Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Alkali metal complexes of a phosphine-borane-stabilised carbanion: influence of co-ligands on structure ; _publ_contact_author_name 'Keith Izod' _publ_contact_author_email K.J.IZOD@NCL.AC.UK loop_ _publ_author_name 'Keith Izod' 'W. Clegg' 'Ross W. Harrington' 'Corrine Wills' # Attachment 'dalton.cif' data_ki260_compound_2a _database_code_depnum_ccdc_archive 'CCDC 649161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H62 B2 K2 O P2 Si4' _chemical_formula_sum 'C22 H62 B2 K2 O P2 Si4' _chemical_formula_weight 616.84 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' 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' 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' _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 12.614(2) _cell_length_b 13.3311(11) _cell_length_c 14.5257(16) _cell_angle_alpha 115.522(6) _cell_angle_beta 113.770(11) _cell_angle_gamma 93.432(8) _cell_volume 1934.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 285 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.873 _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 '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 24649 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7550 _reflns_number_gt 5849 _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^)+(0.0605P)^2^+0.7993P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7550 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.004 _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 0.30359(5) 0.43332(4) 0.79567(5) 0.03336(14) Uani 1 1 d . . . K2 K 0.06618(5) 0.18536(5) 0.75331(5) 0.03608(15) Uani 1 1 d . . . P1 P 0.40162(5) 0.38525(5) 1.14464(5) 0.02230(16) Uani 0.9638(14) 1 d P . 1 P2 P 0.22509(5) 0.07710(5) 0.47983(5) 0.02729(15) Uani 1 1 d . . . Si1 Si 0.54950(6) 0.25022(6) 1.04732(6) 0.03090(18) Uani 0.9638(14) 1 d P . 1 Si2 Si 0.63906(6) 0.37340(6) 1.31624(6) 0.02728(17) Uani 0.9638(14) 1 d P . 1 Si3 Si 0.20339(6) -0.06420(6) 0.23715(6) 0.03297(17) Uani 1 1 d . . . Si4 Si 0.02957(6) 0.08876(6) 0.27913(5) 0.02864(16) Uani 1 1 d . . . O1 O 0.06509(15) 0.40381(15) 0.76403(15) 0.0403(4) Uani 1 1 d . . . B1 B 0.2982(3) 0.3637(3) 0.9926(3) 0.0405(7) Uani 1 1 d . . . H1A H 0.300(2) 0.290(2) 0.929(2) 0.037(7) Uiso 1 1 d . . . H1B H 0.206(3) 0.365(2) 0.993(3) 0.056(9) Uiso 1 1 d . . . H1C H 0.338(3) 0.437(3) 0.995(3) 0.066(10) Uiso 1 1 d . . . B2 B 0.1646(3) 0.1732(3) 0.5805(2) 0.0375(7) Uani 1 1 d . . . H2A H 0.155(3) 0.251(2) 0.572(2) 0.048(8) Uiso 1 1 d . . . H2B H 0.076(3) 0.120(2) 0.555(2) 0.045(8) Uiso 1 1 d . . . H2C H 0.240(2) 0.195(2) 0.667(2) 0.043(7) Uiso 1 1 d . . . C1 C 0.54431(19) 0.36270(18) 1.17531(18) 0.0234(4) Uani 1 1 d . . . C2 C 0.4092(2) 0.5341(2) 1.2405(2) 0.0391(6) Uani 1 1 d . . . H2D H 0.4456 0.5497 1.3207 0.059 Uiso 1 1 calc R . 1 H2E H 0.3275 0.5432 1.2170 0.059 Uiso 1 1 calc R . 1 H2F H 0.4585 0.5887 1.2350 0.059 Uiso 1 1 calc R . 1 C3 C 0.3118(2) 0.3000(2) 1.1725(3) 0.0419(6) Uani 1 1 d . . . H3A H 0.3009 0.2174 1.1247 0.063 Uiso 1 1 calc R . 1 H3B H 0.2327 0.3149 1.1532 0.063 Uiso 1 1 calc R . 1 H3C H 0.3537 0.3221 1.2547 0.063 Uiso 1 1 calc R . 1 C4 C 0.6983(3) 0.2131(3) 1.0890(3) 0.0581(8) Uani 1 1 d . . . H4A H 0.7641 0.2814 1.1222 0.087 Uiso 1 1 calc R . 1 H4B H 0.6960 0.1501 1.0200 0.087 Uiso 1 1 calc R . 1 H4C H 0.7117 0.1885 1.1465 0.087 Uiso 1 1 calc R . 1 C5 C 0.5391(3) 0.2954(3) 0.9378(3) 0.0584(8) Uani 1 1 d . . . H5A H 0.4826 0.3426 0.9324 0.088 Uiso 1 1 calc R . 1 H5B H 0.5102 0.2263 0.8618 0.088 Uiso 1 1 calc R . 1 H5C H 0.6190 0.3408 0.9625 0.088 Uiso 1 1 calc R . 1 C6 C 0.4286(3) 0.1087(2) 0.9647(3) 0.0519(8) Uani 1 1 d . . . H6A H 0.4345 0.0786 1.0169 0.078 Uiso 1 1 calc R . 1 H6B H 0.4395 0.0527 0.9006 0.078 Uiso 1 1 calc R . 1 H6C H 0.3490 0.1213 0.9337 0.078 Uiso 1 1 calc R . 1 C7 C 0.8061(2) 0.4326(2) 1.3712(2) 0.0431(6) Uani 1 1 d . . . H7A H 0.8275 0.3872 1.3109 0.065 Uiso 1 1 calc R . 1 H7B H 0.8534 0.4274 1.4407 0.065 Uiso 1 1 calc R . 1 H7C H 0.8235 0.5138 1.3903 0.065 Uiso 1 1 calc R . 1 C8 C 0.6202(3) 0.2327(3) 1.3174(3) 0.0479(7) Uani 1 1 d . . . H8A H 0.5382 0.2058 1.3032 0.072 Uiso 1 1 calc R . 1 H8B H 0.6789 0.2446 1.3930 0.072 Uiso 1 1 calc R . 1 H8C H 0.6337 0.1743 1.2564 0.072 Uiso 1 1 calc R . 1 C9 C 0.6137(3) 0.4777(3) 1.4390(2) 0.0490(7) Uani 1 1 d . . . H9A H 0.6254 0.5544 1.4458 0.073 Uiso 1 1 calc R . 1 H9B H 0.6713 0.4831 1.5118 0.073 Uiso 1 1 calc R . 1 H9C H 0.5311 0.4494 1.4228 0.073 Uiso 1 1 calc R . 1 C10 C 0.13620(19) 0.01141(18) 0.32968(18) 0.0252(5) Uani 1 1 d . . . C11 C 0.2646(3) -0.0285(2) 0.5272(2) 0.0450(7) Uani 1 1 d . . . H11A H 0.3046 -0.0757 0.4864 0.067 Uiso 1 1 calc R . . H11B H 0.1911 -0.0786 0.5097 0.067 Uiso 1 1 calc R . . H11C H 0.3193 0.0124 0.6110 0.067 Uiso 1 1 calc R . . C12 C 0.3742(2) 0.1679(2) 0.5321(2) 0.0458(7) Uani 1 1 d . . . H12A H 0.4133 0.1223 0.4890 0.069 Uiso 1 1 calc R . . H12B H 0.4240 0.1953 0.6149 0.069 Uiso 1 1 calc R . . H12C H 0.3650 0.2345 0.5202 0.069 Uiso 1 1 calc R . . C13 C 0.0913(3) -0.1974(2) 0.0944(3) 0.0575(9) Uani 1 1 d . . . H13A H 0.0217 -0.1758 0.0538 0.086 Uiso 1 1 calc R . . H13B H 0.0641 -0.2561 0.1098 0.086 Uiso 1 1 calc R . . H13C H 0.1304 -0.2289 0.0461 0.086 Uiso 1 1 calc R . . C14 C 0.2737(3) 0.0308(3) 0.1992(3) 0.0529(8) Uani 1 1 d . . . H14A H 0.3366 0.0982 0.2705 0.079 Uiso 1 1 calc R . . H14B H 0.2115 0.0570 0.1556 0.079 Uiso 1 1 calc R . . H14C H 0.3095 -0.0134 0.1516 0.079 Uiso 1 1 calc R . . C15 C 0.3269(3) -0.1267(3) 0.3002(3) 0.0653(9) Uani 1 1 d . . . H15A H 0.3910 -0.0649 0.3756 0.098 Uiso 1 1 calc R . . H15B H 0.3605 -0.1604 0.2472 0.098 Uiso 1 1 calc R . . H15C H 0.2928 -0.1869 0.3102 0.098 Uiso 1 1 calc R . . C16 C -0.0909(2) 0.0992(2) 0.3259(2) 0.0409(6) Uani 1 1 d . . . H16A H -0.0532 0.1470 0.4105 0.061 Uiso 1 1 calc R . . H16B H -0.1345 0.0215 0.3015 0.061 Uiso 1 1 calc R . . H16C H -0.1477 0.1347 0.2899 0.061 Uiso 1 1 calc R . . C17 C 0.1005(3) 0.2410(2) 0.3219(3) 0.0522(7) Uani 1 1 d . . . H17A H 0.1410 0.2895 0.4066 0.078 Uiso 1 1 calc R . . H17B H 0.0378 0.2727 0.2872 0.078 Uiso 1 1 calc R . . H17C H 0.1598 0.2400 0.2942 0.078 Uiso 1 1 calc R . . C18 C -0.0603(3) 0.0102(3) 0.1155(2) 0.0516(7) Uani 1 1 d . . . H18A H -0.0051 0.0044 0.0827 0.077 Uiso 1 1 calc R . . H18B H -0.1155 0.0533 0.0915 0.077 Uiso 1 1 calc R . . H18C H -0.1070 -0.0677 0.0875 0.077 Uiso 1 1 calc R . . C19 C 0.0585(3) 0.4954(3) 0.8609(2) 0.0506(7) Uani 1 1 d . . . H19A H 0.1078 0.5715 0.8851 0.061 Uiso 1 1 calc R . . H19B H 0.0890 0.4820 0.9278 0.061 Uiso 1 1 calc R . . C20 C -0.0683(3) 0.4931(4) 0.8212(3) 0.1010(17) Uani 1 1 d . . . H20A H -0.0760 0.5730 0.8499 0.121 Uiso 1 1 calc R . . H20B H -0.1049 0.4541 0.8503 0.121 Uiso 1 1 calc R . . C21 C -0.1291(3) 0.4286(4) 0.6930(3) 0.0844(13) Uani 1 1 d . . . H21A H -0.1580 0.4806 0.6621 0.101 Uiso 1 1 calc R . . H21B H -0.1993 0.3641 0.6621 0.101 Uiso 1 1 calc R . . C22 C -0.0387(3) 0.3831(3) 0.6589(2) 0.0517(7) Uani 1 1 d . . . H22A H -0.0722 0.2991 0.6019 0.062 Uiso 1 1 calc R . . H22B H -0.0154 0.4235 0.6236 0.062 Uiso 1 1 calc R . . P1X P 0.4613(15) 0.2844(14) 1.0302(15) 0.029(4) Uiso 0.0362(14) 1 d P . 2 Si1X Si 0.6824(17) 0.3150(16) 1.2481(17) 0.034(5) Uiso 0.0362(14) 1 d P . 2 Si2X Si 0.4785(16) 0.4455(15) 1.2642(15) 0.028(4) Uiso 0.0362(14) 1 d P . 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 K1 0.0343(3) 0.0310(3) 0.0301(3) 0.0145(2) 0.0132(2) 0.0002(2) K2 0.0361(3) 0.0320(3) 0.0284(3) 0.0095(2) 0.0133(2) -0.0055(2) P1 0.0218(3) 0.0219(3) 0.0198(3) 0.0098(2) 0.0079(2) 0.0035(2) P2 0.0270(3) 0.0254(3) 0.0214(3) 0.0090(2) 0.0079(2) 0.0043(2) Si1 0.0350(4) 0.0267(3) 0.0258(4) 0.0074(3) 0.0163(3) 0.0074(3) Si2 0.0239(3) 0.0334(4) 0.0243(3) 0.0158(3) 0.0098(3) 0.0078(3) Si3 0.0349(4) 0.0305(3) 0.0318(4) 0.0088(3) 0.0222(3) 0.0055(3) Si4 0.0283(3) 0.0332(3) 0.0225(3) 0.0134(3) 0.0113(3) 0.0070(3) O1 0.0357(9) 0.0469(10) 0.0301(9) 0.0144(8) 0.0126(8) 0.0194(8) B1 0.0446(18) 0.0416(17) 0.0268(15) 0.0176(14) 0.0086(13) 0.0138(14) B2 0.0455(17) 0.0357(16) 0.0217(14) 0.0082(12) 0.0143(13) 0.0121(14) C1 0.0233(11) 0.0234(11) 0.0202(11) 0.0090(9) 0.0098(9) 0.0029(9) C2 0.0360(14) 0.0332(13) 0.0357(14) 0.0086(11) 0.0153(12) 0.0126(11) C3 0.0301(13) 0.0512(16) 0.0544(17) 0.0334(14) 0.0217(13) 0.0088(12) C4 0.0541(18) 0.0609(19) 0.056(2) 0.0164(16) 0.0359(16) 0.0284(16) C5 0.076(2) 0.067(2) 0.0372(16) 0.0215(15) 0.0367(16) 0.0166(17) C6 0.0536(18) 0.0262(14) 0.0480(17) 0.0041(13) 0.0166(14) 0.0038(12) C7 0.0279(13) 0.0514(16) 0.0374(15) 0.0215(13) 0.0058(11) 0.0078(12) C8 0.0465(16) 0.0532(17) 0.0593(19) 0.0414(16) 0.0234(15) 0.0170(14) C9 0.0447(16) 0.0683(19) 0.0240(13) 0.0181(14) 0.0128(12) 0.0186(14) C10 0.0245(11) 0.0246(11) 0.0200(11) 0.0073(9) 0.0098(9) 0.0025(9) C11 0.0583(18) 0.0435(15) 0.0386(15) 0.0252(13) 0.0217(14) 0.0214(13) C12 0.0279(13) 0.0435(15) 0.0427(16) 0.0174(13) 0.0028(12) -0.0016(11) C13 0.067(2) 0.0387(16) 0.0468(18) -0.0017(14) 0.0367(16) 0.0000(14) C14 0.0590(18) 0.0532(18) 0.0498(18) 0.0179(15) 0.0391(16) 0.0011(14) C15 0.073(2) 0.073(2) 0.071(2) 0.0354(19) 0.050(2) 0.0486(19) C16 0.0348(14) 0.0551(17) 0.0341(14) 0.0214(13) 0.0176(12) 0.0182(12) C17 0.0583(18) 0.0415(16) 0.064(2) 0.0317(15) 0.0296(16) 0.0154(14) C18 0.0475(16) 0.074(2) 0.0275(14) 0.0239(14) 0.0144(13) 0.0187(15) C19 0.0475(16) 0.0459(16) 0.0384(16) 0.0077(13) 0.0164(13) 0.0217(13) C20 0.058(2) 0.128(4) 0.061(2) 0.006(2) 0.0205(19) 0.051(2) C21 0.049(2) 0.130(4) 0.052(2) 0.033(2) 0.0165(17) 0.044(2) C22 0.0398(15) 0.074(2) 0.0355(15) 0.0258(15) 0.0137(13) 0.0176(15) _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 O1 2.8291(19) . ? K1 H1C 2.73(3) . ? K1 H2A 2.78(3) . ? K1 H2C 2.76(3) . ? K1 C1 2.998(2) 2_667 ? K2 O1 2.8498(19) . ? K2 H1A 2.75(3) . ? K2 H1B 2.89(3) . ? K2 H2B 2.68(3) . ? K2 H2C 2.95(3) . ? K2 C10 2.974(2) 2_556 ? P1 B1 1.936(3) . ? P1 C1 1.750(2) . ? P1 C2 1.837(2) . ? P1 C3 1.831(2) . ? P2 B2 1.940(3) . ? P2 C10 1.745(2) . ? P2 C11 1.829(3) . ? P2 C12 1.834(3) . ? Si1 C1 1.848(2) . ? Si1 C4 1.894(3) . ? Si1 C5 1.891(3) . ? Si1 C6 1.885(3) . ? Si2 C1 1.843(2) . ? Si2 C7 1.897(3) . ? Si2 C8 1.885(3) . ? Si2 C9 1.895(3) . ? Si3 C10 1.842(2) . ? Si3 C13 1.901(3) . ? Si3 C14 1.886(3) . ? Si3 C15 1.903(3) . ? Si4 C10 1.853(2) . ? Si4 C16 1.888(3) . ? Si4 C17 1.885(3) . ? Si4 C18 1.890(3) . ? O1 C19 1.451(3) . ? O1 C22 1.450(3) . ? B1 H1A 1.03(3) . ? B1 H1B 1.16(3) . ? B1 H1C 1.05(3) . ? B2 H2A 1.10(3) . ? B2 H2B 1.12(3) . ? B2 H2C 1.12(3) . ? C1 K1 2.998(2) 2_667 ? C2 H2D 0.980 . ? C2 H2E 0.980 . ? C2 H2F 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 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 K2 2.974(2) 2_556 ? 