# Electronic Supplementary Material (ESI) for Chemical Communications
# 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 
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#  except for the purpose of generating routine backup copies 
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data_w
_database_code_depnum_ccdc_archive 'CCDC 911645'
#TrackingRef 'W.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H23 N3 O3'
_chemical_formula_sum            'C26 H23 N3 O3'
_chemical_formula_weight         425.47

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  -p1

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

_cell_length_a                   11.1712(11)
_cell_length_b                   12.0660(12)
_cell_length_c                   17.6929(18)
_cell_angle_alpha                70.489(2)
_cell_angle_beta                 83.942(2)
_cell_angle_gamma                86.093(2)
_cell_volume                     2234.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3000
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      28.4

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_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  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12218
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         26.05
_reflns_number_total             8581
_reflns_number_gt                6027
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97

_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^)+(0.0793P)^2^+1.2545P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8581
_refine_ls_number_parameters     577
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1748
_refine_ls_wR_factor_gt          0.1574
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
N2 N 1.00110(19) 0.23388(18) 0.02644(14) 0.0388(5) Uani 1 1 d . . .
H4 H 1.0617 0.1971 0.0513 0.047 Uiso 1 1 calc R . .
C13 C 1.2804(2) 0.3935(2) 0.18176(16) 0.0332(5) Uani 1 1 d . . .
N1 N 1.05840(17) 0.43412(17) 0.19946(13) 0.0320(5) Uani 1 1 d . . .
N3 N 1.28812(17) 0.49131(18) 0.11591(12) 0.0339(5) Uani 1 1 d . . .
H5 H 1.2250 0.5146 0.0901 0.041 Uiso 1 1 calc R . .
C1 C 1.1532(2) 0.3412(2) 0.20531(15) 0.0322(5) Uani 1 1 d . . .
C3 C 1.0168(2) 0.3524(2) 0.10763(15) 0.0315(5) Uani 1 1 d . . .
C4 C 0.9834(2) 0.4356(2) 0.14469(15) 0.0311(5) Uani 1 1 d . . .
C6 C 0.9553(2) 0.3299(2) 0.04502(15) 0.0336(6) Uani 1 1 d . . .
C2 C 1.1214(2) 0.2881(2) 0.14233(15) 0.0325(5) Uani 1 1 d . . .
O2 O 1.18028(15) 0.20520(16) 0.12926(12) 0.0418(5) Uani 1 1 d . . .
O3 O 1.36340(16) 0.34582(16) 0.22080(12) 0.0466(5) Uani 1 1 d . . .
O5 O 0.69919(17) 0.29374(17) 0.36860(13) 0.0529(5) Uani 1 1 d . . .
O1 O 0.87116(16) 0.39247(15) 0.01210(11) 0.0419(5) Uani 1 1 d . . .
O6 O 0.37897(16) 0.13781(17) 0.51362(12) 0.0489(5) Uani 1 1 d . . .
O4 O 0.88291(17) 0.1556(2) 0.26093(15) 0.0756(8) Uani 1 1 d . . .
C5 C 0.8782(2) 0.5209(2) 0.13102(18) 0.0397(6) Uani 1 1 d . . .
H10A H 0.8782 0.5678 0.1655 0.060 Uiso 1 1 calc R . .
H10B H 0.8050 0.4787 0.1430 0.060 Uiso 1 1 calc R . .
H10C H 0.8838 0.5711 0.0758 0.060 Uiso 1 1 calc R . .
C31 C 0.3892(2) 0.0105(2) 0.39470(17) 0.0412(6) Uani 1 1 d . . .
H10D H 0.3882 -0.0363 0.3603 0.062 Uiso 1 1 calc R . .
H10E H 0.3172 0.0595 0.3908 0.062 Uiso 1 1 calc R . .
H10F H 0.3933 -0.0402 0.4494 0.062 Uiso 1 1 calc R . .
C26 C 1.1486(2) 0.2472(2) 0.28798(16) 0.0404(6) Uani 1 1 d . . .
H10G H 1.1684 0.2808 0.3270 0.061 Uiso 1 1 calc R . .
H10H H 1.2054 0.1843 0.2868 0.061 Uiso 1 1 calc R . .
H10I H 1.0689 0.2172 0.3023 0.061 Uiso 1 1 calc R . .
C38 C 0.6672(2) 0.2576(2) 0.20962(18) 0.0472(7) Uani 1 1 d . . .
