# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_md337b
_database_code_depnum_ccdc_archive 'CCDC 1512924'
_audit_update_record             
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C66 H48 Fe N18), 2(F6 P), Cl, (H2 O), (H O)'
_chemical_formula_sum            'C132 H99 Cl F12 Fe2 N36 O2 P2'
_chemical_formula_weight         2658.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1183 0.1134
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   13.4555(8)
_cell_length_b                   13.4555(8)
_cell_length_c                   37.438(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5870.1(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7373
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      18.98

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             2732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.487
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_process_details   SADABS-2014/4

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23158
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_av_R_equivalents  0.1643
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.245
_diffrn_reflns_theta_max         19.095
_diffrn_reflns_theta_full        19.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1230
_reflns_number_gt                1004
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Due to the
 poor diffraction, resolution and data over parameters ratio,
 all C and N atoms were refined with displacement parameters
 restraints. Hydrogens were placed geometrically on their
 carrier atom and refined with a riding model, except that
 on O1, that was found in a difference Fourier map and refined
 with its thermal parameter 1.5 times that of O1 and a soft 
 distance restraint. Its occupancy was fixed at 1/2, as for
 charge balance it should be either an hydroxide ion or
 a water molecule. Indeed, by symmetry the H1 site forms 
 three hydrogen bonds with either of three N acceptor from
 three neighboring pyridines (N6). The formula thus has
 one hydroxide ion and one water molecule, sharing the same
 position.
;

_vrf_REFNR01_md337b              
;
PROBLEM:  Ratio of reflections to parameters is < 6 for a
            centrosymmetric structure
RESPONSE: Crystals were extremely thin plates, stacked
on each other. Diffraction was observed only up to ca. 1.2
angstrom resolution, systematically on several crystals,
as well as stacks of crystals tested. The present data
were cut at 1.19 angstrom as then I/sigma(I) was below 2
and virtually no significant diffraction was observed.
This poor diffraction, intrinsic to the quality of crystals
available, results in poor values of thetamax,
thetafull, as well as poor data over parameters ratio.

;

_vrf_THETM01_md337b              
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals were extremely thin plates, stacked
on each other. Diffraction was observed only up to ca. 1.2
angstrom resolution, systematically on several crystals,
as well as stacks of crystals tested. The present data
were cut at 1.19 angstrom as then I/sigma(I) was below 2
and virtually no significant diffraction was observed.
This poor diffraction, intrinsic to the quality of crystals
available, results in poor values of thetamax,
thetafull, as well as poor data over parameters ratio.
;

_vrf_PLAT027_md337b              
;
PROBLEM:  _diffrn_reflns_theta_full (too) Low ............      19.00 Degree
RESPONSE: Crystals were extremely thin plates, stacked
on each other. Diffraction was observed only up to ca. 1.2
angstrom resolution, systematically on several crystals,
as well as stacks of crystals tested. The present data
were cut at 1.19 angstrom as then I/sigma(I) was below 2
and virtually no significant diffraction was observed.
This poor diffraction, intrinsic to the quality of crystals
available, results in poor values of thetamax,
thetafull, as well as poor data over parameters ratio.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+341.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1230
_refine_ls_number_parameters     285
_refine_ls_number_restraints     269
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.1402
_refine_ls_wR_factor_ref         0.3137
_refine_ls_wR_factor_gt          0.3014
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      0.979
_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 1.0000 0.0000 0.09674(16) 0.050(2) Uani 1 3 d S T P . .
N1 N 0.8667(16) -0.1130(15) 0.0691(5) 0.039(4) Uani 1 1 d . U . . .
N2 N 0.8786(16) 0.0021(16) 0.1235(5) 0.040(4) Uani 1 1 d . U . . .
N3 N 0.8668(15) 0.0519(14) 0.1524(5) 0.036(4) Uani 1 1 d . U . . .
H3B H 0.9240 0.0976 0.1665 0.043 Uiso 1 1 calc R U . . .
N4 N 0.9048(15) 0.1668(15) 0.2864(5) 0.044(4) Uani 1 1 d . U . . .
H4A H 0.9157 0.1190 0.2733 0.052 Uiso 1 1 calc R U . . .
N5 N 0.9626(16) 0.2165(16) 0.3166(5) 0.047(4) Uani 1 1 d . U . . .
N6 N 0.8991(18) 0.3883(18) 0.3768(5) 0.060(4) Uani 1 1 d . U . . .
C1 C 0.867(2) -0.179(2) 0.0418(6) 0.041(4) Uani 1 1 d . U . . .
H1A H 0.9384 -0.1712 0.0344 0.049 Uiso 1 1 calc R U . . .
C2 C 0.770(2) -0.257(2) 0.0244(6) 0.046(5) Uani 1 1 d . U . . .
H2A H 0.7736 -0.3044 0.0062 0.055 Uiso 1 1 calc R U . . .
C3 C 0.669(2) -0.267(2) 0.0332(6) 0.046(5) Uani 1 1 d . U . . .
H3A H 0.6020 -0.3171 0.0201 0.055 Uiso 1 1 calc R U . . .
C4 C 0.664(2) -0.2035(19) 0.0619(6) 0.042(5) Uani 1 1 d . U . . .
H4 H 0.5938 -0.2098 0.0694 0.051 Uiso 1 1 calc R U . . .
C5 C 0.7625(19) -0.134(2) 0.0781(6) 0.038(4) Uani 1 1 d . U . . .
C6 C 0.7697(19) -0.0666(19) 0.1106(6) 0.036(4) Uani 1 1 d . U . . .
C7 C 0.695(2) -0.0477(19) 0.1308(6) 0.039(4) Uani 1 1 d . U . . .
H7A H 0.6152 -0.0789 0.1268 0.047 Uiso 1 1 calc R U . . .
C8 C 0.758(2) 0.0247(19) 0.1578(6) 0.039(4) Uani 1 1 d . U . . .
C9 C 0.721(2) 0.072(2) 0.1874(6) 0.043(4) Uani 1 1 d . U . . .
C10 C 0.624(2) 0.080(2) 0.1849(6) 0.047(4) Uani 1 1 d . U . . .
H10A H 0.5761 0.0504 0.1644 0.056 Uiso 1 1 calc R U . . .
C11 C 0.594(2) 0.1288(19) 0.2119(6) 0.047(4) Uani 1 1 d . U . . .
H11A H 0.5294 0.1392 0.2086 0.056 Uiso 1 1 calc R U . . .
C12 C 0.654(2) 0.164(2) 0.2435(7) 0.049(4) Uani 1 1 d . U . . .
H12A H 0.6280 0.1905 0.2629 0.058 Uiso 1 1 calc R U . . .
C13 C 0.756(2) 0.1577(19) 0.2462(6) 0.045(4) Uani 1 1 d . U . . .
C14 C 0.788(2) 0.1075(19) 0.2185(6) 0.046(4) Uani 1 1 d . U . . .
H14A H 0.8536 0.0983 0.2209 0.055 Uiso 1 1 calc R U . . .
C15 C 0.828(2) 0.200(2) 0.2792(6) 0.045(4) Uani 1 1 d . U . . .
C16 C 0.830(2) 0.2695(19) 0.3048(6) 0.046(4) Uani 1 1 d . U . . .
H16A H 0.7806 0.3008 0.3077 0.055 Uiso 1 1 calc R U . . .
C17 C 0.925(2) 0.286(2) 0.3273(6) 0.048(4) Uani 1 1 d . U . . .
C18 C 0.968(2) 0.357(2) 0.3593(7) 0.053(4) Uani 1 1 d . U . . .
C19 C 1.082(2) 0.399(2) 0.3699(7) 0.059(5) Uani 1 1 d . U . . .
H19A H 1.1311 0.3799 0.3569 0.071 Uiso 1 1 calc R U . . .
C20 C 1.120(3) 0.465(2) 0.3985(7) 0.068(5) Uani 1 1 d . U . . .
H20A H 1.1956 0.4898 0.4065 0.082 Uiso 1 1 calc R U . . .
C21 C 1.055(3) 0.500(2) 0.4169(7) 0.074(6) Uani 1 1 d . U . . .
H21A H 1.0865 0.5515 0.4363 0.089 Uiso 1 1 calc R U . . .
C22 C 0.942(2) 0.456(2) 0.4061(7) 0.067(5) Uani 1 1 d . U . . .
H22A H 0.8935 0.4732 0.4197 0.080 Uiso 1 1 calc R U . . .
Cl1 Cl 1.0000 0.0000 0.2500 0.088(6) Uani 1 6 d S T P . .
P1 P 0.6667 0.3333 0.5001(4) 0.072(5) Uani 1 3 d S T P . .
F1 F 0.7453(17) 0.3089(18) 0.5229(5) 0.133(8) Uani 1 1 d . . . . .
F2 F 0.770(2) 0.4141(18) 0.4773(5) 0.165(10) Uani 1 1 d . . . . .
O1 O 0.6667 0.3333 0.3554(8) 0.068(9) Uani 1 3 d DS T P . .
H1 H 0.74(2) 0.37(5) 0.369(10) 0.101 Uiso 0.5 1 d D U P . .


_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 N2 1.928(19) 3_765 ?
Fe1 N2 1.928(19) 2_645 ?
Fe1 N2 1.928(19) . ?
Fe1 N1 1.967(18) 2_645 ?
Fe1 N1 1.968(18) 3_765 ?
Fe1 N1 1.968(18) . ?
N1 C5 1.33(3) . ?
N1 C1 1.36(3) . ?
N2 N3 1.32(2) . ?
N2 C6 1.37(3) . ?
N3 C8 1.33(3) . ?
N3 H3B 0.8800 . ?
N4 C15 1.34(3) . ?
N4 N5 1.34(2) . ?
N4 H4A 0.8800 . ?
N5 C17 1.32(3) . ?
N6 C22 1.35(3) . ?
N6 C18 1.37(3) . ?
C1 C2 1.37(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.33(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.40(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.33(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.49(3) . ?
C6 C7 1.38(3) . ?
C7 C8 1.37(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.49(3) . ?
C9 C10 1.37(3) . ?
C9 C14 1.40(3) . ?
C10 C11 1.37(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.38(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.42(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.42(3) . ?
C13 C15 1.50(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.33(3) . ?
C16 C17 1.46(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.46(3) . ?
C18 C19 1.40(3) . ?
C19 C20 1.32(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.36(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.39(3) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
P1 F1 1.517(18) . ?
P1 F1 1.517(18) 3_665 ?
P1 F1 1.517(18) 2_655 ?
P1 F2 1.526(19) 3_665 ?
P1 F2 1.53(2) . ?
P1 F2 1.526(19) 2_655 ?
O1 H1 0.95(2) . ?

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
N2 Fe1 N2 95.5(7) 3_765 2_645 ?
N2 Fe1 N2 95.5(7) 3_765 . ?
N2 Fe1 N2 95.5(7) 2_645 . ?
N2 Fe1 N1 89.5(7) 3_765 2_645 ?
N2 Fe1 N1 80.4(8) 2_645 2_645 ?
N2 Fe1 N1 173.8(7) . 2_645 ?
N2 Fe1 N1 80.4(8) 3_765 3_765 ?
N2 Fe1 N1 173.8(7) 2_645 3_765 ?
N2 Fe1 N1 89.5(7) . 3_765 ?
N1 Fe1 N1 94.9(7) 2_645 3_765 ?
N2 Fe1 N1 173.8(7) 3_765 . ?
N2 Fe1 N1 89.5(7) 2_645 . ?
N2 Fe1 N1 80.4(8) . . ?
N1 Fe1 N1 94.9(7) 2_645 . ?
N1 Fe1 N1 94.9(7) 3_765 . ?
C5 N1 C1 113.7(19) . . ?
C5 N1 Fe1 119.2(15) . . ?
C1 N1 Fe1 126.9(16) . . ?
N3 N2 C6 105.8(18) . . ?
N3 N2 Fe1 138.5(15) . . ?
C6 N2 Fe1 115.7(15) . . ?
N2 N3 C8 112.2(19) . . ?
N2 N3 H3B 123.9 . . ?
C8 N3 H3B 123.9 . . ?
C15 N4 N5 111(2) . . ?
C15 N4 H4A 124.6 . . ?
N5 N4 H4A 124.6 . . ?
C17 N5 N4 106(2) . . ?
C22 N6 C18 118(2) . . ?
N1 C1 C2 123(2) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 120(2) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119(2) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 117(2) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
N1 C5 C4 127(2) . . ?
N1 C5 C6 109.7(19) . . ?
C4 C5 C6 123(2) . . ?
N2 C6 C7 108(2) . . ?
N2 C6 C5 115(2) . . ?
C7 C6 C5 137(2) . . ?
C8 C7 C6 107(2) . . ?
C8 C7 H7A 126.7 . . ?
C6 C7 H7A 126.7 . . ?
N3 C8 C7 107(2) . . ?
N3 C8 C9 124(2) . . ?
C7 C8 C9 129(2) . . ?
C10 C9 C14 121(2) . . ?
C10 C9 C8 122(2) . . ?
C14 C9 C8 118(2) . . ?
C9 C10 C11 121(2) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C10 C11 C12 122(2) . . ?
C10 C11 H11A 119.0 . . ?
C12 C11 H11A 119.0 . . ?
C11 C12 C13 118(2) . . ?
C11 C12 H12A 121.2 . . ?
C13 C12 H12A 121.2 . . ?
C12 C13 C14 121(2) . . ?
C12 C13 C15 120(2) . . ?
C14 C13 C15 119(2) . . ?
C9 C14 C13 118(2) . . ?
C9 C14 H14A 121.2 . . ?
C13 C14 H14A 121.2 . . ?
C16 C15 N4 110(2) . . ?
C16 C15 C13 130(2) . . ?
N4 C15 C13 120(2) . . ?
C15 C16 C17 103(2) . . ?
C15 C16 H16A 128.5 . . ?
C17 C16 H16A 128.5 . . ?
N5 C17 C16 110(2) . . ?
N5 C17 C18 123(2) . . ?
C16 C17 C18 127(2) . . ?
N6 C18 C19 121(2) . . ?
N6 C18 C17 119(2) . . ?
C19 C18 C17 120(2) . . ?
C20 C19 C18 118(3) . . ?
C20 C19 H19A 120.8 . . ?
C18 C19 H19A 120.8 . . ?
C19 C20 C21 123(3) . . ?
C19 C20 H20A 118.4 . . ?
C21 C20 H20A 118.4 . . ?
C20 C21 C22 117(3) . . ?
C20 C21 H21A 121.4 . . ?
C22 C21 H21A 121.4 . . ?
N6 C22 C21 122(3) . . ?
N6 C22 H22A 118.9 . . ?
C21 C22 H22A 118.9 . . ?
F1 P1 F1 91.6(12) . 3_665 ?
F1 P1 F1 91.6(12) . 2_655 ?
F1 P1 F1 91.6(12) 3_665 2_655 ?
F1 P1 F2 87.6(11) . 3_665 ?
F1 P1 F2 89.2(12) 3_665 3_665 ?
F1 P1 F2 178.9(12) 2_655 3_665 ?
F1 P1 F2 89.2(12) . . ?
F1 P1 F2 178.9(12) 3_665 . ?
F1 P1 F2 87.6(11) 2_655 . ?
F2 P1 F2 91.6(14) 3_665 . ?
F1 P1 F2 178.9(12) . 2_655 ?
F1 P1 F2 87.6(11) 3_665 2_655 ?
F1 P1 F2 89.2(12) 2_655 2_655 ?
F2 P1 F2 91.6(14) 3_665 2_655 ?
F2 P1 F2 91.6(14) . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N6 0.95(2) 2.1(3) 2.94(2) 148(51) .

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.099

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_md538_twin5
_database_code_depnum_ccdc_archive 'CCDC 1512925'
_audit_update_record             
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C66 H48 Fe N18), 3(Cl4 Fe), 4(C7 H8), 2(C3 H6 O), Cl'
_chemical_formula_sum            'C166 H140 Cl13 Fe5 N36 O2'
_chemical_formula_weight         3411.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_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                   13.4928(6)
_cell_length_b                   21.3643(10)
_cell_length_c                   28.7728(13)
_cell_angle_alpha                73.320(3)
_cell_angle_beta                 80.537(3)
_cell_angle_gamma                85.230(3)
_cell_volume                     7831.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      33.01

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             3510
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.933
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'TWINABS - Bruker AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34424
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.154
_diffrn_reflns_theta_max         33.119
_diffrn_reflns_theta_full        32.550
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measured_fraction_theta_full 0.860
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_Laue_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_point_group_measured_fraction_full 0.860
_reflns_number_total             34424
_reflns_number_gt                23396
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Refined as a 2-component twin. Several crystals were tested
 and all showed signs of twinning. The twinning of the present
 data was treated with CELL_NOW after inspection of the data
 in RLATT. The twin law was found to be a rotation by 180
 degrees about (real) axis 1.000 0.093 0.071. Cell refinement
 and integration were then performed by SAINT as a 2-component
 twin, keeping the cell of both components identical. TWINABS
 was used for absorption corrections and produced HKLF4 and
 HKLF5 data, respectively for initial structure solution and 
 refinement and final refinement. All non-hydrogens were
 refined anisotropically, except the minor components of species
 disordered over two positions. Those include one FeCl4 anion 
 (main component Fe4 Cl7 Cl8 Cl, minor component Fe4B Cl7B Cl8B
 Cl9B, both sharing Cl6), one lattice toluene molecule (main 
 component C15S-C21S, minor component C35S-C41S), and
 one of the Cl atom of another FeCl4 anion (Cl12 and Cl13).
 All these were refined with distance and displacement
 parameters restraints, and the relative occupancies refined
 to respectively 0.873:, 0.659:, 0.785:. Another lattice
 toluene and acetone molecules were also refined with
 displacement parameters restraints. The disordered lattice
 toluene molecules were refined to be similar to another
 toluene molecule with no disorder using the SAME order.
 Hydrogens on the pyrazole nitrogens were all found in
 difference Fourier maps. Those and the rest of hydrogens
 were placed geometrically on their carrier atom and refined
 with a riding model. Hydrogens on the minor component of
 the disordered lattice toluene molecule are omitted in the
 structural model due to ill-defined positions giving rise 
 to short H H contacts. The final twin proportion as
 given by BASF parameter is 0.294/0.706., Twin
;

_vrf_PLAT029_md538_twin5         
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low
RESPONSE: Crystals were found to be twinned, resulting
in an important fraction of reflections at higher 
resolutions not detectable (likely corresponding to the
minor component), and thus a poor thetafull.  
;

_vrf_PLAT221_md538_twin5         
;
PROBLEM:  Large Solv./Anion Cl     Ueq(max)/Ueq(min) Range       10.0 Ratio
RESPONSE: Two of the FeCl4 anions show some disorder, which
refined splitting the relevant disordered atoms and using
distance and displacement parameters restraints (SIMU/DELU).
The remaining high Umax/Umin ratio is likely due to some
of this disorder still showing up.   
;

_vrf_PLAT911_md538_twin5         
;
PROBLEM:  Missing # FCF Refl Between THmin & STh/L=  0.600       4450
RESPONSE: Crystals were found to be twinned, resulting
in an important fraction of reflections at higher 
resolutions not detectable (likely corresponding to the
minor component).  
;

_vrf_PLAT910_md538_twin5         
;
PROBLEM:  Missing # of FCF Reflection(s) Below Th(Min) ...         13
RESPONSE: The data collection strategy on beamline
11.3.1 typically consists in a fast phi scan and further
omega scans. The fast phi scan then serves to define
strong reflections overloaded in the further scans. This
is typically done through SADABS, but is not possible
when using TWINABS, so that these missing strong
reflections are likely those overloaded.
;

_vrf_PLAT041_md538_twin5         
;
PROBLEM:  Calc. and Reported SumFormula    Strings  Differ 
RESPONSE: Hydrogens on the minor component of the
disordered lattice toluene molecule (C35-C41) are omitted
in the structural model, but included in the formula,
giving rise to this discrepancy between the reported formula
and that derived from atom sites.
;