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 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 C20 1.458(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.479(5) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.481(4) . ? C22 H22A 0.990 . ? C22 H22B 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 O1 K1 H1C 79.0(7) . . ? O1 K1 H2A 73.2(6) . . ? O1 K1 H2C 85.8(6) . . ? O1 K1 C1 126.32(6) . 2_667 ? H1C K1 H2A 125.6(9) . . ? H1C K1 H2C 94.3(9) . . ? H1C K1 C1 116.2(7) . 2_667 ? H2A K1 H2C 38.8(8) . . ? H2A K1 C1 118.0(6) . 2_667 ? H2C K1 C1 137.8(6) . 2_667 ? O1 K2 H1A 86.8(5) . . ? O1 K2 H1B 71.8(6) . . ? O1 K2 H2B 85.3(6) . . ? O1 K2 H2C 81.9(5) . . ? O1 K2 C10 130.53(6) . 2_556 ? H1A K2 H1B 38.8(8) . . ? H1A K2 H2B 106.3(8) . . ? H1A K2 H2C 67.5(8) . . ? H1A K2 C10 136.6(5) . 2_556 ? H1B K2 H2B 137.1(8) . . ? H1B K2 H2C 100.8(8) . . ? H1B K2 C10 123.4(6) . 2_556 ? H2B K2 H2C 38.9(8) . . ? H2B K2 C10 99.1(6) . 2_556 ? H2C K2 C10 129.9(5) . 2_556 ? B1 P1 C1 118.78(13) . . ? B1 P1 C2 101.95(13) . . ? B1 P1 C3 106.82(14) . . ? C1 P1 C2 112.78(11) . . ? C1 P1 C3 112.68(12) . . ? C2 P1 C3 102.04(13) . . ? B2 P2 C10 119.42(12) . . ? B2 P2 C11 103.93(13) . . ? B2 P2 C12 105.01(14) . . ? C10 P2 C11 112.27(12) . . ? C10 P2 C12 112.48(12) . . ? C11 P2 C12 101.94(14) . . ? C1 Si1 C4 111.70(12) . . ? C1 Si1 C5 114.13(13) . . ? C1 Si1 C6 114.29(12) . . ? C4 Si1 C5 103.60(16) . . ? C4 Si1 C6 105.79(15) . . ? C5 Si1 C6 106.45(15) . . ? C1 Si2 C7 112.21(11) . . ? C1 Si2 C8 114.86(12) . . ? C1 Si2 C9 114.33(11) . . ? C7 Si2 C8 106.55(13) . . ? C7 Si2 C9 103.03(13) . . ? C8 Si2 C9 104.82(14) . . ? C10 Si3 C13 113.50(12) . . ? C10 Si3 C14 113.19(12) . . ? C10 Si3 C15 115.55(13) . . ? C13 Si3 C14 106.55(14) . . ? C13 Si3 C15 101.91(16) . . ? C14 Si3 C15 105.04(16) . . ? C10 Si4 C16 114.59(11) . . ? C10 Si4 C17 115.58(12) . . ? C10 Si4 C18 111.38(12) . . ? C16 Si4 C17 105.87(14) . . ? C16 Si4 C18 103.26(13) . . ? C17 Si4 C18 105.01(15) . . ? K1 O1 K2 89.02(5) . . ? K1 O1 C19 111.62(15) . . ? K1 O1 C22 123.44(15) . . ? K2 O1 C19 118.25(17) . . ? K2 O1 C22 107.04(17) . . ? C19 O1 C22 107.2(2) . . ? P1 B1 H1A 110.7(14) . . ? P1 B1 H1B 101.7(15) . . ? P1 B1 H1C 103.4(18) . . ? H1A B1 H1B 117(2) . . ? H1A B1 H1C 109(2) . . ? H1B B1 H1C 113(2) . . ? P2 B2 H2A 110.2(15) . . ? P2 B2 H2B 107.7(14) . . ? P2 B2 H2C 99.8(14) . . ? H2A B2 H2B 111(2) . . ? H2A B2 H2C 112(2) . . ? H2B B2 H2C 115(2) . . ? K1 C1 P1 106.02(9) 2_667 . ? K1 C1 Si1 97.23(8) 2_667 . ? K1 C1 Si2 99.14(8) 2_667 . ? P1 C1 Si1 113.45(12) . . ? P1 C1 Si2 119.02(12) . . ? Si1 C1 Si2 117.19(12) . . ? P2 C10 Si3 118.29(12) . . ? P2 C10 Si4 115.31(12) . . ? Si3 C10 Si4 116.54(12) . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si4 C16 H16A 109.5 . . ? Si4 C16 H16B 109.5 . . ? Si4 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C17 H17A 109.5 . . ? Si4 C17 H17B 109.5 . . ? Si4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C18 H18A 109.5 . . ? Si4 C18 H18B 109.5 . . ? Si4 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 H19A 110.4 . . ? O1 C19 H19B 110.4 . . ? O1 C19 C20 106.8(2) . . ? H19A C19 H19B 108.6 . . ? H19A C19 C20 110.4 . . ? H19B C19 C20 110.4 . . ? C19 C20 H20A 110.3 . . ? C19 C20 H20B 110.3 . . ? C19 C20 C21 106.9(3) . . ? H20A C20 H20B 108.6 . . ? H20A C20 C21 110.3 . . ? H20B C20 C21 110.3 . . ? C20 C21 H21A 110.4 . . ? C20 C21 H21B 110.4 . . ? C20 C21 C22 106.8(3) . . ? H21A C21 H21B 108.6 . . ? H21A C21 C22 110.4 . . ? H21B C21 C22 110.4 . . ? O1 C22 C21 106.7(2) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.352 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.077 #===END data_ki267_compound_2b _database_code_depnum_ccdc_archive 'CCDC 649162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H86 B2 K2 N4 P2 Si4' _chemical_formula_sum 'C30 H86 B2 K2 N4 P2 Si4' _chemical_formula_weight 777.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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 8.7353(6) _cell_length_b 11.3832(8) _cell_length_c 13.5668(10) _cell_angle_alpha 79.174(1) _cell_angle_beta 79.418(1) _cell_angle_gamma 71.435(1) _cell_volume 1244.90(15) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8605 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 0.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.929 _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 9061 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4351 _reflns_number_gt 4098 _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 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^)+(0.0367P)^2^+1.6697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4351 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _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 K1 K 0.37193(8) 0.53561(5) 0.16523(4) 0.03097(17) Uani 1 1 d . . . P1 P 0.27120(10) 0.27467(7) 0.11654(5) 0.03130(19) Uani 1 1 d . A . Si1 Si 0.52731(9) 0.19534(8) 0.26098(7) 0.0379(2) Uani 1 1 d . . . Si2 Si 0.16002(9) 0.28305(7) 0.34571(5) 0.02643(18) Uani 1 1 d . . . N1 N 0.3722(3) 0.6805(2) 0.31509(17) 0.0320(5) Uani 1 1 d . . . N2 N 0.0839(3) 0.7573(2) 0.19705(17) 0.0316(5) Uani 1 1 d . . . B1 B 0.3755(5) 0.3618(4) 0.0011(2) 0.0400(8) Uani 1 1 d . . . H1A H 0.362(5) 0.329(4) -0.068(3) 0.071(12) Uiso 1 1 d . . . H1B H 0.503(5) 0.350(3) 0.013(3) 0.065(11) Uiso 1 1 d . . . H1C H 0.308(4) 0.460(3) 0.000(2) 0.050(9) Uiso 1 1 d . . . C1 C 0.3173(3) 0.2744(2) 0.23556(18) 0.0249(5) Uani 1 1 d . A . C2 C 0.2993(7) 0.1162(4) 0.0902(3) 0.0745(14) Uani 1 1 d . . . H2A H 0.2324 0.0753 0.1427 0.112 Uiso 1 1 calc R A . H2B H 0.4143 0.0675 0.0899 0.112 Uiso 1 1 calc R . . H2C H 0.2662 0.1210 0.0240 0.112 Uiso 1 1 calc R . . C3 C 0.0553(4) 0.3447(4) 0.1084(3) 0.0601(11) Uani 1 1 d . . . H3A H -0.0069 0.2988 0.1599 0.090 Uiso 1 1 calc R A . H3B H 0.0332 0.3409 0.0410 0.090 Uiso 1 1 calc R . . H3C H 0.0230 0.4322 0.1200 0.090 Uiso 1 1 calc R . . C4 C 0.6862(5) 0.1581(5) 0.1520(3) 0.0934(18) Uani 1 1 d . A . H4A H 0.6640 0.0983 0.1172 0.140 Uiso 1 1 calc R . . H4B H 0.7929 0.1212 0.1758 0.140 Uiso 1 1 calc R . . H4C H 0.6860 0.2348 0.1050 0.140 Uiso 1 1 calc R . . C5 C 0.6046(8) 0.2920(9) 0.3351(8) 0.061(3) Uani 0.70(2) 1 d P A 1 H5A H 0.7170 0.2471 0.3472 0.091 Uiso 0.70(2) 1 calc PR A 1 H5B H 0.5349 0.3035 0.4001 0.091 Uiso 0.70(2) 1 calc PR A 1 H5C H 0.6006 0.3739 0.2953 0.091 Uiso 0.70(2) 1 calc PR A 1 C5A C 0.643(2) 0.2991(19) 0.258(3) 0.100(13) Uani 0.30(2) 1 d P A 2 H5A1 H 0.7539 0.2508 0.2711 0.150 Uiso 0.30(2) 1 calc PR A 2 H5A2 H 0.5920 0.3538 0.3103 0.150 Uiso 0.30(2) 1 calc PR A 2 H5A3 H 0.6467 0.3500 0.1914 0.150 Uiso 0.30(2) 1 calc PR A 2 C6 C 0.5563(5) 0.0449(4) 0.3479(3) 0.0717(13) Uani 1 1 d . A . H6A H 0.5374 -0.0176 0.3146 0.108 Uiso 1 1 calc R . . H6B H 0.4790 0.0576 0.4099 0.108 Uiso 1 1 calc R . . H6C H 0.6679 0.0154 0.3649 0.108 Uiso 1 1 calc R . . C7 C -0.0159(4) 0.4308(3) 0.3381(2) 0.0444(8) Uani 1 1 d . A . H7A H 0.0259 0.5033 0.3182 0.067 Uiso 1 1 calc R . . H7B H -0.0829 0.4368 0.4044 0.067 Uiso 1 1 calc R . . H7C H -0.0822 0.4290 0.2878 0.067 Uiso 1 1 calc R . . C8 C 0.2365(4) 0.2855(3) 0.4659(2) 0.0490(8) Uani 1 1 d . A . H8A H 0.2836 0.3549 0.4567 0.073 Uiso 1 1 calc R . . H8B H 0.3199 0.2063 0.4825 0.073 Uiso 1 1 calc R . . H8C H 0.1457 0.2966 0.5212 0.073 Uiso 1 1 calc R . . C9 C 0.0699(4) 0.1479(3) 0.3758(3) 0.0466(8) Uani 1 1 d . A . H9A H 0.1551 0.0701 0.3932 0.070 Uiso 1 1 calc R . . H9B H 0.0249 0.1415 0.3166 0.070 Uiso 1 1 calc R . . H9C H -0.0170 0.1620 0.4332 0.070 Uiso 1 1 calc R . . C10 C 0.5393(4) 0.6805(4) 0.3165(3) 0.0489(8) Uani 1 1 d . A . H10A H 0.5825 0.7154 0.2495 0.073 Uiso 1 1 calc R . . H10B H 0.6072 0.5946 0.3339 0.073 Uiso 1 1 calc R . . H10C H 0.5400 0.7316 0.3670 0.073 Uiso 1 1 calc R . . C11 C 0.3092(5) 0.6258(4) 0.4138(3) 0.0582(10) Uani 1 1 d . A . H11A H 0.2024 0.6169 0.4105 0.087 Uiso 1 1 calc R . . H11B H 0.2982 0.6805 0.4642 0.087 Uiso 1 1 calc R . . H11C H 0.3846 0.5434 0.4331 0.087 Uiso 1 1 calc R . . C12 C 0.2729(4) 0.8091(3) 0.2885(3) 0.0446(8) Uani 1 1 d . A . H12A H 0.3259 0.8457 0.2246 0.053 Uiso 1 1 calc R . . H12B H 0.2702 0.8584 0.3420 0.053 Uiso 1 1 calc R . . C13 C 0.0988(4) 0.8223(3) 0.2756(3) 0.0437(8) Uani 1 1 d . A . H13A H 0.0439 0.7901 0.3408 0.052 