# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_why
_database_code_depnum_ccdc_archive 'CCDC 1439402'
_audit_update_record             
;
2015-11-29 deposited with the CCDC.
2016-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H84 N12 O20'
_chemical_formula_weight         1821.83

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   14.7374(15)
_cell_length_b                   10.6246(9)
_cell_length_c                   19.2318(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.932(6)
_cell_angle_gamma                90.00
_cell_volume                     2438.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3371
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      22.87

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20766
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         27.62
_reflns_number_total             5590
_reflns_number_gt                2672
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1110P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5590
_refine_ls_number_parameters     313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.2111
_refine_ls_wR_factor_gt          0.1509
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.14295(14) 0.50258(15) 0.41076(10) 0.0465(5) Uani 1 1 d . . .
O2 O 0.43398(18) 0.3585(2) 0.64511(13) 0.0776(7) Uani 1 1 d . . .
O5 O 0.2008(2) 0.6791(2) 0.64072(15) 0.0893(8) Uani 1 1 d . . .
O4 O 0.40301(17) 0.5175(2) 0.70514(12) 0.0718(7) Uani 1 1 d . . .
O3 O 0.2924(2) 0.7992(2) 0.60691(15) 0.0903(8) Uani 1 1 d . . .
N1 N 0.3336(3) 0.7001(2) 0.42040(19) 0.0797(9) Uani 1 1 d . . .
N2 N 0.4500(3) 0.3783(3) 0.3571(2) 0.0947(10) Uani 1 1 d . . .
N3 N 0.06342(19) 0.6951(2) 0.41222(13) 0.0511(6) Uani 1 1 d . . .
C11 C 0.2354(2) 0.1990(2) 0.46866(16) 0.0441(6) Uani 1 1 d . . .
C10 C 0.3073(2) 0.3788(2) 0.45023(15) 0.0414(6) Uani 1 1 d . . .
C9 C 0.3122(2) 0.2411(2) 0.45245(16) 0.0437(6) Uani 1 1 d . . .
C23 C 0.2253(2) 0.6021(2) 0.54088(16) 0.0418(6) Uani 1 1 d . . .
C13 C 0.3499(2) 0.4585(2) 0.42218(16) 0.0471(7) Uani 1 1 d . . .
C1 C 0.2297(2) 0.4208(2) 0.47588(15) 0.0416(6) Uani 1 1 d . . .
C17 C -0.0271(2) 0.6948(3) 0.31866(17) 0.0634(8) Uani 1 1 d . . .
C22 C 0.2832(2) 0.4970(2) 0.55775(15) 0.0410(6) Uani 1 1 d . . .
C2 C 0.1827(2) 0.2973(2) 0.48031(16) 0.0458(7) Uani 1 1 d . . .
C16 C 0.1349(2) 0.6087(2) 0.44898(16) 0.0419(6) Uani 1 1 d . . .
C24 C 0.2448(3) 0.7053(3) 0.60014(18) 0.0548(7) Uani 1 1 d . . .
C21 C 0.3817(2) 0.4488(3) 0.64042(17) 0.0514(7) Uani 1 1 d . . .
C8 C 0.3703(2) 0.1529(2) 0.44062(18) 0.0533(7) Uani 1 1 d . . .
H8A H 0.4221 0.1777 0.4305 0.064 Uiso 1 1 calc R . .
C15 C 0.3393(2) 0.5929(3) 0.42152(18) 0.0552(8) Uani 1 1 d . . .
C14 C 0.4071(3) 0.4137(3) 0.38644(19) 0.0582(8) Uani 1 1 d . . .
C6 C 0.2746(3) -0.0149(3) 0.45851(18) 0.0599(8) Uani 1 1 d . . .
H6A H 0.2633 -0.1007 0.4600 0.072 Uiso 1 1 calc R . .
C12 C 0.2135(2) 0.0722(2) 0.47130(18) 0.0529(7) Uani 1 1 d . . .
C7 C 0.3500(2) 0.0252(3) 0.44401(19) 0.0586(8) Uani 1 1 d . . .
H7A H 0.3893 -0.0344 0.4361 0.070 Uiso 1 1 calc R . .
C3 C 0.1036(3) 0.2712(3) 0.4934(2) 0.0642(8) Uani 1 1 d . . .
H3A H 0.0672 0.3353 0.5011 0.077 Uiso 1 1 calc R . .
C5 C 0.1305(3) 0.0474(3) 0.4847(2) 0.0706(9) Uani 1 1 d . . .
H5A H 0.1114 -0.0354 0.4865 0.085 Uiso 1 1 calc R . .
C4 C 0.0785(3) 0.1437(3) 0.4950(2) 0.0774(10) Uani 1 1 d . . .
H4A H 0.0240 0.1245 0.5035 0.093 Uiso 1 1 calc R . .
C19 C -0.0933(4) 0.8139(4) 0.3007(2) 0.1186(16) Uani 1 1 d . . .
H19A H -0.1245 0.8130 0.3327 0.178 Uiso 1 1 calc R . .
H19B H -0.1527 0.8191 0.2405 0.178 Uiso 1 1 calc R . .
H19C H -0.0448 0.8854 0.3176 0.178 Uiso 1 1 calc R . .
C18 C -0.1028(3) 0.5829(4) 0.2951(2) 0.1070(14) Uani 1 1 d . . .
H18A H -0.0613 0.5068 0.3060 0.161 Uiso 1 1 calc R . .
H18B H -0.1642 0.5872 0.2353 0.161 Uiso 1 1 calc R . .
H18C H -0.1312 0.5833 0.3290 0.161 Uiso 1 1 calc R . .
