Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vivian Yam' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong CHINA ; _publ_contact_author_email WWYAM@HKU.HK _publ_section_title ; Synthesis, Luminescence and Ion-Binding Properties of Palladium(II) Complexes with 1,2-Bis[di(benzo-15-crown-5)phosphino]ethane (dbcpe). X-Ray Crystal Structure of dbcpe ; loop_ _publ_author_name 'Vivian Yam' 'Eddie Chung-Chin Cheng' 'Xiao-Xia Lu.' 'Nianyong Zhu.' # Attachment 'Yam-CCDC253656.cif' data_mar294 _database_code_depnum_ccdc_archive 'CCDC 253656' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H80 O20 P2' _chemical_formula_sum 'C58 H80 O20 P2' _chemical_formula_weight 1159.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.426(4) _cell_length_b 5.2270(10) _cell_length_c 27.398(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.48(3) _cell_angle_gamma 90.00 _cell_volume 2970.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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_type 'marresearch IPDS mar300' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9076 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.85 _reflns_number_total 2851 _reflns_number_gt 1779 _reflns_threshold_expression >2sigma(I) _computing_data_collection Marcontrol _computing_cell_refinement Scalepack _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1648P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2851 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2309 _refine_ls_wR_factor_gt 0.2090 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.43425(7) 0.2820(2) 0.45188(5) 0.0652(6) Uani 1 1 d . . . O1 O 0.21093(19) -0.2102(8) 0.41530(17) 0.0986(13) Uani 1 1 d . B . O2 O 0.1348(3) -0.3116(15) 0.4846(3) 0.190(3) Uani 1 1 d . . . O3 O -0.0065(7) -0.123(2) 0.4168(6) 0.275(5) Uiso 1 1 d . . . O4 O 0.0347(4) 0.240(2) 0.3399(5) 0.249(5) Uani 1 1 d . . . O5 O 0.1615(2) 0.0843(10) 0.34064(19) 0.1289(17) Uani 1 1 d . . . O6 O 0.61652(18) 0.5816(7) 0.36994(14) 0.0805(11) Uani 1 1 d . . . O7 O 0.7472(3) 0.6601(14) 0.4088(2) 0.158(2) Uani 1 1 d . . . O8 O 0.8014(7) 0.331(3) 0.3396(5) 0.161(4) Uiso 0.50 1 d P A 1 O9 O 0.7002(5) 0.0813(14) 0.2660(3) 0.073(2) Uiso 0.50 1 d P A 1 O8' O 0.8114(7) 0.525(3) 0.3241(6) 0.155(5) Uiso 0.50 1 d P A 2 O9' O 0.6638(15) 0.207(5) 0.2333(11) 0.250(11) Uiso 0.50 1 d P A 2 O10 O 0.5898(2) 0.2508(7) 0.29809(15) 0.0912(12) Uani 1 1 d . . . C1 C 0.4629(2) -0.0093(9) 0.48779(19) 0.0668(14) Uani 1 1 d . . . H1A H 0.4401 -0.0319 0.5140 0.080 Uiso 1 1 calc R . . H1B H 0.4540 -0.1566 0.4656 0.080 Uiso 1 1 calc R . . C2 C 