# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 207/311

data_pr9822 #Compound 43
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 "J. Chem. Soc., Perkin Transactions 
 Paper 9/00278B
 General Synthesis of 3-phosphorylated myo-inositol phospholipids 
 and their derivatives
 G.F. Painter, S.J.A. Grove, I.H. Gilbert, A.B. Holmes, P.R. Raithby
 M.L. Hill, P.T. Hawkins and L.R. Stephens"
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C52 H56 O10' 
_chemical_formula_weight          840.97 
 
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            Triclinic
_symmetry_space_group_name_H-M    P1 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 
_cell_length_a                    6.164(9) 
_cell_length_b                    14.114(5) 
_cell_length_c                    14.378(5) 
_cell_angle_alpha                 64.94(4) 
_cell_angle_beta                  86.34(4) 
_cell_angle_gamma                 80.33(4) 
_cell_volume                      1117.0(17) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     'Post data collection refinement' 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             White 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.250 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              448 
_exptl_absorpt_coefficient_mu     0.086 
_exptl_absorpt_correction_type    'Interframe scaling' 
_exptl_absorpt_correction_T_min   0.9747 
_exptl_absorpt_correction_T_max   0.9915 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       180(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   RAXIS-IIC
_diffrn_measurement_method        '2 sets of 30 frames, 6 deg. per frame' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6913 
_diffrn_reflns_av_R_equivalents   0.0700 
_diffrn_reflns_av_sigmaI/netI     0.1233 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          3.55 
_diffrn_reflns_theta_max          25.20 
_reflns_number_total              3875 
_reflns_number_gt                 2922 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Rigaku control software' 
_computing_cell_refinement        'Rigaku control software'  
_computing_data_reduction         TeXsan  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL-PLUS (Sheldrick, 1991)' 
_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 w=1/[\s^2^(Fo^2^)+(0.0470P)^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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.282(14) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -1.5(13) 
_refine_ls_number_reflns          3875 
_refine_ls_number_parameters      564 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0736 
_refine_ls_R_factor_gt            0.0553 
_refine_ls_wR_factor_ref          0.1163 
_refine_ls_wR_factor_gt           0.1078 
_refine_ls_goodness_of_fit_ref    1.012 
_refine_ls_restrained_S_all       1.011 
_refine_ls_shift/su_max           0.024 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O -0.0451(5) 1.3769(2) -0.0816(2) 0.0323(7) Uani 1 d . . . 
O2 O -0.3876(5) 1.4963(2) -0.2324(2) 0.0363(8) Uani 1 d . . . 
O3 O -0.1879(5) 1.4321(2) -0.3861(2) 0.0360(8) Uani 1 d . . . 
O4 O 0.1816(5) 1.2716(2) -0.3213(2) 0.0331(7) Uani 1 d . . . 
O5 O 0.1470(5) 1.1015(2) -0.1227(2) 0.0326(7) Uani 1 d . . . 
O6 O -0.0520(5) 1.1576(2) 0.0299(2) 0.0313(7) Uani 1 d . . . 
O7 O -0.3948(5) 1.1219(3) 0.0800(2) 0.0427(9) Uani 1 d . . . 
O8 O -0.9345(5) 1.9597(3) -0.3773(3) 0.0450(9) Uani 1 d . . . 
O9 O -0.3004(6) 0.8981(3) 0.4391(2) 0.0557(11) Uani 1 d . . . 
O10 O -0.2755(5) 1.0231(3) 0.2785(2) 0.0362(8) Uani 1 d . . . 
C1 C -0.2199(7) 1.3306(4) -0.0991(3) 0.0295(10) Uani 1 d . . . 
H1 H -0.3446 1.3331 -0.0517 0.035 Uiso 1 calc R . . 
C2 C -0.3005(7) 1.3886(3) -0.2099(3) 0.0294(10) Uani 1 d . . . 
