# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2004



data_global

_journal_coden_Cambridge         177

loop_
_publ_author_name
'Stuart Warren'
'Thomas Boesen'
'David Fox'
'Warren Galloway'
'Daniel Sejer Pedersen'
'Charles R. Tyzack'

_publ_contact_author_name        'Dr Stuart Warren'
_publ_contact_author_address     
;
Cambridge
UNITED KINGDOM
;

_publ_contact_author_email       SW134@CAM.AC.UK

_publ_requested_journal          'Organic & Biomolecular Chemistry'

_publ_section_title              
;
Asymmetric cyclopropane synthesis via phosphine
oxide mediated cascade reactions
;

data_sw0405
_database_code_depnum_ccdc_archive 'CCDC 249431'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H27 O4 P'
_chemical_formula_sum            'C29 H27 O4 P'
_chemical_formula_weight         470.48

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   10.7399(6)
_cell_length_b                   12.8444(8)
_cell_length_c                   17.6182(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2430.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    38891
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      25.03

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_reflns_number            14107
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         25.07
_reflns_number_total             4251
_reflns_number_gt                2614
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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^)+(0.0482P)^2^+0.7773P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(4)
_refine_ls_number_reflns         4251
_refine_ls_number_parameters     315
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      2.629
_refine_ls_shift/su_max          0.147
_refine_ls_shift/su_mean         0.011

