# Supplementary Information (SI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

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

data_230305b
_database_code_depnum_ccdc_archive 'CCDC 2251334'
loop_
_audit_author_name
_audit_author_address
'wang man'
;University
China
;
_audit_update_record             
;
2023-03-24 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H17 N O2'
_chemical_formula_weight         303.35

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                   7.5526(9)
_cell_length_b                   10.6072(14)
_cell_length_c                   10.6696(14)
_cell_angle_alpha                77.765(3)
_cell_angle_beta                 84.820(4)
_cell_angle_gamma                69.886(2)
_cell_volume                     784.26(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    938
_cell_measurement_theta_min      2.567
_cell_measurement_theta_max      24.234

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             320
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9755
_exptl_absorpt_correction_T_max  0.9967
_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  '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            3795
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2685
_reflns_number_gt                1675
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1333P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2685
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0785
_refine_ls_wR_factor_ref         0.2228
_refine_ls_wR_factor_gt          0.1980
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.970
_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
N1 N 0.6954(4) -0.0438(3) 1.1458(2) 0.0414(7) Uani 1 1 d . . .
H1 H 0.6624 -0.0569 1.2254 0.050 Uiso 1 1 calc R . .
O1 O 0.6015(4) 0.1633(2) 1.3102(2) 0.0564(7) Uani 1 1 d . . .
O2 O 0.5855(4) 0.3819(3) 1.2179(3) 0.0641(8) Uani 1 1 d . . .
C1 C 0.6212(5) 0.2619(4) 1.2074(3) 0.0463(9) Uani 1 1 d . . .
C2 C 0.7115(4) 0.0759(3) 1.0751(3) 0.0374(8) Uani 1 1 d . . .
C3 C 0.7423(5) -0.1427(3) 1.0661(3) 0.0391(8) Uani 1 1 d . . .
C4 C 0.7434(5) -0.2779(3) 1.1041(3) 0.0441(9) Uani 1 1 d . . .
C5 C 0.7871(5) -0.3549(4) 1.0072(3) 0.0502(9) Uani 1 1 d . . .
H5 H 0.7928 -0.4458 1.0276 0.060 Uiso 1 1 calc R . .
C6 C 0.8225(5) -0.2990(4) 0.8808(4) 0.0537(10) Uani 1 1 d . . .
H6 H 0.8460 -0.3526 0.8185 0.064 Uiso 1 1 calc R . .
C7 C 0.8234(5) -0.1644(3) 0.8453(3) 0.0473(9) Uani 1 1 d . . .
H7 H 0.8506 -0.1295 0.7611 0.057 Uiso 1 1 calc R . .
C8 C 0.7823(5) -0.0828(3) 0.9393(3) 0.0406(8) Uani 1 1 d . . .
C9 C 0.7665(4) 0.0600(3) 0.9434(3) 0.0362(8) Uani 1 1 d . . .
C10 C 0.7806(4) 0.1819(3) 0.8735(3) 0.0403(8) Uani 1 1 d . . .
C11 C 0.7274(5) 0.2850(3) 0.9644(3) 0.0446(9) Uani 1 1 d . . .
H11A H 0.8306 0.3181 0.9702 0.053 Uiso 1 1 calc R . .
H11B H 0.6168 0.3624 0.9344 0.053 Uiso 1 1 calc R . .
C12 C 0.6875(5) 0.2061(3) 1.0931(3) 0.0406(8) Uani 1 1 d . . .
C13 C 0.7082(6) -0.3360(4) 1.2424(3) 0.0551(10) Uani 1 1 d . . .
H13A H 0.7063 -0.4272 1.2493 0.083 Uiso 1 1 calc R . .
H13B H 0.5891 -0.2796 1.2715 0.083 Uiso 1 1 calc R . .
H13C H 0.8070 -0.3380 1.2943 0.083 Uiso 1 1 calc R . .
C14 C 0.8361(5) 0.2195(3) 0.7387(3) 0.0416(8) Uani 1 1 d . . .
C15 C 0.9545(5) 0.1217(4) 0.6693(3) 0.0463(9) Uani 1 1 d . . .
H15 H 0.9962 0.0298 0.7087 0.056 Uiso 1 1 calc R . .
C16 C 1.0098(6) 0.1596(4) 0.5437(3) 0.0574(10) Uani 1 1 d . . .
