Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Keith Izod' _publ_contact_author_email K.J.IZOD@NCL.AC.UK loop_ _publ_author_name K.Izod L.J.Bowman W.Clegg R.W.Harrington C.Wills data_ki204_compound4 _database_code_depnum_ccdc_archive 'CCDC 713037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H64 K2 O2 Si4' _chemical_formula_sum 'C44 H64 K2 O2 Si4' _chemical_formula_weight 815.51 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9778(8) _cell_length_b 14.082(2) _cell_length_c 16.708(2) _cell_angle_alpha 93.837(15) _cell_angle_beta 90.063(8) _cell_angle_gamma 100.382(5) _cell_volume 2303.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.5 _exptl_crystal_description slab _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65195 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10520 _reflns_number_gt 7891 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0847P)^2^+1.9198P] 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 SHELXL _refine_ls_extinction_coef 0.0132(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10520 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1650 _refine_ls_wR_factor_gt 0.1481 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 K1 K -0.13070(6) 0.19773(4) -0.12954(4) 0.03234(16) Uani 1 1 d . . . K2 K -0.25868(6) 0.20626(5) 0.37144(4) 0.03604(17) Uani 1 1 d . . . Si1 Si 0.16981(7) 0.21757(5) 0.00152(4) 0.02262(16) Uani 1 1 d . . . Si2 Si -0.11869(7) 0.17742(5) 0.08857(4) 0.02187(16) Uani 1 1 d . . . C1 C 0.0049(2) 0.14443(17) 0.01827(13) 0.0207(5) Uani 1 1 d . . . C2 C -0.0201(2) 0.04148(16) -0.02384(13) 0.0200(5) Uani 1 1 d . . . H2A H 0.0308 0.0440 -0.0747 0.024 Uiso 1 1 calc R . . H2B H -0.1182 0.0236 -0.0380 0.024 Uiso 1 1 calc R . . C3 C 0.2342(3) 0.3242(2) 0.07493(18) 0.0422(7) Uani 1 1 d . . . H3A H 0.1739 0.3719 0.0731 0.063 Uiso 1 1 calc R . . H3B H 0.3266 0.3541 0.0605 0.063 Uiso 1 1 calc R . . H3C H 0.2353 0.3020 0.1292 0.063 Uiso 1 1 calc R . . C4 C 0.3151(3) 0.1475(2) -0.00517(18) 0.0359(6) Uani 1 1 d . . . H4A H 0.3323 0.1257 0.0477 0.054 Uiso 1 1 calc R . . H4B H 0.3973 0.1894 -0.0232 0.054 Uiso 1 1 calc R . . H4C H 0.2908 0.0913 -0.0436 0.054 Uiso 1 1 calc R . . C5 C 0.1739(2) 0.27369(18) -0.10073(16) 0.0260(5) Uani 1 1 d . . . C6 C 0.1900(3) 0.2185(2) -0.17266(17) 0.0345(6) Uani 1 1 d . . . H6 H 0.2110 0.1557 -0.1696 0.041 Uiso 1 1 calc R . . C7 C 0.1760(4) 0.2531(3) -0.24804(19) 0.0477(8) Uani 1 1 d . . . H7 H 0.1861 0.2135 -0.2952 0.057 Uiso 1 1 calc R . . C8 C 0.1474(4) 0.3453(3) -0.2542(2) 0.0512(9) Uani 1 1 d . . . H8 H 0.1382 0.3692 -0.3054 0.061 Uiso 1 1 calc R . . C9 C 0.1325(4) 0.4019(2) -0.1855(2) 0.0480(8) Uani 1 1 d . . . H9 H 0.1138 0.4652 -0.1893 0.058 Uiso 1 1 calc R . . C10 C 0.1448(3) 0.3661(2) -0.10965(18) 0.0355(6) Uani 1 1 d . . . H10 H 0.1330 0.4060 -0.0630 0.043 Uiso 1 1 calc R . . C11 C -0.1029(3) 0.3123(2) 0.11585(18) 0.0369(6) Uani 1 1 d . . . H11A H -0.0198 0.3354 0.1480 0.055 Uiso 1 1 calc R . . H11B H -0.1823 0.3241 0.1469 0.055 Uiso 1 1 calc R . . H11C H -0.0984 0.3470 0.0667 0.055 Uiso 1 1 calc R . . C12 C -0.3027(3) 0.1386(2) 0.05241(16) 0.0307(6) Uani 1 1 d . . . H12A H -0.3187 0.1751 0.0065 0.046 Uiso 1 1 calc R . . H12B H -0.3642 0.1516 0.0959 0.046 Uiso 1 1 calc R . . H12C H -0.3199 0.0693 0.0363 0.046 Uiso 1 1 calc R . . C13 C -0.1176(3) 0.12308(19) 0.19130(14) 0.0253(5) Uani 1 1 d . . . C14 C -0.2239(3) 0.0528(2) 0.21825(15) 0.0306(6) Uani 1 1 d . . . H14 H -0.3049 0.0350 0.1867 0.037 Uiso 1 1 calc R . . C15 C -0.2139(3) 0.0084(2) 0.29002(17) 0.0373(7) Uani 1 1 d . . . H15 H -0.2861 -0.0402 0.3056 0.045 Uiso 1 1 calc R . . C16 C -0.0986(3) 0.0356(2) 0.33810(16) 0.0377(7) Uani 1 1 d . . . H16 H -0.0913 0.0056 0.3868 0.045 Uiso 1 1 calc R . . C17 C 0.0069(3) 0.1074(2) 0.31488(17) 0.0365(7) Uani 1 1 d . . . H17 H 0.0852 0.1277 0.3485 0.044 Uiso 1 1 calc R . . C18 C -0.0028(3) 0.1492(2) 0.24232(16) 0.0315(6) Uani 1 1 d . . . H18 H 0.0705 0.1970 0.2268 0.038 Uiso 1 1 calc R . . Si3 Si -0.28465(7) 0.17032(5) 0.58865(4) 0.02161(16) Uani 1 1 d . . . Si4 Si -0.54756(7) 0.22182(5) 0.50381(4) 0.02301(17) Uani 1 1 d . . . C23 C -0.4251(2) 0.14423(17) 0.51792(14) 0.0209(5) Uani 1 1 d . . . C24 C -0.4595(2) 0.04050(16) 0.47563(13) 0.0207(5) Uani 1 1 d . . . H24A H -0.5123 0.0441 0.4261 0.025 Uiso 1 1 calc R . . H24B H -0.3728 0.0207 0.4592 0.025 Uiso 1 1 calc R . . C25 C -0.2221(3) 0.3042(2) 0.61574(18) 0.0357(6) Uani 1 1 d . . . H25A H -0.2049 0.3384 0.5666 0.054 Uiso 1 1 calc R . . H25B H -0.1376 0.3127 0.6475 0.054 Uiso 1 1 calc R . . H25C H -0.2916 0.3305 0.6471 0.054 Uiso 1 1 calc R . . C26 C -0.1247(3) 0.1250(2) 0.55317(16) 0.0311(6) Uani 1 1 d . . . H26A H -0.1475 0.0557 0.5373 0.047 Uiso 1 1 calc R . . H26B H -0.0568 0.1359 0.5968 0.047 Uiso 1 1 calc R . . H26C H -0.0875 0.1601 0.5071 0.047 Uiso 1 1 calc R . . C27 C -0.3189(2) 0.11708(18) 0.69160(14) 0.0232(5) Uani 1 1 d . . . C28 C -0.2540(3) 0.0448(2) 0.71998(15) 0.0303(6) Uani 1 1 d . . . H28 H -0.1839 0.0238 0.6888 0.036 Uiso 1 1 calc R . . C29 C -0.2888(3) 0.0028(2) 0.79247(17) 0.0381(7) Uani 1 1 d . . . H29 H -0.2441 -0.0467 0.8094 0.046 Uiso 1 1 calc R . . C30 C -0.3891(3) 0.0338(2) 0.83940(16) 0.0364(7) Uani 1 1 d . . . H30 H -0.4140 0.0055 0.8885 0.044 Uiso 1 1 calc R . . C31 C -0.4534(3) 0.1070(2) 0.81411(17) 0.0365(6) Uani 1 1 d . . . H31 H -0.5206 0.1297 0.8467 0.044 Uiso 1 1 calc R . . C32 C -0.4190(3) 0.1467(2) 0.74110(16) 0.0309(6) Uani 1 1 d . . . H32 H -0.4651 0.1956 0.7243 0.037 Uiso 1 1 calc R . . C33 C -0.5486(3) 0.3292(2) 0.57804(18) 0.0390(7) Uani 1 1 d . . . H33A H -0.5612 0.3069 0.6323 0.059 Uiso 1 1 calc R . . H33B H -0.6234 0.3621 0.5645 0.059 Uiso 1 1 calc R . . H33C H -0.4618 0.3743 0.5757 0.059 Uiso 1 1 calc R . . C34 C -0.7309(3) 0.1556(2) 0.4993(2) 0.0381(7) Uani 1 1 d . . . H34A H -0.7393 0.0993 0.4607 0.057 Uiso 1 1 calc R . . H34B H -0.7903 0.1992 0.4825 0.057 Uiso 1 1 calc R . . H34C H -0.7580 0.1341 0.5525 0.057 Uiso 1 1 calc R . . C35 C -0.5245(3) 0.27772(19) 0.40136(16) 0.0267(5) Uani 1 1 d . . . C36 C -0.4508(3) 0.3715(2) 0.39208(18) 0.0358(6) Uani 1 1 d . . . H36 H -0.4223 0.4124 0.4388 0.043 Uiso 1 1 calc R . . C37 C -0.4178(4) 0.4069(2) 0.3172(2) 0.0481(8) Uani 1 1 d . . . H37 H -0.3686 0.4708 0.3135 0.058 Uiso 1 1 calc R . . C38 C -0.4575(4) 0.3482(3) 0.2483(2) 0.0535(9) Uani 1 1 d . . . H38 H -0.4343 0.3711 0.1970 0.064 Uiso 1 1 calc R . . C39 C -0.5315(4) 0.2554(3) 0.25463(19) 0.0481(8) Uani 1 1 d . . . H39 H -0.5589 0.2148 0.2076 0.058 Uiso 1 1 calc R . . C40 C -0.5653(3) 0.2221(2) 0.32987(17) 0.0362(6) Uani 1 1 d . . . H40 H -0.6181 0.1592 0.3329 0.043 Uiso 1 1 calc R . . O1 O -0.2601(3) 0.34889(18) -0.09763(15) 0.0522(6) Uani 1 1 d . . . C19 C -0.3582(4) 0.3827(3) -0.0450(3) 0.0633(10) Uani 1 1 d . . . H19A H -0.3144 0.4389 -0.0096 0.076 Uiso 1 1 calc R . . H19B H -0.4019 0.3308 -0.0114 0.076 Uiso 1 1 calc R . . C20 C -0.4606(4) 0.4112(4) -0.1002(3) 0.0775(14) Uani 1 1 d . . . H20A H -0.4918 0.4701 -0.0776 0.093 Uiso 1 1 calc R . . H20B H -0.5406 0.3584 -0.1083 0.093 Uiso 1 1 calc R . . C21 C -0.3878(5) 0.4303(3) -0.1792(3) 0.0676(12) Uani 1 1 d . . . H21A H -0.4353 0.3877 -0.2239 0.081 Uiso 1 1 calc R . . H21B H -0.3816 0.4986 -0.1918 0.081 Uiso 1 1 calc R . . C22 C -0.2476(4) 0.4072(3) -0.1640(2) 0.0593(10) Uani 1 1 d . . . H22A H -0.2167 0.3720 -0.2118 0.071 Uiso 1 1 calc R . . H22B H -0.1807 0.4675 -0.1518 0.071 Uiso 1 1 calc R . . O2 O -0.0540(3) 0.3606(2) 0.40564(17) 0.0593(7) Uani 1 1 d . B . C45 C -0.0181(7) 0.4208(4) 0.3419(3) 0.0849(16) Uani 1 1 d . . . H45A H -0.0376 0.4867 0.3541 0.102 Uiso 1 1 calc R A 1 H45B H -0.0642 0.3928 0.2909 0.102 Uiso 1 1 calc R A 1 C46 C 0.152(3) 0.4201(17) 