H2 H -0.4185 1.3533 -0.2204 0.035 Uiso 1 calc R . . 
C3 C -0.1085(8) 1.3843(4) -0.2823(3) 0.0311(10) Uani 1 d . . . 
H3 H 0.0050 1.4240 -0.2754 0.037 Uiso 1 calc R . . 
C4 C -0.0047(7) 1.2705(4) -0.2565(3) 0.0295(10) Uani 1 d . . . 
H4 H -0.1142 1.2334 -0.2709 0.035 Uiso 1 calc R . . 
C5 C 0.0696(7) 1.2096(4) -0.1442(3) 0.0285(10) Uani 1 d . . . 
H5 H 0.1891 1.2419 -0.1302 0.034 Uiso 1 calc R . . 
C6 C -0.1278(7) 1.2157(4) -0.0766(3) 0.0300(10) Uani 1 d . . . 
H6 H -0.2446 1.1813 -0.0894 0.036 Uiso 1 calc R . . 
C10 C -0.1071(8) 1.4530(4) -0.0395(4) 0.0449(13) Uani 1 d . . . 
H10A H -0.2358 1.4353 0.0060 0.054 Uiso 1 calc R . . 
H10B H -0.1468 1.5247 -0.0952 0.054 Uiso 1 calc R . . 
C11 C 0.0883(9) 1.4497(4) 0.0209(3) 0.0418(12) Uani 1 d . . . 
C12 C 0.1542(9) 1.5411(4) 0.0126(4) 0.0433(12) Uani 1 d . . . 
H12 H 0.0829 1.6077 -0.0353 0.052 Uiso 1 calc R . . 
C13 C 0.3251(9) 1.5369(5) 0.0740(4) 0.0471(13) Uani 1 d . . . 
H13 H 0.3658 1.6012 0.0681 0.057 Uiso 1 calc R . . 
C14 C 0.4339(12) 1.4445(5) 0.1414(5) 0.0658(18) Uani 1 d . . . 
H14 H 0.5423 1.4433 0.1861 0.079 Uiso 1 calc R . . 
C15 C 0.3853(14) 1.3513(6) 0.1442(6) 0.094(3) Uani 1 d . . . 
H15 H 0.4686 1.2856 0.1874 0.113 Uiso 1 calc R . . 
C16 C 0.2162(13) 1.3532(5) 0.0847(5) 0.081(2) Uani 1 d . . . 
H16 H 0.1855 1.2886 0.0867 0.097 Uiso 1 calc R . . 
C20 C -0.6094(8) 1.5254(4) -0.2694(5) 0.0473(14) Uani 1 d . . . 
H20A H -0.7048 1.4812 -0.2163 0.057 Uiso 1 calc R . . 
H20B H -0.6175 1.5121 -0.3313 0.057 Uiso 1 calc R . . 
C21 C -0.6910(7) 1.6397(4) -0.2953(3) 0.0333(11) Uani 1 d . . . 
C22 C -0.5607(7) 1.7199(4) -0.3423(4) 0.0394(12) Uani 1 d . . . 
H22 H -0.4105 1.7015 -0.3560 0.047 Uiso 1 calc R . . 
C23 C -0.6459(7) 1.8241(4) -0.3687(4) 0.0357(11) Uani 1 d . . . 
H23 H -0.5544 1.8770 -0.4001 0.043 Uiso 1 calc R . . 
C24 C -0.8663(7) 1.8531(4) -0.3497(3) 0.0315(10) Uani 1 d . . . 
C25 C -0.9998(8) 1.7759(4) -0.3050(4) 0.0359(11) Uani 1 d . . . 
H25 H -1.1505 1.7950 -0.2925 0.043 Uiso 1 calc R . . 
C26 C -0.9120(8) 1.6704(4) -0.2786(4) 0.0373(12) Uani 1 d . . . 
H26 H -1.0047 1.6179 -0.2483 0.045 Uiso 1 calc R . . 
