ?
C45 C44 1.368(11) . ?
C45 H45 0.9500 . ?
C27 H27 0.9500 . ?
C42 H42 0.9500 . ?
C37 H37 0.9500 . ?
C44 H44 0.9500 . ?
C34 H34 0.9500 . ?
N11 C49 1.167(13) . ?
C49 C50 1.464(14) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 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 90.64(17) . . ?
O1 Fe1 N1 95.33(16) . . ?
O2 Fe1 N1 89.62(16) . . ?
O1 Fe1 N3 85.98(17) . . ?
O2 Fe1 N3 94.57(16) . . ?
N1 Fe1 N3 175.59(18) . . ?
O1 Fe1 N2 176.63(17) . . ?
O2 Fe1 N2 86.46(17) . . ?
N1 Fe1 N2 82.94(18) . . ?
N3 Fe1 N2 95.96(18) . . ?
O1 Fe1 S1 94.17(13) . . ?
O2 Fe1 S1 175.18(13) . . ?
N1 Fe1 S1 90.27(12) . . ?
N3 Fe1 S1 85.43(13) . . ?
N2 Fe1 S1 88.75(13) . . ?
O4 Fe2 O3 89.1(2) . . ?
O4 Fe2 N9 87.79(18) . . ?
O3 Fe2 N9 106.41(18) . . ?
O4 Fe2 N6 106.22(18) . . ?
O3 Fe2 N6 86.29(17) . . ?
N9 Fe2 N6 161.46(17) . . ?
O4 Fe2 N7 88.59(19) . . ?
O3 Fe2 N7 160.53(18) . . ?
N9 Fe2 N7 92.81(18) . . ?
N6 Fe2 N7 75.82(18) . . ?
O4 Fe2 S2 166.69(13) . . ?
O3 Fe2 S2 94.53(15) . . ?
N9 Fe2 S2 78.91(14) . . ?
N6 Fe2 S2 86.81(14) . . ?
N7 Fe2 S2 92.12(13) . . ?
C24 S1 Fe1 96.21(19) . . ?
C48 S2 Fe2 97.0(2) . . ?
C17 O2 Fe1 123.7(3) . . ?
C7 N1 C8 121.1(4) . . ?
C7 N1 Fe1 124.4(3) . . ?
C8 N1 Fe1 114.4(3) . . ?
C23 N3 N4 115.5(4) . . ?
C23 N3 Fe1 123.4(4) . . ?
N4 N3 Fe1 120.9(3) . . ?
C1 O1 Fe1 125.5(3) . . ?
C15 N2 C16 118.8(4) . . ?
C15 N2 Fe1 128.2(4) . . ?
C16 N2 Fe1 112.8(3) . . ?
C25 O3 Fe2 125.7(4) . . ?
N1 C7 C6 124.4(4) . . ?
N1 C7 H7 117.8 . . ?
C6 C7 H7 117.8 . . ?
C39 N7 C40 118.2(5) . . ?
C39 N7 Fe2 126.4(4) . . ?
C40 N7 Fe2 115.2(3) . . ?
C41 O4 Fe2 135.3(4) . . ?
O1 C1 C6 124.9(4) . . ?
O1 C1 C2 116.3(5) . . ?
C6 C1 C2 118.7(5) . . ?
C9 C8 N1 128.3(4) . . ?
C9 C8 C16 118.5(4) . . ?
N1 C8 C16 113.2(4) . . ?
C24 N4 N3 113.0(4) . . ?
C21 C22 C17 119.1(5) . . ?
C21 C22 C23 117.3(5) . . ?
C17 C22 C23 123.7(5) . . ?
N7 C40 C32 117.9(5) . . ?
N7 C40 C36 122.8(5) . . ?
C32 C40 C36 119.2(5) . . ?
C31 N6 C32 120.2(5) . . ?
C31 N6 Fe2 122.8(4) . . ?
C32 N6 Fe2 116.0(3) . . ?
C8 C9 C10 120.8(5) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
N3 C23 C22 125.9(5) . . ?
N3 C23 H23 117.0 . . ?
C22 C23 H23 117.0 . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
O2 C17 C18 117.8(5) . . ?
O2 C17 C22 124.0(5) . . ?
C18 C17 C22 118.2(5) . . ?
C20 C21 C22 121.6(5) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
N8 C48 N10 117.6(5) . . ?
N8 C48 S2 125.1(5) . . ?
N10 C48 S2 117.2(5) . . ?
C47 N9 N8 112.3(5) . . ?
C47 N9 Fe2 124.1(4) . . ?
N8 N9 Fe2 123.6(4) . . ?
C11 C10 C9 121.0(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
N4 C24 N5 119.4(5) . . ?
N4 C24 S1 124.1(4) . . ?
N5 C24 S1 116.4(4) . . ?
C1 C6 C7 124.2(4) . . ?
C1 C6 C5 119.3(4) . . ?
C7 C6 C5 116.4(4) . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C33 C32 C40 120.4(6) . . ?
C33 C32 N6 125.6(5) . . ?
C40 C32 N6 114.1(5) . . ?
C5 C4 C3 121.9(5) . . ?
C5 C4 Br1 120.1(4) . . ?
C3 C4 Br1 117.9(4) . . ?
C19 C18 C17 121.6(6) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N6 C31 C30 124.7(6) . . ?
N6 C31 H31 117.7 . . ?
C30 C31 H31 117.7 . . ?
C48 N8 N9 115.1(5) . . ?
C14 C13 C12 120.7(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C16 C12 C13 116.3(5) . . ?
C16 C12 C11 118.3(5) . . ?
C13 C12 C11 125.4(5) . . ?
N2 C16 C12 122.5(5) . . ?
N2 C16 C8 116.4(4) . . ?
C12 C16 C8 121.1(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
N7 C39 C38 123.1(6) . . ?
N7 C39 H39 118.4 . . ?
C38 C39 H39 118.4 . . ?
O4 C41 C42 120.6(6) . . ?
O4 C41 C46 121.6(6) . . ?
C42 C41 C46 117.7(6) . . ?
C10 C11 C12 120.3(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C45 C46 C41 119.3(6) . . ?
C45 C46 C47 117.4(6) . . ?
C41 C46 C47 123.2(6) . . ?
C25 C30 C29 121.6(7) . . ?
C25 C30 C31 122.4(6) . . ?
C29 C30 C31 115.9(6) . . ?
C18 C19 C20 120.7(6) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
N2 C15 C14 122.3(5) . . ?
N2 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C21 C20 C19 118.8(5) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C34 C35 C36 121.0(6) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C40 118.8(6) . . ?
C35 C36 C37 125.4(6) . . ?
C40 C36 C37 115.8(6) . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
O3 C25 C30 123.9(6) . . ?
O3 C25 C26 120.4(6) . . ?
C30 C25 C26 115.6(6) . . ?
C32 C33 C34 120.2(6) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C27 C26 C25 123.2(8) . . ?
C27 C26 H26 118.4 . . ?
C25 C26 H26 118.4 . . ?
N9 C47 C46 127.5(6) . . ?
N9 C47 H47 116.2 . . ?
C46 C47 H47 116.2 . . ?
C37 C38 C39 119.1(6) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C27 C28 C29 122.2(7) . . ?
C27 C28 Br2 119.7(6) . . ?
C29 C28 Br2 118.1(7) . . ?
C28 C29 C30 117.9(8) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
C42 C43 C44 121.0(7) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C44 C45 C46 121.4(7) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 H45 119.3 . . ?
C26 C27 C28 119.4(7) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C43 C42 C41 121.6(7) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C38 C37 C36 120.9(6) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C45 C44 C43 118.9(7) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C35 C34 C33 120.4(7) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
N11 C49 C50 176.0(15) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.891
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.912
_refine_diff_density_max         2.151
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.139
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_160K_a
_database_code_depnum_ccdc_archive 'CCDC 1529172'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(qsal-F)(thsa)]2.5MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H49 F2 Fe2 N15 O4 S2'
_chemical_formula_weight         1233.94

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.066(3)
_cell_length_b                   16.467(3)
_cell_length_c                   16.472(3)
_cell_angle_alpha                119.54(3)
_cell_angle_beta                 109.03(3)
_cell_angle_gamma                91.39(3)
_cell_volume                     2840.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    15927
_cell_measurement_theta_min      0.816
_cell_measurement_theta_max      31.857

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.653
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
;
This strcutures has been solved and refined by reasonable model.
Two molecules of MeCN are disorderd over 4 position (molecules of N15-N18). Firstly, the free variables over 
the positions were applied and the overall occupancy were about two. Therefore, SUMP command was applied to set overall
MeCN over 4 positions to be two. ISOR command was used on the positions that showed severely disoder after the anisotropy application.
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1, Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65132
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.457
_diffrn_reflns_theta_max         31.857
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             15927
_reflns_number_gt                14499
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
;