C20 C 0.0230(3) 0.6963(4) 0.2686(2) 0.1019(13) Uani 1 1 d . . .
H20A H 0.0751 0.7648 0.2881 0.153 Uiso 1 1 calc R . .
H20B H -0.0357 0.7067 0.2085 0.153 Uiso 1 1 calc R . .
H20C H 0.0613 0.6183 0.2774 0.153 Uiso 1 1 calc R . .
C25 C 0.5018(3) 0.4849(5) 0.7894(2) 0.1154(15) Uani 1 1 d . . .
H25A H 0.4971 0.3985 0.8016 0.173 Uiso 1 1 calc R . .
H25B H 0.5065 0.5380 0.8318 0.173 Uiso 1 1 calc R . .
H25C H 0.5673 0.4965 0.7906 0.173 Uiso 1 1 calc R . .
C26 C 0.2275(5) 0.7698(5) 0.7076(3) 0.154(2) Uani 1 1 d . . .
H26A H 0.3074 0.7769 0.7481 0.231 Uiso 1 1 calc R . .
H26B H 0.1962 0.7415 0.7367 0.231 Uiso 1 1 calc R . .
H26C H 0.1965 0.8504 0.6819 0.231 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C16 1.389(3) . ?
O1 C1 1.442(3) . ?
O2 C21 1.200(3) . ?
O5 C24 1.304(3) . ?
O5 C26 1.465(4) . ?
O4 C21 1.312(3) . ?
O4 C25 1.448(4) . ?
O3 C24 1.182(3) . ?
N1 C15 1.141(3) . ?
N2 C14 1.132(3) . ?
N3 C16 1.256(3) . ?
N3 C17 1.483(3) . ?
C11 C12 1.394(3) . ?
C11 C2 1.395(3) . ?
C11 C9 1.412(3) . ?
C10 C13 1.342(3) . ?
C10 C9 1.464(4) . ?
C10 C1 1.552(3) . ?
C9 C8 1.375(3) . ?
C23 C22 1.325(3) . ?
C23 C16 1.463(3) . ?
C23 C24 1.483(4) . ?
C13 C15 1.436(4) . ?
C13 C14 1.445(4) . ?
C1 C2 1.510(3) . ?
C1 C22 1.517(3) . ?
C17 C18 1.507(4) . ?
C17 C19 1.510(4) . ?
C17 C20 1.519(5) . ?
C22 C21 1.479(4) . ?
C2 C3 1.359(4) . ?
C8 C7 1.399(4) . ?
C8 H8A 0.9300 . ?
C6 C7 1.363(4) . ?
C6 C12 1.410(4) . ?
C6 H6A 0.9300 . ?
C12 C5 1.415(4) . ?
C7 H7A 0.9300 . ?
C3 C4 1.410(4) . ?
C3 H3A 0.9300 . ?
C5 C4 1.361(4) . ?
C5 H5A 0.9300 . ?
C4 H4A 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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
C16 O1 C1 109.73(17) . . ?
C24 O5 C26 114.4(3) . . ?
C21 O4 C25 116.9(3) . . ?
C16 N3 C17 122.7(2) . . ?
C12 C11 C2 123.7(2) . . ?
C12 C11 C9 123.2(2) . . ?
C2 C11 C9 113.1(2) . . ?
C13 C10 C9 128.0(2) . . ?
C13 C10 C1 123.5(2) . . ?
C9 C10 C1 108.1(2) . . ?
C8 C9 C11 118.6(2) . . ?
C8 C9 C10 134.5(2) . . ?
C11 C9 C10 106.9(2) . . ?
C22 C23 C16 109.6(2) . . ?
C22 C23 C24 128.9(2) . . ?
C16 C23 C24 121.4(2) . . ?
C10 C13 C15 123.9(2) . . ?
C10 C13 C14 121.6(2) . . ?
C15 C13 C14 114.5(2) . . ?
O1 C1 C2 111.73(19) . . ?
O1 C1 C22 103.61(18) . . ?
C2 C1 C22 112.45(19) . . ?
O1 C1 C10 109.89(18) . . ?
C2 C1 C10 102.49(19) . . ?
C22 C1 C10 116.9(2) . . ?
N3 C17 C18 110.3(3) . . ?
N3 C17 C19 106.0(2) . . ?
C18 C17 C19 109.1(3) . . ?
N3 C17 C20 110.1(3) . . ?
C18 C17 C20 111.6(3) . . ?
C19 C17 C20 109.6(3) . . ?
C23 C22 C21 129.8(2) . . ?
C23 C22 C1 109.2(2) . . ?
C21 C22 C1 121.0(2) . . ?
C3 C2 C11 119.8(2) . . ?
C3 C2 C1 131.3(2) . . ?
C11 C2 C1 108.9(2) . . ?
N3 C16 O1 126.8(2) . . ?
N3 C16 C23 125.7(2) . . ?
O1 C16 C23 107.5(2) . . ?
O3 C24 O5 125.8(3) . . ?
O3 C24 C23 122.9(3) . . ?
O5 C24 C23 111.2(3) . . ?
O2 C21 O4 126.0(3) . . ?
O2 C21 C22 122.6(3) . . ?
O4 C21 C22 111.4(2) . . ?
C9 C8 C7 118.9(3) . . ?
C9 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 . . ?
N1 C15 C13 177.6(3) . . ?
N2 C14 C13 178.8(4) . . ?
C7 C6 C12 120.8(3) . . ?
C7 C6 H6A 119.6 . . ?
C12 C6 H6A 119.6 . . ?
C11 C12 C6 116.3(3) . . ?
C11 C12 C5 115.5(3) . . ?
C6 C12 C5 128.2(3) . . ?
