# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

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

data_rk116f_2
_database_code_depnum_ccdc_archive 'CCDC 1430803'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2'
_chemical_formula_sum            'C30 H16 Fe N10 S2'
_chemical_formula_weight         636.50

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   7.7346(7)
_cell_length_b                   14.8899(13)
_cell_length_c                   23.801(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.674(9)
_cell_angle_gamma                90.00
_cell_volume                     2731.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1999
_cell_measurement_theta_min      4.06
_cell_measurement_theta_max      26.42

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8075
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         28.72
_reflns_number_total             2967
_reflns_number_gt                2147
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a molecule, with Fe1 lying on the 
 crystallographic C₂ axis 0, y, 3/4. The C and S atoms of the unique 
 NCS⁻ ligand are disordered over two orientations, whose occupancies 
 refined to 0.60:0.40. These were modelled without restraints. All non-H 
 atoms except the minor ligand disorder site were refined anisotropically,
 while H atoms were placed in calculated positions and refined using a riding 
 model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0312P)²+3.8808P] 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         2967
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.92729(4) 0.2500 0.02868(18) Uani 1 2 d S . .
N2 N 0.1301(3) 0.83585(16) 0.21398(10) 0.0328(6) Uani 1 1 d . . .
C3A C 0.1805(17) 0.7810(8) 0.1831(5) 0.021(2) Uani 0.60 1 d P A 1
S4A S 0.2504(2) 0.70498(9) 0.14224(7) 0.0276(3) Uani 0.60 1 d P A 1
C3B C 0.204(3) 0.7852(15) 0.1921(8) 0.024(5) Uiso 0.40 1 d P A 2
S4B S 0.3071(4) 0.7101(2) 0.15709(12) 0.0404(9) Uiso 0.40 1 d P A 2
C5 C -0.1082(4) 0.98354(19) 0.14044(12) 0.0319(7) Uani 1 1 d . A .
N6 N -0.1609(3) 0.92927(16) 0.18174(10) 0.0327(6) Uani 1 1 d . . .
C7 C -0.3044(4) 0.8807(2) 0.16911(14) 0.0428(8) Uani 1 1 d . A .
H7 H -0.3436 0.8418 0.1970 0.051 Uiso 1 1 calc R . .
C8 C -0.3973(5) 0.8848(2) 0.11743(16) 0.0543(10) Uani 1 1 d . . .
H8 H -0.4969 0.8480 0.1102 0.065 Uiso 1 1 calc R A .
C9 C -0.3477(5) 0.9413(2) 0.07633(15) 0.0521(9) Uani 1 1 d . A .
H9 H -0.4135 0.9455 0.0409 0.063 Uiso 1 1 calc R . .
C10 C -0.1970(4) 0.9929(2) 0.08786(13) 0.0388(7) Uani 1 1 d . . .
C11 C 0.0486(4) 1.03240(18) 0.15579(12) 0.0313(7) Uani 1 1 d . . .
N12 N 0.1206(3) 1.01871(15) 0.20882(10) 0.0303(6) Uani 1 1 d . A .
C13 C 0.2609(4) 1.0656(2) 0.22561(14) 0.0393(7) Uani 1 1 d . . .
H13 H 0.3115 1.0577 0.2630 0.047 Uiso 1 1 calc R A .
C14 C 0.3367(4) 1.1259(2) 0.19033(15) 0.0461(8) Uani 1 1 d . A .
H14 H 0.4373 1.1584 0.2039 0.055 Uiso 1 1 calc R . .
C15 C 0.2679(4) 1.1385(2) 0.13700(15) 0.0464(9) Uani 1 1 d . . .
H15 H 0.3209 1.1786 0.1125 0.056 Uiso 1 1 calc R A .
C16 C 0.1168(4) 1.0915(2) 0.11815(13) 0.0380(8) Uani 1 1 d . A .
C17 C -0.1297(5) 1.0560(2) 0.04833(14) 0.0450(8) Uani 1 1 d . A .
N18 N -0.2184(4) 1.0683(2) -0.00189(12) 0.0572(8) Uani 1 1 d . . .
C19 C -0.1530(6) 1.1281(3) -0.03538(16) 0.0688(12) Uani 1 1 d . A .
H19 H -0.2112 1.1386 -0.0715 0.083 Uiso 1 1 calc R . .
C20 C -0.0033(6) 1.1761(3) -0.01996(18) 0.0696(12) Uani 1 1 d . . .
H20 H 0.0352 1.2191 -0.0457 0.084 Uiso 1 1 calc R A .
N21 N 0.0882(4) 1.1649(2) 0.02855(13) 0.0581(9) Uani 1 1 d . A .
C22 C 0.0242(5) 1.1042(2) 0.06375(14) 0.0439(8) 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 1.934(2) . ?
Fe1 N12 1.958(2) . ?
Fe1 N6 1.964(2) . ?
N2 C3B 1.10(2) . ?
N2 C3A 1.187(13) . ?
C3A S4A 1.613(13) . ?
C3B S4B 1.64(2) . ?
C5 N6 1.360(4) . ?
C5 C10 1.385(4) . ?
C5 C11 1.436(4) . ?
N6 C7 1.338(4) . ?
C7 C8 1.374(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.369(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(5) . ?
C9 H9 0.9500 . ?
C10 C17 1.455(4) . ?
C11 N12 1.353(4) . ?
C11 C16 1.390(4) . ?
N12 C13 1.324(4) . ?
C13 C14 1.392(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.349(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.404(5) . ?
C15 H15 0.9500 . ?
C16 C22 1.440(5) . ?
C17 N18 1.341(4) . ?
C17 C22 1.413(5) . ?
N18 C19 1.323(5) . ?
C19 C20 1.385(6) . ?
C19 H19 0.9500 . ?
C20 N21 1.314(5) . ?
C20 H20 0.9500 . ?
N21 C22 1.353(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 90.51(14) 2 . ?
N2 Fe1 N12 88.93(9) . . ?
N2 Fe1 N12 176.00(10) . 2 ?
N12 Fe1 N12 91.89(13) . 2 ?
N2 Fe1 N6 93.43(10) . 2 ?
N12 Fe1 N6 96.21(10) . 2 ?
N2 Fe1 N6 87.78(10) . . ?
N12 Fe1 N6 82.59(10) . . ?
N6 Fe1 N6 178.28(14) 2 . ?
C3B N2 Fe1 178.0(11) . . ?
C3A N2 Fe1 165.6(7) . . ?
N2 C3A S4A 178.7(11) . . ?
N2 C3B S4B 177.3(16) . . ?
N6 C5 C10 123.8(3) . . ?
N6 C5 C11 114.4(3) . . ?
C10 C5 C11 121.7(3) . . ?
C7 N6 C5 116.8(3) . . ?
C7 N6 Fe1 129.5(2) . . ?
C5 N6 Fe1 113.56(19) . . ?
N6 C7 C8 122.7(3) . . ?
N6 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C9 C8 C7 120.7(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 118.2(3) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C5 C10 C9 117.7(3) . . ?
C5 C10 C17 118.2(3) . . ?
C9 C10 C17 124.2(3) . . ?
N12 C11 C16 123.2(3) . . ?
N12 C11 C5 115.8(2) . . ?
C16 C11 C5 120.9(3) . . ?
C13 N12 C11 117.8(3) . . ?
C13 N12 Fe1 128.9(2) . . ?
C11 N12 Fe1 113.30(18) . . ?
N12 C13 C14 122.2(3) . . ?
N12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.0(3) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C11 C16 C15 117.4(3) . . ?
C11 C16 C22 118.4(3) . . ?
C15 C16 C22 124.2(3) . . ?
N18 C17 C22 121.4(3) . . ?
N18 C17 C10 118.7(3) . . ?
C22 C17 C10 119.9(3) . . ?
C19 N18 C17 115.9(4) . . ?
N18 C19 C20 122.7(4) . . ?
N18 C19 H19 118.7 . . ?
C20 C19 H19 118.7 . . ?
N21 C20 C19 123.1(4) . . ?
N21 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
C20 N21 C22 115.5(4) . . ?
N21 C22 C17 121.4(3) . . ?
N21 C22 C16 117.6(3) . . ?
C17 C22 C16 120.9(3) . . ?

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
C8 H8 S4A 0.95 3.03 3.899(4) 152.9 1_455
C8 H8 S4B 0.95 2.83 3.638(5) 142.9 1_455
C14 H14 S4A 0.95 3.01 3.679(4) 128.4 3
C14 H14 S4B 0.95 3.25 3.989(4) 136.5 3
C19 H19 S4A 0.95 2.88 3.592(4) 133.0 5_575
C19 H19 S4B 0.95 3.09 3.880(5) 142.0 5_575

_diffrn_measured_fraction_theta_max 0.837
_diffrn_reflns_theta_full        28.72
_diffrn_measured_fraction_theta_full 0.837
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.066
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_rk116frt
_database_code_depnum_ccdc_archive 'CCDC 1430804'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2'
_chemical_formula_sum            'C30 H16 Fe N10 S2'
_chemical_formula_weight         636.50

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   7.7581(14)
_cell_length_b                   15.139(3)
_cell_length_c                   23.695(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.796(18)
_cell_angle_gamma                90.00
_cell_volume                     2776.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    1229
_cell_measurement_theta_min      4.35
_cell_measurement_theta_max      22.67

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.989
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6710
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         28.68
_reflns_number_total             2944
_reflns_number_gt                1913
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a molecule, with Fe1 lying on the 
 crystallographic C₂ axis 0, y, 1/4. The C and S atoms of the unique 
 NCS⁻ ligand are disordered over two orientations, whose occupancies 
 refined to 0.58:0.42. Hence, these were modelled without restraints, 
 using a 0.60:0.40 occupancy ratio (the same as in the low-temperature 
 structure). These were modelled without restraints. High displacement 
 ellipsoids on some atoms of the dpq ligand imply that these might also 
 be librationally disordered, but this was not refined. All non-H atoms 
 except the minor ligand disorder site were refined anisotropically, while 
 H atoms were placed in calculated positions and refined using a riding 
 model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0364P)²+3.1599P] 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         2944
_refine_ls_number_parameters     204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1217
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.92838(4) 0.2500 0.0472(2) Uani 1 2 d S . .
N2 N 0.1302(4) 0.83857(19) 0.21356(13) 0.0602(8) Uani 1 1 d . . .
C3A C 0.187(2) 0.7861(11) 0.1834(6) 0.044(3) Uani 0.60 1 d P A 1
S4A S 0.2561(3) 0.70719(12) 0.14445(9) 0.0603(5) Uani 0.60 1 d P A 1
C3B C 0.201(4) 0.7829(19) 0.1943(9) 0.043(6) Uiso 0.40 1 d P A 2
S4B S 0.3163(5) 0.7128(3) 0.16174(16) 0.0759(14) Uiso 0.40 1 d P A 2
C5 C -0.1091(4) 0.9858(2) 0.14059(14) 0.0486(8) Uani 1 1 d . A .
N6 N -0.1605(3) 0.93185(17) 0.18156(11) 0.0518(7) Uani 1 1 d . . .
C7 C -0.3036(5) 0.8852(3) 0.16997(17) 0.0725(11) Uani 1 1 d . A .
H7 H -0.3422 0.8476 0.1975 0.087 Uiso 1 1 calc R . .
C8 C -0.3963(6) 0.8906(3) 0.1187(2) 0.0928(15) Uani 1 1 d . . .
H8 H -0.4938 0.8554 0.1120 0.111 Uiso 1 1 calc R A .
C9 C -0.3483(6) 0.9462(3) 0.07781(18) 0.0844(13) Uani 1 1 d . A .
H9 H -0.4136 0.9510 0.0436 0.101 Uiso 1 1 calc R . .
C10 C -0.1979(5) 0.9965(2) 0.08828(15) 0.0608(9) Uani 1 1 d . . .
C11 C 0.0488(4) 1.03339(19) 0.15524(14) 0.0464(8) Uani 1 1 d . . .
N12 N 0.1201(3) 1.01905(16) 0.20775(11) 0.0468(6) Uani 1 1 d . A .
C13 C 0.2610(5) 1.0645(2) 0.22321(17) 0.0638(10) Uani 1 1 d . . .
H13 H 0.3115 1.0564 0.2595 0.077 Uiso 1 1 calc R A .
C14 C 0.3362(5) 1.1231(3) 0.18806(19) 0.0791(12) Uani 1 1 d . A .
H14 H 0.4354 1.1535 0.2008 0.095 Uiso 1 1 calc R . .
C15 C 0.2668(5) 1.1368(3) 0.13515(19) 0.0727(11) Uani 1 1 d . . .
H15 H 0.3184 1.1757 0.1110 0.087 Uiso 1 1 calc R A .
C16 C 0.1151(5) 1.0912(2) 0.11695(15) 0.0568(9) Uani 1 1 d . A .
C17 C -0.1318(5) 1.0583(3) 0.04856(15) 0.0656(10) Uani 1 1 d . A .
N18 N -0.2209(5) 1.0710(3) -0.00095(15) 0.0893(11) Uani 1 1 d . . .
C19 C -0.1552(8) 1.1291(4) -0.0347(2) 0.1098(18) Uani 1 1 d . A .
H19 H -0.2125 1.1394 -0.0698 0.132 Uiso 1 1 calc R . .
C20 C -0.0059(8) 1.1756(4) -0.0207(2) 0.1054(17) Uani 1 1 d . . .
H20 H 0.0318 1.2167 -0.0464 0.126 Uiso 1 1 calc R A .
N21 N 0.0859(5) 1.1641(2) 0.02756(16) 0.0888(11) Uani 1 1 d . A .
C22 C 0.0228(5) 1.1047(2) 0.06278(16) 0.0631(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.931(3) . ?
Fe1 N12 1.969(3) . ?
Fe1 N6 1.979(3) . ?
N2 C3B 1.12(3) . ?
N2 C3A 1.174(18) . ?
C3A S4A 1.622(18) . ?
C3B S4B 1.62(3) . ?
C5 N6 1.349(4) . ?
C5 C10 1.387(4) . ?
C5 C11 1.444(4) . ?
N6 C7 1.330(4) . ?
C7 C8 1.371(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.355(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.401(5) . ?
C9 H9 0.9300 . ?
C10 C17 1.445(5) . ?
C11 N12 1.345(4) . ?
C11 C16 1.384(4) . ?
N12 C13 1.323(4) . ?
C13 C14 1.373(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.347(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.407(5) . ?
C15 H15 0.9300 . ?
C16 C22 1.442(5) . ?
C17 N18 1.336(5) . ?
C17 C22 1.411(5) . ?
N18 C19 1.314(6) . ?
C19 C20 1.376(7) . ?
C19 H19 0.9300 . ?
C20 N21 1.318(6) . ?
C20 H20 0.9300 . ?
N21 C22 1.341(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 90.49(17) 2 . ?
N2 Fe1 N12 175.61(12) . 2 ?
N2 Fe1 N12 89.11(11) . . ?
N12 Fe1 N12 91.62(15) 2 . ?
N2 Fe1 N6 88.37(12) . . ?
N12 Fe1 N6 81.84(11) . . ?
N2 Fe1 N6 93.78(12) . 2 ?
N12 Fe1 N6 96.02(11) . 2 ?
N6 Fe1 N6 176.96(15) . 2 ?
C3B N2 Fe1 175.9(13) . . ?
C3A N2 Fe1 167.8(9) . . ?
N2 C3A S4A 175.1(13) . . ?
N2 C3B S4B 172(2) . . ?
N6 C5 C10 124.1(3) . . ?
N6 C5 C11 114.5(3) . . ?
C10 C5 C11 121.3(3) . . ?
C7 N6 C5 117.1(3) . . ?
C7 N6 Fe1 128.8(3) . . ?
C5 N6 Fe1 114.0(2) . . ?
N6 C7 C8 122.2(4) . . ?
N6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C9 C8 C7 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 118.4(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
C5 C10 C9 116.9(4) . . ?
C5 C10 C17 118.8(3) . . ?
C9 C10 C17 124.3(4) . . ?
N12 C11 C16 124.1(3) . . ?
N12 C11 C5 115.6(3) . . ?
C16 C11 C5 120.3(3) . . ?
C13 N12 C11 117.0(3) . . ?
C13 N12 Fe1 129.2(2) . . ?
C11 N12 Fe1 113.8(2) . . ?
N12 C13 C14 123.0(4) . . ?
N12 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 119.0(4) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C11 C16 C15 116.7(3) . . ?
C11 C16 C22 119.3(3) . . ?
C15 C16 C22 124.0(3) . . ?
N18 C17 C22 121.4(4) . . ?
N18 C17 C10 118.7(4) . . ?
C22 C17 C10 119.9(3) . . ?
C19 N18 C17 115.6(4) . . ?
N18 C19 C20 123.4(5) . . ?
N18 C19 H19 118.3 . . ?
C20 C19 H19 118.3 . . ?
N21 C20 C19 122.6(5) . . ?
N21 C20 H20 118.7 . . ?
C19 C20 H20 118.7 . . ?
C20 N21 C22 115.5(4) . . ?
N21 C22 C17 121.6(4) . . ?
N21 C22 C16 118.0(4) . . ?
C17 C22 C16 120.4(3) . . ?

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
C8 H8 S4A 0.93 3.10 3.946(5) 152.6 1_455
C8 H8 S4B 0.93 2.91 3.682(6) 141.5 1_455
C14 H14 S4A 0.93 3.01 3.707(5) 132.8 3
C14 H14 S4B 0.93 3.28 4.051(6) 141.7 3
C19 H19 S4A 0.93 2.93 3.640(5) 134.7 5_575
C19 H19 S4B 0.93 3.19 3.982(6) 144.4 5_575

_diffrn_measured_fraction_theta_max 0.818
_diffrn_reflns_theta_full        28.68
_diffrn_measured_fraction_theta_full 0.818
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.050
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_rk89alt
_database_code_depnum_ccdc_archive 'CCDC 1430805'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[iso-thiocyanato][dipyrido[3,2-a:23-c]phenazine]-iron(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H20 Fe N10 S2'
_chemical_formula_sum            'C38 H20 Fe N10 S2'
_chemical_formula_weight         736.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   7.9867(4)
_cell_length_b                   14.6323(6)
_cell_length_c                   28.1005(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.360(5)
_cell_angle_gamma                90.00
_cell_volume                     3278.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2153
_cell_measurement_theta_min      6.32
_cell_measurement_theta_max      73.58

_exptl_crystal_description       fragment
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    5.259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5461
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         73.95
_reflns_number_total             3181
_reflns_number_gt                2691
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a molecule, with Fe1 lying on the 
 crystallographic C₂ axis 0, y, 3/4. No disorder is present in the model,
 and no restraints were applied. All non-H atoms were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. The highest residual Fourier peak of 
 +1.3 e.Å⁻³ is 0.9 Å from S4, and may represent a minor disorder 
 site for the thiocyanate residue.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0887P)²+2.3948P] 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         3181
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1599
_refine_ls_wR_factor_gt          0.1497
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.37856(4) 0.7500 0.0264(2) Uani 1 2 d S . .
N2 N 0.1255(4) 0.28540(19) 0.71842(11) 0.0337(6) Uani 1 1 d . . .
C3 C 0.1811(4) 0.2317(2) 0.69388(12) 0.0303(7) Uani 1 1 d . . .
S4 S 0.25430(15) 0.15336(7) 0.65922(4) 0.0521(3) Uani 1 1 d . . .
C5 C -0.1033(4) 0.4324(2) 0.65747(11) 0.0278(6) Uani 1 1 d . . .
N6 N -0.1559(3) 0.37922(17) 0.69313(10) 0.0287(6) Uani 1 1 d . . .
C7 C -0.2915(4) 0.3266(2) 0.68418(13) 0.0348(7) Uani 1 1 d . . .
H7 H -0.3298 0.2891 0.7089 0.042 Uiso 1 1 calc R . .
C8 C -0.3779(5) 0.3255(2) 0.63965(15) 0.0405(8) Uani 1 1 d . . .
H8 H -0.4723 0.2866 0.6341 0.049 Uiso 1 1 calc R . .
C9 C -0.3264(5) 0.3807(2) 0.60366(14) 0.0387(8) Uani 1 1 d . . .
H9 H -0.3846 0.3804 0.5732 0.046 Uiso 1 1 calc R . .
C10 C -0.1864(4) 0.4375(2) 0.61269(12) 0.0319(7) Uani 1 1 d . . .
C11 C 0.0455(4) 0.4852(2) 0.66929(11) 0.0262(6) Uani 1 1 d . . .
N12 N 0.1160(3) 0.47194(17) 0.71386(9) 0.0260(5) Uani 1 1 d . . .
C13 C 0.2530(4) 0.5202(2) 0.72709(11) 0.0296(6) Uani 1 1 d . . .
H13 H 0.3029 0.5123 0.7583 0.036 Uiso 1 1 calc R . .
C14 C 0.3247(4) 0.5816(2) 0.69641(13) 0.0355(7) Uani 1 1 d . . .
H14 H 0.4228 0.6144 0.7068 0.043 Uiso 1 1 calc R . .
C15 C 0.2540(4) 0.5950(2) 0.65097(12) 0.0313(7) Uani 1 1 d . . .
H15 H 0.3029 0.6363 0.6297 0.038 Uiso 1 1 calc R . .
C16 C 0.1089(4) 0.5464(2) 0.63692(11) 0.0291(6) Uani 1 1 d . . .
C17 C -0.1277(4) 0.5032(2) 0.57833(11) 0.0315(7) Uani 1 1 d . . .
N18 N -0.2130(4) 0.5116(2) 0.53688(10) 0.0360(6) Uani 1 1 d . . .
C19 C -0.1634(5) 0.5781(3) 0.50726(13) 0.0383(8) Uani 1 1 d . . .
C20 C -0.0272(4) 0.6373(3) 0.52108(13) 0.0370(8) Uani 1 1 d . . .
N21 N 0.0640(4) 0.6259(2) 0.56265(10) 0.0340(6) Uani 1 1 d . . .
C22 C 0.0159(4) 0.5596(2) 0.59077(11) 0.0307(7) Uani 1 1 d . . .
C23 C -0.2501(5) 0.5899(3) 0.46234(14) 0.0453(9) Uani 1 1 d . . .
H23 H -0.3386 0.5495 0.4525 0.054 Uiso 1 1 calc R . .
C24 C -0.2064(5) 0.6593(3) 0.43321(14) 0.0490(10) Uani 1 1 d . . .
H24 H -0.2641 0.6667 0.4029 0.059 Uiso 1 1 calc R . .
C25 C -0.0761(5) 0.7203(3) 0.44766(14) 0.0481(10) Uani 1 1 d . . .
H25 H -0.0500 0.7696 0.4273 0.058 Uiso 1 1 calc R . .
C26 C 0.0133(5) 0.7099(3) 0.49031(14) 0.0441(9) Uani 1 1 d . . .
H26 H 0.1018 0.7509 0.4993 0.053 Uiso 1 1 calc R . .


_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 1.938(3) . ?
Fe1 N12 1.966(3) . ?
Fe1 N6 1.968(3) . ?
N2 C3 1.151(5) . ?
C3 S4 1.634(3) . ?
C5 N6 1.355(4) . ?
C5 C10 1.390(5) . ?
C5 C11 1.440(4) . ?
N6 C7 1.340(4) . ?
C7 C8 1.393(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.404(5) . ?
C9 H9 0.9500 . ?
C10 C17 1.460(5) . ?
C11 N12 1.357(4) . ?
C11 C16 1.392(5) . ?
N12 C13 1.337(4) . ?
C13 C14 1.391(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(5) . ?
C15 H15 0.9500 . ?
C16 C22 1.469(5) . ?
C17 N18 1.320(4) . ?
C17 C22 1.439(5) . ?
N18 C19 1.355(5) . ?
C19 C23 1.414(5) . ?
C19 C20 1.426(6) . ?
C20 N21 1.350(5) . ?
C20 C26 1.419(6) . ?
N21 C22 1.322(5) . ?
C23 C24 1.363(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.413(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.367(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?

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 90.59(17) . 2_556 ?
N2 Fe1 N12 175.82(12) . 2_556 ?
N2 Fe1 N12 88.88(12) . . ?
N12 Fe1 N12 91.96(15) 2_556 . ?
N2 Fe1 N6 87.21(12) . . ?
N12 Fe1 N6 82.65(11) . . ?
N2 Fe1 N6 93.19(12) . 2_556 ?
N12 Fe1 N6 96.96(11) . 2_556 ?
N6 Fe1 N6 179.44(15) . 2_556 ?
C3 N2 Fe1 169.2(3) . . ?
N2 C3 S4 178.1(3) . . ?
N6 C5 C10 123.2(3) . . ?
N6 C5 C11 115.2(3) . . ?
C10 C5 C11 121.6(3) . . ?
C7 N6 C5 118.3(3) . . ?
C7 N6 Fe1 128.0(2) . . ?
C5 N6 Fe1 113.2(2) . . ?
N6 C7 C8 121.8(3) . . ?
N6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 C10 118.9(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C5 C10 C9 117.7(3) . . ?
C5 C10 C17 118.6(3) . . ?
C9 C10 C17 123.6(3) . . ?
N12 C11 C16 123.2(3) . . ?
N12 C11 C5 115.3(3) . . ?
C16 C11 C5 121.4(3) . . ?
C13 N12 C11 118.0(3) . . ?
C13 N12 Fe1 128.8(2) . . ?
C11 N12 Fe1 113.2(2) . . ?
N12 C13 C14 121.9(3) . . ?
N12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 118.5(3) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C11 C16 C15 118.1(3) . . ?
C11 C16 C22 118.5(3) . . ?
C15 C16 C22 123.4(3) . . ?
N18 C17 C22 121.6(3) . . ?
N18 C17 C10 118.4(3) . . ?
C22 C17 C10 120.0(3) . . ?
C17 N18 C19 117.0(3) . . ?
N18 C19 C23 119.3(4) . . ?
N18 C19 C20 121.0(3) . . ?
C23 C19 C20 119.7(4) . . ?
N21 C20 C26 119.3(4) . . ?
N21 C20 C19 121.6(3) . . ?
C26 C20 C19 119.1(3) . . ?
C22 N21 C20 116.5(3) . . ?
N21 C22 C17 122.0(3) . . ?
N21 C22 C16 118.3(3) . . ?
C17 C22 C16 119.6(3) . . ?
C24 C23 C19 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C19 C23 H23 120.1 . . ?
C23 C24 C25 120.6(4) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 121.3(4) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C20 119.5(4) . . ?
C25 C26 H26 120.3 . . ?
C20 C26 H26 120.3 . . ?

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
C8 H8 S4 0.95 3.04 3.932(4) 156.9 1_455
C25 H25 S4 0.95 3.06 3.737(4) 129.1 5_566

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.091
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_rk89art
_database_code_depnum_ccdc_archive 'CCDC 1430806'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
Bis[iso-thiocyanato][dipyrido[3,2-a:23-c]phenazine]-iron(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H20 Fe N10 S2'
_chemical_formula_sum            'C38 H20 Fe N10 S2'
_chemical_formula_weight         736.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   8.0689(4)
_cell_length_b                   14.7987(6)
_cell_length_c                   28.0208(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.552(4)
_cell_angle_gamma                90.00
_cell_volume                     3342.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    2863
_cell_measurement_theta_min      6.21
_cell_measurement_theta_max      73.23


_exptl_crystal_description       fragment
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    5.158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7733
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         73.82
_reflns_number_total             3232
_reflns_number_gt                2559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains half a molecule, with Fe1 lying on the 
 crystallographic C₂ axis 0, y, 3/4. The C and S atoms of the unique 
 NCS⁻ ligand are disordered over two orientations, which were modelled 
 without restraints. The occupancies of the disorder sites refined to 
 0.59:0.41, which was rounded to 0.60:0.40 in the final least squares 
 cycles. All non-H atoms except the minor ligand disorder site were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0768P)²+3.1996P] 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         3232
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1636
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.38241(5) 0.7500 0.0500(2) Uani 1 2 d S . .
N2 N 0.1232(4) 0.2902(2) 0.71764(12) 0.0630(8) Uani 1 1 d . . .
C3A C 0.1759(12) 0.2333(6) 0.6913(3) 0.0406(17) Uani 0.60 1 d P A 1
S4A S 0.2452(3) 0.15489(12) 0.65885(8) 0.0641(5) Uani 0.60 1 d P A 1
C3B C 0.199(2) 0.2390(13) 0.7025(5) 0.050(5) Uiso 0.40 1 d P A 2
S4B S 0.3046(5) 0.1640(3) 0.67327(16) 0.0859(14) Uiso 0.40 1 d P A 2
C5 C -0.1052(4) 0.4368(2) 0.65770(12) 0.0513(8) Uani 1 1 d . A .
N6 N -0.1546(3) 0.38348(18) 0.69397(11) 0.0538(7) Uani 1 1 d . . .
C7 C -0.2909(5) 0.3330(3) 0.68450(17) 0.0711(11) Uani 1 1 d . A .
H7 H -0.3289 0.2964 0.7087 0.085 Uiso 1 1 calc R . .
C8 C -0.3760(6) 0.3324(3) 0.6416(2) 0.0841(13) Uani 1 1 d . . .
H8 H -0.4679 0.2950 0.6368 0.101 Uiso 1 1 calc R A .
C9 C -0.3259(6) 0.3874(3) 0.60516(17) 0.0755(12) Uani 1 1 d . A .
H9 H -0.3833 0.3875 0.5756 0.091 Uiso 1 1 calc R . .
C10 C -0.1876(5) 0.4428(2) 0.61334(13) 0.0589(9) Uani 1 1 d . . .
C11 C 0.0439(4) 0.4885(2) 0.66873(11) 0.0480(7) Uani 1 1 d . . .
N12 N 0.1142(3) 0.47481(18) 0.71281(10) 0.0487(6) Uani 1 1 d . A .
C13 C 0.2505(5) 0.5222(3) 0.72512(14) 0.0592(9) Uani 1 1 d . . .
H13 H 0.2996 0.5145 0.7555 0.071 Uiso 1 1 calc R A .
C14 C 0.3215(5) 0.5828(3) 0.69379(15) 0.0688(10) Uani 1 1 d . A .
H14 H 0.4175 0.6141 0.7032 0.083 Uiso 1 1 calc R . .
C15 C 0.2504(5) 0.5962(3) 0.64951(15) 0.0664(10) Uani 1 1 d . . .
H15 H 0.2976 0.6364 0.6285 0.080 Uiso 1 1 calc R A .
C16 C 0.1063(4) 0.5492(2) 0.63561(12) 0.0552(8) Uani 1 1 d . A .
C17 C -0.1285(5) 0.5080(3) 0.57838(13) 0.0600(9) Uani 1 1 d . A .
N18 N -0.2148(4) 0.5159(3) 0.53746(12) 0.0719(9) Uani 1 1 d . . .
C19 C -0.1627(6) 0.5815(3) 0.50738(15) 0.0754(12) Uani 1 1 d . A .
C20 C -0.0272(6) 0.6383(3) 0.51990(15) 0.0733(11) Uani 1 1 d . . .
N21 N 0.0626(4) 0.6269(2) 0.56130(12) 0.0682(9) Uani 1 1 d . A .
C22 C 0.0140(5) 0.5621(3) 0.59031(13) 0.0588(9) Uani 1 1 d . . .
C23 C -0.2498(7) 0.5928(4) 0.46271(17) 0.0941(16) Uani 1 1 d . . .
H23 H -0.3372 0.5546 0.4538 0.113 Uiso 1 1 calc R A .
C24 C -0.2039(8) 0.6602(5) 0.4331(2) 0.1045(19) Uani 1 1 d . A .
H24 H -0.2599 0.6670 0.4036 0.125 Uiso 1 1 calc R . .
C25 C -0.0752(8) 0.7192(5) 0.4459(2) 0.106(2) Uani 1 1 d . . .
H25 H -0.0495 0.7661 0.4254 0.127 Uiso 1 1 calc R A .
C26 C 0.0143(7) 0.7091(4) 0.48848(17) 0.0909(15) Uani 1 1 d . A .
H26 H 0.1012 0.7482 0.4966 0.109 Uiso 1 1 calc R . .


_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 1.937(3) . ?
Fe1 N6 1.962(3) . ?
Fe1 N12 1.972(3) . ?
N2 C3B 1.073(19) . ?
N2 C3A 1.210(10) . ?
C3A S4A 1.591(9) . ?
C3B S4B 1.641(19) . ?
C5 N6 1.360(5) . ?
C5 C10 1.386(5) . ?
C5 C11 1.448(5) . ?
N6 C7 1.346(5) . ?
C7 C8 1.358(7) . ?
C8 C9 1.381(7) . ?
C9 C10 1.396(6) . ?
C10 C17 1.469(6) . ?
C11 N12 1.351(4) . ?
C11 C16 1.401(5) . ?
N12 C13 1.336(4) . ?
C13 C14 1.396(5) . ?
C14 C15 1.358(6) . ?
C15 C16 1.395(5) . ?
C16 C22 1.455(6) . ?
C17 N18 1.320(5) . ?
C17 C22 1.428(6) . ?
N18 C19 1.363(6) . ?
C19 C20 1.411(7) . ?
C19 C23 1.418(7) . ?
C20 N21 1.351(6) . ?
C20 C26 1.418(7) . ?
N21 C22 1.328(5) . ?
C23 C24 1.358(9) . ?
C24 C25 1.392(9) . ?
C25 C26 1.375(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 90.47(19) 2_556 . ?
N2 Fe1 N6 93.38(13) . 2_556 ?
N2 Fe1 N6 87.27(13) . . ?
N6 Fe1 N6 179.07(16) 2_556 . ?
N2 Fe1 N12 175.70(13) . 2_556 ?
N6 Fe1 N12 97.00(11) . 2_556 ?
N2 Fe1 N12 88.81(12) . . ?
N6 Fe1 N12 82.35(11) . . ?
N12 Fe1 N12 92.23(15) 2_556 . ?
C3B N2 Fe1 174.9(9) . . ?
C3A N2 Fe1 167.9(6) . . ?
N2 C3A S4A 177.2(8) . . ?
N2 C3B S4B 173.3(14) . . ?
N6 C5 C10 124.2(3) . . ?
N6 C5 C11 114.6(3) . . ?
C10 C5 C11 121.2(3) . . ?
C7 N6 C5 116.0(3) . . ?
C7 N6 Fe1 129.6(3) . . ?
C5 N6 Fe1 113.9(2) . . ?
N6 C7 C8 123.7(4) . . ?
C7 C8 C9 119.8(4) . . ?
C8 C9 C10 118.9(4) . . ?
C5 C10 C9 117.2(4) . . ?
C5 C10 C17 118.9(3) . . ?
C9 C10 C17 123.8(4) . . ?
N12 C11 C16 123.6(3) . . ?
N12 C11 C5 115.3(3) . . ?
C16 C11 C5 121.1(3) . . ?
C13 N12 C11 117.7(3) . . ?
C13 N12 Fe1 128.7(2) . . ?
C11 N12 Fe1 113.6(2) . . ?
N12 C13 C14 122.1(4) . . ?
C15 C14 C13 120.0(4) . . ?
C14 C15 C16 119.7(3) . . ?
C15 C16 C11 117.0(3) . . ?
C15 C16 C22 124.5(3) . . ?
C11 C16 C22 118.4(3) . . ?
N18 C17 C22 122.8(4) . . ?
N18 C17 C10 117.6(4) . . ?
C22 C17 C10 119.6(3) . . ?
C17 N18 C19 115.8(4) . . ?
N18 C19 C20 121.8(4) . . ?
N18 C19 C23 118.4(5) . . ?
C20 C19 C23 119.8(5) . . ?
N21 C20 C19 121.3(4) . . ?
N21 C20 C26 119.5(5) . . ?
C19 C20 C26 119.2(4) . . ?
C22 N21 C20 117.0(4) . . ?
N21 C22 C17 121.2(4) . . ?
N21 C22 C16 118.3(4) . . ?
C17 C22 C16 120.4(3) . . ?
C24 C23 C19 119.2(6) . . ?
C23 C24 C25 121.6(5) . . ?
C26 C25 C24 120.8(6) . . ?
C25 C26 C20 119.3(6) . . ?