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0520P)²+1.8102P]
 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         15927
_refine_ls_number_parameters     813
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.40779(2) 0.79313(2) 0.25654(2) 0.02064(5) Uani 1 1 d . . . . .
Fe2 Fe 0.47985(2) 0.24785(2) 0.32659(2) 0.02266(5) Uani 1 1 d . . . . .
S1 S 0.51413(3) 0.79120(2) 0.39185(3) 0.02428(7) Uani 1 1 d . . . . .
S2 S 0.36241(3) 0.24563(3) 0.17764(3) 0.03083(9) Uani 1 1 d . . . . .
F1 F 0.08401(11) 1.06491(9) 0.48145(12) 0.0554(3) Uani 1 1 d . . . . .
F2 F -0.03544(11) 0.01346(14) 0.22639(13) 0.0779(5) Uani 1 1 d . . . . .
O1 O 0.27799(9) 0.78249(7) 0.28021(9) 0.0265(2) Uani 1 1 d . . . . .
O2 O 0.32447(9) 0.79605(8) 0.13918(8) 0.0282(2) Uani 1 1 d . . . . .
O3 O 0.36639(10) 0.25111(9) 0.38042(9) 0.0324(2) Uani 1 1 d . . . . .
O4 O 0.59363(10) 0.27965(8) 0.45242(9) 0.0294(2) Uani 1 1 d . . . . .
N1 N 0.44739(10) 0.93139(8) 0.33510(9) 0.0212(2) Uani 1 1 d . . . . .
N2 N 0.54147(11) 0.80795(9) 0.22899(10) 0.0245(2) Uani 1 1 d . . . . .
N3 N 0.38148(10) 0.65425(8) 0.18647(9) 0.0225(2) Uani 1 1 d . . . . .
N4 N 0.43300(11) 0.60791(9) 0.23516(9) 0.0251(2) Uani 1 1 d . . . . .
N5 N 0.54589(12) 0.63217(9) 0.38847(10) 0.0275(2) Uani 1 1 d . . . . .
H5A H 0.5396 0.5700 0.3606 0.033 Uiso 1 1 calc R U . . .
H5B H 0.5866 0.6714 0.4534 0.033 Uiso 1 1 calc R U . . .
N6 N 0.41826(11) 0.09449(9) 0.23270(10) 0.0267(2) Uani 1 1 d . . . . .
N7 N 0.59803(12) 0.19719(10) 0.25852(11) 0.0309(3) Uani 1 1 d . . . . .
N8 N 0.49016(11) 0.42618(9) 0.30755(10) 0.0267(2) Uani 1 1 d . . . . .
N9 N 0.53109(10) 0.39271(8) 0.37185(9) 0.0230(2) Uani 1 1 d . . . . .
N10 N 0.37264(13) 0.39175(10) 0.15274(11) 0.0340(3) Uani 1 1 d . . . . .
H10A H 0.3978 0.4505 0.1703 0.041 Uiso 1 1 calc R U . . .
H10B H 0.3210 0.3517 0.0923 0.041 Uiso 1 1 calc R U . . .
N11 N 0.14414(17) 0.00411(17) 0.00330(15) 0.0579(5) Uani 1 1 d . . . . .
N12 N 0.1476(2) 0.2999(3) -0.0327(2) 0.0859(9) Uani 1 1 d . . . . .
N13 N 0.0839(2) 1.32781(16) 0.7222(2) 0.0676(6) Uani 1 1 d . . . . .
C1 C 0.23743(12) 0.85425(11) 0.33116(11) 0.0249(3) Uani 1 1 d . . . . .
C2 C 0.13771(14) 0.83129(12) 0.33981(13) 0.0317(3) Uani 1 1 d . . . . .
H2 H 0.1052 0.7660 0.3106 0.038 Uiso 1 1 calc R U . . .
C3 C 0.08685(14) 0.90106(13) 0.38941(15) 0.0360(3) Uani 1 1 d . . . . .
H3 H 0.0195 0.8843 0.3937 0.043 Uiso 1 1 calc R U . . .
C4 C 0.13577(15) 0.99649(13) 0.43310(15) 0.0365(4) Uani 1 1 d . . . . .
C5 C 0.23248(14) 1.02341(12) 0.42940(13) 0.0317(3) Uani 1 1 d . . . . .
H5 H 0.2642 1.0894 0.4612 0.038 Uiso 1 1 calc R U . . .
C6 C 0.28579(12) 0.95290(10) 0.37810(11) 0.0247(3) Uani 1 1 d . . . . .
C7 C 0.38781(12) 0.98622(10) 0.37799(11) 0.0233(3) Uani 1 1 d . . . . .
H7 H 0.4139 1.0535 0.4118 0.028 Uiso 1 1 calc R U . . .
C8 C 0.55194(12) 0.97060(10) 0.34460(11) 0.0219(2) Uani 1 1 d . . . . .
C9 C 0.60795(12) 1.06534(10) 0.40402(11) 0.0251(3) Uani 1 1 d . . . . .
H9 H 0.5777 1.1127 0.4459 0.030 Uiso 1 1 calc R U . . .
C10 C 0.71053(13) 1.09168(11) 0.40233(13) 0.0301(3) Uani 1 1 d . . . . .
H10 H 0.7487 1.1571 0.4436 0.036 Uiso 1 1 calc R U . . .
C11 C 0.75638(14) 1.02534(12) 0.34268(13) 0.0314(3) Uani 1 1 d . . . . .
H11 H 0.8253 1.0450 0.3426 0.038 Uiso 1 1 calc R U . . .
C12 C 0.70111(13) 0.92732(11) 0.28112(12) 0.0281(3) Uani 1 1 d . . . . .
C13 C 0.73915(15) 0.85345(13) 0.21416(14) 0.0358(3) Uani 1 1 d . . . . .
H13 H 0.8069 0.8677 0.2092 0.043 Uiso 1 1 calc R U . . .
C14 C 0.67756(16) 0.76154(13) 0.15677(15) 0.0385(4) Uani 1 1 d . . . . .
H14 H 0.7013 0.7118 0.1102 0.046 Uiso 1 1 calc R U . . .
C15 C 0.57906(15) 0.74064(12) 0.16671(13) 0.0324(3) Uani 1 1 d . . . . .
H15 H 0.5381 0.6762 0.1275 0.039 Uiso 1 1 calc R U . . .
C16 C 0.59938(12) 0.90088(10) 0.28423(11) 0.0232(3) Uani 1 1 d . . . . .
C17 C 0.25581(12) 0.72196(11) 0.05251(11) 0.0262(3) Uani 1 1 d . . . . .
C18 C 0.18387(14) 0.73888(13) -0.02031(13) 0.0343(3) Uani 1 1 d . . . . .
H18 H 0.1870 0.8028 -0.0049 0.041 Uiso 1 1 calc R U . . .
C19 C 0.10926(15) 0.66469(14) -0.11322(14) 0.0394(4) Uani 1 1 d . . . . .
H19 H 0.0613 0.6785 -0.1600 0.047 Uiso 1 1 calc R U . . .
C20 C 0.10360(15) 0.56971(14) -0.13901(13) 0.0376(4) Uani 1 1 d . . . . .
H20 H 0.0525 0.5188 -0.2030 0.045 Uiso 1 1 calc R U . . .
C21 C 0.17352(14) 0.55132(12) -0.06987(12) 0.0318(3) Uani 1 1 d . . . . .
H21 H 0.1707 0.4867 -0.0876 0.038 Uiso 1 1 calc R U . . .
C22 C 0.24902(12) 0.62507(11) 0.02617(11) 0.0262(3) Uani 1 1 d . . . . .
C23 C 0.31420(12) 0.59657(10) 0.09330(11) 0.0257(3) Uani 1 1 d . . . . .
H23 H 0.3071 0.5298 0.0668 0.031 Uiso 1 1 calc R U . . .
C24 C 0.49339(12) 0.66727(10) 0.33185(11) 0.0232(3) Uani 1 1 d . . . . .
C25 C 0.26938(14) 0.19269(13) 0.33874(13) 0.0327(3) Uani 1 1 d . . . . .
C26 C 0.18499(17) 0.22705(17) 0.37350(17) 0.0450(4) Uani 1 1 d . . . . .
H26 H 0.1983 0.2926 0.4245 0.054 Uiso 1 1 calc R U . . .
C27 C 0.08324(18) 0.1672(2) 0.3348(2) 0.0548(6) Uani 1 1 d . . . . .
H27 H 0.0269 0.1914 0.3586 0.066 Uiso 1 1 calc R U . . .
C28 C 0.06439(17) 0.0721(2) 0.26128(18) 0.0549(6) Uani 1 1 d . . . . .
C29 C 0.14185(17) 0.03519(17) 0.22425(16) 0.0466(5) Uani 1 1 d . . . . .
H29 H 0.1261 -0.0308 0.1735 0.056 Uiso 1 1 calc R U . . .
C30 C 0.24625(14) 0.09488(13) 0.26112(13) 0.0339(3) Uani 1 1 d . . . . .
C31 C 0.32225(15) 0.05110(12) 0.21509(12) 0.0325(3) Uani 1 1 d . . . . .
H31 H 0.3000 -0.0160 0.1672 0.039 Uiso 1 1 calc R U . . .
C32 C 0.48039(15) 0.04351(11) 0.17488(11) 0.0290(3) Uani 1 1 d . . . . .
C33 C 0.45705(18) -0.05373(12) 0.10711(13) 0.0390(4) Uani 1 1 d . . . . .
H33 H 0.3948 -0.0940 0.0968 0.047 Uiso 1 1 calc R U . . .
C34 C 0.5254(2) -0.09384(14) 0.05281(14) 0.0471(5) Uani 1 1 d . . . . .
H34 H 0.5071 -0.1609 0.0054 0.057 Uiso 1 1 calc R U . . .
C35 C 0.6163(2) -0.03961(15) 0.06632(15) 0.0445(5) Uani 1 1 d . . . . .
H35 H 0.6604 -0.0685 0.0285 0.053 Uiso 1 1 calc R U . . .
C36 C 0.64511(17) 0.06050(14) 0.13727(14) 0.0379(4) Uani 1 1 d . . . . .
C37 C 0.73905(19) 0.12282(18) 0.15805(17) 0.0502(5) Uani 1 1 d . . . . .
H37 H 0.7873 0.0982 0.1236 0.060 Uiso 1 1 calc R U . . .
C38 C 0.7602(2) 0.21800(19) 0.2273(2) 0.0574(6) Uani 1 1 d . . . . .
H38 H 0.8235 0.2603 0.2421 0.069 Uiso 1 1 calc R U . . .
C39 C 0.68746(16) 0.25307(15) 0.27670(17) 0.0452(4) Uani 1 1 d . . . . .
H39 H 0.7030 0.3197 0.3252 0.054 Uiso 1 1 calc R U . . .
C40 C 0.57575(14) 0.10140(12) 0.19025(12) 0.0298(3) Uani 1 1 d . . . . .
C41 C 0.65831(12) 0.35860(11) 0.53562(11) 0.0250(3) Uani 1 1 d . . . . .
C42 C 0.72407(13) 0.35581(13) 0.62079(13) 0.0311(3) Uani 1 1 d . . . . .
H42 H 0.7226 0.2961 0.6166 0.037 Uiso 1 1 calc R U . . .
C43 C 0.79033(15) 0.43817(14) 0.70989(14) 0.0371(4) Uani 1 1 d . . . . .
H43 H 0.8333 0.4345 0.7664 0.044 Uiso 1 1 calc R U . . .
C44 C 0.79550(15) 0.52710(14) 0.71862(14) 0.0391(4) Uani 1 1 d . . . . .
H44 H 0.8415 0.5836 0.7804 0.047 Uiso 1 1 calc R U . . .
C45 C 0.73281(14) 0.53152(12) 0.63609(13) 0.0338(3) Uani 1 1 d . . . . .
H45 H 0.7362 0.5918 0.6415 0.041 Uiso 1 1 calc R U . . .
C46 C 0.66371(12) 0.44852(10) 0.54377(11) 0.0254(3) Uani 1 1 d . . . . .
C47 C 0.60197(13) 0.45944(10) 0.46115(11) 0.0258(3) Uani 1 1 d . . . . .
H47 H 0.6142 0.5221 0.4730 0.031 Uiso 1 1 calc R U . . .
C48 C 0.41335(13) 0.36305(10) 0.21872(11) 0.0254(3) Uani 1 1 d . . . . .
C49 C 0.11340(18) 0.07354(19) 0.03113(18) 0.0506(5) Uani 1 1 d . . . . .
C50 C 0.0732(2) 0.1610(2) 0.0707(3) 0.0760(9) Uani 1 1 d . . . . .
H50A H -0.0038 0.1455 0.0626 0.114 Uiso 1 1 calc R U . . .
H50B H 0.0764 0.1919 0.0336 0.114 Uiso 1 1 calc R U . . .
H50C H 0.1197 0.2044 0.1427 0.114 Uiso 1 1 calc R U . . .
C51 C 0.07140(17) 0.32465(19) -0.05870(16) 0.0515(5) Uani 1 1 d . . . . .
C52 C -0.02522(19) 0.3591(2) -0.0917(2) 0.0621(7) Uani 1 1 d . . . . .
H52A H -0.0338 0.4118 -0.0324 0.093 Uiso 1 1 calc R U . . .
H52B H -0.0916 0.3068 -0.1308 0.093 Uiso 1 1 calc R U . . .
H52C H -0.0155 0.3819 -0.1342 0.093 Uiso 1 1 calc R U . . .
C55 C 0.14594(18) 1.31011(15) 0.68544(17) 0.0451(4) Uani 1 1 d . . . . .
C56 C 0.2264(3) 1.2884(3) 0.6398(3) 0.0827(10) Uani 1 1 d . . . . .
H56A H 0.2840 1.3465 0.6729 0.124 Uiso 1 1 calc R U . . .
H56B H 0.1895 1.2650 0.5676 0.124 Uiso 1 1 calc R U . . .
H56C H 0.2604 1.2391 0.6477 0.124 Uiso 1 1 calc R U . . .
C60 C 0.3763(15) 0.5778(13) -0.1543(13) 0.094(4) Uani 0.531(3) 1 d D . P A 1
H60A H 0.3268 0.6167 -0.1267 0.142 Uiso 0.531(3) 1 calc R U P A 1
H60B H 0.3339 0.5269 -0.2250 0.142 Uiso 0.531(3) 1 calc R U P A 1
H60C H 0.4357 0.6184 -0.1508 0.142 Uiso 0.531(3) 1 calc R U P A 1
N15 N 0.4639(4) 0.5042(3) -0.0469(4) 0.0706(13) Uani 0.531(3) 1 d D . P A 1
C61 C 0.4247(4) 0.5354(4) -0.0954(4) 0.0581(12) Uani 0.531(3) 1 d D . P A 1
C63 C 0.7179(5) 0.4654(5) 0.2800(6) 0.0693(17) Uani 0.487(3) 1 d D . P B 2
N16 N 0.7769(5) 0.4907(6) 0.3597(6) 0.098(2) Uani 0.487(3) 1 d D . P B 2
C64 C -0.0573(8) 0.3933(8) -0.4659(8) 0.116(4) Uani 0.618(3) 1 d D U P C 3
H64A H -0.1091 0.4056 -0.5149 0.174 Uiso 0.618(3) 1 calc R U P C 3
H64B H -0.0830 0.4084 -0.4115 0.174 Uiso 0.618(3) 1 calc R U P C 3
H64C H -0.0538 0.3256 -0.5001 0.174 Uiso 0.618(3) 1 calc R U P C 3
C65 C 0.0540(7) 0.4537(6) -0.4229(6) 0.115(2) Uani 0.618(3) 1 d D U P C 3
N18 N 1.0110(10) 0.3848(7) 0.3605(9) 0.130(4) Uani 0.364(3) 1 d D . P D 4
C67 C 1.0329(8) 0.4683(7) 0.3983(7) 0.088(3) Uani 0.364(3) 1 d D . P D 4
N17 N 0.1435(8) 0.4988(8) -0.3918(9) 0.195(4) Uani 0.618(3) 1 d D U P C 3
C62 C 0.6403(16) 0.4309(17) 0.1767(11) 0.118(7) Uani 0.487(3) 1 d D . P B 2
H62A H 0.5812 0.4665 0.1789 0.177 Uiso 0.487(3) 1 calc R U P B 2
H62B H 0.6076 0.3625 0.1423 0.177 Uiso 0.487(3) 1 calc R U P B 2
H62C H 0.6801 0.4404 0.1398 0.177 Uiso 0.487(3) 1 calc R U P B 2
C66 C 1.0584(9) 0.5718(6) 0.4458(8) 0.0514(19) Uani 0.364(3) 1 d D . P D 4
H66A H 1.1392 0.5961 0.4779 0.077 Uiso 0.364(3) 1 calc R U P D 4
H66B H 1.0266 0.6011 0.4972 0.077 Uiso 0.364(3) 1 calc R U P D 4
H66C H 1.0267 0.5880 0.3944 0.077 Uiso 0.364(3) 1 calc R U P D 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.8824(11) . ?
Fe1 O2 1.9094(13) . ?
Fe1 N1 1.9305(15) . ?
Fe1 N3 1.9444(14) . ?
Fe1 N2 1.9804(13) . ?
Fe1 S1 2.2250(9) . ?
Fe2 O4 1.9137(15) . ?
Fe2 O3 1.9496(12) . ?
Fe2 N9 2.1302(14) . ?
Fe2 N7 2.1463(15) . ?
Fe2 N6 2.1577(17) . ?
Fe2 S2 2.4143(10) . ?
S1 C24 1.7393(16) . ?
S2 C48 1.7301(16) . ?
F1 C4 1.365(2) . ?
F2 C28 1.367(2) . ?
O1 C1 1.3131(18) . ?
O2 C17 1.314(2) . ?
O3 C25 1.314(2) . ?
O4 C41 1.310(2) . ?
N1 C7 1.2978(19) . ?
N1 C8 1.4232(18) . ?
N2 C15 1.325(2) . ?
N2 C16 1.365(2) . ?
N3 C23 1.293(2) . ?
N3 N4 1.3980(17) . ?
N4 C24 1.313(2) . ?
N5 C24 1.3445(18) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 C31 1.297(2) . ?
N6 C32 1.421(2) . ?
N7 C39 1.323(2) . ?
N7 C40 1.361(2) . ?
N8 C48 1.312(2) . ?
N8 N9 1.3900(17) . ?
N9 C47 1.303(2) . ?
N10 C48 1.3523(19) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N11 C49 1.142(3) . ?
N12 C51 1.120(3) . ?
N13 C55 1.125(3) . ?
C1 C2 1.418(2) . ?
C1 C6 1.424(2) . ?
C2 C3 1.376(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.359(2) . ?
C5 C6 1.415(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.430(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(2) . ?
C8 C16 1.415(2) . ?
C9 C10 1.412(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.417(2) . ?
C11 H11 0.9500 . ?
C12 C16 1.413(2) . ?
C12 C13 1.417(2) . ?
C13 C14 1.366(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.405(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C17 C18 1.417(2) . ?
C17 C22 1.424(2) . ?
C18 C19 1.382(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.397(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.407(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.444(2) . ?
C23 H23 0.9500 . ?
C25 C26 1.409(3) . ?
C25 C30 1.419(3) . ?
C26 C27 1.382(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.376(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.354(3) . ?
C29 C30 1.415(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.438(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.376(2) . ?
C32 C40 1.423(2) . ?
C33 C34 1.415(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.355(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.417(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.413(3) . ?
C36 C40 1.415(2) . ?
C37 C38 1.358(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.402(3) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C41 C42 1.410(2) . ?
C41 C46 1.417(2) . ?
C42 C43 1.376(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.397(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.378(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.411(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.438(2) . ?
C47 H47 0.9500 . ?
C49 C50 1.452(4) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.450(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C55 C56 1.437(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C60 C61 1.455(10) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N15 C61 1.146(6) . ?
N15 N15 1.602(10) 2_665 ?
C63 N16 1.130(7) . ?
C63 C62 1.462(11) . ?
C64 C65 1.473(9) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 N17 1.173(7) . ?
N18 C67 1.176(8) . ?
C67 C66 1.454(10) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 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 90.40(6) . . ?
O1 Fe1 N1 95.56(6) . . ?
O2 Fe1 N1 89.55(6) . . ?
O1 Fe1 N3 87.12(6) . . ?
O2 Fe1 N3 95.30(6) . . ?
N1 Fe1 N3 174.44(5) . . ?
O1 Fe1 N2 177.33(5) . . ?
O2 Fe1 N2 87.34(6) . . ?
N1 Fe1 N2 83.00(6) . . ?
N3 Fe1 N2 94.50(6) . . ?
O1 Fe1 S1 93.05(4) . . ?
O2 Fe1 S1 176.54(4) . . ?
N1 Fe1 S1 89.86(6) . . ?
N3 Fe1 S1 85.14(6) . . ?
N2 Fe1 S1 89.20(5) . . ?
O4 Fe2 O3 90.51(6) . . ?
O4 Fe2 N9 86.46(7) . . ?
O3 Fe2 N9 104.13(6) . . ?
O4 Fe2 N7 87.39(6) . . ?
O3 Fe2 N7 160.91(5) . . ?
N9 Fe2 N7 94.68(6) . . ?
O4 Fe2 N6 109.08(6) . . ?
O3 Fe2 N6 86.91(6) . . ?
N9 Fe2 N6 161.08(5) . . ?
N7 Fe2 N6 75.90(6) . . ?
O4 Fe2 S2 165.20(4) . . ?
O3 Fe2 S2 96.87(4) . . ?
N9 Fe2 S2 79.32(6) . . ?
N7 Fe2 S2 89.69(5) . . ?
N6 Fe2 S2 84.20(6) . . ?
C24 S1 Fe1 96.32(7) . . ?
C48 S2 Fe2 97.47(7) . . ?
C1 O1 Fe1 125.69(10) . . ?
C17 O2 Fe1 125.19(10) . . ?
C25 O3 Fe2 130.38(11) . . ?
C41 O4 Fe2 135.95(10) . . ?
C7 N1 C8 121.21(12) . . ?
C7 N1 Fe1 125.06(10) . . ?
C8 N1 Fe1 113.73(10) . . ?
C15 N2 C16 119.00(14) . . ?
C15 N2 Fe1 128.39(11) . . ?
C16 N2 Fe1 112.61(10) . . ?
C23 N3 N4 113.93(12) . . ?
C23 N3 Fe1 124.26(11) . . ?
N4 N3 Fe1 121.79(10) . . ?
C24 N4 N3 113.04(12) . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C31 N6 C32 120.01(14) . . ?
C31 N6 Fe2 123.80(12) . . ?
C32 N6 Fe2 115.21(10) . . ?
C39 N7 C40 119.16(16) . . ?
C39 N7 Fe2 124.26(13) . . ?
C40 N7 Fe2 116.55(11) . . ?
C48 N8 N9 114.85(12) . . ?
C47 N9 N8 112.57(12) . . ?
C47 N9 Fe2 124.87(10) . . ?
N8 N9 Fe2 122.56(10) . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
O1 C1 C2 117.17(14) . . ?
O1 C1 C6 125.07(13) . . ?
C2 C1 C6 117.77(14) . . ?
C3 C2 C1 121.77(15) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 118.77(15) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 F1 119.47(16) . . ?
C5 C4 C3 122.39(16) . . ?
F1 C4 C3 118.15(16) . . ?
C4 C5 C6 119.83(15) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 119.45(14) . . ?
C5 C6 C7 116.92(14) . . ?
C1 C6 C7 123.62(13) . . ?
N1 C7 C6 124.84(13) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C9 C8 C16 119.33(13) . . ?
C9 C8 N1 127.43(14) . . ?
C16 C8 N1 113.24(12) . . ?
C8 C9 C10 119.67(14) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 121.69(15) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 120.00(15) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C16 C12 C13 117.16(15) . . ?
C16 C12 C11 118.22(15) . . ?
C13 C12 C11 124.60(15) . . ?
C14 C13 C12 119.46(16) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.88(16) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N2 C15 C14 122.16(16) . . ?
N2 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
N2 C16 C12 122.25(14) . . ?
N2 C16 C8 116.69(13) . . ?
C12 C16 C8 121.05(14) . . ?
O2 C17 C18 118.23(14) . . ?
O2 C17 C22 124.38(14) . . ?
C18 C17 C22 117.39(15) . . ?
C19 C18 C17 121.66(16) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C18 C19 C20 120.72(17) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 118.73(17) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 122.16(16) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C17 119.33(14) . . ?
C21 C22 C23 116.74(14) . . ?
C17 C22 C23 123.92(14) . . ?
N3 C23 C22 125.49(14) . . ?
N3 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
N4 C24 N5 119.34(13) . . ?
N4 C24 S1 123.60(11) . . ?
N5 C24 S1 117.02(11) . . ?
O3 C25 C26 119.26(18) . . ?
O3 C25 C30 122.66(16) . . ?
C26 C25 C30 118.07(17) . . ?
C27 C26 C25 121.2(2) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C26 119.3(2) . . ?
C28 C27 H27 120.4 . . ?
C26 C27 H27 120.4 . . ?
C29 C28 F2 119.5(3) . . ?
C29 C28 C27 122.2(2) . . ?
F2 C28 C27 118.3(2) . . ?
C28 C29 C30 120.0(2) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 119.24(18) . . ?
C29 C30 C31 116.56(18) . . ?
C25 C30 C31 124.20(15) . . ?
N6 C31 C30 126.20(16) . . ?
N6 C31 H31 116.9 . . ?
C30 C31 H31 116.9 . . ?
C33 C32 N6 126.80(17) . . ?
C33 C32 C40 118.36(17) . . ?
N6 C32 C40 114.83(14) . . ?
C32 C33 C34 120.21(19) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 122.10(18) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 118.9 . . ?
C34 C35 C36 119.61(18) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C37 C36 C40 117.52(18) . . ?
C37 C36 C35 123.90(18) . . ?
C40 C36 C35 118.58(19) . . ?
C38 C37 C36 119.86(19) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 119.2(2) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N7 C39 C38 122.7(2) . . ?
N7 C39 H39 118.6 . . ?
C38 C39 H39 118.6 . . ?
N7 C40 C36 121.53(17) . . ?
N7 C40 C32 117.37(15) . . ?
C36 C40 C32 121.09(16) . . ?
O4 C41 C42 120.02(14) . . ?
O4 C41 C46 121.89(13) . . ?
C42 C41 C46 118.09(15) . . ?
C43 C42 C41 121.06(16) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C42 C43 C44 121.13(16) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C45 C44 C43 118.87(17) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C44 C45 C46 121.44(16) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 H45 119.3 . . ?
C45 C46 C41 119.41(14) . . ?
C45 C46 C47 117.80(14) . . ?
C41 C46 C47 122.79(14) . . ?
N9 C47 C46 127.06(13) . . ?
N9 C47 H47 116.5 . . ?
C46 C47 H47 116.5 . . ?
N8 C48 N10 116.99(14) . . ?
N8 C48 S2 125.68(12) . . ?
N10 C48 S2 117.30(12) . . ?
N11 C49 C50 176.7(3) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N12 C51 C52 178.3(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N13 C55 C56 179.2(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 N15 N15 161.8(6) . 2_665 ?
N15 C61 C60 178.3(9) . . ?
N16 C63 C62 178.7(11) . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N17 C65 C64 177.3(13) . . ?
N18 C67 C66 178.9(12) . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C67 C66 H66A 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C67 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_refine_diff_density_max         0.729
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100K_a
_database_code_depnum_ccdc_archive 'CCDC 1529170'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(qsal-F)(thsa)]2.5MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H49 F2 Fe2 N15 O4 S2'
_chemical_formula_weight         1233.94

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.028(3)
_cell_length_b                   16.447(3)
_cell_length_c                   16.435(3)
_cell_angle_alpha                60.35(3)
_cell_angle_beta                 109.39(3)
_cell_angle_gamma                110.82(3)
_cell_volume                     2807.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15730
_cell_measurement_theta_min      0.820
_cell_measurement_theta_max      31.792

