# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H19 N'
_chemical_formula_weight         309.39

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'

_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                   9.2869(19)
_cell_length_b                   9.636(2)
_cell_length_c                   11.202(2)
_cell_angle_alpha                84.187(3)
_cell_angle_beta                 72.065(3)
_cell_angle_gamma                64.104(3)
_cell_volume                     857.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9782
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4333
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2990
_reflns_number_gt                2680
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0300P)²+0.3000P] 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       0.144(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2990
_refine_ls_number_parameters     219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0998
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.52225(17) 0.23036(16) 1.00438(13) 0.0397(3) Uani 1 1 d . . .
C2 C 0.60494(17) 0.19791(16) 0.87783(12) 0.0391(3) Uani 1 1 d . . .
C3 C 0.48164(17) 0.21525(16) 0.81769(13) 0.0401(3) Uani 1 1 d . . .
C4 C 0.4851(2) 0.20248(18) 0.69263(14) 0.0478(4) Uani 1 1 d . . .
H4 H 0.5847 0.1753 0.6278 0.057 Uiso 1 1 calc R . .
C5 C 0.3378(2) 0.23101(19) 0.66799(16) 0.0557(4) Uani 1 1 d . . .
H5 H 0.3390 0.2237 0.5855 0.067 Uiso 1 1 calc R . .
C6 C 0.1870(2) 0.2706(2) 0.76445(17) 0.0584(4) Uani 1 1 d . . .
H6 H 0.0900 0.2895 0.7447 0.070 Uiso 1 1 calc R . .
C7 C 0.17934(19) 0.28234(19) 0.88800(16) 0.0536(4) Uani 1 1 d . . .
H7 H 0.0793 0.3074 0.9521 0.064 Uiso 1 1 calc R . .
C8 C 0.32786(18) 0.25504(17) 0.91345(13) 0.0434(3) Uani 1 1 d . . .
C9 C 0.2209(2) 0.3123(2) 1.14506(15) 0.0641(5) Uani 1 1 d . . .
H9A H 0.1218 0.3937 1.1309 0.096 Uiso 1 1 calc R . .
H9B H 0.2555 0.3488 1.2029 0.096 Uiso 1 1 calc R . .
H9C H 0.1974 0.2264 1.1795 0.096 Uiso 1 1 calc R . .
C10 C 0.58475(17) 0.24203(16) 1.10818(13) 0.0406(3) Uani 1 1 d . . .
C11 C 0.56927(19) 0.15543(18) 1.21492(14) 0.0490(4) Uani 1 1 d . . .
H11 H 0.5238 0.0853 1.2198 0.059 Uiso 1 1 calc R . .
C12 C 0.6210(2) 0.1728(2) 1.31382(15) 0.0588(4) Uani 1 1 d . . .
H12 H 0.6091 0.1151 1.3849 0.071 Uiso 1 1 calc R . .
C13 C 0.6899(2) 0.2752(2) 1.30731(18) 0.0642(5) Uani 1 1 d . . .
H13 H 0.7228 0.2877 1.3744 0.077 Uiso 1 1 calc R . .
C14 C 0.7100(2) 0.3589(2) 1.20120(19) 0.0624(5) Uani 1 1 d . . .
H14 H 0.7588 0.4264 1.1961 0.075 Uiso 1 1 calc R . .
C15 C 0.65775(19) 0.34298(17) 1.10191(16) 0.0512(4) Uani 1 1 d . . .
H15 H 0.6715 0.4001 1.0307 0.061 Uiso 1 1 calc R . .
C16 C 0.78783(17) 0.14580(16) 0.81668(13) 0.0424(3) Uani 1 1 d . . .
C17 C 0.8997(2) 0.0411(2) 0.86856(16) 0.0603(5) Uani 1 1 d . . .
H17A H 0.8640 -0.0006 0.9442 0.072 Uiso 1 1 calc R . .
H17B H 1.0136 0.0098 0.8291 0.072 Uiso 1 1 calc R . .
C18 C 0.84032(16) 0.21724(16) 0.69665(13) 0.0401(3) Uani 1 1 d . . .
C19 C 0.74503(19) 0.37085(18) 0.67578(14) 0.0496(4) Uani 1 1 d . . .