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
C8 H8 S4A 0.93 3.19 4.075(5) 159.9 1_455
C8 H8 S4B 0.93 2.89 3.721(7) 149.6 1_455
C25 H25 S4A 0.93 3.02 3.689(6) 130.5 5_566
C25 H25 S4B 0.93 3.53 4.125(7) 124.4 5_566

_diffrn_measured_fraction_theta_max 0.953
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.058
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_rk70
_database_code_depnum_ccdc_archive 'CCDC 1430807'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)bis-(1,2-dichloroethane) solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C34 H24 Cl4 Fe N10 S2'
_chemical_formula_weight         834.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.6431(3)
_cell_length_b                   12.5380(5)
_cell_length_c                   16.8933(7)
_cell_angle_alpha                100.234(3)
_cell_angle_beta                 97.965(3)
_cell_angle_gamma                101.090(3)
_cell_volume                     1739.40(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6930
_cell_measurement_theta_min      3.67
_cell_measurement_theta_max      73.71

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    7.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12817
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         73.69
_reflns_number_total             6537
_reflns_number_gt                5705
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains one molecule of the complex, one whole 
 molecule of 1,2-dichloroethane solvent, and two half-molecules of 
 1,2-dichloroethane lying across crystallographic inversion centres. The 
 methylene group of one of these solvent half-molecules is disordered 
 over two sites, with refined occupancies of 0.62:0.38. These were 
 modelled without restraints. All non-H atoms except the disordered 
 methylene group were refined anisotropically, while H atoms were 
 placed in calculated positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0585P)²+1.6843P] 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         6537
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.51934(5) 0.30473(3) 0.25303(2) 0.01604(11) Uani 1 1 d . . .
N2 N 0.2863(3) 0.2365(2) 0.26012(15) 0.0235(5) Uani 1 1 d . . .
C3 C 0.1607(3) 0.1960(2) 0.27121(17) 0.0206(5) Uani 1 1 d . . .
S4 S -0.01595(8) 0.13675(6) 0.28430(5) 0.02962(17) Uani 1 1 d . . .
N5 N 0.4762(3) 0.46338(19) 0.25385(14) 0.0213(5) Uani 1 1 d . . .
C6 C 0.4443(3) 0.5476(2) 0.24823(16) 0.0185(5) Uani 1 1 d . . .
S7 S 0.40003(8) 0.66777(6) 0.24334(5) 0.02740(17) Uani 1 1 d . . .
C8 C 0.7605(3) 0.3234(2) 0.40786(16) 0.0171(5) Uani 1 1 d . . .
N9 N 0.6000(3) 0.29400(18) 0.38050(14) 0.0182(4) Uani 1 1 d . . .
C10 C 0.5073(3) 0.2534(2) 0.43062(18) 0.0237(6) Uani 1 1 d . . .
H10 H 0.3946 0.2321 0.4123 0.028 Uiso 1 1 calc R . .
C11 C 0.5687(4) 0.2411(2) 0.50807(19) 0.0263(6) Uani 1 1 d . . .
H11 H 0.4986 0.2126 0.5417 0.032 Uiso 1 1 calc R . .
C12 C 0.7313(4) 0.2703(2) 0.53596(18) 0.0243(6) Uani 1 1 d . . .
H12 H 0.7749 0.2626 0.5889 0.029 Uiso 1 1 calc R . .
C13 C 0.8317(3) 0.3118(2) 0.48457(16) 0.0189(5) Uani 1 1 d . . .
C14 C 0.8588(3) 0.3713(2) 0.35413(16) 0.0169(5) Uani 1 1 d . . .
N15 N 0.7821(3) 0.37634(17) 0.27998(13) 0.0171(4) Uani 1 1 d . . .
C16 C 0.8704(3) 0.4222(2) 0.23082(17) 0.0207(5) Uani 1 1 d . . .
H16 H 0.8183 0.4259 0.1784 0.025 Uiso 1 1 calc R . .
C17 C 1.0353(3) 0.4649(2) 0.25255(18) 0.0238(6) Uani 1 1 d . . .
H17 H 1.0929 0.4978 0.2158 0.029 Uiso 1 1 calc R . .
C18 C 1.1134(3) 0.4590(2) 0.32726(17) 0.0210(5) Uani 1 1 d . . .
H18 H 1.2258 0.4873 0.3430 0.025 Uiso 1 1 calc R . .
C19 C 1.0246(3) 0.4103(2) 0.38040(16) 0.0178(5) Uani 1 1 d . . .
C20 C 1.0057(3) 0.3458(2) 0.50958(16) 0.0197(5) Uani 1 1 d . . .
N21 N 1.0719(3) 0.32736(19) 0.58162(15) 0.0243(5) Uani 1 1 d . . .
C22 C 1.2296(4) 0.3631(2) 0.60335(18) 0.0268(6) Uani 1 1 d . . .
H22 H 1.2810 0.3513 0.6535 0.032 Uiso 1 1 calc R . .
C23 C 1.3226(3) 0.4176(2) 0.55454(18) 0.0250(6) Uani 1 1 d . . .
H23 H 1.4346 0.4438 0.5738 0.030 Uiso 1 1 calc R . .
N24 N 1.2605(3) 0.43401(19) 0.48271(15) 0.0219(5) Uani 1 1 d . . .
C25 C 1.0992(3) 0.3967(2) 0.45928(16) 0.0177(5) Uani 1 1 d . . .
C26 C 0.6016(3) 0.2013(2) 0.09164(16) 0.0186(5) Uani 1 1 d . . .
N27 N 0.5372(3) 0.28728(18) 0.12219(14) 0.0194(4) Uani 1 1 d . . .
C28 C 0.5118(4) 0.3585(2) 0.07523(17) 0.0242(6) Uani 1 1 d . . .
H28 H 0.4652 0.4180 0.0958 0.029 Uiso 1 1 calc R . .
C29 C 0.5500(4) 0.3506(2) -0.00327(18) 0.0274(6) Uani 1 1 d . . .
H29 H 0.5275 0.4026 -0.0353 0.033 Uiso 1 1 calc R . .
C30 C 0.6206(4) 0.2662(2) -0.03313(17) 0.0262(6) Uani 1 1 d . . .
H30 H 0.6507 0.2603 -0.0855 0.031 Uiso 1 1 calc R . .
C31 C 0.6474(3) 0.1891(2) 0.01468(17) 0.0215(5) Uani 1 1 d . . .
C32 C 0.6155(3) 0.1190(2) 0.14093(16) 0.0182(5) Uani 1 1 d . . .
N33 N 0.5720(3) 0.13734(18) 0.21521(14) 0.0187(4) Uani 1 1 d . . .
C34 C 0.5700(3) 0.0575(2) 0.25780(17) 0.0221(5) Uani 1 1 d . . .
H34 H 0.5395 0.0696 0.3100 0.027 Uiso 1 1 calc R . .
C35 C 0.6106(3) -0.0434(2) 0.22922(18) 0.0235(6) Uani 1 1 d . . .
H35 H 0.6027 -0.0996 0.2604 0.028 Uiso 1 1 calc R . .
C36 C 0.6620(3) -0.0602(2) 0.15542(18) 0.0233(6) Uani 1 1 d . . .
H36 H 0.6937 -0.1270 0.1358 0.028 Uiso 1 1 calc R . .
C37 C 0.6670(3) 0.0225(2) 0.10986(17) 0.0205(5) Uani 1 1 d . . .
C38 C 0.7153(3) 0.0940(2) -0.01418(17) 0.0225(6) Uani 1 1 d . . .
N39 N 0.7683(3) 0.0879(2) -0.08680(15) 0.0281(5) Uani 1 1 d . . .
C40 C 0.8233(4) -0.0007(3) -0.11113(19) 0.0319(7) Uani 1 1 d . . .
H40 H 0.8632 -0.0080 -0.1610 0.038 Uiso 1 1 calc R . .
C41 C 0.8258(4) -0.0850(3) -0.06679(19) 0.0293(6) Uani 1 1 d . . .
H41 H 0.8640 -0.1481 -0.0888 0.035 Uiso 1 1 calc R . .
N42 N 0.7772(3) -0.0806(2) 0.00429(15) 0.0265(5) Uani 1 1 d . . .
C43 C 0.7216(3) 0.0118(2) 0.03155(17) 0.0220(5) Uani 1 1 d . . .
C44 C 0.0176(4) 0.8454(3) 0.2812(2) 0.0357(7) Uani 1 1 d . . .
H44A H -0.0282 0.8146 0.3251 0.043 Uiso 1 1 calc R . .
H44B H -0.0451 0.8987 0.2647 0.043 Uiso 1 1 calc R . .
C45 C 0.0071(4) 0.7542(3) 0.2101(3) 0.0430(8) Uani 1 1 d . . .
H45A H 0.0744 0.7029 0.2255 0.052 Uiso 1 1 calc R . .
H45B H 0.0463 0.7851 0.1647 0.052 Uiso 1 1 calc R . .
Cl46 Cl 0.22420(10) 0.91638(7) 0.31875(6) 0.0442(2) Uani 1 1 d . . .
Cl47 Cl -0.19814(10) 0.68088(7) 0.17855(5) 0.03794(19) Uani 1 1 d . . .
C48 C 0.9541(4) 0.0376(3) 0.4832(2) 0.0409(8) Uani 1 1 d . . .
H48A H 1.0072 0.0687 0.4414 0.049 Uiso 1 1 calc R . .
H48B H 0.9503 0.1000 0.5273 0.049 Uiso 1 1 calc R . .
Cl49 Cl 0.75547(11) -0.03885(9) 0.43829(6) 0.0507(2) Uani 1 1 d . . .
C50A C 0.0191(9) 0.4529(6) -0.0263(5) 0.0543(16) Uiso 0.62 1 d P . 1
H50A H 0.1099 0.4795 -0.0530 0.065 Uiso 0.62 1 calc PR . 1
H50B H -0.0747 0.4149 -0.0695 0.065 Uiso 0.62 1 calc PR . 1
C50B C 0.0247(15) 0.4912(11) 0.0417(7) 0.056(3) Uiso 0.38 1 d P . 2
H50C H -0.0631 0.4963 0.0731 0.067 Uiso 0.38 1 calc PR . 2
H50D H 0.1198 0.5497 0.0704 0.067 Uiso 0.38 1 calc PR . 2
Cl51 Cl 0.07102(15) 0.35807(9) 0.03567(7) 0.0593(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.060(2) . ?
Fe1 N5 2.091(2) . ?
Fe1 N9 2.205(2) . ?
Fe1 N27 2.212(2) . ?
Fe1 N15 2.226(2) . ?
Fe1 N33 2.234(2) . ?
N2 C3 1.161(4) . ?
C3 S4 1.628(3) . ?
N5 C6 1.158(4) . ?
C6 S7 1.637(3) . ?
C8 N9 1.356(3) . ?
C8 C13 1.400(4) . ?
C8 C14 1.455(3) . ?
N9 C10 1.343(3) . ?
C10 C11 1.389(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.405(4) . ?
C12 H12 0.9500 . ?
C13 C20 1.461(4) . ?
C14 N15 1.352(4) . ?
C14 C19 1.402(4) . ?
N15 C16 1.333(3) . ?
C16 C17 1.395(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.368(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.405(4) . ?
C18 H18 0.9500 . ?
C19 C25 1.451(4) . ?
C20 N21 1.349(4) . ?
C20 C25 1.402(4) . ?
N21 C22 1.327(4) . ?
C22 C23 1.402(4) . ?
C22 H22 0.9500 . ?
C23 N24 1.324(4) . ?
C23 H23 0.9500 . ?
N24 C25 1.360(4) . ?
C26 N27 1.361(3) . ?
C26 C31 1.402(4) . ?
C26 C32 1.448(4) . ?
N27 C28 1.324(4) . ?
C28 C29 1.402(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.397(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.465(4) . ?
C32 N33 1.353(3) . ?
C32 C37 1.408(4) . ?
N33 C34 1.332(3) . ?
C34 C35 1.399(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.376(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.394(4) . ?
C36 H36 0.9500 . ?
C37 C43 1.458(4) . ?
C38 N39 1.363(4) . ?
C38 C43 1.398(4) . ?
N39 C40 1.313(4) . ?
C40 C41 1.402(5) . ?
C40 H40 0.9500 . ?
C41 N42 1.322(4) . ?
C41 H41 0.9500 . ?
N42 C43 1.367(4) . ?
C44 C45 1.484(5) . ?
C44 Cl46 1.805(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 Cl47 1.792(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C48 C48 1.482(7) 2_756 ?
C48 Cl49 1.786(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C50A C50A 1.468(14) 2_565 ?
C50A Cl51 1.797(8) . ?
C50A H50A 0.9900 . ?
C50A H50B 0.9900 . ?
C50B C50B 1.48(2) 2_565 ?
C50B H50C 0.9900 . ?
C50B H50D 0.9900 . ?
C50B Cl51 1.779(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 N5 93.58(9) . . ?
N2 Fe1 N9 90.63(9) . . ?
N5 Fe1 N9 108.00(9) . . ?
N2 Fe1 N27 107.88(9) . . ?
N5 Fe1 N27 89.15(9) . . ?
N9 Fe1 N27 154.15(8) . . ?
N2 Fe1 N15 164.90(9) . . ?
N5 Fe1 N15 90.04(8) . . ?
N9 Fe1 N15 74.32(8) . . ?
N27 Fe1 N15 86.82(8) . . ?
N2 Fe1 N33 92.19(9) . . ?
N5 Fe1 N33 163.54(9) . . ?
N9 Fe1 N33 87.32(8) . . ?
N27 Fe1 N33 74.41(8) . . ?
N15 Fe1 N33 88.37(8) . . ?
C3 N2 Fe1 173.5(2) . . ?
N2 C3 S4 178.4(3) . . ?
C6 N5 Fe1 174.4(2) . . ?
N5 C6 S7 178.2(3) . . ?
N9 C8 C13 123.0(2) . . ?
N9 C8 C14 116.8(2) . . ?
C13 C8 C14 120.2(2) . . ?
C10 N9 C8 117.5(2) . . ?
C10 N9 Fe1 126.29(19) . . ?
C8 N9 Fe1 116.00(17) . . ?
N9 C10 C11 122.9(3) . . ?
N9 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 118.6(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C8 C13 C12 118.1(3) . . ?
C8 C13 C20 119.6(2) . . ?
C12 C13 C20 122.3(3) . . ?
N15 C14 C19 123.2(2) . . ?
N15 C14 C8 116.8(2) . . ?
C19 C14 C8 120.1(2) . . ?
C16 N15 C14 117.4(2) . . ?
C16 N15 Fe1 126.99(18) . . ?
C14 N15 Fe1 115.63(16) . . ?
N15 C16 C17 123.3(3) . . ?
N15 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 118.9(3) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C14 C19 C18 117.8(2) . . ?
C14 C19 C25 119.8(2) . . ?
C18 C19 C25 122.3(2) . . ?
N21 C20 C25 121.7(3) . . ?
N21 C20 C13 118.3(2) . . ?
C25 C20 C13 120.0(2) . . ?
C22 N21 C20 116.3(2) . . ?
N21 C22 C23 122.0(3) . . ?
N21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
N24 C23 C22 122.6(3) . . ?
N24 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
C23 N24 C25 116.0(2) . . ?
N24 C25 C20 121.3(2) . . ?
N24 C25 C19 118.5(2) . . ?
C20 C25 C19 120.2(2) . . ?
N27 C26 C31 122.3(2) . . ?
N27 C26 C32 117.0(2) . . ?
C31 C26 C32 120.6(2) . . ?
C28 N27 C26 117.8(2) . . ?
C28 N27 Fe1 126.88(18) . . ?
C26 N27 Fe1 114.66(17) . . ?
N27 C28 C29 123.4(3) . . ?
N27 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C30 C29 C28 118.9(3) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C29 C30 C31 119.0(3) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C26 118.5(3) . . ?
C30 C31 C38 122.3(3) . . ?
C26 C31 C38 119.1(2) . . ?
N33 C32 C37 122.6(2) . . ?
N33 C32 C26 117.4(2) . . ?
C37 C32 C26 120.0(2) . . ?
C34 N33 C32 117.9(2) . . ?
C34 N33 Fe1 127.75(18) . . ?
C32 N33 Fe1 114.36(17) . . ?
N33 C34 C35 123.0(3) . . ?
N33 C34 H34 118.5 . . ?
C35 C34 H34 118.5 . . ?
C36 C35 C34 119.2(3) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C37 119.0(2) . . ?
C35 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C36 C37 C32 118.2(2) . . ?
C36 C37 C43 122.4(2) . . ?
C32 C37 C43 119.4(2) . . ?
N39 C38 C43 121.9(3) . . ?
N39 C38 C31 118.0(3) . . ?
C43 C38 C31 120.2(2) . . ?
C40 N39 C38 115.5(3) . . ?
N39 C40 C41 122.9(3) . . ?
N39 C40 H40 118.5 . . ?
C41 C40 H40 118.5 . . ?
N42 C41 C40 122.8(3) . . ?
N42 C41 H41 118.6 . . ?
C40 C41 H41 118.6 . . ?
C41 N42 C43 115.3(3) . . ?
N42 C43 C38 121.5(3) . . ?
N42 C43 C37 118.3(2) . . ?
C38 C43 C37 120.3(2) . . ?
C45 C44 Cl46 109.8(2) . . ?
C45 C44 H44A 109.7 . . ?
Cl46 C44 H44A 109.7 . . ?
C45 C44 H44B 109.7 . . ?
Cl46 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?
C44 C45 Cl47 108.4(2) . . ?
C44 C45 H45A 110.0 . . ?
Cl47 C45 H45A 110.0 . . ?
C44 C45 H45B 110.0 . . ?
Cl47 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
C48 C48 Cl49 109.1(3) 2_756 . ?
C48 C48 H48A 109.9 2_756 . ?
Cl49 C48 H48A 109.9 . . ?
C48 C48 H48B 109.9 2_756 . ?
Cl49 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C50A C50A Cl51 108.5(7) 2_565 . ?
C50A C50A H50A 110.0 2_565 . ?
Cl51 C50A H50A 110.0 . . ?
C50A C50A H50B 110.0 2_565 . ?
Cl51 C50A H50B 110.0 . . ?
H50A C50A H50B 108.4 . . ?
C50B C50B Cl51 109.8(12) 2_565 . ?
C50B C50B H50C 109.7 2_565 . ?
Cl51 C50B H50C 109.7 . . ?
C50B C50B H50D 109.7 2_565 . ?
Cl51 C50B H50D 109.7 . . ?
H50C C50B H50D 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.930
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.075
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
####################################################################### 
# 
# 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_rk147
_database_code_depnum_ccdc_archive 'CCDC 1430808'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)di-pyridine solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C5 H5 N)'
_chemical_formula_sum            'C40 H26 Fe N12 S2'
_chemical_formula_weight         794.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   13.3290(9)
_cell_length_b                   16.1844(9)
_cell_length_c                   17.3536(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.324(7)
_cell_angle_gamma                90.00
_cell_volume                     3510.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6483
_cell_measurement_theta_min      3.62
_cell_measurement_theta_max      73.87

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14631
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         73.92
_reflns_number_total             6905
_reflns_number_gt                5916
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The pyridine molecule N50-C55 is disordered over two sites, with refined 
 occupancies of 0.59:0.41. This disorder was modelled without the use of 
 restraints. All non-H atoms except the disordered solvent were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0433P)²+1.5204P] 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         6905
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22771(2) 0.744831(18) 0.388959(18) 0.01939(9) Uani 1 1 d . . .
N2 N 0.28350(14) 0.74185(11) 0.29907(11) 0.0271(4) Uani 1 1 d . . .
C3 C 0.31642(16) 0.74570(12) 0.24572(13) 0.0244(4) Uani 1 1 d . . .
S4 S 0.36590(5) 0.74998(3) 0.17142(3) 0.03062(13) Uani 1 1 d . . .
N5 N 0.08003(14) 0.75280(10) 0.31136(11) 0.0244(4) Uani 1 1 d . . .
C6 C -0.00822(17) 0.75916(12) 0.26895(12) 0.0227(4) Uani 1 1 d . . .
S7 S -0.13426(4) 0.76785(3) 0.20893(3) 0.02879(12) Uani 1 1 d . . .
C8 C 0.20082(15) 0.90042(12) 0.45314(12) 0.0236(4) Uani 1 1 d . . .
N9 N 0.23758(13) 0.86744(11) 0.39581(10) 0.0234(4) Uani 1 1 d . . .
C10 C 0.26983(17) 0.92014(14) 0.35006(14) 0.0292(4) Uani 1 1 d . . .
H10 H 0.2951 0.8986 0.3092 0.035 Uiso 1 1 calc R . .
C11 C 0.26799(17) 1.00592(14) 0.35981(14) 0.0333(5) Uani 1 1 d . . .
H11 H 0.2928 1.0413 0.3265 0.040 Uiso 1 1 calc R . .
C12 C 0.23036(17) 1.03909(14) 0.41751(14) 0.0321(5) Uani 1 1 d . . .
H12 H 0.2281 1.0972 0.4242 0.039 Uiso 1 1 calc R . .
C13 C 0.19542(16) 0.98515(13) 0.46621(13) 0.0271(4) Uani 1 1 d . . .
C14 C 0.16495(15) 0.84117(12) 0.49997(12) 0.0223(4) Uani 1 1 d . . .
N15 N 0.17162(13) 0.76041(10) 0.48031(10) 0.0212(3) Uani 1 1 d . . .
C16 C 0.13822(16) 0.70388(13) 0.52187(12) 0.0242(4) Uani 1 1 d . . .
H16 H 0.1437 0.6471 0.5099 0.029 Uiso 1 1 calc R . .
C17 C 0.09554(17) 0.72474(15) 0.58225(13) 0.0292(4) Uani 1 1 d . . .
H17 H 0.0723 0.6826 0.6102 0.035 Uiso 1 1 calc R . .
C18 C 0.08723(16) 0.80600(14) 0.60114(13) 0.0281(4) Uani 1 1 d . . .
H18 H 0.0576 0.8208 0.6417 0.034 Uiso 1 1 calc R . .
C19 C 0.12325(16) 0.86694(13) 0.55942(12) 0.0248(4) Uani 1 1 d . . .
C20 C 0.15243(16) 1.01295(13) 0.52813(13) 0.0291(5) Uani 1 1 d . . .
N21 N 0.14753(16) 1.09539(12) 0.54045(12) 0.0366(5) Uani 1 1 d . . .
C22 C 0.1072(2) 1.11713(16) 0.59728(16) 0.0421(6) Uani 1 1 d . . .
H22 H 0.1032 1.1743 0.6084 0.051 Uiso 1 1 calc R . .
C23 C 0.0703(2) 1.06036(16) 0.64156(15) 0.0403(6) Uani 1 1 d . . .
H23 H 0.0418 1.0800 0.6813 0.048 Uiso 1 1 calc R . .
N24 N 0.07392(15) 0.97942(13) 0.62976(12) 0.0342(4) Uani 1 1 d . . .
C25 C 0.11694(16) 0.95543(14) 0.57356(13) 0.0279(4) Uani 1 1 d . . .
C26 C 0.30470(15) 0.58931(12) 0.45713(12) 0.0211(4) Uani 1 1 d . . .
N27 N 0.22286(13) 0.62276(11) 0.39393(10) 0.0221(3) Uani 1 1 d . . .
C28 C 0.15075(17) 0.57040(14) 0.34556(13) 0.0293(5) Uani 1 1 d . . .
H28 H 0.0929 0.5921 0.3010 0.035 Uiso 1 1 calc R . .
C29 C 0.15702(18) 0.48508(14) 0.35788(14) 0.0346(5) Uani 1 1 d . . .
H29 H 0.1051 0.4500 0.3211 0.041 Uiso 1 1 calc R . .
C30 C 0.23809(18) 0.45155(13) 0.42313(14) 0.0295(5) Uani 1 1 d . . .
H30 H 0.2420 0.3936 0.4327 0.035 Uiso 1 1 calc R . .
C31 C 0.31485(16) 0.50496(12) 0.47520(12) 0.0232(4) Uani 1 1 d . . .
C32 C 0.38523(15) 0.64735(12) 0.50283(12) 0.0202(4) Uani 1 1 d . . .
N33 N 0.37180(13) 0.72592(10) 0.47335(10) 0.0210(3) Uani 1 1 d . . .
C34 C 0.45097(16) 0.77936(13) 0.50747(13) 0.0262(4) Uani 1 1 d . . .
H34 H 0.4447 0.8339 0.4862 0.031 Uiso 1 1 calc R . .
C35 C 0.54276(17) 0.75807(13) 0.57337(14) 0.0286(5) Uani 1 1 d . . .
H35 H 0.5980 0.7976 0.5954 0.034 Uiso 1 1 calc R . .
C36 C 0.55336(16) 0.67980(13) 0.60644(13) 0.0253(4) Uani 1 1 d . . .
H36 H 0.6138 0.6657 0.6530 0.030 Uiso 1 1 calc R . .
C37 C 0.47329(15) 0.62155(12) 0.57006(12) 0.0209(4) Uani 1 1 d . . .
C38 C 0.40347(16) 0.47787(12) 0.54697(12) 0.0228(4) Uani 1 1 d . . .
N39 N 0.41043(14) 0.39646(11) 0.56581(11) 0.0264(4) Uani 1 1 d . . .
C40 C 0.48803(17) 0.37521(13) 0.63415(13) 0.0282(4) Uani 1 1 d . . .
H40 H 0.4959 0.3187 0.6498 0.034 Uiso 1 1 calc R . .
C41 C 0.55899(18) 0.43288(14) 0.68432(14) 0.0311(5) Uani 1 1 d . . .
H41 H 0.6113 0.4143 0.7340 0.037 Uiso 1 1 calc R . .
N42 N 0.55651(14) 0.51236(11) 0.66568(11) 0.0282(4) Uani 1 1 d . . .
C43 C 0.47807(15) 0.53543(12) 0.59527(12) 0.0223(4) Uani 1 1 d . . .
N44 N 0.46314(18) 1.06938(13) 0.58563(14) 0.0421(5) Uani 1 1 d . . .
C45 C 0.4285(2) 1.11191(18) 0.63690(19) 0.0508(7) Uani 1 1 d . . .
H45 H 0.4297 1.1705 0.6347 0.061 Uiso 1 1 calc R . .
C46 C 0.3906(2) 1.0748(2) 0.69370(17) 0.0547(8) Uani 1 1 d . . .
H46 H 0.3670 1.1074 0.7297 0.066 Uiso 1 1 calc R . .
C47 C 0.3880(2) 0.9899(2) 0.69668(15) 0.0465(7) Uani 1 1 d . . .
H47 H 0.3620 0.9627 0.7345 0.056 Uiso 1 1 calc R . .
C48 C 0.42340(18) 0.94532(16) 0.64432(14) 0.0369(5) Uani 1 1 d . . .
H48 H 0.4225 0.8866 0.6450 0.044 Uiso 1 1 calc R . .
C49 C 0.46018(18) 0.98717(15) 0.59084(14) 0.0346(5) Uani 1 1 d . . .
H49 H 0.4853 0.9556 0.5551 0.041 Uiso 1 1 calc R . .
N50A N 0.1308(3) 0.5172(3) 0.5940(3) 0.0393(10) Uiso 0.59 1 d P A 1
C51A C 0.2297(4) 0.5170(4) 0.6447(3) 0.0360(13) Uiso 0.59 1 d P A 1
H51A H 0.2671 0.5681 0.6554 0.043 Uiso 0.59 1 calc PR A 1
C52A C 0.2840(4) 0.4463(3) 0.6843(3) 0.0311(10) Uiso 0.59 1 d P A 1
H52A H 0.3557 0.4499 0.7213 0.037 Uiso 0.59 1 calc PR A 1
C53A C 0.2313(4) 0.3710(4) 0.6688(3) 0.0442(12) Uiso 0.59 1 d P A 1
H53A H 0.2651 0.3218 0.6950 0.053 Uiso 0.59 1 calc PR A 1
C54A C 0.1268(4) 0.3703(3) 0.6131(3) 0.0488(11) Uiso 0.59 1 d P A 1
H54A H 0.0876 0.3202 0.5995 0.059 Uiso 0.59 1 calc PR A 1
C55A C 0.0813(4) 0.4442(3) 0.5780(3) 0.0416(10) Uiso 0.59 1 d P A 1
H55A H 0.0101 0.4429 0.5399 0.050 Uiso 0.59 1 calc PR A 1
N50B N 0.1496(5) 0.4997(4) 0.5796(4) 0.0391(14) Uiso 0.41 1 d P B 2
C51B C 0.2390(6) 0.4929(6) 0.6520(5) 0.039(2) Uiso 0.41 1 d P B 2
H51B H 0.2731 0.5416 0.6793 0.046 Uiso 0.41 1 calc PR B 2
C52B C 0.2785(6) 0.4160(5) 0.6846(4) 0.0349(16) Uiso 0.41 1 d P B 2
H52B H 0.3380 0.4126 0.7344 0.042 Uiso 0.41 1 calc PR B 2
C53B C 0.2324(6) 0.3472(5) 0.6458(5) 0.0435(17) Uiso 0.41 1 d P B 2
H53B H 0.2612 0.2948 0.6668 0.052 Uiso 0.41 1 calc PR B 2
C54B C 0.1452(6) 0.3518(5) 0.5768(5) 0.0505(16) Uiso 0.41 1 d P B 2
H54B H 0.1121 0.3029 0.5492 0.061 Uiso 0.41 1 calc PR B 2
C55B C 0.1052(6) 0.4279(5) 0.5473(5) 0.0485(16) Uiso 0.41 1 d P B 2
H55B H 0.0413 0.4299 0.5007 0.058 Uiso 0.41 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9478(19) . ?
Fe1 N5 1.9656(18) . ?
Fe1 N27 1.9796(17) . ?
Fe1 N9 1.9896(18) . ?
Fe1 N15 1.9897(17) . ?
Fe1 N33 1.9932(17) . ?
N2 C3 1.156(3) . ?
C3 S4 1.641(2) . ?
N5 C6 1.155(3) . ?
C6 S7 1.647(2) . ?
C8 N9 1.361(3) . ?
C8 C13 1.396(3) . ?
C8 C14 1.442(3) . ?
N9 C10 1.334(3) . ?
C10 C11 1.400(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.402(3) . ?
C12 H12 0.9500 . ?
C13 C20 1.454(3) . ?
C14 N15 1.362(3) . ?
C14 C19 1.395(3) . ?
N15 C16 1.334(3) . ?
C16 C17 1.396(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.369(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.403(3) . ?
C18 H18 0.9500 . ?
C19 C25 1.460(3) . ?
C20 N21 1.356(3) . ?
C20 C25 1.404(3) . ?
N21 C22 1.324(4) . ?
C22 C23 1.392(4) . ?
C22 H22 0.9500 . ?
C23 N24 1.329(3) . ?
C23 H23 0.9500 . ?
N24 C25 1.349(3) . ?
C26 N27 1.362(3) . ?
C26 C31 1.397(3) . ?
C26 C32 1.440(3) . ?
N27 C28 1.337(3) . ?
C28 C29 1.395(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.376(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.403(3) . ?
C30 H30 0.9500 . ?
C31 C38 1.455(3) . ?
C32 N33 1.359(3) . ?
C32 C37 1.401(3) . ?
N33 C34 1.333(3) . ?
C34 C35 1.397(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.399(3) . ?
C36 H36 0.9500 . ?
C37 C43 1.456(3) . ?
C38 N39 1.353(3) . ?
C38 C43 1.407(3) . ?
N39 C40 1.320(3) . ?
C40 C41 1.397(3) . ?
C40 H40 0.9500 . ?
C41 N42 1.324(3) . ?
C41 H41 0.9500 . ?
N42 C43 1.356(3) . ?
N44 C45 1.328(4) . ?
N44 C49 1.335(3) . ?
C45 C46 1.391(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.376(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.367(4) . ?
C47 H47 0.9500 . ?
C48 C49 1.370(3) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
N50A C51A 1.306(7) . ?
N50A C55A 1.335(6) . ?
C51A C52A 1.401(7) . ?
C51A H51A 0.9500 . ?
C52A C53A 1.385(7) . ?
C52A H52A 0.9500 . ?
C53A C54A 1.393(7) . ?
C53A H53A 0.9500 . ?
C54A C55A 1.382(7) . ?
C54A H54A 0.9500 . ?
C55A H55A 0.9500 . ?
N50B C55B 1.335(10) . ?
N50B C51B 1.404(10) . ?
C51B C52B 1.391(11) . ?
C51B H51B 0.9500 . ?
C52B C53B 1.336(11) . ?
C52B H52B 0.9500 . ?
C53B C54B 1.350(10) . ?
C53B H53B 0.9500 . ?
C54B C55B 1.370(10) . ?
C54B H54B 0.9500 . ?
C55B H55B 0.9500 . ?