H16 H 1.0886 0.0932 0.5003 0.069 Uiso 1 1 calc R . .
C17 C 0.9485(6) 0.2965(4) 0.4819(4) 0.0664(12) Uani 1 1 d . . .
H17 H 0.9847 0.3216 0.3972 0.080 Uiso 1 1 calc R . .
C18 C 0.8328(6) 0.3948(4) 0.5482(4) 0.0619(11) Uani 1 1 d . . .
H18 H 0.7916 0.4864 0.5078 0.074 Uiso 1 1 calc R . .
C19 C 0.7784(5) 0.3575(4) 0.6741(3) 0.0531(10) Uani 1 1 d . . .
H19 H 0.7019 0.4250 0.7172 0.064 Uiso 1 1 calc R . .
C20 C 0.5204(7) 0.2108(5) 1.4270(4) 0.0705(12) Uani 1 1 d . . .
H20A H 0.5780 0.2731 1.4441 0.106 Uiso 1 1 calc R . .
H20B H 0.5424 0.1341 1.4972 0.106 Uiso 1 1 calc R . .
H20C H 0.3871 0.2568 1.4172 0.106 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C2 1.371(4) . ?
N1 C3 1.420(4) . ?
N1 H1 0.8600 . ?
O1 C1 1.383(4) . ?
O1 C20 1.449(4) . ?
O2 C1 1.235(4) . ?
C1 C12 1.442(5) . ?
C2 C12 1.382(4) . ?
C2 C9 1.457(5) . ?
C3 C4 1.403(5) . ?
C3 C8 1.421(4) . ?
C4 C5 1.398(5) . ?
C4 C13 1.511(5) . ?
C5 C6 1.395(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.400(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.407(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.487(4) . ?
C9 C10 1.383(4) . ?
C10 C14 1.472(4) . ?
C10 C11 1.541(4) . ?
C11 C12 1.513(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.411(5) . ?
C14 C19 1.413(5) . ?
C15 C16 1.385(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.388(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.385(5) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 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
C2 N1 C3 108.9(3) . . ?
C2 N1 H1 125.5 . . ?
C3 N1 H1 125.5 . . ?
C1 O1 C20 116.4(3) . . ?
O2 C1 O1 121.5(3) . . ?
O2 C1 C12 126.5(3) . . ?
O1 C1 C12 111.9(3) . . ?
N1 C2 C12 138.1(3) . . ?
N1 C2 C9 109.7(3) . . ?
C12 C2 C9 112.1(3) . . ?
C4 C3 N1 125.8(3) . . ?
C4 C3 C8 124.5(3) . . ?
N1 C3 C8 109.7(3) . . ?
C5 C4 C3 115.5(3) . . ?
C5 C4 C13 123.2(3) . . ?
C3 C4 C13 121.2(3) . . ?
C6 C5 C4 121.9(3) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C7 121.7(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 118.8(3) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C3 117.6(3) . . ?
C7 C8 C9 136.3(3) . . ?
C3 C8 C9 106.1(3) . . ?
C10 C9 C2 108.9(3) . . ?
C10 C9 C8 145.6(3) . . ?
C2 C9 C8 105.5(3) . . ?
C9 C10 C14 131.0(3) . . ?
C9 C10 C11 107.4(3) . . ?
C14 C10 C11 121.6(3) . . ?
C12 C11 C10 105.2(3) . . ?
C12 C11 H11A 110.7 . . ?
C10 C11 H11A 110.7 . . ?
C12 C11 H11B 110.7 . . ?
C10 C11 H11B 110.7 . . ?
H11A C11 H11B 108.8 . . ?
C2 C12 C1 127.7(3) . . ?
C2 C12 C11 106.4(3) . . ?
C1 C12 C11 125.7(3) . . ?
C4 C13 H13A 109.5 . . ?
C4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C19 116.8(3) . . ?
C15 C14 C10 122.3(3) . . ?
C19 C14 C10 120.9(3) . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 120.5(4) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C19 C18 C17 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C14 121.6(4) . . ?
C18 C19 H19 119.2 . . ?
C14 C19 H19 119.2 . . ?
O1 C20 H20A 109.5 . . ?
O1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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
C20 O1 C1 O2 5.5(5) . . . . ?
C20 O1 C1 C12 -174.9(3) . . . . ?
C3 N1 C2 C12 179.9(4) . . . . ?
