# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1-296K
_database_code_depnum_ccdc_archive 'CCDC 1400827'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 Fe N10 O2, 2(Cl O4)'
_chemical_formula_sum            'C38 H30 Cl2 Fe N10 O10'
_chemical_formula_weight         913.47

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'
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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.801(6)
_cell_length_b                   13.315(6)
_cell_length_c                   17.303(8)
_cell_angle_alpha                110.308(11)
_cell_angle_beta                 91.184(12)
_cell_angle_gamma                104.924(12)
_cell_volume                     2445.6(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    902
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      19.20

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.476
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13569
_diffrn_reflns_av_unetI/netI     0.1678
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.264
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             8529
_reflns_number_gt                3669
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
There are partial occupancy water and solvent molecules in 
the structure,and ClO4 is disorder, so some restraints have 
been used to treat these problems.This crystal data is treated 
with squeeze.
We made several attempts to obtain better quality data for 
this structure however, due to disorder, poor crystal 
quality etc, especially collect data at room temperrature,
 the R1 and wR2 value are high. We are confidant 
the structural characterization is valid.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8529
_refine_ls_number_parameters     631
_refine_ls_number_restraints     414
_refine_ls_R_factor_all          0.2083
_refine_ls_R_factor_gt           0.1351
_refine_ls_wR_factor_ref         0.4000
_refine_ls_wR_factor_gt          0.3517
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.30918(11) 0.19946(10) 0.23582(7) 0.0439(5) Uani 1 1 d . . . . .
C1 C 0.3258(11) 0.2824(11) 0.6163(7) 0.082(4) Uani 1 1 d . . . . .
H1 H 0.3015 0.2197 0.6307 0.098 Uiso 1 1 calc R U . . .
C2 C 0.3342(14) 0.3850(12) 0.6725(7) 0.101(5) Uani 1 1 d . . . . .
H2 H 0.3174 0.3947 0.7264 0.121 Uiso 1 1 calc R U . . .
C3 C 0.3671(11) 0.4718(11) 0.6483(7) 0.081(4) Uani 1 1 d . . . . .
H3 H 0.3732 0.5430 0.6861 0.098 Uiso 1 1 calc R U . . .
C4 C 0.3934(10) 0.4583(10) 0.5657(7) 0.072(3) Uani 1 1 d . . . . .
H4 H 0.4144 0.5197 0.5496 0.087 Uiso 1 1 calc R U . . .
C5 C 0.3547(8) 0.2715(8) 0.5352(5) 0.048(2) Uani 1 1 d . . . . .
C6 C 0.3562(8) 0.1594(7) 0.4732(5) 0.042(2) Uani 1 1 d . . . . .
H6 H 0.2817 0.1047 0.4718 0.050 Uiso 1 1 calc R U . . .
C7 C 0.5609(9) 0.1656(7) 0.4749(5) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.6665(10) 0.1628(8) 0.5199(6) 0.060(3) Uani 1 1 d . . . . .
H8 H 0.6621 0.1338 0.5618 0.072 Uiso 1 1 calc R U . . .
C9 C 0.7725(11) 0.2062(10) 0.4954(8) 0.082(4) Uani 1 1 d . . . . .
H9 H 0.8399 0.1978 0.5183 0.099 Uiso 1 1 calc R U . . .
C10 C 0.7871(10) 0.2581(10) 0.4427(7) 0.067(3) Uani 1 1 d . . . . .
H10 H 0.8626 0.2949 0.4360 0.081 Uiso 1 1 calc R U . . .
C11 C 0.6866(9) 0.2575(8) 0.3963(6) 0.054(2) Uani 1 1 d . . . . .
H11 H 0.6930 0.2861 0.3540 0.065 Uiso 1 1 calc R U . . .
C12 C 0.5752(8) 0.2105(7) 0.4181(6) 0.049(2) Uani 1 1 d . . . . .
C13 C 0.4720(7) 0.2036(6) 0.3653(5) 0.0367(19) Uani 1 1 d . . . . .
C14 C 0.1658(9) 0.1376(8) 0.3575(5) 0.051(2) Uani 1 1 d . . . . .
H14 H 0.1447 0.1224 0.4046 0.061 Uiso 1 1 calc R U . . .
C15 C 0.0756(8) 0.1381(8) 0.2965(7) 0.058(3) Uani 1 1 d . . . . .
C16 C -0.0427(9) 0.1128(9) 0.3047(7) 0.072(3) Uani 1 1 d . . . . .
H16 H -0.0699 0.0932 0.3490 0.086 Uiso 1 1 calc R U . . .
C17 C -0.1194(10) 0.1170(10) 0.2472(7) 0.074(3) Uani 1 1 d . . . . .
H17 H -0.2001 0.0981 0.2509 0.089 Uiso 1 1 calc R U . . .
C18 C -0.0783(9) 0.1488(9) 0.1844(7) 0.071(3) Uani 1 1 d . . . . .
H18 H -0.1291 0.1558 0.1460 0.085 Uiso 1 1 calc R U . . .
C19 C 0.0421(9) 0.1705(9) 0.1791(6) 0.065(3) Uani 1 1 d . . . . .
H19 H 0.0710 0.1868 0.1339 0.078 Uiso 1 1 calc R U . . .
C20 C 0.2164(10) 0.1839(10) -0.1253(6) 0.0717(18) Uani 1 1 d . U . . .
H20 H 0.2811 0.2141 -0.1482 0.086 Uiso 1 1 calc R U . . .
C21 C 0.1035(10) 0.1693(10) -0.1552(7) 0.0757(19) Uani 1 1 d . U . . .
H21 H 0.0895 0.1884 -0.2007 0.091 Uiso 1 1 calc R U . . .
C22 C 0.0083(11) 0.1260(10) -0.1185(7) 0.0767(19) Uani 1 1 d . U . . .
H22 H -0.0694 0.1145 -0.1388 0.092 Uiso 1 1 calc R U . . .
C23 C 0.0334(10) 0.1032(10) -0.0564(7) 0.0721(18) Uani 1 1 d . U . . .
H23 H -0.0307 0.0764 -0.0315 0.087 Uiso 1 1 calc R U . . .
C24 C 0.2290(9) 0.1509(9) -0.0586(6) 0.0635(17) Uani 1 1 d . U . . .
C25 C 0.3545(7) 0.1586(7) -0.0236(5) 0.040(2) Uani 1 1 d . . . . .
H25 H 0.4078 0.2308 -0.0192 0.048 Uiso 1 1 calc R U . . .
C26 C 0.3667(7) -0.0296(7) -0.0707(5) 0.040(2) Uani 1 1 d . . . . .
C27 C 0.3838(9) -0.1247(9) -0.1320(6) 0.061(3) Uani 1 1 d . . . . .
H27 H 0.4185 -0.1160 -0.1779 0.073 Uiso 1 1 calc R U . . .
C28 C 0.3537(9) -0.2257(10) -0.1285(6) 0.068(3) Uani 1 1 d . . . . .
H28 H 0.3623 -0.2862 -0.1729 0.082 Uiso 1 1 calc R U . . .
C29 C 0.3072(10) -0.2420(10) -0.0552(7) 0.081(4) Uani 1 1 d . . . . .
H29 H 0.2869 -0.3121 -0.0511 0.097 Uiso 1 1 calc R U . . .
C30 C 0.2945(9) -0.1515(9) 0.0067(6) 0.065(3) Uani 1 1 d . . . . .
H30 H 0.2661 -0.1589 0.0547 0.078 Uiso 1 1 calc R U . . .
C31 C 0.3238(7) -0.0462(7) -0.0007(5) 0.0366(19) Uani 1 1 d . . . . .
C32 C 0.3225(7) 0.0506(7) 0.0713(5) 0.040(2) Uani 1 1 d . . . . .
C33 C 0.3592(8) 0.3379(7) 0.1301(5) 0.049(2) Uani 1 1 d . . . . .
H33 H 0.3730 0.3578 0.0840 0.059 Uiso 1 1 calc R U . . .
C34 C 0.3500(9) 0.4148(7) 0.2082(6) 0.051(2) Uani 1 1 d . . . . .
C35 C 0.3651(12) 0.5313(10) 0.2278(8) 0.085(4) Uani 1 1 d . . . . .
H35 H 0.3839 0.5598 0.1862 0.102 Uiso 1 1 calc R U . . .
C36 C 0.3545(12) 0.5986(10) 0.2990(7) 0.082(4) Uani 1 1 d . . . . .
H36 H 0.3631 0.6735 0.3084 0.098 Uiso 1 1 calc R U . . .
C37 C 0.3290(10) 0.5558(9) 0.3634(7) 0.076(3) Uani 1 1 d . . . . .
H37 H 0.3212 0.6021 0.4162 0.091 Uiso 1 1 calc R U . . .
C38 C 0.3164(9) 0.4447(8) 0.3457(6) 0.062(3) Uani 1 1 d . . . . .
H38 H 0.3007 0.4165 0.3878 0.074 Uiso 1 1 calc R U . . .
N1 N 0.4521(7) 0.1214(6) 0.4950(5) 0.054(2) Uani 1 1 d . . . . .
H1A H 0.4417 0.0738 0.5193 0.064 Uiso 1 1 calc R U . . .
N2 N 0.3875(7) 0.3580(6) 0.5129(5) 0.059(2) Uani 1 1 d . . . . .
N3 N 0.3651(6) 0.1614(6) 0.3906(4) 0.0451(18) Uani 1 1 d . . . . .
N4 N 0.2711(6) 0.1583(5) 0.3431(4) 0.0388(17) Uani 1 1 d . . . . .
N5 N 0.1189(6) 0.1689(6) 0.2376(5) 0.059(2) Uani 1 1 d . . . . .
N6 N 0.1407(8) 0.1123(7) -0.0212(5) 0.0640(16) Uani 1 1 d . U . . .
N7 N 0.3990(7) 0.0725(6) -0.0764(4) 0.051(2) Uani 1 1 d . . . . .
H7 H 0.4460 0.0852 -0.1114 0.061 Uiso 1 1 calc R U . . .
N8 N 0.3534(6) 0.1526(5) 0.0619(4) 0.0419(17) Uani 1 1 d . . . . .
N9 N 0.3471(6) 0.2391(5) 0.1278(4) 0.0359(16) Uani 1 1 d . . . . .
N10 N 0.3256(7) 0.3755(6) 0.2709(4) 0.052(2) Uani 1 1 d . . . . .
O1 O 0.4738(5) 0.2296(5) 0.3018(3) 0.0434(15) Uani 1 1 d . . . . .
O2 O 0.3005(5) 0.0482(5) 0.1399(3) 0.0487(16) Uani 1 1 d . . . . .
Cl2 Cl 0.5462(7) -0.1020(7) 0.2804(5) 0.1021(19) Uani 0.5573 1 d D U P A 1
O9 O 0.4696(13) -0.1152(12) 0.3389(8) 0.105(3) Uani 0.5573 1 d D U P A 1
O8 O 0.5364(15) -0.2089(10) 0.2223(9) 0.110(3) Uani 0.5573 1 d D U P A 1
O0AA O 0.5145(14) -0.0363(12) 0.2412(9) 0.113(2) Uani 0.5573 1 d D U P A 1
O7 O 0.6618(12) -0.0602(12) 0.3201(9) 0.118(3) Uani 0.5573 1 d D U P A 1
Cl1A Cl 0.5026(9) -0.1001(8) 0.2716(6) 0.102(2) Uani 0.4427 1 d D U P B 2
O1AA O 0.5536(17) -0.1248(15) 0.3363(10) 0.111(3) Uani 0.4427 1 d D U P B 2
O11 O 0.4891(18) -0.1883(14) 0.1925(10) 0.106(3) Uani 0.4427 1 d D U P B 2
O2AA O 0.5805(16) 0.0003(13) 0.2657(11) 0.113(3) Uani 0.4427 1 d D U P B 2
O10 O 0.3893(15) -0.0841(15) 0.2917(11) 0.113(3) Uani 0.4427 1 d D U P B 2
Cl1 Cl 0.5793(8) 0.5019(6) 0.0322(5) 0.118(2) Uani 0.5 1 d D U P C -1
O3 O 0.6801(16) 0.5225(15) -0.0044(12) 0.132(4) Uani 0.5 1 d D U P C -1
O4 O 0.6092(17) 0.4980(14) 0.1080(10) 0.121(4) Uani 0.5 1 d D U P C -1
O5 O 0.526(2) 0.5839(14) 0.0478(13) 0.129(4) Uani 0.5 1 d D U P C -1
O6 O 0.503(2) 0.4016(14) -0.0140(11) 0.132(4) Uani 0.5 1 d D U P C -1
Cl3 Cl -0.0117(6) -0.0561(7) 0.4568(5) 0.126(3) Uani 0.5 1 d DG U P D -1
O12 O 0.0968(9) 0.0222(11) 0.5045(9) 0.142(5) Uani 0.5 1 d DG U P D -1
O13 O -0.0429(12) -0.1498(10) 0.4836(10) 0.126(4) Uani 0.5 1 d DG U P D -1
O14 O -0.1048(11) -0.0021(12) 0.4690(10) 0.142(5) Uani 0.5 1 d DG U P D -1
O15 O 0.0039(14) -0.0948(13) 0.3699(5) 0.146(4) Uani 0.5 1 d DG U P D -1


_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 2.094(6) . ?
Fe1 O1 2.104(6) . ?
Fe1 N4 2.137(6) . ?
Fe1 N9 2.137(6) . ?
Fe1 N10 2.162(7) . ?
Fe1 N5 2.179(8) . ?
C1 C2 1.351(16) . ?
C1 C5 1.417(13) . ?
C1 H1 0.9300 . ?
C2 C3 1.331(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.428(15) . ?
C3 H3 0.9300 . ?
C4 N2 1.314(13) . ?
C4 H4 0.9300 . ?
C5 N2 1.309(11) . ?
C5 C6 1.511(12) . ?
C6 N1 1.445(11) . ?
C6 N3 1.445(10) . ?
C6 H6 0.9800 . ?
C7 C12 1.309(12) . ?
C7 N1 1.374(12) . ?
C7 C8 1.472(14) . ?
C8 C9 1.377(16) . ?
C8 H8 0.9300 . ?
C9 C10 1.312(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.416(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.423(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.472(12) . ?
C13 O1 1.260(9) . ?
C13 N3 1.387(10) . ?
C14 N4 1.251(11) . ?
C14 C15 1.486(14) . ?
C14 H14 0.9300 . ?
C15 N5 1.293(12) . ?
C15 C16 1.372(14) . ?
C16 C17 1.357(15) . ?
C16 H16 0.9300 . ?
C17 C18 1.353(15) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(14) . ?
C18 H18 0.9300 . ?
C19 N5 1.354(12) . ?
C19 H19 0.9300 . ?
C20 C21 1.360(15) . ?
C20 C24 1.388(13) . ?
C20 H20 0.9300 . ?
C21 C22 1.395(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.263(14) . ?
C22 H22 0.9300 . ?
C23 N6 1.351(13) . ?
C23 H23 0.9300 . ?
C24 N6 1.324(12) . ?
C24 C25 1.553(13) . ?
C25 N7 1.425(11) . ?
C25 N8 1.509(10) . ?
C25 H25 0.9800 . ?
C26 N7 1.353(11) . ?
C26 C31 1.389(11) . ?
C26 C27 1.405(13) . ?
C27 C28 1.322(14) . ?
C27 H27 0.9300 . ?
C28 C29 1.455(15) . ?
C28 H28 0.9300 . ?
C29 C30 1.350(14) . ?
C29 H29 0.9300 . ?
C30 C31 1.406(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.453(12) . ?
C32 O2 1.230(9) . ?
C32 N8 1.380(10) . ?
C33 N9 1.273(10) . ?
C33 C34 1.411(12) . ?
C33 H33 0.9300 . ?
C34 N10 1.364(11) . ?
C34 C35 1.428(14) . ?
C35 C36 1.279(15) . ?
C35 H35 0.9300 . ?
C36 C37 1.423(16) . ?
C36 H36 0.9300 . ?
C37 C38 1.368(14) . ?
C37 H37 0.9300 . ?
C38 N10 1.329(12) . ?
C38 H38 0.9300 . ?
N1 H1A 0.8600 . ?
N3 N4 1.350(9) . ?
N7 H7 0.8600 . ?
N8 N9 1.329(9) . ?
Cl2 O0AA 1.391(11) . ?
Cl2 O7 1.396(11) . ?
Cl2 O9 1.398(11) . ?
Cl2 O8 1.401(10) . ?
Cl1A O1AA 1.433(13) . ?
Cl1A O11 1.433(13) . ?
Cl1A O10 1.439(13) . ?
Cl1A O2AA 1.451(13) . ?
Cl1 O5 1.349(15) . ?
Cl1 O6 1.359(15) . ?
Cl1 O3 1.369(14) . ?
Cl1 O4 1.373(14) . ?
Cl3 O13 1.4416 . ?
Cl3 O14 1.4422 . ?
Cl3 O12 1.4425 . ?
Cl3 O15 1.4433 . ?

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 100.3(2) . . ?
O2 Fe1 N4 105.7(2) . . ?
O1 Fe1 N4 74.0(2) . . ?
O2 Fe1 N9 73.8(2) . . ?
O1 Fe1 N9 106.1(2) . . ?
N4 Fe1 N9 179.5(3) . . ?
O2 Fe1 N10 147.1(3) . . ?
O1 Fe1 N10 92.8(3) . . ?
N4 Fe1 N10 106.9(3) . . ?
N9 Fe1 N10 73.6(3) . . ?
O2 Fe1 N5 95.8(3) . . ?
O1 Fe1 N5 147.0(3) . . ?
N4 Fe1 N5 74.0(3) . . ?
N9 Fe1 N5 106.0(3) . . ?
N10 Fe1 N5 88.9(3) . . ?
C2 C1 C5 119.2(11) . . ?
C2 C1 H1 120.4 . . ?
C5 C1 H1 120.4 . . ?
C3 C2 C1 118.0(11) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 121.7(11) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
N2 C4 C3 119.1(11) . . ?
N2 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N2 C5 C1 121.8(9) . . ?
N2 C5 C6 117.6(7) . . ?
C1 C5 C6 120.5(9) . . ?
N1 C6 N3 108.1(7) . . ?
N1 C6 C5 112.6(7) . . ?
N3 C6 C5 111.7(7) . . ?
N1 C6 H6 108.1 . . ?
N3 C6 H6 108.1 . . ?
C5 C6 H6 108.1 . . ?
C12 C7 N1 123.3(9) . . ?
C12 C7 C8 118.5(9) . . ?
N1 C7 C8 118.2(9) . . ?
C9 C8 C7 115.2(10) . . ?
C9 C8 H8 122.4 . . ?
C7 C8 H8 122.4 . . ?
C10 C9 C8 126.0(11) . . ?
C10 C9 H9 117.0 . . ?
C8 C9 H9 117.0 . . ?
C9 C10 C11 119.1(11) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 115.9(9) . . ?
C10 C11 H11 122.0 . . ?
C12 C11 H11 122.0 . . ?
C7 C12 C11 124.6(9) . . ?
C7 C12 C13 120.1(9) . . ?
C11 C12 C13 115.0(8) . . ?
O1 C13 N3 120.3(7) . . ?
O1 C13 C12 126.5(8) . . ?
N3 C13 C12 113.2(7) . . ?
N4 C14 C15 117.6(8) . . ?
N4 C14 H14 121.2 . . ?
C15 C14 H14 121.2 . . ?
N5 C15 C16 123.3(11) . . ?
N5 C15 C14 114.2(8) . . ?
C16 C15 C14 122.4(10) . . ?
C17 C16 C15 118.9(11) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C18 C17 C16 119.9(11) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 117.8(10) . . ?
C17 C18 H18 121.1 . . ?
C19 C18 H18 121.1 . . ?
N5 C19 C18 122.2(9) . . ?
N5 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
C21 C20 C24 115.8(10) . . ?
C21 C20 H20 122.1 . . ?
C24 C20 H20 122.1 . . ?
C20 C21 C22 120.8(10) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 116.5(12) . . ?
C23 C22 H22 121.8 . . ?
C21 C22 H22 121.8 . . ?
C22 C23 N6 128.8(12) . . ?
C22 C23 H23 115.6 . . ?
N6 C23 H23 115.6 . . ?
N6 C24 C20 124.7(10) . . ?
N6 C24 C25 116.0(8) . . ?
C20 C24 C25 119.2(9) . . ?
N7 C25 N8 109.3(7) . . ?
N7 C25 C24 111.9(7) . . ?
N8 C25 C24 110.5(7) . . ?
N7 C25 H25 108.3 . . ?
N8 C25 H25 108.3 . . ?
C24 C25 H25 108.3 . . ?
N7 C26 C31 122.3(7) . . ?
N7 C26 C27 122.5(8) . . ?
C31 C26 C27 115.0(9) . . ?
C28 C27 C26 124.2(10) . . ?
C28 C27 H27 117.9 . . ?
C26 C27 H27 117.9 . . ?
C27 C28 C29 119.9(10) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 117.5(11) . . ?
C30 C29 H29 121.3 . . ?
C28 C29 H29 121.3 . . ?
C29 C30 C31 120.8(10) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 H30 119.6 . . ?
C26 C31 C30 122.4(8) . . ?
C26 C31 C32 118.6(8) . . ?
C30 C31 C32 118.6(8) . . ?
O2 C32 N8 118.4(8) . . ?
O2 C32 C31 124.7(8) . . ?
N8 C32 C31 116.8(7) . . ?
N9 C33 C34 114.7(8) . . ?
N9 C33 H33 122.6 . . ?
C34 C33 H33 122.6 . . ?
N10 C34 C33 117.6(8) . . ?
N10 C34 C35 116.9(9) . . ?
C33 C34 C35 125.5(9) . . ?
C36 C35 C34 124.0(12) . . ?
C36 C35 H35 118.0 . . ?
C34 C35 H35 118.0 . . ?
C35 C36 C37 118.1(12) . . ?
C35 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
C38 C37 C36 118.3(10) . . ?
C38 C37 H37 120.8 . . ?
C36 C37 H37 120.8 . . ?
N10 C38 C37 122.7(10) . . ?
N10 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
C7 N1 C6 116.3(7) . . ?
C7 N1 H1A 121.8 . . ?
C6 N1 H1A 121.8 . . ?
C5 N2 C4 120.2(9) . . ?
N4 N3 C13 112.8(7) . . ?
N4 N3 C6 121.5(7) . . ?
C13 N3 C6 122.3(7) . . ?
C14 N4 N3 126.5(7) . . ?
C14 N4 Fe1 117.6(6) . . ?
N3 N4 Fe1 115.8(5) . . ?
C15 N5 C19 117.7(8) . . ?
C15 N5 Fe1 116.3(7) . . ?
C19 N5 Fe1 125.8(7) . . ?
C24 N6 C23 113.4(9) . . ?
C26 N7 C25 119.2(7) . . ?
C26 N7 H7 120.4 . . ?
C25 N7 H7 120.4 . . ?
N9 N8 C32 115.4(7) . . ?
N9 N8 C25 121.3(6) . . ?
C32 N8 C25 120.4(7) . . ?
C33 N9 N8 125.9(7) . . ?
C33 N9 Fe1 120.1(6) . . ?
N8 N9 Fe1 114.0(5) . . ?
C38 N10 C34 119.9(8) . . ?
C38 N10 Fe1 126.1(7) . . ?
C34 N10 Fe1 114.0(6) . . ?
C13 O1 Fe1 116.7(5) . . ?
C32 O2 Fe1 118.0(5) . . ?
O0AA Cl2 O7 114.2(8) . . ?
O0AA Cl2 O9 110.1(8) . . ?
O7 Cl2 O9 108.3(8) . . ?
O0AA Cl2 O8 110.1(8) . . ?
O7 Cl2 O8 106.7(8) . . ?
O9 Cl2 O8 107.1(8) . . ?
O1AA Cl1A O11 111.5(9) . . ?
O1AA Cl1A O10 108.2(8) . . ?
O11 Cl1A O10 109.9(9) . . ?
O1AA Cl1A O2AA 109.1(9) . . ?
O11 Cl1A O2AA 107.5(8) . . ?
O10 Cl1A O2AA 110.6(9) . . ?
O5 Cl1 O6 110.5(14) . . ?
O5 Cl1 O3 112.7(12) . . ?
O6 Cl1 O3 111.2(12) . . ?
O5 Cl1 O4 106.0(13) . . ?
O6 Cl1 O4 107.6(11) . . ?
O3 Cl1 O4 108.6(13) . . ?
O13 Cl3 O14 109.5 . . ?
O13 Cl3 O12 109.5 . . ?
O14 Cl3 O12 109.5 . . ?
O13 Cl3 O15 109.5 . . ?
O14 Cl3 O15 109.4 . . ?
O12 Cl3 O15 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 1(2) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 N2 -1.6(19) . . . . ?
C2 C1 C5 N2 -1.1(18) . . . . ?
C2 C1 C5 C6 174.9(11) . . . . ?
N2 C5 C6 N1 107.0(9) . . . . ?
C1 C5 C6 N1 -69.2(11) . . . . ?
N2 C5 C6 N3 -14.9(11) . . . . ?
C1 C5 C6 N3 168.9(9) . . . . ?
C12 C7 C8 C9 -1.7(13) . . . . ?
N1 C7 C8 C9 178.6(9) . . . . ?
C7 C8 C9 C10 7.1(17) . . . . ?
C8 C9 C10 C11 -10.0(18) . . . . ?
C9 C10 C11 C12 7.2(15) . . . . ?
N1 C7 C12 C11 179.6(8) . . . . ?
C8 C7 C12 C11 0.0(13) . . . . ?
N1 C7 C12 C13 -7.3(13) . . . . ?
C8 C7 C12 C13 173.1(8) . . . . ?
C10 C11 C12 C7 -2.5(14) . . . . ?
C10 C11 C12 C13 -175.9(8) . . . . ?
C7 C12 C13 O1 -169.9(8) . . . . ?
C11 C12 C13 O1 3.8(12) . . . . ?
C7 C12 C13 N3 8.7(11) . . . . ?
C11 C12 C13 N3 -177.6(7) . . . . ?
N4 C14 C15 N5 -5.0(13) . . . . ?
N4 C14 C15 C16 177.8(9) . . . . ?
N5 C15 C16 C17 1.9(17) . . . . ?
C14 C15 C16 C17 178.8(10) . . . . ?
C15 C16 C17 C18 -1.8(18) . . . . ?
C16 C17 C18 C19 3.3(17) . . . . ?
C17 C18 C19 N5 -5.0(17) . . . . ?
C24 C20 C21 C22 1.4(18) . . . . ?
C20 C21 C22 C23 0.9(19) . . . . ?
C21 C22 C23 N6 -2(2) . . . . ?
C21 C20 C24 N6 -3.3(18) . . . . ?
C21 C20 C24 C25 176.7(10) . . . . ?
N6 C24 C25 N7 105.1(10) . . . . ?
C20 C24 C25 N7 -74.8(12) . . . . ?
N6 C24 C25 N8 -16.9(12) . . . . ?
C20 C24 C25 N8 163.1(9) . . . . ?
N7 C26 C27 C28 179.8(9) . . . . ?
C31 C26 C27 C28 5.2(14) . . . . ?
C26 C27 C28 C29 -4.5(16) . . . . ?
C27 C28 C29 C30 1.2(16) . . . . ?
C28 C29 C30 C31 0.9(16) . . . . ?
N7 C26 C31 C30 -177.4(8) . . . . ?
C27 C26 C31 C30 -2.8(12) . . . . ?
N7 C26 C31 C32 -5.0(12) . . . . ?
C27 C26 C31 C32 169.7(8) . . . . ?
C29 C30 C31 C26 0.0(15) . . . . ?
C29 C30 C31 C32 -172.5(9) . . . . ?
C26 C31 C32 O2 -170.7(8) . . . . ?
C30 C31 C32 O2 2.0(13) . . . . ?
C26 C31 C32 N8 6.3(11) . . . . ?
C30 C31 C32 N8 179.1(8) . . . . ?
N9 C33 C34 N10 -2.2(13) . . . . ?
N9 C33 C34 C35 177.2(10) . . . . ?
N10 C34 C35 C36 -1.7(18) . . . . ?
C33 C34 C35 C36 178.9(12) . . . . ?
C34 C35 C36 C37 2(2) . . . . ?
C35 C36 C37 C38 -0.5(18) . . . . ?
C36 C37 C38 N10 -0.8(17) . . . . ?
C12 C7 N1 C6 -20.9(12) . . . . ?
C8 C7 N1 C6 158.7(8) . . . . ?
N3 C6 N1 C7 43.2(9) . . . . ?
C5 C6 N1 C7 -80.7(9) . . . . ?
C1 C5 N2 C4 -0.6(16) . . . . ?
C6 C5 N2 C4 -176.7(9) . . . . ?
C3 C4 N2 C5 1.9(16) . . . . ?
O1 C13 N3 N4 -3.0(11) . . . . ?
C12 C13 N3 N4 178.3(7) . . . . ?
O1 C13 N3 C6 -162.4(7) . . . . ?
C12 C13 N3 C6 18.8(11) . . . . ?
N1 C6 N3 N4 158.5(7) . . . . ?
C5 C6 N3 N4 -77.0(9) . . . . ?
N1 C6 N3 C13 -43.8(10) . . . . ?
C5 C6 N3 C13 80.6(10) . . . . ?
C15 C14 N4 N3 -179.8(7) . . . . ?
C15 C14 N4 Fe1 2.8(11) . . . . ?
C13 N3 N4 C14 -170.6(8) . . . . ?
C6 N3 N4 C14 -11.0(13) . . . . ?
C13 N3 N4 Fe1 6.9(8) . . . . ?
C6 N3 N4 Fe1 166.5(6) . . . . ?
C16 C15 N5 C19 -3.4(15) . . . . ?
C14 C15 N5 C19 179.4(9) . . . . ?
C16 C15 N5 Fe1 -178.2(8) . . . . ?
C14 C15 N5 Fe1 4.6(11) . . . . ?
C18 C19 N5 C15 5.0(16) . . . . ?
C18 C19 N5 Fe1 179.2(8) . . . . ?
C20 C24 N6 C23 2.5(16) . . . . ?
C25 C24 N6 C23 -177.4(9) . . . . ?
C22 C23 N6 C24 0.2(18) . . . . ?
C31 C26 N7 C25 -20.7(12) . . . . ?
C27 C26 N7 C25 165.0(8) . . . . ?
N8 C25 N7 C26 40.0(10) . . . . ?
C24 C25 N7 C26 -82.7(9) . . . . ?
O2 C32 N8 N9 -5.1(11) . . . . ?
C31 C32 N8 N9 177.6(7) . . . . ?
O2 C32 N8 C25 -166.2(7) . . . . ?
C31 C32 N8 C25 16.6(11) . . . . ?
N7 C25 N8 N9 161.4(7) . . . . ?
C24 C25 N8 N9 -74.9(9) . . . . ?
N7 C25 N8 C32 -38.7(10) . . . . ?
C24 C25 N8 C32 85.0(9) . . . . ?
C34 C33 N9 N8 -179.2(7) . . . . ?
C34 C33 N9 Fe1 2.3(11) . . . . ?
C32 N8 N9 C33 -172.1(8) . . . . ?
C25 N8 N9 C33 -11.2(12) . . . . ?
C32 N8 N9 Fe1 6.5(8) . . . . ?
C25 N8 N9 Fe1 167.4(5) . . . . ?
C37 C38 N10 C34 0.8(15) . . . . ?
C37 C38 N10 Fe1 179.4(8) . . . . ?
C33 C34 N10 C38 179.8(9) . . . . ?
C35 C34 N10 C38 0.4(14) . . . . ?
C33 C34 N10 Fe1 1.0(11) . . . . ?
C35 C34 N10 Fe1 -178.4(8) . . . . ?
N3 C13 O1 Fe1 -2.5(10) . . . . ?
C12 C13 O1 Fe1 176.1(6) . . . . ?
N8 C32 O2 Fe1 1.0(10) . . . . ?
C31 C32 O2 Fe1 178.0(6) . . . . ?