H10J H 0.5874 0.2925 0.2035 0.071 Uiso 1 1 calc R . .
H10K H 0.6890 0.2219 0.1688 0.071 Uiso 1 1 calc R . .
H10L H 0.7232 0.3172 0.2044 0.071 Uiso 1 1 calc R . .
N4 N 0.80602(18) 0.00559(19) 0.36746(13) 0.0383(5) Uani 1 1 d . . .
H2 H 0.7400 -0.0248 0.3931 0.046 Uiso 1 1 calc R . .
N5 N 0.57501(17) 0.07909(18) 0.30805(13) 0.0363(5) Uani 1 1 d . . .
C30 C 0.4964(2) 0.0857(2) 0.36935(16) 0.0354(6) Uani 1 1 d . . .
N6 N 0.5200(2) 0.2759(2) 0.49225(15) 0.0474(6) Uani 1 1 d . . .
H1 H 0.5825 0.3055 0.4612 0.057 Uiso 1 1 calc R . .
C14 C 1.3932(2) 0.5584(2) 0.08634(15) 0.0325(5) Uani 1 1 d . . .
C40 C 0.9160(2) -0.0539(2) 0.39483(16) 0.0346(6) Uani 1 1 d . . .
C15 C 1.4152(2) 0.6131(2) 0.00401(16) 0.0373(6) Uani 1 1 d . . .
H37 H 1.3625 0.6045 -0.0308 0.045 Uiso 1 1 calc R . .
C20 C 1.0390(2) 0.4917(2) 0.25945(16) 0.0353(6) Uani 1 1 d . . .
C32 C 0.4520(2) 0.0610(2) 0.20669(18) 0.0429(7) Uani 1 1 d . . .
H16 H 0.3958 0.1144 0.2188 0.051 Uiso 1 1 calc R . .
C29 C 0.5295(2) 0.1664(2) 0.40352(17) 0.0381(6) Uani 1 1 d . . .
C28 C 0.6375(2) 0.2193(2) 0.35889(17) 0.0395(6) Uani 1 1 d . . .
C41 C 1.0183(2) -0.0510(2) 0.34283(17) 0.0394(6) Uani 1 1 d . . .
H28 H 1.0167 -0.0110 0.2880 0.047 Uiso 1 1 calc R . .
C42 C 1.1231(2) -0.1083(2) 0.37354(19) 0.0446(7) Uani 1 1 d . . .
H27 H 1.1920 -0.1064 0.3388 0.054 Uiso 1 1 calc R . .
C27 C 0.6703(2) 0.1643(2) 0.29229(17) 0.0388(6) Uani 1 1 d . . .
C39 C 0.7975(2) 0.1061(2) 0.30432(17) 0.0422(7) Uani 1 1 d . . .
C7 C 0.9589(2) 0.1882(2) -0.02993(17) 0.0404(6) Uani 1 1 d . . .
C19 C 1.4714(2) 0.5723(2) 0.13779(17) 0.0429(6) Uani 1 1 d . . .
H81 H 1.4567 0.5365 0.1931 0.051 Uiso 1 1 calc R . .
C37 C 0.5541(2) 0.0273(2) 0.24833(17) 0.0397(6) Uani 1 1 d . . .
C45 C 0.9188(3) -0.1158(3) 0.47595(18) 0.0499(7) Uani 1 1 d . . .
H24 H 0.8496 -0.1198 0.5108 0.060 Uiso 1 1 calc R . .
C46 C 0.4679(2) 0.1911(2) 0.47379(17) 0.0398(6) Uani 1 1 d . . .
C16 C 1.5156(3) 0.6802(2) -0.02613(18) 0.0449(7) Uani 1 1 d . . .
H38 H 1.5302 0.7169 -0.0814 0.054 Uiso 1 1 calc R . .
C47 C 0.4866(3) 0.3227(2) 0.55479(18) 0.0485(7) Uani 1 1 d . . .
C8 C 0.8390(3) 0.1925(3) -0.0421(2) 0.0505(7) Uani 1 1 d . . .
H45 H 0.7824 0.2290 -0.0149 0.061 Uiso 1 1 calc R . .
C18 C 1.5717(3) 0.6396(3) 0.1066(2) 0.0511(7) Uani 1 1 d . . .
H40 H 1.6245 0.6487 0.1413 0.061 Uiso 1 1 calc R . .
