# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1444557'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2 C17 H15 N2 O2, Fe, 2 C3 H7 N O'
_chemical_formula_sum            'C40 H44 Fe N6 O6'
_chemical_formula_weight         760.66

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.5879(6)
_cell_length_b                   20.8699(10)
_cell_length_c                   13.6448(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.531(4)
_cell_angle_gamma                90
_cell_volume                     3577.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    5962
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      19.7

_exptl_crystal_description       prisms
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.480
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
SADABS.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            87367
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.621
_diffrn_reflns_theta_max         27.595
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8232
_reflns_number_gt                5241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;



_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'

_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'





_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0331P)²+2.7996P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8232
_refine_ls_number_parameters     500
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1888(2) 0.60162(13) 0.0476(2) 0.0246(6) Uani 1 1 d . . . . .
C2 C -0.1171(2) 0.55221(14) 0.0380(2) 0.0326(7) Uani 1 1 d . . . . .
H2 H -0.1226 0.5190 -0.0097 0.039 Uiso 1 1 calc R U . . .
C3 C -0.0352(2) 0.55967(13) 0.1105(2) 0.0294(7) Uani 1 1 d . . . . .
H3 H 0.0244 0.5321 0.1219 0.035 Uiso 1 1 calc R U . . .
C4 C -0.0563(2) 0.61412(12) 0.16279(19) 0.0188(6) Uani 1 1 d . . . . .
C5 C 0.00834(19) 0.64498(12) 0.24742(19) 0.0179(5) Uani 1 1 d . . . . .
C6 C -0.06479(19) 0.67753(12) 0.31619(18) 0.0180(5) Uani 1 1 d . . . . .
C7 C -0.0562(2) 0.73531(13) 0.3655(2) 0.0242(6) Uani 1 1 d . . . . .
H7 H -0.0006 0.7658 0.3611 0.029 Uiso 1 1 calc R U . . .
C8 C -0.1436(2) 0.74080(14) 0.4229(2) 0.0272(6) Uani 1 1 d . . . . .
H8 H -0.1585 0.7759 0.4643 0.033 Uiso 1 1 calc R U . . .
C9 C -0.20433(19) 0.68644(13) 0.40908(18) 0.0220(6) Uani 1 1 d . . . . .
C10 C -0.2902(2) 0.61205(14) -0.0035(2) 0.0302(7) Uani 1 1 d . . . . .
H10 H -0.3079 0.5857 -0.0589 0.036 Uiso 1 1 calc R U . . .
C11 C -0.3027(2) 0.66896(15) 0.4477(2) 0.0287(7) Uani 1 1 d . . . . .
H11 H -0.3315 0.6973 0.4938 0.034 Uiso 1 1 calc R U . . .
C12 C 0.0699(2) 0.59266(12) 0.3074(2) 0.0255(6) Uani 1 1 d . . . . .
H12A H 0.1083 0.6122 0.3644 0.038 Uiso 1 1 calc R U . . .
H12B H 0.1208 0.5719 0.2661 0.038 Uiso 1 1 calc R U . . .
H12C H 0.0197 0.5607 0.3296 0.038 Uiso 1 1 calc R U . . .
C13 C 0.08322(19) 0.69517(11) 0.20862(19) 0.0176(5) Uani 1 1 d . . . . .
C14 C 0.0666(2) 0.73087(12) 0.1203(2) 0.0207(6) Uani 1 1 d . . . . .
H14 H 0.0103 0.7246 0.0716 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1485(2) 0.77746(12) 0.1171(2) 0.0245(6) Uani 1 1 d . . . . .
H15 H 0.1564 0.8079 0.0663 0.029 Uiso 1 1 calc R U . . .
C16 C 0.2163(2) 0.77052(12) 0.2028(2) 0.0240(6) Uani 1 1 d . . . . .
H16 H 0.2779 0.7954 0.2196 0.029 Uiso 1 1 calc R U . . .
C17 C 0.1765(2) 0.72005(12) 0.2595(2) 0.0204(6) Uani 1 1 d . . . . .
H17 H 0.2068 0.7053 0.3209 0.024 Uiso 1 1 calc R U . . .
C18 C 0.6524(2) 0.50642(12) 0.2025(2) 0.0229(6) Uani 1 1 d . . . . .
C19 C 0.5845(2) 0.48037(13) 0.1303(2) 0.0274(6) Uani 1 1 d . . . . .
H19 H 0.5971 0.4429 0.0934 0.033 Uiso 1 1 calc R U . . .
C20 C 0.4939(2) 0.51881(13) 0.1212(2) 0.0254(6) Uani 1 1 d . . . . .
H20 H 0.4336 0.5122 0.0770 0.031 Uiso 1 1 calc R U . . .
C21 C 0.5074(2) 0.56813(12) 0.18776(19) 0.0178(5) Uani 1 1 d . . . . .
C22 C 0.42904(19) 0.61954(11) 0.21669(19) 0.0174(5) Uani 1 1 d . . . . .
C23 C 0.48610(19) 0.68145(12) 0.24467(18) 0.0182(5) Uani 1 1 d . . . . .
C24 C 0.4633(2) 0.72648(13) 0.3147(2) 0.0242(6) Uani 1 1 d . . . . .
H24 H 0.4053 0.7248 0.3559 0.029 Uiso 1 1 calc R U . . .
C25 C 0.5395(2) 0.77449(13) 0.3146(2) 0.0258(6) Uani 1 1 d . . . . .
H25 H 0.5429 0.8114 0.3553 0.031 Uiso 1 1 calc R U . . .
C26 C 0.6098(2) 0.75869(12) 0.2443(2) 0.0226(6) Uani 1 1 d . . . . .
C27 C 0.7569(2) 0.48674(14) 0.2362(2) 0.0294(7) Uani 1 1 d . . . . .
H27 H 0.7835 0.4484 0.2091 0.035 Uiso 1 1 calc R U . . .
C28 C 0.7077(2) 0.78818(13) 0.2216(2) 0.0268(6) Uani 1 1 d . . . . .
H28 H 0.7249 0.8280 0.2523 0.032 Uiso 1 1 calc R U . . .
C29 C 0.3752(2) 0.59362(12) 0.30677(19) 0.0203(6) Uani 1 1 d . . . . .
H29A H 0.3438 0.5516 0.2912 0.030 Uiso 1 1 calc R U . . .
H29B H 0.3192 0.6233 0.3245 0.030 Uiso 1 1 calc R U . . .
H29C H 0.4283 0.5894 0.3620 0.030 Uiso 1 1 calc R U . . .
C30 C 0.34789(19) 0.63077(11) 0.13078(18) 0.0163(5) Uani 1 1 d . . . . .
C31 C 0.25518(19) 0.59288(12) 0.10626(19) 0.0177(5) Uani 1 1 d . . . . .
H31 H 0.2314 0.5573 0.1425 0.021 Uiso 1 1 calc R U . . .
C32 C 0.2051(2) 0.61780(12) 0.01839(19) 0.0218(6) Uani 1 1 d . . . . .
H32 H 0.1414 0.6021 -0.0140 0.026 Uiso 1 1 calc R U . . .
C33 C 0.2665(2) 0.67017(12) -0.01276(19) 0.0220(6) Uani 1 1 d . . . . .
H33 H 0.2513 0.6955 -0.0697 0.026 Uiso 1 1 calc R U . . .
C34 C 0.35458(19) 0.67789(12) 0.05638(18) 0.0184(5) Uani 1 1 d . . . . .
H34 H 0.4089 0.7093 0.0533 0.022 Uiso 1 1 calc R U . . .
C35 C 0.3189(3) 0.94082(15) 0.0434(2) 0.0332(7) Uani 1 1 d . . . . .
H35 H 0.3165 0.9861 0.0508 0.040 Uiso 1 1 calc R U . . .
C36 C 0.4212(2) 0.84329(13) 0.0637(2) 0.0348(7) Uani 1 1 d . . . . .
H36A H 0.3550 0.8251 0.0339 0.052 Uiso 1 1 calc R U . . .
H36B H 0.4362 0.8246 0.1289 0.052 Uiso 1 1 calc R U . . .
H36C H 0.4799 0.8337 0.0221 0.052 Uiso 1 1 calc R U . . .
C37 C 0.5014(3) 0.94689(18) 0.1130(3) 0.0524(10) Uani 1 1 d . . . . .
H37A H 0.4850 0.9928 0.1131 0.079 Uiso 1 1 calc R U . . .
H37B H 0.5621 0.9391 0.0730 0.079 Uiso 1 1 calc R U . . .
H37C H 0.5190 0.9326 0.1805 0.079 Uiso 1 1 calc R U . . .
C38 C 0.8149(3) 0.95065(14) 0.1793(3) 0.0389(8) Uani 1 1 d . . . . .
H38 H 0.7780 0.9717 0.1257 0.047 Uiso 1 1 calc R U . . .
C39 C 0.9653(3) 0.88800(18) 0.2389(3) 0.0541(10) Uani 1 1 d . . . . .
H39A H 0.9295 0.8916 0.3005 0.081 Uiso 1 1 calc R U . . .
H39B H 1.0370 0.9063 0.2477 0.081 Uiso 1 1 calc R U . . .
H39C H 0.9703 0.8428 0.2205 0.081 Uiso 1 1 calc R U . . .
C40 C 0.9506(3) 0.92327(17) 0.0676(3) 0.0497(9) Uani 1 1 d . . . . .
H40A H 0.9069 0.9506 0.0227 0.075 Uiso 1 1 calc R U . . .
H40B H 0.9521 0.8796 0.0411 0.075 Uiso 1 1 calc R U . . .
H40C H 1.0232 0.9403 0.0744 0.075 Uiso 1 1 calc R U . . .
N1 N -0.14971(17) 0.63894(11) 0.12512(16) 0.0184(5) Uani 1 1 d . . . . .
N2 N -0.15474(17) 0.64823(11) 0.34344(16) 0.0196(5) Uani 1 1 d . . . . .
N3 N 0.60404(17) 0.56030(10) 0.23660(17) 0.0199(5) Uani 1 1 d . . . . .
N4 N 0.57513(17) 0.70152(10) 0.20216(17) 0.0192(5) Uani 1 1 d . . . . .
N5 N 0.40991(18) 0.91179(11) 0.07258(17) 0.0282(6) Uani 1 1 d . . . . .
N6 N 0.90558(19) 0.92219(11) 0.16301(19) 0.0297(6) Uani 1 1 d . . . . .
O1 O -0.35588(16) 0.65201(10) 0.01816(14) 0.0334(5) Uani 1 1 d . . . . .
O2 O -0.35336(15) 0.62009(10) 0.42614(15) 0.0338(5) Uani 1 1 d . . . . .
O3 O 0.81526(15) 0.51482(9) 0.29694(15) 0.0311(5) Uani 1 1 d . . . . .
O4 O 0.77156(15) 0.76626(9) 0.16569(15) 0.0297(5) Uani 1 1 d . . . . .
O5 O 0.23873(18) 0.91482(11) 0.00818(16) 0.0435(6) Uani 1 1 d . . . . .
O6 O 0.77412(19) 0.95189(10) 0.26033(19) 0.0509(7) Uani 1 1 d . . . . .
Fe1 Fe 0.21284(3) 0.68721(2) 0.12347(3) 0.01656(10) Uani 1 1 d . . . . .
H2N H -0.174(2) 0.6096(13) 0.3268(19) 0.016(7) Uiso 1 1 d . . . . .
H4N H 0.602(2) 0.6826(14) 0.151(2) 0.032(8) Uiso 1 1 d . . . . .
H3N H 0.630(2) 0.5824(13) 0.288(2) 0.028(8) Uiso 1 1 d . . . . .
H1N H -0.179(2) 0.6744(14) 0.143(2) 0.032(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.379(3) . ?
C1 C2 1.382(4) . ?
C1 C10 1.433(4) . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.357(3) . ?
C4 C5 1.515(4) . ?
C5 C6 1.515(3) . ?
C5 C13 1.525(3) . ?
C5 C12 1.544(3) . ?
C6 N2 1.359(3) . ?
C6 C7 1.382(4) . ?
C7 C8 1.394(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(4) . ?
C8 H8 0.9500 . ?
C9 N2 1.377(3) . ?
C9 C11 1.423(4) . ?
C10 O1 1.223(3) . ?
C10 H10 0.9500 . ?
C11 O2 1.229(3) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.422(4) . ?
C13 C17 1.425(3) . ?
C13 Fe1 2.067(2) . ?
C14 C15 1.420(4) . ?
C14 Fe1 2.052(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.411(4) . ?
C15 Fe1 2.050(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.416(4) . ?
C16 Fe1 2.047(3) . ?
C16 H16 0.9500 . ?
C17 Fe1 2.056(3) . ?
C17 H17 0.9500 . ?
C18 N3 1.374(3) . ?
C18 C19 1.375(4) . ?
C18 C27 1.427(4) . ?
C19 C20 1.394(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(4) . ?
C20 H20 0.9500 . ?
C21 N3 1.360(3) . ?
C21 C22 1.526(3) . ?
C22 C23 1.516(3) . ?
C22 C30 1.525(3) . ?
C22 C29 1.538(3) . ?
C23 N4 1.359(3) . ?
C23 C24 1.383(4) . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(4) . ?
C25 H25 0.9500 . ?
C26 N4 1.383(3) . ?
C26 C28 1.428(4) . ?
C27 O3 1.222(3) . ?
C27 H27 0.9500 . ?
C28 O4 1.231(3) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C34 1.419(3) . ?
C30 C31 1.432(3) . ?
C30 Fe1 2.066(2) . ?
C31 C32 1.419(4) . ?
C31 Fe1 2.057(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.419(4) . ?
C32 Fe1 2.036(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.420(4) . ?
C33 Fe1 2.047(3) . ?
C33 H33 0.9500 . ?
C34 Fe1 2.064(2) . ?
C34 H34 0.9500 . ?
C35 O5 1.219(3) . ?
C35 N5 1.334(4) . ?
C35 H35 0.9500 . ?
C36 N5 1.442(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 N5 1.445(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 O6 1.247(4) . ?
C38 N6 1.318(4) . ?
C38 H38 0.9500 . ?
C39 N6 1.432(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 N6 1.452(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N1 H1N 0.87(3) . ?
N2 H2N 0.87(3) . ?
N3 H3N 0.88(3) . ?
N4 H4N 0.89(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 106.9(3) . . ?
N1 C1 C10 123.5(3) . . ?
C2 C1 C10 129.4(3) . . ?
C1 C2 C3 107.9(2) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
C4 C3 C2 107.6(3) . . ?
C4 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
N1 C4 C3 108.0(2) . . ?
N1 C4 C5 122.6(2) . . ?
C3 C4 C5 129.4(2) . . ?
C4 C5 C6 110.1(2) . . ?
C4 C5 C13 110.0(2) . . ?
C6 C5 C13 108.6(2) . . ?
C4 C5 C12 109.4(2) . . ?
C6 C5 C12 107.1(2) . . ?
C13 C5 C12 111.6(2) . . ?
N2 C6 C7 107.5(2) . . ?
N2 C6 C5 121.1(2) . . ?
C7 C6 C5 131.3(2) . . ?
C6 C7 C8 107.7(2) . . ?
C6 C7 H7 126.2 . . ?
C8 C7 H7 126.2 . . ?
C9 C8 C7 107.9(2) . . ?
C9 C8 H8 126.1 . . ?
C7 C8 H8 126.1 . . ?
C8 C9 N2 107.3(2) . . ?
C8 C9 C11 130.5(3) . . ?
N2 C9 C11 122.2(3) . . ?
O1 C10 C1 125.6(3) . . ?
O1 C10 H10 117.2 . . ?
C1 C10 H10 117.2 . . ?
O2 C11 C9 125.0(3) . . ?
O2 C11 H11 117.5 . . ?
C9 C11 H11 117.5 . . ?
C5 C12 H12A 109.5 . . ?
C5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C17 107.2(2) . . ?
C14 C13 C5 126.3(2) . . ?
C17 C13 C5 126.1(2) . . ?
C14 C13 Fe1 69.22(14) . . ?
C17 C13 Fe1 69.37(14) . . ?
C5 C13 Fe1 131.75(17) . . ?
C15 C14 C13 108.4(2) . . ?
C15 C14 Fe1 69.68(14) . . ?
C13 C14 Fe1 70.40(14) . . ?
C15 C14 H14 125.8 . . ?
C13 C14 H14 125.8 . . ?
Fe1 C14 H14 125.7 . . ?
C16 C15 C14 107.9(2) . . ?
C16 C15 Fe1 69.75(15) . . ?
C14 C15 Fe1 69.82(15) . . ?
C16 C15 H15 126.0 . . ?
C14 C15 H15 126.0 . . ?
Fe1 C15 H15 126.0 . . ?
C15 C16 C17 108.2(2) . . ?
C15 C16 Fe1 69.94(15) . . ?
C17 C16 Fe1 70.15(14) . . ?
C15 C16 H16 125.9 . . ?
C17 C16 H16 125.9 . . ?
Fe1 C16 H16 125.6 . . ?
C16 C17 C13 108.3(2) . . ?
C16 C17 Fe1 69.47(15) . . ?
C13 C17 Fe1 70.20(15) . . ?
C16 C17 H17 125.9 . . ?
C13 C17 H17 125.9 . . ?
Fe1 C17 H17 126.0 . . ?
N3 C18 C19 107.3(2) . . ?
N3 C18 C27 123.0(3) . . ?
C19 C18 C27 129.6(3) . . ?
C18 C19 C20 107.8(2) . . ?
C18 C19 H19 126.1 . . ?
C20 C19 H19 126.1 . . ?
C21 C20 C19 107.7(2) . . ?
C21 C20 H20 126.2 . . ?
C19 C20 H20 126.2 . . ?
N3 C21 C20 107.7(2) . . ?
N3 C21 C22 122.1(2) . . ?
C20 C21 C22 129.8(2) . . ?
C23 C22 C30 110.3(2) . . ?
C23 C22 C21 111.1(2) . . ?
C30 C22 C21 108.8(2) . . ?
C23 C22 C29 108.9(2) . . ?
C30 C22 C29 111.2(2) . . ?
C21 C22 C29 106.5(2) . . ?
N4 C23 C24 107.3(2) . . ?
N4 C23 C22 123.1(2) . . ?
C24 C23 C22 129.7(2) . . ?
C23 C24 C25 108.5(2) . . ?
C23 C24 H24 125.7 . . ?
C25 C24 H24 125.7 . . ?
C26 C25 C24 107.5(2) . . ?
C26 C25 H25 126.3 . . ?
C24 C25 H25 126.3 . . ?
N4 C26 C25 107.1(2) . . ?
N4 C26 C28 122.4(2) . . ?
C25 C26 C28 130.1(2) . . ?
O3 C27 C18 125.7(3) . . ?
O3 C27 H27 117.1 . . ?
C18 C27 H27 117.1 . . ?
O4 C28 C26 125.4(3) . . ?
O4 C28 H28 117.3 . . ?
C26 C28 H28 117.3 . . ?
C22 C29 H29A 109.5 . . ?
C22 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C22 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C34 C30 C31 107.4(2) . . ?
C34 C30 C22 126.1(2) . . ?
C31 C30 C22 126.3(2) . . ?
C34 C30 Fe1 69.84(14) . . ?
C31 C30 Fe1 69.34(14) . . ?
C22 C30 Fe1 129.43(17) . . ?
C32 C31 C30 108.0(2) . . ?
C32 C31 Fe1 68.95(14) . . ?
C30 C31 Fe1 70.00(14) . . ?
C32 C31 H31 126.0 . . ?
C30 C31 H31 126.0 . . ?
Fe1 C31 H31 126.6 . . ?
C33 C32 C31 108.3(2) . . ?
C33 C32 Fe1 70.09(15) . . ?
C31 C32 Fe1 70.49(15) . . ?
C33 C32 H32 125.9 . . ?
C31 C32 H32 125.9 . . ?
Fe1 C32 H32 125.1 . . ?
C32 C33 C34 107.8(2) . . ?
C32 C33 Fe1 69.26(15) . . ?
C34 C33 Fe1 70.42(15) . . ?
C32 C33 H33 126.1 . . ?
C34 C33 H33 126.1 . . ?
Fe1 C33 H33 125.8 . . ?
C30 C34 C33 108.6(2) . . ?
C30 C34 Fe1 69.95(14) . . ?
C33 C34 Fe1 69.16(14) . . ?
C30 C34 H34 125.7 . . ?
C33 C34 H34 125.7 . . ?
Fe1 C34 H34 126.7 . . ?
O5 C35 N5 126.2(3) . . ?
O5 C35 H35 116.9 . . ?
N5 C35 H35 116.9 . . ?
N5 C36 H36A 109.5 . . ?
N5 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N5 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N5 C37 H37A 109.5 . . ?
N5 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N5 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O6 C38 N6 124.6(3) . . ?
O6 C38 H38 117.7 . . ?
N6 C38 H38 117.7 . . ?
N6 C39 H39A 109.5 . . ?
N6 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N6 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C40 H40A 109.5 . . ?
N6 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N6 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C4 N1 C1 109.6(2) . . ?
C4 N1 H1N 126(2) . . ?
C1 N1 H1N 124(2) . . ?
C6 N2 C9 109.6(2) . . ?
C6 N2 H2N 124.9(17) . . ?
C9 N2 H2N 125.2(17) . . ?
C21 N3 C18 109.5(2) . . ?
C21 N3 H3N 127.0(18) . . ?
C18 N3 H3N 123.0(18) . . ?
C23 N4 C26 109.6(2) . . ?
C23 N4 H4N 124.3(19) . . ?
C26 N4 H4N 125.8(19) . . ?
C35 N5 C36 120.8(2) . . ?
C35 N5 C37 122.2(3) . . ?
C36 N5 C37 117.0(3) . . ?
C38 N6 C39 121.6(3) . . ?
C38 N6 C40 122.3(3) . . ?
C39 N6 C40 116.1(3) . . ?
C32 Fe1 C16 167.18(11) . . ?
C32 Fe1 C33 40.65(10) . . ?
C16 Fe1 C33 129.08(11) . . ?
C32 Fe1 C15 128.48(11) . . ?
C16 Fe1 C15 40.30(11) . . ?
C33 Fe1 C15 105.83(11) . . ?
C32 Fe1 C14 107.27(11) . . ?
C16 Fe1 C14 67.90(11) . . ?
C33 Fe1 C14 113.79(11) . . ?
C15 Fe1 C14 40.50(10) . . ?
C32 Fe1 C17 150.34(10) . . ?
C16 Fe1 C17 40.38(10) . . ?
C33 Fe1 C17 168.95(10) . . ?
C15 Fe1 C17 67.83(11) . . ?
C14 Fe1 C17 67.79(11) . . ?
C32 Fe1 C31 40.55(10) . . ?
C16 Fe1 C31 151.17(11) . . ?
C33 Fe1 C31 68.15(10) . . ?
C15 Fe1 C31 168.27(11) . . ?
C14 Fe1 C31 131.38(10) . . ?
C17 Fe1 C31 119.72(10) . . ?
C32 Fe1 C34 68.03(10) . . ?
C16 Fe1 C34 108.91(10) . . ?
C33 Fe1 C34 40.41(10) . . ?
C15 Fe1 C34 114.70(10) . . ?
C14 Fe1 C34 146.22(10) . . ?
C17 Fe1 C34 132.70(10) . . ?
C31 Fe1 C34 67.79(10) . . ?
C32 Fe1 C30 68.40(10) . . ?
C16 Fe1 C30 117.92(10) . . ?
C33 Fe1 C30 68.18(10) . . ?
C15 Fe1 C30 147.97(10) . . ?
C14 Fe1 C30 171.42(10) . . ?
C17 Fe1 C30 112.01(10) . . ?
C31 Fe1 C30 40.66(9) . . ?
C34 Fe1 C30 40.21(9) . . ?
C32 Fe1 C13 116.59(10) . . ?
C16 Fe1 C13 68.05(10) . . ?
C33 Fe1 C13 147.14(10) . . ?
C15 Fe1 C13 68.07(10) . . ?
C14 Fe1 C13 40.38(10) . . ?
C17 Fe1 C13 40.42(10) . . ?
C31 Fe1 C13 111.11(10) . . ?
C34 Fe1 C13 172.14(10) . . ?
C30 Fe1 C13 133.98(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.5(3) . . . . ?
C10 C1 C2 C3 -174.0(3) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
C2 C3 C4 N1 1.3(3) . . . . ?
C2 C3 C4 C5 -178.2(2) . . . . ?
N1 C4 C5 C6 32.4(3) . . . . ?
C3 C4 C5 C6 -148.2(3) . . . . ?
N1 C4 C5 C13 -87.2(3) . . . . ?
C3 C4 C5 C13 92.2(3) . . . . ?
N1 C4 C5 C12 149.8(2) . . . . ?
C3 C4 C5 C12 -30.8(4) . . . . ?
C4 C5 C6 N2 44.0(3) . . . . ?
C13 C5 C6 N2 164.5(2) . . . . ?
C12 C5 C6 N2 -74.8(3) . . . . ?
C4 C5 C6 C7 -139.6(3) . . . . ?
C13 C5 C6 C7 -19.1(4) . . . . ?
C12 C5 C6 C7 101.5(3) . . . . ?
N2 C6 C7 C8 -0.5(3) . . . . ?
C5 C6 C7 C8 -177.2(3) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C7 C8 C9 N2 -0.3(3) . . . . ?
C7 C8 C9 C11 -177.8(3) . . . . ?
N1 C1 C10 O1 -4.4(4) . . . . ?
C2 C1 C10 O1 169.3(3) . . . . ?
C8 C9 C11 O2 175.9(3) . . . . ?
N2 C9 C11 O2 -1.3(4) . . . . ?
C4 C5 C13 C14 27.7(3) . . . . ?
C6 C5 C13 C14 -92.9(3) . . . . ?
C12 C5 C13 C14 149.3(2) . . . . ?
C4 C5 C13 C17 -159.9(2) . . . . ?
C6 C5 C13 C17 79.5(3) . . . . ?
C12 C5 C13 C17 -38.3(3) . . . . ?
C4 C5 C13 Fe1 -66.0(3) . . . . ?
C6 C5 C13 Fe1 173.35(18) . . . . ?
C12 C5 C13 Fe1 55.5(3) . . . . ?
C17 C13 C14 C15 -0.3(3) . . . . ?
C5 C13 C14 C15 173.2(2) . . . . ?
Fe1 C13 C14 C15 -59.54(18) . . . . ?
C17 C13 C14 Fe1 59.21(17) . . . . ?
C5 C13 C14 Fe1 -127.2(2) . . . . ?
C13 C14 C15 C16 0.4(3) . . . . ?
Fe1 C14 C15 C16 -59.59(18) . . . . ?
C13 C14 C15 Fe1 59.99(18) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
Fe1 C15 C16 C17 -59.95(17) . . . . ?
C14 C15 C16 Fe1 59.63(18) . . . . ?
C15 C16 C17 C13 0.1(3) . . . . ?
Fe1 C16 C17 C13 -59.70(17) . . . . ?
C15 C16 C17 Fe1 59.82(18) . . . . ?
C14 C13 C17 C16 0.1(3) . . . . ?
C5 C13 C17 C16 -173.4(2) . . . . ?
Fe1 C13 C17 C16 59.25(17) . . . . ?
C14 C13 C17 Fe1 -59.12(17) . . . . ?
C5 C13 C17 Fe1 127.3(2) . . . . ?
N3 C18 C19 C20 -0.3(3) . . . . ?
C27 C18 C19 C20 -176.9(3) . . . . ?
C18 C19 C20 C21 0.1(3) . . . . ?
C19 C20 C21 N3 0.1(3) . . . . ?
C19 C20 C21 C22 -172.6(2) . . . . ?
N3 C21 C22 C23 39.7(3) . . . . ?
C20 C21 C22 C23 -148.4(3) . . . . ?
N3 C21 C22 C30 161.4(2) . . . . ?
C20 C21 C22 C30 -26.8(4) . . . . ?
N3 C21 C22 C29 -78.7(3) . . . . ?
C20 C21 C22 C29 93.1(3) . . . . ?
C30 C22 C23 N4 -87.5(3) . . . . ?
C21 C22 C23 N4 33.2(3) . . . . ?
C29 C22 C23 N4 150.2(2) . . . . ?
C30 C22 C23 C24 93.8(3) . . . . ?
C21 C22 C23 C24 -145.4(3) . . . . ?
C29 C22 C23 C24 -28.5(4) . . . . ?
N4 C23 C24 C25 0.0(3) . . . . ?
C22 C23 C24 C25 178.9(2) . . . . ?
C23 C24 C25 C26 -0.2(3) . . . . ?
C24 C25 C26 N4 0.3(3) . . . . ?
C24 C25 C26 C28 -172.9(3) . . . . ?
N3 C18 C27 O3 -0.9(4) . . . . ?
C19 C18 C27 O3 175.2(3) . . . . ?
N4 C26 C28 O4 -1.7(4) . . . . ?
C25 C26 C28 O4 170.6(3) . . . . ?
C23 C22 C30 C34 28.9(3) . . . . ?
C21 C22 C30 C34 -93.3(3) . . . . ?
C29 C22 C30 C34 149.8(2) . . . . ?
C23 C22 C30 C31 -156.1(2) . . . . ?
C21 C22 C30 C31 81.8(3) . . . . ?
C29 C22 C30 C31 -35.1(3) . . . . ?
C23 C22 C30 Fe1 -63.9(3) . . . . ?
C21 C22 C30 Fe1 173.94(17) . . . . ?
C29 C22 C30 Fe1 57.0(3) . . . . ?
C34 C30 C31 C32 -1.1(3) . . . . ?
C22 C30 C31 C32 -176.9(2) . . . . ?
Fe1 C30 C31 C32 58.68(17) . . . . ?
C34 C30 C31 Fe1 -59.74(16) . . . . ?
C22 C30 C31 Fe1 124.4(2) . . . . ?
C30 C31 C32 C33 0.8(3) . . . . ?
Fe1 C31 C32 C33 60.17(18) . . . . ?
C30 C31 C32 Fe1 -59.34(17) . . . . ?
C31 C32 C33 C34 -0.3(3) . . . . ?
Fe1 C32 C33 C34 60.13(18) . . . . ?
C31 C32 C33 Fe1 -60.42(18) . . . . ?
C31 C30 C34 C33 0.9(3) . . . . ?
C22 C30 C34 C33 176.7(2) . . . . ?
Fe1 C30 C34 C33 -58.54(17) . . . . ?
C31 C30 C34 Fe1 59.42(16) . . . . ?
C22 C30 C34 Fe1 -124.7(2) . . . . ?
C32 C33 C34 C30 -0.4(3) . . . . ?
Fe1 C33 C34 C30 59.02(17) . . . . ?
C32 C33 C34 Fe1 -59.40(17) . . . . ?
C3 C4 N1 C1 -1.0(3) . . . . ?
C5 C4 N1 C1 178.5(2) . . . . ?
C2 C1 N1 C4 0.3(3) . . . . ?
C10 C1 N1 C4 175.2(2) . . . . ?
C7 C6 N2 C9 0.3(3) . . . . ?
C5 C6 N2 C9 177.4(2) . . . . ?
C8 C9 N2 C6 0.0(3) . . . . ?
C11 C9 N2 C6 177.8(2) . . . . ?
C20 C21 N3 C18 -0.3(3) . . . . ?
C22 C21 N3 C18 173.1(2) . . . . ?
C19 C18 N3 C21 0.3(3) . . . . ?
C27 C18 N3 C21 177.2(2) . . . . ?
C24 C23 N4 C26 0.2(3) . . . . ?
C22 C23 N4 C26 -178.8(2) . . . . ?
C25 C26 N4 C23 -0.3(3) . . . . ?
C28 C26 N4 C23 173.6(2) . . . . ?
O5 C35 N5 C36 0.3(5) . . . . ?
O5 C35 N5 C37 179.6(3) . . . . ?
O6 C38 N6 C39 1.5(5) . . . . ?
O6 C38 N6 C40 -178.8(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
N1 H1N O4 0.87(3) 2.04(3) 2.901(3) 168(3) 1_455
N2 H2N O3 0.87(3) 2.02(3) 2.875(3) 167(2) 1_455
N3 H3N O2 0.88(3) 2.05(3) 2.892(3) 161(3) 1_655
N4 H4N O1 0.89(3) 2.02(3) 2.897(3) 168(3) 1_655

