# Electronic Supplementary Material (ESI) for Dalton Transactions.
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#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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data_tr7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[2,6-bis(5-aminopyrazol-3-yl)pyridine]iron(II) 
diperchlorate bis(diethyl ether) nitromethane solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C22 H22 Fe N14, 2[Cl O4], 2[C4 H10 O], C H3 N O2'
_chemical_formula_sum            'C31 H45 Cl2 Fe N15 O12'
_chemical_formula_weight         946.57

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   14.5138(7)
_cell_length_b                   23.2609(11)
_cell_length_c                   12.8419(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4335.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    58012
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      29.19

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1968
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            58012
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         29.19
_reflns_number_total             5826
_reflns_number_gt                4568
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

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

 The asymmetric unit contains half a complex dication, with Fe1 lying on 
 the crystallographic C₂ site 1/2, y, 1/4; a perchlorate anion and a 
 diethyl ether molecule, both lying on general crystallographic 
 positions; and, a disordered half-molecule of nitromethane spanning 
 the C₂ axis 1/2, y, 3/4. The disordered nitromethane was modelled 
 over two sites of occupancy 0.25, subject to the fixed restraints 
 C---N = 1.48(2), N---O = 1.22(2), O...O = 2.14(2) and C...O = 
 2.32(2) Å.

 All non-H atoms except the disordered solvent were refined anisotropically,
 while C-bound H atoms were placed in calculated positions and refined using
 a riding model. The N-bound H atoms were all located in the difference map 
 and allowed to refine, subject to the refined restraint N---H = 
 0.84(2) Å. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0406P)²+1.9470P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5826
_refine_ls_number_parameters     313
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0826
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.736137(12) 0.2500 0.02323(8) Uani 1 2 d S . .
N2 N 0.57695(9) 0.73397(5) 0.39362(9) 0.0254(2) Uani 1 1 d . . .
C3 C 0.64831(11) 0.77014(6) 0.40721(11) 0.0273(3) Uani 1 1 d . . .
C4 C 0.69800(12) 0.77145(7) 0.50008(12) 0.0332(3) Uani 1 1 d . . .
H4 H 0.7479 0.7974 0.5090 0.040 Uiso 1 1 calc R . .
C5 C 0.67282(12) 0.73380(7) 0.57939(12) 0.0365(4) Uani 1 1 d . . .
H5 H 0.7058 0.7338 0.6433 0.044 Uiso 1 1 calc R . .
C6 C 0.59953(12) 0.69617(7) 0.56519(12) 0.0340(3) Uani 1 1 d . . .
H6 H 0.5819 0.6701 0.6186 0.041 Uiso 1 1 calc R . .
C7 C 0.55243(11) 0.69768(6) 0.47038(11) 0.0275(3) Uani 1 1 d . . .
C8 C 0.66585(10) 0.80710(6) 0.31651(11) 0.0264(3) Uani 1 1 d . . .
N9 N 0.61018(9) 0.79976(5) 0.23376(9) 0.0261(3) Uani 1 1 d . . .
N10 N 0.63921(9) 0.84012(5) 0.16331(10) 0.0274(3) Uani 1 1 d D . .
H10 H 0.6081(12) 0.8450(8) 0.1073(13) 0.037(5) Uiso 1 1 d D . .
C11 C 0.70976(11) 0.87198(6) 0.20120(12) 0.0297(3) Uani 1 1 d . . .
C12 C 0.72937(11) 0.85121(6) 0.30059(12) 0.0303(3) Uani 1 1 d . . .
H12 H 0.7757 0.8642 0.3472 0.036 Uiso 1 1 calc R . .
N13 N 0.75110(12) 0.91435(7) 0.14515(13) 0.0423(4) Uani 1 1 d D . .
H13A H 0.7271(14) 0.9227(8) 0.0887(14) 0.044(6) Uiso 1 1 d D . .
H13B H 0.7818(14) 0.9396(8) 0.1742(16) 0.050(6) Uiso 1 1 d D . .
C14 C 0.47185(11) 0.66247(6) 0.44387(11) 0.0270(3) Uani 1 1 d . . .
N15 N 0.43417(9) 0.67147(5) 0.34962(9) 0.0279(3) Uani 1 1 d . . .
N16 N 0.36017(10) 0.63506(6) 0.34613(10) 0.0295(3) Uani 1 1 d D . .
H16 H 0.3322(12) 0.6304(8) 0.2897(13) 0.036(5) Uiso 1 1 d D . .
C17 C 0.35277(12) 0.60329(7) 0.43458(12) 0.0319(3) Uani 1 1 d . . .
C18 C 0.42358(12) 0.62051(7) 0.50005(12) 0.0320(3) Uani 1 1 d . . .
H18 H 0.4366 0.6068 0.5682 0.038 Uiso 1 1 calc R . .
N19 N 0.28379(13) 0.56464(8) 0.44825(14) 0.0497(4) Uani 1 1 d D . .
H19A H 0.2466(14) 0.5564(9) 0.3991(15) 0.046(6) Uiso 1 1 d D . .
H19B H 0.2849(17) 0.5435(9) 0.5011(15) 0.058(7) Uiso 1 1 d D . .
Cl20 Cl 0.24257(3) 0.548755(17) 0.15150(3) 0.03640(10) Uani 1 1 d . . .
O21 O 0.29893(9) 0.49798(6) 0.16283(10) 0.0475(3) Uani 1 1 d . . .
O22 O 0.30123(11) 0.59831(6) 0.13957(11) 0.0570(4) Uani 1 1 d . . .
O23 O 0.18487(9) 0.54257(6) 0.06112(10) 0.0445(3) Uani 1 1 d . . .
O24 O 0.18607(12) 0.55562(7) 0.24291(11) 0.0605(4) Uani 1 1 d . . .
C25 C 0.47400(16) 0.93403(9) 0.1109(2) 0.0663(7) Uani 1 1 d . . .
H25A H 0.5366 0.9486 0.1215 0.099 Uiso 1 1 calc R . .
H25B H 0.4612 0.9037 0.1618 0.099 Uiso 1 1 calc R . .
H25C H 0.4297 0.9654 0.1200 0.099 Uiso 1 1 calc R . .
C26 C 0.46552(15) 0.91000(10) 0.0027(2) 0.0631(7) Uani 1 1 d . . .
H26A H 0.4017 0.8965 -0.0095 0.076 Uiso 1 1 calc R . .
H26B H 0.4797 0.9403 -0.0491 0.076 Uiso 1 1 calc R . .
O27 O 0.52860(9) 0.86299(6) -0.00884(10) 0.0455(3) Uani 1 1 d . . .
C28 C 0.53348(16) 0.84175(11) -0.11294(16) 0.0599(6) Uani 1 1 d . . .
H28A H 0.5479 0.8736 -0.1613 0.072 Uiso 1 1 calc R . .
H28B H 0.4733 0.8251 -0.1333 0.072 Uiso 1 1 calc R . .
C29 C 0.60698(18) 0.79664(11) -0.11937(18) 0.0646(6) Uani 1 1 d . . .
H29A H 0.5937 0.7660 -0.0692 0.097 Uiso 1 1 calc R . .
H29B H 0.6669 0.8139 -0.1032 0.097 Uiso 1 1 calc R . .
H29C H 0.6084 0.7805 -0.1899 0.097 Uiso 1 1 calc R . .
C30A C 0.4874(5) 0.4826(3) 0.8086(5) 0.0337(14) Uiso 0.25 1 d PD A 1
H30A H 0.5247 0.4481 0.7964 0.051 Uiso 0.25 1 calc PR A 1
H30B H 0.4221 0.4733 0.7994 0.051 Uiso 0.25 1 calc PR A 1
H30C H 0.4978 0.4964 0.8798 0.051 Uiso 0.25 1 calc PR A 1
N31A N 0.5145(8) 0.5282(3) 0.7332(9) 0.033(3) Uiso 0.25 1 d PD . 1
O32A O 0.4725(6) 0.5752(4) 0.7543(5) 0.0564(19) Uiso 0.25 1 d PD . 1
O33A O 0.5502(6) 0.5087(4) 0.6543(6) 0.063(2) Uiso 0.25 1 d PD . 1
C30B C 0.5000 0.4707(3) 0.7500 0.078(2) Uiso 0.50 2 d SPD B 2
H30D H 0.5291 0.4434 0.7021 0.118 Uiso 0.25 1 calc PR B 2
H30E H 0.4332 0.4647 0.7498 0.118 Uiso 0.25 1 calc PR B 2
H30F H 0.5240 0.4646 0.8205 0.118 Uiso 0.25 1 calc PR B 2
N31B N 0.5198(11) 0.5272(5) 0.7179(10) 0.062(5) Uiso 0.25 1 d PD . 2
O32B O 0.5611(6) 0.5229(4) 0.6389(6) 0.065(3) Uiso 0.25 1 d PD C 2
O33B O 0.5000 0.5762(3) 0.7500 0.0497(17) Uiso 0.50 2 d SPD . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1567(12) . ?
Fe1 N9 2.1888(13) . ?
Fe1 N15 2.1936(12) . ?
N2 C7 1.3458(18) . ?
N2 C3 1.3457(19) . ?
C3 C4 1.394(2) . ?
C3 C8 1.470(2) . ?
C4 C5 1.392(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(2) . ?
C6 H6 0.9500 . ?
C7 C14 1.468(2) . ?
C8 N9 1.3458(18) . ?
C8 C12 1.394(2) . ?
N9 N10 1.3702(17) . ?
N10 C11 1.354(2) . ?
N10 H10 0.857(16) . ?
C11 N13 1.360(2) . ?
C11 C12 1.394(2) . ?
C12 H12 0.9500 . ?
N13 H13A 0.827(16) . ?
N13 H13B 0.827(17) . ?
C14 N15 1.3447(18) . ?
C14 C18 1.401(2) . ?
N15 N16 1.3686(18) . ?
N16 C17 1.3594(19) . ?
N16 H16 0.837(15) . ?
C17 N19 1.357(2) . ?
C17 C18 1.387(2) . ?
C18 H18 0.9500 . ?
N19 H19A 0.852(17) . ?
N19 H19B 0.839(17) . ?
Cl20 O23 1.4384(13) . ?
Cl20 O24 1.4409(15) . ?
Cl20 O22 1.4412(14) . ?
Cl20 O21 1.4441(13) . ?
C25 C26 1.504(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O27 1.434(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O27 C28 1.427(3) . ?
C28 C29 1.499(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30A N31A 1.490(10) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
N31A O33A 1.225(12) . ?
N31A O32A 1.279(10) . ?
C30B N31B 1.408(12) . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
N31B O32B 1.182(12) . ?
N31B O33B 1.247(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
N2 Fe1 N2 177.33(6) 4_655 . ?
N2 Fe1 N9 73.67(5) . . ?
N2 Fe1 N9 108.22(4) . 4_655 ?
N9 Fe1 N9 94.92(7) . 4_655 ?
N2 Fe1 N15 73.19(5) . . ?
N9 Fe1 N15 146.87(5) . . ?
N2 Fe1 N15 104.90(5) . 4_655 ?
N9 Fe1 N15 95.15(5) . 4_655 ?
N15 Fe1 N15 93.42(7) . 4_655 ?
C7 N2 C3 120.05(13) . . ?
C7 N2 Fe1 120.27(10) . . ?
C3 N2 Fe1 119.66(9) . . ?
N2 C3 C4 121.52(14) . . ?
N2 C3 C8 113.34(12) . . ?
C4 C3 C8 125.14(14) . . ?
C5 C4 C3 118.45(15) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C6 C5 C4 120.08(15) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 118.25(15) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
N2 C7 C6 121.65(15) . . ?
N2 C7 C14 113.01(13) . . ?
C6 C7 C14 125.32(14) . . ?
N9 C8 C12 112.00(13) . . ?
N9 C8 C3 116.58(13) . . ?
C12 C8 C3 131.38(13) . . ?
C8 N9 N10 104.46(12) . . ?
C8 N9 Fe1 116.69(9) . . ?
N10 N9 Fe1 138.66(9) . . ?
C11 N10 N9 111.73(12) . . ?
C11 N10 H10 128.8(13) . . ?
N9 N10 H10 118.9(13) . . ?
N10 C11 N13 122.68(15) . . ?
N10 C11 C12 107.08(13) . . ?
N13 C11 C12 130.21(15) . . ?
C11 C12 C8 104.73(13) . . ?
C11 C12 H12 127.6 . . ?
C8 C12 H12 127.6 . . ?
C11 N13 H13A 116.7(14) . . ?
C11 N13 H13B 120.9(15) . . ?
H13A N13 H13B 117(2) . . ?
N15 C14 C18 111.63(14) . . ?
N15 C14 C7 116.48(13) . . ?
C18 C14 C7 131.88(14) . . ?
C14 N15 N16 104.61(12) . . ?
C14 N15 Fe1 117.04(10) . . ?
N16 N15 Fe1 138.34(10) . . ?
C17 N16 N15 111.78(13) . . ?
C17 N16 H16 127.9(13) . . ?
N15 N16 H16 119.2(13) . . ?
N19 C17 N16 121.77(16) . . ?
N19 C17 C18 131.28(15) . . ?
N16 C17 C18 106.92(14) . . ?
C17 C18 C14 105.04(13) . . ?
C17 C18 H18 127.5 . . ?
C14 C18 H18 127.5 . . ?
C17 N19 H19A 121.3(15) . . ?
C17 N19 H19B 118.6(17) . . ?
H19A N19 H19B 119(2) . . ?
O23 Cl20 O24 109.70(9) . . ?
O23 Cl20 O22 109.77(8) . . ?
O24 Cl20 O22 109.52(10) . . ?
O23 Cl20 O21 109.23(8) . . ?
O24 Cl20 O21 109.33(9) . . ?
O22 Cl20 O21 109.29(9) . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O27 C26 C25 109.05(17) . . ?
O27 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
O27 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
C28 O27 C26 113.10(16) . . ?
O27 C28 C29 109.24(16) . . ?
O27 C28 H28A 109.8 . . ?
C29 C28 H28A 109.8 . . ?
O27 C28 H28B 109.8 . . ?
C29 C28 H28B 109.8 . . ?
H28A C28 H28B 108.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N31A C30A H30A 109.5 . . ?
N31A C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
N31A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
O33A N31A O32A 133.9(10) . . ?
O33A N31A C30A 112.6(7) . . ?
O32A N31A C30A 110.2(8) . . ?
N31B C30B H30D 109.5 . . ?
N31B C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
N31B C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
O32B N31B O33B 118.6(10) . . ?
O32B N31B C30B 106.0(9) . . ?
O33B N31B C30B 135.3(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 O27 0.857(16) 1.932(16) 2.7835(18) 172.6(18) .
N13 H13A O23 0.827(16) 2.175(17) 2.991(2) 169(2) 3_565
N13 H13B O21 0.827(17) 2.507(19) 3.217(2) 144.6(19) 6_666
N16 H16 O22 0.837(15) 2.116(16) 2.9153(19) 159.6(18) .
N19 H19A O24 0.852(17) 2.190(18) 3.001(2) 159(2) .
N19 H19B O21 0.839(17) 2.299(18) 3.125(2) 168(2) 8_566
N19 H19B O23 0.839(17) 2.59(2) 3.222(2) 133(2) 8_566

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.19
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 982126'
#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_tdr35_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis-[2,6-bis{5-tertbutylcarboxamido-1H-pyrazol-3-yl}pyridine]iron(II)
di-tetrafluoroborate tris-acetonitrile solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H54 Fe N14 O4, 2[B F4], 3[C2 H3 N]'
_chemical_formula_sum            'C48 H63 B2 F8 Fe N17 O4'
_chemical_formula_weight         1171.62

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'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   12.8890(4)
_cell_length_b                   13.3521(4)
_cell_length_c                   19.1548(6)
_cell_angle_alpha                104.759(2)
_cell_angle_beta                 100.581(2)
_cell_angle_gamma                108.536(2)
_cell_volume                     2893.71(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    61654
_cell_measurement_theta_min      1.71
_cell_measurement_theta_max      32.68

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1220
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            61654
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         32.68
_reflns_number_total             20577
_reflns_number_gt                15523
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

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

 Two of the four tert-butyl groups in the molecule are disordered:
    C28-C31 was refined over two half-occupied sites sharing a common 
 wholly occupied bridgehead C atom C28;
    and, C46-C49 was modelled over three orientations with occupancies 
 of 0.50, 0.25 and 0.25.
 The refined restraints C---C = 1.52(2) and 1,3-C...C = 2.48(2) Å were 
 applied to these groups.