C6 C7 C8 122.3(3) . . ?
C6 C7 H7A 118.8 . . ?
C8 C7 H7A 118.8 . . ?
C2 C3 C4 117.7(3) . . ?
C2 C3 H3A 121.2 . . ?
C4 C3 H3A 121.2 . . ?
C4 C5 C12 120.5(3) . . ?
C4 C5 H5A 119.8 . . ?
C12 C5 H5A 119.8 . . ?
C5 C4 C3 122.9(3) . . ?
C5 C4 H4A 118.6 . . ?
C3 C4 H4A 118.6 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O5 C26 H26A 109.5 . . ?
O5 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O5 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.189
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_why-jie0525
_database_code_depnum_ccdc_archive 'CCDC 1439403'
_audit_update_record             
;
2015-11-29 deposited with the CCDC.
2016-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H21 N3 O5'
_chemical_formula_weight         455.46

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   28.1196(15)
_cell_length_b                   10.6029(6)
_cell_length_c                   31.9973(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.631(3)
_cell_angle_gamma                90.00
_cell_volume                     9431.9(9)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9887
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.26

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3808
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39411
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         27.45
_reflns_number_total             10769
_reflns_number_gt                7367
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0596P)²+4.3687P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10769
_refine_ls_number_parameters     623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1358
_refine_ls_wR_factor_gt          0.1207
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N5 N 0.34985(4) 1.06972(11) 0.05622(4) 0.0352(3) Uani 1 1 d . . .
C2 C 0.42324(5) 0.92164(14) 0.06865(5) 0.0345(3) Uani 1 1 d . . .
C11 C 0.34684(5) 0.84362(14) 0.08318(5) 0.0359(3) Uani 1 1 d . . .
C12 C 0.37724(5) 0.74365(14) 0.07587(5) 0.0360(3) Uani 1 1 d . . .
C3 C 0.42260(5) 0.78360(14) 0.06712(5) 0.0356(3) Uani 1 1 d . . .
C13 C 0.45896(5) 1.00072(15) 0.06170(5) 0.0390(4) Uani 1 1 d . . .
C1 C 0.37452(5) 0.96706(14) 0.08163(5) 0.0332(3) Uani 1 1 d . . .
C22 C 0.34306(5) 1.17258(14) 0.08085(5) 0.0388(4) Uani 1 1 d . . .
C18 C 0.36731(5) 1.14325(15) 0.12438(5) 0.0388(4) Uani 1 1 d . . .
C10 C 0.30192(6) 0.81859(16) 0.09214(6) 0.0458(4) Uani 1 1 d . . .
H10 H 0.2816 0.8837 0.0977 0.055 Uiso 1 1 calc R . .
O4 O 0.41321(5) 1.23532(14) 0.18193(4) 0.0664(4) Uani 1 1 d . . .
C7 C 0.36342(6) 0.61641(15) 0.07711(5) 0.0418(4) Uani 1 1 d . . .
C17 C 0.38396(5) 1.02615(15) 0.12540(5) 0.0353(3) Uani 1 1 d . . .
C4 C 0.45564(6) 0.69274(16) 0.05980(5) 0.0447(4) Uani 1 1 d . . .
H4 H 0.4859 0.7156 0.0540 0.054 Uiso 1 1 calc R . .
C6 C 0.39830(7) 0.52692(16) 0.06943(6) 0.0506(4) Uani 1 1 d . . .
H6 H 0.3912 0.4413 0.0699 0.061 Uiso 1 1 calc R . .
C16 C 0.40931(6) 0.95659(17) 0.16246(5) 0.0457(4) Uani 1 1 d . . .
C5 C 0.44247(7) 0.56489(16) 0.06125(6) 0.0524(5) Uani 1 1 d . . .
H5 H 0.4647 0.5037 0.0564 0.063 Uiso 1 1 calc R . .
C23 C 0.32804(6) 1.06388(16) 0.01020(5) 0.0420(4) Uani 1 1 d . . .
C9 C 0.28683(7) 0.69103(18) 0.09281(6) 0.0532(5) Uani 1 1 d . . .
H9 H 0.2559 0.6735 0.0982 0.064 Uiso 1 1 calc R . .
C8 C 0.31621(7) 0.59313(17) 0.08577(6) 0.0514(4) Uani 1 1 d . . .
H8 H 0.3052 0.5106 0.0867 0.062 Uiso 1 1 calc R . .
C14 C 0.45637(6) 1.13561(18) 0.06549(6) 0.0506(4) Uani 1 1 d . . .
C19 C 0.37019(6) 1.23345(17) 0.16010(6) 0.0503(4) Uani 1 1 d . . .
N1 N 0.53823(6) 0.91891(19) 0.04030(6) 0.0717(5) Uani 1 1 d . . .
O2 O 0.38807(6) 0.96532(17) 0.19513(5) 0.0842(5) Uani 1 1 d . . .
C15 C 0.50329(6) 0.95426(17) 0.04990(6) 0.0469(4) Uani 1 1 d . . .
N2 N 0.45635(7) 1.24249(16) 0.06852(8) 0.0805(6) Uani 1 1 d . . .
O1 O 0.44496(7) 0.9016(2) 0.16186(5) 0.1278(9) Uani 1 1 d . . .
C26 C 0.34421(8) 0.94512(18) -0.01076(6) 0.0598(5) Uani 1 1 d . . .
H26A H 0.3786 0.9447 -0.0085 0.090 Uiso 1 1 calc R . .
H26B H 0.3303 0.9441 -0.0401 0.090 Uiso 1 1 calc R . .
H26C H 0.3339 0.8719 0.0031 0.090 Uiso 1 1 calc R . .