_vrf_PLAT913_md538_twin5         
;
PROBLEM:  Missing # of Very Strong Reflections in FCF ....         51
RESPONSE: The data collection strategy on beamline
11.3.1 typically consists in a fast phi scan and further
omega scans. The fast phi scan then serves to define
strong reflections overloaded in the further scans. This
is typically done through SADABS, but is not possible
when using TWINABS, so that these missing strong
reflections are likely those overloaded.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²+33.8581P] 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         34424
_refine_ls_number_parameters     2057
_refine_ls_number_restraints     434
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0805
_refine_ls_wR_factor_ref         0.2130
_refine_ls_wR_factor_gt          0.1812
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.056
_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 0.62811(5) -0.02600(3) 0.73010(3) 0.01825(15) Uani 1 1 d . . . . .
N1 N 0.5056(3) -0.0793(2) 0.74761(16) 0.0207(9) Uani 1 1 d . . . . .
N2 N 0.5655(3) -0.0029(2) 0.78974(15) 0.0188(9) Uani 1 1 d . . . . .
N3 N 0.5838(3) 0.0377(2) 0.81586(15) 0.0178(8) Uani 1 1 d . . . . .
H3 H 0.6336 0.0647 0.8075 0.021 Uiso 1 1 calc R U . . .
N4 N 0.6513(3) 0.2553(2) 0.85373(15) 0.0216(9) Uani 1 1 d . . . . .
H4 H 0.6351 0.2451 0.8285 0.026 Uiso 1 1 calc R U . . .
N5 N 0.7051(3) 0.3076(2) 0.84942(16) 0.0222(9) Uani 1 1 d . . . . .
N6 N 0.8244(4) 0.3952(2) 0.86426(19) 0.0307(11) Uani 1 1 d . . . . .
N7 N 0.7086(3) -0.1007(2) 0.76898(15) 0.0198(9) Uani 1 1 d . . . . .
N8 N 0.7547(3) 0.0179(2) 0.72266(15) 0.0176(8) Uani 1 1 d . . . . .
N9 N 0.7921(3) 0.0774(2) 0.70219(16) 0.0205(9) Uani 1 1 d . . . . .
H9A H 0.7578 0.1118 0.6868 0.025 Uiso 1 1 calc R U . . .
N10 N 0.8185(3) 0.3328(2) 0.66693(17) 0.0230(9) Uani 1 1 d . . . . .
H10H H 0.7802 0.3035 0.6887 0.028 Uiso 1 1 calc R U . . .
N11 N 0.7872(3) 0.3951(2) 0.64933(17) 0.0240(9) Uani 1 1 d . . . . .
N12 N 0.7701(4) 0.5229(3) 0.5930(2) 0.0372(12) Uani 1 1 d . . . . .
N13 N 0.6700(3) -0.0518(2) 0.66766(16) 0.0223(9) Uani 1 1 d . . . . .
N14 N 0.5639(3) 0.04673(19) 0.68470(15) 0.0170(8) Uani 1 1 d . . . . .
N15 N 0.5105(3) 0.10227(19) 0.68567(16) 0.0193(9) Uani 1 1 d . . . . .
H15A H 0.4960 0.1170 0.7117 0.023 Uiso 1 1 calc R U . . .
N16 N 0.4137(3) 0.3345(2) 0.71514(16) 0.0210(9) Uani 1 1 d . . . . .
H16 H 0.4676 0.3082 0.7173 0.025 Uiso 1 1 calc R U . . .
N17 N 0.3875(3) 0.3769(2) 0.74271(16) 0.0217(9) Uani 1 1 d . . . . .
N18 N 0.1714(4) 0.4889(3) 0.7300(2) 0.0357(12) Uani 1 1 d . . . . .
C1 C 0.4776(4) -0.1188(2) 0.7234(2) 0.0232(11) Uani 1 1 d . . . . .
H1A H 0.5128 -0.1174 0.6917 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3998(4) -0.1611(3) 0.7428(2) 0.0238(11) Uani 1 1 d . . . . .
H2A H 0.3832 -0.1888 0.7248 0.029 Uiso 1 1 calc R U . . .
C3 C 0.3463(4) -0.1632(3) 0.7882(2) 0.0260(11) Uani 1 1 d . . . . .
H3A H 0.2935 -0.1927 0.8024 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3718(4) -0.1210(3) 0.8127(2) 0.0243(11) Uani 1 1 d . . . . .
H4A H 0.3355 -0.1204 0.8438 0.029 Uiso 1 1 calc R U . . .
C5 C 0.4495(4) -0.0801(2) 0.79159(18) 0.0184(10) Uani 1 1 d . . . . .
C6 C 0.4844(4) -0.0348(2) 0.81422(18) 0.0168(10) Uani 1 1 d . . . . .
C7 C 0.4485(4) -0.0150(2) 0.85647(19) 0.0207(10) Uani 1 1 d . . . . .
H7A H 0.3912 -0.0299 0.8800 0.025 Uiso 1 1 calc R U . . .
C8 C 0.5141(4) 0.0306(2) 0.85666(18) 0.0190(10) Uani 1 1 d . . . . .
C9 C 0.5148(4) 0.0688(2) 0.89220(18) 0.0199(10) Uani 1 1 d . . . . .
C10 C 0.4582(4) 0.0474(3) 0.93889(19) 0.0238(11) Uani 1 1 d . . . . .
H10A H 0.4209 0.0089 0.9477 0.029 Uiso 1 1 calc R U . . .
C11 C 0.4579(5) 0.0837(3) 0.9719(2) 0.0294(12) Uani 1 1 d . . . . .
H11A H 0.4188 0.0700 1.0034 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5129(4) 0.1393(3) 0.96029(19) 0.0245(11) Uani 1 1 d . . . . .
H12A H 0.5132 0.1624 0.9840 0.029 Uiso 1 1 calc R U . . .
C13 C 0.5677(4) 0.1611(2) 0.91390(19) 0.0208(10) Uani 1 1 d . . . . .
C14 C 0.5684(4) 0.1248(2) 0.88036(17) 0.0179(10) Uani 1 1 d . . . . .
H14A H 0.6068 0.1390 0.8487 0.022 Uiso 1 1 calc R U . . .
C15 C 0.6247(4) 0.2199(2) 0.90113(19) 0.0216(10) Uani 1 1 d . . . . .
C16 C 0.6664(4) 0.2511(3) 0.9287(2) 0.0252(11) Uani 1 1 d . . . . .
H16A H 0.6625 0.2386 0.9634 0.030 Uiso 1 1 calc R U . . .
C17 C 0.7157(4) 0.3049(3) 0.8953(2) 0.0237(11) Uani 1 1 d . . . . .
C18 C 0.7743(4) 0.3542(3) 0.9041(2) 0.0259(12) Uani 1 1 d . . . . .
C19 C 0.7785(5) 0.3574(3) 0.9508(2) 0.0378(15) Uani 1 1 d . . . . .
H19A H 0.7408 0.3287 0.9783 0.045 Uiso 1 1 calc R U . . .
C20 C 0.8390(6) 0.4035(3) 0.9573(3) 0.0467(18) Uani 1 1 d . . . . .
H20A H 0.8445 0.4061 0.9892 0.056 Uiso 1 1 calc R U . . .
C21 C 0.8892(6) 0.4441(3) 0.9169(3) 0.0484(19) Uani 1 1 d . . . . .
H21A H 0.9297 0.4765 0.9202 0.058 Uiso 1 1 calc R U . . .
C22 C 0.8819(5) 0.4390(3) 0.8712(3) 0.0403(16) Uani 1 1 d . . . . .
H22A H 0.9191 0.4676 0.8434 0.048 Uiso 1 1 calc R U . . .
C23 C 0.6797(4) -0.1610(3) 0.7917(2) 0.0279(12) Uani 1 1 d . . . . .
H23A H 0.6121 -0.1712 0.7925 0.033 Uiso 1 1 calc R U . . .
C24 C 0.7443(4) -0.2100(3) 0.8144(2) 0.0299(13) Uani 1 1 d . . . . .
H24A H 0.7212 -0.2528 0.8301 0.036 Uiso 1 1 calc R U . . .
C25 C 0.8423(5) -0.1958(3) 0.8140(2) 0.0349(14) Uani 1 1 d . . . . .
H25A H 0.8880 -0.2287 0.8292 0.042 Uiso 1 1 calc R U . . .
C26 C 0.8725(4) -0.1329(3) 0.7911(2) 0.0303(13) Uani 1 1 d . . . . .
H26A H 0.9392 -0.1214 0.7906 0.036 Uiso 1 1 calc R U . . .
C27 C 0.8047(4) -0.0873(2) 0.76899(19) 0.0223(11) Uani 1 1 d . . . . .
C28 C 0.8294(4) -0.0197(3) 0.74323(19) 0.0219(11) Uani 1 1 d . . . . .
C29 C 0.9151(4) 0.0161(3) 0.7345(2) 0.0224(11) Uani 1 1 d . . . . .
H29A H 0.9785 0.0010 0.7447 0.027 Uiso 1 1 calc R U . . .
C30 C 0.8888(4) 0.0780(2) 0.7082(2) 0.0203(10) Uani 1 1 d . . . . .
C31 C 0.9488(4) 0.1361(3) 0.6907(2) 0.0240(11) Uani 1 1 d . . . . .
C32 C 1.0544(4) 0.1302(3) 0.6865(2) 0.0314(13) Uani 1 1 d . . . . .
H32A H 1.0865 0.0880 0.6943 0.038 Uiso 1 1 calc R U . . .
C33 C 1.1118(4) 0.1849(3) 0.6713(2) 0.0350(14) Uani 1 1 d . . . . .
H33A H 1.1829 0.1801 0.6694 0.042 Uiso 1 1 calc R U . . .
C34 C 1.0665(4) 0.2466(3) 0.6587(2) 0.0309(13) Uani 1 1 d . . . . .
H34A H 1.1066 0.2840 0.6476 0.037 Uiso 1 1 calc R U . . .
C35 C 0.9624(4) 0.2541(3) 0.6623(2) 0.0240(11) Uani 1 1 d . . . . .
C36 C 0.9045(4) 0.1992(3) 0.6779(2) 0.0233(11) Uani 1 1 d . . . . .
H36A H 0.8335 0.2045 0.6800 0.028 Uiso 1 1 calc R U . . .
C37 C 0.9141(4) 0.3188(3) 0.6485(2) 0.0230(11) Uani 1 1 d . . . . .
C38 C 0.9463(4) 0.3773(3) 0.6159(2) 0.0266(12) Uani 1 1 d . . . . .
H38A H 1.0106 0.3851 0.5966 0.032 Uiso 1 1 calc R U . . .
C39 C 0.8660(4) 0.4228(3) 0.6171(2) 0.0251(11) Uani 1 1 d . . . . .
C40 C 0.8592(4) 0.4914(3) 0.5882(2) 0.0257(11) Uani 1 1 d . . . . .
C41 C 0.9427(4) 0.5201(3) 0.5571(2) 0.0300(13) Uani 1 1 d . . . . .
H41A H 1.0050 0.4962 0.5547 0.036 Uiso 1 1 calc R U . . .
C42 C 0.9331(5) 0.5842(3) 0.5297(3) 0.0415(16) Uani 1 1 d . . . . .
H42A H 0.9892 0.6050 0.5080 0.050 Uiso 1 1 calc R U . . .
C43 C 0.8431(6) 0.6178(3) 0.5338(3) 0.0424(16) Uani 1 1 d . . . . .
H43A H 0.8351 0.6620 0.5150 0.051 Uiso 1 1 calc R U . . .
C44 C 0.7633(5) 0.5852(3) 0.5663(3) 0.0424(16) Uani 1 1 d . . . . .
H44A H 0.7007 0.6085 0.5698 0.051 Uiso 1 1 calc R U . . .
C45 C 0.7277(4) -0.1044(3) 0.6621(2) 0.0249(11) Uani 1 1 d . . . . .
H45A H 0.7575 -0.1314 0.6891 0.030 Uiso 1 1 calc R U . . .
C46 C 0.7447(4) -0.1198(3) 0.6176(2) 0.0306(13) Uani 1 1 d . . . . .
H46A H 0.7866 -0.1568 0.6143 0.037 Uiso 1 1 calc R U . . .
C47 C 0.7013(5) -0.0820(3) 0.5784(2) 0.0317(13) Uani 1 1 d . . . . .
H47A H 0.7112 -0.0932 0.5483 0.038 Uiso 1 1 calc R U . . .
C48 C 0.6428(4) -0.0275(3) 0.5836(2) 0.0290(12) Uani 1 1 d . . . . .
H48A H 0.6117 -0.0004 0.5572 0.035 Uiso 1 1 calc R U . . .
C49 C 0.6307(4) -0.0133(2) 0.62835(19) 0.0212(10) Uani 1 1 d . . . . .
C50 C 0.5720(4) 0.0429(2) 0.63862(18) 0.0178(10) Uani 1 1 d . . . . .
C51 C 0.5220(4) 0.0957(2) 0.61004(19) 0.0203(10) Uani 1 1 d . . . . .
H51A H 0.5166 0.1043 0.5763 0.024 Uiso 1 1 calc R U . . .
C52 C 0.4817(4) 0.1331(2) 0.64122(18) 0.0184(10) Uani 1 1 d . . . . .
C53 C 0.4219(4) 0.1940(2) 0.63139(19) 0.0205(10) Uani 1 1 d . . . . .
C54 C 0.3725(4) 0.2128(3) 0.5902(2) 0.0238(11) Uani 1 1 d . . . . .
H54A H 0.3768 0.1853 0.5692 0.029 Uiso 1 1 calc R U . . .
C55 C 0.3175(4) 0.2714(3) 0.5800(2) 0.0248(11) Uani 1 1 d . . . . .
H55A H 0.2858 0.2842 0.5514 0.030 Uiso 1 1 calc R U . . .
C56 C 0.3077(4) 0.3115(2) 0.6105(2) 0.0218(11) Uani 1 1 d . . . . .
H56A H 0.2680 0.3510 0.6034 0.026 Uiso 1 1 calc R U . . .
C57 C 0.3561(4) 0.2941(2) 0.65210(18) 0.0189(10) Uani 1 1 d . . . . .
C58 C 0.4126(4) 0.2355(2) 0.66201(19) 0.0200(10) Uani 1 1 d . . . . .
H58A H 0.4458 0.2233 0.6902 0.024 Uiso 1 1 calc R U . . .
C59 C 0.3473(4) 0.3374(2) 0.68400(19) 0.0204(10) Uani 1 1 d . . . . .
C60 C 0.2743(4) 0.3841(2) 0.69131(19) 0.0208(10) Uani 1 1 d . . . . .
H60A H 0.2175 0.3980 0.6748 0.025 Uiso 1 1 calc R U . . .
C61 C 0.3021(4) 0.4070(2) 0.7287(2) 0.0217(11) Uani 1 1 d . . . . .
C62 C 0.2471(4) 0.4553(3) 0.7520(2) 0.0244(11) Uani 1 1 d . . . . .
C63 C 0.2703(5) 0.4640(4) 0.7944(3) 0.0422(16) Uani 1 1 d . . . . .
H63A H 0.3242 0.4394 0.8094 0.051 Uiso 1 1 calc R U . . .
C64 C 0.2138(6) 0.5095(4) 0.8152(3) 0.054(2) Uani 1 1 d . . . . .
H64A H 0.2292 0.5164 0.8444 0.065 Uiso 1 1 calc R U . . .
C65 C 0.1372(5) 0.5433(3) 0.7934(3) 0.0457(17) Uani 1 1 d . . . . .
H65A H 0.0970 0.5741 0.8072 0.055 Uiso 1 1 calc R U . . .
C66 C 0.1182(5) 0.5327(3) 0.7511(3) 0.0458(18) Uani 1 1 d . . . . .
H66A H 0.0648 0.5575 0.7357 0.055 Uiso 1 1 calc R U . . .
Fe2 Fe 0.63290(6) 0.51190(3) 0.75321(3) 0.01958(16) Uani 1 1 d . . . . .
N21 N 0.6707(3) 0.5339(2) 0.81067(17) 0.0233(9) Uani 1 1 d . . . . .
N22 N 0.5609(3) 0.44425(19) 0.80677(15) 0.0189(9) Uani 1 1 d . . . . .
N23 N 0.5035(3) 0.3934(2) 0.81235(16) 0.0213(9) Uani 1 1 d . . . . .
H23B H 0.4888 0.3805 0.7879 0.026 Uiso 1 1 calc R U . . .
N24 N 0.4099(3) 0.1687(2) 0.79405(15) 0.0183(8) Uani 1 1 d . . . . .
H24 H 0.4623 0.1936 0.7851 0.022 Uiso 1 1 calc R U . . .
N25 N 0.3915(3) 0.1265(2) 0.76996(16) 0.0202(9) Uani 1 1 d . . . . .
N26 N 0.1856(4) 0.0161(3) 0.81062(19) 0.0344(12) Uani 1 1 d . . . . .
N27 N 0.7191(3) 0.5801(2) 0.70466(17) 0.0219(9) Uani 1 1 d . . . . .
N28 N 0.7578(3) 0.45969(19) 0.74579(17) 0.0206(9) Uani 1 1 d . . . . .
N29 N 0.7908(3) 0.39777(19) 0.76377(16) 0.0198(9) Uani 1 1 d . . . . .
H29 H 0.7527 0.3662 0.7829 0.024 Uiso 1 1 calc R U . . .
N30 N 0.8077(3) 0.1400(2) 0.79977(17) 0.0222(9) Uani 1 1 d . . . . .
H30 H 0.7722 0.1721 0.7826 0.027 Uiso 1 1 calc R U . . .
N31 N 0.7747(3) 0.0789(2) 0.81997(16) 0.0220(9) Uani 1 1 d . . . . .
N32 N 0.9311(4) -0.0541(2) 0.88158(19) 0.0336(11) Uani 1 1 d . . . . .
N33 N 0.5105(3) 0.57181(19) 0.75196(15) 0.0199(9) Uani 1 1 d . . . . .
N34 N 0.5745(3) 0.4930(2) 0.70098(16) 0.0202(9) Uani 1 1 d . . . . .
N35 N 0.5962(3) 0.45281(19) 0.67157(15) 0.0194(9) Uani 1 1 d . . . . .
H35 H 0.6473 0.4243 0.6726 0.023 Uiso 1 1 calc R U . . .
N36 N 0.6664(3) 0.2306(2) 0.62670(16) 0.0224(9) Uani 1 1 d . . . . .
H36B H 0.6472 0.2422 0.6539 0.027 Uiso 1 1 calc R U . . .
N37 N 0.7187(3) 0.1748(2) 0.62497(16) 0.0221(9) Uani 1 1 d . . . . .
N38 N 0.8340(4) 0.0773(2) 0.59581(19) 0.0306(11) Uani 1 1 d . . . . .
C71 C 0.7307(4) 0.5809(3) 0.8103(2) 0.0287(13) Uani 1 1 d . . . . .
H71A H 0.7632 0.6059 0.7795 0.034 Uiso 1 1 calc R U . . .
C72 C 0.7482(5) 0.5954(3) 0.8521(3) 0.0367(15) Uani 1 1 d . . . . .
H72A H 0.7912 0.6295 0.8499 0.044 Uiso 1 1 calc R U . . .
C73 C 0.7021(5) 0.5594(3) 0.8969(3) 0.0399(16) Uani 1 1 d . . . . .
H73A H 0.7130 0.5682 0.9261 0.048 Uiso 1 1 calc R U . . .
C74 C 0.6393(5) 0.5099(3) 0.8990(2) 0.0304(13) Uani 1 1 d . . . . .
H74A H 0.6057 0.4847 0.9295 0.036 Uiso 1 1 calc R U . . .
C75 C 0.6273(4) 0.4983(2) 0.8551(2) 0.0236(11) Uani 1 1 d . . . . .
C76 C 0.5658(4) 0.4471(2) 0.8522(2) 0.0225(11) Uani 1 1 d . . . . .
C77 C 0.5105(4) 0.3989(3) 0.8868(2) 0.0253(11) Uani 1 1 d . . . . .
H77A H 0.5015 0.3910 0.9214 0.030 Uiso 1 1 calc R U . . .
C78 C 0.4710(4) 0.3644(2) 0.86051(19) 0.0201(10) Uani 1 1 d . . . . .
C79 C 0.4083(4) 0.3076(2) 0.87746(19) 0.0210(10) Uani 1 1 d . . . . .
C80 C 0.3549(4) 0.2920(3) 0.9250(2) 0.0279(12) Uani 1 1 d . . . . .
H80A H 0.3583 0.3192 0.9456 0.034 Uiso 1 1 calc R U . . .
C81 C 0.2972(5) 0.2371(3) 0.9423(2) 0.0311(13) Uani 1 1 d . . . . .
H81A H 0.2616 0.2267 0.9748 0.037 Uiso 1 1 calc R U . . .
C82 C 0.2911(4) 0.1970(3) 0.9123(2) 0.0272(12) Uani 1 1 d . . . . .
H82A H 0.2509 0.1596 0.9242 0.033 Uiso 1 1 calc R U . . .
C83 C 0.3442(4) 0.2121(3) 0.86480(19) 0.0215(10) Uani 1 1 d . . . . .
C84 C 0.4010(4) 0.2673(2) 0.84778(19) 0.0210(10) Uani 1 1 d . . . . .
H84A H 0.4358 0.2779 0.8152 0.025 Uiso 1 1 calc R U . . .
C85 C 0.3393(4) 0.1689(2) 0.83354(19) 0.0205(10) Uani 1 1 d . . . . .
C86 C 0.2709(4) 0.1244(3) 0.8350(2) 0.0220(11) Uani 1 1 d . . . . .
H86A H 0.2122 0.1127 0.8584 0.026 Uiso 1 1 calc R U . . .
C87 C 0.3053(4) 0.0996(2) 0.79485(19) 0.0219(11) Uani 1 1 d . . . . .
C88 C 0.2598(4) 0.0505(2) 0.7786(2) 0.0229(11) Uani 1 1 d . . . . .
C89 C 0.2915(4) 0.0423(3) 0.7331(2) 0.0270(12) Uani 1 1 d . . . . .
H89A H 0.3417 0.0689 0.7109 0.032 Uiso 1 1 calc R U . . .
C90 C 0.2487(5) -0.0059(3) 0.7200(2) 0.0379(15) Uani 1 1 d . . . . .
H90A H 0.2709 -0.0133 0.6889 0.046 Uiso 1 1 calc R U . . .
C91 C 0.1758(5) -0.0422(3) 0.7515(3) 0.0410(17) Uani 1 1 d . . . . .
H91A H 0.1465 -0.0754 0.7428 0.049 Uiso 1 1 calc R U . . .
C92 C 0.1445(5) -0.0305(3) 0.7964(2) 0.0369(15) Uani 1 1 d . . . . .
H92A H 0.0924 -0.0558 0.8182 0.044 Uiso 1 1 calc R U . . .
C93 C 0.6937(5) 0.6422(2) 0.6839(2) 0.0272(12) Uani 1 1 d . . . . .
H93A H 0.6260 0.6570 0.6908 0.033 Uiso 1 1 calc R U . . .
C94 C 0.7608(5) 0.6858(3) 0.6531(2) 0.0362(15) Uani 1 1 d . . . . .
H94A H 0.7394 0.7299 0.6395 0.043 Uiso 1 1 calc R U . . .
C95 C 0.8595(5) 0.6657(3) 0.6418(2) 0.0376(15) Uani 1 1 d . . . . .
H95A H 0.9068 0.6957 0.6207 0.045 Uiso 1 1 calc R U . . .
C96 C 0.8878(5) 0.6016(3) 0.6617(2) 0.0323(13) Uani 1 1 d . . . . .
H96A H 0.9549 0.5860 0.6542 0.039 Uiso 1 1 calc R U . . .
C97 C 0.8167(4) 0.5600(3) 0.6930(2) 0.0235(11) Uani 1 1 d . . . . .
C98 C 0.8372(4) 0.4918(2) 0.7173(2) 0.0241(11) Uani 1 1 d . . . . .
C99 C 0.9221(4) 0.4496(3) 0.7180(2) 0.0268(12) Uani 1 1 d . . . . .
H99A H 0.9878 0.4598 0.7009 0.032 Uiso 1 1 calc R U . . .
C100 C 0.8911(4) 0.3903(2) 0.7484(2) 0.0239(11) Uani 1 1 d . . . . .
C101 C 0.9465(4) 0.3279(3) 0.7631(2) 0.0238(11) Uani 1 1 d . . . . .
C102 C 1.0504(5) 0.3268(3) 0.7610(2) 0.0332(13) Uani 1 1 d . . . . .
H10B H 1.0846 0.3667 0.7508 0.040 Uiso 1 1 calc R U . . .
C103 C 1.1039(4) 0.2677(3) 0.7737(3) 0.0399(15) Uani 1 1 d . . . . .
H10C H 1.1749 0.2673 0.7718 0.048 Uiso 1 1 calc R U . . .
C104 C 1.0548(4) 0.2094(3) 0.7890(2) 0.0315(13) Uani 1 1 d . . . . .
H10D H 1.0924 0.1692 0.7977 0.038 Uiso 1 1 calc R U . . .
C105 C 0.9511(4) 0.2091(2) 0.7917(2) 0.0237(11) Uani 1 1 d . . . . .
C106 C 0.8986(4) 0.2686(2) 0.77873(19) 0.0227(11) Uani 1 1 d . . . . .
H10E H 0.8276 0.2690 0.7806 0.027 Uiso 1 1 calc R U . . .
C107 C 0.9009(4) 0.1470(2) 0.80858(19) 0.0222(11) Uani 1 1 d . . . . .
C108 C 0.9299(4) 0.0866(3) 0.8365(2) 0.0249(11) Uani 1 1 d . . . . .
H10F H 0.9916 0.0747 0.8492 0.030 Uiso 1 1 calc R U . . .
C109 C 0.8501(4) 0.0463(3) 0.8423(2) 0.0267(12) Uani 1 1 d . . . . .
C110 C 0.8437(4) -0.0240(3) 0.8709(2) 0.0230(11) Uani 1 1 d . . . . .
C111 C 0.7525(4) -0.0553(3) 0.8852(2) 0.0265(12) Uani 1 1 d . . . . .
H11B H 0.6918 -0.0324 0.8767 0.032 Uiso 1 1 calc R U . . .
C112 C 0.7522(5) -0.1203(3) 0.9121(2) 0.0322(13) Uani 1 1 d . . . . .
H11C H 0.6912 -0.1429 0.9226 0.039 Uiso 1 1 calc R U . . .
C113 C 0.8415(5) -0.1513(3) 0.9233(2) 0.0357(14) Uani 1 1 d . . . . .
H11D H 0.8435 -0.1961 0.9414 0.043 Uiso 1 1 calc R U . . .
C114 C 0.9281(5) -0.1172(3) 0.9083(3) 0.0387(15) Uani 1 1 d . . . . .
H11E H 0.9892 -0.1392 0.9171 0.046 Uiso 1 1 calc R U . . .
C115 C 0.4812(4) 0.6120(2) 0.7807(2) 0.0236(11) Uani 1 1 d . . . . .
H11F H 0.5198 0.6117 0.8055 0.028 Uiso 1 1 calc R U . . .
C116 C 0.3975(4) 0.6534(3) 0.7753(2) 0.0287(12) Uani 1 1 d . . . . .
H11G H 0.3784 0.6804 0.7967 0.034 Uiso 1 1 calc R U . . .
C117 C 0.3415(4) 0.6556(3) 0.7389(2) 0.0291(12) Uani 1 1 d . . . . .
H11H H 0.2845 0.6847 0.7340 0.035 Uiso 1 1 calc R U . . .
C118 C 0.3703(4) 0.6143(3) 0.7096(2) 0.0266(12) Uani 1 1 d . . . . .
H11I H 0.3326 0.6145 0.6844 0.032 Uiso 1 1 calc R U . . .
C119 C 0.4535(4) 0.5728(2) 0.71675(19) 0.0207(10) Uani 1 1 d . . . . .
C120 C 0.4912(4) 0.5273(2) 0.68863(19) 0.0211(10) Uani 1 1 d . . . . .
C121 C 0.4586(4) 0.5099(2) 0.65040(19) 0.0216(10) Uani 1 1 d . . . . .
H12B H 0.4013 0.5268 0.6349 0.026 Uiso 1 1 calc R U . . .
C122 C 0.5281(4) 0.4629(2) 0.64037(18) 0.0202(10) Uani 1 1 d . . . . .
C123 C 0.5317(4) 0.4252(2) 0.60422(18) 0.0194(10) Uani 1 1 d . . . . .
C124 C 0.4780(4) 0.4475(2) 0.56488(19) 0.0237(11) Uani 1 1 d . . . . .
H12C H 0.4397 0.4876 0.5609 0.028 Uiso 1 1 calc R U . . .
C125 C 0.4801(5) 0.4117(3) 0.5317(2) 0.0284(12) Uani 1 1 d . . . . .
H12D H 0.4429 0.4273 0.5051 0.034 Uiso 1 1 calc R U . . .
C126 C 0.5359(5) 0.3533(3) 0.5370(2) 0.0270(12) Uani 1 1 d . . . . .
H12E H 0.5371 0.3291 0.5139 0.032 Uiso 1 1 calc R U . . .
C127 C 0.5897(4) 0.3302(2) 0.57574(19) 0.0223(11) Uani 1 1 d . . . . .
C128 C 0.5868(4) 0.3664(2) 0.60964(19) 0.0209(10) Uani 1 1 d . . . . .
H12F H 0.6229 0.3504 0.6366 0.025 Uiso 1 1 calc R U . . .
C129 C 0.6465(4) 0.2671(2) 0.58228(19) 0.0211(10) Uani 1 1 d . . . . .
C130 C 0.6875(4) 0.2332(3) 0.5498(2) 0.0260(12) Uani 1 1 d . . . . .
H13A H 0.6860 0.2457 0.5154 0.031 Uiso 1 1 calc R U . . .
C131 C 0.7324(4) 0.1760(3) 0.5774(2) 0.0229(11) Uani 1 1 d . . . . .
C132 C 0.7883(4) 0.1215(3) 0.5616(2) 0.0260(12) Uani 1 1 d . . . . .
C133 C 0.7903(5) 0.1164(3) 0.5150(2) 0.0367(14) Uani 1 1 d . . . . .
H13B H 0.7569 0.1486 0.4918 0.044 Uiso 1 1 calc R U . . .
C134 C 0.8428(5) 0.0625(4) 0.5023(3) 0.0454(17) Uani 1 1 d . . . . .
H13C H 0.8462 0.0575 0.4703 0.055 Uiso 1 1 calc R U . . .
C135 C 0.8892(5) 0.0173(3) 0.5375(3) 0.0364(15) Uani 1 1 d . . . . .
H13D H 0.9250 -0.0198 0.5303 0.044 Uiso 1 1 calc R U . . .
C136 C 0.8830(4) 0.0268(3) 0.5823(3) 0.0348(14) Uani 1 1 d . . . . .
H13E H 0.9158 -0.0048 0.6060 0.042 Uiso 1 1 calc R U . . .
Cl1 Cl 0.62674(8) 0.24318(6) 0.74267(5) 0.0208(2) Uani 1 1 d . . . . .
Fe3 Fe 1.04193(7) -0.25374(6) 0.71398(6) 0.0599(3) Uani 1 1 d . . . . .
Cl2 Cl 1.12530(13) -0.22361(10) 0.76274(9) 0.0588(6) Uani 1 1 d . . . . .
Cl3 Cl 1.14155(16) -0.30028(12) 0.66471(10) 0.0756(7) Uani 1 1 d . . . . .
Cl4 Cl 0.93485(16) -0.32489(12) 0.75981(12) 0.0841(9) Uani 1 1 d . . . . .
Cl5 Cl 0.96500(19) -0.16804(14) 0.67079(12) 0.0905(9) Uani 1 1 d . . . . .
Cl6 Cl 0.52098(12) 0.70269(7) 0.85634(5) 0.0335(3) Uani 1 1 d D . . . .
Fe4 Fe 0.53562(10) 0.70908(5) 0.92962(3) 0.0328(3) Uani 0.873(3) 1 d D . P A 1
Cl7 Cl 0.69308(15) 0.70540(9) 0.94143(7) 0.0412(5) Uani 0.873(3) 1 d D . P A 1
Cl8 Cl 0.4636(4) 0.6263(2) 0.98359(13) 0.0844(15) Uani 0.873(3) 1 d D . P A 1
Cl9 Cl 0.4640(2) 0.80315(12) 0.93479(8) 0.0744(9) Uani 0.873(3) 1 d D . P A 1
Fe4B Fe 0.4715(7) 0.7115(4) 0.9297(3) 0.050(3) Uiso 0.127(3) 1 d D . P A 2
Cl7B Cl 0.3290(11) 0.7648(8) 0.9352(6) 0.083(6) Uiso 0.127(3) 1 d D . P A 2
Cl8B Cl 0.4678(11) 0.6154(5) 0.9831(4) 0.011(2) Uiso 0.127(3) 1 d D . P A 2
Cl9B Cl 0.5873(14) 0.7657(10) 0.9478(7) 0.162(14) Uiso 0.127(3) 1 d D . P A 2
Fe5 Fe 0.53449(7) 0.76852(4) 0.57053(3) 0.0343(2) Uani 1 1 d D . . . .
Cl10 Cl 0.52466(11) 0.78100(7) 0.64399(5) 0.0310(3) Uani 1 1 d . . . . .
Cl11 Cl 0.69236(13) 0.77063(8) 0.53529(6) 0.0423(4) Uani 1 1 d . . . . .
Cl12 Cl 0.45453(14) 0.84869(13) 0.52450(6) 0.0663(6) Uani 1 1 d . . . . .
Cl13 Cl 0.4829(3) 0.67059(14) 0.57858(8) 0.0539(13) Uani 0.785(9) 1 d D . P B 1
Cl14 Cl 0.4241(9) 0.6952(5) 0.5755(3) 0.050(3) Uiso 0.215(9) 1 d D . P B 2
C1S C 0.0573(7) 0.0867(5) 0.9558(4) 0.082(3) Uani 1 1 d D . . . .
H1SA H -0.0126 0.0735 0.9628 0.123 Uiso 1 1 calc R U . . .
H1SB H 0.0727 0.1115 0.9212 0.123 Uiso 1 1 calc R U . . .
H1SC H 0.0669 0.1142 0.9766 0.123 Uiso 1 1 calc R U . . .
C2S C 0.1256(5) 0.0276(3) 0.9660(3) 0.0458(17) Uani 1 1 d D . . . .
C3S C 0.1345(6) -0.0172(4) 0.9396(3) 0.057(2) Uani 1 1 d D . . . .
H3SA H 0.0972 -0.0102 0.9132 0.068 Uiso 1 1 calc R U . . .
C4S C 0.1971(6) -0.0726(4) 0.9508(3) 0.059(2) Uani 1 1 d D . . . .
H4SA H 0.2018 -0.1035 0.9324 0.071 Uiso 1 1 calc R U . . .
C5S C 0.2528(6) -0.0829(3) 0.9891(3) 0.056(2) Uani 1 1 d D . . . .
H5SA H 0.2964 -0.1205 0.9965 0.067 Uiso 1 1 calc R U . . .
C6S C 0.2451(6) -0.0395(4) 1.0156(3) 0.055(2) Uani 1 1 d D . . . .
H6SA H 0.2823 -0.0470 1.0421 0.066 Uiso 1 1 calc R U . . .
C7S C 0.1824(5) 0.0163(4) 1.0041(3) 0.0487(18) Uani 1 1 d D . . . .
H7SA H 0.1783 0.0471 1.0226 0.058 Uiso 1 1 calc R U . . .
C8S C 0.2576(7) -0.1306(5) 0.6310(3) 0.075(3) Uani 1 1 d . . . . .
H8SA H 0.3290 -0.1433 0.6314 0.112 Uiso 1 1 calc R U . . .
H8SB H 0.2296 -0.1525 0.6107 0.112 Uiso 1 1 calc R U . . .
H8SC H 0.2215 -0.1435 0.6646 0.112 Uiso 1 1 calc R U . . .
C9S C 0.2461(7) -0.0576(4) 0.6100(3) 0.058(2) Uani 1 1 d . . . . .
C10S C 0.3244(6) -0.0197(5) 0.5814(3) 0.057(2) Uani 1 1 d . . . . .
H10G H 0.3888 -0.0400 0.5755 0.068 Uiso 1 1 calc R U . . .
C11S C 0.3111(8) 0.0471(5) 0.5613(3) 0.072(3) Uani 1 1 d . . . . .
H11J H 0.3659 0.0720 0.5418 0.086 Uiso 1 1 calc R U . . .
C12S C 0.2201(8) 0.0768(5) 0.5694(4) 0.076(3) Uani 1 1 d . . . . .
H12G H 0.2114 0.1226 0.5553 0.091 Uiso 1 1 calc R U . . .
C13S C 0.1403(7) 0.0418(4) 0.5975(3) 0.061(2) Uani 1 1 d . . . . .
H13F H 0.0770 0.0635 0.6032 0.073 Uiso 1 1 calc R U . . .
C14S C 0.1514(6) -0.0258(4) 0.6180(3) 0.0496(18) Uani 1 1 d . . . . .
H14B H 0.0956 -0.0501 0.6371 0.060 Uiso 1 1 calc R U . . .
C15S C 0.1248(11) 0.3447(8) 0.8819(6) 0.096(4) Uani 0.659(9) 1 d D U P C 1
H15B H 0.1635 0.3717 0.8942 0.144 Uiso 0.659(9) 1 calc R U P C 1
H15C H 0.1710 0.3158 0.8667 0.144 Uiso 0.659(9) 1 calc R U P C 1
H15D H 0.0858 0.3729 0.8575 0.144 Uiso 0.659(9) 1 calc R U P C 1
C16S C 0.0545(11) 0.3041(7) 0.9238(6) 0.107(3) Uani 0.659(9) 1 d D U P C 1
C17S C -0.0086(14) 0.2616(9) 0.9168(7) 0.116(3) Uani 0.659(9) 1 d D U P C 1
H17A H -0.0059 0.2555 0.8852 0.140 Uiso 0.659(9) 1 calc R U P C 1
C18S C -0.0768(15) 0.2275(10) 0.9557(7) 0.124(3) Uani 0.659(9) 1 d D U P C 1
H18A H -0.1223 0.1999 0.9499 0.149 Uiso 0.659(9) 1 calc R U P C 1
C19S C -0.0798(14) 0.2329(9) 1.0036(7) 0.123(4) Uani 0.659(9) 1 d D U P C 1
H19B H -0.1272 0.2096 1.0298 0.147 Uiso 0.659(9) 1 calc R U P C 1
C20S C -0.0145(14) 0.2716(9) 1.0117(6) 0.119(3) Uani 0.659(9) 1 d D U P C 1
H20B H -0.0146 0.2755 1.0438 0.143 Uiso 0.659(9) 1 calc R U P C 1
C21S C 0.0543(14) 0.3065(9) 0.9718(6) 0.110(3) Uani 0.659(9) 1 d D U P C 1
H21B H 0.1019 0.3323 0.9779 0.132 Uiso 0.659(9) 1 calc R U P C 1
C35S C 0.092(3) 0.3633(15) 0.8738(14) 0.117(8) Uiso 0.341(9) 1 d D U P C 2
C36S C 0.0540(18) 0.2992(12) 0.9076(10) 0.108(4) Uiso 0.341(9) 1 d D U P C 2
C37S C 0.005(2) 0.2579(15) 0.8906(10) 0.116(4) Uiso 0.341(9) 1 d D U P C 2
C38S C -0.029(3) 0.1987(15) 0.9212(12) 0.121(5) Uiso 0.341(9) 1 d D U P C 2
C39S C -0.010(3) 0.1779(14) 0.9697(11) 0.125(4) Uiso 0.341(9) 1 d D U P C 2
C40S C 0.030(3) 0.2207(15) 0.9872(10) 0.115(4) Uiso 0.341(9) 1 d D U P C 2
C41S C 0.059(3) 0.2820(15) 0.9579(10) 0.112(4) Uiso 0.341(9) 1 d D U P C 2
C22S C 0.1713(16) 0.6719(8) 0.8859(7) 0.224(8) Uani 1 1 d D U . . .
H22B H 0.2332 0.6961 0.8732 0.336 Uiso 1 1 calc R U . . .
H22C H 0.1323 0.6766 0.8592 0.336 Uiso 1 1 calc R U . . .
H22D H 0.1314 0.6895 0.9114 0.336 Uiso 1 1 calc R U . . .
C23S C 0.1979(10) 0.5999(7) 0.9078(5) 0.128(3) Uani 1 1 d D U . . .
C24S C 0.1157(10) 0.5591(7) 0.9276(5) 0.128(3) Uani 1 1 d D U . . .
H24B H 0.0497 0.5751 0.9219 0.154 Uiso 1 1 calc R U . . .
C25S C 0.1313(11) 0.4959(7) 0.9553(5) 0.127(3) Uani 1 1 d D U . . .
H25B H 0.0745 0.4696 0.9689 0.153 Uiso 1 1 calc R U . . .
C26S C 0.2247(10) 0.4689(7) 0.9642(5) 0.125(3) Uani 1 1 d D U . . .
H26B H 0.2318 0.4247 0.9830 0.150 Uiso 1 1 calc R U . . .
C27S C 0.3053(10) 0.5054(7) 0.9464(5) 0.120(3) Uani 1 1 d D U . . .
H27A H 0.3704 0.4872 0.9521 0.144 Uiso 1 1 calc R U . . .
C28S C 0.2929(10) 0.5724(7) 0.9186(5) 0.130(3) Uani 1 1 d D U . . .
H28A H 0.3501 0.5987 0.9072 0.156 Uiso 1 1 calc R U . . .
O1S O 0.1771(5) 0.4656(3) 0.5879(2) 0.0719(17) Uani 1 1 d . . . . .
C29S C 0.2012(5) 0.5220(4) 0.5675(3) 0.054(2) Uani 1 1 d . . . . .
C30S C 0.2294(6) 0.5445(5) 0.5137(3) 0.070(3) Uani 1 1 d . . . . .
H30A H 0.2139 0.5109 0.4991 0.104 Uiso 1 1 calc R U . . .
H30B H 0.3015 0.5523 0.5057 0.104 Uiso 1 1 calc R U . . .
H30C H 0.1914 0.5851 0.5005 0.104 Uiso 1 1 calc R U . . .
C31S C 0.1979(8) 0.5709(6) 0.5956(4) 0.088(3) Uani 1 1 d . . . . .
H31A H 0.1817 0.5493 0.6307 0.133 Uiso 1 1 calc R U . . .
H31B H 0.1464 0.6050 0.5855 0.133 Uiso 1 1 calc R U . . .
H31C H 0.2636 0.5907 0.5890 0.133 Uiso 1 1 calc R U . . .
O2S O 1.0658(7) 0.7194(5) 0.5298(4) 0.123(3) Uani 1 1 d . U . . .
C32S C 1.0134(8) 0.7648(5) 0.5038(4) 0.079(2) Uani 1 1 d . U . . .
C33S C 0.9976(11) 0.7694(6) 0.4563(4) 0.106(3) Uani 1 1 d . U . . .
H33B H 1.0307 0.7317 0.4462 0.159 Uiso 1 1 calc R U . . .
H33C H 1.0256 0.8098 0.4338 0.159 Uiso 1 1 calc R U . . .
H33D H 0.9252 0.7698 0.4553 0.159 Uiso 1 1 calc R U . . .
C34S C 0.9622(7) 0.8184(6) 0.5270(4) 0.093(3) Uani 1 1 d . U . . .
H34B H 0.9976 0.8207 0.5535 0.139 Uiso 1 1 calc R U . . .
H34C H 0.8920 0.8076 0.5402 0.139 Uiso 1 1 calc R U . . .
H34D H 0.9643 0.8606 0.5019 0.139 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.960(4) . ?
Fe1 N14 1.963(4) . ?
Fe1 N8 1.968(4) . ?
Fe1 N1 1.998(4) . ?
Fe1 N13 2.008(4) . ?
Fe1 N7 2.016(4) . ?
N1 C1 1.348(6) . ?
N1 C5 1.360(7) . ?
N2 C6 1.324(6) . ?
N2 N3 1.359(5) . ?
N3 C8 1.358(6) . ?
N3 H3 0.8800 . ?
N4 N5 1.348(6) . ?
N4 C15 1.361(7) . ?
N4 H4 0.8800 . ?
N5 C17 1.337(7) . ?
N6 C22 1.341(8) . ?
N6 C18 1.345(8) . ?
N7 C23 1.326(7) . ?
N7 C27 1.351(7) . ?
N8 N9 1.341(6) . ?
N8 C28 1.342(7) . ?
N9 C30 1.345(7) . ?
N9 H9A 0.8800 . ?
N10 N11 1.339(6) . ?
N10 C37 1.355(7) . ?
N10 H10H 0.8800 . ?
N11 C39 1.344(7) . ?
N12 C40 1.334(7) . ?
N12 C44 1.336(9) . ?
N13 C45 1.345(6) . ?
N13 C49 1.352(7) . ?
N14 C50 1.337(6) . ?
N14 N15 1.341(5) . ?
N15 C52 1.363(6) . ?
N15 H15A 0.8800 . ?
N16 C59 1.354(7) . ?
N16 N17 1.356(6) . ?
N16 H16 0.8800 . ?
N17 C61 1.336(7) . ?
