# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1447594'
_audit_update_record             
;
2016-01-16 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H36 Fe N14 S2'
_chemical_formula_weight         1073.00

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   7.9450(3)
_cell_length_b                   8.8188(3)
_cell_length_c                   17.5482(7)
_cell_angle_alpha                77.665(2)
_cell_angle_beta                 82.466(2)
_cell_angle_gamma                81.092(2)
_cell_volume                     1180.51(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      29.36

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22108
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4148
_reflns_number_gt                3617
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0332P)²+1.0344P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4148
_refine_ls_number_parameters     349
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.0000 0.01005(11) Uani 1 2 d S . .
S1 S 0.20477(6) 0.06947(6) 0.11318(3) 0.01859(14) Uani 1 1 d . . .
N1 N 0.4014(2) 0.31096(19) 0.04772(9) 0.0140(4) Uani 1 1 d . . .
N2 N 0.63846(19) 0.47580(19) 0.09111(9) 0.0121(3) Uani 1 1 d . . .
N3 N 0.33375(19) 0.61006(19) 0.06929(9) 0.0120(3) Uani 1 1 d . . .
N4 N 0.16559(19) 0.67475(19) 0.06964(9) 0.0130(4) Uani 1 1 d . . .
N5 N 0.25806(19) 0.68079(19) 0.18185(9) 0.0110(3) Uani 1 1 d . . .
N6 N 0.2819(2) 0.72793(19) 0.25132(9) 0.0136(4) Uani 1 1 d . . .
N7 N -0.1032(2) 0.8179(2) 0.22902(9) 0.0151(4) Uani 1 1 d . . .
C1 C 0.3198(2) 0.2118(2) 0.07459(11) 0.0116(4) Uani 1 1 d . . .
C2 C 0.7978(2) 0.4003(2) 0.09820(12) 0.0159(4) Uani 1 1 d . . .
H2 H 0.8544 0.3511 0.0570 0.019 Uiso 1 1 calc R . .
C3 C 0.8825(3) 0.3915(2) 0.16337(12) 0.0183(5) Uani 1 1 d . . .
H3 H 0.9948 0.3365 0.1666 0.022 Uiso 1 1 calc R . .
C4 C 0.8029(3) 0.4632(2) 0.22367(12) 0.0166(4) Uani 1 1 d . . .
H4 H 0.8598 0.4584 0.2687 0.020 Uiso 1 1 calc R . .
C5 C 0.6387(2) 0.5424(2) 0.21754(11) 0.0148(4) Uani 1 1 d . . .
H5 H 0.5811 0.5933 0.2580 0.018 Uiso 1 1 calc R . .
C6 C 0.5613(2) 0.5452(2) 0.15127(11) 0.0115(4) Uani 1 1 d . . .
C7 C 0.3885(2) 0.6159(2) 0.13603(11) 0.0117(4) Uani 1 1 d . . .
C8 C 0.1212(2) 0.7194(2) 0.13712(11) 0.0122(4) Uani 1 1 d . . .
C9 C -0.0489(2) 0.8058(2) 0.15467(11) 0.0128(4) Uani 1 1 d . . .
C10 C -0.1448(3) 0.8707(2) 0.09209(13) 0.0196(5) Uani 1 1 d U . .
H10 H -0.1006 0.8607 0.0401 0.023 Uiso 1 1 calc R . .
C11 C -0.3057(3) 0.9500(3) 0.10708(13) 0.0235(5) Uani 1 1 d . . .
H11 H -0.3751 0.9943 0.0656 0.028 Uiso 1 1 calc R . .
C12 C -0.3642(3) 0.9638(3) 0.18326(13) 0.0216(5) Uani 1 1 d . . .
H12 H -0.4743 1.0177 0.1953 0.026 Uiso 1 1 calc R . .
C13 C -0.2591(2) 0.8976(2) 0.24150(12) 0.0179(5) Uani 1 1 d . . .
H13 H -0.2995 0.9090 0.2936 0.021 Uiso 1 1 calc R . .
C14 C 0.1761(2) 0.6789(2) 0.30974(12) 0.0150(4) Uani 1 1 d . . .
