# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_mpmb2
_database_code_depnum_ccdc_archive 'CCDC 1469277'
_audit_update_record             
;
2016-05-01 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H40 Cl2 Fe2 N6 O13'
_chemical_formula_weight         803.22

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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   C2/c

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                   25.674(10)
_cell_length_b                   7.876(3)
_cell_length_c                   20.102(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.068(10)
_cell_angle_gamma                90.00
_cell_volume                     3407(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    987
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      24.45

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_T_max  0.7108
_exptl_absorpt_process_details   'BRUKER SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFARCTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12986
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3700
_reflns_number_gt                2700
_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    ORTEP
_computing_publication_material  ?

_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)+(0.0775P)²+5.5228P] 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         3700
_refine_ls_number_parameters     256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1414
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O -0.06877(10) -0.1593(3) 0.14636(14) 0.0494(6) Uani 1 1 d . . .
Fe1 Fe 0.068227(18) 0.00274(5) 0.27226(2) 0.03545(16) Uani 1 1 d . . .
O1 O 0.0000 0.1160(4) 0.2500 0.0392(6) Uani 1 2 d S . .
O2 O 0.02953(9) -0.1564(3) 0.18063(13) 0.0483(6) Uani 1 1 d . . .
N1 N 0.15755(11) -0.1215(3) 0.31219(15) 0.0402(6) Uani 1 1 d . . .
N2 N 0.13689(12) 0.1543(4) 0.37231(16) 0.0446(6) Uani 1 1 d . . .
H2C H 0.1213(18) 0.193(5) 0.395(2) 0.057(12) Uiso 1 1 d . . .
N3 N 0.08644(12) 0.1983(4) 0.20688(16) 0.0487(7) Uani 1 1 d . . .
C11 C -0.02735(14) -0.1910(4) 0.13368(18) 0.0425(7) Uani 1 1 d . . .
C5 C 0.20377(14) -0.0862(4) 0.38763(19) 0.0444(7) Uani 1 1 d . . .
C3 C 0.26890(16) -0.2937(5) 0.3824(2) 0.0584(10) Uani 1 1 d . . .
H3 H 0.3060 -0.3540 0.4064 0.070 Uiso 1 1 calc R . .
C2 C 0.22201(16) -0.3262(5) 0.3046(2) 0.0544(9) Uani 1 1 d . . .
H2 H 0.2273 -0.4068 0.2751 0.065 Uiso 1 1 calc R . .
C1 C 0.16783(15) -0.2382(4) 0.2720(2) 0.0470(8) Uani 1 1 d . . .
H1 H 0.1365 -0.2599 0.2195 0.056 Uiso 1 1 calc R . .
C4 C 0.25986(15) -0.1709(5) 0.4235(2) 0.0546(9) Uani 1 1 d . . .
H4 H 0.2914 -0.1449 0.4755 0.066 Uiso 1 1 calc R . .
C6 C 0.19012(16) 0.0466(5) 0.4294(2) 0.0552(9) Uani 1 1 d . . .
H6A H 0.1808 -0.0080 0.4650 0.066 Uiso 1 1 calc R . .
H6B H 0.2266 0.1173 0.4610 0.066 Uiso 1 1 calc R . .
C12 C -0.04548(17) -0.2753(6) 0.0572(2) 0.0672(11) Uani 1 1 d . . .
H12A H -0.0695 -0.3751 0.0499 0.101 Uiso 1 1 calc R . .
H12B H -0.0087 -0.3067 0.0586 0.101 Uiso 1 1 calc R . .
H12C H -0.0698 -0.1983 0.0140 0.101 Uiso 1 1 calc R . .
C7 C 0.15434(19) 0.3019(5) 0.3442(2) 0.0621(10) Uani 1 1 d . . .
H7A H 0.1921 0.2767 0.3460 0.075 Uiso 1 1 calc R . .
H7B H 0.1626 0.3978 0.3789 0.075 Uiso 1 1 calc R . .
C8 C 0.1042(2) 0.3469(6) 0.2618(3) 0.0818(13) Uani 1 1 d . . .
H8A H 0.1181 0.4394 0.2433 0.098 Uiso 1 1 calc R . .
H8B H 0.0681 0.3856 0.2612 0.098 Uiso 1 1 calc R . .
C9 C 0.1310(3) 0.1613(8) 0.1867(4) 0.106(2) Uani 1 1 d . . .
H9A H 0.1165 0.0671 0.1505 0.159 Uiso 1 1 calc R . .
H9B H 0.1702 0.1330 0.2339 0.159 Uiso 1 1 calc R . .
H9C H 0.1359 0.2589 0.1620 0.159 Uiso 1 1 calc R . .
C10 C 0.0281(2) 0.2510(8) 0.1340(3) 0.0994(19) Uani 1 1 d . . .
H10A H 0.0356 0.3498 0.1124 0.149 Uiso 1 1 calc R . .
H10B H -0.0023 0.2770 0.1462 0.149 Uiso 1 1 calc R . .
H10C H 0.0131 0.1605 0.0959 0.149 Uiso 1 1 calc R . .
Cl1 Cl 0.14019(4) 0.72000(12) 0.06026(5) 0.0561(3) Uani 1 1 d . . .
O7 O 0.1312(11) 0.640(4) -0.0085(15) 0.077(5) Uani 0.57 1 d P . .
O7A O 0.1512(14) 0.649(5) 0.004(2) 0.086(8) Uani 0.43 1 d P . .
O6 O 0.1983(9) 0.787(2) 0.1273(11) 0.092(5) Uani 0.44 1 d P . .
O6A O 0.2012(7) 0.735(2) 0.1166(11) 0.140(7) Uani 0.56 1 d P . .
O5 O 0.1132(9) 0.8805(19) 0.0243(12) 0.102(4) Uani 0.56 1 d P . .
O5A O 0.1004(11) 0.860(3) 0.0449(15) 0.136(9) Uani 0.44 1 d P . .
O4A O 0.1024(8) 0.637(3) 0.0754(11) 0.101(6) Uani 0.53 1 d P . .
O4 O 0.1250(10) 0.589(3) 0.0978(12) 0.105(7) Uani 0.47 1 d 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
O3 C11 1.247(4) . ?
O3 Fe1 2.069(2) 2 ?
Fe1 O1 1.7913(16) . ?
Fe1 O2 1.988(2) . ?
Fe1 O3 2.069(2) 2 ?
Fe1 N2 2.170(3) . ?
Fe1 N1 2.203(3) . ?
Fe1 N3 2.234(3) . ?
O1 Fe1 1.7914(16) 2 ?
O2 C11 1.262(4) . ?
N1 C1 1.341(4) . ?
N1 C5 1.349(4) . ?
N2 C7 1.466(5) . ?
N2 C6 1.481(4) . ?
N2 H2C 0.81(4) . ?
N3 C9 1.436(5) . ?
N3 C10 1.472(5) . ?
N3 C8 1.499(6) . ?
