Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bertrand, G.' 'Gornitzka, Heinz' 'Romanenko, Vadim D.' 'Rudzevich, Valentyn L.' _publ_contact_author_name 'Prof G Bertrand' _publ_contact_author_address ; Laboratoire Heterochimie Fondamentale et Appliquee Universite Pau Sabtier M8, route de Narbonne 31062 Toulouse Cedex 4 FRANCE ; _publ_contact_author_email 'GBERTRAN@RAMSES.UPS-TLSE.FR' _publ_section_title ; Formation of the Monoanion [Ar*P(BH3)( -BH2)2H]- with a Symmetrically Bridging Hydride from the Attempted Synthesis of the Dianion [Ar*P(BH3)3]2- ; data_1 _database_code_CSD 167806 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H60 B2 Li O3 P' _chemical_formula_weight 528.31 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' 'Li' 'Li' -0.0003 0.0001 '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' 'O' 'O' 0.0106 0.0060 '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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4853(5) _cell_length_b 11.0044(5) _cell_length_c 32.8968(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3433.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7935 _cell_measurement_theta_min 2.226 _cell_measurement_theta_max 29.236 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.811550 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 18214 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7012 _reflns_number_gt 5840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0672P)^2^+0.5772P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(10) _refine_ls_number_reflns 7012 _refine_ls_number_parameters 470 _refine_ls_number_restraints 344 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.081 _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 0.2383(4) 0.1977(2) 0.10831(10) 0.0461(6) Uani 1 1 d . . . H1A H 0.233(3) 0.179(2) 0.0748(8) 0.049(7) Uiso 1 1 d . . . H1B H 0.151(3) 0.156(3) 0.1230(9) 0.056(8) Uiso 1 1 d . . . H1C H 0.340(3) 0.176(3) 0.1210(10) 0.070(9) Uiso 1 1 d . . . B2 B 0.0906(4) 0.4649(3) 0.07487(9) 0.0470(7) Uani 1 1 d . . . H2A H 0.081(4) 0.560(4) 0.0911(11) 0.097(12) Uiso 1 1 d . . . H2B H 0.139(4) 0.476(4) 0.0475(13) 0.108(14) Uiso 1 1 d . . . H2C H 0.001(3) 0.414(3) 0.0744(9) 0.064(9) Uiso 1 1 d . . . P1 P 0.22912(6) 0.37521(5) 0.108681(17) 0.03323(14) Uani 1 1 d . . . H1 H 0.340(2) 0.3997(18) 0.0896(6) 0.019(5) Uiso 1 1 d . . . C1 C 0.2802(2) 0.44249(18) 0.15842(6) 0.0282(4) Uani 1 1 d . . . C2 C 0.4112(2) 0.5072(2) 0.16217(7) 0.0342(5) Uani 1 1 d . . . C3 C 0.4540(2) 0.5454(2) 0.20048(7) 0.0355(5) Uani 1 1 d . . . H3 H 0.5403 0.5888 0.2026 0.043 Uiso 1 1 calc R . . C4 C 0.3786(2) 0.5240(2) 0.23567(7) 0.0342(5) Uani 1 1 d . A . C5 C 0.2517(2) 0.46515(19) 0.23141(6) 0.0328(5) Uani 1 1 d . . . H5 H 0.1976 0.4502 0.2552 0.039 Uiso 1 1 calc R . . C6 C 0.1972(2) 0.42578(19) 0.19394(6) 0.0290(4) Uani 1 1 d . . . C7 C 0.5137(3) 0.5386(3) 0.12657(8) 0.0505(7) Uani 1 1 d . . . C8 C 0.5886(3) 0.4225(3) 0.11115(9) 0.0689(9) Uani 1 1 d . . . H8A H 0.6347 0.4395 0.0851 0.103 Uiso 1 1 calc R . . H8B H 0.5191 0.3575 0.1075 0.103 Uiso 1 1 calc R . . H8C H 0.6595 0.3969 0.1311 0.103 Uiso 1 1 calc R . . C9 C 0.4384(3) 0.6120(3) 0.09269(8) 0.0597(8) Uani 1 1 d . . . H9A H 0.4180 0.6942 0.1026 0.089 Uiso 1 1 calc R . . H9B H 0.3500 0.5715 0.0854 0.089 Uiso 1 1 calc R . . H9C H 0.4995 0.6168 0.0687 0.089 Uiso 1 1 calc R . . C10 C 0.6349(4) 0.6237(4) 0.14025(10) 0.0902(13) Uani 1 1 d . . . H10A H 0.5951 0.6971 0.1527 0.135 Uiso 1 1 calc R . . H10B H 0.6920 0.6464 0.1166 0.135 Uiso 1 1 calc R . . H10C H 0.6942 0.5815 0.1601 0.135 Uiso 1 1 calc R . . C11 C 0.0500(2) 0.3636(2) 0.19815(7) 0.0337(5) Uani 1 1 d . . . C12 C -0.0423(3) 0.4360(3) 0.22801(8) 0.0489(6) Uani 1 1 d . . . H12A H -0.1390 0.4047 0.2272 0.073 Uiso 1 1 calc R . . H12B H -0.0423 0.5220 0.2202 0.073 Uiso 1 1 calc R . . H12C H -0.0045 0.4276 0.2556 0.073 Uiso 1 1 calc R . . C13 C 0.0731(3) 0.2347(2) 0.21490(8) 0.0458(6) Uani 1 1 d . . . H13A H -0.0184 0.1956 0.2194 0.069 Uiso 1 1 calc R . . H13B H 0.1246 0.2394 0.2407 0.069 Uiso 1 1 calc R . . H13C H 0.1277 0.1870 0.1953 0.069 Uiso 1 1 calc R . . C14 C -0.0384(2) 0.3558(3) 0.15938(8) 0.0454(6) Uani 1 1 d . . . H14A H 0.0078 0.3011 0.1400 0.068 Uiso 1 1 calc R . . H14B H -0.0473 0.4368 0.1473 0.068 Uiso 1 1 calc R . . H14C H -0.1323 0.3243 0.1660 0.068 Uiso 1 1 calc R . . C15 C 0.4353(2) 0.5665(2) 0.27727(7) 0.0411(6) Uani 1 1 d DU . . C16 C 0.4452(6) 0.7078(4) 0.27700(14) 0.0603(13) Uani 0.703(6) 1 d PDU A 1 H16A H 0.3517 0.7423 0.2719 0.090 Uiso 0.703(6) 1 calc PR A 1 H16B H 0.5103 0.7338 0.2555 0.090 