H14 H 0.0980 0.6111 0.3047 0.018 Uiso 1 1 calc R . .
C15 C 0.1766(3) 0.7281(2) 0.38410(11) 0.0150(4) Uani 1 1 d . . .
C16 C 0.3171(3) 0.7937(2) 0.39733(12) 0.0179(4) Uani 1 1 d . . .
H16 H 0.4120 0.8026 0.3583 0.021 Uiso 1 1 calc R . .
C17 C 0.3209(3) 0.8453(2) 0.46538(12) 0.0181(5) Uani 1 1 d . . .
H17 H 0.4181 0.8889 0.4729 0.022 Uiso 1 1 calc R . .
C18 C 0.1827(3) 0.8346(2) 0.52405(12) 0.0162(4) Uani 1 1 d . . .
C19 C 0.1810(3) 0.8904(2) 0.59526(12) 0.0195(5) Uani 1 1 d . . .
H19 H 0.2771 0.9350 0.6034 0.023 Uiso 1 1 calc R . .
C20 C 0.0475(3) 0.8813(2) 0.65053(12) 0.0202(5) Uani 1 1 d . . .
H20 H 0.0505 0.9199 0.6968 0.024 Uiso 1 1 calc R . .
C21 C -0.0997(3) 0.8143(2) 0.64107(12) 0.0174(4) Uani 1 1 d . . .
C22 C -0.2411(3) 0.8046(2) 0.69796(12) 0.0212(5) Uani 1 1 d . . .
H22 H -0.2394 0.8409 0.7450 0.025 Uiso 1 1 calc R . .
C23 C -0.3828(3) 0.7426(3) 0.68609(12) 0.0225(5) Uani 1 1 d . . .
H23 H -0.4782 0.7374 0.7249 0.027 Uiso 1 1 calc R . .
C24 C -0.3870(3) 0.6883(2) 0.61821(12) 0.0208(5) Uani 1 1 d . . .
H24 H -0.4852 0.6454 0.6112 0.025 Uiso 1 1 calc R . .
C25 C -0.2499(3) 0.6954(2) 0.55971(12) 0.0172(4) Uani 1 1 d . . .
C26 C -0.2506(3) 0.6437(2) 0.48766(12) 0.0186(5) Uani 1 1 d . . .
H26 H -0.3479 0.6012 0.4792 0.022 Uiso 1 1 calc R . .
C27 C -0.1172(3) 0.6536(2) 0.43168(12) 0.0165(4) Uani 1 1 d . . .
H27 H -0.1235 0.6191 0.3845 0.020 Uiso 1 1 calc R . .
C28 C 0.0344(3) 0.7148(2) 0.44133(11) 0.0152(4) Uani 1 1 d . . .
C29 C 0.0386(3) 0.7689(2) 0.51205(11) 0.0149(4) Uani 1 1 d . . .
C30 C -0.1029(3) 0.7589(2) 0.57106(11) 0.0158(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.9315(17) 2_665 ?
Fe1 N1 1.9315(17) . ?
Fe1 N3 1.9625(15) 2_665 ?
Fe1 N3 1.9625(15) . ?
Fe1 N2 2.0137(16) 2_665 ?
Fe1 N2 2.0137(16) . ?
S1 C1 1.643(2) . ?
N1 C1 1.152(3) . ?
N2 C2 1.344(2) . ?
N2 C6 1.362(2) . ?
N3 C7 1.315(2) . ?
N3 N4 1.369(2) . ?
N4 C8 1.315(2) . ?
N5 C7 1.357(2) . ?
N5 C8 1.382(2) . ?
N5 N6 1.413(2) . ?
N6 C14 1.281(3) . ?
N7 C9 1.341(3) . ?
N7 C13 1.342(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.451(3) . ?
C8 C9 1.474(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.378(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.461(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(3) . ?
C15 C28 1.411(3) . ?
C16 C17 1.371(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.403(3) . ?
C17 H17 0.9500 . ?
C18 C29 1.418(3) . ?
C18 C19 1.435(3) . ?
C19 C20 1.340(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.432(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.402(3) . ?
C21 C30 1.420(3) . ?
C22 C23 1.383(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.395(3) . ?
C24 H24 0.9500 . ?