C11 C12 1.497(5) . ?
C5 C4 1.380(5) . ?
C5 C6 1.497(5) . ?
C3 C4 1.373(6) . ?
C3 C2 1.379(5) . ?
C3 H3 0.9300 . ?
C2 C1 1.360(5) . ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C4 H4 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C7 C8 1.482(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
Cl1 O4A 1.335(17) . ?
Cl1 O6A 1.347(15) . ?
Cl1 O7 1.42(3) . ?
Cl1 O5A 1.42(2) . ?
Cl1 O7A 1.43(4) . ?
Cl1 O5 1.434(17) . ?
Cl1 O4 1.45(2) . ?
Cl1 O6 1.457(18) . ?
O5 O5A 0.67(2) . ?
O4A O4 0.63(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
C11 O3 Fe1 130.3(2) . 2 ?
O1 Fe1 O2 98.98(8) . . ?
O1 Fe1 O3 95.07(8) . 2 ?
O2 Fe1 O3 97.36(11) . 2 ?
O1 Fe1 N2 98.44(10) . . ?
O2 Fe1 N2 161.44(10) . . ?
O3 Fe1 N2 87.41(11) 2 . ?
O1 Fe1 N1 173.69(8) . . ?
O2 Fe1 N1 87.27(9) . . ?
O3 Fe1 N1 83.19(9) 2 . ?
N2 Fe1 N1 75.45(10) . . ?
O1 Fe1 N3 89.99(10) . . ?
O2 Fe1 N3 92.80(11) . . ?
O3 Fe1 N3 167.79(10) 2 . ?
N2 Fe1 N3 80.84(11) . . ?
N1 Fe1 N3 90.58(10) . . ?
Fe1 O1 Fe1 120.28(16) . 2 ?
C11 O2 Fe1 128.2(2) . . ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Fe1 126.4(2) . . ?
C5 N1 Fe1 114.9(2) . . ?
C7 N2 C6 114.0(3) . . ?
C7 N2 Fe1 110.1(2) . . ?
C6 N2 Fe1 110.0(2) . . ?
C7 N2 H2C 106(3) . . ?
C6 N2 H2C 108(3) . . ?
Fe1 N2 H2C 109(3) . . ?
C9 N3 C10 108.1(4) . . ?
C9 N3 C8 113.4(4) . . ?
C10 N3 C8 104.4(4) . . ?
C9 N3 Fe1 118.7(3) . . ?
C10 N3 Fe1 110.7(2) . . ?
C8 N3 Fe1 100.5(2) . . ?
O3 C11 O2 124.9(3) . . ?
O3 C11 C12 118.5(3) . . ?
O2 C11 C12 116.6(3) . . ?
N1 C5 C4 121.0(3) . . ?
N1 C5 C6 116.2(3) . . ?
C4 C5 C6 122.7(3) . . ?
C4 C3 C2 118.9(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C1 C2 C3 118.8(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
N1 C1 C2 123.0(3) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N2 C6 C5 111.5(3) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C7 C8 111.0(3) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 N3 111.4(4) . . ?
C7 C8 H8A 109.3 . . ?
N3 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
N3 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O4A Cl1 O6A 120.4(11) . . ?
O4A Cl1 O7 104.6(14) . . ?
O6A Cl1 O7 110.7(12) . . ?
O4A Cl1 O5A 84.6(13) . . ?
O6A Cl1 O5A 119.0(14) . . ?
O7 Cl1 O5A 114.8(15) . . ?
O4A Cl1 O7A 118.3(17) . . ?
O6A Cl1 O7A 93.4(15) . . ?
O7 Cl1 O7A 18(2) . . ?
O5A Cl1 O7A 124.2(19) . . ?
O4A Cl1 O5 109.6(10) . . ?
O6A Cl1 O5 111.7(11) . . ?
O7 Cl1 O5 97.1(14) . . ?
O5A Cl1 O5 27.3(10) . . ?
O7A Cl1 O5 101.2(18) . . ?
O4A Cl1 O4 25.6(12) . . ?
O6A Cl1 O4 98.2(12) . . ?
O7 Cl1 O4 104.1(15) . . ?
O5A Cl1 O4 107.5(12) . . ?
O7A Cl1 O4 111.4(19) . . ?
O5 Cl1 O4 134.1(10) . . ?
O4A Cl1 O6 118.0(10) . . ?
O6A Cl1 O6 19.5(15) . . ?
O7 Cl1 O6 127.0(12) . . ?
O5A Cl1 O6 99.9(14) . . ?
O7A Cl1 O6 109.3(14) . . ?
O5 Cl1 O6 96.8(11) . . ?
O4 Cl1 O6 101.8(10) . . ?
O5A O5 Cl1 75(3) . . ?
O5 O5A Cl1 78(3) . . ?
O4 O4A Cl1 88(3) . . ?
O4A O4 Cl1 67(3) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_mprl325
_database_code_depnum_ccdc_archive 'CCDC 1469278'
_audit_update_record             
;
2016-05-01 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H44 Cl2 Fe2 N6 O13'
_chemical_formula_weight         927.35

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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   C2/c

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                   34.8958(8)
_cell_length_b                   11.1865(2)
_cell_length_c                   28.5616(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 127.463(2)
_cell_angle_gamma                90.00
_cell_volume                     8849.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1323
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      23.56

_exptl_crystal_description       PLATES
_exptl_crystal_colour            BROWN
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3840
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7927
_exptl_absorpt_correction_T_max  0.9358
_exptl_absorpt_process_details   'BRUKER SADABS'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.583 0.250 245.7 47.6
2 1.000 0.083 0.250 245.7 47.6
3 0.289 0.000 0.201 6.9 0.0
4 0.789 0.500 0.201 6.9 0.0
5 0.211 0.500 0.299 6.9 0.0
6 0.711 0.000 0.299 6.9 0.0
7 0.500 0.417 0.750 245.7 47.5
8 1.000 0.917 0.750 245.7 47.5
9 0.289 0.000 0.701 6.9 -0.1
10 0.789 0.500 0.701 6.9 -0.1
11 0.211 0.500 0.799 6.9 -0.1
12 0.711 0.000 0.799 6.9 -0.1
_platon_squeeze_details          
; ?
;
_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'omega-phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            73976
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_UnetI/netI     0.0418
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.51
_reflns_number_total             8138
_reflns_number_gt                5348
_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    ORTEP
_computing_publication_material  ?

_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)+(0.1088P)²+1.2535P] 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         8138
_refine_ls_number_parameters     522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1887
_refine_ls_wR_factor_gt          0.1725
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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
C20 C 0.0945(2) 0.5204(6) 0.5974(3) 0.107(2) Uani 1 1 d . . .
H20A H 0.0806 0.4525 0.5715 0.160 Uiso 1 1 calc R . .
H20B H 0.0848 0.5923 0.5744 0.160 Uiso 1 1 calc R . .
H20C H 0.0834 0.5227 0.6210 0.160 Uiso 1 1 calc R . .
