# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/2026
 
data_dw0009 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C22.50 H28 Na O1.50 Pb' 
_chemical_formula_weight          552.63 
_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' 
 'Na'  'Na'   0.0362   0.0249 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pb'  'Pb'  -3.3944  10.1111 
 '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)/n
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    9.1145(8) 
_cell_length_b                    15.798(2) 
_cell_length_c                    15.0060(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.230(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2159.1(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.700 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1072 
_exptl_absorpt_coefficient_mu     7.844 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 Very small crystal, poor data, many restraints. 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        NoniusKappaCCD
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10002 
_diffrn_reflns_av_R_equivalents   0.0530 
_diffrn_reflns_av_sigmaI/netI     0.0476 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.87 
_diffrn_reflns_theta_max          22.45 
_reflns_number_total              2798 
_reflns_number_observed           2252 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        maXus 
_computing_cell_refinement        maXus 
_computing_data_reduction         maXus 
_computing_structure_solution     SIR
_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 10 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^)+(0.0986P)^2^+37.3805P] 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_number_reflns          2788 
_refine_ls_number_parameters      60 
_refine_ls_number_restraints      22 
_refine_ls_R_factor_all           0.0838 
_refine_ls_R_factor_obs           0.0676 
_refine_ls_wR_factor_all          0.1950 
_refine_ls_wR_factor_obs          0.1786 
_refine_ls_goodness_of_fit_all    1.068 
_refine_ls_goodness_of_fit_obs    1.092 
_refine_ls_restrained_S_all       1.076 
_refine_ls_restrained_S_obs       1.096 
_refine_ls_shift/esd_max          -0.002 
_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 
Pb1 Pb 0.42196(7) 0.17761(4) 0.51148(4) 0.0542(3) Uani 1 d . . 
Na1 Na 0.9294(8) 0.1581(5) 0.6954(5) 0.070(2) Uani 1 d . . 
O1 O 0.9871(12) 0.0283(7) 0.7572(8) 0.156(5) Uiso 1 d D . 
C1 C 1.2083(12) 0.0961(7) 0.6216(8) 0.108(2) Uiso 1 d RD . 
C2 C 1.1349(12) 0.1029(7) 0.5367(8) 0.108(2) Uiso 1 d R . 
H2 H 1.1088(12) 0.0572(7) 0.4981(8) 0.129 Uiso 1 calc R . 
C3 C 1.1072(12) 0.1900(7) 0.5196(8) 0.108(2) Uiso 1 d R . 
H3 H 1.0594(12) 0.2128(7) 0.4676(8) 0.129 Uiso 1 calc R . 
C4 C 1.1635(12) 0.2370(7) 0.5940(8) 0.108(2) Uiso 1 d R . 
H4 H 1.1600(12) 0.2968(7) 0.6005(8) 0.129 Uiso 1 calc R . 
C5 C 1.2260(12) 0.1790(7) 0.6570(8) 0.108(2) Uiso 1 d R . 
H5 H 1.2717(12) 0.1931(7) 0.7130(8) 0.129 Uiso 1 calc R . 
C6 C 1.2305(29) 0.0166(15) 0.6758(18) 0.108(2) Uiso 1 d D . 
H6A H 1.2920(29) 0.0311(15) 0.7295(18) 0.129 Uiso 1 calc R . 
H6B H 1.2874(29) -0.0236(15) 0.6402(18) 0.129 Uiso 1 calc R . 
C7 C 1.0819(34) -0.0334(18) 0.7092(17) 0.156(5) Uiso 1 d D . 
H7 H 1.0262(34) -0.0589(18) 0.6571(17) 0.188 Uiso 1 calc R . 
C8 C 1.1207(37) -0.1006(18) 0.7781(20) 0.156(5) Uiso 1 d D . 
H8A H 1.0623(37) -0.1525(18) 0.7662(20) 0.188 Uiso 1 calc R . 