0.3530(3) 0.1980(10) 0.4169(2) 0.0677(15) Uani 1 1 d . . . C3 C 0.3160(3) 0.0050(10) 0.4300(2) 0.0693(15) Uani 1 1 d . . . H3 H 0.3346 -0.1043 0.4564 0.083 Uiso 1 1 calc R . . C4 C 0.2524(3) -0.0292(11) 0.4047(2) 0.0780(16) Uani 1 1 d . . . C5 C 0.2252(3) 0.1318(14) 0.3642(3) 0.0883(18) Uani 1 1 d . . . C6 C 0.2608(4) 0.3164(13) 0.3508(2) 0.098(2) Uani 1 1 d . . . H6 H 0.2426 0.4204 0.3234 0.117 Uiso 1 1 calc R . . C7 C 0.3241(3) 0.3558(11) 0.3770(2) 0.0860(17) Uani 1 1 d . . . H7 H 0.3475 0.4891 0.3677 0.103 Uiso 1 1 calc R . . C8 C 0.4786(3) 0.2630(9) 0.40251(19) 0.0630(14) Uani 1 1 d . . . C9 C 0.5288(2) 0.4325(9) 0.40463(19) 0.0637(14) Uani 1 1 d . . . H9 H 0.5380 0.5547 0.4301 0.076 Uiso 1 1 calc R . . C10 C 0.5656(3) 0.4245(10) 0.3698(2) 0.0648(14) Uani 1 1 d . . . C11 C 0.5513(3) 0.2434(11) 0.3314(2) 0.0728(16) Uani 1 1 d . . . C12 C 0.5013(3) 0.0770(11) 0.3282(2) 0.0815(17) Uani 1 1 d . . . H12 H 0.4913 -0.0421 0.3021 0.098 Uiso 1 1 calc R . . C13 C 0.4654(3) 0.0862(10) 0.3637(2) 0.0784(16) Uani 1 1 d . . . H13 H 0.4317 -0.0290 0.3614 0.094 Uiso 1 1 calc R . . C14 C 0.2308(3) -0.3562(11) 0.4611(3) 0.0952(19) Uani 1 1 d . . . H14A H 0.2476 -0.2436 0.4894 0.114 Uiso 1 1 calc R B . H14B H 0.2643 -0.4768 0.4586 0.114 Uiso 1 1 calc R . . C15 C 0.1730(4) -0.4950(15) 0.4680(3) 0.123(2) Uani 1 1 d . B . H15A H 0.1493 -0.5709 0.4365 0.147 Uiso 1 1 calc R . . H15B H 0.1855 -0.6298 0.4929 0.147 Uiso 1 1 calc R . . C16 C 0.083(2) -0.313(8) 0.4875(17) 0.249(17) Uiso 0.50 1 d P B 1 H16A H 0.0857 -0.3294 0.5233 0.298 Uiso 0.50 1 calc PR B 1 H16B H 0.0653 -0.4734 0.4724 0.298 Uiso 0.50 1 calc PR B 1 C17 C 0.034(2) -0.134(7) 0.4702(16) 0.303(17) Uiso 0.50 1 d P B 1 H17A H 0.0537 0.0329 0.4775 0.364 Uiso 0.50 1 calc PR B 1 H17B H 0.0042 -0.1526 0.4915 0.364 Uiso 0.50 1 calc PR B 1 C18 C -0.0348(10) 0.128(4) 0.3944(8) 0.169(7) Uiso 0.50 1 d P B 1 H18A H -0.0801 0.1371 0.3939 0.203 Uiso 0.50 1 calc PR B 1 H18B H -0.0126 0.2698 0.4142 0.203 Uiso 0.50 1 calc PR B 1 C16' C 0.0665(17) -0.336(6) 0.4594(14) 0.219(14) Uiso 0.50 1 d P B 2 H16C H 0.0578 -0.4904 0.4390 0.263 Uiso 0.50 1 calc PR B 2 H16D H 0.0397 -0.3339 0.4831 0.263 Uiso 0.50 1 calc PR B 2 C17' C 0.0593(13) -0.136(5) 0.4324(11) 0.208(10) Uiso 0.50 1 d P B 2 H17C H 0.0787 -0.1542 0.4041 0.250 Uiso 0.50 1 calc PR B 2 H17D H 0.0772 0.0135 0.4519 0.250 Uiso 0.50 1 calc PR B 2 C18' C -0.0229(17) -0.048(8) 0.3743(15) 0.270(16) Uiso 0.50 1 d P B 2 H18C H -0.0680 -0.0968 0.3664 0.323 Uiso 0.50 1 calc PR B 2 H18D H -0.0030 -0.1778 0.3579 0.323 Uiso 0.50 1 calc PR B 2 C19 C -0.0263(9) 0.141(3) 0.3414(6) 