 data_global

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

# 1. SUBMISSION DETAILS
_publ_contact_author             'Prof. Malcolm A. Halcrow'
_publ_contact_address
;
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
_publ_contact_author_phone       '+44 (0)113 3436506'
_publ_contact_author_fax         '+44 (0)113 3436565'
_publ_contact_author_email       m.a.halcrow@@leeds.ac.uk
_publ_requested_journal          'Chemical Communications'
_publ_contact_letter
;
   The following data are for the three structures associated with this 
   paper, that have been pre-deposited with the CCDC.
;

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

# 2. TITLE AND AUTHOR LIST
_publ_section_title
;
Isostructural Salts of the Same Complex Showing Contrasting Thermal Spin-Crossover 
Mediated by Multiple Phase Changes
;

loop_
_publ_author_name
_publ_author_address
   'Thomas D. Roberts'
;      
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
   'Marc A. Little'
;      
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
   'Floriana Tuna'
;      
   School of Chemistry, 
   University of Manchester,
   Oxford Road,
   Manchester M13 9PL,
   UK
;
   'Colin A. Kilner'
;      
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
   'Malcolm A. Halcrow'
;      
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;

#=================================================================
   
 
data_tr11 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]iron(II) 
diperchlorate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C26 H26 Fe N10, 2[Cl O4]'  
_chemical_formula_sum             'C26 H26 Cl2 Fe N10 O8' 
_chemical_formula_weight          733.32 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 
_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M    'P 42/n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x+1/2, z+1/2' 
 '-x+1/2, -y+1/2, z' 
 'y+1/2, -x, z+1/2' 
 '-x, -y, -z' 
 'y, -x-1/2, -z-1/2' 
 'x-1/2, y-1/2, -z' 
 '-y-1/2, x, -z-1/2' 
 
_cell_length_a                    9.7396(3) 
_cell_length_b                    9.7396(3) 
_cell_length_c                    18.0080(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1708.24(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     28726 
_cell_measurement_theta_min       2.26 
_cell_measurement_theta_max       28.38  
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.29 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.426 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              752 
_exptl_absorpt_coefficient_mu     0.658 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.570 
_exptl_absorpt_correction_T_max   0.995 
_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             28726 
_diffrn_reflns_av_R_equivalents   0.0521 
_diffrn_reflns_av_sigmaI/netI     0.0229 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          2.26 
_diffrn_reflns_theta_max          28.38 
_reflns_number_total              2138 
_reflns_number_gt                 1642 
_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 1/4 of a complex dication, with Fe1 occupying 
 the crystallographic S4 site [1/4, 1/4, 1/4] and N2 and C5 lying on the C2 
 axis [1/4, 1/4, z]; and, half a ClO₄⁻ anion that is disordered about 
 the C₂ axis [3/4, 1/4, z]. Three partial environments for this disordered 
 half-anion Cl12-O16 were refined, labelled 'A' (occupancy 0.2), 'B' (0.20) 
 and 'C' (0.10), which shared a common half-occupied Cl atom Cl12. These 
 were subject to the fixed restraints Cl---O = 1.45(2)Å. No angular 
 restraints were applied to these fragments, and the the resultant partial 
 anions are a long way from being tetrahedral. 

 All wholly occupied non-H atoms were refined anisotropically, 
 and all 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)+(0.2000P)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          2138 
_refine_ls_number_parameters      142 
_refine_ls_number_restraints      12 
_refine_ls_R_factor_all           0.1112 
_refine_ls_R_factor_gt            0.0939 
_refine_ls_wR_factor_ref          0.3483 
_refine_ls_wR_factor_gt           0.3195 
_refine_ls_goodness_of_fit_ref    1.532 
_refine_ls_restrained_S_all       1.589 
_refine_ls_shift/su_max           0.009 
_refine_ls_shift/su_mean          0.001 
 
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 0.2500 0.2500 0.2500 0.0428(5) Uani 1 4 d S . . 
N2 N 0.2500 0.2500 0.1372(4) 0.0672(17) Uani 1 2 d S . . 
C3 C 0.3586(5) 0.2973(7) 0.0996(3) 0.0844(15) Uani 1 1 d . . . 
C4 C 0.3596(10) 0.2998(14) 0.0190(4) 0.149(4) Uani 1 1 d . . . 
H4 H 0.4362 0.3359 -0.0071 0.179 Uiso 1 1 calc R . . 
C5 C 0.2500 0.2500 -0.0186(8) 0.183(12) Uani 1 2 d S . . 
H5 H 0.2500 0.2500 -0.0713 0.219 Uiso 1 2 calc SR . . 
C6 C 0.4704(5) 0.3407(5) 0.1489(4) 0.0778(14) Uani 1 1 d . . . 
N7 N 0.4425(3) 0.3297(3) 0.2211(3) 0.0632(10) Uani 1 1 d . . . 
N8 N 0.5564(6) 0.3750(5) 0.2546(3) 0.0799(17) Uani 1 1 d . . . 
H8 H 0.5688 0.3800 0.3029 0.096 Uiso 1 1 calc R . . 
C9 C 0.6515(5) 0.4129(5) 0.2016(5) 0.091(2) Uani 1 1 d . . . 
C10 C 0.5989(6) 0.3908(7) 0.1362(6) 0.101(2) Uani 1 1 d . . . 
H10 H 0.6412 0.4064 0.0894 0.121 Uiso 1 1 calc R . . 
C11 C 0.7930(7) 0.4649(8) 0.2283(7) 0.146(4) Uani 1 1 d . . . 
H11A H 0.8644 0.4001 0.2128 0.219 Uiso 1 1 calc R . . 
H11B H 0.7928 0.4725 0.2825 0.219 Uiso 1 1 calc R . . 
H11C H 0.8115 0.5552 0.2064 0.219 Uiso 1 1 calc R . . 
Cl12 Cl 0.6606(4) 0.3316(3) 0.44156(18) 0.1037(11) Uani 0.50 1 d PD . . 
O13A O 0.5329(18) 0.429(2) 0.4180(17) 0.053(5) Uiso 0.20 1 d PD A 1 
O14A O 0.620(2) 0.1887(15) 0.4330(13) 0.073(5) Uiso 0.20 1 d PD . 1 
O15A O 0.663(3) 0.367(2) 0.5167(9) 0.071(7) Uiso 0.20 1 d PD A 1 
O16A O 0.7868(17) 0.375(2) 0.4086(11) 0.082(4) Uiso 0.20 1 d PD . 1 
O14B O 0.7500 0.2500 0.4130(8) 0.086(3) Uiso 0.40 2 d SPD . 2 
O13B O 0.601(3) 0.4403(19) 0.4029(12) 0.083(5) Uiso 0.20 1 d PD A 2 
O15B O 0.550(3) 0.336(3) 0.4973(15) 0.118(8) Uiso 0.20 1 d PD A 2 
O16B O 0.627(4) 0.349(4) 0.5195(11) 0.103(12) Uiso 0.20 1 d PD A 2 
O13C O 0.529(5) 0.408(9) 0.426(6) 0.11(4) Uiso 0.10 1 d PD A 3 
O14C O 0.674(3) 0.1771(16) 0.4403(14) 0.040(5) Uiso 0.10 1 d PD . 3 
O15C O 0.643(3) 0.199(2) 0.4026(17) 0.052(6) Uiso 0.10 1 d PD . 3 
O16C O 0.545(3) 0.394(5) 0.403(2) 0.056(9) Uiso 0.10 1 d PD A 3 
 
 
_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 2.031(8) . ? 
Fe1 N7 2.095(4) . ? 
N2 C3 1.338(6) . ? 
C3 C4 1.453(10) . ? 
C3 C6 1.467(8) . ? 
C4 C5 1.353(13) . ? 
C4 H4 0.9500 . ? 
C5 H5 0.9500 . ? 
C6 N7 1.332(8) . ? 
C6 C10 1.363(8) . ? 
N7 N8 1.337(6) . ? 
N8 C9 1.379(9) . ? 
N8 H8 0.8800 . ? 
C9 C10 1.302(12) . ? 
C9 C11 1.545(9) . ? 
C10 H10 0.9500 . ? 
C11 H11A 0.9800 . ? 
C11 H11B 0.9800 . ? 
C11 H11C 0.9800 . ? 
Cl12 O15A 1.396(15) . ? 
Cl12 O16A 1.429(14) . ? 
Cl12 O14A 1.455(14) . ? 
Cl12 O13A 1.621(14) . ? 
Cl12 O14B 1.285(7) . ? 
Cl12 O13B 1.394(15) . ? 
Cl12 O16B 1.450(17) . ? 
Cl12 O15B 1.476(17) . ? 
Cl12 O16C 1.458(18) . ? 
Cl12 O15C 1.477(17) . ? 
Cl12 O13C 1.50(2) . ? 
Cl12 O14C 1.510(16) . ? 

 
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 180.00 6_566 . ? 
N2 Fe1 N7 75.62(14) . . ? 
N7 Fe1 N7 151.2(3) 3 . ? 
N2 Fe1 N7 104.38(14) . 6_566 ? 
N7 Fe1 N7 93.54(7) . 6_566 ? 
C3 N2 C3 119.3(7) 3 . ? 
C3 N2 Fe1 120.4(4) 3 . ? 
C3 N2 Fe1 120.4(4) . . ? 
N2 C3 C4 121.1(6) . . ? 
N2 C3 C6 112.4(5) . . ? 
C4 C3 C6 126.6(5) . . ? 
C5 C4 C3 119.3(9) . . ? 
C5 C4 H4 120.4 . . ? 
C3 C4 H4 120.4 . . ? 
C4 C5 C4 120.0(13) . 3 ? 
C4 C5 H5 120.0 . . ? 
N7 C6 C10 112.3(7) . . ? 
N7 C6 C3 114.6(4) . . ? 
C10 C6 C3 133.1(7) . . ? 
C6 N7 N8 104.1(4) . . ? 
C6 N7 Fe1 117.0(3) . . ? 
N8 N7 Fe1 138.8(4) . . ? 
N7 N8 C9 109.5(5) . . ? 
N7 N8 H8 125.3 . . ? 
C9 N8 H8 125.3 . . ? 
C10 C9 N8 108.5(5) . . ? 
C10 C9 C11 133.3(8) . . ? 
N8 C9 C11 118.1(8) . . ? 
C9 C10 C6 105.5(7) . . ? 
C9 C10 H10 127.2 . . ? 
C6 C10 H10 127.2 . . ? 
C9 C11 H11A 109.4 . . ? 
C9 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
C9 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
O15A Cl12 O16A 108.5(14) . . ? 
O15A Cl12 O14A 110.1(13) . . ? 
O16A Cl12 O14A 118.1(13) . . ? 
O15A Cl12 O13A 96.9(15) . . ? 
O16A Cl12 O13A 112.3(13) . . ? 
O14A Cl12 O13A 108.9(13) . . ? 
O14B Cl12 O13B 123.5(12) . . ? 
O14B Cl12 O16B 127.5(16) . . ? 
O13B Cl12 O16B 107.7(17) . . ? 
O14B Cl12 O15B 142.0(13) . . ? 
O13B Cl12 O15B 90.6(16) . . ? 
O16B Cl12 O15B 34.4(14) . . ? 
O16C Cl12 O15C 93(2) . . ? 
O16C Cl12 O13C 18(5) . . ? 
O15C Cl12 O13C 104(5) . . ? 
O16C Cl12 O14C 118(2) . . ? 
O15C Cl12 O14C 29.9(14) . . ? 
O13C Cl12 O14C 124(4) . . ? 
 
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 
N8 H8 O13A  0.88 2.16 3.00(3) 160.2 . 
N8 H8 O13B  0.88 1.92 2.78(2) 165.2 . 
N8 H8 O13C  0.88 2.27 3.12(11) 161.9 . 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              28.38 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.829 
_refine_diff_density_min   -0.585 
_refine_diff_density_rms    0.113 



#=END


 
data_tr11a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]iron(II) 
diperchlorate dimethanol solvate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
'C26 H26 Fe N10, 2[ClO4], 2[C H4 O]' 
_chemical_formula_sum             'C28 H34 Cl2 Fe N10 O10' 
_chemical_formula_weight          797.40 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 21/n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    13.6553(12) 
_cell_length_b                    19.7246(11) 
_cell_length_c                    13.6951(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.326(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      3687.7(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     72389 
_cell_measurement_theta_min       1.81 
_cell_measurement_theta_max       28.45  
 
_exptl_crystal_description        fragment 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.436 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1648 
_exptl_absorpt_coefficient_mu     0.619 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.565 
_exptl_absorpt_correction_T_max   0.714
_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             72389 
_diffrn_reflns_av_R_equivalents   0.0996 
_diffrn_reflns_av_sigmaI/netI     0.1129 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.81 
_diffrn_reflns_theta_max          28.45 
_reflns_number_total              7969 
_reflns_number_gt                 4436 
_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. 

 No disorder was detected during refinement. All non-H atoms were refined
 anisotropically, while C- and N-bound H atoms were placed in calculated 
 positions and refined using a riding model. The methanolic hydroxy H 
 atoms were located in the Fourier map and allowed to refine with the 
 restraints O---H = 0.90(2) and C...H = 1.90(2) Å, and with displacement 
 parameters of 1.2x those of the attached O atom. 