_refine_diff_density_max         0.382
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1444558'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: These reflections were probably omitted due to the overlap with 
the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H36 N6 O6, 2 C H Cl3'
_chemical_formula_sum            'C44 H38 Cl6 N6 O6'
_chemical_formula_weight         959.50

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1932(19)
_cell_length_b                   12.318(2)
_cell_length_c                   19.654(4)
_cell_angle_alpha                72.773(4)
_cell_angle_beta                 77.793(4)
_cell_angle_gamma                81.490(4)
_cell_volume                     2294.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10438
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prisms
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.428
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Rigaku SCX-Mini with Mercury 2+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23595
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.059
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10438
_reflns_number_gt                6357
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;




_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'





_refine_special_details          
;
 A molecule of chloroform was disordered.  The disorder resulted in 
two principal conformations.  The disorder was modeled by assigning 
the variable x to the site occupancy for one component and (1-x) to 
the site occupancy of the alternate component.  The variable x was 
refined while restraining the geometry of the two components to be 
equivalent.  A common isotropic displacement parameter was refined 
while refining x.  In this way, the major component of the disordered 
solvent molecule consisting of atoms, Cl4, Cl5, Cl6 and C1b refined 
to a site occupancy of 53(1)%.  The non-H atoms of both components 
were ultimately refined anisotropically with their displacement 
parameters restrained to be approximately isotropic.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0860P)²+3.5129P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10438
_refine_ls_number_parameters     600
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0937
_refine_ls_wR_factor_ref         0.2589
_refine_ls_wR_factor_gt          0.2330
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.165
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6718(4) 0.9507(3) 0.6047(2) 0.0303(9) Uani 1 1 d . . . . .
C2 C 0.6002(5) 0.8925(4) 0.5771(2) 0.0393(11) Uani 1 1 d . . . . .
H2 H 0.5754 0.9172 0.5306 0.047 Uiso 1 1 calc R U . . .
C3 C 0.5704(5) 0.7905(4) 0.6299(2) 0.0347(10) Uani 1 1 d . . . . .
H3 H 0.5216 0.7334 0.6259 0.042 Uiso 1 1 calc R U . . .
C4 C 0.6251(4) 0.7881(3) 0.6891(2) 0.0230(8) Uani 1 1 d . . . . .
C5 C 0.6318(4) 0.6971(3) 0.76044(19) 0.0211(8) Uani 1 1 d . . . . .
C6 C 0.5722(4) 0.7511(3) 0.82149(19) 0.0219(8) Uani 1 1 d . . . . .
C7 C 0.4891(4) 0.8507(3) 0.8210(2) 0.0255(8) Uani 1 1 d . . . . .
H7 H 0.4509 0.8991 0.7812 0.031 Uiso 1 1 calc R U . . .
C8 C 0.4716(4) 0.8670(3) 0.8893(2) 0.0290(9) Uani 1 1 d . . . . .
H8 H 0.4200 0.9291 0.9046 0.035 Uiso 1 1 calc R U . . .
C9 C 0.5429(4) 0.7764(3) 0.9314(2) 0.0270(9) Uani 1 1 d . . . . .
C10 C 0.5547(4) 0.5977(3) 0.76206(19) 0.0207(8) Uani 1 1 d . . . . .
C11 C 0.4173(4) 0.5961(3) 0.78940(19) 0.0201(8) Uani 1 1 d . . . . .
H11 H 0.3708 0.6552 0.8097 0.024 Uiso 1 1 calc R U . . .
C12 C 0.3474(4) 0.5085(3) 0.78725(18) 0.0208(8) Uani 1 1 d . . . . .
C13 C 0.4160(4) 0.4220(3) 0.75817(19) 0.0208(8) Uani 1 1 d . . . . .
H13 H 0.3688 0.3620 0.7568 0.025 Uiso 1 1 calc R U . . .
C14 C 0.5543(4) 0.4224(3) 0.73091(19) 0.0202(8) Uani 1 1 d . . . . .
C15 C 0.6213(4) 0.5104(3) 0.73364(19) 0.0212(8) Uani 1 1 d . . . . .
H15 H 0.7153 0.5108 0.7155 0.025 Uiso 1 1 calc R U . . .
C16 C 0.1377(4) 0.6012(3) 0.9777(2) 0.0288(9) Uani 1 1 d . . . . .
C17 C 0.0436(4) 0.6787(4) 0.9434(2) 0.0330(10) Uani 1 1 d . . . . .
H17 H -0.0143 0.7348 0.9623 0.040 Uiso 1 1 calc R U . . .
C18 C 0.0482(4) 0.6605(4) 0.8767(2) 0.0317(9) Uani 1 1 d . . . . .
H18 H -0.0052 0.7022 0.8416 0.038 Uiso 1 1 calc R U . . .
C19 C 0.1447(4) 0.5704(3) 0.8704(2) 0.0242(8) Uani 1 1 d . . . . .
C20 C 0.1925(4) 0.5172(3) 0.8080(2) 0.0235(8) Uani 1 1 d . . . . .
C21 C 0.1388(4) 0.4016(3) 0.8261(2) 0.0251(8) Uani 1 1 d . . . . .
C22 C 0.0479(4) 0.3684(4) 0.7940(3) 0.0367(10) Uani 1 1 d . . . . .
H22 H 0.0047 0.4152 0.7557 0.044 Uiso 1 1 calc R U . . .
C23 C 0.0318(5) 0.2539(4) 0.8286(3) 0.0417(11) Uani 1 1 d . . . . .
H23 H -0.0244 0.2082 0.8180 0.050 Uiso 1 1 calc R U . . .
C24 C 0.1127(5) 0.2181(4) 0.8814(2) 0.0362(10) Uani 1 1 d . . . . .
C25 C 0.7562(4) 0.0545(3) 0.8209(2) 0.0264(9) Uani 1 1 d . . . . .
C26 C 0.7101(4) 0.1143(3) 0.8726(2) 0.0302(9) Uani 1 1 d . . . . .
H26 H 0.7153 0.0869 0.9225 0.036 Uiso 1 1 calc R U . . .
C27 C 0.6546(4) 0.2220(3) 0.8377(2) 0.0289(9) Uani 1 1 d . . . . .
H27 H 0.6156 0.2813 0.8595 0.035 Uiso 1 1 calc R U . . .
C28 C 0.6668(4) 0.2267(3) 0.7651(2) 0.0239(8) Uani 1 1 d . . . . .
C29 C 0.6297(4) 0.3233(3) 0.70190(19) 0.0224(8) Uani 1 1 d . . . . .
C30 C 0.5396(4) 0.2838(3) 0.66341(19) 0.0231(8) Uani 1 1 d . . . . .
C31 C 0.4718(4) 0.1863(4) 0.6844(2) 0.0323(10) Uani 1 1 d . . . . .
H31 H 0.4744 0.1261 0.7276 0.039 Uiso 1 1 calc R U . . .
C32 C 0.3993(5) 0.1930(4) 0.6306(2) 0.0359(10) Uani 1 1 d . . . . .
H32 H 0.3439 0.1376 0.6302 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4224(4) 0.2953(3) 0.5775(2) 0.0310(9) Uani 1 1 d . . . . .
C34 C 0.7267(5) 1.0592(4) 0.5744(2) 0.0365(10) Uani 1 1 d . . . . .
H34 H 0.7141 1.1002 0.5267 0.044 Uiso 1 1 calc R U . . .
C35 C 0.5655(4) 0.7591(4) 1.0029(2) 0.0310(9) Uani 1 1 d . . . . .
H35 H 0.5249 0.8156 1.0268 0.037 Uiso 1 1 calc R U . . .
C36 C 0.7820(4) 0.6570(3) 0.7636(2) 0.0237(8) Uani 1 1 d . . . . .
H36A H 0.8260 0.7179 0.7700 0.035 Uiso 1 1 calc R U . . .
H36B H 0.8262 0.6388 0.7185 0.035 Uiso 1 1 calc R U . . .
H36C H 0.7889 0.5889 0.8044 0.035 Uiso 1 1 calc R U . . .
C37 C 0.1766(5) 0.5880(4) 1.0454(2) 0.0339(10) Uani 1 1 d . . . . .
H37 H 0.1301 0.6380 1.0731 0.041 Uiso 1 1 calc R U . . .
C38 C 0.1316(6) 0.1085(4) 0.9316(3) 0.0484(13) Uani 1 1 d . . . . .
H38 H 0.0836 0.0493 0.9296 0.058 Uiso 1 1 calc R U . . .
C39 C 0.1405(4) 0.5965(4) 0.7407(2) 0.0294(9) Uani 1 1 d . . . . .
H39A H 0.1717 0.5634 0.6998 0.044 Uiso 1 1 calc R U . . .
H39B H 0.1749 0.6713 0.7287 0.044 Uiso 1 1 calc R U . . .
H39C H 0.0417 0.6054 0.7506 0.044 Uiso 1 1 calc R U . . .
C40 C 0.8180(4) -0.0582(3) 0.8275(2) 0.0281(9) Uani 1 1 d . . . . .
H40 H 0.8356 -0.1021 0.8739 0.034 Uiso 1 1 calc R U . . .
C41 C 0.7626(4) 0.3576(3) 0.6488(2) 0.0255(8) Uani 1 1 d . . . . .
H41A H 0.8256 0.3743 0.6750 0.038 Uiso 1 1 calc R U . . .
H41B H 0.7430 0.4255 0.6099 0.038 Uiso 1 1 calc R U . . .
H41C H 0.8030 0.2946 0.6280 0.038 Uiso 1 1 calc R U . . .
C42 C 0.3729(5) 0.3398(4) 0.5115(2) 0.0387(11) Uani 1 1 d . . . . .
H42 H 0.3122 0.2965 0.5022 0.046 Uiso 1 1 calc R U . . .
N1 N 0.6872(3) 0.8846(3) 0.67311(17) 0.0249(7) Uani 1 1 d . . . . .
H1 H 0.7308 0.9023 0.7019 0.030 Uiso 1 1 calc R U . . .
N2 N 0.6029(3) 0.7059(3) 0.88839(16) 0.0236(7) Uani 1 1 d . . . . .
H2A H 0.6532 0.6416 0.9023 0.028 Uiso 1 1 calc R U . . .
N3 N 0.1981(3) 0.5349(3) 0.93219(16) 0.0249(7) Uani 1 1 d . . . . .
H3A H 0.2614 0.4785 0.9415 0.030 Uiso 1 1 calc R U . . .
N4 N 0.1765(3) 0.3112(3) 0.87813(17) 0.0284(8) Uani 1 1 d . . . . .
H4 H 0.2335 0.3113 0.9061 0.034 Uiso 1 1 calc R U . . .
N5 N 0.7290(3) 0.1256(3) 0.75585(17) 0.0244(7) Uani 1 1 d . . . . .
H5 H 0.7491 0.1080 0.7144 0.029 Uiso 1 1 calc R U . . .
N6 N 0.5081(3) 0.3483(3) 0.59961(17) 0.0261(7) Uani 1 1 d . . . . .
H6 H 0.5383 0.4149 0.5756 0.031 Uiso 1 1 calc R U . . .
O1 O 0.7878(3) 1.1029(3) 0.60445(16) 0.0412(8) Uani 1 1 d . . . . .
O2 O 0.6330(3) 0.6774(2) 1.03665(15) 0.0357(7) Uani 1 1 d . . . . .
O3 O 0.2644(3) 0.5181(2) 1.07152(15) 0.0384(8) Uani 1 1 d . . . . .
O4 O 0.2043(5) 0.0852(3) 0.9766(2) 0.0693(13) Uani 1 1 d . . . . .
O5 O 0.8505(3) -0.1030(2) 0.77757(16) 0.0334(7) Uani 1 1 d . . . . .
O6 O 0.4006(4) 0.4285(3) 0.46540(17) 0.0459(9) Uani 1 1 d . . . . .
Cl1 Cl 0.75811(19) 1.34516(15) 0.45276(8) 0.0812(6) Uani 1 1 d D . . . .
Cl2 Cl 0.99111(19) 1.19751(16) 0.41490(9) 0.0809(5) Uani 1 1 d D . . . .
Cl3 Cl 1.0229(3) 1.4006(2) 0.44586(15) 0.1369(11) Uani 1 1 d D . . . .
C43 C 0.9199(6) 1.2904(5) 0.4661(3) 0.0631(16) Uani 1 1 d D . . . .
H43 H 0.9159 1.2479 0.5184 0.076 Uiso 1 1 calc R U . . .
Cl4 Cl 0.1411(3) 1.0667(3) 0.56836(16) 0.0763(9) Uani 0.53 1 d D U P A 1
Cl5 Cl 0.0717(4) 1.1255(4) 0.6985(3) 0.1251(19) Uani 0.53 1 d D U P A 1
Cl6 Cl 0.2217(6) 0.9139(3) 0.6951(3) 0.139(3) Uani 0.53 1 d D U P A 1
C1B C 0.0936(9) 1.0150(7) 0.6597(4) 0.058(3) Uani 0.53 1 d D U P A 1
H1B H 0.0075 0.9783 0.6706 0.070 Uiso 0.53 1 calc R U P A 1
Cl7 Cl 0.1498(4) 1.0011(4) 0.7710(3) 0.1069(15) Uani 0.47 1 d D U P B 2
Cl8 Cl 0.2764(5) 0.9073(4) 0.6553(3) 0.115(2) Uani 0.47 1 d D U P B 2
Cl9 Cl 0.0653(6) 1.0796(8) 0.6360(3) 0.189(4) Uani 0.47 1 d D U P B 2
C1C C 0.1252(12) 0.9574(10) 0.6987(5) 0.114(7) Uani 0.47 1 d D U P B 2
H1C H 0.0594 0.8981 0.7152 0.136 Uiso 0.47 1 calc R U P B 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
C1 C2 1.377(6) . ?
C1 N1 1.377(5) . ?
C1 C34 1.436(6) . ?
C2 C3 1.397(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.352(5) . ?
C4 C5 1.522(5) . ?
C5 C6 1.516(5) . ?
C5 C10 1.539(5) . ?
C5 C36 1.545(5) . ?
C6 N2 1.351(5) . ?
C6 C7 1.383(5) . ?
C7 C8 1.386(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(6) . ?
C8 H8 0.9500 . ?
C9 N2 1.380(5) . ?
C9 C35 1.419(5) . ?
C10 C15 1.381(5) . ?
C10 C11 1.391(5) . ?
C11 C12 1.393(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(5) . ?
C12 C20 1.540(5) . ?
C13 C14 1.398(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(5) . ?
C14 C29 1.535(5) . ?
C15 H15 0.9500 . ?
C16 N3 1.377(5) . ?
C16 C17 1.381(6) . ?
C16 C37 1.425(6) . ?
C17 C18 1.385(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(6) . ?
C18 H18 0.9500 . ?
C19 N3 1.364(5) . ?
C19 C20 1.517(5) . ?
C20 C21 1.517(5) . ?
C20 C39 1.537(5) . ?
C21 N4 1.341(5) . ?
C21 C22 1.391(6) . ?
C22 C23 1.389(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(7) . ?
C23 H23 0.9500 . ?
C24 N4 1.380(5) . ?
C24 C38 1.431(7) . ?
C25 N5 1.376(5) . ?
C25 C26 1.391(6) . ?
C25 C40 1.417(6) . ?
C26 C27 1.398(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(5) . ?
C27 H27 0.9500 . ?
C28 N5 1.355(5) . ?
C28 C29 1.513(5) . ?
C29 C30 1.515(5) . ?
C29 C41 1.553(5) . ?
C30 N6 1.346(5) . ?
C30 C31 1.386(5) . ?
C31 C32 1.391(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(6) . ?
C32 H32 0.9500 . ?
C33 N6 1.370(5) . ?
C33 C42 1.419(6) . ?
C34 O1 1.212(5) . ?
C34 H34 0.9500 . ?
C35 O2 1.233(5) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 O3 1.229(5) . ?
C37 H37 0.9500 . ?
C38 O4 1.215(6) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 O5 1.228(5) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O6 1.221(5) . ?
C42 H42 0.9500 . ?
N1 H1 0.8800 . ?
N2 H2A 0.8800 . ?
N3 H3A 0.8800 . ?
N4 H4 0.8800 . ?
N5 H5 0.8800 . ?
N6 H6 0.8800 . ?
Cl1 C43 1.730(6) . ?
Cl2 C43 1.725(6) . ?
Cl3 C43 1.740(6) . ?
C43 H43 1.0000 . ?
Cl4 C1B 1.705(8) . ?
Cl5 C1B 1.713(8) . ?
Cl6 C1B 1.769(9) . ?
C1B H1B 1.0000 . ?
Cl7 C1C 1.736(10) . ?
Cl8 C1C 1.720(10) . ?
Cl9 C1C 1.763(10) . ?
C1C H1C 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 107.4(3) . . ?
C2 C1 C34 131.4(4) . . ?
N1 C1 C34 121.2(4) . . ?
C1 C2 C3 107.7(4) . . ?
C1 C2 H2 126.2 . . ?
C3 C2 H2 126.2 . . ?
C4 C3 C2 107.4(4) . . ?
C4 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
N1 C4 C3 108.0(3) . . ?
N1 C4 C5 120.4(3) . . ?
C3 C4 C5 131.4(3) . . ?
C6 C5 C4 108.1(3) . . ?
C6 C5 C10 112.7(3) . . ?
C4 C5 C10 108.2(3) . . ?
C6 C5 C36 109.2(3) . . ?
C4 C5 C36 107.7(3) . . ?
C10 C5 C36 110.8(3) . . ?
N2 C6 C7 108.5(3) . . ?
N2 C6 C5 121.4(3) . . ?
C7 C6 C5 130.0(3) . . ?
C6 C7 C8 107.4(3) . . ?
C6 C7 H7 126.3 . . ?
C8 C7 H7 126.3 . . ?
C7 C8 C9 107.9(4) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 H8 126.1 . . ?
N2 C9 C8 107.1(3) . . ?
N2 C9 C35 123.4(4) . . ?
C8 C9 C35 129.2(4) . . ?
C15 C10 C11 119.1(3) . . ?
C15 C10 C5 119.8(3) . . ?
C11 C10 C5 121.0(3) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C13 C12 C11 119.5(3) . . ?
C13 C12 C20 120.6(3) . . ?
C11 C12 C20 119.4(3) . . ?
C12 C13 C14 120.5(3) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 C29 121.3(3) . . ?
C13 C14 C29 119.8(3) . . ?
C10 C15 C14 121.6(3) . . ?
C10 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
N3 C16 C17 107.2(3) . . ?
N3 C16 C37 122.6(4) . . ?
C17 C16 C37 130.2(4) . . ?
C16 C17 C18 108.1(4) . . ?
C16 C17 H17 125.9 . . ?
C18 C17 H17 125.9 . . ?
C17 C18 C19 107.7(4) . . ?
C17 C18 H18 126.2 . . ?
C19 C18 H18 126.2 . . ?
N3 C19 C18 107.6(3) . . ?
N3 C19 C20 122.6(3) . . ?
C18 C19 C20 129.7(3) . . ?
C19 C20 C21 110.5(3) . . ?
C19 C20 C39 108.7(3) . . ?
C21 C20 C39 109.2(3) . . ?
C19 C20 C12 111.2(3) . . ?
C21 C20 C12 111.5(3) . . ?
C39 C20 C12 105.6(3) . . ?
N4 C21 C22 108.2(4) . . ?
N4 C21 C20 123.1(3) . . ?
C22 C21 C20 128.7(4) . . ?
C23 C22 C21 107.3(4) . . ?
C23 C22 H22 126.4 . . ?
C21 C22 H22 126.4 . . ?
C22 C23 C24 107.8(4) . . ?
C22 C23 H23 126.1 . . ?
C24 C23 H23 126.1 . . ?
N4 C24 C23 106.8(4) . . ?
N4 C24 C38 123.4(4) . . ?
C23 C24 C38 129.8(4) . . ?
N5 C25 C26 107.0(3) . . ?
N5 C25 C40 122.2(4) . . ?
C26 C25 C40 130.8(4) . . ?
C25 C26 C27 107.6(3) . . ?
C25 C26 H26 126.2 . . ?
C27 C26 H26 126.2 . . ?
C28 C27 C26 107.5(4) . . ?
C28 C27 H27 126.3 . . ?
C26 C27 H27 126.3 . . ?
N5 C28 C27 107.8(3) . . ?
N5 C28 C29 121.6(3) . . ?
C27 C28 C29 130.5(4) . . ?
C28 C29 C30 110.0(3) . . ?
C28 C29 C14 108.6(3) . . ?
C30 C29 C14 109.4(3) . . ?
C28 C29 C41 107.5(3) . . ?
C30 C29 C41 109.2(3) . . ?
C14 C29 C41 112.1(3) . . ?
N6 C30 C31 108.0(3) . . ?
N6 C30 C29 121.7(3) . . ?
C31 C30 C29 130.3(3) . . ?
C30 C31 C32 107.3(4) . . ?
C30 C31 H31 126.3 . . ?
C32 C31 H31 126.3 . . ?
C31 C32 C33 107.7(4) . . ?
C31 C32 H32 126.1 . . ?
C33 C32 H32 126.1 . . ?
N6 C33 C32 106.7(4) . . ?
N6 C33 C42 124.2(4) . . ?
C32 C33 C42 129.1(4) . . ?
O1 C34 C1 125.6(4) . . ?
O1 C34 H34 117.2 . . ?
C1 C34 H34 117.2 . . ?
O2 C35 C9 125.8(4) . . ?
O2 C35 H35 117.1 . . ?
C9 C35 H35 117.1 . . ?
C5 C36 H36A 109.5 . . ?
C5 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C5 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O3 C37 C16 126.3(4) . . ?
O3 C37 H37 116.9 . . ?
C16 C37 H37 116.9 . . ?
O4 C38 C24 125.2(5) . . ?
O4 C38 H38 117.4 . . ?
C24 C38 H38 117.4 . . ?
C20 C39 H39A 109.5 . . ?
C20 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C20 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O5 C40 C25 124.5(4) . . ?
O5 C40 H40 117.7 . . ?
C25 C40 H40 117.7 . . ?
C29 C41 H41A 109.5 . . ?
C29 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C29 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O6 C42 C33 126.3(4) . . ?
O6 C42 H42 116.9 . . ?
C33 C42 H42 116.9 . . ?
C4 N1 C1 109.5(3) . . ?
C4 N1 H1 125.3 . . ?
C1 N1 H1 125.3 . . ?
C6 N2 C9 109.1(3) . . ?
C6 N2 H2A 125.4 . . ?
C9 N2 H2A 125.4 . . ?
C19 N3 C16 109.3(3) . . ?
C19 N3 H3A 125.3 . . ?
C16 N3 H3A 125.3 . . ?
C21 N4 C24 109.9(4) . . ?
C21 N4 H4 125.0 . . ?
C24 N4 H4 125.0 . . ?
C28 N5 C25 110.0(3) . . ?
C28 N5 H5 125.0 . . ?
C25 N5 H5 125.0 . . ?
C30 N6 C33 110.2(3) . . ?
C30 N6 H6 124.9 . . ?
C33 N6 H6 124.9 . . ?
Cl2 C43 Cl1 112.7(3) . . ?
Cl2 C43 Cl3 109.0(3) . . ?
Cl1 C43 Cl3 110.2(3) . . ?
Cl2 C43 H43 108.3 . . ?
Cl1 C43 H43 108.3 . . ?
Cl3 C43 H43 108.3 . . ?
Cl4 C1B Cl5 109.0(5) . . ?
Cl4 C1B Cl6 109.5(5) . . ?
Cl5 C1B Cl6 108.7(5) . . ?
Cl4 C1B H1B 109.9 . . ?
Cl5 C1B H1B 109.9 . . ?
Cl6 C1B H1B 109.9 . . ?
Cl8 C1C Cl7 110.3(7) . . ?
Cl8 C1C Cl9 106.6(6) . . ?
Cl7 C1C Cl9 107.1(6) . . ?
Cl8 C1C H1C 110.9 . . ?
Cl7 C1C H1C 110.9 . . ?
Cl9 C1C H1C 110.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.8(5) . . . . ?
C34 C1 C2 C3 -179.5(5) . . . . ?
C1 C2 C3 C4 -0.2(5) . . . . ?
C2 C3 C4 N1 -0.5(5) . . . . ?
C2 C3 C4 C5 -176.3(4) . . . . ?
N1 C4 C5 C6 58.8(4) . . . . ?
C3 C4 C5 C6 -125.8(5) . . . . ?
N1 C4 C5 C10 -178.9(3) . . . . ?
C3 C4 C5 C10 -3.5(6) . . . . ?
N1 C4 C5 C36 -59.0(4) . . . . ?
C3 C4 C5 C36 116.3(5) . . . . ?
C4 C5 C6 N2 -157.8(3) . . . . ?
C10 C5 C6 N2 82.7(4) . . . . ?
C36 C5 C6 N2 -40.8(4) . . . . ?
C4 C5 C6 C7 18.5(5) . . . . ?
C10 C5 C6 C7 -101.0(4) . . . . ?
C36 C5 C6 C7 135.4(4) . . . . ?
N2 C6 C7 C8 1.3(4) . . . . ?
C5 C6 C7 C8 -175.4(4) . . . . ?
C6 C7 C8 C9 -0.7(5) . . . . ?
C7 C8 C9 N2 -0.1(5) . . . . ?
C7 C8 C9 C35 174.2(4) . . . . ?
C6 C5 C10 C15 -152.1(3) . . . . ?
C4 C5 C10 C15 88.4(4) . . . . ?
C36 C5 C10 C15 -29.5(4) . . . . ?
C6 C5 C10 C11 30.2(5) . . . . ?
C4 C5 C10 C11 -89.2(4) . . . . ?
C36 C5 C10 C11 152.9(3) . . . . ?
C15 C10 C11 C12 -0.9(5) . . . . ?
C5 C10 C11 C12 176.8(3) . . . . ?
C10 C11 C12 C13 0.6(5) . . . . ?
C10 C11 C12 C20 -171.6(3) . . . . ?
C11 C12 C13 C14 -0.2(5) . . . . ?
C20 C12 C13 C14 171.8(3) . . . . ?
C12 C13 C14 C15 0.2(5) . . . . ?
C12 C13 C14 C29 177.4(3) . . . . ?
C11 C10 C15 C14 0.8(5) . . . . ?
C5 C10 C15 C14 -176.9(3) . . . . ?
C13 C14 C15 C10 -0.5(5) . . . . ?
C29 C14 C15 C10 -177.7(3) . . . . ?
N3 C16 C17 C18 -0.8(5) . . . . ?
C37 C16 C17 C18 176.8(4) . . . . ?
C16 C17 C18 C19 0.7(5) . . . . ?
C17 C18 C19 N3 -0.3(5) . . . . ?
C17 C18 C19 C20 -178.5(4) . . . . ?
N3 C19 C20 C21 75.4(4) . . . . ?
C18 C19 C20 C21 -106.6(5) . . . . ?
N3 C19 C20 C39 -164.8(3) . . . . ?
C18 C19 C20 C39 13.2(5) . . . . ?
N3 C19 C20 C12 -48.9(5) . . . . ?
C18 C19 C20 C12 129.1(4) . . . . ?
C13 C12 C20 C19 150.3(3) . . . . ?
C11 C12 C20 C19 -37.6(4) . . . . ?
C13 C12 C20 C21 26.5(5) . . . . ?
C11 C12 C20 C21 -161.4(3) . . . . ?
C13 C12 C20 C39 -91.9(4) . . . . ?
C11 C12 C20 C39 80.1(4) . . . . ?
C19 C20 C21 N4 -66.7(5) . . . . ?
C39 C20 C21 N4 173.8(3) . . . . ?
C12 C20 C21 N4 57.5(5) . . . . ?
C19 C20 C21 C22 114.3(4) . . . . ?
C39 C20 C21 C22 -5.3(6) . . . . ?
C12 C20 C21 C22 -121.6(4) . . . . ?
N4 C21 C22 C23 -0.1(5) . . . . ?
C20 C21 C22 C23 179.1(4) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C22 C23 C24 N4 0.0(5) . . . . ?
C22 C23 C24 C38 179.7(5) . . . . ?
N5 C25 C26 C27 0.2(5) . . . . ?
C40 C25 C26 C27 -178.7(4) . . . . ?
C25 C26 C27 C28 0.3(5) . . . . ?
C26 C27 C28 N5 -0.6(5) . . . . ?
C26 C27 C28 C29 -177.1(4) . . . . ?
N5 C28 C29 C30 57.2(5) . . . . ?
C27 C28 C29 C30 -126.8(4) . . . . ?
N5 C28 C29 C14 176.9(3) . . . . ?
C27 C28 C29 C14 -7.1(6) . . . . ?
N5 C28 C29 C41 -61.6(4) . . . . ?
C27 C28 C29 C41 114.4(4) . . . . ?
C15 C14 C29 C28 93.9(4) . . . . ?
C13 C14 C29 C28 -83.3(4) . . . . ?
C15 C14 C29 C30 -146.0(3) . . . . ?
C13 C14 C29 C30 36.8(4) . . . . ?
C15 C14 C29 C41 -24.7(5) . . . . ?
C13 C14 C29 C41 158.1(3) . . . . ?
C28 C29 C30 N6 -170.5(3) . . . . ?
C14 C29 C30 N6 70.3(4) . . . . ?
C41 C29 C30 N6 -52.7(5) . . . . ?
C28 C29 C30 C31 12.8(6) . . . . ?
C14 C29 C30 C31 -106.5(5) . . . . ?
C41 C29 C30 C31 130.5(4) . . . . ?
N6 C30 C31 C32 0.8(5) . . . . ?
C29 C30 C31 C32 177.9(4) . . . . ?
C30 C31 C32 C33 -0.6(5) . . . . ?
C31 C32 C33 N6 0.2(5) . . . . ?
C31 C32 C33 C42 178.9(5) . . . . ?
C2 C1 C34 O1 179.3(5) . . . . ?
N1 C1 C34 O1 -1.1(7) . . . . ?
N2 C9 C35 O2 -4.7(7) . . . . ?
C8 C9 C35 O2 -178.1(4) . . . . ?
N3 C16 C37 O3 -0.7(7) . . . . ?
C17 C16 C37 O3 -178.0(5) . . . . ?
N4 C24 C38 O4 0.3(8) . . . . ?
C23 C24 C38 O4 -179.4(5) . . . . ?
N5 C25 C40 O5 -1.3(6) . . . . ?
C26 C25 C40 O5 177.4(4) . . . . ?
N6 C33 C42 O6 1.4(8) . . . . ?
C32 C33 C42 O6 -177.0(5) . . . . ?
C3 C4 N1 C1 1.0(5) . . . . ?
C5 C4 N1 C1 177.3(3) . . . . ?
C2 C1 N1 C4 -1.1(5) . . . . ?
C34 C1 N1 C4 179.2(4) . . . . ?
C7 C6 N2 C9 -1.3(4) . . . . ?
C5 C6 N2 C9 175.7(3) . . . . ?
C8 C9 N2 C6 0.9(4) . . . . ?
C35 C9 N2 C6 -173.8(4) . . . . ?
C18 C19 N3 C16 -0.2(4) . . . . ?
C20 C19 N3 C16 178.1(3) . . . . ?
C17 C16 N3 C19 0.7(4) . . . . ?
C37 C16 N3 C19 -177.2(4) . . . . ?
C22 C21 N4 C24 0.1(5) . . . . ?
C20 C21 N4 C24 -179.1(3) . . . . ?
C23 C24 N4 C21 -0.1(5) . . . . ?
C38 C24 N4 C21 -179.8(4) . . . . ?
C27 C28 N5 C25 0.8(4) . . . . ?
C29 C28 N5 C25 177.6(3) . . . . ?
C26 C25 N5 C28 -0.6(4) . . . . ?
C40 C25 N5 C28 178.4(4) . . . . ?
C31 C30 N6 C33 -0.7(5) . . . . ?
C29 C30 N6 C33 -178.1(3) . . . . ?
C32 C33 N6 C30 0.3(5) . . . . ?
C42 C33 N6 C30 -178.5(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
N1 H1 O5 0.88 2.09 2.952(4) 164.4 1_565
N2 H2A O3 0.88 1.98 2.849(4) 167.6 2_667
N3 H3A O2 0.88 2.03 2.888(4) 164.3 2_667
N4 H4 O2 0.88 1.98 2.861(5) 175.5 2_667
N5 H5 O1 0.88 2.13 2.997(4) 167.9 1_545
N6 H6 O6 0.88 2.00 2.870(4) 171.7 2_666
C43 H43 O1 1.00 2.39 3.192(6) 136.4 .
C1B H1B O5 1.00 2.41 3.204(9) 136.3 1_465
C1C H1C O5 1.00 2.22 2.982(13) 131.8 1_465

_refine_diff_density_max         0.945
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-4



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1444559'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT051_shelx               
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      26.11 %     
RESPONSE: A molecule of dichloromethane was disordered and could not 
be adequately modeled.  It was removed by the use of Squeeze.
;
_vrf_PLAT413_shelx               
;
PROBLEM: Short Inter XH3 .. XHn     H42C   ..  H38D    ..       1.83 Ang.  
RESPONSE: There is some disorder and large displacement parameters for 
the n-butyl groups of the cation.  The result is some increased 
uncertainty in the location of the positions of the atoms involved.
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact  O6     ..  O10     ..       2.52 Ang.  
RESPONSE: The pyrophosphate group is H-bounded to itself across a 
crystallographic inversion center.  These two atoms and O7 and O11 are 
H-bound pairs across this symmetry element.  The hydrogen atoms could 
not be located in a difference electron density map and were not 
included in the final refinement model. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H26 N4 O4, 2 C16 H36 N 1+, H2 P2 O7 2-, 1/2 C H2 Cl2'
_chemical_formula_sum            'C62.50 H99 Cl N6 O11 P2'
_chemical_formula_weight         1207.86
# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 1.000 125 41 ' '
2 0.000 0.500 0.500 125 41 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.5077(3)
_cell_length_b                   15.3419(3)
_cell_length_c                   22.1726(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.4010(10)
_cell_angle_gamma                90
_cell_volume                     6606.47(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10978
_cell_measurement_theta_min      3.49
_cell_measurement_theta_max      74.1

_exptl_crystal_description       prisms
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             2604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.457
_shelx_estimated_absorpt_T_min   0.800
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35854
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.886
_diffrn_reflns_theta_max         74.239
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13076
_reflns_number_gt                10231
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;



_computing_data_collection       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'

_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'

_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 tetrapyrrole and the pyrophosphate form H-bound dimers across a 
crystallographic inversion center located at 1/2, 1/2, 1/2.  The 
pyrophospate dianion was H-bound to itself across this center.  Reliable 
coordinates for the hydrogen atoms bound to the pyrophosphate could not 
be located in a difference electron density map.  These hydrogen atoms 
were not included in the final refinement model.

