# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2009



data_global

_journal_coden_Cambridge         177

_publ_requested_journal          'Organic & Biomolecular Chemistry'

loop_
_publ_author_name
C.J.Suckling

_publ_contact_author_name        C.J.Suckling
_publ_contact_author_address     
;
Department of Pure and Applied Chem
University of Strathclyde
295 Cathedral Street
GLASGOW
G1 1XL
UNITED KINGDOM
;

_publ_contact_author_email       C.J.SUCKLING@STRATH.AC.UK

_publ_section_title              
;
Diversity oriented syntheses of fused pyrimidines
designed as potential antifolates
;

# Attachment 'fused_pyrimidines.cif'

data_suc205
_database_code_depnum_ccdc_archive 'CCDC 705654'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16.80 H19.20 N4 O4.80'
_chemical_formula_weight         353.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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'

_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                   7.1471(3)
_cell_length_b                   10.1809(4)
_cell_length_c                   12.3149(5)
_cell_angle_alpha                81.282(3)
_cell_angle_beta                 77.534(2)
_cell_angle_gamma                81.436(3)
_cell_volume                     858.56(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3734
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       'cut needle'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             373
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
1 side of needle white/opaque - solvent loss?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15464
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         27.51
_reflns_number_total             3900
_reflns_number_gt                2695
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Denzo & Collect'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0659P)^2^+0.3762P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3900
_refine_ls_number_parameters     264
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1447
_refine_ls_wR_factor_gt          0.1268
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.15546(19) 0.16242(12) 1.14188(11) 0.0290(3) Uani 1 1 d . . .
O2 O 0.2612(2) -0.13737(14) 1.60674(11) 0.0373(4) Uani 1 1 d . . .
O3 O 0.3629(2) -0.18853(15) 0.93110(13) 0.0434(4) Uani 1 1 d . . .
O4 O 0.3507(2) -0.24641(13) 1.11465(12) 0.0359(4) Uani 1 1 d . . .
N1 N 0.1557(2) 0.25161(18) 0.81451(14) 0.0376(5) Uani 1 1 d . . .
N2 N 0.0975(2) 0.32677(16) 0.99609(14) 0.0327(4) Uani 1 1 d . . .
N3 N 0.0567(3) 0.4724(2) 0.8394(2) 0.0457(5) Uani 1 1 d . . .
N4 N 0.2532(3) 0.0311(2) 0.78540(17) 0.0422(5) Uani 1 1 d . . .
C1 C 0.1041(3) 0.3463(2) 0.88533(18) 0.0354(5) Uani 1 1 d . . .
C2 C 0.1528(3) 0.2002(2) 1.03103(16) 0.0289(4) Uani 1 1 d . . .
