Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name G.Bertrand J.-B.Bourg D.Bourissou G.Fuks A.Rodriguez F.S.Tham _publ_contact_author_name 'Guy Bertrand' _publ_contact_author_email GBERTRAN@UCR.EDU #===END data_gb101m _database_code_depnum_ccdc_archive 'CCDC 669745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H82 B4 P4' _chemical_formula_weight 730.18 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' B B 0.0013 0.0007 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6416(14) _cell_length_b 9.9192(15) _cell_length_c 15.161(2) _cell_angle_alpha 99.409(2) _cell_angle_beta 99.848(2) _cell_angle_gamma 117.657(2) _cell_volume 1215.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6635 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.33 _exptl_crystal_description 'Frag. of prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9583 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9909 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4917 _reflns_number_gt 4296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0663P)^2^+0.2974P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4917 _refine_ls_number_parameters 288 _refine_ls_number_restraints 178 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _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 B1 B 1.11149(18) 0.87044(18) 0.26531(11) 0.0327(3) Uani 1 1 d . A . B2 B 0.98492(18) 0.67133(18) 0.17782(10) 0.0320(3) Uani 1 1 d . A . P1 P 1.06336(5) 0.68382(4) 0.30265(2) 0.03535(12) Uani 1 1 d D . . P2 P 0.89644(4) 0.80357(5) 0.19549(3) 0.04054(13) Uani 1 1 d D . . C1 C 1.27531(18) 1.04214(17) 0.29837(11) 0.0421(3) Uani 1 1 d . . . C2 C 1.2935(2) 1.1263(2) 0.22125(15) 0.0649(5) Uani 1 1 d . A . H2A H 1.2009 1.1412 0.2042 0.097 Uiso 1 1 calc R . . H2B H 1.2976 1.0624 0.1672 0.097 Uiso 1 1 calc R . . H2C H 1.3934 1.2286 0.2435 0.097 Uiso 1 1 calc R . . C3 C 1.2707(3) 1.1468(2) 0.38223(15) 0.0782(7) Uani 1 1 d . A . H3A H 1.3684 1.2506 0.4011 0.117 Uiso 1 1 calc R . . H3B H 1.2654 1.0989 0.4334 0.117 Uiso 1 1 calc R . . H3C H 1.1752 1.1574 0.3655 0.117 Uiso 1 1 calc R . . C4 C 1.4282(2) 1.0291(2) 0.3242(2) 0.0779(7) Uani 1 1 d . A . H4A H 1.5244 1.1340 0.3432 0.117 Uiso 1 1 calc R . . H4B H 1.4323 0.9640 0.2707 0.117 Uiso 1 1 calc R . . H4C H 1.4247 0.9810 0.3752 0.117 Uiso 1 1 calc R . . C5 C 1.2230(2) 0.62919(19) 0.31120(11) 0.0452(4) Uani 1 1 d . A . H5 H 1.2937 0.6853 0.2738 0.054 Uiso 1 1 calc R . . C6 C 1.1478(3) 0.4519(2) 0.26583(15) 0.0668(5) Uani 1 1 d . . . H6A H 1.2339 0.4266 0.2675 0.100 Uiso 1 1 calc R A . H6B H 1.0864 0.4250 0.2016 0.100 Uiso 1 1 calc R . . H6C H 1.0755 0.3917 0.2996 0.100 Uiso 1 1 calc R . . C7 C 1.3353(3) 0.6780(3) 0.40948(15) 0.0748(6) Uani 1 1 d . . . H7A H 1.2745 0.6135 0.4461 0.112 Uiso 1 1 calc R A . H7B H 1.3756 0.7888 0.4390 0.112 Uiso 1 1 calc R . . H7C H 1.4266 0.6628 0.4055 0.112 Uiso 1 1 calc R . . C8 C 0.9616(5) 0.5974(4) 0.3910(2) 0.0521(10) Uani 0.759(7) 1 d PDU A 1 H8A H 1.0244 0.5549 0.4228 0.063 Uiso 0.759(7) 1 calc PR A 1 C9 C 0.9692(10) 0.7283(8) 0.4651(3) 0.079(2) Uani 0.759(7) 1 d PDU A 1 H9A H 0.9104 0.6819 0.5081 0.119 Uiso 0.759(7) 1 calc PR A 1 H9B H 0.9198 0.7808 0.4350 0.119 Uiso 0.759(7) 1 calc PR A 1 H9C H 1.0822 0.8049 0.4990 0.119 Uiso 0.759(7) 1 calc PR A 1 C10 C 0.7869(5) 0.4598(6) 0.3447(4) 0.0880(19) Uani 0.759(7) 1 d PDU A 1 H10A H 0.7334 0.4269 0.3923 0.132 Uiso 0.759(7) 1 calc PR A 1 H10B H 0.7893 0.3716 0.3079 0.132 Uiso 0.759(7) 1 calc PR A 1 H10C H 0.7272 0.4936 0.3046 0.132 Uiso 0.759(7) 1 calc PR A 1 C8D C 0.9212(14) 0.6178(14) 0.3772(7) 0.056(3) Uani 0.241(7) 1 d PDU A 2 H8DA H 0.8319 0.6375 0.3539 0.068 Uiso 0.241(7) 1 calc PR A 2 C9D C 1.004(3) 0.718(2) 0.4784(9) 0.079(7) Uani 0.241(7) 1 d PDU A 2 H9DA H 0.9275 0.6805 0.5150 0.118 Uiso 0.241(7) 1 calc PR A 2 H9DB H 1.0388 0.8278 0.4818 0.118 Uiso 0.241(7) 1 calc PR A 2 H9DC H 1.0981 0.7089 0.5029 0.118 Uiso 0.241(7) 1 calc PR A 2 C10D C 0.8418(17) 0.4401(14) 0.3657(11) 0.078(5) Uani 0.241(7) 1 d PDU A 2 H10D H 0.7652 0.4098 0.4027 0.117 Uiso 0.241(7) 1 calc PR A 2 H10E H 0.9253 0.4146 0.3865 0.117 Uiso 0.241(7) 1 calc PR A 2 H10F H 0.7843 0.3830 0.3006 0.117 Uiso 0.241(7) 1 calc PR A 2 C11 C 0.8821(2) 0.8777(2) 0.09184(13) 0.0549(4) Uani 1 1 d . A . H11 H 0.9893 0.9157 0.0790 0.066 Uiso 1 1 calc R . . C12 C 0.7560(3) 0.7442(3) 0.00473(14) 0.0676(5) Uani 1 1 d . . . H12A H 0.6478 0.7026 0.0135 0.101 Uiso 1 1 calc R A . H12B H 0.7815 0.6602 -0.0053 0.101 Uiso 1 1 calc R . . H12C H 0.7589 0.7857 -0.0490 0.101 Uiso 1 1 calc R . . C13 C 0.8548(3) 1.0196(3) 0.10487(19) 0.0892(8) Uani 1 1 d . . . H13A H 0.8731 1.0649 0.0530 0.134 Uiso 1 1 calc R A . H13B H 0.9305 1.0990 0.1626 0.134 Uiso 1 1 calc R . . H13C H 0.7438 0.9845 0.1072 0.134 Uiso 1 1 calc R . . C14 C 0.7249(4) 0.7677(6) 0.2482(4) 0.0647(15) Uani 0.759(7) 1 d PDU A 1 H14A H 0.7297 0.7052 0.2920 0.078 Uiso 0.759(7) 1 calc PR A 1 C15 C 0.7517(9) 0.9225(9) 0.3074(6) 0.107(4) Uani 0.759(7) 1 d PDU A 1 H15A H 0.6719 0.8991 0.3423 0.161 Uiso 0.759(7) 1 calc PR A 1 H15B H 0.7395 0.9853 0.2672 0.161 Uiso 0.759(7) 1 calc PR A 1 H15C H 0.8607 0.9813 0.3503 0.161 Uiso 0.759(7) 1 calc PR A 1 C16 C 0.5567(4) 0.6665(7) 0.1778(4) 0.0946(18) Uani 0.759(7) 1 d PDU A 1 H16A H 0.4733 0.6422 0.2102 0.142 Uiso 0.759(7) 1 calc PR A 1 H16B H 0.5461 0.5688 0.1440 0.142 Uiso 0.759(7) 1 calc PR A 1 H16C H 0.5435 0.7242 0.1342 0.142 Uiso 0.759(7) 1 calc PR A 1 C14D C 0.7055(11) 0.7832(15) 0.2212(9) 0.056(4) Uani 0.241(7) 1 d PDU A 2 H14B H 0.6608 0.8252 0.1763 0.067 Uiso 0.241(7) 1 calc PR A 2 C15D C 0.741(2) 0.886(2) 0.3183(15) 0.069(4) Uani 0.241(7) 1 d PDU A 2 H15D H 0.8026 0.9969 0.3203 0.103 Uiso 0.241(7) 1 calc PR A 2 H15E H 0.8048 0.8632 0.3640 0.103 Uiso 0.241(7) 1 calc PR A 2 H15F H 0.6394 0.8629 0.3322 0.103 Uiso 0.241(7) 1 calc PR A 2 C16D C 0.5751(11) 0.6100(15) 0.2032(13) 0.088(5) Uani 0.241(7) 1 d PDU A 2 H16D H 0.4871 0.6045 0.2282 0.132 Uiso 0.241(7) 1 calc PR A 2 H16E H 0.6229 0.5562 0.2333 0.132 Uiso 0.241(7) 1 calc PR A 2 H16F H 0.5326 0.5592 0.1366 0.132 Uiso 0.241(7) 1 calc PR A 2 C17 C 0.98886(16) 0.57673(15) 0.08468(9) 0.0301(3) Uani 1 1 d . . . C18 C 0.86576(16) 0.42078(16) 0.03427(9) 0.0319(3) Uani 1 1 d . . . C19 C 1.12018(16) 0.65089(15) 0.04821(9) 0.0321(3) Uani 1 1 d . . . H19 H 1.2036 0.7548 0.0811 0.039 Uiso 1 1 calc R . . C20 C 0.72000(19) 0.33110(18) 0.06860(11) 0.0464(4) Uani 1 1 d . . . H20A H 0.7561 0.3155 0.1279 0.070 Uiso 1 1 calc R A . H20B H 0.6451 0.2289 0.0235 0.070 Uiso 1 1 calc R . . H20C H 0.6651 0.3912 0.0765 0.070 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 B1 0.0313(7) 0.0291(7) 0.0311(7) -0.0017(6) 0.0052(6) 0.0146(6) B2 0.0317(7) 0.0303(7) 0.0282(7) -0.0008(6) 0.0076(6) 0.0144(6) P1 0.0406(2) 0.03120(19) 0.02596(19) 0.00268(14) 0.01217(15) 0.01251(16) P2 0.0321(2) 0.0407(2) 0.0408(2) -0.00833(16) 0.00309(15) 0.02078(17) C1 0.0373(8) 0.0290(7) 0.0460(8) 0.0010(6) 0.0003(6) 0.0126(6) C2 0.0590(11) 0.0393(9) 0.0709(12) 0.0158(9) 0.0051(9) 0.0091(8) C3 0.0851(15) 0.0445(10) 0.0622(12) -0.0183(9) 0.0074(11) 0.0144(10) C4 0.0330(9) 0.0450(10) 0.129(2) 0.0222(11) -0.0033(10) 0.0082(8) C5 0.0536(9) 0.0429(8) 0.0404(8) 0.0133(7) 0.0088(7) 0.0264(7) C6 0.0872(14) 0.0492(10) 0.0725(13) 0.0160(9) 0.0169(11) 0.0432(10) C7 0.0839(15) 0.0796(14) 0.0553(11) 0.0221(10) -0.0031(10) 0.0435(12) C8 0.0591(19) 0.0464(15) 0.0334(15) 0.0089(11) 0.0221(14) 0.0109(14) C9 0.096(3) 0.082(3) 0.0420(19) 0.003(2) 0.042(2) 0.029(2) C10 0.071(3) 0.072(3) 0.069(3) 0.0138(17) 0.036(2) -0.008(2) C8D 0.067(7) 0.071(6) 0.039(5) 0.021(4) 0.025(4) 0.035(5) C9D 0.118(15) 0.061(7) 0.052(6) 0.021(5) 0.040(7) 0.034(8) C10D 0.082(9) 0.065(5) 0.055(7) 0.014(5) 0.029(7) 0.009(6) C11 0.0512(10) 0.0497(9) 0.0583(10) 0.0041(8) -0.0035(8) 0.0311(8) C12 0.0669(12) 0.0711(13) 0.0518(10) 0.0045(9) -0.0092(9) 0.0373(11) C13 0.1006(18) 0.0714(14) 0.1008(18) 0.0106(13) -0.0044(14) 0.0627(14) C14 0.0386(15) 0.079(2) 0.061(3) -0.0145(18) 0.0110(15) 0.0301(16) C15 0.075(3) 0.119(5) 0.106(5) -0.041(4) 0.025(3) 0.056(3) C16 0.0372(15) 0.118(4) 0.091(3) -0.023(3) 0.0101(16) 0.0287(19) C14D 0.044(5) 0.072(6) 0.056(7) -0.002(5) 0.013(5) 0.040(5) C15D 0.042(7) 0.083(8) 0.068(7) -0.008(6) 0.018(6) 0.030(5) C16D 0.042(6) 0.086(7) 0.106(12) -0.007(6) 0.032(6) 0.016(5) C17 0.0334(6) 0.0310(6) 0.0247(6) 0.0016(5) 0.0061(5) 0.0178(5) C18 0.0311(6) 0.0317(6) 0.0295(6) 0.0032(5) 0.0082(5) 0.0149(5) C19 0.0318(6) 0.0265(6) 0.0293(6) -0.0012(5) 0.0053(5) 0.0119(5) C20 0.0411(8) 0.0400(8) 0.0430(8) -0.0003(6) 0.0179(7) 0.0105(7) _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 B1 C1 1.612(2) . ? B1 B2 1.871(2) . ? B1 P1 1.8967(16) . ? B1 P2 1.8979(16) . ? B2 C17 1.5792(18) . ? B2 P1 1.8751(16) . ? B2 P2 1.8768(15) . ? P1 C5 1.8466(16) . ? P1 C8D 1.876(8) . ? P1 C8 1.881(3) . ? P2 C11 1.8511(19) . ? P2 C14 1.870(3) . ? P2 C14D 1.873(7) . ? C1 C3 1.526(2) . ? C1 C4 1.529(2) . ? C1 C2 1.533(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.531(2) . ? C5 C7 1.533(2) . ? C5 H5 0.9900 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C10 1.530(4) . ? C8 C9 1.536(6) . ? C8 H8A 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C8D C10D 1.524(7) . ? C8D C9D 1.526(8) . ? C8D H8DA 0.9900 . