# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Paul Evans'
_publ_contact_author_email       PAUL.EVANS@UCD.IE

_publ_section_title              
;
Selective Generation of Quaternary
All-Carbon-Centres Through Heck-Cyclisations: Application
to the Total Synthesis of Mesembrane
;
loop_
_publ_author_name
'Paul Evans'
'Kimberly Geoghegan'
'Johannes E. M. N. Klein'
'Nicolas Meral'

# Attachment 'eva49.cif'

data_eva49
_database_code_depnum_ccdc_archive 'CCDC 742478'
#TrackingRef 'eva49.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H19 N O4 S'
_chemical_formula_sum            'C16 H19 N O4 S'
_chemical_formula_weight         321.38

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   9.8281(12)
_cell_length_b                   14.6214(18)
_cell_length_c                   10.9381(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.548(2)
_cell_angle_gamma                90.00
_cell_volume                     1471.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3777
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      26.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) for selected reflections was 0.040 before and 0.024 after
correction. The Ratio of minimum to maximum transmission is 0.872500.
The \l/2 correction factor is 0.0015
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.74450
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10783
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         26.35
_reflns_number_total             2600
_reflns_number_gt                2329
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_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^)+(0.0496P)^2^+1.1370P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2600
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
S S 0.31517(6) 0.12923(4) 0.79465(6) 0.02664(19) Uani 1 1 d . . .
O1 O 0.35445(19) 0.11011(11) 0.93110(17) 0.0342(4) Uani 1 1 d . . .
O2 O 0.17456(18) 0.10185(12) 0.70934(18) 0.0346(4) Uani 1 1 d . . .
N N 0.3277(2) 0.24180(13) 0.77743(19) 0.0281(5) Uani 1 1 d . . .
C1 C 0.4490(2) 0.08480(16) 0.7366(2) 0.0245(5) Uani 1 1 d . . .
C2 C 0.4762(2) -0.00865(17) 0.7513(2) 0.0253(5) Uani 1 1 d . . .
H2 H 0.429(2) -0.0436(16) 0.790(2) 0.018(6) Uiso 1 1 d . . .
C3 C 0.5761(2) -0.04858(15) 0.7052(2) 0.0247(5) Uani 1 1 d . . .
O3 O 0.61059(17) -0.13880(10) 0.71214(16) 0.0281(4) Uani 1 1 d . . .
C7 C 0.5316(3) -0.19827(17) 0.7680(3) 0.0294(5) Uani 1 1 d . . .
H7A H 0.427(3) -0.1938(16) 0.720(2) 0.024(6) Uiso 1 1 d . . .
H7B H 0.550(3) -0.1824(17) 0.859(3) 0.033(7) Uiso 1 1 d . . .
H7C H 0.565(3) -0.261(2) 0.764(3) 0.036(7) Uiso 1 1 d . . .
C4 C 0.6506(2) 0.00747(16) 0.6452(2) 0.0245(5) Uani 1 1 d . . .
C5 C 0.6231(2) 0.10034(16) 0.6321(2) 0.0243(5) Uani 1 1 d . . .
H5 H 0.672(3) 0.1367(16) 0.593(2) 0.023(6) Uiso 1 1 d . . .
O4 O 0.74704(17) -0.03694(11) 0.60280(16) 0.0286(4) Uani 1 1 d . . .
C8 C 0.8419(3) 0.01755(18) 0.5585(3) 0.0331(6) Uani 1 1 d . . .
H8A H 0.787(3) 0.0493(18) 0.484(3) 0.030(7) Uiso 1 1 d . . .
H8B H 0.900(3) 0.0588(19) 0.624(3) 0.033(7) Uiso 1 1 d . . .
H8C H 0.905(3) -0.0267(19) 0.539(2) 0.036(7) Uiso 1 1 d . . .
C6 C 0.5214(2) 0.14174(15) 0.6769(2) 0.0237(5) Uani 1 1 d . . .
C9 C 0.4942(2) 0.24488(16) 0.6655(2) 0.0258(5) Uani 1 1 d . . .
C10 C 0.3324(3) 0.26192(16) 0.6436(2) 0.0278(5) Uani 1 1 d . . .
H10 H 0.263(2) 0.2186(15) 0.577(2) 0.016(5) Uiso 1 1 d . . .
C11 C 0.4690(3) 0.27674(16) 0.8650(2) 0.0286(5) Uani 1 1 d . . .
H11 H 0.476(3) 0.2909(16) 0.955(2) 0.025(6) Uiso 1 1 d . . .
C12 C 0.5624(3) 0.28398(16) 0.8044(2) 0.0270(5) Uani 1 1 d . . .