 The highest residual Fourier peak of +1.9 e.Å⁻³ is 0.9 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)+(0.0756P)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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7969 
_refine_ls_number_parameters      472 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.1157 
_refine_ls_R_factor_gt            0.0611 
_refine_ls_wR_factor_ref          0.1512 
_refine_ls_wR_factor_gt           0.1365 
_refine_ls_goodness_of_fit_ref    0.912 
_refine_ls_restrained_S_all       0.912 
_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 0.50913(3) 0.26370(2) 0.78278(4) 0.02047(13) Uani 1 1 d . . . 
N2 N 0.50551(18) 0.16557(14) 0.76306(19) 0.0222(6) Uani 1 1 d . . . 
C3 C 0.5832(2) 0.13324(17) 0.7208(2) 0.0241(7) Uani 1 1 d . . . 
C4 C 0.5825(3) 0.06309(18) 0.7047(3) 0.0329(8) Uani 1 1 d . . . 
H4 H 0.6374 0.0408 0.6779 0.039 Uiso 1 1 calc R . . 
C5 C 0.4977(3) 0.02652(19) 0.7296(3) 0.0392(9) Uani 1 1 d . . . 
H5 H 0.4946 -0.0209 0.7177 0.047 Uiso 1 1 calc R . . 
C6 C 0.4176(3) 0.05980(18) 0.7721(3) 0.0343(8) Uani 1 1 d . . . 
H6 H 0.3605 0.0353 0.7887 0.041 Uiso 1 1 calc R . . 
C7 C 0.4242(2) 0.12983(16) 0.7891(2) 0.0239(7) Uani 1 1 d . . . 
C8 C 0.6615(2) 0.18262(17) 0.6979(2) 0.0242(7) Uani 1 1 d . . . 
N9 N 0.64011(19) 0.24788(14) 0.7224(2) 0.0236(6) Uani 1 1 d . . . 
N10 N 0.7198(2) 0.28497(16) 0.6965(2) 0.0292(6) Uani 1 1 d . . . 
H10 H 0.7249 0.3291 0.7041 0.035 Uiso 1 1 calc R . . 
C11 C 0.7913(2) 0.2448(2) 0.6571(3) 0.0321(8) Uani 1 1 d . . . 
C12 C 0.7569(2) 0.17816(19) 0.6564(3) 0.0297(8) Uani 1 1 d . . . 
H12 H 0.7893 0.1388 0.6336 0.036 Uiso 1 1 calc R . . 
C13 C 0.8877(3) 0.2747(2) 0.6222(3) 0.0444(10) Uani 1 1 d . . . 
H13A H 0.8739 0.3101 0.5736 0.067 Uiso 1 1 calc R . . 
H13B H 0.9270 0.2389 0.5927 0.067 Uiso 1 1 calc R . . 
H13C H 0.9240 0.2943 0.6779 0.067 Uiso 1 1 calc R . . 
C14 C 0.3508(2) 0.17444(16) 0.8338(2) 0.0236(7) Uani 1 1 d . . . 
N15 N 0.37732(18) 0.24087(14) 0.8378(2) 0.0229(6) Uani 1 1 d . . . 
N16 N 0.30115(19) 0.27381(14) 0.8805(2) 0.0254(6) Uani 1 1 d . . . 
H16 H 0.2996 0.3177 0.8918 0.030 Uiso 1 1 calc R . . 
C17 C 0.2264(2) 0.22897(19) 0.9037(3) 0.0289(7) Uani 1 1 d . . . 
C18 C 0.2566(2) 0.16537(19) 0.8752(3) 0.0289(7) Uani 1 1 d . . . 
H18 H 0.2218 0.1240 0.8817 0.035 Uiso 1 1 calc R . . 
C19 C 0.1308(2) 0.2531(2) 0.9474(3) 0.0393(9) Uani 1 1 d . . . 
H19A H 0.1040 0.2172 0.9884 0.059 Uiso 1 1 calc R . . 
H19B H 0.0837 0.2641 0.8947 0.059 Uiso 1 1 calc R . . 
H19C H 0.1433 0.2936 0.9873 0.059 Uiso 1 1 calc R . . 
N20 N 0.51419(19) 0.36209(14) 0.7995(2) 0.0263(6) Uani 1 1 d . . . 
C21 C 0.4804(2) 0.40324(18) 0.7254(3) 0.0297(7) Uani 1 1 d . . . 
C22 C 0.4849(3) 0.47422(19) 0.7348(3) 0.0389(9) Uani 1 1 d . . . 
H22 H 0.4608 0.5028 0.6838 0.047 Uiso 1 1 calc R . . 
C23 C 0.5256(3) 0.5019(2) 0.8209(3) 0.0437(10) Uani 1 1 d . . . 
H23 H 0.5287 0.5497 0.8285 0.052 Uiso 1 1 calc R . . 
C24 C 0.5621(3) 0.45946(19) 0.8961(3) 0.0373(9) Uani 1 1 d . . . 
H24 H 0.5916 0.4782 0.9535 0.045 Uiso 1 1 calc R . . 
C25 C 0.5541(2) 0.38900(18) 0.8844(3) 0.0302(8) Uani 1 1 d . . . 
C26 C 0.4432(2) 0.36283(17) 0.6413(3) 0.0286(7) Uani 1 1 d . . . 
N27 N 0.44889(18) 0.29414(14) 0.6564(2) 0.0241(6) Uani 1 1 d . . . 
N28 N 0.41293(19) 0.26513(15) 0.57157(19) 0.0242(6) Uani 1 1 d . . . 
H28 H 0.4093 0.2211 0.5615 0.029 Uiso 1 1 calc R . . 
C29 C 0.3830(2) 0.31366(19) 0.5037(3) 0.0307(8) Uani 1 1 d . . . 
C30 C 0.4025(3) 0.3766(2) 0.5472(3) 0.0337(8) Uani 1 1 d . . . 
H30 H 0.3907 0.4200 0.5192 0.040 Uiso 1 1 calc R . . 
C31 C 0.3427(3) 0.2941(2) 0.4046(3) 0.0394(9) Uani 1 1 d . . . 
H31A H 0.3969 0.2829 0.3617 0.059 Uiso 1 1 calc R . . 
H31B H 0.3052 0.3320 0.3766 0.059 Uiso 1 1 calc R . . 
H31C H 0.2999 0.2545 0.4108 0.059 Uiso 1 1 calc R . . 
C32 C 0.5855(2) 0.33523(19) 0.9529(3) 0.0310(8) Uani 1 1 d . . . 
N33 N 0.57064(19) 0.27121(14) 0.9176(2) 0.0235(6) Uani 1 1 d . . . 
N34 N 0.60267(19) 0.22774(15) 0.9886(2) 0.0275(6) Uani 1 1 d . . . 
H34 H 0.6013 0.1833 0.9837 0.033 Uiso 1 1 calc R . . 
C35 C 0.6377(2) 0.2630(2) 1.0697(3) 0.0321(8) Uani 1 1 d . . . 
C36 C 0.6280(3) 0.3309(2) 1.0496(3) 0.0337(8) Uani 1 1 d . . . 
H36 H 0.6458 0.3676 1.0913 0.040 Uiso 1 1 calc R . . 
C37 C 0.6778(3) 0.2262(2) 1.1606(3) 0.0430(10) Uani 1 1 d . . . 
H37A H 0.6232 0.2117 1.2009 0.064 Uiso 1 1 calc R . . 
H37B H 0.7205 0.2568 1.1984 0.064 Uiso 1 1 calc R . . 
H37C H 0.7153 0.1863 1.1407 0.064 Uiso 1 1 calc R . . 
Cl38 Cl 0.73688(8) 0.46304(5) 0.61965(9) 0.0476(3) Uani 1 1 d . . . 
O39 O 0.7340(3) 0.42901(16) 0.7154(3) 0.0682(10) Uani 1 1 d . . . 
O40 O 0.6553(3) 0.4399(2) 0.5597(3) 0.0707(11) Uani 1 1 d . . . 
O41 O 0.7300(3) 0.53527(15) 0.6352(3) 0.0599(9) Uani 1 1 d . . . 
O42 O 0.8275(3) 0.4474(2) 0.5716(4) 0.0889(14) Uani 1 1 d . . . 
Cl43 Cl 0.23714(7) 0.45274(4) 0.90053(8) 0.0371(2) Uani 1 1 d . . . 
O44 O 0.3217(2) 0.41554(15) 0.9404(2) 0.0461(7) Uani 1 1 d . . . 
O45 O 0.1581(3) 0.4482(2) 0.9692(4) 0.0912(15) Uani 1 1 d . . . 
O46 O 0.2069(3) 0.42174(19) 0.8091(3) 0.0850(13) Uani 1 1 d . . . 
O47 O 0.2624(2) 0.52329(15) 0.8881(3) 0.0576(9) Uani 1 1 d . . . 
C48 C 0.4096(5) 0.1011(3) 0.4429(4) 0.0676(16) Uani 1 1 d D . . 
H48A H 0.4576 0.1317 0.4141 0.101 Uiso 1 1 calc R . . 
H48B H 0.3517 0.0978 0.3995 0.101 Uiso 1 1 calc R . . 
H48C H 0.4388 0.0560 0.4516 0.101 Uiso 1 1 calc R . . 
O49 O 0.3815(2) 0.12707(15) 0.5359(2) 0.0473(8) Uani 1 1 d D . . 
H49 H 0.356(3) 0.0921(14) 0.5675(18) 0.057 Uiso 1 1 d D . . 
C50 C 0.5840(5) 0.0630(3) 1.0591(4) 0.0782(18) Uani 1 1 d D . . 
H50A H 0.6434 0.0701 1.0994 0.117 Uiso 1 1 calc R . . 
H50B H 0.5724 0.0143 1.0510 0.117 Uiso 1 1 calc R . . 
H50C H 0.5280 0.0837 1.0910 0.117 Uiso 1 1 calc R . . 
O51 O 0.5960(3) 0.09302(17) 0.9668(2) 0.0592(9) Uani 1 1 d D . . 
H51 H 0.6577(19) 0.0877(18) 0.948(2) 0.071 Uiso 1 1 d D . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Fe1 N2 1.955(3) . ? 
Fe1 N20 1.955(3) . ? 
Fe1 N27 1.991(3) . ? 
Fe1 N9 2.012(3) . ? 
Fe1 N33 2.016(3) . ? 
Fe1 N15 2.018(2) . ? 
N2 C7 1.370(4) . ? 
N2 C3 1.377(4) . ? 
C3 C4 1.401(5) . ? 
C3 C8 1.485(5) . ? 
C4 C5 1.413(5) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.413(5) . ? 
C5 H5 0.9500 . ? 
C6 C7 1.404(5) . ? 
C6 H6 0.9500 . ? 
C7 C14 1.478(4) . ? 
C8 N9 1.363(4) . ? 
C8 C12 1.437(4) . ? 
N9 N10 1.365(4) . ? 
N10 C11 1.377(4) . ? 
N10 H10 0.8800 . ? 
C11 C12 1.395(5) . ? 
C11 C13 1.529(5) . ? 
C12 H12 0.9500 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C14 N15 1.360(4) . ? 
C14 C18 1.428(4) . ? 
N15 N16 1.369(4) . ? 
N16 C17 1.393(4) . ? 
N16 H16 0.8800 . ? 
C17 C18 1.380(5) . ? 
C17 C19 1.525(4) . ? 
C18 H18 0.9500 . ? 
C19 H19A 0.9800 . ? 
C19 H19B 0.9800 . ? 
C19 H19C 0.9800 . ? 
N20 C21 1.370(5) . ? 
N20 C25 1.379(5) . ? 
C21 C22 1.407(5) . ? 
C21 C26 1.482(5) . ? 
C22 C23 1.402(6) . ? 
C22 H22 0.9500 . ? 
C23 C24 1.409(6) . ? 
C23 H23 0.9500 . ? 
C24 C25 1.403(5) . ? 
C24 H24 0.9500 . ? 
C25 C32 1.474(5) . ? 
C26 N27 1.373(4) . ? 
C26 C30 1.417(5) . ? 
N27 N28 1.376(4) . ? 
N28 C29 1.389(5) . ? 
N28 H28 0.8800 . ? 
C29 C30 1.400(6) . ? 
C29 C31 1.503(5) . ? 
C30 H30 0.9500 . ? 
C31 H31A 0.9800 . ? 
C31 H31B 0.9800 . ? 
C31 H31C 0.9800 . ? 
C32 N33 1.366(4) . ? 
C32 C36 1.436(5) . ? 
N33 N34 1.361(4) . ? 
N34 C35 1.387(5) . ? 
N34 H34 0.8800 . ? 
C35 C36 1.373(6) . ? 
C35 C37 1.532(5) . ? 
C36 H36 0.9500 . ? 
C37 H37A 0.9800 . ? 
C37 H37B 0.9800 . ? 
C37 H37C 0.9800 . ? 
Cl38 O40 1.442(4) . ? 
Cl38 O41 1.444(3) . ? 
Cl38 O42 1.448(4) . ? 
Cl38 O39 1.474(4) . ? 
Cl43 O47 1.445(3) . ? 
Cl43 O46 1.445(4) . ? 
Cl43 O45 1.450(3) . ? 
Cl43 O44 1.463(3) . ? 
C48 O49 1.434(5) . ? 
C48 H48A 0.9800 . ? 
C48 H48B 0.9800 . ? 
C48 H48C 0.9800 . ? 
O49 H49 0.891(16) . ? 
C50 O51 1.409(6) . ? 
C50 H50A 0.9800 . ? 
C50 H50B 0.9800 . ? 
C50 H50C 0.9800 . ? 
O51 H51 0.891(17) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N2 Fe1 N20 178.63(11) . . ? 
N2 Fe1 N27 99.78(11) . . ? 
N20 Fe1 N27 79.34(12) . . ? 
N2 Fe1 N9 79.02(11) . . ? 
N20 Fe1 N9 99.94(11) . . ? 
N27 Fe1 N9 92.45(11) . . ? 
N2 Fe1 N33 102.00(11) . . ? 
N20 Fe1 N33 78.89(12) . . ? 
N27 Fe1 N33 158.22(11) . . ? 
N9 Fe1 N33 91.86(11) . . ? 
N2 Fe1 N15 79.09(11) . . ? 
N20 Fe1 N15 101.96(11) . . ? 
N27 Fe1 N15 92.15(11) . . ? 
N9 Fe1 N15 158.09(11) . . ? 
N33 Fe1 N15 91.77(11) . . ? 
C7 N2 C3 120.5(3) . . ? 
C7 N2 Fe1 119.5(2) . . ? 
C3 N2 Fe1 120.0(2) . . ? 
N2 C3 C4 121.4(3) . . ? 
N2 C3 C8 110.5(3) . . ? 
C4 C3 C8 128.1(3) . . ? 
C3 C4 C5 117.9(3) . . ? 
C3 C4 H4 121.0 . . ? 
C5 C4 H4 121.0 . . ? 
C4 C5 C6 120.6(3) . . ? 
C4 C5 H5 119.7 . . ? 
C6 C5 H5 119.7 . . ? 
C7 C6 C5 118.6(3) . . ? 
C7 C6 H6 120.7 . . ? 
C5 C6 H6 120.7 . . ? 
N2 C7 C6 120.8(3) . . ? 
N2 C7 C14 111.3(3) . . ? 
C6 C7 C14 127.9(3) . . ? 
N9 C8 C12 110.9(3) . . ? 
N9 C8 C3 114.1(3) . . ? 
C12 C8 C3 135.0(3) . . ? 
C8 N9 N10 105.4(2) . . ? 
C8 N9 Fe1 116.4(2) . . ? 
N10 N9 Fe1 138.2(2) . . ? 
N9 N10 C11 111.7(3) . . ? 
N9 N10 H10 124.2 . . ? 
C11 N10 H10 124.2 . . ? 
N10 C11 C12 107.7(3) . . ? 
N10 C11 C13 121.5(3) . . ? 
C12 C11 C13 130.8(3) . . ? 
C11 C12 C8 104.3(3) . . ? 
C11 C12 H12 127.8 . . ? 
C8 C12 H12 127.8 . . ? 
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 110.3(3) . . ? 
N15 C14 C7 114.0(3) . . ? 
C18 C14 C7 135.7(3) . . ? 
C14 N15 N16 105.6(2) . . ? 
C14 N15 Fe1 116.1(2) . . ? 
N16 N15 Fe1 138.3(2) . . ? 
N15 N16 C17 111.4(3) . . ? 
N15 N16 H16 124.3 . . ? 
C17 N16 H16 124.3 . . ? 
C18 C17 N16 106.7(3) . . ? 
C18 C17 C19 131.3(3) . . ? 
N16 C17 C19 122.0(3) . . ? 
C17 C18 C14 106.0(3) . . ? 
C17 C18 H18 127.0 . . ? 
C14 C18 H18 127.0 . . ? 
C17 C19 H19A 109.5 . . ? 
C17 C19 H19B 109.5 . . ? 
H19A C19 H19B 109.5 . . ? 
C17 C19 H19C 109.5 . . ? 
H19A C19 H19C 109.5 . . ? 
H19B C19 H19C 109.5 . . ? 
C21 N20 C25 121.0(3) . . ? 
C21 N20 Fe1 119.4(2) . . ? 
C25 N20 Fe1 119.5(2) . . ? 
N20 C21 C22 120.6(4) . . ? 
N20 C21 C26 111.1(3) . . ? 
C22 C21 C26 128.3(4) . . ? 
C23 C22 C21 118.7(4) . . ? 
C23 C22 H22 120.7 . . ? 
C21 C22 H22 120.7 . . ? 
C22 C23 C24 120.6(4) . . ? 
C22 C23 H23 119.7 . . ? 
C24 C23 H23 119.7 . . ? 
C25 C24 C23 118.7(4) . . ? 
C25 C24 H24 120.7 . . ? 
C23 C24 H24 120.7 . . ? 
N20 C25 C24 120.4(4) . . ? 
N20 C25 C32 111.3(3) . . ? 
C24 C25 C32 128.2(4) . . ? 
N27 C26 C30 110.3(3) . . ? 
N27 C26 C21 113.3(3) . . ? 
C30 C26 C21 136.4(3) . . ? 
C26 N27 N28 105.3(3) . . ? 
C26 N27 Fe1 116.8(2) . . ? 
N28 N27 Fe1 137.8(2) . . ? 
N27 N28 C29 111.9(3) . . ? 
N27 N28 H28 124.1 . . ? 
C29 N28 H28 124.1 . . ? 
N28 C29 C30 106.0(3) . . ? 
N28 C29 C31 121.5(3) . . ? 
C30 C29 C31 132.4(4) . . ? 
C29 C30 C26 106.5(3) . . ? 
C29 C30 H30 126.8 . . ? 
C26 C30 H30 126.8 . . ? 
C29 C31 H31A 109.5 . . ? 
C29 C31 H31B 109.5 . . ? 
H31A C31 H31B 109.5 . . ? 
C29 C31 H31C 109.5 . . ? 
H31A C31 H31C 109.5 . . ? 
H31B C31 H31C 109.5 . . ? 
N33 C32 C36 109.0(3) . . ? 
N33 C32 C25 113.6(3) . . ? 
C36 C32 C25 137.4(3) . . ? 
N34 N33 C32 106.7(3) . . ? 
N34 N33 Fe1 136.7(2) . . ? 
C32 N33 Fe1 116.6(2) . . ? 
N33 N34 C35 110.8(3) . . ? 
N33 N34 H34 124.6 . . ? 
C35 N34 H34 124.6 . . ? 
C36 C35 N34 107.4(3) . . ? 
C36 C35 C37 131.0(4) . . ? 
N34 C35 C37 121.5(4) . . ? 
C35 C36 C32 106.1(3) . . ? 
C35 C36 H36 126.9 . . ? 
C32 C36 H36 126.9 . . ? 
C35 C37 H37A 109.5 . . ? 
C35 C37 H37B 109.5 . . ? 
H37A C37 H37B 109.5 . . ? 
C35 C37 H37C 109.5 . . ? 
H37A C37 H37C 109.5 . . ? 
H37B C37 H37C 109.5 . . ? 
O40 Cl38 O41 110.2(2) . . ? 
O40 Cl38 O42 109.3(3) . . ? 
O41 Cl38 O42 109.7(2) . . ? 
O40 Cl38 O39 109.0(2) . . ? 
O41 Cl38 O39 108.4(2) . . ? 
O42 Cl38 O39 110.4(3) . . ? 
O47 Cl43 O46 111.7(2) . . ? 
O47 Cl43 O45 108.6(2) . . ? 
O46 Cl43 O45 109.5(3) . . ? 
O47 Cl43 O44 109.79(18) . . ? 
O46 Cl43 O44 108.6(2) . . ? 
O45 Cl43 O44 108.6(2) . . ? 
O49 C48 H48A 109.5 . . ? 
O49 C48 H48B 109.5 . . ? 
H48A C48 H48B 109.5 . . ? 
O49 C48 H48C 109.5 . . ? 
H48A C48 H48C 109.5 . . ? 
H48B C48 H48C 109.5 . . ? 
C48 O49 H49 105.7(18) . . ? 
O51 C50 H50A 109.5 . . ? 
O51 C50 H50B 109.5 . . ? 
H50A C50 H50B 109.5 . . ? 
O51 C50 H50C 109.5 . . ? 
H50A C50 H50C 109.5 . . ? 
H50B C50 H50C 109.5 . . ? 
C50 O51 H51 110(2) . . ? 
 
