# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_C2b
_database_code_depnum_ccdc_archive 'CCDC 1811950'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H26 Fe N8 O2, 2(F6 P)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C29 H26 F12 Fe N8 O2 P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         864.37
_chemical_compound_source        'see text'

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'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   9.917(2)
_cell_length_b                   10.983(3)
_cell_length_c                   16.365(3)
_cell_angle_alpha                98.138(9)
_cell_angle_beta                 92.420(9)
_cell_angle_gamma                105.842(9)
_cell_volume                     1691.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9604
_cell_measurement_theta_min      2.5772
_cell_measurement_theta_max      25.7233
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange

_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.124
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.650
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           10 s per frame
dx                                  34 mm
2167 frames measured in 6 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'FR591 rotating anode'
_diffrn_radiation_monochromator  'MONTEL mirror'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            52861
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             5957
# number of observed reflections (> n sig(I))
_reflns_number_gt                5427
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0371P)²+2.1210P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         5957
_refine_ls_number_parameters     553
_refine_ls_number_restraints     156
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.064

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.44967(3) 0.41285(3) 0.23692(2) 0.01215(9) Uani 1 1 d . U . . .
O1 O 0.34330(17) 0.00379(15) 0.24667(10) 0.0233(4) Uani 1 1 d . . . . .
O2 O 0.41661(19) -0.13992(18) 0.16114(11) 0.0351(4) Uani 1 1 d . . . . .
N1 N 0.30568(19) 0.17137(17) 0.12621(12) 0.0188(4) Uani 1 1 d . . . . .
N2 N 0.47270(19) 0.30361(17) 0.07750(11) 0.0169(4) Uani 1 1 d . . . . .
N3 N 0.59194(18) 0.49549(17) 0.15629(11) 0.0146(4) Uani 1 1 d . . . . .
N4 N 0.21118(18) 0.19554(17) 0.25888(12) 0.0188(4) Uani 1 1 d . . . . .
N5 N 0.27299(18) 0.35341(18) 0.35972(11) 0.0179(4) Uani 1 1 d . . . . .
N6 N 0.46140(18) 0.52593(17) 0.35168(11) 0.0152(4) Uani 1 1 d . . . . .
N7 N 0.59830(18) 0.35027(16) 0.27774(11) 0.0145(4) Uani 1 1 d . U . . .
N8 N 0.32111(18) 0.50100(16) 0.19982(11) 0.0153(4) Uani 1 1 d . U . . .
C1 C 0.4018(2) 0.2872(2) 0.14585(13) 0.0151(4) Uani 1 1 d . U . . .
C2 C 0.3175(3) 0.1163(2) 0.04485(15) 0.0265(5) Uani 1 1 d . . . . .
H2 H 0.2613 0.0357 0.0165 0.032 Uiso 1 1 calc R U . . .
C3 C 0.4219(3) 0.1978(2) 0.01448(15) 0.0246(5) Uani 1 1 d . . . . .
H3 H 0.4549 0.1865 -0.0389 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5770(2) 0.4206(2) 0.08192(13) 0.0158(4) Uani 1 1 d . . . . .
C5 C 0.6536(2) 0.4552(2) 0.01613(14) 0.0206(5) Uani 1 1 d . . . . .
H5 H 0.6381 0.3999 -0.0356 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7530(2) 0.5726(2) 0.02818(15) 0.0247(5) Uani 1 1 d . . . . .
H6 H 0.8066 0.6005 -0.0159 0.030 Uiso 1 1 calc R U . . .
C7 C 0.7747(2) 0.6497(2) 0.10452(16) 0.0247(5) Uani 1 1 d . . . . .
H7 H 0.8446 0.7301 0.1141 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6927(2) 0.6079(2) 0.16684(14) 0.0199(5) Uani 1 1 d . . . . .
H8 H 0.7084 0.6610 0.2195 0.024 Uiso 1 1 calc R U . . .
C9 C 0.2009(2) 0.1109(2) 0.17949(14) 0.0200(5) Uani 1 1 d . . . . .
H9 H 0.1053 0.0966 0.1511 0.024 Uiso 1 1 calc R U . . .
C10 C 0.3069(2) 0.3097(2) 0.28407(13) 0.0152(4) Uani 1 1 d . . . . .
C11 C 0.1183(2) 0.1682(2) 0.32040(16) 0.0272(5) Uani 1 1 d . . . . .
H11 H 0.0417 0.0932 0.3179 0.033 Uiso 1 1 calc R U . . .
C12 C 0.1563(2) 0.2660(2) 0.38332(16) 0.0268(5) Uani 1 1 d . . . . .
H12 H 0.1129 0.2742 0.4337 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3571(2) 0.4755(2) 0.39817(13) 0.0167(4) Uani 1 1 d . . . . .
C14 C 0.3348(3) 0.5356(2) 0.47428(14) 0.0232(5) Uani 1 1 d . . . . .
H14 H 0.2589 0.4973 0.5043 0.028 Uiso 1 1 calc R U . . .
C15 C 0.4277(3) 0.6538(2) 0.50491(15) 0.0266(5) Uani 1 1 d . . . . .
H15 H 0.4159 0.6987 0.5569 0.032 Uiso 1 1 calc R U . . .
C16 C 0.5370(3) 0.7067(2) 0.46029(14) 0.0258(5) Uani 1 1 d . . . . .
H16 H 0.6022 0.7872 0.4814 0.031 Uiso 1 1 calc R U . . .
C17 C 0.5502(2) 0.6405(2) 0.38409(14) 0.0197(5) Uani 1 1 d . . . . .
H17 H 0.6255 0.6776 0.3532 0.024 Uiso 1 1 calc R U . . .
C18 C 0.2172(2) -0.0185(2) 0.19321(16) 0.0250(5) Uani 1 1 d . . . . .
H18A H 0.1348 -0.0661 0.2191 0.030 Uiso 1 1 calc R U . . .
H18B H 0.2240 -0.0701 0.1396 0.030 Uiso 1 1 calc R U . . .
C19 C 0.4328(2) -0.0655(2) 0.22447(15) 0.0216(5) Uani 1 1 d . . . . .
C20 C 0.5512(2) -0.0391(2) 0.28940(14) 0.0196(5) Uani 1 1 d . . . . .
C21 C 0.5460(2) 0.0216(2) 0.36914(15) 0.0230(5) Uani 1 1 d . . . . .
H21 H 0.4667 0.0505 0.3832 0.028 Uiso 1 1 calc R U . . .
C22 C 0.6574(3) 0.0399(2) 0.42837(16) 0.0271(5) Uani 1 1 d . . . . .
H22 H 0.6551 0.0824 0.4828 0.032 Uiso 1 1 calc R U . . .
C23 C 0.7720(3) -0.0042(2) 0.40762(17) 0.0288(6) Uani 1 1 d . . . . .
H23 H 0.8478 0.0076 0.4481 0.035 Uiso 1 1 calc R U . . .
C24 C 0.7760(2) -0.0651(2) 0.32836(17) 0.0284(6) Uani 1 1 d . . . . .
H24 H 0.8543 -0.0958 0.3147 0.034 Uiso 1 1 calc R U . . .
C25 C 0.6667(2) -0.0818(2) 0.26868(16) 0.0242(5) Uani 1 1 d . . . . .
H25 H 0.6706 -0.1222 0.2139 0.029 Uiso 1 1 calc R U . . .
C26 C 0.6989(2) 0.3268(2) 0.29709(13) 0.0168(4) Uani 1 1 d . . . . .
C27 C 0.8284(2) 0.2988(2) 0.32205(15) 0.0231(5) Uani 1 1 d . . . . .
H27A H 0.8292 0.2151 0.2923 0.035 Uiso 1 1 calc R U . . .
H27B H 0.8341 0.2974 0.3818 0.035 Uiso 1 1 calc R U . . .
H27C H 0.9093 0.3651 0.3088 0.035 Uiso 1 1 calc R U . . .
C28 C 0.2389(2) 0.5500(2) 0.18199(13) 0.0166(4) Uani 1 1 d . . . . .
C29 C 0.1326(2) 0.6097(2) 0.15746(15) 0.0246(5) Uani 1 1 d . . . . .
H29A H 0.1587 0.6484 0.1079 0.037 Uiso 1 1 calc R U . . .
H29B H 0.1262 0.6763 0.2026 0.037 Uiso 1 1 calc R U . . .
H29C H 0.0413 0.5447 0.1453 0.037 Uiso 1 1 calc R U . . .
P1 P -0.0328(7) 0.2904(7) 0.6126(4) 0.0208(12) Uani 0.55(2) 1 d D U P A 1
F1 F 0.0222(10) 0.1798(9) 0.5634(5) 0.0485(17) Uani 0.55(2) 1 d D U P A 1
F2 F -0.0974(10) 0.2980(10) 0.5236(5) 0.0467(17) Uani 0.55(2) 1 d D U P A 1
F3 F -0.0847(11) 0.4054(9) 0.6567(6) 0.0294(16) Uani 0.55(2) 1 d D U P A 1
F4 F 0.1180(7) 0.3864(8) 0.6074(5) 0.0637(19) Uani 0.55(2) 1 d D U P A 1
F5 F 0.0264(13) 0.2644(13) 0.6997(5) 0.038(2) Uani 0.55(2) 1 d D U P A 1
F6 F -0.1813(9) 0.1936(10) 0.6237(6) 0.054(2) Uani 0.55(2) 1 d D U P A 1
P1A P -0.0391(10) 0.2796(10) 0.6114(6) 0.036(2) Uani 0.45(2) 1 d D U P A 2
F1A F -0.0267(17) 0.1404(12) 0.5741(7) 0.066(3) Uani 0.45(2) 1 d D U P A 2
F2A F -0.0679(17) 0.3291(15) 0.5267(6) 0.065(3) Uani 0.45(2) 1 d D U P A 2
F3A F -0.0488(16) 0.4149(11) 0.6562(9) 0.044(3) Uani 0.45(2) 1 d D U P A 2
F4A F 0.1214(8) 0.3376(18) 0.5989(6) 0.068(3) Uani 0.45(2) 1 d D U P A 2
F5A F -0.0023(17) 0.2446(15) 0.6994(7) 0.041(3) Uani 0.45(2) 1 d D U P A 2
F6A F -0.1985(10) 0.2207(13) 0.6207(9) 0.068(3) Uani 0.45(2) 1 d D U P A 2
P2 P 0.89182(6) 0.23657(6) 0.07805(4) 0.02055(14) Uani 1 1 d . . . . .
F7 F 0.74865(17) 0.18506(16) 0.02006(12) 0.0494(5) Uani 1 1 d . . . . .
F8 F 0.93762(16) 0.35446(16) 0.02848(10) 0.0383(4) Uani 1 1 d . . . . .
F9 F 0.9632(2) 0.15377(18) 0.01457(12) 0.0526(5) Uani 1 1 d . . . . .
F10 F 0.84813(19) 0.11877(16) 0.12675(12) 0.0509(5) Uani 1 1 d . . . . .
F11 F 0.82184(19) 0.32017(16) 0.14047(10) 0.0415(4) Uani 1 1 d . . . . .
F12 F 1.03677(17) 0.28964(14) 0.13428(11) 0.0446(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C10 1.829(2) . ?
Fe1 C1 1.830(2) . ?
Fe1 N7 1.9212(18) . ?
Fe1 N8 1.9252(18) . ?
Fe1 N6 2.0798(19) . ?
Fe1 N3 2.0863(18) . ?
O1 C19 1.348(3) . ?
O1 C18 1.438(3) . ?
O2 C19 1.201(3) . ?
N1 C1 1.352(3) . ?
N1 C2 1.406(3) . ?
N1 C9 1.465(3) . ?
N2 C1 1.353(3) . ?
N2 C3 1.402(3) . ?
N2 C4 1.402(3) . ?
N3 C8 1.343(3) . ?
N3 C4 1.347(3) . ?
N4 C10 1.347(3) . ?
N4 C11 1.402(3) . ?
N4 C9 1.469(3) . ?
N5 C10 1.353(3) . ?
N5 C12 1.395(3) . ?
N5 C13 1.412(3) . ?
N6 C17 1.344(3) . ?
N6 C13 1.353(3) . ?
N7 C26 1.140(3) . ?
N8 C28 1.141(3) . ?
C2 C3 1.336(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.381(3) . ?
C5 C6 1.375(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C18 1.520(3) . ?
C9 H9 1.0000 . ?
C11 C12 1.338(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C14 C15 1.382(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.488(3) . ?
C20 C21 1.388(3) . ?
C20 C25 1.389(3) . ?
C21 C22 1.390(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.389(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.456(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.456(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
P1 F3 1.584(7) . ?
P1 F2 1.589(7) . ?
P1 F4 1.591(7) . ?
P1 F1 1.594(7) . ?
P1 F6 1.598(7) . ?
P1 F5 1.610(7) . ?
P1A F6A 1.559(10) . ?
P1A F4A 1.579(9) . ?
P1A F3A 1.591(10) . ?
P1A F5A 1.595(10) . ?
P1A F2A 1.600(10) . ?
P1A F1A 1.603(9) . ?
P2 F11 1.5844(16) . ?
P2 F10 1.5849(17) . ?
P2 F12 1.5912(15) . ?
P2 F7 1.5913(16) . ?
P2 F8 1.5964(16) . ?
P2 F9 1.5979(17) . ?

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
C10 Fe1 C1 85.84(10) . . ?
C10 Fe1 N7 96.99(8) . . ?
C1 Fe1 N7 93.08(8) . . ?
C10 Fe1 N8 89.66(8) . . ?
C1 Fe1 N8 93.05(8) . . ?
N7 Fe1 N8 171.26(7) . . ?
C10 Fe1 N6 79.90(8) . . ?
C1 Fe1 N6 165.72(8) . . ?
N7 Fe1 N6 89.43(7) . . ?
N8 Fe1 N6 86.15(7) . . ?
C10 Fe1 N3 165.32(8) . . ?
C1 Fe1 N3 79.59(8) . . ?
N7 Fe1 N3 85.68(7) . . ?
N8 Fe1 N3 89.32(7) . . ?
N6 Fe1 N3 114.63(7) . . ?
C19 O1 C18 117.62(18) . . ?
C1 N1 C2 109.99(19) . . ?
C1 N1 C9 126.22(18) . . ?
C2 N1 C9 123.77(18) . . ?
C1 N2 C3 111.24(19) . . ?
C1 N2 C4 115.86(18) . . ?
C3 N2 C4 132.9(2) . . ?
C8 N3 C4 116.76(18) . . ?
C8 N3 Fe1 130.87(15) . . ?
C4 N3 Fe1 112.37(14) . . ?
C10 N4 C11 109.45(19) . . ?
C10 N4 C9 126.74(18) . . ?
C11 N4 C9 123.80(19) . . ?
C10 N5 C12 111.0(2) . . ?
C10 N5 C13 116.19(18) . . ?
C12 N5 C13 132.8(2) . . ?
C17 N6 C13 116.65(19) . . ?
C17 N6 Fe1 130.69(15) . . ?
C13 N6 Fe1 112.59(14) . . ?
C26 N7 Fe1 170.15(17) . . ?
C28 N8 Fe1 175.17(18) . . ?
N1 C1 N2 105.12(18) . . ?
N1 C1 Fe1 135.51(17) . . ?
N2 C1 Fe1 119.37(15) . . ?
C3 C2 N1 107.7(2) . . ?
C3 C2 H2 126.2 . . ?
N1 C2 H2 126.2 . . ?
C2 C3 N2 106.0(2) . . ?
C2 C3 H3 127.0 . . ?
N2 C3 H3 127.0 . . ?
N3 C4 C5 124.1(2) . . ?
N3 C4 N2 112.77(18) . . ?
C5 C4 N2 123.1(2) . . ?
C6 C5 C4 117.7(2) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
C5 C6 C7 119.7(2) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 118.8(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N3 C8 C7 122.9(2) . . ?
N3 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
N1 C9 N4 110.44(17) . . ?
N1 C9 C18 111.01(19) . . ?
N4 C9 C18 110.80(19) . . ?
N1 C9 H9 108.2 . . ?
N4 C9 H9 108.2 . . ?
C18 C9 H9 108.2 . . ?
N4 C10 N5 105.65(18) . . ?
N4 C10 Fe1 135.11(17) . . ?
N5 C10 Fe1 119.00(16) . . ?
C12 C11 N4 108.1(2) . . ?
C12 C11 H11 126.0 . . ?
N4 C11 H11 126.0 . . ?
C11 C12 N5 105.8(2) . . ?
C11 C12 H12 127.1 . . ?
N5 C12 H12 127.1 . . ?
N6 C13 C14 124.3(2) . . ?
N6 C13 N5 112.03(18) . . ?
C14 C13 N5 123.7(2) . . ?
C13 C14 C15 117.2(2) . . ?
C13 C14 H14 121.4 . . ?
C15 C14 H14 121.4 . . ?
C16 C15 C14 120.2(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 118.8(2) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
N6 C17 C16 123.0(2) . . ?
N6 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
O1 C18 C9 108.01(17) . . ?
O1 C18 H18A 110.1 . . ?
C9 C18 H18A 110.1 . . ?
O1 C18 H18B 110.1 . . ?
C9 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
O2 C19 O1 123.9(2) . . ?
O2 C19 C20 125.1(2) . . ?
O1 C19 C20 110.92(19) . . ?
C21 C20 C25 120.3(2) . . ?
C21 C20 C19 122.0(2) . . ?
C25 C20 C19 117.6(2) . . ?
C20 C21 C22 119.7(2) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 119.7(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.4(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C20 119.6(2) . . ?
C24 C25 H25 120.2 . . ?
C20 C25 H25 120.2 . . ?
N7 C26 C27 179.2(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N8 C28 C29 178.5(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F3 P1 F2 93.3(6) . . ?
F3 P1 F4 90.2(5) . . ?
F2 P1 F4 96.5(5) . . ?
F3 P1 F1 176.3(6) . . ?
F2 P1 F1 83.9(6) . . ?
F4 P1 F1 87.7(4) . . ?
F3 P1 F6 89.3(6) . . ?
F2 P1 F6 87.1(5) . . ?
F4 P1 F6 176.4(6) . . ?
F1 P1 F6 93.0(5) . . ?
F3 P1 F5 92.0(6) . . ?
F2 P1 F5 173.2(7) . . ?
F4 P1 F5 87.8(6) . . ?
F1 P1 F5 91.0(6) . . ?
F6 P1 F5 88.7(6) . . ?
F6A P1A F4A 178.2(9) . . ?
F6A P1A F3A 89.7(8) . . ?
F4A P1A F3A 91.3(7) . . ?
F6A P1A F5A 89.4(8) . . ?
F4A P1A F5A 92.0(7) . . ?
F3A P1A F5A 89.5(8) . . ?
F6A P1A F2A 93.6(8) . . ?
F4A P1A F2A 85.0(7) . . ?
F3A P1A F2A 85.8(8) . . ?
F5A P1A F2A 174.3(11) . . ?
F6A P1A F1A 90.0(7) . . ?
F4A P1A F1A 89.0(6) . . ?
F3A P1A F1A 175.0(9) . . ?
F5A P1A F1A 85.5(8) . . ?
F2A P1A F1A 99.2(10) . . ?
F11 P2 F10 91.92(10) . . ?
F11 P2 F12 90.26(10) . . ?
F10 P2 F12 89.91(10) . . ?
F11 P2 F7 90.37(10) . . ?
F10 P2 F7 91.30(10) . . ?
F12 P2 F7 178.62(11) . . ?
F11 P2 F8 88.84(9) . . ?
F10 P2 F8 179.17(10) . . ?
F12 P2 F8 89.76(9) . . ?
F7 P2 F8 89.03(10) . . ?
F11 P2 F9 179.29(11) . . ?
F10 P2 F9 88.78(11) . . ?
F12 P2 F9 89.65(10) . . ?
F7 P2 F9 89.70(10) . . ?
F8 P2 F9 90.46(10) . . ?