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 91.32(7) . . ?
N2 Fe1 N27 92.15(7) . . ?
N5 Fe1 N27 93.17(7) . . ?
N2 Fe1 N9 92.11(7) . . ?
N5 Fe1 N9 90.30(7) . . ?
N27 Fe1 N9 174.44(7) . . ?
N2 Fe1 N15 174.14(7) . . ?
N5 Fe1 N15 88.48(7) . . ?
N27 Fe1 N15 93.71(7) . . ?
N9 Fe1 N15 82.03(7) . . ?
N2 Fe1 N33 92.65(7) . . ?
N5 Fe1 N33 173.48(7) . . ?
N27 Fe1 N33 81.52(7) . . ?
N9 Fe1 N33 94.73(7) . . ?
N15 Fe1 N33 88.10(7) . . ?
C3 N2 Fe1 175.49(17) . . ?
N2 C3 S4 178.55(19) . . ?
C6 N5 Fe1 176.52(17) . . ?
N5 C6 S7 179.6(2) . . ?
N9 C8 C13 123.8(2) . . ?
N9 C8 C14 115.16(18) . . ?
C13 C8 C14 121.1(2) . . ?
C10 N9 C8 117.16(19) . . ?
C10 N9 Fe1 129.08(15) . . ?
C8 N9 Fe1 113.68(13) . . ?
N9 C10 C11 122.6(2) . . ?
N9 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C12 C11 C10 120.1(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 118.5(2) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C8 C13 C12 117.8(2) . . ?
C8 C13 C20 118.7(2) . . ?
C12 C13 C20 123.5(2) . . ?
N15 C14 C19 123.36(19) . . ?
N15 C14 C8 115.72(18) . . ?
C19 C14 C8 120.89(19) . . ?
C16 N15 C14 117.38(18) . . ?
C16 N15 Fe1 129.22(14) . . ?
C14 N15 Fe1 113.37(13) . . ?
N15 C16 C17 122.6(2) . . ?
N15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C18 C17 C16 120.0(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C14 C19 C18 117.85(19) . . ?
C14 C19 C25 118.59(19) . . ?
C18 C19 C25 123.5(2) . . ?
N21 C20 C25 121.3(2) . . ?
N21 C20 C13 118.3(2) . . ?
C25 C20 C13 120.40(19) . . ?
C22 N21 C20 115.7(2) . . ?
N21 C22 C23 123.2(2) . . ?
N21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
N24 C23 C22 121.8(2) . . ?
N24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 N24 C25 116.2(2) . . ?
N24 C25 C20 121.7(2) . . ?
N24 C25 C19 117.9(2) . . ?
C20 C25 C19 120.4(2) . . ?
N27 C26 C31 123.88(18) . . ?
N27 C26 C32 114.81(17) . . ?
C31 C26 C32 121.23(18) . . ?
C28 N27 C26 117.00(18) . . ?
C28 N27 Fe1 129.25(14) . . ?
C26 N27 Fe1 113.75(13) . . ?
N27 C28 C29 122.6(2) . . ?
N27 C28 H28 118.7 . . ?
C29 C28 H28 118.7 . . ?
C30 C29 C28 120.3(2) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 118.4(2) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
C26 C31 C30 117.74(19) . . ?
C26 C31 C38 118.25(18) . . ?
C30 C31 C38 124.01(19) . . ?
N33 C32 C37 123.72(18) . . ?
N33 C32 C26 115.32(17) . . ?
C37 C32 C26 120.87(18) . . ?
C34 N33 C32 117.34(17) . . ?
C34 N33 Fe1 129.69(14) . . ?
C32 N33 Fe1 112.80(13) . . ?
N33 C34 C35 122.5(2) . . ?
N33 C34 H34 118.8 . . ?
C35 C34 H34 118.8 . . ?
C36 C35 C34 120.12(19) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 118.67(19) . . ?
C35 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
C36 C37 C32 117.52(18) . . ?
C36 C37 C43 124.23(18) . . ?
C32 C37 C43 118.19(18) . . ?
N39 C38 C43 121.72(18) . . ?
N39 C38 C31 117.87(18) . . ?
C43 C38 C31 120.40(18) . . ?
C40 N39 C38 115.94(19) . . ?
N39 C40 C41 122.4(2) . . ?
N39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
N42 C41 C40 122.9(2) . . ?
N42 C41 H41 118.6 . . ?
C40 C41 H41 118.6 . . ?
C41 N42 C43 115.70(19) . . ?
N42 C43 C38 121.24(19) . . ?
N42 C43 C37 118.30(18) . . ?
C38 C43 C37 120.45(18) . . ?
C45 N44 C49 116.5(2) . . ?
N44 C45 C46 123.2(3) . . ?
N44 C45 H45 118.4 . . ?
C46 C45 H45 118.4 . . ?
C47 C46 C45 118.5(3) . . ?
C47 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
C48 C47 C46 118.9(3) . . ?
C48 C47 H47 120.5 . . ?
C46 C47 H47 120.5 . . ?
C47 C48 C49 118.5(3) . . ?
C47 C48 H48 120.8 . . ?
C49 C48 H48 120.8 . . ?
N44 C49 C48 124.4(2) . . ?
N44 C49 H49 117.8 . . ?
C48 C49 H49 117.8 . . ?
C51A N50A C55A 116.6(5) . . ?
N50A C51A C52A 124.2(5) . . ?
N50A C51A H51A 117.9 . . ?
C52A C51A H51A 117.9 . . ?
C53A C52A C51A 118.8(5) . . ?
C53A C52A H52A 120.6 . . ?
C51A C52A H52A 120.6 . . ?
C52A C53A C54A 117.3(5) . . ?
C52A C53A H53A 121.3 . . ?
C54A C53A H53A 121.3 . . ?
C55A C54A C53A 118.6(5) . . ?
C55A C54A H54A 120.7 . . ?
C53A C54A H54A 120.7 . . ?
N50A C55A C54A 124.3(4) . . ?
N50A C55A H55A 117.8 . . ?
C54A C55A H55A 117.8 . . ?
C55B N50B C51B 114.9(7) . . ?
C52B C51B N50B 121.2(7) . . ?
C52B C51B H51B 119.4 . . ?
N50B C51B H51B 119.4 . . ?
C53B C52B C51B 119.8(7) . . ?
C53B C52B H52B 120.1 . . ?
C51B C52B H52B 120.1 . . ?
C52B C53B C54B 120.3(7) . . ?
C52B C53B H53B 119.8 . . ?
C54B C53B H53B 119.8 . . ?
C53B C54B C55B 118.9(8) . . ?
C53B C54B H54B 120.5 . . ?
C55B C54B H54B 120.5 . . ?
N50B C55B C54B 124.6(7) . . ?
N50B C55B H55B 117.7 . . ?
C54B C55B H55B 117.7 . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.052
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'pyridine/diethyl ether'
####################################################################### 
# 
# 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_rk147rt
_database_code_depnum_ccdc_archive 'CCDC 1430809'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)di-pyridine solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C5 H5 N)'
_chemical_formula_sum            'C40 H26 Fe N12 S2'
_chemical_formula_weight         794.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   13.5260(6)
_cell_length_b                   16.3143(6)
_cell_length_c                   17.8163(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.291(5)
_cell_angle_gamma                90.00
_cell_volume                     3687.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    5933
_cell_measurement_theta_min      3.59
_cell_measurement_theta_max      73.12

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18017
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.57
_diffrn_reflns_theta_max         73.75
_reflns_number_total             7093
_reflns_number_gt                4969
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The pyridine molecule N50-C55 is disordered over two sites, with refined 
 occupancies of 0.60:0.40. This disorder was modelled without the use of 
 restraints. No disorder is present in the model, and no restraints were 
 applied. All non-H atoms except the disordered solvent were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0562P)²+1.3933P] 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         7093
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1280
_refine_ls_wR_factor_gt          0.1117
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22093(3) 0.74726(3) 0.37965(2) 0.04624(13) Uani 1 1 d . . .
N2 N 0.2853(2) 0.75217(17) 0.28931(17) 0.0684(7) Uani 1 1 d . . .
C3 C 0.3202(2) 0.75216(16) 0.23893(17) 0.0515(6) Uani 1 1 d . . .
S4 S 0.37017(8) 0.75036(5) 0.16847(5) 0.0731(2) Uani 1 1 d . . .
N5 N 0.0637(2) 0.74574(15) 0.30260(15) 0.0607(6) Uani 1 1 d . . .
C6 C -0.0228(2) 0.75196(16) 0.26180(16) 0.0515(6) Uani 1 1 d . . .
S7 S -0.14611(7) 0.76104(6) 0.20471(5) 0.0737(3) Uani 1 1 d . . .
C8 C 0.1976(2) 0.90950(16) 0.45478(16) 0.0494(6) Uani 1 1 d . . .
N9 N 0.23351(18) 0.87980(14) 0.39794(14) 0.0542(6) Uani 1 1 d . . .
C10 C 0.2658(3) 0.9331(2) 0.3549(2) 0.0672(8) Uani 1 1 d . . .
H10 H 0.2899 0.9134 0.3154 0.081 Uiso 1 1 calc R . .
C11 C 0.2650(3) 1.0174(2) 0.3669(2) 0.0793(11) Uani 1 1 d . . .
H11 H 0.2886 1.0528 0.3358 0.095 Uiso 1 1 calc R . .
C12 C 0.2297(3) 1.0478(2) 0.4239(2) 0.0776(11) Uani 1 1 d . . .
H12 H 0.2291 1.1040 0.4322 0.093 Uiso 1 1 calc R . .
C13 C 0.1942(2) 0.99362(17) 0.47021(19) 0.0596(8) Uani 1 1 d . . .
C14 C 0.16078(19) 0.85060(16) 0.49994(16) 0.0471(6) Uani 1 1 d . . .
N15 N 0.16448(17) 0.77013(13) 0.48094(13) 0.0475(5) Uani 1 1 d . . .
C16 C 0.1287(2) 0.71583(19) 0.52069(18) 0.0575(7) Uani 1 1 d . . .
H16 H 0.1317 0.6606 0.5087 0.069 Uiso 1 1 calc R . .
C17 C 0.0869(3) 0.7369(2) 0.5793(2) 0.0653(8) Uani 1 1 d . . .
H17 H 0.0624 0.6965 0.6053 0.078 Uiso 1 1 calc R . .
C18 C 0.0823(2) 0.8169(2) 0.59816(18) 0.0647(8) Uani 1 1 d . . .
H18 H 0.0543 0.8321 0.6370 0.078 Uiso 1 1 calc R . .
C19 C 0.1203(2) 0.87650(18) 0.55821(17) 0.0542(7) Uani 1 1 d . . .
C20 C 0.1528(2) 1.02036(19) 0.5316(2) 0.0652(9) Uani 1 1 d . . .
N21 N 0.1500(3) 1.10235(17) 0.5447(2) 0.0863(10) Uani 1 1 d . . .
C22 C 0.1106(4) 1.1236(3) 0.6009(3) 0.0980(15) Uani 1 1 d . . .
H22 H 0.1078 1.1789 0.6128 0.118 Uiso 1 1 calc R . .
C23 C 0.0739(3) 1.0670(3) 0.6420(3) 0.0953(14) Uani 1 1 d . . .
H23 H 0.0467 1.0858 0.6801 0.114 Uiso 1 1 calc R . .
N24 N 0.0753(2) 0.9875(2) 0.63017(17) 0.0799(9) Uani 1 1 d . . .
C25 C 0.1168(2) 0.9639(2) 0.57393(19) 0.0626(8) Uani 1 1 d . . .
C26 C 0.30759(19) 0.58497(15) 0.45855(14) 0.0425(6) Uani 1 1 d . . .
N27 N 0.22616(17) 0.61488(14) 0.39611(13) 0.0496(5) Uani 1 1 d . . .
C28 C 0.1566(3) 0.56124(19) 0.35121(19) 0.0666(9) Uani 1 1 d . . .
H28 H 0.0995 0.5810 0.3088 0.080 Uiso 1 1 calc R . .
C29 C 0.1649(3) 0.4778(2) 0.3644(2) 0.0766(10) Uani 1 1 d . . .
H29 H 0.1161 0.4424 0.3300 0.092 Uiso 1 1 calc R . .
C30 C 0.2454(3) 0.44743(18) 0.4286(2) 0.0655(8) Uani 1 1 d . . .
H30 H 0.2509 0.3914 0.4391 0.079 Uiso 1 1 calc R . .
C31 C 0.3189(2) 0.50181(16) 0.47803(16) 0.0489(6) Uani 1 1 d . . .
C32 C 0.38626(19) 0.64373(15) 0.50443(14) 0.0417(5) Uani 1 1 d . . .
N33 N 0.37430(17) 0.72202(13) 0.47725(13) 0.0467(5) Uani 1 1 d . . .
C34 C 0.4493(2) 0.77491(19) 0.5152(2) 0.0629(8) Uani 1 1 d . . .
H34 H 0.4426 0.8288 0.4971 0.075 Uiso 1 1 calc R . .
C35 C 0.5377(3) 0.75401(19) 0.5808(2) 0.0685(9) Uani 1 1 d . . .
H35 H 0.5893 0.7930 0.6044 0.082 Uiso 1 1 calc R . .
C36 C 0.5479(2) 0.67628(18) 0.60985(18) 0.0584(7) Uani 1 1 d . . .
H36 H 0.6051 0.6620 0.6548 0.070 Uiso 1 1 calc R . .
C37 C 0.4712(2) 0.61804(16) 0.57109(15) 0.0460(6) Uani 1 1 d . . .
C38 C 0.4060(2) 0.47529(16) 0.54877(16) 0.0485(6) Uani 1 1 d . . .
N39 N 0.4132(2) 0.39503(15) 0.56764(15) 0.0614(6) Uani 1 1 d . . .
C40 C 0.4901(3) 0.3747(2) 0.6344(2) 0.0693(9) Uani 1 1 d . . .
H40 H 0.4985 0.3199 0.6496 0.083 Uiso 1 1 calc R . .
C41 C 0.5585(3) 0.4321(2) 0.6825(2) 0.0733(10) Uani 1 1 d . . .
H41 H 0.6093 0.4143 0.7298 0.088 Uiso 1 1 calc R . .
N42 N 0.5550(2) 0.51070(15) 0.66450(15) 0.0636(7) Uani 1 1 d . . .
C43 C 0.4775(2) 0.53299(16) 0.59579(16) 0.0483(6) Uani 1 1 d . . .
N44 N 0.4641(3) 1.0661(3) 0.5849(3) 0.1148(13) Uani 1 1 d . . .
C45 C 0.4380(5) 1.1147(4) 0.6335(4) 0.131(2) Uani 1 1 d . . .
H45 H 0.4443 1.1711 0.6287 0.157 Uiso 1 1 calc R . .
C46 C 0.4004(5) 1.0842(6) 0.6931(4) 0.144(3) Uani 1 1 d . . .
H46 H 0.3816 1.1183 0.7277 0.173 Uiso 1 1 calc R . .
C47 C 0.3940(4) 1.0003(5) 0.6957(3) 0.120(2) Uani 1 1 d . . .
H47 H 0.3693 0.9759 0.7330 0.144 Uiso 1 1 calc R . .
C48 C 0.4225(3) 0.9535(3) 0.6457(3) 0.0988(14) Uani 1 1 d . . .
H48 H 0.4180 0.8968 0.6485 0.119 Uiso 1 1 calc R . .
C49 C 0.4568(3) 0.9866(3) 0.5926(3) 0.0887(11) Uani 1 1 d . . .
H49 H 0.4770 0.9523 0.5588 0.106 Uiso 1 1 calc R . .
N50A N 0.1260(6) 0.5229(5) 0.5930(5) 0.101(2) Uiso 0.60 1 d P A 1
C51A C 0.2235(7) 0.5262(5) 0.6377(5) 0.081(2) Uiso 0.60 1 d P A 1
H51A H 0.2579 0.5761 0.6407 0.097 Uiso 0.60 1 calc PR A 1
C52A C 0.2819(7) 0.4619(6) 0.6817(5) 0.082(2) Uiso 0.60 1 d P A 1
H52A H 0.3509 0.4691 0.7162 0.099 Uiso 0.60 1 calc PR A 1
C53A C 0.2319(8) 0.3850(7) 0.6718(6) 0.098(2) Uiso 0.60 1 d P A 1
H53A H 0.2665 0.3389 0.6991 0.118 Uiso 0.60 1 calc PR A 1
C54A C 0.1311(7) 0.3813(5) 0.6205(5) 0.099(2) Uiso 0.60 1 d P A 1
H54A H 0.0953 0.3316 0.6119 0.118 Uiso 0.60 1 calc PR A 1
C55A C 0.0818(7) 0.4492(5) 0.5816(5) 0.093(2) Uiso 0.60 1 d P A 1
H55A H 0.0136 0.4440 0.5451 0.112 Uiso 0.60 1 calc PR A 1
N50B N 0.1508(9) 0.5067(7) 0.5747(6) 0.091(3) Uiso 0.40 1 d P B 2
C51B C 0.2426(13) 0.4994(11) 0.6535(10) 0.103(5) Uiso 0.40 1 d P B 2
H51B H 0.2752 0.5462 0.6807 0.123 Uiso 0.40 1 calc PR B 2
C52B C 0.2765(11) 0.4241(9) 0.6836(7) 0.086(3) Uiso 0.40 1 d P B 2
H52B H 0.3313 0.4196 0.7324 0.103 Uiso 0.40 1 calc PR B 2
C53B C 0.2326(13) 0.3565(10) 0.6441(10) 0.123(5) Uiso 0.40 1 d P B 2
H53B H 0.2617 0.3057 0.6635 0.147 Uiso 0.40 1 calc PR B 2
C54B C 0.1491(12) 0.3596(9) 0.5787(9) 0.119(4) Uiso 0.40 1 d P B 2
H54B H 0.1177 0.3118 0.5528 0.143 Uiso 0.40 1 calc PR B 2
C55B C 0.1104(11) 0.4329(8) 0.5503(8) 0.105(4) Uiso 0.40 1 d P B 2
H55B H 0.0466 0.4325 0.5077 0.126 Uiso 0.40 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.080(3) . ?
Fe1 N5 2.093(2) . ?
Fe1 N27 2.177(2) . ?
Fe1 N9 2.185(2) . ?
Fe1 N15 2.221(2) . ?
Fe1 N33 2.235(2) . ?
N2 C3 1.151(4) . ?
C3 S4 1.619(3) . ?
N5 C6 1.148(4) . ?
C6 S7 1.632(3) . ?
C8 N9 1.355(4) . ?
C8 C13 1.403(4) . ?
C8 C14 1.448(4) . ?
N9 C10 1.330(4) . ?
C10 C11 1.391(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.358(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.402(5) . ?
C12 H12 0.9300 . ?
C13 C20 1.457(5) . ?
C14 N15 1.361(3) . ?
C14 C19 1.396(4) . ?
N15 C16 1.326(4) . ?
C16 C17 1.392(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.355(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.404(5) . ?
C18 H18 0.9300 . ?
C19 C25 1.457(4) . ?
C20 N21 1.361(4) . ?
C20 C25 1.382(5) . ?
N21 C22 1.333(6) . ?
C22 C23 1.374(7) . ?
C22 H22 0.9300 . ?
C23 N24 1.315(5) . ?
C23 H23 0.9300 . ?
N24 C25 1.363(5) . ?
C26 N27 1.356(3) . ?
C26 C31 1.396(4) . ?
C26 C32 1.455(3) . ?
N27 C28 1.330(3) . ?
C28 C29 1.380(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.369(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.394(4) . ?
C30 H30 0.9300 . ?
C31 C38 1.461(4) . ?
C32 N33 1.356(3) . ?
C32 C37 1.400(3) . ?
N33 C34 1.325(4) . ?
C34 C35 1.394(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.359(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.400(4) . ?
C36 H36 0.9300 . ?
C37 C43 1.449(4) . ?
C38 N39 1.347(4) . ?
C38 C43 1.400(4) . ?
N39 C40 1.322(4) . ?
C40 C41 1.384(5) . ?
C40 H40 0.9300 . ?
C41 N42 1.319(4) . ?
C41 H41 0.9300 . ?
N42 C43 1.356(3) . ?
N44 C45 1.309(7) . ?
N44 C49 1.312(6) . ?
C45 C46 1.418(9) . ?
C45 H45 0.9300 . ?
C46 C47 1.372(8) . ?
C46 H46 0.9300 . ?
C47 C48 1.328(7) . ?
C47 H47 0.9300 . ?
C48 C49 1.306(6) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
N50A C51A 1.284(10) . ?
N50A C55A 1.326(10) . ?
C51A C52A 1.381(13) . ?
C51A H51A 0.9300 . ?
C52A C53A 1.407(13) . ?
C52A H52A 0.9300 . ?
C53A C54A 1.354(12) . ?
C53A H53A 0.9300 . ?
C54A C55A 1.353(10) . ?
C54A H54A 0.9300 . ?
C55A H55A 0.9300 . ?
N50B C55B 1.331(15) . ?
N50B C51B 1.52(2) . ?
C51B C52B 1.36(2) . ?
C51B H51B 0.9300 . ?
C52B C53B 1.33(2) . ?
C52B H52B 0.9300 . ?
C53B C54B 1.313(18) . ?
C53B H53B 0.9300 . ?
C54B C55B 1.333(17) . ?
C54B H54B 0.9300 . ?
C55B H55B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N5 95.49(11) . . ?
N2 Fe1 N27 98.03(10) . . ?
N5 Fe1 N27 93.14(9) . . ?
N2 Fe1 N9 92.61(10) . . ?
N5 Fe1 N9 96.80(9) . . ?
N27 Fe1 N9 164.68(9) . . ?
N2 Fe1 N15 167.46(10) . . ?
N5 Fe1 N15 88.72(9) . . ?
N27 Fe1 N15 93.52(9) . . ?
N9 Fe1 N15 75.14(9) . . ?
N2 Fe1 N33 94.85(10) . . ?
N5 Fe1 N33 164.96(9) . . ?
N27 Fe1 N33 74.59(8) . . ?
N9 Fe1 N33 93.62(8) . . ?
N15 Fe1 N33 83.49(8) . . ?
C3 N2 Fe1 177.7(3) . . ?
N2 C3 S4 178.9(3) . . ?
C6 N5 Fe1 174.1(2) . . ?
N5 C6 S7 179.3(3) . . ?
N9 C8 C13 122.7(3) . . ?
N9 C8 C14 117.3(2) . . ?
C13 C8 C14 119.9(3) . . ?
C10 N9 C8 118.1(3) . . ?
C10 N9 Fe1 125.9(2) . . ?
C8 N9 Fe1 115.84(18) . . ?
N9 C10 C11 122.5(4) . . ?
N9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C8 117.4(3) . . ?
C12 C13 C20 123.5(3) . . ?
C8 C13 C20 119.1(3) . . ?
N15 C14 C19 122.3(3) . . ?
N15 C14 C8 116.9(3) . . ?
C19 C14 C8 120.8(3) . . ?
C16 N15 C14 117.4(3) . . ?
C16 N15 Fe1 127.9(2) . . ?
C14 N15 Fe1 114.62(18) . . ?
N15 C16 C17 123.7(3) . . ?
N15 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C18 C17 C16 119.3(3) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 119.0(3) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C14 C19 C18 118.3(3) . . ?
C14 C19 C25 119.1(3) . . ?
C18 C19 C25 122.6(3) . . ?
N21 C20 C25 121.7(4) . . ?
N21 C20 C13 117.7(4) . . ?
C25 C20 C13 120.7(3) . . ?
C22 N21 C20 115.3(4) . . ?
N21 C22 C23 122.5(4) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
N24 C23 C22 123.4(4) . . ?
N24 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C23 N24 C25 115.3(4) . . ?
N24 C25 C20 121.8(3) . . ?
N24 C25 C19 117.8(3) . . ?
C20 C25 C19 120.4(3) . . ?
N27 C26 C31 122.8(2) . . ?
N27 C26 C32 116.8(2) . . ?
C31 C26 C32 120.3(2) . . ?
C28 N27 C26 117.4(2) . . ?
C28 N27 Fe1 126.04(19) . . ?
C26 N27 Fe1 116.53(17) . . ?
N27 C28 C29 123.2(3) . . ?
N27 C28 H28 118.4 . . ?
C29 C28 H28 118.4 . . ?
C30 C29 C28 119.6(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 118.9(3) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C26 118.0(3) . . ?
C30 C31 C38 122.8(3) . . ?
C26 C31 C38 119.2(2) . . ?
N33 C32 C37 123.1(2) . . ?
N33 C32 C26 116.5(2) . . ?
C37 C32 C26 120.3(2) . . ?
C34 N33 C32 117.1(2) . . ?
C34 N33 Fe1 128.1(2) . . ?
C32 N33 Fe1 114.53(16) . . ?
N33 C34 C35 123.4(3) . . ?
N33 C34 H34 118.3 . . ?
C35 C34 H34 118.3 . . ?
C36 C35 C34 119.5(3) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C37 119.0(3) . . ?
C35 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C32 C37 C36 117.7(2) . . ?
C32 C37 C43 119.3(2) . . ?
C36 C37 C43 123.0(2) . . ?
N39 C38 C43 121.9(2) . . ?
N39 C38 C31 118.1(3) . . ?
C43 C38 C31 120.0(2) . . ?
C40 N39 C38 115.7(3) . . ?
N39 C40 C41 122.4(3) . . ?
N39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
N42 C41 C40 123.1(3) . . ?
N42 C41 H41 118.4 . . ?
C40 C41 H41 118.4 . . ?
C41 N42 C43 115.6(3) . . ?
N42 C43 C38 121.1(2) . . ?
N42 C43 C37 118.5(2) . . ?
C38 C43 C37 120.4(2) . . ?
C45 N44 C49 118.8(5) . . ?
N44 C45 C46 122.1(6) . . ?
N44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C47 C46 C45 114.8(5) . . ?
C47 C46 H46 122.6 . . ?
C45 C46 H46 122.6 . . ?
C48 C47 C46 120.9(6) . . ?
C48 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
C49 C48 C47 120.5(5) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C48 C49 N44 122.9(5) . . ?
C48 C49 H49 118.5 . . ?
N44 C49 H49 118.5 . . ?
C51A N50A C55A 116.3(8) . . ?
N50A C51A C52A 125.6(8) . . ?
N50A C51A H51A 117.2 . . ?
C52A C51A H51A 117.2 . . ?
C51A C52A C53A 116.8(8) . . ?
C51A C52A H52A 121.6 . . ?
C53A C52A H52A 121.6 . . ?
C54A C53A C52A 116.9(8) . . ?
C54A C53A H53A 121.6 . . ?
C52A C53A H53A 121.6 . . ?
C55A C54A C53A 120.7(9) . . ?
C55A C54A H54A 119.6 . . ?
C53A C54A H54A 119.6 . . ?
N50A C55A C54A 123.2(8) . . ?
N50A C55A H55A 118.4 . . ?
C54A C55A H55A 118.4 . . ?
C55B N50B C51B 110.0(11) . . ?
C52B C51B N50B 119.4(13) . . ?
C52B C51B H51B 120.3 . . ?
N50B C51B H51B 120.3 . . ?
C53B C52B C51B 121.0(13) . . ?
C53B C52B H52B 119.5 . . ?
C51B C52B H52B 119.5 . . ?
C54B C53B C52B 121.7(15) . . ?
C54B C53B H53B 119.2 . . ?
C52B C53B H53B 119.2 . . ?
C53B C54B C55B 118.4(15) . . ?
C53B C54B H54B 120.8 . . ?
C55B C54B H54B 120.8 . . ?
N50B C55B C54B 128.6(14) . . ?
N50B C55B H55B 115.7 . . ?
C54B C55B H55B 115.7 . . ?

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.042
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pyridine/diethyl ether'
####################################################################### 
# 
# 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_rk119b
_database_code_depnum_ccdc_archive 'CCDC 1430810'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Tris-[dipyrido[3,2-a:23-c]phenazine]iron(II) diperchlorate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H30 Fe N12, 2(Cl O4)'
_chemical_formula_sum            'C54 H30 Cl2 Fe N12 O8'
_chemical_formula_weight         1101.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   24.6343(9)
_cell_length_b                   21.2193(4)
_cell_length_c                   18.1944(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.239(3)
_cell_angle_gamma                90.00
_cell_volume                     9218.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    34342
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      31.21

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4496
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
SADABS (Sheldrick, 2002).  University of Gottingen, Germany.
;