N18 C62 1.339(8) . ?
N18 C66 1.353(8) . ?
C1 C2 1.382(8) . ?
C1 H1A 0.9500 . ?
C2 C3 1.376(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.388(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.368(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.456(6) . ?
C6 C7 1.399(7) . ?
C7 C8 1.371(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.482(7) . ?
C9 C14 1.377(7) . ?
C9 C10 1.402(7) . ?
C10 C11 1.388(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.382(8) . ?
C11 H11A 0.9500 . ?
C12 C13 1.386(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.401(7) . ?
C13 C15 1.451(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.380(7) . ?
C16 C17 1.404(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.468(7) . ?
C18 C19 1.374(8) . ?
C19 C20 1.400(9) . ?
C19 H19A 0.9500 . ?
C20 C21 1.350(11) . ?
C20 H20A 0.9500 . ?
C21 C22 1.371(10) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.386(8) . ?
C23 H23A 0.9500 . ?
C24 C25 1.379(9) . ?
C24 H24A 0.9500 . ?
C25 C26 1.379(8) . ?
C25 H25A 0.9500 . ?
C26 C27 1.370(8) . ?
C26 H26A 0.9500 . ?
C27 C28 1.460(7) . ?
C28 C29 1.389(8) . ?
C29 C30 1.373(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.458(7) . ?
C31 C36 1.400(7) . ?
C31 C32 1.408(8) . ?
C32 C33 1.380(8) . ?
C32 H32A 0.9500 . ?
C33 C34 1.380(8) . ?
C33 H33A 0.9500 . ?
C34 C35 1.390(8) . ?
C34 H34A 0.9500 . ?
C35 C36 1.387(7) . ?
C35 C37 1.454(7) . ?
C36 H36A 0.9500 . ?
C37 C38 1.384(8) . ?
C38 C39 1.396(8) . ?
C38 H38A 0.9500 . ?
C39 C40 1.469(8) . ?
C40 C41 1.383(8) . ?
C41 C42 1.378(8) . ?
C41 H41A 0.9500 . ?
C42 C43 1.364(10) . ?
C42 H42A 0.9500 . ?
C43 C44 1.393(10) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.393(8) . ?
C45 H45A 0.9500 . ?
C46 C47 1.371(9) . ?
C46 H46A 0.9500 . ?
C47 C48 1.382(8) . ?
C47 H47A 0.9500 . ?
C48 C49 1.386(7) . ?
C48 H48A 0.9500 . ?
C49 C50 1.459(7) . ?
C50 C51 1.388(7) . ?
C51 C52 1.384(7) . ?
C51 H51A 0.9500 . ?
C52 C53 1.455(7) . ?
C53 C54 1.396(7) . ?
C53 C58 1.404(7) . ?
C54 C55 1.382(7) . ?
C54 H54A 0.9500 . ?
C55 C56 1.378(7) . ?
C55 H55A 0.9500 . ?
C56 C57 1.399(7) . ?
C56 H56A 0.9500 . ?
C57 C58 1.392(7) . ?
C57 C59 1.464(7) . ?
C58 H58A 0.9500 . ?
C59 C60 1.379(7) . ?
C60 C61 1.415(7) . ?
C60 H60A 0.9500 . ?
C61 C62 1.473(7) . ?
C62 C63 1.372(8) . ?
C63 C64 1.394(9) . ?
C63 H63A 0.9500 . ?
C64 C65 1.347(10) . ?
C64 H64A 0.9500 . ?
C65 C66 1.368(10) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
Fe2 N28 1.958(4) . ?
Fe2 N34 1.959(4) . ?
Fe2 N22 1.967(4) . ?
Fe2 N21 1.994(4) . ?
Fe2 N27 2.002(4) . ?
Fe2 N33 2.003(4) . ?
N21 C71 1.338(7) . ?
N21 C75 1.350(7) . ?
N22 C76 1.339(6) . ?
N22 N23 1.344(6) . ?
N23 C78 1.360(7) . ?
N23 H23B 0.8800 . ?
N24 N25 1.345(6) . ?
N24 C85 1.359(6) . ?
N24 H24 0.8800 . ?
N25 C87 1.340(7) . ?
N26 C88 1.350(8) . ?
N26 C92 1.368(8) . ?
N27 C93 1.331(7) . ?
N27 C97 1.370(7) . ?
N28 N29 1.342(6) . ?
N28 C98 1.342(7) . ?
N29 C100 1.364(7) . ?
N29 H29 0.8800 . ?
N30 N31 1.348(6) . ?
N30 C107 1.350(7) . ?
N30 H30 0.8800 . ?
N31 C109 1.332(7) . ?
N32 C110 1.333(7) . ?
N32 C114 1.347(8) . ?
N33 C115 1.349(6) . ?
N33 C119 1.363(7) . ?
N34 C120 1.331(7) . ?
N34 N35 1.353(6) . ?
N35 C122 1.351(7) . ?
N35 H35 0.8800 . ?
N36 N37 1.343(6) . ?
N36 C129 1.349(7) . ?
N36 H36B 0.8800 . ?
N37 C131 1.343(7) . ?
N38 C136 1.338(7) . ?
N38 C132 1.345(8) . ?
C71 C72 1.386(8) . ?
C71 H71A 0.9500 . ?
C72 C73 1.372(10) . ?
C72 H72A 0.9500 . ?
C73 C74 1.391(9) . ?
C73 H73A 0.9500 . ?
C74 C75 1.393(7) . ?
C74 H74A 0.9500 . ?
C75 C76 1.454(7) . ?
C76 C77 1.379(8) . ?
C77 C78 1.384(7) . ?
C77 H77A 0.9500 . ?
C78 C79 1.457(7) . ?
C79 C84 1.395(7) . ?
C79 C80 1.399(8) . ?
C80 C81 1.386(8) . ?
C80 H80A 0.9500 . ?
C81 C82 1.394(8) . ?
C81 H81A 0.9500 . ?
C82 C83 1.396(7) . ?
C82 H82A 0.9500 . ?
C83 C84 1.383(7) . ?
C83 C85 1.475(7) . ?
C84 H84A 0.9500 . ?
C85 C86 1.366(7) . ?
C86 C87 1.402(7) . ?
C86 H86A 0.9500 . ?
C87 C88 1.476(7) . ?
C88 C89 1.366(8) . ?
C89 C90 1.388(9) . ?
C89 H89A 0.9500 . ?
C90 C91 1.349(10) . ?
C90 H90A 0.9500 . ?
C91 C92 1.378(10) . ?
C91 H91A 0.9500 . ?
C92 H92A 0.9500 . ?
C93 C94 1.368(9) . ?
C93 H93A 0.9500 . ?
C94 C95 1.381(10) . ?
C94 H94A 0.9500 . ?
C95 C96 1.374(8) . ?
C95 H95A 0.9500 . ?
C96 C97 1.385(8) . ?
C96 H96A 0.9500 . ?
C97 C98 1.450(7) . ?
C98 C99 1.397(8) . ?
C99 C100 1.368(8) . ?
C99 H99A 0.9500 . ?
C100 C101 1.460(7) . ?
C101 C106 1.391(7) . ?
C101 C102 1.391(8) . ?
C102 C103 1.385(9) . ?
C102 H10B 0.9500 . ?
C103 C104 1.383(9) . ?
C103 H10C 0.9500 . ?
C104 C105 1.389(8) . ?
C104 H10D 0.9500 . ?
C105 C106 1.388(7) . ?
C105 C107 1.458(7) . ?
C106 H10E 0.9500 . ?
C107 C108 1.375(7) . ?
C108 C109 1.392(8) . ?
C108 H10F 0.9500 . ?
C109 C110 1.493(8) . ?
C110 C111 1.394(8) . ?
C111 C112 1.382(8) . ?
C111 H11B 0.9500 . ?
C112 C113 1.366(9) . ?
C112 H11C 0.9500 . ?
C113 C114 1.371(10) . ?
C113 H11D 0.9500 . ?
C114 H11E 0.9500 . ?
C115 C116 1.377(8) . ?
C115 H11F 0.9500 . ?
C116 C117 1.379(8) . ?
C116 H11G 0.9500 . ?
C117 C118 1.378(8) . ?
C117 H11H 0.9500 . ?
C118 C119 1.377(8) . ?
C118 H11I 0.9500 . ?
C119 C120 1.447(7) . ?
C120 C121 1.401(7) . ?
C121 C122 1.376(7) . ?
C121 H12B 0.9500 . ?
C122 C123 1.480(7) . ?
C123 C128 1.388(7) . ?
C123 C124 1.392(7) . ?
C124 C125 1.379(7) . ?
C124 H12C 0.9500 . ?
C125 C126 1.387(8) . ?
C125 H12D 0.9500 . ?
C126 C127 1.380(8) . ?
C126 H12E 0.9500 . ?
C127 C128 1.401(7) . ?
C127 C129 1.474(7) . ?
C128 H12F 0.9500 . ?
C129 C130 1.364(7) . ?
C130 C131 1.404(8) . ?
C130 H13A 0.9500 . ?
C131 C132 1.476(7) . ?
C132 C133 1.373(8) . ?
C133 C134 1.408(9) . ?
C133 H13B 0.9500 . ?
C134 C135 1.376(10) . ?
C134 H13C 0.9500 . ?
C135 C136 1.350(9) . ?
C135 H13D 0.9500 . ?
C136 H13E 0.9500 . ?
Fe3 Cl4 2.174(3) . ?
Fe3 Cl3 2.183(2) . ?
Fe3 Cl5 2.185(3) . ?
Fe3 Cl2 2.192(2) . ?
Cl6 Fe4B 2.163(8) . ?
Cl6 Fe4 2.1933(16) . ?
Fe4 Cl8 2.167(4) . ?
Fe4 Cl9 2.190(2) . ?
Fe4 Cl7 2.198(2) . ?
Fe4B Cl7B 2.159(12) . ?
Fe4B Cl8B 2.181(11) . ?
Fe4B Cl9B 2.229(12) . ?
Fe5 Cl12 2.171(2) . ?
Fe5 Cl10 2.1868(16) . ?
Fe5 Cl13 2.197(2) . ?
Fe5 Cl11 2.202(2) . ?
Fe5 Cl14 2.209(9) . ?
C1S C2S 1.489(10) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C2S C3S 1.368(9) . ?
C2S C7S 1.393(9) . ?
C3S C4S 1.386(10) . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.389(10) . ?
C4S H4SA 0.9500 . ?
C5S C6S 1.346(10) . ?
C5S H5SA 0.9500 . ?
C6S C7S 1.394(10) . ?
C6S H6SA 0.9500 . ?
C7S H7SA 0.9500 . ?
C8S C9S 1.507(12) . ?
C8S H8SA 0.9800 . ?
C8S H8SB 0.9800 . ?
C8S H8SC 0.9800 . ?
C9S C10S 1.387(12) . ?
C9S C14S 1.413(11) . ?
C10S C11S 1.387(13) . ?
C10S H10G 0.9500 . ?
C11S C12S 1.350(14) . ?
C11S H11J 0.9500 . ?
C12S C13S 1.370(13) . ?
C12S H12G 0.9500 . ?
C13S C14S 1.399(11) . ?
C13S H13F 0.9500 . ?
C14S H14B 0.9500 . ?
C15S C16S 1.505(14) . ?
C15S H15B 0.9800 . ?
C15S H15C 0.9800 . ?
C15S H15D 0.9800 . ?
C16S C17S 1.371(15) . ?
C16S C21S 1.396(15) . ?
C17S C18S 1.391(15) . ?
C17S H17A 0.9500 . ?
C18S C19S 1.408(16) . ?
C18S H18A 0.9500 . ?
C19S C20S 1.346(15) . ?
C19S H19B 0.9500 . ?
C20S C21S 1.417(15) . ?
C20S H20B 0.9500 . ?
C21S H21B 0.9500 . ?
C35S C36S 1.508(16) . ?
C36S C37S 1.382(16) . ?
C36S C41S 1.397(16) . ?
C37S C38S 1.383(17) . ?
C38S C39S 1.397(17) . ?
C39S C40S 1.353(17) . ?
C40S C41S 1.383(17) . ?
C22S C23S 1.523(14) . ?
C22S H22B 0.9800 . ?
C22S H22C 0.9800 . ?
C22S H22D 0.9800 . ?
C23S C24S 1.408(14) . ?
C23S C28S 1.410(14) . ?
C24S C25S 1.374(14) . ?
C24S H24B 0.9500 . ?
C25S C26S 1.374(14) . ?
C25S H25B 0.9500 . ?
C26S C27S 1.335(14) . ?
C26S H26B 0.9500 . ?
C27S C28S 1.436(14) . ?
C27S H27A 0.9500 . ?
C28S H28A 0.9500 . ?
O1S C29S 1.225(10) . ?
C29S C30S 1.478(12) . ?
C29S C31S 1.487(12) . ?
C30S H30A 0.9800 . ?
C30S H30B 0.9800 . ?
C30S H30C 0.9800 . ?
C31S H31A 0.9800 . ?
C31S H31B 0.9800 . ?
C31S H31C 0.9800 . ?
O2S C32S 1.283(13) . ?
C32S C33S 1.393(14) . ?
C32S C34S 1.544(14) . ?
C33S H33B 0.9800 . ?
C33S H33C 0.9800 . ?
C33S H33D 0.9800 . ?
C34S H34B 0.9800 . ?
C34S H34C 0.9800 . ?
C34S H34D 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
N2 Fe1 N14 95.52(17) . . ?
N2 Fe1 N8 95.95(17) . . ?
N14 Fe1 N8 95.55(17) . . ?
N2 Fe1 N1 79.91(17) . . ?
N14 Fe1 N1 92.77(17) . . ?
N8 Fe1 N1 171.04(18) . . ?
N2 Fe1 N13 170.92(18) . . ?
N14 Fe1 N13 80.45(17) . . ?
N8 Fe1 N13 92.54(17) . . ?
N1 Fe1 N13 92.11(17) . . ?
N2 Fe1 N7 91.53(17) . . ?
N14 Fe1 N7 172.28(17) . . ?
N8 Fe1 N7 80.54(17) . . ?
N1 Fe1 N7 91.57(17) . . ?
N13 Fe1 N7 93.01(17) . . ?
C1 N1 C5 116.7(4) . . ?
C1 N1 Fe1 127.8(4) . . ?
C5 N1 Fe1 115.3(3) . . ?
C6 N2 N3 106.2(4) . . ?
C6 N2 Fe1 116.5(3) . . ?
N3 N2 Fe1 137.3(3) . . ?
C8 N3 N2 110.3(4) . . ?
C8 N3 H3 124.9 . . ?
N2 N3 H3 124.9 . . ?
N5 N4 C15 113.1(4) . . ?
N5 N4 H4 123.4 . . ?
C15 N4 H4 123.4 . . ?
C17 N5 N4 105.0(4) . . ?
C22 N6 C18 117.9(5) . . ?
C23 N7 C27 117.6(5) . . ?
C23 N7 Fe1 127.6(4) . . ?
C27 N7 Fe1 114.7(3) . . ?
N9 N8 C28 105.6(4) . . ?
N9 N8 Fe1 138.7(3) . . ?
C28 N8 Fe1 115.7(3) . . ?
N8 N9 C30 111.5(4) . . ?
N8 N9 H9A 124.3 . . ?
C30 N9 H9A 124.3 . . ?
N11 N10 C37 114.5(4) . . ?
N11 N10 H10H 122.8 . . ?
C37 N10 H10H 122.8 . . ?
N10 N11 C39 104.1(4) . . ?
C40 N12 C44 117.2(6) . . ?
C45 N13 C49 118.1(5) . . ?
C45 N13 Fe1 126.7(4) . . ?
C49 N13 Fe1 115.1(3) . . ?
C50 N14 N15 105.9(4) . . ?
C50 N14 Fe1 115.6(3) . . ?
N15 N14 Fe1 138.5(3) . . ?
N14 N15 C52 111.4(4) . . ?
N14 N15 H15A 124.3 . . ?
C52 N15 H15A 124.3 . . ?
C59 N16 N17 112.1(4) . . ?
C59 N16 H16 123.9 . . ?
N17 N16 H16 123.9 . . ?
C61 N17 N16 105.3(4) . . ?
C62 N18 C66 117.0(5) . . ?
N1 C1 C2 122.7(5) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.9(5) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 118.0(5) . . ?
C2 C3 H3A 121.0 . . ?
C4 C3 H3A 121.0 . . ?
C5 C4 C3 119.4(5) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 123.2(5) . . ?
N1 C5 C6 112.4(4) . . ?
C4 C5 C6 124.3(5) . . ?
N2 C6 C7 110.8(4) . . ?
N2 C6 C5 115.3(4) . . ?
C7 C6 C5 133.8(5) . . ?
C8 C7 C6 105.1(5) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 107.6(4) . . ?
N3 C8 C9 122.4(4) . . ?
C7 C8 C9 130.0(5) . . ?
C14 C9 C10 119.6(4) . . ?
C14 C9 C8 121.8(5) . . ?
C10 C9 C8 118.6(5) . . ?
C11 C10 C9 118.5(5) . . ?
C11 C10 H10A 120.7 . . ?
C9 C10 H10A 120.7 . . ?
C12 C11 C10 121.9(5) . . ?
C12 C11 H11A 119.0 . . ?
C10 C11 H11A 119.0 . . ?
C11 C12 C13 119.6(5) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
C12 C13 C14 118.8(5) . . ?
C12 C13 C15 120.1(5) . . ?
C14 C13 C15 121.1(5) . . ?
C9 C14 C13 121.5(5) . . ?
C9 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
N4 C15 C16 105.1(5) . . ?
N4 C15 C13 122.1(4) . . ?
C16 C15 C13 132.8(5) . . ?
C15 C16 C17 106.4(5) . . ?
C15 C16 H16A 126.8 . . ?
C17 C16 H16A 126.8 . . ?
N5 C17 C16 110.4(4) . . ?
N5 C17 C18 119.6(5) . . ?
C16 C17 C18 130.0(5) . . ?
N6 C18 C19 122.0(5) . . ?
N6 C18 C17 116.5(5) . . ?
C19 C18 C17 121.5(5) . . ?
C18 C19 C20 119.2(6) . . ?
C18 C19 H19A 120.4 . . ?
C20 C19 H19A 120.4 . . ?
C21 C20 C19 118.1(6) . . ?
C21 C20 H20A 121.0 . . ?
C19 C20 H20A 121.0 . . ?
C20 C21 C22 120.3(6) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
N6 C22 C21 122.4(7) . . ?
N6 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
N7 C23 C24 122.6(5) . . ?
N7 C23 H23A 118.7 . . ?
C24 C23 H23A 118.7 . . ?
C25 C24 C23 119.4(5) . . ?
C25 C24 H24A 120.3 . . ?
C23 C24 H24A 120.3 . . ?
C26 C25 C24 118.4(5) . . ?
C26 C25 H25A 120.8 . . ?
C24 C25 H25A 120.8 . . ?
C27 C26 C25 119.0(5) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
N7 C27 C26 123.1(5) . . ?
N7 C27 C28 113.6(5) . . ?
C26 C27 C28 123.3(5) . . ?
N8 C28 C29 110.4(5) . . ?
N8 C28 C27 115.3(5) . . ?
C29 C28 C27 134.3(5) . . ?
C30 C29 C28 105.3(5) . . ?
C30 C29 H29A 127.3 . . ?
C28 C29 H29A 127.3 . . ?
N9 C30 C29 107.2(4) . . ?
N9 C30 C31 123.9(5) . . ?
C29 C30 C31 128.8(5) . . ?
C36 C31 C32 117.8(5) . . ?
C36 C31 C30 121.8(5) . . ?
C32 C31 C30 120.4(5) . . ?
C33 C32 C31 120.9(5) . . ?
C33 C32 H32A 119.6 . . ?
C31 C32 H32A 119.6 . . ?
C32 C33 C34 120.3(5) . . ?
C32 C33 H33A 119.9 . . ?
C34 C33 H33A 119.9 . . ?
C33 C34 C35 120.3(5) . . ?
C33 C34 H34A 119.9 . . ?
C35 C34 H34A 119.9 . . ?
C36 C35 C34 119.5(5) . . ?
C36 C35 C37 119.8(5) . . ?
C34 C35 C37 120.7(5) . . ?
C35 C36 C31 121.2(5) . . ?
C35 C36 H36A 119.4 . . ?
C31 C36 H36A 119.4 . . ?
N10 C37 C38 104.2(5) . . ?
N10 C37 C35 123.4(5) . . ?
C38 C37 C35 132.4(5) . . ?
C37 C38 C39 106.7(5) . . ?
C37 C38 H38A 126.7 . . ?
C39 C38 H38A 126.7 . . ?
N11 C39 C38 110.5(5) . . ?
N11 C39 C40 120.5(5) . . ?
C38 C39 C40 128.9(5) . . ?
N12 C40 C41 123.2(5) . . ?
N12 C40 C39 117.1(5) . . ?
C41 C40 C39 119.7(5) . . ?
C42 C41 C40 118.2(6) . . ?
C42 C41 H41A 120.9 . . ?
C40 C41 H41A 120.9 . . ?
C43 C42 C41 120.0(6) . . ?
C43 C42 H42A 120.0 . . ?
C41 C42 H42A 120.0 . . ?
C42 C43 C44 117.8(6) . . ?
C42 C43 H43A 121.1 . . ?
C44 C43 H43A 121.1 . . ?
N12 C44 C43 123.5(6) . . ?
N12 C44 H44A 118.3 . . ?
C43 C44 H44A 118.3 . . ?
N13 C45 C46 121.1(5) . . ?
N13 C45 H45A 119.4 . . ?
C46 C45 H45A 119.4 . . ?
C47 C46 C45 120.4(5) . . ?
C47 C46 H46A 119.8 . . ?
C45 C46 H46A 119.8 . . ?
C46 C47 C48 118.8(5) . . ?
C46 C47 H47A 120.6 . . ?
C48 C47 H47A 120.6 . . ?
C47 C48 C49 118.4(6) . . ?
C47 C48 H48A 120.8 . . ?
C49 C48 H48A 120.8 . . ?
N13 C49 C48 123.0(5) . . ?
N13 C49 C50 112.9(4) . . ?
C48 C49 C50 124.1(5) . . ?
N14 C50 C51 110.9(4) . . ?
N14 C50 C49 115.7(4) . . ?
C51 C50 C49 133.4(5) . . ?
C52 C51 C50 105.4(4) . . ?
C52 C51 H51A 127.3 . . ?
C50 C51 H51A 127.3 . . ?
N15 C52 C51 106.4(4) . . ?
N15 C52 C53 123.8(4) . . ?
C51 C52 C53 129.8(5) . . ?
C54 C53 C58 118.3(5) . . ?
C54 C53 C52 119.8(5) . . ?
C58 C53 C52 121.9(5) . . ?
C55 C54 C53 120.1(5) . . ?
C55 C54 H54A 119.9 . . ?
C53 C54 H54A 119.9 . . ?
C56 C55 C54 121.3(5) . . ?
C56 C55 H55A 119.4 . . ?
C54 C55 H55A 119.4 . . ?
C55 C56 C57 120.0(5) . . ?
C55 C56 H56A 120.0 . . ?
C57 C56 H56A 120.0 . . ?
C58 C57 C56 118.7(5) . . ?
C58 C57 C59 121.3(5) . . ?
C56 C57 C59 120.0(5) . . ?
C57 C58 C53 121.6(5) . . ?
C57 C58 H58A 119.2 . . ?
C53 C58 H58A 119.2 . . ?
N16 C59 C60 106.7(4) . . ?
N16 C59 C57 122.6(4) . . ?
C60 C59 C57 130.6(5) . . ?
C59 C60 C61 105.2(5) . . ?
C59 C60 H60A 127.4 . . ?
C61 C60 H60A 127.4 . . ?
N17 C61 C60 110.6(4) . . ?
N17 C61 C62 121.8(5) . . ?
C60 C61 C62 127.6(5) . . ?
N18 C62 C63 122.1(5) . . ?
N18 C62 C61 115.7(5) . . ?
C63 C62 C61 122.2(5) . . ?
C62 C63 C64 119.4(7) . . ?
C62 C63 H63A 120.3 . . ?
C64 C63 H63A 120.3 . . ?
C65 C64 C63 119.0(7) . . ?
C65 C64 H64A 120.5 . . ?
C63 C64 H64A 120.5 . . ?
C64 C65 C66 118.9(6) . . ?
C64 C65 H65A 120.6 . . ?
C66 C65 H65A 120.6 . . ?
N18 C66 C65 123.6(6) . . ?
N18 C66 H66A 118.2 . . ?
C65 C66 H66A 118.2 . . ?
N28 Fe2 N34 96.33(18) . . ?
N28 Fe2 N22 96.11(18) . . ?
N34 Fe2 N22 95.26(18) . . ?
N28 Fe2 N21 91.71(18) . . ?
N34 Fe2 N21 171.20(19) . . ?
N22 Fe2 N21 80.28(18) . . ?
N28 Fe2 N27 80.34(18) . . ?
N34 Fe2 N27 91.67(18) . . ?
N22 Fe2 N27 172.53(18) . . ?
N21 Fe2 N27 93.20(18) . . ?
N28 Fe2 N33 172.73(18) . . ?
N34 Fe2 N33 80.08(17) . . ?
N22 Fe2 N33 90.54(17) . . ?
N21 Fe2 N33 92.31(17) . . ?
N27 Fe2 N33 93.38(18) . . ?
C71 N21 C75 116.6(5) . . ?
C71 N21 Fe2 127.8(4) . . ?
C75 N21 Fe2 115.6(3) . . ?
C76 N22 N23 105.8(4) . . ?
C76 N22 Fe2 115.7(3) . . ?
N23 N22 Fe2 138.6(3) . . ?
N22 N23 C78 111.3(4) . . ?
N22 N23 H23B 124.3 . . ?
C78 N23 H23B 124.3 . . ?
N25 N24 C85 113.1(4) . . ?
N25 N24 H24 123.5 . . ?
C85 N24 H24 123.5 . . ?
C87 N25 N24 104.1(4) . . ?
C88 N26 C92 116.9(5) . . ?
C93 N27 C97 117.0(5) . . ?
C93 N27 Fe2 128.0(4) . . ?
C97 N27 Fe2 115.0(3) . . ?
N29 N28 C98 106.2(4) . . ?
N29 N28 Fe2 137.3(4) . . ?
C98 N28 Fe2 116.4(3) . . ?
N28 N29 C100 111.0(4) . . ?
N28 N29 H29 124.5 . . ?
C100 N29 H29 124.5 . . ?
N31 N30 C107 113.2(4) . . ?
N31 N30 H30 123.4 . . ?
C107 N30 H30 123.4 . . ?
C109 N31 N30 104.1(4) . . ?
C110 N32 C114 116.9(5) . . ?
C115 N33 C119 117.7(4) . . ?
C115 N33 Fe2 127.2(4) . . ?
C119 N33 Fe2 115.1(3) . . ?
C120 N34 N35 106.5(4) . . ?
C120 N34 Fe2 116.5(3) . . ?
N35 N34 Fe2 137.0(3) . . ?
C122 N35 N34 110.1(4) . . ?
C122 N35 H35 124.9 . . ?
N34 N35 H35 124.9 . . ?
N37 N36 C129 112.8(4) . . ?
N37 N36 H36B 123.6 . . ?
C129 N36 H36B 123.6 . . ?
N36 N37 C131 104.8(4) . . ?
C136 N38 C132 116.5(5) . . ?
N21 C71 C72 123.9(6) . . ?
N21 C71 H71A 118.0 . . ?
C72 C71 H71A 118.0 . . ?
C73 C72 C71 118.5(6) . . ?
C73 C72 H72A 120.7 . . ?
C71 C72 H72A 120.7 . . ?
C72 C73 C74 119.5(6) . . ?
C72 C73 H73A 120.2 . . ?
C74 C73 H73A 120.2 . . ?
C73 C74 C75 117.8(6) . . ?
C73 C74 H74A 121.1 . . ?
C75 C74 H74A 121.1 . . ?
N21 C75 C74 123.5(5) . . ?
N21 C75 C76 113.0(4) . . ?
C74 C75 C76 123.5(5) . . ?
N22 C76 C77 110.9(4) . . ?
N22 C76 C75 115.3(5) . . ?
C77 C76 C75 133.8(5) . . ?
C76 C77 C78 105.7(5) . . ?
C76 C77 H77A 127.2 . . ?
C78 C77 H77A 127.2 . . ?
N23 C78 C77 106.3(5) . . ?
N23 C78 C79 123.3(4) . . ?
C77 C78 C79 130.3(5) . . ?
C84 C79 C80 118.6(5) . . ?
C84 C79 C78 121.8(5) . . ?
C80 C79 C78 119.6(5) . . ?
C81 C80 C79 120.5(5) . . ?
C81 C80 H80A 119.8 . . ?
C79 C80 H80A 119.8 . . ?
C80 C81 C82 120.3(5) . . ?
C80 C81 H81A 119.8 . . ?
C82 C81 H81A 119.8 . . ?
C81 C82 C83 119.7(5) . . ?
C81 C82 H82A 120.2 . . ?
C83 C82 H82A 120.2 . . ?
C84 C83 C82 119.6(5) . . ?
C84 C83 C85 120.9(5) . . ?
C82 C83 C85 119.5(5) . . ?
C83 C84 C79 121.4(5) . . ?
C83 C84 H84A 119.3 . . ?
C79 C84 H84A 119.3 . . ?
N24 C85 C86 106.0(4) . . ?
N24 C85 C83 122.1(4) . . ?
C86 C85 C83 132.0(5) . . ?
C85 C86 C87 105.6(5) . . ?
C85 C86 H86A 127.2 . . ?
C87 C86 H86A 127.2 . . ?
N25 C87 C86 111.2(5) . . ?
N25 C87 C88 120.0(5) . . ?
C86 C87 C88 128.8(5) . . ?
N26 C88 C89 123.1(5) . . ?
N26 C88 C87 116.4(5) . . ?
C89 C88 C87 120.5(5) . . ?
C88 C89 C90 118.4(6) . . ?
C88 C89 H89A 120.8 . . ?
C90 C89 H89A 120.8 . . ?
C91 C90 C89 120.2(6) . . ?
C91 C90 H90A 119.9 . . ?
C89 C90 H90A 119.9 . . ?
C90 C91 C92 119.0(6) . . ?
C90 C91 H91A 120.5 . . ?
C92 C91 H91A 120.5 . . ?
N26 C92 C91 122.4(6) . . ?
N26 C92 H92A 118.8 . . ?
C91 C92 H92A 118.8 . . ?
N27 C93 C94 123.1(6) . . ?
N27 C93 H93A 118.5 . . ?
C94 C93 H93A 118.5 . . ?
C93 C94 C95 120.0(6) . . ?
C93 C94 H94A 120.0 . . ?
C95 C94 H94A 120.0 . . ?
C96 C95 C94 118.6(6) . . ?
C96 C95 H95A 120.7 . . ?
C94 C95 H95A 120.7 . . ?
C95 C96 C97 118.7(6) . . ?
C95 C96 H96A 120.7 . . ?
C97 C96 H96A 120.7 . . ?
N27 C97 C96 122.7(5) . . ?
N27 C97 C98 113.0(5) . . ?
C96 C97 C98 124.3(5) . . ?
N28 C98 C99 110.0(5) . . ?
N28 C98 C97 115.1(5) . . ?
C99 C98 C97 134.9(5) . . ?
C100 C99 C98 105.8(5) . . ?
C100 C99 H99A 127.1 . . ?
C98 C99 H99A 127.1 . . ?
N29 C100 C99 106.9(5) . . ?
N29 C100 C101 122.4(5) . . ?
C99 C100 C101 130.7(5) . . ?
C106 C101 C102 118.4(5) . . ?
C106 C101 C100 121.9(5) . . ?
C102 C101 C100 119.7(5) . . ?
C103 C102 C101 120.1(5) . . ?
C103 C102 H10B 119.9 . . ?
C101 C102 H10B 119.9 . . ?
C102 C103 C104 120.6(5) . . ?
C102 C103 H10C 119.7 . . ?
C104 C103 H10C 119.7 . . ?
C103 C104 C105 120.5(5) . . ?
C103 C104 H10D 119.7 . . ?
C105 C104 H10D 119.7 . . ?
C106 C105 C104 118.3(5) . . ?
C106 C105 C107 122.2(5) . . ?
C104 C105 C107 119.6(5) . . ?
C105 C106 C101 122.1(5) . . ?
C105 C106 H10E 118.9 . . ?
C101 C106 H10E 118.9 . . ?
N30 C107 C108 105.5(5) . . ?
N30 C107 C105 123.2(5) . . ?
C108 C107 C105 131.2(5) . . ?
C107 C108 C109 105.7(5) . . ?
C107 C108 H10F 127.2 . . ?
C109 C108 H10F 127.2 . . ?
N31 C109 C108 111.5(5) . . ?
N31 C109 C110 121.9(5) . . ?
C108 C109 C110 126.6(5) . . ?
N32 C110 C111 122.9(5) . . ?
N32 C110 C109 115.2(5) . . ?
C111 C110 C109 121.9(5) . . ?
C112 C111 C110 118.7(5) . . ?
C112 C111 H11B 120.6 . . ?
C110 C111 H11B 120.6 . . ?
C113 C112 C111 118.6(6) . . ?
C113 C112 H11C 120.7 . . ?
C111 C112 H11C 120.7 . . ?
C112 C113 C114 119.4(6) . . ?
C112 C113 H11D 120.3 . . ?
C114 C113 H11D 120.3 . . ?
N32 C114 C113 123.5(6) . . ?
N32 C114 H11E 118.3 . . ?
C113 C114 H11E 118.3 . . ?
N33 C115 C116 122.5(5) . . ?
N33 C115 H11F 118.8 . . ?
C116 C115 H11F 118.8 . . ?
C115 C116 C117 119.7(5) . . ?
C115 C116 H11G 120.1 . . ?
C117 C116 H11G 120.1 . . ?
C118 C117 C116 118.2(5) . . ?
C118 C117 H11H 120.9 . . ?
C116 C117 H11H 120.9 . . ?
C119 C118 C117 120.1(5) . . ?
C119 C118 H11I 119.9 . . ?
C117 C118 H11I 119.9 . . ?
N33 C119 C118 121.7(5) . . ?
N33 C119 C120 112.9(5) . . ?
C118 C119 C120 125.4(5) . . ?
N34 C120 C121 110.6(4) . . ?
N34 C120 C119 115.4(5) . . ?
C121 C120 C119 134.0(5) . . ?
C122 C121 C120 104.6(5) . . ?
C122 C121 H12B 127.7 . . ?
C120 C121 H12B 127.7 . . ?
N35 C122 C121 108.2(4) . . ?
N35 C122 C123 122.4(5) . . ?
C121 C122 C123 129.4(5) . . ?
C128 C123 C124 119.0(5) . . ?
C128 C123 C122 120.6(5) . . ?
C124 C123 C122 120.4(5) . . ?
C125 C124 C123 120.3(5) . . ?
C125 C124 H12C 119.9 . . ?
C123 C124 H12C 119.9 . . ?
C124 C125 C126 120.6(5) . . ?
C124 C125 H12D 119.7 . . ?
C126 C125 H12D 119.7 . . ?
C127 C126 C125 120.0(5) . . ?
C127 C126 H12E 120.0 . . ?
C125 C126 H12E 120.0 . . ?
C126 C127 C128 119.3(5) . . ?
C126 C127 C129 120.2(5) . . ?
C128 C127 C129 120.5(5) . . ?
C123 C128 C127 120.8(5) . . ?
C123 C128 H12F 119.6 . . ?
C127 C128 H12F 119.6 . . ?
N36 C129 C130 106.3(5) . . ?
N36 C129 C127 121.9(5) . . ?
C130 C129 C127 131.8(5) . . ?
C129 C130 C131 106.0(5) . . ?
C129 C130 H13A 127.0 . . ?
C131 C130 H13A 127.0 . . ?
N37 C131 C130 110.2(4) . . ?
N37 C131 C132 119.9(5) . . ?
C130 C131 C132 130.0(5) . . ?
N38 C132 C133 123.1(5) . . ?
N38 C132 C131 116.0(5) . . ?
C133 C132 C131 120.9(5) . . ?
C132 C133 C134 118.4(6) . . ?
C132 C133 H13B 120.8 . . ?
C134 C133 H13B 120.8 . . ?
C135 C134 C133 118.3(6) . . ?
C135 C134 H13C 120.9 . . ?
C133 C134 H13C 120.9 . . ?
C136 C135 C134 118.8(6) . . ?
C136 C135 H13D 120.6 . . ?
C134 C135 H13D 120.6 . . ?
N38 C136 C135 124.9(6) . . ?
N38 C136 H13E 117.6 . . ?
C135 C136 H13E 117.6 . . ?
Cl4 Fe3 Cl3 108.17(10) . . ?
Cl4 Fe3 Cl5 111.04(12) . . ?
Cl3 Fe3 Cl5 109.43(12) . . ?
Cl4 Fe3 Cl2 107.48(12) . . ?
Cl3 Fe3 Cl2 111.48(9) . . ?
Cl5 Fe3 Cl2 109.24(10) . . ?
Cl8 Fe4 Cl9 113.01(17) . . ?
Cl8 Fe4 Cl6 108.46(14) . . ?
Cl9 Fe4 Cl6 105.84(8) . . ?
Cl8 Fe4 Cl7 107.38(15) . . ?
Cl9 Fe4 Cl7 109.52(10) . . ?
Cl6 Fe4 Cl7 112.72(8) . . ?
Cl7B Fe4B Cl6 112.0(5) . . ?
Cl7B Fe4B Cl8B 111.9(6) . . ?
Cl6 Fe4B Cl8B 110.6(5) . . ?
Cl7B Fe4B Cl9B 108.7(6) . . ?
Cl6 Fe4B Cl9B 107.5(6) . . ?
Cl8B Fe4B Cl9B 105.9(6) . . ?
Cl12 Fe5 Cl10 110.35(8) . . ?
Cl12 Fe5 Cl13 115.20(13) . . ?
Cl10 Fe5 Cl13 107.78(8) . . ?
Cl12 Fe5 Cl11 106.76(8) . . ?
Cl10 Fe5 Cl11 110.10(7) . . ?
Cl13 Fe5 Cl11 106.54(12) . . ?
Cl12 Fe5 Cl14 94.5(3) . . ?
Cl10 Fe5 Cl14 106.7(3) . . ?
Cl11 Fe5 Cl14 126.8(3) . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C3S C2S C7S 118.0(7) . . ?
C3S C2S C1S 122.6(7) . . ?
C7S C2S C1S 119.4(7) . . ?
C2S C3S C4S 121.1(7) . . ?
C2S C3S H3SA 119.4 . . ?
C4S C3S H3SA 119.4 . . ?
C3S C4S C5S 119.8(7) . . ?
C3S C4S H4SA 120.1 . . ?
C5S C4S H4SA 120.1 . . ?
C6S C5S C4S 120.0(7) . . ?
C6S C5S H5SA 120.0 . . ?
C4S C5S H5SA 120.0 . . ?
C5S C6S C7S 120.0(7) . . ?
C5S C6S H6SA 120.0 . . ?
C7S C6S H6SA 120.0 . . ?
C2S C7S C6S 121.0(7) . . ?
C2S C7S H7SA 119.5 . . ?
C6S C7S H7SA 119.5 . . ?
C9S C8S H8SA 109.5 . . ?
C9S C8S H8SB 109.5 . . ?
H8SA C8S H8SB 109.5 . . ?
C9S C8S H8SC 109.5 . . ?
H8SA C8S H8SC 109.5 . . ?
H8SB C8S H8SC 109.5 . . ?
C10S C9S C14S 117.6(8) . . ?
C10S C9S C8S 122.8(8) . . ?
C14S C9S C8S 119.5(8) . . ?
C9S C10S C11S 121.6(9) . . ?
C9S C10S H10G 119.2 . . ?
C11S C10S H10G 119.2 . . ?
C12S C11S C10S 120.0(9) . . ?
C12S C11S H11J 120.0 . . ?
C10S C11S H11J 120.0 . . ?
C11S C12S C13S 120.9(10) . . ?
C11S C12S H12G 119.6 . . ?
C13S C12S H12G 119.6 . . ?
C12S C13S C14S 120.4(9) . . ?
C12S C13S H13F 119.8 . . ?
C14S C13S H13F 119.8 . . ?
C13S C14S C9S 119.5(8) . . ?
C13S C14S H14B 120.2 . . ?
C9S C14S H14B 120.2 . . ?
C16S C15S H15B 109.5 . . ?
C16S C15S H15C 109.5 . . ?
H15B C15S H15C 109.5 . . ?
C16S C15S H15D 109.5 . . ?
H15B C15S H15D 109.5 . . ?
H15C C15S H15D 109.5 . . ?
C17S C16S C21S 117.4(14) . . ?
C17S C16S C15S 121.7(15) . . ?
C21S C16S C15S 120.9(14) . . ?
C16S C17S C18S 120.4(16) . . ?
C16S C17S H17A 119.8 . . ?
C18S C17S H17A 119.8 . . ?
C17S C18S C19S 121.5(16) . . ?
C17S C18S H18A 119.3 . . ?
C19S C18S H18A 119.3 . . ?
C20S C19S C18S 119.0(16) . . ?
C20S C19S H19B 120.5 . . ?
C18S C19S H19B 120.5 . . ?
C19S C20S C21S 119.2(16) . . ?
C19S C20S H20B 120.4 . . ?
C21S C20S H20B 120.4 . . ?
C16S C21S C20S 122.3(15) . . ?
C16S C21S H21B 118.9 . . ?
C20S C21S H21B 118.9 . . ?
C37S C36S C41S 117.4(17) . . ?
C37S C36S C35S 120.6(19) . . ?
C41S C36S C35S 121.6(19) . . ?
C36S C37S C38S 121.1(19) . . ?
C37S C38S C39S 120.3(19) . . ?
C40S C39S C38S 117.9(19) . . ?
C39S C40S C41S 122.2(19) . . ?
C40S C41S C36S 119.9(18) . . ?
C23S C22S H22B 109.5 . . ?
C23S C22S H22C 109.5 . . ?
H22B C22S H22C 109.5 . . ?
C23S C22S H22D 109.5 . . ?
H22B C22S H22D 109.5 . . ?
H22C C22S H22D 109.5 . . ?
C24S C23S C28S 116.3(12) . . ?
C24S C23S C22S 115.7(14) . . ?
C28S C23S C22S 126.8(14) . . ?
C25S C24S C23S 119.8(13) . . ?
C25S C24S H24B 120.1 . . ?
C23S C24S H24B 120.1 . . ?
C24S C25S C26S 123.4(14) . . ?
C24S C25S H25B 118.3 . . ?
C26S C25S H25B 118.3 . . ?
C27S C26S C25S 119.4(14) . . ?
C27S C26S H26B 120.3 . . ?
C25S C26S H26B 120.3 . . ?
C26S C27S C28S 119.5(13) . . ?
C26S C27S H27A 120.3 . . ?
C28S C27S H27A 120.3 . . ?
C23S C28S C27S 121.5(13) . . ?
C23S C28S H28A 119.2 . . ?
C27S C28S H28A 119.2 . . ?
O1S C29S C30S 120.7(9) . . ?
O1S C29S C31S 121.4(9) . . ?
C30S C29S C31S 117.9(9) . . ?
C29S C30S H30A 109.5 . . ?
C29S C30S H30B 109.5 . . ?
H30A C30S H30B 109.5 . . ?
C29S C30S H30C 109.5 . . ?
H30A C30S H30C 109.5 . . ?
H30B C30S H30C 109.5 . . ?
C29S C31S H31A 109.5 . . ?
C29S C31S H31B 109.5 . . ?
H31A C31S H31B 109.5 . . ?
C29S C31S H31C 109.5 . . ?
H31A C31S H31C 109.5 . . ?
H31B C31S H31C 109.5 . . ?
O2S C32S C33S 125.1(11) . . ?
O2S C32S C34S 117.8(11) . . ?
C33S C32S C34S 117.0(11) . . ?
C32S C33S H33B 109.5 . . ?
C32S C33S H33C 109.5 . . ?
H33B C33S H33C 109.5 . . ?
C32S C33S H33D 109.5 . . ?
H33B C33S H33D 109.5 . . ?
H33C C33S H33D 109.5 . . ?
C32S C34S H34B 109.5 . . ?
C32S C34S H34C 109.5 . . ?
H34B C34S H34C 109.5 . . ?
C32S C34S H34D 109.5 . . ?
H34B C34S H34D 109.5 . . ?
H34C C34S H34D 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 N31 0.88 2.06 2.822(6) 144.9 .
N9 H9A N37 0.88 2.02 2.824(6) 151.9 .
N15 H15A N25 0.88 2.05 2.834(6) 147.5 .
N23 H23B N17 0.88 2.06 2.849(6) 149.4 .
N29 H29 N5 0.88 2.00 2.798(6) 150.5 .
N35 H35 N11 0.88 2.01 2.820(6) 153.1 .
N4 H4 Cl1 0.88 2.50 3.351(4) 162.1 .
N10 H10H Cl1 0.88 2.57 3.419(5) 162.7 .
N16 H16 Cl1 0.88 2.55 3.410(5) 164.9 .
N24 H24 Cl1 0.88 2.51 3.359(4) 162.6 .
N30 H30 Cl1 0.88 2.59 3.445(5) 163.5 .
N36 H36B Cl1 0.88 2.53 3.376(5) 161.5 .

