# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_xie4
#TrackingRef 'xie4new.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H17 N3'
_chemical_formula_weight         347.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   8.6890(12)
_cell_length_b                   11.6597(16)
_cell_length_c                   16.959(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1718.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9802
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12909
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3013
_reflns_number_gt                2770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0501P)^2^+0.0508P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3013
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_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
C1 C 0.6696(3) 0.08097(17) 0.59023(12) 0.0351(5) Uani 1 1 d . . .
H1 H 0.5863 0.1137 0.5641 0.042 Uiso 1 1 calc R . .
C2 C 0.7560(3) 0.00141(19) 0.54985(12) 0.0373(5) Uani 1 1 d . . .
H2 H 0.7307 -0.0207 0.4988 0.045 Uiso 1 1 calc R . .
C3 C 0.8814(2) -0.04408(17) 0.58836(12) 0.0348(5) Uani 1 1 d . . .
H3 H 0.9430 -0.0982 0.5634 0.042 Uiso 1 1 calc R . .
C4 C 0.9154(2) -0.00935(16) 0.66369(11) 0.0306(4) Uani 1 1 d . . .
H4 H 1.0010 -0.0383 0.6899 0.037 Uiso 1 1 calc R . .
C5 C 0.8188(2) 0.07035(15) 0.70026(11) 0.0251(4) Uani 1 1 d . . .
C6 C 0.7833(2) 0.19799(15) 0.81788(11) 0.0243(4) Uani 1 1 d . . .
C7 C 0.7283(2) 0.29482(16) 0.77890(12) 0.0300(5) Uani 1 1 d . . .
H7 H 0.7316 0.2996 0.7242 0.036 Uiso 1 1 calc R . .
C8 C 0.6693(2) 0.38284(16) 0.82311(13) 0.0368(5) Uani 1 1 d . . .
H8 H 0.6304 0.4479 0.7985 0.044 Uiso 1 1 calc R . .
C9 C 0.6676(3) 0.37462(18) 0.90430(13) 0.0377(5) Uani 1 1 d . . .
H9 H 0.6266 0.4328 0.9354 0.045 Uiso 1 1 calc R . .
C10 C 0.7284(2) 0.27779(17) 0.93739(12) 0.0356(5) Uani 1 1 d . . .
H10 H 0.7302 0.2728 0.9921 0.043 Uiso 1 1 calc R . .
C11 C 0.9365(2) 0.02374(15) 0.82595(11) 0.0239(4) Uani 1 1 d . . .
C12 C 0.8690(2) -0.08004(16) 0.84867(11) 0.0267(4) Uani 1 1 d . . .
C13 C 0.7142(2) -0.10936(17) 0.83138(11) 0.0315(5) Uani 1 1 d . . .
H13 H 0.6517 -0.0570 0.8052 0.038 Uiso 1 1 calc R . .
C14 C 0.6558(3) -0.21320(18) 0.85269(13) 0.0417(6) Uani 1 1 d . . .
H14 H 0.5540 -0.2309 0.8407 0.050 Uiso 1 1 calc R . .
C15 C 0.7474(3) -0.29404(18) 0.89255(13) 0.0444(6) Uani 1 1 d . . .
H15 H 0.7066 -0.3652 0.9057 0.053 Uiso 1 1 calc R . .
C16 C 0.8941(3) -0.26886(17) 0.91182(12) 0.0398(6) Uani 1 1 d . . .
H16 H 0.9529 -0.3228 0.9387 0.048 Uiso 1 1 calc R . .
C17 C 0.9607(3) -0.16114(16) 0.89177(11) 0.0307(5) Uani 1 1 d . . .
C18 C 1.1113(2) -0.13321(17) 0.91110(11) 0.0329(5) Uani 1 1 d . . .
H18 H 1.1697 -0.1857 0.9395 0.039 Uiso 1 1 calc R . .
C19 C 1.1776(2) -0.02958(18) 0.88939(11) 0.0320(5) Uani 1 1 d . . .
C20 C 1.3327(3) -0.0023(2) 0.90673(13) 0.0413(6) Uani 1 1 d . . .
H20 H 1.3920 -0.0543 0.9352 0.050 Uiso 1 1 calc R . .
C21 C 1.3967(3) 0.0972(2) 0.88301(13) 0.0483(6) Uani 1 1 d . . .
H21 H 1.4986 0.1134 0.8955 0.058 Uiso 1 1 calc R . .
C22 C 1.3095(3) 0.1769(2) 0.83938(13) 0.0444(6) Uani 1 1 d . . .
H22 H 1.3547 0.2452 0.8232 0.053 Uiso 1 1 calc R . .
C23 C 1.1602(2) 0.15522(18) 0.82062(12) 0.0343(5) Uani 1 1 d . . .
H23 H 1.1043 0.2089 0.7919 0.041 Uiso 1 1 calc R . .
C24 C 1.0887(2) 0.05102(17) 0.84453(11) 0.0277(4) Uani 1 1 d . . .
N1 N 0.69665(19) 0.11476(14) 0.66439(9) 0.0308(4) Uani 1 1 d . . .
N2 N 0.84717(18) 0.10218(12) 0.77903(9) 0.0252(4) Uani 1 1 d . . .