C3 N1 C2 C9 1.3(3) . . . . ?
C2 N1 C3 C4 179.6(3) . . . . ?
C2 N1 C3 C8 -2.3(3) . . . . ?
N1 C3 C4 C5 177.5(3) . . . . ?
C8 C3 C4 C5 -0.2(5) . . . . ?
N1 C3 C4 C13 -5.2(5) . . . . ?
C8 C3 C4 C13 177.1(3) . . . . ?
C3 C4 C5 C6 -1.5(5) . . . . ?
C13 C4 C5 C6 -178.7(3) . . . . ?
C4 C5 C6 C7 2.6(6) . . . . ?
C5 C6 C7 C8 -1.8(5) . . . . ?
C6 C7 C8 C3 0.1(5) . . . . ?
C6 C7 C8 C9 -179.3(4) . . . . ?
C4 C3 C8 C7 0.9(5) . . . . ?
N1 C3 C8 C7 -177.2(3) . . . . ?
C4 C3 C8 C9 -179.5(3) . . . . ?
N1 C3 C8 C9 2.4(3) . . . . ?
N1 C2 C9 C10 179.6(3) . . . . ?
C12 C2 C9 C10 0.5(4) . . . . ?
N1 C2 C9 C8 0.2(4) . . . . ?
C12 C2 C9 C8 -178.8(3) . . . . ?
C7 C8 C9 C10 -1.0(8) . . . . ?
C3 C8 C9 C10 179.5(4) . . . . ?
C7 C8 C9 C2 177.9(4) . . . . ?
C3 C8 C9 C2 -1.6(3) . . . . ?
C2 C9 C10 C14 178.0(3) . . . . ?
C8 C9 C10 C14 -3.1(7) . . . . ?
C2 C9 C10 C11 -1.2(3) . . . . ?
C8 C9 C10 C11 177.6(4) . . . . ?
C9 C10 C11 C12 1.5(3) . . . . ?
C14 C10 C11 C12 -177.9(3) . . . . ?
N1 C2 C12 C1 -3.3(6) . . . . ?
C9 C2 C12 C1 175.3(3) . . . . ?
N1 C2 C12 C11 -178.2(4) . . . . ?
C9 C2 C12 C11 0.4(4) . . . . ?
O2 C1 C12 C2 -173.3(3) . . . . ?
O1 C1 C12 C2 7.2(5) . . . . ?
O2 C1 C12 C11 0.7(6) . . . . ?
O1 C1 C12 C11 -178.9(3) . . . . ?
C10 C11 C12 C2 -1.1(3) . . . . ?
C10 C11 C12 C1 -176.2(3) . . . . ?
C9 C10 C14 C15 -25.5(5) . . . . ?
C11 C10 C14 C15 153.6(3) . . . . ?
C9 C10 C14 C19 157.0(4) . . . . ?
C11 C10 C14 C19 -23.8(5) . . . . ?
C19 C14 C15 C16 -0.4(5) . . . . ?
C10 C14 C15 C16 -178.0(3) . . . . ?
C14 C15 C16 C17 -0.4(6) . . . . ?
C15 C16 C17 C18 0.7(6) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C17 C18 C19 C14 -0.7(6) . . . . ?
C15 C14 C19 C18 1.0(5) . . . . ?
C10 C14 C19 C18 178.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.067
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_240105d
_database_code_depnum_ccdc_archive 'CCDC 2323814'
loop_
_audit_author_name
_audit_author_address
'wang man'
;University
China
;
_audit_update_record             
;
2024-01-06 deposited with the CCDC.	2024-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H33 N3 O3'
_chemical_formula_weight         579.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.385(2)
_cell_length_b                   8.8207(9)
_cell_length_c                   33.720(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.974(3)
_cell_angle_gamma                90.00
_cell_volume                     5988.9(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2062
_cell_measurement_theta_min      2.423
_cell_measurement_theta_max      26.88

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9617
_exptl_absorpt_correction_T_max  0.9894
_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  '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            13983
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5241
_reflns_number_gt                2730
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0410P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00112(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5241
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
N1 N 0.13876(11) 0.4961(3) 0.35070(7) 0.0488(7) Uani 1 1 d . . .
H1 H 0.1178 0.5373 0.3293 0.059 Uiso 1 1 calc R . .
