# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

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

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1468980'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2015-07-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            2a
_chemical_name_systematic        2a
_chemical_formula_moiety         'C30 H38 Fe N6 O4, 2(B F4)'
_chemical_formula_sum            'C30 H38 B2 F8 Fe N6 O4'
_chemical_formula_weight         776.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c70 h100 fe1 b1 f4 n6 o6 '
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'
B B 0.0013 0.0007 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.6828(4)
_cell_length_b                   19.9361(6)
_cell_length_c                   25.5286(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6963.7(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16562
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.3000
_cell_measurement_theta_min      3.5000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            76606
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         2.990
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -60.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628  -38.0000  -30.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega  -51.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628    0.0000 -180.0000 130

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega  -20.00   18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000  -30.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega -103.00  -71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega -103.00  -71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  178.0000  120.0000 32

#__ type_ start__ end____ width___ exp.time_
  8 omega  -95.00  -62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566 -178.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
  9 omega  -20.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000 -120.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0011298000
_diffrn_orient_matrix_UB_12      0.0355657000
_diffrn_orient_matrix_UB_13      0.0009430000
_diffrn_orient_matrix_UB_21      -0.0086222000
_diffrn_orient_matrix_UB_22      -0.0013181000
_diffrn_orient_matrix_UB_23      0.0273743000
_diffrn_orient_matrix_UB_31      0.0510883000
_diffrn_orient_matrix_UB_32      0.0005740000
_diffrn_orient_matrix_UB_33      0.0046380000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6564
_reflns_number_total             9640
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0552P)²+7.8990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1486
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.59991(2) 0.68883(2) 0.37764(2) 0.02923(10) Uani 1 1 d . . . . .
O1 O 0.69276(15) 0.70464(11) 0.53686(7) 0.0493(5) Uani 1 1 d . . . . .
O2 O 0.71771(17) 0.52055(10) 0.30083(9) 0.0564(5) Uani 1 1 d . . . . .
O3 O 0.66990(13) 0.87994(8) 0.31978(8) 0.0424(4) Uani 1 1 d . . . . .
O4 O 0.29547(14) 0.65156(12) 0.38650(9) 0.0573(6) Uani 1 1 d . . . . .
N1 N 0.61561(14) 0.72507(10) 0.46063(8) 0.0323(4) Uani 1 1 d . . . . .
N2 N 0.69896(14) 0.62308(10) 0.41358(9) 0.0353(4) Uani 1 1 d . . . . .
N3 N 0.63370(17) 0.61497(10) 0.31712(8) 0.0390(5) Uani 1 1 d . . . . .
N4 N 0.68308(14) 0.77212(9) 0.34449(8) 0.0318(4) Uani 1 1 d . . . . .
N5 N 0.49360(13) 0.75771(10) 0.35352(7) 0.0296(4) Uani 1 1 d . . . . .
N6 N 0.45799(15) 0.64073(10) 0.39617(8) 0.0351(4) Uani 1 1 d . . . . .
C1 C 0.4734(2) 0.78827(19) 0.49523(14) 0.0598(8) Uani 1 1 d . . . . .
H1A H 0.4526 0.8036 0.4605 0.090 Uiso 1 1 calc GR . . . .
H1B H 0.4537 0.8212 0.5217 0.090 Uiso 1 1 calc GR . . . .
H1C H 0.4427 0.7450 0.5030 0.090 Uiso 1 1 calc GR . . . .
C2 C 0.6331(3) 0.84486(15) 0.47937(13) 0.0598(8) Uani 1 1 d . . . . .
H2A H 0.7041 0.8392 0.4814 0.090 Uiso 1 1 calc GR . . . .
H2B H 0.6129 0.8814 0.5026 0.090 Uiso 1 1 calc GR . . . .
H2C H 0.6143 0.8556 0.4433 0.090 Uiso 1 1 calc GR . . . .
C3 C 0.58344(18) 0.78046(13) 0.49607(10) 0.0377(5) Uani 1 1 d . . . . .
C4 C 0.6203(2) 0.75622(17) 0.54934(11) 0.0543(8) Uani 1 1 d . . . . .
H4A H 0.6505 0.7935 0.5692 0.065 Uiso 1 1 calc R . . . .
H4B H 0.5661 0.7372 0.5703 0.065 Uiso 1 1 calc R . . . .
C5 C 0.67486(17) 0.68911(12) 0.48710(10) 0.0355(5) Uani 1 1 d . . . . .
C6 C 0.72374(18) 0.63018(13) 0.46401(10) 0.0382(5) Uani 1 1 d . . . . .
C7 C 0.7850(2) 0.58558(14) 0.48919(13) 0.0481(7) Uani 1 1 d . . . . .
H7 H 0.8006 0.5908 0.5252 0.058 Uiso 1 1 calc R . . . .
C8 C 0.8232(2) 0.53278(15) 0.46017(14) 0.0556(8) Uani 1 1 d . . . . .
H8 H 0.8671 0.5021 0.4761 0.067 Uiso 1 1 calc R . . . .
C9 C 0.7974(2) 0.52484(14) 0.40836(14) 0.0534(7) Uani 1 1 d . . . . .
H9 H 0.8223 0.4885 0.3883 0.064 Uiso 1 1 calc R . . . .
C10 C 0.73434(19) 0.57109(12) 0.38618(11) 0.0410(6) Uani 1 1 d . . . . .
C11 C 0.6937(2) 0.57034(12) 0.33284(11) 0.0428(6) Uani 1 1 d . . . . .
C12 C 0.6546(3) 0.52861(16) 0.25504(13) 0.0640(9) Uani 1 1 d . . . . .
H12A H 0.6048 0.4926 0.2537 0.077 Uiso 1 1 calc R . . . .
H12B H 0.6934 0.5274 0.2223 0.077 Uiso 1 1 calc R . . . .
C13 C 0.6059(2) 0.59785(13) 0.26223(11) 0.0473(7) Uani 1 1 d . . . . .
C14 C 0.4958(3) 0.5945(2) 0.25742(14) 0.0709(10) Uani 1 1 d . . . . .
H14A H 0.4702 0.5613 0.2822 0.106 Uiso 1 1 calc GR . . . .
H14B H 0.4781 0.5813 0.2217 0.106 Uiso 1 1 calc GR . . . .
H14C H 0.4678 0.6386 0.2653 0.106 Uiso 1 1 calc GR . . . .
C15 C 0.6480(3) 0.64968(16) 0.22518(13) 0.0742(11) Uani 1 1 d . . . . .
H15A H 0.6208 0.6939 0.2335 0.111 Uiso 1 1 calc GR . . . .
H15B H 0.6313 0.6378 0.1890 0.111 Uiso 1 1 calc GR . . . .
H15C H 0.7193 0.6509 0.2290 0.111 Uiso 1 1 calc GR . . . .
C16 C 0.8383(3) 0.7944(3) 0.38895(15) 0.0847(14) Uani 1 1 d . . . . .
H16A H 0.8048 0.8249 0.4131 0.127 Uiso 1 1 calc GR . . . .
H16B H 0.9059 0.8093 0.3841 0.127 Uiso 1 1 calc GR . . . .
H16C H 0.8379 0.7489 0.4036 0.127 Uiso 1 1 calc GR . . . .
C17 C 0.8373(2) 0.74929(16) 0.29805(16) 0.0677(10) Uani 1 1 d . . . . .
H17A H 0.8399 0.7035 0.3119 0.102 Uiso 1 1 calc GR . . . .
H17B H 0.9038 0.7656 0.2920 0.102 Uiso 1 1 calc GR . . . .
H17C H 0.8010 0.7494 0.2650 0.102 Uiso 1 1 calc GR . . . .
C18 C 0.78654(17) 0.79442(13) 0.33701(11) 0.0387(6) Uani 1 1 d . . . . .
C19 C 0.7735(2) 0.86552(14) 0.31476(15) 0.0547(8) Uani 1 1 d . . . . .
H19A H 0.8127 0.8983 0.3349 0.066 Uiso 1 1 calc R . . . .
H19B H 0.7939 0.8672 0.2776 0.066 Uiso 1 1 calc R . . . .
C20 C 0.62884(17) 0.82230(11) 0.33326(9) 0.0308(5) Uani 1 1 d . . . . .
C21 C 0.52149(17) 0.81768(11) 0.33630(9) 0.0307(5) Uani 1 1 d . . . . .
C22 C 0.45454(19) 0.86746(13) 0.32429(10) 0.0400(6) Uani 1 1 d . . . . .
H22 H 0.4753 0.9100 0.3117 0.048 Uiso 1 1 calc R . . . .
C23 C 0.35643(19) 0.85309(15) 0.33117(11) 0.0444(6) Uani 1 1 d . . . . .
H23 H 0.3088 0.8865 0.3238 0.053 Uiso 1 1 calc R . . . .
C24 C 0.32693(18) 0.79068(15) 0.34874(10) 0.0415(6) Uani 1 1 d . . . . .
H24 H 0.2596 0.7803 0.3530 0.050 Uiso 1 1 calc R . . . .
C25 C 0.39853(16) 0.74402(13) 0.35987(9) 0.0338(5) Uani 1 1 d . . . . .
C26 C 0.38565(17) 0.67615(14) 0.38137(10) 0.0371(5) Uani 1 1 d . . . . .
C27 C 0.3112(2) 0.58095(18) 0.40088(15) 0.0652(9) Uani 1 1 d . . . . .
H27A H 0.3029 0.5513 0.3701 0.078 Uiso 1 1 calc R . . . .
H27B H 0.2649 0.5669 0.4286 0.078 Uiso 1 1 calc R . . . .
C28 C 0.4163(2) 0.57877(14) 0.42081(11) 0.0454(6) Uani 1 1 d . . . . .
C29 C 0.4211(2) 0.58725(17) 0.47977(12) 0.0573(8) Uani 1 1 d . . . . .
H29A H 0.4893 0.5930 0.4906 0.086 Uiso 1 1 calc GR . . . .
H29B H 0.3939 0.5474 0.4968 0.086 Uiso 1 1 calc GR . . . .
H29C H 0.3833 0.6268 0.4901 0.086 Uiso 1 1 calc GR . . . .
C30 C 0.4717(3) 0.51659(15) 0.40358(15) 0.0644(9) Uani 1 1 d . . . . .
H30A H 0.4708 0.5136 0.3653 0.097 Uiso 1 1 calc GR . . . .
H30B H 0.4405 0.4767 0.4185 0.097 Uiso 1 1 calc GR . . . .
H30C H 0.5394 0.5193 0.4159 0.097 Uiso 1 1 calc GR . . . .
F1 F 0.64722(13) 0.57274(10) 0.69421(9) 0.0707(6) Uani 1 1 d . . . . .
F2 F 0.60948(17) 0.67884(10) 0.71696(10) 0.0800(6) Uani 1 1 d . . . . .
F3 F 0.49050(12) 0.60391(10) 0.70025(9) 0.0684(5) Uani 1 1 d . . . . .
F4 F 0.58332(18) 0.64266(12) 0.63496(9) 0.0821(7) Uani 1 1 d . . . . .
B1 B 0.5826(2) 0.62445(16) 0.68654(14) 0.0452(7) Uani 1 1 d . . . . .
F5 F 0.0050(2) 0.46035(18) 0.41676(18) 0.1561(16) Uani 1 1 d . . . . .
F6A F 0.0078(4) 0.51815(18) 0.35503(14) 0.101(2) Uani 0.615(6) 1 d . . P A 1
F7A F 0.1533(3) 0.4826(3) 0.3875(2) 0.112(3) Uani 0.615(6) 1 d . . P A 1
F8A F 0.0661(4) 0.5614(3) 0.4287(2) 0.120(3) Uani 0.615(6) 1 d . . P A 1
F6B F 0.1125(5) 0.5195(3) 0.35382(19) 0.0574(17) Uani 0.385(6) 1 d . . P A 2
F7B F 0.1122(7) 0.5103(4) 0.4397(2) 0.108(3) Uani 0.385(6) 1 d . . P A 2
F8B F 0.0216(8) 0.5890(3) 0.4029(3) 0.105(3) Uani 0.385(6) 1 d . . P A 2
B2 B 0.0597(3) 0.5139(3) 0.39795(16) 0.0692(12) 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 N1 2.249(2) . ?
Fe1 N2 2.097(2) . ?
Fe1 N3 2.184(2) . ?
Fe1 N4 2.1838(19) . ?
Fe1 N5 2.0930(19) . ?
Fe1 N6 2.217(2) . ?
O1 C4 1.464(4) . ?
O1 C5 1.330(3) . ?
O2 C11 1.327(3) . ?
O2 C12 1.462(4) . ?
O3 C19 1.452(3) . ?
O3 C20 1.325(3) . ?
O4 C26 1.334(3) . ?
O4 C27 1.471(4) . ?
N1 C3 1.494(3) . ?
N1 C5 1.276(3) . ?
N2 C6 1.339(3) . ?
N2 C10 1.341(3) . ?
N3 C11 1.275(3) . ?
N3 C13 1.492(4) . ?
N4 C18 1.496(3) . ?
N4 C20 1.278(3) . ?
N5 C21 1.330(3) . ?
N5 C25 1.339(3) . ?
N6 C26 1.273(3) . ?
N6 C28 1.499(3) . ?
C1 C3 1.514(4) . ?
C2 C3 1.514(4) . ?
C3 C4 1.529(4) . ?
C5 C6 1.475(4) . ?
C6 C7 1.381(4) . ?
C7 C8 1.389(4) . ?
C8 C9 1.378(5) . ?
C9 C10 1.384(4) . ?
C10 C11 1.471(4) . ?
C12 C13 1.544(4) . ?
C13 C14 1.512(5) . ?
C13 C15 1.515(4) . ?
C16 C18 1.503(4) . ?
C17 C18 1.510(4) . ?
C18 C19 1.538(4) . ?
C20 C21 1.474(3) . ?
C21 C22 1.385(3) . ?
C22 C23 1.384(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.381(3) . ?
C25 C26 1.471(4) . ?
C27 C28 1.526(4) . ?
C28 C29 1.516(4) . ?
C28 C30 1.518(5) . ?
F1 B1 1.373(4) . ?
F2 B1 1.384(4) . ?
F3 B1 1.370(3) . ?
F4 B1 1.366(4) . ?
F5 B2 1.389(5) . ?
F6A B2 1.309(5) . ?
F7A B2 1.449(6) . ?
F8A B2 1.233(6) . ?
F6B B2 1.343(6) . ?
F7B B2 1.287(8) . ?
F8B B2 1.592(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 74.15(8) . . ?
N2 Fe1 N3 75.59(8) . . ?
N2 Fe1 N4 107.94(8) . . ?
N2 Fe1 N6 101.68(8) . . ?
N3 Fe1 N1 149.65(8) . . ?
N3 Fe1 N6 92.57(8) . . ?
N4 Fe1 N1 94.07(7) . . ?
N4 Fe1 N3 97.36(8) . . ?
N4 Fe1 N6 150.24(8) . . ?
N5 Fe1 N1 97.63(7) . . ?
N5 Fe1 N2 171.14(8) . . ?
N5 Fe1 N3 112.42(8) . . ?
N5 Fe1 N4 75.48(7) . . ?
N5 Fe1 N6 74.80(8) . . ?
N6 Fe1 N1 91.24(7) . . ?
C5 O1 C4 104.3(2) . . ?
C11 O2 C12 105.3(2) . . ?
C20 O3 C19 105.37(19) . . ?
C26 O4 C27 103.9(2) . . ?
C3 N1 Fe1 141.26(16) . . ?
C5 N1 Fe1 112.29(17) . . ?
C5 N1 C3 106.4(2) . . ?
C6 N2 Fe1 121.22(16) . . ?
C6 N2 C10 119.5(2) . . ?
C10 N2 Fe1 119.24(18) . . ?
C11 N3 Fe1 112.59(19) . . ?
C11 N3 C13 107.5(2) . . ?
C13 N3 Fe1 139.89(17) . . ?
C18 N4 Fe1 140.22(15) . . ?
C20 N4 Fe1 112.29(15) . . ?
C20 N4 C18 106.76(19) . . ?
C21 N5 Fe1 119.19(15) . . ?
C21 N5 C25 120.1(2) . . ?
C25 N5 Fe1 120.39(16) . . ?
C26 N6 Fe1 112.20(16) . . ?
C26 N6 C28 106.6(2) . . ?
C28 N6 Fe1 141.18(17) . . ?
N1 C3 C1 111.1(2) . . ?
N1 C3 C2 108.9(2) . . ?
N1 C3 C4 102.0(2) . . ?
C1 C3 C4 111.9(2) . . ?
C2 C3 C1 110.8(3) . . ?
C2 C3 C4 111.8(3) . . ?
O1 C4 C3 104.6(2) . . ?
O1 C5 C6 118.9(2) . . ?
N1 C5 O1 119.5(2) . . ?
N1 C5 C6 121.6(2) . . ?
N2 C6 C5 110.7(2) . . ?
N2 C6 C7 122.2(3) . . ?
C7 C6 C5 127.0(3) . . ?
C6 C7 C8 117.9(3) . . ?
C9 C8 C7 120.2(3) . . ?
C8 C9 C10 118.4(3) . . ?
N2 C10 C9 121.8(3) . . ?
N2 C10 C11 110.7(2) . . ?
C9 C10 C11 127.4(3) . . ?
O2 C11 C10 119.0(2) . . ?
N3 C11 O2 119.2(3) . . ?
N3 C11 C10 121.8(2) . . ?
O2 C12 C13 105.0(2) . . ?
N3 C13 C12 101.9(2) . . ?
N3 C13 C14 109.9(2) . . ?
N3 C13 C15 109.5(2) . . ?
C14 C13 C12 112.4(3) . . ?
C14 C13 C15 111.0(3) . . ?
C15 C13 C12 111.8(3) . . ?
N4 C18 C16 109.5(2) . . ?
N4 C18 C17 110.0(2) . . ?
N4 C18 C19 102.18(19) . . ?
C16 C18 C17 111.4(3) . . ?
C16 C18 C19 112.4(3) . . ?
C17 C18 C19 111.1(2) . . ?
O3 C19 C18 105.3(2) . . ?
O3 C20 C21 119.4(2) . . ?
N4 C20 O3 119.4(2) . . ?
N4 C20 C21 121.2(2) . . ?
N5 C21 C20 111.07(19) . . ?
N5 C21 C22 121.8(2) . . ?
C22 C21 C20 127.1(2) . . ?
C23 C22 C21 117.7(2) . . ?
C24 C23 C22 120.7(2) . . ?
C25 C24 C23 117.8(2) . . ?
N5 C25 C24 121.8(2) . . ?
N5 C25 C26 110.4(2) . . ?
C24 C25 C26 127.7(2) . . ?
O4 C26 C25 119.0(2) . . ?
N6 C26 O4 119.1(2) . . ?
N6 C26 C25 121.9(2) . . ?
O4 C27 C28 104.4(2) . . ?
N6 C28 C27 101.2(2) . . ?
N6 C28 C29 108.0(2) . . ?
N6 C28 C30 111.2(2) . . ?
C29 C28 C27 111.6(3) . . ?
C29 C28 C30 110.9(3) . . ?
C30 C28 C27 113.4(3) . . ?
F1 B1 F2 109.7(3) . . ?
F3 B1 F1 109.4(3) . . ?
F3 B1 F2 109.6(3) . . ?
F4 B1 F1 109.4(3) . . ?
F4 B1 F2 109.3(3) . . ?
F4 B1 F3 109.4(3) . . ?
F5 B2 F7A 102.1(4) . . ?
F5 B2 F8B 121.3(5) . . ?
F6A B2 F5 92.7(4) . . ?
F6A B2 F7A 110.7(4) . . ?
F8A B2 F5 114.1(5) . . ?
F8A B2 F6A 121.4(6) . . ?
F8A B2 F7A 112.6(4) . . ?
F6B B2 F5 130.1(4) . . ?
F6B B2 F8B 99.5(5) . . ?
F7B B2 F5 88.4(5) . . ?
F7B B2 F6B 113.5(5) . . ?
F7B B2 F8B 99.7(6) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method methanol
_chemical_compound_source        no
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1468981'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            2b
_chemical_name_systematic        2b
_chemical_formula_moiety         'C30 H38 Fe N6 O4, C2 H3 N, 2(B F4)'
_chemical_formula_sum            'C32 H41 B2 F8 Fe N7 O4'
_chemical_formula_weight         817.19
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.918(3)
_cell_length_b                   18.982(4)
_cell_length_c                   23.007(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7388(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    26358
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      29.1051
_cell_measurement_theta_min      2.3949
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.5300
_exptl_crystal_size_mid          0.4500
_exptl_crystal_size_min          0.3700
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.087
_diffrn_reflns_theta_min         2.636
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0658
	          2theta: -20.2082
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0658
	          2theta: -20.2082
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             10728
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0220
_diffrn_orient_matrix_UB_12      -0.0202
_diffrn_orient_matrix_UB_13      -0.0510
_diffrn_orient_matrix_UB_21      0.0425
_diffrn_orient_matrix_UB_22      -0.0304
_diffrn_orient_matrix_UB_23      -0.0063
_diffrn_orient_matrix_UB_31      -0.0199
_diffrn_orient_matrix_UB_32      -0.0322
_diffrn_orient_matrix_UB_33      0.0214
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9537
_reflns_number_total             9874
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9874
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0663
_refine_ls_restrained_S_all      1.264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²+8.2502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1365
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.27432(2) 0.21453(2) 0.38425(2) 0.02035(9) Uani 1 1 d . . . . .
O1 O 0.16552(10) 0.38134(9) 0.48272(7) 0.0275(4) Uani 1 1 d . . . . .
O2 O 0.20650(11) 0.22035(9) 0.20653(7) 0.0304(4) Uani 1 1 d . . . . .
O3 O 0.17475(11) 0.03261(9) 0.46392(9) 0.0349(4) Uani 1 1 d . . . . .
O4 O 0.51913(10) 0.23845(11) 0.42163(8) 0.0374(4) Uani 1 1 d . . . . .
N1 N 0.24247(11) 0.28791(10) 0.45880(8) 0.0219(4) Uani 1 1 d . . . . .
N2 N 0.20288(11) 0.29539(10) 0.34804(8) 0.0215(4) Uani 1 1 d . . . . .
N3 N 0.26371(11) 0.18821(11) 0.29109(8) 0.0237(4) Uani 1 1 d . . . . .
N4 N 0.18711(11) 0.13515(10) 0.41453(8) 0.0233(4) Uani 1 1 d . . . . .
N5 N 0.34021(10) 0.14184(10) 0.43441(8) 0.0207(4) Uani 1 1 d . . . . .
N6 N 0.39844(11) 0.25269(11) 0.38104(8) 0.0255(4) Uani 1 1 d . . . . .
C1 C 0.33920(15) 0.31818(18) 0.53462(12) 0.0421(7) Uani 1 1 d . . . . .
H1A H 0.3750 0.2815 0.5203 0.063 Uiso 1 1 calc GR . . . .
H1B H 0.3472 0.3246 0.5765 0.063 Uiso 1 1 calc GR . . . .
H1C H 0.3502 0.3625 0.5144 0.063 Uiso 1 1 calc GR . . . .
C2 C 0.23388(19) 0.22762(14) 0.55421(11) 0.0374(6) Uani 1 1 d . . . . .
H2A H 0.1819 0.2111 0.5413 0.056 Uiso 1 1 calc GR . . . .
H2B H 0.2329 0.2356 0.5963 0.056 Uiso 1 1 calc GR . . . .
H2C H 0.2739 0.1920 0.5450 0.056 Uiso 1 1 calc GR . . . .
C3 C 0.25404(14) 0.29621(12) 0.52325(9) 0.0232(4) Uani 1 1 d . . . . .
C4 C 0.19509(16) 0.35521(14) 0.53893(10) 0.0299(5) Uani 1 1 d . . . . .
H4A H 0.1512 0.3365 0.5628 0.036 Uiso 1 1 calc R . . . .
H4B H 0.2218 0.3933 0.5608 0.036 Uiso 1 1 calc R . . . .
C5 C 0.19541(13) 0.33731(12) 0.44287(10) 0.0218(4) Uani 1 1 d . . . . .
C6 C 0.17306(13) 0.34701(12) 0.38140(10) 0.0224(4) Uani 1 1 d . . . . .
C7 C 0.12744(14) 0.40104(13) 0.35888(10) 0.0265(5) Uani 1 1 d . . . . .
H7 H 0.1065 0.4367 0.3834 0.032 Uiso 1 1 calc R . . . .
C8 C 0.11298(14) 0.40162(13) 0.29906(11) 0.0276(5) Uani 1 1 d . . . . .
H8 H 0.0825 0.4384 0.2822 0.033 Uiso 1 1 calc R . . . .
C9 C 0.14338(13) 0.34813(13) 0.26448(10) 0.0257(5) Uani 1 1 d . . . . .
