# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Jingui Qin'
_publ_contact_author_email       JGQIN@WHU.EDU.CN

_publ_section_title              
;
Synthesis, crystal structures and nonlinear optical
properties of three TCF-based chromophores
;
loop_
_publ_author_name
'Jingui Qin.'
'Xiao-Ming Chen.'
'Yang Fu.'
'Suyue Li.'
'Ming Li.'
'Tao Liu.'
;
Kuizhan Shao
;
'Zhong-Min Su.'
'Ming-Liang Tong.'

# Attachment 'B811833G-revised.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 635874'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 N4 O2'
_chemical_formula_weight         374.44

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

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

_cell_length_a                   7.7958(10)
_cell_length_b                   11.5638(15)
_cell_length_c                   12.0921(16)
_cell_angle_alpha                75.457(2)
_cell_angle_beta                 74.781(2)
_cell_angle_gamma                80.840(2)
_cell_volume                     1013.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    956
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      21.45

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9808
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      292(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            5122
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3506
_reflns_number_gt                2315
_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 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^)+(0.0572P)^2^+0.4011P] 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     SHELXL
_refine_ls_extinction_coef       0.0045(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3506
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0675
_refine_ls_wR_factor_ref         0.1680
_refine_ls_wR_factor_gt          0.1428
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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 -0.0854(4) 1.2256(3) 0.8259(3) 0.0635(8) Uani 1 1 d . . .
C2 C 0.0572(4) 1.1598(3) 0.8753(2) 0.0523(7) Uani 1 1 d . . .
C3 C 0.0682(4) 1.1809(3) 0.9833(3) 0.0622(8) Uani 1 1 d . . .
C4 C 0.1805(3) 1.0793(2) 0.8229(2) 0.0490(7) Uani 1 1 d . . .
C5 C 0.1951(3) 1.0382(2) 0.7186(2) 0.0482(7) Uani 1 1 d . . .
C6 C 0.0759(4) 1.0759(3) 0.6424(3) 0.0537(7) Uani 1 1 d . . .
C7 C 0.3408(4) 0.9530(2) 0.7057(2) 0.0489(7) Uani 1 1 d . . .
C8 C 0.4303(4) 0.9418(2) 0.8054(2) 0.0517(7) Uani 1 1 d . . .
C9 C 0.4296(4) 0.8192(3) 0.8876(3) 0.0639(9) Uani 1 1 d . . .
H9A H 0.4595 0.8242 0.9582 0.096 Uiso 1 1 calc R . .
H9B H 0.5157 0.7635 0.8500 0.096 Uiso 1 1 calc R . .
H9C H 0.3129 0.7923 0.9066 0.096 Uiso 1 1 calc R . .
C10 C 0.6127(4) 0.9889(3) 0.7671(3) 0.0677(9) Uani 1 1 d . . .
H10A H 0.6020 1.0715 0.7265 0.102 Uiso 1 1 calc R . .
H10B H 0.6928 0.9425 0.7157 0.102 Uiso 1 1 calc R . .
H10C H 0.6586 0.9824 0.8349 0.102 Uiso 1 1 calc R . .
C11 C 0.3902(4) 0.8870(2) 0.6171(2) 0.0537(7) Uani 1 1 d . . .
H11 H 0.3175 0.9012 0.5642 0.064 Uiso 1 1 calc R . .
C12 C 0.5346(4) 0.8041(3) 0.6014(2) 0.0546(7) Uani 1 1 d . . .
H12 H 0.6126 0.7955 0.6501 0.065 Uiso 1 1 calc R . .
C13 C 0.5789(4) 0.7293(2) 0.5186(2) 0.0507(7) Uani 1 1 d . . .
C14 C 0.4696(4) 0.7230(3) 0.4460(2) 0.0570(8) Uani 1 1 d . . .
H14 H 0.3606 0.7701 0.4513 0.068 Uiso 1 1 calc R . .
C15 C 0.5163(4) 0.6504(3) 0.3678(3) 0.0631(9) Uani 1 1 d . . .
H15 H 0.4401 0.6499 0.3203 0.076 Uiso 1 1 calc R . .
C16 C 0.6788(4) 0.5759(3) 0.3578(3) 0.0638(9) Uani 1 1 d . A .
C17 C 0.7906(4) 0.5829(3) 0.4293(3) 0.0693(9) Uani 1 1 d . . .
H17 H 0.9006 0.5370 0.4231 0.083 Uiso 1 1 calc R . .
C18 C 0.7413(4) 0.6557(3) 0.5074(3) 0.0618(8) Uani 1 1 d . . .
H18 H 0.8175 0.6566 0.5548 0.074 Uiso 1 1 calc R . .
C19 C 0.5976(5) 0.4868(4) 0.2131(3) 0.0871(12) Uani 1 1 d . A .
H19A H 0.6211 0.4075 0.1958 0.105 Uiso 1 1 calc R . .
H19B H 0.4752 0.4960 0.2579 0.105 Uiso 1 1 calc R . .
C20 C 0.6224(7) 0.5757(5) 0.1071(4) 0.138(2) Uani 1 1 d . . .
H20A H 0.6144 0.6531 0.1246 0.207 Uiso 1 1 calc R . .
H20B H 0.5317 0.5750 0.0668 0.207 Uiso 1 1 calc R . .
H20C H 0.7380 0.5590 0.0581 0.207 Uiso 1 1 calc R . .
C21 C 0.8631(16) 0.3949(11) 0.2969(7) 0.070(3) Uani 0.61(2) 1 d P A 1
H21A H 0.8749 0.3717 0.3776 0.084 Uiso 0.61(2) 1 calc PR A 1
H21B H 0.8297 0.3268 0.2769 0.084 Uiso 0.61(2) 1 calc PR A 1
C22 C 1.035(2) 0.4326(8) 0.2170(7) 0.080(3) Uani 0.61(2) 1 d P A 1
H22A H 1.0190 0.4628 0.1374 0.096 Uiso 0.61(2) 1 calc PR A 1
H22B H 1.0723 0.4964 0.2413 0.096 Uiso 0.61(2) 1 calc PR A 1
O2 O 1.1677(17) 0.3322(15) 0.2202(13) 0.089(3) Uani 0.61(2) 1 d P A 1
H2 H 1.1362 0.2789 0.1984 0.133 Uiso 0.61(2) 1 calc PR A 1
C21' C 0.922(3) 0.4640(14) 0.2311(11) 0.067(5) Uani 0.39(2) 1 d P A 2
H21C H 0.9452 0.4685 0.1474 0.081 Uiso 0.39(2) 1 calc PR A 2
H21D H 0.9986 0.5152 0.2447 0.081 Uiso 0.39(2) 1 calc PR A 2
C22' C 0.952(2) 0.3370(16) 0.2972(10) 0.075(5) Uani 0.39(2) 1 d P A 2
H22C H 0.9291 0.3356 0.3803 0.090 Uiso 0.39(2) 1 calc PR A 2
H22D H 0.8681 0.2896 0.2867 0.090 Uiso 0.39(2) 1 calc PR A 2
O2' O 1.121(3) 0.286(2) 0.261(2) 0.088(5) Uani 0.39(2) 1 d P A 2
H2' H 1.1397 0.2834 0.1918 0.132 Uiso 0.39(2) 1 calc PR A 2
N1 N -0.1995(4) 1.2808(3) 0.7895(3) 0.0994(11) Uani 1 1 d . . .
N2 N 0.0737(4) 1.1984(3) 1.0715(3) 0.0885(10) Uani 1 1 d . . .
N3 N -0.0167(4) 1.1057(3) 0.5792(3) 0.0792(9) Uani 1 1 d . . .
N4 N 0.7227(4) 0.5005(3) 0.2825(3) 0.0940(11) Uani 1 1 d . . .
O1 O 0.3120(2) 1.02455(17) 0.87496(17) 0.0604(6) 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 0.0526(18) 0.074(2) 0.072(2) -0.0326(17) -0.0226(16) 0.0111(16)
C2 0.0461(16) 0.0560(17) 0.0617(18) -0.0253(14) -0.0200(14) 0.0078(14)
C3 0.0539(18) 0.066(2) 0.074(2) -0.0345(17) -0.0202(16) 0.0126(15)
C4 0.0426(15) 0.0509(16) 0.0570(17) -0.0173(13) -0.0165(13) 0.0027(13)
C5 0.0468(16) 0.0468(16) 0.0513(16) -0.0136(13) -0.0119(13) -0.0007(13)
C6 0.0485(16) 0.0589(18) 0.0580(18) -0.0225(14) -0.0152(15) 0.0029(14)
C7 0.0471(16) 0.0472(16) 0.0495(16) -0.0116(13) -0.0068(13) -0.0024(13)
C8 0.0472(16) 0.0540(17) 0.0541(16) -0.0200(14) -0.0121(13) 0.0083(13)
C9 0.064(2) 0.064(2) 0.0576(18) -0.0119(15) -0.0122(15) 0.0069(16)
C10 0.0573(19) 0.065(2) 0.085(2) -0.0198(18) -0.0226(17) -0.0023(16)
C11 0.0530(17) 0.0557(17) 0.0495(16) -0.0123(14) -0.0108(13) 0.0025(14)
C12 0.0528(17) 0.0621(18) 0.0468(16) -0.0148(14) -0.0107(13) 0.0033(14)
C13 0.0492(16) 0.0564(17) 0.0433(15) -0.0121(13) -0.0102(13) 0.0055(14)
C14 0.0500(17) 0.0666(19) 0.0507(17) -0.0155(15) -0.0139(14) 0.0125(15)
C15 0.0565(18) 0.081(2) 0.0573(18) -0.0282(17) -0.0245(15) 0.0171(16)
C16 0.0578(19) 0.081(2) 0.0601(19) -0.0328(17) -0.0238(15) 0.0164(17)
C17 0.0507(17) 0.093(2) 0.078(2) -0.0465(19) -0.0321(16) 0.0284(17)
C18 0.0539(18) 0.079(2) 0.0614(19) -0.0311(16) -0.0249(15) 0.0132(16)
C19 0.099(3) 0.090(3) 0.079(3) -0.038(2) -0.031(2) 0.019(2)
C20 0.159(5) 0.140(5) 0.095(3) -0.021(3) -0.018(3) 0.015(4)
C21 0.069(6) 0.078(7) 0.071(4) -0.036(4) -0.018(4) 0.004(5)
C22 0.066(8) 0.096(6) 0.078(5) -0.033(4) -0.015(4) 0.010(5)
O2 0.059(5) 0.126(9) 0.104(8) -0.071(6) -0.037(5) 0.032(5)
C21' 0.054(11) 0.089(9) 0.064(6) -0.034(6) -0.015(6) 0.005(7)
C22' 0.073(10) 0.072(10) 0.084(7) -0.034(6) -0.017(6) 0.008(8)
O2' 0.074(10) 0.115(12) 0.095(11) -0.063(8) -0.036(7) 0.028(7)
N1 0.076(2) 0.125(3) 0.114(3) -0.055(2) -0.0546(19) 0.041(2)
N2 0.083(2) 0.113(3) 0.090(2) -0.060(2) -0.0356(17) 0.0200(18)
N3 0.0692(18) 0.099(2) 0.0793(19) -0.0285(17) -0.0347(16) 0.0081(16)
N4 0.0727(19) 0.135(3) 0.105(2) -0.082(2) -0.0550(17) 0.0491(18)
O1 0.0560(12) 0.0670(13) 0.0655(13) -0.0303(10) -0.0270(10) 0.0194(10)