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.69980
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Diamond Light Source station I19'
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            122082
_diffrn_reflns_av_R_equivalents  0.1672
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         24.21
_reflns_number_total             16170
_reflns_number_gt                12179
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains two formula units (Z' = 2), with all moieties
 lying on general crystallographic positions. One anion, Cl73-O77, was 
 clearly disordered and modelled over three orientations, with a 
 0.5:0.25:0.25 occupancy ratio. The fixed restraints Cl---O = 1.45(2) and
 O...O = 2.37(2) Å were applied to this residue. All non-H atoms except 
 the disordered anion were refined anisotropically, while H atoms were
 placed in calculated positions and refined using a riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1045P)²+5.4211P] 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         16170
_refine_ls_number_parameters     1402
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1819
_refine_ls_wR_factor_gt          0.1646
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.98910(2) 0.70938(2) 0.78997(3) 0.02834(14) Uani 1 1 d . . .
C2A C 1.08867(15) 0.75603(16) 0.8868(2) 0.0321(8) Uani 1 1 d . . .
N3A N 1.04417(12) 0.77681(13) 0.83169(17) 0.0320(7) Uani 1 1 d . . .
C4A C 1.04238(16) 0.83913(16) 0.8155(2) 0.0358(8) Uani 1 1 d . . .
H4A H 1.0123 0.8546 0.7763 0.043 Uiso 1 1 calc R . .
C5A C 1.08269(16) 0.88159(17) 0.8536(2) 0.0384(9) Uani 1 1 d . . .
H5A H 1.0801 0.9249 0.8400 0.046 Uiso 1 1 calc R . .
C6A C 1.12624(16) 0.86062(17) 0.9111(2) 0.0372(8) Uani 1 1 d . . .
H6A H 1.1535 0.8893 0.9384 0.045 Uiso 1 1 calc R . .
C7A C 1.12972(15) 0.79598(17) 0.9288(2) 0.0342(8) Uani 1 1 d . . .
C8A C 1.09001(15) 0.68866(17) 0.8991(2) 0.0323(8) Uani 1 1 d . . .
N9A N 1.04864(12) 0.65491(13) 0.85200(16) 0.0306(6) Uani 1 1 d . . .
C10A C 1.04855(16) 0.59211(16) 0.8619(2) 0.0345(8) Uani 1 1 d . . .
H10A H 1.0205 0.5678 0.8289 0.041 Uiso 1 1 calc R . .
C11A C 1.08818(16) 0.56110(18) 0.9189(2) 0.0426(9) Uani 1 1 d . . .
H11A H 1.0864 0.5167 0.9247 0.051 Uiso 1 1 calc R . .
C12A C 1.12999(17) 0.59581(18) 0.9669(2) 0.0435(9) Uani 1 1 d . . .
H12A H 1.1571 0.5756 1.0059 0.052 Uiso 1 1 calc R . .
C13A C 1.13162(15) 0.66118(17) 0.9568(2) 0.0356(8) Uani 1 1 d . . .
C14A C 1.17330(15) 0.76865(17) 0.9907(2) 0.0334(8) Uani 1 1 d . . .
N15A N 1.20963(13) 0.80809(15) 1.03494(18) 0.0397(7) Uani 1 1 d . . .
C16A C 1.24816(17) 0.78174(19) 1.0933(2) 0.0423(9) Uani 1 1 d . . .
C17A C 1.25027(16) 0.7147(2) 1.1049(2) 0.0412(9) Uani 1 1 d . . .
N18A N 1.21292(13) 0.67539(15) 1.06004(18) 0.0400(7) Uani 1 1 d . . .
C19A C 1.17454(15) 0.70172(17) 1.0040(2) 0.0359(8) Uani 1 1 d . . .
C20A C 1.28605(19) 0.8211(2) 1.1452(3) 0.0570(12) Uani 1 1 d . . .
H20A H 1.2849 0.8655 1.1383 0.068 Uiso 1 1 calc R . .
C21A C 1.3238(2) 0.7952(2) 1.2045(3) 0.0610(13) Uani 1 1 d . . .
H21A H 1.3488 0.8218 1.2391 0.073 Uiso 1 1 calc R . .
C22A C 1.32668(18) 0.7293(3) 1.2155(2) 0.0549(12) Uani 1 1 d . . .
H22A H 1.3534 0.7124 1.2577 0.066 Uiso 1 1 calc R . .
C23A C 1.29195(17) 0.6893(2) 1.1668(2) 0.0460(10) Uani 1 1 d . . .
H23A H 1.2954 0.6451 1.1740 0.055 Uiso 1 1 calc R . .
C24A C 0.94272(14) 0.62121(15) 0.67460(18) 0.0279(7) Uani 1 1 d . . .
N25A N 0.93871(12) 0.63903(13) 0.74579(16) 0.0293(6) Uani 1 1 d . . .
C26A C 0.90065(15) 0.60827(16) 0.7740(2) 0.0332(8) Uani 1 1 d . . .
H26A H 0.8976 0.6186 0.8237 0.040 Uiso 1 1 calc R . .
C27A C 0.86531(15) 0.56178(17) 0.7336(2) 0.0347(8) Uani 1 1 d . . .
H27A H 0.8386 0.5420 0.7557 0.042 Uiso 1 1 calc R . .
C28A C 0.86897(15) 0.54456(16) 0.6621(2) 0.0339(8) Uani 1 1 d . . .
H28A H 0.8445 0.5137 0.6338 0.041 Uiso 1 1 calc R . .
C29A C 0.91006(14) 0.57405(15) 0.63196(19) 0.0293(7) Uani 1 1 d . . .
C30A C 0.98478(14) 0.65478(15) 0.64691(19) 0.0289(7) Uani 1 1 d . . .
N31A N 1.01408(12) 0.69945(13) 0.69511(17) 0.0316(7) Uani 1 1 d . . .
C32A C 1.05345(17) 0.73180(18) 0.6712(2) 0.0407(9) Uani 1 1 d . . .
H32A H 1.0756 0.7616 0.7045 0.049 Uiso 1 1 calc R . .
C33A C 1.06325(17) 0.72320(18) 0.5984(2) 0.0431(9) Uani 1 1 d . . .
H33A H 1.0903 0.7484 0.5828 0.052 Uiso 1 1 calc R . .
C34A C 1.03328(16) 0.67791(18) 0.5501(2) 0.0388(9) Uani 1 1 d . . .
H34A H 1.0398 0.6712 0.5013 0.047 Uiso 1 1 calc R . .
C35A C 0.99316(14) 0.64229(16) 0.57467(19) 0.0297(7) Uani 1 1 d . . .
C36A C 0.91939(14) 0.55793(15) 0.55760(19) 0.0302(7) Uani 1 1 d . . .
N37A N 0.88991(13) 0.51052(13) 0.51941(17) 0.0337(7) Uani 1 1 d . . .
C38A C 0.89906(16) 0.49643(16) 0.4508(2) 0.0352(8) Uani 1 1 d . . .
C39A C 0.93823(16) 0.53215(17) 0.4204(2) 0.0367(9) Uani 1 1 d . . .
N40A N 0.96874(13) 0.57979(14) 0.46039(16) 0.0344(7) Uani 1 1 d . . .
C41A C 0.95995(15) 0.59244(16) 0.52842(19) 0.0311(8) Uani 1 1 d . . .
C42A C 0.86895(18) 0.44601(18) 0.4077(2) 0.0420(9) Uani 1 1 d . . .
H42A H 0.8438 0.4214 0.4279 0.050 Uiso 1 1 calc R . .
C43A C 0.87624(19) 0.43297(19) 0.3370(2) 0.0468(10) Uani 1 1 d . . .
H43A H 0.8560 0.3994 0.3083 0.056 Uiso 1 1 calc R . .
C44A C 0.91364(19) 0.4691(2) 0.3065(2) 0.0501(11) Uani 1 1 d . . .
H44A H 0.9174 0.4598 0.2569 0.060 Uiso 1 1 calc R . .
C45A C 0.94472(18) 0.51710(18) 0.3465(2) 0.0418(9) Uani 1 1 d . . .
H45A H 0.9703 0.5401 0.3254 0.050 Uiso 1 1 calc R . .
C46A C 0.91381(14) 0.76158(15) 0.86769(19) 0.0278(7) Uani 1 1 d . . .
N47A N 0.95503(12) 0.71711(13) 0.87742(16) 0.0288(6) Uani 1 1 d . . .
C48A C 0.96429(16) 0.68264(16) 0.94167(19) 0.0323(8) Uani 1 1 d . . .
H48A H 0.9929 0.6516 0.9501 0.039 Uiso 1 1 calc R . .
C49A C 0.93391(16) 0.69047(17) 0.9961(2) 0.0358(8) Uani 1 1 d . . .
H49A H 0.9411 0.6640 1.0395 0.043 Uiso 1 1 calc R . .
C50A C 0.89340(16) 0.73666(17) 0.9870(2) 0.0355(8) Uani 1 1 d . . .
H50A H 0.8728 0.7429 1.0243 0.043 Uiso 1 1 calc R . .
C51A C 0.88313(14) 0.77436(16) 0.92152(19) 0.0292(7) Uani 1 1 d . . .
C52A C 0.90197(14) 0.79457(15) 0.79577(19) 0.0289(7) Uani 1 1 d . . .
N53A N 0.93174(12) 0.77387(13) 0.74650(16) 0.0297(6) Uani 1 1 d . . .
C54A C 0.92190(16) 0.80320(18) 0.6786(2) 0.0377(9) Uani 1 1 d . . .
H54A H 0.9418 0.7896 0.6429 0.045 Uiso 1 1 calc R . .
C55A C 0.88383(17) 0.85260(19) 0.6589(2) 0.0426(9) Uani 1 1 d . . .
H55A H 0.8786 0.8720 0.6106 0.051 Uiso 1 1 calc R . .
C56A C 0.85386(16) 0.87351(18) 0.7085(2) 0.0379(8) Uani 1 1 d . . .
H56A H 0.8281 0.9074 0.6954 0.045 Uiso 1 1 calc R . .
C57A C 0.86255(14) 0.84316(16) 0.7796(2) 0.0300(7) Uani 1 1 d . . .
C58A C 0.84215(14) 0.82581(16) 0.90645(19) 0.0314(8) Uani 1 1 d . . .
N59A N 0.81550(13) 0.83958(14) 0.95993(17) 0.0358(7) Uani 1 1 d . . .
C60A C 0.78050(16) 0.88971(18) 0.9471(2) 0.0372(8) Uani 1 1 d . . .
C61A C 0.77265(15) 0.92632(17) 0.8787(2) 0.0352(8) Uani 1 1 d . . .
N62A N 0.79826(12) 0.91010(13) 0.82315(18) 0.0348(7) Uani 1 1 d . . .
C63A C 0.83249(14) 0.86097(16) 0.8367(2) 0.0312(8) Uani 1 1 d . . .
C64A C 0.75280(17) 0.9081(2) 1.0043(2) 0.0444(10) Uani 1 1 d . . .
H64A H 0.7564 0.8836 1.0489 0.053 Uiso 1 1 calc R . .
C65A C 0.72132(18) 0.9614(2) 0.9934(3) 0.0514(11) Uani 1 1 d . . .
H65A H 0.7034 0.9742 1.0316 0.062 Uiso 1 1 calc R . .
C66A C 0.71434(18) 0.9986(2) 0.9274(3) 0.0510(11) Uani 1 1 d . . .
H66A H 0.6925 1.0360 0.9224 0.061 Uiso 1 1 calc R . .
C67A C 0.73888(17) 0.98143(18) 0.8701(2) 0.0438(9) Uani 1 1 d . . .
H67A H 0.7333 1.0061 0.8253 0.053 Uiso 1 1 calc R . .
Fe1B Fe 0.52621(2) 0.71061(2) 0.68025(3) 0.03415(15) Uani 1 1 d . . .
C2B C 0.42972(15) 0.65696(17) 0.5849(2) 0.0352(8) Uani 1 1 d . . .
N3B N 0.47437(12) 0.63937(14) 0.64220(18) 0.0358(7) Uani 1 1 d . . .
C4B C 0.48339(17) 0.57735(19) 0.6532(3) 0.0453(10) Uani 1 1 d . . .
H4B H 0.5123 0.5638 0.6951 0.054 Uiso 1 1 calc R . .
C5B C 0.45197(17) 0.5319(2) 0.6056(3) 0.0507(11) Uani 1 1 d . . .
H5B H 0.4604 0.4885 0.6147 0.061 Uiso 1 1 calc R . .
C6B C 0.40870(17) 0.54987(19) 0.5454(3) 0.0457(10) Uani 1 1 d . . .
H6B H 0.3882 0.5194 0.5113 0.055 Uiso 1 1 calc R . .
C7B C 0.39576(15) 0.61412(18) 0.5359(2) 0.0379(9) Uani 1 1 d . . .
C8B C 0.42087(16) 0.72416(17) 0.5768(2) 0.0352(8) Uani 1 1 d . . .
N9B N 0.45999(13) 0.76069(14) 0.62306(17) 0.0353(7) Uani 1 1 d . . .
C10B C 0.45009(16) 0.82325(17) 0.6219(2) 0.0370(8) Uani 1 1 d . . .
H10B H 0.4762 0.8497 0.6552 0.044 Uiso 1 1 calc R . .
C11B C 0.40304(16) 0.85081(18) 0.5739(2) 0.0385(9) Uani 1 1 d . . .
H11B H 0.3975 0.8950 0.5758 0.046 Uiso 1 1 calc R . .
C12B C 0.36442(16) 0.81435(17) 0.5238(2) 0.0376(8) Uani 1 1 d . . .
H12B H 0.3326 0.8330 0.4906 0.045 Uiso 1 1 calc R . .
C13B C 0.37352(15) 0.74835(17) 0.5234(2) 0.0352(8) Uani 1 1 d . . .
C14B C 0.34843(15) 0.63845(17) 0.4759(2) 0.0371(8) Uani 1 1 d . . .
N15B N 0.31734(13) 0.59675(15) 0.42842(19) 0.0397(7) Uani 1 1 d . . .
C16B C 0.27509(16) 0.62000(18) 0.3733(2) 0.0390(9) Uani 1 1 d . . .
C17B C 0.26352(16) 0.68665(18) 0.3673(2) 0.0368(8) Uani 1 1 d . . .
N18B N 0.29493(13) 0.72815(15) 0.41679(17) 0.0367(7) Uani 1 1 d . . .
C19B C 0.33732(15) 0.70449(17) 0.4709(2) 0.0350(8) Uani 1 1 d . . .
C20B C 0.24164(16) 0.57851(19) 0.3185(2) 0.0428(9) Uani 1 1 d . . .
H20B H 0.2487 0.5345 0.3214 0.051 Uiso 1 1 calc R . .
C21B C 0.19937(17) 0.6023(2) 0.2616(2) 0.0442(9) Uani 1 1 d . . .
H21B H 0.1773 0.5744 0.2255 0.053 Uiso 1 1 calc R . .
C22B C 0.18816(16) 0.66843(19) 0.2560(2) 0.0398(9) Uani 1 1 d . . .
H22B H 0.1589 0.6839 0.2159 0.048 Uiso 1 1 calc R . .
C23B C 0.21865(16) 0.70979(19) 0.3071(2) 0.0404(9) Uani 1 1 d . . .
H23B H 0.2103 0.7536 0.3031 0.049 Uiso 1 1 calc R . .
C24B C 0.60705(15) 0.79212(16) 0.6441(2) 0.0330(8) Uani 1 1 d . . .
N25B N 0.57790(13) 0.78448(14) 0.69841(18) 0.0362(7) Uani 1 1 d . . .
C26B C 0.58880(17) 0.82548(18) 0.7563(2) 0.0407(9) Uani 1 1 d . . .
H26B H 0.5690 0.8212 0.7947 0.049 Uiso 1 1 calc R . .
C27B C 0.62783(17) 0.87398(19) 0.7628(2) 0.0439(9) Uani 1 1 d . . .
H27B H 0.6338 0.9020 0.8047 0.053 Uiso 1 1 calc R . .
C28B C 0.65778(16) 0.88132(18) 0.7085(2) 0.0384(9) Uani 1 1 d . . .
H28B H 0.6850 0.9137 0.7131 0.046 Uiso 1 1 calc R . .
C29B C 0.64724(15) 0.83992(16) 0.6463(2) 0.0334(8) Uani 1 1 d . . .
C30B C 0.59530(15) 0.74609(17) 0.5835(2) 0.0343(8) Uani 1 1 d . . .
N31B N 0.55572(13) 0.70199(15) 0.58797(18) 0.0381(7) Uani 1 1 d . . .
C32B C 0.54494(18) 0.6574(2) 0.5327(2) 0.0469(10) Uani 1 1 d . . .
H32B H 0.5173 0.6264 0.5338 0.056 Uiso 1 1 calc R . .
C33B C 0.57257(19) 0.6549(2) 0.4745(3) 0.0540(11) Uani 1 1 d . . .
H33B H 0.5637 0.6228 0.4371 0.065 Uiso 1 1 calc R . .
C34B C 0.61268(18) 0.69918(19) 0.4713(2) 0.0454(10) Uani 1 1 d . . .
H34B H 0.6321 0.6976 0.4323 0.054 Uiso 1 1 calc R . .
C35B C 0.62441(15) 0.74660(17) 0.5265(2) 0.0358(8) Uani 1 1 d . . .
C36B C 0.67694(15) 0.84303(17) 0.5852(2) 0.0339(8) Uani 1 1 d . . .
N37B N 0.71324(13) 0.88954(14) 0.58555(17) 0.0358(7) Uani 1 1 d . . .
C38B C 0.74010(16) 0.88991(17) 0.5282(2) 0.0369(8) Uani 1 1 d . . .
C39B C 0.73038(16) 0.84130(18) 0.4716(2) 0.0386(9) Uani 1 1 d . . .
N40B N 0.69234(13) 0.79494(14) 0.47114(18) 0.0375(7) Uani 1 1 d . . .
C41B C 0.66609(15) 0.79569(17) 0.5263(2) 0.0339(8) Uani 1 1 d . . .
C42B C 0.77821(17) 0.93910(18) 0.5241(2) 0.0433(9) Uani 1 1 d . . .
H42B H 0.7843 0.9723 0.5602 0.052 Uiso 1 1 calc R . .
C43B C 0.80625(18) 0.93832(19) 0.4674(3) 0.0485(10) Uani 1 1 d . . .
H43B H 0.8323 0.9709 0.4653 0.058 Uiso 1 1 calc R . .
C44B C 0.79718(18) 0.8900(2) 0.4121(3) 0.0483(10) Uani 1 1 d . . .
H44B H 0.8170 0.8906 0.3734 0.058 Uiso 1 1 calc R . .
C45B C 0.76022(17) 0.84266(19) 0.4140(2) 0.0434(9) Uani 1 1 d . . .
H45B H 0.7544 0.8104 0.3766 0.052 Uiso 1 1 calc R . .
C46B C 0.52969(14) 0.67045(16) 0.8297(2) 0.0332(8) Uani 1 1 d . . .
N47B N 0.50421(13) 0.71554(14) 0.77847(18) 0.0356(7) Uani 1 1 d . . .
C48B C 0.46644(16) 0.75278(18) 0.7992(2) 0.0390(9) Uani 1 1 d . . .
H48B H 0.4491 0.7853 0.7655 0.047 Uiso 1 1 calc R . .
C49B C 0.45156(17) 0.74582(19) 0.8679(2) 0.0434(9) Uani 1 1 d . . .
H49B H 0.4255 0.7741 0.8808 0.052 Uiso 1 1 calc R . .
C50B C 0.47446(16) 0.69826(17) 0.9169(2) 0.0379(9) Uani 1 1 d . . .
H50B H 0.4627 0.6915 0.9622 0.045 Uiso 1 1 calc R . .
C51B C 0.51559(15) 0.65979(17) 0.8986(2) 0.0338(8) Uani 1 1 d . . .
C52B C 0.57419(15) 0.63585(17) 0.8086(2) 0.0341(8) Uani 1 1 d . . .
N53B N 0.58470(12) 0.65291(15) 0.74062(18) 0.0367(7) Uani 1 1 d . . .
C54B C 0.62820(16) 0.62481(19) 0.7221(2) 0.0411(9) Uani 1 1 d . . .
H54B H 0.6370 0.6362 0.6759 0.049 Uiso 1 1 calc R . .
C55B C 0.66111(17) 0.5793(2) 0.7681(2) 0.0453(10) Uani 1 1 d . . .
H55B H 0.6921 0.5614 0.7532 0.054 Uiso 1 1 calc R . .
C56B C 0.64935(17) 0.56036(19) 0.8342(2) 0.0428(9) Uani 1 1 d . . .
H56B H 0.6709 0.5283 0.8643 0.051 Uiso 1 1 calc R . .
C57B C 0.60433(15) 0.58945(17) 0.8570(2) 0.0363(8) Uani 1 1 d . . .
C58B C 0.54363(15) 0.60848(16) 0.9479(2) 0.0332(8) Uani 1 1 d . . .
N59B N 0.52612(13) 0.59472(13) 1.00961(17) 0.0351(7) Uani 1 1 d . . .
C60B C 0.55264(16) 0.54637(16) 1.0537(2) 0.0368(8) Uani 1 1 d . . .
C61B C 0.59832(16) 0.51389(17) 1.0351(2) 0.0387(9) Uani 1 1 d . . .
N62B N 0.61523(13) 0.52740(14) 0.97039(18) 0.0380(7) Uani 1 1 d . . .
C63B C 0.58805(15) 0.57381(17) 0.9270(2) 0.0362(8) Uani 1 1 d . . .
C64B C 0.53497(18) 0.52846(17) 1.1195(2) 0.0429(9) Uani 1 1 d . . .
H64B H 0.5037 0.5486 1.1312 0.051 Uiso 1 1 calc R . .
C65B C 0.56318(19) 0.48220(18) 1.1658(2) 0.0491(10) Uani 1 1 d . . .
H65B H 0.5515 0.4704 1.2099 0.059 Uiso 1 1 calc R . .
C66B C 0.61002(19) 0.45146(19) 1.1484(3) 0.0504(11) Uani 1 1 d . . .
H66B H 0.6295 0.4199 1.1816 0.061 Uiso 1 1 calc R . .
C67B C 0.62724(18) 0.46654(18) 1.0850(2) 0.0453(10) Uani 1 1 d . . .
H67B H 0.6584 0.4455 1.0742 0.054 Uiso 1 1 calc R . .
Cl68 Cl 0.22435(5) 0.59637(5) 0.84043(6) 0.0495(3) Uani 1 1 d . . .
O69 O 0.25050(13) 0.60253(15) 0.92049(17) 0.0568(8) Uani 1 1 d . . .
O70 O 0.26369(16) 0.6051(2) 0.7966(2) 0.0960(14) Uani 1 1 d . . .
O71 O 0.17952(13) 0.64191(13) 0.81743(17) 0.0524(7) Uani 1 1 d . . .
O72 O 0.20084(18) 0.53431(15) 0.8264(2) 0.0804(11) Uani 1 1 d . . .
Cl7A Cl 0.57349(13) 0.43115(15) 0.68132(18) 0.0530(9) Uiso 0.50 1 d PD A 1
O74A O 0.5372(4) 0.4416(5) 0.7347(5) 0.089(3) Uiso 0.50 1 d PD A 1
O75A O 0.6227(4) 0.3987(5) 0.7197(7) 0.120(4) Uiso 0.50 1 d PD A 1
O76A O 0.5848(4) 0.4891(4) 0.6485(5) 0.073(3) Uiso 0.50 1 d PD A 1
O77A O 0.5416(4) 0.3979(5) 0.6187(5) 0.105(3) Uiso 0.50 1 d PD A 1
Cl7B Cl 0.5617(3) 0.4228(3) 0.6914(4) 0.0387(17) Uiso 0.25 1 d PD B 2
O74B O 0.5104(4) 0.4105(5) 0.7072(7) 0.044(3) Uiso 0.25 1 d PD B 2
O75B O 0.6055(6) 0.4027(8) 0.7643(8) 0.093(5) Uiso 0.25 1 d PD B 2
O76B O 0.5793(7) 0.4849(6) 0.6828(10) 0.079(5) Uiso 0.25 1 d PD B 2
O77B O 0.5730(8) 0.3772(7) 0.6380(9) 0.103(6) Uiso 0.25 1 d PD B 2
Cl7C Cl 0.5609(3) 0.4305(3) 0.7089(4) 0.051(2) Uiso 0.25 1 d PD C 3
O74C O 0.5513(5) 0.4654(5) 0.7643(6) 0.043(3) Uiso 0.25 1 d PD C 3
O75C O 0.6063(4) 0.3834(5) 0.7238(6) 0.033(3) Uiso 0.25 1 d PD C 3
O76C O 0.5740(7) 0.4747(7) 0.6474(9) 0.062(5) Uiso 0.25 1 d PD C 3
O77C O 0.5142(5) 0.3934(6) 0.6648(8) 0.069(4) Uiso 0.25 1 d PD C 3
Cl78 Cl 0.95945(5) 0.43663(5) 0.86873(6) 0.0521(3) Uani 1 1 d . . .
O79 O 1.00596(15) 0.43787(16) 0.9344(2) 0.0738(10) Uani 1 1 d . . .
O80 O 0.97794(14) 0.45931(15) 0.80331(19) 0.0614(8) Uani 1 1 d . . .
O81 O 0.91485(16) 0.47615(18) 0.8803(2) 0.0766(10) Uani 1 1 d . . .
O82 O 0.94063(18) 0.37280(16) 0.8553(2) 0.0842(12) Uani 1 1 d . . .
Cl83 Cl 0.76476(5) 0.69976(5) 0.69993(6) 0.0537(3) Uani 1 1 d . . .
O84 O 0.80736(13) 0.69968(15) 0.76915(18) 0.0570(8) Uani 1 1 d . . .
O85 O 0.7847(3) 0.7279(2) 0.6428(3) 0.133(2) Uani 1 1 d . . .
O86 O 0.71804(18) 0.7328(2) 0.7135(3) 0.1109(17) Uani 1 1 d . . .
O87 O 0.74759(13) 0.63530(16) 0.67914(19) 0.0631(9) 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
Fe1A N47A 1.980(3) . ?
Fe1A N31A 1.981(3) . ?
Fe1A N25A 1.981(3) . ?
Fe1A N53A 1.986(3) . ?
Fe1A N9A 1.987(3) . ?
Fe1A N3A 1.989(3) . ?
C2A N3A 1.364(5) . ?
C2A C7A 1.394(5) . ?
C2A C8A 1.446(5) . ?
N3A C4A 1.353(4) . ?
C4A C5A 1.393(5) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.375(6) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.406(5) . ?
C6A H6A 0.9500 . ?
C7A C14A 1.471(5) . ?
C8A N9A 1.362(4) . ?
C8A C13A 1.401(5) . ?
N9A C10A 1.345(4) . ?
C10A C11A 1.401(5) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.386(6) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.401(5) . ?
C12A H12A 0.9500 . ?
C13A C19A 1.466(5) . ?
C14A N15A 1.340(5) . ?
C14A C19A 1.440(5) . ?
N15A C16A 1.358(5) . ?
C16A C20A 1.424(6) . ?
C16A C17A 1.438(6) . ?
C17A N18A 1.355(5) . ?
C17A C23A 1.429(6) . ?
N18A C19A 1.331(5) . ?
C20A C21A 1.356(7) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.411(7) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.365(6) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9500 . ?
C24A N25A 1.376(4) . ?
C24A C29A 1.394(5) . ?
C24A C30A 1.446(5) . ?
N25A C26A 1.344(4) . ?
C26A C27A 1.399(5) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.375(5) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.410(5) . ?
C28A H28A 0.9500 . ?
C29A C36A 1.468(5) . ?
C30A N31A 1.370(4) . ?
C30A C35A 1.405(5) . ?
N31A C32A 1.345(5) . ?
C32A C33A 1.414(5) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.387(6) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.402(5) . ?
C34A H34A 0.9500 . ?
C35A C41A 1.469(5) . ?
C36A N37A 1.332(4) . ?
C36A C41A 1.441(5) . ?
N37A C38A 1.356(5) . ?
C38A C42A 1.423(5) . ?
C38A C39A 1.440(6) . ?
C39A N40A 1.359(5) . ?
C39A C45A 1.429(5) . ?
N40A C41A 1.335(4) . ?
C42A C43A 1.369(6) . ?
C42A H42A 0.9500 . ?
C43A C44A 1.412(6) . ?
C43A H43A 0.9500 . ?
C44A C45A 1.371(6) . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9500 . ?
C46A N47A 1.365(4) . ?
C46A C51A 1.403(5) . ?
C46A C52A 1.449(5) . ?
N47A C48A 1.350(4) . ?
C48A C49A 1.390(5) . ?
C48A H48A 0.9500 . ?
C49A C50A 1.379(5) . ?
C49A H49A 0.9500 . ?
C50A C51A 1.406(5) . ?
C50A H50A 0.9500 . ?
C51A C58A 1.466(5) . ?
C52A N53A 1.363(4) . ?
C52A C57A 1.397(5) . ?
N53A C54A 1.351(5) . ?
C54A C55A 1.394(5) . ?
C54A H54A 0.9500 . ?
C55A C56A 1.372(5) . ?
C55A H55A 0.9500 . ?
C56A C57A 1.414(5) . ?
C56A H56A 0.9500 . ?
C57A C63A 1.467(5) . ?
C58A N59A 1.333(4) . ?
C58A C63A 1.440(5) . ?
N59A C60A 1.353(5) . ?
C60A C64A 1.432(5) . ?
C60A C61A 1.439(5) . ?
C61A N62A 1.360(5) . ?
C61A C67A 1.421(5) . ?
N62A C63A 1.325(4) . ?
C64A C65A 1.358(6) . ?
C64A H64A 0.9500 . ?
C65A C66A 1.412(6) . ?
C65A H65A 0.9500 . ?
C66A C67A 1.377(6) . ?
C66A H66A 0.9500 . ?
C67A H67A 0.9500 . ?
Fe1B N3B 1.990(3) . ?
Fe1B N47B 1.994(3) . ?
Fe1B N25B 1.995(3) . ?
Fe1B N31B 1.995(3) . ?
Fe1B N53B 2.001(3) . ?
Fe1B N9B 2.010(3) . ?
C2B N3B 1.369(5) . ?
C2B C7B 1.398(5) . ?
C2B C8B 1.444(5) . ?
N3B C4B 1.342(5) . ?
C4B C5B 1.396(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.381(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.401(5) . ?
C6B H6B 0.9500 . ?
C7B C14B 1.480(5) . ?
C8B N9B 1.356(5) . ?
C8B C13B 1.418(5) . ?
N9B C10B 1.349(5) . ?
C10B C11B 1.396(5) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.381(5) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.419(5) . ?
C12B H12B 0.9500 . ?
C13B C19B 1.468(5) . ?
C14B N15B 1.338(5) . ?
C14B C19B 1.426(5) . ?
N15B C16B 1.348(5) . ?
C16B C20B 1.430(5) . ?
C16B C17B 1.441(5) . ?
C17B N18B 1.357(5) . ?
C17B C23B 1.437(5) . ?
N18B C19B 1.344(5) . ?
C20B C21B 1.371(6) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.430(6) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.362(6) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C24B N25B 1.366(5) . ?
C24B C29B 1.411(5) . ?
C24B C30B 1.449(5) . ?
N25B C26B 1.342(5) . ?
C26B C27B 1.393(6) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.379(6) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.406(5) . ?
C28B H28B 0.9500 . ?
C29B C36B 1.474(5) . ?
C30B N31B 1.368(5) . ?
C30B C35B 1.398(5) . ?
N31B C32B 1.359(5) . ?
C32B C33B 1.394(6) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.375(6) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.401(5) . ?
C34B H34B 0.9500 . ?
C35B C41B 1.464(5) . ?
C36B N37B 1.331(5) . ?
C36B C41B 1.446(5) . ?
N37B C38B 1.367(5) . ?
C38B C42B 1.418(5) . ?
C38B C39B 1.435(5) . ?
C39B N40B 1.357(5) . ?
C39B C45B 1.421(5) . ?
N40B C41B 1.320(5) . ?
C42B C43B 1.376(6) . ?
C42B H42B 0.9500 . ?
C43B C44B 1.415(6) . ?
C43B H43B 0.9500 . ?
C44B C45B 1.362(6) . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
C46B N47B 1.374(5) . ?
C46B C51B 1.400(5) . ?
C46B C52B 1.447(5) . ?
N47B C48B 1.343(5) . ?
C48B C49B 1.395(5) . ?
C48B H48B 0.9500 . ?
C49B C50B 1.373(5) . ?
C49B H49B 0.9500 . ?
C50B C51B 1.403(5) . ?
C50B H50B 0.9500 . ?
C51B C58B 1.471(5) . ?
C52B N53B 1.374(5) . ?
C52B C57B 1.404(5) . ?
N53B C54B 1.340(5) . ?
C54B C55B 1.398(6) . ?
C54B H54B 0.9500 . ?
C55B C56B 1.365(6) . ?
C55B H55B 0.9500 . ?
C56B C57B 1.417(5) . ?
C56B H56B 0.9500 . ?
C57B C63B 1.464(5) . ?
C58B N59B 1.330(5) . ?
C58B C63B 1.446(5) . ?
N59B C60B 1.366(5) . ?
C60B C64B 1.422(6) . ?
C60B C61B 1.430(6) . ?
C61B N62B 1.372(5) . ?
C61B C67B 1.423(5) . ?
N62B C63B 1.335(5) . ?
C64B C65B 1.367(6) . ?
C64B H64B 0.9500 . ?
C65B C66B 1.427(6) . ?
C65B H65B 0.9500 . ?
C66B C67B 1.360(6) . ?
C66B H66B 0.9500 . ?
C67B H67B 0.9500 . ?
Cl68 O70 1.410(4) . ?
Cl68 O72 1.436(4) . ?
Cl68 O69 1.447(3) . ?
Cl68 O71 1.450(3) . ?
Cl7A O77A 1.405(9) . ?
Cl7A O75A 1.419(9) . ?
Cl7A O76A 1.424(9) . ?
Cl7A O74A 1.490(9) . ?
Cl7B O74B 1.387(11) . ?
Cl7B O76B 1.407(12) . ?
Cl7B O77B 1.447(13) . ?
Cl7B O75B 1.550(12) . ?
Cl7C O74C 1.318(11) . ?
Cl7C O77C 1.462(11) . ?
Cl7C O75C 1.475(10) . ?
Cl7C O76C 1.553(12) . ?
Cl78 O82 1.433(3) . ?
Cl78 O81 1.438(4) . ?
Cl78 O79 1.438(3) . ?
Cl78 O80 1.457(4) . ?
Cl83 O85 1.389(4) . ?
Cl83 O86 1.419(4) . ?
Cl83 O84 1.427(3) . ?
Cl83 O87 1.454(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N47A Fe1A N31A 173.18(12) . . ?
N47A Fe1A N25A 92.37(11) . . ?
N31A Fe1A N25A 82.20(12) . . ?
N47A Fe1A N53A 82.09(11) . . ?
N31A Fe1A N53A 93.98(12) . . ?
N25A Fe1A N53A 92.54(12) . . ?
N47A Fe1A N9A 89.50(12) . . ?
N31A Fe1A N9A 95.10(12) . . ?
N25A Fe1A N9A 95.36(12) . . ?
N53A Fe1A N9A 168.69(12) . . ?
N47A Fe1A N3A 91.02(11) . . ?
N31A Fe1A N3A 94.60(12) . . ?
N25A Fe1A N3A 175.75(11) . . ?
N53A Fe1A N3A 90.46(12) . . ?
N9A Fe1A N3A 82.12(12) . . ?
N3A C2A C7A 123.3(3) . . ?
N3A C2A C8A 114.6(3) . . ?
C7A C2A C8A 122.0(3) . . ?
C4A N3A C2A 117.0(3) . . ?
C4A N3A Fe1A 129.6(3) . . ?
C2A N3A Fe1A 113.4(2) . . ?
N3A C4A C5A 122.8(4) . . ?
N3A C4A H4A 118.6 . . ?
C5A C4A H4A 118.6 . . ?
C6A C5A C4A 119.8(3) . . ?
C6A C5A H5A 120.1 . . ?
C4A C5A H5A 120.1 . . ?
C5A C6A C7A 118.8(4) . . ?
C5A C6A H6A 120.6 . . ?
C7A C6A H6A 120.6 . . ?
C2A C7A C6A 118.2(3) . . ?
C2A C7A C14A 118.3(3) . . ?
C6A C7A C14A 123.5(3) . . ?
N9A C8A C13A 123.3(3) . . ?
N9A C8A C2A 115.9(3) . . ?
C13A C8A C2A 120.8(3) . . ?
C10A N9A C8A 117.5(3) . . ?
C10A N9A Fe1A 128.9(3) . . ?
C8A N9A Fe1A 112.6(2) . . ?
N9A C10A C11A 122.7(3) . . ?
N9A C10A H10A 118.6 . . ?
C11A C10A H10A 118.6 . . ?
C12A C11A C10A 119.4(3) . . ?
C12A C11A H11A 120.3 . . ?
C10A C11A H11A 120.3 . . ?
C11A C12A C13A 119.0(4) . . ?
C11A C12A H12A 120.5 . . ?
C13A C12A H12A 120.5 . . ?
C12A C13A C8A 118.1(3) . . ?
C12A C13A C19A 123.0(3) . . ?
C8A C13A C19A 118.9(3) . . ?
N15A C14A C19A 122.1(3) . . ?
N15A C14A C7A 117.9(3) . . ?
C19A C14A C7A 120.0(3) . . ?
C14A N15A C16A 116.6(3) . . ?
N15A C16A C20A 119.7(4) . . ?
N15A C16A C17A 121.0(4) . . ?
C20A C16A C17A 119.2(4) . . ?
N18A C17A C23A 119.6(4) . . ?
N18A C17A C16A 121.7(4) . . ?
C23A C17A C16A 118.7(4) . . ?
C19A N18A C17A 116.9(3) . . ?
N18A C19A C14A 121.7(3) . . ?
N18A C19A C13A 118.5(3) . . ?
C14A C19A C13A 119.9(3) . . ?
C21A C20A C16A 120.0(5) . . ?
C21A C20A H20A 120.0 . . ?
C16A C20A H20A 120.0 . . ?
C20A C21A C22A 121.0(4) . . ?
C20A C21A H21A 119.5 . . ?
C22A C21A H21A 119.5 . . ?
C23A C22A C21A 121.5(4) . . ?
C23A C22A H22A 119.3 . . ?
C21A C22A H22A 119.3 . . ?
C22A C23A C17A 119.5(4) . . ?
C22A C23A H23A 120.3 . . ?
C17A C23A H23A 120.3 . . ?
N25A C24A C29A 123.8(3) . . ?
N25A C24A C30A 114.6(3) . . ?
C29A C24A C30A 121.6(3) . . ?
C26A N25A C24A 116.4(3) . . ?
C26A N25A Fe1A 129.6(2) . . ?
C24A N25A Fe1A 114.0(2) . . ?
N25A C26A C27A 123.0(3) . . ?
N25A C26A H26A 118.5 . . ?
C27A C26A H26A 118.5 . . ?
C28A C27A C26A 120.5(3) . . ?
C28A C27A H27A 119.7 . . ?
C26A C27A H27A 119.7 . . ?
C27A C28A C29A 118.0(3) . . ?
C27A C28A H28A 121.0 . . ?
C29A C28A H28A 121.0 . . ?
C24A C29A C28A 118.2(3) . . ?
C24A C29A C36A 118.7(3) . . ?
C28A C29A C36A 123.0(3) . . ?
N31A C30A C35A 123.6(3) . . ?
N31A C30A C24A 115.3(3) . . ?
C35A C30A C24A 121.1(3) . . ?
C32A N31A C30A 117.0(3) . . ?
C32A N31A Fe1A 129.1(3) . . ?
C30A N31A Fe1A 113.8(2) . . ?
N31A C32A C33A 122.7(4) . . ?
N31A C32A H32A 118.7 . . ?
C33A C32A H32A 118.7 . . ?
C34A C33A C32A 119.8(4) . . ?
C34A C33A H33A 120.1 . . ?
C32A C33A H33A 120.1 . . ?
C33A C34A C35A 118.5(3) . . ?
C33A C34A H34A 120.7 . . ?
C35A C34A H34A 120.7 . . ?
C34A C35A C30A 118.3(3) . . ?
C34A C35A C41A 122.8(3) . . ?
C30A C35A C41A 118.8(3) . . ?
N37A C36A C41A 122.0(3) . . ?
N37A C36A C29A 117.9(3) . . ?
C41A C36A C29A 120.1(3) . . ?
C36A N37A C38A 117.0(3) . . ?
N37A C38A C42A 119.4(4) . . ?
N37A C38A C39A 121.1(3) . . ?
C42A C38A C39A 119.5(3) . . ?
N40A C39A C45A 119.6(4) . . ?
N40A C39A C38A 121.4(3) . . ?
C45A C39A C38A 118.9(3) . . ?
C41A N40A C39A 116.8(3) . . ?
N40A C41A C36A 121.6(3) . . ?
N40A C41A C35A 118.8(3) . . ?
C36A C41A C35A 119.6(3) . . ?
C43A C42A C38A 119.9(4) . . ?
C43A C42A H42A 120.0 . . ?
C38A C42A H42A 120.0 . . ?
C42A C43A C44A 120.5(4) . . ?
C42A C43A H43A 119.7 . . ?
C44A C43A H43A 119.7 . . ?
C45A C44A C43A 121.8(4) . . ?
C45A C44A H44A 119.1 . . ?
C43A C44A H44A 119.1 . . ?
C44A C45A C39A 119.3(4) . . ?
C44A C45A H45A 120.4 . . ?
C39A C45A H45A 120.4 . . ?
N47A C46A C51A 123.7(3) . . ?
N47A C46A C52A 115.4(3) . . ?
C51A C46A C52A 120.9(3) . . ?
C48A N47A C46A 116.7(3) . . ?
C48A N47A Fe1A 129.5(2) . . ?
C46A N47A Fe1A 113.7(2) . . ?
N47A C48A C49A 123.1(3) . . ?
N47A C48A H48A 118.5 . . ?
C49A C48A H48A 118.5 . . ?
C50A C49A C48A 120.0(3) . . ?
C50A C49A H49A 120.0 . . ?
C48A C49A H49A 120.0 . . ?
C49A C50A C51A 118.7(3) . . ?
C49A C50A H50A 120.7 . . ?
C51A C50A H50A 120.7 . . ?
C46A C51A C50A 117.8(3) . . ?
C46A C51A C58A 118.5(3) . . ?
C50A C51A C58A 123.7(3) . . ?
N53A C52A C57A 123.9(3) . . ?
N53A C52A C46A 114.6(3) . . ?
C57A C52A C46A 121.5(3) . . ?
C54A N53A C52A 116.6(3) . . ?
C54A N53A Fe1A 129.2(2) . . ?
C52A N53A Fe1A 113.9(2) . . ?
N53A C54A C55A 122.7(3) . . ?
N53A C54A H54A 118.6 . . ?
C55A C54A H54A 118.6 . . ?
C56A C55A C54A 120.7(3) . . ?
C56A C55A H55A 119.6 . . ?
C54A C55A H55A 119.6 . . ?
C55A C56A C57A 118.0(3) . . ?
C55A C56A H56A 121.0 . . ?
C57A C56A H56A 121.0 . . ?
C52A C57A C56A 118.0(3) . . ?
C52A C57A C63A 119.1(3) . . ?
C56A C57A C63A 122.8(3) . . ?
N59A C58A C63A 121.7(3) . . ?
N59A C58A C51A 117.8(3) . . ?
C63A C58A C51A 120.5(3) . . ?
C58A N59A C60A 117.0(3) . . ?
N59A C60A C64A 119.1(4) . . ?
N59A C60A C61A 121.2(3) . . ?
C64A C60A C61A 119.6(3) . . ?
N62A C61A C67A 119.5(3) . . ?
N62A C61A C60A 121.2(3) . . ?
C67A C61A C60A 119.3(3) . . ?
C63A N62A C61A 116.8(3) . . ?
N62A C63A C58A 122.1(3) . . ?
N62A C63A C57A 118.7(3) . . ?
C58A C63A C57A 119.2(3) . . ?
C65A C64A C60A 118.6(4) . . ?
C65A C64A H64A 120.7 . . ?
C60A C64A H64A 120.7 . . ?
C64A C65A C66A 122.3(4) . . ?
C64A C65A H65A 118.8 . . ?
C66A C65A H65A 118.8 . . ?
C67A C66A C65A 120.8(4) . . ?
C67A C66A H66A 119.6 . . ?
C65A C66A H66A 119.6 . . ?
C66A C67A C61A 119.2(4) . . ?
C66A C67A H67A 120.4 . . ?
C61A C67A H67A 120.4 . . ?
N3B Fe1B N47B 93.38(12) . . ?
N3B Fe1B N25B 169.48(13) . . ?
N47B Fe1B N25B 96.52(13) . . ?
N3B Fe1B N31B 88.46(13) . . ?
N47B Fe1B N31B 174.10(13) . . ?
N25B Fe1B N31B 82.04(13) . . ?
N3B Fe1B N53B 92.30(13) . . ?
N47B Fe1B N53B 81.83(12) . . ?
N25B Fe1B N53B 92.62(13) . . ?
N31B Fe1B N53B 92.50(13) . . ?
N3B Fe1B N9B 81.48(12) . . ?
N47B Fe1B N9B 94.09(12) . . ?
N25B Fe1B N9B 94.24(12) . . ?
N31B Fe1B N9B 91.73(13) . . ?
N53B Fe1B N9B 172.38(12) . . ?
N3B C2B C7B 123.5(3) . . ?
N3B C2B C8B 114.8(3) . . ?
C7B C2B C8B 121.7(3) . . ?
C4B N3B C2B 117.0(3) . . ?
C4B N3B Fe1B 128.6(3) . . ?
C2B N3B Fe1B 112.6(2) . . ?
N3B C4B C5B 122.6(4) . . ?
N3B C4B H4B 118.7 . . ?
C5B C4B H4B 118.7 . . ?
C6B C5B C4B 120.3(4) . . ?
C6B C5B H5B 119.9 . . ?
C4B C5B H5B 119.9 . . ?
C5B C6B C7B 118.3(4) . . ?
C5B C6B H6B 120.9 . . ?
C7B C6B H6B 120.9 . . ?
C2B C7B C6B 118.1(4) . . ?
C2B C7B C14B 118.9(3) . . ?
C6B C7B C14B 123.0(4) . . ?
N9B C8B C13B 123.9(3) . . ?
N9B C8B C2B 115.8(3) . . ?
C13B C8B C2B 120.3(3) . . ?
C10B N9B C8B 117.1(3) . . ?
C10B N9B Fe1B 130.5(3) . . ?
C8B N9B Fe1B 112.4(2) . . ?
N9B C10B C11B 122.7(4) . . ?
N9B C10B H10B 118.6 . . ?
C11B C10B H10B 118.6 . . ?
C12B C11B C10B 120.6(3) . . ?
C12B C11B H11B 119.7 . . ?
C10B C11B H11B 119.7 . . ?
C11B C12B C13B 118.2(4) . . ?
C11B C12B H12B 120.9 . . ?
C13B C12B H12B 120.9 . . ?
C8B C13B C12B 117.3(3) . . ?
C8B C13B C19B 118.8(3) . . ?
C12B C13B C19B 123.9(3) . . ?
N15B C14B C19B 122.6(3) . . ?
N15B C14B C7B 117.9(3) . . ?
C19B C14B C7B 119.6(3) . . ?
C14B N15B C16B 116.9(3) . . ?
N15B C16B C20B 120.0(4) . . ?
N15B C16B C17B 121.2(4) . . ?
C20B C16B C17B 118.8(4) . . ?
N18B C17B C23B 119.3(3) . . ?
N18B C17B C16B 121.1(3) . . ?
C23B C17B C16B 119.6(4) . . ?
C19B N18B C17B 117.2(3) . . ?
N18B C19B C14B 121.0(3) . . ?
N18B C19B C13B 118.6(3) . . ?
C14B C19B C13B 120.3(3) . . ?
C21B C20B C16B 120.0(4) . . ?
C21B C20B H20B 120.0 . . ?
C16B C20B H20B 120.0 . . ?
C20B C21B C22B 120.8(4) . . ?
C20B C21B H21B 119.6 . . ?
C22B C21B H21B 119.6 . . ?
C23B C22B C21B 121.3(4) . . ?
C23B C22B H22B 119.3 . . ?
C21B C22B H22B 119.3 . . ?
C22B C23B C17B 119.4(4) . . ?
C22B C23B H23B 120.3 . . ?
C17B C23B H23B 120.3 . . ?
N25B C24B C29B 123.7(3) . . ?
N25B C24B C30B 115.4(3) . . ?
C29B C24B C30B 120.9(3) . . ?
C26B N25B C24B 116.8(3) . . ?
C26B N25B Fe1B 129.5(3) . . ?
C24B N25B Fe1B 113.6(2) . . ?
N25B C26B C27B 123.1(4) . . ?
N25B C26B H26B 118.4 . . ?
C27B C26B H26B 118.4 . . ?
C28B C27B C26B 120.1(4) . . ?
C28B C27B H27B 119.9 . . ?
C26B C27B H27B 119.9 . . ?
C27B C28B C29B 118.8(3) . . ?
C27B C28B H28B 120.6 . . ?
C29B C28B H28B 120.6 . . ?
C28B C29B C24B 117.4(3) . . ?
C28B C29B C36B 123.5(3) . . ?
C24B C29B C36B 119.1(3) . . ?
N31B C30B C35B 123.5(3) . . ?
N31B C30B C24B 115.3(3) . . ?
C35B C30B C24B 121.1(3) . . ?
C32B N31B C30B 116.4(3) . . ?
C32B N31B Fe1B 129.9(3) . . ?
C30B N31B Fe1B 113.6(2) . . ?
N31B C32B C33B 123.1(4) . . ?
N31B C32B H32B 118.5 . . ?
C33B C32B H32B 118.5 . . ?
C34B C33B C32B 119.8(4) . . ?
C34B C33B H33B 120.1 . . ?
C32B C33B H33B 120.1 . . ?
C33B C34B C35B 118.9(4) . . ?
C33B C34B H34B 120.5 . . ?
C35B C34B H34B 120.5 . . ?
C30B C35B C34B 118.2(3) . . ?
C30B C35B C41B 119.8(3) . . ?
C34B C35B C41B 122.0(3) . . ?
N37B C36B C41B 121.3(3) . . ?
N37B C36B C29B 119.2(3) . . ?
C41B C36B C29B 119.5(3) . . ?
C36B N37B C38B 116.9(3) . . ?
N37B C38B C42B 119.7(3) . . ?
N37B C38B C39B 121.1(3) . . ?
C42B C38B C39B 119.2(4) . . ?
N40B C39B C45B 119.5(4) . . ?
N40B C39B C38B 121.2(3) . . ?
C45B C39B C38B 119.3(3) . . ?
C41B N40B C39B 116.9(3) . . ?
N40B C41B C36B 122.4(3) . . ?
N40B C41B C35B 118.0(3) . . ?
C36B C41B C35B 119.6(3) . . ?
C43B C42B C38B 119.4(4) . . ?
C43B C42B H42B 120.3 . . ?
C38B C42B H42B 120.3 . . ?
C42B C43B C44B 121.4(4) . . ?
C42B C43B H43B 119.3 . . ?
C44B C43B H43B 119.3 . . ?
C45B C44B C43B 120.4(4) . . ?
C45B C44B H44B 119.8 . . ?
C43B C44B H44B 119.8 . . ?
C44B C45B C39B 120.3(4) . . ?
C44B C45B H45B 119.9 . . ?
C39B C45B H45B 119.9 . . ?
N47B C46B C51B 123.2(3) . . ?
N47B C46B C52B 115.1(3) . . ?
C51B C46B C52B 121.7(3) . . ?
C48B N47B C46B 116.9(3) . . ?
C48B N47B Fe1B 129.9(3) . . ?
C46B N47B Fe1B 113.0(2) . . ?
N47B C48B C49B 122.8(4) . . ?
N47B C48B H48B 118.6 . . ?
C49B C48B H48B 118.6 . . ?
C50B C49B C48B 120.2(4) . . ?
C50B C49B H49B 119.9 . . ?
C48B C49B H49B 119.9 . . ?
C49B C50B C51B 118.6(4) . . ?
C49B C50B H50B 120.7 . . ?
C51B C50B H50B 120.7 . . ?
C46B C51B C50B 118.1(3) . . ?
C46B C51B C58B 118.9(3) . . ?
C50B C51B C58B 123.0(3) . . ?
N53B C52B C57B 124.1(3) . . ?
N53B C52B C46B 115.3(3) . . ?
C57B C52B C46B 120.6(3) . . ?
C54B N53B C52B 116.7(3) . . ?
C54B N53B Fe1B 130.3(3) . . ?
C52B N53B Fe1B 112.7(2) . . ?
N53B C54B C55B 122.6(4) . . ?
N53B C54B H54B 118.7 . . ?
C55B C54B H54B 118.7 . . ?
C56B C55B C54B 120.9(4) . . ?
C56B C55B H55B 119.6 . . ?
C54B C55B H55B 119.6 . . ?
C55B C56B C57B 118.7(4) . . ?
C55B C56B H56B 120.7 . . ?
C57B C56B H56B 120.7 . . ?
C52B C57B C56B 117.0(4) . . ?
C52B C57B C63B 119.2(3) . . ?
C56B C57B C63B 123.8(3) . . ?
N59B C58B C63B 122.3(3) . . ?
N59B C58B C51B 118.5(3) . . ?
C63B C58B C51B 119.2(3) . . ?
C58B N59B C60B 116.9(3) . . ?
N59B C60B C64B 119.6(3) . . ?
N59B C60B C61B 120.9(3) . . ?
C64B C60B C61B 119.5(3) . . ?
N62B C61B C67B 119.1(4) . . ?
N62B C61B C60B 121.7(3) . . ?
C67B C61B C60B 119.3(4) . . ?
C63B N62B C61B 116.6(3) . . ?
N62B C63B C58B 121.4(3) . . ?
N62B C63B C57B 118.5(3) . . ?
C58B C63B C57B 120.1(3) . . ?
C65B C64B C60B 119.8(4) . . ?
C65B C64B H64B 120.1 . . ?
C60B C64B H64B 120.1 . . ?
C64B C65B C66B 120.5(4) . . ?
C64B C65B H65B 119.8 . . ?
C66B C65B H65B 119.8 . . ?
C67B C66B C65B 121.2(4) . . ?
C67B C66B H66B 119.4 . . ?
C65B C66B H66B 119.4 . . ?
C66B C67B C61B 119.7(4) . . ?
C66B C67B H67B 120.1 . . ?
C61B C67B H67B 120.1 . . ?
O70 Cl68 O72 108.9(3) . . ?
O70 Cl68 O69 111.1(2) . . ?
O72 Cl68 O69 108.8(2) . . ?
O70 Cl68 O71 109.2(2) . . ?
O72 Cl68 O71 108.4(2) . . ?
O69 Cl68 O71 110.45(18) . . ?
O77A Cl7A O75A 113.3(7) . . ?
O77A Cl7A O76A 102.9(6) . . ?
O75A Cl7A O76A 113.1(6) . . ?
O77A Cl7A O74A 107.3(6) . . ?
O75A Cl7A O74A 109.1(6) . . ?
O76A Cl7A O74A 110.8(5) . . ?
O74B Cl7B O76B 121.4(9) . . ?
O74B Cl7B O77B 110.3(9) . . ?
O76B Cl7B O77B 115.8(11) . . ?
O74B Cl7B O75B 104.4(9) . . ?
O76B Cl7B O75B 100.7(9) . . ?
O77B Cl7B O75B 100.5(9) . . ?
O74C Cl7C O77C 117.2(9) . . ?
O74C Cl7C O75C 120.7(8) . . ?
O77C Cl7C O75C 101.3(8) . . ?
O74C Cl7C O76C 108.6(9) . . ?
O77C Cl7C O76C 101.8(9) . . ?
O75C Cl7C O76C 105.0(8) . . ?
O82 Cl78 O81 110.4(3) . . ?
O82 Cl78 O79 108.5(2) . . ?
O81 Cl78 O79 110.4(2) . . ?
O82 Cl78 O80 109.0(2) . . ?
O81 Cl78 O80 109.3(2) . . ?
O79 Cl78 O80 109.1(2) . . ?
O85 Cl83 O86 111.6(4) . . ?
O85 Cl83 O84 110.0(3) . . ?
O86 Cl83 O84 107.4(3) . . ?
O85 Cl83 O87 110.1(3) . . ?
O86 Cl83 O87 108.2(2) . . ?
O84 Cl83 O87 109.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.21
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.087
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/1,2-dichloroethane'
####################################################################### 
# 
# 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_rk119f
_database_code_depnum_ccdc_archive 'CCDC 1430811'
_audit_update_record             
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Tris[dipyrido[3,2-a:23-c]benzo[i]phenazine]iron(II) di-tetrafluoroborate hydrate tris-methanol solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H36 Fe N12, 2(B F4), H2 O, 3(C H4 O)'
_chemical_formula_sum            'C69 H50 B2 F8 Fe N12 O4'
_chemical_formula_weight         1340.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.7973(2)
_cell_length_b                   23.8139(8)
_cell_length_c                   27.5891(6)
_cell_angle_alpha                95.037(2)
_cell_angle_beta                 98.452(2)
_cell_angle_gamma                93.612(2)
_cell_volume                     6323.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11572
_cell_measurement_theta_min      3.57
_cell_measurement_theta_max      72.86