 
  A molecule of dichloromethane was found to be 
badly disordered around a crystallographic inversion center at 0, 1/2, 
1/2.  Attempts 
to model the disorder were unsatisfactory.  The contributions to the 
scattering factors due to this solvent molecule were removed by use of 
the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998).  
PLATON98 was used as incorporated in WinGX (Farrugia, 1999).

;








_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0827P)²+5.3705P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13076
_refine_ls_number_parameters     761
_refine_ls_number_restraints     535
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1574
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.030
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.38118(16) 0.8547(2) 0.57874(12) 0.0506(8) Uani 1 1 d . U . . .
H1 H 0.3996 0.7980 0.5740 0.061 Uiso 1 1 calc R U . . .
C2 C 0.33291(14) 0.8876(2) 0.53079(11) 0.0400(6) Uani 1 1 d . U . . .
C3 C 0.29863(15) 0.9662(2) 0.52246(12) 0.0432(6) Uani 1 1 d . U . . .
H3 H 0.3026 1.0151 0.5489 0.052 Uiso 1 1 calc R U . . .
C4 C 0.25687(14) 0.96008(18) 0.46768(12) 0.0367(6) Uani 1 1 d . U . . .
H4 H 0.2273 1.0043 0.4501 0.044 Uiso 1 1 calc R U . . .
C5 C 0.26635(12) 0.87733(16) 0.44344(11) 0.0307(5) Uani 1 1 d . U . . .
C6 C 0.23611(12) 0.83771(16) 0.38420(10) 0.0284(5) Uani 1 1 d . U . . .
C7 C 0.19394(12) 0.75671(16) 0.39473(10) 0.0295(5) Uani 1 1 d . U . . .
C8 C 0.12454(13) 0.73969(18) 0.37896(11) 0.0355(5) Uani 1 1 d . U . . .
H8 H 0.0916 0.7794 0.3606 0.043 Uiso 1 1 calc R U . . .
C9 C 0.11222(14) 0.65331(19) 0.39517(11) 0.0396(6) Uani 1 1 d . U . . .
H9 H 0.0692 0.6238 0.3899 0.048 Uiso 1 1 calc R U . . .
C10 C 0.17368(14) 0.61864(17) 0.42024(11) 0.0351(5) Uani 1 1 d . U . . .
C11 C 0.19265(17) 0.53338(18) 0.44346(12) 0.0430(6) Uani 1 1 d . U . . .
H11 H 0.2388 0.5250 0.4602 0.052 Uiso 1 1 calc R U . . .
C12 C 0.18809(13) 0.90530(17) 0.35076(12) 0.0352(5) Uani 1 1 d . U . . .
H12A H 0.1497 0.9181 0.3749 0.053 Uiso 1 1 calc R U . . .
H12B H 0.1701 0.8819 0.3113 0.053 Uiso 1 1 calc R U . . .
H12C H 0.2139 0.9590 0.3448 0.053 Uiso 1 1 calc R U . . .
C13 C 0.29278(11) 0.81677(15) 0.34248(10) 0.0259(4) Uani 1 1 d . U . . .
C14 C 0.28437(11) 0.75151(16) 0.29909(10) 0.0285(5) Uani 1 1 d . U . . .
H14 H 0.2449 0.7150 0.2977 0.034 Uiso 1 1 calc R U . . .
C15 C 0.33286(12) 0.73861(16) 0.25754(10) 0.0286(5) Uani 1 1 d . U . . .
H15 H 0.3260 0.6934 0.2283 0.034 Uiso 1 1 calc R U . . .
C16 C 0.39093(11) 0.79092(15) 0.25834(9) 0.0257(4) Uani 1 1 d . U . . .
C17 C 0.39969(12) 0.85616(16) 0.30196(10) 0.0286(5) Uani 1 1 d . U . . .
H17 H 0.4391 0.8928 0.3033 0.034 Uiso 1 1 calc R U . . .
C18 C 0.35154(12) 0.86855(16) 0.34364(10) 0.0288(5) Uani 1 1 d . U . . .
H18 H 0.3589 0.9130 0.3734 0.035 Uiso 1 1 calc R U . . .
C19 C 0.44093(11) 0.78240(16) 0.20889(10) 0.0268(5) Uani 1 1 d . U . . .
C20 C 0.51276(11) 0.81323(16) 0.23210(10) 0.0276(5) Uani 1 1 d . U . . .
C21 C 0.55330(13) 0.87794(17) 0.20933(12) 0.0355(5) Uani 1 1 d . U . . .
H21 H 0.5420 0.9115 0.1738 0.043 Uiso 1 1 calc R U . . .
C22 C 0.61390(13) 0.88433(18) 0.24852(13) 0.0403(6) Uani 1 1 d . U . . .
H22 H 0.6511 0.9231 0.2444 0.048 Uiso 1 1 calc R U . . .
C23 C 0.60938(12) 0.82358(17) 0.29433(12) 0.0342(5) Uani 1 1 d . U . . .
C24 C 0.65418(14) 0.8043(2) 0.34774(14) 0.0435(6) Uani 1 1 d . U . . .
H24 H 0.6407 0.7588 0.3732 0.052 Uiso 1 1 calc R U . . .
C25 C 0.44417(11) 0.68937(17) 0.18654(10) 0.0290(5) Uani 1 1 d . U . . .
C26 C 0.43291(12) 0.65533(18) 0.12780(11) 0.0344(5) Uani 1 1 d . U . . .
H26 H 0.4206 0.6878 0.0919 0.041 Uiso 1 1 calc R U . . .
C27 C 0.44289(13) 0.56564(19) 0.13133(12) 0.0376(6) Uani 1 1 d . U . . .
H27 H 0.4389 0.5259 0.0983 0.045 Uiso 1 1 calc R U . . .
C28 C 0.45972(12) 0.54480(17) 0.19182(11) 0.0329(5) Uani 1 1 d . U . . .
C29 C 0.47535(12) 0.46367(18) 0.22265(13) 0.0378(6) Uani 1 1 d . U . . .
H29 H 0.4837 0.4651 0.2655 0.045 Uiso 1 1 calc R U . . .
C30 C 0.41320(13) 0.84178(18) 0.15570(10) 0.0352(5) Uani 1 1 d . U . . .
H30A H 0.4438 0.8381 0.1232 0.053 Uiso 1 1 calc R U . . .
H30B H 0.4114 0.9022 0.1699 0.053 Uiso 1 1 calc R U . . .
H30C H 0.3669 0.8227 0.1404 0.053 Uiso 1 1 calc R U . . .
C31 C 0.18843(17) 0.9784(2) 0.64147(15) 0.0549(8) Uani 1 1 d . U . . .
H31A H 0.2155 1.0261 0.6621 0.066 Uiso 1 1 calc R U . . .
H31B H 0.2123 0.9607 0.6059 0.066 Uiso 1 1 calc R U . . .
C32 C 0.11857(19) 1.0138(3) 0.61889(18) 0.0644(9) Uani 1 1 d . U . . .
H32A H 0.0959 1.0383 0.6533 0.077 Uiso 1 1 calc R U . . .
H32B H 0.0893 0.9662 0.6007 0.077 Uiso 1 1 calc R U . . .
C33 C 0.1261(2) 1.0843(3) 0.57198(18) 0.0687(10) Uani 1 1 d . U . . .
H33A H 0.1568 1.1308 0.5900 0.082 Uiso 1 1 calc R U . . .
H33B H 0.1478 1.0591 0.5373 0.082 Uiso 1 1 calc R U . . .
C34 C 0.0572(2) 1.1236(3) 0.5495(2) 0.0849(13) Uani 1 1 d . U . . .
H34A H 0.0270 1.0780 0.5309 0.127 Uiso 1 1 calc R U . . .
H34B H 0.0640 1.1688 0.5194 0.127 Uiso 1 1 calc R U . . .
H34C H 0.0360 1.1495 0.5836 0.127 Uiso 1 1 calc R U . . .
C35 C 0.26395(18) 0.8772(3) 0.70004(18) 0.0690(10) Uani 1 1 d . U . . .
H35A H 0.2840 0.8624 0.6619 0.083 Uiso 1 1 calc R U . . .
H35B H 0.2887 0.9291 0.7174 0.083 Uiso 1 1 calc R U . . .
C36 C 0.27742(18) 0.8031(3) 0.74326(18) 0.0681(10) Uani 1 1 d . U . . .
H36A H 0.2640 0.7469 0.7236 0.082 Uiso 1 1 calc R U . A 1
H36B H 0.2518 0.8107 0.7794 0.082 Uiso 1 1 calc R U . A 1
C37 C 0.3564(3) 0.8068(5) 0.7608(3) 0.0692(15) Uani 0.7 1 d D U P B 1
H37A H 0.3813 0.8076 0.7239 0.083 Uiso 0.7 1 calc R U P B 1
H37B H 0.3686 0.8603 0.7845 0.083 Uiso 0.7 1 calc R U P B 1
C38 C 0.3761(3) 0.7285(4) 0.7977(3) 0.0753(16) Uani 0.7 1 d D U P B 1
H38A H 0.3510 0.7281 0.8339 0.113 Uiso 0.7 1 calc R U P B 1
H38B H 0.4257 0.7296 0.8097 0.113 Uiso 0.7 1 calc R U P B 1
H38C H 0.3645 0.6760 0.7737 0.113 Uiso 0.7 1 calc R U P B 1
C37A C 0.3519(7) 0.7564(10) 0.7678(6) 0.059(3) Uani 0.3 1 d D U P B 2
H37C H 0.3803 0.7987 0.7929 0.071 Uiso 0.3 1 calc R U P B 2
H37D H 0.3427 0.7060 0.7938 0.071 Uiso 0.3 1 calc R U P B 2
C38A C 0.3912(6) 0.7261(8) 0.7175(5) 0.066(3) Uani 0.3 1 d D U P B 2
H38D H 0.3657 0.6792 0.6953 0.099 Uiso 0.3 1 calc R U P B 2
H38E H 0.4363 0.7043 0.7341 0.099 Uiso 0.3 1 calc R U P B 2
H38F H 0.3975 0.7748 0.6899 0.099 Uiso 0.3 1 calc R U P B 2
C39 C 0.15547(17) 0.9256(2) 0.74139(14) 0.0505(7) Uani 1 1 d . U . . .
H39A H 0.1507 0.8724 0.7659 0.061 Uiso 1 1 calc R U . . .
H39B H 0.1086 0.9484 0.7296 0.061 Uiso 1 1 calc R U . . .
C40 C 0.1963(2) 0.9943(3) 0.78059(17) 0.0696(10) Uani 1 1 d . U . . .
H40A H 0.2427 0.9711 0.7937 0.084 Uiso 1 1 calc R U . . .
H40B H 0.2021 1.0472 0.7561 0.084 Uiso 1 1 calc R U . . .
C41 C 0.1610(3) 1.0176(4) 0.8345(2) 0.1043(18) Uani 1 1 d . U . . .
H41A H 0.1533 0.9642 0.8581 0.125 Uiso 1 1 calc R U . . .
H41B H 0.1155 1.0435 0.8214 0.125 Uiso 1 1 calc R U . . .
C42 C 0.2036(4) 1.0827(4) 0.8749(2) 0.137(3) Uani 1 1 d . U . . .
H42A H 0.2492 1.0579 0.8868 0.205 Uiso 1 1 calc R U . . .
H42B H 0.1802 1.0947 0.9113 0.205 Uiso 1 1 calc R U . . .
H42C H 0.2087 1.1370 0.8525 0.205 Uiso 1 1 calc R U . . .
C43 C 0.14949(17) 0.8246(2) 0.65531(15) 0.0522(7) Uani 1 1 d . U . . .
H43A H 0.1012 0.8426 0.6441 0.063 Uiso 1 1 calc R U . . .
H43B H 0.1489 0.7770 0.6854 0.063 Uiso 1 1 calc R U . . .
C44 C 0.1799(2) 0.7895(3) 0.59853(18) 0.0670(10) Uani 1 1 d . U . . .
H44A H 0.1844 0.8379 0.5696 0.080 Uiso 1 1 calc R U . . .
H44B H 0.2265 0.7657 0.6101 0.080 Uiso 1 1 calc R U . . .
C45 C 0.1344(2) 0.7183(3) 0.56800(17) 0.0785(12) Uani 1 1 d . U . . .
H45A H 0.1602 0.6878 0.5380 0.094 Uiso 1 1 calc R U . . .
H45B H 0.1234 0.6752 0.5989 0.094 Uiso 1 1 calc R U . . .
C46 C 0.0711(3) 0.7521(5) 0.5380(3) 0.140(3) Uani 1 1 d . U . . .
H46A H 0.0384 0.7632 0.5680 0.210 Uiso 1 1 calc R U . . .
H46B H 0.0515 0.7094 0.5083 0.210 Uiso 1 1 calc R U . . .
H46C H 0.0805 0.8066 0.5172 0.210 Uiso 1 1 calc R U . . .
C47 C 0.36318(13) 0.34627(16) 0.38758(11) 0.0321(5) Uani 1 1 d . U . . .
H47A H 0.3727 0.3868 0.4221 0.038 Uiso 1 1 calc R U . . .
H47B H 0.4037 0.3472 0.3639 0.038 Uiso 1 1 calc R U . . .
C48 C 0.30127(13) 0.38010(16) 0.34763(11) 0.0331(5) Uani 1 1 d . U . . .
H48A H 0.2614 0.3854 0.3719 0.040 Uiso 1 1 calc R U . . .
H48B H 0.2890 0.3381 0.3145 0.040 Uiso 1 1 calc R U . . .
C49 C 0.31659(13) 0.46856(17) 0.32079(11) 0.0360(5) Uani 1 1 d . U . . .
H49A H 0.3532 0.4622 0.2931 0.043 Uiso 1 1 calc R U . . .
H49B H 0.3335 0.5090 0.3537 0.043 Uiso 1 1 calc R U . . .
C50 C 0.25223(14) 0.50648(18) 0.28615(11) 0.0368(6) Uani 1 1 d . U . . .
H50A H 0.2325 0.4637 0.2566 0.055 Uiso 1 1 calc R U . . .
H50B H 0.2644 0.5595 0.2649 0.055 Uiso 1 1 calc R U . . .
H50C H 0.2184 0.5207 0.3146 0.055 Uiso 1 1 calc R U . . .
C51 C 0.41663(13) 0.23962(17) 0.45949(11) 0.0345(5) Uani 1 1 d . U . . .
H51A H 0.4594 0.2431 0.4389 0.041 Uiso 1 1 calc R U . . .
H51B H 0.4180 0.2875 0.4895 0.041 Uiso 1 1 calc R U . . .
C52 C 0.41624(14) 0.15375(17) 0.49305(12) 0.0385(6) Uani 1 1 d . U . . .
H52A H 0.4129 0.1052 0.4635 0.046 Uiso 1 1 calc R U . . .
H52B H 0.3755 0.1512 0.5164 0.046 Uiso 1 1 calc R U . . .
C53 C 0.48175(13) 0.14336(18) 0.53620(12) 0.0372(6) Uani 1 1 d . U . . .
H53A H 0.5223 0.1425 0.5126 0.045 Uiso 1 1 calc R U . . .
H53B H 0.4865 0.1938 0.5641 0.045 Uiso 1 1 calc R U . . .
C54 C 0.47966(15) 0.05955(18) 0.57273(12) 0.0402(6) Uani 1 1 d . U . . .
H54A H 0.4436 0.0639 0.6005 0.060 Uiso 1 1 calc R U . . .
H54B H 0.5243 0.0505 0.5960 0.060 Uiso 1 1 calc R U . . .
H54C H 0.4697 0.0103 0.5452 0.060 Uiso 1 1 calc R U . . .
C55 C 0.28816(13) 0.24559(17) 0.44080(12) 0.0369(6) Uani 1 1 d . U . . .
H55A H 0.2847 0.1852 0.4560 0.044 Uiso 1 1 calc R U . . .
H55B H 0.2499 0.2543 0.4088 0.044 Uiso 1 1 calc R U . . .
C56 C 0.27825(14) 0.3077(2) 0.49233(12) 0.0416(6) Uani 1 1 d . U . . .
H56A H 0.2806 0.3687 0.4780 0.050 Uiso 1 1 calc R U . . .
H56B H 0.3153 0.2991 0.5254 0.050 Uiso 1 1 calc R U . . .
C57 C 0.20858(19) 0.2909(3) 0.51567(17) 0.0687(11) Uani 1 1 d . U . . .
H57A H 0.1717 0.3024 0.4829 0.082 Uiso 1 1 calc R U . . .
H57B H 0.2055 0.2289 0.5276 0.082 Uiso 1 1 calc R U . . .
C58 C 0.1978(3) 0.3485(4) 0.56977(18) 0.105(2) Uani 1 1 d . U . . .
H58A H 0.2339 0.3366 0.6025 0.157 Uiso 1 1 calc R U . . .
H58B H 0.1527 0.3361 0.5838 0.157 Uiso 1 1 calc R U . . .
H58C H 0.2000 0.4099 0.5579 0.157 Uiso 1 1 calc R U . . .
C59 C 0.35411(14) 0.18704(18) 0.36191(12) 0.0405(6) Uani 1 1 d . U . . .
H59A H 0.3425 0.1298 0.3789 0.049 Uiso 1 1 calc R U . . .
H59B H 0.3164 0.2025 0.3307 0.049 Uiso 1 1 calc R U . . .
C60 C 0.41951(16) 0.1765(2) 0.33085(15) 0.0535(8) Uani 1 1 d . U . . .
H60A H 0.4573 0.1564 0.3605 0.064 Uiso 1 1 calc R U . . .
H60B H 0.4330 0.2333 0.3144 0.064 Uiso 1 1 calc R U . . .
C61 C 0.40784(17) 0.1100(2) 0.27916(14) 0.0519(8) Uani 1 1 d . U . . .
H61A H 0.3904 0.0550 0.2953 0.062 Uiso 1 1 calc R U . . .
H61B H 0.3723 0.1326 0.2483 0.062 Uiso 1 1 calc R U . . .
C62 C 0.4722(2) 0.0915(3) 0.24983(16) 0.0676(11) Uani 1 1 d . U . . .
H62A H 0.4897 0.1458 0.2337 0.101 Uiso 1 1 calc R U . . .
H62B H 0.4623 0.0498 0.2167 0.101 Uiso 1 1 calc R U . . .
H62C H 0.5070 0.0670 0.2799 0.101 Uiso 1 1 calc R U . . .
N1 N 0.31252(11) 0.83525(15) 0.48195(9) 0.0336(4) Uani 1 1 d . U . . .
H1N H 0.3275 0.7819 0.4767 0.040 Uiso 1 1 calc R U . . .
N2 N 0.22275(11) 0.68293(14) 0.41960(9) 0.0319(4) Uani 1 1 d . U . . .
H2N H 0.2663 0.6771 0.4333 0.038 Uiso 1 1 calc R U . . .
N3 N 0.54720(10) 0.78068(13) 0.28307(8) 0.0279(4) Uani 1 1 d . U . . .
H3N H 0.5323 0.7387 0.3055 0.034 Uiso 1 1 calc R U . . .
N4 N 0.45989(10) 0.62172(13) 0.22411(9) 0.0291(4) Uani 1 1 d . U . . .
H4N H 0.4690 0.6260 0.2636 0.035 Uiso 1 1 calc R U . . .
N5 N 0.18905(13) 0.90163(18) 0.68454(12) 0.0493(6) Uani 1 1 d . U . . .
N6 N 0.35533(10) 0.25449(13) 0.41247(9) 0.0325(4) Uani 1 1 d . U . . .
O1 O 0.39987(13) 0.89472(19) 0.62489(9) 0.0675(7) Uani 1 1 d . U . . .
O2 O 0.15372(13) 0.47124(14) 0.44311(10) 0.0563(6) Uani 1 1 d . U . . .
O3 O 0.70850(11) 0.84198(16) 0.36304(12) 0.0596(6) Uani 1 1 d . U . . .
O4 O 0.47860(10) 0.39310(13) 0.19750(10) 0.0454(5) Uani 1 1 d . U . . .
O5 O 0.34889(12) 0.66912(14) 0.47922(11) 0.0561(6) Uani 1 1 d . U . . .
O6 O 0.45917(11) 0.62400(12) 0.53866(9) 0.0444(5) Uani 1 1 d . U . . .
O7 O 0.38239(10) 0.51273(12) 0.48399(8) 0.0397(4) Uani 1 1 d . U . . .
O8 O 0.44431(11) 0.62529(13) 0.42481(9) 0.0462(5) Uani 1 1 d . U . . .
O9 O 0.51182(11) 0.63529(13) 0.33936(9) 0.0464(5) Uani 1 1 d . U . . .
O10 O 0.49552(10) 0.48877(12) 0.38528(8) 0.0405(4) Uani 1 1 d . U . . .
O11 O 0.57351(9) 0.59973(11) 0.43994(8) 0.0383(4) Uani 1 1 d . U . . .
P1 P 0.50987(3) 0.58450(4) 0.39667(3) 0.03238(15) Uani 1 1 d . U . . .
P2 P 0.40719(3) 0.60655(4) 0.48554(3) 0.03399(15) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.219(4) . ?
C1 C2 1.443(4) . ?
C1 H1 0.9500 . ?
C2 N1 1.376(3) . ?
C2 C3 1.383(4) . ?
C3 C4 1.400(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.346(3) . ?
C5 C6 1.516(3) . ?
C6 C7 1.521(3) . ?
C6 C12 1.540(3) . ?
C6 C13 1.541(3) . ?
C7 N2 1.358(3) . ?
C7 C8 1.391(3) . ?
C8 C9 1.400(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(4) . ?
C9 H9 0.9500 . ?
C10 N2 1.376(3) . ?
C10 C11 1.441(4) . ?
C11 O2 1.218(4) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.387(3) . ?
C13 C18 1.393(3) . ?
C14 C15 1.395(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(3) . ?
C16 C19 1.540(3) . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C25 1.514(3) . ?
C19 C20 1.522(3) . ?
C19 C30 1.547(3) . ?
C20 N3 1.355(3) . ?
C20 C21 1.393(3) . ?
C21 C22 1.403(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(4) . ?
C22 H22 0.9500 . ?
C23 N3 1.382(3) . ?
C23 C24 1.435(4) . ?
C24 O3 1.226(3) . ?
C24 H24 0.9500 . ?
C25 N4 1.348(3) . ?
C25 C26 1.401(3) . ?
C26 C27 1.391(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(4) . ?
C27 H27 0.9500 . ?
C28 N4 1.380(3) . ?
C28 C29 1.439(4) . ?
C29 O4 1.222(3) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.509(5) . ?
C31 N5 1.515(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.517(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.514(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.494(6) . ?
C35 N5 1.516(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.555(7) . ?
C36 C37A 1.665(14) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.482(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C37A C38A 1.486(11) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 0.9800 . ?
C39 N5 1.520(4) . ?
C39 C40 1.539(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.480(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.533(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N5 1.522(4) . ?
C43 C44 1.539(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.524(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.443(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.520(3) . ?
C47 N6 1.525(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.523(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.524(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.513(4) . ?
C51 N6 1.528(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.531(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.522(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 N6 1.512(3) . ?
C55 C56 1.514(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.521(4) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.520(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.515(4) . ?
C59 N6 1.524(3) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.536(4) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.495(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N1 H1N 0.8800 . ?
N2 H2N 0.8800 . ?
N3 H3N 0.8800 . ?
N4 H4N 0.8800 . ?
O5 P2 1.485(2) . ?
O6 P2 1.5040(19) . ?
O7 P2 1.5180(19) . ?
O8 P1 1.602(2) . ?
O8 P2 1.614(2) . ?
O9 P1 1.4940(19) . ?
O10 P1 1.5120(19) . ?
O11 P1 1.5139(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
O1 C1 C2 124.4(4) . . ?
O1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
N1 C2 C3 107.7(2) . . ?
N1 C2 C1 119.7(3) . . ?
C3 C2 C1 132.6(3) . . ?
C2 C3 C4 107.0(2) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
C5 C4 C3 107.9(2) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
N1 C5 C4 107.2(2) . . ?
N1 C5 C6 122.7(2) . . ?
C4 C5 C6 130.0(2) . . ?
C5 C6 C7 111.52(19) . . ?
C5 C6 C12 108.5(2) . . ?
C7 C6 C12 108.1(2) . . ?
C5 C6 C13 111.18(19) . . ?
C7 C6 C13 110.55(19) . . ?
C12 C6 C13 106.83(18) . . ?
N2 C7 C8 107.6(2) . . ?
N2 C7 C6 122.3(2) . . ?
C8 C7 C6 130.0(2) . . ?
C7 C8 C9 107.4(2) . . ?
C7 C8 H8 126.3 . . ?
C9 C8 H8 126.3 . . ?
C10 C9 C8 107.7(2) . . ?
C10 C9 H9 126.1 . . ?
C8 C9 H9 126.1 . . ?
N2 C10 C9 107.4(2) . . ?
N2 C10 C11 119.9(2) . . ?
C9 C10 C11 132.7(3) . . ?
O2 C11 C10 124.7(3) . . ?
O2 C11 H11 117.7 . . ?
C10 C11 H11 117.7 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 117.9(2) . . ?
C14 C13 C6 121.5(2) . . ?
C18 C13 C6 120.4(2) . . ?
C13 C14 C15 121.1(2) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 120.9(2) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 118.2(2) . . ?
C15 C16 C19 120.9(2) . . ?
C17 C16 C19 120.7(2) . . ?
C16 C17 C18 120.9(2) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 121.0(2) . . ?
C17 C18 H18 119.5 . . ?
C13 C18 H18 119.5 . . ?
C25 C19 C20 109.77(18) . . ?
C25 C19 C16 111.20(19) . . ?
C20 C19 C16 110.94(18) . . ?
C25 C19 C30 109.15(19) . . ?
C20 C19 C30 108.64(19) . . ?
C16 C19 C30 107.05(18) . . ?
N3 C20 C21 108.1(2) . . ?
N3 C20 C19 122.4(2) . . ?
C21 C20 C19 129.4(2) . . ?
C20 C21 C22 107.4(2) . . ?
C20 C21 H21 126.3 . . ?
C22 C21 H21 126.3 . . ?
C23 C22 C21 107.4(2) . . ?
C23 C22 H22 126.3 . . ?
C21 C22 H22 126.3 . . ?
N3 C23 C22 107.6(2) . . ?
N3 C23 C24 120.5(2) . . ?
C22 C23 C24 131.8(2) . . ?
O3 C24 C23 125.1(3) . . ?
O3 C24 H24 117.5 . . ?
C23 C24 H24 117.5 . . ?
N4 C25 C26 107.1(2) . . ?
N4 C25 C19 122.52(19) . . ?
C26 C25 C19 130.4(2) . . ?
C27 C26 C25 107.9(2) . . ?
C27 C26 H26 126.0 . . ?
C25 C26 H26 126.0 . . ?
C28 C27 C26 107.5(2) . . ?
C28 C27 H27 126.2 . . ?
C26 C27 H27 126.2 . . ?
N4 C28 C27 107.1(2) . . ?
N4 C28 C29 120.2(2) . . ?
C27 C28 C29 132.7(2) . . ?
O4 C29 C28 124.6(3) . . ?
O4 C29 H29 117.7 . . ?
C28 C29 H29 117.7 . . ?
C19 C30 H30A 109.5 . . ?
C19 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C19 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 N5 116.3(2) . . ?
C32 C31 H31A 108.2 . . ?
N5 C31 H31A 108.2 . . ?
C32 C31 H31B 108.2 . . ?
N5 C31 H31B 108.2 . . ?
H31A C31 H31B 107.4 . . ?
C31 C32 C33 110.0(3) . . ?
C31 C32 H32A 109.7 . . ?
C33 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C34 C33 C32 111.7(3) . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N5 116.2(3) . . ?
C36 C35 H35A 108.2 . . ?
N5 C35 H35A 108.2 . . ?
C36 C35 H35B 108.2 . . ?
N5 C35 H35B 108.2 . . ?
H35A C35 H35B 107.4 . . ?
C35 C36 C37 104.1(4) . . ?
C35 C36 C37A 129.2(6) . . ?
C35 C36 H36A 110.9 . . ?
C37 C36 H36A 110.9 . . ?
C35 C36 H36B 110.9 . . ?
C37 C36 H36B 110.9 . . ?
H36A C36 H36B 109.0 . . ?
C38 C37 C36 107.9(5) . . ?
C38 C37 H37A 110.1 . . ?
C36 C37 H37A 110.1 . . ?
C38 C37 H37B 110.1 . . ?
C36 C37 H37B 110.1 . . ?
H37A C37 H37B 108.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C38A C37A C36 112.7(10) . . ?
C38A C37A H37C 109.1 . . ?
C36 C37A H37C 109.1 . . ?
C38A C37A H37D 109.1 . . ?
C36 C37A H37D 109.1 . . ?
H37C C37A H37D 107.8 . . ?
C37A C38A H38D 109.5 . . ?
C37A C38A H38E 109.5 . . ?
H38D C38A H38E 109.5 . . ?
C37A C38A H38F 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?
N5 C39 C40 113.2(3) . . ?
N5 C39 H39A 108.9 . . ?
C40 C39 H39A 108.9 . . ?
N5 C39 H39B 108.9 . . ?
C40 C39 H39B 108.9 . . ?
H39A C39 H39B 107.8 . . ?
C41 C40 C39 111.5(3) . . ?
C41 C40 H40A 109.3 . . ?
C39 C40 H40A 109.3 . . ?
C41 C40 H40B 109.3 . . ?
C39 C40 H40B 109.3 . . ?
H40A C40 H40B 108.0 . . ?
C40 C41 C42 111.2(4) . . ?
C40 C41 H41A 109.4 . . ?
C42 C41 H41A 109.4 . . ?
C40 C41 H41B 109.4 . . ?
C42 C41 H41B 109.4 . . ?
H41A C41 H41B 108.0 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 C44 113.6(3) . . ?
N5 C43 H43A 108.8 . . ?
C44 C43 H43A 108.8 . . ?
N5 C43 H43B 108.8 . . ?
C44 C43 H43B 108.8 . . ?
H43A C43 H43B 107.7 . . ?
C45 C44 C43 111.2(3) . . ?
C45 C44 H44A 109.4 . . ?
C43 C44 H44A 109.4 . . ?
C45 C44 H44B 109.4 . . ?
C43 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
C46 C45 C44 112.6(5) . . ?
C46 C45 H45A 109.1 . . ?
C44 C45 H45A 109.1 . . ?
C46 C45 H45B 109.1 . . ?
C44 C45 H45B 109.1 . . ?
H45A C45 H45B 107.8 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 N6 115.13(19) . . ?
C48 C47 H47A 108.5 . . ?
N6 C47 H47A 108.5 . . ?
C48 C47 H47B 108.5 . . ?
N6 C47 H47B 108.5 . . ?
H47A C47 H47B 107.5 . . ?
C47 C48 C49 111.0(2) . . ?
C47 C48 H48A 109.4 . . ?
C49 C48 H48A 109.4 . . ?
C47 C48 H48B 109.4 . . ?
C49 C48 H48B 109.4 . . ?
H48A C48 H48B 108.0 . . ?
C48 C49 C50 110.8(2) . . ?
C48 C49 H49A 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 N6 115.2(2) . . ?
C52 C51 H51A 108.5 . . ?
N6 C51 H51A 108.5 . . ?
C52 C51 H51B 108.5 . . ?
N6 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 C53 110.8(2) . . ?
C51 C52 H52A 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C53 C52 H52B 109.5 . . ?
H52A C52 H52B 108.1 . . ?
C54 C53 C52 111.0(2) . . ?
C54 C53 H53A 109.4 . . ?
C52 C53 H53A 109.4 . . ?
C54 C53 H53B 109.4 . . ?
C52 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N6 C55 C56 115.7(2) . . ?
N6 C55 H55A 108.4 . . ?
C56 C55 H55A 108.4 . . ?
N6 C55 H55B 108.4 . . ?
C56 C55 H55B 108.4 . . ?
H55A C55 H55B 107.4 . . ?
C55 C56 C57 109.4(3) . . ?
C55 C56 H56A 109.8 . . ?
C57 C56 H56A 109.8 . . ?
C55 C56 H56B 109.8 . . ?
C57 C56 H56B 109.8 . . ?
H56A C56 H56B 108.3 . . ?
C58 C57 C56 111.3(4) . . ?
C58 C57 H57A 109.4 . . ?
C56 C57 H57A 109.4 . . ?
C58 C57 H57B 109.4 . . ?
C56 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
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 . . ?
C60 C59 N6 116.8(2) . . ?
C60 C59 H59A 108.1 . . ?
N6 C59 H59A 108.1 . . ?
C60 C59 H59B 108.1 . . ?
N6 C59 H59B 108.1 . . ?
H59A C59 H59B 107.3 . . ?
C59 C60 C61 109.8(3) . . ?
C59 C60 H60A 109.7 . . ?
C61 C60 H60A 109.7 . . ?
C59 C60 H60B 109.7 . . ?
C61 C60 H60B 109.7 . . ?
H60A C60 H60B 108.2 . . ?
C62 C61 C60 112.3(3) . . ?
C62 C61 H61A 109.2 . . ?
C60 C61 H61A 109.2 . . ?
C62 C61 H61B 109.2 . . ?
C60 C61 H61B 109.2 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C5 N1 C2 110.2(2) . . ?
C5 N1 H1N 124.9 . . ?
C2 N1 H1N 124.9 . . ?
C7 N2 C10 109.9(2) . . ?
C7 N2 H2N 125.1 . . ?
C10 N2 H2N 125.1 . . ?
C20 N3 C23 109.5(2) . . ?
C20 N3 H3N 125.3 . . ?
C23 N3 H3N 125.3 . . ?
C25 N4 C28 110.4(2) . . ?
C25 N4 H4N 124.8 . . ?
C28 N4 H4N 124.8 . . ?
C31 N5 C35 106.6(3) . . ?
C31 N5 C39 110.9(2) . . ?
C35 N5 C39 110.7(3) . . ?
C31 N5 C43 111.2(3) . . ?
C35 N5 C43 110.1(3) . . ?
C39 N5 C43 107.5(2) . . ?
C55 N6 C59 106.86(19) . . ?
C55 N6 C47 110.74(19) . . ?
C59 N6 C47 110.8(2) . . ?
C55 N6 C51 110.88(19) . . ?
C59 N6 C51 110.95(19) . . ?
C47 N6 C51 106.62(17) . . ?
P1 O8 P2 133.85(13) . . ?
O9 P1 O10 112.57(11) . . ?
O9 P1 O11 111.93(11) . . ?
O10 P1 O11 112.56(10) . . ?
O9 P1 O8 102.28(12) . . ?
O10 P1 O8 107.61(12) . . ?
O11 P1 O8 109.26(11) . . ?
O5 P2 O6 114.38(13) . . ?
O5 P2 O7 111.79(13) . . ?
O6 P2 O7 112.12(10) . . ?
O5 P2 O8 101.88(12) . . ?
O6 P2 O8 107.42(12) . . ?
O7 P2 O8 108.49(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -176.7(3) . . . . ?
O1 C1 C2 C3 2.1(5) . . . . ?
N1 C2 C3 C4 0.3(3) . . . . ?
C1 C2 C3 C4 -178.6(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 N1 -0.4(3) . . . . ?
C3 C4 C5 C6 -177.4(2) . . . . ?
N1 C5 C6 C7 63.6(3) . . . . ?
C4 C5 C6 C7 -119.8(3) . . . . ?
N1 C5 C6 C12 -177.4(2) . . . . ?
C4 C5 C6 C12 -0.9(3) . . . . ?
N1 C5 C6 C13 -60.3(3) . . . . ?
C4 C5 C6 C13 116.3(3) . . . . ?
C5 C6 C7 N2 -65.5(3) . . . . ?
C12 C6 C7 N2 175.4(2) . . . . ?
C13 C6 C7 N2 58.7(3) . . . . ?
C5 C6 C7 C8 119.2(3) . . . . ?
C12 C6 C7 C8 0.1(3) . . . . ?
C13 C6 C7 C8 -116.6(3) . . . . ?
N2 C7 C8 C9 0.1(3) . . . . ?
C6 C7 C8 C9 175.9(2) . . . . ?
C7 C8 C9 C10 -0.2(3) . . . . ?
C8 C9 C10 N2 0.2(3) . . . . ?
C8 C9 C10 C11 -178.3(3) . . . . ?
N2 C10 C11 O2 -176.2(2) . . . . ?
C9 C10 C11 O2 2.3(5) . . . . ?
C5 C6 C13 C14 153.7(2) . . . . ?
C7 C6 C13 C14 29.2(3) . . . . ?
C12 C6 C13 C14 -88.2(3) . . . . ?
C5 C6 C13 C18 -32.3(3) . . . . ?
C7 C6 C13 C18 -156.7(2) . . . . ?
C12 C6 C13 C18 85.9(3) . . . . ?
C18 C13 C14 C15 -0.6(3) . . . . ?
C6 C13 C14 C15 173.6(2) . . . . ?
C13 C14 C15 C16 -0.1(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C14 C15 C16 C19 -174.2(2) . . . . ?
C15 C16 C17 C18 0.0(3) . . . . ?
C19 C16 C17 C18 174.7(2) . . . . ?
C16 C17 C18 C13 -0.8(3) . . . . ?
C14 C13 C18 C17 1.1(3) . . . . ?
C6 C13 C18 C17 -173.2(2) . . . . ?
C15 C16 C19 C25 -32.4(3) . . . . ?
C17 C16 C19 C25 153.1(2) . . . . ?
C15 C16 C19 C20 -154.8(2) . . . . ?
C17 C16 C19 C20 30.6(3) . . . . ?
C15 C16 C19 C30 86.8(3) . . . . ?
C17 C16 C19 C30 -87.7(2) . . . . ?
C25 C19 C20 N3 -68.7(3) . . . . ?
C16 C19 C20 N3 54.6(3) . . . . ?
C30 C19 C20 N3 172.0(2) . . . . ?
C25 C19 C20 C21 114.0(3) . . . . ?
C16 C19 C20 C21 -122.7(3) . . . . ?
C30 C19 C20 C21 -5.3(3) . . . . ?
N3 C20 C21 C22 -0.4(3) . . . . ?
C19 C20 C21 C22 177.2(2) . . . . ?
C20 C21 C22 C23 0.1(3) . . . . ?
C21 C22 C23 N3 0.2(3) . . . . ?
C21 C22 C23 C24 -176.5(3) . . . . ?
N3 C23 C24 O3 -176.1(3) . . . . ?
C22 C23 C24 O3 0.3(5) . . . . ?
C20 C19 C25 N4 67.8(3) . . . . ?
C16 C19 C25 N4 -55.4(3) . . . . ?
C30 C19 C25 N4 -173.3(2) . . . . ?
C20 C19 C25 C26 -112.1(3) . . . . ?
C16 C19 C25 C26 124.7(3) . . . . ?
C30 C19 C25 C26 6.8(3) . . . . ?
N4 C25 C26 C27 -0.5(3) . . . . ?
C19 C25 C26 C27 179.4(2) . . . . ?
C25 C26 C27 C28 0.4(3) . . . . ?
C26 C27 C28 N4 -0.1(3) . . . . ?
C26 C27 C28 C29 179.9(3) . . . . ?
N4 C28 C29 O4 -177.5(2) . . . . ?
C27 C28 C29 O4 2.5(4) . . . . ?
N5 C31 C32 C33 -174.7(3) . . . . ?
C31 C32 C33 C34 -178.3(4) . . . . ?
N5 C35 C36 C37 -168.1(4) . . . . ?
N5 C35 C36 C37A 177.0(7) . . . . ?
C35 C36 C37 C38 -172.8(5) . . . . ?
C35 C36 C37A C38A -54.5(14) . . . . ?
N5 C39 C40 C41 178.4(4) . . . . ?
C39 C40 C41 C42 177.3(5) . . . . ?
N5 C43 C44 C45 -174.7(3) . . . . ?
C43 C44 C45 C46 72.0(5) . . . . ?
N6 C47 C48 C49 -175.1(2) . . . . ?
C47 C48 C49 C50 -174.1(2) . . . . ?
N6 C51 C52 C53 176.7(2) . . . . ?
C51 C52 C53 C54 176.7(2) . . . . ?
N6 C55 C56 C57 179.8(2) . . . . ?
C55 C56 C57 C58 176.9(3) . . . . ?
N6 C59 C60 C61 -176.9(2) . . . . ?
C59 C60 C61 C62 -175.5(3) . . . . ?
C4 C5 N1 C2 0.6(3) . . . . ?
C6 C5 N1 C2 177.8(2) . . . . ?
C3 C2 N1 C5 -0.5(3) . . . . ?
C1 C2 N1 C5 178.5(2) . . . . ?
C8 C7 N2 C10 0.0(3) . . . . ?
C6 C7 N2 C10 -176.2(2) . . . . ?
C9 C10 N2 C7 -0.2(3) . . . . ?
C11 C10 N2 C7 178.6(2) . . . . ?
C21 C20 N3 C23 0.5(3) . . . . ?
C19 C20 N3 C23 -177.3(2) . . . . ?
C22 C23 N3 C20 -0.5(3) . . . . ?
C24 C23 N3 C20 176.7(2) . . . . ?
C26 C25 N4 C28 0.4(3) . . . . ?
C19 C25 N4 C28 -179.5(2) . . . . ?
C27 C28 N4 C25 -0.2(3) . . . . ?
C29 C28 N4 C25 179.8(2) . . . . ?
C32 C31 N5 C35 179.3(3) . . . . ?
C32 C31 N5 C39 -60.2(4) . . . . ?
C32 C31 N5 C43 59.3(4) . . . . ?
C36 C35 N5 C31 179.0(3) . . . . ?
C36 C35 N5 C39 58.4(4) . . . . ?
C36 C35 N5 C43 -60.3(4) . . . . ?
C40 C39 N5 C31 -66.5(4) . . . . ?
C40 C39 N5 C35 51.5(4) . . . . ?
C40 C39 N5 C43 171.8(3) . . . . ?
C44 C43 N5 C31 61.5(4) . . . . ?
C44 C43 N5 C35 -56.4(4) . . . . ?
C44 C43 N5 C39 -177.0(3) . . . . ?
C56 C55 N6 C59 -179.5(2) . . . . ?
C56 C55 N6 C47 -58.7(3) . . . . ?
C56 C55 N6 C51 59.4(3) . . . . ?
C60 C59 N6 C55 -173.6(2) . . . . ?
C60 C59 N6 C47 65.6(3) . . . . ?
C60 C59 N6 C51 -52.6(3) . . . . ?
C48 C47 N6 C55 -49.5(3) . . . . ?
C48 C47 N6 C59 68.9(3) . . . . ?
C48 C47 N6 C51 -170.2(2) . . . . ?
C52 C51 N6 C55 55.5(3) . . . . ?
C52 C51 N6 C59 -63.1(3) . . . . ?
C52 C51 N6 C47 176.1(2) . . . . ?
P2 O8 P1 O9 179.70(18) . . . . ?
P2 O8 P1 O10 60.9(2) . . . . ?
P2 O8 P1 O11 -61.6(2) . . . . ?
P1 O8 P2 O5 -178.78(19) . . . . ?
P1 O8 P2 O6 60.7(2) . . . . ?
P1 O8 P2 O7 -60.7(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
C8 H8 O4 0.95 2.50 3.438(3) 170.2 2
C31 H31A O3 0.99 2.60 3.419(4) 140.2 3_676
C35 H35A O1 0.99 2.53 3.273(4) 132.1 .
C47 H47A O7 0.99 2.37 3.329(3) 163.6 .
C51 H51A O6 0.99 2.60 3.199(3) 118.6 3_666
C51 H51B O11 0.99 2.33 3.317(3) 177.4 3_666
N1 H1N O5 0.88 1.78 2.648(3) 168.3 .
N2 H2N O5 0.88 1.83 2.690(3) 166.3 .
N3 H3N O9 0.88 1.82 2.678(3) 166.0 .
N4 H4N O9 0.88 1.81 2.667(3) 164.2 .

