# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_1_193_K
_database_code_depnum_ccdc_archive 'CCDC 1422607'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Fe K N8'
_chemical_formula_weight         315.21

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   13.702(3)
_cell_length_b                   7.9004(18)
_cell_length_c                   13.703(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.642(6)
_cell_angle_gamma                90.00
_cell_volume                     1405.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    1616
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6113
_exptl_absorpt_correction_T_max  0.7719
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7552
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1602
_reflns_number_gt                1545
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0349P)²+1.2137P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1602
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
K1 K 0.5000 0.71245(7) 0.2500 0.02232(14) Uani 1 2 d S . .
Fe1 Fe 0.7500 0.2500 0.5000 0.01590(13) Uani 1 2 d S . .
N3 N 0.65570(11) -0.0868(2) 0.39607(12) 0.0300(3) Uani 1 1 d . . .
N2 N 0.93890(10) 0.1795(2) 0.42967(11) 0.0267(3) Uani 1 1 d . . .
C1 C 0.68553(12) 0.3765(2) 0.37468(12) 0.0242(3) Uani 1 1 d . . .
C3 C 0.68905(11) 0.0395(2) 0.43409(11) 0.0202(3) Uani 1 1 d . . .
N1 N 0.64901(13) 0.4524(2) 0.30066(12) 0.0392(4) Uani 1 1 d . . .
C2 C 0.86816(12) 0.2060(2) 0.45528(12) 0.0199(3) Uani 1 1 d . . .
H4A H 0.316(2) 0.274(3) 0.404(2) 0.039(7) Uiso 1 1 d . . .
H4B H 0.4134(19) 0.317(3) 0.449(2) 0.045(7) Uiso 1 1 d . . .
H4D H 0.408(2) 0.045(4) 0.411(2) 0.081(10) Uiso 1 1 d . . .
H4E H 0.463(2) 0.153(4) 0.343(2) 0.068(9) Uiso 1 1 d . . .
N4 N 0.37014(13) 0.2872(2) 0.39558(15) 0.0280(3) Uani 1 1 d . . .
C4 C 0.40279(19) 0.1288(3) 0.35819(18) 0.0386(5) Uani 1 1 d . . .
H4C H 0.3661(17) 0.369(3) 0.3504(19) 0.041(7) Uiso 1 1 d . . .
H4F H 0.351(2) 0.099(3) 0.298(2) 0.057(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 N1 2.8224(17) 2_655 ?
K1 N1 2.8224(17) . ?
K1 N2 2.8544(15) 4_655 ?
K1 N2 2.8544(15) 3_455 ?
K1 N3 2.8885(15) 1_565 ?
K1 N3 2.8885(15) 2_665 ?
Fe1 C2 1.9370(16) 7_656 ?
Fe1 C2 1.9370(16) . ?
Fe1 C1 1.9384(17) . ?
Fe1 C1 1.9384(17) 7_656 ?
Fe1 C3 1.9483(17) 7_656 ?
Fe1 C3 1.9483(17) . ?
N3 C3 1.151(2) . ?
N3 K1 2.8885(15) 1_545 ?
N2 C2 1.151(2) . ?
N2 K1 2.8544(15) 3_545 ?
C1 N1 1.147(2) . ?
N4 C4 1.475(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
N1 K1 N1 86.57(8) 2_655 . ?
N1 K1 N2 96.31(5) 2_655 4_655 ?
N1 K1 N2 75.94(5) . 4_655 ?
N1 K1 N2 75.94(5) 2_655 3_455 ?
N1 K1 N2 96.31(5) . 3_455 ?
N2 K1 N2 169.53(7) 4_655 3_455 ?
N1 K1 N3 152.40(5) 2_655 1_565 ?
N1 K1 N3 85.03(5) . 1_565 ?
N2 K1 N3 107.01(4) 4_655 1_565 ?
N2 K1 N3 78.92(4) 3_455 1_565 ?
N1 K1 N3 85.03(5) 2_655 2_665 ?
N1 K1 N3 152.40(5) . 2_665 ?
N2 K1 N3 78.92(4) 4_655 2_665 ?
N2 K1 N3 107.01(4) 3_455 2_665 ?
N3 K1 N3 113.38(7) 1_565 2_665 ?
C2 Fe1 C2 180.0 7_656 . ?
C2 Fe1 C1 89.85(7) 7_656 . ?
C2 Fe1 C1 90.15(7) . . ?
C2 Fe1 C1 90.15(7) 7_656 7_656 ?
C2 Fe1 C1 89.85(7) . 7_656 ?
C1 Fe1 C1 180.00(7) . 7_656 ?
C2 Fe1 C3 88.73(7) 7_656 7_656 ?
C2 Fe1 C3 91.27(7) . 7_656 ?
C1 Fe1 C3 88.70(7) . 7_656 ?
C1 Fe1 C3 91.30(7) 7_656 7_656 ?
C2 Fe1 C3 91.27(7) 7_656 . ?
C2 Fe1 C3 88.73(7) . . ?
C1 Fe1 C3 91.30(7) . . ?
C1 Fe1 C3 88.70(7) 7_656 . ?
C3 Fe1 C3 180.000(1) 7_656 . ?
C3 N3 K1 152.68(13) . 1_545 ?
C2 N2 K1 138.97(13) . 3_545 ?
N1 C1 Fe1 178.83(16) . . ?
N3 C3 Fe1 178.11(14) . . ?
C1 N1 K1 132.48(14) . . ?
N2 C2 Fe1 179.35(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Fe1 C1 N1 141(8) 7_656 . . . ?
C2 Fe1 C1 N1 -39(8) . . . . ?
C1 Fe1 C1 N1 -174(100) 7_656 . . . ?
C3 Fe1 C1 N1 52(8) 7_656 . . . ?
C3 Fe1 C1 N1 -128(8) . . . . ?
K1 N3 C3 Fe1 -159(4) 1_545 . . . ?
C2 Fe1 C3 N3 -141(4) 7_656 . . . ?
C2 Fe1 C3 N3 39(4) . . . . ?
C1 Fe1 C3 N3 129(4) . . . . ?
C1 Fe1 C3 N3 -51(4) 7_656 . . . ?
C3 Fe1 C3 N3 -176(100) 7_656 . . . ?
Fe1 C1 N1 K1 -117(8) . . . . ?
N1 K1 N1 C1 -86.4(2) 2_655 . . . ?
N2 K1 N1 C1 176.2(2) 4_655 . . . ?
N2 K1 N1 C1 -11.0(2) 3_455 . . . ?
N3 K1 N1 C1 67.3(2) 1_565 . . . ?
N3 K1 N1 C1 -158.84(16) 2_665 . . . ?
K1 N2 C2 Fe1 -172(100) 3_545 . . . ?
C2 Fe1 C2 N2 -63(100) 7_656 . . . ?
C1 Fe1 C2 N2 162(15) . . . . ?
C1 Fe1 C2 N2 -18(15) 7_656 . . . ?
C3 Fe1 C2 N2 73(15) 7_656 . . . ?
C3 Fe1 C2 N2 -107(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.081
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_443_K
_database_code_depnum_ccdc_archive 'CCDC 1422608'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Fe K N8'
_chemical_formula_weight         315.21

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'
K K 0.2009 0.2494 '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           cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   11.4770(15)
_cell_length_b                   11.4770(15)
_cell_length_c                   11.4770(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1511.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    443(2)
_cell_measurement_reflns_used    257
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      26.9

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6308
_exptl_absorpt_correction_T_max  0.7854
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      443(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3325
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.27
_reflns_number_total             121
_reflns_number_gt                121
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1090P)²+6.8360P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         121
_refine_ls_number_parameters     21
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1863
_refine_ls_wR_factor_gt          0.1863
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_restrained_S_all      1.196
_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 0.5000 0.0000 0.0469(11) Uani 1 48 d S . .
K1 K 0.0000 0.5000 0.5000 0.0572(14) Uani 1 48 d S . .
C1 C -0.0211(13) 0.4789(13) 0.1661(14) 0.055(7) Uani 0.25 2 d SP . .
N2 N 0.311(3) 0.689(3) 0.189(3) 0.20(6) Uani 0.25 6 d SPD . .
H H 0.3619 0.7228 0.1381 0.301 Uiso 0.08 2 d SPR . .
HA H 0.3428 0.6304 0.2279 0.301 Uiso 0.04 1 d PR . .
H2 H 0.2451 0.6726 0.1567 0.301 Uiso 0.04 1 d PR . .
C2 C 0.276(4) 0.776(4) 0.276(4) 0.12(4) Uani 0.25 6 d SPD . .
HB H 0.3182 0.8506 0.2637 0.181 Uiso 0.04 1 d PR . .
HC H 0.1936 0.8065 0.2802 0.181 Uiso 0.08 2 d SPR . .
H2A H 0.2979 0.7522 0.3561 0.181 Uiso 0.04 1 d PR . .
N1 N -0.036(3) 0.464(3) 0.2578(14) 0.13(2) Uani 0.25 2 d SP . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.937(16) 30 ?
Fe1 C1 1.937(16) 126_554 ?
Fe1 C1 1.937(16) 128_554 ?
Fe1 C1 1.937(16) 31_554 ?
Fe1 C1 1.937(16) 32 ?
Fe1 C1 1.937(16) 127 ?
Fe1 C1 1.937(16) 125 ?
Fe1 C1 1.937(16) 82 ?
Fe1 C1 1.937(16) 29_554 ?
Fe1 C1 1.937(16) 2_565 ?
Fe1 C1 1.937(16) 98 ?
Fe1 C1 1.937(16) 180_455 ?
K1 N1 2.839(19) 173_556 ?
K1 N1 2.839(18) 153_565 ?
K1 N1 2.839(18) 77_455 ?
K1 N1 2.839(18) 176_455 ?
K1 N1 2.839(19) 79 ?
K1 N1 2.839(18) 60_565 ?
K1 N1 2.839(18) 59_465 ?
K1 N1 2.839(18) 97_566 ?
K1 N1 2.839(18) 80_556 ?
K1 N1 2.839(18) 175_456 ?
K1 N1 2.839(18) . ?
K1 N1 2.839(18) 57_455 ?
C1 C1 0.48(3) 99_565 ?
C1 C1 0.48(3) 100 ?
C1 C1 0.68(4) 2_565 ?
C1 N1 1.08(2) . ?
C1 N1 1.25(3) 99_565 ?
C1 N1 1.25(3) 100 ?
C1 N1 1.40(4) 2_565 ?
N2 C2 0.71(14) 28_565 ?
N2 C2 1.47(2) 51 ?
N2 C2 1.47(2) 74_565 ?
N2 C2 1.47(2) . ?
C2 N2 0.71(14) 28_565 ?
C2 C2 0.83(13) 51 ?
C2 C2 0.83(13) 74_565 ?
C2 C2 0.83(13) 28_565 ?
C2 N2 1.47(2) 74_565 ?
C2 N2 1.47(2) 51 ?
N1 N1 0.82(7) 99_565 ?
N1 N1 0.82(7) 100 ?
N1 N1 1.15(10) 2_565 ?
N1 C1 1.25(3) 100 ?
N1 C1 1.25(3) 99_565 ?
N1 C1 1.40(4) 2_565 ?