H8B H 1.2262(37) -0.1152(18) 0.7764(20) 0.188 Uiso 1 calc R . 
C9 C 1.0875(35) -0.0654(20) 0.8650(17) 0.156(5) Uiso 1 d D . 
H9A H 1.1704(35) -0.0313(20) 0.8900(17) 0.188 Uiso 1 calc R . 
H9B H 1.0638(35) -0.1106(20) 0.9078(17) 0.188 Uiso 1 calc R . 
C10 C 0.9512(21) -0.0091(13) 0.8418(12) 0.156(5) Uiso 1 d D . 
H10A H 0.8606(21) -0.0435(13) 0.8359(12) 0.188 Uiso 1 calc R . 
H10B H 0.9383(21) 0.0349(13) 0.8878(12) 0.188 Uiso 1 calc R . 
C11 C 0.6958(21) 0.2181(13) 0.6035(12) 0.108(2) Uiso 1 d R . 
H11 H 0.7230(21) 0.2755(13) 0.5947(12) 0.129 Uiso 1 calc R . 
C12 C 0.6169(11) 0.1860(6) 0.6751(6) 0.108(2) Uiso 1 d . . 
H12 H 0.5788(11) 0.2186(6) 0.7221(6) 0.129 Uiso 1 calc R . 
C13 C 0.6037(11) 0.0968(6) 0.6655(6) 0.108(2) Uiso 1 d R . 
H13 H 0.5573(11) 0.0596(6) 0.7053(6) 0.129 Uiso 1 calc R . 
C14 C 0.6720(11) 0.0731(6) 0.5858(6) 0.108(2) Uiso 1 d R . 
H14 H 0.6794(11) 0.0173(6) 0.5630(6) 0.129 Uiso 1 calc R . 
C15 C 0.7274(11) 0.1476(6) 0.5461(6) 0.108(2) Uiso 1 d R . 
H15 H 0.7766(11) 0.1505(6) 0.4916(6) 0.129 Uiso 1 calc R . 
C16 C 0.3259(11) 0.2144(6) 0.3328(6) 0.108(2) Uiso 1 d R . 
H16 H 0.2349(11) 0.1877(6) 0.3176(6) 0.129 Uiso 1 calc R . 
C17 C 0.3441(11) 0.2943(6) 0.3751(6) 0.108(2) Uiso 1 d R . 
H17 H 0.2674(11) 0.3305(6) 0.3931(6) 0.129 Uiso 1 calc R . 
C18 C 0.4969(11) 0.3107(6) 0.3857(6) 0.108(2) Uiso 1 d R . 
H18 H 0.5405(11) 0.3597(6) 0.4120(6) 0.129 Uiso 1 calc R . 
C19 C 0.5732(11) 0.2408(6) 0.3500(6) 0.108(2) Uiso 1 d R . 
H19 H 0.6768(11) 0.2350(6) 0.3482(6) 0.129 Uiso 1 calc R . 
C20 C 0.4675(11) 0.1813(6) 0.3173(6) 0.108(2) Uiso 1 d R . 
H20 H 0.4879(11) 0.1286(6) 0.2899(6) 0.129 Uiso 1 calc R . 
