Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_paev23

_database_code_CSD	172435


_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Ahsan, Khalid'
'Evans, P Andrew'
'Raina, Sushil'

_publ_contact_author_name     	'Dr P Andrew Evans'  
_publ_contact_author_address 
;
Department of Chemistry
Indiana University
Bloomington
UNITED STATES OF AMERICA
;

_publ_contact_author_email       'PAEVANS@INDIANA.EDU'

_publ_section_title		
;
Intramolecular addition of acyl radicals to a-substituted cinylogous
carbonates: understanding the effect of ring size on acyclic stereocontrol
; 

_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C16 H18 O5' 
_chemical_formula_weight          290.30 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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            Monoclinic
_symmetry_space_group_name_H-M    P2(1) 

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

_cell_length_a                    8.4891(2) 
_cell_length_b                    17.5380(3) 
_cell_length_c                    14.1931(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.9331(7) 
_cell_angle_gamma                 90.00 
_cell_volume                      2108.09(6) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     198(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        Plate 
_exptl_crystal_colour             Colorless
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.372 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              924 
_exptl_absorpt_coefficient_mu     0.102 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       198(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        'Siemen's P4/CCD'
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8835 
_diffrn_reflns_av_R_equivalents   0.0391 
_diffrn_reflns_av_sigmaI/netI     0.0707 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.44 
_diffrn_reflns_theta_max          28.44 
_reflns_number_total              7301 
_reflns_number_observed           6032 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.0000P] 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     ? 
_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    1.49(72) 
_refine_ls_number_reflns          7297 
_refine_ls_number_parameters      568 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0581 
_refine_ls_R_factor_obs           0.0444 
_refine_ls_wR_factor_all          0.1292 
_refine_ls_wR_factor_obs          0.1093 
_refine_ls_goodness_of_fit_all    0.904 
_refine_ls_goodness_of_fit_obs    0.939 
_refine_ls_restrained_S_all       1.003 
_refine_ls_restrained_S_obs       0.939 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
O1A O 0.3431(2) 0.49251(12) 0.56898(13) 0.0327(5) Uani 1 d . . 
O2A O 0.2074(2) 0.60574(11) 0.53763(11) 0.0243(4) Uani 1 d . . 
O3A O 0.3179(2) 0.52545(12) 0.31599(12) 0.0287(4) Uani 1 d . . 
O4A O 0.0646(2) 0.62534(13) 0.23706(13) 0.0336(5) Uani 1 d . . 
O5A O -0.0100(3) 0.5517(2) 0.11502(15) 0.0508(7) Uani 1 d . . 
O1B O 0.2382(2) 0.97180(11) 0.40456(12) 0.0260(4) Uani 1 d . . 
O2B O 0.0706(2) 0.86818(11) 0.37664(11) 0.0222(4) Uani 1 d . . 
O3B O 0.2114(2) 0.93088(11) 0.15321(11) 0.0210(4) Uani 1 d . . 
O4B O 0.1088(2) 0.77524(12) 0.09163(12) 0.0309(5) Uani 1 d . . 
O5B O 0.2893(3) 0.75734(14) -0.01300(14) 0.0422(6) Uani 1 d . . 
O1C O 0.7490(2) 0.65793(11) 0.46169(12) 0.0249(4) Uani 1 d . . 
O2C O 0.5674(2) 0.75418(11) 0.48767(11) 0.0213(4) Uani 1 d . . 
O3C O 0.7025(2) 0.66828(11) 0.71290(11) 0.0221(4) Uani 1 d . . 
O4C O 0.6102(2) 0.81243(12) 0.78832(13) 0.0348(5) Uani 1 d . . 
O5C O 0.8015(3) 0.8090(2) 0.9042(2) 0.0647(8) Uani 1 d . . 
C1A C 0.2112(3) 0.5370(2) 0.5877(2) 0.0234(6) Uani 1 d . . 
H1AA H 0.1124(3) 0.5076(2) 0.5707(2) 0.028 Uiso 1 calc R . 
C2A C 0.3393(4) 0.4722(2) 0.4711(2) 0.0370(7) Uani 1 d . . 