C18 C 0.1604(2) 0.3961(5) 0.6700(2) 0.0859(16) Uani 1 1 d . . .
H18A H 0.1562 0.4064 0.7003 0.103 Uiso 1 1 calc R . .
H18B H 0.1381 0.3346 0.6430 0.103 Uiso 1 1 calc R . .
C15 C 0.2816(2) 0.4938(7) 0.6804(2) 0.093(2) Uani 1 1 d . . .
C17 C 0.2107(2) 0.3583(6) 0.6973(2) 0.0876(16) Uani 1 1 d . . .
H17A H 0.2331 0.4155 0.7273 0.105 Uiso 1 1 calc R . .
H17B H 0.2168 0.2810 0.7161 0.105 Uiso 1 1 calc R . .
C16 C 0.26920(18) 0.3620(7) 0.6767(2) 0.0934(18) Uani 1 1 d . . .
H16A H 0.2751 0.3204 0.6518 0.112 Uiso 1 1 calc R . .
H16B H 0.2894 0.3264 0.7157 0.112 Uiso 1 1 calc R . .
C11 C 0.2534(3) 0.6882(6) 0.6509(3) 0.109(2) Uani 1 1 d . . .
H11 H 0.2280 0.7425 0.6304 0.131 Uiso 1 1 calc R . .
C14 C 0.3283(3) 0.5337(11) 0.7136(3) 0.150(4) Uani 1 1 d . . .
H14 H 0.3537 0.4800 0.7354 0.180 Uiso 1 1 calc R . .
C12 C 0.3011(4) 0.7272(10) 0.6838(4) 0.158(5) Uani 1 1 d . . .
H12 H 0.3077 0.8079 0.6844 0.189 Uiso 1 1 calc R . .
C13 C 0.3371(3) 0.6491(14) 0.7145(4) 0.176(6) Uani 1 1 d . . .
H13 H 0.3689 0.6759 0.7367 0.211 Uiso 1 1 calc R . .
O10 O 0.3266(4) 0.4202(7) 0.8189(3) 0.242(4) Uani 1 1 d . . .
O9 O 0.1405(3) 0.3355(8) 0.2922(4) 0.244(4) Uani 1 1 d . . .
Cl2 Cl 0.33792(6) 0.49603(13) 0.86048(6) 0.0823(4) Uani 1 1 d . . .
O12 O 0.3608(3) 0.4385(7) 0.9135(2) 0.221(4) Uani 1 1 d . . .
O13 O 0.3719(3) 0.5751(8) 0.8646(3) 0.223(4) Uani 1 1 d . . .
O11 O 0.3065(5) 0.5648(13) 0.8512(7) 0.388(9) Uani 1 1 d . . .
C19 C 0.1702(3) 0.6144(6) 0.6771(3) 0.126(3) Uani 1 1 d . . .
H19A H 0.1621 0.6859 0.6542 0.189 Uiso 1 1 calc R . .
H19B H 0.2047 0.6063 0.7040 0.189 Uiso 1 1 calc R . .
H19C H 0.1575 0.6190 0.6988 0.189 Uiso 1 1 calc R . .
C9 C 0.1167(3) 0.8793(5) 0.4527(3) 0.119(3) Uani 1 1 d . . .
H9A H 0.0823 0.8705 0.4245 0.178 Uiso 1 1 calc R . .
H9B H 0.1267 0.9506 0.4442 0.178 Uiso 1 1 calc R . .
H9C H 0.1254 0.8846 0.4917 0.178 Uiso 1 1 calc R . .
C10 C 0.1929(2) 0.7871(6) 0.4922(3) 0.115(2) Uani 1 1 d . . .
H10A H 0.2083 0.7190 0.4897 0.173 Uiso 1 1 calc R . .
H10B H 0.2017 0.7919 0.5312 0.173 Uiso 1 1 calc R . .
H10C H 0.2031 0.8585 0.4839 0.173 Uiso 1 1 calc R . .
C8 C 0.1299(3) 0.7664(6) 0.3899(3) 0.109(2) Uani 1 1 d . . .
H8A H 0.1335 0.8449 0.3786 0.131 Uiso 1 1 calc R . .
H8B H 0.1533 0.7137 0.3927 0.131 Uiso 1 1 calc R . .
Fe1 Fe 0.11561(2) 0.60363(5) 0.46060(3) 0.0500(2) Uani 1 1 d . . .
Fe2 Fe 0.17545(2) 0.48951(5) 0.58472(3) 0.0522(2) Uani 1 1 d . . .
Cl1 Cl 0.10942(6) 0.42533(16) 0.27449(6) 0.0949(5) Uani 1 1 d . . .
O3 O 0.12454(10) 0.3617(2) 0.53583(12) 0.0565(7) Uani 1 1 d . . .
O1 O 0.14467(10) 0.6167(2) 0.53781(12) 0.0548(7) Uani 1 1 d . . .
O4 O 0.21017(10) 0.4342(3) 0.55062(13) 0.0576(7) Uani 1 1 d . . .
O2 O 0.08214(10) 0.4436(3) 0.44671(12) 0.0599(8) Uani 1 1 d . . .
O5 O 0.16720(11) 0.5219(3) 0.46195(14) 0.0651(8) Uani 1 1 d . . .
N1 N 0.04602(14) 0.6751(3) 0.42789(17) 0.0592(9) Uani 1 1 d . . .
C22 C 0.24005(15) 0.4260(4) 0.4949(2) 0.0570(11) Uani 1 1 d . . .
N2 N 0.07327(16) 0.6088(4) 0.36324(18) 0.0651(10) Uani 1 1 d . . .
C29 C 0.05271(14) 0.2677(4) 0.45929(18) 0.0503(10) Uani 1 1 d . . .
C28 C 0.08922(14) 0.3652(3) 0.48268(18) 0.0476(9) Uani 1 1 d . . .
N3 N 0.14066(15) 0.7747(3) 0.44931(19) 0.0722(11) Uani 1 1 d . . .
N6 N 0.14944(17) 0.5101(4) 0.63745(19) 0.0735(11) Uani 1 1 d . . .
N4 N 0.24481(18) 0.5708(5) 0.64947(19) 0.0818(13) Uani 1 1 d . . .
C1 C 0.03741(19) 0.7280(4) 0.4631(3) 0.0737(14) Uani 1 1 d . . .
H1 H 0.0626 0.7395 0.5029 0.088 Uiso 1 1 calc R . .
N5 N 0.21807(14) 0.3508(4) 0.65185(17) 0.0693(11) Uani 1 1 d . . .
C21 C 0.20287(16) 0.4641(4) 0.5037(2) 0.0555(11) Uani 1 1 d . . .
C34 C 0.06417(15) 0.1595(4) 0.48748(19) 0.0562(10) Uani 1 1 d . . .
H34 H 0.0953 0.1466 0.5217 0.067 Uiso 1 1 calc R . .
