# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_071015LRA_work1
_database_code_depnum_ccdc_archive 'CCDC 1522449'
_audit_update_record             
;
2016-12-13 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Fe(C13H11N5O2)2](ClO4)2'
_chemical_formula_moiety         'C26 H22 Fe N10 O4, 2(Cl O4)'
_chemical_formula_sum            'C26 H22 Cl2 Fe N10 O12'
_chemical_formula_weight         793.28

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.476(3)
_cell_length_b                   10.3734(11)
_cell_length_c                   15.7959(18)
_cell_angle_alpha                90
_cell_angle_beta                 127.074(2)
_cell_angle_gamma                90
_cell_volume                     3069.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    6873
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      32.02

_exptl_crystal_preparation       
;
crystallization from acetonitrile/diethylether,
crystal fixed on glass fiber with vacuum grease
;
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             1616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.749
_shelx_estimated_absorpt_T_min   0.759
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      115(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 66
_diffrn_standards_number         'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_reflns_number            21845
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.175
_diffrn_reflns_theta_max         32.020
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5317
_reflns_number_gt                4875
_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       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury 3.8 (Macrae, 2008)'
_computing_publication_material  
'WINGX publication routines v2013.3 (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0494P)²+3.3911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5317
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0898
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.0000 0.14887(2) 0.7500 0.01279(6) Uani 1 2 d S T P . .
N1 N -0.04247(5) 0.28732(9) 0.62267(7) 0.01481(16) Uani 1 1 d . . . . .
N2 N -0.11180(5) 0.11094(9) 0.63985(7) 0.01311(16) Uani 1 1 d . . . . .
N3 N -0.02448(5) -0.00275(9) 0.82038(7) 0.01478(16) Uani 1 1 d . . . . .
N4 N -0.11273(5) 0.26847(9) 0.53827(7) 0.01400(16) Uani 1 1 d . . . . .
N5 N -0.09509(5) -0.03620(9) 0.76022(7) 0.01475(16) Uani 1 1 d . . . . .
O1 O -0.36483(5) 0.05124(10) 0.31989(8) 0.0275(2) Uani 1 1 d . . . . .
O2 O -0.33596(5) -0.12819(9) 0.41862(8) 0.02273(18) Uani 1 1 d . . . . .
C1 C -0.02213(6) 0.39100(11) 0.59749(9) 0.01734(19) Uani 1 1 d . . . . .
C2 C -0.07890(6) 0.44062(11) 0.49786(9) 0.0186(2) Uani 1 1 d . . . . .
C3 C -0.13579(6) 0.36051(11) 0.46229(9) 0.01656(19) Uani 1 1 d . . . . .
C4 C -0.15038(5) 0.16850(10) 0.54505(8) 0.01306(17) Uani 1 1 d . . . . .
C5 C -0.21964(6) 0.13300(11) 0.46286(8) 0.01517(18) Uani 1 1 d . . . . .
C6 C -0.24814(5) 0.03033(11) 0.48360(8) 0.01479(18) Uani 1 1 d . . . . .
C7 C -0.20954(6) -0.03039(11) 0.58200(9) 0.01550(18) Uani 1 1 d . . . . .
C8 C -0.14117(5) 0.01562(10) 0.65775(8) 0.01361(17) Uani 1 1 d . . . . .
C9 C -0.10816(6) -0.12213(12) 0.81192(9) 0.0194(2) Uani 1 1 d . . . . .
C10 C -0.04381(7) -0.14651(12) 0.90785(10) 0.0203(2) Uani 1 1 d . . . . .
C11 C 0.00634(6) -0.07033(11) 0.90934(9) 0.0174(2) Uani 1 1 d . . . . .
C12 C -0.32266(6) -0.01280(12) 0.39698(9) 0.0176(2) Uani 1 1 d . . . . .
C13 C -0.40851(7) -0.17310(15) 0.34661(12) 0.0276(3) Uani 1 1 d . . . . .
H1 H 0.0241(10) 0.4181(17) 0.6438(14) 0.022(4) Uiso 1 1 d . . . . .
H2 H -0.0781(10) 0.5121(19) 0.4637(15) 0.027(5) Uiso 1 1 d . . . . .
H3 H -0.1836(10) 0.3607(17) 0.4020(15) 0.020(4) Uiso 1 1 d . . . . .
H5 H -0.2458(9) 0.1733(17) 0.3940(14) 0.020(4) Uiso 1 1 d . . . . .
H7 H -0.2299(10) -0.1016(19) 0.5934(15) 0.028(5) Uiso 1 1 d . . . . .
H9 H -0.1540(11) -0.1495(18) 0.7819(16) 0.027(5) Uiso 1 1 d . . . . .
H10 H -0.0337(10) -0.2005(19) 0.9613(15) 0.026(5) Uiso 1 1 d . . . . .
H11 H 0.0557(10) -0.0620(19) 0.9611(15) 0.029(5) Uiso 1 1 d . . . . .
H13A H -0.4214(11) -0.187(2) 0.2769(17) 0.032(5) Uiso 1 1 d . . . . .
H13B H -0.4102(11) -0.255(2) 0.3730(16) 0.031(5) Uiso 1 1 d . . . . .
H13C H -0.4418(12) -0.110(2) 0.3426(18) 0.042(6) Uiso 1 1 d . . . . .
Cl1 Cl 0.17622(2) 0.77674(3) 0.15906(2) 0.01885(7) Uani 1 1 d . . . . .
O3 O 0.10271(5) 0.74171(11) 0.10426(9) 0.0319(2) Uani 1 1 d . . . . .
O4 O 0.20076(6) 0.84302(11) 0.25546(8) 0.0338(2) Uani 1 1 d . . . . .
