Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Keith Izod' _publ_contact_author_address ; Department of Chemistry Bedson Building University of Newcastle Newcastle Upon Tyne NE1 7RU UNITED KINGDOM ; _publ_section_title ; Alkali Metal Complexes of Sterically Demanding Amino-Functionalised Secondary Phosphanide Ligands. ; _publ_contact_author_email K.J.IZOD@NCL.AC.UK loop_ _publ_author_name K.Izod W.Clegg R.W.Harrington J.C.Stewart # Attachment 'ki.cif' data_ki250_compound_7 _database_code_depnum_ccdc_archive 'CCDC 622825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H45 Li N O2 P Si2' _chemical_formula_sum 'C23 H45 Li N O2 P Si2' _chemical_formula_weight 461.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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 11.358(2) _cell_length_b 14.476(3) _cell_length_c 17.519(3) _cell_angle_alpha 86.512(12) _cell_angle_beta 89.130(12) _cell_angle_gamma 82.367(17) _cell_volume 2849.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5196 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.920 _exptl_absorpt_correction_T_max 0.960 _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 62419 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0391 _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 3.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9984 _reflns_number_gt 7887 _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^)+(0.0566P)^2^+3.2475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0152(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9984 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.197 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.54251(7) 0.79269(5) 0.01907(4) 0.0237(2) Uani 1 1 d . A . Si1 Si 0.37376(7) 0.68764(6) -0.07118(5) 0.0256(2) Uani 1 1 d . . . Si2 Si 0.37016(8) 0.68665(6) 0.11239(5) 0.0274(2) Uani 1 1 d . . . O1 O 0.6204(2) 0.92797(17) 0.19892(13) 0.0433(6) Uani 1 1 d . . . O2 O 0.7655(2) 0.73949(16) 0.18360(14) 0.0390(6) Uani 1 1 d . . . N1 N 0.7583(2) 0.89261(18) 0.02799(15) 0.0295(6) Uani 1 1 d . . . Li1 Li 0.6659(5) 0.8355(4) 0.1243(3) 0.0313(12) Uani 1 1 d . A . C1 C 0.4584(2) 0.6878(2) 0.02041(16) 0.0227(6) Uani 1 1 d . . . H1 H 0.5187 0.6307 0.0229 0.027 Uiso 1 1 calc R . . C2 C 0.4686(3) 0.7104(3) -0.15674(19) 0.0418(9) Uani 1 1 d . . . H2A H 0.5221 0.6535 -0.1668 0.063 Uiso 1 1 calc R . . H2B H 0.5154 0.7606 -0.1470 0.063 Uiso 1 1 calc R . . H2C H 0.4178 0.7290 -0.2013 0.063 Uiso 1 1 calc R . . C3 C 0.3196(4) 0.5719(2) -0.0840(2) 0.0462(9) Uani 1 1 d . . . H3A H 0.2913 0.5705 -0.1365 0.069 Uiso 1 1 calc R . . H3B H 0.2544 0.5639 -0.0480 0.069 Uiso 1 1 calc R . . H3C H 0.3849 0.5213 -0.0743 0.069 Uiso 1 1 calc R . . C4 C 0.2415(3) 0.7813(2) -0.0738(2) 0.0359(8) Uani 1 1 d . . . H4A H 0.2680 0.8418 -0.0664 0.054 Uiso 1 1 calc R . . H4B H 0.1855 0.7672 -0.0330 0.054 Uiso 1 1 calc R . . H4C H 0.2023 0.7835 -0.1235 0.054 Uiso 1 1 calc R . . C5 C 0.4688(3) 0.6454(3) 0.19603(19) 0.0460(9) Uani 1 1 d . . . H5A H 0.5303 0.6865 0.1994 0.069 Uiso 1 1 calc R . . H5B H 0.5065 0.5815 0.1892 0.069 Uiso 1 1 calc R . . H5C H 0.4213 0.6467 0.2432 0.069 Uiso 1 1 calc R . . C6 C 0.2559(3) 0.6036(3) 0.1112(2) 0.0438(9) Uani 1 1 d . . . H6A H 0.2168 0.6001 0.1613 0.066 Uiso 1 1 calc R . . H6B H 0.2949 0.5414 0.0996 0.066 Uiso 1 1 calc R . . H6C H 0.1965 0.6259 0.0719 0.066 Uiso 1 1 calc R . . C7 C 0.2883(3) 0.8047(2) 0.1317(2) 0.0392(8) Uani 1 1 d . . . H7A H 0.2488 0.8015 0.1817 0.059 Uiso 1 1 calc R . . H7B H 0.2287 0.8236 0.0919 0.059 Uiso 1 1 calc R . . H7C H 0.3447 0.8504 0.1315 0.059 Uiso 1 1 calc R . . C8 C 0.6904(3) 0.7497(2) -0.01679(16) 0.0240(6) Uani 1 1 d . . . C9 C 0.7233(3) 0.6631(2) -0.04907(17) 0.0284(7) Uani 1 1 d . A . H9 H 0.6638 0.6237 -0.0545 0.034 Uiso 1 1 calc R . . C10 C 0.8390(3) 0.6321(2) -0.0735(2) 0.0357(8) Uani 1 1 d . . . H10 H 0.8568 0.5727 -0.0943 0.043 Uiso 1 1 calc R A . C11 C 0.9274(3) 0.6884(2) -0.0672(2) 0.0386(8) Uani 1 1 d . A . H11 H 1.0058 0.6683 -0.0844 0.046 Uiso 1 1 calc R . . C12 C 0.9002(3) 0.7750(2) -0.03538(19) 0.0351(8) Uani 1 1 d . . . H12 H 0.9607 0.8137 -0.0310 0.042 Uiso 1 1 calc R A . C13 C 0.7859(3) 0.8049(2) -0.01013(17) 0.0273(7) Uani 1 1 d . A . C14 C 0.8612(3) 0.9294(3) 0.0590(2) 0.0448(9) Uani 1 1 d . A . H14A H 0.9110 0.8790 0.0878 0.067 Uiso 1 1 calc R . . H14B H 0.8336 0.9793 0.0929 0.067 Uiso 1 1 calc R . . H14C H 0.9077 0.9543 0.0168 0.067 Uiso 1 1 calc R . . C15 C 0.6906(3) 0.9664(2) -0.0232(2) 0.0381(8) Uani 1 1 d . A . H15A H 0.7433 0.9871 -0.0637 0.057 Uiso 1 1 calc R . . H15B H 0.6594 1.0195 0.0066 0.057 Uiso 1 1 calc R . . H15C H 0.6245 0.9411 -0.0462 0.057 Uiso 1 1 calc R . . C16 C 0.5713(5) 1.0223(3) 0.1823(3) 0.0682(14) Uani 0.38(4) 1 d P A 1 H16A H 0.6321 1.0641 0.1893 0.082 Uiso 0.38(4) 1 calc PR A 1 H16B H 0.5442 1.0309 0.1286 0.082 Uiso 0.38(4) 1 calc PR A 1 C16A C 0.5713(5) 1.0223(3) 0.1823(3) 0.0682(14) Uani 0.62(4) 1 d P A 2 H16C H 0.5433 1.0320 0.1288 0.082 Uiso 0.62(4) 1 calc PR A 2 H16D H 0.6304 1.0651 0.1905 0.082 Uiso 0.62(4) 1 calc PR A 2 C17 C 0.482(2) 1.0425(14) 0.2288(17) 0.051(6) Uani 0.38(4) 1 d P A 1 H17A H 0.4081 1.0247 0.2076 0.061 Uiso 0.38(4) 1 calc PR A 1 H17B H 0.4690 1.1104 0.2364 0.061 Uiso 0.38(4) 1 calc PR A 1 C17A C 0.458(2) 1.0391(15) 0.2436(14) 0.090(6) Uani 0.62(4) 1 d P A 2 H17C H 0.4581 1.0984 0.2689 0.108 Uiso 0.62(4) 1 calc PR A 2 H17D H 0.3814 1.0394 0.2178 0.108 Uiso 0.62(4) 1 calc PR A 2 C18 C 0.514(2) 0.9857(15) 0.3068(13) 0.047(5) Uani 0.38(4) 1 d P A 1 H18A H 0.5437 1.0242 0.3451 0.056 Uiso 0.38(4) 1 calc PR A 1 H18B H 0.4464 0.9555 0.3286 0.056 Uiso 0.38(4) 1 calc PR A 1 C18A C 0.481(3) 0.9650(19) 0.2938(16) 0.149(11) Uani 0.62(4) 1 d P A 2 H18C H 0.4068 0.9362 0.3015 0.179 Uiso 0.62(4) 1 calc PR A 2 H18D H 0.5010 0.9877 0.3435 0.179 Uiso 0.62(4) 1 calc PR A 2 C19 C 0.610(5) 0.917(3) 0.2750(17) 0.102(14) Uani 0.38(4) 1 d P A 1 H19A H 0.6871 0.9238 0.2986 0.122 Uiso 0.38(4) 1 calc PR A 1 H19B H 0.5930 0.8524 0.2888 0.122 Uiso 0.38(4) 1 calc PR A 1 C19A C 0.573(2) 0.8948(12) 0.2734(11) 0.081(6) Uani 0.62(4) 1 d P A 2 H19C H 0.5413 0.8348 0.2687 0.098 Uiso 0.62(4) 1 calc PR A 2 H19D H 0.6358 0.8856 0.3126 0.098 Uiso 0.62(4) 1 calc PR A 2 C20 C 0.8616(3) 0.7555(3) 0.2319(2) 0.0473(10) Uani 1 1 d . A . H20A H 0.8436 0.7397 0.2862 0.057 Uiso 1 1 calc R . . H20B H 0.8755 0.8216 0.2263 0.057 Uiso 1 1 calc R . . C21 C 0.9695(4) 0.6917(4) 0.2047(3) 0.0737(14) Uani 1 1 d . . . H21A H 1.0217 0.7274 0.1721 0.088 Uiso 1 1 calc R A . H21B H 1.0159 0.6608 0.2487 0.088 Uiso 1 1 calc R . . C22 C 0.9186(4) 0.6203(3) 0.1592(3) 0.0654(12) Uani 1 1 d . A . H22A H 0.9434 0.6257 0.1049 0.079 Uiso 1 1 calc R . . H22B H 0.9458 0.5561 0.1803 0.079 Uiso 1 1 calc R . . C23 C 0.7865(4) 0.6424(3) 0.1668(2) 0.0490(10) Uani 1 1 d . A . H23A H 0.7470 0.6321 0.1186 0.059 Uiso 1 1 calc R . . H23B H 0.7560 0.6028 0.2087 0.059 Uiso 1 1 calc R . . P2 P 0.04855(6) 0.78674(5) 0.52177(4) 0.02160(19) Uani 1 1 d . B . Si3 Si 0.24500(8) 0.69713(6) 0.62945(5) 0.0302(2) Uani 1 1 d . . . Si4 Si 0.28463(7) 0.70352(6) 0.44733(5) 0.0274(2) Uani 1 1 d . . . O3 O -0.1883(2) 0.70301(15) 0.65570(13) 0.0351(5) Uani 1 1 d . . . O4 O -0.1368(2) 0.90307(16) 0.69114(12) 0.0385(6) Uani 1 1 d . . . N2 N -0.2105(2) 0.86052(17) 0.50812(14) 0.0264(6) Uani 1 1 d . . . Li2 Li -0.1218(4) 0.8116(3) 0.6140(3) 0.0271(11) Uani 1 1 d . B . C24 C 0.1815(2) 0.6928(2) 0.53140(16) 0.0220(6) Uani 1 1 d . . . H24 H 0.1510 0.6312 0.5295 0.026 Uiso 1 1 calc R . . C25 C 0.1449(4) 0.6510(3) 0.7052(2) 0.0482(10) Uani 1 1 d . . . H25A H 0.0640 0.6834 0.6986 0.072 Uiso 1 1 calc R . . H25B H 0.1740 0.6617 0.7559 0.072 Uiso 1 1 calc R . . H25C H 0.1447 0.5839 0.7006 0.072 Uiso 1 1 calc R . . C26 C 0.3928(3) 0.6216(3) 0.6399(2) 0.0500(10) Uani 1 1 d . . . H26A H 0.3857 0.5590 0.6237 0.075 Uiso 1 1 calc R . . H26B H 0.4175 0.6174 0.6935 0.075 Uiso 1 1 calc R . . H26C H 0.4522 0.6491 0.6078 0.075 Uiso 1 1 calc R . . C27 C 0.2649(4) 0.8194(2) 0.6516(2) 0.0444(9) Uani 1 1 d . . . H27A H 0.3317 0.8391 0.6216 0.067 Uiso 1 1 calc R . . H27B H 0.2813 0.8212 0.7062 0.067 Uiso 1 1 calc R . . H27C H 0.1923 0.8616 0.6386 0.067 Uiso 1 1 calc R . . C28 C 0.3912(3) 0.5931(3) 0.4372(2) 0.0493(10) Uani 1 1 d . . . H28A H 0.4503 0.5867 0.4780 0.074 Uiso 1 1 calc R . . H28B H 0.4314 0.5960 0.3874 0.074 Uiso 1 1 calc R . . H28C H 0.3472 0.5391 0.4409 0.074 Uiso 1 1 calc R . . C29 C 0.3740(3) 0.8029(3) 0.4584(2) 0.0480(10) Uani 1 1 d . . . H29A H 0.3200 0.8604 0.4656 0.072 Uiso 1 1 calc R . . H29B H 0.4226 0.8111 0.4124 0.072 Uiso 1 1 calc R . . H29C H 0.4258 0.7887 0.5030 0.072 Uiso 1 1 calc R . . C30 C 0.2047(3) 0.7295(3) 0.35403(18) 0.0373(8) Uani 1 1 d . . . H30A H 0.1806 0.6719 0.3364 0.056 Uiso 1 1 calc R . . H30B H 0.2575 0.7551 0.3159 0.056 Uiso 1 1 calc R . . H30C H 0.1341 0.7752 0.3610 0.056 Uiso 1 1 calc R . . C31 C -0.0615(2) 0.7294(2) 0.47393(16) 0.0219(6) Uani 1 1 d . . . C32 C -0.0395(3) 0.6413(2) 0.44178(17) 0.0280(7) Uani 1 1 d . B . H32 H 0.0402 0.6115 0.4395 0.034 Uiso 1 1 calc R . . C33 C -0.1281(3) 0.5966(2) 0.41359(19) 0.0343(8) Uani 1 1 d . . . H33 H -0.1088 0.5367 0.3938 0.041 Uiso 1 1 calc R B . C34 C -0.2458(3) 0.6385(3) 0.4140(2) 0.0394(8) Uani 1 1 d . B . H34 H -0.3072 0.6079 0.3950 0.047 Uiso 1 1 calc R . . C35 C -0.2713(3) 0.7266(2) 0.44295(18) 0.0320(7) Uani 1 1 d . . . H35 H -0.3509 0.7567 0.4425 0.038 Uiso 1 1 calc R B . C36 C -0.1824(3) 0.7714(2) 0.47251(16) 0.0241(6) Uani 1 1 d . B . C37 C -0.1704(3) 0.9388(2) 0.46037(19) 0.0348(8) Uani 1 1 d . B . H37A H -0.0880 0.9213 0.4440 0.052 Uiso 1 1 calc R . . H37B H -0.1755 0.9942 0.4903 0.052 Uiso 1 1 calc R . . H37C H -0.2213 0.9525 0.4153 0.052 Uiso 1 1 calc R . . C38 C -0.3361(3) 0.8851(3) 0.5306(2) 0.0397(8) Uani 1 1 d . B . H38A H -0.3849 0.8994 0.4847 0.060 Uiso 1 1 calc R . . H38B H -0.3437 0.9399 0.5615 0.060 Uiso 1 1 calc R . . H38C H -0.3631 0.8325 0.5607 0.060 Uiso 1 1 calc R . . C39 C -0.1476(3) 0.6115(2) 0.6288(2) 0.0380(8) Uani 1 1 d . . . H39A H -0.0627 0.6061 0.6140 0.046 Uiso 1 1 calc R . . H39B H -0.1945 0.5990 0.5843 0.046 Uiso 1 1 calc R . . C40 C -0.1667(3) 0.5450(2) 0.6963(2) 0.0415(9) Uani 1 1 d . . . H40A H -0.1014 0.5410 0.7336 0.050 Uiso 1 1 calc R . . H40B H -0.1735 0.4817 0.6798 0.050 Uiso 1 1 calc R . . C41 C -0.2832(3) 0.5900(2) 0.7295(2) 0.0406(8) Uani 1 1 d . . . H41A H -0.3517 0.5691 0.7044 0.049 Uiso 1 1 calc R . . H41B H -0.2878 0.5746 0.7852 0.049 Uiso 1 1 calc R . . C42 C -0.2809(4) 0.6938(3) 0.7130(2) 0.0469(10) Uani 1 1 d . . . H42A H -0.3588 0.7240 0.6934 0.056 Uiso 1 1 calc R . . H42B H -0.2630 0.7235 0.7602 0.056 Uiso 1 1 calc R . . C43 C -0.1072(4) 0.8807(3) 0.7708(2) 0.0521(10) Uani 0.52(3) 1 d P B 1 H43A H -0.0759 0.8137 0.7791 0.063 Uiso 0.52(3) 1 calc PR B 1 H43B H -0.1783 0.8944 0.8036 0.063 Uiso 0.52(3) 1 calc PR B 1 C43A C -0.1072(4) 0.8807(3) 0.7708(2) 0.0521(10) Uani 0.48(3) 1 d P B 2 H43C H -0.0444 0.8264 0.7762 0.063 Uiso 0.48(3) 1 calc PR B 2 H43D H -0.1779 0.8661 0.8005 0.063 Uiso 0.48(3) 1 calc PR B 2 C44 C -0.0174(16) 0.9385(14) 0.7886(11) 0.065(4) Uani 0.52(3) 1 d P B 1 H44A H 0.0637 0.9053 0.7821 0.078 Uiso 0.52(3) 1 calc PR B 1 H44B H -0.0271 0.9594 0.8414 0.078 Uiso 0.52(3) 1 calc PR B 1 C44A C -0.0626(19) 0.9694(13) 0.7985(9) 0.053(4) Uani 0.48(3) 1 d P B 2 H44C H -0.1285 1.0087 0.8233 0.064 Uiso 0.48(3) 1 calc PR B 2 H44D H 0.0015 0.9516 0.8363 0.064 Uiso 0.48(3) 1 calc PR B 2 C45 C -0.043(2) 1.0190(15) 0.7303(14) 0.074(8) Uani 0.52(3) 1 d P B 1 H45A H -0.0884 1.0727 0.7548 0.089 Uiso 0.52(3) 1 calc PR B 1 H45B H 0.0326 1.0384 0.7107 0.089 Uiso 0.52(3) 1 calc PR B 1 C45A C -0.016(2) 1.024(2) 0.7294(11) 0.056(5) Uani 0.48(3) 1 d P B 2 H45C H 0.0677 1.0006 0.7167 0.067 Uiso 0.48(3) 1 calc PR B 2 H45D H -0.0253 1.0917 0.7355 0.067 Uiso 0.48(3) 1 calc PR B 2 C46 C -0.1086(5) 0.9945(3) 0.6692(3) 0.0688(14) Uani 0.52(3) 1 d P B 1 H46A H -0.0608 0.9937 0.6214 0.083 Uiso 0.52(3) 1 calc PR B 1 H46B H -0.1818 1.0391 0.6611 0.083 Uiso 0.52(3) 1 calc PR B 1 C46A C -0.1086(5) 0.9945(3) 0.6692(3) 0.0688(14) Uani 0.48(3) 1 d P B 2 H46C H -0.1819 1.0399 0.6683 0.083 Uiso 0.48(3) 1 calc PR B 2 H46D H -0.0731 0.9950 0.6172 0.083 Uiso 0.48(3) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0214(4) 0.0226(4) 0.0275(4) -0.0037(3) 0.0015(3) -0.0037(3) Si1 0.0245(4) 0.0234(4) 0.0288(5) -0.0035(3) -0.0037(3) -0.0021(3) Si2 0.0281(5) 0.0249(5) 0.0280(5) 0.0014(3) 0.0066(3) -0.0013(4) O1 0.0616(17) 0.0358(14) 0.0305(13) -0.0068(10) 0.0010(11) 0.0023(12) O2 0.0338(13) 0.0341(13) 0.0487(15) -0.0047(11) -0.0164(11) -0.0001(10) N1 0.0285(14) 0.0253(14) 0.0362(15) -0.0036(11) -0.0012(11) -0.0081(11) Li1 0.028(3) 0.032(3) 0.033(3) -0.003(2) -0.003(2) 0.000(2) C1 0.0190(15) 0.0224(15) 0.0264(15) -0.0018(12) 0.0009(12) -0.0024(12) C2 0.042(2) 0.054(2) 0.0283(18) -0.0062(16) -0.0017(15) 0.0004(17) C3 0.061(3) 0.032(2) 0.048(2) -0.0065(16) -0.0172(19) -0.0103(18) C4 0.0258(17) 0.0364(19) 0.045(2) -0.0015(15) -0.0082(15) -0.0016(14) C5 0.051(2) 0.054(2) 0.0293(19) 0.0069(17) 0.0053(16) 0.0005(19) C6 0.042(2) 0.035(2) 0.054(2) 0.0048(17) 0.0162(17) -0.0097(16) C7 0.045(2) 0.0330(19) 0.0365(19) -0.0015(15) 0.0137(16) 0.0022(16) C8 0.0227(15) 0.0257(16) 0.0231(15) -0.0007(12) -0.0004(12) -0.0016(12) C9 0.0231(16) 0.0302(17) 0.0329(17) -0.0065(13) 0.0028(13) -0.0056(13) C10 0.0310(18) 0.0315(18) 0.044(2) -0.0093(15) 0.0058(15) -0.0002(14) C11 0.0203(17) 0.043(2) 0.052(2) -0.0042(17) 0.0085(15) -0.0029(15) C12 0.0237(17) 0.0379(19) 0.045(2) -0.0013(15) 0.0033(14) -0.0103(14) C13 0.0244(16) 0.0291(17) 0.0284(16) 0.0023(13) 0.0001(13) -0.0060(13) C14 0.039(2) 0.042(2) 0.057(2) -0.0114(18) 0.0018(17) -0.0163(17) C15 0.044(2) 0.0270(18) 0.043(2) 0.0039(15) 0.0036(16) -0.0055(15) C16 0.084(4) 0.049(3) 0.062(3) 0.008(2) 0.022(3) 0.018(2) C16A 0.084(4) 0.049(3) 0.062(3) 0.008(2) 0.022(3) 0.018(2) C17 0.046(11) 0.040(9) 0.053(12) 0.028(7) 0.041(9) 0.025(6) C17A 0.063(9) 0.121(12) 0.076(11) -0.010(9) 0.054(8) 0.020(7) C18 0.061(9) 0.034(9) 0.043(9) -0.009(7) 0.004(8) 0.004(6) C18A 0.23(2) 0.073(12) 0.129(18) 0.038(11) 0.129(16) 0.022(13) C19 0.18(3) 0.070(18) 0.034(10) 0.011(11) -0.007(14) 0.07(2) C19A 0.163(14) 0.049(6) 0.032(6) -0.007(4) 0.044(8) -0.013(8) C20 0.049(2) 0.057(2) 0.038(2) -0.0044(18) -0.0138(17) -0.0121(19) C21 0.041(3) 0.095(4) 0.085(3) -0.019(3) -0.018(2) 0.000(2) C22 0.051(3) 0.058(3) 0.084(3) -0.011(2) -0.007(2) 0.011(2) C23 0.050(2) 0.037(2) 0.059(2) -0.0003(18) -0.0156(19) -0.0010(18) P2 0.0181(4) 0.0214(4) 0.0253(4) -0.0032(3) -0.0015(3) -0.0013(3) Si3 0.0321(5) 0.0287(5) 0.0288(5) -0.0050(4) -0.0110(4) 0.0022(4) Si4 0.0193(4) 0.0294(5) 0.0316(5) -0.0001(4) 0.0016(3) 0.0024(3) O3 0.0406(14) 0.0267(12) 0.0374(13) -0.0003(10) 0.0157(10) -0.0044(10) O4 0.0542(16) 0.0334(13) 0.0294(12) -0.0070(10) 0.0004(11) -0.0092(11) N2 0.0209(13) 0.0256(14) 0.0314(14) -0.0019(11) -0.0004(10) 0.0025(10) Li2 0.028(3) 0.023(3) 0.030(3) -0.001(2) 0.000(2) -0.002(2) C24 0.0201(15) 0.0194(15) 0.0265(15) -0.0026(12) -0.0031(12) -0.0024(12) C25 0.063(3) 0.053(2) 0.0275(19) 0.0010(16) -0.0073(17) -0.005(2) C26 0.047(2) 0.054(2) 0.046(2) -0.0136(18) -0.0261(18) 0.0142(19) C27 0.052(2) 0.037(2) 0.045(2) -0.0119(16) -0.0157(18) -0.0013(17) C28 0.043(2) 0.055(2) 0.042(2) -0.0043(18) 0.0035(17) 0.0225(18) C29 0.030(2) 0.054(2) 0.061(3) 0.0020(19) 0.0064(17) -0.0135(17) C30 0.0374(19) 0.041(2) 0.0307(18) 0.0019(15) 0.0053(14) 0.0031(16) C31 0.0205(15) 0.0255(16) 0.0199(14) 0.0018(12) -0.0007(11) -0.0049(12) C32 0.0256(16) 0.0301(17) 0.0281(16) -0.0049(13) 0.0008(13) -0.0017(13) C33 0.039(2) 0.0288(18) 0.0374(19) -0.0107(14) -0.0021(15) -0.0080(15) C34 0.0324(19) 0.043(2) 0.046(2) -0.0111(16) -0.0075(15) -0.0138(16) C35 0.0216(16) 0.0397(19) 0.0346(18) -0.0024(15) -0.0028(13) -0.0033(14) C36 0.0249(16) 0.0266(16) 0.0207(15) 0.0002(12) -0.0020(12) -0.0030(13) C37 0.0343(19) 0.0280(18) 0.0397(19) 0.0049(14) -0.0032(15) 0.0025(14) C38 0.0258(18) 0.043(2) 0.048(2) -0.0097(17) 0.0040(15) 0.0059(15) C39 0.046(2) 0.0302(18) 0.0364(19) -0.0029(15) 0.0077(16) -0.0011(16) C40 0.047(2) 0.0297(19) 0.046(2) 0.0040(16) 0.0062(17) 0.0000(16) C41 0.041(2) 0.034(2) 0.045(2) 0.0065(16) 0.0070(16) -0.0052(16) C42 0.051(2) 0.036(2) 0.054(2) -0.0026(17) 0.0278(19) -0.0087(17) C43 0.074(3) 0.054(3) 0.030(2) -0.0074(17) -0.0047(19) -0.013(2) C43A 0.074(3) 0.054(3) 0.030(2) -0.0074(17) -0.0047(19) -0.013(2) C44 0.061(9) 0.081(12) 0.053(8) -0.010(7) -0.016(7) -0.010(7) C44A 0.065(11) 0.057(9) 0.044(6) -0.024(6) 0.005(7) -0.026(7) C45 0.070(15) 0.033(7) 0.125(16) -0.002(7) -0.042(10) -0.025(7) C45A 0.041(8) 0.088(13) 0.049(8) -0.022(7) 0.001(6) -0.038(7) C46 0.101(4) 0.040(2) 0.071(3) 0.003(2) -0.030(3) -0.029(2) C46A 0.101(4) 0.040(2) 0.071(3) 0.003(2) -0.030(3) -0.029(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 P1 Li1 2.489(5) . ? P1 C1 1.897(3) . ? P1 C8 1.828(3) . ? Si1 C1 1.883(3) . ? Si1 C2 1.871(4) . ? Si1 C3 1.887(4) . ? Si1 C4 1.884(3) . ? Si2 C1 1.885(3) . ? Si2 C5 1.878(4) . ? Si2 C6 1.884(4) . ? Si2 C7 1.880(3) . ? O1 Li1 1.942(6) . ? O1 C16 1.419(5) . ? O1 C19 1.34(3) . ? O1 C19A 1.483(17) . ? O2 Li1 1.933(6) . ? O2 C20 1.441(4) . ? O2 C23 1.442(4) . ? N1 Li1 2.154(6) . ? N1 C13 1.465(4) . ? N1 C14 1.471(4) . ? N1 C15 1.491(4) . ? Li1 C13 2.733(6) . ? C1 H1 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.409(4) . ? C8 C13 1.441(4) . ? C9 H9 0.950 . ? C9 C10 1.401(4) . ? C10 H10 0.950 . ? C10 C11 1.383(5) . ? C11 H11 0.950 . ? C11 C12 1.399(5) . ? C12 H12 0.950 . ? C12 C13 1.387(4) . ? 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 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.31(3) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.57(3) . ? C17A H17C 0.990 . ? C17A H17D 0.990 . ? C17A C18A 1.35(3) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.51(4) . ? C18A H18C 0.990 . ? C18A H18D 0.990 . ? C18A C19A 1.42(3) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19A H19C 0.990 . ? C19A H19D 0.990 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.522(6) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.520(6) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.497(6) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? P2 Li2 2.505(5) . ? P2 C24 1.896(3) . ? P2 C31 1.830(3) . ? Si3 C24 1.881(3) . ? Si3 C25 1.883(4) . ? Si3 C26 1.883(4) . ? Si3 C27 1.878(4) . ? Si4 C24 1.880(3) . ? Si4 C28 1.889(4) . ? Si4 C29 1.888(4) . ? Si4 C30 1.876(3) . ? O3 Li2 1.933(5) . ? O3 C39 1.448(4) . ? O3 C42 1.457(4) . ? O4 Li2 1.939(5) . ? O4 C43 1.447(4) . ? O4 C46 1.431(5) . ? N2 Li2 2.159(6) . ? N2 C36 1.463(4) . ? N2 C37 1.483(4) . ? N2 C38 1.478(4) . ? Li2 C36 2.700(6) . ? C24 H24 1.000 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C27 H27A 0.980 . ? C27 H27B 0.980 . ? C27 H27C 0.980 . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.980 . ? C29 H29B 0.980 . ? C29 H29C 0.980 . ? C30 H30A 0.980 . ? C30 H30B 0.980 . ? C30 H30C 0.980 . ? C31 C32 1.416(4) . ? C31 C36 1.426(4) . ? C32 H32 0.950 . ? C32 C33 1.380(4) . ? C33 H33 0.950 . ? C33 C34 1.392(5) . ? C34 H34 0.950 . ? C34 C35 1.394(5) . ? C35 H35 0.950 . ? C35 C36 1.391(4) . ? C37 H37A 0.980 . ? C37 H37B 0.980 . ? C37 H37C 0.980 . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C39 C40 1.511(5) . ? C40 H40A 0.990 . ? C40 H40B 0.990 . ? C40 C41 1.519(5) . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C41 C42 1.516(5) . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C43 H43A 0.990 . ? C43 H43B 0.990 . ? C43 C44 1.452(17) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C44 C45 1.50(3) . ? C44A H44C 0.990 . ? C44A H44D 0.990 . ? C44A C45A 1.53(3) . ? C45 H45A 0.990 . ? C45 H45B 0.990 . ? C45 C46 1.40(3) . ? C45A H45C 0.990 . ? C45A H45D 0.990 . ? C46 H46A 0.990 . ? C46 H46B 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 Li1 P1 C1 126.28(16) . . ? Li1 P1 C8 80.25(16) . . ? C1 P1 C8 104.46(13) . . ? C1 Si1 C2 111.49(15) . . ? C1 Si1 C3 112.39(15) . . ? C1 Si1 C4 110.58(14) . . ? C2 Si1 C3 106.21(18) . . ? C2 Si1 C4 107.56(17) . . ? C3 Si1 C4 108.38(17) . . ? C1 Si2 C5 111.03(15) . . ? C1 Si2 C6 111.47(15) . . ? C1 Si2 C7 112.59(14) . . ? C5 Si2 C6 106.09(18) . . ? C5 Si2 C7 108.38(17) . . ? C6 Si2 C7 106.98(17) . . ? Li1 O1 C16 125.9(3) . . ? Li1 O1 C19 129.5(15) . . ? Li1 O1 C19A 117.4(7) . . ? C16 O1 C19 103.9(13) . . ? C16 O1 C19A 109.1(8) . . ? C19 O1 C19A 22(3) . . ? Li1 O2 C20 125.0(3) . . ? Li1 O2 C23 125.0(3) . . ? C20 O2 C23 106.5(3) . . ? Li1 N1 C13 96.2(2) . . ? Li1 N1 C14 106.6(3) . . ? Li1 N1 C15 117.9(2) . . ? C13 N1 C14 115.2(3) . . ? C13 N1 C15 111.3(2) . . ? C14 N1 C15 109.2(3) . . ? P1 Li1 O1 127.4(3) . . ? P1 Li1 O2 120.1(3) . . ? P1 Li1 N1 80.70(18) . . ? P1 Li1 C13 65.43(14) . . ? O1 Li1 O2 102.3(3) . . ? O1 Li1 N1 111.7(3) . . ? O1 Li1 C13 143.8(3) . . ? O2 Li1 N1 112.6(3) . . ? O2 Li1 C13 94.9(2) . . ? N1 Li1 C13 32.19(12) . . ? P1 C1 Si1 110.48(15) . . ? P1 C1 Si2 107.11(14) . . ? P1 C1 H1 107.2 . . ? Si1 C1 Si2 117.11(15) . . ? Si1 C1 H1 107.2 . . ? Si2 C1 H1 107.2 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 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 . . ? P1 C8 C9 125.8(2) . . ? P1 C8 C13 119.5(2) . . ? C9 C8 C13 114.7(3) . . ? C8 C9 H9 118.2 . . ? C8 C9 C10 123.5(3) . . ? H9 C9 C10 118.2 . . ? C9 C10 H10 120.2 . . ? C9 C10 C11 119.7(3) . . ? H10 C10 C11 120.2 . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.4(3) . . ? H11 C11 C12 120.3 . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.8(3) . . ? H12 C12 C13 119.6 . . ? N1 C13 Li1 51.56(18) . . ? N1 C13 C8 116.9(3) . . ? N1 C13 C12 121.2(3) . . ? Li1 C13 C8 78.6(2) . . ? Li1 C13 C12 139.1(3) . . ? C8 C13 C12 121.9(3) . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 H16A 110.0 . . ? O1 C16 H16B 110.0 . . ? O1 C16 C17 108.4(9) . . ? H16A C16 H16B 108.4 . . ? H16A C16 C17 110.0 . . ? H16B C16 C17 110.0 . . ? C16 C17 H17A 110.4 . . ? C16 C17 H17B 110.4 . . ? C16 C17 C18 106.8(17) . . ? H17A C17 H17B 108.6 . . ? H17A C17 C18 110.4 . . ? H17B C17 C18 110.4 . . ? H17C C17A H17D 109.2 . . ? H17C C17A C18A 111.3 . . ? H17D C17A C18A 111.3 . . ? C17 C18 H18A 112.5 . . ? C17 C18 H18B 112.5 . . ? C17 C18 C19 96.2(19) . . ? H18A C18 H18B 110.0 . . ? H18A C18 C19 112.5 . . ? H18B C18 C19 112.5 . . ? C17A C18A H18C 108.3 . . ? C17A C18A H18D 108.3 . . ? C17A C18A C19A 116.1(18) . . ? H18C C18A H18D 107.4 . . ? H18C C18A C19A 108.3 . . ? H18D C18A C19A 108.3 . . ? O1 C19 C18 112.2(18) . . ? O1 C19 H19A 109.2 . . ? O1 C19 H19B 109.2 . . ? C18 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O1 C19A C18A 106.2(14) . . ? O1 C19A H19C 110.5 . . ? O1 C19A H19D 110.5 . . ? C18A C19A H19C 110.5 . . ? C18A C19A H19D 110.5 . . ? H19C C19A H19D 108.7 . . ? O2 C20 H20A 110.7 . . ? O2 C20 H20B 110.7 . . ? O2 C20 C21 105.3(3) . . ? H20A C20 H20B 108.8 . . ? H20A C20 C21 110.7 . . ? H20B C20 C21 110.7 . . ? C20 C21 H21A 110.8 . . ? C20 C21 H21B 110.8 . . ? C20 C21 C22 104.8(3) . . ? H21A C21 H21B 108.9 . . ? H21A C21 C22 110.8 . . ? H21B C21 C22 110.8 . . ? C21 C22 H22A 110.7 . . ? C21 C22 H22B 110.7 . . ? C21 C22 C23 105.5(4) . . ? H22A C22 H22B 108.8 . . ? H22A C22 C23 110.7 . . ? H22B C22 C23 110.7 . . ? O2 C23 C22 105.2(3) . . ? O2 C23 H23A 110.7 . . ? O2 C23 H23B 110.7 . . ? C22 C23 H23A 110.7 . . ? C22 C23 H23B 110.7 . . ? H23A C23 H23B 108.8 . . ? Li2 P2 C24 126.37(15) . . ? Li2 P2 C31 79.76(15) . . ? C24 P2 C31 103.37(13) . . ? C24 Si3 C25 110.93(15) . . ? C24 Si3 C26 111.46(15) . . ? C24 Si3 C27 111.78(15) . . ? C25 Si3 C26 106.14(19) . . ? C25 Si3 C27 107.87(18) . . ? C26 Si3 C27 108.43(18) . . ? C24 Si4 C28 111.79(16) . . ? C24 Si4 C29 110.21(15) . . ? C24 Si4 C30 113.12(14) . . ? C28 Si4 C29 108.37(19) . . ? C28 Si4 C30 106.90(16) . . ? C29 Si4 C30 106.17(17) . . ? Li2 O3 C39 120.5(2) . . ? Li2 O3 C42 131.0(2) . . ? C39 O3 C42 108.5(2) . . ? Li2 O4 C43 123.7(3) . . ? Li2 O4 C46 117.7(3) . . ? C43 O4 C46 109.4(3) . . ? Li2 N2 C36 94.4(2) . . ? Li2 N2 C37 120.4(2) . . ? Li2 N2 C38 104.3(2) . . ? C36 N2 C37 111.9(2) . . ? C36 N2 C38 115.5(2) . . ? C37 N2 C38 109.7(3) . . ? P2 Li2 O3 117.9(2) . . ? P2 Li2 O4 124.6(2) . . ? P2 Li2 N2 79.75(17) . . ? P2 Li2 C36 65.37(14) . . ? O3 Li2 O4 107.9(3) . . ? O3 Li2 N2 108.9(3) . . ? O3 Li2 C36 89.4(2) . . ? O4 Li2 N2 113.9(3) . . ? O4 Li2 C36 146.5(3) . . ? N2 Li2 C36 32.69(11) . . ? P2 C24 Si3 107.54(14) . . ? P2 C24 Si4 110.03(15) . . ? P2 C24 H24 107.1 . . ? Si3 C24 Si4 117.38(15) . . ? Si3 C24 H24 107.1 . . ? Si4 C24 H24 107.1 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P2 C31 C32 125.5(2) . . ? P2 C31 C36 119.2(2) . . ? C32 C31 C36 115.2(3) . . ? C31 C32 H32 118.4 . . ? C31 C32 C33 123.1(3) . . ? H32 C32 C33 118.4 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.5(3) . . ? H33 C33 C34 119.8 . . ? C33 C34 H34 120.8 . . ? C33 C34 C35 118.4(3) . . ? H34 C34 C35 120.8 . . ? C34 C35 H35 119.3 . . ? C34 C35 C36 121.3(3) . . ? H35 C35 C36 119.3 . . ? N2 C36 Li2 52.87(17) . . ? N2 C36 C31 117.2(2) . . ? N2 C36 C35 121.2(3) . . ? Li2 C36 C31 80.1(2) . . ? Li2 C36 C35 134.9(2) . . ? C31 C36 C35 121.4(3) . . ? N2 C37 H37A 109.5 . . ? N2 C37 H37B 109.5 . . ? N2 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 H39A 110.9 . . ? O3 C39 H39B 110.9 . . ? O3 C39 C40 104.3(3) . . ? H39A C39 H39B 108.9 . . ? H39A C39 C40 110.9 . . ? H39B C39 C40 110.9 . . ? C39 C40 H40A 111.3 . . ? C39 C40 H40B 111.3 . . ? C39 C40 C41 102.2(3) . . ? H40A C40 H40B 109.2 . . ? H40A C40 C41 111.3 . . ? H40B C40 C41 111.3 . . ? C40 C41 H41A 110.9 . . ? C40 C41 H41B 110.9 . . ? C40 C41 C42 104.2(3) . . ? H41A C41 H41B 108.9 . . ? H41A C41 C42 110.9 . . ? H41B C41 C42 110.9 . . ? O3 C42 C41 106.5(3) . . ? O3 C42 H42A 110.4 . . ? O3 C42 H42B 110.4 . . ? C41 C42 H42A 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? O4 C43 H43A 110.5 . . ? O4 C43 H43B 110.5 . . ? O4 C43 C44 106.3(7) . . ? H43A C43 H43B 108.7 . . ? H43A C43 C44 110.5 . . ? H43B C43 C44 110.5 . . ? C43 C44 H44A 111.5 . . ? C43 C44 H44B 111.5 . . ? C43 C44 C45 101.5(13) . . ? H44A C44 H44B 109.3 . . ? H44A C44 C45 111.5 . . ? H44B C44 C45 111.5 . . ? H44C C44A H44D 108.3 . . ? H44C C44A C45A 110.0 . . ? H44D C44A C45A 110.0 . . ? C44 C45 H45A 109.4 . . ? C44 C45 H45B 109.4 . . ? C44 C45 C46 111.1(16) . . ? H45A C45 H45B 108.0 . . ? H45A C45 C46 109.4 . . ? H45B C45 C46 109.4 . . ? C44A C45A H45C 112.6 . . ? C44A C45A H45D 112.6 . . ? H45C C45A H45D 110.1 . . ? O4 C46 C45 105.1(10) . . ? O4 C46 H46A 110.7 . . ? O4 C46 H46B 110.7 . . ? C45 C46 H46A 110.7 . . ? C45 C46 H46B 110.7 . . ? H46A C46 H46B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.358 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.092 #===END data_ki253_compound_8 _database_code_depnum_ccdc_archive 'CCDC 622826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H45 N3 Na P Si2' _chemical_formula_sum 'C21 H45 N3 Na P Si2' _chemical_formula_weight 449.74 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8078(15) _cell_length_b 11.4689(16) _cell_length_c 13.6466(9) _cell_angle_alpha 90.930(9) _cell_angle_beta 103.882(9) _cell_angle_gamma 103.782(15) _cell_volume 1442.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 406 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31788 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.19 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6595 _reflns_number_gt 5236 _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^)+(0.0441P)^2^+0.3719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6595 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 P P 0.53278(4) 0.11285(3) 0.80415(2) 0.02054(9) Uani 1 1 d . . . Si1 Si 0.38361(5) 0.30397(4) 0.70963(3) 0.03298(11) Uani 1 1 d . . . Si2 Si 0.72951(5) 0.33982(4) 0.74343(3) 0.03354(11) Uani 1 1 d . . . Na Na 0.28866(6) -0.07730(5) 0.80072(4) 0.02903(14) Uani 1 1 d . . . N1 N 0.51251(12) -0.14359(10) 0.87126(8) 0.0227(2) Uani 1 1 d . . . N2 N 0.04808(13) -0.14653(12) 0.83419(9) 0.0326(3) Uani 1 1 d . . . N3 N 0.14392(13) -0.20855(11) 0.64557(9) 0.0309(3) Uani 1 1 d . . . C1 C 0.54181(15) 0.23681(12) 0.71383(10) 0.0237(3) Uani 1 1 d . . . H1A H 0.5250 0.1964 0.6450 0.028 Uiso 1 1 calc R . . C2 C 0.20883(19) 0.19128(18) 0.64750(14) 0.0498(5) Uani 1 1 d . . . H2A H 0.2089 0.1692 0.5779 0.075 Uiso 1 1 calc R . . H2B H 0.1271 0.2267 0.6468 0.075 Uiso 1 1 calc R . . H2C H 0.1994 0.1192 0.6855 0.075 Uiso 1 1 calc R . . C3 C 0.3892(3) 0.43585(17) 0.62941(15) 0.0613(6) Uani 1 1 d . . . H3A H 0.3966 0.4116 0.5621 0.092 Uiso 1 1 calc R . . H3B H 0.4734 0.5015 0.6613 0.092 Uiso 1 1 calc R . . H3C H 0.3003 0.4632 0.6230 0.092 Uiso 1 1 calc R . . C4 C 0.3706(2) 0.35452(19) 0.83782(13) 0.0513(5) Uani 1 1 d . . . H4A H 0.4593 0.4153 0.8711 0.077 Uiso 1 1 calc R . . H4B H 0.3588 0.2854 0.8790 0.077 Uiso 1 1 calc R . . H4C H 0.2869 0.3893 0.8303 0.077 Uiso 1 1 calc R . . C5 C 0.7558(2) 0.43509(18) 0.63426(15) 0.0602(6) Uani 1 1 d . . . H5A H 0.7190 0.3841 0.5706 0.090 Uiso 1 1 calc R . . H5B H 0.8592 0.4727 0.6435 0.090 Uiso 1 1 calc R . . H5C H 0.7027 0.4978 0.6322 0.090 Uiso 1 1 calc R . . C6 C 0.7644(2) 0.44189(17) 0.86065(14) 0.0537(5) Uani 1 1 d . . . H6A H 0.7402 0.3938 0.9156 0.080 Uiso 1 1 calc R . . H6B H 0.7043 0.4997 0.8469 0.080 Uiso 1 1 calc R . . H6C H 0.8670 0.4854 0.8805 0.080 Uiso 1 1 calc R . . C7 C 0.87472(18) 0.25529(18) 0.76552(15) 0.0493(4) Uani 1 1 d . . . H7A H 0.8702 0.2113 0.7022 0.074 Uiso 1 1 calc R . . H7B H 0.8599 0.1982 0.8169 0.074 Uiso 1 1 calc R . . H7C H 0.9699 0.3122 0.7890 0.074 Uiso 1 1 calc R . . C8 C 0.56855(13) -0.01108(11) 0.73698(9) 0.0187(3) Uani 1 1 d . . . C9 C 0.60717(14) -0.00271(12) 0.64278(10) 0.0236(3) Uani 1 1 d . . . H9 H 0.6245 0.0736 0.6157 0.028 Uiso 1 1 calc R . . C10 C 0.62065(15) -0.10147(13) 0.58861(10) 0.0278(3) Uani 1 1 d . . . H10 H 0.6453 -0.0915 0.5255 0.033 Uiso 1 1 calc R . . C11 C 0.59847(16) -0.21408(13) 0.62589(11) 0.0298(3) Uani 1 1 d . . . H11 H 0.6049 -0.2820 0.5881 0.036 Uiso 1 1 calc R . . C12 C 0.56640(15) -0.22596(12) 0.72027(10) 0.0261(3) Uani 1 1 d . . . H12 H 0.5539 -0.3025 0.7473 0.031 Uiso 1 1 calc R . . C13 C 0.55241(13) -0.12823(12) 0.77558(9) 0.0198(3) Uani 1 1 d . . . C14 C 0.45443(18) -0.26836(14) 0.89308(12) 0.0364(4) Uani 1 1 d . . . H14A H 0.5317 -0.3110 0.9048 0.055 Uiso 1 1 calc R . . H14B H 0.3756 -0.3092 0.8354 0.055 Uiso 1 1 calc R . . H14C H 