H19 H 0.6455 0.4284 0.7364 0.060 Uiso 1 1 calc R . .
C20 C 0.7960(2) 0.4391(2) 0.56642(16) 0.0604(4) Uani 1 1 d . . .
H20 H 0.7310 0.5420 0.5547 0.072 Uiso 1 1 calc R . .
C21 C 0.9419(2) 0.3565(2) 0.47462(16) 0.0627(5) Uani 1 1 d . . .
H21 H 0.9756 0.4031 0.4012 0.075 Uiso 1 1 calc R . .
C22 C 1.0376(2) 0.2037(2) 0.49259(15) 0.0620(5) Uani 1 1 d . . .
H22 H 1.1364 0.1469 0.4310 0.074 Uiso 1 1 calc R . .
C23 C 0.98697(19) 0.13462(19) 0.60212(14) 0.0506(4) Uani 1 1 d . . .
H23 H 1.0520 0.0313 0.6127 0.061 Uiso 1 1 calc R . .
N1 N 0.35423(14) 0.26346(14) 1.02650(11) 0.0448(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.3808(19) . ?
C1 N1 1.3932(18) . ?
C1 C10 1.4835(19) . ?
C2 C3 1.4416(19) . ?
C2 C16 1.4880(19) . ?
C3 C4 1.408(2) . ?
C3 C8 1.414(2) . ?
C4 C5 1.382(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.400(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.377(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.401(2) . ?
C7 H7 0.9300 . ?
C8 N1 1.3783(18) . ?
C9 N1 1.4572(19) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.394(2) . ?
C10 C15 1.394(2) . ?
C11 C12 1.386(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.389(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.331(2) . ?
C16 C18 1.490(2) . ?
C17 H17A 0.9300 . ?
C17 H17B 0.9300 . ?
C18 C19 1.394(2) . ?
C18 C23 1.395(2) . ?
C19 C20 1.382(2) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.380(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.386(2) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 109.53(12) . . ?
C2 C1 C10 129.77(12) . . ?
N1 C1 C10 120.58(12) . . ?
C1 C2 C3 106.75(12) . . ?
C1 C2 C16 126.51(13) . . ?
C3 C2 C16 126.65(12) . . ?
C4 C3 C8 118.65(13) . . ?
C4 C3 C2 134.49(13) . . ?
C8 C3 C2 106.85(12) . . ?
C5 C4 C3 118.82(14) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 121.44(15) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C7 C6 C5 121.34(15) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 117.48(15) . . ?
C6 C7 H7 121.3 . . ?
C8 C7 H7 121.3 . . ?
N1 C8 C7 129.42(14) . . ?
N1 C8 C3 108.31(12) . . ?
C7 C8 C3 122.26(14) . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 118.42(14) . . ?
C11 C10 C1 121.22(13) . . ?
C15 C10 C1 120.35(13) . . ?
C12 C11 C10 120.62(15) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 120.29(16) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.87(16) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C15 120.28(16) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C10 120.49(15) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C17 C16 C2 121.07(14) . . ?
C17 C16 C18 121.49(14) . . ?
C2 C16 C18 117.43(12) . . ?
C16 C17 H17A 120.0 . . ?
C16 C17 H17B 120.0 . . ?
H17A C17 H17B 120.0 . . ?
C19 C18 C23 117.49(14) . . ?
C19 C18 C16 120.83(12) . . ?
C23 C18 C16 121.67(13) . . ?
C20 C19 C18 121.06(15) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 120.74(17) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 119.29(16) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C23 120.21(15) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C18 121.20(16) . . ?
C22 C23 H23 119.4 . . ?
C18 C23 H23 119.4 . . ?
C8 N1 C1 108.54(11) . . ?
C8 N1 C9 123.60(12) . . ?
C1 N1 C9 127.67(13) . . ?

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 C3 1.42(15) . . . . ?
C10 C1 C2 C3 -174.73(13) . . . . ?
N1 C1 C2 C16 -175.19(13) . . . . ?
C10 C1 C2 C16 8.7(2) . . . . ?
C1 C2 C3 C4 178.14(15) . . . . ?
C16 C2 C3 C4 -5.3(3) . . . . ?
