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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C36 H36 Fe N6), 4(Cl O4), 3(C N S), 12(O), Cl'
_chemical_formula_sum            'C147 H144 Cl5 Fe4 N27 O28 S3'
_chemical_formula_weight         3233.72

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   10.771(2)
_cell_length_b                   27.332(8)
_cell_length_c                   14.263(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.59(3)
_cell_angle_gamma                90.00
_cell_volume                     4098.0(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6362
_cell_measurement_theta_min      3.1580
_cell_measurement_theta_max      28.6060

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1676
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17634
_diffrn_reflns_av_R_equivalents  0.1436
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3620
_reflns_number_gt                2091
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0893P)²+17.8097P] 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         3620
_refine_ls_number_parameters     282
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0889
_refine_ls_wR_factor_ref         0.2421
_refine_ls_wR_factor_gt          0.2032
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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 0.34707(4) 0.2500 0.0374(4) Uani 1 2 d S . .
N1 N 0.6375(5) 0.34457(18) 0.3657(3) 0.0416(12) Uani 1 1 d . . .
N2 N 0.4299(5) 0.29601(17) 0.3202(4) 0.0418(13) Uani 1 1 d . . .
N3 N 0.4280(5) 0.40185(18) 0.3106(3) 0.0434(13) Uani 1 1 d . . .
C1 C 0.3575(7) 0.2207(2) 0.4297(5) 0.0548(18) Uani 1 1 d . . .
C2 C 0.4626(6) 0.4475(2) 0.2864(4) 0.0445(15) Uani 1 1 d . . .
C3 C 0.4997(6) 0.2850(2) 0.4089(4) 0.0419(15) Uani 1 1 d . . .
C4 C 0.8015(7) 0.3438(3) 0.5485(5) 0.0561(18) Uani 1 1 d . . .
C5 C 0.2849(7) 0.2326(2) 0.3404(6) 0.0597(19) Uani 1 1 d . . .
H5 H 0.2105 0.2155 0.3155 0.072 Uiso 1 1 calc R . .
C6 C 0.7438(6) 0.3714(2) 0.3849(5) 0.0509(17) Uani 1 1 d . . .
H6 H 0.7627 0.3908 0.3363 0.061 Uiso 1 1 calc R . .
C7 C 0.4256(7) 0.4893(3) 0.3273(5) 0.064(2) Uani 1 1 d . . .
H7 H 0.4495 0.5198 0.3085 0.076 Uiso 1 1 calc R . .
C8 C 0.8269(7) 0.3716(3) 0.4736(5) 0.0559(18) Uani 1 1 d . . .
H8 H 0.9004 0.3905 0.4831 0.067 Uiso 1 1 calc R . .
C9 C 0.4639(7) 0.2479(2) 0.4643(5) 0.0528(18) Uani 1 1 d . . .
H9 H 0.5128 0.2415 0.5253 0.063 Uiso 1 1 calc R . .
C10 C 0.6933(7) 0.3148(3) 0.5282(5) 0.0544(18) Uani 1 1 d . . .
H10 H 0.6735 0.2949 0.5759 0.065 Uiso 1 1 calc R . .
C11 C 0.6148(6) 0.3152(2) 0.4375(4) 0.0433(15) Uani 1 1 d . . .
C12 C 0.3511(8) 0.4859(3) 0.3980(5) 0.069(2) Uani 1 1 d . . .
C13 C 0.3233(7) 0.2702(2) 0.2882(5) 0.0509(17) Uani 1 1 d . . .
H13 H 0.2730 0.2778 0.2283 0.061 Uiso 1 1 calc R . .
C14 C 0.3553(7) 0.3992(3) 0.3765(5) 0.059(2) Uani 1 1 d . . .
H14 H 0.3297 0.3685 0.3932 0.070 Uiso 1 1 calc R . .
C15 C 0.3197(9) 0.1775(3) 0.4863(6) 0.082(3) Uani 1 1 d . . .
H15A H 0.3663 0.1791 0.5518 0.123 Uiso 1 1 calc R . .
H15B H 0.3392 0.1473 0.4580 0.123 Uiso 1 1 calc R . .
H15C H 0.2302 0.1789 0.4844 0.123 Uiso 1 1 calc R . .
C16 C 0.3173(8) 0.4396(3) 0.4200(6) 0.071(2) Uani 1 1 d . . .
H16 H 0.2677 0.4356 0.4653 0.085 Uiso 1 1 calc R . .
C17 C 0.8837(8) 0.3464(3) 0.6485(5) 0.080(2) Uani 1 1 d . . .
H17A H 0.9124 0.3141 0.6693 0.121 Uiso 1 1 calc R . .
H17B H 0.8352 0.3597 0.6915 0.121 Uiso 1 1 calc R . .