N2 N 0.27042(12) 0.6012(3) 0.52029(7) 0.0504(7) Uani 1 1 d . . .
H2 H 0.2474 0.6153 0.5393 0.060 Uiso 1 1 calc R . .
N3 N 0.27667(13) 0.4664(3) 0.25450(7) 0.0616(8) Uani 1 1 d . . .
H3 H 0.2666 0.4066 0.2343 0.074 Uiso 1 1 calc R . .
O1 O 0.24306(11) 0.8540(3) 0.38429(6) 0.0697(7) Uani 1 1 d . . .
O2 O 0.19842(13) 0.8253(3) 0.32152(7) 0.0891(9) Uani 1 1 d . . .
O3 O 0.48009(16) 0.1373(5) 0.19540(10) 0.1245(13) Uani 1 1 d . . .
C1 C 0.29269(13) 0.4617(3) 0.41954(7) 0.0365(7) Uani 1 1 d . . .
C2 C 0.31469(13) 0.5857(4) 0.39048(7) 0.0439(8) Uani 1 1 d . . .
H2A H 0.3253 0.6793 0.4052 0.053 Uiso 1 1 calc R . .
H2B H 0.3542 0.5516 0.3804 0.053 Uiso 1 1 calc R . .
C3 C 0.25770(14) 0.6148(3) 0.35451(8) 0.0394(7) Uani 1 1 d . . .
C4 C 0.20430(14) 0.5185(3) 0.36669(8) 0.0403(8) Uani 1 1 d . . .
C5 C 0.22122(13) 0.4365(3) 0.40059(8) 0.0382(7) Uani 1 1 d . . .
C6 C 0.16314(14) 0.3527(3) 0.40672(8) 0.0394(7) Uani 1 1 d . . .
C7 C 0.11315(14) 0.3957(4) 0.37534(8) 0.0440(8) Uani 1 1 d . . .
C8 C 0.04980(15) 0.3364(4) 0.37160(9) 0.0585(9) Uani 1 1 d . . .
H8 H 0.0173 0.3644 0.3503 0.070 Uiso 1 1 calc R . .
C9 C 0.03602(15) 0.2357(4) 0.39990(10) 0.0592(10) Uani 1 1 d . . .
H9 H -0.0066 0.1957 0.3981 0.071 Uiso 1 1 calc R . .
C10 C 0.08481(16) 0.1921(4) 0.43133(9) 0.0553(9) Uani 1 1 d . . .
H10 H 0.0745 0.1226 0.4501 0.066 Uiso 1 1 calc R . .
C11 C 0.14790(15) 0.2499(4) 0.43507(8) 0.0471(8) Uani 1 1 d . . .
H11 H 0.1801 0.2205 0.4563 0.057 Uiso 1 1 calc R . .
C12 C 0.24835(15) 0.5325(3) 0.48435(8) 0.0457(8) Uani 1 1 d . . .
H12 H 0.2055 0.4958 0.4766 0.055 Uiso 1 1 calc R . .
C13 C 0.29724(13) 0.5250(3) 0.46158(8) 0.0379(7) Uani 1 1 d . . .
C14 C 0.35417(14) 0.5960(3) 0.48486(8) 0.0403(8) Uani 1 1 d . . .
C15 C 0.33531(15) 0.6442(4) 0.52115(8) 0.0448(8) Uani 1 1 d . . .
C16 C 0.37711(16) 0.7236(4) 0.54976(9) 0.0587(9) Uani 1 1 d . . .
H16 H 0.3630 0.7572 0.5732 0.070 Uiso 1 1 calc R . .
C17 C 0.44006(17) 0.7514(4) 0.54252(10) 0.0694(11) Uani 1 1 d . . .
H17 H 0.4694 0.8050 0.5613 0.083 Uiso 1 1 calc R . .
C18 C 0.46092(16) 0.7012(4) 0.50756(10) 0.0701(11) Uani 1 1 d . . .
H18 H 0.5041 0.7211 0.5034 0.084 Uiso 1 1 calc R . .
C19 C 0.41922(15) 0.6230(4) 0.47920(9) 0.0573(10) Uani 1 1 d . . .
H19 H 0.4342 0.5879 0.4562 0.069 Uiso 1 1 calc R . .
C20 C 0.24818(15) 0.4642(4) 0.28862(9) 0.0556(9) Uani 1 1 d . . .