H9 H 0.1343 0.3477 0.2237 0.031 Uiso 1 1 calc R . . . .
C10 C 0.18746(13) 0.29519(12) 0.29090(9) 0.0219(4) Uani 1 1 d . . . . .
C11 C 0.22182(13) 0.23229(12) 0.26263(9) 0.0225(4) Uani 1 1 d . . . . .
C12 C 0.23493(17) 0.14790(15) 0.19666(12) 0.0354(6) Uani 1 1 d . . . . .
H12A H 0.2643 0.1446 0.1595 0.042 Uiso 1 1 calc R . . . .
H12B H 0.1902 0.1143 0.1957 0.042 Uiso 1 1 calc R . . . .
C13 C 0.28970(14) 0.13249(13) 0.24856(10) 0.0269(5) Uani 1 1 d . . . . .
C14 C 0.37560(16) 0.14500(17) 0.23253(14) 0.0427(7) Uani 1 1 d . . . . .
H14A H 0.3810 0.1914 0.2143 0.064 Uiso 1 1 calc GR . . . .
H14B H 0.3931 0.1085 0.2053 0.064 Uiso 1 1 calc GR . . . .
H14C H 0.4082 0.1432 0.2677 0.064 Uiso 1 1 calc GR . . . .
C15 C 0.2776(2) 0.05951(15) 0.27357(13) 0.0419(7) Uani 1 1 d . . . . .
H15A H 0.3099 0.0541 0.3087 0.063 Uiso 1 1 calc GR . . . .
H15B H 0.2934 0.0241 0.2448 0.063 Uiso 1 1 calc GR . . . .
H15C H 0.2218 0.0530 0.2835 0.063 Uiso 1 1 calc GR . . . .
C16 C 0.05232(19) 0.1796(2) 0.4303(2) 0.0721(13) Uani 1 1 d . . . . .
H16A H 0.0671 0.1917 0.4702 0.108 Uiso 1 1 calc GR . . . .
H16B H -0.0039 0.1673 0.4289 0.108 Uiso 1 1 calc GR . . . .
H16C H 0.0622 0.2200 0.4048 0.108 Uiso 1 1 calc GR . . . .
C17 C 0.0805(2) 0.0968(3) 0.34802(14) 0.0699(13) Uani 1 1 d . . . . .
H17A H 0.0901 0.1368 0.3220 0.105 Uiso 1 1 calc GR . . . .
H17B H 0.0246 0.0833 0.3459 0.105 Uiso 1 1 calc GR . . . .
H17C H 0.1135 0.0569 0.3361 0.105 Uiso 1 1 calc GR . . . .
C18 C 0.10092(13) 0.11764(14) 0.41006(11) 0.0300(5) Uani 1 1 d . . . . .
C19 C 0.09315(17) 0.05465(18) 0.45163(15) 0.0464(7) Uani 1 1 d . . . . .
H19A H 0.0658 0.0687 0.4879 0.056 Uiso 1 1 calc R . . . .
H19B H 0.0631 0.0159 0.4331 0.056 Uiso 1 1 calc R . . . .
C20 C 0.21914(13) 0.08604(12) 0.44478(10) 0.0236(4) Uani 1 1 d . . . . .
C21 C 0.30346(13) 0.08848(12) 0.46100(10) 0.0232(4) Uani 1 1 d . . . . .
C22 C 0.34105(15) 0.04685(13) 0.50228(11) 0.0286(5) Uani 1 1 d . . . . .
H22 H 0.3137 0.0096 0.5212 0.034 Uiso 1 1 calc R . . . .
C23 C 0.41959(15) 0.06108(14) 0.51508(11) 0.0325(5) Uani 1 1 d . . . . .
H23 H 0.4469 0.0332 0.5429 0.039 Uiso 1 1 calc R . . . .
C24 C 0.45837(14) 0.11622(14) 0.48713(11) 0.0304(5) Uani 1 1 d . . . . .
H24 H 0.5122 0.1266 0.4953 0.037 Uiso 1 1 calc R . . . .
C25 C 0.41603(13) 0.15560(13) 0.44697(10) 0.0238(4) Uani 1 1 d . . . . .
C26 C 0.44418(13) 0.21749(13) 0.41460(10) 0.0265(5) Uani 1 1 d . . . . .
C27 C 0.53112(18) 0.29175(19) 0.37684(15) 0.0514(9) Uani 1 1 d . . . . .
H27A H 0.5613 0.2722 0.3437 0.062 Uiso 1 1 calc R . . . .
H27B H 0.5600 0.3329 0.3926 0.062 Uiso 1 1 calc R . . . .
C28 C 0.44625(15) 0.31294(14) 0.35782(11) 0.0313(5) Uani 1 1 d . . . . .
C29 C 0.4192(3) 0.37975(18) 0.3861(2) 0.0720(13) Uani 1 1 d . . . . .
H29A H 0.3646 0.3897 0.3744 0.108 Uiso 1 1 calc GR . . . .
H29B H 0.4534 0.4187 0.3738 0.108 Uiso 1 1 calc GR . . . .
H29C H 0.4218 0.3746 0.4284 0.108 Uiso 1 1 calc GR . . . .
C30 C 0.4404(2) 0.3158(2) 0.29249(13) 0.0536(9) Uani 1 1 d . . . . .
H30A H 0.4627 0.2727 0.2759 0.080 Uiso 1 1 calc GR . . . .
H30B H 0.4698 0.3567 0.2781 0.080 Uiso 1 1 calc GR . . . .
H30C H 0.3847 0.3200 0.2811 0.080 Uiso 1 1 calc GR . . . .
N7 N 0.4404(2) 0.1794(2) 0.63443(16) 0.0751(10) Uani 1 1 d . . . . .
C31 C 0.3899(2) 0.14424(19) 0.64939(14) 0.0473(7) Uani 1 1 d . . . . .
C32 C 0.32606(19) 0.09933(18) 0.66763(16) 0.0512(8) Uani 1 1 d . . . . .
H32A H 0.3151 0.0646 0.6372 0.077 Uiso 1 1 calc GR . . . .
H32B H 0.2787 0.1279 0.6746 0.077 Uiso 1 1 calc GR . . . .
H32C H 0.3409 0.0750 0.7036 0.077 Uiso 1 1 calc GR . . . .
F1 F 0.45839(11) 0.04484(11) 0.35893(10) 0.0595(6) Uani 1 1 d . . . . .
F2 F 0.54905(12) 0.02151(11) 0.28974(8) 0.0568(5) Uani 1 1 d . . . . .
F3 F 0.58897(12) 0.04752(10) 0.38129(8) 0.0514(5) Uani 1 1 d . . . . .
F4 F 0.53590(12) 0.13263(10) 0.32520(11) 0.0635(6) Uani 1 1 d . . . . .
B1 B 0.53324(18) 0.06149(17) 0.33823(14) 0.0337(6) Uani 1 1 d . . . . .
F5 F 0.65940(11) 0.41819(9) 0.41345(9) 0.0507(5) Uani 1 1 d . . . . .
F6 F 0.60396(13) 0.46166(11) 0.33195(8) 0.0605(5) Uani 1 1 d . . . . .
F7 F 0.57748(10) 0.51229(11) 0.41882(8) 0.0512(5) Uani 1 1 d . . . . .
F8 F 0.69856(11) 0.52418(10) 0.37891(9) 0.0545(5) Uani 1 1 d . . . . .
B2 B 0.63472(17) 0.47944(16) 0.38598(13) 0.0299(6) 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 N1 2.2743(19) . ?
Fe1 N2 2.1239(19) . ?
Fe1 N3 2.2080(19) . ?
Fe1 N4 2.2209(19) . ?
Fe1 N5 2.1163(18) . ?
Fe1 N6 2.2226(19) . ?
O1 C4 1.473(3) . ?
O1 C5 1.340(3) . ?
O2 C11 1.336(3) . ?
O2 C12 1.475(3) . ?
O3 C19 1.470(3) . ?
O3 C20 1.336(3) . ?
O4 C26 1.339(3) . ?
O4 C27 1.459(3) . ?
N1 C3 1.504(3) . ?
N1 C5 1.283(3) . ?
N2 C6 1.343(3) . ?
N2 C10 1.340(3) . ?
N3 C11 1.277(3) . ?
N3 C13 1.507(3) . ?
N4 C18 1.499(3) . ?
N4 C20 1.283(3) . ?
N5 C21 1.337(3) . ?
N5 C25 1.340(3) . ?
N6 C26 1.281(3) . ?
N6 C28 1.499(3) . ?
C1 C3 1.522(3) . ?
C2 C3 1.523(3) . ?
C3 C4 1.542(3) . ?
C5 C6 1.476(3) . ?
C6 C7 1.384(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.389(3) . ?
C9 C10 1.391(3) . ?
C10 C11 1.479(3) . ?
C12 C13 1.539(3) . ?
C13 C14 1.518(4) . ?
C13 C15 1.514(4) . ?
C16 C18 1.508(4) . ?
C17 C18 1.521(4) . ?
C18 C19 1.537(4) . ?
C20 C21 1.475(3) . ?
C21 C22 1.390(3) . ?
C22 C23 1.388(4) . ?
C23 C24 1.393(4) . ?
C24 C25 1.388(3) . ?
C25 C26 1.470(3) . ?
C27 C28 1.554(4) . ?
C28 C29 1.497(4) . ?
C28 C30 1.507(4) . ?
N7 C31 1.136(5) . ?
C31 C32 1.439(5) . ?
F1 B1 1.389(3) . ?
F2 B1 1.376(4) . ?
F3 B1 1.393(3) . ?
F4 B1 1.384(4) . ?
F5 B2 1.388(3) . ?
F6 B2 1.389(3) . ?
F7 B2 1.377(3) . ?
F8 B2 1.384(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 73.64(7) . . ?
N2 Fe1 N3 74.72(7) . . ?
N2 Fe1 N4 103.61(7) . . ?
N2 Fe1 N6 106.80(8) . . ?
N3 Fe1 N1 148.36(7) . . ?
N3 Fe1 N4 95.57(7) . . ?
N3 Fe1 N6 96.80(7) . . ?
N4 Fe1 N1 91.24(7) . . ?
N4 Fe1 N6 149.23(7) . . ?
N5 Fe1 N1 96.48(7) . . ?
N5 Fe1 N2 170.03(7) . . ?
N5 Fe1 N3 115.13(7) . . ?
N5 Fe1 N4 74.72(7) . . ?
N5 Fe1 N6 74.51(7) . . ?
N6 Fe1 N1 92.82(7) . . ?
C5 O1 C4 105.22(17) . . ?
C11 O2 C12 104.11(18) . . ?
C20 O3 C19 104.4(2) . . ?
C26 O4 C27 104.63(19) . . ?
C3 N1 Fe1 140.97(14) . . ?
C5 N1 Fe1 112.27(15) . . ?
C5 N1 C3 106.60(18) . . ?
C6 N2 Fe1 121.12(15) . . ?
C10 N2 Fe1 119.56(15) . . ?
C10 N2 C6 119.31(19) . . ?
C11 N3 Fe1 113.24(15) . . ?
C11 N3 C13 106.79(18) . . ?
C13 N3 Fe1 139.96(15) . . ?
C18 N4 Fe1 140.81(16) . . ?
C20 N4 Fe1 112.49(15) . . ?
C20 N4 C18 106.67(19) . . ?
C21 N5 Fe1 119.91(15) . . ?
C21 N5 C25 119.6(2) . . ?
C25 N5 Fe1 119.64(15) . . ?
C26 N6 Fe1 112.37(15) . . ?
C26 N6 C28 106.67(19) . . ?
C28 N6 Fe1 140.38(16) . . ?
N1 C3 C1 108.73(19) . . ?
N1 C3 C2 110.03(19) . . ?
N1 C3 C4 102.85(17) . . ?
C1 C3 C2 111.5(2) . . ?
C1 C3 C4 111.9(2) . . ?
C2 C3 C4 111.5(2) . . ?
O1 C4 C3 105.00(17) . . ?
O1 C5 C6 118.77(19) . . ?
N1 C5 O1 119.6(2) . . ?
N1 C5 C6 121.6(2) . . ?
N2 C6 C5 111.13(19) . . ?
N2 C6 C7 122.4(2) . . ?
C7 C6 C5 126.4(2) . . ?
C6 C7 C8 118.2(2) . . ?
C9 C8 C7 119.6(2) . . ?
C8 C9 C10 118.5(2) . . ?
N2 C10 C9 122.1(2) . . ?
N2 C10 C11 110.93(19) . . ?
C9 C10 C11 127.0(2) . . ?
O2 C11 C10 119.06(19) . . ?
N3 C11 O2 119.5(2) . . ?
N3 C11 C10 121.4(2) . . ?
O2 C12 C13 104.72(19) . . ?
N3 C13 C12 101.24(18) . . ?
N3 C13 C14 109.1(2) . . ?
N3 C13 C15 110.9(2) . . ?
C14 C13 C12 111.0(2) . . ?
C15 C13 C12 112.8(2) . . ?
C15 C13 C14 111.4(2) . . ?
N4 C18 C16 109.7(2) . . ?
N4 C18 C17 110.1(2) . . ?
N4 C18 C19 102.3(2) . . ?
C16 C18 C17 111.6(3) . . ?
C16 C18 C19 111.6(3) . . ?
C17 C18 C19 111.3(3) . . ?
O3 C19 C18 105.1(2) . . ?
O3 C20 C21 118.9(2) . . ?
N4 C20 O3 119.5(2) . . ?
N4 C20 C21 121.5(2) . . ?
N5 C21 C20 110.97(19) . . ?
N5 C21 C22 122.1(2) . . ?
C22 C21 C20 126.7(2) . . ?
C23 C22 C21 118.2(2) . . ?
C22 C23 C24 120.0(2) . . ?
C25 C24 C23 118.0(2) . . ?
N5 C25 C24 122.2(2) . . ?
N5 C25 C26 110.88(19) . . ?
C24 C25 C26 126.9(2) . . ?
O4 C26 C25 118.9(2) . . ?
N6 C26 O4 119.3(2) . . ?
N6 C26 C25 121.8(2) . . ?
O4 C27 C28 104.5(2) . . ?
N6 C28 C27 101.6(2) . . ?
N6 C28 C30 110.3(2) . . ?
C29 C28 N6 109.1(2) . . ?
C29 C28 C27 112.3(3) . . ?
C29 C28 C30 112.4(3) . . ?
C30 C28 C27 110.6(3) . . ?
N7 C31 C32 179.3(4) . . ?
F1 B1 F3 109.2(3) . . ?
F2 B1 F1 109.2(2) . . ?
F2 B1 F3 109.9(2) . . ?
F2 B1 F4 110.9(3) . . ?
F4 B1 F1 109.0(3) . . ?
F4 B1 F3 108.5(2) . . ?
F5 B2 F6 108.5(2) . . ?
F7 B2 F5 109.9(2) . . ?
F7 B2 F6 109.7(2) . . ?
F7 B2 F8 109.6(2) . . ?
F8 B2 F5 109.4(2) . . ?
F8 B2 F6 109.7(2) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1468982'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2015-07-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            3
_chemical_name_systematic        3
_chemical_formula_moiety         
'2(C30 H38 Fe N6 O4), C2 H3 N, C4 H10 O, 4(F6 P)'
_chemical_formula_sum            'C66 H89 F24 Fe2 N13 O9 P4'
_chemical_formula_weight         1900.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1084(19)
_cell_length_b                   16.260(2)
_cell_length_c                   19.256(4)
_cell_angle_alpha                101.206(2)
_cell_angle_beta                 91.086(2)
_cell_angle_gamma                101.768(2)
_cell_volume                     4234.1(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8616
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.71
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0940 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.8636.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.31
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32821
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.389
_diffrn_reflns_theta_min         1.517
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10606
_reflns_number_total             16754
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         16754
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0712
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1307P)²+2.3860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2314
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B), C34(H34A,H34B),
 C42(H42A,H42B), C49(H49A,H49B), C57(H57A,H57B), C64(H64A,H64B), C65(H65A,H65B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C37(H37), C38(H38),
 C39(H39), C52(H52), C53(H53), C54(H54)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C66(H66A,H66B,
 H66C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.35235(4) 0.04668(3) 0.26435(3) 0.03738(17) Uani 1 1 d . . . . .
Fe2 Fe 0.83242(4) 0.53791(3) 0.27177(3) 0.03934(17) Uani 1 1 d . . . . .
C1 C 0.5863(3) 0.0816(2) 0.2043(2) 0.0454(9) Uani 1 1 d . . . . .
C2 C 0.6230(4) 0.1685(3) 0.2517(3) 0.0662(14) Uani 1 1 d . . . . .
H2A H 0.5726 0.2006 0.2554 0.099 Uiso 1 1 calc GR . . . .
H2B H 0.6781 0.1988 0.2320 0.099 Uiso 1 1 calc GR . . . .
H2C H 0.6415 0.1613 0.2981 0.099 Uiso 1 1 calc GR . . . .
C3 C 0.5601(4) 0.0901(4) 0.1303(2) 0.0704(14) Uani 1 1 d . . . . .
H3A H 0.5378 0.0341 0.1012 0.106 Uiso 1 1 calc GR . . . .
H3B H 0.6162 0.1197 0.1110 0.106 Uiso 1 1 calc GR . . . .
H3C H 0.5097 0.1219 0.1316 0.106 Uiso 1 1 calc GR . . . .
C4 C 0.6594(3) 0.0234(3) 0.2050(3) 0.0628(13) Uani 1 1 d . . . . .
H4A H 0.6747 0.0008 0.1572 0.075 Uiso 1 1 calc R . . . .
H4B H 0.7189 0.0549 0.2320 0.075 Uiso 1 1 calc R . . . .
C5 C 0.5233(3) -0.0308(2) 0.2518(2) 0.0397(9) Uani 1 1 d . . . . .
C6 C 0.4564(3) -0.0909(2) 0.2855(2) 0.0423(9) Uani 1 1 d . . . . .
C7 C 0.4751(4) -0.1613(3) 0.3091(3) 0.0612(12) Uani 1 1 d . . . . .
H7 H 0.5351 -0.1763 0.3037 0.073 Uiso 1 1 calc R . . . .
C8 C 0.4024(4) -0.2092(3) 0.3411(3) 0.0658(13) Uani 1 1 d . . . . .
H8 H 0.4133 -0.2569 0.3573 0.079 Uiso 1 1 calc R . . . .
C9 C 0.3146(4) -0.1861(3) 0.3489(2) 0.0607(12) Uani 1 1 d . . . . .
H9 H 0.2653 -0.2177 0.3703 0.073 Uiso 1 1 calc R . . . .
C10 C 0.3008(3) -0.1147(2) 0.3242(2) 0.0453(9) Uani 1 1 d . . . . .
C11 C 0.2133(3) -0.0774(2) 0.3294(2) 0.0446(9) Uani 1 1 d . . . . .
C12 C 0.0629(4) -0.0668(4) 0.3537(4) 0.091(2) Uani 1 1 d . . . . .
H12A H 0.0410 -0.0510 0.4009 0.109 Uiso 1 1 calc R . . . .
H12B H 0.0072 -0.0974 0.3220 0.109 Uiso 1 1 calc R . . . .
C13 C 0.1138(3) 0.0127(3) 0.3278(2) 0.0536(11) Uani 1 1 d . . . . .
C14 C 0.1277(5) 0.0908(4) 0.3864(4) 0.113(3) Uani 1 1 d . . . . .
H14A H 0.1516 0.0778 0.4291 0.170 Uiso 1 1 calc GR . . . .
H14B H 0.0667 0.1077 0.3941 0.170 Uiso 1 1 calc GR . . . .
H14C H 0.1735 0.1368 0.3734 0.170 Uiso 1 1 calc GR . . . .
C15 C 0.0632(4) 0.0249(5) 0.2629(3) 0.103(2) Uani 1 1 d . . . . .
H15A H 0.1031 0.0697 0.2441 0.155 Uiso 1 1 calc GR . . . .
H15B H 0.0026 0.0404 0.2750 0.155 Uiso 1 1 calc GR . . . .
H15C H 0.0514 -0.0275 0.2280 0.155 Uiso 1 1 calc GR . . . .
C16 C 0.2541(3) -0.0561(3) 0.0945(2) 0.0541(11) Uani 1 1 d . . . . .
C17 C 0.3411(4) -0.0839(4) 0.0620(3) 0.0826(17) Uani 1 1 d . . . . .
H17A H 0.3812 -0.0367 0.0462 0.124 Uiso 1 1 calc GR . . . .
H17B H 0.3203 -0.1306 0.0223 0.124 Uiso 1 1 calc GR . . . .
H17C H 0.3774 -0.1021 0.0966 0.124 Uiso 1 1 calc GR . . . .
C18 C 0.1896(5) -0.1288(4) 0.1205(3) 0.097(2) Uani 1 1 d . . . . .
H18A H 0.2209 -0.1396 0.1615 0.146 Uiso 1 1 calc GR . . . .
H18B H 0.1781 -0.1795 0.0837 0.146 Uiso 1 1 calc GR . . . .
H18C H 0.1290 -0.1135 0.1327 0.146 Uiso 1 1 calc GR . . . .
C19 C 0.2019(6) -0.0156(4) 0.0427(3) 0.099(2) Uani 1 1 d . . . . .
H19A H 0.2355 -0.0155 -0.0008 0.119 Uiso 1 1 calc R . . . .
H19B H 0.1356 -0.0473 0.0310 0.119 Uiso 1 1 calc R . . . .
C20 C 0.2540(3) 0.0808(3) 0.1408(2) 0.0479(10) Uani 1 1 d . . . . .
C21 C 0.2675(3) 0.1642(2) 0.1914(2) 0.0456(9) Uani 1 1 d . . . . .
C22 C 0.2320(4) 0.2346(3) 0.1824(3) 0.0650(13) Uani 1 1 d . . . . .
H22 H 0.1997 0.2350 0.1400 0.078 Uiso 1 1 calc R . . . .
C23 C 0.2452(4) 0.3037(3) 0.2372(3) 0.0733(15) Uani 1 1 d . . . . .
H23 H 0.2221 0.3520 0.2322 0.088 Uiso 1 1 calc R . . . .
C24 C 0.2931(4) 0.3025(3) 0.3006(3) 0.0604(12) Uani 1 1 d . . . . .
H24 H 0.3026 0.3491 0.3384 0.072 Uiso 1 1 calc R . . . .
C25 C 0.3263(3) 0.2290(2) 0.3053(2) 0.0449(9) Uani 1 1 d . . . . .
C26 C 0.3738(3) 0.2118(2) 0.3686(2) 0.0438(9) Uani 1 1 d . . . . .
C27 C 0.4184(6) 0.2289(4) 0.4829(3) 0.094(2) Uani 1 1 d . . . . .
H27A H 0.3676 0.2143 0.5143 0.113 Uiso 1 1 calc R . . . .
H27B H 0.4744 0.2660 0.5108 0.113 Uiso 1 1 calc R . . . .
C28 C 0.4452(3) 0.1482(3) 0.4403(2) 0.0510(10) Uani 1 1 d . . . . .
C29 C 0.5541(4) 0.1598(5) 0.4375(3) 0.095(2) Uani 1 1 d . . . . .
H29A H 0.5695 0.1083 0.4109 0.142 Uiso 1 1 calc GR . . . .
H29B H 0.5832 0.1715 0.4848 0.142 Uiso 1 1 calc GR . . . .
H29C H 0.5786 0.2069 0.4150 0.142 Uiso 1 1 calc GR . . . .
C30 C 0.4025(6) 0.0692(4) 0.4686(3) 0.100(2) Uani 1 1 d . . . . .
H30A H 0.3330 0.0597 0.4650 0.150 Uiso 1 1 calc GR . . . .
H30B H 0.4246 0.0772 0.5174 0.150 Uiso 1 1 calc GR . . . .
H30C H 0.4228 0.0204 0.4415 0.150 Uiso 1 1 calc GR . . . .
C31 C 0.7193(4) 0.4115(3) 0.1105(2) 0.0608(12) Uani 1 1 d . . . . .
C32 C 0.6822(5) 0.3369(3) 0.1455(3) 0.0812(17) Uani 1 1 d . . . . .
H32A H 0.7316 0.3320 0.1786 0.122 Uiso 1 1 calc GR . . . .
H32B H 0.6658 0.2850 0.1101 0.122 Uiso 1 1 calc GR . . . .
H32C H 0.6256 0.3461 0.1702 0.122 Uiso 1 1 calc GR . . . .
C33 C 0.8030(5) 0.3951(4) 0.0648(3) 0.0894(19) Uani 1 1 d . . . . .
H33A H 0.8237 0.4424 0.0416 0.134 Uiso 1 1 calc GR . . . .
H33B H 0.7820 0.3434 0.0297 0.134 Uiso 1 1 calc GR . . . .