H17C H 0.9558 0.3670 0.6483 0.121 Uiso 1 1 calc R . .
C18 C 0.3121(10) 0.5306(3) 0.4439(7) 0.098(3) Uani 1 1 d . . .
H18A H 0.2309 0.5416 0.4080 0.146 Uiso 1 1 calc R . .
H18B H 0.3742 0.5559 0.4448 0.146 Uiso 1 1 calc R . .
H18C H 0.3060 0.5232 0.5085 0.146 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.13156(13) 0.2500 0.1204(16) Uani 1 2 d SDU . .
O1 O -0.1106(9) 0.1052(3) 0.2171(11) 0.240(6) Uani 1 1 d DU . .
O2 O 0.0163(13) 0.1685(5) 0.1835(9) 0.274(7) Uani 1 1 d DU . .
S1 S 0.5000 0.1840(7) 0.7500 0.192(6) Uani 0.75 2 d SPDU A 1
N4 N 0.5000 0.0786(8) 0.7500 0.224(10) Uani 0.75 2 d SPDU A 1
C19 C 0.5000 0.1204(7) 0.7500 0.120(7) Uani 0.75 2 d SPDU A 1
Cl2 Cl 0.5000 0.1734(11) 0.7500 0.109(8) Uani 0.25 2 d SPDU . 2
O3 O 0.599(3) 0.1393(12) 0.793(2) 0.155(10) Uani 0.25 1 d PDU B 2
O4 O 0.471(3) 0.2019(13) 0.8285(17) 0.171(11) Uani 0.25 1 d PDU C 2
O1W O 0.3508(16) 0.0598(7) 0.3663(12) 0.155(6) Uani 0.50 1 d PU . .
O2W O 0.512(3) 0.0201(14) 0.554(3) 0.169(9) Uani 0.25 1 d PU . .
O3W O 0.5000 -0.0107(12) 0.7500 0.201(9) Uani 0.50 2 d SPU . .


_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 1.964(5) 2_655 ?
Fe1 N1 1.964(5) . ?
Fe1 N2 1.962(5) . ?
Fe1 N2 1.962(5) 2_655 ?
Fe1 N3 1.971(5) 2_655 ?
Fe1 N3 1.971(5) . ?
N1 C6 1.336(8) . ?
N1 C11 1.365(7) . ?
N2 C13 1.340(8) . ?
N2 C3 1.358(7) . ?
N3 C14 1.350(7) . ?
N3 C2 1.368(7) . ?
C1 C9 1.364(10) . ?
C1 C5 1.380(10) . ?
C1 C15 1.536(9) . ?
C2 C7 1.380(8) . ?
C2 C2 1.447(11) 2_655 ?
C3 C9 1.390(8) . ?
C3 C11 1.471(9) . ?
C4 C8 1.385(9) . ?
C4 C10 1.387(10) . ?
C4 C17 1.507(9) . ?
C5 C13 1.383(9) . ?
C5 H5 0.9300 . ?
C6 C8 1.381(9) . ?
C6 H6 0.9300 . ?
C7 C12 1.421(10) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.383(9) . ?
C10 H10 0.9300 . ?
C12 C16 1.371(10) . ?
C12 C18 1.491(10) . ?
C13 H13 0.9300 . ?
C14 C16 1.374(9) . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
Cl1 O1 1.384(7) . ?
Cl1 O1 1.384(7) 2 ?
Cl1 O2 1.423(8) 2 ?
Cl1 O2 1.423(8) . ?
S1 C19 1.736(10) . ?
N4 C19 1.142(10) . ?
Cl2 O3 1.448(10) 2_656 ?
Cl2 O3 1.448(10) . ?
Cl2 O4 1.454(10) . ?
Cl2 O4 1.454(10) 2_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
N1 Fe1 N1 176.0(3) 2_655 . ?
N1 Fe1 N2 95.8(2) 2_655 . ?
N1 Fe1 N2 81.4(2) . . ?
N1 Fe1 N2 81.4(2) 2_655 2_655 ?
N1 Fe1 N2 95.8(2) . 2_655 ?
N2 Fe1 N2 89.3(3) . 2_655 ?
N1 Fe1 N3 87.4(2) 2_655 2_655 ?
N1 Fe1 N3 95.6(2) . 2_655 ?
N2 Fe1 N3 175.1(2) . 2_655 ?
N2 Fe1 N3 94.85(19) 2_655 2_655 ?
N1 Fe1 N3 95.6(2) 2_655 . ?
N1 Fe1 N3 87.4(2) . . ?
N2 Fe1 N3 94.85(19) . . ?
N2 Fe1 N3 175.1(2) 2_655 . ?
N3 Fe1 N3 81.1(3) 2_655 . ?
C6 N1 C11 117.0(5) . . ?
C6 N1 Fe1 127.5(4) . . ?