C27 C -1.1616(8) 1.9929(4) -0.3624(4) 0.0492(14) Uani 1 d . . . 
H27A H -1.1885 2.0697 -0.3839 0.074 Uiso 1 calc R . . 
H27B H -1.1979 1.9572 -0.2896 0.074 Uiso 1 calc R . . 
H27C H -1.2539 1.9746 -0.4034 0.074 Uiso 1 calc R . . 
C30 C -0.0830(12) 1.5191(5) -0.4525(4) 0.0624(18) Uani 1 d . . . 
H30A H 0.0788 1.4989 -0.4451 0.075 Uiso 1 calc R . . 
H30B H -0.1270 1.5799 -0.4344 0.075 Uiso 1 calc R . . 
C31 C -0.1497(8) 1.5490(4) -0.5596(3) 0.0364(11) Uani 1 d . . . 
C32 C 0.0041(10) 1.5276(5) -0.6268(5) 0.0634(17) Uani 1 d . . . 
H32 H 0.1509 1.4953 -0.6048 0.076 Uiso 1 calc R . . 
C33 C -0.0636(17) 1.5549(8) -0.7277(6) 0.094(3) Uani 1 d . . . 
H33 H 0.0382 1.5416 -0.7748 0.113 Uiso 1 calc R . . 
C34 C -0.2716(19) 1.5997(7) -0.7573(5) 0.090(3) Uani 1 d . . . 
H34 H -0.3151 1.6169 -0.8255 0.108 Uiso 1 calc R . . 
C35 C -0.4229(13) 1.6212(6) -0.6927(6) 0.078(2) Uani 1 d . . . 
H35 H -0.5690 1.6542 -0.7154 0.093 Uiso 1 calc R . . 
C36 C -0.3597(10) 1.5945(4) -0.5964(4) 0.0549(15) Uani 1 d . . . 
H36 H -0.4661 1.6078 -0.5508 0.066 Uiso 1 calc R . . 
C40 C 0.1723(8) 1.2098(4) -0.3768(4) 0.0400(12) Uani 1 d . . . 
H40A H 0.0277 1.2303 -0.4119 0.048 Uiso 1 calc R . . 
H40B H 0.1866 1.1341 -0.3285 0.048 Uiso 1 calc R . . 
C41 C 0.3534(7) 1.2251(4) -0.4554(3) 0.0326(11) Uani 1 d . . . 
C42 C 0.4987(7) 1.2954(4) -0.4717(3) 0.0369(11) Uani 1 d . . . 
H42 H 0.4879 1.3351 -0.4318 0.044 Uiso 1 calc R . . 
C43 C 0.6612(9) 1.3081(4) -0.5466(4) 0.0476(13) Uani 1 d . . . 
H43 H 0.7601 1.3567 -0.5579 0.057 Uiso 1 calc R . . 
C44 C 0.6778(9) 1.2499(4) -0.6041(4) 0.0508(14) Uani 1 d . . . 
H44 H 0.7885 1.2585 -0.6549 0.061 Uiso 1 calc R . . 
C45 C 0.5336(10) 1.1789(4) -0.5881(4) 0.0520(14) Uani 1 d . . . 
H45 H 0.5438 1.1390 -0.6278 0.062 Uiso 1 calc R . . 
C46 C 0.3737(9) 1.1670(4) -0.5128(4) 0.0414(12) Uani 1 d . . . 
H46 H 0.2762 1.1176 -0.5007 0.050 Uiso 1 calc R . . 
C50 C 0.3821(7) 1.0780(4) -0.1169(4) 0.0348(11) Uani 1 d . . . 
H50A H 0.4344 1.0873 -0.0580 0.042 Uiso 1 calc R . . 
H50B H 0.4452 1.1277 -0.1803 0.042 Uiso 1 calc R . . 
C51 C 0.4589(7) 0.9657(4) -0.1039(3) 0.0306(10) Uani 1 d . . . 