H33C H 0.8560 0.3893 0.0941 0.134 Uiso 1 1 calc GR . . . .
C34 C 0.6376(5) 0.4345(3) 0.0685(3) 0.0868(18) Uani 1 1 d . . . . .
H34A H 0.6447 0.4196 0.0178 0.104 Uiso 1 1 calc R . . . .
H34B H 0.5745 0.4045 0.0790 0.104 Uiso 1 1 calc R . . . .
C35 C 0.7119(3) 0.5492(3) 0.1477(2) 0.0494(10) Uani 1 1 d . . . . .
C36 C 0.7293(3) 0.6371(2) 0.1906(2) 0.0487(10) Uani 1 1 d . . . . .
C37 C 0.6922(4) 0.7040(3) 0.1751(3) 0.0670(14) Uani 1 1 d . . . . .
H37 H 0.6541 0.6974 0.1337 0.080 Uiso 1 1 calc R . . . .
C38 C 0.7138(4) 0.7813(3) 0.2231(3) 0.0743(16) Uani 1 1 d . . . . .
H38 H 0.6901 0.8278 0.2140 0.089 Uiso 1 1 calc R . . . .
C39 C 0.7701(4) 0.7901(3) 0.2844(3) 0.0705(15) Uani 1 1 d . . . . .
H39 H 0.7844 0.8417 0.3172 0.085 Uiso 1 1 calc R . . . .
C40 C 0.8045(3) 0.7200(2) 0.2957(2) 0.0517(11) Uani 1 1 d . . . . .
C41 C 0.8617(3) 0.7134(3) 0.3588(2) 0.0539(11) Uani 1 1 d . . . . .
C42 C 0.9406(8) 0.7552(5) 0.4618(5) 0.160(5) Uani 1 1 d . . . . .
H42A H 0.9122 0.7654 0.5073 0.192 Uiso 1 1 calc R . . . .
H42B H 1.0073 0.7870 0.4672 0.192 Uiso 1 1 calc R . . . .
C43 C 0.9372(4) 0.6613(3) 0.4372(2) 0.0586(12) Uani 1 1 d . . . . .
C44 C 0.8807(8) 0.6096(7) 0.4820(4) 0.212(7) Uani 1 1 d . . . . .
H44A H 0.9235 0.5884 0.5100 0.319 Uiso 1 1 calc GR . . . .
H44B H 0.8364 0.5623 0.4528 0.319 Uiso 1 1 calc GR . . . .
H44C H 0.8448 0.6443 0.5128 0.319 Uiso 1 1 calc GR . . . .
C45 C 1.0355(6) 0.6467(9) 0.4308(4) 0.190(6) Uani 1 1 d . . . . .
H45A H 1.0705 0.6656 0.4763 0.284 Uiso 1 1 calc GR . . . .
H45B H 1.0678 0.6783 0.3977 0.284 Uiso 1 1 calc GR . . . .
H45C H 1.0330 0.5866 0.4142 0.284 Uiso 1 1 calc GR . . . .
C46 C 1.0560(3) 0.5812(3) 0.1988(2) 0.0565(11) Uani 1 1 d . . . . .
C47 C 1.0213(5) 0.5704(5) 0.1229(3) 0.100(2) Uani 1 1 d . . . . .
H47A H 1.0057 0.5105 0.1014 0.149 Uiso 1 1 calc GR . . . .
H47B H 1.0715 0.5996 0.0980 0.149 Uiso 1 1 calc GR . . . .
H47C H 0.9647 0.5942 0.1208 0.149 Uiso 1 1 calc GR . . . .
C48 C 1.0810(5) 0.6743(3) 0.2347(3) 0.0878(18) Uani 1 1 d . . . . .
H48A H 1.0234 0.6972 0.2372 0.132 Uiso 1 1 calc GR . . . .
H48B H 1.1272 0.7054 0.2081 0.132 Uiso 1 1 calc GR . . . .
H48C H 1.1085 0.6797 0.2818 0.132 Uiso 1 1 calc GR . . . .
C49 C 1.1406(4) 0.5368(4) 0.2074(3) 0.0768(15) Uani 1 1 d . . . . .
H49A H 1.1676 0.5205 0.1621 0.092 Uiso 1 1 calc R . . . .
H49B H 1.1915 0.5744 0.2401 0.092 Uiso 1 1 calc R . . . .
C50 C 1.0103(3) 0.4714(2) 0.2530(2) 0.0412(9) Uani 1 1 d . . . . .
C51 C 0.9525(3) 0.4109(2) 0.2917(2) 0.0415(9) Uani 1 1 d . . . . .
C52 C 0.9804(4) 0.3431(3) 0.3143(2) 0.0560(12) Uani 1 1 d . . . . .
H52 H 1.0411 0.3309 0.3057 0.067 Uiso 1 1 calc R . . . .
C53 C 0.9138(4) 0.2941(3) 0.3504(3) 0.0659(14) Uani 1 1 d . . . . .
H53 H 0.9300 0.2477 0.3659 0.079 Uiso 1 1 calc R . . . .
C54 C 0.8245(4) 0.3132(3) 0.3633(2) 0.0554(11) Uani 1 1 d . . . . .
H54 H 0.7803 0.2809 0.3879 0.066 Uiso 1 1 calc R . . . .
C55 C 0.8023(3) 0.3817(2) 0.3387(2) 0.0440(9) Uani 1 1 d . . . . .
C56 C 0.7122(3) 0.4143(2) 0.3471(2) 0.0481(10) Uani 1 1 d . . . . .
C57 C 0.5665(4) 0.4230(4) 0.3825(4) 0.094(2) Uani 1 1 d . . . . .
H57A H 0.5580 0.4451 0.4320 0.113 Uiso 1 1 calc R . . . .
H57B H 0.5046 0.3896 0.3604 0.113 Uiso 1 1 calc R . . . .
C58 C 0.6036(3) 0.4955(3) 0.3453(3) 0.0611(12) Uani 1 1 d . . . . .
C59 C 0.6131(5) 0.5812(4) 0.3949(5) 0.124(3) Uani 1 1 d . . . . .
H59A H 0.6577 0.5849 0.4342 0.186 Uiso 1 1 calc GR . . . .
H59B H 0.5508 0.5869 0.4121 0.186 Uiso 1 1 calc GR . . . .
H59C H 0.6368 0.6263 0.3701 0.186 Uiso 1 1 calc GR . . . .
C60 C 0.5433(4) 0.4893(6) 0.2785(4) 0.113(3) Uani 1 1 d . . . . .
H60A H 0.5679 0.5376 0.2574 0.169 Uiso 1 1 calc GR . . . .
H60B H 0.4772 0.4889 0.2897 0.169 Uiso 1 1 calc GR . . . .
H60C H 0.5463 0.4372 0.2459 0.169 Uiso 1 1 calc GR . . . .
C61 C 0.1002(6) 0.1109(6) 0.9307(5) 0.149(4) Uani 1 1 d . . . . .
H61A H 0.0690 0.1242 0.9741 0.223 Uiso 1 1 calc GR . . . .
H61B H 0.1687 0.1185 0.9410 0.223 Uiso 1 1 calc GR . . . .
H61C H 0.0742 0.0524 0.9078 0.223 Uiso 1 1 calc GR . . . .
C62 C 0.0835(5) 0.1672(6) 0.8845(5) 0.113(3) Uani 1 1 d . . . . .
C63 C 0.6098(9) 0.3322(8) 0.8552(6) 0.191(6) Uani 1 1 d . . . . .
H63A H 0.6700 0.3243 0.8354 0.286 Uiso 1 1 calc GR . . . .
H63B H 0.5567 0.2974 0.8239 0.286 Uiso 1 1 calc GR . . . .
H63C H 0.6063 0.3155 0.9004 0.286 Uiso 1 1 calc GR . . . .
C64 C 0.6038(8) 0.4309(12) 0.8652(7) 0.202(7) Uani 1 1 d . . . . .
H64A H 0.5963 0.4452 0.8191 0.243 Uiso 1 1 calc R . . . .
H64B H 0.5475 0.4405 0.8912 0.243 Uiso 1 1 calc R . . . .
C65 C 0.6931(17) 0.5765(12) 0.9289(9) 0.293(15) Uani 1 1 d . . . . .
H65A H 0.6440 0.5828 0.9631 0.351 Uiso 1 1 calc R . . . .
H65B H 0.6783 0.6018 0.8894 0.351 Uiso 1 1 calc R . . . .
C66 C 0.7927(15) 0.6217(9) 0.9634(10) 0.271(13) Uani 1 1 d . . . . .
H66A H 0.8074 0.5954 1.0017 0.407 Uiso 1 1 calc GR . . . .
H66B H 0.7931 0.6811 0.9814 0.407 Uiso 1 1 calc GR . . . .
H66C H 0.8405 0.6170 0.9288 0.407 Uiso 1 1 calc GR . . . .
N1 N 0.5003(2) 0.03451(18) 0.23535(16) 0.0397(7) Uani 1 1 d . . . . .
N2 N 0.3705(2) -0.06893(17) 0.29314(16) 0.0386(7) Uani 1 1 d . . . . .
N3 N 0.2117(2) -0.0070(2) 0.31171(18) 0.0443(8) Uani 1 1 d . . . . .
N4 N 0.2851(2) 0.0184(2) 0.15559(16) 0.0441(8) Uani 1 1 d . . . . .
N5 N 0.3147(2) 0.16232(18) 0.25120(17) 0.0391(7) Uani 1 1 d . . . . .
N6 N 0.4006(2) 0.14236(19) 0.36823(17) 0.0425(8) Uani 1 1 d . . . . .
N7 N 0.7527(3) 0.49238(19) 0.16570(17) 0.0465(8) Uani 1 1 d . . . . .
N8 N 0.7854(2) 0.64561(18) 0.24940(18) 0.0429(8) Uani 1 1 d . . . . .
N9 N 0.8843(3) 0.6446(2) 0.36625(18) 0.0475(8) Uani 1 1 d . . . . .
N10 N 0.9791(2) 0.5331(2) 0.23683(17) 0.0457(8) Uani 1 1 d . . . . .
N11 N 0.8653(2) 0.42907(18) 0.30326(16) 0.0398(7) Uani 1 1 d . . . . .
N12 N 0.7024(2) 0.4819(2) 0.32701(19) 0.0486(8) Uani 1 1 d . . . . .
N13 N 0.0699(6) 0.2086(6) 0.8471(5) 0.163(3) Uani 1 1 d . . . . .
O1 O 0.6108(2) -0.04628(17) 0.23897(16) 0.0517(7) Uani 1 1 d . . . . .
O2 O 0.1344(2) -0.1198(2) 0.35428(18) 0.0614(8) Uani 1 1 d . . . . .
O3 O 0.2037(3) 0.0713(2) 0.07965(17) 0.0720(10) Uani 1 1 d . . . . .
O4 O 0.3845(3) 0.2704(2) 0.42897(18) 0.0713(10) Uani 1 1 d . . . . .
O5 O 0.6489(3) 0.5276(2) 0.09213(18) 0.0715(10) Uani 1 1 d . . . . .
O6 O 0.8876(4) 0.7827(2) 0.4103(2) 0.0982(14) Uani 1 1 d . . . . .
O7 O 1.0981(2) 0.4608(2) 0.23535(17) 0.0599(8) Uani 1 1 d . . . . .
O8 O 0.6387(3) 0.3704(2) 0.37632(18) 0.0663(9) Uani 1 1 d . . . . .
O9 O 0.6928(6) 0.4872(6) 0.9043(3) 0.167(3) Uani 1 1 d . . . . .
P1 P 0.92558(13) 0.18532(11) 0.13282(9) 0.0811(5) Uani 1 1 d . . . . .
P2 P 0.70897(10) 0.44390(8) 0.59276(7) 0.0590(3) Uani 1 1 d . . . . .
P3 P 0.43070(13) 0.20651(10) 0.98293(9) 0.0833(5) Uani 1 1 d . . . . .
P4 P 0.19610(10) 0.95305(8) 0.58391(7) 0.0621(3) Uani 1 1 d . . . . .
F1 F 0.9925(8) 0.2710(5) 0.1371(5) 0.280(5) Uani 1 1 d . . . . .
F2 F 0.9849(5) 0.1313(6) 0.0879(4) 0.245(4) Uani 1 1 d . . . . .
F3 F 0.8738(6) 0.1937(4) 0.0651(3) 0.198(3) Uani 1 1 d . . . . .
F4 F 0.8641(5) 0.2358(6) 0.1781(3) 0.229(4) Uani 1 1 d . . . . .
F5 F 0.9838(6) 0.1821(4) 0.1980(3) 0.211(3) Uani 1 1 d . . . . .
F6 F 0.8540(7) 0.1009(5) 0.1265(4) 0.251(4) Uani 1 1 d . . . . .
F7 F 0.8036(3) 0.5145(3) 0.6169(2) 0.1150(13) Uani 1 1 d . . . . .
F8 F 0.7504(3) 0.4253(3) 0.51730(18) 0.1130(13) Uani 1 1 d . . . . .
F9 F 0.6565(4) 0.5114(3) 0.5693(2) 0.1287(16) Uani 1 1 d . . . . .
F10 F 0.6717(3) 0.4687(4) 0.6693(2) 0.1370(17) Uani 1 1 d . . . . .
F11 F 0.7589(3) 0.3779(2) 0.6209(2) 0.1112(13) Uani 1 1 d . . . . .
F12 F 0.6140(3) 0.3745(3) 0.5694(3) 0.1361(17) Uani 1 1 d . . . . .
F13 F 0.5429(3) 0.2261(3) 1.0042(2) 0.1253(15) Uani 1 1 d . . . . .
F14 F 0.4541(4) 0.1815(3) 0.9017(2) 0.1451(18) Uani 1 1 d . . . . .
F15 F 0.4246(4) 0.1120(3) 0.9906(3) 0.162(2) Uani 1 1 d . . . . .
F16 F 0.4121(4) 0.2331(4) 1.0620(2) 0.158(2) Uani 1 1 d . . . . .
F17 F 0.4421(3) 0.3042(2) 0.9745(2) 0.1148(13) Uani 1 1 d . . . . .
F18 F 0.3236(4) 0.1906(4) 0.9587(4) 0.199(3) Uani 1 1 d . . . . .
F19 F 0.2958(4) 1.0148(4) 0.6070(2) 0.167(2) Uani 1 1 d . . . . .
F20 F 0.2362(3) 0.9223(3) 0.5104(2) 0.1216(14) Uani 1 1 d . . . . .
F21 F 0.1635(7) 1.0215(5) 0.5539(3) 0.262(5) Uani 1 1 d . . . . .
F22 F 0.1573(4) 0.9894(3) 0.6576(2) 0.1359(17) Uani 1 1 d . . . . .
F23 F 0.2364(5) 0.8885(4) 0.6197(3) 0.167(2) Uani 1 1 d . . . . .
F24 F 0.1009(4) 0.8855(4) 0.5668(3) 0.190(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.208(3) . ?
Fe1 N2 2.122(3) . ?
Fe1 N3 2.281(3) . ?
Fe1 N4 2.207(3) . ?
Fe1 N5 2.114(3) . ?
Fe1 N6 2.279(3) . ?
Fe2 N7 2.229(3) . ?
Fe2 N8 2.109(3) . ?
Fe2 N9 2.250(3) . ?
Fe2 N10 2.199(3) . ?
Fe2 N11 2.111(3) . ?
Fe2 N12 2.257(3) . ?
C1 C2 1.510(6) . ?
C1 C3 1.505(6) . ?
C1 C4 1.537(6) . ?
C1 N1 1.497(5) . ?
C4 O1 1.473(5) . ?
C5 C6 1.471(5) . ?
C5 N1 1.266(5) . ?
C5 O1 1.327(5) . ?
C6 C7 1.381(5) . ?
C6 N2 1.335(5) . ?
C7 C8 1.387(7) . ?
C8 C9 1.368(7) . ?
C9 C10 1.385(6) . ?
C10 C11 1.478(6) . ?
C10 N2 1.332(5) . ?
C11 N3 1.261(5) . ?
C11 O2 1.334(5) . ?
C12 C13 1.524(7) . ?
C12 O2 1.457(6) . ?
C13 C14 1.503(7) . ?
C13 C15 1.493(7) . ?
C13 N3 1.504(5) . ?
C16 C17 1.499(7) . ?
C16 C18 1.511(7) . ?
C16 C19 1.549(7) . ?
C16 N4 1.501(5) . ?
C19 O3 1.448(6) . ?
C20 C21 1.483(6) . ?
C20 N4 1.262(5) . ?
C20 O3 1.329(5) . ?
C21 C22 1.378(6) . ?
C21 N5 1.328(5) . ?
C22 C23 1.363(7) . ?
C23 C24 1.389(7) . ?
C24 C25 1.386(5) . ?
C25 C26 1.480(6) . ?
C25 N5 1.330(5) . ?
C26 N6 1.261(5) . ?
C26 O4 1.336(5) . ?
C27 C28 1.527(7) . ?
C27 O4 1.465(7) . ?
C28 C29 1.512(7) . ?
C28 C30 1.509(7) . ?
C28 N6 1.491(5) . ?
C31 C32 1.508(7) . ?
C31 C33 1.521(8) . ?
C31 C34 1.543(7) . ?
C31 N7 1.506(5) . ?
C34 O5 1.469(6) . ?
C35 C36 1.474(6) . ?
C35 N7 1.280(5) . ?
C35 O5 1.323(5) . ?
C36 C37 1.379(6) . ?
C36 N8 1.337(5) . ?
C37 C38 1.382(7) . ?
C38 C39 1.377(8) . ?
C39 C40 1.378(6) . ?
C40 C41 1.478(7) . ?
C40 N8 1.330(5) . ?
C41 N9 1.258(5) . ?
C41 O6 1.331(5) . ?
C42 C43 1.499(8) . ?
C42 O6 1.423(8) . ?
C43 C44 1.456(8) . ?
C43 C45 1.458(9) . ?
C43 N9 1.494(6) . ?
C46 C47 1.498(7) . ?
C46 C48 1.503(7) . ?
C46 C49 1.537(7) . ?
C46 N10 1.494(5) . ?
C49 O7 1.465(6) . ?
C50 C51 1.472(5) . ?
C50 N10 1.264(5) . ?
C50 O7 1.326(5) . ?
C51 C52 1.384(5) . ?
C51 N11 1.335(5) . ?
C52 C53 1.391(7) . ?
C53 C54 1.374(7) . ?
C54 C55 1.379(6) . ?
C55 C56 1.474(6) . ?
C55 N11 1.341(5) . ?
C56 N12 1.266(5) . ?
C56 O8 1.334(5) . ?
C57 C58 1.507(7) . ?
C57 O8 1.450(7) . ?
C58 C59 1.508(7) . ?
C58 C60 1.502(8) . ?
C58 N12 1.493(6) . ?
C61 C62 1.443(10) . ?
C62 N13 1.116(9) . ?
C63 C64 1.599(17) . ?
C64 O9 1.486(13) . ?
C65 C66 1.52(3) . ?
C65 O9 1.436(16) . ?
P1 F1 1.502(6) . ?
P1 F2 1.501(5) . ?
P1 F3 1.526(5) . ?
P1 F4 1.492(5) . ?
P1 F5 1.502(5) . ?
P1 F6 1.511(6) . ?
P2 F7 1.569(4) . ?
P2 F8 1.575(4) . ?
P2 F9 1.571(4) . ?
P2 F10 1.580(4) . ?
P2 F11 1.568(3) . ?
P2 F12 1.560(4) . ?
P3 F13 1.579(4) . ?
P3 F14 1.595(5) . ?
P3 F15 1.557(4) . ?
P3 F16 1.543(5) . ?
P3 F17 1.604(4) . ?
P3 F18 1.529(5) . ?
P4 F19 1.552(5) . ?
P4 F20 1.564(4) . ?
P4 F21 1.494(5) . ?
P4 F22 1.580(4) . ?
P4 F23 1.553(5) . ?
P4 F24 1.536(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N3 148.70(11) . . ?
N1 Fe1 N6 95.31(12) . . ?
N2 Fe1 N1 75.11(11) . . ?
N2 Fe1 N3 73.59(12) . . ?
N2 Fe1 N4 109.64(12) . . ?
N2 Fe1 N6 100.91(11) . . ?
N4 Fe1 N1 97.32(12) . . ?
N4 Fe1 N3 93.59(13) . . ?
N4 Fe1 N6 149.01(11) . . ?
N5 Fe1 N1 114.87(11) . . ?
N5 Fe1 N2 168.82(12) . . ?
N5 Fe1 N3 96.26(12) . . ?
N5 Fe1 N4 75.09(12) . . ?
N5 Fe1 N6 73.92(12) . . ?
N6 Fe1 N3 90.06(12) . . ?
N7 Fe2 N9 148.97(12) . . ?
N7 Fe2 N12 92.01(13) . . ?
N8 Fe2 N7 74.84(12) . . ?
N8 Fe2 N9 74.14(13) . . ?
N8 Fe2 N10 112.00(12) . . ?
N8 Fe2 N11 172.71(13) . . ?
N8 Fe2 N12 98.99(13) . . ?
N9 Fe2 N12 92.17(13) . . ?
N10 Fe2 N7 97.78(13) . . ?
N10 Fe2 N9 94.30(13) . . ?
N10 Fe2 N12 148.95(12) . . ?
N11 Fe2 N7 106.93(11) . . ?
N11 Fe2 N9 103.77(12) . . ?
N11 Fe2 N10 74.98(12) . . ?
N11 Fe2 N12 73.99(13) . . ?
C2 C1 C4 111.2(4) . . ?
C3 C1 C2 111.1(4) . . ?
C3 C1 C4 112.0(4) . . ?
N1 C1 C2 109.3(3) . . ?
N1 C1 C3 110.5(4) . . ?
N1 C1 C4 102.4(3) . . ?
O1 C4 C1 105.1(3) . . ?
N1 C5 C6 122.2(4) . . ?
N1 C5 O1 119.8(3) . . ?
O1 C5 C6 118.0(3) . . ?
C7 C6 C5 127.4(4) . . ?
N2 C6 C5 111.5(3) . . ?
N2 C6 C7 121.2(4) . . ?
C6 C7 C8 118.5(4) . . ?
C9 C8 C7 120.0(4) . . ?
C8 C9 C10 118.5(4) . . ?
C9 C10 C11 127.1(4) . . ?
N2 C10 C9 121.5(4) . . ?
N2 C10 C11 111.3(3) . . ?
N3 C11 C10 122.0(3) . . ?
N3 C11 O2 119.5(4) . . ?
O2 C11 C10 118.4(3) . . ?
O2 C12 C13 106.0(4) . . ?
C14 C13 C12 110.6(5) . . ?
C14 C13 N3 108.4(4) . . ?
C15 C13 C12 112.4(5) . . ?
C15 C13 C14 111.9(5) . . ?
C15 C13 N3 111.0(4) . . ?
N3 C13 C12 102.1(4) . . ?
C17 C16 C18 110.8(5) . . ?
C17 C16 C19 110.2(5) . . ?
C17 C16 N4 110.3(4) . . ?
C18 C16 C19 114.4(5) . . ?
N4 C16 C18 109.1(4) . . ?
N4 C16 C19 101.6(4) . . ?
O3 C19 C16 105.6(4) . . ?
N4 C20 C21 122.0(4) . . ?
N4 C20 O3 119.8(4) . . ?
O3 C20 C21 118.2(4) . . ?
C22 C21 C20 126.8(4) . . ?
N5 C21 C20 111.1(3) . . ?
N5 C21 C22 122.0(4) . . ?
C23 C22 C21 118.5(5) . . ?
C22 C23 C24 120.3(4) . . ?
C25 C24 C23 117.5(4) . . ?
C24 C25 C26 126.6(4) . . ?
N5 C25 C24 121.9(4) . . ?
N5 C25 C26 111.4(3) . . ?
N6 C26 C25 122.2(3) . . ?
N6 C26 O4 118.9(4) . . ?
O4 C26 C25 118.8(3) . . ?
O4 C27 C28 104.3(4) . . ?
C29 C28 C27 110.7(5) . . ?
C30 C28 C27 112.2(5) . . ?
C30 C28 C29 111.1(5) . . ?
N6 C28 C27 102.5(4) . . ?
N6 C28 C29 109.9(4) . . ?
N6 C28 C30 110.2(4) . . ?
C32 C31 C33 111.0(5) . . ?
C32 C31 C34 112.1(5) . . ?
C33 C31 C34 112.0(5) . . ?
N7 C31 C32 110.2(4) . . ?
N7 C31 C33 109.3(4) . . ?
N7 C31 C34 101.9(4) . . ?
O5 C34 C31 104.7(4) . . ?
N7 C35 C36 121.0(4) . . ?
N7 C35 O5 119.5(4) . . ?
O5 C35 C36 119.3(4) . . ?
C37 C36 C35 126.0(4) . . ?