 All non-H atoms with occupancy >=0.5 were refined anisotropically, while 
 H atoms were placed in calculated positions and refined using a riding 
 model. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0554P)²+0.9463P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         20577
_refine_ls_number_parameters     790
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1290
_refine_ls_wR_factor_gt          0.1170
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.240061(16) 0.011420(15) 0.256817(10) 0.01654(5) Uani 1 1 d . . .
N2 N 0.37802(9) 0.10230(9) 0.35792(6) 0.0186(2) Uani 1 1 d . . .
C3 C 0.38710(11) 0.20352(11) 0.40145(7) 0.0201(2) Uani 1 1 d . . .
C4 C 0.46676(13) 0.25922(12) 0.47240(8) 0.0261(3) Uani 1 1 d . . .
H4 H 0.4718 0.3298 0.5031 0.031 Uiso 1 1 calc R . .
C5 C 0.53868(13) 0.20889(12) 0.49704(8) 0.0287(3) Uani 1 1 d . . .
H5 H 0.5935 0.2452 0.5453 0.034 Uiso 1 1 calc R . .
C6 C 0.53094(12) 0.10514(12) 0.45130(8) 0.0249(3) Uani 1 1 d . . .
H6 H 0.5808 0.0708 0.4673 0.030 Uiso 1 1 calc R . .
C7 C 0.44795(11) 0.05375(11) 0.38166(7) 0.0193(2) Uani 1 1 d . . .
C8 C 0.30605(11) 0.24530(11) 0.36600(7) 0.0199(2) Uani 1 1 d . . .
N9 N 0.23431(10) 0.17755(9) 0.29775(6) 0.0194(2) Uani 1 1 d . . .
N10 N 0.17131(10) 0.23471(9) 0.27707(6) 0.0207(2) Uani 1 1 d . . .
H10 H 0.1173 0.2095 0.2341 0.025 Uiso 1 1 calc R . .
C11 C 0.20189(12) 0.33583(11) 0.33083(8) 0.0223(3) Uani 1 1 d . . .
C12 C 0.28945(12) 0.34633(11) 0.38959(8) 0.0247(3) Uani 1 1 d . . .
H12 H 0.3292 0.4076 0.4353 0.030 Uiso 1 1 calc R . .
N13 N 0.14391(11) 0.40430(10) 0.31818(7) 0.0281(3) Uani 1 1 d . . .
H13 H 0.0778 0.3734 0.2830 0.034 Uiso 1 1 calc R . .
C14 C 0.18313(14) 0.51672(12) 0.35703(10) 0.0335(3) Uani 1 1 d . . .
O15 O 0.27263(14) 0.56309(11) 0.40656(12) 0.0864(8) Uani 1 1 d . . .
C16 C 0.10518(13) 0.57634(12) 0.33399(9) 0.0287(3) Uani 1 1 d . . .
C17 C 0.00527(16) 0.54572(17) 0.36825(12) 0.0443(4) Uani 1 1 d . . .
H17A H -0.0429 0.5872 0.3579 0.067 Uiso 1 1 calc R . .
H17B H 0.0354 0.5654 0.4229 0.067 Uiso 1 1 calc R . .
H17C H -0.0404 0.4650 0.3458 0.067 Uiso 1 1 calc R . .
C18 C 0.05954(16) 0.54170(15) 0.24794(10) 0.0382(4) Uani 1 1 d . . .
H18A H 0.1238 0.5554 0.2263 0.057 Uiso 1 1 calc R . .
H18B H 0.0155 0.5858 0.2355 0.057 Uiso 1 1 calc R . .
H18C H 0.0102 0.4618 0.2271 0.057 Uiso 1 1 calc R . .
C19 C 0.17516(15) 0.70307(13) 0.36637(11) 0.0375(4) Uani 1 1 d . . .
H19A H 0.2435 0.7204 0.3489 0.056 Uiso 1 1 calc R . .
H19B H 0.1980 0.7272 0.4216 0.056 Uiso 1 1 calc R . .
H19C H 0.1287 0.7426 0.3494 0.056 Uiso 1 1 calc R . .
C20 C 0.42433(11) -0.05792(11) 0.32856(7) 0.0194(2) Uani 1 1 d . . .
N21 N 0.33408(10) -0.10026(9) 0.26657(6) 0.0192(2) Uani 1 1 d . . .
N22 N 0.32941(10) -0.20434(9) 0.23028(6) 0.0204(2) Uani 1 1 d . . .
H22 H 0.2780 -0.2511 0.1876 0.024 Uiso 1 1 calc R . .
C23 C 0.41407(11) -0.22647(11) 0.26832(7) 0.0202(2) Uani 1 1 d . . .
C24 C 0.47846(12) -0.13302(11) 0.33258(8) 0.0212(2) Uani 1 1 d . . .
H24 H 0.5438 -0.1227 0.3703 0.025 Uiso 1 1 calc R . .
N25 N 0.43063(11) -0.32657(10) 0.24608(7) 0.0244(2) Uani 1 1 d . . .
H25 H 0.4926 -0.3300 0.2719 0.029 Uiso 1 1 calc R . .
C26 C 0.35674(13) -0.42051(12) 0.18654(8) 0.0251(3) Uani 1 1 d D A .
O27 O 0.27160(10) -0.41946(9) 0.14731(7) 0.0369(3) Uani 1 1 d . . .
C28 C 0.38904(14) -0.52371(12) 0.17173(9) 0.0308(3) Uani 1 1 d D . .
C29A C 0.4609(14) -0.5183(13) 0.1169(10) 0.094(4) Uani 0.50 1 d PD A 1
H29A H 0.4196 -0.5103 0.0716 0.141 Uiso 0.50 1 calc PR A 1
H29B H 0.4755 -0.5873 0.1029 0.141 Uiso 0.50 1 calc PR A 1
H29C H 0.5337 -0.4537 0.1410 0.141 Uiso 0.50 1 calc PR A 1
C30A C 0.2778(6) -0.6290(6) 0.1324(5) 0.0481(16) Uani 0.50 1 d PD A 1
H30A H 0.2343 -0.6207 0.0880 0.072 Uiso 0.50 1 calc PR A 1
H30B H 0.2318 -0.6378 0.1675 0.072 Uiso 0.50 1 calc PR A 1
H30C H 0.2966 -0.6953 0.1167 0.072 Uiso 0.50 1 calc PR A 1
C31A C 0.4502(10) -0.5375(7) 0.2408(4) 0.065(3) Uani 0.50 1 d PD A 1
H31A H 0.4670 -0.6052 0.2263 0.098 Uiso 0.50 1 calc PR A 1
H31B H 0.4018 -0.5444 0.2746 0.098 Uiso 0.50 1 calc PR A 1
H31C H 0.5217 -0.4719 0.2667 0.098 Uiso 0.50 1 calc PR A 1
C29B C 0.4869(14) -0.4985(14) 0.1376(11) 0.114(6) Uani 0.50 1 d PD A 2
H29D H 0.5524 -0.4332 0.1737 0.171 Uiso 0.50 1 calc PR A 2
H29E H 0.4633 -0.4823 0.0915 0.171 Uiso 0.50 1 calc PR A 2
H29F H 0.5086 -0.5635 0.1254 0.171 Uiso 0.50 1 calc PR A 2
C30B C 0.2869(9) -0.6223(7) 0.1178(7) 0.116(5) Uani 0.50 1 d PD A 2
H30D H 0.3054 -0.6893 0.1074 0.174 Uiso 0.50 1 calc PR A 2
H30E H 0.2651 -0.6079 0.0707 0.174 Uiso 0.50 1 calc PR A 2
H30F H 0.2232 -0.6341 0.1400 0.174 Uiso 0.50 1 calc PR A 2
C31B C 0.4269(10) -0.5428(8) 0.2463(5) 0.056(3) Uani 0.50 1 d PD A 2
H31D H 0.4914 -0.4755 0.2813 0.084 Uiso 0.50 1 calc PR A 2
H31E H 0.4504 -0.6068 0.2369 0.084 Uiso 0.50 1 calc PR A 2
H31F H 0.3632 -0.5582 0.2684 0.084 Uiso 0.50 1 calc PR A 2
N32 N 0.06646(10) -0.08250(9) 0.18619(6) 0.0188(2) Uani 1 1 d . . .
C33 C 0.04229(11) -0.09288(11) 0.11273(7) 0.0194(2) Uani 1 1 d . . .
C34 C -0.06666(12) -0.15864(12) 0.06305(8) 0.0252(3) Uani 1 1 d . . .
H34 H -0.0828 -0.1649 0.0113 0.030 Uiso 1 1 calc R . .
C35 C -0.15086(13) -0.21470(13) 0.09115(8) 0.0299(3) Uani 1 1 d . . .
H35 H -0.2254 -0.2609 0.0584 0.036 Uiso 1 1 calc R . .
C36 C -0.12603(13) -0.20325(13) 0.16737(8) 0.0280(3) Uani 1 1 d . . .
H36 H -0.1830 -0.2406 0.1873 0.034 Uiso 1 1 calc R . .
C37 C -0.01588(11) -0.13581(11) 0.21338(7) 0.0204(2) Uani 1 1 d . . .
C38 C 0.14142(11) -0.03175(11) 0.09186(7) 0.0193(2) Uani 1 1 d . . .
N39 N 0.24169(10) 0.02354(9) 0.14640(6) 0.0199(2) Uani 1 1 d . . .
N40 N 0.31780(10) 0.07107(10) 0.11222(6) 0.0215(2) Uani 1 1 d . . .
H40 H 0.3905 0.1129 0.1352 0.026 Uiso 1 1 calc R . .
C41 C 0.26705(12) 0.04566(12) 0.03809(7) 0.0227(3) Uani 1 1 d . . .
C42 C 0.15234(12) -0.01976(12) 0.02275(7) 0.0240(3) Uani 1 1 d . . .
H42 H 0.0944 -0.0496 -0.0240 0.029 Uiso 1 1 calc R . .
N43 N 0.32444(11) 0.07605(11) -0.01275(7) 0.0290(3) Uani 1 1 d . B .
H43 H 0.2863 0.0466 -0.0610 0.035 Uiso 1 1 calc R . .
C44 C 0.43541(14) 0.14803(14) 0.00663(9) 0.0299(3) Uani 1 1 d D . .
O45 O 0.48890(11) 0.19968(12) 0.07293(7) 0.0483(4) Uani 1 1 d . B .
C46A C 0.4864(6) 0.1510(8) -0.0615(4) 0.0305(15) Uani 0.50 1 d PD B 1
C47A C 0.4501(9) 0.2272(9) -0.0949(6) 0.141(6) Uani 0.50 1 d PD B 1
H47A H 0.4757 0.3009 -0.0562 0.211 Uiso 0.50 1 calc PR B 1
H47B H 0.3665 0.1962 -0.1147 0.211 Uiso 0.50 1 calc PR B 1
H47C H 0.4839 0.2348 -0.1361 0.211 Uiso 0.50 1 calc PR B 1
C48A C 0.4459(4) 0.0345(4) -0.1232(2) 0.0545(13) Uani 0.50 1 d PD B 1
H48A H 0.4701 -0.0162 -0.1014 0.082 Uiso 0.50 1 calc PR B 1
H48B H 0.4796 0.0426 -0.1643 0.082 Uiso 0.50 1 calc PR B 1
H48C H 0.3624 0.0034 -0.1429 0.082 Uiso 0.50 1 calc PR B 1
C49A C 0.6168(4) 0.1929(6) -0.0312(3) 0.071(2) Uani 0.50 1 d PD B 1
H49A H 0.6459 0.2667 0.0080 0.107 Uiso 0.50 1 calc PR B 1
H49B H 0.6508 0.1989 -0.0725 0.107 Uiso 0.50 1 calc PR B 1
H49C H 0.6369 0.1399 -0.0099 0.107 Uiso 0.50 1 calc PR B 1
C46B C 0.4861(14) 0.1680(13) -0.0566(9) 0.029(6) Uiso 0.25 1 d PD B 2
C47B C 0.4108(8) 0.1953(8) -0.1139(5) 0.0317(16) Uiso 0.25 1 d PD B 2
H47D H 0.4480 0.2085 -0.1528 0.048 Uiso 0.25 1 calc PR B 2
H47E H 0.3991 0.2627 -0.0884 0.048 Uiso 0.25 1 calc PR B 2
H47F H 0.3367 0.1322 -0.1373 0.048 Uiso 0.25 1 calc PR B 2
C48B C 0.5010(10) 0.0597(8) -0.0932(6) 0.064(3) Uiso 0.25 1 d PD B 2
H48D H 0.5496 0.0441 -0.0552 0.096 Uiso 0.25 1 calc PR B 2
H48E H 0.5368 0.0679 -0.1335 0.096 Uiso 0.25 1 calc PR B 2
H48F H 0.4261 -0.0024 -0.1145 0.096 Uiso 0.25 1 calc PR B 2
C49B C 0.6010(7) 0.2677(7) -0.0253(5) 0.0488(19) Uiso 0.25 1 d PD B 2
H49D H 0.6516 0.2561 0.0140 0.073 Uiso 0.25 1 calc PR B 2
H49E H 0.5890 0.3366 -0.0037 0.073 Uiso 0.25 1 calc PR B 2
H49F H 0.6361 0.2745 -0.0660 0.073 Uiso 0.25 1 calc PR B 2
C46C C 0.4900(14) 0.1690(14) -0.0547(9) 0.048(9) Uiso 0.25 1 d PD B 3
C47C C 0.5127(9) 0.2883(7) -0.0527(5) 0.048(2) Uiso 0.25 1 d PD B 3
H47G H 0.4400 0.2980 -0.0643 0.072 Uiso 0.25 1 calc PR B 3
H47H H 0.5524 0.3036 -0.0902 0.072 Uiso 0.25 1 calc PR B 3
H47I H 0.5604 0.3404 -0.0024 0.072 Uiso 0.25 1 calc PR B 3
C48C C 0.4147(7) 0.0884(7) -0.1330(4) 0.0461(18) Uiso 0.25 1 d PD B 3
H48G H 0.4032 0.0113 -0.1354 0.069 Uiso 0.25 1 calc PR B 3
H48H H 0.4519 0.1065 -0.1709 0.069 Uiso 0.25 1 calc PR B 3
H48I H 0.3405 0.0957 -0.1428 0.069 Uiso 0.25 1 calc PR B 3
C49C C 0.5988(8) 0.1484(8) -0.0373(6) 0.041(2) Uiso 0.25 1 d PD B 3
H49G H 0.5809 0.0725 -0.0348 0.061 Uiso 0.25 1 calc PR B 3
H49H H 0.6503 0.2033 0.0113 0.061 Uiso 0.25 1 calc PR B 3
H49I H 0.6360 0.1558 -0.0770 0.061 Uiso 0.25 1 calc PR B 3
C50 C 0.02487(11) -0.11469(11) 0.29473(7) 0.0198(2) Uani 1 1 d . . .
N51 N 0.13496(10) -0.04663(9) 0.32882(6) 0.0191(2) Uani 1 1 d . . .
N52 N 0.15187(10) -0.03917(9) 0.40224(6) 0.0197(2) Uani 1 1 d . . .
H52 H 0.2171 0.0012 0.4377 0.024 Uiso 1 1 calc R . .
C53 C 0.05527(12) -0.10198(11) 0.41388(7) 0.0210(2) Uani 1 1 d . . .
C54 C -0.02981(12) -0.15220(12) 0.34574(8) 0.0226(3) Uani 1 1 d . . .
H54 H -0.1070 -0.2006 0.3358 0.027 Uiso 1 1 calc R . .
N55 N 0.05271(10) -0.11286(10) 0.48409(6) 0.0234(2) Uani 1 1 d . . .
H55 H -0.0142 -0.1420 0.4915 0.028 Uiso 1 1 calc R . .
C56 C 0.14963(12) -0.08026(12) 0.54242(8) 0.0228(3) Uani 1 1 d . . .
O57 O 0.24461(9) -0.02913(9) 0.53777(6) 0.0282(2) Uani 1 1 d . . .
C58 C 0.13463(13) -0.11501(14) 0.61127(8) 0.0277(3) Uani 1 1 d . . .
C59 C 0.21233(17) -0.01399(18) 0.68227(9) 0.0440(4) Uani 1 1 d . . .
H59A H 0.2919 0.0072 0.6809 0.066 Uiso 1 1 calc R . .
H59B H 0.2055 -0.0344 0.7273 0.066 Uiso 1 1 calc R . .
H59C H 0.1890 0.0494 0.6836 0.066 Uiso 1 1 calc R . .
C60 C 0.1774(2) -0.21046(19) 0.60638(13) 0.0501(5) Uani 1 1 d . . .
H60A H 0.1264 -0.2761 0.5626 0.075 Uiso 1 1 calc R . .
H60B H 0.1784 -0.2301 0.6524 0.075 Uiso 1 1 calc R . .
H60C H 0.2549 -0.1864 0.6010 0.075 Uiso 1 1 calc R . .
C61 C 0.01182(14) -0.15202(16) 0.61575(9) 0.0355(4) Uani 1 1 d . . .
H61A H -0.0166 -0.0926 0.6137 0.053 Uiso 1 1 calc R . .
H61B H 0.0097 -0.1666 0.6632 0.053 Uiso 1 1 calc R . .
H61C H -0.0364 -0.2206 0.5732 0.053 Uiso 1 1 calc R . .
B62 B 0.71580(15) -0.30948(16) 0.39566(11) 0.0316(4) Uani 1 1 d . . .
F63 F 0.64397(13) -0.27046(11) 0.35821(9) 0.0803(5) Uani 1 1 d . . .
F64 F 0.75809(12) -0.36623(11) 0.34384(8) 0.0641(4) Uani 1 1 d . . .
F65 F 0.80506(9) -0.21853(10) 0.45122(6) 0.0485(3) Uani 1 1 d . . .
F66 F 0.65449(12) -0.38331(10) 0.42609(7) 0.0568(3) Uani 1 1 d . . .
B67 B -0.10572(16) 0.18492(16) 0.16233(10) 0.0317(4) Uani 1 1 d . . .
F68 F -0.17402(11) 0.20772(11) 0.10974(6) 0.0538(3) Uani 1 1 d . . .
F69 F -0.15235(12) 0.07292(9) 0.15585(6) 0.0557(3) Uani 1 1 d . . .
F70 F 0.00240(9) 0.20672(12) 0.14978(6) 0.0523(3) Uani 1 1 d . . .
F71 F -0.09007(10) 0.25319(9) 0.23545(5) 0.0432(3) Uani 1 1 d . . .
C72 C 0.6573(2) 0.37296(17) 0.36611(14) 0.0566(6) Uani 1 1 d . . .
H72A H 0.6252 0.4310 0.3738 0.085 Uiso 1 1 calc R . .
H72B H 0.7323 0.4029 0.3580 0.085 Uiso 1 1 calc R . .
H72C H 0.6654 0.3498 0.4107 0.085 Uiso 1 1 calc R . .
C73 C 0.58038(16) 0.27574(16) 0.29978(11) 0.0407(4) Uani 1 1 d . . .
N74 N 0.52029(15) 0.20140(15) 0.24882(10) 0.0487(4) Uani 1 1 d . . .
C75 C 0.7305(2) 0.4114(2) 0.18360(15) 0.0628(6) Uani 1 1 d . . .
H75A H 0.7879 0.3800 0.1957 0.094 Uiso 1 1 calc R . .
H75B H 0.6551 0.3505 0.1597 0.094 Uiso 1 1 calc R . .
H75C H 0.7294 0.4626 0.2300 0.094 Uiso 1 1 calc R . .
C76 C 0.7589(3) 0.4721(2) 0.13246(19) 0.0779(8) Uani 1 1 d . . .
N77 N 0.7823(4) 0.5198(3) 0.0925(2) 0.1300(14) Uani 1 1 d . . .
C78 C 0.0065(2) -0.39180(18) -0.04079(12) 0.0569(6) Uani 1 1 d . . .
H78A H -0.0723 -0.4329 -0.0423 0.085 Uiso 1 1 calc R . .
H78B H 0.0366 -0.4444 -0.0669 0.085 Uiso 1 1 calc R . .
H78C H 0.0078 -0.3360 -0.0658 0.085 Uiso 1 1 calc R . .
C79 C 0.07651(15) -0.33556(14) 0.03713(10) 0.0362(4) Uani 1 1 d . . .
N80 N 0.13046(15) -0.29239(14) 0.09800(10) 0.0495(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1333(11) . ?
Fe1 N32 2.1562(11) . ?
Fe1 N39 2.1654(11) . ?
Fe1 N9 2.1864(11) . ?
Fe1 N51 2.2138(11) . ?
Fe1 N21 2.2214(11) . ?
N2 C7 1.3456(17) . ?
N2 C3 1.3509(16) . ?
C3 C4 1.3932(19) . ?
C3 C8 1.4720(19) . ?
C4 C5 1.389(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.3919(18) . ?
C6 H6 0.9500 . ?
C7 C20 1.4749(18) . ?
C8 N9 1.3432(16) . ?
C8 C12 1.4064(19) . ?
N9 N10 1.3523(16) . ?
N10 C11 1.3576(17) . ?
N10 H10 0.8800 . ?
C11 C12 1.383(2) . ?
C11 N13 1.3905(18) . ?
C12 H12 0.9500 . ?
N13 C14 1.3684(18) . ?
N13 H13 0.8800 . ?
C14 O15 1.208(2) . ?
C14 C16 1.537(2) . ?
C16 C19 1.533(2) . ?
C16 C18 1.536(2) . ?
C16 C17 1.539(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N21 1.3473(17) . ?
C20 C24 1.4009(19) . ?
N21 N22 1.3629(15) . ?
N22 C23 1.3532(17) . ?
N22 H22 0.8800 . ?
C23 N25 1.3922(17) . ?
C23 C24 1.3944(18) . ?
C24 H24 0.9500 . ?
N25 C26 1.3762(18) . ?
N25 H25 0.8800 . ?
C26 O27 1.2172(18) . ?
C26 C28 1.537(2) . ?
C28 C31A 1.496(7) . ?
C28 C29A 1.522(8) . ?
C28 C30A 1.543(6) . ?
C28 C30B 1.496(8) . ?
C28 C29B 1.509(9) . ?
C28 C31B 1.534(8) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
N32 C33 1.3448(16) . ?
N32 C37 1.3474(17) . ?
C33 C34 1.3957(19) . ?
C33 C38 1.4661(18) . ?
C34 C35 1.390(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.393(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.388(2) . ?
C36 H36 0.9500 . ?
C37 C50 1.4714(18) . ?
C38 N39 1.3458(17) . ?
C38 C42 1.3999(18) . ?
N39 N40 1.3584(15) . ?
N40 C41 1.3533(17) . ?
N40 H40 0.8800 . ?
C41 C42 1.387(2) . ?
C41 N43 1.3912(17) . ?
C42 H42 0.9500 . ?
N43 C44 1.363(2) . ?
N43 H43 0.8800 . ?
C44 O45 1.222(2) . ?
C44 C46C 1.516(15) . ?
C44 C46B 1.520(15) . ?
C44 C46A 1.569(6) . ?
C46A C47A 1.480(9) . ?
C46A C49A 1.533(8) . ?
C46A C48A 1.553(10) . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C49A H49A 0.9800 . ?
C49A H49B 0.9800 . ?
C49A H49C 0.9800 . ?
C46B C47B 1.521(15) . ?
C46B C48B 1.526(15) . ?
C46B C49B 1.530(15) . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
C46C C49C 1.508(16) . ?
C46C C47C 1.515(16) . ?
C46C C48C 1.526(16) . ?
C47C H47G 0.9800 . ?
C47C H47H 0.9800 . ?
C47C H47I 0.9800 . ?
C48C H48G 0.9800 . ?
C48C H48H 0.9800 . ?
C48C H48I 0.9800 . ?
C49C H49G 0.9800 . ?
C49C H49H 0.9800 . ?
C49C H49I 0.9800 . ?
C50 N51 1.3428(17) . ?
C50 C54 1.4072(18) . ?
N51 N52 1.3556(15) . ?
N52 C53 1.3552(17) . ?
N52 H52 0.8800 . ?
C53 C54 1.3845(19) . ?
C53 N55 1.3940(16) . ?
C54 H54 0.9500 . ?
N55 C56 1.3756(18) . ?
N55 H55 0.8800 . ?
C56 O57 1.2297(18) . ?
C56 C58 1.5298(19) . ?
C58 C61 1.527(2) . ?
C58 C60 1.531(2) . ?
C58 C59 1.542(2) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
B62 F63 1.377(2) . ?
B62 F66 1.379(2) . ?
B62 F65 1.391(2) . ?
B62 F64 1.391(2) . ?
B67 F68 1.372(2) . ?
B67 F69 1.386(2) . ?
B67 F71 1.401(2) . ?
B67 F70 1.409(2) . ?
C72 C73 1.470(3) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 N74 1.130(3) . ?
C75 C76 1.449(4) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 N77 1.137(4) . ?
C78 C79 1.453(3) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 N80 1.131(2) . ?

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 N32 158.30(4) . . ?
N2 Fe1 N39 125.84(4) . . ?
N32 Fe1 N39 74.46(4) . . ?
N2 Fe1 N9 73.99(4) . . ?
N32 Fe1 N9 99.88(4) . . ?
N39 Fe1 N9 92.19(4) . . ?
N2 Fe1 N51 86.73(4) . . ?
N32 Fe1 N51 72.32(4) . . ?
N39 Fe1 N51 146.60(4) . . ?
N9 Fe1 N51 90.13(4) . . ?
N2 Fe1 N21 74.47(4) . . ?
N32 Fe1 N21 111.41(4) . . ?
N39 Fe1 N21 102.06(4) . . ?
N9 Fe1 N21 148.03(4) . . ?
N51 Fe1 N21 93.16(4) . . ?
C7 N2 C3 120.45(11) . . ?
C7 N2 Fe1 119.78(8) . . ?
C3 N2 Fe1 119.42(9) . . ?
N2 C3 C4 121.29(12) . . ?
N2 C3 C8 113.20(11) . . ?
C4 C3 C8 125.51(12) . . ?
C5 C4 C3 118.26(13) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C4 C5 C6 120.48(13) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 117.95(13) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
N2 C7 C6 121.56(12) . . ?
N2 C7 C20 113.54(11) . . ?
C6 C7 C20 124.86(12) . . ?
N9 C8 C12 111.74(12) . . ?
N9 C8 C3 116.29(11) . . ?
C12 C8 C3 131.96(12) . . ?
C8 N9 N10 104.99(10) . . ?
C8 N9 Fe1 116.22(9) . . ?
N10 N9 Fe1 138.55(8) . . ?
N9 N10 C11 111.53(11) . . ?
N9 N10 H10 124.2 . . ?
C11 N10 H10 124.2 . . ?
N10 C11 C12 107.75(12) . . ?
N10 C11 N13 118.44(12) . . ?
C12 C11 N13 133.81(13) . . ?
C11 C12 C8 104.00(12) . . ?
C11 C12 H12 128.0 . . ?
C8 C12 H12 128.0 . . ?
C14 N13 C11 124.14(13) . . ?
C14 N13 H13 117.9 . . ?
C11 N13 H13 117.9 . . ?
O15 C14 N13 120.65(15) . . ?
O15 C14 C16 123.82(14) . . ?
N13 C14 C16 115.53(13) . . ?
C19 C16 C18 108.90(14) . . ?
C19 C16 C14 108.08(12) . . ?
C18 C16 C14 111.93(13) . . ?
C19 C16 C17 110.24(14) . . ?
C18 C16 C17 110.15(14) . . ?
C14 C16 C17 107.51(14) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N21 C20 C24 111.94(11) . . ?
N21 C20 C7 117.50(11) . . ?
C24 C20 C7 130.51(12) . . ?
C20 N21 N22 104.96(10) . . ?
C20 N21 Fe1 114.52(8) . . ?
N22 N21 Fe1 140.47(9) . . ?
C23 N22 N21 111.23(11) . . ?
C23 N22 H22 124.4 . . ?
N21 N22 H22 124.4 . . ?
N22 C23 N25 124.75(12) . . ?
N22 C23 C24 107.98(11) . . ?
N25 C23 C24 127.27(13) . . ?
C23 C24 C20 103.89(12) . . ?
C23 C24 H24 128.1 . . ?
C20 C24 H24 128.1 . . ?
C26 N25 C23 124.50(12) . . ?
C26 N25 H25 117.7 . . ?
C23 N25 H25 117.7 . . ?
O27 C26 N25 120.65(13) . . ?
O27 C26 C28 122.61(13) . . ?
N25 C26 C28 116.72(13) . . ?
C31A C28 C29A 110.1(8) . . ?
C31A C28 C26 114.9(4) . . ?
C29A C28 C26 108.6(6) . . ?
C31A C28 C30A 107.7(5) . . ?
C29A C28 C30A 107.4(8) . . ?
C26 C28 C30A 107.9(4) . . ?
C30B C28 C29B 111.0(8) . . ?
C30B C28 C31B 111.4(6) . . ?
C29B C28 C31B 110.0(8) . . ?
C30B C28 C26 107.9(4) . . ?
C29B C28 C26 106.7(6) . . ?
C31B C28 C26 109.7(4) . . ?
C28 C29A H29A 109.5 . . ?
C28 C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C28 C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C28 C30A H30A 109.5 . . ?
C28 C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C28 C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C28 C31A H31A 109.5 . . ?
C28 C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C28 C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C28 C29B H29D 109.5 . . ?
C28 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C28 C30B H30D 109.5 . . ?
C28 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C28 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C28 C31B H31D 109.5 . . ?
C28 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C28 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C33 N32 C37 119.85(11) . . ?
C33 N32 Fe1 118.84(9) . . ?
C37 N32 Fe1 121.19(8) . . ?
N32 C33 C34 121.61(12) . . ?
N32 C33 C38 113.12(11) . . ?
C34 C33 C38 125.24(12) . . ?
C35 C34 C33 118.31(13) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C35 C36 120.06(13) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 118.29(13) . . ?
C37 C36 H36 120.9 . . ?
C35 C36 H36 120.9 . . ?
N32 C37 C36 121.86(12) . . ?
N32 C37 C50 112.72(11) . . ?
C36 C37 C50 125.41(12) . . ?
N39 C38 C42 111.42(12) . . ?
N39 C38 C33 117.43(11) . . ?
C42 C38 C33 131.15(12) . . ?
C38 N39 N40 105.32(10) . . ?
C38 N39 Fe1 116.09(8) . . ?
N40 N39 Fe1 138.58(9) . . ?
C41 N40 N39 111.05(11) . . ?
C41 N40 H40 124.5 . . ?
N39 N40 H40 124.5 . . ?
N40 C41 C42 107.92(11) . . ?
N40 C41 N43 124.41(13) . . ?
C42 C41 N43 127.57(13) . . ?
C41 C42 C38 104.28(12) . . ?
C41 C42 H42 127.9 . . ?
C38 C42 H42 127.9 . . ?
C44 N43 C41 124.78(13) . . ?
C44 N43 H43 117.6 . . ?
C41 N43 H43 117.6 . . ?
O45 C44 N43 120.28(14) . . ?
O45 C44 C46C 120.1(6) . . ?
N43 C44 C46C 119.6(6) . . ?
O45 C44 C46B 121.8(6) . . ?
N43 C44 C46B 117.8(6) . . ?
O45 C44 C46A 125.0(3) . . ?
N43 C44 C46A 114.6(3) . . ?
C47A C46A C49A 112.3(7) . . ?
C47A C46A C48A 109.1(7) . . ?
C49A C46A C48A 106.9(6) . . ?
C47A C46A C44 106.8(6) . . ?
C49A C46A C44 108.1(5) . . ?
C48A C46A C44 113.8(5) . . ?
C46A C47A H47A 109.5 . . ?
C46A C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
C46A C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C46A C48A H48A 109.5 . . ?
C46A C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C46A C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C46A C49A H49A 109.5 . . ?
C46A C49A H49B 109.5 . . ?
H49A C49A H49B 109.5 . . ?
C46A C49A H49C 109.5 . . ?
H49A C49A H49C 109.5 . . ?
H49B C49A H49C 109.5 . . ?
C44 C46B C47B 112.9(11) . . ?
C44 C46B C48B 105.0(10) . . ?
C47B C46B C48B 111.1(11) . . ?
C44 C46B C49B 110.7(10) . . ?
C47B C46B C49B 106.2(10) . . ?
C48B C46B C49B 110.9(11) . . ?
C46B C47B H47D 109.5 . . ?
C46B C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C46B C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C46B C48B H48D 109.5 . . ?
C46B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C46B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C46B C49B H49D 109.5 . . ?
C46B C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C46B C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
C49C C46C C47C 112.2(11) . . ?
C49C C46C C44 105.4(10) . . ?
C47C C46C C44 109.2(11) . . ?
C49C C46C C48C 108.7(11) . . ?
C47C C46C C48C 109.1(10) . . ?
C44 C46C C48C 112.2(11) . . ?
C46C C47C H47G 109.5 . . ?
C46C C47C H47H 109.5 . . ?
H47G C47C H47H 109.5 . . ?
C46C C47C H47I 109.5 . . ?
H47G C47C H47I 109.5 . . ?
H47H C47C H47I 109.5 . . ?
C46C C48C H48G 109.5 . . ?
C46C C48C H48H 109.5 . . ?
H48G C48C H48H 109.5 . . ?
C46C C48C H48I 109.5 . . ?
H48G C48C H48I 109.5 . . ?
H48H C48C H48I 109.5 . . ?
C46C C49C H49G 109.5 . . ?
C46C C49C H49H 109.5 . . ?
H49G C49C H49H 109.5 . . ?
C46C C49C H49I 109.5 . . ?
H49G C49C H49I 109.5 . . ?
H49H C49C H49I 109.5 . . ?
N51 C50 C54 111.76(11) . . ?
N51 C50 C37 115.92(11) . . ?
C54 C50 C37 132.32(12) . . ?
C50 N51 N52 105.15(10) . . ?
C50 N51 Fe1 117.49(8) . . ?
N52 N51 Fe1 137.18(9) . . ?
C53 N52 N51 111.18(11) . . ?
C53 N52 H52 124.4 . . ?
N51 N52 H52 124.4 . . ?
N52 C53 C54 108.15(11) . . ?
N52 C53 N55 121.99(12) . . ?
C54 C53 N55 129.78(12) . . ?
C53 C54 C50 103.76(12) . . ?
C53 C54 H54 128.1 . . ?
C50 C54 H54 128.1 . . ?
C56 N55 C53 123.23(12) . . ?
C56 N55 H55 118.4 . . ?
C53 N55 H55 118.4 . . ?
O57 C56 N55 121.00(12) . . ?
O57 C56 C58 121.67(13) . . ?
N55 C56 C58 117.27(12) . . ?
C61 C58 C56 113.92(12) . . ?
C61 C58 C60 110.70(15) . . ?
C56 C58 C60 105.97(12) . . ?
C61 C58 C59 109.29(14) . . ?
C56 C58 C59 107.72(13) . . ?
C60 C58 C59 109.08(16) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
F63 B62 F66 109.12(16) . . ?
F63 B62 F65 108.76(15) . . ?
F66 B62 F65 111.46(15) . . ?
F63 B62 F64 108.39(17) . . ?
F66 B62 F64 108.88(15) . . ?
F65 B62 F64 110.17(14) . . ?
F68 B67 F69 110.53(14) . . ?
F68 B67 F71 110.92(16) . . ?
F69 B67 F71 110.09(14) . . ?
F68 B67 F70 109.25(14) . . ?
F69 B67 F70 107.96(16) . . ?
F71 B67 F70 108.01(13) . . ?
C73 C72 H72A 109.5 . . ?
C73 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C73 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N74 C73 C72 179.2(2) . . ?
C76 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C76 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N77 C76 C75 179.3(4) . . ?
C79 C78 H78A 109.5 . . ?
C79 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C79 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N80 C79 C78 179.4(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 F70 0.88 1.96 2.8094(16) 160.5 .
N13 H13 F71 0.88 2.10 2.9025(16) 151.2 .
N22 H22 O27 0.88 2.15 2.6851(15) 118.5 .
N22 H22 N80 0.88 2.13 2.925(2) 150.7 .
N25 H25 F63 0.88 2.08 2.9046(17) 155.4 .
N40 H40 O45 0.88 2.17 2.6905(16) 117.5 .
N40 H40 N74 0.88 2.24 2.995(2) 143.5 .
N43 H43 F69 0.88 2.11 2.9281(18) 154.5 2
N52 H52 O57 0.88 2.05 2.6014(15) 119.8 .
N55 H55 F65 0.88 2.12 2.9192(16) 150.8 1_455

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        32.68
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 982127'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tdr59

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis-[2,6-bis{5-tertbutylcarboxamido-1H-pyrazol-3-yl}pyridine]iron(II)
diperchlorate tris-acetonitrile solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H54 Fe N14 O4, 2[Cl O4], 3[C2 H3 N]'
_chemical_formula_sum            'C48 H63 Cl2 Fe N17 O12'
_chemical_formula_weight         1196.90

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   12.995(2)
_cell_length_b                   13.3971(19)
_cell_length_c                   19.304(3)
_cell_angle_alpha                104.696(7)
_cell_angle_beta                 100.401(9)
_cell_angle_gamma                108.320(8)
_cell_volume                     2959.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    67966
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      30.36

_exptl_crystal_description       'rectangular prism'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1252
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            67966
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_sigmaI/netI    0.4396
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         30.36
_reflns_number_total             17432
_reflns_number_gt                9219
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

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

 The slightly high value of Rint (0.11) may reflect mild twinning of the 
 crystal, according to CheckCif. If so, this has only a minimal effect on 
 the quality of the refinement.  