_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 1.129(4) . ?
C1 C2 1.422(4) . ?
C2 C4 1.373(4) . ?
C2 C3 1.414(4) . ?
C3 N2 1.147(4) . ?
C4 O1 1.334(3) . ?
C4 C5 1.427(4) . ?
C5 C7 1.383(3) . ?
C5 C6 1.422(4) . ?
C6 N3 1.141(4) . ?
C7 C11 1.408(4) . ?
C7 C8 1.513(4) . ?
C8 O1 1.480(3) . ?
C8 C9 1.513(4) . ?
C8 C10 1.519(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.362(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.425(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C18 1.404(4) . ?
C14 C15 1.362(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.409(4) . ?
C15 H15 0.9300 . ?
C16 N4 1.359(4) . ?
C16 C17 1.402(4) . ?
C17 C18 1.362(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C20 1.417(5) . ?
C19 N4 1.493(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.49(2) . ?
C21 N4 1.512(15) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O2 1.43(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O2 H2 0.8200 . ?
C21' C22' 1.50(3) . ?
C21' N4 1.55(2) . ?
C21' H21C 0.9700 . ?
C21' H21D 0.9700 . ?
C22' O2' 1.36(3) . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?
O2' H2' 0.8200 . ?

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 177.3(3) . . ?
C4 C2 C3 120.2(3) . . ?
C4 C2 C1 123.1(3) . . ?
C3 C2 C1 116.7(2) . . ?
N2 C3 C2 178.7(3) . . ?
O1 C4 C2 118.3(2) . . ?
O1 C4 C5 110.3(2) . . ?
C2 C4 C5 131.4(3) . . ?
C7 C5 C6 125.5(3) . . ?
C7 C5 C4 108.9(2) . . ?
C6 C5 C4 125.5(2) . . ?
N3 C6 C5 178.5(3) . . ?
C5 C7 C11 125.1(3) . . ?
C5 C7 C8 107.7(2) . . ?
C11 C7 C8 127.2(2) . . ?
O1 C8 C9 105.8(2) . . ?
O1 C8 C7 102.8(2) . . ?
C9 C8 C7 114.2(2) . . ?
O1 C8 C10 105.9(2) . . ?
C9 C8 C10 112.8(2) . . ?
C7 C8 C10 114.1(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 126.1(3) . . ?
C12 C11 H11 116.9 . . ?
C7 C11 H11 116.9 . . ?
C11 C12 C13 127.0(3) . . ?
C11 C12 H12 116.5 . . ?
C13 C12 H12 116.5 . . ?
C14 C13 C18 116.3(3) . . ?
C14 C13 C12 124.1(3) . . ?
C18 C13 C12 119.5(3) . . ?
C15 C14 C13 122.5(3) . . ?
C15 C14 H14 118.7 . . ?
C13 C14 H14 118.7 . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
N4 C16 C17 122.1(3) . . ?
N4 C16 C15 120.8(3) . . ?
C17 C16 C15 117.0(3) . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C13 121.9(3) . . ?
C17 C18 H18 119.0 . . ?
C13 C18 H18 119.0 . . ?
C20 C19 N4 108.7(4) . . ?
C20 C19 H19A 109.9 . . ?
N4 C19 H19A 109.9 . . ?
C20 C19 H19B 109.9 . . ?
N4 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N4 107.6(10) . . ?
C22 C21 H21A 110.2 . . ?
N4 C21 H21A 110.2 . . ?
C22 C21 H21B 110.2 . . ?
N4 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
O2 C22 C21 109.4(13) . . ?
O2 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
O2 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
C22 O2 H2 109.5 . . ?
C22' C21' N4 103.4(14) . . ?
C22' C21' H21C 111.1 . . ?
N4 C21' H21C 111.1 . . ?
C22' C21' H21D 111.1 . . ?
N4 C21' H21D 111.1 . . ?
H21C C21' H21D 109.1 . . ?
O2' C22' C21' 112.5(19) . . ?
O2' C22' H22C 109.1 . . ?
C21' C22' H22C 109.1 . . ?
O2' C22' H22D 109.1 . . ?
C21' C22' H22D 109.1 . . ?
H22C C22' H22D 107.8 . . ?
C22' O2' H2' 109.5 . . ?
C16 N4 C19 121.9(3) . . ?
C16 N4 C21 121.0(3) . . ?
C19 N4 C21 113.3(4) . . ?
C16 N4 C21' 119.3(5) . . ?
C19 N4 C21' 114.9(4) . . ?
C21 N4 C21' 39.9(4) . . ?
C4 O1 C8 110.2(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
N1 C1 C2 C4 -164(9) . . . . ?
N1 C1 C2 C3 16(9) . . . . ?
C4 C2 C3 N2 -146(16) . . . . ?
C1 C2 C3 N2 34(16) . . . . ?
C3 C2 C4 O1 -1.7(4) . . . . ?
C1 C2 C4 O1 178.3(3) . . . . ?
C3 C2 C4 C5 176.9(3) . . . . ?
C1 C2 C4 C5 -3.2(5) . . . . ?
O1 C4 C5 C7 0.8(3) . . . . ?
C2 C4 C5 C7 -177.9(3) . . . . ?
O1 C4 C5 C6 178.9(3) . . . . ?
C2 C4 C5 C6 0.2(5) . . . . ?
C7 C5 C6 N3 -32(13) . . . . ?
C4 C5 C6 N3 150(13) . . . . ?
C6 C5 C7 C11 -2.4(4) . . . . ?
C4 C5 C7 C11 175.7(3) . . . . ?
C6 C5 C7 C8 179.5(3) . . . . ?
C4 C5 C7 C8 -2.3(3) . . . . ?
C5 C7 C8 O1 2.9(3) . . . . ?
C11 C7 C8 O1 -175.1(3) . . . . ?
C5 C7 C8 C9 117.0(3) . . . . ?
C11 C7 C8 C9 -61.1(4) . . . . ?
C5 C7 C8 C10 -111.2(3) . . . . ?
C11 C7 C8 C10 70.7(4) . . . . ?
C5 C7 C11 C12 178.9(3) . . . . ?
C8 C7 C11 C12 -3.5(5) . . . . ?
C7 C11 C12 C13 174.4(3) . . . . ?
C11 C12 C13 C14 -5.7(5) . . . . ?
C11 C12 C13 C18 174.6(3) . . . . ?
C18 C13 C14 C15 -0.4(4) . . . . ?
C12 C13 C14 C15 180.0(3) . . . . ?
C13 C14 C15 C16 1.0(5) . . . . ?
C14 C15 C16 N4 177.7(3) . . . . ?
C14 C15 C16 C17 -1.7(5) . . . . ?
N4 C16 C17 C18 -177.4(3) . . . . ?
C15 C16 C17 C18 2.1(5) . . . . ?
C16 C17 C18 C13 -1.6(5) . . . . ?
C14 C13 C18 C17 0.7(5) . . . . ?
C12 C13 C18 C17 -179.7(3) . . . . ?
N4 C21 C22 O2 -175.0(7) . . . . ?
N4 C21' C22' O2' 177.7(12) . . . . ?
C17 C16 N4 C19 175.5(3) . . . . ?
C15 C16 N4 C19 -4.0(6) . . . . ?
C17 C16 N4 C21 18.7(7) . . . . ?
C15 C16 N4 C21 -160.8(5) . . . . ?
C17 C16 N4 C21' -27.7(8) . . . . ?
C15 C16 N4 C21' 152.8(7) . . . . ?
C20 C19 N4 C16 87.1(5) . . . . ?
C20 C19 N4 C21 -114.5(5) . . . . ?
C20 C19 N4 C21' -70.7(7) . . . . ?
C22 C21 N4 C16 -96.5(6) . . . . ?
C22 C21 N4 C19 104.9(5) . . . . ?
C22 C21 N4 C21' 3.4(7) . . . . ?
C22' C21' N4 C16 105.7(7) . . . . ?
C22' C21' N4 C19 -95.9(7) . . . . ?
C22' C21' N4 C21 1.3(6) . . . . ?
C2 C4 O1 C8 -179.9(2) . . . . ?
C5 C4 O1 C8 1.2(3) . . . . ?
C9 C8 O1 C4 -122.5(3) . . . . ?
C7 C8 O1 C4 -2.5(3) . . . . ?
C10 C8 O1 C4 117.5(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2' H2' N2 0.82 2.15 2.86(2) 144.5 1_644
O2 H2 N2 0.82 2.17 2.934(14) 154.9 1_644
C15 H15 N1 0.93 2.49 3.381(4) 159.7 2_576
C12 H12 O2 0.93 2.65 3.504(14) 153.2 2_766
C12 H12 O2' 0.93 2.53 3.41(2) 158.6 2_766