O3 O 0.33708(6) 1.2920(2) 0.16851(6) 0.1129(8) Uani 1 1 d . . .
N6 N 0.13571(5) -0.05879(12) 0.12030(4) 0.0368(3) Uani 1 1 d . . .
C28 C 0.08040(5) 0.09223(15) 0.15391(5) 0.0371(4) Uani 1 1 d . . .
C29 C 0.08016(6) 0.22991(15) 0.15079(5) 0.0399(4) Uani 1 1 d . . .
C27 C 0.13204(5) 0.04551(14) 0.14993(5) 0.0355(3) Uani 1 1 d . . .
C48 C 0.16303(6) -0.15543(15) 0.13987(5) 0.0412(4) Uani 1 1 d . . .
C38 C 0.12613(6) 0.26831(15) 0.14349(5) 0.0402(4) Uani 1 1 d . . .
C37 C 0.15771(6) 0.16791(15) 0.14103(5) 0.0390(4) Uani 1 1 d . . .
C42 C 0.15630(6) 0.06093(17) 0.23187(5) 0.0468(4) Uani 1 1 d . . .
O6 O 0.17935(5) -0.29879(14) 0.22833(5) 0.0698(4) Uani 1 1 d . . .
C39 C 0.04466(6) 0.01438(16) 0.16190(5) 0.0434(4) Uani 1 1 d . . .
O8 O 0.18244(5) 0.00602(12) 0.26394(4) 0.0607(4) Uani 1 1 d . . .
C43 C 0.15637(5) -0.00967(15) 0.19169(5) 0.0382(4) Uani 1 1 d . . .
C33 C 0.13982(7) 0.39530(16) 0.14032(6) 0.0488(4) Uani 1 1 d . . .
C49 C 0.11912(6) -0.05830(17) 0.07324(5) 0.0448(4) Uani 1 1 d . . .
C30 C 0.04618(7) 0.32135(17) 0.15493(6) 0.0502(4) Uani 1 1 d . . .
H30 H 0.0154 0.2992 0.1595 0.060 Uiso 1 1 calc R . .
C41 C 0.05036(6) -0.11974(18) 0.16575(6) 0.0494(4) Uani 1 1 d . . .
O5 O 0.24769(5) -0.19632(15) 0.22402(6) 0.0860(5) Uani 1 1 d . . .
C35 C 0.21823(7) 0.31868(19) 0.13070(6) 0.0578(5) Uani 1 1 d . . .
H35 H 0.2494 0.3352 0.1259 0.069 Uiso 1 1 calc R . .
C44 C 0.17484(6) -0.12211(15) 0.18538(5) 0.0406(4) Uani 1 1 d . . .
C36 C 0.20374(6) 0.19107(18) 0.13485(6) 0.0492(4) Uani 1 1 d . . .
H36 H 0.2252 0.1252 0.1334 0.059 Uiso 1 1 calc R . .
N4 N 0.05314(7) -0.22682(17) 0.16965(7) 0.0747(5) Uani 1 1 d . . .
C31 C 0.05937(7) 0.44894(17) 0.15210(6) 0.0563(5) Uani 1 1 d . . .
H31 H 0.0367 0.5107 0.1551 0.068 Uiso 1 1 calc R . .
C50 C 0.08891(7) 0.05865(19) 0.06002(6) 0.0574(5) Uani 1 1 d . . .
H50A H 0.0608 0.0583 0.0737 0.086 Uiso 1 1 calc R . .
H50B H 0.0795 0.0583 0.0299 0.086 Uiso 1 1 calc R . .
H50C H 0.1075 0.1330 0.0682 0.086 Uiso 1 1 calc R . .
C32 C 0.10417(8) 0.48589(17) 0.14506(6) 0.0583(5) Uani 1 1 d . . .
H32 H 0.1112 0.5713 0.1434 0.070 Uiso 1 1 calc R . .
C34 C 0.18789(7) 0.41693(19) 0.13352(6) 0.0591(5) Uani 1 1 d . . .
H34 H 0.1987 0.4991 0.1310 0.071 Uiso 1 1 calc R . .
O7 O 0.13416(7) 0.15492(18) 0.23436(5) 0.1048(7) Uani 1 1 d . . .
C45 C 0.20522(6) -0.20828(18) 0.21524(6) 0.0498(4) Uani 1 1 d . . .
C40 C -0.00152(7) 0.06022(19) 0.16921(7) 0.0592(5) Uani 1 1 d . . .
C46 C 0.18323(10) 0.0684(2) 0.30471(6) 0.0750(7) Uani 1 1 d . . .
H46A H 0.1952 0.1528 0.3031 0.113 Uiso 1 1 calc R . .
H46B H 0.2038 0.0224 0.3261 0.113 Uiso 1 1 calc R . .
H46C H 0.1512 0.0710 0.3117 0.113 Uiso 1 1 calc R . .
C52 C 0.08795(8) -0.1752(2) 0.06191(7) 0.0686(6) Uani 1 1 d . . .
H52A H 0.1063 -0.2496 0.0707 0.103 Uiso 1 1 calc R . .
H52B H 0.0778 -0.1778 0.0319 0.103 Uiso 1 1 calc R . .
H52C H 0.0602 -0.1716 0.0761 0.103 Uiso 1 1 calc R . .
N3 N -0.03826(7) 0.0910(2) 0.17600(8) 0.0972(7) Uani 1 1 d . . .
C25 C 0.27333(6) 1.0636(2) 0.00733(7) 0.0621(5) Uani 1 1 d . . .
H25A H 0.2632 0.9864 0.0190 0.093 Uiso 1 1 calc R . .