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2752
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            56368
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         74.00
_reflns_number_total             23938
_reflns_number_gt                15545
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The asymmetric unit contains two formula units of the compound (Z' = 2). 
 That is, two complex dications, four BF₄⁻ anions and a number of
 part occupied, disordered solvent molecules that were modelled as a 
 mixture of methanol and water.

 The solvent occupied two different types of channel, which both run
 parallel to the a axis. Both channels are rectangular in shape, with 
 approximate dimensions 8.3 x 8.8 Å and 4.2 x 4.8 Å. The lattice
 contains an equal number of both types of channel. A SQUEEZE analysis 
 from a model containing only the cations and anions showed 1337 Å³ 
 of void space, which is 21 % of the unit cell volume. The voids were 
 occupied by 249 unresolved electrons per unit cell, or 62.25 per formula 
 unit. That is close to a solvent complement of 3x methanol 
 (3x 18 electrons) and 1x water (10 electrons), which would equate to 64 
 electrons in total. That formula was used for the density and F(000) 
 calculations in the cif file. For comparison, the final refinement model 
 contains solvent sites summing to 1.5 equiv of methanol and 0.85 equiv 
 water, per formula unit.

 The original dataset, rather than the SQUEEZEd one, was used in the final
 refinement cycles. The partial methanol C---O bonds were restrained to 
 1.43(2) Å, but no other restraints were applied. All wholly occupied 
 non-H atoms were refined anisotropically, while H atoms were placed in 
 calculated positions and refined using a riding model. The partial water 
 H atoms were not located in Fourier map, and are not included in the 
 model. The slightly high shift/su values from the final least squares
 cycles reflect the H atoms on the partial methanol molecules, which are
 free to precess about the C---O bond under the AFIX procedure. The same
 issue explains some short intermolecular H...H contacts between the 
 complex and partial solvent molecules.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1651P)²+0.9069P] 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         23938
_refine_ls_number_parameters     1700
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0851
_refine_ls_wR_factor_ref         0.2698
_refine_ls_wR_factor_gt          0.2313
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.014

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.24891(7) 0.07202(3) 0.23279(3) 0.03489(17) Uani 1 1 d . A 1
C2A C 0.1560(5) 0.1806(2) 0.22345(16) 0.0370(9) Uani 1 1 d . A 1
N3A N 0.1152(4) 0.13035(17) 0.23792(13) 0.0377(8) Uani 1 1 d . A 1
C4A C -0.0080(5) 0.1260(2) 0.25284(17) 0.0399(10) Uani 1 1 d . A 1
H4A H -0.0398 0.0907 0.2624 0.048 Uiso 1 1 calc R A 1
C5A C -0.0923(5) 0.1708(2) 0.25500(18) 0.0435(11) Uani 1 1 d . A 1
H5A H -0.1779 0.1663 0.2671 0.052 Uiso 1 1 calc R A 1
C6A C -0.0514(5) 0.2214(2) 0.23967(18) 0.0440(11) Uani 1 1 d . A 1
H6A H -0.1080 0.2523 0.2405 0.053 Uiso 1 1 calc R A 1
C7A C 0.0771(5) 0.2265(2) 0.22265(17) 0.0404(10) Uani 1 1 d . A 1
C8A C 0.2920(5) 0.1838(2) 0.20870(16) 0.0366(9) Uani 1 1 d . A 1
N9A N 0.3598(4) 0.13548(17) 0.21219(14) 0.0385(8) Uani 1 1 d . A 1
C10A C 0.4871(5) 0.1365(2) 0.20000(18) 0.0426(10) Uani 1 1 d . A 1
H10A H 0.5362 0.1035 0.2021 0.051 Uiso 1 1 calc R A 1
C11A C 0.5505(5) 0.1842(2) 0.18432(19) 0.0485(12) Uani 1 1 d . A 1
H11A H 0.6414 0.1833 0.1762 0.058 Uiso 1 1 calc R A 1
C12A C 0.4817(5) 0.2328(2) 0.18049(19) 0.0464(11) Uani 1 1 d . A 1
H12A H 0.5234 0.2655 0.1695 0.056 Uiso 1 1 calc R A 1
C13A C 0.3471(5) 0.2326(2) 0.19347(17) 0.0413(10) Uani 1 1 d . A 1
C14A C 0.1282(5) 0.2779(2) 0.20369(17) 0.0423(10) Uani 1 1 d . A 1
N15A N 0.0444(5) 0.31950(18) 0.19927(16) 0.0478(10) Uani 1 1 d . A 1
C16A C 0.0946(6) 0.3667(2) 0.18138(18) 0.0478(12) Uani 1 1 d . A 1
C17A C 0.2322(6) 0.3725(2) 0.16992(19) 0.0490(12) Uani 1 1 d . A 1
N18A N 0.3166(5) 0.32889(18) 0.17492(15) 0.0469(10) Uani 1 1 d . A 1
C19A C 0.2662(5) 0.2824(2) 0.19049(17) 0.0413(10) Uani 1 1 d . A 1
C20A C 0.0071(7) 0.4108(2) 0.1746(2) 0.0581(14) Uani 1 1 d . A 1
H20A H -0.0841 0.4067 0.1823 0.070 Uiso 1 1 calc R A 1
C21A C 0.0528(7) 0.4604(3) 0.1566(2) 0.0605(15) Uani 1 1 d . A 1
C22A C 0.1920(7) 0.4668(2) 0.1458(2) 0.0576(14) Uani 1 1 d . A 1
C23A C 0.2804(6) 0.4224(2) 0.1528(2) 0.0540(13) Uani 1 1 d . A 1
H23A H 0.3724 0.4266 0.1459 0.065 Uiso 1 1 calc R A 1
C24A C -0.0357(8) 0.5049(3) 0.1484(2) 0.0694(17) Uani 1 1 d . A 1
H24A H -0.1283 0.5008 0.1548 0.083 Uiso 1 1 calc RD A 1
C25A C 0.0106(9) 0.5528(3) 0.1315(3) 0.077(2) Uani 1 1 d . A 1
H25A H -0.0494 0.5822 0.1261 0.092 Uiso 1 1 calc R A 1
C26A C 0.1475(9) 0.5596(3) 0.1219(3) 0.0732(19) Uani 1 1 d . A 1
H26A H 0.1790 0.5936 0.1101 0.088 Uiso 1 1 calc R A 1
C27A C 0.2342(7) 0.5186(3) 0.1291(2) 0.0689(17) Uani 1 1 d . A 1
H27A H 0.3265 0.5246 0.1227 0.083 Uiso 1 1 calc RD A 1
C28A C 0.3567(4) -0.0147(2) 0.17648(16) 0.0351(9) Uani 1 1 d . A 1
N29A N 0.3799(4) 0.01283(17) 0.22276(14) 0.0391(8) Uani 1 1 d . A 1
C30A C 0.4785(5) -0.0057(2) 0.25577(18) 0.0434(11) Uani 1 1 d . A 1
H30A H 0.4960 0.0128 0.2883 0.052 Uiso 1 1 calc R A 1
C31A C 0.5550(5) -0.0503(2) 0.2441(2) 0.0466(12) Uani 1 1 d . A 1
H31A H 0.6223 -0.0624 0.2686 0.056 Uiso 1 1 calc R A 1
C32A C 0.5337(5) -0.0772(2) 0.1971(2) 0.0438(11) Uani 1 1 d . A 1
H32A H 0.5876 -0.1073 0.1885 0.053 Uiso 1 1 calc R A 1
C33A C 0.4304(5) -0.0592(2) 0.16186(18) 0.0394(10) Uani 1 1 d . A 1
C34A C 0.2471(4) 0.00581(19) 0.14279(16) 0.0339(9) Uani 1 1 d . A 1
N35A N 0.1788(4) 0.04812(17) 0.16246(13) 0.0358(8) Uani 1 1 d . A 1
C36A C 0.0788(4) 0.0691(2) 0.13205(17) 0.0384(10) Uani 1 1 d . A 1
H36A H 0.0302 0.0990 0.1448 0.046 Uiso 1 1 calc R A 1
C37A C 0.0439(5) 0.0488(2) 0.08280(17) 0.0415(10) Uani 1 1 d . A 1
H37A H -0.0259 0.0654 0.0623 0.050 Uiso 1 1 calc R A 1
C38A C 0.1097(5) 0.0052(2) 0.06374(17) 0.0412(10) Uani 1 1 d . A 1
H38A H 0.0840 -0.0098 0.0304 0.049 Uiso 1 1 calc R A 1
C39A C 0.2165(4) -0.0172(2) 0.09440(16) 0.0369(9) Uani 1 1 d . A 1
C40A C 0.3994(5) -0.0852(2) 0.11148(18) 0.0412(10) Uani 1 1 d . A 1
N41A N 0.4687(4) -0.12813(18) 0.09791(17) 0.0473(10) Uani 1 1 d . A 1
C42A C 0.4326(6) -0.1532(2) 0.0509(2) 0.0511(12) Uani 1 1 d . A 1
C43A C 0.3196(6) -0.1339(2) 0.0185(2) 0.0520(13) Uani 1 1 d . A 1
N44A N 0.2522(4) -0.08860(18) 0.03208(15) 0.0446(9) Uani 1 1 d . A 1
C45A C 0.2905(5) -0.0646(2) 0.07765(17) 0.0399(10) Uani 1 1 d . A 1
C46A C 0.5002(7) -0.1995(2) 0.0359(2) 0.0631(16) Uani 1 1 d . A 1
H46A H 0.5763 -0.2111 0.0572 0.076 Uiso 1 1 calc R A 1
C47A C 0.4570(8) -0.2290(3) -0.0102(3) 0.072(2) Uani 1 1 d . A 1
C48A C 0.3374(8) -0.2122(3) -0.0425(3) 0.0691(18) Uani 1 1 d . A 1
C49A C 0.2768(7) -0.1638(3) -0.0284(2) 0.0584(14) Uani 1 1 d . A 1
H49A H 0.2050 -0.1505 -0.0505 0.070 Uiso 1 1 calc R A 1
C50A C 0.5166(10) -0.2787(3) -0.0267(3) 0.085(2) Uani 1 1 d . A 1
H50A H 0.5951 -0.2905 -0.0068 0.102 Uiso 1 1 calc R A 1
C51A C 0.4666(12) -0.3096(3) -0.0692(3) 0.095(3) Uani 1 1 d . A 1
H51A H 0.5120 -0.3417 -0.0795 0.114 Uiso 1 1 calc R A 1
C52A C 0.3456(12) -0.2948(3) -0.0990(3) 0.099(3) Uani 1 1 d . A 1
H52A H 0.3060 -0.3189 -0.1275 0.118 Uiso 1 1 calc R A 1
C53A C 0.2854(10) -0.2460(3) -0.0871(3) 0.083(2) Uani 1 1 d . A 1
H53A H 0.2092 -0.2349 -0.1086 0.099 Uiso 1 1 calc R A 1
C54A C 0.2770(5) 0.05214(19) 0.33218(17) 0.0368(9) Uani 1 1 d . A 1
N55A N 0.3310(4) 0.08655(17) 0.30269(14) 0.0389(8) Uani 1 1 d . A 1
C56A C 0.4399(5) 0.1228(2) 0.32288(18) 0.0423(10) Uani 1 1 d . A 1
H56A H 0.4781 0.1481 0.3028 0.051 Uiso 1 1 calc R A 1
C57A C 0.4977(5) 0.1243(2) 0.37189(19) 0.0484(12) Uani 1 1 d . A 1
H57A H 0.5764 0.1495 0.3847 0.058 Uiso 1 1 calc R A 1
C58A C 0.4411(5) 0.0893(2) 0.40229(18) 0.0469(11) Uani 1 1 d . A 1
H58A H 0.4796 0.0902 0.4360 0.056 Uiso 1 1 calc R A 1
C59A C 0.3249(5) 0.0522(2) 0.38213(17) 0.0415(10) Uani 1 1 d . A 1
C60A C 0.1619(4) 0.0133(2) 0.30824(16) 0.0363(9) Uani 1 1 d . A 1
N61A N 0.1287(4) 0.01600(16) 0.25908(13) 0.0349(8) Uani 1 1 d . A 1
C62A C 0.0181(4) -0.0177(2) 0.23525(17) 0.0380(10) Uani 1 1 d . A 1
H62A H -0.0079 -0.0164 0.2008 0.046 Uiso 1 1 calc R A 1
C63A C -0.0580(5) -0.0539(2) 0.25960(18) 0.0396(10) Uani 1 1 d . A 1
H63A H -0.1351 -0.0768 0.2417 0.048 Uiso 1 1 calc R A 1
C64A C -0.0234(5) -0.0572(2) 0.30910(18) 0.0418(10) Uani 1 1 d . A 1
H64A H -0.0758 -0.0818 0.3259 0.050 Uiso 1 1 calc R A 1
C65A C 0.0914(5) -0.0231(2) 0.33440(17) 0.0381(10) Uani 1 1 d . A 1
C66A C 0.2544(5) 0.0150(2) 0.41139(17) 0.0414(10) Uani 1 1 d . A 1
N67A N 0.2982(4) 0.01817(19) 0.45885(15) 0.0457(9) Uani 1 1 d . A 1
C68A C 0.2259(5) -0.0149(2) 0.48555(18) 0.0445(11) Uani 1 1 d . A 1
C69A C 0.1075(5) -0.0509(2) 0.46299(18) 0.0429(10) Uani 1 1 d . A 1
N70A N 0.0651(4) -0.05397(18) 0.41315(14) 0.0433(9) Uani 1 1 d . A 1
C71A C 0.1363(5) -0.0218(2) 0.38842(17) 0.0421(10) Uani 1 1 d . A 1
C72A C 0.2662(5) -0.0114(2) 0.53659(18) 0.0453(11) Uani 1 1 d . A 1
H72A H 0.3447 0.0127 0.5516 0.054 Uiso 1 1 calc R A 1
C73A C 0.1920(5) -0.0431(2) 0.56554(19) 0.0446(11) Uani 1 1 d . A 1
C74A C 0.0722(5) -0.0793(2) 0.54246(18) 0.0445(11) Uani 1 1 d . A 1
C75A C 0.0329(6) -0.0827(2) 0.49129(18) 0.0470(11) Uani 1 1 d . A 1
H75A H -0.0452 -0.1069 0.4760 0.056 Uiso 1 1 calc R A 1
C76A C 0.2300(5) -0.0387(2) 0.61786(18) 0.0455(11) Uani 1 1 d . A 1
H76A H 0.3064 -0.0137 0.6332 0.055 Uiso 1 1 calc R A 1
C77A C 0.1581(6) -0.0700(2) 0.64579(19) 0.0484(12) Uani 1 1 d . A 1
H77A H 0.1855 -0.0674 0.6804 0.058 Uiso 1 1 calc R A 1
C78A C 0.0414(6) -0.1067(2) 0.6231(2) 0.0537(13) Uani 1 1 d . A 1
H78A H -0.0083 -0.1286 0.6429 0.064 Uiso 1 1 calc R A 1
C79A C -0.0001(6) -0.1110(2) 0.5734(2) 0.0533(13) Uani 1 1 d . A 1
H79A H -0.0786 -0.1356 0.5592 0.064 Uiso 1 1 calc R A 1
Fe1B Fe 0.44098(7) 0.69912(3) 0.23109(3) 0.03716(18) Uani 1 1 d . B 1
C2B C 0.2854(4) 0.77744(19) 0.18371(16) 0.0358(9) Uani 1 1 d . B 1
N3B N 0.3530(4) 0.77043(16) 0.22930(14) 0.0362(8) Uani 1 1 d . B 1
C4B C 0.3457(5) 0.8096(2) 0.26591(17) 0.0402(10) Uani 1 1 d . B 1
H4B H 0.3946 0.8056 0.2976 0.048 Uiso 1 1 calc R B 1
C5B C 0.2689(5) 0.8564(2) 0.25960(18) 0.0418(10) Uani 1 1 d . B 1
H5B H 0.2671 0.8840 0.2865 0.050 Uiso 1 1 calc R B 1
C6B C 0.1957(5) 0.8625(2) 0.21403(18) 0.0405(10) Uani 1 1 d . B 1
H6B H 0.1419 0.8940 0.2092 0.049 Uiso 1 1 calc R B 1
C7B C 0.2018(4) 0.82150(19) 0.17487(16) 0.0358(9) Uani 1 1 d . B 1
C8B C 0.3048(4) 0.73616(19) 0.14427(16) 0.0346(9) Uani 1 1 d . B 1
N9B N 0.3939(4) 0.69661(16) 0.15839(14) 0.0371(8) Uani 1 1 d . B 1
C10B C 0.4270(5) 0.6603(2) 0.12297(18) 0.0401(10) Uani 1 1 d . B 1
H10B H 0.4908 0.6331 0.1318 0.048 Uiso 1 1 calc R B 1
C11B C 0.3715(5) 0.6610(2) 0.07374(19) 0.0451(11) Uani 1 1 d . B 1
H11B H 0.3993 0.6352 0.0495 0.054 Uiso 1 1 calc R B 1
C12B C 0.2756(5) 0.6992(2) 0.05997(18) 0.0424(10) Uani 1 1 d . B 1
H12B H 0.2340 0.6989 0.0266 0.051 Uiso 1 1 calc R B 1
C13B C 0.2412(4) 0.73830(19) 0.09608(16) 0.0345(9) Uani 1 1 d . B 1
C14B C 0.1221(4) 0.82268(19) 0.12547(16) 0.0342(9) Uani 1 1 d . B 1
N15B N 0.0343(4) 0.86141(16) 0.11981(14) 0.0378(8) Uani 1 1 d . B 1
C16B C -0.0447(4) 0.8600(2) 0.07429(17) 0.0374(9) Uani 1 1 d . B 1
C17B C -0.0284(4) 0.8182(2) 0.03568(17) 0.0376(10) Uani 1 1 d . B 1
N18B N 0.0656(4) 0.77862(17) 0.04217(14) 0.0387(8) Uani 1 1 d . B 1
C19B C 0.1393(4) 0.78043(19) 0.08660(17) 0.0358(9) Uani 1 1 d . B 1
C20B C -0.1424(4) 0.9001(2) 0.06695(17) 0.0377(9) Uani 1 1 d . B 1
H20B H -0.1504 0.9283 0.0927 0.045 Uiso 1 1 calc R B 1
C21B C -0.2278(5) 0.8982(2) 0.02175(17) 0.0396(10) Uani 1 1 d . B 1
C22B C -0.2145(5) 0.8564(2) -0.01706(18) 0.0419(10) Uani 1 1 d . B 1
C23B C -0.1143(5) 0.8176(2) -0.00995(18) 0.0428(10) Uani 1 1 d . B 1
H23B H -0.1041 0.7904 -0.0362 0.051 Uiso 1 1 calc R B 1
C24B C -0.3307(5) 0.9382(2) 0.01402(18) 0.0449(11) Uani 1 1 d . B 1
H24B H -0.3387 0.9670 0.0393 0.054 Uiso 1 1 calc R B 1
C25B C -0.4162(5) 0.9347(2) -0.02969(19) 0.0472(12) Uani 1 1 d . B 1
H25B H -0.4847 0.9610 -0.0346 0.057 Uiso 1 1 calc R B 1
C26B C -0.4053(5) 0.8927(3) -0.06782(19) 0.0512(13) Uani 1 1 d . B 1
H26B H -0.4673 0.8907 -0.0979 0.061 Uiso 1 1 calc R B 1
C27B C -0.3080(5) 0.8553(2) -0.06219(18) 0.0477(12) Uani 1 1 d . B 1
H27B H -0.3013 0.8278 -0.0886 0.057 Uiso 1 1 calc R B 1
C28B C 0.4188(4) 0.58384(19) 0.24341(16) 0.0359(9) Uani 1 1 d . B 1
N29B N 0.5101(4) 0.62274(17) 0.22996(14) 0.0402(9) Uani 1 1 d . B 1
C30B C 0.6333(5) 0.6061(2) 0.22208(19) 0.0427(10) Uani 1 1 d . B 1
H30B H 0.6986 0.6326 0.2127 0.051 Uiso 1 1 calc R B 1
C31B C 0.6684(5) 0.5512(2) 0.2273(2) 0.0481(12) Uani 1 1 d . B 1
H31B H 0.7555 0.5404 0.2201 0.058 Uiso 1 1 calc R B 1
C32B C 0.5784(5) 0.5121(2) 0.24270(19) 0.0452(11) Uani 1 1 d . B 1
H32B H 0.6038 0.4748 0.2473 0.054 Uiso 1 1 calc R B 1
C33B C 0.4491(5) 0.5285(2) 0.25142(18) 0.0411(10) Uani 1 1 d . B 1
C34B C 0.2835(4) 0.6023(2) 0.24723(18) 0.0393(10) Uani 1 1 d . B 1
N35B N 0.2644(4) 0.65624(17) 0.23621(15) 0.0395(8) Uani 1 1 d . B 1
C36B C 0.1388(5) 0.6745(2) 0.2377(2) 0.0462(11) Uani 1 1 d . B 1
H36B H 0.1220 0.7112 0.2285 0.055 Uiso 1 1 calc R B 1
C37B C 0.0315(5) 0.6422(2) 0.2521(2) 0.0520(13) Uani 1 1 d . B 1
H37B H -0.0558 0.6571 0.2532 0.062 Uiso 1 1 calc R B 1
C38B C 0.0523(5) 0.5886(2) 0.2648(2) 0.0516(13) Uani 1 1 d . B 1
H3B8 H -0.0198 0.5662 0.2751 0.062 Uiso 1 1 calc R B 1
C39B C 0.1814(5) 0.5674(2) 0.26229(19) 0.0439(11) Uani 1 1 d . B 1
C40B C 0.3469(5) 0.4914(2) 0.26944(18) 0.0416(10) Uani 1 1 d . B 1
N41B N 0.3813(4) 0.44081(17) 0.28076(16) 0.0447(9) Uani 1 1 d . B 1
C42B C 0.2850(5) 0.4077(2) 0.29900(18) 0.0449(11) Uani 1 1 d . B 1
C43B C 0.1528(6) 0.4277(2) 0.3050(2) 0.0515(12) Uani 1 1 d . B 1
N44B N 0.1187(4) 0.47981(19) 0.29216(18) 0.0503(10) Uani 1 1 d . B 1
C45B C 0.2141(5) 0.5108(2) 0.27531(18) 0.0438(11) Uani 1 1 d . B 1
C46B C 0.3172(5) 0.3547(2) 0.31246(19) 0.0492(12) Uani 1 1 d . B 1
H46B H 0.4039 0.3412 0.3077 0.059 Uiso 1 1 calc R B 1
C47B C 0.2229(5) 0.3211(2) 0.33289(19) 0.0486(12) Uani 1 1 d . B 1
C48B C 0.0919(6) 0.3409(2) 0.3396(2) 0.0527(13) Uani 1 1 d . B 1
C49B C 0.0575(6) 0.3939(2) 0.3242(2) 0.0562(13) Uani 1 1 d . B 1
H49B H -0.0314 0.4065 0.3270 0.067 Uiso 1 1 calc R B 1
C50B C 0.2542(6) 0.2673(2) 0.3488(2) 0.0537(13) Uani 1 1 d . B 1
H50B H 0.3398 0.2528 0.3438 0.064 Uiso 1 1 calc R B 1
C51B C 0.1648(6) 0.2364(3) 0.3707(2) 0.0598(15) Uani 1 1 d . B 1
H51B H 0.1897 0.2014 0.3820 0.072 Uiso 1 1 calc R B 1
C52B C 0.0352(6) 0.2558(3) 0.3769(2) 0.0625(15) Uani 1 1 d . B 1
H52B H -0.0275 0.2334 0.3918 0.075 Uiso 1 1 calc R B 1
C53B C -0.0010(7) 0.3064(3) 0.3618(2) 0.0617(15) Uani 1 1 d . B 1
H53B H -0.0891 0.3188 0.3661 0.074 Uiso 1 1 calc R B 1
C54B C 0.6984(5) 0.7446(2) 0.28236(17) 0.0404(10) Uani 1 1 d . B 1
N55B N 0.6267(4) 0.73917(16) 0.23590(14) 0.0363(8) Uani 1 1 d . B 1
C56B C 0.6849(5) 0.7618(2) 0.20071(18) 0.0403(10) Uani 1 1 d . B 1
H56B H 0.6346 0.7591 0.1683 0.048 Uiso 1 1 calc R B 1
C57B C 0.8183(5) 0.7894(2) 0.21004(18) 0.0449(11) Uani 1 1 d . B 1
H57B H 0.8571 0.8055 0.1844 0.054 Uiso 1 1 calc R B 1
C58B C 0.8918(5) 0.7928(2) 0.25642(18) 0.0417(10) Uani 1 1 d . B 1
H58B H 0.9830 0.8106 0.2630 0.050 Uiso 1 1 calc R B 1
C59B C 0.8324(5) 0.7700(2) 0.29402(18) 0.0426(10) Uani 1 1 d . B 1
C60B C 0.6246(5) 0.7251(2) 0.31988(18) 0.0439(11) Uani 1 1 d . B 1
N61B N 0.4905(4) 0.70606(18) 0.30419(14) 0.0416(9) Uani 1 1 d . B 1
C62B C 0.4150(5) 0.6910(2) 0.3384(2) 0.0493(12) Uani 1 1 d . B 1
H62B H 0.3204 0.6784 0.3282 0.059 Uiso 1 1 calc R B 1
C63B C 0.4686(6) 0.6931(3) 0.3881(2) 0.0565(14) Uani 1 1 d . B 1
H63B H 0.4109 0.6826 0.4112 0.068 Uiso 1 1 calc R B 1
C64B C 0.6059(6) 0.7106(3) 0.4037(2) 0.0567(14) Uani 1 1 d . B 1
H64B H 0.6454 0.7107 0.4373 0.068 Uiso 1 1 calc R B 1
C65B C 0.6861(5) 0.7282(2) 0.36917(18) 0.0482(12) Uani 1 1 d . B 1
C66B C 0.9041(5) 0.7711(2) 0.34484(19) 0.0463(11) Uani 1 1 d . B 1
N67B N 1.0343(4) 0.7918(2) 0.35515(16) 0.0510(10) Uani 1 1 d . B 1
C68B C 1.0985(6) 0.7882(3) 0.4025(2) 0.0567(14) Uani 1 1 d . B 1
C69B C 1.0284(6) 0.7639(3) 0.4376(2) 0.0629(15) Uani 1 1 d . B 1
N70B N 0.8919(5) 0.7457(2) 0.42703(17) 0.0609(12) Uani 1 1 d . B 1
C71B C 0.8317(6) 0.7491(2) 0.38179(19) 0.0515(12) Uani 1 1 d . B 1
C72B C 1.2400(6) 0.8062(3) 0.4149(2) 0.0604(15) Uani 1 1 d . B 1
H72B H 1.2862 0.8253 0.3924 0.072 Uiso 1 1 calc R B 1
C73B C 1.3124(6) 0.7958(3) 0.4607(2) 0.0668(17) Uani 1 1 d . B 1
C74B C 1.2424(7) 0.7686(3) 0.4946(2) 0.0704(18) Uani 1 1 d . B 1
C75B C 1.1008(7) 0.7556(3) 0.4836(2) 0.0730(19) Uani 1 1 d . B 1
H75B H 1.0524 0.7408 0.5077 0.088 Uiso 1 1 calc R B 1
C76B C 1.4603(7) 0.8099(4) 0.4724(3) 0.079(2) Uani 1 1 d . B 1
H76B H 1.5088 0.8302 0.4513 0.094 Uiso 1 1 calc R B 1
C77B C 1.5283(7) 0.7926(4) 0.5157(3) 0.084(2) Uani 1 1 d . B 1
H77B H 1.6257 0.8006 0.5234 0.101 Uiso 1 1 calc R B 1
C78B C 1.4599(8) 0.7640(4) 0.5486(3) 0.088(2) Uani 1 1 d . B 1
H78B H 1.5113 0.7521 0.5774 0.106 Uiso 1 1 calc R B 1
C79B C 1.3210(8) 0.7534(4) 0.5395(2) 0.083(2) Uani 1 1 d . B 1
H79B H 1.2745 0.7357 0.5627 0.100 Uiso 1 1 calc R B 1
B80 B 0.6421(7) 0.2624(3) 0.3153(3) 0.0607(17) Uani 1 1 d . C 1
F81 F 0.7073(4) 0.21705(17) 0.32861(16) 0.0792(11) Uani 1 1 d . C 1
F82 F 0.6439(4) 0.30270(18) 0.35475(14) 0.0774(10) Uani 1 1 d . C 1
F83 F 0.7110(4) 0.2890(2) 0.27980(17) 0.0877(12) Uani 1 1 d . C 1
F84 F 0.5079(4) 0.24788(17) 0.29338(14) 0.0739(10) Uani 1 1 d . C 1
B85 B 0.7308(5) 0.0474(3) 0.1542(2) 0.0435(12) Uani 1 1 d . D 1
F86 F 0.7799(3) 0.09956(13) 0.14149(12) 0.0543(7) Uani 1 1 d . D 1
F87 F 0.7286(3) 0.05213(14) 0.20500(10) 0.0515(7) Uani 1 1 d . D 1
F88 F 0.8164(3) 0.00606(13) 0.14255(10) 0.0500(7) Uani 1 1 d . D 1
F89 F 0.5975(3) 0.03301(14) 0.12938(11) 0.0557(8) Uani 1 1 d . D 1
B90 B 0.8537(7) 0.6918(3) 0.1114(2) 0.0541(15) Uani 1 1 d . E 1
F91 F 0.9739(4) 0.70934(18) 0.14455(16) 0.0781(11) Uani 1 1 d . E 1
F92 F 0.7694(4) 0.65821(15) 0.13596(14) 0.0676(9) Uani 1 1 d . E 1
F93 F 0.8908(6) 0.66074(17) 0.07195(16) 0.0958(14) Uani 1 1 d . E 1
F94 F 0.7877(4) 0.73874(15) 0.09797(13) 0.0686(9) Uani 1 1 d . E 1
B95 B 0.6123(7) 0.8811(3) 0.3649(3) 0.0596(16) Uani 1 1 d . . .
F96 F 0.5398(4) 0.92814(16) 0.35915(15) 0.0759(10) Uani 1 1 d . . .
F97 F 0.7031(5) 0.88701(19) 0.40870(17) 0.1015(16) Uani 1 1 d . . .
F98 F 0.5208(5) 0.83417(17) 0.36538(13) 0.0848(12) Uani 1 1 d . . .
F99 F 0.6820(4) 0.87126(17) 0.32494(16) 0.0805(11) Uani 1 1 d . . .
C100 C 0.1087(11) 0.3343(5) 0.0462(5) 0.090(3) Uiso 0.70 1 d PD . .
H10C H 0.1201 0.3475 0.0143 0.135 Uiso 0.70 1 calc PR . .
H10D H 0.1759 0.3065 0.0545 0.135 Uiso 0.70 1 calc PR . .
H10E H 0.1241 0.3665 0.0716 0.135 Uiso 0.70 1 calc PR . .
O101 O -0.0252(7) 0.3093(3) 0.0437(3) 0.0828(19) Uiso 0.70 1 d PD . .
H101 H -0.0217 0.2746 0.0469 0.099 Uiso 0.70 1 calc PR . .
C102 C 0.8654(13) 0.4345(5) 0.0228(5) 0.083(3) Uiso 0.60 1 d PD . .
H10F H 0.8042 0.4633 0.0116 0.124 Uiso 0.60 1 calc PR . .
H10G H 0.8935 0.4134 -0.0058 0.124 Uiso 0.60 1 calc PR . .
H10H H 0.9477 0.4528 0.0442 0.124 Uiso 0.60 1 calc PR . .
O103 O 0.7963(9) 0.3978(4) 0.0486(3) 0.084(2) Uiso 0.60 1 d PD . .
H103 H 0.8493 0.3735 0.0587 0.101 Uiso 0.60 1 calc PR . .
C104 C 0.590(3) 0.4586(11) 0.0832(7) 0.138(8) Uiso 0.50 1 d PD F 1
H10I H 0.6128 0.4992 0.0834 0.208 Uiso 0.50 1 calc PR F 1
H10J H 0.4895 0.4510 0.0799 0.208 Uiso 0.50 1 calc PR F 1
H10K H 0.6242 0.4383 0.0555 0.208 Uiso 0.50 1 calc PR F 1
O105 O 0.6501(10) 0.4410(4) 0.1256(4) 0.075(2) Uiso 0.50 1 d PD F 1
H105 H 0.5914 0.4216 0.1377 0.090 Uiso 0.50 1 calc PR F 1
C106 C 0.579(3) 0.5220(19) 0.090(2) 0.15(2) Uiso 0.25 1 d PD G 3
H10L H 0.5669 0.5346 0.1233 0.228 Uiso 0.25 1 calc PRD G 3
H10M H 0.6510 0.4951 0.0903 0.228 Uiso 0.25 1 calc PRD G 3
H10N H 0.4918 0.5036 0.0716 0.228 Uiso 0.25 1 calc PRD G 3
O107 O 0.619(2) 0.5682(9) 0.0661(9) 0.083(6) Uiso 0.25 1 d PD G 3
H107 H 0.5624 0.5699 0.0403 0.099 Uiso 0.25 1 calc PR G 3
C108 C 0.650(3) 0.5810(14) 0.0339(9) 0.084(8) Uiso 0.25 1 d PD H 1
H10O H 0.7330 0.5715 0.0549 0.125 Uiso 0.25 1 calc PR H 1
H10P H 0.5674 0.5657 0.0461 0.125 Uiso 0.25 1 calc PR H 1
H10Q H 0.6487 0.6222 0.0346 0.125 Uiso 0.25 1 calc PR H 1
O109 O 0.649(2) 0.5582(9) -0.0134(7) 0.084(5) Uiso 0.25 1 d PD H 1
H109 H 0.7273 0.5463 -0.0160 0.100 Uiso 0.25 1 calc PR H 1
O110 O 0.6005(15) 0.5541(7) 0.0932(6) 0.089(4) Uiso 0.40 1 d P I 2
C111 C 0.959(3) 0.6175(15) 0.3751(10) 0.114(10) Uiso 0.30 1 d PD J 1
H11C H 1.0472 0.6285 0.3647 0.171 Uiso 0.30 1 calc PR J 1
H11D H 0.9563 0.5777 0.3817 0.171 Uiso 0.30 1 calc PR J 1
H11E H 0.9486 0.6411 0.4051 0.171 Uiso 0.30 1 calc PR J 1
O112 O 0.8474(12) 0.6251(5) 0.3368(4) 0.047(3) Uiso 0.30 1 d PD J 1
H112 H 0.7960 0.5950 0.3301 0.057 Uiso 0.30 1 calc PR J 1
C113 C 0.655(4) 0.5588(18) 0.3686(16) 0.091(11) Uiso 0.20 1 d PD K 2
H11F H 0.6389 0.5739 0.4012 0.137 Uiso 0.20 1 calc PR K 2
H11G H 0.6703 0.5185 0.3688 0.137 Uiso 0.20 1 calc PR K 2
H11H H 0.5749 0.5636 0.3441 0.137 Uiso 0.20 1 calc PR K 2
O114 O 0.775(3) 0.5885(15) 0.3564(13) 0.107(10) Uiso 0.20 1 d PD K 2
H114 H 0.8364 0.5939 0.3814 0.128 Uiso 0.20 1 calc PR K 2
C115 C 0.368(5) 0.5054(15) 0.4074(15) 0.093(12) Uiso 0.20 1 d PD . .
H11I H 0.4538 0.5092 0.4313 0.139 Uiso 0.20 1 calc PR . .
H11J H 0.3662 0.4706 0.3854 0.139 Uiso 0.20 1 calc PR . .
H11K H 0.2883 0.5037 0.4249 0.139 Uiso 0.20 1 calc PR . .
O116 O 0.364(3) 0.5515(12) 0.3801(11) 0.096(8) Uiso 0.20 1 d PD . .
H116 H 0.3926 0.5431 0.3533 0.115 Uiso 0.20 1 calc PR . .
O117 O 0.6239(6) 0.3749(3) 0.2069(3) 0.0815(18) Uani 0.80 1 d P . .
O118 O 0.134(3) 0.6167(14) 0.3947(12) 0.105(9) Uiso 0.20 1 d P L 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N55A 1.969(4) . ?
Fe1A N9A 1.978(4) . ?
Fe1A N3A 1.979(4) . ?
Fe1A N61A 1.979(4) . ?
Fe1A N35A 1.981(4) . ?
Fe1A N29A 1.994(4) . ?
C2A N3A 1.349(6) . ?
C2A C7A 1.377(6) . ?
C2A C8A 1.449(6) . ?
N3A C4A 1.332(6) . ?
C4A C5A 1.393(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.367(7) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.409(7) . ?
C6A H6A 0.9500 . ?
C7A C14A 1.462(7) . ?
C8A N9A 1.369(6) . ?
C8A C13A 1.375(7) . ?
N9A C10A 1.339(6) . ?
C10A C11A 1.392(7) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.380(7) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.416(7) . ?
C12A H12A 0.9500 . ?
C13A C19A 1.468(7) . ?
C14A N15A 1.327(6) . ?
C14A C19A 1.452(7) . ?
N15A C16A 1.358(7) . ?
C16A C20A 1.405(7) . ?
C16A C17A 1.431(8) . ?
C17A N18A 1.372(7) . ?
C17A C23A 1.397(8) . ?
N18A C19A 1.316(7) . ?
C20A C21A 1.393(9) . ?
C20A H20A 0.9500 . ?
C21A C24A 1.425(8) . ?
C21A C22A 1.441(10) . ?
C22A C27A 1.413(9) . ?
C22A C23A 1.417(8) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.347(10) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.407(11) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.343(9) . ?
C26A H26A 0.9500 . ?
C27A H27A 0.9500 . ?
C28A N29A 1.364(6) . ?
C28A C33A 1.384(6) . ?
C28A C34A 1.452(6) . ?
N29A C30A 1.350(6) . ?
C30A C31A 1.380(7) . ?
C30A H30A 0.9500 . ?
C31A C32A 1.378(8) . ?
C31A H31A 0.9500 . ?
C32A C33A 1.411(6) . ?
C32A H32A 0.9500 . ?
C33A C40A 1.452(7) . ?
C34A N35A 1.361(6) . ?
C34A C39A 1.381(6) . ?
N35A C36A 1.345(5) . ?
C36A C37A 1.387(7) . ?
C36A H36A 0.9500 . ?
C37A C38A 1.364(7) . ?
C37A H37A 0.9500 . ?
C38A C39A 1.409(6) . ?
C38A H38A 0.9500 . ?
C39A C45A 1.456(7) . ?
C40A N41A 1.319(6) . ?
C40A C45A 1.451(7) . ?
N41A C42A 1.365(7) . ?
C42A C46A 1.385(8) . ?
C42A C43A 1.443(9) . ?
C43A N44A 1.353(7) . ?
C43A C49A 1.413(8) . ?
N44A C45A 1.326(6) . ?
C46A C47A 1.393(10) . ?
C46A H46A 0.9500 . ?
C47A C50A 1.422(9) . ?
C47A C48A 1.464(11) . ?
C48A C49A 1.381(9) . ?
C48A C53A 1.417(10) . ?
C49A H49A 0.9500 . ?
C50A C51A 1.337(12) . ?
C50A H50A 0.9500 . ?
C51A C52A 1.422(14) . ?
C51A H51A 0.9500 . ?
C52A C53A 1.372(12) . ?
C52A H52A 0.9500 . ?
C53A H53A 0.9500 . ?
C54A N55A 1.342(6) . ?
C54A C59A 1.389(6) . ?
C54A C60A 1.450(7) . ?
N55A C56A 1.348(6) . ?
C56A C57A 1.384(7) . ?
C56A H56A 0.9500 . ?
C57A C58A 1.382(7) . ?
C57A H57A 0.9500 . ?
C58A C59A 1.409(7) . ?
C58A H58A 0.9500 . ?
C59A C66A 1.457(7) . ?
C60A N61A 1.355(6) . ?
C60A C65A 1.390(7) . ?
N61A C62A 1.355(6) . ?
C62A C63A 1.386(7) . ?
C62A H62A 0.9500 . ?
C63A C64A 1.368(7) . ?
C63A H63A 0.9500 . ?
C64A C65A 1.403(7) . ?
C64A H64A 0.9500 . ?
C65A C71A 1.487(6) . ?
C66A N67A 1.311(6) . ?
C66A C71A 1.438(7) . ?
N67A C68A 1.360(7) . ?
C68A C72A 1.399(7) . ?
C68A C69A 1.427(7) . ?
C69A N70A 1.371(6) . ?
C69A C75A 1.385(7) . ?
N70A C71A 1.305(7) . ?
C72A C73A 1.394(7) . ?
C72A H72A 0.9500 . ?
C73A C76A 1.429(7) . ?
C73A C74A 1.444(8) . ?
C74A C75A 1.401(7) . ?
C74A C79A 1.422(7) . ?
C75A H75A 0.9500 . ?
C76A C77A 1.356(7) . ?
C76A H76A 0.9500 . ?
C77A C78A 1.425(8) . ?
C77A H77A 0.9500 . ?
C78A C79A 1.366(8) . ?
C78A H78A 0.9500 . ?
C79A H79A 0.9500 . ?
Fe1B N3B 1.953(4) . ?
Fe1B N29B 1.980(4) . ?
Fe1B N55B 1.981(4) . ?
Fe1B N35B 1.982(4) . ?
Fe1B N9B 1.985(4) . ?
Fe1B N61B 1.994(4) . ?
C2B N3B 1.362(5) . ?
C2B C7B 1.387(6) . ?
C2B C8B 1.444(6) . ?
N3B C4B 1.327(6) . ?
C4B C5B 1.393(7) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.377(7) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.402(7) . ?
C6B H6B 0.9500 . ?
C7B C14B 1.471(6) . ?
C8B N9B 1.367(6) . ?
C8B C13B 1.390(6) . ?
N9B C10B 1.337(6) . ?
C10B C11B 1.388(7) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.387(7) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.395(7) . ?
C12B H12B 0.9500 . ?
C13B C19B 1.472(6) . ?
C14B N15B 1.304(6) . ?
C14B C19B 1.440(7) . ?
N15B C16B 1.371(6) . ?
C16B C20B 1.401(6) . ?
C16B C17B 1.427(7) . ?
C17B N18B 1.363(6) . ?
C17B C23B 1.406(6) . ?
N18B C19B 1.324(6) . ?
C20B C21B 1.391(6) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.423(7) . ?
C21B C24B 1.437(6) . ?
C22B C23B 1.395(7) . ?
C22B C27B 1.430(6) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.357(7) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.407(8) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.347(7) . ?
C26B H26B 0.9500 . ?
C27B H27B 0.9500 . ?
C28B N29B 1.360(6) . ?
C28B C33B 1.398(6) . ?
C28B C34B 1.438(6) . ?
N29B C30B 1.335(6) . ?
C30B C31B 1.387(7) . ?
C30B H30B 0.9500 . ?
C31B C32B 1.380(8) . ?
C31B H31B 0.9500 . ?
C32B C33B 1.396(7) . ?
C32B H32B 0.9500 . ?
C33B C40B 1.464(7) . ?
C34B N35B 1.364(6) . ?
C34B C39B 1.393(7) . ?
N35B C36B 1.336(6) . ?
C36B C37B 1.389(8) . ?
C36B H36B 0.9500 . ?
C37B C38B 1.371(8) . ?
C37B H37B 0.9500 . ?
C38B C39B 1.399(7) . ?
C38B H3B8 0.9500 . ?
C39B C45B 1.468(7) . ?
C40B N41B 1.321(6) . ?
C40B C45B 1.435(7) . ?
N41B C42B 1.370(7) . ?
C42B C46B 1.389(7) . ?
C42B C43B 1.435(8) . ?
C43B N44B 1.367(7) . ?
C43B C49B 1.389(8) . ?
N44B C45B 1.318(7) . ?
C46B C47B 1.396(8) . ?
C46B H46B 0.9500 . ?
C47B C48B 1.427(8) . ?
C47B C50B 1.428(8) . ?
C48B C49B 1.411(8) . ?
C48B C53B 1.428(8) . ?
C49B H49B 0.9500 . ?
C50B C51B 1.352(8) . ?
C50B H50B 0.9500 . ?
C51B C52B 1.407(9) . ?
C51B H51B 0.9500 . ?
C52B C53B 1.358(9) . ?
C52B H52B 0.9500 . ?
C53B H53B 0.9500 . ?
C54B N55B 1.360(6) . ?
C54B C59B 1.390(7) . ?
C54B C60B 1.440(7) . ?
N55B C56B 1.332(6) . ?
C56B C57B 1.403(7) . ?
C56B H56B 0.9500 . ?
C57B C58B 1.366(7) . ?
C57B H57B 0.9500 . ?
C58B C59B 1.395(7) . ?
C58B H58B 0.9500 . ?
C59B C66B 1.470(7) . ?
C60B N61B 1.357(6) . ?
C60B C65B 1.398(7) . ?
N61B C62B 1.341(7) . ?
C62B C63B 1.391(8) . ?
C62B H62B 0.9500 . ?
C63B C64B 1.377(8) . ?
C63B H63B 0.9500 . ?
C64B C65B 1.395(8) . ?
C64B H64B 0.9500 . ?
C65B C71B 1.462(8) . ?
C66B N67B 1.320(7) . ?
C66B C71B 1.441(8) . ?
N67B C68B 1.378(7) . ?
C68B C72B 1.408(8) . ?
C68B C69B 1.411(9) . ?
C69B N70B 1.360(8) . ?
C69B C75B 1.396(8) . ?
N70B C71B 1.312(7) . ?
C72B C73B 1.407(8) . ?
C72B H72B 0.9500 . ?
C73B C74B 1.414(11) . ?
C73B C76B 1.448(9) . ?
C74B C75B 1.385(10) . ?
C74B C79B 1.446(8) . ?
C75B H75B 0.9500 . ?
C76B C77B 1.389(10) . ?
C76B H76B 0.9500 . ?
C77B C78B 1.403(12) . ?
C77B H77B 0.9500 . ?
C78B C79B 1.351(11) . ?
C78B H78B 0.9500 . ?
C79B H79B 0.9500 . ?
B80 F81 1.340(8) . ?
B80 F84 1.373(8) . ?
B80 F82 1.385(8) . ?
B80 F83 1.437(8) . ?
B85 F88 1.380(6) . ?
B85 F89 1.390(6) . ?
B85 F86 1.395(7) . ?
B85 F87 1.399(6) . ?
B90 F93 1.369(8) . ?
B90 F94 1.379(7) . ?
B90 F91 1.397(8) . ?
B90 F92 1.398(7) . ?
B95 F96 1.372(8) . ?
B95 F97 1.380(7) . ?
B95 F98 1.391(8) . ?
B95 F99 1.391(9) . ?
C100 O101 1.397(11) . ?
C100 H10C 0.9800 . ?
C100 H10D 0.9800 . ?
C100 H10E 0.9800 . ?
O101 H101 0.8400 . ?
C102 O103 1.381(12) . ?
C102 H10F 0.9800 . ?
C102 H10G 0.9800 . ?
C102 H10H 0.9800 . ?
O103 H103 0.8400 . ?
C104 O105 1.341(16) . ?
C104 H10I 0.9800 . ?
C104 H10J 0.9800 . ?
C104 H10K 0.9800 . ?
O105 H105 0.8400 . ?
C106 O107 1.39(2) . ?
C106 H10L 0.9800 . ?
C106 H10M 0.9800 . ?
C106 H10N 0.9800 . ?
O107 H107 0.8400 . ?
C108 O109 1.368(18) . ?
C108 H10O 0.9800 . ?
C108 H10P 0.9800 . ?
C108 H10Q 0.9800 . ?
O109 H109 0.8400 . ?
C111 O112 1.434(18) . ?
C111 H11C 0.9800 . ?
C111 H11D 0.9800 . ?
C111 H11E 0.9800 . ?
O112 H112 0.8400 . ?
C113 O114 1.428(19) . ?
C113 H11F 0.9800 . ?
C113 H11G 0.9800 . ?
C113 H11H 0.9800 . ?
O114 H114 0.8400 . ?
C115 O116 1.386(19) . ?
C115 H11I 0.9800 . ?
C115 H11J 0.9800 . ?
C115 H11K 0.9800 . ?
O116 H116 0.8400 . ?