N8 C36 C35 111.9(3) . . ?
N8 C36 C37 122.1(4) . . ?
C36 C37 C38 117.8(5) . . ?
C39 C38 C37 120.4(4) . . ?
C38 C39 C40 118.1(4) . . ?
C39 C40 C41 127.3(4) . . ?
N8 C40 C39 122.1(5) . . ?
N8 C40 C41 110.6(3) . . ?
N9 C41 C40 122.6(4) . . ?
N9 C41 O6 119.1(5) . . ?
O6 C41 C40 118.3(4) . . ?
O6 C42 C43 108.2(5) . . ?
C44 C43 C42 112.3(8) . . ?
C44 C43 C45 112.7(8) . . ?
C44 C43 N9 109.2(4) . . ?
C45 C43 C42 109.7(8) . . ?
C45 C43 N9 111.4(4) . . ?
N9 C43 C42 100.9(5) . . ?
C47 C46 C48 111.3(5) . . ?
C47 C46 C49 112.8(5) . . ?
C48 C46 C49 111.4(5) . . ?
N10 C46 C47 109.3(4) . . ?
N10 C46 C48 110.0(4) . . ?
N10 C46 C49 101.7(3) . . ?
O7 C49 C46 105.0(4) . . ?
N10 C50 C51 121.9(4) . . ?
N10 C50 O7 119.4(4) . . ?
O7 C50 C51 118.7(3) . . ?
C52 C51 C50 127.0(4) . . ?
N11 C51 C50 110.9(3) . . ?
N11 C51 C52 122.1(4) . . ?
C51 C52 C53 117.3(4) . . ?
C54 C53 C52 120.8(4) . . ?
C53 C54 C55 118.2(4) . . ?
C54 C55 C56 127.5(4) . . ?
N11 C55 C54 121.7(4) . . ?
N11 C55 C56 110.7(3) . . ?
N12 C56 C55 122.2(4) . . ?
N12 C56 O8 119.3(4) . . ?
O8 C56 C55 118.5(4) . . ?
O8 C57 C58 106.5(4) . . ?
C57 C58 C59 111.0(5) . . ?
C60 C58 C57 112.1(5) . . ?
C60 C58 C59 112.2(6) . . ?
N12 C58 C57 102.3(4) . . ?
N12 C58 C59 109.1(4) . . ?
N12 C58 C60 109.7(4) . . ?
N13 C62 C61 177.9(12) . . ?
O9 C64 C63 110.7(11) . . ?
O9 C65 C66 108.8(13) . . ?
C1 N1 Fe1 140.0(2) . . ?
C5 N1 Fe1 112.4(3) . . ?
C5 N1 C1 107.5(3) . . ?
C6 N2 Fe1 118.6(2) . . ?
C10 N2 Fe1 120.8(3) . . ?
C10 N2 C6 120.3(3) . . ?
C11 N3 Fe1 112.0(3) . . ?
C11 N3 C13 107.2(3) . . ?
C13 N3 Fe1 140.8(3) . . ?
C16 N4 Fe1 139.6(3) . . ?
C20 N4 Fe1 112.5(3) . . ?
C20 N4 C16 107.4(3) . . ?
C21 N5 Fe1 119.2(2) . . ?
C21 N5 C25 119.7(3) . . ?
C25 N5 Fe1 120.5(3) . . ?
C26 N6 Fe1 111.4(3) . . ?
C26 N6 C28 107.2(3) . . ?
C28 N6 Fe1 141.0(2) . . ?
C31 N7 Fe2 140.4(3) . . ?
C35 N7 Fe2 112.3(3) . . ?
C35 N7 C31 106.7(3) . . ?
C36 N8 Fe2 119.5(2) . . ?
C40 N8 Fe2 120.7(3) . . ?
C40 N8 C36 119.6(3) . . ?
C41 N9 Fe2 111.9(3) . . ?
C41 N9 C43 107.5(4) . . ?
C43 N9 Fe2 140.6(3) . . ?
C46 N10 Fe2 139.5(3) . . ?
C50 N10 Fe2 112.8(3) . . ?
C50 N10 C46 107.7(3) . . ?
C51 N11 Fe2 119.2(2) . . ?
C51 N11 C55 119.9(3) . . ?
C55 N11 Fe2 120.8(3) . . ?
C56 N12 Fe2 112.2(3) . . ?
C56 N12 C58 107.0(4) . . ?
C58 N12 Fe2 140.7(3) . . ?
C5 O1 C4 105.2(3) . . ?
C11 O2 C12 105.1(3) . . ?
C20 O3 C19 105.5(4) . . ?
C26 O4 C27 105.2(3) . . ?
C35 O5 C34 105.5(3) . . ?
C41 O6 C42 104.1(4) . . ?
C50 O7 C49 105.0(3) . . ?
C56 O8 C57 104.5(4) . . ?
C65 O9 C64 118.3(13) . . ?
F1 P1 F3 91.3(4) . . ?
F1 P1 F5 84.4(4) . . ?
F1 P1 F6 176.8(6) . . ?
F2 P1 F1 97.9(6) . . ?
F2 P1 F3 88.7(4) . . ?
F2 P1 F5 90.0(4) . . ?
F2 P1 F6 83.6(5) . . ?
F4 P1 F1 84.3(5) . . ?
F4 P1 F2 177.7(6) . . ?
F4 P1 F3 91.7(4) . . ?
F4 P1 F5 89.8(3) . . ?
F4 P1 F6 94.2(6) . . ?
F5 P1 F3 175.3(5) . . ?
F5 P1 F6 98.4(5) . . ?
F6 P1 F3 86.0(4) . . ?
F7 P2 F8 88.0(2) . . ?
F7 P2 F9 91.0(3) . . ?
F7 P2 F10 88.6(3) . . ?
F8 P2 F10 176.2(3) . . ?
F9 P2 F8 90.4(3) . . ?
F9 P2 F10 88.1(3) . . ?
F11 P2 F7 89.0(2) . . ?
F11 P2 F8 93.2(2) . . ?
F11 P2 F9 176.4(3) . . ?
F11 P2 F10 88.3(2) . . ?
F12 P2 F7 179.2(3) . . ?
F12 P2 F8 92.7(3) . . ?
F12 P2 F9 88.5(3) . . ?
F12 P2 F10 90.8(3) . . ?
F12 P2 F11 91.5(2) . . ?
F13 P3 F14 89.2(3) . . ?
F13 P3 F17 88.7(2) . . ?
F14 P3 F17 89.1(2) . . ?
F15 P3 F13 89.0(3) . . ?
F15 P3 F14 89.9(3) . . ?
F15 P3 F17 177.4(3) . . ?
F16 P3 F13 88.8(3) . . ?
F16 P3 F14 177.7(3) . . ?
F16 P3 F15 91.1(3) . . ?
F16 P3 F17 89.8(3) . . ?
F18 P3 F13 176.5(3) . . ?
F18 P3 F14 88.3(4) . . ?
F18 P3 F15 93.5(3) . . ?
F18 P3 F16 93.6(4) . . ?
F18 P3 F17 88.8(3) . . ?
F19 P4 F20 89.0(3) . . ?
F19 P4 F22 89.2(3) . . ?
F19 P4 F23 85.9(4) . . ?
F20 P4 F22 176.8(3) . . ?
F21 P4 F19 89.4(5) . . ?
F21 P4 F20 88.2(3) . . ?
F21 P4 F22 89.2(3) . . ?
F21 P4 F23 174.8(5) . . ?
F21 P4 F24 97.1(5) . . ?
F23 P4 F20 93.9(3) . . ?
F23 P4 F22 88.6(3) . . ?
F24 P4 F19 173.3(4) . . ?
F24 P4 F20 92.9(3) . . ?
F24 P4 F22 89.2(3) . . ?
F24 P4 F23 87.5(4) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-1
_database_code_depnum_ccdc_archive 'CCDC 1468983'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;

_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
   1  0.000  0.061  0.250        58         3
   2  0.000 -0.061  0.750        58         3
   3  0.500 -0.031  0.250       169        35
   4  0.500  0.031  0.750       169        35
   5  0.000  0.181  0.750         6         0
   6  0.000  0.347  0.250        13         1
   7  0.000  0.652  0.750        13         1
   8  0.000  0.819  0.250         5         0
;
_platon_squeeze_details          
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 78e per unit cell, which are accumulated which corresponds 
to 19.5e per formula(C78H78B2FeN6O4). The 19.5e might come from one 
ether molecule and are not included in the formula.
;


_audit_creation_date             2016-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            4-1
_chemical_name_systematic        4-1
_chemical_formula_moiety         'C30 H38 Fe N6 O4, 2(C24 H20 B)'
_chemical_formula_sum            'C78 H78 B2 Fe N6 O4'
_chemical_formula_weight         1240.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C84 H93 Fe1 B2 N7 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   23.3002(4)
_cell_length_b                   13.24618(16)
_cell_length_c                   24.3060(4)
_cell_angle_alpha                90
_cell_angle_beta                 114.454(2)
_cell_angle_gamma                90
_cell_volume                     6828.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10115
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      73.6520
_cell_measurement_theta_min      3.3070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27190
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         3.889
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00    1.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7931   38.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
  2 omega -119.00   -3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7931  -19.0000   90.0000 116

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7931 -125.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega   39.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7931 -125.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
  5 omega   29.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -30.0000   90.0000 48

#__ type_ start__ end____ width___ exp.time_
  6 omega   33.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -45.0000  -90.0000 65

#__ type_ start__ end____ width___ exp.time_
  7 omega   84.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   77.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  8 omega  102.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   77.0000    0.0000 76

#__ type_ start__ end____ width___ exp.time_
  9 omega   68.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -45.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 10 omega   71.00  106.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775  -94.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
 11 omega  111.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   61.0000  -30.0000 67

#__ type_ start__ end____ width___ exp.time_
 12 omega  153.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3775   68.0000   53.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0034195000
_diffrn_orient_matrix_UB_12      -0.0880667000
_diffrn_orient_matrix_UB_13      -0.0399985000
_diffrn_orient_matrix_UB_21      -0.0685643000
_diffrn_orient_matrix_UB_22      0.0208449000
_diffrn_orient_matrix_UB_23      -0.0447816000
_diffrn_orient_matrix_UB_31      0.0237343000
_diffrn_orient_matrix_UB_32      0.0730993000
_diffrn_orient_matrix_UB_33      -0.0352540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10991
_reflns_number_total             13256
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         13256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0501P)²+1.0789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1002
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C71(H71), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.74797(2) 0.25519(2) 0.51568(2) 0.02062(6) Uani 1 1 d . . . . .
O1 O 0.84925(6) 0.47526(9) 0.48116(6) 0.0386(3) Uani 1 1 d . . . . .
O2 O 0.67161(7) 0.02648(9) 0.39608(6) 0.0447(3) Uani 1 1 d . . . . .
O3 O 0.88494(6) 0.11652(11) 0.65931(6) 0.0468(3) Uani 1 1 d . . . . .
O4 O 0.60306(5) 0.39947(9) 0.53379(5) 0.0324(2) Uani 1 1 d . . . . .
N1 N 0.79946(6) 0.38127(9) 0.52518(6) 0.0256(3) Uani 1 1 d . . . . .
N2 N 0.75471(6) 0.25634(9) 0.44030(6) 0.0247(3) Uani 1 1 d . . . . .
N3 N 0.70071(6) 0.12688(10) 0.47816(6) 0.0273(3) Uani 1 1 d . . . . .
N4 N 0.82703(6) 0.17727(10) 0.56589(6) 0.0280(3) Uani 1 1 d . . . . .
N5 N 0.74256(6) 0.25383(9) 0.59176(6) 0.0239(2) Uani 1 1 d . . . . .
N6 N 0.66830(6) 0.33572(9) 0.49509(5) 0.0238(2) Uani 1 1 d . . . . .
C1 C 0.86414(9) 0.42797(14) 0.63344(8) 0.0396(4) Uani 1 1 d . . . . .
H1A H 0.8341 0.4008 0.6484 0.059 Uiso 1 1 calc GR . . . .
H1B H 0.8876 0.4839 0.6594 0.059 Uiso 1 1 calc GR . . . .
H1C H 0.8936 0.3747 0.6340 0.059 Uiso 1 1 calc GR . . . .
C2 C 0.77738(9) 0.53941(14) 0.56552(9) 0.0415(4) Uani 1 1 d . . . . .
H2A H 0.7577 0.5676 0.5246 0.062 Uiso 1 1 calc GR . . . .
H2B H 0.7958 0.5941 0.5947 0.062 Uiso 1 1 calc GR . . . .
H2C H 0.7455 0.5041 0.5748 0.062 Uiso 1 1 calc GR . . . .
C3 C 0.82870(8) 0.46579(12) 0.56936(7) 0.0307(3) Uani 1 1 d . . . . .
C4 C 0.87321(9) 0.51156(14) 0.54388(9) 0.0403(4) Uani 1 1 d . . . . .
H4A H 0.8722 0.5862 0.5451 0.048 Uiso 1 1 calc R . . . .
H4B H 0.9171 0.4885 0.5673 0.048 Uiso 1 1 calc R . . . .
C5 C 0.81235(8) 0.39822(12) 0.47952(7) 0.0285(3) Uani 1 1 d . . . . .
C6 C 0.78739(8) 0.32990(12) 0.42768(7) 0.0296(3) Uani 1 1 d . . . . .
C7 C 0.79502(10) 0.33195(14) 0.37415(8) 0.0396(4) Uani 1 1 d . . . . .
H7 H 0.8182 0.3843 0.3660 0.048 Uiso 1 1 calc R . . . .
C8 C 0.76753(12) 0.25474(15) 0.33268(9) 0.0466(5) Uani 1 1 d . . . . .
H8 H 0.7717 0.2543 0.2954 0.056 Uiso 1 1 calc R . . . .
C9 C 0.73410(11) 0.17851(14) 0.34546(8) 0.0431(4) Uani 1 1 d . . . . .
H9 H 0.7153 0.1255 0.3174 0.052 Uiso 1 1 calc R . . . .
C10 C 0.72884(8) 0.18173(12) 0.40011(7) 0.0306(3) Uani 1 1 d . . . . .
C11 C 0.69896(8) 0.11010(12) 0.42540(7) 0.0309(3) Uani 1 1 d . . . . .
C12 C 0.65617(16) -0.03056(19) 0.43909(12) 0.0714(8) Uani 1 1 d . . . . .
H12A H 0.6834 -0.0910 0.4528 0.086 Uiso 1 1 calc R . . . .
H12B H 0.6116 -0.0526 0.4204 0.086 Uiso 1 1 calc R . . . .
C13 C 0.66752(8) 0.04080(12) 0.49262(8) 0.0339(4) Uani 1 1 d . . . . .
C14 C 0.70896(11) -0.00883(16) 0.55149(11) 0.0554(6) Uani 1 1 d . . . . .
H14A H 0.7496 -0.0261 0.5510 0.083 Uiso 1 1 calc GR . . . .
H14B H 0.6885 -0.0704 0.5568 0.083 Uiso 1 1 calc GR . . . .
H14C H 0.7157 0.0377 0.5849 0.083 Uiso 1 1 calc GR . . . .
C15 C 0.60650(12) 0.07618(18) 0.49296(15) 0.0671(7) Uani 1 1 d . . . . .
H15A H 0.6151 0.1277 0.5243 0.101 Uiso 1 1 calc GR . . . .
H15B H 0.5847 0.0189 0.5014 0.101 Uiso 1 1 calc GR . . . .
H15C H 0.5799 0.1050 0.4534 0.101 Uiso 1 1 calc GR . . . .
C16 C 0.86207(12) 0.05166(18) 0.51083(12) 0.0596(6) Uani 1 1 d . . . . .
H16A H 0.8343 0.0030 0.5181 0.089 Uiso 1 1 calc GR . . . .
H16B H 0.8992 0.0165 0.5111 0.089 Uiso 1 1 calc GR . . . .
H16C H 0.8393 0.0840 0.4715 0.089 Uiso 1 1 calc GR . . . .
C17 C 0.92170(10) 0.21250(17) 0.54758(13) 0.0558(6) Uani 1 1 d . . . . .
H17A H 0.8977 0.2413 0.5074 0.084 Uiso 1 1 calc GR . . . .
H17B H 0.9610 0.1831 0.5492 0.084 Uiso 1 1 calc GR . . . .
H17C H 0.9316 0.2657 0.5781 0.084 Uiso 1 1 calc GR . . . .
C18 C 0.88282(8) 0.13109(14) 0.55994(9) 0.0370(4) Uani 1 1 d . . . . .
C19 C 0.91840(12) 0.0842(2) 0.62274(11) 0.0654(7) Uani 1 1 d . . . . .
H19A H 0.9185 0.0097 0.6199 0.078 Uiso 1 1 calc R . . . .
H19B H 0.9626 0.1082 0.6410 0.078 Uiso 1 1 calc R . . . .
C20 C 0.83418(8) 0.16554(13) 0.62081(8) 0.0311(3) Uani 1 1 d . . . . .
C21 C 0.78745(8) 0.20780(12) 0.63939(7) 0.0291(3) Uani 1 1 d . . . . .
C22 C 0.78589(9) 0.20736(15) 0.69583(8) 0.0381(4) Uani 1 1 d . . . . .
H22 H 0.8176 0.1735 0.7290 0.046 Uiso 1 1 calc R . . . .
C23 C 0.73689(10) 0.25755(15) 0.70270(8) 0.0408(4) Uani 1 1 d . . . . .
H23 H 0.7348 0.2583 0.7409 0.049 Uiso 1 1 calc R . . . .
C24 C 0.69087(9) 0.30676(14) 0.65369(7) 0.0354(4) Uani 1 1 d . . . . .
H24 H 0.6576 0.3426 0.6580 0.042 Uiso 1 1 calc R . . . .
C25 C 0.69490(7) 0.30197(12) 0.59834(7) 0.0260(3) Uani 1 1 d . . . . .
C26 C 0.65406(7) 0.34675(11) 0.54043(7) 0.0257(3) Uani 1 1 d . . . . .
C27 C 0.58325(9) 0.44714(14) 0.47401(8) 0.0361(4) Uani 1 1 d . . . . .
H27A H 0.5962 0.5189 0.4781 0.043 Uiso 1 1 calc R . . . .
H27B H 0.5369 0.4432 0.4511 0.043 Uiso 1 1 calc R . . . .
C28 C 0.61708(7) 0.38609(12) 0.44218(7) 0.0283(3) Uani 1 1 d . . . . .
C29 C 0.57416(8) 0.30555(13) 0.40054(8) 0.0348(4) Uani 1 1 d . . . . .
H29A H 0.5987 0.2623 0.3855 0.052 Uiso 1 1 calc GR . . . .
H29B H 0.5401 0.3381 0.3663 0.052 Uiso 1 1 calc GR . . . .
H29C H 0.5561 0.2645 0.4230 0.052 Uiso 1 1 calc GR . . . .
C30 C 0.64381(9) 0.45419(14) 0.40805(8) 0.0368(4) Uani 1 1 d . . . . .
H30A H 0.6746 0.5007 0.4365 0.055 Uiso 1 1 calc GR . . . .
H30B H 0.6095 0.4930 0.3776 0.055 Uiso 1 1 calc GR . . . .
H30C H 0.6645 0.4128 0.3881 0.055 Uiso 1 1 calc GR . . . .
C31 C 0.39286(7) 0.33462(12) 0.34307(7) 0.0290(3) Uani 1 1 d . . . . .
C32 C 0.40150(8) 0.31327(14) 0.29048(7) 0.0346(4) Uani 1 1 d . . . . .
H32 H 0.3892 0.2490 0.2720 0.041 Uiso 1 1 calc R . . . .
C33 C 0.42735(9) 0.38266(16) 0.26440(8) 0.0414(4) Uani 1 1 d . . . . .
H33 H 0.4323 0.3651 0.2287 0.050 Uiso 1 1 calc R . . . .
C34 C 0.44596(9) 0.47705(15) 0.28985(9) 0.0426(4) Uani 1 1 d . . . . .
H34 H 0.4634 0.5247 0.2718 0.051 Uiso 1 1 calc R . . . .
C35 C 0.43872(9) 0.50086(14) 0.34198(9) 0.0397(4) Uani 1 1 d . . . . .
H35 H 0.4515 0.5652 0.3602 0.048 Uiso 1 1 calc R . . . .
C36 C 0.41279(8) 0.43081(13) 0.36770(8) 0.0343(4) Uani 1 1 d . . . . .
H36 H 0.4084 0.4489 0.4036 0.041 Uiso 1 1 calc R . . . .
C37 C 0.27851(8) 0.28858(13) 0.33253(7) 0.0306(3) Uani 1 1 d . . . . .
C38 C 0.25822(9) 0.38207(14) 0.30310(8) 0.0361(4) Uani 1 1 d . . . . .
H38 H 0.2892 0.4303 0.3051 0.043 Uiso 1 1 calc R . . . .
C39 C 0.19460(10) 0.40692(16) 0.27114(8) 0.0442(4) Uani 1 1 d . . . . .
H39 H 0.1832 0.4710 0.2522 0.053 Uiso 1 1 calc R . . . .
C40 C 0.14849(9) 0.33850(18) 0.26707(9) 0.0474(5) Uani 1 1 d . . . . .
H40 H 0.1052 0.3543 0.2446 0.057 Uiso 1 1 calc R . . . .
C41 C 0.16610(9) 0.24631(17) 0.29617(9) 0.0432(4) Uani 1 1 d . . . . .
H41 H 0.1347 0.1988 0.2941 0.052 Uiso 1 1 calc R . . . .
C42 C 0.22970(8) 0.22292(15) 0.32842(8) 0.0359(4) Uani 1 1 d . . . . .
H42 H 0.2404 0.1596 0.3485 0.043 Uiso 1 1 calc R . . . .
C43 C 0.36718(8) 0.14003(12) 0.35550(7) 0.0295(3) Uani 1 1 d . . . . .
C44 C 0.32665(9) 0.08595(14) 0.30478(8) 0.0377(4) Uani 1 1 d . . . . .
H44 H 0.2888 0.1177 0.2779 0.045 Uiso 1 1 calc R . . . .
C45 C 0.33890(10) -0.01183(15) 0.29166(9) 0.0464(5) Uani 1 1 d . . . . .
H45 H 0.3099 -0.0448 0.2564 0.056 Uiso 1 1 calc R . . . .
C46 C 0.39282(11) -0.06094(15) 0.32961(10) 0.0486(5) Uani 1 1 d . . . . .
H46 H 0.4014 -0.1278 0.3211 0.058 Uiso 1 1 calc R . . . .
C47 C 0.43438(10) -0.01072(16) 0.38062(10) 0.0496(5) Uani 1 1 d . . . . .
H47 H 0.4718 -0.0435 0.4075 0.059 Uiso 1 1 calc R . . . .
C48 C 0.42167(9) 0.08693(14) 0.39258(9) 0.0401(4) Uani 1 1 d . . . . .
H48 H 0.4513 0.1196 0.4276 0.048 Uiso 1 1 calc R . . . .
C49 C 0.37755(8) 0.27337(12) 0.44236(7) 0.0281(3) Uani 1 1 d . . . . .
C50 C 0.33636(8) 0.27648(12) 0.47100(7) 0.0300(3) Uani 1 1 d . . . . .
H50 H 0.2923 0.2740 0.4467 0.036 Uiso 1 1 calc R . . . .
C51 C 0.35722(10) 0.28310(12) 0.53366(8) 0.0369(4) Uani 1 1 d . . . . .
H51 H 0.3275 0.2861 0.5511 0.044 Uiso 1 1 calc R . . . .
C52 C 0.42109(10) 0.28526(14) 0.57029(8) 0.0414(4) Uani 1 1 d . . . . .
H52 H 0.4356 0.2881 0.6130 0.050 Uiso 1 1 calc R . . . .
C53 C 0.46347(10) 0.28318(14) 0.54397(8) 0.0416(4) Uani 1 1 d . . . . .
H53 H 0.5075 0.2845 0.5687 0.050 Uiso 1 1 calc R . . . .
C54 C 0.44201(9) 0.27919(13) 0.48150(8) 0.0347(4) Uani 1 1 d . . . . .
H54 H 0.4721 0.2804 0.4645 0.042 Uiso 1 1 calc R . . . .
B1 B 0.35391(9) 0.25886(14) 0.36897(8) 0.0277(4) Uani 1 1 d . . . . .
C55 C 0.11289(8) 0.23978(11) 0.52284(7) 0.0302(3) Uani 1 1 d . . . . .
C56 C 0.05070(9) 0.26113(13) 0.48225(8) 0.0376(4) Uani 1 1 d . . . . .
H56 H 0.0206 0.2764 0.4980 0.045 Uiso 1 1 calc R . . . .
C57 C 0.03128(10) 0.26088(14) 0.41954(9) 0.0450(5) Uani 1 1 d . . . . .