H25B H 0.2589 1.0703 -0.0217 0.093 Uiso 1 1 calc R . .
H25C H 0.2635 1.1338 0.0229 0.093 Uiso 1 1 calc R . .
C24 C 0.34531(8) 1.17858(19) -0.01235(6) 0.0600(5) Uani 1 1 d . . .
H24A H 0.3348 1.2544 -0.0001 0.090 Uiso 1 1 calc R . .
H24B H 0.3321 1.1755 -0.0418 0.090 Uiso 1 1 calc R . .
H24C H 0.3798 1.1778 -0.0093 0.090 Uiso 1 1 calc R . .
C51 C 0.16309(8) -0.0582(2) 0.05063(6) 0.0685(6) Uani 1 1 d . . .
H51A H 0.1820 0.0159 0.0585 0.103 Uiso 1 1 calc R . .
H51B H 0.1529 -0.0584 0.0206 0.103 Uiso 1 1 calc R . .
H51C H 0.1821 -0.1319 0.0586 0.103 Uiso 1 1 calc R . .
C21 C 0.42028(9) 1.3090(3) 0.22046(7) 0.0832(7) Uani 1 1 d . . .
H21A H 0.4161 1.3969 0.2136 0.125 Uiso 1 1 calc R . .
H21B H 0.4522 1.2950 0.2352 0.125 Uiso 1 1 calc R . .
H21C H 0.3972 1.2839 0.2381 0.125 Uiso 1 1 calc R . .
C47 C 0.20536(10) -0.3945(3) 0.25568(10) 0.1088(11) Uani 1 1 d . . .
H47A H 0.2215 -0.4507 0.2390 0.163 Uiso 1 1 calc R . .
H47B H 0.1831 -0.4413 0.2696 0.163 Uiso 1 1 calc R . .
H47C H 0.2286 -0.3542 0.2765 0.163 Uiso 1 1 calc R . .
C20 C 0.41295(12) 0.9076(3) 0.23402(8) 0.1164(11) Uani 1 1 d . . .
H20A H 0.4216 0.8224 0.2283 0.175 Uiso 1 1 calc R . .
H20B H 0.3921 0.9077 0.2552 0.175 Uiso 1 1 calc R . .
H20C H 0.4415 0.9550 0.2440 0.175 Uiso 1 1 calc R . .
O9 O 0.17591(5) -0.25121(11) 0.12350(4) 0.0569(3) Uani 1 1 d . . .
O10 O 0.32103(5) 1.26896(11) 0.06967(4) 0.0552(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N5 C22 1.375(2) . ?
N5 C1 1.4689(19) . ?
N5 C23 1.509(2) . ?
C2 C13 1.352(2) . ?
C2 C3 1.464(2) . ?
C2 C1 1.566(2) . ?
C11 C10 1.363(2) . ?
C11 C12 1.403(2) . ?
C11 C1 1.527(2) . ?
C12 C7 1.406(2) . ?
C12 C3 1.412(2) . ?
C3 C4 1.382(2) . ?
C13 C14 1.438(2) . ?
C13 C15 1.442(2) . ?
C1 C17 1.521(2) . ?
C22 O10 1.2204(18) . ?
C22 C18 1.489(2) . ?
C18 C17 1.326(2) . ?
C18 C19 1.483(2) . ?
C10 C9 1.419(2) . ?
O4 C19 1.303(2) . ?
O4 C21 1.448(2) . ?
C7 C6 1.413(2) . ?
C7 C8 1.418(3) . ?
C17 C16 1.485(2) . ?
C4 C5 1.408(2) . ?
C6 C5 1.368(3) . ?
C16 O1 1.163(2) . ?
C16 O2 1.283(2) . ?
C23 C25 1.527(2) . ?
C23 C26 1.528(2) . ?
C23 C24 1.530(2) . ?
C9 C8 1.366(3) . ?
C14 N2 1.137(2) . ?
C19 O3 1.183(2) . ?
N1 C15 1.136(2) . ?
O2 C20 1.467(3) . ?
N6 C48 1.374(2) . ?
N6 C27 1.4703(19) . ?
N6 C49 1.508(2) . ?
C28 C39 1.354(2) . ?
C28 C29 1.463(2) . ?
C28 C27 1.558(2) . ?
C29 C30 1.382(2) . ?
C29 C38 1.408(2) . ?
C27 C43 1.524(2) . ?
C27 C37 1.532(2) . ?
C48 O9 1.2221(19) . ?
C48 C44 1.487(2) . ?
C38 C37 1.396(2) . ?
C38 C33 1.408(2) . ?
C37 C36 1.361(2) . ?
C42 O7 1.184(2) . ?
C42 O8 1.306(2) . ?
C42 C43 1.488(2) . ?
O6 C45 1.310(2) . ?
O6 C47 1.462(2) . ?
C39 C41 1.434(3) . ?
C39 C40 1.438(2) . ?
O8 C46 1.460(2) . ?
C43 C44 1.328(2) . ?
C33 C32 1.413(3) . ?
C33 C34 1.420(3) . ?
C49 C51 1.523(3) . ?
C49 C50 1.526(3) . ?
C49 C52 1.530(3) . ?
C30 C31 1.409(3) . ?
C41 N4 1.144(2) . ?
O5 C45 1.192(2) . ?
C35 C34 1.358(3) . ?
C35 C36 1.425(3) . ?
C44 C45 1.494(2) . ?
C31 C32 1.370(3) . ?
C40 N3 1.135(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 N5 C1 111.42(12) . . ?
C22 N5 C23 121.36(12) . . ?
C1 N5 C23 126.77(12) . . ?
C13 C2 C3 128.30(14) . . ?
