# 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_g1862a
_database_code_depnum_ccdc_archive 'CCDC 1024399'
_audit_update_record             
;
2014-09-15 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H42 N8 Cl2 Fe2 O , 2(Cl) , 2(H 2 O)'
_chemical_formula_sum            'C32 H46 Cl4 Fe2 N8 O3'
_chemical_formula_weight         844.27

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                   15.9941(10)
_cell_length_b                   15.4161(10)
_cell_length_c                   15.6472(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.858(3)
_cell_angle_gamma                90.00
_cell_volume                     3628.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9939
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      27.00

_exptl_crystal_description       column
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7795
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_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_measurement_device       'Bruker KAPPA APEX II'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            30537
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3960
_reflns_number_gt                3567
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_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)+(0.0391P)²+4.9213P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3960
_refine_ls_number_parameters     233
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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 0.118844(13) 0.135003(14) 0.788673(14) 0.01263(7) Uani 1 1 d . . .
Cl1 Cl 0.14949(2) 0.11684(3) 0.94285(2) 0.01928(9) Uani 1 1 d . . .
O3 O 0.0000 0.14365(9) 0.7500 0.0140(3) Uani 1 2 d S . .
N1 N 0.10777(9) 0.00124(9) 0.73111(9) 0.0173(3) Uani 1 1 d . . .
N2 N 0.12715(8) 0.16918(8) 0.65515(9) 0.0149(3) Uani 1 1 d . . .
N3 N 0.13088(8) 0.27549(9) 0.78934(8) 0.0156(3) Uani 1 1 d . . .
N4 N 0.26422(9) 0.12967(8) 0.81247(9) 0.0166(3) Uani 1 1 d . . .
C1 C 0.01586(10) -0.03487(10) 0.70890(11) 0.0187(3) Uani 1 1 d . . .
H1A H 0.0148 -0.0950 0.6865 0.022 Uiso 1 1 calc R . .
H1B H -0.0258 0.0000 0.6595 0.022 Uiso 1 1 calc R . .
C2 C 0.12838(11) 0.01087(11) 0.64556(11) 0.0198(3) Uani 1 1 d . . .
H2A H 0.1043 -0.0396 0.6056 0.024 Uiso 1 1 calc R . .
H2B H 0.1937 0.0116 0.6602 0.024 Uiso 1 1 calc R . .
C3 C 0.08902(10) 0.09350(10) 0.59580(10) 0.0178(3) Uani 1 1 d . . .
H3A H 0.1028 0.0979 0.5388 0.021 Uiso 1 1 calc R . .
H3B H 0.0236 0.0928 0.5799 0.021 Uiso 1 1 calc R . .
C4 C 0.17166(11) -0.06043(11) 0.79225(12) 0.0231(3) Uani 1 1 d . . .
H4A H 0.1668 -0.1168 0.7621 0.035 Uiso 1 1 calc R . .
H4B H 0.1582 -0.0671 0.8485 0.035 Uiso 1 1 calc R . .
H4C H 0.2322 -0.0381 0.8066 0.035 Uiso 1 1 calc R . .
C5 C 0.07102(10) 0.24806(10) 0.62742(10) 0.0156(3) Uani 1 1 d . . .
H5A H 0.0075 0.2327 0.6119 0.019 Uiso 1 1 calc R . .
H5B H 0.0795 0.2746 0.5733 0.019 Uiso 1 1 calc R . .
C6 C 0.09830(10) 0.31106(10) 0.70589(10) 0.0156(3) Uani 1 1 d . . .
C7 C 0.08929(11) 0.40022(11) 0.69358(11) 0.0200(3) Uani 1 1 d . . .
H7A H 0.0668 0.4243 0.6342 0.024 Uiso 1 1 calc R . .
C8 C 0.11370(11) 0.45341(11) 0.76942(12) 0.0228(3) Uani 1 1 d . . .
H8A H 0.1063 0.5145 0.7627 0.027 Uiso 1 1 calc R . .
C9 C 0.14905(11) 0.41701(11) 0.85534(12) 0.0217(3) Uani 1 1 d . . .
H9A H 0.1675 0.4526 0.9080 0.026 Uiso 1 1 calc R . .
C10 C 0.15674(10) 0.32759(11) 0.86253(11) 0.0191(3) Uani 1 1 d . . .
H10A H 0.1811 0.3023 0.9211 0.023 Uiso 1 1 calc R . .
C25 C 0.21937(10) 0.18933(11) 0.65886(10) 0.0174(3) Uani 1 1 d . . .
H25A H 0.2225 0.2514 0.6438 0.021 Uiso 1 1 calc R . .
H25B H 0.2329 0.1547 0.6119 0.021 Uiso 1 1 calc R . .
C26 C 0.28936(10) 0.17123(10) 0.74981(10) 0.0158(3) Uani 1 1 d . . .
C27 C 0.37767(11) 0.19432(11) 0.76554(12) 0.0211(3) Uani 1 1 d . . .
H27A H 0.3936 0.2258 0.7211 0.025 Uiso 1 1 calc R . .
C28 C 0.44157(11) 0.17079(12) 0.84662(12) 0.0251(4) Uani 1 1 d . . .
H28A H 0.5020 0.1866 0.8590 0.030 Uiso 1 1 calc R . .
C29 C 0.41677(11) 0.12384(11) 0.90983(12) 0.0227(3) Uani 1 1 d . . .
H29A H 0.4601 0.1048 0.9649 0.027 Uiso 1 1 calc R . .
C30 C 0.32768(10) 0.10538(11) 0.89096(11) 0.0198(3) Uani 1 1 d . . .
H30A H 0.3104 0.0745 0.9348 0.024 Uiso 1 1 calc R . .
O99 O 0.13861(9) 0.79999(9) 0.93039(9) 0.0297(3) Uani 1 1 d . . .
Cl3 Cl 0.16633(3) 0.60790(3) 0.99363(3) 0.02191(10) Uani 1 1 d . . .
H99A H 0.149(2) 0.740(2) 0.952(2) 0.074(9) Uiso 1 1 d . . .
H99B H 0.202(2) 0.827(2) 0.956(2) 0.093(11) 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
Fe1 O3 1.7932(3) . ?
Fe1 N3 2.1741(14) . ?
Fe1 N2 2.2019(13) . ?
Fe1 N4 2.2278(13) . ?
Fe1 N1 2.2330(13) . ?
Fe1 Cl1 2.3099(4) . ?
O3 Fe1 1.7932(3) 2_556 ?
N1 C4 1.483(2) . ?
N1 C2 1.491(2) . ?
N1 C1 1.498(2) . ?
N2 C5 1.4860(19) . ?
N2 C3 1.487(2) . ?
N2 C25 1.4891(19) . ?
N3 C10 1.344(2) . ?
N3 C6 1.347(2) . ?
N4 C26 1.342(2) . ?
N4 C30 1.353(2) . ?
C1 C1 1.535(3) 2_556 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.514(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.509(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.389(2) . ?
C7 C8 1.385(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.388(2) . ?
C8 H8A 0.9500 . ?
C9 C10 1.385(2) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C25 C26 1.508(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.395(2) . ?
C27 C28 1.380(2) . ?
C27 H27A 0.9500 . ?
C28 C29 1.388(3) . ?
C28 H28A 0.9500 . ?
C29 C30 1.383(2) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
O99 H99A 0.99(3) . ?
O99 H99B 1.04(4) . ?

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
O3 Fe1 N3 90.55(6) . . ?
O3 Fe1 N2 93.48(3) . . ?
N3 Fe1 N2 74.48(5) . . ?
O3 Fe1 N4 170.27(4) . . ?
N3 Fe1 N4 87.15(5) . . ?
N2 Fe1 N4 76.79(5) . . ?
O3 Fe1 N1 90.16(5) . . ?
N3 Fe1 N1 156.44(5) . . ?
N2 Fe1 N1 81.98(5) . . ?
N4 Fe1 N1 88.21(5) . . ?
O3 Fe1 Cl1 100.719(14) . . ?
N3 Fe1 Cl1 97.39(4) . . ?
N2 Fe1 Cl1 163.78(4) . . ?
N4 Fe1 Cl1 88.96(4) . . ?
N1 Fe1 Cl1 105.60(4) . . ?
Fe1 O3 Fe1 171.47(9) 2_556 . ?
C4 N1 C2 109.20(12) . . ?
C4 N1 C1 108.56(12) . . ?
C2 N1 C1 109.12(12) . . ?
C4 N1 Fe1 112.89(10) . . ?
C2 N1 Fe1 105.00(9) . . ?
C1 N1 Fe1 111.96(9) . . ?
C5 N2 C3 112.38(12) . . ?
C5 N2 C25 109.44(12) . . ?
C3 N2 C25 112.25(12) . . ?
C5 N2 Fe1 104.34(9) . . ?
C3 N2 Fe1 105.11(9) . . ?
C25 N2 Fe1 113.03(9) . . ?
C10 N3 C6 119.24(14) . . ?
C10 N3 Fe1 126.91(11) . . ?
C6 N3 Fe1 113.35(10) . . ?
C26 N4 C30 118.46(13) . . ?
C26 N4 Fe1 114.52(10) . . ?
C30 N4 Fe1 125.47(11) . . ?
N1 C1 C1 112.53(15) . 2_556 ?
N1 C1 H1A 109.1 . . ?
C1 C1 H1A 109.1 2_556 . ?
N1 C1 H1B 109.1 . . ?
C1 C1 H1B 109.1 2_556 . ?
H1A C1 H1B 107.8 . . ?
N1 C2 C3 111.43(13) . . ?
N1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C2 109.17(12) . . ?
N2 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 108.06(12) . . ?
N2 C5 H5A 110.1 . . ?
C6 C5 H5A 110.1 . . ?
N2 C5 H5B 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?
N3 C6 C7 121.68(14) . . ?
N3 C6 C5 115.87(13) . . ?
C7 C6 C5 122.45(14) . . ?
C8 C7 C6 118.77(15) . . ?
C8 C7 H7A 120.6 . . ?
C6 C7 H7A 120.6 . . ?
C7 C8 C9 119.62(16) . . ?
C7 C8 H8A 120.2 . . ?
C9 C8 H8A 120.2 . . ?
C10 C9 C8 118.48(15) . . ?
C10 C9 H9A 120.8 . . ?
C8 C9 H9A 120.8 . . ?
N3 C10 C9 122.17(15) . . ?
N3 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
N2 C25 C26 113.96(12) . . ?
N2 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N2 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N4 C26 C27 121.98(14) . . ?
N4 C26 C25 117.85(13) . . ?
C27 C26 C25 120.12(14) . . ?
C28 C27 C26 118.97(15) . . ?
C28 C27 H27A 120.5 . . ?
C26 C27 H27A 120.5 . . ?
C27 C28 C29 119.38(15) . . ?
C27 C28 H28A 120.3 . . ?
C29 C28 H28A 120.3 . . ?
C30 C29 C28 118.57(16) . . ?
C30 C29 H29A 120.7 . . ?
C28 C29 H29A 120.7 . . ?
N4 C30 C29 122.52(15) . . ?
N4 C30 H30A 118.7 . . ?
C29 C30 H30A 118.7 . . ?
H99A O99 H99B 102(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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_g2206
_database_code_depnum_ccdc_archive 'CCDC 1024400'
_audit_update_record             
;
2014-09-15 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C32.25 H42.75 N8 Fe2 O1.25 Cl1.75 , 2(Cl O4) , 0.5(C H4 O)'
_chemical_formula_sum            'C32.75 H44.75 Cl3.75 Fe2 N8 O9.75'
_chemical_formula_weight         951.15

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.1738(8)
_cell_length_b                   13.2744(13)
_cell_length_c                   19.1664(19)
_cell_angle_alpha                83.257(5)
_cell_angle_beta                 81.601(5)
_cell_angle_gamma                72.579(4)
_cell_volume                     1956.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9766
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      27.00

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             982
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7047
_exptl_absorpt_correction_T_max  0.8742
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       'Bruker KAPPA APEX II'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            92127
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.79
_diffrn_reflns_theta_max         27.00
_reflns_number_total             8497
_reflns_number_gt                7793
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_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. 