C1 C2 C3 C8 -1.23(15) . . . . ?
C16 C2 C3 C8 175.38(13) . . . . ?
C8 C3 C4 C5 0.7(2) . . . . ?
C2 C3 C4 C5 -178.57(15) . . . . ?
C3 C4 C5 C6 -0.6(2) . . . . ?
C4 C5 C6 C7 -0.2(3) . . . . ?
C5 C6 C7 C8 0.8(2) . . . . ?
C6 C7 C8 N1 177.84(15) . . . . ?
C6 C7 C8 C3 -0.7(2) . . . . ?
C4 C3 C8 N1 -178.90(12) . . . . ?
C2 C3 C8 N1 0.59(15) . . . . ?
C4 C3 C8 C7 -0.1(2) . . . . ?
C2 C3 C8 C7 179.37(13) . . . . ?
C2 C1 C10 C11 -125.74(17) . . . . ?
N1 C1 C10 C11 58.49(19) . . . . ?
C2 C1 C10 C15 55.6(2) . . . . ?
N1 C1 C10 C15 -120.23(15) . . . . ?
C15 C10 C11 C12 1.8(2) . . . . ?
C1 C10 C11 C12 -176.93(14) . . . . ?
C10 C11 C12 C13 -0.6(2) . . . . ?
C11 C12 C13 C14 -1.0(3) . . . . ?
C12 C13 C14 C15 1.4(3) . . . . ?
C13 C14 C15 C10 -0.1(2) . . . . ?
C11 C10 C15 C14 -1.5(2) . . . . ?
C1 C10 C15 C14 177.30(14) . . . . ?
C1 C2 C16 C17 41.7(2) . . . . ?
C3 C2 C16 C17 -134.26(17) . . . . ?
C1 C2 C16 C18 -137.27(14) . . . . ?
C3 C2 C16 C18 46.78(19) . . . . ?
C17 C16 C18 C19 -144.95(16) . . . . ?
C2 C16 C18 C19 34.01(19) . . . . ?
C17 C16 C18 C23 34.0(2) . . . . ?
C2 C16 C18 C23 -147.01(14) . . . . ?
C23 C18 C19 C20 -1.2(2) . . . . ?
C16 C18 C19 C20 177.84(14) . . . . ?
C18 C19 C20 C21 0.6(3) . . . . ?
C19 C20 C21 C22 0.1(3) . . . . ?
C20 C21 C22 C23 0.0(3) . . . . ?
C21 C22 C23 C18 -0.7(2) . . . . ?
C19 C18 C23 C22 1.2(2) . . . . ?
C16 C18 C23 C22 -177.78(14) . . . . ?
C7 C8 N1 C1 -178.39(15) . . . . ?
C3 C8 N1 C1 0.27(16) . . . . ?
C7 C8 N1 C9 -3.1(2) . . . . ?
C3 C8 N1 C9 175.59(14) . . . . ?
C2 C1 N1 C8 -1.07(16) . . . . ?
C10 C1 N1 C8 175.48(12) . . . . ?
C2 C1 N1 C9 -176.15(15) . . . . ?
C10 C1 N1 C9 0.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.033
_database_code_depnum_ccdc_archive 'CCDC 1000775'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H19 N'
_chemical_formula_weight         273.36

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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.859(4)
_cell_length_b                   7.981(4)
_cell_length_c                   23.406(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.401(9)
_cell_angle_gamma                90.00
_cell_volume                     1466.8(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9789
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9507
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         31.11
_reflns_number_total             6654
_reflns_number_gt                4730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.4800P)²+0.7512P] 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       0.24(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_number_reflns         6654
_refine_ls_number_parameters     384
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1756
_refine_ls_R_factor_gt           0.1541
_refine_ls_wR_factor_ref         0.5295
_refine_ls_wR_factor_gt          0.4980
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.017

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 0.8538(8) 0.1499(10) 0.0734(3) 0.0483(16) Uani 1 1 d . . .
H1 H 0.9180 0.1895 0.1048 0.058 Uiso 1 1 calc R . .
C2 C 0.9339(10) 0.1232(19) 0.0233(3) 0.079(3) Uani 1 1 d . . .