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
C1 Fe1 C1 180.0 30 126_554 ?
C1 Fe1 C1 14.3(9) 30 128_554 ?
C1 Fe1 C1 165.7(9) 126_554 128_554 ?
C1 Fe1 C1 165.7(9) 30 31_554 ?
C1 Fe1 C1 14.3(9) 126_554 31_554 ?
C1 Fe1 C1 159.7(12) 128_554 31_554 ?
C1 Fe1 C1 165.7(9) 30 32 ?
C1 Fe1 C1 14.3(9) 126_554 32 ?
C1 Fe1 C1 180.0 128_554 32 ?
C1 Fe1 C1 20.3(12) 31_554 32 ?
C1 Fe1 C1 14.3(9) 30 127 ?
C1 Fe1 C1 165.7(9) 126_554 127 ?
C1 Fe1 C1 20.3(12) 128_554 127 ?
C1 Fe1 C1 180.0(18) 31_554 127 ?
C1 Fe1 C1 159.7(12) 32 127 ?
C1 Fe1 C1 159.7(12) 30 125 ?
C1 Fe1 C1 20.3(12) 126_554 125 ?
C1 Fe1 C1 165.7(9) 128_554 125 ?
C1 Fe1 C1 14.3(9) 31_554 125 ?
C1 Fe1 C1 14.3(9) 32 125 ?
C1 Fe1 C1 165.7(9) 127 125 ?
C1 Fe1 C1 74.9(10) 30 82 ?
C1 Fe1 C1 105.1(10) 126_554 82 ?
C1 Fe1 C1 76.7(7) 128_554 82 ?
C1 Fe1 C1 90.89(11) 31_554 82 ?
C1 Fe1 C1 103.3(7) 32 82 ?
C1 Fe1 C1 89.11(11) 127 82 ?
C1 Fe1 C1 89.11(11) 125 82 ?
C1 Fe1 C1 20.3(12) 30 29_554 ?
C1 Fe1 C1 159.7(12) 126_554 29_554 ?
C1 Fe1 C1 14.3(9) 128_554 29_554 ?
C1 Fe1 C1 165.7(9) 31_554 29_554 ?
C1 Fe1 C1 165.7(9) 32 29_554 ?
C1 Fe1 C1 14.3(9) 127 29_554 ?
C1 Fe1 C1 180.0(9) 125 29_554 ?
C1 Fe1 C1 90.89(11) 82 29_554 ?
C1 Fe1 C1 74.9(10) 30 2_565 ?
C1 Fe1 C1 105.1(10) 126_554 2_565 ?
C1 Fe1 C1 89.11(11) 128_554 2_565 ?
C1 Fe1 C1 103.3(7) 31_554 2_565 ?
C1 Fe1 C1 90.89(11) 32 2_565 ?
C1 Fe1 C1 76.7(7) 127 2_565 ?
C1 Fe1 C1 89.11(11) 125 2_565 ?
C1 Fe1 C1 74.9(10) 82 2_565 ?
C1 Fe1 C1 90.89(11) 29_554 2_565 ?
C1 Fe1 C1 105.1(10) 30 98 ?
C1 Fe1 C1 74.9(10) 126_554 98 ?
C1 Fe1 C1 90.89(11) 128_554 98 ?
C1 Fe1 C1 76.7(7) 31_554 98 ?
C1 Fe1 C1 89.11(11) 32 98 ?
C1 Fe1 C1 103.3(7) 127 98 ?
C1 Fe1 C1 90.89(11) 125 98 ?
C1 Fe1 C1 105.1(10) 82 98 ?
C1 Fe1 C1 89.11(11) 29_554 98 ?
C1 Fe1 C1 180.0(9) 2_565 98 ?
C1 Fe1 C1 89.11(11) 30 180_455 ?
C1 Fe1 C1 90.89(11) 126_554 180_455 ?
C1 Fe1 C1 90.89(11) 128_554 180_455 ?
C1 Fe1 C1 76.7(7) 31_554 180_455 ?
C1 Fe1 C1 89.11(11) 32 180_455 ?
C1 Fe1 C1 103.3(7) 127 180_455 ?
C1 Fe1 C1 74.9(10) 125 180_455 ?
C1 Fe1 C1 14.3(9) 82 180_455 ?
C1 Fe1 C1 105.1(10) 29_554 180_455 ?
C1 Fe1 C1 76.7(7) 2_565 180_455 ?
C1 Fe1 C1 103.3(7) 98 180_455 ?
N1 K1 N1 72.4(15) 173_556 153_565 ?
N1 K1 N1 180.000(1) 173_556 77_455 ?
N1 K1 N1 107.6(15) 153_565 77_455 ?
N1 K1 N1 163.5(13) 173_556 176_455 ?
N1 K1 N1 91.18(19) 153_565 176_455 ?
N1 K1 N1 16.5(13) 77_455 176_455 ?
N1 K1 N1 16.5(13) 173_556 79 ?
N1 K1 N1 74.9(11) 153_565 79 ?
N1 K1 N1 163.5(13) 77_455 79 ?
N1 K1 N1 156.6(19) 176_455 79 ?
N1 K1 N1 74.9(11) 173_556 60_565 ?
N1 K1 N1 16.5(13) 153_565 60_565 ?
N1 K1 N1 105.1(11) 77_455 60_565 ?
N1 K1 N1 88.82(19) 176_455 60_565 ?
N1 K1 N1 72.4(15) 79 60_565 ?
N1 K1 N1 88.82(19) 173_556 59_465 ?
N1 K1 N1 16.5(13) 153_565 59_465 ?
N1 K1 N1 91.18(19) 77_455 59_465 ?
N1 K1 N1 74.9(11) 176_455 59_465 ?
N1 K1 N1 91.2(2) 79 59_465 ?
N1 K1 N1 23.4(19) 60_565 59_465 ?
N1 K1 N1 72.4(15) 173_556 97_566 ?
N1 K1 N1 72.4(15) 153_565 97_566 ?
N1 K1 N1 107.6(15) 77_455 97_566 ?
N1 K1 N1 105.1(11) 176_455 97_566 ?
N1 K1 N1 88.8(2) 79 97_566 ?
N1 K1 N1 88.82(19) 60_565 97_566 ?
N1 K1 N1 74.9(11) 59_465 97_566 ?
N1 K1 N1 16.5(13) 173_556 80_556 ?
N1 K1 N1 88.82(19) 153_565 80_556 ?
N1 K1 N1 163.5(13) 77_455 80_556 ?
N1 K1 N1 180.000(2) 176_455 80_556 ?
N1 K1 N1 23.4(19) 79 80_556 ?
N1 K1 N1 91.2(2) 60_565 80_556 ?
N1 K1 N1 105.1(11) 59_465 80_556 ?
N1 K1 N1 74.9(11) 97_566 80_556 ?
N1 K1 N1 163.5(13) 173_556 175_456 ?
N1 K1 N1 105.1(11) 153_565 175_456 ?
N1 K1 N1 16.5(13) 77_455 175_456 ?
N1 K1 N1 23.4(19) 176_455 175_456 ?
N1 K1 N1 180.000(1) 79 175_456 ?
N1 K1 N1 107.6(15) 60_565 175_456 ?
N1 K1 N1 88.82(19) 59_465 175_456 ?
N1 K1 N1 91.18(19) 97_566 175_456 ?
N1 K1 N1 156.6(19) 80_556 175_456 ?
N1 K1 N1 107.6(15) 173_556 . ?
N1 K1 N1 107.6(15) 153_565 . ?
N1 K1 N1 72.4(15) 77_455 . ?
N1 K1 N1 74.9(11) 176_455 . ?
N1 K1 N1 91.18(19) 79 . ?
N1 K1 N1 91.18(19) 60_565 . ?
N1 K1 N1 105.1(11) 59_465 . ?
N1 K1 N1 180.000(3) 97_566 . ?
N1 K1 N1 105.1(11) 80_556 . ?
N1 K1 N1 88.8(2) 175_456 . ?
N1 K1 N1 107.6(15) 173_556 57_455 ?
N1 K1 N1 180.000(2) 153_565 57_455 ?
N1 K1 N1 72.4(15) 77_455 57_455 ?
N1 K1 N1 88.8(2) 176_455 57_455 ?
N1 K1 N1 105.1(11) 79 57_455 ?
N1 K1 N1 163.5(13) 60_565 57_455 ?
N1 K1 N1 163.5(13) 59_465 57_455 ?
N1 K1 N1 107.6(15) 97_566 57_455 ?
N1 K1 N1 91.18(19) 80_556 57_455 ?
N1 K1 N1 74.9(11) 175_456 57_455 ?
N1 K1 N1 72.4(15) . 57_455 ?
C1 C1 C1 90.00(2) 99_565 100 ?
C1 C1 C1 45.000(7) 99_565 2_565 ?
C1 C1 C1 45.000(3) 100 2_565 ?
C1 C1 N1 99(2) 99_565 . ?
C1 C1 N1 99(2) 100 . ?
C1 C1 N1 103(3) 2_565 . ?
C1 C1 N1 58.6(14) 99_565 99_565 ?
C1 C1 N1 97.6(17) 100 99_565 ?
C1 C1 N1 74.1(10) 2_565 99_565 ?
N1 C1 N1 40(3) . 99_565 ?
C1 C1 N1 97.6(17) 99_565 100 ?
C1 C1 N1 58.6(14) 100 100 ?
C1 C1 N1 74.1(10) 2_565 100 ?
N1 C1 N1 40(3) . 100 ?
N1 C1 N1 55(4) 99_565 100 ?
C1 C1 N1 62.3(10) 99_565 2_565 ?
C1 C1 N1 62.3(10) 100 2_565 ?
C1 C1 N1 48.9(17) 2_565 2_565 ?
N1 C1 N1 54(4) . 2_565 ?
N1 C1 N1 35(2) 99_565 2_565 ?
N1 C1 N1 35(2) 100 2_565 ?
C1 C1 Fe1 82.8(4) 99_565 . ?
C1 C1 Fe1 82.8(4) 100 . ?
C1 C1 Fe1 79.8(6) 2_565 . ?
N1 C1 Fe1 178(3) . . ?
N1 C1 Fe1 141.4(16) 99_565 . ?
N1 C1 Fe1 141.4(16) 100 . ?
N1 C1 Fe1 129(2) 2_565 . ?
C2 N2 C2 19(3) 28_565 51 ?
C2 N2 C2 19(3) 28_565 74_565 ?
C2 N2 C2 33(5) 51 74_565 ?
C2 N2 C2 19(3) 28_565 . ?
C2 N2 C2 33(5) 51 . ?
C2 N2 C2 33(5) 74_565 . ?
N2 C2 C2 144.74(4) 28_565 51 ?
N2 C2 C2 144.74(4) 28_565 74_565 ?
C2 C2 C2 60.000(6) 51 74_565 ?
N2 C2 C2 144.74(4) 28_565 28_565 ?
C2 C2 C2 60.000(12) 51 28_565 ?
C2 C2 C2 60.000(11) 74_565 28_565 ?
N2 C2 N2 129(3) 28_565 74_565 ?
C2 C2 N2 16(3) 51 74_565 ?
C2 C2 N2 74(3) 74_565 74_565 ?
C2 C2 N2 74(3) 28_565 74_565 ?
N2 C2 N2 129(3) 28_565 51 ?
C2 C2 N2 74(3) 51 51 ?
C2 C2 N2 16(3) 74_565 51 ?
C2 C2 N2 74(3) 28_565 51 ?
N2 C2 N2 85(5) 74_565 51 ?
N2 C2 N2 129(3) 28_565 . ?
C2 C2 N2 74(3) 51 . ?
C2 C2 N2 74(3) 74_565 . ?
C2 C2 N2 16(3) 28_565 . ?
N2 C2 N2 85(5) 74_565 . ?
N2 C2 N2 85(5) 51 . ?
N1 N1 N1 90.000(16) 99_565 100 ?
N1 N1 C1 81(2) 99_565 . ?
N1 N1 C1 81(2) 100 . ?
N1 N1 N1 45.000(13) 99_565 2_565 ?
N1 N1 N1 45.000(4) 100 2_565 ?
C1 N1 N1 77(3) . 2_565 ?
N1 N1 C1 82.4(17) 99_565 100 ?
N1 N1 C1 58.6(14) 100 100 ?
C1 N1 C1 22.5(16) . 100 ?
N1 N1 C1 62(2) 2_565 100 ?
N1 N1 C1 58.6(14) 99_565 99_565 ?
N1 N1 C1 82.4(17) 100 99_565 ?
C1 N1 C1 22.5(16) . 99_565 ?
N1 N1 C1 62(2) 2_565 99_565 ?
C1 N1 C1 32(2) 100 99_565 ?
N1 N1 C1 62.3(10) 99_565 2_565 ?
N1 N1 C1 62.3(10) 100 2_565 ?
C1 N1 C1 29(2) . 2_565 ?
N1 N1 C1 48.9(17) 2_565 2_565 ?
C1 N1 C1 20.1(13) 100 2_565 ?
C1 N1 C1 20.1(13) 99_565 2_565 ?
N1 N1 K1 81.7(7) 99_565 . ?
N1 N1 K1 81.7(7) 100 . ?
C1 N1 K1 156(4) . . ?
N1 N1 K1 78.3(10) 2_565 . ?
C1 N1 K1 137(3) 100 . ?
C1 N1 K1 137(3) 99_565 . ?
C1 N1 K1 127(3) 2_565 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Fe1 C1 C1 82.9(4) 30 . . 99_565 ?
C1 Fe1 C1 C1 -97.1(4) 126_554 . . 99_565 ?
C1 Fe1 C1 C1 84.5(2) 128_554 . . 99_565 ?
C1 Fe1 C1 C1 -82.9(4) 31_554 . . 99_565 ?
C1 Fe1 C1 C1 -95.5(2) 32 . . 99_565 ?
C1 Fe1 C1 C1 97.1(4) 127 . . 99_565 ?
C1 Fe1 C1 C1 -80.9(7) 125 . . 99_565 ?
C1 Fe1 C1 C1 8.0(5) 82 . . 99_565 ?
C1 Fe1 C1 C1 99.1(7) 29_554 . . 99_565 ?
C1 Fe1 C1 C1 45.45(6) 2_565 . . 99_565 ?
C1 Fe1 C1 C1 -134.55(5) 98 . . 99_565 ?
C1 Fe1 C1 C1 -6.2(3) 180_455 . . 99_565 ?
C1 Fe1 C1 C1 -8.0(5) 30 . . 100 ?
C1 Fe1 C1 C1 172.0(5) 126_554 . . 100 ?
C1 Fe1 C1 C1 -6.4(4) 128_554 . . 100 ?
C1 Fe1 C1 C1 -173.8(3) 31_554 . . 100 ?
C1 Fe1 C1 C1 173.6(4) 32 . . 100 ?
C1 Fe1 C1 C1 6.2(3) 127 . . 100 ?
C1 Fe1 C1 C1 -171.8(6) 125 . . 100 ?
C1 Fe1 C1 C1 -82.9(4) 82 . . 100 ?
C1 Fe1 C1 C1 8.2(6) 29_554 . . 100 ?
C1 Fe1 C1 C1 -45.45(5) 2_565 . . 100 ?
C1 Fe1 C1 C1 134.55(5) 98 . . 100 ?
C1 Fe1 C1 C1 -97.1(4) 180_455 . . 100 ?
C1 Fe1 C1 C1 37.4(5) 30 . . 2_565 ?
C1 Fe1 C1 C1 -142.6(5) 126_554 . . 2_565 ?
C1 Fe1 C1 C1 39.0(3) 128_554 . . 2_565 ?
C1 Fe1 C1 C1 -128.3(4) 31_554 . . 2_565 ?
C1 Fe1 C1 C1 -141.0(3) 32 . . 2_565 ?
C1 Fe1 C1 C1 51.7(4) 127 . . 2_565 ?
C1 Fe1 C1 C1 -126.3(6) 125 . . 2_565 ?
C1 Fe1 C1 C1 -37.4(5) 82 . . 2_565 ?
C1 Fe1 C1 C1 53.7(6) 29_554 . . 2_565 ?
C1 Fe1 C1 C1 180.000(8) 98 . . 2_565 ?
C1 Fe1 C1 C1 -51.7(4) 180_455 . . 2_565 ?
C1 Fe1 C1 N1 -142.6(5) 30 . . . ?
C1 Fe1 C1 N1 37.4(5) 126_554 . . . ?
C1 Fe1 C1 N1 -141.0(3) 128_554 . . . ?
C1 Fe1 C1 N1 51.7(4) 31_554 . . . ?
C1 Fe1 C1 N1 39.0(3) 32 . . . ?
C1 Fe1 C1 N1 -128.3(4) 127 . . . ?
C1 Fe1 C1 N1 53.7(6) 125 . . . ?
C1 Fe1 C1 N1 142.6(5) 82 . . . ?
C1 Fe1 C1 N1 -126.3(6) 29_554 . . . ?
C1 Fe1 C1 N1 180(4) 2_565 . . . ?
C1 Fe1 C1 N1 0.00(11) 98 . . . ?
C1 Fe1 C1 N1 128.3(4) 180_455 . . . ?
C1 Fe1 C1 N1 85(3) 30 . . 99_565 ?
C1 Fe1 C1 N1 -95(3) 126_554 . . 99_565 ?
C1 Fe1 C1 N1 87(3) 128_554 . . 99_565 ?
C1 Fe1 C1 N1 -81(3) 31_554 . . 99_565 ?
C1 Fe1 C1 N1 -93(3) 32 . . 99_565 ?
C1 Fe1 C1 N1 99(3) 127 . . 99_565 ?
C1 Fe1 C1 N1 -78(3) 125 . . 99_565 ?
C1 Fe1 C1 N1 10(3) 82 . . 99_565 ?
C1 Fe1 C1 N1 102(3) 29_554 . . 99_565 ?
C1 Fe1 C1 N1 48(3) 2_565 . . 99_565 ?
C1 Fe1 C1 N1 -132(3) 98 . . 99_565 ?
C1 Fe1 C1 N1 -4(3) 180_455 . . 99_565 ?
C1 Fe1 C1 N1 -10(3) 30 . . 100 ?
C1 Fe1 C1 N1 170(3) 126_554 . . 100 ?
C1 Fe1 C1 N1 -9(3) 128_554 . . 100 ?
C1 Fe1 C1 N1 -176(3) 31_554 . . 100 ?
C1 Fe1 C1 N1 171(3) 32 . . 100 ?
C1 Fe1 C1 N1 4(3) 127 . . 100 ?
C1 Fe1 C1 N1 -174(4) 125 . . 100 ?
C1 Fe1 C1 N1 -85(3) 82 . . 100 ?
C1 Fe1 C1 N1 6(4) 29_554 . . 100 ?
C1 Fe1 C1 N1 -48(3) 2_565 . . 100 ?
C1 Fe1 C1 N1 132(3) 98 . . 100 ?
C1 Fe1 C1 N1 -99(3) 180_455 . . 100 ?
C1 Fe1 C1 N1 37.4(5) 30 . . 2_565 ?
C1 Fe1 C1 N1 -142.6(5) 126_554 . . 2_565 ?
C1 Fe1 C1 N1 39.0(3) 128_554 . . 2_565 ?
C1 Fe1 C1 N1 -128.3(4) 31_554 . . 2_565 ?
C1 Fe1 C1 N1 -141.0(3) 32 . . 2_565 ?
C1 Fe1 C1 N1 51.7(4) 127 . . 2_565 ?
C1 Fe1 C1 N1 -126.3(6) 125 . . 2_565 ?
C1 Fe1 C1 N1 -37.4(5) 82 . . 2_565 ?
C1 Fe1 C1 N1 53.7(6) 29_554 . . 2_565 ?
C1 Fe1 C1 N1 0.000(5) 2_565 . . 2_565 ?
C1 Fe1 C1 N1 180.000(5) 98 . . 2_565 ?
C1 Fe1 C1 N1 -51.7(4) 180_455 . . 2_565 ?
C2 N2 C2 N2 180.0 28_565 . . 28_565 ?
C2 N2 C2 N2 -148.6(5) 51 . . 28_565 ?
C2 N2 C2 N2 148.6(5) 74_565 . . 28_565 ?
C2 N2 C2 C2 -31.4(5) 28_565 . . 51 ?
C2 N2 C2 C2 -62.9(10) 74_565 . . 51 ?
C2 N2 C2 C2 31.4(5) 28_565 . . 74_565 ?
C2 N2 C2 C2 62.9(10) 51 . . 74_565 ?
C2 N2 C2 C2 31.4(5) 51 . . 28_565 ?
C2 N2 C2 C2 -31.4(5) 74_565 . . 28_565 ?
C2 N2 C2 N2 -43(2) 28_565 . . 74_565 ?
C2 N2 C2 N2 -11(2) 51 . . 74_565 ?
C2 N2 C2 N2 -74.2(15) 74_565 . . 74_565 ?
C2 N2 C2 N2 43(2) 28_565 . . 51 ?
C2 N2 C2 N2 74.2(15) 51 . . 51 ?
C2 N2 C2 N2 11(2) 74_565 . . 51 ?
C1 C1 N1 N1 0.000(15) 99_565 . . 99_565 ?
C1 C1 N1 N1 91.4(6) 100 . . 99_565 ?
C1 C1 N1 N1 45.7(3) 2_565 . . 99_565 ?
N1 C1 N1 N1 91.4(6) 100 . . 99_565 ?
N1 C1 N1 N1 45.7(3) 2_565 . . 99_565 ?
Fe1 C1 N1 N1 -134.3(4) . . . 99_565 ?
C1 C1 N1 N1 -91.4(6) 99_565 . . 100 ?
C1 C1 N1 N1 0.000(5) 100 . . 100 ?
C1 C1 N1 N1 -45.7(3) 2_565 . . 100 ?
N1 C1 N1 N1 -91.4(6) 99_565 . . 100 ?
N1 C1 N1 N1 -45.7(3) 2_565 . . 100 ?
Fe1 C1 N1 N1 134.3(2) . . . 100 ?
C1 C1 N1 N1 -45.7(3) 99_565 . . 2_565 ?
C1 C1 N1 N1 45.7(3) 100 . . 2_565 ?
C1 C1 N1 N1 0.000(5) 2_565 . . 2_565 ?
N1 C1 N1 N1 -45.7(3) 99_565 . . 2_565 ?
N1 C1 N1 N1 45.7(3) 100 . . 2_565 ?
Fe1 C1 N1 N1 180(4) . . . 2_565 ?
C1 C1 N1 C1 -91.4(6) 99_565 . . 100 ?
C1 C1 N1 C1 -45.7(3) 2_565 . . 100 ?
N1 C1 N1 C1 -91.4(6) 99_565 . . 100 ?
N1 C1 N1 C1 0.000(9) 100 . . 100 ?
N1 C1 N1 C1 -45.7(3) 2_565 . . 100 ?
Fe1 C1 N1 C1 134.3(2) . . . 100 ?
C1 C1 N1 C1 91.4(6) 100 . . 99_565 ?
C1 C1 N1 C1 45.7(3) 2_565 . . 99_565 ?
N1 C1 N1 C1 0.00(3) 99_565 . . 99_565 ?
N1 C1 N1 C1 91.4(6) 100 . . 99_565 ?
N1 C1 N1 C1 45.7(3) 2_565 . . 99_565 ?
Fe1 C1 N1 C1 -134.3(4) . . . 99_565 ?
C1 C1 N1 C1 -45.7(3) 99_565 . . 2_565 ?
C1 C1 N1 C1 45.7(3) 100 . . 2_565 ?
N1 C1 N1 C1 -45.7(3) 99_565 . . 2_565 ?
N1 C1 N1 C1 45.7(3) 100 . . 2_565 ?
N1 C1 N1 C1 0.000(7) 2_565 . . 2_565 ?
Fe1 C1 N1 C1 180(4) . . . 2_565 ?
C1 C1 N1 K1 -45.7(3) 99_565 . . . ?
C1 C1 N1 K1 45.7(3) 100 . . . ?
C1 C1 N1 K1 0.000(12) 2_565 . . . ?
N1 C1 N1 K1 -45.7(3) 99_565 . . . ?
N1 C1 N1 K1 45.7(3) 100 . . . ?
N1 C1 N1 K1 0.000(7) 2_565 . . . ?
Fe1 C1 N1 K1 180(4) . . . . ?
N1 K1 N1 N1 -83.9(3) 173_556 . . 99_565 ?
N1 K1 N1 N1 -7.3(5) 153_565 . . 99_565 ?
N1 K1 N1 N1 96.1(3) 77_455 . . 99_565 ?
N1 K1 N1 N1 79.1(11) 176_455 . . 99_565 ?
N1 K1 N1 N1 -81.8(6) 79 . . 99_565 ?
N1 K1 N1 N1 -9.4(9) 60_565 . . 99_565 ?
N1 K1 N1 N1 9.7(9) 59_465 . . 99_565 ?
N1 K1 N1 N1 -11(100) 97_566 . . 99_565 ?
N1 K1 N1 N1 -100.9(11) 80_556 . . 99_565 ?
N1 K1 N1 N1 98.2(6) 175_456 . . 99_565 ?
N1 K1 N1 N1 172.7(5) 57_455 . . 99_565 ?
N1 K1 N1 N1 7.3(5) 173_556 . . 100 ?
N1 K1 N1 N1 83.9(3) 153_565 . . 100 ?
N1 K1 N1 N1 -172.7(5) 77_455 . . 100 ?
N1 K1 N1 N1 170.3(9) 176_455 . . 100 ?
N1 K1 N1 N1 9.4(8) 79 . . 100 ?
N1 K1 N1 N1 81.8(6) 60_565 . . 100 ?
N1 K1 N1 N1 100.9(11) 59_465 . . 100 ?
N1 K1 N1 N1 80(91) 97_566 . . 100 ?
N1 K1 N1 N1 -9.7(9) 80_556 . . 100 ?
N1 K1 N1 N1 -170.6(8) 175_456 . . 100 ?
N1 K1 N1 N1 -96.1(3) 57_455 . . 100 ?
N1 K1 N1 C1 -38.3(4) 173_556 . . . ?
N1 K1 N1 C1 38.3(4) 153_565 . . . ?
N1 K1 N1 C1 141.7(4) 77_455 . . . ?
N1 K1 N1 C1 124.7(10) 176_455 . . . ?
N1 K1 N1 C1 -36.2(7) 79 . . . ?
N1 K1 N1 C1 36.2(7) 60_565 . . . ?
N1 K1 N1 C1 55.3(10) 59_465 . . . ?
N1 K1 N1 C1 35(100) 97_566 . . . ?
N1 K1 N1 C1 -55.3(10) 80_556 . . . ?
N1 K1 N1 C1 143.8(7) 175_456 . . . ?
N1 K1 N1 C1 -141.7(4) 57_455 . . . ?
N1 K1 N1 N1 -38.3(4) 173_556 . . 2_565 ?
N1 K1 N1 N1 38.3(4) 153_565 . . 2_565 ?
N1 K1 N1 N1 141.7(4) 77_455 . . 2_565 ?
N1 K1 N1 N1 124.7(10) 176_455 . . 2_565 ?
N1 K1 N1 N1 -36.2(7) 79 . . 2_565 ?
N1 K1 N1 N1 36.2(8) 60_565 . . 2_565 ?
N1 K1 N1 N1 55.3(10) 59_465 . . 2_565 ?
N1 K1 N1 N1 35(100) 97_566 . . 2_565 ?
N1 K1 N1 N1 -55.3(10) 80_556 . . 2_565 ?
N1 K1 N1 N1 143.8(7) 175_456 . . 2_565 ?
N1 K1 N1 N1 -141.7(4) 57_455 . . 2_565 ?
N1 K1 N1 C1 -14.6(19) 173_556 . . 100 ?
N1 K1 N1 C1 62(3) 153_565 . . 100 ?
N1 K1 N1 C1 165.4(19) 77_455 . . 100 ?
N1 K1 N1 C1 148(3) 176_455 . . 100 ?
N1 K1 N1 C1 -12.5(17) 79 . . 100 ?
N1 K1 N1 C1 60(3) 60_565 . . 100 ?
N1 K1 N1 C1 79.0(15) 59_465 . . 100 ?
N1 K1 N1 C1 58(100) 97_566 . . 100 ?
N1 K1 N1 C1 -32(3) 80_556 . . 100 ?
N1 K1 N1 C1 167.5(17) 175_456 . . 100 ?
N1 K1 N1 C1 -118(3) 57_455 . . 100 ?
N1 K1 N1 C1 -62(3) 173_556 . . 99_565 ?
N1 K1 N1 C1 14.6(19) 153_565 . . 99_565 ?
N1 K1 N1 C1 118(3) 77_455 . . 99_565 ?
N1 K1 N1 C1 101.0(15) 176_455 . . 99_565 ?
N1 K1 N1 C1 -60(3) 79 . . 99_565 ?
N1 K1 N1 C1 12.5(17) 60_565 . . 99_565 ?
N1 K1 N1 C1 32(3) 59_465 . . 99_565 ?
N1 K1 N1 C1 11(100) 97_566 . . 99_565 ?
N1 K1 N1 C1 -79.0(15) 80_556 . . 99_565 ?
N1 K1 N1 C1 120(3) 175_456 . . 99_565 ?
N1 K1 N1 C1 -165.4(19) 57_455 . . 99_565 ?
N1 K1 N1 C1 -38.3(4) 173_556 . . 2_565 ?
N1 K1 N1 C1 38.3(4) 153_565 . . 2_565 ?
N1 K1 N1 C1 141.7(4) 77_455 . . 2_565 ?
N1 K1 N1 C1 124.7(10) 176_455 . . 2_565 ?
N1 K1 N1 C1 -36.2(7) 79 . . 2_565 ?
N1 K1 N1 C1 36.2(7) 60_565 . . 2_565 ?
N1 K1 N1 C1 55.3(10) 59_465 . . 2_565 ?
N1 K1 N1 C1 35(100) 97_566 . . 2_565 ?
N1 K1 N1 C1 -55.3(10) 80_556 . . 2_565 ?
N1 K1 N1 C1 143.8(7) 175_456 . . 2_565 ?
N1 K1 N1 C1 -141.7(4) 57_455 . . 2_565 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.27
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.111
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2_165_K
_database_code_depnum_ccdc_archive 'CCDC 1422609'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 Fe K N8'
_chemical_formula_weight         343.26