H2AA H 0.2447(4) 0.4409(2) 0.4537(2) 0.044 Uiso 1 calc R . 
H2AB H 0.4342(4) 0.4421(2) 0.4585(2) 0.044 Uiso 1 calc R . 
C3A C 0.3349(3) 0.5444(2) 0.4139(2) 0.0256(6) Uani 1 d . . 
H3AA H 0.4349(3) 0.5736(2) 0.4277(2) 0.031 Uiso 1 calc R . 
C4A C 0.1956(3) 0.5923(2) 0.4384(2) 0.0227(6) Uani 1 d . . 
H4AA H 0.0956(3) 0.5642(2) 0.4206(2) 0.027 Uiso 1 calc R . 
C5A C 0.1954(4) 0.6666(2) 0.3861(2) 0.0332(7) Uani 1 d . . 
H5AA H 0.2834(4) 0.6989(2) 0.4125(2) 0.040 Uiso 1 calc R . 
H5AB H 0.0952(4) 0.6939(2) 0.3942(2) 0.040 Uiso 1 calc R . 
C6A C 0.2134(3) 0.6530(2) 0.2821(2) 0.0310(6) Uani 1 d . . 
H6AA H 0.2429(3) 0.7020(2) 0.2517(2) 0.037 Uiso 1 calc R . 
C7A C 0.3296(3) 0.5916(2) 0.2590(2) 0.0288(6) Uani 1 d . . 
H7AA H 0.4402(3) 0.6115(2) 0.2611(2) 0.035 Uiso 1 calc R . 
C8A C 0.2687(3) 0.5708(2) 0.1588(2) 0.0297(6) Uani 1 d . . 
H8AA H 0.3048(3) 0.6111(2) 0.1153(2) 0.036 Uiso 1 calc R . 
C9A C 0.0936(3) 0.5795(2) 0.1645(2) 0.0311(7) Uani 1 d . . 
C10A C 0.1583(3) 0.6219(2) 0.7241(2) 0.0266(6) Uani 1 d . . 
H10A H 0.1093(3) 0.6572(2) 0.6806(2) 0.032 Uiso 1 calc R . 
C11A C 0.1667(3) 0.6378(2) 0.8202(2) 0.0334(7) Uani 1 d . . 
H11A H 0.1231(3) 0.6837(2) 0.8423(2) 0.040 Uiso 1 calc R . 
C12A C 0.2382(4) 0.5870(2) 0.8833(2) 0.0389(8) Uani 1 d . . 
H12A H 0.2441(4) 0.5980(2) 0.9490(2) 0.047 Uiso 1 calc R . 
C13A C 0.3011(4) 0.5203(2) 0.8516(2) 0.0386(8) Uani 1 d . . 
H13A H 0.3513(4) 0.4856(2) 0.8954(2) 0.046 Uiso 1 calc R . 
C14A C 0.2918(3) 0.5037(2) 0.7564(2) 0.0294(6) Uani 1 d . . 
H14A H 0.3338(3) 0.4571(2) 0.7349(2) 0.035 Uiso 1 calc R . 
C15A C 0.2210(3) 0.5549(2) 0.6919(2) 0.0220(6) Uani 1 d . . 
C16A C 0.3179(5) 0.4950(2) 0.1221(2) 0.0537(10) Uani 1 d . . 
H16A H 0.4331(5) 0.4936(2) 0.1204(2) 0.081 Uiso 1 calc R . 
H16B H 0.2691(5) 0.4873(2) 0.0582(2) 0.081 Uiso 1 calc R . 
H16C H 0.2838(5) 0.4545(2) 0.1636(2) 0.081 Uiso 1 calc R . 
C1B C 0.1989(3) 0.8980(2) 0.4338(2) 0.0203(5) Uani 1 d . . 
H1BA H 0.2926(3) 0.8639(2) 0.4298(2) 0.024 Uiso 1 calc R . 
C2B C 0.2877(3) 0.9728(2) 0.3101(2) 0.0246(6) Uani 1 d . . 
H2BA H 0.3851(3) 0.9422(2) 0.3065(2) 0.030 Uiso 1 calc R . 