 Two of the four tert-butyl groups in the molecule are disordered:
    C28-C31 was refined over two half-occupied sites sharing a common 
 wholly occupied bridgehead C atom C28;
    and, C46-C49 was modelled over three orientations with occupancies 
 of 0.50, 0.25 and 0.25.
 The refined restraints C---C = 1.53(2) and 1,3-C...C = 2.50(2) Å were 
 applied to these groups.

 All non-H atoms with occupancy >=0.5 were refined anisotropically, while 
 H atoms were placed in calculated positions and refined using a riding 
 model. The highest residual Fourier peak of +1.0 e.Å⁻³ lies 
 0.8 Å from Fe1.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0936P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17432
_refine_ls_number_parameters     790
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.2463
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1771
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.24167(3) 0.01285(2) 0.256863(19) 0.01796(10) Uani 1 1 d . . .
N2 N 0.37914(17) 0.10212(11) 0.35618(11) 0.0195(5) Uani 1 1 d . . .
C3 C 0.3902(2) 0.20454(14) 0.39951(14) 0.0215(6) Uani 1 1 d . . .
C4 C 0.4708(2) 0.25968(15) 0.46863(15) 0.0290(6) Uani 1 1 d . . .
H4 H 0.4779 0.3312 0.4985 0.035 Uiso 1 1 calc R . .
C5 C 0.5411(2) 0.20802(16) 0.49341(15) 0.0288(6) Uani 1 1 d . . .
H5 H 0.5957 0.2437 0.5409 0.035 Uiso 1 1 calc R . .
C6 C 0.5311(2) 0.10308(15) 0.44805(15) 0.0277(6) Uani 1 1 d . . .
H6 H 0.5796 0.0678 0.4636 0.033 Uiso 1 1 calc R . .
C7 C 0.4485(2) 0.05267(14) 0.38002(14) 0.0203(5) Uani 1 1 d . . .
C8 C 0.3096(2) 0.24664(14) 0.36432(13) 0.0199(5) Uani 1 1 d . . .
N9 N 0.23647(17) 0.17929(12) 0.29755(11) 0.0198(5) Uani 1 1 d . . .
N10 N 0.17311(17) 0.23601(12) 0.27717(12) 0.0215(5) Uani 1 1 d . . .
H10 H 0.1185 0.2108 0.2353 0.026 Uiso 1 1 calc R . .
C11 C 0.2060(2) 0.33813(14) 0.33075(14) 0.0230(6) Uani 1 1 d . . .
C12 C 0.2929(2) 0.34821(14) 0.38785(15) 0.0262(6) Uani 1 1 d . . .
H12 H 0.3327 0.4093 0.4328 0.031 Uiso 1 1 calc R . .
N13 N 0.14732(19) 0.40652(13) 0.31814(13) 0.0311(6) Uani 1 1 d . . .
H13 H 0.0814 0.3759 0.2840 0.037 Uiso 1 1 calc R . .
C14 C 0.1872(2) 0.51876(16) 0.35628(17) 0.0341(7) Uani 1 1 d . . .
O15 O 0.2767(2) 0.56456(14) 0.40347(18) 0.0875(11) Uani 1 1 d . . .
C16 C 0.1087(2) 0.57815(15) 0.33366(16) 0.0306(7) Uani 1 1 d . . .
C17 C 0.0096(3) 0.5474(2) 0.3678(2) 0.0472(9) Uani 1 1 d . . .
H17A H -0.0382 0.5889 0.3578 0.071 Uiso 1 1 calc R . .
H17B H 0.0392 0.5664 0.4219 0.071 Uiso 1 1 calc R . .
H17C H -0.0354 0.4672 0.3454 0.071 Uiso 1 1 calc R . .
C18 C 0.0650(3) 0.54537(19) 0.24870(18) 0.0407(8) Uani 1 1 d . . .
H18A H 0.1291 0.5596 0.2276 0.061 Uiso 1 1 calc R . .
H18B H 0.0213 0.5896 0.2366 0.061 Uiso 1 1 calc R . .
H18C H 0.0165 0.4660 0.2276 0.061 Uiso 1 1 calc R . .
C19 C 0.1780(2) 0.70521(16) 0.36687(18) 0.0386(8) Uani 1 1 d . . .
H19A H 0.2447 0.7233 0.3484 0.058 Uiso 1 1 calc R . .
H19B H 0.2021 0.7277 0.4215 0.058 Uiso 1 1 calc R . .
H19C H 0.1312 0.7451 0.3518 0.058 Uiso 1 1 calc R . .
C20 C 0.4230(2) -0.05949(14) 0.32655(14) 0.0201(5) Uani 1 1 d . . .
N21 N 0.33430(17) -0.10007(12) 0.26573(11) 0.0207(5) Uani 1 1 d . . .
N22 N 0.32851(17) -0.20428(12) 0.22920(11) 0.0215(5) Uani 1 1 d . . .
H22 H 0.2775 -0.2502 0.1870 0.026 Uiso 1 1 calc R . .
C23 C 0.4120(2) -0.22742(14) 0.26674(14) 0.0231(6) Uani 1 1 d . . .
C24 C 0.4765(2) -0.13538(14) 0.33094(14) 0.0216(6) Uani 1 1 d . . .
H24 H 0.5405 -0.1263 0.3683 0.026 Uiso 1 1 calc R . .
N25 N 0.42806(18) -0.32817(13) 0.24433(12) 0.0264(5) Uani 1 1 d . . .
H25 H 0.4885 -0.3328 0.2702 0.032 Uiso 1 1 calc R . .
C26 C 0.3551(2) -0.42102(15) 0.18411(15) 0.0263(6) Uani 1 1 d D A .
O27 O 0.27138(17) -0.41844(12) 0.14560(12) 0.0383(5) Uani 1 1 d . . .
C28 C 0.3882(2) -0.52404(16) 0.16894(16) 0.0311(7) Uani 1 1 d D . .
C29A C 0.4512(17) -0.5211(15) 0.1102(11) 0.099(8) Uani 0.50 1 d PD A 1
H29A H 0.4046 -0.5165 0.0660 0.149 Uiso 0.50 1 calc PR A 1
H29B H 0.4673 -0.5890 0.0963 0.149 Uiso 0.50 1 calc PR A 1
H29C H 0.5223 -0.4558 0.1303 0.149 Uiso 0.50 1 calc PR A 1
C30A C 0.2739(11) -0.6269(7) 0.1327(9) 0.061(4) Uani 0.50 1 d PD A 1
H30A H 0.2275 -0.6156 0.0917 0.091 Uiso 0.50 1 calc PR A 1
H30B H 0.2335 -0.6355 0.1704 0.091 Uiso 0.50 1 calc PR A 1
H30C H 0.2891 -0.6943 0.1133 0.091 Uiso 0.50 1 calc PR A 1
C31A C 0.4524(15) -0.5346(13) 0.2367(8) 0.093(7) Uani 0.50 1 d PD A 1
H31A H 0.5224 -0.4684 0.2607 0.139 Uiso 0.50 1 calc PR A 1
H31B H 0.4707 -0.6012 0.2227 0.139 Uiso 0.50 1 calc PR A 1
H31C H 0.4065 -0.5410 0.2716 0.139 Uiso 0.50 1 calc PR A 1
C29B C 0.4860(15) -0.4982(14) 0.1340(12) 0.088(6) Uani 0.50 1 d PD A 2
H29D H 0.5097 -0.5617 0.1233 0.131 Uiso 0.50 1 calc PR A 2
H29E H 0.5497 -0.4318 0.1688 0.131 Uiso 0.50 1 calc PR A 2
H29F H 0.4613 -0.4845 0.0875 0.131 Uiso 0.50 1 calc PR A 2
C30B C 0.2893(12) -0.6230(9) 0.1134(9) 0.094(7) Uani 0.50 1 d PD A 2
H30D H 0.2246 -0.6374 0.1340 0.140 Uiso 0.50 1 calc PR A 2
H30E H 0.3098 -0.6886 0.1031 0.140 Uiso 0.50 1 calc PR A 2
H30F H 0.2692 -0.6075 0.0670 0.140 Uiso 0.50 1 calc PR A 2
C31B C 0.4270(14) -0.5475(12) 0.2396(7) 0.047(3) Uani 0.50 1 d PD A 2
H31D H 0.3644 -0.5660 0.2618 0.070 Uiso 0.50 1 calc PR A 2
H31E H 0.4902 -0.4813 0.2750 0.070 Uiso 0.50 1 calc PR A 2
H31F H 0.4515 -0.6103 0.2277 0.070 Uiso 0.50 1 calc PR A 2
N32 N 0.06952(17) -0.07917(12) 0.18696(11) 0.0199(5) Uani 1 1 d . . .
C33 C 0.0456(2) -0.08940(14) 0.11426(14) 0.0202(5) Uani 1 1 d . . .
C34 C -0.0622(2) -0.15506(16) 0.06457(15) 0.0255(6) Uani 1 1 d . . .
H34 H -0.0779 -0.1612 0.0133 0.031 Uiso 1 1 calc R . .
C35 C -0.1458(2) -0.21112(18) 0.09298(16) 0.0310(7) Uani 1 1 d . . .
H35 H -0.2193 -0.2575 0.0607 0.037 Uiso 1 1 calc R . .
C36 C -0.1213(2) -0.19906(16) 0.16863(15) 0.0279(6) Uani 1 1 d . . .
H36 H -0.1780 -0.2357 0.1885 0.033 Uiso 1 1 calc R . .
C37 C -0.0125(2) -0.13254(14) 0.21465(14) 0.0208(5) Uani 1 1 d . . .
C38 C 0.1442(2) -0.02755(14) 0.09296(14) 0.0210(6) Uani 1 1 d . . .
N39 N 0.24346(17) 0.02580(12) 0.14707(11) 0.0212(5) Uani 1 1 d . . .
N40 N 0.31882(19) 0.07398(13) 0.11279(12) 0.0228(5) Uani 1 1 d . . .
H40 H 0.3909 0.1147 0.1352 0.027 Uiso 1 1 calc R . .
C41 C 0.2680(2) 0.05072(15) 0.03966(14) 0.0239(6) Uani 1 1 d . . .
C42 C 0.1547(2) -0.01391(16) 0.02493(14) 0.0234(6) Uani 1 1 d . . .
H42 H 0.0972 -0.0425 -0.0211 0.028 Uiso 1 1 calc R . .
N43 N 0.32584(19) 0.08217(15) -0.01076(13) 0.0285(5) Uani 1 1 d . B .
H43 H 0.2880 0.0539 -0.0584 0.034 Uiso 1 1 calc R . .
C44 C 0.4366(2) 0.15349(18) 0.00793(15) 0.0287(6) Uani 1 1 d D . .
O45 O 0.48977(18) 0.20377(15) 0.07395(12) 0.0430(6) Uani 1 1 d . B .
C46A C 0.4808(9) 0.1570(9) -0.0621(6) 0.033(4) Uani 0.50 1 d PD B 1
C47A C 0.4173(9) 0.2060(8) -0.1092(5) 0.063(3) Uani 0.50 1 d PD B 1
H47A H 0.4263 0.2805 -0.0786 0.095 Uiso 0.50 1 calc PR B 1
H47B H 0.3369 0.1578 -0.1277 0.095 Uiso 0.50 1 calc PR B 1
H47C H 0.4478 0.2114 -0.1515 0.095 Uiso 0.50 1 calc PR B 1
C48A C 0.4661(8) 0.0411(5) -0.1104(5) 0.057(2) Uani 0.50 1 d PD B 1
H48A H 0.5051 0.0079 -0.0802 0.086 Uiso 0.50 1 calc PR B 1
H48B H 0.4982 0.0471 -0.1520 0.086 Uiso 0.50 1 calc PR B 1
H48C H 0.3854 -0.0062 -0.1300 0.086 Uiso 0.50 1 calc PR B 1
C49A C 0.6060(8) 0.2371(12) -0.0317(6) 0.168(10) Uani 0.50 1 d PD B 1
H49A H 0.6115 0.3105 -0.0015 0.252 Uiso 0.50 1 calc PR B 1
H49B H 0.6372 0.2443 -0.0735 0.252 Uiso 0.50 1 calc PR B 1
H49C H 0.6486 0.2075 -0.0008 0.252 Uiso 0.50 1 calc PR B 1
C46B C 0.4926(15) 0.1736(13) -0.0525(9) 0.019(6) Uiso 0.25 1 d PD B 2
C47B C 0.4156(14) 0.1796(12) -0.1180(8) 0.036(4) Uiso 0.25 1 d PD B 2
H47D H 0.4568 0.1943 -0.1544 0.054 Uiso 0.25 1 calc PR B 2
H47E H 0.3890 0.2398 -0.1009 0.054 Uiso 0.25 1 calc PR B 2
H47F H 0.3507 0.1086 -0.1413 0.054 Uiso 0.25 1 calc PR B 2
C48B C 0.5250(11) 0.0721(8) -0.0790(8) 0.033(3) Uiso 0.25 1 d PD B 2
H48D H 0.5582 0.0774 -0.1203 0.049 Uiso 0.25 1 calc PR B 2
H48E H 0.4573 0.0035 -0.0960 0.049 Uiso 0.25 1 calc PR B 2
H48F H 0.5801 0.0708 -0.0376 0.049 Uiso 0.25 1 calc PR B 2
C49B C 0.6038(12) 0.2746(9) -0.0202(10) 0.041(3) Uiso 0.25 1 d PD B 2
H49D H 0.6354 0.2889 -0.0607 0.062 Uiso 0.25 1 calc PR B 2
H49E H 0.6573 0.2600 0.0148 0.062 Uiso 0.25 1 calc PR B 2
H49F H 0.5902 0.3400 0.0062 0.062 Uiso 0.25 1 calc PR B 2
C46C C 0.4917(16) 0.1688(15) -0.0541(10) 0.051(16) Uiso 0.25 1 d PD B 3
C47C C 0.5056(14) 0.2844(9) -0.0575(8) 0.058(3) Uiso 0.25 1 d PD B 3
H47G H 0.5496 0.3404 -0.0084 0.087 Uiso 0.25 1 calc PR B 3
H47H H 0.4310 0.2883 -0.0715 0.087 Uiso 0.25 1 calc PR B 3
H47I H 0.5452 0.2990 -0.0947 0.087 Uiso 0.25 1 calc PR B 3
C48C C 0.4229(14) 0.0794(11) -0.1291(7) 0.072(4) Uiso 0.25 1 d PD B 3
H48G H 0.4184 0.0063 -0.1262 0.108 Uiso 0.25 1 calc PR B 3
H48H H 0.4594 0.0946 -0.1675 0.108 Uiso 0.25 1 calc PR B 3
H48I H 0.3466 0.0797 -0.1420 0.108 Uiso 0.25 1 calc PR B 3
C49C C 0.6079(11) 0.1614(10) -0.0305(9) 0.057(4) Uiso 0.25 1 d PD B 3
H49G H 0.6537 0.2216 0.0165 0.086 Uiso 0.25 1 calc PR B 3
H49H H 0.6461 0.1686 -0.0693 0.086 Uiso 0.25 1 calc PR B 3
H49I H 0.5978 0.0893 -0.0236 0.086 Uiso 0.25 1 calc PR B 3
C50 C 0.0276(2) -0.11211(14) 0.29476(14) 0.0209(5) Uani 1 1 d . . .
N51 N 0.13704(17) -0.04428(12) 0.32921(11) 0.0211(5) Uani 1 1 d . . .
N52 N 0.15328(18) -0.03759(12) 0.40186(11) 0.0204(5) Uani 1 1 d . . .
H52 H 0.2176 0.0023 0.4369 0.024 Uiso 1 1 calc R . .
C53 C 0.0573(2) -0.10054(15) 0.41372(14) 0.0231(6) Uani 1 1 d . . .
C54 C -0.0253(2) -0.14944(16) 0.34623(15) 0.0248(6) Uani 1 1 d . . .
H54 H -0.1015 -0.1978 0.3365 0.030 Uiso 1 1 calc R . .
N55 N 0.05486(19) -0.11171(14) 0.48342(12) 0.0249(5) Uani 1 1 d . . .
H55 H -0.0114 -0.1403 0.4908 0.030 Uiso 1 1 calc R . .
C56 C 0.1502(2) -0.08057(17) 0.54121(15) 0.0253(6) Uani 1 1 d . . .
O57 O 0.24499(17) -0.03020(13) 0.53628(11) 0.0310(5) Uani 1 1 d . . .
C58 C 0.1355(3) -0.11545(19) 0.60977(16) 0.0323(7) Uani 1 1 d . . .
C59 C 0.2126(3) -0.0152(3) 0.68021(18) 0.0479(8) Uani 1 1 d . . .
H59A H 0.2914 0.0049 0.6789 0.072 Uiso 1 1 calc R . .
H59B H 0.2050 -0.0354 0.7249 0.072 Uiso 1 1 calc R . .
H59C H 0.1903 0.0485 0.6814 0.072 Uiso 1 1 calc R . .
C60 C 0.1780(4) -0.2116(3) 0.6048(2) 0.0583(11) Uani 1 1 d . . .
H60A H 0.1276 -0.2766 0.5616 0.087 Uiso 1 1 calc R . .
H60B H 0.1787 -0.2312 0.6504 0.087 Uiso 1 1 calc R . .
H60C H 0.2547 -0.1881 0.5994 0.087 Uiso 1 1 calc R . .
C61 C 0.0139(3) -0.1507(2) 0.61551(18) 0.0374(7) Uani 1 1 d . . .
H61A H -0.0127 -0.0898 0.6157 0.056 Uiso 1 1 calc R . .
H61B H 0.0118 -0.1676 0.6618 0.056 Uiso 1 1 calc R . .
H61C H -0.0351 -0.2170 0.5727 0.056 Uiso 1 1 calc R . .
Cl62 Cl 0.71513(6) -0.30635(4) 0.39827(4) 0.03289(18) Uani 1 1 d . . .
O63 O 0.6450(3) -0.26821(18) 0.3561(2) 0.1244(17) Uani 1 1 d . . .
O64 O 0.7639(3) -0.36241(17) 0.34845(19) 0.0881(12) Uani 1 1 d . . .
O65 O 0.8007(2) -0.21243(17) 0.45663(15) 0.0600(7) Uani 1 1 d . . .
O66 O 0.6488(3) -0.38541(17) 0.42572(16) 0.0737(9) Uani 1 1 d . . .
Cl67 Cl -0.10866(6) 0.18555(4) 0.16167(4) 0.03158(17) Uani 1 1 d . . .
O68 O -0.1809(2) 0.20670(16) 0.10695(13) 0.0475(6) Uani 1 1 d . . .
O69 O -0.1541(2) 0.07039(13) 0.15729(12) 0.0525(7) Uani 1 1 d . . .
O70 O 0.00217(19) 0.20908(17) 0.14820(13) 0.0485(6) Uani 1 1 d . . .
O71 O -0.09373(19) 0.25646(13) 0.23658(11) 0.0444(6) Uani 1 1 d . . .
C72 C 0.6592(3) 0.3703(2) 0.3619(2) 0.0640(11) Uani 1 1 d . . .
H72A H 0.6244 0.4255 0.3724 0.096 Uiso 1 1 calc R . .
H72B H 0.7310 0.4038 0.3516 0.096 Uiso 1 1 calc R . .
H72C H 0.6732 0.3459 0.4052 0.096 Uiso 1 1 calc R . .
C73 C 0.5825(3) 0.2734(2) 0.2961(2) 0.0425(8) Uani 1 1 d . . .
N74 N 0.5216(3) 0.1993(2) 0.24677(18) 0.0545(8) Uani 1 1 d . . .
C75 C 0.7323(3) 0.4183(3) 0.1842(3) 0.0674(12) Uani 1 1 d . . .
H75A H 0.7906 0.3907 0.2004 0.101 Uiso 1 1 calc R . .
H75B H 0.6602 0.3552 0.1583 0.101 Uiso 1 1 calc R . .
H75C H 0.7242 0.4684 0.2278 0.101 Uiso 1 1 calc R . .
C76 C 0.7647(4) 0.4785(3) 0.1337(3) 0.0798(14) Uani 1 1 d . . .
N77 N 0.7926(5) 0.5254(3) 0.0940(3) 0.133(2) Uani 1 1 d . . .
C78 C 0.0033(3) -0.3919(2) -0.03853(19) 0.0551(10) Uani 1 1 d . . .
H78A H -0.0728 -0.4340 -0.0373 0.083 Uiso 1 1 calc R . .
H78B H 0.0331 -0.4432 -0.0659 0.083 Uiso 1 1 calc R . .
H78C H -0.0002 -0.3374 -0.0635 0.083 Uiso 1 1 calc R . .
C79 C 0.0770(3) -0.33407(18) 0.03737(18) 0.0357(7) Uani 1 1 d . . .
N80 N 0.1335(2) -0.28893(18) 0.09670(17) 0.0521(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.134(2) . ?
Fe1 N32 2.163(2) . ?
Fe1 N39 2.174(2) . ?
Fe1 N9 2.1952(15) . ?
Fe1 N51 2.2268(19) . ?
Fe1 N21 2.2291(18) . ?
N2 C7 1.358(3) . ?
N2 C3 1.361(2) . ?
C3 C4 1.390(4) . ?
C3 C8 1.478(3) . ?
C4 C5 1.396(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(4) . ?
C6 H6 0.9500 . ?
C7 C20 1.487(2) . ?
C8 N9 1.344(3) . ?
C8 C12 1.419(2) . ?
N9 N10 1.356(3) . ?
N10 C11 1.371(2) . ?
N10 H10 0.8800 . ?
C11 C12 1.374(4) . ?
C11 N13 1.402(3) . ?
C12 H12 0.9500 . ?
N13 C14 1.372(2) . ?
N13 H13 0.8800 . ?
C14 O15 1.201(4) . ?
C14 C16 1.547(4) . ?
C16 C18 1.532(4) . ?
C16 C17 1.541(4) . ?
C16 C19 1.547(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N21 1.341(3) . ?
C20 C24 1.410(3) . ?
N21 N22 1.3665(19) . ?
N22 C23 1.357(3) . ?
N22 H22 0.8800 . ?
C23 C24 1.399(3) . ?
C23 N25 1.402(2) . ?
C24 H24 0.9500 . ?
N25 C26 1.387(3) . ?
N25 H25 0.8800 . ?
C26 O27 1.217(3) . ?
C26 C28 1.546(3) . ?
C28 C31A 1.484(11) . ?
C28 C29A 1.515(11) . ?
C28 C30A 1.563(10) . ?
C28 C30B 1.506(10) . ?
C28 C31B 1.511(10) . ?
C28 C29B 1.531(11) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
N32 C33 1.343(3) . ?
N32 C37 1.361(3) . ?
C33 C34 1.403(4) . ?
C33 C38 1.481(3) . ?
C34 C35 1.398(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.393(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(4) . ?
C36 H36 0.9500 . ?
C37 C50 1.464(4) . ?
C38 N39 1.349(3) . ?
C38 C42 1.396(3) . ?
N39 N40 1.366(3) . ?
N40 C41 1.355(3) . ?
N40 H40 0.8800 . ?
C41 C42 1.386(3) . ?
C41 N43 1.401(3) . ?
C42 H42 0.9500 . ?
N43 C44 1.374(3) . ?
N43 H43 0.8800 . ?
C44 O45 1.229(3) . ?
C44 C46B 1.519(16) . ?
C44 C46C 1.526(17) . ?
C44 C46A 1.567(9) . ?
C46A C47A 1.521(11) . ?
C46A C48A 1.527(11) . ?
C46A C49A 1.542(11) . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C49A H49A 0.9800 . ?
C49A H49B 0.9800 . ?
C49A H49C 0.9800 . ?
C46B C47B 1.500(16) . ?
C46B C49B 1.525(16) . ?
C46B C48B 1.540(14) . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
C46C C48C 1.520(17) . ?
C46C C47C 1.522(17) . ?
C46C C49C 1.538(17) . ?
C47C H47G 0.9800 . ?
C47C H47H 0.9800 . ?
C47C H47I 0.9800 . ?
C48C H48G 0.9800 . ?
C48C H48H 0.9800 . ?
C48C H48I 0.9800 . ?
C49C H49G 0.9800 . ?
C49C H49H 0.9800 . ?
C49C H49I 0.9800 . ?
C50 N51 1.353(3) . ?
C50 C54 1.412(3) . ?
N51 N52 1.355(3) . ?
N52 C53 1.364(3) . ?
N52 H52 0.8800 . ?
C53 C54 1.378(4) . ?
C53 N55 1.396(3) . ?
C54 H54 0.9500 . ?
N55 C56 1.376(4) . ?
N55 H55 0.8800 . ?
C56 O57 1.239(3) . ?
C56 C58 1.535(4) . ?
C58 C61 1.535(4) . ?
C58 C60 1.541(3) . ?
C58 C59 1.547(4) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
Cl62 O63 1.411(3) . ?
Cl62 O66 1.421(2) . ?
Cl62 O65 1.427(2) . ?
Cl62 O64 1.429(2) . ?
Cl67 O68 1.428(2) . ?
Cl67 O69 1.4419(17) . ?
Cl67 O71 1.4550(19) . ?
Cl67 O70 1.460(2) . ?
C72 C73 1.478(5) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 N74 1.128(4) . ?
C75 C76 1.454(7) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 N77 1.146(7) . ?
C78 C79 1.454(5) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 N80 1.133(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 N32 158.91(7) . . ?
N2 Fe1 N39 125.39(7) . . ?
N32 Fe1 N39 74.31(8) . . ?
N2 Fe1 N9 74.24(7) . . ?
N32 Fe1 N9 99.78(7) . . ?
N39 Fe1 N9 91.88(7) . . ?
N2 Fe1 N51 87.07(8) . . ?
N32 Fe1 N51 72.57(8) . . ?
N39 Fe1 N51 146.67(8) . . ?
N9 Fe1 N51 90.10(6) . . ?
N2 Fe1 N21 74.41(7) . . ?
N32 Fe1 N21 111.39(6) . . ?
N39 Fe1 N21 102.07(7) . . ?
N9 Fe1 N21 148.23(8) . . ?
N51 Fe1 N21 93.34(7) . . ?
C7 N2 C3 119.9(2) . . ?
C7 N2 Fe1 120.16(12) . . ?
C3 N2 Fe1 119.62(17) . . ?
N2 C3 C4 121.2(2) . . ?
N2 C3 C8 112.6(2) . . ?
C4 C3 C8 126.15(17) . . ?
C3 C4 C5 118.75(18) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 118.1(2) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
N2 C7 C6 121.96(17) . . ?
N2 C7 C20 112.6(2) . . ?
C6 C7 C20 125.4(2) . . ?
N9 C8 C12 111.1(2) . . ?
N9 C8 C3 117.00(15) . . ?
C12 C8 C3 131.9(2) . . ?
C8 N9 N10 105.82(15) . . ?
C8 N9 Fe1 115.82(15) . . ?
N10 N9 Fe1 138.16(15) . . ?
N9 N10 C11 110.6(2) . . ?
N9 N10 H10 124.7 . . ?
C11 N10 H10 124.7 . . ?
N10 C11 C12 108.23(18) . . ?
N10 C11 N13 117.5(2) . . ?
C12 C11 N13 134.29(18) . . ?
C11 C12 C8 104.26(19) . . ?
C11 C12 H12 127.9 . . ?
C8 C12 H12 127.9 . . ?
C14 N13 C11 123.5(2) . . ?
C14 N13 H13 118.3 . . ?
C11 N13 H13 118.3 . . ?
O15 C14 N13 120.8(2) . . ?
O15 C14 C16 124.28(18) . . ?
N13 C14 C16 114.9(2) . . ?
C18 C16 C17 110.6(3) . . ?
C18 C16 C14 111.88(19) . . ?
C17 C16 C14 107.8(2) . . ?
C18 C16 C19 109.0(2) . . ?
C17 C16 C19 109.86(19) . . ?
C14 C16 C19 107.6(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N21 C20 C24 112.50(17) . . ?
N21 C20 C7 117.95(19) . . ?
C24 C20 C7 129.5(2) . . ?
C20 N21 N22 105.16(18) . . ?
C20 N21 Fe1 114.64(11) . . ?
N22 N21 Fe1 140.16(17) . . ?
C23 N22 N21 110.80(19) . . ?
C23 N22 H22 124.6 . . ?
N21 N22 H22 124.6 . . ?
N22 C23 C24 108.55(17) . . ?
N22 C23 N25 124.7(2) . . ?
C24 C23 N25 126.7(2) . . ?
C23 C24 C20 103.0(2) . . ?
C23 C24 H24 128.5 . . ?
C20 C24 H24 128.5 . . ?
C26 N25 C23 124.4(2) . . ?
C26 N25 H25 117.8 . . ?
C23 N25 H25 117.8 . . ?
O27 C26 N25 120.52(18) . . ?
O27 C26 C28 123.3(2) . . ?
N25 C26 C28 116.2(2) . . ?
C31A C28 C29A 112.4(9) . . ?
C31A C28 C26 114.2(6) . . ?
C29A C28 C26 107.8(7) . . ?
C31A C28 C30A 109.5(7) . . ?
C29A C28 C30A 107.1(9) . . ?
C26 C28 C30A 105.4(6) . . ?
C30B C28 C31B 111.2(8) . . ?
C30B C28 C29B 108.8(9) . . ?
C31B C28 C29B 108.7(9) . . ?
C30B C28 C26 108.9(6) . . ?
C31B C28 C26 112.3(6) . . ?
C29B C28 C26 106.7(6) . . ?
C28 C29A H29A 109.5 . . ?
C28 C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C28 C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C28 C30A H30A 109.5 . . ?
C28 C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C28 C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C28 C31A H31A 109.5 . . ?
C28 C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C28 C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C28 C29B H29D 109.5 . . ?
C28 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C28 C30B H30D 109.5 . . ?
C28 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C28 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C28 C31B H31D 109.5 . . ?
C28 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C28 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C33 N32 C37 119.9(2) . . ?
C33 N32 Fe1 119.13(15) . . ?
C37 N32 Fe1 120.78(17) . . ?
N32 C33 C34 122.1(2) . . ?
N32 C33 C38 113.2(2) . . ?
C34 C33 C38 124.7(2) . . ?
C35 C34 C33 117.8(3) . . ?
C35 C34 H34 121.1 . . ?
C33 C34 H34 121.1 . . ?
C36 C35 C34 120.0(2) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 119.0(2) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
N32 C37 C36 121.1(2) . . ?
N32 C37 C50 112.9(2) . . ?
C36 C37 C50 126.0(2) . . ?
N39 C38 C42 111.8(2) . . ?
N39 C38 C33 116.8(2) . . ?
C42 C38 C33 131.4(2) . . ?
C38 N39 N40 104.8(2) . . ?
C38 N39 Fe1 116.49(15) . . ?
N40 N39 Fe1 138.75(17) . . ?
C41 N40 N39 111.1(2) . . ?
C41 N40 H40 124.5 . . ?
N39 N40 H40 124.5 . . ?
N40 C41 C42 107.9(2) . . ?
N40 C41 N43 123.8(2) . . ?
C42 C41 N43 128.1(2) . . ?
C41 C42 C38 104.4(2) . . ?
C41 C42 H42 127.8 . . ?
C38 C42 H42 127.8 . . ?
C44 N43 C41 125.5(2) . . ?
C44 N43 H43 117.2 . . ?
C41 N43 H43 117.2 . . ?
O45 C44 N43 119.8(2) . . ?
O45 C44 C46B 119.7(7) . . ?
N43 C44 C46B 120.5(7) . . ?
O45 C44 C46C 121.0(8) . . ?
N43 C44 C46C 119.2(8) . . ?
O45 C44 C46A 127.5(5) . . ?
N43 C44 C46A 112.6(5) . . ?
C47A C46A C48A 108.8(8) . . ?
C47A C46A C49A 107.9(9) . . ?
C48A C46A C49A 112.2(9) . . ?
C47A C46A C44 109.8(7) . . ?
C48A C46A C44 111.8(7) . . ?
C49A C46A C44 106.1(7) . . ?
C46A C47A H47A 109.5 . . ?
C46A C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
C46A C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C46A C48A H48A 109.5 . . ?
C46A C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C46A C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C46A C49A H49A 109.5 . . ?
C46A C49A H49B 109.5 . . ?
H49A C49A H49B 109.5 . . ?
C46A C49A H49C 109.5 . . ?
H49A C49A H49C 109.5 . . ?
H49B C49A H49C 109.5 . . ?
C47B C46B C44 113.2(12) . . ?
C47B C46B C49B 112.4(12) . . ?
C44 C46B C49B 111.2(12) . . ?
C47B C46B C48B 108.8(12) . . ?
C44 C46B C48B 104.9(10) . . ?
C49B C46B C48B 105.7(11) . . ?
C46B C47B H47D 109.5 . . ?
C46B C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C46B C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C46B C48B H48D 109.5 . . ?
C46B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C46B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C46B C49B H49D 109.5 . . ?
C46B C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C46B C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
C48C C46C C47C 111.1(13) . . ?
C48C C46C C44 112.3(13) . . ?
C47C C46C C44 107.2(12) . . ?
C48C C46C C49C 109.5(13) . . ?
C47C C46C C49C 110.4(13) . . ?
C44 C46C C49C 106.2(12) . . ?
C46C C47C H47G 109.5 . . ?
C46C C47C H47H 109.5 . . ?
H47G C47C H47H 109.5 . . ?
C46C C47C H47I 109.5 . . ?
H47G C47C H47I 109.5 . . ?
H47H C47C H47I 109.5 . . ?
C46C C48C H48G 109.5 . . ?
C46C C48C H48H 109.5 . . ?
H48G C48C H48H 109.5 . . ?
C46C C48C H48I 109.5 . . ?
H48G C48C H48I 109.5 . . ?
H48H C48C H48I 109.5 . . ?
C46C C49C H49G 109.5 . . ?
C46C C49C H49H 109.5 . . ?
H49G C49C H49H 109.5 . . ?
C46C C49C H49I 109.5 . . ?
H49G C49C H49I 109.5 . . ?
H49H C49C H49I 109.5 . . ?
N51 C50 C54 110.5(2) . . ?
N51 C50 C37 116.5(2) . . ?
C54 C50 C37 133.0(2) . . ?
C50 N51 N52 105.50(19) . . ?
C50 N51 Fe1 116.80(16) . . ?
N52 N51 Fe1 137.47(16) . . ?
N51 N52 C53 111.4(2) . . ?
N51 N52 H52 124.3 . . ?
C53 N52 H52 124.3 . . ?
N52 C53 C54 107.4(2) . . ?
N52 C53 N55 122.0(2) . . ?
C54 C53 N55 130.5(2) . . ?
C53 C54 C50 105.2(2) . . ?
C53 C54 H54 127.4 . . ?
C50 C54 H54 127.4 . . ?
C56 N55 C53 123.8(2) . . ?
C56 N55 H55 118.1 . . ?
C53 N55 H55 118.1 . . ?
O57 C56 N55 120.7(2) . . ?
O57 C56 C58 121.4(3) . . ?
N55 C56 C58 117.9(2) . . ?
C56 C58 C61 114.1(3) . . ?
C56 C58 C60 106.2(2) . . ?
C61 C58 C60 111.0(2) . . ?
C56 C58 C59 107.8(2) . . ?
C61 C58 C59 108.6(2) . . ?
C60 C58 C59 109.0(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
O63 Cl62 O66 109.8(2) . . ?
O63 Cl62 O65 108.63(15) . . ?
O66 Cl62 O65 112.62(17) . . ?
O63 Cl62 O64 107.0(2) . . ?
O66 Cl62 O64 107.76(14) . . ?
O65 Cl62 O64 110.87(16) . . ?
O68 Cl67 O69 110.77(14) . . ?
O68 Cl67 O71 111.00(13) . . ?
O69 Cl67 O71 109.15(12) . . ?
O68 Cl67 O70 109.33(14) . . ?
O69 Cl67 O70 108.24(14) . . ?
O71 Cl67 O70 108.28(13) . . ?
C73 C72 H72A 109.5 . . ?
C73 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C73 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N74 C73 C72 178.2(4) . . ?
C76 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C76 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N77 C76 C75 178.3(6) . . ?
C79 C78 H78A 109.5 . . ?
C79 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C79 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N80 C79 C78 179.3(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 O70 0.88 2.04 2.882(3) 160.3 .
N13 H13 O71 0.88 2.19 2.998(3) 152.5 .
N22 H22 O27 0.88 2.16 2.696(2) 118.5 .
N22 H22 N80 0.88 2.14 2.938(4) 151.1 .
N25 H25 O63 0.88 2.14 2.958(4) 154.1 .
N40 H40 O45 0.88 2.19 2.712(3) 118.0 .
N40 H40 N74 0.88 2.24 3.002(4) 144.0 .
N43 H43 O69 0.88 2.19 3.013(3) 154.9 2
N52 H52 O57 0.88 2.07 2.616(3) 119.6 .
N55 H55 O65 0.88 2.22 3.037(3) 153.8 1_455