_refine_diff_density_max         1.034
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.057




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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1444560'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H26 N4 O4, H2 P O4 1-, C16 H36 N 1+, 1/2 C H Cl3'
_chemical_formula_sum            'C46.50 H64.50 Cl1.50 N5 O8 P'
_chemical_formula_weight         905.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9599(4)
_cell_length_b                   14.6932(6)
_cell_length_c                   16.4802(5)
_cell_angle_alpha                81.050(3)
_cell_angle_beta                 75.273(3)
_cell_angle_gamma                88.017(3)
_cell_volume                     2304.10(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13482
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      74.0

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_F_000             966
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.802
_shelx_estimated_absorpt_T_min   0.749
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed microfocus tube'
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24272
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.805
_diffrn_reflns_theta_max         74.533
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             9074
_reflns_number_gt                8086
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;



_computing_data_collection       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'

_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'





_refine_special_details          
;
A molecule of chloroform was found to be disordered near a crystallographic 
inversion center at 0, 1/2, 1/2.  The C-Cl bond lengths and the Cl-C-Cl bond 
angles were restrained to be equivalent throughout the refinement.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+2.5503P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9074
_refine_ls_number_parameters     607
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.049
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.89080(4) 0.20046(3) 0.31923(3) 0.01150(11) Uani 1 1 d . . . . .
O1 O 1.39806(15) -0.02384(10) 0.16064(10) 0.0255(3) Uani 1 1 d . . . . .
O2 O 1.08364(16) 0.40205(10) 0.29767(9) 0.0248(3) Uani 1 1 d . . . . .
O3 O 0.74719(16) 0.60487(10) 0.29679(10) 0.0267(3) Uani 1 1 d . . . . .
O4 O 0.56821(14) 0.08327(9) 0.44013(9) 0.0177(3) Uani 1 1 d . . . . .
O5 O 1.00144(14) 0.19067(9) 0.24066(9) 0.0182(3) Uani 1 1 d . . . . .
O6 O 0.76641(13) 0.25600(9) 0.30684(9) 0.0174(3) Uani 1 1 d . . . . .
O7 O 0.84184(14) 0.10236(9) 0.37019(9) 0.0167(3) Uani 1 1 d . . . . .
H7O H 0.756(3) 0.099(2) 0.3899(19) 0.039(8) Uiso 1 1 d . . . . .
O8 O 0.95704(15) 0.24143(10) 0.38387(9) 0.0195(3) Uani 1 1 d . . . . .
H8O H 1.002(3) 0.287(2) 0.359(2) 0.044(9) Uiso 1 1 d . . . . .
N1 N 1.17341(16) 0.15140(10) 0.09274(10) 0.0121(3) Uani 1 1 d . . . . .
H1N H 1.112(3) 0.1560(16) 0.1382(17) 0.021(6) Uiso 1 1 d . . . . .
N2 N 1.07777(15) 0.35271(11) 0.13062(10) 0.0127(3) Uani 1 1 d . . . . .
H2N H 1.044(3) 0.3005(19) 0.1719(18) 0.032(7) Uiso 1 1 d . . . . .
N3 N 0.66308(16) 0.40261(11) 0.22162(10) 0.0129(3) Uani 1 1 d . . . . .
H3N H 0.706(3) 0.3570(19) 0.2478(18) 0.032(7) Uiso 1 1 d . . . . .
N4 N 0.52339(16) 0.19712(10) 0.28800(10) 0.0128(3) Uani 1 1 d . . . . .
H4N H 0.608(3) 0.2057(18) 0.2893(17) 0.033(7) Uiso 1 1 d . . . . .
N5 N 0.59380(17) 0.20803(11) 0.63935(10) 0.0162(3) Uani 1 1 d . . . . .
C1 C 1.3009(2) 0.02955(13) 0.15897(13) 0.0180(4) Uani 1 1 d . . . . .
H1 H 1.2306 0.0297 0.2102 0.022 Uiso 1 1 calc R U . . .
C2 C 1.28483(18) 0.09169(12) 0.08591(12) 0.0136(4) Uani 1 1 d . . . . .
C3 C 1.36359(19) 0.10736(13) 0.00207(12) 0.0155(4) Uani 1 1 d . . . . .
H3 H 1.4465 0.0765 -0.0213 0.019 Uiso 1 1 calc R U . . .
C4 C 1.29743(19) 0.17733(12) -0.04125(12) 0.0136(4) Uani 1 1 d . . . . .
H4 H 1.3273 0.2024 -0.0997 0.016 Uiso 1 1 calc R U . . .
C5 C 1.17997(18) 0.20360(12) 0.01663(11) 0.0109(3) Uani 1 1 d . . . . .
C6 C 1.07149(18) 0.27631(12) 0.00441(11) 0.0117(3) Uani 1 1 d . . . . .
C7 C 1.09733(17) 0.35793(12) 0.04512(12) 0.0125(4) Uani 1 1 d . . . . .
C8 C 1.15329(19) 0.44406(13) 0.00605(12) 0.0151(4) Uani 1 1 d . . . . .
H8 H 1.1767 0.4662 -0.0531 0.018 Uiso 1 1 calc R U . . .
C9 C 1.16859(19) 0.49168(13) 0.07021(13) 0.0173(4) Uani 1 1 d . . . . .
H9 H 1.2048 0.5523 0.0625 0.021 Uiso 1 1 calc R U . . .
C10 C 1.12143(19) 0.43463(12) 0.14743(12) 0.0146(4) Uani 1 1 d . . . . .
C11 C 1.1223(2) 0.45323(13) 0.22981(13) 0.0187(4) Uani 1 1 d . . . . .
H11 H 1.1567 0.5119 0.2323 0.022 Uiso 1 1 calc R U . . .
C12 C 1.08835(19) 0.30772(13) -0.09117(12) 0.0153(4) Uani 1 1 d . . . . .
H12A H 1.0208 0.3561 -0.0994 0.023 Uiso 1 1 calc R U . . .
H12B H 1.0725 0.2552 -0.1178 0.023 Uiso 1 1 calc R U . . .
H12C H 1.1825 0.3318 -0.1172 0.023 Uiso 1 1 calc R U . . .
C13 C 0.92491(18) 0.23417(12) 0.04164(11) 0.0115(3) Uani 1 1 d . . . . .
C14 C 0.81134(18) 0.28515(12) 0.08027(11) 0.0111(3) Uani 1 1 d . . . . .
H14 H 0.8251 0.3471 0.0864 0.013 Uiso 1 1 calc R U . . .
C15 C 0.67878(18) 0.24647(12) 0.10984(11) 0.0113(3) Uani 1 1 d . . . . .
C16 C 0.66014(19) 0.15535(13) 0.10039(12) 0.0141(4) Uani 1 1 d . . . . .
H16 H 0.5708 0.1276 0.1214 0.017 Uiso 1 1 calc R U . . .
C17 C 0.7709(2) 0.10505(13) 0.06060(13) 0.0170(4) Uani 1 1 d . . . . .
H17 H 0.7566 0.0437 0.0530 0.020 Uiso 1 1 calc R U . . .
C18 C 0.90240(19) 0.14391(13) 0.03192(12) 0.0160(4) Uani 1 1 d . . . . .
H18 H 0.9780 0.1087 0.0054 0.019 Uiso 1 1 calc R U . . .
C19 C 0.54865(18) 0.30022(12) 0.14807(12) 0.0119(3) Uani 1 1 d . . . . .
C20 C 0.57893(18) 0.39244(12) 0.17035(12) 0.0129(4) Uani 1 1 d . . . . .
C21 C 0.52416(19) 0.47874(13) 0.14835(13) 0.0169(4) Uani 1 1 d . . . . .
H21 H 0.4623 0.4924 0.1127 0.020 Uiso 1 1 calc R U . . .
C22 C 0.5766(2) 0.54145(13) 0.18815(13) 0.0182(4) Uani 1 1 d . . . . .
H22 H 0.5568 0.6054 0.1847 0.022 Uiso 1 1 calc R U . . .
C23 C 0.66276(19) 0.49348(13) 0.23366(12) 0.0160(4) Uani 1 1 d . . . . .
C24 C 0.7441(2) 0.52503(14) 0.28471(13) 0.0194(4) Uani 1 1 d . . . . .
H24 H 0.7988 0.4811 0.3106 0.023 Uiso 1 1 calc R U . . .
C25 C 0.46362(18) 0.24120(12) 0.22772(12) 0.0122(3) Uani 1 1 d . . . . .
C26 C 0.32194(19) 0.22043(13) 0.25279(12) 0.0151(4) Uani 1 1 d . . . . .
H26 H 0.2549 0.2420 0.2224 0.018 Uiso 1 1 calc R U . . .
C27 C 0.29665(19) 0.16240(13) 0.33030(12) 0.0149(4) Uani 1 1 d . . . . .
H27 H 0.2093 0.1371 0.3625 0.018 Uiso 1 1 calc R U . . .
C28 C 0.42340(19) 0.14801(12) 0.35231(12) 0.0142(4) Uani 1 1 d . . . . .
C29 C 0.45250(19) 0.09390(12) 0.42472(12) 0.0143(4) Uani 1 1 d . . . . .
H29 H 0.3763 0.0628 0.4653 0.017 Uiso 1 1 calc R U . . .
C30 C 0.46172(19) 0.31777(13) 0.08169(12) 0.0154(4) Uani 1 1 d . . . . .
H30A H 0.3747 0.3481 0.1057 0.023 Uiso 1 1 calc R U . . .
H30B H 0.4410 0.2589 0.0664 0.023 Uiso 1 1 calc R U . . .
H30C H 0.5143 0.3574 0.0309 0.023 Uiso 1 1 calc R U . . .
C31 C 0.5392(2) 0.29570(13) 0.59698(12) 0.0170(4) Uani 1 1 d . . . . .
H31A H 0.6134 0.3431 0.5817 0.020 Uiso 1 1 calc R U . . .
H31B H 0.4606 0.3181 0.6391 0.020 Uiso 1 1 calc R U . . .
C32 C 0.4906(2) 0.28830(13) 0.51767(12) 0.0176(4) Uani 1 1 d . . . . .
H32A H 0.4100 0.2458 0.5324 0.021 Uiso 1 1 calc R U . . .
H32B H 0.5661 0.2634 0.4753 0.021 Uiso 1 1 calc R U . . .
C33 C 0.4495(2) 0.38370(14) 0.48041(13) 0.0215(4) Uani 1 1 d . . . . .
H33A H 0.3863 0.4123 0.5262 0.026 Uiso 1 1 calc R U . . .
H33B H 0.5338 0.4228 0.4583 0.026 Uiso 1 1 calc R U . . .
C34 C 0.3782(2) 0.38146(15) 0.40913(13) 0.0231(4) Uani 1 1 d . . . . .
H34A H 0.4395 0.3523 0.3640 0.035 Uiso 1 1 calc R U . . .
H34B H 0.3577 0.4445 0.3862 0.035 Uiso 1 1 calc R U . . .
H34C H 0.2915 0.3461 0.4314 0.035 Uiso 1 1 calc R U . . .
C35 C 0.7287(2) 0.18006(13) 0.58111(13) 0.0185(4) Uani 1 1 d . . . . .
H35A H 0.7887 0.2353 0.5591 0.022 Uiso 1 1 calc R U . . .
H35B H 0.7068 0.1584 0.5320 0.022 Uiso 1 1 calc R U . . .
C36 C 0.8106(2) 0.10499(14) 0.62243(14) 0.0235(4) Uani 1 1 d . . . . .
H36A H 0.7609 0.0454 0.6328 0.028 Uiso 1 1 calc R U . . .
H36B H 0.8166 0.1199 0.6779 0.028 Uiso 1 1 calc R U . . .
C37 C 0.9578(3) 0.09571(16) 0.56619(15) 0.0296(5) Uani 1 1 d . . . . .
H37A H 0.9995 0.0383 0.5887 0.036 Uiso 1 1 calc R U . . .
H37B H 0.9513 0.0900 0.5082 0.036 Uiso 1 1 calc R U . . .
C38 C 1.0535(2) 0.17616(18) 0.56077(15) 0.0311(5) Uani 1 1 d . . . . .
H38A H 1.0189 0.2323 0.5323 0.047 Uiso 1 1 calc R U . . .
H38B H 1.1473 0.1631 0.5284 0.047 Uiso 1 1 calc R U . . .
H38C H 1.0559 0.1850 0.6181 0.047 Uiso 1 1 calc R U . . .
C39 C 0.4908(2) 0.12845(13) 0.65788(13) 0.0177(4) Uani 1 1 d . . . . .
H39A H 0.4790 0.1149 0.6031 0.021 Uiso 1 1 calc R U . . .
H39B H 0.5322 0.0732 0.6846 0.021 Uiso 1 1 calc R U . . .
C40 C 0.3483(2) 0.14291(14) 0.71439(14) 0.0226(4) Uani 1 1 d . . . . .
H40A H 0.3063 0.1995 0.6904 0.027 Uiso 1 1 calc R U . . .
H40B H 0.3564 0.1505 0.7716 0.027 Uiso 1 1 calc R U . . .
C41 C 0.2562(2) 0.05992(15) 0.72081(15) 0.0253(5) Uani 1 1 d . . . . .
H41A H 0.2446 0.0552 0.6637 0.030 Uiso 1 1 calc R U . . .
H41B H 0.3029 0.0032 0.7404 0.030 Uiso 1 1 calc R U . . .
C42 C 0.1137(2) 0.06567(17) 0.78126(16) 0.0317(5) Uani 1 1 d . . . . .
H42A H 0.1243 0.0696 0.8381 0.048 Uiso 1 1 calc R U . . .
H42B H 0.0595 0.0106 0.7834 0.048 Uiso 1 1 calc R U . . .
H42C H 0.0656 0.1206 0.7612 0.048 Uiso 1 1 calc R U . . .
C43 C 0.6154(2) 0.22629(13) 0.72380(12) 0.0189(4) Uani 1 1 d . . . . .
H43A H 0.6332 0.1668 0.7568 0.023 Uiso 1 1 calc R U . . .
H43B H 0.5284 0.2516 0.7564 0.023 Uiso 1 1 calc R U . . .
C44 C 0.7347(2) 0.29274(14) 0.71636(13) 0.0222(4) Uani 1 1 d . . . . .
H44A H 0.7001 0.3569 0.7115 0.027 Uiso 1 1 calc R U . . .
H44B H 0.8084 0.2870 0.6643 0.027 Uiso 1 1 calc R U . . .
C45 C 0.7955(2) 0.27211(15) 0.79389(14) 0.0258(5) Uani 1 1 d . . . . .
H45A H 0.8312 0.2083 0.7977 0.031 Uiso 1 1 calc R U . . .
H45B H 0.8748 0.3142 0.7859 0.031 Uiso 1 1 calc R U . . .
C46 C 0.6912(2) 0.28274(16) 0.87636(15) 0.0285(5) Uani 1 1 d . . . . .
H46A H 0.6529 0.3452 0.8725 0.043 Uiso 1 1 calc R U . . .
H46B H 0.7371 0.2722 0.9230 0.043 Uiso 1 1 calc R U . . .
H46C H 0.6159 0.2378 0.8871 0.043 Uiso 1 1 calc R U . . .
C47 C 0.0335(4) 0.5024(3) 0.4640(3) 0.0335(11) Uani 0.5 1 d D . P A -1
H47 H 0.0953 0.4643 0.4246 0.040 Uiso 0.5 1 calc R U P A -1
Cl1 Cl -0.06275(12) 0.57706(8) 0.40652(8) 0.0342(3) Uani 0.5 1 d D . P A -1
Cl2 Cl 0.13840(12) 0.56665(8) 0.50788(7) 0.0312(2) Uani 0.5 1 d D . P A -1
Cl3 Cl -0.07643(17) 0.42923(10) 0.54494(11) 0.0578(4) Uani 0.5 1 d D . P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O5 1.4944(14) . ?
P1 O6 1.4998(13) . ?
P1 O7 1.5763(14) . ?
P1 O8 1.5864(13) . ?
O1 C1 1.228(2) . ?
O2 C11 1.226(3) . ?
O3 C24 1.223(2) . ?
O4 C29 1.241(2) . ?
O7 H7O 0.83(3) . ?
O8 H8O 0.81(3) . ?
N1 C5 1.352(2) . ?
N1 C2 1.383(2) . ?
N1 H1N 0.85(3) . ?
N2 C7 1.363(2) . ?
N2 C10 1.384(2) . ?
N2 H2N 0.95(3) . ?
N3 C20 1.359(2) . ?
N3 C23 1.380(2) . ?
N3 H3N 0.90(3) . ?
N4 C25 1.354(2) . ?
N4 C28 1.382(2) . ?
N4 H4N 0.87(3) . ?
N5 C31 1.519(2) . ?
N5 C35 1.525(2) . ?
N5 C39 1.525(2) . ?
N5 C43 1.526(2) . ?
C1 C2 1.433(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(3) . ?
C3 C4 1.402(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.521(2) . ?
C6 C7 1.521(2) . ?
C6 C12 1.539(2) . ?
C6 C13 1.543(2) . ?
C7 C8 1.393(3) . ?
C8 C9 1.397(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.428(3) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.393(3) . ?
C13 C14 1.403(2) . ?
C14 C15 1.394(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(2) . ?
C15 C19 1.539(2) . ?
C16 C17 1.386(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.517(2) . ?
C19 C25 1.524(3) . ?
C19 C30 1.546(2) . ?
C20 C21 1.395(3) . ?
C21 C22 1.396(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.440(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(3) . ?
C26 C27 1.391(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.400(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.416(3) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.525(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.526(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.524(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.527(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.536(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.522(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.515(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.526(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.520(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.532(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.533(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.512(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 Cl3 1.739(4) . ?
C47 Cl1 1.757(4) . ?
C47 Cl2 1.781(4) . ?
C47 H47 1.0000 . ?