O5 O 0.21841(7) 0.66129(13) 0.18664(11) 0.0405(3) Uani 1 1 d . . . . .
O6 O 0.18223(8) 0.85778(15) 0.09149(11) 0.0483(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1365(9) 2_556 ?
Fe1 N2 2.1366(9) . ?
Fe1 N1 2.1642(10) 2_556 ?
Fe1 N1 2.1643(10) . ?
Fe1 N3 2.1932(10) 2_556 ?
Fe1 N3 2.1932(10) . ?
N1 C1 1.3312(15) . ?
N1 N4 1.3729(12) . ?
N2 C8 1.3295(14) . ?
N2 C4 1.3357(13) . ?
N3 C11 1.3281(14) . ?
N3 N5 1.3683(12) . ?
N4 C3 1.3645(14) . ?
N4 C4 1.4078(14) . ?
N5 C9 1.3629(15) . ?
N5 C8 1.4029(13) . ?
O1 C12 1.2045(15) . ?
O2 C12 1.3325(15) . ?
O2 C13 1.4408(15) . ?
C1 C2 1.4103(16) . ?
C1 H1 0.914(18) . ?
C2 C3 1.3730(16) . ?
C2 H2 0.92(2) . ?
C3 H3 0.938(19) . ?
C4 C5 1.3856(14) . ?
C5 C6 1.3977(15) . ?
C5 H5 0.964(18) . ?
C6 C7 1.3913(15) . ?
C6 C12 1.4989(15) . ?
C7 C8 1.3857(14) . ?
C7 H7 0.95(2) . ?
C9 C10 1.3719(16) . ?
C9 H9 0.92(2) . ?
C10 C11 1.4063(16) . ?
C10 H10 0.917(19) . ?
C11 H11 0.94(2) . ?
C13 H13A 0.96(2) . ?
C13 H13B 0.96(2) . ?
C13 H13C 0.99(2) . ?
Cl1 O6 1.4308(12) . ?
Cl1 O3 1.4348(10) . ?
Cl1 O4 1.4372(11) . ?
Cl1 O5 1.4439(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
N2 Fe1 N2 158.77(5) 2_556 . ?
N2 Fe1 N1 73.37(3) 2_556 2_556 ?
N2 Fe1 N1 122.04(4) . 2_556 ?
N2 Fe1 N1 122.04(4) 2_556 . ?
N2 Fe1 N1 73.38(3) . . ?
N1 Fe1 N1 96.85(5) 2_556 . ?
N2 Fe1 N3 73.27(3) 2_556 2_556 ?
N2 Fe1 N3 91.36(4) . 2_556 ?
N1 Fe1 N3 146.33(3) 2_556 2_556 ?
N1 Fe1 N3 96.86(4) . 2_556 ?
N2 Fe1 N3 91.36(4) 2_556 . ?
N2 Fe1 N3 73.27(3) . . ?
N1 Fe1 N3 96.86(4) 2_556 . ?
N1 Fe1 N3 146.33(3) . . ?
N3 Fe1 N3 88.36(5) 2_556 . ?
C1 N1 N4 105.21(9) . . ?
C1 N1 Fe1 140.04(8) . . ?
N4 N1 Fe1 114.75(7) . . ?
C8 N2 C4 118.87(9) . . ?
C8 N2 Fe1 120.24(7) . . ?
C4 N2 Fe1 120.02(7) . . ?
C11 N3 N5 105.07(9) . . ?
C11 N3 Fe1 140.61(8) . . ?
N5 N3 Fe1 114.07(7) . . ?
C3 N4 N1 111.21(9) . . ?
C3 N4 C4 130.39(9) . . ?
N1 N4 C4 118.22(9) . . ?
C9 N5 N3 111.46(9) . . ?
C9 N5 C8 130.28(9) . . ?
N3 N5 C8 118.21(9) . . ?
C12 O2 C13 115.87(10) . . ?
N1 C1 C2 111.12(10) . . ?
N1 C1 H1 118.4(11) . . ?
C2 C1 H1 130.4(11) . . ?
C3 C2 C1 105.52(10) . . ?
C3 C2 H2 127.2(12) . . ?
C1 C2 H2 127.3(12) . . ?
N4 C3 C2 106.93(10) . . ?
N4 C3 H3 119.5(11) . . ?
C2 C3 H3 133.5(11) . . ?
N2 C4 C5 123.45(10) . . ?
N2 C4 N4 112.47(9) . . ?
C5 C4 N4 124.09(10) . . ?
C4 C5 C6 116.11(10) . . ?
C4 C5 H5 122.1(11) . . ?
C6 C5 H5 121.7(11) . . ?
C7 C6 C5 121.70(10) . . ?
C7 C6 C12 120.02(10) . . ?
C5 C6 C12 118.27(10) . . ?
C8 C7 C6 116.36(10) . . ?
C8 C7 H7 123.7(12) . . ?
C6 C7 H7 119.9(12) . . ?
N2 C8 C7 123.48(10) . . ?
N2 C8 N5 113.10(9) . . ?
C7 C8 N5 123.39(10) . . ?
N5 C9 C10 106.66(10) . . ?
N5 C9 H9 120.6(12) . . ?
C10 C9 H9 132.7(12) . . ?
C9 C10 C11 105.56(10) . . ?
C9 C10 H10 129.2(12) . . ?
C11 C10 H10 125.3(12) . . ?
N3 C11 C10 111.25(10) . . ?
N3 C11 H11 118.3(12) . . ?
C10 C11 H11 130.5(12) . . ?
O1 C12 O2 125.29(11) . . ?
O1 C12 C6 123.63(11) . . ?
O2 C12 C6 111.04(10) . . ?
O2 C13 H13A 111.0(13) . . ?