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.660
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
;
This strcutures has been solved and refined by reasonable model.
Two molecules of MeCN are disorderd over 4 position (molecules of N15-N18). Firstly, the free variables over 
the positions were applied and the overall occupancy were about two. Therefore, SUMP command was applied to set overall
MeCN over 4 positions to be two. ISOR command was used on the positions that showed severely disoder after the anisotropy 
application.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1, Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60189
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.453
_diffrn_reflns_theta_max         31.792
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             15730
_reflns_number_gt                10896
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0821P)²+11.1543P]
 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         15730
_refine_ls_number_parameters     813
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2432
_refine_ls_wR_factor_gt          0.2150
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.094
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.59175(5) 0.20973(4) 0.53460(4) 0.02755(15) Uani 1 1 d . . . . .
Fe2 Fe 0.52185(6) 0.75221(5) -0.07476(5) 0.03213(16) Uani 1 1 d . . . . .
S1 S 0.48534(10) 0.21014(8) 0.39658(7) 0.0296(2) Uani 1 1 d . . . . .
S2 S 0.63967(11) 0.75750(8) 0.06939(8) 0.0351(3) Uani 1 1 d . . . . .
O1 O 0.7231(3) 0.2202(2) 0.5021(2) 0.0323(7) Uani 1 1 d . . . . .
F1 F 0.9168(3) -0.0643(2) 0.5846(3) 0.0562(9) Uani 1 1 d . . . . .
O4 O 0.4091(3) 0.7246(3) -0.1720(2) 0.0395(8) Uani 1 1 d . . . . .
O2 O 0.6743(3) 0.2078(2) 0.6552(2) 0.0363(7) Uani 1 1 d . . . . .
N1 N 0.5520(3) 0.0710(3) 0.5945(2) 0.0275(7) Uani 1 1 d . . . . .
N8 N 0.5126(3) 0.5756(3) 0.1186(2) 0.0306(8) Uani 1 1 d . . . . .
N4 N 0.5674(3) 0.3949(3) 0.3712(2) 0.0298(7) Uani 1 1 d . . . . .
O3 O 0.6341(3) 0.7439(3) -0.1232(4) 0.0566(11) Uani 1 1 d . . . . .
N9 N 0.4706(3) 0.6090(3) 0.0206(2) 0.0286(7) Uani 1 1 d . . . . .
N5 N 0.4547(3) 0.3693(3) 0.2414(2) 0.0325(8) Uani 1 1 d . . . . .
H5A H 0.4613 0.4317 0.2074 0.039 Uiso 1 1 calc R U . . .
H5B H 0.4139 0.3295 0.2154 0.039 Uiso 1 1 calc R U . . .
N10 N 0.6309(4) 0.6119(3) 0.2398(3) 0.0361(9) Uani 1 1 d . . . . .
H10A H 0.6068 0.5527 0.2808 0.043 Uiso 1 1 calc R U . . .
H10B H 0.6824 0.6531 0.2602 0.043 Uiso 1 1 calc R U . . .
N2 N 0.4564(3) 0.1952(3) 0.5752(2) 0.0308(8) Uani 1 1 d . . . . .
N3 N 0.6195(3) 0.3493(3) 0.4666(2) 0.0292(7) Uani 1 1 d . . . . .
N6 N 0.5823(4) 0.9028(3) -0.1360(3) 0.0391(9) Uani 1 1 d . . . . .
N7 N 0.4049(4) 0.8004(4) -0.0560(3) 0.0455(10) Uani 1 1 d . . . . .
C9 C 0.3916(4) -0.0634(3) 0.6607(3) 0.0317(9) Uani 1 1 d . . . . .
H9 H 0.4226 -0.1108 0.6669 0.038 Uiso 1 1 calc R U . . .
F2 F 1.0355(4) 0.9807(5) -0.2110(3) 0.1029(19) Uani 1 1 d . . . . .
C10 C 0.2884(4) -0.0913(4) 0.6894(3) 0.0345(10) Uani 1 1 d . . . . .
H10 H 0.2507 -0.1573 0.7146 0.041 Uiso 1 1 calc R U . . .
C8 C 0.4467(4) 0.0313(3) 0.6243(3) 0.0289(8) Uani 1 1 d . . . . .
C47 C 0.4002(4) 0.5425(3) -0.0036(3) 0.0303(9) Uani 1 1 d . . . . .
H47 H 0.3881 0.4793 0.0461 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2964(4) 0.0749(4) 0.6438(3) 0.0338(9) Uani 1 1 d . . . . .
C1 C 0.7639(4) 0.1477(3) 0.5232(3) 0.0302(9) Uani 1 1 d . . . . .
C24 C 0.5071(4) 0.3348(3) 0.3335(3) 0.0284(8) Uani 1 1 d . . . . .
C7 C 0.6128(4) 0.0159(3) 0.6076(3) 0.0303(9) Uani 1 1 d . . . . .
H7 H 0.5867 -0.0516 0.6413 0.036 Uiso 1 1 calc R U . . .
C46 C 0.3380(4) 0.5537(3) -0.0978(3) 0.0328(9) Uani 1 1 d . . . . .
C41 C 0.3435(4) 0.6450(4) -0.1781(3) 0.0352(10) Uani 1 1 d . . . . .
C11 C 0.2426(4) -0.0233(4) 0.6811(3) 0.0350(10) Uani 1 1 d . . . . .
H11 H 0.1735 -0.0431 0.7007 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3989(4) 0.1017(3) 0.6138(3) 0.0294(8) Uani 1 1 d . . . . .
C17 C 0.7442(4) 0.2823(4) 0.6686(3) 0.0349(10) Uani 1 1 d . . . . .
C40 C 0.4241(5) 0.8955(4) -0.0861(3) 0.0406(11) Uani 1 1 d . . . . .
C6 C 0.7150(4) 0.0489(3) 0.5752(3) 0.0308(9) Uani 1 1 d . . . . .
C42 C 0.2757(4) 0.6470(5) -0.2660(3) 0.0484(14) Uani 1 1 d . . . . .
H42 H 0.2763 0.7071 -0.3205 0.058 Uiso 1 1 calc R U . . .
C48 C 0.5888(4) 0.6396(3) 0.1451(3) 0.0314(9) Uani 1 1 d . . . . .
C23 C 0.6868(4) 0.4073(3) 0.5024(3) 0.0326(9) Uani 1 1 d . . . . .
H23 H 0.6946 0.4742 0.4625 0.039 Uiso 1 1 calc R U . . .
C22 C 0.7522(4) 0.3793(4) 0.5990(3) 0.0334(9) Uani 1 1 d . . . . .
C32 C 0.5188(5) 0.9540(4) -0.1301(3) 0.0405(11) Uani 1 1 d . . . . .
C2 C 0.8643(4) 0.1700(4) 0.4924(3) 0.0368(10) Uani 1 1 d . . . . .
H2 H 0.8977 0.2354 0.4569 0.044 Uiso 1 1 calc R U . . .
C31 C 0.6768(5) 0.9451(4) -0.1629(3) 0.0441(12) Uani 1 1 d . . . . .
H31 H 0.6983 1.0130 -0.1849 0.053 Uiso 1 1 calc R U . . .
C21 C 0.8298(4) 0.4537(4) 0.6218(4) 0.0382(10) Uani 1 1 d . . . . .
H21 H 0.8343 0.5185 0.5752 0.046 Uiso 1 1 calc R U . . .
C4 C 0.8659(4) 0.0054(4) 0.5640(4) 0.0406(11) Uani 1 1 d . . . . .
C3 C 0.9143(4) 0.1005(4) 0.5123(3) 0.0398(11) Uani 1 1 d . . . . .
H3 H 0.9814 0.1172 0.4909 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2584(4) 0.1497(4) 0.6350(4) 0.0415(11) Uani 1 1 d . . . . .
H13 H 0.1903 0.1358 0.6539 0.050 Uiso 1 1 calc R U . . .
C5 C 0.7687(4) -0.0210(4) 0.5941(3) 0.0375(10) Uani 1 1 d . . . . .
H5 H 0.7366 -0.0872 0.6281 0.045 Uiso 1 1 calc R U . . .
C45 C 0.2675(4) 0.4711(4) -0.1094(4) 0.0412(11) Uani 1 1 d . . . . .
H45 H 0.2635 0.4105 -0.0553 0.049 Uiso 1 1 calc R U . . .
N12 N 1.1423(5) 0.2909(5) 0.6698(5) 0.0704(17) Uani 1 1 d . . . . .
N11 N 0.8563(5) 0.9978(5) 0.0002(5) 0.0659(15) Uani 1 1 d . . . . .
C30 C 0.7535(5) 0.9004(5) -0.1631(4) 0.0479(13) Uani 1 1 d . . . . .
C19 C 0.8933(5) 0.3412(4) 0.7772(4) 0.0457(12) Uani 1 1 d . . . . .
H19 H 0.9423 0.3280 0.8375 0.055 Uiso 1 1 calc R U . . .
C20 C 0.8988(4) 0.4353(4) 0.7094(4) 0.0448(12) Uani 1 1 d . . . . .
H20 H 0.9499 0.4867 0.7234 0.054 Uiso 1 1 calc R U . . .
C15 C 0.4197(4) 0.2635(4) 0.5690(4) 0.0385(10) Uani 1 1 d . . . . .
H15 H 0.4610 0.3283 0.5436 0.046 Uiso 1 1 calc R U . . .
C43 C 0.2087(5) 0.5642(5) -0.2750(4) 0.0539(16) Uani 1 1 d . . . . .
H43 H 0.1652 0.5681 -0.3354 0.065 Uiso 1 1 calc R U . . .
C14 C 0.3199(5) 0.2421(4) 0.5993(4) 0.0434(12) Uani 1 1 d . . . . .
H14 H 0.2954 0.2924 0.5949 0.052 Uiso 1 1 calc R U . . .
C33 C 0.5395(6) 1.0523(4) -0.1625(4) 0.0520(14) Uani 1 1 d . . . . .
H33 H 0.6005 1.0934 -0.1940 0.062 Uiso 1 1 calc R U . . .
C36 C 0.3529(5) 0.9369(5) -0.0748(4) 0.0482(13) Uani 1 1 d . . . . .
C51 C 1.0685(5) 0.3216(5) 0.6187(4) 0.0480(13) Uani 1 1 d . . . . .
C25 C 0.7303(5) 0.8028(5) -0.1405(4) 0.0511(14) Uani 1 1 d . . . . .
C18 C 0.8172(5) 0.2659(4) 0.7583(4) 0.0435(11) Uani 1 1 d . . . . .
H18 H 0.8139 0.2019 0.8064 0.052 Uiso 1 1 calc R U . . .
C35 C 0.3796(6) 1.0368(5) -0.1068(4) 0.0542(15) Uani 1 1 d . . . . .
H35 H 0.3344 1.0657 -0.0988 0.065 Uiso 1 1 calc R U . . .
C44 C 0.2044(5) 0.4752(5) -0.1964(4) 0.0523(14) Uani 1 1 d . . . . .
H44 H 0.1585 0.4183 -0.2027 0.063 Uiso 1 1 calc R U . . .
C34 C 0.4692(6) 1.0924(4) -0.1489(4) 0.0552(16) Uani 1 1 d . . . . .
H34 H 0.4859 1.1601 -0.1699 0.066 Uiso 1 1 calc R U . . .
C37 C 0.2612(5) 0.8729(5) -0.0315(5) 0.0584(16) Uani 1 1 d . . . . .
H37 H 0.2118 0.8974 -0.0227 0.070 Uiso 1 1 calc R U . . .
C39 C 0.3153(5) 0.7427(5) -0.0163(6) 0.0613(18) Uani 1 1 d . . . . .
H39 H 0.3013 0.6756 0.0030 0.074 Uiso 1 1 calc R U . . .
N13 N 0.0792(5) 0.3244(4) 0.3907(5) 0.0757(19) Uani 1 1 d . . . . .
C29 C 0.8587(6) 0.9600(6) -0.1868(4) 0.0652(19) Uani 1 1 d . . . . .
H29 H 0.8752 1.0268 -0.2034 0.078 Uiso 1 1 calc R U . . .
C52 C 0.9745(5) 0.3608(5) 0.5511(6) 0.0627(17) Uani 1 1 d . . . . .
H52A H 0.9906 0.3942 0.4865 0.094 Uiso 1 1 calc R U . . .
H52B H 0.9621 0.4064 0.5669 0.094 Uiso 1 1 calc R U . . .
H52C H 0.9073 0.3085 0.5541 0.094 Uiso 1 1 calc R U . . .
C28 C 0.9358(6) 0.9211(8) -0.1859(5) 0.077(3) Uani 1 1 d . . . . .
C55 C 0.1438(5) 0.3074(4) 0.3713(5) 0.0524(14) Uani 1 1 d . . . . .
C26 C 0.8160(5) 0.7665(6) -0.1404(5) 0.0651(19) Uani 1 1 d . . . . .
H26 H 0.8021 0.7001 -0.1245 0.078 Uiso 1 1 calc R U . . .
C27 C 0.9155(6) 0.8248(8) -0.1624(6) 0.075(2) Uani 1 1 d . . . . .
H27 H 0.9712 0.7996 -0.1618 0.090 Uiso 1 1 calc R U . . .
C50 C 0.9290(6) 0.8392(5) 0.0896(6) 0.073(2) Uani 1 1 d . . . . .
H50A H 0.8878 0.7983 0.0560 0.110 Uiso 1 1 calc R U . . .
H50B H 0.9188 0.8042 0.1560 0.110 Uiso 1 1 calc R U . . .
H50C H 1.0088 0.8569 0.0880 0.110 Uiso 1 1 calc R U . . .
C49 C 0.8870(6) 0.9258(5) 0.0432(5) 0.0582(15) Uani 1 1 d . . . . .
C38 C 0.2418(6) 0.7764(6) -0.0020(6) 0.071(2) Uani 1 1 d . . . . .
H38 H 0.1798 0.7333 0.0276 0.085 Uiso 1 1 calc R U . . .
C60 C 0.628(2) 0.425(3) 0.7324(15) 0.073(7) Uani 0.517(3) 1 d D . P A 2
H60A H 0.7054 0.4265 0.7372 0.110 Uiso 0.517(3) 1 calc R U P A 2
H60B H 0.5874 0.3590 0.7655 0.110 Uiso 0.517(3) 1 calc R U P A 2
H60C H 0.6274 0.4645 0.7618 0.110 Uiso 0.517(3) 1 calc R U P A 2
C56 C 0.2263(8) 0.2892(7) 0.3485(6) 0.086(3) Uani 1 1 d . . . . .
H56A H 0.2021 0.2938 0.2835 0.130 Uiso 1 1 calc R U . . .
H56B H 0.2373 0.2244 0.3935 0.130 Uiso 1 1 calc R U . . .
H56C H 0.2968 0.3366 0.3529 0.130 Uiso 1 1 calc R U . . .
N15 N 0.5322(9) 0.4946(7) 0.5514(7) 0.058(3) Uani 0.517(3) 1 d D . P A 2
C61 C 0.5729(10) 0.4651(9) 0.6306(8) 0.053(3) Uani 0.517(3) 1 d D . P A 2
N17 N 0.8561(12) 0.5049(17) 0.8898(12) 0.173(10) Uani 0.634(3) 1 d D . P B 5
C63 C 0.2800(11) 0.5291(11) 0.1857(10) 0.067(4) Uani 0.526(3) 1 d D . P C 3
C62 C 0.366(3) 0.565(3) 0.254(3) 0.118(15) Uani 0.526(3) 1 d D . P C 3
H62A H 0.4220 0.6194 0.2204 0.177 Uiso 0.526(3) 1 calc R U P C 3
H62B H 0.4016 0.5133 0.3047 0.177 Uiso 0.526(3) 1 calc R U P C 3
H62C H 0.3296 0.5857 0.2820 0.177 Uiso 0.526(3) 1 calc R U P C 3
C64 C 1.0611(14) 0.6037(18) 0.8680(19) 0.140(12) Uani 0.634(3) 1 d D . P B 5
H64A H 1.1067 0.6010 0.9298 0.210 Uiso 0.634(3) 1 calc R U P B 5
H64B H 1.0572 0.6704 0.8240 0.210 Uiso 0.634(3) 1 calc R U P B 5
H64C H 1.0951 0.5795 0.8418 0.210 Uiso 0.634(3) 1 calc R U P B 5
C65 C 0.9468(12) 0.5436(13) 0.8806(11) 0.096(5) Uani 0.634(3) 1 d D . P B 5
N16 N 0.2197(11) 0.5041(12) 0.1294(10) 0.089(5) Uani 0.526(3) 1 d D . P C 3
N18 N -0.010(2) 0.6069(15) 0.0329(19) 0.104(8) Uani 0.323(3) 1 d D U P D 4
C67 C -0.035(3) 0.5243(15) 0.072(2) 0.093(8) Uani 0.323(3) 1 d D U P D 4
C66 C -0.063(3) 0.4190(12) 0.1311(19) 0.039(5) Uani 0.323(3) 1 d D U P D 4
H66A H -0.0731 0.4064 0.1931 0.059 Uiso 0.323(3) 1 calc R U P D 4
H66B H -0.0022 0.3917 0.1405 0.059 Uiso 0.323(3) 1 calc R U P D 4
H66C H -0.1326 0.3892 0.0988 0.059 Uiso 0.323(3) 1 calc R U P D 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.884(3) . ?
Fe1 O2 1.906(3) . ?
Fe1 N1 1.929(4) . ?
Fe1 N3 1.946(4) . ?
Fe1 N2 1.984(4) . ?
Fe1 S1 2.2295(15) . ?
Fe2 O4 1.899(4) . ?
Fe2 O3 1.954(4) . ?
Fe2 N9 2.091(4) . ?
Fe2 N6 2.107(5) . ?
Fe2 N7 2.111(4) . ?
Fe2 S2 2.3812(16) . ?
S1 C24 1.743(4) . ?
S2 C48 1.731(5) . ?
O1 C1 1.320(5) . ?
F1 C4 1.370(6) . ?
O4 C41 1.316(6) . ?
O2 C17 1.311(6) . ?
N1 C7 1.303(5) . ?
N1 C8 1.429(5) . ?
N8 C48 1.306(6) . ?
N8 N9 1.396(5) . ?
N4 C24 1.306(6) . ?
N4 N3 1.406(5) . ?
O3 C25 1.301(7) . ?
N9 C47 1.293(6) . ?
N5 C24 1.349(5) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N10 C48 1.356(5) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N2 C15 1.318(6) . ?
N2 C16 1.364(6) . ?
N3 C23 1.282(6) . ?
N6 C31 1.282(7) . ?
N6 C32 1.426(7) . ?
N7 C40 1.338(7) . ?
N7 C39 1.340(7) . ?
C9 C8 1.366(6) . ?
C9 C10 1.417(6) . ?
C9 H9 0.9500 . ?
F2 C28 1.367(8) . ?
C10 C11 1.375(7) . ?
C10 H10 0.9500 . ?
C8 C16 1.415(6) . ?
C47 C46 1.441(6) . ?
C47 H47 0.9500 . ?
C12 C11 1.407(7) . ?
C12 C13 1.411(7) . ?
C12 C16 1.422(6) . ?
C1 C2 1.420(6) . ?
C1 C6 1.424(6) . ?
C7 C6 1.423(6) . ?
C7 H7 0.9500 . ?
C46 C45 1.407(7) . ?
C46 C41 1.423(6) . ?
C41 C42 1.413(7) . ?
C11 H11 0.9500 . ?
C17 C18 1.417(7) . ?
C17 C22 1.421(7) . ?
C40 C32 1.425(8) . ?
C40 C36 1.430(7) . ?
C6 C5 1.407(6) . ?
C42 C43 1.381(9) . ?
C42 H42 0.9500 . ?
C23 C22 1.454(6) . ?
C23 H23 0.9500 . ?
C22 C21 1.409(7) . ?
C32 C33 1.380(8) . ?
C2 C3 1.362(7) . ?
C2 H2 0.9500 . ?
C31 C30 1.438(8) . ?
C31 H31 0.9500 . ?
C21 C20 1.369(7) . ?
C21 H21 0.9500 . ?
C4 C5 1.360(7) . ?
C4 C3 1.381(8) . ?
C3 H3 0.9500 . ?
C13 C14 1.364(8) . ?
C13 H13 0.9500 . ?
C5 H5 0.9500 . ?
C45 C44 1.375(7) . ?
C45 H45 0.9500 . ?
N12 C51 1.129(8) . ?
N11 C49 1.176(9) . ?
C30 C25 1.395(9) . ?
C30 C29 1.419(9) . ?
C19 C20 1.382(8) . ?
C19 C18 1.384(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C15 C14 1.412(7) . ?
C15 H15 0.9500 . ?
C43 C44 1.390(9) . ?
C43 H43 0.9500 . ?
C14 H14 0.9500 . ?
C33 C34 1.426(8) . ?
C33 H33 0.9500 . ?
C36 C35 1.399(9) . ?
C36 C37 1.403(9) . ?
C51 C52 1.449(9) . ?
C25 C26 1.441(8) . ?
C18 H18 0.9500 . ?
C35 C34 1.353(10) . ?
C35 H35 0.9500 . ?
C44 H44 0.9500 . ?
C34 H34 0.9500 . ?
C37 C38 1.361(10) . ?
C37 H37 0.9500 . ?
C39 C38 1.391(8) . ?
C39 H39 0.9500 . ?
N13 C55 1.151(8) . ?
C29 C28 1.363(11) . ?
C29 H29 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C28 C27 1.376(13) . ?
C55 C56 1.411(9) . ?
C26 C27 1.347(11) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C50 C49 1.453(10) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C38 H38 0.9500 . ?
C60 C61 1.482(18) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
N15 C61 1.145(11) . ?
N15 N15 1.57(2) 2_666 ?
N17 C65 1.146(12) . ?
C63 N16 1.143(12) . ?
C63 C62 1.485(18) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C64 C65 1.481(17) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
N18 C67 1.151(13) . ?
C67 C66 1.483(18) . ?
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 90.48(15) . . ?
O1 Fe1 N1 95.55(15) . . ?
O2 Fe1 N1 88.94(15) . . ?
O1 Fe1 N3 87.00(15) . . ?
O2 Fe1 N3 95.27(16) . . ?
N1 Fe1 N3 175.07(16) . . ?
O1 Fe1 N2 177.31(14) . . ?
O2 Fe1 N2 87.20(15) . . ?
N1 Fe1 N2 83.05(15) . . ?
N3 Fe1 N2 94.57(16) . . ?
O1 Fe1 S1 93.14(11) . . ?
O2 Fe1 S1 176.36(11) . . ?
N1 Fe1 S1 90.35(12) . . ?
N3 Fe1 S1 85.29(12) . . ?
N2 Fe1 S1 89.18(12) . . ?
O4 Fe2 O3 89.59(17) . . ?
O4 Fe2 N9 88.14(15) . . ?
O3 Fe2 N9 101.66(18) . . ?
O4 Fe2 N6 105.34(16) . . ?
O3 Fe2 N6 87.87(18) . . ?
N9 Fe2 N6 163.67(15) . . ?
O4 Fe2 N7 87.17(17) . . ?
O3 Fe2 N7 163.5(2) . . ?
N9 Fe2 N7 94.38(17) . . ?
N6 Fe2 N7 77.45(18) . . ?
O4 Fe2 S2 167.82(11) . . ?
O3 Fe2 S2 96.95(14) . . ?
N9 Fe2 S2 80.50(11) . . ?
N6 Fe2 S2 85.24(12) . . ?
N7 Fe2 S2 89.33(14) . . ?
C24 S1 Fe1 96.10(16) . . ?
C48 S2 Fe2 97.11(17) . . ?
C1 O1 Fe1 125.7(3) . . ?
C41 O4 Fe2 134.2(3) . . ?
C17 O2 Fe1 125.2(3) . . ?
C7 N1 C8 121.3(4) . . ?
C7 N1 Fe1 124.9(3) . . ?
C8 N1 Fe1 113.8(3) . . ?
C48 N8 N9 114.9(4) . . ?
C24 N4 N3 113.2(3) . . ?
C25 O3 Fe2 128.7(4) . . ?
C47 N9 N8 113.1(4) . . ?
C47 N9 Fe2 124.8(3) . . ?
N8 N9 Fe2 122.1(3) . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C15 N2 C16 119.7(4) . . ?
C15 N2 Fe1 127.7(3) . . ?
C16 N2 Fe1 112.6(3) . . ?
C23 N3 N4 114.2(4) . . ?
C23 N3 Fe1 124.4(3) . . ?
N4 N3 Fe1 121.4(3) . . ?
C31 N6 C32 121.3(5) . . ?
C31 N6 Fe2 123.7(4) . . ?
C32 N6 Fe2 114.1(3) . . ?
C40 N7 C39 119.2(5) . . ?
C40 N7 Fe2 116.3(4) . . ?
C39 N7 Fe2 124.5(4) . . ?
C8 C9 C10 120.5(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C11 C10 C9 120.4(5) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C9 C8 C16 119.5(4) . . ?
C9 C8 N1 127.5(4) . . ?
C16 C8 N1 113.1(4) . . ?
N9 C47 C46 127.2(4) . . ?
N9 C47 H47 116.4 . . ?
C46 C47 H47 116.4 . . ?
C11 C12 C13 125.4(4) . . ?
C11 C12 C16 117.8(4) . . ?
C13 C12 C16 116.8(4) . . ?
O1 C1 C2 117.6(4) . . ?
O1 C1 C6 124.8(4) . . ?
C2 C1 C6 117.6(4) . . ?
N4 C24 N5 119.3(4) . . ?
N4 C24 S1 123.9(3) . . ?
N5 C24 S1 116.8(3) . . ?
N1 C7 C6 125.1(4) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
C45 C46 C41 119.4(4) . . ?
C45 C46 C47 118.1(4) . . ?
C41 C46 C47 122.4(5) . . ?
O4 C41 C42 120.7(4) . . ?
O4 C41 C46 122.2(4) . . ?
C42 C41 C46 117.1(5) . . ?
C10 C11 C12 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
N2 C16 C8 116.9(4) . . ?
N2 C16 C12 122.2(4) . . ?
C8 C16 C12 120.9(4) . . ?
O2 C17 C18 118.3(4) . . ?
O2 C17 C22 124.4(4) . . ?
C18 C17 C22 117.2(5) . . ?
N7 C40 C32 117.1(5) . . ?
N7 C40 C36 121.7(5) . . ?
C32 C40 C36 121.2(5) . . ?
C5 C6 C7 117.5(4) . . ?
C5 C6 C1 118.7(4) . . ?
C7 C6 C1 123.8(4) . . ?
C43 C42 C41 121.9(5) . . ?
C43 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
N8 C48 N10 117.5(4) . . ?
N8 C48 S2 125.3(3) . . ?
N10 C48 S2 117.1(4) . . ?
N3 C23 C22 125.5(4) . . ?
N3 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
C21 C22 C17 119.5(4) . . ?
C21 C22 C23 116.8(4) . . ?
C17 C22 C23 123.7(4) . . ?
C33 C32 C40 118.0(5) . . ?
C33 C32 N6 126.9(5) . . ?
C40 C32 N6 115.0(5) . . ?
C3 C2 C1 122.1(5) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
N6 C31 C30 126.8(6) . . ?
N6 C31 H31 116.6 . . ?
C30 C31 H31 116.6 . . ?
C20 C21 C22 121.7(5) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C5 C4 F1 119.3(5) . . ?
C5 C4 C3 121.9(5) . . ?
F1 C4 C3 118.9(4) . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C13 C12 119.6(4) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C44 C45 C46 122.1(5) . . ?
C44 C45 H45 119.0 . . ?
C46 C45 H45 119.0 . . ?
C25 C30 C29 119.2(6) . . ?
C25 C30 C31 123.7(5) . . ?
C29 C30 C31 117.2(6) . . ?
C20 C19 C18 120.8(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C21 C20 C19 119.4(5) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
N2 C15 C14 121.2(5) . . ?
N2 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C42 C43 C44 120.7(5) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C13 C14 C15 120.4(5) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C32 C33 C34 120.1(6) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C36 C37 125.1(6) . . ?
C35 C36 C40 118.2(6) . . ?
C37 C36 C40 116.7(6) . . ?
N12 C51 C52 178.5(7) . . ?
O3 C25 C30 123.5(5) . . ?
O3 C25 C26 118.4(6) . . ?
C30 C25 C26 118.1(6) . . ?
C19 C18 C17 121.4(5) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C34 C35 C36 120.5(5) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C45 C44 C43 118.8(6) . . ?
C45 C44 H44 120.6 . . ?
C43 C44 H44 120.6 . . ?
C35 C34 C33 121.8(6) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C38 C37 C36 121.3(5) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
N7 C39 C38 123.2(7) . . ?
N7 C39 H39 118.4 . . ?
C38 C39 H39 118.4 . . ?
C28 C29 C30 119.7(8) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C29 C28 F2 118.4(9) . . ?
C29 C28 C27 122.2(7) . . ?
F2 C28 C27 119.4(8) . . ?
N13 C55 C56 177.7(8) . . ?
C27 C26 C25 121.4(8) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 119.5(7) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N11 C49 C50 175.3(7) . . ?
C37 C38 C39 118.0(6) . . ?
C37 C38 H38 121.0 . . ?
C39 C38 H38 121.0 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C61 N15 N15 164.4(14) . 2_666 ?
N15 C61 C60 178.0(19) . . ?
N16 C63 C62 175(2) . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N17 C65 C64 173(2) . . ?
N18 C67 C66 174(3) . . ?
C67 C66 H66A 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C67 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_refine_diff_density_max         1.093
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.116