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        30.36
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.119
_database_code_depnum_ccdc_archive 'CCDC 982128'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tdr128

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis[2,6-bis(5-tertbutyl-1H-pyrazol-3-yl)pyridine]iron(II) 
ditetrafluoroborate 2,2,2-trifluoroethanol di-isopropyl ether solvate 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C38 H50 Fe N10, 2[B F4], 0.73[C2 H3 F3 O], 0.35[C6 H14 O]'
_chemical_formula_sum            'C41.55 H57.08 B2 F10.18 Fe N10 O1.08'
_chemical_formula_weight         984.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   17.588(2)
_cell_length_b                   19.509(2)
_cell_length_c                   32.399(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11117(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    124468
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      25.34

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4100
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            124468
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.34
_reflns_number_total             20237
_reflns_number_gt                15975
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

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

 The asymmetric unit contains two formula units of the compound. That is, 
 two complex dications labelled 'A' and 'B'; four BF₄⁻ anions, three 
 partially occupied 2,2,2-trifluoroethanol sites whose occupancies sum to 
 1.45, and a disordered part-occupied di-isopropyl ether molecule with total 
 occupancy 0.7. The solvent occupies channels in the lattice, running parallel 
 to (111).

 Three tertbutyl groups in the model were modelled as disordered, over two 
 equally occupied orientations. These were refined using the refined restraints
 C---C = 1.54(2) and 1,3-C...C = 2.51(2) Å. The BF₄⁻ anion B65-F69 is 
 also disordered, and was modelled over two orientations sharing a common wholly 
 occupied B atom. The occupancy ratio of the two sites refined to 0.59:0.41, 
 and the refined restraints B---F = 1.39(2) and F...F = 2.27(2) Å were applied 
 to that residue. Slightly high displacement parameters on some other tert-butyl 
 groups and anions may also indicate a degree of disorder in those residues, 
 but this was not modelled.

 The three 2,2,2-trifluoroethanol molecules were refined with occupancies of 
 0.70, 0.50 and 0.25. The latter required the following fixed restraints to 
 refine stably: C---C = 1.52(2), C---O = 1.43(2), C---F = 1.33(2), 
 F...F = 2.17(2), 1,3-C...F = 2.33(2) and 1,3-C...O = 2.40(2) Å. Lastly, the 
 two partial di-isopropyl ether sites were refined with occupancies of 0.30 
 and 0.40, subject to the fixed restraints C---C = 1.52(2), C---O = 1.43(2), 
 1,3-CH₃...CH₃ = 2.48(2) and 1,3-CH...CH = 2.34(2) Å.