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C9D H9DC 0.9700 . ? C10D H10D 0.9700 . ? C10D H10E 0.9700 . ? C10D H10F 0.9700 . ? C11 C12 1.536(2) . ? C11 C13 1.536(3) . ? C11 H11 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C16 1.524(5) . ? C14 C15 1.527(6) . ? C14 H14A 0.9900 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C14D C15D 1.527(8) . ? C14D C16D 1.527(8) . ? C14D H14B 0.9900 . ? C15D H15D 0.9700 . ? C15D H15E 0.9700 . ? C15D H15F 0.9700 . ? C16D H16D 0.9700 . ? C16D H16E 0.9700 . ? C16D H16F 0.9700 . ? C17 C19 1.3992(19) . ? C17 C18 1.4087(18) . ? C18 C19 1.3944(18) 2_765 ? C18 C20 1.5093(19) . ? C19 C18 1.3944(18) 2_765 ? C19 H19 0.9400 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? 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 C1 B1 B2 147.67(12) . . ? C1 B1 P1 130.76(11) . . ? B2 B1 P1 59.68(7) . . ? C1 B1 P2 130.74(11) . . ? B2 B1 P2 59.72(7) . . ? P1 B1 P2 97.60(7) . . ? C17 B2 B1 139.22(11) . . ? C17 B2 P1 131.02(10) . . ? B1 B2 P1 60.83(7) . . ? C17 B2 P2 129.87(10) . . ? B1 B2 P2 60.85(7) . . ? P1 B2 P2 99.10(7) . . ? C5 P1 B2 108.42(7) . . ? C5 P1 C8D 118.2(4) . . ? B2 P1 C8D 120.9(4) . . ? C5 P1 C8 101.64(15) . . ? B2 P1 C8 133.49(14) . . ? C8D P1 C8 16.6(4) . . ? C5 P1 B1 115.70(7) . . ? B2 P1 B1 59.48(7) . . ? C8D P1 B1 120.3(4) . . ? C8 P1 B1 133.58(14) . . ? C11 P2 C14 113.1(2) . . ? C11 P2 C14D 97.9(4) . . ? C14 P2 C14D 15.3(5) . . ? C11 P2 B2 108.78(8) . . ? C14 P2 B2 126.0(2) . . ? C14D P2 B2 135.8(4) . . ? C11 P2 B1 115.32(8) . . ? C14 P2 B1 123.85(17) . . ? C14D P2 B1 136.8(4) . . ? B2 P2 B1 59.43(6) . . ? C3 C1 C4 109.33(17) . . ? C3 C1 C2 107.85(16) . . ? C4 C1 C2 106.46(16) . . ? C3 C1 B1 109.73(14) . . ? C4 C1 B1 111.49(13) . . ? C2 C1 B1 111.85(13) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 110.46(15) . . ? C6 C5 P1 110.63(13) . . ? C7 C5 P1 115.69(14) . . ? C6 C5 H5 106.5 . . ? C7 C5 H5 106.5 . . ? P1 C5 H5 106.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 112.3(5) . . ? C10 C8 P1 111.6(3) . . ? C9 C8 P1 109.9(3) . . ? C10 C8 H8A 107.6 . . ? C9 C8 H8A 107.6 . . ? P1 C8 H8A 107.6 . . ? C10D C8D C9D 113.5(8) . . ? C10D C8D P1 111.9(6) . . ? C9D C8D P1 111.6(7) . . ? C10D C8D H8DA 106.4 . . ? C9D C8D H8DA 106.4 . . ? P1 C8D H8DA 106.4 . . ? C8D C9D H9DA 109.5 . . ? C8D C9D H9DB 109.5 . . ? H9DA C9D H9DB 109.5 . . ? C8D C9D H9DC 109.5 . . ? H9DA C9D H9DC 109.5 . . ? H9DB C9D H9DC 109.5 . . ? C8D C10D H10D 109.5 . . ? C8D C10D H10E 109.5 . . ? H10D C10D H10E 109.5 . . ? C8D C10D H10F 109.5 . . ? H10D C10D H10F 109.5 . . ? H10E C10D H10F 109.5 . . ? C12 C11 C13 110.94(16) . . ? C12 C11 P2 111.93(14) . . ? C13 C11 P2 115.25(16) . . ? C12 C11 H11 106.0 . . ? C13 C11 H11 106.0 . . ? P2 C11 H11 106.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 113.6(6) . . ? C16 C14 P2 113.5(3) . . ? C15 C14 P2 111.3(3) . . ? C16 C14 H14A 105.9 . . ? C15 C14 H14A 105.9 . . ? P2 C14 H14A 105.9 . . ? C15D C14D C16D 113.4(9) . . ? C15D C14D P2 111.7(6) . . ? C16D C14D P2 111.9(6) . . ? C15D C14D H14B 106.4 . . ? C16D C14D H14B 106.4 . . ? P2 C14D H14B 106.4 . . ? C14D C15D H15D 109.5 . . ? C14D C15D H15E 109.5 . . ? H15D C15D H15E 109.5 . . ? C14D C15D H15F 109.5 . . ? H15D C15D H15F 109.5 . . ? H15E C15D H15F 109.5 . . ? C14D C16D H16D 109.5 . . ? C14D C16D H16E 109.5 . . ? H16D C16D H16E 109.5 . . ? C14D C16D H16F 109.5 . . ? H16D C16D H16F 109.5 . . ? H16E C16D H16F 109.5 . . ? C19 C17 C18 117.11(11) . . ? C19 C17 B2 119.01(11) . . ? C18 C17 B2 123.87(12) . . ? C19 C18 C17 119.22(12) 2_765 . ? C19 C18 C20 119.95(12) 2_765 . ? C17 C18 C20 120.83(12) . . ? C18 C19 C17 123.67(12) 2_765 . ? C18 C19 H19 118.2 2_765 . ? C17 C19 H19 118.2 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? 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 C1 B1 B2 C17 -0.9(3) . . . . ? P1 B1 B2 C17 -120.25(18) . . . . ? P2 B1 B2 C17 118.51(18) . . . . ? C1 B1 B2 P1 119.4(2) . . . . ? P2 B1 B2 P1 -121.25(7) . . . . ? C1 B1 B2 P2 -119.4(2) . . . . ? P1 B1 B2 P2 121.25(7) . . . . ? C17 B2 P1 C5 22.07(15) . . . . ? B1 B2 P1 C5 -109.53(8) . . . . ? P2 B2 P1 C5 -158.65(7) . . . . ? C17 B2 P1 C8D -119.2(5) . . . . ? B1 B2 P1 C8D 109.2(4) . . . . ? P2 B2 P1 C8D 60.1(4) . . . . ? C17 B2 P1 C8 -105.5(2) . . . . ? B1 B2 P1 C8 122.95(19) . . . . ? P2 B2 P1 C8 73.82(19) . . . . ? C17 B2 P1 B1 131.59(15) . . . . ? P2 B2 P1 B1 -49.13(7) . . . . ? C1 B1 P1 C5 -44.94(16) . . . . ? B2 B1 P1 C5 97.08(8) . . . . ? P2 B1 P1 C5 145.23(7) . . . . ? C1 B1 P1 B2 -142.02(16) . . . . ? P2 B1 P1 B2 48.15(7) . . . . ? C1 B1 P1 C8D 107.7(5) . . . . ? B2 B1 P1 C8D -110.2(4) . . . . ? P2 B1 P1 C8D -62.1(4) . . . . ? C1 B1 P1 C8 95.2(2) . . . . ? B2 B1 P1 C8 -122.82(18) . . . . ? P2 B1 P1 C8 -74.67(19) . . . . ? C17 B2 P2 C11 -22.70(15) . . . . ? B1 B2 P2 C11 108.89(9) . . . . ? P1 B2 P2 C11 158.01(8) . . . . ? C17 B2 P2 C14 116.6(2) . . . . ? B1 B2 P2 C14 -111.77(19) . . . . ? P1 B2 P2 C14 -62.6(2) . . . . ? C17 B2 P2 C14D 101.1(6) . . . . ? B1 B2 P2 C14D -127.3(6) . . . . ? P1 B2 P2 C14D -78.2(6) . . . . ? C17 B2 P2 B1 -131.59(15) . . . . ? P1 B2 P2 B1 49.12(7) . . . . ? C1 B1 P2 C11 44.33(16) . . . . ? B2 B1 P2 C11 -97.72(9) . . . . ? P1 B1 P2 C11 -145.84(7) . . . . ? C1 B1 P2 C14 -102.8(3) . . . . ? B2 B1 P2 C14 115.2(2) . . . . ? P1 B1 P2 C14 67.0(2) . . . . ? C1 B1 P2 C14D -92.1(6) . . . . ? B2 B1 P2 C14D 125.9(6) . . . . ? P1 B1 P2 C14D 77.8(6) . . . . ? C1 B1 P2 B2 142.04(16) . . . . ? P1 B1 P2 B2 -48.12(7) . . . . ? B2 B1 C1 C3 174.3(2) . . . . ? P1 B1 C1 C3 -89.01(18) . . . . ? P2 B1 C1 C3 77.64(19) . . . . ? B2 B1 C1 C4 -64.4(3) . . . . ? P1 B1 C1 C4 32.3(2) . . . . ? P2 B1 C1 C4 -161.09(15) . . . . ? B2 B1 C1 C2 54.7(3) . . . . ? P1 B1 C1 C2 151.34(14) . . . . ? P2 B1 C1 C2 -42.0(2) . . . . ? B2 P1 C5 C6 -70.59(14) . . . . ? C8D P1 C5 C6 71.8(5) . . . . ? C8 P1 C5 C6 73.43(16) . . . . ? B1 P1 C5 C6 -134.89(12) . . . . ? B2 P1 C5 C7 162.86(14) . . . . ? C8D P1 C5 C7 -54.7(5) . . . . ? C8 P1 C5 C7 -53.12(18) . . . . ? B1 P1 C5 C7 98.56(15) . . . . ? C5 P1 C8 C10 -112.7(4) . . . . ? B2 P1 C8 C10 17.1(5) . . . . ? C8D P1 C8 C10 62.4(17) . . . . ? B1 P1 C8 C10 103.4(3) . . . . ? C5 P1 C8 C9 122.0(5) . . . . ? B2 P1 C8 C9 -108.2(5) . . . . ? C8D P1 C8 C9 -62.9(17) . . . . ? B1 P1 C8 C9 -21.8(6) . . . . ? C5 P1 C8D C10D -52.5(10) . . . . ? B2 P1 C8D C10D 85.2(10) . . . . ? C8 P1 C8D C10D -57.9(15) . . . . ? B1 P1 C8D C10D 155.5(8) . . . . ? C5 P1 C8D C9D 75.9(13) . . . . ? B2 P1 C8D C9D -146.5(12) . . . . ? C8 P1 C8D C9D 70.5(18) . . . . ? B1 P1 C8D C9D -76.1(13) . . . . ? C14 P2 C11 C12 -77.8(2) . . . . ? C14D P2 C11 C12 -76.9(4) . . . . ? B2 P2 C11 C12 67.25(15) . . . . ? B1 P2 C11 C12 131.57(13) . . . . ? C14 P2 C11 C13 50.2(2) . . . . ? C14D P2 C11 C13 51.1(4) . . . . ? B2 P2 C11 C13 -164.74(16) . . . . ? B1 P2 C11 C13 -100.42(17) . . . . ? C11 P2 C14 C16 50.8(5) . . . . ? C14D P2 C14 C16 47.6(17) . . . . ? B2 P2 C14 C16 -87.1(5) . . . . ? B1 P2 C14 C16 -161.4(4) . . . . ? C11 P2 C14 C15 -78.8(6) . . . . ? C14D P2 C14 C15 -82(2) . . . . ? B2 P2 C14 C15 143.3(6) . . . . ? B1 P2 C14 C15 69.0(7) . . . . ? C11 P2 C14D C15D -120.2(14) . . . . ? C14 P2 C14D C15D 56.8(18) . . . . ? B2 P2 C14D C15D 112.4(15) . . . . ? B1 P2 C14D C15D 20.8(17) . . . . ? C11 P2 C14D C16D 111.4(10) . . . . ? C14 P2 C14D C16D -72(2) . . . . ? B2 P2 C14D C16D -16.0(13) . . . . ? B1 P2 C14D C16D -107.6(9) . . . . ? B1 B2 C17 C19 -0.5(2) . . . . ? P1 B2 C17 C19 -91.61(16) . . . . ? P2 B2 C17 C19 89.32(16) . . . . ? B1 B2 C17 C18 -179.53(14) . . . . ? P1 B2 C17 C18 89.35(17) . . . . ? P2 B2 C17 C18 -89.73(17) . . . . ? C19 C17 C18 C19 -0.2(2) . . . 2_765 ? B2 C17 C18 C19 178.82(12) . . . 2_765 ? C19 C17 C18 C20 179.63(13) . . . . ? B2 C17 C18 C20 -1.3(2) . . . . ? C18 C17 C19 C18 0.3(2) . . . 2_765 ? B2 C17 C19 C18 -178.86(12) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.323 _refine_diff_density_min -0.167 _refine_diff_density_rms 0.042 #===END data_gb231m _database_code_depnum_ccdc_archive 'CCDC 669746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H80 B4 P4' _chemical_formula_weight 716.15 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' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.184(2) _cell_length_b 9.8153(12) _cell_length_c 28.413(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.509(4) _cell_angle_gamma 90.00 _cell_volume 4696.