# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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_Fe_T100K
_database_code_depnum_ccdc_archive 'CCDC 1558084'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;


#v153GuillotICMMO

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H44 B2 Fe N12'
_chemical_formula_sum            'C30 H44 B2 Fe N12'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            pink

_diffrn_ambient_temperature      100(1)
_chemical_formula_weight         650.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0016 0.0007 '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'
Fe Fe 0.3460 0.8476 '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                   8.7244(5)
_cell_length_b                   10.4918(6)
_cell_length_c                   10.8211(6)
_cell_angle_alpha                115.322(2)
_cell_angle_beta                 98.499(3)
_cell_angle_gamma                109.477(3)
_cell_volume                     793.58(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.009
_exptl_absorpt_coefficient_mu    0.518
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9712
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26912
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.215
_diffrn_reflns_theta_max         30.647
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4888
_reflns_number_gt                3749
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0677P)²+0.5073P] 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         4888
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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
C1 C 0.4525(3) 0.1020(3) 0.2979(2) 0.0175(5) Uani 1 1 d . . . . .
H1A H 0.3810 0.1449 0.2711 0.026 Uiso 1 1 calc R U . . .
H1B H 0.3807 0.0026 0.2859 0.026 Uiso 1 1 calc R U . . .
H1C H 0.5222 0.0873 0.2370 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5675(3) 0.2132(2) 0.4537(2) 0.0126(4) Uani 1 1 d . . . . .
C3 C 0.6690(3) 0.1807(3) 0.5384(2) 0.0146(4) Uani 1 1 d . . . . .
H3 H 0.6770 0.0867 0.5095 0.017 Uiso 1 1 calc R U . . .
C4 C 0.7544(3) 0.3163(3) 0.6732(2) 0.0120(4) Uani 1 1 d . . . . .
C5 C 0.8794(3) 0.3483(3) 0.8055(3) 0.0171(5) Uani 1 1 d . . . . .
H5A H 0.9906 0.4286 0.8278 0.026 Uiso 1 1 calc R U . . .
H5B H 0.8887 0.2538 0.7875 0.026 Uiso 1 1 calc R U . . .
H5C H 0.8390 0.3831 0.8860 0.026 Uiso 1 1 calc R U . . .
C6 C 0.1716(3) 0.5681(3) 0.6457(2) 0.0163(4) Uani 1 1 d . . . . .
H6A H 0.1782 0.6665 0.6590 0.024 Uiso 1 1 calc R U . . .
H6B H 0.0771 0.5205 0.6716 0.024 Uiso 1 1 calc R U . . .
H6C H 0.1534 0.4992 0.5457 0.024 Uiso 1 1 calc R U . . .
C7 C 0.3365(3) 0.5959(3) 0.7400(2) 0.0123(4) Uani 1 1 d . . . . .
C8 C 0.3868(3) 0.6523(3) 0.8897(2) 0.0130(4) Uani 1 1 d . . . . .
H8 H 0.3240 0.6801 0.9504 0.016 Uiso 1 1 calc R U . . .
C9 C 0.5482(3) 0.6584(2) 0.9294(2) 0.0111(4) Uani 1 1 d . . . . .
C10 C 0.6614(3) 0.7054(3) 1.0738(2) 0.0168(5) Uani 1 1 d . . . . .
H10A H 0.6650 0.6141 1.0719 0.025 Uiso 1 1 calc R U . . .
H10B H 0.6160 0.7524 1.1474 0.025 Uiso 1 1 calc R U . . .
H10C H 0.7761 0.7799 1.0951 0.025 Uiso 1 1 calc R U . . .
C11 C 0.7847(3) 0.7911(3) 0.4389(2) 0.0156(4) Uani 1 1 d . . . . .
H11A H 0.8379 0.7455 0.3719 0.023 Uiso 1 1 calc R U . . .
H11B H 0.8205 0.8990 0.4655 0.023 Uiso 1 1 calc R U . . .
H11C H 0.6612 0.7341 0.3939 0.023 Uiso 1 1 calc R U . . .
C12 C 0.8383(3) 0.7828(2) 0.5722(2) 0.0117(4) Uani 1 1 d . . . . .
C13 C 0.9975(3) 0.8820(3) 0.6859(2) 0.0137(4) Uani 1 1 d . . . . .
H13 H 1.0888 0.9659 0.6939 0.016 Uiso 1 1 calc R U . . .
C14 C 0.9919(3) 0.8304(2) 0.7839(2) 0.0111(4) Uani 1 1 d . . . . .
