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

 
data_R6
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          
'C16 H13 N O4' 
_chemical_formula_sum 
 'C16 H13 N O4' 
_chemical_formula_weight          283.27 
 
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_Hall      '-C 2yc'
_symmetry_space_group_name_H-M       'C 2/c'
_symmetry_Int_Tables_number                 15
 
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                    32.374(8) 
_cell_length_b                    5.4040(12) 
_cell_length_c                    16.122(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  114.805(9) 
_cell_angle_gamma                 90.00 
_cell_volume                      2560.3(10) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     261(2) 
_cell_measurement_reflns_used     825 
_cell_measurement_theta_min       2.77 
_cell_measurement_theta_max       20.80 
 
_exptl_crystal_description        'plate' 
_exptl_crystal_colour             'colourless' 
_exptl_crystal_size_max           0.28 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.470 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1184 
_exptl_absorpt_coefficient_mu     0.107 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9707 
_exptl_absorpt_correction_T_max   0.9873 
_exptl_absorpt_process_details    SADABS 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       261(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_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             21895 
_diffrn_reflns_av_R_equivalents   0.6463 
_diffrn_reflns_av_sigmaI/netI     0.3255 
_diffrn_reflns_limit_h_min        -42 
_diffrn_reflns_limit_h_max        41 
_diffrn_reflns_limit_k_min        -6 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.54 
_diffrn_reflns_theta_max          27.66 
_reflns_number_total              2953 
_reflns_number_gt                 1072 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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)+(0.0177P)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     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2953 
_refine_ls_number_parameters      192 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2715 
_refine_ls_R_factor_gt            0.0792 
_refine_ls_wR_factor_ref          0.1825 
_refine_ls_wR_factor_gt           0.1300 
_refine_ls_goodness_of_fit_ref    0.951 
_refine_ls_restrained_S_all       0.951 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 

_iucr_refine_instruction_details
;
TITL R6_C in C2/c
CELL 0.71073 32.3736 5.4040 16.1220 90.000 114.805 90.000
ZERR 8.00 0.0080 0.0012 0.0036 0.000 0.009 0.000
LATT 7
SYMM -x, y, -z+1/2
SFAC C H N O
UNIT 128 104 8 32
TEMP -105.950
ACTA
TEMP -12
SIZE 0.28 0.18 0.12
L.S. 12
FMAP 2
PLAN 5
BOND $H
HTAB
CONF
WGHT    0.017700
FVAR       0.06913
N1    3    0.176451    0.629954    0.137972    11.00000    0.01676    0.02575 =
         0.01681    0.00282    0.00233   -0.00218
AFIX  43
H1    2    0.200542    0.591816    0.185723    11.00000   -1.20000
AFIX   0
O1    4    0.028336    0.894132   -0.127945    11.00000    0.06044    0.06892 =
         0.03769   -0.02139   -0.01562    0.04118
O2    4    0.014852    1.242380   -0.072181    11.00000    0.02509    0.05088 =
         0.02789   -0.00342   -0.00045    0.01730
O3    4    0.243586    0.260148    0.176203    11.00000    0.02154    0.03160 =
         0.01941   -0.00130    0.00566    0.00073
O4    4    0.236243    0.000262    0.062046    11.00000    0.02562    0.03188 =
         0.02078    0.00154    0.00497    0.01402
 