C11 N1 Fe1 115.2(4) . . ?
C13 N2 C3 117.4(5) . . ?
C13 N2 Fe1 126.7(4) . . ?
C3 N2 Fe1 115.9(4) . . ?
C14 N3 C2 117.2(5) . . ?
C14 N3 Fe1 127.4(4) . . ?
C2 N3 Fe1 115.3(4) . . ?
C9 C1 C5 117.9(6) . . ?
C9 C1 C15 121.8(7) . . ?
C5 C1 C15 120.3(7) . . ?
N3 C2 C7 121.9(6) . . ?
N3 C2 C2 114.0(3) . 2_655 ?
C7 C2 C2 124.1(4) . 2_655 ?
N2 C3 C9 121.7(6) . . ?
N2 C3 C11 113.3(5) . . ?
C9 C3 C11 125.0(6) . . ?
C8 C4 C10 116.8(6) . . ?
C8 C4 C17 122.0(7) . . ?
C10 C4 C17 121.1(7) . . ?
C1 C5 C13 119.7(7) . . ?
C1 C5 H5 120.1 . . ?
C13 C5 H5 120.1 . . ?
N1 C6 C8 123.0(6) . . ?
N1 C6 H6 118.5 . . ?
C8 C6 H6 118.5 . . ?
C2 C7 C12 120.3(7) . . ?
C2 C7 H7 119.8 . . ?
C12 C7 H7 119.8 . . ?
C6 C8 C4 120.4(7) . . ?
C6 C8 H8 119.8 . . ?
C4 C8 H8 119.8 . . ?
C1 C9 C3 120.4(7) . . ?
C1 C9 H9 119.8 . . ?
C3 C9 H9 119.8 . . ?
C11 C10 C4 120.3(6) . . ?
C11 C10 H10 119.9 . . ?
C4 C10 H10 119.9 . . ?
N1 C11 C10 122.3(6) . . ?
N1 C11 C3 113.6(5) . . ?
C10 C11 C3 124.1(6) . . ?
C16 C12 C7 116.3(6) . . ?
C16 C12 C18 122.7(7) . . ?
C7 C12 C18 121.0(7) . . ?
N2 C13 C5 122.8(7) . . ?
N2 C13 H13 118.6 . . ?
C5 C13 H13 118.6 . . ?
N3 C14 C16 123.1(6) . . ?
N3 C14 H14 118.5 . . ?
C16 C14 H14 118.5 . . ?
C1 C15 H15A 109.5 . . ?
C1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C12 121.2(7) . . ?
C14 C16 H16 119.4 . . ?
C12 C16 H16 119.4 . . ?
C4 C17 H17A 109.5 . . ?
C4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 Cl1 O1 117.2(9) . 2 ?
O1 Cl1 O2 111.9(8) . 2 ?
O1 Cl1 O2 111.4(8) 2 2 ?
O1 Cl1 O2 111.4(8) . . ?
O1 Cl1 O2 111.9(8) 2 . ?
O2 Cl1 O2 89.5(13) 2 . ?
N4 C19 S1 180.000(2) . . ?
O3 Cl2 O3 100(4) 2_656 . ?
O3 Cl2 O4 114(2) 2_656 . ?
O3 Cl2 O4 106.4(11) . . ?
O3 Cl2 O4 106.4(11) 2_656 2_656 ?
O3 Cl2 O4 114(2) . 2_656 ?
O4 Cl2 O4 115(3) . 2_656 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1015467'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H36 Fe N6), C Cl N O2 S, 2(C N S), 6(O)'
_chemical_formula_sum            'C75 H72 Cl Fe2 N15 O8 S3'
_chemical_formula_weight         1554.81

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   10.5927(6)
_cell_length_b                   27.0994(14)
_cell_length_c                   14.2354(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.551(5)
_cell_angle_gamma                90.00
_cell_volume                     3988.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    6694
_cell_measurement_theta_min      3.5130
_cell_measurement_theta_max      28.3520

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4368
_exptl_crystal_size_mid          0.3266
_exptl_crystal_size_min          0.1454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      240(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19641
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         27.10
_reflns_number_total             4373
_reflns_number_gt                3577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0639P)²+9.5629P] 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         4373
_refine_ls_number_parameters     281
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1563
_refine_ls_wR_factor_gt          0.1447
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.004

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 0.346619(18) 0.2500 0.02827(18) Uani 1 2 d S . .
N1 N 0.6397(2) 0.34424(8) 0.36578(16) 0.0316(5) Uani 1 1 d . . .
N2 N 0.4298(2) 0.29526(8) 0.32020(16) 0.0312(5) Uani 1 1 d . . .
N3 N 0.4261(2) 0.40174(8) 0.31015(16) 0.0321(5) Uani 1 1 d . . .