H12 H 0.667(3) 0.3040(17) 0.845(3) 0.030(7) Uiso 1 1 d . . .
C13 C 0.5453(3) 0.29065(16) 0.5636(2) 0.0275(5) Uani 1 1 d . . .
H13A H 0.651(3) 0.2887(17) 0.594(2) 0.029(6) Uiso 1 1 d . . .
H13B H 0.511(3) 0.2536(17) 0.486(3) 0.026(6) Uiso 1 1 d . . .
C14 C 0.4934(3) 0.38910(17) 0.5359(3) 0.0317(6) Uani 1 1 d . . .
H14A H 0.525(3) 0.4118(17) 0.463(2) 0.027(6) Uiso 1 1 d . . .
H14B H 0.538(3) 0.4266(19) 0.620(3) 0.035(7) Uiso 1 1 d . . .
C15 C 0.3286(3) 0.39463(19) 0.4958(3) 0.0344(6) Uani 1 1 d . . .
H15A H 0.283(3) 0.3558(18) 0.418(3) 0.030(7) Uiso 1 1 d . . .
H15B H 0.288(3) 0.459(2) 0.467(3) 0.047(8) Uiso 1 1 d . . .
C16 C 0.2800(3) 0.35904(17) 0.6045(3) 0.0313(6) Uani 1 1 d . . .
H16A H 0.176(3) 0.3581(16) 0.576(2) 0.023(6) Uiso 1 1 d . . .
H16B H 0.319(3) 0.3971(18) 0.685(3) 0.031(7) Uiso 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
S 0.0268(3) 0.0260(3) 0.0306(3) -0.0022(2) 0.0144(2) -0.0013(2)
O1 0.0432(10) 0.0316(9) 0.0350(10) 0.0009(7) 0.0228(8) 0.0000(8)
O2 0.0274(9) 0.0353(10) 0.0450(11) -0.0062(8) 0.0175(8) -0.0026(7)
N 0.0301(11) 0.0262(11) 0.0300(11) -0.0003(8) 0.0132(9) 0.0013(8)
C1 0.0224(11) 0.0266(12) 0.0249(12) -0.0019(9) 0.0085(9) 0.0006(9)
C2 0.0226(12) 0.0289(13) 0.0248(12) 0.0004(10) 0.0086(10) -0.0050(10)
C3 0.0240(11) 0.0229(12) 0.0237(12) -0.0015(9) 0.0040(9) -0.0009(9)
O3 0.0295(9) 0.0213(9) 0.0360(10) 0.0007(7) 0.0146(7) -0.0007(6)
C7 0.0350(15) 0.0262(13) 0.0312(14) 0.0010(11) 0.0167(12) -0.0022(10)
C4 0.0213(11) 0.0269(12) 0.0244(12) -0.0033(9) 0.0071(9) -0.0010(9)
C5 0.0221(11) 0.0262(12) 0.0244(12) 0.0015(9) 0.0077(10) -0.0023(9)
O4 0.0283(9) 0.0249(8) 0.0382(10) -0.0003(7) 0.0186(8) -0.0005(7)
C8 0.0322(14) 0.0271(13) 0.0472(17) -0.0010(13) 0.0229(13) -0.0004(11)
C6 0.0223(11) 0.0251(12) 0.0222(11) -0.0015(9) 0.0057(9) -0.0012(9)
C9 0.0251(12) 0.0248(12) 0.0272(13) -0.0010(9) 0.0087(10) -0.0001(9)
C10 0.0247(12) 0.0290(13) 0.0290(13) -0.0026(10) 0.0088(10) -0.0020(10)
C11 0.0309(13) 0.0245(12) 0.0285(13) -0.0032(10) 0.0081(11) -0.0001(10)
C12 0.0291(13) 0.0220(12) 0.0272(13) -0.0014(9) 0.0064(10) 0.0011(10)
C13 0.0274(13) 0.0255(12) 0.0289(13) 0.0002(10) 0.0089(10) -0.0028(10)
C14 0.0334(13) 0.0272(13) 0.0342(14) 0.0032(11) 0.0115(11) 0.0002(10)
C15 0.0343(14) 0.0290(14) 0.0348(15) 0.0048(11) 0.0060(11) 0.0034(11)
C16 0.0257(13) 0.0301(13) 0.0352(14) 0.0006(11) 0.0070(11) 0.0026(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
S O2 1.4267(18) . ?
S O1 1.4319(18) . ?
S N 1.666(2) . ?
S C1 1.772(2) . ?
N C11 1.474(3) . ?
N C10 1.509(3) . ?