O2 C13 H13B 106.4(13) . . ?
H13A C13 H13B 107.7(17) . . ?
O2 C13 H13C 110.4(13) . . ?
H13A C13 H13C 109.4(17) . . ?
H13B C13 H13C 112.0(18) . . ?
O6 Cl1 O3 108.81(8) . . ?
O6 Cl1 O4 110.64(9) . . ?
O3 Cl1 O4 109.18(7) . . ?
O6 Cl1 O5 110.75(9) . . ?
O3 Cl1 O5 109.19(8) . . ?
O4 Cl1 O5 108.25(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1 O1 0.914(18) 2.427(18) 3.2704(15) 153.4(15) 8_556
C2 H2 O3 0.92(2) 2.53(2) 3.4033(17) 157.3(16) 2
C3 H3 O4 0.938(19) 2.276(19) 3.2117(16) 175.2(15) 3_445
C5 H5 O4 0.964(18) 2.480(18) 3.4044(16) 160.5(14) 3_445
C7 H7 O5 0.95(2) 2.486(19) 3.2875(16) 141.6(15) 8_456
C9 H9 O5 0.92(2) 2.41(2) 3.3081(17) 164.4(16) 8_456
C10 H10 O3 0.917(19) 2.644(19) 3.1520(16) 115.7(14) 1_546
C11 H11 O6 0.94(2) 2.53(2) 3.4001(19) 155.5(16) 1_546

_refine_diff_density_max         0.748
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_211014NB2_2_work7
_database_code_depnum_ccdc_archive 'CCDC 1522450'
_audit_update_record             
;
2016-12-13 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_compound_source        synthesis
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_iupac          '[Fe(C16H18N6O4)2](ClO4)2.CH3CN'
_chemical_formula_moiety         'C32 H36 Fe N12 O8, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C34 H39 Cl2 Fe N13 O16'
_chemical_formula_weight         1012.53

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0675(10)
_cell_length_b                   16.2407(11)
_cell_length_c                   18.2548(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.045(2)
_cell_angle_gamma                90
_cell_volume                     4093.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    4759
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      24.74

_exptl_crystal_preparation       
;
crystallization from acetonitrile/diethylether,
crystal fixed on glass fiber with vacuum grease
;
_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             2088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.590
_shelx_estimated_absorpt_T_min   0.862
_shelx_estimated_absorpt_T_max   0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8APEX four-circle diffractometer'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean 66
_diffrn_standards_number         'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_decay_%        'not measured'
_diffrn_reflns_number            40776
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.635
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8447
_reflns_number_gt                5581
_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       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury 3.8 (Macrae, 2008)'
_computing_publication_material  
'WINGX publication routines v2013.3 (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1947P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8447
_refine_ls_number_parameters     679
_refine_ls_number_restraints     179
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0928
_refine_ls_wR_factor_ref         0.2869
_refine_ls_wR_factor_gt          0.2568
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.80502(4) 0.24483(4) 0.18320(3) 0.0204(2) Uani 1 1 d . . . . .
N1 N 0.8625(2) 0.1592(2) 0.12856(19) 0.0236(8) Uani 1 1 d . . . . .
N2 N 0.9323(3) 0.2422(2) 0.2407(2) 0.0221(8) Uani 1 1 d . . . . .
N3 N 0.7927(2) 0.3297(2) 0.2577(2) 0.0256(8) Uani 1 1 d . . . . .
N7 N 0.9567(2) 0.1424(2) 0.1611(2) 0.0253(8) Uani 1 1 d . . . . .
N8 N 0.8786(3) 0.3427(2) 0.3079(2) 0.0254(8) Uani 1 1 d . . . . .
C1 C 0.8401(3) 0.1066(3) 0.0724(2) 0.0286(10) Uani 1 1 d . . . . .
H1 H 0.7793 0.1044 0.0391 0.034 Uiso 1 1 calc R U . . .
C2 C 0.9188(4) 0.0544(3) 0.0690(3) 0.0337(11) Uani 1 1 d . . . . .
H2 H 0.9210 0.0112 0.0343 0.040 Uiso 1 1 calc R U . . .
C3 C 0.9923(4) 0.0788(3) 0.1264(3) 0.0330(11) Uani 1 1 d . . . . .
H3 H 1.0553 0.0557 0.1390 0.040 Uiso 1 1 calc R U . . .
C4 C 0.9982(3) 0.1916(3) 0.2225(2) 0.0234(9) Uani 1 1 d . . . . .
C5 C 1.0926(3) 0.1909(3) 0.2586(2) 0.0265(9) Uani 1 1 d . . . . .
H5 H 1.1388 0.1549 0.2439 0.032 Uiso 1 1 calc R U . . .
C6 C 1.1184(3) 0.2463(3) 0.3190(3) 0.0265(10) Uani 1 1 d . . . . .
C7 C 1.0503(3) 0.2956(3) 0.3411(2) 0.0255(9) Uani 1 1 d . . . . .
H7 H 1.0662 0.3303 0.3836 0.031 Uiso 1 1 calc R U . . .
C8 C 0.9569(3) 0.2930(3) 0.2991(2) 0.0266(9) Uani 1 1 d . . . . .
C9 C 0.8674(4) 0.4007(3) 0.3590(3) 0.0322(10) Uani 1 1 d . . . . .
H9 H 0.9155 0.4193 0.3994 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7737(4) 0.4274(3) 0.3409(3) 0.0361(11) Uani 1 1 d . . . . .
H10 H 0.7440 0.4685 0.3660 0.043 Uiso 1 1 calc R U . . .
C11 C 0.7301(3) 0.3821(3) 0.2782(3) 0.0310(10) Uani 1 1 d . . . . .