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.035

# Attachment '3.cif'

data_3
_database_code_depnum_ccdc_archive 'CCDC 635875'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H32 N6 O3'
_chemical_formula_weight         536.63

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   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                   21.2261(18)
_cell_length_b                   7.0551(6)
_cell_length_c                   19.1150(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.781(1)
_cell_angle_gamma                90.00
_cell_volume                     2820.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9737
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21462
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4955
_reflns_number_gt                4199
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998'

_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^)+(0.0882P)^2^+8.4878P] 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         4955
_refine_ls_number_parameters     502
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0971
_refine_ls_wR_factor_ref         0.2649
_refine_ls_wR_factor_gt          0.2567
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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 0.46795(11) 0.8172(4) 0.33109(12) 0.0330(6) Uani 1 1 d . . .
N1 N 0.57779(17) 0.8178(5) 0.21767(18) 0.0454(9) Uani 1 1 d . . .
N2 N 0.39227(17) 0.6823(6) 0.08725(17) 0.0498(9) Uani 1 1 d . . .
N3 N 0.26965(19) 0.6834(8) 0.1846(2) 0.0705(13) Uani 1 1 d . . .
C1 C 0.43025(16) 0.7784(5) 0.27028(18) 0.0274(8) Uani 1 1 d . . .
C2 C 0.36538(17) 0.7518(5) 0.2814(2) 0.0314(8) Uani 1 1 d . . .
C3 C 0.3646(2) 0.7675(5) 0.3525(2) 0.0386(9) Uani 1 1 d . . .
C4 C 0.43104(19) 0.8113(6) 0.38991(19) 0.0367(9) Uani 1 1 d . . .
C5 C 0.45648(17) 0.7678(5) 0.20942(18) 0.0288(8) Uani 1 1 d . . .
C6 C 0.52411(18) 0.7951(5) 0.21429(18) 0.0306(8) Uani 1 1 d . . .
C7 C 0.42030(19) 0.7209(6) 0.1421(2) 0.0365(9) Uani 1 1 d . . .
C8 C 0.31304(19) 0.7133(6) 0.2276(2) 0.0445(10) Uani 1 1 d . . .
C9 C 0.4355(2) 1.0058(6) 0.4244(2) 0.0438(10) Uani 1 1 d . . .
H9A H 0.4115 1.0976 0.3918 0.066 Uiso 1 1 calc R . .
H9B H 0.4804 1.0447 0.4355 0.066 Uiso 1 1 calc R . .
H9C H 0.4174 1.0006 0.4683 0.066 Uiso 1 1 calc R . .
C10 C 0.4606(2) 0.6534(6) 0.4394(2) 0.0472(11) Uani 1 1 d . . .
H10A H 0.4563 0.5324 0.4138 0.071 Uiso 1 1 calc R . .
H10B H 0.4386 0.6457 0.4803 0.071 Uiso 1 1 calc R . .
H10C H 0.5060 0.6806 0.4557 0.071 Uiso 1 1 calc R . .
C11 C 0.3158(2) 0.7551(7) 0.3962(3) 0.0580(13) Uani 1 1 d . . .
H11 H 0.3291 0.7541 0.4462 0.070 Uiso 1 1 calc R . .
C12 C 0.2553(2) 0.7452(6) 0.3723(2) 0.0469(11) Uani 1 1 d . . .
H12 H 0.2426 0.7390 0.3223 0.056 Uiso 1 1 calc R . .
C13 C 0.2040(2) 0.7426(5) 0.4158(2) 0.0443(10) Uani 1 1 d . A .
C14 C 0.1439(3) 0.7402(12) 0.3844(3) 0.095(2) Uani 1 1 d . . .
H14 H 0.1345 0.7380 0.3340 0.114 Uiso 1 1 calc R . .
C15 C 0.0942(3) 0.7409(12) 0.4220(3) 0.100(3) Uani 1 1 d . A .
H15 H 0.0516 0.7368 0.3967 0.120 Uiso 1 1 calc R . .
C16 C 0.10371(17) 0.7470(5) 0.4940(2) 0.0360(9) Uani 1 1 d . . .
C17 C 0.1655(2) 0.7491(10) 0.5290(3) 0.078(2) Uani 1 1 d . A .
H17 H 0.1747 0.7533 0.5794 0.094 Uiso 1 1 calc R . .
C18 C 0.2155(2) 0.7449(10) 0.4885(4) 0.082(2) Uani 1 1 d . . .
H18 H 0.2585 0.7437 0.5126 0.098 Uiso 1 1 calc R A .
N4 N 0.04932(14) 0.7504(4) 0.52772(18) 0.0346(8) Uani 0.50 1 d P A 1
N5 N 0.0579(3) 0.8156(10) 0.5899(3) 0.0312(14) Uani 0.50 1 d P A 1
N6 N -0.1400(5) 0.8034(12) 0.7505(5) 0.0271(19) Uani 0.50 1 d P A 1
C19 C 0.0062(4) 0.8082(13) 0.6262(4) 0.0271(18) Uani 0.50 1 d P A 1
C20 C -0.0526(7) 0.7173(15) 0.6024(7) 0.033(3) Uani 0.50 1 d P A 1
H20 H -0.0596 0.6552 0.5577 0.040 Uiso 0.50 1 calc PR A 1
C21 C -0.0995(5) 0.7178(13) 0.6431(6) 0.027(2) Uani 0.50 1 d P A 1
H21 H -0.1388 0.6555 0.6258 0.033 Uiso 0.50 1 calc PR A 1
C22 C -0.0918(5) 0.8081(13) 0.7105(6) 0.029(2) Uani 0.50 1 d P A 1
C23 C -0.0325(3) 0.8979(10) 0.7337(4) 0.0284(15) Uani 0.50 1 d P A 1
H23 H -0.0250 0.9597 0.7785 0.034 Uiso 0.50 1 calc PR A 1
C24 C 0.0146(3) 0.8971(10) 0.6924(4) 0.0311(16) Uani 0.50 1 d P A 1
H24 H 0.0540 0.9588 0.7094 0.037 Uiso 0.50 1 calc PR A 1
C25 C -0.1344(4) 0.9158(11) 0.8171(4) 0.0345(16) Uani 0.50 1 d P A 1
H25A H -0.1779 0.9506 0.8248 0.041 Uiso 0.50 1 calc PR A 1
H25B H -0.1112 1.0347 0.8110 0.041 Uiso 0.50 1 calc PR A 1
C26 C -0.1006(5) 0.8154(16) 0.8819(5) 0.038(2) Uani 0.50 1 d PD A 1
H26A H -0.0575 0.7783 0.8739 0.046 Uiso 0.50 1 calc PR A 1
H26B H -0.0953 0.9045 0.9225 0.046 Uiso 0.50 1 calc PR A 1
O2A O -0.1323(8) 0.6557(15) 0.8995(8) 0.064(4) Uani 0.25 1 d PD A 1
C27 C -0.1934(3) 0.6740(11) 0.7356(4) 0.0348(16) Uani 0.50 1 d P A 1
H27A H -0.2067 0.6338 0.7805 0.042 Uiso 0.50 1 calc PR A 1
H27B H -0.1807 0.5598 0.7113 0.042 Uiso 0.50 1 calc PR A 1
C28 C -0.2494(17) 0.773(4) 0.6881(13) 0.052(6) Uani 0.50 1 d PD A 1
H28A H -0.2642 0.8797 0.7139 0.078 Uiso 0.50 1 calc PR A 1
H28B H -0.2845 0.6826 0.6751 0.078 Uiso 0.50 1 calc PR A 1
H28C H -0.2353 0.8197 0.6450 0.078 Uiso 0.50 1 calc PR A 1
N4' N 0.04932(14) 0.7504(4) 0.52772(18) 0.0346(8) Uani 0.50 1 d P A 2
N5' N 0.0580(3) 0.6889(10) 0.5877(3) 0.0317(14) Uani 0.50 1 d P A 2
N6' N -0.1348(5) 0.7194(12) 0.7531(6) 0.032(2) Uani 0.50 1 d P A 2
C19' C 0.0067(4) 0.7046(14) 0.6251(4) 0.0294(18) Uani 0.50 1 d P A 2
C20' C -0.0497(7) 0.8010(16) 0.6025(7) 0.035(3) Uani 0.50 1 d P A 2
H20' H -0.0560 0.8650 0.5582 0.041 Uiso 0.50 1 calc PR A 2