H57 H -0.0113 0.2761 0.3937 0.054 Uiso 1 1 calc R . . . .
C58 C 0.07362(11) 0.23857(14) 0.39487(9) 0.0464(5) Uani 1 1 d . . . . .
H58 H 0.0604 0.2375 0.3523 0.056 Uiso 1 1 calc R . . . .
C59 C 0.13553(11) 0.21788(14) 0.43309(9) 0.0443(4) Uani 1 1 d . . . . .
H59 H 0.1653 0.2031 0.4168 0.053 Uiso 1 1 calc R . . . .
C60 C 0.15441(9) 0.21863(13) 0.49551(8) 0.0361(4) Uani 1 1 d . . . . .
H60 H 0.1972 0.2042 0.5208 0.043 Uiso 1 1 calc R . . . .
C61 C 0.20976(8) 0.26639(12) 0.63080(7) 0.0288(3) Uani 1 1 d . . . . .
C62 C 0.22863(9) 0.36483(13) 0.65263(8) 0.0350(4) Uani 1 1 d . . . . .
H62 H 0.1970 0.4137 0.6476 0.042 Uiso 1 1 calc R . . . .
C63 C 0.29148(10) 0.39357(15) 0.68127(9) 0.0433(4) Uani 1 1 d . . . . .
H63 H 0.3019 0.4609 0.6952 0.052 Uiso 1 1 calc R . . . .
C64 C 0.33874(9) 0.32477(16) 0.68952(9) 0.0444(4) Uani 1 1 d . . . . .
H64 H 0.3818 0.3440 0.7096 0.053 Uiso 1 1 calc R . . . .
C65 C 0.32263(9) 0.22704(16) 0.66814(9) 0.0408(4) Uani 1 1 d . . . . .
H65 H 0.3547 0.1788 0.6733 0.049 Uiso 1 1 calc R . . . .
C66 C 0.25945(8) 0.19987(14) 0.63906(8) 0.0337(3) Uani 1 1 d . . . . .
H66 H 0.2495 0.1330 0.6241 0.040 Uiso 1 1 calc R . . . .
C67 C 0.07002(8) 0.06130(12) 0.57896(7) 0.0300(3) Uani 1 1 d . . . . .
H67 H 0.0420 0.0887 0.5413 0.036 Uiso 1 1 calc R . . . .
C68 C 0.05533(9) -0.03140(13) 0.59667(8) 0.0378(4) Uani 1 1 d . . . . .
H68 H 0.0178 -0.0656 0.5713 0.045 Uiso 1 1 calc R . . . .
C69 C 0.09520(10) -0.07403(14) 0.65118(9) 0.0431(4) Uani 1 1 d . . . . .
H69 H 0.0852 -0.1372 0.6636 0.052 Uiso 1 1 calc R . . . .
C70 C 0.14980(9) -0.02320(14) 0.68726(8) 0.0418(4) Uani 1 1 d . . . . .
H70 H 0.1778 -0.0514 0.7247 0.050 Uiso 1 1 calc R . . . .
C71 C 0.16359(8) 0.06916(13) 0.66855(7) 0.0334(3) Uani 1 1 d . . . . .
H71 H 0.2016 0.1022 0.6938 0.040 Uiso 1 1 calc R . . . .
C72 C 0.12431(8) 0.11620(12) 0.61420(7) 0.0267(3) Uani 1 1 d . . . . .
C73 C 0.09382(8) 0.30768(13) 0.62032(8) 0.0345(4) Uani 1 1 d . . . . .
C74 C 0.07887(9) 0.28234(17) 0.66846(9) 0.0431(4) Uani 1 1 d . . . . .
H74 H 0.0878 0.2159 0.6845 0.052 Uiso 1 1 calc R . . . .
C75 C 0.05119(10) 0.3509(2) 0.69409(11) 0.0628(7) Uani 1 1 d . . . . .
H75 H 0.0427 0.3314 0.7276 0.075 Uiso 1 1 calc R . . . .
C76 C 0.03631(11) 0.4474(2) 0.67030(14) 0.0722(9) Uani 1 1 d . . . . .
H76 H 0.0178 0.4947 0.6875 0.087 Uiso 1 1 calc R . . . .
C77 C 0.04850(11) 0.47384(18) 0.62191(15) 0.0674(8) Uani 1 1 d . . . . .
H77 H 0.0378 0.5395 0.6050 0.081 Uiso 1 1 calc R . . . .
C78 C 0.07648(9) 0.40528(15) 0.59723(11) 0.0490(5) Uani 1 1 d . . . . .
H78 H 0.0841 0.4254 0.5634 0.059 Uiso 1 1 calc R . . . .
B2 B 0.13529(9) 0.23273(14) 0.59652(8) 0.0279(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.0131(13) . ?
Fe1 N2 1.9028(13) . ?
Fe1 N3 2.0253(13) . ?
Fe1 N4 2.0216(13) . ?
Fe1 N5 1.9049(12) . ?
Fe1 N6 2.0163(13) . ?
O1 C4 1.470(2) . ?
O1 C5 1.3243(19) . ?
O2 C11 1.328(2) . ?
O2 C12 1.451(3) . ?
O3 C19 1.468(3) . ?
O3 C20 1.334(2) . ?
O4 C26 1.3293(19) . ?
O4 C27 1.472(2) . ?
N1 C3 1.5049(19) . ?
N1 C5 1.284(2) . ?
N2 C6 1.348(2) . ?
N2 C10 1.344(2) . ?
N3 C11 1.285(2) . ?
N3 C13 1.499(2) . ?
N4 C18 1.497(2) . ?
N4 C20 1.284(2) . ?
N5 C21 1.343(2) . ?
N5 C25 1.346(2) . ?
N6 C26 1.284(2) . ?
N6 C28 1.5009(19) . ?
C1 C3 1.515(2) . ?
C2 C3 1.516(2) . ?
C3 C4 1.536(2) . ?
C5 C6 1.462(2) . ?
C6 C7 1.384(2) . ?
C7 C8 1.392(3) . ?
C8 C9 1.387(3) . ?
C9 C10 1.384(2) . ?
C10 C11 1.455(2) . ?
C12 C13 1.540(3) . ?
C13 C14 1.506(3) . ?
C13 C15 1.500(3) . ?
C16 C18 1.513(3) . ?
C17 C18 1.516(3) . ?
C18 C19 1.534(3) . ?
C20 C21 1.453(2) . ?
C21 C22 1.387(2) . ?
C22 C23 1.390(3) . ?
C23 C24 1.391(3) . ?
C24 C25 1.388(2) . ?
C25 C26 1.459(2) . ?
C27 C28 1.542(2) . ?
C28 C29 1.525(2) . ?
C28 C30 1.522(2) . ?
C31 C32 1.403(2) . ?
C31 C36 1.403(2) . ?
C31 B1 1.643(2) . ?
C32 C33 1.388(3) . ?
C33 C34 1.383(3) . ?
C34 C35 1.382(3) . ?
C35 C36 1.389(3) . ?
C37 C38 1.410(3) . ?
C37 C42 1.402(3) . ?
C37 B1 1.654(2) . ?
C38 C39 1.399(3) . ?
C39 C40 1.378(3) . ?
C40 C41 1.386(3) . ?
C41 C42 1.395(3) . ?
C43 C44 1.400(2) . ?
C43 C48 1.404(3) . ?
C43 B1 1.663(2) . ?
C44 C45 1.391(3) . ?
C45 C46 1.376(3) . ?
C46 C47 1.387(3) . ?
C47 C48 1.385(3) . ?
C49 C50 1.400(2) . ?
C49 C54 1.408(2) . ?
C49 B1 1.646(2) . ?
C50 C51 1.397(2) . ?
C51 C52 1.382(3) . ?
C52 C53 1.381(3) . ?
C53 C54 1.389(2) . ?
C55 C56 1.403(3) . ?
C55 C60 1.410(3) . ?
C55 B2 1.648(2) . ?
C56 C57 1.399(3) . ?
C57 C58 1.382(3) . ?
C58 C59 1.382(3) . ?
C59 C60 1.394(3) . ?
C61 C62 1.408(2) . ?
C61 C66 1.402(2) . ?
C61 B2 1.645(2) . ?
C62 C63 1.389(3) . ?
C63 C64 1.379(3) . ?
C64 C65 1.388(3) . ?
C65 C66 1.391(3) . ?
C67 C68 1.390(2) . ?
C67 C72 1.402(2) . ?
C68 C69 1.385(3) . ?
C69 C70 1.385(3) . ?
C70 C71 1.388(3) . ?
C71 C72 1.404(2) . ?
C72 B2 1.650(2) . ?
C73 C74 1.393(3) . ?
C73 C78 1.401(3) . ?
C73 B2 1.648(2) . ?
C74 C75 1.401(3) . ?
C75 C76 1.386(4) . ?
C76 C77 1.365(4) . ?
C77 C78 1.390(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N3 159.23(5) . . ?
N1 Fe1 N4 90.20(5) . . ?
N1 Fe1 N6 91.91(5) . . ?
N2 Fe1 N1 79.69(5) . . ?
N2 Fe1 N3 79.59(5) . . ?
N2 Fe1 N4 99.65(5) . . ?
N2 Fe1 N5 179.14(6) . . ?
N2 Fe1 N6 101.03(5) . . ?
N4 Fe1 N3 91.90(5) . . ?
N5 Fe1 N1 99.92(5) . . ?
N5 Fe1 N3 100.78(5) . . ?
N5 Fe1 N4 79.58(5) . . ?
N5 Fe1 N6 79.74(5) . . ?
N6 Fe1 N3 93.39(5) . . ?
N6 Fe1 N4 159.26(5) . . ?
C5 O1 C4 104.26(13) . . ?
C11 O2 C12 104.75(14) . . ?
C20 O3 C19 104.84(14) . . ?
C26 O4 C27 104.15(12) . . ?
C3 N1 Fe1 140.47(10) . . ?
C5 N1 Fe1 112.80(10) . . ?
C5 N1 C3 106.73(13) . . ?
C6 N2 Fe1 120.30(11) . . ?
C10 N2 Fe1 120.20(11) . . ?
C10 N2 C6 119.45(13) . . ?
C11 N3 Fe1 112.40(11) . . ?
C11 N3 C13 107.22(13) . . ?
C13 N3 Fe1 140.35(11) . . ?
C18 N4 Fe1 139.56(11) . . ?
C20 N4 Fe1 112.51(11) . . ?
C20 N4 C18 107.87(14) . . ?
C21 N5 Fe1 120.02(11) . . ?
C21 N5 C25 119.93(13) . . ?
C25 N5 Fe1 120.01(10) . . ?
C26 N6 Fe1 112.68(10) . . ?
C26 N6 C28 106.77(12) . . ?
C28 N6 Fe1 140.51(10) . . ?
N1 C3 C1 112.38(13) . . ?
N1 C3 C2 108.80(13) . . ?
N1 C3 C4 100.83(13) . . ?
C1 C3 C2 110.88(15) . . ?
C1 C3 C4 111.93(15) . . ?
C2 C3 C4 111.63(15) . . ?
O1 C4 C3 105.01(13) . . ?
O1 C5 C6 121.63(14) . . ?
N1 C5 O1 119.35(15) . . ?
N1 C5 C6 119.00(14) . . ?
N2 C6 C5 108.17(13) . . ?
N2 C6 C7 122.17(15) . . ?
C7 C6 C5 129.62(15) . . ?
C6 C7 C8 117.81(16) . . ?
C9 C8 C7 120.37(16) . . ?
C10 C9 C8 118.27(17) . . ?
N2 C10 C9 121.92(16) . . ?
N2 C10 C11 108.75(13) . . ?
C9 C10 C11 129.30(16) . . ?
O2 C11 C10 121.61(14) . . ?
N3 C11 O2 119.30(15) . . ?
N3 C11 C10 119.06(14) . . ?
O2 C12 C13 106.39(15) . . ?
N3 C13 C12 101.16(14) . . ?
N3 C13 C14 111.40(15) . . ?
N3 C13 C15 110.22(15) . . ?
C14 C13 C12 110.68(19) . . ?
C15 C13 C12 111.4(2) . . ?
C15 C13 C14 111.55(19) . . ?
N4 C18 C16 110.73(16) . . ?
N4 C18 C17 110.03(14) . . ?
N4 C18 C19 101.68(14) . . ?
C16 C18 C17 111.11(19) . . ?
C16 C18 C19 111.61(19) . . ?
C17 C18 C19 111.33(19) . . ?
O3 C19 C18 106.30(15) . . ?
O3 C20 C21 122.05(15) . . ?
N4 C20 O3 118.92(15) . . ?
N4 C20 C21 119.02(14) . . ?
N5 C21 C20 108.87(14) . . ?
N5 C21 C22 121.64(15) . . ?
C22 C21 C20 129.47(15) . . ?
C21 C22 C23 118.41(16) . . ?
C22 C23 C24 120.11(16) . . ?
C25 C24 C23 118.09(16) . . ?
N5 C25 C24 121.79(15) . . ?
N5 C25 C26 108.57(13) . . ?
C24 C25 C26 129.61(15) . . ?
O4 C26 C25 121.58(13) . . ?
N6 C26 O4 119.42(14) . . ?
N6 C26 C25 118.99(14) . . ?
O4 C27 C28 104.69(12) . . ?
N6 C28 C27 101.15(12) . . ?
N6 C28 C29 109.15(13) . . ?
N6 C28 C30 111.77(13) . . ?
C29 C28 C27 111.65(14) . . ?
C30 C28 C27 111.84(14) . . ?
C30 C28 C29 110.90(14) . . ?
C32 C31 B1 122.44(15) . . ?
C36 C31 C32 115.15(15) . . ?
C36 C31 B1 121.94(14) . . ?
C33 C32 C31 122.41(17) . . ?
C34 C33 C32 120.64(17) . . ?
C35 C34 C33 118.81(17) . . ?
C34 C35 C36 120.06(18) . . ?
C35 C36 C31 122.93(16) . . ?
C38 C37 B1 122.63(15) . . ?
C42 C37 C38 114.64(16) . . ?
C42 C37 B1 122.73(15) . . ?
C39 C38 C37 122.97(18) . . ?
C40 C39 C38 120.06(19) . . ?
C39 C40 C41 119.07(18) . . ?
C40 C41 C42 120.26(19) . . ?
C41 C42 C37 122.97(18) . . ?
C44 C43 C48 114.20(16) . . ?
C44 C43 B1 123.03(15) . . ?
C48 C43 B1 122.71(15) . . ?
C45 C44 C43 123.40(18) . . ?
C46 C45 C44 120.23(19) . . ?
C45 C46 C47 118.58(18) . . ?
C48 C47 C46 120.3(2) . . ?
C47 C48 C43 123.26(18) . . ?
C50 C49 C54 114.92(15) . . ?
C50 C49 B1 123.46(15) . . ?
C54 C49 B1 121.56(15) . . ?
C51 C50 C49 122.90(17) . . ?
C52 C51 C50 119.98(17) . . ?
C53 C52 C51 119.11(16) . . ?
C52 C53 C54 120.27(19) . . ?
C53 C54 C49 122.76(17) . . ?
C31 B1 C37 106.38(13) . . ?
C31 B1 C43 108.99(12) . . ?
C31 B1 C49 110.71(13) . . ?
C37 B1 C43 111.27(13) . . ?
C49 B1 C37 110.94(13) . . ?
C49 B1 C43 108.54(13) . . ?
C56 C55 C60 114.77(16) . . ?
C56 C55 B2 123.09(16) . . ?
C60 C55 B2 122.03(15) . . ?
C57 C56 C55 122.67(19) . . ?
C58 C57 C56 120.40(19) . . ?
C59 C58 C57 119.01(18) . . ?
C58 C59 C60 120.1(2) . . ?
C59 C60 C55 123.04(19) . . ?
C62 C61 B2 122.77(15) . . ?
C66 C61 C62 114.69(16) . . ?
C66 C61 B2 122.52(14) . . ?
C63 C62 C61 122.86(18) . . ?
C64 C63 C62 120.30(18) . . ?
C63 C64 C65 119.10(18) . . ?
C64 C65 C66 119.80(18) . . ?
C65 C66 C61 123.22(17) . . ?
C68 C67 C72 122.99(16) . . ?
C69 C68 C67 120.19(16) . . ?
C70 C69 C68 118.95(17) . . ?
C69 C70 C71 119.84(17) . . ?
C70 C71 C72 123.39(16) . . ?
C67 C72 C71 114.62(15) . . ?
C67 C72 B2 121.60(14) . . ?
C71 C72 B2 123.32(14) . . ?
C74 C73 C78 115.34(18) . . ?
C74 C73 B2 122.44(16) . . ?
C78 C73 B2 121.94(17) . . ?
C73 C74 C75 122.6(2) . . ?
C76 C75 C74 119.6(2) . . ?
C77 C76 C75 119.4(2) . . ?
C76 C77 C78 120.4(2) . . ?
C77 C78 C73 122.6(2) . . ?
C55 B2 C72 108.82(12) . . ?
C55 B2 C73 112.29(14) . . ?
C61 B2 C55 109.16(13) . . ?
C61 B2 C72 111.49(13) . . ?
C61 B2 C73 107.91(13) . . ?
C73 B2 C72 107.18(13) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-2
_database_code_depnum_ccdc_archive 'CCDC 1468984'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;

_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000 -0.126  0.250        67         3
   2  0.000  0.126  0.750        67         3
   3  0.500  0.056  0.250       209        41
   4  0.500 -0.056  0.750       209        41
   5  0.017  0.458  0.508         7         0
   6  0.983  0.458  0.992         6         0
   7  0.022  0.556  0.011         5         0
   8  0.978  0.556  0.489         5         0
;
_platon_squeeze_details          
;
The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 88e per unit cell, which are accumulated which corresponds 
to 22e per formula(C78H78B2FeN6O4). The 22e might come from one 
ether molecule and are not included in the formula.
;

_audit_creation_date             2016-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            4-2
_chemical_name_systematic        4-2
_chemical_formula_moiety         'C30 H38 Fe N6 O4, 2(C24 H20 B)'
_chemical_formula_sum            'C78 H78 B2 Fe N6 O4'
_chemical_formula_weight         1240.93
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   23.401(2)
_cell_length_b                   13.5170(13)
_cell_length_c                   24.582(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.6560(10)
_cell_angle_gamma                90
_cell_volume                     7122.2(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8576
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      52.044
_cell_measurement_theta_min      1.9
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0664 before and 0.0427 after correction.
The Ratio of minimum to maximum transmission is 0.9131.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53558
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         0.950
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8448
_reflns_number_total             13913
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     828
_refine_ls_number_reflns         13913
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0624P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1274
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C12(H12A,H12B), C19(H19A,H19B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25263(2) 0.24831(2) 0.48859(2) 0.03958(10) Uani 1 1 d . . . . .
O1 O 0.39953(7) 0.40163(12) 0.46658(7) 0.0605(4) Uani 1 1 d . . . . .
O2 O 0.11805(10) 0.13639(18) 0.32700(9) 0.1068(7) Uani 1 1 d . . . . .
O3 O 0.14429(8) 0.45563(12) 0.53449(8) 0.0723(5) Uani 1 1 d . . . . .
O4 O 0.31998(10) 0.01499(12) 0.61233(7) 0.0812(6) Uani 1 1 d . . . . .
N1 N 0.33866(8) 0.33415(12) 0.50793(7) 0.0424(4) Uani 1 1 d . . . . .
N2 N 0.26087(8) 0.25927(12) 0.40725(7) 0.0434(4) Uani 1 1 d . . . . .
N3 N 0.16957(8) 0.17186(13) 0.42399(9) 0.0528(5) Uani 1 1 d . . . . .
N4 N 0.19665(8) 0.37972(12) 0.48680(8) 0.0467(4) Uani 1 1 d . . . . .
N5 N 0.23973(8) 0.24208(12) 0.56785(8) 0.0438(4) Uani 1 1 d . . . . .
N6 N 0.30034(8) 0.11219(12) 0.53276(8) 0.0481(5) Uani 1 1 d . . . . .
C1 C 0.43126(11) 0.30015(18) 0.59871(11) 0.0652(7) Uani 1 1 d . . . . .
H1A H 0.4066 0.2599 0.6132 0.098 Uiso 1 1 calc GR . . . .
H1B H 0.4649 0.3296 0.6316 0.098 Uiso 1 1 calc GR . . . .
H1C H 0.4479 0.2599 0.5764 0.098 Uiso 1 1 calc GR . . . .
C2 C 0.36476(13) 0.44802(19) 0.59345(11) 0.0713(8) Uani 1 1 d . . . . .
H2A H 0.3385 0.4975 0.5673 0.107 Uiso 1 1 calc GR . . . .
H2B H 0.3986 0.4795 0.6252 0.107 Uiso 1 1 calc GR . . . .
H2C H 0.3409 0.4093 0.6095 0.107 Uiso 1 1 calc GR . . . .
C3 C 0.39065(10) 0.38112(16) 0.55898(9) 0.0498(6) Uani 1 1 d . . . . .
C4 C 0.42488(12) 0.43968(18) 0.52743(11) 0.0665(7) Uani 1 1 d . . . . .
H4A H 0.4168 0.5100 0.5279 0.080 Uiso 1 1 calc R . . . .
H4B H 0.4695 0.4286 0.5465 0.080 Uiso 1 1 calc R . . . .
C5 C 0.34942(10) 0.34896(15) 0.46184(9) 0.0431(5) Uani 1 1 d . . . . .
C6 C 0.30791(10) 0.31072(16) 0.40349(9) 0.0466(5) Uani 1 1 d . . . . .
C7 C 0.31220(13) 0.3276(2) 0.34997(11) 0.0700(7) Uani 1 1 d . . . . .
H7 H 0.3450 0.3643 0.3480 0.084 Uiso 1 1 calc R . . . .
C8 C 0.26662(16) 0.2888(3) 0.29953(12) 0.0915(10) Uani 1 1 d . . . . .
H8 H 0.2690 0.2970 0.2629 0.110 Uiso 1 1 calc R . . . .
C9 C 0.21751(14) 0.2376(2) 0.30333(12) 0.0840(9) Uani 1 1 d . . . . .
H9 H 0.1856 0.2131 0.2693 0.101 Uiso 1 1 calc R . . . .
C10 C 0.21627(11) 0.22341(18) 0.35810(10) 0.0561(6) Uani 1 1 d . . . . .
C11 C 0.16740(11) 0.17477(19) 0.37174(12) 0.0623(7) Uani 1 1 d . . . . .
C12 C 0.07737(19) 0.1001(4) 0.35432(19) 0.1497(18) Uani 1 1 d . . . . .
H12A H 0.0702 0.0297 0.3474 0.180 Uiso 1 1 calc R . . . .
H12B H 0.0374 0.1339 0.3379 0.180 Uiso 1 1 calc R . . . .
C13 C 0.11061(13) 0.1213(2) 0.42049(14) 0.0737(8) Uani 1 1 d . . . . .
C14 C 0.12715(16) 0.0305(3) 0.4587(2) 0.1465(18) Uani 1 1 d . . . . .
H14A H 0.1530 -0.0119 0.4468 0.220 Uiso 1 1 calc GR . . . .
H14B H 0.0897 -0.0040 0.4543 0.220 Uiso 1 1 calc GR . . . .
H14C H 0.1494 0.0493 0.4995 0.220 Uiso 1 1 calc GR . . . .
C15 C 0.07367(14) 0.1907(2) 0.44170(17) 0.1078(12) Uani 1 1 d . . . . .
H15A H 0.0970 0.2054 0.4830 0.162 Uiso 1 1 calc GR . . . .
H15B H 0.0348 0.1602 0.4366 0.162 Uiso 1 1 calc GR . . . .
H15C H 0.0657 0.2509 0.4191 0.162 Uiso 1 1 calc GR . . . .
C16 C 0.21755(14) 0.5404(2) 0.45283(16) 0.1018(11) Uani 1 1 d . . . . .
H16A H 0.2375 0.5640 0.4929 0.153 Uiso 1 1 calc GR . . . .
H16B H 0.1996 0.5952 0.4267 0.153 Uiso 1 1 calc GR . . . .
H16C H 0.2478 0.5081 0.4417 0.153 Uiso 1 1 calc GR . . . .
C17 C 0.13113(15) 0.4375(2) 0.38453(13) 0.0916(10) Uani 1 1 d . . . . .
H17A H 0.1597 0.4118 0.3689 0.137 Uiso 1 1 calc GR . . . .
H17B H 0.1099 0.4940 0.3616 0.137 Uiso 1 1 calc GR . . . .
H17C H 0.1012 0.3875 0.3824 0.137 Uiso 1 1 calc GR . . . .
C18 C 0.16672(12) 0.46792(16) 0.44846(11) 0.0591(7) Uani 1 1 d . . . . .