C24 C 0.9371(3) 0.5059(3) 0.3818(2) 0.0590(8) Uani 1 1 d . . .
H32 H 0.8777 0.4808 0.4242 0.071 Uiso 1 1 calc R . .
C33 C 0.4343(3) 0.0150(3) 0.1472(2) 0.0528(8) Uani 1 1 d . . .
H17 H 0.3650 0.0362 0.1200 0.063 Uiso 1 1 calc R . .
C17 C 1.5941(2) 0.6934(3) 0.0248(2) 0.0492(7) Uani 1 1 d . . .
H39 H 1.6619 0.7382 0.0041 0.059 Uiso 1 1 calc R . .
C25 C 0.9503(3) 0.4543(3) 0.32195(18) 0.0465(7) Uani 1 1 d . . .
H33 H 0.8998 0.3950 0.3239 0.056 Uiso 1 1 calc R . .
C36 C 0.6381(3) -0.0511(3) 0.2295(2) 0.0544(8) Uani 1 1 d . . .
H20 H 0.7067 -0.0739 0.2574 0.065 Uiso 1 1 calc R . .
C43 C 1.1273(3) -0.1679(3) 0.4541(2) 0.0502(7) Uani 1 1 d . . .
H26 H 1.1986 -0.2051 0.4739 0.060 Uiso 1 1 calc R . .
C44 C 1.0252(3) -0.1722(3) 0.5052(2) 0.0570(8) Uani 1 1 d . . .
H25 H 1.0272 -0.2131 0.5599 0.068 Uiso 1 1 calc R . .
C12 C 1.0426(3) 0.1326(3) -0.07032(19) 0.0505(7) Uani 1 1 d . . .
H41 H 1.1238 0.1297 -0.0622 0.061 Uiso 1 1 calc R . .
C21 C 1.1136(3) 0.5798(3) 0.2567(2) 0.0548(8) Uani 1 1 d . . .
H35 H 1.1739 0.6045 0.2149 0.066 Uiso 1 1 calc R . .
C48 C 0.5718(3) 0.3871(3) 0.5725(2) 0.0633(9) Uani 1 1 d . . .
H5A H 0.6486 0.3937 0.5457 0.076 Uiso 1 1 calc R . .
C9 C 0.8034(3) 0.1419(3) -0.0955(2) 0.0608(9) Uani 1 1 d . . .
H44 H 0.7225 0.1459 -0.1044 0.073 Uiso 1 1 calc R . .
C10 C 0.8848(3) 0.0862(3) -0.1354(2) 0.0599(9) Uani 1 1 d . . .
H43 H 0.8592 0.0521 -0.1706 0.072 Uiso 1 1 calc R . .
C34 C 0.5192(3) -0.0628(3) 0.1278(2) 0.0637(9) Uani 1 1 d . . .
H18 H 0.5079 -0.0926 0.0870 0.076 Uiso 1 1 calc R . .
C52 C 0.3728(3) 0.3122(3) 0.5958(2) 0.0635(9) Uani 1 1 d . . .
H3 H 0.3151 0.2690 0.5848 0.076 Uiso 1 1 calc R . .
C23 C 1.0111(3) 0.5936(3) 0.3788(2) 0.0668(10) Uani 1 1 d . . .
H31 H 1.0021 0.6278 0.4192 0.080 Uiso 1 1 calc R . .
C11 C 1.0045(3) 0.0814(3) -0.1229(2) 0.0611(9) Uani 1 1 d . . .
H42 H 1.0604 0.0437 -0.1498 0.073 Uiso 1 1 calc R . .
C35 C 0.6199(3) -0.0953(3) 0.1692(3) 0.0693(10) Uani 1 1 d . . .
H19 H 0.6767 -0.1479 0.1566 0.083 Uiso 1 1 calc R . .
C51 C 0.3461(4) 0.3672(3) 0.6537(2) 0.0746(11) Uani 1 1 d . . .
H2A H 0.2702 0.3596 0.6817 0.090 Uiso 1 1 calc R . .
C50 C 0.4294(4) 0.4323(3) 0.6701(2) 0.0752(11) Uani 1 1 d . . .
H1A H 0.4095 0.4699 0.7080 0.090 Uiso 1 1 calc R . .
C22 C 1.0986(3) 0.6310(3) 0.3161(2) 0.0726(11) Uani 1 1 d . . .
H48 H 1.1480 0.6912 0.3137 0.087 Uiso 1 1 calc R . .