N3 N 0.78547(19) 0.18987(13) 0.89620(9) 0.0301(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0399(12) 0.0363(11) 0.0290(11) 0.0014(9) -0.0100(10) 0.0008(9)
C2 0.0480(13) 0.0382(11) 0.0258(11) -0.0018(9) -0.0050(10) -0.0045(10)
C3 0.0434(13) 0.0326(11) 0.0282(11) -0.0041(9) 0.0066(10) 0.0017(10)
C4 0.0316(11) 0.0313(10) 0.0288(10) 0.0005(9) -0.0003(8) 0.0022(9)
C5 0.0267(10) 0.0244(9) 0.0241(9) 0.0026(8) 0.0000(8) -0.0065(8)
C6 0.0222(10) 0.0244(9) 0.0262(10) -0.0002(8) -0.0005(8) -0.0055(8)
C7 0.0376(12) 0.0247(9) 0.0276(11) 0.0025(8) -0.0025(9) -0.0036(9)
C8 0.0427(13) 0.0223(10) 0.0454(13) 0.0003(9) -0.0058(10) 0.0022(9)
C9 0.0454(13) 0.0280(10) 0.0397(13) -0.0093(9) 0.0060(10) -0.0008(10)
C10 0.0472(13) 0.0315(11) 0.0282(11) -0.0060(9) 0.0026(10) -0.0037(9)
C11 0.0285(10) 0.0249(9) 0.0184(9) -0.0020(8) 0.0000(8) 0.0042(8)
C12 0.0343(11) 0.0268(9) 0.0190(9) -0.0031(8) 0.0027(8) 0.0035(8)
C13 0.0345(11) 0.0330(10) 0.0270(10) -0.0010(9) 0.0031(9) -0.0003(9)
C14 0.0471(13) 0.0411(12) 0.0369(12) -0.0062(10) 0.0085(11) -0.0135(11)
C15 0.0707(17) 0.0264(11) 0.0361(13) 0.0018(9) 0.0144(12) -0.0093(11)
C16 0.0652(16) 0.0268(11) 0.0274(11) 0.0018(9) 0.0080(11) 0.0063(11)
C17 0.0464(13) 0.0265(10) 0.0192(10) -0.0019(8) 0.0069(9) 0.0072(9)
C18 0.0419(12) 0.0364(11) 0.0204(10) 0.0012(9) -0.0008(9) 0.0157(10)
C19 0.0318(11) 0.0436(12) 0.0206(9) -0.0033(9) 0.0002(8) 0.0080(9)
C20 0.0312(12) 0.0624(15) 0.0304(11) -0.0056(11) -0.0047(10) 0.0128(11)
C21 0.0236(11) 0.0851(19) 0.0362(13) -0.0084(13) -0.0018(9) -0.0069(12)
C22 0.0397(12) 0.0584(15) 0.0351(13) -0.0050(11) 0.0038(10) -0.0140(12)
C23 0.0359(12) 0.0392(11) 0.0278(11) -0.0010(9) -0.0013(9) -0.0046(9)
C24 0.0291(10) 0.0339(10) 0.0202(9) -0.0030(8) 0.0020(8) 0.0011(9)
N1 0.0331(9) 0.0322(8) 0.0272(9) -0.0002(7) -0.0049(7) 0.0021(8)
N2 0.0303(9) 0.0239(8) 0.0213(8) 0.0002(6) -0.0021(7) 0.0007(7)
N3 0.0390(10) 0.0271(8) 0.0241(9) -0.0016(7) -0.0019(7) -0.0028(7)

_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 1.339(3) . ?
C1 C2 1.376(3) . ?
C2 C3 1.377(3) . ?
C3 C4 1.372(3) . ?
C4 C5 1.397(3) . ?
C5 N1 1.329(2) . ?
C5 N2 1.408(2) . ?
C6 N3 1.332(2) . ?
C6 C7 1.393(3) . ?
C6 N2 1.411(2) . ?
C7 C8 1.371(3) . ?
C8 C9 1.380(3) . ?
C9 C10 1.367(3) . ?
C10 N3 1.336(2) . ?
C11 C24 1.396(3) . ?
C11 C12 1.399(3) . ?
C11 N2 1.439(2) . ?
C12 C13 1.419(3) . ?
C12 C17 1.436(3) . ?
C13 C14 1.362(3) . ?
C14 C15 1.407(3) . ?
C15 C16 1.348(3) . ?
C16 C17 1.424(3) . ?
C17 C18 1.388(3) . ?
C18 C19 1.388(3) . ?
C19 C20 1.416(3) . ?
C19 C24 1.435(3) . ?
C20 C21 1.348(3) . ?
C21 C22 1.408(3) . ?
C22 C23 1.360(3) . ?
C23 C24 1.424(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 124.77(19) . . ?
C1 C2 C3 117.09(19) . . ?
C4 C3 C2 119.88(19) . . ?
C3 C4 C5 118.71(19) . . ?
N1 C5 C4 122.40(17) . . ?
N1 C5 N2 118.13(17) . . ?
C4 C5 N2 119.43(17) . . ?
N3 C6 C7 122.42(18) . . ?
N3 C6 N2 113.82(16) . . ?
C7 C6 N2 123.71(17) . . ?
C8 C7 C6 118.40(18) . . ?
C7 C8 C9 119.84(19) . . ?
C10 C9 C8 117.57(19) . . ?
N3 C10 C9 124.22(19) . . ?
C24 C11 C12 122.12(17) . . ?
C24 C11 N2 119.38(17) . . ?
C12 C11 N2 118.44(17) . . ?
C11 C12 C13 123.28(17) . . ?
C11 C12 C17 118.53(18) . . ?
C13 C12 C17 118.19(18) . . ?
C14 C13 C12 120.8(2) . . ?
C13 C14 C15 120.8(2) . . ?
C16 C15 C14 120.4(2) . . ?
C15 C16 C17 121.2(2) . . ?
C18 C17 C16 122.3(2) . . ?
C18 C17 C12 119.25(18) . . ?
C16 C17 C12 118.5(2) . . ?
C17 C18 C19 122.20(19) . . ?
C18 C19 C20 122.4(2) . . ?
C18 C19 C24 119.16(19) . . ?
C20 C19 C24 118.4(2) . . ?
C21 C20 C19 121.6(2) . . ?
C20 C21 C22 120.2(2) . . ?
C23 C22 C21 120.9(2) . . ?
C22 C23 C24 120.5(2) . . ?
C11 C24 C23 122.92(18) . . ?
C11 C24 C19 118.72(18) . . ?
C23 C24 C19 118.36(18) . . ?