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 O39  0.88 1.98 2.859(5) 177.5 . 
N16 H16 O44  0.88 2.06 2.925(4) 167.0 . 
N28 H28 O49  0.88 1.92 2.798(4) 171.7 . 
N34 H34 O51  0.88 1.80 2.675(4) 176.8 . 
O49 H49 O47  0.891(16) 2.205(17) 3.038(4) 155(4) 2_546 
O51 H51 O41  0.891(17) 2.193(17) 3.007(5) 152(4) 2_646 
 
_diffrn_measured_fraction_theta_max    0.856 
_diffrn_reflns_theta_full              28.45 
_diffrn_measured_fraction_theta_full   0.856 
_refine_diff_density_max    1.947 
_refine_diff_density_min   -0.416 
_refine_diff_density_rms    0.093 


#=END


 
data_tr11b 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
Bis[2,6-bis(5-methylpyrazol-3-yl)pyridine]iron(II) diperchlorate 
nitromethane (1/0.83) diethyl ether (0.33) solvate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
'C26 H26 Fe N10, 2[ClO4], 0.83 [C H3 N O2], 0.33 [C4 H10 O]'   
_chemical_formula_sum 
 'C28.17 H31.83 Cl2 Fe N10.83 O10' 
_chemical_formula_weight          808.89 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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                    13.1968(7) 
_cell_length_b                    20.4571(12) 
_cell_length_c                    20.6896(12) 
_cell_angle_alpha                 86.131(2) 
_cell_angle_beta                  75.642(2) 
_cell_angle_gamma                 81.923(2) 
_cell_volume                      5354.3(5) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     108015 
_cell_measurement_theta_min       1.02 
_cell_measurement_theta_max       26.38  
 
_exptl_crystal_description        fragment 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.37 
_exptl_crystal_size_mid           0.28 
_exptl_crystal_size_min           0.13 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.505 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2500 
_exptl_absorpt_coefficient_mu     0.642 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.793 
_exptl_absorpt_correction_T_max   0.884 
_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             108015 
_diffrn_reflns_av_R_equivalents   0.0408 
_diffrn_reflns_av_sigmaI/netI     0.0347 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.02 
_diffrn_reflns_theta_max          26.38 
_reflns_number_total              21517 
_reflns_number_gt                 17306 
_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 three complex cations, six perchlorate anions 
 (two of which are disordered), three nitromethane molecules (one of which is 
 half-occupied) and one molecule of diethyl ether.

 The disordered anions were refined over two orientations, with the following 
 refined occupancies: 
    Cl58A-O62A (0.64) and Cl58B-O62B (0.36) 
    Cl63A-O67A (0.56) and Cl63B-O67B (0.44) 
 These were refined using the refined restraints Cl---O = 1.39(2) and 
 O...O = 2.27(2) Å. 

 All wholly occupied non-H atoms, plus the part-occupied Cl sites, were 
 refined anisotropically, while H atoms were placed in calculated positions 
 and refined using a riding model. There are six residual Fourier peaks of 
 >1.5 e.Å⁻³, which all lie within the disordered anion Cl63-O67. 
; 
 