C25 C30 1.424(3) . ?
C25 C26 1.434(3) . ?
C26 C27 1.347(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.437(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.427(3) . ?
C29 C30 1.425(3) . ?

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
N1 Fe1 N1 180.00(10) 2_665 . ?
N1 Fe1 N3 88.05(7) 2_665 2_665 ?
N1 Fe1 N3 91.95(7) . 2_665 ?
N1 Fe1 N3 91.95(7) 2_665 . ?
N1 Fe1 N3 88.05(7) . . ?
N3 Fe1 N3 180.00(11) 2_665 . ?
N1 Fe1 N2 91.13(6) 2_665 2_665 ?
N1 Fe1 N2 88.87(6) . 2_665 ?
N3 Fe1 N2 80.27(6) 2_665 2_665 ?
N3 Fe1 N2 99.73(6) . 2_665 ?
N1 Fe1 N2 88.87(6) 2_665 . ?
N1 Fe1 N2 91.13(6) . . ?
N3 Fe1 N2 99.73(6) 2_665 . ?
N3 Fe1 N2 80.28(6) . . ?
N2 Fe1 N2 180.00(5) 2_665 . ?
C1 N1 Fe1 169.94(15) . . ?
C2 N2 C6 117.26(16) . . ?
C2 N2 Fe1 126.99(13) . . ?
C6 N2 Fe1 115.75(12) . . ?
C7 N3 N4 108.75(15) . . ?
C7 N3 Fe1 114.67(13) . . ?
N4 N3 Fe1 136.35(12) . . ?
C8 N4 N3 107.04(15) . . ?
C7 N5 C8 105.28(15) . . ?
C7 N5 N6 123.09(15) . . ?
C8 N5 N6 130.01(15) . . ?
C14 N6 N5 113.23(16) . . ?
C9 N7 C13 116.55(17) . . ?
N1 C1 S1 179.6(2) . . ?
N2 C2 C3 122.41(19) . . ?
N2 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 119.66(18) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 118.96(19) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 118.33(18) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
N2 C6 C5 123.37(17) . . ?
N2 C6 C7 110.40(16) . . ?
C5 C6 C7 126.20(18) . . ?
N3 C7 N5 109.29(16) . . ?
N3 C7 C6 118.83(17) . . ?
N5 C7 C6 131.64(17) . . ?
N4 C8 N5 109.59(16) . . ?
N4 C8 C9 121.45(17) . . ?
N5 C8 C9 128.85(17) . . ?
N7 C9 C10 123.50(18) . . ?
N7 C9 C8 119.17(17) . . ?
C10 C9 C8 117.33(17) . . ?
C11 C10 C9 118.5(2) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 118.9(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C13 C12 C11 118.53(19) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N7 C13 C12 123.98(19) . . ?
N7 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
N6 C14 C15 119.51(18) . . ?
N6 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C28 119.95(18) . . ?
C16 C15 C14 119.48(18) . . ?
C28 C15 C14 120.54(18) . . ?
C17 C16 C15 121.42(19) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 120.79(19) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C29 118.92(18) . . ?
C17 C18 C19 122.21(19) . . ?
C29 C18 C19 118.87(19) . . ?
C20 C19 C18 121.7(2) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C21 121.2(2) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C30 119.3(2) . . ?
C22 C21 C20 122.05(19) . . ?
C30 C21 C20 118.63(19) . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 120.6(2) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 121.2(2) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C30 118.89(19) . . ?
C24 C25 C26 123.0(2) . . ?
C30 C25 C26 118.10(18) . . ?
C27 C26 C25 121.8(2) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C26 C27 C28 121.82(19) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C15 C28 C29 118.48(18) . . ?
C15 C28 C27 123.68(18) . . ?
C29 C28 C27 117.81(18) . . ?
C18 C29 C30 119.29(18) . . ?
C18 C29 C28 120.45(18) . . ?
C30 C29 C28 120.26(19) . . ?
C21 C30 C25 119.48(19) . . ?
C21 C30 C29 120.31(19) . . ?