C23 C 0.28297(16) 0.3735(4) 0.5414(2) 0.0688(13) Uani 1 1 d . . .
H23 H 0.2892 0.3617 0.5777 0.083 Uiso 1 1 calc R . .
C27 C 0.23067(18) 0.4426(4) 0.4417(2) 0.0695(13) Uani 1 1 d . . .
H27 H 0.2019 0.4786 0.4112 0.083 Uiso 1 1 calc R . .
C26 C 0.2635(2) 0.4063(5) 0.4323(3) 0.0901(18) Uani 1 1 d . . .
H26 H 0.2568 0.4159 0.3957 0.108 Uiso 1 1 calc R . .
C30 C 0.00576(17) 0.2871(5) 0.4091(2) 0.0850(16) Uani 1 1 d . . .
H30 H -0.0027 0.3599 0.3895 0.102 Uiso 1 1 calc R . .
C33 C 0.03055(18) 0.0699(4) 0.4662(2) 0.0725(13) Uani 1 1 d . . .
H33 H 0.0393 -0.0041 0.4848 0.087 Uiso 1 1 calc R . .
C24 C 0.3165(2) 0.3388(5) 0.5327(3) 0.0860(17) Uani 1 1 d . . .
H24 H 0.3456 0.3042 0.5632 0.103 Uiso 1 1 calc R . .
C5 C 0.01000(17) 0.6560(4) 0.3708(2) 0.0680(12) Uani 1 1 d . . .
C32 C -0.0156(2) 0.0899(5) 0.4176(3) 0.0967(19) Uani 1 1 d . . .
H32 H -0.0387 0.0303 0.4038 0.116 Uiso 1 1 calc R . .
C7 C 0.0819(2) 0.7223(5) 0.3444(3) 0.0897(16) Uani 1 1 d . . .
H7A H 0.0783 0.7093 0.3084 0.108 Uiso 1 1 calc R . .
H7B H 0.0582 0.7812 0.3364 0.108 Uiso 1 1 calc R . .
C2 C -0.0092(3) 0.7655(5) 0.4399(4) 0.097(2) Uani 1 1 d . . .
H2A H -0.0154 0.8005 0.4643 0.116 Uiso 1 1 calc R . .
C6 C 0.02215(18) 0.5922(5) 0.3357(2) 0.0785(14) Uani 1 1 d . . .
H6A H 0.0151 0.5077 0.3338 0.094 Uiso 1 1 calc R . .
H6B H 0.0027 0.6234 0.2957 0.094 Uiso 1 1 calc R . .
C3 C -0.0458(2) 0.7502(6) 0.3810(4) 0.110(2) Uani 1 1 d . . .
H3 H -0.0768 0.7776 0.3645 0.132 Uiso 1 1 calc R . .
C25 C 0.3060(2) 0.3562(5) 0.4783(4) 0.095(2) Uani 1 1 d . . .
H25 H 0.3286 0.3332 0.4727 0.114 Uiso 1 1 calc R . .
O6 O 0.0768(2) 0.4180(7) 0.2150(2) 0.198(3) Uani 1 1 d . . .
C31 C -0.02829(19) 0.1982(6) 0.3886(3) 0.110(2) Uani 1 1 d . . .
H31 H -0.0598 0.2112 0.3552 0.131 Uiso 1 1 calc R . .
C4 C -0.0360(2) 0.6943(5) 0.3468(3) 0.0957(18) Uani 1 1 d . . .
H4 H -0.0608 0.6818 0.3070 0.115 Uiso 1 1 calc R . .
O7 O 0.0873(4) 0.4133(8) 0.2987(4) 0.250(4) Uani 1 1 d . . .
O8 O 0.1279(3) 0.5383(7) 0.2895(4) 0.253(5) Uani 1 1 d . . .
H2 H 0.0870(17) 0.550(5) 0.360(2) 0.071(16) Uiso 1 1 d . . .
H5 H 0.2119(14) 0.283(4) 0.6392(17) 0.041(12) Uiso 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
C20 N6 1.527(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 C17 1.484(7) . ?
C18 N6 1.485(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C15 N4 1.338(8) . ?
C15 C14 1.368(9) . ?
C15 C16 1.522(9) . ?
C17 N5 1.472(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16 N5 1.471(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C11 N4 1.342(7) . ?
C11 C12 1.392(10) . ?
C11 H11 0.9300 . ?
C14 C13 1.324(15) . ?
C14 H14 0.9300 . ?
C12 C13 1.331(16) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
O10 Cl2 1.309(7) . ?
O9 Cl1 1.333(6) . ?
Cl2 O11 1.229(9) . ?
Cl2 O12 1.369(6) . ?
Cl2 O13 1.425(6) . ?
C19 N6 1.472(7) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C9 N3 1.476(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N3 1.458(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8 C7 1.445(8) . ?
C8 N3 1.502(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
Fe1 O1 1.787(3) . ?
Fe1 O5 1.999(3) . ?
Fe1 O2 2.040(3) . ?
Fe1 N1 2.156(4) . ?
Fe1 N3 2.208(4) . ?
Fe1 N2 2.218(4) . ?
Fe2 O1 1.795(3) . ?
Fe2 O3 2.032(3) . ?
Fe2 O4 2.058(3) . ?
Fe2 N4 2.159(4) . ?
Fe2 N6 2.193(4) . ?
Fe2 N5 2.197(4) . ?
Cl1 O7 1.320(7) . ?
Cl1 O6 1.355(5) . ?
Cl1 O8 1.363(7) . ?
O3 C28 1.245(4) . ?
O4 C21 1.247(5) . ?
O2 C28 1.256(5) . ?
O5 C21 1.259(5) . ?
N1 C5 1.338(6) . ?
N1 C1 1.349(5) . ?
C22 C27 1.359(6) . ?
C22 C23 1.390(7) . ?
C22 C21 1.524(5) . ?
N2 C6 1.459(6) . ?
N2 C7 1.479(6) . ?
N2 H2 0.85(5) . ?
C29 C34 1.372(6) . ?
C29 C30 1.389(6) . ?
C29 C28 1.491(5) . ?
C1 C2 1.396(7) . ?
C1 H1 0.9300 . ?
N5 H5 0.81(4) . ?
C34 C33 1.372(6) . ?
C34 H34 0.9300 . ?
C23 C24 1.391(7) . ?
C23 H23 0.9300 . ?
C27 C26 1.388(6) . ?
C27 H27 0.9300 . ?
C26 C25 1.367(9) . ?
C26 H26 0.9300 . ?
C30 C31 1.377(7) . ?
C30 H30 0.9300 . ?
C33 C32 1.360(7) . ?
C33 H33 0.9300 . ?
C24 C25 1.376(9) . ?
C24 H24 0.9300 . ?
C5 C4 1.377(7) . ?
C5 C6 1.489(7) . ?
C32 C31 1.379(8) . ?
C32 H32 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C2 C3 1.372(9) . ?
C2 H2A 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 C4 1.364(9) . ?