C13 C2 C1 123.64(13) . . ?
C3 C2 C1 108.03(13) . . ?
C10 C11 C12 119.67(15) . . ?
C10 C11 C1 131.82(14) . . ?
C12 C11 C1 108.41(13) . . ?
C11 C12 C7 122.84(15) . . ?
C11 C12 C3 113.43(13) . . ?
C7 C12 C3 123.73(14) . . ?
C4 C3 C12 118.34(14) . . ?
C4 C3 C2 134.19(15) . . ?
C12 C3 C2 107.46(13) . . ?
C2 C13 C14 123.68(14) . . ?
C2 C13 C15 121.59(15) . . ?
C14 C13 C15 114.74(15) . . ?
N5 C1 C17 101.95(11) . . ?
N5 C1 C11 116.89(12) . . ?
C17 C1 C11 110.03(12) . . ?
N5 C1 C2 116.13(12) . . ?
C17 C1 C2 109.40(12) . . ?
C11 C1 C2 102.44(11) . . ?
O10 C22 N5 127.17(16) . . ?
O10 C22 C18 126.16(15) . . ?
N5 C22 C18 106.66(13) . . ?
C17 C18 C19 127.36(15) . . ?
C17 C18 C22 109.22(14) . . ?
C19 C18 C22 123.40(14) . . ?
C11 C10 C9 118.54(16) . . ?
C19 O4 C21 117.55(16) . . ?
C12 C7 C6 115.95(16) . . ?
C12 C7 C8 116.31(15) . . ?
C6 C7 C8 127.74(16) . . ?
C18 C17 C16 127.61(15) . . ?
C18 C17 C1 110.55(13) . . ?
C16 C17 C1 121.83(13) . . ?
C3 C4 C5 118.60(16) . . ?
C5 C6 C7 120.65(16) . . ?
O1 C16 O2 123.91(18) . . ?
O1 C16 C17 123.21(16) . . ?
O2 C16 C17 112.87(15) . . ?
C6 C5 C4 122.72(16) . . ?
N5 C23 C25 108.48(14) . . ?
N5 C23 C26 110.98(13) . . ?
C25 C23 C26 109.60(15) . . ?
N5 C23 C24 108.44(14) . . ?
C25 C23 C24 111.19(15) . . ?
C26 C23 C24 108.15(15) . . ?
C8 C9 C10 122.14(16) . . ?
C9 C8 C7 120.47(16) . . ?
N2 C14 C13 177.14(19) . . ?
O3 C19 O4 124.67(17) . . ?
O3 C19 C18 124.06(17) . . ?
O4 C19 C18 111.21(15) . . ?
C16 O2 C20 116.12(18) . . ?
N1 C15 C13 179.2(2) . . ?
C48 N6 C27 110.84(13) . . ?
C48 N6 C49 121.71(13) . . ?
C27 N6 C49 126.87(12) . . ?
C39 C28 C29 128.70(15) . . ?
C39 C28 C27 123.30(14) . . ?
C29 C28 C27 107.84(13) . . ?
C30 C29 C38 118.59(15) . . ?
C30 C29 C28 133.60(16) . . ?
C38 C29 C28 107.77(13) . . ?
N6 C27 C43 102.18(12) . . ?
N6 C27 C37 115.89(12) . . ?
C43 C27 C37 109.04(12) . . ?
N6 C27 C28 116.65(12) . . ?
C43 C27 C28 110.59(12) . . ?
C37 C27 C28 102.53(12) . . ?
O9 C48 N6 127.29(16) . . ?
O9 C48 C44 125.46(15) . . ?
N6 C48 C44 107.25(13) . . ?
C37 C38 C29 113.36(14) . . ?
C37 C38 C33 122.81(16) . . ?
C29 C38 C33 123.80(15) . . ?
C36 C37 C38 119.84(15) . . ?
C36 C37 C27 131.66(15) . . ?
C38 C37 C27 108.30(13) . . ?
O7 C42 O8 124.19(17) . . ?
O7 C42 C43 123.41(16) . . ?
O8 C42 C43 112.39(15) . . ?
C45 O6 C47 116.59(17) . . ?
C28 C39 C41 122.96(15) . . ?
C28 C39 C40 122.58(16) . . ?
C41 C39 C40 114.39(16) . . ?
C42 O8 C46 115.56(16) . . ?
C44 C43 C42 129.37(15) . . ?
C44 C43 C27 110.23(14) . . ?
C42 C43 C27 120.39(14) . . ?
C38 C33 C32 115.87(17) . . ?
C38 C33 C34 116.25(17) . . ?
C32 C33 C34 127.87(17) . . ?
N6 C49 C51 108.83(14) . . ?
N6 C49 C50 110.82(13) . . ?
C51 C49 C50 108.98(16) . . ?
N6 C49 C52 108.30(14) . . ?
C51 C49 C52 111.42(16) . . ?
C50 C49 C52 108.50(16) . . ?
C29 C30 C31 118.36(17) . . ?
N4 C41 C39 177.0(2) . . ?
C34 C35 C36 122.07(18) . . ?
C43 C44 C48 109.11(14) . . ?
C43 C44 C45 130.61(16) . . ?
C48 C44 C45 120.21(14) . . ?
C37 C36 C35 118.45(17) . . ?
C32 C31 C30 122.86(17) . . ?
C31 C32 C33 120.53(17) . . ?
C35 C34 C33 120.55(17) . . ?
O5 C45 O6 125.96(17) . . ?
O5 C45 C44 122.84(18) . . ?
O6 C45 C44 111.14(15) . . ?
N3 C40 C39 176.6(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
C10 C11 C12 C7 0.4(2) . . . . ?