C15 C 1.1258(3) 0.8933(3) 0.9254(2) 0.0158(4) Uani 1 1 d . . . . .
H15A H 1.0783 0.9218 1.0021 0.024 Uiso 1 1 calc R U . . .
H15B H 1.2242 0.9843 0.9448 0.024 Uiso 1 1 calc R U . . .
H15C H 1.1608 0.8140 0.9201 0.024 Uiso 1 1 calc R U . . .
B1 B 0.7565(3) 0.5952(3) 0.7859(3) 0.0106(4) Uani 1 1 d . . . . .
H1 H 0.8384 0.6250 0.8771 0.013 Uiso 1 1 calc R U . . .
N1 N 0.5901(2) 0.3618(2) 0.53277(18) 0.0099(3) Uani 1 1 d . . . . .
N2 N 0.4618(2) 0.5698(2) 0.69087(19) 0.0100(3) Uani 1 1 d . . . . .
N3 N 0.7394(2) 0.6756(2) 0.59901(18) 0.0103(3) Uani 1 1 d . . . . .
N4 N 0.7055(2) 0.4245(2) 0.66819(18) 0.0100(3) Uani 1 1 d . . . . .
N5 N 0.5911(2) 0.6077(2) 0.80831(18) 0.0095(3) Uani 1 1 d . . . . .
N6 N 0.8359(2) 0.7051(2) 0.72913(18) 0.0095(3) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.00753(12) Uani 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.498(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.344(3) . ?
C2 C3 1.403(3) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 N4 1.357(3) . ?
C4 C5 1.494(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.492(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.342(3) . ?
C7 C8 1.401(3) . ?
C8 C9 1.381(3) . ?
C8 H8 0.9300 . ?
C9 N5 1.350(3) . ?
C9 C10 1.490(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.497(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.341(3) . ?
C12 C13 1.401(3) . ?
C13 C14 1.381(3) . ?
C13 H13 0.9300 . ?
C14 N6 1.354(3) . ?
C14 C15 1.496(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
B1 N5 1.536(3) . ?
B1 N4 1.542(3) . ?
B1 N6 1.545(3) . ?
B1 H1 0.9800 . ?
N1 N4 1.375(2) . ?
N1 Fe1 1.9908(17) . ?
N2 N5 1.375(2) . ?
N2 Fe1 1.9966(17) . ?
N3 N6 1.375(2) . ?
N3 Fe1 1.9975(17) . ?
Fe1 N1 1.9909(17) 2_666 ?
Fe1 N2 1.9967(17) 2_666 ?
Fe1 N3 1.9975(18) 2_666 ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 109.69(19) . . ?
N1 C2 C1 124.25(19) . . ?
C3 C2 C1 126.1(2) . . ?
C4 C3 C2 106.2(2) . . ?
C4 C3 H3 126.9 . . ?
C2 C3 H3 126.9 . . ?
N4 C4 C3 107.44(19) . . ?
N4 C4 C5 123.34(19) . . ?
C3 C4 C5 129.2(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 109.31(19) . . ?
N2 C7 C6 123.59(19) . . ?
C8 C7 C6 127.1(2) . . ?
C9 C8 C7 106.43(19) . . ?
C9 C8 H8 126.8 . . ?
C7 C8 H8 126.8 . . ?
N5 C9 C8 107.31(18) . . ?
N5 C9 C10 122.8(2) . . ?
C8 C9 C10 129.9(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 109.63(19) . . ?
N3 C12 C11 124.29(19) . . ?
C13 C12 C11 126.1(2) . . ?
C14 C13 C12 106.39(19) . . ?
C14 C13 H13 126.8 . . ?
C12 C13 H13 126.8 . . ?
N6 C14 C13 107.10(18) . . ?
N6 C14 C15 123.38(19) . . ?
C13 C14 C15 129.5(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 B1 N4 108.27(17) . . ?
N5 B1 N6 107.50(17) . . ?
N4 B1 N6 108.55(17) . . ?
N5 B1 H1 110.8 . . ?
N4 B1 H1 110.8 . . ?
N6 B1 H1 110.8 . . ?
C2 N1 N4 106.44(17) . . ?
C2 N1 Fe1 136.21(15) . . ?
N4 N1 Fe1 117.36(13) . . ?
C7 N2 N5 106.68(16) . . ?
C7 N2 Fe1 135.58(15) . . ?
N5 N2 Fe1 117.71(13) . . ?
C12 N3 N6 106.42(17) . . ?
C12 N3 Fe1 135.67(15) . . ?
N6 N3 Fe1 117.90(13) . . ?
C4 N4 N1 110.25(17) . . ?
C4 N4 B1 130.79(18) . . ?
N1 N4 B1 118.96(16) . . ?
C9 N5 N2 110.27(17) . . ?
C9 N5 B1 131.14(18) . . ?
N2 N5 B1 118.51(16) . . ?
C14 N6 N3 110.46(17) . . ?
C14 N6 B1 131.41(17) . . ?
N3 N6 B1 118.12(16) . . ?
N1 Fe1 N1 180.0 . 2_666 ?
N1 Fe1 N2 89.97(7) . . ?
N1 Fe1 N2 90.03(7) 2_666 . ?
N1 Fe1 N2 90.03(7) . 2_666 ?
N1 Fe1 N2 89.97(7) 2_666 2_666 ?
N2 Fe1 N2 180.00(12) . 2_666 ?
N1 Fe1 N3 89.60(7) . . ?
N1 Fe1 N3 90.40(7) 2_666 . ?
N2 Fe1 N3 89.82(7) . . ?
N2 Fe1 N3 90.17(7) 2_666 . ?
N1 Fe1 N3 90.40(7) . 2_666 ?
N1 Fe1 N3 89.60(7) 2_666 2_666 ?
N2 Fe1 N3 90.17(7) . 2_666 ?
N2 Fe1 N3 89.83(7) 2_666 2_666 ?
N3 Fe1 N3 180.0 . 2_666 ?