_refine_diff_density_max         1.688
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.152


# start Validation Reply Form
_vrf_PLAT602_1-296K              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: The crystal data is treated with squeeze.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-100K
_database_code_depnum_ccdc_archive 'CCDC 1400828'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 Fe N10 O2, 2(B F4)'
_chemical_formula_sum            'C38 H30 B2 F8 Fe N10 O2'
_chemical_formula_weight         888.19

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8910(19)
_cell_length_b                   12.235(2)
_cell_length_c                   18.064(3)
_cell_angle_alpha                72.999(4)
_cell_angle_beta                 75.187(3)
_cell_angle_gamma                86.189(3)
_cell_volume                     2429.6(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4721
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.381
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12814
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.741
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             8412
_reflns_number_gt                5934
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
High Uiq in the pyridine ring atoms, we treated these problem 
with some restraints. R1 and wR2 are high, for the poor crystal 
quality of this series of crystal. The crystal data is treated 
with squeeze.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8412
_refine_ls_number_parameters     622
_refine_ls_number_restraints     391
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2841
_refine_ls_wR_factor_gt          0.2567
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.212
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.30685(5) 0.99798(5) 0.27045(4) 0.0249(3) Uani 1 1 d . . . . .
C1 C 0.2669(5) 1.3331(5) 0.1119(3) 0.0435(13) Uani 1 1 d . . . . .
H1 H 0.2645 1.4077 0.1181 0.052 Uiso 1 1 calc R U . . .
C2 C 0.2578(5) 1.3161(6) 0.0414(3) 0.0553(16) Uani 1 1 d . . . . .
H2 H 0.2471 1.3794 -0.0015 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2639(5) 1.2106(6) 0.0337(3) 0.0497(15) Uani 1 1 d . . . . .
H3 H 0.2600 1.1991 -0.0154 0.060 Uiso 1 1 calc R U . . .
C4 C 0.2762(4) 1.1165(5) 0.0977(3) 0.0394(12) Uani 1 1 d . . . . .
H4 H 0.2790 1.0417 0.0916 0.047 Uiso 1 1 calc R U . . .
C5 C 0.2797(4) 1.2366(4) 0.1740(3) 0.0344(11) Uani 1 1 d . . . . .
C6 C 0.2906(4) 1.2467(4) 0.2506(3) 0.0308(10) Uani 1 1 d . . . . .
H6 H 0.2874 1.3182 0.2618 0.037 Uiso 1 1 calc R U . . .
C7 C 0.1571(4) 1.2358(4) 0.4498(3) 0.0284(10) Uani 1 1 d . . . . .
C9 C -0.0057(4) 1.3229(4) 0.5141(3) 0.0374(12) Uani 1 1 d . . . . .
H9 H -0.0390 1.3812 0.5378 0.045 Uiso 1 1 calc R U . . .
C10 C -0.0745(4) 1.2371(4) 0.5151(3) 0.0319(11) Uani 1 1 d . . . . .
H10 H -0.1560 1.2354 0.5378 0.038 Uiso 1 1 calc R U . . .
C11 C -0.0213(4) 1.1529(4) 0.4817(3) 0.0319(11) Uani 1 1 d . . . . .
H11 H -0.0686 1.0934 0.4816 0.038 Uiso 1 1 calc R U . . .
N3 N 0.0937(3) 1.1503(3) 0.4493(2) 0.0305(9) Uani 1 1 d . . . . .
C12 C 0.2878(4) 1.2319(4) 0.4154(3) 0.0299(10) Uani 1 1 d . . . . .
H12 H 0.3136 1.3069 0.3750 0.036 Uiso 1 1 calc R U . . .
C13 C 0.3213(3) 1.0287(4) 0.4201(3) 0.0272(10) Uani 1 1 d . . . . .
C14 C 0.3359(3) 1.0086(4) 0.4998(3) 0.0305(11) Uani 1 1 d . . . . .
C15 C 0.3392(4) 0.8974(5) 0.5493(3) 0.0355(12) Uani 1 1 d . . . . .
H15 H 0.3228 0.8350 0.5323 0.043 Uiso 1 1 calc R U . . .
C16 C 0.3654(4) 0.8761(6) 0.6213(3) 0.0419(13) Uani 1 1 d . . . . .
H16 H 0.3667 0.8001 0.6545 0.050 Uiso 1 1 calc R U . . .
C17 C 0.3899(4) 0.9683(6) 0.6449(3) 0.0441(14) Uani 1 1 d . . . . .
H17 H 0.4096 0.9539 0.6947 0.053 Uiso 1 1 calc R U . . .
C18 C 0.3868(4) 1.0798(5) 0.5989(3) 0.0409(14) Uani 1 1 d . . . . .
H18 H 0.4047 1.1407 0.6168 0.049 Uiso 1 1 calc R U . . .
C19 C 0.3567(4) 1.1031(5) 0.5245(3) 0.0341(12) Uani 1 1 d . . . . .
C20 C 0.6382(4) 0.7154(5) 0.1848(3) 0.0367(12) Uani 1 1 d . . . . .
C21 C 0.7521(5) 0.6707(5) 0.1704(3) 0.0441(13) Uani 1 1 d . . . . .
H21 H 0.7643 0.5925 0.1721 0.053 Uiso 1 1 calc R U . . .
C22 C 0.8446(4) 0.7431(6) 0.1537(3) 0.0498(15) Uani 1 1 d . . . . .
H22 H 0.9212 0.7133 0.1448 0.060 Uiso 1 1 calc R U . . .
C23 C 0.8306(4) 0.8564(6) 0.1495(3) 0.0463(14) Uani 1 1 d . . . . .
H23 H 0.8965 0.9050 0.1350 0.056 Uiso 1 1 calc R U . . .
C24 C 0.7182(4) 0.9000(5) 0.1668(3) 0.0350(11) Uani 1 1 d . . . . .
H24 H 0.7071 0.9779 0.1659 0.042 Uiso 1 1 calc R U . . .
C25 C 0.6225(4) 0.8280(4) 0.1852(3) 0.0284(10) Uani 1 1 d . . . . .
C26 C 0.5049(4) 0.8714(4) 0.2095(3) 0.0267(10) Uani 1 1 d . . . . .
C27 C 0.4332(4) 0.6985(4) 0.1903(3) 0.0350(11) Uani 1 1 d . . . . .
H27 H 0.3687 0.6420 0.2207 0.042 Uiso 1 1 calc R U . . .
C28 C 0.4314(4) 0.7374(4) 0.1006(3) 0.0324(11) Uani 1 1 d . . . . .
N7 N 0.4371(3) 0.8472(3) 0.0650(2) 0.0302(9) Uani 1 1 d . . . . .
C32 C 0.4376(5) 0.8784(5) -0.0123(3) 0.0407(12) Uani 1 1 d . . . . .
H32 H 0.4418 0.9578 -0.0395 0.049 Uiso 1 1 calc R U . . .
C31 C 0.4326(5) 0.8041(5) -0.0551(4) 0.0468(14) Uani 1 1 d . . . . .
H31 H 0.4339 0.8309 -0.1103 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4254(6) 0.6898(5) -0.0157(4) 0.0582(17) Uani 1 1 d . . . . .
H30 H 0.4211 0.6353 -0.0431 0.070 Uiso 1 1 calc R U . . .
C33 C 0.2145(4) 0.7954(4) 0.2456(3) 0.0295(10) Uani 1 1 d . . . . .
H33 H 0.2121 0.7291 0.2288 0.035 Uiso 1 1 calc R U . . .
C34 C 0.1093(4) 0.8542(4) 0.2763(3) 0.0275(10) Uani 1 1 d . . . . .
C35 C 0.0000(4) 0.8121(4) 0.2876(3) 0.0326(11) Uani 1 1 d . . . . .
H35 H -0.0096 0.7439 0.2748 0.039 Uiso 1 1 calc R U . . .
C36 C -0.0967(4) 0.8714(5) 0.3182(3) 0.0390(12) Uani 1 1 d . . . . .
H36 H -0.1734 0.8448 0.3262 0.047 Uiso 1 1 calc R U . . .
C37 C -0.0784(4) 0.9681(5) 0.3363(3) 0.0391(12) Uani 1 1 d . . . . .
H37 H -0.1426 1.0090 0.3583 0.047 Uiso 1 1 calc R U . . .
C38 C 0.0353(4) 1.0071(5) 0.3222(3) 0.0339(11) Uani 1 1 d . . . . .
H38 H 0.0468 1.0757 0.3340 0.041 Uiso 1 1 calc R U . . .
N1 N 0.3539(3) 1.2108(4) 0.4756(3) 0.0361(10) Uani 1 1 d . . . . .
H1A H 0.3915 1.2669 0.4804 0.043 Uiso 1 1 calc R U . . .
N2 N 0.3188(3) 1.1407(3) 0.3757(2) 0.0274(8) Uani 1 1 d . . . . .
C8 C 0.1104(4) 1.3250(5) 0.4793(3) 0.0389(12) Uani 1 1 d . . . . .
H8 H 0.1581 1.3867 0.4754 0.047 Uiso 1 1 calc R U . . .
N4 N 0.3047(3) 1.1517(3) 0.3019(2) 0.0246(8) Uani 1 1 d . . . . .
N5 N 0.2840(3) 1.1299(3) 0.1672(2) 0.0291(9) Uani 1 1 d . . . . .
N6 N 0.5421(4) 0.6466(4) 0.2019(3) 0.0436(11) Uani 1 1 d . . . . .
H6A H 0.5473 0.5718 0.2196 0.052 Uiso 1 1 calc R U . . .
C29 C 0.4246(6) 0.6540(5) 0.0651(4) 0.0551(16) Uani 1 1 d . . . . .
H29 H 0.4195 0.5754 0.0943 0.066 Uiso 1 1 calc R U . . .
N8 N 0.4165(3) 0.7956(3) 0.2224(2) 0.0276(8) Uani 1 1 d . . . . .
N9 N 0.3102(3) 0.8408(3) 0.2433(2) 0.0238(8) Uani 1 1 d . . . . .
N10 N 0.1261(3) 0.9524(3) 0.2934(2) 0.0263(8) Uani 1 1 d . . . . .
O1 O 0.3194(3) 0.9509(3) 0.38949(19) 0.0293(7) Uani 1 1 d . . . . .
O2 O 0.4856(2) 0.9642(3) 0.22235(18) 0.0267(7) Uani 1 1 d . . . . .
F8 F 0.0815(3) 0.3974(3) 0.2861(2) 0.0629(10) Uani 1 1 d D U . . .
F3AA F 0.0645(4) 0.5480(3) 0.3366(2) 0.0866(13) Uani 1 1 d D U . . .
F4AA F 0.2384(4) 0.4927(4) 0.2807(4) 0.1255(19) Uani 1 1 d D U . . .
F5 F 0.1198(6) 0.5780(4) 0.2049(3) 0.1363(19) Uani 1 1 d D U . . .
B2 B 0.1237(5) 0.5032(4) 0.2772(3) 0.0723(16) Uani 1 1 d D U . . .
F0AA F 0.5752(9) 1.2553(7) 0.2124(7) 0.0655(19) Uani 0.5032 1 d D U P A 1
F2 F 0.6462(11) 1.3907(12) 0.2545(6) 0.079(2) Uani 0.5032 1 d D U P A 1
F1AA F 0.4960(9) 1.4194(8) 0.1828(9) 0.083(2) Uani 0.5032 1 d D U P A 1
F2AA F 0.6761(13) 1.4398(10) 0.1265(8) 0.090(2) Uani 0.5032 1 d D U P A 1
B1 B 0.6016(6) 1.3672(5) 0.1972(4) 0.071(2) Uani 1 1 d D U . . .
F1 F 0.6575(18) 1.2649(13) 0.1903(16) 0.068(3) Uani 0.2424 1 d D U P A 2
F5AA F 0.6248(16) 1.2548(11) 0.2012(15) 0.064(3) Uani 0.2544 1 d D U P A 3
F3 F 0.4874(12) 1.3929(16) 0.2365(12) 0.087(2) Uani 0.2424 1 d D U P A 2
F4 F 0.666(2) 1.408(2) 0.2377(14) 0.085(3) Uani 0.2424 1 d D U P A 2
F6 F 0.5971(19) 1.386(2) 0.2679(10) 0.086(3) Uani 0.2544 1 d D U P A 3
F7 F 0.6070(19) 1.4570(14) 0.1298(9) 0.088(2) Uani 0.2424 1 d D U P A 2
F9 F 0.684(2) 1.4125(19) 0.1237(13) 0.084(3) Uani 0.2544 1 d D U P A 3
F11 F 0.4963(15) 1.3882(19) 0.1790(16) 0.082(2) Uani 0.2544 1 d D U P A 3


_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 O1 2.099(3) . ?
Fe1 N4 2.115(4) . ?
Fe1 N9 2.115(4) . ?
Fe1 O2 2.143(3) . ?
Fe1 N5 2.145(4) . ?
Fe1 N10 2.161(3) . ?
C1 C2 1.379(8) . ?
C1 C5 1.402(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.334(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(8) . ?
C3 H3 0.9500 . ?
C4 N5 1.339(6) . ?
C4 H4 0.9500 . ?
C5 N5 1.343(6) . ?
C5 C6 1.464(7) . ?
C6 N4 1.289(6) . ?
C6 H6 0.9500 . ?
C7 N3 1.333(6) . ?
C7 C8 1.375(7) . ?
C7 C12 1.523(6) . ?
C9 C8 1.362(7) . ?
C9 C10 1.367(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(7) . ?
C10 H10 0.9500 . ?
C11 N3 1.344(6) . ?
C11 H11 0.9500 . ?
C12 N1 1.454(6) . ?
C12 N2 1.474(6) . ?
C12 H12 1.0000 . ?
C13 O1 1.236(5) . ?
C13 N2 1.373(6) . ?
C13 C14 1.442(6) . ?
C14 C15 1.397(7) . ?
C14 C19 1.412(7) . ?
C15 C16 1.361(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.423(7) . ?
C18 H18 0.9500 . ?
C19 N1 1.359(7) . ?
C20 C25 1.380(7) . ?
C20 N6 1.381(7) . ?
C20 C21 1.416(7) . ?
C21 C22 1.375(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.367(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.399(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.396(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.467(6) . ?
C26 O2 1.219(5) . ?
C26 N8 1.378(6) . ?
C27 N6 1.441(6) . ?
C27 N8 1.449(6) . ?
C27 C28 1.555(7) . ?
C27 H27 1.0000 . ?
C28 N7 1.306(6) . ?
C28 C29 1.370(7) . ?
N7 C32 1.333(7) . ?
C32 C31 1.368(8) . ?
C32 H32 0.9500 . ?
C31 C30 1.369(9) . ?
C31 H31 0.9500 . ?
C30 C29 1.393(9) . ?
C30 H30 0.9500 . ?
C33 N9 1.285(6) . ?
C33 C34 1.466(6) . ?
C33 H33 0.9500 . ?
C34 N10 1.363(6) . ?
C34 C35 1.374(6) . ?
C35 C36 1.397(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.359(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.401(7) . ?
C37 H37 0.9500 . ?
C38 N10 1.305(6) . ?
C38 H38 0.9500 . ?
N1 H1A 0.8800 . ?
N2 N4 1.352(5) . ?
C8 H8 0.9500 . ?
N6 H6A 0.8800 . ?
C29 H29 0.9500 . ?
N8 N9 1.353(5) . ?
F8 B2 1.369(5) . ?
F3AA B2 1.362(5) . ?
F4AA B2 1.378(5) . ?
F5 B2 1.367(5) . ?
F0AA B1 1.357(9) . ?
F2 B1 1.381(10) . ?
F1AA B1 1.420(10) . ?
F2AA B1 1.438(11) . ?
B1 F6 1.348(13) . ?
B1 F11 1.364(13) . ?
B1 F5AA 1.369(12) . ?
B1 F7 1.371(12) . ?
B1 F4 1.384(13) . ?
B1 F1 1.401(13) . ?
B1 F9 1.418(13) . ?
B1 F3 1.424(12) . ?