H2 H 1.0453 0.1596 0.0196 0.094 Uiso 1 1 calc R . .
C3 C 0.8506(10) 0.0433(13) -0.0209(3) 0.060(2) Uani 1 1 d . . .
H3 H 0.9059 0.0200 -0.0544 0.072 Uiso 1 1 calc R . .
C4 C 0.6856(11) -0.0018(13) -0.0155(3) 0.061(2) Uani 1 1 d . . .
H4 H 0.6286 -0.0591 -0.0451 0.073 Uiso 1 1 calc R . .
C5 C 0.5995(9) 0.0371(11) 0.0344(3) 0.0501(17) Uani 1 1 d . . .
C6 C 0.4175(9) -0.0068(13) 0.0370(3) 0.0546(19) Uani 1 1 d . . .
H6A H 0.3898 -0.0958 0.0099 0.066 Uiso 1 1 calc R . .
H6B H 0.3480 0.0899 0.0268 0.066 Uiso 1 1 calc R . .
C7 C 0.3791(9) -0.0647(12) 0.0979(3) 0.0525(17) Uani 1 1 d . . .
H7A H 0.2571 -0.0752 0.1015 0.063 Uiso 1 1 calc R . .
H7B H 0.4305 -0.1734 0.1054 0.063 Uiso 1 1 calc R . .
C8 C 0.4490(9) 0.0597(10) 0.1397(3) 0.0539(17) Uani 1 1 d . . .
H8 H 0.3888 0.0794 0.1724 0.065 Uiso 1 1 calc R . .
C9 C 0.5942(6) 0.1459(8) 0.1331(2) 0.0328(12) Uani 1 1 d . . .
C10 C 0.6823(8) 0.1211(11) 0.0795(3) 0.0479(16) Uani 1 1 d . . .
C11 C 0.6651(8) 0.2591(11) 0.1756(3) 0.0483(16) Uani 1 1 d . . .
C12 C 0.7275(8) 0.4276(11) 0.1674(3) 0.0455(15) Uani 1 1 d . . .
C13 C 0.7446(9) 0.5326(11) 0.1193(3) 0.0509(17) Uani 1 1 d . . .
H13 H 0.7134 0.4953 0.0827 0.061 Uiso 1 1 calc R . .
C14 C 0.8110(11) 0.6967(11) 0.1284(4) 0.064(2) Uani 1 1 d . . .
H14 H 0.8248 0.7688 0.0978 0.076 Uiso 1 1 calc R . .
C15 C 0.8531(11) 0.7455(13) 0.1816(4) 0.071(2) Uani 1 1 d . . .
H15 H 0.8905 0.8553 0.1865 0.085 Uiso 1 1 calc R . .
C16 C 0.8460(9) 0.6506(11) 0.2281(3) 0.0546(19) Uani 1 1 d . . .
H16 H 0.8829 0.6914 0.2637 0.065 Uiso 1 1 calc R . .
C17 C 0.7818(9) 0.4883(9) 0.2221(3) 0.0477(16) Uani 1 1 d . . .
C18 C 0.6845(9) 0.2276(11) 0.2336(3) 0.0493(16) Uani 1 1 d . . .
C19 C 0.6532(11) 0.0695(10) 0.2673(3) 0.0521(18) Uani 1 1 d . . .
H19A H 0.7553 0.0389 0.2887 0.078 Uiso 1 1 calc R . .
H19B H 0.6210 -0.0196 0.2414 0.078 Uiso 1 1 calc R . .
H19C H 0.5634 0.0888 0.2931 0.078 Uiso 1 1 calc R . .
C20 C 0.7973(9) 0.3851(13) 0.3220(2) 0.053(2) Uani 1 1 d . . .
H20A H 0.7066 0.3393 0.3433 0.080 Uiso 1 1 calc R . .
H20B H 0.8112 0.5017 0.3311 0.080 Uiso 1 1 calc R . .
H20C H 0.9011 0.3263 0.3317 0.080 Uiso 1 1 calc R . .
C21 C 0.3157(7) 0.6795(8) 0.4217(2) 0.0357(12) Uani 1 1 d . . .
C22 C 0.1438(8) 0.6254(11) 0.4254(3) 0.0502(16) Uani 1 1 d . . .