C19 C 0.12252(15) 0.5052(2) 0.47604(14) 0.0877(9) Uani 1 1 d . . . . .
H19A H 0.1251 0.5765 0.4806 0.105 Uiso 1 1 calc R . . . .
H19B H 0.0797 0.4871 0.4516 0.105 Uiso 1 1 calc R . . . .
C20 C 0.18261(11) 0.38493(15) 0.53174(11) 0.0500(6) Uani 1 1 d . . . . .
C21 C 0.20705(11) 0.31303(15) 0.58080(10) 0.0488(6) Uani 1 1 d . . . . .
C22 C 0.19917(13) 0.31295(19) 0.63332(11) 0.0692(7) Uani 1 1 d . . . . .
H22 H 0.1765 0.3627 0.6418 0.083 Uiso 1 1 calc R . . . .
C23 C 0.22566(16) 0.2374(2) 0.67311(13) 0.0844(9) Uani 1 1 d . . . . .
H23 H 0.2217 0.2365 0.7093 0.101 Uiso 1 1 calc R . . . .
C24 C 0.25815(14) 0.1628(2) 0.65936(11) 0.0759(8) Uani 1 1 d . . . . .
H24 H 0.2753 0.1105 0.6854 0.091 Uiso 1 1 calc R . . . .
C25 C 0.26442(11) 0.16803(16) 0.60624(9) 0.0502(6) Uani 1 1 d . . . . .
C26 C 0.29641(11) 0.09765(15) 0.58208(10) 0.0527(6) Uani 1 1 d . . . . .
C27 C 0.34162(19) -0.0419(2) 0.57430(14) 0.1075(12) Uani 1 1 d . . . . .
H27A H 0.3171 -0.1018 0.5608 0.129 Uiso 1 1 calc R . . . .
H27B H 0.3851 -0.0602 0.5955 0.129 Uiso 1 1 calc R . . . .
C28 C 0.33369(12) 0.02503(17) 0.52161(11) 0.0596(7) Uani 1 1 d . . . . .
C29 C 0.39587(15) 0.0581(2) 0.52322(18) 0.1136(13) Uani 1 1 d . . . . .
H29A H 0.3894 0.1066 0.4928 0.170 Uiso 1 1 calc GR . . . .
H29B H 0.4176 0.0022 0.5166 0.170 Uiso 1 1 calc GR . . . .
H29C H 0.4202 0.0866 0.5613 0.170 Uiso 1 1 calc GR . . . .
C30 C 0.29473(14) -0.0207(2) 0.46280(13) 0.0885(9) Uani 1 1 d . . . . .
H30A H 0.2554 -0.0413 0.4627 0.133 Uiso 1 1 calc GR . . . .
H30B H 0.3161 -0.0771 0.4562 0.133 Uiso 1 1 calc GR . . . .
H30C H 0.2877 0.0269 0.4318 0.133 Uiso 1 1 calc GR . . . .
C31 C 0.12193(10) -0.11554(15) 0.61867(10) 0.0469(5) Uani 1 1 d . . . . .
C32 C 0.07530(11) -0.05456(17) 0.57970(10) 0.0562(6) Uani 1 1 d . . . . .
H32 H 0.0521 -0.0774 0.5414 0.067 Uiso 1 1 calc R . . . .
C33 C 0.06187(13) 0.03834(19) 0.59528(12) 0.0733(8) Uani 1 1 d . . . . .
H33 H 0.0300 0.0758 0.5677 0.088 Uiso 1 1 calc R . . . .
C34 C 0.09507(14) 0.0754(2) 0.65080(14) 0.0828(9) Uani 1 1 d . . . . .
H34 H 0.0857 0.1374 0.6614 0.099 Uiso 1 1 calc R . . . .
C35 C 0.14241(14) 0.01976(19) 0.69059(12) 0.0794(8) Uani 1 1 d . . . . .
H35 H 0.1655 0.0438 0.7286 0.095 Uiso 1 1 calc R . . . .
C36 C 0.15560(12) -0.07242(18) 0.67394(11) 0.0658(7) Uani 1 1 d . . . . .
H36 H 0.1889 -0.1077 0.7012 0.079 Uiso 1 1 calc R . . . .
C37 C 0.10701(12) -0.24310(15) 0.53069(10) 0.0543(6) Uani 1 1 d . . . . .
C38 C 0.14631(14) -0.22547(16) 0.50106(11) 0.0649(7) Uani 1 1 d . . . . .
H38 H 0.1878 -0.2092 0.5235 0.078 Uiso 1 1 calc R . . . .
C39 C 0.1262(2) -0.23121(19) 0.44028(14) 0.0872(10) Uani 1 1 d . . . . .
H39 H 0.1541 -0.2190 0.4227 0.105 Uiso 1 1 calc R . . . .
C40 C 0.0658(2) -0.2546(2) 0.40565(14) 0.1002(13) Uani 1 1 d . . . . .
H40 H 0.0523 -0.2591 0.3646 0.120 Uiso 1 1 calc R . . . .
C41 C 0.02520(17) -0.2714(2) 0.43198(14) 0.0905(11) Uani 1 1 d . . . . .
H41 H -0.0163 -0.2864 0.4087 0.109 Uiso 1 1 calc R . . . .
C42 C 0.04589(13) -0.26605(18) 0.49410(12) 0.0695(8) Uani 1 1 d . . . . .
H42 H 0.0176 -0.2783 0.5112 0.083 Uiso 1 1 calc R . . . .
C43 C 0.09245(10) -0.30317(17) 0.63051(11) 0.0521(6) Uani 1 1 d . . . . .
C44 C 0.07598(12) -0.39969(18) 0.61143(14) 0.0735(8) Uani 1 1 d . . . . .
H44 H 0.0823 -0.4218 0.5784 0.088 Uiso 1 1 calc R . . . .
C45 C 0.05040(14) -0.4651(2) 0.63959(19) 0.0998(11) Uani 1 1 d . . . . .
H45 H 0.0403 -0.5293 0.6254 0.120 Uiso 1 1 calc R . . . .
C46 C 0.04031(16) -0.4350(3) 0.6877(2) 0.1099(13) Uani 1 1 d . . . . .
H46 H 0.0246 -0.4790 0.7073 0.132 Uiso 1 1 calc R . . . .
C47 C 0.05338(14) -0.3400(3) 0.70684(14) 0.0932(10) Uani 1 1 d . . . . .
H47 H 0.0454 -0.3182 0.7390 0.112 Uiso 1 1 calc R . . . .
C48 C 0.07860(11) -0.2756(2) 0.67839(11) 0.0639(7) Uani 1 1 d . . . . .
H48 H 0.0867 -0.2108 0.6920 0.077 Uiso 1 1 calc R . . . .
C49 C 0.20564(11) -0.26528(16) 0.63427(9) 0.0487(6) Uani 1 1 d . . . . .
C50 C 0.22388(12) -0.36374(17) 0.64741(10) 0.0583(6) Uani 1 1 d . . . . .
H50 H 0.1930 -0.4115 0.6395 0.070 Uiso 1 1 calc R . . . .
C51 C 0.28548(14) -0.3939(2) 0.67162(12) 0.0729(8) Uani 1 1 d . . . . .
H51 H 0.2950 -0.4606 0.6793 0.087 Uiso 1 1 calc R . . . .
C52 C 0.33229(14) -0.3267(2) 0.68426(12) 0.0763(8) Uani 1 1 d . . . . .
H52 H 0.3737 -0.3469 0.7010 0.092 Uiso 1 1 calc R . . . .
C53 C 0.31766(13) -0.2287(2) 0.67199(13) 0.0784(8) Uani 1 1 d . . . . .
H53 H 0.3492 -0.1819 0.6802 0.094 Uiso 1 1 calc R . . . .
C54 C 0.25523(12) -0.1996(2) 0.64709(11) 0.0667(7) Uani 1 1 d . . . . .
H54 H 0.2462 -0.1329 0.6386 0.080 Uiso 1 1 calc R . . . .
B1 B 0.13173(13) -0.23159(18) 0.60317(11) 0.0475(6) Uani 1 1 d . . . . .
C55 C 0.37335(12) 0.27273(15) 0.94272(10) 0.0508(6) Uani 1 1 d . . . . .
C56 C 0.33384(13) 0.28172(16) 0.97232(11) 0.0561(6) Uani 1 1 d . . . . .
H56 H 0.2910 0.2819 0.9499 0.067 Uiso 1 1 calc R . . . .
C57 C 0.35514(16) 0.29038(17) 1.03330(12) 0.0667(7) Uani 1 1 d . . . . .
H57 H 0.3267 0.2970 1.0508 0.080 Uiso 1 1 calc R . . . .
C58 C 0.41776(18) 0.28926(19) 1.06805(12) 0.0777(9) Uani 1 1 d . . . . .
H58 H 0.4321 0.2930 1.1092 0.093 Uiso 1 1 calc R . . . .
C59 C 0.45900(15) 0.2826(2) 1.04155(12) 0.0772(8) Uani 1 1 d . . . . .
H59 H 0.5017 0.2828 1.0646 0.093 Uiso 1 1 calc R . . . .
C60 C 0.43705(13) 0.27563(18) 0.98008(11) 0.0660(7) Uani 1 1 d . . . . .
H60 H 0.4659 0.2727 0.9629 0.079 Uiso 1 1 calc R . . . .
C61 C 0.38799(10) 0.32723(17) 0.84314(9) 0.0485(5) Uani 1 1 d . . . . .
C62 C 0.39663(11) 0.3028(2) 0.79198(10) 0.0627(7) Uani 1 1 d . . . . .
H62 H 0.3846 0.2403 0.7755 0.075 Uiso 1 1 calc R . . . .
C63 C 0.42252(13) 0.3681(2) 0.76459(12) 0.0768(8) Uani 1 1 d . . . . .
H63 H 0.4275 0.3487 0.7304 0.092 Uiso 1 1 calc R . . . .
C64 C 0.44080(13) 0.4608(2) 0.78748(14) 0.0786(9) Uani 1 1 d . . . . .
H64 H 0.4573 0.5050 0.7686 0.094 Uiso 1 1 calc R . . . .
C65 C 0.43441(12) 0.48773(19) 0.83882(13) 0.0709(7) Uani 1 1 d . . . . .
H65 H 0.4475 0.5498 0.8555 0.085 Uiso 1 1 calc R . . . .
C66 C 0.40828(11) 0.42125(17) 0.86527(11) 0.0565(6) Uani 1 1 d . . . . .
H66 H 0.4041 0.4407 0.8998 0.068 Uiso 1 1 calc R . . . .
C67 C 0.27465(12) 0.28564(19) 0.83654(10) 0.0564(6) Uani 1 1 d . . . . .
C68 C 0.25435(13) 0.3751(2) 0.80624(12) 0.0706(7) Uani 1 1 d . . . . .
H68 H 0.2843 0.4197 0.8055 0.085 Uiso 1 1 calc R . . . .
C69 C 0.19189(15) 0.4010(3) 0.77719(13) 0.0859(9) Uani 1 1 d . . . . .
H69 H 0.1810 0.4620 0.7583 0.103 Uiso 1 1 calc R . . . .
C70 C 0.14685(16) 0.3370(3) 0.77647(14) 0.0961(11) Uani 1 1 d . . . . .
H70 H 0.1050 0.3533 0.7563 0.115 Uiso 1 1 calc R . . . .
C71 C 0.16354(15) 0.2478(3) 0.80584(14) 0.0919(10) Uani 1 1 d . . . . .
H71 H 0.1330 0.2039 0.8059 0.110 Uiso 1 1 calc R . . . .
C72 C 0.22620(13) 0.2240(2) 0.83536(11) 0.0722(8) Uani 1 1 d . . . . .
H72 H 0.2365 0.1639 0.8554 0.087 Uiso 1 1 calc R . . . .
C73 C 0.36090(12) 0.13775(17) 0.85832(11) 0.0566(6) Uani 1 1 d . . . . .
C74 C 0.31990(14) 0.08235(19) 0.81194(12) 0.0761(8) Uani 1 1 d . . . . .
H74 H 0.2828 0.1120 0.7868 0.091 Uiso 1 1 calc R . . . .
C75 C 0.33057(18) -0.0153(2) 0.80045(14) 0.0980(11) Uani 1 1 d . . . . .
H75 H 0.3011 -0.0483 0.7682 0.118 Uiso 1 1 calc R . . . .
C76 C 0.38333(18) -0.0623(2) 0.83575(17) 0.0972(10) Uani 1 1 d . . . . .
H76 H 0.3908 -0.1273 0.8281 0.117 Uiso 1 1 calc R . . . .
C77 C 0.42593(16) -0.0116(2) 0.88353(17) 0.1007(11) Uani 1 1 d . . . . .
H77 H 0.4623 -0.0427 0.9088 0.121 Uiso 1 1 calc R . . . .
C78 C 0.41451(13) 0.0858(2) 0.89387(14) 0.0825(9) Uani 1 1 d . . . . .
H78 H 0.4442 0.1182 0.9263 0.099 Uiso 1 1 calc R . . . .
B2 B 0.34927(13) 0.2552(2) 0.87057(12) 0.0514(7) 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 N1 2.2039(17) . ?
Fe1 N2 2.0895(17) . ?
Fe1 N3 2.2114(19) . ?
Fe1 N4 2.1971(16) . ?
Fe1 N5 2.0898(17) . ?
Fe1 N6 2.1995(17) . ?
O1 C4 1.463(3) . ?
O1 C5 1.336(2) . ?
O2 C11 1.339(3) . ?
O2 C12 1.453(4) . ?
O3 C19 1.478(3) . ?
O3 C20 1.330(2) . ?
O4 C26 1.333(2) . ?
O4 C27 1.450(3) . ?
N1 C3 1.494(3) . ?
N1 C5 1.271(2) . ?
N2 C6 1.336(3) . ?
N2 C10 1.331(3) . ?
N3 C11 1.266(3) . ?
N3 C13 1.511(3) . ?
N4 C18 1.507(3) . ?
N4 C20 1.275(3) . ?
N5 C21 1.342(3) . ?
N5 C25 1.337(3) . ?
N6 C26 1.267(3) . ?
N6 C28 1.498(3) . ?
C1 C3 1.520(3) . ?
C2 C3 1.521(3) . ?
C3 C4 1.539(3) . ?
C5 C6 1.466(3) . ?
C6 C7 1.378(3) . ?
C7 C8 1.375(4) . ?
C8 C9 1.376(4) . ?
C9 C10 1.372(3) . ?
C10 C11 1.470(3) . ?
C12 C13 1.523(5) . ?
C13 C14 1.499(4) . ?
C13 C15 1.503(4) . ?
C16 C18 1.511(3) . ?
C17 C18 1.511(4) . ?
C18 C19 1.532(4) . ?
C20 C21 1.474(3) . ?
C21 C22 1.375(3) . ?
C22 C23 1.377(4) . ?
C23 C24 1.384(4) . ?
C24 C25 1.373(3) . ?
C25 C26 1.475(3) . ?
C27 C28 1.529(4) . ?
C28 C29 1.507(4) . ?
C28 C30 1.499(3) . ?
C31 C32 1.396(3) . ?
C31 C36 1.396(3) . ?
C31 B1 1.652(3) . ?
C32 C33 1.385(3) . ?
C33 C34 1.366(4) . ?
C34 C35 1.371(4) . ?
C35 C36 1.384(3) . ?
C37 C38 1.404(3) . ?
C37 C42 1.385(3) . ?
C37 B1 1.645(3) . ?
C38 C39 1.377(4) . ?
C39 C40 1.364(5) . ?
C40 C41 1.366(5) . ?
C41 C42 1.406(4) . ?
C43 C44 1.388(3) . ?
C43 C48 1.391(3) . ?
C43 B1 1.652(4) . ?
C44 C45 1.398(4) . ?
C45 C46 1.357(5) . ?
C46 C47 1.361(5) . ?
C47 C48 1.388(4) . ?
C49 C50 1.395(3) . ?
C49 C54 1.393(3) . ?
C49 B1 1.650(3) . ?
C50 C51 1.382(3) . ?
C51 C52 1.360(4) . ?
C52 C53 1.371(4) . ?
C53 C54 1.395(3) . ?
C55 C56 1.392(3) . ?
C55 C60 1.403(3) . ?
C55 B2 1.649(3) . ?
C56 C57 1.382(3) . ?
C57 C58 1.369(4) . ?
C58 C59 1.367(4) . ?
C59 C60 1.390(3) . ?
C61 C62 1.391(3) . ?
C61 C66 1.389(3) . ?
C61 B2 1.647(3) . ?
C62 C63 1.388(3) . ?
C63 C64 1.370(4) . ?
C64 C65 1.378(4) . ?
C65 C66 1.387(3) . ?
C67 C68 1.400(3) . ?
C67 C72 1.398(3) . ?
C67 B2 1.657(4) . ?
C68 C69 1.390(4) . ?
C69 C70 1.358(4) . ?
C70 C71 1.379(4) . ?
C71 C72 1.388(4) . ?
C73 C74 1.380(3) . ?
C73 C78 1.397(4) . ?
C73 B2 1.659(3) . ?
C74 C75 1.393(4) . ?
C75 C76 1.349(4) . ?
C76 C77 1.379(4) . ?
C77 C78 1.386(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N3 149.84(7) . . ?
N2 Fe1 N1 75.06(7) . . ?
N2 Fe1 N3 74.82(7) . . ?
N2 Fe1 N4 101.94(7) . . ?
N2 Fe1 N5 176.74(7) . . ?
N2 Fe1 N6 107.95(6) . . ?
N4 Fe1 N1 93.69(6) . . ?
N4 Fe1 N3 91.04(7) . . ?
N4 Fe1 N6 150.06(7) . . ?
N5 Fe1 N1 106.33(7) . . ?
N5 Fe1 N3 103.68(7) . . ?
N5 Fe1 N4 75.11(7) . . ?
N5 Fe1 N6 74.96(6) . . ?
N6 Fe1 N1 95.46(6) . . ?
N6 Fe1 N3 95.13(7) . . ?
C5 O1 C4 104.95(17) . . ?
C11 O2 C12 105.1(2) . . ?
C20 O3 C19 104.63(18) . . ?
C26 O4 C27 104.97(19) . . ?
C3 N1 Fe1 140.38(14) . . ?
C5 N1 Fe1 112.39(14) . . ?
C5 N1 C3 107.22(17) . . ?
C6 N2 Fe1 119.86(14) . . ?
C10 N2 Fe1 120.19(15) . . ?
C10 N2 C6 119.63(19) . . ?
C11 N3 Fe1 112.33(16) . . ?
C11 N3 C13 107.0(2) . . ?
C13 N3 Fe1 140.51(17) . . ?
C18 N4 Fe1 140.88(15) . . ?
C20 N4 Fe1 112.73(14) . . ?
C20 N4 C18 106.37(18) . . ?
C21 N5 Fe1 120.10(14) . . ?
C25 N5 Fe1 120.32(14) . . ?
C25 N5 C21 119.57(18) . . ?
C26 N6 Fe1 112.63(14) . . ?
C26 N6 C28 107.22(18) . . ?
C28 N6 Fe1 140.00(15) . . ?
N1 C3 C1 108.79(17) . . ?
N1 C3 C2 110.39(19) . . ?
N1 C3 C4 102.02(17) . . ?
C1 C3 C2 110.9(2) . . ?
C1 C3 C4 112.1(2) . . ?
C2 C3 C4 112.3(2) . . ?
O1 C4 C3 104.77(17) . . ?
O1 C5 C6 119.13(19) . . ?
N1 C5 O1 119.13(19) . . ?
N1 C5 C6 121.7(2) . . ?
N2 C6 C5 110.89(18) . . ?
N2 C6 C7 122.0(2) . . ?
C7 C6 C5 127.0(2) . . ?
C8 C7 C6 118.1(3) . . ?
C7 C8 C9 119.8(2) . . ?
C10 C9 C8 119.0(3) . . ?
N2 C10 C9 121.5(2) . . ?
N2 C10 C11 110.7(2) . . ?
C9 C10 C11 127.7(2) . . ?
O2 C11 C10 118.7(2) . . ?
N3 C11 O2 119.4(2) . . ?
N3 C11 C10 121.8(2) . . ?
O2 C12 C13 106.4(3) . . ?
N3 C13 C12 102.1(2) . . ?
C14 C13 N3 109.5(2) . . ?
C14 C13 C12 114.1(3) . . ?
C14 C13 C15 109.5(3) . . ?
C15 C13 N3 109.7(2) . . ?
C15 C13 C12 111.7(3) . . ?
N4 C18 C16 108.3(2) . . ?
N4 C18 C17 111.07(19) . . ?
N4 C18 C19 102.12(19) . . ?
C16 C18 C19 114.0(2) . . ?
C17 C18 C16 109.9(2) . . ?
C17 C18 C19 111.2(2) . . ?
O3 C19 C18 104.5(2) . . ?
O3 C20 C21 118.7(2) . . ?
N4 C20 O3 119.8(2) . . ?
N4 C20 C21 121.49(19) . . ?
N5 C21 C20 110.37(18) . . ?
N5 C21 C22 121.7(2) . . ?
C22 C21 C20 127.9(2) . . ?
C21 C22 C23 118.4(2) . . ?
C22 C23 C24 120.1(2) . . ?
C25 C24 C23 118.3(2) . . ?
N5 C25 C24 121.9(2) . . ?
N5 C25 C26 110.12(18) . . ?
C24 C25 C26 128.0(2) . . ?
O4 C26 C25 118.6(2) . . ?
N6 C26 O4 119.4(2) . . ?
N6 C26 C25 121.91(19) . . ?
O4 C27 C28 106.1(2) . . ?
N6 C28 C27 101.86(19) . . ?
N6 C28 C29 109.3(2) . . ?
N6 C28 C30 109.9(2) . . ?
C29 C28 C27 111.4(3) . . ?
C30 C28 C27 113.1(3) . . ?
C30 C28 C29 110.8(2) . . ?
C32 C31 B1 123.0(2) . . ?
C36 C31 C32 113.7(2) . . ?
C36 C31 B1 123.0(2) . . ?
C33 C32 C31 123.2(2) . . ?
C34 C33 C32 120.5(2) . . ?
C33 C34 C35 119.0(2) . . ?
C34 C35 C36 119.7(2) . . ?
C35 C36 C31 123.9(2) . . ?
C38 C37 B1 121.8(2) . . ?
C42 C37 C38 115.0(2) . . ?
C42 C37 B1 123.2(2) . . ?
C39 C38 C37 123.0(3) . . ?
C40 C39 C38 120.5(3) . . ?
C39 C40 C41 119.2(3) . . ?
C40 C41 C42 120.3(3) . . ?
C37 C42 C41 122.2(3) . . ?
C44 C43 C48 114.2(2) . . ?
C44 C43 B1 122.5(2) . . ?
C48 C43 B1 123.0(2) . . ?
C43 C44 C45 122.9(3) . . ?
C46 C45 C44 120.0(3) . . ?
C45 C46 C47 119.4(3) . . ?
C46 C47 C48 120.0(3) . . ?
C47 C48 C43 123.3(3) . . ?
C50 C49 B1 122.5(2) . . ?
C54 C49 C50 113.9(2) . . ?
C54 C49 B1 123.5(2) . . ?
C51 C50 C49 123.4(3) . . ?
C52 C51 C50 120.5(3) . . ?
C51 C52 C53 119.2(3) . . ?
C52 C53 C54 119.6(3) . . ?
C49 C54 C53 123.4(2) . . ?
C37 B1 C31 108.58(17) . . ?
C37 B1 C43 112.0(2) . . ?
C37 B1 C49 108.87(19) . . ?
C43 B1 C31 108.12(19) . . ?
C49 B1 C31 111.84(19) . . ?
C49 B1 C43 107.50(17) . . ?
C56 C55 C60 114.2(2) . . ?
C56 C55 B2 124.2(2) . . ?
C60 C55 B2 121.5(2) . . ?
C57 C56 C55 123.2(3) . . ?
C58 C57 C56 120.4(3) . . ?
C59 C58 C57 119.2(3) . . ?
C58 C59 C60 119.9(3) . . ?
C59 C60 C55 123.1(3) . . ?
C62 C61 B2 122.2(2) . . ?
C66 C61 C62 114.9(2) . . ?
C66 C61 B2 122.6(2) . . ?
C63 C62 C61 122.5(3) . . ?
C64 C63 C62 120.5(3) . . ?
C63 C64 C65 119.2(3) . . ?
C64 C65 C66 119.2(3) . . ?
C65 C66 C61 123.7(2) . . ?
C68 C67 B2 123.2(2) . . ?
C72 C67 C68 113.9(2) . . ?
C72 C67 B2 122.9(2) . . ?
C69 C68 C67 123.6(3) . . ?
C70 C69 C68 119.8(3) . . ?
C69 C70 C71 119.7(3) . . ?
C70 C71 C72 119.6(3) . . ?