H2BB H 0.3106(3) 1.0258(2) 0.2911(2) 0.030 Uiso 1 calc R . 
C3B C 0.1567(3) 0.9398(2) 0.2448(2) 0.0204(5) Uani 1 d . . 
H3BA H 0.0628(3) 0.9743(2) 0.2421(2) 0.024 Uiso 1 calc R . 
C4B C 0.1123(3) 0.8624(2) 0.2809(2) 0.0199(5) Uani 1 d . . 
H4BA H 0.2045(3) 0.8272(2) 0.2781(2) 0.024 Uiso 1 calc R . 
C5B C -0.0260(3) 0.8306(2) 0.2200(2) 0.0273(6) Uani 1 d . . 
H5BA H -0.0425(3) 0.7765(2) 0.2365(2) 0.033 Uiso 1 calc R . 
H5BB H -0.1230(3) 0.8592(2) 0.2324(2) 0.033 Uiso 1 calc R . 
C6B C 0.0037(3) 0.8367(2) 0.1169(2) 0.0271(6) Uani 1 d . . 
H6BA H -0.0991(3) 0.8314(2) 0.0786(2) 0.033 Uiso 1 calc R . 
C7B C 0.0862(3) 0.9084(2) 0.0859(2) 0.0242(6) Uani 1 d . . 
H7BA H 0.0098(3) 0.9509(2) 0.0718(2) 0.029 Uiso 1 calc R . 
C8B C 0.1595(3) 0.8810(2) -0.0021(2) 0.0271(6) Uani 1 d . . 
H8BA H 0.0744(3) 0.8809(2) -0.0545(2) 0.032 Uiso 1 calc R . 
C9B C 0.1966(3) 0.7991(2) 0.0219(2) 0.0294(7) Uani 1 d . . 
C10B C 0.0747(3) 0.8402(2) 0.5701(2) 0.0275(6) Uani 1 d . . 
H10B H 0.0489(3) 0.7974(2) 0.5310(2) 0.033 Uiso 1 calc R . 
C11B C 0.0323(3) 0.8412(2) 0.6630(2) 0.0322(7) Uani 1 d . . 
H11B H -0.0248(3) 0.7996(2) 0.6868(2) 0.039 Uiso 1 calc R . 
C12B C 0.0724(4) 0.9018(2) 0.7202(2) 0.0399(8) Uani 1 d . . 
H12B H 0.0435(4) 0.9024(2) 0.7837(2) 0.048 Uiso 1 calc R . 
C13B C 0.1547(4) 0.9617(2) 0.6854(2) 0.0400(8) Uani 1 d . . 
H13B H 0.1835(4) 1.0037(2) 0.7253(2) 0.048 Uiso 1 calc R . 
C14B C 0.1962(3) 0.9618(2) 0.5925(2) 0.0314(6) Uani 1 d . . 
H14B H 0.2534(3) 1.0034(2) 0.5689(2) 0.038 Uiso 1 calc R . 
C15B C 0.1540(3) 0.9010(2) 0.5348(2) 0.0204(5) Uani 1 d . . 
C16B C 0.2977(3) 0.9253(2) -0.0364(2) 0.0353(7) Uani 1 d . . 
H16D H 0.2649(3) 0.9778(2) -0.0507(2) 0.053 Uiso 1 calc R . 
H16E H 0.3331(3) 0.9012(2) -0.0936(2) 0.053 Uiso 1 calc R . 
H16F H 0.3845(3) 0.9255(2) 0.0128(2) 0.053 Uiso 1 calc R . 
C1C C 0.6997(3) 0.7322(2) 0.4391(2) 0.0194(5) Uani 1 d . . 
H1CA H 0.7886(3) 0.7683(2) 0.4556(2) 0.023 Uiso 1 calc R . 
C2C C 0.7959(3) 0.6501(2) 0.5601(2) 0.0238(6) Uani 1 d . . 
H2CA H 0.8868(3) 0.6838(2) 0.5775(2) 0.029 Uiso 1 calc R . 
H2CB H 0.8275(3) 0.5968(2) 0.5745(2) 0.029 Uiso 1 calc R . 
C3C C 0.6566(3) 0.6720(2) 0.6147(2) 0.0194(5) Uani 1 d . . 