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_295K_a
_database_code_depnum_ccdc_archive 'CCDC 1529173'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(qsal-F)(thsa)]2.5MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H49 F2 Fe2 N15 O4 S2'
_chemical_formula_weight         1233.94

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.300(3)
_cell_length_b                   16.543(3)
_cell_length_c                   16.559(3)
_cell_angle_alpha                60.50(3)
_cell_angle_beta                 71.52(3)
_cell_angle_gamma                69.61(3)
_cell_volume                     2924.6(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    16505
_cell_measurement_theta_min      0.819
_cell_measurement_theta_max      31.906

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.634
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
;
This strcutures has been solved and refined by reasonable model.
The acetonitril molecules, N11 and N11', are disorder over two position and the total occupancy is one. 
Two molecules of MeCN are disorderd over 4 position (molecules of N15-N18). This has been treated the same as the structure at 100 K that shows no solvent loss after 
the warming after 320 K.
However, the anisotropy cannot applied on N17 and N18 molecules because of the thermal effect resulting in the weak diffractions and severly disorder of the solvents. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1, Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67502
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.436
_diffrn_reflns_theta_max         31.906
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             16505
_reflns_number_gt                13166
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0749P)²+0.7629P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16505
_refine_ls_number_parameters     813
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1410
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.40705(2) 0.21174(2) 0.53139(2) 0.04272(7) Uani 1 1 d . . . . .
Fe2 Fe 0.47752(2) 0.75541(2) -0.07745(2) 0.04584(8) Uani 1 1 d . . . . .
S1 S 0.51178(4) 0.21147(3) 0.39619(3) 0.04872(11) Uani 1 1 d . . . . .
S2 S 0.36037(5) 0.75607(3) 0.06738(4) 0.06101(13) Uani 1 1 d . . . . .
O1 O 0.28007(11) 0.22040(9) 0.49750(9) 0.0536(3) Uani 1 1 d . . . . .
N9 N 0.52935(13) 0.61059(10) 0.01999(10) 0.0469(3) Uani 1 1 d . . . . .
O4 O 0.59123(12) 0.72409(9) -0.16951(9) 0.0575(3) Uani 1 1 d . . . . .
O2 O 0.32627(12) 0.21192(10) 0.64940(9) 0.0585(3) Uani 1 1 d . . . . .
O3 O 0.36837(13) 0.75055(11) -0.12935(11) 0.0634(4) Uani 1 1 d . . . . .
N1 N 0.44659(12) 0.07331(10) 0.59230(9) 0.0428(3) Uani 1 1 d . . . . .
N3 N 0.37966(13) 0.35030(10) 0.46245(10) 0.0454(3) Uani 1 1 d . . . . .
N2 N 0.53837(14) 0.19765(11) 0.57363(11) 0.0495(3) Uani 1 1 d . . . . .
N6 N 0.41458(15) 0.90870(11) -0.13795(10) 0.0541(4) Uani 1 1 d . . . . .
N4 N 0.42916(14) 0.39521(10) 0.36859(10) 0.0494(3) Uani 1 1 d . . . . .
N8 N 0.48689(15) 0.57658(11) 0.11595(11) 0.0553(4) Uani 1 1 d . . . . .
F1 F 0.09548(16) -0.06330(13) 0.57518(16) 0.1125(7) Uani 1 1 d . . . . .
N5 N 0.54061(15) 0.36888(11) 0.24239(10) 0.0544(4) Uani 1 1 d . . . . .
H5A H 0.5335 0.4294 0.2092 0.065 Uiso 1 1 calc R U . . .
H5B H 0.5804 0.3301 0.2179 0.065 Uiso 1 1 calc R U . . .
N10 N 0.36826(18) 0.61030(13) 0.23412(12) 0.0702(5) Uani 1 1 d . . . . .
H10A H 0.3919 0.5529 0.2737 0.084 Uiso 1 1 calc R U . . .
H10B H 0.3177 0.6494 0.2536 0.084 Uiso 1 1 calc R U . . .
C23 C 0.31255(16) 0.40901(13) 0.49627(13) 0.0516(4) Uani 1 1 d . . . . .
H23 H 0.3037 0.4739 0.4565 0.062 Uiso 1 1 calc R U . . .
C41 C 0.65743(15) 0.64567(13) -0.17425(12) 0.0490(4) Uani 1 1 d . . . . .
C24 C 0.48952(15) 0.33482(12) 0.33254(11) 0.0452(3) Uani 1 1 d . . . . .
N7 N 0.58954(16) 0.80944(13) -0.05810(13) 0.0619(4) Uani 1 1 d . . . . .
C16 C 0.59487(15) 0.10488(13) 0.61332(12) 0.0465(4) Uani 1 1 d . . . . .
C7 C 0.38842(15) 0.01832(12) 0.60393(12) 0.0466(4) Uani 1 1 d . . . . .
H7 H 0.4135 -0.0472 0.6370 0.056 Uiso 1 1 calc R U . . .
C47 C 0.60102(16) 0.54481(13) -0.00295(13) 0.0525(4) Uani 1 1 d . . . . .
H47 H 0.6131 0.4835 0.0455 0.063 Uiso 1 1 calc R U . . .
C8 C 0.54819(14) 0.03463(12) 0.62375(11) 0.0437(3) Uani 1 1 d . . . . .
C22 C 0.25007(16) 0.38208(15) 0.59096(14) 0.0545(4) Uani 1 1 d . . . . .
C9 C 0.60214(16) -0.05977(13) 0.66176(12) 0.0505(4) Uani 1 1 d . . . . .
H9 H 0.5731 -0.1066 0.6680 0.061 Uiso 1 1 calc R U . . .
C46 C 0.66360(16) 0.55619(13) -0.09462(13) 0.0522(4) Uani 1 1 d . . . . .
C10 C 0.70184(18) -0.08528(15) 0.69126(14) 0.0600(5) Uani 1 1 d . . . . .
H10 H 0.7380 -0.1493 0.7170 0.072 Uiso 1 1 calc R U . . .
C32 C 0.4746(2) 0.96175(14) -0.13282(13) 0.0630(6) Uani 1 1 d . . . . .
C1 C 0.24164(15) 0.14836(13) 0.51783(12) 0.0499(4) Uani 1 1 d . . . . .
C12 C 0.69380(17) 0.07919(15) 0.64369(14) 0.0560(4) Uani 1 1 d . . . . .
C42 C 0.72259(18) 0.64918(17) -0.26046(14) 0.0616(5) Uani 1 1 d . . . . .
H42 H 0.7199 0.7075 -0.3135 0.074 Uiso 1 1 calc R U . . .
C25 C 0.27322(19) 0.80896(19) -0.14787(16) 0.0668(6) Uani 1 1 d . . . . .
C17 C 0.25993(17) 0.28651(16) 0.66110(13) 0.0563(4) Uani 1 1 d . . . . .
C2 C 0.14440(19) 0.17030(17) 0.48554(16) 0.0641(5) Uani 1 1 d . . . . .
H2 H 0.1127 0.2338 0.4502 0.077 Uiso 1 1 calc R U . . .
C6 C 0.28929(16) 0.05052(13) 0.57003(13) 0.0498(4) Uani 1 1 d . . . . .
C40 C 0.5674(2) 0.90552(17) -0.08851(14) 0.0642(5) Uani 1 1 d . . . . .
C48 C 0.41040(16) 0.63891(13) 0.14152(13) 0.0510(4) Uani 1 1 d . . . . .
C5 C 0.23794(19) -0.02016(15) 0.58821(17) 0.0637(5) Uani 1 1 d . . . . .
H5 H 0.2686 -0.0843 0.6220 0.076 Uiso 1 1 calc R U . . .
C15 C 0.5754(2) 0.26575(16) 0.56734(17) 0.0646(5) Uani 1 1 d . . . . .
H15 H 0.5367 0.3289 0.5412 0.078 Uiso 1 1 calc R U . . .
F2 F -0.02617(18) 0.9850(3) -0.2173(2) 0.1801(14) Uani 1 1 d . . . . .
C31 C 0.3208(2) 0.95036(16) -0.16381(15) 0.0699(6) Uani 1 1 d . . . . .
H31 H 0.2980 1.0159 -0.1821 0.084 Uiso 1 1 calc R U . . .
C30 C 0.2486(2) 0.90587(19) -0.16708(16) 0.0711(6) Uani 1 1 d . . . . .
C11 C 0.74628(19) -0.01820(17) 0.68288(15) 0.0634(5) Uani 1 1 d . . . . .
H11 H 0.8118 -0.0369 0.7032 0.076 Uiso 1 1 calc R U . . .
C45 C 0.7340(2) 0.47449(16) -0.10494(17) 0.0697(6) Uani 1 1 d . . . . .
H45 H 0.7381 0.4155 -0.0528 0.084 Uiso 1 1 calc R U . . .
C21 C 0.17649(19) 0.45664(18) 0.61245(18) 0.0689(6) Uani 1 1 d . . . . .
H21 H 0.1718 0.5193 0.5665 0.083 Uiso 1 1 calc R U . . .
C43 C 0.7902(2) 0.5680(2) -0.26804(17) 0.0737(6) Uani 1 1 d . . . . .
H43 H 0.8324 0.5720 -0.3261 0.088 Uiso 1 1 calc R U . . .
C18 C 0.1926(2) 0.2715(2) 0.75021(16) 0.0759(7) Uani 1 1 d . . . . .
H18 H 0.1974 0.2097 0.7979 0.091 Uiso 1 1 calc R U . . .
C36 C 0.6347(3) 0.9492(2) -0.07829(19) 0.0878(9) Uani 1 1 d . . . . .
C3 C 0.0959(2) 0.10019(19) 0.50513(19) 0.0739(6) Uani 1 1 d . . . . .
H3 H 0.0314 0.1159 0.4843 0.089 Uiso 1 1 calc R U . . .
C13 C 0.7310(2) 0.15376(19) 0.63513(19) 0.0731(6) Uani 1 1 d . . . . .
H13 H 0.7960 0.1404 0.6541 0.088 Uiso 1 1 calc R U . . .
C20 C 0.1111(2) 0.4394(2) 0.7000(2) 0.0824(7) Uani 1 1 d . . . . .
H20 H 0.0620 0.4895 0.7127 0.099 Uiso 1 1 calc R U . . .
C33 C 0.4530(3) 1.05889(17) -0.16628(17) 0.0876(9) Uani 1 1 d . . . . .
H33 H 0.3943 1.0976 -0.1972 0.105 Uiso 1 1 calc R U . . .
C29 C 0.1458(3) 0.9649(3) -0.1913(2) 0.1020(11) Uani 1 1 d . . . . .
H29 H 0.1294 1.0295 -0.2058 0.122 Uiso 1 1 calc R U . . .
C4 C 0.1448(2) 0.00520(18) 0.5567(2) 0.0743(7) Uani 1 1 d . . . . .
C44 C 0.7966(2) 0.4800(2) -0.19015(19) 0.0811(7) Uani 1 1 d . . . . .
H44 H 0.8429 0.4253 -0.1958 0.097 Uiso 1 1 calc R U . . .
C14 C 0.6713(2) 0.24513(19) 0.5990(2) 0.0773(7) Uani 1 1 d . . . . .
H14 H 0.6941 0.2941 0.5954 0.093 Uiso 1 1 calc R U . . .
C19 C 0.1200(2) 0.3463(2) 0.76811(19) 0.0897(9) Uani 1 1 d . . . . .
H19 H 0.0761 0.3339 0.8273 0.108 Uiso 1 1 calc R U . . .
C26 C 0.1926(2) 0.7729(3) -0.1499(2) 0.0925(9) Uani 1 1 d . . . . .
H26 H 0.2062 0.7087 -0.1359 0.111 Uiso 1 1 calc R U . . .
C35 C 0.6064(4) 1.0483(3) -0.1107(2) 0.1102(14) Uani 1 1 d . . . . .
H35 H 0.6476 1.0781 -0.1024 0.132 Uiso 1 1 calc R U . . .
C39 C 0.6763(2) 0.7554(2) -0.0185(2) 0.0885(8) Uani 1 1 d . . . . .
H39 H 0.6915 0.6898 0.0017 0.106 Uiso 1 1 calc R U . . .
C37 C 0.7250(3) 0.8883(4) -0.0344(3) 0.1132(13) Uani 1 1 d . . . . .
H37 H 0.7703 0.9138 -0.0252 0.136 Uiso 1 1 calc R U . . .
C34 C 0.5207(4) 1.1004(2) -0.1536(2) 0.1151(15) Uani 1 1 d . . . . .
H34 H 0.5045 1.1664 -0.1760 0.138 Uiso 1 1 calc R U . . .
C28 C 0.0729(3) 0.9278(4) -0.1933(3) 0.1212(15) Uani 1 1 d . . . . .
C51 C -0.0743(3) 0.3221(3) 0.6218(3) 0.1028(11) Uani 1 1 d . . . . .
C27 C 0.0922(3) 0.8342(4) -0.1729(3) 0.1211(14) Uani 1 1 d . . . . .
H27 H 0.0387 0.8108 -0.1743 0.145 Uiso 1 1 calc R U . . .
N13 N -0.0795(4) 0.3168(3) 0.3921(4) 0.186(2) Uani 1 1 d . . . . .
C38 C 0.7465(3) 0.7930(4) -0.0056(3) 0.1183(13) Uani 1 1 d . . . . .
H38 H 0.8070 0.7529 0.0225 0.142 Uiso 1 1 calc R U . . .
C55 C -0.1449(3) 0.3050(3) 0.3712(3) 0.1123(12) Uani 1 1 d . . . . .
N12 N -0.1530(3) 0.3097(4) 0.6593(4) 0.1713(19) Uani 1 1 d . . . . .
C52 C 0.0249(3) 0.3510(5) 0.5621(5) 0.180(3) Uani 1 1 d . . . . .
H52A H 0.0237 0.3678 0.4979 0.270 Uiso 1 1 calc R U . . .
H52B H 0.0866 0.2993 0.5823 0.270 Uiso 1 1 calc R U . . .
H52C H 0.0302 0.4052 0.5662 0.270 Uiso 1 1 calc R U . . .
C56 C -0.2290(4) 0.2920(4) 0.3489(4) 0.1474(18) Uani 1 1 d . . . . .
H56A H -0.2778 0.2630 0.4057 0.221 Uiso 1 1 calc R U . . .
H56B H -0.1991 0.2514 0.3169 0.221 Uiso 1 1 calc R U . . .
H56C H -0.2682 0.3528 0.3086 0.221 Uiso 1 1 calc R U . . .
C49' C 0.0835(8) 0.8302(7) 0.0808(9) 0.156(4) Uani 0.670(3) 1 d D . P A 3
H49A H 0.1115 0.7855 0.0534 0.234 Uiso 0.670(3) 1 calc R U P A 3
H49B H 0.0805 0.7963 0.1477 0.234 Uiso 0.670(3) 1 calc R U P A 3
H49C H 0.1304 0.8735 0.0543 0.234 Uiso 0.670(3) 1 calc R U P A 3
N11' N -0.1074(5) 0.9260(5) 0.0443(4) 0.1240(18) Uani 0.670(3) 1 d D . P A 3
N11 N 0.1408(8) 0.9927(8) 0.0054(8) 0.104(3) Uani 0.330(3) 1 d D . P B 2
C50' C -0.0242(5) 0.8832(5) 0.0610(4) 0.1090(18) Uani 0.670(3) 1 d D . P A 3
C50 C 0.1111(7) 0.9254(9) 0.0447(9) 0.101(3) Uani 0.330(3) 1 d D . P B 2
C49 C 0.060(2) 0.8464(13) 0.096(3) 0.29(3) Uani 0.330(3) 1 d D . P B 2
H49D H 0.0313 0.8385 0.1597 0.439 Uiso 0.330(3) 1 calc R U P B 2
H49E H 0.1119 0.7892 0.0958 0.439 Uiso 0.330(3) 1 calc R U P B 2
H49F H 0.0009 0.8586 0.0663 0.439 Uiso 0.330(3) 1 calc R U P B 2
C60 C 0.383(2) 0.4245(19) 0.7301(17) 0.152(7) Uani 0.531(3) 1 d . . P C 4
H60A H 0.3847 0.4636 0.7571 0.228 Uiso 0.531(3) 1 calc R U P C 4
H60B H 0.4230 0.3605 0.7621 0.228 Uiso 0.531(3) 1 calc R U P C 4
H60C H 0.3083 0.4241 0.7370 0.228 Uiso 0.531(3) 1 calc R U P C 4
N15 N 0.4678(7) 0.4945(5) 0.5521(6) 0.131(3) Uani 0.531(3) 1 d . . P C 4
C61 C 0.4313(8) 0.4634(6) 0.6295(8) 0.115(3) Uani 0.531(3) 1 d . . P C 4
N16 N 0.7766(11) 0.5149(9) 0.1353(8) 0.168(4) Uani 0.508(3) 1 d . . P D 5
C63 C 0.7149(9) 0.5352(8) 0.1903(8) 0.129(3) Uani 0.508(3) 1 d . . P D 5
C62 C 0.634(2) 0.564(3) 0.261(2) 0.193(12) Uani 0.508(3) 1 d . . P D 5
H62A H 0.6402 0.6237 0.2525 0.290 Uiso 0.508(3) 1 calc R U P D 5
H62B H 0.6466 0.5159 0.3232 0.290 Uiso 0.508(3) 1 calc R U P D 5
H62C H 0.5622 0.5699 0.2546 0.290 Uiso 0.508(3) 1 calc R U P D 5
C64 C -0.0609(8) 0.5735(7) 0.8827(7) 0.138(3) Uiso 0.565(3) 1 d D . P E 6
H64A H -0.0725 0.6233 0.8213 0.207 Uiso 0.565(3) 1 calc R U P E 6
H64B H -0.1011 0.5966 0.9295 0.207 Uiso 0.565(3) 1 calc R U P E 6
H64C H -0.0855 0.5199 0.8945 0.207 Uiso 0.565(3) 1 calc R U P E 6
C67 C 1.030(2) 0.362(2) 0.0725(18) 0.271(11) Uiso 0.396(3) 1 d D . P F 7
C66 C 1.0617(15) 0.3603(14) 0.1482(13) 0.183(7) Uiso 0.396(3) 1 d D . P F 7
H66A H 1.0489 0.3039 0.2045 0.275 Uiso 0.396(3) 1 calc R U P F 7
H66B H 1.0200 0.4158 0.1585 0.275 Uiso 0.396(3) 1 calc R U P F 7
H66C H 1.1378 0.3597 0.1324 0.275 Uiso 0.396(3) 1 calc R U P F 7
C65 C 0.0529(11) 0.5446(18) 0.8867(19) 0.312(10) Uiso 0.565(3) 1 d D . P E 6
N18 N 1.006(2) 0.3643(19) 0.0108(17) 0.327(12) Uiso 0.396(3) 1 d D . P F 7
N17 N 0.1451(11) 0.522(2) 0.884(2) 0.409(16) Uiso 0.565(3) 1 d D . P E 6