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4/mnc

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

_cell_length_a                   8.2769(4)
_cell_length_b                   8.2769(4)
_cell_length_c                   11.6742(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     799.77(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    165(2)
_cell_measurement_reflns_used    4450
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             354
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7137
_exptl_absorpt_correction_T_max  0.7137
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      165(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'R-AXIS SPIDER'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4156
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.99
_reflns_number_total             419
_reflns_number_gt                397
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.038(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         419
_refine_ls_number_parameters     34
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1776
_refine_ls_wR_factor_gt          0.1761
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.067
_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
C1 C 0.7966(9) 0.1240(8) 0.0000 0.0267(15) Uani 1 2 d S . .
C2 C 1.0000 0.0000 0.1659(9) 0.032(2) Uani 1 4 d S . .
N1 N 0.6797(9) 0.1933(9) 0.0000 0.054(2) Uani 1 2 d S . .
N2 N 1.0000 0.0000 0.2636(8) 0.050(3) Uani 1 4 d S . .
K1 K 0.5000 0.5000 0.0000 0.0265(9) Uani 1 8 d S . .
Fe1 Fe 1.0000 0.0000 0.0000 0.0216(8) Uani 1 8 d S . .
C3 C 0.3940(8) 0.1060(8) 0.2500 0.066(3) Uani 1 2 d SD . .
H3A H 0.3817 0.2221 0.2500 0.099 Uiso 0.50 1 d PR A -1
H3B H 0.3437 0.0625 0.1829 0.099 Uiso 0.50 1 d PR A -1
H3C H 0.3437 0.0625 0.3171 0.099 Uiso 0.50 1 d PR A -1
N3 N 0.5656(11) 0.0656(11) 0.2500 0.054(4) Uani 0.50 2 d SPD . .
H3D H 0.6112 0.1113 0.3121 0.065 Uiso 0.25 1 d PR B -1
H3E H 0.6112 0.1113 0.1879 0.065 Uiso 0.25 1 d PR B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.125(10) . ?
C1 Fe1 1.971(7) . ?
C2 N2 1.141(14) . ?
C2 Fe1 1.937(10) . ?
N1 K1 2.942(7) . ?
N2 K1 2.759(10) 5 ?
K1 N2 2.759(10) 13_765 ?
K1 N2 2.759(10) 5_455 ?
K1 N1 2.942(7) 10_565 ?
K1 N1 2.942(7) 2_655 ?
K1 N1 2.942(7) 9_665 ?
Fe1 C2 1.937(10) 9_755 ?
Fe1 C1 1.971(7) 2_645 ?
Fe1 C1 1.971(7) 10_665 ?
Fe1 C1 1.971(7) 9_755 ?
C3 N3 1.459(8) . ?
C3 N3 1.459(8) 3_655 ?
N3 C3 1.459(8) 3_655 ?
N3 N3 1.54(3) 3_655 ?