At the atom Fe2 a disorder of a Cl- ligand with an MeO- ligand in a ratio 
of 75%/25% was refined. The solvent MeOH molecule is disordered around 
a crystallographic centre of inversion.
;

_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)+(0.0284P)²+1.5183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8497
_refine_ls_number_parameters     530
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0627
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.49865(3) 0.058382(15) 0.231758(11) 0.01230(5) Uani 1 1 d . A .
Fe2 Fe 0.18959(3) 0.290302(16) 0.296844(11) 0.01469(6) Uani 1 1 d . . .
Cl1 Cl 0.73133(5) 0.12278(3) 0.19528(2) 0.02510(9) Uani 1 1 d . . .
Cl2 Cl -0.02189(14) 0.21151(5) 0.34984(3) 0.02252(13) Uani 0.75 1 d P A 1
O98 O 0.0652(9) 0.2171(4) 0.3491(3) 0.0257(13) Uani 0.25 1 d P A 2
C98 C -0.1066(14) 0.2114(7) 0.3653(5) 0.0299(19) Uani 0.25 1 d P A 2
H98A H -0.1862 0.2774 0.3476 0.045 Uiso 0.25 1 calc PR A 2
H98B H -0.1334 0.2009 0.4167 0.045 Uiso 0.25 1 calc PR A 2
H98C H -0.1190 0.1518 0.3429 0.045 Uiso 0.25 1 calc PR A 2
O3 O 0.34440(14) 0.17746(8) 0.25873(5) 0.0172(2) Uani 1 1 d . A .
N1 N 0.53024(18) 0.00041(10) 0.34613(7) 0.0192(3) Uani 1 1 d . . .
N2 N 0.31763(16) -0.03881(10) 0.24941(6) 0.0146(2) Uani 1 1 d . . .
N3 N 0.39222(16) 0.07652(9) 0.13245(6) 0.0139(2) Uani 1 1 d . . .
N4 N 0.66044(16) -0.10386(10) 0.20143(7) 0.0154(2) Uani 1 1 d . . .
N41 N 0.3644(2) 0.28347(10) 0.37883(7) 0.0232(3) Uani 1 1 d . A .
N44 N 0.02605(18) 0.44261(10) 0.33473(7) 0.0210(3) Uani 1 1 d . A .
N42 N 0.32513(16) 0.40559(9) 0.24356(6) 0.0148(2) Uani 1 1 d . A .
N43 N 0.08685(16) 0.34200(10) 0.19680(7) 0.0148(2) Uani 1 1 d . A .
C1 C 0.4425(2) 0.08522(12) 0.39502(8) 0.0246(4) Uani 1 1 d . A .
H1A H 0.4595 0.0559 0.4442 0.029 Uiso 1 1 calc R . .
H1B H 0.3170 0.1071 0.3913 0.029 Uiso 1 1 calc R . .
C2 C 0.4402(2) -0.08344(12) 0.36136(8) 0.0211(3) Uani 1 1 d . A .
H2A H 0.4138 -0.0962 0.4131 0.025 Uiso 1 1 calc R . .
H2B H 0.5164 -0.1503 0.3428 0.025 Uiso 1 1 calc R . .
C3 C 0.2741(2) -0.04988(13) 0.32719(8) 0.0198(3) Uani 1 1 d . A .
H3A H 0.2108 -0.1036 0.3401 0.024 Uiso 1 1 calc R . .
H3B H 0.1994 0.0184 0.3441 0.024 Uiso 1 1 calc R . .
C4 C 0.7126(2) -0.04483(13) 0.36035(9) 0.0267(4) Uani 1 1 d . A .
H4A H 0.7702 0.0112 0.3529 0.040 Uiso 1 1 calc R . .
H4B H 0.7719 -0.1001 0.3282 0.040 Uiso 1 1 calc R . .
H4C H 0.7163 -0.0754 0.4094 0.040 Uiso 1 1 calc R . .
C5 C 0.16950(19) 0.02662(13) 0.21299(8) 0.0186(3) Uani 1 1 d . A .
H5A H 0.1073 0.0894 0.2394 0.022 Uiso 1 1 calc R . .
H5B H 0.0882 -0.0149 0.2108 0.022 Uiso 1 1 calc R . .
C6 C 0.2352(2) 0.06115(12) 0.13932(8) 0.0175(3) Uani 1 1 d . A .
C7 C 0.1395(2) 0.07938(15) 0.08277(9) 0.0278(4) Uani 1 1 d . . .
H7 H 0.0297 0.0668 0.0884 0.033 Uiso 1 1 calc R A .
C8 C 0.2073(3) 0.11635(15) 0.01786(9) 0.0318(4) Uani 1 1 d . A .
H8 H 0.1438 0.1299 -0.0217 0.038 Uiso 1 1 calc R . .
C9 C 0.3670(2) 0.13332(13) 0.01086(9) 0.0262(4) Uani 1 1 d . . .
H9 H 0.4148 0.1591 -0.0333 0.031 Uiso 1 1 calc R A .
C10 C 0.4569(2) 0.11235(12) 0.06916(8) 0.0191(3) Uani 1 1 d . A .
H10 H 0.5676 0.1236 0.0643 0.023 Uiso 1 1 calc R . .
C25 C 0.3857(2) -0.14375(12) 0.21995(8) 0.0178(3) Uani 1 1 d . A .
H25A H 0.3289 -0.1422 0.1775 0.021 Uiso 1 1 calc R . .
H25B H 0.3550 -0.1977 0.2553 0.021 Uiso 1 1 calc R . .
C26 C 0.5771(2) -0.17630(12) 0.20018(7) 0.0151(3) Uani 1 1 d . A .
C27 C 0.6609(2) -0.27704(12) 0.17797(8) 0.0212(3) Uani 1 1 d . . .
H27 H 0.5989 -0.3274 0.1786 0.025 Uiso 1 1 calc R A .
C28 C 0.8349(2) -0.30253(13) 0.15509(9) 0.0243(4) Uani 1 1 d . A .
H28 H 0.8942 -0.3703 0.1387 0.029 Uiso 1 1 calc R . .
C29 C 0.9224(2) -0.22837(13) 0.15617(8) 0.0228(3) Uani 1 1 d . . .
H29 H 1.0427 -0.2443 0.1411 0.027 Uiso 1 1 calc R A .
C30 C 0.8313(2) -0.13118(13) 0.17958(8) 0.0197(3) Uani 1 1 d . A .
H30 H 0.8918 -0.0805 0.1804 0.024 Uiso 1 1 calc R . .
C41 C 0.5084(2) 0.18267(12) 0.37979(9) 0.0249(4) Uani 1 1 d . . .
H41A H 0.5820 0.1831 0.4164 0.030 Uiso 1 1 calc R A .
H41B H 0.5807 0.1785 0.3334 0.030 Uiso 1 1 calc R . .
C42 C 0.4418(2) 0.37281(13) 0.35727(9) 0.0260(4) Uani 1 1 d . . .
H42A H 0.5479 0.3600 0.3802 0.031 Uiso 1 1 calc R A .
H42B H 0.3591 0.4398 0.3729 0.031 Uiso 1 1 calc R . .
C43 C 0.4851(2) 0.38222(12) 0.27780(9) 0.0205(3) Uani 1 1 d . A .
H43A H 0.5404 0.4397 0.2638 0.025 Uiso 1 1 calc R . .
H43B H 0.5674 0.3152 0.2621 0.025 Uiso 1 1 calc R . .
C44 C 0.2728(3) 0.29638(14) 0.45151(9) 0.0326(4) Uani 1 1 d . . .
H44A H 0.3562 0.2910 0.4847 0.049 Uiso 1 1 calc R A .
H44B H 0.2154 0.2407 0.4649 0.049 Uiso 1 1 calc R . .
H44C H 0.1866 0.3659 0.4529 0.049 Uiso 1 1 calc R . .
C45 C 0.35998(19) 0.38099(11) 0.16832(7) 0.0141(3) Uani 1 1 d . . .
H45A H 0.4516 0.3130 0.1629 0.017 Uiso 1 1 calc R A .
H45B H 0.3996 0.4374 0.1386 0.017 Uiso 1 1 calc R . .
C46 C 0.19547(18) 0.37359(11) 0.14541(8) 0.0135(3) Uani 1 1 d . A .
C47 C 0.1585(2) 0.39565(12) 0.07593(8) 0.0189(3) Uani 1 1 d . . .
H47 H 0.2370 0.4175 0.0402 0.023 Uiso 1 1 calc R A .
C48 C 0.0048(2) 0.38527(13) 0.05962(9) 0.0247(4) Uani 1 1 d . A .
H48 H -0.0228 0.3995 0.0123 0.030 Uiso 1 1 calc R . .
C49 C -0.1083(2) 0.35404(14) 0.11272(10) 0.0263(4) Uani 1 1 d . . .
H49 H -0.2152 0.3478 0.1027 0.032 Uiso 1 1 calc R A .
C50 C -0.0620(2) 0.33227(12) 0.18042(9) 0.0213(3) Uani 1 1 d . A .
H50 H -0.1381 0.3095 0.2169 0.026 Uiso 1 1 calc R . .
C65 C 0.2194(2) 0.51728(11) 0.24983(8) 0.0187(3) Uani 1 1 d . . .
H65A H 0.1800 0.5473 0.2034 0.022 Uiso 1 1 calc R A .
H65B H 0.2929 0.5585 0.2619 0.022 Uiso 1 1 calc R . .
C66 C 0.0648(2) 0.53006(12) 0.30454(8) 0.0177(3) Uani 1 1 d . A .
C67 C -0.0351(2) 0.63039(12) 0.32188(8) 0.0231(3) Uani 1 1 d . . .
H67 H -0.0037 0.6914 0.3007 0.028 Uiso 1 1 calc R A .
C68 C -0.1801(2) 0.64045(13) 0.37014(9) 0.0278(4) Uani 1 1 d . A .
H68 H -0.2509 0.7086 0.3821 0.033 Uiso 1 1 calc R . .
C69 C -0.2219(2) 0.55074(14) 0.40102(9) 0.0272(4) Uani 1 1 d . . .
H69 H -0.3220 0.5560 0.4342 0.033 Uiso 1 1 calc R A .
C70 C -0.1154(2) 0.45374(14) 0.38270(9) 0.0266(4) Uani 1 1 d . A .
H70 H -0.1424 0.3918 0.4047 0.032 Uiso 1 1 calc R . .
Cl3 Cl -0.25389(6) 0.31776(3) 0.57423(2) 0.02582(9) Uani 1 1 d . . .
O31 O -0.09297(18) 0.23542(10) 0.57599(8) 0.0374(3) Uani 1 1 d . . .
O32 O -0.34387(19) 0.32698(11) 0.64448(7) 0.0350(3) Uani 1 1 d . . .
O33 O -0.2203(2) 0.41609(10) 0.54836(7) 0.0445(4) Uani 1 1 d . . .
O34 O -0.3578(2) 0.29047(13) 0.52932(9) 0.0519(4) Uani 1 1 d . . .
Cl4 Cl -0.37731(5) 0.33986(3) -0.050966(19) 0.01744(8) Uani 1 1 d . . .
O41 O -0.52806(16) 0.41111(10) -0.07871(7) 0.0315(3) Uani 1 1 d . . .
O42 O -0.41230(17) 0.32062(10) 0.02404(6) 0.0288(3) Uani 1 1 d . . .
O43 O -0.23517(15) 0.38559(9) -0.06700(6) 0.0219(2) Uani 1 1 d . . .
O44 O -0.33158(17) 0.24083(10) -0.08351(7) 0.0292(3) Uani 1 1 d . . .
C1M C 0.0000 0.0000 0.5000 0.0265(14) Uiso 0.70 2 d SP . .
O1M O -0.1810(5) 0.0634(3) 0.49497(18) 0.0264(7) Uiso 0.35 1 d P . .
O1MB O -0.063(2) -0.0487(13) 0.4897(9) 0.079(4) Uiso 0.15 1 d P . .
C1MB C 0.044(3) -0.0057(13) 0.5087(8) 0.035(4) Uiso 0.15 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
Fe1 O3 1.7786(10) . ?
Fe1 N3 2.1653(12) . ?
Fe1 N2 2.2052(13) . ?
Fe1 N4 2.2559(13) . ?
Fe1 N1 2.2614(13) . ?
Fe1 Cl1 2.2982(5) . ?
Fe1 Fe2 3.5693(4) . ?
Fe2 O98 1.745(6) . ?
Fe2 O3 1.7974(10) . ?
Fe2 N43 2.1608(13) . ?
Fe2 N44 2.2011(13) . ?
Fe2 N42 2.2204(13) . ?
Fe2 N41 2.2501(14) . ?
Fe2 Cl2 2.3311(11) . ?
O98 C98 1.416(10) . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
N1 C4 1.484(2) . ?
N1 C2 1.489(2) . ?
N1 C1 1.493(2) . ?
N2 C5 1.4772(19) . ?
N2 C3 1.4817(19) . ?
N2 C25 1.4825(19) . ?
N3 C10 1.3435(19) . ?
N3 C6 1.344(2) . ?
N4 C26 1.3387(19) . ?
N4 C30 1.349(2) . ?
N41 C44 1.485(2) . ?
N41 C41 1.495(2) . ?
N41 C42 1.495(2) . ?
N44 C66 1.338(2) . ?
N44 C70 1.350(2) . ?
N42 C43 1.4823(19) . ?
N42 C45 1.4841(18) . ?
N42 C65 1.4844(18) . ?
N43 C46 1.3434(19) . ?
N43 C50 1.346(2) . ?
C1 C41 1.527(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.516(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.505(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.385(2) . ?
C7 C8 1.383(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(2) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C25 C26 1.496(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.392(2) . ?
C27 C28 1.377(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.382(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.372(2) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.512(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.507(2) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.387(2) . ?
C47 C48 1.387(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.385(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.379(2) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C65 C66 1.501(2) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.387(2) . ?
C67 C68 1.376(3) . ?
C67 H67 0.9500 . ?
C68 C69 1.380(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.373(2) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
Cl3 O33 1.4310(14) . ?
Cl3 O32 1.4368(13) . ?
Cl3 O34 1.4370(15) . ?
Cl3 O31 1.4384(14) . ?
Cl4 O42 1.4323(12) . ?
Cl4 O41 1.4392(13) . ?
Cl4 O43 1.4445(11) . ?
Cl4 O44 1.4447(12) . ?
C1M C1MB 0.40(2) 2_556 ?
C1M O1MB 0.988(17) . ?
C1M O1MB 0.988(17) 2_556 ?
C1M O1M 1.477(4) . ?
C1M O1M 1.477(4) 2_556 ?
O1M C1MB 1.149(19) 2_556 ?
O1M O1MB 1.519(17) . ?
O1M C1MB 1.84(2) . ?
O1MB C1MB 0.79(2) 2_556 ?
O1MB C1MB 1.29(3) . ?
C1MB O1MB 0.79(2) 2_556 ?
C1MB C1MB 0.80(4) 2_556 ?
C1MB O1M 1.149(19) 2_556 ?