Uiso 0.703(6) 1 calc PR A 1 H16C H 0.4800 0.7362 0.3034 0.090 Uiso 0.703(6) 1 calc PR A 1 C17 C 0.3369(5) 0.5328(5) 0.31264(10) 0.0602(14) Uani 0.703(6) 1 d PDU A 1 H17A H 0.3754 0.5651 0.3381 0.090 Uiso 0.703(6) 1 calc PR A 1 H17B H 0.3294 0.4441 0.3146 0.090 Uiso 0.703(6) 1 calc PR A 1 H17C H 0.2433 0.5676 0.3078 0.090 Uiso 0.703(6) 1 calc PR A 1 C18 C 0.5781(5) 0.5141(5) 0.28433(13) 0.0571(13) Uani 0.703(6) 1 d PDU A 1 H18A H 0.6414 0.5390 0.2623 0.086 Uiso 0.703(6) 1 calc PR A 1 H18B H 0.5717 0.4252 0.2850 0.086 Uiso 0.703(6) 1 calc PR A 1 H18C H 0.6151 0.5436 0.3103 0.086 Uiso 0.703(6) 1 calc PR A 1 C16' C 0.4448(13) 0.4493(10) 0.3056(3) 0.072(3) Uani 0.297(6) 1 d PDU A 2 H16D H 0.4949 0.4700 0.3307 0.107 Uiso 0.297(6) 1 calc PR A 2 H16E H 0.4958 0.3848 0.2913 0.107 Uiso 0.297(6) 1 calc PR A 2 H16F H 0.3495 0.4212 0.3122 0.107 Uiso 0.297(6) 1 calc PR A 2 C17' C 0.5903(9) 0.6113(15) 0.2752(3) 0.070(4) Uani 0.297(6) 1 d PDU A 2 H17D H 0.5947 0.6872 0.2597 0.105 Uiso 0.297(6) 1 calc PR A 2 H17E H 0.6486 0.5496 0.2619 0.105 Uiso 0.297(6) 1 calc PR A 2 H17F H 0.6255 0.6254 0.3028 0.105 Uiso 0.297(6) 1 calc PR A 2 C18' C 0.3393(12) 0.6554(13) 0.2953(3) 0.080(4) Uani 0.297(6) 1 d PDU A 2 H18D H 0.3753 0.6805 0.3219 0.120 Uiso 0.297(6) 1 calc PR A 2 H18E H 0.2458 0.6189 0.2985 0.120 Uiso 0.297(6) 1 calc PR A 2 H18F H 0.3325 0.7265 0.2774 0.120 Uiso 0.297(6) 1 calc PR A 2 Li1 Li 0.1086(5) 0.0261(4) 0.08074(13) 0.0465(10) Uani 1 1 d . B . O1 O 0.2265(3) -0.0604(2) 0.04319(8) 0.0814(7) Uani 1 1 d DU . . C19 C 0.1700(17) -0.1802(10) 0.0322(5) 0.049(3) Uani 0.310(11) 1 d PDU B 1 H19A H 0.0697 -0.1732 0.0242 0.059 Uiso 0.310(11) 1 calc PR B 1 H19B H 0.1771 -0.2365 0.0556 0.059 Uiso 0.310(11) 1 calc PR B 1 C20 C 0.2554(19) -0.2261(13) -0.0025(6) 0.066(4) Uani 0.310(11) 1 d PDU B 1 H20A H 0.3224 -0.2897 0.0064 0.079 Uiso 0.310(11) 1 calc PR B 1 H20B H 0.1944 -0.2592 -0.0243 0.079 Uiso 0.310(11) 1 calc PR B 1 C21 C 0.3307(18) -0.1151(11) -0.0163(4) 0.082(4) Uani 0.310(11) 1 d PDU B 1 H21A H 0.4285 -0.1359 -0.0241 0.099 Uiso 0.310(11) 1 calc PR B 1 H21B H 0.2826 -0.0803 -0.0403 0.099 Uiso 0.310(11) 1 calc PR B 1 C22 C 0.332(2) -0.0294(16) 0.0157(6) 0.103(7) Uani 0.310(11) 1 d PDU B 1 H22A H 0.4249 -0.0298 0.0294 0.124 Uiso 0.310(11) 1 calc PR B 1 H22B H 0.3148 0.0532 0.0048 0.124 Uiso 0.310(11) 1 calc PR B 1 C19' C 0.1838(11) -0.1672(10) 0.0221(4) 0.121(4) Uani 0.690(11) 1 d PDU B 2 H19C H 0.0953 -0.1524 0.0069 0.145 Uiso 0.690(11) 1 calc PR B 2 H19D H 0.1683 -0.2350 0.0413 0.145 Uiso 0.690(11) 1 calc PR B 2 C20' C 0.3003(13) -0.1960(10) -0.0062(3) 0.120(4) Uani 0.690(11) 1 d PDU B 2 H20C H 0.2789 -0.1657 -0.0339 0.144 Uiso 0.690(11) 1 calc PR B 2 H20D H 0.3159 -0.2848 -0.0076 0.144 Uiso 0.690(11) 1 calc PR B 2 C21' C 0.4266(8) -0.1336(5) 0.0106(2) 0.097(3) Uani 0.690(11) 1 d PDU B 2 H21C H 0.4797 -0.1883 0.0290 0.116 Uiso 0.690(11) 1 calc PR B 2 H21D H 0.4900 -0.1062 -0.0114 0.116 Uiso 0.690(11) 1 calc PR B 2 C22' C 0.3703(7) -0.0316(8) 0.0327(3) 0.095(3) Uani 0.690(11) 1 d PDU B 2 H22C H 0.3734 0.0425 0.0156 0.113 Uiso 0.690(11) 1 calc PR B 2 H22D H 0.4264 -0.0167 0.0576 0.113 Uiso 0.690(11) 1 calc PR B 2 O2 O 0.0650(2) -0.09349(16) 0.12185(6) 0.0576(5) Uani 1 1 d D . . C23 C 0.1636(3) -0.1168(3) 0.15351(11) 0.0712(9) Uani 1 1 d D B . H23A H 0.1534 -0.0555 0.1753 0.085 Uiso 1 1 calc R . . H23B H 0.2610 -0.1125 0.1428 0.085 Uiso 1 1 calc R . . C24 C 0.1351(4) -0.2389(3) 0.16957(10) 0.0645(8) Uani 1 1 d D . . H24A H 0.1558 -0.2433 0.1990 0.077 Uiso 1 1 calc R B . H24B H 0.1915 -0.3011 0.1552 0.077 Uiso 1 1 calc R . . C25 C -0.0185(4) -0.2548(3) 0.16152(10) 0.0685(9) Uani 1 1 d D B . H25A H -0.0413 -0.3414 0.1567 0.082 Uiso 1 1 calc R . . H25B H -0.0752 -0.2251 0.1847 0.082 Uiso 1 1 calc R . . C26 C -0.0460(4) -0.1818(3) 0.12481(12) 0.0743(10) Uani 1 1 d D B . H26A H -0.0468 -0.2344 0.1004 0.089 Uiso 1 1 calc R . . H26B H -0.1385 -0.1407 0.1270 0.089 Uiso 1 1 calc R . . O3 O -0.0668(2) 0.0576(2) 0.05380(6) 0.0664(6) Uani 1 1 d DU . . C27 C -0.0815(9) 0.1414(12) 0.0190(3) 0.075(3) Uani 0.523(14) 1 d PDU B 1 H27A H -0.0814 0.0945 -0.0067 0.090 Uiso 0.523(14) 1 calc PR B 1 H27B H -0.0007 0.1982 0.0184 0.090 Uiso 0.523(14) 1 calc PR B 1 C28 C -0.2146(13) 0.2107(9) 0.0225(4) 0.076(3) Uani 0.523(14) 1 d PDU B 1 H28A H -0.1982 0.2910 0.0352 0.092 Uiso 0.523(14) 1 calc PR B 1 H28B H -0.2588 0.2227 -0.0045 0.092 Uiso 0.523(14) 1 calc PR B 1 C29 C -0.3023(9) 0.1339(10) 0.0484(3) 0.078(2) Uani 0.523(14) 1 d PDU B 1 H29A H -0.3687 0.1836 0.0646 0.094 Uiso 0.523(14) 1 calc PR B 1 H29B H -0.3567 0.0749 0.0320 