C25 C30 C29 120.20(18) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1447595'
_audit_update_record             
;
2016-01-16 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H36 Fe N14 S2'
_chemical_formula_weight         1073.00

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   8.0020(6)
_cell_length_b                   9.1057(7)
_cell_length_c                   17.7358(14)
_cell_angle_alpha                76.787(4)
_cell_angle_beta                 82.257(4)
_cell_angle_gamma                80.099(4)
_cell_volume                     1233.20(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    277(2)
_cell_measurement_reflns_used    7555
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      24.04

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8998
_exptl_absorpt_correction_T_max  0.9155
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      277(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23829
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4342
_reflns_number_gt                3091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0421P)²+0.3185P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4342
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.0000 0.03534(17) Uani 1 2 d S . .
S1 S 0.18379(11) -0.41147(9) 0.11627(5) 0.0649(3) Uani 1 1 d . . .
N1 N 0.3934(3) -0.1935(3) 0.05634(14) 0.0582(7) Uani 1 1 d . . .
N2 N 0.6397(2) -0.0130(2) 0.10039(11) 0.0404(5) Uani 1 1 d . . .
N3 N 0.3269(2) 0.1221(2) 0.07377(11) 0.0402(5) Uani 1 1 d . . .
N4 N 0.1610(2) 0.1883(2) 0.07362(12) 0.0428(5) Uani 1 1 d . . .
N5 N 0.2537(2) 0.1932(2) 0.18386(11) 0.0343(5) Uani 1 1 d . . .
N6 N 0.2766(2) 0.2365(2) 0.25292(11) 0.0394(5) Uani 1 1 d . . .
N7 N -0.1060(3) 0.3331(3) 0.22907(12) 0.0488(6) Uani 1 1 d . . .
C1 C 0.3061(3) -0.2834(3) 0.08046(15) 0.0411(6) Uani 1 1 d . . .
C2 C 0.7987(3) -0.0826(3) 0.10965(17) 0.0518(7) Uani 1 1 d . . .
H2 H 0.8581 -0.1304 0.0709 0.062 Uiso 1 1 calc R . .
C3 C 0.8784(3) -0.0866(3) 0.17418(18) 0.0565(8) Uani 1 1 d . . .
H3 H 0.9891 -0.1368 0.1790 0.068 Uiso 1 1 calc R . .
C4 C 0.7933(3) -0.0164(3) 0.23067(17) 0.0526(7) Uani 1 1 d . . .
H4 H 0.8450 -0.0186 0.2749 0.063 Uiso 1 1 calc R . .
C5 C 0.6292(3) 0.0586(3) 0.22225(15) 0.0450(7) Uani 1 1 d . . .
H5 H 0.5699 0.1088 0.2601 0.054 Uiso 1 1 calc R . .
C6 C 0.5557(3) 0.0576(3) 0.15680(14) 0.0346(6) Uani 1 1 d . . .
C7 C 0.3821(3) 0.1265(3) 0.13944(13) 0.0334(6) Uani 1 1 d . . .
C8 C 0.1167(3) 0.2330(3) 0.13987(14) 0.0365(6) Uani 1 1 d . . .
C9 C -0.0526(3) 0.3192(3) 0.15644(15) 0.0381(6) Uani 1 1 d . . .
C10 C -0.1487(3) 0.3811(3) 0.09494(17) 0.0569(8) Uani 1 1 d . . .
H10 H -0.1068 0.3694 0.0448 0.068 Uiso 1 1 calc R . .
C11 C -0.3073(4) 0.4600(4) 0.10905(19) 0.0720(10) Uani 1 1 d . . .
H11 H -0.3753 0.5020 0.0686 0.086 Uiso 1 1 calc R . .
C12 C -0.3644(4) 0.4764(4) 0.18295(19) 0.0673(9) Uani 1 1 d . . .
H12 H -0.4716 0.5298 0.1939 0.081 Uiso 1 1 calc R . .
C13 C -0.2613(3) 0.4129(3) 0.24010(17) 0.0578(8) Uani 1 1 d . . .
H13 H -0.3008 0.4256 0.2903 0.069 Uiso 1 1 calc R . .
C14 C 0.1721(3) 0.1898(3) 0.31027(14) 0.0406(6) Uani 1 1 d . . .
H14 H 0.0961 0.1269 0.3051 0.049 Uiso 1 1 calc R . .