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 8156 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.60 _exptl_crystal_description 'prism frag.' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9383 _exptl_absorpt_correction_T_max 0.9746 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41048 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9606 _reflns_number_gt 6245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0660P)^2^+4.5143P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9606 _refine_ls_number_parameters 481 _refine_ls_number_restraints 95 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.034 _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 0.37719(5) 0.83051(8) 0.65503(3) 0.0422(2) Uani 1 1 d D . . P2 P 0.39652(5) 0.61562(9) 0.59037(3) 0.0444(2) Uani 1 1 d D . . P3 P 0.14900(5) 1.00916(7) 0.34912(3) 0.03641(19) Uani 1 1 d . . . P4 P 0.09097(4) 1.20709(7) 0.40716(3) 0.03525(19) Uani 1 1 d . . . B1 B 0.33118(19) 0.6582(3) 0.63489(12) 0.0365(7) Uani 1 1 d . A . B2 B 0.3486(2) 0.7883(4) 0.58971(13) 0.0420(8) Uani 1 1 d . A . B3 B 0.0575(2) 1.0394(3) 0.37600(11) 0.0344(7) Uani 1 1 d . . . B4 B 0.1593(2) 1.0553(3) 0.41401(12) 0.0355(7) Uani 1 1 d . . . C1 C 0.26873(17) 0.5664(3) 0.65555(10) 0.0387(7) Uani 1 1 d . . . C2 C 0.2082(2) 0.6501(4) 0.67523(14) 0.0626(10) Uani 1 1 d . A . H2A H 0.1716 0.5896 0.6869 0.094 Uiso 1 1 calc R . . H2B H 0.1790 0.7075 0.6500 0.094 Uiso 1 1 calc R . . H2C H 0.2353 0.7067 0.7014 0.094 Uiso 1 1 calc R . . C3 C 0.2209(2) 0.4734(4) 0.61685(13) 0.0613(10) Uani 1 1 d . A . H3A H 0.1827 0.4217 0.6305 0.092 Uiso 1 1 calc R . . H3B H 0.2566 0.4114 0.6052 0.092 Uiso 1 1 calc R . . H3C H 0.1930 0.5285 0.5904 0.092 Uiso 1 1 calc R . . C4 C 0.3135(2) 0.4758(4) 0.69562(14) 0.0725(12) Uani 1 1 d . A . H4A H 0.2760 0.4190 0.7080 0.109 Uiso 1 1 calc R . . H4B H 0.3424 0.5323 0.7213 0.109 Uiso 1 1 calc R . . H4C H 0.3506 0.4185 0.6830 0.109 Uiso 1 1 calc R . . C5 C 0.3070(2) 0.9557(3) 0.67182(13) 0.0549(9) Uani 1 1 d . A . H5A H 0.2531 0.9205 0.6586 0.066 Uiso 1 1 calc R . . C6 C 0.3126(3) 1.0936(4) 0.64790(18) 0.0834(14) Uani 1 1 d . . . H6A H 0.2718 1.1538 0.6551 0.125 Uiso 1 1 calc R A . H6B H 0.3051 1.0815 0.6134 0.125 Uiso 1 1 calc R . . H6C H 0.3645 1.1332 0.6600 0.125 Uiso 1 1 calc R . . C7 C 0.3120(3) 0.9721(5) 0.72604(15) 0.0839(14) Uani 1 1 d . . . H7A H 0.2656 1.0209 0.7316 0.126 Uiso 1 1 calc R A . H7B H 0.3595 1.0228 0.7398 0.126 Uiso 1 1 calc R . . H7C H 0.3140 0.8829 0.7409 0.126 Uiso 1 1 calc R . . C8 C 0.4827(3) 0.8541(7) 0.6864(2) 0.0564(16) Uani 0.664(6) 1 d PDU A 1 H8A H 0.5136 0.7913 0.6700 0.068 Uiso 0.664(6) 1 calc PR A 1 C9 C 0.5149(6) 0.9944(8) 0.6792(4) 0.078(3) Uani 0.664(6) 1 d PDU A 1 H9A H 0.5712 0.9972 0.6931 0.117 Uiso 0.664(6) 1 calc PR A 1 H9B H 0.4873 1.0618 0.6947 0.117 Uiso 0.664(6) 1 calc PR A 1 H9C H 0.5069 1.0140 0.6451 0.117 Uiso 0.664(6) 1 calc PR A 1 C10 C 0.4946(5) 0.8011(9) 0.7379(2) 0.076(2) Uani 0.664(6) 1 d PDU A 1 H10A H 0.5508 0.8018 0.7523 0.114 Uiso 0.664(6) 1 calc PR A 1 H10B H 0.4744 0.7088 0.7377 0.114 Uiso 0.664(6) 1 calc PR A 1 H10C H 0.4662 0.8591 0.7564 0.114 Uiso 0.664(6) 1 calc PR A 1 C8D C 0.4684(6) 0.8924(11) 0.6984(4) 0.049(4) Uiso 0.336(6) 1 d PDU A 2 H8DA H 0.4521 0.9590 0.7207 0.059 Uiso 0.336(6) 1 calc PR A 2 C9D C 0.5257(12) 0.9612(19) 0.6711(7) 0.068(6) Uiso 0.336(6) 1 d PDU A 2 H9DA H 0.5695 1.0007 0.6938 0.103 Uiso 0.336(6) 1 calc PR A 2 H9DB H 0.4980 1.0323 0.6506 0.103 Uiso 0.336(6) 1 calc PR A 2 H9DC H 0.5459 0.8942 0.6514 0.103 Uiso 0.336(6) 1 calc PR A 2 C10D C 0.5128(10) 0.7748(16) 0.7274(6) 0.066(5) Uiso 0.336(6) 1 d PDU A 2 H10D H 0.5616 0.8087 0.7471 0.099 Uiso 0.336(6) 1 calc PR A 2 H10E H 0.5252 0.7057 0.7056 0.099 Uiso 0.336(6) 1 calc PR A 2 H10F H 0.4797 0.7356 0.7478 0.099 Uiso 0.336(6) 1 calc PR A 2 C11 C 0.3465(2) 0.5210(4) 0.53654(13) 0.0613(10) Uani 1 1 d . A . H11A H 0.2887 0.5352 0.5337 0.074 Uiso 1 1 calc R . . C12 C 0.3687(3) 0.5825(6) 0.49124(14) 0.0874(14) Uani 1 1 d . . . H12A H 0.3428 0.5313 0.4633 0.131 Uiso 1 1 calc R A . H12B H 0.4258 0.5782 0.4939 0.131 Uiso 1 1 calc R . . H12C H 0.3514 0.6767 0.4879 0.131 Uiso 1 1 calc R . . C13 C 0.3606(3) 0.3682(5) 0.53920(19) 0.0926(15) Uani 1 1 d . . . H13A H 0.3251 0.3240 0.5127 0.139 Uiso 1 1 calc R A . H13B H 0.3504 0.3337 0.5694 0.139 Uiso 1 1 calc R . . H13C H 0.4152 0.3492 0.5372 0.139 Uiso 1 1 calc R . . C14 C 0.5048(3) 0.5776(8) 0.5954(3) 0.077(2) Uani 0.664(6) 1 d PDU A 1 H14A H 0.5049 0.5073 0.5705 0.092 Uiso 0.664(6) 1 calc PR A 1 C15 C 0.5531(4) 0.6896(8) 0.5804(3) 0.074(2) Uani 0.664(6) 1 d PDU A 1 H15A H 0.6072 0.6584 0.5823 0.110 Uiso 0.664(6) 1 calc PR A 1 H15B H 0.5530 0.7674 0.6014 0.110 Uiso 0.664(6) 1 calc PR A 1 H15C H 0.5305 0.7160 0.5476 0.110 Uiso 0.664(6) 1 calc PR A 1 C16 C 0.5385(5) 0.5040(10) 0.6410(3) 0.092(3) Uani 0.664(6) 1 d PDU A 1 H16A H 0.5899 0.4663 0.6390 0.138 Uiso 0.664(6) 1 calc PR A 1 H16B H 0.5029 0.4308 0.6458 0.138 Uiso 0.664(6) 1 calc PR A 1 H16C H 0.5445 0.5669 0.6678 0.138 Uiso 0.664(6) 1 calc PR A 1 C14D C 0.4976(5) 0.5353(12) 0.6006(5) 0.046(3) Uiso 0.336(6) 1 d PD A 2 H14B H 0.4985 0.4803 0.5715 0.055 Uiso 0.336(6) 1 calc PR A 2 C15D C 0.5607(11) 0.6411(18) 0.6019(7) 0.099(6) Uiso 0.336(6) 1 d PD A 2 H15D H 0.6123 0.6014 0.6146 0.148 Uiso 0.336(6) 1 calc PR A 2 H15E H 0.5511 0.7161 0.6222 0.148 Uiso 0.336(6) 1 calc PR A 2 H15F H 0.5595 0.6745 0.5696 0.148 Uiso 0.336(6) 1 calc PR A 2 C16D C 0.5171(11) 0.4382(18) 0.6417(6) 0.086(6) Uiso 0.336(6) 1 d PD A 2 H16D H 0.5739 0.4221 0.6491 0.129 Uiso 0.336(6) 1 calc PR A 2 H16E H 0.4896 0.3527 0.6331 0.129 Uiso 0.336(6) 1 calc PR A 2 H16F H 0.5005 0.4767 0.6696 0.129 Uiso 0.336(6) 1 calc PR A 2 C17 C 0.30064(18) 0.8672(3) 0.54504(11) 0.0418(7) Uani 1 1 d . . . C18 C 0.33568(19) 0.9598(4) 0.51792(12) 0.0507(8) Uani 1 1 d D A . H18A H 0.3896 0.9825 0.5278 0.061 Uiso 0.336(6) 1 calc PR A 2 C23 C 0.4228(3) 1.0039(8) 0.5340(2) 0.089(3) Uani 0.664(6) 1 d PD A 1 H23A H 0.4330 1.0828 0.5156 0.133 Uiso 0.664(6) 1 calc PR A 1 H23B H 0.4575 0.9298 0.5288 0.133 Uiso 0.664(6) 1 calc PR A 1 H23C H 0.4330 1.0270 0.5679 0.133 Uiso 0.664(6) 1 calc PR A 1 C19 C 0.29124(19) 1.0183(3) 0.47657(11) 0.0473(8) Uani 1 1 d D . . H19A H 0.3165 1.0792 0.4589 0.057 Uiso 0.664(6) 1 calc PR A 1 C23D C 0.3355(6) 1.1033(10) 0.4464(3) 0.052(3) Uiso 0.336(6) 1 d PD A 2 H23D H 0.3057 1.1857 0.4363 0.078 Uiso 0.336(6) 1 calc PR A 2 H23E H 0.3421 1.0517 0.4184 0.078 Uiso 0.336(6) 1 calc PR A 2 H23F H 0.3873 1.1272 0.4652 0.078 Uiso 0.336(6) 1 calc PR A 2 C20 C 0.21125(17) 0.9906(3) 0.46033(10) 0.0371(6) Uani 1 1 d . A . C21 C 0.17675(17) 0.8997(3) 0.48812(11) 0.0427(7) Uani 1 1 d . . . H21A H 0.1226 0.8783 0.4786 0.051 Uiso 1 1 calc R A . C22 C 0.22018(18) 0.8406(3) 0.52904(11) 0.0440(7) Uani 1 1 d . A . H22A H 0.1946 0.7804 0.5467 0.053 Uiso 1 1 calc R . . C24 C -0.02646(18) 0.9628(3) 0.36659(11) 0.0391(7) Uani 1 1 d . . . C25 C -0.0173(2) 0.8076(3) 0.37072(14) 0.0583(9) Uani 1 1 d . . . H25A H -0.0694 0.7657 0.3664 0.087 Uiso 1 1 calc R . . H25B H 0.0133 0.7843 0.4022 0.087 Uiso 1 1 calc R . . H25C H 0.0099 0.7746 0.3462 0.087 Uiso 1 1 calc R . . C26 C -0.0773(2) 1.0049(4) 0.40301(13) 0.0565(9) Uani 1 1 d . . . H26A H -0.1279 0.9578 0.3957 0.085 Uiso 1 1 calc R . . H26B H -0.0862 1.1025 0.4011 0.085 Uiso 1 1 calc R . . H26C H -0.0498 0.9808 0.4352 0.085 Uiso 1 1 calc R . . C27 C -0.0732(2) 0.9973(4) 0.31621(12) 0.0607(9) Uani 1 1 d . . . H27A H -0.1238 0.9503 0.3106 0.091 Uiso 1 1 calc R . . H27B H -0.0431 0.9687 0.2924 0.091 Uiso 1 1 calc R . . H27C H -0.0822 1.0948 0.3137 0.091 Uiso 1 1 calc R . . C28 C 0.1881(2) 1.0934(3) 0.29933(11) 0.0498(8) Uani 1 1 d . . . H28A H 0.2086 1.0192 0.2815 0.060 Uiso 1 1 calc R . . C29 C 0.2583(3) 1.1865(4) 0.31764(15) 0.0722(11) Uani 1 1 d . . . H29A H 0.2805 1.2183 0.2908 0.108 Uiso 1 1 calc R . . H29B H 0.2985 1.1367 0.3399 0.108 Uiso 1 1 calc R . . H29C H 0.2407 1.2640 0.3340 0.108 Uiso 1 1 calc R . . C30 C 0.1220(3) 1.1622(4) 0.26349(13) 0.0734(12) Uani 1 1 d . . . H30A H 0.1435 1.1989 0.2371 0.110 Uiso 1 1 calc R . . H30B H 0.0993 1.2354 0.2793 0.110 Uiso 1 1 calc R . . H30C H 0.0810 1.0960 0.2513 0.110 Uiso 1 1 calc R . . C31 C 0.1745(2) 0.8279(3) 0.34336(12) 0.0501(8) Uani 1 1 d . . . H31A H 0.1525 0.7777 0.3680 0.060 Uiso 1 1 calc R . . C32 C 0.2644(2) 0.8067(4) 0.35538(17) 