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
N1 C1 Fe1 179.3(7) . . ?
N2 C2 Fe1 180.0 . . ?
C1 N1 K1 151.0(6) . . ?
C2 N2 K1 180.0 . 5 ?
N2 K1 N2 180.0 13_765 5_455 ?
N2 K1 N1 90.0 13_765 10_565 ?
N2 K1 N1 90.0 5_455 10_565 ?
N2 K1 N1 90.0 13_765 2_655 ?
N2 K1 N1 90.0 5_455 2_655 ?
N1 K1 N1 180.0 10_565 2_655 ?
N2 K1 N1 90.0 13_765 . ?
N2 K1 N1 90.0 5_455 . ?
N1 K1 N1 90.0 10_565 . ?
N1 K1 N1 90.0 2_655 . ?
N2 K1 N1 90.0 13_765 9_665 ?
N2 K1 N1 90.0 5_455 9_665 ?
N1 K1 N1 90.0 10_565 9_665 ?
N1 K1 N1 90.0 2_655 9_665 ?
N1 K1 N1 180.000(1) . 9_665 ?
C2 Fe1 C2 180.0 9_755 . ?
C2 Fe1 C1 90.0 9_755 2_645 ?
C2 Fe1 C1 90.0 . 2_645 ?
C2 Fe1 C1 90.0 9_755 10_665 ?
C2 Fe1 C1 90.0 . 10_665 ?
C1 Fe1 C1 180.0(2) 2_645 10_665 ?
C2 Fe1 C1 90.0 9_755 . ?
C2 Fe1 C1 90.0 . . ?
C1 Fe1 C1 90.0 2_645 . ?
C1 Fe1 C1 90.0 10_665 . ?
C2 Fe1 C1 90.0 9_755 9_755 ?
C2 Fe1 C1 90.0 . 9_755 ?
C1 Fe1 C1 90.0 2_645 9_755 ?
C1 Fe1 C1 90.0 10_665 9_755 ?
C1 Fe1 C1 180.0(4) . 9_755 ?
N3 C3 N3 63.5(11) . 3_655 ?
C3 N3 C3 116.5(11) 3_655 . ?
C3 N3 N3 58.2(5) 3_655 3_655 ?
C3 N3 N3 58.2(5) . 3_655 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 C1 N1 K1 180.0 . . . . ?
Fe1 C2 N2 K1 0.0 . . . 5 ?
C1 N1 K1 N2 90.0 . . . 13_765 ?
C1 N1 K1 N2 -90.0 . . . 5_455 ?
C1 N1 K1 N1 180.0 . . . 10_565 ?
C1 N1 K1 N1 0.0 . . . 2_655 ?
C1 N1 K1 N1 180.0 . . . 9_665 ?
N2 C2 Fe1 C2 0.0 . . . 9_755 ?
N2 C2 Fe1 C1 121(100) . . . 2_645 ?
N2 C2 Fe1 C1 -59(100) . . . 10_665 ?
N2 C2 Fe1 C1 -149(100) . . . . ?
N2 C2 Fe1 C1 31(100) . . . 9_755 ?
N1 C1 Fe1 C2 90.0 . . . 9_755 ?
N1 C1 Fe1 C2 -90.0 . . . . ?
N1 C1 Fe1 C1 0.0 . . . 2_645 ?
N1 C1 Fe1 C1 180.0 . . . 10_665 ?
N1 C1 Fe1 C1 0(100) . . . 9_755 ?
N3 C3 N3 C3 0.0 3_655 . . 3_655 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.164
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2_298_K
_database_code_depnum_ccdc_archive 'CCDC 1422610'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 Fe K N8'
_chemical_formula_weight         343.26

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4/mnc

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

_cell_length_a                   8.3101(13)
_cell_length_b                   8.3101(13)
_cell_length_c                   11.684(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     806.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4004
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             354
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_T_max  0.7156
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'R-AXIS SPIDER'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5089
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.57
_reflns_number_total             498
_reflns_number_gt                403
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.1500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         498
_refine_ls_number_parameters     35
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.064
_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 1.0000 0.0000 0.0000 0.0295(3) Uani 1 8 d S . .
K1 K 0.5000 0.5000 0.0000 0.0372(3) Uani 1 8 d S . .
C1 C 0.8041(3) 0.1278(3) 0.0000 0.0423(5) Uani 1 2 d S . .
N1 N 0.6883(4) 0.2014(4) 0.0000 0.0744(9) Uani 1 2 d S . .
C2 C 1.0000 0.0000 0.1654(3) 0.0497(9) Uani 1 4 d S . .
N2 N 1.0000 0.0000 0.2627(3) 0.088(2) Uani 1 4 d S . .
C3 C 0.3970(4) 0.1030(4) 0.2500 0.117(2) Uani 1 2 d SD . .
H3BD H 0.3788 0.2168 0.2500 0.176 Uiso 0.25 1 d PR A -1
H3BF H 0.3493 0.0561 0.1829 0.176 Uiso 0.25 1 d PR A -1
H3BE H 0.3493 0.0561 0.3171 0.176 Uiso 0.25 1 d PR A -1
H3AA H 0.3299 0.1699 0.2968 0.176 Uiso 0.25 1 d PR A -2
H3AB H 0.4642 0.1690 0.2026 0.176 Uiso 0.25 1 d PR A -2
H3AC H 0.3308 0.0356 0.2026 0.176 Uiso 0.25 1 d PR A -2
N3 N 0.5708(7) 0.0708(7) 0.2500 0.086(4) Uani 0.288(8) 2 d SPD . 1
H H 0.6154 0.1211 0.3126 0.103 Uiso 0.144(4) 1 d PR . -1
HA H 0.6154 0.1211 0.1874 0.103 Uiso 0.144(4) 1 d PR . -1
N3' N 0.5000 0.0000 0.3242(9) 0.086(4) Uani 0.212(8) 2 d SPD . 2
HB H 0.4377 -0.0623 0.3690 0.103 Uiso 0.106(4) 1 d PR . -2
HC H 0.5623 0.0623 0.3690 0.103 Uiso 0.106(4) 1 d PR . -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 C2 1.932(4) 9_755 ?
Fe1 C2 1.932(4) . ?
Fe1 C1 1.944(3) 10_665 ?
Fe1 C1 1.944(3) 9_755 ?
Fe1 C1 1.944(3) 2_645 ?
Fe1 C1 1.944(3) . ?
K1 N2 2.773(4) 13_765 ?
K1 N2 2.773(4) 5_455 ?
K1 N1 2.934(2) 2_655 ?
K1 N1 2.934(2) 10_565 ?
K1 N1 2.934(2) . ?
K1 N1 2.934(2) 9_665 ?
C1 N1 1.140(3) . ?
C2 N2 1.137(5) . ?
N2 K1 2.773(4) 5 ?
C3 N3 1.469(5) 3_655 ?
C3 N3 1.469(5) . ?
C3 N3' 1.489(5) 7_545 ?
C3 N3' 1.489(5) . ?
N3 C3 1.469(5) 3_655 ?
N3 N3 1.665(17) 3_655 ?
N3' C3 1.489(5) 3_655 ?
N3' N3' 1.73(2) 7_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Fe1 C2 180.0 9_755 . ?
C2 Fe1 C1 90.0 9_755 10_665 ?
C2 Fe1 C1 90.0 . 10_665 ?
C2 Fe1 C1 90.0 9_755 9_755 ?
C2 Fe1 C1 90.0 . 9_755 ?
C1 Fe1 C1 90.0 10_665 9_755 ?
C2 Fe1 C1 90.0 9_755 2_645 ?
C2 Fe1 C1 90.0 . 2_645 ?
C1 Fe1 C1 180.00(8) 10_665 2_645 ?
C1 Fe1 C1 90.0 9_755 2_645 ?
C2 Fe1 C1 90.0 9_755 . ?
C2 Fe1 C1 90.0 . . ?
C1 Fe1 C1 90.0 10_665 . ?
C1 Fe1 C1 180.00(8) 9_755 . ?
C1 Fe1 C1 90.0 2_645 . ?
N2 K1 N2 180.0 13_765 5_455 ?
N2 K1 N1 90.0 13_765 2_655 ?
N2 K1 N1 90.0 5_455 2_655 ?
N2 K1 N1 90.0 13_765 10_565 ?
N2 K1 N1 90.0 5_455 10_565 ?
N1 K1 N1 180.0 2_655 10_565 ?
N2 K1 N1 90.0 13_765 . ?
N2 K1 N1 90.0 5_455 . ?
N1 K1 N1 90.0 2_655 . ?
N1 K1 N1 90.0 10_565 . ?
N2 K1 N1 90.0 13_765 9_665 ?
N2 K1 N1 90.0 5_455 9_665 ?
N1 K1 N1 90.0 2_655 9_665 ?
N1 K1 N1 90.0 10_565 9_665 ?
N1 K1 N1 180.0 . 9_665 ?
N1 C1 Fe1 179.3(3) . . ?
C1 N1 K1 154.7(3) . . ?
N2 C2 Fe1 180.0 . . ?
C2 N2 K1 180.0 . 5 ?
N3 C3 N3 69.1(7) 3_655 . ?
N3 C3 N3' 48.0(4) 3_655 7_545 ?
N3 C3 N3' 48.0(4) . 7_545 ?
N3 C3 N3' 48.0(4) 3_655 . ?
N3 C3 N3' 48.0(4) . . ?
N3' C3 N3' 71.2(8) 7_545 . ?
C3 N3 C3 110.9(7) 3_655 . ?
C3 N3 N3 55.5(3) 3_655 3_655 ?
C3 N3 N3 55.5(3) . 3_655 ?
C3 N3' C3 108.8(8) 3_655 . ?
C3 N3' N3' 54.4(4) 3_655 7_545 ?
C3 N3' N3' 54.4(4) . 7_545 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Fe1 C1 N1 90.0 9_755 . . . ?
C2 Fe1 C1 N1 -90.0 . . . . ?
C1 Fe1 C1 N1 180.0 10_665 . . . ?
C1 Fe1 C1 N1 0.0 9_755 . . . ?
C1 Fe1 C1 N1 0.0 2_645 . . . ?
Fe1 C1 N1 K1 180.0 . . . . ?
N2 K1 N1 C1 90.0 13_765 . . . ?
N2 K1 N1 C1 -90.0 5_455 . . . ?
N1 K1 N1 C1 0.0 2_655 . . . ?
N1 K1 N1 C1 180.0 10_565 . . . ?
N1 K1 N1 C1 180.0 9_665 . . . ?
C2 Fe1 C2 N2 0.0 9_755 . . . ?
C1 Fe1 C2 N2 -57(61) 10_665 . . . ?
C1 Fe1 C2 N2 33(61) 9_755 . . . ?
C1 Fe1 C2 N2 123(61) 2_645 . . . ?
C1 Fe1 C2 N2 -147(61) . . . . ?
Fe1 C2 N2 K1 0.0 . . . 5 ?
N3 C3 N3 C3 0.0 3_655 . . 3_655 ?
N3' C3 N3 C3 -51.7(3) 7_545 . . 3_655 ?
N3' C3 N3 C3 51.7(3) . . . 3_655 ?
N3' C3 N3 N3 -51.7(3) 7_545 . . 3_655 ?
N3' C3 N3 N3 51.7(3) . . . 3_655 ?
N3 C3 N3' C3 49.7(3) 3_655 . . 3_655 ?
N3 C3 N3' C3 -49.7(3) . . . 3_655 ?
N3' C3 N3' C3 0.0 7_545 . . 3_655 ?
N3 C3 N3' N3' 49.7(3) 3_655 . . 7_545 ?
N3 C3 N3' N3' -49.7(3) . . . 7_545 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.062
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_113_K
_database_code_depnum_ccdc_archive 'CCDC 1422611'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Fe K N8'
_chemical_formula_weight         371.31

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   15.3805(17)
_cell_length_b                   8.4335(10)
_cell_length_c                   13.8969(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.583(3)
_cell_angle_gamma                90.00
_cell_volume                     1718.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    2346
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.3

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6737
_exptl_absorpt_correction_T_max  0.7975
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13728
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1970
_reflns_number_gt                1947
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0241P)²+2.1965P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1970
_refine_ls_number_parameters     139
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0580
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.003