C15 C 0.1707(3) 0.2346(3) 0.38449(14) 0.0394(6) Uani 1 1 d . . .
C16 C 0.3080(3) 0.2991(3) 0.39739(15) 0.0477(7) Uani 1 1 d . . .
H16 H 0.3997 0.3101 0.3593 0.057 Uiso 1 1 calc R . .
C17 C 0.3096(4) 0.3462(3) 0.46497(16) 0.0526(7) Uani 1 1 d . . .
H17 H 0.4028 0.3881 0.4723 0.063 Uiso 1 1 calc R . .
C18 C 0.1741(3) 0.3325(3) 0.52328(14) 0.0450(7) Uani 1 1 d . . .
C19 C 0.1714(4) 0.3848(3) 0.59403(16) 0.0551(8) Uani 1 1 d . . .
H19 H 0.2634 0.4277 0.6018 0.066 Uiso 1 1 calc R . .
C20 C 0.0395(4) 0.3730(3) 0.64897(16) 0.0577(8) Uani 1 1 d . . .
H20 H 0.0415 0.4086 0.6939 0.069 Uiso 1 1 calc R . .
C21 C -0.1043(4) 0.3070(3) 0.64027(15) 0.0507(7) Uani 1 1 d . . .
C22 C -0.2437(4) 0.2943(4) 0.69617(16) 0.0620(9) Uani 1 1 d . . .
H22 H -0.2434 0.3276 0.7420 0.074 Uiso 1 1 calc R . .
C23 C -0.3806(4) 0.2340(4) 0.68509(18) 0.0682(9) Uani 1 1 d . . .
H23 H -0.4728 0.2275 0.7231 0.082 Uiso 1 1 calc R . .
C24 C -0.3840(4) 0.1827(3) 0.61817(16) 0.0600(8) Uani 1 1 d . . .
H24 H -0.4782 0.1414 0.6117 0.072 Uiso 1 1 calc R . .
C25 C -0.2482(3) 0.1919(3) 0.56013(15) 0.0468(7) Uani 1 1 d . . .
C26 C -0.2476(3) 0.1440(3) 0.48868(16) 0.0517(7) Uani 1 1 d . . .
H26 H -0.3407 0.1029 0.4806 0.062 Uiso 1 1 calc R . .
C27 C -0.1163(3) 0.1566(3) 0.43303(15) 0.0471(7) Uani 1 1 d . . .
H27 H -0.1216 0.1249 0.3873 0.057 Uiso 1 1 calc R . .
C28 C 0.0314(3) 0.2174(3) 0.44195(14) 0.0389(6) Uani 1 1 d . . .
C29 C 0.0346(3) 0.2675(3) 0.51196(14) 0.0382(6) Uani 1 1 d . . .
C30 C -0.1057(3) 0.2544(3) 0.57077(14) 0.0416(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.077(3) 2_655 ?
Fe1 N1 2.077(3) . ?
Fe1 N3 2.1243(19) . ?
Fe1 N3 2.1243(19) 2_655 ?
Fe1 N2 2.197(2) . ?
Fe1 N2 2.197(2) 2_655 ?
S1 C1 1.615(3) . ?
N1 C1 1.139(3) . ?
N2 C2 1.334(3) . ?
N2 C6 1.353(3) . ?
N3 C7 1.311(3) . ?
N3 N4 1.361(3) . ?
N4 C8 1.315(3) . ?
N5 C7 1.353(3) . ?
N5 C8 1.381(3) . ?
N5 N6 1.412(3) . ?
N6 C14 1.269(3) . ?
N7 C9 1.329(3) . ?
N7 C13 1.341(3) . ?
C2 C3 1.374(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.355(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.465(3) . ?
C8 C9 1.473(3) . ?
C9 C10 1.377(3) . ?
C10 C11 1.368(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.362(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.355(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.463(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.398(3) . ?
C15 C28 1.410(3) . ?
C16 C17 1.364(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(4) . ?
C17 H17 0.9300 . ?
C18 C29 1.407(4) . ?
C18 C19 1.436(3) . ?
C19 C20 1.338(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.427(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.391(4) . ?