Uiso 1 1 calc R . . H13B H 0.0405 0.9123 0.2599 0.052 Uiso 1 1 calc R . . C14 C -0.0855(3) 0.7570(3) 0.2050(3) 0.0419(7) Uani 1 1 d . A . H14A H -0.1197 0.7194 0.2732 0.063 Uiso 1 1 calc R . . H14B H -0.0945 0.7083 0.1551 0.063 Uiso 1 1 calc R . . H14C H -0.1556 0.8432 0.1920 0.063 Uiso 1 1 calc R . . C15 C 0.1297(4) 0.8193(4) 0.0971(3) 0.0530(9) Uani 1 1 d . A . H15A H 0.2428 0.8205 0.0909 0.080 Uiso 1 1 calc R . . H15B H 0.0579 0.9054 0.0879 0.080 Uiso 1 1 calc R . . H15C H 0.1194 0.7739 0.0452 0.080 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 K1 0.0398(4) 0.0289(3) 0.0254(3) -0.0056(2) 0.0011(2) -0.0138(3) P1 0.0468(4) 0.0323(4) 0.0206(3) -0.0022(3) -0.0023(3) -0.0217(3) Si1 0.0234(4) 0.0367(4) 0.0418(5) 0.0058(4) 0.0011(3) -0.0018(3) Si2 0.0254(4) 0.0262(4) 0.0240(4) -0.0026(3) 0.0047(3) -0.0074(3) N1 0.0265(12) 0.0401(13) 0.0315(12) -0.0103(10) -0.0031(9) -0.0099(10) N2 0.0270(12) 0.0345(13) 0.0339(12) -0.0060(10) -0.0020(10) -0.0103(10) B1 0.056(2) 0.043(2) 0.0221(16) 0.0015(14) 0.0020(15) -0.0236(18) C1 0.0256(13) 0.0279(13) 0.0185(12) -0.0018(10) 0.0011(10) -0.0070(10) C2 0.150(4) 0.050(2) 0.040(2) -0.0107(17) -0.001(2) -0.056(3) C3 0.047(2) 0.103(3) 0.0408(19) 0.0089(19) -0.0194(16) -0.040(2) C4 0.050(2) 0.121(4) 0.059(3) 0.008(3) 0.013(2) 0.023(3) C5 0.036(3) 0.081(5) 0.075(6) -0.034(4) -0.019(3) -0.010(3) C5A 0.024(8) 0.081(12) 0.18(3) 0.043(15) -0.043(13) -0.008(7) C6 0.049(2) 0.066(3) 0.060(2) 0.029(2) 0.0021(18) 0.0121(19) C7 0.0371(17) 0.0349(16) 0.0477(18) -0.0049(14) 0.0095(14) -0.0006(13) C8 0.062(2) 0.057(2) 0.0238(15) -0.0078(14) 0.0002(14) -0.0144(17) C9 0.0401(18) 0.0374(17) 0.058(2) -0.0009(15) 0.0091(15) -0.0168(14) C10 0.0349(17) 0.069(2) 0.0489(19) -0.0179(17) -0.0094(14) -0.0160(16) C11 0.057(2) 0.078(3) 0.0389(18) 0.0019(18) -0.0047(16) -0.027(2) C12 0.0424(18) 0.0381(17) 0.060(2) -0.0177(15) -0.0164(15) -0.0099(14) C13 0.0358(17) 0.0421(18) 0.0522(19) -0.0190(15) -0.0090(14) -0.0013(14) C14 0.0295(16) 0.0443(18) 0.0517(19) 0.0013(14) -0.0079(14) -0.0137(13) C15 0.046(2) 0.066(2) 0.0443(19) 0.0055(17) -0.0026(15) -0.0220(17) _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 N1 2.849(2) . ? K1 N2 2.975(2) . ? K1 H1B 3.05(4) . ? K1 H1C 2.75(3) . ? K1 C1 3.107(3) . ? P1 B1 1.933(3) . ? P1 C1 1.733(3) . ? P1 C2 1.836(3) . ? P1 C3 1.814(4) . ? Si1 C1 1.833(3) . ? Si1 C4 1.844(4) . ? Si1 C5 1.953(6) . ? Si1 C5A 1.773(19) . ? Si1 C6 1.861(4) . ? Si2 C1 1.829(2) . ? Si2 C7 1.883(3) . ? Si2 C8 1.880(3) . ? Si2 C9 1.890(3) . ? N1 C10 1.463(4) . ? N1 C11 1.455(4) . ? N1 C12 1.461(4) . ? N2 C13 1.452(4) . ? N2 C14 1.465(4) . ? N2 C15 1.455(4) . ? B1 H1A 1.11(4) . ? B1 H1B 1.12(4) . ? B1 H1C 1.08(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 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C5A H5A1 0.980 . ? C5A H5A2 0.980 . ? C5A H5A3 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 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.520(4) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 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 N1 K1 N2 62.82(6) . . ? N1 K1 H1B 159.0(7) . . ? N1 K1 H1C 163.4(7) . . ? N1 K1 C1 118.60(7) . . ? N2 K1 H1B 136.7(7) . . ? N2 K1 H1C 101.6(7) . . ? N2 K1 C1 116.75(7) . . ? H1B K1 H1C 35.2(10) . . ? H1B K1 C1 63.9(7) . . ? H1C K1 C1 72.6(7) . . ? B1 P1 C1 118.21(14) . . ? B1 P1 C2 108.38(17) . . ? B1 P1 C3 104.04(17) . . ? C1 P1 C2 112.22(16) . . ? C1 P1 C3 111.67(15) . . ? C2 P1 C3 100.6(2) . . ? C1 Si1 C4 117.96(17) . . ? C1 Si1 C5 111.8(2) . . ? C1 Si1 C5A 113.8(5) . . ? C1 Si1 C6 115.02(16) . . ? C4 Si1 C5 105.1(4) . . ? C4 Si1 C5A 77.0(15) . . ? C4 Si1 C6 104.2(2) . . ? C5 Si1 C6 101.0(4) . . ? C5A Si1 C6 122.6(8) . . ? C1 Si2 C7 114.23(13) . . ? C1 Si2 C8 112.96(14) . . ? C1 Si2 C9 114.71(13) . . ? C7 Si2 C8 102.42(16) . . ? C7 Si2 C9 106.82(15) . . ? C8 Si2 C9 104.53(16) . . ? K1 N1 C10 109.03(18) . . ? K1 N1 C11 109.4(2) . . ? K1 N1 C12 108.91(17) . . ? C10 N1 C11 109.6(3) . . ? C10 N1 C12 108.8(2) . . ? C11 N1 C12 111.2(3) . . ? K1 N2 C13 111.67(17) . . ? K1 N2 C14 124.36(18) . . ? K1 N2 C15 90.25(18) . . ? C13 N2 C14 109.2(2) . . ? C13 N2 C15 110.7(3) . . ? C14 N2 C15 108.7(2) . . ? P1 B1 H1A 108(2) . . ? P1 B1 H1B 109.5(19) . . ? P1 B1 H1C 105.5(18) . . ? H1A B1 H1B 116(3) . . ? H1A B1 H1C 110(3) . . ? H1B B1 H1C 108(3) . . ? K1 C1 P1 89.95(10) . . ? K1 C1 Si1 94.69(10) . . ? K1 C1 Si2 109.37(11) . . ? P1 C1 Si1 117.72(14) . . ? P1 C1 Si2 120.44(15) . . ? Si1 C1 Si2 116.05(13) . . ? 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 C5A H5A1 109.5 . . ? Si1 C5A H5A2 109.5 . . ? Si1 C5A H5A3 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 108.6 . . ? N1 C12 H12B 108.6 . . ? N1 C12 C13 114.5(3) . . ? H12A C12 H12B 107.6 . . ? H12A C12 C13 108.6 . . ? H12B C12 C13 108.6 . . ? N2 C13 C12 114.7(2) . . ? N2 C13 H13A 108.6 . . ? N2 C13 H13B 108.6 . . ? C12 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.860 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.055 #===END data_ki268_compound_2c _database_code_depnum_ccdc_archive 'CCDC 649163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H100 B2 K2 N6 P2 Si4' _chemical_formula_sum 'C36 H100 B2 K2 N6 P2 Si4' _chemical_formula_weight 891.34 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' N N 0.0061 0.0033 '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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.817(6) _cell_length_b 9.323(4) _cell_length_c 29.024(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.034(16) _cell_angle_gamma 90.00 _cell_volume 5774(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.937 _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 '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 64754 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5038 _reflns_number_gt 4290 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _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^)+(0.0793P)^2^+9.3890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5038 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 0.54178(3) 0.19867(6) 0.672946(19) 0.02982(18) Uani 1 1 d . . . P1 P 0.39932(3) 0.42359(7) 0.66496(2) 0.02384(18) Uani 1 1 d . . . Si1 Si 0.39746(3) 0.45392(8) 0.55881(2) 0.0280(2) Uani 1 1 d . . . Si2 Si 0.36009(3) 0.16861(8) 0.60194(2) 0.0292(2) Uani 1 1 d . . . N1 N 0.64559(12) 0.3381(3) 0.64205(8) 0.0408(6) Uani 1 1 d . . . N2 N 0.59230(10) 0.0609(3) 0.59771(8) 0.0369(6) Uani 1 1 d . . . N3 N 0.61097(12) -0.0685(3) 0.69571(8) 0.0397(6) Uani 1 1 d . . . B1 B 0.39814(16) 0.3069(4) 0.72035(10) 0.0350(7) Uani 1 1 d . . . H1A H 0.3547(15) 0.243(4) 0.7186(11) 0.050(9) Uiso 1 1 d . . . H1B H 0.3994(15) 0.382(4) 0.7496(11) 0.047(9) Uiso 1 1 d . . . H1C H 0.4403(17) 0.229(4) 0.7277(13) 0.062(10) Uiso 1 1 d . . . C1 C 0.40297(11) 0.3406(3) 0.61181(8) 0.0236(5) Uani 1 1 d . . . C2 C 0.33201(13) 0.5463(3) 0.66006(11) 0.0404(7) Uani 1 1 d . . . H2A H 0.3344 0.6204 0.6365 0.061 Uiso 1 1 calc R . . H2B H 0.3329 0.5916 0.6906 0.061 Uiso 1 1 calc R . . H2C H 0.2930 0.4921 0.6504 0.061 Uiso 1 1 calc R . . C3 C 0.46447(12) 0.5491(3) 0.68384(9) 0.0317(6) Uani 1 1 d . . . H3A H 0.4681 0.6122 0.6575 0.048 Uiso 1 1 calc R . . H3B H 0.5035 0.4952 0.6939 0.048 Uiso 1 1 calc R . . H3C H 0.4566 0.6070 0.7102 0.048 Uiso 1 1 calc R . . C4 C 0.31415(15) 0.4917(4) 0.52667(11) 0.0548(9) Uani 1 1 d . . . H4A H 0.2930 0.4011 0.5163 0.082 Uiso 1 1 calc R . . H4B H 0.3148 0.5524 0.4992 0.082 Uiso 1 1 calc R . . H4C H 0.2916 0.5413 0.5479 0.082 Uiso 1 1 calc R . . C5 C 0.43785(14) 0.3730(4) 0.51308(9) 0.0404(7) Uani 1 1 d . . . H5A H 0.4160 0.2851 0.5005 0.061 Uiso 1 1 calc R . . H5B H 0.4814 0.3502 0.5277 0.061 Uiso 1 1 calc R . . H5C H 0.4370 0.4418 0.4874 0.061 Uiso 1 1 calc R . . C6 C 0.43424(15) 0.6389(3) 0.56893(10) 0.0405(7) Uani 1 1 d . . . H6A H 0.4143 0.6925 0.5909 0.061 Uiso 1 1 calc R . . H6B H 0.4283 0.6903 0.5389 0.061 Uiso 1 1 calc R . . H6C H 0.4792 0.6292 0.5823 0.061 Uiso 1 1 calc R . . C7 C 0.27517(14) 0.1820(4) 0.60762(12) 0.0500(8) Uani 1 1 d . . . H7A H 0.2539 0.2563 0.5862 0.075 Uiso 1 1 calc R . . H7B H 0.2735 0.2070 0.6401 0.075 Uiso 1 1 calc R . . H7C H 0.2543 0.0896 0.5994 0.075 Uiso 1 1 calc R . . C8 C 0.39681(17) 0.0170(3) 0.64190(11) 0.0490(8) Uani 1 1 d . . . H8A H 0.4367 -0.0103 0.6340 0.074 Uiso 1 1 calc R . . H8B H 0.3685 -0.0657 0.6376 0.074 Uiso 1 1 calc R . . H8C H 0.4042 0.0488 0.6748 0.074 Uiso 1 1 calc R . . C9 C 0.35430(14) 0.0907(3) 0.54108(10) 0.0412(7) Uani 1 1 d . . . H9A H 0.3965 0.0736 0.5356 0.062 Uiso 1 1 calc R . . H9B H 0.3322 0.1582 0.5175 0.062 Uiso 1 1 calc R . . H9C H 0.3312 -0.0001 0.5386 0.062 Uiso 1 1 calc R . . C10 C 0.69803(19) 0.3899(5) 0.68043(12) 0.0665(11) Uani 1 1 d . . . H10A H 0.7223 0.3076 0.6953 0.100 Uiso 1 1 calc R . . H10B H 0.6807 0.4421 0.7041 0.100 Uiso 1 1 calc R . . H10C H 0.7254 0.4538 0.6670 0.100 Uiso 1 1 calc R . . C11 C 0.60929(16) 0.4615(3) 0.62184(13) 0.0488(8) Uani 1 1 d . . . H11A H 0.5711 0.4291 0.6003 0.073 Uiso 1 1 calc R . . H11B H 0.6343 0.5199 0.6045 0.073 Uiso 1 1 calc R . . H11C H 0.5980 0.5191 0.6471 0.073 Uiso 1 1 calc R . . C12 C 0.67304(16) 0.2591(4) 0.60780(12) 0.0504(8) Uani 1 1 d . . . H12A H 0.7060 0.1942 0.6248 0.060 Uiso 1 1 calc R . . H12B H 0.6932 0.3280 0.5897 0.060 Uiso 1 1 calc R . . C13 C 0.62614(16) 0.1734(4) 0.57451(11) 0.0505(8) Uani 1 1 d . . . H13A H 0.6476 0.1250 0.5519 0.061 Uiso 1 1 calc R . . H13B H 0.5946 0.2395 0.5563 0.061 Uiso 1 1 calc R . . C14 