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
P1 P 0.3257(3) 0.8430(2) 0.59732(16) 0.0353(8) Uani 1 1 d . . .
O1 O 0.4375(8) 0.7553(6) 0.4402(4) 0.043(2) Uani 1 1 d . . .
O2 O 0.1979(8) 0.5776(6) 0.4294(4) 0.039(2) Uani 1 1 d D . .
H2A H 0.119(7) 0.603(10) 0.413(6) 0.07(4) Uiso 1 1 d D . .
O3 O 0.1308(9) 0.3915(7) 0.4851(5) 0.051(3) Uani 1 1 d D . .
H3 H 0.123(13) 0.411(11) 0.438(8) 0.07(5) Uiso 1 1 d . . .
O4 O 0.4616(7) 0.8633(6) 0.5954(4) 0.045(2) Uani 1 1 d . . .
C1 C 0.3282(12) 0.7777(9) 0.4495(6) 0.033(3) Uani 1 1 d . . .
C2 C 0.2682(10) 0.7502(9) 0.5257(6) 0.033(3) Uani 1 1 d . . .
H2 H 0.1765 0.7618 0.5204 0.040 Uiso 1 1 calc R . .
C3 C 0.2880(11) 0.6314(8) 0.5454(6) 0.035(3) Uani 1 1 d . . .
H3A H 0.3711 0.6090 0.5273 0.043 Uiso 1 1 calc RD . .
H3B H 0.2855 0.6220 0.6011 0.043 Uiso 1 1 calc R . .
C4 C 0.1920(11) 0.5657(8) 0.5102(5) 0.032(3) Uani 1 1 d . . .
H4 H 0.1079 0.5876 0.5287 0.039 Uiso 1 1 calc R . .
C5 C 0.2129(11) 0.4509(9) 0.5289(6) 0.036(3) Uani 1 1 d . . .
H5 H 0.3005 0.4314 0.5159 0.043 Uiso 1 1 calc R . .
C6 C 0.2576(10) 0.8324(9) 0.3892(6) 0.031(3) Uani 1 1 d . . .
C7 C 0.1308(12) 0.8503(11) 0.3925(7) 0.048(3) Uani 1 1 d . . .
H7 H 0.0853 0.8330 0.4370 0.058 Uiso 1 1 calc R . .
C8 C 0.0695(13) 0.8940(11) 0.3302(7) 0.054(4) Uani 1 1 d . . .
H8 H -0.0177 0.9062 0.3328 0.065 Uiso 1 1 calc R . .
C9 C 0.1325(12) 0.9194(11) 0.2658(7) 0.047(4) Uani 1 1 d . . .
H9 H 0.0900 0.9484 0.2235 0.057 Uiso 1 1 calc R . .
C10 C 0.2579(13) 0.9024(13) 0.2630(8) 0.064(5) Uani 1 1 d . . .
H10 H 0.3030 0.9207 0.2186 0.077 Uiso 1 1 calc R . .
C11 C 0.3202(13) 0.8590(11) 0.3239(7) 0.054(4) Uani 1 1 d . . .
H11 H 0.4074 0.8474 0.3206 0.065 Uiso 1 1 calc R . .
C12 C 0.1903(12) 0.4302(9) 0.6125(6) 0.036(3) Uani 1 1 d . . .
C13 C 0.2873(12) 0.4060(10) 0.6607(7) 0.051(4) Uani 1 1 d . . .
H13 H 0.3685 0.3969 0.6404 0.062 Uiso 1 1 calc R . .
C14 C 0.2687(14) 0.3949(13) 0.7374(8) 0.062(4) Uani 1 1 d . . .
H14 H 0.3371 0.3791 0.7697 0.074 Uiso 1 1 calc R . .
C15 C 0.1519(14) 0.4063(11) 0.7678(7) 0.055(4) Uani 1 1 d . . .
H15 H 0.1387 0.3994 0.8208 0.066 Uiso 1 1 calc R . .
C16 C 0.0549(14) 0.4279(11) 0.7200(7) 0.053(4) Uani 1 1 d . . .
H16 H -0.0266 0.4351 0.7402 0.064 Uiso 1 1 calc R . .
C17 C 0.0734(12) 0.4392(10) 0.6427(7) 0.045(3) Uani 1 1 d . . .
H17 H 0.0046 0.4534 0.6105 0.054 Uiso 1 1 calc R . .
C18 C 0.2780(12) 0.7934(9) 0.6890(6) 0.037(3) Uani 1 1 d . . .
C19 C 0.1665(13) 0.7443(10) 0.7030(6) 0.044(3) Uani 1 1 d . . .
H19 H 0.1096 0.7340 0.6625 0.053 Uiso 1 1 calc R . .
C20 C 0.1355(12) 0.7099(10) 0.7742(7) 0.048(4) Uani 1 1 d . . .
H20 H 0.0585 0.6754 0.7827 0.058 Uiso 1 1 calc R . .
C21 C 0.2167(14) 0.7257(11) 0.8331(7) 0.057(4) Uani 1 1 d . . .
H21 H 0.1953 0.7033 0.8828 0.068 Uiso 1 1 calc R . .
C22 C 0.3286(15) 0.7737(12) 0.8205(7) 0.065(4) Uani 1 1 d . . .
H22 H 0.3853 0.7834 0.8612 0.078 Uiso 1 1 calc R . .
C23 C 0.3594(13) 0.8081(10) 0.7482(7) 0.050(4) Uani 1 1 d . . .
H23 H 0.4368 0.8419 0.7397 0.060 Uiso 1 1 calc R . .
C24 C 0.2369(12) 0.9598(9) 0.5784(6) 0.035(3) Uani 1 1 d . . .
C25 C 0.1092(12) 0.9635(10) 0.5882(6) 0.039(3) Uani 1 1 d . . .
H25 H 0.0652 0.9031 0.6040 0.047 Uiso 1 1 calc R . .
C26 C 0.0453(14) 1.0558(11) 0.5748(7) 0.049(4) Uani 1 1 d . . .
H26 H -0.0423 1.0578 0.5822 0.058 Uiso 1 1 calc R . .
C27 C 0.1054(16) 1.1434(11) 0.5512(7) 0.057(4) Uani 1 1 d . . .
H27 H 0.0606 1.2061 0.5423 0.069 Uiso 1 1 calc R . .
C28 C 0.2322(17) 1.1393(12) 0.5403(8) 0.062(4) Uani 1 1 d . . .
H28 H 0.2749 1.1996 0.5230 0.074 Uiso 1 1 calc R . .
C29 C 0.2998(13) 1.0477(10) 0.5545(6) 0.047(3) Uani 1 1 d . . .
H29 H 0.3875 1.0462 0.5477 0.057 Uiso 1 1 calc R . .