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 N1 C1 N2 -0.2(2) . . . . ?
C9 N1 C1 N2 -178.69(18) . . . . ?
C2 N1 C1 Fe1 179.74(18) . . . . ?
C9 N1 C1 Fe1 1.2(3) . . . . ?
C3 N2 C1 N1 -0.2(2) . . . . ?
C4 N2 C1 N1 178.13(16) . . . . ?
C3 N2 C1 Fe1 179.84(14) . . . . ?
C4 N2 C1 Fe1 -1.8(2) . . . . ?
C10 Fe1 C1 N1 -1.2(2) . . . . ?
N7 Fe1 C1 N1 95.6(2) . . . . ?
N8 Fe1 C1 N1 -90.6(2) . . . . ?
N6 Fe1 C1 N1 -4.3(5) . . . . ?
N3 Fe1 C1 N1 -179.4(2) . . . . ?
C10 Fe1 C1 N2 178.71(17) . . . . ?
N7 Fe1 C1 N2 -84.50(16) . . . . ?
N8 Fe1 C1 N2 89.28(16) . . . . ?
N6 Fe1 C1 N2 175.7(2) . . . . ?
N3 Fe1 C1 N2 0.53(15) . . . . ?
C1 N1 C2 C3 0.5(3) . . . . ?
C9 N1 C2 C3 179.1(2) . . . . ?
N1 C2 C3 N2 -0.6(3) . . . . ?
C1 N2 C3 C2 0.6(3) . . . . ?
C4 N2 C3 C2 -177.4(2) . . . . ?
C8 N3 C4 C5 -3.2(3) . . . . ?
Fe1 N3 C4 C5 176.92(16) . . . . ?
C8 N3 C4 N2 177.99(18) . . . . ?
Fe1 N3 C4 N2 -1.9(2) . . . . ?
C1 N2 C4 N3 2.4(2) . . . . ?
C3 N2 C4 N3 -179.7(2) . . . . ?
C1 N2 C4 C5 -176.44(19) . . . . ?
C3 N2 C4 C5 1.5(4) . . . . ?
N3 C4 C5 C6 1.3(3) . . . . ?
N2 C4 C5 C6 -179.98(19) . . . . ?
C4 C5 C6 C7 1.1(3) . . . . ?
C5 C6 C7 C8 -1.5(3) . . . . ?
C4 N3 C8 C7 2.7(3) . . . . ?
Fe1 N3 C8 C7 -177.40(16) . . . . ?
C6 C7 C8 N3 -0.4(3) . . . . ?
C1 N1 C9 N4 1.3(3) . . . . ?
C2 N1 C9 N4 -176.99(19) . . . . ?
C1 N1 C9 C18 -122.0(2) . . . . ?
C2 N1 C9 C18 59.7(3) . . . . ?
C10 N4 C9 N1 -3.9(3) . . . . ?
C11 N4 C9 N1 175.26(19) . . . . ?
C10 N4 C9 C18 119.5(2) . . . . ?
C11 N4 C9 C18 -61.3(3) . . . . ?
C11 N4 C10 N5 -0.8(2) . . . . ?
C9 N4 C10 N5 178.50(18) . . . . ?
C11 N4 C10 Fe1 -174.74(18) . . . . ?
C9 N4 C10 Fe1 4.5(3) . . . . ?
C12 N5 C10 N4 0.8(2) . . . . ?
C13 N5 C10 N4 -178.03(16) . . . . ?
C12 N5 C10 Fe1 175.99(15) . . . . ?
C13 N5 C10 Fe1 -2.9(2) . . . . ?
C1 Fe1 C10 N4 -1.6(2) . . . . ?
N7 Fe1 C10 N4 -94.2(2) . . . . ?
N8 Fe1 C10 N4 91.5(2) . . . . ?
N6 Fe1 C10 N4 177.6(2) . . . . ?
N3 Fe1 C10 N4 5.5(5) . . . . ?
C1 Fe1 C10 N5 -174.99(17) . . . . ?
N7 Fe1 C10 N5 92.41(16) . . . . ?
N8 Fe1 C10 N5 -81.90(16) . . . . ?
N6 Fe1 C10 N5 4.24(15) . . . . ?
N3 Fe1 C10 N5 -167.9(2) . . . . ?
C10 N4 C11 C12 0.4(3) . . . . ?
C9 N4 C11 C12 -178.9(2) . . . . ?
N4 C11 C12 N5 0.1(3) . . . . ?
C10 N5 C12 C11 -0.6(3) . . . . ?
C13 N5 C12 C11 178.0(2) . . . . ?
C17 N6 C13 C14 2.0(3) . . . . ?
Fe1 N6 C13 C14 -175.24(17) . . . . ?
C17 N6 C13 N5 -177.97(17) . . . . ?
Fe1 N6 C13 N5 4.8(2) . . . . ?
C10 N5 C13 N6 -1.7(2) . . . . ?
C12 N5 C13 N6 179.7(2) . . . . ?
C10 N5 C13 C14 178.35(19) . . . . ?
C12 N5 C13 C14 -0.2(4) . . . . ?
N6 C13 C14 C15 -1.3(3) . . . . ?
N5 C13 C14 C15 178.6(2) . . . . ?
C13 C14 C15 C16 -0.3(3) . . . . ?
C14 C15 C16 C17 1.1(3) . . . . ?
C13 N6 C17 C16 -1.1(3) . . . . ?
Fe1 N6 C17 C16 175.57(16) . . . . ?
C15 C16 C17 N6 -0.5(3) . . . . ?
C19 O1 C18 C9 -132.8(2) . . . . ?
N1 C9 C18 O1 71.5(2) . . . . ?
N4 C9 C18 O1 -51.6(2) . . . . ?
C18 O1 C19 O2 3.6(3) . . . . ?
C18 O1 C19 C20 -175.26(18) . . . . ?
O2 C19 C20 C21 -163.2(2) . . . . ?
O1 C19 C20 C21 15.6(3) . . . . ?
O2 C19 C20 C25 14.3(3) . . . . ?
O1 C19 C20 C25 -166.8(2) . . . . ?
C25 C20 C21 C22 0.2(3) . . . . ?
C19 C20 C21 C22 177.7(2) . . . . ?
C20 C21 C22 C23 -0.9(3) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C22 C23 C24 C25 0.6(4) . . . . ?
C23 C24 C25 C20 -1.3(3) . . . . ?
C21 C20 C25 C24 0.9(3) . . . . ?
C19 C20 C25 C24 -176.7(2) . . . . ?


####################################################################### 
# 
# 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_C1
_database_code_depnum_ccdc_archive 'CCDC 1811952'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H38 Ag3 N14 O2, 2.993(F6 P), 2(C2 H3 N)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C44 H44 Ag3 F17.96 N16 O2 P3'
_chemical_formula_iupac          ?
_chemical_formula_weight         1586.46
_chemical_compound_source        'see text'

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'
Ag Ag -0.8971 1.1015 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_Int_Tables_number      33

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

_cell_length_a                   12.6724(6)
_cell_length_b                   16.1107(7)
_cell_length_c                   27.7100(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5657.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      2.5184
_cell_measurement_theta_max      25.7114
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colourless'

_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.129
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             3134
_exptl_absorpt_coefficient_mu    1.226
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.5152
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           60 s per frame
dx                                  56 mm
1935 frames measured in 5 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph monochromator'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Apex II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            52753
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             9984
# number of observed reflections (> n sig(I))
_reflns_number_gt                8019
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0306P)²+32.0498P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed


_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.51(5)

_chemical_absolute_configuration unk

_refine_ls_number_reflns         9984
_refine_ls_number_parameters     901
_refine_ls_number_restraints     1126
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1126
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.006
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.149