C52 C 0.3289(7) 0.9084(4) -0.1283(4) 0.0385(11) Uani 1 d . . . 
H52 H 0.1822 0.9388 -0.1519 0.046 Uiso 1 calc R . . 
C53 C 0.4107(9) 0.8069(4) -0.1186(4) 0.0445(12) Uani 1 d . . . 
H53 H 0.3228 0.7689 -0.1380 0.053 Uiso 1 calc R . . 
C54 C 0.6212(9) 0.7617(4) -0.0806(4) 0.0455(13) Uani 1 d . . . 
H54 H 0.6758 0.6912 -0.0716 0.055 Uiso 1 calc R . . 
C55 C 0.7524(9) 0.8168(4) -0.0556(4) 0.0507(14) Uani 1 d . . . 
H55 H 0.8972 0.7850 -0.0299 0.061 Uiso 1 calc R . . 
C56 C 0.6731(8) 0.9189(4) -0.0679(4) 0.0406(12) Uani 1 d . . . 
H56 H 0.7650 0.9576 -0.0518 0.049 Uiso 1 calc R . . 
C60 C -0.2042(7) 1.1124(3) 0.0994(3) 0.0290(10) Uani 1 d . . . 
C61 C -0.0972(7) 1.0460(4) 0.2043(3) 0.0292(10) Uani 1 d . . . 
C62 C 0.0635(8) 1.0916(4) 0.2441(3) 0.0381(11) Uani 1 d . . . 
H62A H -0.0130 1.1496 0.2613 0.046 Uiso 1 calc R . . 
H62B H 0.1802 1.1181 0.1935 0.046 Uiso 1 calc R . . 
C63 C 0.1582(8) 0.9939(4) 0.3414(4) 0.0393(12) Uani 1 d . . . 
H63A H 0.1199 1.0057 0.4040 0.047 Uiso 1 calc R . . 
H63B H 0.3203 0.9779 0.3376 0.047 Uiso 1 calc R . . 
C64 C 0.0461(7) 0.9022(4) 0.3412(3) 0.0314(10) Uani 1 d . . . 
C65 C -0.1890(8) 0.9344(4) 0.3636(3) 0.0375(11) Uani 1 d . . . 
C66 C 0.0228(7) 0.9326(3) 0.2245(3) 0.0288(10) Uani 1 d . . . 
C67 C 0.2413(8) 0.9300(4) 0.1678(4) 0.0455(14) Uani 1 d . . . 
H67A H 0.3355 0.9716 0.1824 0.068 Uiso 1 calc R . . 
H67B H 0.2129 0.9601 0.0937 0.068 Uiso 1 calc R . . 
H67C H 0.3153 0.8566 0.1910 0.068 Uiso 1 calc R . . 
C68 C -0.1210(9) 0.8651(4) 0.2026(4) 0.0441(12) Uani 1 d . . . 
H68A H -0.0463 0.7916 0.2283 0.066 Uiso 1 calc R . . 
H68B H -0.1456 0.8930 0.1284 0.066 Uiso 1 calc R . . 
H68C H -0.2628 0.8677 0.2371 0.066 Uiso 1 calc R . . 
C69 C 0.1480(9) 0.7917(4) 0.4114(3) 0.0421(12) Uani 1 d . . . 
H69A H 0.1316 0.7824 0.4829 0.063 Uiso 1 calc R . . 
H69B H 0.3046 0.7804 0.3956 0.063 Uiso 1 calc R . . 