C3 H3 0.9300 . ?
C25 H25 0.9300 . ?
C31 H31 0.9300 . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 N6 110.2(4) . . ?
C17 C18 H18A 109.6 . . ?
N6 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
N6 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N4 C15 C14 120.5(8) . . ?
N4 C15 C16 117.3(5) . . ?
C14 C15 C16 122.2(8) . . ?
N5 C17 C18 109.7(4) . . ?
N5 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
N5 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N5 C16 C15 109.1(5) . . ?
N5 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
N5 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
N4 C11 C12 118.7(8) . . ?
N4 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C14 C15 119.8(10) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C13 C12 C11 120.1(10) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 120.7(9) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
O11 Cl2 O10 118.2(10) . . ?
O11 Cl2 O12 112.0(7) . . ?
O10 Cl2 O12 110.5(5) . . ?
O11 Cl2 O13 102.6(8) . . ?
O10 Cl2 O13 104.7(6) . . ?
O12 Cl2 O13 107.7(5) . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C8 N3 113.2(5) . . ?
C7 C8 H8A 108.9 . . ?
N3 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
N3 C8 H8B 108.9 . . ?
H8A C8 H8B 107.8 . . ?
O1 Fe1 O5 100.69(13) . . ?
O1 Fe1 O2 98.04(12) . . ?
O5 Fe1 O2 90.27(13) . . ?
O1 Fe1 N1 98.54(13) . . ?
O5 Fe1 N1 160.37(14) . . ?
O2 Fe1 N1 83.14(13) . . ?
O1 Fe1 N3 97.55(14) . . ?
O5 Fe1 N3 88.12(14) . . ?
O2 Fe1 N3 164.35(14) . . ?
N1 Fe1 N3 93.26(14) . . ?
O1 Fe1 N2 172.00(15) . . ?
O5 Fe1 N2 86.64(15) . . ?
O2 Fe1 N2 85.02(13) . . ?
N1 Fe1 N2 74.41(15) . . ?
N3 Fe1 N2 79.35(15) . . ?
O1 Fe2 O3 99.70(12) . . ?
O1 Fe2 O4 98.20(12) . . ?
O3 Fe2 O4 89.05(12) . . ?
O1 Fe2 N4 98.96(18) . . ?
O3 Fe2 N4 160.19(18) . . ?
O4 Fe2 N4 81.72(14) . . ?
O1 Fe2 N6 96.86(14) . . ?
O3 Fe2 N6 89.53(14) . . ?
O4 Fe2 N6 164.90(14) . . ?
N4 Fe2 N6 94.83(16) . . ?
O1 Fe2 N5 172.41(15) . . ?
O3 Fe2 N5 87.00(14) . . ?
O4 Fe2 N5 85.39(14) . . ?
N4 Fe2 N5 74.86(19) . . ?
N6 Fe2 N5 79.52(16) . . ?
O7 Cl1 O9 109.1(6) . . ?
O7 Cl1 O6 109.7(6) . . ?
O9 Cl1 O6 107.4(5) . . ?
O7 Cl1 O8 104.1(6) . . ?
O9 Cl1 O8 117.4(6) . . ?
O6 Cl1 O8 109.0(5) . . ?
C28 O3 Fe2 128.3(3) . . ?
Fe1 O1 Fe2 119.27(14) . . ?
C21 O4 Fe2 129.3(3) . . ?
C28 O2 Fe1 130.5(3) . . ?
C21 O5 Fe1 127.8(3) . . ?
C5 N1 C1 120.5(4) . . ?
C5 N1 Fe1 116.4(3) . . ?
C1 N1 Fe1 122.8(3) . . ?
C27 C22 C23 120.8(4) . . ?
C27 C22 C21 119.8(4) . . ?
C23 C22 C21 119.5(4) . . ?
C6 N2 C7 111.5(5) . . ?
C6 N2 Fe1 109.7(3) . . ?
C7 N2 Fe1 110.5(3) . . ?
C6 N2 H2 115(3) . . ?
C7 N2 H2 112(3) . . ?
Fe1 N2 H2 97(3) . . ?
C34 C29 C30 118.9(4) . . ?
C34 C29 C28 121.2(4) . . ?
C30 C29 C28 119.9(4) . . ?
O3 C28 O2 125.2(4) . . ?
O3 C28 C29 117.8(4) . . ?
O2 C28 C29 117.1(4) . . ?
C10 N3 C9 109.8(5) . . ?
C10 N3 C8 106.3(5) . . ?
C9 N3 C8 111.3(5) . . ?
C10 N3 Fe1 111.3(3) . . ?
C9 N3 Fe1 112.7(3) . . ?
C8 N3 Fe1 105.2(3) . . ?
C19 N6 C18 112.4(5) . . ?
C19 N6 C20 108.9(5) . . ?
C18 N6 C20 105.1(4) . . ?
C19 N6 Fe2 113.2(3) . . ?
C18 N6 Fe2 106.4(3) . . ?
C20 N6 Fe2 110.4(3) . . ?
C15 N4 C11 120.2(6) . . ?
C15 N4 Fe2 114.9(4) . . ?
C11 N4 Fe2 123.5(5) . . ?
N1 C1 C2 120.1(6) . . ?
N1 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C16 N5 C17 112.4(4) . . ?
C16 N5 Fe2 109.8(4) . . ?
C17 N5 Fe2 109.9(4) . . ?
C16 N5 H5 102(3) . . ?
C17 N5 H5 108(3) . . ?
Fe2 N5 H5 115(3) . . ?
O4 C21 O5 126.5(4) . . ?
O4 C21 C22 117.6(4) . . ?
O5 C21 C22 115.9(4) . . ?
C29 C34 C33 121.3(4) . . ?
C29 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C22 C23 C24 118.8(5) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C22 C27 C26 120.7(5) . . ?
C22 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C25 C26 C27 118.4(6) . . ?
C25 C26 H26 120.8 . . ?
C27 C26 H26 120.8 . . ?
C31 C30 C29 119.8(5) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C32 C33 C34 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C25 C24 C23 119.2(6) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N1 C5 C4 120.3(5) . . ?
N1 C5 C6 117.2(4) . . ?
C4 C5 C6 122.6(5) . . ?
C33 C32 C31 120.4(5) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C8 C7 N2 110.3(5) . . ?
C8 C7 H7A 109.6 . . ?
N2 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
N2 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C3 C2 C1 119.4(6) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
N2 C6 C5 109.3(4) . . ?
N2 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C26 C25 C24 122.0(5) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C30 C31 C32 120.0(5) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C3 C4 C5 120.6(6) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.51
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_18mpmbf
_database_code_depnum_ccdc_archive 'CCDC 1469279'
_audit_update_record             
;
2016-05-01 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H55 Cl2 Fe2 N7 O13'
_chemical_formula_weight         928.43

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'

_symmetry_cell_setting           ORTHORHOMBIC
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   10.9602(7)
_cell_length_b                   18.5001(12)
_cell_length_c                   20.8260(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4222.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3224
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      25.34

_exptl_crystal_description       BLOCKS
_exptl_crystal_colour            BROWN
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7141
_exptl_absorpt_correction_T_max  0.8298
_exptl_absorpt_process_details   'BRUKER SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFARCTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25416
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         28.31
_reflns_number_total             9827
_reflns_number_gt                9032
_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    ORTEP
_computing_publication_material  ?