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
O1 Fe1 N4 73.64(13) . . ?
O1 Fe1 N9 104.16(13) . . ?
N4 Fe1 N9 177.80(14) . . ?
O1 Fe1 O2 94.82(12) . . ?
N4 Fe1 O2 106.57(12) . . ?
N9 Fe1 O2 73.24(12) . . ?
O1 Fe1 N5 148.70(15) . . ?
N4 Fe1 N5 75.18(15) . . ?
N9 Fe1 N5 107.02(15) . . ?
O2 Fe1 N5 96.57(13) . . ?
O1 Fe1 N10 97.81(13) . . ?
N4 Fe1 N10 105.29(14) . . ?
N9 Fe1 N10 75.08(13) . . ?
O2 Fe1 N10 147.89(13) . . ?
N5 Fe1 N10 87.70(14) . . ?
C2 C1 C5 117.8(5) . . ?
C2 C1 H1 121.1 . . ?
C5 C1 H1 121.1 . . ?
C3 C2 C1 119.8(5) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N5 C4 C3 121.3(5) . . ?
N5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
N5 C5 C1 122.7(5) . . ?
N5 C5 C6 115.7(4) . . ?
C1 C5 C6 121.5(5) . . ?
N4 C6 C5 115.3(4) . . ?
N4 C6 H6 122.3 . . ?
C5 C6 H6 122.3 . . ?
N3 C7 C8 123.5(4) . . ?
N3 C7 C12 116.8(4) . . ?
C8 C7 C12 119.7(4) . . ?
C8 C9 C10 120.1(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 117.6(4) . . ?
C9 C10 H10 121.2 . . ?
C11 C10 H10 121.2 . . ?
N3 C11 C10 123.8(4) . . ?
N3 C11 H11 118.1 . . ?
C10 C11 H11 118.1 . . ?
C7 N3 C11 116.4(4) . . ?
N1 C12 N2 106.6(4) . . ?
N1 C12 C7 113.1(4) . . ?
N2 C12 C7 111.5(3) . . ?
N1 C12 H12 108.5 . . ?
N2 C12 H12 108.5 . . ?
C7 C12 H12 108.5 . . ?
O1 C13 N2 120.0(4) . . ?
O1 C13 C14 123.0(4) . . ?
N2 C13 C14 116.8(4) . . ?
C15 C14 C19 120.4(4) . . ?
C15 C14 C13 120.7(4) . . ?
C19 C14 C13 118.7(5) . . ?
C16 C15 C14 121.7(5) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 118.4(6) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C18 C17 C16 122.5(5) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C17 C18 C19 119.6(5) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
N1 C19 C14 119.8(4) . . ?
N1 C19 C18 122.6(5) . . ?
C14 C19 C18 117.4(5) . . ?
C25 C20 N6 119.3(4) . . ?
C25 C20 C21 119.8(5) . . ?
N6 C20 C21 120.8(5) . . ?
C22 C21 C20 118.4(5) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
C23 C22 C21 122.4(5) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 119.3(5) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 119.4(5) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C20 C25 C24 120.5(4) . . ?
C20 C25 C26 120.1(4) . . ?
C24 C25 C26 119.3(4) . . ?
O2 C26 N8 121.7(4) . . ?
O2 C26 C25 123.4(4) . . ?
N8 C26 C25 114.7(4) . . ?
N6 C27 N8 107.7(4) . . ?
N6 C27 C28 111.9(4) . . ?
N8 C27 C28 110.3(4) . . ?
N6 C27 H27 109.0 . . ?
N8 C27 H27 109.0 . . ?
C28 C27 H27 109.0 . . ?
N7 C28 C29 125.3(5) . . ?
N7 C28 C27 117.2(4) . . ?
C29 C28 C27 117.5(5) . . ?
C28 N7 C32 116.1(4) . . ?
N7 C32 C31 124.6(5) . . ?
N7 C32 H32 117.7 . . ?
C31 C32 H32 117.7 . . ?
C32 C31 C30 117.6(6) . . ?
C32 C31 H31 121.2 . . ?
C30 C31 H31 121.2 . . ?
C31 C30 C29 119.4(5) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
N9 C33 C34 114.6(4) . . ?
N9 C33 H33 122.7 . . ?
C34 C33 H33 122.7 . . ?
N10 C34 C35 122.0(4) . . ?
N10 C34 C33 116.3(4) . . ?
C35 C34 C33 121.7(4) . . ?
C34 C35 C36 118.8(5) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C37 C36 C35 118.4(4) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C36 C37 C38 119.8(5) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
N10 C38 C37 122.2(5) . . ?
N10 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C19 N1 C12 119.0(4) . . ?
C19 N1 H1A 120.5 . . ?
C12 N1 H1A 120.5 . . ?
N4 N2 C13 112.9(3) . . ?
N4 N2 C12 122.5(4) . . ?
C13 N2 C12 120.4(4) . . ?
C9 C8 C7 118.5(5) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C6 N4 N2 125.5(4) . . ?
C6 N4 Fe1 118.6(3) . . ?
N2 N4 Fe1 115.9(3) . . ?
C4 N5 C5 118.0(4) . . ?
C4 N5 Fe1 126.9(4) . . ?
C5 N5 Fe1 115.2(3) . . ?
C20 N6 C27 119.3(4) . . ?
C20 N6 H6A 120.4 . . ?
C27 N6 H6A 120.4 . . ?
C28 C29 C30 117.0(6) . . ?
C28 C29 H29 121.5 . . ?
C30 C29 H29 121.5 . . ?
N9 N8 C26 112.1(4) . . ?
N9 N8 C27 121.9(3) . . ?
C26 N8 C27 122.5(4) . . ?
C33 N9 N8 124.1(4) . . ?
C33 N9 Fe1 119.6(3) . . ?
N8 N9 Fe1 116.2(3) . . ?
C38 N10 C34 118.7(4) . . ?
C38 N10 Fe1 127.1(3) . . ?
C34 N10 Fe1 114.1(3) . . ?
C13 O1 Fe1 117.3(3) . . ?
C26 O2 Fe1 115.7(3) . . ?
F3AA B2 F5 109.2(4) . . ?
F3AA B2 F8 111.6(4) . . ?
F5 B2 F8 111.9(4) . . ?
F3AA B2 F4AA 107.7(4) . . ?
F5 B2 F4AA 107.6(5) . . ?
F8 B2 F4AA 108.7(4) . . ?
F6 B1 F11 110.5(14) . . ?
F6 B1 F5AA 110.5(14) . . ?
F11 B1 F5AA 105.9(12) . . ?
F0AA B1 F2 114.2(8) . . ?
F7 B1 F4 102.2(13) . . ?
F7 B1 F1 119.3(15) . . ?
F4 B1 F1 103.2(14) . . ?
F6 B1 F9 127.1(18) . . ?
F11 B1 F9 104.6(15) . . ?
F5AA B1 F9 95.8(12) . . ?
F0AA B1 F1AA 100.8(7) . . ?
F2 B1 F1AA 118.9(10) . . ?
F7 B1 F3 94.5(11) . . ?
F4 B1 F3 99.7(13) . . ?
F1 B1 F3 133.2(13) . . ?
F0AA B1 F2AA 127.8(9) . . ?
F2 B1 F2AA 99.4(9) . . ?
F1AA B1 F2AA 95.7(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -1.5(8) . . . . ?
C1 C2 C3 C4 1.9(9) . . . . ?
C2 C3 C4 N5 -1.2(8) . . . . ?
C2 C1 C5 N5 0.4(8) . . . . ?
C2 C1 C5 C6 179.7(5) . . . . ?
N5 C5 C6 N4 1.0(6) . . . . ?
C1 C5 C6 N4 -178.4(4) . . . . ?
C8 C9 C10 C11 1.7(7) . . . . ?
C9 C10 C11 N3 0.7(8) . . . . ?
C8 C7 N3 C11 -1.7(7) . . . . ?
C12 C7 N3 C11 178.3(4) . . . . ?
C10 C11 N3 C7 -0.7(7) . . . . ?
N3 C7 C12 N1 -111.2(5) . . . . ?
C8 C7 C12 N1 68.9(6) . . . . ?
N3 C7 C12 N2 8.9(6) . . . . ?
C8 C7 C12 N2 -171.1(4) . . . . ?
O1 C13 C14 C15 -5.2(6) . . . . ?
N2 C13 C14 C15 179.8(4) . . . . ?
O1 C13 C14 C19 169.4(4) . . . . ?
N2 C13 C14 C19 -5.5(6) . . . . ?
C19 C14 C15 C16 -1.8(6) . . . . ?
C13 C14 C15 C16 172.8(4) . . . . ?
C14 C15 C16 C17 -0.5(7) . . . . ?
C15 C16 C17 C18 1.1(7) . . . . ?
C16 C17 C18 C19 0.5(7) . . . . ?
C15 C14 C19 N1 179.6(4) . . . . ?
C13 C14 C19 N1 4.9(6) . . . . ?
C15 C14 C19 C18 3.3(6) . . . . ?
C13 C14 C19 C18 -171.4(4) . . . . ?
C17 C18 C19 N1 -178.9(4) . . . . ?
C17 C18 C19 C14 -2.6(6) . . . . ?
C25 C20 C21 C22 -2.6(7) . . . . ?
N6 C20 C21 C22 -180.0(5) . . . . ?
C20 C21 C22 C23 -1.0(8) . . . . ?
C21 C22 C23 C24 3.4(8) . . . . ?
C22 C23 C24 C25 -2.2(7) . . . . ?
N6 C20 C25 C24 -178.8(4) . . . . ?
C21 C20 C25 C24 3.8(7) . . . . ?
N6 C20 C25 C26 4.8(7) . . . . ?
C21 C20 C25 C26 -172.6(4) . . . . ?
C23 C24 C25 C20 -1.3(7) . . . . ?
C23 C24 C25 C26 175.1(4) . . . . ?
C20 C25 C26 O2 169.0(4) . . . . ?
C24 C25 C26 O2 -7.4(7) . . . . ?
C20 C25 C26 N8 -6.7(6) . . . . ?
C24 C25 C26 N8 176.8(4) . . . . ?
N6 C27 C28 N7 -107.8(5) . . . . ?
N8 C27 C28 N7 12.0(6) . . . . ?
N6 C27 C28 C29 71.9(6) . . . . ?
N8 C27 C28 C29 -168.3(5) . . . . ?
C29 C28 N7 C32 -0.8(7) . . . . ?
C27 C28 N7 C32 178.8(4) . . . . ?
C28 N7 C32 C31 0.1(7) . . . . ?
N7 C32 C31 C30 0.6(9) . . . . ?
C32 C31 C30 C29 -0.5(9) . . . . ?
N9 C33 C34 N10 4.0(6) . . . . ?
N9 C33 C34 C35 -175.6(4) . . . . ?
N10 C34 C35 C36 -0.6(7) . . . . ?
C33 C34 C35 C36 179.0(4) . . . . ?
C34 C35 C36 C37 -0.6(7) . . . . ?
C35 C36 C37 C38 1.5(8) . . . . ?
C36 C37 C38 N10 -1.3(8) . . . . ?
C14 C19 N1 C12 23.7(6) . . . . ?
C18 C19 N1 C12 -160.2(4) . . . . ?
N2 C12 N1 C19 -46.4(5) . . . . ?
C7 C12 N1 C19 76.4(5) . . . . ?
O1 C13 N2 N4 5.0(5) . . . . ?
C14 C13 N2 N4 -179.9(3) . . . . ?
O1 C13 N2 C12 162.6(4) . . . . ?
C14 C13 N2 C12 -22.3(5) . . . . ?
N1 C12 N2 N4 -158.3(4) . . . . ?
C7 C12 N2 N4 77.9(5) . . . . ?
N1 C12 N2 C13 46.3(5) . . . . ?
C7 C12 N2 C13 -77.5(5) . . . . ?
C10 C9 C8 C7 -3.9(8) . . . . ?
N3 C7 C8 C9 4.0(8) . . . . ?
C12 C7 C8 C9 -176.0(5) . . . . ?
C5 C6 N4 N2 178.7(4) . . . . ?
C5 C6 N4 Fe1 -1.2(5) . . . . ?
C13 N2 N4 C6 174.4(4) . . . . ?
C12 N2 N4 C6 17.4(6) . . . . ?
C13 N2 N4 Fe1 -5.7(4) . . . . ?
C12 N2 N4 Fe1 -162.7(3) . . . . ?
C3 C4 N5 C5 0.1(7) . . . . ?
C3 C4 N5 Fe1 -178.5(4) . . . . ?
C1 C5 N5 C4 0.3(7) . . . . ?
C6 C5 N5 C4 -179.0(4) . . . . ?
C1 C5 N5 Fe1 179.1(4) . . . . ?
C6 C5 N5 Fe1 -0.3(5) . . . . ?
C25 C20 N6 C27 23.1(7) . . . . ?
C21 C20 N6 C27 -159.6(5) . . . . ?
N8 C27 N6 C20 -44.2(6) . . . . ?
C28 C27 N6 C20 77.1(6) . . . . ?
N7 C28 C29 C30 0.9(9) . . . . ?
C27 C28 C29 C30 -178.7(5) . . . . ?
C31 C30 C29 C28 -0.2(9) . . . . ?
O2 C26 N8 N9 5.3(6) . . . . ?
C25 C26 N8 N9 -178.9(3) . . . . ?
O2 C26 N8 C27 164.8(4) . . . . ?
C25 C26 N8 C27 -19.4(6) . . . . ?
N6 C27 N8 N9 -159.3(4) . . . . ?
C28 C27 N8 N9 78.4(5) . . . . ?
N6 C27 N8 C26 43.2(6) . . . . ?
C28 C27 N8 C26 -79.1(5) . . . . ?
C34 C33 N9 N8 175.1(4) . . . . ?
C34 C33 N9 Fe1 -6.4(5) . . . . ?
C26 N8 N9 C33 168.0(4) . . . . ?
C27 N8 N9 C33 8.4(7) . . . . ?
C26 N8 N9 Fe1 -10.5(4) . . . . ?
C27 N8 N9 Fe1 -170.1(3) . . . . ?
C37 C38 N10 C34 0.2(7) . . . . ?
C37 C38 N10 Fe1 -178.6(4) . . . . ?
C35 C34 N10 C38 0.8(7) . . . . ?
C33 C34 N10 C38 -178.8(4) . . . . ?
C35 C34 N10 Fe1 179.7(4) . . . . ?
C33 C34 N10 Fe1 0.1(5) . . . . ?
N2 C13 O1 Fe1 -1.8(5) . . . . ?
C14 C13 O1 Fe1 -176.6(3) . . . . ?
N8 C26 O2 Fe1 2.4(5) . . . . ?
C25 C26 O2 Fe1 -173.0(3) . . . . ?

_refine_diff_density_max         1.378
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.124


# start Validation Reply Form
_vrf_PLAT602_2-100K              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: The crystal data is treated with squeeze.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-180K
_database_code_depnum_ccdc_archive 'CCDC 1400829'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 Fe N10 O2, 2(B F4)'
_chemical_formula_sum            'C38 H30 B2 F8 Fe N10 O2'
_chemical_formula_weight         888.19

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.893(3)
_cell_length_b                   12.353(3)
_cell_length_c                   18.068(5)
_cell_angle_alpha                73.665(5)
_cell_angle_beta                 75.689(5)
_cell_angle_gamma                86.462(5)
_cell_volume                     2468.1(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    4721
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.375
_shelx_estimated_absorpt_T_min   0.925
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12986
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.718
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             8548
_reflns_number_gt                5437
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
High Uiq in the pyridine ring atoms, we treated these problem 
with some restraints. R1 and wR2 are high, for the poor crystal 
quality of this series of crystal.The crystal data is treated 
with squeeze. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8548
_refine_ls_number_parameters     623
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0962
_refine_ls_wR_factor_ref         0.3096
_refine_ls_wR_factor_gt          0.2812
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.19361(6) 0.00353(6) 0.22902(5) 0.0294(3) Uani 1 1 d . . . . .
C3 C 0.0755(8) 0.3044(7) 0.5198(5) 0.070(2) Uani 1 1 d . . . . .
H3 H 0.0759 0.3581 0.5485 0.084 Uiso 1 1 calc R U . . .
C2 C 0.0706(6) 0.1916(7) 0.5569(4) 0.0533(17) Uani 1 1 d . . . . .
H2 H 0.0716 0.1643 0.6114 0.064 Uiso 1 1 calc R U . . .
C1 C 0.0642(6) 0.1200(6) 0.5138(4) 0.0483(16) Uani 1 1 d . . . . .
H1 H 0.0579 0.0417 0.5405 0.058 Uiso 1 1 calc R U . . .
N1 N 0.0659(4) 0.1502(4) 0.4373(3) 0.0371(11) Uani 1 1 d . . . . .
C5 C 0.0720(5) 0.2599(5) 0.4013(3) 0.0355(13) Uani 1 1 d . . . . .
C6 C 0.0698(5) 0.2984(5) 0.3133(4) 0.0366(13) Uani 1 1 d . . . . .
H6 H 0.1343 0.3539 0.2838 0.044 Uiso 1 1 calc R U . . .
C7 C -0.1333(5) 0.2837(5) 0.3173(3) 0.0404(14) Uani 1 1 d . . . . .
C8 C -0.2464(6) 0.3290(6) 0.3313(4) 0.0534(18) Uani 1 1 d . . . . .
H8 H -0.2583 0.4059 0.3309 0.064 Uiso 1 1 calc R U . . .
C9 C -0.3385(5) 0.2576(7) 0.3456(4) 0.0547(19) Uani 1 1 d . . . . .
H9 H -0.4149 0.2869 0.3542 0.066 Uiso 1 1 calc R U . . .
C10 C -0.3239(5) 0.1448(7) 0.3479(4) 0.0524(18) Uani 1 1 d . . . . .
H10 H -0.3896 0.0972 0.3605 0.063 Uiso 1 1 calc R U . . .
C11 C -0.2136(5) 0.1019(6) 0.3320(4) 0.0393(14) Uani 1 1 d . . . . .
H11 H -0.2028 0.0252 0.3316 0.047 Uiso 1 1 calc R U . . .
C12 C -0.1198(4) 0.1704(5) 0.3167(3) 0.0321(12) Uani 1 1 d . . . . .
C13 C -0.0032(4) 0.1287(5) 0.2919(3) 0.0269(11) Uani 1 1 d . . . . .
C14 C 0.2877(5) 0.2014(5) 0.2553(3) 0.0358(13) Uani 1 1 d . . . . .
H14 H 0.2911 0.2659 0.2735 0.043 Uiso 1 1 calc R U . . .
C15 C 0.3899(5) 0.1471(5) 0.2238(3) 0.0326(12) Uani 1 1 d . . . . .
C16 C 0.5020(5) 0.1884(5) 0.2115(4) 0.0407(14) Uani 1 1 d . . . . .
H16 H 0.5130 0.2555 0.2248 0.049 Uiso 1 1 calc R U . . .
C17 C 0.5950(5) 0.1316(6) 0.1803(4) 0.0463(16) Uani 1 1 d . . . . .
H17 H 0.6715 0.1592 0.1711 0.056 Uiso 1 1 calc R U . . .
C18 C 0.5773(5) 0.0333(6) 0.1621(4) 0.0473(16) Uani 1 1 d . . . . .
H18 H 0.6412 -0.0073 0.1401 0.057 Uiso 1 1 calc R U . . .
C19 C 0.4640(5) -0.0047(5) 0.1768(4) 0.0399(14) Uani 1 1 d . . . . .
H19 H 0.4516 -0.0720 0.1642 0.048 Uiso 1 1 calc R U . . .
C22 C 0.5048(6) -0.3216(6) -0.0134(4) 0.0502(17) Uani 1 1 d . . . . .
H22 H 0.5374 -0.3806 -0.0360 0.060 Uiso 1 1 calc R U . . .
C21 C 0.5734(5) -0.2371(5) -0.0136(4) 0.0432(15) Uani 1 1 d . . . . .
H21 H 0.6548 -0.2359 -0.0354 0.052 Uiso 1 1 calc R U . . .
C20 C 0.5193(5) -0.1525(6) 0.0196(4) 0.0476(16) Uani 1 1 d . . . . .
H20 H 0.5668 -0.0940 0.0205 0.057 Uiso 1 1 calc R U . . .
N6 N 0.4078(4) -0.1480(4) 0.0494(3) 0.0386(12) Uani 1 1 d . . . . .
C24 C 0.3431(5) -0.2331(5) 0.0492(3) 0.0327(12) Uani 1 1 d . . . . .
C25 C 0.2130(5) -0.2273(5) 0.0823(4) 0.0352(13) Uani 1 1 d . . . . .
H25 H 0.1862 -0.3009 0.1221 0.042 Uiso 1 1 calc R U . . .
C26 C 0.1440(5) -0.0999(5) -0.0261(3) 0.0362(13) Uani 1 1 d . . . . .
C27 C 0.1125(5) -0.0783(7) -0.0994(4) 0.0496(18) Uani 1 1 d . . . . .
H27 H 0.0925 -0.1385 -0.1170 0.060 Uiso 1 1 calc R U . . .
C28 C 0.1113(5) 0.0328(6) -0.1450(4) 0.0464(16) Uani 1 1 d . . . . .
H28 H 0.0931 0.0471 -0.1952 0.056 Uiso 1 1 calc R U . . .
C29 C 0.1356(5) 0.1235(7) -0.1205(4) 0.0492(17) Uani 1 1 d . . . . .
H29 H 0.1330 0.1988 -0.1524 0.059 Uiso 1 1 calc R U . . .
C30 C 0.1631(5) 0.1010(5) -0.0496(4) 0.0411(14) Uani 1 1 d . . . . .
H30 H 0.1820 0.1623 -0.0327 0.049 Uiso 1 1 calc R U . . .
C31 C 0.1651(4) -0.0076(5) 0.0000(3) 0.0308(12) Uani 1 1 d . . . . .
C32 C 0.1796(4) -0.0277(4) 0.0802(3) 0.0273(12) Uani 1 1 d . . . . .
C33 C 0.2102(5) -0.2410(5) 0.2462(3) 0.0353(13) Uani 1 1 d . . . . .
H33 H 0.2149 -0.3112 0.2337 0.042 Uiso 1 1 calc R U . . .
C34 C 0.2184(5) -0.2325(5) 0.3247(4) 0.0391(14) Uani 1 1 d . . . . .
C35 C 0.2315(6) -0.3248(6) 0.3847(4) 0.0496(16) Uani 1 1 d . . . . .
H35 H 0.2348 -0.3982 0.3773 0.060 Uiso 1 1 calc R U . . .
C36 C 0.2396(7) -0.3109(7) 0.4537(5) 0.067(2) Uani 1 1 d . . . . .
H36 H 0.2496 -0.3745 0.4956 0.080 Uiso 1 1 calc R U . . .
C37 C 0.2335(6) -0.2048(7) 0.4643(4) 0.0571(19) Uani 1 1 d . . . . .
H37 H 0.2376 -0.1936 0.5135 0.069 Uiso 1 1 calc R U . . .
C38 C 0.2211(5) -0.1156(6) 0.4017(4) 0.0460(15) Uani 1 1 d . . . . .
H38 H 0.2162 -0.0419 0.4086 0.055 Uiso 1 1 calc R U . . .
C4 C 0.0800(7) 0.3386(6) 0.4390(5) 0.0571(18) Uani 1 1 d . . . . .
H4 H 0.0886 0.4162 0.4106 0.069 Uiso 1 1 calc R U . . .
N2 N -0.0385(4) 0.3500(4) 0.3014(3) 0.0466(13) Uani 1 1 d . . . . .
H2A H -0.0433 0.4238 0.2839 0.056 Uiso 1 1 calc R U . . .
N3 N 0.0859(4) 0.2017(4) 0.2799(3) 0.0317(10) Uani 1 1 d . . . . .
N4 N 0.1910(3) 0.1590(4) 0.2579(2) 0.0264(9) Uani 1 1 d . . . . .
N5 N 0.3751(3) 0.0482(4) 0.2068(3) 0.0310(10) Uani 1 1 d . . . . .
C23 C 0.3879(5) -0.3201(5) 0.0198(4) 0.0450(15) Uani 1 1 d . . . . .
H23 H 0.3389 -0.3795 0.0221 0.054 Uiso 1 1 calc R U . . .
N7 N 0.1468(4) -0.2055(5) 0.0218(3) 0.0407(12) Uani 1 1 d . . . . .
H7 H 0.1090 -0.2607 0.0164 0.049 Uiso 1 1 calc R U . . .
N8 N 0.1830(4) -0.1373(4) 0.1216(3) 0.0324(11) Uani 1 1 d . . . . .
N9 N 0.1964(3) -0.1488(4) 0.1965(2) 0.0260(9) Uani 1 1 d . . . . .
N10 N 0.2158(4) -0.1274(4) 0.3317(3) 0.0322(11) Uani 1 1 d . . . . .
B1 B 0.3709(7) 0.4946(6) 0.2239(5) 0.073(3) Uani 1 1 d D . . . .
B2 B -0.0867(8) -0.3693(5) 0.2924(5) 0.087(3) Uani 1 1 d D U . . .
F1 F 0.3512(15) 0.4229(10) 0.2972(5) 0.114(4) Uani 0.5771 1 d D U P A 1
F2 F 0.2597(7) 0.5123(8) 0.2060(7) 0.088(3) Uani 0.5771 1 d D U P A 1
F3 F 0.4415(12) 0.4515(16) 0.1676(10) 0.091(4) Uani 0.5771 1 d D U P A 1
F4 F 0.409(2) 0.5985(11) 0.2219(17) 0.080(7) Uani 0.5771 1 d D U P A 1
F5 F 0.0182(8) -0.4190(8) 0.3046(8) 0.112(4) Uani 0.641(8) 1 d D U P B 1
F6 F -0.1617(10) -0.4295(8) 0.3650(6) 0.132(4) Uani 0.641(8) 1 d D U P B 1
F7 F -0.1277(10) -0.3915(7) 0.2360(5) 0.097(3) Uani 0.641(8) 1 d D U P B 1
F8 F -0.0707(10) -0.2575(6) 0.2839(7) 0.087(3) Uani 0.641(8) 1 d D U P B 1
F6A F -0.0041(14) -0.3589(14) 0.2197(8) 0.129(5) Uani 0.359(8) 1 d D U P B 2
F5A F -0.0390(19) -0.4378(13) 0.3490(9) 0.103(5) Uani 0.359(8) 1 d D U P B 2
F7A F -0.1800(14) -0.4225(15) 0.2833(13) 0.133(6) Uani 0.359(8) 1 d D U P B 2
F8A F -0.1308(18) -0.2690(10) 0.3043(12) 0.094(5) Uani 0.359(8) 1 d D U P B 2
O1 O 0.0160(3) 0.0375(3) 0.2763(2) 0.0322(9) Uani 1 1 d . . . . .
O2 O 0.1824(3) 0.0489(3) 0.1101(2) 0.0354(9) Uani 1 1 d . . . . .
F1A F 0.4324(16) 0.4264(13) 0.2793(10) 0.119(5) Uani 0.4229 1 d D U P A 2
F3A F 0.3973(18) 0.446(2) 0.1629(12) 0.092(6) Uani 0.4229 1 d D U P A 2
F2A F 0.2617(12) 0.4920(14) 0.2660(13) 0.124(6) Uani 0.4229 1 d D U P A 2
F4A F 0.420(3) 0.6013(14) 0.204(2) 0.063(5) Uani 0.4229 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 2.099(4) . ?
Fe1 N9 2.119(4) . ?
Fe1 N4 2.124(4) . ?
Fe1 O1 2.138(4) . ?
Fe1 N10 2.152(5) . ?
Fe1 N5 2.172(4) . ?
C3 C2 1.363(11) . ?
C3 C4 1.389(11) . ?
C3 H3 0.9500 . ?
C2 C1 1.349(9) . ?
C2 H2 0.9500 . ?
C1 N1 1.322(8) . ?
C1 H1 0.9500 . ?
N1 C5 1.326(7) . ?
C5 C4 1.354(8) . ?
C5 C6 1.533(8) . ?
C6 N2 1.439(7) . ?
C6 N3 1.465(7) . ?
C6 H6 1.0000 . ?
C7 N2 1.358(8) . ?
C7 C12 1.403(8) . ?
C7 C8 1.416(8) . ?
C8 C9 1.377(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.457(7) . ?
C13 O1 1.231(6) . ?
C13 N3 1.370(7) . ?
C14 N4 1.277(7) . ?
C14 C15 1.423(8) . ?
C14 H14 0.9500 . ?
C15 N5 1.372(7) . ?
C15 C16 1.401(7) . ?
C16 C17 1.361(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(8) . ?
C18 H18 0.9500 . ?
C19 N5 1.292(7) . ?
C19 H19 0.9500 . ?
C22 C21 1.362(9) . ?
C22 C23 1.373(9) . ?
C22 H22 0.9500 . ?
C21 C20 1.394(9) . ?
C21 H21 0.9500 . ?
C20 N6 1.306(7) . ?
C20 H20 0.9500 . ?
N6 C24 1.342(7) . ?
C24 C23 1.352(8) . ?
C24 C25 1.520(8) . ?
C25 N7 1.456(8) . ?
C25 N8 1.462(7) . ?
C25 H25 1.0000 . ?
C26 N7 1.351(8) . ?
C26 C31 1.409(8) . ?
C26 C27 1.413(8) . ?
C27 C28 1.389(10) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.349(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.451(8) . ?
C32 O2 1.220(6) . ?
C32 N8 1.354(7) . ?
C33 N9 1.266(7) . ?
C33 C34 1.479(8) . ?
C33 H33 0.9500 . ?
C34 N10 1.337(8) . ?
C34 C35 1.366(9) . ?
C35 C36 1.332(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.372(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.370(10) . ?
C37 H37 0.9500 . ?
C38 N10 1.330(7) . ?
C38 H38 0.9500 . ?
C4 H4 0.9500 . ?
N2 H2A 0.8800 . ?
N3 N4 1.339(6) . ?
C23 H23 0.9500 . ?
N7 H7 0.8800 . ?
N8 N9 1.369(6) . ?
B1 F2A 1.331(11) . ?
B1 F1 1.344(10) . ?
B1 F3 1.359(11) . ?
B1 F3A 1.363(13) . ?
B1 F4 1.375(12) . ?
B1 F4A 1.388(12) . ?
B1 F2 1.427(10) . ?
B1 F1A 1.434(12) . ?
B2 F7 1.331(8) . ?
B2 F5A 1.350(8) . ?
B2 F8 1.367(8) . ?
B2 F8A 1.367(9) . ?
B2 F7A 1.389(9) . ?
B2 F5 1.396(8) . ?
B2 F6A 1.411(9) . ?
B2 F6 1.422(8) . ?