C1 C 0.3553(3) 0.21914(11) 0.4304(2) 0.0422(7) Uani 1 1 d . . .
C2 C 0.4604(3) 0.44723(10) 0.2864(2) 0.0345(6) Uani 1 1 d . . .
C3 C 0.5000(3) 0.28456(10) 0.40951(19) 0.0335(6) Uani 1 1 d . . .
C4 C 0.8051(3) 0.34494(11) 0.5485(2) 0.0434(7) Uani 1 1 d . . .
C5 C 0.2831(3) 0.23116(11) 0.3403(2) 0.0457(7) Uani 1 1 d . . .
H5 H 0.2070 0.2135 0.3146 0.055 Uiso 1 1 calc R . .
C6 C 0.7478(3) 0.37163(11) 0.3845(2) 0.0381(6) Uani 1 1 d . . .
H6 H 0.7674 0.3911 0.3348 0.046 Uiso 1 1 calc R . .
C7 C 0.4247(3) 0.48956(11) 0.3283(2) 0.0478(8) Uani 1 1 d . . .
H7 H 0.4510 0.5207 0.3104 0.057 Uiso 1 1 calc R . .
C8 C 0.8313(3) 0.37250(12) 0.4733(2) 0.0451(7) Uani 1 1 d . . .
H8 H 0.9065 0.3919 0.4828 0.054 Uiso 1 1 calc R . .
C9 C 0.4647(3) 0.24727(11) 0.4651(2) 0.0412(7) Uani 1 1 d . . .
H9 H 0.5153 0.2410 0.5268 0.049 Uiso 1 1 calc R . .
C10 C 0.6957(3) 0.31521(12) 0.5284(2) 0.0440(7) Uani 1 1 d . . .
H10 H 0.6755 0.2950 0.5768 0.053 Uiso 1 1 calc R . .
C11 C 0.6166(3) 0.31517(10) 0.4376(2) 0.0346(6) Uani 1 1 d . . .
C12 C 0.3495(3) 0.48596(12) 0.3971(3) 0.0504(8) Uani 1 1 d . . .
C13 C 0.3216(3) 0.26883(11) 0.2879(2) 0.0401(7) Uani 1 1 d . . .
H13 H 0.2702 0.2764 0.2271 0.048 Uiso 1 1 calc R . .
C14 C 0.3525(3) 0.39887(12) 0.3755(2) 0.0467(8) Uani 1 1 d . . .
H14 H 0.3262 0.3675 0.3921 0.056 Uiso 1 1 calc R . .
C15 C 0.3168(4) 0.17724(13) 0.4868(3) 0.0582(9) Uani 1 1 d . . .
H15A H 0.3467 0.1837 0.5551 0.087 Uiso 1 1 calc R . .
H15B H 0.3553 0.1469 0.4702 0.087 Uiso 1 1 calc R . .
H15C H 0.2233 0.1740 0.4718 0.087 Uiso 1 1 calc R . .
C16 C 0.3138(4) 0.43944(13) 0.4195(3) 0.0550(9) Uani 1 1 d . . .
H16 H 0.2625 0.4354 0.4652 0.066 Uiso 1 1 calc R . .
C17 C 0.8886(4) 0.34776(15) 0.6484(3) 0.0612(10) Uani 1 1 d . . .
H17A H 0.9122 0.3147 0.6719 0.092 Uiso 1 1 calc R . .
H17B H 0.8411 0.3639 0.6908 0.092 Uiso 1 1 calc R . .
H17C H 0.9662 0.3665 0.6470 0.092 Uiso 1 1 calc R . .
C18 C 0.3082(5) 0.53135(15) 0.4431(3) 0.0757(13) Uani 1 1 d . . .
H18A H 0.2180 0.5383 0.4150 0.114 Uiso 1 1 calc R . .
H18B H 0.3609 0.5591 0.4322 0.114 Uiso 1 1 calc R . .
H18C H 0.3188 0.5259 0.5117 0.114 Uiso 1 1 calc R . .
S1 S 0.5000 0.18578(16) 0.7500 0.1328(11) Uani 1 2 d SU . .
C19 C 0.5000 0.1269(6) 0.7500 0.122(4) Uani 1 2 d SU . .
N4 N 0.5000 0.0843(7) 0.7500 0.222(7) Uani 1 2 d SU . .
C20 C -0.211(2) 0.0898(9) 0.185(2) 0.124(6) Uani 0.25 1 d PDU A 1
S2 S -0.3522(15) 0.0609(5) 0.1343(10) 0.200(5) Uani 0.25 1 d PDU A 1
N5 N -0.122(3) 0.1138(11) 0.225(4) 0.145(9) Uani 0.25 1 d PDU A 1
Cl1 Cl 0.0000 0.13156(12) 0.2500 0.1005(15) Uani 0.50 2 d SPDU . 2
O1 O 0.0184(15) 0.1551(5) 0.1726(9) 0.218(6) Uani 0.50 1 d PDU B 2
O2 O -0.1016(11) 0.1033(6) 0.2012(16) 0.185(7) Uani 0.50 1 d PDU C 2
O1W O 0.514(4) -0.0135(9) 0.728(4) 0.343(18) Uani 0.50 1 d PU . .