H69C H 0.0740 0.7404 0.4014 0.063 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 
O1 0.0306(16) 0.0361(19) 0.0368(16) -0.0211(14) -0.0013(14) -0.0062(14) 
O2 0.0337(18) 0.0282(19) 0.0438(17) -0.0124(15) -0.0109(15) 0.0005(14) 
O3 0.0445(19) 0.0322(19) 0.0281(16) -0.0064(13) -0.0018(14) -0.0141(15) 
O4 0.0343(17) 0.0382(19) 0.0337(16) -0.0212(14) 0.0080(13) -0.0093(14) 
O5 0.0286(17) 0.0262(17) 0.0417(17) -0.0138(14) -0.0008(14) -0.0018(13) 
O6 0.0277(16) 0.0356(19) 0.0242(14) -0.0053(12) 0.0018(12) -0.0091(13) 
O7 0.0260(18) 0.056(2) 0.0358(17) -0.0082(15) -0.0029(14) -0.0102(16) 
O8 0.0373(19) 0.031(2) 0.058(2) -0.0114(16) -0.0054(16) -0.0023(15) 
O9 0.044(2) 0.073(3) 0.0328(18) -0.0058(17) 0.0118(16) -0.0125(19) 
O10 0.0269(16) 0.044(2) 0.0313(16) -0.0117(14) 0.0060(13) -0.0013(14) 
C1 0.027(2) 0.028(3) 0.036(2) -0.0147(19) 0.0006(19) -0.0054(19) 
C2 0.029(2) 0.023(2) 0.036(2) -0.0101(19) -0.0012(19) -0.0072(19) 
C3 0.035(2) 0.025(3) 0.031(2) -0.0081(19) -0.0027(19) -0.007(2) 
C4 0.030(2) 0.031(3) 0.031(2) -0.0143(19) 0.0059(18) -0.011(2) 
C5 0.025(2) 0.028(3) 0.032(2) -0.0116(19) -0.0011(18) -0.0037(19) 
C6 0.030(2) 0.030(3) 0.025(2) -0.0069(18) -0.0040(18) -0.001(2) 
C10 0.049(3) 0.043(3) 0.050(3) -0.027(2) 0.000(2) -0.010(3) 
C11 0.056(3) 0.034(3) 0.038(3) -0.015(2) 0.000(2) -0.013(2) 
C12 0.049(3) 0.035(3) 0.049(3) -0.020(2) 0.000(2) -0.010(2) 
C13 0.048(3) 0.053(4) 0.048(3) -0.025(3) 0.002(3) -0.022(3) 
C14 0.090(5) 0.058(4) 0.060(4) -0.030(3) -0.026(4) -0.017(4) 
C15 0.120(7) 0.068(5) 0.082(5) -0.011(4) -0.066(5) -0.014(5) 
C16 0.130(6) 0.038(4) 0.065(4) -0.003(3) -0.038(4) -0.025(4) 
C20 0.028(3) 0.039(3) 0.076(4) -0.025(3) -0.008(2) -0.004(2) 
C21 0.029(2) 0.031(3) 0.036(2) -0.010(2) -0.007(2) -0.003(2) 
C22 0.024(2) 0.046(3) 0.052(3) -0.024(2) 0.002(2) -0.004(2) 
C23 0.029(2) 0.032(3) 0.046(3) -0.015(2) 0.004(2) -0.012(2) 
C24 0.033(2) 0.028(3) 0.029(2) -0.0088(19) -0.0043(19) -0.002(2) 
C25 0.025(2) 0.034(3) 0.047(3) -0.017(2) -0.001(2) -0.001(2) 
C26 0.033(3) 0.031(3) 0.043(3) -0.011(2) 0.005(2) -0.008(2) 
C27 0.037(3) 0.040(3) 0.069(4) -0.024(3) -0.001(3) 0.001(2) 
C30 0.102(5) 0.045(4) 0.038(3) -0.005(2) 0.001(3) -0.044(4) 