C 0.53632(14) 0.0154(4) 0.56344(10) 0.0453(8) Uani 1 1 d . . . H14A H 0.5132 -0.0556 0.5780 0.068 Uiso 1 1 calc R . . H14B H 0.5489 -0.0273 0.5360 0.068 Uiso 1 1 calc R . . H14C H 0.5094 0.0987 0.5534 0.068 Uiso 1 1 calc R . . C15 C 0.63285(16) -0.0594(4) 0.61386(11) 0.0494(8) Uani 1 1 d . . . H15A H 0.6757 -0.0232 0.6266 0.059 Uiso 1 1 calc R . . H15B H 0.6348 -0.1219 0.5866 0.059 Uiso 1 1 calc R . . C16 C 0.61206(18) -0.1467(3) 0.65086(12) 0.0531(9) Uani 1 1 d . . . H16A H 0.6403 -0.2304 0.6583 0.064 Uiso 1 1 calc R . . H16B H 0.5694 -0.1837 0.6378 0.064 Uiso 1 1 calc R . . C17 C 0.5777(2) -0.1570(4) 0.72354(13) 0.0685(11) Uani 1 1 d . . . H17A H 0.5743 -0.1056 0.7524 0.103 Uiso 1 1 calc R . . H17B H 0.6007 -0.2468 0.7319 0.103 Uiso 1 1 calc R . . H17C H 0.5357 -0.1783 0.7052 0.103 Uiso 1 1 calc R . . C18 C 0.67270(18) -0.0323(5) 0.72082(15) 0.0692(11) Uani 1 1 d . . . H18A H 0.6707 0.0035 0.7522 0.104 Uiso 1 1 calc R . . H18B H 0.6903 0.0420 0.7035 0.104 Uiso 1 1 calc R . . H18C H 0.6994 -0.1178 0.7239 0.104 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 K1 0.0303(3) 0.0362(3) 0.0237(3) -0.0042(2) 0.0073(2) 0.0016(2) P1 0.0219(3) 0.0329(4) 0.0162(3) -0.0005(3) 0.0028(2) 0.0010(3) Si1 0.0261(4) 0.0396(4) 0.0166(3) 0.0036(3) 0.0003(3) -0.0014(3) Si2 0.0276(4) 0.0345(4) 0.0266(4) -0.0050(3) 0.0081(3) -0.0073(3) N1 0.0500(15) 0.0411(14) 0.0357(13) 0.0027(11) 0.0190(11) -0.0014(12) N2 0.0295(12) 0.0554(15) 0.0236(11) -0.0120(11) 0.0003(9) 0.0043(11) N3 0.0516(15) 0.0345(13) 0.0338(13) -0.0019(10) 0.0103(11) -0.0051(11) B1 0.0402(18) 0.0478(19) 0.0182(14) 0.0023(13) 0.0085(13) -0.0015(15) C1 0.0222(12) 0.0331(13) 0.0147(11) -0.0003(10) 0.0023(9) -0.0026(10) C2 0.0308(15) 0.0512(18) 0.0393(16) -0.0050(14) 0.0074(12) 0.0114(13) C3 0.0319(14) 0.0380(15) 0.0232(13) -0.0056(11) 0.0009(11) -0.0043(12) C4 0.0408(18) 0.080(2) 0.0365(17) 0.0160(17) -0.0083(14) 0.0068(17) C5 0.0469(17) 0.0518(18) 0.0247(14) -0.0013(13) 0.0124(12) -0.0089(14) C6 0.0526(18) 0.0387(16) 0.0302(15) 0.0102(13) 0.0084(13) 0.0007(14) C7 0.0384(17) 0.060(2) 0.057(2) -0.0144(16) 0.0213(15) -0.0189(15) C8 0.070(2) 0.0372(17) 0.0416(17) 0.0004(14) 0.0159(16) -0.0032(16) C9 0.0321(15) 0.0543(18) 0.0361(16) -0.0149(14) 0.0047(12) -0.0132(14) C10 0.066(2) 0.087(3) 0.0434(19) 0.007(2) 0.0023(17) -0.023(2) C11 0.0488(19) 0.0395(17) 0.059(2) -0.0024(15) 0.0143(16) 0.0000(14) C12 0.056(2) 0.0513(19) 0.0501(19) 0.0031(16) 0.0244(16) -0.0004(16) C13 0.0514(19) 0.073(2) 0.0313(15) -0.0025(16) 0.0178(14) -0.0025(17) C14 0.0364(16) 0.0569(19) 0.0361(16) -0.0103(15) -0.0070(13) 0.0010(14) C15 0.0484(19) 0.059(2) 0.0376(17) -0.0118(15) 0.0019(14) 0.0191(16) C16 0.071(2) 0.0332(16) 0.055(2) -0.0072(15) 0.0123(17) 0.0015(16) C17 0.096(3) 0.062(2) 0.050(2) 0.0022(18) 0.022(2) -0.026(2) C18 0.060(2) 0.070(3) 0.069(3) -0.021(2) -0.0047(19) 0.003(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 N1 2.910(3) . ? K1 N2 2.939(2) . ? K1 N3 2.916(3) . ? K1 H1C 3.00(4) . ? K1 C1 3.440(3) . ? P1 B1 1.946(3) . ? P1 C1 1.742(2) . ? P1 C2 1.843(3) . ? P1 C3 1.834(3) . ? Si1 C1 1.849(2) . ? Si1 C4 1.895(3) . ? Si1 C5 1.896(3) . ? Si1 C6 1.899(3) . ? Si2 C1 1.848(3) . ? Si2 C7 1.898(3) . ? Si2 C8 1.897(3) . ? Si2 C9 1.890(3) . ? N1 C10 1.500(4) . ? N1 C11 1.450(4) . ? N1 C12 1.462(4) . ? N2 C13 1.519(4) . ? N2 C14 1.468(3) . ? N2 C15 1.445(4) . ? N3 C16 1.497(4) . ? N3 C17 1.451(4) . ? N3 C18 1.431(4) . ? B1 H1A 1.11(3) . ? B1 H1B 1.10(3) . ? B1 H1C 1.16(4) . ? 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 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 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.486(5) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.492(5) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 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 N1 K1 N2 61.95(7) . . ? N1 K1 N3 92.97(7) . . ? N1 K1 H1C 146.1(7) . . ? N1 K1 C1 109.11(7) . . ? N2 K1 N3 62.51(7) . . ? N2 K1 H1C 150.3(7) . . ? N2 K1 C1 102.19(6) . . ? N3 K1 H1C 111.4(7) . . ? N3 K1 C1 143.52(7) . . ? H1C K1 C1 64.5(7) . . ? B1 P1 C1 119.61(14) . . ? B1 P1 C2 105.26(15) . . ? B1 P1 C3 104.64(14) . . ? C1 P1 C2 112.95(13) . . ? C1 P1 C3 111.85(12) . . ? C2 P1 C3 100.50(14) . . ? C1 Si1 C4 113.90(14) . . ? C1 Si1 C5 113.32(13) . . ? C1 Si1 C6 115.97(12) . . ? C4 Si1 C5 105.52(15) . . ? C4 Si1 C6 103.78(16) . . ? C5 Si1 C6 103.09(14) . . ? C1 Si2 C7 113.65(13) . . ? C1 Si2 C8 114.59(14) . . ? C1 Si2 C9 114.30(12) . . ? C7 Si2 C8 106.93(16) . . ? C7 Si2 C9 103.31(14) . . ? C8 Si2 C9 102.86(15) . . ? K1 N1 C10 115.91(19) . . ? K1 N1 C11 94.86(18) . . ? K1 N1 C12 116.12(19) . . ? C10 N1 C11 108.2(3) . . ? C10 N1 C12 108.1(3) . . ? C11 N1 C12 113.0(3) . . ? K1 N2 C13 108.66(17) . . ? K1 N2 C14 104.00(17) . . ? K1 N2 C15 113.42(17) . . ? C13 N2 C14 108.2(2) . . ? C13 N2 C15 111.0(2) . . ? C14 N2 C15 111.2(3) . . ? K1 N3 C16 108.70(18) . . ? K1 N3 C17 108.5(2) . . ? K1 N3 C18 107.6(2) . . ? C16 N3 C17 107.9(3) . . ? C16 N3 C18 111.9(3) . . ? C17 N3 C18 112.2(3) . . ? P1 B1 H1A 114.9(17) . . ? P1 B1 H1B 106.2(17) . . ? P1 B1 H1C 111.0(18) . . ? H1A B1 H1B 105(2) . . ? H1A B1 H1C 108(3) . . ? H1B B1 H1C 112(2) . . ? K1 C1 P1 84.94(8) . . ? K1 C1 Si1 123.12(10) . . ? K1 C1 Si2 96.25(10) . . ? P1 C1 Si1 118.42(14) . . ? P1 C1 Si2 114.04(13) . . ? Si1 C1 Si2 115.06(12) . . ? 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 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.0 . . ? N1 C12 H12B 109.0 . . ? N1 C12 C13 112.9(3) . . ? H12A C12 H12B 107.8 . . ? H12A C12 C13 109.0 . . ? H12B C12 C13 109.0 . . ? N2 C13 C12 114.6(3) . . ? N2 C13 H13A 108.6 . . ? N2 C13 H13B 108.6 . . ? C12 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 108.9 . . ? N2 C15 H15B 108.9 . . ? N2 C15 C16 113.6(3) . . ? H15A C15 H15B 107.7 . . ? H15A C15 C16 108.9 . . ? H15B C15 C16 108.9 . . ? N3 C16 C15 115.0(3) . . ? N3 C16 H16A 108.5 . . ? N3 C16 H16B 108.5 . . ? C15 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.784 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.073 #===END data_ki271_compound_2d _database_code_depnum_ccdc_archive 'CCDC 649164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H59 B K O8 P Si2' _chemical_formula_sum 'C25 H59 B K O8 P Si2' _chemical_formula_weight 624.78 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.526(8) _cell_length_b 15.475(9) _cell_length_c 18.411(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3569(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 25.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6905 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 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_% 5 _diffrn_reflns_number 21325 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 22.56 _reflns_number_total 5086 _reflns_number_gt 4632 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _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^)+(0.0794P)^2^+15.4087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(2) _refine_ls_number_reflns 5086 _refine_ls_number_parameters 461 _refine_ls_number_restraints 580 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.2714 _refine_ls_wR_factor_gt 0.2661 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.004 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 0.5060(4) 0.07629(12) 0.68669(10) 0.0956(11) Uani 1 1 d . . . P1 P 0.4995(2) -0.00517(10) 1.13658(10) 0.0419(5) Uani 1 1 d . . . Si1 Si 0.4901(3) 0.12516(13) 1.26454(12) 0.0595(7) Uani 1 1 d . . . Si2 Si 0.4876(3) 0.18567(12) 1.10280(12) 0.0554(7) Uani 1 1 d . . . C2 C 0.3984(8) -0.0758(7) 1.1746(7) 0.071(3) Uani 1 1 d . . . H2D H 0.4019 -0.0737 1.2277 0.106 Uiso 1 1 calc R . . H2E H 0.4110 -0.1352 1.1581 0.106 Uiso 1 1 calc R . . H2F H 0.3276 -0.0568 1.1584 0.106 Uiso 1 1 calc R . . C1 C 0.4812(13) 0.0995(5) 1.1683(5) 0.083(4) Uani 1 1 d . . . B1 B 0.6181(9) -0.0508(10) 1.1719(7) 0.067(3) Uani 1 1 d . . . H1A H 0.6800 -0.0255 1.1473 0.100 Uiso 1 1 calc R . . H1B H 0.6175 -0.1134 1.1641 0.100 Uiso 1 1 calc R . . H1C H 0.6226 -0.0388 1.2241 0.100 Uiso 1 1 calc R . . C3 C 0.5106(9) -0.0296(5) 1.0329(5) 0.064(2) Uani 1 1 d . . . H3A H 0.5844 -0.0206 1.0169 0.096 Uiso 1 1 calc R . . H3B H 0.4631 0.0093 1.0060 0.096 Uiso 1 1 calc R . . H3C H 0.4898 -0.0896 1.0237 0.096 Uiso 1 1 calc R . . C4 C 0.6270(10) 0.1831(11) 1.2872(10) 0.111(5) Uani 1 1 d . . . H4A H 0.6857 0.1517 1.2638 0.167 Uiso 1 1 calc R . . H4B H 0.6380 0.1835 1.3399 0.167 Uiso 1 1 calc R . . H4C H 0.6252 0.2426 1.2690 0.167 Uiso 1 1 calc R . . C5 C 0.3866(11) 0.1908(9) 1.2970(7) 0.095(4) Uani 1 1 d . . . H5A H 0.3239 0.1551 1.3075 0.142 Uiso 1 1 calc R . . H5B H 0.3682 0.2340 1.2601 0.142 Uiso 1 1 calc R . . H5C H 0.4098 0.2201 1.3414 0.142 Uiso 1 1 calc R . . C6 C 0.4894(17) 0.0320(6) 1.3291(5) 0.120(6) Uani 1 1 d . . . H6A H 0.4310 -0.0073 1.3166 0.179 Uiso 1 1 calc R . . H6B H 0.4794 0.0534 1.3788 0.179 Uiso 1 1 calc R . . H6C H 0.5576 0.0011 1.3259 0.179 Uiso 1 1 calc R . . C7 C 0.4686(11) 0.2969(5) 1.1466(6) 0.086(4) Uani 1 1 d . . . H7A H 0.5218 0.3048 1.1851 0.129 Uiso 1 1 calc R . . H7B H 0.3968 0.3007 1.1675 0.129 Uiso 1 1 calc R . . H7C H 0.4776 0.3419 1.1097 0.129 Uiso 1 1 calc R . . C8 C 0.3777(7) 0.1881(7) 1.0380(8) 0.077(4) Uani 1 1 d . . . H8A H 0.3789 0.1354 1.0084 0.115 Uiso 1 1 calc R . . H8B H 0.3852 0.2387 1.0063 0.115 Uiso 1 1 calc R . . H8C H 0.3098 0.1916 1.0642 0.115 Uiso 1 1 calc R . . C9 C 0.6182(9) 0.1883(8) 1.0475(8) 0.090(4) Uani 1 1 d . . . H9A H 0.6296 