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
N55A Fe1A N9A 94.11(16) . . ?
N55A Fe1A N3A 93.34(16) . . ?
N9A Fe1A N3A 82.01(16) . . ?
N55A Fe1A N61A 82.10(16) . . ?
N9A Fe1A N61A 172.56(16) . . ?
N3A Fe1A N61A 91.79(15) . . ?
N55A Fe1A N35A 172.49(16) . . ?
N9A Fe1A N35A 88.79(16) . . ?
N3A Fe1A N35A 93.92(15) . . ?
N61A Fe1A N35A 95.76(15) . . ?
N55A Fe1A N29A 90.43(16) . . ?
N9A Fe1A N29A 97.10(16) . . ?
N3A Fe1A N29A 176.18(15) . . ?
N61A Fe1A N29A 89.36(16) . . ?
N35A Fe1A N29A 82.34(15) . . ?
N3A C2A C7A 123.8(4) . . ?
N3A C2A C8A 115.2(4) . . ?
C7A C2A C8A 121.0(4) . . ?
C4A N3A C2A 117.1(4) . . ?
C4A N3A Fe1A 128.7(3) . . ?
C2A N3A Fe1A 114.2(3) . . ?
N3A C4A C5A 122.9(5) . . ?
N3A C4A H4A 118.5 . . ?
C5A C4A H4A 118.5 . . ?
C6A C5A C4A 119.7(5) . . ?
C6A C5A H5A 120.2 . . ?
C4A C5A H5A 120.2 . . ?
C5A C6A C7A 118.2(4) . . ?
C5A C6A H6A 120.9 . . ?
C7A C6A H6A 120.9 . . ?
C2A C7A C6A 118.1(5) . . ?
C2A C7A C14A 119.3(4) . . ?
C6A C7A C14A 122.6(4) . . ?
N9A C8A C13A 123.9(4) . . ?
N9A C8A C2A 114.7(4) . . ?
C13A C8A C2A 121.4(4) . . ?
C10A N9A C8A 117.2(4) . . ?
C10A N9A Fe1A 129.0(3) . . ?
C8A N9A Fe1A 113.7(3) . . ?
N9A C10A C11A 122.6(5) . . ?
N9A C10A H10A 118.7 . . ?
C11A C10A H10A 118.7 . . ?
C12A C11A C10A 120.2(5) . . ?
C12A C11A H11A 119.9 . . ?
C10A C11A H11A 119.9 . . ?
C11A C12A C13A 118.1(5) . . ?
C11A C12A H12A 121.0 . . ?
C13A C12A H12A 121.0 . . ?
C8A C13A C12A 118.1(4) . . ?
C8A C13A C19A 120.1(4) . . ?
C12A C13A C19A 121.8(5) . . ?
N15A C14A C19A 122.2(5) . . ?
N15A C14A C7A 117.7(4) . . ?
C19A C14A C7A 120.1(4) . . ?
C14A N15A C16A 116.3(5) . . ?
N15A C16A C20A 117.9(5) . . ?
N15A C16A C17A 122.2(5) . . ?
C20A C16A C17A 119.9(5) . . ?
N18A C17A C23A 119.7(5) . . ?
N18A C17A C16A 120.2(5) . . ?
C23A C17A C16A 120.0(5) . . ?
C19A N18A C17A 117.6(5) . . ?
N18A C19A C14A 121.4(4) . . ?
N18A C19A C13A 120.6(5) . . ?
C14A C19A C13A 118.0(4) . . ?
C21A C20A C16A 120.7(6) . . ?
C21A C20A H20A 119.6 . . ?
C16A C20A H20A 119.6 . . ?
C20A C21A C24A 121.4(7) . . ?
C20A C21A C22A 119.6(5) . . ?
C24A C21A C22A 119.0(6) . . ?
C27A C22A C23A 123.0(6) . . ?
C27A C22A C21A 117.2(6) . . ?
C23A C22A C21A 119.7(5) . . ?
C17A C23A C22A 120.0(6) . . ?
C17A C23A H23A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C25A C24A C21A 120.6(7) . . ?
C25A C24A H24A 119.7 . . ?
C21A C24A H24A 119.7 . . ?
C24A C25A C26A 120.3(6) . . ?
C24A C25A H25A 119.9 . . ?
C26A C25A H25A 119.8 . . ?
C27A C26A C25A 121.0(6) . . ?
C27A C26A H26A 119.5 . . ?
C25A C26A H26A 119.5 . . ?
C26A C27A C22A 121.8(7) . . ?
C26A C27A H27A 119.1 . . ?
C22A C27A H27A 119.1 . . ?
N29A C28A C33A 123.5(4) . . ?
N29A C28A C34A 115.1(4) . . ?
C33A C28A C34A 121.4(4) . . ?
C30A N29A C28A 117.3(4) . . ?
C30A N29A Fe1A 129.2(3) . . ?
C28A N29A Fe1A 113.3(3) . . ?
N29A C30A C31A 122.6(5) . . ?
N29A C30A H30A 118.7 . . ?
C31A C30A H30A 118.7 . . ?
C32A C31A C30A 120.1(4) . . ?
C32A C31A H31A 120.0 . . ?
C30A C31A H31A 120.0 . . ?
C31A C32A C33A 118.7(4) . . ?
C31A C32A H32A 120.7 . . ?
C33A C32A H32A 120.7 . . ?
C28A C33A C32A 117.9(4) . . ?
C28A C33A C40A 119.3(4) . . ?
C32A C33A C40A 122.8(4) . . ?
N35A C34A C39A 123.8(4) . . ?
N35A C34A C28A 115.4(4) . . ?
C39A C34A C28A 120.8(4) . . ?
C36A N35A C34A 117.1(4) . . ?
C36A N35A Fe1A 129.1(3) . . ?
C34A N35A Fe1A 113.7(3) . . ?
N35A C36A C37A 122.4(4) . . ?
N35A C36A H36A 118.8 . . ?
C37A C36A H36A 118.8 . . ?
C38A C37A C36A 120.2(4) . . ?
C38A C37A H37A 119.9 . . ?
C36A C37A H37A 119.9 . . ?
C37A C38A C39A 118.9(4) . . ?
C37A C38A H38A 120.6 . . ?
C39A C38A H38A 120.6 . . ?
C34A C39A C38A 117.7(4) . . ?
C34A C39A C45A 119.5(4) . . ?
C38A C39A C45A 122.8(4) . . ?
N41A C40A C45A 121.5(5) . . ?
N41A C40A C33A 119.1(4) . . ?
C45A C40A C33A 119.4(4) . . ?
C40A N41A C42A 117.5(5) . . ?
N41A C42A C46A 119.1(6) . . ?
N41A C42A C43A 120.3(5) . . ?
C46A C42A C43A 120.5(6) . . ?
N44A C43A C49A 119.2(6) . . ?
N44A C43A C42A 121.8(5) . . ?
C49A C43A C42A 118.9(5) . . ?
C45A N44A C43A 116.6(5) . . ?
N44A C45A C40A 122.2(4) . . ?
N44A C45A C39A 118.3(4) . . ?
C40A C45A C39A 119.5(4) . . ?
C42A C46A C47A 120.3(7) . . ?
C42A C46A H46A 119.9 . . ?
C47A C46A H46A 119.9 . . ?
C46A C47A C50A 123.1(8) . . ?
C46A C47A C48A 120.1(6) . . ?
C50A C47A C48A 116.6(7) . . ?
C49A C48A C53A 121.6(8) . . ?
C49A C48A C47A 118.8(6) . . ?
C53A C48A C47A 119.6(7) . . ?
C48A C49A C43A 121.1(7) . . ?
C48A C49A H49A 119.5 . . ?
C43A C49A H49A 119.5 . . ?
C51A C50A C47A 122.7(9) . . ?
C51A C50A H50A 118.7 . . ?
C47A C50A H50A 118.7 . . ?
C50A C51A C52A 120.3(8) . . ?
C50A C51A H51A 119.9 . . ?
C52A C51A H51A 119.9 . . ?
C53A C52A C51A 120.8(8) . . ?
C53A C52A H52A 119.6 . . ?
C51A C52A H52A 119.6 . . ?
C52A C53A C48A 119.8(9) . . ?
C52A C53A H53A 120.1 . . ?
C48A C53A H53A 120.1 . . ?
N55A C54A C59A 124.1(4) . . ?
N55A C54A C60A 115.2(4) . . ?
C59A C54A C60A 120.6(4) . . ?
C54A N55A C56A 117.7(4) . . ?
C54A N55A Fe1A 114.1(3) . . ?
C56A N55A Fe1A 128.0(3) . . ?
N55A C56A C57A 122.2(5) . . ?
N55A C56A H56A 118.9 . . ?
C57A C56A H56A 118.9 . . ?
C58A C57A C56A 120.0(5) . . ?
C58A C57A H57A 120.0 . . ?
C56A C57A H57A 120.0 . . ?
C57A C58A C59A 118.6(4) . . ?
C57A C58A H58A 120.7 . . ?
C59A C58A H58A 120.7 . . ?
C54A C59A C58A 117.3(4) . . ?
C54A C59A C66A 119.8(4) . . ?
C58A C59A C66A 122.9(4) . . ?
N61A C60A C65A 123.3(4) . . ?
N61A C60A C54A 114.9(4) . . ?
C65A C60A C54A 121.8(4) . . ?
C62A N61A C60A 117.3(4) . . ?
C62A N61A Fe1A 129.1(3) . . ?
C60A N61A Fe1A 113.5(3) . . ?
N61A C62A C63A 122.0(4) . . ?
N61A C62A H62A 119.0 . . ?
C63A C62A H62A 119.0 . . ?
C64A C63A C62A 120.8(4) . . ?
C64A C63A H63A 119.6 . . ?
C62A C63A H63A 119.6 . . ?
C63A C64A C65A 118.2(5) . . ?
C63A C64A H64A 120.9 . . ?
C65A C64A H64A 120.9 . . ?
C60A C65A C64A 118.4(4) . . ?
C60A C65A C71A 118.5(4) . . ?
C64A C65A C71A 123.0(4) . . ?
N67A C66A C71A 121.8(5) . . ?
N67A C66A C59A 118.1(4) . . ?
C71A C66A C59A 120.0(4) . . ?
C66A N67A C68A 116.8(4) . . ?
N67A C68A C72A 118.6(5) . . ?
N67A C68A C69A 121.5(4) . . ?
C72A C68A C69A 119.8(5) . . ?
N70A C69A C75A 119.1(5) . . ?
N70A C69A C68A 120.5(4) . . ?
C75A C69A C68A 120.4(5) . . ?
C71A N70A C69A 116.7(4) . . ?
N70A C71A C66A 122.7(4) . . ?
N70A C71A C65A 118.2(4) . . ?
C66A C71A C65A 119.2(4) . . ?
C73A C72A C68A 120.5(5) . . ?
C73A C72A H72A 119.8 . . ?
C68A C72A H72A 119.8 . . ?
C72A C73A C76A 121.0(5) . . ?
C72A C73A C74A 119.4(5) . . ?
C76A C73A C74A 119.6(5) . . ?
C75A C74A C79A 122.8(5) . . ?
C75A C74A C73A 119.7(5) . . ?
C79A C74A C73A 117.5(5) . . ?
C69A C75A C74A 120.2(5) . . ?
C69A C75A H75A 119.9 . . ?
C74A C75A H75A 119.9 . . ?
C77A C76A C73A 120.7(5) . . ?
C77A C76A H76A 119.6 . . ?
C73A C76A H76A 119.7 . . ?
C76A C77A C78A 120.0(5) . . ?
C76A C77A H77A 120.0 . . ?
C78A C77A H77A 120.0 . . ?
C79A C78A C77A 121.0(5) . . ?
C79A C78A H78A 119.5 . . ?
C77A C78A H78A 119.5 . . ?
C78A C79A C74A 121.1(5) . . ?
C78A C79A H79A 119.4 . . ?
C74A C79A H79A 119.4 . . ?
N3B Fe1B N29B 173.77(16) . . ?
N3B Fe1B N55B 91.24(16) . . ?
N29B Fe1B N55B 94.68(16) . . ?
N3B Fe1B N35B 92.08(16) . . ?
N29B Fe1B N35B 82.31(16) . . ?
N55B Fe1B N35B 171.59(16) . . ?
N3B Fe1B N9B 82.86(15) . . ?
N29B Fe1B N9B 94.58(16) . . ?
N55B Fe1B N9B 96.04(16) . . ?
N35B Fe1B N9B 92.04(16) . . ?
N3B Fe1B N61B 94.73(16) . . ?
N29B Fe1B N61B 88.00(16) . . ?
N55B Fe1B N61B 82.12(16) . . ?
N35B Fe1B N61B 89.90(17) . . ?
N9B Fe1B N61B 176.96(17) . . ?
N3B C2B C7B 122.7(4) . . ?
N3B C2B C8B 116.3(4) . . ?
C7B C2B C8B 121.0(4) . . ?
C4B N3B C2B 118.2(4) . . ?
C4B N3B Fe1B 129.1(3) . . ?
C2B N3B Fe1B 112.6(3) . . ?
N3B C4B C5B 122.5(4) . . ?
N3B C4B H4B 118.8 . . ?
C5B C4B H4B 118.7 . . ?
C6B C5B C4B 119.5(4) . . ?
C6B C5B H5B 120.2 . . ?
C4B C5B H5B 120.2 . . ?
C5B C6B C7B 118.8(4) . . ?
C5B C6B H6B 120.6 . . ?
C7B C6B H6B 120.6 . . ?
C2B C7B C6B 118.0(4) . . ?
C2B C7B C14B 119.0(4) . . ?
C6B C7B C14B 123.0(4) . . ?
N9B C8B C13B 123.7(4) . . ?
N9B C8B C2B 114.1(4) . . ?
C13B C8B C2B 122.1(4) . . ?
C10B N9B C8B 117.3(4) . . ?
C10B N9B Fe1B 130.1(3) . . ?
C8B N9B Fe1B 112.3(3) . . ?
N9B C10B C11B 122.3(4) . . ?
N9B C10B H10B 118.8 . . ?
C11B C10B H10B 118.8 . . ?
C12B C11B C10B 120.1(5) . . ?
C12B C11B H11B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C11B C12B C13B 118.7(4) . . ?
C11B C12B H12B 120.6 . . ?
C13B C12B H12B 120.6 . . ?
C8B C13B C12B 117.7(4) . . ?
C8B C13B C19B 118.1(4) . . ?
C12B C13B C19B 124.2(4) . . ?
N15B C14B C19B 123.2(4) . . ?
N15B C14B C7B 117.2(4) . . ?
C19B C14B C7B 119.6(4) . . ?
C14B N15B C16B 116.5(4) . . ?
N15B C16B C20B 118.4(4) . . ?
N15B C16B C17B 120.6(4) . . ?
C20B C16B C17B 121.0(4) . . ?
N18B C17B C23B 119.6(4) . . ?
N18B C17B C16B 121.9(4) . . ?
C23B C17B C16B 118.4(4) . . ?
C19B N18B C17B 116.3(4) . . ?
N18B C19B C14B 121.5(4) . . ?
N18B C19B C13B 118.8(4) . . ?
C14B C19B C13B 119.7(4) . . ?
C21B C20B C16B 119.6(4) . . ?
C21B C20B H20B 120.2 . . ?
C16B C20B H20B 120.2 . . ?
C20B C21B C22B 120.3(4) . . ?
C20B C21B C24B 120.2(5) . . ?
C22B C21B C24B 119.5(4) . . ?
C23B C22B C21B 119.9(4) . . ?
C23B C22B C27B 122.3(5) . . ?
C21B C22B C27B 117.9(4) . . ?
C22B C23B C17B 120.8(5) . . ?
C22B C23B H23B 119.6 . . ?
C17B C23B H23B 119.6 . . ?
C25B C24B C21B 119.5(5) . . ?
C25B C24B H24B 120.2 . . ?
C21B C24B H24B 120.2 . . ?
C24B C25B C26B 121.1(5) . . ?
C24B C25B H25B 119.4 . . ?
C26B C25B H25B 119.4 . . ?
C27B C26B C25B 120.8(5) . . ?
C27B C26B H26B 119.6 . . ?
C25B C26B H26B 119.6 . . ?
C26B C27B C22B 121.1(5) . . ?
C26B C27B H27B 119.4 . . ?
C22B C27B H27B 119.5 . . ?
N29B C28B C33B 123.7(4) . . ?
N29B C28B C34B 115.6(4) . . ?
C33B C28B C34B 120.7(4) . . ?
C30B N29B C28B 117.7(4) . . ?
C30B N29B Fe1B 129.7(4) . . ?
C28B N29B Fe1B 112.3(3) . . ?
N29B C30B C31B 121.8(5) . . ?
N29B C30B H30B 119.1 . . ?
C31B C30B H30B 119.1 . . ?
C32B C31B C30B 120.9(5) . . ?
C32B C31B H31B 119.6 . . ?
C30B C31B H31B 119.6 . . ?
C31B C32B C33B 118.4(5) . . ?
C31B C32B H32B 120.8 . . ?
C33B C32B H32B 120.8 . . ?
C32B C33B C28B 117.4(4) . . ?
C32B C33B C40B 123.4(4) . . ?
C28B C33B C40B 119.1(4) . . ?
N35B C34B C39B 123.0(4) . . ?
N35B C34B C28B 115.2(4) . . ?
C39B C34B C28B 121.7(4) . . ?
C36B N35B C34B 117.2(4) . . ?
C36B N35B Fe1B 129.8(3) . . ?
C34B N35B Fe1B 112.2(3) . . ?
N35B C36B C37B 123.0(5) . . ?
N35B C36B H36B 118.5 . . ?
C37B C36B H36B 118.5 . . ?
C38B C37B C36B 119.7(5) . . ?
C38B C37B H37B 120.2 . . ?
C36B C37B H37B 120.2 . . ?
C37B C38B C39B 119.0(5) . . ?
C37B C38B H3B8 120.5 . . ?
C39B C38B H3B8 120.5 . . ?
C34B C39B C38B 118.0(5) . . ?
C34B C39B C45B 118.9(4) . . ?
C38B C39B C45B 123.1(5) . . ?
N41B C40B C45B 121.8(5) . . ?
N41B C40B C33B 118.5(4) . . ?
C45B C40B C33B 119.7(4) . . ?
C40B N41B C42B 117.2(4) . . ?
N41B C42B C46B 119.4(5) . . ?
N41B C42B C43B 120.6(5) . . ?
C46B C42B C43B 119.9(5) . . ?
N44B C43B C49B 119.1(5) . . ?
N44B C43B C42B 121.1(5) . . ?
C49B C43B C42B 119.8(5) . . ?
C45B N44B C43B 116.7(4) . . ?
N44B C45B C40B 122.6(5) . . ?
N44B C45B C39B 117.9(4) . . ?
C40B C45B C39B 119.5(4) . . ?
C42B C46B C47B 120.5(5) . . ?
C42B C46B H46B 119.8 . . ?
C47B C46B H46B 119.8 . . ?
C46B C47B C48B 120.1(5) . . ?
C46B C47B C50B 122.1(5) . . ?
C48B C47B C50B 117.9(5) . . ?
C49B C48B C47B 119.3(5) . . ?
C49B C48B C53B 121.8(5) . . ?
C47B C48B C53B 118.9(5) . . ?
C43B C49B C48B 120.4(5) . . ?
C43B C49B H49B 119.8 . . ?
C48B C49B H49B 119.8 . . ?
C51B C50B C47B 121.5(6) . . ?
C51B C50B H50B 119.3 . . ?
C47B C50B H50B 119.2 . . ?
C50B C51B C52B 120.4(5) . . ?
C50B C51B H51B 119.8 . . ?
C52B C51B H51B 119.8 . . ?
C53B C52B C51B 120.6(6) . . ?
C53B C52B H52B 119.7 . . ?
C51B C52B H52B 119.7 . . ?
C52B C53B C48B 120.7(6) . . ?
C52B C53B H53B 119.7 . . ?
C48B C53B H53B 119.7 . . ?
N55B C54B C59B 122.8(5) . . ?
N55B C54B C60B 115.8(4) . . ?
C59B C54B C60B 121.3(4) . . ?
C56B N55B C54B 118.3(4) . . ?
C56B N55B Fe1B 128.7(3) . . ?
C54B N55B Fe1B 113.0(3) . . ?
N55B C56B C57B 122.0(4) . . ?
N55B C56B H56B 119.0 . . ?
C57B C56B H56B 119.0 . . ?
C58B C57B C56B 119.3(5) . . ?
C58B C57B H57B 120.3 . . ?
C56B C57B H57B 120.3 . . ?
C57B C58B C59B 119.7(4) . . ?
C57B C58B H58B 120.1 . . ?
C59B C58B H58B 120.1 . . ?
C54B C59B C58B 117.7(4) . . ?
C54B C59B C66B 118.7(5) . . ?
C58B C59B C66B 123.6(4) . . ?
N61B C60B C65B 123.0(5) . . ?
N61B C60B C54B 115.2(4) . . ?
C65B C60B C54B 121.8(5) . . ?
C62B N61B C60B 117.3(4) . . ?
C62B N61B Fe1B 129.6(4) . . ?
C60B N61B Fe1B 112.9(3) . . ?
N61B C62B C63B 123.1(5) . . ?
N61B C62B H62B 118.5 . . ?
C63B C62B H62B 118.5 . . ?
C64B C63B C62B 119.5(5) . . ?
C64B C63B H63B 120.3 . . ?
C62B C63B H63B 120.3 . . ?
C63B C64B C65B 118.7(5) . . ?
C63B C64B H64B 120.6 . . ?
C65B C64B H64B 120.6 . . ?
C64B C65B C60B 118.4(5) . . ?
C64B C65B C71B 123.4(5) . . ?
C60B C65B C71B 118.2(5) . . ?
N67B C66B C71B 121.8(5) . . ?
N67B C66B C59B 118.6(5) . . ?
C71B C66B C59B 119.6(4) . . ?
C66B N67B C68B 115.9(5) . . ?
N67B C68B C72B 118.5(6) . . ?
N67B C68B C69B 121.6(5) . . ?
C72B C68B C69B 119.7(5) . . ?
N70B C69B C75B 118.6(6) . . ?
N70B C69B C68B 121.5(5) . . ?
C75B C69B C68B 119.9(6) . . ?
C71B N70B C69B 116.4(5) . . ?
N70B C71B C66B 122.6(5) . . ?
N70B C71B C65B 117.3(5) . . ?
C66B C71B C65B 120.0(4) . . ?
C73B C72B C68B 119.5(6) . . ?
C73B C72B H72B 120.2 . . ?
C68B C72B H72B 120.2 . . ?
C72B C73B C74B 120.1(6) . . ?
C72B C73B C76B 120.3(7) . . ?
C74B C73B C76B 119.6(6) . . ?
C75B C74B C73B 119.7(6) . . ?
C75B C74B C79B 121.1(8) . . ?
C73B C74B C79B 119.2(6) . . ?
C74B C75B C69B 120.8(7) . . ?
C74B C75B H75B 119.6 . . ?
C69B C75B H75B 119.6 . . ?
C77B C76B C73B 117.4(8) . . ?
C77B C76B H76B 121.3 . . ?
C73B C76B H76B 121.3 . . ?
C76B C77B C78B 123.1(7) . . ?
C76B C77B H77B 118.5 . . ?
C78B C77B H77B 118.5 . . ?
C79B C78B C77B 120.0(7) . . ?
C79B C78B H78B 120.0 . . ?
C77B C78B H78B 120.0 . . ?
C78B C79B C74B 120.5(8) . . ?
C78B C79B H79B 119.7 . . ?
C74B C79B H79B 119.7 . . ?
F81 B80 F84 111.8(6) . . ?
F81 B80 F82 111.9(6) . . ?
F84 B80 F82 109.5(5) . . ?
F81 B80 F83 109.7(5) . . ?
F84 B80 F83 106.9(5) . . ?
F82 B80 F83 106.6(6) . . ?
F88 B85 F89 109.7(5) . . ?
F88 B85 F86 110.4(4) . . ?
F89 B85 F86 109.8(4) . . ?
F88 B85 F87 109.2(4) . . ?
F89 B85 F87 109.4(4) . . ?
F86 B85 F87 108.4(5) . . ?
F93 B90 F94 112.2(5) . . ?
F93 B90 F91 108.0(5) . . ?
F94 B90 F91 108.9(5) . . ?
F93 B90 F92 110.4(5) . . ?
F94 B90 F92 110.0(5) . . ?
F91 B90 F92 107.1(5) . . ?
F96 B95 F97 111.5(6) . . ?
F96 B95 F98 109.6(5) . . ?
F97 B95 F98 108.0(5) . . ?
F96 B95 F99 109.1(5) . . ?
F97 B95 F99 111.1(6) . . ?
F98 B95 F99 107.5(6) . . ?
O101 C100 H10C 109.5 . . ?
O101 C100 H10D 109.5 . . ?
H10C C100 H10D 109.5 . . ?
O101 C100 H10E 109.5 . . ?
H10C C100 H10E 109.5 . . ?
H10D C100 H10E 109.5 . . ?
C100 O101 H101 109.5 . . ?
O103 C102 H10F 109.5 . . ?
O103 C102 H10G 109.5 . . ?
H10F C102 H10G 109.5 . . ?
O103 C102 H10H 109.5 . . ?
H10F C102 H10H 109.5 . . ?
H10G C102 H10H 109.5 . . ?
C102 O103 H103 109.5 . . ?
O114 C113 H11F 109.5 . . ?
O114 C113 H11G 109.5 . . ?
H11F C113 H11G 109.5 . . ?
O114 C113 H11H 109.5 . . ?
H11F C113 H11H 109.5 . . ?
H11G C113 H11H 109.5 . . ?
C113 O114 H114 109.5 . . ?
O116 C115 H11I 109.5 . . ?
O116 C115 H11J 109.5 . . ?
H11I C115 H11J 109.5 . . ?
O116 C115 H11K 109.5 . . ?
H11I C115 H11K 109.5 . . ?
H11J C115 H11K 109.5 . . ?
C115 O116 H116 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.932
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.106
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
####################################################################### 
# 
# 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_rk147160
_database_code_depnum_ccdc_archive 'CCDC 1456588'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)di-pyridine solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C5 H5 N)'
_chemical_formula_sum            'C40 H26 Fe N12 S2'
_chemical_formula_weight         794.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   13.3521(4)
_cell_length_b                   16.1985(5)
_cell_length_c                   17.4429(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.287(3)
_cell_angle_gamma                90.00
_cell_volume                     3538.59(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    4513
_cell_measurement_theta_min      3.63
_cell_measurement_theta_max      73.46