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.08429(7) 0.58136(6) 0.44926(7) 0.0147(2) Uani 1 1 d . . . . .
H1 H -0.152(4) 0.687(5) 0.594(3) 0.018 Uiso 1 1 d D U . . .
Ag2 Ag 0.30251(8) 0.57780(6) 0.52733(7) 0.0166(2) Uani 1 1 d . . . . .
Ag3 Ag 0.19795(9) 0.43586(6) 0.48405(7) 0.0201(2) Uani 1 1 d . . . . .
O1 O -0.1005(7) 0.7103(6) 0.6078(4) 0.027(2) Uani 1 1 d D . . . .
O2 O 0.4770(7) 0.7518(5) 0.4433(4) 0.024(2) Uani 1 1 d D . . . .
N1 N 0.0024(8) 0.5790(7) 0.5540(4) 0.0147(2) Uani 1 1 d . . . . .
N2 N -0.0429(8) 0.4672(6) 0.5196(4) 0.0143(9) Uani 1 1 d . U . . .
N3 N 0.0333(8) 0.3820(7) 0.4610(4) 0.0168(13) Uani 1 1 d . U . . .
N4 N 0.1335(9) 0.6517(7) 0.6002(4) 0.020(3) Uani 1 1 d . . . . .
H4 H 0.521(4) 0.713(3) 0.445(5) 0.024 Uiso 1 1 d D U . . .
N5 N 0.2800(9) 0.6227(7) 0.6341(4) 0.018(3) Uani 1 1 d . . . . .
N6 N 0.4272(9) 0.5498(7) 0.6063(4) 0.023(3) Uani 1 1 d . . . . .
N7 N 0.2590(9) 0.6533(7) 0.3769(4) 0.0152(8) Uani 1 1 d . U . . .
N8 N 0.1114(9) 0.6241(7) 0.3428(4) 0.0153(8) Uani 1 1 d . U . . .
N9 N -0.0382(9) 0.5582(7) 0.3723(4) 0.021(3) Uani 1 1 d . . . . .
N10 N 0.3922(9) 0.5867(7) 0.4235(4) 0.0166(8) Uani 1 1 d . U . . .
N11 N 0.4429(8) 0.4747(6) 0.4565(4) 0.0165(7) Uani 1 1 d . U . . .
N12 N 0.3642(9) 0.3839(7) 0.5108(4) 0.0173(9) Uani 1 1 d . U . . .
C1 C 0.0158(10) 0.5354(8) 0.5124(5) 0.0147(2) Uani 1 1 d . U . . .
C2 C -0.0582(10) 0.5355(8) 0.5876(5) 0.0147(2) Uani 1 1 d . . . . .
H2 H -0.0731 0.5514 0.6199 0.018 Uiso 1 1 calc R U . . .
C3 C -0.0913(10) 0.4661(8) 0.5647(5) 0.0147(2) Uani 1 1 d . . . . .
H3 H -0.1380 0.4250 0.5770 0.018 Uiso 1 1 calc R U . . .
C4 C -0.0560(10) 0.4029(8) 0.4845(5) 0.0147(2) Uani 1 1 d . . . . .
C5 C -0.1506(10) 0.3668(7) 0.4770(5) 0.0155(9) Uani 1 1 d . U . . .
H5 H -0.2107 0.3842 0.4948 0.019 Uiso 1 1 calc R U . . .
C6 C -0.1592(10) 0.3044(7) 0.4433(5) 0.0147(2) Uani 1 1 d . U . . .
H6 H -0.2247 0.2771 0.4380 0.018 Uiso 1 1 calc R U . . .
C7 C -0.0706(10) 0.2821(8) 0.4171(5) 0.0162(8) Uani 1 1 d . U . . .
H7 H -0.0746 0.2404 0.3929 0.019 Uiso 1 1 calc R U . . .
C8 C 0.0234(11) 0.3214(8) 0.4269(5) 0.0168(11) Uani 1 1 d . U . . .
H8 H 0.0842 0.3057 0.4090 0.020 Uiso 1 1 calc R U . . .
C9 C 0.0525(11) 0.6600(8) 0.5619(5) 0.017(3) Uani 1 1 d . . . . .
H9 H 0.0909 0.6742 0.5315 0.021 Uiso 1 1 calc R U . . .
C10 C 0.2315(11) 0.6231(8) 0.5906(5) 0.0166(2) Uani 1 1 d . . . . .
C11 C 0.1218(12) 0.6685(9) 0.6492(5) 0.022(3) Uani 1 1 d . . . . .
H11 H 0.0600 0.6887 0.6646 0.027 Uiso 1 1 calc R U . . .
C12 C 0.2136(10) 0.6508(8) 0.6706(5) 0.0147(2) Uani 1 1 d . . . . .
H12 H 0.2301 0.6563 0.7039 0.018 Uiso 1 1 calc R U . . .
C13 C 0.3884(11) 0.6020(9) 0.6399(5) 0.020(3) Uani 1 1 d . . . . .
C14 C 0.4486(11) 0.6354(9) 0.6769(6) 0.025(4) Uani 1 1 d . . . . .
H14 H 0.4191 0.6727 0.6998 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5522(12) 0.6124(10) 0.6790(6) 0.032(2) Uani 1 1 d . U . . .
H15 H 0.5958 0.6342 0.7039 0.038 Uiso 1 1 calc R U . . .
C16 C 0.5950(13) 0.5583(10) 0.6460(6) 0.031(2) Uani 1 1 d . U . . .
H16 H 0.6667 0.5414 0.6479 0.038 Uiso 1 1 calc R U . . .
C17 C 0.5301(13) 0.5301(10) 0.6105(6) 0.031(2) Uani 1 1 d . U . . .
H17 H 0.5595 0.4940 0.5869 0.038 Uiso 1 1 calc R U . . .
C18 C -0.0262(12) 0.7281(9) 0.5704(6) 0.025(3) Uani 1 1 d . . . . .
H18A H 0.0122 0.7796 0.5787 0.030 Uiso 1 1 calc R U . . .
H18B H -0.0652 0.7384 0.5400 0.030 Uiso 1 1 calc R U . . .
C19 C 0.1594(10) 0.6259(8) 0.3867(5) 0.0147(2) Uani 1 1 d . U . . .
C20 C 0.2708(11) 0.6644(8) 0.3271(5) 0.0156(9) Uani 1 1 d . U . . .
H20 H 0.3334 0.6819 0.3113 0.019 Uiso 1 1 calc R U . . .
C21 C 0.1814(11) 0.6465(9) 0.3060(5) 0.0155(9) Uani 1 1 d . U . . .
H21 H 0.1669 0.6483 0.2724 0.019 Uiso 1 1 calc R U . . .
C22 C 0.0028(11) 0.6037(8) 0.3362(5) 0.017(3) Uani 1 1 d . . . . .
C23 C -0.0551(11) 0.6347(9) 0.2980(5) 0.022(4) Uani 1 1 d . . . . .
H23 H -0.0229 0.6674 0.2735 0.026 Uiso 1 1 calc R U . . .
C24 C -0.1613(13) 0.6161(9) 0.2967(6) 0.027(2) Uani 1 1 d . U . . .
H24 H -0.2034 0.6353 0.2706 0.032 Uiso 1 1 calc R U . . .
C25 C -0.2073(12) 0.5694(9) 0.3335(5) 0.027(2) Uani 1 1 d . U . . .
H25 H -0.2806 0.5569 0.3335 0.032 Uiso 1 1 calc R U . . .
C26 C -0.1417(12) 0.5422(9) 0.3701(6) 0.026(2) Uani 1 1 d . U . . .
H26 H -0.1720 0.5101 0.3953 0.032 Uiso 1 1 calc R U . . .
C27 C 0.3363(11) 0.6643(8) 0.4145(5) 0.0166(2) Uani 1 1 d . . . . .
H27 H 0.2974 0.6789 0.4448 0.020 Uiso 1 1 calc R U . . .
C28 C 0.3799(11) 0.5414(8) 0.4636(5) 0.0166(2) Uani 1 1 d . U . . .
C29 C 0.4662(10) 0.5503(8) 0.3923(5) 0.0170(9) Uani 1 1 d . U . . .
H29 H 0.4899 0.5716 0.3623 0.020 Uiso 1 1 calc R U . . .
C30 C 0.4963(11) 0.4808(8) 0.4130(5) 0.0169(9) Uani 1 1 d . U . . .
H30 H 0.5456 0.4419 0.4005 0.020 Uiso 1 1 calc R U . . .
C31 C 0.4538(11) 0.4082(8) 0.4898(5) 0.0168(7) Uani 1 1 d . U . . .
C32 C 0.5513(11) 0.3761(8) 0.4999(5) 0.0171(7) Uani 1 1 d . U . . .
H32 H 0.6126 0.3961 0.4839 0.020 Uiso 1 1 calc R U . . .
C33 C 0.5579(10) 0.3132(8) 0.5344(5) 0.0166(2) Uani 1 1 d . U . . .
H33 H 0.6238 0.2881 0.5418 0.020 Uiso 1 1 calc R U . . .
C34 C 0.4679(11) 0.2884(8) 0.5571(5) 0.0178(8) Uani 1 1 d . U . . .
H34 H 0.4706 0.2465 0.5812 0.021 Uiso 1 1 calc R U . . .
C35 C 0.3728(11) 0.3245(8) 0.5449(5) 0.0179(9) Uani 1 1 d . U . . .
H35 H 0.3109 0.3068 0.5612 0.021 Uiso 1 1 calc R U . . .
C36 C 0.4115(11) 0.7367(8) 0.4030(5) 0.0166(2) Uani 1 1 d . . . . .
H36A H 0.4554 0.7226 0.3746 0.020 Uiso 1 1 calc R U . . .
H36B H 0.3702 0.7871 0.3953 0.020 Uiso 1 1 calc R U . . .
P1 P 0.7045(6) 0.6285(4) 0.4943(3) 0.0287(9) Uani 0.663(15) 1 d D U P A 5
F1 F 0.7035(11) 0.5315(6) 0.4880(7) 0.0330(15) Uani 0.663(15) 1 d D U P A 5
F2 F 0.7056(11) 0.7278(6) 0.5029(5) 0.0319(14) Uani 0.663(15) 1 d D U P A 5
F3 F 0.7353(10) 0.6187(9) 0.5510(4) 0.0310(15) Uani 0.663(15) 1 d D U P A 5
F4 F 0.8252(7) 0.6302(8) 0.4798(5) 0.0333(15) Uani 0.663(15) 1 d D U P A 5
F5 F 0.6706(9) 0.6448(10) 0.4392(4) 0.0314(15) Uani 0.663(15) 1 d D U P A 5
F6 F 0.5817(8) 0.6272(8) 0.5091(5) 0.0328(15) Uani 0.663(15) 1 d D U P A 5
P1A P 0.6992(9) 0.6271(7) 0.4983(4) 0.0297(10) Uani 0.337(15) 1 d D U P A 6
F1A F 0.7085(18) 0.5335(9) 0.5138(10) 0.0311(16) Uani 0.337(15) 1 d D U P A 6
F2A F 0.6889(19) 0.7244(9) 0.4846(9) 0.0314(16) Uani 0.337(15) 1 d D U P A 6
F3A F 0.7158(18) 0.6565(16) 0.5539(5) 0.0310(16) Uani 0.337(15) 1 d D U P A 6
F4A F 0.8223(11) 0.6300(13) 0.4892(8) 0.0321(17) Uani 0.337(15) 1 d D U P A 6
F5A F 0.6784(17) 0.6044(16) 0.4425(6) 0.0317(16) Uani 0.337(15) 1 d D U P A 6
F6A F 0.5738(11) 0.6245(13) 0.5075(7) 0.0320(16) Uani 0.337(15) 1 d D U P A 6
P2 P 0.7290(3) 0.3183(3) 0.67073(15) 0.0286(10) Uani 1 1 d . . . . .
F7 F 0.6861(8) 0.3916(7) 0.7045(4) 0.057(3) Uani 1 1 d . . . . .
F8 F 0.7724(9) 0.2461(9) 0.6382(4) 0.084(4) Uani 1 1 d . . . . .
F9 F 0.7257(9) 0.2585(6) 0.7157(3) 0.055(3) Uani 1 1 d . . . . .
F10 F 0.8471(7) 0.3430(7) 0.6856(4) 0.059(3) Uani 1 1 d . . . . .
F11 F 0.7298(10) 0.3796(9) 0.6259(4) 0.088(5) Uani 1 1 d . . . . .
F12 F 0.6127(8) 0.2911(7) 0.6574(4) 0.060(3) Uani 1 1 d . . . . .
P3 P 0.6682(8) 0.3324(7) 0.3159(4) 0.0318(12) Uani 0.500(12) 1 d D U P B 1
F13 F 0.6906(15) 0.3892(11) 0.3624(5) 0.0321(14) Uani 0.500(12) 1 d D U P B 1
F14 F 0.6495(14) 0.2713(10) 0.2706(5) 0.0322(14) Uani 0.500(12) 1 d D U P B 1
F15 F 0.7078(16) 0.2529(10) 0.3458(7) 0.0318(14) Uani 0.500(12) 1 d D U P B 1
F16 F 0.5513(12) 0.3178(10) 0.3341(8) 0.0322(13) Uani 0.500(12) 1 d D U P B 1
F17 F 0.6267(16) 0.4104(9) 0.2863(6) 0.0324(14) Uani 0.500(12) 1 d D U P B 1
F18 F 0.7834(13) 0.3532(12) 0.2955(7) 0.0323(13) Uani 0.500(12) 1 d D U P B 1
P3A P 0.6644(11) 0.3418(9) 0.3163(5) 0.0319(12) Uani 0.253(11) 1 d D U P C 2
F13A F 0.714(2) 0.3976(15) 0.3585(8) 0.0320(14) Uani 0.253(11) 1 d D U P C 2
F14A F 0.619(2) 0.2830(15) 0.2740(8) 0.0322(14) Uani 0.253(11) 1 d D U P C 2
F15A F 0.747(2) 0.2697(16) 0.3290(11) 0.0321(13) Uani 0.253(11) 1 d D U P C 2
F16A F 0.583(2) 0.3047(16) 0.3537(9) 0.0321(13) Uani 0.253(11) 1 d D U P C 2
F17A F 0.581(2) 0.4124(14) 0.3042(11) 0.0322(13) Uani 0.253(11) 1 d D U P C 2
F18A F 0.741(3) 0.3855(19) 0.2781(9) 0.0321(13) Uani 0.253(11) 1 d D U P C 2
P3B P 0.6788(12) 0.3335(11) 0.3121(6) 0.0319(12) Uani 0.240(11) 1 d D U P D 3
F13B F 0.679(2) 0.3964(17) 0.3570(8) 0.0320(14) Uani 0.240(11) 1 d D U P D 3
F14B F 0.686(2) 0.2715(17) 0.2665(9) 0.0321(13) Uani 0.240(11) 1 d D U P D 3
F15B F 0.8043(16) 0.3241(19) 0.3174(11) 0.0321(13) Uani 0.240(11) 1 d D U P D 3
F16B F 0.661(2) 0.2580(17) 0.3478(10) 0.0321(14) Uani 0.240(11) 1 d D U P D 3
F17B F 0.5541(16) 0.3407(19) 0.3072(11) 0.0322(13) Uani 0.240(11) 1 d D U P D 3
F18B F 0.687(3) 0.4107(15) 0.2759(10) 0.0321(14) Uani 0.240(11) 1 d D U P D 3
N13 N 0.1492(11) 0.3981(9) 0.5729(5) 0.039(3) Uani 1 1 d . U . . .
C37 C 0.1295(13) 0.4067(11) 0.6130(7) 0.039(2) Uani 1 1 d . U . . .
C38 C 0.1026(13) 0.4160(11) 0.6634(6) 0.040(3) Uani 1 1 d . U . . .
H38A H 0.0264 0.4089 0.6675 0.060 Uiso 1 1 calc R U . . .
H38B H 0.1233 0.4715 0.6744 0.060 Uiso 1 1 calc R U . . .
H38C H 0.1400 0.3740 0.6824 0.060 Uiso 1 1 calc R U . . .
N14 N 0.2468(10) 0.4133(9) 0.3944(5) 0.035(2) Uani 1 1 d . U . . .
C39 C 0.2777(12) 0.4156(11) 0.3565(6) 0.035(2) Uani 1 1 d . U . . .
C40 C 0.3173(12) 0.4154(11) 0.3069(6) 0.036(3) Uani 1 1 d . U . . .
H40A H 0.3015 0.3619 0.2918 0.054 Uiso 1 1 calc R U . . .
H40B H 0.3939 0.4243 0.3072 0.054 Uiso 1 1 calc R U . . .
H40C H 0.2832 0.4600 0.2886 0.054 Uiso 1 1 calc R U . . .
N15 N 0.0935(17) 0.4332(12) 0.2116(8) 0.085(5) Uani 1 1 d . U . . .
C41 C 0.055(2) 0.4149(15) 0.2479(10) 0.084(5) Uani 1 1 d . U . . .
N16 N 0.5356(10) 0.6595(9) 0.2899(5) 0.038(3) Uani 1 1 d . U . . .
C43 C 0.5558(13) 0.6338(11) 0.2533(7) 0.038(2) Uani 1 1 d . U . . .
C42 C 0.016(2) 0.3919(14) 0.2943(9) 0.083(5) Uani 1 1 d . U . . .
H42A H 0.0751 0.3728 0.3144 0.125 Uiso 1 1 calc R U . . .
H42B H -0.0353 0.3471 0.2907 0.125 Uiso 1 1 calc R U . . .
H42C H -0.0173 0.4400 0.3095 0.125 Uiso 1 1 calc R U . . .
C44 C 0.5829(12) 0.6001(11) 0.2063(6) 0.040(3) Uani 1 1 d . U . . .
H44A H 0.5197 0.5766 0.1912 0.059 Uiso 1 1 calc R U . . .
H44B H 0.6363 0.5566 0.2101 0.059 Uiso 1 1 calc R U . . .
H44C H 0.6111 0.6445 0.1858 0.059 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 C1 2.089(13) . ?
Ag1 C19 2.105(13) . ?
Ag1 Ag3 2.9153(14) . ?
Ag2 C10 2.100(14) . ?
Ag2 C28 2.104(13) . ?
Ag2 Ag3 2.9024(14) . ?
Ag3 N3 2.348(11) . ?
Ag3 N12 2.385(11) . ?
Ag3 N14 2.585(14) . ?
Ag3 N13 2.611(14) . ?
O1 C18 1.430(17) . ?
O1 H1 0.8400(16) . ?
O2 C36 1.414(16) . ?
O2 H4 0.8400(17) . ?
N1 C1 1.360(17) . ?
N1 C2 1.395(17) . ?
N1 C9 1.468(17) . ?
N2 C1 1.342(16) . ?
N2 C3 1.393(17) . ?
N2 C4 1.431(16) . ?
N3 C4 1.349(16) . ?
N3 C8 1.365(16) . ?
N4 C10 1.351(18) . ?
N4 C11 1.391(17) . ?
N4 C9 1.484(17) . ?
N5 C10 1.355(18) . ?
N5 C12 1.390(17) . ?
N5 C13 1.422(18) . ?
N6 C13 1.346(18) . ?
N6 C17 1.347(19) . ?
N7 C19 1.365(17) . ?
N7 C20 1.398(17) . ?
N7 C27 1.442(17) . ?
N8 C19 1.361(17) . ?
N8 C21 1.397(18) . ?
N8 C22 1.426(18) . ?
N9 C26 1.338(18) . ?
N9 C22 1.344(18) . ?
N10 C28 1.340(16) . ?
N10 C29 1.403(17) . ?
N10 C27 1.457(17) . ?
N11 C28 1.352(16) . ?
N11 C30 1.385(17) . ?
N11 C31 1.421(16) . ?
N12 C31 1.336(17) . ?
N12 C35 1.348(16) . ?
C2 C3 1.352(18) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.349(17) . ?
C5 C6 1.377(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.376(18) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C18 1.500(19) . ?
C9 H9 1.0000 . ?
C11 C12 1.335(19) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.39(2) . ?
C14 C15 1.37(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.38(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.36(2) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 C21 1.306(19) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.382(19) . ?
C23 C24 1.38(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.40(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.38(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C36 1.540(18) . ?
C27 H27 1.0000 . ?
C29 C30 1.315(18) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.368(19) . ?
C32 C33 1.396(19) . ?
C32 H32 0.9500 . ?
C33 C34 1.362(18) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(19) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
P1 F1 1.573(10) . ?
P1 F4 1.581(9) . ?
P1 F6 1.610(9) . ?
P1 F5 1.610(11) . ?
P1 F2 1.617(9) . ?
P1 F3 1.625(11) . ?