C3 C 0.2098(3) 0.09213(19) 0.97183(16) 0.0290(4) Uani 1 1 d . . .
C4 C 0.2077(3) 0.1239(2) 0.85597(17) 0.0336(5) Uani 1 1 d . . .
C5 C 0.2508(3) -0.02228(19) 1.05341(16) 0.0283(4) Uani 1 1 d . . .
C6 C 0.2150(3) 0.02555(18) 1.15500(16) 0.0274(4) Uani 1 1 d . . .
C7 C 0.2260(3) -0.02449(18) 1.27207(16) 0.0272(4) Uani 1 1 d . . .
C8 C 0.1714(3) -0.14755(19) 1.32464(16) 0.0290(4) Uani 1 1 d . . .
H8 H 0.1270 -0.2043 1.2835 0.035 Uiso 1 1 calc R . .
C9 C 0.1807(3) -0.18894(19) 1.43640(17) 0.0307(5) Uani 1 1 d . . .
H9 H 0.1441 -0.2737 1.4711 0.037 Uiso 1 1 calc R . .
C10 C 0.2438(3) -0.10606(19) 1.49708(16) 0.0294(4) Uani 1 1 d . . .
C11 C 0.2944(3) 0.01871(19) 1.44611(17) 0.0305(4) Uani 1 1 d . . .
H11 H 0.3350 0.0764 1.4880 0.037 Uiso 1 1 calc R . .
C12 C 0.2860(3) 0.05884(19) 1.33524(17) 0.0295(4) Uani 1 1 d . . .
H12 H 0.3213 0.1441 1.3011 0.035 Uiso 1 1 calc R . .
C13 C 0.2102(3) -0.2638(2) 1.66302(18) 0.0384(5) Uani 1 1 d . . .
H13A H 0.0738 -0.2687 1.6642 0.058 Uiso 1 1 calc R . .
H13B H 0.2313 -0.2740 1.7400 0.058 Uiso 1 1 calc R . .
H13C H 0.2903 -0.3355 1.6235 0.058 Uiso 1 1 calc R . .
C14 C 0.3263(3) -0.1583(2) 1.02585(18) 0.0315(5) Uani 1 1 d . . .
C15 C 0.4152(3) -0.3845(2) 1.0924(2) 0.0388(5) Uani 1 1 d . . .
H15A H 0.5446 -0.3909 1.0432 0.047 Uiso 1 1 calc R . .
H15B H 0.3241 -0.4165 1.0550 0.047 Uiso 1 1 calc R . .
C16 C 0.4220(3) -0.4674(2) 1.2038(2) 0.0491(6) Uani 1 1 d . . .
H16A H 0.5123 -0.4346 1.2400 0.074 Uiso 1 1 calc R . .
H16B H 0.4652 -0.5611 1.1923 0.074 Uiso 1 1 calc R . .
H16C H 0.2930 -0.4604 1.2515 0.074 Uiso 1 1 calc R . .
O5 O 0.1338(4) 0.4028(2) 0.6073(2) 0.0250(6) Uani 0.50 1 d P A 1
H1S H 0.1436 0.3537 0.6715 0.038 Uiso 0.50 1 d PR A 1
C17 C 0.2797(13) 0.3912(7) 0.5313(5) 0.072(3) Uani 0.50 1 d P A 1
H17A H 0.3352 0.4761 0.5123 0.108 Uiso 0.50 1 calc PR A 1
H17B H 0.2436 0.3678 0.4650 0.108 Uiso 0.50 1 calc PR A 1
H17C H 0.3752 0.3205 0.5570 0.108 Uiso 0.50 1 calc PR A 1
O6 O 0.0681(7) 0.4693(6) 0.5700(4) 0.0410(12) Uiso 0.30 1 d P B 2
H2S H 0.0658 0.4185 0.6279 0.061 Uiso 0.30 1 d PRD B 2
C18 C 0.2700(14) 0.3833(16) 0.5066(8) 0.045(3) Uiso 0.30 1 d PD B 2
H18A H 0.3488 0.4451 0.4538 0.068 Uiso 0.30 1 calc PR B 2
H18B H 0.2363 0.3174 0.4661 0.068 Uiso 0.30 1 calc PR B 2
H18C H 0.3432 0.3372 0.5630 0.068 Uiso 0.30 1 calc PR B 2
H1N H 0.009(5) 0.533(3) 0.883(3) 0.078(11) Uiso 1 1 d . . .
H2N H 0.058(3) 0.489(2) 0.765(2) 0.047(7) Uiso 1 1 d . . .
H3N H 0.244(4) 0.057(3) 0.711(2) 0.063(8) Uiso 1 1 d . . .
H4N H 0.303(4) -0.064(3) 0.821(2) 0.075(9) 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
O1 0.0320(7) 0.0227(7) 0.0309(8) -0.0006(5) -0.0073(6) -0.0001(5)
O2 0.0489(9) 0.0328(8) 0.0300(8) 0.0020(6) -0.0095(6) -0.0075(6)
O3 0.0499(10) 0.0402(9) 0.0404(9) -0.0139(7) -0.0049(7) -0.0027(7)
O4 0.0378(8) 0.0258(7) 0.0410(9) -0.0050(6) -0.0043(6) 0.0015(6)