_refine_diff_density_max         0.574
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.171

_shelxl_version_number           2013-4


_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# 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_Fe_T240K
_database_code_depnum_ccdc_archive 'CCDC 1558085'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H22 B Fe0.50 N6'
_chemical_formula_weight         325.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0016 0.0007 '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'
Fe Fe 0.3460 0.8476 '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                   8.7770(9)
_cell_length_b                   10.7908(10)
_cell_length_c                   10.9916(17)
_cell_angle_alpha                106.485(7)
_cell_angle_beta                 108.711(7)
_cell_angle_gamma                109.714(5)
_cell_volume                     833.71(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    240(1)
_cell_measurement_reflns_used    7827
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      25.89

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.453
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      240(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29746
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.232
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5099
_reflns_number_gt                3460
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0821P)²+0.2198P] 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         5099
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1656
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
C1 C 0.3235(5) 0.5638(4) 0.9460(3) 0.0546(8) Uani 1 1 d . . . . .
H1A H 0.4436 0.5964 1.0186 0.082 Uiso 1 1 calc R U . . .
H1B H 0.2342 0.5023 0.9643 0.082 Uiso 1 1 calc R U . . .
H1C H 0.3060 0.6471 0.9470 0.082 Uiso 1 1 calc R U . . .
C2 C 0.3031(4) 0.4791(3) 0.8031(3) 0.0395(6) Uani 1 1 d . . . . .
C3 C 0.1952(4) 0.3325(4) 0.7125(3) 0.0477(7) Uani 1 1 d . . . . .
H3 H 0.1142 0.2630 0.7263 0.057 Uiso 1 1 calc R U . . .
C4 C 0.2310(4) 0.3086(3) 0.5963(3) 0.0416(6) Uani 1 1 d . . . . .
C5 C 0.1495(5) 0.1659(3) 0.4668(4) 0.0589(9) Uani 1 1 d . . . . .
H5A H 0.0232 0.1354 0.4096 0.088 Uiso 1 1 calc R U . . .
H5B H 0.1597 0.0925 0.4969 0.088 Uiso 1 1 calc R U . . .
H5C H 0.2137 0.1789 0.4115 0.088 Uiso 1 1 calc R U . . .
C6 C 0.4325(5) 0.9597(3) 0.8139(3) 0.0473(7) Uani 1 1 d . . . . .
H6A H 0.3408 0.9040 0.8340 0.071 Uiso 1 1 calc R U . . .
H6B H 0.4112 1.0371 0.7992 0.071 Uiso 1 1 calc R U . . .
H6C H 0.5507 1.0010 0.8931 0.071 Uiso 1 1 calc R U . . .
C7 C 0.4244(4) 0.8617(3) 0.6821(3) 0.0328(5) Uani 1 1 d . . . . .
C8 C 0.3744(4) 0.8629(3) 0.5511(3) 0.0397(6) Uani 1 1 d . . . . .
H8 H 0.3374 0.9267 0.5248 0.048 Uiso 1 1 calc R U . . .
C9 C 0.3896(4) 0.7504(3) 0.4655(3) 0.0370(6) Uani 1 1 d . . . . .
C10 C 0.3499(5) 0.7043(4) 0.3120(3) 0.0511(8) Uani 1 1 d . . . . .
H10A H 0.3774 0.6254 0.2818 0.077 Uiso 1 1 calc R U . . .
H10B H 0.4236 0.7857 0.3019 0.077 Uiso 1 1 calc R U . . .
H10C H 0.2233 0.6721 0.2540 0.077 Uiso 1 1 calc R U . . .
C11 C 0.9057(4) 0.8764(3) 1.0773(3) 0.0495(8) Uani 1 1 d . . . . .
H11A H 0.8932 0.9602 1.0725 0.074 Uiso 1 1 calc R U . . .
H11B H 1.0251 0.9084 1.1503 0.074 Uiso 1 1 calc R U . . .
H11C H 0.8153 0.8226 1.0997 0.074 Uiso 1 1 calc R U . . .
C12 C 0.8797(4) 0.7800(3) 0.9362(3) 0.0353(6) Uani 1 1 d . . . . .
C13 C 1.0033(4) 0.7468(3) 0.9020(3) 0.0434(7) Uani 1 1 d . . . . .
H13 H 1.1242 0.7789 0.9642 0.052 Uiso 1 1 calc R U . . .
C14 C 0.9116(4) 0.6557(3) 0.7563(3) 0.0392(6) Uani 1 1 d . . . . .
C15 C 0.9827(4) 0.5900(4) 0.6632(4) 0.0529(8) Uani 1 1 d . . . . .
H15A H 0.9888 0.5073 0.6763 0.079 Uiso 1 1 calc R U . . .
H15B H 1.1024 0.6618 0.6886 0.079 Uiso 1 1 calc R U . . .
H15C H 0.9026 0.5588 0.5649 0.079 Uiso 1 1 calc R U . . .
B1 B 0.5335(4) 0.7006(3) 0.7904(3) 0.0311(6) Uani 1 1 d . . . . .
H1 H 0.5436 0.7633 0.8800 0.037 Uiso 1 1 calc R U . . .
N1 N 0.3535(3) 0.4343(2) 0.6127(2) 0.0335(5) Uani 1 1 d . . . . .
N2 N 0.4468(3) 0.6827(2) 0.5400(2) 0.0312(5) Uani 1 1 d . . . . .
N3 N 0.7394(3) 0.6327(2) 0.7027(2) 0.0321(5) Uani 1 1 d . . . . .
N4 N 0.3968(3) 0.5405(2) 0.7411(2) 0.0305(5) Uani 1 1 d . . . . .
N5 N 0.4680(3) 0.7524(2) 0.6750(2) 0.0279(4) Uani 1 1 d . . . . .
N6 N 0.7212(3) 0.7106(2) 0.8152(2) 0.0295(4) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.02396(16) Uani 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.493(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N4 1.352(3) . ?
C2 C3 1.372(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 N1 1.335(3) . ?
C4 C5 1.505(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.495(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N5 1.347(3) . ?
C7 C8 1.370(4) . ?
C8 C9 1.385(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.333(3) . ?
C9 C10 1.499(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.496(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N6 1.345(3) . ?
C12 C13 1.376(4) . ?
C13 C14 1.387(4) . ?
C13 H13 0.9300 . ?
C14 N3 1.336(3) . ?
C14 C15 1.496(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
B1 N4 1.540(4) . ?
B1 N6 1.542(3) . ?
B1 N5 1.550(4) . ?
B1 H1 0.9800 . ?
N1 N4 1.377(3) . ?
N1 Fe1 2.144(2) . ?
N2 N5 1.377(3) . ?
N2 Fe1 2.136(2) . ?
N3 N6 1.375(3) . ?
N3 Fe1 2.141(2) . ?
Fe1 N2 2.136(2) 2_666 ?
Fe1 N3 2.141(2) 2_666 ?
Fe1 N1 2.144(2) 2_666 ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N4 C2 C3 107.6(3) . . ?
N4 C2 C1 123.2(3) . . ?
C3 C2 C1 129.2(3) . . ?
C2 C3 C4 106.3(3) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 H3 126.8 . . ?
N1 C4 C3 110.1(3) . . ?
N1 C4 C5 122.1(3) . . ?
C3 C4 C5 127.8(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C7 C8 107.8(2) . . ?
N5 C7 C6 123.4(2) . . ?
C8 C7 C6 128.8(2) . . ?
C7 C8 C9 106.4(2) . . ?
C7 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
N2 C9 C8 109.8(2) . . ?
N2 C9 C10 122.2(2) . . ?
C8 C9 C10 128.0(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 C13 107.5(2) . . ?
N6 C12 C11 123.2(3) . . ?
C13 C12 C11 129.3(3) . . ?
C12 C13 C14 106.3(2) . . ?
C12 C13 H13 126.9 . . ?
C14 C13 H13 126.9 . . ?
N3 C14 C13 109.9(2) . . ?
N3 C14 C15 121.4(3) . . ?
C13 C14 C15 128.7(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 B1 N6 108.8(2) . . ?
N4 B1 N5 110.1(2) . . ?
N6 B1 N5 109.7(2) . . ?
N4 B1 H1 109.4 . . ?
N6 B1 H1 109.4 . . ?
N5 B1 H1 109.4 . . ?
C4 N1 N4 106.3(2) . . ?
C4 N1 Fe1 136.34(19) . . ?
N4 N1 Fe1 117.18(15) . . ?
C9 N2 N5 106.5(2) . . ?
C9 N2 Fe1 136.87(17) . . ?
N5 N2 Fe1 116.54(15) . . ?
C14 N3 N6 106.3(2) . . ?
C14 N3 Fe1 136.20(18) . . ?
N6 N3 Fe1 117.35(14) . . ?
C2 N4 N1 109.7(2) . . ?
C2 N4 B1 131.0(2) . . ?
N1 N4 B1 119.31(19) . . ?
C7 N5 N2 109.5(2) . . ?
C7 N5 B1 130.3(2) . . ?
N2 N5 B1 120.20(19) . . ?
C12 N6 N3 110.1(2) . . ?
C12 N6 B1 130.5(2) . . ?
N3 N6 B1 119.35(19) . . ?
N2 Fe1 N2 180.0 . 2_666 ?
N2 Fe1 N3 86.72(8) . . ?
N2 Fe1 N3 93.28(8) 2_666 . ?
N2 Fe1 N3 93.28(8) . 2_666 ?
N2 Fe1 N3 86.72(8) 2_666 2_666 ?
N3 Fe1 N3 180.00(11) . 2_666 ?
N2 Fe1 N1 86.84(8) . . ?
N2 Fe1 N1 93.16(8) 2_666 . ?
N3 Fe1 N1 87.57(8) . . ?
N3 Fe1 N1 92.43(8) 2_666 . ?
N2 Fe1 N1 93.16(8) . 2_666 ?
N2 Fe1 N1 86.84(8) 2_666 2_666 ?
N3 Fe1 N1 92.44(8) . 2_666 ?
N3 Fe1 N1 87.57(8) 2_666 2_666 ?
N1 Fe1 N1 180.0 . 2_666 ?