H3CA H 0.5672(3) 0.6359(2) 0.5994(2) 0.023 Uiso 1 calc R . 
C4C C 0.6065(3) 0.7521(2) 0.5878(2) 0.0197(5) Uani 1 d . . 
H4CA H 0.6960(3) 0.7878(2) 0.6039(2) 0.024 Uiso 1 calc R . 
C5C C 0.4658(3) 0.7758(2) 0.6404(2) 0.0266(6) Uani 1 d . . 
H5CA H 0.3707(3) 0.7480(2) 0.6149(2) 0.032 Uiso 1 calc R . 
H5CB H 0.4465(3) 0.8311(2) 0.6315(2) 0.032 Uiso 1 calc R . 
C6C C 0.4961(3) 0.7584(2) 0.7448(2) 0.0262(6) Uani 1 d . . 
H6CA H 0.3947(3) 0.7626(2) 0.7764(2) 0.031 Uiso 1 calc R . 
C7C C 0.5717(3) 0.6822(2) 0.7686(2) 0.0237(6) Uani 1 d . . 
H7CA H 0.4936(3) 0.6394(2) 0.7652(2) 0.028 Uiso 1 calc R . 
C8C C 0.6401(3) 0.6969(2) 0.8688(2) 0.0284(6) Uani 1 d . . 
H8CA H 0.5508(3) 0.6974(2) 0.9112(2) 0.034 Uiso 1 calc R . 
C9C C 0.6966(4) 0.7774(2) 0.8589(2) 0.0370(7) Uani 1 d . . 
C10C C 0.5668(3) 0.7952(2) 0.2968(2) 0.0275(6) Uani 1 d . . 
H10C H 0.5275(3) 0.8327(2) 0.3373(2) 0.033 Uiso 1 calc R . 
C11C C 0.5325(3) 0.8002(2) 0.2005(2) 0.0355(7) Uani 1 d . . 
H11C H 0.4682(3) 0.8406(2) 0.1752(2) 0.043 Uiso 1 calc R . 
C12C C 0.5911(3) 0.7468(2) 0.1411(2) 0.0345(7) Uani 1 d . . 
H12C H 0.5684(3) 0.7505(2) 0.0747(2) 0.041 Uiso 1 calc R . 
C13C C 0.6840(3) 0.6873(2) 0.1786(2) 0.0308(7) Uani 1 d . . 
H13C H 0.7244(3) 0.6503(2) 0.1378(2) 0.037 Uiso 1 calc R . 
C14C C 0.7173(3) 0.6819(2) 0.2745(2) 0.0248(6) Uani 1 d . . 
H14C H 0.7809(3) 0.6412(2) 0.2997(2) 0.030 Uiso 1 calc R . 
C15C C 0.6582(3) 0.7358(2) 0.3347(2) 0.0212(6) Uani 1 d . . 
C16C C 0.7637(4) 0.6409(2) 0.9094(2) 0.0390(8) Uani 1 d . . 
H16G H 0.7164(4) 0.5901(2) 0.9133(2) 0.059 Uiso 1 calc R . 
H16H H 0.8024(4) 0.6576(2) 0.9727(2) 0.059 Uiso 1 calc R . 