C21' C -0.0970(4) 0.8050(14) 0.6441(5) 0.027(2) Uani 0.50 1 d P A 2
H21' H -0.1359 0.8694 0.6271 0.033 Uiso 0.50 1 calc PR A 2
C22' C -0.0891(5) 0.7160(15) 0.7112(6) 0.031(2) Uani 0.50 1 d P A 2
C23' C -0.0307(3) 0.6191(10) 0.7336(4) 0.0313(15) Uani 0.50 1 d P A 2
H23' H -0.0236 0.5557 0.7781 0.038 Uiso 0.50 1 calc PR A 2
C24' C 0.0157(3) 0.6160(11) 0.6916(4) 0.0343(16) Uani 0.50 1 d P A 2
H24' H 0.0549 0.5523 0.7080 0.041 Uiso 0.50 1 calc PR A 2
C25' C -0.1323(4) 0.6022(11) 0.8169(4) 0.0364(17) Uani 0.50 1 d P A 2
H25C H -0.1100 0.4820 0.8102 0.044 Uiso 0.50 1 calc PR A 2
H25D H -0.1764 0.5707 0.8233 0.044 Uiso 0.50 1 calc PR A 2
C26' C -0.0982(4) 0.7001(17) 0.8830(5) 0.039(2) Uani 0.50 1 d PD A 2
H26C H -0.0906 0.6083 0.9227 0.047 Uiso 0.50 1 calc PR A 2
H26D H -0.0562 0.7473 0.8747 0.047 Uiso 0.50 1 calc PR A 2
O2C O -0.1347(6) 0.8517(14) 0.9011(6) 0.043(3) Uani 0.25 1 d PD A 2
C27' C -0.1907(4) 0.8497(11) 0.7385(4) 0.0393(18) Uani 0.50 1 d P A 2
H27C H -0.1805 0.9546 0.7078 0.047 Uiso 0.50 1 calc PR A 2
H27D H -0.1983 0.9055 0.7838 0.047 Uiso 0.50 1 calc PR A 2
C28' C -0.2537(17) 0.747(4) 0.7010(10) 0.040(5) Uani 0.50 1 d PD A 2
H28D H -0.2470 0.6969 0.6550 0.059 Uiso 0.50 1 calc PR A 2
H28E H -0.2890 0.8382 0.6937 0.059 Uiso 0.50 1 calc PR A 2
H28F H -0.2639 0.6429 0.7310 0.059 Uiso 0.50 1 calc PR A 2
O2D O -0.2449(5) 0.749(2) 0.6305(6) 0.048(4) Uani 0.25 1 d PD B 3
O2B O -0.2874(5) 0.8775(16) 0.7275(7) 0.047(3) Uani 0.25 1 d PD C 3
O3 O 0.3484(3) 0.3306(7) 0.4975(3) 0.1082(17) Uani 1 1 d . . .
C29 C 0.2523(4) 0.2415(17) 0.5318(5) 0.153(5) Uani 1 1 d . . .
H29A H 0.2458 0.1433 0.4950 0.230 Uiso 1 1 calc R . .
H29B H 0.2256 0.3517 0.5159 0.230 Uiso 1 1 calc R . .
H29C H 0.2406 0.1914 0.5757 0.230 Uiso 1 1 calc R . .
C30 C 0.3203(2) 0.2988(7) 0.5452(3) 0.0548(12) Uani 1 1 d . . .
C31 C 0.3480(4) 0.3100(10) 0.6199(4) 0.102(2) Uani 1 1 d . . .
H31A H 0.3944 0.3274 0.6248 0.153 Uiso 1 1 calc R . .
H31B H 0.3390 0.1925 0.6437 0.153 Uiso 1 1 calc R . .
H31C H 0.3294 0.4175 0.6416 0.153 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
O1 0.0336(13) 0.0450(15) 0.0222(12) 0.0000(11) 0.0104(10) 0.0007(12)
N1 0.044(2) 0.051(2) 0.046(2) -0.0076(17) 0.0218(16) -0.0087(17)
N2 0.051(2) 0.071(3) 0.0282(18) -0.0044(17) 0.0085(15) 0.0010(19)
N3 0.041(2) 0.106(4) 0.063(3) -0.005(3) 0.006(2) -0.024(2)
C1 0.0306(18) 0.0238(17) 0.0294(18) 0.0010(14) 0.0096(14) 0.0028(14)
C2 0.0299(18) 0.0244(18) 0.043(2) 0.0031(15) 0.0138(15) -0.0004(14)
C3 0.047(2) 0.0280(19) 0.048(2) 0.0068(16) 0.0279(19) 0.0060(17)
C4 0.046(2) 0.041(2) 0.0289(18) 0.0052(16) 0.0216(16) 0.0029(18)
C5 0.0320(18) 0.0312(19) 0.0242(17) 0.0004(14) 0.0079(14) -0.0001(15)
C6 0.038(2) 0.0329(19) 0.0245(17) -0.0032(15) 0.0147(14) -0.0053(16)
C7 0.042(2) 0.041(2) 0.030(2) 0.0002(16) 0.0133(17) -0.0012(17)
C8 0.032(2) 0.052(3) 0.051(2) 0.002(2) 0.0131(19) -0.0063(19)
C9 0.058(3) 0.046(2) 0.032(2) 0.0025(17) 0.0207(18) -0.002(2)
C10 0.066(3) 0.047(2) 0.034(2) 0.0083(18) 0.0215(19) 0.011(2)
C11 0.053(3) 0.054(3) 0.076(3) 0.008(2) 0.035(3) 0.002(2)
C12 0.055(3) 0.035(2) 0.051(3) -0.0017(19) 0.011(2) -0.0007(19)
C13 0.053(3) 0.028(2) 0.059(3) 0.0014(18) 0.028(2) 0.0031(18)
C14 0.057(3) 0.167(8) 0.071(4) -0.027(4) 0.039(3) -0.016(4)
C15 0.050(3) 0.196(9) 0.060(3) -0.030(4) 0.032(3) -0.019(4)
C16 0.0284(19) 0.0251(18) 0.058(2) -0.0024(17) 0.0177(17) -0.0014(15)
C17 0.033(2) 0.140(6) 0.066(3) 0.020(3) 0.019(2) 0.002(3)
C18 0.020(2) 0.120(5) 0.105(5) 0.019(4) 0.009(2) 0.003(3)
N4 0.0286(16) 0.0305(17) 0.048(2) -0.0039(15) 0.0159(14) -0.0016(13)
N5 0.025(3) 0.025(4) 0.045(4) 0.003(3) 0.010(3) -0.001(3)
N6 0.027(5) 0.021(4) 0.035(4) -0.002(4) 0.011(3) 0.007(4)
C19 0.023(4) 0.020(4) 0.041(4) -0.001(4) 0.011(3) 0.000(4)
C20 0.032(5) 0.031(6) 0.037(5) -0.006(6) 0.009(4) -0.004(6)
C21 0.029(4) 0.009(4) 0.045(5) -0.005(5) 0.011(3) -0.008(4)
C22 0.030(4) 0.021(5) 0.038(5) -0.002(5) 0.007(3) 0.001(5)
C23 0.033(4) 0.021(3) 0.033(4) -0.002(3) 0.008(3) -0.003(3)
C24 0.023(3) 0.024(4) 0.046(4) 0.001(3) 0.006(3) -0.003(3)
C25 0.036(4) 0.029(4) 0.041(4) -0.001(3) 0.012(3) 0.003(3)
C26 0.047(6) 0.026(5) 0.042(5) 0.000(4) 0.008(4) 0.005(5)
O2A 0.077(10) 0.025(7) 0.087(11) 0.001(7) 0.009(9) 0.001(7)
C27 0.037(4) 0.029(4) 0.041(4) -0.004(3) 0.013(3) -0.003(3)
C28 0.030(8) 0.051(9) 0.077(13) 0.029(8) 0.017(8) -0.002(7)
N4' 0.0286(16) 0.0305(17) 0.048(2) -0.0039(15) 0.0159(14) -0.0016(13)
N5' 0.029(3) 0.026(4) 0.043(4) -0.002(3) 0.012(3) -0.001(3)
N6' 0.032(4) 0.028(5) 0.038(4) 0.005(5) 0.009(3) 0.016(5)
C19' 0.029(4) 0.026(5) 0.035(4) -0.001(4) 0.012(3) -0.001(4)
C20' 0.039(6) 0.036(7) 0.030(5) 0.005(6) 0.010(4) -0.002(7)
C21' 0.027(4) 0.017(5) 0.039(5) 0.005(5) 0.007(3) 0.003(4)
C22' 0.029(4) 0.032(5) 0.032(5) -0.002(5) 0.007(3) 0.001(5)
C23' 0.037(4) 0.025(3) 0.034(4) 0.003(3) 0.011(3) 0.003(3)
C24' 0.028(4) 0.028(4) 0.048(4) -0.001(3) 0.009(3) 0.002(3)
C25' 0.035(4) 0.033(4) 0.044(4) -0.002(3) 0.016(3) -0.004(3)
C26' 0.043(5) 0.038(6) 0.037(5) 0.002(4) 0.010(4) -0.014(5)
O2C 0.048(7) 0.027(6) 0.057(7) -0.009(5) 0.022(6) -0.004(5)
C27' 0.046(5) 0.031(4) 0.045(5) 0.006(3) 0.020(4) 0.008(4)
C28' 0.032(7) 0.044(9) 0.047(7) 0.008(7) 0.018(6) -0.004(7)
O2D 0.034(6) 0.092(11) 0.022(6) -0.006(6) 0.016(5) -0.012(6)
O2B 0.036(6) 0.035(6) 0.074(8) -0.018(6) 0.024(6) 0.002(5)
O3 0.136(4) 0.093(3) 0.120(4) 0.018(3) 0.090(3) 0.020(3)
C29 0.104(6) 0.236(13) 0.105(6) 0.032(7) -0.024(5) -0.066(7)
C30 0.065(3) 0.048(3) 0.056(3) -0.001(2) 0.025(2) 0.010(2)
C31 0.136(6) 0.076(4) 0.081(4) -0.005(4) -0.019(4) -0.010(4)