_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)+(0.0631P)²+1.4672P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(13)
_refine_ls_number_reflns         9827
_refine_ls_number_parameters     524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1096
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.82544(4) 0.65547(2) 0.79104(2) 0.01664(10) Uani 1 1 d . . .
Fe2 Fe 0.95254(4) 0.70698(2) 0.668555(19) 0.01595(10) Uani 1 1 d . . .
Cl1 Cl 0.43801(7) 0.73490(4) 0.62405(4) 0.02475(17) Uani 1 1 d . . .
Cl2 Cl 0.47780(9) 0.90284(5) 0.96300(4) 0.0365(2) Uani 1 1 d . . .
O1 O 1.0683(2) 0.63039(12) 0.70133(10) 0.0211(5) Uani 1 1 d . . .
O2 O 0.9640(2) 0.58019(12) 0.78187(11) 0.0236(5) Uani 1 1 d . . .
O3 O 0.9550(2) 0.72419(12) 0.82550(10) 0.0242(5) Uani 1 1 d . . .
O4 O 1.0328(2) 0.77336(12) 0.73637(10) 0.0218(5) Uani 1 1 d . . .
O5 O 0.81320(19) 0.68511(11) 0.70919(9) 0.0182(4) Uani 1 1 d . . .
O6 O 0.4701(3) 0.80831(16) 0.60805(16) 0.0517(8) Uani 1 1 d . . .
O7 O 0.3813(3) 0.70368(18) 0.56811(14) 0.0469(7) Uani 1 1 d . . .
O8 O 0.5456(3) 0.69601(16) 0.63914(16) 0.0480(8) Uani 1 1 d . . .
O9 O 0.3522(3) 0.7313(2) 0.67564(14) 0.0629(11) Uani 1 1 d . . .
O10 O 0.5685(4) 0.9177(3) 0.91704(17) 0.0854(15) Uani 1 1 d . . .
O11 O 0.3724(4) 0.9468(2) 0.95527(19) 0.0804(14) Uani 1 1 d . . .
O12 O 0.5257(3) 0.9159(2) 1.02502(15) 0.0618(10) Uani 1 1 d . . .
O13 O 0.4447(4) 0.8284(2) 0.9609(3) 0.1013(18) Uani 1 1 d . . .
N1 N 0.7020(2) 0.56600(14) 0.78290(12) 0.0201(5) Uani 1 1 d . . .
N2 N 0.8095(3) 0.61289(16) 0.88892(13) 0.0240(6) Uani 1 1 d . . .
H2C H 0.870(4) 0.624(2) 0.906(2) 0.038(13) Uiso 1 1 d . . .
N3 N 0.6870(3) 0.73053(15) 0.83062(13) 0.0237(6) Uani 1 1 d . . .
N4 N 0.8897(2) 0.80352(14) 0.62057(12) 0.0185(5) Uani 1 1 d . . .
N5 N 1.1030(3) 0.73825(15) 0.60586(12) 0.0211(6) Uani 1 1 d . . .
H5C H 1.181(3) 0.7205(17) 0.6204(15) 0.012(8) Uiso 1 1 d . . .
N6 N 0.9197(2) 0.63178(15) 0.58696(12) 0.0201(6) Uani 1 1 d . . .
N7 N 0.4737(5) 0.5266(3) 0.9557(2) 0.0704(13) Uani 1 1 d . . .
C1 C 0.6317(3) 0.55320(18) 0.73076(16) 0.0233(7) Uani 1 1 d . . .
H1 H 0.6301 0.5871 0.6978 0.028 Uiso 1 1 calc R . .
C2 C 0.5619(3) 0.49101(19) 0.72512(18) 0.0303(8) Uani 1 1 d . . .
H2 H 0.5154 0.4826 0.6885 0.036 Uiso 1 1 calc R . .
C3 C 0.5630(3) 0.44168(19) 0.77503(18) 0.0314(8) Uani 1 1 d . . .
H3 H 0.5169 0.3996 0.7724 0.038 Uiso 1 1 calc R . .
C4 C 0.6323(3) 0.45534(18) 0.82813(19) 0.0283(7) Uani 1 1 d . . .
H4 H 0.6321 0.4231 0.8624 0.034 Uiso 1 1 calc R . .
C5 C 0.7030(3) 0.51751(17) 0.83093(17) 0.0236(7) Uani 1 1 d . . .
C6 C 0.7878(3) 0.53451(19) 0.88608(16) 0.0252(7) Uani 1 1 d . . .
H6A H 0.7518 0.5182 0.9261 0.030 Uiso 1 1 calc R . .
H6B H 0.8646 0.5094 0.8802 0.030 Uiso 1 1 calc R . .
C7 C 0.7133(3) 0.6516(2) 0.92461(15) 0.0279(7) Uani 1 1 d . . .
H7A H 0.7316 0.6507 0.9702 0.033 Uiso 1 1 calc R . .
H7B H 0.6355 0.6279 0.9180 0.033 Uiso 1 1 calc R . .
C8 C 0.7060(3) 0.72874(19) 0.90175(15) 0.0274(7) Uani 1 1 d . . .
H8A H 0.6388 0.7531 0.9230 0.033 Uiso 1 1 calc R . .
H8B H 0.7808 0.7539 0.9126 0.033 Uiso 1 1 calc R . .
C9 C 0.7084(4) 0.80486(19) 0.80664(18) 0.0334(8) Uani 1 1 d . . .
H9A H 0.6492 0.8370 0.8250 0.050 Uiso 1 1 calc R . .
H9B H 0.7011 0.8055 0.7607 0.050 Uiso 1 1 calc R . .
H9C H 0.7889 0.8203 0.8186 0.050 Uiso 1 1 calc R . .
C10 C 0.5593(3) 0.7110(2) 0.81434(17) 0.0317(8) Uani 1 1 d . . .
H10A H 0.5048 0.7464 0.8319 0.048 Uiso 1 1 calc R . .
H10B H 0.5405 0.6644 0.8321 0.048 Uiso 1 1 calc R . .
H10C H 0.5501 0.7094 0.7685 0.048 Uiso 1 1 calc R . .
C11 C 0.7718(3) 0.82422(18) 0.61761(15) 0.0219(7) Uani 1 1 d . . .
H11 H 0.7127 0.7961 0.6376 0.026 Uiso 1 1 calc R . .
C12 C 0.7369(3) 0.88631(17) 0.58560(16) 0.0237(7) Uani 1 1 d . . .
H12 H 0.6558 0.9010 0.5854 0.028 Uiso 1 1 calc R . .