0.3400(14) 0.078(7) Uani 0.56(5) 1 d P B 1 H46A H 0.1726 0.3610 0.3106 0.094 Uiso 0.56(5) 1 calc PR B 1 H46B H 0.2033 0.4779 0.3157 0.094 Uiso 0.56(5) 1 calc PR B 1 C46A C 0.107(3) 0.4337(19) 0.3218(17) 0.067(5) Uani 0.44(5) 1 d P B 2 H46C H 0.1421 0.5022 0.3117 0.081 Uiso 0.44(5) 1 calc PR B 2 H46D H 0.1210 0.3921 0.2735 0.081 Uiso 0.44(5) 1 calc PR B 2 C47 C 0.184(2) 0.4216(12) 0.4277(14) 0.067(4) Uani 0.56(5) 1 d P B 1 H47A H 0.2601 0.3871 0.4374 0.081 Uiso 0.56(5) 1 calc PR B 1 H47B H 0.2077 0.4887 0.4519 0.081 Uiso 0.56(5) 1 calc PR B 1 C47A C 0.178(2) 0.403(3) 0.398(3) 0.099(12) Uani 0.44(5) 1 d P B 2 H47C H 0.2452 0.4583 0.4217 0.119 Uiso 0.44(5) 1 calc PR B 2 H47D H 0.2252 0.3487 0.3833 0.119 Uiso 0.44(5) 1 calc PR B 2 C48 C 0.0593(4) 0.3723(4) 0.4585(3) 0.0782(14) Uani 1 1 d . . . H48A H 0.0725 0.3075 0.4730 0.094 Uiso 1 1 calc R B 1 H48B H 0.0382 0.4084 0.5084 0.094 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0278(3) 0.0351(3) 0.0329(3) 0.0019(2) -0.0065(2) 0.0027(2) K2 0.0344(3) 0.0430(4) 0.0341(3) 0.0023(3) 0.0061(2) 0.0161(3) Si1 0.0210(3) 0.0235(3) 0.0222(3) 0.0019(3) -0.0003(2) 0.0008(3) Si2 0.0227(3) 0.0250(3) 0.0185(3) 0.0003(2) 0.0013(2) 0.0064(3) C1 0.0229(11) 0.0213(11) 0.0173(11) 0.0005(9) 0.0006(9) 0.0025(9) C2 0.0229(11) 0.0207(11) 0.0163(11) 0.0010(9) 0.0001(8) 0.0037(9) C3 0.0429(17) 0.0398(17) 0.0365(16) -0.0074(13) -0.0014(13) -0.0093(13) C4 0.0234(13) 0.0440(17) 0.0416(16) 0.0125(13) 0.0036(11) 0.0060(12) C5 0.0195(11) 0.0268(13) 0.0307(13) 0.0066(10) 0.0032(10) -0.0004(10) C6 0.0352(15) 0.0379(15) 0.0311(14) 0.0056(11) 0.0080(11) 0.0071(12) C7 0.0510(19) 0.063(2) 0.0295(16) 0.0080(14) 0.0036(13) 0.0101(16) C8 0.054(2) 0.063(2) 0.0382(18) 0.0255(16) -0.0016(15) 0.0069(17) C9 0.0507(19) 0.0389(17) 0.057(2) 0.0218(15) -0.0042(16) 0.0075(14) C10 0.0367(15) 0.0284(14) 0.0411(16) 0.0074(12) 0.0000(12) 0.0029(12) C11 0.0456(17) 0.0289(14) 0.0378(16) -0.0051(12) 0.0020(13) 0.0137(12) C12 0.0246(13) 0.0425(16) 0.0264(13) 0.0028(11) 0.0002(10) 0.0094(11) C13 0.0283(13) 0.0301(13) 0.0185(11) -0.0007(9) 0.0033(9) 0.0091(10) C14 0.0334(14) 0.0348(14) 0.0230(13) -0.0005(10) 0.0019(10) 0.0049(11) C15 0.0535(18) 0.0321(15) 0.0267(14) 0.0050(11) 0.0108(12) 0.0080(13) C16 0.0560(19) 0.0410(16) 0.0230(13) 0.0064(11) 0.0061(12) 0.0251(14) C17 0.0371(15) 0.0509(18) 0.0269(14) -0.0004(12) -0.0051(11) 0.0233(13) C18 0.0269(13) 0.0413(15) 0.0276(13) 0.0019(11) 0.0012(10) 0.0100(11) Si3 0.0211(3) 0.0245(3) 0.0185(3) 0.0006(2) -0.0014(2) 0.0026(3) Si4 0.0241(3) 0.0228(3) 0.0233(3) 0.0019(3) -0.0002(3) 0.0075(3) C23 0.0243(12) 0.0205(11) 0.0184(11) 0.0006(9) -0.0031(9) 0.0059(9) C24 0.0232(11) 0.0214(11) 0.0180(11) 0.0021(9) -0.0012(9) 0.0053(9) C25 0.0376(15) 0.0292(14) 0.0364(15) -0.0033(11) -0.0013(12) -0.0023(12) C26 0.0230(12) 0.0414(15) 0.0291(13) 0.0030(11) 0.0014(10) 0.0062(11) C27 0.0235(12) 0.0266(12) 0.0180(11) 0.0005(9) -0.0043(9) 0.0010(9) C28 0.0362(14) 0.0328(14) 0.0228(12) 0.0000(10) -0.0035(10) 0.0091(11) C29 0.0517(18) 0.0342(15) 0.0277(14) 0.0066(11) -0.0114(12) 0.0046(13) C30 0.0381(15) 0.0420(16) 0.0234(13) 0.0072(11) -0.0032(11) -0.0098(12) C31 0.0289(14) 0.0499(18) 0.0274(14) 0.0020(12) 0.0048(11) -0.0013(12) C32 0.0244(12) 0.0409(15) 0.0280(13) 0.0049(11) -0.0012(10) 0.0060(11) C33 0.0492(18) 0.0366(16) 0.0351(15) -0.0033(12) -0.0007(13) 0.0200(14) C34 0.0254(13) 0.0403(16) 0.0508(18) 0.0131(13) 0.0005(12) 0.0083(12) C35 0.0256(12) 0.0287(13) 0.0289(13) 0.0065(10) -0.0010(10) 0.0119(10) C36 0.0408(16) 0.0292(14) 0.0395(16) 0.0075(12) 0.0029(12) 0.0095(12) C37 0.054(2) 0.0412(18) 0.053(2) 0.0215(15) 0.0122(16) 0.0127(15) C38 0.067(2) 0.065(2) 0.0365(18) 0.0252(16) 0.0107(16) 0.0240(19) C39 0.058(2) 0.060(2) 0.0298(15) 0.0048(14) -0.0057(14) 0.0202(17) C40 0.0419(16) 0.0382(16) 0.0298(14) 0.0037(12) -0.0071(12) 0.0100(13) O1 0.0596(15) 0.0496(14) 0.0528(14) 0.0069(11) 0.0070(11) 0.0233(12) C19 0.064(2) 0.060(2) 0.070(3) 0.014(2) 0.024(2) 0.0187(19) C20 0.037(2) 0.073(3) 0.124(4) 0.020(3) 0.007(2) 0.0088(19) C21 0.081(3) 0.067(3) 0.060(2) -0.011(2) -0.021(2) 0.034(2) C22 0.079(3) 0.061(2) 0.044(2) 0.0042(17) 0.0079(18) 0.030(2) O2 0.0490(14) 0.0633(16) 0.0642(17) 0.0111(13) -0.0038(12) 0.0039(12) C45 0.126(5) 0.074(3) 0.050(3) 0.014(2) -0.017(3) 0.000(3) C46 0.110(16) 0.054(7) 0.062(11) 0.004(7) 0.042(10) -0.009(9) C46A 0.091(13) 0.046(8) 0.058(9) 0.001(6) 0.005(9) -0.004(8) C47 0.059(7) 0.048(5) 0.095(11) 0.028(6) -0.006(7) 0.003(4) C47A 0.032(7) 0.13(2) 0.14(3) 0.06(2) 0.013(12) 0.011(9) C48 0.053(2) 0.101(4) 0.085(3) 0.036(3) -0.004(2) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 C1 3.016(2) . ? K1 C2 3.251(2) . ? K1 C5 3.061(2) . ? K1 C6 3.246(3) . ? K1 C10 3.292(3) . ? K1 C28 3.284(3) 1_554 ? K1 C29 3.111(3) 1_554 ? K1 C30 3.152(3) 1_554 ? K1 C31 3.352(3) 1_554 ? K1 C32 3.535(3) 1_554 ? K1 O1 2.706(2) . ? K1 C22 3.444(4) . ? K2 C14 3.298(3) . ? K2 C15 3.123(3) . ? K2 C16 3.137(3) . ? K2 C17 3.319(3) . ? K2 C18 3.512(3) . ? K2 C23 3.047(2) . ? K2 C24 3.370(2) . ? K2 C35 3.032(3) . ? K2 C36 3.272(3) . ? K2 C40 3.187(3) . ? K2 O2 2.730(3) . ? Si1 C1 1.810(2) . ? Si1 C3 1.891(3) . ? Si1 C4 1.894(3) . ? Si1 C5 1.927(3) . ? Si2 C1 1.803(2) . ? Si2 C11 1.902(3) . ? Si2 C12 1.904(3) . ? Si2 C13 1.926(3) . ? C1 C2 1.546(3) . ? C2 C2 1.566(4) 2 ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 C6 1.412(4) . ? C5 C10 1.401(4) . ? C6 H6 0.950 . ? C6 C7 1.396(4) . ? C7 H7 0.950 . ? C7 C8 1.390(5) . ? C8 H8 0.950 . ? C8 C9 1.377(5) . ? C9 H9 0.950 . ? C9 C10 1.407(4) . ? C10 H10 0.950 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 C14 1.410(4) . ? C13 C18 1.406(4) . ? C14 H14 0.950 . ? C14 C15 1.400(4) . ? C15 H15 0.950 . ? C15 C16 1.383(4) . ? C16 H16 0.950 . ? C16 C17 1.397(5) . ? C17 H17 0.950 . ? C17 C18 1.394(4) . ? C18 H18 0.950 . ? Si3 C23 1.802(2) . ? Si3 C25 1.900(3) . ? Si3 C26 1.904(3) . ? Si3 C27 1.928(2) . ? Si4 C23 1.805(2) . ? Si4 C33 1.892(3) . ? Si4 C34 1.897(3) . ? Si4 C35 1.928(3) . ? C23 C24 1.559(3) . ? C24 C24 1.553(4) 2_456 ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C27 K1 3.537(2) 1_556 ? C27 C28 1.408(4) . ? C27 C32 1.401(4) . ? C28 K1 3.284(3) 1_556 ? C28 H28 0.950 . ? C28 C29 1.400(4) . ? C29 K1 3.111(3) 1_556 ? C29 H29 0.950 . ? C29 C30 1.386(4) . ? C30 K1 3.152(3) 1_556 ? C30 H30 0.950 . ? C30 C31 1.395(4) . ? C31 K1 3.352(3) 1_556 ? C31 H31 0.950 . ? C31 C32 1.393(4) . ? C32 K1 3.535(3) 1_556 ? C32 H32 0.950 . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? C35 C36 1.410(4) . ? C35 C40 1.402(4) . ? C36 H36 0.950 . ? C36 C37 1.395(4) . ? C37 H37 0.950 . ? C37 C38 1.386(5) . ? C38 H38 0.950 . ? C38 C39 1.390(5) . ? C39 H39 0.950 . ? C39 C40 1.392(4) . ? C40 H40 0.950 . ? O1 C19 1.439(4) . ? O1 C22 1.416(4) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.499(6) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.524(7) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.517(6) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? O2 C45 1.413(5) . ? O2 C48 1.413(5) . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C45 C46 1.70(3) . ? C45 C46A 1.28(3) . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C46 C47 1.50(3) . ? C46A H46C 0.990 . ? C46A H46D 0.990 . ? C46A C47A 1.57(3) . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C47 C48 1.43(2) . ? C47A H47C 0.990 . ? C47A H47D 0.990 . ? C47A C48 1.58(3) . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? 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 K1 C2 28.25(6) . . ? C1 K1 C5 60.93(7) . . ? C1 K1 C6 74.61(7) . . ? C1 K1 C10 77.38(7) . . ? C1 K1 C28 124.86(7) . 1_554 ? C1 K1 C29 105.08(7) . 1_554 ? C1 K1 C30 105.00(7) . 1_554 ? C1 K1 C31 124.12(7) . 