H11 H 0.6646 0.3881 0.2536 0.037 Uiso 1 1 calc R U . . .
C23 C 1.2220(3) 0.2537(3) 0.3596(3) 0.0316(11) Uani 1 1 d . . . . .
O1 O 1.2403(2) 0.2583(2) 0.42825(19) 0.0363(8) Uani 1 1 d . . . . .
N11 N 1.2865(3) 0.2556(3) 0.3160(2) 0.0356(10) Uani 1 1 d . . . . .
H11A H 1.2647 0.2477 0.2680 0.043 Uiso 1 1 calc R U . . .
C24 C 1.3924(3) 0.2697(3) 0.3396(3) 0.0320(11) Uani 1 1 d . . . . .
C25 C 1.4362(4) 0.2149(4) 0.4046(3) 0.0444(13) Uani 1 1 d . . . . .
H25A H 1.3986 0.1630 0.4011 0.053 Uiso 1 1 calc R U . . .
H25B H 1.5031 0.2007 0.3997 0.053 Uiso 1 1 calc R U . . .
C26 C 1.4103(4) 0.3615(4) 0.3613(4) 0.0522(15) Uani 1 1 d . . . . .
H26A H 1.3757 0.3755 0.4021 0.063 Uiso 1 1 calc R U . . .
H26B H 1.4804 0.3707 0.3798 0.063 Uiso 1 1 calc R U . . .
O2 O 1.4389(3) 0.2503(3) 0.4775(2) 0.0536(11) Uani 1 1 d . . . . .
H2A H 1.3855 0.2424 0.4906 0.064 Uiso 1 1 calc R U . . .
O3 O 1.3773(4) 0.4135(3) 0.2989(4) 0.104(2) Uani 1 1 d . . . . .
H3A H 1.4245 0.4393 0.2881 0.125 Uiso 1 1 calc R U . . .
C27A C 1.4376(10) 0.2411(9) 0.2708(9) 0.034(4) Uani 0.586(3) 1 d D . P A 1
H27A H 1.4440 0.1804 0.2712 0.041 Uiso 0.586(3) 1 calc R U P A 1
H27B H 1.3942 0.2573 0.2237 0.041 Uiso 0.586(3) 1 calc R U P A 1
O4A O 1.5318(4) 0.2786(4) 0.2747(3) 0.0386(15) Uani 0.586(3) 1 d D . P A 1
H4A H 1.5705 0.2601 0.3119 0.046 Uiso 0.586(3) 1 calc R U P A 1
C27B C 1.4388(16) 0.2626(16) 0.2776(12) 0.034(4) Uani 0.414(3) 1 d D . P A 2
H27C H 1.4462 0.2035 0.2668 0.041 Uiso 0.414(3) 1 calc R U P A 2
H27D H 1.5045 0.2866 0.2911 0.041 Uiso 0.414(3) 1 calc R U P A 2
O4B O 1.3876(6) 0.3028(6) 0.2103(5) 0.050(2) Uani 0.414(3) 1 d D . P A 2
H4B H 1.3899 0.3541 0.2164 0.060 Uiso 0.414(3) 1 calc R U P A 2
N4 N 0.7453(2) 0.1599(2) 0.23689(19) 0.0227(8) Uani 1 1 d . . . . .
N5 N 0.6776(3) 0.2461(2) 0.1259(2) 0.0208(8) Uani 1 1 d . . . . .
N6 N 0.8195(2) 0.3295(2) 0.10923(19) 0.0231(8) Uani 1 1 d . . . . .
N9 N 0.6498(2) 0.1456(2) 0.2044(2) 0.0246(8) Uani 1 1 d . . . . .
N10 N 0.7332(2) 0.3480(2) 0.06192(19) 0.0223(7) Uani 1 1 d . . . . .
C12 C 0.7646(3) 0.1084(3) 0.2940(2) 0.0290(10) Uani 1 1 d . . . . .
H12 H 0.8256 0.1039 0.3269 0.035 Uiso 1 1 calc R U . . .
C13 C 0.6818(4) 0.0607(3) 0.2994(3) 0.0322(11) Uani 1 1 d . . . . .
H13 H 0.6767 0.0195 0.3353 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6110(3) 0.0866(3) 0.2423(3) 0.0297(10) Uani 1 1 d . . . . .
H14 H 0.5462 0.0669 0.2311 0.036 Uiso 1 1 calc R U . . .
C15 C 0.6102(3) 0.1960(3) 0.1438(2) 0.0237(9) Uani 1 1 d . . . . .
C16 C 0.5161(3) 0.1971(3) 0.1067(2) 0.0257(9) Uani 1 1 d . . . . .
H16 H 0.4691 0.1610 0.1201 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4916(3) 0.2538(3) 0.0481(2) 0.0236(9) Uani 1 1 d . . . . .
C18 C 0.5614(3) 0.3044(2) 0.0271(2) 0.0229(9) Uani 1 1 d . . . . .
H18 H 0.5462 0.3407 -0.0143 0.027 Uiso 1 1 calc R U . . .
C19 C 0.6531(3) 0.2998(3) 0.0690(2) 0.0219(9) Uani 1 1 d . . . . .
C20 C 0.7447(3) 0.4088(3) 0.0138(3) 0.0300(10) Uani 1 1 d . . . . .
H20 H 0.6958 0.4318 -0.0238 0.036 Uiso 1 1 calc R U . . .
C21 C 0.8405(4) 0.4308(3) 0.0296(3) 0.0321(10) Uani 1 1 d . . . . .
H21 H 0.8710 0.4721 0.0053 0.039 Uiso 1 1 calc R U . . .
C22 C 0.8848(3) 0.3801(3) 0.0890(3) 0.0305(10) Uani 1 1 d . . . . .