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
K1 K 0.5000 0.78005(2) 0.2500 0.01627(4) Uani 1 2 d S . .
C1 C 0.68696(3) 0.43878(6) 0.43054(4) 0.01594(12) Uani 1 1 d . . .
N1 N 0.64609(3) 0.54778(6) 0.39134(4) 0.02460(13) Uani 1 1 d . . .
Fe1 Fe 0.7500 0.2500 0.5000 0.01109(2) Uani 1 2 d S . .
C2 C 0.66491(3) 0.12016(6) 0.39849(4) 0.01667(12) Uani 1 1 d . . .
N2 N 0.61384(3) 0.04506(6) 0.33794(4) 0.02952(14) Uani 1 1 d . . .
N3 N 0.88911(3) 0.24558(6) 0.37880(3) 0.02534(14) Uani 1 1 d . . .
C3 C 0.83635(3) 0.24825(6) 0.42231(4) 0.01636(13) Uani 1 1 d . . .
N4B N 0.37797(6) 0.30994(12) 0.40251(7) 0.0191(2) Uani 0.4945(8) 1 d P A 1
H4B H 0.3753 0.3835 0.4514 0.023 Uiso 0.4945(8) 1 calc PR A 1
C6B C 0.28993(7) 0.31798(16) 0.32222(9) 0.02567(15) Uani 0.4945(8) 1 d PU A 1
H6BA H 0.2807 0.4255 0.2942 0.039 Uiso 0.4945(8) 1 calc PR A 1
H6BB H 0.2405 0.2913 0.3504 0.039 Uiso 0.4945(8) 1 calc PR A 1
H6BC H 0.2900 0.2424 0.2687 0.039 Uiso 0.4945(8) 1 calc PR A 1
C5B C 0.45427(7) 0.35413(16) 0.36791(9) 0.0306(3) Uani 0.4945(8) 1 d PU A 1
H5BA H 0.4598 0.2787 0.3164 0.046 Uiso 0.4945(8) 1 calc PR A 1
H5BB H 0.5104 0.3527 0.4249 0.046 Uiso 0.4945(8) 1 calc PR A 1
H5BC H 0.4444 0.4609 0.3389 0.046 Uiso 0.4945(8) 1 calc PR A 1
C4B C 0.39087(9) 0.15570(17) 0.45086(11) 0.0408(4) Uani 0.4945(8) 1 d PU A 1
H4BA H 0.3437 0.1385 0.4839 0.061 Uiso 0.4945(8) 1 calc PR A 1
H4BB H 0.4512 0.1513 0.5013 0.061 Uiso 0.4945(8) 1 calc PR A 1
H4BC H 0.3865 0.0731 0.4000 0.061 Uiso 0.4945(8) 1 calc PR A 1
N4A N 0.38190(6) 0.24885(10) 0.34831(7) 0.0159(2) Uani 0.5055(8) 1 d P A 2
H4A H 0.3791 0.1842 0.2932 0.019 Uiso 0.5055(8) 1 calc PR A 2
C6A C 0.29254(8) 0.32822(17) 0.32689(10) 0.02567(15) Uani 0.5055(8) 1 d PU A 2
H6AA H 0.2923 0.3962 0.3840 0.039 Uiso 0.5055(8) 1 calc PR A 2
H6AB H 0.2444 0.2482 0.3166 0.039 Uiso 0.5055(8) 1 calc PR A 2
H6AC H 0.2816 0.3930 0.2659 0.039 Uiso 0.5055(8) 1 calc PR A 2
C5A C 0.45671(7) 0.36620(15) 0.35603(10) 0.0221(3) Uani 0.5055(8) 1 d PU A 2
H5AA H 0.4437 0.4263 0.2929 0.033 Uiso 0.5055(8) 1 calc PR A 2
H5AB H 0.5148 0.3100 0.3682 0.033 Uiso 0.5055(8) 1 calc PR A 2
H5AC H 0.4606 0.4392 0.4120 0.033 Uiso 0.5055(8) 1 calc PR A 2
C4A C 0.40312(9) 0.14510(18) 0.43793(13) 0.0409(4) Uani 0.5055(8) 1 d PU A 2
H4AA H 0.4083 0.2094 0.4982 0.061 Uiso 0.5055(8) 1 calc PR A 2
H4AB H 0.4609 0.0900 0.4454 0.061 Uiso 0.5055(8) 1 calc PR A 2
H4AC H 0.3542 0.0670 0.4297 0.061 Uiso 0.5055(8) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 N3 2.8357(6) 3_455 ?
K1 N3 2.8357(6) 4_655 ?
K1 N2 2.8743(6) 1_565 ?
K1 N2 2.8743(6) 2_665 ?
K1 N1 3.1744(5) 2_655 ?
K1 N1 3.1744(5) . ?
C1 N1 1.1533(7) . ?
C1 Fe1 1.9599(5) . ?
Fe1 C2 1.9458(5) . ?
Fe1 C2 1.9458(5) 7_656 ?
Fe1 C3 1.9484(6) 7_656 ?
Fe1 C3 1.9484(6) . ?
Fe1 C1 1.9599(5) 7_656 ?
C2 N2 1.1519(7) . ?
N2 K1 2.8743(6) 1_545 ?
N3 C3 1.1494(8) . ?
N3 K1 2.8357(6) 3_545 ?
N4B C5B 1.4451(16) . ?
N4B C4B 1.4499(18) . ?
N4B C6B 1.4732(13) . ?
N4A C4A 1.4756(18) . ?
N4A C6A 1.4760(15) . ?
N4A C5A 1.4967(15) . ?

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
N3 K1 N3 168.23(2) 3_455 4_655 ?
N3 K1 N2 102.510(17) 3_455 1_565 ?
N3 K1 N2 86.722(17) 4_655 1_565 ?
N3 K1 N2 86.722(17) 3_455 2_665 ?
N3 K1 N2 102.510(17) 4_655 2_665 ?
N2 K1 N2 77.92(2) 1_565 2_665 ?
N3 K1 N1 83.054(16) 3_455 2_655 ?
N3 K1 N1 89.680(16) 4_655 2_655 ?
N2 K1 N1 165.762(14) 1_565 2_655 ?
N2 K1 N1 89.445(15) 2_665 2_655 ?
N3 K1 N1 89.680(16) 3_455 . ?
N3 K1 N1 83.054(16) 4_655 . ?
N2 K1 N1 89.445(15) 1_565 . ?
N2 K1 N1 165.762(14) 2_665 . ?
N1 K1 N1 103.80(2) 2_655 . ?
N1 C1 Fe1 176.47(5) . . ?
C1 N1 K1 165.25(4) . . ?
C2 Fe1 C2 180.000(1) . 7_656 ?
C2 Fe1 C3 89.10(2) . 7_656 ?
C2 Fe1 C3 90.90(2) 7_656 7_656 ?
C2 Fe1 C3 90.90(2) . . ?
C2 Fe1 C3 89.10(2) 7_656 . ?
C3 Fe1 C3 180.0 7_656 . ?
C2 Fe1 C1 88.61(2) . . ?
C2 Fe1 C1 91.39(2) 7_656 . ?
C3 Fe1 C1 87.03(2) 7_656 . ?
C3 Fe1 C1 92.97(2) . . ?
C2 Fe1 C1 91.39(2) . 7_656 ?
C2 Fe1 C1 88.61(2) 7_656 7_656 ?
C3 Fe1 C1 92.97(2) 7_656 7_656 ?
C3 Fe1 C1 87.03(2) . 7_656 ?
C1 Fe1 C1 180.00(3) . 7_656 ?
N2 C2 Fe1 179.09(5) . . ?
C2 N2 K1 158.67(5) . 1_545 ?
C3 N3 K1 170.02(4) . 3_545 ?
N3 C3 Fe1 178.09(4) . . ?
C5B N4B C4B 111.99(10) . . ?
C5B N4B C6B 112.90(9) . . ?
C4B N4B C6B 110.98(9) . . ?
C4A N4A C6A 113.21(11) . . ?
C4A N4A C5A 111.25(9) . . ?
C6A N4A C5A 111.31(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 C1 N1 K1 -64.2(9) . . . . ?
N3 K1 N1 C1 83.57(18) 3_455 . . . ?
N3 K1 N1 C1 -87.15(18) 4_655 . . . ?
N2 K1 N1 C1 -173.92(18) 1_565 . . . ?
N2 K1 N1 C1 158.82(16) 2_665 . . . ?
N1 K1 N1 C1 0.80(18) 2_655 . . . ?
N1 C1 Fe1 C2 70.0(8) . . . . ?
N1 C1 Fe1 C2 -110.0(8) . . . 7_656 ?
N1 C1 Fe1 C3 -19.1(8) . . . 7_656 ?
N1 C1 Fe1 C3 160.9(8) . . . . ?
N1 C1 Fe1 C1 67(100) . . . 7_656 ?
C2 Fe1 C2 N2 -131(52) 7_656 . . . ?
C3 Fe1 C2 N2 76(4) 7_656 . . . ?
C3 Fe1 C2 N2 -104(4) . . . . ?
C1 Fe1 C2 N2 -11(4) . . . . ?
C1 Fe1 C2 N2 169(68) 7_656 . . . ?
Fe1 C2 N2 K1 -138(4) . . . 1_545 ?
K1 N3 C3 Fe1 -156.6(13) 3_545 . . . ?
C2 Fe1 C3 N3 -124.5(15) . . . . ?
C2 Fe1 C3 N3 55.5(15) 7_656 . . . ?
C3 Fe1 C3 N3 -120(100) 7_656 . . . ?
C1 Fe1 C3 N3 146.9(15) . . . . ?
C1 Fe1 C3 N3 -33.1(15) 7_656 . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.053
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_350_K
_database_code_depnum_ccdc_archive 'CCDC 1422612'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Fe K N8'
_chemical_formula_weight         371.31

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'
K K 0.2009 0.2494 '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           Cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   12.104(2)
_cell_length_b                   12.104(2)
_cell_length_c                   12.104(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1773.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    841
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      27.3

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_T_max  0.8029
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4120
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         27.30
_reflns_number_total             136
_reflns_number_gt                134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0572P)²+0.7656P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         136
_refine_ls_number_parameters     24
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_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 0.5000 0.0000 0.0667(6) Uani 1 48 d S . .
K1 K 0.0000 0.5000 0.5000 0.0790(7) Uani 1 48 d S . .
C1 C -0.0159(9) 0.4841(9) 0.1596(6) 0.066(4) Uani 0.25 2 d SP . .
N1 N 0.019(2) 0.519(2) 0.2538(4) 0.106(11) Uani 0.25 2 d SP . .
N2 N 0.2269(7) 0.7269(7) 0.2269(7) 0.097(6) Uani 0.25 6 d SP . .
H2A H 0.1839 0.6839 0.1840 0.116 Uiso 0.25 6 d SPR . .
C2 C 0.2326(8) 0.6707(9) 0.3293(9) 0.158(9) Uani 0.25 2 d SP . .
H2B H 0.2594 0.7200 0.3876 0.237 Uiso 0.13 1 d PR . .
H2C H 0.1604 0.6446 0.3553 0.237 Uiso 0.25 2 d SPR . .
H2D H 0.2820 0.6090 0.3247 0.237 Uiso 0.13 1 d PR . .


_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 C1 1.951(7) 30 ?
Fe1 C1 1.951(7) 82 ?
Fe1 C1 1.951(7) 128_554 ?
Fe1 C1 1.951(7) 180_455 ?
Fe1 C1 1.951(7) 98 ?
Fe1 C1 1.951(7) 179 ?
Fe1 C1 1.951(7) 2_565 ?
Fe1 C1 1.951(7) 127 ?
Fe1 C1 1.951(7) 29_554 ?
Fe1 C1 1.951(7) 3 ?
Fe1 C1 1.951(7) 99_565 ?
Fe1 C1 1.951(7) 178_455 ?
K1 N1 2.998(6) 154_465 ?
K1 N1 2.998(6) 59_465 ?
K1 N1 2.998(6) 60_565 ?
K1 N1 2.998(6) 2_565 ?
K1 N1 2.998(6) 98_556 ?
K1 N1 2.998(6) 153_565 ?
K1 N1 2.998(6) 99_565 ?
K1 N1 2.998(6) 174 ?
K1 N1 2.998(6) 100 ?
K1 N1 2.998(6) 78_456 ?
K1 N1 2.998(6) . ?
K1 N1 2.998(6) 58 ?
C1 C1 0.39(2) 99_565 ?
C1 C1 0.39(2) 100 ?
C1 C1 0.55(3) 2_565 ?
C1 N1 1.142(8) 2_565 ?
C1 N1 1.218(13) 100 ?
C1 N1 1.218(13) 99_565 ?
C1 N1 1.289(19) . ?
N1 N1 0.46(5) 99_565 ?
N1 N1 0.46(5) 100 ?
N1 N1 0.66(7) 2_565 ?
N1 C1 1.142(8) 2_565 ?
N1 C1 1.218(13) 99_565 ?
N1 C1 1.218(13) 100 ?
N2 N2 0.79(2) 74_565 ?
N2 N2 0.79(2) 28_565 ?
N2 N2 0.79(2) 51 ?
N2 C2 1.080(15) 55_564 ?
N2 C2 1.080(15) 51 ?
N2 C2 1.080(15) 59_465 ?
N2 C2 1.416(15) 81_455 ?
N2 C2 1.416(15) 28_565 ?
N2 C2 1.416(16) 29_554 ?
N2 C2 1.416(15) 80_556 ?
N2 C2 1.416(16) 12_665 ?
N2 C2 1.416(15) . ?
N2 H2A 0.8997 . ?
C2 C2 1.06(2) 59_465 ?
C2 C2 1.06(2) 80_556 ?
C2 N2 1.080(15) 51 ?
C2 N2 1.416(15) 28_565 ?
C2 C2 1.66(2) 6_566 ?
C2 C2 1.656(19) 12_665 ?
C2 N2 1.82(2) 74_565 ?
C2 C2 1.97(2) 74_565 ?
C2 C2 1.97(2) 51 ?
C2 H2B 0.9790 . ?
C2 H2C 0.9807 . ?
C2 H2D 0.9582 . ?