_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 O1 1.8817(14) . ?
Fe1 O2 1.9094(15) . ?
Fe1 N1 1.9391(15) . ?
Fe1 N3 1.9479(16) . ?
Fe1 N2 1.9809(17) . ?
Fe1 S1 2.2319(9) . ?
Fe2 O4 1.9106(16) . ?
Fe2 O3 1.9474(15) . ?
Fe2 N9 2.1365(17) . ?
Fe2 N7 2.1525(18) . ?
Fe2 N6 2.1645(18) . ?
Fe2 S2 2.4133(10) . ?
S1 C24 1.7380(18) . ?
S2 C48 1.727(2) . ?
O1 C1 1.310(2) . ?
N9 C47 1.301(2) . ?
N9 N8 1.390(2) . ?
O4 C41 1.313(2) . ?
O2 C17 1.307(3) . ?
O3 C25 1.316(3) . ?
N1 C7 1.299(2) . ?
N1 C8 1.422(2) . ?
N3 C23 1.292(2) . ?
N3 N4 1.399(2) . ?
N2 C15 1.327(2) . ?
N2 C16 1.367(2) . ?
N6 C31 1.290(3) . ?
N6 C32 1.421(3) . ?
N4 C24 1.313(2) . ?
N8 C48 1.305(3) . ?
F1 C4 1.362(3) . ?
N5 C24 1.343(2) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N10 C48 1.347(2) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
C23 C22 1.446(3) . ?
C23 H23 0.9300 . ?
C41 C42 1.401(3) . ?
C41 C46 1.413(3) . ?
N7 C39 1.321(3) . ?
N7 C40 1.359(3) . ?
C16 C12 1.409(3) . ?
C16 C8 1.415(2) . ?
C7 C6 1.422(3) . ?
C7 H7 0.9300 . ?
C47 C46 1.435(3) . ?
C47 H47 0.9300 . ?
C8 C9 1.374(2) . ?
C22 C21 1.406(3) . ?
C22 C17 1.417(3) . ?
C9 C10 1.412(3) . ?
C9 H9 0.9300 . ?
C46 C45 1.406(3) . ?
C10 C11 1.361(3) . ?
C10 H10 0.9300 . ?
C32 C33 1.369(3) . ?
C32 C40 1.424(4) . ?
C1 C2 1.418(3) . ?
C1 C6 1.422(3) . ?
C12 C11 1.406(3) . ?
C12 C13 1.413(3) . ?
C42 C43 1.372(3) . ?
C42 H42 0.9300 . ?
C25 C30 1.406(4) . ?
C25 C26 1.412(4) . ?
C17 C18 1.413(3) . ?
C2 C3 1.373(3) . ?
C2 H2 0.9300 . ?
C6 C5 1.416(3) . ?
C40 C36 1.420(3) . ?
C5 C4 1.348(3) . ?
C5 H5 0.9300 . ?
C15 C14 1.401(3) . ?
C15 H15 0.9300 . ?
F2 C28 1.371(4) . ?
C31 C30 1.425(4) . ?
C31 H31 0.9300 . ?
C30 C29 1.420(3) . ?
C11 H11 0.9300 . ?
C45 C44 1.369(3) . ?
C45 H45 0.9300 . ?
C21 C20 1.380(4) . ?
C21 H21 0.9300 . ?
C43 C44 1.387(4) . ?
C43 H43 0.9300 . ?
C18 C19 1.378(4) . ?
C18 H18 0.9300 . ?
C36 C35 1.397(5) . ?
C36 C37 1.404(5) . ?
C3 C4 1.393(4) . ?
C3 H3 0.9300 . ?
C13 C14 1.359(4) . ?
C13 H13 0.9300 . ?
C20 C19 1.380(4) . ?
C20 H20 0.9300 . ?
C33 C34 1.420(5) . ?
C33 H33 0.9300 . ?
C29 C28 1.332(6) . ?
C29 H29 0.9300 . ?
C44 H44 0.9300 . ?
C14 H14 0.9300 . ?
C19 H19 0.9300 . ?
C26 C27 1.398(5) . ?
C26 H26 0.9300 . ?
C35 C34 1.331(6) . ?
C35 H35 0.9300 . ?
C39 C38 1.401(4) . ?
C39 H39 0.9300 . ?
C37 C38 1.351(6) . ?
C37 H37 0.9300 . ?
C34 H34 0.9300 . ?
C28 C27 1.357(6) . ?
C51 N12 1.065(5) . ?
C51 C52 1.448(6) . ?
C27 H27 0.9300 . ?
N13 C55 1.136(5) . ?
C38 H38 0.9300 . ?
C55 C56 1.394(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C49' C50' 1.437(11) . ?
C49' H49A 0.9600 . ?
C49' H49B 0.9600 . ?
C49' H49C 0.9600 . ?
N11' C50' 1.122(7) . ?
N11 C50 1.117(9) . ?
C50 C49 1.437(14) . ?
C49 H49D 0.9600 . ?
C49 H49E 0.9600 . ?
C49 H49F 0.9600 . ?
C60 C61 1.47(3) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N15 C61 1.128(11) . ?
N15 N15 1.614(17) 2_666 ?
N16 C63 1.120(14) . ?
C63 C62 1.47(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 C65 1.433(8) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C67 N18 1.141(10) . ?
C67 C66 1.428(10) . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C65 N17 1.144(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
O1 Fe1 O2 90.87(7) . . ?
O1 Fe1 N1 95.31(7) . . ?
O2 Fe1 N1 89.42(7) . . ?
O1 Fe1 N3 87.21(7) . . ?
O2 Fe1 N3 94.99(7) . . ?
N1 Fe1 N3 174.89(6) . . ?
O1 Fe1 N2 177.04(6) . . ?
O2 Fe1 N2 86.99(7) . . ?
N1 Fe1 N2 82.64(7) . . ?
N3 Fe1 N2 95.00(7) . . ?
O1 Fe1 S1 93.15(5) . . ?
O2 Fe1 S1 175.97(5) . . ?
N1 Fe1 S1 90.44(6) . . ?
N3 Fe1 S1 84.98(6) . . ?
N2 Fe1 S1 89.00(5) . . ?
O4 Fe2 O3 90.84(7) . . ?
O4 Fe2 N9 86.28(7) . . ?
O3 Fe2 N9 103.65(7) . . ?
O4 Fe2 N7 87.43(7) . . ?
O3 Fe2 N7 160.35(7) . . ?
N9 Fe2 N7 95.77(7) . . ?
O4 Fe2 N6 108.17(7) . . ?
O3 Fe2 N6 86.35(7) . . ?
N9 Fe2 N6 162.51(6) . . ?
N7 Fe2 N6 75.64(8) . . ?
O4 Fe2 S2 164.76(4) . . ?
O3 Fe2 S2 96.60(6) . . ?
N9 Fe2 S2 79.06(6) . . ?
N7 Fe2 S2 89.91(6) . . ?
N6 Fe2 S2 85.64(6) . . ?
C24 S1 Fe1 96.31(7) . . ?
C48 S2 Fe2 97.70(8) . . ?
C1 O1 Fe1 125.85(12) . . ?
C47 N9 N8 112.80(15) . . ?
C47 N9 Fe2 124.71(12) . . ?
N8 N9 Fe2 122.49(12) . . ?
C41 O4 Fe2 136.23(12) . . ?
C17 O2 Fe1 125.33(13) . . ?
C25 O3 Fe2 130.34(15) . . ?
C7 N1 C8 121.25(15) . . ?
C7 N1 Fe1 124.79(12) . . ?
C8 N1 Fe1 113.95(11) . . ?
C23 N3 N4 113.72(15) . . ?
C23 N3 Fe1 124.37(13) . . ?
N4 N3 Fe1 121.86(12) . . ?
C15 N2 C16 118.82(17) . . ?
C15 N2 Fe1 128.10(15) . . ?
C16 N2 Fe1 113.08(12) . . ?
C31 N6 C32 119.98(19) . . ?
C31 N6 Fe2 123.78(17) . . ?
C32 N6 Fe2 115.37(14) . . ?
C24 N4 N3 113.05(14) . . ?
C48 N8 N9 114.94(15) . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
N3 C23 C22 125.34(18) . . ?
N3 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
O4 C41 C42 119.86(17) . . ?
O4 C41 C46 121.81(17) . . ?
C42 C41 C46 118.32(19) . . ?
N4 C24 N5 119.02(15) . . ?
N4 C24 S1 123.72(13) . . ?
N5 C24 S1 117.22(14) . . ?
C39 N7 C40 118.9(2) . . ?
C39 N7 Fe2 124.31(19) . . ?
C40 N7 Fe2 116.74(16) . . ?
N2 C16 C12 122.44(17) . . ?
N2 C16 C8 116.51(16) . . ?
C12 C16 C8 121.04(17) . . ?
N1 C7 C6 125.06(16) . . ?
N1 C7 H7 117.5 . . ?
C6 C7 H7 117.5 . . ?
N9 C47 C46 127.31(16) . . ?
N9 C47 H47 116.3 . . ?
C46 C47 H47 116.3 . . ?
C9 C8 C16 119.17(16) . . ?
C9 C8 N1 127.56(16) . . ?
C16 C8 N1 113.27(15) . . ?
C21 C22 C17 119.7(2) . . ?
C21 C22 C23 116.6(2) . . ?
C17 C22 C23 123.71(19) . . ?
C8 C9 C10 119.68(18) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C45 C46 C41 119.03(19) . . ?
C45 C46 C47 118.17(18) . . ?
C41 C46 C47 122.80(18) . . ?
C11 C10 C9 121.44(19) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C33 C32 N6 127.1(3) . . ?
C33 C32 C40 118.2(3) . . ?
N6 C32 C40 114.75(17) . . ?
O1 C1 C2 117.02(17) . . ?
O1 C1 C6 125.18(16) . . ?
C2 C1 C6 117.80(18) . . ?
C11 C12 C16 118.15(19) . . ?
C11 C12 C13 124.8(2) . . ?
C16 C12 C13 117.0(2) . . ?
C43 C42 C41 121.1(2) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
O3 C25 C30 123.1(2) . . ?
O3 C25 C26 118.5(3) . . ?
C30 C25 C26 118.4(2) . . ?
O2 C17 C18 118.0(2) . . ?
O2 C17 C22 124.95(18) . . ?
C18 C17 C22 117.0(2) . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C5 C6 C7 117.10(17) . . ?
C5 C6 C1 119.22(18) . . ?
C7 C6 C1 123.67(16) . . ?
N7 C40 C36 121.8(3) . . ?
N7 C40 C32 117.5(2) . . ?
C36 C40 C32 120.8(2) . . ?
N8 C48 N10 117.36(17) . . ?
N8 C48 S2 125.75(14) . . ?
N10 C48 S2 116.87(15) . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
N2 C15 C14 121.8(2) . . ?
N2 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
N6 C31 C30 126.4(2) . . ?
N6 C31 H31 116.8 . . ?
C30 C31 H31 116.8 . . ?
C25 C30 C29 119.3(3) . . ?
C25 C30 C31 124.2(2) . . ?
C29 C30 C31 116.5(3) . . ?
C10 C11 C12 120.50(19) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C44 C45 C46 121.4(2) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 H45 119.3 . . ?
C20 C21 C22 121.8(2) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C42 C43 C44 120.8(2) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C19 C18 C17 121.6(2) . . ?
C19 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C35 C36 C37 124.6(3) . . ?
C35 C36 C40 118.5(4) . . ?
C37 C36 C40 116.9(3) . . ?
C2 C3 C4 118.9(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C19 C20 C21 118.6(2) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
C32 C33 C34 119.8(3) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C28 C29 C30 120.0(4) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C5 C4 F1 119.8(2) . . ?
C5 C4 C3 122.2(2) . . ?
F1 C4 C3 118.0(2) . . ?
C45 C44 C43 119.3(2) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
C13 C14 C15 120.2(2) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C18 C19 C20 121.3(2) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C27 C26 C25 119.7(4) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
N7 C39 C38 122.7(3) . . ?
N7 C39 H39 118.6 . . ?
C38 C39 H39 118.6 . . ?
C38 C37 C36 120.6(3) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C35 C34 C33 122.5(3) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C29 C28 C27 122.7(3) . . ?
C29 C28 F2 120.0(5) . . ?
C27 C28 F2 117.4(4) . . ?
N12 C51 C52 172.3(6) . . ?
C28 C27 C26 119.8(4) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C37 C38 C39 119.1(4) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
N13 C55 C56 177.1(6) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C50' C49' H49A 109.5 . . ?
C50' C49' H49B 109.5 . . ?
H49A C49' H49B 109.5 . . ?
C50' C49' H49C 109.5 . . ?
H49A C49' H49C 109.5 . . ?
H49B C49' H49C 109.5 . . ?
N11' C50' C49' 178.6(9) . . ?
N11 C50 C49 172.9(15) . . ?
C50 C49 H49D 109.5 . . ?
C50 C49 H49E 109.5 . . ?
H49D C49 H49E 109.5 . . ?
C50 C49 H49F 109.5 . . ?
H49D C49 H49F 109.5 . . ?
H49E C49 H49F 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 N15 N15 162.7(10) . 2_666 ?
N15 C61 C60 179.0(17) . . ?
N16 C63 C62 179(2) . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N18 C67 C66 178(4) . . ?
C67 C66 H66A 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C67 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N17 C65 C64 176(4) . . ?

_refine_diff_density_max         0.423
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.051

_shelxl_version_number           2013-2

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ws101
_database_code_depnum_ccdc_archive 'CCDC 1529169'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Fe(qsal-Br)(thsa)]MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H20 Br Fe N6 O2 S'
_chemical_formula_weight         616.30

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                   12.438(3)
_cell_length_b                   13.804(3)
_cell_length_c                   16.809(3)
_cell_angle_alpha                102.88(3)
_cell_angle_beta                 98.96(3)
_cell_angle_gamma                109.28(3)
_cell_volume                     2571.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12187
_cell_measurement_theta_min      0.985
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Bar
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    2.258
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9562
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_process_details   'XScale within XDS'

_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 Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43526
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         27.48
_reflns_number_total             11597
_reflns_number_gt                8586
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BluIce (McPhillips, 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. 
;