C5 N1 C1 117.11(17) . . ?
C5 N2 C6 125.65(15) . . ?
C5 N2 C11 116.83(14) . . ?
C6 N2 C11 117.20(14) . . ?
C6 N3 C10 117.50(18) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.037


_database_code_depnum_ccdc_archive 'CCDC 895653'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_111220f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H46 N4 O'
_chemical_formula_weight         682.88

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           ?
_symmetry_space_group_name_H-M   P2(1)/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                   24.460(2)
_cell_length_b                   10.4080(10)
_cell_length_c                   15.1901(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2550(10)
_cell_angle_gamma                90.00
_cell_volume                     3856.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9723
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18184
_diffrn_reflns_av_R_equivalents  0.1171
_diffrn_reflns_av_sigmaI/netI    0.2000
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         24.25
_reflns_number_total             6191
_reflns_number_gt                2273
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1161P)^2^+4.1159P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6191
_refine_ls_number_parameters     508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2338
_refine_ls_R_factor_gt           0.0930
_refine_ls_wR_factor_ref         0.3489
_refine_ls_wR_factor_gt          0.2253
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
N1 N 0.3702(3) 0.9024(7) 0.4044(5) 0.076(2) Uani 1 1 d . . .
H1 H 0.3352 0.9103 0.3964 0.091 Uiso 1 1 calc R . .
N2 N 0.3647(3) 1.0510(8) 0.2961(5) 0.091(2) Uani 1 1 d . . .
N3 N 0.4407(2) 0.7850(6) 0.4779(4) 0.0581(16) Uani 1 1 d . . .
N4 N 0.7917(2) 0.5676(5) 0.5969(4) 0.0482(15) Uani 1 1 d . . .
O1 O 0.2579(3) 0.9572(9) 0.2425(6) 0.133(3) Uani 1 1 d . . .
H1A H 0.2862 0.9971 0.2559 0.200 Uiso 1 1 calc R . .
C1 C 0.3989(4) 0.9837(8) 0.3539(6) 0.072(2) Uani 1 1 d . . .
C2 C 0.4545(4) 0.9974(9) 0.3577(6) 0.084(3) Uani 1 1 d . . .
H2 H 0.4768 0.9480 0.3966 0.101 Uiso 1 1 calc R . .
C3 C 0.4771(5) 1.0855(10) 0.3031(8) 0.100(3) Uani 1 1 d . . .
H3 H 0.5149 1.0971 0.3049 0.120 Uiso 1 1 calc R . .
C4 C 0.4429(6) 1.1553(10) 0.2462(7) 0.103(3) Uani 1 1 d . . .
H4 H 0.4569 1.2159 0.2090 0.124 Uiso 1 1 calc R . .
C5 C 0.3891(6) 1.1349(11) 0.2451(7) 0.108(3) Uani 1 1 d . . .
H5 H 0.3666 1.1831 0.2056 0.129 Uiso 1 1 calc R . .
C6 C 0.3873(3) 0.8101(7) 0.4658(5) 0.057(2) Uani 1 1 d . . .
C7 C 0.3475(3) 0.7449(8) 0.5094(5) 0.065(2) Uani 1 1 d . . .
H7 H 0.3105 0.7640 0.4980 0.078 Uiso 1 1 calc R . .
C8 C 0.3639(3) 0.6527(7) 0.5689(5) 0.064(2) Uani 1 1 d . . .
H8 H 0.3383 0.6092 0.6000 0.076 Uiso 1 1 calc R . .
C9 C 0.4189(3) 0.6242(7) 0.5827(5) 0.060(2) Uani 1 1 d . . .
H9 H 0.4310 0.5607 0.6226 0.072 Uiso 1 1 calc R . .
C10 C 0.4554(3) 0.6919(7) 0.5361(5) 0.0541(19) Uani 1 1 d . . .
C11 C 0.5132(3) 0.6673(7) 0.5474(5) 0.057(2) Uani 1 1 d . . .
C12 C 0.5616(3) 0.6498(7) 0.5580(5) 0.055(2) Uani 1 1 d . . .
C13 C 0.6199(3) 0.6323(6) 0.5697(5) 0.0481(18) Uani 1 1 d . . .
C14 C 0.6414(3) 0.5346(6) 0.6273(4) 0.0442(17) Uani 1 1 d . . .
C15 C 0.6071(3) 0.4555(7) 0.6756(5) 0.056(2) Uani 1 1 d . . .
H15 H 0.5693 0.4658 0.6683 0.067 Uiso 1 1 calc R . .
C16 C 0.6287(3) 0.3648(7) 0.7324(5) 0.061(2) Uani 1 1 d . . .
H16 H 0.6057 0.3150 0.7645 0.073 Uiso 1 1 calc R . .
C17 C 0.6857(3) 0.3458(7) 0.7428(5) 0.062(2) Uani 1 1 d . . .
H17 H 0.7002 0.2827 0.7812 0.075 Uiso 1 1 calc R . .
C18 C 0.7198(3) 0.4188(6) 0.6973(4) 0.0498(18) Uani 1 1 d . . .
H18 H 0.7574 0.4054 0.7051 0.060 Uiso 1 1 calc R . .
C19 C 0.6990(3) 0.5155(6) 0.6380(4) 0.0421(17) Uani 1 1 d . . .
C20 C 0.7331(3) 0.5892(6) 0.5887(4) 0.0461(17) Uani 1 1 d . . .
C21 C 0.7120(3) 0.6886(6) 0.5320(5) 0.0478(18) Uani 1 1 d . . .
C22 C 0.7459(3) 0.7624(7) 0.4796(5) 0.062(2) Uani 1 1 d . . .
H22 H 0.7834 0.7472 0.4831 0.075 Uiso 1 1 calc R . .
C23 C 0.7244(4) 0.8548(8) 0.4246(6) 0.076(2) Uani 1 1 d . . .
H23 H 0.7470 0.9013 0.3896 0.091 Uiso 1 1 calc R . .