0.094 Uiso 0.523(14) 1 calc PR B 1 C30 C -0.2021(12) 0.0723(15) 0.0745(4) 0.083(4) Uani 0.523(14) 1 d PDU B 1 H30A H -0.2397 -0.0085 0.0821 0.099 Uiso 0.523(14) 1 calc PR B 1 H30B H -0.1885 0.1200 0.0997 0.099 Uiso 0.523(14) 1 calc PR B 1 C27' C -0.0560(12) 0.0833(10) 0.0109(2) 0.067(3) Uani 0.477(14) 1 d PDU B 2 H27C H -0.1049 0.0215 -0.0058 0.080 Uiso 0.477(14) 1 calc PR B 2 H27D H 0.0433 0.0906 0.0020 0.080 Uiso 0.477(14) 1 calc PR B 2 C28' C -0.1294(17) 0.2009(8) 0.0102(3) 0.075(3) Uani 0.477(14) 1 d PDU B 2 H28C H -0.1721 0.2161 -0.0168 0.090 Uiso 0.477(14) 1 calc PR B 2 H28D H -0.0639 0.2681 0.0167 0.090 Uiso 0.477(14) 1 calc PR B 2 C29' C -0.2409(17) 0.1887(13) 0.0422(4) 0.098(4) Uani 0.477(14) 1 d PDU B 2 H29C H -0.2633 0.2693 0.0539 0.117 Uiso 0.477(14) 1 calc PR B 2 H29D H -0.3280 0.1542 0.0303 0.117 Uiso 0.477(14) 1 calc PR B 2 C30' C -0.1866(14) 0.1095(15) 0.0731(3) 0.076(4) Uani 0.477(14) 1 d PDU B 2 H30C H -0.1594 0.1554 0.0977 0.091 Uiso 0.477(14) 1 calc PR B 2 H30D H -0.2563 0.0464 0.0805 0.091 Uiso 0.477(14) 1 calc PR B 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 B1 0.0628(18) 0.0330(13) 0.0423(14) -0.0054(13) -0.0022(16) -0.0005(13) B2 0.0526(17) 0.0540(19) 0.0345(14) 0.0087(14) -0.0117(13) 0.0021(15) P1 0.0420(3) 0.0310(3) 0.0267(2) -0.0002(3) -0.0049(2) -0.0016(2) C1 0.0322(10) 0.0252(9) 0.0273(10) 0.0014(8) -0.0070(8) 0.0006(9) C2 0.0349(11) 0.0353(12) 0.0324(11) 0.0043(10) -0.0007(9) -0.0034(10) C3 0.0314(11) 0.0371(12) 0.0380(12) 0.0005(10) -0.0041(9) -0.0066(10) C4 0.0373(12) 0.0331(11) 0.0323(11) -0.0011(10) -0.0067(9) 0.0034(9) C5 0.0362(12) 0.0350(11) 0.0273(10) 0.0027(9) 0.0005(9) 0.0016(9) C6 0.0320(11) 0.0257(9) 0.0293(10) 0.0032(9) -0.0055(8) 0.0012(8) C7 0.0453(14) 0.0712(19) 0.0349(12) 0.0044(13) 0.0043(11) -0.0201(13) C8 0.0470(15) 0.108(3) 0.0517(16) -0.0021(18) 0.0089(14) 0.0124(16) C9 0.084(2) 0.0524(17) 0.0426(13) 0.0119(13) 0.0115(14) -0.0191(16) C10 0.072(2) 0.140(4) 0.0590(19) 0.002(2) 0.0121(15) -0.064(2) C11 0.0333(10) 0.0320(11) 0.0356(11) 0.0013(10) 0.0011(9) -0.0041(10) C12 0.0389(13) 0.0493(15) 0.0584(16) -0.0073(13) 0.0083(11) -0.0074(12) C13 0.0556(15) 0.0342(13) 0.0477(14) 0.0072(11) -0.0003(12) -0.0096(11) C14 0.0340(12) 0.0550(16) 0.0473(14) -0.0013(13) -0.0025(10) -0.0092(11) C15 0.0407(13) 0.0479(14) 0.0345(12) -0.0080(11) -0.0077(10) 0.0007(11) C16 0.081(3) 0.047(2) 0.053(2) -0.0175(19) -0.017(2) 0.007(2) C17 0.070(3) 0.089(4) 0.0226(17) -0.007(2) -0.0074(16) -0.009(2) C18 0.055(2) 0.067(3) 0.049(2) -0.014(2) -0.0224(19) 0.010(2) C16' 0.083(8) 0.097(7) 0.036(5) 0.007(5) -0.025(5) 0.000(6) C17' 0.047(5) 0.126(12) 0.036(5) -0.024(6) -0.015(4) -0.018(6) C18' 0.072(7) 0.113(10) 0.054(7) -0.042(7) -0.019(6) 0.021(7) Li1 0.049(2) 0.045(2) 0.045(2) -0.003(2) -0.0029(19) -0.0048(19) O1 0.0736(14) 0.0765(14) 0.0942(16) -0.0395(14) 0.0250(13) -0.0079(13) C19 0.072(7) 0.027(5) 0.049(6) -0.004(5) 0.007(5) 0.006(4) C20 0.083(9) 0.055(6) 0.060(7) 0.009(5) 0.035(6) 0.000(6) C21 0.108(10) 0.062(7) 0.076(7) 0.025(6) 0.046(7) 0.004(7) C22 0.123(14) 0.067(8) 0.119(13) 0.004(7) 0.055(11) -0.030(9) C19' 0.111(6) 0.126(8) 0.126(8) -0.084(7) 0.004(5) -0.001(5) C20' 0.171(9) 0.114(9) 0.074(5) -0.026(6) 0.040(6) 0.034(7) C21' 0.126(5) 0.057(3) 0.106(5) 0.026(3) 0.072(4) 0.021(3) C22' 0.068(4) 0.101(5) 0.115(6) -0.005(5) 0.037(4) 0.020(3) O2 0.0629(12) 0.0474(11) 0.0624(12) 0.0178(9) -0.0222(9) -0.0184(9) C23 0.0661(18) 0.074(2) 0.074(2) 0.0207(19) -0.0215(16) -0.0158(18) C24 0.081(2) 0.0520(17) 0.0607(19) 0.0131(15) -0.0038(15) 0.0132(16) C25 0.080(2) 0.0599(19) 0.0655(19) 0.0162(17) -0.0076(17) -0.0194(16) C26 0.065(2) 0.068(2) 0.090(2) 0.0219(19) -0.0122(18) -0.0195(16) O3 0.0570(12) 0.0908(16) 0.0515(11) 0.0229(11) -0.0081(9) -0.0014(11) C27 0.073(5) 0.081(8) 0.070(6) 0.031(5) -0.011(4) -0.003(5) C28 0.082(7) 0.068(5) 0.079(7) 0.012(5) -0.018(6) 0.009(5) C29 0.067(4) 0.072(5) 0.096(6) -0.002(5) -0.004(4) 0.014(4) C30 0.061(5) 0.084(8) 0.104(7) 0.032(6) 0.012(4) 0.017(5) C27' 0.094(6) 0.061(6) 0.046(4) 0.010(4) -0.018(3) 0.007(4) C28' 0.116(10) 0.053(5) 0.056(5) 0.004(4) -0.016(5) 0.009(5) C29' 0.097(9) 0.072(8) 0.124(9) 0.015(7) 0.003(7) 0.032(6) C30' 0.079(6) 0.086(9) 0.063(5) 0.010(5) -0.011(4) 0.003(5) _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 P1 1.955(3) . ? B1 Li1 2.430(5) . ? B1 H1A 1.12(3) . ? B1 H1B 1.06(3) . ? B1 H1C 1.08(3) . ? B2 P1 1.984(3) . ? B2 H2A 1.18(4) . ? B2 H2B 1.02(4) . ? B2 H2C 1.02(3) . ? P1 C1 1.860(2) . ? P1 H1 1.252(19) . ? C1 C6 1.421(3) . ? C1 C2 1.437(3) . ? C2 C3 1.390(3) . ? C2 C7 1.561(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(3) . ? C4 C15 1.543(3) . ? C5 C6 1.405(3) . ? C5 H5 0.9500 . ? C6 C11 1.561(3) . ? C7 C8 1.548(4) . ? C7 C10 1.550(4) . ? C7 C9 1.551(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.528(3) . ? C11 C13 1.537(3) . ? C11 C12 1.539(3) . ? 