H22 H 0.9515 0.3816 0.1115 0.037 Uiso 1 1 calc R U . . .
C28 C 0.3886(3) 0.2625(3) 0.0076(2) 0.0253(9) Uani 1 1 d . . . . .
O5 O 0.3694(2) 0.2712(2) -0.06059(18) 0.0334(8) Uani 1 1 d . . . . .
N12 N 0.3237(3) 0.2607(2) 0.0519(2) 0.0289(9) Uani 1 1 d . . . . .
H12A H 0.3461 0.2522 0.0997 0.035 Uiso 1 1 calc R U . . .
C29 C 0.2182(3) 0.2713(3) 0.0289(3) 0.0300(10) Uani 1 1 d . . . . .
C30 C 0.1962(4) 0.3613(3) 0.0095(3) 0.0427(13) Uani 1 1 d . . . . .
H30A H 0.2282 0.3774 -0.0321 0.051 Uiso 1 1 calc R U . . .
H30B H 0.1255 0.3684 -0.0072 0.051 Uiso 1 1 calc R U . . .
O6 O 0.2293(3) 0.4133(2) 0.0722(2) 0.0524(10) Uani 1 1 d . . . . .
H6 H 0.2890 0.4215 0.0763 0.063 Uiso 1 1 calc R U . . .
C31 C 0.1753(4) 0.2153(4) -0.0371(3) 0.0391(12) Uani 1 1 d . . . . .
H31A H 0.2137 0.1639 -0.0336 0.047 Uiso 1 1 calc R U . . .
H31B H 0.1084 0.2004 -0.0329 0.047 Uiso 1 1 calc R U . . .
O7 O 0.1734(3) 0.2510(2) -0.1082(2) 0.0429(9) Uani 1 1 d . . . . .
H7A H 0.2302 0.2550 -0.1159 0.052 Uiso 1 1 calc R U . . .
C32A C 0.1737(4) 0.2440(3) 0.0943(3) 0.0404(13) Uani 0.586(3) 1 d D . P A 3
H32A H 0.1036 0.2570 0.0841 0.049 Uiso 0.586(3) 1 calc R U P A 3
H32B H 0.1810 0.1837 0.1009 0.049 Uiso 0.586(3) 1 calc R U P A 3
O8A O 0.2201(5) 0.2849(4) 0.1609(3) 0.0429(16) Uani 0.586(3) 1 d D . P A 3
H8A H 0.2217 0.3358 0.1529 0.052 Uiso 0.586(3) 1 calc R U P A 3
C32B C 0.1737(4) 0.2440(3) 0.0943(3) 0.0404(13) Uani 0.250(3) 1 d D . P A 4
H32C H 0.1787 0.2903 0.1302 0.049 Uiso 0.250(3) 1 calc R U P A 4
H32D H 0.1039 0.2337 0.0756 0.049 Uiso 0.250(3) 1 calc R U P A 4
O8B O 0.2156(11) 0.1699(8) 0.1354(8) 0.050(3) Uiso 0.250(3) 1 d D . P A 4
H8B H 0.2104 0.1296 0.1062 0.060 Uiso 0.250(3) 1 calc R U P A 4
C32C C 0.1737(4) 0.2440(3) 0.0943(3) 0.0404(13) Uani 0.164(3) 1 d D . P A 5
H32E H 0.1718 0.1831 0.0948 0.049 Uiso 0.164(3) 1 calc R U P A 5
H32F H 0.2166 0.2619 0.1410 0.049 Uiso 0.164(3) 1 calc R U P A 5
O8C O 0.0765(10) 0.2747(14) 0.0946(14) 0.050(3) Uiso 0.164(3) 1 d D . P A 5
H8C H 0.0386 0.2583 0.0561 0.060 Uiso 0.164(3) 1 calc R U P A 5
Cl1 Cl 0.49626(9) 0.48833(7) 0.13766(7) 0.0392(3) Uani 1 1 d D . . B 6
O9 O 0.5844(3) 0.4747(3) 0.1128(3) 0.0799(16) Uani 1 1 d D U . B 6
O10 O 0.4642(5) 0.5682(3) 0.1207(3) 0.097(2) Uani 1 1 d D U . B 6
O11 O 0.5142(6) 0.4842(5) 0.2162(3) 0.127(3) Uani 1 1 d D U . B 6
O12 O 0.4284(4) 0.4335(4) 0.1012(5) 0.149(3) Uani 1 1 d D U . B 6
Cl2A Cl 0.3585(3) 0.0017(2) 0.0679(3) 0.0637(13) Uani 0.531(7) 1 d D U P C 7
O13A O 0.3835(7) -0.0670(5) 0.0258(5) 0.086(3) Uani 0.531(7) 1 d D U P C 7
O14A O 0.4234(6) 0.0063(5) 0.1328(5) 0.081(3) Uani 0.531(7) 1 d D U P C 7
O15A O 0.3673(11) 0.0719(6) 0.0231(6) 0.102(4) Uani 0.531(7) 1 d D U P C 7
O16A O 0.2605(7) -0.0034(10) 0.0704(8) 0.121(5) Uani 0.531(7) 1 d D U P C 7
Cl2B Cl 0.3162(4) 0.0225(3) 0.0965(3) 0.0669(14) Uani 0.469(7) 1 d D U P C 8
O13B O 0.3454(8) 0.0826(5) 0.1487(4) 0.075(3) Uani 0.469(7) 1 d D U P C 8
O14B O 0.3292(14) 0.0390(10) 0.0238(6) 0.121(5) Uani 0.469(7) 1 d D U P C 8
O15B O 0.3077(10) -0.0573(5) 0.1182(9) 0.119(5) Uani 0.469(7) 1 d D U P C 8
O16B O 0.2115(7) 0.0395(8) 0.0764(9) 0.116(4) Uani 0.469(7) 1 d D U P C 8
N13A N 0.4227(11) -0.0746(11) 0.2972(8) 0.137(6) Uani 0.589(9) 1 d D . P D 9
C33A C 0.3673(11) -0.0244(9) 0.2898(10) 0.085(4) Uani 0.589(9) 1 d D . P D 9
C34A C 0.2867(11) 0.0340(10) 0.288(2) 0.093(6) Uani 0.589(9) 1 d D . P D 9
H34A H 0.2540 0.0432 0.2364 0.139 Uiso 0.589(9) 1 calc R U P D 9
H34B H 0.3120 0.0864 0.3105 0.139 Uiso 0.589(9) 1 calc R U P D 9
H34C H 0.2404 0.0113 0.3167 0.139 Uiso 0.589(9) 1 calc R U P D 9
N13B N 0.4543(14) 0.0099(16) 0.3478(12) 0.137(6) Uani 0.411(9) 1 d D . P D 10
C33B C 0.3752(14) 0.0107(14) 0.3206(15) 0.085(4) Uani 0.411(9) 1 d D . P D 10
C34B C 0.2700(15) 0.0116(19) 0.291(4) 0.093(6) Uani 0.411(9) 1 d D . P D 10
H34D H 0.2392 0.0525 0.3187 0.139 Uiso 0.411(9) 1 calc R U P D 10
H34E H 0.2430 -0.0430 0.2978 0.139 Uiso 0.411(9) 1 calc R U P D 10
H34F H 0.2579 0.0259 0.2382 0.139 Uiso 0.411(9) 1 calc R U P D 10


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.894(4) . ?