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
O3 Fe1 N3 90.94(5) . . ?
O3 Fe1 N2 95.88(5) . . ?
N3 Fe1 N2 75.09(5) . . ?
O3 Fe1 N4 171.18(5) . . ?
N3 Fe1 N4 86.89(5) . . ?
N2 Fe1 N4 75.31(5) . . ?
O3 Fe1 N1 90.29(5) . . ?
N3 Fe1 N1 156.18(5) . . ?
N2 Fe1 N1 81.12(5) . . ?
N4 Fe1 N1 88.28(5) . . ?
O3 Fe1 Cl1 98.95(4) . . ?
N3 Fe1 Cl1 99.89(4) . . ?
N2 Fe1 Cl1 164.44(4) . . ?
N4 Fe1 Cl1 89.84(3) . . ?
N1 Fe1 Cl1 103.41(4) . . ?
O3 Fe1 Fe2 3.53(3) . . ?
N3 Fe1 Fe2 93.92(3) . . ?
N2 Fe1 Fe2 94.82(3) . . ?
N4 Fe1 Fe2 169.55(3) . . ?
N1 Fe1 Fe2 86.80(3) . . ?
Cl1 Fe1 Fe2 100.262(14) . . ?
O98 Fe2 O3 95.02(19) . . ?
O98 Fe2 N43 109.1(2) . . ?
O3 Fe2 N43 90.59(5) . . ?
O98 Fe2 N44 93.77(19) . . ?
O3 Fe2 N44 171.17(5) . . ?
N43 Fe2 N44 87.31(5) . . ?
O98 Fe2 N42 169.78(19) . . ?
O3 Fe2 N42 94.60(5) . . ?
N43 Fe2 N42 74.17(5) . . ?
N44 Fe2 N42 76.57(5) . . ?
O98 Fe2 N41 95.7(2) . . ?
O3 Fe2 N41 90.14(5) . . ?
N43 Fe2 N41 154.94(5) . . ?
N44 Fe2 N41 88.16(5) . . ?
N42 Fe2 N41 80.81(5) . . ?
O98 Fe2 Cl2 12.7(2) . . ?
O3 Fe2 Cl2 99.62(4) . . ?
N43 Fe2 Cl2 97.18(4) . . ?
N44 Fe2 Cl2 89.15(4) . . ?
N42 Fe2 Cl2 163.46(4) . . ?
N41 Fe2 Cl2 107.39(4) . . ?
O98 Fe2 Fe1 92.67(19) . . ?
O3 Fe2 Fe1 3.49(3) . . ?
N43 Fe2 Fe1 93.80(3) . . ?
N44 Fe2 Fe1 172.72(4) . . ?
N42 Fe2 Fe1 96.79(3) . . ?
N41 Fe2 Fe1 87.81(4) . . ?
Cl2 Fe2 Fe1 97.846(19) . . ?
C98 O98 Fe2 142.1(6) . . ?
O98 C98 H98A 109.5 . . ?
O98 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
O98 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
Fe1 O3 Fe2 172.98(7) . . ?
C4 N1 C2 109.45(12) . . ?
C4 N1 C1 108.76(12) . . ?
C2 N1 C1 107.71(13) . . ?
C4 N1 Fe1 113.97(11) . . ?
C2 N1 Fe1 104.66(9) . . ?
C1 N1 Fe1 112.02(9) . . ?
C5 N2 C3 112.57(12) . . ?
C5 N2 C25 109.76(12) . . ?
C3 N2 C25 111.21(12) . . ?
C5 N2 Fe1 103.29(9) . . ?
C3 N2 Fe1 105.10(9) . . ?
C25 N2 Fe1 114.67(9) . . ?
C10 N3 C6 119.03(13) . . ?
C10 N3 Fe1 126.84(11) . . ?
C6 N3 Fe1 113.63(10) . . ?
C26 N4 C30 117.58(13) . . ?
C26 N4 Fe1 116.92(10) . . ?
C30 N4 Fe1 125.31(10) . . ?
C44 N41 C41 108.54(13) . . ?
C44 N41 C42 108.91(13) . . ?
C41 N41 C42 107.88(14) . . ?
C44 N41 Fe2 113.54(12) . . ?
C41 N41 Fe2 111.92(9) . . ?
C42 N41 Fe2 105.86(9) . . ?
C66 N44 C70 118.38(14) . . ?
C66 N44 Fe2 117.03(10) . . ?
C70 N44 Fe2 124.46(11) . . ?
C43 N42 C45 112.66(12) . . ?
C43 N42 C65 111.33(12) . . ?
C45 N42 C65 110.21(11) . . ?
C43 N42 Fe2 105.26(9) . . ?
C45 N42 Fe2 104.32(8) . . ?
C65 N42 Fe2 112.80(9) . . ?
C46 N43 C50 119.07(13) . . ?
C46 N43 Fe2 114.55(10) . . ?
C50 N43 Fe2 125.80(11) . . ?
N1 C1 C41 113.50(14) . . ?
N1 C1 H1A 108.9 . . ?
C41 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C41 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C3 110.21(12) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C2 108.66(13) . . ?
N2 C3 H3A 110.0 . . ?
C2 C3 H3A 110.0 . . ?
N2 C3 H3B 110.0 . . ?
C2 C3 H3B 110.0 . . ?
H3A C3 H3B 108.3 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 108.89(12) . . ?
N2 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N2 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N3 C6 C7 121.93(15) . . ?
N3 C6 C5 115.21(13) . . ?
C7 C6 C5 122.82(15) . . ?
C8 C7 C6 118.54(17) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C9 C8 C7 119.66(16) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 118.94(15) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N3 C10 C9 121.89(15) . . ?
N3 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N2 C25 C26 113.75(12) . . ?
N2 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N2 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N4 C26 C27 122.32(14) . . ?
N4 C26 C25 117.58(13) . . ?
C27 C26 C25 120.01(14) . . ?
C28 C27 C26 118.97(15) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 119.21(15) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.43(15) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N4 C30 C29 123.48(15) . . ?
N4 C30 H30 118.3 . . ?
C29 C30 H30 118.3 . . ?
N41 C41 C1 112.18(15) . . ?
N41 C41 H41A 109.2 . . ?
C1 C41 H41A 109.2 . . ?
N41 C41 H41B 109.2 . . ?
C1 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
N41 C42 C43 109.93(12) . . ?
N41 C42 H42A 109.7 . . ?
C43 C42 H42A 109.7 . . ?
N41 C42 H42B 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
N42 C43 C42 109.58(14) . . ?
N42 C43 H43A 109.8 . . ?
C42 C43 H43A 109.8 . . ?
N42 C43 H43B 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.2 . . ?
N41 C44 H44A 109.5 . . ?
N41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N42 C45 C46 108.33(12) . . ?
N42 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
N42 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
N43 C46 C47 121.63(14) . . ?
N43 C46 C45 115.49(12) . . ?
C47 C46 C45 122.87(13) . . ?
C46 C47 C48 118.82(15) . . ?
C46 C47 H47 120.6 . . ?
C48 C47 H47 120.6 . . ?
C49 C48 C47 119.59(15) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C50 C49 C48 118.35(15) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
N43 C50 C49 122.52(15) . . ?
N43 C50 H50 118.7 . . ?
C49 C50 H50 118.7 . . ?
N42 C65 C66 113.69(12) . . ?
N42 C65 H65A 108.8 . . ?
C66 C65 H65A 108.8 . . ?
N42 C65 H65B 108.8 . . ?
C66 C65 H65B 108.8 . . ?
H65A C65 H65B 107.7 . . ?
N44 C66 C67 121.75(15) . . ?
N44 C66 C65 118.12(13) . . ?
C67 C66 C65 120.12(14) . . ?
C68 C67 C66 119.15(16) . . ?
C68 C67 H67 120.4 . . ?
C66 C67 H67 120.4 . . ?
C67 C68 C69 119.46(15) . . ?
C67 C68 H68 120.3 . . ?
C69 C68 H68 120.3 . . ?
C70 C69 C68 118.44(16) . . ?
C70 C69 H69 120.8 . . ?
C68 C69 H69 120.8 . . ?
N44 C70 C69 122.80(16) . . ?
N44 C70 H70 118.6 . . ?
C69 C70 H70 118.6 . . ?
O33 Cl3 O32 109.33(8) . . ?
O33 Cl3 O34 110.64(10) . . ?
O32 Cl3 O34 109.05(10) . . ?
O33 Cl3 O31 109.38(10) . . ?
O32 Cl3 O31 109.33(9) . . ?
O34 Cl3 O31 109.09(9) . . ?
O42 Cl4 O41 109.89(8) . . ?
O42 Cl4 O43 109.82(7) . . ?
O41 Cl4 O43 109.56(8) . . ?
O42 Cl4 O44 109.26(8) . . ?
O41 Cl4 O44 109.24(8) . . ?
O43 Cl4 O44 109.05(7) . . ?
C1MB C1M O1MB 49(2) 2_556 . ?
C1MB C1M O1MB 131(2) 2_556 2_556 ?
O1MB C1M O1MB 180.0(11) . 2_556 ?
C1MB C1M O1M 30(2) 2_556 . ?
O1MB C1M O1M 73.0(10) . . ?
O1MB C1M O1M 107.0(10) 2_556 . ?
C1MB C1M O1M 150(2) 2_556 2_556 ?
O1MB C1M O1M 107.0(10) . 2_556 ?
O1MB C1M O1M 73.0(10) 2_556 2_556 ?
O1M C1M O1M 180.0(3) . 2_556 ?
C1MB O1M C1M 10.2(9) 2_556 . ?
C1MB O1M O1MB 30.4(11) 2_556 . ?
C1M O1M O1MB 38.5(7) . . ?
C1MB O1M C1MB 16.6(14) 2_556 . ?
C1M O1M C1MB 6.4(5) . . ?
O1MB O1M C1MB 43.9(9) . . ?
C1MB O1MB C1M 22.7(18) 2_556 . ?
C1MB O1MB C1MB 36(3) 2_556 . ?
C1M O1MB C1MB 13.6(9) . . ?
C1MB O1MB O1M 47.8(19) 2_556 . ?
C1M O1MB O1M 68.5(10) . . ?
C1MB O1MB O1M 81.2(13) . . ?
O1MB C1MB C1MB 108(3) 2_556 2_556 ?
O1MB C1MB O1M 102(3) 2_556 2_556 ?
C1MB C1MB O1M 139(3) 2_556 2_556 ?
O1MB C1MB O1MB 144(3) 2_556 . ?
C1MB C1MB O1MB 35.4(17) 2_556 . ?
O1M C1MB O1MB 110.4(15) 2_556 . ?
O1MB C1MB O1M 90(2) 2_556 . ?
C1MB C1MB O1M 24.0(18) 2_556 . ?
O1M C1MB O1M 163.4(14) 2_556 . ?
O1MB C1MB O1M 54.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.051
####################################################################### 
# 
# 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_g2214
_database_code_depnum_ccdc_archive 'CCDC 1024401'
_audit_update_record             
;
2014-09-15 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H42 N8 Fe2 Cl2 , 2(Cl O4) , 0.5(C2 H6 O)'
_chemical_formula_sum            'C33 H45 Cl4 Fe2 N8 O9.50'
_chemical_formula_weight         959.27