C71 C72 C67 123.4(3) . . ?
C74 C73 C78 113.3(2) . . ?
C74 C73 B2 124.0(2) . . ?
C78 C73 B2 122.7(2) . . ?
C73 C74 C75 124.1(3) . . ?
C76 C75 C74 120.5(3) . . ?
C75 C76 C77 118.4(3) . . ?
C76 C77 C78 120.1(3) . . ?
C77 C78 C73 123.6(3) . . ?
C55 B2 C67 110.10(19) . . ?
C55 B2 C73 108.83(19) . . ?
C61 B2 C55 110.41(19) . . ?
C61 B2 C67 106.73(19) . . ?
C61 B2 C73 109.52(18) . . ?
C67 B2 C73 111.2(2) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1468985'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2015-07-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            5
_chemical_name_systematic        5
_chemical_formula_moiety         'C22 H22 Fe N6 O4, 2(Cl O4)'
_chemical_formula_sum            'C22 H22 Cl2 Fe N6 O12'
_chemical_formula_weight         689.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.386(3)
_cell_length_b                   10.700(2)
_cell_length_c                   16.934(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.31(3)
_cell_angle_gamma                90
_cell_volume                     2713.2(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8809
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4849
_cell_measurement_theta_min      1.2356
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_primary    'dark red'
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.175
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17804
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.613
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 39.9087
	          2theta: -20.0080
scan:
	Number of images: 180
	           Slice: -110.0000 - -20.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 39.9087
	          2theta: -20.0080
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             6525
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0619
_diffrn_orient_matrix_UB_12      -0.0041
_diffrn_orient_matrix_UB_13      -0.0249
_diffrn_orient_matrix_UB_21      -0.0328
_diffrn_orient_matrix_UB_22      -0.0211
_diffrn_orient_matrix_UB_23      0.0850
_diffrn_orient_matrix_UB_31      -0.0212
_diffrn_orient_matrix_UB_32      0.0566
_diffrn_orient_matrix_UB_33      0.0059
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5410
_reflns_number_total             6190
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6190
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+2.7994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1227
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O9B-O10B = O9B-O11B = O9B-O12B = O10B-O11B = O10B-O12B = O11B-O12B
 2.35 with sigma of 0.02
 O9A-O10A = O9A-O11A = O9A-O12A = O10A-O11A = O10A-O12A = O11A-O12A
 2.35 with sigma of 0.02
 Cl2-O9A = Cl2-O10A = Cl2-O11A = Cl2-O12A = Cl2-O9B = Cl2-O10B = Cl2-O11B
 1.44 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9B) \\sim Ueq, Uanis(O10B) \\sim Ueq, Uanis(O11B) \\sim Ueq, Uanis(O12B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9A) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(O12A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.51014(3) 0.59944(4) 0.25014(3) 0.02009(12) Uani 1 1 d . . . . .
Cl1 Cl 0.64672(5) 0.23586(7) 0.08234(5) 0.02743(18) Uani 1 1 d . . . . .
Cl2 Cl 0.35177(6) 0.94944(7) 0.40678(5) 0.0339(2) Uani 1 1 d D . . . .
C1 C 0.5914(2) 0.7710(3) 0.4078(2) 0.0324(7) Uani 1 1 d . . . . .
H1A H 0.5393 0.8265 0.4051 0.039 Uiso 1 1 calc R . . . .
H1B H 0.6370 0.8162 0.3861 0.039 Uiso 1 1 calc R . . . .
C2 C 0.6295(2) 0.7268(3) 0.4943(2) 0.0359(8) Uani 1 1 d . . . . .
H2A H 0.6935 0.7489 0.5121 0.043 Uiso 1 1 calc R . . . .
H2B H 0.5968 0.7650 0.5322 0.043 Uiso 1 1 calc R . . . .
C3 C 0.58205(19) 0.5643(3) 0.41398(19) 0.0257(6) Uani 1 1 d . . . . .
C4 C 0.56038(19) 0.4374(3) 0.38421(19) 0.0243(6) Uani 1 1 d . . . . .
C5 C 0.5719(2) 0.3250(3) 0.4252(2) 0.0297(7) Uani 1 1 d . . . . .
H5 H 0.5995 0.3220 0.4814 0.036 Uiso 1 1 calc R . . . .
C6 C 0.5424(2) 0.2163(3) 0.3826(2) 0.0292(7) Uani 1 1 d . . . . .
H6 H 0.5495 0.1380 0.4097 0.035 Uiso 1 1 calc R . . . .
C7 C 0.50255(19) 0.2219(3) 0.3004(2) 0.0256(6) Uani 1 1 d . . . . .
H7 H 0.4818 0.1481 0.2708 0.031 Uiso 1 1 calc R . . . .
C8 C 0.49370(18) 0.3368(3) 0.26262(18) 0.0208(6) Uani 1 1 d . . . . .
C9 C 0.45510(18) 0.3711(3) 0.17914(18) 0.0208(6) Uani 1 1 d . . . . .
C10 C 0.3841(2) 0.3641(3) 0.04803(19) 0.0311(7) Uani 1 1 d . . . . .
H10A H 0.3185 0.3584 0.0279 0.037 Uiso 1 1 calc R . . . .
H10B H 0.4132 0.3346 0.0050 0.037 Uiso 1 1 calc R . . . .
C11 C 0.4127(2) 0.4992(3) 0.07348(19) 0.0276(7) Uani 1 1 d . . . . .
H11A H 0.4536 0.5324 0.0412 0.033 Uiso 1 1 calc R . . . .
H11B H 0.3601 0.5549 0.0667 0.033 Uiso 1 1 calc R . . . .
C12 C 0.31796(19) 0.5961(3) 0.2949(2) 0.0282(7) Uani 1 1 d . . . . .
H12A H 0.3367 0.5937 0.3549 0.034 Uiso 1 1 calc R . . . .
H12B H 0.3009 0.5109 0.2743 0.034 Uiso 1 1 calc R . . . .
C13 C 0.2411(2) 0.6887(3) 0.2663(2) 0.0338(8) Uani 1 1 d . . . . .
H13A H 0.1894 0.6468 0.2305 0.041 Uiso 1 1 calc R . . . .
H13B H 0.2217 0.7251 0.3133 0.041 Uiso 1 1 calc R . . . .
C14 C 0.36066(19) 0.7496(3) 0.22334(19) 0.0260(6) Uani 1 1 d . . . . .
C15 C 0.4211(2) 0.8200(3) 0.1846(2) 0.0272(7) Uani 1 1 d . . . . .
C16 C 0.4101(2) 0.9340(3) 0.1453(2) 0.0363(8) Uani 1 1 d . . . . .
H16 H 0.3556 0.9790 0.1384 0.044 Uiso 1 1 calc R . . . .
C17 C 0.4804(2) 0.9809(3) 0.1161(2) 0.0374(8) Uani 1 1 d . . . . .
H17 H 0.4747 1.0598 0.0897 0.045 Uiso 1 1 calc R . . . .
C18 C 0.5593(2) 0.9136(3) 0.1252(2) 0.0347(8) Uani 1 1 d . . . . .
H18 H 0.6077 0.9453 0.1051 0.042 Uiso 1 1 calc R . . . .
C19 C 0.5657(2) 0.7994(3) 0.16430(19) 0.0266(7) Uani 1 1 d . . . . .
C20 C 0.6372(2) 0.7081(3) 0.18038(19) 0.0266(7) Uani 1 1 d . . . . .
C21 C 0.7617(2) 0.6028(3) 0.1785(2) 0.0355(8) Uani 1 1 d . . . . .
H21A H 0.8237 0.6178 0.2094 0.043 Uiso 1 1 calc R . . . .
H21B H 0.7633 0.5542 0.1291 0.043 Uiso 1 1 calc R . . . .
C22 C 0.70815(19) 0.5336(3) 0.2308(2) 0.0295(7) Uani 1 1 d . . . . .
H22A H 0.6949 0.4468 0.2116 0.035 Uiso 1 1 calc R . . . .
H22B H 0.7407 0.5320 0.2885 0.035 Uiso 1 1 calc R . . . .
N1 N 0.56459(15) 0.6540(2) 0.36257(16) 0.0243(5) Uani 1 1 d . . . . .
N2 N 0.52231(15) 0.4428(2) 0.30414(15) 0.0208(5) Uani 1 1 d . . . . .
N3 N 0.45808(15) 0.4871(2) 0.15904(15) 0.0217(5) Uani 1 1 d . . . . .
N4 N 0.38918(15) 0.6476(2) 0.25917(15) 0.0231(5) Uani 1 1 d . . . . .
N5 N 0.49776(16) 0.7549(2) 0.19459(15) 0.0236(5) Uani 1 1 d . . . . .
N6 N 0.62605(16) 0.6083(2) 0.21956(16) 0.0238(5) Uani 1 1 d . . . . .
O1 O 0.61755(15) 0.5891(2) 0.49141(14) 0.0337(5) Uani 1 1 d . . . . .
O2 O 0.41420(14) 0.29050(19) 0.12284(13) 0.0268(5) Uani 1 1 d . . . . .
O3 O 0.27742(14) 0.7864(2) 0.22165(15) 0.0334(5) Uani 1 1 d . . . . .
O4 O 0.71392(14) 0.7219(2) 0.15718(15) 0.0346(6) Uani 1 1 d . . . . .
O5 O 0.69554(15) 0.3480(2) 0.07494(15) 0.0377(6) Uani 1 1 d . . . . .
O6 O 0.69956(17) 0.1294(2) 0.07160(17) 0.0464(7) Uani 1 1 d . . . . .
O7 O 0.62720(16) 0.2312(2) 0.16116(15) 0.0422(6) Uani 1 1 d . . . . .
O8 O 0.56489(15) 0.2348(2) 0.02166(16) 0.0423(6) Uani 1 1 d . . . . .
O9A O 0.3707(8) 0.8175(6) 0.4107(8) 0.0304(19) Uani 0.55(2) 1 d D U P A 1
O10A O 0.2587(4) 0.9645(9) 0.3641(5) 0.0375(18) Uani 0.55(2) 1 d D U P A 1
O11A O 0.4083(6) 1.0103(12) 0.3654(8) 0.061(3) Uani 0.55(2) 1 d D U P A 1
O12A O 0.3568(10) 0.9925(8) 0.4895(3) 0.057(3) Uani 0.55(2) 1 d D U P A 1
O9B O 0.3453(10) 0.8188(7) 0.4187(10) 0.036(3) Uani 0.45(2) 1 d D U P A 2
O10B O 0.2685(7) 1.0110(17) 0.3840(9) 0.065(4) Uani 0.45(2) 1 d D U P A 2
O11B O 0.3989(7) 0.9706(10) 0.3417(6) 0.037(2) Uani 0.45(2) 1 d D U P A 2
O12B O 0.4111(11) 1.0076(7) 0.4774(5) 0.054(3) Uani 0.45(2) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.983(3) . ?
Fe1 N2 1.898(2) . ?
Fe1 N3 1.974(3) . ?
Fe1 N4 1.971(2) . ?
Fe1 N5 1.899(2) . ?
Fe1 N6 1.971(2) . ?
Cl1 O5 1.437(2) . ?
Cl1 O6 1.435(2) . ?
Cl1 O7 1.435(2) . ?
Cl1 O8 1.430(3) . ?
Cl2 O9A 1.440(6) . ?
Cl2 O10A 1.457(6) . ?
Cl2 O11A 1.397(6) . ?
Cl2 O12A 1.460(5) . ?
Cl2 O9B 1.419(7) . ?
Cl2 O10B 1.413(7) . ?
Cl2 O11B 1.470(6) . ?
Cl2 O12B 1.466(7) . ?
C1 C2 1.523(5) . ?
C1 N1 1.476(4) . ?
C2 O1 1.485(4) . ?
C3 C4 1.460(4) . ?
C3 N1 1.282(4) . ?
C3 O1 1.326(4) . ?
C4 C5 1.379(4) . ?
C4 N2 1.349(4) . ?
C5 C6 1.390(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.378(4) . ?
C8 C9 1.449(4) . ?
C8 N2 1.353(4) . ?
C9 N3 1.290(4) . ?
C9 O2 1.332(3) . ?
C10 C11 1.543(4) . ?
C10 O2 1.473(4) . ?
C11 N3 1.462(4) . ?
C12 C13 1.534(4) . ?
C12 N4 1.475(4) . ?
C13 O3 1.474(4) . ?
C14 C15 1.464(4) . ?
C14 N4 1.277(4) . ?
C14 O3 1.334(3) . ?
C15 C16 1.382(4) . ?
C15 N5 1.346(4) . ?
C16 C17 1.383(5) . ?
C17 C18 1.390(5) . ?
C18 C19 1.382(4) . ?
C19 C20 1.451(4) . ?
C19 N5 1.353(4) . ?
C20 N6 1.289(4) . ?
C20 O4 1.335(3) . ?
C21 C22 1.533(4) . ?
C21 O4 1.474(4) . ?
C22 N6 1.470(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 79.89(11) . . ?
N2 Fe1 N3 79.40(10) . . ?
N2 Fe1 N4 100.58(10) . . ?
N2 Fe1 N5 179.14(11) . . ?
N2 Fe1 N6 100.04(10) . . ?
N3 Fe1 N1 159.25(10) . . ?
N4 Fe1 N1 92.65(10) . . ?
N4 Fe1 N3 89.96(10) . . ?
N5 Fe1 N1 100.93(11) . . ?
N5 Fe1 N3 99.78(10) . . ?
N5 Fe1 N4 79.66(10) . . ?
N5 Fe1 N6 79.71(10) . . ?
N6 Fe1 N1 91.73(10) . . ?
N6 Fe1 N3 93.04(10) . . ?
N6 Fe1 N4 159.36(10) . . ?
O6 Cl1 O5 109.23(14) . . ?
O7 Cl1 O5 109.61(15) . . ?
O7 Cl1 O6 109.66(15) . . ?
O8 Cl1 O5 109.58(15) . . ?
O8 Cl1 O6 109.49(17) . . ?
O8 Cl1 O7 109.26(15) . . ?
O9A Cl2 O10A 107.2(5) . . ?
O9A Cl2 O12A 107.5(5) . . ?
O10A Cl2 O12A 105.7(4) . . ?
O11A Cl2 O9A 109.7(5) . . ?
O11A Cl2 O10A 110.7(5) . . ?
O11A Cl2 O12A 115.6(4) . . ?
O9B Cl2 O11B 108.7(6) . . ?
O9B Cl2 O12B 110.7(7) . . ?
O10B Cl2 O9B 114.1(7) . . ?
O10B Cl2 O11B 107.2(6) . . ?
O10B Cl2 O12B 112.4(5) . . ?
O12B Cl2 O11B 103.0(5) . . ?
N1 C1 C2 103.6(3) . . ?
O1 C2 C1 105.0(3) . . ?
N1 C3 C4 117.8(3) . . ?
N1 C3 O1 119.8(3) . . ?
O1 C3 C4 122.4(3) . . ?
C5 C4 C3 130.1(3) . . ?
N2 C4 C3 108.6(3) . . ?
N2 C4 C5 121.3(3) . . ?
C4 C5 C6 118.7(3) . . ?
C7 C6 C5 120.0(3) . . ?
C8 C7 C6 118.6(3) . . ?
C7 C8 C9 130.8(3) . . ?
N2 C8 C7 121.4(3) . . ?
N2 C8 C9 107.8(2) . . ?
N3 C9 C8 118.0(3) . . ?
N3 C9 O2 118.3(3) . . ?
O2 C9 C8 123.7(3) . . ?
O2 C10 C11 104.3(2) . . ?
N3 C11 C10 103.6(2) . . ?
N4 C12 C13 102.8(2) . . ?
O3 C13 C12 105.3(2) . . ?
N4 C14 C15 117.9(3) . . ?
N4 C14 O3 119.1(3) . . ?
O3 C14 C15 123.0(3) . . ?
C16 C15 C14 130.5(3) . . ?
N5 C15 C14 107.8(3) . . ?
N5 C15 C16 121.7(3) . . ?
C15 C16 C17 118.2(3) . . ?
C16 C17 C18 120.5(3) . . ?
C19 C18 C17 118.4(3) . . ?
C18 C19 C20 130.8(3) . . ?
N5 C19 C18 121.2(3) . . ?
N5 C19 C20 108.1(3) . . ?
N6 C20 C19 118.0(3) . . ?
N6 C20 O4 118.4(3) . . ?
O4 C20 C19 123.6(3) . . ?
O4 C21 C22 104.8(2) . . ?
N6 C22 C21 102.8(3) . . ?
C1 N1 Fe1 138.9(2) . . ?
C3 N1 Fe1 114.1(2) . . ?
C3 N1 C1 107.0(3) . . ?
C4 N2 Fe1 119.6(2) . . ?
C4 N2 C8 120.0(3) . . ?
C8 N2 Fe1 120.4(2) . . ?
C9 N3 Fe1 114.3(2) . . ?
C9 N3 C11 108.0(3) . . ?
C11 N3 Fe1 137.4(2) . . ?
C12 N4 Fe1 137.6(2) . . ?
C14 N4 Fe1 114.47(19) . . ?
C14 N4 C12 107.9(2) . . ?
C15 N5 Fe1 120.1(2) . . ?
C15 N5 C19 120.0(3) . . ?
C19 N5 Fe1 119.9(2) . . ?
C20 N6 Fe1 114.3(2) . . ?
C20 N6 C22 107.7(2) . . ?
C22 N6 Fe1 137.9(2) . . ?
C3 O1 C2 104.5(3) . . ?
C9 O2 C10 105.8(2) . . ?
C14 O3 C13 104.8(2) . . ?
C20 O4 C21 104.9(2) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1468986'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            6
_chemical_name_systematic        6
_chemical_formula_moiety         'C22 H22 Fe N6 O4, 2(B F4)'
_chemical_formula_sum            'C22 H22 B2 F8 Fe N6 O4'
_chemical_formula_weight         663.92
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.5545(11)
_cell_length_b                   10.6057(8)
_cell_length_c                   17.0270(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.9860(10)
_cell_angle_gamma                90
_cell_volume                     2725.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8441
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0469 before and 0.0331 after correction.
The Ratio of minimum to maximum transmission is 0.9175.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20104
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.014
_diffrn_reflns_theta_min         1.592
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4527
_reflns_number_total             5310
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0552
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1080P)²+2.5430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1748
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.00993(3) 0.40362(4) 0.25231(2) 0.03497(17) Uani 1 1 d . . . . .
O1 O -0.22054(17) 0.2125(3) 0.21838(17) 0.0641(7) Uani 1 1 d . . . . .
O2 O 0.21245(18) 0.2842(3) 0.16006(18) 0.0652(7) Uani 1 1 d . . . . .
O3 O 0.1198(2) 0.4128(3) 0.49341(15) 0.0640(7) Uani 1 1 d . . . . .
O4 O -0.08662(15) 0.7166(2) 0.12624(13) 0.0482(5) Uani 1 1 d . . . . .
N1 N -0.11009(17) 0.3528(3) 0.25953(16) 0.0427(6) Uani 1 1 d . . . . .
N2 N -0.00153(18) 0.2472(2) 0.19580(16) 0.0431(6) Uani 1 1 d . . . . .
N3 N 0.12542(18) 0.3962(2) 0.22276(17) 0.0440(6) Uani 1 1 d . . . . .
N4 N 0.06482(17) 0.3486(3) 0.36522(17) 0.0439(6) Uani 1 1 d . . . . .
N5 N 0.02177(16) 0.5621(2) 0.30681(15) 0.0367(5) Uani 1 1 d . . . . .
N6 N -0.04293(16) 0.5183(2) 0.16128(15) 0.0381(5) Uani 1 1 d . . . . .
C1 C -0.1820(2) 0.4041(4) 0.2933(3) 0.0561(9) Uani 1 1 d . . . . .
H1A H -0.1989 0.4881 0.2728 0.067 Uiso 1 1 calc R . . . .
H1B H -0.1648 0.4066 0.3519 0.067 Uiso 1 1 calc R . . . .
C2 C -0.2574(2) 0.3095(4) 0.2630(3) 0.0692(12) Uani 1 1 d . . . . .
H2A H -0.2761 0.2721 0.3082 0.083 Uiso 1 1 calc R . . . .
H2B H -0.3079 0.3507 0.2277 0.083 Uiso 1 1 calc R . . . .
C3 C -0.1380(2) 0.2504(3) 0.2219(2) 0.0479(8) Uani 1 1 d . . . . .
C4 C -0.0780(2) 0.1811(3) 0.1844(2) 0.0490(8) Uani 1 1 d . . . . .
C5 C -0.0876(3) 0.0677(4) 0.1438(3) 0.0648(11) Uani 1 1 d . . . . .
H5 H -0.1400 0.0221 0.1363 0.078 Uiso 1 1 calc R . . . .
C6 C -0.0174(4) 0.0221(4) 0.1141(3) 0.0736(13) Uani 1 1 d . . . . .
H6 H -0.0227 -0.0549 0.0871 0.088 Uiso 1 1 calc R . . . .
C7 C 0.0592(3) 0.0904(3) 0.1245(2) 0.0632(11) Uani 1 1 d . . . . .
H7 H 0.1061 0.0609 0.1045 0.076 Uiso 1 1 calc R . . . .
C8 C 0.0656(2) 0.2047(3) 0.1655(2) 0.0477(8) Uani 1 1 d . . . . .
C9 C 0.1365(2) 0.2975(3) 0.1834(2) 0.0479(8) Uani 1 1 d . . . . .
C10 C 0.2613(3) 0.4019(4) 0.1855(3) 0.0719(12) Uani 1 1 d . . . . .
H10A H 0.2659 0.4515 0.1388 0.086 Uiso 1 1 calc R . . . .
H10B H 0.3205 0.3842 0.2178 0.086 Uiso 1 1 calc R . . . .
C11 C 0.2069(2) 0.4722(4) 0.2357(3) 0.0583(9) Uani 1 1 d . . . . .
H11A H 0.2377 0.4744 0.2925 0.070 Uiso 1 1 calc R . . . .
H11B H 0.1940 0.5578 0.2163 0.070 Uiso 1 1 calc R . . . .
C12 C 0.0923(3) 0.2298(4) 0.4108(2) 0.0601(10) Uani 1 1 d . . . . .
H12A H 0.1348 0.1836 0.3885 0.072 Uiso 1 1 calc R . . . .
H12B H 0.0417 0.1762 0.4102 0.072 Uiso 1 1 calc R . . . .
C13 C 0.1342(3) 0.2759(4) 0.4958(2) 0.0681(11) Uani 1 1 d . . . . .
H13A H 0.1062 0.2366 0.5347 0.082 Uiso 1 1 calc R . . . .
H13B H 0.1970 0.2566 0.5106 0.082 Uiso 1 1 calc R . . . .
C14 C 0.0827(2) 0.4388(3) 0.41591(19) 0.0450(7) Uani 1 1 d . . . . .
C15 C 0.0601(2) 0.5676(3) 0.38696(19) 0.0441(7) Uani 1 1 d . . . . .
C16 C 0.0714(2) 0.6808(4) 0.4279(2) 0.0546(9) Uani 1 1 d . . . . .
H16 H 0.0986 0.6838 0.4829 0.066 Uiso 1 1 calc R . . . .
C17 C 0.0413(2) 0.7899(3) 0.3854(2) 0.0546(9) Uani 1 1 d . . . . .
H17 H 0.0479 0.8672 0.4120 0.066 Uiso 1 1 calc R . . . .
C18 C 0.0016(2) 0.7845(3) 0.3034(2) 0.0456(7) Uani 1 1 d . . . . .
H18 H -0.0187 0.8573 0.2743 0.055 Uiso 1 1 calc R . . . .
C19 C -0.00721(19) 0.6681(3) 0.26587(18) 0.0375(6) Uani 1 1 d . . . . .
C20 C -0.04593(19) 0.6340(3) 0.18187(18) 0.0369(6) Uani 1 1 d . . . . .
C21 C -0.1151(3) 0.6428(4) 0.0505(2) 0.0592(9) Uani 1 1 d . . . . .
H21A H -0.0856 0.6727 0.0099 0.071 Uiso 1 1 calc R . . . .
H21B H -0.1786 0.6490 0.0290 0.071 Uiso 1 1 calc R . . . .
C22 C -0.0880(2) 0.5070(4) 0.0748(2) 0.0537(9) Uani 1 1 d . . . . .
H22A H -0.1394 0.4524 0.0672 0.064 Uiso 1 1 calc R . . . .
H22B H -0.0482 0.4741 0.0438 0.064 Uiso 1 1 calc R . . . .
F5 F 0.6021(2) 0.5172(4) 0.1490(3) 0.1320(15) Uani 1 1 d . . . . .
F6 F 0.7364(2) 0.5226(5) 0.1290(2) 0.1262(15) Uani 1 1 d . . . . .