C49 C 0.5423(4) 0.4416(3) 0.6301(2) 0.0747(11) Uani 1 1 d . . .
H6 H 0.5994 0.4848 0.6417 0.090 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
N2 0.0378(12) 0.0382(12) 0.0434(13) -0.0152(10) -0.0111(10) -0.0004(9)
C13 0.0286(12) 0.0355(13) 0.0350(14) -0.0105(11) -0.0056(11) 0.0004(10)
N1 0.0288(10) 0.0302(10) 0.0353(12) -0.0082(9) -0.0044(9) -0.0004(8)
N3 0.0268(10) 0.0386(12) 0.0323(12) -0.0052(9) -0.0055(9) -0.0016(8)
C1 0.0287(12) 0.0312(13) 0.0344(14) -0.0068(11) -0.0065(10) 0.0003(10)
C3 0.0297(12) 0.0266(12) 0.0345(14) -0.0037(10) -0.0051(10) -0.0041(9)
C4 0.0275(12) 0.0259(12) 0.0347(14) -0.0024(10) -0.0027(10) -0.0051(9)
C6 0.0319(13) 0.0314(13) 0.0335(14) -0.0037(11) -0.0057(11) -0.0058(10)
C2 0.0310(12) 0.0292(13) 0.0338(14) -0.0057(11) -0.0016(10) -0.0039(10)
O2 0.0373(10) 0.0398(10) 0.0513(12) -0.0186(9) -0.0099(8) 0.0056(8)
O3 0.0323(9) 0.0467(11) 0.0508(12) -0.0001(9) -0.0141(9) -0.0001(8)
O5 0.0437(11) 0.0493(12) 0.0637(14) -0.0142(10) 0.0011(10) -0.0205(9)
O1 0.0421(10) 0.0364(10) 0.0458(11) -0.0076(8) -0.0184(9) 0.0004(8)
O6 0.0381(10) 0.0462(11) 0.0534(13) -0.0057(9) 0.0038(9) -0.0070(9)
O4 0.0281(10) 0.0740(15) 0.0825(17) 0.0294(13) 0.0015(11) -0.0092(10)
C5 0.0319(13) 0.0328(13) 0.0524(17) -0.0111(12) -0.0072(12) 0.0025(10)
C31 0.0273(12) 0.0396(14) 0.0484(17) -0.0013(12) -0.0063(11) -0.0072(11)
C26 0.0389(14) 0.0378(14) 0.0379(15) -0.0031(12) -0.0053(12) -0.0026(11)
C38 0.0371(14) 0.0398(15) 0.0526(18) 0.0036(13) -0.0091(13) -0.0065(12)
N4 0.0239(10) 0.0422(12) 0.0398(13) -0.0014(10) -0.0004(9) -0.0055(9)
N5 0.0266(10) 0.0343(11) 0.0423(13) -0.0035(10) -0.0049(9) -0.0065(8)
C30 0.0251(12) 0.0298(13) 0.0410(15) 0.0032(11) -0.0085(11) -0.0001(10)
N6 0.0454(13) 0.0419(13) 0.0489(15) -0.0077(11) 0.0016(11) -0.0067(11)
C14 0.0281(12) 0.0313(13) 0.0365(14) -0.0094(11) -0.0018(10) 0.0005(10)
C40 0.0274(12) 0.0348(13) 0.0419(15) -0.0120(12) -0.0047(11) -0.0022(10)
C15 0.0391(14) 0.0373(14) 0.0336(14) -0.0095(11) -0.0029(11) -0.0008(11)
C20 0.0349(13) 0.0339(13) 0.0364(15) -0.0112(11) -0.0028(11) 0.0009(10)
C32 0.0369(14) 0.0342(14) 0.0524(18) -0.0055(13) -0.0108(13) -0.0004(11)
C29 0.0285(12) 0.0325(13) 0.0448(16) -0.0007(12) -0.0048(11) -0.0031(10)
C28 0.0306(13) 0.0345(14) 0.0457(16) -0.0011(12) -0.0079(11) -0.0047(11)
C41 0.0358(14) 0.0447(15) 0.0387(15) -0.0145(12) -0.0032(11) -0.0050(11)
C42 0.0290(13) 0.0487(16) 0.061(2) -0.0252(15) -0.0021(13) -0.0023(12)