O2W O 0.522(2) 0.0173(9) 0.5641(15) 0.316(11) Uani 0.50 1 d PU . .


_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 1.953(2) . ?
Fe1 N2 1.953(2) 2_655 ?
Fe1 N1 1.962(2) 2_655 ?
Fe1 N1 1.962(2) . ?
Fe1 N3 1.967(2) 2_655 ?
Fe1 N3 1.967(2) . ?
N1 C6 1.342(4) . ?
N1 C11 1.355(4) . ?
N2 C13 1.344(4) . ?
N2 C3 1.357(4) . ?
N3 C14 1.339(4) . ?
N3 C2 1.349(3) . ?
C1 C5 1.382(5) . ?
C1 C9 1.385(4) . ?
C1 C15 1.498(4) . ?
C2 C7 1.383(4) . ?
C2 C2 1.467(5) 2_655 ?
C3 C9 1.384(4) . ?
C3 C11 1.470(4) . ?
C4 C8 1.382(5) . ?
C4 C10 1.389(5) . ?
C4 C17 1.505(4) . ?
C5 C13 1.378(4) . ?
C5 H5 0.9400 . ?
C6 C8 1.377(4) . ?
C6 H6 0.9400 . ?
C7 C12 1.394(5) . ?
C7 H7 0.9400 . ?
C8 H8 0.9400 . ?
C9 H9 0.9400 . ?
C10 C11 1.379(4) . ?
C10 H10 0.9400 . ?
C12 C16 1.373(5) . ?
C12 C18 1.502(4) . ?
C13 H13 0.9400 . ?
C14 C16 1.372(4) . ?
C14 H14 0.9400 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 H16 0.9400 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
S1 C19 1.595(15) . ?
C19 N4 1.154(17) . ?
C20 N5 1.180(11) . ?
C20 S2 1.708(10) . ?
Cl1 O1 1.324(9) 2 ?
Cl1 O1 1.324(9) . ?
Cl1 O2 1.380(10) . ?
Cl1 O2 1.380(10) 2 ?
O1W O1W 0.76(11) 2_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
N2 Fe1 N2 89.07(13) . 2_655 ?
N2 Fe1 N1 96.01(9) . 2_655 ?
N2 Fe1 N1 81.28(9) 2_655 2_655 ?
N2 Fe1 N1 81.28(9) . . ?
N2 Fe1 N1 96.01(9) 2_655 . ?
N1 Fe1 N1 176.24(13) 2_655 . ?
N2 Fe1 N3 174.96(9) . 2_655 ?
N2 Fe1 N3 94.96(9) 2_655 2_655 ?
N1 Fe1 N3 87.60(9) 2_655 2_655 ?
N1 Fe1 N3 95.26(9) . 2_655 ?
N2 Fe1 N3 94.96(9) . . ?
N2 Fe1 N3 174.96(9) 2_655 . ?
N1 Fe1 N3 95.26(9) 2_655 . ?
N1 Fe1 N3 87.60(9) . . ?
N3 Fe1 N3 81.17(13) 2_655 . ?
C6 N1 C11 117.3(2) . . ?
C6 N1 Fe1 127.2(2) . . ?
C11 N1 Fe1 115.23(19) . . ?
C13 N2 C3 117.3(2) . . ?
C13 N2 Fe1 126.59(19) . . ?
C3 N2 Fe1 116.07(18) . . ?
C14 N3 C2 117.2(2) . . ?
C14 N3 Fe1 127.2(2) . . ?
C2 N3 Fe1 115.47(18) . . ?
C5 C1 C9 116.9(3) . . ?
C5 C1 C15 121.1(3) . . ?
C9 C1 C15 122.0(3) . . ?
N3 C2 C7 122.4(3) . . ?
N3 C2 C2 113.82(15) . 2_655 ?
C7 C2 C2 123.82(18) . 2_655 ?
N2 C3 C9 122.0(3) . . ?
N2 C3 C11 113.1(2) . . ?
C9 C3 C11 124.9(3) . . ?
C8 C4 C10 116.9(3) . . ?
C8 C4 C17 121.9(3) . . ?
C10 C4 C17 121.1(3) . . ?
C13 C5 C1 120.5(3) . . ?
C13 C5 H5 119.8 . . ?
C1 C5 H5 119.8 . . ?
N1 C6 C8 122.8(3) . . ?
N1 C6 H6 118.6 . . ?