C13 C 0.8249(4) 0.92590(18) 0.55403(15) 0.0282(8) Uani 1 1 d . . .
H13 H 0.8029 0.9669 0.5309 0.034 Uiso 1 1 calc R . .
C14 C 0.9458(4) 0.90479(18) 0.55665(15) 0.0257(7) Uani 1 1 d . . .
H14 H 1.0059 0.9312 0.5355 0.031 Uiso 1 1 calc R . .
C15 C 0.9754(3) 0.84360(18) 0.59142(14) 0.0215(6) Uani 1 1 d . . .
C16 C 1.1043(3) 0.81754(18) 0.60036(15) 0.0220(7) Uani 1 1 d . . .
H16A H 1.1539 0.8320 0.5640 0.026 Uiso 1 1 calc R . .
H16B H 1.1389 0.8387 0.6389 0.026 Uiso 1 1 calc R . .
C17 C 1.0891(3) 0.70329(19) 0.54196(15) 0.0240(7) Uani 1 1 d . . .
H17A H 1.1680 0.6999 0.5211 0.029 Uiso 1 1 calc R . .
H17B H 1.0359 0.7323 0.5151 0.029 Uiso 1 1 calc R . .
C18 C 1.0358(3) 0.62893(18) 0.55027(15) 0.0231(7) Uani 1 1 d . . .
H18A H 1.0209 0.6077 0.5084 0.028 Uiso 1 1 calc R . .
H18B H 1.0937 0.5985 0.5728 0.028 Uiso 1 1 calc R . .
C19 C 0.8186(3) 0.6581(2) 0.54510(16) 0.0268(7) Uani 1 1 d . . .
H19A H 0.8409 0.7037 0.5265 0.040 Uiso 1 1 calc R . .
H19B H 0.7459 0.6639 0.5703 0.040 Uiso 1 1 calc R . .
H19C H 0.8039 0.6236 0.5115 0.040 Uiso 1 1 calc R . .
C20 C 0.8861(3) 0.55783(19) 0.60750(16) 0.0276(7) Uani 1 1 d . . .
H20A H 0.8768 0.5275 0.5704 0.041 Uiso 1 1 calc R . .
H20B H 0.8106 0.5594 0.6309 0.041 Uiso 1 1 calc R . .
H20C H 0.9491 0.5386 0.6346 0.041 Uiso 1 1 calc R . .
C21 C 1.0540(3) 0.58258(17) 0.74407(14) 0.0194(6) Uani 1 1 d . . .
C22 C 1.1547(3) 0.52637(19) 0.75175(17) 0.0258(7) Uani 1 1 d . . .
C23 C 1.0977(4) 0.45280(19) 0.77054(17) 0.0311(8) Uani 1 1 d . . .
H23A H 1.1609 0.4172 0.7745 0.047 Uiso 1 1 calc R . .
H23B H 1.0409 0.4380 0.7380 0.047 Uiso 1 1 calc R . .
H23C H 1.0558 0.4576 0.8108 0.047 Uiso 1 1 calc R . .
C24 C 1.2390(4) 0.5532(2) 0.8052(2) 0.0426(10) Uani 1 1 d . . .
H24A H 1.2753 0.5982 0.7927 0.064 Uiso 1 1 calc R . .
H24B H 1.3019 0.5181 0.8127 0.064 Uiso 1 1 calc R . .
H24C H 1.1926 0.5600 0.8439 0.064 Uiso 1 1 calc R . .
C25 C 1.2254(4) 0.5169(2) 0.6894(2) 0.0374(9) Uani 1 1 d . . .
H25A H 1.2660 0.5613 0.6788 0.056 Uiso 1 1 calc R . .
H25B H 1.1700 0.5042 0.6555 0.056 Uiso 1 1 calc R . .
H25C H 1.2848 0.4792 0.6946 0.056 Uiso 1 1 calc R . .
C26 C 1.0289(3) 0.76459(16) 0.79650(15) 0.0192(6) Uani 1 1 d . . .
C27 C 1.1229(3) 0.80437(18) 0.83834(15) 0.0241(7) Uani 1 1 d . . .
C28 C 1.2046(4) 0.8543(2) 0.79889(18) 0.0385(9) Uani 1 1 d . . .
H28A H 1.2415 0.8273 0.7646 0.058 Uiso 1 1 calc R . .
H28B H 1.2671 0.8741 0.8260 0.058 Uiso 1 1 calc R . .
H28C H 1.1564 0.8928 0.7812 0.058 Uiso 1 1 calc R . .
C29 C 1.0566(4) 0.8468(2) 0.89052(17) 0.0350(8) Uani 1 1 d . . .
H29A H 1.1143 0.8756 0.9139 0.053 Uiso 1 1 calc R . .
H29B H 1.0171 0.8137 0.9194 0.053 Uiso 1 1 calc R . .
H29C H 0.9966 0.8777 0.8711 0.053 Uiso 1 1 calc R . .
C30 C 1.2006(4) 0.7460(2) 0.8707(2) 0.0410(10) Uani 1 1 d . . .
H30A H 1.2433 0.7187 0.8385 0.062 Uiso 1 1 calc R . .
H30B H 1.1488 0.7142 0.8949 0.062 Uiso 1 1 calc R . .
H30C H 1.2585 0.7684 0.8990 0.062 Uiso 1 1 calc R . .
C31 C 0.3210(5) 0.6228(3) 0.9887(3) 0.0653(15) Uani 1 1 d . . .
H31A H 0.2521 0.6219 0.9602 0.098 Uiso 1 1 calc R . .
H31B H 0.3569 0.6702 0.9883 0.098 Uiso 1 1 calc R . .
H31C H 0.2948 0.6113 1.0314 0.098 Uiso 1 1 calc R . .
C32 C 0.4086(4) 0.5712(2) 0.9680(2) 0.0415(10) 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 O5 1.796(2) . ?
Fe1 O3 2.037(2) . ?
Fe1 O2 2.069(2) . ?
Fe1 N1 2.145(3) . ?
Fe1 N2 2.192(3) . ?
Fe1 N3 2.216(3) . ?
Fe2 O5 1.792(2) . ?
Fe2 O1 2.021(2) . ?
Fe2 O4 2.068(2) . ?
Fe2 N4 2.159(3) . ?
Fe2 N5 2.181(3) . ?
Fe2 N6 2.225(3) . ?
Cl1 O8 1.416(3) . ?
Cl1 O9 1.430(3) . ?
Cl1 O7 1.441(3) . ?
Cl1 O6 1.442(3) . ?
Cl2 O10 1.407(4) . ?
Cl2 O12 1.415(3) . ?
Cl2 O11 1.422(4) . ?
Cl2 O13 1.425(4) . ?
O1 C21 1.265(4) . ?
O2 C21 1.263(4) . ?
O3 C26 1.257(4) . ?
O4 C26 1.263(4) . ?
N1 C5 1.344(4) . ?
N1 C1 1.352(4) . ?