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16044
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         73.76
_reflns_number_total             6708
_reflns_number_gt                5140
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The pyridine molecule N50-C55 is disordered over two sites, with refined 
 occupancies of 0.63:0.37. This disorder was modelled without the use of 
 restraints. All non-H atoms except the disordered solvent were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0764P)²+0.7231P] 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         6708
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1290
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22628(3) 0.74521(3) 0.38687(3) 0.02782(14) Uani 1 1 d . . .
N2 N 0.2836(2) 0.74379(18) 0.29750(19) 0.0433(7) Uani 1 1 d . . .
C3 C 0.3181(3) 0.74667(18) 0.2441(2) 0.0368(7) Uani 1 1 d . . .
S4 S 0.36752(8) 0.74996(5) 0.17096(5) 0.0450(2) Uani 1 1 d . . .
N5 N 0.0771(2) 0.75125(15) 0.30957(15) 0.0348(6) Uani 1 1 d . . .
C6 C -0.0106(3) 0.75747(18) 0.26767(18) 0.0334(6) Uani 1 1 d . . .
S7 S -0.13674(7) 0.76626(5) 0.20817(5) 0.0428(2) Uani 1 1 d . . .
C8 C 0.2002(2) 0.90226(19) 0.45323(17) 0.0324(6) Uani 1 1 d . . .
N9 N 0.23669(18) 0.87002(16) 0.39569(14) 0.0330(6) Uani 1 1 d . . .
C10 C 0.2690(3) 0.9224(2) 0.3503(2) 0.0429(8) Uani 1 1 d . . .
H10 H 0.2940 0.9010 0.3095 0.051 Uiso 1 1 calc R . .
C11 C 0.2673(3) 1.0074(2) 0.3605(2) 0.0483(9) Uani 1 1 d . . .
H11 H 0.2921 1.0428 0.3275 0.058 Uiso 1 1 calc R . .
C12 C 0.2302(3) 1.0407(2) 0.4177(2) 0.0455(8) Uani 1 1 d . . .
H12 H 0.2281 1.0988 0.4244 0.055 Uiso 1 1 calc R . .
C13 C 0.1954(2) 0.98678(19) 0.46623(19) 0.0379(7) Uani 1 1 d . . .
C14 C 0.1639(2) 0.84317(18) 0.49952(17) 0.0301(6) Uani 1 1 d . . .
N15 N 0.16991(19) 0.76237(15) 0.48029(15) 0.0304(5) Uani 1 1 d . . .
C16 C 0.1357(2) 0.7064(2) 0.52138(18) 0.0361(7) Uani 1 1 d . . .
H16 H 0.1405 0.6496 0.5094 0.043 Uiso 1 1 calc R . .
C17 C 0.0930(3) 0.7278(2) 0.5814(2) 0.0401(7) Uani 1 1 d . . .
H17 H 0.0688 0.6859 0.6090 0.048 Uiso 1 1 calc R . .
C18 C 0.0859(2) 0.8086(2) 0.60037(19) 0.0395(7) Uani 1 1 d . . .
H18 H 0.0567 0.8238 0.6408 0.047 Uiso 1 1 calc R . .
C19 C 0.1228(2) 0.8691(2) 0.55892(17) 0.0343(7) Uani 1 1 d . . .
C20 C 0.1529(2) 1.0146(2) 0.5287(2) 0.0408(8) Uani 1 1 d . . .
N21 N 0.1484(2) 1.09703(18) 0.54086(19) 0.0520(8) Uani 1 1 d . . .
C22 C 0.1088(3) 1.1189(3) 0.5975(2) 0.0596(11) Uani 1 1 d . . .
H22 H 0.1051 1.1759 0.6088 0.072 Uiso 1 1 calc R . .
C23 C 0.0721(3) 1.0621(3) 0.6414(2) 0.0564(11) Uani 1 1 d . . .
H23 H 0.0441 1.0817 0.6812 0.068 Uiso 1 1 calc R . .
N24 N 0.0749(2) 0.98178(19) 0.62943(17) 0.0471(7) Uani 1 1 d . . .
C25 C 0.1176(2) 0.9575(2) 0.57326(18) 0.0390(7) Uani 1 1 d . . .
C26 C 0.3046(2) 0.58832(17) 0.45727(15) 0.0274(6) Uani 1 1 d . . .
N27 N 0.22315(18) 0.62106(15) 0.39428(13) 0.0297(5) Uani 1 1 d . . .
C28 C 0.1514(2) 0.5684(2) 0.34683(18) 0.0383(7) Uani 1 1 d . . .
H28 H 0.0934 0.5898 0.3024 0.046 Uiso 1 1 calc R . .
C29 C 0.1577(3) 0.4837(2) 0.3596(2) 0.0472(9) Uani 1 1 d . . .
H29 H 0.1059 0.4483 0.3234 0.057 Uiso 1 1 calc R . .
C30 C 0.2391(3) 0.4508(2) 0.4245(2) 0.0395(7) Uani 1 1 d . . .
H30 H 0.2435 0.3929 0.4342 0.047 Uiso 1 1 calc R . .
C31 C 0.3150(2) 0.50421(19) 0.47592(17) 0.0318(6) Uani 1 1 d . . .
C32 C 0.3849(2) 0.64630(17) 0.50290(16) 0.0281(6) Uani 1 1 d . . .
N33 N 0.37215(19) 0.72487(15) 0.47411(14) 0.0298(5) Uani 1 1 d . . .
C34 C 0.4502(2) 0.7786(2) 0.5086(2) 0.0370(7) Uani 1 1 d . . .
H34 H 0.4435 0.8333 0.4877 0.044 Uiso 1 1 calc R . .
C35 C 0.5419(3) 0.75729(19) 0.5747(2) 0.0412(8) Uani 1 1 d . . .
H35 H 0.5970 0.7968 0.5970 0.049 Uiso 1 1 calc R . .
C36 C 0.5519(2) 0.6792(2) 0.60688(18) 0.0364(7) Uani 1 1 d . . .
H36 H 0.6119 0.6648 0.6534 0.044 Uiso 1 1 calc R . .
C37 C 0.4722(2) 0.62102(18) 0.57000(16) 0.0296(6) Uani 1 1 d . . .
C38 C 0.4037(2) 0.47750(19) 0.54749(17) 0.0318(6) Uani 1 1 d . . .
N39 N 0.4101(2) 0.39616(16) 0.56638(16) 0.0381(6) Uani 1 1 d . . .
C40 C 0.4877(3) 0.3752(2) 0.63465(19) 0.0415(7) Uani 1 1 d . . .
H40 H 0.4953 0.3188 0.6506 0.050 Uiso 1 1 calc R . .
C41 C 0.5587(3) 0.4328(2) 0.6840(2) 0.0442(8) Uani 1 1 d . . .
H41 H 0.6116 0.4143 0.7331 0.053 Uiso 1 1 calc R . .
N42 N 0.5558(2) 0.51186(17) 0.66540(16) 0.0402(6) Uani 1 1 d . . .
C43 C 0.4773(2) 0.53486(18) 0.59537(17) 0.0311(6) Uani 1 1 d . . .
N44 N 0.4635(3) 1.0687(2) 0.5848(2) 0.0598(9) Uani 1 1 d . . .
C45 C 0.4309(4) 1.1133(3) 0.6356(3) 0.0694(12) Uani 1 1 d . . .
H45 H 0.4335 1.1718 0.6328 0.083 Uiso 1 1 calc R . .
C46 C 0.3926(4) 1.0771(4) 0.6932(3) 0.0774(16) Uani 1 1 d . . .
H46 H 0.3699 1.1103 0.7291 0.093 Uiso 1 1 calc R . .
C47 C 0.3889(3) 0.9925(4) 0.6964(2) 0.0667(13) Uani 1 1 d . . .
H47 H 0.3628 0.9659 0.7343 0.080 Uiso 1 1 calc R . .
C48 C 0.4228(3) 0.9475(3) 0.6446(2) 0.0534(10) Uani 1 1 d . . .
H48 H 0.4214 0.8889 0.6461 0.064 Uiso 1 1 calc R . .
C49 C 0.4589(3) 0.9868(2) 0.5908(2) 0.0481(8) Uani 1 1 d . . .
H49 H 0.4823 0.9541 0.5550 0.058 Uiso 1 1 calc R . .
N50A N 0.1301(5) 0.5187(4) 0.5926(4) 0.0569(16) Uiso 0.63 1 d P A 1
C51A C 0.2286(6) 0.5190(5) 0.6427(4) 0.051(2) Uiso 0.63 1 d P A 1
H51A H 0.2657 0.5701 0.6519 0.062 Uiso 0.63 1 calc PR A 1
C52A C 0.2840(6) 0.4490(5) 0.6844(4) 0.0471(16) Uiso 0.63 1 d P A 1
H52A H 0.3554 0.4532 0.7214 0.056 Uiso 0.63 1 calc PR A 1
C53A C 0.2314(6) 0.3741(5) 0.6698(5) 0.0576(17) Uiso 0.63 1 d P A 1
H53A H 0.2655 0.3252 0.6963 0.069 Uiso 0.63 1 calc PR A 1
C54A C 0.1269(6) 0.3724(5) 0.6152(5) 0.0679(18) Uiso 0.63 1 d P A 1
H54A H 0.0874 0.3223 0.6034 0.082 Uiso 0.63 1 calc PR A 1
C55A C 0.0822(6) 0.4455(4) 0.5785(4) 0.0564(15) Uiso 0.63 1 d P A 1
H55A H 0.0116 0.4434 0.5400 0.068 Uiso 0.63 1 calc PR A 1
N50B N 0.1512(9) 0.4991(7) 0.5785(6) 0.056(3) Uiso 0.37 1 d P B 2
C51B C 0.2413(12) 0.4938(11) 0.6524(9) 0.059(4) Uiso 0.37 1 d P B 2
H51B H 0.2757 0.5425 0.6792 0.070 Uiso 0.37 1 calc PR B 2
C52B C 0.2781(11) 0.4165(10) 0.6846(8) 0.055(3) Uiso 0.37 1 d P B 2
H52B H 0.3358 0.4122 0.7351 0.066 Uiso 0.37 1 calc PR B 2
C53B C 0.2321(11) 0.3476(10) 0.6444(9) 0.067(3) Uiso 0.37 1 d P B 2
H53B H 0.2601 0.2949 0.6647 0.081 Uiso 0.37 1 calc PR B 2
C54B C 0.1486(11) 0.3533(9) 0.5772(8) 0.070(3) Uiso 0.37 1 d P B 2
H54B H 0.1164 0.3044 0.5494 0.084 Uiso 0.37 1 calc PR B 2
C55B C 0.1071(10) 0.4281(8) 0.5466(8) 0.061(3) Uiso 0.37 1 d P B 2
H55B H 0.0435 0.4293 0.5001 0.074 Uiso 0.37 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.961(3) . ?
Fe1 N5 1.983(3) . ?
Fe1 N27 2.017(3) . ?
Fe1 N9 2.029(3) . ?
Fe1 N15 2.037(3) . ?
Fe1 N33 2.040(2) . ?
N2 C3 1.174(5) . ?
C3 S4 1.628(4) . ?
N5 C6 1.149(4) . ?
C6 S7 1.650(3) . ?
C8 N9 1.363(4) . ?
C8 C13 1.393(4) . ?
C8 C14 1.441(4) . ?
N9 C10 1.330(4) . ?
C10 C11 1.389(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.369(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.402(5) . ?
C12 H12 0.9500 . ?
C13 C20 1.464(5) . ?
C14 N15 1.360(4) . ?
C14 C19 1.395(4) . ?
N15 C16 1.331(4) . ?
C16 C17 1.399(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.361(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.404(5) . ?
C18 H18 0.9500 . ?
C19 C25 1.459(5) . ?
C20 N21 1.356(4) . ?
C20 C25 1.391(5) . ?
N21 C22 1.321(6) . ?
C22 C23 1.389(7) . ?
C22 H22 0.9500 . ?
C23 N24 1.320(5) . ?
C23 H23 0.9500 . ?
N24 C25 1.352(5) . ?
C26 N27 1.358(3) . ?
C26 C31 1.396(4) . ?
C26 C32 1.440(4) . ?
N27 C28 1.335(4) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.376(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.397(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.457(4) . ?
C32 N33 1.357(4) . ?
C32 C37 1.396(4) . ?
N33 C34 1.331(4) . ?
C34 C35 1.404(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.372(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.400(4) . ?
C36 H36 0.9500 . ?
C37 C43 1.459(4) . ?
C38 N39 1.354(4) . ?
C38 C43 1.400(4) . ?
N39 C40 1.324(4) . ?
C40 C41 1.395(5) . ?
C40 H40 0.9500 . ?
C41 N42 1.318(4) . ?
C41 H41 0.9500 . ?
N42 C43 1.357(4) . ?
N44 C45 1.327(6) . ?
N44 C49 1.334(5) . ?
C45 C46 1.405(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.374(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.355(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.354(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
N50A C51A 1.303(9) . ?
N50A C55A 1.327(10) . ?
C51A C52A 1.411(11) . ?
C51A H51A 0.9500 . ?
C52A C53A 1.381(11) . ?
C52A H52A 0.9500 . ?
C53A C54A 1.390(11) . ?
C53A H53A 0.9500 . ?
C54A C55A 1.381(10) . ?
C54A H54A 0.9500 . ?
C55A H55A 0.9500 . ?
N50B C55B 1.324(16) . ?
N50B C51B 1.428(18) . ?
C51B C52B 1.39(2) . ?
C51B H51B 0.9500 . ?
C52B C53B 1.35(2) . ?
C52B H52B 0.9500 . ?
C53B C54B 1.311(18) . ?
C53B H53B 0.9500 . ?
C54B C55B 1.361(18) . ?
C54B H54B 0.9500 . ?
C55B H55B 0.9500 . ?

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 92.13(11) . . ?
N2 Fe1 N27 93.53(11) . . ?
N5 Fe1 N27 93.12(10) . . ?
N2 Fe1 N9 92.10(11) . . ?
N5 Fe1 N9 91.64(10) . . ?
N27 Fe1 N9 172.48(10) . . ?
N2 Fe1 N15 172.76(11) . . ?
N5 Fe1 N15 88.54(10) . . ?
N27 Fe1 N15 93.63(10) . . ?
N9 Fe1 N15 80.68(10) . . ?
N2 Fe1 N33 93.21(11) . . ?
N5 Fe1 N33 171.56(10) . . ?
N27 Fe1 N33 80.02(10) . . ?
N9 Fe1 N33 94.70(10) . . ?
N15 Fe1 N33 86.99(10) . . ?
C3 N2 Fe1 177.0(3) . . ?
N2 C3 S4 179.1(3) . . ?
C6 N5 Fe1 176.4(3) . . ?
N5 C6 S7 179.5(3) . . ?
N9 C8 C13 123.0(3) . . ?
N9 C8 C14 115.7(3) . . ?
C13 C8 C14 121.2(3) . . ?
C10 N9 C8 117.8(3) . . ?
C10 N9 Fe1 128.2(2) . . ?
C8 N9 Fe1 113.9(2) . . ?
N9 C10 C11 122.2(4) . . ?
N9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C8 C13 C12 118.0(3) . . ?
C8 C13 C20 118.4(3) . . ?
C12 C13 C20 123.6(3) . . ?
N15 C14 C19 123.0(3) . . ?
N15 C14 C8 116.1(3) . . ?
C19 C14 C8 120.8(3) . . ?
C16 N15 C14 117.5(3) . . ?
C16 N15 Fe1 128.9(2) . . ?
C14 N15 Fe1 113.5(2) . . ?
N15 C16 C17 122.6(3) . . ?
N15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 118.7(3) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C14 C19 C18 118.1(3) . . ?
C14 C19 C25 118.5(3) . . ?
C18 C19 C25 123.4(3) . . ?
N21 C20 C25 121.8(3) . . ?
N21 C20 C13 117.9(3) . . ?
C25 C20 C13 120.3(3) . . ?
C22 N21 C20 115.5(4) . . ?
N21 C22 C23 123.0(4) . . ?
N21 C22 H22 118.5 . . ?
C23 C22 H22 118.5 . . ?
N24 C23 C22 122.0(4) . . ?
N24 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C23 N24 C25 116.3(4) . . ?
N24 C25 C20 121.3(3) . . ?
N24 C25 C19 117.8(3) . . ?
C20 C25 C19 120.8(3) . . ?
N27 C26 C31 123.8(3) . . ?
N27 C26 C32 115.3(2) . . ?
C31 C26 C32 120.9(2) . . ?
C28 N27 C26 117.0(3) . . ?
C28 N27 Fe1 128.6(2) . . ?
C26 N27 Fe1 114.38(19) . . ?
N27 C28 C29 122.8(3) . . ?
N27 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 120.1(3) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 118.6(3) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C26 C31 C30 117.6(3) . . ?
C26 C31 C38 118.4(3) . . ?
C30 C31 C38 124.0(3) . . ?
N33 C32 C37 123.1(3) . . ?
N33 C32 C26 115.7(2) . . ?
C37 C32 C26 121.1(3) . . ?
C34 N33 C32 117.9(3) . . ?
C34 N33 Fe1 128.8(2) . . ?
C32 N33 Fe1 113.11(19) . . ?
N33 C34 C35 122.2(3) . . ?
N33 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 118.8(3) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C32 C37 C36 117.9(3) . . ?
C32 C37 C43 118.2(3) . . ?
C36 C37 C43 123.8(3) . . ?
N39 C38 C43 121.9(3) . . ?
N39 C38 C31 117.5(3) . . ?
C43 C38 C31 120.5(3) . . ?
C40 N39 C38 115.6(3) . . ?
N39 C40 C41 122.4(3) . . ?
N39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
N42 C41 C40 122.8(3) . . ?
N42 C41 H41 118.6 . . ?
C40 C41 H41 118.6 . . ?
C41 N42 C43 115.9(3) . . ?
N42 C43 C38 121.2(3) . . ?
N42 C43 C37 118.5(3) . . ?
C38 C43 C37 120.3(2) . . ?
C45 N44 C49 117.0(4) . . ?
N44 C45 C46 122.4(5) . . ?
N44 C45 H45 118.8 . . ?
C46 C45 H45 118.8 . . ?
C47 C46 C45 118.2(4) . . ?
C47 C46 H46 120.9 . . ?
C45 C46 H46 120.9 . . ?
C48 C47 C46 119.0(4) . . ?
C48 C47 H47 120.5 . . ?
C46 C47 H47 120.5 . . ?
C49 C48 C47 119.4(4) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.3 . . ?
N44 C49 C48 124.0(4) . . ?
N44 C49 H49 118.0 . . ?
C48 C49 H49 118.0 . . ?
C51A N50A C55A 115.9(7) . . ?
N50A C51A C52A 124.8(8) . . ?
N50A C51A H51A 117.6 . . ?
C52A C51A H51A 117.6 . . ?
C53A C52A C51A 117.9(6) . . ?
C53A C52A H52A 121.0 . . ?
C51A C52A H52A 121.0 . . ?
C52A C53A C54A 118.1(7) . . ?
C52A C53A H53A 121.0 . . ?
C54A C53A H53A 121.0 . . ?
C55A C54A C53A 118.0(8) . . ?
C55A C54A H54A 121.0 . . ?
C53A C54A H54A 121.0 . . ?
N50A C55A C54A 125.3(7) . . ?
N50A C55A H55A 117.4 . . ?
C54A C55A H55A 117.4 . . ?
C55B N50B C51B 116.1(12) . . ?
C52B C51B N50B 119.2(13) . . ?
C52B C51B H51B 120.4 . . ?
N50B C51B H51B 120.4 . . ?
C53B C52B C51B 120.1(12) . . ?
C53B C52B H52B 120.0 . . ?
C51B C52B H52B 120.0 . . ?
C54B C53B C52B 120.0(14) . . ?
C54B C53B H53B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C53B C54B C55B 121.2(14) . . ?
C53B C54B H54B 119.4 . . ?
C55B C54B H54B 119.4 . . ?
N50B C55B C54B 123.1(12) . . ?
N50B C55B H55B 118.4 . . ?
C54B C55B H55B 118.4 . . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.953
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.068
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'pyridine/diethyl ether'
####################################################################### 
# 
# 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_rk147200
_database_code_depnum_ccdc_archive 'CCDC 1456589'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)di-pyridine solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C5 H5 N)'
_chemical_formula_sum            'C40 H26 Fe N12 S2'
_chemical_formula_weight         794.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   13.4396(3)
_cell_length_b                   16.2494(3)
_cell_length_c                   17.5932(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.306(2)
_cell_angle_gamma                90.00
_cell_volume                     3603.32(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4505
_cell_measurement_theta_min      4.44
_cell_measurement_theta_max      73.50