H22 H 0.0872 0.5681 0.3957 0.060 Uiso 1 1 calc R . .
C23 C 0.0641(10) 0.6641(10) 0.4771(3) 0.0578(19) Uani 1 1 d . . .
H23 H -0.0494 0.6342 0.4806 0.069 Uiso 1 1 calc R . .
C24 C 0.1474(11) 0.744(2) 0.5218(4) 0.080(3) Uani 1 1 d . . .
H24 H 0.0917 0.7674 0.5551 0.096 Uiso 1 1 calc R . .
C25 C 0.3163(10) 0.7879(12) 0.5165(3) 0.057(2) Uani 1 1 d . . .
H25 H 0.3745 0.8375 0.5475 0.069 Uiso 1 1 calc R . .
C26 C 0.4016(8) 0.7614(10) 0.4671(2) 0.0440(14) Uani 1 1 d . . .
C27 C 0.5890(9) 0.8090(12) 0.4596(3) 0.0546(18) Uani 1 1 d . . .
H27A H 0.6195 0.9009 0.4851 0.066 Uiso 1 1 calc R . .
H27B H 0.6610 0.7142 0.4701 0.066 Uiso 1 1 calc R . .
C28 C 0.6211(9) 0.8593(14) 0.3995(3) 0.058(2) Uani 1 1 d . . .
H28A H 0.7429 0.8676 0.3948 0.069 Uiso 1 1 calc R . .
H28B H 0.5716 0.9689 0.3920 0.069 Uiso 1 1 calc R . .
C29 C 0.5467(7) 0.7358(12) 0.3572(2) 0.0473(17) Uani 1 1 d . . .
H29 H 0.5999 0.7190 0.3230 0.057 Uiso 1 1 calc R . .
C30 C 0.3308(7) 0.5294(8) 0.3225(2) 0.0360(12) Uani 1 1 d . . .
C31 C 0.3065(8) 0.5619(9) 0.2651(2) 0.0397(14) Uani 1 1 d . . .
C32 C 0.3493(9) 0.7104(14) 0.2340(3) 0.059(2) Uani 1 1 d . . .
H32A H 0.3460 0.8058 0.2589 0.088 Uiso 1 1 calc R . .
H32B H 0.2689 0.7257 0.2024 0.088 Uiso 1 1 calc R . .
H32C H 0.4617 0.6989 0.2199 0.088 Uiso 1 1 calc R . .
C33 C 0.2761(8) 0.3606(9) 0.3314(3) 0.0416(14) Uani 1 1 d . . .
C34 C 0.2668(8) 0.2567(11) 0.3767(3) 0.0504(16) Uani 1 1 d . . .
H34 H 0.3073 0.2947 0.4123 0.060 Uiso 1 1 calc R . .
C35 C 0.2026(9) 0.1026(11) 0.3729(3) 0.0544(18) Uani 1 1 d . . .
H35 H 0.1981 0.0360 0.4054 0.065 Uiso 1 1 calc R . .
C36 C 0.1389(10) 0.0383(10) 0.3174(4) 0.0595(19) Uani 1 1 d . . .
H36 H 0.0908 -0.0680 0.3145 0.071 Uiso 1 1 calc R . .
C37 C 0.1517(9) 0.1406(10) 0.2682(4) 0.0555(19) Uani 1 1 d . . .
H37 H 0.1160 0.1043 0.2319 0.067 Uiso 1 1 calc R . .
C38 C 0.2210(7) 0.2979(10) 0.2779(3) 0.0436(16) Uani 1 1 d . . .
C39 C 0.2016(11) 0.4248(13) 0.1773(3) 0.061(2) Uani 1 1 d . . .
H39A H 0.2929 0.3761 0.1570 0.092 Uiso 1 1 calc R . .
H39B H 0.1834 0.5381 0.1647 0.092 Uiso 1 1 calc R . .
H39C H 0.0995 0.3609 0.1701 0.092 Uiso 1 1 calc R . .
C40 C 0.4057(10) 0.6490(10) 0.3675(3) 0.0561(19) Uani 1 1 d . . .
N1 N 0.7556(6) 0.3664(9) 0.25992(19) 0.0424(13) Uani 1 1 d . . .