H16I H 0.8520(4) 0.6389(2) 0.8684(2) 0.059 Uiso 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 
O1A 0.0350(10) 0.0388(14) 0.0237(9) -0.0034(8) -0.0013(8) 0.0164(9) 
O2A 0.0286(9) 0.0244(12) 0.0200(9) -0.0034(7) 0.0028(7) 0.0018(8) 
O3A 0.0319(9) 0.0323(13) 0.0215(9) -0.0057(8) 0.0005(7) 0.0059(8) 
O4A 0.0306(9) 0.0425(14) 0.0276(10) 0.0030(9) 0.0018(8) 0.0071(9) 
O5A 0.0460(12) 0.069(2) 0.0351(11) -0.0035(11) -0.0150(10) -0.0124(12) 
O1B 0.0347(9) 0.0192(12) 0.0245(9) -0.0059(7) 0.0062(8) -0.0066(8) 
O2B 0.0198(8) 0.0284(12) 0.0184(8) -0.0026(7) 0.0017(6) -0.0068(8) 
O3B 0.0202(8) 0.0230(11) 0.0200(8) -0.0018(7) 0.0025(6) -0.0032(7) 
O4B 0.0421(10) 0.0273(13) 0.0230(9) -0.0029(8) -0.0012(8) -0.0067(9) 
O5B 0.0473(12) 0.044(2) 0.0353(11) -0.0165(10) 0.0007(9) 0.0059(11) 
O1C 0.0314(9) 0.0221(12) 0.0215(9) 0.0028(7) 0.0035(7) 0.0061(8) 
O2C 0.0198(8) 0.0265(11) 0.0175(8) 0.0012(7) 0.0001(6) 0.0050(7) 
O3C 0.0210(8) 0.0274(12) 0.0177(8) 0.0026(7) 0.0012(6) 0.0017(7) 
O4C 0.0504(12) 0.0246(13) 0.0281(10) -0.0050(8) -0.0073(9) -0.0034(10) 
O5C 0.086(2) 0.050(2) 0.0522(14) -0.0047(12) -0.0352(14) -0.0260(15) 
C1A 0.0168(11) 0.031(2) 0.0224(12) -0.0020(11) 0.0014(10) -0.0003(10) 
C2A 0.049(2) 0.038(2) 0.0239(13) -0.0064(12) -0.0005(12) 0.018(2) 
C3A 0.0212(11) 0.037(2) 0.0191(12) -0.0075(11) 0.0013(9) 0.0002(11) 
C4A 0.0229(11) 0.024(2) 0.0210(12) -0.0062(10) 0.0025(10) 0.0002(10) 
C5A 0.052(2) 0.021(2) 0.0268(14) -0.0048(11) 0.0048(12) 0.0025(14) 
C6A 0.044(2) 0.019(2) 0.0294(14) -0.0011(11) 0.0022(12) -0.0083(13) 
C7A 0.0257(12) 0.035(2) 0.0262(13) -0.0016(12) 0.0068(10) -0.0075(12) 
C8A 0.0355(14) 0.033(2) 0.0215(13) 0.0005(11) 0.0063(11) 0.0018(13) 
C9A 0.0386(14) 0.034(2) 0.0207(13) 0.0039(11) 0.0002(11) -0.0021(13) 
C10A 0.0214(11) 0.034(2) 0.0245(13) -0.0023(11) 0.0002(10) -0.0013(11) 
C11A 0.0323(13) 0.038(2) 0.0303(14) -0.0057(13) 0.0044(12) -0.0021(13) 
C12A 0.044(2) 0.057(2) 0.0160(13) -0.0016(13) 0.0057(12) -0.004(2) 
C13A 0.040(2) 0.051(2) 0.0256(14) 0.0092(14) 0.0015(12) 0.001(2) 
C14A 0.0284(13) 0.033(2) 0.0276(14) 0.0046(12) 0.0044(11) -0.0030(12) 
C15A 0.0150(10) 0.026(2) 0.0247(12) -0.0010(11) 0.0025(9) -0.0056(10) 
C16A 0.077(2) 0.055(3) 0.030(2) -0.009(2) 0.004(2) 0.025(2) 
C1B 0.0186(10) 0.018(2) 0.0235(12) -0.0018(10) -0.0008(9) -0.0005(10) 
C2B 0.0283(12) 0.020(2) 0.0266(13) -0.0045(11) 0.0079(10) -0.0076(11) 
C3B 0.0223(11) 0.019(2) 0.0206(11) -0.0011(10) 0.0047(9) 0.0002(10) 
C4B 0.0184(10) 0.022(2) 0.0191(11) -0.0010(10) 0.0023(9) -0.0029(10) 