N1 0.0311(9) 0.0452(11) 0.0346(10) 0.0076(8) -0.0074(7) -0.0095(8)
N2 0.0318(9) 0.0279(9) 0.0366(10) 0.0058(7) -0.0090(7) -0.0044(7)
N3 0.0432(12) 0.0419(12) 0.0475(14) 0.0168(11) -0.0132(10) -0.0067(9)
N4 0.0386(11) 0.0569(13) 0.0306(11) -0.0092(10) -0.0042(8) -0.0043(9)
C1 0.0255(10) 0.0397(12) 0.0389(13) 0.0071(10) -0.0075(8) -0.0077(8)
C2 0.0240(10) 0.0322(11) 0.0302(11) 0.0013(8) -0.0072(8) -0.0047(8)
C3 0.0235(10) 0.0327(11) 0.0296(11) -0.0003(8) -0.0035(8) -0.0055(8)
C4 0.0227(10) 0.0449(13) 0.0328(11) -0.0014(9) -0.0050(8) -0.0070(8)
C5 0.0224(9) 0.0297(10) 0.0322(11) -0.0036(8) -0.0037(8) -0.0038(7)
C6 0.0217(9) 0.0230(10) 0.0363(11) -0.0003(8) -0.0059(8) -0.0018(7)
C7 0.0232(9) 0.0242(10) 0.0325(11) -0.0021(8) -0.0058(8) 0.0017(7)
C8 0.0285(10) 0.0250(10) 0.0336(11) -0.0048(8) -0.0065(8) -0.0015(8)
C9 0.0309(10) 0.0245(10) 0.0343(11) 0.0001(8) -0.0041(8) -0.0032(8)
C10 0.0279(10) 0.0287(10) 0.0294(11) -0.0027(8) -0.0045(8) 0.0010(8)
C11 0.0311(10) 0.0261(10) 0.0352(11) -0.0060(8) -0.0084(8) -0.0016(8)
C12 0.0291(10) 0.0223(10) 0.0359(11) -0.0001(8) -0.0071(8) -0.0015(8)
C13 0.0473(13) 0.0310(11) 0.0317(12) 0.0026(9) -0.0026(9) -0.0024(9)
C14 0.0245(10) 0.0322(11) 0.0377(12) -0.0064(9) -0.0036(8) -0.0047(8)
C15 0.0314(11) 0.0276(11) 0.0553(14) -0.0098(10) -0.0038(10) 0.0004(8)
C16 0.0429(13) 0.0323(12) 0.0697(17) -0.0002(11) -0.0131(12) -0.0003(10)
O5 0.0316(14) 0.0206(13) 0.0215(14) 0.0084(10) -0.0130(11) 0.0012(11)
C17 0.168(8) 0.021(3) 0.017(3) -0.009(2) 0.020(4) -0.029(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.364(2) . ?
O1 C6 1.391(2) . ?
O2 C10 1.368(2) . ?
O2 C13 1.425(2) . ?
O3 C14 1.216(2) . ?
O4 C14 1.330(2) . ?
O4 C15 1.461(2) . ?
N1 C4 1.351(3) . ?
N1 C1 1.355(3) . ?
N2 C2 1.325(2) . ?
N2 C1 1.340(3) . ?
N3 C1 1.348(3) . ?
N3 H1N 0.86(3) . ?
N3 H2N 0.90(3) . ?
N4 C4 1.337(3) . ?
N4 H3N 0.93(3) . ?
N4 H4N 1.04(3) . ?
C2 C3 1.375(3) . ?
C3 C4 1.417(3) . ?
C3 C5 1.457(3) . ?
C5 C6 1.370(3) . ?
C5 C14 1.471(3) . ?
C6 C7 1.469(3) . ?
C7 C8 1.390(3) . ?
C7 C12 1.401(3) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(3) . ?
C11 C12 1.376(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 C16 1.503(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O5 C17 1.246(7) . ?
O5 H1S 0.8802 . ?
O5 H2S 0.5123 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O6 C18 1.674(8) . ?
O6 H2S 0.8133 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C6 107.33(15) . . ?
C10 O2 C13 117.83(16) . . ?
C14 O4 C15 115.86(16) . . ?
C4 N1 C1 119.02(18) . . ?
C2 N2 C1 111.64(18) . . ?
C1 N3 H1N 119(2) . . ?
C1 N3 H2N 119.6(16) . . ?
H1N N3 H2N 121(3) . . ?
C4 N4 H3N 118.8(17) . . ?
C4 N4 H4N 114.7(16) . . ?
H3N N4 H4N 126(2) . . ?
N2 C1 N3 117.1(2) . . ?
N2 C1 N1 126.30(19) . . ?
N3 C1 N1 116.6(2) . . ?
N2 C2 O1 119.54(18) . . ?
N2 C2 C3 129.90(19) . . ?
O1 C2 C3 110.54(16) . . ?