F7 F 0.6417(3) 0.6795(3) 0.08660(17) 0.1081(12) Uani 1 1 d . . . . .
F8 F 0.6201(5) 0.5023(4) 0.0210(2) 0.207(3) Uani 1 1 d . . . . .
B2 B 0.6497(3) 0.5531(4) 0.0942(3) 0.0622(12) Uani 1 1 d . . . . .
F1 F 0.1200(2) 0.7705(4) 0.1567(2) 0.1083(11) Uani 1 1 d . . . . .
F2 F 0.0685(3) 0.7608(4) 0.0240(2) 0.1280(13) Uani 1 1 d . . . . .
F3 F 0.1890(3) 0.8705(4) 0.0718(3) 0.1262(14) Uani 1 1 d . . . . .
F4 F 0.1929(3) 0.6573(4) 0.0776(2) 0.1189(12) Uani 1 1 d . . . . .
B1 B 0.1452(3) 0.7609(5) 0.0841(3) 0.0654(12) 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 N1 1.975(3) . ?
Fe1 N2 1.905(3) . ?
Fe1 N3 1.981(3) . ?
Fe1 N4 1.993(3) . ?
Fe1 N5 1.907(3) . ?
Fe1 N6 1.985(3) . ?
O1 C2 1.474(6) . ?
O1 C3 1.333(4) . ?
O2 C9 1.342(4) . ?
O2 C10 1.471(6) . ?
O3 C13 1.469(5) . ?
O3 C14 1.335(4) . ?
O4 C20 1.333(4) . ?
O4 C21 1.482(4) . ?
N1 C1 1.479(4) . ?
N1 C3 1.281(4) . ?
N2 C4 1.353(4) . ?
N2 C8 1.349(4) . ?
N3 C9 1.277(4) . ?
N3 C11 1.473(4) . ?
N4 C12 1.488(4) . ?
N4 C14 1.273(4) . ?
N5 C15 1.352(4) . ?
N5 C19 1.342(4) . ?
N6 C20 1.280(4) . ?
N6 C22 1.474(4) . ?
C1 C2 1.534(6) . ?
C3 C4 1.452(5) . ?
C4 C5 1.377(5) . ?
C5 C6 1.396(7) . ?
C6 C7 1.369(7) . ?
C7 C8 1.391(5) . ?
C8 C9 1.454(5) . ?
C10 C11 1.534(6) . ?
C12 C13 1.516(6) . ?
C14 C15 1.466(5) . ?
C15 C16 1.377(5) . ?
C16 C17 1.385(5) . ?
C17 C18 1.385(5) . ?
C18 C19 1.381(4) . ?
C19 C20 1.457(4) . ?
C21 C22 1.530(6) . ?
F5 B2 1.377(6) . ?
F6 B2 1.375(6) . ?
F7 B2 1.350(5) . ?
F8 B2 1.333(6) . ?
F1 B1 1.388(6) . ?
F2 B1 1.372(6) . ?
F3 B1 1.388(6) . ?
F4 B1 1.345(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N3 159.02(12) . . ?
N1 Fe1 N4 92.93(11) . . ?
N1 Fe1 N6 89.80(10) . . ?
N2 Fe1 N1 79.58(12) . . ?
N2 Fe1 N3 79.44(11) . . ?
N2 Fe1 N4 101.44(11) . . ?
N2 Fe1 N5 178.74(11) . . ?
N2 Fe1 N6 99.71(11) . . ?
N3 Fe1 N4 91.72(11) . . ?
N3 Fe1 N6 93.21(11) . . ?
N5 Fe1 N1 101.06(11) . . ?
N5 Fe1 N3 99.90(11) . . ?
N5 Fe1 N4 79.63(11) . . ?
N5 Fe1 N6 79.23(10) . . ?
N6 Fe1 N4 158.82(11) . . ?
C3 O1 C2 104.9(3) . . ?
C9 O2 C10 104.7(3) . . ?
C14 O3 C13 105.0(3) . . ?
C20 O4 C21 105.2(3) . . ?
C1 N1 Fe1 137.6(2) . . ?
C3 N1 Fe1 114.3(2) . . ?
C3 N1 C1 108.0(3) . . ?
C4 N2 Fe1 119.7(2) . . ?
C8 N2 Fe1 119.8(2) . . ?
C8 N2 C4 120.5(3) . . ?
C9 N3 Fe1 114.3(2) . . ?
C9 N3 C11 107.9(3) . . ?
C11 N3 Fe1 137.8(2) . . ?
C12 N4 Fe1 138.9(2) . . ?
C14 N4 Fe1 114.0(2) . . ?
C14 N4 C12 107.1(3) . . ?
C15 N5 Fe1 119.8(2) . . ?
C19 N5 Fe1 120.3(2) . . ?
C19 N5 C15 119.9(3) . . ?
C20 N6 Fe1 114.1(2) . . ?
C20 N6 C22 108.2(3) . . ?
C22 N6 Fe1 137.5(2) . . ?
N1 C1 C2 102.5(3) . . ?
O1 C2 C1 105.6(3) . . ?
O1 C3 C4 122.8(3) . . ?
N1 C3 O1 118.9(3) . . ?
N1 C3 C4 118.2(3) . . ?
N2 C4 C3 108.1(3) . . ?
N2 C4 C5 120.6(4) . . ?
C5 C4 C3 131.3(4) . . ?
C4 C5 C6 119.0(4) . . ?
C7 C6 C5 120.2(4) . . ?
C6 C7 C8 118.7(4) . . ?
N2 C8 C7 121.0(4) . . ?
N2 C8 C9 108.2(3) . . ?
C7 C8 C9 130.8(4) . . ?
O2 C9 C8 123.0(3) . . ?
N3 C9 O2 118.8(3) . . ?
N3 C9 C8 118.2(3) . . ?
O2 C10 C11 105.1(3) . . ?
N3 C11 C10 102.8(3) . . ?
N4 C12 C13 103.2(3) . . ?
O3 C13 C12 105.3(3) . . ?
O3 C14 C15 122.4(3) . . ?
N4 C14 O3 119.1(3) . . ?
N4 C14 C15 118.5(3) . . ?
N5 C15 C14 108.1(3) . . ?
N5 C15 C16 121.3(3) . . ?
C16 C15 C14 130.6(3) . . ?
C15 C16 C17 118.5(3) . . ?
C18 C17 C16 120.3(3) . . ?
C19 C18 C17 118.3(3) . . ?
N5 C19 C18 121.7(3) . . ?
N5 C19 C20 108.0(3) . . ?
C18 C19 C20 130.3(3) . . ?
O4 C20 C19 123.2(3) . . ?
N6 C20 O4 118.6(3) . . ?
N6 C20 C19 118.2(3) . . ?
O4 C21 C22 104.9(3) . . ?
N6 C22 C21 103.1(3) . . ?
F6 B2 F5 105.9(4) . . ?
F7 B2 F5 106.7(4) . . ?
F7 B2 F6 109.4(4) . . ?
F8 B2 F5 113.7(5) . . ?
F8 B2 F6 112.9(5) . . ?
F8 B2 F7 108.0(4) . . ?
F2 B1 F1 106.4(4) . . ?
F2 B1 F3 105.0(5) . . ?
F3 B1 F1 109.1(4) . . ?
F4 B1 F1 114.4(5) . . ?
F4 B1 F2 109.6(4) . . ?
F4 B1 F3 111.8(4) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile/ether
_chemical_compound_source        no
####################################################################### 
# 
# 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_7-1
_database_code_depnum_ccdc_archive 'CCDC 1468987'
_audit_update_record             
;
2016-03-16 deposited with the CCDC.
2016-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            7-1
_chemical_name_systematic        7-1
_chemical_formula_moiety         'C22 H22 Fe N6 O4, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C24 H25 F12 Fe N7 O4 P2'
_chemical_formula_weight         821.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.352(3)
_cell_length_b                   10.908(2)
_cell_length_c                   20.708(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.05(3)
_cell_angle_gamma                90
_cell_volume                     3391.2(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11043
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      28.8199
_cell_measurement_theta_min      2.0112
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Chip
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21602
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         2.011
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.7082
	          2theta: -19.8280
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.7082
	          2theta: -19.8280
;
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             9260
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0038
_diffrn_orient_matrix_UB_12      0.0520
_diffrn_orient_matrix_UB_13      -0.0414
_diffrn_orient_matrix_UB_21      -0.0626
_diffrn_orient_matrix_UB_22      0.0444
_diffrn_orient_matrix_UB_23      0.0501
_diffrn_orient_matrix_UB_31      0.0358
_diffrn_orient_matrix_UB_32      0.0271
_diffrn_orient_matrix_UB_33      0.0207
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           90.0000
_diffrn_source_power             4.5000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4146
_reflns_number_total             6621
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.078
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6621
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0879
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1720P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2413
_refine_ls_wR_factor_ref         0.2731
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.27775(5) 0.90760(6) 0.11051(3) 0.0445(3) Uani 1 1 d . . . . .
O1 O 0.3083(3) 1.2169(3) 0.00461(16) 0.0565(10) Uani 1 1 d . . . . .
O2 O 0.1562(3) 0.9191(3) 0.26897(17) 0.0573(10) Uani 1 1 d . . . . .
O3 O 0.1222(3) 0.6988(3) -0.03337(18) 0.0573(10) Uani 1 1 d . . . . .
O4 O 0.5331(3) 0.8083(4) 0.19590(19) 0.0614(10) Uani 1 1 d . . . . .
N1 N 0.3115(3) 1.0224(4) 0.04382(19) 0.0473(10) Uani 1 1 d . . . . .
N2 N 0.2360(3) 1.0632(4) 0.13758(19) 0.0455(10) Uani 1 1 d . . . . .
N3 N 0.2232(3) 0.8534(4) 0.1866(2) 0.0481(10) Uani 1 1 d . . . . .
N4 N 0.1732(3) 0.8453(4) 0.0435(2) 0.0457(10) Uani 1 1 d . . . . .
N5 N 0.3246(3) 0.7557(4) 0.0835(2) 0.0464(10) Uani 1 1 d . . . . .
N6 N 0.3995(3) 0.9092(4) 0.1675(2) 0.0492(10) Uani 1 1 d . . . . .
C1 C 0.3540(4) 1.0113(6) -0.0152(3) 0.0607(15) Uani 1 1 d . . . . .
H1A H 0.3198 0.9575 -0.0484 0.073 Uiso 1 1 calc R . . . .
H1B H 0.4145 0.9806 -0.0026 0.073 Uiso 1 1 calc R . . . .
C2 C 0.3525(4) 1.1427(6) -0.0400(3) 0.0593(14) Uani 1 1 d . . . . .
H2A H 0.4126 1.1720 -0.0383 0.071 Uiso 1 1 calc R . . . .
H2B H 0.3193 1.1480 -0.0852 0.071 Uiso 1 1 calc R . . . .
C3 C 0.2895(4) 1.1350(5) 0.0489(2) 0.0482(12) Uani 1 1 d . . . . .
C4 C 0.2473(4) 1.1678(4) 0.1033(2) 0.0467(12) Uani 1 1 d . . . . .
C5 C 0.2188(4) 1.2819(5) 0.1236(3) 0.0625(16) Uani 1 1 d . . . . .
H5 H 0.2256 1.3525 0.0999 0.075 Uiso 1 1 calc R . . . .
C6 C 0.1807(5) 1.2890(5) 0.1788(3) 0.0684(18) Uani 1 1 d . . . . .
H6 H 0.1622 1.3639 0.1927 0.082 Uiso 1 1 calc R . . . .
C7 C 0.1708(4) 1.1798(5) 0.2133(3) 0.0614(15) Uani 1 1 d . . . . .
H7 H 0.1462 1.1821 0.2507 0.074 Uiso 1 1 calc R . . . .
C8 C 0.1978(4) 1.0702(5) 0.1913(3) 0.0510(13) Uani 1 1 d . . . . .
C9 C 0.1925(4) 0.9431(5) 0.2167(3) 0.0493(12) Uani 1 1 d . . . . .
C10 C 0.1590(4) 0.7822(5) 0.2756(3) 0.0621(15) Uani 1 1 d . . . . .
H10A H 0.0992 0.7486 0.2687 0.074 Uiso 1 1 calc R . . . .
H10B H 0.1917 0.7580 0.3190 0.074 Uiso 1 1 calc R . . . .
C11 C 0.2073(4) 0.7371(5) 0.2210(3) 0.0553(14) Uani 1 1 d . . . . .
H11A H 0.2630 0.6968 0.2402 0.066 Uiso 1 1 calc R . . . .
H11B H 0.1701 0.6809 0.1909 0.066 Uiso 1 1 calc R . . . .
C12 C 0.0813(3) 0.8880(5) 0.0145(3) 0.0530(13) Uani 1 1 d . . . . .
H12A H 0.0819 0.9651 -0.0088 0.064 Uiso 1 1 calc R . . . .
H12B H 0.0461 0.8973 0.0480 0.064 Uiso 1 1 calc R . . . .
C13 C 0.0447(4) 0.7801(5) -0.0348(3) 0.0630(16) Uani 1 1 d . . . . .
H13A H -0.0029 0.7365 -0.0203 0.076 Uiso 1 1 calc R . . . .
H13B H 0.0223 0.8114 -0.0790 0.076 Uiso 1 1 calc R . . . .
C14 C 0.1877(3) 0.7448(4) 0.0150(2) 0.0471(12) Uani 1 1 d . . . . .
C15 C 0.2758(4) 0.6836(4) 0.0368(2) 0.0470(12) Uani 1 1 d . . . . .
C16 C 0.3064(4) 0.5737(5) 0.0163(3) 0.0568(15) Uani 1 1 d . . . . .
H16 H 0.2709 0.5264 -0.0162 0.068 Uiso 1 1 calc R . . . .
C17 C 0.3932(4) 0.5359(5) 0.0463(3) 0.0576(14) Uani 1 1 d . . . . .
H17 H 0.4158 0.4622 0.0343 0.069 Uiso 1 1 calc R . . . .
C18 C 0.4443(4) 0.6097(5) 0.0939(3) 0.0556(14) Uani 1 1 d . . . . .
H18 H 0.5018 0.5858 0.1139 0.067 Uiso 1 1 calc R . . . .
C19 C 0.4095(4) 0.7206(5) 0.1120(2) 0.0492(12) Uani 1 1 d . . . . .
C20 C 0.4480(4) 0.8167(5) 0.1593(3) 0.0521(13) Uani 1 1 d . . . . .
C21 C 0.5452(4) 0.9248(6) 0.2356(3) 0.0672(17) Uani 1 1 d . . . . .
H21A H 0.5894 0.9770 0.2223 0.081 Uiso 1 1 calc R . . . .
H21B H 0.5639 0.9070 0.2824 0.081 Uiso 1 1 calc R . . . .
C22 C 0.4536(4) 0.9866(5) 0.2210(3) 0.0611(15) Uani 1 1 d . . . . .
H22A H 0.4276 0.9872 0.2599 0.073 Uiso 1 1 calc R . . . .
H22B H 0.4578 1.0702 0.2060 0.073 Uiso 1 1 calc R . . . .
P2 P 0.56043(10) 0.24692(13) 0.12009(7) 0.0501(4) Uani 1 1 d . . . . .
F7 F 0.4591(2) 0.2769(4) 0.12377(17) 0.0756(10) Uani 1 1 d . . . . .
F8 F 0.5849(3) 0.3901(3) 0.13014(18) 0.0763(11) Uani 1 1 d . . . . .
F9 F 0.5826(2) 0.2265(3) 0.19888(15) 0.0675(10) Uani 1 1 d . . . . .
F10 F 0.5350(3) 0.1030(3) 0.10950(16) 0.0721(10) Uani 1 1 d . . . . .
F11 F 0.5371(3) 0.2656(4) 0.04112(16) 0.0755(10) Uani 1 1 d . . . . .
F12 F 0.6618(2) 0.2173(3) 0.11666(17) 0.0722(10) Uani 1 1 d . . . . .
P1 P 0.09773(11) 1.05945(14) -0.16020(7) 0.0533(4) Uani 1 1 d . . . . .
F1 F 0.0445(3) 1.1738(3) -0.1972(2) 0.0864(12) Uani 1 1 d . . . . .
F2 F 0.0852(3) 0.9887(4) -0.22904(18) 0.0968(14) Uani 1 1 d . . . . .
F3 F 0.1869(3) 1.1198(5) -0.1701(2) 0.118(2) Uani 1 1 d . . . . .
F4 F 0.1102(3) 1.1293(4) -0.08961(18) 0.0922(13) Uani 1 1 d . . . . .
F5 F 0.0062(2) 1.0033(4) -0.14721(19) 0.0815(11) Uani 1 1 d . . . . .
F6 F 0.1503(3) 0.9448(4) -0.12180(18) 0.0808(11) Uani 1 1 d . . . . .
N7 N 0.0927(5) 0.5330(6) 0.0831(3) 0.0861(18) Uani 1 1 d . . . . .
C23 C 0.0247(6) 0.5445(6) 0.0962(3) 0.0704(18) Uani 1 1 d . . . . .
C24 C -0.0601(6) 0.5586(7) 0.1154(4) 0.101(3) Uani 1 1 d . . . . .
H24A H -0.1062 0.5222 0.0825 0.152 Uiso 1 1 calc GR . . . .
H24B H -0.0725 0.6442 0.1194 0.152 Uiso 1 1 calc GR . . . .
H24C H -0.0579 0.5188 0.1570 0.152 Uiso 1 1 calc GR . . . .


_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 N1 2.011(4) . ?
Fe1 N2 1.938(4) . ?
Fe1 N3 2.020(4) . ?
Fe1 N4 2.008(4) . ?
Fe1 N5 1.935(4) . ?
Fe1 N6 1.992(5) . ?
O1 C2 1.493(7) . ?
O1 C3 1.355(6) . ?
O2 C9 1.343(6) . ?
O2 C10 1.499(7) . ?
O3 C13 1.480(7) . ?
O3 C14 1.358(6) . ?
O4 C20 1.369(6) . ?
O4 C21 1.504(7) . ?
N1 C1 1.505(6) . ?
N1 C3 1.285(6) . ?
N2 C4 1.373(6) . ?
N2 C8 1.364(6) . ?
N3 C9 1.301(7) . ?
N3 C11 1.500(6) . ?
N4 C12 1.488(6) . ?
N4 C14 1.287(6) . ?
N5 C15 1.347(6) . ?
N5 C19 1.368(6) . ?
N6 C20 1.286(7) . ?
N6 C22 1.497(6) . ?
C1 C2 1.522(8) . ?
C3 C4 1.455(7) . ?
C4 C5 1.412(7) . ?
C5 C6 1.392(8) . ?
C6 C7 1.414(8) . ?
C7 C8 1.374(7) . ?
C8 C9 1.490(7) . ?
C10 C11 1.554(8) . ?
C12 C13 1.581(8) . ?
C14 C15 1.490(7) . ?
C15 C16 1.386(7) . ?
C16 C17 1.409(8) . ?
C17 C18 1.382(8) . ?
C18 C19 1.405(7) . ?
C19 C20 1.472(8) . ?
C21 C22 1.532(8) . ?
P2 F7 1.606(4) . ?
P2 F8 1.610(4) . ?
P2 F9 1.611(3) . ?
P2 F10 1.622(3) . ?
P2 F11 1.612(3) . ?
P2 F12 1.605(4) . ?
P1 F1 1.596(4) . ?
P1 F2 1.597(4) . ?
P1 F3 1.570(4) . ?
P1 F4 1.624(4) . ?
P1 F5 1.606(4) . ?
P1 F6 1.606(4) . ?
N7 C23 1.139(9) . ?
C23 C24 1.446(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N3 157.81(17) . . ?
N2 Fe1 N1 78.54(17) . . ?
N2 Fe1 N3 79.35(17) . . ?
N2 Fe1 N4 103.37(18) . . ?
N2 Fe1 N6 98.44(18) . . ?
N4 Fe1 N1 91.13(17) . . ?
N4 Fe1 N3 92.16(17) . . ?
N5 Fe1 N1 99.78(17) . . ?
N5 Fe1 N2 177.37(19) . . ?
N5 Fe1 N3 102.38(18) . . ?
N5 Fe1 N4 78.62(17) . . ?
N5 Fe1 N6 79.58(18) . . ?
N6 Fe1 N1 93.26(17) . . ?
N6 Fe1 N3 91.79(18) . . ?
N6 Fe1 N4 158.19(18) . . ?
C3 O1 C2 104.5(4) . . ?
C9 O2 C10 105.0(4) . . ?
C14 O3 C13 105.2(4) . . ?
C20 O4 C21 104.0(4) . . ?
C1 N1 Fe1 136.5(4) . . ?
C3 N1 Fe1 115.4(4) . . ?
C3 N1 C1 108.1(5) . . ?
C4 N2 Fe1 119.5(3) . . ?
C8 N2 Fe1 120.6(3) . . ?
C8 N2 C4 119.8(4) . . ?
C9 N3 Fe1 113.8(3) . . ?
C9 N3 C11 107.3(4) . . ?
C11 N3 Fe1 138.9(4) . . ?
C12 N4 Fe1 136.6(3) . . ?
C14 N4 Fe1 114.5(3) . . ?
C14 N4 C12 108.8(4) . . ?
C15 N5 Fe1 121.5(3) . . ?
C15 N5 C19 118.9(4) . . ?
C19 N5 Fe1 119.6(3) . . ?
C20 N6 Fe1 114.3(4) . . ?
C20 N6 C22 107.1(5) . . ?
C22 N6 Fe1 138.6(4) . . ?
N1 C1 C2 102.7(4) . . ?
O1 C2 C1 106.2(4) . . ?
O1 C3 C4 123.7(4) . . ?
N1 C3 O1 118.5(5) . . ?
N1 C3 C4 117.8(5) . . ?
N2 C4 C3 108.7(4) . . ?
N2 C4 C5 119.9(5) . . ?
C5 C4 C3 131.4(5) . . ?
C6 C5 C4 120.2(5) . . ?
C5 C6 C7 118.5(5) . . ?
C8 C7 C6 119.6(6) . . ?
N2 C8 C7 122.0(5) . . ?
N2 C8 C9 107.5(4) . . ?
C7 C8 C9 130.5(5) . . ?
O2 C9 C8 121.9(5) . . ?
N3 C9 O2 119.5(5) . . ?
N3 C9 C8 118.6(5) . . ?
O2 C10 C11 105.0(4) . . ?
N3 C11 C10 103.2(4) . . ?
N4 C12 C13 101.9(4) . . ?
O3 C13 C12 104.9(4) . . ?
O3 C14 C15 122.9(4) . . ?
N4 C14 O3 118.7(5) . . ?
N4 C14 C15 118.5(4) . . ?
N5 C15 C14 106.8(4) . . ?
N5 C15 C16 123.4(5) . . ?
C16 C15 C14 129.8(5) . . ?
C15 C16 C17 118.0(5) . . ?
C18 C17 C16 119.2(5) . . ?
C17 C18 C19 120.0(5) . . ?
N5 C19 C18 120.5(5) . . ?
N5 C19 C20 107.5(4) . . ?
C18 C19 C20 132.0(5) . . ?
O4 C20 C19 121.7(5) . . ?
N6 C20 O4 119.3(5) . . ?
N6 C20 C19 119.0(5) . . ?
O4 C21 C22 105.0(4) . . ?
N6 C22 C21 104.0(5) . . ?
F7 P2 F8 89.9(2) . . ?
F7 P2 F9 89.0(2) . . ?
F7 P2 F10 89.8(2) . . ?
F7 P2 F11 90.6(2) . . ?
F8 P2 F9 90.52(19) . . ?
F8 P2 F10 179.5(2) . . ?
F8 P2 F11 90.3(2) . . ?
F9 P2 F10 89.83(18) . . ?
F9 P2 F11 179.1(2) . . ?
F11 P2 F10 89.36(19) . . ?
F12 P2 F7 179.8(2) . . ?
F12 P2 F8 89.9(2) . . ?
F12 P2 F9 90.9(2) . . ?
F12 P2 F10 90.4(2) . . ?
F12 P2 F11 89.6(2) . . ?
F1 P1 F2 89.7(2) . . ?
F1 P1 F4 91.0(2) . . ?
F1 P1 F5 90.0(2) . . ?
F1 P1 F6 178.9(2) . . ?
F2 P1 F4 179.1(2) . . ?
F2 P1 F5 91.1(2) . . ?
F2 P1 F6 91.1(2) . . ?
F3 P1 F1 89.0(2) . . ?
F3 P1 F2 91.8(3) . . ?
F3 P1 F4 88.8(3) . . ?
F3 P1 F5 177.0(3) . . ?
F3 P1 F6 91.7(2) . . ?
F5 P1 F4 88.4(2) . . ?
F5 P1 F6 89.3(2) . . ?
F6 P1 F4 88.1(2) . . ?
N7 C23 C24 177.9(8) . . ?