P1A F1A 1.573(10) . ?
P1A F4A 1.581(9) . ?
P1A F5A 1.609(12) . ?
P1A F6A 1.610(9) . ?
P1A F2A 1.617(9) . ?
P1A F3A 1.625(11) . ?
P2 F8 1.570(11) . ?
P2 F9 1.575(10) . ?
P2 F12 1.581(10) . ?
P2 F11 1.588(11) . ?
P2 F7 1.602(11) . ?
P2 F10 1.603(10) . ?
P3 F16 1.583(14) . ?
P3 F17 1.590(14) . ?
P3 F18 1.600(14) . ?
P3 F13 1.604(11) . ?
P3 F15 1.605(15) . ?
P3 F14 1.614(11) . ?
P3A F16A 1.582(14) . ?
P3A F17A 1.592(15) . ?
P3A F18A 1.601(15) . ?
P3A F15A 1.603(15) . ?
P3A F13A 1.605(11) . ?
P3A F14A 1.612(12) . ?
P3B F16B 1.582(15) . ?
P3B F17B 1.590(15) . ?
P3B F18B 1.602(15) . ?
P3B F13B 1.604(11) . ?
P3B F15B 1.604(15) . ?
P3B F14B 1.614(12) . ?
N13 C37 1.15(2) . ?
C37 C38 1.45(2) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N14 C39 1.122(19) . ?
C39 C40 1.46(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N15 C41 1.16(3) . ?
C41 C42 1.42(3) . ?
N16 C43 1.12(2) . ?
C43 C44 1.45(2) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ag1 C19 177.6(5) . . ?
C1 Ag1 Ag3 69.1(4) . . ?
C19 Ag1 Ag3 108.9(4) . . ?
C10 Ag2 C28 175.5(5) . . ?
C10 Ag2 Ag3 115.0(4) . . ?
C28 Ag2 Ag3 69.3(4) . . ?
N3 Ag3 N12 137.7(3) . . ?
N3 Ag3 N14 84.2(4) . . ?
N12 Ag3 N14 92.2(4) . . ?
N3 Ag3 N13 87.7(4) . . ?
N12 Ag3 N13 80.4(4) . . ?
N14 Ag3 N13 158.5(4) . . ?
N3 Ag3 Ag2 144.0(3) . . ?
N12 Ag3 Ag2 75.2(3) . . ?
N14 Ag3 Ag2 113.5(3) . . ?
N13 Ag3 Ag2 84.4(3) . . ?
N3 Ag3 Ag1 76.6(3) . . ?
N12 Ag3 Ag1 145.2(3) . . ?
N14 Ag3 Ag1 85.0(3) . . ?
N13 Ag3 Ag1 112.5(3) . . ?
Ag2 Ag3 Ag1 74.26(3) . . ?
C18 O1 H1 105(6) . . ?
C36 O2 H4 109(9) . . ?
C1 N1 C2 112.0(11) . . ?
C1 N1 C9 122.1(11) . . ?
C2 N1 C9 125.8(11) . . ?
C1 N2 C3 112.9(11) . . ?
C1 N2 C4 123.8(11) . . ?
C3 N2 C4 123.4(10) . . ?
C4 N3 C8 115.9(11) . . ?
C4 N3 Ag3 121.5(8) . . ?
C8 N3 Ag3 122.3(9) . . ?
C10 N4 C11 110.9(12) . . ?
C10 N4 C9 121.6(11) . . ?
C11 N4 C9 127.4(12) . . ?
C10 N5 C12 111.8(12) . . ?
C10 N5 C13 122.6(12) . . ?
C12 N5 C13 125.5(12) . . ?
C13 N6 C17 116.2(13) . . ?
C19 N7 C20 109.6(11) . . ?
C19 N7 C27 121.6(11) . . ?
C20 N7 C27 128.8(11) . . ?
C19 N8 C21 111.2(11) . . ?
C19 N8 C22 123.4(11) . . ?
C21 N8 C22 125.4(12) . . ?
C26 N9 C22 116.7(12) . . ?
C28 N10 C29 111.0(11) . . ?
C28 N10 C27 123.5(11) . . ?
C29 N10 C27 125.4(11) . . ?
C28 N11 C30 111.1(11) . . ?
C28 N11 C31 124.2(11) . . ?
C30 N11 C31 124.7(11) . . ?
C31 N12 C35 116.4(12) . . ?
C31 N12 Ag3 120.8(8) . . ?
C35 N12 Ag3 122.6(9) . . ?
N2 C1 N1 103.2(11) . . ?
N2 C1 Ag1 130.2(10) . . ?
N1 C1 Ag1 125.3(9) . . ?
C3 C2 N1 105.9(12) . . ?
C3 C2 H2 127.0 . . ?
N1 C2 H2 127.0 . . ?
C2 C3 N2 105.8(11) . . ?
C2 C3 H3 127.1 . . ?
N2 C3 H3 127.1 . . ?
C5 C4 N3 124.3(13) . . ?
C5 C4 N2 121.4(12) . . ?
N3 C4 N2 114.3(11) . . ?
C4 C5 C6 119.4(13) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C7 118.8(12) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C8 C7 C6 118.7(13) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N3 C8 C7 123.1(13) . . ?
N3 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N1 C9 N4 109.0(10) . . ?
N1 C9 C18 112.7(11) . . ?
N4 C9 C18 114.5(12) . . ?
N1 C9 H9 106.7 . . ?
N4 C9 H9 106.7 . . ?
C18 C9 H9 106.7 . . ?
N4 C10 N5 104.0(12) . . ?
N4 C10 Ag2 132.7(10) . . ?
N5 C10 Ag2 123.2(10) . . ?
C12 C11 N4 107.4(13) . . ?
C12 C11 H11 126.3 . . ?
N4 C11 H11 126.3 . . ?
C11 C12 N5 106.0(12) . . ?
C11 C12 H12 127.0 . . ?
N5 C12 H12 127.0 . . ?
N6 C13 C14 123.5(14) . . ?
N6 C13 N5 114.9(12) . . ?
C14 C13 N5 121.5(13) . . ?
C15 C14 C13 117.1(15) . . ?
C15 C14 H14 121.5 . . ?
C13 C14 H14 121.5 . . ?
C14 C15 C16 121.5(16) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 117.1(16) . . ?
C17 C16 H16 121.4 . . ?
C15 C16 H16 121.4 . . ?
N6 C17 C16 124.6(16) . . ?
N6 C17 H17 117.7 . . ?
C16 C17 H17 117.7 . . ?
O1 C18 C9 113.9(12) . . ?
O1 C18 H18A 108.8 . . ?
C9 C18 H18A 108.8 . . ?
O1 C18 H18B 108.8 . . ?
C9 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
N8 C19 N7 104.1(11) . . ?
N8 C19 Ag1 121.8(9) . . ?
N7 C19 Ag1 133.8(10) . . ?
C21 C20 N7 108.7(12) . . ?
C21 C20 H20 125.7 . . ?
N7 C20 H20 125.7 . . ?
C20 C21 N8 106.4(13) . . ?
C20 C21 H21 126.8 . . ?
N8 C21 H21 126.8 . . ?
N9 C22 C23 124.2(13) . . ?
N9 C22 N8 113.8(12) . . ?
C23 C22 N8 121.7(13) . . ?
C24 C23 C22 117.3(14) . . ?
C24 C23 H23 121.3 . . ?
C22 C23 H23 121.3 . . ?
C23 C24 C25 120.4(15) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 117.1(14) . . ?
C26 C25 H25 121.5 . . ?
C24 C25 H25 121.5 . . ?
N9 C26 C25 124.2(14) . . ?
N9 C26 H26 117.9 . . ?
C25 C26 H26 117.9 . . ?
N7 C27 N10 110.4(10) . . ?
N7 C27 C36 111.2(11) . . ?
N10 C27 C36 112.6(11) . . ?
N7 C27 H27 107.5 . . ?
N10 C27 H27 107.5 . . ?
C36 C27 H27 107.5 . . ?
N10 C28 N11 104.1(11) . . ?
N10 C28 Ag2 126.8(10) . . ?
N11 C28 Ag2 128.2(10) . . ?
C30 C29 N10 106.4(12) . . ?
C30 C29 H29 126.8 . . ?
N10 C29 H29 126.8 . . ?
C29 C30 N11 107.3(12) . . ?
C29 C30 H30 126.4 . . ?
N11 C30 H30 126.4 . . ?
N12 C31 C32 124.6(12) . . ?
N12 C31 N11 115.0(11) . . ?
C32 C31 N11 120.4(12) . . ?
C31 C32 C33 118.0(13) . . ?
C31 C32 H32 121.0 . . ?
C33 C32 H32 121.0 . . ?
C34 C33 C32 118.6(13) . . ?
C34 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C33 C34 C35 119.7(13) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
N12 C35 C34 122.8(13) . . ?
N12 C35 H35 118.6 . . ?
C34 C35 H35 118.6 . . ?
O2 C36 C27 109.3(11) . . ?
O2 C36 H36A 109.8 . . ?
C27 C36 H36A 109.8 . . ?
O2 C36 H36B 109.8 . . ?
C27 C36 H36B 109.8 . . ?
H36A C36 H36B 108.3 . . ?
F1 P1 F4 89.8(6) . . ?
F1 P1 F6 90.4(6) . . ?
F4 P1 F6 179.8(7) . . ?
F1 P1 F5 93.1(8) . . ?
F4 P1 F5 90.8(6) . . ?
F6 P1 F5 89.1(5) . . ?
F1 P1 F2 177.9(8) . . ?
F4 P1 F2 90.7(5) . . ?
F6 P1 F2 89.1(6) . . ?
F5 P1 F2 88.9(7) . . ?
F1 P1 F3 90.8(8) . . ?
F4 P1 F3 90.9(6) . . ?
F6 P1 F3 89.1(6) . . ?
F5 P1 F3 175.8(7) . . ?
F2 P1 F3 87.3(7) . . ?
F1A P1A F4A 89.8(6) . . ?
F1A P1A F5A 93.2(8) . . ?
F4A P1A F5A 90.8(6) . . ?
F1A P1A F6A 90.3(6) . . ?
F4A P1A F6A 179.9(7) . . ?
F5A P1A F6A 89.1(5) . . ?
F1A P1A F2A 177.8(8) . . ?
F4A P1A F2A 90.8(6) . . ?
F5A P1A F2A 88.9(7) . . ?
F6A P1A F2A 89.0(6) . . ?
F1A P1A F3A 90.7(8) . . ?
F4A P1A F3A 90.9(6) . . ?
F5A P1A F3A 175.8(8) . . ?
F6A P1A F3A 89.2(6) . . ?
F2A P1A F3A 87.2(7) . . ?
F8 P2 F9 90.6(7) . . ?
F8 P2 F12 89.3(7) . . ?
F9 P2 F12 89.5(6) . . ?
F8 P2 F11 90.6(8) . . ?
F9 P2 F11 178.6(8) . . ?
F12 P2 F11 89.8(6) . . ?
F8 P2 F7 179.1(7) . . ?
F9 P2 F7 88.8(6) . . ?
F12 P2 F7 91.4(6) . . ?
F11 P2 F7 90.0(7) . . ?
F8 P2 F10 90.3(6) . . ?
F9 P2 F10 88.4(6) . . ?
F12 P2 F10 177.8(7) . . ?
F11 P2 F10 92.3(7) . . ?
F7 P2 F10 89.0(6) . . ?
F16 P3 F17 88.3(10) . . ?
F16 P3 F18 175.7(13) . . ?
F17 P3 F18 87.4(10) . . ?
F16 P3 F13 89.7(8) . . ?
F17 P3 F13 91.2(8) . . ?
F18 P3 F13 90.2(8) . . ?
F16 P3 F15 90.6(9) . . ?
F17 P3 F15 178.8(11) . . ?
F18 P3 F15 93.7(11) . . ?
F13 P3 F15 89.2(7) . . ?
F16 P3 F14 91.2(8) . . ?
F17 P3 F14 91.9(8) . . ?
F18 P3 F14 89.3(8) . . ?
F13 P3 F14 176.9(8) . . ?
F15 P3 F14 87.8(8) . . ?
F16A P3A F17A 88.3(11) . . ?
F16A P3A F18A 175.5(14) . . ?
F17A P3A F18A 87.2(11) . . ?
F16A P3A F15A 90.6(11) . . ?
F17A P3A F15A 178.9(13) . . ?
F18A P3A F15A 93.9(13) . . ?
F16A P3A F13A 89.6(9) . . ?
F17A P3A F13A 90.9(9) . . ?
F18A P3A F13A 89.7(8) . . ?
F15A P3A F13A 89.2(8) . . ?
F16A P3A F14A 91.2(9) . . ?
F17A P3A F14A 91.7(9) . . ?
F18A P3A F14A 89.7(9) . . ?
F15A P3A F14A 88.2(9) . . ?
F13A P3A F14A 177.3(10) . . ?
F16B P3B F17B 88.4(11) . . ?
F16B P3B F18B 175.7(14) . . ?
F17B P3B F18B 87.4(11) . . ?
F16B P3B F13B 90.1(9) . . ?
F17B P3B F13B 91.2(9) . . ?
F18B P3B F13B 89.8(9) . . ?
F16B P3B F15B 90.5(10) . . ?
F17B P3B F15B 178.7(13) . . ?
F18B P3B F15B 93.8(12) . . ?
F13B P3B F15B 89.4(9) . . ?
F16B P3B F14B 91.2(9) . . ?
F17B P3B F14B 91.9(9) . . ?
F18B P3B F14B 89.2(9) . . ?
F13B P3B F14B 176.8(10) . . ?
F15B P3B F14B 87.6(9) . . ?
C37 N13 Ag3 159.5(14) . . ?
N13 C37 C38 179(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 N14 Ag3 168.2(13) . . ?
N14 C39 C40 178.0(19) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N15 C41 C42 175(3) . . ?
N16 C43 C44 179(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 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
C3 N2 C1 N1 -0.9(14) . . . . ?
C4 N2 C1 N1 178.0(11) . . . . ?
C3 N2 C1 Ag1 -168.1(10) . . . . ?
C4 N2 C1 Ag1 10.8(19) . . . . ?
C2 N1 C1 N2 3.9(14) . . . . ?
C9 N1 C1 N2 -179.3(11) . . . . ?
C2 N1 C1 Ag1 171.9(9) . . . . ?
C9 N1 C1 Ag1 -11.3(17) . . . . ?
C1 N1 C2 C3 -5.5(15) . . . . ?
C9 N1 C2 C3 177.9(11) . . . . ?
N1 C2 C3 N2 4.5(14) . . . . ?
C1 N2 C3 C2 -2.4(15) . . . . ?
C4 N2 C3 C2 178.7(11) . . . . ?
C8 N3 C4 C5 1.6(19) . . . . ?
Ag3 N3 C4 C5 -171.6(10) . . . . ?
C8 N3 C4 N2 -179.4(10) . . . . ?
Ag3 N3 C4 N2 7.4(15) . . . . ?
C1 N2 C4 C5 -138.7(14) . . . . ?
C3 N2 C4 C5 40.1(18) . . . . ?
C1 N2 C4 N3 42.2(17) . . . . ?
C3 N2 C4 N3 -138.9(12) . . . . ?
N3 C4 C5 C6 0(2) . . . . ?
N2 C4 C5 C6 -179.1(12) . . . . ?
C4 C5 C6 C7 -1.6(19) . . . . ?
C5 C6 C7 C8 1.9(19) . . . . ?
C4 N3 C8 C7 -1.3(18) . . . . ?
Ag3 N3 C8 C7 171.8(10) . . . . ?
C6 C7 C8 N3 0(2) . . . . ?
C1 N1 C9 N4 -112.0(13) . . . . ?
C2 N1 C9 N4 64.3(15) . . . . ?
C1 N1 C9 C18 119.8(14) . . . . ?
C2 N1 C9 C18 -64.0(17) . . . . ?
C10 N4 C9 N1 82.4(15) . . . . ?
C11 N4 C9 N1 -95.6(15) . . . . ?
C10 N4 C9 C18 -150.4(13) . . . . ?
C11 N4 C9 C18 31.6(19) . . . . ?
C11 N4 C10 N5 -0.2(15) . . . . ?
C9 N4 C10 N5 -178.5(11) . . . . ?
C11 N4 C10 Ag2 175.0(11) . . . . ?
C9 N4 C10 Ag2 -3(2) . . . . ?
C12 N5 C10 N4 -0.1(15) . . . . ?
C13 N5 C10 N4 -175.5(12) . . . . ?
C12 N5 C10 Ag2 -175.9(9) . . . . ?
C13 N5 C10 Ag2 8.7(18) . . . . ?
C10 N4 C11 C12 0.5(16) . . . . ?
C9 N4 C11 C12 178.6(12) . . . . ?
N4 C11 C12 N5 -0.5(15) . . . . ?
C10 N5 C12 C11 0.4(16) . . . . ?
C13 N5 C12 C11 175.6(13) . . . . ?
C17 N6 C13 C14 0(2) . . . . ?
C17 N6 C13 N5 179.0(12) . . . . ?
C10 N5 C13 N6 -28.1(19) . . . . ?
C12 N5 C13 N6 157.2(13) . . . . ?
C10 N5 C13 C14 150.5(14) . . . . ?
C12 N5 C13 C14 -24(2) . . . . ?
N6 C13 C14 C15 -1(2) . . . . ?
N5 C13 C14 C15 -179.2(13) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C14 C15 C16 C17 1(2) . . . . ?
C13 N6 C17 C16 1(2) . . . . ?
C15 C16 C17 N6 -2(2) . . . . ?
N1 C9 C18 O1 52.8(16) . . . . ?
N4 C9 C18 O1 -72.5(15) . . . . ?
C21 N8 C19 N7 2.6(15) . . . . ?
C22 N8 C19 N7 -176.0(11) . . . . ?
C21 N8 C19 Ag1 -172.0(9) . . . . ?
C22 N8 C19 Ag1 9.3(17) . . . . ?
C20 N7 C19 N8 -2.4(14) . . . . ?
C27 N7 C19 N8 179.8(11) . . . . ?
C20 N7 C19 Ag1 171.3(11) . . . . ?
C27 N7 C19 Ag1 -7(2) . . . . ?
C19 N7 C20 C21 1.4(15) . . . . ?
C27 N7 C20 C21 179.0(12) . . . . ?
N7 C20 C21 N8 0.3(15) . . . . ?
C19 N8 C21 C20 -1.9(16) . . . . ?
C22 N8 C21 C20 176.7(12) . . . . ?
C26 N9 C22 C23 0(2) . . . . ?
C26 N9 C22 N8 175.2(12) . . . . ?
C19 N8 C22 N9 -23.1(18) . . . . ?
C21 N8 C22 N9 158.4(13) . . . . ?
C19 N8 C22 C23 151.9(13) . . . . ?
C21 N8 C22 C23 -27(2) . . . . ?
N9 C22 C23 C24 -1(2) . . . . ?
N8 C22 C23 C24 -175.5(13) . . . . ?
C22 C23 C24 C25 1(2) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
C22 N9 C26 C25 0(2) . . . . ?
C24 C25 C26 N9 0(2) . . . . ?
C19 N7 C27 N10 86.9(15) . . . . ?
C20 N7 C27 N10 -90.5(15) . . . . ?
C19 N7 C27 C36 -147.5(12) . . . . ?
C20 N7 C27 C36 35.2(18) . . . . ?
C28 N10 C27 N7 -109.7(14) . . . . ?
C29 N10 C27 N7 71.4(16) . . . . ?
C28 N10 C27 C36 125.4(13) . . . . ?
C29 N10 C27 C36 -53.6(17) . . . . ?
C29 N10 C28 N11 -2.6(14) . . . . ?
C27 N10 C28 N11 178.3(11) . . . . ?
C29 N10 C28 Ag2 167.4(9) . . . . ?
C27 N10 C28 Ag2 -11.7(18) . . . . ?
C30 N11 C28 N10 2.2(14) . . . . ?
C31 N11 C28 N10 -178.9(11) . . . . ?
C30 N11 C28 Ag2 -167.6(10) . . . . ?
C31 N11 C28 Ag2 11.4(18) . . . . ?
C28 N10 C29 C30 2.1(15) . . . . ?
C27 N10 C29 C30 -178.8(12) . . . . ?
N10 C29 C30 N11 -0.7(14) . . . . ?
C28 N11 C30 C29 -0.9(15) . . . . ?
C31 N11 C30 C29 -179.9(12) . . . . ?
C35 N12 C31 C32 1(2) . . . . ?
Ag3 N12 C31 C32 -173.8(11) . . . . ?
C35 N12 C31 N11 -175.9(11) . . . . ?
Ag3 N12 C31 N11 9.0(15) . . . . ?
C28 N11 C31 N12 40.6(18) . . . . ?
C30 N11 C31 N12 -140.6(12) . . . . ?
C28 N11 C31 C32 -136.7(14) . . . . ?
C30 N11 C31 C32 42.1(19) . . . . ?
N12 C31 C32 C33 0(2) . . . . ?
N11 C31 C32 C33 177.4(12) . . . . ?
C31 C32 C33 C34 -2(2) . . . . ?
C32 C33 C34 C35 1(2) . . . . ?
C31 N12 C35 C34 -1.7(19) . . . . ?
Ag3 N12 C35 C34 173.3(10) . . . . ?
C33 C34 C35 N12 0(2) . . . . ?
N7 C27 C36 O2 172.7(10) . . . . ?
N10 C27 C36 O2 -62.9(14) . . . . ?