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 . ? C15 C18' 1.462(10) . ? C15 C18 1.490(5) . ? C15 C17 1.537(5) . ? C15 C17' 1.552(9) . ? C15 C16 1.558(5) . ? C15 C16' 1.593(10) . ? 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 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? Li1 O3 1.917(5) . ? Li1 O1 1.919(5) . ? Li1 O2 1.931(5) . ? Li1 H1A 2.06(3) . ? Li1 H1B 2.03(3) . ? O1 C22 1.392(12) . ? O1 C19' 1.424(8) . ? O1 C22' 1.443(7) . ? O1 C19 1.468(11) . ? C19 C20 1.488(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.485(13) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.412(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C19' C20' 1.479(9) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' C21' 1.488(10) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' C22' 1.439(9) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? O2 C23 1.423(3) . ? O2 C26 1.436(3) . ? C23 C24 1.468(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.491(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.474(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O3 C30' 1.421(10) . ? O3 C27' 1.442(8) . ? O3 C30 1.461(9) . ? O3 C27 1.477(8) . ? C27 C28 1.479(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.460(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.448(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C27' C28' 1.469(10) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28' C29' 1.498(11) . ? C28' H28C 0.9900 . ? C28' H28D 0.9900 . ? C29' C30' 1.434(11) . ? C29' H29C 0.9900 . ? C29' H29D 0.9900 . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? 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 P1 B1 Li1 139.2(2) . . ? P1 B1 H1A 100.9(14) . . ? Li1 B1 H1A 57.8(14) . . ? P1 B1 H1B 113.3(15) . . ? Li1 B1 H1B 55.8(15) . . ? H1A B1 H1B 109(2) . . ? P1 B1 H1C 105.2(17) . . ? Li1 B1 H1C 115.0(17) . . ? H1A B1 H1C 112(2) . . ? H1B B1 H1C 115(2) . . ? P1 B2 H2A 103.8(18) . . ? P1 B2 H2B 105(2) . . ? H2A B2 H2B 109(3) . . ? P1 B2 H2C 106.7(17) . . ? H2A B2 H2C 116(2) . . ? H2B B2 H2C 115(3) . . ? C1 P1 B1 113.05(11) . . ? C1 P1 B2 117.88(12) . . ? B1 P1 B2 121.52(14) . . ? C1 P1 H1 97.9(9) . . ? B1 P1 H1 100.1(9) . . ? B2 P1 H1 99.6(9) . . ? C6 C1 C2 118.18(18) . . ? C6 C1 P1 121.85(15) . . ? C2 C1 P1 119.86(16) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C7 115.5(2) . . ? C1 C2 C7 125.73(19) . . ? C4 C3 C2 123.8(2) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 116.7(2) . . ? C5 C4 C15 122.6(2) . . ? C3 C4 C15 120.7(2) . . ? C4 C5 C6 123.8(2) . . ? C4 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C5 C6 C1 118.56(19) . . ? C5 C6 C11 112.72(18) . . ? C1 C6 C11 128.69(18) . . ? C8 C7 C10 104.7(3) . . ? C8 C7 C9 114.0(2) . . ? C10 C7 C9 103.6(3) . . ? C8 C7 C2 110.4(2) . . ? C10 C7 C2 112.2(2) . . ? C9 C7 C2 111.6(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 109.0(2) . . ? C14 C11 C12 104.46(19) . . ? C13 C11 C12 109.3(2) . . ? C14 C11 C6 116.18(18) . . ? C13 C11 C6 107.99(18) . . ? C12 C11 C6 109.79(18) . . ? 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 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18' C15 C18 139.6(5) . . ? C18' C15 C17 58.5(6) . . ? C18 C15 C17 109.9(3) . . ? C18' C15 C4 110.1(4) . . ? C18 C15 C4 109.8(2) . . ? C17 C15 C4 112.8(2) . . ? C18' C15 C17' 113.3(8) . . ? C18 C15 C17' 43.0(6) . . ? C17 C15 C17' 133.2(4) . . ? C4 C15 C17' 112.8(4) . . ? C18' C15 C16 51.1(6) . . ? C18 C15 C16 109.4(3) . . ? C17 C15 C16 106.4(3) . . ? C4 C15 C16 108.6(2) . . ? C17' C15 C16 68.0(6) . . ? C18' C15 C16' 109.9(7) . . ? C18 C15 C16' 62.9(5) . . ? C17 C15 C16' 52.8(5) . . ? C4 C15 C16' 107.1(4) . . ? C17' C15 C16' 103.2(7) . . ? C16 C15 C16' 143.8(4) . . ? 