_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)+(0.1226P)²+17.2359P] 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          21517 
_refine_ls_number_parameters      1430 
_refine_ls_number_restraints      40 
_refine_ls_R_factor_all           0.0948 
_refine_ls_R_factor_gt            0.0781 
_refine_ls_wR_factor_ref          0.2363 
_refine_ls_wR_factor_gt           0.2227 
_refine_ls_goodness_of_fit_ref    1.063 
_refine_ls_restrained_S_all       1.088 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Fe1A Fe 0.13207(5) 0.32066(3) 0.29114(3) 0.02137(15) Uani 1 1 d . . . 
N2A N 0.1189(3) 0.41367(17) 0.30837(18) 0.0248(7) Uani 1 1 d . . . 
C3A C 0.0228(4) 0.4464(2) 0.3360(2) 0.0317(10) Uani 1 1 d . . . 
C4A C 0.0100(4) 0.5134(2) 0.3478(3) 0.0426(12) Uani 1 1 d . . . 
H4A H -0.0579 0.5364 0.3656 0.051 Uiso 1 1 calc R . . 
C5A C 0.0986(5) 0.5457(2) 0.3329(3) 0.0432(12) Uani 1 1 d . . . 
H5A H 0.0917 0.5913 0.3414 0.052 Uiso 1 1 calc R . . 
C6A C 0.1970(4) 0.5124(2) 0.3056(2) 0.0355(11) Uani 1 1 d . . . 
H6A H 0.2580 0.5345 0.2958 0.043 Uiso 1 1 calc R . . 
C7A C 0.2049(3) 0.4458(2) 0.2930(2) 0.0259(9) Uani 1 1 d . . . 
C8A C -0.0577(4) 0.4016(2) 0.3510(2) 0.0323(10) Uani 1 1 d . . . 
N9A N -0.0207(3) 0.33887(18) 0.33383(18) 0.0268(8) Uani 1 1 d . . . 
N10A N -0.1056(3) 0.3054(2) 0.35214(19) 0.0303(8) Uani 1 1 d . . . 
H10A H -0.1036 0.2631 0.3461 0.036 Uiso 1 1 calc R . . 
C11A C -0.1944(4) 0.3456(3) 0.3809(3) 0.0368(11) Uani 1 1 d . . . 
C12A C -0.1660(4) 0.4076(3) 0.3806(3) 0.0388(11) Uani 1 1 d . . . 
H12A H -0.2106 0.4466 0.3970 0.047 Uiso 1 1 calc R . . 
C13A C -0.2986(4) 0.3209(3) 0.4051(3) 0.0464(13) Uani 1 1 d . . . 
H13A H -0.3490 0.3549 0.4312 0.070 Uiso 1 1 calc R . . 
H13B H -0.2911 0.2809 0.4333 0.070 Uiso 1 1 calc R . . 
H13C H -0.3242 0.3107 0.3669 0.070 Uiso 1 1 calc R . . 
C14A C 0.2992(3) 0.4011(2) 0.2619(2) 0.0255(9) Uani 1 1 d . . . 
N15A N 0.2804(3) 0.33894(17) 0.25636(17) 0.0244(7) Uani 1 1 d . . . 
N16A N 0.3744(3) 0.30651(18) 0.22577(18) 0.0255(7) Uani 1 1 d . . . 
H16A H 0.3844 0.2646 0.2156 0.031 Uiso 1 1 calc R . . 
C17A C 0.4517(4) 0.3462(2) 0.2125(2) 0.0283(9) Uani 1 1 d . . . 
C18A C 0.4052(4) 0.4079(2) 0.2346(2) 0.0312(10) Uani 1 1 d . . . 
H18A H 0.4382 0.4467 0.2318 0.037 Uiso 1 1 calc R . . 
C19A C 0.5639(4) 0.3213(3) 0.1806(3) 0.0399(11) Uani 1 1 d . . . 
H19A H 0.5670 0.2792 0.1598 0.060 Uiso 1 1 calc R . . 
H19B H 0.6048 0.3148 0.2147 0.060 Uiso 1 1 calc R . . 
H19C H 0.5935 0.3536 0.1465 0.060 Uiso 1 1 calc R . . 
N20A N 0.1398(3) 0.22808(17) 0.27453(18) 0.0258(7) Uani 1 1 d . . . 
C21A C 0.1225(4) 0.2099(2) 0.2167(2) 0.0316(10) Uani 1 1 d . . . 
C22A C 0.1229(4) 0.1437(3) 0.2048(3) 0.0420(12) Uani 1 1 d . . . 
H22A H 0.1093 0.1312 0.1647 0.050 Uiso 1 1 calc R . . 
C23A C 0.1434(5) 0.0964(3) 0.2525(3) 0.0457(13) Uani 1 1 d . . . 
H23A H 0.1448 0.0510 0.2450 0.055 Uiso 1 1 calc R . . 
C24A C 0.1622(4) 0.1155(2) 0.3117(3) 0.0400(12) Uani 1 1 d . . . 
H24A H 0.1768 0.0833 0.3446 0.048 Uiso 1 1 calc R . . 
C25A C 0.1591(4) 0.1821(2) 0.3216(2) 0.0299(9) Uani 1 1 d . . . 
C26A C 0.1052(4) 0.2675(2) 0.1734(2) 0.0299(9) Uani 1 1 d . . . 
N27A N 0.1085(3) 0.32541(18) 0.20019(18) 0.0266(8) Uani 1 1 d . . . 
N28A N 0.0968(3) 0.3723(2) 0.15238(19) 0.0296(8) Uani 1 1 d . . . 
H28A H 0.0963 0.4148 0.1570 0.035 Uiso 1 1 calc R . . 
C29A C 0.0861(4) 0.3460(3) 0.0969(2) 0.0348(10) Uani 1 1 d . . . 
C30A C 0.0909(4) 0.2785(3) 0.1086(2) 0.0353(11) Uani 1 1 d . . . 
H30A H 0.0856 0.2464 0.0790 0.042 Uiso 1 1 calc R . . 
C31A C 0.0726(5) 0.3893(3) 0.0368(3) 0.0450(13) Uani 1 1 d . . . 
H31A H 0.0504 0.4352 0.0502 0.068 Uiso 1 1 calc R . . 
H31B H 0.0189 0.3743 0.0180 0.068 Uiso 1 1 calc R . . 
H31C H 0.1398 0.3867 0.0030 0.068 Uiso 1 1 calc R . . 
C32A C 0.1717(3) 0.2131(2) 0.3796(2) 0.0281(9) Uani 1 1 d . . . 
N33A N 0.1614(3) 0.27947(18) 0.37459(18) 0.0263(8) Uani 1 1 d . . . 
N34A N 0.1728(3) 0.2993(2) 0.43278(19) 0.0304(8) Uani 1 1 d . . . 
H34A H 0.1699 0.3409 0.4423 0.036 Uiso 1 1 calc R . . 
C35A C 0.1894(4) 0.2475(3) 0.4749(2) 0.0354(11) Uani 1 1 d . . . 
C36A C 0.1894(4) 0.1910(2) 0.4419(2) 0.0344(10) Uani 1 1 d . . . 
H36A H 0.1994 0.1466 0.4581 0.041 Uiso 1 1 calc R . . 
C37A C 0.2006(5) 0.2581(3) 0.5436(3) 0.0485(14) Uani 1 1 d . . . 
H37A H 0.2070 0.3047 0.5477 0.073 Uiso 1 1 calc R . . 
H37B H 0.2637 0.2306 0.5513 0.073 Uiso 1 1 calc R . . 
H37C H 0.1383 0.2461 0.5766 0.073 Uiso 1 1 calc R . . 
Fe1B Fe 0.79908(5) 0.28273(3) 0.97366(3) 0.02904(17) Uani 1 1 d . . . 
N2B N 0.8160(3) 0.1901(2) 1.01193(19) 0.0347(9) Uani 1 1 d . . . 
C3B C 0.7298(4) 0.1623(3) 1.0433(2) 0.0383(11) Uani 1 1 d . . . 
C4B C 0.7386(5) 0.0984(3) 1.0712(3) 0.0473(14) Uani 1 1 d . . . 
H4B H 0.6776 0.0787 1.0934 0.057 Uiso 1 1 calc R . . 
C5B C 0.8383(5) 0.0645(3) 1.0656(3) 0.0521(15) Uani 1 1 d . . . 
H5B H 0.8461 0.0208 1.0839 0.062 Uiso 1 1 calc R . . 
C6B C 0.9278(5) 0.0935(3) 1.0336(3) 0.0462(13) Uani 1 1 d . . . 
H6B H 0.9965 0.0702 1.0301 0.055 Uiso 1 1 calc R . . 
C7B C 0.9136(4) 0.1576(2) 1.0069(2) 0.0365(11) Uani 1 1 d . . . 
C8B C 0.6331(4) 0.2055(3) 1.0412(2) 0.0406(12) Uani 1 1 d . . . 
N9B N 0.6469(3) 0.2646(2) 1.0103(2) 0.0372(9) Uani 1 1 d . . . 
N10B N 0.5493(3) 0.2965(3) 1.0125(2) 0.0486(12) Uani 1 1 d . . . 
H10B H 0.5366 0.3368 0.9960 0.058 Uiso 1 1 calc R . . 
C11B C 0.4737(5) 0.2590(4) 1.0432(3) 0.0614(19) Uani 1 1 d . . . 
C12B C 0.5232(5) 0.2014(4) 1.0635(3) 0.0604(19) Uani 1 1 d . . . 
H12B H 0.4908 0.1656 1.0877 0.072 Uiso 1 1 calc R . . 
C13B C 0.3584(5) 0.2846(6) 1.0522(4) 0.089(3) Uani 1 1 d . . . 
H13D H 0.3179 0.2473 1.0558 0.134 Uiso 1 1 calc R . . 
H13E H 0.3486 0.3132 1.0137 0.134 Uiso 1 1 calc R . . 
H13F H 0.3336 0.3098 1.0930 0.134 Uiso 1 1 calc R . . 
C14B C 0.9949(4) 0.1969(3) 0.9702(2) 0.0399(12) Uani 1 1 d . . . 
N15B N 0.9584(4) 0.2571(2) 0.9493(2) 0.0440(11) Uani 1 1 d . . . 
N16B N 1.0441(5) 0.2846(3) 0.9158(2) 0.0552(14) Uani 1 1 d . . . 
H16B H 1.0421 0.3244 0.8967 0.066 Uiso 1 1 calc R . . 
C17B C 1.1338(6) 0.2431(4) 0.9155(3) 0.063(2) Uani 1 1 d . . . 
C18B C 1.1052(5) 0.1856(3) 0.9504(3) 0.0506(14) Uani 1 1 d . . . 
H18B H 1.1502 0.1473 0.9589 0.061 Uiso 1 1 calc R . . 
C19B C 1.2416(6) 0.2610(5) 0.8814(4) 0.083(3) Uani 1 1 d . . . 
H19D H 1.2604 0.2474 0.8350 0.124 Uiso 1 1 calc R . . 
H19E H 1.2934 0.2384 0.9048 0.124 Uiso 1 1 calc R . . 
H19F H 1.2410 0.3089 0.8824 0.124 Uiso 1 1 calc R . . 
N20B N 0.7593(3) 0.37562(18) 0.94342(19) 0.0284(8) Uani 1 1 d . . . 
C21B C 0.7448(4) 0.4253(2) 0.9857(2) 0.0302(9) Uani 1 1 d . . . 
C22B C 0.7024(4) 0.4888(2) 0.9702(3) 0.0403(12) Uani 1 1 d . . . 
H22B H 0.6923 0.5236 1.0004 0.048 Uiso 1 1 calc R . . 
C23B C 0.6755(5) 0.4998(3) 0.9097(3) 0.0490(14) Uani 1 1 d . . . 
H23B H 0.6459 0.5427 0.8980 0.059 Uiso 1 1 calc R . . 
C24B C 0.6909(5) 0.4496(3) 0.8662(3) 0.0429(12) Uani 1 1 d . . . 
H24B H 0.6729 0.4575 0.8245 0.052 Uiso 1 1 calc R . . 
C25B C 0.7334(4) 0.3866(2) 0.8842(2) 0.0311(10) Uani 1 1 d . . . 
C26B C 0.7731(4) 0.4022(2) 1.0479(2) 0.0305(9) Uani 1 1 d . . . 
N27B N 0.8002(3) 0.33644(19) 1.05356(19) 0.0317(8) Uani 1 1 d . . . 
N28B N 0.8219(3) 0.3262(2) 1.1140(2) 0.0390(10) Uani 1 1 d . . . 
H28B H 0.8421 0.2871 1.1303 0.047 Uiso 1 1 calc R . . 
C29B C 0.8093(4) 0.3833(3) 1.1468(3) 0.0417(12) Uani 1 1 d . . . 
C30B C 0.7780(4) 0.4336(3) 1.1053(2) 0.0363(11) Uani 1 1 d . . . 
H30B H 0.7631 0.4795 1.1137 0.044 Uiso 1 1 calc R . . 
C31B C 0.8252(5) 0.3837(4) 1.2156(3) 0.0544(15) Uani 1 1 d . . . 
H31D H 0.7594 0.3769 1.2482 0.082 Uiso 1 1 calc R . . 
H31E H 0.8458 0.4264 1.2227 0.082 Uiso 1 1 calc R . . 
H31F H 0.8808 0.3482 1.2212 0.082 Uiso 1 1 calc R . . 
C32B C 0.7540(4) 0.3266(2) 0.8465(2) 0.0326(10) Uani 1 1 d . . . 
N33B N 0.7881(3) 0.2716(2) 0.8791(2) 0.0342(9) Uani 1 1 d . . . 
N34B N 0.8060(4) 0.2223(2) 0.8367(2) 0.0448(11) Uani 1 1 d . . . 