C1 C2 1.391(3) . ?
C1 C6 1.397(3) . ?
C2 C3 1.381(3) . ?
C2 H2 0.89(2) . ?
C3 O3 1.357(3) . ?
C3 C4 1.406(3) . ?
O3 C7 1.437(3) . ?
C7 H7A 0.98(3) . ?
C7 H7B 0.98(3) . ?
C7 H7C 0.98(3) . ?
C4 O4 1.358(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.396(3) . ?
C5 H5 0.91(3) . ?
O4 C8 1.433(3) . ?
C8 H8A 0.93(3) . ?
C8 H8B 0.95(3) . ?
C8 H8C 0.97(3) . ?
C6 C9 1.529(3) . ?
C9 C13 1.528(3) . ?
C9 C12 1.540(3) . ?
C9 C10 1.543(3) . ?
C10 C16 1.520(3) . ?
C10 H10 1.02(2) . ?
C11 C12 1.312(3) . ?
C11 H11 0.98(2) . ?
C12 H12 1.01(3) . ?
C13 C14 1.522(3) . ?
C13 H13A 0.98(3) . ?
C13 H13B 0.96(3) . ?
C14 C15 1.524(4) . ?
C14 H14A 1.01(3) . ?
C14 H14B 1.03(3) . ?
C15 C16 1.521(4) . ?
C15 H15A 0.99(3) . ?
C15 H15B 1.03(3) . ?
C16 H16A 0.96(3) . ?
C16 H16B 0.99(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 S O1 118.15(11) . . ?
O2 S N 107.25(11) . . ?
O1 S N 107.88(10) . . ?
O2 S C1 109.46(10) . . ?
O1 S C1 109.83(11) . . ?
N S C1 103.16(10) . . ?
C11 N C10 102.75(18) . . ?
C11 N S 111.05(15) . . ?
C10 N S 109.32(15) . . ?
C2 C1 C6 122.1(2) . . ?
C2 C1 S 117.08(17) . . ?
C6 C1 S 120.85(17) . . ?
C3 C2 C1 120.4(2) . . ?
C3 C2 H2 119.1(15) . . ?
C1 C2 H2 120.5(15) . . ?
O3 C3 C2 125.9(2) . . ?
O3 C3 C4 115.6(2) . . ?
C2 C3 C4 118.5(2) . . ?
C3 O3 C7 116.75(18) . . ?
O3 C7 H7A 110.5(14) . . ?
O3 C7 H7B 110.9(15) . . ?
H7A C7 H7B 109(2) . . ?
O3 C7 H7C 107.7(15) . . ?
H7A C7 H7C 110(2) . . ?
H7B C7 H7C 109(2) . . ?
O4 C4 C5 124.7(2) . . ?
O4 C4 C3 114.9(2) . . ?
C5 C4 C3 120.4(2) . . ?
C4 C5 C6 121.8(2) . . ?
C4 C5 H5 120.4(15) . . ?
C6 C5 H5 117.8(15) . . ?
C4 O4 C8 117.66(18) . . ?
O4 C8 H8A 109.0(16) . . ?
O4 C8 H8B 112.9(16) . . ?
H8A C8 H8B 110(2) . . ?
O4 C8 H8C 104.0(16) . . ?
H8A C8 H8C 111(2) . . ?
H8B C8 H8C 109(2) . . ?
C5 C6 C1 116.8(2) . . ?
C5 C6 C9 121.7(2) . . ?
C1 C6 C9 121.5(2) . . ?
C13 C9 C6 113.47(19) . . ?
C13 C9 C12 114.6(2) . . ?
C6 C9 C12 106.44(18) . . ?
C13 C9 C10 113.6(2) . . ?
C6 C9 C10 108.25(18) . . ?
C12 C9 C10 99.28(18) . . ?
N C10 C16 109.42(19) . . ?
N C10 C9 101.45(18) . . ?
C16 C10 C9 115.1(2) . . ?
N C10 H10 109.6(12) . . ?
C16 C10 H10 107.6(12) . . ?
C9 C10 H10 113.4(12) . . ?
C12 C11 N 111.5(2) . . ?
C12 C11 H11 132.1(14) . . ?
N C11 H11 116.5(14) . . ?
C11 C12 C9 109.2(2) . . ?
C11 C12 H12 126.1(15) . . ?
C9 C12 H12 124.2(15) . . ?
C14 C13 C9 112.8(2) . . ?
C14 C13 H13A 109.8(15) . . ?
C9 C13 H13A 108.8(15) . . ?
C14 C13 H13B 111.5(15) . . ?