0.4173 -0.2679 0.9536 0.055 Uiso 1 1 calc R . . C15 C 0.63134(16) -0.08385(13) 0.95848(10) 0.0287(3) Uani 1 1 d . . . H15A H 0.7091 -0.1259 0.9684 0.043 Uiso 1 1 calc R . . H15B H 0.5948 -0.0859 1.0194 0.043 Uiso 1 1 calc R . . H15C H 0.6692 0.0000 0.9456 0.043 Uiso 1 1 calc R . . C16 C -0.01552(19) -0.04147(17) 0.82600(15) 0.0477(4) Uani 1 1 d . . . H16A H -0.1159 -0.0665 0.8316 0.072 Uiso 1 1 calc R . . H16B H -0.0139 -0.0084 0.7604 0.072 Uiso 1 1 calc R . . H16C H 0.0410 0.0202 0.8806 0.072 Uiso 1 1 calc R . . C17 C 0.0435(2) -0.1960(2) 0.93250(13) 0.0526(5) Uani 1 1 d . . . H17A H -0.0576 -0.2254 0.9355 0.079 Uiso 1 1 calc R . . H17B H 0.0943 -0.1329 0.9871 0.079 Uiso 1 1 calc R . . H17C H 0.0908 -0.2628 0.9403 0.079 Uiso 1 1 calc R . . C18 C -0.03444(15) -0.24119(15) 0.75219(11) 0.0329(3) Uani 1 1 d . . . H18A H -0.1393 -0.2535 0.7473 0.040 Uiso 1 1 calc R . . H18B H -0.0083 -0.3177 0.7701 0.040 Uiso 1 1 calc R . . C19 C -0.00661(16) -0.21135(15) 0.64939(11) 0.0331(3) Uani 1 1 d . . . H19A H -0.0750 -0.2722 0.5969 0.040 Uiso 1 1 calc R . . H19B H -0.0257 -0.1319 0.6336 0.040 Uiso 1 1 calc R . . C20 C 0.1792(2) -0.14783(18) 0.55755(13) 0.0494(5) Uani 1 1 d . . . H20A H 0.1144 -0.1925 0.4952 0.074 Uiso 1 1 calc R . . H20B H 0.2800 -0.1448 0.5578 0.074 Uiso 1 1 calc R . . H20C H 0.1667 -0.0657 0.5609 0.074 Uiso 1 1 calc R . . C21 C 0.16200(18) -0.33175(15) 0.63772(14) 0.0436(4) Uani 1 1 d . . . H21A H 0.0939 -0.3758 0.5763 0.065 Uiso 1 1 calc R . . H21B H 0.1426 -0.3729 0.6972 0.065 Uiso 1 1 calc R . . H21C H 0.2615 -0.3286 0.6345 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.02470(18) 0.01822(17) 0.02052(17) 0.00249(12) 0.00945(13) 0.00496(13) Si1 0.0470(3) 0.0316(2) 0.0269(2) 0.00360(16) 0.00883(18) 0.02255(19) Si2 0.0392(2) 0.0261(2) 0.0300(2) 0.00304(16) 0.01149(18) -0.00483(17) Na 0.0190(3) 0.0282(3) 0.0386(3) 0.0002(2) 0.0079(2) 0.0029(2) N1 0.0232(6) 0.0240(6) 0.0212(5) 0.0067(4) 0.0071(4) 0.0045(4) N2 0.0221(6) 0.0409(7) 0.0328(7) -0.0001(5) 0.0090(5) 0.0023(5) N3 0.0240(6) 0.0345(7) 0.0334(7) -0.0012(5) 0.0105(5) 0.0025(5) C1 0.0320(7) 0.0183(6) 0.0213(6) 0.0022(5) 0.0081(5) 0.0057(5) C2 0.0373(9) 0.0666(13) 0.0493(10) 0.0027(9) 0.0053(8) 0.0260(9) C3 0.1087(18) 0.0429(11) 0.0466(11) 0.0136(8) 0.0197(11) 0.0454(12) C4 0.0692(13) 0.0623(12) 0.0368(9) 0.0024(8) 0.0181(9) 0.0390(10) C5 0.0733(14) 0.0480(11) 0.0501(11) 0.0159(9) 0.0238(10) -0.0116(10) C6 0.0611(12) 0.0417(10) 0.0455(10) -0.0092(8) 0.0090(9) -0.0060(9) C7 0.0292(9) 0.0554(11) 0.0575(11) 0.0008(9) 0.0133(8) -0.0026(8) C8 0.0160(6) 0.0212(6) 0.0185(6) 0.0012(5) 0.0041(5) 0.0039(5) C9 0.0248(7) 0.0253(7) 0.0229(7) 0.0045(5) 0.0092(5) 0.0070(5) C10 0.0279(7) 0.0377(8) 0.0205(6) -0.0007(6) 0.0085(5) 0.0107(6) C11 0.0320(8) 0.0292(8) 0.0289(7) -0.0061(6) 0.0061(6) 0.0110(6) C12 0.0259(7) 0.0216(7) 0.0300(7) 0.0015(5) 0.0043(6) 0.0072(5) C13 0.0161(6) 0.0230(7) 0.0197(6) 0.0025(5) 0.0036(5) 0.0044(5) C14 0.0420(9) 0.0296(8) 0.0354(8) 0.0124(6) 0.0121(7) 0.0019(7) C15 0.0309(7) 0.0340(8) 0.0206(7) 0.0044(6) 0.0054(6) 0.0083(6) C16 0.0371(9) 0.0493(11) 0.0597(11) -0.0075(9) 0.0199(8) 0.0096(8) C17 0.0457(10) 0.0710(13) 0.0339(9) 0.0037(9) 0.0122(8) -0.0013(9) C18 0.0201(7) 0.0394(9) 0.0363(8) 0.0005(6) 0.0079(6) 0.0008(6) C19 0.0246(7) 0.0407(9) 0.0325(8) 0.0008(6) 0.0044(6) 0.0084(6) C20 0.0506(11) 0.0567(12) 0.0418(10) 0.0044(8) 0.0231(8) 0.0030(9) C21 0.0355(9) 0.0412(10) 0.0526(10) -0.0098(8) 0.0089(8) 0.0101(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P Na 2.8189(8) . ? P C1 1.8967(13) . ? P C8 1.8257(13) . ? Si1 C1 1.8794(14) . ? Si1 C2 1.881(2) . ? Si1 C3 1.8794(18) . ? Si1 C4 1.8768(17) . ? Si2 C1 1.8813(15) . ? Si2 C5 1.8928(18) . ? Si2 C6 1.8793(18) . ? Si2 C7 1.876(2) . ? Na N1 2.4758(13) . ? Na N2 2.4582(13) . ? Na N3 2.4900(14) . ? Na C8 3.0072(14) . ? Na C13 2.8792(14) . ? N1 C13 1.4522(16) . ? N1 C14 1.4723(18) . ? N1 C15 1.4737(18) . ? N2 C16 1.477(2) . ? N2 C17 1.472(2) . ? N2 C18 1.4809(19) . ? N3 C19 1.4825(18) . ? N3 C20 1.469(2) . ? N3 C21 1.471(2) . ? C1 H1A 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.4231(17) . ? C8 C13 1.4385(18) . ? C9 H9 0.950 . ? C9 C10 1.3922(19) . ? C10 H10 0.950 . ? C10 C11 1.384(2) . ? C11 H11 0.950 . ? C11 C12 1.399(2) . ? C12 H12 0.950 . ? C12 C13 1.3930(19) . ? 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 0.990 . ? C18 H18B 0.990 . ? C18 C19 1.521(2) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 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 Na P C1 126.06(5) . . ? Na P C8 77.45(4) . . ? C1 P C8 103.91(6) . . ? C1 Si1 C2 110.18(7) . . ? C1 Si1 C3 111.61(9) . . ? C1 Si1 C4 113.56(7) . . ? C2 Si1 C3 105.20(10) . . ? C2 Si1 C4 107.78(9) . . ? C3 Si1 C4 108.10(9) . . ? C1 Si2 C5 110.82(8) . . ? C1 Si2 C6 111.09(8) . . ? C1 Si2 C7 112.52(7) . . ? C5 Si2 C6 108.92(9) . . ? C5 Si2 C7 106.20(10) . . ? C6 Si2 C7 107.07(9) . . ? P Na N1 70.53(3) . . ? P Na N2 148.88(4) . . ? P Na N3 123.52(4) . . ? P Na C8 36.34(3) . . ? P Na C13 59.87(3) . . ? N1 Na N2 128.96(5) . . ? N1 Na N3 109.32(4) . . ? N1 Na C8 52.68(4) . . ? N1 Na C13 30.29(4) . . ? N2 Na N3 76.74(4) . . ? N2 Na C8 173.28(4) . . ? N2 Na C13 149.74(5) . . ? N3 Na C8 96.55(4) . . ? N3 Na C13 91.34(4) . . ? C8 Na C13 28.18(3) . . ? Na N1 C13 90.41(7) . . ? Na N1 C14 102.19(9) . . ? Na N1 C15 125.99(9) . . ? C13 N1 C14 116.21(11) . . ? C13 N1 C15 112.70(10) . . ? C14 N1 C15 108.70(11) . . ? Na N2 C16 106.28(10) . . ? Na N2 C17 116.73(10) . . ? Na N2 C18 105.06(8) . . ? C16 N2 C17 108.93(14) . . ? C16 N2 C18 110.79(13) . . ? C17 N2 C18 108.95(13) . . ? Na N3 C19 101.90(9) . . ? Na N3 C20 107.90(10) . . ? Na N3 C21 117.48(10) . . ? C19 N3 C20 110.95(13) . . ? C19 N3 C21 110.31(12) . . ? C20 N3 C21 108.16(13) . . ? P C1 Si1 107.92(7) . . ? P C1 Si2 110.44(7) . . ? P C1 H1A 106.3 . . ? Si1 C1 Si2 118.71(7) . . ? Si1 C1 H1A 106.3 . . ? Si2 C1 H1A 106.3 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 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 . . ? P C8 Na 66.20(4) . . ? P C8 C9 124.14(10) . . ? P C8 C13 120.75(9) . . ? Na C8 C9 135.31(9) . . ? Na C8 C13 70.96(7) . . ? C9 C8 C13 115.05(11) . . ? C8 C9 H9 118.5 . . ? C8 C9 C10 122.91(13) . . ? H9 C9 C10 118.5 . . ? C9 C10 H10 119.7 . . ? C9 C10 C11 120.54(13) . . ? H10 C10 C11 119.7 . . ? C10 C11 H11 120.6 . . ? C10 C11 C12 118.71(13) . . ? H11 C11 C12 120.6 . . ? C11 C12 H12 119.2 . . ? C11 C12 C13 121.56(13) . . ? H12 C12 C13 119.2 . . ? Na C13 N1 59.31(6) . . ? Na C13 C8 80.86(7) . . ? Na C13 C12 127.56(9) . . ? N1 C13 C8 118.09(11) . . ? N1 C13 C12 120.70(12) . . ? C8 C13 C12 121.12(12) . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 108.9 . . ? N2 C18 H18B 108.9 . . ? N2 C18 C19 113.44(12) . . ? H18A C18 H18B 107.7 . . ? H18A C18 C19 108.9 . . ? H18B C18 C19 108.9 . . ? N3 C19 C18 112.58(12) . . ? N3 C19 H19A 109.1 . . ? N3 C19 H19B 109.1 . . ? C18 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.264 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.045 #===END data_ki257_compound_9 _database_code_depnum_ccdc_archive 'CCDC 622827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H52 K N4 P Si2' _chemical_formula_sum 'C24 H52 K N4 P Si2' _chemical_formula_weight 522.95 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' 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 '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 14.4291(19) _cell_length_b 11.2424(15) _cell_length_c 19.756(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.555(2) _cell_angle_gamma 90.00 _cell_volume 3198.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6111 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.915 _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 22885 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5630 _reflns_number_gt 4544 _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 SIR2002 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0600P)^2^+4.7914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5630 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 K K 0.76082(5) 0.38693(7) 0.36405(3) 0.0405(2) Uani 1 1 d . A . P P 0.79376(5) 0.57487(6) 0.48616(4) 0.02544(19) Uani 1 1 d . A . Si1 Si 0.72011(6) 0.79076(8) 0.40912(5) 0.0347(2) Uani 1 1 d . . . Si2 Si 0.73462(7) 0.78435(8) 0.57260(5) 0.0398(2) Uani 1 1 d . . . N1 N 0.85351(17) 0.3146(2) 0.49000(13) 0.0320(6) Uani 1 1 d . . . N2 N 0.58944(19) 0.3475(3) 0.28985(15) 0.0464(7) Uani 1 1 d . . . N3 N 0.7662(2) 0.2223(3) 0.25357(14) 0.0456(7) Uani 1 1 d . A . N4 N 0.9127(2) 0.4081(3) 0.28357(16) 0.0546(8) Uani 1 1 d . . . C1 C 0.71184(19) 0.7066(2) 0.49002(15) 0.0288(6) Uani 1 1 d . . . H1 H 0.6474 0.6737 0.4898 0.035 Uiso 1 1 calc R . . C2 C 0.6492(3) 0.9312(3) 0.4080(2) 0.0537(10) Uani 1 1 d . . . H2A H 0.5857 0.9125 0.4195 0.081 Uiso 1 1 calc R . . H2B H 0.6478 0.9667 0.3626 0.081 Uiso 1 1 calc R . . H2C H 0.6770 0.9875 0.4412 0.081 Uiso 1 1 calc R . . C3 C 0.6694(3) 0.6986(3) 0.33702(18) 0.0504(9) Uani 1 1 d . . . H3A H 0.7128 0.6348 0.3270 0.076 Uiso 1 1 calc R . . H3B H 0.6583 0.7489 0.2968 0.076 Uiso 1 1 calc R . . H3C H 0.6105 0.6639 0.3495 0.076 Uiso 1 1 calc R . . C4 C 0.8421(2) 0.8307(3) 0.3909(2) 0.0511(9) Uani 1 1 d . . . H4A H 0.8826 0.7617 0.3996 0.077 Uiso 1 1 calc R . . H4B H 0.8635 0.8968 0.4203 0.077 Uiso 1 1 calc R . . H4C H 0.8440 0.8546 0.3433 0.077 Uiso 1 1 calc R . . C5 C 0.7359(3) 0.6791(3) 0.64606(17) 0.0490(9) Uani 1 1 d . . . H5A H 0.7768 0.6118 0.6376 0.074 Uiso 1 1 calc R . . H5B H 0.6728 0.6498 0.6515 0.074 Uiso 1 1 calc R . . H5C H 0.7587 0.7205 0.6875 0.074 Uiso 1 1 calc R . . C6 C 0.8506(3) 0.8605(4) 0.5736(2) 0.0659(12) Uani 1 1 d . . . H6A H 0.8981 0.8032 0.5616 0.099 Uiso 1 1 calc R . . H6B H 0.8665 0.8922 0.6191 0.099 Uiso 1 1 calc R . . H6C H 0.8477 0.9258 0.5407 0.099 Uiso 1 1 calc R . . C7 C 0.6441(4) 0.9006(3) 0.5880(3) 0.0727(14) Uani 1 1 d . . . H7A H 0.5821 0.8663 0.5793 0.109 Uiso 1 1 calc R . . H7B H 0.6517 0.9682 0.5575 0.109 Uiso 1 1 calc R . . H7C H 0.6515 0.9277 0.6351 0.109 Uiso 1 1 calc R . . C8 C 0.72545(18) 0.4507(2) 0.51381(13) 0.0235(6) Uani 1 