_refine_diff_density_max         1.176
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.115

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_md521a2
_database_code_depnum_ccdc_archive 'CCDC 1512926'
_audit_update_record             
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C66 H48 Fe N18), 2(C3 H6 O), 2(C H4 O), 3I, 0.6(I3), 0.8(H O), 1.2(H2 O)'
_chemical_formula_sum            'C140 H119.20 Fe2 I4.80 N36 O6'
_chemical_formula_weight         3126.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
I I -0.3071 2.1212
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.9867(8)
_cell_length_b                   13.4513(5)
_cell_length_c                   40.6047(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.448(2)
_cell_angle_gamma                90
_cell_volume                     13097.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9405
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      29.33

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_F_000             6270
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    1.778
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83698
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         2.127
_diffrn_reflns_theta_max         28.967
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13380
_reflns_number_gt                10068
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. The I3-
 anion (atom site I3 and I4) was refined with a partial
 occupancy that was first refined and then fixed at the
 converged value of 0.6. When refining this anion with
 full occupancy, the Ueq of I3 and I4 have too large values
 and there appear a number of too high residual peaks and
 holes. The missing charge is compensated by the oxygen
 O1 being either an hydroxide (0.4) either a water
 molecule (0.6). This is also supported by the Cl and
 Br analogues that both have one full hydroxide ion
 per pair of Fe complexes. A lattice methanol molecule
 is disordered over two positions with relative
 occupancies xxx:xxx, and was refined with displacement
 parameters restraints. Hydrogens were placed geometrically
 on their carrier atom and refined with a riding model,
 where possible. Hydrogens on the disordered methanol
 molecule are omitted in the structural model. Hydrogens
 on the O1 oxygens were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times
 that of O1, and distance restraints. Their positions
 is supported by their participation with three pyridine
 N acceptor (N6, N12, N18). Their occupancies were
 fixed at 0.6, 0.3 and 0.3 respectively for H1, H2, H3.
 H1 corresponded to a residual Q peak about twice stronger
 H2 and H3, and would thus pertain to both the hydroxide
 and the water forms of of O1. H2 and H3 on the other
 correspond to the two possible positions of the second
 hydrogen of the H2O form of O1.
;

_vrf_PLAT413_md521a2             
;
PROBLEM:  Short Inter XH3 .. XHn     H2SA   ..  H1A     ..       1.94 Ang. 
RESPONSE: This short H H contact involves one of the hydrogens
from the lattice acetone molecule, that were fixed at calculated
positions with AFIX 137. This short contact could be due to an
ill-defined position and/or to some disorder of the lattice
solvent molecule.
;

_vrf_PLAT972_md521a2             
;
PROBLEM:  Check Calcd Residual Density  0.30A From      I1      -3.39 eA-3 
RESPONSE: Refining the I1 site with less electron density,
either considering a partial occupancy or the potential
presence of a Br or Cl from an impurity results in much
poorer R values, as well as the arising of stronger 
residual peaks and holes. Thus, these residual negative
densities close to one of the heavier atom in the
structure may be due to non-ideal absorption corrections.
;

_vrf_PLAT045_md521a2             
;
PROBLEM:  Calculated and Reported Z Differ by ............       2.00 Ratio
RESPONSE: Z was intentionaly fixed to 4 instead of 8
to properly describe the charge balance situation, with
the central I- anion being shared by two Fe complexes,
the I3- anion sitting on a special position and being
partially occupied, with its charge compensated by a
partial hydroxide/water site.
;