C1    1    0.161844    0.514247    0.055274    11.00000    0.01580    0.02763 =
         0.01736    0.00111    0.00714   -0.00367
C2    1    0.121594    0.630001   -0.007350    11.00000    0.01252    0.02403 =
         0.02570   -0.00256    0.00899   -0.00268
C3    1    0.100911    0.538010   -0.096589    11.00000    0.02052    0.03241 =
         0.01538   -0.00019    0.00624   -0.00021
AFIX  43
H3    2    0.074619    0.611369   -0.139383    11.00000   -1.20000
AFIX   0
C4    1    0.120010    0.336691   -0.120456    11.00000    0.02349    0.03789 =
         0.01470    0.00037    0.00587   -0.00065
AFIX  43
H4    2    0.106030    0.274342   -0.179577    11.00000   -1.20000
AFIX   0
C5    1    0.159230    0.226347   -0.058779    11.00000    0.02434    0.02820 =
         0.02395   -0.00247    0.01330    0.00449
AFIX  43
H5    2    0.171009    0.090746   -0.077151    11.00000   -1.20000
AFIX   0
C6    1    0.181793    0.313535    0.030960    11.00000    0.01717    0.02573 =
         0.02025    0.00248    0.00591   -0.00007
C7    1    0.146438    0.818616    0.133127    11.00000    0.01921    0.02321 =
         0.01804    0.00108    0.00727    0.00090
C8    1    0.111054    0.826075    0.043161    11.00000    0.01824    0.02214 =
         0.01921   -0.00123    0.00874   -0.00661
C9    1    0.077592    1.010312    0.025078    11.00000    0.01493    0.02677 =
         0.02443    0.00309    0.00713    0.00279
C10   1    0.080629    1.172279    0.094120    11.00000    0.02186    0.02993 =
         0.02453    0.00033    0.00883   -0.00039
AFIX  43
H10   2    0.058809    1.295615    0.081781    11.00000   -1.20000
AFIX   0
C11   1    0.115920    1.154183    0.182245    11.00000    0.03704    0.02500 =
         0.02969   -0.00746    0.01868   -0.00522
AFIX  43
H11   2    0.116854    1.264136    0.227375    11.00000   -1.20000
AFIX   0
C12   1    0.149016    0.976819    0.202728    11.00000    0.02186    0.03155 =
         0.02120   -0.00234    0.00883   -0.00513
AFIX  43
H12   2    0.172312    0.963223    0.261130    11.00000   -1.20000
AFIX   0
C13   1    0.038844    1.037025   -0.065852    11.00000    0.02136    0.03022 =
         0.02541    0.00383    0.01145    0.00882
C14   1   -0.022892    1.293215   -0.157636    11.00000    0.02323    0.04836 =
         0.03332   -0.00006    0.00915    0.01151
AFIX 137
H14A  2   -0.024524    1.168604   -0.201346    11.00000   -1.50000
H14B  2   -0.018884    1.452557   -0.179551    11.00000   -1.50000
H14C  2   -0.050551    1.292535   -0.149252    11.00000   -1.50000
AFIX   0
C15   1    0.223137    0.192913    0.097219    11.00000    0.01683    0.02507 =
         0.02719    0.00165    0.01131   -0.00046
C16   1    0.275061   -0.135740    0.125111    11.00000    0.02746    0.04089 =
         0.03100    0.00233    0.01139    0.01312
AFIX 137
H16A  2    0.301289   -0.029842    0.147586    11.00000   -1.50000
H16B  2    0.280678   -0.275080    0.094354    11.00000   -1.50000
H16C  2    0.269048   -0.192803    0.175361    11.00000   -1.50000
HKLF   4
 
REM  R6_C in C2/c
REM R1 =  0.0792 for   1072 Fo > 4sig(Fo)  and  0.2715 for all   2953 data
REM    192 parameters refined using      0 restraints
 
END  
     
WGHT      0.0177      0.0000 
REM Highest difference peak  0.337,  deepest hole -0.309,  1-sigma level  0.073
Q1    1   0.1983  0.7988  0.2305  11.00000  0.05    0.34
Q2    1  -0.0340  1.5174 -0.1435  11.00000  0.05    0.30
Q3    1   0.1483 -0.0150 -0.0496  11.00000  0.05    0.28
Q4    1   0.1349  1.1669  0.1906  11.00000  0.05    0.26
Q5    1   0.2129  0.9110  0.3142  11.00000  0.05    0.26
;
 