1 d . . . C9 C 0.6334(2) 0.4591(3) 0.53435(14) 0.0295(6) Uani 1 1 d . A . H9A H 0.6077 0.5361 0.5396 0.035 Uiso 1 1 calc R . . C10 C 0.5791(2) 0.3620(3) 0.54715(16) 0.0357(7) Uani 1 1 d . . . H10A H 0.5172 0.3733 0.5596 0.043 Uiso 1 1 calc R A . C11 C 0.6143(2) 0.2482(3) 0.54190(17) 0.0380(7) Uani 1 1 d . A . H11A H 0.5766 0.1807 0.5495 0.046 Uiso 1 1 calc R . . C12 C 0.7058(2) 0.2346(3) 0.52535(15) 0.0330(7) Uani 1 1 d . . . H12A H 0.7311 0.1568 0.5231 0.040 Uiso 1 1 calc R A . C13 C 0.76135(19) 0.3313(2) 0.51207(13) 0.0256(6) Uani 1 1 d . A . C14 C 0.8763(3) 0.1937(3) 0.4690(2) 0.0518(10) Uani 1 1 d . . . H14A H 0.8279 0.1648 0.4361 0.078 Uiso 1 1 calc R . . H14B H 0.8799 0.1413 0.5088 0.078 Uiso 1 1 calc R . . H14C H 0.9362 0.1941 0.4482 0.078 Uiso 1 1 calc R . . C15 C 0.9279(2) 0.3608(3) 0.53666(18) 0.0410(8) Uani 1 1 d . . . H15A H 0.9112 0.4404 0.5520 0.061 Uiso 1 1 calc R . . H15B H 0.9858 0.3650 0.5133 0.061 Uiso 1 1 calc R . . H15C H 0.9364 0.3077 0.5759 0.061 Uiso 1 1 calc R . . C16 C 0.6012(3) 0.2892(5) 0.2233(3) 0.0746(13) Uani 1 1 d . . . H16A H 0.5408 0.2550 0.2066 0.090 Uiso 1 1 calc R . . H16B H 0.6183 0.3506 0.1904 0.090 Uiso 1 1 calc R . . C17 C 0.6717(3) 0.1945(4) 0.2252(2) 0.0569(10) Uani 1 1 d . . . H17A H 0.6769 0.1658 0.1783 0.068 Uiso 1 1 calc R . . H17B H 0.6480 0.1274 0.2516 0.068 Uiso 1 1 calc R . . C18 C 0.8135(4) 0.2917(5) 0.2024(2) 0.0860(17) Uani 1 1 d . . . H18A H 0.8182 0.2417 0.1615 0.103 Uiso 1 1 calc R A . H18B H 0.7744 0.3613 0.1893 0.103 Uiso 1 1 calc R . . C19 C 0.9069(3) 0.3342(5) 0.2243(3) 0.0822(15) Uani 1 1 d . A . H19A H 0.9475 0.2642 0.2330 0.099 Uiso 1 1 calc R . . H19B H 0.9318 0.3793 0.1864 0.099 Uiso 1 1 calc R . . C20 C 0.5251(3) 0.4445(4) 0.2723(3) 0.0778(14) Uani 1 1 d . . . H20A H 0.5123 0.4889 0.3134 0.117 Uiso 1 1 calc R . . H20B H 0.4670 0.4118 0.2518 0.117 Uiso 1 1 calc R . . H20C H 0.5528 0.4980 0.2399 0.117 Uiso 1 1 calc R . . C21 C 0.5488(4) 0.2736(6) 0.3383(3) 0.100(2) Uani 1 1 d . . . H21A H 0.5388 0.3198 0.3793 0.150 Uiso 1 1 calc R . . H21B H 0.5904 0.2067 0.3499 0.150 Uiso 1 1 calc R . . H21C H 0.4891 0.2431 0.3192 0.150 Uiso 1 1 calc R . . C22 C 0.8118(3) 0.1120(4) 0.2729(3) 0.0881(17) Uani 1 1 d . . . H22A H 0.7721 0.0660 0.3017 0.132 Uiso 1 1 calc R A . H22B H 0.8710 0.1292 0.2980 0.132 Uiso 1 1 calc R . . H22C H 0.8233 0.0660 0.2321 0.132 Uiso 1 1 calc R . . C23 C 0.984(3) 0.440(6) 0.337(2) 0.059(11) Uani 0.21(5) 1 d P A 1 H23A H 0.9574 0.4970 0.3685 0.089 Uiso 0.21(5) 1 calc PR A 1 H23B H 1.0372 0.4761 0.3170 0.089 Uiso 0.21(5) 1 calc PR A 1 H23C H 1.0036 0.3683 0.3625 0.089 Uiso 0.21(5) 1 calc PR A 1 C23A C 1.0067(11) 0.3876(19) 0.3166(10) 0.086(4) Uani 0.79(5) 1 d P A 2 H23D H 1.0146 0.4363 0.3577 0.130 Uiso 0.79(5) 1 calc PR A 2 H23E H 1.0538 0.4097 0.2852 0.130 Uiso 0.79(5) 1 calc PR A 2 H23F H 1.0136 0.3034 0.3287 0.130 Uiso 0.79(5) 1 calc PR A 2 C24 C 0.8970(4) 0.5318(5) 0.2660(3) 0.0946(17) Uani 1 1 d . A . H24A H 0.8358 0.5404 0.2420 0.142 Uiso 1 1 calc R . . H24B H 0.9450 0.5588 0.2366 0.142 Uiso 1 1 calc R . . H24C H 0.8994 0.5800 0.3074 0.142 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 K 0.0523(4) 0.0402(4) 0.0285(4) -0.0072(3) -0.0015(3) 0.0032(3) P 0.0247(4) 0.0197(4) 0.0321(4) 0.0008(3) 0.0037(3) -0.0008(3) Si1 0.0323(5) 0.0271(4) 0.0445(5) 0.0089(4) 0.0000(4) 0.0010(3) Si2 0.0474(5) 0.0280(5) 0.0454(5) -0.0083(4) 0.0146(4) -0.0049(4) N1 0.0281(13) 0.0254(13) 0.0430(15) 0.0039(11) 0.0058(11) 0.0025(10) N2 0.0363(15) 0.0491(18) 0.0547(18) -0.0019(14) 0.0089(13) -0.0061(13) N3 0.0500(17) 0.0435(17) 0.0444(16) -0.0155(13) 0.0119(13) -0.0081(14) N4 0.0498(18) 0.060(2) 0.0529(19) 0.0032(16) -0.0030(15) -0.0202(16) C1 0.0258(14) 0.0210(14) 0.0400(16) 0.0016(12) 0.0052(12) 0.0003(11) C2 0.051(2) 0.0348(19) 0.074(3) 0.0117(18) -0.0046(19) 0.0085(16) C3 0.056(2) 0.048(2) 0.045(2) 0.0041(16) -0.0041(17) 0.0027(17) C4 0.042(2) 0.047(2) 0.065(2) 0.0217(18) 0.0098(17) -0.0019(16) C5 0.060(2) 0.050(2) 0.0384(19) -0.0074(16) 0.0091(16) 0.0006(18) C6 0.072(3) 0.066(3) 0.060(2) -0.021(2) 0.009(2) -0.033(2) C7 0.101(4) 0.034(2) 0.089(3) 0.000(2) 0.051(3) 0.015(2) C8 0.0242(14) 0.0229(14) 0.0232(13) 0.0008(11) -0.0005(11) -0.0020(11) C9 0.0295(15) 0.0267(15) 0.0325(15) 0.0021(12) 0.0042(12) 0.0020(12) C10 0.0262(15) 0.0415(18) 0.0399(17) 0.0059(14) 0.0052(13) -0.0039(13) C11 0.0373(17) 0.0320(17) 0.0449(18) 0.0048(14) 0.0035(14) -0.0137(14) C12 0.0391(17) 0.0252(15) 0.0344(16) 0.0018(12) 0.0006(13) -0.0014(13) C13 0.0276(14) 0.0250(14) 0.0241(14) 0.0007(11) 0.0005(11) -0.0019(11) C14 0.048(2) 0.0307(18) 0.079(3) -0.0013(17) 0.0204(19) 0.0085(15) C15 0.0287(16) 0.0409(19) 0.053(2) 0.0150(16) -0.0013(14) 0.0006(14) C16 0.057(3) 0.086(3) 0.080(3) -0.018(3) -0.006(2) -0.011(2) C17 0.062(2) 0.054(2) 0.053(2) -0.0177(18) -0.0107(19) -0.0012(19) C18 0.086(3) 0.127(5) 0.047(2) -0.028(3) 0.018(2) -0.039(3) C19 0.061(3) 0.109(4) 0.080(3) -0.022(3) 0.033(2) -0.021(3) C20 0.071(3) 0.061(3) 0.097(4) 0.010(3) -0.027(3) -0.005(2) C21 0.068(3) 0.128(5) 0.106(4) 0.056(4) 0.011(3) -0.002(3) C22 0.065(3) 0.066(3) 0.129(5) -0.042(3) -0.021(3) 0.020(2) C23 0.039(14) 0.08(2) 0.063(18) 0.018(15) -0.007(11) -0.011(13) C23A 0.060(6) 0.095(8) 0.101(8) 0.013(7) -0.021(5) -0.019(6) C24 0.094(4) 0.076(4) 0.115(5) 0.007(3) 0.013(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K N4 2.797(3) . ? K N2 2.830(3) . ? K N3 2.866(3) . ? K N1 2.869(3) . ? K C13 2.990(3) . ? K C8 3.117(3) . ? K P 3.2198(10) . ? K C18 3.496(4) . ? P C8 1.812(3) . ? P C1 1.899(3) . ? Si1 C1 1.867(3) . ? Si1 C4 1.873(3) . ? Si1 C3 1.873(4) . ? Si1 C2 1.881(4) . ? Si2 C1 1.862(3) . ? Si2 C5 1.872(4) . ? Si2 C6 1.879(4) . ? Si2 C7 1.885(4) . ? N1 C13 1.437(4) . ? N1 C14 1.464(4) . ? N1 C15 1.465(4) . ? N2 C21 1.422(5) . ? N2 C20 1.460(5) . ? N2 C16 1.488(5) . ? N3 C22 1.444(5) . ? N3 C17 1.474(5) . ? N3 C18 1.477(6) . ? N4 C19 1.435(6) . ? N4 C24 1.448(6) . ? N4 C23 1.47(3) . ? N4 C23A 1.486(12) . ? C1 H1 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.416(4) . ? C8 C13 1.440(4) . ? C9 C10 1.376(4) . ? C9 H9A 0.950 . ? C10 C11 1.383(5) . ? C10 H10A 0.950 . ? C11 C12 1.389(4) . ? C11 H11A 0.950 . ? C12 C13 1.385(4) . ? C12 H12A 0.950 . ? 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 C17 1.473(6) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 C19 1.469(6) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C23A H23D 0.980 . ? C23A H23E 0.980 . ? C23A H23F 0.980 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 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 N4 K N2 114.16(9) . . ? N4 K N3 64.09(9) . . ? N2 K N3 64.43(9) . . ? N4 K N1 100.23(9) . . ? N2 K N1 138.62(8) . . ? N3 K N1 116.39(8) . . ? N4 K C13 128.26(9) . . ? N2 K C13 115.02(8) . . ? N3 K C13 127.68(9) . . ? N1 K C13 28.31(7) . . ? N4 K C8 134.45(8) . . ? N2 K C8 109.78(8) . . ? N3 K C8 152.27(8) . . ? N1 K C8 48.46(7) . . ? C13 K C8 27.18(7) . . ? N4 K P 106.59(7) . . ? N2 K P 125.05(7) . . ? N3 K P 169.90(7) . . ? N1 K P 59.79(5) . . ? C13 K P 54.06(6) . . ? C8 K P 33.18(5) . . ? N4 K C18 44.31(10) . . ? N2 K C18 73.23(10) . . ? N3 K C18 24.36(11) . . ? N1 K C18 126.12(12) . . ? C13 K C18 147.33(12) . . ? C8 K C18 174.35(12) . . ? P K C18 148.76(9) . . ? C8 P C1 103.70(12) . . ? C8 P K 70.29(9) . . ? C1 P K 118.59(10) . . ? C1 Si1 C4 113.37(15) . . ? C1 Si1 C3 109.14(15) . . ? C4 Si1 C3 108.31(19) . . ? C1 Si1 C2 111.85(16) . . ? C4 Si1 C2 108.27(17) . . ? C3 Si1 C2 105.56(18) . . ? C1 Si2 C5 112.03(15) . . ? C1 Si2 C6 109.39(16) . . ? C5 Si2 C6 108.3(2) . . ? C1 Si2 C7 112.3(2) . . ? C5 Si2 C7 106.69(18) . . ? C6 Si2 C7 107.9(2) . . ? C13 N1 C14 115.8(2) . . ? C13 N1 C15 114.7(2) . . ? C14 N1 C15 109.8(3) . . ? C13 N1 K 80.55(15) . . ? C14 N1 K 96.8(2) . . ? C15 N1 K 136.83(19) . . ? C21 N2 C20 108.3(4) . . ? C21 N2 C16 114.3(4) . . ? C20 N2 C16 103.0(4) . . ? C21 N2 K 97.3(3) . . ? C20 N2 K 121.9(2) . . ? C16 N2 K 112.5(2) . . ? C22 N3 C17 108.3(3) . . ? C22 N3 C18 114.3(4) . . ? C17 N3 C18 107.9(3) . . ? C22 N3 K 112.7(3) . . ? C17 N3 K 111.0(2) . . ? C18 N3 K 102.5(2) . . ? C19 N4 C24 111.1(4) . . ? C19 N4 C23 137(3) . . ? C24 N4 C23 92(2) . . ? C19 N4 C23A 106.0(12) . . ? C24 N4 C23A 112.3(7) . . ? C23 N4 C23A 31.4(19) . . ? C19 N4 K 114.0(2) . . ? C24 N4 K 95.8(3) . . ? C23 N4 K 98.3(19) . . ? C23A N4 K 117.6(8) . . ? Si2 C1 Si1 119.65(15) . . ? Si2 C1 P 108.95(15) . . ? Si1 C1 P 106.73(14) . . ? Si2 C1 H1 107.0 . . ? Si1 C1 H1 107.0 . . ? P C1 H1 107.0 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 114.5(2) . . ? C9 C8 P 124.9(2) . . ? C13 C8 P 120.5(2) . . ? C9 C8 K 119.94(18) . . ? C13 C8 K 71.49(15) . . ? P C8 K 76.53(9) . . ? C10 C9 C8 123.7(3) . . ? C10 C9 H9A 118.1 . . ? C8 C9 H9A 118.1 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 118.5(3) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C13 C12 C11 121.9(3) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 N1 120.8(3) . . ? C12 C13 C8 120.9(3) . . ? N1 C13 C8 118.0(2) . . ? C12 C13 K 112.51(19) . . ? N1 C13 K 71.15(15) . . ? C8 C13 K 81.33(15) . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 114.3(4) . . ? C17 C16 H16A 108.7 . . ? N2 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? N2 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 N3 118.5(3) . . ? C16 C17 H17A 107.7 . . ? N3 C17 H17A 107.7 . . ? C16 C17 H17B 107.7 . . ? N3 C17 H17B 107.7 . . ? H17A C17 H17B 107.1 . . ? C19 C18 N3 115.2(4) . . ? C19 C18 K 83.1(2) . . ? N3 C18 K 53.18(18) . . ? C19 C18 H18A 108.5 . . ? N3 C18 H18A 108.5 . . ? K C18 H18A 161.7 . . ? C19 C18 H18B 108.5 . . ? N3 C18 H18B 108.5 . . ? K C18 H18B 81.1 . . ? H18A C18 H18B 107.5 . . ? N4 C19 C18 115.8(4) . . ? N4 C19 H19A 108.3 . . ? C18 C19 H19A 108.3 . . ? N4 C19 H19B 108.3 . . ? C18 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C23A H23D 109.5 . . ? N4 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? N4 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.287 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.062 #===END data_ki254_compound_11 _database_code_depnum_ccdc_archive 'CCDC 622828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H112 N4 Na4 O2 P4 Si8' _chemical_formula_sum 'C56 H112 N4 Na4 O2 P4 Si8' _chemical_formula_weight 1314.06 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' 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' 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 11.1503(15) _cell_length_b 13.5201(18) _cell_length_c 15.406(2) _cell_angle_alpha 109.582(2) _cell_angle_beta 97.502(2) _cell_angle_gamma 110.175(2) _cell_volume 1972.