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
P1 0.037(2) 0.0373(18) 0.0312(16) 0.0006(14) 0.0018(14) -0.0040(17)
O1 0.040(6) 0.048(6) 0.039(4) 0.003(4) 0.007(4) 0.005(5)
O2 0.042(6) 0.046(5) 0.029(4) 0.005(4) -0.001(4) 0.006(4)
O3 0.072(7) 0.043(5) 0.040(5) -0.007(4) -0.004(5) -0.005(5)
O4 0.037(5) 0.054(6) 0.045(5) 0.004(4) 0.001(4) -0.003(4)
C1 0.035(8) 0.031(7) 0.033(6) -0.004(5) 0.000(6) -0.006(6)
C2 0.028(7) 0.038(7) 0.033(6) 0.002(5) 0.002(5) -0.001(6)
C3 0.042(8) 0.033(7) 0.032(6) 0.003(5) 0.004(5) 0.008(6)
C4 0.033(7) 0.035(7) 0.028(6) 0.002(5) 0.000(5) 0.002(6)
C5 0.042(8) 0.033(7) 0.033(6) -0.003(5) 0.007(6) 0.000(6)
C6 0.032(7) 0.029(7) 0.031(7) -0.005(5) 0.004(5) -0.002(6)
C7 0.043(9) 0.065(9) 0.037(7) 0.010(7) 0.004(6) 0.004(7)
C8 0.039(9) 0.071(10) 0.054(8) 0.018(7) -0.005(7) 0.007(8)
C9 0.044(9) 0.058(9) 0.040(7) 0.020(6) -0.001(6) 0.002(7)
C10 0.055(11) 0.087(12) 0.050(9) 0.032(8) 0.009(7) 0.003(9)
C11 0.039(8) 0.079(10) 0.046(7) 0.020(7) 0.007(7) 0.007(8)
C12 0.040(8) 0.029(7) 0.040(7) 0.000(5) 0.001(6) -0.002(6)
C13 0.037(8) 0.070(10) 0.047(9) 0.005(7) 0.005(6) 0.009(7)
C14 0.051(10) 0.093(12) 0.043(9) 0.011(8) -0.006(7) 0.010(9)
C15 0.068(12) 0.061(9) 0.036(7) 0.014(6) 0.002(8) 0.004(9)
C16 0.049(9) 0.062(10) 0.048(8) 0.006(7) 0.013(7) 0.000(8)
C17 0.045(9) 0.044(8) 0.045(8) 0.011(6) -0.002(6) -0.001(7)
C18 0.041(8) 0.040(7) 0.030(7) -0.001(5) -0.001(5) -0.001(6)
C19 0.041(9) 0.051(8) 0.041(7) 0.004(6) -0.003(6) 0.000(8)
C20 0.042(9) 0.063(9) 0.039(8) 0.018(6) -0.002(6) -0.009(7)
C21 0.065(11) 0.066(10) 0.039(8) 0.013(7) 0.005(7) -0.008(9)
C22 0.068(11) 0.089(11) 0.039(7) 0.005(7) -0.013(7) -0.024(10)
C23 0.049(10) 0.059(9) 0.042(8) 0.010(6) -0.001(6) -0.017(7)
C24 0.045(9) 0.033(8) 0.027(6) -0.002(5) -0.003(5) -0.005(6)
C25 0.044(9) 0.039(8) 0.035(7) -0.005(6) -0.005(6) -0.004(7)
C26 0.057(9) 0.043(9) 0.046(8) -0.008(6) -0.014(6) 0.013(8)
C27 0.078(12) 0.037(9) 0.057(9) 0.001(7) -0.005(8) 0.013(9)
C28 0.091(13) 0.041(10) 0.052(9) 0.007(7) 0.008(8) -0.012(9)
C29 0.056(9) 0.043(9) 0.044(7) 0.000(6) -0.003(7) 0.001(8)