 All non-H atoms with occupancy >0.5 were refined anisotropically, and H 
 atoms were placed in calculated positions and refined using a riding model.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1392P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(15)
_refine_ls_number_reflns         20237
_refine_ls_number_parameters     1223
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1932
_refine_ls_wR_factor_gt          0.1768
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1A Fe 0.37292(3) 0.52054(3) 0.251161(19) 0.02778(15) Uani 1 1 d . . .
N2A N 0.4096(2) 0.59818(18) 0.20947(12) 0.0326(8) Uani 1 1 d . . .
C3A C 0.4727(3) 0.5888(2) 0.18630(15) 0.0359(10) Uani 1 1 d . . .
C4A C 0.4979(3) 0.6393(3) 0.15861(16) 0.0483(12) Uani 1 1 d . . .
H4A H 0.5423 0.6323 0.1425 0.058 Uiso 1 1 calc R . .
C5A C 0.4565(4) 0.6999(3) 0.15525(18) 0.0565(15) Uani 1 1 d . . .
H5A H 0.4725 0.7348 0.1367 0.068 Uiso 1 1 calc R . .
C6A C 0.3908(3) 0.7091(2) 0.17945(17) 0.0479(13) Uani 1 1 d . . .
H6A H 0.3620 0.7501 0.1776 0.057 Uiso 1 1 calc R . .
C7A C 0.3691(3) 0.6569(2) 0.20599(15) 0.0368(10) Uani 1 1 d . . .
C8A C 0.5095(2) 0.5226(2) 0.19458(13) 0.0324(9) Uani 1 1 d . . .
N9A N 0.4684(2) 0.47578(19) 0.21584(11) 0.0324(8) Uani 1 1 d . . .
N10A N 0.51624(19) 0.42167(18) 0.22177(12) 0.0330(8) Uani 1 1 d . A .
H10A H 0.5034 0.3840 0.2350 0.040 Uiso 1 1 calc R . .
C11A C 0.5862(3) 0.4324(2) 0.20491(17) 0.0439(12) Uani 1 1 d D . .
C12A C 0.5837(3) 0.4978(3) 0.18693(18) 0.0493(14) Uani 1 1 d . A .
H12A H 0.6235 0.5206 0.1726 0.059 Uiso 1 1 calc R . .
C13A C 0.6529(6) 0.3815(6) 0.2183(4) 0.045(3) Uiso 0.50 1 d PD A 1
C14A C 0.6266(11) 0.3104(7) 0.2044(7) 0.062(11) Uiso 0.50 1 d PD A 1
H14A H 0.6147 0.3115 0.1748 0.092 Uiso 0.50 1 calc PR A 1
H14B H 0.5812 0.2972 0.2199 0.092 Uiso 0.50 1 calc PR A 1
H14C H 0.6672 0.2771 0.2094 0.092 Uiso 0.50 1 calc PR A 1
C15A C 0.7240(6) 0.4032(7) 0.1925(4) 0.065(3) Uiso 0.50 1 d PD A 1
H15A H 0.7115 0.4017 0.1631 0.098 Uiso 0.50 1 calc PR A 1
H15B H 0.7660 0.3717 0.1982 0.098 Uiso 0.50 1 calc PR A 1
H15C H 0.7390 0.4499 0.2001 0.098 Uiso 0.50 1 calc PR A 1
C16A C 0.6720(7) 0.3825(6) 0.2638(3) 0.056(3) Uiso 0.50 1 d PD A 1
H16A H 0.6268 0.3701 0.2798 0.084 Uiso 0.50 1 calc PR A 1
H16B H 0.6888 0.4286 0.2717 0.084 Uiso 0.50 1 calc PR A 1
H16C H 0.7127 0.3495 0.2693 0.084 Uiso 0.50 1 calc PR A 1
C13C C 0.6508(5) 0.3812(5) 0.2047(3) 0.035(3) Uiso 0.50 1 d PD A 2
C14C C 0.6213(9) 0.3072(5) 0.2059(5) 0.030(6) Uiso 0.50 1 d PD A 2
H14G H 0.6645 0.2754 0.2057 0.044 Uiso 0.50 1 calc PR A 2
H14H H 0.5891 0.2987 0.1818 0.044 Uiso 0.50 1 calc PR A 2
H14I H 0.5916 0.3002 0.2312 0.044 Uiso 0.50 1 calc PR A 2
C15C C 0.7073(5) 0.3933(5) 0.1692(3) 0.042(2) Uiso 0.50 1 d PD A 2
H15G H 0.7481 0.3591 0.1707 0.063 Uiso 0.50 1 calc PR A 2
H15H H 0.7291 0.4393 0.1717 0.063 Uiso 0.50 1 calc PR A 2
H15I H 0.6809 0.3890 0.1427 0.063 Uiso 0.50 1 calc PR A 2
C16C C 0.6932(6) 0.3952(5) 0.2471(3) 0.044(2) Uiso 0.50 1 d PD A 2
H16G H 0.7370 0.3644 0.2495 0.066 Uiso 0.50 1 calc PR A 2
H16H H 0.6581 0.3870 0.2700 0.066 Uiso 0.50 1 calc PR A 2
H16I H 0.7107 0.4429 0.2478 0.066 Uiso 0.50 1 calc PR A 2
C17A C 0.3012(3) 0.6583(2) 0.23366(15) 0.0359(10) Uani 1 1 d . . .
N18A N 0.2977(2) 0.6088(2) 0.26244(12) 0.0383(9) Uani 1 1 d . . .
N19A N 0.2292(2) 0.6195(2) 0.28208(13) 0.0416(9) Uani 1 1 d . . .
H19A H 0.2124 0.5939 0.3025 0.050 Uiso 1 1 calc R . .
C20A C 0.1907(3) 0.6738(2) 0.26637(17) 0.0426(12) Uani 1 1 d . . .
C21A C 0.2355(3) 0.6994(2) 0.23491(16) 0.0417(12) Uani 1 1 d . . .
H21A H 0.2242 0.7373 0.2176 0.050 Uiso 1 1 calc R . .
C22A C 0.1124(3) 0.6943(3) 0.2821(2) 0.0567(15) Uani 1 1 d . . .
C23A C 0.0589(3) 0.6316(4) 0.2794(3) 0.077(2) Uani 1 1 d . . .
H23A H 0.0552 0.6166 0.2506 0.116 Uiso 1 1 calc R . .
H23B H 0.0083 0.6444 0.2895 0.116 Uiso 1 1 calc R . .
H23C H 0.0793 0.5943 0.2963 0.116 Uiso 1 1 calc R . .
C24A C 0.1185(4) 0.7190(4) 0.3270(2) 0.075(2) Uani 1 1 d . . .
H24A H 0.1434 0.6836 0.3437 0.112 Uiso 1 1 calc R . .
H24B H 0.0675 0.7279 0.3379 0.112 Uiso 1 1 calc R . .
H24C H 0.1486 0.7612 0.3280 0.112 Uiso 1 1 calc R . .
C25A C 0.0818(4) 0.7537(4) 0.2549(3) 0.087(2) Uani 1 1 d . . .
H25A H 0.1133 0.7945 0.2590 0.130 Uiso 1 1 calc R . .
H25B H 0.0292 0.7639 0.2626 0.130 Uiso 1 1 calc R . .
H25C H 0.0837 0.7401 0.2258 0.130 Uiso 1 1 calc R . .
N26A N 0.3551(2) 0.43535(18) 0.29192(12) 0.0321(8) Uani 1 1 d . . .
C27A C 0.2947(3) 0.3932(2) 0.28522(15) 0.0388(11) Uani 1 1 d . . .
C28A C 0.2814(3) 0.3371(3) 0.31094(18) 0.0516(13) Uani 1 1 d . . .
H28A H 0.2390 0.3078 0.3064 0.062 Uiso 1 1 calc R . .
C29A C 0.3311(4) 0.3252(3) 0.34318(18) 0.0601(16) Uani 1 1 d . . .
H29A H 0.3232 0.2868 0.3607 0.072 Uiso 1 1 calc R . .
C30A C 0.3927(3) 0.3685(3) 0.35036(16) 0.0480(13) Uani 1 1 d . . .
H30A H 0.4265 0.3608 0.3727 0.058 Uiso 1 1 calc R . .
C31A C 0.4030(3) 0.4239(2) 0.32342(14) 0.0322(10) Uani 1 1 d . . .
C32A C 0.2487(3) 0.4139(2) 0.24940(15) 0.0379(10) Uani 1 1 d . . .
N33A N 0.2749(2) 0.4662(2) 0.22585(12) 0.0358(9) Uani 1 1 d . . .
N34A N 0.2211(2) 0.4763(2) 0.19609(13) 0.0426(9) Uani 1 1 d . B .
H34A H 0.2244 0.5081 0.1769 0.051 Uiso 1 1 calc R . .
C35A C 0.1623(3) 0.4322(3) 0.19933(16) 0.0461(13) Uani 1 1 d D . .
C36A C 0.1777(3) 0.3907(3) 0.23335(17) 0.0477(13) Uani 1 1 d . B .
H36A H 0.1472 0.3544 0.2437 0.057 Uiso 1 1 calc R . .
C37A C 0.0929(7) 0.4403(7) 0.1691(4) 0.044(5) Uiso 0.50 1 d PD B 1
C38A C 0.1206(7) 0.4387(7) 0.1246(3) 0.052(3) Uiso 0.50 1 d PD B 1
H38A H 0.1493 0.3964 0.1198 0.078 Uiso 0.50 1 calc PR B 1
H38B H 0.1535 0.4784 0.1196 0.078 Uiso 0.50 1 calc PR B 1
H38C H 0.0769 0.4404 0.1059 0.078 Uiso 0.50 1 calc PR B 1
C39A C 0.0409(6) 0.3777(6) 0.1800(4) 0.060(3) Uiso 0.50 1 d PD B 1
H39A H 0.0680 0.3350 0.1740 0.090 Uiso 0.50 1 calc PR B 1
H39B H -0.0058 0.3797 0.1636 0.090 Uiso 0.50 1 calc PR B 1
H39C H 0.0280 0.3791 0.2095 0.090 Uiso 0.50 1 calc PR B 1
C40A C 0.0499(7) 0.5061(6) 0.1797(4) 0.067(3) Uiso 0.50 1 d PD B 1
H40A H 0.0332 0.5044 0.2085 0.100 Uiso 0.50 1 calc PR B 1
H40B H 0.0055 0.5106 0.1616 0.100 Uiso 0.50 1 calc PR B 1
H40C H 0.0835 0.5457 0.1757 0.100 Uiso 0.50 1 calc PR B 1
C37C C 0.0928(7) 0.4269(7) 0.1722(4) 0.049(5) Uiso 0.50 1 d PD B 2
C38C C 0.1128(9) 0.4645(8) 0.1303(4) 0.081(5) Uiso 0.50 1 d PD B 2
H38G H 0.0690 0.4621 0.1116 0.122 Uiso 0.50 1 calc PR B 2
H38H H 0.1566 0.4419 0.1174 0.122 Uiso 0.50 1 calc PR B 2
H38I H 0.1251 0.5125 0.1359 0.122 Uiso 0.50 1 calc PR B 2
C39C C 0.0707(7) 0.3551(5) 0.1617(4) 0.060(3) Uiso 0.50 1 d PD B 2
H39G H 0.0253 0.3556 0.1441 0.091 Uiso 0.50 1 calc PR B 2
H39H H 0.0598 0.3297 0.1871 0.091 Uiso 0.50 1 calc PR B 2
H39I H 0.1126 0.3327 0.1469 0.091 Uiso 0.50 1 calc PR B 2
C40C C 0.0287(8) 0.4661(9) 0.1932(5) 0.104(6) Uiso 0.50 1 d PD B 2
H40G H -0.0174 0.4633 0.1763 0.157 Uiso 0.50 1 calc PR B 2
H40H H 0.0434 0.5142 0.1966 0.157 Uiso 0.50 1 calc PR B 2
H40I H 0.0187 0.4460 0.2204 0.157 Uiso 0.50 1 calc PR B 2
C41A C 0.4641(2) 0.4753(2) 0.32609(13) 0.0286(9) Uani 1 1 d . . .
N42A N 0.45847(19) 0.53089(17) 0.30133(11) 0.0278(8) Uani 1 1 d . . .
N43A N 0.52091(19) 0.57000(18) 0.30971(11) 0.0292(8) Uani 1 1 d . . .
H43A H 0.5306 0.6095 0.2977 0.035 Uiso 1 1 calc R . .
C44A C 0.5667(2) 0.5409(2) 0.33893(14) 0.0320(10) Uani 1 1 d . . .
C45A C 0.5310(2) 0.4790(2) 0.35028(13) 0.0304(9) Uani 1 1 d . . .
H45A H 0.5483 0.4466 0.3700 0.037 Uiso 1 1 calc R . .
C46A C 0.6382(3) 0.5764(3) 0.35477(15) 0.0404(11) Uani 1 1 d . . .
C47A C 0.6913(3) 0.5902(3) 0.31828(19) 0.0580(15) Uani 1 1 d . . .
H47A H 0.7036 0.5469 0.3046 0.087 Uiso 1 1 calc R . .
H47B H 0.7382 0.6117 0.3283 0.087 Uiso 1 1 calc R . .
H47C H 0.6662 0.6210 0.2986 0.087 Uiso 1 1 calc R . .
C48A C 0.6146(3) 0.6450(3) 0.37594(17) 0.0514(13) Uani 1 1 d . . .
H48A H 0.5966 0.6774 0.3550 0.077 Uiso 1 1 calc R . .
H48B H 0.6586 0.6646 0.3903 0.077 Uiso 1 1 calc R . .
H48C H 0.5739 0.6362 0.3959 0.077 Uiso 1 1 calc R . .
C49A C 0.6774(3) 0.5279(3) 0.38665(18) 0.0558(15) Uani 1 1 d . . .
H49A H 0.6418 0.5175 0.4091 0.084 Uiso 1 1 calc R . .
H49B H 0.7226 0.5504 0.3980 0.084 Uiso 1 1 calc R . .
H49C H 0.6923 0.4852 0.3729 0.084 Uiso 1 1 calc R . .
Fe1B Fe 0.25187(3) 0.37064(3) 0.004626(16) 0.02433(14) Uani 1 1 d . . .
N2B N 0.20310(18) 0.35680(17) -0.05632(11) 0.0266(8) Uani 1 1 d . . .
C3B C 0.2258(2) 0.3035(2) -0.07998(13) 0.0257(9) Uani 1 1 d . . .
C4B C 0.1955(3) 0.2917(2) -0.11905(14) 0.0346(10) Uani 1 1 d . . .
H4B H 0.2130 0.2546 -0.1354 0.042 Uiso 1 1 calc R . .
C5B C 0.1389(3) 0.3358(2) -0.13368(14) 0.0368(10) Uani 1 1 d . . .
H5B H 0.1166 0.3284 -0.1600 0.044 Uiso 1 1 calc R . .
C6B C 0.1152(3) 0.3908(2) -0.10914(14) 0.0338(10) Uani 1 1 d . . .
H6B H 0.0768 0.4215 -0.1183 0.041 Uiso 1 1 calc R . .
C7B C 0.1498(2) 0.3992(2) -0.07067(13) 0.0269(9) Uani 1 1 d . . .
C8B C 0.2839(2) 0.2600(2) -0.05995(13) 0.0274(9) Uani 1 1 d . . .
N9B N 0.31378(18) 0.28173(17) -0.02359(11) 0.0267(8) Uani 1 1 d . . .
N10B N 0.36196(19) 0.23105(19) -0.01149(11) 0.0313(8) Uani 1 1 d . . .
H10B H 0.3882 0.2320 0.0116 0.038 Uiso 1 1 calc R . .
C11B C 0.3649(2) 0.1784(2) -0.03941(13) 0.0314(10) Uani 1 1 d . . .
C12B C 0.3149(2) 0.1958(2) -0.07108(14) 0.0328(10) Uani 1 1 d . . .
H12B H 0.3039 0.1699 -0.0952 0.039 Uiso 1 1 calc R . .
C13B C 0.4143(3) 0.1153(3) -0.03340(16) 0.0441(12) Uani 1 1 d . . .
C14B C 0.4995(3) 0.1376(3) -0.0309(2) 0.0667(17) Uani 1 1 d . . .
H14D H 0.5122 0.1659 -0.0550 0.100 Uiso 1 1 calc R . .
H14E H 0.5320 0.0968 -0.0306 0.100 Uiso 1 1 calc R . .
H14F H 0.5079 0.1642 -0.0057 0.100 Uiso 1 1 calc R . .
C15B C 0.3867(5) 0.0769(3) 0.0061(2) 0.077(2) Uani 1 1 d . . .
H15D H 0.4136 0.0331 0.0084 0.116 Uiso 1 1 calc R . .
H15E H 0.3319 0.0685 0.0041 0.116 Uiso 1 1 calc R . .
H15F H 0.3973 0.1050 0.0305 0.116 Uiso 1 1 calc R . .
C16B C 0.4043(3) 0.0672(3) -0.07103(19) 0.0570(15) Uani 1 1 d . . .
H16D H 0.4233 0.0901 -0.0959 0.086 Uiso 1 1 calc R . .
H16E H 0.3503 0.0563 -0.0746 0.086 Uiso 1 1 calc R . .
H16F H 0.4330 0.0248 -0.0664 0.086 Uiso 1 1 calc R . .
C17B C 0.1314(2) 0.4558(2) -0.04193(13) 0.0287(9) Uani 1 1 d . . .
N18B N 0.16687(19) 0.45689(17) -0.00475(11) 0.0276(8) Uani 1 1 d . . .
N19B N 0.1428(2) 0.51528(18) 0.01327(12) 0.0341(9) Uani 1 1 d . . .
H19B H 0.1576 0.5286 0.0379 0.041 Uiso 1 1 calc R . .
C20B C 0.0933(3) 0.5516(2) -0.01063(15) 0.0366(11) Uani 1 1 d . . .
C21B C 0.0835(3) 0.5132(2) -0.04649(15) 0.0359(10) Uani 1 1 d . . .
H21B H 0.0513 0.5235 -0.0692 0.043 Uiso 1 1 calc R . .
C22B C 0.0611(3) 0.6214(2) 0.00129(18) 0.0502(13) Uani 1 1 d . . .
C23B C 0.0357(4) 0.6226(4) 0.0459(2) 0.075(2) Uani 1 1 d . . .
H23D H 0.0008 0.5845 0.0510 0.113 Uiso 1 1 calc R . .
H23E H 0.0098 0.6661 0.0517 0.113 Uiso 1 1 calc R . .
H23F H 0.0802 0.6182 0.0640 0.113 Uiso 1 1 calc R . .
C24B C 0.1249(4) 0.6747(3) -0.0059(3) 0.088(2) Uani 1 1 d . . .
H24D H 0.1614 0.6726 0.0168 0.132 Uiso 1 1 calc R . .
H24E H 0.1027 0.7207 -0.0073 0.132 Uiso 1 1 calc R . .
H24F H 0.1509 0.6645 -0.0320 0.132 Uiso 1 1 calc R . .
C25B C -0.0072(4) 0.6384(3) -0.0274(2) 0.080(2) Uani 1 1 d . . .
H25D H 0.0097 0.6377 -0.0563 0.120 Uiso 1 1 calc R . .
H25E H -0.0269 0.6840 -0.0207 0.120 Uiso 1 1 calc R . .
H25F H -0.0474 0.6042 -0.0235 0.120 Uiso 1 1 calc R . .
N26B N 0.29398(19) 0.37020(18) 0.06746(11) 0.0289(8) Uani 1 1 d . . .
C27B C 0.2693(2) 0.3224(2) 0.09511(14) 0.0322(10) Uani 1 1 d . . .
C28B C 0.2978(3) 0.3198(3) 0.13518(14) 0.0379(11) Uani 1 1 d . . .
H28B H 0.2802 0.2861 0.1541 0.046 Uiso 1 1 calc R . .
C29B C 0.3533(3) 0.3679(3) 0.14721(14) 0.0432(12) Uani 1 1 d . . .
H29B H 0.3736 0.3671 0.1744 0.052 Uiso 1 1 calc R . .
C30B C 0.3778(3) 0.4160(3) 0.11926(15) 0.0421(11) Uani 1 1 d . . .
H30B H 0.4151 0.4488 0.1270 0.050 Uiso 1 1 calc R . .
C31B C 0.3474(3) 0.4164(2) 0.07905(14) 0.0335(10) Uani 1 1 d . . .
C32B C 0.2113(2) 0.2761(2) 0.07827(14) 0.0321(10) Uani 1 1 d . . .
N33B N 0.18676(19) 0.28804(18) 0.03886(12) 0.0298(8) Uani 1 1 d . . .
N34B N 0.1368(2) 0.23614(19) 0.03107(13) 0.0381(9) Uani 1 1 d . C .
H34B H 0.1135 0.2307 0.0073 0.046 Uiso 1 1 calc R . .
C35B C 0.1266(3) 0.1936(2) 0.06411(18) 0.0481(13) Uani 1 1 d D . .
C36B C 0.1738(3) 0.2171(3) 0.09470(17) 0.0447(13) Uani 1 1 d . C .
H36B H 0.1802 0.1981 0.1215 0.054 Uiso 1 1 calc R . .
C37B C 0.0682(5) 0.1384(5) 0.0702(3) 0.037(2) Uiso 0.50 1 d PD C 1
C38B C -0.0117(5) 0.1636(6) 0.0586(4) 0.055(3) Uiso 0.50 1 d PD C 1
H38D H -0.0485 0.1266 0.0629 0.083 Uiso 0.50 1 calc PR C 1
H38E H -0.0122 0.1773 0.0295 0.083 Uiso 0.50 1 calc PR C 1
H38F H -0.0253 0.2030 0.0758 0.083 Uiso 0.50 1 calc PR C 1
C39B C 0.0936(7) 0.0802(6) 0.0394(4) 0.062(3) Uiso 0.50 1 d PD C 1
H39D H 0.0582 0.0416 0.0414 0.093 Uiso 0.50 1 calc PR C 1
H39E H 0.1449 0.0648 0.0465 0.093 Uiso 0.50 1 calc PR C 1
H39F H 0.0933 0.0982 0.0112 0.093 Uiso 0.50 1 calc PR C 1
C40B C 0.0665(7) 0.1092(6) 0.1146(3) 0.059(3) Uiso 0.50 1 d PD C 1
H40D H 0.0273 0.0737 0.1165 0.089 Uiso 0.50 1 calc PR C 1
H40E H 0.0549 0.1461 0.1342 0.089 Uiso 0.50 1 calc PR C 1
H40F H 0.1162 0.0893 0.1213 0.089 Uiso 0.50 1 calc PR C 1
C37D C 0.0785(5) 0.1250(5) 0.0556(3) 0.035(2) Uiso 0.50 1 d PD C 2
C38D C -0.0031(5) 0.1470(5) 0.0442(3) 0.043(3) Uiso 0.50 1 d PD C 2
H38J H -0.0238 0.1760 0.0662 0.064 Uiso 0.50 1 calc PR C 2
H38K H -0.0350 0.1063 0.0409 0.064 Uiso 0.50 1 calc PR C 2
H38L H -0.0022 0.1729 0.0183 0.064 Uiso 0.50 1 calc PR C 2
C39D C 0.1128(7) 0.0799(6) 0.0224(4) 0.065(4) Uiso 0.50 1 d PD C 2
H39J H 0.1127 0.1045 -0.0039 0.097 Uiso 0.50 1 calc PR C 2
H39K H 0.0827 0.0379 0.0198 0.097 Uiso 0.50 1 calc PR C 2
H39L H 0.1652 0.0682 0.0300 0.097 Uiso 0.50 1 calc PR C 2
C40D C 0.0770(6) 0.0884(5) 0.0977(3) 0.045(2) Uiso 0.50 1 d PD C 2
H40J H 0.0548 0.1190 0.1185 0.068 Uiso 0.50 1 calc PR C 2
H40K H 0.1290 0.0764 0.1058 0.068 Uiso 0.50 1 calc PR C 2
H40L H 0.0463 0.0466 0.0956 0.068 Uiso 0.50 1 calc PR C 2
C41B C 0.3677(2) 0.4640(2) 0.04527(14) 0.0326(10) Uani 1 1 d . . .
N42B N 0.3374(2) 0.45285(17) 0.00792(12) 0.0307(8) Uani 1 1 d . . .
N43B N 0.3613(2) 0.50667(19) -0.01571(13) 0.0412(10) Uani 1 1 d . . .
H43B H 0.3501 0.5120 -0.0420 0.049 Uiso 1 1 calc R . .
C44B C 0.4048(3) 0.5513(2) 0.00667(18) 0.0469(13) Uani 1 1 d . . .
C45B C 0.4115(3) 0.5241(3) 0.04590(17) 0.0470(13) Uani 1 1 d . . .
H45B H 0.4397 0.5422 0.0684 0.056 Uiso 1 1 calc R . .
C46B C 0.4346(4) 0.6186(3) -0.0118(2) 0.0694(19) Uani 1 1 d . . .
C47B C 0.4780(4) 0.6052(4) -0.0515(3) 0.084(2) Uani 1 1 d . . .
H47D H 0.5193 0.5726 -0.0461 0.126 Uiso 1 1 calc R . .
H47E H 0.4993 0.6483 -0.0618 0.126 Uiso 1 1 calc R . .
H47F H 0.4434 0.5859 -0.0722 0.126 Uiso 1 1 calc R . .
C48B C 0.3647(5) 0.6654(3) -0.0205(3) 0.091(2) Uani 1 1 d . . .
H48D H 0.3320 0.6436 -0.0412 0.136 Uiso 1 1 calc R . .
H48E H 0.3823 0.7098 -0.0310 0.136 Uiso 1 1 calc R . .
H48F H 0.3360 0.6723 0.0050 0.136 Uiso 1 1 calc R . .
C49B C 0.4859(6) 0.6521(4) 0.0222(4) 0.154(5) Uani 1 1 d . . .
H49D H 0.4537 0.6703 0.0444 0.231 Uiso 1 1 calc R . .
H49E H 0.5155 0.6896 0.0100 0.231 Uiso 1 1 calc R . .
H49F H 0.5205 0.6175 0.0335 0.231 Uiso 1 1 calc R . .
B50 B 0.2504(5) 0.6143(4) 0.1094(2) 0.0639(19) Uani 1 1 d . . .
F51 F 0.2814(3) 0.57430(19) 0.13981(12) 0.0876(13) Uani 1 1 d . . .
F52 F 0.2258(3) 0.5723(2) 0.07724(13) 0.0973(14) Uani 1 1 d . . .
F53 F 0.3036(3) 0.6602(2) 0.09458(12) 0.0878(12) Uani 1 1 d . . .
F54 F 0.1876(3) 0.6497(3) 0.12482(17) 0.1129(16) Uani 1 1 d . . .
B55 B 0.4176(3) 0.2405(3) 0.24739(19) 0.0430(13) Uani 1 1 d . . .
F56 F 0.45494(18) 0.30067(14) 0.26074(11) 0.0610(9) Uani 1 1 d . . .
F57 F 0.3605(2) 0.2571(2) 0.22013(11) 0.0793(11) Uani 1 1 d . . .
F58 F 0.47226(19) 0.19833(16) 0.22793(13) 0.0695(10) Uani 1 1 d . . .
F59 F 0.3872(2) 0.20669(17) 0.28102(11) 0.0685(9) Uani 1 1 d . . .
B60 B 0.5142(4) 0.2912(4) 0.0711(2) 0.0575(17) Uani 1 1 d . . .
F61 F 0.4436(2) 0.2702(3) 0.05882(11) 0.0810(12) Uani 1 1 d . . .
F62 F 0.5231(2) 0.2805(3) 0.11224(11) 0.0912(14) Uani 1 1 d . . .
F63 F 0.5195(4) 0.3623(3) 0.0625(2) 0.148(2) Uani 1 1 d . . .
F64 F 0.5699(2) 0.2567(2) 0.04820(11) 0.0843(13) Uani 1 1 d . . .
B65 B 0.1711(3) 0.4966(4) 0.3701(2) 0.0583(18) Uani 1 1 d D . .
F66A F 0.2220(8) 0.5310(8) 0.3472(5) 0.185(8) Uiso 0.59 1 d PD D 1
F67A F 0.1054(6) 0.5302(6) 0.3811(4) 0.143(4) Uiso 0.59 1 d PD D 1
F68A F 0.2060(4) 0.4744(4) 0.4058(2) 0.071(2) Uiso 0.59 1 d PD D 1
F69A F 0.1436(5) 0.4390(5) 0.3468(3) 0.111(3) Uiso 0.59 1 d PD D 1
F66B F 0.2273(4) 0.5147(5) 0.3416(3) 0.050(2) Uiso 0.41 1 d PD D 2
F67B F 0.1506(8) 0.5591(6) 0.3913(4) 0.117(4) Uiso 0.41 1 d PD D 2
F68B F 0.2005(8) 0.4512(7) 0.3983(4) 0.102(5) Uiso 0.41 1 d PD D 2
F69B F 0.1054(8) 0.4772(9) 0.3522(5) 0.152(6) Uiso 0.41 1 d PD D 2
O70 O 0.0204(3) 0.3940(4) 0.3016(2) 0.0743(19) Uani 0.70 1 d P . .
H70 H 0.0433 0.4311 0.2974 0.089 Uiso 0.70 1 calc PR . .
C71 C -0.0452(5) 0.4065(5) 0.3241(3) 0.071(3) Uani 0.70 1 d P . .
H71A H -0.0316 0.4265 0.3512 0.085 Uiso 0.70 1 calc PR . .
H71B H -0.0722 0.3627 0.3291 0.085 Uiso 0.70 1 calc PR . .
C72 C -0.0970(4) 0.4551(4) 0.3012(3) 0.059(2) Uani 0.70 1 d P . .
F73 F -0.1177(3) 0.4304(3) 0.2646(2) 0.0891(18) Uani 0.70 1 d P . .
F74 F -0.1616(3) 0.4639(3) 0.3241(2) 0.098(2) Uani 0.70 1 d P . .
F75 F -0.0677(4) 0.5158(3) 0.2948(2) 0.106(2) Uani 0.70 1 d P . .
O76 O 0.2029(6) 0.7914(6) 0.1406(3) 0.091(3) Uiso 0.50 1 d P . .
H76 H 0.1816 0.7590 0.1280 0.109 Uiso 0.50 1 calc PR . .
C77 C 0.2554(8) 0.8204(7) 0.1159(4) 0.074(4) Uiso 0.50 1 d P . .
H77A H 0.2941 0.7854 0.1089 0.089 Uiso 0.50 1 calc PR . .
H77B H 0.2813 0.8572 0.1315 0.089 Uiso 0.50 1 calc PR . .
C78 C 0.2257(9) 0.8503(9) 0.0764(5) 0.088(4) Uiso 0.50 1 d P . .
F79 F 0.1757(6) 0.9032(6) 0.0874(3) 0.111(3) Uiso 0.50 1 d P . .
F80 F 0.2831(6) 0.8836(6) 0.0529(3) 0.110(3) Uiso 0.50 1 d P . .
F81 F 0.1861(7) 0.8061(7) 0.0554(4) 0.136(4) Uiso 0.50 1 d P . .
C82A C 0.0992(12) 0.2624(9) 0.3687(7) 0.087(6) Uiso 0.40 1 d PD E 1
H82A H 0.1488 0.2849 0.3711 0.131 Uiso 0.40 1 calc PR E 1
H82B H 0.0758 0.2590 0.3961 0.131 Uiso 0.40 1 calc PR E 1
H82C H 0.0663 0.2894 0.3505 0.131 Uiso 0.40 1 calc PR E 1
C83A C 0.1103(10) 0.1855(9) 0.3495(5) 0.080(5) Uiso 0.40 1 d PD E 1
H83A H 0.1424 0.1573 0.3685 0.096 Uiso 0.40 1 calc PR E 1
C84A C 0.0299(11) 0.1590(11) 0.3498(8) 0.097(7) Uiso 0.40 1 d PD E 1
H84A H 0.0290 0.1122 0.3387 0.146 Uiso 0.40 1 calc PR E 1
H84B H -0.0022 0.1887 0.3328 0.146 Uiso 0.40 1 calc PR E 1
H84C H 0.0106 0.1587 0.3782 0.146 Uiso 0.40 1 calc PR E 1
O85A O 0.1484(5) 0.1981(5) 0.3148(3) 0.047(2) Uiso 0.40 1 d PD E 1
C86A C 0.1478(7) 0.1501(6) 0.2804(4) 0.031(3) Uiso 0.40 1 d PD E 1
H86A H 0.0963 0.1285 0.2792 0.037 Uiso 0.40 1 calc PR E 1
C87A C 0.1585(9) 0.1900(8) 0.2417(5) 0.038(4) Uiso 0.40 1 d PD E 1
H87A H 0.1180 0.2243 0.2393 0.056 Uiso 0.40 1 calc PR E 1
H87B H 0.1566 0.1590 0.2180 0.056 Uiso 0.40 1 calc PR E 1
H87C H 0.2079 0.2132 0.2424 0.056 Uiso 0.40 1 calc PR E 1
C88A C 0.2057(11) 0.0931(9) 0.2850(7) 0.073(6) Uiso 0.40 1 d PD E 1
H88A H 0.1960 0.0680 0.3107 0.109 Uiso 0.40 1 calc PR E 1
H88B H 0.2570 0.1128 0.2858 0.109 Uiso 0.40 1 calc PR E 1
H88C H 0.2016 0.0616 0.2615 0.109 Uiso 0.40 1 calc PR E 1
C82B C 0.1278(18) 0.237(2) 0.3795(8) 0.132(13) Uiso 0.30 1 d PD F 2
H82D H 0.1794 0.2540 0.3749 0.197 Uiso 0.30 1 calc PR F 2
H82E H 0.1298 0.1963 0.3976 0.197 Uiso 0.30 1 calc PR F 2
H82F H 0.0968 0.2723 0.3925 0.197 Uiso 0.30 1 calc PR F 2
C83B C 0.0905(7) 0.2155(7) 0.3359(4) 0.032(3) Uiso 0.30 1 d PD F 2
H83B H 0.0866 0.2561 0.3172 0.039 Uiso 0.30 1 calc PR F 2
C84B C 0.0160(10) 0.1889(13) 0.3459(7) 0.066(6) Uiso 0.30 1 d PD F 2
H84D H -0.0105 0.1765 0.3204 0.099 Uiso 0.30 1 calc PR F 2
H84E H -0.0132 0.2239 0.3606 0.099 Uiso 0.30 1 calc PR F 2
H84F H 0.0213 0.1482 0.3634 0.099 Uiso 0.30 1 calc PR F 2
O85B O 0.1592(5) 0.1782(5) 0.3284(3) 0.024(2) Uiso 0.30 1 d PD F 2
C86B C 0.1575(10) 0.1413(8) 0.2904(5) 0.034(5) Uiso 0.30 1 d PD F 2
H86B H 0.1102 0.1130 0.2886 0.041 Uiso 0.30 1 calc PR F 2
C87B C 0.1652(14) 0.1858(11) 0.2525(7) 0.053(7) Uiso 0.30 1 d PD F 2
H87D H 0.1198 0.2146 0.2496 0.080 Uiso 0.30 1 calc PR F 2
H87E H 0.1704 0.1567 0.2280 0.080 Uiso 0.30 1 calc PR F 2
H87F H 0.2102 0.2150 0.2552 0.080 Uiso 0.30 1 calc PR F 2
C88B C 0.2273(11) 0.0951(10) 0.2920(7) 0.050(6) Uiso 0.30 1 d PD F 2
H88D H 0.2243 0.0654 0.3163 0.075 Uiso 0.30 1 calc PR F 2
H88E H 0.2733 0.1234 0.2936 0.075 Uiso 0.30 1 calc PR F 2
H88F H 0.2293 0.0669 0.2670 0.075 Uiso 0.30 1 calc PR F 2
O89 O 0.2803(9) 0.1725(8) 0.3823(5) 0.059(4) Uiso 0.25 1 d PD . .
H89 H 0.2952 0.1405 0.3670 0.071 Uiso 0.25 1 calc PR . .
C90 C 0.2650(15) 0.1466(8) 0.4222(6) 0.092(9) Uiso 0.25 1 d PD . .
H90A H 0.2097 0.1484 0.4277 0.110 Uiso 0.25 1 calc PR . .
H90B H 0.2913 0.1748 0.4432 0.110 Uiso 0.25 1 calc PR . .
C91 C 0.2938(10) 0.0704(8) 0.4245(5) 0.062(6) Uiso 0.25 1 d PD . .
F92 F 0.2647(7) 0.0343(6) 0.3944(4) 0.062(3) Uiso 0.25 1 d PD . .
F93 F 0.2710(8) 0.0472(7) 0.4608(4) 0.074(4) Uiso 0.25 1 d PD . .
F94 F 0.3661(8) 0.0739(10) 0.4201(6) 0.124(7) Uiso 0.25 1 d PD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1A N2A 2.129(4) . ?
Fe1A N26A 2.146(4) . ?
Fe1A N33A 2.183(4) . ?
Fe1A N18A 2.202(4) . ?
Fe1A N9A 2.212(4) . ?
Fe1A N42A 2.224(3) . ?
N2A C3A 1.353(6) . ?
N2A C7A 1.354(6) . ?
C3A C4A 1.405(7) . ?
C3A C8A 1.468(7) . ?
C4A C5A 1.392(8) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.407(8) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.386(7) . ?
C6A H6A 0.9500 . ?
C7A C17A 1.494(7) . ?
C8A N9A 1.354(6) . ?
C8A C12A 1.415(7) . ?
N9A N10A 1.364(5) . ?
N10A C11A 1.362(6) . ?
N10A H10A 0.8800 . ?
C11A C12A 1.403(7) . ?
C11A C13C 1.513(10) . ?
C11A C13A 1.596(11) . ?
C12A H12A 0.9500 . ?
C13A C16A 1.511(13) . ?
C13A C14A 1.530(13) . ?
C13A C15A 1.562(13) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C13C C14C 1.534(12) . ?
C13C C15C 1.537(12) . ?
C13C C16C 1.587(12) . ?
C14C H14G 0.9800 . ?
C14C H14H 0.9800 . ?
C14C H14I 0.9800 . ?
C15C H15G 0.9800 . ?
C15C H15H 0.9800 . ?
C15C H15I 0.9800 . ?
C16C H16G 0.9800 . ?
C16C H16H 0.9800 . ?
C16C H16I 0.9800 . ?
C17A N18A 1.343(6) . ?
C17A C21A 1.408(6) . ?
N18A N19A 1.378(5) . ?
N19A C20A 1.356(6) . ?
N19A H19A 0.8800 . ?
C20A C21A 1.382(8) . ?
C20A C22A 1.523(7) . ?
C21A H21A 0.9500 . ?
C22A C24A 1.536(9) . ?
C22A C23A 1.545(9) . ?
C22A C25A 1.552(9) . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
N26A C31A 1.343(6) . ?
N26A C27A 1.360(6) . ?
C27A C28A 1.395(7) . ?
C27A C32A 1.472(7) . ?
C28A C29A 1.382(8) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.394(8) . ?
C29A H29A 0.9500 . ?
C30A C31A 1.400(7) . ?
C30A H30A 0.9500 . ?
C31A C41A 1.471(6) . ?
C32A N33A 1.355(6) . ?
C32A C36A 1.427(7) . ?
N33A N34A 1.365(5) . ?
N34A C35A 1.349(6) . ?
N34A H34A 0.8800 . ?
C35A C36A 1.394(8) . ?
C35A C37C 1.510(13) . ?
C35A C37A 1.574(12) . ?
C36A H36A 0.9500 . ?
C37A C38A 1.520(13) . ?
C37A C40A 1.530(14) . ?
C37A C39A 1.566(14) . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C39A H39A 0.9800 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9800 . ?