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5598 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _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 14338 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6865 _reflns_number_gt 5944 _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^)+(0.0315P)^2^+1.7210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6865 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.257 _refine_ls_restrained_S_all 1.257 _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 Na1 Na 0.11773(10) 0.13534(9) 0.05939(8) 0.0266(3) Uani 1 1 d . . . Na2 Na 0.08817(11) 0.14773(10) 0.27846(8) 0.0323(3) Uani 1 1 d . . . P1 P 0.16985(7) 0.34202(6) 0.23339(5) 0.02295(17) Uani 1 1 d . . . P2 P -0.15090(7) -0.03472(6) 0.12698(5) 0.01937(16) Uani 1 1 d . . . Si1 Si 0.25244(8) 0.58426(7) 0.39471(6) 0.0284(2) Uani 1 1 d . . . Si2 Si 0.10385(8) 0.51210(7) 0.17469(6) 0.02617(19) Uani 1 1 d . . . Si3 Si -0.27498(8) 0.00376(7) 0.30042(6) 0.02776(19) Uani 1 1 d . . . Si4 Si -0.33732(8) -0.24870(6) 0.14102(6) 0.02559(19) Uani 1 1 d . . . O1 O 0.1992(2) 0.15074(17) 0.42026(14) 0.0338(5) Uani 1 1 d . . . N1 N 0.2926(2) 0.20340(19) 0.20985(17) 0.0284(5) Uani 1 1 d . . . N2 N -0.1213(2) 0.07149(19) 0.00823(16) 0.0229(5) Uani 1 1 d . . . C1 C 0.2232(3) 0.4997(2) 0.26416(18) 0.0196(5) Uani 1 1 d . . . H1 H 0.3113 0.5271 0.2507 0.024 Uiso 1 1 calc R . . C2 C 0.3593(4) 0.5464(3) 0.4701(2) 0.0544(10) Uani 1 1 d . . . H2A H 0.4468 0.5663 0.4578 0.082 Uiso 1 1 calc R . . H2B H 0.3173 0.4634 0.4541 0.082 Uiso 1 1 calc R . . H2C H 0.3700 0.5897 0.5381 0.082 Uiso 1 1 calc R . . C3 C 0.0914(4) 0.5555(3) 0.4249(3) 0.0614(11) Uani 1 1 d . . . H3A H 0.0431 0.5910 0.3970 0.092 Uiso 1 1 calc R . . H3B H 0.1080 0.5884 0.4947 0.092 Uiso 1 1 calc R . . H3C H 0.0381 0.4720 0.3988 0.092 Uiso 1 1 calc R . . C4 C 0.3440(4) 0.7431(3) 0.4302(2) 0.0466(9) Uani 1 1 d . . . H4A H 0.2840 0.7724 0.4059 0.070 Uiso 1 1 calc R . . H4B H 0.4198 0.7572 0.4030 0.070 Uiso 1 1 calc R . . H4C H 0.3762 0.7829 0.5003 0.070 Uiso 1 1 calc R . . C5 C -0.0727(3) 0.4308(3) 0.1683(3) 0.0460(9) Uani 1 1 d . . . H5A H -0.0890 0.3509 0.1566 0.069 Uiso 1 1 calc R . . H5B H -0.1318 0.4317 0.1158 0.069 Uiso 1 1 calc R . . H5C H -0.0902 0.4672 0.2290 0.069 Uiso 1 1 calc R . . C6 C 0.1334(3) 0.6667(3) 0.2057(2) 0.0404(8) Uani 1 1 d . . . H6A H 0.1060 0.6957 0.2635 0.061 Uiso 1 1 calc R . . H6B H 0.0814 0.6720 0.1524 0.061 Uiso 1 1 calc R . . H6C H 0.2282 0.7131 0.2174 0.061 Uiso 1 1 calc R . . C7 C 0.1345(4) 0.4552(3) 0.0550(2) 0.0446(8) Uani 1 1 d . . . H7A H 0.1231 0.3752 0.0380 0.067 Uiso 1 1 calc R . . H7B H 0.2253 0.5027 0.0580 0.067 Uiso 1 1 calc R . . H7C H 0.0710 0.4578 0.0064 0.067 Uiso 1 1 calc R . . C8 C 0.3182(3) 0.3185(2) 0.23720(18) 0.0217(6) Uani 1 1 d . . . C9 C 0.4501(3) 0.3997(2) 0.2600(2) 0.0268(6) Uani 1 1 d . . . H9 H 0.4692 0.4795 0.2816 0.032 Uiso 1 1 calc R . . C10 C 0.5507(3) 0.3646(3) 0.2513(2) 0.0357(7) Uani 1 1 d . . . H10 H 0.6392 0.4196 0.2656 0.043 Uiso 1 1 calc R . . C11 C 0.5231(3) 0.2478(3) 0.2214(2) 0.0420(8) Uani 1 1 d . . . H11 H 0.5913 0.2212 0.2143 0.050 Uiso 1 1 calc R . . C12 C 0.3937(3) 0.1727(3) 0.2027(2) 0.0363(7) Uani 1 1 d . . . H12 H 0.3748 0.0931 0.1833 0.044 Uiso 1 1 calc R . . C13 C -0.2961(3) -0.0914(2) 0.17393(19) 0.0207(6) Uani 1 1 d . . . H13 H -0.3731 -0.0895 0.1342 0.025 Uiso 1 1 calc R . . C14 C -0.2019(3) 0.1610(2) 0.3241(2) 0.0361(7) Uani 1 1 d . . . H14A H -0.1581 0.1718 0.2747 0.054 Uiso 1 1 calc R . . H14B H -0.1367 0.2053 0.3873 0.054 Uiso 1 1 calc R . . H14C H -0.2729 0.1880 0.3225 0.054 Uiso 1 1 calc R . . C15 C -0.4417(3) -0.0296(3) 0.3248(3) 0.0546(11) Uani 1 1 d . . . H15A H -0.4833 -0.1111 0.3139 0.082 Uiso 1 1 calc R . . H15B H -0.4985 -0.0141 0.2817 0.082 Uiso 1 1 calc R . . H15C H -0.4304 0.0190 0.3915 0.082 Uiso 1 1 calc R . . C16 C -0.1629(4) -0.0170(3) 0.3874(2) 0.0445(9) Uani 1 1 d . . . H16A H -0.2012 -0.0975 0.3796 0.067 Uiso 1 1 calc R . . H16B H -0.1534 0.0339 0.4530 0.067 Uiso 1 1 calc R . . H16C H -0.0754 0.0018 0.3753 0.067 Uiso 1 1 calc R . . C17 C -0.4649(3) -0.3138(3) 0.1976(3) 0.0426(8) Uani 1 1 d . . . H17A H -0.5450 -0.3023 0.1794 0.064 Uiso 1 1 calc R . . H17B H -0.4286 -0.2764 0.2676 0.064 Uiso 1 1 calc R . . H17C H -0.4877 -0.3967 0.1755 0.064 Uiso 1 1 calc R . . C18 C -0.1874(3) -0.2726(3) 0.1800(3) 0.0416(8) Uani 1 1 d . . . H18A H -0.1179 -0.2389 0.1524 0.062 Uiso 1 1 calc R . . H18B H -0.2114 -0.3556 0.1579 0.062 Uiso 1 1 calc R . . H18C H -0.1542 -0.2356 0.2501 0.062 Uiso 1 1 calc R . . C19 C -0.4116(3) -0.3289(3) 0.0082(2) 0.0419(8) Uani 1 1 d . . . H19A H -0.3498 -0.2953 -0.0244 0.063 Uiso 1 1 calc R . . H19B H -0.4957 -0.3232 -0.0101 0.063 Uiso 1 1 calc R . . H19C H -0.4281 -0.4102 -0.0105 0.063 Uiso 1 1 calc R . . C20 C -0.2017(2) 0.0417(2) 0.06396(18) 0.0197(6) Uani 1 1 d . . . C21 C -0.3116(3) 0.0699(2) 0.0649(2) 0.0253(6) Uani 1 1 d . . . H21 H -0.3676 0.0499 0.1033 0.030 Uiso 1 1 calc R . . C22 C -0.3389(3) 0.1263(2) 0.0107(2) 0.0304(7) Uani 1 1 d . . . H22 H -0.4134 0.1452 0.0120 0.037 Uiso 1 1 calc R . . C23 C -0.2575(3) 0.1554(2) -0.0457(2) 0.0312(7) Uani 1 1 d . . . H23 H -0.2749 0.1936 -0.0843 0.037 Uiso 1 1 calc R . . C24 C -0.1503(3) 0.1266(2) -0.0434(2) 0.0285(6) Uani 1 1 d . . . H24 H -0.0932 0.1473 -0.0810 0.034 Uiso 1 1 calc R . . C25 C 0.2095(4) -0.0230(3) 0.3222(3) 0.0579(10) Uani 1 1 d . . . H25A H 0.2667 -0.0645 0.3111 0.087 Uiso 1 1 calc R . . H25B H 0.1792 -0.0138 0.2640 0.087 Uiso 1 1 calc R . . H25C H 0.1324 -0.0670 0.3385 0.087 Uiso 1 1 calc R . . C26 C 0.2864(3) 0.0933(3) 0.4031(3) 0.0417(8) Uani 1 1 d . . . H26A H 0.3207 0.0848 0.4616 0.050 Uiso 1 1 calc R . . H26B H 0.3630 0.1392 0.3864 0.050 Uiso 1 1 calc R . . C27 C 0.2595(3) 0.2563(3) 0.5038(2) 0.0446(9) Uani 1 1 d . . . H27E H 0.3298 0.3146 0.4918 0.054 Uiso 1 1 calc R . . H27F H 0.3010 0.2440 0.5578 0.054 Uiso 1 1 calc R . . C28 C 0.1562(4) 0.2980(3) 0.5286(3) 0.0642(11) Uani 1 1 d . . . H28F H 0.1968 0.3697 0.5870 0.096 Uiso 1 1 calc R . . H28G H 0.0863 0.2394 0.5394 0.096 Uiso 1 1 calc R . . H28H H 0.1175 0.3125 0.4757 0.096 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 0.0236(6) 0.0254(6) 0.0244(6) 0.0045(5) 0.0069(5) 0.0084(5) Na2 0.0311(6) 0.0307(6) 0.0295(6) 0.0152(5) 0.0037(5) 0.0055(5) P1 0.0207(4) 0.0148(3) 0.0314(4) 0.0077(3) 0.0063(3) 0.0073(3) P2 0.0181(3) 0.0191(3) 0.0230(4) 0.0097(3) 0.0090(3) 0.0078(3) Si1 0.0375(5) 0.0204(4) 0.0217(4) 0.0067(3) 0.0092(3) 0.0072(3) Si2 0.0289(4) 0.0227(4) 0.0263(4) 0.0074(3) 0.0027(3) 0.0144(3) Si3 0.0275(4) 0.0238(4) 0.0272(4) 0.0054(3) 0.0140(3) 0.0078(3) Si4 0.0298(4) 0.0185(4) 0.0286(4) 0.0105(3) 0.0132(3) 0.0076(3) O1 0.0334(12) 0.0326(11) 0.0327(12) 0.0140(10) 0.0045(9) 0.0120(10) N1 0.0316(14) 0.0202(12) 0.0315(14) 0.0062(10) 0.0039(11) 0.0147(11) N2 0.0220(12) 0.0222(12) 0.0229(12) 0.0095(10) 0.0074(10) 0.0068(10) C1 0.0192(13) 0.0142(12) 0.0243(14) 0.0074(11) 0.0058(11) 0.0063(11) C2 0.071(3) 0.045(2) 0.0316(19) 0.0128(17) -0.0041(18) 0.0165(19) C3 0.063(3) 0.059(2) 0.047(2) 0.0065(19) 0.035(2) 0.016(2) C4 0.060(2) 0.0257(17) 0.0369(19) 0.0066(15) 0.0031(17) 0.0081(16) C5 0.0296(18) 0.041(2) 0.054(2) 0.0082(17) 0.0004(16) 0.0148(15) C6 0.047(2) 0.0311(17) 0.046(2) 0.0179(15) 0.0031(16) 0.0206(15) C7 0.059(2) 0.051(2) 0.0276(17) 0.0142(16) 0.0066(16) 0.0299(18) C8 0.0259(15) 0.0231(14) 0.0160(13) 0.0068(11) 0.0052(11) 0.0114(12) C9 0.0265(15) 0.0273(15) 0.0254(15) 0.0092(12) 0.0053(12) 0.0120(13) C10 0.0240(16) 0.0416(19) 0.0356(18) 0.0113(15) 0.0052(13) 0.0127(14) C11 0.0344(19) 0.051(2) 0.043(2) 0.0108(16) 0.0084(15) 0.0291(17) C12 0.0427(19) 0.0301(16) 0.0349(18) 0.0058(14) 0.0034(14) 0.0238(15) C13 0.0192(13) 0.0187(13) 0.0234(14) 0.0080(11) 0.0089(11) 0.0063(11) C14 0.0362(18) 0.0262(16) 0.0384(18) 0.0051(14) 0.0086(14) 0.0130(14) C15 0.043(2) 0.041(2) 0.062(2) 0.0018(18) 0.0359(19) 0.0083(17) C16 0.056(2) 0.0383(19) 0.0274(17) 0.0131(15) 0.0084(16) 0.0086(17) C17 0.049(2) 0.0267(16) 0.049(2) 0.0175(15) 0.0268(17) 0.0058(15) C18 0.051(2) 0.0397(19) 0.047(2) 0.0225(16) 0.0182(17) 0.0270(17) C19 0.049(2) 0.0250(16) 0.0345(18) 0.0039(14) 0.0089(16) 0.0058(15) C20 0.0177(13) 0.0139(12) 0.0205(13) 0.0042(11) 0.0041(11) 0.0018(10) C21 0.0230(14) 0.0208(14) 0.0314(16) 0.0098(12) 0.0087(12) 0.0088(12) C22 0.0233(15) 0.0229(15) 0.0420(18) 0.0108(13) 0.0042(13) 0.0102(12) C23 0.0375(18) 0.0241(15) 0.0312(16) 0.0146(13) 0.0034(13) 0.0108(13) C24 0.0312(16) 0.0249(15) 0.0244(15) 0.0106(12) 0.0081(12) 0.0055(13) C25 0.053(2) 0.043(2) 0.075(3) 0.014(2) 0.020(2) 0.0256(19) C26 0.0327(18) 0.051(2) 0.052(2) 0.0301(18) 0.0132(16) 0.0196(16) C27 0.047(2) 0.0327(18) 0.040(2) 0.0142(16) -0.0021(16) 0.0064(16) C28 0.069(3) 0.045(2) 0.056(3) 0.0006(19) 0.013(2) 0.018(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 Na1 Na1 3.356(2) 2 ? Na1 Na2 3.3878(16) . ? Na1 P1 2.9638(13) . ? Na1 P2 2.8701(13) 2 ? Na1 N1 2.485(3) . ? Na1 N2 2.425(2) . ? Na1 N2 2.654(2) 2 ? Na1 C8 2.944(3) . ? Na1 C20 3.029(3) 2 ? Na2 P1 2.8195(13) . ? Na2 P2 2.9356(13) . ? Na2 O1 2.346(2) . ? Na2 N1 2.619(3) . ? Na2 C8 3.104(3) . ? P1 C1 1.870(2) . ? P1 C8 1.786(3) . ? P2 Na1 2.8701(13) 2 ? P2 C13 1.885(3) . ? P2 C20 1.806(3) . ? Si1 C1 1.868(3) . ? Si1 C2 1.868(4) . ? Si1 C3 1.857(4) . ? Si1 C4 1.874(3) . ? Si2 C1 1.878(3) . ? Si2 C5 1.865(3) . ? Si2 C6 1.876(3) . ? Si2 C7 1.872(3) . ? Si3 C13 1.870(3) . ? Si3 C14 1.878(3) . ? Si3 C15 1.875(3) . ? Si3 C16 1.869(3) . ? Si4 C13 1.880(3) . ? Si4 C17 1.880(3) . ? Si4 C18 1.871(3) . ? Si4 C19 1.871(3) . ? O1 C26 1.438(4) . ? O1 C27 1.423(4) . ? N1 C8 1.379(3) . ? N1 C12 1.335(4) . ? N2 Na1 2.654(2) 2 ? N2 C20 1.373(3) . ? N2 C24 1.338(4) . ? C1 H1 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.409(4) . ? C9 H9 0.950 . ? C9 C10 1.367(4) . ? C10 H10 0.950 . ? C10 C11 1.392(5) . ? C11 H11 0.950 . ? C11 C12 1.372(5) . ? C12 H12 0.950 . ? C13 H13 1.000 . ? 