1_554 ? C1 K1 C32 146.41(7) . 1_554 ? C1 K1 O1 111.89(7) . . ? C1 K1 C22 129.46(8) . . ? C2 K1 C5 73.78(6) . . ? C2 K1 C6 75.29(7) . . ? C2 K1 C10 96.53(7) . . ? C2 K1 C28 96.61(6) . 1_554 ? C2 K1 C29 78.27(7) . 1_554 ? C2 K1 C30 84.65(7) . 1_554 ? C2 K1 C31 108.21(7) . 1_554 ? C2 K1 C32 125.25(6) . 1_554 ? C2 K1 O1 135.48(7) . . ? C2 K1 C22 156.58(8) . . ? C5 K1 C6 25.66(7) . . ? C5 K1 C10 25.15(7) . . ? C5 K1 C28 123.70(7) . 1_554 ? C5 K1 C29 131.94(8) . 1_554 ? C5 K1 C30 154.10(8) . 1_554 ? C5 K1 C31 172.48(7) . 1_554 ? C5 K1 C32 150.50(7) . 1_554 ? C5 K1 O1 106.95(8) . . ? C5 K1 C22 101.54(9) . . ? C6 K1 C10 42.75(8) . . ? C6 K1 C28 98.05(7) . 1_554 ? C6 K1 C29 109.37(8) . 1_554 ? C6 K1 C30 134.61(8) . 1_554 ? C6 K1 C31 147.07(8) . 1_554 ? C6 K1 C32 129.37(7) . 1_554 ? C6 K1 O1 124.40(8) . . ? C6 K1 C22 110.63(9) . . ? C10 K1 C28 132.30(8) . 1_554 ? C10 K1 C29 151.20(8) . 1_554 ? C10 K1 C30 176.17(8) . 1_554 ? C10 K1 C31 155.05(8) . 1_554 ? C10 K1 C32 136.06(7) . 1_554 ? C10 K1 O1 83.29(8) . . ? C10 K1 C22 76.41(9) . . ? C28 K1 C29 25.11(7) 1_554 1_554 ? C28 K1 C30 43.87(7) 1_554 1_554 ? C28 K1 C31 49.25(7) 1_554 1_554 ? C28 K1 C32 40.70(7) 1_554 1_554 ? C28 K1 O1 116.27(8) 1_554 . ? C28 K1 C22 104.65(9) 1_554 . ? C29 K1 C30 25.56(8) 1_554 1_554 ? C29 K1 C31 43.47(8) 1_554 1_554 ? C29 K1 C32 48.88(7) 1_554 1_554 ? C29 K1 O1 120.34(8) 1_554 . ? C29 K1 C22 118.41(9) 1_554 . ? C30 K1 C31 24.52(8) 1_554 1_554 ? C30 K1 C32 41.85(7) 1_554 1_554 ? C30 K1 O1 98.43(9) 1_554 . ? C30 K1 C22 103.89(10) 1_554 . ? C31 K1 C32 23.15(6) 1_554 1_554 ? C31 K1 O1 76.92(8) 1_554 . ? C31 K1 C22 79.50(10) 1_554 . ? C32 K1 O1 76.09(8) 1_554 . ? C32 K1 C22 69.56(9) 1_554 . ? O1 K1 C22 22.83(8) . . ? C14 K2 C15 25.00(7) . . ? C14 K2 C16 43.86(7) . . ? C14 K2 C17 49.56(7) . . ? C14 K2 C18 40.95(7) . . ? C14 K2 C23 122.15(7) . . ? C14 K2 C24 94.62(6) . . ? C14 K2 C35 121.56(7) . . ? C14 K2 C36 130.63(8) . . ? C14 K2 C40 95.69(7) . . ? C14 K2 O2 118.75(8) . . ? C15 K2 C16 25.53(8) . . ? C15 K2 C17 43.72(8) . . ? C15 K2 C18 49.06(8) . . ? C15 K2 C23 102.30(7) . . ? C15 K2 C24 76.09(7) . . ? C15 K2 C35 128.53(8) . . ? C15 K2 C36 148.18(9) . . ? C15 K2 C40 105.79(8) . . ? C15 K2 O2 123.95(9) . . ? C16 K2 C17 24.79(8) . . ? C16 K2 C18 42.11(7) . . ? C16 K2 C23 102.25(7) . . ? C16 K2 C24 82.21(7) . . ? C16 K2 C35 150.20(8) . . ? C16 K2 C36 173.71(8) . . ? C16 K2 C40 130.76(9) . . ? C16 K2 O2 102.45(9) . . ? C17 K2 C18 23.32(7) . . ? C17 K2 C23 121.83(7) . . ? C17 K2 C24 106.02(7) . . ? C17 K2 C35 171.12(8) . . ? C17 K2 C36 157.87(8) . . ? C17 K2 C40 145.24(8) . . ? C17 K2 O2 80.38(8) . . ? C18 K2 C23 144.04(7) . . ? C18 K2 C24 123.11(7) . . ? C18 K2 C35 151.28(7) . . ? C18 K2 C36 137.73(7) . . ? C18 K2 C40 129.02(7) . . ? C18 K2 O2 78.69(8) . . ? C23 K2 C24 27.54(6) . . ? C23 K2 C35 60.82(7) . . ? C23 K2 C36 78.23(7) . . ? C23 K2 C40 73.85(7) . . ? C23 K2 O2 112.97(8) . . ? C24 K2 C35 72.63(6) . . ? C24 K2 C36 96.09(7) . . ? C24 K2 C40 73.41(7) . . ? C24 K2 O2 136.67(7) . . ? C35 K2 C36 25.47(7) . . ? C35 K2 C40 25.90(7) . . ? C35 K2 O2 106.76(8) . . ? C36 K2 C40 43.17(8) . . ? C36 K2 O2 82.96(8) . . ? C40 K2 O2 124.69(8) . . ? C1 Si1 C3 118.58(13) . . ? C1 Si1 C4 114.36(12) . . ? C1 Si1 C5 111.06(11) . . ? C3 Si1 C4 104.15(15) . . ? C3 Si1 C5 103.91(13) . . ? C4 Si1 C5 103.18(12) . . ? C1 Si2 C11 115.36(13) . . ? C1 Si2 C12 113.98(11) . . ? C1 Si2 C13 115.33(11) . . ? C11 Si2 C12 103.80(13) . . ? C11 Si2 C13 103.36(12) . . ? C12 Si2 C13 103.48(12) . . ? K1 C1 Si1 95.73(9) . . ? K1 C1 Si2 96.21(9) . . ? K1 C1 C2 84.33(12) . . ? Si1 C1 Si2 124.80(13) . . ? Si1 C1 C2 115.57(16) . . ? Si2 C1 C2 119.14(16) . . ? K1 C2 C1 67.42(12) . . ? K1 C2 C2 174.1(2) . 2 ? K1 C2 H2A 72.7 . . ? K1 C2 H2B 66.5 . . ? C1 C2 C2 117.2(2) . 2 ? C1 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C2 C2 H2A 108.0 2 . ? C2 C2 H2B 108.0 2 . ? H2A C2 H2B 107.2 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? K1 C5 Si1 91.85(9) . . ? K1 C5 C6 84.52(16) . . ? K1 C5 C10 86.67(16) . . ? Si1 C5 C6 121.0(2) . . ? Si1 C5 C10 122.7(2) . . ? C6 C5 C10 115.8(3) . . ? K1 C6 C5 69.82(15) . . ? K1 C6 H6 105.7 . . ? K1 C6 C7 94.85(19) . . ? C5 C6 H6 118.9 . . ? C5 C6 C7 122.3(3) . . ? H6 C6 C7 118.9 . . ? C6 C7 H7 120.0 . . ? C6 C7 C8 120.1(3) . . ? H7 C7 C8 120.0 . . ? C7 C8 H8 120.3 . . ? C7 C8 C9 119.4(3) . . ? H8 C8 C9 120.3 . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.3(3) . . ? H9 C9 C10 119.9 . . ? K1 C10 C5 68.19(15) . . ? K1 C10 C9 95.33(19) . . ? K1 C10 H10 106.7 . . ? C5 C10 C9 122.2(3) . . ? C5 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 C14 123.86(19) . . ? Si2 C13 C18 119.9(2) . . ? C14 C13 C18 116.2(2) . . ? K2 C14 C13 88.03(15) . . ? K2 C14 H14 112.4 . . ? K2 C14 C15 70.52(15) . . ? C13 C14 H14 118.9 . . ? C13 C14 C15 122.2(3) . . ? H14 C14 C15 118.9 . . ? K2 C15 C14 84.48(17) . . ? K2 C15 H15 107.9 . . ? K2 C15 C16 77.79(17) . . ? C14 C15 H15 120.1 . . ? C14 C15 C16 119.8(3) . . ? H15 C15 C16 120.1 . . ? K2 C16 C15 76.68(17) . . ? K2 C16 H16 108.6 . . ? K2 C16 C17 84.90(17) . . ? C15 C16 H16 120.1 . . ? C15 C16 C17 119.8(3) . . ? H16 C16 C17 120.1 . . ? K2 C17 C16 70.31(16) . . ? K2 C17 H17 113.8 . . ? K2 C17 C18 86.15(16) . . ? C16 C17 H17 120.1 . . ? C16 C17 C18 119.8(3) . . ? H17 C17 C18 120.1 . . ? K2 C18 C13 79.68(15) . . ? K2 C18 C17 70.53(15) . . ? K2 C18 H18 122.0 . . ? C13 C18 C17 122.2(3) . . ? C13 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C23 Si3 C25 114.56(12) . . ? C23 Si3 C26 114.46(12) . . ? C23 Si3 C27 115.67(11) . . ? C25 Si3 C26 103.62(13) . . ? C25 Si3 C27 103.30(12) . . ? C26 Si3 C27 103.70(12) . . ? C23 Si4 C33 118.76(12) . . ? C23 Si4 C34 113.78(12) . . ? C23 Si4 C35 110.97(11) . . ? C33 Si4 C34 104.51(15) . . ? C33 Si4 C35 104.09(13) . . ? C34 Si4 C35 103.18(13) . . ? K2 C23 Si3 96.10(10) . . ? K2 C23 Si4 94.61(9) . . ? K2 C23 C24 87.87(13) . . ? Si3 C23 Si4 124.95(13) . . ? Si3 C23 C24 118.18(16) . . ? Si4 C23 C24 116.05(16) . . ? K2 C24 C23 64.59(12) . . ? K2 C24 C24 174.7(2) . 2_456 ? K2 C24 H24A 75.3 . . ? K2 C24 H24B 66.9 . . ? C23 C24 C24 117.3(2) . 2_456 ? C23 C24 H24A 108.0 . . ? C23 C24 H24B 108.0 . . ? C24 C24 H24A 108.0 2_456 . ? C24 C24 H24B 108.0 2_456 . ? H24A C24 H24B 107.2 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? K1 C27 Si3 125.77(10) 1_556 . ? K1 C27 C28 68.13(14) 1_556 . ? K1 C27 C32 78.49(14) 1_556 . ? Si3 C27 C28 124.10(19) . . ? Si3 C27 C32 119.69(19) . . ? C28 C27 C32 116.1(2) . . ? K1 C28 C27 88.43(15) 1_556 . ? K1 C28 H28 112.0 1_556 . ? K1 C28 C29 70.53(16) 1_556 . ? C27 C28 H28 118.8 . . ? C27 C28 C29 122.4(3) . . ? H28 C28 C29 118.8 . . ? K1 C29 C28 84.36(17) 1_556 . ? K1 C29 H29 106.8 1_556 . ? K1 C29 C30 78.87(17) 1_556 . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.5(3) . . ? H29 C29 C30 120.2 . . ? K1 C30 C29 75.57(17) 1_556 . ? K1 C30 H30 108.7 1_556 . ? K1 C30 C31 85.79(17) 1_556 . ? C29 C30 H30 120.2 . . ? C29 C30 C31 119.6(3) . . ? H30 C30 C31 120.2 . . ? K1 C31 C30 69.69(16) 1_556 . ? K1 C31 H31 114.8 1_556 . ? K1 C31 C32 85.82(16) 1_556 . ? C30 C31 H31 120.0 . . ? C30 C31 C32 120.0(3) . . ? H31 C31 C32 120.0 . . ? K1 C32 C27 78.66(14) 1_556 . ? K1 C32 C31 71.04(15) 1_556 . ? K1 C32 H32 122.7 1_556 . ? C27 C32 C31 122.3(3) . . ? C27 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? Si4 C33 H33A 109.5 . . ? Si4 C33 H33B 109.5 . . ? Si4 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si4 C34 H34A 109.5 . . ? Si4 C34 H34B 109.5 . . ? Si4 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? K2 C35 Si4 92.50(9) . . ? K2 C35 C36 86.81(16) . . ? K2 C35 C40 83.20(16) . . ? Si4 C35 C36 122.9(2) . . ? Si4 C35 C40 121.1(2) . . ? C36 C35 C40 115.5(3) . . ? K2 C36 C35 67.71(15) . . ? K2 C36 H36 109.0 . . ? K2 C36 C37 93.93(19) . . ? C35 C36 H36 118.6 . . ? C35 C36 C37 122.8(3) . . ? H36 C36 C37 118.6 . . ? C36 C37 H37 120.3 . . ? C36 C37 C38 119.5(3) . . ? H37 C37 C38 120.3 . . ? C37 C38 H38 120.2 . . ? C37 C38 C39 119.6(3) . . ? H38 C38 C39 120.2 . . ? C38 C39 H39 120.0 . . ? C38 C39 C40 120.0(3) . . ? H39 C39 C40 120.0 . . ? K2 C40 C35 70.89(15) . . ? K2 C40 C39 92.9(2) . . ? K2 C40 H40 106.7 . . ? C35 C40 C39 122.5(3) . . ? C35 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? K1 O1 C19 142.6(2) . . ? K1 O1 C22 109.30(19) . . ? C19 O1 C22 106.7(3) . . ? O1 C19 H19A 110.8 . . ? O1 C19 H19B 110.8 . . ? O1 C19 C20 104.7(3) . . ? H19A C19 H19B 108.9 . . ? H19A C19 C20 110.8 . . ? H19B C19 C20 110.8 . . ? C19 C20 H20A 110.5 . . ? C19 C20 H20B 110.5 . . ? C19 C20 C21 106.0(3) . . ? H20A C20 H20B 108.7 . . ? H20A C20 C21 110.5 . . ? H20B C20 C21 110.5 . . ? C20 C21 H21A 111.1 . . ? C20 C21 H21B 111.1 . . ? C20 C21 C22 103.4(3) . . ? H21A C21 H21B 109.0 . . ? H21A C21 C22 111.1 . . ? H21B C21 C22 111.1 . . ? K1 C22 O1 47.87(15) . . ? K1 C22 C21 133.7(3) . . ? K1 C22 H22A 64.0 . . ? K1 C22 H22B 114.7 . . ? O1 C22 C21 106.5(3) . . ? O1 C22 H22A 110.4 . . ? O1 C22 H22B 110.4 . . ? C21 C22 H22A 110.4 . . ? C21 C22 H22B 110.4 . . ? H22A C22 H22B 108.6 . . ? K2 O2 C45 115.1(3) . . ? K2 O2 C48 131.0(3) . . ? C45 O2 C48 108.0(3) . . ? O2 C45 H45A 112.0 . . ? O2 C45 H45B 112.0 . . ? O2 C45 C46 99.0(9) . . ? O2 C45 C46A 115.9(13) . . ? H45A C45 H45B 109.6 . . ? H45A C45 C46 112.0 . . ? H45A C45 C46A 105.1 . . ? H45B C45 C46 112.0 . . ? H45B C45 C46A 101.6 . . ? C45 C46 H46A 111.6 . . ? C45 C46 H46B 111.6 . . ? C45 C46 C47 100.9(14) . . ? H46A C46 H46B 109.4 . . ? H46A C46 C47 111.6 . . ? H46B C46 C47 111.6 . . ? C45 C46A H46C 111.3 . . ? C45 C46A H46D 111.3 . . ? C45 C46A C47A 102.2(18) . . ? H46C C46A H46D 109.2 . . ? H46C C46A C47A 111.3 . . ? H46D C46A C47A 111.3 . . ? C46 C47 H47A 111.3 . . ? C46 C47 H47B 111.3 . . ? C46 C47 C48 102.4(15) . . ? H47A C47 H47B 109.2 . . ? H47A C47 C48 111.3 . . ? H47B C47 C48 111.3 . . ? C46A C47A H47C 110.6 . . ? C46A C47A H47D 110.6 . . ? C46A C47A C48 105.8(17) . . ? H47C C47A H47D 108.7 . . ? H47C C47A C48 110.6 . . ? H47D C47A C48 110.6 . . ? O2 C48 C47 115.0(10) . . ? O2 C48 C47A 99.6(15) . . ? O2 C48 H48A 108.5 . . ? O2 C48 H48B 108.5 . . ? C47 C48 H48A 108.5 . . ? C47 C48 H48B 108.5 . . ? C47A C48 H48A 103.8 . . ? C47A C48 H48B 127.7 . . ? H48A C48 H48B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.225 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.100 #===END data_ki202_compound5 _database_code_depnum_ccdc_archive 'CCDC 713038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H96 B2 Li2 O6 P2 Si2, 2 C4 H8 O' _chemical_formula_sum 'C66 H112 B2 Li2 O8 P2 Si2' _chemical_formula_weight 1187.18 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' 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' Si Si 0.0817 0.0704 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3298(12) _cell_length_b 13.2276(13) _cell_length_c 15.0800(15) _cell_angle_alpha 106.405(8) _cell_angle_beta 108.263(7) _cell_angle_gamma 99.787(9) _cell_volume 1799.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 582 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39378 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6322 _reflns_number_gt 4956 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. The structure contains highly disordered uncoordinated THF molecules (two per molecule of the dinuclear complex), which could not be modelled with discrete atoms. This was treated by the SQUEEZE option of PLATON, and the disordered THF is included in the chemical formula and derived quantities. ; _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^)+(0.1314P)^2^+0.4330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.107(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6322 _refine_ls_number_parameters 371 _refine_ls_number_restraints 347 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1985 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.076 _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 P P 0.86849(6) 0.06888(5) 0.31069(4) 0.0219(2) Uani 1 1 d . . . Si Si 0.91045(7) -0.16412(5) 0.27422(5) 0.0267(2) Uani 1 1 d . . . B B 0.8965(3) 0.2123(2) 0.4080(2) 0.0272(6) Uani 1 1 d . . . H1A H 0.841(3) 0.203(2) 0.461(2) 0.052(9) Uiso 1 1 d . . . H1B H 0.846(3) 0.259(2) 0.364(2) 0.036(7) Uiso 1 1 d . . . H1C H 1.009(3) 0.249(2) 0.446(2) 0.034(7) Uiso 1 1 d . . . Li Li 0.7056(5) 0.3004(4) 0.4188(3) 0.0352(10) Uani 1 1 d . A . O1 O 0.5973(2) 0.33566(16) 0.30252(15) 0.0455(5) Uani 1 1 d U . . O2 O 0.5492(2) 0.23459(18) 0.44843(16) 0.0475(5) Uani 1 1 d U . . O3 O 0.8050(2) 0.43961(16) 0.52696(15) 0.0504(6) Uani 1 1 d U . . C1 C 0.9425(2) -0.02268(19) 0.35410(16) 0.0244(5) Uani 1 1 d U . . C2 C 1.0370(2) 0.01521(19) 0.46650(16) 0.0237(5) Uani 1 1 d U . . H2A H 1.1179 -0.0168 0.4729 0.028 Uiso 1 1 calc R . . H2B H 1.0766 0.0961 0.4924 0.028 Uiso 1 1 calc R . . C3 C 1.0824(4) -0.1997(3) 0.2836(3) 0.0625(10) Uani 1 1 d . . . H3A H 1.1348 -0.1552 0.2570 0.094 Uiso 1 1 calc R . . H3B H 1.0616 -0.2778 0.2448 0.094 Uiso 1 1 calc R . . H3C H 1.1400 -0.1845 0.3538 0.094 Uiso 1 1 calc R . . C4 C 0.8095(4) -0.2743(2) 0.3043(2) 0.0540(9) Uani 1 1 d . . . H4A H 0.8625 -0.2690 0.3727 0.081 Uiso 1 1 calc R . . H4B H 0.7979 -0.3468 0.2573 0.081 Uiso 1 1 calc R . . H4C H 0.7157 -0.2643 0.2985 0.081 Uiso 1 1 calc R . . C5 C 0.8081(4) -0.1961(2) 0.1365(2) 0.0463(8) Uani 1 1 d . . . H5A H 0.7094 -0.1960 0.1253 0.069 Uiso 1 1 calc R . . H5B H 0.8099 -0.2687 0.0976 0.069 Uiso 1 1 calc R . . H5C H 0.8519 -0.1404 0.1154 0.069 Uiso 1 1 calc R . . C6 C 0.6732(2) 0.01309(19) 0.24243(18) 0.0257(5) Uani 1 1 d U . . C7 C 0.5978(3) -0.0171(2) 0.13956(19) 0.0341(6) Uani 1 1 d U . . H7 H 0.6479 -0.0087 0.0978 0.041 Uiso 1 1 calc R . . C8 C 0.4505(3) -0.0590(2) 0.0977(2) 0.0418(7) Uani 1 1 d U . . H8 H 0.4014 -0.0797 0.0276 0.050 Uiso 1 1 calc R . . C9 C 0.3743(3) -0.0709(2) 0.1573(2) 0.0422(7) Uani 1 1 d U . . H9 H 0.2736 -0.0982 0.1286 0.051 Uiso 1 1 calc R . . C10 C 0.4472(3) -0.0424(2) 0.2592(2) 0.0425(7) Uani 1 1 d U . . H10 H 0.3965 -0.0509 0.3006 0.051 Uiso 1 1 calc R . . C11 C 0.5946(3) -0.0015(2) 0.30081(19) 0.0346(6) Uani 1 1 d U . . H11 H 0.6432 0.0171 0.3707 0.042 Uiso 1 1 calc R . . C12 C 0.9266(2) 0.10381(19) 0.21542(17) 0.0259(5) Uani 1 1 d U . . C13 C 0.8695(3) 0.1715(2) 0.16725(18) 0.0331(6) Uani 1 1 d U . . H13 H 0.7940 0.1969 0.1798 0.040 Uiso 1 1 calc R . . C14 C 0.9218(3) 0.2026(2) 0.10063(19) 0.0408(7) Uani 1 1 d U . . H14 H 0.8812 0.2481 0.0682 0.049 Uiso 1 1 calc R . . C15 C 1.0318(3) 0.1674(2) 0.0823(2) 0.0452(7) Uani 1 1 d U . . H15 H 1.0670 0.1884 0.0371 0.054 Uiso 1 1 calc R . . C16 C 1.0918(3) 0.1008(2) 0.1300(2) 0.0412(7) Uani 1 1 d U . . H16 H 1.1679 0.0766 0.1174 0.049 Uiso 1 1 calc R . . C17 C 1.0399(3) 0.0697(2) 0.19619(18) 0.0319(6) Uani 1 1 d U . . H17 H 1.0818 0.0248 0.2288 0.038 Uiso 1 1 calc R . . C18 C 0.6296(4) 0.4380(3) 0.2870(3) 0.0619(10) Uani 0.74(2) 1 d PU A 1 H18A H 0.7261 0.4847 0.3341 0.074 Uiso 0.74(2) 1 calc PR A 1 H18B H 0.5600 0.4788 0.2964 0.074 Uiso 0.74(2) 1 calc PR A 1 C18A C 0.6296(4) 0.4380(3) 0.2870(3) 0.0619(10) Uani 0.26(2) 1 d PU A 2 H18C H 0.7324 0.4638 0.3016 0.074 Uiso 0.26(2) 1 calc PR A 2 H18D H 0.6041 0.4949 0.3316 0.074 Uiso 0.26(2) 1 calc PR A 2 C19 C 0.6202(13) 0.4054(7) 0.1796(6) 0.076(2) Uani 0.74(2) 1 d PU A 1 H19A H 0.5876 0.4583 0.1491 0.092 Uiso 0.74(2) 1 calc PR A 1 H19B H 0.7134 0.4014 0.1762 0.092 Uiso 0.74(2) 1 calc PR A 1 C19A C 0.545(5) 0.4178(19) 