_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)+(0.0787P)²+20.5935P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11597
_refine_ls_number_parameters     669
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0831
_refine_ls_wR_factor_ref         0.2243
_refine_ls_wR_factor_gt          0.2018
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.143
_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 0.91278(6) 0.41333(6) 0.13510(5) 0.03010(18) Uani 1 1 d . . .
Fe1 Fe 0.64016(8) 0.75819(7) -0.01712(5) 0.0181(2) Uani 1 1 d . . .
Fe2 Fe 0.55877(8) 0.69966(8) 0.38603(6) 0.0221(2) Uani 1 1 d . . .
Br2 Br 1.11343(7) 0.73952(9) 0.26798(6) 0.0532(3) Uani 1 1 d . . .
S1 S 0.53736(15) 0.62072(13) -0.13162(10) 0.0243(3) Uani 1 1 d . . .
S2 S 0.73638(15) 0.82356(14) 0.49275(10) 0.0263(3) Uani 1 1 d . . .
O2 O 0.7153(4) 0.8801(4) 0.0794(3) 0.0235(9) Uani 1 1 d . . .
N3 N 0.6940(5) 0.8357(4) -0.0968(3) 0.0199(10) Uani 1 1 d . . .
O1 O 0.7778(4) 0.7291(4) -0.0107(3) 0.0239(9) Uani 1 1 d . . .
O3 O 0.6340(5) 0.6049(4) 0.3382(3) 0.0305(11) Uani 1 1 d . . .
N1 N 0.5791(4) 0.6738(4) 0.0548(3) 0.0181(10) Uani 1 1 d . . .
O4 O 0.4082(5) 0.5919(4) 0.3233(3) 0.0304(11) Uani 1 1 d . . .
N2 N 0.4982(5) 0.7931(4) -0.0166(3) 0.0233(11) Uani 1 1 d . . .
N4 N 0.6503(5) 0.7919(5) -0.1836(3) 0.0246(11) Uani 1 1 d . . .
C1 C 0.8029(5) 0.6609(5) 0.0242(4) 0.0195(12) Uani 1 1 d . . .
C7 C 0.6237(6) 0.6095(5) 0.0812(4) 0.0203(12) Uani 1 1 d . . .
H7 H 0.5827 0.5674 0.1126 0.024 Uiso 1 1 calc R . .
C5 C 0.7620(6) 0.5236(5) 0.0989(4) 0.0232(13) Uani 1 1 d . . .
H5 H 0.7113 0.4799 0.1248 0.028 Uiso 1 1 calc R . .
C23 C 0.7802(6) 0.9298(5) -0.0728(4) 0.0200(12) Uani 1 1 d . . .
H23 H 0.8034 0.9597 -0.1161 0.024 Uiso 1 1 calc R . .
C17 C 0.8111(6) 0.9648(5) 0.0845(4) 0.0221(12) Uani 1 1 d . . .
N8 N 0.5904(6) 0.7131(5) 0.5756(3) 0.0289(13) Uani 1 1 d . . .
N5 N 0.5265(6) 0.6349(5) -0.2859(4) 0.0328(14) Uani 1 1 d . . .
H5A H 0.5416 0.6671 -0.3249 0.039 Uiso 1 1 calc R . .
H5B H 0.4782 0.5673 -0.3004 0.039 Uiso 1 1 calc R . .
N10 N 0.7635(6) 0.8490(5) 0.6565(4) 0.0305(13) Uani 1 1 d . . .
H10A H 0.7432 0.8360 0.7020 0.037 Uiso 1 1 calc R . .
H10B H 0.8308 0.9005 0.6610 0.037 Uiso 1 1 calc R . .
C24 C 0.5769(6) 0.6888(5) -0.2046(4) 0.0238(13) Uani 1 1 d . . .
C48 C 0.6905(6) 0.7894(6) 0.5787(4) 0.0256(13) Uani 1 1 d . . .
N9 N 0.5184(5) 0.6589(5) 0.4952(3) 0.0234(11) Uani 1 1 d . . .
C16 C 0.4339(5) 0.7482(5) 0.0353(4) 0.0186(11) Uani 1 1 d . . .
C18 C 0.8797(6) 1.0297(5) 0.1644(4) 0.0264(14) Uani 1 1 d . . .
H18 H 0.8584 1.0118 0.2126 0.032 Uiso 1 1 calc R . .
C4 C 0.8677(6) 0.5142(5) 0.0933(4) 0.0244(13) Uani 1 1 d . . .
N6 N 0.6206(5) 0.7900(5) 0.3033(3) 0.0240(11) Uani 1 1 d . . .
C21 C 0.9417(6) 1.0849(5) 0.0250(4) 0.0229(13) Uani 1 1 d . . .
H21 H 0.9630 1.1045 -0.0227 0.028 Uiso 1 1 calc R . .
C22 C 0.8430(5) 0.9920(5) 0.0119(4) 0.0196(12) Uani 1 1 d . . .
C3 C 0.9437(6) 0.5787(6) 0.0558(4) 0.0261(14) Uani 1 1 d . . .
H3 H 1.0174 0.5732 0.0536 0.031 Uiso 1 1 calc R . .
N7 N 0.4785(5) 0.8181(5) 0.3998(3) 0.0242(11) Uani 1 1 d . . .
C8 C 0.4753(6) 0.6824(5) 0.0749(4) 0.0198(12) Uani 1 1 d . . .
C9 C 0.4156(6) 0.6370(6) 0.1286(4) 0.0250(13) Uani 1 1 d . . .
H9 H 0.4418 0.5925 0.1558 0.030 Uiso 1 1 calc R . .
C12 C 0.3338(6) 0.7692(5) 0.0486(4) 0.0241(13) Uani 1 1 d . . .
C19 C 0.9785(6) 1.1200(6) 0.1748(4) 0.0296(15) Uani 1 1 d . . .
H19 H 1.0253 1.1620 0.2299 0.036 Uiso 1 1 calc R . .
C6 C 0.7290(6) 0.5983(5) 0.0663(4) 0.0206(12) Uani 1 1 d . . .
C31 C 0.7158(6) 0.7930(6) 0.2781(4) 0.0292(15) Uani 1 1 d . . .
H31 H 0.7452 0.8441 0.2493 0.035 Uiso 1 1 calc R . .
C20 C 1.0101(6) 1.1498(5) 0.1046(4) 0.0243(13) Uani 1 1 d . . .
H20 H 1.0766 1.2127 0.1115 0.029 Uiso 1 1 calc R . .
C30 C 0.7787(7) 0.7258(6) 0.2904(4) 0.0317(16) Uani 1 1 d . . .
C2 C 0.9112(6) 0.6497(5) 0.0221(4) 0.0251(13) Uani 1 1 d . . .
H2 H 0.9633 0.6926 -0.0035 0.030 Uiso 1 1 calc R . .
C40 C 0.4936(6) 0.8786(5) 0.3459(4) 0.0227(13) Uani 1 1 d . . .
C15 C 0.4651(7) 0.8558(6) -0.0537(5) 0.0288(14) Uani 1 1 d . . .
H15 H 0.5100 0.8867 -0.0889 0.035 Uiso 1 1 calc R . .
C38 C 0.3568(7) 0.9063(6) 0.4544(5) 0.0345(16) Uani 1 1 d . . .
H38 H 0.3118 0.9154 0.4943 0.041 Uiso 1 1 calc R . .
C33 C 0.5815(7) 0.9189(6) 0.2325(4) 0.0311(15) Uani 1 1 d . . .
H33 H 0.6289 0.9081 0.1949 0.037 Uiso 1 1 calc R . .
C41 C 0.3214(6) 0.5243(6) 0.3413(4) 0.0275(14) Uani 1 1 d . . .
C32 C 0.5686(6) 0.8633(6) 0.2908(4) 0.0264(14) Uani 1 1 d . . .
C13 C 0.3013(7) 0.8363(6) 0.0076(5) 0.0314(15) Uani 1 1 d . . .
H13 H 0.2342 0.8522 0.0154 0.038 Uiso 1 1 calc R . .
C11 C 0.2741(6) 0.7218(6) 0.1050(5) 0.0276(14) Uani 1 1 d . . .
H11 H 0.2068 0.7348 0.1164 0.033 Uiso 1 1 calc R . .
C28 C 0.9587(7) 0.6956(7) 0.2866(5) 0.0370(18) Uani 1 1 d . . .
C36 C 0.4393(7) 0.9523(6) 0.3418(4) 0.0300(15) Uani 1 1 d . . .
C46 C 0.3260(6) 0.5147(6) 0.4239(4) 0.0283(14) Uani 1 1 d . . .
C10 C 0.3149(6) 0.6575(6) 0.1426(4) 0.0273(14) Uani 1 1 d . . .
H10 H 0.2739 0.6257 0.1792 0.033 Uiso 1 1 calc R . .
C25 C 0.7382(6) 0.6352(6) 0.3212(4) 0.0285(14) Uani 1 1 d . . .
C29 C 0.8920(7) 0.7545(7) 0.2717(4) 0.0352(17) Uani 1 1 d . . .
H29 H 0.9201 0.8130 0.2495 0.042 Uiso 1 1 calc R . .
C47 C 0.4243(7) 0.5819(6) 0.4950(4) 0.0297(15) Uani 1 1 d . . .
H47 H 0.4194 0.5681 0.5475 0.036 Uiso 1 1 calc R . .
C42 C 0.2175(7) 0.4581(6) 0.2780(5) 0.0326(16) Uani 1 1 d . . .
H42 H 0.2117 0.4631 0.2222 0.039 Uiso 1 1 calc R . .
C14 C 0.3655(7) 0.8792(6) -0.0435(5) 0.0309(15) Uani 1 1 d . . .
H14 H 0.3431 0.9244 -0.0719 0.037 Uiso 1 1 calc R . .
C39 C 0.4121(6) 0.8314(6) 0.4525(4) 0.0279(14) Uani 1 1 d . . .
H39 H 0.4012 0.7891 0.4903 0.034 Uiso 1 1 calc R . .
C45 C 0.2303(7) 0.4384(7) 0.4394(5) 0.0382(18) Uani 1 1 d . . .
H45 H 0.2356 0.4307 0.4945 0.046 Uiso 1 1 calc R . .
C27 C 0.9220(7) 0.6083(7) 0.3170(5) 0.0382(18) Uani 1 1 d . . .
H27 H 0.9714 0.5703 0.3269 0.046 Uiso 1 1 calc R . .
C37 C 0.3683(6) 0.9644(6) 0.3996(5) 0.0325(16) Uani 1 1 d . . .
H37 H 0.3294 1.0132 0.3992 0.039 Uiso 1 1 calc R . .
C26 C 0.8112(7) 0.5774(7) 0.3327(5) 0.0364(17) Uani 1 1 d . . .
H26 H 0.7839 0.5159 0.3517 0.044 Uiso 1 1 calc R . .
C43 C 0.1245(7) 0.3864(7) 0.2961(6) 0.0397(18) Uani 1 1 d . . .
H43 H 0.0552 0.3440 0.2524 0.048 Uiso 1 1 calc R . .
C34 C 0.5260(8) 0.9912(7) 0.2276(5) 0.0387(18) Uani 1 1 d . . .
H34 H 0.5366 1.0289 0.1867 0.046 Uiso 1 1 calc R . .
C35 C 0.4559(8) 1.0091(6) 0.2810(5) 0.0363(17) Uani 1 1 d . . .
H35 H 0.4193 1.0589 0.2771 0.044 Uiso 1 1 calc R . .
C44 C 0.1287(7) 0.3742(7) 0.3767(6) 0.0421(19) Uani 1 1 d . . .
H44 H 0.0643 0.3237 0.3881 0.050 Uiso 1 1 calc R . .
N11 N 1.0414(8) 0.9707(8) 0.6356(5) 0.061(2) Uani 1 1 d . . .
C49 C 1.0462(8) 0.9243(8) 0.5716(5) 0.046(2) Uani 1 1 d . . .
C50 C 1.0471(9) 0.8654(9) 0.4895(6) 0.054(2) Uani 1 1 d . . .
H50A H 0.9675 0.8350 0.4525 0.081 Uiso 1 1 calc R . .
H50B H 1.0740 0.8074 0.4946 0.081 Uiso 1 1 calc R . .
H50C H 1.1005 0.9139 0.4655 0.081 Uiso 1 1 calc R . .
N12 N 0.7625(14) 0.2479(15) 0.4206(9) 0.122(6) Uani 1 1 d . . .
C51 C 0.7518(12) 0.2578(12) 0.3545(8) 0.075(4) Uani 1 1 d . . .
C52 C 0.7352(17) 0.2706(12) 0.2723(9) 0.096(5) Uani 1 1 d . . .
H52A H 0.6546 0.2659 0.2530 0.145 Uiso 1 1 calc R . .
H52B H 0.7487 0.2139 0.2335 0.145 Uiso 1 1 calc R . .
H52C H 0.7908 0.3409 0.2739 0.145 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
Br1 C4 1.891(7) . ?
Fe1 O1 1.876(5) . ?
Fe1 O2 1.900(5) . ?
Fe1 N1 1.930(5) . ?
Fe1 N3 1.958(5) . ?
Fe1 N2 1.978(6) . ?
Fe1 S1 2.223(2) . ?
Fe2 O4 1.918(5) . ?
Fe2 O3 1.951(5) . ?
Fe2 N9 2.120(5) . ?
Fe2 N6 2.133(6) . ?
Fe2 N7 2.170(6) . ?
Fe2 S2 2.434(2) . ?
Br2 C28 1.916(8) . ?
S1 C24 1.740(7) . ?
S2 C48 1.737(7) . ?
O2 C17 1.342(8) . ?
N3 C23 1.308(8) . ?
N3 N4 1.389(7) . ?
O1 C1 1.308(8) . ?
O3 C25 1.322(9) . ?
N1 C7 1.310(8) . ?
N1 C8 1.419(8) . ?
O4 C41 1.300(8) . ?
N2 C15 1.305(9) . ?
N2 C16 1.383(8) . ?
N4 C24 1.342(9) . ?
C1 C2 1.412(9) . ?
C1 C6 1.428(8) . ?
C7 C6 1.422(8) . ?
C7 H7 0.9500 . ?
C5 C4 1.379(9) . ?
C5 C6 1.412(9) . ?
C5 H5 0.9500 . ?
C23 C22 1.428(9) . ?
C23 H23 0.9500 . ?
C17 C18 1.392(9) . ?
C17 C22 1.429(8) . ?
N8 C48 1.323(9) . ?
N8 N9 1.385(8) . ?
N5 C24 1.335(9) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N10 C48 1.366(9) . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
N9 C47 1.294(9) . ?
C16 C12 1.407(8) . ?
C16 C8 1.417(9) . ?
C18 C19 1.384(10) . ?
C18 H18 0.9500 . ?
C4 C3 1.401(9) . ?
N6 C31 1.309(9) . ?
N6 C32 1.405(9) . ?
C21 C20 1.388(10) . ?
C21 C22 1.397(9) . ?
C21 H21 0.9500 . ?
C3 C2 1.371(10) . ?
C3 H3 0.9500 . ?
N7 C39 1.324(8) . ?
N7 C40 1.357(8) . ?
C8 C9 1.384(9) . ?
C9 C10 1.414(9) . ?
C9 H9 0.9500 . ?
C12 C13 1.394(10) . ?
C12 C11 1.433(9) . ?
C19 C20 1.404(9) . ?
C19 H19 0.9500 . ?
C31 C30 1.424(11) . ?
C31 H31 0.9500 . ?
C20 H20 0.9500 . ?
C30 C25 1.428(11) . ?
C30 C29 1.437(10) . ?
C2 H2 0.9500 . ?
C40 C36 1.401(10) . ?
C40 C32 1.443(9) . ?
C15 C14 1.406(10) . ?
C15 H15 0.9500 . ?
C38 C37 1.346(11) . ?
C38 C39 1.416(11) . ?
C38 H38 0.9500 . ?
C33 C32 1.370(10) . ?
C33 C34 1.399(11) . ?
C33 H33 0.9500 . ?
C41 C42 1.413(10) . ?
C41 C46 1.418(9) . ?
C13 C14 1.361(10) . ?
C13 H13 0.9500 . ?
C11 C10 1.376(10) . ?
C11 H11 0.9500 . ?
C28 C29 1.374(12) . ?
C28 C27 1.379(13) . ?
C36 C35 1.420(10) . ?
C36 C37 1.430(10) . ?
C46 C45 1.409(10) . ?
C46 C47 1.444(10) . ?
C10 H10 0.9500 . ?
C25 C26 1.411(11) . ?
C29 H29 0.9500 . ?
C47 H47 0.9500 . ?
C42 C43 1.378(11) . ?
C42 H42 0.9500 . ?
C14 H14 0.9500 . ?
C39 H39 0.9500 . ?
C45 C44 1.387(11) . ?
C45 H45 0.9500 . ?
C27 C26 1.388(11) . ?
C27 H27 0.9500 . ?
C37 H37 0.9500 . ?
C26 H26 0.9500 . ?
C43 C44 1.397(12) . ?
C43 H43 0.9500 . ?
C34 C35 1.383(11) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C44 H44 0.9500 . ?
N11 C49 1.144(12) . ?
C49 C50 1.441(12) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N12 C51 1.141(16) . ?
C51 C52 1.424(18) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 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 91.1(2) . . ?
O1 Fe1 N1 95.0(2) . . ?
O2 Fe1 N1 89.1(2) . . ?
O1 Fe1 N3 86.0(2) . . ?
O2 Fe1 N3 94.7(2) . . ?
N1 Fe1 N3 176.0(2) . . ?
O1 Fe1 N2 176.6(2) . . ?
O2 Fe1 N2 85.8(2) . . ?
N1 Fe1 N2 83.4(2) . . ?
N3 Fe1 N2 95.8(2) . . ?
O1 Fe1 S1 94.46(16) . . ?
O2 Fe1 S1 174.33(16) . . ?
N1 Fe1 S1 91.16(16) . . ?
N3 Fe1 S1 84.87(16) . . ?
N2 Fe1 S1 88.63(17) . . ?
O4 Fe2 O3 89.4(2) . . ?
O4 Fe2 N9 87.5(2) . . ?
O3 Fe2 N9 106.1(2) . . ?
O4 Fe2 N6 106.0(2) . . ?
O3 Fe2 N6 86.3(2) . . ?
N9 Fe2 N6 162.0(2) . . ?
O4 Fe2 N7 88.9(2) . . ?
O3 Fe2 N7 160.7(2) . . ?
N9 Fe2 N7 93.1(2) . . ?
N6 Fe2 N7 75.7(2) . . ?
O4 Fe2 S2 166.93(15) . . ?
O3 Fe2 S2 94.13(17) . . ?
N9 Fe2 S2 79.41(16) . . ?
N6 Fe2 S2 86.81(16) . . ?
N7 Fe2 S2 91.79(16) . . ?
C24 S1 Fe1 96.6(2) . . ?
C48 S2 Fe2 96.7(2) . . ?
C17 O2 Fe1 124.1(4) . . ?
C23 N3 N4 114.6(5) . . ?
C23 N3 Fe1 122.5(4) . . ?
N4 N3 Fe1 122.8(4) . . ?
C1 O1 Fe1 126.6(4) . . ?
C25 O3 Fe2 126.1(5) . . ?
C7 N1 C8 120.9(5) . . ?
C7 N1 Fe1 124.8(4) . . ?
C8 N1 Fe1 114.2(4) . . ?
C41 O4 Fe2 135.4(4) . . ?
C15 N2 C16 119.2(6) . . ?
C15 N2 Fe1 128.3(5) . . ?
C16 N2 Fe1 112.3(4) . . ?
C24 N4 N3 111.7(5) . . ?
O1 C1 C2 118.2(6) . . ?
O1 C1 C6 124.4(6) . . ?
C2 C1 C6 117.4(6) . . ?
N1 C7 C6 124.7(6) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C4 C5 C6 120.1(6) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N3 C23 C22 126.5(5) . . ?
N3 C23 H23 116.7 . . ?
C22 C23 H23 116.7 . . ?
O2 C17 C18 117.7(6) . . ?
O2 C17 C22 122.8(6) . . ?
C18 C17 C22 119.4(6) . . ?
C48 N8 N9 114.5(5) . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
N5 C24 N4 119.2(6) . . ?
N5 C24 S1 116.9(5) . . ?
N4 C24 S1 123.8(5) . . ?
N8 C48 N10 117.5(6) . . ?
N8 C48 S2 125.9(5) . . ?
N10 C48 S2 116.6(5) . . ?
C47 N9 N8 112.2(5) . . ?
C47 N9 Fe2 124.5(5) . . ?
N8 N9 Fe2 123.3(4) . . ?
N2 C16 C12 121.1(6) . . ?
N2 C16 C8 116.6(5) . . ?
C12 C16 C8 122.3(6) . . ?
C19 C18 C17 121.2(6) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 Br1 120.8(5) . . ?
C3 C4 Br1 118.5(5) . . ?
C31 N6 C32 120.3(6) . . ?
C31 N6 Fe2 122.3(5) . . ?
C32 N6 Fe2 116.2(4) . . ?
C20 C21 C22 122.9(6) . . ?
C20 C21 H21 118.5 . . ?
C22 C21 H21 118.5 . . ?
C21 C22 C23 118.4(5) . . ?
C21 C22 C17 117.7(6) . . ?
C23 C22 C17 123.9(6) . . ?
C2 C3 C4 119.8(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C39 N7 C40 118.6(6) . . ?
C39 N7 Fe2 125.5(5) . . ?
C40 N7 Fe2 115.8(4) . . ?
C9 C8 C16 119.1(6) . . ?
C9 C8 N1 127.6(6) . . ?
C16 C8 N1 113.4(5) . . ?
C8 C9 C10 119.2(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C13 C12 C16 117.9(6) . . ?
C13 C12 C11 124.6(6) . . ?
C16 C12 C11 117.5(6) . . ?
C18 C19 C20 120.5(6) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C5 C6 C7 116.4(6) . . ?
C5 C6 C1 120.0(6) . . ?
C7 C6 C1 123.6(6) . . ?
N6 C31 C30 125.1(7) . . ?
N6 C31 H31 117.4 . . ?
C30 C31 H31 117.4 . . ?
C21 C20 C19 118.2(6) . . ?
C21 C20 H20 120.9 . . ?
C19 C20 H20 120.9 . . ?
C31 C30 C25 124.8(7) . . ?
C31 C30 C29 116.3(7) . . ?
C25 C30 C29 118.9(7) . . ?
C3 C2 C1 122.1(6) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
N7 C40 C36 122.9(6) . . ?
N7 C40 C32 116.8(6) . . ?
C36 C40 C32 120.4(6) . . ?
N2 C15 C14 122.4(6) . . ?
N2 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C37 C38 C39 119.7(7) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C32 C33 C34 120.9(7) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
O4 C41 C42 120.2(6) . . ?
O4 C41 C46 122.2(6) . . ?
C42 C41 C46 117.6(7) . . ?
C33 C32 N6 126.7(6) . . ?
C33 C32 C40 118.7(7) . . ?
N6 C32 C40 114.6(6) . . ?
C14 C13 C12 120.0(7) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C10 C11 C12 119.6(6) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C29 C28 C27 123.6(7) . . ?
C29 C28 Br2 118.4(7) . . ?
C27 C28 Br2 118.0(6) . . ?
C40 C36 C35 119.2(7) . . ?
C40 C36 C37 117.0(7) . . ?
C35 C36 C37 123.8(7) . . ?
C45 C46 C41 119.7(7) . . ?
C45 C46 C47 117.3(6) . . ?
C41 C46 C47 123.0(6) . . ?
C11 C10 C9 122.4(6) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
O3 C25 C26 120.1(7) . . ?
O3 C25 C30 121.1(7) . . ?
C26 C25 C30 118.8(7) . . ?
C28 C29 C30 118.6(8) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
N9 C47 C46 127.2(6) . . ?
N9 C47 H47 116.4 . . ?
C46 C47 H47 116.4 . . ?
C43 C42 C41 121.0(7) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C13 C14 C15 119.3(7) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N7 C39 C38 122.3(7) . . ?
N7 C39 H39 118.8 . . ?
C38 C39 H39 118.8 . . ?
C44 C45 C46 122.0(7) . . ?
C44 C45 H45 119.0 . . ?
C46 C45 H45 119.0 . . ?
C28 C27 C26 118.5(8) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C38 C37 C36 119.5(7) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C27 C26 C25 121.6(8) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C42 C43 C44 122.1(8) . . ?
C42 C43 H43 118.9 . . ?
C44 C43 H43 118.9 . . ?
C35 C34 C33 121.4(7) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C34 C35 C36 119.4(7) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C45 C44 C43 117.5(8) . . ?
C45 C44 H44 121.2 . . ?
C43 C44 H44 121.2 . . ?
N11 C49 C50 177.6(11) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N12 C51 C52 178.2(17) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.169
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ws100_a
_database_code_depnum_ccdc_archive 'CCDC 1529175'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_audit_creation_date             2016-03-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            '[Fe(qsal-I)(thsa)]'
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H17 Fe I N5 O2 S'
_chemical_formula_sum            'C24 H17 Fe I N5 O2 S'
_chemical_formula_weight         622.24
_chemical_melting_point          ?
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5930(17)
_cell_length_b                   17.495(4)
_cell_length_c                   15.888(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.27(3)
_cell_angle_gamma                90.00
_cell_volume                     2304.2(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      0.993
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9589
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Bar
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19487
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         1.77
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4780
_reflns_number_total             5045
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.594
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0623
_refine_ls_restrained_S_all      1.234
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0174P)²+46.7478P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1744
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C5(H5), C23(H23), C7(H7), C3(H3), C13(H13), C11(H11), C14(H14),
 C9(H9), C19(H19), C21(H21), C15(H15), C10(H10), C20(H20), C2(H2)
2.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
I1 I -0.20073(6) 0.53468(3) 0.28250(4) 0.02700(18) Uani 1 d . . .
Fe1 Fe 0.49666(12) 0.25941(6) 0.42344(6) 0.0137(2) Uani 1 d . . .
S1 S 0.6292(2) 0.35991(11) 0.49634(12) 0.0186(4) Uani 1 d . . .
O1 O 0.3043(6) 0.2863(3) 0.4522(3) 0.0161(10) Uani 1 d . . .
O2 O 0.4006(6) 0.1695(3) 0.3604(3) 0.0202(11) Uani 1 d . . .
N3 N 0.5567(7) 0.2075(4) 0.5355(4) 0.0156(12) Uani 1 d . . .
N1 N 0.4437(7) 0.3123(3) 0.3134(4) 0.0135(11) Uani 1 d . . .
N2 N 0.6955(7) 0.2332(3) 0.3889(4) 0.0147(11) Uani 1 d . . .
N4 N 0.6606(7) 0.2403(4) 0.6091(4) 0.0195(13) Uani 1 d . . .
C17 C 0.3420(8) 0.1126(4) 0.3961(5) 0.0168(14) Uani 1 d . . .
C4 C -0.0267(9) 0.4519(4) 0.3390(5) 0.0203(15) Uani 1 d . . .
C18 C 0.2283(9) 0.0635(4) 0.3415(5) 0.0176(14) Uani 1 d . . .
H18 H 0.2043 0.0696 0.2800 0.021 Uiso 1 calc . . R
C16 C 0.6901(8) 0.2570(4) 0.3059(4) 0.0138(13) Uani 1 d . . .
N5 N 0.7956(9) 0.3506(4) 0.6612(5) 0.0280(15) Uani 1 d . . .
H5A H 0.8324 0.3286 0.7124 0.034 Uiso 1 calc . . R
H5B H 0.8224 0.3981 0.6533 0.034 Uiso 1 calc . . R
C5 C 0.0884(9) 0.4320(4) 0.2977(5) 0.0173(14) Uani 1 d . . .
H5 H 0.0896 0.4560 0.2443 0.021 Uiso 1 calc . . R
C8 C 0.5525(8) 0.2988(4) 0.2621(4) 0.0148(13) Uani 1 d . . .
C23 C 0.4978(9) 0.1437(4) 0.5512(5) 0.0178(14) Uani 1 d . . .
H23 H 0.5325 0.1244 0.6090 0.021 Uiso 1 calc . . R
C7 C 0.3197(8) 0.3579(4) 0.2865(5) 0.0159(13) Uani 1 d . . .
H7 H 0.3048 0.3808 0.2307 0.019 Uiso 1 calc . . R
C1 C 0.2047(9) 0.3393(4) 0.4143(5) 0.0169(14) Uani 1 d . . .
C12 C 0.8149(8) 0.2405(4) 0.2663(5) 0.0158(13) Uani 1 d . . .
C22 C 0.3819(9) 0.0981(4) 0.4877(5) 0.0174(14) Uani 1 d . . .
C3 C -0.0279(9) 0.4186(5) 0.4186(5) 0.0204(15) Uani 1 d . . .
H3 H -0.1068 0.4337 0.4474 0.024 Uiso 1 calc . . R
C13 C 0.9502(9) 0.2000(4) 0.3158(5) 0.0176(14) Uani 1 d . . .
H13 H 1.0387 0.1892 0.2923 0.021 Uiso 1 calc . . R
C6 C 0.2059(8) 0.3758(4) 0.3340(5) 0.0161(14) Uani 1 d . . .
C11 C 0.7979(9) 0.2641(4) 0.1800(5) 0.0185(14) Uani 1 d . . .
H11 H 0.8809 0.2541 0.1521 0.022 Uiso 1 calc . . R
C14 C 0.9520(9) 0.1764(5) 0.3988(5) 0.0194(15) Uani 1 d . . .
H14 H 1.0411 0.1483 0.4329 0.023 Uiso 1 calc . . R
C9 C 0.5366(9) 0.3201(4) 0.1765(5) 0.0173(14) Uani 1 d . . .
H9 H 0.4431 0.3467 0.1450 0.021 Uiso 1 calc . . R
C19 C 0.1507(9) 0.0065(5) 0.3759(6) 0.0233(16) Uani 1 d . . .
H19 H 0.0708 -0.0239 0.3378 0.028 Uiso 1 calc . . R
C21 C 0.3047(9) 0.0377(5) 0.5192(5) 0.0224(16) Uani 1 d . . .
H21 H 0.3340 0.0272 0.5801 0.027 Uiso 1 calc . . R
C15 C 0.8220(9) 0.1939(4) 0.4324(5) 0.0181(14) Uani 1 d . . .
H15 H 0.8246 0.1767 0.4894 0.022 Uiso 1 calc . . R
C24 C 0.6980(9) 0.3114(5) 0.5947(5) 0.0191(15) Uani 1 d . . .
C10 C 0.6601(10) 0.3019(5) 0.1361(5) 0.0226(16) Uani 1 d . . .
H10 H 0.6476 0.3162 0.0770 0.027 Uiso 1 calc . . R
C20 C 0.1879(10) -0.0068(5) 0.4648(6) 0.0239(16) Uani 1 d . . .
H20 H 0.1342 -0.0458 0.4879 0.029 Uiso 1 calc . . R
C2 C 0.0848(9) 0.3639(5) 0.4556(5) 0.0206(15) Uani 1 d . . .
H2 H 0.0825 0.3420 0.5100 0.025 Uiso 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
I1 C4 2.105(8) . ?
Fe1 S1 2.244(2) . ?
Fe1 O1 1.887(5) . ?
Fe1 O2 1.929(6) . ?
Fe1 N3 1.944(6) . ?
Fe1 N1 1.924(6) . ?
Fe1 N2 1.981(6) . ?
S1 C24 1.739(8) . ?
O1 C1 1.298(9) . ?
O2 C17 1.310(9) . ?
N3 N4 1.394(9) . ?
N3 C23 1.277(10) . ?
N1 C8 1.413(8) . ?
N1 C7 1.309(9) . ?
N2 C16 1.371(9) . ?
N2 C15 1.317(9) . ?
N4 C24 1.319(10) . ?
C17 C18 1.413(10) . ?
C17 C22 1.427(10) . ?
C4 C5 1.368(10) . ?
C4 C3 1.394(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(11) . ?
C16 C8 1.409(10) . ?
C16 C12 1.409(9) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C24 1.350(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.419(10) . ?
C8 C9 1.381(10) . ?
C23 H23 0.9500 . ?
C23 C22 1.455(11) . ?
C7 H7 0.9500 . ?
C7 C6 1.420(10) . ?
C1 C6 1.428(10) . ?
C1 C2 1.425(10) . ?
C12 C13 1.411(10) . ?
C12 C11 1.402(10) . ?
C22 C21 1.409(10) . ?
C3 H3 0.9500 . ?
C3 C2 1.378(11) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(10) . ?
C11 H11 0.9500 . ?
C11 C10 1.375(11) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.414(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(12) . ?
C21 H21 0.9500 . ?
C21 C20 1.379(12) . ?
C15 H15 0.9500 . ?
C10 H10 0.9500 . ?
C20 H20 0.9500 . ?
C2 H2 0.9500 . ?