C40A H40A 0.9800 . ?
C40A H40B 0.9800 . ?
C40A H40C 0.9800 . ?
C37C C39C 1.494(14) . ?
C37C C40C 1.523(14) . ?
C37C C38C 1.582(14) . ?
C38C H38G 0.9800 . ?
C38C H38H 0.9800 . ?
C38C H38I 0.9800 . ?
C39C H39G 0.9800 . ?
C39C H39H 0.9800 . ?
C39C H39I 0.9800 . ?
C40C H40G 0.9800 . ?
C40C H40H 0.9800 . ?
C40C H40I 0.9800 . ?
C41A N42A 1.353(6) . ?
C41A C45A 1.416(6) . ?
N42A N43A 1.365(5) . ?
N43A C44A 1.366(6) . ?
N43A H43A 0.8800 . ?
C44A C45A 1.410(7) . ?
C44A C46A 1.525(6) . ?
C45A H45A 0.9500 . ?
C46A C47A 1.531(8) . ?
C46A C48A 1.559(7) . ?
C46A C49A 1.562(7) . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C49A H49A 0.9800 . ?
C49A H49B 0.9800 . ?
C49A H49C 0.9800 . ?
Fe1B N26B 2.166(3) . ?
Fe1B N2B 2.170(3) . ?
Fe1B N42B 2.202(3) . ?
Fe1B N9B 2.243(3) . ?
Fe1B N33B 2.267(4) . ?
Fe1B N18B 2.271(3) . ?
N2B C7B 1.334(5) . ?
N2B C3B 1.352(5) . ?
C3B C4B 1.392(6) . ?
C3B C8B 1.479(6) . ?
C4B C5B 1.399(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.399(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.397(6) . ?
C6B H6B 0.9500 . ?
C7B C17B 1.480(6) . ?
C8B N9B 1.358(6) . ?
C8B C12B 1.412(6) . ?
N9B N10B 1.360(5) . ?
N10B C11B 1.369(6) . ?
N10B H10B 0.8800 . ?
C11B C12B 1.393(6) . ?
C11B C13B 1.520(6) . ?
C12B H12B 0.9500 . ?
C13B C16B 1.548(8) . ?
C13B C15B 1.559(8) . ?
C13B C14B 1.564(8) . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17B N18B 1.356(6) . ?
C17B C21B 1.409(6) . ?
N18B N19B 1.348(5) . ?
N19B C20B 1.364(6) . ?
N19B H19B 0.8800 . ?
C20B C21B 1.393(7) . ?
C20B C22B 1.525(6) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.513(9) . ?
C22B C24B 1.547(9) . ?
C22B C25B 1.556(8) . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
N26B C31B 1.354(6) . ?
N26B C27B 1.364(6) . ?
C27B C28B 1.392(6) . ?
C27B C32B 1.469(6) . ?
C28B C29B 1.410(7) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.374(7) . ?
C29B H29B 0.9500 . ?
C30B C31B 1.409(7) . ?
C30B H30B 0.9500 . ?
C31B C41B 1.479(7) . ?
C32B N33B 1.368(6) . ?
C32B C36B 1.429(6) . ?
N33B N34B 1.365(5) . ?
N34B C35B 1.367(6) . ?
N34B H34B 0.8800 . ?
C35B C36B 1.372(7) . ?
C35B C37B 1.500(9) . ?
C35B C37D 1.607(10) . ?
C36B H36B 0.9500 . ?
C37B C38B 1.536(12) . ?
C37B C40B 1.548(12) . ?
C37B C39B 1.576(12) . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39B H39D 0.9800 . ?
C39B H39E 0.9800 . ?
C39B H39F 0.9800 . ?
C40B H40D 0.9800 . ?
C40B H40E 0.9800 . ?
C40B H40F 0.9800 . ?
C37D C39D 1.513(12) . ?
C37D C40D 1.541(11) . ?
C37D C38D 1.543(11) . ?
C38D H38J 0.9800 . ?
C38D H38K 0.9800 . ?
C38D H38L 0.9800 . ?
C39D H39J 0.9800 . ?
C39D H39K 0.9800 . ?
C39D H39L 0.9800 . ?
C40D H40J 0.9800 . ?
C40D H40K 0.9800 . ?
C40D H40L 0.9800 . ?
C41B N42B 1.340(6) . ?
C41B C45B 1.404(6) . ?
N42B N43B 1.366(5) . ?
N43B C44B 1.368(6) . ?
N43B H43B 0.8800 . ?
C44B C45B 1.382(8) . ?
C44B C46B 1.534(7) . ?
C45B H45B 0.9500 . ?
C46B C47B 1.520(11) . ?
C46B C48B 1.557(10) . ?
C46B C49B 1.567(11) . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
B50 F51 1.370(8) . ?
B50 F53 1.382(9) . ?
B50 F52 1.393(7) . ?
B50 F54 1.395(10) . ?
B55 F57 1.376(7) . ?
B55 F59 1.381(7) . ?
B55 F56 1.414(6) . ?
B55 F58 1.414(7) . ?
B60 F62 1.357(8) . ?
B60 F61 1.367(8) . ?
B60 F64 1.401(8) . ?
B60 F63 1.418(9) . ?
B65 F66A 1.342(12) . ?
B65 F67A 1.375(10) . ?
B65 F68A 1.379(9) . ?
B65 F69A 1.438(10) . ?
B65 F69B 1.348(12) . ?
B65 F68B 1.374(11) . ?
B65 F66B 1.399(9) . ?
B65 F67B 1.444(11) . ?
O70 C71 1.387(11) . ?
O70 H70 0.8400 . ?
C71 C72 1.510(13) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 F75 1.309(11) . ?
C72 F73 1.330(10) . ?
C72 F74 1.367(10) . ?
O76 C77 1.348(17) . ?
O76 H76 0.8400 . ?
C77 C78 1.50(2) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 F81 1.302(19) . ?
C78 F79 1.402(18) . ?
C78 F80 1.421(18) . ?
C82A C83A 1.636(16) . ?
C82A H82A 0.9800 . ?
C82A H82B 0.9800 . ?
C82A H82C 0.9800 . ?
C83A O85A 1.330(14) . ?
C83A C84A 1.506(16) . ?
C83A H83A 1.0000 . ?
C84A H84A 0.9800 . ?
C84A H84B 0.9800 . ?
C84A H84C 0.9800 . ?
O85A C86A 1.458(12) . ?
C86A C87A 1.487(14) . ?
C86A C88A 1.515(15) . ?
C86A H86A 1.0000 . ?
C87A H87A 0.9800 . ?
C87A H87B 0.9800 . ?
C87A H87C 0.9800 . ?
C88A H88A 0.9800 . ?
C88A H88B 0.9800 . ?
C88A H88C 0.9800 . ?
C82B C83B 1.609(18) . ?
C82B H82D 0.9800 . ?
C82B H82E 0.9800 . ?
C82B H82F 0.9800 . ?
C83B O85B 1.430(13) . ?
C83B C84B 1.446(16) . ?
C83B H83B 1.0000 . ?
C84B H84D 0.9800 . ?
C84B H84E 0.9800 . ?
C84B H84F 0.9800 . ?
O85B C86B 1.428(14) . ?
C86B C87B 1.510(17) . ?
C86B C88B 1.525(16) . ?
C86B H86B 1.0000 . ?
C87B H87D 0.9800 . ?
C87B H87E 0.9800 . ?
C87B H87F 0.9800 . ?
C88B H88D 0.9800 . ?
C88B H88E 0.9800 . ?
C88B H88F 0.9800 . ?
O89 C90 1.413(17) . ?
O89 H89 0.8400 . ?
C90 C91 1.572(15) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 F94 1.281(16) . ?
C91 F92 1.307(15) . ?
C91 F93 1.323(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Fe1A N26A 170.27(13) . . ?
N2A Fe1A N33A 110.24(14) . . ?
N26A Fe1A N33A 74.91(14) . . ?
N2A Fe1A N18A 74.39(15) . . ?
N26A Fe1A N18A 114.55(14) . . ?
N33A Fe1A N18A 88.13(14) . . ?
N2A Fe1A N9A 73.91(14) . . ?
N26A Fe1A N9A 97.11(14) . . ?
N33A Fe1A N9A 102.32(13) . . ?
N18A Fe1A N9A 148.29(15) . . ?
N2A Fe1A N42A 101.20(13) . . ?
N26A Fe1A N42A 73.72(13) . . ?
N33A Fe1A N42A 148.51(14) . . ?
N18A Fe1A N42A 102.38(13) . . ?
N9A Fe1A N42A 84.29(13) . . ?
C3A N2A C7A 120.1(4) . . ?
C3A N2A Fe1A 120.2(3) . . ?
C7A N2A Fe1A 119.7(3) . . ?
N2A C3A C4A 121.2(4) . . ?
N2A C3A C8A 112.3(4) . . ?
C4A C3A C8A 126.5(4) . . ?
C5A C4A C3A 118.8(5) . . ?
C5A C4A H4A 120.6 . . ?
C3A C4A H4A 120.6 . . ?
C4A C5A C6A 119.6(5) . . ?
C4A C5A H5A 120.2 . . ?
C6A C5A H5A 120.2 . . ?
C7A C6A C5A 118.6(5) . . ?
C7A C6A H6A 120.7 . . ?
C5A C6A H6A 120.7 . . ?
N2A C7A C6A 121.8(5) . . ?
N2A C7A C17A 112.7(4) . . ?
C6A C7A C17A 125.5(4) . . ?
N9A C8A C12A 110.5(4) . . ?
N9A C8A C3A 116.8(4) . . ?
C12A C8A C3A 132.5(4) . . ?
C8A N9A N10A 105.3(3) . . ?
C8A N9A Fe1A 113.7(3) . . ?
N10A N9A Fe1A 134.5(3) . . ?
C11A N10A N9A 112.5(4) . . ?
C11A N10A H10A 123.8 . . ?
N9A N10A H10A 123.8 . . ?
N10A C11A C12A 106.1(4) . . ?
N10A C11A C13C 125.4(5) . . ?
C12A C11A C13C 128.4(5) . . ?
N10A C11A C13A 117.4(5) . . ?
C12A C11A C13A 134.4(6) . . ?
C11A C12A C8A 105.5(4) . . ?
C11A C12A H12A 127.3 . . ?
C8A C12A H12A 127.3 . . ?
C16A C13A C14A 111.5(11) . . ?
C16A C13A C15A 109.9(9) . . ?
C14A C13A C15A 109.2(11) . . ?
C16A C13A C11A 114.9(9) . . ?
C14A C13A C11A 105.2(10) . . ?
C15A C13A C11A 105.9(8) . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C13A C15A H15A 109.5 . . ?
C13A C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
C13A C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C13A C16A H16A 109.5 . . ?
C13A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C13A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C11A C13C C14C 111.6(8) . . ?
C11A C13C C15C 112.9(8) . . ?
C14C C13C C15C 112.5(9) . . ?
C11A C13C C16C 103.6(7) . . ?
C14C C13C C16C 107.3(9) . . ?
C15C C13C C16C 108.4(8) . . ?
C13C C14C H14G 109.5 . . ?
C13C C14C H14H 109.5 . . ?
H14G C14C H14H 109.5 . . ?
C13C C14C H14I 109.5 . . ?
H14G C14C H14I 109.5 . . ?
H14H C14C H14I 109.5 . . ?
C13C C15C H15G 109.5 . . ?
C13C C15C H15H 109.5 . . ?
H15G C15C H15H 109.5 . . ?
C13C C15C H15I 109.5 . . ?
H15G C15C H15I 109.5 . . ?
H15H C15C H15I 109.5 . . ?
C13C C16C H16G 109.5 . . ?
C13C C16C H16H 109.5 . . ?
H16G C16C H16H 109.5 . . ?
C13C C16C H16I 109.5 . . ?
H16G C16C H16I 109.5 . . ?
H16H C16C H16I 109.5 . . ?
N18A C17A C21A 110.6(4) . . ?
N18A C17A C7A 116.1(4) . . ?
C21A C17A C7A 133.1(4) . . ?
C17A N18A N19A 104.6(4) . . ?
C17A N18A Fe1A 114.8(3) . . ?
N19A N18A Fe1A 136.0(3) . . ?
C20A N19A N18A 112.4(4) . . ?
C20A N19A H19A 123.8 . . ?
N18A N19A H19A 123.8 . . ?
N19A C20A C21A 106.0(4) . . ?
N19A C20A C22A 122.1(5) . . ?
C21A C20A C22A 131.9(5) . . ?
C20A C21A C17A 106.4(4) . . ?
C20A C21A H21A 126.8 . . ?
C17A C21A H21A 126.8 . . ?
C20A C22A C24A 109.6(5) . . ?
C20A C22A C23A 108.9(4) . . ?
C24A C22A C23A 110.2(6) . . ?
C20A C22A C25A 108.6(5) . . ?
C24A C22A C25A 109.2(5) . . ?
C23A C22A C25A 110.3(5) . . ?
C22A C23A H23A 109.5 . . ?
C22A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C22A C24A H24A 109.5 . . ?
C22A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C22A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22A C25A H25A 109.5 . . ?
C22A C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C22A C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C31A N26A C27A 120.7(4) . . ?
C31A N26A Fe1A 120.3(3) . . ?
C27A N26A Fe1A 119.0(3) . . ?
N26A C27A C28A 120.7(5) . . ?
N26A C27A C32A 112.9(4) . . ?
C28A C27A C32A 126.4(4) . . ?
C29A C28A C27A 118.5(5) . . ?
C29A C28A H28A 120.8 . . ?
C27A C28A H28A 120.8 . . ?
C28A C29A C30A 121.1(5) . . ?
C28A C29A H29A 119.5 . . ?
C30A C29A H29A 119.5 . . ?
C29A C30A C31A 117.7(5) . . ?
C29A C30A H30A 121.2 . . ?
C31A C30A H30A 121.2 . . ?
N26A C31A C30A 121.4(4) . . ?
N26A C31A C41A 112.9(4) . . ?
C30A C31A C41A 125.7(4) . . ?
N33A C32A C36A 109.4(4) . . ?
N33A C32A C27A 117.7(4) . . ?
C36A C32A C27A 132.9(4) . . ?
C32A N33A N34A 105.7(4) . . ?
C32A N33A Fe1A 115.0(3) . . ?
N34A N33A Fe1A 138.0(3) . . ?
C35A N34A N33A 112.6(4) . . ?
C35A N34A H34A 123.7 . . ?
N33A N34A H34A 123.7 . . ?
N34A C35A C36A 106.4(4) . . ?
N34A C35A C37C 128.2(7) . . ?
C36A C35A C37C 125.3(7) . . ?
N34A C35A C37A 118.9(6) . . ?
C36A C35A C37A 134.5(6) . . ?
C35A C36A C32A 105.9(4) . . ?
C35A C36A H36A 127.1 . . ?
C32A C36A H36A 127.1 . . ?
C38A C37A C40A 112.8(10) . . ?
C38A C37A C39A 112.8(10) . . ?
C40A C37A C39A 108.4(9) . . ?
C38A C37A C35A 109.8(9) . . ?
C40A C37A C35A 109.1(9) . . ?
C39A C37A C35A 103.5(9) . . ?
C37A C38A H38A 109.5 . . ?
C37A C38A H38B 109.5 . . ?
H38A C38A H38B 109.5 . . ?
C37A C38A H38C 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
C37A C39A H39A 109.5 . . ?
C37A C39A H39B 109.5 . . ?
H39A C39A H39B 109.5 . . ?
C37A C39A H39C 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C37A C40A H40A 109.5 . . ?
C37A C40A H40B 109.5 . . ?
H40A C40A H40B 109.5 . . ?
C37A C40A H40C 109.5 . . ?
H40A C40A H40C 109.5 . . ?
H40B C40A H40C 109.5 . . ?
C39C C37C C35A 114.0(10) . . ?
C39C C37C C40C 112.4(11) . . ?
C35A C37C C40C 107.7(10) . . ?
C39C C37C C38C 107.2(10) . . ?
C35A C37C C38C 106.8(10) . . ?
C40C C37C C38C 108.5(11) . . ?
C37C C38C H38G 109.5 . . ?
C37C C38C H38H 109.5 . . ?
H38G C38C H38H 109.5 . . ?
C37C C38C H38I 109.5 . . ?
H38G C38C H38I 109.5 . . ?
H38H C38C H38I 109.5 . . ?
C37C C39C H39G 109.5 . . ?
C37C C39C H39H 109.5 . . ?
H39G C39C H39H 109.5 . . ?
C37C C39C H39I 109.5 . . ?
H39G C39C H39I 109.5 . . ?
H39H C39C H39I 109.5 . . ?
C37C C40C H40G 109.5 . . ?
C37C C40C H40H 109.5 . . ?
H40G C40C H40H 109.5 . . ?
C37C C40C H40I 109.5 . . ?
H40G C40C H40I 109.5 . . ?
H40H C40C H40I 109.5 . . ?
N42A C41A C45A 110.3(4) . . ?
N42A C41A C31A 117.3(4) . . ?
C45A C41A C31A 132.4(4) . . ?
C41A N42A N43A 105.8(3) . . ?
C41A N42A Fe1A 114.2(3) . . ?
N43A N42A Fe1A 137.8(3) . . ?
N42A N43A C44A 112.3(3) . . ?
N42A N43A H43A 123.8 . . ?
C44A N43A H43A 123.8 . . ?
N43A C44A C45A 105.9(4) . . ?
N43A C44A C46A 122.0(4) . . ?
C45A C44A C46A 132.0(4) . . ?
C44A C45A C41A 105.6(4) . . ?
C44A C45A H45A 127.2 . . ?
C41A C45A H45A 127.2 . . ?
C44A C46A C47A 108.9(4) . . ?
C44A C46A C48A 108.6(4) . . ?
C47A C46A C48A 110.6(4) . . ?
C44A C46A C49A 108.1(4) . . ?
C47A C46A C49A 110.3(4) . . ?
C48A C46A C49A 110.3(4) . . ?
C46A C47A H47A 109.5 . . ?
C46A C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
C46A C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C46A C48A H48A 109.5 . . ?
C46A C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C46A C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C46A C49A H49A 109.5 . . ?
C46A C49A H49B 109.5 . . ?
H49A C49A H49B 109.5 . . ?
C46A C49A H49C 109.5 . . ?
H49A C49A H49C 109.5 . . ?
H49B C49A H49C 109.5 . . ?
N26B Fe1B N2B 171.85(13) . . ?
N26B Fe1B N42B 73.96(13) . . ?
N2B Fe1B N42B 113.88(13) . . ?
N26B Fe1B N9B 102.36(13) . . ?
N2B Fe1B N9B 74.02(12) . . ?
N42B Fe1B N9B 104.55(13) . . ?
N26B Fe1B N33B 73.15(13) . . ?
N2B Fe1B N33B 99.04(13) . . ?
N42B Fe1B N33B 147.08(13) . . ?
N9B Fe1B N33B 83.97(13) . . ?
N26B Fe1B N18B 110.71(13) . . ?
N2B Fe1B N18B 73.16(13) . . ?
N42B Fe1B N18B 85.22(13) . . ?
N9B Fe1B N18B 146.93(13) . . ?
N33B Fe1B N18B 105.05(12) . . ?
C7B N2B C3B 119.1(4) . . ?
C7B N2B Fe1B 121.2(3) . . ?
C3B N2B Fe1B 119.7(3) . . ?
N2B C3B C4B 122.0(4) . . ?
N2B C3B C8B 113.4(3) . . ?
C4B C3B C8B 124.6(4) . . ?
C3B C4B C5B 118.6(4) . . ?
C3B C4B H4B 120.7 . . ?
C5B C4B H4B 120.7 . . ?
C4B C5B C6B 119.4(4) . . ?
C4B C5B H5B 120.3 . . ?
C6B C5B H5B 120.3 . . ?
C7B C6B C5B 117.8(4) . . ?
C7B C6B H6B 121.1 . . ?
C5B C6B H6B 121.1 . . ?
N2B C7B C6B 123.0(4) . . ?
N2B C7B C17B 113.4(4) . . ?
C6B C7B C17B 123.6(4) . . ?
N9B C8B C12B 110.4(4) . . ?
N9B C8B C3B 118.0(3) . . ?
C12B C8B C3B 131.6(4) . . ?
C8B N9B N10B 105.3(3) . . ?
C8B N9B Fe1B 114.0(3) . . ?
N10B N9B Fe1B 138.4(3) . . ?
N9B N10B C11B 112.2(3) . . ?
N9B N10B H10B 123.9 . . ?
C11B N10B H10B 123.9 . . ?
N10B C11B C12B 106.3(4) . . ?
N10B C11B C13B 123.0(4) . . ?
C12B C11B C13B 130.7(4) . . ?
C11B C12B C8B 105.7(4) . . ?
C11B C12B H12B 127.1 . . ?
C8B C12B H12B 127.1 . . ?
C11B C13B C16B 109.0(4) . . ?
C11B C13B C15B 108.5(4) . . ?
C16B C13B C15B 108.6(5) . . ?
C11B C13B C14B 109.2(4) . . ?
C16B C13B C14B 108.5(5) . . ?
C15B C13B C14B 113.0(5) . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C13B C15B H15D 109.5 . . ?
C13B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C13B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C13B C16B H16D 109.5 . . ?
C13B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C13B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
N18B C17B C21B 110.8(4) . . ?
N18B C17B C7B 118.0(4) . . ?
C21B C17B C7B 131.1(4) . . ?
N19B N18B C17B 104.7(3) . . ?
N19B N18B Fe1B 140.8(3) . . ?
C17B N18B Fe1B 114.2(3) . . ?
N18B N19B C20B 113.2(4) . . ?
N18B N19B H19B 123.4 . . ?
C20B N19B H19B 123.4 . . ?
N19B C20B C21B 105.9(4) . . ?
N19B C20B C22B 123.9(4) . . ?
C21B C20B C22B 130.2(4) . . ?
C20B C21B C17B 105.4(4) . . ?
C20B C21B H21B 127.3 . . ?
C17B C21B H21B 127.3 . . ?
C23B C22B C20B 111.5(5) . . ?
C23B C22B C24B 110.4(6) . . ?
C20B C22B C24B 107.0(4) . . ?
C23B C22B C25B 109.9(5) . . ?
C20B C22B C25B 109.0(4) . . ?
C24B C22B C25B 109.0(5) . . ?
C22B C23B H23D 109.5 . . ?
C22B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C22B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C22B C24B H24D 109.5 . . ?
C22B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C22B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C22B C25B H25D 109.5 . . ?
C22B C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C22B C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C31B N26B C27B 119.5(4) . . ?
C31B N26B Fe1B 119.7(3) . . ?
C27B N26B Fe1B 120.8(3) . . ?
N26B C27B C28B 121.6(4) . . ?
N26B C27B C32B 113.4(4) . . ?
C28B C27B C32B 125.0(4) . . ?
C27B C28B C29B 118.8(4) . . ?
C27B C28B H28B 120.6 . . ?
C29B C28B H28B 120.6 . . ?
C30B C29B C28B 119.4(4) . . ?
C30B C29B H29B 120.3 . . ?
C28B C29B H29B 120.3 . . ?
C29B C30B C31B 119.6(4) . . ?
C29B C30B H30B 120.2 . . ?
C31B C30B H30B 120.2 . . ?
N26B C31B C30B 121.1(4) . . ?
N26B C31B C41B 112.4(4) . . ?
C30B C31B C41B 126.5(4) . . ?
N33B C32B C36B 109.8(4) . . ?
N33B C32B C27B 117.5(4) . . ?
C36B C32B C27B 132.7(4) . . ?
N34B N33B C32B 104.4(3) . . ?
N34B N33B Fe1B 139.7(3) . . ?
C32B N33B Fe1B 114.7(3) . . ?
N33B N34B C35B 113.0(4) . . ?
N33B N34B H34B 123.5 . . ?
C35B N34B H34B 123.5 . . ?
N34B C35B C36B 106.4(4) . . ?
N34B C35B C37B 129.0(5) . . ?
C36B C35B C37B 124.0(6) . . ?
N34B C35B C37D 116.1(5) . . ?
C36B C35B C37D 136.2(5) . . ?
C35B C36B C32B 106.3(4) . . ?
C35B C36B H36B 126.9 . . ?
C32B C36B H36B 126.9 . . ?
C35B C37B C38B 111.4(7) . . ?
C35B C37B C40B 113.6(8) . . ?
C38B C37B C40B 109.2(8) . . ?
C35B C37B C39B 103.8(8) . . ?
C38B C37B C39B 109.4(9) . . ?
C40B C37B C39B 109.2(8) . . ?
C37B C38B H38D 109.5 . . ?
C37B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C37B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C37B C39B H39D 109.5 . . ?
C37B C39B H39E 109.5 . . ?
H39D C39B H39E 109.5 . . ?
C37B C39B H39F 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
C37B C40B H40D 109.5 . . ?
C37B C40B H40E 109.5 . . ?
H40D C40B H40E 109.5 . . ?
C37B C40B H40F 109.5 . . ?
H40D C40B H40F 109.5 . . ?
H40E C40B H40F 109.5 . . ?
C39D C37D C40D 111.5(8) . . ?
C39D C37D C38D 111.3(8) . . ?
C40D C37D C38D 109.0(8) . . ?
C39D C37D C35B 113.3(8) . . ?
C40D C37D C35B 104.0(7) . . ?
C38D C37D C35B 107.4(7) . . ?
C37D C38D H38J 109.5 . . ?
C37D C38D H38K 109.5 . . ?
H38J C38D H38K 109.5 . . ?
C37D C38D H38L 109.5 . . ?
H38J C38D H38L 109.5 . . ?
H38K C38D H38L 109.5 . . ?
C37D C39D H39J 109.5 . . ?
C37D C39D H39K 109.5 . . ?
H39J C39D H39K 109.5 . . ?
C37D C39D H39L 109.5 . . ?
H39J C39D H39L 109.5 . . ?
H39K C39D H39L 109.5 . . ?
C37D C40D H40J 109.5 . . ?
C37D C40D H40K 109.5 . . ?
H40J C40D H40K 109.5 . . ?
C37D C40D H40L 109.5 . . ?
H40J C40D H40L 109.5 . . ?
H40K C40D H40L 109.5 . . ?
N42B C41B C45B 111.5(4) . . ?
N42B C41B C31B 118.0(4) . . ?
C45B C41B C31B 130.3(4) . . ?
C41B N42B N43B 105.0(3) . . ?
C41B N42B Fe1B 115.7(3) . . ?
N43B N42B Fe1B 138.0(3) . . ?
N42B N43B C44B 111.4(4) . . ?
N42B N43B H43B 124.3 . . ?
C44B N43B H43B 124.3 . . ?
N43B C44B C45B 106.9(4) . . ?
N43B C44B C46B 121.9(5) . . ?
C45B C44B C46B 131.1(5) . . ?
C44B C45B C41B 105.1(4) . . ?
C44B C45B H45B 127.4 . . ?
C41B C45B H45B 127.4 . . ?
C47B C46B C44B 110.7(5) . . ?
C47B C46B C48B 110.1(6) . . ?
C44B C46B C48B 107.7(5) . . ?
C47B C46B C49B 112.2(7) . . ?
C44B C46B C49B 106.2(6) . . ?
C48B C46B C49B 109.7(7) . . ?
C46B C47B H47D 109.5 . . ?
C46B C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C46B C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C46B C48B H48D 109.5 . . ?
C46B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C46B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C46B C49B H49D 109.5 . . ?
C46B C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C46B C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
F51 B50 F53 110.5(6) . . ?
F51 B50 F52 109.1(5) . . ?
F53 B50 F52 109.4(6) . . ?
F51 B50 F54 109.8(6) . . ?
F53 B50 F54 109.8(6) . . ?
F52 B50 F54 108.2(6) . . ?
F57 B55 F59 109.6(5) . . ?
F57 B55 F56 109.9(4) . . ?
F59 B55 F56 109.6(5) . . ?
F57 B55 F58 110.3(5) . . ?
F59 B55 F58 109.7(4) . . ?
F56 B55 F58 107.7(4) . . ?
F62 B60 F61 110.2(6) . . ?
F62 B60 F64 111.5(5) . . ?
F61 B60 F64 109.6(6) . . ?
F62 B60 F63 109.8(7) . . ?
F61 B60 F63 107.1(6) . . ?
F64 B60 F63 108.6(6) . . ?
F66A B65 F67A 117.8(9) . . ?
F66A B65 F68A 108.9(9) . . ?
F67A B65 F68A 108.0(7) . . ?
F66A B65 F69A 108.9(9) . . ?
F67A B65 F69A 103.0(7) . . ?
F68A B65 F69A 110.0(7) . . ?
F69B B65 F68B 115.3(10) . . ?
F69B B65 F66B 113.0(9) . . ?
F68B B65 F66B 109.6(8) . . ?
F69B B65 F67B 103.2(9) . . ?
F68B B65 F67B 108.8(9) . . ?
F66B B65 F67B 106.2(8) . . ?
C71 O70 H70 109.5 . . ?
O70 C71 C72 110.8(8) . . ?
O70 C71 H71A 109.5 . . ?
C72 C71 H71A 109.5 . . ?
O70 C71 H71B 109.5 . . ?
C72 C71 H71B 109.5 . . ?
H71A C71 H71B 108.1 . . ?
F75 C72 F73 107.1(9) . . ?
F75 C72 F74 107.4(7) . . ?
F73 C72 F74 107.7(6) . . ?
F75 C72 C71 114.1(7) . . ?
F73 C72 C71 112.1(7) . . ?
F74 C72 C71 108.3(8) . . ?
C77 O76 H76 109.5 . . ?
O76 C77 C78 115.6(13) . . ?
O76 C77 H77A 108.4 . . ?
C78 C77 H77A 108.4 . . ?
O76 C77 H77B 108.4 . . ?
C78 C77 H77B 108.4 . . ?
H77A C77 H77B 107.4 . . ?
F81 C78 F79 106.5(13) . . ?
F81 C78 F80 113.8(15) . . ?
F79 C78 F80 104.2(12) . . ?
F81 C78 C77 112.0(14) . . ?
F79 C78 C77 106.8(13) . . ?
F80 C78 C77 112.8(13) . . ?
C83A C82A H82A 109.5 . . ?
C83A C82A H82B 109.5 . . ?
H82A C82A H82B 109.5 . . ?
C83A C82A H82C 109.5 . . ?
H82A C82A H82C 109.5 . . ?
H82B C82A H82C 109.5 . . ?
O85A C83A C84A 122.8(16) . . ?
O85A C83A C82A 102.2(13) . . ?
C84A C83A C82A 101.6(12) . . ?
O85A C83A H83A 109.7 . . ?
C84A C83A H83A 109.7 . . ?
C82A C83A H83A 109.7 . . ?
C83A C84A H84A 109.5 . . ?
C83A C84A H84B 109.5 . . ?
H84A C84A H84B 109.5 . . ?
C83A C84A H84C 109.5 . . ?
H84A C84A H84C 109.5 . . ?
H84B C84A H84C 109.5 . . ?
C83A O85A C86A 121.6(10) . . ?
O85A C86A C87A 107.9(11) . . ?
O85A C86A C88A 113.0(13) . . ?
C87A C86A C88A 112.6(11) . . ?
O85A C86A H86A 107.7 . . ?
C87A C86A H86A 107.7 . . ?
C88A C86A H86A 107.7 . . ?
C86A C87A H87A 109.5 . . ?
C86A C87A H87B 109.5 . . ?
H87A C87A H87B 109.5 . . ?
C86A C87A H87C 109.5 . . ?
H87A C87A H87C 109.5 . . ?
H87B C87A H87C 109.5 . . ?
C86A C88A H88A 109.5 . . ?
C86A C88A H88B 109.5 . . ?
H88A C88A H88B 109.5 . . ?
C86A C88A H88C 109.5 . . ?
H88A C88A H88C 109.5 . . ?
H88B C88A H88C 109.5 . . ?
C83B C82B H82D 109.5 . . ?
C83B C82B H82E 109.5 . . ?
H82D C82B H82E 109.5 . . ?
C83B C82B H82F 109.5 . . ?
H82D C82B H82F 109.5 . . ?
H82E C82B H82F 109.5 . . ?
O85B C83B C84B 128.4(15) . . ?
O85B C83B C82B 86.3(17) . . ?
C84B C83B C82B 105.4(14) . . ?
O85B C83B H83B 110.9 . . ?
C84B C83B H83B 110.9 . . ?
C82B C83B H83B 110.9 . . ?
C83B C84B H84D 109.5 . . ?
C83B C84B H84E 109.5 . . ?
H84D C84B H84E 109.5 . . ?
C83B C84B H84F 109.5 . . ?
H84D C84B H84F 109.5 . . ?
H84E C84B H84F 109.5 . . ?
C86B O85B C83B 112.6(10) . . ?
O85B C86B C87B 114.3(15) . . ?
O85B C86B C88B 104.6(14) . . ?
C87B C86B C88B 107.1(12) . . ?
O85B C86B H86B 110.2 . . ?
C87B C86B H86B 110.2 . . ?
C88B C86B H86B 110.2 . . ?
C86B C87B H87D 109.5 . . ?
C86B C87B H87E 109.5 . . ?
H87D C87B H87E 109.5 . . ?
C86B C87B H87F 109.5 . . ?
H87D C87B H87F 109.5 . . ?
H87E C87B H87F 109.5 . . ?
C86B C88B H88D 109.5 . . ?
C86B C88B H88E 109.5 . . ?
H88D C88B H88E 109.5 . . ?
C86B C88B H88F 109.5 . . ?
H88D C88B H88F 109.5 . . ?
H88E C88B H88F 109.5 . . ?
C90 O89 H89 109.5 . . ?
O89 C90 C91 108.8(13) . . ?
O89 C90 H90A 109.9 . . ?
C91 C90 H90A 109.9 . . ?
O89 C90 H90B 109.9 . . ?
C91 C90 H90B 109.9 . . ?
H90A C90 H90B 108.3 . . ?
F94 C91 F92 109.5(15) . . ?
F94 C91 F93 114.8(15) . . ?
F92 C91 F93 111.1(13) . . ?
F94 C91 C90 105.3(14) . . ?
F92 C91 C90 110.3(13) . . ?
F93 C91 C90 105.6(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10A H10A F56 0.88 2.02 2.886(5) 169.5 .
N19A H19A F66A 0.88 1.91 2.730(14) 155.0 .
N19A H19A F66B 0.88 2.02 2.810(9) 149.7 .
N34A H34A F51 0.88 2.03 2.847(6) 154.1 .
N43A H43A F58 0.88 1.92 2.787(5) 167.3 4_655
N10B H10B F61 0.88 1.96 2.799(5) 158.8 .
N19B H19B F52 0.88 1.95 2.768(5) 154.9 .
N34B H34B F64 0.88 1.97 2.828(5) 165.1 3_455
N43B H43B F68A 0.88 1.98 2.830(8) 162.9 2_564
N43B H43B F67B 0.88 2.57 3.281(14) 138.8 2_564
N43B H43B F68B 0.88 2.25 3.101(15) 163.5 2_564
O70 H70 F69B 0.84 2.27 2.749(15) 116.5 .
O76 H76 F54 0.84 2.14 2.824(12) 138.8 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 982129'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tdr166lt