C2 C3 C4 113.57(18) . . ?
C2 C3 C5 106.04(17) . . ?
C4 C3 C5 140.38(19) . . ?
N4 C4 N1 118.2(2) . . ?
N4 C4 C3 122.2(2) . . ?
N1 C4 C3 119.54(19) . . ?
C6 C5 C3 106.21(17) . . ?
C6 C5 C14 128.99(18) . . ?
C3 C5 C14 124.71(18) . . ?
C5 C6 O1 109.87(16) . . ?
C5 C6 C7 138.69(18) . . ?
O1 C6 C7 111.41(16) . . ?
C8 C7 C12 118.40(18) . . ?
C8 C7 C6 123.33(17) . . ?
C12 C7 C6 118.20(17) . . ?
C7 C8 C9 121.03(18) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C10 C9 C8 119.73(18) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
O2 C10 C9 124.65(17) . . ?
O2 C10 C11 115.60(17) . . ?
C9 C10 C11 119.75(18) . . ?
C12 C11 C10 120.25(19) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 120.80(18) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 O4 122.59(18) . . ?
O3 C14 C5 123.64(19) . . ?
O4 C14 C5 113.76(17) . . ?
O4 C15 C16 107.00(18) . . ?
O4 C15 H15A 110.3 . . ?
C16 C15 H15A 110.3 . . ?
O4 C15 H15B 110.3 . . ?
C16 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 O5 H1S 115.2 . . ?
C17 O5 H2S 160.7 . . ?
H1S O5 H2S 84.2 . . ?
C18 O6 H2S 91.9 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C2 N2 C1 N3 -177.95(18) . . . . ?
C2 N2 C1 N1 1.4(3) . . . . ?
C4 N1 C1 N2 -0.4(3) . . . . ?
C4 N1 C1 N3 178.90(18) . . . . ?
C1 N2 C2 O1 179.81(16) . . . . ?
C1 N2 C2 C3 -1.2(3) . . . . ?
C6 O1 C2 N2 178.88(16) . . . . ?
C6 O1 C2 C3 -0.3(2) . . . . ?
N2 C2 C3 C4 0.0(3) . . . . ?
O1 C2 C3 C4 179.12(15) . . . . ?
N2 C2 C3 C5 -178.98(19) . . . . ?
O1 C2 C3 C5 0.1(2) . . . . ?
C1 N1 C4 N4 178.25(18) . . . . ?
C1 N1 C4 C3 -0.9(3) . . . . ?
C2 C3 C4 N4 -178.06(18) . . . . ?
C5 C3 C4 N4 0.5(4) . . . . ?
C2 C3 C4 N1 1.0(3) . . . . ?
C5 C3 C4 N1 179.6(2) . . . . ?
C2 C3 C5 C6 0.2(2) . . . . ?
C4 C3 C5 C6 -178.4(2) . . . . ?
C2 C3 C5 C14 -176.65(17) . . . . ?
C4 C3 C5 C14 4.8(4) . . . . ?
C3 C5 C6 O1 -0.3(2) . . . . ?
C14 C5 C6 O1 176.27(17) . . . . ?
C3 C5 C6 C7 -178.3(2) . . . . ?
C14 C5 C6 C7 -1.6(4) . . . . ?
C2 O1 C6 C5 0.4(2) . . . . ?
C2 O1 C6 C7 178.93(14) . . . . ?
C5 C6 C7 C8 -40.6(3) . . . . ?
O1 C6 C7 C8 141.52(18) . . . . ?
C5 C6 C7 C12 142.5(2) . . . . ?
O1 C6 C7 C12 -35.4(2) . . . . ?
C12 C7 C8 C9 -1.7(3) . . . . ?
C6 C7 C8 C9 -178.59(17) . . . . ?
C7 C8 C9 C10 0.6(3) . . . . ?
C13 O2 C10 C9 -0.3(3) . . . . ?
C13 O2 C10 C11 179.67(17) . . . . ?
C8 C9 C10 O2 -179.03(18) . . . . ?
C8 C9 C10 C11 1.0(3) . . . . ?
O2 C10 C11 C12 178.64(17) . . . . ?
C9 C10 C11 C12 -1.4(3) . . . . ?
C10 C11 C12 C7 0.2(3) . . . . ?
C8 C7 C12 C11 1.3(3) . . . . ?
C6 C7 C12 C11 178.36(17) . . . . ?
C15 O4 C14 O3 -3.0(3) . . . . ?
C15 O4 C14 C5 176.68(16) . . . . ?
C6 C5 C14 O3 -175.78(19) . . . . ?
C3 C5 C14 O3 0.3(3) . . . . ?
C6 C5 C14 O4 4.5(3) . . . . ?
C3 C5 C14 O4 -179.47(16) . . . . ?
C14 O4 C15 C16 -176.80(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.050

#===END