C24 C 0.6678(4) 0.8804(8) 0.4207(6) 0.074(2) Uani 1 1 d . . .
H24 H 0.6537 0.9472 0.3853 0.089 Uiso 1 1 calc R . .
C25 C 0.6337(3) 0.8114(7) 0.4664(5) 0.061(2) Uani 1 1 d . . .
H25 H 0.5964 0.8291 0.4614 0.073 Uiso 1 1 calc R . .
C26 C 0.6546(3) 0.7092(6) 0.5237(5) 0.0470(17) Uani 1 1 d . . .
C27 C 0.8123(3) 0.4535(6) 0.5602(4) 0.0425(16) Uani 1 1 d . . .
C28 C 0.7912(3) 0.4094(7) 0.4791(5) 0.0513(19) Uani 1 1 d . . .
H28 H 0.7628 0.4538 0.4482 0.062 Uiso 1 1 calc R . .
C29 C 0.8121(3) 0.2990(7) 0.4436(5) 0.0527(19) Uani 1 1 d . . .
H29 H 0.7966 0.2702 0.3894 0.063 Uiso 1 1 calc R . .
C30 C 0.8552(3) 0.2289(6) 0.4847(4) 0.0452(17) Uani 1 1 d . . .
C31 C 0.8752(3) 0.2753(6) 0.5669(4) 0.0508(18) Uani 1 1 d . . .
H31 H 0.9036 0.2311 0.5977 0.061 Uiso 1 1 calc R . .
C32 C 0.8546(3) 0.3843(7) 0.6046(5) 0.0520(19) Uani 1 1 d . . .
H32 H 0.8691 0.4115 0.6598 0.062 Uiso 1 1 calc R . .
C33 C 0.8810(3) 0.1112(7) 0.4453(5) 0.0557(19) Uani 1 1 d . . .
C34 C 0.9429(3) 0.1296(9) 0.4452(7) 0.105(3) Uani 1 1 d . . .
H34A H 0.9505 0.1998 0.4069 0.157 Uiso 1 1 calc R . .
H34B H 0.9592 0.0525 0.4245 0.157 Uiso 1 1 calc R . .
H34C H 0.9578 0.1482 0.5040 0.157 Uiso 1 1 calc R . .
C35 C 0.8578(4) 0.0848(9) 0.3520(6) 0.100(3) Uani 1 1 d . . .
H35A H 0.8192 0.0686 0.3519 0.150 Uiso 1 1 calc R . .
H35B H 0.8757 0.0111 0.3293 0.150 Uiso 1 1 calc R . .
H35C H 0.8639 0.1580 0.3156 0.150 Uiso 1 1 calc R . .
C36 C 0.8699(5) -0.0061(8) 0.5018(6) 0.104(3) Uani 1 1 d . . .
H36A H 0.8876 0.0051 0.5599 0.156 Uiso 1 1 calc R . .
H36B H 0.8841 -0.0816 0.4753 0.156 Uiso 1 1 calc R . .
H36C H 0.8312 -0.0154 0.5058 0.156 Uiso 1 1 calc R . .
C37 C 0.8260(2) 0.6512(6) 0.6494(4) 0.0435(17) Uani 1 1 d . . .
C38 C 0.8804(3) 0.6684(6) 0.6316(5) 0.0522(19) Uani 1 1 d . . .
H38 H 0.8939 0.6270 0.5835 0.063 Uiso 1 1 calc R . .
C39 C 0.9146(3) 0.7465(7) 0.6847(5) 0.0543(19) Uani 1 1 d . . .
H39 H 0.9511 0.7542 0.6722 0.065 Uiso 1 1 calc R . .
C40 C 0.8965(3) 0.8133(6) 0.7553(4) 0.0463(17) Uani 1 1 d . A .
C41 C 0.8418(3) 0.7981(7) 0.7712(5) 0.0521(19) Uani 1 1 d . . .
H41 H 0.8278 0.8422 0.8178 0.063 Uiso 1 1 calc R . .
C42 C 0.8079(3) 0.7194(7) 0.7197(5) 0.0519(19) Uani 1 1 d . . .
H42 H 0.7714 0.7116 0.7324 0.062 Uiso 1 1 calc R . .
C43 C 0.9359(3) 0.8970(7) 0.8139(5) 0.0544(19) Uani 1 1 d . . .
C44 C 0.9178(14) 1.037(2) 0.804(2) 0.100(12) Uani 0.48(3) 1 d P A 1
H44A H 0.9126 1.0727 0.8608 0.149 Uiso 0.48(3) 1 calc PR A 1
H44B H 0.8839 1.0414 0.7676 0.149 Uiso 0.48(3) 1 calc PR A 1
H44C H 0.9454 1.0853 0.7764 0.149 Uiso 0.48(3) 1 calc PR A 1
C45 C 0.9947(7) 0.896(3) 0.790(2) 0.089(12) Uani 0.48(3) 1 d P A 1
H45A H 1.0155 0.9575 0.8259 0.133 Uiso 0.48(3) 1 calc PR A 1
H45B H 0.9961 0.9185 0.7289 0.133 Uiso 0.48(3) 1 calc PR A 1
H45C H 1.0100 0.8120 0.8001 0.133 Uiso 0.48(3) 1 calc PR A 1
C46 C 0.9307(14) 0.872(4) 0.9068(17) 0.104(12) Uani 0.48(3) 1 d P A 1
H46A H 0.9469 0.7901 0.9222 0.157 Uiso 0.48(3) 1 calc PR A 1
H46B H 0.8926 0.8709 0.9181 0.157 Uiso 0.48(3) 1 calc PR A 1
H46C H 0.9492 0.9381 0.9415 0.157 Uiso 0.48(3) 1 calc PR A 1
C44' C 0.9514(11) 1.012(2) 0.7581(17) 0.093(10) Uani 0.52(3) 1 d P A 2
H44D H 0.9669 1.0782 0.7960 0.139 Uiso 0.52(3) 1 calc PR A 2
H44E H 0.9192 1.0438 0.7253 0.139 Uiso 0.52(3) 1 calc PR A 2
H44F H 0.9777 0.9852 0.7180 0.139 Uiso 0.52(3) 1 calc PR A 2
C45' C 0.9825(11) 0.818(3) 0.850(2) 0.107(14) Uani 0.52(3) 1 d P A 2
H45D H 1.0121 0.8732 0.8710 0.161 Uiso 0.52(3) 1 calc PR A 2
H45E H 0.9944 0.7627 0.8047 0.161 Uiso 0.52(3) 1 calc PR A 2
H45F H 0.9712 0.7669 0.8981 0.161 Uiso 0.52(3) 1 calc PR A 2
C46' C 0.9079(11) 0.959(3) 0.8905(18) 0.096(10) Uani 0.52(3) 1 d P A 2
H46D H 0.8939 0.8927 0.9267 0.144 Uiso 0.52(3) 1 calc PR A 2
H46E H 0.8783 1.0123 0.8674 0.144 Uiso 0.52(3) 1 calc PR A 2
H46F H 0.9341 1.0099 0.9253 0.144 Uiso 0.52(3) 1 calc PR A 2
C47 C 0.2289(5) 0.9364(12) 0.3199(9) 0.130(4) Uani 1 1 d . . .