H20 H 0.2150 0.3976 0.2936 0.067 Uiso 1 1 calc R . .
C21 C 0.27559(14) 0.5737(4) 0.31405(8) 0.0434(8) Uani 1 1 d . . .
C22 C 0.32379(14) 0.6485(4) 0.29464(8) 0.0428(8) Uani 1 1 d . . .
C23 C 0.32351(15) 0.5779(4) 0.25742(8) 0.0488(9) Uani 1 1 d . . .
C24 C 0.36442(16) 0.6225(5) 0.23048(9) 0.0615(10) Uani 1 1 d . . .
H24 H 0.3630 0.5744 0.2058 0.074 Uiso 1 1 calc R . .
C25 C 0.40688(16) 0.7398(5) 0.24154(10) 0.0680(11) Uani 1 1 d . . .
H25 H 0.4350 0.7725 0.2241 0.082 Uiso 1 1 calc R . .
C26 C 0.40888(16) 0.8110(4) 0.27821(10) 0.0663(10) Uani 1 1 d . . .
H26 H 0.4387 0.8900 0.2850 0.080 Uiso 1 1 calc R . .
C27 C 0.36804(15) 0.7681(4) 0.30478(9) 0.0581(9) Uani 1 1 d . . .
H27 H 0.3697 0.8179 0.3292 0.070 Uiso 1 1 calc R . .
C28 C 0.33210(13) 0.3151(4) 0.41923(8) 0.0411(8) Uani 1 1 d . . .
C29 C 0.34912(14) 0.2277(4) 0.45302(9) 0.0509(9) Uani 1 1 d . . .
H29 H 0.3382 0.2620 0.4772 0.061 Uiso 1 1 calc R . .
C30 C 0.38203(16) 0.0901(4) 0.45241(11) 0.0632(10) Uani 1 1 d . . .
H30 H 0.3930 0.0340 0.4759 0.076 Uiso 1 1 calc R . .
C31 C 0.39790(17) 0.0386(4) 0.41738(12) 0.0712(11) Uani 1 1 d . . .
H31 H 0.4194 -0.0541 0.4166 0.085 Uiso 1 1 calc R . .
C32 C 0.38242(18) 0.1221(5) 0.38299(12) 0.0783(12) Uani 1 1 d . . .
H32 H 0.3944 0.0872 0.3591 0.094 Uiso 1 1 calc R . .
C33 C 0.34896(16) 0.2585(4) 0.38365(9) 0.0637(10) Uani 1 1 d . . .
H33 H 0.3376 0.3130 0.3600 0.076 Uiso 1 1 calc R . .
C34 C 0.23147(15) 0.7772(4) 0.35146(9) 0.0474(9) Uani 1 1 d . . .
C35 C 0.21466(18) 1.0062(4) 0.38195(11) 0.0857(13) Uani 1 1 d . . .
H35A H 0.2294 1.0607 0.3603 0.128 Uiso 1 1 calc R . .
H35B H 0.2288 1.0587 0.4068 0.128 Uiso 1 1 calc R . .
H35C H 0.1671 0.9994 0.3773 0.128 Uiso 1 1 calc R . .
C36 C 0.5796(3) 0.2577(8) 0.21920(16) 0.183(3) Uani 1 1 d . . .
H36A H 0.5808 0.1906 0.2417 0.274 Uiso 1 1 calc R . .
H36B H 0.5884 0.3595 0.2287 0.274 Uiso 1 1 calc R . .
H36C H 0.6127 0.2275 0.2034 0.274 Uiso 1 1 calc R . .
C37 C 0.5126(3) 0.2509(8) 0.19398(16) 0.1156(19) Uani 1 1 d . . .
C38 C 0.4889(4) 0.3755(9) 0.1680(3) 0.253(5) Uani 1 1 d . . .
H38A H 0.4419 0.3658 0.1597 0.380 Uiso 1 1 calc R . .
H38B H 0.5109 0.3742 0.1448 0.380 Uiso 1 1 calc R . .
H38C H 0.4983 0.4693 0.1822 0.380 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C7 1.372(3) . ?
N1 C4 1.375(3) . ?
N1 H1 0.8600 . ?
N2 C12 1.367(3) . ?
N2 C15 1.372(3) . ?
N2 H2 0.8600 . ?
N3 C23 1.364(4) . ?
N3 C20 1.368(3) . ?
N3 H3 0.8600 . ?