0.181(2) 0.093(7) Uani 0.26(2) 1 d PU A 2 H19C H 0.6005 0.4599 0.1535 0.112 Uiso 0.26(2) 1 calc PR A 2 H19D H 0.4562 0.4386 0.1741 0.112 Uiso 0.26(2) 1 calc PR A 2 C20 C 0.5147(6) 0.2958(4) 0.1289(3) 0.0953(15) Uani 0.74(2) 1 d PU A 1 H20A H 0.5490 0.2444 0.0861 0.114 Uiso 0.74(2) 1 calc PR A 1 H20B H 0.4231 0.3010 0.0863 0.114 Uiso 0.74(2) 1 calc PR A 1 C20A C 0.5147(6) 0.2958(4) 0.1289(3) 0.0953(15) Uani 0.26(2) 1 d PU A 2 H20C H 0.4271 0.2662 0.0675 0.114 Uiso 0.26(2) 1 calc PR A 2 H20D H 0.5952 0.2773 0.1122 0.114 Uiso 0.26(2) 1 calc PR A 2 C21 C 0.4964(4) 0.2560(3) 0.2089(3) 0.0650(10) Uani 1 1 d U A . H21A H 0.3984 0.2492 0.2068 0.078 Uiso 1 1 calc R B 1 H21B H 0.5141 0.1832 0.1995 0.078 Uiso 1 1 calc R B 1 C22 C 0.4033(3) 0.2300(3) 0.4010(3) 0.0613(10) Uani 1 1 d U A . H22A H 0.3486 0.1590 0.3456 0.074 Uiso 1 1 calc R C 1 H22B H 0.3936 0.2913 0.3763 0.074 Uiso 1 1 calc R C 1 C23 C 0.358(2) 0.2431(19) 0.497(2) 0.063(4) Uani 0.299(18) 1 d PU A 1 H23A H 0.3601 0.3204 0.5273 0.075 Uiso 0.299(18) 1 calc PR A 1 H23B H 0.2599 0.1964 0.4741 0.075 Uiso 0.299(18) 1 calc PR A 1 C23A C 0.3251(10) 0.1963(12) 0.4605(9) 0.077(3) Uani 0.701(18) 1 d PU A 2 H23C H 0.3065 0.2603 0.5022 0.093 Uiso 0.701(18) 1 calc PR A 2 H23D H 0.2333 0.1403 0.4160 0.093 Uiso 0.701(18) 1 calc PR A 2 C24 C 0.4317(18) 0.219(2) 0.5549(15) 0.068(4) Uani 0.299(18) 1 d PU A 1 H24A H 0.3786 0.1513 0.5583 0.082 Uiso 0.299(18) 1 calc PR A 1 H24B H 0.4640 0.2780 0.6212 0.082 Uiso 0.299(18) 1 calc PR A 1 C24A C 0.4191(7) 0.1503(10) 0.5238(7) 0.067(2) Uani 0.701(18) 1 d PU A 2 H24C H 0.3911 0.0692 0.4928 0.080 Uiso 0.701(18) 1 calc PR A 2 H24D H 0.4137 0.1703 0.5907 0.080 Uiso 0.701(18) 1 calc PR A 2 C25 C 0.5648(4) 0.1982(4) 0.5322(3) 0.0671(10) Uani 1 1 d U A . H25A H 0.6545 0.2424 0.5899 0.081 Uiso 1 1 calc R D 1 H25B H 0.5614 0.1195 0.5135 0.081 Uiso 1 1 calc R D 1 C26 C 0.9458(3) 0.4689(3) 0.6023(2) 0.0591(9) Uani 1 1 d U A . H26A H 1.0144 0.5200 0.5902 0.071 Uiso 1 1 calc R . . H26B H 0.9782 0.4027 0.6026 0.071 Uiso 1 1 calc R . . C27 C 0.9318(5) 0.5226(3) 0.6979(3) 0.0788(13) Uani 1 1 d U . . H27A H 1.0218 0.5782 0.7468 0.095 Uiso 1 1 calc R A . H27B H 0.9057 0.4678 0.7271 0.095 Uiso 1 1 calc R . . C28 C 0.8141(4) 0.5763(3) 0.6697(3) 0.0703(11) Uani 1 1 d U A . H28A H 0.7511 0.5681 0.7065 0.084 Uiso 1 1 calc R . . H28B H 0.8541 0.6555 0.6847 0.084 Uiso 1 1 calc R . . C29 C 0.7360(5) 0.5178(3) 0.5618(3) 0.0859(15) Uani 1 1 d U A . H29A H 0.6367 0.4799 0.5482 0.103 Uiso 1 1 calc R . . H29B H 0.7342 0.5706 0.5265 0.103 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 P 0.0228(3) 0.0248(3) 0.0179(3) 0.0087(2) 0.0064(2) 0.0066(2) Si 0.0303(4) 0.0252(4) 0.0227(4) 0.0078(3) 0.0076(3) 0.0087(3) B 0.0286(15) 0.0255(14) 0.0274(14) 0.0086(12) 0.0109(12) 0.0080(12) Li 0.031(2) 0.036(2) 0.035(2) 0.0113(19) 0.0086(19) 0.0113(19) O1 0.0429(11) 0.0419(11) 0.0420(11) 0.0194(9) 0.0031(9) 0.0063(9) O2 0.0317(10) 0.0679(14) 0.0558(13) 0.0349(11) 0.0193(9) 0.0194(10) O3 0.0439(12) 0.0427(11) 0.0451(12) -0.0020(9) 0.0052(10) 0.0170(9) C1 0.0277(12) 0.0264(12) 0.0176(11) 0.0094(9) 0.0050(10) 0.0084(10) C2 0.0214(11) 0.0277(12) 0.0191(11) 0.0091(10) 0.0043(10) 0.0049(9) C3 0.0463(19) 0.053(2) 0.077(2) 0.0074(18) 0.0178(18) 0.0257(16) C4 0.077(2) 0.0368(16) 0.0419(17) 0.0110(14) 0.0256(16) 0.0003(15) C5 0.069(2) 0.0338(15) 0.0255(14) 0.0051(12) 0.0092(14) 0.0140(14) C6 0.0274(12) 0.0243(12) 0.0251(12) 0.0117(10) 0.0063(10) 0.0091(10) C7 0.0334(14) 0.0369(14) 0.0264(13) 0.0127(11) 0.0052(11) 0.0056(11) C8 0.0376(15) 0.0414(16) 0.0315(14) 0.0140(12) -0.0032(12) 0.0045(12) C9 0.0246(13) 0.0418(16) 0.0479(17) 0.0130(13) 0.0033(12) 0.0043(12) C10 0.0336(15) 0.0478(17) 0.0454(16) 0.0168(14) 0.0166(13) 0.0065(13) C11 0.0317(14) 0.0396(15) 0.0286(13) 0.0124(11) 0.0088(11) 0.0053(11) C12 0.0272(12) 0.0257(12) 0.0199(11) 0.0075(10) 0.0063(10) 0.0021(10) C13 0.0333(14) 0.0347(14) 0.0280(13) 0.0140(11) 0.0068(11) 0.0067(11) C14 0.0545(18) 0.0358(15) 0.0268(14) 0.0177(12) 0.0088(13) 0.0014(13) C15 0.0594(19) 0.0413(16) 0.0280(14) 0.0110(12) 0.0199(14) -0.0066(14) C16 0.0410(16) 0.0440(16) 0.0370(15) 0.0090(13) 0.0221(13) 0.0037(13) C17 0.0319(13) 0.0327(13) 0.0278(13) 0.0096(11) 0.0101(11) 0.0056(11) C18 0.072(2) 0.0460(18) 0.0539(19) 0.0226(15) 0.0105(17) 0.0019(16) C18A 0.072(2) 0.0460(18) 0.0539(19) 0.0226(15) 0.0105(17) 0.0019(16) C19 0.091(6) 0.081(4) 0.059(3) 0.036(3) 0.027(4) 0.013(4) C19A 0.110(14) 0.078(7) 0.075(9) 0.046(6) 0.001(11) 0.017(11) C20 0.129(4) 0.084(3) 0.047(2) 0.021(2) 0.004(2) 0.027(3) C20A 0.129(4) 0.084(3) 0.047(2) 0.021(2) 0.004(2) 0.027(3) C21 0.064(2) 0.0500(19) 0.051(2) 0.0093(16) -0.0007(17) 0.0001(16) C22 0.0336(16) 0.087(3) 0.083(2) 0.055(2) 0.0232(17) 0.0220(17) C23 0.046(9) 0.078(10) 0.118(11) 0.072(9) 0.058(8) 0.036(8) C23A 0.042(4) 0.124(9) 0.093(6) 0.073(6) 0.030(4) 0.022(5) C24 0.071(8) 0.086(12) 0.086(8) 0.052(8) 0.054(7) 0.033(8) C24A 0.065(3) 0.082(5) 0.097(5) 0.064(5) 0.051(3) 0.033(4) C25 0.0489(19) 0.114(3) 0.060(2) 0.052(2) 0.0241(17) 0.032(2) C26 0.0406(17) 0.057(2) 0.053(2) -0.0017(16) 0.0040(15) 0.0124(15) C27 0.099(3) 0.076(3) 0.045(2) 0.0062(18) 0.007(2) 0.048(2) C28 0.077(3) 0.067(2) 0.053(2) 0.0010(18) 0.0187(19) 0.035(2) C29 0.074(3) 0.071(3) 0.074(3) -0.014(2) 0.000(2) 0.047(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P B 1.952(3) . ? P C1 1.711(2) . ? P C6 1.854(2) . ? P C12 1.860(2) . ? Si C1 1.824(2) . ? Si C3 1.887(3) . ? Si C4 1.890(3) . ? Si C5 1.893(3) . ? B H1A 1.13(3) . ? B H1B 1.10(3) . ? B H1C 1.08(3) . ? B Li 2.480(5) . ? Li H1A 2.13(3) . ? Li H1B 1.97(3) . ? Li O1 1.989(5) . ? Li O2 1.940(5) . ? Li O3 1.927(5) . ? O1 C18 1.440(4) . ? O1 C21 1.433(4) . ? O2 C22 1.433(4) . ? O2 C25 1.447(4) . ? O3 C26 1.442(4) . ? O3 C29 1.426(4) . ? C1 C2 1.547(3) . ? C2 C2 1.541(4) 2_756 ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 C7 1.400(3) . ? C6 C11 1.401(4) . ? C7 H7 0.950 . ? C7 C8 1.391(4) . ? C8 H8 0.950 . ? C8 C9 1.391(4) . ? C9 H9 0.950 . ? C9 C10 1.386(4) . ? C10 H10 0.950 . ? C10 C11 1.390(4) . ? C11 H11 0.950 . ? C12 C13 1.399(3) . ? C12 C17 1.405(4) . ? C13 H13 0.950 . ? C13 C14 1.403(4) . ? C14 H14 0.950 . ? C14 C15 1.375(4) . ? C15 H15 0.950 . ? C15 C16 1.393(4) . ? C16 H16 0.950 . ? C16 C17 1.395(4) . ? C17 H17 0.950 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.520(8) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.479(9) . ? C19A H19C 0.990 . ? C19A H19D 0.990 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.495(6) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.63(3) . ? C22 C23A 1.489(11) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.13(3) . ? C23A H23C 0.990 . ? C23A H23D 0.990 . ? C23A C24A 1.473(12) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 C25 1.567(16) . ? C24A H24C 0.990 . ? C24A H24D 0.990 . ? C24A C25 1.482(7) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.481(5) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.518(5) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.467(5) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? 