0.259(6) Uiso 1 1 d . . . H19C H -0.0521 0.2783 0.3501 0.311 Uiso 0.50 1 calc PR B 2 H19D H -0.0481 0.0796 0.3081 0.311 Uiso 0.50 1 calc PR B 2 H19A H -0.0360 -0.0153 0.3220 0.311 Uiso 0.50 1 d PR B 1 H19B H -0.0569 0.2704 0.3251 0.311 Uiso 0.50 1 d PR B 1 C20 C 0.0559(7) 0.197(3) 0.2987(5) 0.221(6) Uani 1 1 d . . . H20A H 0.0310 0.2984 0.2709 0.265 Uiso 1 1 calc R B . H20B H 0.0503 0.0183 0.2894 0.265 Uiso 1 1 calc R . . C21 C 0.1261(4) 0.2683(19) 0.3085(4) 0.172(4) Uani 1 1 d . B . H21A H 0.1392 0.2728 0.2771 0.207 Uiso 1 1 calc R . . H21B H 0.1334 0.4360 0.3241 0.207 Uiso 1 1 calc R . . C22 C 0.6410(3) 0.7363(11) 0.4131(2) 0.0914(19) Uani 1 1 d . . . H22A H 0.6496 0.6335 0.4436 0.110 Uiso 1 1 calc R . . H22B H 0.6104 0.8694 0.4157 0.110 Uiso 1 1 calc R . . C23 C 0.7022(4) 0.8511(15) 0.4060(3) 0.126(3) Uani 1 1 d . . . H23A H 0.6941 0.9350 0.3734 0.152 Uiso 1 1 calc R . . H23B H 0.7183 0.9780 0.4319 0.152 Uiso 1 1 calc R . . C24 C 0.8041(5) 0.735(3) 0.3965(5) 0.209(6) Uani 1 1 d . A . H24A H 0.7967 0.9043 0.3816 0.251 Uiso 1 1 calc R . . H24B H 0.8370 0.7527 0.4278 0.251 Uiso 1 1 calc R . . C25 C 0.8278(7) 0.597(3) 0.3669(9) 0.318(12) Uani 1 1 d . . . H25C H 0.8690 0.6776 0.3686 0.381 Uiso 0.50 1 calc PR A 2 H25D H 0.8382 0.4382 0.3856 0.381 Uiso 0.50 1 calc PR A 2 H25A H 0.8722 0.5615 0.3842 0.381 Uiso 0.50 1 d PR A 1 H25B H 0.8295 0.7128 0.3397 0.381 Uiso 0.50 1 d PR A 1 C26 C 0.7887(13) 0.368(5) 0.2897(10) 0.184(8) Uiso 0.50 1 d P A 1 H26A H 0.8132 0.2426 0.2760 0.221 Uiso 0.50 1 calc PR A 1 H26B H 0.8048 0.5353 0.2839 0.221 Uiso 0.50 1 calc PR A 1 C27 C 0.7241(15) 0.352(6) 0.2622(14) 0.199(13) Uiso 0.50 1 d P A 1 H27A H 0.7205 0.3948 0.2272 0.238 Uiso 0.50 1 calc PR A 1 H27B H 0.6981 0.4715 0.2757 0.238 Uiso 0.50 1 calc PR A 1 C26' C 0.7440(18) 0.411(6) 0.3060(15) 0.258(14) Uiso 0.50 1 d P A 2 H26C H 0.7334 0.3343 0.3351 0.309 Uiso 0.50 1 calc PR A 2 H26D H 0.7145 0.5533 0.2956 0.309 Uiso 0.50 1 calc PR A 2 C27' C 0.7299(19) 0.231(9) 0.2673(14) 0.228(16) Uiso 0.50 1 d P A 2 H27C H 0.7413 0.0651 0.2828 0.274 Uiso 0.50 1 calc PR A 2 H27D H 0.7591 0.2632 0.2460 0.274 Uiso 0.50 1 calc PR A 2 C28 C 0.6386(5) 0.066(2) 0.2387(4) 0.156(4) Uani 1 1 d . . . H28C H 0.6702 -0.0646 0.2529 0.187 Uiso 0.50 1 calc PR A 2 H28D H 0.6179 0.0065 0.2050 0.187 Uiso 0.50 1 calc PR A 2 H28A H 0.6353 -0.0788 0.2160 0.187 Uiso 0.50 1 d PR A 1 H28B H 0.6289 0.2184 0.2181 0.187 Uiso 0.50 1 d PR A 1 C29 C 0.5888(3) 0.0360(13) 0.2666(2) 0.0960(19) Uani 1 1 d . A . H29A H 0.5468 0.0211 0.2431 0.115 Uiso 1 1 calc R . . H29B H 0.5968 -0.1185 0.2868 0.115 