0.0755(12) Uani 1 1 d . . . H32A H 0.2762 0.7103 0.3539 0.113 Uiso 1 1 calc R . . H32B H 0.2855 0.8407 0.3875 0.113 Uiso 1 1 calc R . . H32C H 0.2887 0.8557 0.3324 0.113 Uiso 1 1 calc R . . C33 C 0.1371(3) 0.7651(4) 0.29483(14) 0.0721(12) Uani 1 1 d . . . H33A H 0.1459 0.6675 0.2960 0.108 Uiso 1 1 calc R . . H33B H 0.1612 0.8047 0.2699 0.108 Uiso 1 1 calc R . . H33C H 0.0805 0.7834 0.2878 0.108 Uiso 1 1 calc R . . C34 C 0.1037(2) 1.3708(3) 0.37693(13) 0.0502(8) Uani 1 1 d . . . H34A H 0.1334 1.3466 0.3517 0.060 Uiso 1 1 calc R . . C35 C 0.1561(3) 1.4740(4) 0.40820(17) 0.0848(14) Uani 1 1 d . . . H35A H 0.1691 1.5474 0.3883 0.127 Uiso 1 1 calc R . . H35B H 0.2045 1.4298 0.4245 0.127 Uiso 1 1 calc R . . H35C H 0.1280 1.5106 0.4318 0.127 Uiso 1 1 calc R . . C36 C 0.0258(2) 1.4302(4) 0.34974(16) 0.0747(12) Uani 1 1 d . . . H36A H 0.0368 1.5010 0.3282 0.112 Uiso 1 1 calc R . . H36B H -0.0036 1.4685 0.3724 0.112 Uiso 1 1 calc R . . H36C H -0.0054 1.3587 0.3313 0.112 Uiso 1 1 calc R . . C37 C 0.0574(2) 1.2373(3) 0.46426(11) 0.0471(8) Uani 1 1 d . . . H37A H 0.0388 1.1480 0.4738 0.057 Uiso 1 1 calc R . . C38 C 0.1254(2) 1.2802(4) 0.50534(12) 0.0651(10) Uani 1 1 d . . . H38A H 0.1064 1.2816 0.5353 0.098 Uiso 1 1 calc R . . H38B H 0.1438 1.3704 0.4989 0.098 Uiso 1 1 calc R . . H38C H 0.1688 1.2157 0.5078 0.098 Uiso 1 1 calc R . . C39 C -0.0135(2) 1.3345(4) 0.46082(15) 0.0672(11) Uani 1 1 d . . . H39A H -0.0336 1.3302 0.4903 0.101 Uiso 1 1 calc R . . H39B H -0.0550 1.3079 0.4340 0.101 Uiso 1 1 calc R . . H39C H 0.0034 1.4268 0.4559 0.101 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 0.0400(4) 0.0388(4) 0.0422(4) 0.0014(3) -0.0056(3) -0.0028(3) P2 0.0387(4) 0.0511(5) 0.0441(5) 0.0007(4) 0.0103(3) 0.0060(4) P3 0.0471(4) 0.0313(4) 0.0330(4) 0.0070(3) 0.0133(3) 0.0036(3) P4 0.0410(4) 0.0268(3) 0.0367(4) -0.0006(3) 0.0048(3) -0.0024(3) B1 0.0357(17) 0.0374(17) 0.0335(17) 0.0017(14) -0.0002(13) 0.0053(13) B2 0.0372(18) 0.0447(19) 0.0424(19) 0.0090(16) 0.0041(15) -0.0009(15) B3 0.0429(18) 0.0289(15) 0.0307(16) 0.0026(13) 0.0057(14) 0.0020(13) B4 0.0409(18) 0.0326(16) 0.0345(17) 0.0056(13) 0.0113(14) -0.0019(14) C1 0.0438(17) 0.0363(15) 0.0357(16) 0.0030(12) 0.0074(13) 0.0008(13) C2 0.063(2) 0.057(2) 0.078(3) -0.0042(19) 0.039(2) -0.0044(18) C3 0.066(2) 0.057(2) 0.063(2) -0.0061(18) 0.0177(18) -0.0227(18) C4 0.072(3) 0.073(3) 0.070(3) 0.039(2) 0.009(2) 0.001(2) C5 0.057(2) 0.0389(17) 0.062(2) -0.0091(16) -0.0048(17) 0.0016(15) C6 0.081(3) 0.0350(19) 0.127(4) 0.000(2) 0.001(3) 0.0029(19) C7 0.095(3) 0.082(3) 0.069(3) -0.035(2) 0.002(2) 0.011(2) C8 0.039(3) 0.066(4) 0.058(3) -0.010(3) -0.005(3) 0.001(3) C9 0.054(5) 0.076(5) 0.096(6) -0.026(5) -0.003(4) -0.028(4) C10 0.059(5) 0.107(6) 0.049(4) -0.013(4) -0.020(4) 0.005(4) C11 0.059(2) 0.074(3) 0.053(2) -0.0189(19) 0.0172(17) 0.0024(19) C12 0.081(3) 0.131(4) 0.054(2) -0.019(3) 0.023(2) 0.001(3) C13 0.103(4) 0.072(3) 0.110(4) -0.038(3) 0.039(3) 0.000(3) C14 0.047(4) 0.068(5) 0.118(6) 0.012(5) 0.022(4) 0.009(3) C15 0.040(3) 0.105(6) 0.080(5) -0.018(4) 0.023(3) -0.013(3) C16 0.060(5) 0.100(7) 0.109(6) 0.003(5) -0.001(4) 0.040(5) C17 0.0410(16) 0.0463(17) 0.0367(16) 0.0082(13) 0.0042(13) -0.0011(13) C18 0.0418(18) 0.061(2) 0.0476(19) 0.0137(16) 0.0044(14) -0.0101(15) C23 0.058(4) 0.118(6) 0.082(5) 0.056(4) -0.007(3) -0.030(4) C19 0.0456(18) 0.0515(18) 0.0443(18) 0.0171(15) 0.0080(14) -0.0080(15) C20 0.0390(16) 0.0373(15) 0.0352(15) 0.0062(12) 0.0080(12) 0.0017(12) C21 0.0324(15) 0.0512(18) 0.0438(17) 0.0141(14) 0.0058(13) 0.0000(13) C22 0.0403(16) 0.0487(17) 0.0442(18) 0.0161(14) 0.0110(13) 0.0011(14) C24 0.0443(17) 0.0307(14) 0.0416(16) -0.0050(12) 0.0068(13) -0.0035(12) C25 0.059(2) 0.0328(16) 0.085(3) -0.0053(17) 0.0193(19) -0.0092(15) C26 0.0466(19) 0.058(2) 0.069(2) -0.0176(18) 0.0208(17) -0.0131(16) C27 0.056(2) 0.066(2) 0.053(2) -0.0071(18) -0.0071(17) -0.0069(18) C28 0.068(2) 0.0468(18) 0.0400(18) 0.0089(14) 0.0246(16) 0.0018(16) C29 0.084(3) 0.065(2) 0.079(3) 0.010(2) 0.042(2) -0.014(2) C30 0.105(3) 0.070(3) 0.046(2) 0.0223(19) 0.018(2) 0.010(2) C31 0.069(2) 0.0368(16) 0.052(2) 0.0076(14) 0.0310(17) 0.0118(15) C32 0.080(3) 0.054(2) 0.103(3) 0.013(2) 0.042(2) 0.027(2) C33 0.118(4) 0.045(2) 0.063(2) -0.0106(18) 0.044(2) -0.002(2) C34 0.057(2) 0.0313(15) 0.061(2) 0.0091(15) 0.0079(16) -0.0049(14) C35 0.099(3) 0.046(2) 0.098(3) 0.009(2) -0.007(3) -0.032(2) C36 0.079(3) 0.047(2) 0.091(3) 0.020(2) 0.000(2) 0.0116(19) C37 0.058(2) 0.0381(16) 0.0468(18) -0.0124(14) 0.0139(15) -0.0103(14) C38 0.080(3) 0.067(2) 0.047(2) -0.0148(18) 0.0097(18) -0.013(2) C39 0.067(2) 0.055(2) 0.085(3) -0.029(2) 0.027(2) -0.0025(18) _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 C5 1.850(4) . ? P1 C8 1.868(4) . ? P1 B2 1.869(4) . ? P1 C8D 1.890(8) . ? P1 B1 1.906(3) . ? P2 C11 1.848(4) . ? P2 C14 1.874(5) . ? P2 C14D 1.877(8) . ? P2 B2 1.883(4) . ? P2 B1 1.898(4) . ? P3 C31 1.847(3) . ? P3 B4 1.872(3) . ? P3 C28 1.875(3) . ? P3 B3 1.904(3) . ? P4 C37 1.851(3) . ? P4 C34 1.856(3) . ? P4 B4 1.883(3) . ? P4 B3 1.903(3) . ? B1 C1 1.600(4) . ? B1 B2 1.877(5) . ? B2 C17 1.573(4) . ? B3 C24 1.601(4) . ? B3 B4 1.870(5) . ? B4 C20 1.570(4) . ? C1 C2 1.517(4) . ? C1 C4 1.526(4) . ? C1 C3 1.536(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.526(5) . ? C5 C7 1.534(5) . ? C5 H5A 0.9900 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.513(6) . ? C8 C10 1.527(6) . ? C8 H8A 0.9900 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C8D C9D 1.527(8) . ? C8D C10D 1.530(8) . ? C8D H8DA 0.9900 . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C9D H9DC 0.9700 . ? C10D H10D 0.9700 . ? C10D H10E 0.9700 . ? C10D H10F 0.9700 . ? C11 C13 1.519(6) . ? C11 C12 1.537(6) . ? C11 H11A 0.9900 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 C15 1.491(7) . ? C14 C16 1.495(6) . ? C14 H14A 0.9900 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C14D C16D 1.493(8) . ? C14D C15D 1.496(8) . ? C14D H14B 0.9900 . ? C15D H15D 0.9700 . ? C15D H15E 0.9700 . ? C15D H15F 0.9700 . ? C16D H16D 0.9700 . ? C16D H16E 0.9700 . ? C16D H16F 0.9700 . ? C17 C22 1.391(4) . ? C17 C18 1.402(4) . ? C18 C19 1.391(4) . ? C18 C23 1.539(6) . ? C18 H18A 0.9400 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C19 C20 1.387(4) . ? C19 C23D 1.506(8) . ? C19 H19A 0.9400 . ? C23D H23D 0.9700 . ? C23D H23E 0.9700 . ? C23D H23F 0.9700 . ? C20 C21 1.400(4) . ? C21 C22 1.378(4) . ? C21 H21A 0.9400 . ? C22 H22A 0.9400 . ? C24 C27 1.533(4) . ? C24 C25 1.534(4) . ? C24 C26 1.538(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.521(5) . ? C28 C30 1.524(5) . ? C28 H28A 0.9900 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 C32 1.529(5) . ? C31 C33 1.530(5) . ? C31 H31A 0.9900 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 C35 1.518(5) . ? C34 C36 1.521(5) . ? C34 H34A 0.9900 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 C39 1.535(5) . ? C37 C38 1.536(5) . ? C37 H37A 0.9900 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? 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 P1 C8 114.5(3) . . ? C5 P1 B2 110.36(16) . . ? C8 P1 B2 122.6(3) . . ? C5 P1 C8D 96.7(4) . . ? C8 P1 C8D 18.1(4) . . ? B2 P1 C8D 137.5(4) . . ? C5 P1 B1 114.48(15) . . ? C8 P1 B1 123.9(2) . . ? B2 P1 B1 59.62(15) . . ? C8D P1 B1 136.2(4) . . ? C11 P2 C14 104.7(3) . . ? C11 P2 C14D 100.4(5) . . ? C14 P2 C14D 14.3(4) . . ? C11 P2 B2 108.30(17) . . ? C14 P2 B2 127.2(3) . . ? C14D P2 B2 140.3(4) . . ? C11 P2 B1 115.01(16) . . ? C14 P2 B1 134.6(3) . . ? C14D P2 B1 129.9(4) . . ? B2 P2 B1 59.52(15) . . ? C31 P3 B4 110.03(15) . . ? C31 P3 C28 103.36(15) . . ? B4 P3 C28 131.22(15) . . ? C31 P3 B3 114.51(14) . . ? B4 P3 B3 59.36(14) . . ? C28 P3 B3 133.09(14) . . ? C37 P4 C34 110.65(15) . . ? C37 P4 B4 109.45(15) . . ? C34 P4 B4 127.22(15) . . ? C37 P4 B3 115.36(14) . . ? C34 P4 B3 125.92(15) . . ? B4 P4 B3 59.19(14) . . ? C1 B1 B2 147.6(2) . . ? C1 B1 P2 130.5(2) . . ? B2 B1 P2 59.83(16) . . ? C1 B1 P1 131.2(2) . . ? B2 B1 P1 59.22(15) . . ? P2 B1 P1 97.50(16) . . ? C17 B2 P1 133.1(3) . . ? C17 B2 B1 139.2(3) . . ? P1 B2 B1 61.16(15) . . ? C17 B2 P2 127.5(3) . . ? P1 B2 P2 99.33(16) . . ? B1 B2 P2 60.65(15) . . ? C24 B3 B4 147.5(2) . . ? C24 B3 P4 131.5(2) . . ? B4 B3 P4 59.87(14) . . ? C24 B3 P3 130.4(2) . . ? B4 B3 P3 59.48(15) . . ? P4 B3 P3 97.12(15) . . ? C20 B4 B3 139.5(2) . . ? C20 B4 P3 130.9(2) . . ? B3 B4 P3 61.17(15) . . ? C20 B4 P4 130.2(2) . . ? B3 B4 P4 60.94(14) . . ? P3 B4 P4 98.93(15) . . ? C2 C1 C4 108.7(3) . . ? C2 C1 C3 106.1(3) . . ? C4 C1 C3 107.8(3) . . ? C2 C1 B1 112.9(3) . . ? C4 C1 B1 109.1(3) . . ? C3 C1 B1 112.0(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 111.0(3) . . ? C6 C5 P1 111.9(3) . . ? C7 C5 P1 114.8(3) . . ? C6 C5 H5A 106.2 . . ? C7 C5 H5A 106.2 . . ? P1 C5 H5A 106.