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 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C16' H16D 109.5 . . ? C15 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15 C17' H17D 109.5 . . ? C15 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C15 C18' H18D 109.5 . . ? C15 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C15 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? O3 Li1 O1 107.3(2) . . ? O3 Li1 O2 105.1(2) . . ? O1 Li1 O2 103.7(2) . . ? O3 Li1 B1 118.1(2) . . ? O1 Li1 B1 109.3(2) . . ? O2 Li1 B1 112.1(2) . . ? O3 Li1 H1A 107.7(8) . . ? O1 Li1 H1A 90.6(8) . . ? O2 Li1 H1A 138.1(8) . . ? B1 Li1 H1A 27.4(7) . . ? O3 Li1 H1B 111.2(8) . . ? O1 Li1 H1B 132.3(8) . . ? O2 Li1 H1B 92.4(9) . . ? B1 Li1 H1B 25.6(8) . . ? H1A Li1 H1B 51.6(11) . . ? C22 O1 C19' 95.1(7) . . ? C22 O1 C22' 27.2(11) . . ? C19' O1 C22' 109.5(5) . . ? C22 O1 C19 108.8(8) . . ? C19' O1 C19 15.2(9) . . ? C22' O1 C19 118.9(7) . . ? C22 O1 Li1 135.7(7) . . ? C19' O1 Li1 123.9(5) . . ? C22' O1 Li1 126.6(4) . . ? C19 O1 Li1 113.1(6) . . ? O1 C19 C20 107.2(9) . . ? O1 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O1 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.5 . . ? C21 C20 C19 102.5(10) . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C20 109.1(10) . . ? C22 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? C22 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O1 C22 C21 108.3(9) . . ? O1 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O1 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? O1 C19' C20' 105.7(7) . . ? O1 C19' H19C 110.6 . . ? C20' C19' H19C 110.6 . . ? O1 C19' H19D 110.6 . . ? C20' C19' H19D 110.6 . . ? H19C C19' H19D 108.7 . . ? C19' C20' C21' 105.6(6) . . ? C19' C20' H20C 110.6 . . ? C21' C20' H20C 110.6 . . ? C19' C20' H20D 110.6 . . ? C21' C20' H20D 110.6 . . ? H20C C20' H20D 108.8 . . ? C22' C21' C20' 104.4(6) . . ? C22' C21' H21C 110.9 . . ? C20' C21' H21C 110.9 . . ? C22' C21' H21D 110.9 . . ? C20' C21' H21D 110.9 . . ? H21C C21' H21D 108.9 . . ? C21' C22' O1 107.5(6) . . ? C21' C22' H22C 110.2 . . ? O1 C22' H22C 110.2 . . ? C21' C22' H22D 110.2 . . ? O1 C22' H22D 110.2 . . ? H22C C22' H22D 108.5 . . ? C23 O2 C26 108.1(2) . . ? C23 O2 Li1 119.7(2) . . ? C26 O2 Li1 131.7(2) . . ? O2 C23 C24 107.9(2) . . ? O2 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O2 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C23 C24 C25 102.9(3) . . ? C23 C24 H24A 111.2 . . ? C25 C24 H24A 111.2 . . ? C23 C24 H24B 111.2 . . ? C25 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? C26 C25 C24 104.7(3) . . ? C26 C25 H25A 110.8 . . ? C24 C25 H25A 110.8 . . ? C26 C25 H25B 110.8 . . ? C24 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? O2 C26 C25 107.2(3) . . ? O2 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O2 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.5 . . ? C30' O3 C27' 114.4(6) . . ? C30' O3 C30 17.4(12) . . ? C27' O3 C30 119.7(7) . . ? C30' O3 C27 91.1(6) . . ? C27' O3 C27 29.0(4) . . ? C30 O3 C27 102.0(5) . . ? C30' O3 Li1 124.1(6) . . ? C27' O3 Li1 115.2(5) . . ? C30 O3 Li1 124.6(6) . . ? C27 O3 Li1 123.6(4) . . ? O3 C27 C28 110.0(6) . . ? O3 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? O3 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C29 C28 C27 103.5(7) . . ? C29 C28 H28A 111.1 . . ? C27 C28 H28A 111.1 . . ? C29 C28 H28B 111.1 . . ? C27 C28 H28B 111.1 . . ? H28A C28 H28B 109.0 . . ? C30 C29 C28 104.0(7) . . ? C30 C29 H29A 111.0 . . ? C28 C29 H29A 111.0 . . ? C30 C29 H29B 111.0 . . ? C28 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? C29 C30 O3 110.7(8) . . ? C29 C30 H30A 109.5 . . ? O3 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O3 C27' C28' 99.0(6) . . ? O3 C27' H27C 112.0 . . ? C28' C27' H27C 112.0 . . ? O3 C27' H27D 112.0 . . ? C28' C27' H27D 112.0 . . ? H27C C27' H27D 109.7 . . ? C27' C28' C29' 104.1(8) . . ? C27' C28' H28C 110.9 . . ? C29' C28' H28C 110.9 . . ? C27' C28' H28D 110.9 . . ? C29' C28' H28D 110.9 . . ? H28C C28' H28D 109.0 . . ? C30' C29' C28' 107.4(8) . . ? C30' C29' H29C 110.2 . . ? C28' C29' H29C 110.2 . . ? C30' C29' H29D 110.2 . . ? C28' C29' H29D 110.2 . . ? H29C C29' H29D 108.5 . . ? O3 C30' C29' 102.5(7) . . ? O3 C30' H30C 111.3 . . ? C29' C30' H30C 111.3 . . ? O3 C30' H30D 111.3 . . ? C29' C30' H30D 111.3 . . ? H30C C30' H30D 109.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.036 data_2 _database_code_CSD 167807 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H61 B3 Li O2 P' _chemical_formula_weight 560.16 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' 'Li' 'Li' -0.0003 0.0001 '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' 'O' 'O' 0.0106 0.0060 '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 9.8395(8) _cell_length_b 11.2345(9) _cell_length_c 16.5435(13) _cell_angle_alpha 96.708(2) _cell_angle_beta 98.842(2) _cell_angle_gamma 91.449(2) _cell_volume 1792.