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 N9 73.47(16) . . ?
O2 Fe1 N4 104.79(16) . . ?
N9 Fe1 N4 178.25(16) . . ?
O2 Fe1 O1 95.41(14) . . ?
N9 Fe1 O1 106.96(14) . . ?
N4 Fe1 O1 73.23(14) . . ?
O2 Fe1 N10 148.18(17) . . ?
N9 Fe1 N10 74.84(17) . . ?
N4 Fe1 N10 106.89(17) . . ?
O1 Fe1 N10 96.42(15) . . ?
O2 Fe1 N5 97.23(16) . . ?
N9 Fe1 N5 104.80(16) . . ?
N4 Fe1 N5 75.14(16) . . ?
O1 Fe1 N5 147.99(16) . . ?
N10 Fe1 N5 88.05(17) . . ?
C2 C3 C4 118.2(6) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C1 C2 C3 117.9(7) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
N1 C1 C2 125.1(7) . . ?
N1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?
C1 N1 C5 116.6(5) . . ?
N1 C5 C4 122.8(6) . . ?
N1 C5 C6 118.1(5) . . ?
C4 C5 C6 119.1(6) . . ?
N2 C6 N3 107.4(5) . . ?
N2 C6 C5 112.2(5) . . ?
N3 C6 C5 110.3(5) . . ?
N2 C6 H6 109.0 . . ?
N3 C6 H6 109.0 . . ?
C5 C6 H6 109.0 . . ?
N2 C7 C12 120.1(5) . . ?
N2 C7 C8 120.7(6) . . ?
C12 C7 C8 119.1(6) . . ?
C9 C8 C7 117.7(6) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C8 C9 C10 122.4(5) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 119.6(6) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 121.4(5) . . ?
C11 C12 C13 119.7(5) . . ?
C7 C12 C13 118.6(5) . . ?
O1 C13 N3 120.8(4) . . ?
O1 C13 C12 123.1(5) . . ?
N3 C13 C12 115.8(5) . . ?
N4 C14 C15 116.6(5) . . ?
N4 C14 H14 121.7 . . ?
C15 C14 H14 121.7 . . ?
N5 C15 C16 119.8(5) . . ?
N5 C15 C14 116.9(5) . . ?
C16 C15 C14 123.3(5) . . ?
C17 C16 C15 119.4(6) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C19 118.6(6) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
N5 C19 C18 122.5(6) . . ?
N5 C19 H19 118.8 . . ?
C18 C19 H19 118.8 . . ?
C21 C22 C23 119.0(6) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C22 C21 C20 117.3(6) . . ?
C22 C21 H21 121.3 . . ?
C20 C21 H21 121.3 . . ?
N6 C20 C21 124.5(6) . . ?
N6 C20 H20 117.8 . . ?
C21 C20 H20 117.8 . . ?
C20 N6 C24 116.5(5) . . ?
N6 C24 C23 123.3(5) . . ?
N6 C24 C25 116.8(5) . . ?
C23 C24 C25 119.9(5) . . ?
N7 C25 N8 106.0(4) . . ?
N7 C25 C24 113.4(5) . . ?
N8 C25 C24 111.8(4) . . ?
N7 C25 H25 108.5 . . ?
N8 C25 H25 108.5 . . ?
C24 C25 H25 108.5 . . ?
N7 C26 C31 119.1(5) . . ?
N7 C26 C27 122.2(5) . . ?
C31 C26 C27 118.6(6) . . ?
C28 C27 C26 118.5(6) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C29 C28 C27 122.9(6) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 117.5(7) . . ?
C30 C29 H29 121.3 . . ?
C28 C29 H29 121.3 . . ?
C29 C30 C31 123.3(6) . . ?
C29 C30 H30 118.4 . . ?
C31 C30 H30 118.4 . . ?
C30 C31 C26 119.0(5) . . ?
C30 C31 C32 121.6(5) . . ?
C26 C31 C32 119.2(5) . . ?
O2 C32 N8 121.8(5) . . ?
O2 C32 C31 122.3(5) . . ?
N8 C32 C31 115.8(5) . . ?
N9 C33 C34 115.7(5) . . ?
N9 C33 H33 122.1 . . ?
C34 C33 H33 122.1 . . ?
N10 C34 C35 122.5(6) . . ?
N10 C34 C33 115.0(5) . . ?
C35 C34 C33 122.5(6) . . ?
C36 C35 C34 119.3(7) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C37 120.1(7) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C38 C37 C36 117.8(6) . . ?
C38 C37 H37 121.1 . . ?
C36 C37 H37 121.1 . . ?
N10 C38 C37 123.0(7) . . ?
N10 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C5 C4 C3 119.1(7) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C7 N2 C6 119.3(5) . . ?
C7 N2 H2A 120.3 . . ?
C6 N2 H2A 120.3 . . ?
N4 N3 C13 113.4(4) . . ?
N4 N3 C6 121.6(4) . . ?
C13 N3 C6 121.9(4) . . ?
C14 N4 N3 125.9(4) . . ?
C14 N4 Fe1 118.2(4) . . ?
N3 N4 Fe1 115.8(3) . . ?
C19 N5 C15 120.2(5) . . ?
C19 N5 Fe1 126.9(4) . . ?
C15 N5 Fe1 112.8(3) . . ?
C24 C23 C22 119.3(6) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C26 N7 C25 119.6(4) . . ?
C26 N7 H7 120.2 . . ?
C25 N7 H7 120.2 . . ?
C32 N8 N9 112.1(4) . . ?
C32 N8 C25 122.1(5) . . ?
N9 N8 C25 122.1(5) . . ?
C33 N9 N8 125.6(5) . . ?
C33 N9 Fe1 118.9(4) . . ?
N8 N9 Fe1 115.4(3) . . ?
C38 N10 C34 117.2(5) . . ?
C38 N10 Fe1 127.3(4) . . ?
C34 N10 Fe1 115.4(4) . . ?
F1 B1 F3 113.3(11) . . ?
F2A B1 F3A 119.3(13) . . ?
F1 B1 F4 112.1(13) . . ?
F3 B1 F4 112.0(14) . . ?
F2A B1 F4A 111.3(15) . . ?
F3A B1 F4A 112.9(19) . . ?
F1 B1 F2 104.9(9) . . ?
F3 B1 F2 107.8(10) . . ?
F4 B1 F2 106.1(12) . . ?
F2A B1 F1A 104.2(12) . . ?
F3A B1 F1A 103.0(13) . . ?
F4A B1 F1A 104.2(14) . . ?
F7 B2 F8 115.2(7) . . ?
F5A B2 F8A 117.6(11) . . ?
F5A B2 F7A 110.6(11) . . ?
F8A B2 F7A 104.2(11) . . ?
F7 B2 F5 117.2(9) . . ?
F8 B2 F5 104.2(8) . . ?
F5A B2 F6A 106.0(10) . . ?
F8A B2 F6A 114.3(10) . . ?
F7A B2 F6A 103.3(10) . . ?
F7 B2 F6 104.8(8) . . ?
F8 B2 F6 115.8(8) . . ?
F5 B2 F6 98.9(7) . . ?
C13 O1 Fe1 115.9(3) . . ?
C32 O2 Fe1 117.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C3 C2 C1 -3.4(12) . . . . ?
C3 C2 C1 N1 2.2(11) . . . . ?
C2 C1 N1 C5 -1.5(10) . . . . ?
C1 N1 C5 C4 2.2(9) . . . . ?
C1 N1 C5 C6 -177.9(5) . . . . ?
N1 C5 C6 N2 107.6(6) . . . . ?
C4 C5 C6 N2 -72.4(7) . . . . ?
N1 C5 C6 N3 -12.0(7) . . . . ?
C4 C5 C6 N3 167.9(5) . . . . ?
N2 C7 C8 C9 178.8(6) . . . . ?
C12 C7 C8 C9 1.5(9) . . . . ?
C7 C8 C9 C10 1.1(10) . . . . ?
C8 C9 C10 C11 -3.0(10) . . . . ?
C9 C10 C11 C12 2.3(9) . . . . ?
C10 C11 C12 C7 0.3(9) . . . . ?
C10 C11 C12 C13 -173.8(5) . . . . ?
N2 C7 C12 C11 -179.5(6) . . . . ?
C8 C7 C12 C11 -2.2(8) . . . . ?
N2 C7 C12 C13 -5.4(8) . . . . ?
C8 C7 C12 C13 171.9(5) . . . . ?
C11 C12 C13 O1 7.2(8) . . . . ?
C7 C12 C13 O1 -167.1(5) . . . . ?
C11 C12 C13 N3 -178.3(5) . . . . ?
C7 C12 C13 N3 7.4(7) . . . . ?
N4 C14 C15 N5 -6.4(8) . . . . ?
N4 C14 C15 C16 175.0(5) . . . . ?
N5 C15 C16 C17 2.1(9) . . . . ?
C14 C15 C16 C17 -179.4(6) . . . . ?
C15 C16 C17 C18 -0.7(10) . . . . ?
C16 C17 C18 C19 -0.3(10) . . . . ?
C17 C18 C19 N5 -0.1(10) . . . . ?
C23 C22 C21 C20 -0.9(10) . . . . ?
C22 C21 C20 N6 -1.1(10) . . . . ?
C21 C20 N6 C24 1.6(10) . . . . ?
C20 N6 C24 C23 -0.3(9) . . . . ?
C20 N6 C24 C25 -178.8(6) . . . . ?
N6 C24 C25 N7 110.0(6) . . . . ?
C23 C24 C25 N7 -68.6(7) . . . . ?
N6 C24 C25 N8 -9.8(7) . . . . ?
C23 C24 C25 N8 171.6(5) . . . . ?
N7 C26 C27 C28 179.8(5) . . . . ?
C31 C26 C27 C28 4.3(8) . . . . ?
C26 C27 C28 C29 -2.4(8) . . . . ?
C27 C28 C29 C30 1.1(9) . . . . ?
C28 C29 C30 C31 -1.7(9) . . . . ?
C29 C30 C31 C26 3.7(8) . . . . ?
C29 C30 C31 C32 -171.5(5) . . . . ?
N7 C26 C31 C30 179.5(5) . . . . ?
C27 C26 C31 C30 -4.9(7) . . . . ?
N7 C26 C31 C32 -5.2(7) . . . . ?
C27 C26 C31 C32 170.4(5) . . . . ?
C30 C31 C32 O2 5.3(7) . . . . ?
C26 C31 C32 O2 -169.9(5) . . . . ?
C30 C31 C32 N8 -178.4(5) . . . . ?
C26 C31 C32 N8 6.4(7) . . . . ?
N9 C33 C34 N10 -3.1(7) . . . . ?
N9 C33 C34 C35 179.0(5) . . . . ?
N10 C34 C35 C36 1.5(10) . . . . ?
C33 C34 C35 C36 179.3(6) . . . . ?
C34 C35 C36 C37 0.7(11) . . . . ?
C35 C36 C37 C38 -1.2(11) . . . . ?
C36 C37 C38 N10 -0.5(10) . . . . ?
N1 C5 C4 C3 -3.6(11) . . . . ?
C6 C5 C4 C3 176.5(6) . . . . ?
C2 C3 C4 C5 4.1(12) . . . . ?
C12 C7 N2 C6 -23.3(8) . . . . ?
C8 C7 N2 C6 159.5(6) . . . . ?
N3 C6 N2 C7 44.7(7) . . . . ?
C5 C6 N2 C7 -76.6(7) . . . . ?
O1 C13 N3 N4 -6.0(7) . . . . ?
C12 C13 N3 N4 179.4(4) . . . . ?
O1 C13 N3 C6 -166.5(5) . . . . ?
C12 C13 N3 C6 18.9(7) . . . . ?
N2 C6 N3 N4 157.7(5) . . . . ?
C5 C6 N3 N4 -79.7(6) . . . . ?
N2 C6 N3 C13 -43.3(7) . . . . ?
C5 C6 N3 C13 79.3(6) . . . . ?
C15 C14 N4 N3 -174.9(5) . . . . ?
C15 C14 N4 Fe1 7.4(7) . . . . ?
C13 N3 N4 C14 -168.1(5) . . . . ?
C6 N3 N4 C14 -7.5(8) . . . . ?
C13 N3 N4 Fe1 9.6(5) . . . . ?
C6 N3 N4 Fe1 170.2(4) . . . . ?
C18 C19 N5 C15 1.6(9) . . . . ?
C18 C19 N5 Fe1 177.6(4) . . . . ?
C16 C15 N5 C19 -2.5(8) . . . . ?
C14 C15 N5 C19 178.8(5) . . . . ?
C16 C15 N5 Fe1 -179.1(4) . . . . ?
C14 C15 N5 Fe1 2.3(6) . . . . ?
N6 C24 C23 C22 -1.6(10) . . . . ?
C25 C24 C23 C22 176.9(6) . . . . ?
C21 C22 C23 C24 2.1(10) . . . . ?
C31 C26 N7 C25 -23.8(7) . . . . ?
C27 C26 N7 C25 160.7(5) . . . . ?
N8 C25 N7 C26 46.1(6) . . . . ?
C24 C25 N7 C26 -77.0(6) . . . . ?
O2 C32 N8 N9 -3.4(6) . . . . ?
C31 C32 N8 N9 -179.7(4) . . . . ?
O2 C32 N8 C25 -162.1(5) . . . . ?
C31 C32 N8 C25 21.7(6) . . . . ?
N7 C25 N8 C32 -45.8(6) . . . . ?
C24 C25 N8 C32 78.2(6) . . . . ?
N7 C25 N8 N9 157.7(4) . . . . ?
C24 C25 N8 N9 -78.3(6) . . . . ?
C34 C33 N9 N8 -177.8(4) . . . . ?
C34 C33 N9 Fe1 2.4(6) . . . . ?
C32 N8 N9 C33 -174.9(5) . . . . ?
C25 N8 N9 C33 -16.3(7) . . . . ?
C32 N8 N9 Fe1 4.9(5) . . . . ?
C25 N8 N9 Fe1 163.5(4) . . . . ?
C37 C38 N10 C34 2.6(9) . . . . ?
C37 C38 N10 Fe1 178.8(5) . . . . ?
C35 C34 N10 C38 -3.1(8) . . . . ?
C33 C34 N10 C38 179.0(5) . . . . ?
C35 C34 N10 Fe1 -179.8(5) . . . . ?
C33 C34 N10 Fe1 2.3(6) . . . . ?
N3 C13 O1 Fe1 -0.7(6) . . . . ?
C12 C13 O1 Fe1 173.5(4) . . . . ?
N8 C32 O2 Fe1 0.3(6) . . . . ?
C31 C32 O2 Fe1 176.3(3) . . . . ?

_refine_diff_density_max         1.097
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.126


# start Validation Reply Form
_vrf_PLAT602_2-180K              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: The crystal data is treated with squeeze.
;
####################################################################### 
# 
# 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_3-200K
_database_code_depnum_ccdc_archive 'CCDC 1400830'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 Fe N10 O2, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H30 F6 Fe N10 O8 S2'
_chemical_formula_weight         1012.71

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8477(19)
_cell_length_b                   14.823(2)
_cell_length_c                   16.192(4)
_cell_angle_alpha                104.000(5)
_cell_angle_beta                 98.380(5)
_cell_angle_gamma                113.241(4)
_cell_volume                     2440.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    1687
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      23.75

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.475
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13459
_diffrn_reflns_av_unetI/netI     0.1394
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.583
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             8482
_reflns_number_gt                4666
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
MeOH in the structure are disorder, this crystal data is treated 
with squeeze. R1 and wR2 are high, for the poor crystal quality 
of this series of crystal. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8482
_refine_ls_number_parameters     604
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_gt           0.1121
_refine_ls_wR_factor_ref         0.3498
_refine_ls_wR_factor_gt          0.3086
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.43047(10) 0.74979(8) 0.21511(7) 0.0246(4) Uani 1 1 d . . . . .
C1 C 0.5701(9) 0.8213(6) 0.4178(5) 0.039(2) Uani 1 1 d . . . . .
H1 H 0.6070 0.8876 0.4133 0.047 Uiso 1 1 calc R U . . .
C2 C 0.6030(10) 0.8088(7) 0.4989(6) 0.049(2) Uani 1 1 d . . . . .
H2 H 0.6589 0.8655 0.5482 0.059 Uiso 1 1 calc R U . . .
C3 C 0.5518(9) 0.7127(7) 0.5038(6) 0.045(2) Uani 1 1 d . . . . .
H3 H 0.5721 0.7028 0.5576 0.054 Uiso 1 1 calc R U . . .
C4 C 0.4679(9) 0.6264(6) 0.4296(5) 0.042(2) Uani 1 1 d . . . . .
H4 H 0.4329 0.5593 0.4325 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4396(8) 0.6467(6) 0.3507(5) 0.0328(19) Uani 1 1 d . . . . .
C6 C 0.3494(8) 0.5633(5) 0.2707(5) 0.0320(19) Uani 1 1 d . . . . .
H6 H 0.3125 0.4941 0.2679 0.038 Uiso 1 1 calc R U . . .
C7 C 0.2530(7) 0.5756(6) 0.0619(5) 0.0275(17) Uani 1 1 d . . . . .
C8 C 0.1634(8) 0.5074(6) -0.0267(5) 0.0327(19) Uani 1 1 d . . . . .
C9 C 0.1695(9) 0.5494(7) -0.0959(6) 0.041(2) Uani 1 1 d . . . . .
H9 H 0.2346 0.6141 -0.0888 0.049 Uiso 1 1 calc R U . . .
C10 C 0.0754(11) 0.4911(8) -0.1752(6) 0.056(3) Uani 1 1 d . . . . .
H10 H 0.0754 0.5170 -0.2221 0.067 Uiso 1 1 calc R U . . .
C11 C -0.0194(11) 0.3932(9) -0.1842(7) 0.060(3) Uani 1 1 d . . . . .
H11 H -0.0800 0.3540 -0.2385 0.071 Uiso 1 1 calc R U . . .
C12 C -0.0271(8) 0.3525(7) -0.1168(6) 0.044(2) Uani 1 1 d . . . . .
H12 H -0.0940 0.2891 -0.1232 0.053 Uiso 1 1 calc R U . . .
C13 C 0.0707(9) 0.4109(6) -0.0370(6) 0.038(2) Uani 1 1 d . . . . .
C14 C 0.1822(8) 0.4151(5) 0.1041(5) 0.0317(18) Uani 1 1 d . . . . .
H14 H 0.1573 0.4000 0.1562 0.038 Uiso 1 1 calc R U . . .
C15 C 0.2766(8) 0.3712(5) 0.0854(5) 0.0276(17) Uani 1 1 d . . . . .
C16 C 0.4505(8) 0.3860(7) 0.0361(6) 0.038(2) Uani 1 1 d . . . . .
H16 H 0.5184 0.4245 0.0170 0.045 Uiso 1 1 calc R U . . .
C17 C 0.4379(9) 0.2914(7) 0.0412(6) 0.042(2) Uani 1 1 d . . . . .
H17 H 0.4947 0.2662 0.0249 0.050 Uiso 1 1 calc R U . . .
C18 C 0.3434(9) 0.2375(6) 0.0698(6) 0.039(2) Uani 1 1 d . . . . .
H18 H 0.3335 0.1737 0.0746 0.047 Uiso 1 1 calc R U . . .
C19 C 0.2579(9) 0.2754(6) 0.0930(5) 0.038(2) Uani 1 1 d . . . . .
H19 H 0.1905 0.2377 0.1129 0.046 Uiso 1 1 calc R U . . .
C20 C 0.6440(8) 0.6817(6) 0.1834(5) 0.0298(17) Uani 1 1 d . . . . .
H20 H 0.5894 0.6179 0.1865 0.036 Uiso 1 1 calc R U . . .
C21 C 0.7622(8) 0.6962(7) 0.1651(5) 0.036(2) Uani 1 1 d . . . . .
H21 H 0.7839 0.6414 0.1538 0.043 Uiso 1 1 calc R U . . .
C22 C 0.8388(8) 0.7854(7) 0.1642(6) 0.040(2) Uani 1 1 d . . . . .
H22 H 0.9171 0.7943 0.1539 0.048 Uiso 1 1 calc R U . . .
C23 C 0.8103(8) 0.8711(7) 0.1780(5) 0.0354(19) Uani 1 1 d . . . . .
H23 H 0.8657 0.9348 0.1752 0.042 Uiso 1 1 calc R U . . .
C24 C 0.6961(8) 0.8538(6) 0.1957(5) 0.0281(17) Uani 1 1 d . . . . .
C25 C 0.6555(8) 0.9361(6) 0.2146(5) 0.0297(18) Uani 1 1 d . . . . .
H25 H 0.7079 1.0046 0.2202 0.036 Uiso 1 1 calc R U . . .
C26 C 0.3694(7) 0.9251(5) 0.2548(5) 0.0231(16) Uani 1 1 d . . . . .
C27 C 0.3009(8) 0.9882(6) 0.2745(5) 0.0345(19) Uani 1 1 d . . . . .
C28 C 0.1878(8) 0.9495(7) 0.2959(6) 0.042(2) Uani 1 1 d . . . . .
H28 H 0.1568 0.8843 0.3027 0.051 Uiso 1 1 calc R U . . .
C29 C 0.1181(9) 1.0062(8) 0.3076(6) 0.054(3) Uani 1 1 d . . . . .
H29 H 0.0432 0.9825 0.3250 0.064 Uiso 1 1 calc R U . . .
C30 C 0.1690(10) 1.1027(9) 0.2914(7) 0.070(4) Uani 1 1 d . . . . .
H30 H 0.1210 1.1396 0.2938 0.084 Uiso 1 1 calc R U . . .
C31 C 0.2791(10) 1.1433(7) 0.2733(6) 0.047(2) Uani 1 1 d . . . . .
H31 H 0.3088 1.2085 0.2664 0.057 Uiso 1 1 calc R U . . .
C32 C 0.3536(8) 1.0865(6) 0.2640(5) 0.0323(16) Uani 1 1 d . U . . .
C33 C 0.5575(8) 1.0855(6) 0.2679(5) 0.0334(17) Uani 1 1 d . U . . .
H33 H 0.6229 1.1033 0.2359 0.040 Uiso 1 1 calc R U . . .
C34 C 0.6227(8) 1.1294(7) 0.3680(6) 0.0371(16) Uani 1 1 d . U . . .
C35 C 0.5905(8) 1.0650(7) 0.4147(5) 0.0339(15) Uani 1 1 d . U . . .
H35 H 0.5333 0.9951 0.3878 0.041 Uiso 1 1 calc R U . . .
C36 C 0.6433(10) 1.1048(8) 0.5009(6) 0.051(2) Uani 1 1 d . U . . .
H36 H 0.6200 1.0612 0.5347 0.061 Uiso 1 1 calc R U . . .
C37 C 0.7317(10) 1.2080(8) 0.5442(7) 0.054(2) Uani 1 1 d . U . . .
H37 H 0.7683 1.2319 0.6049 0.064 Uiso 1 1 calc R U . . .
C38 C 0.7635(10) 1.2729(8) 0.4963(7) 0.059(2) Uani 1 1 d . U . . .
H38 H 0.8213 1.3427 0.5232 0.071 Uiso 1 1 calc R U . . .
C39 C 0.7185(13) 0.5101(9) 0.3931(8) 0.072(3) Uani 1 1 d . . . . .
C40 C -0.0476(11) -0.3478(8) -0.3312(7) 0.108(4) Uani 1 1 d D U . . .
N1 N 0.3698(6) 0.4266(5) 0.0573(4) 0.0333(16) Uani 1 1 d . . . . .
N2 N 0.0669(6) 0.3705(5) 0.0332(5) 0.0392(18) Uani 1 1 d . . . . .
H2A H -0.0019 0.3207 0.0338 0.047 Uiso 1 1 calc R U . . .
N3 N 0.2430(6) 0.5263(5) 0.1258(4) 0.0290(15) Uani 1 1 d . . . . .
N4 N 0.3249(6) 0.5910(4) 0.2059(4) 0.0253(14) Uani 1 1 d . . . . .
N5 N 0.4865(6) 0.7410(5) 0.3450(4) 0.0269(14) Uani 1 1 d . . . . .
N6 N 0.4694(7) 1.1253(5) 0.2442(5) 0.0399(16) Uani 1 1 d . U . . .
H6A H 0.4881 1.1717 0.2185 0.048 Uiso 1 1 calc R U . . .
N7 N 0.7073(10) 1.2320(6) 0.4056(6) 0.069(2) Uani 1 1 d . U . . .
N8 N 0.4835(6) 0.9712(4) 0.2396(4) 0.0282(15) Uani 1 1 d . . . . .
N9 N 0.5414(6) 0.9058(4) 0.2227(4) 0.0258(14) Uani 1 1 d . . . . .
N10 N 0.6103(5) 0.7594(4) 0.1962(4) 0.0212(13) Uani 1 1 d . . . . .
S1 S 0.5801(3) 0.42901(19) 0.29815(17) 0.0579(8) Uani 1 1 d . . . . .
S2 S 0.0631(4) -0.2388(3) -0.2348(3) 0.0891(11) Uani 1 1 d D U . . .
F1 F 0.8275(8) 0.5382(7) 0.3682(6) 0.121(3) Uani 1 1 d . . . . .
F2 F 0.7145(8) 0.5927(6) 0.4386(5) 0.121(3) Uani 1 1 d . . . . .
F3 F 0.7316(9) 0.4628(7) 0.4483(5) 0.108(3) Uani 1 1 d . . . . .
F4 F -0.1599(11) -0.3447(8) -0.3449(8) 0.160(4) Uani 1 1 d D U . . .
F5 F -0.0842(11) -0.4414(8) -0.3228(7) 0.151(4) Uani 1 1 d D U . . .
F6 F -0.0152(11) -0.3524(9) -0.4056(7) 0.159(4) Uani 1 1 d D U . . .
O1 O 0.3230(5) 0.6690(4) 0.0817(3) 0.0263(12) Uani 1 1 d . . . . .
O2 O 0.3217(5) 0.8306(4) 0.2491(4) 0.0321(13) Uani 1 1 d . . . . .
O3 O 0.5895(11) 0.4957(6) 0.2473(6) 0.112(4) Uani 1 1 d . . . . .
O4 O 0.6009(8) 0.3414(5) 0.2601(5) 0.065(2) Uani 1 1 d . . . . .
O5 O 0.4762(8) 0.4048(6) 0.3384(6) 0.082(2) Uani 1 1 d . . . . .
O6 O 0.0888(11) -0.1491(7) -0.2620(9) 0.134(4) Uani 1 1 d D U . . .
O7 O 0.1753(11) -0.2546(11) -0.2259(9) 0.151(4) Uani 1 1 d D U . . .
O8B O 0.0157(13) -0.2498(9) -0.1616(8) 0.176(6) Uani 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.114(5) . ?
Fe1 O2 2.122(5) . ?
Fe1 N9 2.123(6) . ?
Fe1 N4 2.139(6) . ?
Fe1 N10 2.151(5) . ?
Fe1 N5 2.162(6) . ?
C1 N5 1.356(11) . ?
C1 C2 1.391(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.339(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.405(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(11) . ?
C4 H4 0.9300 . ?
C5 N5 1.317(10) . ?
C5 C6 1.459(11) . ?
C6 N4 1.252(10) . ?
C6 H6 0.9300 . ?
C7 O1 1.228(9) . ?
C7 N3 1.396(10) . ?
C7 C8 1.489(11) . ?
C8 C13 1.367(12) . ?
C8 C9 1.406(12) . ?
C9 C10 1.387(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.397(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.367(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.411(12) . ?
C12 H12 0.9300 . ?
C13 N2 1.406(11) . ?
C14 N3 1.438(9) . ?
C14 N2 1.444(11) . ?
C14 C15 1.531(11) . ?
C14 H14 0.9800 . ?
C15 N1 1.308(9) . ?
C15 C19 1.388(10) . ?
C16 N1 1.359(10) . ?
C16 C17 1.375(11) . ?
C16 H16 0.9300 . ?
C17 C18 1.316(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.392(12) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 N10 1.341(9) . ?
C20 C21 1.418(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.280(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.415(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.362(10) . ?
C23 H23 0.9300 . ?
C24 N10 1.371(9) . ?
C24 C25 1.462(9) . ?
C25 N9 1.284(10) . ?
C25 H25 0.9300 . ?
C26 O2 1.259(8) . ?
C26 N8 1.343(9) . ?
C26 C27 1.472(9) . ?
C27 C28 1.368(12) . ?
C27 C32 1.406(11) . ?
C28 C29 1.392(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.424(16) . ?
C29 H29 0.9300 . ?
C30 C31 1.314(15) . ?
C30 H30 0.9300 . ?
C31 C32 1.441(10) . ?
C31 H31 0.9300 . ?
C32 N6 1.383(11) . ?
C33 N6 1.436(10) . ?
C33 N8 1.478(9) . ?
C33 C34 1.540(12) . ?
C33 H33 0.9800 . ?
C34 C35 1.332(11) . ?
C34 N7 1.364(12) . ?
C35 C36 1.320(12) . ?
C35 H35 0.9300 . ?
C36 C37 1.389(14) . ?
C36 H36 0.9300 . ?
C37 C38 1.353(14) . ?
C37 H37 0.9300 . ?
C38 N7 1.390(13) . ?
C38 H38 0.9300 . ?
C39 F2 1.290(13) . ?
C39 F3 1.291(13) . ?
C39 F1 1.346(15) . ?
C39 S1 1.820(12) . ?
C40 F6 1.311(9) . ?
C40 F5 1.328(9) . ?
C40 F4 1.338(9) . ?
C40 S2 1.810(9) . ?
N2 H2A 0.8600 . ?
N3 N4 1.357(9) . ?
N6 H6A 0.8600 . ?
N8 N9 1.392(8) . ?
S1 O3 1.416(7) . ?
S1 O4 1.427(7) . ?
S1 O5 1.438(9) . ?
S2 O8B 1.400(7) . ?
S2 O7 1.431(8) . ?
S2 O6 1.435(7) . ?