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 B P C1 117.88(12) . . ? B P C6 104.89(12) . . ? B P C12 103.40(11) . . ? C1 P C6 112.15(11) . . ? C1 P C12 114.77(11) . . ? C6 P C12 102.04(10) . . ? C1 Si C3 111.49(13) . . ? C1 Si C4 115.96(13) . . ? C1 Si C5 114.43(12) . . ? C3 Si C4 103.50(18) . . ? C3 Si C5 106.02(16) . . ? C4 Si C5 104.36(15) . . ? P B H1A 110.7(15) . . ? P B H1B 105.6(14) . . ? P B H1C 106.8(14) . . ? P B Li 125.05(17) . . ? H1A B H1B 109(2) . . ? H1A B H1C 113(2) . . ? H1A B Li 58.8(15) . . ? H1B B H1C 111.3(19) . . ? H1B B Li 50.4(14) . . ? H1C B Li 127.4(14) . . ? B Li H1A 27.1(8) . . ? B Li H1B 25.6(8) . . ? B Li O1 118.7(2) . . ? B Li O2 121.7(2) . . ? B Li O3 103.7(2) . . ? H1A Li H1B 52.7(11) . . ? H1A Li O1 142.5(9) . . ? H1A Li O2 97.9(9) . . ? H1A Li O3 100.7(8) . . ? H1B Li O1 94.3(8) . . ? H1B Li O2 140.3(8) . . ? H1B Li O3 105.7(8) . . ? O1 Li O2 99.6(2) . . ? O1 Li O3 105.9(2) . . ? O2 Li O3 105.9(2) . . ? Li O1 C18 126.5(2) . . ? Li O1 C21 124.9(2) . . ? C18 O1 C21 107.0(2) . . ? Li O2 C22 125.3(2) . . ? Li O2 C25 124.8(2) . . ? C22 O2 C25 109.2(2) . . ? Li O3 C26 126.6(2) . . ? Li O3 C29 123.5(2) . . ? C26 O3 C29 107.7(2) . . ? P C1 Si 122.77(13) . . ? P C1 C2 118.55(16) . . ? Si C1 C2 118.66(16) . . ? C1 C2 C2 115.9(2) . 2_756 ? C1 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? C2 C2 H2A 108.3 2_756 . ? C2 C2 H2B 108.3 2_756 . ? H2A C2 H2B 107.4 . . ? Si C3 H3A 109.5 . . ? Si C3 H3B 109.5 . . ? Si C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si C4 H4A 109.5 . . ? Si C4 H4B 109.5 . . ? Si C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si C5 H5A 109.5 . . ? Si C5 H5B 109.5 . . ? Si C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P C6 C7 126.88(19) . . ? P C6 C11 115.76(18) . . ? C7 C6 C11 117.4(2) . . ? C6 C7 H7 119.5 . . ? C6 C7 C8 121.0(3) . . ? H7 C7 C8 119.5 . . ? C7 C8 H8 119.7 . . ? C7 C8 C9 120.7(3) . . ? H8 C8 C9 119.7 . . ? C8 C9 H9 120.4 . . ? C8 C9 C10 119.2(2) . . ? H9 C9 C10 120.4 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.1(3) . . ? H10 C10 C11 120.0 . . ? C6 C11 C10 121.7(2) . . ? C6 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? P C12 C13 122.22(19) . . ? P C12 C17 119.86(18) . . ? C13 C12 C17 117.7(2) . . ? C12 C13 H13 119.5 . . ? C12 C13 C14 121.1(3) . . ? H13 C13 C14 119.5 . . ? C13 C14 H14 119.9 . . ? C13 C14 C15 120.1(3) . . ? H14 C14 C15 119.9 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0(2) . . ? H15 C15 C16 120.0 . . ? C15 C16 H16 120.0 . . ? C15 C16 C17 120.0(3) . . ? H16 C16 C17 120.0 . . ? C12 C17 C16 121.1(2) . . ? C12 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? O1 C18 H18A 110.8 . . ? O1 C18 H18B 110.8 . . ? O1 C18 C19 104.9(4) . . ? H18A C18 H18B 108.8 . . ? H18A C18 C19 110.8 . . ? H18B C18 C19 110.8 . . ? C18 C19 H19A 111.0 . . ? C18 C19 H19B 111.0 . . ? C18 C19 C20 103.7(5) . . ? H19A C19 H19B 109.0 . . ? H19A C19 C20 111.0 . . ? H19B C19 C20 111.0 . . ? H19C C19A H19D 108.9 . . ? C19 C20 H20A 110.3 . . ? C19 C20 H20B 110.3 . . ? C19 C20 C21 107.1(4) . . ? H20A C20 H20B 108.6 . . ? H20A C20 C21 110.3 . . ? H20B C20 C21 110.3 . . ? O1 C21 C20 106.8(3) . . ? O1 C21 H21A 110.4 . . ? O1 C21 H21B 110.4 . . ? C20 C21 H21A 110.4 . . ? C20 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? O2 C22 H22A 112.1 . . ? O2 C22 H22B 112.1 . . ? O2 C22 C23 98.2(9) . . ? O2 C22 C23A 107.7(4) . . ? H22A C22 H22B 109.8 . . ? H22A C22 C23 112.1 . . ? H22A C22 C23A 88.6 . . ? H22B C22 C23 112.1 . . ? H22B C22 C23A 124.3 . . ? C22 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C22 C23 C24 111.9(17) . . ? H23A C23 H23B 107.9 . . ? H23A C23 C24 109.2 . . ? H23B C23 C24 109.2 . . ? C22 C23A H23C 110.7 . . ? C22 C23A H23D 110.7 . . ? C22 C23A C24A 105.3(7) . . ? H23C C23A H23D 108.8 . . ? H23C C23A C24A 110.7 . . ? H23D C23A C24A 110.7 . . ? C23 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C23 C24 C25 112.7(15) . . ? H24A C24 H24B 107.8 . . ? H24A C24 C25 109.1 . . ? H24B C24 C25 109.1 . . ? C23A C24A H24C 110.5 . . ? C23A C24A H24D 110.5 . . ? C23A C24A C25 106.2(5) . . ? H24C C24A H24D 108.7 . . ? H24C C24A C25 110.5 . . ? H24D C24A C25 110.5 . . ? O2 C25 C24 101.0(7) . . ? O2 C25 C24A 106.5(3) . . ? O2 C25 H25A 111.6 . . ? O2 C25 H25B 111.6 . . ? C24 C25 H25A 111.6 . . ? C24 C25 H25B 111.6 . . ? C24A C25 H25A 133.1 . . ? C24A C25 H25B 79.9 . . ? H25A C25 H25B 109.4 . . ? O3 C26 H26A 110.8 . . ? O3 C26 H26B 110.8 . . ? O3 C26 C27 104.8(3) . . ? H26A C26 H26B 108.9 . . ? H26A C26 C27 110.8 . . ? H26B C26 C27 110.8 . . ? C26 C27 H27A 110.9 . . ? C26 C27 H27B 110.9 . . ? C26 C27 C28 104.4(3) . . ? H27A C27 H27B 108.9 . . ? H27A C27 C28 110.9 . . ? H27B C27 C28 110.9 . . ? C27 C28 H28A 110.8 . . ? C27 C28 H28B 110.8 . . ? C27 C28 C29 104.7(3) . . ? H28A C28 H28B 108.9 . . ? H28A C28 C29 110.8 . . ? H28B C28 C29 110.8 . . ? O3 C29 C28 108.8(3) . . ? O3 C29 H29A 109.9 . . ? O3 C29 H29B 109.9 . . ? C28 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.468 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.132 #===END data_ki338_compound6 _database_code_depnum_ccdc_archive 'CCDC 713039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H54 B2 P2 Si4' _chemical_formula_sum 'C18 H54 B2 P2 Si4' _chemical_formula_weight 466.53 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' Si Si 0.0817 0.0704 '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 6.6106(1) _cell_length_b 8.7160(2) _cell_length_c 13.3995(4) _cell_angle_alpha 81.709(2) _cell_angle_beta 86.352(2) _cell_angle_gamma 77.554(2) _cell_volume 745.61(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4476 _cell_measurement_theta_min 3.0244 _cell_measurement_theta_max 29.4671 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 258 _exptl_absorpt_coefficient_mu 0.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 0.997 _exptl_absorpt_process_details Scalepack/CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6863 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 29.53 _reflns_number_total 3477 _reflns_number_gt 2720 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution SIR97 _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3477 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.68963(6) 0.20022(4) 0.63215(3) 0.02142(10) Uani 1 1 d . . . Si1 Si 0.87904(5) 0.02964(4) 0.83952(3) 0.01746(10) Uani 1 1 d . . . Si2 Si 0.71068(6) 0.40668(4) 0.79940(3) 0.01937(10) Uani 1 1 d . . . B1 B 0.3923(3) 0.2415(2) 0.64114(17) 0.0335(4) Uani 1 1 d . . . H1 H 0.332(3) 0.355(2) 0.6572(14) 0.044(5) Uiso 1 1 d . . . H2 H 0.346(3) 0.230(2) 0.5680(18) 0.065(6) Uiso 1 1 d . . . H3 H 0.351(3) 0.154(2) 0.6998(16) 0.058(6) Uiso 1 1 d . . . C1 C 0.82538(19) 0.21667(13) 0.74334(11) 0.0157(3) Uani 1 1 d . . . H1A H 0.9659 0.2306 0.7165 0.019 Uiso 1 1 calc R . . C2 C 0.7912(3) 0.32191(18) 0.52784(13) 0.0334(4) Uani 1 1 d . . . H2A H 0.9429 0.2986 0.5289 0.050 Uiso 1 1 calc R . . H2B H 0.7378 0.4341 0.5343 0.050 Uiso 1 1 calc R . . H2C H 0.7477 0.2988 0.4640 0.050 Uiso 1 1 calc R . . C3 C 0.7779(3) 0.00335(17) 0.59557(13) 0.0335(4) Uani 1 1 d . . . H3A H 0.9297 -0.0236 0.5934 0.050 Uiso 1 1 calc R . . H3B H 0.7270 0.0015 0.5287 0.050 Uiso 1 1 calc R . . H3C H 0.7245 -0.0740 0.6449 0.050 Uiso 1 1 calc R . . C4 C 1.0889(2) -0.12475(16) 0.78961(13) 0.0296(3) Uani 1 1 d . . . H4A H 1.1519 -0.2009 0.8460 0.044 Uiso 1 1 calc R . . H4B H 1.1950 -0.0737 0.7528 0.044 Uiso 1 1 calc R . . H4C H 1.0296 -0.1803 0.7440 0.044 Uiso 1 1 calc R . . C5 C 0.6405(2) -0.05144(16) 0.87155(12) 0.0235(3) Uani 1 1 d . . . H5A H 0.6729 -0.1476 0.9205 0.035 Uiso 1 1 calc R . . H5B H 0.5893 -0.0771 0.8102 0.035 Uiso 1 1 calc R . . H5C H 0.5338 0.0278 0.9008 0.035 Uiso 1 1 calc R . . C6 C 0.9773(2) 0.07324(14) 0.95881(11) 0.0230(3) Uani 1 1 d . . . H6A H 1.1061 0.1137 0.9424 0.028 Uiso 1 1 calc R . . H6B H 0.8732 0.1579 0.9862 0.028 Uiso 1 1 calc R . . C7 C 0.6185(3) 0.57933(16) 0.70173(14) 0.0364(4) Uani 1 1 d . . . H7A H 0.5591 0.6729 0.7348 0.055 Uiso 1 1 calc R . . H7B H 0.5126 0.5552 0.6620 0.055 Uiso 1 1 calc R . . H7C H 0.7354 0.6005 0.6571 0.055 Uiso 1 1 calc R . . C8 C 0.9152(2) 0.46851(16) 0.86385(14) 0.0316(4) Uani 1 1 d . . . H8A H 0.8586 0.5710 0.8874 0.047 Uiso 1 1 calc R . . H8B H 1.0324 0.4782 0.8165 0.047 Uiso 1 1 calc R . . H8C