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7292 _cell_measurement_theta_min 2.267 _cell_measurement_theta_max 29.382 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.494284 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 10510 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7210 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0742P)^2^+0.7401P] 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 7210 _refine_ls_number_parameters 434 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.039 _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 0.5399(2) 0.41777(16) 0.40409(11) 0.0288(4) Uani 1 1 d . . . H1BA H 0.569(2) 0.502(2) 0.3782(13) 0.050(6) Uiso 1 1 d . . . H1BB H 0.616(2) 0.4048(17) 0.4570(12) 0.034(5) Uiso 1 1 d . . . H1BC H 0.433(2) 0.4195(18) 0.4205(13) 0.044(6) Uiso 1 1 d . . . B2 B 0.3937(2) 0.15975(19) 0.30476(13) 0.0366(4) Uani 1 1 d . . . H2BA H 0.366(2) 0.112(2) 0.2406(14) 0.053(6) Uiso 1 1 d . . . H2BB H 0.311(2) 0.186(2) 0.3419(14) 0.055(6) Uiso 1 1 d . . . H32B H 0.461(2) 0.078(2) 0.3443(14) 0.059(7) Uiso 1 1 d . . . B3 B 0.5818(2) 0.13028(18) 0.36253(13) 0.0371(4) Uani 1 1 d . . . H3BA H 0.644(2) 0.068(2) 0.3274(14) 0.055(6) Uiso 1 1 d . . . H3BB H 0.600(2) 0.1391(18) 0.4307(13) 0.041(5) Uiso 1 1 d . . . P1 P 0.54199(4) 0.27921(3) 0.32040(2) 0.02354(12) Uani 1 1 d . . . C1 C 0.61290(15) 0.28669(13) 0.22406(9) 0.0222(3) Uani 1 1 d . . . C2 C 0.75059(16) 0.25423(13) 0.21881(9) 0.0250(3) Uani 1 1 d . . . C3 C 0.78208(16) 0.21149(15) 0.14127(10) 0.0286(3) Uani 1 1 d . . . H3 H 0.8727 0.1861 0.1380 0.034 Uiso 1 1 calc R . . C5 C 0.56214(16) 0.25349(14) 0.07489(9) 0.0278(3) Uani 1 1 d . . . H5 H 0.4996 0.2574 0.0255 0.033 Uiso 1 1 calc R . . C6 C 0.52206(15) 0.29788(13) 0.15006(9) 0.0241(3) Uani 1 1 d . . . C7 C 0.87732(16) 0.26792(16) 0.28907(10) 0.0313(4) Uani 1 1 d . . . C8 C 0.85267(19) 0.33274(19) 0.37199(11) 0.0419(4) Uani 1 1 d . . . H8A H 0.8025 0.4054 0.3628 0.063 Uiso 1 1 calc R . . H8B H 0.9413 0.3546 0.4072 0.063 Uiso 1 1 calc R . . H8C H 0.7984 0.2796 0.3990 0.063 Uiso 1 1 calc R . . C9 C 0.9362(2) 0.14542(19) 0.30274(13) 0.0467(5) Uani 1 1 d . . . H9A H 0.8670 0.0948 0.3208 0.070 Uiso 1 1 calc R . . H9B H 1.0184 0.1565 0.3450 0.070 Uiso 1 1 calc R . . H9C H 0.9608 0.1068 0.2511 0.070 Uiso 1 1 calc R . . C10 C 0.98944(19) 0.3461(2) 0.26197(12) 0.0459(5) Uani 1 1 d . . . H10A H 1.0128 0.3084 0.2097 0.069 Uiso 1 1 calc R . . H10B H 1.0717 0.3538 0.3042 0.069 Uiso 1 1 calc R . . H10C H 0.9549 0.4259 0.2547 0.069 Uiso 1 1 calc R . . C4 C 0.68854(17) 0.20412(14) 0.06901(9) 0.0281(3) Uani 1 1 d DU A . C11 C 0.72527(19) 0.15003(17) -0.01413(10) 0.0356(4) Uani 1 1 d DU . . C12 C 0.8579(5) 0.0820(5) -0.0061(3) 0.0457(11) Uani 0.501(4) 1 d PDU A 1 H12A H 0.8687 0.0405 -0.0601 0.069 Uiso 0.501(4) 1 calc PR A 1 H12B H 0.8537 0.0231 0.0328 0.069 Uiso 0.501(4) 1 calc PR A 1 H12C H 0.9365 0.1386 0.0142 0.069 Uiso 0.501(4) 1 calc PR A 1 C13 C 0.7235(6) 0.2399(4) -0.0720(2) 0.0530(13) Uani 0.501(4) 1 d PDU A 1 H13A H 0.7955 0.3024 -0.0505 0.079 Uiso 0.501(4) 1 calc PR A 1 H13B H 0.6334 0.2761 -0.0786 0.079 Uiso 0.501(4) 1 calc PR A 1 H13C H 0.7403 0.2012 -0.1256 0.079 Uiso 0.501(4) 1 calc PR A 1 C14 C 0.6068(5) 0.0481(4) -0.0521(3) 0.0519(12) Uani 0.501(4) 1 d PDU A 1 H14A H 0.5173 0.0850 -0.0604 0.078 Uiso 0.501(4) 1 calc PR A 1 H14B H 0.6047 -0.0121 -0.0139 0.078 Uiso 0.501(4) 1 calc PR A 1 H14C H 0.6264 0.0095 -0.1051 0.078 Uiso 0.501(4) 1 calc PR A 1 C12' C 0.7783(7) 0.0301(4) -0.0082(3) 0.0544(13) Uani 0.499(4) 1 d PDU A 2 H12D H 0.8054 -0.0016 -0.0609 0.082 Uiso 0.499(4) 1 calc PR A 2 H12E H 0.7065 -0.0233 0.0048 0.082 Uiso 0.499(4) 1 calc PR A 2 H12F H 0.8585 0.0349 0.0354 0.082 Uiso 0.499(4) 1 calc PR A 2 C13' C 0.8471(4) 0.2356(4) -0.0337(2) 0.0461(11) Uani 0.499(4) 1 d PDU A 2 H13D H 0.8718 0.2061 -0.0874 0.069 Uiso 0.499(4) 1 calc PR A 2 H13E H 0.9277 0.2352 0.0092 0.069 Uiso 0.499(4) 1 calc PR A 2 H13F H 0.8158 0.3177 -0.0347 0.069 Uiso 0.499(4) 1 calc PR A 2 C14' C 0.6109(4) 0.1535(5) -0.0864(2) 0.0512(12) Uani 0.499(4) 1 d PDU A 2 H14D H 0.5863 0.2367 -0.0908 0.077 Uiso 0.499(4) 1 calc PR A 2 H14E H 0.5301 0.1065 -0.0779 0.077 Uiso 0.499(4) 1 calc PR A 2 H14F H 0.6422 0.1195 -0.1373 0.077 Uiso 0.499(4) 1 calc PR A 2 C15 C 0.38293(17) 0.36146(15) 0.14041(10) 0.0309(4) Uani 1 1 d . . . C16 C 0.3923(2) 0.45468(18) 0.07963(12) 0.0439(5) Uani 1 1 d . . . H16A H 0.4011 0.4133 0.0253 0.066 Uiso 1 1 calc R . . H16B H 0.4728 0.5091 0.0998 0.066 Uiso 1 1 calc R . . H16C H 0.3088 0.5008 0.0752 0.066 Uiso 1 1 calc R . . C17 C 0.3475(2) 0.43303(18) 0.21886(11) 0.0417(4) Uani 1 1 d . . . H17A H 0.2664 0.4798 0.2045 0.063 Uiso 1 1 calc R . . H17B H 0.4256 0.4874 0.2446 0.063 Uiso 1 1 calc R . . H17C H 0.3277 0.3775 0.2575 0.063 Uiso 1 1 calc R . . C18 