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
O1 Fe1 O2 96.5(2) . . ?
O1 Fe1 N9 106.1(2) . . ?
O2 Fe1 N9 73.6(2) . . ?
O1 Fe1 N4 73.7(2) . . ?
O2 Fe1 N4 108.9(2) . . ?
N9 Fe1 N4 177.6(2) . . ?
O1 Fe1 N10 96.9(2) . . ?
O2 Fe1 N10 147.2(2) . . ?
N9 Fe1 N10 74.0(2) . . ?
N4 Fe1 N10 103.6(2) . . ?
O1 Fe1 N5 147.3(2) . . ?
O2 Fe1 N5 96.1(2) . . ?
N9 Fe1 N5 106.4(2) . . ?
N4 Fe1 N5 73.6(2) . . ?
N10 Fe1 N5 88.5(2) . . ?
N5 C1 C2 122.7(8) . . ?
N5 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.1(8) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 121.4(8) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 116.5(8) . . ?
C5 C4 H4 121.8 . . ?
C3 C4 H4 121.8 . . ?
N5 C5 C4 123.1(7) . . ?
N5 C5 C6 115.9(7) . . ?
C4 C5 C6 121.0(7) . . ?
N4 C6 C5 115.7(7) . . ?
N4 C6 H6 122.2 . . ?
C5 C6 H6 122.2 . . ?
O1 C7 N3 121.1(7) . . ?
O1 C7 C8 124.9(7) . . ?
N3 C7 C8 113.7(7) . . ?
C13 C8 C9 121.7(8) . . ?
C13 C8 C7 120.2(8) . . ?
C9 C8 C7 117.8(7) . . ?
C10 C9 C8 117.8(9) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C9 C10 C11 119.6(9) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 122.9(9) . . ?
C12 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
C11 C12 C13 117.2(9) . . ?
C11 C12 H12 121.4 . . ?
C13 C12 H12 121.4 . . ?
C8 C13 N2 120.7(8) . . ?
C8 C13 C12 120.6(8) . . ?
N2 C13 C12 118.7(8) . . ?
N3 C14 N2 109.6(6) . . ?
N3 C14 C15 110.3(6) . . ?
N2 C14 C15 114.3(6) . . ?
N3 C14 H14 107.4 . . ?
N2 C14 H14 107.4 . . ?
C15 C14 H14 107.4 . . ?
N1 C15 C19 123.1(7) . . ?
N1 C15 C14 115.8(6) . . ?
C19 C15 C14 121.0(7) . . ?
N1 C16 C17 124.0(8) . . ?
N1 C16 H16 118.0 . . ?
C17 C16 H16 118.0 . . ?
C18 C17 C16 118.2(8) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C19 120.4(8) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C15 C19 C18 117.9(8) . . ?
C15 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
N10 C20 C21 120.5(7) . . ?
N10 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 119.3(7) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 123.3(7) . . ?
C21 C22 H22 118.3 . . ?
C23 C22 H22 118.3 . . ?
C24 C23 C22 115.3(7) . . ?
C24 C23 H23 122.3 . . ?
C22 C23 H23 122.3 . . ?
C23 C24 N10 123.4(7) . . ?
C23 C24 C25 121.6(7) . . ?
N10 C24 C25 115.0(6) . . ?
N9 C25 C24 114.3(6) . . ?
N9 C25 H25 122.9 . . ?
C24 C25 H25 122.9 . . ?
O2 C26 N8 120.9(6) . . ?
O2 C26 C27 121.8(7) . . ?
N8 C26 C27 117.2(6) . . ?
C28 C27 C32 122.3(7) . . ?
C28 C27 C26 121.2(7) . . ?
C32 C27 C26 116.3(7) . . ?
C27 C28 C29 121.1(9) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C30 115.7(9) . . ?
C28 C29 H29 122.2 . . ?
C30 C29 H29 122.2 . . ?
C31 C30 C29 124.5(8) . . ?
C31 C30 H30 117.7 . . ?
C29 C30 H30 117.7 . . ?
C30 C31 C32 119.8(9) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
N6 C32 C27 121.6(6) . . ?
N6 C32 C31 122.1(7) . . ?
C27 C32 C31 116.3(8) . . ?
N6 C33 N8 106.8(7) . . ?
N6 C33 C34 112.3(6) . . ?
N8 C33 C34 110.1(6) . . ?
N6 C33 H33 109.2 . . ?
N8 C33 H33 109.2 . . ?
C34 C33 H33 109.2 . . ?
C35 C34 N7 122.6(9) . . ?
C35 C34 C33 117.9(8) . . ?
N7 C34 C33 119.4(7) . . ?
C36 C35 C34 117.2(9) . . ?
C36 C35 H35 121.4 . . ?
C34 C35 H35 121.4 . . ?
C35 C36 C37 123.8(10) . . ?
C35 C36 H36 118.1 . . ?
C37 C36 H36 118.1 . . ?
C38 C37 C36 118.7(10) . . ?
C38 C37 H37 120.7 . . ?
C36 C37 H37 120.7 . . ?
C37 C38 N7 118.0(10) . . ?
C37 C38 H38 121.0 . . ?
N7 C38 H38 121.0 . . ?
F2 C39 F3 105.5(11) . . ?
F2 C39 F1 108.9(10) . . ?
F3 C39 F1 104.6(11) . . ?
F2 C39 S1 113.2(9) . . ?
F3 C39 S1 113.0(9) . . ?
F1 C39 S1 111.2(9) . . ?
F6 C40 F5 107.5(11) . . ?
F6 C40 F4 106.6(11) . . ?
F5 C40 F4 99.7(10) . . ?
F6 C40 S2 116.4(9) . . ?
F5 C40 S2 116.2(9) . . ?
F4 C40 S2 108.7(8) . . ?
C15 N1 C16 116.4(7) . . ?
C13 N2 C14 117.8(6) . . ?
C13 N2 H2A 121.1 . . ?
C14 N2 H2A 121.1 . . ?
N4 N3 C7 112.1(6) . . ?
N4 N3 C14 122.4(6) . . ?
C7 N3 C14 123.1(6) . . ?
C6 N4 N3 125.1(6) . . ?
C6 N4 Fe1 118.9(5) . . ?
N3 N4 Fe1 115.7(4) . . ?
C5 N5 C1 118.2(7) . . ?
C5 N5 Fe1 115.4(5) . . ?
C1 N5 Fe1 126.2(5) . . ?
C32 N6 C33 117.8(6) . . ?
C32 N6 H6A 121.1 . . ?
C33 N6 H6A 121.1 . . ?
C34 N7 C38 119.8(8) . . ?
C26 N8 N9 113.0(5) . . ?
C26 N8 C33 122.2(6) . . ?
N9 N8 C33 121.7(6) . . ?
C25 N9 N8 123.6(6) . . ?
C25 N9 Fe1 120.8(4) . . ?
N8 N9 Fe1 115.6(4) . . ?
C20 N10 C24 118.0(6) . . ?
C20 N10 Fe1 126.1(5) . . ?
C24 N10 Fe1 115.8(4) . . ?
O3 S1 O4 115.3(5) . . ?
O3 S1 O5 116.8(6) . . ?
O4 S1 O5 113.5(5) . . ?
O3 S1 C39 102.2(6) . . ?
O4 S1 C39 104.0(5) . . ?
O5 S1 C39 102.6(6) . . ?
O8B S2 O7 108.9(9) . . ?
O8B S2 O6 122.6(8) . . ?
O7 S2 O6 107.9(8) . . ?
O8B S2 C40 108.2(7) . . ?
O7 S2 C40 102.6(7) . . ?
O6 S2 C40 104.8(7) . . ?
C7 O1 Fe1 117.0(5) . . ?
C26 O2 Fe1 116.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N5 C1 C2 C3 1.7(14) . . . . ?
C1 C2 C3 C4 0.4(14) . . . . ?
C2 C3 C4 C5 -0.9(14) . . . . ?
C3 C4 C5 N5 -0.9(13) . . . . ?
C3 C4 C5 C6 -177.4(8) . . . . ?
N5 C5 C6 N4 -1.2(11) . . . . ?
C4 C5 C6 N4 175.5(7) . . . . ?
O1 C7 C8 C13 -165.9(7) . . . . ?
N3 C7 C8 C13 8.3(9) . . . . ?
O1 C7 C8 C9 7.8(10) . . . . ?
N3 C7 C8 C9 -178.0(6) . . . . ?
C13 C8 C9 C10 2.1(11) . . . . ?
C7 C8 C9 C10 -171.5(7) . . . . ?
C8 C9 C10 C11 -1.3(12) . . . . ?
C9 C10 C11 C12 2.4(13) . . . . ?
C10 C11 C12 C13 -3.9(12) . . . . ?
C9 C8 C13 N2 179.8(7) . . . . ?
C7 C8 C13 N2 -6.8(11) . . . . ?
C9 C8 C13 C12 -3.8(11) . . . . ?
C7 C8 C13 C12 169.6(6) . . . . ?
C11 C12 C13 C8 4.6(11) . . . . ?
C11 C12 C13 N2 -178.9(7) . . . . ?
N3 C14 C15 N1 -26.2(9) . . . . ?
N2 C14 C15 N1 97.8(8) . . . . ?
N3 C14 C15 C19 157.6(7) . . . . ?
N2 C14 C15 C19 -78.4(9) . . . . ?
N1 C16 C17 C18 -1.3(14) . . . . ?
C16 C17 C18 C19 0.8(14) . . . . ?
N1 C15 C19 C18 0.3(13) . . . . ?
C14 C15 C19 C18 176.2(7) . . . . ?
C17 C18 C19 C15 -0.4(13) . . . . ?
N10 C20 C21 C22 2.6(12) . . . . ?
C20 C21 C22 C23 -2.0(14) . . . . ?
C21 C22 C23 C24 2.2(13) . . . . ?
C22 C23 C24 N10 -3.1(12) . . . . ?
C22 C23 C24 C25 177.8(7) . . . . ?
C23 C24 C25 N9 174.5(7) . . . . ?
N10 C24 C25 N9 -4.7(10) . . . . ?
O2 C26 C27 C28 6.4(12) . . . . ?
N8 C26 C27 C28 -176.1(7) . . . . ?
O2 C26 C27 C32 -169.3(7) . . . . ?
N8 C26 C27 C32 8.2(10) . . . . ?
C32 C27 C28 C29 0.6(13) . . . . ?
C26 C27 C28 C29 -174.8(8) . . . . ?
C27 C28 C29 C30 3.2(13) . . . . ?
C28 C29 C30 C31 -5.4(15) . . . . ?
C29 C30 C31 C32 3.4(15) . . . . ?
C28 C27 C32 N6 178.6(8) . . . . ?
C26 C27 C32 N6 -5.7(11) . . . . ?
C28 C27 C32 C31 -2.6(12) . . . . ?
C26 C27 C32 C31 173.0(7) . . . . ?
C30 C31 C32 N6 179.4(8) . . . . ?
C30 C31 C32 C27 0.6(12) . . . . ?
N6 C33 C34 C35 109.5(8) . . . . ?
N8 C33 C34 C35 -9.3(10) . . . . ?
N6 C33 C34 N7 -68.6(10) . . . . ?
N8 C33 C34 N7 172.6(8) . . . . ?
N7 C34 C35 C36 0.7(13) . . . . ?
C33 C34 C35 C36 -177.3(7) . . . . ?
C34 C35 C36 C37 -1.7(14) . . . . ?
C35 C36 C37 C38 2.0(15) . . . . ?
C36 C37 C38 N7 -1.1(15) . . . . ?
C19 C15 N1 C16 -0.7(12) . . . . ?
C14 C15 N1 C16 -176.8(7) . . . . ?
C17 C16 N1 C15 1.2(13) . . . . ?
C8 C13 N2 C14 -20.1(10) . . . . ?
C12 C13 N2 C14 163.5(7) . . . . ?
N3 C14 N2 C13 41.7(8) . . . . ?
C15 C14 N2 C13 -82.8(8) . . . . ?
O1 C7 N3 N4 -4.9(9) . . . . ?
C8 C7 N3 N4 -179.4(5) . . . . ?
O1 C7 N3 C14 -167.9(7) . . . . ?
C8 C7 N3 C14 17.7(9) . . . . ?
N2 C14 N3 N4 156.9(6) . . . . ?
C15 C14 N3 N4 -76.4(8) . . . . ?
N2 C14 N3 C7 -41.8(9) . . . . ?
C15 C14 N3 C7 84.9(8) . . . . ?
C5 C6 N4 N3 -179.3(6) . . . . ?
C5 C6 N4 Fe1 6.6(9) . . . . ?
C7 N3 N4 C6 -168.6(7) . . . . ?
C14 N3 N4 C6 -5.5(11) . . . . ?
C7 N3 N4 Fe1 5.7(7) . . . . ?
C14 N3 N4 Fe1 168.8(5) . . . . ?
C4 C5 N5 C1 2.9(11) . . . . ?
C6 C5 N5 C1 179.6(7) . . . . ?
C4 C5 N5 Fe1 178.8(6) . . . . ?
C6 C5 N5 Fe1 -4.5(9) . . . . ?
C2 C1 N5 C5 -3.4(12) . . . . ?
C2 C1 N5 Fe1 -178.8(6) . . . . ?
C27 C32 N6 C33 -24.0(11) . . . . ?
C31 C32 N6 C33 157.3(8) . . . . ?
N8 C33 N6 C32 45.9(9) . . . . ?
C34 C33 N6 C32 -74.9(9) . . . . ?
C35 C34 N7 C38 0.0(14) . . . . ?
C33 C34 N7 C38 178.0(8) . . . . ?
C37 C38 N7 C34 0.2(15) . . . . ?
O2 C26 N8 N9 -3.2(10) . . . . ?
C27 C26 N8 N9 179.2(6) . . . . ?
O2 C26 N8 C33 -163.5(7) . . . . ?
C27 C26 N8 C33 18.9(10) . . . . ?
N6 C33 N8 C26 -45.0(9) . . . . ?
C34 C33 N8 C26 77.2(9) . . . . ?
N6 C33 N8 N9 156.4(6) . . . . ?
C34 C33 N8 N9 -81.4(8) . . . . ?
C24 C25 N9 N8 -179.2(6) . . . . ?
C24 C25 N9 Fe1 3.0(9) . . . . ?
C26 N8 N9 C25 -173.3(7) . . . . ?
C33 N8 N9 C25 -12.9(10) . . . . ?
C26 N8 N9 Fe1 4.6(8) . . . . ?
C33 N8 N9 Fe1 165.1(5) . . . . ?
C21 C20 N10 C24 -3.3(11) . . . . ?
C21 C20 N10 Fe1 175.2(5) . . . . ?
C23 C24 N10 C20 3.8(11) . . . . ?
C25 C24 N10 C20 -177.0(6) . . . . ?
C23 C24 N10 Fe1 -174.9(6) . . . . ?
C25 C24 N10 Fe1 4.3(8) . . . . ?
F2 C39 S1 O3 62.2(12) . . . . ?
F3 C39 S1 O3 -178.0(10) . . . . ?
F1 C39 S1 O3 -60.7(10) . . . . ?
F2 C39 S1 O4 -177.5(10) . . . . ?
F3 C39 S1 O4 -57.8(11) . . . . ?
F1 C39 S1 O4 59.6(9) . . . . ?
F2 C39 S1 O5 -59.1(11) . . . . ?
F3 C39 S1 O5 60.7(11) . . . . ?
F1 C39 S1 O5 178.0(8) . . . . ?
F6 C40 S2 O8B -177.2(12) . . . . ?
F5 C40 S2 O8B -49.0(13) . . . . ?
F4 C40 S2 O8B 62.5(12) . . . . ?
F6 C40 S2 O7 -62.2(13) . . . . ?
F5 C40 S2 O7 66.0(12) . . . . ?
F4 C40 S2 O7 177.5(10) . . . . ?
F6 C40 S2 O6 50.5(12) . . . . ?
F5 C40 S2 O6 178.7(10) . . . . ?
F4 C40 S2 O6 -69.9(11) . . . . ?
N3 C7 O1 Fe1 1.6(8) . . . . ?
C8 C7 O1 Fe1 175.4(5) . . . . ?
N8 C26 O2 Fe1 0.2(9) . . . . ?
C27 C26 O2 Fe1 177.6(5) . . . . ?

_refine_diff_density_max         2.149
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.155


# start Validation Reply Form
_vrf_PLAT602_3-200K              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: The crystal data is treated with squeeze.
;
####################################################################### 
# 
# 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_4-100K
_database_code_depnum_ccdc_archive 'CCDC 1400831'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H34 Fe N8 O4, 2(Cl O4), O'
_chemical_formula_sum            'C42 H34 Cl2 Fe N8 O13'
_chemical_formula_weight         985.52

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'
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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   33.209(4)
_cell_length_b                   14.8798(18)
_cell_length_c                   18.8479(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9313.6(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2943
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      21.78

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             4048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.360
_exptl_absorpt_coefficient_mu    0.509
_shelx_estimated_absorpt_T_min   0.803
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14543
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.848
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5205
_reflns_number_gt                3483
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_max     0.945
_reflns_Friedel_fraction_full    0.994