N2 C6 1.471(5) . ?
N2 C7 1.475(5) . ?
N2 H2C 0.78(5) . ?
N3 C9 1.482(4) . ?
N3 C10 1.485(5) . ?
N3 C8 1.496(4) . ?
N4 C15 1.342(4) . ?
N4 C11 1.348(4) . ?
N5 C16 1.472(4) . ?
N5 C17 1.487(4) . ?
N5 H5C 0.97(4) . ?
N6 C20 1.480(4) . ?
N6 C18 1.485(4) . ?
N6 C19 1.492(4) . ?
N7 C32 1.121(6) . ?
C1 C2 1.386(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.383(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.365(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.510(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.506(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.382(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.504(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.505(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.525(4) . ?
C22 C25 1.522(5) . ?
C22 C24 1.530(5) . ?
C22 C23 1.548(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.537(4) . ?
C27 C29 1.525(5) . ?
C27 C28 1.525(5) . ?
C27 C30 1.532(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.421(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Fe1 O3 101.31(9) . . ?
O5 Fe1 O2 99.95(9) . . ?
O3 Fe1 O2 86.61(10) . . ?
O5 Fe1 N1 96.52(10) . . ?
O3 Fe1 N1 161.72(9) . . ?
O2 Fe1 N1 86.34(10) . . ?
O5 Fe1 N2 170.54(11) . . ?
O3 Fe1 N2 87.26(10) . . ?
O2 Fe1 N2 84.41(10) . . ?
N1 Fe1 N2 75.28(11) . . ?
O5 Fe1 N3 96.35(10) . . ?
O3 Fe1 N3 87.45(10) . . ?
O2 Fe1 N3 163.46(10) . . ?
N1 Fe1 N3 94.65(10) . . ?
N2 Fe1 N3 79.90(11) . . ?
O5 Fe2 O1 102.55(9) . . ?
O5 Fe2 O4 100.03(9) . . ?
O1 Fe2 O4 85.32(9) . . ?
O5 Fe2 N4 97.66(10) . . ?
O1 Fe2 N4 159.49(10) . . ?
O4 Fe2 N4 87.75(9) . . ?
O5 Fe2 N5 170.61(10) . . ?
O1 Fe2 N5 85.04(10) . . ?
O4 Fe2 N5 85.97(9) . . ?
N4 Fe2 N5 75.22(10) . . ?
O5 Fe2 N6 94.68(10) . . ?
O1 Fe2 N6 85.48(9) . . ?
O4 Fe2 N6 164.04(10) . . ?
N4 Fe2 N6 96.44(10) . . ?
N5 Fe2 N6 80.27(10) . . ?
O8 Cl1 O9 110.93(19) . . ?
O8 Cl1 O7 109.6(2) . . ?
O9 Cl1 O7 107.77(19) . . ?
O8 Cl1 O6 109.07(19) . . ?
O9 Cl1 O6 112.2(2) . . ?
O7 Cl1 O6 107.2(2) . . ?
O10 Cl2 O12 109.0(2) . . ?
O10 Cl2 O11 112.6(2) . . ?
O12 Cl2 O11 107.9(3) . . ?
O10 Cl2 O13 110.3(3) . . ?
O12 Cl2 O13 106.7(3) . . ?
O11 Cl2 O13 110.1(3) . . ?
C21 O1 Fe2 130.6(2) . . ?
C21 O2 Fe1 127.4(2) . . ?
C26 O3 Fe1 130.6(2) . . ?
C26 O4 Fe2 125.9(2) . . ?
Fe2 O5 Fe1 116.96(11) . . ?
C5 N1 C1 119.1(3) . . ?
C5 N1 Fe1 116.8(2) . . ?
C1 N1 Fe1 123.9(2) . . ?
C6 N2 C7 112.6(3) . . ?
C6 N2 Fe1 109.3(2) . . ?
C7 N2 Fe1 110.6(2) . . ?
C6 N2 H2C 114(3) . . ?
C7 N2 H2C 104(3) . . ?
Fe1 N2 H2C 105(3) . . ?
C9 N3 C10 107.4(3) . . ?
C9 N3 C8 109.4(3) . . ?
C10 N3 C8 110.6(3) . . ?
C9 N3 Fe1 110.3(2) . . ?
C10 N3 Fe1 114.1(2) . . ?
C8 N3 Fe1 105.0(2) . . ?
C15 N4 C11 119.5(3) . . ?
C15 N4 Fe2 116.3(2) . . ?
C11 N4 Fe2 124.2(2) . . ?
C16 N5 C17 111.4(3) . . ?
C16 N5 Fe2 108.5(2) . . ?
C17 N5 Fe2 110.1(2) . . ?
C16 N5 H5C 110.8(19) . . ?
C17 N5 H5C 102.9(19) . . ?
Fe2 N5 H5C 113.2(19) . . ?
C20 N6 C18 109.2(3) . . ?
C20 N6 C19 106.6(3) . . ?
C18 N6 C19 110.3(2) . . ?
C20 N6 Fe2 113.42(19) . . ?
C18 N6 Fe2 106.06(19) . . ?
C19 N6 Fe2 111.3(2) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.1(3) . . ?
N1 C5 C6 115.6(3) . . ?
C4 C5 C6 123.2(3) . . ?
N2 C6 C5 109.6(3) . . ?
N2 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 C8 109.8(3) . . ?
N2 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N2 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N3 C8 C7 110.0(3) . . ?
N3 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N3 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 121.5(3) . . ?
N4 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C14 120.1(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
N4 C15 C14 121.7(3) . . ?
N4 C15 C16 115.1(3) . . ?
C14 C15 C16 123.2(3) . . ?
N5 C16 C15 108.7(3) . . ?
N5 C16 H16A 110.0 . . ?
C15 C16 H16A 110.0 . . ?
N5 C16 H16B 110.0 . . ?
C15 C16 H16B 110.0 . . ?
H16A C16 H16B 108.3 . . ?
N5 C17 C18 109.5(3) . . ?
N5 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
N5 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
N6 C18 C17 111.1(3) . . ?
N6 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
N6 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 O1 124.0(3) . . ?
O2 C21 C22 118.4(3) . . ?
O1 C21 C22 117.5(3) . . ?
C25 C22 C21 110.9(3) . . ?
C25 C22 C24 110.6(3) . . ?
C21 C22 C24 107.0(3) . . ?
C25 C22 C23 108.7(3) . . ?
C21 C22 C23 109.5(3) . . ?
C24 C22 C23 110.2(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O3 C26 O4 125.1(3) . . ?
O3 C26 C27 116.4(3) . . ?
O4 C26 C27 118.5(3) . . ?
C29 C27 C28 110.6(3) . . ?
C29 C27 C30 108.3(3) . . ?
C28 C27 C30 109.7(3) . . ?
C29 C27 C26 109.3(3) . . ?
C28 C27 C26 112.2(3) . . ?
C30 C27 C26 106.5(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N7 C32 C31 174.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.092