N2 N 0.2440(8) 0.4241(9) 0.2362(2) 0.0492(15) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.369(9) . ?
C1 C10 1.380(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.357(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.409(10) . ?
C4 H4 0.9300 . ?
C5 C10 1.389(8) . ?
C5 C6 1.477(10) . ?
C6 C7 1.540(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.483(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.347(8) . ?
C8 H8 0.9300 . ?
C9 C11 1.438(9) . ?
C9 C10 1.472(7) . ?
C11 C18 1.383(10) . ?
C11 C12 1.447(12) . ?
C12 C13 1.415(9) . ?
C12 C17 1.417(10) . ?
C13 C14 1.423(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.331(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.329(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(11) . ?
C16 H16 0.9300 . ?
C17 N1 1.337(9) . ?
C18 N1 1.375(10) . ?
C18 C19 1.514(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N1 1.483(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.397(8) . ?
C21 C22 1.424(9) . ?
C21 C40 1.497(8) . ?
C22 C23 1.420(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.385(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.376(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.539(9) . ?
C27 C28 1.494(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.498(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C40 1.337(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.373(7) . ?
C30 C33 1.432(10) . ?
C30 C40 1.523(11) . ?
C31 N2 1.371(9) . ?
C31 C32 1.438(11) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.350(10) . ?
C33 C38 1.401(8) . ?
C34 C35 1.330(13) . ?
C34 H34 0.9300 . ?
C35 C36 1.466(11) . ?
C35 H35 0.9300 . ?
C36 C37 1.420(11) . ?
C36 H36 0.9300 . ?
C37 C38 1.383(11) . ?
C37 H37 0.9300 . ?
C38 N2 1.420(10) . ?
C39 N2 1.403(8) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 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 C1 C10 123.3(7) . . ?
C2 C1 H1 118.4 . . ?
C10 C1 H1 118.4 . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 119.0(6) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.9(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C10 C5 C4 120.7(7) . . ?
C10 C5 C6 120.5(7) . . ?
C4 C5 C6 118.8(6) . . ?
C5 C6 C7 109.7(5) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C6 109.2(7) . . ?
C8 C7 H7A 109.9 . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
C9 C8 C7 124.0(7) . . ?
C9 C8 H8 118.0 . . ?
C7 C8 H8 118.0 . . ?
C8 C9 C11 123.2(6) . . ?
C8 C9 C10 117.4(6) . . ?
C11 C9 C10 119.4(5) . . ?
C1 C10 C5 115.5(6) . . ?
C1 C10 C9 124.2(5) . . ?
C5 C10 C9 119.4(6) . . ?
C18 C11 C9 126.0(8) . . ?
C18 C11 C12 105.9(7) . . ?
C9 C11 C12 128.0(7) . . ?
C13 C12 C17 118.8(7) . . ?
C13 C12 C11 134.4(7) . . ?
C17 C12 C11 106.8(6) . . ?
C12 C13 C14 118.2(7) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C15 C14 C13 119.0(8) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 125.5(9) . . ?
C14 C15 H15 117.2 . . ?
C16 C15 H15 117.3 . . ?
C15 C16 C17 118.3(7) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.9 . . ?
N1 C17 C16 132.4(7) . . ?
N1 C17 C12 107.5(7) . . ?
C16 C17 C12 120.1(7) . . ?
N1 C18 C11 108.6(7) . . ?
N1 C18 C19 120.7(6) . . ?
C11 C18 C19 130.5(7) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.4 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 121.6(5) . . ?
C26 C21 C40 119.3(6) . . ?
C22 C21 C40 119.0(6) . . ?
C23 C22 C21 116.1(7) . . ?
C23 C22 H22 122.0 . . ?
C21 C22 H22 122.0 . . ?
C24 C23 C22 122.6(7) . . ?
C24 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
C23 C24 C25 118.7(8) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.6 . . ?
C26 C25 C24 122.6(8) . . ?
C26 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
C25 C26 C21 118.3(6) . . ?
C25 C26 C27 124.1(7) . . ?
C21 C26 C27 117.5(5) . . ?