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
methoxyl group is disorder in the structure, 
we treated this group with some restrains. R1 and wR2 
are high, for the poor crystal quality of this series of crystal. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.063(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5205
_refine_ls_number_parameters     346
_refine_ls_number_restraints     443
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.0961
_refine_ls_wR_factor_ref         0.2876
_refine_ls_wR_factor_gt          0.2473
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.2500 0.2500 0.78390(9) 0.0427(5) Uani 1 2 d S T P . .
Cl1 Cl 0.11178(9) -0.3051(3) 0.94485(18) 0.0844(10) Uani 1 1 d . U . . .
O1 O 0.29511(17) 0.2650(4) 0.8627(3) 0.0439(14) Uani 1 1 d . . . . .
N4 N 0.2253(2) 0.1658(7) 0.7030(4) 0.067(2) Uani 1 1 d D U . . .
N2 N 0.2976(2) 0.1131(6) 0.8624(4) 0.0494(18) Uani 1 1 d . . . . .
N3 N 0.2718(2) 0.1189(6) 0.8068(4) 0.0497(18) Uani 1 1 d . . . . .
C10 C 0.3764(4) 0.2754(13) 1.0346(7) 0.085(4) Uani 1 1 d . . . . .
H10 H 0.3829 0.3295 1.0564 0.102 Uiso 1 1 calc R U . . .
C8 C 0.3371(2) 0.1960(8) 0.9477(5) 0.053(2) Uani 1 1 d . . . . .
C11 C 0.3936(3) 0.1997(13) 1.0567(6) 0.082(4) Uani 1 1 d . . . . .
H11 H 0.4130 0.2015 1.0922 0.098 Uiso 1 1 calc R U . . .
C12 C 0.3824(3) 0.1166(11) 1.0266(6) 0.076(4) Uani 1 1 d . . . . .
H12 H 0.3939 0.0633 1.0425 0.091 Uiso 1 1 calc R U . . .
C13 C 0.3530(3) 0.1156(9) 0.9710(6) 0.061(3) Uani 1 1 d . . . . .
C7 C 0.3087(2) 0.1957(7) 0.8900(4) 0.048(2) Uani 1 1 d . . . . .
C9 C 0.3487(3) 0.2743(10) 0.9788(5) 0.065(3) Uani 1 1 d . . . . .
H9 H 0.3380 0.3283 0.9626 0.078 Uiso 1 1 calc R U . . .
C14 C 0.3067(3) 0.0268(9) 0.8954(7) 0.071(3) Uani 1 1 d . . . . .
N1 N 0.3422(3) 0.0380(8) 0.9401(6) 0.068(3) Uani 1 1 d . . . . .
H1 H 0.3572 -0.0082 0.9471 0.082 Uiso 1 1 calc R U . . .
O14 O 0.1130(4) -0.2485(8) 1.0042(8) 0.107(3) Uani 1 1 d . U . . .
C2 C 0.1835(4) 0.1294(11) 0.6048(7) 0.095(4) Uani 1 1 d D U . . .
H2 H 0.1674 0.1478 0.5672 0.114 Uiso 1 1 calc R U . . .
C5 C 0.2312(3) 0.0775(9) 0.7141(6) 0.077(3) Uani 1 1 d D U . . .
C3 C 0.1900(5) 0.0427(12) 0.6186(8) 0.103(5) Uani 1 1 d D U . . .
H3 H 0.1780 -0.0001 0.5896 0.124 Uiso 1 1 calc R U . . .
C4 C 0.2135(4) 0.0141(12) 0.6731(8) 0.097(5) Uani 1 1 d D U . . .
H4 H 0.2173 -0.0468 0.6819 0.116 Uiso 1 1 calc R U . . .
C1 C 0.2015(3) 0.1889(11) 0.6483(6) 0.078(3) Uani 1 1 d D U . . .
H1A H 0.1972 0.2498 0.6400 0.094 Uiso 1 1 calc R U . . .
C15 C 0.2671(5) -0.0313(13) 0.9128(11) 0.076(4) Uani 0.4901 1 d G U P A 1
C16 C 0.2529(6) -0.1095(13) 0.8812(10) 0.080(4) Uani 0.4901 1 d G U P A 1
H16 H 0.2662 -0.1334 0.8420 0.096 Uiso 0.4901 1 calc R U P A 1
C17 C 0.2189(6) -0.1521(11) 0.9081(11) 0.090(4) Uani 0.4901 1 d G U P A 1
H17 H 0.2095 -0.2045 0.8870 0.107 Uiso 0.4901 1 calc R U P A 1
C18 C 0.1991(5) -0.1165(13) 0.9667(12) 0.090(4) Uani 0.4901 1 d G U P A 1
H18 H 0.1764 -0.1450 0.9847 0.107 Uiso 0.4901 1 calc R U P A 1
C19 C 0.2133(6) -0.0383(14) 0.9983(10) 0.083(4) Uani 0.4901 1 d G U P A 1
H19 H 0.2001 -0.0145 1.0375 0.100 Uiso 0.4901 1 calc R U P A 1
C20 C 0.2473(6) 0.0043(12) 0.9714(11) 0.078(3) Uani 0.4901 1 d DG U P A 1
C6 C 0.2579(3) 0.0546(9) 0.7717(7) 0.069(3) Uani 1 1 d . U . . .
H6 H 0.2645 -0.0047 0.7822 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2399(9) 0.120(3) 1.0612(16) 0.087(6) Uani 0.4901 1 d D U P A 1
H21A H 0.2530 0.1742 1.0755 0.130 Uiso 0.4901 1 calc R U P A 1
H21B H 0.2125 0.1325 1.0484 0.130 Uiso 0.4901 1 calc R U P A 1
H21C H 0.2404 0.0774 1.0996 0.130 Uiso 0.4901 1 calc R U P A 1
O2 O 0.2609(6) 0.0817(12) 1.0003(11) 0.073(3) Uani 0.4901 1 d D U P A 1
O13 O 0.1490(3) -0.3211(8) 0.9129(6) 0.106(3) Uani 1 1 d . U . . .
O12 O 0.1033(3) -0.3924(9) 0.9839(7) 0.102(3) Uani 1 1 d . U . . .
O11 O 0.0760(4) -0.2809(13) 0.9125(8) 0.137(3) Uani 1 1 d . U . . .
O1W O 0.1579(9) -0.273(2) 0.7276(18) 0.123(8) Uiso 0.5 1 d . . P . .
C15A C 0.2710(5) -0.0083(11) 0.9365(10) 0.067(3) Uani 0.5099 1 d G U P A 2
C16A C 0.2569(5) -0.0934(10) 0.9190(9) 0.078(4) Uani 0.5099 1 d G U P A 2
H16A H 0.2699 -0.1269 0.8841 0.094 Uiso 0.5099 1 calc R U P A 2
C17A C 0.2234(5) -0.1285(10) 0.9535(11) 0.085(4) Uani 0.5099 1 d G U P A 2
H17A H 0.2140 -0.1855 0.9417 0.102 Uiso 0.5099 1 calc R U P A 2
C18A C 0.2040(5) -0.0785(12) 1.0056(11) 0.084(4) Uani 0.5099 1 d G U P A 2
H18A H 0.1816 -0.1020 1.0287 0.101 Uiso 0.5099 1 calc R U P A 2
C19A C 0.2181(5) 0.0066(11) 1.0232(9) 0.080(4) Uani 0.5099 1 d G U P A 2
H19A H 0.2052 0.0400 1.0580 0.095 Uiso 0.5099 1 calc R U P A 2
C20A C 0.2516(5) 0.0417(10) 0.9886(10) 0.073(3) Uani 0.5099 1 d DG U P A 2
O2A O 0.2660(7) 0.1232(12) 1.0056(12) 0.085(4) Uani 0.5099 1 d D U P A 2
C21A C 0.2485(9) 0.178(2) 1.0611(14) 0.085(6) Uani 0.5099 1 d D U P A 2
H21D H 0.2632 0.2338 1.0647 0.128 Uiso 0.5099 1 calc R U P A 2
H21E H 0.2209 0.1910 1.0498 0.128 Uiso 0.5099 1 calc R U P A 2
H21F H 0.2499 0.1469 1.1055 0.128 Uiso 0.5099 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.121(6) . ?
Fe1 O1 2.121(6) 14 ?
Fe1 N3 2.125(9) 14 ?
Fe1 N3 2.125(9) . ?
Fe1 N4 2.137(9) . ?
Fe1 N4 2.137(9) 14 ?
Cl1 O11 1.384(14) . ?
Cl1 O13 1.396(10) . ?
Cl1 O14 1.401(14) . ?
Cl1 O12 1.519(13) . ?
O1 C7 1.239(11) . ?
N4 C1 1.343(11) . ?
N4 C5 1.344(13) . ?
N2 N3 1.355(11) . ?
N2 C7 1.385(14) . ?
N2 C14 1.460(15) . ?
N3 C6 1.251(14) . ?
C10 C11 1.33(2) . ?
C10 C9 1.397(14) . ?
C10 H10 0.9300 . ?
C8 C9 1.361(18) . ?
C8 C13 1.380(16) . ?
C8 C7 1.439(12) . ?
C11 C12 1.41(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.431(16) . ?
C12 H12 0.9300 . ?
C13 N1 1.342(18) . ?
C9 H9 0.9300 . ?
C14 N1 1.459(16) . ?
C14 C15A 1.509(16) . ?
C14 C15 1.607(18) . ?
N1 H1 0.8600 . ?
C2 C3 1.334(12) . ?
C2 C1 1.346(12) . ?
C2 H2 0.9300 . ?
C5 C4 1.354(12) . ?
C5 C6 1.443(19) . ?
C3 C4 1.356(12) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C1 H1A 0.9300 . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C16 H16 0.9300 . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 H18 0.9300 . ?
C19 C20 1.3900 . ?
C19 H19 0.9300 . ?
C20 O2 1.351(12) . ?
C6 H6 0.9300 . ?
C21 O2 1.46(2) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C15A C16A 1.3900 . ?
C15A C20A 1.3900 . ?
C16A C17A 1.3900 . ?
C16A H16A 0.9300 . ?
C17A C18A 1.3900 . ?
C17A H17A 0.9300 . ?
C18A C19A 1.3900 . ?
C18A H18A 0.9300 . ?
C19A C20A 1.3900 . ?
C19A H19A 0.9300 . ?
C20A O2A 1.342(16) . ?
O2A C21A 1.45(2) . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 91.1(3) . 14 ?
O1 Fe1 N3 90.1(3) . 14 ?
O1 Fe1 N3 73.4(3) 14 14 ?
O1 Fe1 N3 73.4(3) . . ?
O1 Fe1 N3 90.1(3) 14 . ?
N3 Fe1 N3 156.6(4) 14 . ?
O1 Fe1 N4 146.3(3) . . ?
O1 Fe1 N4 99.6(3) 14 . ?
N3 Fe1 N4 123.5(3) 14 . ?
N3 Fe1 N4 74.8(3) . . ?
O1 Fe1 N4 99.6(3) . 14 ?
O1 Fe1 N4 146.3(3) 14 14 ?
N3 Fe1 N4 74.8(3) 14 14 ?
N3 Fe1 N4 123.5(3) . 14 ?
N4 Fe1 N4 88.9(5) . 14 ?
O11 Cl1 O13 128.0(9) . . ?
O11 Cl1 O14 102.8(9) . . ?
O13 Cl1 O14 114.9(8) . . ?
O11 Cl1 O12 106.1(9) . . ?
O13 Cl1 O12 103.1(7) . . ?
O14 Cl1 O12 97.6(8) . . ?
C7 O1 Fe1 117.4(6) . . ?
C1 N4 C5 117.1(11) . . ?
C1 N4 Fe1 128.5(9) . . ?
C5 N4 Fe1 114.0(6) . . ?
N3 N2 C7 113.7(7) . . ?
N3 N2 C14 121.1(9) . . ?
C7 N2 C14 124.4(9) . . ?
C6 N3 N2 126.3(10) . . ?
C6 N3 Fe1 118.0(8) . . ?
N2 N3 Fe1 115.5(6) . . ?
C11 C10 C9 120.6(16) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C9 C8 C13 119.7(10) . . ?
C9 C8 C7 121.0(9) . . ?
C13 C8 C7 119.3(11) . . ?
C10 C11 C12 120.3(11) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 118.9(11) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
N1 C13 C8 120.3(10) . . ?
N1 C13 C12 120.6(11) . . ?
C8 C13 C12 119.0(13) . . ?
O1 C7 N2 119.1(8) . . ?
O1 C7 C8 123.3(10) . . ?
N2 C7 C8 117.5(9) . . ?
C8 C9 C10 121.4(13) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
N1 C14 N2 108.2(10) . . ?
N1 C14 C15A 112.2(11) . . ?
N2 C14 C15A 111.2(11) . . ?
N1 C14 C15 127.3(12) . . ?
N2 C14 C15 113.0(11) . . ?
C13 N1 C14 124.5(10) . . ?
C13 N1 H1 117.7 . . ?
C14 N1 H1 117.7 . . ?
C3 C2 C1 116.4(14) . . ?
C3 C2 H2 121.8 . . ?
C1 C2 H2 121.8 . . ?
N4 C5 C4 121.9(14) . . ?
N4 C5 C6 115.9(9) . . ?
C4 C5 C6 122.1(15) . . ?
C2 C3 C4 123.0(15) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C5 C4 C3 117.5(16) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
N4 C1 C2 124.0(13) . . ?
N4 C1 H1A 118.0 . . ?
C2 C1 H1A 118.0 . . ?
C16 C15 C20 120.0 . . ?
C16 C15 C14 129.8(12) . . ?
C20 C15 C14 110.1(12) . . ?
C17 C16 C15 120.0 . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
O2 C20 C19 120.8(15) . . ?
O2 C20 C15 119.2(15) . . ?
C19 C20 C15 120.0 . . ?
N3 C6 C5 116.3(12) . . ?
N3 C6 H6 121.8 . . ?
C5 C6 H6 121.8 . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 O2 C21 119(2) . . ?
C16A C15A C20A 120.0 . . ?
C16A C15A C14 117.2(11) . . ?
C20A C15A C14 122.8(11) . . ?
C15A C16A C17A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
C17A C16A H16A 120.0 . . ?
C16A C17A C18A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C18A C17A H17A 120.0 . . ?
C19A C18A C17A 120.0 . . ?
C19A C18A H18A 120.0 . . ?
C17A C18A H18A 120.0 . . ?
C18A C19A C20A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C20A C19A H19A 120.0 . . ?
O2A C20A C19A 120.9(14) . . ?
O2A C20A C15A 119.1(14) . . ?
C19A C20A C15A 120.0 . . ?
C20A O2A C21A 123(2) . . ?
O2A C21A H21D 109.5 . . ?
O2A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
O2A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N2 N3 C6 178.5(8) . . . . ?
C14 N2 N3 C6 -10.8(13) . . . . ?
C7 N2 N3 Fe1 -6.7(9) . . . . ?
C14 N2 N3 Fe1 164.0(7) . . . . ?
C9 C10 C11 C12 -3.3(18) . . . . ?
C10 C11 C12 C13 1.3(16) . . . . ?
C9 C8 C13 N1 -179.1(9) . . . . ?
C7 C8 C13 N1 0.1(13) . . . . ?
C9 C8 C13 C12 -1.5(13) . . . . ?
C7 C8 C13 C12 177.7(8) . . . . ?
C11 C12 C13 N1 178.8(10) . . . . ?
C11 C12 C13 C8 1.1(14) . . . . ?
Fe1 O1 C7 N2 7.7(10) . . . . ?
Fe1 O1 C7 C8 -175.2(6) . . . . ?
N3 N2 C7 O1 -0.6(11) . . . . ?
C14 N2 C7 O1 -170.9(8) . . . . ?
N3 N2 C7 C8 -177.9(6) . . . . ?
C14 N2 C7 C8 11.8(12) . . . . ?
C9 C8 C7 O1 4.4(12) . . . . ?
C13 C8 C7 O1 -174.8(8) . . . . ?
C9 C8 C7 N2 -178.4(8) . . . . ?
C13 C8 C7 N2 2.4(11) . . . . ?
C13 C8 C9 C10 -0.5(14) . . . . ?
C7 C8 C9 C10 -179.7(9) . . . . ?
C11 C10 C9 C8 3.0(17) . . . . ?
N3 N2 C14 N1 165.5(8) . . . . ?
C7 N2 C14 N1 -24.8(13) . . . . ?
N3 N2 C14 C15A -70.8(14) . . . . ?
C7 N2 C14 C15A 98.9(13) . . . . ?
N3 N2 C14 C15 -48.1(14) . . . . ?
C7 N2 C14 C15 121.5(12) . . . . ?
C8 C13 N1 C14 -17.1(15) . . . . ?
C12 C13 N1 C14 165.3(9) . . . . ?
N2 C14 N1 C13 27.7(14) . . . . ?
C15A C14 N1 C13 -95.4(13) . . . . ?
C15 C14 N1 C13 -112.5(15) . . . . ?
C1 N4 C5 C4 -1.1(17) . . . . ?
Fe1 N4 C5 C4 171.8(10) . . . . ?
C1 N4 C5 C6 178.1(9) . . . . ?
Fe1 N4 C5 C6 -9.0(12) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
N4 C5 C4 C3 1(2) . . . . ?
C6 C5 C4 C3 -177.6(12) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C5 N4 C1 C2 0.0(17) . . . . ?
Fe1 N4 C1 C2 -171.7(10) . . . . ?
C3 C2 C1 N4 1(2) . . . . ?
N1 C14 C15 C16 -112.1(19) . . . . ?
N2 C14 C15 C16 109.3(17) . . . . ?
N1 C14 C15 C20 64.0(18) . . . . ?
N2 C14 C15 C20 -74.6(14) . . . . ?
C20 C15 C16 C17 0.0 . . . . ?
C14 C15 C16 C17 176(2) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 O2 178(2) . . . . ?
C18 C19 C20 C15 0.0 . . . . ?
C16 C15 C20 O2 -178(2) . . . . ?
C14 C15 C20 O2 5.2(19) . . . . ?
C16 C15 C20 C19 0.0 . . . . ?
C14 C15 C20 C19 -176.5(18) . . . . ?
N2 N3 C6 C5 -179.4(8) . . . . ?
Fe1 N3 C6 C5 6.0(12) . . . . ?
N4 C5 C6 N3 2.3(14) . . . . ?
C4 C5 C6 N3 -178.6(11) . . . . ?
C19 C20 O2 C21 1(3) . . . . ?
C15 C20 O2 C21 179(2) . . . . ?
N1 C14 C15A C16A -114.5(14) . . . . ?
N2 C14 C15A C16A 124.1(13) . . . . ?
N1 C14 C15A C20A 67.4(16) . . . . ?
N2 C14 C15A C20A -54.0(16) . . . . ?
C20A C15A C16A C17A 0.0 . . . . ?
C14 C15A C16A C17A -178.2(17) . . . . ?
C15A C16A C17A C18A 0.0 . . . . ?
C16A C17A C18A C19A 0.0 . . . . ?
C17A C18A C19A C20A 0.0 . . . . ?
C18A C19A C20A O2A -179(2) . . . . ?
C18A C19A C20A C15A 0.0 . . . . ?
C16A C15A C20A O2A 179(2) . . . . ?
C14 C15A C20A O2A -3(2) . . . . ?
C16A C15A C20A C19A 0.0 . . . . ?
C14 C15A C20A C19A 178.1(18) . . . . ?
C19A C20A O2A C21A 1(3) . . . . ?
C15A C20A O2A C21A -178(2) . . . . ?

_refine_diff_density_max         1.137
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.244

####################################################################### 
# 
# 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_4-296K
_database_code_depnum_ccdc_archive 'CCDC 1400832'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H34 Fe N8 O4, 2(Cl O4), O'
_chemical_formula_sum            'C42 H35.33 Cl2 Fe N8 O12.67'
_chemical_formula_weight         981.52

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'
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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   33.402(6)
_cell_length_b                   15.304(3)
_cell_length_c                   19.044(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9734(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2943
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      21.78

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             4037
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.360
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   0.811
_shelx_estimated_absorpt_T_max   0.844
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12941
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.813
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_point_group_measured_fraction_full 0.898
_reflns_number_total             3868
_reflns_number_gt                3021
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_max     0.788
_reflns_Friedel_fraction_full    0.788

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
methoxyl group is disorder in the structure,
we treated this group with some restraints. R1 and wR2 
are high, for the poor crystal quality of this series of crystal. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1014 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3868
_refine_ls_number_parameters     353
_refine_ls_number_restraints     504
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.2491
_refine_ls_wR_factor_gt          0.2336
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.27761(10) 0.0567(5) Uani 1 2 d S T P . .
N2 N 0.02095(19) 0.3708(5) 0.2561(4) 0.0592(17) Uani 1 1 d . . . . .
N3 N 0.04678(19) 0.3623(5) 0.2016(4) 0.0614(17) Uani 1 1 d . . . . .
N1 N -0.0254(2) 0.4205(6) 0.3586(4) 0.073(2) Uani 1 1 d . U . . .
C14 C 0.0865(2) 0.4422(7) 0.1160(5) 0.066(2) Uani 1 1 d . . . . .
C9 C 0.1018(3) 0.3601(8) 0.0933(6) 0.078(3) Uani 1 1 d . . . . .
N4 N 0.0907(3) 0.2866(7) 0.1247(5) 0.086(3) Uani 1 1 d . . . . .
H4 H 0.1053 0.2411 0.1177 0.104 Uiso 1 1 calc R U . . .
C15 C 0.0582(2) 0.4416(5) 0.1739(4) 0.0574(19) Uani 1 1 d . . . . .
C16 C 0.0066(3) 0.3091(6) 0.2918(5) 0.070(2) Uani 1 1 d . . . . .
H16 H 0.0122 0.2510 0.2816 0.084 Uiso 1 1 calc R U . . .
C8 C 0.0551(3) 0.2765(7) 0.1712(6) 0.075(3) Uani 1 1 d D . . . .
C13 C 0.0983(3) 0.5158(9) 0.0845(6) 0.085(3) Uani 1 1 d . . . . .
H13 H 0.0870 0.5686 0.0984 0.102 Uiso 1 1 calc R U . . .
C10 C 0.1307(3) 0.3599(9) 0.0387(6) 0.089(3) Uani 1 1 d . U . . .
H10 H 0.1421 0.3079 0.0233 0.107 Uiso 1 1 calc R U . . .
O1 O 0.04538(17) 0.5100(4) 0.1998(3) 0.0634(15) Uani 1 1 d . . . . .
C11 C 0.1416(3) 0.4394(10) 0.0089(7) 0.100(4) Uani 1 1 d . U . . .
H11 H 0.1597 0.4392 -0.0282 0.120 Uiso 1 1 calc R U . . .
C17 C -0.0192(3) 0.3340(7) 0.3500(5) 0.073(2) Uani 1 1 d . U . . .
C12 C 0.1272(4) 0.5159(10) 0.0309(8) 0.101(4) Uani 1 1 d . U . . .
H12 H 0.1360 0.5680 0.0112 0.121 Uiso 1 1 calc R U . . .
C20 C -0.0650(4) 0.3884(13) 0.4589(8) 0.114(4) Uani 1 1 d . U . . .
H20 H -0.0799 0.4078 0.4971 0.137 Uiso 1 1 calc R U . . .
C21 C -0.0479(4) 0.4465(10) 0.4134(7) 0.097(3) Uani 1 1 d . U . . .
H21 H -0.0518 0.5060 0.4206 0.116 Uiso 1 1 calc R U . . .
C18 C -0.0366(4) 0.2739(11) 0.3942(8) 0.103(4) Uani 1 1 d . U . . .
H18 H -0.0325 0.2142 0.3880 0.124 Uiso 1 1 calc R U . . .
C19 C -0.0600(4) 0.3050(12) 0.4474(8) 0.113(4) Uani 1 1 d . U . . .
H19 H -0.0728 0.2652 0.4766 0.136 Uiso 1 1 calc R U . . .
Cl1 Cl 0.11164(8) 0.3077(3) 0.37125(18) 0.1076(11) Uani 1 1 d D U . . .
O12 O 0.1483(3) 0.3162(10) 0.4074(8) 0.205(7) Uani 1 1 d D U . . .
O13 O 0.1146(5) 0.2434(8) 0.3171(6) 0.177(6) Uani 1 1 d D U . . .
O14 O 0.1050(4) 0.3907(6) 0.3345(7) 0.157(5) Uani 1 1 d D U . . .
O2 O 0.0110(6) 0.3344(11) 0.0615(11) 0.102(3) Uani 0.523 1 d D U P A 1
C7 C 0.0178(5) 0.2239(12) 0.1474(11) 0.100(4) Uani 0.523 1 d DG U P A 1
C6 C 0.0053(5) 0.1450(12) 0.1763(10) 0.108(4) Uani 0.523 1 d G U P A 1
H6 H 0.0194 0.1206 0.2136 0.129 Uiso 0.523 1 calc R U P A 1
C5 C -0.0282(6) 0.1028(10) 0.1495(12) 0.117(4) Uani 0.523 1 d G U P A 1
H5 H -0.0366 0.0500 0.1688 0.140 Uiso 0.523 1 calc R U P A 1
C4 C -0.0493(5) 0.1393(12) 0.0938(11) 0.115(5) Uani 0.523 1 d G U P A 1
H4A H -0.0717 0.1110 0.0759 0.138 Uiso 0.523 1 calc R U P A 1
C3 C -0.0368(5) 0.2182(13) 0.0649(10) 0.108(4) Uani 0.523 1 d G U P A 1
H3 H -0.0509 0.2426 0.0276 0.130 Uiso 0.523 1 calc R U P A 1
C2 C -0.0033(6) 0.2604(11) 0.0917(11) 0.102(3) Uani 0.523 1 d DG U P A 1
C1 C -0.0147(10) 0.361(2) 0.0066(18) 0.118(6) Uani 0.523 1 d D U P A 1
H1A H -0.0001 0.3620 -0.0368 0.177 Uiso 0.523 1 calc R U P A 1
H1B H -0.0248 0.4187 0.0165 0.177 Uiso 0.523 1 calc R U P A 1
H1C H -0.0367 0.3210 0.0029 0.177 Uiso 0.523 1 calc R U P A 1
O1W O 0.0861(16) 0.023(3) 0.341(2) 0.165(16) Uani 0.3333 1 d . . P . .
H1WA H 0.0746 0.0070 0.3036 0.198 Uiso 0.3333 1 d R U P . .
H1WB H 0.0925 -0.0139 0.3723 0.198 Uiso 0.3333 1 d R U P . .
O11 O 0.0787(4) 0.2909(12) 0.4150(8) 0.255(8) Uani 1 1 d D U . . .
C7A C 0.0183(6) 0.2444(12) 0.1291(12) 0.096(4) Uani 0.477 1 d DG U P A 2
C6A C 0.0048(6) 0.1611(12) 0.1459(11) 0.106(4) Uani 0.477 1 d G U P A 2
H6A H 0.0177 0.1287 0.1804 0.127 Uiso 0.477 1 calc R U P A 2
C5A C -0.0281(6) 0.1261(11) 0.1110(13) 0.113(4) Uani 0.477 1 d G U P A 2
H5A H -0.0371 0.0704 0.1222 0.135 Uiso 0.477 1 calc R U P A 2
C4A C -0.0475(5) 0.1745(14) 0.0594(13) 0.114(5) Uani 0.477 1 d G U P A 2
H4AA H -0.0694 0.1511 0.0361 0.136 Uiso 0.477 1 calc R U P A 2
C3A C -0.0339(6) 0.2578(13) 0.0426(11) 0.106(4) Uani 0.477 1 d G U P A 2
H3A H -0.0469 0.2902 0.0081 0.127 Uiso 0.477 1 calc R U P A 2
C2A C -0.0011(6) 0.2928(11) 0.0775(13) 0.101(4) Uani 0.477 1 d DG U P A 2
O2A O 0.0150(8) 0.3716(13) 0.0623(14) 0.113(4) Uani 0.477 1 d D U P A 2
C1A C -0.0030(9) 0.415(2) 0.0048(17) 0.106(7) Uani 0.477 1 d D U P A 2
H1AA H -0.0100 0.3724 -0.0305 0.159 Uiso 0.477 1 calc R U P A 2
H1AB H 0.0155 0.4560 -0.0146 0.159 Uiso 0.477 1 calc R U P A 2
H1AC H -0.0267 0.4444 0.0203 0.159 Uiso 0.477 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.125(6) . ?
Fe1 O1 2.125(6) 2_565 ?
Fe1 N2 2.137(7) . ?
Fe1 N2 2.138(7) 2_565 ?
Fe1 N1 2.141(8) 2_565 ?
Fe1 N1 2.141(8) . ?
N2 C16 1.258(12) . ?
N2 N3 1.355(10) . ?
N3 C15 1.378(12) . ?
N3 C8 1.463(12) . ?
N1 C21 1.344(15) . ?
N1 C17 1.350(15) . ?
C14 C13 1.336(16) . ?
C14 C9 1.424(14) . ?
C14 C15 1.451(12) . ?
C9 N4 1.327(16) . ?
C9 C10 1.419(16) . ?
N4 C8 1.489(15) . ?
N4 H4 0.8600 . ?
C15 O1 1.233(10) . ?
C16 C17 1.455(15) . ?
C16 H16 0.9300 . ?
C8 C7A 1.548(14) . ?
C8 C7 1.553(14) . ?
C13 C12 1.405(16) . ?
C13 H13 0.9300 . ?
C10 C11 1.39(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.33(2) . ?
C11 H11 0.9300 . ?
C17 C18 1.375(16) . ?
C12 H12 0.9300 . ?
C20 C19 1.31(2) . ?
C20 C21 1.367(19) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C18 C19 1.37(2) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
Cl1 O11 1.404(8) . ?
Cl1 O12 1.412(7) . ?
Cl1 O13 1.428(8) . ?
Cl1 O14 1.467(7) . ?
O2 C2 1.357(12) . ?
O2 C1 1.41(3) . ?
C7 C6 1.3900 . ?
C7 C2 1.3900 . ?
C6 C5 1.3900 . ?
C6 H6 0.9300 . ?
C5 C4 1.3900 . ?
C5 H5 0.9300 . ?
C4 C3 1.3900 . ?
C4 H4A 0.9300 . ?
C3 C2 1.3900 . ?
C3 H3 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8503 . ?
C7A C6A 1.3900 . ?
C7A C2A 1.3900 . ?
C6A C5A 1.3900 . ?
C6A H6A 0.9300 . ?
C5A C4A 1.3900 . ?
C5A H5A 0.9300 . ?
C4A C3A 1.3900 . ?
C4A H4AA 0.9300 . ?
C3A C2A 1.3900 . ?
C3A H3A 0.9300 . ?
C2A O2A 1.351(16) . ?
O2A C1A 1.41(3) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 91.6(3) . 2_565 ?
O1 Fe1 N2 72.5(3) . . ?
O1 Fe1 N2 91.9(2) 2_565 . ?
O1 Fe1 N2 91.9(2) . 2_565 ?
O1 Fe1 N2 72.5(3) 2_565 2_565 ?
N2 Fe1 N2 157.9(4) . 2_565 ?
O1 Fe1 N1 100.3(3) . 2_565 ?
O1 Fe1 N1 145.7(3) 2_565 2_565 ?
N2 Fe1 N1 122.3(3) . 2_565 ?
N2 Fe1 N1 75.1(3) 2_565 2_565 ?
O1 Fe1 N1 145.7(3) . . ?
O1 Fe1 N1 100.3(3) 2_565 . ?
N2 Fe1 N1 75.1(3) . . ?
N2 Fe1 N1 122.3(3) 2_565 . ?
N1 Fe1 N1 87.8(5) 2_565 . ?
C16 N2 N3 125.8(8) . . ?
C16 N2 Fe1 117.7(6) . . ?
N3 N2 Fe1 116.3(5) . . ?
N2 N3 C15 112.7(6) . . ?
N2 N3 C8 120.7(8) . . ?
C15 N3 C8 125.9(7) . . ?
C21 N1 C17 118.1(10) . . ?
C21 N1 Fe1 127.7(9) . . ?
C17 N1 Fe1 114.1(6) . . ?
C13 C14 C9 120.1(9) . . ?
C13 C14 C15 122.6(9) . . ?
C9 C14 C15 117.3(10) . . ?
N4 C9 C10 121.2(9) . . ?
N4 C9 C14 120.7(9) . . ?
C10 C9 C14 118.0(12) . . ?
C9 N4 C8 125.4(8) . . ?
C9 N4 H4 117.3 . . ?
C8 N4 H4 117.3 . . ?
O1 C15 N3 119.8(7) . . ?
O1 C15 C14 121.7(8) . . ?
N3 C15 C14 118.5(7) . . ?
N2 C16 C17 116.2(9) . . ?
N2 C16 H16 121.9 . . ?
C17 C16 H16 121.9 . . ?
N3 C8 N4 107.1(8) . . ?
N3 C8 C7A 109.8(11) . . ?
N4 C8 C7A 111.1(12) . . ?
N3 C8 C7 115.3(11) . . ?
N4 C8 C7 121.5(12) . . ?
C14 C13 C12 122.0(12) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C11 C10 C9 118.3(10) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C15 O1 Fe1 117.8(5) . . ?
C12 C11 C10 123.0(11) . . ?
C12 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
N1 C17 C18 121.1(12) . . ?
N1 C17 C16 116.2(8) . . ?
C18 C17 C16 122.7(12) . . ?
C11 C12 C13 118.4(13) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C19 C20 C21 118.3(14) . . ?
C19 C20 H20 120.8 . . ?
C21 C20 H20 120.8 . . ?
N1 C21 C20 122.2(14) . . ?
N1 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
C19 C18 C17 117.5(15) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C20 C19 C18 122.6(14) . . ?
C20 C19 H19 118.7 . . ?
C18 C19 H19 118.7 . . ?
O11 Cl1 O12 114.1(7) . . ?
O11 Cl1 O13 110.8(6) . . ?
O12 Cl1 O13 110.9(6) . . ?
O11 Cl1 O14 108.8(7) . . ?
O12 Cl1 O14 106.6(6) . . ?
O13 Cl1 O14 105.2(6) . . ?
C2 O2 C1 110(2) . . ?
C6 C7 C2 120.0 . . ?
C6 C7 C8 125.1(12) . . ?
C2 C7 C8 114.9(12) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
O2 C2 C3 121.1(14) . . ?
O2 C2 C7 118.7(14) . . ?
C3 C2 C7 120.0 . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1WA O1W H1WB 120.0 . . ?
C6A C7A C2A 120.0 . . ?
C6A C7A C8 115.5(12) . . ?
C2A C7A C8 124.5(12) . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C3A C4A C5A 120.0 . . ?
C3A C4A H4AA 120.0 . . ?
C5A C4A H4AA 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
O2A C2A C3A 123.7(16) . . ?
O2A C2A C7A 116.2(16) . . ?
C3A C2A C7A 120.0 . . ?
C2A O2A C1A 114(2) . . ?
O2A C1A H1AA 109.5 . . ?
O2A C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
O2A C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N2 N3 C15 -178.2(7) . . . . ?
Fe1 N2 N3 C15 6.3(8) . . . . ?
C16 N2 N3 C8 10.9(11) . . . . ?
Fe1 N2 N3 C8 -164.6(6) . . . . ?
C13 C14 C9 N4 179.1(10) . . . . ?
C15 C14 C9 N4 -0.6(12) . . . . ?
C13 C14 C9 C10 2.4(13) . . . . ?
C15 C14 C9 C10 -177.4(8) . . . . ?
C10 C9 N4 C8 -166.4(9) . . . . ?
C14 C9 N4 C8 16.9(14) . . . . ?
N2 N3 C15 O1 1.1(10) . . . . ?
C8 N3 C15 O1 171.4(8) . . . . ?
N2 N3 C15 C14 178.9(6) . . . . ?
C8 N3 C15 C14 -10.8(12) . . . . ?
C13 C14 C15 O1 -4.3(13) . . . . ?
C9 C14 C15 O1 175.4(8) . . . . ?
C13 C14 C15 N3 177.9(9) . . . . ?
C9 C14 C15 N3 -2.4(11) . . . . ?
N3 N2 C16 C17 177.3(7) . . . . ?
Fe1 N2 C16 C17 -7.2(9) . . . . ?
N2 N3 C8 N4 -167.5(7) . . . . ?
C15 N3 C8 N4 22.9(11) . . . . ?
N2 N3 C8 C7A 71.8(13) . . . . ?
C15 N3 C8 C7A -97.8(13) . . . . ?
N2 N3 C8 C7 53.9(13) . . . . ?
C15 N3 C8 C7 -115.6(12) . . . . ?
C9 N4 C8 N3 -26.2(12) . . . . ?
C9 N4 C8 C7A 93.6(13) . . . . ?
C9 N4 C8 C7 109.3(14) . . . . ?
C9 C14 C13 C12 -3.0(16) . . . . ?
C15 C14 C13 C12 176.7(10) . . . . ?
N4 C9 C10 C11 -178.8(10) . . . . ?
C14 C9 C10 C11 -2.0(14) . . . . ?
N3 C15 O1 Fe1 -8.0(10) . . . . ?
C14 C15 O1 Fe1 174.2(5) . . . . ?
C9 C10 C11 C12 2.5(18) . . . . ?
C21 N1 C17 C18 2.6(14) . . . . ?
Fe1 N1 C17 C18 -174.3(8) . . . . ?
C21 N1 C17 C16 -177.5(9) . . . . ?
Fe1 N1 C17 C16 5.6(10) . . . . ?
N2 C16 C17 N1 0.9(12) . . . . ?
N2 C16 C17 C18 -179.1(9) . . . . ?
C10 C11 C12 C13 -3(2) . . . . ?
C14 C13 C12 C11 3(2) . . . . ?
C17 N1 C21 C20 -1.5(16) . . . . ?
Fe1 N1 C21 C20 174.9(9) . . . . ?
C19 C20 C21 N1 -2(2) . . . . ?
N1 C17 C18 C19 -0.7(18) . . . . ?
C16 C17 C18 C19 179.4(11) . . . . ?
C21 C20 C19 C18 4(2) . . . . ?
C17 C18 C19 C20 -3(2) . . . . ?
N3 C8 C7 C6 -115.6(15) . . . . ?
N4 C8 C7 C6 112.3(16) . . . . ?
N3 C8 C7 C2 65.8(16) . . . . ?
N4 C8 C7 C2 -66.3(16) . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C8 C7 C6 C5 -178(2) . . . . ?
C7 C6 C5 C4 0.0 . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C1 O2 C2 C3 5(3) . . . . ?
C1 O2 C2 C7 -180(2) . . . . ?
C4 C3 C2 O2 176(2) . . . . ?
C4 C3 C2 C7 0.0 . . . . ?
C6 C7 C2 O2 -176(2) . . . . ?
C8 C7 C2 O2 3(2) . . . . ?
C6 C7 C2 C3 0.0 . . . . ?
C8 C7 C2 C3 178.6(19) . . . . ?
N3 C8 C7A C6A -128.2(13) . . . . ?
N4 C8 C7A C6A 113.5(14) . . . . ?
N3 C8 C7A C2A 51.9(19) . . . . ?
N4 C8 C7A C2A -66.3(17) . . . . ?
C2A C7A C6A C5A 0.0 . . . . ?
C8 C7A C6A C5A -180(2) . . . . ?
C7A C6A C5A C4A 0.0 . . . . ?
C6A C5A C4A C3A 0.0 . . . . ?
C5A C4A C3A C2A 0.0 . . . . ?
C4A C3A C2A O2A 177(3) . . . . ?
C4A C3A C2A C7A 0.0 . . . . ?
C6A C7A C2A O2A -177(2) . . . . ?
C8 C7A C2A O2A 3(2) . . . . ?
C6A C7A C2A C3A 0.0 . . . . ?
C8 C7A C2A C3A 180(2) . . . . ?
C3A C2A O2A C1A -3(3) . . . . ?
C7A C2A O2A C1A 174(2) . . . . ?