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 0.17645(11) 0.6300(6) 0.1380(2) 0.0214(9) Uani 1 1 d . . . 
H1 H 0.2005 0.5918 0.1857 0.026 Uiso 1 1 calc R . . 
O1 O 0.02834(12) 0.8941(8) -0.1279(3) 0.0680(13) Uani 1 1 d . . . 
O2 O 0.01485(9) 1.2424(6) -0.0722(2) 0.0385(10) Uani 1 1 d . . . 
O3 O 0.24359(9) 0.2601(5) 0.1762(2) 0.0252(8) Uani 1 1 d . . . 
O4 O 0.23624(9) 0.0003(6) 0.0620(2) 0.0277(8) Uani 1 1 d . . . 
C1 C 0.16184(13) 0.5142(9) 0.0553(3) 0.0202(11) Uani 1 1 d . . . 
C2 C 0.12159(12) 0.6300(8) -0.0073(3) 0.0204(11) Uani 1 1 d . . . 
C3 C 0.10091(13) 0.5380(9) -0.0966(3) 0.0232(11) Uani 1 1 d . . . 
H3 H 0.0746 0.6114 -0.1394 0.028 Uiso 1 1 calc R . . 
C4 C 0.12001(14) 0.3367(9) -0.1205(3) 0.0261(12) Uani 1 1 d . . . 
H4 H 0.1060 0.2743 -0.1796 0.031 Uiso 1 1 calc R . . 
C5 C 0.15923(13) 0.2263(8) -0.0588(3) 0.0244(12) Uani 1 1 d . . . 
H5 H 0.1710 0.0907 -0.0772 0.029 Uiso 1 1 calc R . . 
C6 C 0.18179(13) 0.3135(9) 0.0310(3) 0.0217(11) Uani 1 1 d . . . 
C7 C 0.14644(13) 0.8186(8) 0.1331(3) 0.0203(11) Uani 1 1 d . . . 
C8 C 0.11105(13) 0.8261(8) 0.0432(3) 0.0196(11) Uani 1 1 d . . . 
C9 C 0.07759(13) 1.0103(9) 0.0251(3) 0.0224(11) Uani 1 1 d . . . 
C10 C 0.08063(14) 1.1723(9) 0.0941(3) 0.0257(12) Uani 1 1 d . . . 
H10 H 0.0588 1.2956 0.0818 0.031 Uiso 1 1 calc R . . 
C11 C 0.11592(14) 1.1542(9) 0.1822(3) 0.0290(12) Uani 1 1 d . . . 
H11 H 0.1169 1.2641 0.2274 0.035 Uiso 1 1 calc R . . 
C12 C 0.14902(13) 0.9768(8) 0.2027(3) 0.0249(12) Uani 1 1 d . . . 
H12 H 0.1723 0.9632 0.2611 0.030 Uiso 1 1 calc R . . 
C13 C 0.03884(14) 1.0370(9) -0.0659(3) 0.0251(12) Uani 1 1 d . . . 
C14 C -0.02289(14) 1.2932(9) -0.1576(3) 0.0359(14) Uani 1 1 d . . . 
H14A H -0.0245 1.1686 -0.2013 0.054 Uiso 1 1 calc R . . 
H14B H -0.0189 1.4526 -0.1796 0.054 Uiso 1 1 calc R . . 
H14C H -0.0506 1.2925 -0.1493 0.054 Uiso 1 1 calc R . . 
C15 C 0.22314(14) 0.1929(9) 0.0972(3) 0.0223(11) Uani 1 1 d . . . 
C16 C 0.27506(14) -0.1357(9) 0.1251(3) 0.0334(13) Uani 1 1 d . . . 
H16A H 0.3013 -0.0298 0.1476 0.050 Uiso 1 1 calc R . . 
H16B H 0.2807 -0.2751 0.0944 0.050 Uiso 1 1 calc R . . 
H16C H 0.2690 -0.1928 0.1754 0.050 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 C1 1.365(5) . ? 
N1 C7 1.388(5) . ? 
N1 H1 0.8600 . ? 
O1 C13 1.195(5) . ? 
O2 C13 1.334(5) . ? 
O2 C14 1.433(5) . ? 
O3 C15 1.218(5) . ? 
O4 C15 1.337(5) . ? 
O4 C16 1.443(5) . ? 
C1 C6 1.400(6) . ? 
C1 C2 1.416(5) . ? 
C2 C3 1.399(6) . ? 
C2 C8 1.461(6) . ? 
C3 C4 1.383(6) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.377(6) . ? 
C4 H4 0.9300 . ? 
C5 C6 1.401(6) . ? 
C5 H5 0.9300 . ? 
C6 C15 1.469(6) . ? 
C7 C12 1.385(5) . ? 
C7 C8 1.422(6) . ? 
C8 C9 1.409(6) . ? 
C9 C10 1.387(6) . ? 
C9 C13 1.483(6) . ? 
C10 C11 1.404(6) . ? 
C10 H10 0.9300 . ? 
C11 C12 1.371(6) . ? 
C11 H11 0.9300 . ? 
C12 H12 0.9300 . ? 
C14 H14A 0.9600 . ? 
C14 H14B 0.9600 . ? 
C14 H14C 0.9600 . ? 
C16 H16A 0.9600 . ? 
C16 H16B 0.9600 . ? 
C16 H16C 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 
C1 N1 C7 109.5(4) . . ? 
C1 N1 H1 125.2 . . ? 
C7 N1 H1 125.2 . . ? 
C13 O2 C14 117.9(4) . . ? 
C15 O4 C16 115.8(3) . . ? 