Fe1 N5 1.895(4) . ?
Fe1 N6 1.965(4) . ?
Fe1 N3 1.967(4) . ?
Fe1 N4 1.972(3) . ?
Fe1 N1 1.973(4) . ?
N1 C1 1.326(6) . ?
N1 N7 1.372(5) . ?
N2 C4 1.328(5) . ?
N2 C8 1.340(6) . ?
N3 C11 1.329(6) . ?
N3 N8 1.387(5) . ?
N7 C3 1.356(6) . ?
N7 C4 1.409(5) . ?
N8 C9 1.355(6) . ?
N8 C8 1.400(5) . ?
C1 C2 1.405(7) . ?
C2 C3 1.381(7) . ?
C4 C5 1.364(6) . ?
C5 C6 1.416(6) . ?
C6 C7 1.369(6) . ?
C6 C23 1.508(6) . ?
C7 C8 1.389(6) . ?
C9 C10 1.367(7) . ?
C10 C11 1.399(7) . ?
C23 O1 1.232(6) . ?
C23 N11 1.317(7) . ?
N11 C24 1.487(6) . ?
C24 C27B 1.42(3) . ?
C24 C25 1.516(7) . ?
C24 C26 1.550(8) . ?
C24 C27A 1.583(19) . ?
C25 O2 1.444(7) . ?
C26 O3 1.422(7) . ?
C27A O4A 1.449(11) . ?
C27B O4B 1.455(11) . ?
N4 C12 1.324(5) . ?
N4 N9 1.379(5) . ?
N5 C15 1.336(5) . ?
N5 C19 1.349(5) . ?
N6 C22 1.336(5) . ?
N6 N10 1.382(5) . ?
N9 C14 1.357(5) . ?
N9 C15 1.402(5) . ?
N10 C20 1.353(5) . ?
N10 C19 1.397(5) . ?
C12 C13 1.418(7) . ?
C13 C14 1.362(7) . ?
C15 C16 1.367(6) . ?
C16 C17 1.403(6) . ?
C17 C18 1.389(6) . ?
C17 C28 1.503(6) . ?
C18 C19 1.370(6) . ?
C20 C21 1.370(7) . ?
C21 C22 1.410(7) . ?
C28 O5 1.229(5) . ?
C28 N12 1.331(6) . ?
N12 C29 1.473(6) . ?
C29 C32C 1.517(7) . ?
C29 C32B 1.517(7) . ?
C29 C32A 1.517(7) . ?
C29 C30 1.520(7) . ?
C29 C31 1.538(7) . ?
C30 O6 1.426(6) . ?
C31 O7 1.417(6) . ?
C32A O8A 1.429(7) . ?
C32B O8B 1.480(10) . ?
C32C O8C 1.456(10) . ?
Cl1 O12 1.380(5) . ?
Cl1 O10 1.390(4) . ?
Cl1 O11 1.409(5) . ?
Cl1 O9 1.417(4) . ?
Cl2A O14A 1.353(7) . ?
Cl2A O16A 1.390(8) . ?
Cl2A O15A 1.422(8) . ?
Cl2A O13A 1.436(8) . ?
Cl2B O15B 1.366(8) . ?
Cl2B O13B 1.370(7) . ?
Cl2B O14B 1.401(9) . ?
Cl2B O16B 1.475(9) . ?
N13A C33A 1.119(8) . ?
C33A C34A 1.474(9) . ?
N13B C33B 1.127(9) . ?
C33B C34B 1.475(9) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C5 H5 0.9500 . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
N11 H11A 0.8800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O2 H2A 0.8400 . ?
O3 H3A 0.8400 . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
O4A H4A 0.8400 . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
O4B H4B 0.8400 . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
N12 H12A 0.8800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
O6 H6 0.8400 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
O7 H7A 0.8400 . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
O8A H8A 0.8400 . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
O8B H8B 0.8400 . ?
C32C H32E 0.9900 . ?
C32C H32F 0.9900 . ?
O8C H8C 0.8400 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?

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 N5 179.30(15) . . ?