_vrf_PLAT041_md521a2             
;
PROBLEM:  Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Hydrogens on the disordered lattice methanol
molecule are omitted in the structural model but included
in the formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0782P)²+317.5933P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13380
_refine_ls_number_parameters     889
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2253
_refine_ls_wR_factor_gt          0.2120
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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
I1 I 0.5000 0.36334(6) 0.2500 0.0376(2) Uani 1 2 d S T P . .
I2 I 0.33470(3) 0.85518(5) 0.45149(2) 0.0431(2) Uani 1 1 d . . . . .
I3 I 0.17025(4) 0.35075(8) 0.45660(2) 0.0381(3) Uani 0.6 1 d . . P . .
I4 I 0.2500 0.2500 0.5000 0.0382(3) Uani 0.6 2 d S . P . .
Fe1 Fe 0.50432(4) 0.36445(7) 0.39121(2) 0.0169(2) Uani 1 1 d . . . . .
N1 N 0.4507(2) 0.2858(5) 0.41756(14) 0.0204(13) Uani 1 1 d . . . . .
N2 N 0.5041(2) 0.2398(5) 0.36616(14) 0.0193(12) Uani 1 1 d . . . . .
N3 N 0.5296(2) 0.2040(4) 0.33958(14) 0.0186(12) Uani 1 1 d . . . . .
H3B H 0.5522 0.2381 0.3271 0.022 Uiso 1 1 calc R U . . .
N4 N 0.5834(3) 0.1783(5) 0.21605(15) 0.0230(13) Uani 1 1 d . . . . .
H4B H 0.5598 0.2134 0.2276 0.028 Uiso 1 1 calc R U . . .
N5 N 0.6075(3) 0.2123(5) 0.18884(15) 0.0238(13) Uani 1 1 d . . . . .
N6 N 0.6872(3) 0.0634(6) 0.13338(16) 0.0322(16) Uani 1 1 d D . . . .
N7 N 0.5696(3) 0.3169(5) 0.41764(14) 0.0218(13) Uani 1 1 d . . . . .
N8 N 0.5637(2) 0.4279(4) 0.36694(14) 0.0187(12) Uani 1 1 d . . . . .
N9 N 0.5686(2) 0.4877(4) 0.34055(14) 0.0184(12) Uani 1 1 d . . . . .
H9A H 0.5404 0.5069 0.3278 0.022 Uiso 1 1 calc R U . . .
N10 N 0.5483(3) 0.5837(5) 0.21691(15) 0.0255(14) Uani 1 1 d . . . . .
H10B H 0.5424 0.5312 0.2293 0.031 Uiso 1 1 calc R U . . .
N11 N 0.5188(3) 0.6040(5) 0.18893(15) 0.0247(14) Uani 1 1 d . . . . .
N12 N 0.5502(3) 0.7986(5) 0.13095(17) 0.0365(17) Uani 1 1 d . . . . .
N13 N 0.4943(3) 0.4858(4) 0.41865(14) 0.0206(13) Uani 1 1 d . . . . .
N14 N 0.4425(2) 0.4257(4) 0.36668(14) 0.0175(12) Uani 1 1 d . . . . .
N15 N 0.4108(2) 0.4046(4) 0.33981(14) 0.0182(12) Uani 1 1 d . . . . .
H15A H 0.4159 0.3535 0.3267 0.022 Uiso 1 1 calc R U . . .
N16 N 0.3667(3) 0.3311(5) 0.21651(15) 0.0245(14) Uani 1 1 d . . . . .
H16B H 0.3959 0.3510 0.2283 0.029 Uiso 1 1 calc R U . . .
N17 N 0.3702(3) 0.2739(5) 0.18894(15) 0.0236(13) Uani 1 1 d . . . . .
N18 N 0.2562(3) 0.2161(6) 0.13258(17) 0.0326(16) Uani 1 1 d . . . . .
C1 C 0.4242(3) 0.3146(6) 0.44458(18) 0.0235(16) Uani 1 1 d . . . . .
H1A H 0.4284 0.3816 0.4517 0.028 Uiso 1 1 calc R U . . .
C2 C 0.3912(4) 0.2519(6) 0.4626(2) 0.0318(18) Uani 1 1 d . . . . .
H2A H 0.3738 0.2750 0.4819 0.038 Uiso 1 1 calc R U . . .
C3 C 0.3839(4) 0.1561(7) 0.4522(2) 0.0326(19) Uani 1 1 d . . . . .
H3A H 0.3610 0.1123 0.4643 0.039 Uiso 1 1 calc R U . . .
C4 C 0.4098(3) 0.1226(6) 0.42415(19) 0.0274(17) Uani 1 1 d . . . . .
H4A H 0.4054 0.0561 0.4167 0.033 Uiso 1 1 calc R U . . .
C5 C 0.4427(3) 0.1906(6) 0.40735(17) 0.0218(15) Uani 1 1 d . . . . .
C6 C 0.4732(3) 0.1664(5) 0.37811(17) 0.0198(15) Uani 1 1 d . . . . .
C7 C 0.4802(3) 0.0804(5) 0.35896(18) 0.0234(16) Uani 1 1 d . . . . .
H7A H 0.4637 0.0171 0.3622 0.028 Uiso 1 1 calc R U . . .
C8 C 0.5152(3) 0.1066(5) 0.33498(17) 0.0190(14) Uani 1 1 d . . . . .
C9 C 0.5382(3) 0.0464(6) 0.30773(18) 0.0232(16) Uani 1 1 d . . . . .
C10 C 0.5420(4) -0.0543(6) 0.3111(2) 0.0341(19) Uani 1 1 d . . . . .
H10A H 0.5301 -0.0854 0.3307 0.041 Uiso 1 1 calc R U . . .
C11 C 0.5635(4) -0.1115(6) 0.2857(2) 0.042(2) Uani 1 1 d . . . . .
H11A H 0.5655 -0.1817 0.2880 0.050 Uiso 1 1 calc R U . . .
C12 C 0.5818(4) -0.0669(6) 0.2572(2) 0.036(2) Uani 1 1 d . . . . .
H12A H 0.5968 -0.1061 0.2401 0.043 Uiso 1 1 calc R U . . .
C13 C 0.5782(3) 0.0358(6) 0.25376(19) 0.0240(16) Uani 1 1 d . . . . .
C14 C 0.5578(3) 0.0910(6) 0.27936(18) 0.0240(16) Uani 1 1 d . . . . .
H14A H 0.5571 0.1614 0.2776 0.029 Uiso 1 1 calc R U . . .
C15 C 0.5988(3) 0.0851(6) 0.22391(18) 0.0244(16) Uani 1 1 d . . . . .
C16 C 0.6337(3) 0.0548(6) 0.19943(18) 0.0228(15) Uani 1 1 d . . . . .
H16A H 0.6508 -0.0085 0.1973 0.027 Uiso 1 1 calc R U . . .
C17 C 0.6389(3) 0.1362(6) 0.17844(18) 0.0264(16) Uani 1 1 d . . . . .
C18 C 0.6740(3) 0.1485(6) 0.14954(18) 0.0265(16) Uani 1 1 d . . . . .
C19 C 0.6903(4) 0.2404(7) 0.1391(2) 0.036(2) Uani 1 1 d . . . . .
H19A H 0.6794 0.2990 0.1504 0.044 Uiso 1 1 calc R U . . .
C20 C 0.7237(4) 0.2450(8) 0.1112(2) 0.049(3) Uani 1 1 d . . . . .
H20A H 0.7366 0.3074 0.1035 0.059 Uiso 1 1 calc R U . . .
C21 C 0.7375(4) 0.1591(8) 0.0952(2) 0.045(2) Uani 1 1 d . . . . .
H21A H 0.7599 0.1616 0.0762 0.054 Uiso 1 1 calc R U . . .
C22 C 0.7191(4) 0.0711(8) 0.1065(2) 0.038(2) Uani 1 1 d . . . . .
H22A H 0.7289 0.0121 0.0951 0.046 Uiso 1 1 calc R U . . .
C23 C 0.5700(3) 0.2556(6) 0.44391(19) 0.0276(17) Uani 1 1 d . . . . .
H23A H 0.5356 0.2284 0.4507 0.033 Uiso 1 1 calc R U . . .
C24 C 0.6184(4) 0.2302(7) 0.4615(2) 0.0339(19) Uani 1 1 d . . . . .
H24A H 0.6167 0.1871 0.4800 0.041 Uiso 1 1 calc R U . . .
C25 C 0.6683(3) 0.2678(7) 0.4521(2) 0.0314(19) Uani 1 1 d . . . . .
H25A H 0.7016 0.2518 0.4641 0.038 Uiso 1 1 calc R U . . .
C26 C 0.6699(3) 0.3296(6) 0.4248(2) 0.0279(17) Uani 1 1 d . . . . .
H26A H 0.7042 0.3560 0.4176 0.034 Uiso 1 1 calc R U . . .
C27 C 0.6200(3) 0.3521(6) 0.40812(17) 0.0219(15) Uani 1 1 d . . . . .
C28 C 0.6160(3) 0.4160(5) 0.37935(17) 0.0187(14) Uani 1 1 d . . . . .
C29 C 0.6539(3) 0.4688(6) 0.36077(17) 0.0222(15) Uani 1 1 d . . . . .
H29A H 0.6932 0.4728 0.3642 0.027 Uiso 1 1 calc R U . . .
C30 C 0.6219(3) 0.5143(5) 0.33615(18) 0.0208(15) Uani 1 1 d . . . . .
C31 C 0.6390(3) 0.5798(6) 0.30897(18) 0.0231(15) Uani 1 1 d . . . . .
C32 C 0.6892(3) 0.6321(7) 0.3118(2) 0.0324(18) Uani 1 1 d . . . . .
H32A H 0.7120 0.6269 0.3312 0.039 Uiso 1 1 calc R U . . .
C33 C 0.7052(3) 0.6915(7) 0.2859(2) 0.0335(19) Uani 1 1 d . . . . .
H33A H 0.7388 0.7285 0.2880 0.040 Uiso 1 1 calc R U . . .
C34 C 0.6732(3) 0.6983(7) 0.2570(2) 0.0312(18) Uani 1 1 d . . . . .
H34A H 0.6854 0.7384 0.2393 0.037 Uiso 1 1 calc R U . . .
C35 C 0.6232(3) 0.6463(6) 0.25402(18) 0.0249(16) Uani 1 1 d . . . . .
C36 C 0.6071(3) 0.5866(5) 0.28015(17) 0.0206(15) Uani 1 1 d . . . . .
H36A H 0.5735 0.5497 0.2782 0.025 Uiso 1 1 calc R U . . .
C37 C 0.5883(3) 0.6529(6) 0.22399(18) 0.0218(15) Uani 1 1 d . . . . .
C38 C 0.5848(3) 0.7220(6) 0.19861(18) 0.0275(17) Uani 1 1 d . . . . .
H38A H 0.6071 0.7795 0.1958 0.033 Uiso 1 1 calc R U . . .
C39 C 0.5408(3) 0.6880(6) 0.17799(18) 0.0255(16) Uani 1 1 d . . . . .
C40 C 0.5171(4) 0.7350(6) 0.14801(18) 0.0264(17) Uani 1 1 d . . . . .
C41 C 0.4631(4) 0.7144(7) 0.1387(2) 0.0341(19) Uani 1 1 d . . . . .
H41A H 0.4413 0.6694 0.1509 0.041 Uiso 1 1 calc R U . . .
C42 C 0.4417(4) 0.7601(8) 0.1114(2) 0.048(3) Uani 1 1 d . . . . .
H42A H 0.4041 0.7481 0.1048 0.057 Uiso 1 1 calc R U . . .
C43 C 0.4734(5) 0.8228(8) 0.0934(2) 0.051(3) Uani 1 1 d . . . . .
H43A H 0.4582 0.8531 0.0740 0.061 Uiso 1 1 calc R U . . .
C44 C 0.5260(5) 0.8417(7) 0.1030(2) 0.045(2) Uani 1 1 d . . . . .
H44A H 0.5476 0.8860 0.0904 0.054 Uiso 1 1 calc R U . . .
C45 C 0.5246(3) 0.5127(6) 0.44558(18) 0.0244(16) Uani 1 1 d . . . . .
H45A H 0.5567 0.4749 0.4518 0.029 Uiso 1 1 calc R U . . .
C46 C 0.5100(4) 0.5946(7) 0.46458(19) 0.0327(19) Uani 1 1 d . . . . .
H46A H 0.5315 0.6114 0.4837 0.039 Uiso 1 1 calc R U . . .
C47 C 0.4650(4) 0.6501(6) 0.4556(2) 0.0335(19) Uani 1 1 d . . . . .
H47A H 0.4545 0.7057 0.4685 0.040 Uiso 1 1 calc R U . . .
C48 C 0.4341(3) 0.6249(6) 0.42735(19) 0.0255(16) Uani 1 1 d . . . . .
H48A H 0.4025 0.6630 0.4206 0.031 Uiso 1 1 calc R U . . .
C49 C 0.4503(3) 0.5437(5) 0.40927(17) 0.0204(15) Uani 1 1 d . . . . .
C50 C 0.4216(3) 0.5079(5) 0.37968(17) 0.0189(14) Uani 1 1 d . . . . .
C51 C 0.3752(3) 0.5416(5) 0.36103(17) 0.0206(15) Uani 1 1 d . . . . .
H51A H 0.3528 0.5984 0.3649 0.025 Uiso 1 1 calc R U . . .
C52 C 0.3696(3) 0.4733(5) 0.33572(17) 0.0196(15) Uani 1 1 d . . . . .
C53 C 0.3280(3) 0.4678(5) 0.30838(18) 0.0193(14) Uani 1 1 d . . . . .
C54 C 0.2761(3) 0.5124(6) 0.3113(2) 0.0305(18) Uani 1 1 d . . . . .
H54A H 0.2674 0.5467 0.3310 0.037 Uiso 1 1 calc R U . . .
C55 C 0.2367(4) 0.5070(7) 0.2855(2) 0.036(2) Uani 1 1 d . . . . .
H55A H 0.2013 0.5381 0.2875 0.043 Uiso 1 1 calc R U . . .
C56 C 0.2493(3) 0.4561(6) 0.25699(19) 0.0304(18) Uani 1 1 d . . . . .
H56A H 0.2224 0.4525 0.2395 0.036 Uiso 1 1 calc R U . . .
C57 C 0.3004(3) 0.4105(6) 0.25362(17) 0.0207(15) Uani 1 1 d . . . . .
C58 C 0.3397(3) 0.4160(5) 0.27953(17) 0.0197(15) Uani 1 1 d . . . . .
H58A H 0.3749 0.3843 0.2775 0.024 Uiso 1 1 calc R U . . .
C59 C 0.3138(3) 0.3539(6) 0.22377(17) 0.0226(15) Uani 1 1 d . . . . .
C60 C 0.2808(3) 0.3111(6) 0.19909(18) 0.0226(15) Uani 1 1 d . . . . .
H60A H 0.2413 0.3148 0.1967 0.027 Uiso 1 1 calc R U . . .
C61 C 0.3170(3) 0.2619(6) 0.17862(18) 0.0229(15) Uani 1 1 d . . . . .
C62 C 0.3044(3) 0.1996(6) 0.14940(17) 0.0244(16) Uani 1 1 d . . . . .
C63 C 0.3411(4) 0.1245(6) 0.1417(2) 0.0328(19) Uani 1 1 d . . . . .
H63A H 0.3746 0.1144 0.1543 0.039 Uiso 1 1 calc R U . . .
C64 C 0.3274(5) 0.0652(9) 0.1153(3) 0.058(3) Uani 1 1 d . . . . .
H64A H 0.3519 0.0132 0.1092 0.069 Uiso 1 1 calc R U . . .
C65 C 0.2786(5) 0.0802(8) 0.0975(2) 0.051(3) Uani 1 1 d . . . . .
H65A H 0.2688 0.0382 0.0794 0.062 Uiso 1 1 calc R U . . .
C66 C 0.2446(4) 0.1569(8) 0.1062(2) 0.043(2) Uani 1 1 d . . . . .
H66A H 0.2116 0.1691 0.0934 0.052 Uiso 1 1 calc R U . . .
O1 O 0.6672(3) -0.1419(5) 0.15562(16) 0.0435(15) Uani 1 1 d D . . . .
H1 H 0.670(5) -0.087(4) 0.1431(18) 0.065 Uiso 1 1 d D U . . .
H2 H 0.637(5) -0.16(3) 0.144(3) 0.065 Uiso 0.3 1 d D U P . .
H3 H 0.686(9) -0.18(2) 0.142(3) 0.065 Uiso 0.3 1 d D U P . .
C1S C 0.3315(4) 0.5094(9) 0.4820(3) 0.059(3) Uani 1 1 d D . . . .
C2S C 0.3293(5) 0.4871(10) 0.4503(4) 0.075(4) Uani 1 1 d D . . . .
H2SA H 0.3669 0.4717 0.4429 0.112 Uiso 1 1 calc R U . . .
H2SB H 0.3143 0.5437 0.4378 0.112 Uiso 1 1 calc R U . . .
H2SC H 0.3051 0.4291 0.4467 0.112 Uiso 1 1 calc R U . . .
C3S C 0.2859(6) 0.5604(14) 0.4912(4) 0.105(6) Uani 1 1 d D . . . .
H3SA H 0.2823 0.5556 0.5152 0.157 Uiso 1 1 calc R U . . .
H3SB H 0.2526 0.5321 0.4803 0.157 Uiso 1 1 calc R U . . .
H3SC H 0.2897 0.6303 0.4849 0.157 Uiso 1 1 calc R U . . .
O1S O 0.3717(4) 0.4861(8) 0.4982(3) 0.092(3) Uani 1 1 d . . . . .
O2S O 0.4546(6) -0.0475(7) 0.4876(3) 0.047(3) Uani 0.553(14) 1 d D U P A 1
C4S C 0.4994(10) -0.1148(15) 0.4949(5) 0.061(5) Uani 0.553(14) 1 d D U P A 1
O3S O 0.5230(11) 0.0110(16) 0.4694(6) 0.086(5) Uani 0.447(14) 1 d . U P A 2
C5S C 0.5117(11) -0.029(2) 0.4910(8) 0.074(5) Uani 0.447(14) 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I3 I4 2.9037(10) . ?
I4 I3 2.9036(10) 7_556 ?
Fe1 N14 1.948(6) . ?
Fe1 N8 1.949(6) . ?
Fe1 N2 1.961(6) . ?
Fe1 N7 1.981(6) . ?
Fe1 N13 1.994(6) . ?
Fe1 N1 1.997(6) . ?
N1 C1 1.339(9) . ?
N1 C5 1.357(10) . ?
N2 C6 1.332(9) . ?
N2 N3 1.344(8) . ?
N3 C8 1.367(9) . ?
N3 H3B 0.8800 . ?
N4 N5 1.341(9) . ?
N4 C15 1.343(10) . ?
N4 H4B 0.8800 . ?
N5 C17 1.345(10) . ?
N6 C22 1.353(11) . ?
N6 C18 1.362(11) . ?
N7 C23 1.349(10) . ?
N7 C27 1.364(10) . ?
N8 N9 1.347(8) . ?
N8 C28 1.350(9) . ?
N9 C30 1.345(9) . ?
N9 H9A 0.8800 . ?
N10 N11 1.351(9) . ?
N10 C37 1.361(10) . ?
N10 H10B 0.8800 . ?
N11 C39 1.328(10) . ?
N12 C40 1.368(11) . ?
N12 C44 1.387(12) . ?
N13 C45 1.347(9) . ?
N13 C49 1.358(10) . ?
N14 C50 1.329(9) . ?
N14 N15 1.345(8) . ?
N15 C52 1.358(9) . ?
N15 H15A 0.8800 . ?
N16 C59 1.344(10) . ?
N16 N17 1.363(8) . ?
N16 H16B 0.8800 . ?
N17 C61 1.344(10) . ?
N18 C62 1.346(10) . ?
N18 C66 1.358(12) . ?
C1 C2 1.379(11) . ?
C1 H1A 0.9500 . ?
C2 C3 1.365(12) . ?
C2 H2A 0.9500 . ?
C3 C4 1.387(11) . ?
C3 H3A 0.9500 . ?
C4 C5 1.398(11) . ?
C4 H4A 0.9500 . ?
C5 C6 1.447(10) . ?
C6 C7 1.407(10) . ?
C7 C8 1.348(11) . ?
C7 H7A 0.9500 . ?
C8 C9 1.488(10) . ?
C9 C10 1.364(11) . ?
C9 C14 1.392(11) . ?
C10 C11 1.396(12) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(12) . ?
C11 H11A 0.9500 . ?
C12 C13 1.391(12) . ?
C12 H12A 0.9500 . ?
C13 C14 1.377(11) . ?
C13 C15 1.477(11) . ?
C14 H14A 0.9500 . ?
C15 C16 1.378(11) . ?
C16 C17 1.395(11) . ?
C16 H16A 0.9500 . ?
C17 C18 1.470(11) . ?
C18 C19 1.366(12) . ?
C19 C20 1.406(13) . ?
C19 H19A 0.9500 . ?
C20 C21 1.371(15) . ?
C20 H20A 0.9500 . ?
C21 C22 1.349(14) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.390(11) . ?
C23 H23A 0.9500 . ?
C24 C25 1.364(12) . ?
C24 H24A 0.9500 . ?
C25 C26 1.386(11) . ?
C25 H25A 0.9500 . ?
C26 C27 1.394(10) . ?
C26 H26A 0.9500 . ?
C27 C28 1.451(10) . ?
C28 C29 1.390(10) . ?
C29 C30 1.387(10) . ?
C29 H29A 0.9500 . ?
C30 C31 1.478(10) . ?
C31 C36 1.384(10) . ?
C31 C32 1.396(11) . ?
C32 C33 1.382(12) . ?
C32 H32A 0.9500 . ?
C33 C34 1.391(12) . ?
C33 H33A 0.9500 . ?
C34 C35 1.390(11) . ?
C34 H34A 0.9500 . ?
C35 C36 1.392(11) . ?
C35 C37 1.465(10) . ?
C36 H36A 0.9500 . ?
C37 C38 1.388(11) . ?
C38 C39 1.406(11) . ?
C38 H38A 0.9500 . ?
C39 C40 1.474(11) . ?
C40 C41 1.367(12) . ?
C41 C42 1.356(13) . ?
C41 H41A 0.9500 . ?
C42 C43 1.361(16) . ?
C42 H42A 0.9500 . ?
C43 C44 1.336(16) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.395(12) . ?
C45 H45A 0.9500 . ?
C46 C47 1.355(13) . ?
C46 H46A 0.9500 . ?
C47 C48 1.392(11) . ?
C47 H47A 0.9500 . ?
C48 C49 1.378(10) . ?
C48 H48A 0.9500 . ?
C49 C50 1.452(10) . ?
C50 C51 1.404(10) . ?
C51 C52 1.382(10) . ?
C51 H51A 0.9500 . ?
C52 C53 1.477(10) . ?
C53 C54 1.390(11) . ?
C53 C58 1.398(10) . ?
C54 C55 1.395(11) . ?
C54 H54A 0.9500 . ?
C55 C56 1.387(12) . ?
C55 H55A 0.9500 . ?
C56 C57 1.381(11) . ?
C56 H56A 0.9500 . ?
C57 C58 1.397(10) . ?
C57 C59 1.474(10) . ?
C58 H58A 0.9500 . ?
C59 C60 1.387(10) . ?
C60 C61 1.386(11) . ?
C60 H60A 0.9500 . ?
C61 C62 1.477(10) . ?
C62 C63 1.381(12) . ?
C63 C64 1.371(14) . ?
C63 H63A 0.9500 . ?
C64 C65 1.376(16) . ?
C64 H64A 0.9500 . ?
C65 C66 1.368(15) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
O1 H1 0.90(2) . ?
O1 H2 0.90(2) . ?
O1 H3 0.90(2) . ?
C1S O1S 1.194(14) . ?
C1S C2S 1.323(14) . ?
C1S C3S 1.353(14) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
O2S C4S 1.43(2) . ?
O3S C5S 1.07(3) . ?
O3S C5S 1.85(4) 5_656 ?
C5S C5S 1.22(6) 5_656 ?
C5S O3S 1.85(4) 5_656 ?

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
I3 I4 I3 180.0 7_556 . ?
N14 Fe1 N8 96.5(2) . . ?
N14 Fe1 N2 96.0(2) . . ?
N8 Fe1 N2 96.0(2) . . ?
N14 Fe1 N7 173.8(3) . . ?
N8 Fe1 N7 80.6(2) . . ?
N2 Fe1 N7 89.8(2) . . ?
N14 Fe1 N13 80.7(2) . . ?
N8 Fe1 N13 91.4(2) . . ?
N2 Fe1 N13 172.2(2) . . ?
N7 Fe1 N13 93.8(3) . . ?
N14 Fe1 N1 90.4(2) . . ?
N8 Fe1 N1 172.6(3) . . ?
N2 Fe1 N1 80.3(2) . . ?
N7 Fe1 N1 92.8(2) . . ?
N13 Fe1 N1 92.6(2) . . ?
C1 N1 C5 117.2(6) . . ?
C1 N1 Fe1 127.6(5) . . ?
C5 N1 Fe1 115.1(5) . . ?
C6 N2 N3 107.2(6) . . ?
C6 N2 Fe1 116.0(5) . . ?
N3 N2 Fe1 136.7(5) . . ?
N2 N3 C8 109.5(6) . . ?
N2 N3 H3B 125.2 . . ?
C8 N3 H3B 125.2 . . ?
N5 N4 C15 113.1(6) . . ?
N5 N4 H4B 123.5 . . ?
C15 N4 H4B 123.5 . . ?
N4 N5 C17 104.9(6) . . ?
C22 N6 C18 117.9(8) . . ?
C23 N7 C27 116.6(6) . . ?
C23 N7 Fe1 128.0(5) . . ?
C27 N7 Fe1 115.4(5) . . ?
N9 N8 C28 105.6(6) . . ?
N9 N8 Fe1 138.0(5) . . ?
C28 N8 Fe1 116.4(5) . . ?
C30 N9 N8 111.5(6) . . ?
C30 N9 H9A 124.2 . . ?
N8 N9 H9A 124.2 . . ?
N11 N10 C37 113.0(6) . . ?
N11 N10 H10B 123.5 . . ?
C37 N10 H10B 123.5 . . ?
C39 N11 N10 104.4(6) . . ?
C40 N12 C44 116.0(8) . . ?
C45 N13 C49 118.2(6) . . ?
C45 N13 Fe1 127.1(5) . . ?
C49 N13 Fe1 114.6(5) . . ?
C50 N14 N15 106.6(6) . . ?
C50 N14 Fe1 116.1(5) . . ?
N15 N14 Fe1 137.2(5) . . ?
N14 N15 C52 110.5(6) . . ?
N14 N15 H15A 124.7 . . ?
C52 N15 H15A 124.7 . . ?
C59 N16 N17 112.8(6) . . ?
C59 N16 H16B 123.6 . . ?
N17 N16 H16B 123.6 . . ?
C61 N17 N16 104.2(6) . . ?
C62 N18 C66 117.4(8) . . ?
N1 C1 C2 123.2(7) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C3 C2 C1 119.1(7) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 120.2(7) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C5 117.3(7) . . ?
C3 C4 H4A 121.4 . . ?
C5 C4 H4A 121.4 . . ?
N1 C5 C4 123.0(7) . . ?
N1 C5 C6 113.1(6) . . ?
C4 C5 C6 123.8(7) . . ?
N2 C6 C7 109.5(6) . . ?
N2 C6 C5 115.4(6) . . ?
C7 C6 C5 135.1(7) . . ?
C8 C7 C6 105.6(6) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
C7 C8 N3 108.2(6) . . ?
C7 C8 C9 130.0(7) . . ?
N3 C8 C9 121.8(6) . . ?
C10 C9 C14 119.2(7) . . ?
C10 C9 C8 119.4(7) . . ?
C14 C9 C8 121.3(7) . . ?
C9 C10 C11 119.9(8) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C12 C11 C10 120.6(8) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 119.5(8) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C14 C13 C12 118.9(7) . . ?
C14 C13 C15 120.7(7) . . ?
C12 C13 C15 120.3(7) . . ?
C13 C14 C9 121.8(7) . . ?
C13 C14 H14A 119.1 . . ?
C9 C14 H14A 119.1 . . ?
N4 C15 C16 105.9(7) . . ?
N4 C15 C13 121.2(7) . . ?
C16 C15 C13 132.9(7) . . ?
C15 C16 C17 105.9(7) . . ?
C15 C16 H16A 127.0 . . ?
C17 C16 H16A 127.0 . . ?
N5 C17 C16 110.2(7) . . ?
N5 C17 C18 120.1(7) . . ?
C16 C17 C18 129.6(7) . . ?
N6 C18 C19 122.7(7) . . ?
N6 C18 C17 115.8(7) . . ?
C19 C18 C17 121.5(8) . . ?
C18 C19 C20 117.6(9) . . ?
C18 C19 H19A 121.2 . . ?
C20 C19 H19A 121.2 . . ?
C21 C20 C19 119.6(9) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C22 C21 C20 119.6(9) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 N6 122.6(9) . . ?
C21 C22 H22A 118.7 . . ?
N6 C22 H22A 118.7 . . ?
N7 C23 C24 123.1(8) . . ?
N7 C23 H23A 118.4 . . ?
C24 C23 H23A 118.4 . . ?
C25 C24 C23 119.5(7) . . ?
C25 C24 H24A 120.3 . . ?
C23 C24 H24A 120.3 . . ?
C24 C25 C26 119.2(7) . . ?
C24 C25 H25A 120.4 . . ?
C26 C25 H25A 120.4 . . ?
C25 C26 C27 118.6(8) . . ?
C25 C26 H26A 120.7 . . ?
C27 C26 H26A 120.7 . . ?
N7 C27 C26 122.9(7) . . ?
N7 C27 C28 113.2(6) . . ?
C26 C27 C28 123.9(7) . . ?
N8 C28 C29 110.6(6) . . ?
N8 C28 C27 114.3(6) . . ?
C29 C28 C27 135.1(7) . . ?
C30 C29 C28 105.1(6) . . ?
C30 C29 H29A 127.5 . . ?
C28 C29 H29A 127.5 . . ?
N9 C30 C29 107.2(6) . . ?
N9 C30 C31 122.7(6) . . ?
C29 C30 C31 130.0(7) . . ?
C36 C31 C32 119.5(7) . . ?
C36 C31 C30 120.9(7) . . ?
C32 C31 C30 119.5(7) . . ?
C33 C32 C31 118.9(8) . . ?
C33 C32 H32A 120.6 . . ?
C31 C32 H32A 120.6 . . ?
C32 C33 C34 121.5(8) . . ?
C32 C33 H33A 119.2 . . ?
C34 C33 H33A 119.2 . . ?
C35 C34 C33 119.8(7) . . ?
C35 C34 H34A 120.1 . . ?
C33 C34 H34A 120.1 . . ?
C34 C35 C36 118.5(7) . . ?
C34 C35 C37 121.0(7) . . ?
C36 C35 C37 120.4(7) . . ?
C31 C36 C35 121.7(7) . . ?
C31 C36 H36A 119.2 . . ?
C35 C36 H36A 119.2 . . ?
N10 C37 C38 105.8(7) . . ?
N10 C37 C35 121.2(7) . . ?
C38 C37 C35 133.0(7) . . ?
C37 C38 C39 104.8(7) . . ?
C37 C38 H38A 127.6 . . ?
C39 C38 H38A 127.6 . . ?
N11 C39 C38 112.0(7) . . ?
N11 C39 C40 119.5(7) . . ?
C38 C39 C40 128.4(8) . . ?
C41 C40 N12 123.0(8) . . ?
C41 C40 C39 119.0(7) . . ?
N12 C40 C39 117.9(7) . . ?
C42 C41 C40 118.0(9) . . ?
C42 C41 H41A 121.0 . . ?
C40 C41 H41A 121.0 . . ?
C41 C42 C43 121.0(9) . . ?
C41 C42 H42A 119.5 . . ?
C43 C42 H42A 119.5 . . ?
C44 C43 C42 119.8(9) . . ?
C44 C43 H43A 120.1 . . ?
C42 C43 H43A 120.1 . . ?
C43 C44 N12 122.2(9) . . ?
C43 C44 H44A 118.9 . . ?
N12 C44 H44A 118.9 . . ?
N13 C45 C46 121.5(7) . . ?
N13 C45 H45A 119.3 . . ?
C46 C45 H45A 119.3 . . ?
C47 C46 C45 119.8(7) . . ?
C47 C46 H46A 120.1 . . ?
C45 C46 H46A 120.1 . . ?
C46 C47 C48 119.4(8) . . ?
C46 C47 H47A 120.3 . . ?
C48 C47 H47A 120.3 . . ?
C49 C48 C47 118.8(8) . . ?
C49 C48 H48A 120.6 . . ?
C47 C48 H48A 120.6 . . ?
N13 C49 C48 122.2(7) . . ?
N13 C49 C50 113.0(6) . . ?
C48 C49 C50 124.7(7) . . ?
N14 C50 C51 110.9(6) . . ?
N14 C50 C49 115.4(6) . . ?
C51 C50 C49 133.8(7) . . ?
C52 C51 C50 104.3(6) . . ?
C52 C51 H51A 127.8 . . ?
C50 C51 H51A 127.8 . . ?
N15 C52 C51 107.7(6) . . ?
N15 C52 C53 122.3(6) . . ?
C51 C52 C53 130.0(7) . . ?
C54 C53 C58 119.2(7) . . ?
C54 C53 C52 120.3(7) . . ?
C58 C53 C52 120.5(6) . . ?
C53 C54 C55 120.3(7) . . ?
C53 C54 H54A 119.9 . . ?
C55 C54 H54A 119.9 . . ?
C56 C55 C54 119.7(8) . . ?
C56 C55 H55A 120.2 . . ?
C54 C55 H55A 120.2 . . ?
C57 C56 C55 121.1(7) . . ?
C57 C56 H56A 119.5 . . ?
C55 C56 H56A 119.5 . . ?
C56 C57 C58 119.1(7) . . ?
C56 C57 C59 121.6(7) . . ?
C58 C57 C59 119.3(7) . . ?
C57 C58 C53 120.7(7) . . ?
C57 C58 H58A 119.6 . . ?
C53 C58 H58A 119.6 . . ?
N16 C59 C60 105.8(6) . . ?
N16 C59 C57 121.6(6) . . ?
C60 C59 C57 132.5(7) . . ?
C61 C60 C59 106.0(7) . . ?
C61 C60 H60A 127.0 . . ?
C59 C60 H60A 127.0 . . ?
N17 C61 C60 111.1(7) . . ?
N17 C61 C62 119.5(7) . . ?
C60 C61 C62 129.3(7) . . ?
N18 C62 C63 123.4(7) . . ?
N18 C62 C61 118.0(7) . . ?
C63 C62 C61 118.4(7) . . ?
C64 C63 C62 117.4(8) . . ?
C64 C63 H63A 121.3 . . ?
C62 C63 H63A 121.3 . . ?
C63 C64 C65 120.7(10) . . ?
C63 C64 H64A 119.7 . . ?
C65 C64 H64A 119.7 . . ?
C66 C65 C64 118.7(9) . . ?
C66 C65 H65A 120.6 . . ?
C64 C65 H65A 120.6 . . ?
N18 C66 C65 122.3(9) . . ?
N18 C66 H66A 118.8 . . ?
C65 C66 H66A 118.8 . . ?
H1 O1 H2 89(10) . . ?
H1 O1 H3 96(10) . . ?
H2 O1 H3 86(10) . . ?
O1S C1S C2S 119.3(11) . . ?
O1S C1S C3S 128.9(13) . . ?
C2S C1S C3S 111.8(12) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4B I1 0.88 2.65 3.498(6) 162.1 .
N10 H10B I1 0.88 2.62 3.467(7) 160.6 .
N16 H16B I1 0.88 2.63 3.471(6) 159.4 .
O1 H1 N6 0.90(2) 2.11(3) 2.948(10) 155(7) .
O1 H2 N12 0.90(2) 2.19(4) 3.061(11) 162(13) 1_545
O1 H3 N18 0.90(2) 2.21(4) 3.030(10) 150(8) 3_545

_refine_diff_density_max         1.387
_refine_diff_density_min         -3.425
_refine_diff_density_rms         0.172

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_md422k_a
_database_code_depnum_ccdc_archive 'CCDC 1512927'
_audit_update_record             
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C66 H48 Fe N18), 2(F6 P), Br, (H2 O), (H O)'
_chemical_formula_sum            'C132 H99 Br F12 Fe2 N36 O2 P2'
_chemical_formula_weight         2703.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1183 0.1134
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Br Br -0.7406 2.7887
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   13.5619(5)
_cell_length_b                   13.5619(5)
_cell_length_c                   37.307(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5942.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      31.12