_refine_diff_density_max         0.741
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.124

####################################################################### 
# 
# 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_5-296K
_database_code_depnum_ccdc_archive 'CCDC 1400833'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H34 Fe N8 O4, 2(Cl O4)'
_chemical_formula_sum            'C42 H34 Cl2 Fe N8 O12'
_chemical_formula_weight         969.52

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'
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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'

_cell_length_a                   32.579(10)
_cell_length_b                   17.101(4)
_cell_length_c                   18.604(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10365(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1406
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      16.70

_exptl_crystal_description       block
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_F_000             3984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.455
_shelx_estimated_absorpt_T_min   0.861
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16152
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.734
_diffrn_reflns_theta_max         27.674
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_point_group_measured_fraction_full 0.796
_reflns_number_total             4609
_reflns_number_gt                1951
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.498
_reflns_Friedel_fraction_max     0.521
_reflns_Friedel_fraction_full    0.578

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
methoxyl group is disorder in the structure,
we treated these problem with some restraints. R1 and wR2 
are high, for the poor crystal quality of this series of crystal. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1740P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 509 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4609
_refine_ls_number_parameters     342
_refine_ls_number_restraints     410
_refine_ls_R_factor_all          0.2022
_refine_ls_R_factor_gt           0.0958
_refine_ls_wR_factor_ref         0.3048
_refine_ls_wR_factor_gt          0.2304
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.46570(14) 0.0660(7) Uani 1 2 d S T P . .
C7 C -0.0232(6) 0.7268(13) 0.3119(14) 0.106(4) Uani 0.6115 1 d DG U P A 1
C3 C -0.0142(6) 0.8045(12) 0.3273(12) 0.116(4) Uani 0.6115 1 d DG U P A 1
H3 H -0.0314 0.8331 0.3573 0.140 Uiso 0.6115 1 calc R U P A 1
C2 C 0.0204(6) 0.8394(9) 0.2977(13) 0.128(4) Uani 0.6115 1 d DG U P A 1
C4 C 0.0461(5) 0.7966(12) 0.2528(13) 0.124(4) Uani 0.6115 1 d DG U P A 1
H4 H 0.0693 0.8200 0.2331 0.148 Uiso 0.6115 1 calc R U P A 1
C5 C 0.0371(5) 0.7190(11) 0.2374(12) 0.117(4) Uani 0.6115 1 d DG U P A 1
H5 H 0.0543 0.6903 0.2074 0.140 Uiso 0.6115 1 calc R U P A 1
C6 C 0.0024(6) 0.6841(9) 0.2670(13) 0.109(4) Uani 0.6115 1 d G U P A 1
H6 H -0.0036 0.6321 0.2567 0.131 Uiso 0.6115 1 calc R U P A 1
C8 C -0.0597(4) 0.6925(8) 0.3492(8) 0.080(4) Uani 1 1 d D . . . .
C9 C -0.1046(4) 0.6142(10) 0.2712(7) 0.075(4) Uani 1 1 d . . . . .
C10 C -0.1330(4) 0.6121(10) 0.2140(9) 0.103(4) Uani 1 1 d D U . . .
H10 H -0.1441 0.6584 0.1962 0.124 Uiso 1 1 calc R U . . .
C11 C -0.1441(5) 0.5424(9) 0.1849(10) 0.126(6) Uani 1 1 d D U . . .
H11 H -0.1632 0.5413 0.1477 0.152 Uiso 1 1 calc R U . . .
C12 C -0.1278(5) 0.4739(11) 0.2094(10) 0.127(6) Uani 1 1 d D . . . .
H12 H -0.1358 0.4269 0.1885 0.152 Uiso 1 1 calc R U . . .
C13 C -0.0998(5) 0.4734(11) 0.2642(8) 0.107(5) Uani 1 1 d D . . . .
H13 H -0.0891 0.4267 0.2815 0.129 Uiso 1 1 calc R U . . .
C14 C -0.0875(4) 0.5458(9) 0.2940(7) 0.077(3) Uani 1 1 d . . . . .
C15 C -0.0596(3) 0.5432(8) 0.3547(6) 0.062(3) Uani 1 1 d . . . . .
C16 C -0.0109(3) 0.6725(8) 0.4739(8) 0.079(3) Uani 1 1 d . . . . .
H16 H -0.0172 0.7235 0.4609 0.095 Uiso 1 1 calc R U . . .
C17 C 0.0154(4) 0.6520(9) 0.5372(8) 0.084(4) Uani 1 1 d . U . . .
C18 C 0.0303(5) 0.7120(10) 0.5788(9) 0.109(5) Uani 1 1 d D U . . .
H18 H 0.0241 0.7639 0.5684 0.131 Uiso 1 1 calc R U . . .
C19 C 0.0544(5) 0.6927(11) 0.6358(10) 0.121(5) Uani 1 1 d D U . . .
H19 H 0.0647 0.7309 0.6664 0.145 Uiso 1 1 calc R U . . .
C20 C 0.0627(5) 0.6164(10) 0.6465(10) 0.114(5) Uani 1 1 d D U . . .
H20 H 0.0795 0.6009 0.6843 0.137 Uiso 1 1 calc R U . . .
C21 C 0.0464(5) 0.5625(10) 0.6015(9) 0.106(5) Uani 1 1 d D U . . .
H21 H 0.0521 0.5101 0.6107 0.127 Uiso 1 1 calc R U . . .
N1 N 0.0232(3) 0.5789(8) 0.5458(6) 0.080(3) Uani 1 1 d . . . . .
N2 N -0.0237(3) 0.6121(6) 0.4397(5) 0.068(3) Uani 1 1 d . . . . .
N3 N -0.0498(3) 0.6142(6) 0.3833(6) 0.073(3) Uani 1 1 d . . . . .
N4 N -0.0939(3) 0.6815(8) 0.3017(7) 0.088(3) Uani 1 1 d . . . . .
H4A H -0.1087 0.7218 0.2921 0.106 Uiso 1 1 calc R U . . .
Cl1 Cl -0.11049(13) 0.6304(3) 0.5592(3) 0.1097(14) Uani 1 1 d . U . . .
O1 O -0.0468(2) 0.4848(5) 0.3846(5) 0.071(2) Uani 1 1 d . . . . .
O14 O -0.1068(4) 0.5662(7) 0.5094(7) 0.126(4) Uani 1 1 d . U . . .
O13 O -0.1426(6) 0.6228(12) 0.6035(11) 0.211(8) Uani 1 1 d . U . . .
O12 O -0.0752(6) 0.6308(11) 0.6006(9) 0.185(7) Uani 1 1 d . U . . .
O11 O -0.1072(5) 0.7008(9) 0.5152(11) 0.168(5) Uani 1 1 d . U . . .
O2 O 0.0257(7) 0.9147(10) 0.3175(13) 0.145(5) Uani 0.6115 1 d D U P A 1
C1A C 0.0637(10) 0.945(2) 0.275(2) 0.167(8) Uani 0.6115 1 d D U P A 1
H1AA H 0.0689 0.9983 0.2869 0.251 Uiso 0.6115 1 calc R U P A 1
H1AB H 0.0873 0.9136 0.2869 0.251 Uiso 0.6115 1 calc R U P A 1
H1AC H 0.0584 0.9405 0.2241 0.251 Uiso 0.6115 1 calc R U P A 1
C1B C 0.1008(12) 0.862(4) 0.274(4) 0.172(11) Uani 0.3885 1 d D U P A 2
H1BA H 0.1156 0.9102 0.2820 0.258 Uiso 0.3885 1 calc R U P A 2
H1BB H 0.1127 0.8215 0.3026 0.258 Uiso 0.3885 1 calc R U P A 2
H1BC H 0.1024 0.8486 0.2241 0.258 Uiso 0.3885 1 calc R U P A 2
O2A O 0.0546(10) 0.8740(17) 0.296(2) 0.140(5) Uani 0.3885 1 d D U P A 2
C7A C -0.0220(9) 0.715(2) 0.307(2) 0.107(4) Uani 0.3885 1 d DG U P A 2
C3A C -0.0032(10) 0.7854(19) 0.3240(18) 0.116(4) Uani 0.3885 1 d G U P A 2
H3A H -0.0139 0.8168 0.3603 0.140 Uiso 0.3885 1 calc R U P A 2
C2A C 0.0315(9) 0.8091(17) 0.2866(19) 0.125(4) Uani 0.3885 1 d DG U P A 2
C4A C 0.0475(8) 0.7622(19) 0.2324(19) 0.118(5) Uani 0.3885 1 d G U P A 2
H4AA H 0.0708 0.7781 0.2073 0.142 Uiso 0.3885 1 calc R U P A 2
C5A C 0.0287(9) 0.6915(17) 0.2156(17) 0.115(5) Uani 0.3885 1 d G U P A 2
H5A H 0.0394 0.6601 0.1793 0.138 Uiso 0.3885 1 calc R U P A 2
C6A C -0.0060(9) 0.6678(16) 0.253(2) 0.111(4) Uani 0.3885 1 d G U P A 2
H6A H -0.0186 0.6205 0.2417 0.133 Uiso 0.3885 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.123(10) 2_565 ?
Fe1 N2 2.123(10) . ?
Fe1 N1 2.148(11) . ?
Fe1 N1 2.148(11) 2_565 ?
Fe1 O1 2.160(8) 2_565 ?
Fe1 O1 2.160(8) . ?
C7 C3 1.3900 . ?
C7 C6 1.3900 . ?
C7 C8 1.496(16) . ?
C3 C2 1.3900 . ?
C3 H3 0.9300 . ?
C2 O2 1.350(11) . ?
C2 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 N4 1.435(16) . ?
C8 C7A 1.504(18) . ?
C8 N3 1.517(16) . ?
C9 N4 1.328(18) . ?
C9 C14 1.363(19) . ?
C9 C10 1.41(2) . ?
C10 C11 1.359(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.370(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.41(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.451(16) . ?
C15 O1 1.217(13) . ?
C15 N3 1.363(15) . ?
C16 N2 1.284(15) . ?
C16 C17 1.50(2) . ?
C16 H16 0.9300 . ?
C17 N1 1.285(17) . ?
C17 C18 1.37(2) . ?
C18 C19 1.359(13) . ?
C18 H18 0.9300 . ?
C19 C20 1.349(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.353(13) . ?
C20 H20 0.9300 . ?
C21 N1 1.315(18) . ?
C21 H21 0.9300 . ?
N2 N3 1.350(14) . ?
N4 H4A 0.8600 . ?
Cl1 O13 1.338(15) . ?
Cl1 O12 1.384(15) . ?
Cl1 O14 1.442(13) . ?
Cl1 O11 1.459(18) . ?
O2 C1A 1.560(12) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C1B O2A 1.574(17) . ?
C1B H1BA 0.9600 . ?
C1B H1BB 0.9600 . ?
C1B H1BC 0.9600 . ?
O2A C2A 1.352(16) . ?
C7A C3A 1.3900 . ?
C7A C6A 1.3900 . ?
C3A C2A 1.3900 . ?
C3A H3A 0.9300 . ?
C2A C4A 1.3900 . ?
C4A C5A 1.3900 . ?
C4A H4AA 0.9300 . ?
C5A C6A 1.3900 . ?
C5A H5A 0.9300 . ?
C6A H6A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 153.6(5) 2_565 . ?
N2 Fe1 N1 126.7(4) 2_565 . ?
N2 Fe1 N1 73.7(4) . . ?
N2 Fe1 N1 73.7(4) 2_565 2_565 ?
N2 Fe1 N1 126.7(4) . 2_565 ?
N1 Fe1 N1 92.2(7) . 2_565 ?
N2 Fe1 O1 72.1(4) 2_565 2_565 ?
N2 Fe1 O1 89.4(3) . 2_565 ?
N1 Fe1 O1 99.3(4) . 2_565 ?
N1 Fe1 O1 143.9(4) 2_565 2_565 ?
N2 Fe1 O1 89.4(3) 2_565 . ?
N2 Fe1 O1 72.1(4) . . ?
N1 Fe1 O1 143.9(4) . . ?
N1 Fe1 O1 99.3(4) 2_565 . ?
O1 Fe1 O1 91.4(4) 2_565 . ?
C3 C7 C6 120.0 . . ?
C3 C7 C8 116.5(15) . . ?
C6 C7 C8 123.4(15) . . ?
C2 C3 C7 120.0 . . ?
C2 C3 H3 120.0 . . ?
C7 C3 H3 120.0 . . ?
O2 C2 C3 113.9(17) . . ?
O2 C2 C4 126.1(17) . . ?
C3 C2 C4 120.0 . . ?
C5 C4 C2 120.0 . . ?
C5 C4 H4 120.0 . . ?
C2 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
N4 C8 C7 112.5(15) . . ?
N4 C8 C7A 110(2) . . ?
N4 C8 N3 107.9(10) . . ?
C7 C8 N3 111.8(14) . . ?
C7A C8 N3 105.5(18) . . ?
N4 C9 C14 120.3(12) . . ?
N4 C9 C10 121.0(13) . . ?
C14 C9 C10 118.7(15) . . ?
C11 C10 C9 119.8(14) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 121.1(15) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C13 120.9(17) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C13 C14 118.4(17) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C9 C14 C13 121.0(13) . . ?
C9 C14 C15 121.5(14) . . ?
C13 C14 C15 117.1(13) . . ?
O1 C15 N3 118.1(10) . . ?
O1 C15 C14 126.6(12) . . ?
N3 C15 C14 115.1(12) . . ?
N2 C16 C17 112.9(13) . . ?
N2 C16 H16 123.5 . . ?
C17 C16 H16 123.5 . . ?
N1 C17 C18 125.9(15) . . ?
N1 C17 C16 116.0(12) . . ?
C18 C17 C16 118.1(15) . . ?
C19 C18 C17 117.5(16) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C20 C19 C18 117.8(16) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?
C19 C20 C21 119.3(16) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
N1 C21 C20 124.6(16) . . ?
N1 C21 H21 117.7 . . ?
C20 C21 H21 117.7 . . ?
C17 N1 C21 114.9(12) . . ?
C17 N1 Fe1 117.1(9) . . ?
C21 N1 Fe1 127.9(11) . . ?
C16 N2 N3 124.8(11) . . ?
C16 N2 Fe1 119.6(9) . . ?
N3 N2 Fe1 115.5(8) . . ?
N2 N3 C15 115.3(9) . . ?
N2 N3 C8 118.8(10) . . ?
C15 N3 C8 125.0(11) . . ?
C9 N4 C8 125.4(11) . . ?
C9 N4 H4A 117.3 . . ?
C8 N4 H4A 117.3 . . ?
O13 Cl1 O12 107.8(13) . . ?
O13 Cl1 O14 112.8(10) . . ?
O12 Cl1 O14 107.0(10) . . ?
O13 Cl1 O11 119.0(12) . . ?
O12 Cl1 O11 104.3(10) . . ?
O14 Cl1 O11 105.2(10) . . ?
C15 O1 Fe1 117.6(7) . . ?
C2 O2 C1A 106(2) . . ?
O2 C1A H1AA 109.5 . . ?
O2 C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
O2 C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
O2A C1B H1BA 109.5 . . ?
O2A C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
O2A C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C2A O2A C1B 113(4) . . ?
C3A C7A C6A 120.0 . . ?
C3A C7A C8 118(2) . . ?
C6A C7A C8 122(2) . . ?
C7A C3A C2A 120.0 . . ?
C7A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
O2A C2A C3A 129(3) . . ?
O2A C2A C4A 111(3) . . ?
C3A C2A C4A 120.0 . . ?
C5A C4A C2A 120.0 . . ?
C5A C4A H4AA 120.0 . . ?
C2A C4A H4AA 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C5A C6A C7A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C7A C6A H6A 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C7 C3 C2 0.0 . . . . ?
C8 C7 C3 C2 177(2) . . . . ?
C7 C3 C2 O2 -179(2) . . . . ?
C7 C3 C2 C4 0.0 . . . . ?
O2 C2 C4 C5 179(2) . . . . ?
C3 C2 C4 C5 0.0 . . . . ?
C2 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C3 C7 C6 C5 0.0 . . . . ?
C8 C7 C6 C5 -176(3) . . . . ?
C3 C7 C8 N4 107.2(16) . . . . ?
C6 C7 C8 N4 -76(2) . . . . ?
C3 C7 C8 N3 -131.2(14) . . . . ?
C6 C7 C8 N3 45(2) . . . . ?
N4 C9 C10 C11 -178.5(15) . . . . ?
C14 C9 C10 C11 3(2) . . . . ?
C9 C10 C11 C12 -1(3) . . . . ?
C10 C11 C12 C13 0(3) . . . . ?
C11 C12 C13 C14 -1(3) . . . . ?
N4 C9 C14 C13 177.3(13) . . . . ?
C10 C9 C14 C13 -4(2) . . . . ?
N4 C9 C14 C15 4.4(19) . . . . ?
C10 C9 C14 C15 -176.9(12) . . . . ?
C12 C13 C14 C9 3(2) . . . . ?
C12 C13 C14 C15 176.5(14) . . . . ?
C9 C14 C15 O1 170.3(12) . . . . ?
C13 C14 C15 O1 -2.9(19) . . . . ?
C9 C14 C15 N3 -4.5(17) . . . . ?
C13 C14 C15 N3 -177.7(12) . . . . ?
N2 C16 C17 N1 3.8(17) . . . . ?
N2 C16 C17 C18 -178.8(13) . . . . ?
N1 C17 C18 C19 -2(3) . . . . ?
C16 C17 C18 C19 -179.5(15) . . . . ?
C17 C18 C19 C20 2(3) . . . . ?
C18 C19 C20 C21 -1(3) . . . . ?
C19 C20 C21 N1 2(3) . . . . ?
C18 C17 N1 C21 2(2) . . . . ?
C16 C17 N1 C21 179.7(12) . . . . ?
C18 C17 N1 Fe1 -174.2(13) . . . . ?
C16 C17 N1 Fe1 3.0(15) . . . . ?
C20 C21 N1 C17 -2(2) . . . . ?
C20 C21 N1 Fe1 174.2(13) . . . . ?
C17 C16 N2 N3 175.9(10) . . . . ?
C17 C16 N2 Fe1 -9.0(13) . . . . ?
C16 N2 N3 C15 -179.8(11) . . . . ?
Fe1 N2 N3 C15 4.9(12) . . . . ?
C16 N2 N3 C8 10.5(16) . . . . ?
Fe1 N2 N3 C8 -164.7(8) . . . . ?
O1 C15 N3 N2 5.0(15) . . . . ?
C14 C15 N3 N2 -179.7(10) . . . . ?
O1 C15 N3 C8 173.9(10) . . . . ?
C14 C15 N3 C8 -10.8(16) . . . . ?
N4 C8 N3 N2 -168.1(10) . . . . ?
C7 C8 N3 N2 67.8(18) . . . . ?
C7A C8 N3 N2 74(2) . . . . ?
N4 C8 N3 C15 23.4(16) . . . . ?
C7 C8 N3 C15 -100.8(16) . . . . ?
C7A C8 N3 C15 -94(2) . . . . ?
C14 C9 N4 C8 12(2) . . . . ?
C10 C9 N4 C8 -166.5(12) . . . . ?
C7 C8 N4 C9 99.8(16) . . . . ?
C7A C8 N4 C9 91(2) . . . . ?
N3 C8 N4 C9 -23.9(17) . . . . ?
N3 C15 O1 Fe1 -12.4(14) . . . . ?
C14 C15 O1 Fe1 172.9(9) . . . . ?
C3 C2 O2 C1A -176(2) . . . . ?
C4 C2 O2 C1A 5(3) . . . . ?
N4 C8 C7A C3A 121(2) . . . . ?
N3 C8 C7A C3A -122(2) . . . . ?
N4 C8 C7A C6A -58(3) . . . . ?
N3 C8 C7A C6A 58(3) . . . . ?
C6A C7A C3A C2A 0.0 . . . . ?
C8 C7A C3A C2A -180(4) . . . . ?
C1B O2A C2A C3A 151(4) . . . . ?
C1B O2A C2A C4A -27(5) . . . . ?
C7A C3A C2A O2A -178(4) . . . . ?
C7A C3A C2A C4A 0.0 . . . . ?
O2A C2A C4A C5A 178(4) . . . . ?
C3A C2A C4A C5A 0.0 . . . . ?
C2A C4A C5A C6A 0.0 . . . . ?
C4A C5A C6A C7A 0.0 . . . . ?
C3A C7A C6A C5A 0.0 . . . . ?
C8 C7A C6A C5A 180(4) . . . . ?