O1 C34 1.288(3) . ?
O1 C35 1.460(4) . ?
O2 C34 1.201(3) . ?
O3 C37 1.206(6) . ?
C1 C13 1.513(4) . ?
C1 C5 1.513(3) . ?
C1 C28 1.524(4) . ?
C1 C2 1.579(4) . ?
C2 C3 1.564(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.488(4) . ?
C3 C21 1.510(4) . ?
C3 C34 1.526(4) . ?
C4 C5 1.351(4) . ?
C5 C6 1.438(4) . ?
C6 C11 1.388(4) . ?
C6 C7 1.402(4) . ?
C7 C8 1.381(4) . ?
C8 C9 1.365(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.390(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.371(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.351(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.439(4) . ?
C14 C19 1.389(4) . ?
C14 C15 1.404(4) . ?
C15 C16 1.375(4) . ?
C16 C17 1.365(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.364(4) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.354(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.425(4) . ?
C22 C27 1.395(4) . ?
C22 C23 1.400(4) . ?
C23 C24 1.383(4) . ?
C24 C25 1.363(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.368(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C29 1.375(4) . ?
C28 C33 1.391(4) . ?
C29 C30 1.389(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.351(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.368(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.384(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.494(7) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.440(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 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
C7 N1 C4 107.1(2) . . ?
C7 N1 H1 126.5 . . ?
C4 N1 H1 126.5 . . ?
C12 N2 C15 108.9(2) . . ?
C12 N2 H2 125.5 . . ?
C15 N2 H2 125.5 . . ?
C23 N3 C20 109.5(3) . . ?
C23 N3 H3 125.2 . . ?
C20 N3 H3 125.2 . . ?
C34 O1 C35 114.8(3) . . ?
C13 C1 C5 111.3(2) . . ?
C13 C1 C28 111.4(2) . . ?
C5 C1 C28 110.3(2) . . ?
C13 C1 C2 110.1(2) . . ?
C5 C1 C2 100.8(2) . . ?
C28 C1 C2 112.5(2) . . ?
C3 C2 C1 110.3(2) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C21 113.7(2) . . ?
C4 C3 C34 106.9(2) . . ?
C21 C3 C34 107.2(2) . . ?
C4 C3 C2 100.3(2) . . ?
C21 C3 C2 114.0(2) . . ?
C34 C3 C2 114.6(2) . . ?
C5 C4 N1 111.0(3) . . ?
C5 C4 C3 116.0(3) . . ?
N1 C4 C3 133.0(3) . . ?
C4 C5 C6 106.8(2) . . ?
C4 C5 C1 112.4(3) . . ?
C6 C5 C1 140.8(3) . . ?
C11 C6 C7 118.8(3) . . ?
C11 C6 C5 135.5(3) . . ?
C7 C6 C5 105.7(2) . . ?
N1 C7 C8 128.9(3) . . ?
N1 C7 C6 109.3(2) . . ?
C8 C7 C6 121.7(3) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C6 119.2(3) . . ?
C10 C11 H11 120.4 . . ?
C6 C11 H11 120.4 . . ?
C13 C12 N2 110.8(3) . . ?
C13 C12 H12 124.6 . . ?
N2 C12 H12 124.6 . . ?
C12 C13 C14 105.8(2) . . ?
C12 C13 C1 127.4(3) . . ?
C14 C13 C1 126.7(2) . . ?
C19 C14 C15 117.7(3) . . ?
C19 C14 C13 134.8(3) . . ?
C15 C14 C13 107.5(2) . . ?
N2 C15 C16 130.2(3) . . ?
N2 C15 C14 107.0(3) . . ?
C16 C15 C14 122.8(3) . . ?
C17 C16 C15 117.6(3) . . ?
C17 C16 H16 121.2 . . ?
C15 C16 H16 121.2 . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C14 119.6(3) . . ?
C18 C19 H19 120.2 . . ?
C14 C19 H19 120.2 . . ?
C21 C20 N3 109.6(3) . . ?
C21 C20 H20 125.2 . . ?
N3 C20 H20 125.2 . . ?
C20 C21 C22 106.6(2) . . ?
C20 C21 C3 127.6(3) . . ?
C22 C21 C3 125.8(3) . . ?
C27 C22 C23 117.9(3) . . ?
C27 C22 C21 134.7(3) . . ?