C27 0.0272(12) 0.0371(14) 0.0438(16) -0.0005(12) -0.0046(11) -0.0094(10)
C39 0.0273(13) 0.0425(15) 0.0465(17) 0.0006(13) -0.0033(12) -0.0078(11)
C7 0.0479(15) 0.0348(14) 0.0385(15) -0.0102(12) -0.0062(12) -0.0069(12)
C19 0.0422(15) 0.0491(16) 0.0345(15) -0.0084(12) -0.0040(12) -0.0096(12)
C37 0.0332(13) 0.0334(14) 0.0452(16) -0.0020(12) -0.0041(12) -0.0063(11)
C45 0.0376(15) 0.0545(18) 0.0453(18) -0.0027(14) 0.0004(13) 0.0065(13)
C46 0.0339(13) 0.0328(13) 0.0443(16) -0.0002(12) -0.0085(12) -0.0004(11)
C16 0.0477(16) 0.0382(15) 0.0422(16) -0.0075(12) 0.0074(13) -0.0044(12)
C47 0.0537(17) 0.0390(15) 0.0458(18) -0.0046(13) -0.0098(14) 0.0056(13)
C8 0.0463(16) 0.0486(17) 0.064(2) -0.0266(15) -0.0104(15) -0.0031(13)
C18 0.0422(16) 0.0546(18) 0.057(2) -0.0157(15) -0.0118(14) -0.0100(13)
C24 0.063(2) 0.066(2) 0.0443(19) -0.0188(16) 0.0098(15) 0.0020(17)
C33 0.0505(17) 0.0433(16) 0.065(2) -0.0137(15) -0.0191(15) -0.0040(13)
C17 0.0359(14) 0.0446(16) 0.061(2) -0.0110(14) 0.0059(14) -0.0101(12)
C25 0.0421(15) 0.0449(16) 0.0478(18) -0.0104(14) 0.0024(13) -0.0035(12)
C36 0.0386(15) 0.0567(18) 0.070(2) -0.0221(17) -0.0130(15) 0.0053(13)
C43 0.0360(15) 0.0523(17) 0.064(2) -0.0193(16) -0.0161(14) 0.0093(13)
C44 0.0511(18) 0.063(2) 0.0459(18) -0.0040(15) -0.0089(15) 0.0104(15)
C12 0.0493(17) 0.0571(18) 0.0491(18) -0.0228(15) 0.0004(14) -0.0093(14)
C21 0.0559(18) 0.0551(18) 0.059(2) -0.0286(16) 0.0125(15) -0.0195(15)
C48 0.071(2) 0.056(2) 0.062(2) -0.0145(17) -0.0174(18) -0.0001(17)
C9 0.0583(19) 0.060(2) 0.074(2) -0.0300(18) -0.0195(17) -0.0076(16)
C10 0.073(2) 0.064(2) 0.052(2) -0.0285(17) -0.0110(17) -0.0132(17)
C34 0.062(2) 0.063(2) 0.074(2) -0.0312(19) -0.0134(18) -0.0029(17)
C52 0.066(2) 0.061(2) 0.061(2) -0.0190(17) -0.0022(17) 0.0056(17)
C23 0.078(2) 0.075(2) 0.058(2) -0.0395(19) -0.0002(19) -0.001(2)
C11 0.073(2) 0.062(2) 0.054(2) -0.0294(17) 0.0083(17) -0.0076(17)
C35 0.0521(19) 0.071(2) 0.095(3) -0.042(2) -0.0114(19) 0.0107(17)
C51 0.078(3) 0.075(3) 0.066(3) -0.022(2) -0.005(2) 0.018(2)
C50 0.106(3) 0.067(2) 0.052(2) -0.0178(18) -0.020(2) 0.021(2)
C22 0.077(2) 0.074(2) 0.085(3) -0.051(2) 0.012(2) -0.026(2)
C49 0.100(3) 0.068(2) 0.061(2) -0.021(2) -0.030(2) 0.003(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
N2 C6 1.360(3) . ?
N2 C7 1.422(3) . ?
N2 H4 0.8600 . ?
C13 O3 1.211(3) . ?
C13 N3 1.353(3) . ?
C13 C1 1.553(3) . ?
N1 C4 1.341(3) . ?
N1 C20 1.442(3) . ?
N1 C1 1.475(3) . ?
N3 C14 1.422(3) . ?
N3 H5 0.8600 . ?
C1 C26 1.520(3) . ?