_refine_diff_density_max         0.514
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.112


# start Validation Reply Form
_vrf_PLAT601_5-296K              
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        268 Ang3  
RESPONSE: This structure lose its long-range ordering 
when solvent molecules leave the crystal.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-120K
_database_code_depnum_ccdc_archive 'CCDC 1449552'
_audit_update_record             
;
2016-02-20 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 Fe N10 O2, 2(Cl O4)'
_chemical_formula_sum            'C38 H30 Cl2 Fe N10 O10'
_chemical_formula_weight         913.47

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.988(4)
_cell_length_b                   12.347(4)
_cell_length_c                   18.255(5)
_cell_angle_alpha                72.264(7)
_cell_angle_beta                 74.636(7)
_cell_angle_gamma                86.982(8)
_cell_volume                     2480.4(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    902
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      19.20

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.469
_shelx_estimated_absorpt_T_min   0.888
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13444
_diffrn_reflns_av_unetI/netI     0.1695
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.732
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             8546
_reflns_number_gt                3961
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
There are partial occupancy water and solvent molecules in 
the structure,and ClO4 is disorder, so some restraints have 
been used to treat these problems.This crystal data is treated 
with squeeze.
We made several attempts to obtain better quality data for 
this structure however, due to disorder, poor crystal 
quality etc. the R1 and wR2 value are high. We are confidant 
the structural characterization is valid.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²+9.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8546
_refine_ls_number_parameters     500
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.1070
_refine_ls_wR_factor_ref         0.2631
_refine_ls_wR_factor_gt          0.2343
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.19275(10) 0.49540(10) 0.22995(6) 0.0300(3) Uani 1 1 d . . . . .
C1 C -0.2148(7) 0.5966(8) 0.3312(4) 0.042(2) Uani 1 1 d . . . . .
H1A H -0.2062 0.5205 0.3334 0.050 Uiso 1 1 calc R U . . .
C2 C -0.3242(8) 0.6397(10) 0.3469(5) 0.052(3) Uani 1 1 d . . . . .
H2A H -0.3893 0.5923 0.3617 0.063 Uiso 1 1 calc R U . . .
C3 C -0.3364(8) 0.7538(10) 0.3406(5) 0.055(3) Uani 1 1 d . . . . .
H3A H -0.4100 0.7838 0.3476 0.065 Uiso 1 1 calc R U . . .
C4 C -0.2421(8) 0.8235(9) 0.3241(5) 0.056(3) Uani 1 1 d . . . . .
H4A H -0.2521 0.8996 0.3216 0.067 Uiso 1 1 calc R U . . .
C5 C -0.1289(7) 0.7799(8) 0.3107(4) 0.039(2) Uani 1 1 d . . . . .
C6 C -0.1172(6) 0.6664(7) 0.3123(4) 0.034(2) Uani 1 1 d . . . . .
C7 C -0.0032(7) 0.6259(7) 0.2881(4) 0.0304(18) Uani 1 1 d . . . . .
C8 C 0.0758(7) 0.7588(8) 0.3939(5) 0.038(2) Uani 1 1 d . . . . .
C9 C 0.0817(9) 0.8439(8) 0.4280(5) 0.056(3) Uani 1 1 d . . . . .
H9A H 0.0863 0.9206 0.3989 0.067 Uiso 1 1 calc R U . . .
C10 C 0.0803(10) 0.8080(10) 0.5075(6) 0.073(3) Uani 1 1 d . . . . .
H10A H 0.0857 0.8610 0.5334 0.088 Uiso 1 1 calc R U . . .
C11 C 0.0711(8) 0.6960(9) 0.5477(5) 0.052(3) Uani 1 1 d . . . . .
H11A H 0.0678 0.6719 0.6017 0.062 Uiso 1 1 calc R U . . .
C12 C 0.0668(8) 0.6190(9) 0.5099(5) 0.053(3) Uani 1 1 d . . . . .
H12A H 0.0624 0.5422 0.5384 0.064 Uiso 1 1 calc R U . . .
C13 C 0.0730(7) 0.7967(7) 0.3050(5) 0.041(2) Uani 1 1 d . . . . .
H13A H 0.1369 0.8518 0.2738 0.049 Uiso 1 1 calc R U . . .
C14 C 0.2896(6) 0.6944(7) 0.2528(4) 0.0320(19) Uani 1 1 d . . . . .
H14A H 0.2926 0.7567 0.2708 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3936(7) 0.6376(7) 0.2227(4) 0.0333(19) Uani 1 1 d . . . . .
C16 C 0.5019(7) 0.6820(8) 0.2109(5) 0.046(2) Uani 1 1 d . . . . .
H16A H 0.5116 0.7483 0.2229 0.056 Uiso 1 1 calc R U . . .
C17 C 0.5958(7) 0.6245(8) 0.1803(5) 0.049(2) Uani 1 1 d . . . . .
H17A H 0.6707 0.6508 0.1722 0.059 Uiso 1 1 calc R U . . .
C18 C 0.5774(7) 0.5285(9) 0.1621(5) 0.049(2) Uani 1 1 d . . . . .
H18A H 0.6396 0.4898 0.1402 0.058 Uiso 1 1 calc R U . . .
C19 C 0.4651(7) 0.4898(8) 0.1767(4) 0.041(2) Uani 1 1 d . . . . .
H19A H 0.4535 0.4233 0.1655 0.049 Uiso 1 1 calc R U . . .
C20 C 0.2187(7) 0.3778(8) 0.4039(5) 0.044(2) Uani 1 1 d . . . . .
H20A H 0.2143 0.4505 0.4092 0.053 Uiso 1 1 calc R U . . .
C21 C 0.2320(9) 0.2865(10) 0.4681(6) 0.059(3) Uani 1 1 d . . . . .
H21A H 0.2396 0.2988 0.5143 0.071 Uiso 1 1 calc R U . . .
C22 C 0.2339(8) 0.1800(10) 0.4622(6) 0.059(3) Uani 1 1 d . . . . .
H22A H 0.2376 0.1181 0.5058 0.071 Uiso 1 1 calc R U . . .
C23 C 0.2303(8) 0.1628(8) 0.3910(6) 0.054(3) Uani 1 1 d . . . . .
H23A H 0.2360 0.0902 0.3852 0.065 Uiso 1 1 calc R U . . .
C24 C 0.2181(7) 0.2563(8) 0.3293(5) 0.043(2) Uani 1 1 d . . . . .
C25 C 0.2100(7) 0.2491(8) 0.2506(5) 0.038(2) Uani 1 1 d . . . . .
H25A H 0.2159 0.1812 0.2380 0.045 Uiso 1 1 calc R U . . .
C26 C 0.1782(6) 0.4630(7) 0.0834(4) 0.0306(19) Uani 1 1 d . . . . .
C27 C 0.1425(7) 0.3907(9) -0.0197(5) 0.044(2) Uani 1 1 d . . . . .
C28 C 0.1146(7) 0.4079(10) -0.0928(5) 0.051(3) Uani 1 1 d . . . . .
H28A H 0.0986 0.3463 -0.1080 0.061 Uiso 1 1 calc R U . . .
C29 C 0.1113(8) 0.5173(11) -0.1410(6) 0.062(3) Uani 1 1 d . . . . .
H29A H 0.0940 0.5296 -0.1896 0.075 Uiso 1 1 calc R U . . .
C30 C 0.1336(7) 0.6102(11) -0.1180(5) 0.065(3) Uani 1 1 d . . . . .
H30A H 0.1317 0.6839 -0.1510 0.078 Uiso 1 1 calc R U . . .
C31 C 0.1591(7) 0.5910(9) -0.0441(5) 0.047(2) Uani 1 1 d . . . . .
H31A H 0.1730 0.6521 -0.0277 0.056 Uiso 1 1 calc R U . . .
C32 C 0.1634(6) 0.4824(8) 0.0032(5) 0.036(2) Uani 1 1 d . . . . .
C33 C 0.3422(7) 0.2613(7) 0.0533(4) 0.035(2) Uani 1 1 d . . . . .
C34 C 0.5202(8) 0.3488(8) 0.0175(5) 0.046(2) Uani 1 1 d . . . . .
H34A H 0.5663 0.4081 0.0162 0.056 Uiso 1 1 calc R U . . .
C35 C 0.5727(8) 0.2679(8) -0.0153(5) 0.044(2) Uani 1 1 d . . . . .
H35A H 0.6521 0.2724 -0.0382 0.053 Uiso 1 1 calc R U . . .
C36 C 0.5064(9) 0.1791(8) -0.0143(5) 0.052(2) Uani 1 1 d . . . . .
H36A H 0.5401 0.1234 -0.0371 0.062 Uiso 1 1 calc R U . . .
C37 C 0.3876(7) 0.1748(7) 0.0216(5) 0.040(2) Uani 1 1 d . . . . .
H37A H 0.3404 0.1156 0.0242 0.047 Uiso 1 1 calc R U . . .
C38 C 0.2104(7) 0.2616(7) 0.0898(5) 0.036(2) Uani 1 1 d . . . . .
H38A H 0.1851 0.1881 0.1301 0.043 Uiso 1 1 calc R U . . .
N1 N -0.0329(6) 0.8466(6) 0.2926(4) 0.0441(18) Uani 1 1 d . . . . .
H1B H -0.0361 0.9192 0.2736 0.053 Uiso 1 1 calc R U . . .
N2 N 0.0686(6) 0.6494(6) 0.4309(4) 0.0394(17) Uani 1 1 d . . . . .
N3 N 0.0882(5) 0.6963(5) 0.2750(3) 0.0300(15) Uani 1 1 d . . . . .
N4 N 0.3748(5) 0.5423(6) 0.2055(3) 0.0326(16) Uani 1 1 d . . . . .
N5 N 0.1924(5) 0.6524(5) 0.2529(3) 0.0296(15) Uani 1 1 d . . . . .
N6 N 0.1461(5) 0.2821(7) 0.0298(4) 0.0442(19) Uani 1 1 d . . . . .
H6A H 0.1107 0.2267 0.0252 0.053 Uiso 1 1 calc R U . . .
N7 N 0.4053(6) 0.3488(6) 0.0521(4) 0.0414(18) Uani 1 1 d . . . . .
N8 N 0.1829(6) 0.3515(6) 0.1271(4) 0.0353(16) Uani 1 1 d . . . . .
N9 N 0.1945(5) 0.3436(6) 0.2026(4) 0.0345(16) Uani 1 1 d . . . . .
N10 N 0.2119(5) 0.3649(6) 0.3345(3) 0.0357(17) Uani 1 1 d . . . . .
Cl1 Cl -0.3906(2) 2.0070(2) 0.77608(16) 0.0647(7) Uiso 1 1 d . . . . .
O1 O 0.0150(4) 0.5303(5) 0.2773(3) 0.0339(13) Uani 1 1 d . . . . .
Cl2 Cl 0.0942(2) 0.8682(2) 0.70038(15) 0.0633(7) Uiso 1 1 d D . . . .
O2 O 0.1812(4) 0.5424(4) 0.1112(3) 0.0312(12) Uani 1 1 d . . . . .
O11 O -0.4324(6) 1.8949(6) 0.7865(4) 0.074(2) Uiso 1 1 d . . . . .
O12 O -0.2763(8) 1.9980(7) 0.7831(5) 0.102(3) Uiso 1 1 d . . . . .
O13 O -0.3955(8) 2.0880(8) 0.7029(6) 0.112(3) Uiso 1 1 d . . . . .
O14 O -0.4557(7) 2.0475(7) 0.8417(5) 0.086(2) Uiso 1 1 d . . . . .
O21 O 0.1410(8) 0.8831(7) 0.7616(4) 0.144(4) Uiso 1 1 d D . . . .
O22 O 0.0881(6) 0.7509(4) 0.7071(4) 0.072(2) Uiso 1 1 d D . . . .
O34 O 0.1668(7) 0.9307(7) 0.6249(4) 0.150(4) Uiso 1 1 d D . . . .
O33 O -0.0193(6) 0.9137(8) 0.7095(6) 0.196(6) Uiso 1 1 d 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 N9 2.079(7) . ?
Fe1 N5 2.103(6) . ?
Fe1 O2 2.108(5) . ?
Fe1 N10 2.147(7) . ?
Fe1 O1 2.151(5) . ?
Fe1 N4 2.181(6) . ?
C1 C2 1.381(12) . ?
C1 C6 1.394(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.380(13) . ?
C2 H2A 0.9300 . ?
C3 C4 1.370(13) . ?
C3 H3A 0.9300 . ?
C4 C5 1.421(11) . ?
C4 H4A 0.9300 . ?
C5 N1 1.358(11) . ?
C5 C6 1.393(12) . ?
C6 C7 1.434(10) . ?
C7 O1 1.254(9) . ?
C7 N3 1.359(9) . ?
C8 N2 1.308(10) . ?
C8 C9 1.388(11) . ?
C8 C13 1.555(11) . ?
C9 C10 1.379(13) . ?
C9 H9A 0.9300 . ?
C10 C11 1.348(13) . ?
C10 H10A 0.9300 . ?
C11 C12 1.345(12) . ?
C11 H11A 0.9300 . ?
C12 N2 1.369(10) . ?
C12 H12A 0.9300 . ?
C13 N1 1.424(10) . ?
C13 N3 1.486(9) . ?
C13 H13A 0.9800 . ?
C14 N5 1.300(9) . ?
C14 C15 1.459(10) . ?
C14 H14A 0.9300 . ?
C15 N4 1.350(10) . ?
C15 C16 1.373(11) . ?
C16 C17 1.380(12) . ?
C16 H16A 0.9300 . ?
C17 C18 1.368(12) . ?
C17 H17A 0.9300 . ?
C18 C19 1.382(12) . ?
C18 H18A 0.9300 . ?
C19 N4 1.305(9) . ?
C19 H19A 0.9300 . ?
C20 N10 1.348(9) . ?
C20 C21 1.395(12) . ?
C20 H20A 0.9300 . ?
C21 C22 1.350(14) . ?
C21 H21A 0.9300 . ?
C22 C23 1.391(13) . ?
C22 H22A 0.9300 . ?
C23 C24 1.379(12) . ?
C23 H23A 0.9300 . ?
C24 N10 1.369(10) . ?
C24 C25 1.494(11) . ?
C25 N9 1.267(10) . ?
C25 H25A 0.9300 . ?
C26 O2 1.239(8) . ?
C26 N8 1.371(10) . ?
C26 C32 1.467(10) . ?
C27 C32 1.375(11) . ?
C27 N6 1.376(11) . ?
C27 C28 1.413(12) . ?
C28 C29 1.375(14) . ?
C28 H28A 0.9300 . ?
C29 C30 1.397(15) . ?
C29 H29A 0.9300 . ?
C30 C31 1.408(11) . ?
C30 H30A 0.9300 . ?
C31 C32 1.363(12) . ?
C31 H31A 0.9300 . ?
C33 N7 1.342(10) . ?
C33 C37 1.385(10) . ?
C33 C38 1.544(11) . ?
C34 N7 1.355(10) . ?
C34 C35 1.362(11) . ?
C34 H34A 0.9300 . ?
C35 C36 1.380(12) . ?
C35 H35A 0.9300 . ?
C36 C37 1.398(12) . ?
C36 H36A 0.9300 . ?
C37 H37A 0.9300 . ?
C38 N6 1.456(10) . ?
C38 N8 1.451(9) . ?
C38 H38A 0.9800 . ?
N1 H1B 0.8600 . ?
N3 N5 1.346(8) . ?
N6 H6A 0.8600 . ?
N8 N9 1.395(8) . ?
Cl1 O12 1.406(9) . ?
Cl1 O13 1.418(9) . ?
Cl1 O11 1.437(7) . ?
Cl1 O14 1.457(8) . ?
Cl2 O22 1.419(5) . ?
Cl2 O34 1.428(5) . ?
Cl2 O33 1.433(5) . ?
Cl2 O21 1.436(5) . ?

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
N9 Fe1 N5 177.8(3) . . ?
N9 Fe1 O2 74.6(2) . . ?
N5 Fe1 O2 103.3(2) . . ?
N9 Fe1 N10 74.6(3) . . ?
N5 Fe1 N10 107.5(2) . . ?
O2 Fe1 N10 149.2(2) . . ?
N9 Fe1 O1 107.5(2) . . ?
N5 Fe1 O1 73.1(2) . . ?
O2 Fe1 O1 94.25(18) . . ?
N10 Fe1 O1 96.8(2) . . ?
N9 Fe1 N4 104.8(2) . . ?
N5 Fe1 N4 74.8(2) . . ?
O2 Fe1 N4 98.0(2) . . ?
N10 Fe1 N4 87.9(2) . . ?
O1 Fe1 N4 147.5(2) . . ?
C2 C1 C6 120.4(9) . . ?
C2 C1 H1A 119.8 . . ?
C6 C1 H1A 119.8 . . ?
C3 C2 C1 119.6(9) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C4 C3 C2 121.1(9) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C5 120.2(9) . . ?
C3 C4 H4A 119.9 . . ?
C5 C4 H4A 119.9 . . ?
N1 C5 C6 119.7(7) . . ?
N1 C5 C4 122.0(9) . . ?
C6 C5 C4 118.2(9) . . ?
C5 C6 C1 120.4(8) . . ?
C5 C6 C7 118.5(8) . . ?
C1 C6 C7 120.9(8) . . ?
O1 C7 N3 119.4(7) . . ?
O1 C7 C6 122.9(7) . . ?
N3 C7 C6 117.7(7) . . ?
N2 C8 C9 125.6(8) . . ?
N2 C8 C13 117.2(7) . . ?
C9 C8 C13 117.2(8) . . ?
C10 C9 C8 116.0(9) . . ?
C10 C9 H9A 122.0 . . ?
C8 C9 H9A 122.0 . . ?
C11 C10 C9 119.9(9) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C12 C11 C10 120.2(9) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 N2 122.5(10) . . ?
C11 C12 H12A 118.7 . . ?
N2 C12 H12A 118.7 . . ?
N1 C13 N3 107.2(6) . . ?
N1 C13 C8 113.3(7) . . ?
N3 C13 C8 109.4(7) . . ?
N1 C13 H13A 108.9 . . ?
N3 C13 H13A 108.9 . . ?
C8 C13 H13A 108.9 . . ?
N5 C14 C15 115.8(7) . . ?
N5 C14 H14A 122.1 . . ?
C15 C14 H14A 122.1 . . ?
N4 C15 C16 123.6(8) . . ?
N4 C15 C14 115.2(7) . . ?
C16 C15 C14 121.1(8) . . ?
C15 C16 C17 117.5(9) . . ?
C15 C16 H16A 121.3 . . ?
C17 C16 H16A 121.3 . . ?
C18 C17 C16 119.2(9) . . ?
C18 C17 H17A 120.4 . . ?
C16 C17 H17A 120.4 . . ?
C17 C18 C19 119.1(8) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
N4 C19 C18 122.9(8) . . ?
N4 C19 H19A 118.5 . . ?
C18 C19 H19A 118.5 . . ?
N10 C20 C21 122.7(9) . . ?
N10 C20 H20A 118.6 . . ?
C21 C20 H20A 118.6 . . ?
C22 C21 C20 119.2(9) . . ?
C22 C21 H21A 120.4 . . ?
C20 C21 H21A 120.4 . . ?
C21 C22 C23 120.1(9) . . ?
C21 C22 H22A 119.9 . . ?
C23 C22 H22A 119.9 . . ?
C24 C23 C22 118.1(9) . . ?
C24 C23 H23A 121.0 . . ?
C22 C23 H23A 121.0 . . ?
N10 C24 C23 123.1(8) . . ?
N10 C24 C25 113.5(7) . . ?
C23 C24 C25 123.4(9) . . ?
N9 C25 C24 114.2(8) . . ?
N9 C25 H25A 122.9 . . ?
C24 C25 H25A 122.9 . . ?
O2 C26 N8 122.0(7) . . ?
O2 C26 C32 121.9(8) . . ?
N8 C26 C32 116.0(7) . . ?
C32 C27 N6 119.8(8) . . ?
C32 C27 C28 120.2(9) . . ?
N6 C27 C28 120.0(9) . . ?
C29 C28 C27 118.9(9) . . ?
C29 C28 H28A 120.6 . . ?
C27 C28 H28A 120.6 . . ?
C28 C29 C30 120.8(9) . . ?
C28 C29 H29A 119.6 . . ?
C30 C29 H29A 119.6 . . ?
C29 C30 C31 119.3(10) . . ?
C29 C30 H30A 120.3 . . ?
C31 C30 H30A 120.3 . . ?
C32 C31 C30 119.7(10) . . ?
C32 C31 H31A 120.1 . . ?
C30 C31 H31A 120.1 . . ?
C31 C32 C27 121.1(8) . . ?
C31 C32 C26 119.4(8) . . ?
C27 C32 C26 119.2(8) . . ?
N7 C33 C37 124.1(8) . . ?
N7 C33 C38 116.7(7) . . ?
C37 C33 C38 119.1(7) . . ?
N7 C34 C35 124.3(9) . . ?
N7 C34 H34A 117.8 . . ?
C35 C34 H34A 117.8 . . ?
C36 C35 C34 119.1(9) . . ?
C36 C35 H35A 120.4 . . ?
C34 C35 H35A 120.4 . . ?
C35 C36 C37 118.5(8) . . ?
C35 C36 H36A 120.7 . . ?
C37 C36 H36A 120.7 . . ?
C33 C37 C36 118.1(8) . . ?
C33 C37 H37A 121.0 . . ?
C36 C37 H37A 121.0 . . ?
N6 C38 N8 107.1(7) . . ?
N6 C38 C33 111.9(6) . . ?
N8 C38 C33 110.1(6) . . ?
N6 C38 H38A 109.2 . . ?
N8 C38 H38A 109.2 . . ?
C33 C38 H38A 109.2 . . ?
C5 N1 C13 120.2(7) . . ?
C5 N1 H1B 119.9 . . ?
C13 N1 H1B 119.9 . . ?
C8 N2 C12 115.8(8) . . ?
N5 N3 C7 114.4(6) . . ?
N5 N3 C13 122.6(6) . . ?
C7 N3 C13 120.9(6) . . ?
C19 N4 C15 117.6(7) . . ?
C19 N4 Fe1 127.8(6) . . ?
C15 N4 Fe1 114.6(5) . . ?
C14 N5 N3 124.3(7) . . ?
C14 N5 Fe1 118.7(5) . . ?
N3 N5 Fe1 116.6(5) . . ?
C27 N6 C38 119.5(7) . . ?
C27 N6 H6A 120.3 . . ?
C38 N6 H6A 120.3 . . ?
C33 N7 C34 115.9(7) . . ?
C26 N8 N9 110.8(6) . . ?
C26 N8 C38 121.9(6) . . ?
N9 N8 C38 124.3(7) . . ?
C25 N9 N8 121.5(7) . . ?
C25 N9 Fe1 121.8(6) . . ?
N8 N9 Fe1 116.6(5) . . ?
C20 N10 C24 116.7(7) . . ?
C20 N10 Fe1 127.6(6) . . ?
C24 N10 Fe1 115.7(5) . . ?
O12 Cl1 O13 110.4(6) . . ?
O12 Cl1 O11 107.7(5) . . ?
O13 Cl1 O11 114.2(5) . . ?
O12 Cl1 O14 105.3(5) . . ?
O13 Cl1 O14 109.2(5) . . ?
O11 Cl1 O14 109.7(5) . . ?
C7 O1 Fe1 116.0(5) . . ?
O22 Cl2 O34 111.0(4) . . ?
O22 Cl2 O33 109.9(4) . . ?
O34 Cl2 O33 109.1(4) . . ?
O22 Cl2 O21 110.2(4) . . ?
O34 Cl2 O21 108.2(4) . . ?
O33 Cl2 O21 108.4(4) . . ?
C26 O2 Fe1 115.9(5) . . ?

_refine_diff_density_max         1.257
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.119


# start Validation Reply Form
_vrf_PLAT602_1-120K              
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PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: The crystal data is treated with squeeze.
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