_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
P1 O4 1.483(8) . ?
P1 C24 1.809(13) . ?
P1 C18 1.810(11) . ?
P1 C2 1.843(11) . ?
O1 C1 1.220(13) . ?
O2 C4 1.433(11) . ?
O2 H2A 0.96(5) . ?
O3 C5 1.399(14) . ?
O3 H3 0.87(13) . ?
C1 C6 1.482(16) . ?
C1 C2 1.531(14) . ?
C2 C3 1.579(17) . ?
C2 H2 1.0000 . ?
C3 C4 1.469(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.527(15) . ?
C4 H4 1.0000 . ?
C5 C12 1.515(15) . ?
C5 H5 1.0000 . ?
C6 C11 1.377(15) . ?
C6 C7 1.382(16) . ?
C7 C8 1.398(16) . ?
C7 H7 0.9500 . ?
C8 C9 1.360(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.365(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(18) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.368(17) . ?
C12 C13 1.379(16) . ?
C13 C14 1.375(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.368(18) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(16) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.377(16) . ?
C18 C23 1.374(16) . ?
C19 C20 1.370(15) . ?
C19 H19 0.9500 . ?
C20 C21 1.371(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.369(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(17) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.384(16) . ?
C24 C29 1.381(17) . ?
C25 C26 1.390(17) . ?
C25 H25 0.9500 . ?
C26 C27 1.362(19) . ?
C26 H26 0.9500 . ?
C27 C28 1.377(19) . ?
C27 H27 0.9500 . ?
C28 C29 1.405(19) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

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
O4 P1 C24 111.7(5) . . ?
O4 P1 C18 111.1(5) . . ?
C24 P1 C18 107.9(5) . . ?
O4 P1 C2 115.4(5) . . ?
C24 P1 C2 103.5(5) . . ?
C18 P1 C2 106.7(5) . . ?
C4 O2 H2A 108(7) . . ?
C5 O3 H3 116(10) . . ?
O1 C1 C6 120.5(10) . . ?
O1 C1 C2 117.9(10) . . ?
C6 C1 C2 121.5(11) . . ?
C1 C2 C3 111.0(9) . . ?
C1 C2 P1 108.0(7) . . ?
C3 C2 P1 115.5(7) . . ?
C1 C2 H2 107.3 . . ?
C3 C2 H2 107.3 . . ?
P1 C2 H2 107.3 . . ?
C4 C3 C2 111.6(9) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O2 C4 C3 109.1(9) . . ?
O2 C4 C5 108.1(8) . . ?
C3 C4 C5 111.1(9) . . ?
O2 C4 H4 109.5 . . ?
C3 C4 H4 109.5 . . ?
C5 C4 H4 109.5 . . ?
O3 C5 C12 109.9(9) . . ?
O3 C5 C4 108.3(9) . . ?
C12 C5 C4 110.8(9) . . ?
O3 C5 H5 109.2 . . ?
C12 C5 H5 109.3 . . ?
C4 C5 H5 109.3 . . ?
C11 C6 C7 118.4(11) . . ?
C11 C6 C1 117.8(10) . . ?
C7 C6 C1 123.6(11) . . ?
C6 C7 C8 119.8(12) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C9 C8 C7 121.1(12) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 118.9(12) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C9 C10 C11 121.0(13) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C6 120.8(12) . . ?
C10 C11 H11 119.6 . . ?
C6 C11 H11 119.6 . . ?
C17 C12 C13 118.1(10) . . ?
C17 C12 C5 120.7(11) . . ?
C13 C12 C5 121.1(11) . . ?
C14 C13 C12 121.3(12) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 120.3(13) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 118.6(12) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 121.2(13) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C12 C17 C16 120.4(12) . . ?
C12 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C18 C23 118.7(10) . . ?
C19 C18 P1 124.6(9) . . ?
C23 C18 P1 116.7(9) . . ?
C20 C19 C18 121.5(11) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C21 C20 C19 119.4(12) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C22 120.1(12) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C23 120.2(12) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C18 C23 C22 120.1(13) . . ?
C18 C23 H23 119.9 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C29 119.7(12) . . ?
C25 C24 P1 121.9(10) . . ?
C29 C24 P1 118.4(10) . . ?
C24 C25 C26 119.8(13) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 121.5(14) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 118.7(14) . . ?
C26 C27 H27 120.7 . . ?
C28 C27 H27 120.7 . . ?
C27 C28 C29 121.2(14) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C24 C29 C28 119.1(13) . . ?
C24 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?