C1 C2 1.539(3) . ?
C3 C4 1.384(4) . ?
C3 C2 1.432(3) . ?
C3 C6 1.470(3) . ?
C4 C5 1.493(3) . ?
C6 O1 1.232(3) . ?
C2 O2 1.233(3) . ?
O5 C28 1.234(3) . ?
O6 C46 1.238(3) . ?
O4 C39 1.214(3) . ?
C5 H10A 0.9600 . ?
C5 H10B 0.9600 . ?
C5 H10C 0.9600 . ?
C31 C30 1.490(3) . ?
C31 H10D 0.9600 . ?
C31 H10E 0.9600 . ?
C31 H10F 0.9600 . ?
C26 H10G 0.9600 . ?
C26 H10H 0.9600 . ?
C26 H10I 0.9600 . ?
C38 C27 1.521(4) . ?
C38 H10J 0.9600 . ?
C38 H10K 0.9600 . ?
C38 H10L 0.9600 . ?
N4 C39 1.352(3) . ?
N4 C40 1.425(3) . ?
N4 H2 0.8600 . ?
N5 C30 1.342(3) . ?
N5 C37 1.440(4) . ?
N5 C27 1.471(3) . ?
C30 C29 1.393(4) . ?
N6 C46 1.356(3) . ?
N6 C47 1.409(4) . ?
N6 H1 0.8600 . ?
C14 C19 1.382(4) . ?
C14 C15 1.386(4) . ?
C40 C45 1.382(4) . ?
C40 C41 1.384(4) . ?
C15 C16 1.382(4) . ?
C15 H37 0.9300 . ?
C20 C21 1.380(4) . ?
C20 C25 1.380(4) . ?
C32 C33 1.381(4) . ?
C32 C37 1.386(4) . ?
C32 H16 0.9300 . ?
C29 C28 1.433(3) . ?
C29 C46 1.465(4) . ?
C28 C27 1.536(4) . ?
C41 C42 1.385(4) . ?
C41 H28 0.9300 . ?
C42 C43 1.369(4) . ?
C42 H27 0.9300 . ?
C27 C39 1.545(4) . ?
C7 C8 1.374(4) . ?
C7 C12 1.388(4) . ?
C19 C18 1.384(4) . ?
C19 H81 0.9300 . ?
C37 C36 1.383(4) . ?
C45 C44 1.388(4) . ?
C45 H24 0.9300 . ?
C16 C17 1.374(4) . ?
C16 H38 0.9300 . ?
C47 C52 1.387(4) . ?
C47 C48 1.391(4) . ?
C8 C9 1.385(4) . ?
C8 H45 0.9300 . ?
C18 C17 1.378(4) . ?
C18 H40 0.9300 . ?
C24 C23 1.371(5) . ?
C24 C25 1.387(4) . ?
C24 H32 0.9300 . ?
C33 C34 1.387(5) . ?
C33 H17 0.9300 . ?
C17 H39 0.9300 . ?
C25 H33 0.9300 . ?
C36 C35 1.380(5) . ?
C36 H20 0.9300 . ?
C43 C44 1.372(4) . ?
C43 H26 0.9300 . ?
C44 H25 0.9300 . ?
C12 C11 1.390(4) . ?
C12 H41 0.9300 . ?
C21 C22 1.377(4) . ?
C21 H35 0.9300 . ?
C48 C49 1.389(5) . ?
C48 H5A 0.9300 . ?
C9 C10 1.369(5) . ?
C9 H44 0.9300 . ?
C10 C11 1.372(5) . ?
C10 H43 0.9300 . ?
C34 C35 1.371(5) . ?
C34 H18 0.9300 . ?
C52 C51 1.394(5) . ?
C52 H3 0.9300 . ?
C23 C22 1.373(5) . ?
C23 H31 0.9300 . ?
C11 H42 0.9300 . ?
C35 H19 0.9300 . ?
C51 C50 1.369(6) . ?
C51 H2A 0.9300 . ?
C50 C49 1.371(6) . ?
C50 H1A 0.9300 . ?
C22 H48 0.9300 . ?
C49 H6 0.9300 . ?

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
C6 N2 C7 126.5(2) . . ?
C6 N2 H4 116.7 . . ?
C7 N2 H4 116.7 . . ?
O3 C13 N3 125.2(2) . . ?
O3 C13 C1 119.9(2) . . ?
N3 C13 C1 114.9(2) . . ?