C5B 0.0224(11) 0.035(2) 0.0246(13) -0.0013(11) 0.0020(10) -0.0130(12) 
C6B 0.0231(11) 0.033(2) 0.0238(13) -0.0016(11) -0.0062(10) -0.0053(12) 
C7B 0.0207(11) 0.031(2) 0.0207(12) 0.0043(11) -0.0023(9) 0.0026(11) 
C8B 0.0229(11) 0.039(2) 0.0188(12) 0.0039(11) -0.0035(10) -0.0038(12) 
C9B 0.0302(13) 0.040(2) 0.0177(12) -0.0104(12) -0.0049(10) -0.0037(13) 
C10B 0.0255(11) 0.034(2) 0.0227(13) -0.0025(11) -0.0009(10) -0.0019(12) 
C11B 0.0282(12) 0.044(2) 0.0249(13) 0.0040(13) 0.0016(10) -0.0023(13) 
C12B 0.052(2) 0.049(2) 0.0186(13) 0.0030(13) 0.0046(13) 0.011(2) 
C13B 0.062(2) 0.034(2) 0.0234(14) -0.0052(13) -0.0003(13) 0.002(2) 
C14B 0.045(2) 0.024(2) 0.0244(13) 0.0000(11) -0.0039(12) 0.0020(13) 
C15B 0.0190(10) 0.023(2) 0.0186(12) -0.0003(10) -0.0014(9) 0.0057(10) 
C16B 0.0327(14) 0.047(2) 0.0269(14) -0.0015(13) 0.0062(11) -0.0065(14) 
C1C 0.0162(10) 0.019(2) 0.0232(12) 0.0008(10) 0.0020(9) -0.0013(10) 
C2C 0.0259(11) 0.019(2) 0.0265(13) 0.0046(10) -0.0003(10) 0.0041(11) 
C3C 0.0199(10) 0.0182(15) 0.0199(11) -0.0003(10) -0.0007(9) -0.0043(10) 
C4C 0.0202(11) 0.021(2) 0.0174(11) -0.0003(10) -0.0026(9) 0.0018(10) 
C5C 0.0253(12) 0.029(2) 0.0255(13) 0.0006(11) -0.0010(10) 0.0094(11) 
C6C 0.0247(12) 0.030(2) 0.0237(12) -0.0073(11) 0.0016(10) 0.0017(11) 
C7C 0.0221(11) 0.028(2) 0.0214(12) 0.0011(11) 0.0039(9) -0.0009(11) 
C8C 0.0322(13) 0.034(2) 0.0195(12) -0.0006(11) 0.0037(10) -0.0032(13) 
C9C 0.051(2) 0.034(2) 0.0254(14) -0.0037(12) -0.0068(13) -0.0068(15) 
C10C 0.0223(11) 0.036(2) 0.0247(12) 0.0041(12) 0.0038(10) 0.0077(12) 
C11C 0.0253(12) 0.054(2) 0.0270(13) 0.0109(14) 0.0013(11) 0.0090(13) 
C12C 0.0277(13) 0.055(2) 0.0208(13) 0.0021(13) 0.0002(11) -0.0051(14) 
C13C 0.0268(12) 0.038(2) 0.0287(13) -0.0062(12) 0.0063(11) -0.0054(13) 
C14C 0.0215(11) 0.024(2) 0.0287(13) -0.0010(11) 0.0039(10) -0.0012(11) 
C15C 0.0154(10) 0.024(2) 0.0246(12) 0.0003(10) 0.0021(9) -0.0047(10) 
C16C 0.045(2) 0.048(2) 0.0237(14) 0.0077(13) 0.0002(12) 0.007(2) 

_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 
O1A C1A 1.405(3) . ? 
O1A C2A 1.433(3) . ? 
O2A C1A 1.398(3) . ? 
O2A C4A 1.425(3) . ? 
O3A C7A 1.422(4) . ? 
O3A C3A 1.427(3) . ? 
O4A C9A 1.343(4) . ? 
O4A C6A 1.459(3) . ? 
O5A C9A 1.191(3) . ? 
O1B C1B 1.406(3) . ? 
O1B C2B 1.432(3) . ? 
O2B C1B 1.413(3) . ? 
O2B C4B 1.431(3) . ? 
O3B C3B 1.419(3) . ? 
O3B C7B 1.434(3) . ? 
O4B C9B 1.345(3) . ? 
O4B C6B 1.459(4) . ? 
O5B C9B 1.207(3) . ? 
O1C C1C 1.399(3) . ? 
O1C C2C 1.432(3) . ? 