H 0.9624 0.3889 0.9216 0.047 Uiso 1 1 calc R . . C9 C 0.4895(2) 0.37908(18) 0.88873(13) 0.0318(4) Uani 1 1 d . . . H9A H 0.4164 0.4822 0.9067 0.048 Uiso 1 1 calc R . . H9B H 0.5420 0.3095 0.9498 0.048 Uiso 1 1 calc R . . H9C H 0.3940 0.3310 0.8566 0.048 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 0.02393(19) 0.02264(18) 0.0179(2) -0.00095(14) -0.00373(15) -0.00564(14) Si1 0.01726(18) 0.01470(17) 0.0190(2) 0.00161(14) -0.00198(15) -0.00245(13) Si2 0.02028(19) 0.01492(17) 0.0225(2) -0.00148(14) -0.00495(16) -0.00213(13) B1 0.0255(9) 0.0377(10) 0.0388(13) -0.0036(9) -0.0119(9) -0.0079(7) C1 0.0148(6) 0.0157(6) 0.0161(7) 0.0005(5) -0.0016(5) -0.0035(5) C2 0.0421(10) 0.0354(8) 0.0205(9) 0.0046(7) -0.0019(7) -0.0086(7) C3 0.0464(10) 0.0312(8) 0.0244(9) -0.0098(7) -0.0013(8) -0.0076(7) C4 0.0265(8) 0.0212(7) 0.0361(10) 0.0005(6) 0.0022(7) 0.0018(6) C5 0.0252(7) 0.0234(7) 0.0222(8) -0.0003(6) 0.0011(6) -0.0085(5) C6 0.0270(7) 0.0185(6) 0.0225(9) 0.0056(6) -0.0099(6) -0.0057(5) C7 0.0504(10) 0.0191(7) 0.0368(11) 0.0014(7) -0.0147(8) -0.0006(6) C8 0.0351(8) 0.0205(7) 0.0417(11) -0.0032(6) -0.0126(8) -0.0085(6) C9 0.0276(8) 0.0325(8) 0.0350(10) -0.0116(7) 0.0042(7) -0.0026(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 B1 1.9198(19) . ? P1 C1 1.8256(13) . ? P1 C2 1.8135(16) . ? P1 C3 1.8165(15) . ? Si1 C1 1.9097(13) . ? Si1 C4 1.8762(15) . ? Si1 C5 1.8649(14) . ? Si1 C6 1.8803(15) . ? Si2 C1 1.9045(13) . ? Si2 C7 1.8673(15) . ? Si2 C8 1.8606(14) . ? Si2 C9 1.8636(17) . ? B1 H1 1.031(17) . ? B1 H2 1.07(2) . ? B1 H3 1.08(2) . ? C1 H1A 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 C6 1.552(3) 2_757 ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? 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 B1 P1 C1 117.60(8) . . ? B1 P1 C2 113.32(9) . . ? B1 P1 C3 107.35(8) . . ? C1 P1 C2 106.12(7) . . ? C1 P1 C3 109.70(7) . . ? C2 P1 C3 101.57(8) . . ? C1 Si1 C4 110.24(7) . . ? C1 Si1 C5 111.30(6) . . ? C1 Si1 C6 110.47(6) . . ? C4 Si1 C5 109.86(7) . . ? C4 Si1 C6 106.24(7) . . ? C5 Si1 C6 108.59(7) . . ? C1 Si2 C7 113.05(7) . . ? C1 Si2 C8 109.76(6) . . ? C1 Si2 C9 110.78(6) . . ? C7 Si2 C8 103.93(7) . . ? C7 Si2 C9 108.42(8) . . ? C8 Si2 C9 110.72(8) . . ? P1 B1 H1 111.1(9) . . ? P1 B1 H2 105.1(12) . . ? P1 B1 H3 106.3(10) . . ? H1 B1 H2 109.6(14) . . ? H1 B1 H3 111.3(15) . . ? H2 B1 H3 113.3(15) . . ? P1 C1 Si1 115.19(6) . . ? P1 C1 Si2 112.23(6) . . ? P1 C1 H1A 104.4 . . ? Si1 C1 Si2 114.73(7) . . ? Si1 C1 H1A 104.4 . . ? Si2 C1 H1A 104.4 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 C6 113.46(12) . 2_757 ? Si1 C6 H6A 108.9 . . ? Si1 C6 H6B 108.9 . . ? C6 C6 H6A 108.9 2_757 . ? C6 C6 H6B 108.9 2_757 . ? H6A C6 H6B 107.7 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 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 B1 P1 C1 Si1 86.23(10) . . . . ? B1 P1 C1 Si2 -47.54(10) . . . . ? C2 P1 C1 Si1 -145.74(8) . . . . ? C2 P1 C1 Si2 80.49(9) . . . . ? C3 P1 C1 Si1 -36.77(10) . . . . ? C3 P1 C1 Si2 -170.53(7) . . . . ? C7 Si2 C1 P1 -35.97(10) . . . . ? C7 Si2 C1 Si1 -169.96(7) . . . . ? C8 Si2 C1 P1 -151.48(8) . . . . ? C8 Si2 C1 Si1 74.53(9) . . . . ? C9 Si2 C1 P1 85.94(9) . . . . ? C9 Si2 C1 Si1 -48.05(9) . . . . ? C4 Si1 C1 P1 72.48(9) . . . . ? C4 Si1 C1 Si2 -154.91(7) . . . . ? C5 Si1 C1 P1 -49.68(9) . . . . ? C5 Si1 C1 Si2 82.92(8) . . . . ? C6 Si1 C1 P1 -170.40(7) . . . . ? C6 Si1 C1 Si2 -37.79(9) . . . . ? C1 Si1 C6 C6 179.48(13) . . . 2_757 ? C4 Si1 C6 C6 -60.96(16) . . . 2_757 ? C5 Si1 C6 C6 57.15(16) . . . 2_757 ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.381 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.048 #===END data_ki293_compound10 _database_code_depnum_ccdc_archive 'CCDC 713040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H84 B2 K2 O4 P2 Si4' _chemical_formula_sum 'C34 H84 B2 K2 O4 P2 Si4' _chemical_formula_weight 831.13 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' K K 0.2009 0.2494 '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 9.3401(9) _cell_length_b 11.3130(11) _cell_length_c 13.0533(13) _cell_angle_alpha 78.290(2) _cell_angle_beta 76.748(2) _cell_angle_gamma 71.916(1) _cell_volume 1263.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8852 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description slab _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9090 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4402 _reflns_number_gt 4011 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0541P)^2^+0.7862P] 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 4402 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 K K 0.70337(5) 0.44378(4) 0.83785(4) 0.04417(15) Uani 1 1 d . . . Si1 Si 0.76211(7) 0.76511(5) 0.66464(4) 0.03876(16) Uani 1 1 d . . . Si2 Si 0.91361(5) 0.66220(4) 0.86768(4) 0.02623(13) Uani 1 1 d . A . P P 0.57044(5) 0.76390(5) 0.89089(4) 0.03144(14) Uani 1 1 d . A . O1 O 0.6295(2) 0.4103(2) 0.65953(17) 0.0749(6) Uani 1 1 d . A . O2 O 0.95231(18) 0.25532(15) 0.80068(15) 0.0538(4) Uani 1 1 d . A . C1 C 0.7410(2) 0.70535(17) 0.80693(14) 0.0279(4) Uani 1 1 d . A . C2 C 1.0973(2) 0.6261(2) 0.76754(17) 0.0433(5) Uani 1 1 d . . . H2A H 1.1849 0.6029 0.8041 0.065 Uiso 1 1 calc R A . H2B H 1.1011 0.7006 0.7145 0.065 Uiso 1 1 calc R . . H2C H 1.1012 0.5563 0.7322 0.065 Uiso 1 1 calc R . . C3 C 0.9254(2) 0.79167(19) 0.93391(17) 0.0378(4) Uani 1 1 d . . . H3A H 1.0219 0.7660 0.9608 0.057 Uiso 1 1 calc R A . H3B H 0.8393 0.8081 0.9932 0.057 Uiso 1 1 calc R . . H3C H 0.9211 0.8682 0.8822 0.057 Uiso 1 1 calc R . . C4 C 0.9357(2) 0.51318(16) 0.96749(14) 0.0284(4) Uani 1 1 d . . . H4A H 0.8375 0.5183 1.0175 0.034 Uiso 1 1 calc R . . H4B H 0.9562 0.4411 0.9290 0.034 Uiso 1 1 calc R . . C5 C 0.4058(2) 0.7372(2) 0.8545(2) 0.0531(6) Uani 1 1 d . . . H5A H 0.3120 0.7749 0.9020 0.080 Uiso 1 1 calc R A . H5B H 0.4195 0.6467 0.8610 0.080 Uiso 1 1 calc R . . H5C H 0.3980 0.7757 0.7809 0.080 Uiso 1 1 calc R . . C6 C 0.5151(3) 0.9354(2) 0.87875(18) 0.0459(5) Uani 1 1 d . . . H6A H 0.4146 0.9645 0.9230 0.069 Uiso 1 1 calc R A . H6B H 0.5100 0.9715 0.8044 0.069 Uiso 1 1 calc R . . H6C H 0.5911 0.9620 0.9024 0.069 Uiso 1 1 calc R . . C7 C 0.8721(3) 0.6376(3) 0.58098(19) 0.0585(6) Uani 1 1 d . A . H7A H 0.8165 0.5740 0.5932 0.088 Uiso 1 1 calc R . . H7B H 0.9734 0.5985 0.6004 0.088 Uiso 1 1 calc R . . H7C H 0.8837 0.6738 0.5057 0.088 Uiso 1 1 calc R . . C8 C 0.5779(3) 0.8331(3) 0.6103(2) 0.0725(9) Uani 1 1 d . A . H8A H 0.5298 0.7662 0.6145 0.109 Uiso 1 1 calc R . . H8B H 0.6001 0.8707 0.5359 0.109 Uiso 1 1 calc R . . H8C H 0.5082 0.8977 0.6522 0.109 Uiso 1 1 calc R . . C9 C 0.8582(4) 0.8959(3) 0.6230(2) 0.0689(8) Uani 1 1 d . A . H9A H 0.9644 0.8637 0.6345 0.103 Uiso 1 1 calc R . . H9B H 0.8033 0.9640 0.6654 0.103 Uiso 1 1 calc R . . H9C H 0.8569 0.9278 0.5475 0.103 Uiso 1 1 calc R . . C10 C 0.4883(15) 0.3636(14) 0.6570(10) 0.078(4) Uani 0.525(17) 1 d P A 1 H10A H 0.4183 0.3621 0.7265 0.093 Uiso 0.525(17) 1 calc PR A 1 H10B H 0.4305 0.4143 0.6006 0.093 Uiso 0.525(17) 1 calc PR A 1 C10A C 0.4878(17) 0.4172(17) 0.6652(12) 0.076(4) Uani 0.475(17) 1 d P A 2 H10C H 0.4330 0.5011 0.6325 0.091 Uiso 0.475(17) 1 calc PR A 2 H10D H 0.4376 0.4026 0.7403 0.091 Uiso 0.475(17) 1 calc PR A 2 C11 C 0.5730(13) 0.2371(8) 0.6324(6) 0.072(3) Uani 0.525(17) 1 d P A 1 H11A H 0.6264 0.1854 0.6906 0.087 Uiso 0.525(17) 1 calc PR A 1 H11B H 0.5059 0.1931 0.6163 0.087 Uiso 0.525(17) 1 calc PR A 1 C11A C 0.4862(16) 0.3146(19) 0.6043(11) 0.108(6) Uani 0.475(17) 1 d P A 2 H11C H 0.4175 0.3491 0.5514 0.130 Uiso 0.475(17) 1 calc PR A 2 H11D H 0.4543 0.2446 0.6534 0.130 Uiso 0.475(17) 1 calc PR A 2 C12 C 0.6735(7) 0.2675(5) 0.5439(4) 0.1285(18) Uani 