0.1320 1.0244 0.134 Uiso 1 1 calc R . . H9B H 0.6782 0.2012 1.0799 0.134 Uiso 1 1 calc R . . H9C H 0.6133 0.2331 1.0100 0.134 Uiso 1 1 calc R . . O1 O 0.5870(11) -0.0402(7) 0.7926(7) 0.063(3) Uani 0.549(9) 1 d PDU A 1 C10 C 0.5184(16) -0.068(2) 0.8445(14) 0.079(5) Uani 0.549(9) 1 d PDU A 1 H10A H 0.5160 -0.0291 0.8870 0.095 Uiso 0.549(9) 1 calc PR A 1 H10B H 0.5350 -0.1279 0.8607 0.095 Uiso 0.549(9) 1 calc PR A 1 C11 C 0.4158(18) -0.0642(13) 0.7989(16) 0.081(5) Uani 0.549(9) 1 d PDU A 1 H11A H 0.3537 -0.0428 0.8269 0.098 Uiso 0.549(9) 1 calc PR A 1 H11B H 0.3983 -0.1199 0.7754 0.098 Uiso 0.549(9) 1 calc PR A 1 O2 O 0.3809(10) 0.0108(8) 0.7833(7) 0.070(3) Uani 0.549(9) 1 d PDU A 1 C12 C 0.329(3) 0.0621(13) 0.8369(14) 0.086(5) Uani 0.549(9) 1 d PDU A 1 H12A H 0.3674 0.0593 0.8839 0.103 Uiso 0.549(9) 1 calc PR A 1 H12B H 0.2543 0.0433 0.8442 0.103 Uiso 0.549(9) 1 calc PR A 1 C13 C 0.3340(15) 0.1507(13) 0.8054(15) 0.084(5) Uani 0.549(9) 1 d PDU A 1 H13A H 0.2917 0.1497 0.7600 0.100 Uiso 0.549(9) 1 calc PR A 1 H13B H 0.2963 0.1896 0.8394 0.100 Uiso 0.549(9) 1 calc PR A 1 O3 O 0.4293(11) 0.1887(8) 0.7893(9) 0.080(4) Uani 0.549(9) 1 d PDU A 1 C14 C 0.5064(18) 0.226(2) 0.8382(16) 0.085(5) Uani 0.549(9) 1 d PDU A 1 H14A H 0.4913 0.2885 0.8456 0.102 Uiso 0.549(9) 1 calc PR A 1 H14B H 0.5042 0.1968 0.8859 0.102 Uiso 0.549(9) 1 calc PR A 1 C15 C 0.6013(15) 0.2156(10) 0.8071(14) 0.078(4) Uani 0.549(9) 1 d PDU A 1 H15A H 0.6538 0.2462 0.8380 0.094 Uiso 0.549(9) 1 calc PR A 1 H15B H 0.5989 0.2472 0.7603 0.094 Uiso 0.549(9) 1 calc PR A 1 O4 O 0.6454(12) 0.1326(9) 0.7919(9) 0.077(4) Uani 0.549(9) 1 d PDU A 1 C16 C 0.670(2) 0.0808(12) 0.8561(12) 0.084(5) Uani 0.549(9) 1 d PDU A 1 H16A H 0.7371 0.1004 0.8796 0.101 Uiso 0.549(9) 1 calc PR A 1 H16B H 0.6114 0.0827 0.8920 0.101 Uiso 0.549(9) 1 calc PR A 1 C17 C 0.6820(15) -0.0043(12) 0.8255(13) 0.085(4) Uani 0.549(9) 1 d PDU A 1 H17A H 0.7061 -0.0440 0.8643 0.102 Uiso 0.549(9) 1 calc PR A 1 H17B H 0.7390 -0.0022 0.7883 0.102 Uiso 0.549(9) 1 calc PR A 1 O1A O 0.4802(14) -0.0803(16) 0.8357(11) 0.078(4) Uani 0.451(9) 1 d PDU A 2 C10A C 0.4148(17) -0.0617(15) 0.7794(15) 0.071(6) Uani 0.451(9) 1 d PDU A 2 H10C H 0.3891 -0.1155 0.7561 0.085 Uiso 0.451(9) 1 calc PR A 2 H10D H 0.4528 -0.0266 0.7426 0.085 Uiso 0.451(9) 1 calc PR A 2 C11A C 0.3238(14) -0.0123(14) 0.8106(14) 0.076(5) Uani 0.451(9) 1 d PDU A 2 H11C H 0.3286 0.0061 0.8620 0.091 Uiso 0.451(9) 1 calc PR A 2 H11D H 0.2510 -0.0258 0.7931 0.091 Uiso 0.451(9) 1 calc PR A 2 O2A O 0.335(3) 0.0839(15) 0.8540(14) 0.103(7) Uani 0.451(9) 1 d PDU A 2 C12A C 0.3469(15) 0.1323(12) 0.7870(13) 0.058(5) Uani 0.451(9) 1 d PDU A 2 H12C H 0.2781 0.1396 0.7613 0.070 Uiso 0.451(9) 1 calc PR A 2 H12D H 0.4001 0.1058 0.7539 0.070 Uiso 0.451(9) 1 calc PR A 2 C13A C 0.3859(15) 0.2146(13) 0.8191(15) 0.069(4) Uani 0.451(9) 1 d PDU A 2 H13C H 0.3812 0.2609 0.7821 0.083 Uiso 0.451(9) 1 calc PR A 2 H13D H 0.3390 0.2309 0.8601 0.083 Uiso 0.451(9) 1 calc PR A 2 O3A O 0.4963(16) 0.2083(16) 0.8451(13) 0.087(5) Uani 0.451(9) 1 d PDU A 2 C14A C 0.5728(14) 0.1894(12) 0.7896(15) 0.067(5) Uani 0.451(9) 1 d PDU A 2 H14C H 0.5383 0.1536 0.7518 0.080 Uiso 0.451(9) 1 calc PR A 2 H14D H 0.5956 0.2442 0.7666 0.080 Uiso 0.451(9) 1 calc PR A 2 C15A C 0.6597(17) 0.1476(14) 0.815(2) 0.084(5) Uani 0.451(9) 1 d PDU A 2 H15C H 0.6792 0.1744 0.8617 0.100 Uiso 0.451(9) 1 calc PR A 2 H15D H 0.7190 0.1597 0.7806 0.100 Uiso 0.451(9) 1 calc PR A 2 O4A O 0.6569(15) 0.0551(11) 0.8259(13) 0.098(5) Uani 0.451(9) 1 d PDU A 2 C16A C 0.6413(17) -0.0106(13) 0.7759(13) 0.078(5) Uani 0.451(9) 1 d PDU A 2 H16C H 0.7107 -0.0293 0.7556 0.094 Uiso 0.451(9) 1 calc PR A 2 H16D H 0.5959 0.0102 0.7356 0.094 Uiso 0.451(9) 1 calc PR A 2 C17A C 0.5910(15) -0.0807(13) 0.8116(15) 0.074(5) Uani 0.451(9) 1 d PDU A 2 H17C H 0.6347 -0.0932 0.8552 0.089 Uiso 0.451(9) 1 calc PR A 2 H17D H 0.5988 -0.1312 0.7791 0.089 Uiso 0.451(9) 1 calc PR A 2 O5 O 0.5001(7) 0.2043(3) 0.5802(3) 0.0751(16) Uani 1 1 d DU A . C18 C 0.5653(10) 0.2053(7) 0.5229(7) 0.090(3) Uani 1 1 d DU . . H18A H 0.5823 0.2651 0.5077 0.108 Uiso 1 1 calc R A . H18B H 0.5340 0.1737 0.4812 0.108 Uiso 1 1 calc R . . C19 C 0.6617(10) 0.1601(9) 0.5517(10) 0.115(4) Uani 1 1 d DU A . H19A H 0.7135 0.1548 0.5113 0.138 Uiso 1 1 calc R . . H19B H 0.6946 0.1982 0.5886 0.138 Uiso 1 1 calc R . . O6 O 0.6499(5) 0.0802(5) 0.5820(6) 0.082(2) Uani 1 1 d DU A . C20 C 0.6595(9) 0.0158(8) 0.5295(8) 0.092(3) Uani 1 1 d DU . . H20A H 0.7351 0.0081 0.5152 0.111 Uiso 1 1 calc R A . H20B H 0.6173 0.0306 0.4858 0.111 Uiso 1 1 calc R . . C21 C 0.6178(10) -0.0639(7) 0.5638(8) 0.094(3) Uani 1 1 d DU A . H21A H 0.6234 -0.1119 0.5285 0.113 Uiso 1 1 calc R . . H21B H 0.6636 -0.0785 0.6059 0.113 Uiso 1 1 calc R . . O7 O 0.5094(7) -0.0582(3) 0.5882(3) 0.0748(17) Uani 1 1 d DU A . C22 C 0.4285(11) -0.0600(7) 0.5346(8) 0.100(4) Uani 1 1 d DU . . H22A H 0.4536 -0.0309 0.4899 0.121 Uiso 1 1 calc R A . H22B H 0.4101 -0.1206 0.5224 0.121 Uiso 1 1 calc R . . C23 C 0.3411(9) -0.0185(9) 0.5615(10) 0.112(4) Uani 1 1 d DU A . H23A H 0.3148 -0.0530 0.6031 0.134 Uiso 1 1 calc R . . H23B H 0.2852 -0.0209 0.5236 0.134 Uiso 1 1 calc R . . O8 O 0.3479(5) 0.0696(5) 0.5854(6) 0.090(3) Uani 1 1 d DU A . C24 C 0.3396(10) 0.1344(10) 0.5308(9) 0.122(5) Uani 1 1 d DU . . H24A H 0.3752 0.1149 0.4857 0.147 Uiso 1 1 calc R A . H24B H 0.2636 0.1461 0.5197 0.147 Uiso 1 1 calc R . . C25 C 0.3897(10) 0.2105(7) 0.5574(8) 0.103(4) Uani 1 1 d DU A . H25A H 0.3475 0.2317 0.5992 0.124 Uiso 1 1 calc R . . H25B H 0.3853 0.2551 0.5190 0.124 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 K1 0.203(3) 0.0420(10) 0.0420(10) 0.0010(7) -0.009(2) 0.033(2) P1 0.0505(10) 0.0243(8) 0.0508(10) -0.0019(7) -0.0032(12) -0.0119(11) Si1 0.100(2) 0.0287(10) 0.0497(12) -0.0032(9) -0.0042(17) -0.0051(15) Si2 0.0922(19) 0.0237(10) 0.0504(12) 0.0038(8) -0.0060(16) -0.0080(14) C2 0.071(7) 0.059(7) 0.082(8) -0.002(5) -0.008(6) -0.040(5) C1 0.174(13) 0.014(3) 0.060(5) 0.000(3) -0.026(8) 0.011(6) B1 0.060(7) 0.093(10) 0.048(7) -0.005(6) -0.006(5) 0.006(7) C3 0.078(6) 0.037(4) 0.077(6) -0.002(4) -0.005(6) -0.009(5) C4 0.064(7) 0.123(12) 0.147(14) 0.009(12) -0.015(8) -0.006(8) C5 0.131(11) 0.101(10) 0.052(7) 0.012(7) 0.033(7) -0.025(9) C6 0.261(19) 0.047(5) 0.051(5) 0.004(4) -0.060(11) 0.020(10) C7 0.157(12) 0.026(4) 0.074(6) 0.006(4) -0.032(7) -0.006(6) C8 0.036(5) 0.045(6) 0.149(12) 0.027(7) -0.005(6) -0.003(5) C9 0.069(7) 0.055(7) 0.145(13) 0.033(8) -0.013(7) -0.014(6) O1 0.113(7) 0.028(6) 0.048(7) 0.011(5) 0.016(6) 0.015(6) C10 0.090(10) 0.075(10) 0.072(10) 0.028(9) -0.008(8) 0.010(10) C11 0.101(8) 0.084(10) 0.059(11) -0.033(9) -0.025(9) 0.004(9) O2 0.085(8) 0.067(7) 0.058(7) 0.000(6) -0.024(6) -0.048(6) C12 0.083(10) 0.068(9) 0.107(11) -0.015(8) -0.026(9) -0.019(8) C13 0.069(8) 0.077(8) 0.105(12) 0.008(9) -0.039(9) 0.001(8) O3 0.089(7) 0.057(7) 0.093(8) -0.001(6) -0.020(7) 0.001(6) C14 0.080(8) 0.063(10) 0.112(10) -0.009(8) -0.006(8) -0.013(8) C15 0.087(8) 0.058(8) 0.089(10) 0.010(8) 0.020(8) -0.010(8) O4 0.085(8) 0.063(7) 0.084(9) 0.023(7) 0.021(7) -0.005(6) C16 0.086(10) 0.072(9) 0.095(11) 0.009(8) -0.026(10) -0.007(8) C17 0.098(9) 0.062(8) 0.095(11) 0.020(8) 0.023(8) 0.012(8) O1A 0.090(8) 0.072(9) 0.073(8) 0.015(7) -0.004(8) 0.002(8) C10A 0.089(9) 0.083(11) 0.040(11) -0.016(9) -0.012(8) -0.002(9) C11A 0.083(10) 0.071(10) 0.073(11) -0.026(9) -0.014(9) -0.003(9) O2A 0.099(12) 0.093(12) 0.118(13) -0.015(10) 0.024(13) -0.027(11) C12A 0.053(9) 0.043(9) 0.080(10) -0.033(7) -0.020(8) 0.019(7) C13A 0.060(7) 0.053(8) 0.095(11) -0.031(8) 0.005(8) 0.009(8) O3A 0.082(7) 0.067(10) 0.113(9) -0.023(8) -0.008(7) -0.019(8) C14A 0.051(8) 0.052(9) 0.098(11) 0.024(9) 0.010(8) -0.021(7) C15A 0.076(9) 0.069(8) 0.106(12) 0.038(9) 0.015(9) -0.006(8) O4A 0.102(10) 0.069(8) 0.124(11) 0.023(8) 0.009(10) 0.013(8) C16A 0.092(11) 0.065(9) 0.077(12) 0.030(8) 0.020(10) 0.020(9) C17A 0.089(8) 0.060(9) 0.073(11) 0.034(9) 0.001(8) 0.023(9) O5 0.121(5) 0.030(3) 0.075(4) 0.001(2) 0.007(5) -0.003(4) C18 0.136(8) 0.049(6) 0.086(7) 0.014(5) 0.032(6) 0.001(6) C19 0.098(7) 0.096(7) 0.151(11) 0.033(7) 0.015(8) -0.017(6) O6 0.044(4) 0.056(4) 0.147(8) -0.008(4) -0.019(4) -0.002(3) C20 0.071(6) 0.087(6) 0.118(9) 0.006(6) 0.016(6) 0.018(6) C21 0.117(7) 0.047(5) 0.119(9) -0.001(6) 0.007(7) 0.030(6) O7 0.110(5) 0.032(3) 0.083(4) -0.006(3) -0.012(5) 0.019(4) C22 0.135(8) 0.044(6) 0.122(9) -0.029(6) -0.036(7) -0.021(6) C23 0.076(6) 0.102(7) 0.158(11) -0.015(8) -0.011(7) -0.038(6) O8 0.037(4) 0.086(5) 0.145(8) 0.018(5) 0.024(4) -0.009(4) C24 0.070(7) 0.129(8) 0.167(12) 0.056(8) -0.026(8) -0.025(7) C25 0.124(7) 0.057(6) 0.129(10) 0.015(6) -0.024(7) 0.045(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 K1 O1 2.842(12) . ? K1 O2 2.577(14) . ? K1 O3 2.742(16) . ? K1 O4 2.749(17) . ? K1 O5 2.788(6) . ? K1 O6 2.639(10) . ? K1 O7 2.762(6) . ? K1 O8 2.723(10) . ? P1 C2 1.814(10) . ? P1 C1 1.737(8) . ? P1 B1 1.769(12) . ? P1 C3 1.951(9) . ? Si1 C1 1.819(9) . ? Si1 C4 1.979(13) . ? Si1 C5 1.753(14) . ? Si1 C6 1.869(9) . ? Si2 C1 1.800(8) . ? Si2 C7 1.915(9) . ? Si2 C8 1.823(11) . ? Si2 C9 1.928(13) . ? C2 H2D 0.980 . ? C2 H2E 0.980 . ? C2 H2F 0.980 . ? B1 H1A 0.980 . ? B1 H1B 0.980 . ? B1 H1C 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 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 . ? O1 C10 1.358(18) . ? O1 C17 1.446(18) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.54(2) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? O2 