C31 0.050(3) 0.025(3) 0.033(2) -0.010(2) 0.001(2) -0.008(2) 
C32 0.053(4) 0.056(4) 0.085(4) -0.032(3) 0.020(3) -0.020(3) 
C33 0.137(8) 0.126(7) 0.064(4) -0.067(5) 0.072(5) -0.090(6) 
C34 0.142(8) 0.093(6) 0.041(3) -0.009(4) -0.012(5) -0.078(6) 
C35 0.082(5) 0.057(5) 0.069(5) 0.004(3) -0.022(4) -0.020(4) 
C36 0.066(4) 0.036(3) 0.053(3) -0.010(3) 0.004(3) -0.007(3) 
C40 0.040(3) 0.045(3) 0.047(3) -0.029(2) 0.009(2) -0.015(2) 
C41 0.032(2) 0.033(3) 0.034(2) -0.016(2) 0.0009(19) -0.003(2) 
C42 0.038(3) 0.038(3) 0.039(2) -0.022(2) 0.005(2) -0.003(2) 
C43 0.050(3) 0.045(3) 0.050(3) -0.021(3) 0.014(2) -0.017(3) 
C44 0.061(3) 0.044(3) 0.040(3) -0.016(2) 0.013(3) 0.002(3) 
C45 0.079(4) 0.034(3) 0.044(3) -0.020(2) 0.007(3) -0.001(3) 
C46 0.051(3) 0.032(3) 0.038(2) -0.011(2) -0.001(2) -0.010(2) 
C50 0.026(2) 0.035(3) 0.048(3) -0.022(2) -0.001(2) -0.003(2) 
C51 0.028(2) 0.036(3) 0.026(2) -0.0140(19) 0.0055(18) -0.001(2) 
C52 0.027(2) 0.036(3) 0.051(3) -0.019(2) -0.003(2) 0.001(2) 
C53 0.051(3) 0.035(3) 0.049(3) -0.020(2) 0.001(2) -0.008(2) 
C54 0.050(3) 0.030(3) 0.051(3) -0.016(2) 0.002(3) 0.005(2) 
C55 0.040(3) 0.041(3) 0.065(4) -0.019(3) -0.010(3) 0.003(3) 
C56 0.037(3) 0.043(3) 0.047(3) -0.025(2) -0.007(2) -0.001(2) 
C60 0.030(2) 0.025(2) 0.031(2) -0.0116(18) 0.0028(19) -0.0043(19) 
C61 0.023(2) 0.035(3) 0.029(2) -0.0133(19) 0.0107(18) -0.0094(19) 
C62 0.040(3) 0.038(3) 0.036(3) -0.014(2) 0.001(2) -0.012(2) 
C63 0.039(3) 0.040(3) 0.036(2) -0.012(2) -0.001(2) -0.012(2) 
C64 0.029(2) 0.038(3) 0.026(2) -0.0113(19) 0.0042(18) -0.009(2) 
C65 0.037(3) 0.040(3) 0.031(2) -0.010(2) 0.004(2) -0.007(2) 
C66 0.029(2) 0.028(2) 0.025(2) -0.0079(18) 0.0037(18) -0.0024(19) 
C67 0.036(3) 0.048(3) 0.042(3) -0.017(2) 0.012(2) 0.008(2) 
C68 0.059(3) 0.034(3) 0.041(2) -0.016(2) -0.005(2) -0.012(2) 
C69 0.047(3) 0.041(3) 0.035(3) -0.011(2) -0.002(2) -0.010(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 
O1 C10 1.431(6) . ? 
O1 C1 1.437(6) . ? 
O2 C2 1.427(5) . ? 
O2 C20 1.428(6) . ? 
O3 C30 1.426(6) . ? 
O3 C3 1.432(5) . ? 
O4 C40 1.419(6) . ? 
O4 C4 1.429(5) . ? 
O5 C5 1.424(5) . ? 
O5 C50 1.430(6) . ? 
O6 C60 1.351(5) . ? 
O6 C6 1.461(5) . ? 
O7 C60 1.197(5) . ? 
O8 C24 1.379(6) . ? 
O8 C27 1.433(6) . ? 
O9 C65 1.211(5) . ? 