C8 C6 H6 118.6 . . ?
C2 C7 C12 119.8(3) . . ?
C2 C7 H7 120.1 . . ?
C12 C7 H7 120.1 . . ?
C6 C8 C4 120.3(3) . . ?
C6 C8 H8 119.8 . . ?
C4 C8 H8 119.8 . . ?
C1 C9 C3 120.4(3) . . ?
C1 C9 H9 119.8 . . ?
C3 C9 H9 119.8 . . ?
C11 C10 C4 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C4 C10 H10 119.9 . . ?
N1 C11 C10 122.3(3) . . ?
N1 C11 C3 113.7(2) . . ?
C10 C11 C3 124.0(3) . . ?
C16 C12 C7 117.1(3) . . ?
C16 C12 C18 122.0(3) . . ?
C7 C12 C18 120.9(3) . . ?
N2 C13 C5 122.7(3) . . ?
N2 C13 H13 118.6 . . ?
C5 C13 H13 118.6 . . ?
N3 C14 C16 123.2(3) . . ?
N3 C14 H14 118.4 . . ?
C16 C14 H14 118.4 . . ?
C1 C15 H15A 109.5 . . ?
C1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C12 120.3(3) . . ?
C14 C16 H16 119.8 . . ?
C12 C16 H16 119.8 . . ?
C4 C17 H17A 109.5 . . ?
C4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 S1 180.000(2) . . ?
N5 C20 S2 172(3) . . ?
O1 Cl1 O1 122.3(14) 2 . ?
O1 Cl1 O2 116.6(11) 2 . ?
O1 Cl1 O2 95.1(13) . . ?
O1 Cl1 O2 95.1(13) 2 2 ?
O1 Cl1 O2 116.6(11) . 2 ?
O2 Cl1 O2 112.5(15) . 2 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.072
_database_code_depnum_ccdc_archive 'CCDC 1015468'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_x-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H36 Fe N6), C Cl N O2 S, 2(C N S), 6(O)'
_chemical_formula_sum            'C75 H72 Cl Fe2 N15 O8 S3'
_chemical_formula_weight         1554.81

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   10.4193(6)
_cell_length_b                   26.9922(11)
_cell_length_c                   14.3238(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.761(6)
_cell_angle_gamma                90.00
_cell_volume                     3928.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6362
_cell_measurement_theta_min      3.1580
_cell_measurement_theta_max      28.6060

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4368
_exptl_crystal_size_mid          0.3266
_exptl_crystal_size_min          0.1454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      130(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         27.10
_reflns_number_total             4292
_reflns_number_gt                3539
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0250P)²+26.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4292
_refine_ls_number_parameters     281
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1550
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.004
_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 0.34662(2) 0.2500 0.0267(2) Uani 1 2 d S . .
N1 N 0.6415(3) 0.34438(10) 0.3658(2) 0.0285(6) Uani 1 1 d . . .
N2 N 0.4274(3) 0.29487(10) 0.3193(2) 0.0278(6) Uani 1 1 d . . .
N3 N 0.4246(3) 0.40202(10) 0.3096(2) 0.0287(6) Uani 1 1 d . . .
C1 C 0.3506(4) 0.21894(13) 0.4281(3) 0.0363(9) Uani 1 1 d . . .
C2 C 0.4601(3) 0.44773(12) 0.2863(2) 0.0276(7) Uani 1 1 d . . .
C3 C 0.4980(4) 0.28427(12) 0.4078(3) 0.0304(8) Uani 1 1 d . . .
C4 C 0.8088(4) 0.34494(14) 0.5487(3) 0.0378(9) Uani 1 1 d . . .
C5 C 0.2775(4) 0.23074(14) 0.3384(3) 0.0382(9) Uani 1 1 d . . .
H5 H 0.1993 0.2128 0.3121 0.046 Uiso 1 1 calc R . .
C6 C 0.7516(4) 0.37177(13) 0.3851(3) 0.0332(8) Uani 1 1 d . . .
H6 H 0.7724 0.3913 0.3354 0.040 Uiso 1 1 calc R . .
C7 C 0.4244(4) 0.49016(13) 0.3290(3) 0.0347(8) Uani 1 1 d . . .
H7 H 0.4520 0.5217 0.3115 0.042 Uiso 1 1 calc R . .
C8 C 0.8355(4) 0.37278(14) 0.4734(3) 0.0387(9) Uani 1 1 d . . .
H8 H 0.9126 0.3926 0.4833 0.046 Uiso 1 1 calc R . .
C9 C 0.4620(4) 0.24684(13) 0.4638(3) 0.0345(8) Uani 1 1 d . . .
H9 H 0.5135 0.2405 0.5262 0.041 Uiso 1 1 calc R . .
C10 C 0.6974(4) 0.31508(14) 0.5280(3) 0.0378(9) Uani 1 1 d . . .