C23 C22 C21 107.4(3) . . ?
N3 C23 C24 130.2(3) . . ?
N3 C23 C22 106.9(3) . . ?
C24 C23 C22 122.9(3) . . ?
C25 C24 C23 117.3(3) . . ?
C25 C24 H24 121.4 . . ?
C23 C24 H24 121.4 . . ?
C24 C25 C26 121.2(3) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C27 C26 C25 121.6(3) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C22 119.0(3) . . ?
C26 C27 H27 120.5 . . ?
C22 C27 H27 120.5 . . ?
C29 C28 C33 116.7(3) . . ?
C29 C28 C1 122.4(2) . . ?
C33 C28 C1 120.8(3) . . ?
C28 C29 C30 122.5(3) . . ?
C28 C29 H29 118.7 . . ?
C30 C29 H29 118.7 . . ?
C31 C30 C29 119.3(3) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 120.3(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C33 120.2(3) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C32 C33 C28 120.9(3) . . ?
C32 C33 H33 119.5 . . ?
C28 C33 H33 119.5 . . ?
O2 C34 O1 122.7(3) . . ?
O2 C34 C3 122.2(3) . . ?
O1 C34 C3 114.9(3) . . ?
O1 C35 H35A 109.5 . . ?
O1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O3 C37 C38 121.6(6) . . ?
O3 C37 C36 118.0(6) . . ?
C38 C37 C36 120.3(6) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

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
C13 C1 C2 C3 -122.7(2) . . . . ?
C5 C1 C2 C3 -5.1(3) . . . . ?
C28 C1 C2 C3 112.4(3) . . . . ?
C1 C2 C3 C4 5.2(3) . . . . ?
C1 C2 C3 C21 -116.7(3) . . . . ?
C1 C2 C3 C34 119.2(3) . . . . ?
C7 N1 C4 C5 -0.2(3) . . . . ?
C7 N1 C4 C3 -178.8(3) . . . . ?
C21 C3 C4 C5 118.6(3) . . . . ?
C34 C3 C4 C5 -123.3(3) . . . . ?
C2 C3 C4 C5 -3.5(3) . . . . ?
C21 C3 C4 N1 -62.8(4) . . . . ?
C34 C3 C4 N1 55.3(4) . . . . ?
C2 C3 C4 N1 175.1(3) . . . . ?
N1 C4 C5 C6 1.2(3) . . . . ?
C3 C4 C5 C6 -179.9(2) . . . . ?
N1 C4 C5 C1 -178.6(2) . . . . ?
C3 C4 C5 C1 0.3(4) . . . . ?
C13 C1 C5 C4 119.7(3) . . . . ?
C28 C1 C5 C4 -116.1(3) . . . . ?
C2 C1 C5 C4 2.9(3) . . . . ?
C13 C1 C5 C6 -59.9(5) . . . . ?
C28 C1 C5 C6 64.3(4) . . . . ?
C2 C1 C5 C6 -176.6(3) . . . . ?
C4 C5 C6 C11 179.5(3) . . . . ?
C1 C5 C6 C11 -0.9(6) . . . . ?
C4 C5 C6 C7 -1.7(3) . . . . ?
C1 C5 C6 C7 178.0(3) . . . . ?
C4 N1 C7 C8 -179.0(3) . . . . ?
C4 N1 C7 C6 -0.9(3) . . . . ?
C11 C6 C7 N1 -179.4(2) . . . . ?
C5 C6 C7 N1 1.6(3) . . . . ?
C11 C6 C7 C8 -1.2(4) . . . . ?
C5 C6 C7 C8 179.8(3) . . . . ?
N1 C7 C8 C9 179.1(3) . . . . ?
C6 C7 C8 C9 1.3(5) . . . . ?
C7 C8 C9 C10 -1.0(5) . . . . ?
C8 C9 C10 C11 0.6(5) . . . . ?
C9 C10 C11 C6 -0.5(5) . . . . ?
C7 C6 C11 C10 0.7(4) . . . . ?
C5 C6 C11 C10 179.4(3) . . . . ?
C15 N2 C12 C13 1.5(4) . . . . ?
N2 C12 C13 C14 -0.6(3) . . . . ?
N2 C12 C13 C1 -178.2(3) . . . . ?
C5 C1 C13 C12 12.9(4) . . . . ?
C28 C1 C13 C12 -110.6(3) . . . . ?