O2C C1C 1.411(3) . ? 
O2C C4C 1.438(3) . ? 
O3C C3C 1.422(3) . ? 
O3C C7C 1.428(3) . ? 
O4C C9C 1.348(4) . ? 
O4C C6C 1.461(3) . ? 
O5C C9C 1.199(4) . ? 
C1A C15A 1.509(3) . ? 
C2A C3A 1.502(4) . ? 
C3A C4A 1.510(4) . ? 
C4A C5A 1.499(4) . ? 
C5A C6A 1.513(4) . ? 
C6A C7A 1.512(4) . ? 
C7A C8A 1.523(4) . ? 
C8A C16A 1.498(5) . ? 
C8A C9A 1.502(4) . ? 
C10A C15A 1.381(4) . ? 
C10A C11A 1.389(4) . ? 
C11A C12A 1.374(5) . ? 
C12A C13A 1.374(5) . ? 
C13A C14A 1.379(4) . ? 
C14A C15A 1.389(4) . ? 
C1B C15B 1.509(3) . ? 
C2B C3B 1.514(3) . ? 
C3B C4B 1.507(4) . ? 
C4B C5B 1.516(3) . ? 
C5B C6B 1.506(4) . ? 
C6B C7B 1.518(4) . ? 
C7B C8B 1.512(4) . ? 
C8B C9B 1.503(5) . ? 
C8B C16B 1.515(4) . ? 
C10B C15B 1.374(4) . ? 
C10B C11B 1.392(4) . ? 
C11B C12B 1.365(5) . ? 
C12B C13B 1.374(5) . ? 
C13B C14B 1.388(4) . ? 
C14B C15B 1.377(4) . ? 
C1C C15C 1.501(3) . ? 
C2C C3C 1.508(3) . ? 
C3C C4C 1.509(4) . ? 
C4C C5C 1.509(3) . ? 
C5C C6C 1.518(3) . ? 
C6C C7C 1.511(4) . ? 
C7C C8C 1.520(3) . ? 
C8C C9C 1.500(5) . ? 
C8C C16C 1.523(4) . ? 
C10C C11C 1.380(4) . ? 
C10C C15C 1.384(4) . ? 
C11C C12C 1.376(5) . ? 
C12C C13C 1.391(4) . ? 
C13C C14C 1.374(4) . ? 
C14C C15C 1.392(4) . ? 

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 
C1A O1A C2A 110.9(2) . . ? 
C1A O2A C4A 111.0(2) . . ? 
C7A O3A C3A 111.0(2) . . ? 
C9A O4A C6A 109.7(2) . . ? 
C1B O1B C2B 112.2(2) . . ? 
C1B O2B C4B 109.9(2) . . ? 
C3B O3B C7B 111.5(2) . . ? 
C9B O4B C6B 109.2(2) . . ? 
C1C O1C C2C 111.8(2) . . ? 
C1C O2C C4C 109.8(2) . . ? 
C3C O3C C7C 111.3(2) . . ? 
C9C O4C C6C 109.2(2) . . ? 
O2A C1A O1A 112.0(2) . . ? 
O2A C1A C15A 108.5(2) . . ? 
O1A C1A C15A 108.0(2) . . ? 
O1A C2A C3A 108.2(2) . . ? 
O3A C3A C2A 109.1(2) . . ? 
O3A C3A C4A 109.0(2) . . ? 
C2A C3A C4A 109.6(2) . . ? 
O2A C4A C5A 110.1(2) . . ? 
O2A C4A C3A 108.4(2) . . ? 
C5A C4A C3A 110.2(2) . . ? 
C4A C5A C6A 110.5(2) . . ? 
O4A C6A C7A 103.0(2) . . ? 
O4A C6A C5A 109.7(2) . . ? 
C7A C6A C5A 115.8(2) . . ? 
O3A C7A C6A 112.7(2) . . ? 
O3A C7A C8A 107.7(2) . . ? 
C6A C7A C8A 100.9(2) . . ? 
C16A C8A C9A 114.2(3) . . ? 
C16A C8A C7A 116.9(2) . . ? 
C9A C8A C7A 101.5(2) . . ? 