C 0.26220(18) 0.27177(19) 0.10469(12) 0.0426(4) Uani 1 1 d . . . H18A H 0.2513 0.2152 0.1443 0.064 Uiso 1 1 calc R . . H18B H 0.2808 0.2277 0.0531 0.064 Uiso 1 1 calc R . . H18C H 0.1775 0.3152 0.0939 0.064 Uiso 1 1 calc R . . Li1 Li 0.4923(3) 0.6351(3) 0.45419(18) 0.0336(6) Uani 1 1 d . . . O1 O 0.65184(12) 0.74111(10) 0.45996(8) 0.0353(3) Uani 1 1 d . . . C19 C 0.7902(2) 0.70068(19) 0.47497(17) 0.0567(6) Uani 1 1 d . . . H19A H 0.8005 0.6271 0.4376 0.068 Uiso 1 1 calc R . . H19B H 0.8145 0.6837 0.5327 0.068 Uiso 1 1 calc R . . C20 C 0.8800(2) 0.8034(2) 0.45818(15) 0.0565(6) Uani 1 1 d . . . H20A H 0.9745 0.8027 0.4889 0.068 Uiso 1 1 calc R . . H20B H 0.8843 0.8009 0.3986 0.068 Uiso 1 1 calc R . . C21 C 0.8060(2) 0.91112(19) 0.48911(15) 0.0523(5) Uani 1 1 d . . . H21A H 0.8293 0.9302 0.5497 0.063 Uiso 1 1 calc R . . H21B H 0.8281 0.9823 0.4627 0.063 Uiso 1 1 calc R . . C22 C 0.65736(19) 0.87016(16) 0.46374(12) 0.0370(4) Uani 1 1 d . . . H22A H 0.6014 0.9059 0.5045 0.044 Uiso 1 1 calc R . . H22B H 0.6212 0.8946 0.4092 0.044 Uiso 1 1 calc R . . O2 O 0.33762(13) 0.69834(11) 0.38723(8) 0.0389(3) Uani 1 1 d . . . C23 C 0.3269(3) 0.8088(3) 0.35160(19) 0.0693(7) Uani 1 1 d . . . H23A H 0.3831 0.8081 0.3068 0.083 Uiso 1 1 calc R . . H23B H 0.3596 0.8775 0.3939 0.083 Uiso 1 1 calc R . . C24 C 0.1757(2) 0.8186(2) 0.31799(16) 0.0633(6) Uani 1 1 d . . . H24A H 0.1287 0.8675 0.3582 0.076 Uiso 1 1 calc R . . H24B H 0.1641 0.8546 0.2657 0.076 Uiso 1 1 calc R . . C25 C 0.1215(2) 0.6916(2) 0.30449(15) 0.0615(7) Uani 1 1 d . . . H25A H 0.1373 0.6511 0.2505 0.074 Uiso 1 1 calc R . . H25B H 0.0218 0.6864 0.3075 0.074 Uiso 1 1 calc R . . C26 C 0.2040(2) 0.6383(2) 0.37431(14) 0.0506(5) Uani 1 1 d . . . H26A H 0.1607 0.6520 0.4246 0.061 Uiso 1 1 calc R . . H26B H 0.2111 0.5509 0.3599 0.061 Uiso 1 1 calc R . . C27 C 0.8230(2) 0.64300(19) 0.14069(12) 0.0493(5) Uani 1 1 d . . . C28 C 0.8334(3) 0.7645(2) 0.13296(13) 0.0586(6) Uani 1 1 d . . . H28 H 0.8914 0.7913 0.0972 0.070 Uiso 1 1 calc R . . C29 C 0.7616(3) 0.8474(2) 0.17600(15) 0.0664(7) Uani 1 1 d . . . H29 H 0.7704 0.9300 0.1695 0.080 Uiso 1 1 calc R . . C30 C 0.6779(3) 0.8109(2) 0.22795(15) 0.0706(7) Uani 1 1 d . . . H30 H 0.6278 0.8678 0.2572 0.085 Uiso 1 1 calc R . . C31 C 0.6670(3) 0.6917(2) 0.23746(16) 0.0685(7) Uani 1 1 d . . . H31 H 0.6103 0.6662 0.2743 0.082 Uiso 1 1 calc R . . C32 C 0.7373(3) 0.6084(2) 0.19407(15) 0.0570(6) Uani 1 1 d . . . H32 H 0.7272 0.5260 0.2007 0.068 Uiso 1 1 calc R . . C33 C 0.9005(3) 0.5528(3) 0.09434(16) 0.0706(7) Uani 1 1 d . . . H33A H 0.9051 0.5761 0.0395 0.106 Uiso 1 1 calc R . . H33B H 0.8533 0.4737 0.0887 0.106 Uiso 1 1 calc R . . H33C H 0.9940 0.5494 0.1244 0.106 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 0.0380(10) 0.0263(9) 0.0222(8) -0.0026(7) 0.0089(7) 0.0060(7) B2 0.0381(11) 0.0374(10) 0.0342(10) -0.0004(8) 0.0108(8) -0.0076(8) B3 0.0481(12) 0.0306(10) 0.0366(10) 0.0068(8) 0.0163(9) 0.0066(8) P1 0.0285(2) 0.0231(2) 0.02003(19) -0.00036(14) 0.00887(14) 0.00300(14) C1 0.0258(7) 0.0209(7) 0.0205(7) -0.0017(5) 0.0081(6) 0.0019(5) C2 0.0267(8) 0.0255(7) 0.0234(7) 0.0015(6) 0.0062(6) 0.0037(6) C3 0.0238(7) 0.0354(8) 0.0281(8) 0.0005(6) 0.0105(6) 0.0063(6) C5 0.0301(8) 0.0332(8) 0.0195(7) -0.0003(6) 0.0047(6) 0.0037(6) C6 0.0251(7) 0.0252(7) 0.0224(7) 0.0002(6) 0.0063(6) 0.0030(6) C7 0.0257(8) 0.0398(9) 0.0278(8) 0.0010(7) 0.0038(6) 0.0056(7) C8 0.0325(9) 0.0597(12) 0.0286(9) -0.0074(8) -0.0013(7) 0.0039(8) C9 0.0403(10) 0.0535(12) 0.0444(11) 0.0068(9) -0.0024(8) 0.0163(9) C10 0.0302(9) 0.0644(13) 0.0407(10) 0.0014(9) 0.0035(8) -0.0070(9) C4 0.0316(8) 0.0306(8) 0.0234(7) -0.0005(6) 0.0111(6) 0.0034(6) C11 0.0408(9) 0.0429(10) 0.0248(8) -0.0027(7) 0.0143(7) 0.0089(7) C12 0.045(2) 0.056(3) 0.038(2) -0.0046(18) 0.0210(18) 0.016(2) C13 0.086(4) 0.047(2) 0.034(2) 0.0064(16) 0.032(2) 0.018(2) C14 0.053(2) 0.054(3) 0.045(2) -0.0208(19) 0.0145(19) 0.0015(19) C12' 0.080(4) 0.042(2) 0.046(2) -0.0034(18) 0.031(2) 0.014(2) C13' 0.051(2) 0.057(2) 0.034(2) 0.0019(17) 0.0241(18) -0.0031(18) C14' 0.050(2) 0.077(3) 0.0250(18) -0.0096(18) 0.0136(16) 0.003(2) C15 0.0290(8) 0.0390(9) 0.0242(8) -0.0001(6) 0.0042(6) 0.0112(7) C16 0.0485(11) 0.0475(11) 0.0365(10) 0.0092(8) 0.0031(8) 0.0188(9) C17 0.0407(10) 0.0515(11) 0.0317(9) -0.0039(8) 0.0050(7) 0.0256(8) C18 0.0279(9) 0.0607(12) 0.0365(9) -0.0034(8) 0.0027(7) 0.0064(8) Li1 0.0321(14) 0.0354(15) 0.0337(14) 0.0062(11) 0.0051(11) 0.0026(11) O1 0.0285(6) 0.0305(6) 0.0461(7) 0.0037(5) 0.0040(5) 0.0035(5) C19 0.0322(10) 0.0410(11) 0.0908(17) -0.0045(11) -0.0016(10) 0.0104(8) C20 