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.147

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_Fe_T298K
_database_code_depnum_ccdc_archive 'CCDC 1558087'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H44 B2 Fe N12'
_chemical_formula_weight         650.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0016 0.0007 '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'
Fe Fe 0.3460 0.8476 '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                   8.8124(3)
_cell_length_b                   10.1928(3)
_cell_length_c                   10.7673(4)
_cell_angle_alpha                116.3380(10)
_cell_angle_beta                 85.244(2)
_cell_angle_gamma                100.143(2)
_cell_volume                     853.19(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_F_000             344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50969
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         30.564
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5236
_reflns_number_gt                3766
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0840P)²+0.1145P] 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         5236
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1519
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.6502(4) 0.1600(3) 0.4566(3) 0.0779(8) Uani 1 1 d . . . . .
H1A H 0.5473 0.1482 0.4259 0.117 Uiso 1 1 calc R U . . .
H1B H 0.6615 0.0763 0.4718 0.117 Uiso 1 1 calc R U . . .
H1C H 0.7227 0.1668 0.3873 0.117 Uiso 1 1 calc R U . . .
C2 C 0.6798(3) 0.2979(3) 0.5884(3) 0.0557(6) Uani 1 1 d . . . . .
C3 C 0.7467(3) 0.3166(3) 0.7094(3) 0.0681(7) Uani 1 1 d . . . . .
H3 H 0.7821 0.2442 0.7245 0.082 Uiso 1 1 calc R U . . .
C4 C 0.7500(3) 0.4616(3) 0.8011(3) 0.0577(6) Uani 1 1 d . . . . .
C5 C 0.8057(5) 0.5420(4) 0.9472(3) 0.0931(11) Uani 1 1 d . . . . .
H5A H 0.8950 0.6136 0.9529 0.140 Uiso 1 1 calc R U . . .
H5B H 0.8321 0.4725 0.9764 0.140 Uiso 1 1 calc R U . . .
H5C H 0.7258 0.5916 1.0063 0.140 Uiso 1 1 calc R U . . .
C6 C 0.1141(3) 0.5742(3) 0.6570(3) 0.0644(7) Uani 1 1 d . . . . .
H6A H 0.0541 0.6498 0.6712 0.097 Uiso 1 1 calc R U . . .
H6B H 0.0525 0.4993 0.6786 0.097 Uiso 1 1 calc R U . . .
H6C H 0.1472 0.5304 0.5620 0.097 Uiso 1 1 calc R U . . .
C7 C 0.2521(2) 0.6414(2) 0.7493(2) 0.0468(5) Uani 1 1 d . . . . .
C8 C 0.2572(3) 0.7310(3) 0.8912(2) 0.0560(6) Uani 1 1 d . . . . .
H8 H 0.1737 0.7617 0.9496 0.067 Uiso 1 1 calc R U . . .
C9 C 0.4088(3) 0.7651(2) 0.9280(2) 0.0486(5) Uani 1 1 d . . . . .
C10 C 0.4803(4) 0.8577(3) 1.0685(2) 0.0706(7) Uani 1 1 d . . . . .
H10A H 0.5189 0.7950 1.0996 0.106 Uiso 1 1 calc R U . . .
H10B H 0.4041 0.9078 1.1328 0.106 Uiso 1 1 calc R U . . .
H10C H 0.5637 0.9295 1.0627 0.106 Uiso 1 1 calc R U . . .
C11 C 0.7239(4) 0.7392(3) 0.3482(2) 0.0684(7) Uani 1 1 d . . . . .
H11A H 0.6672 0.6411 0.3019 0.103 Uiso 1 1 calc R U . . .
H11B H 0.8202 0.7459 0.3011 0.103 Uiso 1 1 calc R U . . .
H11C H 0.6649 0.8098 0.3478 0.103 Uiso 1 1 calc R U . . .
C12 C 0.7538(3) 0.7719(2) 0.4946(2) 0.0476(5) Uani 1 1 d . . . . .
C13 C 0.8642(3) 0.8795(3) 0.5843(2) 0.0578(6) Uani 1 1 d . . . . .
H13 H 0.9345 0.9485 0.5662 0.069 Uiso 1 1 calc R U . . .
C14 C 0.8490(2) 0.8641(2) 0.7045(2) 0.0458(5) Uani 1 1 d . . . . .
C15 C 0.9418(3) 0.9495(3) 0.8339(3) 0.0664(7) Uani 1 1 d . . . . .
H15A H 0.8739 0.9867 0.9119 0.100 Uiso 1 1 calc R U . . .
H15B H 1.0095 1.0309 0.8272 0.100 Uiso 1 1 calc R U . . .
H15C H 1.0016 0.8858 0.8457 0.100 Uiso 1 1 calc R U . . .