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 S1 92.15(17) . . ?
O1 Fe1 O2 92.7(2) . . ?
O1 Fe1 N3 86.2(2) . . ?
O1 Fe1 N1 95.0(2) . . ?
O1 Fe1 N2 177.8(2) . . ?
O2 Fe1 S1 175.04(18) . . ?
O2 Fe1 N3 93.9(2) . . ?
O2 Fe1 N2 87.1(2) . . ?
N3 Fe1 S1 85.3(2) . . ?
N3 Fe1 N2 96.1(2) . . ?
N1 Fe1 S1 93.38(18) . . ?
N1 Fe1 O2 87.4(2) . . ?
N1 Fe1 N3 178.2(3) . . ?
N1 Fe1 N2 82.8(2) . . ?
N2 Fe1 S1 88.11(19) . . ?
C24 S1 Fe1 95.0(3) . . ?
C1 O1 Fe1 125.4(4) . . ?
C17 O2 Fe1 123.8(5) . . ?
N4 N3 Fe1 122.2(5) . . ?
C23 N3 Fe1 124.3(5) . . ?
C23 N3 N4 113.3(6) . . ?
C8 N1 Fe1 114.2(5) . . ?
C7 N1 Fe1 124.6(5) . . ?
C7 N1 C8 121.2(6) . . ?
C16 N2 Fe1 112.5(5) . . ?
C15 N2 Fe1 128.9(5) . . ?
C15 N2 C16 118.5(6) . . ?
C24 N4 N3 112.0(6) . . ?
O2 C17 C18 118.6(7) . . ?
O2 C17 C22 124.0(7) . . ?
C18 C17 C22 117.3(7) . . ?
C5 C4 I1 119.5(6) . . ?
C5 C4 C3 120.5(7) . . ?
C3 C4 I1 120.0(5) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.4(7) . . ?
C19 C18 H18 119.3 . . ?
N2 C16 C8 116.4(6) . . ?
N2 C16 C12 122.0(6) . . ?
C12 C16 C8 121.6(6) . . ?
H5A N5 H5B 120.0 . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(7) . . ?
C6 C5 H5 119.7 . . ?
C16 C8 N1 113.5(6) . . ?
C9 C8 N1 127.9(7) . . ?
C9 C8 C16 118.6(6) . . ?
N3 C23 H23 117.3 . . ?
N3 C23 C22 125.3(7) . . ?
C22 C23 H23 117.3 . . ?
N1 C7 H7 117.4 . . ?
N1 C7 C6 125.2(7) . . ?
C6 C7 H7 117.4 . . ?
O1 C1 C6 125.0(6) . . ?
O1 C1 C2 118.1(6) . . ?
C2 C1 C6 116.9(7) . . ?
C16 C12 C13 117.8(6) . . ?
C11 C12 C16 118.7(7) . . ?
C11 C12 C13 123.5(7) . . ?
C17 C22 C23 123.1(7) . . ?
C21 C22 C17 119.2(7) . . ?
C21 C22 C23 117.7(7) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 C4 120.3(7) . . ?
C2 C3 H3 119.8 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 118.9(7) . . ?
C14 C13 H13 120.5 . . ?
C5 C6 C1 120.0(6) . . ?
C7 C6 C5 116.9(6) . . ?
C7 C6 C1 123.0(7) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 C12 119.5(6) . . ?
C10 C11 H11 120.3 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.5(7) . . ?
C15 C14 H14 120.3 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(7) . . ?
C10 C9 H9 120.2 . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.1(7) . . ?
C20 C19 H19 119.4 . . ?
C22 C21 H21 118.9 . . ?
C20 C21 C22 122.2(7) . . ?
C20 C21 H21 118.9 . . ?
N2 C15 C14 123.3(7) . . ?
N2 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N4 C24 S1 125.1(6) . . ?
N4 C24 N5 118.2(7) . . ?
N5 C24 S1 116.7(6) . . ?
C11 C10 C9 121.8(7) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C19 C20 H20 120.7 . . ?
C21 C20 C19 118.6(7) . . ?
C21 C20 H20 120.7 . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.7(7) . . ?
C3 C2 H2 119.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_270_a
_database_code_depnum_ccdc_archive 'CCDC 1529174'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(qsal-F)(thsa)]2.5MeCN'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H49 F2 Fe2 N15 O4 S2'
_chemical_formula_weight         1233.94

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   13.273(3)
_cell_length_b                   16.547(3)
_cell_length_c                   16.540(3)
_cell_angle_alpha                60.35(3)
_cell_angle_beta                 108.54(3)
_cell_angle_gamma                110.33(3)
_cell_volume                     2912.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    16505
_cell_measurement_theta_min      0.824
_cell_measurement_theta_max      31.889

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.636
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'XScale within XDS'

_exptl_special_details           
;
This strcutures has been solved and refined by reasonable model.
The acetonitril molecules, N11 and N11', are disorder over two position and the total occupancy is one. 
Two molecules of MeCN are disorderd over 4 position (molecules of N15-N18). 
This has been treated the same as the structure at 100 K that shows no solvent loss after 
the warming after 320 K.
However, the anisotropy cannot applied on N17 and N18 molecules because of the thermal effect 
resulting in the weak diffractions and severly disorder of the solvents.
;

_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1, Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67098
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.440
_diffrn_reflns_theta_max         31.889
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             16505
_reflns_number_gt                14001
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0698P)²+0.9124P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16505
_refine_ls_number_parameters     813
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.1297
_refine_ls_wR_factor_gt          0.1239
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.40733(2) 0.78929(2) -0.03232(2) 0.03630(6) Uani 1 1 d . . . . .
Fe2 Fe 0.47804(2) 0.24523(2) 0.57779(2) 0.03934(7) Uani 1 1 d . . . . .
S1 S 0.51248(4) 0.78918(3) 0.10307(3) 0.04173(9) Uani 1 1 d . . . . .
S2 S 0.36112(4) 0.24443(3) 0.43252(3) 0.05278(11) Uani 1 1 d . . . . .
O2 O 0.32575(11) 0.78959(9) -0.15059(8) 0.0499(3) Uani 1 1 d . . . . .
O1 O 0.28012(10) 0.78012(8) 0.00200(9) 0.0456(3) Uani 1 1 d . . . . .
O4 O 0.59162(11) 0.27666(9) 0.67019(8) 0.0504(3) Uani 1 1 d . . . . .
O3 O 0.36833(12) 0.24981(10) 0.62946(10) 0.0551(3) Uani 1 1 d . . . . .
N1 N 0.44675(11) 0.92767(9) -0.09319(9) 0.0366(2) Uani 1 1 d . . . . .
N9 N 0.53005(12) 0.39019(9) 0.47993(9) 0.0403(3) Uani 1 1 d . . . . .
N3 N 0.38014(11) 0.65087(9) 0.03662(9) 0.0392(3) Uani 1 1 d . . . . .
N2 N 0.53884(12) 0.80346(10) -0.07476(10) 0.0421(3) Uani 1 1 d . . . . .
N4 N 0.43033(13) 0.60567(9) 0.13055(9) 0.0428(3) Uani 1 1 d . . . . .
N8 N 0.48799(13) 0.42412(10) 0.38354(10) 0.0475(3) Uani 1 1 d . . . . .
F1 F 0.09368(15) 1.06377(12) -0.07664(15) 0.0999(6) Uani 1 1 d . . . . .
N6 N 0.41546(14) 0.09185(10) 0.63801(10) 0.0470(3) Uani 1 1 d . . . . .
N10 N 0.37016(16) 0.39051(12) 0.26476(11) 0.0606(4) Uani 1 1 d . . . . .
H10A H 0.3942 0.4479 0.2252 0.073 Uiso 1 1 calc R U . . .
H10B H 0.3198 0.3516 0.2449 0.073 Uiso 1 1 calc R U . . .
N5 N 0.54224(13) 0.63149(10) 0.25719(10) 0.0472(3) Uani 1 1 d . . . . .
H5A H 0.5356 0.5709 0.2905 0.057 Uiso 1 1 calc R U . . .
H5B H 0.5819 0.6702 0.2817 0.057 Uiso 1 1 calc R U . . .
C23 C 0.31295(14) 0.59206(12) 0.00250(12) 0.0446(3) Uani 1 1 d . . . . .
H23 H 0.3046 0.5271 0.0422 0.053 Uiso 1 1 calc R U . . .
C16 C 0.59517(14) 0.89588(12) -0.11408(11) 0.0401(3) Uani 1 1 d . . . . .
N7 N 0.59131(14) 0.19176(13) 0.55891(12) 0.0545(4) Uani 1 1 d . . . . .
C47 C 0.60107(15) 0.45608(12) 0.50268(12) 0.0452(3) Uani 1 1 d . . . . .
H47 H 0.6130 0.5174 0.4539 0.054 Uiso 1 1 calc R U . . .
C7 C 0.38837(14) 0.98247(11) -0.10480(11) 0.0402(3) Uani 1 1 d . . . . .
H7 H 0.4135 1.0480 -0.1379 0.048 Uiso 1 1 calc R U . . .
C41 C 0.65693(14) 0.35505(12) 0.67474(11) 0.0426(3) Uani 1 1 d . . . . .
C8 C 0.54861(13) 0.96629(11) -0.12415(10) 0.0373(3) Uani 1 1 d . . . . .
C22 C 0.24993(14) 0.61939(13) -0.09234(13) 0.0466(4) Uani 1 1 d . . . . .
C46 C 0.66325(14) 0.44485(12) 0.59478(12) 0.0444(3) Uani 1 1 d . . . . .
C24 C 0.49052(14) 0.66567(11) 0.16682(11) 0.0394(3) Uani 1 1 d . . . . .
C17 C 0.25888(15) 0.71509(14) -0.16230(12) 0.0484(4) Uani 1 1 d . . . . .
C1 C 0.24127(14) 0.85225(12) -0.01856(11) 0.0424(3) Uani 1 1 d . . . . .
C25 C 0.27295(17) 0.19173(17) 0.64740(14) 0.0581(5) Uani 1 1 d . . . . .
C12 C 0.69448(15) 0.92161(14) -0.14454(13) 0.0486(4) Uani 1 1 d . . . . .
C48 C 0.41147(15) 0.36149(12) 0.35793(12) 0.0438(3) Uani 1 1 d . . . . .
C6 C 0.28863(14) 0.95017(12) -0.07084(12) 0.0430(3) Uani 1 1 d . . . . .
C9 C 0.60282(14) 1.06075(12) -0.16176(11) 0.0437(3) Uani 1 1 d . . . . .
H9 H 0.5737 1.1076 -0.1679 0.052 Uiso 1 1 calc R U . . .
C32 C 0.4759(2) 0.03925(13) 0.63245(12) 0.0551(5) Uani 1 1 d . . . . .
C42 C 0.72235(16) 0.35140(15) 0.76176(13) 0.0534(4) Uani 1 1 d . . . . .
H42 H 0.7201 0.2930 0.8150 0.064 Uiso 1 1 calc R U . . .
C5 C 0.23685(17) 1.02100(14) -0.08949(15) 0.0555(4) Uani 1 1 d . . . . .
H5 H 0.2673 1.0853 -0.1235 0.067 Uiso 1 1 calc R U . . .
C2 C 0.14411(17) 0.83036(15) 0.01388(15) 0.0554(4) Uani 1 1 d . . . . .
H2 H 0.1126 0.7669 0.0495 0.066 Uiso 1 1 calc R U . . .
C15 C 0.57570(18) 0.73529(14) -0.06877(15) 0.0561(4) Uani 1 1 d . . . . .
H15 H 0.5367 0.6722 -0.0427 0.067 Uiso 1 1 calc R U . . .
C10 C 0.70299(16) 1.08623(14) -0.19098(13) 0.0519(4) Uani 1 1 d . . . . .
H10 H 0.7393 1.1503 -0.2163 0.062 Uiso 1 1 calc R U . . .
C40 C 0.56875(19) 0.09558(15) 0.58871(13) 0.0563(5) Uani 1 1 d . . . . .
F2 F -0.02733(16) 0.0147(2) 0.7163(2) 0.1594(12) Uani 1 1 d . . . . .
C45 C 0.73299(18) 0.52666(15) 0.60484(15) 0.0598(5) Uani 1 1 d . . . . .
H45 H 0.7371 0.5856 0.5523 0.072 Uiso 1 1 calc R U . . .
C21 C 0.17594(17) 0.54495(16) -0.11407(16) 0.0582(5) Uani 1 1 d . . . . .
H21 H 0.1719 0.4821 -0.0684 0.070 Uiso 1 1 calc R U . . .
C11 C 0.74762(16) 1.01943(15) -0.18303(14) 0.0551(4) Uani 1 1 d . . . . .
H11 H 0.8135 1.0383 -0.2031 0.066 Uiso 1 1 calc R U . . .
C31 C 0.3213(2) 0.04992(15) 0.66384(14) 0.0612(5) Uani 1 1 d . . . . .
H31 H 0.2988 -0.0156 0.6822 0.073 Uiso 1 1 calc R U . . .
C43 C 0.78949(19) 0.43293(18) 0.76917(16) 0.0645(5) Uani 1 1 d . . . . .
H43 H 0.8316 0.4289 0.8274 0.077 Uiso 1 1 calc R U . . .
C18 C 0.19052(19) 0.73071(18) -0.25177(15) 0.0656(6) Uani 1 1 d . . . . .
H18 H 0.1952 0.7927 -0.2996 0.079 Uiso 1 1 calc R U . . .
C3 C 0.09515(18) 0.90035(17) -0.00585(17) 0.0637(5) Uani 1 1 d . . . . .
H3 H 0.0308 0.8846 0.0153 0.076 Uiso 1 1 calc R U . . .
C30 C 0.24830(18) 0.09421(18) 0.66702(15) 0.0628(5) Uani 1 1 d . . . . .
C36 C 0.6371(3) 0.0529(2) 0.57801(17) 0.0766(8) Uani 1 1 d . . . . .
C20 C 0.10956(19) 0.56288(19) -0.20114(18) 0.0703(6) Uani 1 1 d . . . . .
H20 H 0.0601 0.5129 -0.2138 0.084 Uiso 1 1 calc R U . . .
C33 C 0.4535(3) -0.05818(16) 0.66524(16) 0.0774(8) Uani 1 1 d . . . . .
H33 H 0.3942 -0.0970 0.6957 0.093 Uiso 1 1 calc R U . . .
C44 C 0.7956(2) 0.52148(18) 0.69090(17) 0.0690(6) Uani 1 1 d . . . . .
H44 H 0.8411 0.5763 0.6966 0.083 Uiso 1 1 calc R U . . .
C13 C 0.73154(19) 0.84725(17) -0.13636(17) 0.0629(5) Uani 1 1 d . . . . .
H13 H 0.7967 0.8607 -0.1553 0.075 Uiso 1 1 calc R U . . .
C26 C 0.1913(2) 0.2270(3) 0.6490(2) 0.0819(8) Uani 1 1 d . . . . .
H26 H 0.2044 0.2912 0.6348 0.098 Uiso 1 1 calc R U . . .
C4 C 0.14350(19) 0.99504(16) -0.05790(18) 0.0652(6) Uani 1 1 d . . . . .
C14 C 0.6714(2) 0.75557(17) -0.10049(18) 0.0671(6) Uani 1 1 d . . . . .
H14 H 0.6940 0.7066 -0.0971 0.080 Uiso 1 1 calc R U . . .
C19 C 0.1173(2) 0.6560(2) -0.26934(17) 0.0760(7) Uani 1 1 d . . . . .
H19 H 0.0724 0.6685 -0.3283 0.091 Uiso 1 1 calc R U . . .
C39 C 0.6782(2) 0.2460(2) 0.5196(2) 0.0775(7) Uani 1 1 d . . . . .
H39 H 0.6934 0.3116 0.4998 0.093 Uiso 1 1 calc R U . . .
C37 C 0.7279(3) 0.1142(3) 0.5348(2) 0.1006(11) Uani 1 1 d . . . . .
H37 H 0.7739 0.0890 0.5259 0.121 Uiso 1 1 calc R U . . .
C51 C 0.0743(2) 0.3236(3) 0.1200(3) 0.0889(9) Uani 1 1 d . . . . .
C28 C 0.0716(2) 0.0726(3) 0.6924(3) 0.1065(13) Uani 1 1 d . . . . .
C35 C 0.6085(4) -0.0465(3) 0.6097(2) 0.0967(11) Uani 1 1 d . . . . .
H35 H 0.6501 -0.0760 0.6012 0.116 Uiso 1 1 calc R U . . .
C29 C 0.1456(2) 0.0350(3) 0.6912(2) 0.0899(9) Uani 1 1 d . . . . .
H29 H 0.1296 -0.0296 0.7061 0.108 Uiso 1 1 calc R U . . .
C34 C 0.5218(4) -0.0993(2) 0.6521(2) 0.1002(12) Uani 1 1 d . . . . .
H34 H 0.5054 -0.1652 0.6739 0.120 Uiso 1 1 calc R U . . .
C38 C 0.7488(3) 0.2085(3) 0.5064(3) 0.1022(11) Uani 1 1 d . . . . .
H38 H 0.8093 0.2488 0.4783 0.123 Uiso 1 1 calc R U . . .
C55 C 0.1456(3) 1.3060(2) -0.1266(3) 0.0880(8) Uani 1 1 d . . . . .
C27 C 0.0907(3) 0.1658(4) 0.6718(3) 0.1053(12) Uani 1 1 d . . . . .
H27 H 0.0370 0.1892 0.6728 0.126 Uiso 1 1 calc R U . . .
N13 N 0.0823(3) 1.3201(3) -0.1058(3) 0.1399(14) Uani 1 1 d . . . . .
N12 N 0.1529(3) 0.3089(4) 0.1607(3) 0.1497(16) Uani 1 1 d . . . . .
C52 C -0.0241(3) 0.3522(4) 0.0591(4) 0.1421(18) Uani 1 1 d . . . . .
H52A H -0.0239 0.4128 0.0536 0.213 Uiso 1 1 calc R U . . .
H52B H -0.0862 0.3052 0.0854 0.213 Uiso 1 1 calc R U . . .
H52C H -0.0278 0.3577 -0.0023 0.213 Uiso 1 1 calc R U . . .
C56 C 0.2295(4) 1.2914(3) -0.1501(3) 0.1253(14) Uani 1 1 d . . . . .
H56A H 0.2786 1.2619 -0.0934 0.188 Uiso 1 1 calc R U . . .
H56B H 0.2690 1.3517 -0.1909 0.188 Uiso 1 1 calc R U . . .
H56C H 0.1980 1.2506 -0.1818 0.188 Uiso 1 1 calc R U . . .
C60 C 0.377(2) 0.5781(18) -0.2355(17) 0.167(9) Uani 0.527(3) 1 d D . P A 4
H60A H 0.3233 0.6098 -0.2451 0.251 Uiso 0.527(3) 1 calc R U P A 4
H60B H 0.3433 0.5273 -0.2548 0.251 Uiso 0.527(3) 1 calc R U P A 4
H60C H 0.4326 0.6231 -0.2725 0.251 Uiso 0.527(3) 1 calc R U P A 4
N15 N 0.4667(6) 0.5052(4) -0.0517(5) 0.119(2) Uani 0.527(3) 1 d D . P A 4
C61 C 0.4296(6) 0.5367(5) -0.1303(6) 0.102(2) Uani 0.527(3) 1 d D . P A 4
N16 N 0.7790(7) 0.4879(7) 0.3660(6) 0.147(3) Uani 0.507(3) 1 d D . P B 5
C63 C 0.7157(7) 0.4638(6) 0.3112(6) 0.108(2) Uani 0.507(3) 1 d D . P B 5
C62 C 0.6320(15) 0.4346(16) 0.2358(18) 0.136(8) Uani 0.507(3) 1 d D . P B 5
H62A H 0.5642 0.4496 0.2263 0.204 Uiso 0.507(3) 1 calc R U P B 5
H62B H 0.6203 0.3671 0.2566 0.204 Uiso 0.507(3) 1 calc R U P B 5
H62C H 0.6591 0.4688 0.1774 0.204 Uiso 0.507(3) 1 calc R U P B 5
C49 C -0.0785(17) -0.173(2) 0.603(2) 0.275(19) Uani 0.435(3) 1 d . . P C 2
H49A H -0.0226 -0.1733 0.5778 0.413 Uiso 0.435(3) 1 calc R U P C 2
H49B H -0.1412 -0.2232 0.5998 0.413 Uiso 0.435(3) 1 calc R U P C 2
H49C H -0.0515 -0.1826 0.6673 0.413 Uiso 0.435(3) 1 calc R U P C 2
N11 N -0.1401(5) -0.0055(6) 0.5040(6) 0.0934(19) Uani 0.435(3) 1 d D . P C 2
C50 C -0.1111(5) -0.0752(6) 0.5434(6) 0.088(2) Uani 0.435(3) 1 d D . P C 2
N11' N 0.1069(5) -0.0715(6) 0.5428(4) 0.1072(17) Uani 0.565(3) 1 d . . P D 3
C50' C 0.0227(5) -0.1158(5) 0.5604(4) 0.0928(17) Uani 0.565(3) 1 d . . P D 3
C49' C -0.0747(12) -0.1586(11) 0.5806(10) 0.113(3) Uani 0.565(3) 1 d . . P D 3
H49D H -0.1105 -0.1125 0.5712 0.169 Uiso 0.565(3) 1 calc R U P D 3
H49E H -0.0695 -0.2055 0.6453 0.169 Uiso 0.565(3) 1 calc R U P D 3
H49F H -0.1160 -0.1895 0.5400 0.169 Uiso 0.565(3) 1 calc R U P D 3
N18 N 0.9396(7) 0.4307(8) 0.6191(7) 0.095(2) Uiso 0.351(3) 1 d D . P E 7
C65 C 0.0416(14) 0.4332(16) -0.3846(16) 0.326(10) Uiso 0.615(3) 1 d D . P F 6
C67 C 0.963(2) 0.5154(10) 0.5780(16) 0.226(10) Uiso 0.351(3) 1 d D . P E 7
N17 N 0.1306(14) 0.4825(13) -0.3885(14) 0.331(9) Uiso 0.615(3) 1 d D . P F 6
C64 C -0.0611(9) 0.3766(9) -0.3579(8) 0.177(4) Uiso 0.615(3) 1 d D . P F 6
H64A H -0.0860 0.4048 -0.3314 0.265 Uiso 0.615(3) 1 calc R U P F 6
H64B H -0.0537 0.3133 -0.3118 0.265 Uiso 0.615(3) 1 calc R U P F 6
H64C H -0.1131 0.3734 -0.4126 0.265 Uiso 0.615(3) 1 calc R U P F 6
C66 C 1.0014(18) 0.6153(12) 0.5140(14) 0.224(9) Uiso 0.351(3) 1 d D . P E 7
H66A H 0.9540 0.6522 0.5062 0.337 Uiso 0.351(3) 1 calc R U P E 7
H66B H 1.0007 0.6198 0.4537 0.337 Uiso 0.351(3) 1 calc R U P E 7
H66C H 1.0744 0.6395 0.5402 0.337 Uiso 0.351(3) 1 calc R U P E 7