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
O5 P1 O6 116.22(8) . . ?
O5 P1 O7 109.92(8) . . ?
O6 P1 O7 109.33(8) . . ?
O5 P1 O8 109.29(8) . . ?
O6 P1 O8 109.76(8) . . ?
O7 P1 O8 101.29(8) . . ?
P1 O7 H7O 113(2) . . ?
P1 O8 H8O 109(2) . . ?
C5 N1 C2 109.67(16) . . ?
C5 N1 H1N 125.2(16) . . ?
C2 N1 H1N 125.1(17) . . ?
C7 N2 C10 108.77(16) . . ?
C7 N2 H2N 125.9(16) . . ?
C10 N2 H2N 125.2(16) . . ?
C20 N3 C23 109.47(15) . . ?
C20 N3 H3N 125.8(17) . . ?
C23 N3 H3N 124.5(17) . . ?
C25 N4 C28 109.51(15) . . ?
C25 N4 H4N 124.3(18) . . ?
C28 N4 H4N 125.5(18) . . ?
C31 N5 C35 109.56(15) . . ?
C31 N5 C39 111.73(15) . . ?
C35 N5 C39 108.07(14) . . ?
C31 N5 C43 108.09(14) . . ?
C35 N5 C43 111.53(15) . . ?
C39 N5 C43 107.89(15) . . ?
O1 C1 C2 125.25(19) . . ?
O1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?
N1 C2 C3 107.56(16) . . ?
N1 C2 C1 119.94(17) . . ?
C3 C2 C1 132.50(17) . . ?
C2 C3 C4 107.02(16) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
C5 C4 C3 107.84(16) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
N1 C5 C4 107.91(15) . . ?
N1 C5 C6 121.81(16) . . ?
C4 C5 C6 130.28(16) . . ?
C5 C6 C7 107.85(14) . . ?
C5 C6 C12 109.10(14) . . ?
C7 C6 C12 109.19(15) . . ?
C5 C6 C13 109.66(14) . . ?
C7 C6 C13 113.39(14) . . ?
C12 C6 C13 107.60(14) . . ?
N2 C7 C8 108.64(16) . . ?
N2 C7 C6 122.32(16) . . ?
C8 C7 C6 128.83(17) . . ?
C7 C8 C9 107.12(17) . . ?
C7 C8 H8 126.4 . . ?
C9 C8 H8 126.4 . . ?
C10 C9 C8 107.85(16) . . ?
C10 C9 H9 126.1 . . ?
C8 C9 H9 126.1 . . ?
N2 C10 C9 107.62(16) . . ?
N2 C10 C11 124.87(18) . . ?
C9 C10 C11 127.45(17) . . ?
O2 C11 C10 127.41(18) . . ?
O2 C11 H11 116.3 . . ?
C10 C11 H11 116.3 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 118.61(16) . . ?
C18 C13 C6 118.80(16) . . ?
C14 C13 C6 122.47(15) . . ?
C15 C14 C13 121.18(16) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 118.78(16) . . ?
C14 C15 C19 123.72(15) . . ?
C16 C15 C19 117.40(15) . . ?
C17 C16 C15 120.53(17) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 120.23(17) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C13 120.64(17) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C20 C19 C25 108.89(14) . . ?
C20 C19 C15 114.37(14) . . ?
C25 C19 C15 109.00(14) . . ?
C20 C19 C30 108.17(14) . . ?
C25 C19 C30 108.84(14) . . ?
C15 C19 C30 107.45(14) . . ?
N3 C20 C21 107.69(16) . . ?
N3 C20 C19 123.44(16) . . ?
C21 C20 C19 128.78(16) . . ?
C20 C21 C22 107.62(17) . . ?
C20 C21 H21 126.2 . . ?
C22 C21 H21 126.2 . . ?
C23 C22 C21 107.59(17) . . ?
C23 C22 H22 126.2 . . ?
C21 C22 H22 126.2 . . ?
N3 C23 C22 107.63(16) . . ?
N3 C23 C24 121.90(17) . . ?
C22 C23 C24 130.46(18) . . ?
O3 C24 C23 124.00(19) . . ?
O3 C24 H24 118.0 . . ?
C23 C24 H24 118.0 . . ?
N4 C25 C26 108.16(16) . . ?
N4 C25 C19 121.57(16) . . ?
C26 C25 C19 130.26(16) . . ?
C27 C26 C25 107.61(16) . . ?
C27 C26 H26 126.2 . . ?
C25 C26 H26 126.2 . . ?
C26 C27 C28 107.53(16) . . ?
C26 C27 H27 126.2 . . ?
C28 C27 H27 126.2 . . ?
N4 C28 C27 107.19(16) . . ?
N4 C28 C29 123.52(16) . . ?
C27 C28 C29 129.29(18) . . ?
O4 C29 C28 126.10(18) . . ?
O4 C29 H29 116.9 . . ?
C28 C29 H29 116.9 . . ?
C19 C30 H30A 109.5 . . ?
C19 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C19 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 C32 116.49(15) . . ?
N5 C31 H31A 108.2 . . ?
C32 C31 H31A 108.2 . . ?
N5 C31 H31B 108.2 . . ?
C32 C31 H31B 108.2 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 C33 109.15(15) . . ?
C31 C32 H32A 109.9 . . ?
C33 C32 H32A 109.9 . . ?
C31 C32 H32B 109.9 . . ?
C33 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
C34 C33 C32 113.07(16) . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 C36 115.09(17) . . ?
N5 C35 H35A 108.5 . . ?
C36 C35 H35A 108.5 . . ?
N5 C35 H35B 108.5 . . ?
C36 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C35 C36 C37 111.53(18) . . ?
C35 C36 H36A 109.3 . . ?
C37 C36 H36A 109.3 . . ?
C35 C36 H36B 109.3 . . ?
C37 C36 H36B 109.3 . . ?
H36A C36 H36B 108.0 . . ?
C38 C37 C36 113.92(18) . . ?
C38 C37 H37A 108.8 . . ?
C36 C37 H37A 108.8 . . ?
C38 C37 H37B 108.8 . . ?
C36 C37 H37B 108.8 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N5 116.46(15) . . ?
C40 C39 H39A 108.2 . . ?
N5 C39 H39A 108.2 . . ?
C40 C39 H39B 108.2 . . ?
N5 C39 H39B 108.2 . . ?
H39A C39 H39B 107.3 . . ?
C39 C40 C41 109.36(16) . . ?
C39 C40 H40A 109.8 . . ?
C41 C40 H40A 109.8 . . ?
C39 C40 H40B 109.8 . . ?
C41 C40 H40B 109.8 . . ?
H40A C40 H40B 108.2 . . ?
C42 C41 C40 112.90(18) . . ?
C42 C41 H41A 109.0 . . ?
C40 C41 H41A 109.0 . . ?
C42 C41 H41B 109.0 . . ?
C40 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C43 C44 114.92(16) . . ?
N5 C43 H43A 108.5 . . ?
C44 C43 H43A 108.5 . . ?
N5 C43 H43B 108.5 . . ?
C44 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C43 C44 C45 110.98(17) . . ?
C43 C44 H44A 109.4 . . ?
C45 C44 H44A 109.4 . . ?
C43 C44 H44B 109.4 . . ?
C45 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
C46 C45 C44 113.18(18) . . ?
C46 C45 H45A 108.9 . . ?
C44 C45 H45A 108.9 . . ?
C46 C45 H45B 108.9 . . ?
C44 C45 H45B 108.9 . . ?
H45A C45 H45B 107.8 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Cl3 C47 Cl1 110.6(2) . . ?
Cl3 C47 Cl2 109.7(2) . . ?
Cl1 C47 Cl2 110.3(2) . . ?
Cl3 C47 H47 108.7 . . ?
Cl1 C47 H47 108.7 . . ?
Cl2 C47 H47 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C2 C3 -0.1(2) . . . . ?
C5 N1 C2 C1 179.52(16) . . . . ?
O1 C1 C2 N1 -177.32(18) . . . . ?
O1 C1 C2 C3 2.2(3) . . . . ?
N1 C2 C3 C4 -0.1(2) . . . . ?
C1 C2 C3 C4 -179.68(19) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C2 N1 C5 C4 0.30(19) . . . . ?
C2 N1 C5 C6 -179.67(15) . . . . ?
C3 C4 C5 N1 -0.3(2) . . . . ?
C3 C4 C5 C6 179.61(17) . . . . ?
N1 C5 C6 C7 74.2(2) . . . . ?
C4 C5 C6 C7 -105.7(2) . . . . ?
N1 C5 C6 C12 -167.30(15) . . . . ?
C4 C5 C6 C12 12.7(2) . . . . ?
N1 C5 C6 C13 -49.7(2) . . . . ?
C4 C5 C6 C13 130.36(19) . . . . ?
C10 N2 C7 C8 -0.4(2) . . . . ?
C10 N2 C7 C6 174.68(15) . . . . ?
C5 C6 C7 N2 -67.4(2) . . . . ?
C12 C6 C7 N2 174.13(15) . . . . ?
C13 C6 C7 N2 54.2(2) . . . . ?
C5 C6 C7 C8 106.6(2) . . . . ?
C12 C6 C7 C8 -11.9(2) . . . . ?
C13 C6 C7 C8 -131.83(19) . . . . ?
N2 C7 C8 C9 0.4(2) . . . . ?
C6 C7 C8 C9 -174.23(17) . . . . ?
C7 C8 C9 C10 -0.3(2) . . . . ?
C7 N2 C10 C9 0.2(2) . . . . ?
C7 N2 C10 C11 -177.24(17) . . . . ?
C8 C9 C10 N2 0.1(2) . . . . ?
C8 C9 C10 C11 177.41(18) . . . . ?
N2 C10 C11 O2 -1.3(3) . . . . ?
C9 C10 C11 O2 -178.2(2) . . . . ?
C5 C6 C13 C18 -38.2(2) . . . . ?
C7 C6 C13 C18 -158.79(16) . . . . ?
C12 C6 C13 C18 80.4(2) . . . . ?
C5 C6 C13 C14 145.90(16) . . . . ?
C7 C6 C13 C14 25.3(2) . . . . ?
C12 C6 C13 C14 -95.56(19) . . . . ?
C18 C13 C14 C15 1.1(3) . . . . ?
C6 C13 C14 C15 177.00(16) . . . . ?
C13 C14 C15 C16 0.0(3) . . . . ?
C13 C14 C15 C19 -176.36(16) . . . . ?
C14 C15 C16 C17 -1.5(3) . . . . ?
C19 C15 C16 C17 175.10(17) . . . . ?
C15 C16 C17 C18 1.9(3) . . . . ?
C16 C17 C18 C13 -0.8(3) . . . . ?
C14 C13 C18 C17 -0.6(3) . . . . ?
C6 C13 C18 C17 -176.73(17) . . . . ?
C14 C15 C19 C20 -13.6(2) . . . . ?
C16 C15 C19 C20 170.06(16) . . . . ?
C14 C15 C19 C25 -135.70(17) . . . . ?
C16 C15 C19 C25 47.9(2) . . . . ?
C14 C15 C19 C30 106.52(19) . . . . ?
C16 C15 C19 C30 -69.9(2) . . . . ?
C23 N3 C20 C21 0.5(2) . . . . ?
C23 N3 C20 C19 -176.34(16) . . . . ?
C25 C19 C20 N3 67.6(2) . . . . ?
C15 C19 C20 N3 -54.6(2) . . . . ?
C30 C19 C20 N3 -174.29(16) . . . . ?
C25 C19 C20 C21 -108.6(2) . . . . ?
C15 C19 C20 C21 129.3(2) . . . . ?
C30 C19 C20 C21 9.6(3) . . . . ?
N3 C20 C21 C22 -0.4(2) . . . . ?
C19 C20 C21 C22 176.20(18) . . . . ?
C20 C21 C22 C23 0.2(2) . . . . ?
C20 N3 C23 C22 -0.4(2) . . . . ?
C20 N3 C23 C24 -179.32(17) . . . . ?
C21 C22 C23 N3 0.1(2) . . . . ?
C21 C22 C23 C24 178.9(2) . . . . ?
N3 C23 C24 O3 179.75(19) . . . . ?
C22 C23 C24 O3 1.1(4) . . . . ?
C28 N4 C25 C26 -0.2(2) . . . . ?
C28 N4 C25 C19 -179.25(15) . . . . ?
C20 C19 C25 N4 -78.1(2) . . . . ?
C15 C19 C25 N4 47.2(2) . . . . ?
C30 C19 C25 N4 164.14(16) . . . . ?
C20 C19 C25 C26 103.0(2) . . . . ?
C15 C19 C25 C26 -131.62(19) . . . . ?
C30 C19 C25 C26 -14.7(3) . . . . ?
N4 C25 C26 C27 0.1(2) . . . . ?
C19 C25 C26 C27 179.06(17) . . . . ?
C25 C26 C27 C28 0.0(2) . . . . ?
C25 N4 C28 C27 0.2(2) . . . . ?
C25 N4 C28 C29 179.61(16) . . . . ?
C26 C27 C28 N4 -0.1(2) . . . . ?
C26 C27 C28 C29 -179.51(18) . . . . ?
N4 C28 C29 O4 0.0(3) . . . . ?
C27 C28 C29 O4 179.25(18) . . . . ?
C35 N5 C31 C32 66.9(2) . . . . ?
C39 N5 C31 C32 -52.8(2) . . . . ?
C43 N5 C31 C32 -171.35(17) . . . . ?
N5 C31 C32 C33 -175.94(17) . . . . ?
C31 C32 C33 C34 -170.97(18) . . . . ?
C31 N5 C35 C36 167.97(16) . . . . ?
C39 N5 C35 C36 -70.1(2) . . . . ?
C43 N5 C35 C36 48.3(2) . . . . ?
N5 C35 C36 C37 -167.79(16) . . . . ?
C35 C36 C37 C38 70.8(2) . . . . ?
C31 N5 C39 C40 -58.7(2) . . . . ?
C35 N5 C39 C40 -179.32(16) . . . . ?
C43 N5 C39 C40 60.0(2) . . . . ?
N5 C39 C40 C41 175.89(16) . . . . ?
C39 C40 C41 C42 176.12(18) . . . . ?
C31 N5 C43 C44 -69.2(2) . . . . ?
C35 N5 C43 C44 51.3(2) . . . . ?
C39 N5 C43 C44 169.83(16) . . . . ?
N5 C43 C44 C45 -152.03(17) . . . . ?
C43 C44 C45 C46 -61.2(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
C3 H3 O1 0.95 2.63 3.452(2) 144.8 2_855
C26 H26 O5 0.95 2.59 3.297(2) 131.4 1_455
C29 H29 O4 0.95 2.58 3.127(2) 117.0 2_656
C31 H31A Cl2 0.99 2.79 3.732(2) 158.1 2_666
C31 H31B O3 0.99 2.40 3.362(2) 162.7 2_666
C43 H43A O1 0.99 2.30 3.260(2) 162.3 2_756
C44 H44B Cl3 0.99 2.70 3.367(3) 125.0 1_655
C47 H47 O2 1.00 2.44 3.233(5) 135.8 1_455
N2 H2N O5 0.95(3) 1.82(3) 2.760(2) 171(2) .
N1 H1N O5 0.85(3) 1.90(3) 2.730(2) 166(2) .
N3 H3N O6 0.90(3) 1.82(3) 2.704(2) 171(3) .
N4 H4N O6 0.87(3) 1.87(3) 2.704(2) 162(3) .
O7 H7O O4 0.83(3) 1.85(3) 2.6814(19) 175(3) .
O8 H8O O2 0.81(3) 1.92(3) 2.726(2) 171(3) .

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.063



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1444561'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0104 Ang.  
RESPONSE: The structure suffers from a large amount of disordered solvent 
and highly anisotropic cations.
;
_vrf_PLAT410_shelx               
;
PROBLEM: Short Intra H...H Contact  H10D   ..  H13A    ..       1.87 Ang.  
RESPONSE: These 'short' H...H contacts are bound to the carbon atoms of the 
highly anisotropic alkyl chains on the cations and have high associated 
standard uncertainties. 
;
_vrf_PLAT413_shelx               
;
PROBLEM: Short Inter XH3 .. XHn     H4B1   ..  H12D    ..       1.90 Ang.  
RESPONSE: see above
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact  O1     ..  O3A     ..       2.76 Ang.  
RESPONSE: This is an H-bonding interaction between a carbonyl oxygen atom, O1, 
and a hydroxy oxygen atom on the anion.  The hydrogen atoms on the 
dihydrogen phosphate anions could not be located in a difference 
electron density map and were not included in the refinement model.
;
# end Validation Reply Form




_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2 C42 H36 N6 O6, 2 C16 H36 N, 2 H2 P O4, 3 C H Cl3'

_chemical_formula_sum            'C119 H151 Cl9 N14 O20 P2'
_chemical_formula_weight         2478.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.0755(7)
_cell_length_b                   18.9299(7)
_cell_length_c                   24.4976(6)
_cell_angle_alpha                93.415(2)
_cell_angle_beta                 96.103(3)
_cell_angle_gamma                111.261(4)
_cell_volume                     6869.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6140
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      72.7

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_F_000             2612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.423
_shelx_estimated_absorpt_T_min   0.561
_shelx_estimated_absorpt_T_max   0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed microfocus tube'
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40560
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.950
_diffrn_reflns_theta_max         74.200
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             26292
_reflns_number_gt                14638
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;



_computing_data_collection       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'

_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'

_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 two tetrakis-n-butyl ammonium ions had highly anisotropic 
displacement parameters.  One of the ions was refined with a disorder model.  
The disorder was modeled by assigning the variable x to the site occupancy 
for one component of the disorder and (1-x) to the site occupancy for 
the alternate component.  The geometry of the two components was restrained by 
the extensive use of SADI instructions to maintain the C-C bonds and C-C-C 
angles to be equivalent.  A common isotropic displacement parameter was 
assigned to the nitrogen atoms and the methylene carbon atoms while refining 
the variable x.  A separate isotropic displacement parameter was refined 
for the methyl carbon atoms.

  There are several regions of unidentified disordered solvent.  The solvent 
was badly disordered and could not be reliably identified but was probably a 
mixture of the solvents used for crystallization, chloroform and n-hexane.  
The quantity and identity of the solvent in these voids was in doubt.  The 
squeezed out solvent was not included in the UNIT card.  The contributions to the 
scattering factors due to these solvent molecules were removed by use of 
the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998).  
PLATON98 was used as incorporated in WinGX (Farrugia, 1999). 

;

# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.039 0.164 0.234 348 112 ' '
2 0.039 -0.164 0.766 349 112 ' '
3 0.000 0.500 0.500 57 15 ' '
4 0.103 0.921 0.469 19 2 ' '
5 0.362 0.814 0.462 77 16 ' '
6 0.638 0.186 0.538 76 16 ' '
7 0.897 0.078 0.531 19 1 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?