N2 Fe1 N6 100.66(15) . . ?
N5 Fe1 N6 79.91(14) . . ?
N2 Fe1 N3 80.36(14) . . ?
N5 Fe1 N3 100.05(15) . . ?
N6 Fe1 N3 91.09(16) . . ?
N2 Fe1 N4 99.00(14) . . ?
N5 Fe1 N4 80.43(14) . . ?
N6 Fe1 N4 160.34(14) . . ?
N3 Fe1 N4 92.55(15) . . ?
N2 Fe1 N1 80.12(14) . . ?
N5 Fe1 N1 99.47(14) . . ?
N6 Fe1 N1 92.25(15) . . ?
N3 Fe1 N1 160.48(14) . . ?
N4 Fe1 N1 90.75(15) . . ?
C1 N1 N7 105.9(3) . . ?
C1 N1 Fe1 141.8(3) . . ?
N7 N1 Fe1 112.1(3) . . ?
C4 N2 C8 119.5(4) . . ?
C4 N2 Fe1 120.5(3) . . ?
C8 N2 Fe1 120.0(3) . . ?
C11 N3 N8 104.8(4) . . ?
C11 N3 Fe1 142.7(3) . . ?
N8 N3 Fe1 112.5(3) . . ?
C3 N7 N1 111.2(4) . . ?
C3 N7 C4 132.1(4) . . ?
N1 N7 C4 116.8(3) . . ?
C9 N8 N3 111.1(4) . . ?
C9 N8 C8 132.7(4) . . ?
N3 N8 C8 116.2(3) . . ?
N1 C1 C2 110.5(4) . . ?
C3 C2 C1 106.0(4) . . ?
N7 C3 C2 106.5(4) . . ?
N2 C4 C5 123.2(4) . . ?
N2 C4 N7 110.3(4) . . ?
C5 C4 N7 126.6(4) . . ?
C4 C5 C6 116.8(4) . . ?
C7 C6 C5 120.8(4) . . ?
C7 C6 C23 118.3(4) . . ?
C5 C6 C23 120.9(4) . . ?
C6 C7 C8 117.4(4) . . ?
N2 C8 C7 122.1(4) . . ?
N2 C8 N8 111.0(4) . . ?
C7 C8 N8 126.9(4) . . ?
N8 C9 C10 106.8(4) . . ?
C9 C10 C11 106.4(4) . . ?
N3 C11 C10 111.0(4) . . ?
O1 C23 N11 125.4(4) . . ?
O1 C23 C6 119.9(4) . . ?
N11 C23 C6 114.6(4) . . ?
C23 N11 C24 126.5(4) . . ?
C27B C24 N11 110.2(9) . . ?
C27B C24 C25 113.4(8) . . ?
N11 C24 C25 111.8(4) . . ?
C27B C24 C26 101.9(11) . . ?
N11 C24 C26 109.1(4) . . ?
C25 C24 C26 110.1(4) . . ?
N11 C24 C27A 104.9(6) . . ?
C25 C24 C27A 106.4(6) . . ?
C26 C24 C27A 114.5(6) . . ?
O2 C25 C24 115.0(5) . . ?
O3 C26 C24 110.7(5) . . ?
O4A C27A C24 109.9(10) . . ?
C24 C27B O4B 114.2(18) . . ?
C12 N4 N9 105.6(3) . . ?
C12 N4 Fe1 142.3(3) . . ?
N9 N4 Fe1 112.1(2) . . ?
C15 N5 C19 119.7(4) . . ?
C15 N5 Fe1 119.9(3) . . ?
C19 N5 Fe1 120.4(3) . . ?
C22 N6 N10 105.2(3) . . ?
C22 N6 Fe1 142.0(3) . . ?
N10 N6 Fe1 112.8(2) . . ?
C14 N9 N4 110.7(3) . . ?
C14 N9 C15 132.6(4) . . ?
N4 N9 C15 116.6(3) . . ?
C20 N10 N6 111.4(3) . . ?
C20 N10 C19 131.9(4) . . ?
N6 N10 C19 116.6(3) . . ?
N4 C12 C13 110.6(4) . . ?
C14 C13 C12 105.6(4) . . ?
N9 C14 C13 107.5(4) . . ?
N5 C15 C16 122.3(4) . . ?
N5 C15 N9 110.8(4) . . ?
C16 C15 N9 126.8(4) . . ?
C15 C16 C17 117.4(4) . . ?
C18 C17 C16 121.0(4) . . ?
C18 C17 C28 118.3(4) . . ?
C16 C17 C28 120.7(4) . . ?
C19 C18 C17 116.9(4) . . ?
N5 C19 C18 122.6(4) . . ?
N5 C19 N10 110.0(3) . . ?
C18 C19 N10 127.4(4) . . ?
N10 C20 C21 106.9(4) . . ?
C20 C21 C22 106.3(4) . . ?
N6 C22 C21 110.3(4) . . ?
O5 C28 N12 125.1(4) . . ?
O5 C28 C17 120.9(4) . . ?
N12 C28 C17 114.0(4) . . ?
C28 N12 C29 126.5(4) . . ?
N12 C29 C32C 106.7(4) . . ?
N12 C29 C32B 106.7(4) . . ?
N12 C29 C32A 106.7(4) . . ?
N12 C29 C30 109.2(4) . . ?
C32C C29 C30 111.6(4) . . ?
C32B C29 C30 111.6(4) . . ?
C32A C29 C30 111.6(4) . . ?
N12 C29 C31 112.1(4) . . ?
C32C C29 C31 106.5(4) . . ?
C32B C29 C31 106.5(4) . . ?
C32A C29 C31 106.5(4) . . ?
C30 C29 C31 110.7(4) . . ?
O6 C30 C29 111.2(4) . . ?