H34B H 0.8284 0.1811 0.8460 0.054 Uiso 1 1 calc R . . 
C35B C 0.7853(4) 0.2441(3) 0.7780(3) 0.0470(14) Uani 1 1 d . . . 
C36B C 0.7510(4) 0.3104(3) 0.7825(3) 0.0462(13) Uani 1 1 d . . . 
H36B H 0.7296 0.3394 0.7491 0.055 Uiso 1 1 calc R . . 
C37B C 0.8025(5) 0.1988(4) 0.7206(3) 0.068(2) Uani 1 1 d . . . 
H37D H 0.8304 0.1543 0.7336 0.102 Uiso 1 1 calc R . . 
H37E H 0.8529 0.2154 0.6819 0.102 Uiso 1 1 calc R . . 
H37F H 0.7353 0.1974 0.7089 0.102 Uiso 1 1 calc R . . 
Fe1C Fe 0.50447(5) 0.24081(3) 0.63248(3) 0.02355(15) Uani 1 1 d . . . 
N2C N 0.4651(3) 0.33964(18) 0.65045(18) 0.0276(8) Uani 1 1 d . . . 
C3C C 0.3633(4) 0.3640(2) 0.6765(2) 0.0306(10) Uani 1 1 d . . . 
C4C C 0.3342(4) 0.4305(3) 0.6898(3) 0.0429(12) Uani 1 1 d . . . 
H4C H 0.2627 0.4471 0.7084 0.051 Uiso 1 1 calc R . . 
C5C C 0.4116(5) 0.4720(3) 0.6752(3) 0.0509(15) Uani 1 1 d . . . 
H5C H 0.3931 0.5177 0.6839 0.061 Uiso 1 1 calc R . . 
C6C C 0.5152(5) 0.4477(3) 0.6480(3) 0.0465(13) Uani 1 1 d . . . 
H6C H 0.5684 0.4762 0.6378 0.056 Uiso 1 1 calc R . . 
C7C C 0.5403(4) 0.3802(2) 0.6359(2) 0.0321(10) Uani 1 1 d . . . 
C8C C 0.2942(4) 0.3121(2) 0.6890(2) 0.0326(10) Uani 1 1 d . . . 
N9C N 0.3415(3) 0.25089(19) 0.6754(2) 0.0320(8) Uani 1 1 d . . . 
N10C N 0.2628(4) 0.2120(2) 0.6937(2) 0.0406(10) Uani 1 1 d . . . 
H10C H 0.2719 0.1688 0.6903 0.049 Uiso 1 1 calc R . . 
C11C C 0.1687(4) 0.2483(3) 0.7177(3) 0.0454(13) Uani 1 1 d . . . 
C12C C 0.1853(4) 0.3126(3) 0.7151(3) 0.0428(12) Uani 1 1 d . . . 
H12C H 0.1341 0.3498 0.7281 0.051 Uiso 1 1 calc R . . 
C13C C 0.0699(5) 0.2158(4) 0.7420(4) 0.070(2) Uani 1 1 d . . . 
H13G H 0.0700 0.1811 0.7115 0.106 Uiso 1 1 calc R . . 
H13H H 0.0080 0.2488 0.7434 0.106 Uiso 1 1 calc R . . 
H13I H 0.0673 0.1963 0.7868 0.106 Uiso 1 1 calc R . . 
C14C C 0.6437(4) 0.3455(2) 0.6065(2) 0.0312(10) Uani 1 1 d . . . 
N15C N 0.6482(3) 0.2797(2) 0.6005(2) 0.0327(9) Uani 1 1 d . . . 
N16C N 0.7499(3) 0.2596(2) 0.5698(2) 0.0414(10) Uani 1 1 d . . . 
H16C H 0.7749 0.2184 0.5597 0.050 Uiso 1 1 calc R . . 
C17C C 0.8088(4) 0.3103(3) 0.5562(3) 0.0452(13) Uani 1 1 d . . . 
C18C C 0.7428(4) 0.3665(3) 0.5791(3) 0.0437(13) Uani 1 1 d . . . 
H18C H 0.7605 0.4102 0.5770 0.052 Uiso 1 1 calc R . . 
C19C C 0.9232(4) 0.3008(4) 0.5217(3) 0.0634(19) Uani 1 1 d . . . 
H19G H 0.9415 0.3405 0.4945 0.095 Uiso 1 1 calc R . . 
H19H H 0.9379 0.2628 0.4929 0.095 Uiso 1 1 calc R . . 
H19I H 0.9653 0.2928 0.5550 0.095 Uiso 1 1 calc R . . 
N20C N 0.5481(3) 0.1424(2) 0.6118(2) 0.0344(9) Uani 1 1 d . . . 
C21C C 0.5512(4) 0.1213(3) 0.5511(2) 0.0406(12) Uani 1 1 d . . . 
C22C C 0.5801(6) 0.0552(3) 0.5357(3) 0.0556(16) Uani 1 1 d . . . 
H22C H 0.5828 0.0410 0.4924 0.067 Uiso 1 1 calc R . . 
C23C C 0.6047(6) 0.0102(3) 0.5845(3) 0.0616(18) Uani 1 1 d . . . 
H23C H 0.6243 -0.0353 0.5749 0.074 Uiso 1 1 calc R . . 
C24C C 0.6007(5) 0.0321(3) 0.6478(3) 0.0519(15) Uani 1 1 d . . . 
H24C H 0.6168 0.0021 0.6820 0.062 Uiso 1 1 calc R . . 
C25C C 0.5724(4) 0.0993(3) 0.6593(2) 0.0373(11) Uani 1 1 d . . . 
C26C C 0.5196(4) 0.1748(3) 0.5069(2) 0.0419(12) Uani 1 1 d . . . 
N27C N 0.4930(3) 0.2350(2) 0.5338(2) 0.0361(9) Uani 1 1 d . . . 
N28C N 0.4670(3) 0.2752(3) 0.4842(2) 0.0529(13) Uani 1 1 d . . . 
H28C H 0.4468 0.3179 0.4878 0.064 Uiso 1 1 calc R . . 
C29C C 0.4757(5) 0.2418(4) 0.4283(3) 0.064(2) Uani 1 1 d . . . 
C30C C 0.5098(6) 0.1769(4) 0.4406(3) 0.0599(18) Uani 1 1 d . . . 
H30C H 0.5237 0.1414 0.4111 0.072 Uiso 1 1 calc R . . 
C31C C 0.4516(6) 0.2779(6) 0.3664(4) 0.094(3) Uani 1 1 d . . . 
H31G H 0.5127 0.2696 0.3285 0.141 Uiso 1 1 calc R . . 
H31H H 0.4361 0.3254 0.3739 0.141 Uiso 1 1 calc R . . 
H31I H 0.3904 0.2620 0.3567 0.141 Uiso 1 1 calc R . . 
C32C C 0.5645(4) 0.1309(3) 0.7218(3) 0.0404(12) Uani 1 1 d . . . 
N33C N 0.5347(3) 0.1968(2) 0.7215(2) 0.0400(10) Uani 1 1 d . . . 
N34C N 0.5309(4) 0.2135(3) 0.7846(2) 0.0573(15) Uani 1 1 d . . . 
H34C H 0.5127 0.2540 0.7990 0.069 Uiso 1 1 calc R . . 
C35C C 0.5585(5) 0.1604(5) 0.8230(3) 0.066(2) Uani 1 1 d . . . 
C36C C 0.5794(5) 0.1068(4) 0.7845(3) 0.0582(17) Uani 1 1 d . . . 
H36C H 0.5997 0.0624 0.7972 0.070 Uiso 1 1 calc R . . 
C37C C 0.5560(7) 0.1685(6) 0.8950(3) 0.099(3) Uani 1 1 d . . . 
H37G H 0.4936 0.1515 0.9235 0.149 Uiso 1 1 calc R . . 
H37H H 0.5532 0.2155 0.9032 0.149 Uiso 1 1 calc R . . 
H37I H 0.6197 0.1440 0.9054 0.149 Uiso 1 1 calc R . . 
Cl38 Cl 0.46234(11) 0.12472(6) 0.23734(6) 0.0426(3) Uani 1 1 d . . . 
O39 O 0.4285(5) 0.1165(2) 0.3084(2) 0.0670(13) Uani 1 1 d . . . 
O40 O 0.3828(3) 0.16942(17) 0.2136(2) 0.0440(9) Uani 1 1 d . . . 
O41 O 0.4735(4) 0.0633(2) 0.2063(2) 0.0697(14) Uani 1 1 d . . . 
O42 O 0.5595(4) 0.1527(3) 0.2197(3) 0.0739(14) Uani 1 1 d . . . 
Cl43 Cl -0.12767(12) 0.13078(7) 0.41728(8) 0.0504(3) Uani 1 1 d . . . 
O44 O -0.2013(5) 0.1749(3) 0.4605(3) 0.0934(19) Uani 1 1 d . . . 
O45 O -0.1705(5) 0.0744(3) 0.4059(3) 0.0781(16) Uani 1 1 d . . . 
O46 O -0.0901(4) 0.1652(2) 0.3527(2) 0.0611(12) Uani 1 1 d . . . 
O47 O -0.0378(4) 0.1099(3) 0.4447(2) 0.0704(13) Uani 1 1 d . . . 
Cl48 Cl -0.00297(11) 0.55358(7) 0.16712(7) 0.0488(3) Uani 1 1 d . . . 
O49 O -0.0146(7) 0.5578(4) 0.1011(3) 0.121(3) Uani 1 1 d . . . 
O50 O 0.0858(4) 0.5053(2) 0.1709(3) 0.0762(16) Uani 1 1 d . . . 
O51 O 0.0196(4) 0.6158(2) 0.1848(3) 0.0780(16) Uani 1 1 d . . . 
O52 O -0.0929(4) 0.5349(3) 0.2131(3) 0.0793(16) Uani 1 1 d . . . 
Cl53 Cl 0.43725(13) 0.39541(9) 0.86818(10) 0.0672(5) Uani 1 1 d . . . 
O54 O 0.4720(9) 0.3309(7) 0.8497(9) 0.291(10) Uani 1 1 d . . . 
O55 O 0.3273(4) 0.4042(3) 0.8860(4) 0.095(2) Uani 1 1 d . . . 
O56 O 0.4751(8) 0.4458(7) 0.8284(5) 0.232(8) Uani 1 1 d . . . 
O57 O 0.4725(5) 0.3992(4) 0.9287(3) 0.114(2) Uani 1 1 d . . . 
Cl58A Cl 0.9427(6) 0.0472(3) 0.8399(2) 0.0459(10) Uani 0.64 1 d PD A 1 
O59A O 1.0249(6) 0.0698(4) 0.8616(4) 0.076(2) Uiso 0.64 1 d PD A 1 
O60A O 0.8469(6) 0.0851(4) 0.8730(4) 0.077(2) Uiso 0.64 1 d PD A 1 
O61A O 0.9399(7) -0.0194(4) 0.8636(4) 0.067(2) Uiso 0.64 1 d PD A 1 
O62A O 0.9614(8) 0.0501(5) 0.7712(4) 0.088(3) Uiso 0.64 1 d PD A 1 
Cl58B Cl 0.9206(12) 0.0445(6) 0.8429(7) 0.081(5) Uani 0.36 1 d PD B 2 
O59B O 0.8413(13) 0.0608(9) 0.8065(9) 0.107(6) Uiso 0.36 1 d PD B 2 
O60B O 0.9298(12) 0.1028(6) 0.8692(7) 0.081(4) Uiso 0.36 1 d PD B 2 
O61B O 0.8902(13) -0.0083(6) 0.8851(7) 0.073(4) Uiso 0.36 1 d PD B 2 
O62B O 1.0140(15) 0.0246(12) 0.7945(11) 0.169(11) Uiso 0.36 1 d PD B 2 
Cl63A Cl 0.1657(2) 0.45360(13) 0.50076(14) 0.0543(6) Uani 0.56 1 d PD C 1 
O64A O 0.2247(6) 0.4427(4) 0.5501(4) 0.059(2) Uiso 0.56 1 d PD C 1 
O65A O 0.1186(6) 0.5209(4) 0.5012(4) 0.060(2) Uiso 0.56 1 d PD C 1 
O66A O 0.0937(6) 0.4223(4) 0.4914(4) 0.061(2) Uiso 0.56 1 d PD C 1 
O67A O 0.2358(8) 0.4373(5) 0.4380(4) 0.085(3) Uiso 0.56 1 d PD C 1 
Cl63B Cl 0.3666(3) 0.44866(14) 0.48512(19) 0.0513(8) Uani 0.44 1 d PD D 2 
O64B O 0.4562(7) 0.4182(5) 0.4895(5) 0.058(2) Uiso 0.44 1 d PD D 2 
O65B O 0.3731(9) 0.5108(5) 0.5098(5) 0.067(3) Uiso 0.44 1 d PD D 2 
O66B O 0.3108(10) 0.4601(6) 0.4371(6) 0.087(4) Uiso 0.44 1 d PD D 2 
O67B O 0.3123(12) 0.4035(7) 0.5333(7) 0.115(5) Uiso 0.44 1 d PD D 2 
C68 C 0.9712(7) 0.0417(4) 0.5973(5) 0.087(3) Uani 1 1 d . . . 
H68A H 1.0397 0.0362 0.5648 0.130 Uiso 1 1 calc R . . 
H68B H 0.9258 0.0117 0.5872 0.130 Uiso 1 1 calc R . . 
H68C H 0.9815 0.0314 0.6423 0.130 Uiso 1 1 calc R . . 
N69 N 0.9237(6) 0.1071(3) 0.5935(4) 0.0794(18) Uani 1 1 d . . . 
O70 O 0.9822(6) 0.1509(3) 0.5871(3) 0.100(2) Uani 1 1 d . . . 
O71 O 0.8253(5) 0.1159(3) 0.5969(3) 0.0828(16) Uani 1 1 d . . . 
C72 C 0.8046(7) 0.1159(3) 1.2449(4) 0.068(2) Uani 1 1 d . . . 
H72D H 0.7511 0.0991 1.2274 0.102 Uiso 1 1 calc R . . 
H72E H 0.7836 0.1146 1.2938 0.102 Uiso 1 1 calc R . . 
H72F H 0.8726 0.0884 1.2299 0.102 Uiso 1 1 calc R . . 
N73 N 0.8146(5) 0.1845(3) 1.2203(3) 0.0562(13) Uani 1 1 d . . . 
O74 O 0.7587(5) 0.2292(3) 1.2545(3) 0.0802(15) Uani 1 1 d . . . 