_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26292
_refine_ls_number_parameters     1638
_refine_ls_number_restraints     3337
_refine_ls_R_factor_all          0.1811
_refine_ls_R_factor_gt           0.1255
_refine_ls_wR_factor_ref         0.3446
_refine_ls_wR_factor_gt          0.3052
_refine_ls_goodness_of_fit_ref   1.544
_refine_ls_restrained_S_all      1.606
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P2 P 0.62939(10) 0.55773(8) 0.26925(6) 0.0418(3) Uani 1 1 d . U . . .
O5A O 0.6189(3) 0.5333(2) 0.32583(17) 0.0482(10) Uani 1 1 d . U . . .
O6A O 0.7011(3) 0.6418(2) 0.27664(19) 0.0537(11) Uani 1 1 d . U . . .
O7A O 0.5478(3) 0.5528(2) 0.23109(17) 0.0448(9) Uani 1 1 d . U . . .
O8A O 0.6750(3) 0.5062(2) 0.23936(17) 0.0480(10) Uani 1 1 d . U . . .
P1 P 0.25598(11) 0.80335(8) 0.22298(6) 0.0414(3) Uani 1 1 d . U . . .
O1A O 0.2734(3) 0.8214(2) 0.16569(16) 0.0475(10) Uani 1 1 d . U . . .
O2A O 0.1767(3) 0.7227(2) 0.21654(17) 0.0448(9) Uani 1 1 d . U . . .
O3A O 0.2153(3) 0.8632(2) 0.24600(17) 0.0472(10) Uani 1 1 d . U . . .
O4A O 0.3328(3) 0.8059(2) 0.26404(17) 0.0476(9) Uani 1 1 d . U . . .
O7 O 0.7195(4) 0.3180(3) 0.1475(2) 0.0718(15) Uani 1 1 d . U . . .
O8 O 0.8017(6) 0.5930(5) 0.4412(4) 0.128(3) Uani 1 1 d . U . . .
O9 O 0.1500(3) 0.6418(3) 0.30024(18) 0.0518(10) Uani 1 1 d . U . . .
O10 O 0.7468(3) 0.7644(3) 0.4313(2) 0.0640(13) Uani 1 1 d . U . . .
O11 O 0.4405(3) 0.6829(2) 0.18036(18) 0.0485(10) Uani 1 1 d . U . . .
O12 O 0.6427(3) 0.4773(3) 0.12866(18) 0.0601(12) Uani 1 1 d . U . . .
N7 N 0.6286(3) 0.3467(3) 0.27200(19) 0.0429(11) Uani 1 1 d . U . . .
H7N H 0.6490 0.3965 0.2797 0.051 Uiso 1 1 calc R U . . .
N8 N 0.6690(4) 0.4406(3) 0.3969(2) 0.0555(13) Uani 1 1 d . U . . .
H8N H 0.6541 0.4715 0.3759 0.067 Uiso 1 1 calc R U . . .
N9 N 0.3154(3) 0.5772(3) 0.36567(18) 0.0379(10) Uani 1 1 d . U . . .
H9N H 0.3665 0.6096 0.3576 0.045 Uiso 1 1 calc R U . . .
N10 N 0.5470(3) 0.5925(3) 0.40679(18) 0.0396(10) Uani 1 1 d . U . . .
H10N H 0.5578 0.5642 0.3807 0.047 Uiso 1 1 calc R U . . .
N11 N 0.3623(3) 0.5249(2) 0.20321(18) 0.0372(9) Uani 1 1 d . U . . .
H11N H 0.4210 0.5372 0.2066 0.045 Uiso 1 1 calc R U . . .
N12 N 0.4638(3) 0.4173(3) 0.16645(18) 0.0405(10) Uani 1 1 d . U . . .
H12N H 0.4950 0.4601 0.1875 0.049 Uiso 1 1 calc R U . . .
C43 C 0.4811(4) 0.3650(3) 0.3386(2) 0.0364(11) Uani 1 1 d . U . . .
C44 C 0.4640(4) 0.4095(3) 0.3811(2) 0.0359(11) Uani 1 1 d . U . . .
H44 H 0.4916 0.4131 0.4180 0.043 Uiso 1 1 calc R U . . .
C45 C 0.4058(4) 0.4484(3) 0.3686(2) 0.0339(10) Uani 1 1 d . U . . .
C46 C 0.3653(4) 0.4417(3) 0.3153(2) 0.0355(11) Uani 1 1 d . U . . .
H46 H 0.3265 0.4684 0.3069 0.043 Uiso 1 1 calc R U . . .
C47 C 0.3800(4) 0.3965(3) 0.2735(2) 0.0357(10) Uani 1 1 d . U . . .
C48 C 0.4380(4) 0.3588(3) 0.2854(2) 0.0365(11) Uani 1 1 d . U . . .
H48 H 0.4483 0.3281 0.2568 0.044 Uiso 1 1 calc R U . . .
C49 C 0.5416(4) 0.3202(3) 0.3531(2) 0.0425(12) Uani 1 1 d . U . . .
C50 C 0.5747(4) 0.2957(3) 0.3019(2) 0.0454(13) Uani 1 1 d . U . . .
C51 C 0.5578(5) 0.2228(4) 0.2766(3) 0.0537(15) Uani 1 1 d . U . . .
H51 H 0.5220 0.1760 0.2888 0.064 Uiso 1 1 calc R U . . .
C52 C 0.6024(5) 0.2310(4) 0.2306(3) 0.0570(16) Uani 1 1 d . U . . .
H52 H 0.6024 0.1906 0.2056 0.068 Uiso 1 1 calc R U . . .
C53 C 0.6472(4) 0.3084(4) 0.2271(2) 0.0495(14) Uani 1 1 d . U . . .
C54 C 0.7049(5) 0.3485(4) 0.1893(3) 0.0604(17) Uani 1 1 d . U . . .
H54 H 0.7337 0.4023 0.1970 0.073 Uiso 1 1 calc R U . . .
C55 C 0.6232(4) 0.3637(4) 0.3947(2) 0.0495(13) Uani 1 1 d . U . . .
C56 C 0.6684(5) 0.3367(5) 0.4340(3) 0.0610(16) Uani 1 1 d . U . . .
H56 H 0.6520 0.2852 0.4419 0.073 Uiso 1 1 calc R U . . .
C57 C 0.7445(6) 0.4000(5) 0.4606(3) 0.0749(19) Uani 1 1 d . U . . .
H57 H 0.7882 0.3985 0.4894 0.090 Uiso 1 1 calc R U . . .
C58 C 0.7431(5) 0.4618(5) 0.4376(3) 0.0658(17) Uani 1 1 d . U . . .
C59 C 0.8075(7) 0.5408(7) 0.4555(5) 0.095(3) Uani 1 1 d . U . . .
H59 H 0.8583 0.5468 0.4816 0.114 Uiso 1 1 calc R U . . .
C60 C 0.4841(5) 0.2476(3) 0.3779(2) 0.0501(14) Uani 1 1 d . U . . .
H60A H 0.5208 0.2174 0.3873 0.075 Uiso 1 1 calc R U . . .
H60B H 0.4321 0.2171 0.3508 0.075 Uiso 1 1 calc R U . . .
H60C H 0.4631 0.2624 0.4113 0.075 Uiso 1 1 calc R U . . .
C61 C 0.3899(4) 0.4991(3) 0.4153(2) 0.0339(10) Uani 1 1 d . U . . .
C62 C 0.3080(4) 0.5181(3) 0.3955(2) 0.0382(11) Uani 1 1 d . U . . .
C63 C 0.2171(4) 0.4813(4) 0.3994(2) 0.0455(13) Uani 1 1 d . U . . .
H63 H 0.1916 0.4373 0.4179 0.055 Uiso 1 1 calc R U . . .
C64 C 0.1697(4) 0.5200(4) 0.3715(2) 0.0500(14) Uani 1 1 d . U . . .
H64 H 0.1065 0.5076 0.3682 0.060 Uiso 1 1 calc R U . . .
C65 C 0.2312(4) 0.5798(3) 0.3493(2) 0.0417(12) Uani 1 1 d . U . . .
C66 C 0.2231(4) 0.6355(3) 0.3164(2) 0.0442(12) Uani 1 1 d . U . . .
H66 H 0.2764 0.6707 0.3056 0.053 Uiso 1 1 calc R U . . .
C67 C 0.4700(4) 0.5733(3) 0.4298(2) 0.0362(11) Uani 1 1 d . U . . .
C68 C 0.4800(4) 0.6347(3) 0.4689(2) 0.0409(12) Uani 1 1 d . U . . .
H68 H 0.4363 0.6373 0.4913 0.049 Uiso 1 1 calc R U . . .
C69 C 0.5632(4) 0.6898(3) 0.4688(2) 0.0431(12) Uani 1 1 d . U . . .
H69 H 0.5871 0.7375 0.4909 0.052 Uiso 1 1 calc R U . . .
C70 C 0.6067(4) 0.6640(3) 0.4307(2) 0.0399(12) Uani 1 1 d . U . . .
C71 C 0.6932(4) 0.7004(4) 0.4127(3) 0.0534(15) Uani 1 1 d . U . . .
H71 H 0.7099 0.6733 0.3847 0.064 Uiso 1 1 calc R U . . .
C72 C 0.3701(4) 0.4567(3) 0.4668(2) 0.0397(12) Uani 1 1 d . U . . .
H72A H 0.4223 0.4448 0.4809 0.060 Uiso 1 1 calc R U . . .
H72B H 0.3174 0.4093 0.4570 0.060 Uiso 1 1 calc R U . . .
H72C H 0.3579 0.4889 0.4952 0.060 Uiso 1 1 calc R U . . .
C73 C 0.3254(4) 0.3858(3) 0.2157(2) 0.0384(11) Uani 1 1 d . U . . .
C74 C 0.3001(4) 0.4533(3) 0.2050(2) 0.0358(10) Uani 1 1 d . U . . .
C75 C 0.2151(4) 0.4570(4) 0.1978(2) 0.0460(13) Uani 1 1 d . U . . .
H75 H 0.1594 0.4155 0.1968 0.055 Uiso 1 1 calc R U . . .
C76 C 0.2266(4) 0.5343(3) 0.1919(2) 0.0443(12) Uani 1 1 d . U . . .
H76 H 0.1800 0.5539 0.1867 0.053 Uiso 1 1 calc R U . . .
C77 C 0.3175(4) 0.5751(3) 0.1952(2) 0.0367(11) Uani 1 1 d . U . . .
C78 C 0.3614(4) 0.6536(3) 0.1862(2) 0.0421(12) Uani 1 1 d . U . . .
H78 H 0.3263 0.6847 0.1847 0.051 Uiso 1 1 calc R U . . .
C79 C 0.3780(4) 0.3699(3) 0.1707(2) 0.0401(12) Uani 1 1 d . U . . .
C80 C 0.3519(4) 0.3090(3) 0.1304(2) 0.0471(13) Uani 1 1 d . U . . .
H80 H 0.2952 0.2679 0.1240 0.057 Uiso 1 1 calc R U . . .
C81 C 0.4243(5) 0.3189(4) 0.1009(2) 0.0504(14) Uani 1 1 d . U . . .
H81 H 0.4260 0.2855 0.0709 0.060 Uiso 1 1 calc R U . . .
C82 C 0.4935(4) 0.3865(4) 0.1234(2) 0.0486(14) Uani 1 1 d . U . . .
C83 C 0.5811(5) 0.4193(4) 0.1072(2) 0.0540(15) Uani 1 1 d . U . . .
H83 H 0.5928 0.3931 0.0764 0.065 Uiso 1 1 calc R U . . .
C84 C 0.2384(4) 0.3154(3) 0.2141(2) 0.0454(13) Uani 1 1 d . U . . .
H84A H 0.2059 0.3226 0.2443 0.068 Uiso 1 1 calc R U . . .
H84B H 0.2536 0.2701 0.2183 0.068 Uiso 1 1 calc R U . . .
H84C H 0.2003 0.3084 0.1787 0.068 Uiso 1 1 calc R U . . .
O1 O 0.2433(4) 0.8795(4) 0.3598(2) 0.0803(17) Uani 1 1 d . U . . .
O2 O 0.4386(3) 0.6811(2) 0.30986(17) 0.0482(10) Uani 1 1 d . U . . .
O3 O 0.0147(5) 0.7684(4) 0.0369(4) 0.119(3) Uani 1 1 d . U . . .
O4 O 0.1402(5) 0.9677(3) 0.3108(3) 0.100(2) Uani 1 1 d . U . . .
O5 O 0.7255(3) 0.7270(3) 0.1961(2) 0.0724(15) Uani 1 1 d . U . . .
O6 O 0.1383(3) 0.6040(3) 0.0440(2) 0.0598(12) Uani 1 1 d . U . . .
N1 N 0.4216(4) 0.9462(3) 0.3270(2) 0.0494(12) Uani 1 1 d . U . . .
H1N H 0.3903 0.9050 0.3043 0.059 Uiso 1 1 calc R U . . .
N2 N 0.5200(3) 0.8397(3) 0.28919(19) 0.0442(11) Uani 1 1 d . U . . .
H2N H 0.4612 0.8272 0.2842 0.053 Uiso 1 1 calc R U . . .
N3 N 0.2133(4) 0.9164(3) 0.1087(2) 0.0515(12) Uani 1 1 d . U . . .
H3N H 0.2354 0.8917 0.1317 0.062 Uiso 1 1 calc R U . . .
N4 N 0.2528(4) 1.0240(3) 0.2254(2) 0.0490(12) Uani 1 1 d . U . . .
H4N H 0.2306 0.9738 0.2199 0.059 Uiso 1 1 calc R U . . .
N5 N 0.5626(4) 0.7892(3) 0.1253(2) 0.0477(11) Uani 1 1 d . U . . .
H5N H 0.5105 0.7554 0.1307 0.057 Uiso 1 1 calc R U . . .
N6 N 0.3420(3) 0.7706(3) 0.0812(2) 0.0452(11) Uani 1 1 d . U . . .
H6N H 0.3372 0.7880 0.1143 0.054 Uiso 1 1 calc R U . . .
C1 C 0.5020(4) 0.9685(3) 0.2199(2) 0.0433(12) Uani 1 1 d . U . . .
C2 C 0.4431(4) 1.0059(3) 0.2092(2) 0.0429(12) Uani 1 1 d . U . . .
H2 H 0.4329 1.0358 0.2383 0.051 Uiso 1 1 calc R U . . .
C3 C 0.3982(4) 0.9996(3) 0.1554(2) 0.0459(12) Uani 1 1 d . U . . .
C4 C 0.4161(4) 0.9559(3) 0.1132(2) 0.0450(13) Uani 1 1 d . U . . .
H4 H 0.3870 0.9519 0.0766 0.054 Uiso 1 1 calc R U . . .
C5 C 0.4750(4) 0.9186(3) 0.1234(2) 0.0443(12) Uani 1 1 d . U . . .
C6 C 0.5181(4) 0.9253(3) 0.1773(2) 0.0450(13) Uani 1 1 d . U . . .
H6 H 0.5588 0.9000 0.1848 0.054 Uiso 1 1 calc R U . . .
C7 C 0.5567(4) 0.9793(3) 0.2775(3) 0.0469(13) Uani 1 1 d . U . . .
C8 C 0.5052(4) 0.9928(3) 0.3230(3) 0.0503(14) Uani 1 1 d . U . . .
C9 C 0.5326(5) 1.0523(4) 0.3657(3) 0.0606(17) Uani 1 1 d . U . . .
H9 H 0.5887 1.0941 0.3723 0.073 Uiso 1 1 calc R U . . .
C10 C 0.4612(5) 1.0380(4) 0.3968(3) 0.068(2) Uani 1 1 d . U . . .
H10 H 0.4602 1.0679 0.4291 0.082 Uiso 1 1 calc R U . . .
C11 C 0.3912(5) 0.9715(4) 0.3715(3) 0.0632(18) Uani 1 1 d . U . . .
C12 C 0.3043(6) 0.9336(5) 0.3865(3) 0.075(2) Uani 1 1 d . U . . .
H12 H 0.2925 0.9520 0.4206 0.090 Uiso 1 1 calc R U . . .
C13 C 0.5829(4) 0.9106(3) 0.2886(2) 0.0472(13) Uani 1 1 d . U . . .
C14 C 0.6690(5) 0.9072(4) 0.2972(3) 0.0585(16) Uani 1 1 d . U . . .
H14 H 0.7248 0.9486 0.2981 0.070 Uiso 1 1 calc R U . . .
C15 C 0.6572(5) 0.8313(4) 0.3042(3) 0.0568(15) Uani 1 1 d . U . . .
H15 H 0.7034 0.8115 0.3111 0.068 Uiso 1 1 calc R U . . .
C16 C 0.5651(4) 0.7905(3) 0.2991(2) 0.0453(13) Uani 1 1 d . U . . .
C17 C 0.5194(4) 0.7117(3) 0.3074(2) 0.0456(13) Uani 1 1 d . U . . .
H17 H 0.5548 0.6811 0.3113 0.055 Uiso 1 1 calc R U . . .
C18 C 0.6450(5) 1.0508(4) 0.2785(3) 0.0549(15) Uani 1 1 d . U . . .
H18A H 0.6296 1.0957 0.2731 0.082 Uiso 1 1 calc R U . . .
H18B H 0.6779 1.0426 0.2488 0.082 Uiso 1 1 calc R U . . .
H18C H 0.6828 1.0590 0.3142 0.082 Uiso 1 1 calc R U . . .
C19 C 0.3346(5) 1.0419(3) 0.1417(2) 0.0470(13) Uani 1 1 d . U . . .
C20 C 0.2514(5) 0.9917(4) 0.1046(2) 0.0524(13) Uani 1 1 d . U . . .
C21 C 0.1961(6) 1.0087(5) 0.0641(3) 0.0694(19) Uani 1 1 d . U . . .
H21 H 0.2064 1.0577 0.0523 0.083 Uiso 1 1 calc R U . . .
C22 C 0.1228(7) 0.9416(5) 0.0435(3) 0.077(2) Uani 1 1 d . U . . .
H22 H 0.0746 0.9368 0.0157 0.093 Uiso 1 1 calc R U . . .
C23 C 0.1346(6) 0.8830(5) 0.0719(3) 0.0662(17) Uani 1 1 d . U . . .
C24 C 0.0833(6) 0.8020(5) 0.0668(4) 0.076(2) Uani 1 1 d . U . . .
H24 H 0.1065 0.7725 0.0895 0.091 Uiso 1 1 calc R U . . .
C25 C 0.3075(4) 1.0718(3) 0.1930(2) 0.0460(13) Uani 1 1 d . U . . .
C26 C 0.3281(5) 1.1466(3) 0.2151(2) 0.0513(15) Uani 1 1 d . U . . .
H26 H 0.3649 1.1915 0.2011 0.062 Uiso 1 1 calc R U . . .
C27 C 0.2839(5) 1.1430(3) 0.2625(3) 0.0521(15) Uani 1 1 d . U . . .
H27 H 0.2855 1.1853 0.2861 0.062 Uiso 1 1 calc R U . . .
C28 C 0.2380(5) 1.0669(3) 0.2682(3) 0.0523(15) Uani 1 1 d . U . . .
C29 C 0.1819(6) 1.0353(4) 0.3088(3) 0.0667(19) Uani 1 1 d . U . . .
H29 H 0.1767 1.0699 0.3367 0.080 Uiso 1 1 calc R U . . .
C30 C 0.3857(6) 1.1116(4) 0.1123(3) 0.066(2) Uani 1 1 d . U . . .
H30A H 0.4011 1.0943 0.0777 0.099 Uiso 1 1 calc R U . . .
H30B H 0.4410 1.1439 0.1363 0.099 Uiso 1 1 calc R U . . .
H30C H 0.3474 1.1410 0.1044 0.099 Uiso 1 1 calc R U . . .
C31 C 0.4954(4) 0.8731(3) 0.0759(2) 0.0455(12) Uani 1 1 d . U . . .
C32 C 0.5727(5) 0.8495(4) 0.0961(3) 0.0526(14) Uani 1 1 d . U . . .
C33 C 0.6667(5) 0.8894(4) 0.0984(4) 0.0707(19) Uani 1 1 d . U . . .
H33 H 0.6945 0.9346 0.0816 0.085 Uiso 1 1 calc R U . . .
C34 C 0.7107(5) 0.8520(5) 0.1287(4) 0.073(2) Uani 1 1 d . U . . .
H34 H 0.7741 0.8666 0.1370 0.088 Uiso 1 1 calc R U . . .
C35 C 0.6453(5) 0.7884(4) 0.1454(3) 0.0569(15) Uani 1 1 d . U . . .
C36 C 0.6533(5) 0.7310(4) 0.1784(3) 0.0565(15) Uani 1 1 d . U . . .
H36 H 0.5997 0.6937 0.1871 0.068 Uiso 1 1 calc R U . . .
C37 C 0.4123(4) 0.8016(3) 0.0534(2) 0.0471(13) Uani 1 1 d . U . . .
C38 C 0.3951(5) 0.7570(4) 0.0032(3) 0.0582(16) Uani 1 1 d . U . . .
H38 H 0.4339 0.7648 -0.0244 0.070 Uiso 1 1 calc R U . . .
C39 C 0.3116(5) 0.6997(4) 0.0005(3) 0.0575(16) Uani 1 1 d . U . . .
H39 H 0.2821 0.6617 -0.0296 0.069 Uiso 1 1 calc R U . . .
C40 C 0.2784(4) 0.7071(3) 0.0495(3) 0.0483(13) Uani 1 1 d . U . . .
C41 C 0.1954(4) 0.6622(4) 0.0695(3) 0.0486(13) Uani 1 1 d . U . . .
H41 H 0.1846 0.6789 0.1045 0.058 Uiso 1 1 calc R U . . .
C42 C 0.5222(5) 0.9214(4) 0.0284(3) 0.0578(17) Uani 1 1 d . U . . .
H42A H 0.5732 0.9687 0.0421 0.087 Uiso 1 1 calc R U . . .
H42B H 0.4710 0.9337 0.0126 0.087 Uiso 1 1 calc R U . . .
H42C H 0.5395 0.8929 -0.0001 0.087 Uiso 1 1 calc R U . . .
N1B N 0.9733(5) 0.7449(4) 0.3469(3) 0.128(2) Uani 1 1 d D U . . .
C1B C 0.9090(6) 0.6627(4) 0.3433(4) 0.124(3) Uani 1 1 d D U . . .
H1B1 H 0.8809 0.6559 0.3777 0.148 Uiso 1 1 calc R U . . .
H1B2 H 0.8603 0.6546 0.3125 0.148 Uiso 1 1 calc R U . . .
C2B C 0.9451(7) 0.6001(5) 0.3351(6) 0.138(3) Uani 1 1 d D U . . .
H2B1 H 0.9868 0.6126 0.3071 0.165 Uiso 1 1 calc R U . . .
H2B2 H 0.9794 0.5966 0.3702 0.165 Uiso 1 1 calc R U . . .
C3B C 0.8709(7) 0.5251(5) 0.3168(6) 0.127(3) Uani 1 1 d D U . . .
H3B1 H 0.8206 0.5202 0.3383 0.152 Uiso 1 1 calc R U . . .
H3B2 H 0.8483 0.5241 0.2775 0.152 Uiso 1 1 calc R U . . .
C4B C 0.8979(10) 0.4582(6) 0.3234(8) 0.195(6) Uani 1 1 d D U . . .
H4B1 H 0.9316 0.4526 0.2935 0.292 Uiso 1 1 calc R U . . .
H4B2 H 0.8439 0.4120 0.3221 0.292 Uiso 1 1 calc R U . . .
H4B3 H 0.9359 0.4661 0.3590 0.292 Uiso 1 1 calc R U . . .
C5B C 1.0036(6) 0.7639(6) 0.2909(3) 0.117(3) Uani 1 1 d D U . . .
H5B1 H 1.0376 0.8196 0.2935 0.141 Uiso 1 1 calc R U . . .
H5B2 H 1.0463 0.7387 0.2840 0.141 Uiso 1 1 calc R U . . .
C6B C 0.9319(7) 0.7423(7) 0.2412(4) 0.132(3) Uani 1 1 d D U . . .
H6B1 H 0.9041 0.6861 0.2343 0.158 Uiso 1 1 calc R U . . .
H6B2 H 0.8843 0.7614 0.2494 0.158 Uiso 1 1 calc R U . . .
C7B C 0.9682(8) 0.7739(7) 0.1904(4) 0.129(3) Uani 1 1 d D U . . .
H7B1 H 0.9235 0.7472 0.1577 0.155 Uiso 1 1 calc R U . . .
H7B2 H 1.0238 0.7639 0.1866 0.155 Uiso 1 1 calc R U . . .
C8B C 0.9892(9) 0.8580(7) 0.1916(5) 0.137(4) Uani 1 1 d D U . . .
H8B1 H 0.9328 0.8673 0.1865 0.205 Uiso 1 1 calc R U . . .
H8B2 H 1.0244 0.8779 0.1618 0.205 Uiso 1 1 calc R U . . .
H8B3 H 1.0240 0.8838 0.2272 0.205 Uiso 1 1 calc R U . . .
C9B C 0.9234(7) 0.7951(5) 0.3643(5) 0.158(3) Uani 1 1 d D U . . .
H9B1 H 0.8820 0.7979 0.3323 0.190 Uiso 1 1 calc R U . . .
H9B2 H 0.8871 0.7727 0.3935 0.190 Uiso 1 1 calc R U . . .
C10B C 0.9888(9) 0.8732(7) 0.3853(8) 0.199(5) Uani 1 1 d D U . . .
H10C H 1.0221 0.8967 0.3552 0.239 Uiso 1 1 calc R U . . .
H10D H 1.0331 0.8698 0.4153 0.239 Uiso 1 1 calc R U . . .
C11B C 0.9416(13) 0.9235(8) 0.4069(7) 0.214(5) Uani 1 1 d D U . . .
H111 H 0.8900 0.8925 0.4248 0.257 Uiso 1 1 calc R U . . .
H112 H 0.9840 0.9639 0.4349 0.257 Uiso 1 1 calc R U . . .
C12B C 0.9085(14) 0.9594(12) 0.3604(9) 0.250(8) Uani 1 1 d D U . . .
H121 H 0.8783 0.9915 0.3749 0.300 Uiso 1 1 calc R U . . .
H122 H 0.9598 0.9906 0.3430 0.300 Uiso 1 1 calc R U . . .
H123 H 0.8660 0.9193 0.3329 0.300 Uiso 1 1 calc R U . . .
C13B C 1.0552(6) 0.7573(7) 0.3888(3) 0.147(3) Uani 1 1 d D U . . .
H13A H 1.0961 0.8112 0.3900 0.177 Uiso 1 1 calc R U . . .
H13B H 1.0871 0.7256 0.3746 0.177 Uiso 1 1 calc R U . . .
C14B C 1.0416(8) 0.7404(11) 0.4480(4) 0.180(4) Uani 1 1 d D U . . .
H14A H 1.0171 0.7762 0.4649 0.217 Uiso 1 1 calc R U . . .
H14B H 0.9971 0.6880 0.4478 0.217 Uiso 1 1 calc R U . . .
C15B C 1.1288(10) 0.7482(12) 0.4818(5) 0.203(5) Uani 1 1 d D U . . .
H151 H 1.1782 0.7930 0.4723 0.244 Uiso 1 1 calc R U . . .
H152 H 1.1428 0.7023 0.4731 0.244 Uiso 1 1 calc R U . . .
C16B C 1.1228(13) 0.7576(14) 0.5436(5) 0.266(8) Uani 1 1 d D U . . .