0.0308(10) 0.0842(17) 0.0542(13) 0.0086(11) 0.0062(9) -0.0023(10) C21 0.0468(12) 0.0456(11) 0.0613(13) 0.0166(10) -0.0075(10) -0.0078(9) C22 0.0389(9) 0.0316(9) 0.0422(10) 0.0069(7) 0.0094(8) 0.0023(7) O2 0.0322(6) 0.0409(7) 0.0422(7) 0.0078(5) -0.0006(5) 0.0038(5) C23 0.0474(13) 0.0738(16) 0.0913(19) 0.0460(15) -0.0019(12) 0.0051(11) C24 0.0530(13) 0.0736(16) 0.0620(14) 0.0165(12) -0.0046(11) 0.0210(12) C25 0.0463(12) 0.0712(15) 0.0560(13) -0.0158(11) -0.0112(10) 0.0174(11) C26 0.0350(10) 0.0517(12) 0.0613(13) 0.0018(10) 0.0001(9) 0.0007(9) C27 0.0579(13) 0.0498(11) 0.0329(10) 0.0033(8) -0.0133(9) -0.0063(9) C28 0.0780(16) 0.0586(14) 0.0379(11) 0.0134(10) 0.0024(10) -0.0135(12) C29 0.104(2) 0.0408(12) 0.0499(13) 0.0030(10) 0.0005(13) -0.0124(12) C30 0.108(2) 0.0565(14) 0.0451(13) -0.0033(11) 0.0134(13) -0.0010(14) C31 0.0845(19) 0.0670(16) 0.0574(15) 0.0141(12) 0.0182(13) -0.0060(14) C32 0.0639(14) 0.0434(11) 0.0590(14) 0.0121(10) -0.0069(11) -0.0129(10) C33 0.0797(18) 0.0754(17) 0.0502(14) 0.0010(12) -0.0078(12) 0.0175(14) _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 P1 1.9615(17) . ? B1 Li1 2.548(3) 2_666 ? B1 Li1 2.563(3) . ? B2 P1 1.924(2) . ? B2 B3 2.002(3) . ? B3 P1 1.913(2) . ? P1 C1 1.8452(15) . ? C1 C6 1.421(2) . ? C1 C2 1.425(2) . ? C2 C3 1.399(2) . ? C2 C7 1.560(2) . ? C3 C4 1.385(2) . ? C5 C4 1.387(2) . ? C5 C6 1.402(2) . ? C6 C15 1.555(2) . ? C7 C8 1.532(2) . ? C7 C9 1.534(3) . ? C7 C10 1.544(3) . ? C4 C11 1.536(2) . ? C11 C12' 1.466(5) . ? C11 C13 1.469(4) . ? C11 C14' 1.516(4) . ? C11 C12 1.525(4) . ? C11 C13' 1.613(4) . ? C11 C14 1.614(4) . ? C15 C18 1.536(3) . ? C15 C17 1.537(2) . ? C15 C16 1.545(3) . ? Li1 O1 1.930(3) . ? Li1 O2 1.942(3) . ? Li1 B1 2.548(3) 2_666 ? O1 C19 1.440(2) . ? O1 C22 1.443(2) . ? C19 C20 1.513(3) . ? C20 C21 1.507(3) . ? C21 C22 1.503(3) . ? O2 C23 1.434(3) . ? O2 C26 1.437(2) . ? C23 C24 1.518(3) . ? C24 C25 1.491(4) . ? C25 C26 1.500(3) . ? C27 C28 1.389(3) . ? C27 C32 1.390(3) . ? C27 C33 1.495(3) . ? C28 C29 1.381(4) . ? C29 C30 1.367(4) . ? C30 C31 1.370(4) . ? C31 C32 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 B1 Li1 114.66(11) . 2_666 ? P1 B1 Li1 154.39(11) . . ? Li1 B1 Li1 87.78(11) 2_666 . ? P1 B2 B3 58.29(8) . . ? P1 B3 B2 58.81(9) . . ? C1 P1 B3 110.68(8) . . ? C1 P1 B2 110.94(8) . . ? B3 P1 B2 62.91(10) . . ? C1 P1 B1 123.45(7) . . ? B3 P1 B1 115.26(9) . . ? B2 P1 B1 118.27(9) . . ? C6 C1 C2 118.67(13) . . ? C6 C1 P1 119.37(11) . . ? C2 C1 P1 120.41(11) . . ? C3 C2 C1 118.04(13) . . ? C3 C2 C7 113.95(13) . . ? C1 C2 C7 127.88(13) . . ? C4 C3 C2 123.64(14) . . ? C4 C5 C6 123.25(14) . . ? C5 C6 C1 118.32(13) . . ? C5 C6 C15 113.78(13) . . ? C1 C6 C15 127.80(13) . . ? C8 C7 C9 108.97(15) . . ? C8 C7 C10 104.93(15) . . ? C9 C7 C10 108.19(15) . . ? C8 C7 C2 115.76(13) . . ? C9 C7 C2 110.82(14) . . ? C10 C7 C2 107.77(14) . . ? C3 C4 C5 116.49(14) . . ? C3 C4 C11 121.83(14) . . ? C5 C4 C11 121.61(14) . . ? C12' C11 C13 136.5(3) . . ? C12' C11 C14' 113.1(3) . . ? C13 C11 C14' 57.1(3) . . ? C12' C11 C12 37.3(2) . . ? C13 C11 C12 112.7(3) . . ? C14' C11 C12 131.3(2) . . ? C12' C11 C4 110.5(2) . . ? C13 C11 C4 111.62(19) . . ? C14' C11 C4 113.98(19) . . ? C12 C11 C4 113.5(2) . . ? C12' C11 C13' 108.0(3) . . ? C13 C11 C13' 49.1(3) . . ? C14' C11 C13' 104.2(3) . . ? C12 C11 C13' 71.7(3) . . ? C4 C11 C13' 106.57(18) . . ? C12' C11 C14 69.4(3) . . ? C13 C11 C14 108.0(3) . . ? C14' C11 C14 52.0(3) . . ? C12 C11 C14 104.2(3) . . ? C4 C11 C14 106.18(19) . . ? C13' C11 C14 145.6(2) . . ? C18 C15 C17 108.11(15) . . ? C18 C15 C16 108.62(15) . . ? C17 C15 C16 105.24(15) . . ? C18 C15 C6 111.21(14) . . ? C17 C15 C6 116.06(13) . . ? C16 C15 C6 107.22(14) . . ? O1 Li1 O2 108.58(15) . . ? O1 Li1 B1 111.83(14) . 2_666 ? O2 Li1 B1 118.10(14) . 2_666 ? O1 Li1 B1 111.77(14) . . ? O2 Li1 B1 113.61(14) . . ? B1 Li1 B1 92.22(11) 2_666 . ? C19 O1 C22 108.87(14) . . ? C19 O1 Li1 122.33(14) . . ? C22 O1 Li1 128.10(13) . . ? O1 C19 C20 104.78(17) . . ? C21 C20 C19 102.02(17) . . ? C22 C21 C20 102.36(17) . . ? O1 C22 C21 106.80(15) . . ? C23 O2 C26 109.01(15) . . ? C23 O2 Li1 130.23(16) . . ? C26 O2 Li1 120.44(15) . . ? O2 C23 C24 106.3(2) . . ? C25 C24 C23 103.35(19) . . ? C24 C25 C26 102.48(18) . . ? O2 C26 C25 105.67(19) . . ? C28 C27 C32 117.0(2) . . ? C28 C27 C33 121.9(2) . . ? C32 C27 C33 121.1(2) . . ? C29 C28 C27 121.6(2) . . ? C30 C29 C28 120.2(2) . . ? C29 C30 C31 119.4(3) . . ? C30 C31 C32 120.7(3) . . ? C31 C32 C27 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.484 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.043