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15490
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.82
_diffrn_reflns_theta_max         73.57
_reflns_number_total             6836
_reflns_number_gt                5079
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The pyridine molecule N50-C55 is disordered over two sites, with refined 
 occupancies of 0.63:0.37. This disorder was modelled without the use of 
 restraints. All non-H atoms except the disordered solvent were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0686P)²+0.8365P] 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         6836
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1389
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22430(3) 0.74625(3) 0.38221(3) 0.03772(13) Uani 1 1 d . . .
N2 N 0.2855(2) 0.74867(18) 0.29066(19) 0.0594(7) Uani 1 1 d . . .
C3 C 0.3202(2) 0.74999(18) 0.2395(2) 0.0472(7) Uani 1 1 d . . .
S4 S 0.37079(8) 0.75056(5) 0.16840(6) 0.0597(2) Uani 1 1 d . . .
N5 N 0.0702(2) 0.74836(15) 0.30470(16) 0.0488(6) Uani 1 1 d . . .
C6 C -0.0174(3) 0.75464(17) 0.26366(18) 0.0443(7) Uani 1 1 d . . .
S7 S -0.14188(7) 0.76392(6) 0.20545(5) 0.0576(2) Uani 1 1 d . . .
C8 C 0.1996(2) 0.90637(18) 0.45374(17) 0.0418(6) Uani 1 1 d . . .
N9 N 0.23623(18) 0.87535(16) 0.39659(15) 0.0451(6) Uani 1 1 d . . .
C10 C 0.2689(3) 0.9283(2) 0.3525(2) 0.0564(8) Uani 1 1 d . . .
H10 H 0.2939 0.9075 0.3120 0.068 Uiso 1 1 calc R . .
C11 C 0.2676(3) 1.0132(2) 0.3635(2) 0.0641(10) Uani 1 1 d . . .
H11 H 0.2925 1.0490 0.3314 0.077 Uiso 1 1 calc R . .
C12 C 0.2306(3) 1.0448(2) 0.4203(2) 0.0622(10) Uani 1 1 d . . .
H12 H 0.2286 1.1026 0.4276 0.075 Uiso 1 1 calc R . .
C13 C 0.1955(2) 0.99051(18) 0.4680(2) 0.0496(8) Uani 1 1 d . . .
C14 C 0.1630(2) 0.84748(17) 0.49979(17) 0.0406(6) Uani 1 1 d . . .
N15 N 0.16774(18) 0.76650(14) 0.48053(13) 0.0382(5) Uani 1 1 d . . .
C16 C 0.1327(2) 0.71118(19) 0.52081(17) 0.0453(7) Uani 1 1 d . . .
H16 H 0.1371 0.6546 0.5088 0.054 Uiso 1 1 calc R . .
C17 C 0.0897(3) 0.7323(2) 0.5801(2) 0.0526(8) Uani 1 1 d . . .
H17 H 0.0644 0.6908 0.6069 0.063 Uiso 1 1 calc R . .
C18 C 0.0846(2) 0.8130(2) 0.59877(18) 0.0514(7) Uani 1 1 d . . .
H18 H 0.0559 0.8285 0.6390 0.062 Uiso 1 1 calc R . .
C19 C 0.1220(2) 0.87315(19) 0.55839(17) 0.0453(7) Uani 1 1 d . . .
C20 C 0.1534(2) 1.0183(2) 0.5295(2) 0.0532(8) Uani 1 1 d . . .
N21 N 0.1495(2) 1.10025(18) 0.5428(2) 0.0686(9) Uani 1 1 d . . .
C22 C 0.1101(3) 1.1220(3) 0.5987(3) 0.0783(13) Uani 1 1 d . . .
H22 H 0.1072 1.1788 0.6103 0.094 Uiso 1 1 calc R . .
C23 C 0.0727(3) 1.0653(3) 0.6414(2) 0.0714(11) Uani 1 1 d . . .
H23 H 0.0443 1.0848 0.6805 0.086 Uiso 1 1 calc R . .
N24 N 0.0751(2) 0.98495(19) 0.62942(17) 0.0618(8) Uani 1 1 d . . .
C25 C 0.1173(2) 0.9612(2) 0.57331(19) 0.0503(8) Uani 1 1 d . . .
C26 C 0.3068(2) 0.58614(16) 0.45819(15) 0.0360(6) Uani 1 1 d . . .
N27 N 0.22516(18) 0.61729(14) 0.39496(13) 0.0405(5) Uani 1 1 d . . .
C28 C 0.1538(2) 0.5642(2) 0.34887(18) 0.0521(8) Uani 1 1 d . . .
H28 H 0.0957 0.5850 0.3049 0.063 Uiso 1 1 calc R . .
C29 C 0.1609(3) 0.4801(2) 0.3625(2) 0.0591(9) Uani 1 1 d . . .
H29 H 0.1098 0.4444 0.3269 0.071 Uiso 1 1 calc R . .
C30 C 0.2418(3) 0.44816(19) 0.4273(2) 0.0525(8) Uani 1 1 d . . .
H30 H 0.2464 0.3907 0.4379 0.063 Uiso 1 1 calc R . .
C31 C 0.3172(2) 0.50248(17) 0.47720(16) 0.0403(6) Uani 1 1 d . . .
C32 C 0.3867(2) 0.64439(16) 0.50356(15) 0.0349(5) Uani 1 1 d . . .
N33 N 0.37472(18) 0.72295(14) 0.47508(14) 0.0391(5) Uani 1 1 d . . .
C34 C 0.4512(2) 0.7764(2) 0.5113(2) 0.0500(7) Uani 1 1 d . . .
H34 H 0.4447 0.8313 0.4916 0.060 Uiso 1 1 calc R . .
C35 C 0.5415(3) 0.75484(19) 0.5777(2) 0.0534(8) Uani 1 1 d . . .
H35 H 0.5954 0.7944 0.6012 0.064 Uiso 1 1 calc R . .
C36 C 0.5514(2) 0.67728(19) 0.60827(18) 0.0469(7) Uani 1 1 d . . .
H36 H 0.6108 0.6627 0.6544 0.056 Uiso 1 1 calc R . .
C37 C 0.4724(2) 0.61883(17) 0.57071(15) 0.0374(6) Uani 1 1 d . . .
C38 C 0.4049(2) 0.47564(17) 0.54873(17) 0.0405(6) Uani 1 1 d . . .
N39 N 0.4118(2) 0.39513(15) 0.56803(16) 0.0486(6) Uani 1 1 d . . .
C40 C 0.4885(3) 0.3742(2) 0.6355(2) 0.0550(8) Uani 1 1 d . . .
H40 H 0.4961 0.3180 0.6513 0.066 Uiso 1 1 calc R . .
C41 C 0.5590(3) 0.4317(2) 0.6843(2) 0.0576(8) Uani 1 1 d . . .
H41 H 0.6115 0.4134 0.7330 0.069 Uiso 1 1 calc R . .
N42 N 0.5559(2) 0.51081(16) 0.66549(15) 0.0516(6) Uani 1 1 d . . .
C43 C 0.4784(2) 0.53347(17) 0.59596(16) 0.0398(6) Uani 1 1 d . . .
N44 N 0.4635(3) 1.0680(2) 0.5839(2) 0.0802(10) Uani 1 1 d . . .
C45 C 0.4343(4) 1.1131(3) 0.6354(4) 0.0931(15) Uani 1 1 d . . .
H45 H 0.4392 1.1713 0.6329 0.112 Uiso 1 1 calc R . .
C46 C 0.3965(4) 1.0785(5) 0.6933(3) 0.1035(19) Uani 1 1 d . . .
H46 H 0.3752 1.1120 0.7293 0.124 Uiso 1 1 calc R . .
C47 C 0.3918(3) 0.9947(4) 0.6956(3) 0.0860(14) Uani 1 1 d . . .
H47 H 0.3666 0.9686 0.7338 0.103 Uiso 1 1 calc R . .
C48 C 0.4224(3) 0.9491(3) 0.6446(2) 0.0690(10) Uani 1 1 d . . .
H48 H 0.4195 0.8908 0.6464 0.083 Uiso 1 1 calc R . .
C49 C 0.4574(3) 0.9869(2) 0.5906(2) 0.0638(9) Uani 1 1 d . . .
H49 H 0.4792 0.9533 0.5550 0.077 Uiso 1 1 calc R . .
N50A N 0.1284(5) 0.5208(4) 0.5935(4) 0.0714(17) Uiso 0.63 1 d P A 1
C51A C 0.2272(6) 0.5228(5) 0.6415(4) 0.0600(18) Uiso 0.63 1 d P A 1
H51A H 0.2637 0.5739 0.6485 0.072 Uiso 0.63 1 calc PR A 1
C52A C 0.2827(6) 0.4548(5) 0.6834(4) 0.0599(17) Uiso 0.63 1 d P A 1
H52A H 0.3537 0.4601 0.7196 0.072 Uiso 0.63 1 calc PR A 1
C53A C 0.2322(7) 0.3798(6) 0.6709(5) 0.0745(19) Uiso 0.63 1 d P A 1
H53A H 0.2677 0.3318 0.6978 0.089 Uiso 0.63 1 calc PR A 1
C54A C 0.1271(6) 0.3763(5) 0.6176(4) 0.0766(18) Uiso 0.63 1 d P A 1
H54A H 0.0885 0.3261 0.6077 0.092 Uiso 0.63 1 calc PR A 1
C55A C 0.0813(6) 0.4487(4) 0.5796(4) 0.0682(16) Uiso 0.63 1 d P A 1
H55A H 0.0114 0.4459 0.5410 0.082 Uiso 0.63 1 calc PR A 1
N50B N 0.1500(8) 0.5045(6) 0.5768(6) 0.064(3) Uiso 0.37 1 d P B 2
C51B C 0.2403(12) 0.4961(10) 0.6524(9) 0.075(4) Uiso 0.37 1 d P B 2
H51B H 0.2734 0.5445 0.6800 0.091 Uiso 0.37 1 calc PR B 2
C52B C 0.2787(11) 0.4217(10) 0.6846(8) 0.068(3) Uiso 0.37 1 d P B 2
H52B H 0.3372 0.4185 0.7340 0.081 Uiso 0.37 1 calc PR B 2
C53B C 0.2321(12) 0.3513(10) 0.6452(9) 0.086(4) Uiso 0.37 1 d P B 2
H53B H 0.2597 0.2988 0.6658 0.104 Uiso 0.37 1 calc PR B 2
C54B C 0.1509(11) 0.3572(9) 0.5802(8) 0.086(4) Uiso 0.37 1 d P B 2
H54B H 0.1193 0.3082 0.5529 0.104 Uiso 0.37 1 calc PR B 2
C55B C 0.1086(10) 0.4303(8) 0.5490(8) 0.076(3) Uiso 0.37 1 d P B 2
H55B H 0.0443 0.4294 0.5037 0.092 Uiso 0.37 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N5 2.047(3) . ?
Fe1 N2 2.047(3) . ?
Fe1 N27 2.107(2) . ?
Fe1 N9 2.112(3) . ?
Fe1 N15 2.143(2) . ?
Fe1 N33 2.146(2) . ?
N2 C3 1.148(5) . ?
C3 S4 1.619(4) . ?
N5 C6 1.152(4) . ?
C6 S7 1.638(3) . ?
C8 N9 1.360(4) . ?
C8 C13 1.394(4) . ?
C8 C14 1.446(4) . ?
N9 C10 1.331(4) . ?
C10 C11 1.393(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.361(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.407(5) . ?
C12 H12 0.9500 . ?
C13 C20 1.456(5) . ?
C14 N15 1.366(4) . ?
C14 C19 1.391(4) . ?
N15 C16 1.328(4) . ?
C16 C17 1.399(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.360(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.399(5) . ?
C18 H18 0.9500 . ?
C19 C25 1.460(4) . ?
C20 N21 1.356(4) . ?
C20 C25 1.397(5) . ?
N21 C22 1.316(6) . ?
C22 C23 1.389(7) . ?
C22 H22 0.9500 . ?
C23 N24 1.324(5) . ?
C23 H23 0.9500 . ?
N24 C25 1.354(4) . ?
C26 N27 1.360(3) . ?
C26 C31 1.395(4) . ?
C26 C32 1.446(4) . ?
N27 C28 1.335(4) . ?
C28 C29 1.385(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.400(4) . ?
C30 H30 0.9500 . ?
C31 C38 1.461(4) . ?
C32 N33 1.361(3) . ?
C32 C37 1.396(4) . ?
N33 C34 1.328(4) . ?
C34 C35 1.406(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.358(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.407(4) . ?
C36 H36 0.9500 . ?
C37 C43 1.450(4) . ?
C38 N39 1.347(4) . ?
C38 C43 1.407(4) . ?
N39 C40 1.318(4) . ?
C40 C41 1.394(5) . ?
C40 H40 0.9500 . ?
C41 N42 1.324(4) . ?
C41 H41 0.9500 . ?
N42 C43 1.354(4) . ?
N44 C45 1.325(6) . ?
N44 C49 1.329(5) . ?
C45 C46 1.405(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.365(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.334(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.346(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
N50A C51A 1.304(9) . ?
N50A C55A 1.314(9) . ?
C51A C52A 1.392(11) . ?
C51A H51A 0.9500 . ?
C52A C53A 1.374(11) . ?
C52A H52A 0.9500 . ?
C53A C54A 1.400(11) . ?
C53A H53A 0.9500 . ?
C54A C55A 1.387(10) . ?
C54A H54A 0.9500 . ?
C55A H55A 0.9500 . ?
N50B C55B 1.347(16) . ?
N50B C51B 1.464(19) . ?
C51B C52B 1.36(2) . ?
C51B H51B 0.9500 . ?
C52B C53B 1.37(2) . ?
C52B H52B 0.9500 . ?
C53B C54B 1.281(18) . ?
C53B H53B 0.9500 . ?
C54B C55B 1.349(18) . ?
C54B H54B 0.9500 . ?
C55B H55B 0.9500 . ?

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
N5 Fe1 N2 93.73(11) . . ?
N5 Fe1 N27 93.13(9) . . ?
N2 Fe1 N27 96.54(11) . . ?
N5 Fe1 N9 94.61(10) . . ?
N2 Fe1 N9 92.33(11) . . ?
N27 Fe1 N9 167.83(9) . . ?
N5 Fe1 N15 88.57(10) . . ?
N2 Fe1 N15 169.77(11) . . ?
N27 Fe1 N15 93.28(9) . . ?
N9 Fe1 N15 77.54(9) . . ?
N5 Fe1 N33 167.97(10) . . ?
N2 Fe1 N33 94.18(10) . . ?
N27 Fe1 N33 76.98(9) . . ?
N9 Fe1 N33 94.11(9) . . ?
N15 Fe1 N33 85.23(9) . . ?
C3 N2 Fe1 179.7(3) . . ?
N2 C3 S4 178.9(3) . . ?
C6 N5 Fe1 175.2(3) . . ?
N5 C6 S7 179.8(3) . . ?
N9 C8 C13 122.9(3) . . ?
N9 C8 C14 116.7(3) . . ?
C13 C8 C14 120.4(3) . . ?
C10 N9 C8 117.9(3) . . ?
C10 N9 Fe1 126.8(2) . . ?
C8 N9 Fe1 115.13(19) . . ?
N9 C10 C11 122.4(4) . . ?
N9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C8 C13 C12 117.7(3) . . ?
C8 C13 C20 119.2(3) . . ?
C12 C13 C20 123.0(3) . . ?
N15 C14 C19 122.5(3) . . ?
N15 C14 C8 116.4(3) . . ?
C19 C14 C8 121.1(3) . . ?
C16 N15 C14 117.6(3) . . ?
C16 N15 Fe1 128.1(2) . . ?
C14 N15 Fe1 114.12(19) . . ?
N15 C16 C17 123.1(3) . . ?
N15 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C18 C17 C16 119.0(3) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C14 C19 C18 118.1(3) . . ?
C14 C19 C25 118.7(3) . . ?
C18 C19 C25 123.2(3) . . ?
N21 C20 C25 121.0(3) . . ?
N21 C20 C13 118.8(3) . . ?
C25 C20 C13 120.2(3) . . ?
C22 N21 C20 116.2(4) . . ?
N21 C22 C23 122.8(4) . . ?
N21 C22 H22 118.6 . . ?
C23 C22 H22 118.6 . . ?
N24 C23 C22 122.3(4) . . ?
N24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 N24 C25 115.9(4) . . ?
N24 C25 C20 121.8(3) . . ?
N24 C25 C19 117.7(3) . . ?
C20 C25 C19 120.5(3) . . ?
N27 C26 C31 123.0(2) . . ?
N27 C26 C32 116.2(2) . . ?
C31 C26 C32 120.8(2) . . ?
C28 N27 C26 117.5(2) . . ?
C28 N27 Fe1 127.0(2) . . ?
C26 N27 Fe1 115.48(17) . . ?
N27 C28 C29 122.7(3) . . ?
N27 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C28 120.2(3) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 118.3(3) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
C26 C31 C30 118.3(3) . . ?
C26 C31 C38 118.8(2) . . ?
C30 C31 C38 123.0(3) . . ?
N33 C32 C37 123.2(2) . . ?
N33 C32 C26 116.1(2) . . ?
C37 C32 C26 120.6(2) . . ?
C34 N33 C32 117.7(2) . . ?
C34 N33 Fe1 128.1(2) . . ?
C32 N33 Fe1 113.93(17) . . ?
N33 C34 C35 122.4(3) . . ?
N33 C34 H34 118.8 . . ?
C35 C34 H34 118.8 . . ?
C36 C35 C34 119.9(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 119.1(3) . . ?
C35 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?
C32 C37 C36 117.6(3) . . ?
C32 C37 C43 119.1(2) . . ?
C36 C37 C43 123.3(2) . . ?
N39 C38 C43 121.8(3) . . ?
N39 C38 C31 118.1(3) . . ?
C43 C38 C31 120.0(3) . . ?
C40 N39 C38 116.2(3) . . ?
N39 C40 C41 122.2(3) . . ?
N39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
N42 C41 C40 122.8(3) . . ?
N42 C41 H41 118.6 . . ?
C40 C41 H41 118.6 . . ?
C41 N42 C43 115.9(3) . . ?
N42 C43 C38 121.0(3) . . ?
N42 C43 C37 118.7(3) . . ?
C38 C43 C37 120.3(2) . . ?
C45 N44 C49 116.5(4) . . ?
N44 C45 C46 122.9(5) . . ?
N44 C45 H45 118.6 . . ?
C46 C45 H45 118.6 . . ?
C47 C46 C45 116.9(5) . . ?
C47 C46 H46 121.6 . . ?
C45 C46 H46 121.6 . . ?
C48 C47 C46 120.4(5) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 H47 119.8 . . ?
C47 C48 C49 119.2(4) . . ?
C47 C48 H48 120.4 . . ?
C49 C48 H48 120.4 . . ?
N44 C49 C48 124.2(4) . . ?
N44 C49 H49 117.9 . . ?
C48 C49 H49 117.9 . . ?
C51A N50A C55A 117.3(7) . . ?
N50A C51A C52A 124.1(7) . . ?
N50A C51A H51A 117.9 . . ?
C52A C51A H51A 117.9 . . ?
C53A C52A C51A 118.4(7) . . ?
C53A C52A H52A 120.8 . . ?
C51A C52A H52A 120.8 . . ?
C52A C53A C54A 118.1(7) . . ?
C52A C53A H53A 121.0 . . ?
C54A C53A H53A 121.0 . . ?
C55A C54A C53A 117.6(7) . . ?
C55A C54A H54A 121.2 . . ?
C53A C54A H54A 121.2 . . ?
N50A C55A C54A 124.2(7) . . ?
N50A C55A H55A 117.9 . . ?
C54A C55A H55A 117.9 . . ?
C55B N50B C51B 110.7(11) . . ?
C52B C51B N50B 122.5(13) . . ?
C52B C51B H51B 118.7 . . ?
N50B C51B H51B 118.7 . . ?
C51B C52B C53B 119.4(13) . . ?
C51B C52B H52B 120.3 . . ?
C53B C52B H52B 120.3 . . ?
C54B C53B C52B 119.2(14) . . ?
C54B C53B H53B 120.4 . . ?
C52B C53B H53B 120.4 . . ?
C53B C54B C55B 122.5(15) . . ?
C53B C54B H54B 118.8 . . ?
C55B C54B H54B 118.8 . . ?
N50B C55B C54B 125.3(12) . . ?
N50B C55B H55B 117.3 . . ?
C54B C55B H55B 117.3 . . ?

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.052
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'pyridine/diethyl ether'
####################################################################### 
# 
# 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_rk147240
_database_code_depnum_ccdc_archive 'CCDC 1456590'
_audit_update_record             
;
2016-02-29 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Bis[1,4,8,9-tetraaza-triphenylene]-di[isothiocyanato]iron(II)di-pyridine solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H16 Fe N10 S2, 2(C5 H5 N)'
_chemical_formula_sum            'C40 H26 Fe N12 S2'
_chemical_formula_weight         794.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   13.4781(9)
_cell_length_b                   16.2943(12)
_cell_length_c                   17.6998(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.310(8)
_cell_angle_gamma                90.00
_cell_volume                     3645.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    3897
_cell_measurement_theta_min      4.44
_cell_measurement_theta_max      73.31

_exptl_crystal_description       fragment
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    4.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16575
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.80
_diffrn_reflns_theta_max         73.58
_reflns_number_total             6870
_reflns_number_gt                4477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 The pyridine molecule N50-C55 is disordered over two sites, with refined 
 occupancies of 0.67:0.33. This disorder was modelled without the use of 
 restraints. All non-H atoms except the disordered solvent were refined 
 anisotropically, while H atoms were placed in calculated positions and 
 refined using a riding model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0928P)²+0.3122P] 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         6870
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1860
_refine_ls_wR_factor_gt          0.1517
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22239(4) 0.74696(4) 0.37992(3) 0.04513(18) Uani 1 1 d . . .
N2 N 0.2855(3) 0.7511(2) 0.2884(2) 0.0661(10) Uani 1 1 d . . .
C3 C 0.3212(3) 0.7518(2) 0.2377(2) 0.0524(9) Uani 1 1 d . . .
S4 S 0.37169(11) 0.75068(7) 0.16763(7) 0.0691(3) Uani 1 1 d . . .
N5 N 0.0657(3) 0.7466(2) 0.3028(2) 0.0567(8) Uani 1 1 d . . .
C6 C -0.0215(3) 0.7528(2) 0.2615(2) 0.0509(9) Uani 1 1 d . . .
S7 S -0.14529(9) 0.76189(8) 0.20432(7) 0.0687(3) Uani 1 1 d . . .
C8 C 0.1989(3) 0.9087(2) 0.4543(2) 0.0500(9) Uani 1 1 d . . .
N9 N 0.2353(2) 0.87910(19) 0.39714(19) 0.0497(7) Uani 1 1 d . . .
C10 C 0.2680(3) 0.9322(3) 0.3538(3) 0.0657(11) Uani 1 1 d . . .
H10 H 0.2929 0.9121 0.3139 0.079 Uiso 1 1 calc R . .
C11 C 0.2667(4) 1.0163(3) 0.3655(3) 0.0720(13) Uani 1 1 d . . .
H11 H 0.2906 1.0521 0.3339 0.086 Uiso 1 1 calc R . .
C12 C 0.2305(4) 1.0473(3) 0.4230(3) 0.0737(13) Uani 1 1 d . . .
H12 H 0.2295 1.1042 0.4313 0.088 Uiso 1 1 calc R . .
C13 C 0.1952(3) 0.9927(3) 0.4691(3) 0.0580(10) Uani 1 1 d . . .
C14 C 0.1616(3) 0.8500(2) 0.4999(2) 0.0463(8) Uani 1 1 d . . .
N15 N 0.1655(2) 0.7692(2) 0.48089(17) 0.0464(7) Uani 1 1 d . . .
C16 C 0.1300(3) 0.7147(3) 0.5206(2) 0.0553(9) Uani 1 1 d . . .
H16 H 0.1334 0.6589 0.5084 0.066 Uiso 1 1 calc R . .
C17 C 0.0875(3) 0.7355(3) 0.5798(3) 0.0618(11) Uani 1 1 d . . .
H17 H 0.0623 0.6948 0.6061 0.074 Uiso 1 1 calc R . .
C18 C 0.0835(3) 0.8162(3) 0.5982(2) 0.0597(10) Uani 1 1 d . . .
H18 H 0.0555 0.8317 0.6379 0.072 Uiso 1 1 calc R . .
C19 C 0.1212(3) 0.8762(3) 0.5581(2) 0.0537(9) Uani 1 1 d . . .
C20 C 0.1532(3) 1.0203(3) 0.5309(3) 0.0614(11) Uani 1 1 d . . .
N21 N 0.1506(3) 1.1022(3) 0.5438(3) 0.0816(13) Uani 1 1 d . . .
C22 C 0.1106(5) 1.1239(4) 0.5998(4) 0.0902(19) Uani 1 1 d . . .
H22 H 0.1071 1.1799 0.6114 0.108 Uiso 1 1 calc R . .
C23 C 0.0738(4) 1.0668(4) 0.6416(3) 0.0891(19) Uani 1 1 d . . .
H23 H 0.0465 1.0858 0.6806 0.107 Uiso 1 1 calc R . .
N24 N 0.0753(3) 0.9871(3) 0.6295(2) 0.0740(11) Uani 1 1 d . . .
C25 C 0.1171(3) 0.9632(3) 0.5737(2) 0.0578(10) Uani 1 1 d . . .
C26 C 0.3078(3) 0.5849(2) 0.45848(19) 0.0426(7) Uani 1 1 d . . .
N27 N 0.2262(2) 0.61537(19) 0.39567(17) 0.0462(7) Uani 1 1 d . . .
C28 C 0.1554(3) 0.5620(3) 0.3502(2) 0.0616(11) Uani 1 1 d . . .
H28 H 0.0980 0.5822 0.3068 0.074 Uiso 1 1 calc R . .
C29 C 0.1625(4) 0.4784(3) 0.3641(3) 0.0714(13) Uani 1 1 d . . .
H29 H 0.1117 0.4429 0.3297 0.086 Uiso 1 1 calc R . .
C30 C 0.2443(3) 0.4471(3) 0.4285(3) 0.0626(11) Uani 1 1 d . . .
H30 H 0.2501 0.3904 0.4389 0.075 Uiso 1 1 calc R . .
C31 C 0.3184(3) 0.5020(2) 0.4779(2) 0.0472(8) Uani 1 1 d . . .
C32 C 0.3870(3) 0.6436(2) 0.5040(2) 0.0418(7) Uani 1 1 d . . .
N33 N 0.3751(2) 0.72207(19) 0.47643(17) 0.0456(7) Uani 1 1 d . . .
C34 C 0.4507(3) 0.7753(3) 0.5135(3) 0.0616(11) Uani 1 1 d . . .
H34 H 0.4444 0.8296 0.4946 0.074 Uiso 1 1 calc R . .
C35 C 0.5399(3) 0.7537(3) 0.5798(3) 0.0632(11) Uani 1 1 d . . .
H35 H 0.5927 0.7928 0.6037 0.076 Uiso 1 1 calc R . .
C36 C 0.5496(3) 0.6763(3) 0.6092(2) 0.0558(10) Uani 1 1 d . . .
H36 H 0.6080 0.6618 0.6548 0.067 Uiso 1 1 calc R . .
C37 C 0.4721(3) 0.6181(2) 0.5713(2) 0.0453(8) Uani 1 1 d . . .
C38 C 0.4055(3) 0.4752(2) 0.5492(2) 0.0478(8) Uani 1 1 d . . .
N39 N 0.4124(3) 0.3947(2) 0.5685(2) 0.0585(8) Uani 1 1 d . . .
C40 C 0.4894(4) 0.3742(3) 0.6355(3) 0.0657(11) Uani 1 1 d . . .
H40 H 0.4974 0.3187 0.6509 0.079 Uiso 1 1 calc R . .
C41 C 0.5592(4) 0.4312(3) 0.6841(3) 0.0682(12) Uani 1 1 d . . .
H41 H 0.6109 0.4132 0.7321 0.082 Uiso 1 1 calc R . .
N42 N 0.5554(3) 0.5104(2) 0.66511(19) 0.0601(9) Uani 1 1 d . . .
C43 C 0.4780(3) 0.5329(2) 0.5960(2) 0.0465(8) Uani 1 1 d . . .
N44 N 0.4644(4) 1.0672(4) 0.5842(3) 0.1000(15) Uani 1 1 d . . .
C45 C 0.4371(6) 1.1133(5) 0.6343(5) 0.112(2) Uani 1 1 d . . .
H45 H 0.4430 1.1705 0.6307 0.134 Uiso 1 1 calc R . .
C46 C 0.3993(6) 1.0817(7) 0.6931(4) 0.127(3) Uani 1 1 d . . .
H46 H 0.3796 1.1159 0.7282 0.153 Uiso 1 1 calc R . .
C47 C 0.3932(5) 0.9973(6) 0.6958(4) 0.107(2) Uani 1 1 d . . .
H47 H 0.3684 0.9722 0.7337 0.128 Uiso 1 1 calc R . .
C48 C 0.4223(4) 0.9510(4) 0.6448(3) 0.0834(16) Uani 1 1 d . . .
H48 H 0.4182 0.8935 0.6467 0.100 Uiso 1 1 calc R . .
C49 C 0.4572(4) 0.9869(4) 0.5914(3) 0.0802(14) Uani 1 1 d . . .
H49 H 0.4780 0.9531 0.5565 0.096 Uiso 1 1 calc R . .
N50A N 0.1281(7) 0.5226(5) 0.5926(5) 0.090(2) Uiso 0.67 1 d P A 1
C51A C 0.2248(8) 0.5236(7) 0.6397(6) 0.080(3) Uiso 0.67 1 d P A 1
H51A H 0.2613 0.5737 0.6456 0.096 Uiso 0.67 1 calc PR A 1
C52A C 0.2797(7) 0.4575(7) 0.6822(6) 0.075(2) Uiso 0.67 1 d P A 1
H52A H 0.3491 0.4637 0.7187 0.090 Uiso 0.67 1 calc PR A 1
C53A C 0.2310(9) 0.3826(8) 0.6702(7) 0.093(3) Uiso 0.67 1 d P A 1
H53A H 0.2665 0.3354 0.6966 0.112 Uiso 0.67 1 calc PR A 1
C54A C 0.1280(8) 0.3787(7) 0.6180(6) 0.098(3) Uiso 0.67 1 d P A 1
H54A H 0.0902 0.3291 0.6097 0.117 Uiso 0.67 1 calc PR A 1
C55A C 0.0819(8) 0.4488(6) 0.5785(6) 0.089(2) Uiso 0.67 1 d P A 1
H55A H 0.0139 0.4447 0.5393 0.107 Uiso 0.67 1 calc PR A 1
N50B N 0.1520(12) 0.5035(10) 0.5749(9) 0.077(4) Uiso 0.33 1 d P B 2
C51B C 0.244(2) 0.5006(18) 0.6535(15) 0.091(7) Uiso 0.33 1 d P B 2
H51B H 0.2768 0.5484 0.6804 0.109 Uiso 0.33 1 calc PR B 2
C52B C 0.2787(16) 0.4189(15) 0.6850(12) 0.079(5) Uiso 0.33 1 d P B 2
H52B H 0.3348 0.4136 0.7344 0.095 Uiso 0.33 1 calc PR B 2
C53B C 0.2327(19) 0.3510(16) 0.6452(14) 0.104(7) Uiso 0.33 1 d P B 2
H53B H 0.2580 0.2988 0.6654 0.125 Uiso 0.33 1 calc PR B 2
C54B C 0.1542(17) 0.3580(14) 0.5796(13) 0.104(6) Uiso 0.33 1 d P B 2
H54B H 0.1229 0.3098 0.5526 0.124 Uiso 0.33 1 calc PR B 2
C55B C 0.1142(16) 0.4296(12) 0.5472(12) 0.088(5) Uiso 0.33 1 d P B 2
H55B H 0.0536 0.4280 0.5004 0.106 Uiso 0.33 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.075(4) . ?
Fe1 N5 2.079(3) . ?
Fe1 N27 2.161(3) . ?
Fe1 N9 2.173(3) . ?
Fe1 N15 2.206(3) . ?
Fe1 N33 2.208(3) . ?
N2 C3 1.155(6) . ?
C3 S4 1.610(4) . ?
N5 C6 1.153(5) . ?
C6 S7 1.630(4) . ?
C8 N9 1.356(5) . ?
C8 C13 1.398(6) . ?
C8 C14 1.449(5) . ?
N9 C10 1.329(5) . ?
C10 C11 1.388(7) . ?
C10 H10 0.9400 . ?
C11 C12 1.367(8) . ?
C11 H11 0.9400 . ?
C12 C13 1.398(7) . ?
C12 H12 0.9400 . ?
C13 C20 1.466(7) . ?
C14 N15 1.365(5) . ?
C14 C19 1.390(5) . ?
N15 C16 1.321(5) . ?
C16 C17 1.398(6) . ?
C16 H16 0.9400 . ?
C17 C18 1.359(6) . ?
C17 H17 0.9400 . ?
C18 C19 1.403(6) . ?
C18 H18 0.9400 . ?
C19 C25 1.448(6) . ?
C20 N21 1.358(6) . ?
C20 C25 1.389(7) . ?
N21 C22 1.330(8) . ?
C22 C23 1.383(9) . ?
C22 H22 0.9400 . ?
C23 N24 1.318(7) . ?
C23 H23 0.9400 . ?
N24 C25 1.353(6) . ?
C26 N27 1.357(4) . ?
C26 C31 1.389(5) . ?
C26 C32 1.452(5) . ?
N27 C28 1.335(5) . ?
C28 C29 1.382(7) . ?
C28 H28 0.9400 . ?
C29 C30 1.380(6) . ?
C29 H29 0.9400 . ?
C30 C31 1.399(5) . ?
C30 H30 0.9400 . ?
C31 C38 1.460(5) . ?
C32 N33 1.358(5) . ?
C32 C37 1.400(5) . ?
N33 C34 1.326(5) . ?
C34 C35 1.402(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.354(6) . ?
C35 H35 0.9400 . ?
C36 C37 1.398(5) . ?
C36 H36 0.9400 . ?
C37 C43 1.449(5) . ?
C38 N39 1.351(5) . ?
C38 C43 1.401(5) . ?
N39 C40 1.319(5) . ?
C40 C41 1.388(7) . ?
C40 H40 0.9400 . ?
C41 N42 1.329(6) . ?
C41 H41 0.9400 . ?
N42 C43 1.354(5) . ?
N44 C45 1.308(9) . ?
N44 C49 1.322(8) . ?
C45 C46 1.405(11) . ?
C45 H45 0.9400 . ?
C46 C47 1.380(11) . ?
C46 H46 0.9400 . ?
C47 C48 1.336(9) . ?
C47 H47 0.9400 . ?
C48 C49 1.329(7) . ?
C48 H48 0.9400 . ?
C49 H49 0.9400 . ?
N50A C51A 1.281(13) . ?
N50A C55A 1.337(12) . ?
C51A C52A 1.373(15) . ?
C51A H51A 0.9400 . ?
C52A C53A 1.368(15) . ?
C52A H52A 0.9400 . ?
C53A C54A 1.375(15) . ?
C53A H53A 0.9400 . ?
C54A C55A 1.371(13) . ?
C54A H54A 0.9400 . ?
C55A H55A 0.9400 . ?
N50B C55B 1.33(2) . ?
N50B C51B 1.51(3) . ?
C51B C52B 1.46(3) . ?
C51B H51B 0.9400 . ?
C52B C53B 1.34(3) . ?
C52B H52B 0.9400 . ?
C53B C54B 1.28(3) . ?
C53B H53B 0.9400 . ?
C54B C55B 1.33(3) . ?
C54B H54B 0.9400 . ?
C55B H55B 0.9400 . ?

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 94.95(14) . . ?
N2 Fe1 N27 97.75(13) . . ?
N5 Fe1 N27 93.15(12) . . ?
N2 Fe1 N9 92.46(14) . . ?
N5 Fe1 N9 96.24(12) . . ?
N27 Fe1 N9 165.48(12) . . ?
N2 Fe1 N15 168.20(14) . . ?
N5 Fe1 N15 88.43(12) . . ?
N27 Fe1 N15 93.34(12) . . ?
N9 Fe1 N15 75.92(12) . . ?
N2 Fe1 N33 94.88(13) . . ?
N5 Fe1 N33 165.64(13) . . ?
N27 Fe1 N33 75.16(11) . . ?
N9 Fe1 N33 93.77(11) . . ?
N15 Fe1 N33 84.04(11) . . ?
C3 N2 Fe1 178.6(3) . . ?
N2 C3 S4 178.7(4) . . ?
C6 N5 Fe1 174.6(3) . . ?
N5 C6 S7 179.1(4) . . ?
N9 C8 C13 122.2(4) . . ?
N9 C8 C14 117.8(3) . . ?
C13 C8 C14 119.9(4) . . ?
C10 N9 C8 118.6(4) . . ?
C10 N9 Fe1 126.2(3) . . ?
C8 N9 Fe1 115.1(2) . . ?
N9 C10 C11 122.1(5) . . ?
N9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 118.8(5) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C8 C13 C12 118.2(4) . . ?
C8 C13 C20 119.2(4) . . ?
C12 C13 C20 122.6(4) . . ?
N15 C14 C19 122.5(4) . . ?
N15 C14 C8 116.7(3) . . ?
C19 C14 C8 120.8(4) . . ?
C16 N15 C14 117.7(3) . . ?
C16 N15 Fe1 127.8(3) . . ?
C14 N15 Fe1 114.4(2) . . ?
N15 C16 C17 123.6(4) . . ?
N15 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C18 C17 C16 118.3(4) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C14 C19 C18 117.7(4) . . ?
C14 C19 C25 119.5(4) . . ?
C18 C19 C25 122.8(4) . . ?
N21 C20 C25 122.2(4) . . ?
N21 C20 C13 117.8(5) . . ?
C25 C20 C13 120.0(4) . . ?
C22 N21 C20 115.3(5) . . ?
N21 C22 C23 122.2(5) . . ?
N21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
N24 C23 C22 123.2(5) . . ?
N24 C23 H23 118.4 . . ?
C22 C23 H23 118.4 . . ?
C23 N24 C25 115.9(5) . . ?
N24 C25 C20 121.2(4) . . ?
N24 C25 C19 118.2(4) . . ?
C20 C25 C19 120.5(4) . . ?
N27 C26 C31 122.9(3) . . ?
N27 C26 C32 116.4(3) . . ?
C31 C26 C32 120.7(3) . . ?
C28 N27 C26 117.5(3) . . ?
C28 N27 Fe1 126.1(3) . . ?
C26 N27 Fe1 116.4(2) . . ?
N27 C28 C29 122.9(4) . . ?
N27 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 119.9(4) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 118.2(4) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 H30 120.9 . . ?
C26 C31 C30 118.5(3) . . ?
C26 C31 C38 119.2(3) . . ?
C30 C31 C38 122.3(4) . . ?
N33 C32 C37 123.0(3) . . ?
N33 C32 C26 116.6(3) . . ?
C37 C32 C26 120.3(3) . . ?
C34 N33 C32 117.6(3) . . ?
C34 N33 Fe1 127.8(3) . . ?
C32 N33 Fe1 114.4(2) . . ?
N33 C34 C35 122.6(4) . . ?
N33 C34 H34 118.7 . . ?
C35 C34 H34 118.7 . . ?
C36 C35 C34 119.8(4) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 119.3(4) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C36 C37 C32 117.6(3) . . ?
C36 C37 C43 123.5(3) . . ?
C32 C37 C43 118.9(3) . . ?
N39 C38 C43 122.0(3) . . ?
N39 C38 C31 118.2(3) . . ?
C43 C38 C31 119.8(3) . . ?
C40 N39 C38 115.9(4) . . ?
N39 C40 C41 122.7(4) . . ?
N39 C40 H40 118.6 . . ?
C41 C40 H40 118.6 . . ?
N42 C41 C40 122.3(4) . . ?
N42 C41 H41 118.8 . . ?
C40 C41 H41 118.8 . . ?
C41 N42 C43 116.2(4) . . ?
N42 C43 C38 120.8(4) . . ?
N42 C43 C37 118.5(3) . . ?
C38 C43 C37 120.7(3) . . ?
C45 N44 C49 117.0(6) . . ?
N44 C45 C46 123.5(7) . . ?
N44 C45 H45 118.2 . . ?
C46 C45 H45 118.2 . . ?
C47 C46 C45 115.6(7) . . ?
C47 C46 H46 122.2 . . ?
C45 C46 H46 122.2 . . ?
C48 C47 C46 120.2(7) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C49 C48 C47 119.4(6) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.3 . . ?
N44 C49 C48 124.1(6) . . ?
N44 C49 H49 117.9 . . ?
C48 C49 H49 117.9 . . ?
C51A N50A C55A 115.8(9) . . ?
N50A C51A C52A 125.4(10) . . ?
N50A C51A H51A 117.3 . . ?
C52A C51A H51A 117.3 . . ?
C53A C52A C51A 118.5(9) . . ?
C53A C52A H52A 120.8 . . ?
C51A C52A H52A 120.8 . . ?
C52A C53A C54A 117.6(10) . . ?
C52A C53A H53A 121.2 . . ?
C54A C53A H53A 121.2 . . ?
C55A C54A C53A 118.5(10) . . ?
C55A C54A H54A 120.7 . . ?
C53A C54A H54A 120.7 . . ?
N50A C55A C54A 123.7(9) . . ?
N50A C55A H55A 118.2 . . ?
C54A C55A H55A 118.2 . . ?
C55B N50B C51B 113.4(17) . . ?
C52B C51B N50B 115.7(19) . . ?
C52B C51B H51B 122.1 . . ?
N50B C51B H51B 122.1 . . ?
C53B C52B C51B 121.6(19) . . ?
C53B C52B H52B 119.2 . . ?
C51B C52B H52B 119.2 . . ?
C54B C53B C52B 119(2) . . ?
C54B C53B H53B 120.3 . . ?
C52B C53B H53B 120.3 . . ?
C53B C54B C55B 124(2) . . ?
C53B C54B H54B 118.1 . . ?
C55B C54B H54B 118.1 . . ?
C54B C55B N50B 126.1(19) . . ?
C54B C55B H55B 117.0 . . ?
N50B C55B H55B 117.0 . . ?

_diffrn_measured_fraction_theta_max 0.934
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.946
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.066
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'pyridine/diethyl ether'