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_F_000             2768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.867
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            86965
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.234
_diffrn_reflns_theta_max         31.183
_diffrn_reflns_theta_full        31.100
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4960
_reflns_number_gt                4203
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. The F sites
 of the PF6 anion, F1 and F2, were refined with displacement
 parameters restraints. Hydrogens were placed geometrically on
 their carrier atom and refined with a riding model, except that
 on O1, that was found in a difference Fourier map and refined
 with its thermal parameter 1.5 times that of O1 and a soft 
 distance restraint. Its occupancy was fixed at 1/2, as for
 charge balance it should be either an hydroxide ion or
 a water molecule. Indeed, by symmetry the H1 site forms 
 three hydrogen bonds with either of three N acceptor from
 three neighboring pyridines (N6). The formula thus has
 one hydroxide ion and one water molecule, sharing the same
 position.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0630P)²+14.9133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4960
_refine_ls_number_parameters     285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1725
_refine_ls_wR_factor_gt          0.1644
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_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
Br1 Br 1.0000 1.0000 0.7500 0.0435(3) Uani 1 6 d S T P . .
Fe1 Fe 1.0000 1.0000 0.90262(2) 0.01799(17) Uani 1 3 d S T P . .
N1 N 0.8673(2) 0.9820(2) 0.93089(6) 0.0211(5) Uani 1 1 d . . . . .
N2 N 0.8770(2) 0.87646(19) 0.87596(6) 0.0184(5) Uani 1 1 d . . . . .
N3 N 0.8670(2) 0.81287(19) 0.84711(6) 0.0192(5) Uani 1 1 d . . . . .
H3 H 0.9241 0.8231 0.8333 0.029 Uiso 1 1 calc R U . . .
N4 N 0.9043(2) 0.7340(2) 0.71294(6) 0.0218(5) Uani 1 1 d . . . . .
H4 H 0.9160 0.7932 0.7259 0.033 Uiso 1 1 calc R U . . .
N5 N 0.9629(2) 0.7407(2) 0.68298(6) 0.0230(5) Uani 1 1 d . . . . .
N6 N 0.9002(3) 0.5097(3) 0.62207(7) 0.0368(7) Uani 1 1 d . . . . .
C1 C 0.8686(3) 1.0476(3) 0.95809(7) 0.0242(6) Uani 1 1 d . . . . .
H1A H 0.9395 1.1101 0.9654 0.029 Uiso 1 1 calc R U . . .
C2 C 0.7710(3) 1.0277(3) 0.97591(8) 0.0283(6) Uani 1 1 d . . . . .
H2A H 0.7752 1.0774 0.9945 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6672(3) 0.9353(3) 0.96650(8) 0.0292(6) Uani 1 1 d . . . . .
H3A H 0.5998 0.9188 0.9791 0.035 Uiso 1 1 calc R U . . .
C4 C 0.6640(3) 0.8672(3) 0.93825(8) 0.0250(6) Uani 1 1 d . . . . .
H4A H 0.5942 0.8028 0.9312 0.030 Uiso 1 1 calc R U . . .
C5 C 0.7644(2) 0.8946(2) 0.92057(7) 0.0204(5) Uani 1 1 d . . . . .
C6 C 0.7718(2) 0.8347(2) 0.88940(7) 0.0196(5) Uani 1 1 d . . . . .
C7 C 0.6930(2) 0.7427(2) 0.86875(7) 0.0215(5) Uani 1 1 d . . . . .
H7A H 0.6130 0.6982 0.8723 0.026 Uiso 1 1 calc R U . . .
C8 C 0.7571(2) 0.7307(2) 0.84209(7) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.7227(2) 0.6487(2) 0.81253(7) 0.0207(5) Uani 1 1 d . . . . .
C10 C 0.6247(3) 0.5420(3) 0.81579(8) 0.0277(6) Uani 1 1 d . . . . .
H10A H 0.5806 0.5229 0.8371 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5918(3) 0.4641(3) 0.78809(9) 0.0327(7) Uani 1 1 d . . . . .
H11A H 0.5249 0.3918 0.7904 0.039 Uiso 1 1 calc R U . . .
C12 C 0.6559(3) 0.4909(3) 0.75686(8) 0.0287(6) Uani 1 1 d . . . . .
H12A H 0.6326 0.4371 0.7379 0.034 Uiso 1 1 calc R U . . .
C13 C 0.7545(2) 0.5968(2) 0.75330(7) 0.0208(5) Uani 1 1 d . . . . .
C14 C 0.7863(2) 0.6749(2) 0.78132(7) 0.0202(5) Uani 1 1 d . . . . .
H14A H 0.8529 0.7474 0.7790 0.024 Uiso 1 1 calc R U . . .
C15 C 0.8255(2) 0.6255(2) 0.72068(7) 0.0203(5) Uani 1 1 d . . . . .
C16 C 0.8317(3) 0.5580(2) 0.69415(7) 0.0224(6) Uani 1 1 d . . . . .
H16A H 0.7861 0.4778 0.6917 0.027 Uiso 1 1 calc R U . . .
C17 C 0.9200(2) 0.6335(2) 0.67152(7) 0.0222(6) Uani 1 1 d . . . . .
C18 C 0.9683(3) 0.6088(3) 0.63965(8) 0.0262(6) Uani 1 1 d . . . . .
C19 C 1.0790(3) 0.6843(3) 0.62955(9) 0.0360(8) Uani 1 1 d . . . . .
H19A H 1.1241 0.7537 0.6421 0.043 Uiso 1 1 calc R U . . .
C20 C 1.1214(4) 0.6543(5) 0.60018(12) 0.0560(13) Uani 1 1 d . . . . .
H20A H 1.1978 0.7032 0.5928 0.067 Uiso 1 1 calc R U . . .
C21 C 1.0550(5) 0.5554(5) 0.58178(11) 0.0632(15) Uani 1 1 d . . . . .
H21A H 1.0843 0.5352 0.5617 0.076 Uiso 1 1 calc R U . . .
C22 C 0.9463(5) 0.4870(4) 0.59298(9) 0.0501(12) Uani 1 1 d . . . . .
H22A H 0.8997 0.4194 0.5798 0.060 Uiso 1 1 calc R U . . .
P1 P 0.6667 0.3333 0.50073(5) 0.0501(5) Uani 1 3 d S T P . .
F1 F 0.7724(5) 0.3576(6) 0.52283(16) 0.189(3) Uani 1 1 d . . . . .
F2 F 0.7478(4) 0.4406(4) 0.47731(12) 0.1155(15) Uani 1 1 d . . . . .
O1 O 0.6667 0.3333 0.64352(12) 0.0378(9) Uani 1 3 d DS T P . .
H1 H 0.731(5) 0.389(6) 0.633(2) 0.057 Uiso 0.5 1 d D U P . .


_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 N2 1.946(2) 3_675 ?
Fe1 N2 1.946(2) . ?
Fe1 N2 1.946(2) 2_765 ?
Fe1 N1 1.992(2) . ?
Fe1 N1 1.992(2) 3_675 ?
Fe1 N1 1.992(2) 2_765 ?
N1 C1 1.344(4) . ?
N1 C5 1.360(4) . ?
N2 C6 1.341(3) . ?
N2 N3 1.343(3) . ?
N3 C8 1.356(4) . ?
N3 H3 0.8800 . ?
N4 N5 1.348(3) . ?
N4 C15 1.349(4) . ?
N4 H4 0.8800 . ?
N5 C17 1.338(4) . ?
N6 C18 1.359(4) . ?
N6 C22 1.363(5) . ?
C1 C2 1.383(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.382(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.388(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.451(4) . ?
C6 C7 1.400(4) . ?
C7 C8 1.383(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.467(4) . ?
C9 C14 1.385(4) . ?
C9 C10 1.397(4) . ?
C10 C11 1.383(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.389(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.396(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.394(4) . ?
C13 C15 1.478(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.379(4) . ?
C16 C17 1.403(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.475(4) . ?
C18 C19 1.381(5) . ?
C19 C20 1.390(6) . ?
C19 H19A 0.9500 . ?
C20 C21 1.369(8) . ?
C20 H20A 0.9500 . ?
C21 C22 1.357(8) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
P1 F1 1.540(5) 3_665 ?
P1 F1 1.540(5) . ?
P1 F1 1.540(5) 2_655 ?
P1 F2 1.578(4) 3_665 ?
P1 F2 1.578(4) . ?
P1 F2 1.578(4) 2_655 ?
O1 H1 0.91(2) . ?

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
N2 Fe1 N2 96.20(9) 3_675 . ?
N2 Fe1 N2 96.20(9) 3_675 2_765 ?
N2 Fe1 N2 96.20(9) . 2_765 ?
N2 Fe1 N1 89.16(9) 3_675 . ?
N2 Fe1 N1 80.33(10) . . ?
N2 Fe1 N1 173.92(10) 2_765 . ?
N2 Fe1 N1 80.33(10) 3_675 3_675 ?
N2 Fe1 N1 173.92(10) . 3_675 ?
N2 Fe1 N1 89.16(10) 2_765 3_675 ?
N1 Fe1 N1 94.57(9) . 3_675 ?
N2 Fe1 N1 173.92(10) 3_675 2_765 ?
N2 Fe1 N1 89.16(10) . 2_765 ?
N2 Fe1 N1 80.33(9) 2_765 2_765 ?
N1 Fe1 N1 94.57(9) . 2_765 ?
N1 Fe1 N1 94.57(9) 3_675 2_765 ?
C1 N1 C5 117.3(2) . . ?
C1 N1 Fe1 127.4(2) . . ?
C5 N1 Fe1 115.33(18) . . ?
C6 N2 N3 106.5(2) . . ?
C6 N2 Fe1 116.45(18) . . ?
N3 N2 Fe1 136.88(19) . . ?
N2 N3 C8 110.7(2) . . ?
N2 N3 H3 124.6 . . ?
C8 N3 H3 124.6 . . ?
N5 N4 C15 111.7(2) . . ?
N5 N4 H4 124.2 . . ?
C15 N4 H4 124.2 . . ?
C17 N5 N4 105.7(2) . . ?
C18 N6 C22 116.5(4) . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 H3A 120.8 . . ?
C4 C3 H3A 120.8 . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
N1 C5 C4 122.8(3) . . ?
N1 C5 C6 112.7(2) . . ?
C4 C5 C6 124.5(3) . . ?
N2 C6 C7 110.3(2) . . ?
N2 C6 C5 114.9(2) . . ?
C7 C6 C5 134.8(3) . . ?
C8 C7 C6 104.8(2) . . ?
C8 C7 H7A 127.6 . . ?
C6 C7 H7A 127.6 . . ?
N3 C8 C7 107.6(2) . . ?
N3 C8 C9 121.9(2) . . ?
C7 C8 C9 130.5(3) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 C8 121.1(3) . . ?
C10 C9 C8 119.8(3) . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 C15 120.3(3) . . ?
C12 C13 C15 120.8(3) . . ?
C9 C14 C13 121.3(3) . . ?
C9 C14 H14A 119.4 . . ?
C13 C14 H14A 119.4 . . ?
N4 C15 C16 107.0(2) . . ?
N4 C15 C13 121.3(2) . . ?
C16 C15 C13 131.7(3) . . ?
C15 C16 C17 105.1(3) . . ?
C15 C16 H16A 127.4 . . ?
C17 C16 H16A 127.4 . . ?
N5 C17 C16 110.4(2) . . ?
N5 C17 C18 120.3(3) . . ?
C16 C17 C18 129.3(3) . . ?
N6 C18 C19 123.5(3) . . ?
N6 C18 C17 117.0(3) . . ?
C19 C18 C17 119.5(3) . . ?
C18 C19 C20 117.0(4) . . ?
C18 C19 H19A 121.5 . . ?
C20 C19 H19A 121.5 . . ?
C21 C20 C19 121.1(4) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C22 C21 C20 118.3(3) . . ?
C22 C21 H21A 120.9 . . ?
C20 C21 H21A 120.9 . . ?
C21 C22 N6 123.7(4) . . ?
C21 C22 H22A 118.1 . . ?
N6 C22 H22A 118.1 . . ?
F1 P1 F1 94.0(4) 3_665 . ?
F1 P1 F1 94.0(4) 3_665 2_655 ?
F1 P1 F1 94.0(4) . 2_655 ?
F1 P1 F2 87.4(3) 3_665 3_665 ?
F1 P1 F2 86.3(3) . 3_665 ?
F1 P1 F2 178.6(4) 2_655 3_665 ?
F1 P1 F2 178.6(3) 3_665 . ?
F1 P1 F2 87.4(3) . . ?
F1 P1 F2 86.3(3) 2_655 . ?
F2 P1 F2 92.3(3) 3_665 . ?
F1 P1 F2 86.3(3) 3_665 2_655 ?
F1 P1 F2 178.6(4) . 2_655 ?
F1 P1 F2 87.4(3) 2_655 2_655 ?
F2 P1 F2 92.3(3) 3_665 2_655 ?
F2 P1 F2 92.3(3) . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N6 0.91(2) 2.09(3) 2.969(4) 163(8) .
N4 H4 Br1 0.88 2.60 3.453(2) 162.6 .

_refine_diff_density_max         1.416
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.088

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_md451b
_database_code_depnum_ccdc_archive 'CCDC 1512928'
_audit_update_record             
;
2016-10-28 deposited with the CCDC.
2016-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C66 H48 Fe N18), 2.23(P F6), 1.21(I), 0.56(I3), 2(C H4 O)'
_chemical_formula_sum            'C134 H104 F13.39 Fe2 I2.88 N36 O2 P2.23'
_chemical_formula_weight         3051.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0211 0.0125
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1183 0.1134
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3555 0.9930
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
I I -0.3071 2.1212
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   24.3560(10)
_cell_length_b                   13.6794(7)
_cell_length_c                   39.437(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.682(3)
_cell_angle_gamma                90
_cell_volume                     13021.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9071
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      25.51

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             6140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.274
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            141679
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.042
_diffrn_reflns_theta_max         25.610
_diffrn_reflns_theta_full        30.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.644
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.644
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.644
_reflns_number_total             18863
_reflns_number_gt                13842
_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       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically. The three PF6
 anions were disordered with either an I3 anion (P2 and P3) or
 an I- anion (P1), sharing the same space. All these were refined
 with displacement parameters restraints and 1,2 and 1,3 distance
 restraints. The relative occupancies were first refined and then
 fixed at the converged values, respectively: 0.79:0.21 for P1:I2,
 0.692:0.308 for P2:(I3-I4-I5) and 0.75:0.15:0.10 for 
 P3:(I6-I7-I8):(I9-I10-I11). Displacements parameters restraints 
 were also used to refine the lattice methanol molecules O1S-C1S
 and O2S-C2S. Hydrogens were fixed geometrically on their carrier
 atom and refined with a riding model, except those on the lattice
 methanol O1S and O2S that were refined freely with their thermal 
 parameter 1.5 that of their carrier O and distance restraints.
 The pyridyl ring with N18 site is likely disordered over two
 equivalent position rotated by 180 degrees rotation. Because
 no additional information was gained, this disorder was not 
 modeled.
;

_vrf_THETM01_md451b              
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Crystals were extremely thin plates, and 
significant diffraction was observed only up to ca. 0.9
angstrom resolution. The present data were cut at 0.90
angstrom as then I/sigma(I) was below 2, resulting in a
relatively poor value of thetamax.
;

_vrf_RFACR01_md451b              
;
PROBLEM:  The value of the weighted R factor is > 0.35
RESPONSE: Crystals were extremely thin plates, and 
significant diffraction was observed only up to ca. 0.9
angstrom resolution. The present data were cut at 0.90
angstrom as then I/sigma(I) was below 2. In addition,
the structure has significant disorder involving sites
of the heaviest atom present, I. The rather poor values
of R1 and wR2 are likely in part a consequence of the
relatively poor diffraction and heavy disorder present.
;

_vrf_PLAT084_md451b              
;
PROBLEM:  High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE: Crystals were extremely thin plates, and 
significant diffraction was observed only up to ca. 0.9
angstrom resolution. The present data were cut at 0.90
angstrom as then I/sigma(I) was below 2. In addition,
the structure has significant disorder involving sites
of the heaviest atom present, I. The rather poor values
of R1 and wR2 are likely in part a consequence of the
relatively poor diffraction and heavy disorder present.
;

_vrf_RFACG01_md451b              
;
PROBLEM:  The value of the R factor is > 0.10
RESPONSE: Crystals were extremely thin plates, and 
significant diffraction was observed only up to ca. 0.9
angstrom resolution. The present data were cut at 0.90
angstrom as then I/sigma(I) was below 2. In addition,
the structure has significant disorder involving sites
of the heaviest atom present, I. The rather poor values
of R1 and wR2 are likely in part a consequence of the
relatively poor diffraction and heavy disorder present.
;

_vrf_PLAT971_md451b              
;
PROBLEM:  Check Calcd Residual Density
RESPONSE: The structure has significant disorder involving
sites of the heaviest atom present, I. Most residual densities
are close to some I or Fe sites, so that they may be ascribed
to a combination of the heavy disorder and non-ideal
absorption corrections. The residual density close to N18 on
the other hand is likely due to the fact the corresponding 
pyridyl ring is disordered by rotation. Because no additional 
information was gained, this disorder was not modeled.
;

_vrf_PLAT972_md451b              
;
PROBLEM:  Check Calcd Residual Density
RESPONSE: The structure has significant disorder involving
sites of the heaviest atom present, I. Most residual densities
are close to some I or Fe sites, so that they may be ascribed
to a combination of the heavy disorder and non-ideal
absorption corrections.
;