O75 O 0.8752(4) 0.1937(2) 1.1653(3) 0.0672(13) Uani 1 1 d . . . 
C76 C 0.6519(8) -0.0362(5) 0.9101(5) 0.0319(19) Uiso 0.50 1 d P . . 
H76A H 0.6850 -0.0702 0.8775 0.048 Uiso 0.50 1 calc PR . . 
H76B H 0.6887 0.0030 0.8990 0.048 Uiso 0.50 1 calc PR . . 
H76C H 0.5778 -0.0242 0.9089 0.048 Uiso 0.50 1 calc PR . . 
N77 N 0.6580(8) -0.0617(5) 0.9765(5) 0.047(2) Uiso 0.50 1 d P . . 
O78 O 0.6213(10) -0.0284(6) 1.0196(6) 0.089(3) Uiso 0.50 1 d P . . 
O79 O 0.6918(10) -0.1169(7) 0.9783(6) 0.093(4) Uiso 0.50 1 d P . . 
C80 C 0.2986(6) 0.0888(4) 0.8125(3) 0.0630(18) Uani 1 1 d . . . 
H80A H 0.3570 0.1152 0.7967 0.094 Uiso 1 1 calc R . . 
H80B H 0.3061 0.0646 0.8540 0.094 Uiso 1 1 calc R . . 
H80C H 0.2315 0.1180 0.8209 0.094 Uiso 1 1 calc R . . 
C81 C 0.3006(6) 0.0414(3) 0.7614(3) 0.0607(17) Uani 1 1 d . . . 
H81A H 0.3673 0.0109 0.7540 0.073 Uiso 1 1 calc R . . 
H81B H 0.2414 0.0148 0.7772 0.073 Uiso 1 1 calc R . . 
O82 O 0.2918(3) 0.07551(18) 0.70013(19) 0.0452(9) Uani 1 1 d . . . 
C83 C 0.2761(6) 0.0338(3) 0.6515(3) 0.0574(16) Uani 1 1 d . . . 
H83A H 0.2120 0.0121 0.6702 0.069 Uiso 1 1 calc R . . 
H83B H 0.3370 -0.0011 0.6401 0.069 Uiso 1 1 calc R . . 
C84 C 0.2642(6) 0.0734(3) 0.5903(3) 0.0554(15) Uani 1 1 d . . . 
H84A H 0.2027 0.1071 0.6014 0.083 Uiso 1 1 calc R . . 
H84B H 0.2546 0.0443 0.5571 0.083 Uiso 1 1 calc R . . 
H84C H 0.3277 0.0949 0.5719 0.083 Uiso 1 1 calc R . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Fe1A N20A 1.932(4) . ? 
Fe1A N2A 1.935(3) . ? 
Fe1A N33A 1.971(4) . ? 
Fe1A N27A 1.976(4) . ? 
Fe1A N9A 1.983(4) . ? 
Fe1A N15A 1.990(4) . ? 
N2A C7A 1.350(6) . ? 
N2A C3A 1.355(6) . ? 
C3A C4A 1.387(7) . ? 
C3A C8A 1.463(7) . ? 
C4A C5A 1.381(8) . ? 
C4A H4A 0.9500 . ? 
C5A C6A 1.382(8) . ? 
C5A H5A 0.9500 . ? 
C6A C7A 1.390(6) . ? 
C6A H6A 0.9500 . ? 
C7A C14A 1.470(6) . ? 
C8A N9A 1.345(6) . ? 
C8A C12A 1.400(7) . ? 
N9A N10A 1.356(5) . ? 
N10A C11A 1.360(6) . ? 
N10A H10A 0.8800 . ? 
C11A C12A 1.372(7) . ? 
C11A C13A 1.489(7) . ? 
C12A H12A 0.9500 . ? 
C13A H13A 0.9800 . ? 
C13A H13B 0.9800 . ? 
C13A H13C 0.9800 . ? 
C14A N15A 1.347(5) . ? 
C14A C18A 1.395(6) . ? 
N15A N16A 1.347(5) . ? 
N16A C17A 1.356(6) . ? 
N16A H16A 0.8800 . ? 
C17A C18A 1.379(7) . ? 
C17A C19A 1.495(6) . ? 
C18A H18A 0.9500 . ? 
C19A H19A 0.9800 . ? 
C19A H19B 0.9800 . ? 
C19A H19C 0.9800 . ? 
N20A C25A 1.353(6) . ? 
N20A C21A 1.357(6) . ? 
C21A C22A 1.392(7) . ? 
C21A C26A 1.458(7) . ? 
C22A C23A 1.382(8) . ? 
C22A H22A 0.9500 . ? 
C23A C24A 1.399(8) . ? 
C23A H23A 0.9500 . ? 
C24A C25A 1.386(6) . ? 
C24A H24A 0.9500 . ? 
C25A C32A 1.448(7) . ? 
C26A N27A 1.352(6) . ? 
C26A C30A 1.397(7) . ? 
N27A N28A 1.352(5) . ? 
N28A C29A 1.346(6) . ? 
N28A H28A 0.8800 . ? 
C29A C30A 1.380(7) . ? 
C29A C31A 1.511(7) . ? 
C30A H30A 0.9500 . ? 
C31A H31A 0.9800 . ? 
C31A H31B 0.9800 . ? 
C31A H31C 0.9800 . ? 
C32A N33A 1.346(6) . ? 
C32A C36A 1.401(7) . ? 
N33A N34A 1.345(5) . ? 
N34A C35A 1.355(6) . ? 
N34A H34A 0.8800 . ? 
C35A C36A 1.381(7) . ? 
C35A C37A 1.498(7) . ? 
C36A H36A 0.9500 . ? 
C37A H37A 0.9800 . ? 
C37A H37B 0.9800 . ? 
C37A H37C 0.9800 . ? 
Fe1B N20B 2.000(4) . ? 
Fe1B N2B 2.009(4) . ? 
Fe1B N33B 2.026(4) . ? 
Fe1B N15B 2.037(5) . ? 
Fe1B N9B 2.040(4) . ? 
Fe1B N27B 2.050(4) . ? 
N2B C3B 1.343(6) . ? 
N2B C7B 1.347(7) . ? 
C3B C4B 1.394(8) . ? 
C3B C8B 1.455(8) . ? 
C4B C5B 1.380(9) . ? 
C4B H4B 0.9500 . ? 
C5B C6B 1.393(8) . ? 
C5B H5B 0.9500 . ? 
C6B C7B 1.396(8) . ? 
C6B H6B 0.9500 . ? 
C7B C14B 1.459(7) . ? 
C8B N9B 1.344(7) . ? 
C8B C12B 1.422(8) . ? 
N9B N10B 1.350(6) . ? 
N10B C11B 1.350(8) . ? 
N10B H10B 0.8800 . ? 
C11B C12B 1.359(11) . ? 
C11B C13B 1.508(9) . ? 
C12B H12B 0.9500 . ? 
C13B H13D 0.9800 . ? 
C13B H13E 0.9800 . ? 
C13B H13F 0.9800 . ? 
C14B N15B 1.342(7) . ? 
C14B C18B 1.400(8) . ? 
N15B N16B 1.347(6) . ? 
N16B C17B 1.354(10) . ? 
N16B H16B 0.8800 . ? 
C17B C18B 1.386(9) . ? 
C17B C19B 1.506(9) . ? 
C18B H18B 0.9500 . ? 
C19B H19D 0.9800 . ? 
C19B H19E 0.9800 . ? 
C19B H19F 0.9800 . ? 
N20B C25B 1.348(6) . ? 
N20B C21B 1.349(6) . ? 
C21B C22B 1.390(7) . ? 
C21B C26B 1.458(7) . ? 
C22B C23B 1.381(8) . ? 
C22B H22B 0.9500 . ? 
C23B C24B 1.372(8) . ? 
C23B H23B 0.9500 . ? 
C24B C25B 1.396(7) . ? 
C24B H24B 0.9500 . ? 
C25B C32B 1.454(7) . ? 
C26B N27B 1.347(6) . ? 
C26B C30B 1.408(7) . ? 
N27B N28B 1.347(6) . ? 
N28B C29B 1.360(7) . ? 
N28B H28B 0.8800 . ? 
C29B C30B 1.378(7) . ? 
C29B C31B 1.491(7) . ? 
C30B H30B 0.9500 . ? 
C31B H31D 0.9800 . ? 
C31B H31E 0.9800 . ? 
C31B H31F 0.9800 . ? 
C32B N33B 1.353(6) . ? 
C32B C36B 1.398(7) . ? 
N33B N34B 1.339(6) . ? 
N34B C35B 1.344(8) . ? 
N34B H34B 0.8800 . ? 
C35B C36B 1.371(9) . ? 
C35B C37B 1.508(8) . ? 
C36B H36B 0.9500 . ? 
C37B H37D 0.9800 . ? 
C37B H37E 0.9800 . ? 
C37B H37F 0.9800 . ? 
Fe1C N2C 2.051(4) . ? 
Fe1C N20C 2.058(4) . ? 
Fe1C N27C 2.096(4) . ? 
Fe1C N15C 2.097(4) . ? 
Fe1C N33C 2.098(5) . ? 
Fe1C N9C 2.100(4) . ? 
N2C C7C 1.346(6) . ? 
N2C C3C 1.354(6) . ? 
C3C C4C 1.387(7) . ? 
C3C C8C 1.463(7) . ? 
C4C C5C 1.383(8) . ? 
C4C H4C 0.9500 . ? 
C5C C6C 1.378(8) . ? 
C5C H5C 0.9500 . ? 
C6C C7C 1.400(7) . ? 
C6C H6C 0.9500 . ? 
C7C C14C 1.452(7) . ? 
C8C N9C 1.334(6) . ? 
C8C C12C 1.404(7) . ? 
N9C N10C 1.361(6) . ? 
N10C C11C 1.351(8) . ? 
N10C H10C 0.8800 . ? 
C11C C12C 1.358(8) . ? 
C11C C13C 1.507(7) . ? 
C12C H12C 0.9500 . ? 
C13C H13G 0.9800 . ? 
C13C H13H 0.9800 . ? 
C13C H13I 0.9800 . ? 
C14C N15C 1.352(6) . ? 
C14C C18C 1.405(7) . ? 
N15C N16C 1.353(6) . ? 
N16C C17C 1.357(7) . ? 
N16C H16C 0.8800 . ? 
C17C C18C 1.375(8) . ? 
C17C C19C 1.493(7) . ? 
C18C H18C 0.9500 . ? 
C19C H19G 0.9800 . ? 
C19C H19H 0.9800 . ? 
C19C H19I 0.9800 . ? 
N20C C25C 1.344(7) . ? 
N20C C21C 1.344(6) . ? 
C21C C22C 1.389(8) . ? 
C21C C26C 1.462(8) . ? 
C22C C23C 1.387(9) . ? 
C22C H22C 0.9500 . ? 
C23C C24C 1.401(8) . ? 
C23C H23C 0.9500 . ? 
C24C C25C 1.392(8) . ? 
C24C H24C 0.9500 . ? 
C25C C32C 1.459(7) . ? 
C26C N27C 1.350(7) . ? 
C26C C30C 1.407(7) . ? 
N27C N28C 1.353(6) . ? 
N28C C29C 1.354(9) . ? 
N28C H28C 0.8800 . ? 
C29C C30C 1.368(11) . ? 
C29C C31C 1.516(8) . ? 
C30C H30C 0.9500 . ? 
C31C H31G 0.9800 . ? 
C31C H31H 0.9800 . ? 
C31C H31I 0.9800 . ? 
C32C N33C 1.349(7) . ? 
C32C C36C 1.407(8) . ? 
N33C N34C 1.359(6) . ? 
N34C C35C 1.365(10) . ? 
N34C H34C 0.8800 . ? 
C35C C36C 1.355(10) . ? 
C35C C37C 1.502(8) . ? 
C36C H36C 0.9500 . ? 
C37C H37G 0.9800 . ? 
C37C H37H 0.9800 . ? 
C37C H37I 0.9800 . ? 
Cl38 O41 1.423(4) . ? 
Cl38 O42 1.431(5) . ? 
Cl38 O39 1.433(4) . ? 
Cl38 O40 1.451(4) . ? 
Cl43 O44 1.410(5) . ? 
Cl43 O45 1.412(5) . ? 
Cl43 O47 1.438(5) . ? 
Cl43 O46 1.473(5) . ? 
Cl48 O52 1.407(5) . ? 
Cl48 O49 1.407(6) . ? 
Cl48 O51 1.437(5) . ? 
Cl48 O50 1.437(5) . ? 
Cl53 O56 1.347(8) . ? 
Cl53 O54 1.381(10) . ? 
Cl53 O55 1.394(5) . ? 
Cl53 O57 1.451(7) . ? 
Cl58A O62A 1.379(10) . ? 
Cl58A O59A 1.416(10) . ? 
Cl58A O61A 1.420(9) . ? 
Cl58A O60A 1.428(10) . ? 
Cl58B O60B 1.376(14) . ? 
Cl58B O61B 1.383(14) . ? 
Cl58B O62B 1.410(16) . ? 
Cl58B O59B 1.426(15) . ? 
Cl63A O66A 1.276(8) . ? 
Cl63A O64A 1.419(7) . ? 
Cl63A O67A 1.425(9) . ? 
Cl63A O65A 1.428(7) . ? 
Cl63B O64B 1.278(9) . ? 
Cl63B O66B 1.367(10) . ? 
Cl63B O65B 1.423(9) . ? 
Cl63B O67B 1.439(11) . ? 
C68 N69 1.401(10) . ? 
C68 H68A 0.9800 . ? 
C68 H68B 0.9800 . ? 
C68 H68C 0.9800 . ? 
N69 O70 1.243(9) . ? 
N69 O71 1.271(9) . ? 
C72 N73 1.471(8) . ? 
C72 H72D 0.9800 . ? 
C72 H72E 0.9800 . ? 
C72 H72F 0.9800 . ? 
N73 O74 1.234(7) . ? 
N73 O75 1.238(7) . ? 
C76 N77 1.454(13) . ? 
C76 H76A 0.9800 . ? 
C76 H76B 0.9800 . ? 
C76 H76C 0.9800 . ? 
N77 O78 1.126(14) . ? 
N77 O79 1.158(15) . ? 
C80 C81 1.476(10) . ? 
C80 H80A 0.9800 . ? 
C80 H80B 0.9800 . ? 
C80 H80C 0.9800 . ? 
C81 O82 1.427(7) . ? 
C81 H81A 0.9900 . ? 
C81 H81B 0.9900 . ? 
O82 C83 1.433(7) . ? 
C83 C84 1.487(9) . ? 
C83 H83A 0.9900 . ? 
C83 H83B 0.9900 . ? 
C84 H84A 0.9800 . ? 
C84 H84B 0.9800 . ? 