H47A H 0.2454 0.8661 0.3532 0.195 Uiso 1 1 calc R . .
H47B H 0.1913 0.9164 0.3028 0.195 Uiso 1 1 calc R . .
H47C H 0.2307 1.0127 0.3555 0.195 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.065(4) 0.077(5) 0.085(5) 0.010(4) 0.003(4) 0.011(4)
N2 0.112(6) 0.083(5) 0.079(6) 0.014(5) 0.009(5) 0.018(5)
N3 0.041(4) 0.062(4) 0.070(4) -0.006(3) -0.001(3) 0.009(3)
N4 0.033(3) 0.053(4) 0.058(4) -0.013(3) 0.000(3) 0.002(3)
O1 0.124(7) 0.145(8) 0.127(7) -0.010(6) -0.022(5) 0.026(5)
C1 0.081(7) 0.064(6) 0.071(6) -0.004(5) 0.004(5) 0.013(5)
C2 0.093(8) 0.076(6) 0.085(7) 0.002(5) 0.019(6) -0.004(6)
C3 0.117(9) 0.086(7) 0.100(8) -0.010(7) 0.026(7) -0.017(7)
C4 0.146(11) 0.083(7) 0.082(8) 0.000(6) 0.020(8) -0.018(8)
C5 0.136(11) 0.096(9) 0.091(9) 0.011(7) 0.012(8) 0.005(8)
C6 0.050(5) 0.057(5) 0.064(5) -0.003(4) -0.001(4) 0.008(4)
C7 0.042(4) 0.075(6) 0.075(6) -0.007(5) -0.005(4) 0.006(4)
C8 0.051(5) 0.067(5) 0.073(6) -0.006(5) 0.005(4) 0.002(4)
C9 0.051(5) 0.060(5) 0.066(5) 0.003(4) -0.006(4) 0.005(4)
C10 0.039(4) 0.057(5) 0.065(5) -0.007(4) -0.005(4) 0.009(4)
C11 0.046(5) 0.057(5) 0.066(5) -0.008(4) -0.005(4) 0.005(4)
C12 0.046(5) 0.055(5) 0.062(5) -0.009(4) 0.000(4) 0.007(4)
C13 0.042(4) 0.049(4) 0.053(5) -0.008(4) -0.002(3) 0.007(3)
C14 0.039(4) 0.043(4) 0.051(5) -0.008(3) 0.003(3) -0.001(3)
C15 0.044(4) 0.060(5) 0.062(5) 0.001(4) 0.006(4) 0.005(4)
C16 0.054(5) 0.060(5) 0.069(5) 0.010(4) 0.013(4) -0.001(4)
C17 0.062(5) 0.060(5) 0.065(5) 0.007(4) 0.008(4) 0.011(4)
C18 0.046(4) 0.051(4) 0.053(5) -0.002(4) 0.004(4) 0.010(4)
C19 0.037(4) 0.044(4) 0.045(4) -0.004(3) -0.001(3) 0.004(3)
C20 0.036(4) 0.051(4) 0.051(4) -0.007(4) 0.002(3) 0.004(3)
C21 0.043(4) 0.046(4) 0.055(5) -0.002(4) 0.004(3) -0.001(3)
C22 0.054(5) 0.061(5) 0.072(6) 0.005(4) 0.002(4) -0.005(4)
C23 0.075(6) 0.075(6) 0.078(6) 0.011(5) 0.003(5) -0.016(5)
C24 0.085(7) 0.058(5) 0.077(6) 0.010(5) -0.007(5) 0.000(5)
C25 0.062(5) 0.055(5) 0.064(5) 0.006(4) -0.004(4) 0.006(4)
C26 0.044(4) 0.044(4) 0.052(5) -0.002(4) -0.001(3) -0.002(3)
C27 0.037(4) 0.045(4) 0.046(4) -0.004(3) 0.004(3) -0.002(3)
C28 0.036(4) 0.059(5) 0.057(5) -0.004(4) -0.004(3) -0.001(3)
C29 0.047(4) 0.058(5) 0.052(5) -0.012(4) 0.000(4) -0.007(4)
C30 0.047(4) 0.047(4) 0.042(4) -0.007(3) 0.004(3) -0.007(3)
C31 0.049(4) 0.050(4) 0.053(5) -0.002(4) -0.001(4) 0.005(3)
C32 0.049(4) 0.055(4) 0.051(5) -0.007(4) -0.008(4) 0.001(4)
C33 0.065(5) 0.046(4) 0.056(5) -0.007(4) 0.006(4) 0.000(4)
C34 0.075(7) 0.099(7) 0.141(9) -0.038(7) 0.019(6) 0.022(5)
C35 0.137(9) 0.083(6) 0.078(7) -0.021(5) -0.011(6) 0.028(6)
C36 0.163(10) 0.053(5) 0.099(8) -0.001(5) 0.019(7) 0.007(6)
C37 0.031(4) 0.048(4) 0.052(5) -0.007(3) 0.004(3) -0.003(3)
C38 0.042(4) 0.060(5) 0.056(5) -0.013(4) 0.009(4) -0.001(4)
C39 0.037(4) 0.065(5) 0.062(5) -0.009(4) 0.009(4) -0.007(4)
C40 0.040(4) 0.049(4) 0.050(5) -0.009(4) 0.005(3) 0.001(3)
C41 0.043(4) 0.058(5) 0.056(5) -0.013(4) 0.010(4) 0.000(4)
C42 0.037(4) 0.060(5) 0.059(5) -0.011(4) 0.008(4) -0.001(4)
C43 0.049(5) 0.059(5) 0.054(5) -0.013(4) 0.001(4) -0.004(4)
C44 0.10(2) 0.085(16) 0.11(3) -0.040(16) -0.010(19) -0.010(15)
C45 0.051(12) 0.12(3) 0.10(2) -0.039(19) -0.004(12) -0.034(13)
C46 0.10(3) 0.13(3) 0.078(18) -0.023(19) -0.007(16) -0.04(2)
C44' 0.09(2) 0.090(17) 0.099(18) -0.012(14) 0.006(13) -0.046(16)
C45' 0.092(19) 0.097(17) 0.12(3) -0.036(16) -0.05(2) 0.021(14)
C46' 0.092(17) 0.11(2) 0.087(19) -0.046(19) 0.012(14) -0.004(14)
C47 0.116(10) 0.141(10) 0.137(11) 0.028(9) 0.031(8) 0.025(8)