C4 N1 C20 127.0(2) . . ?
C4 N1 C1 110.6(2) . . ?
C20 N1 C1 120.8(2) . . ?
C13 N3 C14 124.7(2) . . ?
C13 N3 H5 117.7 . . ?
C14 N3 H5 117.7 . . ?
N1 C1 C26 112.7(2) . . ?
N1 C1 C2 102.03(18) . . ?
C26 C1 C2 109.9(2) . . ?
N1 C1 C13 111.42(18) . . ?
C26 C1 C13 110.4(2) . . ?
C2 C1 C13 110.1(2) . . ?
C4 C3 C2 108.2(2) . . ?
C4 C3 C6 126.8(2) . . ?
C2 C3 C6 125.0(2) . . ?
N1 C4 C3 112.3(2) . . ?
N1 C4 C5 119.4(2) . . ?
C3 C4 C5 128.3(2) . . ?
O1 C6 N2 123.3(2) . . ?
O1 C6 C3 123.3(2) . . ?
N2 C6 C3 113.4(2) . . ?
O2 C2 C3 130.9(2) . . ?
O2 C2 C1 122.2(2) . . ?
C3 C2 C1 106.9(2) . . ?
C4 C5 H10A 109.5 . . ?
C4 C5 H10B 109.5 . . ?
H10A C5 H10B 109.5 . . ?
C4 C5 H10C 109.5 . . ?
H10A C5 H10C 109.5 . . ?
H10B C5 H10C 109.5 . . ?
C30 C31 H10D 109.5 . . ?
C30 C31 H10E 109.5 . . ?
H10D C31 H10E 109.5 . . ?
C30 C31 H10F 109.5 . . ?
H10D C31 H10F 109.5 . . ?
H10E C31 H10F 109.5 . . ?
C1 C26 H10G 109.5 . . ?
C1 C26 H10H 109.5 . . ?
H10G C26 H10H 109.5 . . ?
C1 C26 H10I 109.5 . . ?
H10G C26 H10I 109.5 . . ?
H10H C26 H10I 109.5 . . ?
C27 C38 H10J 109.5 . . ?
C27 C38 H10K 109.5 . . ?
H10J C38 H10K 109.5 . . ?
C27 C38 H10L 109.5 . . ?
H10J C38 H10L 109.5 . . ?
H10K C38 H10L 109.5 . . ?
C39 N4 C40 125.1(2) . . ?
C39 N4 H2 117.5 . . ?
C40 N4 H2 117.5 . . ?
C30 N5 C37 126.0(2) . . ?
C30 N5 C27 110.7(2) . . ?
C37 N5 C27 120.5(2) . . ?
N5 C30 C29 112.2(2) . . ?
N5 C30 C31 120.6(2) . . ?
C29 C30 C31 127.2(3) . . ?
C46 N6 C47 129.5(2) . . ?
C46 N6 H1 115.3 . . ?
C47 N6 H1 115.3 . . ?
C19 C14 C15 119.7(2) . . ?
C19 C14 N3 121.5(2) . . ?
C15 C14 N3 118.7(2) . . ?
C45 C40 C41 119.8(2) . . ?
C45 C40 N4 118.2(2) . . ?
C41 C40 N4 122.0(2) . . ?
C16 C15 C14 119.8(3) . . ?
C16 C15 H37 120.1 . . ?
C14 C15 H37 120.1 . . ?
C21 C20 C25 120.1(3) . . ?
C21 C20 N1 119.8(2) . . ?
C25 C20 N1 120.0(2) . . ?
C33 C32 C37 119.8(3) . . ?
C33 C32 H16 120.1 . . ?
C37 C32 H16 120.1 . . ?
C30 C29 C28 107.6(2) . . ?
C30 C29 C46 126.6(2) . . ?
C28 C29 C46 125.7(2) . . ?
O5 C28 C29 130.0(3) . . ?
O5 C28 C27 122.7(2) . . ?
C29 C28 C27 107.3(2) . . ?
C40 C41 C42 119.2(3) . . ?
C40 C41 H28 120.4 . . ?
C42 C41 H28 120.4 . . ?
C43 C42 C41 121.3(3) . . ?
C43 C42 H27 119.3 . . ?
C41 C42 H27 119.3 . . ?
N5 C27 C38 112.0(2) . . ?
N5 C27 C28 102.0(2) . . ?