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.1714(4)
_cell_length_b                   13.1963(6)
_cell_length_c                   19.2643(10)
_cell_angle_alpha                83.133(2)
_cell_angle_beta                 81.364(2)
_cell_angle_gamma                72.765(2)
_cell_volume                     1955.33(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9954
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.00

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             990
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7664
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_process_details   'TWINABS 2012/1 (Bruker AXS, 2012)'

_exptl_special_details           
; 
The crystal was twinned, ratio 54:46 , by rotation of about 180 degrees
about reciprocal axes 0 0 1. The solvent EtOH molecule is disordered 
around a crystallographic centre of inversion.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       'Bruker KAPPA APEX II'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            75009
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         27.00
_reflns_number_total             8055
_reflns_number_gt                7683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_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)+(0.0533P)²+2.3249P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8055
_refine_ls_number_parameters     508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0983
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.013
_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 0.99509(6) 0.05749(4) 0.22971(3) 0.01091(10) Uani 1 1 d . . .
Fe2 Fe 0.68777(6) 0.28974(4) 0.29636(3) 0.01253(11) Uani 1 1 d . . .
O3 O 0.8396(3) 0.17584(18) 0.25791(13) 0.0131(4) Uani 1 1 d . . .
Cl1 Cl 1.22678(10) 0.12349(7) 0.19291(5) 0.01995(18) Uani 1 1 d . . .
Cl2 Cl 0.48014(12) 0.20945(7) 0.35080(5) 0.0255(2) Uani 1 1 d . . .
N1 N 1.0300(4) -0.0018(2) 0.34278(16) 0.0160(6) Uani 1 1 d . . .
N2 N 0.8159(3) -0.0415(2) 0.24762(15) 0.0130(5) Uani 1 1 d . . .
N3 N 0.8879(3) 0.0759(2) 0.13170(15) 0.0132(6) Uani 1 1 d . . .
N4 N 1.1580(4) -0.1050(2) 0.19872(16) 0.0143(6) Uani 1 1 d . . .
N41 N 0.8651(4) 0.2818(2) 0.37684(16) 0.0177(6) Uani 1 1 d . . .
N42 N 0.8234(3) 0.4057(2) 0.24289(14) 0.0119(5) Uani 1 1 d . . .
N43 N 0.5833(3) 0.3419(2) 0.19765(15) 0.0135(6) Uani 1 1 d . . .
N44 N 0.5244(4) 0.4423(2) 0.33476(16) 0.0169(6) Uani 1 1 d . . .
C1 C 0.9438(5) 0.0822(3) 0.39227(19) 0.0198(7) Uani 1 1 d . . .
H1A H 0.9631 0.0520 0.4409 0.024 Uiso 1 1 calc R . .
H1B H 0.8179 0.1036 0.3897 0.024 Uiso 1 1 calc R . .
C2 C 0.9406(5) -0.0871(3) 0.3582(2) 0.0195(7) Uani 1 1 d . . .
H2A H 0.9155 -0.1006 0.4098 0.023 Uiso 1 1 calc R . .
H2B H 1.0168 -0.1538 0.3392 0.023 Uiso 1 1 calc R . .
C3 C 0.7738(4) -0.0538(3) 0.32519(18) 0.0161(7) Uani 1 1 d . . .
H3A H 0.7113 -0.1085 0.3381 0.019 Uiso 1 1 calc R . .
H3B H 0.6989 0.0144 0.3426 0.019 Uiso 1 1 calc R . .
C4 C 1.2128(5) -0.0465(3) 0.3551(2) 0.0230(8) Uani 1 1 d . . .
H4A H 1.2709 0.0097 0.3457 0.034 Uiso 1 1 calc R . .
H4B H 1.2698 -0.1032 0.3236 0.034 Uiso 1 1 calc R . .
H4C H 1.2189 -0.0759 0.4042 0.034 Uiso 1 1 calc R . .
C5 C 0.6662(4) 0.0241(3) 0.21251(18) 0.0161(7) Uani 1 1 d . . .
H5A H 0.6047 0.0869 0.2391 0.019 Uiso 1 1 calc R . .
H5B H 0.5849 -0.0179 0.2109 0.019 Uiso 1 1 calc R . .
C6 C 0.7302(4) 0.0597(3) 0.13874(18) 0.0157(7) Uani 1 1 d . . .
C7 C 0.6351(5) 0.0775(3) 0.0835(2) 0.0225(8) Uani 1 1 d . . .
H7 H 0.5258 0.0639 0.0895 0.027 Uiso 1 1 calc R . .
C8 C 0.7020(6) 0.1161(3) 0.0182(2) 0.0296(9) Uani 1 1 d . . .
H8 H 0.6377 0.1302 -0.0208 0.035 Uiso 1 1 calc R . .
C9 C 0.8612(5) 0.1333(3) 0.0108(2) 0.0235(8) Uani 1 1 d . . .
H9 H 0.9087 0.1593 -0.0334 0.028 Uiso 1 1 calc R . .
C10 C 0.9519(4) 0.1125(3) 0.06852(18) 0.0161(7) Uani 1 1 d . . .
H10 H 1.0624 0.1245 0.0633 0.019 Uiso 1 1 calc R . .
C25 C 0.8842(4) -0.1466(3) 0.21807(19) 0.0161(7) Uani 1 1 d . . .
H25A H 0.8279 -0.1448 0.1757 0.019 Uiso 1 1 calc R . .
H25B H 0.8530 -0.2011 0.2531 0.019 Uiso 1 1 calc R . .
C26 C 1.0765(4) -0.1788(3) 0.19843(18) 0.0148(7) Uani 1 1 d . . .
C27 C 1.1608(5) -0.2805(3) 0.1775(2) 0.0202(7) Uani 1 1 d . . .
H27 H 1.0990 -0.3315 0.1787 0.024 Uiso 1 1 calc R . .
C28 C 1.3347(5) -0.3060(3) 0.1550(2) 0.0224(8) Uani 1 1 d . . .
H28 H 1.3947 -0.3746 0.1398 0.027 Uiso 1 1 calc R . .
C29 C 1.4219(5) -0.2298(3) 0.1549(2) 0.0206(7) Uani 1 1 d . . .
H29 H 1.5423 -0.2452 0.1398 0.025 Uiso 1 1 calc R . .
C30 C 1.3292(4) -0.1314(3) 0.17726(19) 0.0178(7) Uani 1 1 d . . .
H30 H 1.3887 -0.0796 0.1776 0.021 Uiso 1 1 calc R . .
C41 C 1.0082(5) 0.1808(3) 0.3769(2) 0.0185(7) Uani 1 1 d . . .
H41A H 1.0828 0.1811 0.4129 0.022 Uiso 1 1 calc R . .
H41B H 1.0794 0.1772 0.3304 0.022 Uiso 1 1 calc R . .
C42 C 0.9422(5) 0.3720(3) 0.35533(19) 0.0200(7) Uani 1 1 d . . .
H42A H 1.0484 0.3593 0.3779 0.024 Uiso 1 1 calc R . .
H42B H 0.8596 0.4391 0.3710 0.024 Uiso 1 1 calc R . .
C43 C 0.9849(4) 0.3815(3) 0.27613(19) 0.0170(7) Uani 1 1 d . . .
H43A H 1.0410 0.4390 0.2619 0.020 Uiso 1 1 calc R . .
H43B H 1.0659 0.3140 0.2603 0.020 Uiso 1 1 calc R . .
C44 C 0.7739(6) 0.2944(3) 0.44987(19) 0.0262(8) Uani 1 1 d . . .
H44A H 0.7183 0.2375 0.4638 0.039 Uiso 1 1 calc R . .
H44B H 0.6862 0.3636 0.4513 0.039 Uiso 1 1 calc R . .
H44C H 0.8574 0.2905 0.4824 0.039 Uiso 1 1 calc R . .
C45 C 0.8575(4) 0.3813(3) 0.16763(18) 0.0126(6) Uani 1 1 d . . .
H45A H 0.9488 0.3132 0.1619 0.015 Uiso 1 1 calc R . .
H45B H 0.8970 0.4382 0.1380 0.015 Uiso 1 1 calc R . .
C46 C 0.6918(4) 0.3739(2) 0.14547(18) 0.0130(6) Uani 1 1 d . . .
C47 C 0.6551(5) 0.3960(3) 0.0772(2) 0.0185(7) Uani 1 1 d . . .
H47 H 0.7336 0.4180 0.0413 0.022 Uiso 1 1 calc R . .
C48 C 0.5001(5) 0.3855(3) 0.0616(2) 0.0217(8) Uani 1 1 d . . .
H48 H 0.4717 0.4000 0.0147 0.026 Uiso 1 1 calc R . .
C49 C 0.3886(5) 0.3541(3) 0.1145(2) 0.0250(8) Uani 1 1 d . . .
H49 H 0.2816 0.3475 0.1049 0.030 Uiso 1 1 calc R . .
C50 C 0.4344(4) 0.3322(3) 0.1817(2) 0.0195(7) Uani 1 1 d . . .
H50 H 0.3580 0.3095 0.2182 0.023 Uiso 1 1 calc R . .
C65 C 0.7192(4) 0.5176(3) 0.24927(19) 0.0171(7) Uani 1 1 d . . .
H65A H 0.6790 0.5480 0.2032 0.020 Uiso 1 1 calc R . .
H65B H 0.7933 0.5590 0.2609 0.020 Uiso 1 1 calc R . .
C66 C 0.5651(4) 0.5298(3) 0.30461(18) 0.0159(7) Uani 1 1 d . . .
C67 C 0.4658(5) 0.6308(3) 0.32202(19) 0.0213(8) Uani 1 1 d . . .
H67 H 0.4969 0.6922 0.3005 0.026 Uiso 1 1 calc R . .
C68 C 0.3214(5) 0.6407(3) 0.3710(2) 0.0252(8) Uani 1 1 d . . .
H68 H 0.2517 0.7092 0.3833 0.030 Uiso 1 1 calc R . .
C69 C 0.2791(5) 0.5512(3) 0.4018(2) 0.0224(8) Uani 1 1 d . . .
H69 H 0.1796 0.5566 0.4353 0.027 Uiso 1 1 calc R . .
C70 C 0.3838(5) 0.4536(3) 0.38316(19) 0.0213(7) Uani 1 1 d . . .
H70 H 0.3562 0.3914 0.4053 0.026 Uiso 1 1 calc R . .
Cl3 Cl 0.87785(10) 0.66029(7) 0.04943(4) 0.01645(17) Uani 1 1 d . . .
O31 O 1.0284(4) 0.5893(2) 0.07722(17) 0.0318(7) Uani 1 1 d . . .
O32 O 0.7355(3) 0.6144(2) 0.06604(14) 0.0206(5) Uani 1 1 d . . .
O33 O 0.8321(4) 0.7609(2) 0.08059(16) 0.0291(6) Uani 1 1 d . . .
O34 O 0.9145(4) 0.6781(2) -0.02522(14) 0.0277(6) Uani 1 1 d . . .
Cl4 Cl 0.24337(13) 0.32143(7) 0.57427(5) 0.0251(2) Uani 1 1 d . . .
O41 O 0.2794(5) 0.4199(2) 0.54931(17) 0.0393(8) Uani 1 1 d . . .
O42 O 0.1385(5) 0.2956(3) 0.5289(2) 0.0498(10) Uani 1 1 d . . .
O43 O 0.4028(4) 0.2376(2) 0.57565(19) 0.0356(7) Uani 1 1 d . . .
O44 O 0.1520(4) 0.3299(2) 0.64403(17) 0.0345(7) Uani 1 1 d . . .
O1S O 0.2993(8) 0.0664(5) 0.4948(4) 0.0382(15) Uiso 0.50 1 d P . .
C1S C 0.4246(13) -0.0065(8) 0.4825(6) 0.063(2) Uiso 0.70 1 d P . .
C2S C 0.5000 0.0000 0.5000 0.097(7) Uiso 0.60 2 d SP . .