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 0.0667(11) 0.0622(10) 0.0729(11) -0.0028(7) 0.0287(8) -0.0010(7) O1 0.069(3) 0.104(3) 0.118(4) 0.017(3) 0.015(3) -0.013(2) O2 0.101(5) 0.259(8) 0.236(8) 0.002(6) 0.091(6) 0.006(5) O4 0.120(7) 0.308(10) 0.333(15) 0.026(10) 0.084(8) 0.018(6) O5 0.081(4) 0.172(4) 0.122(4) 0.044(3) 0.004(3) -0.005(3) O6 0.081(3) 0.090(3) 0.078(3) -0.007(2) 0.034(2) -0.017(2) O7 0.080(4) 0.237(7) 0.159(5) 0.019(5) 0.034(4) -0.024(4) O10 0.104(3) 0.103(3) 0.080(3) -0.014(2) 0.046(3) -0.009(2) C1 0.065(3) 0.070(3) 0.066(4) 0.003(3) 0.019(3) -0.003(3) C2 0.071(4) 0.065(3) 0.073(4) 0.002(3) 0.030(3) 0.003(3) C3 0.057(4) 0.068(3) 0.082(4) 0.006(3) 0.016(3) 0.005(3) C4 0.069(5) 0.079(4) 0.090(5) 0.009(3) 0.027(4) 0.003(4) C5 0.051(4) 0.126(5) 0.085(5) 0.011(4) 0.010(4) 0.000(4) C6 0.078(5) 0.131(5) 0.084(5) 0.031(4) 0.021(4) 0.013(4) C7 0.067(5) 0.105(4) 0.091(5) 0.022(4) 0.029(4) -0.001(3) C8 0.070(4) 0.057(3) 0.063(4) 0.002(3) 0.020(3) -0.002(3) C9 0.068(4) 0.059(3) 0.065(4) 0.001(3) 0.019(3) -0.003(3) C10 0.069(4) 0.062(4) 0.069(4) 0.003(3) 0.028(3) -0.007(3) C11 0.074(4) 0.087(4) 0.064(4) 0.004(3) 0.028(3) 0.005(3) C12 0.087(4) 0.086(4) 0.076(4) -0.018(3) 0.030(4) -0.011(4) C13 0.079(4) 0.073(4) 0.091(4) -0.013(3) 0.035(4) -0.014(3) C14 0.088(5) 0.094(4) 0.105(5) 0.013(4) 0.025(4) -0.008(4) C15 0.103(6) 0.128(6) 0.146(7) 0.023(5) 0.048(5) -0.024(5) C20 0.128(13) 0.297(15) 0.204(14) 0.060(12) -0.024(10) 0.029(10) C21 0.088(7) 0.236(10) 0.172(9) 0.075(8) -0.007(6) 0.010(6) C22 0.088(5) 0.102(4) 0.086(5) -0.005(4) 0.025(4) -0.026(4) C23 0.115(7) 0.151(7) 0.119(6) -0.012(5) 0.040(5) -0.056(6) C24 0.121(9) 0.355(19) 0.168(10) -0.016(11) 0.069(8) -0.045(10) C25 0.220(15) 0.34(2) 0.46(3) -0.22(2) 0.214(19) -0.134(15) C28 0.167(11) 0.197(10) 0.126(7) -0.046(7) 0.081(8) -0.021(8) C29 0.105(5) 0.121(5) 0.075(4) -0.016(4) 0.046(4) 0.005(4) _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 C2 1.819(6) . ? P1 C1 1.833(5) . ? P1 C8 1.839(5) . ? O1 C4 1.377(7) . ? O1 C14 1.438(7) . ? O2 C16 1.14(4) . ? O2 C15 1.407(9) . ? O2 C16' 1.46(3) . ? O3 C18' 1.20(4) . ? O3 C17' 1.37(2) . ? O3 C17 1.50(4) . ? O3 C18 1.51(2) . ? O4 C20 1.337(15) . ? O4 C19 1.415(17) . ? O5 C5 1.378(7) . ? O5 C21 1.393(9) . ? O6 C10 1.365(6) . ? O6 C22 1.421(6) . ? O7 C23 1.377(9) . ? O7 C24 1.399(11) . ? O8 C26 1.34(2) . ? O8 C25 1.610(18) . ? O9 C28 1.346(12) . ? O9 C27 1.51(3) . ? O8' C25 1.20(2) . ? O8' C26' 1.52(4) . ? O9' C28 0.95(2) . ? O9' C27' 1.49(4) . ? O10 C11 1.373(6) . ? O10 C29 1.414(6) . ? C1 C1 1.568(9) 3_656 ? C2 C3 1.384(7) . ? C2 