C12 1.42(2) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.49(2) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 O3 1.364(18) . ? O3 C14 1.442(19) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.33(2) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 O4 1.426(19) . ? O4 C16 1.463(19) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.44(2) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? O1A C10A 1.352(18) . ? O1A C17A 1.457(18) . ? C10A H10C 0.990 . ? C10A H10D 0.990 . ? C10A C11A 1.49(2) . ? C11A H11C 0.990 . ? C11A H11D 0.990 . ? O2A C12A 1.45(2) . ? C12A H12C 0.990 . ? C12A H12D 0.990 . ? C12A C13A 1.49(2) . ? C13A H13C 0.990 . ? C13A H13D 0.990 . ? C13A O3A 1.467(19) . ? O3A C14A 1.430(18) . ? C14A H14C 0.990 . ? C14A H14D 0.990 . ? C14A C15A 1.35(2) . ? C15A H15C 0.990 . ? C15A H15D 0.990 . ? C15A O4A 1.45(2) . ? O4A C16A 1.38(2) . ? C16A H16C 0.990 . ? C16A H16D 0.990 . ? C16A C17A 1.42(2) . ? C17A H17C 0.990 . ? C17A H17D 0.990 . ? O5 C18 1.334(12) . ? O5 C25 1.449(13) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.492(16) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19 O6 1.365(15) . ? O6 C20 1.394(14) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.480(15) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 O7 1.432(13) . ? O7 C22 1.415(13) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.362(16) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 O8 1.434(15) . ? O8 C24 1.424(15) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 C25 1.421(17) . ? C25 H25A 0.990 . ? C25 H25B 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 O1 K1 O2 59.7(4) . . ? O1 K1 O3 93.2(4) . . ? O1 K1 O4 59.4(4) . . ? O1 K1 O5 160.4(4) . . ? O1 K1 O6 105.7(4) . . ? O1 K1 O7 88.1(3) . . ? O1 K1 O8 134.9(3) . . ? O2 K1 O3 64.0(4) . . ? O2 K1 O4 91.4(4) . . ? O2 K1 O5 138.4(4) . . ? O2 K1 O6 158.1(3) . . ? O2 K1 O7 99.6(3) . . ? O2 K1 O8 90.9(3) . . ? O3 K1 O4 62.4(4) . . ? O3 K1 O5 91.4(3) . . ? O3 K1 O6 136.7(3) . . ? O3 K1 O7 159.5(4) . . ? O3 K1 O8 104.0(4) . . ? O4 K1 O5 106.7(4) . . ? O4 K1 O6 94.2(4) . . ? O4 K1 O7 133.8(4) . . ? O4 K1 O8 163.1(3) . . ? O5 K1 O6 59.2(2) . . ? O5 K1 O7 94.24(18) . . ? O5 K1 O8 61.7(2) . . ? O6 K1 O7 61.8(2) . . ? O6 K1 O8 89.9(2) . . ? O7 K1 O8 62.1(2) . . ? C2 P1 C1 109.9(6) . . ? C2 P1 B1 101.8(6) . . ? C2 P1 C3 108.1(5) . . ? C1 P1 B1 111.1(7) . . ? C1 P1 C3 121.3(4) . . ? B1 P1 C3 102.9(5) . . ? C1 Si1 C4 110.9(7) . . ? C1 Si1 C5 114.4(6) . . ? C1 Si1 C6 116.8(4) . . ? C4 Si1 C5 107.9(6) . . ? C4 Si1 C6 102.7(7) . . ? C5 Si1 C6 103.1(7) . . ? C1 Si2 C7 112.2(4) . . ? C1 Si2 C8 114.9(6) . . ? C1 Si2 C9 114.0(6) . . ? C7 Si2 C8 99.4(5) . . ? C7 Si2 C9 108.0(6) . . ? C8 Si2 C9 107.1(5) . . ? P1 C2 H2D 109.5 . . ? P1 C2 H2E 109.5 . . ? P1 C2 H2F 109.5 . . ? H2D C2 H2E 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? P1 C1 Si1 121.6(5) . . ? P1 C1 Si2 117.4(5) . . ? Si1 C1 Si2 119.2(4) . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1B 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 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 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 . . ? K1 O1 C10 117.4(13) . . ? K1 O1 C17 109.7(10) . . ? C10 O1 C17 110.4(16) . . ? O1 C10 H10A 112.3 . . ? O1 C10 H10B 112.3 . . ? O1 C10 C11 97.5(15) . . ? H10A C10 H10B 109.9 . . ? H10A C10 C11 112.3 . . ? H10B C10 C11 112.3 . . ? C10 C11 H11A 112.8 . . ? C10 C11 H11B 112.7 . . ? H11A C11 H11B 110.2 . . ? K1 O2 C12 122.5(11) . . ? O2 C12 H12A 111.2 . . ? O2 C12 H12B 111.2 . . ? O2 C12 C13 102.8(16) . . ? H12A C12 H12B 109.1 . . ? H12A C12 C13 111.2 . . ? H12B C12 C13 111.2 . . ? C12 C13 H13A 107.0 . . ? C12 C13 H13B 107.0 . . ? C12 C13 O3 121.2(19) . . ? H13A C13 H13B 106.8 . . ? H13A C13 O3 107.0 . . ? H13B C13 O3 107.0 . . ? K1 O3 C13 100.5(13) . . ? K1 O3 C14 116.8(12) . . ? C13 O3 C14 128.6(18) . . ? O3 C14 H14A 110.5 . . ? O3 C14 H14B 110.5 . . ? O3 C14 C15 106.2(17) . . ? H14A C14 H14B 108.7 . . ? H14A C14 C15 110.5 . . ? H14B C14 C15 110.5 . . ? C14 C15 H15A 106.6 . . ? C14 C15 H15B 106.6 . . ? C14 C15 O4 122.9(18) . . ? H15A C15 H15B 106.6 . . ? H15A C15 O4 106.6 . . ? H15B C15 O4 106.6 . . ? K1 O4 C15 100.2(12) . . ? K1 O4 C16 122.1(12) . . ? C15 O4 C16 114.7(16) . . ? O4 C16 H16A 111.4 . . ? O4 C16 H16B 111.4 . . ? O4 C16 C17 101.9(16) . . ? H16A C16 H16B 109.3 . . ? H16A C16 C17 111.4 . . ? H16B C16 C17 111.4 . . ? O1 C17 C16 115.6(16) . . ? O1 C17 H17A 108.4 . . ? O1 C17 H17B 108.4 . . ? C16 C17 H17A 108.4 . . ? C16 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C10A O1A C17A 110.2(16) . . ? O1A C10A H10C 110.5 . . ? O1A C10A H10D 110.5 . . ? O1A C10A C11A 106.1(18) . . ? H10C C10A H10D 108.7 . . ? H10C C10A C11A 110.5 . . ? H10D C10A C11A 110.5 . . ? C10A C11A H11C 118.1 . . ? C10A C11A H11D 118.1 . . ? H11C C11A H11D 115.3 . . ? O2A C12A H12C 112.2 . . ? O2A C12A H12D 112.2 . . ? O2A C12A C13A 97.9(17) . . ? H12C C12A H12D 109.8 . . ? H12C C12A C13A 112.2 . . ? H12D C12A C13A 112.2 . . ? C12A C13A H13C 109.1 . . ? C12A C13A H13D 109.1 . . ? C12A C13A O3A 112.5(16) . . ? H13C C13A H13D 107.8 . . ? H13C C13A O3A 109.1 . . ? H13D C13A O3A 109.1 . . ? C13A O3A C14A 114.3(17) . . ? O3A C14A H14C 108.9 . . ? O3A C14A H14D 108.9 . . ? O3A C14A C15A 113(2) . . ? H14C C14A H14D 107.8 . . ? H14C C14A C15A 108.9 . . ? H14D C14A C15A 108.9 . . ? C14A C15A H15C 107.2 . . ? C14A C15A H15D 107.2 . . ? C14A C15A O4A 120.3(17) . . ? H15C C15A H15D 106.9 . . ? H15C C15A O4A 107.3 . . ? H15D C15A O4A 107.3 . . ? K1 O4A C15A 78.4(14) . . ? K1 O4A C16A 57.3(11) . . ? C15A O4A C16A 129(2) . . ? O4A C16A H16C 110.0 . . ? O4A C16A H16D 110.0 . . ? O4A C16A C17A 108.4(18) . . ? H16C C16A H16D 108.4 . . ? H16C C16A C17A 110.0 . . ? H16D C16A C17A 110.0 . . ? O1A C17A C16A 124.1(17) . . ? O1A C17A H17C 106.3 . . ? O1A C17A H17D 106.3 . . ? C16A C17A H17C 106.3 . . ? C16A C17A H17D 106.3 . . ? H17C C17A H17D 106.4 . . ? K1 O5 C18 123.2(6) . . ? K1 O5 C25 106.0(6) . . ? C18 O5 C25 110.8(10) . . ? O5 C18 H18A 111.4 . . ? O5 C18 H18B 111.4 . . ? O5 C18 C19 102.0(10) . . ? H18A C18 H18B 109.2 . . ? H18A C18 C19 111.4 . . ? H18B C18 C19 111.4 . . ? C18 C19 H19A 107.6 . . ? C18 C19 H19B 107.6 . . ? C18 C19 O6 118.8(10) . . ? H19A C19 H19B 107.0 . . ? H19A C19 O6 107.6 . . ? H19B C19 O6 107.6 . . ? K1 O6 C19 113.2(8) . . ? K1 O6 C20 123.2(6) . . ? C19 O6 C20 110.8(12) . . ? O6 C20 H20A 110.6 . . ? O6 C20 H20B 110.6 . . ? O6 C20 C21 105.7(10) . . ? H20A C20 H20B 108.7 . . ? H20A C20 C21 110.6 . . ? H20B C20 C21 110.6 . . ? C20 C21 H21A 108.6 . . ? C20 C21 H21B 108.6 . . ? C20 C21 O7 114.7(9) . . ? H21A C21 H21B 107.6 . . ? H21A C21 O7 108.6 . . ? H21B C21 O7 108.6 . . ? K1 O7 C21 105.4(7) . . ? K1 O7 C22 117.5(6) . . ? C21 O7 C22 117.4(10) . . ? O7 C22 H22A 110.1 . . ? O7 C22 H22B 110.1 . . ? O7 C22 C23 108.2(11) . . ? H22A C22 H22B 108.4 . . ? H22A C22 C23 110.1 . . ? H22B C22 C23 110.1 . . ? C22 C23 H23A 107.1 . . ? C22 C23 H23B 107.1 . . ? C22 C23 O8 120.9(9) . . ? H23A C23 H23B 106.8 . . ? H23A C23 O8 107.1 . . ? H23B C23 O8 107.1 . . ? K1 O8 C23 106.8(8) . . ? K1 O8 C24 120.6(7) . . ? C23 O8 C24 116.7(12) . . ? O8 C24 H24A 110.1 . . ? O8 C24 H24B 110.1 . . ? O8 C24 C25 108.0(12) . . ? H24A C24 H24B 108.4 . . ? H24A C24 C25 110.1 . . ? H24B C24 C25 110.1 . . ? O5 C25 C24 117.8(9) . . ? O5 C25 H25A 107.9 . . ? O5 C25 H25B 107.9 . . ? C24 C25 H25A 107.9 . . ? C24 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 22.56 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.723 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.086 #===END data_ki265_compound_6 _database_code_depnum_ccdc_archive 'CCDC 649165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H50 B N3 Na P Si2' _chemical_formula_sum 'C18 H50 B N3 Na P Si2' _chemical_formula_weight 429.56 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1995(10) _cell_length_b 15.3391(17) _cell_length_c 20.149(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.899(2) _cell_angle_gamma 90.00 _cell_volume 2801.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5940 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.922 _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 24703 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6788 _reflns_number_gt 5163 _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^)+(0.0417P)^2^+1.4288P] 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 6788 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Na1 Na 0.18280(7) 0.33687(4) 0.33233(3) 0.02388(15) Uani 1 1 d . . . P1 P 0.36944(5) 0.16667(3) 0.38192(2) 0.02404(11) Uani 1 1 d . . . Si1 Si 0.40164(6) 0.27718(3) 0.51159(2) 0.02958(12) Uani 1 1 d . . . Si2 Si 0.11338(5) 0.17784(3) 0.45798(2) 0.02543(12) Uani 1 1 d . . . N1 N -0.06662(16) 0.34530(10) 0.25155(7) 0.0303(3) Uani 1 1 d . . . N2 N 0.07023(16) 0.48210(9) 0.35103(7) 0.0279(3) Uani 1 1 d . . . N3 N 0.34348(16) 0.45616(10) 0.29047(8) 0.0298(3) Uani 1 1 d . . . B1 B 0.2863(3) 0.17636(14) 0.28724(10) 0.0332(5) Uani 1 1 d . . . H1C H 0.319(2) 0.2462(14) 0.2739(10) 0.039(6) Uiso 1 1 d . . . H1B H 0.345(2) 0.1272(14) 0.2617(11) 0.046(6) Uiso 1 1 d . . . H1A H 0.168(3) 0.1677(14) 0.2790(11) 0.050(7) Uiso 1 1 d . . . C1 C 0.28449(18) 0.22626(10) 0.43888(8) 0.0212(3) Uani 1 1 d . . . C2 C 0.5606(2) 0.19933(14) 0.38494(12) 0.0432(5) Uani 1 1 d . . . H2A H 0.6130 0.1965 0.4315 0.065 Uiso 1 1 calc R . . H2B H 0.5639 0.2591 0.3681 0.065 Uiso 1 1 calc R . . H2C H 