_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 O3 1.780(2) . ?
Fe1 N3 2.157(3) . ?
Fe1 N2 2.201(3) . ?
Fe1 N1 2.255(3) . ?
Fe1 N4 2.259(3) . ?
Fe1 Cl1 2.2961(10) . ?
Fe1 Fe2 3.5721(7) . ?
Fe2 O3 1.798(2) . ?
Fe2 N43 2.155(3) . ?
Fe2 N44 2.202(3) . ?
Fe2 N42 2.217(3) . ?
Fe2 N41 2.249(3) . ?
Fe2 Cl2 2.3166(11) . ?
N1 C4 1.478(4) . ?
N1 C1 1.491(4) . ?
N1 C2 1.493(5) . ?
N2 C5 1.478(4) . ?
N2 C25 1.480(4) . ?
N2 C3 1.483(4) . ?
N3 C10 1.344(4) . ?
N3 C6 1.353(4) . ?
N4 C26 1.334(4) . ?
N4 C30 1.349(4) . ?
N41 C41 1.491(4) . ?
N41 C44 1.493(5) . ?
N41 C42 1.495(5) . ?
N42 C65 1.479(4) . ?
N42 C43 1.486(4) . ?
N42 C45 1.490(4) . ?
N43 C50 1.343(4) . ?
N43 C46 1.352(4) . ?
N44 C66 1.338(5) . ?
N44 C70 1.350(4) . ?
C1 C41 1.524(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.515(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.508(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.368(5) . ?
C7 C8 1.395(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.370(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C25 C26 1.502(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.391(5) . ?
C27 C28 1.374(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.394(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.512(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.513(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.371(5) . ?
C47 C48 1.393(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.373(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.375(6) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C65 C66 1.505(5) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.390(5) . ?
C67 C68 1.379(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.371(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.373(5) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
Cl3 O34 1.430(3) . ?
Cl3 O31 1.440(3) . ?
Cl3 O32 1.443(3) . ?
Cl3 O33 1.446(3) . ?
Cl4 O41 1.428(3) . ?
Cl4 O44 1.436(3) . ?
Cl4 O43 1.439(3) . ?
Cl4 O42 1.443(3) . ?
O1S C1S 1.194(11) . ?
O1S C2S 1.626(7) . ?
C1S C2S 0.775(10) . ?
C1S C1S 1.55(2) 2_656 ?
C2S C1S 0.775(10) 2_656 ?
C2S O1S 1.626(7) 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
O3 Fe1 N3 91.16(11) . . ?
O3 Fe1 N2 95.62(10) . . ?
N3 Fe1 N2 75.10(10) . . ?
O3 Fe1 N1 90.17(11) . . ?
N3 Fe1 N1 156.41(11) . . ?
N2 Fe1 N1 81.33(11) . . ?
O3 Fe1 N4 170.87(11) . . ?
N3 Fe1 N4 86.95(10) . . ?
N2 Fe1 N4 75.25(10) . . ?
N1 Fe1 N4 88.03(10) . . ?
O3 Fe1 Cl1 99.42(8) . . ?
N3 Fe1 Cl1 99.97(8) . . ?
N2 Fe1 Cl1 164.29(8) . . ?
N1 Fe1 Cl1 103.04(8) . . ?
N4 Fe1 Cl1 89.71(8) . . ?
O3 Fe1 Fe2 3.26(8) . . ?
N3 Fe1 Fe2 94.22(7) . . ?
N2 Fe1 Fe2 95.32(7) . . ?
N1 Fe1 Fe2 86.91(7) . . ?
N4 Fe1 Fe2 169.89(8) . . ?
Cl1 Fe1 Fe2 99.96(3) . . ?
O3 Fe2 N43 90.44(11) . . ?
O3 Fe2 N44 172.00(11) . . ?
N43 Fe2 N44 87.28(11) . . ?
O3 Fe2 N42 95.17(10) . . ?
N43 Fe2 N42 74.38(10) . . ?
N44 Fe2 N42 76.83(11) . . ?
O3 Fe2 N41 90.28(11) . . ?
N43 Fe2 N41 155.07(11) . . ?
N44 Fe2 N41 88.57(11) . . ?
N42 Fe2 N41 80.74(11) . . ?
O3 Fe2 Cl2 98.75(8) . . ?
N43 Fe2 Cl2 97.78(8) . . ?
N44 Fe2 Cl2 89.16(8) . . ?
N42 Fe2 Cl2 164.10(7) . . ?
N41 Fe2 Cl2 106.73(9) . . ?
O3 Fe2 Fe1 3.23(8) . . ?
N43 Fe2 Fe1 93.61(7) . . ?
N44 Fe2 Fe1 172.90(8) . . ?
N42 Fe2 Fe1 96.61(7) . . ?
N41 Fe2 Fe1 87.67(7) . . ?
Cl2 Fe2 Fe1 97.69(3) . . ?
Fe1 O3 Fe2 173.51(15) . . ?
C4 N1 C1 108.9(3) . . ?
C4 N1 C2 109.6(3) . . ?
C1 N1 C2 107.8(3) . . ?
C4 N1 Fe1 113.5(2) . . ?
C1 N1 Fe1 112.3(2) . . ?
C2 N1 Fe1 104.5(2) . . ?
C5 N2 C25 110.1(3) . . ?
C5 N2 C3 112.3(3) . . ?
C25 N2 C3 111.0(3) . . ?
C5 N2 Fe1 103.3(2) . . ?
C25 N2 Fe1 114.86(19) . . ?
C3 N2 Fe1 105.1(2) . . ?
C10 N3 C6 118.8(3) . . ?
C10 N3 Fe1 126.8(2) . . ?
C6 N3 Fe1 113.9(2) . . ?
C26 N4 C30 117.7(3) . . ?
C26 N4 Fe1 117.1(2) . . ?
C30 N4 Fe1 125.1(2) . . ?
C41 N41 C44 108.8(3) . . ?
C41 N41 C42 108.1(3) . . ?
C44 N41 C42 108.7(3) . . ?
C41 N41 Fe2 111.9(2) . . ?
C44 N41 Fe2 113.2(2) . . ?
C42 N41 Fe2 105.9(2) . . ?
C65 N42 C43 111.6(3) . . ?
C65 N42 C45 110.1(2) . . ?
C43 N42 C45 112.3(3) . . ?
C65 N42 Fe2 113.0(2) . . ?
C43 N42 Fe2 105.3(2) . . ?
C45 N42 Fe2 104.37(19) . . ?
C50 N43 C46 118.5(3) . . ?
C50 N43 Fe2 126.2(2) . . ?
C46 N43 Fe2 114.7(2) . . ?
C66 N44 C70 118.6(3) . . ?
C66 N44 Fe2 116.4(2) . . ?
C70 N44 Fe2 124.9(2) . . ?
N1 C1 C41 113.5(3) . . ?
N1 C1 H1A 108.9 . . ?
C41 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C41 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C3 110.3(3) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C2 108.5(3) . . ?
N2 C3 H3A 110.0 . . ?
C2 C3 H3A 110.0 . . ?
N2 C3 H3B 110.0 . . ?
C2 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 108.7(3) . . ?
N2 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N2 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N3 C6 C7 122.2(3) . . ?
N3 C6 C5 114.6(3) . . ?
C7 C6 C5 123.1(3) . . ?
C6 C7 C8 118.6(3) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N3 C10 C9 121.7(3) . . ?
N3 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N2 C25 C26 113.6(3) . . ?
N2 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N2 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N4 C26 C27 122.7(3) . . ?
N4 C26 C25 117.3(3) . . ?
C27 C26 C25 119.9(3) . . ?
C28 C27 C26 119.0(3) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 119.0(3) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C30 C29 C28 118.3(3) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N4 C30 C29 123.3(3) . . ?
N4 C30 H30 118.4 . . ?
C29 C30 H30 118.4 . . ?
N41 C41 C1 112.8(3) . . ?
N41 C41 H41A 109.0 . . ?
C1 C41 H41A 109.0 . . ?
N41 C41 H41B 109.0 . . ?
C1 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
N41 C42 C43 109.6(3) . . ?
N41 C42 H42A 109.7 . . ?
C43 C42 H42A 109.7 . . ?
N41 C42 H42B 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
N42 C43 C42 109.3(3) . . ?
N42 C43 H43A 109.8 . . ?
C42 C43 H43A 109.8 . . ?
N42 C43 H43B 109.8 . . ?
C42 C43 H43B 109.8 . . ?
H43A C43 H43B 108.3 . . ?
N41 C44 H44A 109.5 . . ?
N41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N42 C45 C46 108.2(3) . . ?
N42 C45 H45A 110.1 . . ?
C46 C45 H45A 110.1 . . ?
N42 C45 H45B 110.1 . . ?
C46 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
N43 C46 C47 122.2(3) . . ?
N43 C46 C45 115.2(3) . . ?
C47 C46 C45 122.6(3) . . ?
C46 C47 C48 118.4(3) . . ?
C46 C47 H47 120.8 . . ?
C48 C47 H47 120.8 . . ?
C49 C48 C47 119.6(3) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C48 C49 C50 118.8(3) . . ?
C48 C49 H49 120.6 . . ?
C50 C49 H49 120.6 . . ?
N43 C50 C49 122.4(3) . . ?
N43 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
N42 C65 C66 113.3(3) . . ?
N42 C65 H65A 108.9 . . ?
C66 C65 H65A 108.9 . . ?
N42 C65 H65B 108.9 . . ?
C66 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
N44 C66 C67 121.4(3) . . ?
N44 C66 C65 118.7(3) . . ?
C67 C66 C65 119.9(3) . . ?
C68 C67 C66 119.1(4) . . ?
C68 C67 H67 120.4 . . ?
C66 C67 H67 120.4 . . ?
C69 C68 C67 119.6(3) . . ?
C69 C68 H68 120.2 . . ?
C67 C68 H68 120.2 . . ?
C68 C69 C70 118.6(3) . . ?
C68 C69 H69 120.7 . . ?
C70 C69 H69 120.7 . . ?
N44 C70 C69 122.7(4) . . ?
N44 C70 H70 118.7 . . ?
C69 C70 H70 118.7 . . ?
O34 Cl3 O31 109.41(18) . . ?
O34 Cl3 O32 110.05(17) . . ?
O31 Cl3 O32 109.65(17) . . ?
O34 Cl3 O33 109.05(18) . . ?
O31 Cl3 O33 109.54(18) . . ?
O32 Cl3 O33 109.12(16) . . ?
O41 Cl4 O44 109.44(19) . . ?
O41 Cl4 O43 109.5(2) . . ?
O44 Cl4 O43 109.5(2) . . ?
O41 Cl4 O42 110.7(2) . . ?
O44 Cl4 O42 108.8(2) . . ?
O43 Cl4 O42 108.9(2) . . ?
C1S O1S C2S 26.7(5) . . ?
C2S C1S O1S 109.5(11) . . ?
C2S C1S C1S 0.0(6) . 2_656 ?
O1S C1S C1S 109.5(11) . 2_656 ?
C1S C2S C1S 180.0(19) 2_656 . ?
C1S C2S O1S 43.8(8) 2_656 2_656 ?
C1S C2S O1S 136.2(8) . 2_656 ?
C1S C2S O1S 136.2(8) 2_656 . ?
C1S C2S O1S 43.8(8) . . ?
O1S C2S O1S 179.998(1) 2_656 . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_gl1609
_database_code_depnum_ccdc_archive 'CCDC 1024402'
_audit_update_record             
;
2014-09-15 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H58 Fe2 N4 O5, C H2 Cl2'
_chemical_formula_sum            'C45 H60 Cl2 Fe2 N4 O5'
_chemical_formula_weight         919.57