C28 C27 C26 112.0(6) . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
C26 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C27 C28 C29 111.6(8) . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C29 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
C40 C29 C28 121.7(6) . . ?
C40 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C31 C30 C33 106.9(6) . . ?
C31 C30 C40 126.4(6) . . ?
C33 C30 C40 126.7(6) . . ?
C30 C31 N2 111.3(6) . . ?
C30 C31 C32 128.6(6) . . ?
N2 C31 C32 119.9(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 117.2(7) . . ?
C34 C33 C30 136.0(6) . . ?
C38 C33 C30 106.8(6) . . ?
C35 C34 C33 123.3(8) . . ?
C35 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?
C34 C35 C36 119.8(8) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 119.0(7) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C38 C37 C36 115.4(7) . . ?
C38 C37 H37 122.3 . . ?
C36 C37 H37 122.3 . . ?
C37 C38 C33 125.2(8) . . ?
C37 C38 N2 126.3(6) . . ?
C33 C38 N2 108.5(6) . . ?
N2 C39 H39A 109.5 . . ?
N2 C39 H39B 109.4 . . ?
H39A C39 H39B 109.5 . . ?
N2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C29 C40 C21 119.5(7) . . ?
C29 C40 C30 119.9(6) . . ?
C21 C40 C30 120.4(6) . . ?
C17 N1 C18 111.1(5) . . ?
C17 N1 C20 122.8(7) . . ?
C18 N1 C20 126.1(7) . . ?
C31 N2 C39 123.1(7) . . ?
C31 N2 C38 106.4(5) . . ?
C39 N2 C38 130.2(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C1 C2 C3 -9.4(17) . . . . ?
C1 C2 C3 C4 3.0(17) . . . . ?
C2 C3 C4 C5 1.7(15) . . . . ?
C3 C4 C5 C10 -0.6(14) . . . . ?
C3 C4 C5 C6 176.8(9) . . . . ?
C10 C5 C6 C7 -39.6(11) . . . . ?
C4 C5 C6 C7 142.9(8) . . . . ?
C5 C6 C7 C8 49.8(10) . . . . ?
C6 C7 C8 C9 -35.0(11) . . . . ?
C7 C8 C9 C11 -176.4(7) . . . . ?
C7 C8 C9 C10 3.7(11) . . . . ?
C2 C1 C10 C5 10.0(14) . . . . ?
C2 C1 C10 C9 178.8(9) . . . . ?
C4 C5 C10 C1 -5.0(13) . . . . ?
C6 C5 C10 C1 177.6(8) . . . . ?
C4 C5 C10 C9 -174.3(8) . . . . ?
C6 C5 C10 C9 8.3(12) . . . . ?
C8 C9 C10 C1 -156.6(8) . . . . ?
C11 C9 C10 C1 23.4(12) . . . . ?
C8 C9 C10 C5 11.7(11) . . . . ?
C11 C9 C10 C5 -168.2(7) . . . . ?
C8 C9 C11 C18 46.3(11) . . . . ?
C10 C9 C11 C18 -133.8(7) . . . . ?
C8 C9 C11 C12 -132.6(8) . . . . ?
C10 C9 C11 C12 47.4(10) . . . . ?
C18 C11 C12 C13 179.2(8) . . . . ?
C9 C11 C12 C13 -1.7(13) . . . . ?
C18 C11 C12 C17 0.0(8) . . . . ?
C9 C11 C12 C17 179.1(6) . . . . ?
C17 C12 C13 C14 -1.9(10) . . . . ?
C11 C12 C13 C14 179.0(8) . . . . ?
C12 C13 C14 C15 -0.5(12) . . . . ?
C13 C14 C15 C16 3.3(14) . . . . ?
C14 C15 C16 C17 -3.3(13) . . . . ?
C15 C16 C17 N1 -178.4(7) . . . . ?
C15 C16 C17 C12 0.6(11) . . . . ?
C13 C12 C17 N1 -178.9(6) . . . . ?
C11 C12 C17 N1 0.4(8) . . . . ?
C13 C12 C17 C16 1.9(10) . . . . ?
C11 C12 C17 C16 -178.8(6) . . . . ?
C9 C11 C18 N1 -179.5(6) . . . . ?