0.6079 0.1599 0.3568 0.065 Uiso 1 1 calc R . . C3 C 0.3975(2) 0.05187(12) 0.40570(10) 0.0396(5) Uani 1 1 d . . . H3A H 0.4396 0.0478 0.4537 0.059 Uiso 1 1 calc R . . H3B H 0.4653 0.0251 0.3791 0.059 Uiso 1 1 calc R . . H3C H 0.3027 0.0212 0.3971 0.059 Uiso 1 1 calc R . . C4 C 0.5297(3) 0.20047(17) 0.56704(11) 0.0560(6) Uani 1 1 d . . . H4A H 0.4728 0.1518 0.5809 0.084 Uiso 1 1 calc R . . H4B H 0.5788 0.2318 0.6071 0.084 Uiso 1 1 calc R . . H4C H 0.6041 0.1780 0.5420 0.084 Uiso 1 1 calc R . . C5 C 0.5224(3) 0.36794(15) 0.48913(12) 0.0506(6) Uani 1 1 d . . . H5A H 0.4619 0.4100 0.4599 0.076 Uiso 1 1 calc R . . H5B H 0.5978 0.3438 0.4654 0.076 Uiso 1 1 calc R . . H5C H 0.5704 0.3972 0.5304 0.076 Uiso 1 1 calc R . . C6 C 0.2929(2) 0.33219(14) 0.57081(10) 0.0432(5) Uani 1 1 d . . . H6A H 0.2228 0.3733 0.5455 0.065 Uiso 1 1 calc R . . H6B H 0.3604 0.3637 0.6056 0.065 Uiso 1 1 calc R . . H6C H 0.2388 0.2882 0.5921 0.065 Uiso 1 1 calc R . . C7 C 0.1440(3) 0.10525(15) 0.53476(10) 0.0475(5) Uani 1 1 d . . . H7A H 0.2172 0.0605 0.5295 0.071 Uiso 1 1 calc R . . H7B H 0.0507 0.0772 0.5397 0.071 Uiso 1 1 calc R . . H7C H 0.1798 0.1404 0.5749 0.071 Uiso 1 1 calc R . . C8 C -0.0274(2) 0.26078(14) 0.47367(11) 0.0427(5) Uani 1 1 d . . . H8A H -0.0477 0.3008 0.4353 0.064 Uiso 1 1 calc R . . H8B H 0.0107 0.2938 0.5146 0.064 Uiso 1 1 calc R . . H8C H -0.1188 0.2310 0.4793 0.064 Uiso 1 1 calc R . . C9 C 0.0097(2) 0.10607(13) 0.39009(10) 0.0367(4) Uani 1 1 d . . . H9A H 0.0754 0.0601 0.3789 0.055 Uiso 1 1 calc R . . H9B H -0.0254 0.1412 0.3499 0.055 Uiso 1 1 calc R . . H9C H -0.0747 0.0796 0.4062 0.055 Uiso 1 1 calc R . . C10 C -0.0485(3) 0.31968(16) 0.18319(10) 0.0482(5) Uani 1 1 d . . . H10A H 0.0243 0.3579 0.1677 0.072 Uiso 1 1 calc R . . H10B H -0.1432 0.3250 0.1527 0.072 Uiso 1 1 calc R . . H10C H -0.0143 0.2591 0.1836 0.072 Uiso 1 1 calc R . . C11 C -0.1757(2) 0.28663(14) 0.27249(11) 0.0435(5) Uani 1 1 d . . . H11A H -0.1906 0.3022 0.3180 0.065 Uiso 1 1 calc R . . H11B H -0.1402 0.2264 0.2723 0.065 Uiso 1 1 calc R . . H11C H -0.2693 0.2920 0.2412 0.065 Uiso 1 1 calc R . . C12 C -0.1161(2) 0.43616(13) 0.25271(10) 0.0343(4) Uani 1 1 d . . . H12A H -0.2230 0.4388 0.2345 0.041 Uiso 1 1 calc R . . H12B H -0.0643 0.4712 0.2227 0.041 Uiso 1 1 calc R . . C13 C -0.0888(2) 0.47623(12) 0.32212(10) 0.0335(4) Uani 1 1 d . . . H13A H -0.1322 0.5354 0.3197 0.040 Uiso 1 1 calc R . . H13B H -0.1392 0.4408 0.3524 0.040 Uiso 1 1 calc R . . C14 C 0.0876(2) 0.49877(14) 0.42359(10) 0.0411(5) Uani 1 1 d . . . H14A H 0.1928 0.5031 0.4426 0.062 Uiso 1 1 calc R . . H14B H 0.0434 0.4508 0.4454 0.062 Uiso 1 1 calc R . . H14C H 0.0382 0.5535 0.4313 0.062 Uiso 1 1 calc R . . C15 C 0.1426(2) 0.55140(12) 0.31868(10) 0.0355(4) Uani 1 1 d . . . H15A H 0.1267 0.6077 0.3403 0.043 Uiso 1 1 calc R . . H15B H 0.0960 0.5553 0.2707 0.043 Uiso 1 1 calc R . . C16 C 0.3069(2) 0.53681(12) 0.32298(10) 0.0351(4) Uani 1 1 d . . . H16A H 0.3492 0.5868 0.3017 0.042 Uiso 1 1 calc R . . H16B H 0.3539 0.5353 0.3710 0.042 Uiso 1 1 calc R . . C17 C 0.2994(2) 0.46126(16) 0.21739(10) 0.0476(5) Uani 1 1 d . . . H17A H 0.1927 0.4712 0.2062 0.071 Uiso 1 1 calc R . . H17B H 0.3241 0.4064 0.1970 0.071 Uiso 1 1 calc R . . H17C H 0.3516 0.5095 0.2000 0.071 Uiso 1 1 calc R . . C18 C 0.5029(2) 0.44259(16) 0.30542(13) 0.0503(6) Uani 1 1 d . . . H18A H 0.5279 0.3885 0.2841 0.075 Uiso 1 1 calc R . . H18B H 0.5348 0.4384 0.3543 0.075 Uiso 1 1 calc R . . H18C H 0.5529 0.4917 0.2879 0.075 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 Na1 0.0239(3) 0.0216(3) 0.0260(3) 0.0023(3) 0.0041(3) 0.0022(3) P1 0.0266(2) 0.0202(2) 0.0254(2) -0.00059(17) 0.00473(17) 0.00306(17) Si1 0.0311(3) 0.0306(3) 0.0236(2) -0.00411(19) -0.00501(19) -0.0005(2) Si2 0.0304(3) 0.0245(2) 0.0221(2) -0.00120(18) 0.00643(18) -0.00435(19) N1 0.0258(7) 0.0356(8) 0.0287(8) 0.0026(6) 0.0023(6) -0.0017(6) N2 0.0311(8) 0.0242(7) 0.0293(8) 0.0021(6) 0.0080(6) 0.0049(6) N3 0.0269(8) 0.0308(8) 0.0332(8) 0.0041(6) 0.0089(6) -0.0020(6) B1 0.0435(13) 0.0323(11) 0.0249(10) -0.0040(8) 0.0090(9) 0.0055(9) C1 0.0253(8) 0.0194(7) 0.0181(7) -0.0009(6) 0.0014(6) 0.0000(6) C2 0.0284(10) 0.0476(12) 0.0559(13) -0.0073(10) 0.0138(9) 0.0007(9) C3 0.0525(13) 0.0243(9) 0.0418(11) 0.0034(8) 0.0079(9) 0.0132(8) C4 0.0533(14) 0.0662(16) 0.0394(12) 0.0022(11) -0.0176(10) 0.0147(12) C5 0.0540(14) 0.0456(12) 0.0507(13) -0.0173(10) 0.0049(11) -0.0201(11) C6 0.0516(13) 0.0468(12) 0.0286(10) -0.0145(9) -0.0005(9) -0.0007(10) C7 0.0678(15) 0.0458(12) 0.0311(11) 0.0085(9) 0.0148(10) -0.0116(11) C8 0.0301(10) 0.0463(12) 0.0535(13) -0.0133(10) 0.0127(9) -0.0022(9) C9 0.0399(11) 0.0346(10) 0.0354(10) -0.0053(8) 0.0060(8) -0.0144(8) C10 0.0465(13) 0.0645(15) 0.0337(11) -0.0080(10) 0.0068(9) -0.0127(11) C11 0.0423(12) 0.0434(12) 0.0440(12) 0.0053(9) 0.0051(9) -0.0096(9) C12 0.0243(9) 0.0401(10) 0.0372(10) 0.0138(8) 0.0014(7) 0.0034(8) C13 0.0280(9) 0.0324(10) 0.0421(11) 0.0086(8) 0.0114(8) 0.0115(7) C14 0.0530(13) 0.0386(11) 0.0333(10) -0.0059(9) 0.0124(9) 0.0018(9) C15 0.0427(11) 0.0219(9) 0.0429(11) 0.0044(8) 0.0100(9) 0.0027(8) C16 0.0373(10) 0.0273(9) 0.0401(11) 0.0008(8) 0.0050(8) -0.0079(8) C17 0.0473(13) 0.0639(15) 0.0337(11) 0.0010(10) 0.0124(9) -0.0045(11) C18 0.0299(11) 0.0586(14) 0.0647(15) 0.0112(12) 0.0148(10) 0.0032(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 Na1 N1 2.5782(16) . ? Na1 N2 2.5122(15) . ? Na1 N3 2.5832(16) . ? Na1 H1C 2.32(2) . ? Na1 C1 2.7700(17) . ? P1 B1 1.935(2) . ? P1 C1 1.7526(16) . ? P1 C2 1.820(2) . ? P1 C3 1.8315(18) . ? Si1 C1 1.8372(16) . ? Si1 C4 1.889(2) . ? Si1 C5 1.884(2) . ? Si1 C6 1.883(2) . ? Si2 C1 1.8401(17) . ? Si2 C7 1.887(2) . ? Si2 C8 1.881(2) . ? Si2 C9 1.8826(19) . ? N1 C10 1.469(2) . ? N1 C11 1.463(2) . ? N1 C12 1.467(2) . ? N2 C13 1.481(2) . ? N2 C14 1.466(2) . ? N2 C15 1.465(2) . ? N3 C16 1.466(2) . ? N3 C17 1.461(2) . ? N3 C18 1.460(2) . ? B1 H1C 1.16(2) . ? B1 H1B 1.10(2) . ? B1 H1A 1.08(2) . ? 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 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 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.509(3) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.516(3) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 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 N1 Na1 N2 72.85(5) . . ? N1 Na1 N3 104.80(5) . . ? N1 Na1 H1C 102.1(5) . . ? N1 Na1 C1 131.71(5) . . ? N2 Na1 N3 72.22(5) . . ? N2 Na1 H1C 151.5(5) . . ? N2 Na1 C1 121.32(5) . . ? N3 Na1 H1C 82.5(5) . . ? N3 Na1 C1 123.43(5) . . ? H1C Na1 C1 83.5(5) . . ? B1 P1 C1 117.41(9) . . ? B1 P1 C2 103.16(10) . . ? B1 P1 C3 110.23(10) . . ? C1 P1 C2 111.82(9) . . ? C1 P1 C3 112.88(9) . . ? C2 P1 C3 99.43(10) . . ? C1 Si1 C4 115.32(9) . . ? C1 Si1 C5 114.33(9) . . ? C1 Si1 C6 113.14(9) . . ? C4 Si1 C5 105.57(12) . . ? C4 Si1 C6 104.46(11) . . ? C5 Si1 C6 102.74(10) . . ? C1 Si2 C7 113.41(9) . . ? C1 Si2 C8 113.63(9) . . ? C1 Si2 C9 115.37(8) . . ? C7 Si2 C8 105.74(11) . . ? C7 Si2 C9 103.66(10) . . ? C8 Si2 C9 103.90(10) . . ? Na1 N1 C10 110.25(12) . . ? Na1 N1 C11 111.54(12) . . ? Na1 N1 C12 106.39(11) . . ? C10 N1 C11 107.46(16) . . ? C10 N1 C12 110.76(16) . . ? C11 N1 C12 110.48(15) . . ? Na1 N2 C13 106.96(10) . . ? Na1 N2 C14 109.10(11) . . ? Na1 N2 C15 110.24(10) . . ? C13 N2 C14 109.51(15) . . ? C13 N2 C15 111.26(14) . . ? C14 N2 C15 109.70(15) . . ? Na1 N3 C16 105.30(10) . . ? Na1 N3 C17 106.95(12) . . ? Na1 N3 C18 116.25(12) . . ? C16 N3 C17 111.11(16) . . ? C16 N3 C18 109.12(16) . . ? C17 N3 C18 108.10(16) . . ? P1 B1 H1C 103.0(10) . . ? P1 B1 H1B 105.5(11) . . ? P1 B1 H1A 111.0(12) . . ? H1C B1 H1B 110.9(15) . . ? H1C B1 H1A 112.0(15) . . ? H1B B1 H1A 113.7(16) . . ? Na1 C1 P1 86.62(6) . . ? Na1 C1 Si1 115.55(7) . . ? Na1 C1 Si2 102.85(7) . . ? P1 C1 Si1 118.52(9) . . ? P1 C1 Si2 114.85(9) . . ? Si1 C1 Si2 114.23(8) . . ? 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 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 108.9 . . ? N1 C12 H12B 108.9 . . ? N1 C12 C13 113.53(15) . . ? H12A C12 H12B 107.7 . . ? H12A C12 C13 108.9 . . ? H12B C12 C13 108.9 . . ? N2 C13 C12 112.64(14) . . ? N2 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C12 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.0 . . ? N2 C15 H15B 109.0 . . ? N2 C15 C16 113.10(15) . . ? H15A C15 H15B 107.8 . . ? H15A C15 C16 109.0 . . ? H15B C15 C16 109.0 . . ? N3 C16 C15 113.71(15) . . ? N3 C16 H16A 108.8 . . ? N3 C16 H16B 108.8 . . ? C15 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.358 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.050 #===END data_ki262_compound_7 _database_code_depnum_ccdc_archive 'CCDC 649166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H100 B2 N6 P2 Rb2 Si4' _chemical_formula_sum 'C36 H100 B2 N6 P2 Rb2 Si4' _chemical_formula_weight 984.08 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' N N 0.0061 0.0033 '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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.233(6) _cell_length_b 9.272(4) _cell_length_c 29.117(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.86(3) _cell_angle_gamma 90.00 _cell_volume 5851(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 364 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.463 _exptl_absorpt_correction_T_max 0.556 _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 '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 44061 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5129 _reflns_number_gt 