_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 O1 1.8821(13) . ?
Fe1 O2 1.9096(14) . ?
Fe1 N1 1.9369(15) . ?
Fe1 N3 1.9443(15) . ?
Fe1 N2 1.9814(15) . ?
Fe1 S1 2.2301(9) . ?
Fe2 O4 1.9119(15) . ?
Fe2 O3 1.9465(14) . ?
Fe2 N9 2.1374(17) . ?
Fe2 N7 2.1532(17) . ?
Fe2 N6 2.1641(17) . ?
Fe2 S2 2.4141(10) . ?
S1 C24 1.7386(17) . ?
S2 C48 1.7265(19) . ?
O2 C17 1.308(2) . ?
O1 C1 1.312(2) . ?
O4 C41 1.309(2) . ?
O3 C25 1.314(2) . ?
N1 C7 1.297(2) . ?
N1 C8 1.419(2) . ?
N9 C47 1.298(2) . ?
N9 N8 1.3910(19) . ?
N3 C23 1.297(2) . ?
N3 N4 1.3983(19) . ?
N2 C15 1.328(2) . ?
N2 C16 1.361(2) . ?
N4 C24 1.310(2) . ?
N8 C48 1.309(2) . ?
F1 C4 1.368(2) . ?
N6 C31 1.292(3) . ?
N6 C32 1.422(3) . ?
N10 C48 1.349(2) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N5 C24 1.344(2) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C23 C22 1.446(3) . ?
C23 H23 0.9300 . ?
C16 C12 1.412(2) . ?
C16 C8 1.418(2) . ?
N7 C39 1.319(3) . ?
N7 C40 1.361(3) . ?
C47 C46 1.436(2) . ?
C47 H47 0.9300 . ?
C7 C6 1.428(2) . ?
C7 H7 0.9300 . ?
C41 C42 1.409(2) . ?
C41 C46 1.416(2) . ?
C8 C9 1.374(2) . ?
C22 C21 1.409(3) . ?
C22 C17 1.416(3) . ?
C46 C45 1.404(3) . ?
C17 C18 1.418(3) . ?
C1 C2 1.416(2) . ?
C1 C6 1.421(2) . ?
C25 C26 1.411(3) . ?
C25 C30 1.414(3) . ?
C12 C13 1.410(3) . ?
C12 C11 1.413(3) . ?
C6 C5 1.417(2) . ?
C9 C10 1.413(3) . ?
C9 H9 0.9300 . ?
C32 C33 1.373(3) . ?
C32 C40 1.419(3) . ?
C42 C43 1.374(3) . ?
C42 H42 0.9300 . ?
C5 C4 1.346(3) . ?
C5 H5 0.9300 . ?
C2 C3 1.373(3) . ?
C2 H2 0.9300 . ?
C15 C14 1.398(3) . ?
C15 H15 0.9300 . ?
C10 C11 1.361(3) . ?
C10 H10 0.9300 . ?
C40 C36 1.423(3) . ?
F2 C28 1.371(3) . ?
C45 C44 1.378(3) . ?
C45 H45 0.9300 . ?
C21 C20 1.375(3) . ?
C21 H21 0.9300 . ?
C11 H11 0.9300 . ?
C31 C30 1.429(4) . ?
C31 H31 0.9300 . ?
C43 C44 1.392(3) . ?
C43 H43 0.9300 . ?
C18 C19 1.378(3) . ?
C18 H18 0.9300 . ?
C3 C4 1.388(3) . ?
C3 H3 0.9300 . ?
C30 C29 1.417(3) . ?
C36 C35 1.402(4) . ?
C36 C37 1.404(5) . ?
C20 C19 1.378(4) . ?
C20 H20 0.9300 . ?
C33 C34 1.425(5) . ?
C33 H33 0.9300 . ?
C44 H44 0.9300 . ?
C13 C14 1.364(3) . ?
C13 H13 0.9300 . ?
C26 C27 1.397(4) . ?
C26 H26 0.9300 . ?
C14 H14 0.9300 . ?
C19 H19 0.9300 . ?
C39 C38 1.407(4) . ?
C39 H39 0.9300 . ?
C37 C38 1.337(5) . ?
C37 H37 0.9300 . ?
C51 N12 1.081(4) . ?
C51 C52 1.436(5) . ?
C28 C29 1.342(5) . ?
C28 C27 1.351(6) . ?
C35 C34 1.338(5) . ?
C35 H35 0.9300 . ?
C29 H29 0.9300 . ?
C34 H34 0.9300 . ?
C38 H38 0.9300 . ?
C55 N13 1.131(4) . ?
C55 C56 1.416(5) . ?
C27 H27 0.9300 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C60 C61 1.54(3) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
N15 C61 1.142(7) . ?
N15 N15 1.610(14) 2_665 ?
N16 C63 1.152(8) . ?
C63 C62 1.54(3) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C49 C50 1.55(3) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
N11 C50 1.143(8) . ?
N11' C50' 1.140(8) . ?
C50' C49' 1.299(15) . ?
C49' H49D 0.9600 . ?
C49' H49E 0.9600 . ?
C49' H49F 0.9600 . ?
N18 C67 1.189(9) . ?
C65 N17 1.180(9) . ?
C65 C64 1.420(9) . ?
C67 C66 1.461(10) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O2 90.69(6) . . ?
O1 Fe1 N1 95.48(6) . . ?
O2 Fe1 N1 89.46(7) . . ?
O1 Fe1 N3 87.02(6) . . ?
O2 Fe1 N3 95.02(7) . . ?
N1 Fe1 N3 174.85(6) . . ?
O1 Fe1 N2 177.21(6) . . ?
O2 Fe1 N2 87.20(6) . . ?
N1 Fe1 N2 82.68(7) . . ?
N3 Fe1 N2 94.98(7) . . ?
O1 Fe1 S1 93.15(5) . . ?
O2 Fe1 S1 176.15(4) . . ?
N1 Fe1 S1 90.35(5) . . ?
N3 Fe1 S1 85.01(6) . . ?
N2 Fe1 S1 88.96(5) . . ?
O4 Fe2 O3 90.79(6) . . ?
O4 Fe2 N9 86.20(6) . . ?
O3 Fe2 N9 103.83(7) . . ?
O4 Fe2 N7 87.35(7) . . ?
O3 Fe2 N7 160.43(7) . . ?
N9 Fe2 N7 95.48(7) . . ?
O4 Fe2 N6 108.42(7) . . ?
O3 Fe2 N6 86.50(7) . . ?
N9 Fe2 N6 162.20(5) . . ?
N7 Fe2 N6 75.67(7) . . ?
O4 Fe2 S2 164.78(4) . . ?
O3 Fe2 S2 96.68(5) . . ?
N9 Fe2 S2 79.16(5) . . ?
N7 Fe2 S2 89.93(6) . . ?
N6 Fe2 S2 85.34(6) . . ?
C24 S1 Fe1 96.27(7) . . ?
C48 S2 Fe2 97.67(7) . . ?
C17 O2 Fe1 125.35(12) . . ?
C1 O1 Fe1 125.70(11) . . ?
C41 O4 Fe2 136.10(11) . . ?
C25 O3 Fe2 130.41(13) . . ?
C7 N1 C8 121.36(14) . . ?
C7 N1 Fe1 124.73(11) . . ?
C8 N1 Fe1 113.91(10) . . ?
C47 N9 N8 112.71(14) . . ?
C47 N9 Fe2 124.86(11) . . ?
N8 N9 Fe2 122.42(11) . . ?
C23 N3 N4 113.70(14) . . ?
C23 N3 Fe1 124.41(12) . . ?
N4 N3 Fe1 121.86(11) . . ?
C15 N2 C16 118.96(16) . . ?
C15 N2 Fe1 128.04(14) . . ?
C16 N2 Fe1 112.99(11) . . ?
C24 N4 N3 113.11(13) . . ?
C48 N8 N9 114.91(14) . . ?
C31 N6 C32 120.07(18) . . ?
C31 N6 Fe2 123.73(15) . . ?
C32 N6 Fe2 115.31(13) . . ?
C48 N10 H10A 120.0 . . ?
C48 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C24 N5 H5A 120.0 . . ?
C24 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
N3 C23 C22 125.26(16) . . ?
N3 C23 H23 117.4 . . ?
C22 C23 H23 117.4 . . ?
N2 C16 C12 122.34(15) . . ?
N2 C16 C8 116.63(14) . . ?
C12 C16 C8 121.03(16) . . ?
C39 N7 C40 119.2(2) . . ?
C39 N7 Fe2 124.29(17) . . ?
C40 N7 Fe2 116.51(14) . . ?
N9 C47 C46 127.25(15) . . ?
N9 C47 H47 116.4 . . ?
C46 C47 H47 116.4 . . ?
N1 C7 C6 125.19(15) . . ?
N1 C7 H7 117.4 . . ?
C6 C7 H7 117.4 . . ?
O4 C41 C42 119.70(16) . . ?
O4 C41 C46 122.10(15) . . ?
C42 C41 C46 118.20(17) . . ?
C9 C8 C16 119.28(15) . . ?
C9 C8 N1 127.53(15) . . ?
C16 C8 N1 113.19(14) . . ?
C21 C22 C17 119.58(18) . . ?
C21 C22 C23 116.68(18) . . ?
C17 C22 C23 123.75(16) . . ?
C45 C46 C41 119.32(17) . . ?
C45 C46 C47 118.12(16) . . ?
C41 C46 C47 122.56(16) . . ?
N4 C24 N5 119.21(14) . . ?
N4 C24 S1 123.65(12) . . ?
N5 C24 S1 117.09(13) . . ?
O2 C17 C22 124.89(16) . . ?
O2 C17 C18 117.92(18) . . ?
C22 C17 C18 117.19(19) . . ?
O1 C1 C2 117.11(16) . . ?
O1 C1 C6 125.27(15) . . ?
C2 C1 C6 117.62(16) . . ?
O3 C25 C26 119.1(2) . . ?
O3 C25 C30 123.0(2) . . ?
C26 C25 C30 117.9(2) . . ?
C13 C12 C16 117.03(18) . . ?
C13 C12 C11 124.95(18) . . ?
C16 C12 C11 117.99(17) . . ?
N8 C48 N10 117.00(16) . . ?
N8 C48 S2 125.77(13) . . ?
N10 C48 S2 117.21(14) . . ?
C5 C6 C1 119.40(16) . . ?
C5 C6 C7 117.10(16) . . ?
C1 C6 C7 123.48(15) . . ?
C8 C9 C10 119.59(17) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C33 C32 C40 118.5(2) . . ?
C33 C32 N6 126.7(2) . . ?
C40 C32 N6 114.82(16) . . ?
C43 C42 C41 120.96(19) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C4 C5 C6 119.86(19) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C3 C2 C1 121.78(19) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
N2 C15 C14 121.95(19) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C11 C10 C9 121.65(18) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N7 C40 C32 117.65(18) . . ?
N7 C40 C36 121.1(2) . . ?
C32 C40 C36 121.2(2) . . ?
C44 C45 C46 121.5(2) . . ?
C44 C45 H45 119.3 . . ?
C46 C45 H45 119.3 . . ?
C20 C21 C22 121.7(2) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C10 C11 C12 120.44(17) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
N6 C31 C30 126.53(19) . . ?
N6 C31 H31 116.7 . . ?
C30 C31 H31 116.7 . . ?
C42 C43 C44 121.07(19) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C19 C18 C17 121.3(2) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C2 C3 C4 118.75(19) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C25 C30 C29 119.5(3) . . ?
C25 C30 C31 123.90(19) . . ?
C29 C30 C31 116.6(3) . . ?
C35 C36 C37 124.7(3) . . ?
C35 C36 C40 118.1(3) . . ?
C37 C36 C40 117.2(3) . . ?
C21 C20 C19 119.0(2) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C32 C33 C34 119.3(3) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C45 C44 C43 119.0(2) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C14 C13 C12 119.65(19) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C27 C26 C25 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C5 C4 F1 119.5(2) . . ?
C5 C4 C3 122.56(19) . . ?
F1 C4 C3 117.91(19) . . ?
C13 C14 C15 119.96(19) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C18 C19 C20 121.2(2) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
N7 C39 C38 122.6(3) . . ?
N7 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C38 C37 C36 120.7(3) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
N12 C51 C52 174.0(5) . . ?
C29 C28 C27 122.6(3) . . ?
C29 C28 F2 119.5(4) . . ?
C27 C28 F2 117.9(4) . . ?
C34 C35 C36 120.3(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C28 C29 C30 119.8(3) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C35 C34 C33 122.5(3) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C37 C38 C39 119.2(3) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
N13 C55 C56 176.7(5) . . ?
C28 C27 C26 119.9(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C61 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C61 N15 N15 162.4(9) . 2_665 ?
N15 C61 C60 178.8(13) . . ?
N16 C63 C62 178.3(13) . . ?
C63 C62 H62A 109.5 . . ?
C63 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C63 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N11 C50 C49 175.2(13) . . ?
N11' C50' C49' 174.0(10) . . ?
C50' C49' H49D 109.5 . . ?
C50' C49' H49E 109.5 . . ?
H49D C49' H49E 109.5 . . ?
C50' C49' H49F 109.5 . . ?
H49D C49' H49F 109.5 . . ?
H49E C49' H49F 109.5 . . ?
N17 C65 C64 165(3) . . ?
N18 C67 C66 167(3) . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C67 C66 H66A 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C67 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_refine_diff_density_max         0.531
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.050

_shelxl_version_number           2013-2