C1 C11 C12 C7 177.03(14) . . . . ?
C10 C11 C12 C3 -179.80(15) . . . . ?
C1 C11 C12 C3 -3.14(18) . . . . ?
C11 C12 C3 C4 179.41(14) . . . . ?
C7 C12 C3 C4 -0.8(2) . . . . ?
C11 C12 C3 C2 0.10(18) . . . . ?
C7 C12 C3 C2 179.93(14) . . . . ?
C13 C2 C3 C4 1.9(3) . . . . ?
C1 C2 C3 C4 -176.25(17) . . . . ?
C13 C2 C3 C12 -178.98(15) . . . . ?
C1 C2 C3 C12 2.90(16) . . . . ?
C3 C2 C13 C14 -177.75(16) . . . . ?
C1 C2 C13 C14 0.1(2) . . . . ?
C3 C2 C13 C15 2.0(3) . . . . ?
C1 C2 C13 C15 179.82(14) . . . . ?
C22 N5 C1 C17 -2.72(15) . . . . ?
C23 N5 C1 C17 -175.09(13) . . . . ?
C22 N5 C1 C11 117.27(14) . . . . ?
C23 N5 C1 C11 -55.10(19) . . . . ?
C22 N5 C1 C2 -121.54(14) . . . . ?
C23 N5 C1 C2 66.09(18) . . . . ?
C10 C11 C1 N5 -51.2(2) . . . . ?
C12 C11 C1 N5 132.68(13) . . . . ?
C10 C11 C1 C17 64.4(2) . . . . ?
C12 C11 C1 C17 -111.73(14) . . . . ?
C10 C11 C1 C2 -179.36(17) . . . . ?
C12 C11 C1 C2 4.54(15) . . . . ?
C13 C2 C1 N5 48.7(2) . . . . ?
C3 C2 C1 N5 -133.11(13) . . . . ?
C13 C2 C1 C17 -66.01(18) . . . . ?
C3 C2 C1 C17 112.22(14) . . . . ?
C13 C2 C1 C11 177.28(14) . . . . ?
C3 C2 C1 C11 -4.49(15) . . . . ?
C1 N5 C22 O10 -174.83(15) . . . . ?
C23 N5 C22 O10 -2.0(2) . . . . ?
C1 N5 C22 C18 4.38(16) . . . . ?
C23 N5 C22 C18 177.23(13) . . . . ?
O10 C22 C18 C17 174.73(16) . . . . ?
N5 C22 C18 C17 -4.49(17) . . . . ?
O10 C22 C18 C19 -3.8(3) . . . . ?
N5 C22 C18 C19 177.00(15) . . . . ?
C12 C11 C10 C9 -1.5(2) . . . . ?
C1 C11 C10 C9 -177.23(16) . . . . ?
C11 C12 C7 C6 -179.45(15) . . . . ?
C3 C12 C7 C6 0.7(2) . . . . ?
C11 C12 C7 C8 0.7(2) . . . . ?
C3 C12 C7 C8 -179.11(15) . . . . ?
C19 C18 C17 C16 0.3(3) . . . . ?
C22 C18 C17 C16 -178.17(15) . . . . ?
C19 C18 C17 C1 -178.75(15) . . . . ?
C22 C18 C17 C1 2.81(17) . . . . ?
N5 C1 C17 C18 -0.21(16) . . . . ?
C11 C1 C17 C18 -124.91(14) . . . . ?
C2 C1 C17 C18 123.28(14) . . . . ?
N5 C1 C17 C16 -179.30(13) . . . . ?
C11 C1 C17 C16 56.01(18) . . . . ?
C2 C1 C17 C16 -55.80(18) . . . . ?
C12 C3 C4 C5 0.2(2) . . . . ?
C2 C3 C4 C5 179.32(17) . . . . ?
C12 C7 C6 C5 -0.2(2) . . . . ?
C8 C7 C6 C5 179.61(18) . . . . ?
C18 C17 C16 O1 -131.3(2) . . . . ?
C1 C17 C16 O1 47.6(3) . . . . ?
C18 C17 C16 O2 47.8(2) . . . . ?
C1 C17 C16 O2 -133.31(17) . . . . ?
C7 C6 C5 C4 -0.3(3) . . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C22 N5 C23 C25 -64.08(19) . . . . ?
C1 N5 C23 C25 107.60(17) . . . . ?
C22 N5 C23 C26 175.46(15) . . . . ?
C1 N5 C23 C26 -12.9(2) . . . . ?
C22 N5 C23 C24 56.80(19) . . . . ?
C1 N5 C23 C24 -131.52(15) . . . . ?
C11 C10 C9 C8 1.6(3) . . . . ?
C10 C9 C8 C7 -0.5(3) . . . . ?
C12 C7 C8 C9 -0.6(3) . . . . ?
C6 C7 C8 C9 179.55(18) . . . . ?
C2 C13 C14 N2 164(5) . . . . ?
C15 C13 C14 N2 -15(5) . . . . ?
C21 O4 C19 O3 3.5(3) . . . . ?
C21 O4 C19 C18 -173.61(18) . . . . ?
C17 C18 C19 O3 -131.1(2) . . . . ?
C22 C18 C19 O3 47.1(3) . . . . ?
C17 C18 C19 O4 46.0(2) . . . . ?
C22 C18 C19 O4 -135.73(17) . . . . ?
O1 C16 O2 C20 3.8(4) . . . . ?
C17 C16 O2 C20 -175.3(2) . . . . ?
C2 C13 C15 N1 144(70) . . . . ?
C14 C13 C15 N1 -36(18) . . . . ?
C39 C28 C29 C30 0.6(3) . . . . ?