N1 C1 C6 128.1(4) . . ? 
N1 C1 C2 109.4(4) . . ? 
C6 C1 C2 122.5(4) . . ? 
C3 C2 C1 118.5(4) . . ? 
C3 C2 C8 135.1(4) . . ? 
C1 C2 C8 106.4(4) . . ? 
C4 C3 C2 119.2(4) . . ? 
C4 C3 H3 120.4 . . ? 
C2 C3 H3 120.4 . . ? 
C5 C4 C3 121.6(4) . . ? 
C5 C4 H4 119.2 . . ? 
C3 C4 H4 119.2 . . ? 
C4 C5 C6 121.6(4) . . ? 
C4 C5 H5 119.2 . . ? 
C6 C5 H5 119.2 . . ? 
C1 C6 C5 116.6(4) . . ? 
C1 C6 C15 121.8(4) . . ? 
C5 C6 C15 121.5(4) . . ? 
C12 C7 N1 127.2(4) . . ? 
C12 C7 C8 123.9(4) . . ? 
N1 C7 C8 108.9(4) . . ? 
C9 C8 C7 116.8(4) . . ? 
C9 C8 C2 137.4(4) . . ? 
C7 C8 C2 105.7(4) . . ? 
C10 C9 C8 119.4(4) . . ? 
C10 C9 C13 118.5(4) . . ? 
C8 C9 C13 122.1(4) . . ? 
C9 C10 C11 121.5(4) . . ? 
C9 C10 H10 119.3 . . ? 
C11 C10 H10 119.3 . . ? 
C12 C11 C10 121.0(4) . . ? 
C12 C11 H11 119.5 . . ? 
C10 C11 H11 119.5 . . ? 
C11 C12 C7 117.5(4) . . ? 
C11 C12 H12 121.3 . . ? 
C7 C12 H12 121.3 . . ? 
O1 C13 O2 121.4(4) . . ? 
O1 C13 C9 126.2(4) . . ? 
O2 C13 C9 112.4(4) . . ? 
O2 C14 H14A 109.5 . . ? 
O2 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
O2 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
O3 C15 O4 123.1(4) . . ? 
O3 C15 C6 123.9(4) . . ? 
O4 C15 C6 113.1(4) . . ? 
O4 C16 H16A 109.5 . . ? 
O4 C16 H16B 109.5 . . ? 
H16A C16 H16B 109.5 . . ? 
O4 C16 H16C 109.5 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 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 
C7 N1 C1 C6 -179.2(4) . . . . ? 
C7 N1 C1 C2 1.1(4) . . . . ? 
N1 C1 C2 C3 -179.8(3) . . . . ? 
C6 C1 C2 C3 0.6(6) . . . . ? 
N1 C1 C2 C8 -1.4(4) . . . . ? 
C6 C1 C2 C8 179.0(4) . . . . ? 
C1 C2 C3 C4 0.7(6) . . . . ? 
C8 C2 C3 C4 -177.1(4) . . . . ? 
C2 C3 C4 C5 -0.8(6) . . . . ? 
C3 C4 C5 C6 -0.3(7) . . . . ? 
N1 C1 C6 C5 178.8(4) . . . . ? 
C2 C1 C6 C5 -1.7(6) . . . . ? 
N1 C1 C6 C15 1.5(6) . . . . ? 
C2 C1 C6 C15 -178.9(4) . . . . ? 
C4 C5 C6 C1 1.5(6) . . . . ? 
C4 C5 C6 C15 178.8(4) . . . . ? 
C1 N1 C7 C12 179.2(4) . . . . ? 
C1 N1 C7 C8 -0.4(4) . . . . ? 
C12 C7 C8 C9 1.4(6) . . . . ? 
N1 C7 C8 C9 -179.0(3) . . . . ? 
C12 C7 C8 C2 179.9(4) . . . . ? 
N1 C7 C8 C2 -0.5(4) . . . . ? 
C3 C2 C8 C9 -2.8(9) . . . . ? 
C1 C2 C8 C9 179.2(5) . . . . ? 
C3 C2 C8 C7 179.1(4) . . . . ? 
C1 C2 C8 C7 1.1(4) . . . . ? 
C7 C8 C9 C10 0.1(6) . . . . ? 
C2 C8 C9 C10 -177.8(4) . . . . ? 
C7 C8 C9 C13 -179.8(4) . . . . ? 
C2 C8 C9 C13 2.3(8) . . . . ? 
C8 C9 C10 C11 -1.1(6) . . . . ? 
C13 C9 C10 C11 178.7(4) . . . . ? 
C9 C10 C11 C12 0.8(7) . . . . ? 
C10 C11 C12 C7 0.5(6) . . . . ? 
N1 C7 C12 C11 178.8(4) . . . . ? 
C8 C7 C12 C11 -1.7(6) . . . . ? 
C14 O2 C13 O1 -2.9(7) . . . . ? 
C14 O2 C13 C9 178.4(4) . . . . ? 
C10 C9 C13 O1 -169.7(5) . . . . ? 
C8 C9 C13 O1 10.2(7) . . . . ? 
C10 C9 C13 O2 8.9(6) . . . . ? 
C8 C9 C13 O2 -171.2(4) . . . . ? 
C16 O4 C15 O3 3.6(6) . . . . ? 
C16 O4 C15 C6 -176.4(3) . . . . ? 
C1 C6 C15 O3 -1.9(6) . . . . ? 
C5 C6 C15 O3 -179.1(4) . . . . ? 
C1 C6 C15 O4 178.1(4) . . . . ? 
C5 C6 C15 O4 0.9(6) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              27.66 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.337 
_refine_diff_density_min   -0.309 
_refine_diff_density_rms    0.073 