C84 H84C 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 
N20A Fe1A N2A 177.94(15) . . ? 
N20A Fe1A N33A 78.85(15) . . ? 
N2A Fe1A N33A 101.64(15) . . ? 
N20A Fe1A N27A 78.93(15) . . ? 
N2A Fe1A N27A 100.59(15) . . ? 
N33A Fe1A N27A 157.76(15) . . ? 
N20A Fe1A N9A 99.01(15) . . ? 
N2A Fe1A N9A 79.00(15) . . ? 
N33A Fe1A N9A 91.41(15) . . ? 
N27A Fe1A N9A 93.09(15) . . ? 
N20A Fe1A N15A 103.22(15) . . ? 
N2A Fe1A N15A 78.78(15) . . ? 
N33A Fe1A N15A 92.28(15) . . ? 
N27A Fe1A N15A 91.73(15) . . ? 
N9A Fe1A N15A 157.76(15) . . ? 
C7A N2A C3A 120.1(4) . . ? 
C7A N2A Fe1A 120.2(3) . . ? 
C3A N2A Fe1A 119.6(3) . . ? 
N2A C3A C4A 121.3(5) . . ? 
N2A C3A C8A 110.8(4) . . ? 
C4A C3A C8A 128.0(5) . . ? 
C5A C4A C3A 118.2(5) . . ? 
C5A C4A H4A 120.9 . . ? 
C3A C4A H4A 120.9 . . ? 
C4A C5A C6A 120.8(5) . . ? 
C4A C5A H5A 119.6 . . ? 
C6A C5A H5A 119.6 . . ? 
C5A C6A C7A 118.5(5) . . ? 
C5A C6A H6A 120.7 . . ? 
C7A C6A H6A 120.7 . . ? 
N2A C7A C6A 121.0(4) . . ? 
N2A C7A C14A 110.6(4) . . ? 
C6A C7A C14A 128.4(4) . . ? 
N9A C8A C12A 110.6(4) . . ? 
N9A C8A C3A 114.1(4) . . ? 
C12A C8A C3A 135.3(4) . . ? 
C8A N9A N10A 105.2(4) . . ? 
C8A N9A Fe1A 116.4(3) . . ? 
N10A N9A Fe1A 138.3(3) . . ? 
N9A N10A C11A 111.6(4) . . ? 
N9A N10A H10A 124.2 . . ? 
C11A N10A H10A 124.2 . . ? 
N10A C11A C12A 106.9(4) . . ? 
N10A C11A C13A 122.2(5) . . ? 
C12A C11A C13A 130.9(5) . . ? 
C11A C12A C8A 105.7(4) . . ? 
C11A C12A H12A 127.2 . . ? 
C8A C12A H12A 127.2 . . ? 
C11A C13A H13A 109.5 . . ? 
C11A C13A H13B 109.5 . . ? 
H13A C13A H13B 109.5 . . ? 
C11A C13A H13C 109.5 . . ? 
H13A C13A H13C 109.5 . . ? 
H13B C13A H13C 109.5 . . ? 
N15A C14A C18A 110.9(4) . . ? 
N15A C14A C7A 113.9(4) . . ? 
C18A C14A C7A 135.1(4) . . ? 
N16A N15A C14A 105.1(3) . . ? 
N16A N15A Fe1A 138.4(3) . . ? 
C14A N15A Fe1A 116.4(3) . . ? 
N15A N16A C17A 111.9(4) . . ? 
N15A N16A H16A 124.1 . . ? 
C17A N16A H16A 124.1 . . ? 
N16A C17A C18A 106.9(4) . . ? 
N16A C17A C19A 122.2(4) . . ? 
C18A C17A C19A 130.9(4) . . ? 
C17A C18A C14A 105.2(4) . . ? 
C17A C18A H18A 127.4 . . ? 
C14A C18A H18A 127.4 . . ? 
C17A C19A H19A 109.5 . . ? 
C17A C19A H19B 109.5 . . ? 
H19A C19A H19B 109.5 . . ? 
C17A C19A H19C 109.5 . . ? 
H19A C19A H19C 109.5 . . ? 
H19B C19A H19C 109.5 . . ? 
C25A N20A C21A 120.7(4) . . ? 
C25A N20A Fe1A 119.6(3) . . ? 
C21A N20A Fe1A 119.7(3) . . ? 
N20A C21A C22A 120.8(5) . . ? 
N20A C21A C26A 110.9(4) . . ? 
C22A C21A C26A 128.3(4) . . ? 
C23A C22A C21A 118.8(5) . . ? 
C23A C22A H22A 120.6 . . ? 
C21A C22A H22A 120.6 . . ? 
C22A C23A C24A 120.1(5) . . ? 
C22A C23A H23A 119.9 . . ? 
C24A C23A H23A 119.9 . . ? 
C25A C24A C23A 118.8(5) . . ? 
C25A C24A H24A 120.6 . . ? 
C23A C24A H24A 120.6 . . ? 
N20A C25A C24A 120.7(4) . . ? 
N20A C25A C32A 110.9(4) . . ? 
C24A C25A C32A 128.4(5) . . ? 
N27A C26A C30A 110.2(4) . . ? 
N27A C26A C21A 113.6(4) . . ? 
C30A C26A C21A 136.1(4) . . ? 
N28A N27A C26A 105.4(4) . . ? 
N28A N27A Fe1A 137.8(3) . . ? 
C26A N27A Fe1A 116.8(3) . . ? 
C29A N28A N27A 111.8(4) . . ? 
C29A N28A H28A 124.1 . . ? 
N27A N28A H28A 124.1 . . ? 
N28A C29A C30A 107.2(4) . . ? 
N28A C29A C31A 120.8(5) . . ? 
C30A C29A C31A 132.0(5) . . ? 
C29A C30A C26A 105.4(4) . . ? 
C29A C30A H30A 127.3 . . ? 
C26A C30A H30A 127.3 . . ? 
C29A C31A H31A 109.5 . . ? 
C29A C31A H31B 109.5 . . ? 
H31A C31A H31B 109.5 . . ? 
C29A C31A H31C 109.5 . . ? 
H31A C31A H31C 109.5 . . ? 
H31B C31A H31C 109.5 . . ? 
N33A C32A C36A 110.2(4) . . ? 
N33A C32A C25A 114.1(4) . . ? 
C36A C32A C25A 135.7(4) . . ? 
N34A N33A C32A 105.8(4) . . ? 
N34A N33A Fe1A 137.6(3) . . ? 
C32A N33A Fe1A 116.6(3) . . ? 
N33A N34A C35A 111.8(4) . . ? 
N33A N34A H34A 124.1 . . ? 
C35A N34A H34A 124.1 . . ? 
N34A C35A C36A 106.8(4) . . ? 
N34A C35A C37A 120.9(5) . . ? 
C36A C35A C37A 132.3(5) . . ? 
C35A C36A C32A 105.5(4) . . ? 
C35A C36A H36A 127.3 . . ? 
C32A C36A H36A 127.3 . . ? 
C35A C37A H37A 109.5 . . ? 
C35A C37A H37B 109.5 . . ? 
H37A C37A H37B 109.5 . . ? 
C35A C37A H37C 109.5 . . ? 
H37A C37A H37C 109.5 . . ? 
H37B C37A H37C 109.5 . . ? 
N20B Fe1B N2B 171.23(17) . . ? 
N20B Fe1B N33B 77.43(16) . . ? 
N2B Fe1B N33B 104.47(16) . . ? 
N20B Fe1B N15B 111.43(17) . . ? 
N2B Fe1B N15B 77.18(17) . . ? 
N33B Fe1B N15B 92.53(17) . . ? 
N20B Fe1B N9B 94.28(17) . . ? 
N2B Fe1B N9B 77.21(18) . . ? 
N33B Fe1B N9B 90.71(16) . . ? 
N15B Fe1B N9B 154.18(18) . . ? 
N20B Fe1B N27B 77.08(15) . . ? 
N2B Fe1B N27B 101.18(15) . . ? 
N33B Fe1B N27B 154.33(16) . . ? 
N15B Fe1B N27B 93.97(17) . . ? 
N9B Fe1B N27B 94.11(16) . . ? 
C3B N2B C7B 121.3(5) . . ? 
C3B N2B Fe1B 119.4(4) . . ? 
C7B N2B Fe1B 119.3(3) . . ? 
N2B C3B C4B 121.0(5) . . ? 
N2B C3B C8B 111.9(5) . . ? 
C4B C3B C8B 127.2(5) . . ? 
C5B C4B C3B 118.1(5) . . ? 
C5B C4B H4B 121.0 . . ? 
C3B C4B H4B 121.0 . . ? 
C4B C5B C6B 121.1(5) . . ? 
C4B C5B H5B 119.5 . . ? 
C6B C5B H5B 119.5 . . ? 
C5B C6B C7B 118.0(6) . . ? 
C5B C6B H6B 121.0 . . ? 
C7B C6B H6B 121.0 . . ? 
N2B C7B C6B 120.6(5) . . ? 
N2B C7B C14B 111.8(5) . . ? 
C6B C7B C14B 127.5(5) . . ? 
N9B C8B C12B 108.8(6) . . ? 
N9B C8B C3B 115.2(4) . . ? 
C12B C8B C3B 136.1(6) . . ? 
C8B N9B N10B 106.2(4) . . ? 
C8B N9B Fe1B 116.3(4) . . ? 
N10B N9B Fe1B 137.4(4) . . ? 
C11B N10B N9B 111.6(6) . . ? 
C11B N10B H10B 124.2 . . ? 
N9B N10B H10B 124.2 . . ? 
N10B C11B C12B 107.2(5) . . ? 
N10B C11B C13B 121.2(8) . . ? 
C12B C11B C13B 131.6(7) . . ? 
C11B C12B C8B 106.2(6) . . ? 
C11B C12B H12B 126.9 . . ? 
C8B C12B H12B 126.9 . . ? 
C11B C13B H13D 109.5 . . ? 
C11B C13B H13E 109.5 . . ? 
H13D C13B H13E 109.5 . . ? 
C11B C13B H13F 109.5 . . ? 
H13D C13B H13F 109.5 . . ? 
H13E C13B H13F 109.5 . . ? 
N15B C14B C18B 111.0(5) . . ? 
N15B C14B C7B 114.8(5) . . ? 
C18B C14B C7B 134.2(6) . . ? 
C14B N15B N16B 105.8(5) . . ? 
C14B N15B Fe1B 116.8(3) . . ? 
N16B N15B Fe1B 137.4(4) . . ? 
N15B N16B C17B 111.2(5) . . ? 
N15B N16B H16B 124.4 . . ? 
C17B N16B H16B 124.4 . . ? 
N16B C17B C18B 107.6(6) . . ? 
N16B C17B C19B 122.6(7) . . ? 
C18B C17B C19B 129.8(8) . . ? 
C17B C18B C14B 104.4(6) . . ? 
C17B C18B H18B 127.8 . . ? 
C14B C18B H18B 127.8 . . ? 
C17B C19B H19D 109.5 . . ? 
C17B C19B H19E 109.5 . . ? 
H19D C19B H19E 109.5 . . ? 
C17B C19B H19F 109.5 . . ? 
H19D C19B H19F 109.5 . . ? 
H19E C19B H19F 109.5 . . ? 
C25B N20B C21B 120.5(4) . . ? 
C25B N20B Fe1B 119.1(3) . . ? 
C21B N20B Fe1B 119.8(3) . . ? 
N20B C21B C22B 121.5(4) . . ? 
N20B C21B C26B 111.5(4) . . ? 
C22B C21B C26B 126.9(4) . . ? 
C23B C22B C21B 117.9(5) . . ? 
C23B C22B H22B 121.1 . . ? 
C21B C22B H22B 121.1 . . ? 
C24B C23B C22B 120.8(5) . . ? 
C24B C23B H23B 119.6 . . ? 
C22B C23B H23B 119.6 . . ? 
C23B C24B C25B 119.2(5) . . ? 
C23B C24B H24B 120.4 . . ? 
C25B C24B H24B 120.4 . . ? 
N20B C25B C24B 120.2(4) . . ? 
N20B C25B C32B 111.8(4) . . ? 
C24B C25B C32B 128.1(5) . . ? 
N27B C26B C30B 111.0(4) . . ? 
N27B C26B C21B 115.0(4) . . ? 
C30B C26B C21B 134.1(4) . . ? 
N28B N27B C26B 104.9(4) . . ? 
N28B N27B Fe1B 138.8(3) . . ? 
C26B N27B Fe1B 116.3(3) . . ? 
N27B N28B C29B 112.3(4) . . ? 
N27B N28B H28B 123.9 . . ? 
C29B N28B H28B 123.9 . . ? 
N28B C29B C30B 106.8(4) . . ? 
N28B C29B C31B 121.7(5) . . ? 
C30B C29B C31B 131.5(6) . . ? 
C29B C30B C26B 105.0(5) . . ? 
C29B C30B H30B 127.5 . . ? 
C26B C30B H30B 127.5 . . ? 
C29B C31B H31D 109.5 . . ? 
C29B C31B H31E 109.5 . . ? 
H31D C31B H31E 109.5 . . ? 
C29B C31B H31F 109.5 . . ? 
H31D C31B H31F 109.5 . . ? 
H31E C31B H31F 109.5 . . ? 
N33B C32B C36B 109.2(5) . . ? 
N33B C32B C25B 114.6(4) . . ? 
C36B C32B C25B 136.2(5) . . ? 
N34B N33B C32B 106.3(4) . . ? 
N34B N33B Fe1B 137.1(4) . . ? 
C32B N33B Fe1B 116.5(3) . . ? 
N33B N34B C35B 111.3(5) . . ? 
N33B N34B H34B 124.4 . . ? 
C35B N34B H34B 124.4 . . ? 
N34B C35B C36B 107.5(5) . . ? 
N34B C35B C37B 121.9(6) . . ? 
C36B C35B C37B 130.6(6) . . ? 
C35B C36B C32B 105.7(5) . . ? 
C35B C36B H36B 127.1 . . ? 
C32B C36B H36B 127.1 . . ? 