O7 C31 C29 114.3(4) . . ?
O8A C32A C29 110.1(5) . . ?
O8B C32B C29 116.9(7) . . ?
O8C C32C C29 115.6(10) . . ?
O12 Cl1 O10 109.3(4) . . ?
O12 Cl1 O11 115.6(5) . . ?
O10 Cl1 O11 105.0(4) . . ?
O12 Cl1 O9 108.2(3) . . ?
O10 Cl1 O9 110.0(4) . . ?
O11 Cl1 O9 108.7(4) . . ?
O14A Cl2A O16A 118.8(8) . . ?
O14A Cl2A O15A 109.9(6) . . ?
O16A Cl2A O15A 105.2(8) . . ?
O14A Cl2A O13A 108.5(6) . . ?
O16A Cl2A O13A 108.5(7) . . ?
O15A Cl2A O13A 105.0(7) . . ?
O15B Cl2B O13B 120.4(8) . . ?
O15B Cl2B O14B 119.4(9) . . ?
O13B Cl2B O14B 116.5(7) . . ?
O15B Cl2B O16B 96.4(8) . . ?
O13B Cl2B O16B 101.1(7) . . ?
O14B Cl2B O16B 91.9(9) . . ?
N13A C33A C34A 171(2) . . ?
N13B C33B C34B 175(4) . . ?
N1 C1 H1 124.8 . . ?
C2 C1 H1 124.8 . . ?
C3 C2 H2 127.0 . . ?
C1 C2 H2 127.0 . . ?
N7 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C6 C7 H7 121.3 . . ?
C8 C7 H7 121.3 . . ?
N8 C9 H9 126.6 . . ?
C10 C9 H9 126.6 . . ?
C9 C10 H10 126.8 . . ?
C11 C10 H10 126.8 . . ?
N3 C11 H11 124.5 . . ?
C10 C11 H11 124.5 . . ?
C23 N11 H11A 116.7 . . ?
C24 N11 H11A 116.7 . . ?
O2 C25 H25A 108.5 . . ?
C24 C25 H25A 108.5 . . ?
O2 C25 H25B 108.5 . . ?
C24 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
O3 C26 H26A 109.5 . . ?
C24 C26 H26A 109.5 . . ?
O3 C26 H26B 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
C25 O2 H2A 109.5 . . ?
C26 O3 H3A 109.5 . . ?
O4A C27A H27A 109.7 . . ?
C24 C27A H27A 109.7 . . ?
O4A C27A H27B 109.7 . . ?
C24 C27A H27B 109.7 . . ?
H27A C27A H27B 108.2 . . ?
C27A O4A H4A 109.5 . . ?
C24 C27B H27C 108.7 . . ?
O4B C27B H27C 108.7 . . ?
C24 C27B H27D 108.7 . . ?
O4B C27B H27D 108.7 . . ?
H27C C27B H27D 107.6 . . ?
C27B O4B H4B 109.5 . . ?
N4 C12 H12 124.7 . . ?
C13 C12 H12 124.7 . . ?
C14 C13 H13 127.2 . . ?
C12 C13 H13 127.2 . . ?
N9 C14 H14 126.2 . . ?
C13 C14 H14 126.2 . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
C19 C18 H18 121.5 . . ?
C17 C18 H18 121.5 . . ?
N10 C20 H20 126.6 . . ?
C21 C20 H20 126.6 . . ?
C20 C21 H21 126.8 . . ?
C22 C21 H21 126.8 . . ?
N6 C22 H22 124.9 . . ?
C21 C22 H22 124.9 . . ?
C28 N12 H12A 116.8 . . ?
C29 N12 H12A 116.8 . . ?
O6 C30 H30A 109.4 . . ?
C29 C30 H30A 109.4 . . ?
O6 C30 H30B 109.4 . . ?
C29 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C30 O6 H6 109.5 . . ?
O7 C31 H31A 108.7 . . ?
C29 C31 H31A 108.7 . . ?
O7 C31 H31B 108.7 . . ?
C29 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C31 O7 H7A 109.5 . . ?
O8A C32A H32A 109.6 . . ?
C29 C32A H32A 109.6 . . ?
O8A C32A H32B 109.6 . . ?
C29 C32A H32B 109.6 . . ?
H32A C32A H32B 108.2 . . ?
C32A O8A H8A 109.5 . . ?
O8B C32B H32C 108.1 . . ?
C29 C32B H32C 108.1 . . ?
O8B C32B H32D 108.1 . . ?
C29 C32B H32D 108.1 . . ?
H32C C32B H32D 107.3 . . ?
C32B O8B H8B 109.5 . . ?
O8C C32C H32E 108.4 . . ?
C29 C32C H32E 108.4 . . ?
O8C C32C H32F 108.4 . . ?
C29 C32C H32F 108.4 . . ?
H32E C32C H32F 107.4 . . ?
C32C O8C H8C 109.5 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11A O8A 0.88 2.03 2.846(7) 154.2 1_655
O2 H2A O1 0.84 2.16 2.770(5) 129.8 .
O3 H3A O11 0.84 2.12 2.902(10) 155.4 1_655
O4A H4A O7 0.84 1.86 2.671(7) 163.0 4_766
O4B H4B O3 0.84 1.83 2.441(13) 128.7 .
N12 H12A O4B 0.88 2.15 2.940(10) 148.4 1_455
O6 H6 O12 0.84 1.94 2.769(7) 171.1 .
O7 H7A O5 0.84 2.04 2.747(5) 141.3 .
O8A H8A O6 0.84 1.96 2.658(8) 140.4 .
O8C H8C O2 0.84 1.81 2.63(2) 163.5 4_465

_refine_diff_density_max         3.946
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.164