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
C1 Fe1 C1 78.1(6) 30 82 ?
C1 Fe1 C1 11.3(6) 30 128_554 ?
C1 Fe1 C1 79.3(5) 82 128_554 ?
C1 Fe1 C1 89.44(6) 30 180_455 ?
C1 Fe1 C1 11.3(6) 82 180_455 ?
C1 Fe1 C1 90.56(6) 128_554 180_455 ?
C1 Fe1 C1 101.9(7) 30 98 ?
C1 Fe1 C1 101.9(6) 82 98 ?
C1 Fe1 C1 90.56(6) 128_554 98 ?
C1 Fe1 C1 100.7(5) 180_455 98 ?
C1 Fe1 C1 79.3(5) 30 179 ?
C1 Fe1 C1 11.3(6) 82 179 ?
C1 Fe1 C1 78.1(6) 128_554 179 ?
C1 Fe1 C1 16.1(8) 180_455 179 ?
C1 Fe1 C1 90.56(6) 98 179 ?
C1 Fe1 C1 78.1(6) 30 2_565 ?
C1 Fe1 C1 78.1(6) 82 2_565 ?
C1 Fe1 C1 89.44(6) 128_554 2_565 ?
C1 Fe1 C1 79.3(5) 180_455 2_565 ?
C1 Fe1 C1 180.00(6) 98 2_565 ?
C1 Fe1 C1 89.44(6) 179 2_565 ?
C1 Fe1 C1 11.3(6) 30 127 ?
C1 Fe1 C1 89.44(6) 82 127 ?
C1 Fe1 C1 16.1(8) 128_554 127 ?
C1 Fe1 C1 100.7(5) 180_455 127 ?
C1 Fe1 C1 100.7(5) 98 127 ?
C1 Fe1 C1 90.56(6) 179 127 ?
C1 Fe1 C1 79.3(5) 2_565 127 ?
C1 Fe1 C1 16.1(8) 30 29_554 ?
C1 Fe1 C1 90.56(6) 82 29_554 ?
C1 Fe1 C1 11.3(6) 128_554 29_554 ?
C1 Fe1 C1 101.9(7) 180_455 29_554 ?
C1 Fe1 C1 89.44(6) 98 29_554 ?
C1 Fe1 C1 89.44(6) 179 29_554 ?
C1 Fe1 C1 90.56(6) 2_565 29_554 ?
C1 Fe1 C1 11.3(6) 127 29_554 ?
C1 Fe1 C1 90.56(6) 30 3 ?
C1 Fe1 C1 100.7(5) 82 3 ?
C1 Fe1 C1 79.3(5) 128_554 3 ?
C1 Fe1 C1 101.9(6) 180_455 3 ?
C1 Fe1 C1 11.3(6) 98 3 ?
C1 Fe1 C1 89.44(6) 179 3 ?
C1 Fe1 C1 168.7(6) 2_565 3 ?
C1 Fe1 C1 89.44(6) 127 3 ?
C1 Fe1 C1 78.1(6) 29_554 3 ?
C1 Fe1 C1 89.44(6) 30 99_565 ?
C1 Fe1 C1 79.3(5) 82 99_565 ?
C1 Fe1 C1 100.7(5) 128_554 99_565 ?
C1 Fe1 C1 78.1(6) 180_455 99_565 ?
C1 Fe1 C1 168.7(6) 98 99_565 ?
C1 Fe1 C1 90.56(6) 179 99_565 ?
C1 Fe1 C1 11.3(6) 2_565 99_565 ?
C1 Fe1 C1 90.56(6) 127 99_565 ?
C1 Fe1 C1 101.9(6) 29_554 99_565 ?
C1 Fe1 C1 180.000(1) 3 99_565 ?
C1 Fe1 C1 101.9(7) 30 178_455 ?
C1 Fe1 C1 180.0(6) 82 178_455 ?
C1 Fe1 C1 100.7(5) 128_554 178_455 ?
C1 Fe1 C1 168.7(6) 180_455 178_455 ?
C1 Fe1 C1 78.1(6) 98 178_455 ?
C1 Fe1 C1 168.7(6) 179 178_455 ?
C1 Fe1 C1 101.9(6) 2_565 178_455 ?
C1 Fe1 C1 90.56(6) 127 178_455 ?
C1 Fe1 C1 89.44(6) 29_554 178_455 ?
C1 Fe1 C1 79.3(5) 3 178_455 ?
C1 Fe1 C1 100.7(5) 99_565 178_455 ?
N1 K1 N1 8.9(9) 154_465 59_465 ?
N1 K1 N1 8.9(9) 154_465 60_565 ?
N1 K1 N1 12.6(13) 59_465 60_565 ?
N1 K1 N1 99.2(10) 154_465 2_565 ?
N1 K1 N1 90.34(7) 59_465 2_565 ?
N1 K1 N1 98.5(8) 60_565 2_565 ?
N1 K1 N1 80.8(10) 154_465 98_556 ?
N1 K1 N1 89.66(7) 59_465 98_556 ?
N1 K1 N1 81.5(8) 60_565 98_556 ?
N1 K1 N1 180.000(3) 2_565 98_556 ?
N1 K1 N1 12.6(13) 154_465 153_565 ?
N1 K1 N1 8.9(9) 59_465 153_565 ?
N1 K1 N1 8.9(9) 60_565 153_565 ?
N1 K1 N1 89.66(7) 2_565 153_565 ?
N1 K1 N1 90.34(7) 98_556 153_565 ?
N1 K1 N1 98.5(8) 154_465 99_565 ?
N1 K1 N1 89.66(7) 59_465 99_565 ?
N1 K1 N1 99.2(10) 60_565 99_565 ?
N1 K1 N1 8.9(9) 2_565 99_565 ?
N1 K1 N1 171.1(9) 98_556 99_565 ?
N1 K1 N1 90.34(7) 153_565 99_565 ?
N1 K1 N1 80.8(10) 154_465 174 ?
N1 K1 N1 81.5(8) 59_465 174 ?
N1 K1 N1 89.66(8) 60_565 174 ?
N1 K1 N1 99.2(10) 2_565 174 ?
N1 K1 N1 80.8(10) 98_556 174 ?
N1 K1 N1 90.34(7) 153_565 174 ?
N1 K1 N1 90.34(7) 99_565 174 ?
N1 K1 N1 90.34(7) 154_465 100 ?
N1 K1 N1 81.5(8) 59_465 100 ?
N1 K1 N1 89.66(7) 60_565 100 ?
N1 K1 N1 8.9(9) 2_565 100 ?
N1 K1 N1 171.1(9) 98_556 100 ?
N1 K1 N1 80.8(10) 153_565 100 ?
N1 K1 N1 12.6(13) 99_565 100 ?
N1 K1 N1 98.5(8) 174 100 ?
N1 K1 N1 99.2(10) 154_465 78_456 ?
N1 K1 N1 98.5(8) 59_465 78_456 ?
N1 K1 N1 90.34(7) 60_565 78_456 ?
N1 K1 N1 80.8(10) 2_565 78_456 ?
N1 K1 N1 99.2(10) 98_556 78_456 ?
N1 K1 N1 89.66(7) 153_565 78_456 ?
N1 K1 N1 89.66(7) 99_565 78_456 ?
N1 K1 N1 180.000(1) 174 78_456 ?
N1 K1 N1 81.5(8) 100 78_456 ?
N1 K1 N1 89.66(7) 154_465 . ?
N1 K1 N1 80.8(10) 59_465 . ?
N1 K1 N1 90.34(7) 60_565 . ?
N1 K1 N1 12.6(13) 2_565 . ?
N1 K1 N1 167.4(13) 98_556 . ?
N1 K1 N1 81.5(8) 153_565 . ?
N1 K1 N1 8.9(9) 99_565 . ?
N1 K1 N1 89.66(7) 174 . ?
N1 K1 N1 8.9(9) 100 . ?
N1 K1 N1 90.34(7) 78_456 . ?
N1 K1 N1 180.000(1) 154_465 58 ?
N1 K1 N1 171.1(9) 59_465 58 ?
N1 K1 N1 171.1(9) 60_565 58 ?
N1 K1 N1 80.8(10) 2_565 58 ?
N1 K1 N1 99.2(10) 98_556 58 ?
N1 K1 N1 167.4(13) 153_565 58 ?
N1 K1 N1 81.5(8) 99_565 58 ?
N1 K1 N1 99.2(10) 174 58 ?
N1 K1 N1 89.66(7) 100 58 ?
N1 K1 N1 80.8(10) 78_456 58 ?
N1 K1 N1 90.34(7) . 58 ?
C1 C1 C1 90.00(2) 99_565 100 ?
C1 C1 C1 45.000(6) 99_565 2_565 ?
C1 C1 C1 45.000(2) 100 2_565 ?
C1 C1 N1 92.0(13) 99_565 2_565 ?
C1 C1 N1 92.0(13) 100 2_565 ?
C1 C1 N1 92.8(19) 2_565 2_565 ?
C1 C1 N1 69.6(11) 99_565 100 ?
C1 C1 N1 91.9(13) 100 100 ?
C1 C1 N1 77.1(7) 2_565 100 ?
N1 C1 N1 22(2) 2_565 100 ?
C1 C1 N1 91.9(13) 99_565 99_565 ?
C1 C1 N1 69.6(11) 100 99_565 ?
C1 C1 N1 77.1(7) 2_565 99_565 ?
N1 C1 N1 22(2) 2_565 99_565 ?
N1 C1 N1 31(3) 100 99_565 ?
C1 C1 N1 70.8(10) 99_565 . ?
C1 C1 N1 70.8(10) 100 . ?
C1 C1 N1 62.2(14) 2_565 . ?
N1 C1 N1 31(3) 2_565 . ?
N1 C1 N1 21(2) 100 . ?
N1 C1 N1 21(2) 99_565 . ?
C1 C1 Fe1 84.3(3) 99_565 . ?
C1 C1 Fe1 84.3(3) 100 . ?
C1 C1 Fe1 82.0(4) 2_565 . ?
N1 C1 Fe1 175(2) 2_565 . ?
N1 C1 Fe1 153.7(12) 100 . ?
N1 C1 Fe1 153.7(12) 99_565 . ?
N1 C1 Fe1 144.2(16) . . ?
N1 N1 N1 90.0 99_565 100 ?
N1 N1 N1 45.00(2) 99_565 2_565 ?
N1 N1 N1 45.000(19) 100 2_565 ?
N1 N1 C1 88.0(14) 99_565 2_565 ?
N1 N1 C1 88.0(14) 100 2_565 ?
N1 N1 C1 87.2(19) 2_565 2_565 ?
N1 N1 C1 88.1(13) 99_565 99_565 ?
N1 N1 C1 69.6(11) 100 99_565 ?
N1 N1 C1 74.4(16) 2_565 99_565 ?
C1 N1 C1 18.4(10) 2_565 99_565 ?
N1 N1 C1 69.6(11) 99_565 100 ?
N1 N1 C1 88.1(13) 100 100 ?
N1 N1 C1 74.4(16) 2_565 100 ?
C1 N1 C1 18.4(10) 2_565 100 ?
C1 N1 C1 25.9(14) 99_565 100 ?
N1 N1 C1 70.8(10) 99_565 . ?
N1 N1 C1 70.8(10) 100 . ?
N1 N1 C1 62.2(14) 2_565 . ?
C1 N1 C1 25.0(14) 2_565 . ?
C1 N1 C1 17.4(9) 99_565 . ?
C1 N1 C1 17.4(9) 100 . ?
N1 N1 K1 85.6(5) 99_565 . ?
N1 N1 K1 85.6(5) 100 . ?
N1 N1 K1 83.7(7) 2_565 . ?
C1 N1 K1 171(3) 2_565 . ?
C1 N1 K1 154.3(19) 99_565 . ?
C1 N1 K1 154.3(19) 100 . ?
C1 N1 K1 146(2) . . ?
N2 N2 N2 60.000(1) 74_565 28_565 ?
N2 N2 N2 60.000(2) 74_565 51 ?
N2 N2 N2 60.000(2) 28_565 51 ?
N2 N2 C2 97.1(9) 74_565 55_564 ?
N2 N2 C2 97.1(9) 28_565 55_564 ?
N2 N2 C2 153.0(10) 51 55_564 ?
N2 N2 C2 97.1(9) 74_565 51 ?
N2 N2 C2 153.0(10) 28_565 51 ?
N2 N2 C2 97.1(9) 51 51 ?
C2 N2 C2 100.1(13) 55_564 51 ?
N2 N2 C2 153.0(10) 74_565 59_465 ?
N2 N2 C2 97.1(9) 28_565 59_465 ?
N2 N2 C2 97.1(9) 51 59_465 ?
C2 N2 C2 100.1(13) 55_564 59_465 ?
C2 N2 C2 100.1(13) 51 59_465 ?
N2 N2 C2 73.8(5) 74_565 81_455 ?
N2 N2 C2 49.2(6) 28_565 81_455 ?
N2 N2 C2 107.8(6) 51 81_455 ?
C2 N2 C2 47.9(8) 55_564 81_455 ?
C2 N2 C2 143.2(5) 51 81_455 ?
C2 N2 C2 103.1(2) 59_465 81_455 ?
N2 N2 C2 49.2(6) 74_565 28_565 ?
N2 N2 C2 73.8(5) 28_565 28_565 ?
N2 N2 C2 107.8(6) 51 28_565 ?
C2 N2 C2 47.9(8) 55_564 28_565 ?
C2 N2 C2 103.1(2) 51 28_565 ?
C2 N2 C2 143.2(5) 59_465 28_565 ?
C2 N2 C2 43.9(7) 81_455 28_565 ?
N2 N2 C2 49.2(6) 74_565 29_554 ?
N2 N2 C2 107.8(6) 28_565 29_554 ?
N2 N2 C2 73.8(5) 51 29_554 ?
C2 N2 C2 103.1(2) 55_564 29_554 ?
C2 N2 C2 47.9(8) 51 29_554 ?
C2 N2 C2 143.2(5) 59_465 29_554 ?
C2 N2 C2 113.7(5) 81_455 29_554 ?
C2 N2 C2 71.6(7) 28_565 29_554 ?
N2 N2 C2 107.8(6) 74_565 80_556 ?
N2 N2 C2 49.2(6) 28_565 80_556 ?
N2 N2 C2 73.8(5) 51 80_556 ?
C2 N2 C2 103.1(2) 55_564 80_556 ?
C2 N2 C2 143.2(5) 51 80_556 ?
C2 N2 C2 47.9(8) 59_465 80_556 ?
C2 N2 C2 71.6(7) 81_455 80_556 ?
C2 N2 C2 113.7(5) 28_565 80_556 ?
C2 N2 C2 147.0(11) 29_554 80_556 ?
N2 N2 C2 73.8(5) 74_565 12_665 ?
N2 N2 C2 107.8(6) 28_565 12_665 ?
N2 N2 C2 49.2(6) 51 12_665 ?
C2 N2 C2 143.2(5) 55_564 12_665 ?
C2 N2 C2 47.9(8) 51 12_665 ?
C2 N2 C2 103.1(2) 59_465 12_665 ?
C2 N2 C2 147.0(11) 81_455 12_665 ?
C2 N2 C2 113.7(5) 28_565 12_665 ?
C2 N2 C2 43.9(7) 29_554 12_665 ?
C2 N2 C2 113.7(5) 80_556 12_665 ?
N2 N2 C2 107.8(6) 74_565 . ?
N2 N2 C2 73.8(5) 28_565 . ?
N2 N2 C2 49.2(6) 51 . ?
C2 N2 C2 143.2(5) 55_564 . ?
C2 N2 C2 103.1(2) 51 . ?
C2 N2 C2 47.9(8) 59_465 . ?
C2 N2 C2 113.7(5) 81_455 . ?
C2 N2 C2 147.0(11) 28_565 . ?
C2 N2 C2 113.7(5) 29_554 . ?
C2 N2 C2 43.9(7) 80_556 . ?
C2 N2 C2 71.6(7) 12_665 . ?
N2 N2 H2A 144.7 74_565 . ?
N2 N2 H2A 144.7 28_565 . ?
N2 N2 H2A 144.7 51 . ?
C2 N2 H2A 62.3 55_564 . ?
C2 N2 H2A 62.3 51 . ?
C2 N2 H2A 62.3 59_465 . ?
C2 N2 H2A 104.9 81_455 . ?
C2 N2 H2A 104.9 28_565 . ?
C2 N2 H2A 104.9 29_554 . ?
C2 N2 H2A 104.9 80_556 . ?
C2 N2 H2A 104.9 12_665 . ?
C2 N2 H2A 104.9 . . ?
C2 C2 C2 60.000(3) 59_465 80_556 ?
C2 C2 N2 82.9(9) 59_465 51 ?
C2 C2 N2 82.9(9) 80_556 51 ?
C2 C2 N2 68.0(3) 59_465 28_565 ?
C2 C2 N2 49.2(6) 80_556 28_565 ?
N2 C2 N2 33.7(12) 51 28_565 ?
C2 C2 N2 49.2(6) 59_465 . ?
C2 C2 N2 68.0(3) 80_556 . ?
N2 C2 N2 33.7(12) 51 . ?
N2 C2 N2 32.5(10) 28_565 . ?
C2 C2 C2 120.000(5) 59_465 6_566 ?
C2 C2 C2 90.000(1) 80_556 6_566 ?
N2 C2 C2 39.9(6) 51 6_566 ?
N2 C2 C2 54.2(4) 28_565 6_566 ?
N2 C2 C2 72.2(6) . 6_566 ?
C2 C2 C2 90.000(5) 59_465 12_665 ?
C2 C2 C2 120.000(5) 80_556 12_665 ?
N2 C2 C2 39.9(6) 51 12_665 ?
N2 C2 C2 72.2(6) 28_565 12_665 ?
N2 C2 C2 54.2(4) . 12_665 ?
C2 C2 C2 60.000(2) 6_566 12_665 ?
C2 C2 N2 73.1(3) 59_465 74_565 ?
C2 C2 N2 73.1(3) 80_556 74_565 ?
N2 C2 N2 11.4(7) 51 74_565 ?
N2 C2 N2 24.5(7) 28_565 74_565 ?
N2 C2 N2 24.5(7) . 74_565 ?
C2 C2 N2 47.8(3) 6_566 74_565 ?
C2 C2 N2 47.8(3) 12_665 74_565 ?
C2 C2 C2 98.7(4) 59_465 74_565 ?
C2 C2 C2 57.4(6) 80_556 74_565 ?
N2 C2 C2 44.55(19) 51 74_565 ?
N2 C2 C2 32.3(3) 28_565 74_565 ?
N2 C2 C2 62.7(6) . 74_565 ?
C2 C2 C2 32.6(6) 6_566 74_565 ?
C2 C2 C2 81.3(4) 12_665 74_565 ?
N2 C2 C2 43.70(11) 74_565 74_565 ?
C2 C2 C2 57.4(6) 59_465 51 ?
C2 C2 C2 98.7(4) 80_556 51 ?
N2 C2 C2 44.55(19) 51 51 ?
N2 C2 C2 62.7(6) 28_565 51 ?
N2 C2 C2 32.3(3) . 51 ?
C2 C2 C2 81.3(4) 6_566 51 ?
C2 C2 C2 32.6(6) 12_665 51 ?
N2 C2 C2 43.70(11) 74_565 51 ?
C2 C2 C2 87.4(3) 74_565 51 ?
C2 C2 H2B 138.0 59_465 . ?
C2 C2 H2B 78.7 80_556 . ?
N2 C2 H2B 85.4 51 . ?
N2 C2 H2B 80.1 28_565 . ?
N2 C2 H2B 110.8 . . ?
C2 C2 H2B 48.3 6_566 . ?
C2 C2 H2B 106.0 12_665 . ?
N2 C2 H2B 89.2 74_565 . ?
C2 C2 H2B 48.2 74_565 . ?
C2 C2 H2B 129.2 51 . ?
C2 C2 H2C 66.2 59_465 . ?
C2 C2 H2C 66.3 80_556 . ?
N2 C2 H2C 144.1 51 . ?
N2 C2 H2C 113.1 28_565 . ?
N2 C2 H2C 113.1 . . ?
C2 C2 H2C 149.0 6_566 . ?
C2 C2 H2C 149.0 12_665 . ?
N2 C2 H2C 132.7 74_565 . ?
C2 C2 H2C 120.4 74_565 . ?
C2 C2 H2C 120.3 51 . ?
H2B C2 H2C 105.1 . . ?
C2 C2 H2D 113.6 59_465 . ?
C2 C2 H2D 172.9 80_556 . ?
N2 C2 H2D 99.8 51 . ?
N2 C2 H2D 133.2 28_565 . ?
N2 C2 H2D 110.7 . . ?
C2 C2 H2D 96.3 6_566 . ?
C2 C2 H2D 61.1 12_665 . ?
N2 C2 H2D 108.8 74_565 . ?
C2 C2 H2D 128.8 74_565 . ?
C2 C2 H2D 79.0 51 . ?
H2B C2 H2D 108.0 . . ?
H2C C2 H2D 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.30
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.112
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.046
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_298_K
_database_code_depnum_ccdc_archive 'CCDC 1422613'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H24 Fe K N8'
_chemical_formula_weight         399.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2010 0.2490 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4/m