H161 H 1.1802 0.7625 0.5648 0.399 Uiso 1 1 calc R U . . .
H162 H 1.1098 0.8034 0.5524 0.399 Uiso 1 1 calc R U . . .
H163 H 1.0744 0.7129 0.5531 0.399 Uiso 1 1 calc R U . . .
N1C N 0.1822(5) 0.4084(4) -0.0007(3) 0.0673(18) Uani 0.56 1 d D U P A 1
C1C C 0.2482(6) 0.4771(5) 0.0348(4) 0.0523(19) Uani 0.56 1 d D U P A 1
H1C1 H 0.2257 0.5192 0.0325 0.063 Uiso 0.56 1 calc R U P A 1
H1C2 H 0.2506 0.4653 0.0736 0.063 Uiso 0.56 1 calc R U P A 1
C2C C 0.3405(7) 0.5035(8) 0.0201(5) 0.062(2) Uani 0.56 1 d D U P A 1
H2C1 H 0.3433 0.5333 -0.0120 0.075 Uiso 0.56 1 calc R U P A 1
H2C2 H 0.3555 0.4588 0.0092 0.075 Uiso 0.56 1 calc R U P A 1
C3C C 0.4089(7) 0.5521(9) 0.0674(5) 0.067(3) Uani 0.56 1 d D U P A 1
H3C1 H 0.4108 0.5207 0.0981 0.080 Uiso 0.56 1 calc R U P A 1
H3C2 H 0.3903 0.5937 0.0809 0.080 Uiso 0.56 1 calc R U P A 1
C4C C 0.5018(8) 0.5861(7) 0.0505(4) 0.049(2) Uani 0.56 1 d D U P A 1
H4C1 H 0.5444 0.6173 0.0822 0.073 Uiso 0.56 1 calc R U P A 1
H4C2 H 0.5208 0.5450 0.0377 0.073 Uiso 0.56 1 calc R U P A 1
H4C3 H 0.5004 0.6180 0.0206 0.073 Uiso 0.56 1 calc R U P A 1
C5C C 0.0870(6) 0.3968(7) 0.0138(4) 0.076(2) Uani 0.56 1 d D U P A 1
H5C1 H 0.0777 0.4456 0.0120 0.091 Uiso 0.56 1 calc R U P A 1
H5C2 H 0.0418 0.3590 -0.0146 0.091 Uiso 0.56 1 calc R U P A 1
C6C C 0.0697(8) 0.3705(9) 0.0694(5) 0.072(2) Uani 0.56 1 d D U P A 1
H6C1 H 0.1133 0.4088 0.0982 0.086 Uiso 0.56 1 calc R U P A 1
H6C2 H 0.0796 0.3221 0.0718 0.086 Uiso 0.56 1 calc R U P A 1
C7C C -0.0245(9) 0.3587(9) 0.0802(5) 0.067(3) Uani 0.56 1 d D U P A 1
H7C1 H -0.0342 0.4072 0.0777 0.080 Uiso 0.56 1 calc R U P A 1
H7C2 H -0.0679 0.3205 0.0512 0.080 Uiso 0.56 1 calc R U P A 1
C8C C -0.0431(10) 0.3322(11) 0.1355(5) 0.087(4) Uani 0.56 1 d D U P A 1
H8C1 H -0.1051 0.3255 0.1403 0.131 Uiso 0.56 1 calc R U P A 1
H8C2 H -0.0350 0.2836 0.1380 0.131 Uiso 0.56 1 calc R U P A 1
H8C3 H -0.0012 0.3703 0.1645 0.131 Uiso 0.56 1 calc R U P A 1
C9C C 0.1793(8) 0.4175(6) -0.0616(3) 0.067(2) Uani 0.56 1 d D U P A 1
H9C1 H 0.2385 0.4231 -0.0728 0.081 Uiso 0.56 1 calc R U P A 1
H9C2 H 0.1336 0.3707 -0.0825 0.081 Uiso 0.56 1 calc R U P A 1
C10C C 0.1573(10) 0.4842(7) -0.0766(5) 0.065(2) Uani 0.56 1 d D U P A 1
H10A H 0.2126 0.5308 -0.0713 0.078 Uiso 0.56 1 calc R U P A 1
H10B H 0.1145 0.4921 -0.0529 0.078 Uiso 0.56 1 calc R U P A 1
C11C C 0.1151(9) 0.4680(9) -0.1369(5) 0.072(3) Uani 0.56 1 d D U P A 1
H11A H 0.1204 0.5169 -0.1515 0.087 Uiso 0.56 1 calc R U P A 1
H11B H 0.1498 0.4451 -0.1582 0.087 Uiso 0.56 1 calc R U P A 1
C12C C 0.0179(9) 0.4157(9) -0.1463(7) 0.086(4) Uani 0.56 1 d D U P A 1
H12A H -0.0045 0.4079 -0.1858 0.128 Uiso 0.56 1 calc R U P A 1
H12B H 0.0121 0.3666 -0.1329 0.128 Uiso 0.56 1 calc R U P A 1
H12C H -0.0173 0.4385 -0.1262 0.128 Uiso 0.56 1 calc R U P A 1
C13C C 0.2038(9) 0.3382(6) 0.0102(5) 0.073(2) Uani 0.56 1 d D U P A 1
H13C H 0.2317 0.3467 0.0492 0.087 Uiso 0.56 1 calc R U P A 1
H13D H 0.1451 0.2954 0.0079 0.087 Uiso 0.56 1 calc R U P A 1
C14C C 0.2616(11) 0.3090(9) -0.0223(7) 0.088(3) Uani 0.56 1 d D U P A 1
H14C H 0.2449 0.3108 -0.0621 0.106 Uiso 0.56 1 calc R U P A 1
H14D H 0.3255 0.3432 -0.0120 0.106 Uiso 0.56 1 calc R U P A 1
C15C C 0.2527(11) 0.2286(8) -0.0129(8) 0.091(3) Uani 0.56 1 d D U P A 1
H15E H 0.2946 0.2144 -0.0339 0.109 Uiso 0.56 1 calc R U P A 1
H15F H 0.2705 0.2268 0.0267 0.109 Uiso 0.56 1 calc R U P A 1
C16C C 0.1585(11) 0.1714(10) -0.0303(9) 0.097(4) Uani 0.56 1 d D U P A 1
H16D H 0.1564 0.1204 -0.0234 0.116 Uiso 0.56 1 calc R U P A 1
H16E H 0.1167 0.1845 -0.0091 0.116 Uiso 0.56 1 calc R U P A 1
H16F H 0.1409 0.1721 -0.0698 0.116 Uiso 0.56 1 calc R U P A 1
N1D N 0.1901(6) 0.4383(5) -0.0108(4) 0.0717(19) Uani 0.44 1 d D U P B 2
C1D C 0.2927(6) 0.4789(8) 0.0056(5) 0.067(2) Uani 0.44 1 d D U P B 2
H1D1 H 0.3169 0.4545 -0.0223 0.080 Uiso 0.44 1 calc R U P B 2
H1D2 H 0.3036 0.5306 -0.0055 0.080 Uiso 0.44 1 calc R U P B 2
C2D C 0.3614(10) 0.4944(9) 0.0550(6) 0.066(3) Uani 0.44 1 d D U P B 2
H2D1 H 0.3890 0.4554 0.0551 0.079 Uiso 0.44 1 calc R U P B 2
H2D2 H 0.3339 0.4944 0.0893 0.079 Uiso 0.44 1 calc R U P B 2
C3D C 0.4306(12) 0.5717(9) 0.0507(8) 0.073(3) Uani 0.44 1 d D U P B 2
H3D1 H 0.4352 0.5798 0.0114 0.088 Uiso 0.44 1 calc R U P B 2
H3D2 H 0.4129 0.6118 0.0679 0.088 Uiso 0.44 1 calc R U P B 2
C4D C 0.5191(12) 0.5761(12) 0.0794(9) 0.082(4) Uani 0.44 1 d D U P B 2
H4D1 H 0.5649 0.6264 0.0768 0.123 Uiso 0.44 1 calc R U P B 2
H4D2 H 0.5141 0.5684 0.1183 0.123 Uiso 0.44 1 calc R U P B 2
H4D3 H 0.5363 0.5365 0.0619 0.123 Uiso 0.44 1 calc R U P B 2
C5D C 0.1452(8) 0.4380(8) 0.0397(5) 0.069(2) Uani 0.44 1 d D U P B 2
H5D1 H 0.1850 0.4311 0.0709 0.082 Uiso 0.44 1 calc R U P B 2
H5D2 H 0.1437 0.4895 0.0472 0.082 Uiso 0.44 1 calc R U P B 2
C6D C 0.0526(10) 0.3819(11) 0.0417(8) 0.077(3) Uani 0.44 1 d D U P B 2
H6D1 H 0.0551 0.3306 0.0432 0.093 Uiso 0.44 1 calc R U P B 2
H6D2 H 0.0138 0.3808 0.0072 0.093 Uiso 0.44 1 calc R U P B 2
C7D C 0.0105(12) 0.3991(12) 0.0899(7) 0.079(3) Uani 0.44 1 d D U P B 2
H7D1 H 0.0431 0.3930 0.1248 0.094 Uiso 0.44 1 calc R U P B 2
H7D2 H 0.0126 0.4521 0.0913 0.094 Uiso 0.44 1 calc R U P B 2
C8D C -0.0849(13) 0.3442(13) 0.0821(10) 0.098(5) Uani 0.44 1 d D U P B 2
H8D1 H -0.1148 0.3537 0.1130 0.147 Uiso 0.44 1 calc R U P B 2
H8D2 H -0.1164 0.3508 0.0474 0.147 Uiso 0.44 1 calc R U P B 2
H8D3 H -0.0861 0.2920 0.0807 0.147 Uiso 0.44 1 calc R U P B 2
C9D C 0.1607(9) 0.4829(7) -0.0540(5) 0.067(3) Uani 0.44 1 d D U P B 2
H9D1 H 0.1465 0.5222 -0.0327 0.081 Uiso 0.44 1 calc R U P B 2
H9D2 H 0.2156 0.5107 -0.0703 0.081 Uiso 0.44 1 calc R U P B 2
C10D C 0.0856(9) 0.4518(9) -0.1026(5) 0.064(3) Uani 0.44 1 d D U P B 2
H10E H 0.0753 0.3975 -0.1124 0.077 Uiso 0.44 1 calc R U P B 2
H10F H 0.0296 0.4538 -0.0905 0.077 Uiso 0.44 1 calc R U P B 2
C11D C 0.1023(11) 0.4928(11) -0.1539(6) 0.066(3) Uani 0.44 1 d D U P B 2
H11C H 0.1272 0.5484 -0.1428 0.079 Uiso 0.44 1 calc R U P B 2
H11D H 0.1485 0.4799 -0.1715 0.079 Uiso 0.44 1 calc R U P B 2
C12D C 0.0200(10) 0.4739(13) -0.1960(7) 0.078(4) Uani 0.44 1 d D U P B 2
H12D H 0.0364 0.5026 -0.2278 0.117 Uiso 0.44 1 calc R U P B 2
H12E H -0.0044 0.4192 -0.2082 0.117 Uiso 0.44 1 calc R U P B 2
H12F H -0.0256 0.4878 -0.1795 0.117 Uiso 0.44 1 calc R U P B 2
C13D C 0.1711(10) 0.3590(6) -0.0370(5) 0.066(2) Uani 0.44 1 d D U P B 2
H13E H 0.1053 0.3312 -0.0471 0.079 Uiso 0.44 1 calc R U P B 2
H13F H 0.2000 0.3613 -0.0709 0.079 Uiso 0.44 1 calc R U P B 2
C14D C 0.2082(15) 0.3193(10) 0.0040(6) 0.070(2) Uani 0.44 1 d D U P B 2
H14E H 0.1735 0.3079 0.0356 0.084 Uiso 0.44 1 calc R U P B 2
H14F H 0.2728 0.3481 0.0175 0.084 Uiso 0.44 1 calc R U P B 2
C15D C 0.1932(15) 0.2485(9) -0.0339(7) 0.083(3) Uani 0.44 1 d D U P B 2
H15G H 0.1310 0.2289 -0.0538 0.100 Uiso 0.44 1 calc R U P B 2
H15H H 0.2355 0.2612 -0.0615 0.100 Uiso 0.44 1 calc R U P B 2
C16D C 0.2074(18) 0.1881(12) -0.0012(9) 0.089(5) Uani 0.44 1 d D U P B 2
H16J H 0.1975 0.1426 -0.0262 0.133 Uiso 0.44 1 calc R U P B 2
H16K H 0.2692 0.2073 0.0181 0.133 Uiso 0.44 1 calc R U P B 2
H16L H 0.1649 0.1750 0.0258 0.133 Uiso 0.44 1 calc R U P B 2
Cl1 Cl -0.38119(14) 0.10529(11) 0.11230(8) 0.0778(6) Uani 1 1 d D U . . .
Cl2 Cl -0.24105(15) 0.13153(12) 0.04278(8) 0.0791(6) Uani 1 1 d D U . . .
Cl3 Cl -0.1980(2) 0.1506(3) 0.16089(12) 0.1571(16) Uani 1 1 d D U . . .
C1S C -0.2687(4) 0.1602(4) 0.1055(2) 0.074(2) Uani 1 1 d D U . . .
H1S H -0.2616 0.2150 0.1062 0.089 Uiso 1 1 calc R U . . .
Cl7 Cl 0.2417(2) 1.25274(19) 0.39167(15) 0.1430(15) Uani 1 1 d D U . . .
Cl8 Cl 0.1239(4) 1.2846(2) 0.4595(2) 0.201(2) Uani 1 1 d D U . . .
Cl9 Cl 0.0859(4) 1.1316(3) 0.4232(3) 0.249(3) Uani 1 1 d D U . . .
C1U C 0.1727(6) 1.2192(4) 0.4426(4) 0.139(4) Uani 1 1 d D U . . .
H1U H 0.2109 1.2149 0.4763 0.167 Uiso 1 1 calc R U . . .
Cl4 Cl 0.4309(4) 1.1104(3) 0.55922(18) 0.205(2) Uani 1 1 d D U . . .
Cl5 Cl 0.2923(4) 1.1011(3) 0.46820(18) 0.197(2) Uani 1 1 d D U . . .
Cl6 Cl 0.2506(4) 0.9996(3) 0.5521(2) 0.253(3) Uani 1 1 d D U . . .
C1T C 0.3151(6) 1.0923(7) 0.5394(4) 0.213(7) Uani 1 1 d D U . . .
H1T H 0.2976 1.1295 0.5617 0.255 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P2 O5A 1.494(4) . ?
P2 O7A 1.497(5) . ?
P2 O6A 1.576(4) . ?
P2 O8A 1.605(4) . ?
P1 O4A 1.491(5) . ?
P1 O1A 1.495(4) . ?
P1 O2A 1.580(4) . ?
P1 O3A 1.602(4) . ?
O7 C54 1.232(7) . ?
O8 C59 1.099(13) . ?
O9 C66 1.248(7) . ?
O10 C71 1.230(8) . ?
O11 C78 1.217(7) . ?
O12 C83 1.223(8) . ?
N7 C50 1.353(7) . ?
N7 C53 1.398(7) . ?
N7 H7N 0.8800 . ?
N8 C55 1.367(9) . ?
N8 C58 1.387(9) . ?
N8 H8N 0.8800 . ?
N9 C62 1.349(7) . ?
N9 C65 1.390(7) . ?
N9 H9N 0.8800 . ?
N10 C67 1.352(7) . ?
N10 C70 1.393(7) . ?
N10 H10N 0.8800 . ?
N11 C74 1.368(7) . ?
N11 C77 1.396(7) . ?
N11 H11N 0.8800 . ?
N12 C79 1.366(7) . ?
N12 C82 1.383(6) . ?
N12 H12N 0.8800 . ?
C43 C48 1.387(8) . ?
C43 C44 1.411(6) . ?
C43 C49 1.535(8) . ?
C44 C45 1.406(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.371(7) . ?
C45 C61 1.553(6) . ?
C46 C47 1.390(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.383(8) . ?
C47 C73 1.547(8) . ?
C48 H48 0.9500 . ?
C49 C55 1.505(9) . ?
C49 C50 1.525(7) . ?
C49 C60 1.552(8) . ?
C50 C51 1.397(8) . ?
C51 C52 1.387(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.391(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.432(9) . ?
C54 H54 0.9500 . ?
C55 C56 1.378(10) . ?
C56 C57 1.425(11) . ?
C56 H56 0.9500 . ?
C57 C58 1.335(12) . ?
C57 H57 0.9500 . ?
C58 C59 1.485(13) . ?
C59 H59 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C67 1.514(7) . ?
C61 C62 1.525(8) . ?
C61 C72 1.534(7) . ?
C62 C63 1.389(8) . ?
C63 C64 1.392(9) . ?
C63 H63 0.9500 . ?
C64 C65 1.390(8) . ?
C64 H64 0.9500 . ?
C65 C66 1.400(8) . ?
C66 H66 0.9500 . ?
C67 C68 1.412(7) . ?
C68 C69 1.366(8) . ?
C68 H68 0.9500 . ?
C69 C70 1.391(7) . ?
C69 H69 0.9500 . ?
C70 C71 1.440(8) . ?
C71 H71 0.9500 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C74 1.505(8) . ?
C73 C84 1.537(7) . ?
C73 C79 1.537(7) . ?
C74 C75 1.385(8) . ?
C75 C76 1.425(8) . ?
C75 H75 0.9500 . ?
C76 C77 1.374(8) . ?
C76 H76 0.9500 . ?
C77 C78 1.438(8) . ?
C78 H78 0.9500 . ?
C79 C80 1.380(8) . ?
C80 C81 1.396(8) . ?
C80 H80 0.9500 . ?
C81 C82 1.390(9) . ?
C81 H81 0.9500 . ?
C82 C83 1.428(9) . ?
C83 H83 0.9500 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
O1 C12 1.223(9) . ?
O2 C17 1.225(7) . ?
O3 C24 1.192(10) . ?
O4 C29 1.216(9) . ?
O5 C36 1.225(8) . ?
O6 C41 1.229(8) . ?
N1 C8 1.332(8) . ?
N1 C11 1.369(7) . ?
N1 H1N 0.8800 . ?
N2 C13 1.358(7) . ?
N2 C16 1.388(8) . ?
N2 H2N 0.8800 . ?
N3 C20 1.346(8) . ?
N3 C23 1.387(9) . ?
N3 H3N 0.8800 . ?
N4 C25 1.373(7) . ?
N4 C28 1.380(7) . ?
N4 H4N 0.8800 . ?
N5 C32 1.351(8) . ?
N5 C35 1.373(9) . ?
N5 H5N 0.8800 . ?
N6 C37 1.348(7) . ?
N6 C40 1.386(8) . ?
N6 H6N 0.8800 . ?
C1 C2 1.385(8) . ?
C1 C6 1.392(7) . ?
C1 C7 1.542(9) . ?
C2 C3 1.412(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(7) . ?
C3 C19 1.533(9) . ?
C4 C5 1.384(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(9) . ?
C5 C31 1.539(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.520(8) . ?
C7 C13 1.536(8) . ?
C7 C18 1.563(8) . ?
C8 C9 1.399(9) . ?
C9 C10 1.398(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.419(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(10) . ?
C14 C15 1.404(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.443(8) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.493(10) . ?
C19 C25 1.517(7) . ?
C19 C30 1.545(8) . ?
C20 C21 1.392(10) . ?
C21 C22 1.403(12) . ?
C21 H21 0.9500 . ?
C22 C23 1.402(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.444(11) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(8) . ?
C26 C27 1.416(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.427(9) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.512(9) . ?
C31 C42 1.526(8) . ?
C31 C37 1.537(9) . ?
C32 C33 1.417(10) . ?
C33 C34 1.367(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.396(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.428(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.390(8) . ?
C38 C39 1.378(10) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.453(9) . ?
C41 H41 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N1B C1B 1.516(7) . ?
N1B C13B 1.516(7) . ?
N1B C9B 1.518(7) . ?
N1B C5B 1.525(7) . ?
C1B C2B 1.508(8) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B C3B 1.490(8) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B C4B 1.493(8) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B H4B1 0.9800 . ?
C4B H4B2 0.9800 . ?
C4B H4B3 0.9800 . ?
C5B C6B 1.509(8) . ?
C5B H5B1 0.9900 . ?
C5B H5B2 0.9900 . ?
C6B C7B 1.496(8) . ?
C6B H6B1 0.9900 . ?
C6B H6B2 0.9900 . ?
C7B C8B 1.502(9) . ?
C7B H7B1 0.9900 . ?
C7B H7B2 0.9900 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B C10B 1.492(9) . ?
C9B H9B1 0.9900 . ?
C9B H9B2 0.9900 . ?
C10B C11B 1.519(9) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B C12B 1.506(10) . ?
C11B H111 0.9900 . ?
C11B H112 0.9900 . ?
C12B H121 0.9800 . ?
C12B H122 0.9800 . ?
C12B H123 0.9800 . ?
C13B C14B 1.524(8) . ?
C13B H13A 0.9900 . ?
C13B H13B 0.9900 . ?
C14B C15B 1.505(9) . ?
C14B H14A 0.9900 . ?
C14B H14B 0.9900 . ?
C15B C16B 1.530(9) . ?
C15B H151 0.9900 . ?
C15B H152 0.9900 . ?
C16B H161 0.9800 . ?
C16B H162 0.9800 . ?
C16B H163 0.9800 . ?
N1C C1C 1.496(7) . ?
N1C C9C 1.510(7) . ?
N1C C13C 1.521(7) . ?
N1C C5C 1.550(7) . ?
C1C C2C 1.476(8) . ?
C1C H1C1 0.9900 . ?
C1C H1C2 0.9900 . ?
C2C C3C 1.505(9) . ?
C2C H2C1 0.9900 . ?
C2C H2C2 0.9900 . ?
C3C C4C 1.510(9) . ?
C3C H3C1 0.9900 . ?
C3C H3C2 0.9900 . ?
C4C H4C1 0.9800 . ?
C4C H4C2 0.9800 . ?
C4C H4C3 0.9800 . ?
C5C C6C 1.495(9) . ?
C5C H5C1 0.9900 . ?
C5C H5C2 0.9900 . ?
C6C C7C 1.504(9) . ?
C6C H6C1 0.9900 . ?
C6C H6C2 0.9900 . ?
C7C C8C 1.495(9) . ?
C7C H7C1 0.9900 . ?
C7C H7C2 0.9900 . ?
C8C H8C1 0.9800 . ?
C8C H8C2 0.9800 . ?
C8C H8C3 0.9800 . ?
C9C C10C 1.484(9) . ?
C9C H9C1 0.9900 . ?
C9C H9C2 0.9900 . ?
C10C C11C 1.523(9) . ?
C10C H10A 0.9900 . ?
C10C H10B 0.9900 . ?
C11C C12C 1.499(9) . ?
C11C H11A 0.9900 . ?
C11C H11B 0.9900 . ?
C12C H12A 0.9800 . ?
C12C H12B 0.9800 . ?
C12C H12C 0.9800 . ?
C13C C14C 1.510(9) . ?
C13C H13C 0.9900 . ?
C13C H13D 0.9900 . ?
C14C C15C 1.509(10) . ?
C14C H14C 0.9900 . ?
C14C H14D 0.9900 . ?
C15C C16C 1.506(9) . ?
C15C H15E 0.9900 . ?
C15C H15F 0.9900 . ?
C16C H16D 0.9800 . ?
C16C H16E 0.9800 . ?
C16C H16F 0.9800 . ?
N1D C5D 1.496(7) . ?
N1D C13D 1.507(7) . ?
N1D C9D 1.531(7) . ?
N1D C1D 1.542(7) . ?
C1D C2D 1.487(9) . ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
C2D C3D 1.501(10) . ?
C2D H2D1 0.9900 . ?
C2D H2D2 0.9900 . ?
C3D C4D 1.489(10) . ?
C3D H3D1 0.9900 . ?
C3D H3D2 0.9900 . ?
C4D H4D1 0.9800 . ?
C4D H4D2 0.9800 . ?
C4D H4D3 0.9800 . ?
C5D C6D 1.490(9) . ?
C5D H5D1 0.9900 . ?
C5D H5D2 0.9900 . ?
C6D C7D 1.498(10) . ?
C6D H6D1 0.9900 . ?
C6D H6D2 0.9900 . ?
C7D C8D 1.491(10) . ?
C7D H7D1 0.9900 . ?
C7D H7D2 0.9900 . ?
C8D H8D1 0.9800 . ?
C8D H8D2 0.9800 . ?
C8D H8D3 0.9800 . ?
C9D C10D 1.521(9) . ?
C9D H9D1 0.9900 . ?
C9D H9D2 0.9900 . ?
C10D C11D 1.514(9) . ?
C10D H10E 0.9900 . ?
C10D H10F 0.9900 . ?
C11D C12D 1.506(10) . ?
C11D H11C 0.9900 . ?
C11D H11D 0.9900 . ?
C12D H12D 0.9800 . ?
C12D H12E 0.9800 . ?
C12D H12F 0.9800 . ?
C13D C14D 1.489(10) . ?
C13D H13E 0.9900 . ?
C13D H13F 0.9900 . ?
C14D C15D 1.512(10) . ?
C14D H14E 0.9900 . ?
C14D H14F 0.9900 . ?
C15D C16D 1.503(10) . ?
C15D H15G 0.9900 . ?
C15D H15H 0.9900 . ?
C16D H16J 0.9800 . ?
C16D H16K 0.9800 . ?
C16D H16L 0.9800 . ?
Cl1 C1S 1.761(5) . ?
Cl2 C1S 1.754(5) . ?
Cl3 C1S 1.736(6) . ?
C1S H1S 1.0000 . ?
Cl7 C1U 1.752(7) . ?
Cl8 C1U 1.741(7) . ?
Cl9 C1U 1.735(7) . ?
C1U H1U 1.0000 . ?
Cl4 C1T 1.773(7) . ?
Cl5 C1T 1.775(7) . ?
Cl6 C1T 1.750(7) . ?
C1T H1T 1.0000 . ?