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
O1 C1 C2 C3 -53.1(13) . . . . ?
C6 C1 C2 C3 128.6(10) . . . . ?
O1 C1 C2 P1 74.5(11) . . . . ?
C6 C1 C2 P1 -103.7(10) . . . . ?
O4 P1 C2 C1 -45.0(10) . . . . ?
C24 P1 C2 C1 77.3(9) . . . . ?
C18 P1 C2 C1 -169.0(8) . . . . ?
O4 P1 C2 C3 80.0(9) . . . . ?
C24 P1 C2 C3 -157.7(8) . . . . ?
C18 P1 C2 C3 -44.0(9) . . . . ?
C1 C2 C3 C4 -85.1(11) . . . . ?
P1 C2 C3 C4 151.5(8) . . . . ?
C2 C3 C4 O2 60.4(12) . . . . ?
C2 C3 C4 C5 179.4(8) . . . . ?
O2 C4 C5 O3 -51.6(12) . . . . ?
C3 C4 C5 O3 -171.2(9) . . . . ?
O2 C4 C5 C12 -172.2(10) . . . . ?
C3 C4 C5 C12 68.2(12) . . . . ?
O1 C1 C6 C11 -1.5(16) . . . . ?
C2 C1 C6 C11 176.7(11) . . . . ?
O1 C1 C6 C7 172.9(12) . . . . ?
C2 C1 C6 C7 -8.9(17) . . . . ?
C11 C6 C7 C8 0(2) . . . . ?
C1 C6 C7 C8 -174.1(12) . . . . ?
C6 C7 C8 C9 0(2) . . . . ?
C7 C8 C9 C10 -1(2) . . . . ?
C8 C9 C10 C11 1(2) . . . . ?
C9 C10 C11 C6 0(2) . . . . ?
C7 C6 C11 C10 0(2) . . . . ?
C1 C6 C11 C10 174.6(13) . . . . ?
O3 C5 C12 C17 -52.7(14) . . . . ?
C4 C5 C12 C17 67.0(14) . . . . ?
O3 C5 C12 C13 130.0(12) . . . . ?
C4 C5 C12 C13 -110.3(13) . . . . ?
C17 C12 C13 C14 -2.3(19) . . . . ?
C5 C12 C13 C14 175.1(12) . . . . ?
C12 C13 C14 C15 1(2) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C17 -1(2) . . . . ?
C13 C12 C17 C16 2.2(18) . . . . ?
C5 C12 C17 C16 -175.2(11) . . . . ?
C15 C16 C17 C12 -1(2) . . . . ?
O4 P1 C18 C19 -163.6(10) . . . . ?
C24 P1 C18 C19 73.7(12) . . . . ?
C2 P1 C18 C19 -37.0(12) . . . . ?
O4 P1 C18 C23 17.5(11) . . . . ?
C24 P1 C18 C23 -105.2(10) . . . . ?
C2 P1 C18 C23 144.1(10) . . . . ?
C23 C18 C19 C20 -0.2(19) . . . . ?
P1 C18 C19 C20 -179.1(10) . . . . ?
C18 C19 C20 C21 1(2) . . . . ?
C19 C20 C21 C22 -1(2) . . . . ?
C20 C21 C22 C23 1(2) . . . . ?
C19 C18 C23 C22 0.1(19) . . . . ?
P1 C18 C23 C22 179.0(11) . . . . ?
C21 C22 C23 C18 -1(2) . . . . ?
O4 P1 C24 C25 -170.3(9) . . . . ?
C18 P1 C24 C25 -47.8(11) . . . . ?
C2 P1 C24 C25 65.0(10) . . . . ?
O4 P1 C24 C29 8.8(11) . . . . ?
C18 P1 C24 C29 131.2(9) . . . . ?
C2 P1 C24 C29 -115.9(9) . . . . ?
C29 C24 C25 C26 -0.7(17) . . . . ?
P1 C24 C25 C26 178.3(8) . . . . ?
C24 C25 C26 C27 0.8(18) . . . . ?
C25 C26 C27 C28 0(2) . . . . ?
C26 C27 C28 C29 -1(2) . . . . ?
C25 C24 C29 C28 -0.2(18) . . . . ?
P1 C24 C29 C28 -179.3(9) . . . . ?
C27 C28 C29 C24 1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.057

data_sw0401
_database_code_depnum_ccdc_archive 'CCDC 249432'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H16 O2'
_chemical_formula_sum            'C17 H16 O2'
_chemical_formula_weight         252.30