_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
N1 C1 1.371(11) . ?
N1 C6 1.383(9) . ?
N1 H1 0.8600 . ?
N2 C5 1.337(12) . ?
N2 C1 1.361(10) . ?
N3 C6 1.331(8) . ?
N3 C10 1.343(9) . ?
N4 C37 1.413(8) . ?
N4 C27 1.421(8) . ?
N4 C20 1.447(8) . ?
O1 C47 1.432(12) . ?
O1 H1A 0.8200 . ?
C1 C2 1.362(12) . ?
C2 C3 1.381(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.366(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.332(13) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.395(10) . ?
C7 C8 1.358(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.375(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.434(10) . ?
C11 C12 1.196(9) . ?
C12 C13 1.434(9) . ?
C13 C26 1.393(9) . ?
C13 C14 1.417(9) . ?
C14 C15 1.418(9) . ?
C14 C19 1.419(8) . ?
C15 C16 1.359(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.405(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.354(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.419(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.393(9) . ?
C20 C21 1.419(9) . ?
C21 C26 1.415(9) . ?
C21 C22 1.417(9) . ?
C22 C23 1.354(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.408(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.333(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.443(9) . ?
C25 H25 0.9300 . ?
C27 C28 1.379(9) . ?
C27 C32 1.393(9) . ?
C28 C29 1.383(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.391(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.393(8) . ?
C30 C33 1.521(9) . ?
C31 C32 1.382(9) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C35 1.512(10) . ?
C33 C34 1.526(10) . ?
C33 C36 1.527(11) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C42 1.381(9) . ?
C37 C38 1.389(8) . ?
C38 C39 1.382(9) . ?
C38 H38 0.9300 . ?
C39 C40 1.379(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.386(9) . ?
C40 C43 1.534(9) . ?
C41 C42 1.370(9) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C46 1.45(3) . ?
C43 C45' 1.478(19) . ?
C43 C45 1.51(2) . ?
C43 C44' 1.53(2) . ?
C43 C44 1.53(2) . ?
C43 C46' 1.53(2) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C44' H44D 0.9600 . ?
C44' H44E 0.9600 . ?
C44' H44F 0.9600 . ?
C45' H45D 0.9600 . ?
C45' H45E 0.9600 . ?
C45' H45F 0.9600 . ?
C46' H46D 0.9600 . ?
C46' H46E 0.9600 . ?
C46' H46F 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 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
C1 N1 C6 131.6(7) . . ?
C1 N1 H1 114.2 . . ?
C6 N1 H1 114.2 . . ?
C5 N2 C1 115.5(10) . . ?
C6 N3 C10 116.4(6) . . ?
C37 N4 C27 121.5(5) . . ?
C37 N4 C20 119.7(5) . . ?
C27 N4 C20 118.3(5) . . ?
C47 O1 H1A 109.5 . . ?
N2 C1 C2 122.5(10) . . ?
N2 C1 N1 111.2(9) . . ?
C2 C1 N1 126.3(9) . . ?
C1 C2 C3 119.2(10) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 118.6(11) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 118.9(11) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 N2 125.4(12) . . ?
C4 C5 H5 117.3 . . ?
N2 C5 H5 117.3 . . ?
N3 C6 N1 118.3(7) . . ?
N3 C6 C7 123.5(7) . . ?
N1 C6 C7 118.1(7) . . ?
C8 C7 C6 118.5(7) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
C7 C8 C9 119.3(8) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 118.4(7) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
N3 C10 C9 123.7(6) . . ?
N3 C10 C11 115.0(7) . . ?
C9 C10 C11 121.3(7) . . ?
C12 C11 C10 178.3(8) . . ?
C11 C12 C13 178.5(8) . . ?
C26 C13 C14 120.6(6) . . ?
C26 C13 C12 120.2(6) . . ?
C14 C13 C12 119.2(7) . . ?
C13 C14 C15 121.9(6) . . ?
C13 C14 C19 119.5(6) . . ?
C15 C14 C19 118.6(6) . . ?