C35B C37B H37D 109.5 . . ? 
C35B C37B H37E 109.5 . . ? 
H37D C37B H37E 109.5 . . ? 
C35B C37B H37F 109.5 . . ? 
H37D C37B H37F 109.5 . . ? 
H37E C37B H37F 109.5 . . ? 
N2C Fe1C N20C 178.05(16) . . ? 
N2C Fe1C N27C 103.27(16) . . ? 
N20C Fe1C N27C 75.74(17) . . ? 
N2C Fe1C N15C 75.90(15) . . ? 
N20C Fe1C N15C 102.38(16) . . ? 
N27C Fe1C N15C 91.55(16) . . ? 
N2C Fe1C N33C 105.32(16) . . ? 
N20C Fe1C N33C 75.69(17) . . ? 
N27C Fe1C N33C 151.40(18) . . ? 
N15C Fe1C N33C 95.65(16) . . ? 
N2C Fe1C N9C 75.87(15) . . ? 
N20C Fe1C N9C 105.86(15) . . ? 
N27C Fe1C N9C 96.00(15) . . ? 
N15C Fe1C N9C 151.75(16) . . ? 
N33C Fe1C N9C 90.63(16) . . ? 
C7C N2C C3C 120.2(4) . . ? 
C7C N2C Fe1C 120.0(3) . . ? 
C3C N2C Fe1C 119.8(3) . . ? 
N2C C3C C4C 121.2(4) . . ? 
N2C C3C C8C 111.8(4) . . ? 
C4C C3C C8C 127.0(4) . . ? 
C5C C4C C3C 118.5(5) . . ? 
C5C C4C H4C 120.7 . . ? 
C3C C4C H4C 120.7 . . ? 
C6C C5C C4C 120.6(5) . . ? 
C6C C5C H5C 119.7 . . ? 
C4C C5C H5C 119.7 . . ? 
C5C C6C C7C 118.6(5) . . ? 
C5C C6C H6C 120.7 . . ? 
C7C C6C H6C 120.7 . . ? 
N2C C7C C6C 120.9(5) . . ? 
N2C C7C C14C 112.2(4) . . ? 
C6C C7C C14C 126.9(4) . . ? 
N9C C8C C12C 110.9(4) . . ? 
N9C C8C C3C 116.1(4) . . ? 
C12C C8C C3C 133.0(5) . . ? 
C8C N9C N10C 105.0(4) . . ? 
C8C N9C Fe1C 116.4(3) . . ? 
N10C N9C Fe1C 138.6(3) . . ? 
C11C N10C N9C 111.2(4) . . ? 
C11C N10C H10C 124.4 . . ? 
N9C N10C H10C 124.4 . . ? 
N10C C11C C12C 107.7(4) . . ? 
N10C C11C C13C 120.8(6) . . ? 
C12C C11C C13C 131.5(6) . . ? 
C11C C12C C8C 105.2(5) . . ? 
C11C C12C H12C 127.4 . . ? 
C8C C12C H12C 127.4 . . ? 
C11C C13C H13G 109.5 . . ? 
C11C C13C H13H 109.5 . . ? 
H13G C13C H13H 109.5 . . ? 
C11C C13C H13I 109.5 . . ? 
H13G C13C H13I 109.5 . . ? 
H13H C13C H13I 109.5 . . ? 
N15C C14C C18C 110.8(4) . . ? 
N15C C14C C7C 115.9(4) . . ? 
C18C C14C C7C 133.2(5) . . ? 
C14C N15C N16C 104.7(4) . . ? 
C14C N15C Fe1C 116.0(3) . . ? 
N16C N15C Fe1C 139.1(3) . . ? 
N15C N16C C17C 112.2(5) . . ? 
N15C N16C H16C 123.9 . . ? 
C17C N16C H16C 123.9 . . ? 
N16C C17C C18C 107.0(5) . . ? 
N16C C17C C19C 122.3(6) . . ? 
C18C C17C C19C 130.7(6) . . ? 
C17C C18C C14C 105.3(5) . . ? 
C17C C18C H18C 127.4 . . ? 
C14C C18C H18C 127.4 . . ? 
C17C C19C H19G 109.5 . . ? 
C17C C19C H19H 109.5 . . ? 
H19G C19C H19H 109.5 . . ? 
C17C C19C H19I 109.5 . . ? 
H19G C19C H19I 109.5 . . ? 
H19H C19C H19I 109.5 . . ? 
C25C N20C C21C 120.1(5) . . ? 
C25C N20C Fe1C 119.9(3) . . ? 
C21C N20C Fe1C 120.0(4) . . ? 
N20C C21C C22C 121.4(5) . . ? 
N20C C21C C26C 112.2(5) . . ? 
C22C C21C C26C 126.3(5) . . ? 
C23C C22C C21C 118.9(5) . . ? 
C23C C22C H22C 120.5 . . ? 
C21C C22C H22C 120.5 . . ? 
C22C C23C C24C 119.7(6) . . ? 
C22C C23C H23C 120.2 . . ? 
C24C C23C H23C 120.2 . . ? 
C25C C24C C23C 118.1(6) . . ? 
C25C C24C H24C 121.0 . . ? 
C23C C24C H24C 121.0 . . ? 
N20C C25C C24C 121.8(5) . . ? 
N20C C25C C32C 112.5(5) . . ? 
C24C C25C C32C 125.7(5) . . ? 
N27C C26C C30C 111.7(6) . . ? 
N27C C26C C21C 115.4(4) . . ? 
C30C C26C C21C 132.9(6) . . ? 
C26C N27C N28C 104.2(5) . . ? 
C26C N27C Fe1C 116.6(3) . . ? 
N28C N27C Fe1C 139.2(4) . . ? 
N27C N28C C29C 112.0(6) . . ? 
N27C N28C H28C 124.0 . . ? 
C29C N28C H28C 124.0 . . ? 
N28C C29C C30C 107.9(5) . . ? 
N28C C29C C31C 120.4(8) . . ? 
C30C C29C C31C 131.7(8) . . ? 
C29C C30C C26C 104.2(6) . . ? 
C29C C30C H30C 127.9 . . ? 
C26C C30C H30C 127.9 . . ? 
C29C C31C H31G 109.5 . . ? 
C29C C31C H31H 109.5 . . ? 
H31G C31C H31H 109.5 . . ? 
C29C C31C H31I 109.5 . . ? 
H31G C31C H31I 109.5 . . ? 
H31H C31C H31I 109.5 . . ? 
N33C C32C C36C 111.4(5) . . ? 
N33C C32C C25C 115.3(5) . . ? 
C36C C32C C25C 133.3(6) . . ? 
C32C N33C N34C 103.8(5) . . ? 
C32C N33C Fe1C 116.6(3) . . ? 
N34C N33C Fe1C 139.5(4) . . ? 
N33C N34C C35C 112.3(6) . . ? 
N33C N34C H34C 123.9 . . ? 
C35C N34C H34C 123.9 . . ? 
C36C C35C N34C 107.0(5) . . ? 
C36C C35C C37C 132.6(8) . . ? 
N34C C35C C37C 120.3(8) . . ? 
C35C C36C C32C 105.5(7) . . ? 
C35C C36C H36C 127.2 . . ? 
C32C C36C H36C 127.2 . . ? 
C35C C37C H37G 109.5 . . ? 
C35C C37C H37H 109.5 . . ? 
H37G C37C H37H 109.5 . . ? 
C35C C37C H37I 109.5 . . ? 
H37G C37C H37I 109.5 . . ? 
H37H C37C H37I 109.5 . . ? 
O41 Cl38 O42 110.7(3) . . ? 
O41 Cl38 O39 110.6(3) . . ? 
O42 Cl38 O39 110.1(3) . . ? 
O41 Cl38 O40 107.8(3) . . ? 
O42 Cl38 O40 108.7(3) . . ? 
O39 Cl38 O40 108.8(3) . . ? 
O44 Cl43 O45 112.7(4) . . ? 
O44 Cl43 O47 109.8(4) . . ? 
O45 Cl43 O47 108.9(3) . . ? 
O44 Cl43 O46 109.1(3) . . ? 
O45 Cl43 O46 108.6(3) . . ? 
O47 Cl43 O46 107.6(3) . . ? 
O52 Cl48 O49 112.2(4) . . ? 
O52 Cl48 O51 109.8(3) . . ? 
O49 Cl48 O51 110.0(4) . . ? 
O52 Cl48 O50 108.8(4) . . ? 
O49 Cl48 O50 108.5(4) . . ? 
O51 Cl48 O50 107.4(3) . . ? 
O56 Cl53 O54 120.2(10) . . ? 
O56 Cl53 O55 111.3(6) . . ? 
O54 Cl53 O55 108.8(6) . . ? 
O56 Cl53 O57 104.9(5) . . ? 
O54 Cl53 O57 103.4(8) . . ? 
O55 Cl53 O57 107.1(4) . . ? 
O62A Cl58A O59A 111.5(7) . . ? 
O62A Cl58A O61A 109.7(6) . . ? 
O59A Cl58A O61A 106.1(6) . . ? 
O62A Cl58A O60A 114.3(7) . . ? 
O59A Cl58A O60A 106.6(6) . . ? 
O61A Cl58A O60A 108.2(7) . . ? 
O60B Cl58B O61B 119.8(12) . . ? 
O60B Cl58B O62B 109.3(14) . . ? 
O61B Cl58B O62B 110.3(13) . . ? 
O60B Cl58B O59B 105.4(12) . . ? 
O61B Cl58B O59B 105.7(12) . . ? 
O62B Cl58B O59B 105.1(13) . . ? 
O66A Cl63A O64A 129.6(5) . . ? 
O66A Cl63A O67A 94.1(6) . . ? 
O64A Cl63A O67A 107.7(5) . . ? 
O66A Cl63A O65A 103.0(5) . . ? 
O64A Cl63A O65A 109.4(5) . . ? 
O67A Cl63A O65A 111.9(5) . . ? 
O64B Cl63B O66B 136.6(8) . . ? 
O64B Cl63B O65B 99.6(6) . . ? 
O66B Cl63B O65B 107.8(7) . . ? 
O64B Cl63B O67B 91.3(7) . . ? 
O66B Cl63B O67B 105.7(8) . . ? 
O65B Cl63B O67B 115.5(8) . . ? 
N69 C68 H68A 109.5 . . ? 
N69 C68 H68B 109.5 . . ? 
H68A C68 H68B 109.5 . . ? 
N69 C68 H68C 109.5 . . ? 
H68A C68 H68C 109.5 . . ? 
H68B C68 H68C 109.5 . . ? 
O70 N69 O71 126.3(8) . . ? 
O70 N69 C68 116.6(8) . . ? 
O71 N69 C68 117.1(7) . . ? 
N73 C72 H72D 109.5 . . ? 
N73 C72 H72E 109.5 . . ? 
H72D C72 H72E 109.5 . . ? 
N73 C72 H72F 109.5 . . ? 
H72D C72 H72F 109.5 . . ? 
H72E C72 H72F 109.5 . . ? 
O74 N73 O75 123.9(6) . . ? 
O74 N73 C72 117.9(6) . . ? 
O75 N73 C72 118.1(6) . . ? 
N77 C76 H76A 109.5 . . ? 
N77 C76 H76B 109.5 . . ? 
H76A C76 H76B 109.5 . . ? 
N77 C76 H76C 109.5 . . ? 
H76A C76 H76C 109.5 . . ? 
H76B C76 H76C 109.5 . . ? 
O78 N77 O79 128.1(13) . . ? 
O78 N77 C76 117.7(11) . . ? 
O79 N77 C76 113.8(11) . . ? 
C81 C80 H80A 109.5 . . ? 
C81 C80 H80B 109.5 . . ? 
H80A C80 H80B 109.5 . . ? 
C81 C80 H80C 109.5 . . ? 
H80A C80 H80C 109.5 . . ? 
H80B C80 H80C 109.5 . . ? 
O82 C81 C80 110.4(5) . . ? 
O82 C81 H81A 109.6 . . ? 
C80 C81 H81A 109.6 . . ? 
O82 C81 H81B 109.6 . . ? 
C80 C81 H81B 109.6 . . ? 
H81A C81 H81B 108.1 . . ? 
C81 O82 C83 113.5(5) . . ? 
O82 C83 C84 110.1(5) . . ? 
O82 C83 H83A 109.6 . . ? 
C84 C83 H83A 109.6 . . ? 
O82 C83 H83B 109.6 . . ? 
C84 C83 H83B 109.6 . . ? 
H83A C83 H83B 108.1 . . ? 
C83 C84 H84A 109.5 . . ? 
C83 C84 H84B 109.5 . . ? 
H84A C84 H84B 109.5 . . ? 
C83 C84 H84C 109.5 . . ? 
H84A C84 H84C 109.5 . . ? 
H84B C84 H84C 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 
N10A H10A O46  0.88 1.98 2.847(6) 166.8 . 
N16A H16A O40  0.88 1.95 2.817(5) 166.4 . 
N28A H28A O50  0.88 1.87 2.752(6) 176.0 . 
N34A H34A O66A  0.88 2.02 2.817(9) 150.8 . 
N10B H10B O57  0.88 2.08 2.868(8) 148.6 . 
N16B H16B O51  0.88 2.27 3.002(8) 141.2 2_666 
N28B H28B O75  0.88 2.03 2.902(6) 173.9 . 
N34B H34B O60A  0.88 2.00 2.868(10) 167.8 . 
N34B H34B O60B  0.88 2.05 2.881(15) 157.6 . 
N10C H10C O82  0.88 1.89 2.763(6) 169.3 . 
N16C H16C O71  0.88 2.25 3.029(7) 147.2 . 
N28C H28C O64B  0.88 2.08 2.918(11) 159.8 . 
N34C H34C O54  0.88 1.89 2.754(10) 166.6 . 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              26.38 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    2.683 
_refine_diff_density_min   -1.084 
_refine_diff_density_rms    0.115 