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pccn

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

_cell_length_a                   13.1650(8)
_cell_length_b                   28.102(2)
_cell_length_c                   7.2735(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2690.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    75913
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      22.46

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)

_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_reflns_number            8455
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         22.45
_reflns_number_total             1731
_reflns_number_gt                1374
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_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^)+(0.0257P)^2^+2.4881P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1731
_refine_ls_number_parameters     175
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1265
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_restrained_S_all      1.269
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002

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 0.28199(18) 0.53284(8) -0.3799(3) 0.0505(7) Uani 1 1 d . . .
O2 O 0.10624(17) 0.45106(7) 0.0895(3) 0.0426(6) Uani 1 1 d D . .
H2A H 0.138(2) 0.4828(7) 0.086(4) 0.051 Uiso 1 1 d D . .
C1 C 0.1961(3) 0.54562(11) -0.3349(4) 0.0377(8) Uani 1 1 d . . .
C2 C 0.1161(2) 0.51073(10) -0.2894(4) 0.0355(8) Uani 1 1 d . . .
H2 H 0.0526 0.5237 -0.2330 0.043 Uiso 1 1 calc R . .
C3 C 0.1454(2) 0.46040(10) -0.2352(4) 0.0341(8) Uani 1 1 d . . .
H3 H 0.2200 0.4538 -0.2300 0.041 Uiso 1 1 calc R . .
C4 C 0.1033(3) 0.46862(11) -0.4199(4) 0.0419(9) Uani 1 1 d . . .
H4A H 0.0335 0.4573 -0.4446 0.050 Uiso 1 1 calc R . .
H4B H 0.1504 0.4664 -0.5258 0.050 Uiso 1 1 calc R . .
C5 C 0.0819(2) 0.43546(10) -0.0937(4) 0.0347(8) Uani 1 1 d . . .
H5 H 0.0089 0.4431 -0.1181 0.042 Uiso 1 1 calc R . .
C6 C 0.0950(2) 0.38214(10) -0.1046(4) 0.0332(8) Uani 1 1 d . . .
C7 C 0.0347(3) 0.35543(11) -0.2227(5) 0.0432(9) Uani 1 1 d . . .
H7 H -0.0158 0.3708 -0.2946 0.052 Uiso 1 1 calc R . .
C8 C 0.0473(3) 0.30678(12) -0.2369(5) 0.0500(10) Uani 1 1 d . . .
H8 H 0.0057 0.2890 -0.3186 0.060 Uiso 1 1 calc R . .
C9 C 0.1201(3) 0.28391(12) -0.1331(5) 0.0492(10) Uani 1 1 d . . .
H9 H 0.1283 0.2504 -0.1418 0.059 Uiso 1 1 calc R . .
C10 C 0.1809(3) 0.31007(12) -0.0165(5) 0.0485(10) Uani 1 1 d . . .
H10 H 0.2313 0.2945 0.0550 0.058 Uiso 1 1 calc R . .
C11 C 0.1687(3) 0.35874(11) -0.0032(5) 0.0421(9) Uani 1 1 d . . .
H11 H 0.2115 0.3764 0.0767 0.050 Uiso 1 1 calc R . .
C12 C 0.1724(3) 0.59758(11) -0.3319(4) 0.0368(8) Uani 1 1 d . . .
C13 C 0.2485(3) 0.62927(12) -0.3819(5) 0.0498(10) Uani 1 1 d . . .
H13 H 0.3134 0.6174 -0.4158 0.060 Uiso 1 1 calc R . .
C14 C 0.2312(3) 0.67754(12) -0.3831(6) 0.0652(12) Uani 1 1 d . . .
H14 H 0.2838 0.6989 -0.4177 0.078 Uiso 1 1 calc R . .
C15 C 0.1367(3) 0.69473(13) -0.3334(6) 0.0648(12) Uani 1 1 d . . .
H15 H 0.1241 0.7280 -0.3352 0.078 Uiso 1 1 calc R . .
C16 C 0.0610(3) 0.66396(12) -0.2816(5) 0.0544(10) Uani 1 1 d . . .
H16 H -0.0033 0.6760 -0.2452 0.065 Uiso 1 1 calc R . .
C17 C 0.0782(3) 0.61553(11) -0.2825(4) 0.0404(9) Uani 1 1 d . . .
H17 H 0.0251 0.5943 -0.2489 0.048 Uiso 1 1 calc R . .