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 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 Na1 3.029(3) 2 ? C20 C21 1.404(4) . ? C21 H21 0.950 . ? C21 C22 1.375(4) . ? C22 H22 0.950 . ? C22 C23 1.387(4) . ? C23 H23 0.950 . ? C23 C24 1.378(4) . ? C24 H24 0.950 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C25 C26 1.496(5) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27E 0.990 . ? C27 H27F 0.990 . ? C27 C28 1.486(5) . ? C28 H28F 0.980 . ? C28 H28G 0.980 . ? C28 H28H 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 Na1 Na1 Na2 94.37(5) 2 . ? Na1 Na1 P1 137.50(5) 2 . ? Na1 Na1 P2 70.32(4) 2 2 ? Na1 Na1 N1 124.86(8) 2 . ? Na1 Na1 N2 51.64(6) 2 . ? Na1 Na1 N2 45.77(5) 2 2 ? Na1 Na1 C8 149.66(8) 2 . ? Na1 Na1 C20 63.31(6) 2 2 ? Na2 Na1 P1 52.19(3) . . ? Na2 Na1 P2 154.86(5) . 2 ? Na2 Na1 N1 50.13(6) . . ? Na2 Na1 N2 87.97(6) . . ? Na2 Na1 N2 97.40(6) . 2 ? Na2 Na1 C8 58.21(6) . . ? Na2 Na1 C20 119.98(6) . 2 ? P1 Na1 P2 150.01(4) . 2 ? P1 Na1 N1 57.11(6) . . ? P1 Na1 N2 96.59(6) . . ? P1 Na1 N2 145.84(7) . 2 ? P1 Na1 C8 35.20(5) . . ? P1 Na1 C20 151.82(6) . 2 ? P2 Na1 N1 122.46(7) 2 . ? P2 Na1 N2 96.94(6) 2 . ? P2 Na1 N2 57.56(5) 2 2 ? P2 Na1 C8 129.16(7) 2 . ? P2 Na1 C20 35.53(5) 2 2 ? N1 Na1 N2 137.91(9) . . ? N1 Na1 N2 92.56(8) . 2 ? N1 Na1 C8 27.82(7) . . ? N1 Na1 C20 96.28(8) . 2 ? N2 Na1 N2 97.41(8) . 2 ? N2 Na1 C8 130.99(8) . . ? N2 Na1 C8 119.48(8) 2 . ? N2 Na1 C20 110.73(8) . 2 ? N2 Na1 C20 26.94(7) 2 2 ? C8 Na1 C20 116.64(8) . 2 ? Na1 Na2 P1 56.14(3) . . ? Na1 Na2 P2 69.14(3) . . ? Na1 Na2 O1 142.23(7) . . ? Na1 Na2 N1 46.74(6) . . ? Na1 Na2 C8 53.72(5) . . ? P1 Na2 P2 108.17(4) . . ? P1 Na2 O1 121.72(7) . . ? P1 Na2 N1 57.90(5) . . ? P1 Na2 C8 34.68(5) . . ? P2 Na2 O1 130.05(7) . . ? P2 Na2 N1 111.31(7) . . ? P2 Na2 C8 122.55(6) . . ? O1 Na2 N1 97.72(8) . . ? O1 Na2 C8 101.49(8) . . ? N1 Na2 C8 26.17(7) . . ? Na1 P1 Na2 71.67(4) . . ? Na1 P1 C1 135.74(9) . . ? Na1 P1 C8 71.80(9) . . ? Na2 P1 C1 152.58(9) . . ? Na2 P1 C8 81.42(9) . . ? C1 P1 C8 105.92(12) . . ? Na1 P2 Na2 116.88(4) 2 . ? Na1 P2 C13 128.18(9) 2 . ? Na1 P2 C20 77.06(9) 2 . ? Na2 P2 C13 113.36(9) . . ? Na2 P2 C20 102.97(8) . . ? C13 P2 C20 103.61(12) . . ? C1 Si1 C2 111.28(15) . . ? C1 Si1 C3 110.10(15) . . ? C1 Si1 C4 111.74(14) . . ? C2 Si1 C3 109.0(2) . . ? C2 Si1 C4 105.44(17) . . ? C3 Si1 C4 109.20(18) . . ? C1 Si2 C5 111.92(14) . . ? C1 Si2 C6 111.21(13) . . ? C1 Si2 C7 107.79(14) . . ? C5 Si2 C6 107.91(16) . . ? C5 Si2 C7 110.31(17) . . ? C6 Si2 C7 107.62(16) . . ? C13 Si3 C14 112.42(13) . . ? C13 Si3 C15 109.45(14) . . ? C13 Si3 C16 111.13(14) . . ? C14 Si3 C15 106.67(15) . . ? C14 Si3 C16 107.42(15) . . ? C15 Si3 C16 109.62(18) . . ? C13 Si4 C17 112.12(13) . . ? C13 Si4 C18 111.85(14) . . ? C13 Si4 C19 108.65(14) . . ? C17 Si4 C18 107.02(16) . . ? C17 Si4 C19 106.66(16) . . ? C18 Si4 C19 110.42(16) . . ? Na2 O1 C26 111.76(18) . . ? Na2 O1 C27 119.03(18) . . ? C26 O1 C27 112.2(2) . . ? Na1 N1 Na2 83.13(8) . . ? Na1 N1 C8 94.95(16) . . ? Na1 N1 C12 117.41(19) . . ? Na2 N1 C8 96.97(16) . . ? Na2 N1 C12 135.1(2) . . ? C8 N1 C12 118.4(3) . . ? Na1 N2 Na1 82.59(8) . 2 ? Na1 N2 C20 122.12(17) . . ? Na1 N2 C20 91.96(15) 2 . ? Na1 N2 C24 109.65(17) . . ? Na1 N2 C24 126.59(18) 2 . ? C20 N2 C24 118.9(2) . . ? P1 C1 Si1 112.11(13) . . ? P1 C1 Si2 106.61(13) . . ? P1 C1 H1 106.2 . . ? Si1 C1 Si2 118.73(14) . . ? Si1 C1 H1 106.2 . . ? Si2 C1 H1 106.2 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 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 . . ? Na1 C8 Na2 68.06(6) . . ? Na1 C8 P1 73.00(9) . . ? Na1 C8 N1 57.23(14) . . ? Na1 C8 C9 135.10(18) . . ? Na2 C8 P1 63.90(8) . . ? Na2 C8 N1 56.86(14) . . ? Na2 C8 C9 153.32(19) . . ? P1 C8 N1 112.26(19) . . ? P1 C8 C9 128.5(2) . . ? N1 C8 C9 119.2(2) . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.5(3) . . ? H9 C9 C10 119.7 . . ? C9 C10 H10 120.1 . . ? C9 C10 C11 119.8(3) . . ? H10 C10 C11 120.1 . . ? C10 C11 H11 121.3 . . ? C10 C11 C12 117.4(3) . . ? H11 C11 C12 121.3 . . ? N1 C12 C11 124.7(3) . . ? N1 C12 H12 117.7 . . ? C11 C12 H12 117.7 . . ? P2 C13 Si3 113.40(13) . . ? P2 C13 Si4 106.71(13) . . ? P2 C13 H13 105.5 . . ? Si3 C13 Si4 119.21(14) . . ? Si3 C13 H13 105.5 . . ? Si4 C13 H13 105.5 . . ? 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 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? Si3 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 . . ? Si4 C19 H19A 109.5 . . ? Si4 C19 H19B 109.5 . . ? Si4 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Na1 C20 P2 67.42(8) 2 . ? Na1 C20 N2 61.11(13) 2 . ? Na1 C20 C21 140.33(18) 2 . ? P2 C20 N2 113.29(19) . . ? P2 C20 C21 127.7(2) . . ? N2 C20 C21 119.0(2) . . ? C20 C21 H21 119.7 . . ? C20 C21 C22 120.7(3) . . ? H21 C21 C22 119.7 . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.8(3) . . ? H22 C22 C23 120.1 . . ? C22 C23 H23 121.4 . . ? C22 C23 C24 117.2(3) . . ? H23 C23 C24 121.4 . . ? N2 C24 C23 124.4(3) . . ? N2 C24 H24 117.8 . . ? C23 C24 H24 117.8 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25A C25 C26 109.5 . . ? H25B C25 H25C 109.5 . . ? H25B C25 C26 109.5 . . ? H25C C25 C26 109.5 . . ? O1 C26 C25 108.4(3) . . ? O1 C26 H26A 110.0 . . ? O1 C26 H26B 110.0 . . ? C25 C26 H26A 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O1 C27 H27E 109.9 . . ? O1 C27 H27F 109.9 . . ? O1 C27 C28 109.1(3) . . ? H27E C27 H27F 108.3 . . ? H27E C27 C28 109.9 . . ? H27F C27 C28 109.9 . . ? C27 C28 H28F 109.5 . . ? C27 C28 H28G 109.5 . . ? C27 C28 H28H 109.5 . . ? H28F C28 H28G 109.5 . . ? H28F C28 H28H 109.5 . . ? H28G C28 H28H 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.381 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.057 #===END data_ki273_compound_12 _database_code_depnum_ccdc_archive 'CCDC 622829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H92 K2 N8 P2 Si4' _chemical_formula_sum 'C42 H92 K2 N8 P2 Si4' _chemical_formula_weight 961.74 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' 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' P P 0.1023 0.0942 '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' _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 14.603(2) _cell_length_b 10.0903(14) _cell_length_c 23.551(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.270(6) _cell_angle_gamma 90.00 _cell_volume 2934.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6218 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.905 _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 25376 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7075 _reflns_number_gt 5611 _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^)+(0.0463P)^2^+1.7605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7075 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.41035(4) 0.55099(4) 0.40632(2) 0.02988(11) Uani 1 1 d . . . P1 P 0.27159(4) 0.40761(5) 0.46665(2) 0.02742(12) Uani 1 1 d . A . Si1 Si 0.02212(5) 0.45636(8) 0.37276(3) 0.04355(17) Uani 1 1 d . . . Si2 Si 0.12086(5) 0.19160(6) 0.46030(3) 0.03835(15) Uani 1 1 d . . . N1 N 0.40612(12) 0.61119(16) 0.52416(8) 0.0271(3) Uani 1 1 d . . . N2 N 0.29153(15) 0.39372(19) 0.28472(9) 0.0393(4) Uani 1 1 d . A . N3 N 0.42860(17) 0.61490(18) 0.29102(10) 0.0430(5) Uani 1 1 d . . . N4 N 0.39759(15) 0.82096(17) 0.37015(9) 0.0390(4) Uani 1 1 d . . . C1 C 0.13278(15) 0.3746(2) 0.45095(9) 0.0294(4) Uani 1 1 d . . . H1A H 0.1320 0.4174 0.4890 0.035 Uiso 1 1 calc R . . C2 C -0.0122(2) 0.3511(4) 0.29816(12) 0.0681(9) Uani 1 1 d . . . H2A H 0.0547 0.3222 0.3017 0.102 Uiso 1 1 calc R . . H2B H -0.0559 0.4028 0.2569 0.102 Uiso 1 1 calc R . . H2C H -0.0534 0.2733 0.2970 0.102 Uiso 1 1 calc R . . C3 C 0.0580(2) 0.6254(3) 0.35834(14) 0.0591(7) Uani 1 1 d . . . H3A H 0.0626 0.6867 0.3921 0.089 Uiso 1 1 calc R . . H3B H 0.0021 0.6562 0.3134 0.089 Uiso 1 1 calc R . . H3C H 0.1280 0.6221 0.3620 0.089 Uiso 1 1 calc R . . C4 C -0.1028(2) 0.4774(4) 0.37612(16) 0.0723(10) Uani 1 1 d . . . H4A H -0.0864 0.5348 0.4140 0.108 Uiso 1 1 calc R . . H4B H -0.1269 0.3906 0.3819 0.108 Uiso 1 1 calc R . . H4C H -0.1603 0.5178 0.3342 0.108 Uiso 1 1 calc R . . C5 C -0.0207(2) 0.1419(3) 0.43282(14) 0.0609(8) Uani 1 1 d . . . H5A H -0.0235 0.0459 0.4380 0.091 Uiso 1 1 calc R . . H5B H -0.0701 0.1662 0.3856 0.091 Uiso 1 1 calc R . . H5C H -0.0424 0.1877 0.4605 0.091 Uiso 1 1 calc R . . C6 C 0.1648(3) 0.0889(3) 0.41324(17) 0.0715(9) Uani 1 1 d . . . H6A H 0.1635 -0.0050 0.4235 0.107 Uiso 1 1 calc R . . H6B H 0.2385 0.1140 0.4266 0.107 Uiso 1 1 calc R . . H6C H 0.1154 0.1036 0.3649 0.107 Uiso 1 1 calc R . . C7 C 0.2077(2) 0.1485(3) 0.55131(13) 0.0534(6) Uani 1 1 d . . . H7A H 0.2023 0.0533 0.5572 0.080 Uiso 1 1 calc R . . H7B H 0.1831 0.1981 0.5766 0.080 Uiso 1 1 calc R . . H7C H 0.2831 0.1716 0.5680 0.080 Uiso 1 1 calc R . . C8 C 0.30745(14) 0.56265(18) 0.50936(8) 0.0241(4) Uani 1 1 d . . . C9 C 0.24834(16) 0.6365(2) 0.53086(10) 0.0330(4) Uani 1 1 d . A . H9A H 0.1790 0.6064 0.5198 0.040 Uiso 1 1 calc R . . C10 C 0.29002(19) 0.7503(2) 0.56729(12) 0.0409(5) Uani 1 1 d . . . H10A H 0.2502 0.7979 0.5820 0.049 Uiso 1 1 calc R A . C11 C 0.39065(19) 0.7966(2) 0.58294(12) 0.0420(5) Uani 1 1 d . A . H11A H 0.4216 0.8748 0.6087 0.050 Uiso 1 1 calc R . . C12 C 0.44322(16) 0.7235(2) 0.55937(10) 0.0331(4) Uani 1 1 d . . . H12A H 0.5112 0.7554 0.5689 0.040 Uiso 1 1 calc R A . C13 C 0.1903(2) 0.4655(3) 0.25542(18) 0.0707(9) Uani 1 1 d . . . H13A H 0.1592 0.4525 0.2830 0.106 Uiso 1 1 calc R . . H13B H 0.1397 0.4324 0.2099 0.106 Uiso 1 1 calc R . . H13C H 0.2035 0.5601 0.2535 0.106 Uiso 1 1 calc R . . C14 C 0.2740(2) 0.2560(3) 0.29515(13) 0.0552(6) Uani 1 1 d . . . H14A H 0.3417 0.2063 0.3130 0.083 Uiso 1 1 calc R . . H14B H 0.2180 0.2171 0.2523 0.083 Uiso 1 1 calc R . . H14C H 0.2506 0.2520 0.3271 0.083 Uiso 1 1 calc R . . C15 C 