C16 C15 C14 120.9(7) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.4(7) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 120.4(7) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 121.1(6) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C20 C19 C14 119.3(6) . . ?
C20 C19 C18 122.0(6) . . ?
C14 C19 C18 118.6(6) . . ?
C19 C20 C21 121.5(6) . . ?
C19 C20 N4 119.8(6) . . ?
C21 C20 N4 118.6(6) . . ?
C26 C21 C22 119.1(6) . . ?
C26 C21 C20 118.5(6) . . ?
C22 C21 C20 122.3(6) . . ?
C23 C22 C21 121.0(7) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 119.7(8) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C25 C24 C23 121.8(8) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C26 120.3(7) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C13 C26 C21 120.5(6) . . ?
C13 C26 C25 121.6(6) . . ?
C21 C26 C25 118.0(7) . . ?
C28 C27 C32 118.4(6) . . ?
C28 C27 N4 120.6(6) . . ?
C32 C27 N4 121.0(6) . . ?
C27 C28 C29 120.0(6) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 123.4(6) . . ?
C28 C29 H29 118.3 . . ?
C30 C29 H29 118.3 . . ?
C29 C30 C31 115.1(6) . . ?
C29 C30 C33 124.6(6) . . ?
C31 C30 C33 120.2(6) . . ?
C32 C31 C30 122.8(6) . . ?
C32 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
C31 C32 C27 120.3(6) . . ?
C31 C32 H32 119.9 . . ?
C27 C32 H32 119.9 . . ?
C35 C33 C30 112.2(6) . . ?
C35 C33 C34 108.9(7) . . ?
C30 C33 C34 109.9(6) . . ?
C35 C33 C36 108.2(7) . . ?
C30 C33 C36 109.1(6) . . ?
C34 C33 C36 108.6(7) . . ?
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 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C42 C37 C38 116.8(6) . . ?
C42 C37 N4 122.8(6) . . ?
C38 C37 N4 120.4(6) . . ?
C39 C38 C37 120.7(7) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 C38 122.3(6) . . ?
C40 C39 H39 118.9 . . ?
C38 C39 H39 118.9 . . ?
C39 C40 C41 116.6(6) . . ?
C39 C40 C43 120.9(6) . . ?
C41 C40 C43 122.5(6) . . ?
C42 C41 C40 121.4(6) . . ?
C42 C41 H41 119.3 . . ?
C40 C41 H41 119.3 . . ?
C41 C42 C37 122.2(6) . . ?
C41 C42 H42 118.9 . . ?
C37 C42 H42 118.9 . . ?
C46 C43 C45' 70.0(15) . . ?
C46 C43 C45 112.8(15) . . ?
C45' C43 C45 50.5(11) . . ?
C46 C43 C44' 136.4(14) . . ?
C45' C43 C44' 115.2(15) . . ?
C45 C43 C44' 65.9(13) . . ?
C46 C43 C44 103.0(17) . . ?
C45' C43 C44 141.1(13) . . ?
C45 C43 C44 104.8(15) . . ?
C44' C43 C44 44.0(11) . . ?
C46 C43 C46' 42.4(12) . . ?
C45' C43 C46' 109.0(15) . . ?
C45 C43 C46' 132.2(13) . . ?
C44' C43 C46' 103.7(14) . . ?
C44 C43 C46' 62.3(14) . . ?
C46 C43 C40 111.4(11) . . ?
C45' C43 C40 109.5(10) . . ?
C45 C43 C40 115.2(9) . . ?
C44' C43 C40 107.0(9) . . ?
C44 C43 C40 108.6(10) . . ?
C46' C43 C40 112.4(11) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
C43 C44' H44D 109.5 . . ?
C43 C44' H44E 109.5 . . ?
H44D C44' H44E 109.5 . . ?
C43 C44' H44F 109.5 . . ?
H44D C44' H44F 109.5 . . ?
H44E C44' H44F 109.5 . . ?
C43 C45' H45D 109.5 . . ?
C43 C45' H45E 109.5 . . ?
H45D C45' H45E 109.5 . . ?
C43 C45' H45F 109.5 . . ?
H45D C45' H45F 109.5 . . ?
H45E C45' H45F 109.5 . . ?
C43 C46' H46D 109.5 . . ?
C43 C46' H46E 109.5 . . ?
H46D C46' H46E 109.5 . . ?
C43 C46' H46F 109.5 . . ?
H46D C46' H46F 109.5 . . ?
H46E C46' H46F 109.5 . . ?
O1 C47 H47A 109.5 . . ?
O1 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
O1 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?

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 N2 C1 C2 -2.2(13) . . . . ?
C5 N2 C1 N1 178.7(8) . . . . ?
C6 N1 C1 N2 174.4(7) . . . . ?
C6 N1 C1 C2 -4.7(14) . . . . ?
N2 C1 C2 C3 2.1(14) . . . . ?
N1 C1 C2 C3 -178.9(8) . . . . ?
C1 C2 C3 C4 -0.6(14) . . . . ?
C2 C3 C4 C5 -0.6(15) . . . . ?
C3 C4 C5 N2 0.5(18) . . . . ?
C1 N2 C5 C4 0.9(15) . . . . ?
C10 N3 C6 N1 -178.0(6) . . . . ?
C10 N3 C6 C7 -0.6(10) . . . . ?
C1 N1 C6 N3 -4.7(12) . . . . ?
C1 N1 C6 C7 177.8(8) . . . . ?
N3 C6 C7 C8 1.6(11) . . . . ?
N1 C6 C7 C8 179.0(7) . . . . ?
C6 C7 C8 C9 -1.7(11) . . . . ?
C7 C8 C9 C10 0.8(11) . . . . ?
C6 N3 C10 C9 -0.4(10) . . . . ?
C6 N3 C10 C11 180.0(6) . . . . ?
C8 C9 C10 N3 0.3(11) . . . . ?
C8 C9 C10 C11 179.9(7) . . . . ?