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 0.0455(16) 0.0434(14) 0.0627(17) 0.0025(12) 0.0153(13) 0.0056(11)
O2 0.0526(15) 0.0381(13) 0.0372(13) -0.0032(11) 0.0025(12) -0.0071(11)
C1 0.040(2) 0.042(2) 0.0314(18) 0.0028(15) 0.0019(16) 0.0010(17)
C2 0.0371(19) 0.0318(18) 0.0377(19) -0.0009(15) 0.0014(16) 0.0046(15)
C3 0.0349(18) 0.0320(18) 0.0353(19) -0.0005(15) 0.0007(15) 0.0013(14)
C4 0.047(2) 0.042(2) 0.0357(19) -0.0011(15) -0.0036(17) 0.0001(16)
C5 0.0329(19) 0.0356(19) 0.0356(19) -0.0014(15) -0.0035(15) -0.0015(15)
C6 0.0319(19) 0.0351(19) 0.0327(18) -0.0003(15) 0.0010(16) -0.0023(15)
C7 0.045(2) 0.041(2) 0.044(2) 0.0005(17) -0.0076(18) -0.0020(17)
C8 0.059(2) 0.041(2) 0.051(2) -0.0064(18) -0.003(2) -0.0095(18)
C9 0.064(3) 0.034(2) 0.050(2) -0.0001(18) 0.009(2) 0.0013(19)
C10 0.055(2) 0.042(2) 0.048(2) 0.0040(18) -0.001(2) 0.0112(18)
C11 0.042(2) 0.043(2) 0.041(2) -0.0015(17) -0.0041(17) 0.0010(17)
C12 0.042(2) 0.036(2) 0.0328(19) -0.0021(15) 0.0047(16) 0.0016(16)
C13 0.047(2) 0.047(2) 0.056(2) -0.0082(18) 0.016(2) -0.0043(19)
C14 0.074(3) 0.036(2) 0.086(3) -0.007(2) 0.029(3) -0.014(2)
C15 0.082(3) 0.034(2) 0.079(3) 0.001(2) 0.024(3) 0.002(2)
C16 0.058(2) 0.039(2) 0.066(3) 0.0057(19) 0.018(2) 0.0060(19)
C17 0.047(2) 0.033(2) 0.041(2) 0.0042(15) 0.0058(17) 0.0015(16)

_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 C1 1.231(4) . ?
O2 C5 1.439(4) . ?
O2 H2A 0.986(18) . ?
C1 C2 1.476(4) . ?
C1 C12 1.494(4) . ?
C2 C3 1.518(4) . ?
C2 C4 1.526(4) . ?
C2 H2 1.0000 . ?
C3 C4 1.472(4) . ?
C3 C5 1.501(4) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.510(4) . ?
C5 H5 1.0000 . ?
C6 C11 1.385(4) . ?
C6 C7 1.390(4) . ?
C7 C8 1.381(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C17 1.386(4) . ?
C12 C13 1.389(4) . ?
C13 C14 1.375(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?