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                   17.5005(9)
_cell_length_b                   11.7785(6)
_cell_length_c                   21.6508(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6970(10)
_cell_angle_gamma                90.00
_cell_volume                     4422.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    2715
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      24.55

_exptl_crystal_description       rhomb
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9146
_exptl_absorpt_correction_T_max  0.9837
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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 AXS SMART 1K'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12835
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         26.99
_reflns_number_total             4802
_reflns_number_gt                3405
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2001)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0496P)²+8.6082P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4802
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.39921(2) 0.28615(4) 0.24889(2) 0.02199(13) Uani 1 1 d . . .
O1 O 0.36853(13) 0.18237(19) 0.30656(11) 0.0340(6) Uani 1 1 d . . .
O2 O 0.37323(13) 0.2592(2) 0.16250(11) 0.0405(6) Uani 1 1 d . . .
O3 O 0.5000 0.2608(3) 0.2500 0.0262(7) Uani 1 2 d S . .
N1 N 0.42667(15) 0.4491(2) 0.30069(12) 0.0273(6) Uani 1 1 d . . .
N2 N 0.28010(15) 0.3695(2) 0.24403(12) 0.0247(6) Uani 1 1 d . . .
C1 C 0.49791(18) 0.5048(3) 0.28492(15) 0.0303(7) Uani 1 1 d . . .
H1A H 0.5435 0.4646 0.3066 0.036 Uiso 1 1 calc R . .
H1B H 0.4996 0.5841 0.3002 0.036 Uiso 1 1 calc R . .
C2 C 0.36056(18) 0.5285(3) 0.28837(16) 0.0302(7) Uani 1 1 d . . .
H2A H 0.3615 0.5656 0.2475 0.036 Uiso 1 1 calc R . .
H2B H 0.3652 0.5884 0.3208 0.036 Uiso 1 1 calc R . .
C3 C 0.28457(19) 0.4660(3) 0.28842(16) 0.0316(8) Uani 1 1 d . . .
H3A H 0.2805 0.4375 0.3309 0.038 Uiso 1 1 calc R . .
H3B H 0.2411 0.5188 0.2763 0.038 Uiso 1 1 calc R . .
C4 C 0.4404(2) 0.4179(3) 0.36794(16) 0.0357(8) Uani 1 1 d . . .
H4A H 0.4555 0.4857 0.3929 0.054 Uiso 1 1 calc R . .
H4B H 0.4817 0.3613 0.3747 0.054 Uiso 1 1 calc R . .
H4C H 0.3930 0.3862 0.3805 0.054 Uiso 1 1 calc R . .
C5 C 0.22304(18) 0.2828(3) 0.25930(15) 0.0299(7) Uani 1 1 d . . .
H5A H 0.2212 0.2204 0.2285 0.036 Uiso 1 1 calc R . .
H5B H 0.1713 0.3182 0.2550 0.036 Uiso 1 1 calc R . .
C6 C 0.24050(18) 0.2334(3) 0.32371(16) 0.0296(7) Uani 1 1 d . . .
C7 C 0.31371(19) 0.1869(3) 0.34404(16) 0.0291(7) Uani 1 1 d . . .
C8 C 0.32911(19) 0.1419(3) 0.40452(15) 0.0310(8) Uani 1 1 d . . .
C9 C 0.2693(2) 0.1352(3) 0.44038(16) 0.0360(8) Uani 1 1 d . . .
H9A H 0.2793 0.1025 0.4808 0.043 Uiso 1 1 calc R . .
C10 C 0.1951(2) 0.1742(3) 0.41980(17) 0.0385(9) Uani 1 1 d . . .
C11 C 0.1826(2) 0.2244(3) 0.36197(17) 0.0353(8) Uani 1 1 d . . .
H11A H 0.1329 0.2540 0.3476 0.042 Uiso 1 1 calc R . .
C12 C 0.4096(2) 0.1018(3) 0.42774(18) 0.0401(9) Uani 1 1 d . . .
H12A H 0.4457 0.1655 0.4279 0.060 Uiso 1 1 calc R . .
H12B H 0.4243 0.0417 0.4003 0.060 Uiso 1 1 calc R . .
H12C H 0.4112 0.0719 0.4702 0.060 Uiso 1 1 calc R . .
C16 C 0.1299(2) 0.1588(4) 0.4590(2) 0.0542(11) Uani 1 1 d . . .
H16A H 0.0906 0.2172 0.4479 0.081 Uiso 1 1 calc R . .
H16B H 0.1503 0.1657 0.5032 0.081 Uiso 1 1 calc R . .
H16C H 0.1069 0.0835 0.4511 0.081 Uiso 1 1 calc R . .
C25 C 0.2544(2) 0.4113(3) 0.17909(16) 0.0331(8) Uani 1 1 d . . .
H25A H 0.2935 0.4646 0.1668 0.040 Uiso 1 1 calc R . .
H25B H 0.2053 0.4533 0.1784 0.040 Uiso 1 1 calc R . .
C26 C 0.24313(19) 0.3154(3) 0.13260(16) 0.0303(8) Uani 1 1 d . . .
C27 C 0.30421(19) 0.2413(3) 0.12800(15) 0.0326(8) Uani 1 1 d . . .
C28 C 0.2939(2) 0.1477(3) 0.08754(16) 0.0366(8) Uani 1 1 d . . .
C29 C 0.2234(2) 0.1346(3) 0.05077(17) 0.0385(9) Uani 1 1 d . . .
H29A H 0.2166 0.0722 0.0228 0.046 Uiso 1 1 calc R . .
C30 C 0.16184(19) 0.2090(3) 0.05305(16) 0.0358(8) Uani 1 1 d . . .
C31 C 0.17268(19) 0.2987(3) 0.09467(16) 0.0341(8) Uani 1 1 d . . .
H31A H 0.1314 0.3500 0.0976 0.041 Uiso 1 1 calc R . .
C32 C 0.3589(2) 0.0653(4) 0.0848(2) 0.0567(12) Uani 1 1 d . . .
H32A H 0.3666 0.0532 0.0413 0.085 Uiso 1 1 calc R . .
H32B H 0.3463 -0.0071 0.1033 0.085 Uiso 1 1 calc R . .
H32C H 0.4063 0.0962 0.1081 0.085 Uiso 1 1 calc R . .
C36 C 0.0867(2) 0.1916(4) 0.01062(19) 0.0496(11) Uani 1 1 d . . .
H36A H 0.0664 0.1158 0.0176 0.074 Uiso 1 1 calc R . .
H36B H 0.0957 0.1987 -0.0329 0.074 Uiso 1 1 calc R . .
H36C H 0.0493 0.2491 0.0197 0.074 Uiso 1 1 calc R . .
C100 C 0.5000 -0.0222(7) 0.2500 0.124(4) Uani 1 2 d S . .
H10A H 0.4555 0.0254 0.2402 0.149 Uiso 1 1 d R . .
Cl1 Cl 0.51202(8) -0.10933(15) 0.18523(8) 0.0907(5) 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 O3 1.7858(7) . ?
Fe1 O1 1.877(2) . ?
Fe1 O2 1.892(2) . ?
Fe1 N1 2.242(3) . ?
Fe1 N2 2.294(3) . ?
Fe1 Fe1 3.5215(9) 2_655 ?
O1 C7 1.338(4) . ?
O2 C27 1.349(4) . ?
O3 Fe1 1.7858(7) 2_655 ?
N1 C2 1.484(4) . ?
N1 C1 1.488(4) . ?
N1 C4 1.490(4) . ?
N2 C3 1.484(4) . ?
N2 C5 1.496(4) . ?
N2 C25 1.501(4) . ?
C1 C1 1.524(7) 2_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.520(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.504(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.396(5) . ?
C6 C7 1.409(4) . ?
C7 C8 1.405(5) . ?
C8 C9 1.387(5) . ?
C8 C12 1.507(5) . ?
C9 C10 1.393(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.375(5) . ?
C10 C16 1.520(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 C26 1.508(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.394(5) . ?
C26 C31 1.401(4) . ?
C27 C28 1.405(5) . ?
C28 C29 1.385(5) . ?
C28 C32 1.503(5) . ?
C29 C30 1.394(5) . ?
C29 H29A 0.9500 . ?
C30 C31 1.385(5) . ?
C30 C36 1.514(5) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C100 Cl1 1.773(5) . ?
C100 Cl1 1.773(5) 2_655 ?
C100 H10A 0.9602 . ?