O2 O 0.9062(52) 0.4291(26) 0.5709(27) 0.161(10) Uiso 0.50 d PD -1 
C21 C 0.9467(77) 0.5076(36) 0.6170(30) 0.161(10) Uiso 0.50 d PD -1 
H21A H 0.8575(77) 0.5363(36) 0.6376(30) 0.194 Uiso 0.50 calc PR -1 
H21B H 1.0116(77) 0.4951(36) 0.6698(30) 0.194 Uiso 0.50 calc PR -1 
C22 C 1.0220(103) 0.5620(34) 0.5561(39) 0.161(10) Uiso 0.50 d PD -1 
H22A H 1.1206(103) 0.5767(34) 0.5814(39) 0.194 Uiso 0.50 calc PR -1 
H22B H 0.9658(103) 0.6151(34) 0.5461(39) 0.194 Uiso 0.50 calc PR -1 
C23 C 1.0356(90) 0.5143(33) 0.4675(34) 0.161(10) Uiso 0.50 d PD -1 
H23A H 0.9838(90) 0.5449(33) 0.4181(34) 0.194 Uiso 0.50 calc PR -1 
H23B H 1.1400(90) 0.5074(33) 0.4530(34) 0.194 Uiso 0.50 calc PR -1 
C24 C 0.9646(54) 0.4290(23) 0.4830(23) 0.161(10) Uiso 1 d D -1 
H24A H 0.8848(54) 0.4190(23) 0.4376(23) 0.194 Uiso 1 calc R -1 
H24B H 1.0382(54) 0.3833(23) 0.4782(23) 0.194 Uiso 1 calc R -1 
 
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 
Pb1 0.0437(5) 0.0724(5) 0.0465(5) -0.0016(3) 0.0019(3) -0.0021(3) 
Na1 0.055(4) 0.079(5) 0.076(5) 0.004(4) 0.001(4) 0.010(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 
Pb1 C17 2.825(9) . ? 
Pb1 C16 2.848(9) . ? 
Pb1 C15 2.852(10) . ? 
Pb1 C4 2.862(11) 1_455 ? 
Na1 O1 2.304(13) . ? 
Na1 C11 2.67(2) . ? 
Na1 C5 2.805(13) . ? 
Na1 C15 2.847(12) . ? 
Na1 C12 2.886(12) . ? 
Na1 C17 2.933(12) 4_666 ? 
Na1 C18 2.939(12) 4_666 ? 
Na1 C4 2.945(13) . ? 
Na1 C1 2.978(13) . ? 
Na1 C16 3.058(12) 4_666 ? 
Na1 C19 3.068(12) 4_666 ? 
Na1 C14 3.116(12) . ? 
O1 C10 1.45(2) . ? 
O1 C7 1.51(2) . ? 
C1 C2 1.42 . ? 
C1 C5 1.42 . ? 
C1 C6 1.51(2) . ? 
C2 C3 1.42 . ? 
C3 C4 1.42 . ? 
C4 C5 1.42 . ? 
C4 Pb1 2.862(11) 1_655 ? 
C6 C7 1.66(3) . ? 
C7 C8 1.51(3) . ? 
C8 C9 1.46(3) . ? 
C9 C10 1.56(2) . ? 
C11 C12 1.41(2) . ? 
C11 C15 1.44(2) . ? 
C12 C13 1.42 . ? 
C13 C14 1.42 . ? 
C14 C15 1.42 . ? 
C16 C20 1.42 . ? 
C16 C17 1.42 . ? 
C16 Na1 3.058(12) 4_565 ? 
C17 C18 1.42 . ? 
C17 Na1 2.933(12) 4_565 ? 
C18 C19 1.42 . ? 
C18 Na1 2.939(12) 4_565 ? 
C19 C20 1.42 . ? 
C19 Na1 3.068(12) 4_565 ? 
O2 C24 1.44(3) . ? 
O2 C21 1.46(3) . ? 
C21 C22 1.45(3) . ? 
C22 C23 1.54(3) . ? 
C23 C24 1.52(3) . ? 
 
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 
C17 Pb1 C16 28.99(9) . . ? 
C17 Pb1 C15 117.2(3) . . ? 
C16 Pb1 C15 117.9(3) . . ? 
C17 Pb1 C4 84.9(3) . 1_455 ? 
C16 Pb1 C4 96.5(3) . 1_455 ? 
C15 Pb1 C4 142.2(3) . 1_455 ? 
O1 Na1 C11 133.7(6) . . ? 
O1 Na1 C5 88.9(4) . . ? 
C11 Na1 C5 127.5(6) . . ? 