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
O5A P2 O7A 119.4(2) . . ?
O5A P2 O6A 106.8(2) . . ?
O7A P2 O6A 109.9(3) . . ?
O5A P2 O8A 106.6(2) . . ?
O7A P2 O8A 107.3(2) . . ?
O6A P2 O8A 106.0(2) . . ?
O4A P1 O1A 118.6(3) . . ?
O4A P1 O2A 111.2(2) . . ?
O1A P1 O2A 106.1(2) . . ?
O4A P1 O3A 108.4(2) . . ?
O1A P1 O3A 105.8(2) . . ?
O2A P1 O3A 105.9(2) . . ?
C50 N7 C53 109.9(5) . . ?
C50 N7 H7N 125.1 . . ?
C53 N7 H7N 125.1 . . ?
C55 N8 C58 108.6(6) . . ?
C55 N8 H8N 125.7 . . ?
C58 N8 H8N 125.7 . . ?
C62 N9 C65 110.7(5) . . ?
C62 N9 H9N 124.6 . . ?
C65 N9 H9N 124.6 . . ?
C67 N10 C70 109.5(4) . . ?
C67 N10 H10N 125.2 . . ?
C70 N10 H10N 125.2 . . ?
C74 N11 C77 109.0(5) . . ?
C74 N11 H11N 125.5 . . ?
C77 N11 H11N 125.5 . . ?
C79 N12 C82 108.3(5) . . ?
C79 N12 H12N 125.8 . . ?
C82 N12 H12N 125.8 . . ?
C48 C43 C44 119.2(5) . . ?
C48 C43 C49 121.5(4) . . ?
C44 C43 C49 119.2(5) . . ?
C45 C44 C43 119.5(5) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C46 C45 C44 119.7(5) . . ?
C46 C45 C61 121.3(5) . . ?
C44 C45 C61 119.1(5) . . ?
C45 C46 C47 121.1(5) . . ?
C45 C46 H46 119.4 . . ?
C47 C46 H46 119.4 . . ?
C48 C47 C46 119.6(5) . . ?
C48 C47 C73 122.0(4) . . ?
C46 C47 C73 118.3(5) . . ?
C47 C48 C43 120.9(5) . . ?
C47 C48 H48 119.6 . . ?
C43 C48 H48 119.6 . . ?
C55 C49 C50 107.6(5) . . ?
C55 C49 C43 113.7(5) . . ?
C50 C49 C43 111.2(5) . . ?
C55 C49 C60 108.2(5) . . ?
C50 C49 C60 108.5(5) . . ?
C43 C49 C60 107.5(5) . . ?
N7 C50 C51 107.7(5) . . ?
N7 C50 C49 122.3(5) . . ?
C51 C50 C49 130.0(6) . . ?
C52 C51 C50 107.8(6) . . ?
C52 C51 H51 126.1 . . ?
C50 C51 H51 126.1 . . ?
C51 C52 C53 108.4(5) . . ?
C51 C52 H52 125.8 . . ?
C53 C52 H52 125.8 . . ?
C52 C53 N7 106.3(5) . . ?
C52 C53 C54 132.0(5) . . ?
N7 C53 C54 121.7(6) . . ?
O7 C54 C53 124.4(7) . . ?
O7 C54 H54 117.8 . . ?
C53 C54 H54 117.8 . . ?
N8 C55 C56 107.5(6) . . ?
N8 C55 C49 123.3(6) . . ?
C56 C55 C49 129.1(6) . . ?
C55 C56 C57 107.5(8) . . ?
C55 C56 H56 126.3 . . ?
C57 C56 H56 126.3 . . ?
C58 C57 C56 107.4(8) . . ?
C58 C57 H57 126.3 . . ?
C56 C57 H57 126.3 . . ?
C57 C58 N8 109.0(7) . . ?
C57 C58 C59 124.9(9) . . ?
N8 C58 C59 126.0(9) . . ?
O8 C59 C58 125.8(13) . . ?
O8 C59 H59 117.1 . . ?
C58 C59 H59 117.1 . . ?
C49 C60 H60A 109.5 . . ?
C49 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C49 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C67 C61 C62 107.9(4) . . ?
C67 C61 C72 110.3(4) . . ?
C62 C61 C72 107.8(4) . . ?
C67 C61 C45 111.0(4) . . ?
C62 C61 C45 109.0(4) . . ?
C72 C61 C45 110.8(4) . . ?
N9 C62 C63 107.1(5) . . ?
N9 C62 C61 121.4(5) . . ?
C63 C62 C61 131.3(5) . . ?
C62 C63 C64 108.1(5) . . ?
C62 C63 H63 125.9 . . ?
C64 C63 H63 125.9 . . ?
C65 C64 C63 108.0(5) . . ?
C65 C64 H64 126.0 . . ?
C63 C64 H64 126.0 . . ?
C64 C65 N9 106.0(5) . . ?
C64 C65 C66 133.8(6) . . ?
N9 C65 C66 120.2(5) . . ?
O9 C66 C65 123.9(5) . . ?
O9 C66 H66 118.0 . . ?
C65 C66 H66 118.0 . . ?
N10 C67 C68 107.1(5) . . ?
N10 C67 C61 125.1(4) . . ?
C68 C67 C61 127.8(5) . . ?
C69 C68 C67 108.3(5) . . ?
C69 C68 H68 125.9 . . ?
C67 C68 H68 125.9 . . ?
C68 C69 C70 108.1(5) . . ?
C68 C69 H69 125.9 . . ?
C70 C69 H69 125.9 . . ?
C69 C70 N10 107.0(5) . . ?
C69 C70 C71 131.1(5) . . ?
N10 C70 C71 121.8(5) . . ?
O10 C71 C70 124.1(6) . . ?
O10 C71 H71 118.0 . . ?
C70 C71 H71 118.0 . . ?
C61 C72 H72A 109.5 . . ?
C61 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C61 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C74 C73 C84 108.5(5) . . ?
C74 C73 C79 110.8(4) . . ?
C84 C73 C79 108.0(4) . . ?
C74 C73 C47 111.8(4) . . ?
C84 C73 C47 107.1(4) . . ?
C79 C73 C47 110.5(5) . . ?
N11 C74 C75 108.2(5) . . ?
N11 C74 C73 123.1(5) . . ?
C75 C74 C73 128.7(5) . . ?
C74 C75 C76 107.5(5) . . ?
C74 C75 H75 126.2 . . ?
C76 C75 H75 126.2 . . ?
C77 C76 C75 107.3(5) . . ?
C77 C76 H76 126.4 . . ?
C75 C76 H76 126.4 . . ?
C76 C77 N11 108.0(5) . . ?
C76 C77 C78 127.7(5) . . ?
N11 C77 C78 124.0(5) . . ?
O11 C78 C77 124.2(5) . . ?
O11 C78 H78 117.9 . . ?
C77 C78 H78 117.9 . . ?
N12 C79 C80 108.9(5) . . ?
N12 C79 C73 122.1(5) . . ?
C80 C79 C73 129.0(5) . . ?
C79 C80 C81 107.4(5) . . ?
C79 C80 H80 126.3 . . ?
C81 C80 H80 126.3 . . ?
C82 C81 C80 107.6(5) . . ?
C82 C81 H81 126.2 . . ?
C80 C81 H81 126.2 . . ?
N12 C82 C81 107.8(5) . . ?
N12 C82 C83 124.6(6) . . ?
C81 C82 C83 127.6(5) . . ?
O12 C83 C82 127.1(5) . . ?
O12 C83 H83 116.4 . . ?
C82 C83 H83 116.4 . . ?
C73 C84 H84A 109.5 . . ?
C73 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C73 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C8 N1 C11 110.2(6) . . ?
C8 N1 H1N 124.9 . . ?
C11 N1 H1N 124.9 . . ?
C13 N2 C16 107.8(5) . . ?
C13 N2 H2N 126.1 . . ?
C16 N2 H2N 126.1 . . ?
C20 N3 C23 111.2(6) . . ?
C20 N3 H3N 124.4 . . ?
C23 N3 H3N 124.4 . . ?
C25 N4 C28 109.2(5) . . ?
C25 N4 H4N 125.4 . . ?
C28 N4 H4N 125.4 . . ?
C32 N5 C35 110.3(5) . . ?
C32 N5 H5N 124.9 . . ?
C35 N5 H5N 124.9 . . ?
C37 N6 C40 109.5(5) . . ?
C37 N6 H6N 125.2 . . ?
C40 N6 H6N 125.2 . . ?
C2 C1 C6 120.0(6) . . ?
C2 C1 C7 121.1(5) . . ?
C6 C1 C7 118.7(5) . . ?
C1 C2 C3 120.5(5) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 118.2(6) . . ?
C4 C3 C19 119.8(6) . . ?
C2 C3 C19 121.9(5) . . ?
C5 C4 C3 121.7(6) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 C31 120.5(6) . . ?
C6 C5 C31 120.6(5) . . ?
C1 C6 C5 120.7(6) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C13 108.8(5) . . ?
C8 C7 C1 111.6(5) . . ?
C13 C7 C1 112.0(5) . . ?
C8 C7 C18 109.2(5) . . ?
C13 C7 C18 108.4(5) . . ?
C1 C7 C18 106.6(5) . . ?
N1 C8 C9 108.8(5) . . ?
N1 C8 C7 122.2(5) . . ?
C9 C8 C7 128.9(6) . . ?
C8 C9 C10 106.5(6) . . ?
C8 C9 H9 126.8 . . ?
C10 C9 H9 126.8 . . ?
C11 C10 C9 107.5(6) . . ?
C11 C10 H10 126.3 . . ?
C9 C10 H10 126.3 . . ?
N1 C11 C10 106.9(6) . . ?
N1 C11 C12 123.4(7) . . ?
C10 C11 C12 129.6(6) . . ?
O1 C12 C11 126.3(7) . . ?
O1 C12 H12 116.9 . . ?
C11 C12 H12 116.9 . . ?
N2 C13 C14 109.1(6) . . ?
N2 C13 C7 121.9(6) . . ?
C14 C13 C7 128.9(5) . . ?
C15 C14 C13 107.1(6) . . ?
C15 C14 H14 126.4 . . ?
C13 C14 H14 126.4 . . ?
C16 C15 C14 106.8(6) . . ?
C16 C15 H15 126.6 . . ?
C14 C15 H15 126.6 . . ?
C15 C16 N2 109.1(5) . . ?
C15 C16 C17 127.8(6) . . ?
N2 C16 C17 122.8(6) . . ?
O2 C17 C16 125.2(6) . . ?
O2 C17 H17 117.4 . . ?
C16 C17 H17 117.4 . . ?
C7 C18 H18A 109.5 . . ?
C7 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C7 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C25 108.9(5) . . ?
C20 C19 C3 111.1(5) . . ?
C25 C19 C3 112.3(5) . . ?
C20 C19 C30 109.5(6) . . ?
C25 C19 C30 107.2(5) . . ?
C3 C19 C30 107.7(5) . . ?
N3 C20 C21 106.8(7) . . ?
N3 C20 C19 122.0(6) . . ?
C21 C20 C19 131.1(6) . . ?
C20 C21 C22 108.9(7) . . ?
C20 C21 H21 125.6 . . ?
C22 C21 H21 125.6 . . ?
C21 C22 C23 106.6(7) . . ?
C21 C22 H22 126.7 . . ?
C23 C22 H22 126.7 . . ?
N3 C23 C22 106.5(7) . . ?
N3 C23 C24 121.6(7) . . ?
C22 C23 C24 131.9(8) . . ?
O3 C24 C23 126.3(9) . . ?
O3 C24 H24 116.8 . . ?
C23 C24 H24 116.8 . . ?
N4 C25 C26 108.2(5) . . ?
N4 C25 C19 122.0(5) . . ?
C26 C25 C19 129.8(5) . . ?
C25 C26 C27 107.0(5) . . ?
C25 C26 H26 126.5 . . ?
C27 C26 H26 126.5 . . ?
C28 C27 C26 107.6(5) . . ?
C28 C27 H27 126.2 . . ?
C26 C27 H27 126.2 . . ?
N4 C28 C27 108.0(5) . . ?
N4 C28 C29 123.9(6) . . ?
C27 C28 C29 128.1(6) . . ?
O4 C29 C28 125.5(6) . . ?
O4 C29 H29 117.2 . . ?
C28 C29 H29 117.2 . . ?
C19 C30 H30A 109.5 . . ?
C19 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C19 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C42 108.1(5) . . ?
C32 C31 C37 109.2(5) . . ?
C42 C31 C37 107.8(5) . . ?
C32 C31 C5 109.9(5) . . ?
C42 C31 C5 110.7(5) . . ?
C37 C31 C5 111.0(5) . . ?
N5 C32 C33 106.4(6) . . ?
N5 C32 C31 123.1(6) . . ?
C33 C32 C31 129.6(6) . . ?
C34 C33 C32 108.5(7) . . ?
C34 C33 H33 125.8 . . ?
C32 C33 H33 125.8 . . ?
C33 C34 C35 107.5(7) . . ?
C33 C34 H34 126.3 . . ?
C35 C34 H34 126.3 . . ?
N5 C35 C34 107.4(6) . . ?
N5 C35 C36 121.4(6) . . ?
C34 C35 C36 131.2(7) . . ?
O5 C36 C35 123.7(6) . . ?
O5 C36 H36 118.1 . . ?
C35 C36 H36 118.1 . . ?
N6 C37 C38 107.7(6) . . ?
N6 C37 C31 123.8(5) . . ?
C38 C37 C31 128.5(5) . . ?
C39 C38 C37 107.9(6) . . ?
C39 C38 H38 126.0 . . ?
C37 C38 H38 126.0 . . ?
C38 C39 C40 108.0(6) . . ?
C38 C39 H39 126.0 . . ?
C40 C39 H39 126.0 . . ?
C39 C40 N6 106.9(6) . . ?
C39 C40 C41 131.8(6) . . ?
N6 C40 C41 121.3(5) . . ?
O6 C41 C40 123.9(6) . . ?
O6 C41 H41 118.0 . . ?
C40 C41 H41 118.0 . . ?
C31 C42 H42A 109.5 . . ?
C31 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C31 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C1B N1B C13B 109.4(5) . . ?
C1B N1B C9B 107.7(5) . . ?
C13B N1B C9B 110.9(5) . . ?
C1B N1B C5B 110.3(5) . . ?
C13B N1B C5B 109.1(5) . . ?
C9B N1B C5B 109.3(5) . . ?
C2B C1B N1B 118.9(7) . . ?
C2B C1B H1B1 107.6 . . ?
N1B C1B H1B1 107.6 . . ?
C2B C1B H1B2 107.6 . . ?
N1B C1B H1B2 107.6 . . ?
H1B1 C1B H1B2 107.0 . . ?
C3B C2B C1B 111.4(7) . . ?
C3B C2B H2B1 109.4 . . ?
C1B C2B H2B1 109.4 . . ?
C3B C2B H2B2 109.4 . . ?
C1B C2B H2B2 109.4 . . ?
H2B1 C2B H2B2 108.0 . . ?
C4B C3B C2B 114.0(8) . . ?
C4B C3B H3B1 108.8 . . ?
C2B C3B H3B1 108.8 . . ?
C4B C3B H3B2 108.8 . . ?
C2B C3B H3B2 108.8 . . ?
H3B1 C3B H3B2 107.7 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
C6B C5B N1B 117.8(7) . . ?
C6B C5B H5B1 107.9 . . ?
N1B C5B H5B1 107.9 . . ?
C6B C5B H5B2 107.9 . . ?
N1B C5B H5B2 107.9 . . ?
H5B1 C5B H5B2 107.2 . . ?
C7B C6B C5B 112.7(7) . . ?
C7B C6B H6B1 109.1 . . ?
C5B C6B H6B1 109.1 . . ?
C7B C6B H6B2 109.1 . . ?
C5B C6B H6B2 109.1 . . ?
H6B1 C6B H6B2 107.8 . . ?
C6B C7B C8B 112.6(7) . . ?
C6B C7B H7B1 109.1 . . ?
C8B C7B H7B1 109.1 . . ?
C6B C7B H7B2 109.1 . . ?
C8B C7B H7B2 109.1 . . ?
H7B1 C7B H7B2 107.8 . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C10B C9B N1B 110.1(8) . . ?
C10B C9B H9B1 109.6 . . ?
N1B C9B H9B1 109.6 . . ?
C10B C9B H9B2 109.6 . . ?
N1B C9B H9B2 109.6 . . ?
H9B1 C9B H9B2 108.2 . . ?
C9B C10B C11B 111.5(8) . . ?
C9B C10B H10C 109.3 . . ?
C11B C10B H10C 109.3 . . ?
C9B C10B H10D 109.3 . . ?
C11B C10B H10D 109.3 . . ?
H10C C10B H10D 108.0 . . ?
C12B C11B C10B 110.4(9) . . ?
C12B C11B H111 109.6 . . ?
C10B C11B H111 109.6 . . ?
C12B C11B H112 109.6 . . ?
C10B C11B H112 109.6 . . ?
H111 C11B H112 108.1 . . ?
C11B C12B H121 109.5 . . ?
C11B C12B H122 109.5 . . ?
H121 C12B H122 109.5 . . ?
C11B C12B H123 109.5 . . ?
H121 C12B H123 109.5 . . ?
H122 C12B H123 109.5 . . ?
N1B C13B C14B 118.8(8) . . ?
N1B C13B H13A 107.6 . . ?
C14B C13B H13A 107.6 . . ?
N1B C13B H13B 107.6 . . ?
C14B C13B H13B 107.6 . . ?
H13A C13B H13B 107.1 . . ?
C15B C14B C13B 111.2(8) . . ?
C15B C14B H14A 109.4 . . ?
C13B C14B H14A 109.4 . . ?
C15B C14B H14B 109.4 . . ?
C13B C14B H14B 109.4 . . ?
H14A C14B H14B 108.0 . . ?
C14B C15B C16B 110.9(9) . . ?
C14B C15B H151 109.5 . . ?
C16B C15B H151 109.5 . . ?
C14B C15B H152 109.5 . . ?
C16B C15B H152 109.5 . . ?
H151 C15B H152 108.0 . . ?
C15B C16B H161 109.5 . . ?
C15B C16B H162 109.5 . . ?
H161 C16B H162 109.5 . . ?
C15B C16B H163 109.5 . . ?
H161 C16B H163 109.5 . . ?
H162 C16B H163 109.5 . . ?
C1C N1C C9C 113.1(5) . . ?
C1C N1C C13C 110.5(5) . . ?
C9C N1C C13C 109.2(5) . . ?
C1C N1C C5C 107.8(5) . . ?
C9C N1C C5C 106.6(5) . . ?
C13C N1C C5C 109.7(5) . . ?
C2C C1C N1C 114.7(7) . . ?
C2C C1C H1C1 108.6 . . ?
N1C C1C H1C1 108.6 . . ?
C2C C1C H1C2 108.6 . . ?
N1C C1C H1C2 108.6 . . ?
H1C1 C1C H1C2 107.6 . . ?
C1C C2C C3C 111.8(8) . . ?
C1C C2C H2C1 109.3 . . ?
C3C C2C H2C1 109.3 . . ?
C1C C2C H2C2 109.3 . . ?
C3C C2C H2C2 109.3 . . ?
H2C1 C2C H2C2 107.9 . . ?
C2C C3C C4C 111.7(9) . . ?
C2C C3C H3C1 109.3 . . ?
C4C C3C H3C1 109.3 . . ?
C2C C3C H3C2 109.3 . . ?
C4C C3C H3C2 109.3 . . ?
H3C1 C3C H3C2 107.9 . . ?
C3C C4C H4C1 109.5 . . ?
C3C C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 109.5 . . ?
C3C C4C H4C3 109.5 . . ?
H4C1 C4C H4C3 109.5 . . ?
H4C2 C4C H4C3 109.5 . . ?
C6C C5C N1C 115.0(8) . . ?
C6C C5C H5C1 108.5 . . ?
N1C C5C H5C1 108.5 . . ?
C6C C5C H5C2 108.5 . . ?
N1C C5C H5C2 108.5 . . ?
H5C1 C5C H5C2 107.5 . . ?
C5C C6C C7C 112.2(10) . . ?
C5C C6C H6C1 109.2 . . ?
C7C C6C H6C1 109.2 . . ?
C5C C6C H6C2 109.2 . . ?
C7C C6C H6C2 109.2 . . ?
H6C1 C6C H6C2 107.9 . . ?
C8C C7C C6C 112.9(11) . . ?
C8C C7C H7C1 109.0 . . ?
C6C C7C H7C1 109.0 . . ?
C8C C7C H7C2 109.0 . . ?
C6C C7C H7C2 109.0 . . ?
H7C1 C7C H7C2 107.8 . . ?
C7C C8C H8C1 109.5 . . ?
C7C C8C H8C2 109.5 . . ?
H8C1 C8C H8C2 109.5 . . ?
C7C C8C H8C3 109.5 . . ?
H8C1 C8C H8C3 109.5 . . ?
H8C2 C8C H8C3 109.5 . . ?
C10C C9C N1C 113.3(7) . . ?
C10C C9C H9C1 108.9 . . ?
N1C C9C H9C1 108.9 . . ?
C10C C9C H9C2 108.9 . . ?
N1C C9C H9C2 108.9 . . ?
H9C1 C9C H9C2 107.7 . . ?
C9C C10C C11C 107.7(10) . . ?
C9C C10C H10A 110.2 . . ?
C11C C10C H10A 110.2 . . ?
C9C C10C H10B 110.2 . . ?
C11C C10C H10B 110.2 . . ?
H10A C10C H10B 108.5 . . ?
C12C C11C C10C 114.0(13) . . ?
C12C C11C H11A 108.7 . . ?
C10C C11C H11A 108.7 . . ?
C12C C11C H11B 108.7 . . ?
C10C C11C H11B 108.7 . . ?
H11A C11C H11B 107.6 . . ?
C11C C12C H12A 109.5 . . ?
C11C C12C H12B 109.5 . . ?
H12A C12C H12B 109.5 . . ?
C11C C12C H12C 109.5 . . ?
H12A C12C H12C 109.5 . . ?
H12B C12C H12C 109.5 . . ?
C14C C13C N1C 124.8(10) . . ?
C14C C13C H13C 106.1 . . ?
N1C C13C H13C 106.1 . . ?
C14C C13C H13D 106.1 . . ?
N1C C13C H13D 106.1 . . ?
H13C C13C H13D 106.3 . . ?
C15C C14C C13C 113.6(12) . . ?
C15C C14C H14C 108.9 . . ?
C13C C14C H14C 108.9 . . ?
C15C C14C H14D 108.9 . . ?
C13C C14C H14D 108.9 . . ?
H14C C14C H14D 107.7 . . ?
C16C C15C C14C 112.8(15) . . ?
C16C C15C H15E 109.0 . . ?
C14C C15C H15E 109.0 . . ?
C16C C15C H15F 109.0 . . ?
C14C C15C H15F 109.0 . . ?
H15E C15C H15F 107.8 . . ?
C15C C16C H16D 109.5 . . ?
C15C C16C H16E 109.5 . . ?
H16D C16C H16E 109.5 . . ?
C15C C16C H16F 109.5 . . ?
H16D C16C H16F 109.5 . . ?
H16E C16C H16F 109.5 . . ?
C5D N1D C13D 112.3(6) . . ?
C5D N1D C9D 111.4(6) . . ?
C13D N1D C9D 108.6(5) . . ?
C5D N1D C1D 108.6(5) . . ?
C13D N1D C1D 108.6(5) . . ?
C9D N1D C1D 107.2(5) . . ?
C2D C1D N1D 138.9(10) . . ?
C2D C1D H1D1 102.4 . . ?
N1D C1D H1D1 102.4 . . ?
C2D C1D H1D2 102.4 . . ?
N1D C1D H1D2 102.4 . . ?
H1D1 C1D H1D2 104.9 . . ?
C1D C2D C3D 105.3(12) . . ?
C1D C2D H2D1 110.7 . . ?
C3D C2D H2D1 110.7 . . ?
C1D C2D H2D2 110.7 . . ?
C3D C2D H2D2 110.7 . . ?
H2D1 C2D H2D2 108.8 . . ?
C4D C3D C2D 108.6(14) . . ?
C4D C3D H3D1 110.0 . . ?
C2D C3D H3D1 110.0 . . ?
C4D C3D H3D2 110.0 . . ?
C2D C3D H3D2 110.0 . . ?
H3D1 C3D H3D2 108.3 . . ?
C3D C4D H4D1 109.5 . . ?
C3D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
C3D C4D H4D3 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?
C6D C5D N1D 120.6(10) . . ?
C6D C5D H5D1 107.2 . . ?
N1D C5D H5D1 107.2 . . ?
C6D C5D H5D2 107.2 . . ?
N1D C5D H5D2 107.2 . . ?
H5D1 C5D H5D2 106.8 . . ?
C5D C6D C7D 113.8(12) . . ?
C5D C6D H6D1 108.8 . . ?
C7D C6D H6D1 108.8 . . ?
C5D C6D H6D2 108.8 . . ?
C7D C6D H6D2 108.8 . . ?
H6D1 C6D H6D2 107.7 . . ?
C8D C7D C6D 107.1(15) . . ?
C8D C7D H7D1 110.3 . . ?
C6D C7D H7D1 110.3 . . ?
C8D C7D H7D2 110.3 . . ?
C6D C7D H7D2 110.3 . . ?
H7D1 C7D H7D2 108.5 . . ?
C7D C8D H8D1 109.5 . . ?
C7D C8D H8D2 109.5 . . ?
H8D1 C8D H8D2 109.5 . . ?
C7D C8D H8D3 109.5 . . ?
H8D1 C8D H8D3 109.5 . . ?
H8D2 C8D H8D3 109.5 . . ?
C10D C9D N1D 127.8(10) . . ?
C10D C9D H9D1 105.3 . . ?
N1D C9D H9D1 105.3 . . ?
C10D C9D H9D2 105.3 . . ?
N1D C9D H9D2 105.3 . . ?
H9D1 C9D H9D2 106.0 . . ?
C11D C10D C9D 115.6(11) . . ?
C11D C10D H10E 108.4 . . ?
C9D C10D H10E 108.4 . . ?
C11D C10D H10F 108.4 . . ?
C9D C10D H10F 108.4 . . ?
H10E C10D H10F 107.4 . . ?
C12D C11D C10D 114.5(13) . . ?
C12D C11D H11C 108.6 . . ?
C10D C11D H11C 108.6 . . ?
C12D C11D H11D 108.6 . . ?
C10D C11D H11D 108.6 . . ?
H11C C11D H11D 107.6 . . ?
C11D C12D H12D 109.5 . . ?
C11D C12D H12E 109.5 . . ?
H12D C12D H12E 109.5 . . ?
C11D C12D H12F 109.5 . . ?
H12D C12D H12F 109.5 . . ?
H12E C12D H12F 109.5 . . ?
C14D C13D N1D 107.5(9) . . ?
C14D C13D H13E 110.2 . . ?
N1D C13D H13E 110.2 . . ?
C14D C13D H13F 110.2 . . ?
N1D C13D H13F 110.2 . . ?
H13E C13D H13F 108.5 . . ?
C13D C14D C15D 97.2(11) . . ?
C13D C14D H14E 112.3 . . ?
C15D C14D H14E 112.3 . . ?
C13D C14D H14F 112.3 . . ?
C15D C14D H14F 112.3 . . ?
H14E C14D H14F 109.9 . . ?
C16D C15D C14D 110.4(15) . . ?
C16D C15D H15G 109.6 . . ?
C14D C15D H15G 109.6 . . ?
C16D C15D H15H 109.6 . . ?
C14D C15D H15H 109.6 . . ?
H15G C15D H15H 108.1 . . ?
C15D C16D H16J 109.5 . . ?
C15D C16D H16K 109.5 . . ?
H16J C16D H16K 109.5 . . ?
C15D C16D H16L 109.5 . . ?
H16J C16D H16L 109.5 . . ?
H16K C16D H16L 109.5 . . ?
Cl3 C1S Cl2 110.7(4) . . ?
Cl3 C1S Cl1 109.2(4) . . ?
Cl2 C1S Cl1 110.4(3) . . ?
Cl3 C1S H1S 108.8 . . ?
Cl2 C1S H1S 108.8 . . ?
Cl1 C1S H1S 108.8 . . ?
Cl9 C1U Cl8 107.4(5) . . ?
Cl9 C1U Cl7 114.3(5) . . ?
Cl8 C1U Cl7 109.1(5) . . ?
Cl9 C1U H1U 108.6 . . ?
Cl8 C1U H1U 108.6 . . ?
Cl7 C1U H1U 108.6 . . ?
Cl6 C1T Cl4 109.4(6) . . ?
Cl6 C1T Cl5 108.6(6) . . ?
Cl4 C1T Cl5 111.3(6) . . ?
Cl6 C1T H1T 109.2 . . ?
Cl4 C1T H1T 109.2 . . ?
Cl5 C1T H1T 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C48 C43 C44 C45 -1.9(8) . . . . ?
C49 C43 C44 C45 -177.5(5) . . . . ?
C43 C44 C45 C46 1.1(8) . . . . ?
C43 C44 C45 C61 -178.1(4) . . . . ?
C44 C45 C46 C47 0.6(8) . . . . ?
C61 C45 C46 C47 179.7(5) . . . . ?
C45 C46 C47 C48 -1.3(8) . . . . ?
C45 C46 C47 C73 174.5(5) . . . . ?
C46 C47 C48 C43 0.4(8) . . . . ?
C73 C47 C48 C43 -175.2(5) . . . . ?
C44 C43 C48 C47 1.2(8) . . . . ?
C49 C43 C48 C47 176.7(5) . . . . ?
C48 C43 C49 C55 143.1(5) . . . . ?
C44 C43 C49 C55 -41.5(7) . . . . ?
C48 C43 C49 C50 21.5(7) . . . . ?
C44 C43 C49 C50 -163.1(5) . . . . ?
C48 C43 C49 C60 -97.2(6) . . . . ?
C44 C43 C49 C60 78.3(6) . . . . ?
C53 N7 C50 C51 0.2(8) . . . . ?
C53 N7 C50 C49 -179.2(6) . . . . ?
C55 C49 C50 N7 -61.5(8) . . . . ?
C43 C49 C50 N7 63.6(8) . . . . ?
C60 C49 C50 N7 -178.3(6) . . . . ?
C55 C49 C50 C51 119.2(8) . . . . ?
C43 C49 C50 C51 -115.7(8) . . . . ?
C60 C49 C50 C51 2.4(10) . . . . ?
N7 C50 C51 C52 -0.3(8) . . . . ?
C49 C50 C51 C52 179.1(7) . . . . ?
C50 C51 C52 C53 0.2(9) . . . . ?
C51 C52 C53 N7 -0.1(8) . . . . ?
C51 C52 C53 C54 177.9(8) . . . . ?
C50 N7 C53 C52 -0.1(8) . . . . ?
C50 N7 C53 C54 -178.4(6) . . . . ?
C52 C53 C54 O7 6.5(14) . . . . ?
N7 C53 C54 O7 -175.8(7) . . . . ?
C58 N8 C55 C56 0.0(7) . . . . ?
C58 N8 C55 C49 -176.7(5) . . . . ?
C50 C49 C55 N8 88.4(6) . . . . ?
C43 C49 C55 N8 -35.2(7) . . . . ?
C60 C49 C55 N8 -154.5(5) . . . . ?
C50 C49 C55 C56 -87.5(7) . . . . ?
C43 C49 C55 C56 148.8(6) . . . . ?
C60 C49 C55 C56 29.5(8) . . . . ?
N8 C55 C56 C57 -0.2(7) . . . . ?
C49 C55 C56 C57 176.3(6) . . . . ?
C55 C56 C57 C58 0.3(8) . . . . ?
C56 C57 C58 N8 -0.3(8) . . . . ?
C56 C57 C58 C59 176.2(6) . . . . ?
C55 N8 C58 C57 0.2(7) . . . . ?
C55 N8 C58 C59 -176.2(6) . . . . ?
C57 C58 C59 O8 -170.5(10) . . . . ?
N8 C58 C59 O8 5.3(14) . . . . ?
C46 C45 C61 C67 -103.5(6) . . . . ?
C44 C45 C61 C67 75.7(6) . . . . ?
C46 C45 C61 C62 15.2(6) . . . . ?
C44 C45 C61 C62 -165.7(5) . . . . ?
C46 C45 C61 C72 133.6(5) . . . . ?
C44 C45 C61 C72 -47.2(6) . . . . ?
C65 N9 C62 C63 -0.5(6) . . . . ?
C65 N9 C62 C61 175.9(4) . . . . ?
C67 C61 C62 N9 35.9(6) . . . . ?
C72 C61 C62 N9 155.0(5) . . . . ?
C45 C61 C62 N9 -84.7(6) . . . . ?
C67 C61 C62 C63 -148.7(6) . . . . ?
C72 C61 C62 C63 -29.7(7) . . . . ?
C45 C61 C62 C63 90.7(6) . . . . ?
N9 C62 C63 C64 -0.5(7) . . . . ?
C61 C62 C63 C64 -176.3(5) . . . . ?
C62 C63 C64 C65 1.3(7) . . . . ?
C63 C64 C65 N9 -1.5(7) . . . . ?
C63 C64 C65 C66 177.6(6) . . . . ?
C62 N9 C65 C64 1.2(6) . . . . ?
C62 N9 C65 C66 -178.1(5) . . . . ?
C64 C65 C66 O9 1.2(11) . . . . ?
N9 C65 C66 O9 -179.7(5) . . . . ?
C70 N10 C67 C68 1.0(6) . . . . ?
C70 N10 C67 C61 -178.8(5) . . . . ?
C62 C61 C67 N10 -121.6(6) . . . . ?
C72 C61 C67 N10 121.0(6) . . . . ?
C45 C61 C67 N10 -2.2(8) . . . . ?
C62 C61 C67 C68 58.7(7) . . . . ?
C72 C61 C67 C68 -58.7(7) . . . . ?
C45 C61 C67 C68 178.1(5) . . . . ?
N10 C67 C68 C69 -0.2(7) . . . . ?
C61 C67 C68 C69 179.6(5) . . . . ?
C67 C68 C69 C70 -0.7(7) . . . . ?
C68 C69 C70 N10 1.3(7) . . . . ?
C68 C69 C70 C71 176.9(7) . . . . ?
C67 N10 C70 C69 -1.4(7) . . . . ?
C67 N10 C70 C71 -177.5(6) . . . . ?
C69 C70 C71 O10 2.5(12) . . . . ?
N10 C70 C71 O10 177.6(7) . . . . ?
C48 C47 C73 C74 -155.6(5) . . . . ?
C46 C47 C73 C74 28.8(6) . . . . ?
C48 C47 C73 C84 85.7(6) . . . . ?
C46 C47 C73 C84 -89.9(6) . . . . ?
C48 C47 C73 C79 -31.7(7) . . . . ?
C46 C47 C73 C79 152.7(5) . . . . ?
C77 N11 C74 C75 0.5(6) . . . . ?
C77 N11 C74 C73 -177.2(4) . . . . ?
C84 C73 C74 N11 -179.4(4) . . . . ?
C79 C73 C74 N11 -61.0(6) . . . . ?
C47 C73 C74 N11 62.7(6) . . . . ?
C84 C73 C74 C75 3.4(7) . . . . ?
C79 C73 C74 C75 121.8(6) . . . . ?
C47 C73 C74 C75 -114.5(6) . . . . ?
N11 C74 C75 C76 -0.7(6) . . . . ?
C73 C74 C75 C76 176.9(5) . . . . ?
C74 C75 C76 C77 0.6(6) . . . . ?
C75 C76 C77 N11 -0.3(6) . . . . ?
C75 C76 C77 C78 173.3(5) . . . . ?
C74 N11 C77 C76 -0.1(6) . . . . ?
C74 N11 C77 C78 -174.0(5) . . . . ?
C76 C77 C78 O11 -166.7(6) . . . . ?
N11 C77 C78 O11 5.9(9) . . . . ?
C82 N12 C79 C80 -0.3(7) . . . . ?
C82 N12 C79 C73 178.1(5) . . . . ?
C74 C73 C79 N12 70.3(7) . . . . ?
C84 C73 C79 N12 -171.0(5) . . . . ?
C47 C73 C79 N12 -54.2(7) . . . . ?
C74 C73 C79 C80 -111.6(7) . . . . ?
C84 C73 C79 C80 7.1(9) . . . . ?
C47 C73 C79 C80 123.9(7) . . . . ?
N12 C79 C80 C81 0.6(7) . . . . ?
C73 C79 C80 C81 -177.7(6) . . . . ?
C79 C80 C81 C82 -0.6(8) . . . . ?
C79 N12 C82 C81 0.0(7) . . . . ?
C79 N12 C82 C83 -178.6(6) . . . . ?
C80 C81 C82 N12 0.4(8) . . . . ?
C80 C81 C82 C83 178.9(7) . . . . ?
N12 C82 C83 O12 1.3(12) . . . . ?
C81 C82 C83 O12 -176.9(7) . . . . ?
C6 C1 C2 C3 0.8(8) . . . . ?
C7 C1 C2 C3 175.6(5) . . . . ?
C1 C2 C3 C4 -1.1(8) . . . . ?
C1 C2 C3 C19 -178.2(5) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C19 C3 C4 C5 178.1(5) . . . . ?
C3 C4 C5 C6 -0.4(9) . . . . ?
C3 C4 C5 C31 -178.2(5) . . . . ?
C2 C1 C6 C5 -0.2(8) . . . . ?
C7 C1 C6 C5 -175.2(5) . . . . ?
C4 C5 C6 C1 0.1(9) . . . . ?
C31 C5 C6 C1 177.9(5) . . . . ?
C2 C1 C7 C8 32.1(7) . . . . ?
C6 C1 C7 C8 -152.9(5) . . . . ?
C2 C1 C7 C13 154.5(5) . . . . ?
C6 C1 C7 C13 -30.6(7) . . . . ?
C2 C1 C7 C18 -87.1(6) . . . . ?
C6 C1 C7 C18 87.8(6) . . . . ?
C11 N1 C8 C9 -0.6(8) . . . . ?
C11 N1 C8 C7 180.0(6) . . . . ?
C13 C7 C8 N1 -71.6(8) . . . . ?
C1 C7 C8 N1 52.6(8) . . . . ?
C18 C7 C8 N1 170.3(6) . . . . ?
C13 C7 C8 C9 109.2(8) . . . . ?
C1 C7 C8 C9 -126.7(8) . . . . ?
C18 C7 C8 C9 -8.9(10) . . . . ?
N1 C8 C9 C10 1.3(9) . . . . ?
C7 C8 C9 C10 -179.3(7) . . . . ?
C8 C9 C10 C11 -1.5(10) . . . . ?
C8 N1 C11 C10 -0.3(9) . . . . ?
C8 N1 C11 C12 -179.9(8) . . . . ?
C9 C10 C11 N1 1.1(10) . . . . ?
C9 C10 C11 C12 -179.3(9) . . . . ?
N1 C11 C12 O1 -7.7(16) . . . . ?
C10 C11 C12 O1 172.8(10) . . . . ?
C16 N2 C13 C14 1.0(7) . . . . ?
C16 N2 C13 C7 178.7(5) . . . . ?
C8 C7 C13 N2 62.6(7) . . . . ?
C1 C7 C13 N2 -61.3(7) . . . . ?
C18 C7 C13 N2 -178.7(5) . . . . ?
C8 C7 C13 C14 -120.1(7) . . . . ?
C1 C7 C13 C14 116.0(7) . . . . ?
C18 C7 C13 C14 -1.4(9) . . . . ?
N2 C13 C14 C15 -1.0(7) . . . . ?
C7 C13 C14 C15 -178.6(6) . . . . ?
C13 C14 C15 C16 0.7(8) . . . . ?
C14 C15 C16 N2 -0.1(7) . . . . ?
C14 C15 C16 C17 -174.5(6) . . . . ?
C13 N2 C16 C15 -0.5(7) . . . . ?
C13 N2 C16 C17 174.2(5) . . . . ?
C15 C16 C17 O2 169.3(6) . . . . ?
N2 C16 C17 O2 -4.3(10) . . . . ?
C4 C3 C19 C20 45.5(7) . . . . ?
C2 C3 C19 C20 -137.4(6) . . . . ?
C4 C3 C19 C25 167.8(5) . . . . ?
C2 C3 C19 C25 -15.1(8) . . . . ?
C4 C3 C19 C30 -74.4(7) . . . . ?
C2 C3 C19 C30 102.7(6) . . . . ?
C23 N3 C20 C21 0.3(7) . . . . ?
C23 N3 C20 C19 177.0(5) . . . . ?
C25 C19 C20 N3 -89.1(6) . . . . ?
C3 C19 C20 N3 35.2(7) . . . . ?
C30 C19 C20 N3 154.0(5) . . . . ?
C25 C19 C20 C21 86.7(8) . . . . ?
C3 C19 C20 C21 -149.0(7) . . . . ?
C30 C19 C20 C21 -30.1(9) . . . . ?
N3 C20 C21 C22 0.1(8) . . . . ?
C19 C20 C21 C22 -176.2(6) . . . . ?
C20 C21 C22 C23 -0.4(9) . . . . ?
C20 N3 C23 C22 -0.5(8) . . . . ?
C20 N3 C23 C24 177.4(7) . . . . ?
C21 C22 C23 N3 0.6(9) . . . . ?
C21 C22 C23 C24 -177.0(8) . . . . ?
N3 C23 C24 O3 179.1(9) . . . . ?
C22 C23 C24 O3 -3.6(16) . . . . ?
C28 N4 C25 C26 -0.1(8) . . . . ?
C28 N4 C25 C19 -178.6(6) . . . . ?
C20 C19 C25 N4 54.7(8) . . . . ?
C3 C19 C25 N4 -68.8(8) . . . . ?
C30 C19 C25 N4 173.1(6) . . . . ?
C20 C19 C25 C26 -123.4(8) . . . . ?
C3 C19 C25 C26 113.1(8) . . . . ?
C30 C19 C25 C26 -5.0(10) . . . . ?
N4 C25 C26 C27 -0.1(8) . . . . ?
C19 C25 C26 C27 178.3(7) . . . . ?
C25 C26 C27 C28 0.2(8) . . . . ?
C25 N4 C28 C27 0.2(8) . . . . ?
C25 N4 C28 C29 178.1(7) . . . . ?
C26 C27 C28 N4 -0.3(9) . . . . ?
C26 C27 C28 C29 -178.1(8) . . . . ?
N4 C28 C29 O4 -0.5(15) . . . . ?
C27 C28 C29 O4 177.0(9) . . . . ?
C4 C5 C31 C32 170.4(5) . . . . ?
C6 C5 C31 C32 -7.3(8) . . . . ?
C4 C5 C31 C42 51.1(8) . . . . ?
C6 C5 C31 C42 -126.7(6) . . . . ?
C4 C5 C31 C37 -68.6(7) . . . . ?
C6 C5 C31 C37 113.6(6) . . . . ?
C35 N5 C32 C33 -0.8(7) . . . . ?
C35 N5 C32 C31 -170.5(6) . . . . ?
C42 C31 C32 N5 -159.3(6) . . . . ?
C37 C31 C32 N5 -42.2(8) . . . . ?
C5 C31 C32 N5 79.8(7) . . . . ?
C42 C31 C32 C33 33.5(9) . . . . ?
C37 C31 C32 C33 150.6(7) . . . . ?
C5 C31 C32 C33 -87.4(8) . . . . ?
N5 C32 C33 C34 0.2(9) . . . . ?
C31 C32 C33 C34 169.1(7) . . . . ?
C32 C33 C34 C35 0.4(10) . . . . ?
C32 N5 C35 C34 1.0(8) . . . . ?
C32 N5 C35 C36 179.1(6) . . . . ?
C33 C34 C35 N5 -0.9(9) . . . . ?
C33 C34 C35 C36 -178.7(8) . . . . ?
N5 C35 C36 O5 178.3(7) . . . . ?
C34 C35 C36 O5 -4.1(13) . . . . ?
C40 N6 C37 C38 -0.9(7) . . . . ?
C40 N6 C37 C31 179.8(6) . . . . ?
C32 C31 C37 N6 102.5(6) . . . . ?
C42 C31 C37 N6 -140.2(6) . . . . ?
C5 C31 C37 N6 -18.8(8) . . . . ?
C32 C31 C37 C38 -76.6(8) . . . . ?
C42 C31 C37 C38 40.7(9) . . . . ?
C5 C31 C37 C38 162.1(7) . . . . ?
N6 C37 C38 C39 1.7(8) . . . . ?
C31 C37 C38 C39 -179.1(6) . . . . ?
C37 C38 C39 C40 -1.8(8) . . . . ?
C38 C39 C40 N6 1.3(8) . . . . ?
C38 C39 C40 C41 -178.7(7) . . . . ?
C37 N6 C40 C39 -0.2(7) . . . . ?
C37 N6 C40 C41 179.8(6) . . . . ?
C39 C40 C41 O6 2.6(12) . . . . ?
N6 C40 C41 O6 -177.4(6) . . . . ?
C13B N1B C1B C2B -50.4(12) . . . . ?
C9B N1B C1B C2B -171.0(11) . . . . ?
C5B N1B C1B C2B 69.7(11) . . . . ?
N1B C1B C2B C3B -164.0(10) . . . . ?
C1B C2B C3B C4B -163.4(13) . . . . ?
C1B N1B C5B C6B 49.1(11) . . . . ?
C13B N1B C5B C6B 169.4(10) . . . . ?
C9B N1B C5B C6B -69.2(11) . . . . ?
N1B C5B C6B C7B 171.6(8) . . . . ?
C5B C6B C7B C8B -74.1(14) . . . . ?
C1B N1B C9B C10B 162.5(11) . . . . ?
C13B N1B C9B C10B 42.8(12) . . . . ?
C5B N1B C9B C10B -77.5(12) . . . . ?
N1B C9B C10B C11B -175.9(10) . . . . ?
C9B C10B C11B C12B -85(2) . . . . ?
C1B N1B C13B C14B -58.0(13) . . . . ?
C9B N1B C13B C14B 60.7(14) . . . . ?
C5B N1B C13B C14B -178.8(12) . . . . ?
N1B C13B C14B C15B 174.1(13) . . . . ?
C13B C14B C15B C16B 161.2(17) . . . . ?
C9C N1C C1C C2C -53.2(11) . . . . ?
C13C N1C C1C C2C 69.5(11) . . . . ?
C5C N1C C1C C2C -170.7(10) . . . . ?
N1C C1C C2C C3C -159.3(11) . . . . ?
C1C C2C C3C C4C -173.9(12) . . . . ?
C1C N1C C5C C6C -70.5(11) . . . . ?
C9C N1C C5C C6C 167.8(10) . . . . ?
C13C N1C C5C C6C 49.8(11) . . . . ?
N1C C5C C6C C7C -178.7(11) . . . . ?
C5C C6C C7C C8C 179.9(13) . . . . ?
C1C N1C C9C C10C -57.4(11) . . . . ?
C13C N1C C9C C10C 179.2(10) . . . . ?
C5C N1C C9C C10C 60.8(11) . . . . ?
N1C C9C C10C C11C -154.6(9) . . . . ?
C9C C10C C11C C12C 78.9(17) . . . . ?
C1C N1C C13C C14C -93.5(13) . . . . ?
C9C N1C C13C C14C 31.4(14) . . . . ?
C5C N1C C13C C14C 147.9(13) . . . . ?
N1C C13C C14C C15C -165.0(11) . . . . ?
C13C C14C C15C C16C 62(2) . . . . ?
C5D N1D C1D C2D 26.3(19) . . . . ?
C13D N1D C1D C2D -96.2(18) . . . . ?
C9D N1D C1D C2D 146.7(17) . . . . ?
N1D C1D C2D C3D -145.7(16) . . . . ?
C1D C2D C3D C4D -152.2(16) . . . . ?
C13D N1D C5D C6D -39.0(16) . . . . ?
C9D N1D C5D C6D 83.0(16) . . . . ?
C1D N1D C5D C6D -159.2(15) . . . . ?
N1D C5D C6D C7D -168.2(15) . . . . ?
C5D C6D C7D C8D 173.1(19) . . . . ?
C5D N1D C9D C10D -94.6(14) . . . . ?
C13D N1D C9D C10D 29.6(15) . . . . ?
C1D N1D C9D C10D 146.7(13) . . . . ?
N1D C9D C10D C11D -146.3(14) . . . . ?
C9D C10D C11D C12D -166.1(15) . . . . ?
C5D N1D C13D C14D -61.7(13) . . . . ?
C9D N1D C13D C14D 174.7(12) . . . . ?
C1D N1D C13D C14D 58.5(13) . . . . ?
N1D C13D C14D C15D -172.4(13) . . . . ?
C13D C14D C15D C16D -168.7(18) . . . . ?

_refine_diff_density_max         1.140
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.115




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform/n-pentane'