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
O3 Fe1 O1 104.62(10) . . ?
O3 Fe1 O2 95.25(8) . . ?
O1 Fe1 O2 119.76(11) . . ?
O3 Fe1 N1 89.49(11) . . ?
O1 Fe1 N1 106.61(10) . . ?
O2 Fe1 N1 130.18(11) . . ?
O3 Fe1 N2 164.15(11) . . ?
O1 Fe1 N2 88.28(9) . . ?
O2 Fe1 N2 85.98(10) . . ?
N1 Fe1 N2 77.83(9) . . ?
O3 Fe1 Fe1 9.61(10) . 2_655 ?
O1 Fe1 Fe1 111.49(7) . 2_655 ?
O2 Fe1 Fe1 96.96(7) . 2_655 ?
N1 Fe1 Fe1 81.14(7) . 2_655 ?
N2 Fe1 Fe1 154.58(6) . 2_655 ?
C7 O1 Fe1 132.0(2) . . ?
C27 O2 Fe1 130.7(2) . . ?
Fe1 O3 Fe1 160.78(19) 2_655 . ?
C2 N1 C1 109.7(3) . . ?
C2 N1 C4 110.5(3) . . ?
C1 N1 C4 107.6(2) . . ?
C2 N1 Fe1 109.88(18) . . ?
C1 N1 Fe1 113.10(19) . . ?
C4 N1 Fe1 105.87(19) . . ?
C3 N2 C5 111.0(3) . . ?
C3 N2 C25 109.8(2) . . ?
C5 N2 C25 107.8(2) . . ?
C3 N2 Fe1 109.23(18) . . ?
C5 N2 Fe1 109.10(19) . . ?
C25 N2 Fe1 109.85(19) . . ?
N1 C1 C1 112.4(3) . 2_655 ?
N1 C1 H1A 109.1 . . ?
C1 C1 H1A 109.1 2_655 . ?
N1 C1 H1B 109.1 . . ?
C1 C1 H1B 109.1 2_655 . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C3 110.8(3) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C2 109.9(3) . . ?
N2 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 114.2(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C11 C6 C7 119.2(3) . . ?
C11 C6 C5 120.4(3) . . ?
C7 C6 C5 120.2(3) . . ?
O1 C7 C8 119.1(3) . . ?
O1 C7 C6 121.5(3) . . ?
C8 C7 C6 119.4(3) . . ?
C9 C8 C7 118.6(3) . . ?
C9 C8 C12 122.5(3) . . ?
C7 C8 C12 118.9(3) . . ?
C8 C9 C10 122.9(3) . . ?
C8 C9 H9A 118.5 . . ?
C10 C9 H9A 118.5 . . ?
C11 C10 C9 117.4(3) . . ?
C11 C10 C16 121.3(4) . . ?
C9 C10 C16 121.2(4) . . ?
C10 C11 C6 122.2(3) . . ?
C10 C11 H11A 118.9 . . ?
C6 C11 H11A 118.9 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C16 H16A 109.5 . . ?
C10 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C10 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C25 C26 112.1(3) . . ?
N2 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
N2 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C27 C26 C31 119.6(3) . . ?
C27 C26 C25 118.9(3) . . ?
C31 C26 C25 121.5(3) . . ?
O2 C27 C26 120.1(3) . . ?
O2 C27 C28 119.9(3) . . ?
C26 C27 C28 120.0(3) . . ?
C29 C28 C27 118.5(3) . . ?
C29 C28 C32 121.8(3) . . ?
C27 C28 C32 119.7(3) . . ?
C28 C29 C30 122.9(3) . . ?
C28 C29 H29A 118.6 . . ?
C30 C29 H29A 118.6 . . ?
C31 C30 C29 117.6(3) . . ?
C31 C30 C36 122.0(3) . . ?
C29 C30 C36 120.4(3) . . ?
C30 C31 C26 121.5(3) . . ?
C30 C31 H31A 119.3 . . ?
C26 C31 H31A 119.3 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Cl1 C100 Cl1 109.2(4) . 2_655 ?
Cl1 C100 H10A 110.0 . . ?
Cl1 C100 H10A 109.5 2_655 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_gl1679
_database_code_depnum_ccdc_archive 'CCDC 1024403'
_audit_update_record             
;
2014-10-14 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================




_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H58 Cl2 Fe2 N4 O4 , 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H62 Cl6 Fe2 N4 O4'
_chemical_formula_weight         1059.40

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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.5710(5)
_cell_length_b                   9.9468(6)
_cell_length_c                   28.6201(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3430(10)
_cell_angle_gamma                90.00
_cell_volume                     2429.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    5808
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.92

_exptl_crystal_description       plates
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_T_max  0.9439
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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 AXS SMART 1K'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13502
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5154
_reflns_number_gt                3973
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2001)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0779P)²+1.8582P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5154
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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 0.49695(5) 0.93647(4) 0.609161(14) 0.02434(14) Uani 1 1 d . . .
O1 O 0.4686(2) 0.7517(2) 0.60251(8) 0.0304(5) Uani 1 1 d . . .
O2 O 0.5227(2) 1.0122(2) 0.66776(7) 0.0305(5) Uani 1 1 d . . .
N2 N 0.2397(3) 0.9578(2) 0.61094(8) 0.0252(5) Uani 1 1 d . . .
N1 N 0.4409(3) 1.0919(2) 0.55436(8) 0.0268(5) Uani 1 1 d . . .
Cl1 Cl 0.75645(11) 0.94275(9) 0.59230(3) 0.0442(2) Uani 1 1 d . . .
C1 C 0.5144(4) 1.0710(3) 0.50960(10) 0.0282(7) Uani 1 1 d . . .
H1A H 0.6286 1.0870 0.5151 0.034 Uiso 1 1 calc R . .
H1B H 0.4707 1.1370 0.4860 0.034 Uiso 1 1 calc R . .
C2 C 0.2683(4) 1.1095(3) 0.54447(11) 0.0307(7) Uani 1 1 d . . .
H2A H 0.2273 1.0441 0.5203 0.037 Uiso 1 1 calc R . .
H2B H 0.2453 1.2012 0.5322 0.037 Uiso 1 1 calc R . .
C3 C 0.1880(4) 1.0879(3) 0.58929(11) 0.0294(7) Uani 1 1 d . . .
H3A H 0.2154 1.1622 0.6116 0.035 Uiso 1 1 calc R . .
H3B H 0.0729 1.0875 0.5819 0.035 Uiso 1 1 calc R . .
C4 C 0.5090(4) 1.2176(3) 0.57675(11) 0.0339(7) Uani 1 1 d . . .
H4A H 0.4888 1.2934 0.5552 0.051 Uiso 1 1 calc R . .
H4B H 0.6223 1.2064 0.5839 0.051 Uiso 1 1 calc R . .
H4C H 0.4604 1.2352 0.6058 0.051 Uiso 1 1 calc R . .
C5 C 0.1623(4) 0.8450(3) 0.58297(10) 0.0281(6) Uani 1 1 d . . .
H5A H 0.1989 0.8452 0.5512 0.034 Uiso 1 1 calc R . .
H5B H 0.0476 0.8598 0.5796 0.034 Uiso 1 1 calc R . .
C6 C 0.1966(4) 0.7103(3) 0.60533(10) 0.0268(6) Uani 1 1 d . . .
C7 C 0.3529(4) 0.6712(3) 0.61536(10) 0.0262(6) Uani 1 1 d . . .
C8 C 0.3888(4) 0.5485(3) 0.63824(10) 0.0270(6) Uani 1 1 d . . .
C9 C 0.2652(4) 0.4680(3) 0.64960(11) 0.0301(7) Uani 1 1 d . . .
H9A H 0.2884 0.3849 0.6650 0.036 Uiso 1 1 calc R . .
C10 C 0.1082(4) 0.5042(3) 0.63931(11) 0.0320(7) Uani 1 1 d . . .
C11 C 0.0775(4) 0.6272(3) 0.61749(11) 0.0292(6) Uani 1 1 d . . .
H11A H -0.0283 0.6551 0.6107 0.035 Uiso 1 1 calc R . .
C12 C 0.5565(4) 0.5091(3) 0.65121(12) 0.0336(7) Uani 1 1 d . . .
H12A H 0.5605 0.4347 0.6737 0.050 Uiso 1 1 calc R . .
H12B H 0.6143 0.5862 0.6654 0.050 Uiso 1 1 calc R . .
H12C H 0.6041 0.4809 0.6230 0.050 Uiso 1 1 calc R . .
C16 C -0.0228(4) 0.4147(4) 0.65322(14) 0.0446(9) Uani 1 1 d . . .
H16A H -0.1092 0.4152 0.6283 0.067 Uiso 1 1 calc R . .
H16B H -0.0602 0.4482 0.6824 0.067 Uiso 1 1 calc R . .
H16C H 0.0164 0.3227 0.6580 0.067 Uiso 1 1 calc R . .
C25 C 0.1943(4) 0.9513(3) 0.66013(10) 0.0282(6) Uani 1 1 d . . .
H25A H 0.2245 0.8622 0.6735 0.034 Uiso 1 1 calc R . .
H25B H 0.0789 0.9590 0.6593 0.034 Uiso 1 1 calc R . .
C26 C 0.2680(4) 1.0587(3) 0.69187(10) 0.0269(6) Uani 1 1 d . . .
C27 C 0.4301(4) 1.0823(3) 0.69509(10) 0.0263(6) Uani 1 1 d . . .
C28 C 0.4985(4) 1.1769(3) 0.72649(11) 0.0308(7) Uani 1 1 d . . .
C29 C 0.4021(4) 1.2486(3) 0.75434(11) 0.0330(7) Uani 1 1 d . . .
H29A H 0.4479 1.3140 0.7756 0.040 Uiso 1 1 calc R . .
C30 C 0.2411(4) 1.2273(3) 0.75197(11) 0.0339(7) Uani 1 1 d . . .
C31 C 0.1759(4) 1.1321(3) 0.72054(11) 0.0301(7) Uani 1 1 d . . .
H31A H 0.0661 1.1165 0.7185 0.036 Uiso 1 1 calc R . .
C32 C 0.6729(4) 1.1989(4) 0.73060(13) 0.0417(8) Uani 1 1 d . . .
H32A H 0.7107 1.1951 0.6993 0.063 Uiso 1 1 calc R . .
H32B H 0.7245 1.1287 0.7505 0.063 Uiso 1 1 calc R . .
H32C H 0.6971 1.2872 0.7446 0.063 Uiso 1 1 calc R . .
C36 C 0.1394(5) 1.3059(4) 0.78301(13) 0.0473(9) Uani 1 1 d . . .
H36A H 0.0456 1.2534 0.7879 0.071 Uiso 1 1 calc R . .
H36B H 0.1084 1.3913 0.7678 0.071 Uiso 1 1 calc R . .
H36C H 0.1986 1.3238 0.8133 0.071 Uiso 1 1 calc R . .
C101 C 0.7558(5) 0.4548(4) 0.49361(13) 0.0467(9) Uani 1 1 d . . .
H10A H 0.8089 0.5018 0.4690 0.056 Uiso 1 1 calc R . .
H10B H 0.6654 0.4049 0.4780 0.056 Uiso 1 1 calc R . .
Cl11 Cl 0.88757(13) 0.34013(11) 0.52352(4) 0.0568(3) Uani 1 1 d . . .
Cl12 Cl 0.68804(13) 0.57404(10) 0.53262(3) 0.0499(3) 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 O2 1.833(2) . ?
Fe1 O1 1.862(2) . ?
Fe1 N2 2.220(3) . ?
Fe1 N1 2.223(2) . ?
Fe1 Cl1 2.3202(10) . ?
Fe1 Fe1 6.3799(8) 3_676 ?
O1 C7 1.352(3) . ?
O2 C27 1.358(3) . ?
N2 C3 1.485(4) . ?
N2 C25 1.497(4) . ?
N2 C5 1.497(4) . ?
N1 C2 1.490(4) . ?
N1 C1 1.494(3) . ?
N1 C4 1.498(4) . ?
C1 C1 1.527(6) 3_676 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.526(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.502(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.383(4) . ?
C6 C7 1.399(4) . ?
C7 C8 1.405(4) . ?
C8 C9 1.390(4) . ?
C8 C12 1.503(4) . ?
C9 C10 1.397(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.388(4) . ?
C10 C16 1.515(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 C26 1.503(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.396(4) . ?
C26 C27 1.404(5) . ?
C27 C28 1.392(4) . ?
C28 C29 1.396(4) . ?
C28 C32 1.504(5) . ?
C29 C30 1.391(5) . ?
C29 H29A 0.9500 . ?
C30 C31 1.388(5) . ?
C30 C36 1.518(4) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C101 Cl12 1.764(4) . ?
C101 Cl11 1.769(4) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?