O10 C65 1.381(6) . ? 
O10 C61 1.459(5) . ? 
C1 C2 1.521(6) . ? 
C1 C6 1.524(6) . ? 
C2 C3 1.536(6) . ? 
C3 C4 1.520(6) . ? 
C4 C5 1.531(6) . ? 
C5 C6 1.522(6) . ? 
C10 C11 1.512(7) . ? 
C11 C12 1.373(7) . ? 
C11 C16 1.411(8) . ? 
C12 C13 1.396(7) . ? 
C13 C14 1.344(8) . ? 
C14 C15 1.381(9) . ? 
C15 C16 1.380(9) . ? 
C20 C21 1.495(7) . ? 
C21 C26 1.396(7) . ? 
C21 C22 1.404(7) . ? 
C22 C23 1.370(7) . ? 
C23 C24 1.396(6) . ? 
C24 C25 1.385(7) . ? 
C25 C26 1.389(7) . ? 
C30 C31 1.480(7) . ? 
C31 C36 1.375(7) . ? 
C31 C32 1.399(8) . ? 
C32 C33 1.405(11) . ? 
C33 C34 1.339(12) . ? 
C34 C35 1.363(12) . ? 
C35 C36 1.337(9) . ? 
C40 C41 1.511(6) . ? 
C41 C46 1.376(7) . ? 
C41 C42 1.384(6) . ? 
C42 C43 1.398(6) . ? 
C43 C44 1.380(8) . ? 
C44 C45 1.388(8) . ? 
C45 C46 1.392(7) . ? 
C50 C51 1.509(6) . ? 
C51 C52 1.383(7) . ? 
C51 C56 1.398(7) . ? 
C52 C53 1.387(7) . ? 
C53 C54 1.381(7) . ? 
C54 C55 1.369(8) . ? 
C55 C56 1.379(7) . ? 
C60 C61 1.520(6) . ? 
C61 C62 1.523(7) . ? 
C61 C66 1.560(6) . ? 
C62 C63 1.549(7) . ? 
C63 C64 1.567(7) . ? 
C64 C65 1.501(6) . ? 
C64 C69 1.505(7) . ? 
C64 C66 1.556(6) . ? 
C66 C67 1.532(6) . ? 
C66 C68 1.538(7) . ? 
 
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 
C10 O1 C1 116.3(4) . . ? 
C2 O2 C20 112.9(3) . . ? 
C30 O3 C3 114.0(4) . . ? 
C40 O4 C4 112.6(3) . . ? 
C5 O5 C50 111.9(3) . . ? 
C60 O6 C6 116.2(3) . . ? 
C24 O8 C27 117.4(4) . . ? 
C65 O10 C61 105.6(3) . . ? 
O1 C1 C2 110.9(4) . . ? 
O1 C1 C6 107.2(4) . . ? 
C2 C1 C6 109.5(3) . . ? 
O2 C2 C1 110.3(4) . . ? 
O2 C2 C3 109.6(3) . . ? 
C1 C2 C3 109.5(4) . . ? 
O3 C3 C4 108.6(4) . . ? 
O3 C3 C2 109.5(4) . . ? 
C4 C3 C2 110.8(3) . . ? 
O4 C4 C3 108.3(3) . . ? 
O4 C4 C5 109.1(4) . . ? 
C3 C4 C5 112.7(4) . . ? 
O5 C5 C6 109.0(3) . . ? 
O5 C5 C4 110.0(4) . . ? 
C6 C5 C4 108.2(3) . . ? 
O6 C6 C5 107.1(3) . . ? 
O6 C6 C1 110.7(3) . . ? 
C5 C6 C1 110.8(4) . . ? 
O1 C10 C11 107.3(4) . . ? 
C12 C11 C16 117.0(5) . . ? 
C12 C11 C10 121.2(5) . . ? 
C16 C11 C10 121.8(5) . . ? 