_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 C1 1.323(4) . ?
O1 C4 1.476(4) . ?
N1 C6 1.142(5) . ?
N2 C7 1.147(5) . ?
N3 C8 1.145(6) . ?
C1 C5 1.374(5) . ?
C1 C2 1.441(5) . ?
C2 C3 1.366(5) . ?
C2 C8 1.406(6) . ?
C3 C11 1.439(6) . ?
C3 C4 1.501(6) . ?
C4 C9 1.518(6) . ?
C4 C10 1.526(6) . ?
C5 C7 1.421(5) . ?
C5 C6 1.436(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.288(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.479(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.314(8) . ?
C13 C18 1.370(8) . ?
C14 C15 1.375(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.357(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.367(6) . ?
C16 N4 1.415(5) . ?
C17 C18 1.415(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
N4 N5 1.259(7) . ?
N5 C19 1.396(10) . ?
N6 C22 1.377(14) . ?
N6 C27 1.446(12) . ?
N6 C25 1.487(12) . ?
C19 C24 1.396(11) . ?
C19 C20 1.407(16) . ?
C20 C21 1.365(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.422(16) . ?
C21 H21 0.9500 . ?
C22 C23 1.412(12) . ?
C23 C24 1.375(9) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.499(12) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 O2A 1.382(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.54(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N5' C19' 1.405(10) . ?
N6' C22' 1.359(14) . ?
N6' C25' 1.467(12) . ?
N6' C27' 1.488(10) . ?
C19' C20' 1.380(17) . ?
C19' C24' 1.400(11) . ?
C20' C21' 1.383(16) . ?
C20' H20' 0.9500 . ?
C21' C22' 1.412(15) . ?
C21' H21' 0.9500 . ?
C22' C23' 1.418(12) . ?
C23' C24' 1.373(10) . ?
C23' H23' 0.9500 . ?
C24' H24' 0.9500 . ?
C25' C26' 1.512(12) . ?
C25' H25C 0.9900 . ?
C25' H25D 0.9900 . ?
C26' O2C 1.399(9) . ?
C26' H26C 0.9900 . ?
C26' H26D 0.9900 . ?
C27' C28' 1.58(4) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' H28D 0.9800 . ?
C28' H28E 0.9800 . ?
C28' H28F 0.9800 . ?
O3 C30 1.192(6) . ?
C29 C30 1.478(9) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.451(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C4 110.1(3) . . ?
O1 C1 C5 118.9(3) . . ?
O1 C1 C2 110.3(3) . . ?
C5 C1 C2 130.8(3) . . ?
C3 C2 C8 127.0(4) . . ?
C3 C2 C1 108.1(3) . . ?
C8 C2 C1 125.0(3) . . ?
C2 C3 C11 134.7(4) . . ?
C2 C3 C4 108.7(3) . . ?
C11 C3 C4 116.5(4) . . ?
O1 C4 C3 102.7(3) . . ?
O1 C4 C9 107.7(3) . . ?
C3 C4 C9 112.2(3) . . ?
O1 C4 C10 106.1(3) . . ?
C3 C4 C10 113.5(3) . . ?
C9 C4 C10 113.7(3) . . ?
C1 C5 C7 123.0(3) . . ?
C1 C5 C6 118.8(3) . . ?
C7 C5 C6 118.1(3) . . ?
N1 C6 C5 179.4(4) . . ?
N2 C7 C5 178.5(4) . . ?
N3 C8 C2 178.7(5) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C3 124.8(5) . . ?
C12 C11 H11 117.6 . . ?
C3 C11 H11 117.6 . . ?
C11 C12 C13 126.0(5) . . ?
C11 C12 H12 117.0 . . ?
C13 C12 H12 117.0 . . ?
C14 C13 C18 117.1(4) . . ?
C14 C13 C12 119.6(5) . . ?
C18 C13 C12 123.3(4) . . ?
C13 C14 C15 122.2(6) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 122.3(6) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C15 C16 C17 117.5(4) . . ?
C15 C16 N4 118.0(4) . . ?
C17 C16 N4 124.5(4) . . ?
C16 C17 C18 118.6(5) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C13 C18 C17 122.3(5) . . ?
C13 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
N5 N4 C16 116.0(4) . . ?
N4 N5 C19 117.2(6) . . ?
C22 N6 C27 122.5(8) . . ?
C22 N6 C25 120.2(8) . . ?
C27 N6 C25 116.8(8) . . ?
N5 C19 C24 116.3(7) . . ?
N5 C19 C20 125.8(9) . . ?
C24 C19 C20 117.9(8) . . ?
C21 C20 C19 120.5(11) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 122.3(10) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
N6 C22 C23 122.9(9) . . ?
N6 C22 C21 120.6(9) . . ?
C23 C22 C21 116.5(9) . . ?
C24 C23 C22 121.0(7) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C19 121.9(7) . . ?
C23 C24 H24 119.1 . . ?
C19 C24 H24 119.1 . . ?
N6 C25 C26 114.4(7) . . ?
N6 C25 H25A 108.7 . . ?
C26 C25 H25A 108.7 . . ?
N6 C25 H25B 108.7 . . ?
C26 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
O2A C26 C25 113.7(9) . . ?
O2A C26 H26A 108.8 . . ?
C25 C26 H26A 108.8 . . ?
O2A C26 H26B 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
N6 C27 C28 109.4(15) . . ?
N6 C27 H27A 109.8 . . ?
C28 C27 H27A 109.8 . . ?
N6 C27 H27B 109.8 . . ?
C28 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
C22' N6' C25' 123.4(8) . . ?
C22' N6' C27' 121.7(9) . . ?
C25' N6' C27' 114.8(8) . . ?
C20' C19' C24' 118.8(8) . . ?
C20' C19' N5' 125.9(9) . . ?
C24' C19' N5' 115.3(7) . . ?
C19' C20' C21' 120.4(10) . . ?
C19' C20' H20' 119.8 . . ?
C21' C20' H20' 119.8 . . ?
C20' C21' C22' 121.9(9) . . ?
C20' C21' H21' 119.1 . . ?
C22' C21' H21' 119.1 . . ?
N6' C22' C21' 122.8(9) . . ?
N6' C22' C23' 120.4(9) . . ?
C21' C22' C23' 116.8(8) . . ?
C24' C23' C22' 120.6(7) . . ?
C24' C23' H23' 119.7 . . ?
C22' C23' H23' 119.7 . . ?
C23' C24' C19' 121.5(7) . . ?
C23' C24' H24' 119.2 . . ?
C19' C24' H24' 119.2 . . ?
N6' C25' C26' 112.5(8) . . ?
N6' C25' H25C 109.1 . . ?
C26' C25' H25C 109.1 . . ?
N6' C25' H25D 109.1 . . ?
C26' C25' H25D 109.1 . . ?
H25C C25' H25D 107.8 . . ?
O2C C26' C25' 110.4(8) . . ?
O2C C26' H26C 109.6 . . ?
C25' C26' H26C 109.6 . . ?
O2C C26' H26D 109.6 . . ?
C25' C26' H26D 109.6 . . ?
H26C C26' H26D 108.1 . . ?
N6' C27' C28' 112.8(11) . . ?
N6' C27' H27C 109.0 . . ?
C28' C27' H27C 109.0 . . ?
N6' C27' H27D 109.0 . . ?
C28' C27' H27D 109.0 . . ?
H27C C27' H27D 107.8 . . ?
C27' C28' H28D 109.5 . . ?
C27' C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C27' C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O3 C30 C31 124.7(6) . . ?
O3 C30 C29 121.3(6) . . ?
C31 C30 C29 114.0(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.064