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 117.2(6) . . ? C9 C8 P1 113.2(5) . . ? C10 C8 P1 110.3(4) . . ? C9 C8 H8A 104.9 . . ? C10 C8 H8A 104.9 . . ? P1 C8 H8A 104.9 . . ? C9D C8D C10D 107.8(12) . . ? C9D C8D P1 110.2(11) . . ? C10D C8D P1 111.6(10) . . ? C9D C8D H8DA 109.1 . . ? C10D C8D H8DA 109.1 . . ? P1 C8D H8DA 109.1 . . ? C8D C9D H9DA 109.5 . . ? C8D C9D H9DB 109.5 . . ? H9DA C9D H9DB 109.5 . . ? C8D C9D H9DC 109.5 . . ? H9DA C9D H9DC 109.5 . . ? H9DB C9D H9DC 109.5 . . ? C8D C10D H10D 109.5 . . ? C8D C10D H10E 109.5 . . ? H10D C10D H10E 109.5 . . ? C8D C10D H10F 109.5 . . ? H10D C10D H10F 109.5 . . ? H10E C10D H10F 109.5 . . ? C13 C11 C12 111.4(3) . . ? C13 C11 P2 114.3(3) . . ? C12 C11 P2 110.1(3) . . ? C13 C11 H11A 106.8 . . ? C12 C11 H11A 106.8 . . ? P2 C11 H11A 106.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 117.6(7) . . ? C15 C14 P2 115.6(4) . . ? C16 C14 P2 111.7(5) . . ? C15 C14 H14A 103.1 . . ? C16 C14 H14A 103.1 . . ? P2 C14 H14A 103.1 . . ? C16D C14D C15D 112.1(11) . . ? C16D C14D P2 116.5(10) . . ? C15D C14D P2 110.8(10) . . ? C16D C14D H14B 105.5 . . ? C15D C14D H14B 105.5 . . ? P2 C14D H14B 105.5 . . ? C14D C15D H15D 109.5 . . ? C14D C15D H15E 109.5 . . ? H15D C15D H15E 109.5 . . ? C14D C15D H15F 109.5 . . ? H15D C15D H15F 109.5 . . ? H15E C15D H15F 109.5 . . ? C14D C16D H16D 109.5 . . ? C14D C16D H16E 109.5 . . ? H16D C16D H16E 109.5 . . ? C14D C16D H16F 109.5 . . ? H16D C16D H16F 109.5 . . ? H16E C16D H16F 109.5 . . ? C22 C17 C18 116.7(3) . . ? C22 C17 B2 119.9(3) . . ? C18 C17 B2 123.3(3) . . ? C19 C18 C17 120.5(3) . . ? C19 C18 C23 118.2(3) . . ? C17 C18 C23 121.2(3) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C23 C18 H18A 2.7 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? C20 C19 C18 122.7(3) . . ? C20 C19 C23D 119.9(5) . . ? C18 C19 C23D 117.0(5) . . ? C20 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? C23D C19 H19A 5.8 . . ? C19 C23D H23D 109.5 . . ? C19 C23D H23E 109.5 . . ? H23D C23D H23E 109.5 . . ? C19 C23D H23F 109.5 . . ? H23D C23D H23F 109.5 . . ? H23E C23D H23F 109.5 . . ? C19 C20 C21 116.2(3) . . ? C19 C20 B4 124.1(3) . . ? C21 C20 B4 119.8(3) . . ? C22 C21 C20 121.7(3) . . ? C22 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C21 C22 C17 122.2(3) . . ? C21 C22 H22A 118.9 . . ? C17 C22 H22A 118.9 . . ? C27 C24 C25 108.5(3) . . ? C27 C24 C26 107.9(3) . . ? C25 C24 C26 106.2(3) . . ? C27 C24 B3 109.8(3) . . ? C25 C24 B3 112.2(3) . . ? C26 C24 B3 112.1(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 113.4(3) . . ? C29 C28 P3 112.7(2) . . ? C30 C28 P3 111.6(3) . . ? C29 C28 H28A 106.2 . . ? C30 C28 H28A 106.2 . . ? P3 C28 H28A 106.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C33 111.7(3) . . ? C32 C31 P3 111.0(3) . . ? C33 C31 P3 113.8(2) . . ? C32 C31 H31A 106.6 . . ? C33 C31 H31A 106.6 . . ? P3 C31 H31A 106.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C36 113.6(3) . . ? C35 C34 P4 114.7(3) . . ? C36 C34 P4 113.2(2) . . ? C35 C34 H34A 104.7 . . ? C36 C34 H34A 104.7 . . ? P4 C34 H34A 104.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 110.6(3) . . ? C39 C37 P4 115.2(2) . . ? C38 C37 P4 112.8(2) . . ? C39 C37 H37A 105.8 . . ? C38 C37 H37A 105.8 . . ? P4 C37 H37A 105.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 C11 P2 B1 C1 44.7(3) . . . . ? C14 P2 B1 C1 -104.0(4) . . . . ? C14D P2 B1 C1 -85.8(6) . . . . ? B2 P2 B1 C1 142.0(3) . . . . ? C11 P2 B1 B2 -97.3(2) . . . . ? C14 P2 B1 B2 113.9(4) . . . . ? C14D P2 B1 B2 132.1(5) . . . . ? C11 P2 B1 P1 -144.98(16) . . . . ? C14 P2 B1 P1 66.2(4) . . . . ? C14D P2 B1 P1 84.5(5) . . . . ? B2 P2 B1 P1 -47.66(15) . . . . ? C5 P1 B1 C1 -41.6(3) . . . . ? C8 P1 B1 C1 107.3(4) . . . . ? B2 P1 B1 C1 -141.7(3) . . . . ? C8D P1 B1 C1 89.7(6) . . . . ? C5 P1 B1 B2 100.15(19) . . . . ? C8 P1 B1 B2 -111.0(3) . . . . ? C8D P1 B1 B2 -128.6(6) . . . . ? C5 P1 B1 P2 148.21(15) . . . . ? C8 P1 B1 P2 -62.9(3) . . . . ? B2 P1 B1 P2 48.06(15) . . . . ? C8D P1 B1 P2 -80.5(6) . . . . ? C5 P1 B2 C17 24.8(4) . . . . ? C8 P1 B2 C17 -114.9(4) . . . . ? C8D P1 B2 C17 -101.3(6) . . . . ? B1 P1 B2 C17 132.0(4) . . . . ? C5 P1 B2 B1 -107.14(18) . . . . ? C8 P1 B2 B1 113.2(3) . . . . ? C8D P1 B2 B1 126.7(5) . . . . ? C5 P1 B2 P2 -156.03(15) . . . . ? C8 P1 B2 P2 64.3(3) . . . . ? C8D P1 B2 P2 77.8(6) . . . . ? B1 P1 B2 P2 -48.89(15) . . . . ? C1 B1 B2 C17 -4.4(8) . . . . ? P2 B1 B2 C17 114.7(4) . . . . ? P1 B1 B2 C17 -123.8(4) . . . . ? C1 B1 B2 P1 119.4(5) . . . . ? P2 B1 B2 P1 -121.46(15) . . . . ? C1 B1 B2 P2 -119.1(5) . . . . ? P1 B1 B2 P2 121.46(15) . . . . ? C11 P2 B2 C17 -22.8(3) . . . . ? C14 P2 B2 C17 103.2(4) . . . . ? C14D P2 B2 C17 111.2(7) . . . . ? B1 P2 B2 C17 -131.6(3) . . . . ? C11 P2 B2 P1 158.01(16) . . . . ? C14 P2 B2 P1 -76.0(4) . . . . ? C14D P2 B2 P1 -68.0(7) . . . . ? B1 P2 B2 P1 49.22(15) . . . . ? C11 P2 B2 B1 108.79(19) . . . . ? C14 P2 B2 B1 -125.2(4) . . . . ? C14D P2 B2 B1 -117.2(7) . . . . ? C37 P4 B3 C24 43.6(3) . . . . ? C34 P4 B3 C24 -102.0(3) . . . . ? B4 P4 B3 C24 142.1(3) . . . . ? C37 P4 B3 B4 -98.42(18) . . . . ? C34 P4 B3 B4 115.96(19) . . . . ? C37 P4 B3 P3 -146.79(14) . . . . ? C34 P4 B3 P3 67.6(2) . . . . ? B4 P4 B3 P3 -48.37(14) . . . . ? C31 P3 B3 C24 -42.0(3) . . . . ? B4 P3 B3 C24 -141.6(3) . . . . ? C28 P3 B3 C24 98.7(3) . . . . ? C31 P3 B3 B4 99.64(18) . . . . ? C28 P3 B3 B4 -119.6(2) . . . . ? C31 P3 B3 P4 148.26(15) . . . . ? B4 P3 B3 P4 48.63(14) . . . . ? C28 P3 B3 P4 -71.0(2) . . . . ? C24 B3 B4 C20 -1.9(7) . . . . ? P4 B3 B4 C20 119.1(4) . . . . ? P3 B3 B4 C20 -120.3(4) . . . . ? C24 B3 B4 P3 118.4(5) . . . . ? P4 B3 B4 P3 -120.57(14) . . . . ? C24 B3 B4 P4 -121.0(5) . . . . ? P3 B3 B4 P4 120.57(14) . . . . ? C31 P3 B4 C20 24.9(3) . . . . ? C28 P3 B4 C20 -105.3(3) . . . . ? B3 P3 B4 C20 132.2(3) . . . . ? C31 P3 B4 B3 -107.30(17) . . . . ? C28 P3 B4 B3 122.4(2) . . . . ? C31 P3 B4 P4 -156.92(15) . . . . ? C28 P3 B4 P4 72.8(2) . . . . ? B3 P3 B4 P4 -49.63(14) . . . . ? C37 P4 B4 C20 -23.5(3) . . . . ? C34 P4 B4 C20 114.1(3) . . . . ? B3 P4 B4 C20 -132.1(3) . . . . ? C37 P4 B4 B3 108.56(17) . . . . ? C34 P4 B4 B3 -113.87(19) . . . . ? C37 P4 B4 P3 158.33(14) . . . . ? C34 P4 B4 P3 -64.1(2) . . . . ? B3 P4 B4 P3 49.78(15) . . . . ? B2 B1 C1 C2 -62.1(6) . . . . ? P2 B1 C1 C2 -158.7(3) . . . . ? P1 B1 C1 C2 34.2(4) . . . . ? B2 B1 C1 C4 176.9(4) . . . . ? P2 B1 C1 C4 80.3(4) . . . . ? P1 B1 C1 C4 -86.9(3) . . . . ? B2 B1 C1 C3 57.6(6) . . . . ? P2 B1 C1 C3 -38.9(4) . . . . ? P1 B1 C1 C3 153.9(3) . . . . ? C8 P1 C5 C6 76.8(3) . . . . ? B2 P1 C5 C6 -66.4(3) . . . . ? C8D P1 C5 C6 80.2(4) . . . . ? B1 P1 C5 C6 -131.4(3) . . . . ? C8 P1 C5 C7 -50.9(4) . . . . ? B2 P1 C5 C7 165.9(3) . . . . ? C8D P1 C5 C7 -47.4(5) . . . . ? B1 P1 C5 C7 101.0(3) . . . . ? C5 P1 C8 C9 -56.8(7) . . . . ? B2 P1 C8 C9 81.4(7) . . . . ? C8D P1 C8 C9 -68.0(15) . . . . ? B1 P1 C8 C9 154.4(6) . . . . ? C5 P1 C8 C10 76.8(6) . . . . ? B2 P1 C8 C10 -145.0(5) . . . . ? C8D P1 C8 C10 65.6(14) . . . . ? B1 P1 C8 C10 -72.0(7) . . . . ? C5 P1 C8D C9D -109.8(10) . . . . ? C8 P1 C8D C9D 59.9(15) . . . . ? B2 P1 C8D C9D 20.5(13) . . . . ? B1 P1 C8D C9D 113.7(10) . . . . ? C5 P1 C8D C10D 130.5(9) . . . . ? C8 P1 C8D C10D -59.8(14) . . . . ? B2 P1 C8D C10D -99.2(10) . . . . ? B1 P1 C8D C10D -6.0(13) . . . . ? C14 P2 C11 C13 59.2(4) . . . . ? C14D P2 C11 C13 45.3(5) . . . . ? B2 P2 C11 C13 -162.5(3) . . . . ? B1 P2 C11 C13 -98.3(3) . . . . ? C14 P2 C11 C12 -67.1(4) . . . . ? C14D P2 C11 C12 -81.0(5) . . . . ? B2 P2 C11 C12 71.1(3) . . . . ? B1 P2 C11 C12 135.3(3) . . . . ? C11 P2 C14 C15 104.4(6) . . . . ? C14D P2 C14 C15 178(3) . . . . ? B2 P2 C14 C15 -23.0(8) . . . . ? B1 P2 C14 C15 -104.7(6) . . . . ? C11 P2 C14 C16 -117.5(6) . . . . ? C14D P2 C14 C16 -44(2) . . . . ? B2 P2 C14 C16 115.1(5) . . . . ? B1 P2 C14 C16 33.4(8) . . . . ? C11 P2 C14D C16D -105.9(11) . . . . ? C14 P2 C14D C16D 145(3) . . . . ? B2 P2 C14D C16D 118.0(10) . . . . ? B1 P2 C14D C16D 29.7(13) . . . . ? C11 P2 C14D C15D 124.4(11) . . . . ? C14 P2 C14D C15D 15(2) . . . . ? B2 P2 C14D C15D -11.6(15) . . . . ? B1 P2 C14D C15D -100.0(11) . . . . ? P1 B2 C17 C22 -96.5(4) . . . . ? B1 B2 C17 C22 -2.3(6) . . . . ? P2 B2 C17 C22 84.5(4) . . . . ? P1 B2 C17 C18 87.2(4) . . . . ? B1 B2 C17 C18 -178.5(4) . . . . ? P2 B2 C17 C18 -91.7(4) . . . . ? C22 C17 C18 C19 -1.4(5) . . . . ? B2 C17 C18 C19 174.9(3) . . . . ? C22 C17 C18 C23 176.0(5) . . . . ? B2 C17 C18 C23 -7.6(6) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C23 