B1 B 0.6653(3) 0.6909(3) 0.7920(2) 0.0407(5) Uani 1 1 d . . . . .
H1 H 0.7174 0.7502 0.8813 0.049 Uiso 1 1 calc R U . . .
N1 N 0.6428(2) 0.42617(19) 0.60623(18) 0.0447(4) Uani 1 1 d . . . . .
N2 N 0.39393(19) 0.62083(18) 0.70089(16) 0.0409(4) Uani 1 1 d . . . . .
N3 N 0.67437(19) 0.69418(17) 0.55640(15) 0.0396(4) Uani 1 1 d . . . . .
N4 N 0.68894(19) 0.5281(2) 0.73763(17) 0.0427(4) Uani 1 1 d . . . . .
N5 N 0.49157(19) 0.69797(18) 0.81194(15) 0.0402(4) Uani 1 1 d . . . . .
N6 N 0.73369(18) 0.75269(17) 0.68777(15) 0.0375(3) Uani 1 1 d . . . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.03350(14) Uani 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.490(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.331(3) . ?
C2 C3 1.396(4) . ?
C3 C4 1.361(4) . ?
C3 H3 0.9300 . ?
C4 N4 1.348(3) . ?
C4 C5 1.493(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.496(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.329(3) . ?
C7 C8 1.388(3) . ?
C8 C9 1.366(3) . ?
C8 H8 0.9300 . ?
C9 N5 1.352(3) . ?
C9 C10 1.502(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.495(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.325(3) . ?
C12 C13 1.387(3) . ?
C13 C14 1.365(3) . ?
C13 H13 0.9300 . ?
C14 N6 1.341(3) . ?
C14 C15 1.493(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
B1 N5 1.538(3) . ?
B1 N4 1.543(3) . ?
B1 N6 1.549(3) . ?
B1 H1 0.9800 . ?
N1 N4 1.374(2) . ?
N1 Fe1 2.1893(16) . ?
N2 N5 1.373(2) . ?
N2 Fe1 2.1853(15) . ?
N3 N6 1.376(2) . ?
N3 Fe1 2.1597(16) . ?
Fe1 N3 2.1597(16) 2_666 ?
Fe1 N2 2.1853(15) 2_666 ?
Fe1 N1 2.1893(16) 2_666 ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 109.4(2) . . ?
N1 C2 C1 122.6(2) . . ?
C3 C2 C1 128.0(2) . . ?
C4 C3 C2 106.7(2) . . ?
C4 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
N4 C4 C3 107.5(2) . . ?
N4 C4 C5 122.7(3) . . ?
C3 C4 C5 129.8(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 109.7(2) . . ?
N2 C7 C6 122.01(19) . . ?
C8 C7 C6 128.3(2) . . ?
C9 C8 C7 106.56(19) . . ?
C9 C8 H8 126.7 . . ?
C7 C8 H8 126.7 . . ?
N5 C9 C8 107.50(19) . . ?
N5 C9 C10 123.2(2) . . ?
C8 C9 C10 129.3(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 109.79(19) . . ?
N3 C12 C11 122.2(2) . . ?
C13 C12 C11 127.9(2) . . ?
C14 C13 C12 106.34(19) . . ?
C14 C13 H13 126.8 . . ?
C12 C13 H13 126.8 . . ?
N6 C14 C13 107.77(18) . . ?
N6 C14 C15 123.7(2) . . ?
C13 C14 C15 128.6(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N5 B1 N4 108.65(17) . . ?
N5 B1 N6 110.32(16) . . ?
N4 B1 N6 110.12(16) . . ?
N5 B1 H1 109.2 . . ?
N4 B1 H1 109.2 . . ?
N6 B1 H1 109.2 . . ?
C2 N1 N4 106.56(17) . . ?
C2 N1 Fe1 136.66(16) . . ?
N4 N1 Fe1 115.69(12) . . ?
C7 N2 N5 106.75(16) . . ?
C7 N2 Fe1 136.58(14) . . ?
N5 N2 Fe1 116.67(12) . . ?
C12 N3 N6 106.49(16) . . ?
C12 N3 Fe1 137.27(14) . . ?
N6 N3 Fe1 116.00(11) . . ?
C4 N4 N1 109.86(19) . . ?
C4 N4 B1 129.84(19) . . ?
N1 N4 B1 120.30(15) . . ?
C9 N5 N2 109.51(17) . . ?
C9 N5 B1 130.54(17) . . ?
N2 N5 B1 119.87(15) . . ?
C14 N6 N3 109.60(15) . . ?
C14 N6 B1 129.51(16) . . ?
N3 N6 B1 120.87(15) . . ?
N3 Fe1 N3 180.0 2_666 . ?
N3 Fe1 N2 86.30(6) 2_666 2_666 ?
N3 Fe1 N2 93.70(6) . 2_666 ?
N3 Fe1 N2 93.70(6) 2_666 . ?
N3 Fe1 N2 86.30(6) . . ?
N2 Fe1 N2 180.0 2_666 . ?
N3 Fe1 N1 93.77(6) 2_666 . ?
N3 Fe1 N1 86.23(6) . . ?
N2 Fe1 N1 92.50(6) 2_666 . ?
N2 Fe1 N1 87.50(6) . . ?
N3 Fe1 N1 86.23(6) 2_666 2_666 ?
N3 Fe1 N1 93.77(6) . 2_666 ?
N2 Fe1 N1 87.50(6) 2_666 2_666 ?
N2 Fe1 N1 92.50(6) . 2_666 ?
N1 Fe1 N1 180.00(11) . 2_666 ?