_vrf_PLAT973_md451b              
;
PROBLEM:  Check Calcd Positive Density
RESPONSE: The structure has significant disorder involving
sites of the heaviest atom present, I. Most residual densities
are close to some I or Fe sites, so that they may be ascribed
to a combination of the heavy disorder and non-ideal
absorption corrections.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1952P)²+207.2605P] 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         18863
_refine_ls_number_parameters     1861
_refine_ls_number_restraints     536
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.1231
_refine_ls_wR_factor_ref         0.3705
_refine_ls_wR_factor_gt          0.3389
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.090
_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
I1 I 0.61762(4) 0.46936(7) 0.36832(2) 0.0577(3) Uani 1 1 d . . . . .
Fe1 Fe 0.80913(6) 0.41785(11) 0.46719(4) 0.0287(4) Uani 1 1 d . . . . .
N1 N 0.8504(4) 0.5298(6) 0.4896(2) 0.034(2) Uani 1 1 d . . . . .
N2 N 0.7476(3) 0.4980(6) 0.4783(2) 0.0269(19) Uani 1 1 d . . . . .
N3 N 0.6917(3) 0.4942(6) 0.4733(2) 0.0269(19) Uani 1 1 d . . . . .
H3B H 0.6720 0.4470 0.4624 0.032 Uiso 1 1 calc R U . . .
N4 N 0.4926(4) 0.4718(6) 0.4037(2) 0.032(2) Uani 1 1 d . . . . .
H4B H 0.5265 0.4753 0.3984 0.039 Uiso 1 1 calc R U . . .
N5 N 0.4504(3) 0.4255(6) 0.3840(2) 0.031(2) Uani 1 1 d . . . . .
N6 N 0.3107(4) 0.4237(9) 0.4048(3) 0.051(3) Uani 1 1 d . . . . .
N7 N 0.8102(4) 0.3417(7) 0.5099(2) 0.032(2) Uani 1 1 d . . . . .
N8 N 0.7652(3) 0.3055(6) 0.4496(2) 0.0272(19) Uani 1 1 d . . . . .
N9 N 0.7397(3) 0.2740(6) 0.4193(2) 0.0252(18) Uani 1 1 d . . . . .
H9A H 0.7362 0.3084 0.4003 0.030 Uiso 1 1 calc R U . . .
N10 N 0.5974(4) 0.2824(6) 0.3071(2) 0.032(2) Uani 1 1 d . . . . .
H10G H 0.6022 0.3174 0.3260 0.039 Uiso 1 1 calc R U . . .
N11 N 0.5763(4) 0.3186(7) 0.2763(2) 0.035(2) Uani 1 1 d . . . . .
N12 N 0.5437(4) 0.1724(9) 0.1995(3) 0.051(3) Uani 1 1 d . . . . .
N13 N 0.8764(4) 0.3499(7) 0.4549(3) 0.038(2) Uani 1 1 d . . . . .
N14 N 0.8142(3) 0.4785(6) 0.4227(2) 0.030(2) Uani 1 1 d . . . . .
N15 N 0.7866(3) 0.5471(6) 0.4026(2) 0.029(2) Uani 1 1 d . . . . .
H15A H 0.7560 0.5760 0.4070 0.035 Uiso 1 1 calc R U . . .
N16 N 0.6158(4) 0.6850(6) 0.3214(2) 0.030(2) Uani 1 1 d . . . . .
H16B H 0.6241 0.6320 0.3336 0.036 Uiso 1 1 calc R U . . .
N17 N 0.5634(4) 0.7188(6) 0.3133(2) 0.031(2) Uani 1 1 d . . . . .
N18 N 0.5257(6) 0.9182(7) 0.2553(3) 0.057(3) Uani 1 1 d . . . . .
C1 C 0.9055(5) 0.5446(9) 0.4928(3) 0.046(3) Uani 1 1 d . . . . .
H1A H 0.9282 0.4970 0.4840 0.056 Uiso 1 1 calc R U . . .
C2 C 0.9306(6) 0.6277(10) 0.5088(4) 0.059(4) Uani 1 1 d . . . . .
H2A H 0.9696 0.6363 0.5104 0.071 Uiso 1 1 calc R U . . .
C3 C 0.8992(5) 0.6958(10) 0.5220(4) 0.055(4) Uani 1 1 d . . . . .
H3A H 0.9159 0.7516 0.5335 0.066 Uiso 1 1 calc R U . . .
C4 C 0.8426(5) 0.6830(9) 0.5187(3) 0.046(3) Uani 1 1 d . . . . .
H4A H 0.8199 0.7300 0.5277 0.055 Uiso 1 1 calc R U . . .
C5 C 0.8191(5) 0.6007(8) 0.5019(3) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.7609(4) 0.5807(7) 0.4956(2) 0.028(2) Uani 1 1 d . . . . .
C7 C 0.7133(4) 0.6311(8) 0.5021(3) 0.031(2) Uani 1 1 d . . . . .
H7A H 0.7116 0.6912 0.5140 0.037 Uiso 1 1 calc R U . . .
C8 C 0.6697(4) 0.5748(7) 0.4875(3) 0.027(2) Uani 1 1 d . . . . .
C9 C 0.6103(4) 0.5913(7) 0.4853(3) 0.029(2) Uani 1 1 d . . . . .
C10 C 0.5895(5) 0.6593(8) 0.5070(3) 0.032(2) Uani 1 1 d . . . . .
H10A H 0.6142 0.6944 0.5233 0.039 Uiso 1 1 calc R U . . .
C11 C 0.5335(4) 0.6754(8) 0.5046(3) 0.032(2) Uani 1 1 d . . . . .
H11A H 0.5201 0.7207 0.5198 0.038 Uiso 1 1 calc R U . . .
C12 C 0.4962(5) 0.6281(8) 0.4809(3) 0.035(3) Uani 1 1 d . . . . .
H12A H 0.4576 0.6409 0.4799 0.042 Uiso 1 1 calc R U . . .
C13 C 0.5152(4) 0.5609(7) 0.4581(3) 0.029(2) Uani 1 1 d . . . . .
C14 C 0.5722(4) 0.5439(7) 0.4608(2) 0.025(2) Uani 1 1 d . . . . .
H14A H 0.5856 0.4987 0.4456 0.030 Uiso 1 1 calc R U . . .
C15 C 0.4771(4) 0.5121(7) 0.4325(3) 0.030(2) Uani 1 1 d . . . . .
C16 C 0.4213(5) 0.4894(8) 0.4316(3) 0.033(2) Uani 1 1 d . . . . .
H16A H 0.3975 0.5066 0.4479 0.040 Uiso 1 1 calc R U . . .
C17 C 0.4080(5) 0.4361(7) 0.4017(3) 0.034(3) Uani 1 1 d . . . . .
C18 C 0.3532(5) 0.3896(9) 0.3905(3) 0.037(3) Uani 1 1 d . . . . .
C19 C 0.3476(6) 0.3104(10) 0.3673(4) 0.053(3) Uani 1 1 d . . . . .
H19A H 0.3785 0.2864 0.3574 0.063 Uiso 1 1 calc R U . . .
C20 C 0.2953(6) 0.2687(13) 0.3596(4) 0.069(4) Uani 1 1 d . . . . .
H20A H 0.2897 0.2150 0.3443 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2532(7) 0.3050(12) 0.3741(4) 0.069(4) Uani 1 1 d . . . . .
H21A H 0.2172 0.2776 0.3689 0.083 Uiso 1 1 calc R U . . .
C22 C 0.2619(6) 0.3815(12) 0.3962(4) 0.061(4) Uani 1 1 d . . . . .
H22A H 0.2312 0.4061 0.4060 0.073 Uiso 1 1 calc R U . . .
C23 C 0.8365(5) 0.3661(9) 0.5412(3) 0.044(3) Uani 1 1 d . . . . .
H23A H 0.8529 0.4290 0.5446 0.053 Uiso 1 1 calc R U . . .
C24 C 0.8400(5) 0.3004(11) 0.5686(3) 0.051(3) Uani 1 1 d . . . . .
H24A H 0.8577 0.3199 0.5905 0.062 Uiso 1 1 calc R U . . .
C25 C 0.8188(5) 0.2104(11) 0.5643(3) 0.053(4) Uani 1 1 d . . . . .
H25A H 0.8229 0.1651 0.5828 0.064 Uiso 1 1 calc R U . . .
C26 C 0.7903(5) 0.1832(9) 0.5322(3) 0.040(3) Uani 1 1 d . . . . .
H26A H 0.7738 0.1205 0.5286 0.047 Uiso 1 1 calc R U . . .
C27 C 0.7873(4) 0.2507(8) 0.5063(3) 0.034(3) Uani 1 1 d . . . . .
C28 C 0.7608(4) 0.2317(7) 0.4714(3) 0.029(2) Uani 1 1 d . . . . .
C29 C 0.7325(4) 0.1527(8) 0.4557(3) 0.032(2) Uani 1 1 d . . . . .
H29A H 0.7237 0.0925 0.4657 0.039 Uiso 1 1 calc R U . . .
C30 C 0.7201(4) 0.1826(7) 0.4219(3) 0.031(2) Uani 1 1 d . . . . .
C31 C 0.6902(5) 0.1308(8) 0.3925(3) 0.035(3) Uani 1 1 d . . . . .
C32 C 0.6863(6) 0.0281(8) 0.3925(3) 0.050(3) Uani 1 1 d . . . . .
H32A H 0.7024 -0.0080 0.4119 0.060 Uiso 1 1 calc R U . . .
C33 C 0.6592(7) -0.0199(9) 0.3646(4) 0.062(4) Uani 1 1 d . . . . .
H33A H 0.6581 -0.0893 0.3646 0.074 Uiso 1 1 calc R U . . .
C34 C 0.6334(6) 0.0308(8) 0.3364(3) 0.053(4) Uani 1 1 d . . . . .
H34A H 0.6140 -0.0036 0.3176 0.063 Uiso 1 1 calc R U . . .
C35 C 0.6363(5) 0.1328(8) 0.3359(3) 0.036(3) Uani 1 1 d . . . . .
C36 C 0.6634(4) 0.1814(7) 0.3636(3) 0.031(2) Uani 1 1 d . . . . .
H36A H 0.6643 0.2508 0.3634 0.037 Uiso 1 1 calc R U . . .
C37 C 0.6103(5) 0.1873(8) 0.3058(3) 0.033(2) Uani 1 1 d . . . . .
C38 C 0.5967(4) 0.1592(8) 0.2719(3) 0.035(3) Uani 1 1 d . . . . .
H38A H 0.6007 0.0963 0.2623 0.042 Uiso 1 1 calc R U . . .
C39 C 0.5759(4) 0.2434(8) 0.2550(3) 0.033(3) Uani 1 1 d . . . . .
C40 C 0.5552(4) 0.2576(8) 0.2183(3) 0.034(3) Uani 1 1 d . . . . .
C41 C 0.5494(5) 0.3475(9) 0.2045(4) 0.051(3) Uani 1 1 d . . . . .
H41A H 0.5577 0.4045 0.2180 0.062 Uiso 1 1 calc R U . . .
C42 C 0.5303(7) 0.3535(15) 0.1688(5) 0.085(6) Uani 1 1 d . . . . .
H42A H 0.5260 0.4156 0.1581 0.102 Uiso 1 1 calc R U . . .
C43 C 0.5183(6) 0.2712(19) 0.1500(4) 0.081(6) Uani 1 1 d . . . . .
H43A H 0.5055 0.2751 0.1262 0.097 Uiso 1 1 calc R U . . .
C44 C 0.5249(5) 0.1833(13) 0.1659(3) 0.056(4) Uani 1 1 d . . . . .
H44A H 0.5158 0.1262 0.1526 0.068 Uiso 1 1 calc R U . . .
C45 C 0.9048(5) 0.2770(9) 0.4720(3) 0.044(3) Uani 1 1 d . . . . .
H45A H 0.8933 0.2560 0.4929 0.053 Uiso 1 1 calc R U . . .
C46 C 0.9489(5) 0.2312(10) 0.4613(4) 0.053(4) Uani 1 1 d . . . . .
H46A H 0.9666 0.1779 0.4738 0.063 Uiso 1 1 calc R U . . .
C47 C 0.9675(6) 0.2651(11) 0.4314(4) 0.060(4) Uani 1 1 d . . . . .
H47A H 0.9992 0.2366 0.4237 0.072 Uiso 1 1 calc R U . . .
C48 C 0.9393(5) 0.3407(10) 0.4131(3) 0.052(3) Uani 1 1 d . . . . .
H48A H 0.9510 0.3647 0.3926 0.062 Uiso 1 1 calc R U . . .
C49 C 0.8931(4) 0.3804(8) 0.4255(3) 0.034(3) Uani 1 1 d . . . . .
C50 C 0.8585(4) 0.4540(8) 0.4074(3) 0.034(3) Uani 1 1 d . . . . .
C51 C 0.8593(5) 0.5062(9) 0.3775(3) 0.037(3) Uani 1 1 d . . . . .
H51A H 0.8861 0.5024 0.3620 0.045 Uiso 1 1 calc R U . . .
C52 C 0.8122(4) 0.5658(8) 0.3748(3) 0.031(2) Uani 1 1 d . . . . .
C53 C 0.7900(5) 0.6364(9) 0.3481(3) 0.037(3) Uani 1 1 d . . . . .
C54 C 0.8256(5) 0.6849(11) 0.3289(4) 0.056(4) Uani 1 1 d . . . . .
H54A H 0.8644 0.6738 0.3336 0.068 Uiso 1 1 calc R U . . .
C55 C 0.8056(6) 0.7481(12) 0.3035(4) 0.064(4) Uani 1 1 d . . . . .
H55A H 0.8305 0.7781 0.2900 0.076 Uiso 1 1 calc R U . . .
C56 C 0.7496(5) 0.7693(11) 0.2969(4) 0.056(4) Uani 1 1 d . . . . .
H56A H 0.7361 0.8157 0.2799 0.067 Uiso 1 1 calc R U . . .
C57 C 0.7137(5) 0.7215(8) 0.3158(3) 0.034(3) Uani 1 1 d . . . . .
C58 C 0.7340(5) 0.6557(8) 0.3410(3) 0.033(3) Uani 1 1 d . . . . .
H58A H 0.7089 0.6232 0.3537 0.040 Uiso 1 1 calc R U . . .
C59 C 0.6542(5) 0.7412(8) 0.3087(3) 0.032(2) Uani 1 1 d . . . . .
C60 C 0.6238(5) 0.8150(8) 0.2911(3) 0.036(3) Uani 1 1 d . . . . .
H60A H 0.6381 0.8669 0.2789 0.043 Uiso 1 1 calc R U . . .
C61 C 0.5690(5) 0.7993(7) 0.2945(3) 0.032(2) Uani 1 1 d . . . . .
C62 C 0.5182(5) 0.8566(8) 0.2811(3) 0.042(3) Uani 1 1 d . . . . .
C63 C 0.4692(5) 0.8464(8) 0.2946(3) 0.045(3) Uani 1 1 d . . . . .
H63A H 0.4661 0.8042 0.3134 0.054 Uiso 1 1 calc R U . . .
C64 C 0.4239(6) 0.9021(10) 0.2790(4) 0.064(4) Uani 1 1 d . . . . .
H64A H 0.3886 0.8960 0.2865 0.077 Uiso 1 1 calc R U . . .
C65 C 0.4309(9) 0.9637(10) 0.2533(5) 0.081(6) Uani 1 1 d . . . . .
H65A H 0.4010 1.0030 0.2431 0.097 Uiso 1 1 calc R U . . .
C66 C 0.4809(9) 0.9690(10) 0.2422(4) 0.072(5) Uani 1 1 d . . . . .
H66A H 0.4845 1.0119 0.2237 0.086 Uiso 1 1 calc R U . . .
Fe2 Fe 0.42209(6) 0.51059(11) 0.26835(4) 0.0298(4) Uani 1 1 d . . . . .
N21 N 0.3457(4) 0.4907(7) 0.2804(2) 0.037(2) Uani 1 1 d . . . . .
N22 N 0.4294(3) 0.5778(6) 0.3123(2) 0.029(2) Uani 1 1 d . . . . .
N23 N 0.4686(3) 0.6263(6) 0.3329(2) 0.0273(19) Uani 1 1 d . . . . .
H23B H 0.5032 0.6323 0.3290 0.033 Uiso 1 1 calc R U . . .
N24 N 0.6568(3) 0.6863(6) 0.4136(2) 0.0275(19) Uani 1 1 d . . . . .
H24B H 0.6403 0.6361 0.4026 0.033 Uiso 1 1 calc R U . . .
N25 N 0.7124(4) 0.6961(6) 0.4204(2) 0.031(2) Uani 1 1 d . . . . .
N26 N 0.7809(4) 0.8884(7) 0.4730(3) 0.043(2) Uani 1 1 d D . . . .
N27 N 0.4089(4) 0.4310(7) 0.2254(2) 0.036(2) Uani 1 1 d . . . . .
N28 N 0.4434(3) 0.3832(6) 0.2871(2) 0.030(2) Uani 1 1 d . . . . .
N29 N 0.4612(3) 0.3440(6) 0.3177(2) 0.031(2) Uani 1 1 d . . . . .
H29B H 0.4679 0.3777 0.3368 0.038 Uiso 1 1 calc R U . . .
N30 N 0.6004(4) 0.2929(6) 0.4297(2) 0.034(2) Uani 1 1 d . . . . .
H30A H 0.5984 0.3296 0.4113 0.041 Uiso 1 1 calc R U . . .
N31 N 0.6304(4) 0.3182(6) 0.4604(2) 0.030(2) Uani 1 1 d . . . . .
N32 N 0.6500(4) 0.1600(8) 0.5347(3) 0.048(3) Uani 1 1 d . . . . .
N33 N 0.4016(3) 0.6320(7) 0.2428(2) 0.032(2) Uani 1 1 d . . . . .
N34 N 0.4955(3) 0.5489(6) 0.2576(2) 0.0261(19) Uani 1 1 d . . . . .
N35 N 0.5477(4) 0.5153(6) 0.2639(2) 0.030(2) Uani 1 1 d . . . . .
H35A H 0.5579 0.4634 0.2764 0.036 Uiso 1 1 calc R U . . .
N36 N 0.7343(4) 0.3950(6) 0.3330(2) 0.033(2) Uani 1 1 d . . . . .
H36B H 0.7042 0.4234 0.3383 0.039 Uiso 1 1 calc R U . . .
N37 N 0.7644(4) 0.3306(6) 0.3536(2) 0.033(2) Uani 1 1 d . . . . .
N38 N 0.8974(5) 0.2384(9) 0.3400(3) 0.057(3) Uani 1 1 d . . . . .
C71 C 0.3030(5) 0.4436(10) 0.2613(3) 0.050(3) Uani 1 1 d . . . . .
H71A H 0.3093 0.4140 0.2404 0.060 Uiso 1 1 calc R U . . .
C72 C 0.2507(6) 0.4371(11) 0.2713(4) 0.058(4) Uani 1 1 d . . . . .
H72A H 0.2214 0.4048 0.2574 0.070 Uiso 1 1 calc R U . . .
C73 C 0.2421(6) 0.4795(13) 0.3027(4) 0.066(4) Uani 1 1 d . . . . .
H73A H 0.2070 0.4742 0.3105 0.079 Uiso 1 1 calc R U . . .
C74 C 0.2836(5) 0.5277(11) 0.3216(3) 0.052(3) Uani 1 1 d . . . . .
H74A H 0.2778 0.5583 0.3425 0.062 Uiso 1 1 calc R U . . .
C75 C 0.3357(5) 0.5320(9) 0.3101(3) 0.039(3) Uani 1 1 d . . . . .
C76 C 0.3832(4) 0.5829(8) 0.3278(3) 0.031(2) Uani 1 1 d . . . . .
C77 C 0.3922(4) 0.6379(8) 0.3574(3) 0.034(3) Uani 1 1 d . . . . .
H77A H 0.3661 0.6537 0.3724 0.041 Uiso 1 1 calc R U . . .
C78 C 0.4482(4) 0.6654(7) 0.3606(3) 0.028(2) Uani 1 1 d . . . . .
C79 C 0.4805(4) 0.7228(7) 0.3866(3) 0.028(2) Uani 1 1 d . . . . .
C80 C 0.4537(4) 0.7867(8) 0.4064(3) 0.032(2) Uani 1 1 d . . . . .
H80A H 0.4146 0.7943 0.4021 0.039 Uiso 1 1 calc R U . . .
C81 C 0.4841(5) 0.8393(8) 0.4325(3) 0.036(3) Uani 1 1 d . . . . .
H81A H 0.4653 0.8819 0.4461 0.044 Uiso 1 1 calc R U . . .
C82 C 0.5408(5) 0.8315(8) 0.4393(3) 0.034(3) Uani 1 1 d . . . . .
H82A H 0.5608 0.8682 0.4573 0.041 Uiso 1 1 calc R U . . .
C83 C 0.5687(4) 0.7696(7) 0.4194(3) 0.027(2) Uani 1 1 d . . . . .
C84 C 0.5382(4) 0.7160(7) 0.3931(2) 0.028(2) Uani 1 1 d . . . . .
H84A H 0.5572 0.6743 0.3793 0.034 Uiso 1 1 calc R U . . .
C85 C 0.6289(4) 0.7619(8) 0.4256(3) 0.030(2) Uani 1 1 d . . . . .
C86 C 0.6688(4) 0.8230(7) 0.4414(3) 0.029(2) Uani 1 1 d . . . . .
H86A H 0.6629 0.8819 0.4532 0.034 Uiso 1 1 calc R U . . .
C87 C 0.7195(5) 0.7823(7) 0.4371(3) 0.031(2) Uani 1 1 d . . . . .
C88 C 0.7755(5) 0.8218(8) 0.4468(3) 0.036(3) Uani 1 1 d . . . . .
C89 C 0.8191(5) 0.7977(10) 0.4299(3) 0.044(3) Uani 1 1 d . . . . .
H89A H 0.8143 0.7512 0.4119 0.053 Uiso 1 1 calc R U . . .
C90 C 0.8705(5) 0.8411(10) 0.4392(4) 0.051(3) Uani 1 1 d . . . . .
H90A H 0.9009 0.8254 0.4274 0.061 Uiso 1 1 calc R U . . .
C91 C 0.8766(6) 0.9070(10) 0.4656(4) 0.057(4) Uani 1 1 d . . . . .
H91A H 0.9115 0.9362 0.4731 0.069 Uiso 1 1 calc R U . . .
C92 C 0.8304(6) 0.9298(10) 0.4810(4) 0.055(3) Uani 1 1 d . . . . .
H92A H 0.8342 0.9781 0.4985 0.065 Uiso 1 1 calc R U . . .
C93 C 0.3917(5) 0.4622(10) 0.1932(3) 0.044(3) Uani 1 1 d . . . . .
H93A H 0.3858 0.5302 0.1895 0.053 Uiso 1 1 calc R U . . .
C94 C 0.3823(6) 0.4001(11) 0.1656(3) 0.057(4) Uani 1 1 d . . . . .
H94A H 0.3697 0.4246 0.1434 0.068 Uiso 1 1 calc R U . . .
C95 C 0.3915(5) 0.3025(11) 0.1709(3) 0.052(3) Uani 1 1 d . . . . .
H95A H 0.3856 0.2584 0.1521 0.063 Uiso 1 1 calc R U . . .
C96 C 0.4091(5) 0.2687(10) 0.2026(3) 0.044(3) Uani 1 1 d . . . . .
H96A H 0.4149 0.2007 0.2065 0.053 Uiso 1 1 calc R U . . .
C97 C 0.4187(4) 0.3351(9) 0.2297(3) 0.035(3) Uani 1 1 d . . . . .
C98 C 0.4380(4) 0.3072(8) 0.2652(3) 0.034(3) Uani 1 1 d . . . . .
C99 C 0.4523(5) 0.2207(8) 0.2819(3) 0.037(3) Uani 1 1 d . . . . .
H99A H 0.4517 0.1571 0.2721 0.045 Uiso 1 1 calc R U . . .
C100 C 0.4677(4) 0.2453(7) 0.3155(3) 0.033(2) Uani 1 1 d . . . . .
C101 C 0.4876(5) 0.1831(8) 0.3445(3) 0.037(3) Uani 1 1 d . . . . .
C102 C 0.4776(6) 0.0853(9) 0.3440(3) 0.056(4) Uani 1 1 d . . . . .
H10B H 0.4546 0.0582 0.3250 0.068 Uiso 1 1 calc R U . . .
C103 C 0.4999(8) 0.0238(10) 0.3702(4) 0.075(5) Uani 1 1 d . . . . .
H10C H 0.4938 -0.0447 0.3687 0.090 Uiso 1 1 calc R U . . .
C104 C 0.5314(7) 0.0641(9) 0.3986(3) 0.058(4) Uani 1 1 d . . . . .
H10D H 0.5465 0.0227 0.4168 0.069 Uiso 1 1 calc R U . . .
C105 C 0.5414(5) 0.1652(8) 0.4010(3) 0.042(3) Uani 1 1 d . . . . .
C106 C 0.5206(5) 0.2232(7) 0.3735(3) 0.034(3) Uani 1 1 d . . . . .
H10E H 0.5287 0.2911 0.3740 0.041 Uiso 1 1 calc R U . . .
C107 C 0.5742(5) 0.2055(8) 0.4308(3) 0.037(3) Uani 1 1 d . . . . .
C108 C 0.5864(4) 0.1738(8) 0.4643(3) 0.036(3) Uani 1 1 d . . . . .
H10F H 0.5739 0.1153 0.4738 0.043 Uiso 1 1 calc R U . . .
C109 C 0.6206(4) 0.2450(8) 0.4814(3) 0.033(3) Uani 1 1 d . . . . .
C110 C 0.6457(4) 0.2465(8) 0.5170(3) 0.033(3) Uani 1 1 d . . . . .
C111 C 0.6657(4) 0.3315(8) 0.5313(3) 0.033(2) Uani 1 1 d . . . . .
H11B H 0.6627 0.3903 0.5184 0.039 Uiso 1 1 calc R U . . .
C112 C 0.6899(6) 0.3319(10) 0.5641(4) 0.054(4) Uani 1 1 d . . . . .
H11C H 0.7033 0.3912 0.5746 0.065 Uiso 1 1 calc R U . . .
C113 C 0.6950(5) 0.2437(11) 0.5826(3) 0.050(3) Uani 1 1 d . . . . .
H11D H 0.7127 0.2432 0.6056 0.059 Uiso 1 1 calc R U . . .
C114 C 0.6747(5) 0.1599(10) 0.5678(3) 0.045(3) Uani 1 1 d . . . . .
H11E H 0.6777 0.1007 0.5805 0.054 Uiso 1 1 calc R U . . .
C115 C 0.3504(5) 0.6678(9) 0.2343(3) 0.041(3) Uani 1 1 d . . . . .
H11F H 0.3210 0.6401 0.2447 0.049 Uiso 1 1 calc R U . . .
C116 C 0.3384(6) 0.7428(9) 0.2112(3) 0.049(3) Uani 1 1 d . . . . .
H11G H 0.3015 0.7653 0.2053 0.058 Uiso 1 1 calc R U . . .
C117 C 0.3821(5) 0.7852(9) 0.1967(3) 0.047(3) Uani 1 1 d . . . . .
H11H H 0.3750 0.8370 0.1807 0.056 Uiso 1 1 calc R U . . .
C118 C 0.4341(5) 0.7528(8) 0.2054(3) 0.041(3) Uani 1 1 d . . . . .
H11I H 0.4638 0.7821 0.1958 0.049 Uiso 1 1 calc R U . . .
C119 C 0.4442(5) 0.6763(7) 0.2285(3) 0.032(2) Uani 1 1 d . . . . .
C120 C 0.4975(5) 0.6295(7) 0.2385(2) 0.031(2) Uani 1 1 d . . . . .
C121 C 0.5509(4) 0.6477(7) 0.2321(3) 0.029(2) Uani 1 1 d . . . . .
H12B H 0.5630 0.7005 0.2193 0.034 Uiso 1 1 calc R U . . .
C122 C 0.5833(4) 0.5734(7) 0.2481(2) 0.028(2) Uani 1 1 d . . . . .
C123 C 0.6424(5) 0.5543(7) 0.2502(3) 0.030(2) Uani 1 1 d . . . . .
C124 C 0.6731(5) 0.5991(9) 0.2268(3) 0.042(3) Uani 1 1 d . . . . .
H12C H 0.6550 0.6411 0.2097 0.051 Uiso 1 1 calc R U . . .
C125 C 0.7293(6) 0.5826(10) 0.2286(3) 0.053(3) Uani 1 1 d . . . . .
H12D H 0.7497 0.6137 0.2127 0.064 Uiso 1 1 calc R U . . .
C126 C 0.7566(5) 0.5203(8) 0.2536(3) 0.040(3) Uani 1 1 d . . . . .
H12E H 0.7953 0.5090 0.2548 0.048 Uiso 1 1 calc R U . . .
C127 C 0.7262(5) 0.4754(8) 0.2768(3) 0.032(2) Uani 1 1 d . . . . .
C128 C 0.6702(4) 0.4923(7) 0.2749(2) 0.030(2) Uani 1 1 d . . . . .
H12F H 0.6499 0.4610 0.2908 0.035 Uiso 1 1 calc R U . . .
C129 C 0.7548(5) 0.4118(8) 0.3035(3) 0.032(2) Uani 1 1 d . . . . .
C130 C 0.8020(5) 0.3553(8) 0.3048(3) 0.037(3) Uani 1 1 d . . . . .
H13A H 0.8266 0.3507 0.2881 0.045 Uiso 1 1 calc R U . . .
C131 C 0.8055(5) 0.3058(8) 0.3365(3) 0.037(3) Uani 1 1 d . . . . .
C132 C 0.8478(6) 0.2326(9) 0.3501(3) 0.047(3) Uani 1 1 d . . . . .
C133 C 0.8333(6) 0.1607(10) 0.3726(3) 0.056(4) Uani 1 1 d . . . . .
H13B H 0.7976 0.1589 0.3797 0.067 Uiso 1 1 calc R U . . .
C134 C 0.8743(9) 0.0915(12) 0.3840(4) 0.077(5) Uani 1 1 d . . . . .
H13C H 0.8664 0.0408 0.3991 0.093 Uiso 1 1 calc R U . . .
C135 C 0.9239(8) 0.0967(15) 0.3737(4) 0.083(6) Uani 1 1 d . . . . .
H13D H 0.9519 0.0505 0.3814 0.099 Uiso 1 1 calc R U . . .
C136 C 0.9338(7) 0.1692(16) 0.3520(4) 0.080(6) Uani 1 1 d . . . . .
H13E H 0.9694 0.1711 0.3446 0.096 Uiso 1 1 calc R U . . .
P1 P 0.4201(2) -0.0304(4) 0.12521(12) 0.0735(14) Uani 0.79 1 d D U P A 1
F1 F 0.3991(6) -0.0251(9) 0.0873(3) 0.127(3) Uani 0.79 1 d D U P A 1
F2 F 0.4284(6) -0.1431(7) 0.1232(3) 0.124(3) Uani 0.79 1 d D U P A 1
F3 F 0.4824(5) -0.0144(10) 0.1178(4) 0.128(4) Uani 0.79 1 d D U P A 1
F4 F 0.4457(5) -0.0346(8) 0.1646(3) 0.108(3) Uani 0.79 1 d D U P A 1
F5 F 0.4172(5) 0.0844(7) 0.1281(3) 0.091(3) Uani 0.79 1 d D U P A 1
F6 F 0.3628(4) -0.0432(10) 0.1359(3) 0.122(3) Uani 0.79 1 d D U P A 1
P2 P 0.2128(3) 0.4594(5) 0.16364(16) 0.0732(17) Uani 0.692 1 d D U P B 1
F7 F 0.1765(7) 0.5190(13) 0.1855(4) 0.109(4) Uani 0.692 1 d D U P B 1
F8 F 0.2614(6) 0.5292(12) 0.1779(4) 0.106(4) Uani 0.692 1 d D U P B 1
F9 F 0.1931(8) 0.5341(12) 0.1337(4) 0.112(4) Uani 0.692 1 d D U P B 1
F10 F 0.2490(6) 0.4067(15) 0.1384(4) 0.115(4) Uani 0.692 1 d D U P B 1
F11 F 0.1629(7) 0.3874(14) 0.1499(5) 0.100(4) Uani 0.692 1 d D U P B 1
F12 F 0.2296(9) 0.3785(14) 0.1909(5) 0.129(4) Uani 0.692 1 d D U P B 1
P3 P 0.4453(3) 0.4645(6) 0.0656(2) 0.097(2) Uani 0.75 1 d D U P C 1
F13 F 0.5060(5) 0.4395(10) 0.0684(3) 0.109(3) Uani 0.75 1 d D U P C 1
F14 F 0.4319(5) 0.3777(9) 0.0874(3) 0.102(3) Uani 0.75 1 d D U P C 1
F15 F 0.4257(6) 0.4151(11) 0.0323(3) 0.118(3) Uani 0.75 1 d D U P C 1
F16 F 0.4523(6) 0.5618(9) 0.0481(3) 0.117(4) Uani 0.75 1 d D U P C 1
F17 F 0.4557(6) 0.5267(10) 0.1005(3) 0.116(3) Uani 0.75 1 d D U P C 1
F18 F 0.3825(5) 0.5011(11) 0.0646(4) 0.119(3) Uani 0.75 1 d D U P C 1
I2 I 0.3851(4) 0.0309(5) 0.1506(2) 0.115(3) Uani 0.21 1 d . U P D 2
I3 I 0.29806(12) 0.1755(2) 0.24828(10) 0.0701(9) Uani 0.308 1 d D U P E 2
I4 I 0.23462(12) 0.2963(2) 0.19481(9) 0.0631(8) Uani 0.308 1 d D U P E 2
I5 I 0.1744(3) 0.4507(4) 0.15422(12) 0.1018(16) Uani 0.308 1 d D U P E 2
I6 I 0.4752(4) 0.3272(9) 0.0466(3) 0.122(3) Uani 0.15 1 d D U P F 2
I7 I 0.4327(5) 0.5046(9) 0.0747(4) 0.104(3) Uani 0.15 1 d D U P F 2
I8 I 0.3957(4) 0.6667(8) 0.1139(3) 0.116(3) Uani 0.15 1 d D U P F 2
I9 I 0.4164(6) 0.5572(9) 0.0785(4) 0.096(3) Uani 0.1 1 d D U P G 3
I10 I 0.4619(5) 0.3644(9) 0.0637(4) 0.088(3) Uani 0.1 1 d D U P G 3
I11 I 0.4977(4) 0.1606(8) 0.0596(2) 0.078(3) Uani 0.1 1 d D U P G 3
O1S O 0.7159(6) 0.8862(15) 0.5265(3) 0.133(6) Uani 1 1 d D U . . .
H1S H 0.7305 0.9161 0.5114 0.200 Uiso 1 1 calc DR U . . .
C1S C 0.7469(8) 0.9041(19) 0.5591(4) 0.106(6) Uani 1 1 d D U . . .
H1S1 H 0.7787 0.9459 0.5564 0.160 Uiso 1 1 calc R U . . .
H1S2 H 0.7600 0.8419 0.5695 0.160 Uiso 1 1 calc R U . . .
H1S3 H 0.7232 0.9368 0.5739 0.160 Uiso 1 1 calc R U . . .
O2S O 0.6072(9) 0.9457(15) 0.5120(5) 0.162(7) Uani 1 1 d D U . . .
H2S H 0.6398 0.9623 0.5193 0.243 Uiso 1 1 calc DR U . . .
C2S C 0.5796(12) 0.9123(16) 0.5405(7) 0.146(8) Uani 1 1 d D U . . .
H2S1 H 0.6059 0.8750 0.5566 0.219 Uiso 1 1 calc R U . . .
H2S2 H 0.5482 0.8704 0.5319 0.219 Uiso 1 1 calc R U . . .
H2S3 H 0.5663 0.9689 0.5523 0.219 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N8 1.947(8) . ?
Fe1 N2 1.954(8) . ?
Fe1 N14 1.960(9) . ?
Fe1 N1 1.973(9) . ?
Fe1 N7 1.977(9) . ?
Fe1 N13 1.998(9) . ?
N1 C1 1.348(15) . ?
N1 C5 1.362(14) . ?
N2 C6 1.338(13) . ?
N2 N3 1.350(12) . ?
N3 C8 1.378(13) . ?
N3 H3B 0.8800 . ?
N4 N5 1.359(12) . ?
N4 C15 1.362(14) . ?
N4 H4B 0.8800 . ?
N5 C17 1.330(14) . ?
N6 C22 1.324(17) . ?
N6 C18 1.327(16) . ?
N7 C23 1.356(15) . ?
N7 C27 1.364(15) . ?
N8 C28 1.341(13) . ?
N8 N9 1.341(12) . ?
N9 C30 1.346(13) . ?
N9 H9A 0.8800 . ?
N10 C37 1.340(14) . ?
N10 N11 1.351(12) . ?
N10 H10G 0.8800 . ?
N11 C39 1.327(14) . ?
N12 C44 1.354(17) . ?
N12 C40 1.388(16) . ?
N13 C45 1.342(16) . ?
N13 C49 1.346(15) . ?
N14 C50 1.345(14) . ?
N14 N15 1.348(12) . ?
N15 C52 1.359(14) . ?
N15 H15A 0.8800 . ?
N16 N17 1.356(12) . ?
N16 C59 1.356(14) . ?
N16 H16B 0.8800 . ?
N17 C61 1.344(14) . ?
N18 C66 1.34(2) . ?
N18 C62 1.350(16) . ?
C1 C2 1.400(18) . ?
C1 H1A 0.9500 . ?
C2 C3 1.353(19) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(18) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(16) . ?