O1 Na1 C15 113.3(5) . . ? 
C11 Na1 C15 30.1(5) . . ? 
C5 Na1 C15 116.4(4) . . ? 
O1 Na1 C12 112.8(4) . . ? 
C11 Na1 C12 29.1(4) . . ? 
C5 Na1 C12 156.3(4) . . ? 
C15 Na1 C12 47.2(2) . . ? 
O1 Na1 C17 85.5(4) . 4_666 ? 
C11 Na1 C17 98.6(5) . 4_666 ? 
C5 Na1 C17 116.8(4) . 4_666 ? 
C15 Na1 C17 123.5(4) . 4_666 ? 
C12 Na1 C17 76.2(3) . 4_666 ? 
O1 Na1 C18 73.8(4) . 4_666 ? 
C11 Na1 C18 125.2(5) . 4_666 ? 
C5 Na1 C18 90.7(4) . 4_666 ? 
C15 Na1 C18 151.4(5) . 4_666 ? 
C12 Na1 C18 104.2(4) . 4_666 ? 
C17 Na1 C18 27.98(11) 4_666 4_666 ? 
O1 Na1 C4 115.2(5) . . ? 
C11 Na1 C4 99.4(5) . . ? 
C5 Na1 C4 28.46(13) . . ? 
C15 Na1 C4 94.5(4) . . ? 
C12 Na1 C4 127.8(4) . . ? 
C17 Na1 C4 126.1(4) 4_666 . ? 
C18 Na1 C4 107.6(4) 4_666 . ? 
O1 Na1 C1 70.8(3) . . ? 
C11 Na1 C1 127.0(5) . . ? 
C5 Na1 C1 28.22(12) . . ? 
C15 Na1 C1 102.9(4) . . ? 
C12 Na1 C1 149.8(4) . . ? 
C17 Na1 C1 133.4(4) 4_666 . ? 
C18 Na1 C1 105.5(4) 4_666 . ? 
C4 Na1 C1 45.6(2) . . ? 
O1 Na1 C16 112.7(4) . 4_666 ? 
C11 Na1 C16 81.6(5) . 4_666 ? 
C5 Na1 C16 112.7(4) . 4_666 ? 
C15 Na1 C16 111.2(4) . 4_666 ? 
C12 Na1 C16 69.0(3) . 4_666 ? 
C17 Na1 C16 27.32(11) 4_666 4_666 ? 
C18 Na1 C16 45.0(2) 4_666 4_666 ? 
C4 Na1 C16 108.6(4) . 4_666 ? 
C1 Na1 C16 139.3(4) . 4_666 ? 
O1 Na1 C19 94.3(4) . 4_666 ? 
C11 Na1 C19 121.0(5) . 4_666 ? 
C5 Na1 C19 73.0(4) . 4_666 ? 
C15 Na1 C19 150.4(3) . 4_666 ? 
C12 Na1 C19 113.0(3) . 4_666 ? 
C17 Na1 C19 45.0(2) 4_666 4_666 ? 
C18 Na1 C19 27.24(11) 4_666 4_666 ? 
C4 Na1 C19 82.7(4) . 4_666 ? 
C1 Na1 C19 96.1(4) . 4_666 ? 
C16 Na1 C19 44.1(2) 4_666 4_666 ? 
O1 Na1 C14 89.1(4) . . ? 
C11 Na1 C14 46.4(5) . . ? 
C5 Na1 C14 130.8(4) . . ? 
C15 Na1 C14 27.07(11) . . ? 
C12 Na1 C14 44.8(2) . . ? 
C17 Na1 C14 112.0(4) 4_666 . ? 
C18 Na1 C14 135.2(4) 4_666 . ? 
C4 Na1 C14 117.1(4) . . ? 
C1 Na1 C14 107.3(4) . . ? 
C16 Na1 C14 113.2(4) 4_666 . ? 
C19 Na1 C14 156.1(4) 4_666 . ? 