_refine_diff_density_max         0.510
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.195

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_Fe_T253k_tetragonal
_database_code_depnum_ccdc_archive 'CCDC 1558086'
_audit_update_record             
;
2017-06-23 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H88 B4 Fe2 N24 O0'
_chemical_formula_weight         1300.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0031 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 0.0016 0.0007 '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'
Fe Fe 0.3460 0.8476 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_H-M_alt        'P -4 21 m'
_space_group_name_Hall           'P -4 2ab'

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

_cell_length_a                   20.669(5)
_cell_length_b                   20.669(5)
_cell_length_c                   8.603(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3675(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    253(2)
_cell_measurement_reflns_used    307
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      14.45

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             1376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.411
_shelx_estimated_absorpt_T_min   0.988
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9912
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_process_details   SADABS
_diffrn_ambient_temperature      253(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42038
_diffrn_reflns_av_unetI/netI     0.3063
_diffrn_reflns_av_R_equivalents  1.3178
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.203
_diffrn_reflns_theta_max         20.694
_diffrn_reflns_theta_full        20.694
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1998
_reflns_number_gt                712
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1091P)²+20.5174P] 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 170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.42(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1998
_refine_ls_number_parameters     117
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.3011
_refine_ls_R_factor_gt           0.1233
_refine_ls_wR_factor_ref         0.3314
_refine_ls_wR_factor_gt          0.2503
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.011 216 43 ' '
2 0.500 0.500 -0.015 216 43 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