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
Bis-[2-{5-methyl-1H-pyrazol-3-yl}-6-2-{5-tertbutyl-1H-pyrazol-3-yl}pyridine]-
iron(II) ditetrafluoroborate diethyl ether/2,2,2-trifluoroethanol 
solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C32 H38 Fe N10, 2[B F4], 2.6[C4 H10 O], 0.25[C2 H3 F3 O]]'
_chemical_formula_sum            'C42.90 H64.75 B2 F8.75 Fe N10 O2.85'
_chemical_formula_weight         1009.92

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'
Fe Fe 0.3463 0.8444 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   15.1739(5)
_cell_length_b                   17.9832(6)
_cell_length_c                   19.9978(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1170(10)
_cell_angle_gamma                90.00
_cell_volume                     5435.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    58452
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      28.23

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2119
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of 
G/ottingen, Germany.
;

_exptl_special_details           
; 
 Rotating anode power 3 kW.
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            58452
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         28.23
_reflns_number_total             13077
_reflns_number_gt                9242
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'

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

 The asymmetric unit contains: one complex dication; two disordered BF₄⁻ 
 anions; two fully occupied ordered diethyl ether molecules, one of which is
 disordered over two half-occupied sites; one complete 0.2-occupied diethyl 
 ether molecule spanning the inversion centre at 0, 0.5, 0.5; and, an 
 additional disordered region that was modelled using partial diethyl ether 
 (occupancy 0.4) and 2,2,2-trifluoroethanol (occupancy 0.25) sites.

 The disordered anions were each refined over two orientations, whose 
 occupancies each converged to a ratio of 0.66:0.34. These were modelled 
 using the refined restraints B---F = 1.38(2) and F...F = 2.25(2) Å. The 
 following fixed restraints were also applied to the disordered and partly 
 occupied solvent moieties. For diethyl ether: C---C = 1.52(2), C---O = 1.43(2), 
 1,3-C...C = 2.28(2) and 1,3-C...O = 2.34(2) Å. For 2,2,2-trifluoroethanol:
 C---C = 1.52(2), C---O = 1.43(2), C---F = 1.38(2), 1,3-C...F = F...F = 2.28(2) 
 and 1,3-C...O = 2.34(2) Å. The displacement ellipsoids on the tert-butyl C 
 atoms imply that these groups may also be disordered, but attempts to refine 
 this gave unrealistic results. Hence these groups were left as ordered in the 
 final least squares cycles.