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
C5 O2 H2A 110.2(19) . . ?
O1 C1 C2 121.4(3) . . ?
O1 C1 C12 118.8(3) . . ?
C2 C1 C12 119.8(3) . . ?
C1 C2 C3 119.7(3) . . ?
C1 C2 C4 117.0(3) . . ?
C3 C2 C4 57.81(19) . . ?
C1 C2 H2 116.5 . . ?
C3 C2 H2 116.5 . . ?
C4 C2 H2 116.5 . . ?
C4 C3 C5 119.3(3) . . ?
C4 C3 C2 61.4(2) . . ?
C5 C3 C2 118.1(3) . . ?
C4 C3 H3 115.7 . . ?
C5 C3 H3 115.7 . . ?
C2 C3 H3 115.7 . . ?
C3 C4 C2 60.8(2) . . ?
C3 C4 H4A 117.7 . . ?
C2 C4 H4A 117.7 . . ?
C3 C4 H4B 117.7 . . ?
C2 C4 H4B 117.7 . . ?
H4A C4 H4B 114.8 . . ?
O2 C5 C3 111.6(2) . . ?
O2 C5 C6 109.0(2) . . ?
C3 C5 C6 111.3(2) . . ?
O2 C5 H5 108.3 . . ?
C3 C5 H5 108.3 . . ?
C6 C5 H5 108.3 . . ?
C11 C6 C7 118.2(3) . . ?
C11 C6 C5 121.6(3) . . ?
C7 C6 C5 120.2(3) . . ?
C8 C7 C6 120.8(3) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 119.5(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C6 120.9(3) . . ?
C10 C11 H11 119.5 . . ?
C6 C11 H11 119.5 . . ?
C17 C12 C13 118.7(3) . . ?
C17 C12 C1 123.1(3) . . ?
C13 C12 C1 118.2(3) . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 120.1(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C12 120.5(3) . . ?
C16 C17 H17 119.8 . . ?
C12 C17 H17 119.8 . . ?

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
O1 C1 C2 C3 20.4(4) . . . . ?
C12 C1 C2 C3 -161.3(3) . . . . ?
O1 C1 C2 C4 -46.1(4) . . . . ?
C12 C1 C2 C4 132.1(3) . . . . ?
C1 C2 C3 C4 -105.0(3) . . . . ?
C1 C2 C3 C5 145.1(3) . . . . ?
C4 C2 C3 C5 -109.9(3) . . . . ?
C5 C3 C4 C2 108.0(3) . . . . ?
C1 C2 C4 C3 109.6(3) . . . . ?
C4 C3 C5 O2 -149.9(3) . . . . ?
C2 C3 C5 O2 -78.7(3) . . . . ?
C4 C3 C5 C6 88.1(3) . . . . ?
C2 C3 C5 C6 159.2(3) . . . . ?
O2 C5 C6 C11 -33.1(4) . . . . ?
C3 C5 C6 C11 90.4(4) . . . . ?
O2 C5 C6 C7 149.0(3) . . . . ?
C3 C5 C6 C7 -87.4(3) . . . . ?
C11 C6 C7 C8 0.7(5) . . . . ?
C5 C6 C7 C8 178.6(3) . . . . ?
C6 C7 C8 C9 0.2(5) . . . . ?
C7 C8 C9 C10 -0.7(5) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C10 C11 C6 0.7(5) . . . . ?
C7 C6 C11 C10 -1.1(5) . . . . ?
C5 C6 C11 C10 -179.0(3) . . . . ?
O1 C1 C12 C17 -179.7(3) . . . . ?
C2 C1 C12 C17 2.0(5) . . . . ?
O1 C1 C12 C13 0.6(5) . . . . ?
C2 C1 C12 C13 -177.7(3) . . . . ?
C17 C12 C13 C14 -0.2(5) . . . . ?
C1 C12 C13 C14 179.6(3) . . . . ?
C12 C13 C14 C15 0.1(6) . . . . ?
C13 C14 C15 C16 0.6(6) . . . . ?
C14 C15 C16 C17 -1.3(6) . . . . ?
C15 C16 C17 C12 1.3(6) . . . . ?
C13 C12 C17 C16 -0.5(5) . . . . ?
C1 C12 C17 C16 179.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        22.45
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.040