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 0.7501(4) 0.2501(4) 0.7284(7) 0.059(2) Uani 1 2 d S T P . .
C1 C 0.9642(17) 0.298(2) 0.352(5) 0.086(6) Uani 1 1 d . . . . .
H1A H 0.986806 0.270592 0.279534 0.129 Uiso 1 1 calc R U . . .
H1B H 0.994348 0.314837 0.426430 0.129 Uiso 1 1 calc R U . . .
H1C H 0.943568 0.332438 0.297849 0.129 Uiso 1 1 calc R U . . .
N1 N 0.8292(15) 0.2252(17) 0.573(4) 0.086(6) Uani 1 1 d . . . . .
N2 N 0.8149(14) 0.3149(14) 0.846(6) 0.087(9) Uani 1 2 d S T P . .
C2 C 0.9150(18) 0.259(2) 0.434(5) 0.086(6) Uani 1 1 d . . . . .
N3 N 0.6786(14) 0.1786(14) 0.620(4) 0.039(6) Uani 1 2 d S T P . .
C3 C 0.9128(17) 0.190(2) 0.425(5) 0.086(6) Uani 1 1 d . . . . .
H3 H 0.940883 0.161561 0.373974 0.103 Uiso 1 1 calc R U . . .
N4 N 0.6728(15) 0.2716(15) 0.893(3) 0.066(5) Uani 1 1 d . . . . .
C4 C 0.858(2) 0.175(2) 0.511(6) 0.086(6) Uani 1 1 d . . . . .
C5 C 0.8322(17) 0.1084(18) 0.544(5) 0.086(6) Uani 1 1 d . . . . .
H5A H 0.798134 0.111157 0.619746 0.129 Uiso 1 1 calc R U . . .
H5B H 0.866354 0.081550 0.583954 0.129 Uiso 1 1 calc R U . . .
H5C H 0.815638 0.089900 0.449952 0.129 Uiso 1 1 calc R U . . .
B1 B 0.848(3) 0.348(3) 0.554(10) 0.090(18) Uani 1 2 d S TU P . .
H1 H 0.877519 0.377520 0.503589 0.108 Uiso 1 2 calc R U P . .
C7 C 0.8959(16) 0.3959(16) 0.829(8) 0.087(9) Uani 1 2 d S T P . .
N7 N 0.8666(16) 0.2787(16) 0.528(4) 0.086(6) Uani 1 1 d . U . . .
B2 B 0.650(2) 0.150(2) 0.884(6) 0.030(13) Uani 1 2 d S TU P . .
H2 H 0.620362 0.120361 0.935544 0.036 Uiso 1 2 calc R U P . .
C6 C 0.9399(17) 0.4399(17) 0.779(6) 0.087(9) Uani 1 2 d S T P . .
H6A H 0.967345 0.452341 0.863488 0.131 Uiso 0.5 1 calc R U P . .
H6B H 0.917827 0.477361 0.739235 0.131 Uiso 0.5 1 calc R U P . .
H6C H 0.965732 0.421201 0.697373 0.131 Uiso 0.5 1 calc R U P . .
N9 N 0.6360(16) 0.2222(14) 0.954(4) 0.066(5) Uani 1 1 d . U . . .
C9 C 0.8364(17) 0.3364(17) 0.995(8) 0.087(9) Uani 1 2 d S T P . .
N8 N 0.8522(15) 0.3522(15) 0.739(6) 0.087(9) Uani 1 2 d S TU P . .
C8 C 0.8828(17) 0.3828(17) 0.969(8) 0.087(9) Uani 1 2 d S T P . .
H8 H 0.903724 0.403724 1.050293 0.105 Uiso 1 2 calc R U P . .
N10 N 0.6420(15) 0.1420(15) 0.724(4) 0.039(6) Uani 1 2 d S TU P . .
C10 C 0.8012(15) 0.3012(15) 1.124(6) 0.087(9) Uani 1 2 d S T P . .
H10A H 0.755990 0.298481 1.098716 0.131 Uiso 0.5 1 calc R U P . .
H10B H 0.806510 0.324280 1.219678 0.131 Uiso 0.5 1 calc R U P . .
H10C H 0.818618 0.258358 1.134385 0.131 Uiso 0.5 1 calc R U P . .
C11 C 0.6786(17) 0.3933(16) 0.919(4) 0.066(5) Uani 1 1 d . . . . .
H11A H 0.721106 0.386897 0.875980 0.098 Uiso 1 1 calc R U . . .
H11B H 0.681823 0.417395 1.013565 0.098 Uiso 1 1 calc R U . . .
H11C H 0.652537 0.416724 0.845477 0.098 Uiso 1 1 calc R U . . .
C12 C 0.6482(19) 0.329(2) 0.951(5) 0.066(5) Uani 1 1 d . . . . .
C13 C 0.5962(18) 0.3119(18) 1.040(5) 0.066(5) Uani 1 1 d . . . . .
H13 H 0.570999 0.341021 1.096097 0.079 Uiso 1 1 calc R U . . .
C14 C 0.5864(18) 0.249(2) 1.037(4) 0.066(5) Uani 1 1 d . . . . .
C15 C 0.5365(17) 0.2023(18) 1.103(4) 0.066(5) Uani 1 1 d . . . . .
H15A H 0.529245 0.212125 1.211128 0.098 Uiso 1 1 calc R U . . .
H15B H 0.552344 0.158832 1.093944 0.098 Uiso 1 1 calc R U . . .
H15C H 0.496620 0.206462 1.047183 0.098 Uiso 1 1 calc R U . . .
C16 C 0.6976(16) 0.1976(16) 0.332(4) 0.039(6) Uani 1 2 d S T P . .
H16A H 0.668940 0.230264 0.293089 0.058 Uiso 0.5 1 calc R U P . .
H16B H 0.701531 0.163398 0.257513 0.058 Uiso 0.5 1 calc R U P . .
H16C H 0.739378 0.216189 0.351592 0.058 Uiso 0.5 1 calc R U P . .
C17 C 0.6707(17) 0.1707(17) 0.482(5) 0.039(6) Uani 1 2 d S T P . .
C18 C 0.6196(16) 0.1196(16) 0.472(5) 0.039(6) Uani 1 2 d S T P . .
H18 H 0.600458 0.100458 0.385814 0.047 Uiso 1 2 calc R U P . .
C19 C 0.6101(17) 0.1101(17) 0.617(5) 0.039(6) Uani 1 2 d S T P . .
C20 C 0.5585(18) 0.0585(18) 0.726(4) 0.039(6) Uani 1 2 d S T P . .
H20A H 0.538364 0.082743 0.807561 0.058 Uiso 0.5 1 calc R U P . .
H20B H 0.583415 0.023821 0.769494 0.058 Uiso 0.5 1 calc R U P . .
H20C H 0.525780 0.040994 0.658459 0.058 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.15(5) . ?
Fe1 N1 2.18(3) 8_545 ?
Fe1 N1 2.18(3) . ?
Fe1 N4 2.18(3) 8_545 ?
Fe1 N4 2.18(3) . ?
Fe1 N3 2.29(4) . ?
C1 C2 1.47(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
N1 C4 1.31(5) . ?
N1 N7 1.40(4) . ?
N2 N8 1.43(6) . ?
N2 C9 1.43(7) . ?
C2 N7 1.35(5) . ?
C2 C3 1.44(6) . ?
N3 C17 1.21(5) . ?
N3 N10 1.39(5) . ?
C3 C4 1.38(5) . ?
C3 H3 0.9300 . ?
N4 N9 1.38(3) . ?
N4 C12 1.38(5) . ?
C4 C5 1.51(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
B1 N7 1.49(5) . ?
B1 N7 1.49(5) 8_545 ?
B1 N8 1.59(8) . ?
B1 H1 0.9800 . ?
C7 C8 1.26(7) . ?
C7 C6 1.36(6) . ?
C7 N8 1.49(7) . ?
B2 N10 1.40(5) . ?
B2 N9 1.63(4) . ?
B2 N9 1.63(4) 8_545 ?
B2 H2 0.9800 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N9 C14 1.37(4) . ?
C9 C8 1.38(7) . ?
C9 C10 1.51(7) . ?
C8 H8 0.9300 . ?
N10 C19 1.31(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 H10A 1.0(4) 8_545 ?
C10 H10B 0.96(6) 8_545 ?
C10 H10C 0.96(5) 8_545 ?
C11 C12 1.49(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.37(4) . ?
C13 C14 1.31(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.53(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.51(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16A 0.96(4) 8_545 ?
C16 H16B 0.96(4) 8_545 ?
C16 H16C 1.0(3) 8_545 ?
C17 C18 1.50(6) . ?
C18 C19 1.28(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.77(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20 H20A 0.96(15) 8_545 ?
C20 H20B 0.96(8) 8_545 ?
C20 H20C 1.0(3) 8_545 ?