C27 C28 C29 C30 -174.85(18) . . . . ?
C39 C28 C29 C38 178.00(16) . . . . ?
C27 C28 C29 C38 2.54(17) . . . . ?
C48 N6 C27 C43 -6.47(16) . . . . ?
C49 N6 C27 C43 -177.76(13) . . . . ?
C48 N6 C27 C37 111.93(14) . . . . ?
C49 N6 C27 C37 -59.36(19) . . . . ?
C48 N6 C27 C28 -127.19(14) . . . . ?
C49 N6 C27 C28 61.52(19) . . . . ?
C39 C28 C27 N6 52.3(2) . . . . ?
C29 C28 C27 N6 -131.97(14) . . . . ?
C39 C28 C27 C43 -63.88(19) . . . . ?
C29 C28 C27 C43 111.88(14) . . . . ?
C39 C28 C27 C37 179.99(15) . . . . ?
C29 C28 C27 C37 -4.25(16) . . . . ?
C27 N6 C48 O9 -174.24(16) . . . . ?
C49 N6 C48 O9 -2.4(2) . . . . ?
C27 N6 C48 C44 5.32(17) . . . . ?
C49 N6 C48 C44 177.13(13) . . . . ?
C30 C29 C38 C37 178.33(15) . . . . ?
C28 C29 C38 C37 0.48(19) . . . . ?
C30 C29 C38 C33 0.3(2) . . . . ?
C28 C29 C38 C33 -177.52(15) . . . . ?
C29 C38 C37 C36 -178.78(15) . . . . ?
C33 C38 C37 C36 -0.8(2) . . . . ?
C29 C38 C37 C27 -3.35(18) . . . . ?
C33 C38 C37 C27 174.67(15) . . . . ?
N6 C27 C37 C36 -52.6(2) . . . . ?
C43 C27 C37 C36 62.0(2) . . . . ?
C28 C27 C37 C36 179.22(17) . . . . ?
N6 C27 C37 C38 132.73(14) . . . . ?
C43 C27 C37 C38 -112.72(14) . . . . ?
C28 C27 C37 C38 4.53(16) . . . . ?
C29 C28 C39 C41 -177.49(16) . . . . ?
C27 C28 C39 C41 -2.7(3) . . . . ?
C29 C28 C39 C40 -0.5(3) . . . . ?
C27 C28 C39 C40 174.31(16) . . . . ?
O7 C42 O8 C46 -0.1(3) . . . . ?
C43 C42 O8 C46 -178.65(16) . . . . ?
O7 C42 C43 C44 -171.5(2) . . . . ?
O8 C42 C43 C44 7.1(3) . . . . ?
O7 C42 C43 C27 7.4(3) . . . . ?
O8 C42 C43 C27 -173.98(14) . . . . ?
N6 C27 C43 C44 5.38(16) . . . . ?
C37 C27 C43 C44 -117.77(15) . . . . ?
C28 C27 C43 C44 130.22(14) . . . . ?
N6 C27 C43 C42 -173.73(14) . . . . ?
C37 C27 C43 C42 63.11(18) . . . . ?
C28 C27 C43 C42 -48.90(19) . . . . ?
C37 C38 C33 C32 -177.67(16) . . . . ?
C29 C38 C33 C32 0.1(2) . . . . ?
C37 C38 C33 C34 1.3(2) . . . . ?
C29 C38 C33 C34 179.08(16) . . . . ?
C48 N6 C49 C51 -61.0(2) . . . . ?
C27 N6 C49 C51 109.47(18) . . . . ?
C48 N6 C49 C50 179.22(15) . . . . ?
C27 N6 C49 C50 -10.3(2) . . . . ?
C48 N6 C49 C52 60.32(19) . . . . ?
C27 N6 C49 C52 -129.25(17) . . . . ?
C38 C29 C30 C31 -0.7(2) . . . . ?
C28 C29 C30 C31 176.49(18) . . . . ?
C28 C39 C41 N4 163(5) . . . . ?
C40 C39 C41 N4 -14(5) . . . . ?
C42 C43 C44 C48 176.53(16) . . . . ?
C27 C43 C44 C48 -2.49(18) . . . . ?
C42 C43 C44 C45 -6.6(3) . . . . ?
C27 C43 C44 C45 174.39(16) . . . . ?
O9 C48 C44 C43 177.88(16) . . . . ?
N6 C48 C44 C43 -1.69(18) . . . . ?
O9 C48 C44 C45 0.6(3) . . . . ?
N6 C48 C44 C45 -178.95(14) . . . . ?
C38 C37 C36 C35 -0.5(3) . . . . ?
C27 C37 C36 C35 -174.70(17) . . . . ?
C34 C35 C36 C37 1.3(3) . . . . ?
C29 C30 C31 C32 0.6(3) . . . . ?
C30 C31 C32 C33 -0.1(3) . . . . ?
C38 C33 C32 C31 -0.2(3) . . . . ?
C34 C33 C32 C31 -179.04(19) . . . . ?
C36 C35 C34 C33 -0.7(3) . . . . ?
C38 C33 C34 C35 -0.5(3) . . . . ?
C32 C33 C34 C35 178.28(19) . . . . ?
C47 O6 C45 O5 -1.0(3) . . . . ?
C47 O6 C45 C44 176.2(2) . . . . ?
C43 C44 C45 O5 -82.5(3) . . . . ?
C48 C44 C45 O5 94.1(2) . . . . ?
C43 C44 C45 O6 100.2(2) . . . . ?
C48 C44 C45 O6 -83.2(2) . . . . ?
C28 C39 C40 N3 -158(4) . . . . ?
C41 C39 C40 N3 20(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.040