####################################################################### 
# 
# 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_C2
_database_code_depnum_ccdc_archive 'CCDC 1811953'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C22 H22 Fe N8 O, 2(F6 P)'
_chemical_formula_sum            'C22 H22 F12 Fe N8 O P2'
_chemical_formula_weight         760.27

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'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   8.7083(5)
_cell_length_b                   13.7335(7)
_cell_length_c                   23.8833(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.431(3)
_cell_angle_gamma                90
_cell_volume                     2855.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    6291
_cell_measurement_theta_min      2.2605
_cell_measurement_theta_max      24.0139

_exptl_crystal_description       fragment
_exptl_crystal_colour            red

_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.429
_exptl_crystal_size_min          0.136
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.5717
_exptl_absorpt_correction_T_max  0.7452

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           10 s per frame
dx                                  35 mm
2458 frames measured in 9 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            75517
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             5278
# number of observed reflections (> n sig(I))
_reflns_number_gt                3777
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2013 (Sheldrick, 2013), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0564P)²+8.2080P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom

_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         5278
_refine_ls_number_parameters     456
_refine_ls_number_restraints     66
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1483
_refine_ls_wR_factor_gt          0.1294
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.097

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.48691(7) 0.24330(4) 0.39689(2) 0.01566(18) Uani 1 1 d . . . . .
O1 O 0.6733(4) 0.4047(3) 0.27336(16) 0.0411(9) Uani 1 1 d . . . . .
H1 H 0.7234 0.3526 0.2715 0.049 Uiso 1 1 calc R U . . .
N1 N 0.3672(4) 0.3885(3) 0.31707(15) 0.0228(8) Uani 1 1 d . . . . .
N2 N 0.3432(4) 0.4216(2) 0.40443(15) 0.0190(8) Uani 1 1 d . . . . .
N3 N 0.4411(4) 0.3166(3) 0.47094(14) 0.0181(8) Uani 1 1 d . . . . .
N4 N 0.4614(4) 0.2422(3) 0.27404(14) 0.0223(8) Uani 1 1 d . . . . .
N5 N 0.5488(4) 0.1121(3) 0.31288(14) 0.0219(8) Uani 1 1 d . . . . .
N6 N 0.5860(4) 0.1047(3) 0.40802(14) 0.0191(8) Uani 1 1 d . . . . .
N7 N 0.6878(4) 0.2996(3) 0.39795(14) 0.0203(8) Uani 1 1 d . . . . .
N8 N 0.2910(4) 0.1801(3) 0.40306(14) 0.0178(8) Uani 1 1 d . . . . .
C1 C 0.3982(5) 0.3539(3) 0.36872(17) 0.0188(9) Uani 1 1 d . . . . .
C2 C 0.2971(5) 0.4792(3) 0.3204(2) 0.0280(11) Uani 1 1 d . . . . .
H2 H 0.2660 0.5190 0.2896 0.034 Uiso 1 1 calc R U . . .
C3 C 0.2812(5) 0.5003(3) 0.3747(2) 0.0268(11) Uani 1 1 d . . . . .
H3 H 0.2368 0.5574 0.3899 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3645(5) 0.4011(3) 0.46190(18) 0.0187(9) Uani 1 1 d . . . . .
C5 C 0.3152(5) 0.4610(3) 0.5040(2) 0.0258(11) Uani 1 1 d . . . . .
H5 H 0.2602 0.5192 0.4959 0.031 Uiso 1 1 calc R U . . .
C6 C 0.3488(5) 0.4332(3) 0.55841(19) 0.0262(11) Uani 1 1 d . . . . .
H6 H 0.3154 0.4723 0.5886 0.031 Uiso 1 1 calc R U . . .
C7 C 0.4306(5) 0.3492(3) 0.56925(19) 0.0252(10) Uani 1 1 d . . . . .
H7 H 0.4560 0.3301 0.6066 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4744(5) 0.2934(3) 0.52424(18) 0.0227(10) Uani 1 1 d . . . . .
H8 H 0.5312 0.2356 0.5315 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4142(6) 0.3433(3) 0.26394(19) 0.0277(11) Uani 1 1 d . . . . .
H9 H 0.3234 0.3429 0.2375 0.033 Uiso 1 1 calc R U . . .
C10 C 0.4999(5) 0.2036(3) 0.32388(18) 0.0189(9) Uani 1 1 d . . . . .
C11 C 0.4882(6) 0.1751(4) 0.23125(19) 0.0290(11) Uani 1 1 d . . . . .
H11 H 0.4707 0.1857 0.1923 0.035 Uiso 1 1 calc R U . . .
C12 C 0.5426(6) 0.0940(4) 0.25476(19) 0.0306(12) Uani 1 1 d . . . . .
H12 H 0.5713 0.0358 0.2362 0.037 Uiso 1 1 calc R U . . .
C13 C 0.5963(5) 0.0562(3) 0.35899(18) 0.0203(10) Uani 1 1 d . . . . .
C14 C 0.6458(5) -0.0386(3) 0.3545(2) 0.0271(11) Uani 1 1 d . . . . .
H14 H 0.6495 -0.0700 0.3191 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6896(6) -0.0863(3) 0.4029(2) 0.0313(12) Uani 1 1 d . . . . .
H15 H 0.7249 -0.1517 0.4016 0.038 Uiso 1 1 calc R U . . .
C16 C 0.6819(5) -0.0384(3) 0.4531(2) 0.0286(11) Uani 1 1 d . . . . .
H16 H 0.7111 -0.0704 0.4870 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6313(5) 0.0566(3) 0.45399(18) 0.0213(10) Uani 1 1 d . . . . .
H17 H 0.6286 0.0894 0.4890 0.026 Uiso 1 1 calc R U . . .
C18 C 0.5411(6) 0.3990(4) 0.2371(2) 0.0352(12) Uani 1 1 d . . . . .
H18A H 0.5688 0.3666 0.2018 0.042 Uiso 1 1 calc R U . . .
H18B H 0.5049 0.4656 0.2280 0.042 Uiso 1 1 calc R U . . .
C19 C 0.8070(5) 0.3343(3) 0.39903(18) 0.0229(10) Uani 1 1 d . . . . .
C20 C 0.9588(5) 0.3777(4) 0.3997(2) 0.0322(12) Uani 1 1 d . . . . .
H20A H 0.9503 0.4479 0.4064 0.048 Uiso 1 1 calc R U . . .
H20B H 1.0065 0.3666 0.3635 0.048 Uiso 1 1 calc R U . . .
H20C H 1.0222 0.3480 0.4295 0.048 Uiso 1 1 calc R U . . .
C21 C 0.1743(5) 0.1416(3) 0.40517(17) 0.0194(9) Uani 1 1 d . . . . .
C22 C 0.0274(5) 0.0929(4) 0.4086(2) 0.0287(11) Uani 1 1 d . . . . .
H22A H -0.0352 0.1076 0.3750 0.043 Uiso 1 1 calc R U . . .
H22B H -0.0257 0.1157 0.4418 0.043 Uiso 1 1 calc R U . . .
H22C H 0.0437 0.0225 0.4112 0.043 Uiso 1 1 calc R U . . .
P1 P 0.51708(16) 0.72071(11) 0.25581(6) 0.0358(4) Uani 1 1 d . . . . .
F1 F 0.4713(5) 0.8278(3) 0.23769(18) 0.0824(14) Uani 1 1 d . . . . .
F2 F 0.3969(4) 0.7265(3) 0.30440(14) 0.0586(10) Uani 1 1 d . . . . .
F3 F 0.3862(4) 0.6763(4) 0.21656(16) 0.0945(17) Uani 1 1 d . . . . .
F4 F 0.5657(4) 0.6143(2) 0.27629(16) 0.0617(10) Uani 1 1 d . . . . .
F5 F 0.6365(4) 0.7117(3) 0.20681(13) 0.0654(11) Uani 1 1 d . . . . .
F6 F 0.6484(4) 0.7611(2) 0.29650(14) 0.0513(9) Uani 1 1 d . . . . .
P2 P 0.04912(15) 0.74531(9) 0.44190(5) 0.0277(3) Uani 1 1 d . U . . .
F7 F 0.1874(3) 0.7283(2) 0.40029(12) 0.0429(8) Uani 1 1 d . . . . .
F8 F -0.0889(3) 0.7602(2) 0.48352(12) 0.0379(7) Uani 1 1 d . . . . .
F9_c F 0.1664(4) 0.7704(4) 0.49119(17) 0.0576(15) Uani 0.847(7) 1 d D U P A 3
F10_c F 0.0575(6) 0.6331(3) 0.4607(2) 0.0552(14) Uani 0.847(7) 1 d D U P A 3
F11_c F -0.0742(5) 0.7167(4) 0.39512(15) 0.0483(13) Uani 0.847(7) 1 d D U P A 3
F12_c F 0.0363(5) 0.8551(3) 0.4253(2) 0.0603(15) Uani 0.847(7) 1 d D U P A 3
F9A_d F 0.139(3) 0.6769(18) 0.4803(8) 0.048(6) Uani 0.153(7) 1 d D U P A 4
F10A_d F -0.023(2) 0.6631(15) 0.4056(8) 0.036(5) Uani 0.153(7) 1 d D U P A 4
F11A_d F -0.006(3) 0.8237(17) 0.3920(9) 0.052(6) Uani 0.153(7) 1 d D U P A 4
F12A_d F 0.149(3) 0.8372(17) 0.4687(9) 0.050(6) Uani 0.153(7) 1 d D U P A 4


_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 1.826(4) . ?
Fe1 C10 1.833(4) . ?
Fe1 N7 1.913(4) . ?
Fe1 N8 1.923(4) . ?
Fe1 N3 2.082(3) . ?
Fe1 N6 2.104(4) . ?
O1 C18 1.425(6) . ?
N1 C1 1.342(5) . ?
N1 C2 1.390(6) . ?
N1 C9 1.480(6) . ?
N2 C1 1.357(5) . ?
N2 C3 1.395(6) . ?
N2 C4 1.409(5) . ?
N3 C8 1.337(5) . ?
N3 C4 1.353(5) . ?
N4 C10 1.338(5) . ?
N4 C11 1.400(6) . ?
N4 C9 1.465(6) . ?
N5 C10 1.354(6) . ?
N5 C13 1.397(6) . ?
N5 C12 1.410(6) . ?
N6 C17 1.333(5) . ?
N6 C13 1.353(5) . ?
N7 C19 1.142(6) . ?
N8 C21 1.147(5) . ?
C2 C3 1.341(7) . ?
C4 C5 1.376(6) . ?
C5 C6 1.379(7) . ?
C6 C7 1.377(7) . ?
C7 C8 1.381(6) . ?
C9 C18 1.501(7) . ?
C11 C12 1.330(7) . ?
C13 C14 1.375(6) . ?
C14 C15 1.375(7) . ?
C15 C16 1.372(7) . ?
C16 C17 1.377(6) . ?
C19 C20 1.450(6) . ?
C21 C22 1.448(6) . ?
P1 F3 1.580(4) . ?
P1 F1 1.582(4) . ?
P1 F6 1.582(3) . ?
P1 F2 1.584(3) . ?
P1 F5 1.590(3) . ?
P1 F4 1.595(4) . ?
P2 F9A_d 1.516(18) . ?
P2 F10A_d 1.545(17) . ?
P2 F12_c 1.563(4) . ?
P2 F9_c 1.577(4) . ?
P2 F11_c 1.580(4) . ?
P2 F8 1.592(3) . ?
P2 F7 1.597(3) . ?
P2 F10_c 1.606(4) . ?
P2 F12A_d 1.654(19) . ?
P2 F11A_d 1.667(18) . ?

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 C10 86.13(19) . . ?
C1 Fe1 N7 92.71(17) . . ?
C10 Fe1 N7 93.12(17) . . ?
C1 Fe1 N8 92.06(17) . . ?
C10 Fe1 N8 90.85(17) . . ?
N7 Fe1 N8 173.99(15) . . ?
C1 Fe1 N3 79.77(16) . . ?
C10 Fe1 N3 165.80(17) . . ?
N7 Fe1 N3 89.31(14) . . ?
N8 Fe1 N3 87.94(14) . . ?
C1 Fe1 N6 165.47(16) . . ?
C10 Fe1 N6 79.41(16) . . ?
N7 Fe1 N6 89.54(14) . . ?
N8 Fe1 N6 86.76(14) . . ?
N3 Fe1 N6 114.62(14) . . ?
C1 N1 C2 110.0(4) . . ?
C1 N1 C9 125.9(4) . . ?
C2 N1 C9 123.8(4) . . ?
C1 N2 C3 110.4(4) . . ?
C1 N2 C4 115.8(4) . . ?
C3 N2 C4 133.7(4) . . ?
C8 N3 C4 116.8(4) . . ?
C8 N3 Fe1 130.7(3) . . ?
C4 N3 Fe1 112.5(3) . . ?
C10 N4 C11 110.2(4) . . ?
C10 N4 C9 125.8(4) . . ?
C11 N4 C9 123.7(4) . . ?
C10 N5 C13 116.5(4) . . ?
C10 N5 C12 110.5(4) . . ?
C13 N5 C12 133.0(4) . . ?
C17 N6 C13 116.4(4) . . ?
C17 N6 Fe1 131.7(3) . . ?
C13 N6 Fe1 111.9(3) . . ?
C19 N7 Fe1 179.0(4) . . ?
C21 N8 Fe1 178.0(3) . . ?
N1 C1 N2 105.7(4) . . ?
N1 C1 Fe1 134.9(3) . . ?
N2 C1 Fe1 119.4(3) . . ?
C3 C2 N1 107.8(4) . . ?
C2 C3 N2 106.0(4) . . ?
N3 C4 C5 123.9(4) . . ?
N3 C4 N2 112.3(4) . . ?
C5 C4 N2 123.8(4) . . ?
C4 C5 C6 117.4(4) . . ?
C7 C6 C5 120.4(4) . . ?
C6 C7 C8 118.0(4) . . ?
N3 C8 C7 123.5(4) . . ?
N4 C9 N1 109.8(3) . . ?
N4 C9 C18 110.3(4) . . ?
N1 C9 C18 112.0(4) . . ?
N4 C10 N5 105.6(4) . . ?
N4 C10 Fe1 135.1(3) . . ?
N5 C10 Fe1 119.2(3) . . ?
C12 C11 N4 107.9(4) . . ?
C11 C12 N5 105.8(4) . . ?
N6 C13 C14 124.2(4) . . ?
N6 C13 N5 112.7(4) . . ?
C14 C13 N5 123.1(4) . . ?
C15 C14 C13 117.8(4) . . ?
C16 C15 C14 119.2(4) . . ?
C15 C16 C17 119.4(4) . . ?
N6 C17 C16 123.1(4) . . ?
O1 C18 C9 111.2(4) . . ?
N7 C19 C20 179.2(5) . . ?
N8 C21 C22 179.3(5) . . ?
F3 P1 F1 91.3(3) . . ?
F3 P1 F6 177.7(3) . . ?
F1 P1 F6 90.9(2) . . ?
F3 P1 F2 88.5(2) . . ?
F1 P1 F2 89.2(2) . . ?
F6 P1 F2 90.7(2) . . ?
F3 P1 F5 90.5(2) . . ?
F1 P1 F5 92.1(2) . . ?
F6 P1 F5 90.2(2) . . ?
F2 P1 F5 178.4(2) . . ?
F3 P1 F4 90.6(3) . . ?
F1 P1 F4 177.8(2) . . ?
F6 P1 F4 87.15(19) . . ?
F2 P1 F4 89.8(2) . . ?
F5 P1 F4 88.9(2) . . ?
F9A_d P2 F10A_d 94.6(12) . . ?
F12_c P2 F9_c 91.1(3) . . ?
F12_c P2 F11_c 91.0(3) . . ?
F9_c P2 F11_c 176.5(3) . . ?
F9A_d P2 F8 95.1(9) . . ?
F10A_d P2 F8 98.2(7) . . ?
F12_c P2 F8 89.1(2) . . ?
F9_c P2 F8 89.47(19) . . ?
F11_c P2 F8 87.87(19) . . ?
F9A_d P2 F7 84.3(9) . . ?
F10A_d P2 F7 81.1(7) . . ?
F12_c P2 F7 91.9(2) . . ?
F9_c P2 F7 90.7(2) . . ?
F11_c P2 F7 91.92(19) . . ?
F8 P2 F7 178.98(19) . . ?
F12_c P2 F10_c 177.9(2) . . ?
F9_c P2 F10_c 88.7(3) . . ?
F11_c P2 F10_c 89.1(3) . . ?
F8 P2 F10_c 88.82(19) . . ?
F7 P2 F10_c 90.18(19) . . ?
F9A_d P2 F12A_d 88.8(11) . . ?
F10A_d P2 F12A_d 167.4(11) . . ?
F8 P2 F12A_d 93.5(8) . . ?
F7 P2 F12A_d 87.3(8) . . ?
F9A_d P2 F11A_d 165.3(13) . . ?
F10A_d P2 F11A_d 88.1(10) . . ?
F8 P2 F11A_d 98.9(9) . . ?
F7 P2 F11A_d 81.8(9) . . ?
F12A_d P2 F11A_d 85.6(11) . . ?

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 N1 C1 N2 1.8(5) . . . . ?
C9 N1 C1 N2 175.8(4) . . . . ?
C2 N1 C1 Fe1 -179.8(4) . . . . ?
C9 N1 C1 Fe1 -5.8(7) . . . . ?
C3 N2 C1 N1 -1.7(5) . . . . ?
C4 N2 C1 N1 -179.4(3) . . . . ?
C3 N2 C1 Fe1 179.6(3) . . . . ?
C4 N2 C1 Fe1 2.0(5) . . . . ?
C10 Fe1 C1 N1 -3.1(5) . . . . ?
N7 Fe1 C1 N1 89.9(5) . . . . ?
N8 Fe1 C1 N1 -93.8(5) . . . . ?
N3 Fe1 C1 N1 178.7(5) . . . . ?
N6 Fe1 C1 N1 -8.7(10) . . . . ?
C10 Fe1 C1 N2 175.1(4) . . . . ?
N7 Fe1 C1 N2 -91.9(3) . . . . ?
N8 Fe1 C1 N2 84.4(3) . . . . ?
N3 Fe1 C1 N2 -3.1(3) . . . . ?
N6 Fe1 C1 N2 169.5(5) . . . . ?
C1 N1 C2 C3 -1.3(5) . . . . ?
C9 N1 C2 C3 -175.4(4) . . . . ?
N1 C2 C3 N2 0.3(5) . . . . ?
C1 N2 C3 C2 0.9(5) . . . . ?
C4 N2 C3 C2 178.0(4) . . . . ?
C8 N3 C4 C5 -2.5(6) . . . . ?
Fe1 N3 C4 C5 177.3(3) . . . . ?
C8 N3 C4 N2 176.4(4) . . . . ?
Fe1 N3 C4 N2 -3.8(4) . . . . ?
C1 N2 C4 N3 1.5(5) . . . . ?
C3 N2 C4 N3 -175.5(4) . . . . ?
C1 N2 C4 C5 -179.5(4) . . . . ?
C3 N2 C4 C5 3.5(7) . . . . ?
N3 C4 C5 C6 1.1(7) . . . . ?
N2 C4 C5 C6 -177.8(4) . . . . ?
C4 C5 C6 C7 0.9(7) . . . . ?
C5 C6 C7 C8 -1.2(7) . . . . ?
C4 N3 C8 C7 2.1(6) . . . . ?
Fe1 N3 C8 C7 -177.6(3) . . . . ?
C6 C7 C8 N3 -0.3(7) . . . . ?
C10 N4 C9 N1 -18.0(6) . . . . ?
C11 N4 C9 N1 169.2(4) . . . . ?
C10 N4 C9 C18 105.8(5) . . . . ?
C11 N4 C9 C18 -66.9(6) . . . . ?
C1 N1 C9 N4 15.9(6) . . . . ?
C2 N1 C9 N4 -171.0(4) . . . . ?
C1 N1 C9 C18 -107.0(5) . . . . ?
C2 N1 C9 C18 66.1(6) . . . . ?
C11 N4 C10 N5 -0.9(5) . . . . ?
C9 N4 C10 N5 -174.4(4) . . . . ?
C11 N4 C10 Fe1 -175.7(4) . . . . ?
C9 N4 C10 Fe1 10.7(7) . . . . ?
C13 N5 C10 N4 179.9(4) . . . . ?
C12 N5 C10 N4 0.9(5) . . . . ?
C13 N5 C10 Fe1 -4.3(5) . . . . ?
C12 N5 C10 Fe1 176.7(3) . . . . ?
C1 Fe1 C10 N4 0.7(5) . . . . ?
N7 Fe1 C10 N4 -91.8(5) . . . . ?
N8 Fe1 C10 N4 92.7(5) . . . . ?
N3 Fe1 C10 N4 7.7(10) . . . . ?
N6 Fe1 C10 N4 179.2(5) . . . . ?
C1 Fe1 C10 N5 -173.6(4) . . . . ?
N7 Fe1 C10 N5 93.9(4) . . . . ?
N8 Fe1 C10 N5 -81.6(4) . . . . ?
N3 Fe1 C10 N5 -166.5(5) . . . . ?
N6 Fe1 C10 N5 5.0(3) . . . . ?
C10 N4 C11 C12 0.6(5) . . . . ?
C9 N4 C11 C12 174.3(4) . . . . ?
N4 C11 C12 N5 0.0(5) . . . . ?
C10 N5 C12 C11 -0.6(5) . . . . ?
C13 N5 C12 C11 -179.4(4) . . . . ?
C17 N6 C13 C14 1.9(6) . . . . ?
Fe1 N6 C13 C14 -174.9(4) . . . . ?
C17 N6 C13 N5 -179.1(4) . . . . ?
Fe1 N6 C13 N5 4.1(4) . . . . ?
C10 N5 C13 N6 -0.4(5) . . . . ?
C12 N5 C13 N6 178.3(4) . . . . ?
C10 N5 C13 C14 178.6(4) . . . . ?
C12 N5 C13 C14 -2.6(8) . . . . ?
N6 C13 C14 C15 -1.0(7) . . . . ?
N5 C13 C14 C15 -180.0(4) . . . . ?
C13 C14 C15 C16 0.3(7) . . . . ?
C14 C15 C16 C17 -0.4(7) . . . . ?
C13 N6 C17 C16 -2.0(6) . . . . ?
Fe1 N6 C17 C16 174.0(3) . . . . ?
C15 C16 C17 N6 1.3(7) . . . . ?
N4 C9 C18 O1 -63.3(5) . . . . ?
N1 C9 C18 O1 59.3(5) . . . . ?