C2 C1 C13 C12 123.9(3) . . . . ?
C5 C1 C13 C14 -164.1(3) . . . . ?
C28 C1 C13 C14 72.4(4) . . . . ?
C2 C1 C13 C14 -53.1(4) . . . . ?
C12 C13 C14 C19 178.9(3) . . . . ?
C1 C13 C14 C19 -3.6(6) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C1 C13 C14 C15 177.1(3) . . . . ?
C12 N2 C15 C16 176.1(3) . . . . ?
C12 N2 C15 C14 -1.7(3) . . . . ?
C19 C14 C15 N2 -178.1(3) . . . . ?
C13 C14 C15 N2 1.3(3) . . . . ?
C19 C14 C15 C16 3.9(5) . . . . ?
C13 C14 C15 C16 -176.7(3) . . . . ?
N2 C15 C16 C17 -179.6(3) . . . . ?
C14 C15 C16 C17 -2.1(5) . . . . ?
C15 C16 C17 C18 0.0(5) . . . . ?
C16 C17 C18 C19 0.3(6) . . . . ?
C17 C18 C19 C14 1.5(6) . . . . ?
C15 C14 C19 C18 -3.5(5) . . . . ?
C13 C14 C19 C18 177.3(3) . . . . ?
C23 N3 C20 C21 0.2(4) . . . . ?
N3 C20 C21 C22 0.1(4) . . . . ?
N3 C20 C21 C3 178.0(3) . . . . ?
C4 C3 C21 C20 1.1(5) . . . . ?
C34 C3 C21 C20 -116.8(4) . . . . ?
C2 C3 C21 C20 115.3(4) . . . . ?
C4 C3 C21 C22 178.6(3) . . . . ?
C34 C3 C21 C22 60.7(4) . . . . ?
C2 C3 C21 C22 -67.2(4) . . . . ?
C20 C21 C22 C27 -179.8(4) . . . . ?
C3 C21 C22 C27 2.2(6) . . . . ?
C20 C21 C22 C23 -0.4(4) . . . . ?
C3 C21 C22 C23 -178.3(3) . . . . ?
C20 N3 C23 C24 -179.7(3) . . . . ?
C20 N3 C23 C22 -0.5(4) . . . . ?
C27 C22 C23 N3 -179.9(3) . . . . ?
C21 C22 C23 N3 0.5(3) . . . . ?
C27 C22 C23 C24 -0.6(5) . . . . ?
C21 C22 C23 C24 179.8(3) . . . . ?
N3 C23 C24 C25 179.7(3) . . . . ?
C22 C23 C24 C25 0.6(5) . . . . ?
C23 C24 C25 C26 0.0(5) . . . . ?
C24 C25 C26 C27 -0.7(6) . . . . ?
C25 C26 C27 C22 0.6(5) . . . . ?
C23 C22 C27 C26 0.0(5) . . . . ?
C21 C22 C27 C26 179.4(3) . . . . ?
C13 C1 C28 C29 20.7(4) . . . . ?
C5 C1 C28 C29 -103.4(3) . . . . ?
C2 C1 C28 C29 144.9(3) . . . . ?
C13 C1 C28 C33 -163.4(3) . . . . ?
C5 C1 C28 C33 72.4(3) . . . . ?
C2 C1 C28 C33 -39.2(4) . . . . ?
C33 C28 C29 C30 0.6(5) . . . . ?
C1 C28 C29 C30 176.6(3) . . . . ?
C28 C29 C30 C31 -0.4(5) . . . . ?
C29 C30 C31 C32 0.8(5) . . . . ?
C30 C31 C32 C33 -1.5(6) . . . . ?
C31 C32 C33 C28 1.8(6) . . . . ?
C29 C28 C33 C32 -1.3(5) . . . . ?
C1 C28 C33 C32 -177.4(3) . . . . ?
C35 O1 C34 O2 -1.9(5) . . . . ?
C35 O1 C34 C3 -176.6(3) . . . . ?
C4 C3 C34 O2 -85.8(3) . . . . ?
C21 C3 C34 O2 36.5(4) . . . . ?
C2 C3 C34 O2 164.1(3) . . . . ?
C4 C3 C34 O1 89.0(3) . . . . ?
C21 C3 C34 O1 -148.7(3) . . . . ?
C2 C3 C34 O1 -21.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.046