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 N1 88.2(14) . 8_545 ?
N2 Fe1 N1 88.2(14) . . ?
N1 Fe1 N1 88.6(18) 8_545 . ?
N2 Fe1 N4 91.4(12) . 8_545 ?
N1 Fe1 N4 177.1(15) 8_545 8_545 ?
N1 Fe1 N4 94.3(8) . 8_545 ?
N2 Fe1 N4 91.4(12) . . ?
N1 Fe1 N4 94.3(8) 8_545 . ?
N1 Fe1 N4 177.1(15) . . ?
N4 Fe1 N4 82.9(16) 8_545 . ?
N2 Fe1 N3 176.0(19) . . ?
N1 Fe1 N3 94.7(11) 8_545 . ?
N1 Fe1 N3 94.7(11) . . ?
N4 Fe1 N3 85.6(12) 8_545 . ?
N4 Fe1 N3 85.6(12) . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 N1 N7 105(3) . . ?
C4 N1 Fe1 141(3) . . ?
N7 N1 Fe1 113(2) . . ?
N8 N2 C9 104(4) . . ?
N8 N2 Fe1 112(4) . . ?
C9 N2 Fe1 144(4) . . ?
N7 C2 C3 108(4) . . ?
N7 C2 C1 129(4) . . ?
C3 C2 C1 122(4) . . ?
C17 N3 N10 119(4) . . ?
C17 N3 Fe1 125(4) . . ?
N10 N3 Fe1 116(2) . . ?
C4 C3 C2 102(4) . . ?
C4 C3 H3 128.9 . . ?
C2 C3 H3 128.9 . . ?
N9 N4 C12 108(3) . . ?
N9 N4 Fe1 120(2) . . ?
C12 N4 Fe1 132(2) . . ?
N1 C4 C3 115(4) . . ?
N1 C4 C5 119(4) . . ?
C3 C4 C5 126(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N7 B1 N7 119(6) . 8_545 ?
N7 B1 N8 101(4) . . ?
N7 B1 N8 101(4) 8_545 . ?
N7 B1 H1 111.5 . . ?
N7 B1 H1 111.5 8_545 . ?
N8 B1 H1 111.5 . . ?
C8 C7 C6 126(6) . . ?
C8 C7 N8 104(5) . . ?
C6 C7 N8 130(6) . . ?
C2 N7 N1 110(4) . . ?
C2 N7 B1 125(5) . . ?
N1 N7 B1 124(4) . . ?
N10 B2 N9 117(3) . . ?
N10 B2 N9 117(3) . 8_545 ?
N9 B2 N9 101(4) . 8_545 ?
N10 B2 H2 107.1 . . ?
N9 B2 H2 107.1 . . ?
N9 B2 H2 107.1 8_545 . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C14 N9 N4 108(3) . . ?
C14 N9 B2 134(4) . . ?
N4 N9 B2 116(3) . . ?
C8 C9 N2 106(6) . . ?
C8 C9 C10 143(7) . . ?
N2 C9 C10 111(4) . . ?
N2 N8 C7 109(5) . . ?
N2 N8 B1 125(5) . . ?
C7 N8 B1 126(5) . . ?
C7 C8 C9 117(7) . . ?
C7 C8 H8 121.4 . . ?
C9 C8 H8 121.4 . . ?
C19 N10 N3 96(3) . . ?
C19 N10 B2 144(5) . . ?
N3 N10 B2 120(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C10 H10A 109(4) . 8_545 ?
H10A C10 H10A 80.6 . 8_545 ?
H10B C10 H10A 133.1 . 8_545 ?
H10C C10 H10A 31.4 . 8_545 ?
C9 C10 H10B 109(10) . 8_545 ?
H10A C10 H10B 133.1 . 8_545 ?
H10B C10 H10B 31.4 . 8_545 ?
H10C C10 H10B 80.6 . 8_545 ?
H10A C10 H10B 109.5 8_545 8_545 ?
C9 C10 H10C 109(5) . 8_545 ?
H10A C10 H10C 31.4 . 8_545 ?
H10B C10 H10C 80.6 . 8_545 ?
H10C C10 H10C 133.1 . 8_545 ?
H10A C10 H10C 109.5 8_545 8_545 ?
H10B C10 H10C 109.5 8_545 8_545 ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N4 105(3) . . ?
C13 C12 C11 132(4) . . ?
N4 C12 C11 123(3) . . ?
C14 C13 C12 111(4) . . ?
C14 C13 H13 124.3 . . ?
C12 C13 H13 124.3 . . ?
C13 C14 N9 107(3) . . ?
C13 C14 C15 136(4) . . ?
N9 C14 C15 116(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5(17) . 8_545 ?
H16A C16 H16A 138.0 . 8_545 ?
H16B C16 H16A 41.4 . 8_545 ?
H16C C16 H16A 71.0 . 8_545 ?
C17 C16 H16B 109(6) . 8_545 ?
H16A C16 H16B 41.4 . 8_545 ?
H16B C16 H16B 71.0 . 8_545 ?
H16C C16 H16B 138.0 . 8_545 ?
H16A C16 H16B 109.5 8_545 8_545 ?
C17 C16 H16C 109(2) . 8_545 ?
H16A C16 H16C 71.0 . 8_545 ?
H16B C16 H16C 138.0 . 8_545 ?
H16C C16 H16C 41.4 . 8_545 ?
H16A C16 H16C 109.5 8_545 8_545 ?
H16B C16 H16C 109.5 8_545 8_545 ?
N3 C17 C18 104(4) . . ?
N3 C17 C16 138(5) . . ?
C18 C17 C16 118(4) . . ?
C19 C18 C17 99(4) . . ?
C19 C18 H18 130.3 . . ?
C17 C18 H18 130.3 . . ?
C18 C19 N10 122(5) . . ?
C18 C19 C20 134(4) . . ?
N10 C19 C20 104(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C20 H20A 109(10) . 8_545 ?
H20A C20 H20A 85.0 . 8_545 ?
H20B C20 H20A 26.8 . 8_545 ?
H20C C20 H20A 130.3 . 8_545 ?
C19 C20 H20B 109(7) . 8_545 ?
H20A C20 H20B 26.8 . 8_545 ?
H20B C20 H20B 130.3 . 8_545 ?
H20C C20 H20B 85.0 . 8_545 ?
H20A C20 H20B 109.5 8_545 8_545 ?
C19 C20 H20C 109(10) . 8_545 ?
H20A C20 H20C 130.3 . 8_545 ?
H20B C20 H20C 85.0 . 8_545 ?
H20C C20 H20C 26.8 . 8_545 ?
H20A C20 H20C 109.5 8_545 8_545 ?
H20B C20 H20C 109.5 8_545 8_545 ?

_refine_diff_density_max         1.035
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.084