C9 C13 H13B 107.1(15) . . ?
H13A C13 H13B 107(2) . . ?
C13 C14 C15 110.8(2) . . ?
C13 C14 H14A 107.2(14) . . ?
C15 C14 H14A 110.3(14) . . ?
C13 C14 H14B 108.6(15) . . ?
C15 C14 H14B 108.0(15) . . ?
H14A C14 H14B 112(2) . . ?
C16 C15 C14 110.5(2) . . ?
C16 C15 H15A 107.6(15) . . ?
C14 C15 H15A 109.4(15) . . ?
C16 C15 H15B 111.2(16) . . ?
C14 C15 H15B 113.2(16) . . ?
H15A C15 H15B 105(2) . . ?
C10 C16 C15 111.8(2) . . ?
C10 C16 H16A 107.2(14) . . ?
C15 C16 H16A 110.1(14) . . ?
C10 C16 H16B 106.6(15) . . ?
C15 C16 H16B 111.6(15) . . ?
H16A C16 H16B 109(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
O2 S N C11 178.49(15) . . . . ?
O1 S N C11 50.22(18) . . . . ?
C1 S N C11 -65.99(17) . . . . ?
O2 S N C10 -68.83(17) . . . . ?
O1 S N C10 162.90(15) . . . . ?
C1 S N C10 46.70(17) . . . . ?
O2 S C1 C2 -72.8(2) . . . . ?
O1 S C1 C2 58.5(2) . . . . ?
N S C1 C2 173.31(17) . . . . ?
O2 S C1 C6 106.2(2) . . . . ?
O1 S C1 C6 -122.56(19) . . . . ?
N S C1 C6 -7.7(2) . . . . ?
C6 C1 C2 C3 -0.7(3) . . . . ?
S C1 C2 C3 178.21(17) . . . . ?
C1 C2 C3 O3 -179.1(2) . . . . ?
C1 C2 C3 C4 0.9(3) . . . . ?
C2 C3 O3 C7 2.6(3) . . . . ?
C4 C3 O3 C7 -177.4(2) . . . . ?
O3 C3 C4 O4 -0.2(3) . . . . ?
C2 C3 C4 O4 179.87(19) . . . . ?
O3 C3 C4 C5 179.5(2) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
O4 C4 C5 C6 179.4(2) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C5 C4 O4 C8 9.4(3) . . . . ?
C3 C4 O4 C8 -170.9(2) . . . . ?
C4 C5 C6 C1 0.5(3) . . . . ?
C4 C5 C6 C9 178.4(2) . . . . ?
C2 C1 C6 C5 0.0(3) . . . . ?
S C1 C6 C5 -178.87(16) . . . . ?
C2 C1 C6 C9 -177.9(2) . . . . ?
S C1 C6 C9 3.3(3) . . . . ?
C5 C6 C9 C13 19.8(3) . . . . ?
C1 C6 C9 C13 -162.4(2) . . . . ?
C5 C6 C9 C12 -107.2(2) . . . . ?
C1 C6 C9 C12 70.6(3) . . . . ?
C5 C6 C9 C10 146.9(2) . . . . ?
C1 C6 C9 C10 -35.3(3) . . . . ?
C11 N C10 C16 -85.9(2) . . . . ?
S N C10 C16 156.06(16) . . . . ?
C11 N C10 C9 36.1(2) . . . . ?
S N C10 C9 -81.95(18) . . . . ?
C13 C9 C10 N -159.80(19) . . . . ?
C6 C9 C10 N 73.2(2) . . . . ?
C12 C9 C10 N -37.7(2) . . . . ?
C13 C9 C10 C16 -41.8(3) . . . . ?
C6 C9 C10 C16 -168.8(2) . . . . ?
C12 C9 C10 C16 80.3(2) . . . . ?
C10 N C11 C12 -20.3(3) . . . . ?
S N C11 C12 96.5(2) . . . . ?
N C11 C12 C9 -5.0(3) . . . . ?
C13 C9 C12 C11 148.8(2) . . . . ?
C6 C9 C12 C11 -84.9(2) . . . . ?
C10 C9 C12 C11 27.4(2) . . . . ?
C6 C9 C13 C14 169.6(2) . . . . ?
C12 C9 C13 C14 -67.8(3) . . . . ?
C10 C9 C13 C14 45.3(3) . . . . ?
C9 C13 C14 C15 -55.2(3) . . . . ?
C13 C14 C15 C16 60.7(3) . . . . ?
N C10 C16 C15 160.7(2) . . . . ?
C9 C10 C16 C15 47.3(3) . . . . ?
C14 C15 C16 C10 -56.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.051