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_C2a
_database_code_depnum_ccdc_archive 'CCDC 1811954'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H32 Fe N8 O2, 2(F6 P), C2 H3 N'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C30 H35 F12 Fe N9 O2 P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         899.46
_chemical_compound_source        'see text'

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'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   8.7808(6)
_cell_length_b                   14.7730(11)
_cell_length_c                   15.2524(11)
_cell_angle_alpha                76.461(2)
_cell_angle_beta                 87.564(2)
_cell_angle_gamma                79.042(2)
_cell_volume                     1888.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9864
_cell_measurement_theta_min      2.3625
_cell_measurement_theta_max      25.6805
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear orange'

_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.107
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             916
_exptl_absorpt_coefficient_mu    0.586
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           20 s per frame
dx                                  34 mm
2247 frames measured in 5 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            63057
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6669
# number of observed reflections (> n sig(I))
_reflns_number_gt                5808
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0427P)²+11.1838P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6669
_refine_ls_number_parameters     556
_refine_ls_number_restraints     55
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.1658
_refine_ls_wR_factor_gt          0.1601
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.102

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.57460(7) 0.24176(4) 0.20147(4) 0.01276(17) Uani 1 1 d . . . . .
O1 O 0.5984(4) 0.3164(3) 0.5303(2) 0.0303(9) Uani 1 1 d . . . . .
O2 O 0.7237(5) 0.4303(3) 0.5470(3) 0.0354(9) Uani 1 1 d . . . . .
N1 N 0.5427(4) 0.2162(3) 0.3980(3) 0.0179(8) Uani 1 1 d . . . . .
N2 N 0.6776(5) 0.0992(3) 0.3503(3) 0.0198(9) Uani 1 1 d . . . . .
N3 N 0.7171(4) 0.1118(3) 0.1987(3) 0.0171(8) Uani 1 1 d . . . . .
N4 N 0.4055(4) 0.3658(3) 0.3132(3) 0.0163(8) Uani 1 1 d . . . . .
N5 N 0.3721(4) 0.4141(3) 0.1697(3) 0.0153(8) Uani 1 1 d . . . . .
N6 N 0.5012(4) 0.3243(3) 0.0753(3) 0.0152(8) Uani 1 1 d . . . . .
N7 N 0.7547(4) 0.2983(3) 0.1923(3) 0.0161(8) Uani 1 1 d . . . . .
N8 N 0.3975(4) 0.1826(3) 0.2009(3) 0.0171(8) Uani 1 1 d . . . . .
C1 C 0.5998(5) 0.1900(3) 0.3228(3) 0.0162(9) Uani 1 1 d . . . . .
C2 C 0.5838(6) 0.1409(4) 0.4735(3) 0.0258(11) Uani 1 1 d . . . . .
H2 H 0.5572 0.1414 0.5345 0.031 Uiso 1 1 calc R U . . .
C3 C 0.6676(6) 0.0683(4) 0.4437(3) 0.0281(12) Uani 1 1 d . . . . .
H3 H 0.7114 0.0077 0.4792 0.034 Uiso 1 1 calc R U . . .
C4 C 0.7469(5) 0.0558(3) 0.2816(3) 0.0189(10) Uani 1 1 d . . . . .
C5 C 0.8354(7) -0.0345(4) 0.2977(4) 0.0298(12) Uani 1 1 d . . . . .
H5 H 0.8548 -0.0714 0.3575 0.036 Uiso 1 1 calc R U . . .
C6 C 0.8947(7) -0.0697(4) 0.2244(4) 0.0317(13) Uani 1 1 d . . . . .
H6 H 0.9533 -0.1322 0.2329 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8681(6) -0.0132(4) 0.1390(4) 0.0284(12) Uani 1 1 d . . . . .
H7 H 0.9098 -0.0357 0.0879 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7792(5) 0.0773(3) 0.1284(3) 0.0210(10) Uani 1 1 d . . . . .
H8 H 0.7618 0.1161 0.0692 0.025 Uiso 1 1 calc R U . . .
C9 C 0.4503(5) 0.3431(3) 0.2340(3) 0.0143(9) Uani 1 1 d . . . . .
C10 C 0.3006(5) 0.4529(3) 0.2978(3) 0.0186(10) Uani 1 1 d . . . . .
H10 H 0.2532 0.4843 0.3425 0.022 Uiso 1 1 calc R U . . .
C11 C 0.2799(5) 0.4834(3) 0.2076(3) 0.0187(10) Uani 1 1 d . . . . .
H11 H 0.2159 0.5402 0.1764 0.022 Uiso 1 1 calc R U . . .
C12 C 0.3968(5) 0.4033(3) 0.0797(3) 0.0148(9) Uani 1 1 d . . . . .
C13 C 0.3229(5) 0.4671(3) 0.0065(3) 0.0194(10) Uani 1 1 d . . . . .
H13 H 0.2494 0.5211 0.0135 0.023 Uiso 1 1 calc R U . . .
C14 C 0.3602(6) 0.4495(3) -0.0781(3) 0.0209(10) Uani 1 1 d . . . . .
H14 H 0.3128 0.4919 -0.1307 0.025 Uiso 1 1 calc R U . . .
C15 C 0.4673(6) 0.3694(3) -0.0849(3) 0.0219(10) Uani 1 1 d . . . . .
H15 H 0.4938 0.3562 -0.1423 0.026 Uiso 1 1 calc R U . . .
C16 C 0.5346(5) 0.3092(3) -0.0080(3) 0.0185(10) Uani 1 1 d . . . . .
H16 H 0.6079 0.2546 -0.0136 0.022 Uiso 1 1 calc R U . . .
C17 C 0.4619(5) 0.3115(3) 0.4024(3) 0.0181(10) Uani 1 1 d . . . . .
H17 H 0.3714 0.3059 0.4440 0.022 Uiso 1 1 calc R U . . .
C18 C 0.5690(6) 0.3656(3) 0.4373(3) 0.0215(10) Uani 1 1 d . . . . .
H18A H 0.6668 0.3645 0.4025 0.026 Uiso 1 1 calc R U . . .
H18B H 0.5180 0.4323 0.4329 0.026 Uiso 1 1 calc R U . . .
C19 C 0.6810(7) 0.3561(4) 0.5777(4) 0.0327(13) Uani 1 1 d . . . . .
C20 C 0.7026(16) 0.2933(8) 0.6772(9) 0.0375(19) Uani 0.560(10) 1 d D U P A 1
H20A H 0.8148 0.2686 0.6879 0.045 Uiso 0.560(10) 1 calc R U P A 1
H20B H 0.6677 0.3349 0.7193 0.045 Uiso 0.560(10) 1 calc R U P A 1
C21 C 0.6224(15) 0.2138(7) 0.7002(6) 0.0387(19) Uani 0.560(10) 1 d D U P A 1
H21A H 0.6589 0.1704 0.6599 0.046 Uiso 0.560(10) 1 calc R U P A 1
H21B H 0.5099 0.2375 0.6893 0.046 Uiso 0.560(10) 1 calc R U P A 1
C22 C 0.6484(13) 0.1562(7) 0.8024(6) 0.0398(18) Uani 0.560(10) 1 d D U P A 1
H22A H 0.7572 0.1220 0.8105 0.048 Uiso 0.560(10) 1 calc R U P A 1
H22B H 0.6307 0.2012 0.8424 0.048 Uiso 0.560(10) 1 calc R U P A 1
C23 C 0.5364(14) 0.0831(8) 0.8303(7) 0.0413(19) Uani 0.560(10) 1 d D U P A 1
H23A H 0.4275 0.1167 0.8299 0.050 Uiso 0.560(10) 1 calc R U P A 1
H23B H 0.5460 0.0412 0.7876 0.050 Uiso 0.560(10) 1 calc R U P A 1
C24 C 0.5840(15) 0.0235(8) 0.9274(7) 0.046(2) Uani 0.560(10) 1 d D U P A 1
H24A H 0.5318 -0.0312 0.9420 0.069 Uiso 0.560(10) 1 calc R U P A 1
H24B H 0.5535 0.0630 0.9710 0.069 Uiso 0.560(10) 1 calc R U P A 1
H24C H 0.6966 0.0014 0.9301 0.069 Uiso 0.560(10) 1 calc R U P A 1
C20A C 0.735(2) 0.3069(11) 0.6701(17) 0.074(3) Uani 0.440(10) 1 d D U P A 2
H20C H 0.8477 0.3055 0.6749 0.089 Uiso 0.440(10) 1 calc R U P A 2
H20D H 0.6805 0.3417 0.7138 0.089 Uiso 0.440(10) 1 calc R U P A 2
C21A C 0.7058(15) 0.2109(9) 0.6913(13) 0.074(3) Uani 0.440(10) 1 d D U P A 2
H21C H 0.7720 0.1730 0.7429 0.089 Uiso 0.440(10) 1 calc R U P A 2
H21D H 0.7353 0.1825 0.6390 0.089 Uiso 0.440(10) 1 calc R U P A 2
C22A C 0.5288(15) 0.2057(9) 0.7159(12) 0.075(3) Uani 0.440(10) 1 d D U P A 2
H22C H 0.4920 0.2464 0.7585 0.090 Uiso 0.440(10) 1 calc R U P A 2
H22D H 0.4650 0.2305 0.6605 0.090 Uiso 0.440(10) 1 calc R U P A 2
C23A C 0.5066(18) 0.1016(10) 0.7594(11) 0.076(3) Uani 0.440(10) 1 d D U P A 2
H23C H 0.3956 0.0971 0.7586 0.091 Uiso 0.440(10) 1 calc R U P A 2
H23D H 0.5659 0.0572 0.7252 0.091 Uiso 0.440(10) 1 calc R U P A 2
C24A C 0.567(3) 0.0763(14) 0.8586(10) 0.078(4) Uani 0.440(10) 1 d D U P A 2
H24D H 0.5985 0.0074 0.8790 0.117 Uiso 0.440(10) 1 calc R U P A 2
H24E H 0.4847 0.0992 0.8977 0.117 Uiso 0.440(10) 1 calc R U P A 2
H24F H 0.6567 0.1064 0.8614 0.117 Uiso 0.440(10) 1 calc R U P A 2
C25 C 0.8620(5) 0.3319(3) 0.1866(3) 0.0189(10) Uani 1 1 d . . . . .
C26 C 0.9988(6) 0.3758(3) 0.1798(4) 0.0256(11) Uani 1 1 d . . . . .
H26A H 1.0636 0.3602 0.1296 0.038 Uiso 1 1 calc R U . . .
H26B H 1.0584 0.3520 0.2361 0.038 Uiso 1 1 calc R U . . .
H26C H 0.9664 0.4447 0.1693 0.038 Uiso 1 1 calc R U . . .
C27 C 0.2892(6) 0.1510(3) 0.2034(3) 0.0227(11) Uani 1 1 d . . . . .
C28 C 0.1464(7) 0.1124(4) 0.2076(5) 0.0396(14) Uani 1 1 d . . . . .
H28A H 0.1722 0.0431 0.2211 0.059 Uiso 1 1 calc R U . . .
H28B H 0.0925 0.1358 0.1494 0.059 Uiso 1 1 calc R U . . .
H28C H 0.0790 0.1326 0.2550 0.059 Uiso 1 1 calc R U . . .
P1 P 1.03349(15) 0.27740(9) -0.06720(9) 0.0245(3) Uani 1 1 d . . . . .
F1 F 1.0511(5) 0.3831(2) -0.1131(3) 0.0568(11) Uani 1 1 d . . . . .
F2 F 1.0128(5) 0.1719(2) -0.0215(3) 0.0535(10) Uani 1 1 d . . . . .
F3 F 1.1544(4) 0.2747(2) 0.0089(2) 0.0405(8) Uani 1 1 d . . . . .
F4 F 1.1727(5) 0.2372(3) -0.1253(3) 0.0584(11) Uani 1 1 d . . . . .
F5 F 0.9136(5) 0.2812(3) -0.1444(3) 0.0629(12) Uani 1 1 d . . . . .
F6 F 0.8940(4) 0.3166(3) -0.0090(3) 0.0639(12) Uani 1 1 d . . . . .
P2 P 1.06119(15) 0.22333(9) 0.45030(9) 0.0251(3) Uani 1 1 d . . . . .
F7 F 1.0642(6) 0.3322(3) 0.4417(3) 0.0703(13) Uani 1 1 d . . . . .
F8 F 1.0639(5) 0.1150(3) 0.4618(3) 0.0621(12) Uani 1 1 d . . . . .
F9 F 1.2104(4) 0.1977(3) 0.5154(2) 0.0576(12) Uani 1 1 d . . . . .
F10 F 1.1730(4) 0.2276(3) 0.3654(2) 0.0458(9) Uani 1 1 d . . . . .
F11 F 0.9150(4) 0.2478(3) 0.3855(3) 0.0558(11) Uani 1 1 d . . . . .
F12 F 0.9515(4) 0.2222(3) 0.5360(3) 0.0592(11) Uani 1 1 d . . . . .
N9 N 0.6567(9) 0.5464(6) 0.2970(5) 0.086(3) Uani 1 1 d . . . . .
C29 C 0.7565(8) 0.5659(5) 0.3284(5) 0.0493(17) Uani 1 1 d . . . . .
C30 C 0.8930(10) 0.5839(7) 0.3672(6) 0.077(3) Uani 1 1 d . . . . .
H30A H 0.8610 0.6292 0.4053 0.116 Uiso 1 1 calc R U . . .
H30B H 0.9600 0.6103 0.3187 0.116 Uiso 1 1 calc R U . . .
H30C H 0.9500 0.5244 0.4037 0.116 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C9 1.833(4) . ?
Fe1 C1 1.835(5) . ?
Fe1 N7 1.910(4) . ?
Fe1 N8 1.924(4) . ?
Fe1 N6 2.077(4) . ?
Fe1 N3 2.091(4) . ?
O1 C19 1.342(6) . ?
O1 C18 1.443(6) . ?
O2 C19 1.208(7) . ?
N1 C1 1.341(6) . ?
N1 C2 1.407(6) . ?
N1 C17 1.467(6) . ?
N2 C1 1.361(6) . ?
N2 C3 1.396(6) . ?
N2 C4 1.410(6) . ?
N3 C4 1.345(6) . ?
N3 C8 1.345(6) . ?
N4 C9 1.351(6) . ?
N4 C10 1.409(6) . ?
N4 C17 1.460(6) . ?
N5 C9 1.355(6) . ?
N5 C11 1.401(6) . ?
N5 C12 1.421(6) . ?
N6 C16 1.351(6) . ?
N6 C12 1.352(6) . ?