# Attachment '2.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 693973'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 N4 O2'
_chemical_formula_weight         476.56

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

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

_cell_length_a                   8.0729(7)
_cell_length_b                   12.3815(11)
_cell_length_c                   14.1342(13)
_cell_angle_alpha                67.973(2)
_cell_angle_beta                 88.486(2)
_cell_angle_gamma                83.183(2)
_cell_volume                     1300.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             504
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9770
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      292(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            8911
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4538
_reflns_number_gt                2710
_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 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^)+(0.1038P)^2^+0.0640P] 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         4538
_refine_ls_number_parameters     338
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.2009
_refine_ls_wR_factor_gt          0.1680
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.033
_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 1.0607(4) 0.6996(3) 0.0442(2) 0.0610(9) Uani 1 1 d . . .
C2 C 0.9323(3) 0.6397(2) 0.0244(2) 0.0489(7) Uani 1 1 d . . .
C3 C 0.9012(3) 0.6597(2) -0.0791(3) 0.0540(8) Uani 1 1 d . . .
C4 C 0.8400(3) 0.5713(2) 0.1009(2) 0.0430(6) Uani 1 1 d . . .
C5 C 0.9735(4) 0.5647(3) 0.2643(2) 0.0678(9) Uani 1 1 d . . .
C6 C 0.8493(3) 0.5386(2) 0.2088(2) 0.0477(7) Uani 1 1 d . . .
C7 C 0.7205(3) 0.4751(2) 0.2536(2) 0.0449(7) Uani 1 1 d . . .
C8 C 0.6233(3) 0.4616(2) 0.16914(19) 0.0452(7) Uani 1 1 d . . .
C9 C 0.4470(3) 0.5239(3) 0.1520(2) 0.0611(8) Uani 1 1 d . . .
H9A H 0.4485 0.6031 0.1473 0.092 Uiso 1 1 calc R . .
H9B H 0.3792 0.4836 0.2080 0.092 Uiso 1 1 calc R . .
H9C H 0.4017 0.5244 0.0897 0.092 Uiso 1 1 calc R . .
C10 C 0.6337(4) 0.3358(3) 0.1771(2) 0.0661(9) Uani 1 1 d . . .
H10A H 0.5877 0.3336 0.1160 0.099 Uiso 1 1 calc R . .
H10B H 0.5717 0.2919 0.2348 0.099 Uiso 1 1 calc R . .
H10C H 0.7483 0.3020 0.1855 0.099 Uiso 1 1 calc R . .
C11 C 0.6872(4) 0.4308(3) 0.3594(2) 0.0533(8) Uani 1 1 d . . .
H11 H 0.7668 0.4363 0.4032 0.064 Uiso 1 1 calc R . .
C12 C 0.5502(4) 0.3812(3) 0.4018(2) 0.0547(8) Uani 1 1 d . . .
H12 H 0.4732 0.3748 0.3570 0.066 Uiso 1 1 calc R . .
C13 C 0.5083(4) 0.3372(2) 0.5076(2) 0.0532(7) Uani 1 1 d . . .
C14 C 0.6185(4) 0.3217(3) 0.5879(2) 0.0587(8) Uani 1 1 d . . .
H14 H 0.7256 0.3433 0.5736 0.070 Uiso 1 1 calc R . .
C15 C 0.3474(4) 0.3059(3) 0.5345(2) 0.0659(9) Uani 1 1 d . . .
H15 H 0.2709 0.3157 0.4830 0.079 Uiso 1 1 calc R . .
C16 C 0.5692(4) 0.2744(3) 0.6886(2) 0.0642(9) Uani 1 1 d . . .
H16 H 0.6445 0.2639 0.7409 0.077 Uiso 1 1 calc R . .
C17 C 0.2993(4) 0.2614(3) 0.6335(2) 0.0671(9) Uani 1 1 d . . .
H17 H 0.1904 0.2437 0.6478 0.081 Uiso 1 1 calc R . .
C18 C 0.4085(4) 0.2421(3) 0.7131(2) 0.0590(8) Uani 1 1 d . . .
C19 C 0.3486(5) 0.1915(3) 0.8180(3) 0.0715(9) Uani 1 1 d . . .
H19 H 0.2382 0.1757 0.8249 0.086 Uiso 1 1 calc R . .
C20 C 0.4330(4) 0.1665(3) 0.9020(3) 0.0642(9) Uani 1 1 d . . .
H20 H 0.5434 0.1823 0.8953 0.077 Uiso 1 1 calc R . .
C21 C 0.3720(4) 0.1156(2) 1.0069(2) 0.0546(8) Uani 1 1 d . . .
C22 C 0.4635(4) 0.1180(3) 1.0865(2) 0.0562(8) Uani 1 1 d . . .
H22 H 0.5657 0.1478 1.0732 0.067 Uiso 1 1 calc R . .
C23 C 0.2249(4) 0.0637(3) 1.0319(2) 0.0622(8) Uani 1 1 d . . .
H23 H 0.1626 0.0568 0.9805 0.075 Uiso 1 1 calc R . .
C24 C 0.4095(4) 0.0783(3) 1.1834(2) 0.0557(8) Uani 1 1 d . . .
H24 H 0.4749 0.0836 1.2344 0.067 Uiso 1 1 calc R . .
C25 C 0.1684(4) 0.0218(3) 1.1316(2) 0.0574(8) Uani 1 1 d . . .
H25 H 0.0689 -0.0116 1.1455 0.069 Uiso 1 1 calc R . .
C26 C 0.2590(3) 0.0294(2) 1.2104(2) 0.0460(7) Uani 1 1 d . A .
C27 C 0.0452(4) -0.0569(3) 1.3337(3) 0.0695(9) Uani 1 1 d . A .
H27A H 0.0438 -0.1029 1.4063 0.083 Uiso 1 1 calc R . .
H27B H 0.0382 -0.1097 1.2980 0.083 Uiso 1 1 calc R . .
C28 C -0.1070(4) 0.0344(4) 1.3050(3) 0.1003(13) Uani 1 1 d . . .
H28A H -0.1009 0.0874 1.3396 0.151 Uiso 1 1 calc R . .
H28B H -0.2061 -0.0038 1.3247 0.151 Uiso 1 1 calc R . .
H28C H -0.1101 0.0775 1.2326 0.151 Uiso 1 1 calc R . .
C29 C 0.3043(4) -0.0103(3) 1.3934(2) 0.0704(9) Uani 1 1 d . A .
H29A H 0.4206 -0.0242 1.3775 0.084 Uiso 1 1 calc R . .
H29B H 0.2805 -0.0762 1.4540 0.084 Uiso 1 1 calc R . .
C30 C 0.2808(7) 0.0967(4) 1.4171(4) 0.1006(13) Uani 1 1 d D . .
H30A H 0.1652 0.1067 1.4359 0.121 Uiso 0.619(8) 1 calc PR A 1
H30B H 0.3481 0.0810 1.4777 0.121 Uiso 0.619(8) 1 calc PR A 1
H30C H 0.3027 0.0711 1.4900 0.121 Uiso 0.381(8) 1 d PR A 2
H30D H 0.3662 0.1437 1.3828 0.121 Uiso 0.381(8) 1 d PR A 2
N1 N 1.1608(4) 0.7503(3) 0.0569(3) 0.0925(10) Uani 1 1 d . . .
N2 N 0.8803(3) 0.6740(2) -0.1639(2) 0.0753(8) Uani 1 1 d . . .
N3 N 1.0713(4) 0.5811(4) 0.3119(3) 0.1143(13) Uani 1 1 d . . .
N4 N 0.2023(3) -0.0072(2) 1.30970(17) 0.0555(6) Uani 1 1 d . . .
O1 O 0.7150(2) 0.52471(16) 0.07677(13) 0.0509(5) Uani 1 1 d . . .
O2 O 0.3140(5) 0.1993(4) 1.3494(3) 0.087(2) Uani 0.619(8) 1 d PD A 1
H2 H 0.3045 0.1998 1.2916 0.130 Uiso 0.619(8) 1 calc PR A 1
O2' O 0.1332(10) 0.1746(8) 1.3976(6) 0.119(4) Uani 0.381(8) 1 d PD A 2
H2' H 0.1112 0.2014 1.3362 0.179 Uiso 0.381(8) 1 calc PR A 2