0.3382(2) 0.3985(3) 0.24342(11) 0.0505(6) Uani 1 1 d . . . H15A H 0.2879 0.3549 0.1999 0.061 Uiso 1 1 calc R A . H15B H 0.4068 0.3476 0.2660 0.061 Uiso 1 1 calc R . . C16 C 0.3608(2) 0.5368(3) 0.23026(11) 0.0541(7) Uani 1 1 d . A . H16A H 0.3968 0.5315 0.2047 0.065 Uiso 1 1 calc R . . H16B H 0.2910 0.5834 0.2018 0.065 Uiso 1 1 calc R . . C17 C 0.5409(2) 0.5710(3) 0.32415(12) 0.0508(6) Uani 1 1 d . A . H17A H 0.5447 0.4752 0.3321 0.076 Uiso 1 1 calc R . . H17B H 0.5846 0.6172 0.3672 0.076 Uiso 1 1 calc R . . H17C H 0.5690 0.5910 0.2955 0.076 Uiso 1 1 calc R . . C18 C 0.4060(4) 0.7522(4) 0.2686(2) 0.0365(9) Uani 0.677(7) 1 d P A 1 H18A H 0.3269 0.7642 0.2376 0.044 Uiso 0.677(7) 1 calc PR A 1 H18B H 0.4413 0.7736 0.2437 0.044 Uiso 0.677(7) 1 calc PR A 1 C18A C 0.4582(9) 0.7687(9) 0.3000(5) 0.041(2) Uani 0.323(7) 1 d P A 2 H18C H 0.5310 0.7831 0.3406 0.049 Uiso 0.323(7) 1 calc PR A 2 H18D H 0.4581 0.8025 0.2605 0.049 Uiso 0.323(7) 1 calc PR A 2 C19 C 0.4467(4) 0.8461(3) 0.32752(18) 0.0369(10) Uani 0.677(7) 1 d P A 1 H19A H 0.4300 0.9381 0.3104 0.044 Uiso 0.677(7) 1 calc PR A 1 H19B H 0.5265 0.8378 0.3566 0.044 Uiso 0.677(7) 1 calc PR A 1 C19A C 0.3742(9) 0.8394(8) 0.3068(4) 0.047(2) Uani 0.323(7) 1 d P A 2 H19C H 0.3746 0.9352 0.2978 0.057 Uiso 0.323(7) 1 calc PR A 2 H19D H 0.3013 0.8037 0.2741 0.057 Uiso 0.323(7) 1 calc PR A 2 C20 C 0.2865(3) 0.8488(4) 0.3325(3) 0.0528(12) Uani 0.677(7) 1 d P A 1 H20A H 0.2504 0.7904 0.2932 0.079 Uiso 0.677(7) 1 calc PR A 1 H20B H 0.2753 0.9414 0.3177 0.079 Uiso 0.677(7) 1 calc PR A 1 H20C H 0.2560 0.8341 0.3603 0.079 Uiso 0.677(7) 1 calc PR A 1 C20A C 0.2936(9) 0.8671(11) 0.3731(7) 0.072(4) Uani 0.323(7) 1 d P A 2 H20D H 0.3051 0.8431 0.4168 0.107 Uiso 0.323(7) 1 calc PR A 2 H20E H 0.2284 0.8228 0.3373 0.107 Uiso 0.323(7) 1 calc PR A 2 H20F H 0.2846 0.9634 0.3670 0.107 Uiso 0.323(7) 1 calc PR A 2 C21 C 0.4640(3) 0.8989(3) 0.42867(15) 0.0729(9) Uani 1 1 d . A . H21A H 0.5398 0.8718 0.4495 0.109 Uiso 1 1 calc R . . H21B H 0.4413 0.8859 0.4606 0.109 Uiso 1 1 calc R . . H21C H 0.4567 0.9927 0.4161 0.109 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 0.0429(2) 0.0272(2) 0.0267(2) 0.00201(16) 0.02344(19) 0.00270(17) P1 0.0265(2) 0.0318(3) 0.0273(2) -0.00581(19) 0.0166(2) -0.0077(2) Si1 0.0267(3) 0.0701(5) 0.0310(3) 0.0132(3) 0.0135(2) -0.0052(3) Si2 0.0381(3) 0.0414(3) 0.0357(3) -0.0049(2) 0.0198(3) -0.0172(3) N1 0.0252(7) 0.0328(9) 0.0255(8) -0.0037(6) 0.0151(6) -0.0052(6) N2 0.0381(9) 0.0492(11) 0.0320(9) -0.0012(8) 0.0198(8) -0.0035(8) N3 0.0673(13) 0.0357(10) 0.0476(11) 0.0087(8) 0.0451(11) 0.0064(9) N4 0.0470(10) 0.0286(9) 0.0385(10) 0.0003(7) 0.0210(9) 0.0008(8) C1 0.0265(9) 0.0395(11) 0.0240(9) -0.0010(8) 0.0145(8) -0.0085(8) C2 0.0503(15) 0.114(3) 0.0304(12) -0.0020(14) 0.0151(11) -0.0332(16) C3 0.0464(14) 0.0699(18) 0.0535(15) 0.0294(13) 0.0216(12) 0.0049(13) C4 0.0391(14) 0.112(3) 0.0723(19) 0.0379(19) 0.0341(14) 0.0159(15) C5 0.0461(14) 0.0749(19) 0.0515(15) 0.0042(13) 0.0192(12) -0.0318(13) C6 0.100(2) 0.0506(16) 0.089(2) -0.0228(15) 0.067(2) -0.0251(16) C7 0.0469(14) 0.0497(14) 0.0519(15) 0.0143(12) 0.0186(12) -0.0080(11) C8 0.0231(8) 0.0298(9) 0.0204(8) 0.0014(7) 0.0123(7) -0.0016(7) C9 0.0292(10) 0.0380(11) 0.0382(11) -0.0024(8) 0.0225(9) -0.0027(8) C10 0.0457(12) 0.0374(12) 0.0538(13) -0.0078(10) 0.0361(11) -0.0016(10) C11 0.0519(13) 0.0341(11) 0.0491(13) -0.0148(10) 0.0330(11) -0.0128(10) C12 0.0329(10) 0.0354(11) 0.0341(10) -0.0052(8) 0.0200(9) -0.0102(8) C13 0.0507(16) 0.075(2) 0.097(2) 0.0238(18) 0.0466(17) 0.0082(14) C14 0.0557(15) 0.0499(15) 0.0503(14) -0.0105(12) 0.0217(12) -0.0163(12) C15 0.0503(14) 0.0746(18) 0.0306(11) -0.0169(11) 0.0242(11) -0.0138(13) C16 0.0521(14) 0.087(2) 0.0313(11) 0.0132(12) 0.0280(11) 0.0055(13) C17 0.0585(15) 0.0538(15) 0.0364(12) -0.0016(10) 0.0230(12) -0.0093(12) C18 0.048(2) 0.0363(18) 0.029(2) 0.0044(16) 0.0232(18) -0.0045(17) C18A 0.049(5) 0.043(5) 0.036(5) 0.013(4) 0.027(4) 0.003(4) C19 0.041(2) 0.0326(17) 0.0413(19) 0.0005(14) 0.0249(18) -0.0097(15) C19A 0.054(6) 0.038(4) 0.056(5) 0.020(3) 0.033(5) 0.011(4) C20 0.045(2) 0.047(2) 0.071(3) -0.009(2) 0.034(2) -0.0026(16) C20A 0.075(7) 0.077(7) 0.090(8) 0.026(6) 0.062(7) 0.039(6) C21 0.100(2) 0.0562(17) 0.0538(16) -0.0097(14) 0.0356(17) -0.0325(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 2.8029(17) 3_666 ? K1 N4 2.8305(19) . ? K1 N1 2.8737(16) . ? K1 N2 2.9023(19) . ? K1 N3 2.9382(17) . ? K1 C12 3.324(2) 3_666 ? K1 P1 3.3605(7) . ? K1 C8 3.4721(18) . ? K1 K1 3.8793(10) 3_666 ? P1 C8 1.7807(19) . ? P1 C1 1.8858(19) . ? Si1 C3 1.868(3) . ? Si1 C1 1.872(2) . ? Si1 C2 1.878(3) . ? Si1 C4 1.880(3) . ? Si2 C6 1.864(3) . ? Si2 C7 1.868(3) . ? Si2 C5 1.875(2) . ? Si2 C1 1.879(2) . ? N1 C12 1.336(2) . ? N1 C8 1.379(2) . ? N1 K1 2.8029(17) 3_666 ? N2 C13 1.448(3) . ? N2 C15 1.457(3) . ? N2 C14 1.457(3) . ? N3 C18 1.457(4) . ? N3 C17 1.459(3) . ? N3 C16 1.462(3) . ? N3 C18A 1.595(9) . ? N4 C19A 1.353(8) . ? N4 C20 1.401(4) . ? N4 C21 1.425(3) . ? N4 C19 1.535(4) . ? N4 C20A 1.625(9) . ? C1 H1A 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.423(3) . ? C9 C10 1.366(3) . ? C9 H9A 0.950 . ? C10 C11 1.391(3) . ? C10 H10A 0.950 . ? C11 C12 1.377(3) . ? C11 H11A 0.950 . ? C12 K1 3.324(2) 3_666 ? C12 H12A 0.950 . ? 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 C16 1.503(4) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 C19 1.515(6) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C18A C19A 1.499(13) . ? C18A H18C 0.990 . ? C18A H18D 0.990 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C19A H19C 0.990 . ? C19A H19D 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C20A H20D 0.980 . ? C20A H20E 0.980 . ? C20A H20F 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 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 N4 128.79(5) 3_666 . ? N1 K1 N1 93.79(4) 3_666 . ? N4 K1 N1 93.17(5) . . ? N1 K1 N2 97.97(5) 3_666 . ? N4 K1 N2 108.70(5) . . ? N1 K1 N2 139.34(5) . . ? N1 K1 N3 97.92(5) 3_666 . ? N4 K1 N3 62.26(5) . . ? N1 K1 N3 154.88(5) . . ? N2 K1 N3 60.63(5) . . ? N1 K1 C12 23.25(5) 3_666 3_666 ? N4 K1 C12 143.65(5) . 3_666 ? N1 K1 C12 106.50(5) . 3_666 ? N2 K1 C12 75.67(5) . 3_666 ? N3 K1 C12 92.50(5) . 3_666 ? N1 K1 P1 96.08(4) 3_666 . ? N4 K1 P1 125.73(4) . . ? N1 K1 P1 49.75(3) . . ? N2 K1 P1 90.23(4) . . ? N3 K1 P1 149.09(5) . . ? C12 K1 P1 89.62(4) 3_666 . ? N1 K1 C8 104.31(4) 3_666 . ? N4 K1 C8 101.20(5) . . ? N1 K1 C8 22.68(4) . . ? N2 K1 C8 117.02(5) . . ? N3 K1 C8 157.69(5) . . ? C12 K1 C8 108.70(5) 3_666 . ? P1 K1 C8 30.16(3) . . ? N1 K1 K1 47.66(3) 3_666 3_666 ? N4 K1 K1 119.58(4) . 3_666 ? N1 K1 K1 46.13(3) . 3_666 ? N2 K1 K1 131.46(4) . 3_666 ? N3 K1 K1 140.38(5) . 3_666 ? C12 K1 K1 63.04(4) 3_666 3_666 ? P1 K1 K1 66.294(17) . 3_666 ? C8 K1 K1 59.67(3) . 3_666 ? C8 P1 C1 103.13(9) . . ? C8 P1 K1 78.39(6) . . ? C1 P1 K1 145.17(6) . . ? C3 Si1 C1 113.75(10) . . ? C3 Si1 C2 107.91(13) . . ? C1 Si1 C2 109.27(13) . . ? C3 Si1 C4 106.07(15) . . ? C1 Si1 C4 110.84(11) . . ? C2 Si1 C4 108.84(15) . . ? C6 Si2 C7 108.35(15) . . ? C6 Si2 C5 108.19(15) . . ? C7 Si2 C5 106.36(12) . . ? C6 Si2 C1 113.21(11) . . ? C7 Si2 C1 108.33(10) . . ? C5 Si2 C1 112.11(12) . . ? C12 N1 C8 118.73(16) . . ? C12 N1 K1 100.84(12) . 3_666 ? C8 N1 K1 118.98(12) . 3_666 ? C12 N1 K1 124.62(12) . . ? C8 N1 K1 103.84(10) . . ? K1 N1 K1 86.21(4) 3_666 . ? C13 N2 C15 112.8(2) . . ? C13 N2 C14 109.3(2) . . ? C15 N2 C14 109.3(2) . . ? C13 N2 K1 96.74(17) . . ? C15 N2 K1 113.21(13) . . ? C14 N2 K1 114.92(14) . . ? C18 N3 C17 117.1(3) . . ? C18 N3 C16 104.7(3) . . ? C17 N3 C16 109.90(19) . . ? C18 N3 C18A 27.8(3) . . ? C17 N3 C18A 94.4(4) . . ? C16 N3 C18A 130.5(4) . . ? C18 N3 K1 115.39(17) . . ? C17 N3 K1 94.01(13) . . ? C16 N3 K1 115.97(13) . . ? C18A N3 K1 104.0(3) . . ? C19A N4 C20 75.5(5) . . ? C19A N4 C21 129.1(5) . . ? C20 N4 C21 117.5(3) . . ? C19A N4 C19 35.7(4) . . ? C20 N4 C19 110.0(3) . . ? C21 N4 C19 103.1(2) . . ? C19A N4 C20A 108.4(6) . . ? C20 N4 C20A 34.5(4) . . ? C21 N4 C20A 88.3(6) . . ? C19 N4 C20A 139.0(4) . . ? C19A N4 K1 113.7(4) . . ? C20 N4 K1 104.6(2) . . ? C21 N4 K1 109.80(16) . . ? C19 N4 K1 112.15(16) . . ? C20A N4 K1 100.1(4) . . ? Si1 C1 Si2 117.59(10) . . ? Si1 C1 P1 112.83(10) . . ? Si2 C1 P1 107.93(10) . . ? Si1 C1 H1A 105.9 . . ? Si2 C1 H1A 105.9 . . ? P1 C1 H1A 105.9 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 118.34(17) . . ? N1 C8 P1 114.03(13) . . ? C9 C8 P1 127.59(14) . . ? N1 C8 K1 53.48(9) . . ? C9 C8 K1 146.91(13) . . ? P1 C8 K1 71.45(6) . . ? C10 C9 C8 120.81(18) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 120.13(19) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 116.80(19) . . ? C12 C11 H11A 121.6 . . ? C10 C11 H11A 121.6 . . ? N1 C12 C11 125.15(18) . . ? N1 C12 K1 55.91(10) . 3_666 ? C11 C12 K1 140.61(15) . 3_666 ? N1 C12 H12A 117.4 . . ? C11 C12 H12A 117.4 . . ? K1 C12 H12A 76.7 3_666 . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 113.6(2) . . ? N2 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N2 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N3 C16 C15 114.03(18) . . ? N3 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? N3 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C19 111.1(3) . . ? N3 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N3 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C19A C18A N3 107.4(7) . . ? C19A C18A H18C 110.2 . . ? N3 C18A H18C 110.2 . . ? C19A C18A H18D 110.2 . . ? N3 C18A H18D 110.2 . . ? H18C C18A H18D 108.5 . . ? C18 C19 N4 113.8(3) . . ? C18 C19 H19A 108.8 . . ? N4 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? N4 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N4 C19A C18A 108.2(8) . . ? N4 C19A H19C 110.1 . . ? C18A C19A H19C 110.1 . . ? N4 C19A H19D 110.1 . . ? C18A C19A H19D 110.1 . . ? H19C C19A H19D 108.4 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? N4 C20A H20D 109.5 . . ? N4 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? N4 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.450 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.053 #===END