N7 C25 1.137(6) . ?
N8 C27 1.132(6) . ?
C2 C3 1.341(7) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.383(7) . ?
C5 C6 1.383(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(7) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C10 C11 1.353(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.376(7) . ?
C13 C14 1.389(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.528(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20A 1.48(2) . ?
C19 C20 1.581(14) . ?
C20 C21 1.448(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.594(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.571(13) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.563(12) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C20A C21A 1.448(11) . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C21A C22A 1.595(12) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A C23A 1.571(13) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A C24A 1.563(12) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25 C26 1.460(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.466(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
P1 F6 1.582(4) . ?
P1 F4 1.584(4) . ?
P1 F1 1.589(4) . ?
P1 F2 1.593(4) . ?
P1 F3 1.595(3) . ?
P1 F5 1.596(4) . ?
P2 F8 1.565(4) . ?
P2 F11 1.587(3) . ?
P2 F7 1.588(4) . ?
P2 F10 1.588(3) . ?
P2 F12 1.590(4) . ?
P2 F9 1.610(4) . ?
N9 C29 1.129(9) . ?
C29 C30 1.453(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 Fe1 C1 86.0(2) . . ?
C9 Fe1 N7 92.97(17) . . ?
C1 Fe1 N7 93.81(18) . . ?
C9 Fe1 N8 90.24(17) . . ?
C1 Fe1 N8 90.03(18) . . ?
N7 Fe1 N8 175.16(16) . . ?
C9 Fe1 N6 79.71(17) . . ?
C1 Fe1 N6 165.39(17) . . ?
N7 Fe1 N6 90.13(15) . . ?
N8 Fe1 N6 86.88(15) . . ?
C9 Fe1 N3 165.77(18) . . ?
C1 Fe1 N3 79.80(17) . . ?
N7 Fe1 N3 89.29(15) . . ?
N8 Fe1 N3 88.47(15) . . ?
N6 Fe1 N3 114.35(15) . . ?
C19 O1 C18 115.6(4) . . ?
C1 N1 C2 109.8(4) . . ?
C1 N1 C17 125.4(4) . . ?
C2 N1 C17 124.5(4) . . ?
C1 N2 C3 110.3(4) . . ?
C1 N2 C4 116.1(4) . . ?
C3 N2 C4 133.5(4) . . ?
C4 N3 C8 117.3(4) . . ?
C4 N3 Fe1 112.5(3) . . ?
C8 N3 Fe1 130.2(3) . . ?
C9 N4 C10 110.2(4) . . ?
C9 N4 C17 125.8(4) . . ?
C10 N4 C17 124.0(4) . . ?
C9 N5 C11 111.3(4) . . ?
C9 N5 C12 115.4(4) . . ?
C11 N5 C12 133.3(4) . . ?
C16 N6 C12 116.3(4) . . ?
C16 N6 Fe1 130.6(3) . . ?
C12 N6 Fe1 112.9(3) . . ?
C25 N7 Fe1 179.8(4) . . ?
C27 N8 Fe1 176.2(4) . . ?
N1 C1 N2 105.9(4) . . ?
N1 C1 Fe1 134.9(3) . . ?
N2 C1 Fe1 118.6(3) . . ?
C3 C2 N1 107.4(4) . . ?
C3 C2 H2 126.3 . . ?
N1 C2 H2 126.3 . . ?
C2 C3 N2 106.5(4) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
N3 C4 C5 123.6(4) . . ?
N3 C4 N2 112.6(4) . . ?
C5 C4 N2 123.8(4) . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C7 C6 C5 119.2(5) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 119.2(5) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
N3 C8 C7 122.4(5) . . ?
N3 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
N4 C9 N5 105.4(4) . . ?
N4 C9 Fe1 134.9(3) . . ?
N5 C9 Fe1 119.6(3) . . ?
C11 C10 N4 107.2(4) . . ?
C11 C10 H10 126.4 . . ?
N4 C10 H10 126.4 . . ?
C10 C11 N5 105.9(4) . . ?
C10 C11 H11 127.1 . . ?
N5 C11 H11 127.1 . . ?
N6 C12 C13 124.8(4) . . ?
N6 C12 N5 112.1(4) . . ?
C13 C12 N5 123.0(4) . . ?
C12 C13 C14 117.3(4) . . ?
C12 C13 H13 121.3 . . ?
C14 C13 H13 121.3 . . ?
C15 C14 C13 119.2(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 119.4(5) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
N6 C16 C15 122.9(4) . . ?
N6 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
N4 C17 N1 110.6(4) . . ?
N4 C17 C18 108.3(4) . . ?
N1 C17 C18 111.3(4) . . ?
N4 C17 H17 108.9 . . ?
N1 C17 H17 108.9 . . ?
C18 C17 H17 108.9 . . ?
O1 C18 C17 104.8(4) . . ?
O1 C18 H18A 110.8 . . ?
C17 C18 H18A 110.8 . . ?
O1 C18 H18B 110.8 . . ?
C17 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
O2 C19 O1 123.2(5) . . ?
O2 C19 C20A 115.8(7) . . ?
O1 C19 C20A 120.9(8) . . ?
O2 C19 C20 127.8(6) . . ?
O1 C19 C20 108.9(6) . . ?
C21 C20 C19 116.9(9) . . ?
C21 C20 H20A 108.1 . . ?
C19 C20 H20A 108.1 . . ?
C21 C20 H20B 108.1 . . ?
C19 C20 H20B 108.1 . . ?
H20A C20 H20B 107.3 . . ?
C20 C21 C22 113.1(8) . . ?
C20 C21 H21A 109.0 . . ?
C22 C21 H21A 109.0 . . ?
C20 C21 H21B 109.0 . . ?
C22 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C23 C22 C21 111.8(7) . . ?
C23 C22 H22A 109.2 . . ?
C21 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C21 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C22 107.4(7) . . ?
C24 C23 H23A 110.2 . . ?
C22 C23 H23A 110.2 . . ?
C24 C23 H23B 110.2 . . ?
C22 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21A C20A C19 110.2(16) . . ?
C21A C20A H20C 109.6 . . ?
C19 C20A H20C 109.6 . . ?
C21A C20A H20D 109.6 . . ?
C19 C20A H20D 109.6 . . ?
H20C C20A H20D 108.1 . . ?
C20A C21A C22A 112.9(8) . . ?
C20A C21A H21C 109.0 . . ?
C22A C21A H21C 109.0 . . ?
C20A C21A H21D 109.0 . . ?
C22A C21A H21D 109.0 . . ?
H21C C21A H21D 107.8 . . ?
C23A C22A C21A 111.9(7) . . ?
C23A C22A H22C 109.2 . . ?
C21A C22A H22C 109.2 . . ?
C23A C22A H22D 109.2 . . ?
C21A C22A H22D 109.2 . . ?
H22C C22A H22D 107.9 . . ?
C24A C23A C22A 107.4(8) . . ?
C24A C23A H23C 110.2 . . ?
C22A C23A H23C 110.2 . . ?
C24A C23A H23D 110.2 . . ?
C22A C23A H23D 110.2 . . ?
H23C C23A H23D 108.5 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
N7 C25 C26 179.4(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N8 C27 C28 178.4(6) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
F6 P1 F4 179.5(2) . . ?
F6 P1 F1 89.5(2) . . ?
F4 P1 F1 91.0(2) . . ?
F6 P1 F2 89.8(2) . . ?
F4 P1 F2 89.7(2) . . ?
F1 P1 F2 179.0(2) . . ?
F6 P1 F3 90.9(2) . . ?
F4 P1 F3 89.3(2) . . ?
F1 P1 F3 89.79(19) . . ?
F2 P1 F3 90.9(2) . . ?
F6 P1 F5 89.5(2) . . ?
F4 P1 F5 90.3(2) . . ?
F1 P1 F5 89.5(2) . . ?
F2 P1 F5 89.8(2) . . ?
F3 P1 F5 179.2(2) . . ?
F8 P2 F11 90.4(2) . . ?
F8 P2 F7 177.6(3) . . ?
F11 P2 F7 92.1(3) . . ?
F8 P2 F10 92.5(2) . . ?
F11 P2 F10 90.0(2) . . ?
F7 P2 F10 87.7(2) . . ?
F8 P2 F12 89.3(3) . . ?
F11 P2 F12 90.9(2) . . ?
F7 P2 F12 90.4(2) . . ?
F10 P2 F12 177.9(2) . . ?
F8 P2 F9 89.2(2) . . ?
F11 P2 F9 179.4(3) . . ?
F7 P2 F9 88.4(3) . . ?
F10 P2 F9 89.5(2) . . ?
F12 P2 F9 89.5(2) . . ?
N9 C29 C30 175.2(9) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 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
C2 N1 C1 N2 -0.5(5) . . . . ?
C17 N1 C1 N2 174.2(4) . . . . ?
C2 N1 C1 Fe1 170.6(4) . . . . ?
C17 N1 C1 Fe1 -14.7(7) . . . . ?
C3 N2 C1 N1 0.5(5) . . . . ?
C4 N2 C1 N1 179.2(4) . . . . ?
C3 N2 C1 Fe1 -172.2(3) . . . . ?
C4 N2 C1 Fe1 6.5(5) . . . . ?
C9 Fe1 C1 N1 3.1(5) . . . . ?
N7 Fe1 C1 N1 95.8(5) . . . . ?
N8 Fe1 C1 N1 -87.1(5) . . . . ?
N6 Fe1 C1 N1 -9.5(10) . . . . ?
N3 Fe1 C1 N1 -175.6(5) . . . . ?
C9 Fe1 C1 N2 173.3(4) . . . . ?
N7 Fe1 C1 N2 -94.0(4) . . . . ?
N8 Fe1 C1 N2 83.0(4) . . . . ?
N6 Fe1 C1 N2 160.7(5) . . . . ?
N3 Fe1 C1 N2 -5.4(3) . . . . ?
C1 N1 C2 C3 0.2(6) . . . . ?
C17 N1 C2 C3 -174.5(4) . . . . ?
N1 C2 C3 N2 0.1(6) . . . . ?
C1 N2 C3 C2 -0.4(6) . . . . ?
C4 N2 C3 C2 -178.8(5) . . . . ?
C8 N3 C4 C5 -0.7(7) . . . . ?
Fe1 N3 C4 C5 178.5(4) . . . . ?
C8 N3 C4 N2 179.4(4) . . . . ?
Fe1 N3 C4 N2 -1.4(5) . . . . ?
C1 N2 C4 N3 -2.8(6) . . . . ?
C3 N2 C4 N3 175.5(5) . . . . ?
C1 N2 C4 C5 177.3(5) . . . . ?
C3 N2 C4 C5 -4.4(8) . . . . ?
N3 C4 C5 C6 -1.0(8) . . . . ?
N2 C4 C5 C6 178.9(5) . . . . ?
C4 C5 C6 C7 2.0(8) . . . . ?
C5 C6 C7 C8 -1.3(8) . . . . ?
C4 N3 C8 C7 1.4(7) . . . . ?
Fe1 N3 C8 C7 -177.6(4) . . . . ?
C6 C7 C8 N3 -0.4(8) . . . . ?
C10 N4 C9 N5 -1.2(5) . . . . ?
C17 N4 C9 N5 -178.3(4) . . . . ?
C10 N4 C9 Fe1 -177.1(4) . . . . ?
C17 N4 C9 Fe1 5.7(7) . . . . ?
C11 N5 C9 N4 1.4(5) . . . . ?
C12 N5 C9 N4 -177.6(3) . . . . ?
C11 N5 C9 Fe1 178.1(3) . . . . ?
C12 N5 C9 Fe1 -0.9(5) . . . . ?
C1 Fe1 C9 N4 1.4(5) . . . . ?
N7 Fe1 C9 N4 -92.3(5) . . . . ?
N8 Fe1 C9 N4 91.4(5) . . . . ?
N6 Fe1 C9 N4 178.2(5) . . . . ?
N3 Fe1 C9 N4 6.6(10) . . . . ?
C1 Fe1 C9 N5 -174.1(4) . . . . ?
N7 Fe1 C9 N5 92.3(4) . . . . ?
N8 Fe1 C9 N5 -84.1(4) . . . . ?
N6 Fe1 C9 N5 2.7(3) . . . . ?
N3 Fe1 C9 N5 -168.8(5) . . . . ?
C9 N4 C10 C11 0.6(5) . . . . ?
C17 N4 C10 C11 177.8(4) . . . . ?
N4 C10 C11 N5 0.3(5) . . . . ?
C9 N5 C11 C10 -1.1(5) . . . . ?
C12 N5 C11 C10 177.7(4) . . . . ?
C16 N6 C12 C13 0.8(6) . . . . ?
Fe1 N6 C12 C13 -176.0(4) . . . . ?
C16 N6 C12 N5 -178.6(4) . . . . ?
Fe1 N6 C12 N5 4.6(4) . . . . ?
C9 N5 C12 N6 -2.7(5) . . . . ?
C11 N5 C12 N6 178.6(4) . . . . ?
C9 N5 C12 C13 177.9(4) . . . . ?
C11 N5 C12 C13 -0.8(7) . . . . ?
N6 C12 C13 C14 -0.9(7) . . . . ?
N5 C12 C13 C14 178.5(4) . . . . ?
C12 C13 C14 C15 0.5(7) . . . . ?
C13 C14 C15 C16 -0.2(7) . . . . ?
C12 N6 C16 C15 -0.3(6) . . . . ?
Fe1 N6 C16 C15 175.8(3) . . . . ?
C14 C15 C16 N6 0.1(7) . . . . ?
C9 N4 C17 N1 -15.0(6) . . . . ?
C10 N4 C17 N1 168.3(4) . . . . ?
C9 N4 C17 C18 107.2(5) . . . . ?
C10 N4 C17 C18 -69.6(5) . . . . ?
C1 N1 C17 N4 19.0(6) . . . . ?
C2 N1 C17 N4 -167.0(4) . . . . ?
C1 N1 C17 C18 -101.4(5) . . . . ?
C2 N1 C17 C18 72.5(6) . . . . ?
C19 O1 C18 C17 -174.8(4) . . . . ?
N4 C17 C18 O1 170.7(4) . . . . ?
N1 C17 C18 O1 -67.6(5) . . . . ?
C18 O1 C19 O2 2.9(8) . . . . ?
C18 O1 C19 C20A -172.6(11) . . . . ?
C18 O1 C19 C20 -179.9(6) . . . . ?
O2 C19 C20 C21 171.9(9) . . . . ?
O1 C19 C20 C21 -5.2(13) . . . . ?
C19 C20 C21 C22 -178.8(9) . . . . ?
C20 C21 C22 C23 169.3(11) . . . . ?
C21 C22 C23 C24 174.0(10) . . . . ?
O2 C19 C20A C21A -167.5(8) . . . . ?
O1 C19 C20A C21A 8.3(16) . . . . ?
C19 C20A C21A C22A -77.6(17) . . . . ?
C20A C21A C22A C23A -167.1(16) . . . . ?
C21A C22A C23A C24A 75.4(19) . . . . ?