H10 H 0.6764 0.2946 0.5765 0.045 Uiso 1 1 calc R . .
C11 C 0.6173(4) 0.31510(12) 0.4374(3) 0.0306(8) Uani 1 1 d . . .
C12 C 0.3486(4) 0.48670(14) 0.3971(3) 0.0380(9) Uani 1 1 d . . .
C13 C 0.3180(4) 0.26865(13) 0.2864(3) 0.0343(8) Uani 1 1 d . . .
H13 H 0.2659 0.2763 0.2249 0.041 Uiso 1 1 calc R . .
C14 C 0.3497(4) 0.39906(14) 0.3744(3) 0.0415(10) Uani 1 1 d . . .
H14 H 0.3222 0.3672 0.3905 0.050 Uiso 1 1 calc R . .
C15 C 0.3111(5) 0.17666(14) 0.4845(3) 0.0459(10) Uani 1 1 d . . .
H15A H 0.3471 0.1821 0.5529 0.069 Uiso 1 1 calc R . .
H15B H 0.3455 0.1455 0.4647 0.069 Uiso 1 1 calc R . .
H15C H 0.2149 0.1749 0.4725 0.069 Uiso 1 1 calc R . .
C16 C 0.3110(4) 0.43969(14) 0.4186(3) 0.0439(10) Uani 1 1 d . . .
H16 H 0.2580 0.4355 0.4642 0.053 Uiso 1 1 calc R . .
C17 C 0.8926(5) 0.34792(17) 0.6486(3) 0.0497(11) Uani 1 1 d . . .
H17A H 0.9185 0.3145 0.6720 0.075 Uiso 1 1 calc R . .
H17B H 0.8423 0.3636 0.6909 0.075 Uiso 1 1 calc R . .
H17C H 0.9715 0.3676 0.6481 0.075 Uiso 1 1 calc R . .
C18 C 0.3075(5) 0.53231(16) 0.4429(4) 0.0532(12) Uani 1 1 d . . .
H18A H 0.2166 0.5407 0.4119 0.080 Uiso 1 1 calc R . .
H18B H 0.3656 0.5599 0.4356 0.080 Uiso 1 1 calc R . .
H18C H 0.3135 0.5261 0.5111 0.080 Uiso 1 1 calc R . .
S1 S 0.5000 0.17995(11) 0.7500 0.0825(7) Uani 1 2 d SU . .
C19 C 0.5000 0.1209(5) 0.7500 0.101(3) Uani 1 2 d SU . .
N4 N 0.5000 0.0776(6) 0.7500 0.177(5) Uani 1 2 d SU . .
C20 C -0.199(2) 0.0941(10) 0.191(3) 0.115(7) Uani 0.25 1 d PDU A 1
S2 S -0.3406(17) 0.0654(5) 0.1379(11) 0.185(5) Uani 0.25 1 d PDU A 1
N5 N -0.102(4) 0.113(2) 0.233(4) 0.151(10) Uani 0.25 1 d PDU A 1
Cl1 Cl 0.0000 0.13099(11) 0.2500 0.0724(15) Uani 0.50 2 d SPDU . 2
O1 O 0.0208(14) 0.1570(5) 0.1755(8) 0.180(6) Uani 0.50 1 d PDU B 2
O2 O -0.1063(14) 0.1027(6) 0.1976(14) 0.192(7) Uani 0.50 1 d PDU C 2
O1W O 0.500(6) -0.0172(7) 0.772(4) 0.253(14) Uani 0.50 1 d PU . .
O2W O 0.5434(19) 0.0123(8) 0.5734(14) 0.241(9) Uani 0.50 1 d PU . .


_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 1.959(3) 2_655 ?
Fe1 N2 1.959(3) . ?
Fe1 N1 1.961(3) 2_655 ?
Fe1 N1 1.961(3) . ?
Fe1 N3 1.969(3) . ?
Fe1 N3 1.969(3) 2_655 ?
N1 C6 1.342(5) . ?
N1 C11 1.362(4) . ?
N2 C13 1.336(5) . ?
N2 C3 1.349(5) . ?
N3 C14 1.340(4) . ?
N3 C2 1.351(4) . ?
C1 C5 1.379(6) . ?
C1 C9 1.383(6) . ?
C1 C15 1.507(5) . ?
C2 C7 1.387(5) . ?
C2 C2 1.468(6) 2_655 ?
C3 C9 1.393(5) . ?
C3 C11 1.478(5) . ?
C4 C10 1.390(6) . ?
C4 C8 1.393(6) . ?
C4 C17 1.505(6) . ?
C5 C13 1.385(5) . ?
C5 H5 0.9500 . ?
C6 C8 1.369(6) . ?
C6 H6 0.9500 . ?
C7 C12 1.388(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.379(5) . ?