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

_cell_length_a                   8.843(2)
_cell_length_b                   8.843(2)
_cell_length_c                   12.150(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     950.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    983
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      27.3

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             418
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7484
_exptl_absorpt_correction_T_max  0.8211
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4344
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         25.94
_reflns_number_total             489
_reflns_number_gt                477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0411P)²+0.7311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         489
_refine_ls_number_parameters     36
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 1.0000 0.0260(3) Uani 1 8 d S . .
K1 K 0.5000 0.5000 0.5000 0.0469(4) Uani 1 8 d S . .
N1 N 0.5000 0.5000 0.7445(2) 0.0423(8) Uani 1 4 d S . .
N2 N 0.7772(3) 0.7163(3) 1.0000 0.0404(6) Uani 1 2 d S . .
C2 C 0.6753(3) 0.6356(3) 1.0000 0.0302(5) Uani 1 2 d S . .
C1 C 0.5000 0.5000 0.8391(3) 0.0318(7) Uani 1 4 d S . .
N3 N 0.5000 0.0000 0.7500 0.0265(6) Uani 1 4 d S . .
C3 C 0.5775(3) 0.1122(3) 0.6799(2) 0.0625(7) Uani 1 1 d . . .
H3A H 0.6503 0.0618 0.6342 0.094 Uiso 1 1 calc R . .
H3B H 0.6281 0.1849 0.7256 0.094 Uiso 1 1 calc R . .
H3C H 0.5046 0.1628 0.6344 0.094 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 C1 1.955(4) 9_667 ?
Fe1 C1 1.955(4) . ?
Fe1 C2 1.959(3) . ?
Fe1 C2 1.959(3) 9_667 ?
Fe1 C2 1.959(3) 2_655 ?
Fe1 C2 1.959(3) 10_567 ?
N1 C1 1.150(4) . ?
N2 C2 1.150(3) . ?
N3 C3 1.476(2) 3_655 ?
N3 C3 1.476(2) 14_556 ?
N3 C3 1.476(2) . ?
N3 C3 1.476(2) 16_546 ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 180.000(1) 9_667 . ?
C1 Fe1 C2 90.000(1) 9_667 . ?
C1 Fe1 C2 90.000(1) . . ?
C1 Fe1 C2 90.000(1) 9_667 9_667 ?
C1 Fe1 C2 90.000(1) . 9_667 ?
C2 Fe1 C2 180.00(15) . 9_667 ?
C1 Fe1 C2 90.0 9_667 2_655 ?
C1 Fe1 C2 90.0 . 2_655 ?
C2 Fe1 C2 90.000(1) . 2_655 ?
C2 Fe1 C2 90.000(1) 9_667 2_655 ?
C1 Fe1 C2 90.0 9_667 10_567 ?
C1 Fe1 C2 90.0 . 10_567 ?
C2 Fe1 C2 90.000(1) . 10_567 ?
C2 Fe1 C2 90.000(1) 9_667 10_567 ?
C2 Fe1 C2 180.000(1) 2_655 10_567 ?
N2 C2 Fe1 179.3(2) . . ?
N1 C1 Fe1 180.000(1) . . ?
C3 N3 C3 109.44(12) 3_655 14_556 ?
C3 N3 C3 109.5(2) 3_655 . ?
C3 N3 C3 109.44(12) 14_556 . ?
C3 N3 C3 109.44(12) 3_655 16_546 ?
C3 N3 C3 109.5(2) 14_556 16_546 ?
C3 N3 C3 109.44(12) . 16_546 ?
N3 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Fe1 C2 N2 -90.0 9_667 . . . ?
C1 Fe1 C2 N2 90.0 . . . . ?
C2 Fe1 C2 N2 0.0 9_667 . . . ?
C2 Fe1 C2 N2 0.0 2_655 . . . ?
C2 Fe1 C2 N2 180.0 10_567 . . . ?
C1 Fe1 C1 N1 0(100) 9_667 . . . ?
C2 Fe1 C1 N1 -87(100) . . . . ?
C2 Fe1 C1 N1 93(100) 9_667 . . . ?
C2 Fe1 C1 N1 3(100) 2_655 . . . ?
C2 Fe1 C1 N1 -177(100) 10_567 . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.94
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.047
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_373_K
_database_code_depnum_ccdc_archive 'CCDC 1422614'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H24 Fe K N8'
_chemical_formula_weight         399.36

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'
K K 0.2009 0.2494 '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           cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   12.451(2)
_cell_length_b                   12.451(2)
_cell_length_c                   12.451(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1930.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    573
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      27.2

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             836
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7515
_exptl_absorpt_correction_T_max  0.8236
_exptl_absorpt_process_details   'REQAB; Jacobson, 1998'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      373(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       '/w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3714
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.40
_reflns_number_total             147
_reflns_number_gt                138
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-V (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0257P)²+1.3507P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         147
_refine_ls_number_parameters     20
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_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 0.5000 0.0000 0.5000 0.0391(4) Uani 1 48 d S . .
K1 K 0.5000 0.5000 0.5000 0.0629(6) Uani 1 48 d S . .
N1 N 0.5000 0.2488(2) 0.5000 0.0763(12) Uani 1 8 d S . .
C1 C 0.5000 0.1571(3) 0.5000 0.0515(9) Uani 1 8 d S . .
N2 N 0.7500 0.2500 0.7500 0.0389(10) Uani 1 24 d S . .
C2 C 0.7328(8) 0.318(3) 0.655(4) 0.105(14) Uani 0.17 1 d P . .
H2A H 0.6569 0.3290 0.6569 0.157 Uiso 0.33 2 d SPR . .
H2B H 0.7659 0.3850 0.6757 0.157 Uiso 0.17 1 d PR . .
H2C H 0.7628 0.2945 0.5883 0.157 Uiso 0.17 1 d PR . .