4294 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _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^)+(0.0758P)^2^+19.0719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5129 _refine_ls_number_parameters 262 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.007 _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 Rb Rb 0.460253(16) 0.19827(4) 0.827354(12) 0.02904(17) Uani 1 1 d . . . P1 P 0.60259(4) 0.43019(10) 0.83626(3) 0.0230(2) Uani 1 1 d . . . Si1 Si 0.60304(5) 0.45495(12) 0.94158(3) 0.0270(3) Uani 1 1 d . . . Si2 Si 0.64107(5) 0.17085(12) 0.89814(4) 0.0287(3) Uani 1 1 d . . . B1 B 0.6043(3) 0.3160(6) 0.78070(16) 0.0367(11) Uani 1 1 d . . . H1A H 0.6040(19) 0.389(5) 0.7535(15) 0.038(11) Uiso 1 1 d . . . H1B H 0.567(2) 0.233(5) 0.7733(17) 0.047(13) Uiso 1 1 d . . . H1C H 0.645(2) 0.248(5) 0.7841(15) 0.037(11) Uiso 1 1 d . . . N1 N 0.3554(2) 0.3346(4) 0.86246(14) 0.0474(10) Uani 1 1 d . . . N2 N 0.40563(15) 0.0476(4) 0.90182(11) 0.0407(9) Uani 1 1 d . . . N3 N 0.38303(19) -0.0749(4) 0.80336(13) 0.0447(9) Uani 1 1 d . . . C1 C 0.59905(15) 0.3440(4) 0.88873(11) 0.0221(7) Uani 1 1 d . . . C2 C 0.66868(19) 0.5554(5) 0.84270(15) 0.0392(10) Uani 1 1 d . . . H2A H 0.6657 0.6292 0.8662 0.059 Uiso 1 1 calc R . . H2B H 0.6681 0.6018 0.8124 0.059 Uiso 1 1 calc R . . H2C H 0.7073 0.5016 0.8530 0.059 Uiso 1 1 calc R . . C3 C 0.53747(18) 0.5550(4) 0.81701(14) 0.0334(9) Uani 1 1 d . . . H3A H 0.5328 0.6155 0.8436 0.050 Uiso 1 1 calc R . . H3B H 0.4995 0.4997 0.8056 0.050 Uiso 1 1 calc R . . H3C H 0.5454 0.6164 0.7916 0.050 Uiso 1 1 calc R . . C4 C 0.6850(2) 0.4937(6) 0.97561(16) 0.0545(13) Uani 1 1 d . . . H4A H 0.7060 0.4026 0.9860 0.082 Uiso 1 1 calc R . . H4B H 0.6837 0.5535 1.0031 0.082 Uiso 1 1 calc R . . H4C H 0.7074 0.5450 0.9552 0.082 Uiso 1 1 calc R . . C5 C 0.5617(2) 0.3697(5) 0.98477(14) 0.0404(10) Uani 1 1 d . . . H5A H 0.5194 0.3456 0.9686 0.061 Uiso 1 1 calc R . . H5B H 0.5608 0.4377 1.0104 0.061 Uiso 1 1 calc R . . H5C H 0.5834 0.2818 0.9977 0.061 Uiso 1 1 calc R . . C6 C 0.5665(2) 0.6407(5) 0.93173(15) 0.0407(10) Uani 1 1 d . . . H6A H 0.5228 0.6310 0.9162 0.061 Uiso 1 1 calc R . . H6B H 0.5877 0.6978 0.9118 0.061 Uiso 1 1 calc R . . H6C H 0.5701 0.6892 0.9621 0.061 Uiso 1 1 calc R . . C7 C 0.7253(2) 0.1845(5) 0.89365(19) 0.0505(13) Uani 1 1 d . . . H7A H 0.7457 0.2618 0.9143 0.076 Uiso 1 1 calc R . . H7B H 0.7272 0.2060 0.8610 0.076 Uiso 1 1 calc R . . H7C H 0.7462 0.0928 0.9033 0.076 Uiso 1 1 calc R . . C8 C 0.6457(2) 0.0903(5) 0.95820(15) 0.0412(10) Uani 1 1 d . . . H8A H 0.6039 0.0723 0.9627 0.062 Uiso 1 1 calc R . . H8B H 0.6670 0.1576 0.9824 0.062 Uiso 1 1 calc R . . H8C H 0.6686 -0.0007 0.9608 0.062 Uiso 1 1 calc R . . C9 C 0.6050(2) 0.0196(5) 0.85731(16) 0.0468(11) Uani 1 1 d . . . H9A H 0.5665 -0.0113 0.8655 0.070 Uiso 1 1 calc R . . H9B H 0.6336 -0.0620 0.8606 0.070 Uiso 1 1 calc R . . H9C H 0.5961 0.0540 0.8247 0.070 Uiso 1 1 calc R . . C10 C 0.3031(3) 0.3845(9) 0.8238(2) 0.086(2) Uani 1 1 d . . . H10A H 0.2792 0.3009 0.8094 0.129 Uiso 1 1 calc R . . H10B H 0.3196 0.4358 0.7998 0.129 Uiso 1 1 calc R . . H10C H 0.2764 0.4494 0.8368 0.129 Uiso 1 1 calc R . . C11 C 0.3893(2) 0.4615(5) 0.88189(19) 0.0518(12) Uani 1 1 d . . . H11A H 0.4278 0.4326 0.9035 0.078 Uiso 1 1 calc R . . H11B H 0.3643 0.5184 0.8991 0.078 Uiso 1 1 calc R . . H11C H 0.3988 0.5198 0.8563 0.078 Uiso 1 1 calc R . . C12 C 0.3293(3) 0.2548(6) 0.8959(2) 0.0676(16) Uani 1 1 d U . . H12A H 0.3124 0.3238 0.9157 0.081 Uiso 1 1 calc R . . H12B H 0.2946 0.1956 0.8784 0.081 Uiso 1 1 calc R . . C13 C 0.3721(3) 0.1640(8) 0.92529(19) 0.0760(19) Uani 1 1 d U . . H13A H 0.3502 0.1140 0.9468 0.091 Uiso 1 1 calc R . . H13B H 0.4039 0.2259 0.9450 0.091 Uiso 1 1 calc R . . C14 C 0.4617(2) 0.0057(5) 0.93521(15) 0.0438(11) Uani 1 1 d . . . H14A H 0.4857 -0.0599 0.9198 0.066 Uiso 1 1 calc R . . H14B H 0.4510 -0.0430 0.9622 0.066 Uiso 1 1 calc R . . H14C H 0.4864 0.0918 0.9461 0.066 Uiso 1 1 calc R . . C15 C 0.3662(3) -0.0706(7) 0.88598(18) 0.0713(18) Uani 1 1 d U . . H15A H 0.3235 -0.0338 0.8757 0.086 Uiso 1 1 calc R . . H15B H 0.3671 -0.1360 0.9130 0.086 Uiso 1 1 calc R . . C16 C 0.3806(4) -0.1537(6) 0.8480(2) 0.0774(19) Uani 1 1 d U . . H16A H 0.3495 -0.2314 0.8400 0.093 Uiso 1 1 calc R . . H16B H 0.4211 -0.2005 0.8599 0.093 Uiso 1 1 calc R . . C17 C 0.3239(3) -0.0340(9) 0.7765(3) 0.114(3) Uani 1 1 d . . . H17A H 0.3280 0.0051 0.7461 0.171 Uiso 1 1 calc R . . H17B H 0.3061 0.0396 0.7937 0.171 Uiso 1 1 calc R . . H17C H 0.2968 -0.1186 0.7713 0.171 Uiso 1 1 calc R . . C18 C 0.4162(3) -0.1649(7) 0.7769(2) 0.0763(19) Uani 1 1 d . . . H18A H 0.3934 -0.2549 0.7682 0.114 Uiso 1 1 calc R . . H18B H 0.4572 -0.1868 0.7963 0.114 Uiso 1 1 calc R . . H18C H 0.4206 -0.1140 0.7484 0.114 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 Rb 0.0289(2) 0.0357(3) 0.0234(2) 0.00431(15) 0.00778(15) -0.00392(15) P1 0.0222(5) 0.0283(5) 0.0181(4) 0.0017(4) 0.0041(3) -0.0015(4) Si1 0.0270(5) 0.0343(6) 0.0182(5) -0.0033(4) 0.0019(4) 0.0011(4) Si2 0.0273(5) 0.0307(6) 0.0303(5) 0.0053(4) 0.0107(4) 0.0078(4) B1 0.050(3) 0.045(3) 0.019(2) -0.002(2) 0.016(2) -0.003(2) N1 0.064(3) 0.035(2) 0.055(2) -0.0070(18) 0.037(2) -0.0056(18) N2 0.0312(18) 0.063(2) 0.0257(16) 0.0174(16) 0.0022(14) -0.0075(17) N3 0.065(3) 0.0302(19) 0.042(2) 0.0004(16) 0.0204(19) 0.0045(18) C1 0.0207(17) 0.0275(19) 0.0180(16) 0.0014(14) 0.0041(14) 0.0007(14) C2 0.032(2) 0.046(3) 0.040(2) 0.005(2) 0.0089(18) -0.0099(19) C3 0.035(2) 0.033(2) 0.0292(19) 0.0061(17) 0.0013(16) 0.0004(17) C4 0.041(3) 0.079(4) 0.037(2) -0.018(2) -0.006(2) -0.005(2) C5 0.050(3) 0.047(3) 0.028(2) 0.0007(19) 0.0165(19) 0.008(2) C6 0.056(3) 0.032(2) 0.036(2) -0.0073(19) 0.014(2) 0.002(2) C7 0.035(2) 0.056(3) 0.066(3) 0.016(2) 0.022(2) 0.017(2) C8 0.037(2) 0.048(3) 0.039(2) 0.016(2) 0.0092(19) 0.014(2) C9 0.068(3) 0.030(2) 0.043(2) -0.002(2) 0.015(2) 0.005(2) C10 0.066(4) 0.133(6) 0.057(3) -0.029(4) 0.008(3) 0.007(4) C11 0.048(3) 0.034(2) 0.071(3) 0.002(2) 0.009(2) -0.003(2) C12 0.094(4) 0.050(3) 0.076(4) -0.004(3) 0.054(3) 0.003(3) C13 0.062(3) 0.136(6) 0.040(3) 0.017(3) 0.031(3) 0.018(4) C14 0.041(2) 0.048(3) 0.036(2) 0.010(2) -0.0032(19) -0.003(2) C15 0.077(4) 0.092(4) 0.040(3) 0.015(3) 0.002(3) -0.047(3) C16 0.127(6) 0.027(3) 0.090(4) 0.005(3) 0.049(4) -0.009(3) C17 0.064(4) 0.090(5) 0.175(8) 0.068(6) -0.002(5) -0.001(4) C18 0.109(5) 0.062(4) 0.064(4) -0.004(3) 0.030(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rb H1B 3.14(5) . ? Rb N1 3.022(4) . ? Rb N2 3.049(3) . ? Rb N3 3.052(4) . ? P1 B1 1.941(5) . ? P1 C1 1.742(3) . ? P1 C2 1.849(4) . ? P1 C3 1.841(4) . ? Si1 C1 1.837(4) . ? Si1 C4 1.905(5) . ? Si1 C5 1.888(4) . ? Si1 C6 1.899(4) . ? Si2 C1 1.846(4) . ? Si2 C7 1.910(5) . ? Si2 C8 1.883(4) . ? Si2 C9 1.897(5) . ? B1 H1A 1.04(4) . ? B1 H1B 1.12(5) . ? B1 H1C 1.09(5) . ? N1 C10 1.501(8) . ? N1 C11 1.443(6) . ? N1 C12 1.443(7) . ? N2 C13 1.554(7) . ? N2 C14 1.454(5) . ? N2 C15 1.415(6) . ? N3 C16 1.504(7) . ? N3 C17 1.423(8) . ? N3 C18 1.444(6) . ? 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 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 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.408(8) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.440(8) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 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 H1B Rb N1 148.4(9) . . ? H1B Rb N2 150.2(9) . . ? H1B Rb N3 114.8(9) . . ? N1 Rb N2 59.47(11) . . ? N1 Rb N3 89.29(11) . . ? N2 Rb N3 59.33(10) . . ? B1 P1 C1 119.6(2) . . ? B1 P1 C2 105.3(2) . . ? B1 P1 C3 104.4(2) . . ? C1 P1 C2 112.91(18) . . ? C1 P1 C3 111.70(18) . . ? C2 P1 C3 100.9(2) . . ? C1 Si1 C4 113.81(19) . . ? C1 Si1 C5 112.57(19) . . ? C1 Si1 C6 116.25(18) . . ? C4 Si1 C5 106.5(2) . . ? C4 Si1 C6 103.6(2) . . ? C5 Si1 C6 103.0(2) . . ? C1 Si2 C7 113.79(19) . . ? C1 Si2 C8 113.81(18) . . ? C1 Si2 C9 114.82(19) . . ? C7 Si2 C8 103.8(2) . . ? C7 Si2 C9 106.9(2) . . ? C8 Si2 C9 102.5(2) . . ? P1 B1 H1A 106(2) . . ? P1 B1 H1B 113(2) . . ? P1 B1 H1C 114(2) . . ? H1A B1 H1B 115(3) . . ? H1A B1 H1C 108(3) . . ? H1B B1 H1C 101(3) . . ? Rb N1 C10 113.7(3) . . ? Rb N1 C11 95.7(3) . . ? Rb N1 C12 118.0(3) . . ? C10 N1 C11 107.0(4) . . ? C10 N1 C12 107.7(5) . . ? C11 N1 C12 114.0(4) . . ? Rb N2 C13 107.5(3) . . ? Rb N2 C14 100.3(2) . . ? Rb N2 C15 116.0(3) . . ? C13 N2 C14 108.4(4) . . ? C13 N2 C15 111.0(4) . . ? C14 N2 C15 112.8(4) . . ? Rb N3 C16 109.4(3) . . ? Rb N3 C17 108.0(4) . . ? Rb N3 C18 105.9(4) . . ? C16 N3 C17 113.4(5) . . ? C16 N3 C18 107.5(4) . . ? C17 N3 C18 112.4(6) . . ? P1 C1 Si1 118.3(2) . . ? P1 C1 Si2 114.15(19) . . ? Si1 C1 Si2 115.73(18) . . ? 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 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 108.9 . . ? N1 C12 H12B 108.9 . . ? N1 C12 C13 113.5(5) . . ? H12A C12 H12B 107.7 . . ? H12A C12 C13 108.9 . . ? H12B C12 C13 108.9 . . ? N2 C13 C12 118.2(4) . . ? N2 C13 H13A 107.8 . . ? N2 C13 H13B 107.8 . . ? C12 C13 H13A 107.8 . . ? C12 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 108.3 . . ? N2 C15 H15B 108.3 . . ? N2 C15 C16 115.9(5) . . ? H15A C15 H15B 107.4 . . ? H15A C15 C16 108.3 . . ? H15B C15 C16 108.3 . . ? N3 C16 C15 117.5(4) . . ? N3 C16 H16A 107.9 . . ? N3 C16 H16B 107.9 . . ? C15 C16 H16A 107.9 . . ? C15 C16 H16B 107.9 . . ? H16A C16 H16B 107.2 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.360 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.105 #===END