0.525(17) 1 d P A 1 H12A H 0.6202 0.3120 0.4838 0.154 Uiso 0.525(17) 1 calc PR A 1 H12B H 0.7540 0.1919 0.5218 0.154 Uiso 0.525(17) 1 calc PR A 1 C12A C 0.6735(7) 0.2675(5) 0.5439(4) 0.1285(18) Uani 0.475(17) 1 d P A 2 H12C H 0.7214 0.1778 0.5677 0.154 Uiso 0.475(17) 1 calc PR A 2 H12D H 0.6845 0.2823 0.4655 0.154 Uiso 0.475(17) 1 calc PR A 2 C13 C 0.7346(4) 0.3467(5) 0.5805(3) 0.1064(15) Uani 1 1 d . . . H13A H 0.8279 0.2961 0.6091 0.128 Uiso 1 1 calc R A 1 H13B H 0.7641 0.4084 0.5203 0.128 Uiso 1 1 calc R A 1 C14 C 0.9516(3) 0.1260(2) 0.8239(3) 0.0645(7) Uani 1 1 d . . . H14A H 0.8632 0.1151 0.8009 0.077 Uiso 1 1 calc R A . H14B H 0.9447 0.0967 0.9012 0.077 Uiso 1 1 calc R . . C15 C 1.0936(4) 0.0557(3) 0.7661(5) 0.136(2) Uani 1 1 d . A . H15A H 1.1496 -0.0114 0.8158 0.164 Uiso 1 1 calc R . . H15B H 1.0717 0.0157 0.7128 0.164 Uiso 1 1 calc R . . C16 C 1.1843(3) 0.1371(3) 0.7146(3) 0.0767(9) Uani 1 1 d . . . H16A H 1.1964 0.1438 0.6365 0.092 Uiso 1 1 calc R A . H16B H 1.2871 0.1052 0.7345 0.092 Uiso 1 1 calc R . . C17 C 1.1031(3) 0.2623(2) 0.75006(19) 0.0495(5) Uani 1 1 d . A . H17A H 1.1562 0.2794 0.8006 0.059 Uiso 1 1 calc R . . H17B H 1.0986 0.3299 0.6884 0.059 Uiso 1 1 calc R . . B B 0.5508(3) 0.6980(2) 1.04034(19) 0.0398(5) Uani 1 1 d . . . H1A H 0.560(3) 0.594(2) 1.0468(19) 0.049(6) Uiso 1 1 d . . . H1B H 0.641(3) 0.714(2) 1.078(2) 0.054(7) Uiso 1 1 d . . . H1C H 0.432(3) 0.750(2) 1.072(2) 0.057(7) Uiso 1 1 d . . . 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 K 0.0346(2) 0.0381(3) 0.0616(3) -0.0178(2) 0.0050(2) -0.01561(19) Si1 0.0482(3) 0.0404(3) 0.0268(3) -0.0020(2) -0.0126(2) -0.0086(3) Si2 0.0238(2) 0.0282(3) 0.0276(3) -0.00082(19) -0.00616(19) -0.00940(19) P 0.0252(2) 0.0332(3) 0.0358(3) -0.0068(2) -0.00848(19) -0.00448(19) O1 0.0724(13) 0.0955(15) 0.0691(12) -0.0326(11) 0.0131(10) -0.0459(12) O2 0.0413(9) 0.0415(9) 0.0780(12) -0.0203(8) -0.0026(8) -0.0089(7) C1 0.0275(9) 0.0290(9) 0.0274(9) -0.0037(7) -0.0083(7) -0.0057(7) C2 0.0301(10) 0.0546(13) 0.0414(11) -0.0017(10) -0.0015(9) -0.0128(9) C3 0.0439(11) 0.0339(10) 0.0426(11) 0.0002(8) -0.0158(9) -0.0182(9) C4 0.0262(9) 0.0274(9) 0.0332(9) -0.0008(7) -0.0101(7) -0.0085(7) C5 0.0285(11) 0.0605(15) 0.0738(16) -0.0197(12) -0.0176(11) -0.0051(10) C6 0.0501(13) 0.0352(11) 0.0460(12) -0.0104(9) -0.0106(10) 0.0015(9) C7 0.0707(17) 0.0668(16) 0.0342(12) -0.0168(11) -0.0019(11) -0.0130(13) C8 0.0718(18) 0.096(2) 0.0406(13) -0.0059(14) -0.0303(13) 0.0019(16) C9 0.106(2) 0.0558(16) 0.0458(14) 0.0156(12) -0.0178(15) -0.0356(16) C10 0.052(4) 0.132(11) 0.047(6) 0.001(6) 0.004(4) -0.040(7) C10A 0.050(5) 0.128(11) 0.051(4) -0.022(7) -0.025(3) -0.009(6) C11 0.081(6) 0.082(5) 0.074(4) -0.008(3) -0.020(4) -0.048(4) C11A 0.080(7) 0.186(16) 0.100(7) -0.046(9) -0.012(6) -0.082(9) C12 0.180(5) 0.110(3) 0.112(3) -0.042(3) 0.015(3) -0.076(3) C12A 0.180(5) 0.110(3) 0.112(3) -0.042(3) 0.015(3) -0.076(3) C13 0.0555(19) 0.179(4) 0.095(3) -0.068(3) -0.0094(18) -0.019(2) C14 0.0575(15) 0.0444(13) 0.092(2) -0.0224(13) 0.0057(14) -0.0202(12) C15 0.062(2) 0.0530(18) 0.271(6) -0.059(3) 0.054(3) -0.0212(16) C16 0.0586(17) 0.0536(16) 0.090(2) -0.0030(15) 0.0155(15) -0.0017(13) C17 0.0494(13) 0.0529(13) 0.0471(13) -0.0043(10) -0.0050(10) -0.0197(11) B 0.0313(12) 0.0452(13) 0.0385(12) -0.0028(10) 0.0017(9) -0.0124(10) _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 K O1 2.701(2) . ? K O2 2.6481(16) . ? K C1 3.0232(19) . ? K C4 3.3868(18) . ? Si1 C1 1.8305(18) . ? Si1 C7 1.880(2) . ? Si1 C8 1.890(3) . ? Si1 C9 1.888(3) . ? Si2 C1 1.8454(18) . ? Si2 C2 1.890(2) . ? Si2 C3 1.888(2) . ? Si2 C4 1.8968(18) . ? P C1 1.7371(18) . ? P C5 1.834(2) . ? P C6 1.829(2) . ? P B 1.930(2) . ? O1 C10 1.574(14) . ? O1 C10A 1.287(15) . ? O1 C13 1.394(4) . ? O2 C14 1.434(3) . ? O2 C17 1.431(3) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 C4 1.547(3) 2_767 ? C4 H4A 0.990 . ? C4 H4B 0.990 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.465(15) . ? C10A H10C 0.990 . ? C10A H10D 0.990 . ? C10A C11A 1.539(16) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.369(8) . ? C11A H11C 0.990 . ? C11A H11D 0.990 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.404(6) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.446(4) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.411(4) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.494(4) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? B H1A 1.14(2) . ? B H1B 1.14(3) . ? B H1C 1.11(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K O2 86.83(6) . . ? O1 K C1 108.49(6) . . ? O1 K C4 152.10(5) . . ? O2 K C1 118.04(5) . . ? O2 K C4 80.16(5) . . ? C1 K C4 58.36(4) . . ? C1 Si1 C7 112.01(10) . . ? C1 Si1 C8 115.67(11) . . ? C1 Si1 C9 114.37(10) . . ? C7 Si1 C8 102.77(13) . . ? C7 Si1 C9 107.55(14) . . ? C8 Si1 C9 103.39(15) . . ? C1 Si2 C2 112.89(9) . . ? C1 Si2 C3 112.87(9) . . ? C1 Si2 C4 114.16(8) . . ? C2 Si2 C3 105.04(10) . . ? C2 Si2 C4 102.81(9) . . ? C3 Si2 C4 108.21(9) . . ? C1 P C5 112.48(10) . . ? C1 P C6 112.32(10) . . ? C1 P B 118.61(10) . . ? C5 P C6 101.34(11) . . ? C5 P B 102.45(12) . . ? C6 P B 107.86(11) . . ? K O1 C10 124.6(5) . . ? K O1 C10A 115.6(6) . . ? K O1 C13 123.8(2) . . ? C10 O1 C13 98.6(5) . . ? C10A O1 C13 116.8(7) . . ? K O2 C14 123.23(14) . . ? K O2 C17 127.76(13) . . ? C14 O2 C17 108.90(18) . . ? K C1 Si1 108.27(8) . . ? K C1 Si2 96.80(7) . . ? K C1 P 94.43(7) . . ? Si1 C1 Si2 117.02(10) . . ? Si1 C1 P 119.52(10) . . ? Si2 C1 P 114.64(10) . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? K C4 Si2 84.63(6) . . ? K C4 C4 156.94(16) . 2_767 ? K C4 H4A 73.8 . . ? K C4 H4B 50.9 . . ? Si2 C4 C4 114.96(16) . 2_767 ? Si2 C4 H4A 108.5 . . ? Si2 C4 H4B 108.5 . . ? C4 C4 H4A 108.5 2_767 . ? C4 C4 H4B 108.5 2_767 . ? H4A C4 H4B 107.5 . . ? P C5 H5A 109.5 . . ? P C5 H5B 109.5 . . ? P C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P C6 H6A 109.5 . . ? P C6 H6B 109.5 . . ? P C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 H10A 112.2 . . ? O1 C10 H10B 112.2 . . ? O1 C10 C11 97.9(8) . . ? H10A C10 H10B 109.8 . . ? H10A C10 C11 112.2 . . ? H10B C10 C11 112.2 . . ? O1 C10A H10C 110.5 . . ? O1 C10A H10D 110.5 . . ? O1 C10A C11A 106.3(11) . . ? H10C C10A H10D 108.7 . . ? H10C C10A C11A 110.5 . . ? H10D C10A C11A 110.5 . . ? C10 C11 H11A 111.9 . . ? C10 C11 H11B 111.9 . . ? C10 C11 C12 99.3(7) . . ? H11A C11 H11B 109.6 . . ? H11A C11 C12 111.9 . . ? H11B C11 C12 111.9 . . ? C10A C11A H11C 111.4 . . ? C10A C11A H11D 111.4 . . ? H11C C11A H11D 109.2 . . ? C11 C12 H12A 111.4 . . ? C11 C12 H12B 111.4 . . ? C11 C12 C13 101.7(5) . . ? H12A C12 H12B 109.3 . . ? H12A C12 C13 111.4 . . ? H12B C12 C13 111.4 . . ? O1 C13 C12 111.5(4) . . ? O1 C13 H13A 109.3 . . ? O1 C13 H13B 109.3 . . ? C12 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? O2 C14 H14A 110.4 . . ? O2 C14 H14B 110.4 . . ? O2 C14 C15 106.7(2) . . ? H14A C14 H14B 108.6 . . ? H14A C14 C15 110.4 . . ? H14B C14 C15 110.4 . . ? C14 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? C14 C15 C16 109.6(3) . . ? H15A C15 H15B 108.2 . . ? H15A C15 C16 109.8 . . ? H15B C15 C16 109.8 . . ? C15 C16 H16A 110.4 . . ? C15 C16 H16B 110.4 . . ? C15 C16 C17 106.7(2) . . ? H16A C16 H16B 108.6 . . ? H16A C16 C17 110.4 . . ? H16B C16 C17 110.4 . . ? O2 C17 C16 105.7(2) . . ? O2 C17 H17A 110.6 . . ? O2 C17 H17B 110.6 . . ? C16 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? P B H1A 106.6(12) . . ? P B H1B 111.9(13) . . ? P B H1C 102.2(13) . . ? H1A B H1B 112.3(18) . . ? H1A B H1C 109.7(18) . . ? H1B B H1C 113.4(18) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.626 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.048 #===END