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 0.0448(17) 0.053(2) 0.072(2) -0.0088(16) 0.0038(15) -0.0082(15)
C2 0.0408(15) 0.0459(17) 0.0523(17) -0.0107(13) 0.0074(13) -0.0028(13)
C3 0.0545(18) 0.0410(18) 0.056(2) -0.0077(15) 0.0108(15) -0.0035(13)
C4 0.0402(14) 0.0387(16) 0.0486(16) -0.0149(13) 0.0045(12) -0.0046(12)
C5 0.0543(19) 0.091(3) 0.062(2) -0.0290(18) 0.0058(16) -0.0221(18)
C6 0.0443(15) 0.0496(18) 0.0486(17) -0.0174(13) 0.0011(12) -0.0063(13)
C7 0.0434(15) 0.0453(16) 0.0453(16) -0.0174(13) 0.0031(12) -0.0019(13)
C8 0.0492(16) 0.0467(17) 0.0402(15) -0.0149(12) 0.0089(12) -0.0140(13)
C9 0.0538(18) 0.073(2) 0.0570(19) -0.0227(16) -0.0031(14) -0.0136(16)
C10 0.086(2) 0.056(2) 0.063(2) -0.0264(16) 0.0198(16) -0.0245(17)
C11 0.0558(18) 0.0587(19) 0.0445(17) -0.0175(14) -0.0019(13) -0.0089(15)
C12 0.0640(19) 0.059(2) 0.0430(16) -0.0191(14) 0.0037(14) -0.0170(15)
C13 0.070(2) 0.0480(18) 0.0438(17) -0.0180(13) 0.0053(14) -0.0145(15)
C14 0.0670(19) 0.060(2) 0.0491(18) -0.0200(15) 0.0052(15) -0.0090(16)
C15 0.075(2) 0.078(2) 0.0537(19) -0.0285(17) 0.0141(16) -0.0315(18)
C16 0.087(2) 0.056(2) 0.0475(18) -0.0193(15) -0.0088(16) 0.0007(17)
C17 0.079(2) 0.075(2) 0.054(2) -0.0255(17) 0.0177(17) -0.0324(18)
C18 0.082(2) 0.0438(18) 0.0508(19) -0.0163(14) 0.0223(16) -0.0172(16)
C19 0.083(2) 0.063(2) 0.073(2) -0.0307(18) 0.0068(19) -0.0084(18)
C20 0.073(2) 0.0473(19) 0.073(2) -0.0253(16) 0.0017(17) 0.0016(16)
C21 0.068(2) 0.0387(17) 0.0512(18) -0.0112(13) 0.0186(15) -0.0064(14)
C22 0.0613(19) 0.057(2) 0.0551(19) -0.0256(15) 0.0158(15) -0.0115(15)
C23 0.085(2) 0.058(2) 0.0452(18) -0.0236(15) -0.0119(16) 0.0034(17)
C24 0.0596(18) 0.059(2) 0.0547(19) -0.0277(15) 0.0029(14) -0.0105(15)
C25 0.0615(18) 0.059(2) 0.0539(19) -0.0223(15) 0.0006(15) -0.0129(15)
C26 0.0534(17) 0.0405(16) 0.0442(16) -0.0164(13) 0.0053(13) -0.0047(13)
C27 0.072(2) 0.068(2) 0.060(2) -0.0127(16) 0.0189(16) -0.0170(18)
C28 0.064(2) 0.110(3) 0.112(3) -0.027(3) 0.011(2) -0.002(2)
C29 0.090(2) 0.076(3) 0.0416(17) -0.0163(16) -0.0008(16) -0.0140(19)
C30 0.118(4) 0.111(4) 0.089(3) -0.056(3) -0.015(3) -0.007(3)
N1 0.0566(17) 0.081(2) 0.127(3) -0.0193(19) -0.0103(17) -0.0227(16)
N2 0.083(2) 0.072(2) 0.0565(19) -0.0098(15) 0.0099(15) -0.0027(15)
N3 0.083(2) 0.190(4) 0.090(2) -0.063(2) -0.0041(18) -0.055(2)
N4 0.0633(15) 0.0606(16) 0.0412(14) -0.0159(11) 0.0093(11) -0.0145(12)
O1 0.0578(12) 0.0543(12) 0.0421(11) -0.0156(9) 0.0072(9) -0.0216(10)
O2 0.111(4) 0.097(4) 0.061(3) -0.034(3) -0.003(2) -0.033(3)
O2' 0.146(9) 0.131(8) 0.101(6) -0.072(5) 0.003(5) 0.003(6)

_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 1.136(4) . ?
C1 C2 1.434(4) . ?
C2 C4 1.364(4) . ?
C2 C3 1.414(4) . ?
C3 N2 1.157(4) . ?
C4 O1 1.331(3) . ?
C4 C6 1.426(4) . ?
C5 N3 1.134(4) . ?
C5 C6 1.425(4) . ?
C6 C7 1.373(4) . ?
C7 C11 1.416(4) . ?
C7 C8 1.517(4) . ?
C8 O1 1.478(3) . ?
C8 C10 1.511(4) . ?
C8 C9 1.515(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.345(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.433(4) . ?
C12 H12 0.9300 . ?
C13 C15 1.402(4) . ?
C13 C14 1.402(4) . ?
C14 C16 1.388(4) . ?
C14 H14 0.9300 . ?
C15 C17 1.363(4) . ?
C15 H15 0.9300 . ?
C16 C18 1.399(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.378(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.470(4) . ?
C19 C20 1.299(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.474(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.373(4) . ?
C21 C23 1.391(4) . ?
C22 C24 1.350(4) . ?
C22 H22 0.9300 . ?
C23 C25 1.392(4) . ?
C23 H23 0.9300 . ?
C24 C26 1.402(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.386(4) . ?
C25 H25 0.9300 . ?
C26 N4 1.387(3) . ?
C27 N4 1.452(4) . ?
C27 C28 1.518(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 N4 1.445(4) . ?
C29 C30 1.474(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O2 1.326(5) . ?
C30 O2' 1.404(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 H30C 0.9720 . ?
C30 H30D 0.9566 . ?
O2 H30D 0.7571 . ?
O2 H2 0.8200 . ?
O2' H2' 0.8200 . ?