 All non-H atoms with occupancies >0.5 were refined anisotropically, and all 
 H atoms were placed in calculated positions and refined using a riding model. 
 The highest residual Fourier peak of +1.2 e.Å⁻³ lies within the partial
 diethyl molecule close to the crystallographic inversion centre. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1572P)²+5.3495P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13077
_refine_ls_number_parameters     677
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_ref         0.2626
_refine_ls_wR_factor_gt          0.2349
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.35271(3) 0.52220(2) 0.24112(2) 0.02573(15) Uani 1 1 d . . .
N2 N 0.38251(16) 0.55871(16) 0.14510(13) 0.0306(6) Uani 1 1 d . . .
C3 C 0.3980(2) 0.6311(2) 0.13430(17) 0.0344(7) Uani 1 1 d . . .
C4 C 0.4163(2) 0.6563(2) 0.07139(19) 0.0436(9) Uani 1 1 d . . .
H4 H 0.4275 0.7075 0.0638 0.052 Uiso 1 1 calc R . .
C5 C 0.4179(3) 0.6048(3) 0.0201(2) 0.0483(10) Uani 1 1 d . . .
H5 H 0.4294 0.6210 -0.0235 0.058 Uiso 1 1 calc R . .
C6 C 0.4033(2) 0.5306(2) 0.03124(19) 0.0417(8) Uani 1 1 d . . .
H6 H 0.4053 0.4951 -0.0038 0.050 Uiso 1 1 calc R . .
C7 C 0.3854(2) 0.5089(2) 0.09561(17) 0.0337(7) Uani 1 1 d . . .
C8 C 0.3931(2) 0.6775(2) 0.19477(19) 0.0379(8) Uani 1 1 d . . .
N9 N 0.3741(2) 0.64219(16) 0.25041(15) 0.0377(6) Uani 1 1 d . . .
N10 N 0.3756(2) 0.69594(17) 0.29764(17) 0.0469(8) Uani 1 1 d . . .
H10 H 0.3648 0.6880 0.3396 0.056 Uiso 1 1 calc R . .
C11 C 0.3954(3) 0.7633(2) 0.2732(2) 0.0512(10) Uani 1 1 d . . .
C12 C 0.4062(3) 0.7536(2) 0.2068(2) 0.0470(9) Uani 1 1 d . . .
H12 H 0.4198 0.7906 0.1754 0.056 Uiso 1 1 calc R . .
C13 C 0.4017(4) 0.8313(2) 0.3175(3) 0.0713(15) Uani 1 1 d . . .
H13A H 0.4528 0.8612 0.3073 0.107 Uiso 1 1 calc R . .
H13B H 0.4088 0.8160 0.3647 0.107 Uiso 1 1 calc R . .
H13C H 0.3476 0.8609 0.3092 0.107 Uiso 1 1 calc R . .
C14 C 0.3680(2) 0.4326(2) 0.11602(17) 0.0347(7) Uani 1 1 d . . .
N15 N 0.34770(18) 0.42163(15) 0.17934(14) 0.0315(6) Uani 1 1 d . . .
N16 N 0.3357(2) 0.34750(15) 0.18490(15) 0.0373(6) Uani 1 1 d . A .
H16 H 0.3218 0.3252 0.2217 0.045 Uiso 1 1 calc R . .
C17 C 0.3479(3) 0.3116(2) 0.12650(19) 0.0454(9) Uani 1 1 d . . .
C18 C 0.3689(3) 0.3648(2) 0.08191(18) 0.0435(8) Uani 1 1 d . A .
H18 H 0.3817 0.3572 0.0367 0.052 Uiso 1 1 calc R . .
C19 C 0.3375(4) 0.2276(2) 0.1189(2) 0.0608(12) Uani 1 1 d . A 1
C20 C 0.3496(6) 0.1886(3) 0.1862(3) 0.100(2) Uani 1 1 d . A 1
H20A H 0.3442 0.1347 0.1795 0.151 Uiso 1 1 calc R A 1
H20B H 0.3042 0.2056 0.2146 0.151 Uiso 1 1 calc R A 1
H20C H 0.4084 0.2002 0.2082 0.151 Uiso 1 1 calc R A 1
C21 C 0.2475(4) 0.2118(3) 0.0812(4) 0.103(2) Uani 1 1 d . A 1
H21A H 0.2400 0.1580 0.0751 0.154 Uiso 1 1 calc R A 1
H21B H 0.2440 0.2362 0.0373 0.154 Uiso 1 1 calc R A 1
H21C H 0.2006 0.2310 0.1072 0.154 Uiso 1 1 calc R A 1
C22 C 0.4124(4) 0.1994(3) 0.0768(3) 0.0785(16) Uani 1 1 d . A 1
H22A H 0.4076 0.1453 0.0713 0.118 Uiso 1 1 calc R A 1
H22B H 0.4701 0.2118 0.1000 0.118 Uiso 1 1 calc R A 1
H22C H 0.4065 0.2232 0.0326 0.118 Uiso 1 1 calc R A 1
N23 N 0.33435(18) 0.49120(14) 0.34115(14) 0.0287(6) Uani 1 1 d . . .
C24 C 0.4039(2) 0.47328(18) 0.38386(17) 0.0331(7) Uani 1 1 d . . .
C25 C 0.3941(3) 0.4567(2) 0.45069(19) 0.0459(9) Uani 1 1 d . . .
H25 H 0.4435 0.4424 0.4805 0.055 Uiso 1 1 calc R . .
C26 C 0.3104(3) 0.4615(2) 0.4726(2) 0.0497(10) Uani 1 1 d . . .
H26 H 0.3023 0.4520 0.5183 0.060 Uiso 1 1 calc R . .
C27 C 0.2389(3) 0.4800(2) 0.42865(19) 0.0437(9) Uani 1 1 d . . .
H27 H 0.1812 0.4825 0.4434 0.052 Uiso 1 1 calc R . .
C28 C 0.2528(2) 0.49459(19) 0.36290(18) 0.0332(7) Uani 1 1 d . . .
C29 C 0.4882(2) 0.47523(18) 0.35282(17) 0.0334(7) Uani 1 1 d . . .
N30 N 0.48460(17) 0.49875(15) 0.28942(14) 0.0300(6) Uani 1 1 d . . .
N31 N 0.56864(18) 0.49677(17) 0.27291(16) 0.0351(6) Uani 1 1 d . . .
H31 H 0.5851 0.5101 0.2336 0.041(11) Uiso 1 1 calc R . .
C32 C 0.6250(2) 0.4714(2) 0.3248(2) 0.0410(8) Uani 1 1 d . . .
C33 C 0.5746(2) 0.4570(2) 0.37689(19) 0.0418(8) Uani 1 1 d . . .
H33 H 0.5943 0.4384 0.4201 0.050 Uiso 1 1 calc R . .
C34 C 0.7221(3) 0.4632(3) 0.3194(3) 0.0614(12) Uani 1 1 d . . .
H34A H 0.7399 0.4118 0.3295 0.092 Uiso 1 1 calc R . .
H34B H 0.7546 0.4968 0.3514 0.092 Uiso 1 1 calc R . .
H34C H 0.7355 0.4757 0.2737 0.092 Uiso 1 1 calc R . .
C35 C 0.1842(2) 0.51550(19) 0.30969(18) 0.0352(7) Uani 1 1 d . . .
N36 N 0.20983(18) 0.52749(16) 0.24824(15) 0.0335(6) Uani 1 1 d . . .
N37 N 0.13384(19) 0.54487(18) 0.20991(17) 0.0403(7) Uani 1 1 d . B .
H37 H 0.1315 0.5558 0.1669 0.048 Uiso 1 1 calc R . .
C38 C 0.0623(2) 0.5433(2) 0.2459(2) 0.0448(9) Uani 1 1 d . . .
C39 C 0.0928(2) 0.5241(2) 0.3103(2) 0.0444(9) Uani 1 1 d . B .
H39 H 0.0588 0.5180 0.3476 0.053 Uiso 1 1 calc R . .
C40 C -0.0319(3) 0.5567(3) 0.2166(3) 0.0570(11) Uani 1 1 d . B 1
C41 C -0.0353(3) 0.6037(3) 0.1532(3) 0.0685(14) Uani 1 1 d . B 1
H41A H -0.0093 0.6526 0.1640 0.103 Uiso 1 1 calc R B 1
H41B H -0.0970 0.6098 0.1350 0.103 Uiso 1 1 calc R B 1
H41C H -0.0018 0.5789 0.1199 0.103 Uiso 1 1 calc R B 1
C42 C -0.0748(3) 0.4807(3) 0.2001(4) 0.0816(19) Uani 1 1 d . B 1
H42A H -0.0416 0.4547 0.1673 0.122 Uiso 1 1 calc R B 1
H42B H -0.1361 0.4880 0.1812 0.122 Uiso 1 1 calc R B 1
H42C H -0.0742 0.4509 0.2412 0.122 Uiso 1 1 calc R B 1
C43 C -0.0831(3) 0.5972(4) 0.2687(3) 0.0780(16) Uani 1 1 d . B 1
H43A H -0.0819 0.5672 0.3097 0.117 Uiso 1 1 calc R B 1
H43B H -0.1446 0.6046 0.2504 0.117 Uiso 1 1 calc R B 1
H43C H -0.0555 0.6455 0.2792 0.117 Uiso 1 1 calc R B 1
B44A B 0.3320(9) 0.6761(5) 0.4765(5) 0.079(7) Uani 0.66 1 d PD C 1
F45A F 0.3325(6) 0.6377(2) 0.4171(2) 0.103(3) Uani 0.66 1 d PD C 1
F46A F 0.3083(4) 0.7510(2) 0.4590(3) 0.0702(14) Uani 0.66 1 d PD C 1
F47A F 0.4136(3) 0.6727(2) 0.5133(2) 0.0714(12) Uani 0.66 1 d PD C 1
F48A F 0.2722(3) 0.6470(3) 0.5156(3) 0.0833(14) Uani 0.66 1 d PD C 1
B44B B 0.3229(12) 0.6784(11) 0.4677(9) 0.073(10) Uiso 0.34 1 d PD D 2
F45B F 0.3711(10) 0.6281(8) 0.4338(7) 0.106(6) Uiso 0.34 1 d PD D 2
F46B F 0.3470(9) 0.7479(7) 0.4452(7) 0.093(5) Uiso 0.34 1 d PD D 2
F47B F 0.3421(10) 0.6738(7) 0.5356(6) 0.114(4) Uiso 0.34 1 d PD D 2
F48B F 0.2351(9) 0.6580(9) 0.4566(9) 0.157(6) Uiso 0.34 1 d PD D 2
B49A B 0.6750(5) 0.5521(6) 0.1299(3) 0.043(2) Uani 0.66 1 d PD E 1
F50A F 0.5871(3) 0.5331(4) 0.1387(3) 0.072(2) Uani 0.66 1 d PD E 1
F51A F 0.7223(3) 0.4865(3) 0.1177(2) 0.0640(11) Uani 0.66 1 d PD E 1
F52A F 0.6793(3) 0.5983(2) 0.07696(18) 0.0616(11) Uani 0.66 1 d PD E 1
F53A F 0.7138(3) 0.5824(3) 0.1893(2) 0.0630(13) Uani 0.66 1 d PD E 1
B49B B 0.6641(12) 0.5675(11) 0.1303(9) 0.088(12) Uiso 0.34 1 d PD F 2
F50B F 0.6012(7) 0.5139(5) 0.1381(6) 0.042(3) Uiso 0.34 1 d PD F 2
F51B F 0.7363(8) 0.5378(8) 0.1030(7) 0.113(4) Uiso 0.34 1 d PD F 2
F52B F 0.6291(7) 0.6191(5) 0.0843(5) 0.074(3) Uiso 0.34 1 d PD F 2
F53B F 0.6877(7) 0.6016(6) 0.1913(6) 0.069(4) Uiso 0.34 1 d PD F 2
C54 C 0.3880(4) 0.2723(4) 0.3621(3) 0.0787(17) Uani 1 1 d . . .
H54A H 0.4004 0.2331 0.3302 0.118 Uiso 1 1 calc R . .
H54B H 0.4151 0.2593 0.4069 0.118 Uiso 1 1 calc R . .
H54C H 0.4125 0.3195 0.3477 0.118 Uiso 1 1 calc R . .
C55 C 0.2902(4) 0.2798(3) 0.3642(3) 0.0684(14) Uani 1 1 d . . .
H55A H 0.2645 0.2310 0.3746 0.082 Uiso 1 1 calc R . .
H55B H 0.2775 0.3152 0.4000 0.082 Uiso 1 1 calc R . .
O56 O 0.25151(18) 0.30546(15) 0.30202(14) 0.0479(6) Uani 1 1 d . . .
C57 C 0.1566(3) 0.3101(3) 0.2999(3) 0.0602(12) Uani 1 1 d . . .
H57A H 0.1397 0.3456 0.3343 0.072 Uiso 1 1 calc R . .
H57B H 0.1319 0.2607 0.3098 0.072 Uiso 1 1 calc R . .
C58 C 0.1202(3) 0.3353(3) 0.2319(3) 0.0688(13) Uani 1 1 d . . .
H58A H 0.1452 0.3839 0.2222 0.103 Uiso 1 1 calc R . .
H58B H 0.0556 0.3393 0.2307 0.103 Uiso 1 1 calc R . .
H58C H 0.1357 0.2992 0.1982 0.103 Uiso 1 1 calc R . .
C59A C 0.1303(9) 0.4371(6) 0.0542(7) 0.072(3) Uiso 0.50 1 d PD G 1
H59A H 0.1242 0.4001 0.0181 0.107 Uiso 0.50 1 calc PR G 1
H59B H 0.0760 0.4382 0.0774 0.107 Uiso 0.50 1 calc PR G 1
H59C H 0.1806 0.4240 0.0862 0.107 Uiso 0.50 1 calc PR G 1
C60A C 0.1456(7) 0.5122(5) 0.0249(5) 0.057(2) Uiso 0.50 1 d PD G 1
H60A H 0.1996 0.5104 0.0006 0.068 Uiso 0.50 1 calc PR G 1
H60B H 0.0951 0.5246 -0.0081 0.068 Uiso 0.50 1 calc PR G 1
O61A O 0.1552(4) 0.5695(4) 0.0742(3) 0.0514(17) Uiso 0.50 1 d PD G 1
C62A C 0.1695(6) 0.6393(5) 0.0453(5) 0.051(2) Uiso 0.50 1 d PD G 1
H62A H 0.1195 0.6516 0.0119 0.062 Uiso 0.50 1 calc PR G 1
H62B H 0.2244 0.6381 0.0221 0.062 Uiso 0.50 1 calc PR G 1
C63A C 0.1776(8) 0.7001(6) 0.1022(7) 0.077(3) Uiso 0.50 1 d PD G 1
H63A H 0.1885 0.7487 0.0824 0.116 Uiso 0.50 1 calc PR G 1
H63B H 0.2269 0.6875 0.1353 0.116 Uiso 0.50 1 calc PR G 1
H63C H 0.1225 0.7019 0.1243 0.116 Uiso 0.50 1 calc PR G 1
C59B C 0.1247(9) 0.4139(7) 0.0661(7) 0.073(3) Uiso 0.50 1 d PD H 2
H59D H 0.1198 0.3690 0.0382 0.109 Uiso 0.50 1 calc PR H 2
H59E H 0.0689 0.4222 0.0861 0.109 Uiso 0.50 1 calc PR H 2
H59F H 0.1728 0.4077 0.1018 0.109 Uiso 0.50 1 calc PR H 2
C60B C 0.1443(7) 0.4799(5) 0.0231(5) 0.055(2) Uiso 0.50 1 d PD H 2
H60C H 0.2006 0.4723 0.0027 0.065 Uiso 0.50 1 calc PR H 2
H60D H 0.0963 0.4867 -0.0133 0.065 Uiso 0.50 1 calc PR H 2
O61B O 0.1503(4) 0.5430(4) 0.0654(3) 0.0432(14) Uiso 0.50 1 d PD H 2
C62B C 0.1685(7) 0.6086(6) 0.0297(5) 0.064(3) Uiso 0.50 1 d PD H 2
H62C H 0.1227 0.6145 -0.0084 0.077 Uiso 0.50 1 calc PR H 2
H62D H 0.2263 0.6028 0.0108 0.077 Uiso 0.50 1 calc PR H 2
C63B C 0.1710(8) 0.6769(7) 0.0709(7) 0.073(3) Uiso 0.50 1 d PD H 2
H63D H 0.1856 0.7195 0.0434 0.109 Uiso 0.50 1 calc PR H 2
H63E H 0.2160 0.6716 0.1089 0.109 Uiso 0.50 1 calc PR H 2
H63F H 0.1130 0.6848 0.0877 0.109 Uiso 0.50 1 calc PR H 2
C68A C 0.0791(12) 0.7358(10) 0.3836(7) 0.084(5) Uiso 0.40 1 d PD I 1
H68A H 0.1119 0.7189 0.4252 0.127 Uiso 0.40 1 calc PR I 1
H68B H 0.0315 0.7006 0.3704 0.127 Uiso 0.40 1 calc PR I 1
H68C H 0.0538 0.7850 0.3906 0.127 Uiso 0.40 1 calc PR I 1
O66A O 0.0936(9) 0.7647(7) 0.2712(5) 0.080(3) Uiso 0.40 1 d PD I 1
C67A C 0.1414(8) 0.7405(8) 0.3284(6) 0.066(3) Uiso 0.40 1 d PD I 1
H67A H 0.1903 0.7756 0.3414 0.079 Uiso 0.40 1 calc PR I 1
H67B H 0.1673 0.6910 0.3207 0.079 Uiso 0.40 1 calc PR I 1
C65A C 0.1473(10) 0.7772(10) 0.2194(6) 0.088(4) Uiso 0.40 1 d PD I 1
H65A H 0.1729 0.7293 0.2062 0.106 Uiso 0.40 1 calc PR I 1
H65B H 0.1967 0.8103 0.2357 0.106 Uiso 0.40 1 calc PR I 1
C64A C 0.0974(12) 0.8117(11) 0.1591(7) 0.106(6) Uiso 0.40 1 d PD I 1
H64A H 0.1377 0.8200 0.1242 0.159 Uiso 0.40 1 calc PR I 1
H64B H 0.0723 0.8593 0.1719 0.159 Uiso 0.40 1 calc PR I 1
H64C H 0.0495 0.7783 0.1420 0.159 Uiso 0.40 1 calc PR I 1
O64B O 0.116(2) 0.7434(18) 0.4018(11) 0.165(13) Uiso 0.25 1 d PD J 2
H64D H 0.1569 0.7301 0.4302 0.198 Uiso 0.25 1 calc PR J 2
C65B C 0.1479(13) 0.7957(9) 0.3584(6) 0.069(5) Uiso 0.25 1 d PD J 2
H65C H 0.2083 0.8111 0.3758 0.083 Uiso 0.25 1 calc PR J 2
H65D H 0.1095 0.8403 0.3566 0.083 Uiso 0.25 1 calc PR J 2
C66B C 0.1500(8) 0.7655(7) 0.2920(6) 0.038(3) Uiso 0.25 1 d PD J 2
F67B F 0.1924(6) 0.7016(5) 0.2891(5) 0.055(2) Uiso 0.25 1 d PD J 2
F68B F 0.0667(8) 0.7567(9) 0.2596(8) 0.092(6) Uiso 0.25 1 d PD J 2
F69B F 0.1892(7) 0.8176(5) 0.2534(5) 0.060(3) Uiso 0.25 1 d PD J 2
C70 C -0.009(2) 0.3634(12) 0.4473(16) 0.089(9) Uiso 0.20 1 d PD . .
H70A H -0.0475 0.3212 0.4550 0.133 Uiso 0.20 1 calc PR . .
H70B H 0.0514 0.3525 0.4668 0.133 Uiso 0.20 1 calc PR . .
H70C H -0.0082 0.3717 0.3989 0.133 Uiso 0.20 1 calc PR . .
C71 C -0.043(2) 0.4330(13) 0.4802(19) 0.102(11) Uiso 0.20 1 d PD . .
H71A H -0.1034 0.4452 0.4599 0.122 Uiso 0.20 1 calc PR . .
H71B H -0.0462 0.4244 0.5289 0.122 Uiso 0.20 1 calc PR . .
O72 O 0.0143(16) 0.4914(10) 0.4703(13) 0.106(7) Uiso 0.20 1 d PD . .
C73 C -0.013(2) 0.5613(12) 0.4972(19) 0.103(11) Uiso 0.20 1 d PD . .
H73A H -0.0141 0.5584 0.5465 0.124 Uiso 0.20 1 calc PR . .
H73B H -0.0718 0.5761 0.4767 0.124 Uiso 0.20 1 calc PR . .
C74 C 0.0571(19) 0.6149(12) 0.4786(16) 0.083(8) Uiso 0.20 1 d PD . .
H74A H 0.0433 0.6649 0.4944 0.124 Uiso 0.20 1 calc PR . .
H74B H 0.0586 0.6156 0.4298 0.124 Uiso 0.20 1 calc PR . .
H74C H 0.1149 0.5993 0.4997 0.124 Uiso 0.20 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.116(3) . ?
Fe1 N23 2.119(3) . ?
Fe1 N30 2.184(3) . ?
Fe1 N36 2.187(3) . ?
Fe1 N9 2.187(3) . ?
Fe1 N15 2.188(3) . ?
N2 C7 1.339(5) . ?
N2 C3 1.344(4) . ?
C3 C4 1.388(5) . ?
C3 C8 1.477(5) . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(5) . ?
C6 H6 0.9500 . ?
C7 C14 1.461(5) . ?
C8 N9 1.335(4) . ?
C8 C12 1.400(5) . ?
N9 N10 1.350(4) . ?
N10 C11 1.351(5) . ?
N10 H10 0.8800 . ?
C11 C12 1.364(6) . ?
C11 C13 1.507(6) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 N15 1.345(4) . ?
C14 C18 1.399(5) . ?
N15 N16 1.351(4) . ?
N16 C17 1.362(5) . ?
N16 H16 0.8800 . ?
C17 C18 1.365(6) . ?
C17 C19 1.525(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.514(8) . ?
C19 C21 1.526(8) . ?
C19 C22 1.559(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N23 C24 1.336(4) . ?
N23 C28 1.349(4) . ?
C24 C25 1.390(5) . ?
C24 C29 1.472(5) . ?
C25 C26 1.382(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.374(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.376(5) . ?
C27 H27 0.9500 . ?
C28 C35 1.469(5) . ?
C29 N30 1.333(4) . ?
C29 C33 1.395(5) . ?
N30 N31 1.346(4) . ?
N31 C32 1.363(5) . ?
N31 H31 0.8800 . ?
C32 C33 1.370(6) . ?
C32 C34 1.495(6) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N36 1.339(5) . ?
C35 C39 1.397(5) . ?
N36 N37 1.363(4) . ?
N37 C38 1.356(5) . ?
N37 H37 0.8800 . ?
C38 C39 1.374(6) . ?
C38 C40 1.515(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.520(7) . ?
C40 C42 1.536(7) . ?
C40 C43 1.538(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
B44A F48A 1.355(11) . ?
B44A F45A 1.376(9) . ?
B44A F47A 1.384(12) . ?
B44A F46A 1.430(9) . ?
B44B F47B 1.366(17) . ?
B44B F45B 1.379(17) . ?
B44B F48B 1.381(16) . ?
B44B F46B 1.388(16) . ?
B49A F52A 1.352(9) . ?
B49A F53A 1.388(7) . ?
B49A F50A 1.403(7) . ?
B49A F51A 1.414(12) . ?
B49B F51B 1.375(17) . ?
B49B F50B 1.376(17) . ?
B49B F52B 1.379(17) . ?
B49B F53B 1.382(17) . ?
C54 C55 1.494(8) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 O56 1.404(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
O56 C57 1.439(5) . ?
C57 C58 1.492(7) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59A C60A 1.498(13) . ?
C59A H59A 0.9800 . ?
C59A H59B 0.9800 . ?
C59A H59C 0.9800 . ?
C60A O61A 1.424(11) . ?
C60A H60A 0.9900 . ?
C60A H60B 0.9900 . ?
O61A C62A 1.407(10) . ?
C62A C63A 1.574(12) . ?
C62A H62A 0.9900 . ?
C62A H62B 0.9900 . ?
C63A H63A 0.9800 . ?
C63A H63B 0.9800 . ?
C63A H63C 0.9800 . ?
C59B C60B 1.510(13) . ?
C59B H59D 0.9800 . ?
C59B H59E 0.9800 . ?
C59B H59F 0.9800 . ?
C60B O61B 1.412(10) . ?
C60B H60C 0.9900 . ?
C60B H60D 0.9900 . ?
O61B C62B 1.420(10) . ?
C62B C63B 1.477(13) . ?
C62B H62C 0.9900 . ?
C62B H62D 0.9900 . ?
C63B H63D 0.9800 . ?
C63B H63E 0.9800 . ?
C63B H63F 0.9800 . ?
C68A C67A 1.518(14) . ?
C68A H68A 0.9800 . ?
C68A H68B 0.9800 . ?
C68A H68C 0.9800 . ?
O66A C67A 1.370(13) . ?
O66A C65A 1.392(14) . ?
C67A H67A 0.9900 . ?
C67A H67B 0.9900 . ?
C65A C64A 1.499(15) . ?
C65A H65A 0.9900 . ?
C65A H65B 0.9900 . ?
C64A H64A 0.9800 . ?
C64A H64B 0.9800 . ?
C64A H64C 0.9800 . ?
O64B C65B 1.396(17) . ?
O64B H64D 0.8400 . ?
C65B C66B 1.438(14) . ?
C65B H65C 0.9900 . ?
C65B H65D 0.9900 . ?
C66B F67B 1.321(13) . ?
C66B F68B 1.378(14) . ?
C66B F69B 1.381(13) . ?
C70 C71 1.529(18) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 O72 1.391(18) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
O72 C73 1.440(18) . ?
C73 C74 1.503(18) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N23 174.33(10) . . ?
N2 Fe1 N30 101.51(10) . . ?
N23 Fe1 N30 73.99(10) . . ?
N2 Fe1 N36 109.81(10) . . ?
N23 Fe1 N36 74.66(11) . . ?
N30 Fe1 N36 148.65(11) . . ?
N2 Fe1 N9 74.27(11) . . ?
N23 Fe1 N9 102.14(10) . . ?
N30 Fe1 N9 91.71(11) . . ?
N36 Fe1 N9 95.28(11) . . ?
N2 Fe1 N15 75.14(11) . . ?
N23 Fe1 N15 108.35(10) . . ?
N30 Fe1 N15 94.26(10) . . ?
N36 Fe1 N15 95.05(11) . . ?
N9 Fe1 N15 149.41(11) . . ?
C7 N2 C3 120.8(3) . . ?
C7 N2 Fe1 119.1(2) . . ?
C3 N2 Fe1 120.1(2) . . ?
N2 C3 C4 120.9(3) . . ?
N2 C3 C8 113.2(3) . . ?
C4 C3 C8 125.9(3) . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 118.0(4) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 H6 121.0 . . ?
N2 C7 C6 121.1(3) . . ?
N2 C7 C14 113.8(3) . . ?
C6 C7 C14 125.1(3) . . ?
N9 C8 C12 111.1(3) . . ?
N9 C8 C3 116.4(3) . . ?
C12 C8 C3 132.5(3) . . ?
C8 N9 N10 104.5(3) . . ?
C8 N9 Fe1 116.1(2) . . ?
N10 N9 Fe1 139.3(2) . . ?
N9 N10 C11 112.3(3) . . ?
N9 N10 H10 123.8 . . ?
C11 N10 H10 123.8 . . ?
N10 C11 C12 106.7(3) . . ?
N10 C11 C13 121.3(4) . . ?
C12 C11 C13 132.0(4) . . ?
C11 C12 C8 105.4(3) . . ?
C11 C12 H12 127.3 . . ?
C8 C12 H12 127.3 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N15 C14 C18 110.1(3) . . ?
N15 C14 C7 117.6(3) . . ?
C18 C14 C7 132.3(3) . . ?
C14 N15 N16 105.5(3) . . ?
C14 N15 Fe1 114.3(2) . . ?
N16 N15 Fe1 140.1(2) . . ?
N15 N16 C17 111.6(3) . . ?
N15 N16 H16 124.2 . . ?
C17 N16 H16 124.2 . . ?
N16 C17 C18 106.5(3) . . ?
N16 C17 C19 122.3(4) . . ?
C18 C17 C19 131.2(4) . . ?
C17 C18 C14 106.3(3) . . ?
C17 C18 H18 126.9 . . ?
C14 C18 H18 126.9 . . ?
C20 C19 C17 111.5(4) . . ?
C20 C19 C21 112.7(6) . . ?
C17 C19 C21 108.3(4) . . ?
C20 C19 C22 107.0(5) . . ?
C17 C19 C22 107.5(4) . . ?
C21 C19 C22 109.6(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 N23 C28 120.0(3) . . ?
C24 N23 Fe1 120.3(2) . . ?
C28 N23 Fe1 119.6(2) . . ?
N23 C24 C25 121.4(3) . . ?
N23 C24 C29 113.0(3) . . ?
C25 C24 C29 125.6(3) . . ?
C26 C25 C24 118.1(4) . . ?
C26 C25 H25 121.0 . . ?
C24 C25 H25 121.0 . . ?
C27 C26 C25 120.6(4) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 118.5(4) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 H27 120.7 . . ?
N23 C28 C27 121.5(3) . . ?
N23 C28 C35 112.9(3) . . ?
C27 C28 C35 125.6(3) . . ?
N30 C29 C33 111.2(3) . . ?
N30 C29 C24 116.4(3) . . ?
C33 C29 C24 132.4(3) . . ?
C29 N30 N31 105.4(3) . . ?
C29 N30 Fe1 116.1(2) . . ?
N31 N30 Fe1 138.4(2) . . ?
N30 N31 C32 111.5(3) . . ?
N30 N31 H31 124.3 . . ?
C32 N31 H31 124.3 . . ?
N31 C32 C33 106.7(3) . . ?
N31 C32 C34 122.2(4) . . ?
C33 C32 C34 131.0(4) . . ?
C32 C33 C29 105.3(3) . . ?
C32 C33 H33 127.4 . . ?
C29 C33 H33 127.4 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N36 C35 C39 111.1(3) . . ?
N36 C35 C28 117.5(3) . . ?
C39 C35 C28 131.4(3) . . ?
C35 N36 N37 104.7(3) . . ?
C35 N36 Fe1 115.0(2) . . ?
N37 N36 Fe1 140.1(2) . . ?
C38 N37 N36 112.0(3) . . ?
C38 N37 H37 124.0 . . ?
N36 N37 H37 124.0 . . ?
N37 C38 C39 106.5(3) . . ?
N37 C38 C40 124.3(4) . . ?
C39 C38 C40 129.1(4) . . ?
C38 C39 C35 105.8(3) . . ?
C38 C39 H39 127.1 . . ?
C35 C39 H39 127.1 . . ?
C38 C40 C41 111.8(3) . . ?
C38 C40 C42 108.1(4) . . ?
C41 C40 C42 109.5(5) . . ?
C38 C40 C43 109.2(4) . . ?
C41 C40 C43 108.6(4) . . ?
C42 C40 C43 109.7(4) . . ?
F48A B44A F45A 111.0(8) . . ?
F48A B44A F47A 106.8(7) . . ?
F45A B44A F47A 111.4(9) . . ?
F48A B44A F46A 109.8(8) . . ?
F45A B44A F46A 106.4(7) . . ?
F47A B44A F46A 111.4(7) . . ?
F47B B44B F45B 111.9(15) . . ?
F47B B44B F48B 105.0(13) . . ?
F45B B44B F48B 107.0(14) . . ?
F47B B44B F46B 109.9(14) . . ?
F45B B44B F46B 105.3(13) . . ?
F48B B44B F46B 117.7(15) . . ?
F52A B49A F53A 112.5(7) . . ?
F52A B49A F50A 111.1(7) . . ?
F53A B49A F50A 109.0(5) . . ?
F52A B49A F51A 108.5(5) . . ?
F53A B49A F51A 107.0(7) . . ?
F50A B49A F51A 108.7(7) . . ?
F51B B49B F50B 110.9(14) . . ?
F51B B49B F52B 105.7(14) . . ?
F50B B49B F52B 108.5(14) . . ?
F51B B49B F53B 111.7(14) . . ?
F50B B49B F53B 109.8(14) . . ?
F52B B49B F53B 110.2(14) . . ?
C55 C54 H54A 109.5 . . ?
C55 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C55 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O56 C55 C54 110.0(4) . . ?
O56 C55 H55A 109.7 . . ?
C54 C55 H55A 109.7 . . ?
O56 C55 H55B 109.7 . . ?
C54 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C55 O56 C57 112.5(4) . . ?
O56 C57 C58 109.5(4) . . ?
O56 C57 H57A 109.8 . . ?
C58 C57 H57A 109.8 . . ?
O56 C57 H57B 109.8 . . ?
C58 C57 H57B 109.8 . . ?
H57A C57 H57B 108.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60A C59A H59A 109.5 . . ?
C60A C59A H59B 109.5 . . ?
H59A C59A H59B 109.5 . . ?
C60A C59A H59C 109.5 . . ?
H59A C59A H59C 109.5 . . ?
H59B C59A H59C 109.5 . . ?
O61A C60A C59A 113.0(9) . . ?
O61A C60A H60A 109.0 . . ?
C59A C60A H60A 109.0 . . ?
O61A C60A H60B 109.0 . . ?
C59A C60A H60B 109.0 . . ?
H60A C60A H60B 107.8 . . ?
C62A O61A C60A 111.8(7) . . ?
O61A C62A C63A 109.2(7) . . ?
O61A C62A H62A 109.8 . . ?
C63A C62A H62A 109.8 . . ?
O61A C62A H62B 109.8 . . ?
C63A C62A H62B 109.8 . . ?
H62A C62A H62B 108.3 . . ?
C62A C63A H63A 109.5 . . ?
C62A C63A H63B 109.5 . . ?
H63A C63A H63B 109.5 . . ?
C62A C63A H63C 109.5 . . ?
H63A C63A H63C 109.5 . . ?
H63B C63A H63C 109.5 . . ?
C60B C59B H59D 109.5 . . ?
C60B C59B H59E 109.5 . . ?
H59D C59B H59E 109.5 . . ?
C60B C59B H59F 109.5 . . ?
H59D C59B H59F 109.5 . . ?
H59E C59B H59F 109.5 . . ?
O61B C60B C59B 107.2(9) . . ?
O61B C60B H60C 110.3 . . ?
C59B C60B H60C 110.3 . . ?
O61B C60B H60D 110.3 . . ?
C59B C60B H60D 110.3 . . ?
H60C C60B H60D 108.5 . . ?
C60B O61B C62B 111.8(7) . . ?
O61B C62B C63B 114.0(9) . . ?
O61B C62B H62C 108.8 . . ?
C63B C62B H62C 108.8 . . ?
O61B C62B H62D 108.8 . . ?
C63B C62B H62D 108.8 . . ?
H62C C62B H62D 107.7 . . ?
C62B C63B H63D 109.5 . . ?
C62B C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C62B C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
C67A C68A H68A 109.5 . . ?
C67A C68A H68B 109.5 . . ?
H68A C68A H68B 109.5 . . ?
C67A C68A H68C 109.5 . . ?
H68A C68A H68C 109.5 . . ?
H68B C68A H68C 109.5 . . ?
C67A O66A C65A 111.8(11) . . ?
O66A C67A C68A 107.8(11) . . ?
O66A C67A H67A 110.1 . . ?
C68A C67A H67A 110.1 . . ?
O66A C67A H67B 110.1 . . ?
C68A C67A H67B 110.1 . . ?
H67A C67A H67B 108.5 . . ?
O66A C65A C64A 112.2(12) . . ?
O66A C65A H65A 109.2 . . ?
C64A C65A H65A 109.2 . . ?
O66A C65A H65B 109.2 . . ?
C64A C65A H65B 109.2 . . ?
H65A C65A H65B 107.9 . . ?
C65A C64A H64A 109.5 . . ?
C65A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C65A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
C65B O64B H64D 109.5 . . ?
O64B C65B C66B 111.0(15) . . ?
O64B C65B H65C 109.4 . . ?
C66B C65B H65C 109.4 . . ?
O64B C65B H65D 109.4 . . ?
C66B C65B H65D 109.4 . . ?
H65C C65B H65D 108.0 . . ?
F67B C66B F68B 108.0(11) . . ?
F67B C66B F69B 109.3(10) . . ?
F68B C66B F69B 103.8(11) . . ?
F67B C66B C65B 114.8(11) . . ?
F68B C66B C65B 112.4(12) . . ?
F69B C66B C65B 107.9(11) . . ?
C71 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C71 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
O72 C71 C70 108.3(17) . . ?
O72 C71 H71A 110.0 . . ?
C70 C71 H71A 110.0 . . ?
O72 C71 H71B 110.0 . . ?
C70 C71 H71B 110.0 . . ?
H71A C71 H71B 108.4 . . ?
C71 O72 C73 113.8(16) . . ?
O72 C73 C74 103.8(16) . . ?
O72 C73 H73A 111.0 . . ?
C74 C73 H73A 111.0 . . ?
O72 C73 H73B 111.0 . . ?
C74 C73 H73B 111.0 . . ?
H73A C73 H73B 109.0 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 F45A 0.88 1.90 2.740(6) 160.0 .
N10 H10 F45B 0.88 2.16 2.990(16) 155.9 .
N16 H16 O56 0.88 2.04 2.868(4) 157.0 .
N31 H31 F50A 0.88 1.95 2.801(7) 163.9 .
N31 H31 F50B 0.88 1.95 2.800(13) 163.0 .
N37 H37 O61A 0.88 1.94 2.797(7) 165.9 .
N37 H37 O61B 0.88 2.09 2.923(7) 158.2 .
O64B H64D F46A 0.84 2.35 3.04(3) 140.5 .
O64B H64D F48B 0.84 1.80 2.55(4) 146.3 .

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        28.23
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.150
_database_code_depnum_ccdc_archive 'CCDC 982130'