####################################################################### 
# 
# 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_C3
_database_code_depnum_ccdc_archive 'CCDC 1811951'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-01-05 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C44 H44 Fe2 N16 O2, 4(F6 P), 4(C2 H3 N)'
_chemical_formula_sum            'C52 H56 F24 Fe2 N20 O2 P4'
_chemical_formula_weight         1684.75

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'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   11.6283(4)
_cell_length_b                   22.8419(9)
_cell_length_c                   12.9950(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.920(2)
_cell_angle_gamma                90
_cell_volume                     3335.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9558
_cell_measurement_theta_min      2.4106
_cell_measurement_theta_max      25.6516

_exptl_crystal_description       fragment
_exptl_crystal_colour            red

_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.324
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           1 s per frame
dx                                  35 mm
3368 frames measured in 6 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_monochromator  'Montel mirror optics'

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            89648
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6096
# number of observed reflections (> n sig(I))
_reflns_number_gt                5687
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0298P)²+3.2282P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed

_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     shelxl
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC²Λ³/SIN(2Θ)]^-1/4^
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6096
_refine_ls_number_parameters     533
_refine_ls_number_restraints     78
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.053

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.30953(2) 0.09154(2) 0.41881(2) 0.01551(9) Uani 1 1 d . . . . .
O1 O 0.67472(14) 0.04579(7) 0.82385(11) 0.0293(3) Uani 1 1 d . . . . .
N1 N 0.49875(14) -0.09607(6) 0.67088(12) 0.0191(3) Uani 1 1 d . . . . .
N2 N 0.51879(13) -0.00383(6) 0.65187(11) 0.0166(3) Uani 1 1 d . . . . .
N3 N 0.62241(14) -0.16414(6) 0.62820(11) 0.0189(3) Uani 1 1 d . . . . .
N4 N 0.48454(14) 0.09910(6) 0.64419(12) 0.0182(3) Uani 1 1 d . . . . .
N5 N 0.32262(14) 0.14881(6) 0.60959(12) 0.0193(3) Uani 1 1 d . . . . .
N6 N 0.17841(14) 0.13903(6) 0.45419(12) 0.0189(3) Uani 1 1 d . . . . .
N7 N 0.24358(13) 0.02216(6) 0.46630(12) 0.0186(3) Uani 1 1 d . . . . .
N8 N 0.21323(14) 0.07955(7) 0.27193(12) 0.0200(3) Uani 1 1 d . . . . .
C1 C 0.56194(16) -0.05607(7) 0.62834(13) 0.0168(4) Uani 1 1 d . . . . .
C2 C 0.43250(17) -0.01171(8) 0.70872(14) 0.0214(4) Uani 1 1 d . . . . .
H2 H 0.3908 0.0184 0.7343 0.026 Uiso 1 1 calc R U . . .
C3 C 0.41962(17) -0.06933(8) 0.72030(15) 0.0224(4) Uani 1 1 d . . . . .
H3 H 0.3672 -0.0881 0.7551 0.027 Uiso 1 1 calc R U . . .
C4 C 0.52901(17) -0.15542(8) 0.66959(14) 0.0209(4) Uani 1 1 d . . . . .
C5 C 0.4697(2) -0.19980(9) 0.70744(17) 0.0307(5) Uani 1 1 d . . . . .
H5 H 0.4045 -0.1914 0.7366 0.037 Uiso 1 1 calc R U . . .
C6 C 0.5082(2) -0.25637(9) 0.70143(18) 0.0342(5) Uani 1 1 d . . . . .
H6 H 0.4699 -0.2879 0.7268 0.041 Uiso 1 1 calc R U . . .
C7 C 0.6029(2) -0.26682(9) 0.65814(17) 0.0304(5) Uani 1 1 d . . . . .
H7 H 0.6300 -0.3056 0.6528 0.037 Uiso 1 1 calc R U . . .
C8 C 0.65746(18) -0.22027(8) 0.62287(15) 0.0242(4) Uani 1 1 d . . . . .
H8 H 0.7227 -0.2279 0.5934 0.029 Uiso 1 1 calc R U . . .
C9 C 0.57138(16) 0.05392(7) 0.63847(14) 0.0176(4) Uani 1 1 d . . . . .
H9 H 0.5867 0.0553 0.5662 0.021 Uiso 1 1 calc R U . . .
C10 C 0.38574(16) 0.11028(7) 0.56452(14) 0.0171(4) Uani 1 1 d . . . . .
C11 C 0.48221(18) 0.13078(8) 0.73700(15) 0.0245(4) Uani 1 1 d . . . . .
H11 H 0.5414 0.1303 0.8029 0.029 Uiso 1 1 calc R U . . .
C12 C 0.38126(18) 0.16150(8) 0.71471(15) 0.0249(4) Uani 1 1 d . . . . .
H12 H 0.3546 0.1870 0.7615 0.030 Uiso 1 1 calc R U . . .
C13 C 0.20821(16) 0.16523(8) 0.55024(15) 0.0194(4) Uani 1 1 d . . . . .
C14 C 0.13564(18) 0.20389(8) 0.58575(16) 0.0256(4) Uani 1 1 d . . . . .
H14 H 0.1607 0.2215 0.6541 0.031 Uiso 1 1 calc R U . . .
C15 C 0.02529(19) 0.21608(9) 0.51861(17) 0.0288(5) Uani 1 1 d . . . . .
H15 H -0.0271 0.2426 0.5400 0.035 Uiso 1 1 calc R U . . .
C16 C -0.00819(18) 0.18922(9) 0.42001(17) 0.0281(4) Uani 1 1 d . . . . .
H16 H -0.0840 0.1969 0.3731 0.034 Uiso 1 1 calc R U . . .
C17 C 0.06969(17) 0.15106(8) 0.39039(16) 0.0243(4) Uani 1 1 d . . . . .
H17 H 0.0459 0.1326 0.3227 0.029 Uiso 1 1 calc R U . . .
C18 C 0.68934(17) 0.06215(8) 0.72179(15) 0.0230(4) Uani 1 1 d . . . . .
H18A H 0.7515 0.0375 0.7037 0.028 Uiso 1 1 calc R U . . .
H18B H 0.7147 0.1036 0.7231 0.028 Uiso 1 1 calc R U . . .
C19 C 0.19592(17) -0.01385(8) 0.50054(14) 0.0201(4) Uani 1 1 d . . . . .
C20 C 0.13471(19) -0.05970(9) 0.54337(16) 0.0276(4) Uani 1 1 d . . . . .
H20A H 0.1417 -0.0521 0.6189 0.041 Uiso 1 1 calc R U . . .
H20B H 0.1708 -0.0977 0.5356 0.041 Uiso 1 1 calc R U . . .
H20C H 0.0505 -0.0602 0.5044 0.041 Uiso 1 1 calc R U . . .
C21 C 0.16317(17) 0.06963(8) 0.18622(15) 0.0220(4) Uani 1 1 d . . . . .
C22 C 0.0986(2) 0.05615(10) 0.07734(16) 0.0335(5) Uani 1 1 d . . . . .
H22A H 0.0664 0.0924 0.0405 0.050 Uiso 0.5 1 calc R U P . .
H22B H 0.0331 0.0293 0.0779 0.050 Uiso 0.5 1 calc R U P . .
H22C H 0.1526 0.0378 0.0402 0.050 Uiso 0.5 1 calc R U P . .
H22D H 0.1017 0.0139 0.0653 0.050 Uiso 0.5 1 calc R U P . .
H22E H 0.1350 0.0770 0.0278 0.050 Uiso 0.5 1 calc R U P . .
H22F H 0.0154 0.0685 0.0655 0.050 Uiso 0.5 1 calc R U P . .
H1 H 0.726(3) 0.0616(12) 0.868(2) 0.047(8) Uiso 1 1 d . . . . .
P1 P 0.77877(5) 0.14212(2) 1.07643(4) 0.02360(13) Uani 1 1 d . U . . .
F1_a F 0.70606(16) 0.08276(7) 1.07471(17) 0.0495(5) Uani 0.943(2) 1 d D . P A 1
F2_a F 0.88664(16) 0.11581(7) 1.16459(12) 0.0509(5) Uani 0.943(2) 1 d D . P A 1
F3_a F 0.84859(16) 0.20180(7) 1.07624(13) 0.0452(4) Uani 0.943(2) 1 d D . P A 1
F4_a F 0.83415(13) 0.11587(7) 0.98456(11) 0.0391(4) Uani 0.943(2) 1 d D . P A 1
F5_a F 0.72391(16) 0.16798(6) 1.16760(13) 0.0482(5) Uani 0.943(2) 1 d D . P A 1
F6_a F 0.67075(16) 0.16815(7) 0.98563(14) 0.0507(5) Uani 0.943(2) 1 d D . P A 1
F1A_b F 0.731(2) 0.0804(9) 1.034(2) 0.040(5) Uani 0.057(2) 1 d D U P A 2
F2A_b F 0.8243(19) 0.1173(9) 1.1938(15) 0.033(4) Uani 0.057(2) 1 d D U P A 2
F3A_b F 0.8205(19) 0.2079(8) 1.120(2) 0.037(5) Uani 0.057(2) 1 d D U P A 2
F4A_b F 0.8974(19) 0.1321(10) 1.047(2) 0.050(5) Uani 0.057(2) 1 d D U P A 2
F5A_b F 0.6504(16) 0.1567(9) 1.1022(18) 0.034(4) Uani 0.057(2) 1 d D U P A 2
F6A_b F 0.726(2) 0.1708(11) 0.9650(17) 0.043(5) Uani 0.057(2) 1 d D U P A 2
P2 P 0.06926(5) 0.06728(2) -0.23651(4) 0.02664(13) Uani 1 1 d . . . . .
F7 F -0.00632(12) 0.01348(5) -0.29707(10) 0.0388(3) Uani 1 1 d . . . . .
F8 F 0.14591(14) 0.12107(6) -0.17620(13) 0.0571(4) Uani 1 1 d . . . . .
F9 F -0.02100(15) 0.07380(8) -0.16266(11) 0.0580(4) Uani 1 1 d . . . . .
F10 F -0.01172(13) 0.11185(6) -0.31849(10) 0.0453(4) Uani 1 1 d . . . . .
F11 F 0.15798(15) 0.06134(6) -0.31076(14) 0.0576(4) Uani 1 1 d . . . . .
F12 F 0.14782(13) 0.02329(6) -0.15191(12) 0.0514(4) Uani 1 1 d . . . . .
N9 N 0.3545(3) 0.16314(14) 1.0548(3) 0.0858(10) Uani 1 1 d . . . . .
C23 C 0.3778(2) 0.11857(14) 1.0281(2) 0.0532(7) Uani 1 1 d . . . . .
C24 C 0.4078(2) 0.06147(13) 0.9961(2) 0.0529(7) Uani 1 1 d . . . . .
H24A H 0.4888 0.0622 0.9868 0.079 Uiso 1 1 calc R U . . .
H24B H 0.3518 0.0506 0.9287 0.079 Uiso 1 1 calc R U . . .
H24C H 0.4034 0.0328 1.0510 0.079 Uiso 1 1 calc R U . . .
N10 N 0.6891(2) 0.16796(11) 0.5413(2) 0.0591(6) Uani 1 1 d . . . . .
C25 C 0.6639(2) 0.21148(13) 0.5701(2) 0.0471(6) Uani 1 1 d . . . . .
C26 C 0.6292(3) 0.26688(16) 0.6073(3) 0.0782(11) Uani 1 1 d . . . . .
H26A H 0.7005 0.2900 0.6390 0.117 Uiso 1 1 calc R U . . .
H26B H 0.5851 0.2597 0.6610 0.117 Uiso 1 1 calc R U . . .
H26C H 0.5786 0.2884 0.5473 0.117 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C10 1.9209(18) . ?
Fe1 N7 1.9299(15) . ?
Fe1 C1 1.9333(18) 3_656 ?
Fe1 N8 1.9676(16) . ?
Fe1 N3 1.9996(15) 3_656 ?
Fe1 N6 2.0183(15) . ?
O1 C18 1.430(2) . ?
O1 H1 0.80(3) . ?
N1 C1 1.375(2) . ?
N1 C3 1.392(2) . ?
N1 C4 1.402(2) . ?
N2 C1 1.359(2) . ?
N2 C2 1.402(2) . ?
N2 C9 1.483(2) . ?
N3 C4 1.345(2) . ?
N3 C8 1.353(2) . ?
N3 Fe1 1.9995(15) 3_656 ?
N4 C10 1.358(2) . ?
N4 C11 1.413(2) . ?
N4 C9 1.459(2) . ?
N5 C10 1.370(2) . ?
N5 C12 1.391(2) . ?
N5 C13 1.406(2) . ?
N6 C13 1.347(2) . ?
N6 C17 1.350(2) . ?
N7 C19 1.144(2) . ?
N8 C21 1.139(2) . ?
C1 Fe1 1.9334(18) 3_656 ?
C2 C3 1.337(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C5 C6 1.376(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.376(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C18 1.525(3) . ?
C9 H9 1.0000 . ?
C11 C12 1.334(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C14 C15 1.382(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.455(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.454(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H22D 0.9800 . ?
C22 H22E 0.9800 . ?
C22 H22F 0.9800 . ?
P1 F4A_b 1.543(18) . ?
P1 F6A_b 1.563(19) . ?
P1 F1A_b 1.56(2) . ?
P1 F2_a 1.5833(15) . ?
P1 F2A_b 1.586(18) . ?
P1 F3_a 1.5871(15) . ?
P1 F1_a 1.5949(15) . ?
P1 F5_a 1.5965(14) . ?
P1 F6_a 1.6002(15) . ?
P1 F4_a 1.6110(13) . ?
P1 F3A_b 1.636(19) . ?
P1 F5A_b 1.646(16) . ?
P2 F11 1.5894(14) . ?
P2 F12 1.5924(14) . ?
P2 F10 1.5942(14) . ?
P2 F7 1.5956(13) . ?
P2 F8 1.5995(14) . ?
P2 F9 1.6011(15) . ?
N9 C23 1.131(4) . ?
C23 C24 1.439(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N10 C25 1.127(4) . ?
C25 C26 1.449(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Fe1 N7 89.32(7) . . ?
C10 Fe1 C1 101.99(7) . 3_656 ?
N7 Fe1 C1 99.23(7) . 3_656 ?
C10 Fe1 N8 171.95(7) . . ?
N7 Fe1 N8 91.27(6) . . ?
C1 Fe1 N8 85.85(7) 3_656 . ?
C10 Fe1 N3 89.89(7) . 3_656 ?
N7 Fe1 N3 179.04(6) . 3_656 ?
C1 Fe1 N3 81.47(7) 3_656 3_656 ?
N8 Fe1 N3 89.44(6) . 3_656 ?
C10 Fe1 N6 80.77(7) . . ?
N7 Fe1 N6 89.01(6) . . ?
C1 Fe1 N6 171.29(7) 3_656 . ?
N8 Fe1 N6 91.21(6) . . ?
N3 Fe1 N6 90.32(6) 3_656 . ?
C18 O1 H1 108(2) . . ?
C1 N1 C3 112.28(15) . . ?
C1 N1 C4 118.44(15) . . ?
C3 N1 C4 128.89(15) . . ?
C1 N2 C2 111.18(14) . . ?
C1 N2 C9 124.55(14) . . ?
C2 N2 C9 123.28(14) . . ?
C4 N3 C8 116.48(16) . . ?
C4 N3 Fe1 115.04(12) . 3_656 ?
C8 N3 Fe1 128.48(13) . 3_656 ?
C10 N4 C11 110.86(15) . . ?
C10 N4 C9 123.70(14) . . ?
C11 N4 C9 124.85(15) . . ?
C10 N5 C12 111.86(16) . . ?
C10 N5 C13 118.17(15) . . ?
C12 N5 C13 129.67(16) . . ?
C13 N6 C17 117.11(16) . . ?
C13 N6 Fe1 114.88(12) . . ?
C17 N6 Fe1 127.78(13) . . ?
C19 N7 Fe1 170.77(15) . . ?
C21 N8 Fe1 175.13(16) . . ?
N2 C1 N1 103.10(15) . . ?
N2 C1 Fe1 143.08(13) . 3_656 ?
N1 C1 Fe1 112.69(12) . 3_656 ?
C3 C2 N2 107.56(16) . . ?
C3 C2 H2 126.2 . . ?
N2 C2 H2 126.2 . . ?
C2 C3 N1 105.87(16) . . ?
C2 C3 H3 127.1 . . ?
N1 C3 H3 127.1 . . ?
N3 C4 C5 124.10(18) . . ?
N3 C4 N1 112.27(15) . . ?
C5 C4 N1 123.63(17) . . ?
C6 C5 C4 117.90(19) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 C7 119.38(19) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C8 C7 C6 119.14(19) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N3 C8 C7 123.00(18) . . ?
N3 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N4 C9 N2 108.14(14) . . ?
N4 C9 C18 112.62(14) . . ?
N2 C9 C18 110.43(14) . . ?
N4 C9 H9 108.5 . . ?
N2 C9 H9 108.5 . . ?
C18 C9 H9 108.5 . . ?
N4 C10 N5 103.65(15) . . ?
N4 C10 Fe1 142.62(13) . . ?
N5 C10 Fe1 113.73(13) . . ?
C12 C11 N4 107.06(17) . . ?
C12 C11 H11 126.5 . . ?
N4 C11 H11 126.5 . . ?
C11 C12 N5 106.57(16) . . ?
C11 C12 H12 126.7 . . ?
N5 C12 H12 126.7 . . ?
N6 C13 C14 124.10(18) . . ?
N6 C13 N5 111.79(15) . . ?
C14 C13 N5 124.11(17) . . ?
C13 C14 C15 117.79(19) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C14 C15 C16 119.32(18) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 119.33(19) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
N6 C17 C16 122.35(19) . . ?
N6 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
O1 C18 C9 109.06(15) . . ?
O1 C18 H18A 109.9 . . ?
C9 C18 H18A 109.9 . . ?
O1 C18 H18B 109.9 . . ?
C9 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
N7 C19 C20 179.6(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N8 C21 C22 179.1(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C22 H22D 109.5 . . ?
H22A C22 H22D 141.1 . . ?
H22B C22 H22D 56.3 . . ?
H22C C22 H22D 56.3 . . ?
C21 C22 H22E 109.5 . . ?
H22A C22 H22E 56.3 . . ?
H22B C22 H22E 141.1 . . ?
H22C C22 H22E 56.3 . . ?
H22D C22 H22E 109.5 . . ?
C21 C22 H22F 109.5 . . ?
H22A C22 H22F 56.3 . . ?
H22B C22 H22F 56.3 . . ?
H22C C22 H22F 141.1 . . ?
H22D C22 H22F 109.5 . . ?
H22E C22 H22F 109.5 . . ?
F4A_b P1 F6A_b 89.5(12) . . ?
F4A_b P1 F1A_b 92.1(12) . . ?
F6A_b P1 F1A_b 91.7(12) . . ?
F4A_b P1 F2A_b 95.2(11) . . ?
F6A_b P1 F2A_b 174.4(12) . . ?
F1A_b P1 F2A_b 91.2(11) . . ?
F2_a P1 F3_a 90.97(10) . . ?
F2_a P1 F1_a 90.34(10) . . ?
F3_a P1 F1_a 178.69(11) . . ?
F2_a P1 F5_a 89.83(9) . . ?
F3_a P1 F5_a 89.17(9) . . ?
F1_a P1 F5_a 90.76(9) . . ?
F2_a P1 F6_a 178.92(10) . . ?
F3_a P1 F6_a 89.10(10) . . ?
F1_a P1 F6_a 89.60(10) . . ?
F5_a P1 F6_a 91.25(10) . . ?
F2_a P1 F4_a 90.09(9) . . ?
F3_a P1 F4_a 90.93(9) . . ?
F1_a P1 F4_a 89.13(9) . . ?
F5_a P1 F4_a 179.87(9) . . ?
F6_a P1 F4_a 88.83(9) . . ?
F4A_b P1 F3A_b 91.1(11) . . ?
F6A_b P1 F3A_b 87.0(11) . . ?
F1A_b P1 F3A_b 176.5(12) . . ?
F2A_b P1 F3A_b 89.9(11) . . ?
F4A_b P1 F5A_b 175.9(11) . . ?
F6A_b P1 F5A_b 86.8(11) . . ?
F1A_b P1 F5A_b 89.8(11) . . ?
F2A_b P1 F5A_b 88.4(10) . . ?
F3A_b P1 F5A_b 86.9(10) . . ?
F11 P2 F12 91.07(9) . . ?
F11 P2 F10 90.74(9) . . ?
F12 P2 F10 178.16(9) . . ?
F11 P2 F7 89.77(8) . . ?
F12 P2 F7 89.98(8) . . ?
F10 P2 F7 90.38(7) . . ?
F11 P2 F8 89.78(9) . . ?
F12 P2 F8 89.90(8) . . ?
F10 P2 F8 89.75(8) . . ?
F7 P2 F8 179.54(9) . . ?
F11 P2 F9 179.34(10) . . ?
F12 P2 F9 89.60(9) . . ?
F10 P2 F9 88.60(8) . . ?
F7 P2 F9 90.25(9) . . ?
F8 P2 F9 90.20(10) . . ?
N9 C23 C24 178.9(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N10 C25 C26 178.8(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
C2 N2 C1 N1 0.81(19) . . . . ?
C9 N2 C1 N1 169.70(15) . . . . ?
C2 N2 C1 Fe1 -164.83(17) . . . 3_656 ?
C9 N2 C1 Fe1 4.1(3) . . . 3_656 ?
C3 N1 C1 N2 -0.61(19) . . . . ?
C4 N1 C1 N2 -174.16(15) . . . . ?
C3 N1 C1 Fe1 170.10(12) . . . 3_656 ?
C4 N1 C1 Fe1 -3.4(2) . . . 3_656 ?
C1 N2 C2 C3 -0.7(2) . . . . ?
C9 N2 C2 C3 -169.81(16) . . . . ?
N2 C2 C3 N1 0.3(2) . . . . ?
C1 N1 C3 C2 0.2(2) . . . . ?
C4 N1 C3 C2 172.88(18) . . . . ?
C8 N3 C4 C5 1.0(3) . . . . ?
Fe1 N3 C4 C5 -179.54(16) 3_656 . . . ?
C8 N3 C4 N1 -179.46(16) . . . . ?
Fe1 N3 C4 N1 0.0(2) 3_656 . . . ?
C1 N1 C4 N3 2.3(2) . . . . ?
C3 N1 C4 N3 -170.07(17) . . . . ?
C1 N1 C4 C5 -178.19(18) . . . . ?
C3 N1 C4 C5 9.5(3) . . . . ?
N3 C4 C5 C6 -0.6(3) . . . . ?
N1 C4 C5 C6 179.90(19) . . . . ?
C4 C5 C6 C7 -0.2(3) . . . . ?
C5 C6 C7 C8 0.6(3) . . . . ?
C4 N3 C8 C7 -0.6(3) . . . . ?
Fe1 N3 C8 C7 -179.97(15) 3_656 . . . ?
C6 C7 C8 N3 -0.2(3) . . . . ?
C10 N4 C9 N2 -74.6(2) . . . . ?
C11 N4 C9 N2 95.77(19) . . . . ?
C10 N4 C9 C18 163.06(16) . . . . ?
C11 N4 C9 C18 -26.5(2) . . . . ?
C1 N2 C9 N4 165.01(15) . . . . ?
C2 N2 C9 N4 -27.4(2) . . . . ?
C1 N2 C9 C18 -71.4(2) . . . . ?
C2 N2 C9 C18 96.24(19) . . . . ?
C11 N4 C10 N5 -0.34(19) . . . . ?
C9 N4 C10 N5 171.24(15) . . . . ?
C11 N4 C10 Fe1 179.48(17) . . . . ?
C9 N4 C10 Fe1 -8.9(3) . . . . ?
C12 N5 C10 N4 0.31(19) . . . . ?
C13 N5 C10 N4 -174.10(14) . . . . ?
C12 N5 C10 Fe1 -179.57(12) . . . . ?
C13 N5 C10 Fe1 6.0(2) . . . . ?
C10 N4 C11 C12 0.2(2) . . . . ?
C9 N4 C11 C12 -171.21(17) . . . . ?
N4 C11 C12 N5 0.0(2) . . . . ?
C10 N5 C12 C11 -0.2(2) . . . . ?
C13 N5 C12 C11 173.42(18) . . . . ?
C17 N6 C13 C14 -1.1(3) . . . . ?
Fe1 N6 C13 C14 173.77(14) . . . . ?
C17 N6 C13 N5 179.36(15) . . . . ?
Fe1 N6 C13 N5 -5.72(18) . . . . ?
C10 N5 C13 N6 0.0(2) . . . . ?
C12 N5 C13 N6 -173.29(17) . . . . ?
C10 N5 C13 C14 -179.54(17) . . . . ?
C12 N5 C13 C14 7.2(3) . . . . ?
N6 C13 C14 C15 0.4(3) . . . . ?
N5 C13 C14 C15 179.86(17) . . . . ?
C13 C14 C15 C16 0.4(3) . . . . ?
C14 C15 C16 C17 -0.4(3) . . . . ?
C13 N6 C17 C16 1.1(3) . . . . ?
Fe1 N6 C17 C16 -173.09(14) . . . . ?
C15 C16 C17 N6 -0.3(3) . . . . ?
N4 C9 C18 O1 74.22(18) . . . . ?
N2 C9 C18 O1 -46.79(19) . . . . ?

_shelxl_version_number           2014-1