_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 C1 1.956(3) 125_645 ?
Fe1 C1 1.956(3) 29 ?
Fe1 C1 1.956(3) . ?
Fe1 C1 1.956(3) 97_656 ?
Fe1 C1 1.956(3) 74_545 ?
Fe1 C1 1.956(3) 170_556 ?
K1 N1 3.127(3) 98_566 ?
K1 N1 3.127(3) 2_655 ?
K1 N1 3.127(3) 101_656 ?
K1 N1 3.127(3) 97_666 ?
K1 N1 3.127(3) . ?
K1 N1 3.127(3) 5_565 ?
N1 C1 1.142(4) . ?
N2 C2 1.472(14) 66_566 ?
N2 C2 1.472(14) 64_665 ?
N2 C2 1.472(14) 146_566 ?
N2 C2 1.472(14) 151_665 ?
N2 C2 1.472(14) 167_656 ?
N2 C2 1.472(14) 57_656 ?
N2 C2 1.472(14) 173_646 ?
N2 C2 1.472(14) 115_665 ?
N2 C2 1.472(14) 39_646 ?
N2 C2 1.472(14) 14_566 ?
N2 C2 1.472(14) 75_655 ?
N2 C2 1.472(14) 130_556 ?
C2 C2 0.46(12) 117_566 ?
C2 C2 0.90(6) 115_665 ?
C2 C2 1.20(5) 14_566 ?
C2 C2 1.20(5) 13_665 ?
C2 C2 1.37(7) 120 ?
C2 C2 1.51(7) 188_545 ?
C2 C2 1.76(8) 75_655 ?
C2 C2 1.79(2) 66_566 ?
C2 C2 1.79(2) 89_646 ?
C2 C2 1.97(6) 167_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C1 180.0 125_645 29 ?
C1 Fe1 C1 90.0 125_645 . ?
C1 Fe1 C1 90.0 29 . ?
C1 Fe1 C1 90.0 125_645 97_656 ?
C1 Fe1 C1 90.0 29 97_656 ?
C1 Fe1 C1 180.0 . 97_656 ?
C1 Fe1 C1 90.0 125_645 74_545 ?
C1 Fe1 C1 90.0 29 74_545 ?
C1 Fe1 C1 90.0 . 74_545 ?
C1 Fe1 C1 90.000(1) 97_656 74_545 ?
C1 Fe1 C1 90.0 125_645 170_556 ?
C1 Fe1 C1 90.0 29 170_556 ?
C1 Fe1 C1 90.000(1) . 170_556 ?
C1 Fe1 C1 90.0 97_656 170_556 ?
C1 Fe1 C1 180.0 74_545 170_556 ?
N1 K1 N1 180.0 98_566 2_655 ?
N1 K1 N1 90.0 98_566 101_656 ?
N1 K1 N1 90.0 2_655 101_656 ?
N1 K1 N1 90.0 98_566 97_666 ?
N1 K1 N1 90.0 2_655 97_666 ?
N1 K1 N1 90.0 101_656 97_666 ?
N1 K1 N1 90.0 98_566 . ?
N1 K1 N1 90.0 2_655 . ?
N1 K1 N1 90.0 101_656 . ?
N1 K1 N1 180.0 97_666 . ?
N1 K1 N1 90.0 98_566 5_565 ?
N1 K1 N1 90.0 2_655 5_565 ?
N1 K1 N1 180.0 101_656 5_565 ?
N1 K1 N1 90.0 97_666 5_565 ?
N1 K1 N1 90.0 . 5_565 ?
C1 N1 K1 180.0 . . ?
N1 C1 Fe1 180.0 . . ?
C2 N2 C2 48.3(16) 66_566 64_665 ?
C2 N2 C2 55(3) 66_566 146_566 ?
C2 N2 C2 18(5) 64_665 146_566 ?
C2 N2 C2 36(3) 66_566 151_665 ?
C2 N2 C2 55(3) 64_665 151_665 ?
C2 N2 C2 48.3(16) 146_566 151_665 ?
C2 N2 C2 18(5) 66_566 167_656 ?
C2 N2 C2 36(3) 64_665 167_656 ?
C2 N2 C2 48.3(16) 146_566 167_656 ?
C2 N2 C2 48.3(16) 151_665 167_656 ?
C2 N2 C2 48.3(16) 66_566 57_656 ?
C2 N2 C2 48.3(16) 64_665 57_656 ?
C2 N2 C2 36(3) 146_566 57_656 ?
C2 N2 C2 18(5) 151_665 57_656 ?
C2 N2 C2 55(3) 167_656 57_656 ?
C2 N2 C2 130(3) 66_566 173_646 ?
C2 N2 C2 110(2) 64_665 173_646 ?
C2 N2 C2 119.8(3) 146_566 173_646 ?
C2 N2 C2 163.3(8) 151_665 173_646 ?
C2 N2 C2 115.6(12) 167_656 173_646 ?
C2 N2 C2 155(3) 57_656 173_646 ?
C2 N2 C2 110(2) 66_566 115_665 ?
C2 N2 C2 155(3) 64_665 115_665 ?
C2 N2 C2 163.3(8) 146_566 115_665 ?
C2 N2 C2 115.6(13) 151_665 115_665 ?
C2 N2 C2 119.8(3) 167_656 115_665 ?
C2 N2 C2 130(3) 57_656 115_665 ?
C2 N2 C2 74.7(6) 173_646 115_665 ?
C2 N2 C2 163.3(8) 66_566 39_646 ?
C2 N2 C2 119.8(3) 64_665 39_646 ?
C2 N2 C2 110(2) 146_566 39_646 ?
C2 N2 C2 130(3) 151_665 39_646 ?
C2 N2 C2 155(3) 167_656 39_646 ?
C2 N2 C2 115.6(13) 57_656 39_646 ?
C2 N2 C2 62(4) 173_646 39_646 ?
C2 N2 C2 84(2) 115_665 39_646 ?
C2 N2 C2 115.6(12) 66_566 14_566 ?
C2 N2 C2 163.3(8) 64_665 14_566 ?
C2 N2 C2 155(3) 146_566 14_566 ?
C2 N2 C2 110(2) 151_665 14_566 ?
C2 N2 C2 130(3) 167_656 14_566 ?
C2 N2 C2 119.8(3) 57_656 14_566 ?
C2 N2 C2 84(2) 173_646 14_566 ?
C2 N2 C2 18(5) 115_665 14_566 ?
C2 N2 C2 74.7(6) 39_646 14_566 ?
C2 N2 C2 119.8(3) 66_566 75_655 ?
C2 N2 C2 115.6(12) 64_665 75_655 ?
C2 N2 C2 130(3) 146_566 75_655 ?
C2 N2 C2 155(3) 151_665 75_655 ?
C2 N2 C2 110(2) 167_656 75_655 ?
C2 N2 C2 163.3(8) 57_656 75_655 ?
C2 N2 C2 18(5) 173_646 75_655 ?
C2 N2 C2 62(4) 115_665 75_655 ?
C2 N2 C2 74.7(6) 39_646 75_655 ?
C2 N2 C2 74.7(6) 14_566 75_655 ?
C2 N2 C2 155(3) 66_566 130_556 ?
C2 N2 C2 130(3) 64_665 130_556 ?
C2 N2 C2 115.6(13) 146_566 130_556 ?
C2 N2 C2 119.8(3) 151_665 130_556 ?
C2 N2 C2 163.3(8) 167_656 130_556 ?
C2 N2 C2 110(2) 57_656 130_556 ?
C2 N2 C2 74.7(6) 173_646 130_556 ?
C2 N2 C2 74.7(6) 115_665 130_556 ?
C2 N2 C2 18(5) 39_646 130_556 ?
C2 N2 C2 62(4) 14_566 130_556 ?
C2 N2 C2 84(2) 75_655 130_556 ?
C2 C2 C2 120.00(5) 117_566 115_665 ?
C2 C2 C2 100(5) 117_566 14_566 ?
C2 C2 C2 20(5) 115_665 14_566 ?
C2 C2 C2 40(5) 117_566 13_665 ?
C2 C2 C2 80(5) 115_665 13_665 ?
C2 C2 C2 60.000(15) 14_566 13_665 ?
C2 C2 C2 60.000(10) 117_566 120 ?
C2 C2 C2 60.000(9) 115_665 120 ?
C2 C2 C2 40(5) 14_566 120 ?
C2 C2 C2 20(5) 13_665 120 ?
C2 C2 N2 81(2) 117_566 . ?
C2 C2 N2 72.1(13) 115_665 . ?
C2 C2 N2 65.9(8) 14_566 . ?
C2 C2 N2 65.9(8) 13_665 . ?
C2 C2 N2 62.3(13) 120 . ?
C2 C2 C2 120.00(6) 117_566 188_545 ?
C2 C2 C2 90.000(3) 115_665 188_545 ?
C2 C2 C2 101(3) 14_566 188_545 ?
C2 C2 C2 124.6(6) 13_665 188_545 ?
C2 C2 C2 120.000(4) 120 188_545 ?
N2 C2 C2 59.2(18) . 188_545 ?
C2 C2 C2 133.30(16) 117_566 75_655 ?
C2 C2 C2 59.1(7) 115_665 75_655 ?
C2 C2 C2 71(4) 14_566 75_655 ?
C2 C2 C2 113(3) 13_665 75_655 ?
C2 C2 C2 99.9(5) 120 75_655 ?
N2 C2 C2 53(2) . 75_655 ?
C2 C2 C2 30.9(7) 188_545 75_655 ?
C2 C2 C2 47(3) 117_566 66_566 ?
C2 C2 C2 123.5(7) 115_665 66_566 ?
C2 C2 C2 111(3) 14_566 66_566 ?
C2 C2 C2 69(6) 13_665 66_566 ?
C2 C2 C2 82.5(19) 120 66_566 ?
N2 C2 C2 52.6(3) . 66_566 ?
C2 C2 C2 73(3) 188_545 66_566 ?
C2 C2 C2 92(3) 75_655 66_566 ?
C2 C2 C2 107(3) 117_566 89_646 ?
C2 C2 C2 97.5(19) 115_665 89_646 ?
C2 C2 C2 105(3) 14_566 89_646 ?
C2 C2 C2 115(3) 13_665 89_646 ?
C2 C2 C2 115.0(15) 120 89_646 ?
N2 C2 C2 52.6(3) . 89_646 ?
C2 C2 C2 13(3) 188_545 89_646 ?
C2 C2 C2 40(2) 75_655 89_646 ?
C2 C2 C2 60.000(3) 66_566 89_646 ?
C2 C2 C2 60.00(3) 117_566 167_656 ?
C2 C2 C2 120.000(5) 115_665 167_656 ?
C2 C2 C2 112(2) 14_566 167_656 ?
C2 C2 C2 79(3) 13_665 167_656 ?
C2 C2 C2 90.000(14) 120 167_656 ?
N2 C2 C2 47.9(11) . 167_656 ?
C2 C2 C2 60.000(2) 188_545 167_656 ?
C2 C2 C2 80.1(5) 75_655 167_656 ?
C2 C2 C2 13(3) 66_566 167_656 ?
C2 C2 C2 47(3) 89_646 167_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 K1 N1 C1 0(100) 98_566 . . . ?
N1 K1 N1 C1 180(100) 2_655 . . . ?
N1 K1 N1 C1 90(100) 101_656 . . . ?
N1 K1 N1 C1 0(100) 97_666 . . . ?
N1 K1 N1 C1 -90(100) 5_565 . . . ?
K1 N1 C1 Fe1 0(100) . . . . ?
C1 Fe1 C1 N1 -90(100) 125_645 . . . ?
C1 Fe1 C1 N1 90(100) 29 . . . ?
C1 Fe1 C1 N1 0.0 97_656 . . . ?
C1 Fe1 C1 N1 180(100) 74_545 . . . ?
C1 Fe1 C1 N1 0(100) 170_556 . . . ?
C2 N2 C2 C2 -42(3) 66_566 . . 117_566 ?
C2 N2 C2 C2 -60(3) 64_665 . . 117_566 ?
C2 N2 C2 C2 -41.2(12) 146_566 . . 117_566 ?
C2 N2 C2 C2 -9.6(4) 151_665 . . 117_566 ?
C2 N2 C2 C2 -57.5(19) 167_656 . . 117_566 ?
C2 N2 C2 C2 -7.3(5) 57_656 . . 117_566 ?
C2 N2 C2 C2 -173.1(6) 173_646 . . 117_566 ?
C2 N2 C2 C2 125.7(7) 115_665 . . 117_566 ?
C2 N2 C2 C2 129(4) 39_646 . . 117_566 ?
C2 N2 C2 C2 106(4) 14_566 . . 117_566 ?
C2 N2 C2 C2 -170.0(5) 75_655 . . 117_566 ?
C2 N2 C2 C2 112.7(11) 130_556 . . 117_566 ?
C2 N2 C2 C2 -167.3(19) 66_566 . . 115_665 ?
C2 N2 C2 C2 175(4) 64_665 . . 115_665 ?
C2 N2 C2 C2 -166.9(7) 146_566 . . 115_665 ?
C2 N2 C2 C2 -135.3(8) 151_665 . . 115_665 ?
C2 N2 C2 C2 177(3) 167_656 . . 115_665 ?
C2 N2 C2 C2 -133.0(4) 57_656 . . 115_665 ?
C2 N2 C2 C2 61.2(13) 173_646 . . 115_665 ?
C2 N2 C2 C2 4(3) 39_646 . . 115_665 ?
C2 N2 C2 C2 -20(5) 14_566 . . 115_665 ?
C2 N2 C2 C2 64.3(6) 75_655 . . 115_665 ?
C2 N2 C2 C2 -13.0(17) 130_556 . . 115_665 ?
C2 N2 C2 C2 -148(6) 66_566 . . 14_566 ?
C2 N2 C2 C2 -165.5(8) 64_665 . . 14_566 ?
C2 N2 C2 C2 -147(5) 146_566 . . 14_566 ?
C2 N2 C2 C2 -115(4) 151_665 . . 14_566 ?
C2 N2 C2 C2 -163(2) 167_656 . . 14_566 ?
C2 N2 C2 C2 -113(4) 57_656 . . 14_566 ?
C2 N2 C2 C2 81(3) 173_646 . . 14_566 ?
C2 N2 C2 C2 20(5) 115_665 . . 14_566 ?
C2 N2 C2 C2 23(7) 39_646 . . 14_566 ?
C2 N2 C2 C2 84(4) 75_655 . . 14_566 ?
C2 N2 C2 C2 7(3) 130_556 . . 14_566 ?
C2 N2 C2 C2 -81(7) 66_566 . . 13_665 ?
C2 N2 C2 C2 -99.0(10) 64_665 . . 13_665 ?
C2 N2 C2 C2 -81(6) 146_566 . . 13_665 ?
C2 N2 C2 C2 -49(4) 151_665 . . 13_665 ?
C2 N2 C2 C2 -97(2) 167_656 . . 13_665 ?
C2 N2 C2 C2 -47(5) 57_656 . . 13_665 ?
C2 N2 C2 C2 148(4) 173_646 . . 13_665 ?
C2 N2 C2 C2 86(5) 115_665 . . 13_665 ?
C2 N2 C2 C2 90(8) 39_646 . . 13_665 ?
C2 N2 C2 C2 66.5(5) 14_566 . . 13_665 ?
C2 N2 C2 C2 151(5) 75_655 . . 13_665 ?
C2 N2 C2 C2 73(3) 130_556 . . 13_665 ?
C2 N2 C2 C2 -102.4(15) 66_566 . . 120 ?
C2 N2 C2 C2 -120(5) 64_665 . . 120 ?
C2 N2 C2 C2 -102.0(4) 146_566 . . 120 ?
C2 N2 C2 C2 -70.4(12) 151_665 . . 120 ?
C2 N2 C2 C2 -118(3) 167_656 . . 120 ?
C2 N2 C2 C2 -68.1(8) 57_656 . . 120 ?
C2 N2 C2 C2 126.1(16) 173_646 . . 120 ?
C2 N2 C2 C2 64.9(4) 115_665 . . 120 ?
C2 N2 C2 C2 69(3) 39_646 . . 120 ?
C2 N2 C2 C2 45(5) 14_566 . . 120 ?
C2 N2 C2 C2 129.2(8) 75_655 . . 120 ?
C2 N2 C2 C2 52(2) 130_556 . . 120 ?
C2 N2 C2 C2 92(3) 66_566 . . 188_545 ?
C2 N2 C2 C2 74(3) 64_665 . . 188_545 ?
C2 N2 C2 C2 92(2) 146_566 . . 188_545 ?
C2 N2 C2 C2 123.6(9) 151_665 . . 188_545 ?
C2 N2 C2 C2 75.8(10) 167_656 . . 188_545 ?
C2 N2 C2 C2 125.9(13) 57_656 . . 188_545 ?
C2 N2 C2 C2 -39.8(6) 173_646 . . 188_545 ?
C2 N2 C2 C2 -101.1(16) 115_665 . . 188_545 ?
C2 N2 C2 C2 -97(5) 39_646 . . 188_545 ?
C2 N2 C2 C2 -121(3) 14_566 . . 188_545 ?
C2 N2 C2 C2 -36.7(14) 75_655 . . 188_545 ?
C2 N2 C2 C2 -114.04(17) 130_556 . . 188_545 ?
C2 N2 C2 C2 128(2) 66_566 . . 75_655 ?
C2 N2 C2 C2 110(4) 64_665 . . 75_655 ?
C2 N2 C2 C2 128.7(8) 146_566 . . 75_655 ?
C2 N2 C2 C2 160.3(9) 151_665 . . 75_655 ?
C2 N2 C2 C2 112(2) 167_656 . . 75_655 ?
C2 N2 C2 C2 162.6(7) 57_656 . . 75_655 ?
C2 N2 C2 C2 -3.1(9) 173_646 . . 75_655 ?
C2 N2 C2 C2 -64.3(6) 115_665 . . 75_655 ?
C2 N2 C2 C2 -61(3) 39_646 . . 75_655 ?
C2 N2 C2 C2 -84(4) 14_566 . . 75_655 ?
C2 N2 C2 C2 -77.3(15) 130_556 . . 75_655 ?
C2 N2 C2 C2 -18(6) 64_665 . . 66_566 ?
C2 N2 C2 C2 0.4(14) 146_566 . . 66_566 ?
C2 N2 C2 C2 32(3) 151_665 . . 66_566 ?
C2 N2 C2 C2 -16(4) 167_656 . . 66_566 ?
C2 N2 C2 C2 34(2) 57_656 . . 66_566 ?
C2 N2 C2 C2 -131(3) 173_646 . . 66_566 ?
C2 N2 C2 C2 167.3(19) 115_665 . . 66_566 ?
C2 N2 C2 C2 171.0(12) 39_646 . . 66_566 ?
C2 N2 C2 C2 148(6) 14_566 . . 66_566 ?
C2 N2 C2 C2 -128(2) 75_655 . . 66_566 ?
C2 N2 C2 C2 154(4) 130_556 . . 66_566 ?
C2 N2 C2 C2 78.0(4) 66_566 . . 89_646 ?
C2 N2 C2 C2 60(6) 64_665 . . 89_646 ?
C2 N2 C2 C2 78.4(13) 146_566 . . 89_646 ?
C2 N2 C2 C2 110(2) 151_665 . . 89_646 ?
C2 N2 C2 C2 62(4) 167_656 . . 89_646 ?
C2 N2 C2 C2 112(2) 57_656 . . 89_646 ?
C2 N2 C2 C2 -53(3) 173_646 . . 89_646 ?
C2 N2 C2 C2 -114.7(17) 115_665 . . 89_646 ?
C2 N2 C2 C2 -111.1(13) 39_646 . . 89_646 ?
C2 N2 C2 C2 -135(6) 14_566 . . 89_646 ?
C2 N2 C2 C2 -50(2) 75_655 . . 89_646 ?
C2 N2 C2 C2 -128(3) 130_556 . . 89_646 ?
C2 N2 C2 C2 16(4) 66_566 . . 167_656 ?
C2 N2 C2 C2 -2.1(16) 64_665 . . 167_656 ?
C2 N2 C2 C2 16(3) 146_566 . . 167_656 ?
C2 N2 C2 C2 47.9(18) 151_665 . . 167_656 ?
C2 N2 C2 C2 50(2) 57_656 . . 167_656 ?
C2 N2 C2 C2 -115.6(13) 173_646 . . 167_656 ?
C2 N2 C2 C2 -177(3) 115_665 . . 167_656 ?
C2 N2 C2 C2 -173(5) 39_646 . . 167_656 ?
C2 N2 C2 C2 163(2) 14_566 . . 167_656 ?
C2 N2 C2 C2 -112(2) 75_655 . . 167_656 ?
C2 N2 C2 C2 170.2(9) 130_556 . . 167_656 ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.033