O5A C9A O4A 122.0(3) . . ? 
O5A C9A C8A 128.3(3) . . ? 
O4A C9A C8A 109.6(2) . . ? 
C15A C10A C11A 120.0(3) . . ? 
C12A C11A C10A 120.1(3) . . ? 
C11A C12A C13A 120.1(3) . . ? 
C12A C13A C14A 120.2(3) . . ? 
C13A C14A C15A 120.1(3) . . ? 
C10A C15A C14A 119.4(2) . . ? 
C10A C15A C1A 120.3(2) . . ? 
C14A C15A C1A 120.2(3) . . ? 
O1B C1B O2B 111.1(2) . . ? 
O1B C1B C15B 109.2(2) . . ? 
O2B C1B C15B 108.8(2) . . ? 
O1B C2B C3B 108.5(2) . . ? 
O3B C3B C4B 108.5(2) . . ? 
O3B C3B C2B 109.3(2) . . ? 
C4B C3B C2B 109.1(2) . . ? 
O2B C4B C3B 110.1(2) . . ? 
O2B C4B C5B 109.6(2) . . ? 
C3B C4B C5B 109.8(2) . . ? 
C6B C5B C4B 110.7(2) . . ? 
O4B C6B C5B 109.4(2) . . ? 
O4B C6B C7B 103.8(2) . . ? 
C5B C6B C7B 116.8(2) . . ? 
O3B C7B C8B 108.1(2) . . ? 
O3B C7B C6B 111.7(2) . . ? 
C8B C7B C6B 101.5(2) . . ? 
C9B C8B C7B 102.0(2) . . ? 
C9B C8B C16B 114.1(2) . . ? 
C7B C8B C16B 118.3(2) . . ? 
O5B C9B O4B 121.5(3) . . ? 
O5B C9B C8B 128.2(3) . . ? 
O4B C9B C8B 110.3(2) . . ? 
C15B C10B C11B 120.1(3) . . ? 
C12B C11B C10B 120.2(3) . . ? 
C11B C12B C13B 119.6(3) . . ? 
C12B C13B C14B 120.7(3) . . ? 
C15B C14B C13B 119.5(3) . . ? 
C10B C15B C14B 119.9(2) . . ? 
C10B C15B C1B 118.8(2) . . ? 
C14B C15B C1B 121.3(2) . . ? 
O1C C1C O2C 112.2(2) . . ? 
O1C C1C C15C 108.2(2) . . ? 
O2C C1C C15C 109.3(2) . . ? 
O1C C2C C3C 107.6(2) . . ? 
O3C C3C C2C 108.7(2) . . ? 
O3C C3C C4C 110.1(2) . . ? 
C2C C3C C4C 108.9(2) . . ? 
O2C C4C C3C 108.4(2) . . ? 
O2C C4C C5C 110.2(2) . . ? 
C3C C4C C5C 110.5(2) . . ? 
C4C C5C C6C 109.9(2) . . ? 
O4C C6C C7C 102.7(2) . . ? 
O4C C6C C5C 110.2(2) . . ? 
C7C C6C C5C 115.9(2) . . ? 
O3C C7C C6C 111.2(2) . . ? 
O3C C7C C8C 106.6(2) . . ? 
C6C C7C C8C 100.8(2) . . ? 
C9C C8C C7C 100.2(2) . . ? 
C9C C8C C16C 115.2(2) . . ? 
C7C C8C C16C 117.0(3) . . ? 
O5C C9C O4C 122.2(3) . . ? 
O5C C9C C8C 128.0(3) . . ? 
O4C C9C C8C 109.7(2) . . ? 
C11C C10C C15C 120.5(3) . . ? 
C12C C11C C10C 120.2(3) . . ? 
C11C C12C C13C 119.6(2) . . ? 
C14C C13C C12C 120.3(3) . . ? 
C13C C14C C15C 120.2(3) . . ? 
C10C C15C C14C 119.3(2) . . ? 
C10C C15C C1C 120.2(2) . . ? 
C14C C15C C1C 120.5(2) . . ? 

_refine_diff_density_max    0.311 
_refine_diff_density_min   -0.255 
_refine_diff_density_rms    0.054