C18 C19 C20 -176.7(5) . . . . ? C17 C18 C19 C23D -172.9(5) . . . . ? C23 C18 C19 C23D 9.6(7) . . . . ? C18 C19 C20 C21 0.2(5) . . . . ? C23D C19 C20 C21 173.7(5) . . . . ? C18 C19 C20 B4 179.7(3) . . . . ? C23D C19 C20 B4 -6.8(7) . . . . ? B3 B4 C20 C19 172.7(3) . . . . ? P3 B4 C20 C19 80.9(4) . . . . ? P4 B4 C20 C19 -96.7(4) . . . . ? B3 B4 C20 C21 -7.8(5) . . . . ? P3 B4 C20 C21 -99.6(3) . . . . ? P4 B4 C20 C21 82.8(4) . . . . ? C19 C20 C21 C22 -0.4(5) . . . . ? B4 C20 C21 C22 180.0(3) . . . . ? C20 C21 C22 C17 -0.3(5) . . . . ? C18 C17 C22 C21 1.2(5) . . . . ? B2 C17 C22 C21 -175.3(3) . . . . ? B4 B3 C24 C27 -166.0(4) . . . . ? P4 B3 C24 C27 95.9(3) . . . . ? P3 B3 C24 C27 -70.5(3) . . . . ? B4 B3 C24 C25 -45.2(6) . . . . ? P4 B3 C24 C25 -143.3(3) . . . . ? P3 B3 C24 C25 50.3(4) . . . . ? B4 B3 C24 C26 74.1(5) . . . . ? P4 B3 C24 C26 -24.0(4) . . . . ? P3 B3 C24 C26 169.7(2) . . . . ? C31 P3 C28 C29 -111.9(3) . . . . ? B4 P3 C28 C29 20.7(4) . . . . ? B3 P3 C28 C29 104.4(3) . . . . ? C31 P3 C28 C30 119.2(3) . . . . ? B4 P3 C28 C30 -108.3(3) . . . . ? B3 P3 C28 C30 -24.5(4) . . . . ? B4 P3 C31 C32 -76.7(3) . . . . ? C28 P3 C31 C32 67.2(3) . . . . ? B3 P3 C31 C32 -141.2(2) . . . . ? B4 P3 C31 C33 156.3(3) . . . . ? C28 P3 C31 C33 -59.9(3) . . . . ? B3 P3 C31 C33 91.7(3) . . . . ? C37 P4 C34 C35 52.7(3) . . . . ? B4 P4 C34 C35 -84.5(4) . . . . ? B3 P4 C34 C35 -160.3(3) . . . . ? C37 P4 C34 C36 -79.9(3) . . . . ? B4 P4 C34 C36 143.0(3) . . . . ? B3 P4 C34 C36 67.1(3) . . . . ? C34 P4 C37 C39 49.2(3) . . . . ? B4 P4 C37 C39 -165.8(2) . . . . ? B3 P4 C37 C39 -101.5(3) . . . . ? C34 P4 C37 C38 -79.0(3) . . . . ? B4 P4 C37 C38 65.9(3) . . . . ? B3 P4 C37 C38 130.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.495 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.058 data_gb367i2a _database_code_depnum_ccdc_archive 'CCDC 680338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 B2 P2' _chemical_formula_weight 440.17 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' B B 0.0013 0.0007 '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 Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 23.670(16) _cell_length_b 8.918(6) _cell_length_c 25.608(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.142(19) _cell_angle_gamma 90.00 _cell_volume 5406(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.73 _exptl_crystal_description 'thin plate' _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9731 _exptl_absorpt_correction_T_max 0.9966 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5367 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 20.18 _reflns_number_total 2421 _reflns_number_gt 1731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0454P)^2^+4.3391P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2421 _refine_ls_number_parameters 377 _refine_ls_number_restraints 421 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.000 _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 0.06386(9) 0.14795(19) 0.36268(7) 0.0409(6) Uani 1 1 d D . . P2 P 0.18289(9) 0.14641(18) 0.36808(7) 0.0351(5) Uani 1 1 d D . . B1 B 0.1210(5) 0.0324(7) 0.3944(2) 0.033(2) Uani 1 1 d D A . B2 B 0.1264(4) 0.0884(7) 0.3227(2) 0.038(2) Uani 1 1 d D A . C1 C 0.1316(4) 0.0302(6) 0.2644(2) 0.043(2) Uani 1 1 d U . . C2 C 0.1142(3) 0.1115(6) 0.2233(2) 0.0408(19) Uani 1 1 d U B . H2 H 0.0963 0.2048 0.2299 0.049 Uiso 1 1 calc R . . C3 C 0.1210(4) 0.0664(7) 0.1699(2) 0.0408(17) Uani 1 1 d U . . C4 C 0.1034(3) 0.1529(8) 0.1282(3) 0.061(2) Uani 1 1 d U B . H4 H 0.0848 0.2454 0.1346 0.073 Uiso 1 1 calc R . . C5 C 0.1123(5) 0.1073(8) 0.0776(3) 0.073(3) Uani 1 1 d U . . H5 H 0.1000 0.1687 0.0494 0.087 Uiso 1 1 calc R B . C6 C 0.1386(5) -0.0255(10) 0.0675(3) 0.089(4) Uani 1 1 d U B . H6 H 0.1434 -0.0568 0.0324 0.106 Uiso 1 1 calc R . . C7 C 0.1580(4) -0.1132(9) 0.1065(3) 0.081(3) Uani 1 1 d U . . H7 H 0.1776 -0.2033 0.0985 0.097 Uiso 1 1 calc R B . C8 C 0.1493(4) -0.0713(8) 0.1605(3) 0.060(3) Uani 1 1 d U B . C9 C 0.1675(4) -0.1570(8) 0.2023(3) 0.077(3) Uani 1 1 d U . . H9 H 0.1858 -0.2501 0.1962 0.093 Uiso 1 1 calc R B . C10 C 0.1594(4) -0.1090(7) 0.2523(3) 0.061(2) Uani 1 1 d U B . H10 H 0.1726 -0.1698 0.2803 0.073 Uiso 1 1 calc R . . C11 C 0.1170(5) -0.1015(11) 0.4345(4) 0.036(5) Uani 0.532(14) 1 d PDU A 1 C12 C 0.0556(6) -0.1400(19) 0.4452(6) 0.048(5) Uani 0.532(14) 1 d PDU A 1 H12A H 0.0383 -0.1811 0.4135 0.071 Uiso 0.532(14) 1 calc PR A 1 H12B H 0.0353 -0.0492 0.4557 0.071 Uiso 0.532(14) 1 calc PR A 1 H12C H 0.0536 -0.2144 0.4733 0.071 Uiso 0.532(14) 1 calc PR A 1 C13 C 0.1513(7) -0.2342(13) 0.4151(5) 0.045(5) Uani 0.532(14) 1 d PDU A 1 H13A H 0.1500 -0.3151 0.4409 0.067 Uiso 0.532(14) 1 calc PR A 1 H13B H 0.1906 -0.2032 0.4098 0.067 Uiso 0.532(14) 1 calc PR A 1 H13C H 0.1355 -0.2699 0.3819 0.067 Uiso 0.532(14) 1 calc PR A 1 C14 C 0.1443(10) -0.0351(16) 0.4831(5) 0.050(6) Uani 0.532(14) 1 d PDU A 1 H14A H 0.1508 -0.1146 0.5088 0.075 Uiso 0.532(14) 1 calc PR A 1 H14B H 0.1193 0.0411 0.4980 0.075 Uiso 0.532(14) 1 calc PR A 1 H14C H 0.1805 0.0111 0.4738 0.075 Uiso 0.532(14) 1 calc PR A 1 C11D C 0.1183(6) -0.0838(14) 0.4408(5) 0.049(6) Uani 0.468(14) 1 d PDU A 2 C12D C 0.0794(11) -0.227(2) 0.4320(7) 0.063(6) Uani 0.468(14) 1 d PDU A 2 H12D H 0.0402 -0.2015 0.4408 0.094 Uiso 0.468(14) 1 calc PR A 2 H12E H 0.0925 -0.3087 0.4544 0.094 Uiso 0.468(14) 1 calc PR A 2 H12F H 0.0814 -0.2576 0.3953 0.094 Uiso 0.468(14) 1 calc PR A 2 C13D C 0.1770(7) -0.1609(17) 0.4546(6) 0.052(6) Uani 0.468(14) 1 d PDU A 2 H13D H 0.1710 -0.2397 0.4807 0.078 Uiso 0.468(14) 1 calc PR A 2 H13E H 0.2030 -0.0855 0.4687 0.078 Uiso 0.468(14) 1 calc PR A 2 H13F H 0.1932 -0.2051 0.4229 0.078 Uiso 0.468(14) 1 calc PR A 2 C14D C 0.0988(10) -0.0259(19) 0.4966(5) 0.044(5) Uani 0.468(14) 1 d PDU A 2 H14D H 0.0588 0.0024 0.4951 0.067 Uiso 0.468(14) 1 calc PR A 2 H14E H 0.1214 0.0615 0.5066 0.067 Uiso 0.468(14) 1 calc PR A 2 H14F H 0.1040 -0.1059 0.5224 0.067 Uiso 0.468(14) 1 calc PR A 2 C15 C 0.2482(3) 0.0399(8) 0.3546(3) 0.040(2) Uani 1 1 d DU B . H15 H 0.2367 -0.0667 0.3488 0.048 Uiso 1 1 calc R . . C16 C 0.2773(4) 0.0927(8) 0.3042(3) 0.054(2) Uani 1 1 d U . . H16A H 0.2908 0.1957 0.3088 0.081 Uiso 1 1 calc R B . H16B H 0.2503 0.0890 0.2752 0.081 Uiso 1 1 calc R . . H16C H 0.3094 0.0269 0.2966 0.081 Uiso 1 1 calc R . . C17 C 0.2908(4) 0.0394(10) 0.3997(3) 0.070(3) Uani 1 1 d U . . H17A H 0.3251 -0.0135 0.3890 0.104 Uiso 1 1 calc R B . H17B H 0.2742 -0.0115 0.4300 0.104 Uiso 1 1 calc R . . H17C H 0.3003 0.1429 0.4092 0.104 Uiso 1 1 calc R . . C18 C 0.2130(6) 0.3332(8) 0.3844(3) 0.034(3) Uani 0.747(17) 1 d PDU B 1 H18 H 0.2551 0.3241 0.3823 0.041 Uiso 0.747(17) 1 calc PR B 1 C19 C 0.1948(8) 0.4544(12) 0.3445(4) 0.051(5) Uani 0.747(17) 1 d PDU B 1 H19A H 0.1542 0.4725 0.3477 0.077 Uiso 0.747(17) 1 calc PR B 1 H19B H 0.2034 0.4199 0.3091 0.077 Uiso 0.747(17) 1 calc PR B 1 H19C H 0.2154 0.5476 0.3516 0.077 Uiso 0.747(17) 1 calc PR B 1 C20 C 0.1985(8) 0.3818(13) 0.4409(4) 0.064(4) Uani 0.747(17) 1 d PDU B 1 H20A H 0.2127 0.4835 0.4471 0.096 Uiso 0.747(17) 1 calc PR B 1 H20B H 0.2162 0.3125 0.4657 0.096 Uiso 0.747(17) 1 calc PR B 1 H20C H 0.1574 0.3802 0.4456 0.096 Uiso 0.747(17) 1 calc PR B 1 C18D C 0.1864(13) 0.3472(13) 0.3873(9) 0.030(10) Uiso 0.253(17) 1 d PDU B 2 H18D H 0.1471 0.3885 0.3884 0.036 Uiso 0.253(17) 1 calc PR B 2 C19D C 0.2207(16) 0.435(4) 0.3461(10) 0.025(11) Uiso 0.253(17) 1 d PDU B 2 H19D H 0.2085 0.5403 0.3459 0.038 Uiso 0.253(17) 1 calc PR B 2 H19E H 0.2144 0.3913 0.3115 0.038 Uiso 0.253(17) 1 calc PR B 2 H19F H 0.2610 0.4303 0.3548 0.038 Uiso 0.253(17) 1 calc PR B 2 C20D C 0.2133(14) 0.362(3) 0.4421(8) 0.008(8) Uiso 0.253(17) 1 d PDU B 2 H20D H 0.2530 0.3316 0.4406 0.011 Uiso 0.253(17) 1 calc PR B 2 H20E H 0.1931 0.2982 0.4668 0.011 Uiso 0.253(17) 1 calc PR B 2 H20F H 0.2110 0.4670 0.4536 0.011 Uiso 0.253(17) 1 calc PR B 2 C21 C 0.0479(8) 0.3459(10) 0.3803(4) 0.038(4) Uani 0.661(13) 1 d PDU C 1 H21 H 0.0838 0.3927 0.3930 0.046 Uiso 0.661(13) 1 calc PR C 1 C22 C 0.0240(7) 0.4468(13) 0.3366(4) 0.042(4) Uani 0.661(13) 1 d PDU C 1 H22A H -0.0138 0.4121 0.3269 0.063 Uiso 0.661(13) 1 calc PR C 1 H22B H 0.0489 0.4419 0.3061 0.063 Uiso 0.661(13) 1 calc PR C 1 H22C H 0.0219 0.5505 0.3491 0.063 Uiso 0.661(13) 1 calc PR C 1 C23 C 0.0054(6) 0.3455(13) 0.4266(4) 0.064(4) Uani 0.661(13) 1 d PDU C 1 H23A H 0.0007 0.4479 0.4398 0.096 Uiso 0.661(13) 1 calc PR C 1 H23B H 0.0198 0.2811 0.4546 0.096 Uiso 0.661(13) 1 calc PR C 1 H23C H -0.0312 0.3073 0.4146 0.096 Uiso 0.661(13) 1 calc PR C 1 C21D C 0.0275(11) 0.3247(15) 0.3816(6) 0.029(9) Uiso 0.339(13) 1 d PDU C 2 H21D H -0.0142 0.3102 0.3780 0.035 Uiso 