N3 C10 C11 C12 69(30) . . . . ?
C9 C10 C11 C12 -111(30) . . . . ?
C10 C11 C12 C13 -46(52) . . . . ?
C11 C12 C13 C26 -21(31) . . . . ?
C11 C12 C13 C14 160(30) . . . . ?
C26 C13 C14 C15 179.5(6) . . . . ?
C12 C13 C14 C15 -1.7(9) . . . . ?
C26 C13 C14 C19 0.1(9) . . . . ?
C12 C13 C14 C19 179.0(6) . . . . ?
C13 C14 C15 C16 -178.1(7) . . . . ?
C19 C14 C15 C16 1.3(10) . . . . ?
C14 C15 C16 C17 -1.4(11) . . . . ?
C15 C16 C17 C18 0.9(11) . . . . ?
C16 C17 C18 C19 -0.3(11) . . . . ?
C13 C14 C19 C20 -2.9(9) . . . . ?
C15 C14 C19 C20 177.7(6) . . . . ?
C13 C14 C19 C18 178.8(6) . . . . ?
C15 C14 C19 C18 -0.6(9) . . . . ?
C17 C18 C19 C20 -178.1(6) . . . . ?
C17 C18 C19 C14 0.1(9) . . . . ?
C14 C19 C20 C21 4.0(9) . . . . ?
C18 C19 C20 C21 -177.7(6) . . . . ?
C14 C19 C20 N4 -177.9(6) . . . . ?
C18 C19 C20 N4 0.3(9) . . . . ?
C37 N4 C20 C19 -100.9(7) . . . . ?
C27 N4 C20 C19 71.6(8) . . . . ?
C37 N4 C20 C21 77.2(8) . . . . ?
C27 N4 C20 C21 -110.3(7) . . . . ?
C19 C20 C21 C26 -2.3(10) . . . . ?
N4 C20 C21 C26 179.7(6) . . . . ?
C19 C20 C21 C22 -178.4(6) . . . . ?
N4 C20 C21 C22 3.6(10) . . . . ?
C26 C21 C22 C23 2.4(11) . . . . ?
C20 C21 C22 C23 178.6(7) . . . . ?
C21 C22 C23 C24 1.5(12) . . . . ?
C22 C23 C24 C25 -3.6(13) . . . . ?
C23 C24 C25 C26 1.6(12) . . . . ?
C14 C13 C26 C21 1.7(10) . . . . ?
C12 C13 C26 C21 -177.2(6) . . . . ?
C14 C13 C26 C25 -178.4(6) . . . . ?
C12 C13 C26 C25 2.8(10) . . . . ?
C22 C21 C26 C13 175.6(6) . . . . ?
C20 C21 C26 C13 -0.6(10) . . . . ?
C22 C21 C26 C25 -4.3(9) . . . . ?
C20 C21 C26 C25 179.4(6) . . . . ?
C24 C25 C26 C13 -177.6(7) . . . . ?
C24 C25 C26 C21 2.4(10) . . . . ?
C37 N4 C27 C28 -146.3(6) . . . . ?
C20 N4 C27 C28 41.2(9) . . . . ?
C37 N4 C27 C32 33.0(9) . . . . ?
C20 N4 C27 C32 -139.4(7) . . . . ?
C32 C27 C28 C29 -0.2(10) . . . . ?
N4 C27 C28 C29 179.2(6) . . . . ?
C27 C28 C29 C30 -1.4(10) . . . . ?
C28 C29 C30 C31 2.0(10) . . . . ?
C28 C29 C30 C33 -176.8(6) . . . . ?
C29 C30 C31 C32 -1.1(10) . . . . ?
C33 C30 C31 C32 177.8(6) . . . . ?
C30 C31 C32 C27 -0.4(11) . . . . ?
C28 C27 C32 C31 1.1(10) . . . . ?
N4 C27 C32 C31 -178.3(6) . . . . ?
C29 C30 C33 C35 5.0(10) . . . . ?
C31 C30 C33 C35 -173.7(7) . . . . ?
C29 C30 C33 C34 126.3(8) . . . . ?
C31 C30 C33 C34 -52.4(9) . . . . ?
C29 C30 C33 C36 -114.8(8) . . . . ?
C31 C30 C33 C36 66.5(9) . . . . ?
C27 N4 C37 C42 -145.9(7) . . . . ?
C20 N4 C37 C42 26.5(9) . . . . ?
C27 N4 C37 C38 34.3(9) . . . . ?
C20 N4 C37 C38 -153.3(6) . . . . ?
C42 C37 C38 C39 2.5(10) . . . . ?
N4 C37 C38 C39 -177.7(6) . . . . ?
C37 C38 C39 C40 -1.9(11) . . . . ?
C38 C39 C40 C41 0.2(10) . . . . ?
C38 C39 C40 C43 178.8(7) . . . . ?
C39 C40 C41 C42 0.7(10) . . . . ?
C43 C40 C41 C42 -177.8(7) . . . . ?
C40 C41 C42 C37 0.0(11) . . . . ?
C38 C37 C42 C41 -1.6(10) . . . . ?
N4 C37 C42 C41 178.6(6) . . . . ?
C39 C40 C43 C46 -132(2) . . . . ?
C41 C40 C43 C46 46(2) . . . . ?
C39 C40 C43 C45' -57(2) . . . . ?
C41 C40 C43 C45' 121.9(19) . . . . ?
C39 C40 C43 C45 -2(2) . . . . ?
C41 C40 C43 C45 176.5(18) . . . . ?
C39 C40 C43 C44' 68.9(16) . . . . ?
C41 C40 C43 C44' -112.6(15) . . . . ?
C39 C40 C43 C44 115.2(18) . . . . ?
C41 C40 C43 C44 -66.3(19) . . . . ?
C39 C40 C43 C46' -177.9(16) . . . . ?
C41 C40 C43 C46' 0.6(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        24.25
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 959339'