C10 H10 0.9500 . ?
C12 C16 1.383(5) . ?
C12 C18 1.501(5) . ?
C13 H13 0.9500 . ?
C14 C16 1.370(5) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
S1 C19 1.595(13) . ?
C19 N4 1.168(15) . ?
C20 N5 1.168(11) . ?
C20 S2 1.693(11) . ?
Cl1 O1 1.335(10) 2 ?
Cl1 O1 1.335(10) . ?
Cl1 O2 1.416(10) . ?
Cl1 O2 1.416(10) 2 ?
O1W O1W 0.63(10) 2_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
N2 Fe1 N2 89.05(16) 2_655 . ?
N2 Fe1 N1 81.49(12) 2_655 2_655 ?
N2 Fe1 N1 95.97(12) . 2_655 ?
N2 Fe1 N1 95.97(12) 2_655 . ?
N2 Fe1 N1 81.49(12) . . ?
N1 Fe1 N1 176.46(16) 2_655 . ?
N2 Fe1 N3 175.15(12) 2_655 . ?
N2 Fe1 N3 94.94(11) . . ?
N1 Fe1 N3 95.32(12) 2_655 . ?
N1 Fe1 N3 87.38(12) . . ?
N2 Fe1 N3 94.94(11) 2_655 2_655 ?
N2 Fe1 N3 175.15(12) . 2_655 ?
N1 Fe1 N3 87.38(12) 2_655 2_655 ?
N1 Fe1 N3 95.32(12) . 2_655 ?
N3 Fe1 N3 81.22(16) . 2_655 ?
C6 N1 C11 117.1(3) . . ?
C6 N1 Fe1 127.3(3) . . ?
C11 N1 Fe1 115.2(2) . . ?
C13 N2 C3 117.7(3) . . ?
C13 N2 Fe1 126.5(2) . . ?
C3 N2 Fe1 115.8(2) . . ?
C14 N3 C2 117.3(3) . . ?
C14 N3 Fe1 127.2(2) . . ?
C2 N3 Fe1 115.4(2) . . ?
C5 C1 C9 117.7(3) . . ?
C5 C1 C15 121.0(4) . . ?
C9 C1 C15 121.4(4) . . ?
N3 C2 C7 122.1(3) . . ?
N3 C2 C2 113.83(18) . 2_655 ?
C7 C2 C2 124.1(2) . 2_655 ?
N2 C3 C9 122.4(3) . . ?
N2 C3 C11 113.6(3) . . ?
C9 C3 C11 124.0(3) . . ?
C10 C4 C8 116.6(4) . . ?
C10 C4 C17 121.0(4) . . ?
C8 C4 C17 122.3(4) . . ?
C1 C5 C13 120.0(4) . . ?
C1 C5 H5 120.0 . . ?
C13 C5 H5 120.0 . . ?
N1 C6 C8 123.0(4) . . ?
N1 C6 H6 118.5 . . ?
C8 C6 H6 118.5 . . ?
C2 C7 C12 120.2(3) . . ?
C2 C7 H7 119.9 . . ?
C12 C7 H7 119.9 . . ?
C6 C8 C4 120.6(4) . . ?
C6 C8 H8 119.7 . . ?
C4 C8 H8 119.7 . . ?
C1 C9 C3 119.5(4) . . ?
C1 C9 H9 120.2 . . ?
C3 C9 H9 120.2 . . ?
C11 C10 C4 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C4 C10 H10 119.9 . . ?
N1 C11 C10 122.3(3) . . ?
N1 C11 C3 113.2(3) . . ?
C10 C11 C3 124.5(3) . . ?
C16 C12 C7 116.9(3) . . ?
C16 C12 C18 122.2(3) . . ?
C7 C12 C18 120.9(4) . . ?
N2 C13 C5 122.7(4) . . ?
N2 C13 H13 118.7 . . ?
C5 C13 H13 118.7 . . ?
N3 C14 C16 123.2(3) . . ?
N3 C14 H14 118.4 . . ?
C16 C14 H14 118.4 . . ?
C1 C15 H15A 109.5 . . ?
C1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C12 120.3(3) . . ?
C14 C16 H16 119.8 . . ?
C12 C16 H16 119.8 . . ?
C4 C17 H17A 109.5 . . ?
C4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 S1 180.000(1) . . ?
N5 C20 S2 176(4) . . ?
O1 Cl1 O1 116.6(13) 2 . ?
O1 Cl1 O2 117.5(11) 2 . ?
O1 Cl1 O2 96.0(11) . . ?
O1 Cl1 O2 96.0(11) 2 2 ?
O1 Cl1 O2 117.5(11) . 2 ?
O2 Cl1 O2 114.8(15) . 2 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.090
_database_code_depnum_ccdc_archive 'CCDC 1015469'