C7 1.386(7) . ? C3 C4 1.377(7) . ? C4 C5 1.399(8) . ? C5 C6 1.337(8) . ? C6 C7 1.382(8) . ? C8 C13 1.384(7) . ? C8 C9 1.384(6) . ? C9 C10 1.382(7) . ? C10 C11 1.391(7) . ? C11 C12 1.367(7) . ? C12 C13 1.383(7) . ? C14 C15 1.489(8) . ? C16 C17 1.39(5) . ? C18 C19 1.51(2) . ? C16' C17' 1.27(3) . ? C18' C19 1.33(4) . ? C20 C21 1.506(15) . ? C22 C23 1.498(9) . ? C24 C25 1.282(15) . ? C26 C27 1.40(4) . ? C26' C27' 1.39(5) . ? C28 C29 1.467(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C1 103.3(2) . . ? C2 P1 C8 101.6(2) . . ? C1 P1 C8 100.7(2) . . ? C4 O1 C14 118.8(5) . . ? C16 O2 C15 133(2) . . ? C16 O2 C16' 32(3) . . ? C15 O2 C16' 112.4(16) . . ? C18' O3 C17' 110(3) . . ? C18' O3 C17 157(3) . . ? C17' O3 C17 52.9(16) . . ? C18' O3 C18 47.7(19) . . ? C17' O3 C18 116.4(17) . . ? C17 O3 C18 120.2(19) . . ? C20 O4 C19 118.4(15) . . ? C5 O5 C21 119.4(6) . . ? C10 O6 C22 118.3(4) . . ? C23 O7 C24 115.1(8) . . ? C26 O8 C25 108.0(17) . . ? C28 O9 C27 108.7(14) . . ? C25 O8' C26' 118(2) . . ? C28 O9' C27' 117(3) . . ? C11 O10 C29 117.7(4) . . ? C1 C1 P1 110.2(4) 3_656 . ? C3 C2 C7 117.8(5) . . ? C3 C2 P1 125.0(4) . . ? C7 C2 P1 116.9(4) . . ? C4 C3 C2 121.6(5) . . ? O1 C4 C3 126.4(6) . . ? O1 C4 C5 114.6(6) . . ? C3 C4 C5 118.9(5) . . ? C6 C5 O5 124.6(7) . . ? C6 C5 C4 119.9(6) . . ? O5 C5 C4 115.5(6) . . ? C5 C6 C7 121.3(6) . . ? C6 C7 C2 120.5(5) . . ? C13 C8 C9 117.8(5) . . ? C13 C8 P1 123.9(4) . . ? C9 C8 P1 118.2(4) . . ? C10 C9 C8 121.5(5) . . ? O6 C10 C9 124.9(5) . . ? O6 C10 C11 115.8(5) . . ? C9 C10 C11 119.2(5) . . ? C12 C11 O10 124.5(5) . . ? C12 C11 C10 120.1(5) . . ? O10 C11 C10 115.4(5) . . ? C11 C12 C13 119.8(5) . . ? C12 C13 C8 121.5(5) . . ? O1 C14 C15 107.2(5) . . ? O2 C15 C14 106.2(7) . . ? O2 C16 C17 130(4) . . ? C16 C17 O3 124(3) . . ? C19 C18 O3 107.4(17) . . ? C17' C16' O2 99(3) . . ? C16' C17' O3 101(3) . . ? O3 C18' C19 149(3) . . ? C18' C19 O4 113(2) . . ? C18' C19 C18 46.6(16) . . ? O4 C19 C18 112.3(16) . . ? O4 C20 C21 110.0(13) . . ? O5 C21 C20 107.8(8) . . ? O6 C22 C23 105.8(5) . . ? O7 C23 C22 109.0(6) . . ? C25 C24 O7 120.1(13) . . ? O8' C25 C24 137(2) . . ? O8' C25 O8 45.0(8) . . ? C24 C25 O8 129.1(13) . . ? O8 C26 C27 117(2) . . ? C26 C27 O9 109(2) . . ? C27' C26' O8' 121(3) . . ? C26' C27' O9' 122(3) . . ? O9' C28 O9 61(2) . . ? O9' C28 C29 133(2) . . ? O9 C28 C29 117.1(9) . . ? O10 C29 C28 109.5(6) . . ? _diffrn_measured_fraction_theta_max 0.625 _diffrn_reflns_theta_full 23.85 _diffrn_measured_fraction_theta_full 0.625 _refine_diff_density_max 0.368 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.052