0.339(13) 1 calc PR C 2 C22D C 0.0472(11) 0.441(2) 0.3411(6) 0.030(9) Uiso 0.339(13) 1 d PDU C 2 H22D H 0.0336 0.5407 0.3513 0.044 Uiso 0.339(13) 1 calc PR C 2 H22E H 0.0319 0.4150 0.3067 0.044 Uiso 0.339(13) 1 calc PR C 2 H22F H 0.0885 0.4418 0.3397 0.044 Uiso 0.339(13) 1 calc PR C 2 C23D C 0.0406(9) 0.3820(16) 0.4374(5) 0.017(6) Uiso 0.339(13) 1 d PDU C 2 H23D H 0.0811 0.4028 0.4406 0.025 Uiso 0.339(13) 1 calc PR C 2 H23E H 0.0297 0.3055 0.4629 0.025 Uiso 0.339(13) 1 calc PR C 2 H23F H 0.0192 0.4741 0.4440 0.025 Uiso 0.339(13) 1 calc PR C 2 C24 C -0.0007(8) 0.031(3) 0.3562(8) 0.048(7) Uani 0.500(10) 1 d PDU C 1 H24 H 0.0107 -0.0759 0.3518 0.058 Uiso 0.500(10) 1 calc PR C 1 C25 C -0.0456(7) 0.041(2) 0.3992(6) 0.070(6) Uani 0.500(10) 1 d PDU C 1 H25A H -0.0574 0.1459 0.4034 0.104 Uiso 0.500(10) 1 calc PR C 1 H25B H -0.0297 0.0045 0.4322 0.104 Uiso 0.500(10) 1 calc PR C 1 H25C H -0.0783 -0.0200 0.3895 0.104 Uiso 0.500(10) 1 calc PR C 1 C26 C -0.0287(19) 0.086(4) 0.3057(12) 0.059(8) Uani 0.500(10) 1 d PDU C 1 H26A H -0.0616 0.0231 0.2979 0.088 Uiso 0.500(10) 1 calc PR C 1 H26B H -0.0016 0.0793 0.2769 0.088 Uiso 0.500(10) 1 calc PR C 1 H26C H -0.0408 0.1903 0.3100 0.088 Uiso 0.500(10) 1 calc PR C 1 C24D C 0.0005(6) 0.044(2) 0.3400(10) 0.029(6) Uani 0.500(10) 1 d PDU C 2 H24D H -0.0201 0.0143 0.3724 0.035 Uiso 0.500(10) 1 calc PR C 2 C25D C -0.044(2) 0.122(4) 0.3054(16) 0.064(9) Uani 0.500(10) 1 d PDU C 2 H25D H -0.0247 0.1713 0.2761 0.096 Uiso 0.500(10) 1 calc PR C 2 H25E H -0.0641 0.1965 0.3260 0.096 Uiso 0.500(10) 1 calc PR C 2 H25F H -0.0703 0.0469 0.2919 0.096 Uiso 0.500(10) 1 calc PR C 2 C26D C 0.0165(6) -0.1025(12) 0.3130(5) 0.041(4) Uani 0.500(10) 1 d PDU C 2 H26D H -0.0175 -0.1629 0.3073 0.061 Uiso 0.500(10) 1 calc PR C 2 H26E H 0.0431 -0.1581 0.3351 0.061 Uiso 0.500(10) 1 calc PR C 2 H26F H 0.0342 -0.0804 0.2793 0.061 Uiso 0.500(10) 1 calc PR C 2 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 0.0451(16) 0.0303(10) 0.0474(12) -0.0053(10) -0.0076(11) 0.0022(10) P2 0.0455(16) 0.0299(10) 0.0298(10) 0.0005(9) -0.0019(11) -0.0061(10) B1 0.038(6) 0.029(4) 0.032(4) -0.003(3) 0.015(5) 0.000(5) B2 0.049(7) 0.034(4) 0.031(4) -0.003(3) -0.005(5) -0.002(5) C1 0.047(6) 0.033(4) 0.050(4) -0.011(3) -0.012(4) 0.000(4) C2 0.037(6) 0.035(4) 0.050(4) -0.006(3) 0.003(4) 0.001(4) C3 0.041(5) 0.040(4) 0.042(3) -0.015(3) 0.003(4) -0.013(4) C4 0.094(8) 0.048(4) 0.041(4) -0.007(4) 0.001(4) -0.018(4) C5 0.106(9) 0.068(5) 0.044(4) 0.001(4) 0.008(5) -0.028(5) C6 0.140(12) 0.080(6) 0.047(4) -0.012(4) 0.021(6) -0.022(6) C7 0.123(10) 0.054(5) 0.067(5) -0.027(4) 0.013(5) 0.002(5) C8 0.088(8) 0.041(4) 0.052(4) -0.012(3) 0.002(4) -0.005(4) C9 0.107(9) 0.049(5) 0.076(5) -0.029(4) -0.006(5) 0.018(5) C10 0.094(8) 0.030(4) 0.059(4) -0.018(4) -0.018(4) 0.004(4) C11 0.046(10) 0.011(9) 0.051(10) 0.010(7) -0.001(9) 0.001(9) C12 0.054(9) 0.044(11) 0.045(10) 0.038(9) 0.021(7) 0.000(8) C13 0.072(11) 0.014(7) 0.049(9) 0.013(6) 0.009(8) 0.011(7) C14 0.088(15) 0.042(9) 0.021(8) 0.021(6) -0.005(9) -0.002(10) C11D 0.049(12) 0.059(13) 0.038(12) -0.012(12) 0.011(12) -0.010(10) C12D 0.092(16) 0.044(12) 0.052(11) 0.016(9) -0.016(12) -0.017(12) C13D 0.063(11) 0.048(10) 0.047(11) 0.006(9) 0.031(8) 0.003(8) C14D 0.035(13) 0.064(12) 0.035(9) 0.006(7) 0.021(9) -0.002(9) C15 0.036(6) 0.046(4) 0.039(4) -0.002(4) 0.000(4) -0.007(4) C16 0.060(7) 0.053(5) 0.049(4) -0.001(4) 0.028(4) -0.002(4) C17 0.056(8) 0.088(6) 0.064(5) 0.004(5) -0.019(5) 0.003(5) C18 0.030(10) 0.043(6) 0.031(6) -0.002(4) 0.006(5) -0.015(5) C19 0.079(15) 0.031(6) 0.045(6) -0.002(4) 0.017(7) -0.017(8) C20 0.090(10) 0.053(6) 0.048(5) 0.000(4) 0.013(5) 0.030(6) C21 0.048(12) 0.043(7) 0.023(6) 0.016(5) 0.014(5) -0.008(7) C22 0.027(11) 0.039(8) 0.060(7) -0.005(5) -0.014(7) 0.009(7) C23 0.090(10) 0.053(6) 0.048(5) 0.000(4) 0.013(5) 0.030(6) C24 0.037(14) 0.075(13) 0.033(13) 0.001(11) 0.001(8) -0.003(10) C25 0.031(14) 0.108(14) 0.070(10) -0.045(11) 0.013(9) -0.006(11) C26 0.04(3) 0.071(18) 0.065(11) -0.003(14) -0.018(13) 0.008(15) C24D 0.020(11) 0.035(10) 0.032(13) 0.000(9) -0.005(9) -0.005(8) C25D 0.04(2) 0.081(18) 0.070(13) 0.010(13) -0.019(12) 0.019(13) C26D 0.050(12) 0.029(7) 0.043(9) -0.010(6) -0.002(7) -0.020(6) _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 C24D 1.854(10) . ? P1 C24 1.855(11) . ? P1 C21D 1.860(10) . ? P1 C21 1.861(8) . ? P1 B2 1.878(9) . ? P1 B1 1.883(9) . ? P2 B2 1.844(8) . ? P2 C15 1.849(7) . ? P2 C18D 1.859(9) . ? P2 C18 1.859(7) . ? P2 B1 1.909(10) . ? B1 C11 1.577(9) . ? B1 C11D 1.578(10) . ? B1 B2 1.908(8) . ? B2 C1 1.586(8) . ? C1 C2 1.342(8) . ? C1 C10 1.439(9) . ? C2 C3 1.435(8) . ? C2 H2 0.9500 . ? C3 C4 1.381(8) . ? C3 C8 1.420(9) . ? C4 C5 1.376(9) . ? C4 H4 0.9500 . ? C5 C6 1.363(11) . ? C5 H5 0.9500 . ? C6 C7 1.348(10) . ? C6 H6 0.9500 . ? C7 C8 1.447(9) . ? C7 H7 0.9500 . ? C8 C9 1.384(9) . ? C9 C10 1.365(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.519(10) . ? C11 C13 1.520(10) . ? C11 C14 1.521(10) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C11D C14D 1.588(12) . ? C11D C12D 1.588(12) . ? C11D C13D 1.589(12) . ? C12D H12D 0.9800 . ? C12D H12E 0.9800 . ? C12D H12F 0.9800 . ? C13D H13D 0.9800 . ? C13D H13E 0.9800 . ? C13D H13F 0.9800 . ? C14D H14D 0.9800 . ? C14D H14E 0.9800 . ? C14D H14F 0.9800 . ? C15 C17 1.532(10) . ? C15 C16 1.537(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.547(10) . ? C18 C20 1.550(10) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18D C20D 1.546(11) . ? C18D C19D 1.548(11) . ? C18D H18D 1.0000 . ? C19D H19D 0.9800 . ? C19D H19E 0.9800 . ? C19D H19F 0.9800 . ? C20D H20D 0.9800 . ? C20D H20E 0.9800 . ? C20D H20F 0.9800 . ? C21 C22 1.542(11) . ? C21 C23 1.558(11) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C21D C22D 1.540(12) . ? C21D C23D 1.548(12) . ? C21D H21D 1.0000 . ? C22D H22D 0.9800 . ? C22D H22E 0.9800 . ? C22D H22F 0.9800 . ? C23D H23D 0.9800 . ? C23D H23E 0.9800 . ? C23D H23F 0.9800 . ? C24 C26 1.531(14) . ? C24 C25 1.535(15) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24D C26D 1.528(15) . ? C24D C25D 1.532(14) . ? C24D H24D 1.0000 . ? C25D H25D 0.9800 . ? C25D H25E 0.9800 . ? C25D H25F 0.9800 . ? C26D H26D 0.9800 . ? C26D H26E 0.9800 . ? C26D H26F 0.9800 . ? 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 C24D P1 C24 13.4(13) . . ? C24D P1 C21D 97.5(10) . . ? C24 P1 C21D 96.8(13) . . ? C24D P1 C21 112.6(8) . . ? C24 P1 C21 112.7(11) . . ? C21D P1 C21 16.1(12) . . ? C24D P1 B2 109.0(6) . . ? C24 P1 B2 116.2(8) . . ? C21D P1 B2 138.3(7) . . ? C21 P1 B2 124.1(5) . . ? C24D P1 B1 116.2(8) . . ? C24 P1 B1 108.7(11) . . ? C21D P1 B1 133.1(7) . . ? C21 P1 B1 124.1(6) . . ? B2 P1 B1 61.0(3) . . ? B2 P2 C15 110.1(3) . . ? B2 P2 C18D 118.0(9) . . ? C15 P2 C18D 120.5(10) . . ? B2 P2 C18 132.1(4) . . ? C15 P2 C18 100.5(5) . . ? C18D P2 C18 20.0(11) . . ? B2 P2 B1 61.1(3) . . ? C15 P2 B1 115.8(3) . . ? C18D P2 B1 117.0(10) . . ? C18 P2 B1 133.8(4) . . ? C11 B1 C11D 8.3(9) . . ? C11 B1 P1 130.7(8) . . ? C11D B1 P1 130.9(8) . . ? C11 B1 B2 146.0(6) . . ? C11D B1 B2 154.2(7) . . ? P1 B1 B2 59.4(3) . . ? C11 B1 P2 132.8(8) . . ? C11D B1 P2 130.4(8) . . ? P1 B1 P2 96.1(3) . . ? B2 B1 P2 57.8(4) . . ? C1 B2 P2 128.8(7) . . ? C1 B2 P1 132.0(7) . . ? P2 B2 P1 98.6(3) . . ? C1 B2 B1 145.7(5) . . ? P2 B2 B1 61.1(4) . . ? P1 B2 B1 59.6(4) . . ? C2 C1 C10 115.9(6) . . ? C2 C1 B2 122.5(6) . . ? C10 C1 B2 121.4(6) . . ? C1 C2 C3 124.2(6) . . ? C1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C4 C3 C8 119.6(6) . . ? C4 C3 C2 123.1(6) . . ? C8 C3 C2 117.3(6) . . ? C5 C4 C3 121.1(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 120.4(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 121.3(8) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 120.5(8) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C3 119.5(7) . . ? C9 C8 C7 123.5(7) . . ? C3 C8 C7 117.0(7) . . ? C10 C9 C8 120.6(7) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C1 122.5(7) . . ? C9 C10 H10 118.7 . . ? C1 C10 H10 118.7 . . ? C12 C11 C13 113.3(11) . . ? C12 C11 C14 110.2(13) . . ? C13 C11 C14 110.2(12) . . ? C12 C11 B1 110.3(9) . . ? C13 C11 B1 110.1(8) . . ? C14 C11 B1 102.2(8) . . ? B1 C11D C14D 118.4(10) . . ? B1 C11D C12D 116.3(11) . . ? C14D C11D C12D 102.6(12) . . ? B1 C11D C13D 114.5(10) . . ? C14D C11D C13D 101.4(12) . . ? C12D C11D C13D 101.0(13) . . ? C11D C12D H12D 109.5 . . ? C11D C12D H12E 109.5 . . ? H12D C12D H12E 109.5 . . ? C11D C12D H12F 109.5 . . ? H12D C12D H12F 109.5 . . ? H12E C12D H12F 109.5 . . ? C11D C13D H13D 109.5 . . ? C11D C13D H13E 109.5 . . ? H13D C13D H13E 109.5 . . ? C11D C13D H13F 109.5 . . ? H13D C13D H13F 109.5 . . ? H13E C13D H13F 109.5 . . ? C11D C14D H14D 109.5 . . ? C11D C14D H14E 109.5 . . ? H14D C14D H14E 109.5 . . ? C11D C14D H14F 109.5 . . ? H14D C14D H14F 109.5 . . ? H14E C14D H14F 109.5 . . ? C17 C15 C16 109.8(6) . . ? C17 C15 P2 114.2(5) . . ? C16 C15 P2 112.1(5) . . ? C17 C15 H15 106.8 . . ? C16 C15 H15 106.8 . . ? P2 C15 H15 106.