C12 C11 C18 N1 -0.5(8) . . . . ?
C9 C11 C18 C19 5.6(12) . . . . ?
C12 C11 C18 C19 -175.3(7) . . . . ?
C26 C21 C22 C23 1.8(10) . . . . ?
C40 C21 C22 C23 -177.6(7) . . . . ?
C21 C22 C23 C24 -2.1(14) . . . . ?
C22 C23 C24 C25 -0.1(17) . . . . ?
C23 C24 C25 C26 2.8(17) . . . . ?
C24 C25 C26 C21 -3.0(14) . . . . ?
C24 C25 C26 C27 180.0(10) . . . . ?
C22 C21 C26 C25 0.6(11) . . . . ?
C40 C21 C26 C25 -179.9(7) . . . . ?
C22 C21 C26 C27 177.8(7) . . . . ?
C40 C21 C26 C27 -2.7(10) . . . . ?
C25 C26 C27 C28 -147.3(9) . . . . ?
C21 C26 C27 C28 35.6(11) . . . . ?
C26 C27 C28 C29 -48.3(10) . . . . ?
C27 C28 C29 C40 31.3(12) . . . . ?
C33 C30 C31 N2 -1.6(7) . . . . ?
C40 C30 C31 N2 177.1(6) . . . . ?
C33 C30 C31 C32 -176.5(7) . . . . ?
C40 C30 C31 C32 2.1(11) . . . . ?
C31 C30 C33 C34 -179.8(7) . . . . ?
C40 C30 C33 C34 1.6(12) . . . . ?
C31 C30 C33 C38 0.3(7) . . . . ?
C40 C30 C33 C38 -178.4(6) . . . . ?
C38 C33 C34 C35 -2.7(10) . . . . ?
C30 C33 C34 C35 177.4(7) . . . . ?
C33 C34 C35 C36 0.5(11) . . . . ?
C34 C35 C36 C37 1.8(11) . . . . ?
C35 C36 C37 C38 -1.8(10) . . . . ?
C36 C37 C38 C33 -0.5(10) . . . . ?
C36 C37 C38 N2 -178.6(6) . . . . ?
C34 C33 C38 C37 2.7(10) . . . . ?
C30 C33 C38 C37 -177.3(6) . . . . ?
C34 C33 C38 N2 -178.9(5) . . . . ?
C30 C33 C38 N2 1.1(7) . . . . ?
C28 C29 C40 C21 2.1(12) . . . . ?
C28 C29 C40 C30 177.8(7) . . . . ?
C26 C21 C40 C29 -17.3(11) . . . . ?
C22 C21 C40 C29 162.1(7) . . . . ?
C26 C21 C40 C30 167.0(6) . . . . ?
C22 C21 C40 C30 -13.5(10) . . . . ?
C31 C30 C40 C29 -45.7(11) . . . . ?
C33 C30 C40 C29 132.7(8) . . . . ?
C31 C30 C40 C21 129.9(7) . . . . ?
C33 C30 C40 C21 -51.7(10) . . . . ?
C16 C17 N1 C18 178.3(7) . . . . ?
C12 C17 N1 C18 -0.8(8) . . . . ?
C16 C17 N1 C20 -0.8(12) . . . . ?
C12 C17 N1 C20 -179.9(5) . . . . ?
C11 C18 N1 C17 0.8(8) . . . . ?
C19 C18 N1 C17 176.2(6) . . . . ?
C11 C18 N1 C20 179.9(6) . . . . ?
C19 C18 N1 C20 -4.7(10) . . . . ?
C30 C31 N2 C39 177.6(7) . . . . ?
C32 C31 N2 C39 -7.0(10) . . . . ?
C30 C31 N2 C38 2.2(7) . . . . ?
C32 C31 N2 C38 177.7(6) . . . . ?
C37 C38 N2 C31 176.4(6) . . . . ?
C33 C38 N2 C31 -2.0(7) . . . . ?
C37 C38 N2 C39 1.5(12) . . . . ?
C33 C38 N2 C39 -176.9(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.865
_diffrn_reflns_theta_full        31.11
_diffrn_measured_fraction_theta_full 0.865
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.177
_database_code_depnum_ccdc_archive 'CCDC 1000776'