C4 H4A 0.9500 . ?
C5 C6 1.432(16) . ?
C6 C7 1.401(15) . ?
C7 C8 1.374(15) . ?
C7 H7A 0.9500 . ?
C8 C9 1.454(15) . ?
C9 C10 1.403(15) . ?
C9 C14 1.406(15) . ?
C10 C11 1.372(15) . ?
C10 H10A 0.9500 . ?
C11 C12 1.376(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.406(15) . ?
C12 H12A 0.9500 . ?
C13 C14 1.398(15) . ?
C13 C15 1.441(15) . ?
C14 H14A 0.9500 . ?
C15 C16 1.390(15) . ?
C16 C17 1.388(16) . ?
C16 H16A 0.9500 . ?
C17 C18 1.491(16) . ?
C18 C19 1.413(18) . ?
C19 C20 1.39(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.34(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.36(2) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.400(19) . ?
C23 H23A 0.9500 . ?
C24 C25 1.34(2) . ?
C24 H24A 0.9500 . ?
C25 C26 1.412(18) . ?
C25 H25A 0.9500 . ?
C26 C27 1.372(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.460(15) . ?
C28 C29 1.383(15) . ?
C29 C30 1.389(15) . ?
C29 H29A 0.9500 . ?
C30 C31 1.468(15) . ?
C31 C32 1.408(16) . ?
C31 C36 1.414(15) . ?
C32 C33 1.371(18) . ?
C32 H32A 0.9500 . ?
C33 C34 1.388(19) . ?
C33 H33A 0.9500 . ?
C34 C35 1.398(16) . ?
C34 H34A 0.9500 . ?
C35 C36 1.370(16) . ?
C35 C37 1.472(16) . ?
C36 H36A 0.9500 . ?
C37 C38 1.390(16) . ?
C38 C39 1.392(16) . ?
C38 H38A 0.9500 . ?
C39 C40 1.478(16) . ?
C40 C41 1.344(17) . ?
C41 C42 1.43(2) . ?
C41 H41A 0.9500 . ?
C42 C43 1.36(3) . ?
C42 H42A 0.9500 . ?
C43 C44 1.35(3) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.358(18) . ?
C45 H45A 0.9500 . ?
C46 C47 1.40(2) . ?
C46 H46A 0.9500 . ?
C47 C48 1.39(2) . ?
C47 H47A 0.9500 . ?
C48 C49 1.395(17) . ?
C48 H48A 0.9500 . ?
C49 C50 1.441(16) . ?
C50 C51 1.384(17) . ?
C51 C52 1.399(16) . ?
C51 H51A 0.9500 . ?
C52 C53 1.477(16) . ?
C53 C58 1.380(16) . ?
C53 C54 1.393(17) . ?
C54 C55 1.37(2) . ?
C54 H54A 0.9500 . ?
C55 C56 1.384(19) . ?
C55 H55A 0.9500 . ?
C56 C57 1.385(17) . ?
C56 H56A 0.9500 . ?
C57 C58 1.382(16) . ?
C57 C59 1.462(16) . ?
C58 H58A 0.9500 . ?
C59 C60 1.385(16) . ?
C60 C61 1.377(16) . ?
C60 H60A 0.9500 . ?
C61 C62 1.499(16) . ?
C62 C63 1.377(18) . ?
C63 C64 1.414(19) . ?
C63 H63A 0.9500 . ?
C64 C65 1.35(2) . ?
C64 H64A 0.9500 . ?
C65 C66 1.35(3) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
Fe2 N28 1.936(9) . ?
Fe2 N22 1.950(9) . ?
Fe2 N34 1.962(8) . ?
Fe2 N33 1.972(9) . ?
Fe2 N21 1.999(9) . ?
Fe2 N27 2.003(9) . ?
N21 C75 1.352(15) . ?
N21 C71 1.361(16) . ?
N22 N23 1.342(12) . ?
N22 C76 1.351(13) . ?
N23 C78 1.369(13) . ?
N23 H23B 0.8800 . ?
N24 N25 1.353(12) . ?
N24 C85 1.357(13) . ?
N24 H24B 0.8800 . ?
N25 C87 1.350(14) . ?
N26 C92 1.331(16) . ?
N26 C88 1.372(15) . ?
N27 C97 1.338(15) . ?
N27 C93 1.351(15) . ?
N28 N29 1.340(12) . ?
N28 C98 1.347(14) . ?
N29 C100 1.363(14) . ?
N29 H29B 0.8800 . ?
N30 C107 1.359(14) . ?
N30 N31 1.372(13) . ?
N30 H30A 0.8800 . ?
N31 C109 1.341(14) . ?
N32 C114 1.363(16) . ?
N32 C110 1.372(15) . ?
N33 C115 1.341(15) . ?
N33 C119 1.384(14) . ?
N34 C120 1.343(13) . ?
N34 N35 1.343(12) . ?
N35 C122 1.383(13) . ?
N35 H35A 0.8800 . ?
N36 C129 1.347(14) . ?
N36 N37 1.348(12) . ?
N36 H36B 0.8800 . ?
N37 C131 1.324(15) . ?
N38 C132 1.325(18) . ?
N38 C136 1.34(2) . ?
C71 C72 1.387(19) . ?
C71 H71A 0.9500 . ?
C72 C73 1.41(2) . ?
C72 H72A 0.9500 . ?
C73 C74 1.35(2) . ?
C73 H73A 0.9500 . ?
C74 C75 1.405(17) . ?
C74 H74A 0.9500 . ?
C75 C76 1.449(16) . ?
C76 C77 1.381(16) . ?
C77 C78 1.403(15) . ?
C77 H77A 0.9500 . ?
C78 C79 1.438(15) . ?
C79 C80 1.395(15) . ?
C79 C84 1.398(15) . ?
C80 C81 1.386(16) . ?
C80 H80A 0.9500 . ?
C81 C82 1.376(16) . ?
C81 H81A 0.9500 . ?
C82 C83 1.390(15) . ?
C82 H82A 0.9500 . ?
C83 C84 1.401(15) . ?
C83 C85 1.459(15) . ?
C84 H84A 0.9500 . ?
C85 C86 1.366(16) . ?
C86 C87 1.387(15) . ?
C86 H86A 0.9500 . ?
C87 C88 1.469(16) . ?
C88 C89 1.366(16) . ?
C89 C90 1.389(18) . ?
C89 H89A 0.9500 . ?
C90 C91 1.371(19) . ?
C90 H90A 0.9500 . ?
C91 C92 1.38(2) . ?
C91 H91A 0.9500 . ?
C92 H92A 0.9500 . ?
C93 C94 1.377(18) . ?
C93 H93A 0.9500 . ?
C94 C95 1.36(2) . ?
C94 H94A 0.9500 . ?
C95 C96 1.351(18) . ?
C95 H95A 0.9500 . ?
C96 C97 1.397(17) . ?
C96 H96A 0.9500 . ?
C97 C98 1.467(16) . ?
C98 C99 1.377(16) . ?
C99 C100 1.371(16) . ?
C99 H99A 0.9500 . ?
C100 C101 1.456(16) . ?
C101 C102 1.360(17) . ?
C101 C106 1.416(16) . ?
C102 C103 1.39(2) . ?
C102 H10B 0.9500 . ?
C103 C104 1.38(2) . ?
C103 H10C 0.9500 . ?
C104 C105 1.405(17) . ?
C104 H10D 0.9500 . ?
C105 C106 1.384(16) . ?
C105 C107 1.441(17) . ?
C106 H10E 0.9500 . ?
C107 C108 1.386(16) . ?
C108 C109 1.394(16) . ?
C108 H10F 0.9500 . ?
C109 C110 1.453(16) . ?
C110 C111 1.355(16) . ?
C111 C112 1.346(18) . ?
C111 H11B 0.9500 . ?
C112 C113 1.41(2) . ?
C112 H11C 0.9500 . ?
C113 C114 1.349(19) . ?
C113 H11D 0.9500 . ?
C114 H11E 0.9500 . ?
C115 C116 1.377(17) . ?
C115 H11F 0.9500 . ?
C116 C117 1.399(19) . ?
C116 H11G 0.9500 . ?
C117 C118 1.342(17) . ?
C117 H11H 0.9500 . ?
C118 C119 1.387(16) . ?
C118 H11I 0.9500 . ?
C119 C120 1.454(16) . ?
C120 C121 1.380(15) . ?
C121 C122 1.387(15) . ?
C121 H12B 0.9500 . ?
C122 C123 1.455(15) . ?
C123 C128 1.398(15) . ?
C123 C124 1.401(15) . ?
C124 C125 1.381(18) . ?
C124 H12C 0.9500 . ?
C125 C126 1.404(18) . ?
C125 H12D 0.9500 . ?
C126 C127 1.392(16) . ?
C126 H12E 0.9500 . ?
C127 C128 1.376(15) . ?
C127 C129 1.469(15) . ?
C128 H12F 0.9500 . ?
C129 C130 1.379(16) . ?
C130 C131 1.416(16) . ?
C130 H13A 0.9500 . ?
C131 C132 1.482(17) . ?
C132 C133 1.40(2) . ?
C133 C134 1.41(2) . ?
C133 H13B 0.9500 . ?
C134 C135 1.33(3) . ?
C134 H13C 0.9500 . ?
C135 C136 1.35(3) . ?
C135 H13D 0.9500 . ?
C136 H13E 0.9500 . ?
P1 F1 1.517(10) . ?
P1 F6 1.520(11) . ?
P1 F2 1.557(10) . ?
P1 F5 1.578(10) . ?
P1 F4 1.597(10) . ?
P1 F3 1.599(11) . ?
P2 F7 1.545(12) . ?
P2 F12 1.559(13) . ?
P2 F8 1.566(12) . ?
P2 F9 1.587(12) . ?
P2 F10 1.588(12) . ?
P2 F11 1.601(12) . ?
P3 F15 1.497(12) . ?
P3 F13 1.506(12) . ?
P3 F16 1.518(12) . ?
P3 F14 1.528(12) . ?
P3 F18 1.606(12) . ?
P3 F17 1.609(12) . ?
I3 I4 2.949(5) . ?
I4 I5 2.923(6) . ?
I6 I7 2.915(12) . ?
I7 I8 2.915(11) . ?
I9 I10 2.949(12) . ?
I10 I11 2.933(11) . ?
O1S C1S 1.423(15) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.458(18) . ?
O2S H2S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
N8 Fe1 N2 96.9(3) . . ?
N8 Fe1 N14 96.5(4) . . ?
N2 Fe1 N14 96.0(3) . . ?
N8 Fe1 N1 174.0(4) . . ?
N2 Fe1 N1 79.9(4) . . ?
N14 Fe1 N1 89.0(4) . . ?
N8 Fe1 N7 80.3(4) . . ?
N2 Fe1 N7 91.6(3) . . ?
N14 Fe1 N7 172.0(3) . . ?
N1 Fe1 N7 94.6(4) . . ?
N8 Fe1 N13 88.6(4) . . ?
N2 Fe1 N13 173.6(4) . . ?
N14 Fe1 N13 80.1(4) . . ?
N1 Fe1 N13 94.9(4) . . ?
N7 Fe1 N13 92.5(4) . . ?
C1 N1 C5 117.1(9) . . ?
C1 N1 Fe1 126.9(7) . . ?
C5 N1 Fe1 115.9(7) . . ?
C6 N2 N3 106.2(8) . . ?
C6 N2 Fe1 116.6(7) . . ?
N3 N2 Fe1 137.3(6) . . ?
N2 N3 C8 110.4(8) . . ?
N2 N3 H3B 124.8 . . ?
C8 N3 H3B 124.8 . . ?
N5 N4 C15 113.1(9) . . ?
N5 N4 H4B 123.5 . . ?
C15 N4 H4B 123.5 . . ?
C17 N5 N4 103.3(9) . . ?
C22 N6 C18 117.4(13) . . ?
C23 N7 C27 117.2(10) . . ?
C23 N7 Fe1 126.7(8) . . ?
C27 N7 Fe1 115.7(7) . . ?
C28 N8 N9 105.3(8) . . ?
C28 N8 Fe1 116.9(7) . . ?
N9 N8 Fe1 137.6(7) . . ?
N8 N9 C30 110.9(8) . . ?
N8 N9 H9A 124.5 . . ?
C30 N9 H9A 124.5 . . ?
C37 N10 N11 112.6(9) . . ?
C37 N10 H10G 123.7 . . ?
N11 N10 H10G 123.7 . . ?
C39 N11 N10 104.8(9) . . ?
C44 N12 C40 116.6(12) . . ?
C45 N13 C49 117.8(10) . . ?
C45 N13 Fe1 127.5(9) . . ?
C49 N13 Fe1 114.6(7) . . ?
C50 N14 N15 106.1(9) . . ?
C50 N14 Fe1 116.4(7) . . ?
N15 N14 Fe1 137.2(7) . . ?
N14 N15 C52 111.0(8) . . ?
N14 N15 H15A 124.5 . . ?
C52 N15 H15A 124.5 . . ?
N17 N16 C59 113.3(9) . . ?
N17 N16 H16B 123.4 . . ?
C59 N16 H16B 123.4 . . ?
C61 N17 N16 104.3(9) . . ?
C66 N18 C62 115.4(14) . . ?
N1 C1 C2 122.4(11) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.8(12) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.0(12) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 C5 119.5(12) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
N1 C5 C4 122.1(11) . . ?
N1 C5 C6 113.0(9) . . ?
C4 C5 C6 124.9(10) . . ?
N2 C6 C7 111.0(9) . . ?
N2 C6 C5 114.7(9) . . ?
C7 C6 C5 134.2(10) . . ?
C8 C7 C6 105.1(9) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
C7 C8 N3 107.3(9) . . ?
C7 C8 C9 130.2(9) . . ?
N3 C8 C9 122.5(9) . . ?
C10 C9 C14 117.6(10) . . ?
C10 C9 C8 120.3(10) . . ?
C14 C9 C8 122.0(9) . . ?
C11 C10 C9 120.2(10) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 122.1(10) . . ?
C10 C11 H11A 118.9 . . ?
C12 C11 H11A 118.9 . . ?
C11 C12 C13 119.8(10) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C14 C13 C12 118.0(10) . . ?
C14 C13 C15 121.1(9) . . ?
C12 C13 C15 121.0(10) . . ?
C13 C14 C9 122.3(9) . . ?
C13 C14 H14A 118.9 . . ?
C9 C14 H14A 118.9 . . ?
N4 C15 C16 105.6(9) . . ?
N4 C15 C13 123.2(9) . . ?
C16 C15 C13 131.1(10) . . ?
C17 C16 C15 104.8(10) . . ?
C17 C16 H16A 127.6 . . ?
C15 C16 H16A 127.6 . . ?
N5 C17 C16 113.2(10) . . ?
N5 C17 C18 121.7(10) . . ?
C16 C17 C18 125.0(10) . . ?
N6 C18 C19 122.2(11) . . ?
N6 C18 C17 116.2(11) . . ?
C19 C18 C17 121.5(11) . . ?
C20 C19 C18 117.4(14) . . ?
C20 C19 H19A 121.3 . . ?
C18 C19 H19A 121.3 . . ?
C21 C20 C19 119.2(16) . . ?
C21 C20 H20A 120.4 . . ?
C19 C20 H20A 120.4 . . ?
C20 C21 C22 119.7(14) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
N6 C22 C21 124.1(15) . . ?
N6 C22 H22A 118.0 . . ?
C21 C22 H22A 118.0 . . ?
N7 C23 C24 121.2(12) . . ?
N7 C23 H23A 119.4 . . ?
C24 C23 H23A 119.4 . . ?
C25 C24 C23 120.7(12) . . ?
C25 C24 H24A 119.6 . . ?
C23 C24 H24A 119.6 . . ?
C24 C25 C26 119.4(13) . . ?
C24 C25 H25A 120.3 . . ?
C26 C25 H25A 120.3 . . ?
C27 C26 C25 117.6(12) . . ?
C27 C26 H26A 121.2 . . ?
C25 C26 H26A 121.2 . . ?
N7 C27 C26 123.7(10) . . ?
N7 C27 C28 112.6(9) . . ?
C26 C27 C28 123.7(11) . . ?
N8 C28 C29 112.2(9) . . ?
N8 C28 C27 114.1(9) . . ?
C29 C28 C27 133.7(10) . . ?
C28 C29 C30 103.4(10) . . ?
C28 C29 H29A 128.3 . . ?
C30 C29 H29A 128.3 . . ?
N9 C30 C29 108.2(9) . . ?
N9 C30 C31 122.1(9) . . ?
C29 C30 C31 129.7(10) . . ?
C32 C31 C36 117.8(10) . . ?
C32 C31 C30 120.5(10) . . ?
C36 C31 C30 121.7(9) . . ?
C33 C32 C31 120.1(11) . . ?
C33 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C32 C33 C34 121.4(11) . . ?
C32 C33 H33A 119.3 . . ?
C34 C33 H33A 119.3 . . ?
C33 C34 C35 119.4(12) . . ?
C33 C34 H34A 120.3 . . ?
C35 C34 H34A 120.3 . . ?
C36 C35 C34 119.5(11) . . ?
C36 C35 C37 120.5(10) . . ?
C34 C35 C37 120.0(10) . . ?
C35 C36 C31 121.7(10) . . ?
C35 C36 H36A 119.2 . . ?
C31 C36 H36A 119.2 . . ?
N10 C37 C38 106.2(9) . . ?
N10 C37 C35 122.6(10) . . ?
C38 C37 C35 131.2(10) . . ?
C37 C38 C39 104.9(10) . . ?
C37 C38 H38A 127.6 . . ?
C39 C38 H38A 127.6 . . ?
N11 C39 C38 111.5(10) . . ?
N11 C39 C40 119.3(10) . . ?
C38 C39 C40 129.2(10) . . ?
C41 C40 N12 123.3(11) . . ?
C41 C40 C39 121.3(11) . . ?
N12 C40 C39 115.4(10) . . ?
C40 C41 C42 117.0(14) . . ?
C40 C41 H41A 121.5 . . ?
C42 C41 H41A 121.5 . . ?
C43 C42 C41 120.7(15) . . ?
C43 C42 H42A 119.7 . . ?
C41 C42 H42A 119.7 . . ?
C44 C43 C42 118.7(15) . . ?
C44 C43 H43A 120.7 . . ?
C42 C43 H43A 120.7 . . ?
C43 C44 N12 123.6(15) . . ?
C43 C44 H44A 118.2 . . ?
N12 C44 H44A 118.2 . . ?
N13 C45 C46 124.2(13) . . ?
N13 C45 H45A 117.9 . . ?
C46 C45 H45A 117.9 . . ?
C45 C46 C47 118.0(13) . . ?
C45 C46 H46A 121.0 . . ?
C47 C46 H46A 121.0 . . ?
C48 C47 C46 119.4(12) . . ?
C48 C47 H47A 120.3 . . ?
C46 C47 H47A 120.3 . . ?
C47 C48 C49 118.1(14) . . ?
C47 C48 H48A 120.9 . . ?
C49 C48 H48A 120.9 . . ?
N13 C49 C48 122.3(11) . . ?
N13 C49 C50 114.7(10) . . ?
C48 C49 C50 122.9(12) . . ?
N14 C50 C51 111.0(10) . . ?
N14 C50 C49 113.8(10) . . ?
C51 C50 C49 135.2(10) . . ?
C50 C51 C52 105.1(10) . . ?
C50 C51 H51A 127.5 . . ?
C52 C51 H51A 127.5 . . ?
N15 C52 C51 106.8(10) . . ?
N15 C52 C53 122.3(9) . . ?
C51 C52 C53 130.9(10) . . ?
C58 C53 C54 118.0(11) . . ?
C58 C53 C52 121.9(10) . . ?
C54 C53 C52 120.1(10) . . ?
C55 C54 C53 120.8(12) . . ?
C55 C54 H54A 119.6 . . ?
C53 C54 H54A 119.6 . . ?
C54 C55 C56 121.1(12) . . ?
C54 C55 H55A 119.5 . . ?
C56 C55 H55A 119.5 . . ?
C55 C56 C57 118.6(13) . . ?
C55 C56 H56A 120.7 . . ?
C57 C56 H56A 120.7 . . ?
C58 C57 C56 120.1(11) . . ?
C58 C57 C59 120.5(10) . . ?
C56 C57 C59 119.4(11) . . ?
C53 C58 C57 121.3(10) . . ?
C53 C58 H58A 119.3 . . ?
C57 C58 H58A 119.3 . . ?
N16 C59 C60 104.4(10) . . ?
N16 C59 C57 122.7(10) . . ?
C60 C59 C57 132.8(10) . . ?
C61 C60 C59 107.3(10) . . ?
C61 C60 H60A 126.3 . . ?
C59 C60 H60A 126.3 . . ?
N17 C61 C60 110.7(10) . . ?
N17 C61 C62 118.9(10) . . ?
C60 C61 C62 130.4(10) . . ?
N18 C62 C63 124.5(12) . . ?
N18 C62 C61 113.8(12) . . ?
C63 C62 C61 121.7(11) . . ?
C62 C63 C64 116.3(13) . . ?
C62 C63 H63A 121.8 . . ?
C64 C63 H63A 121.8 . . ?
C65 C64 C63 119.7(16) . . ?
C65 C64 H64A 120.2 . . ?
C63 C64 H64A 120.2 . . ?
C64 C65 C66 119.2(15) . . ?
C64 C65 H65A 120.4 . . ?
C66 C65 H65A 120.4 . . ?
N18 C66 C65 124.8(15) . . ?
N18 C66 H66A 117.6 . . ?
C65 C66 H66A 117.6 . . ?
N28 Fe2 N22 95.6(4) . . ?
N28 Fe2 N34 96.7(3) . . ?
N22 Fe2 N34 95.1(3) . . ?
N28 Fe2 N33 171.7(4) . . ?
N22 Fe2 N33 92.6(4) . . ?
N34 Fe2 N33 80.8(3) . . ?
N28 Fe2 N21 89.8(4) . . ?
N22 Fe2 N21 80.2(4) . . ?
N34 Fe2 N21 172.3(4) . . ?
N33 Fe2 N21 93.2(4) . . ?
N28 Fe2 N27 80.6(4) . . ?
N22 Fe2 N27 173.5(4) . . ?
N34 Fe2 N27 90.6(3) . . ?
N33 Fe2 N27 91.4(4) . . ?
N21 Fe2 N27 94.4(4) . . ?
C75 N21 C71 117.6(10) . . ?
C75 N21 Fe2 115.4(7) . . ?
C71 N21 Fe2 126.9(9) . . ?
N23 N22 C76 105.7(8) . . ?
N23 N22 Fe2 137.9(7) . . ?
C76 N22 Fe2 116.3(7) . . ?
N22 N23 C78 111.7(8) . . ?
N22 N23 H23B 124.2 . . ?
C78 N23 H23B 124.2 . . ?
N25 N24 C85 112.9(9) . . ?
N25 N24 H24B 123.5 . . ?
C85 N24 H24B 123.5 . . ?
C87 N25 N24 104.0(8) . . ?
C92 N26 C88 117.0(11) . . ?
C97 N27 C93 117.0(10) . . ?
C97 N27 Fe2 114.9(7) . . ?
C93 N27 Fe2 128.1(8) . . ?
N29 N28 C98 105.1(8) . . ?
N29 N28 Fe2 137.9(7) . . ?
C98 N28 Fe2 116.9(7) . . ?
N28 N29 C100 111.5(9) . . ?
N28 N29 H29B 124.3 . . ?
C100 N29 H29B 124.3 . . ?
C107 N30 N31 113.0(9) . . ?
C107 N30 H30A 123.5 . . ?
N31 N30 H30A 123.5 . . ?
C109 N31 N30 103.8(8) . . ?
C114 N32 C110 118.9(11) . . ?
C115 N33 C119 117.5(9) . . ?
C115 N33 Fe2 126.7(8) . . ?
C119 N33 Fe2 115.2(7) . . ?
C120 N34 N35 106.2(8) . . ?
C120 N34 Fe2 116.3(7) . . ?
N35 N34 Fe2 137.4(6) . . ?
N34 N35 C122 110.9(8) . . ?
N34 N35 H35A 124.6 . . ?
C122 N35 H35A 124.6 . . ?
C129 N36 N37 113.5(9) . . ?
C129 N36 H36B 123.2 . . ?
N37 N36 H36B 123.2 . . ?
C131 N37 N36 104.3(9) . . ?
C132 N38 C136 116.1(15) . . ?
N21 C71 C72 122.4(13) . . ?
N21 C71 H71A 118.8 . . ?
C72 C71 H71A 118.8 . . ?
C71 C72 C73 118.4(13) . . ?
C71 C72 H72A 120.8 . . ?
C73 C72 H72A 120.8 . . ?
C74 C73 C72 120.0(12) . . ?
C74 C73 H73A 120.0 . . ?
C72 C73 H73A 120.0 . . ?
C73 C74 C75 119.0(13) . . ?
C73 C74 H74A 120.5 . . ?
C75 C74 H74A 120.5 . . ?
N21 C75 C74 122.6(11) . . ?
N21 C75 C76 113.2(10) . . ?
C74 C75 C76 124.1(11) . . ?
N22 C76 C77 111.2(9) . . ?
N22 C76 C75 114.6(10) . . ?
C77 C76 C75 134.1(10) . . ?
C76 C77 C78 105.3(9) . . ?
C76 C77 H77A 127.3 . . ?
C78 C77 H77A 127.3 . . ?
N23 C78 C77 106.0(9) . . ?
N23 C78 C79 124.0(9) . . ?
C77 C78 C79 129.9(9) . . ?
C80 C79 C84 118.3(10) . . ?
C80 C79 C78 119.4(10) . . ?
C84 C79 C78 122.4(9) . . ?
C81 C80 C79 119.9(10) . . ?
C81 C80 H80A 120.0 . . ?
C79 C80 H80A 120.0 . . ?
C82 C81 C80 121.8(10) . . ?
C82 C81 H81A 119.1 . . ?
C80 C81 H81A 119.1 . . ?
C81 C82 C83 119.4(11) . . ?
C81 C82 H82A 120.3 . . ?
C83 C82 H82A 120.3 . . ?
C82 C83 C84 119.2(10) . . ?
C82 C83 C85 120.3(10) . . ?
C84 C83 C85 120.5(9) . . ?
C79 C84 C83 121.4(9) . . ?
C79 C84 H84A 119.3 . . ?
C83 C84 H84A 119.3 . . ?
N24 C85 C86 105.5(9) . . ?
N24 C85 C83 122.3(10) . . ?
C86 C85 C83 132.1(10) . . ?
C85 C86 C87 106.8(9) . . ?
C85 C86 H86A 126.6 . . ?
C87 C86 H86A 126.6 . . ?
N25 C87 C86 110.7(10) . . ?
N25 C87 C88 120.1(10) . . ?
C86 C87 C88 129.2(10) . . ?
C89 C88 N26 121.6(11) . . ?
C89 C88 C87 122.7(10) . . ?
N26 C88 C87 115.6(10) . . ?
C88 C89 C90 120.2(12) . . ?
C88 C89 H89A 119.9 . . ?
C90 C89 H89A 119.9 . . ?
C91 C90 C89 118.8(12) . . ?
C91 C90 H90A 120.6 . . ?
C89 C90 H90A 120.6 . . ?
C90 C91 C92 118.1(13) . . ?
C90 C91 H91A 121.0 . . ?
C92 C91 H91A 121.0 . . ?
N26 C92 C91 124.3(13) . . ?
N26 C92 H92A 117.9 . . ?
C91 C92 H92A 117.9 . . ?
N27 C93 C94 123.1(12) . . ?
N27 C93 H93A 118.4 . . ?
C94 C93 H93A 118.4 . . ?
C95 C94 C93 118.5(13) . . ?
C95 C94 H94A 120.8 . . ?
C93 C94 H94A 120.8 . . ?
C96 C95 C94 120.1(13) . . ?
C96 C95 H95A 119.9 . . ?
C94 C95 H95A 119.9 . . ?
C95 C96 C97 119.0(12) . . ?
C95 C96 H96A 120.5 . . ?
C97 C96 H96A 120.5 . . ?
N27 C97 C96 122.3(11) . . ?
N27 C97 C98 113.8(10) . . ?
C96 C97 C98 123.9(11) . . ?
N28 C98 C99 111.1(10) . . ?
N28 C98 C97 113.8(10) . . ?
C99 C98 C97 135.2(10) . . ?
C100 C99 C98 105.7(10) . . ?
C100 C99 H99A 127.2 . . ?
C98 C99 H99A 127.2 . . ?
N29 C100 C99 106.6(9) . . ?
N29 C100 C101 123.9(10) . . ?
C99 C100 C101 129.4(10) . . ?
C102 C101 C106 118.3(11) . . ?
C102 C101 C100 121.5(11) . . ?
C106 C101 C100 120.1(10) . . ?
C101 C102 C103 122.3(13) . . ?
C101 C102 H10B 118.9 . . ?
C103 C102 H10B 118.9 . . ?
C104 C103 C102 118.7(12) . . ?
C104 C103 H10C 120.6 . . ?
C102 C103 H10C 120.6 . . ?
C103 C104 C105 121.2(12) . . ?
C103 C104 H10D 119.4 . . ?
C105 C104 H10D 119.4 . . ?
C106 C105 C104 118.0(11) . . ?
C106 C105 C107 121.7(10) . . ?
C104 C105 C107 120.2(11) . . ?
C105 C106 C101 121.3(10) . . ?
C105 C106 H10E 119.4 . . ?
C101 C106 H10E 119.4 . . ?
N30 C107 C108 105.3(10) . . ?
N30 C107 C105 121.6(10) . . ?
C108 C107 C105 133.1(11) . . ?
C107 C108 C109 106.3(10) . . ?
C107 C108 H10F 126.9 . . ?
C109 C108 H10F 126.9 . . ?
N31 C109 C108 111.5(10) . . ?
N31 C109 C110 119.8(10) . . ?
C108 C109 C110 128.6(10) . . ?
C111 C110 N32 121.9(11) . . ?
C111 C110 C109 119.9(10) . . ?
N32 C110 C109 118.2(10) . . ?
C112 C111 C110 119.4(11) . . ?
C112 C111 H11B 120.3 . . ?
C110 C111 H11B 120.3 . . ?
C111 C112 C113 119.5(13) . . ?
C111 C112 H11C 120.3 . . ?
C113 C112 H11C 120.3 . . ?
C114 C113 C112 120.2(12) . . ?
C114 C113 H11D 119.9 . . ?
C112 C113 H11D 119.9 . . ?
C113 C114 N32 120.1(12) . . ?
C113 C114 H11E 119.9 . . ?
N32 C114 H11E 119.9 . . ?
N33 C115 C116 123.0(12) . . ?
N33 C115 H11F 118.5 . . ?
C116 C115 H11F 118.5 . . ?
C115 C116 C117 118.3(12) . . ?
C115 C116 H11G 120.9 . . ?
C117 C116 H11G 120.9 . . ?
C118 C117 C116 120.1(12) . . ?
C118 C117 H11H 119.9 . . ?
C116 C117 H11H 119.9 . . ?
C117 C118 C119 119.7(12) . . ?
C117 C118 H11I 120.1 . . ?
C119 C118 H11I 120.1 . . ?
N33 C119 C118 121.4(10) . . ?
N33 C119 C120 112.8(9) . . ?
C118 C119 C120 125.6(10) . . ?
N34 C120 C121 110.9(9) . . ?
N34 C120 C119 114.5(9) . . ?
C121 C120 C119 134.5(9) . . ?
C120 C121 C122 106.1(9) . . ?
C120 C121 H12B 127.0 . . ?
C122 C121 H12B 127.0 . . ?
N35 C122 C121 105.9(9) . . ?
N35 C122 C123 123.2(9) . . ?
C121 C122 C123 130.9(9) . . ?
C128 C123 C124 118.2(10) . . ?
C128 C123 C122 122.1(9) . . ?
C124 C123 C122 119.7(9) . . ?
C125 C124 C123 120.6(11) . . ?
C125 C124 H12C 119.7 . . ?
C123 C124 H12C 119.7 . . ?
C124 C125 C126 120.4(11) . . ?
C124 C125 H12D 119.8 . . ?
C126 C125 H12D 119.8 . . ?
C127 C126 C125 119.1(11) . . ?
C127 C126 H12E 120.4 . . ?
C125 C126 H12E 120.4 . . ?
C128 C127 C126 120.1(10) . . ?
C128 C127 C129 120.6(10) . . ?
C126 C127 C129 119.2(10) . . ?
C127 C128 C123 121.5(10) . . ?
C127 C128 H12F 119.2 . . ?
C123 C128 H12F 119.2 . . ?
N36 C129 C130 106.0(9) . . ?
N36 C129 C127 121.7(10) . . ?
C130 C129 C127 132.3(10) . . ?
C129 C130 C131 104.7(10) . . ?
C129 C130 H13A 127.6 . . ?
C131 C130 H13A 127.6 . . ?
N37 C131 C130 111.5(10) . . ?
N37 C131 C132 121.7(11) . . ?
C130 C131 C132 126.7(11) . . ?
N38 C132 C133 123.3(12) . . ?
N38 C132 C131 118.0(12) . . ?
C133 C132 C131 118.7(13) . . ?
C132 C133 C134 116.6(15) . . ?
C132 C133 H13B 121.7 . . ?
C134 C133 H13B 121.7 . . ?
C135 C134 C133 120.2(17) . . ?
C135 C134 H13C 119.9 . . ?
C133 C134 H13C 119.9 . . ?
C134 C135 C136 118.6(15) . . ?
C134 C135 H13D 120.7 . . ?
C136 C135 H13D 120.7 . . ?
N38 C136 C135 125.1(17) . . ?
N38 C136 H13E 117.4 . . ?
C135 C136 H13E 117.4 . . ?
F1 P1 F6 94.5(7) . . ?
F1 P1 F2 91.5(6) . . ?
F6 P1 F2 91.8(6) . . ?
F1 P1 F5 90.7(6) . . ?
F6 P1 F5 92.4(6) . . ?
F2 P1 F5 175.1(7) . . ?
F1 P1 F4 176.7(7) . . ?
F6 P1 F4 88.8(6) . . ?
F2 P1 F4 88.7(6) . . ?
F5 P1 F4 88.9(6) . . ?
F1 P1 F3 90.9(6) . . ?
F6 P1 F3 174.4(7) . . ?
F2 P1 F3 89.6(6) . . ?
F5 P1 F3 86.0(6) . . ?
F4 P1 F3 85.8(6) . . ?
F7 P2 F12 96.2(12) . . ?
F7 P2 F8 86.5(10) . . ?
F12 P2 F8 93.9(11) . . ?
F7 P2 F9 86.4(11) . . ?
F12 P2 F9 174.7(11) . . ?
F8 P2 F9 90.8(10) . . ?
F7 P2 F10 174.2(12) . . ?
F12 P2 F10 89.6(12) . . ?
F8 P2 F10 92.5(10) . . ?
F9 P2 F10 87.9(11) . . ?
F7 P2 F11 92.9(11) . . ?
F12 P2 F11 85.1(11) . . ?
F8 P2 F11 178.8(11) . . ?
F9 P2 F11 90.2(10) . . ?
F10 P2 F11 88.1(10) . . ?
F15 P3 F13 99.1(8) . . ?
F15 P3 F16 92.3(7) . . ?
F13 P3 F16 93.7(8) . . ?
F15 P3 F14 94.4(7) . . ?
F13 P3 F14 93.7(7) . . ?
F16 P3 F14 169.2(9) . . ?
F15 P3 F18 85.9(7) . . ?
F13 P3 F18 174.2(8) . . ?
F16 P3 F18 83.1(9) . . ?
F14 P3 F18 88.8(7) . . ?
F15 P3 F17 169.8(10) . . ?
F13 P3 F17 90.9(7) . . ?
F16 P3 F17 84.8(7) . . ?
F14 P3 F17 87.1(7) . . ?
F18 P3 F17 84.0(7) . . ?
I5 I4 I3 166.69(18) . . ?
I6 I7 I8 170.4(7) . . ?
I11 I10 I9 169.6(7) . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4B I1 0.88 2.65 3.514(9) 166.5 .
N10 H10G I1 0.88 2.66 3.506(9) 161.3 .
N16 H16B I1 0.88 2.63 3.480(9) 163.4 .
N24 H24B I1 0.88 2.67 3.529(9) 165.1 .
N30 H30A I1 0.88 2.64 3.484(9) 161.6 .
N36 H36B I1 0.88 2.63 3.480(9) 163.2 .
N3 H3B N31 0.88 2.03 2.842(12) 153.2 .
N9 H9A N37 0.88 2.07 2.844(12) 146.1 .
N15 H15A N25 0.88 2.06 2.871(12) 152.3 .
N23 H23B N17 0.88 2.04 2.828(12) 148.1 .
N29 H29B N5 0.88 2.07 2.887(12) 154.0 .
N35 H35A N11 0.88 2.03 2.806(12) 146.2 .
O1S H1S N26 0.84 2.11 2.800(17) 139.9 .
O2S H2S O1S 0.84 2.11 2.76(3) 133.3 .

_refine_diff_density_max         2.747
_refine_diff_density_min         -3.424
_refine_diff_density_rms         0.196

_shelxl_version_number           2014-3