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
O2 Fe1 O1 120.18(10) . . ?
O2 Fe1 N2 88.58(9) . . ?
O1 Fe1 N2 88.63(9) . . ?
O2 Fe1 N1 111.08(9) . . ?
O1 Fe1 N1 126.65(10) . . ?
N2 Fe1 N1 78.46(9) . . ?
O2 Fe1 Cl1 98.22(7) . . ?
O1 Fe1 Cl1 97.11(7) . . ?
N2 Fe1 Cl1 167.27(7) . . ?
N1 Fe1 Cl1 89.03(7) . . ?
O2 Fe1 Fe1 143.46(7) . 3_676 ?
O1 Fe1 Fe1 96.22(7) . 3_676 ?
N2 Fe1 Fe1 95.87(6) . 3_676 ?
N1 Fe1 Fe1 36.11(6) . 3_676 ?
Cl1 Fe1 Fe1 72.28(2) . 3_676 ?
C7 O1 Fe1 130.45(17) . . ?
C27 O2 Fe1 135.3(2) . . ?
C3 N2 C25 109.7(2) . . ?
C3 N2 C5 109.3(2) . . ?
C25 N2 C5 109.2(2) . . ?
C3 N2 Fe1 109.38(18) . . ?
C25 N2 Fe1 111.31(19) . . ?
C5 N2 Fe1 107.94(17) . . ?
C2 N1 C1 110.1(2) . . ?
C2 N1 C4 108.9(2) . . ?
C1 N1 C4 107.7(2) . . ?
C2 N1 Fe1 111.20(18) . . ?
C1 N1 Fe1 115.32(17) . . ?
C4 N1 Fe1 103.21(18) . . ?
N1 C1 C1 111.8(3) . 3_676 ?
N1 C1 H1A 109.3 . . ?
C1 C1 H1A 109.3 3_676 . ?
N1 C1 H1B 109.3 . . ?
C1 C1 H1B 109.3 3_676 . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C3 109.9(2) . . ?
N1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C2 109.5(2) . . ?
N2 C3 H3A 109.8 . . ?
C2 C3 H3A 109.8 . . ?
N2 C3 H3B 109.8 . . ?
C2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 112.4(2) . . ?
N2 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?
C11 C6 C7 119.8(3) . . ?
C11 C6 C5 121.4(3) . . ?
C7 C6 C5 118.8(3) . . ?
O1 C7 C6 119.5(3) . . ?
O1 C7 C8 120.4(3) . . ?
C6 C7 C8 120.1(3) . . ?
C9 C8 C7 118.1(3) . . ?
C9 C8 C12 121.6(3) . . ?
C7 C8 C12 120.3(3) . . ?
C8 C9 C10 122.8(3) . . ?
C8 C9 H9A 118.6 . . ?
C10 C9 H9A 118.6 . . ?
C11 C10 C9 117.4(3) . . ?
C11 C10 C16 121.5(3) . . ?
C9 C10 C16 121.1(3) . . ?
C6 C11 C10 121.8(3) . . ?
C6 C11 H11A 119.1 . . ?
C10 C11 H11A 119.1 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C16 H16A 109.5 . . ?
C10 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C10 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C25 C26 114.0(2) . . ?
N2 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N2 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C31 C26 C27 118.9(3) . . ?
C31 C26 C25 119.9(3) . . ?
C27 C26 C25 121.1(3) . . ?
O2 C27 C28 119.1(3) . . ?
O2 C27 C26 120.3(3) . . ?
C28 C27 C26 120.7(3) . . ?
C27 C28 C29 118.6(3) . . ?
C27 C28 C32 120.3(3) . . ?
C29 C28 C32 121.2(3) . . ?
C30 C29 C28 122.1(3) . . ?
C30 C29 H29A 118.9 . . ?
C28 C29 H29A 118.9 . . ?
C31 C30 C29 118.2(3) . . ?
C31 C30 C36 120.8(3) . . ?
C29 C30 C36 120.9(3) . . ?
C30 C31 C26 121.5(3) . . ?
C30 C31 H31A 119.3 . . ?
C26 C31 H31A 119.3 . . ?
C28 C32 H32A 109.5 . . ?
C28 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C28 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Cl12 C101 Cl11 111.1(2) . . ?
Cl12 C101 H10A 109.4 . . ?
Cl11 C101 H10A 109.4 . . ?
Cl12 C101 H10B 109.4 . . ?
Cl11 C101 H10B 109.4 . . ?
H10A C101 H10B 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_gl1721
_database_code_depnum_ccdc_archive 'CCDC 1024404'
_audit_update_record             
;
2014-09-15 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
#=========================================================================





_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 Fe2 N4 O11 , 7(H2 O)'
_chemical_formula_sum            'C16 H44 Fe2 N4 O18'
_chemical_formula_weight         692.25

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'
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

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

_cell_length_a                   19.6588(12)
_cell_length_b                   7.7101(5)
_cell_length_c                   10.0166(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.5190(10)
_cell_angle_gamma                90.00
_cell_volume                     1455.56(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2597
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      26.98

_exptl_crystal_description       plates
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8294
_exptl_absorpt_correction_T_max  0.9381
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 AXS SMART 1K'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4085
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2624
_reflns_number_gt                2597
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker AXS, 2001)'
_computing_cell_refinement       'SAINT (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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. 

The compound which crystallizes in a non-centrosymmetric space group, 
was refined as racemic twin.
;

_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)+(0.0458P)²+4.2405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_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   0.50(3)
_refine_ls_number_reflns         2624
_refine_ls_number_parameters     183
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_restrained_S_all      1.246
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.90953(3) 0.74942(7) 0.40567(5) 0.01034(16) Uani 1 1 d . . .
O1 O 0.91095(16) 0.8648(4) 0.2240(3) 0.0171(7) Uani 1 1 d . . .
O2 O 0.85988(16) 0.6385(4) 0.5365(3) 0.0168(7) Uani 1 1 d . . .
O3 O 1.0000 0.7804(5) 0.5000 0.0106(10) Uani 1 2 d S . .
O81 O 0.87565(17) 0.9850(4) 0.4668(3) 0.0178(7) Uani 1 1 d . . .
N1 N 0.9284(2) 0.4839(5) 0.3471(4) 0.0139(8) Uani 1 1 d . . .
N2 N 0.80197(19) 0.6993(5) 0.2632(4) 0.0160(9) Uani 1 1 d . . .
O6 O 0.84548(19) 1.0339(5) 0.0526(4) 0.0240(8) Uani 1 1 d . . .
O26 O 0.75749(19) 0.5872(5) 0.5805(4) 0.0298(9) Uani 1 1 d . . .
C1 C 0.9606(2) 0.3611(6) 0.4644(5) 0.0161(9) Uani 1 1 d . . .
H1A H 0.9478 0.2422 0.4286 0.019 Uiso 1 1 calc R . .
H1B H 0.9365 0.3816 0.5374 0.019 Uiso 1 1 calc R . .
C2 C 0.8574(3) 0.4097(6) 0.2760(5) 0.0200(10) Uani 1 1 d . . .
H2A H 0.8345 0.3694 0.3467 0.024 Uiso 1 1 calc R . .
H2B H 0.8631 0.3082 0.2196 0.024 Uiso 1 1 calc R . .
C3 C 0.8104(3) 0.5428(7) 0.1827(5) 0.0210(11) Uani 1 1 d . . .
H3A H 0.8314 0.5766 0.1078 0.025 Uiso 1 1 calc R . .
H3B H 0.7632 0.4912 0.1388 0.025 Uiso 1 1 calc R . .
C4 C 0.9724(3) 0.4878(7) 0.2479(5) 0.0197(10) Uani 1 1 d . . .
H4A H 0.9808 0.3690 0.2217 0.030 Uiso 1 1 calc R . .
H4B H 1.0180 0.5439 0.2925 0.030 Uiso 1 1 calc R . .
H4C H 0.9474 0.5531 0.1645 0.030 Uiso 1 1 calc R . .
C5 C 0.7845(2) 0.8499(6) 0.1700(4) 0.0153(10) Uani 1 1 d . . .
H5A H 0.7617 0.9405 0.2127 0.018 Uiso 1 1 calc R . .
H5B H 0.7506 0.8150 0.0806 0.018 Uiso 1 1 calc R . .
C6 C 0.8514(3) 0.9221(7) 0.1437(5) 0.0183(10) Uani 1 1 d . . .
C25 C 0.7531(2) 0.6685(7) 0.3498(5) 0.0205(10) Uani 1 1 d . . .
H25A H 0.7211 0.5707 0.3100 0.025 Uiso 1 1 calc R . .
H25B H 0.7234 0.7729 0.3470 0.025 Uiso 1 1 calc R . .
C26 C 0.7925(2) 0.6277(6) 0.5001(5) 0.0164(9) Uani 1 1 d . . .
O101 O 1.0000 0.7815(9) 1.0000 0.057(2) Uani 1 2 d S . .
O102 O 0.92742(19) 1.2289(6) 0.9296(3) 0.0277(9) Uani 1 1 d . . .
O103 O 0.9586(2) 1.0525(6) 0.7140(4) 0.0369(10) Uani 1 1 d . . .
O104 O 0.8796(2) 0.5729(6) 0.8723(4) 0.0407(11) 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 O3 1.7769(8) . ?
Fe1 O2 2.032(3) . ?
Fe1 O1 2.033(3) . ?
Fe1 O81 2.085(3) . ?
Fe1 N1 2.190(4) . ?
Fe1 N2 2.223(4) . ?
Fe1 Fe1 36.343(2) 2_556 ?
O1 C6 1.295(6) . ?
O2 C26 1.273(6) . ?
O3 Fe1 1.7770(8) 2_756 ?
N1 C2 1.490(6) . ?
N1 C4 1.492(5) . ?
N1 C1 1.501(6) . ?
N2 C5 1.468(6) . ?
N2 C25 1.485(6) . ?
N2 C3 1.486(6) . ?
O6 C6 1.236(6) . ?
O26 C26 1.239(6) . ?
C1 C1 1.510(9) 2_756 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.513(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.520(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C25 C26 1.517(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?

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
O3 Fe1 O2 107.77(10) . . ?
O3 Fe1 O1 98.68(11) . . ?
O2 Fe1 O1 153.24(13) . . ?
O3 Fe1 O81 94.70(15) . . ?
O2 Fe1 O81 85.72(14) . . ?
O1 Fe1 O81 88.19(13) . . ?
O3 Fe1 N1 92.72(15) . . ?
O2 Fe1 N1 85.89(14) . . ?
O1 Fe1 N1 97.05(14) . . ?
O81 Fe1 N1 170.17(13) . . ?
O3 Fe1 N2 172.03(11) . . ?
O2 Fe1 N2 78.29(13) . . ?
O1 Fe1 N2 75.77(13) . . ?
O81 Fe1 N2 90.86(13) . . ?
N1 Fe1 N2 82.43(14) . . ?
O3 Fe1 Fe1 145.42(3) . 2_556 ?
O2 Fe1 Fe1 46.08(9) . 2_556 ?
O1 Fe1 Fe1 108.10(9) . 2_556 ?
O81 Fe1 Fe1 65.40(9) . 2_556 ?
N1 Fe1 Fe1 104.96(10) . 2_556 ?
N2 Fe1 Fe1 42.51(9) . 2_556 ?
C6 O1 Fe1 117.7(3) . . ?
C26 O2 Fe1 119.6(3) . . ?
Fe1 O3 Fe1 164.6(3) . 2_756 ?
C2 N1 C4 109.3(4) . . ?
C2 N1 C1 105.1(4) . . ?
C4 N1 C1 109.8(4) . . ?
C2 N1 Fe1 106.2(3) . . ?
C4 N1 Fe1 109.5(3) . . ?
C1 N1 Fe1 116.5(3) . . ?
C5 N2 C25 115.1(4) . . ?
C5 N2 C3 109.8(4) . . ?
C25 N2 C3 112.2(4) . . ?
C5 N2 Fe1 106.2(3) . . ?
C25 N2 Fe1 108.0(3) . . ?
C3 N2 Fe1 104.9(3) . . ?
N1 C1 C1 121.1(4) . 2_756 ?
N1 C1 H1A 107.0 . . ?
C1 C1 H1A 107.0 2_756 . ?
N1 C1 H1B 107.0 . . ?
C1 C1 H1B 107.0 2_756 . ?
H1A C1 H1B 106.8 . . ?
N1 C2 C3 111.1(4) . . ?
N1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C2 111.0(4) . . ?
N2 C3 H3A 109.4 . . ?
C2 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 110.0(4) . . ?
N2 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
N2 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O6 C6 O1 125.2(4) . . ?
O6 C6 C5 118.6(4) . . ?
O1 C6 C5 116.2(4) . . ?
N2 C25 C26 112.3(4) . . ?
N2 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
N2 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
O26 C26 O2 123.7(4) . . ?
O26 C26 C25 118.4(4) . . ?
O2 C26 C25 117.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.097