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 111.0(10) . . ? C19 C18 P2 111.8(8) . . ? C20 C18 P2 112.0(8) . . ? C19 C18 H18 107.2 . . ? C20 C18 H18 107.2 . . ? P2 C18 H18 107.2 . . ? C20D C18D C19D 111.0(12) . . ? C20D C18D P2 110.0(17) . . ? C19D C18D P2 109(2) . . ? C20D C18D H18D 108.8 . . ? C19D C18D H18D 108.8 . . ? P2 C18D H18D 108.8 . . ? C18D C19D H19D 109.5 . . ? C18D C19D H19E 109.5 . . ? H19D C19D H19E 109.5 . . ? C18D C19D H19F 109.5 . . ? H19D C19D H19F 109.5 . . ? H19E C19D H19F 109.5 . . ? C18D C20D H20D 109.5 . . ? C18D C20D H20E 109.5 . . ? H20D C20D H20E 109.5 . . ? C18D C20D H20F 109.5 . . ? H20D C20D H20F 109.5 . . ? H20E C20D H20F 109.5 . . ? C22 C21 C23 108.5(11) . . ? C22 C21 P1 116.9(8) . . ? C23 C21 P1 108.3(8) . . ? C22 C21 H21 107.6 . . ? C23 C21 H21 107.6 . . ? P1 C21 H21 107.6 . . ? C22D C21D C23D 109.8(13) . . ? C22D C21D P1 104.8(11) . . ? C23D C21D P1 115.4(12) . . ? C22D C21D H21D 108.9 . . ? C23D C21D H21D 108.9 . . ? P1 C21D H21D 108.9 . . ? C21D C22D H22D 109.5 . . ? C21D C22D H22E 109.5 . . ? H22D C22D H22E 109.5 . . ? C21D C22D H22F 109.5 . . ? H22D C22D H22F 109.5 . . ? H22E C22D H22F 109.5 . . ? C21D C23D H23D 109.5 . . ? C21D C23D H23E 109.5 . . ? H23D C23D H23E 109.5 . . ? C21D C23D H23F 109.5 . . ? H23D C23D H23F 109.5 . . ? H23E C23D H23F 109.5 . . ? C26 C24 C25 106.8(16) . . ? C26 C24 P1 105(3) . . ? C25 C24 P1 118.3(13) . . ? C26 C24 H24 108.9 . . ? C25 C24 H24 108.9 . . ? P1 C24 H24 108.9 . . ? C26D C24D C25D 107.1(16) . . ? C26D C24D P1 111.6(10) . . ? C25D C24D P1 120(3) . . ? C26D C24D H24D 105.6 . . ? C25D C24D H24D 105.6 . . ? P1 C24D H24D 105.6 . . ? C24D C25D H25D 109.5 . . ? C24D C25D H25E 109.5 . . ? H25D C25D H25E 109.5 . . ? C24D C25D H25F 109.5 . . ? H25D C25D H25F 109.5 . . ? H25E C25D H25F 109.5 . . ? C24D C26D H26D 109.5 . . ? C24D C26D H26E 109.5 . . ? H26D C26D H26E 109.5 . . ? C24D C26D H26F 109.5 . . ? H26D C26D H26F 109.5 . . ? H26E C26D H26F 109.5 . . ? 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 C24D P1 B1 C11 -41.4(11) . . . . ? C24 P1 B1 C11 -29.4(10) . . . . ? C21D P1 B1 C11 89.8(13) . . . . ? C21 P1 B1 C11 106.9(9) . . . . ? B2 P1 B1 C11 -139.6(8) . . . . ? C24D P1 B1 C11D -52.4(12) . . . . ? C24 P1 B1 C11D -40.4(11) . . . . ? C21D P1 B1 C11D 78.8(14) . . . . ? C21 P1 B1 C11D 95.9(11) . . . . ? B2 P1 B1 C11D -150.6(10) . . . . ? C24D P1 B1 B2 98.2(9) . . . . ? C24 P1 B1 B2 110.2(7) . . . . ? C21D P1 B1 B2 -130.6(10) . . . . ? C21 P1 B1 B2 -113.5(6) . . . . ? C24D P1 B1 P2 144.8(8) . . . . ? C24 P1 B1 P2 156.9(7) . . . . ? C21D P1 B1 P2 -83.9(10) . . . . ? C21 P1 B1 P2 -66.9(6) . . . . ? B2 P1 B1 P2 46.6(3) . . . . ? B2 P2 B1 C11 138.8(8) . . . . ? C15 P2 B1 C11 39.0(9) . . . . ? C18D P2 B1 C11 -112.6(11) . . . . ? C18 P2 B1 C11 -99.2(10) . . . . ? B2 P2 B1 C11D 149.4(9) . . . . ? C15 P2 B1 C11D 49.6(9) . . . . ? C18D P2 B1 C11D -102.0(12) . . . . ? C18 P2 B1 C11D -88.5(10) . . . . ? B2 P2 B1 P1 -47.7(3) . . . . ? C15 P2 B1 P1 -147.5(3) . . . . ? C18D P2 B1 P1 61.0(9) . . . . ? C18 P2 B1 P1 74.4(6) . . . . ? C15 P2 B1 B2 -99.8(4) . . . . ? C18D P2 B1 B2 108.7(9) . . . . ? C18 P2 B1 B2 122.1(6) . . . . ? C15 P2 B2 C1 -31.0(6) . . . . ? C18D P2 B2 C1 112.8(11) . . . . ? C18 P2 B2 C1 95.3(8) . . . . ? B1 P2 B2 C1 -140.1(6) . . . . ? C15 P2 B2 P1 157.3(3) . . . . ? C18D P2 B2 P1 -58.9(11) . . . . ? C18 P2 B2 P1 -76.3(6) . . . . ? B1 P2 B2 P1 48.2(3) . . . . ? C15 P2 B2 B1 109.1(4) . . . . ? C18D P2 B2 B1 -107.1(10) . . . . ? C18 P2 B2 B1 -124.6(6) . . . . ? C24D P1 B2 C1 29.5(11) . . . . ? C24 P1 B2 C1 41.7(13) . . . . ? C21D P1 B2 C1 -97.0(13) . . . . ? C21 P1 B2 C1 -107.0(8) . . . . ? B1 P1 B2 C1 139.5(7) . . . . ? C24D P1 B2 P2 -159.2(9) . . . . ? C24 P1 B2 P2 -147.0(11) . . . . ? C21D P1 B2 P2 74.3(12) . . . . ? C21 P1 B2 P2 64.3(6) . . . . ? B1 P1 B2 P2 -49.2(3) . . . . ? C24D P1 B2 B1 -110.0(9) . . . . ? C24 P1 B2 B1 -97.8(11) . . . . ? C21D P1 B2 B1 123.5(12) . . . . ? C21 P1 B2 B1 113.5(6) . . . . ? C11 B1 B2 C1 -3(2) . . . . ? C11D B1 B2 C1 0(3) . . . . ? P1 B1 B2 C1 -121.1(14) . . . . ? P2 B1 B2 C1 117.6(14) . . . . ? C11 B1 B2 P2 -120.2(15) . . . . ? C11D B1 B2 P2 -117(2) . . . . ? P1 B1 B2 P2 121.3(3) . . . . ? C11 B1 B2 P1 118.5(16) . . . . ? C11D B1 B2 P1 122(2) . . . . ? P2 B1 B2 P1 -121.3(3) . . . . ? P2 B2 C1 C2 -110.2(9) . . . . ? P1 B2 C1 C2 58.8(10) . . . . ? B1 B2 C1 C2 155.2(12) . . . . ? P2 B2 C1 C10 65.0(9) . . . . ? P1 B2 C1 C10 -126.1(8) . . . . ? B1 B2 C1 C10 -29.6(18) . . . . ? C10 C1 C2 C3 1.1(12) . . . . ? B2 C1 C2 C3 176.5(8) . . . . ? C1 C2 C3 C4 -179.2(8) . . . . ? C1 C2 C3 C8 -1.8(11) . . . . ? C8 C3 C4 C5 0.7(11) . . . . ? C2 C3 C4 C5 178.0(8) . . . . ? C3 C4 C5 C6 0.3(13) . . . . ? C4 C5 C6 C7 -1.9(16) . . . . ? C5 C6 C7 C8 2.5(16) . . . . ? C4 C3 C8 C9 179.3(8) . . . . ? C2 C3 C8 C9 1.8(11) . . . . ? C4 C3 C8 C7 -0.1(11) . . . . ? C2 C3 C8 C7 -177.6(8) . . . . ? C6 C7 C8 C9 179.2(9) . . . . ? C6 C7 C8 C3 -1.5(13) . . . . ? C3 C8 C9 C10 -1.2(12) . . . . ? C7 C8 C9 C10 178.1(8) . . . . ? C8 C9 C10 C1 0.5(13) . . . . ? C2 C1 C10 C9 -0.4(12) . . . . ? B2 C1 C10 C9 -175.8(8) . . . . ? C11D B1 C11 C12 98(6) . . . . ? P1 B1 C11 C12 2.9(14) . . . . ? B2 B1 C11 C12 -91.3(18) . . . . ? P2 B1 C11 C12 174.4(9) . . . . ? C11D B1 C11 C13 -136(6) . . . . ? P1 B1 C11 C13 128.6(9) . . . . ? B2 B1 C11 C13 34(2) . . . . ? P2 B1 C11 C13 -59.8(13) . . . . ? C11D B1 C11 C14 -19(5) . . . . ? P1 B1 C11 C14 -114.3(11) . . . . ? B2 B1 C11 C14 151.5(16) . . . . ? P2 B1 C11 C14 57.3(14) . . . . ? C11 B1 C11D C14D -154(6) . . . . ? P1 B1 C11D C14D -62.0(19) . . . . ? B2 B1 C11D C14D -166.1(19) . . . . ? P2 B1 C11D C14D 95.3(15) . . . . ? C11 B1 C11D C12D -31(5) . . . . ? P1 B1 C11D C12D 61.0(17) . . . . ? B2 B1 C11D C12D -43(3) . . . . ? P2 B1 C11D C12D -141.7(12) . . . . ? C11 B1 C11D C13D 86(5) . . . . ? P1 B1 C11D C13D 178.4(8) . . . . ? B2 B1 C11D C13D 74(3) . . . . ? P2 B1 C11D C13D -24.3(16) . . . . ? B2 P2 C15 C17 -160.8(6) . . . . ? C18D P2 C15 C17 56.5(11) . . . . ? C18 P2 C15 C17 56.6(6) . . . . ? B1 P2 C15 C17 -94.0(6) . . . . ? B2 P2 C15 C16 73.5(6) . . . . ? C18D P2 C15 C16 -69.2(10) . . . . ? C18 P2 C15 C16 -69.0(6) . . . . ? B1 P2 C15 C16 140.3(5) . . . . ? B2 P2 C18 C19 -13.7(14) . . . . ? C15 P2 C18 C19 116.0(11) . . . . ? C18D P2 C18 C19 -64(3) . . . . ? B1 P2 C18 C19 -101.7(10) . . . . ? B2 P2 C18 C20 111.6(10) . . . . ? C15 P2 C18 C20 -118.7(11) . . . . ? C18D P2 C18 C20 61(3) . . . . ? B1 P2 C18 C20 23.7(14) . . . . ? B2 P2 C18D C20D 152.0(16) . . . . ? C15 P2 C18D C20D -68(2) . . . . ? C18 P2 C18D C20D -69(3) . . . . ? B1 P2 C18D C20D 82(2) . . . . ? B2 P2 C18D C19D -85.8(17) . . . . ? C15 P2 C18D C19D 54.2(18) . . . . ? C18 P2 C18D C19D 54(2) . . . . ? B1 P2 C18D C19D -155.6(14) . . . . ? C24D P1 C21 C22 -60.5(16) . . . . ? C24 P1 C21 C22 -75.1(15) . . . . ? C21D P1 C21 C22 -81(3) . . . . ? B2 P1 C21 C22 74.6(15) . . . . ? B1 P1 C21 C22 150.2(11) . . . . ? C24D P1 C21 C23 62.3(15) . . . . ? C24 P1 C21 C23 47.8(15) . . . . ? C21D P1 C21 C23 42(2) . . . . ? B2 P1 C21 C23 -162.5(9) . . . . ? B1 P1 C21 C23 -87.0(13) . . . . ? C24D P1 C21D C22D -110.6(17) . . . . ? C24 P1 C21D C22D -124.1(16) . . . . ? C21 P1 C21D C22D 51(2) . . . . ? B2 P1 C21D C22D 19(2) . . . . ? B1 P1 C21D C22D 112.3(15) . . . . ? C24D P1 C21D C23D 128.5(16) . . . . ? C24 P1 C21D C23D 115.1(16) . . . . ? C21 P1 C21D C23D -70(3) . . . . ? B2 P1 C21D C23D -101.5(13) . . . . ? B1 P1 C21D C23D -9(2) . . . . ? C24D P1 C24 C26 -21(5) . . . . ? C21D P1 C24 C26 73.2(18) . . . . ? C21 P1 C24 C26 71.6(17) . . . . ? B2 P1 C24 C26 -81(2) . . . . ? B1 P1 C24 C26 -146.8(17) . . . . ? C24D P1 C24 C25 -139(8) . . . . ? C21D P1 C24 C25 -45(2) . . . . ? C21 P1 C24 C25 -47(2) . . . . ? B2 P1 C24 C25 160.8(18) . . . . ? B1 P1 C24 C25 95(2) . . . . ? C24 P1 C24D C26D -101(7) . . . . ? C21D P1 C24D C26D 171.1(15) . . . . ? C21 P1 C24D C26D 165.6(12) . . . . ? B2 P1 C24D C26D 23.7(18) . . . . ? B1 P1 C24D C26D -42.5(18) . . . . ? C24 P1 C24D C25D 132(7) . . . . ? C21D P1 C24D C25D 44(2) . . . . ? C21 P1 C24D C25D 39(2) . . . . ? B2 P1 C24D C25D -103(2) . . . . ? B1 P1 C24D C25D -169(2) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 20.18 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.254 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.055