C11 C12 C13 120.5(5) . . ? 
C14 C13 C12 121.9(6) . . ? 
C13 C14 C15 118.7(6) . . ? 
C16 C15 C14 120.3(7) . . ? 
C15 C16 C11 121.0(7) . . ? 
O2 C20 C21 111.0(4) . . ? 
C26 C21 C22 117.5(4) . . ? 
C26 C21 C20 118.9(4) . . ? 
C22 C21 C20 123.5(4) . . ? 
C23 C22 C21 121.3(4) . . ? 
C22 C23 C24 120.4(4) . . ? 
O8 C24 C25 124.6(4) . . ? 
O8 C24 C23 115.8(4) . . ? 
C25 C24 C23 119.6(4) . . ? 
C24 C25 C26 119.6(4) . . ? 
C25 C26 C21 121.6(4) . . ? 
O3 C30 C31 108.6(4) . . ? 
C36 C31 C32 117.6(5) . . ? 
C36 C31 C30 123.0(5) . . ? 
C32 C31 C30 119.4(5) . . ? 
C31 C32 C33 118.5(7) . . ? 
C34 C33 C32 120.0(6) . . ? 
C33 C34 C35 122.1(6) . . ? 
C36 C35 C34 118.1(7) . . ? 
C35 C36 C31 123.7(6) . . ? 
O4 C40 C41 111.2(4) . . ? 
C46 C41 C42 119.1(4) . . ? 
C46 C41 C40 118.6(4) . . ? 
C42 C41 C40 122.3(4) . . ? 
C41 C42 C43 120.2(5) . . ? 
C44 C43 C42 119.9(5) . . ? 
C43 C44 C45 120.3(5) . . ? 
C44 C45 C46 118.9(5) . . ? 
C41 C46 C45 121.6(5) . . ? 
O5 C50 C51 110.4(4) . . ? 
C52 C51 C56 118.8(4) . . ? 
C52 C51 C50 123.0(4) . . ? 
C56 C51 C50 118.2(4) . . ? 
C51 C52 C53 120.6(4) . . ? 
C54 C53 C52 119.3(5) . . ? 
C55 C54 C53 121.0(5) . . ? 
C54 C55 C56 119.7(5) . . ? 
C55 C56 C51 120.6(5) . . ? 
O7 C60 O6 124.5(4) . . ? 
O7 C60 C61 125.2(4) . . ? 
O6 C60 C61 110.3(4) . . ? 
O10 C61 C60 106.6(3) . . ? 
O10 C61 C62 106.2(3) . . ? 
C60 C61 C62 119.3(4) . . ? 
O10 C61 C66 101.8(3) . . ? 
C60 C61 C66 117.0(4) . . ? 
C62 C61 C66 104.2(4) . . ? 
C61 C62 C63 101.8(4) . . ? 
C62 C63 C64 103.8(4) . . ? 
C65 C64 C69 115.3(4) . . ? 
C65 C64 C66 99.0(3) . . ? 
C69 C64 C66 119.5(4) . . ? 
C65 C64 C63 101.9(4) . . ? 
C69 C64 C63 115.9(4) . . ? 
C66 C64 C63 102.5(3) . . ? 
O9 C65 O10 120.3(4) . . ? 
O9 C65 C64 131.7(4) . . ? 
O10 C65 C64 108.0(3) . . ? 
C67 C66 C68 108.8(4) . . ? 
C67 C66 C64 114.7(4) . . ? 
C68 C66 C64 112.7(4) . . ? 
C67 C66 C61 114.4(4) . . ? 
C68 C66 C61 113.7(4) . . ? 
C64 C66 C61 91.8(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.959 
_diffrn_reflns_theta_full              25.20 
_diffrn_measured_fraction_theta_full   0.959 
_refine_diff_density_max    0.329 
_refine_diff_density_min   -0.301 
_refine_diff_density_rms    0.061