C21 C30 1.423(3) . ?
C22 C23 1.361(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.376(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(4) . ?
C24 H24 0.9300 . ?
C25 C30 1.411(4) . ?
C25 C26 1.430(4) . ?
C26 C27 1.342(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.429(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.422(3) . ?
C29 C30 1.427(3) . ?

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
N1 Fe1 N1 180.00(17) 2_655 . ?
N1 Fe1 N3 92.29(9) 2_655 . ?
N1 Fe1 N3 87.71(9) . . ?
N1 Fe1 N3 87.71(9) 2_655 2_655 ?
N1 Fe1 N3 92.29(9) . 2_655 ?
N3 Fe1 N3 180.00(13) . 2_655 ?
N1 Fe1 N2 88.94(9) 2_655 . ?
N1 Fe1 N2 91.06(9) . . ?
N3 Fe1 N2 75.45(7) . . ?
N3 Fe1 N2 104.55(7) 2_655 . ?
N1 Fe1 N2 91.06(9) 2_655 2_655 ?
N1 Fe1 N2 88.94(9) . 2_655 ?
N3 Fe1 N2 104.55(7) . 2_655 ?
N3 Fe1 N2 75.45(7) 2_655 2_655 ?
N2 Fe1 N2 180.00(5) . 2_655 ?
C1 N1 Fe1 166.0(2) . . ?
C2 N2 C6 118.0(2) . . ?
C2 N2 Fe1 125.70(18) . . ?
C6 N2 Fe1 116.25(15) . . ?
C7 N3 N4 108.83(18) . . ?
C7 N3 Fe1 115.55(15) . . ?
N4 N3 Fe1 135.30(15) . . ?
C8 N4 N3 107.40(19) . . ?
C7 N5 C8 105.56(18) . . ?
C7 N5 N6 123.56(19) . . ?
C8 N5 N6 129.71(19) . . ?
C14 N6 N5 113.5(2) . . ?
C9 N7 C13 116.2(2) . . ?
N1 C1 S1 178.9(3) . . ?
N2 C2 C3 122.6(3) . . ?
N2 C2 H2 118.7 . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 119.0(2) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N2 C6 C5 122.0(2) . . ?
N2 C6 C7 112.0(2) . . ?
C5 C6 C7 126.0(2) . . ?
N3 C7 N5 109.2(2) . . ?
N3 C7 C6 120.7(2) . . ?
N5 C7 C6 130.0(2) . . ?
N4 C8 N5 109.0(2) . . ?
N4 C8 C9 121.5(2) . . ?
N5 C8 C9 129.4(2) . . ?
N7 C9 C10 123.1(2) . . ?
N7 C9 C8 119.3(2) . . ?
C10 C9 C8 117.6(2) . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C12 C11 C10 119.3(3) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 H12 120.8 . . ?
C11 C12 H12 120.8 . . ?
N7 C13 C12 124.4(3) . . ?
N7 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
N6 C14 C15 120.2(2) . . ?
N6 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C28 119.9(2) . . ?
C16 C15 C14 119.2(2) . . ?
C28 C15 C14 120.9(2) . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 121.2(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C29 118.9(2) . . ?
C17 C18 C19 122.1(3) . . ?
C29 C18 C19 118.9(2) . . ?
C20 C19 C18 121.5(3) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 121.6(3) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C30 118.8(3) . . ?
C22 C21 C20 122.8(3) . . ?
C30 C21 C20 118.3(3) . . ?
C23 C22 C21 121.2(3) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 120.7(3) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 120.9(3) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C30 119.1(3) . . ?
C24 C25 C26 123.0(3) . . ?
C30 C25 C26 117.9(2) . . ?
C27 C26 C25 121.8(3) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C26 C27 C28 122.0(2) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
C15 C28 C29 118.5(2) . . ?
C15 C28 C27 123.8(2) . . ?
C29 C28 C27 117.7(2) . . ?
C18 C29 C28 120.5(2) . . ?
C18 C29 C30 119.5(2) . . ?
C28 C29 C30 120.0(2) . . ?
C25 C30 C21 119.3(2) . . ?
C25 C30 C29 120.5(2) . . ?
C21 C30 C29 120.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.047