C38 C27 C28 110.6(2) . . ?
N5 C27 C39 113.3(2) . . ?
C38 C27 C39 110.9(2) . . ?
C28 C27 C39 107.5(2) . . ?
O4 C39 N4 124.4(2) . . ?
O4 C39 C27 119.2(2) . . ?
N4 C39 C27 116.3(2) . . ?
C8 C7 C12 119.9(3) . . ?
C8 C7 N2 122.2(3) . . ?
C12 C7 N2 117.8(2) . . ?
C14 C19 C18 119.7(3) . . ?
C14 C19 H81 120.1 . . ?
C18 C19 H81 120.1 . . ?
C36 C37 C32 119.9(3) . . ?
C36 C37 N5 120.3(2) . . ?
C32 C37 N5 119.7(2) . . ?
C40 C45 C44 119.8(3) . . ?
C40 C45 H24 120.1 . . ?
C44 C45 H24 120.1 . . ?
O6 C46 N6 123.3(3) . . ?
O6 C46 C29 123.5(2) . . ?
N6 C46 C29 113.2(2) . . ?
C17 C16 C15 120.6(3) . . ?
C17 C16 H38 119.7 . . ?
C15 C16 H38 119.7 . . ?
C52 C47 C48 119.5(3) . . ?
C52 C47 N6 123.2(3) . . ?
C48 C47 N6 117.1(3) . . ?
C7 C8 C9 119.2(3) . . ?
C7 C8 H45 120.4 . . ?
C9 C8 H45 120.4 . . ?
C17 C18 C19 120.6(3) . . ?
C17 C18 H40 119.7 . . ?
C19 C18 H40 119.7 . . ?
C23 C24 C25 120.4(3) . . ?
C23 C24 H32 119.8 . . ?
C25 C24 H32 119.8 . . ?
C32 C33 C34 120.3(3) . . ?
C32 C33 H17 119.8 . . ?
C34 C33 H17 119.8 . . ?
C16 C17 C18 119.5(3) . . ?
C16 C17 H39 120.3 . . ?
C18 C17 H39 120.3 . . ?
C20 C25 C24 119.4(3) . . ?
C20 C25 H33 120.3 . . ?
C24 C25 H33 120.3 . . ?
C35 C36 C37 119.7(3) . . ?
C35 C36 H20 120.2 . . ?
C37 C36 H20 120.2 . . ?
C42 C43 C44 119.3(3) . . ?
C42 C43 H26 120.3 . . ?
C44 C43 H26 120.3 . . ?
C43 C44 C45 120.5(3) . . ?
C43 C44 H25 119.8 . . ?
C45 C44 H25 119.8 . . ?
C7 C12 C11 119.8(3) . . ?
C7 C12 H41 120.1 . . ?
C11 C12 H41 120.1 . . ?
C22 C21 C20 119.8(3) . . ?
C22 C21 H35 120.1 . . ?
C20 C21 H35 120.1 . . ?
C49 C48 C47 120.0(4) . . ?
C49 C48 H5A 120.0 . . ?
C47 C48 H5A 120.0 . . ?
C10 C9 C8 121.5(3) . . ?
C10 C9 H44 119.3 . . ?
C8 C9 H44 119.3 . . ?
C9 C10 C11 119.3(3) . . ?
C9 C10 H43 120.3 . . ?
C11 C10 H43 120.3 . . ?
C35 C34 C33 119.4(3) . . ?
C35 C34 H18 120.3 . . ?
C33 C34 H18 120.3 . . ?
C47 C52 C51 119.1(4) . . ?
C47 C52 H3 120.5 . . ?
C51 C52 H3 120.5 . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H31 120.1 . . ?
C22 C23 H31 120.1 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H42 119.9 . . ?
C12 C11 H42 119.9 . . ?
C34 C35 C36 120.9(3) . . ?
C34 C35 H19 119.6 . . ?
C36 C35 H19 119.6 . . ?
C50 C51 C52 121.3(4) . . ?
C50 C51 H2A 119.3 . . ?
C52 C51 H2A 119.3 . . ?
C51 C50 C49 119.6(4) . . ?
C51 C50 H1A 120.2 . . ?
C49 C50 H1A 120.2 . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H48 119.8 . . ?
C21 C22 H48 119.8 . . ?
C50 C49 C48 120.5(4) . . ?
C50 C49 H6 119.8 . . ?
C48 C49 H6 119.8 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.047