C10 O1 C7 108.0(12) . . ? 
C10 O1 Na1 131.3(10) . . ? 
C7 O1 Na1 120.7(11) . . ? 
C2 C1 C5 108.0 . . ? 
C2 C1 C6 126.6(12) . . ? 
C5 C1 C6 123.8(12) . . ? 
C2 C1 Na1 85.9(3) . . ? 
C5 C1 Na1 69.1(3) . . ? 
C6 C1 Na1 99.9(11) . . ? 
C1 C2 C3 108.0 . . ? 
C4 C3 C2 108.0 . . ? 
C5 C4 C3 108.0 . . ? 
C5 C4 Pb1 76.2(2) . 1_655 ? 
C3 C4 Pb1 76.5(2) . 1_655 ? 
C5 C4 Na1 70.3(3) . . ? 
C3 C4 Na1 86.4(3) . . ? 
Pb1 C4 Na1 135.2(4) 1_655 . ? 
C4 C5 C1 108.0 . . ? 
C4 C5 Na1 81.2(3) . . ? 
C1 C5 Na1 82.7(3) . . ? 
C1 C6 C7 117.8(19) . . ? 
O1 C7 C8 104.5(13) . . ? 
O1 C7 C6 109.0(21) . . ? 
C8 C7 C6 111.6(25) . . ? 
C9 C8 C7 107.0(16) . . ? 
C8 C9 C10 102.1(15) . . ? 
O1 C10 C9 102.9(13) . . ? 
C12 C11 C15 107.2(15) . . ? 
C12 C11 Na1 84.2(9) . . ? 
C15 C11 Na1 81.9(9) . . ? 
C11 C12 C13 108.9(9) . . ? 
C11 C12 Na1 66.7(9) . . ? 
C13 C12 Na1 86.5(2) . . ? 
C14 C13 C12 108.0 . . ? 
C13 C14 C15 108.0 . . ? 
C13 C14 Na1 77.7(2) . . ? 
C15 C14 Na1 65.9(2) . . ? 
C14 C15 C11 107.9(8) . . ? 
C14 C15 Na1 87.0(2) . . ? 
C11 C15 Na1 67.9(9) . . ? 
C14 C15 Pb1 81.6(2) . . ? 
C11 C15 Pb1 76.4(9) . . ? 
Na1 C15 Pb1 136.9(4) . . ? 
C20 C16 C17 108.0 . . ? 
C20 C16 Pb1 80.3(2) . . ? 
C17 C16 Pb1 74.6(2) . . ? 
C20 C16 Na1 79.9(2) . 4_565 ? 
C17 C16 Na1 71.4(2) . 4_565 ? 
Pb1 C16 Na1 132.7(4) . 4_565 ? 
C16 C17 C18 108.0 . . ? 
C16 C17 Pb1 76.4(2) . . ? 
C18 C17 Pb1 79.6(2) . . ? 
C16 C17 Na1 81.3(2) . 4_565 ? 
C18 C17 Na1 76.2(2) . 4_565 ? 
Pb1 C17 Na1 139.9(4) . 4_565 ? 
C19 C18 C17 108.0 . . ? 
C19 C18 Na1 81.4(2) . 4_565 ? 
C17 C18 Na1 75.8(2) . 4_565 ? 
C18 C19 C20 108.0 . . ? 
C18 C19 Na1 71.3(2) . 4_565 ? 
C20 C19 Na1 79.6(2) . 4_565 ? 
C16 C20 C19 108.0 . . ? 
C24 O2 C21 109.8(16) . . ? 
C22 C21 O2 108.8(16) . . ? 
C21 C22 C23 108.1(16) . . ? 
C24 C23 C22 104.7(14) . . ? 
O2 C24 C23 108.3(15) . . ? 
 
_refine_diff_density_max    1.661 
_refine_diff_density_min   -1.224 
_refine_diff_density_rms    0.219