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 177.7(3) . . ?
C4 C2 C3 121.7(3) . . ?
C4 C2 C1 121.9(3) . . ?
C3 C2 C1 116.4(2) . . ?
N2 C3 C2 177.9(3) . . ?
O1 C4 C2 118.9(2) . . ?
O1 C4 C6 109.7(2) . . ?
C2 C4 C6 131.4(2) . . ?
N3 C5 C6 177.0(4) . . ?
C7 C6 C5 123.9(3) . . ?
C7 C6 C4 109.8(2) . . ?
C5 C6 C4 126.3(2) . . ?
C6 C7 C11 125.7(3) . . ?
C6 C7 C8 107.2(2) . . ?
C11 C7 C8 127.1(2) . . ?
O1 C8 C10 106.5(2) . . ?
O1 C8 C9 105.6(2) . . ?
C10 C8 C9 113.3(2) . . ?
O1 C8 C7 102.77(19) . . ?
C10 C8 C7 112.8(2) . . ?
C9 C8 C7 114.5(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 125.6(3) . . ?
C12 C11 H11 117.2 . . ?
C7 C11 H11 117.2 . . ?
C11 C12 C13 128.0(3) . . ?
C11 C12 H12 116.0 . . ?
C13 C12 H12 116.0 . . ?
C15 C13 C14 116.7(3) . . ?
C15 C13 C12 118.8(3) . . ?
C14 C13 C12 124.5(3) . . ?
C16 C14 C13 120.6(3) . . ?
C16 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C17 C15 C13 122.2(3) . . ?
C17 C15 H15 118.9 . . ?
C13 C15 H15 118.9 . . ?
C14 C16 C18 121.4(3) . . ?
C14 C16 H16 119.3 . . ?
C18 C16 H16 119.3 . . ?
C15 C17 C18 121.5(3) . . ?
C15 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C16 117.6(3) . . ?
C17 C18 C19 118.3(3) . . ?
C16 C18 C19 124.0(3) . . ?
C20 C19 C18 127.1(4) . . ?
C20 C19 H19 116.4 . . ?
C18 C19 H19 116.4 . . ?
C19 C20 C21 126.8(3) . . ?
C19 C20 H20 116.6 . . ?
C21 C20 H20 116.6 . . ?
C22 C21 C23 116.6(3) . . ?
C22 C21 C20 119.4(3) . . ?
C23 C21 C20 124.0(3) . . ?
C24 C22 C21 122.0(3) . . ?
C24 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C21 C23 C25 122.0(3) . . ?
C21 C23 H23 119.0 . . ?
C25 C23 H23 119.0 . . ?
C22 C24 C26 122.6(3) . . ?
C22 C24 H24 118.7 . . ?
C26 C24 H24 118.7 . . ?
C26 C25 C23 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C23 C25 H25 119.7 . . ?
C25 C26 N4 121.9(3) . . ?
C25 C26 C24 116.1(3) . . ?
N4 C26 C24 122.0(3) . . ?
N4 C27 C28 113.6(3) . . ?
N4 C27 H27A 108.8 . . ?
C28 C27 H27A 108.8 . . ?
N4 C27 H27B 108.8 . . ?
C28 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 C30 115.1(3) . . ?
N4 C29 H29A 108.5 . . ?
C30 C29 H29A 108.5 . . ?
N4 C29 H29B 108.5 . . ?
C30 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
O2 C30 O2' 72.1(5) . . ?
O2 C30 C29 121.4(4) . . ?
O2' C30 C29 124.7(5) . . ?
O2 C30 H30A 107.0 . . ?
O2' C30 H30A 35.0 . . ?
C29 C30 H30A 107.0 . . ?
O2 C30 H30B 107.0 . . ?
O2' C30 H30B 120.0 . . ?
C29 C30 H30B 107.0 . . ?
H30A C30 H30B 106.7 . . ?
O2 C30 H30C 123.8 . . ?
O2' C30 H30C 105.4 . . ?
C29 C30 H30C 106.1 . . ?
H30A C30 H30C 84.0 . . ?
H30B C30 H30C 24.5 . . ?
O2 C30 H30D 34.1 . . ?
O2' C30 H30D 105.4 . . ?
C29 C30 H30D 107.0 . . ?
H30A C30 H30D 139.2 . . ?
H30B C30 H30D 84.0 . . ?
H30C C30 H30D 107.3 . . ?
C26 N4 C29 121.7(2) . . ?
C26 N4 C27 119.9(2) . . ?
C29 N4 C27 118.0(2) . . ?
C4 O1 C8 110.44(19) . . ?
C30 O2 H30D 45.2 . . ?
C30 O2 H2 109.5 . . ?
H30D O2 H2 110.1 . . ?
C30 O2' H2' 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
N1 C1 C2 C4 -141(9) . . . . ?
N1 C1 C2 C3 36(9) . . . . ?
C4 C2 C3 N2 -111(9) . . . . ?
C1 C2 C3 N2 72(9) . . . . ?
C3 C2 C4 O1 -1.7(4) . . . . ?
C1 C2 C4 O1 175.3(2) . . . . ?
C3 C2 C4 C6 179.5(3) . . . . ?
C1 C2 C4 C6 -3.6(5) . . . . ?
N3 C5 C6 C7 29(8) . . . . ?
N3 C5 C6 C4 -150(7) . . . . ?
O1 C4 C6 C7 -3.5(3) . . . . ?
C2 C4 C6 C7 175.4(3) . . . . ?
O1 C4 C6 C5 175.5(3) . . . . ?
C2 C4 C6 C5 -5.6(5) . . . . ?
C5 C6 C7 C11 2.8(5) . . . . ?
C4 C6 C7 C11 -178.2(2) . . . . ?
C5 C6 C7 C8 -176.9(3) . . . . ?
C4 C6 C7 C8 2.1(3) . . . . ?
C6 C7 C8 O1 -0.2(3) . . . . ?
C11 C7 C8 O1 -179.8(2) . . . . ?
C6 C7 C8 C10 114.2(3) . . . . ?
C11 C7 C8 C10 -65.5(3) . . . . ?
C6 C7 C8 C9 -114.1(3) . . . . ?
C11 C7 C8 C9 66.2(4) . . . . ?
C6 C7 C11 C12 171.4(3) . . . . ?
C8 C7 C11 C12 -9.0(5) . . . . ?
C7 C11 C12 C13 -178.6(3) . . . . ?
C11 C12 C13 C15 170.0(3) . . . . ?
C11 C12 C13 C14 -10.7(5) . . . . ?
C15 C13 C14 C16 1.7(4) . . . . ?
C12 C13 C14 C16 -177.6(3) . . . . ?
C14 C13 C15 C17 -0.6(5) . . . . ?
C12 C13 C15 C17 178.8(3) . . . . ?
C13 C14 C16 C18 -0.8(5) . . . . ?
C13 C15 C17 C18 -1.7(5) . . . . ?
C15 C17 C18 C16 2.6(5) . . . . ?
C15 C17 C18 C19 -178.6(3) . . . . ?
C14 C16 C18 C17 -1.4(5) . . . . ?
C14 C16 C18 C19 179.9(3) . . . . ?
C17 C18 C19 C20 179.5(3) . . . . ?
C16 C18 C19 C20 -1.9(5) . . . . ?
C18 C19 C20 C21 -179.9(3) . . . . ?
C19 C20 C21 C22 -165.8(3) . . . . ?
C19 C20 C21 C23 14.3(5) . . . . ?
C23 C21 C22 C24 -3.7(4) . . . . ?
C20 C21 C22 C24 176.5(3) . . . . ?
C22 C21 C23 C25 3.3(4) . . . . ?
C20 C21 C23 C25 -176.9(3) . . . . ?
C21 C22 C24 C26 1.6(5) . . . . ?
C21 C23 C25 C26 -0.7(5) . . . . ?
C23 C25 C26 N4 177.3(3) . . . . ?
C23 C25 C26 C24 -1.5(4) . . . . ?
C22 C24 C26 C25 1.1(4) . . . . ?
C22 C24 C26 N4 -177.7(3) . . . . ?
N4 C29 C30 O2 -62.0(6) . . . . ?
N4 C29 C30 O2' 27.1(7) . . . . ?
C25 C26 N4 C29 173.7(3) . . . . ?
C24 C26 N4 C29 -7.6(4) . . . . ?
C25 C26 N4 C27 1.0(4) . . . . ?
C24 C26 N4 C27 179.8(3) . . . . ?
C30 C29 N4 C26 92.5(4) . . . . ?
C30 C29 N4 C27 -94.7(4) . . . . ?
C28 C27 N4 C26 -79.3(4) . . . . ?
C28 C27 N4 C29 107.8(3) . . . . ?
C2 C4 O1 C8 -175.7(2) . . . . ?
C6 C4 O1 C8 3.4(3) . . . . ?
C10 C8 O1 C4 -120.9(2) . . . . ?
C9 C8 O1 C4 118.3(2) . . . . ?
C7 C8 O1 C4 -2.0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 N2 0.82 2.32 2.888(5) 126.6 2_666
O2' H2' N2 0.82 2.35 3.125(9) 158.2 2_666
C20 H20 N1 0.93 2.80 3.675(4) 157.3 2_766
C14 H14 N3 0.93 2.80 3.450(4) 128.2 2_766

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.043