# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1410 # Combined CIF for three structures in manuscript # Monomeric alkali metal complexes of a sterically demanding, # donor-functionalized secondary phosphide ligand # by W.Clegg, S.Doherty, K.Izod, H.Kagerer, P.O'Shaughnessy and J.M.Sheffield # submitted to J.Chem.Soc.Dalton Trans. on 1 February 1999 # CIF supplied by W. Clegg data_compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H47 Li N O2 P Si2' _chemical_formula_weight 475.72 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' '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' '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 11.0847(15) _cell_length_b 15.223(2) _cell_length_c 17.755(3) _cell_angle_alpha 95.503(3) _cell_angle_beta 90.037(4) _cell_angle_gamma 99.812(4) _cell_volume 2938.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 7537 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 27.96 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.589 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20997 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.1608 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.39 _reflns_number_total 12641 _reflns_number_gt 5664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material '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 w=1/[\s^2^(Fo^2^)+(0.1229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12641 _refine_ls_number_parameters 671 _refine_ls_number_restraints 343 _refine_ls_R_factor_all 0.1819 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.2450 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.1773(7) 0.1791(5) 0.6133(4) 0.0390(19) Uani 1 d . . . Li2 Li 0.6111(7) 0.8138(5) -0.1072(4) 0.0389(19) Uani 1 d . . . P1 P 0.05644(11) 0.21448(8) 0.50220(7) 0.0332(3) Uani 1 d . . . P2 P 0.47122(10) 0.77944(8) 0.00297(7) 0.0311(3) Uani 1 d . . . Si1 Si -0.13289(13) 0.30552(9) 0.59396(8) 0.0415(4) Uani 1 d . . . Si2 Si -0.10988(12) 0.31507(9) 0.41429(8) 0.0365(3) Uani 1 d . . . Si3 Si 0.23762(13) 0.71001(9) -0.09394(8) 0.0405(4) Uani 1 d . . . Si4 Si 0.23693(12) 0.69813(9) 0.08548(8) 0.0388(4) Uani 1 d . . . N1 N 0.2782(4) 0.0960(3) 0.5450(2) 0.0496(11) Uani 1 d . . . N2 N 0.7633(3) 0.8723(2) -0.0386(2) 0.0364(9) Uani 1 d . . . C1 C -0.0348(4) 0.3094(3) 0.5079(2) 0.0329(11) Uani 1 d . . . H1 H 0.0267 0.3657 0.5169 0.039 Uiso 1 calc R . . C2 C -0.1487(6) 0.4285(4) 0.4064(3) 0.0698(18) Uani 1 d . . . H2A H -0.2130 0.4390 0.4423 0.084 Uiso 1 calc R . . H2B H -0.1778 0.4320 0.3548 0.084 Uiso 1 calc R . . H2C H -0.0756 0.4741 0.4178 0.084 Uiso 1 calc R . . C3 C -0.2523(5) 0.2314(4) 0.4000(3) 0.0576(15) Uani 1 d . . . H3A H -0.2338 0.1715 0.4047 0.069 Uiso 1 calc R . . H3B H -0.2866 0.2335 0.3495 0.069 Uiso 1 calc R . . H3C H -0.3117 0.2451 0.4383 0.069 Uiso 1 calc R . . C4 C -0.0111(6) 0.2923(5) 0.3316(3) 0.081(2) Uani 1 d . . . H4A H 0.0633 0.3378 0.3343 0.098 Uiso 1 calc R . . H4B H -0.0561 0.2943 0.2845 0.098 Uiso 1 calc R . . H4C H 0.0114 0.2329 0.3328 0.098 Uiso 1 calc R . . C5 C -0.0346(5) 0.3293(4) 0.6821(3) 0.0626(16) Uani 1 d . . . H5A H 0.0072 0.2785 0.6879 0.075 Uiso 1 calc R . . H5B H -0.0861 0.3383 0.7261 0.075 Uiso 1 calc R . . H5C H 0.0262 0.3835 0.6784 0.075 Uiso 1 calc R . . C6 C -0.2312(5) 0.3946(4) 0.5983(3) 0.0646(17) Uani 1 d . . . H6A H -0.1800 0.4526 0.5922 0.078 Uiso 1 calc R . . H6B H -0.2715 0.3975 0.6474 0.078 Uiso 1 calc R . . H6C H -0.2933 0.3803 0.5577 0.078 Uiso 1 calc R . . C7 C -0.2362(5) 0.1961(4) 0.5986(3) 0.0597(16) Uani 1 d . . . H7A H -0.3016 0.1895 0.5602 0.072 Uiso 1 calc R . . H7B H -0.2723 0.1940 0.6489 0.072 Uiso 1 calc R . . H7C H -0.1893 0.1473 0.5890 0.072 Uiso 1 calc R . . C8 C 0.2045(4) 0.2651(3) 0.4688(2) 0.0310(10) Uani 1 d . . . C9 C 0.2402(4) 0.3556(3) 0.4576(3) 0.0415(12) Uani 1 d . . . H9 H 0.1814 0.3941 0.4656 0.050 Uiso 1 calc R . . C10 C 0.3567(5) 0.3923(4) 0.4354(3) 0.0511(14) Uani 1 d . . . H10 H 0.3768 0.4546 0.4302 0.061 Uiso 1 calc R . . C11 C 0.4447(5) 0.3364(4) 0.4207(3) 0.0534(15) Uani 1 d . . . H11 H 0.5246 0.3599 0.4049 0.064 Uiso 1 calc R . . C12 C 0.4119(4) 0.2477(4) 0.4298(3) 0.0466(13) Uani 1 d . . . H12 H 0.4707 0.2096 0.4198 0.056 Uiso 1 calc R . . C13 C 0.2963(4) 0.2104(3) 0.4532(3) 0.0359(11) Uani 1 d . . . C14 C 0.2672(5) 0.1128(3) 0.4652(3) 0.0447(13) Uani 1 d . . . H14A H 0.1826 0.0886 0.4467 0.054 Uiso 1 calc R . . H14B H 0.3233 0.0802 0.4347 0.054 Uiso 1 calc R . . C15 C 0.4084(7) 0.1165(5) 0.5701(3) 0.088(2) Uani 1 d . . . H15A H 0.4152 0.1020 0.6224 0.105 Uiso 1 calc R . . H15B H 0.4397 0.1803 0.5674 0.105 Uiso 1 calc R . . H15C H 0.4564 0.0807 0.5372 0.105 Uiso 1 calc R . . C16 C 0.2277(8) 0.0028(4) 0.5524(4) 0.106(3) Uani 1 d . . . H16A H 0.2726 -0.0358 0.5200 0.127 Uiso 1 calc R . . H16B H 0.1411 -0.0091 0.5370 0.127 Uiso 1 calc R . . H16C H 0.2355 -0.0095 0.6052 0.127 Uiso 1 calc R . . O4 O 0.5792(3) 0.9044(2) -0.17443(18) 0.0456(9) Uani 1 d D . . C45 C 0.5649(6) 0.8870(4) -0.2548(3) 0.0630(16) Uani 1 d DU . . H45A H 0.5052 0.8315 -0.2682 0.076 Uiso 1 calc R . . H45B H 0.6442 0.8798 -0.2781 0.076 Uiso 1 calc R . . C46 C 0.5194(7) 0.9668(5) -0.2826(3) 0.083(2) Uani 1 d DU . . H46A H 0.5880 1.0108 -0.2993 0.100 Uiso 1 calc R . . H46B H 0.4595 0.9479 -0.3249 0.100 Uiso 1 calc R . . C47 C 0.4598(6) 1.0049(4) -0.2136(3) 0.0705(18) Uani 1 d DU . . H47A H 0.4621 1.0701 -0.2144 0.085 Uiso 1 calc R . . H47B H 0.3736 0.9751 -0.2103 0.085 Uiso 1 calc R . . C48 C 0.5347(5) 0.9862(3) -0.1491(3) 0.0592(15) Uani 1 d DU . . H48A H 0.6039 1.0360 -0.1369 0.071 Uiso 1 calc R . . H48B H 0.4842 0.9782 -0.1035 0.071 Uiso 1 calc R . . O1 O 0.2875(4) 0.2737(2) 0.6717(2) 0.0604(11) Uani 1 d D . . C17 C 0.3768(8) 0.2849(6) 0.7270(5) 0.049(3) Uani 0.560(7) d PDU A 1 H17A H 0.4172 0.2316 0.7254 0.058 Uiso 0.560(7) calc PR A 1 H17B H 0.3416 0.2947 0.7777 0.058 Uiso 0.560(7) calc PR A 1 C18 C 0.4656(11) 0.3653(9) 0.7098(8) 0.105(5) Uani 0.560(7) d PDU A 1 H18A H 0.4893 0.4056 0.7565 0.126 Uiso 0.560(7) calc PR A 1 H18B H 0.5404 0.3474 0.6871 0.126 Uiso 0.560(7) calc PR A 1 C19 C 0.4024(13) 0.4105(11) 0.6560(11) 0.101(6) Uani 0.560(7) d PDU A 1 H19A H 0.4379 0.4042 0.6051 0.121 Uiso 0.560(7) calc PR A 1 H19B H 0.4091 0.4750 0.6730 0.121 Uiso 0.560(7) calc PR A 1 C20 C 0.2728(10) 0.3655(6) 0.6547(8) 0.080(4) Uani 0.560(7) d PDU A 1 H20A H 0.2336 0.3647 0.6044 0.096 Uiso 0.560(7) calc PR A 1 H20B H 0.2248 0.3942 0.6939 0.096 Uiso 0.560(7) calc PR A 1 C17A C 0.2874(11) 0.3128(6) 0.7454(5) 0.046(3) Uani 0.440(7) d PDU A 2 H17C H 0.3492 0.2932 0.7772 0.055 Uiso 0.440(7) calc PR A 2 H17D H 0.2058 0.2984 0.7682 0.055 Uiso 0.440(7) calc PR A 2 C18A C 0.3204(13) 0.4128(7) 0.7353(7) 0.065(4) Uani 0.440(7) d PDU A 2 H18C H 0.2479 0.4425 0.7423 0.078 Uiso 0.440(7) calc PR A 2 H18D H 0.3855 0.4428 0.7718 0.078 Uiso 0.440(7) calc PR A 2 C19A C 0.364(2) 0.4151(10) 0.6566(11) 0.092(6) Uani 0.440(7) d PDU A 2 H19C H 0.4360 0.4631 0.6534 0.110 Uiso 0.440(7) calc PR A 2 H19D H 0.2988 0.4250 0.6221 0.110 Uiso 0.440(7) calc PR A 2 C20A C 0.3989(11) 0.3238(9) 0.6371(8) 0.068(4) Uani 0.440(7) d PDU A 2 H20C H 0.4029 0.3079 0.5819 0.082 Uiso 0.440(7) calc PR A 2 H20D H 0.4761 0.3171 0.6623 0.082 Uiso 0.440(7) calc PR A 2 O2 O 0.0916(3) 0.1035(2) 0.6878(2) 0.0559(10) Uani 1 d . . . C21 C -0.0332(13) 0.0613(13) 0.6820(11) 0.066(4) Uani 0.61(3) d PU B 1 H21A H -0.0856 0.1072 0.6942 0.080 Uiso 0.61(3) calc PR B 1 H21B H -0.0519 0.0358 0.6291 0.080 Uiso 0.61(3) calc PR B 1 C22 C -0.0620(18) -0.0050(15) 0.7287(12) 0.082(5) Uani 0.61(3) d PU B 1 H22A H -0.0574 -0.0644 0.7020 0.098 Uiso 0.61(3) calc PR B 1 H22B H -0.1449 -0.0057 0.7496 0.098 Uiso 0.61(3) calc PR B 1 C23 C 0.0353(19) 0.0211(12) 0.7897(10) 0.069(5) Uani 0.61(3) d PU B 1 H23A H -0.0002 0.0443 0.8372 0.082 Uiso 0.61(3) calc PR B 1 H23B H 0.0729 -0.0311 0.7998 0.082 Uiso 0.61(3) calc PR B 1 C21A C -0.005(2) 0.0225(17) 0.6620(13) 0.061(5) Uani 0.39(3) d PU B 2 H21C H -0.0833 0.0412 0.6500 0.073 Uiso 0.39(3) calc PR B 2 H21D H 0.0224 -0.0112 0.6164 0.073 Uiso 0.39(3) calc PR B 2 C22A C -0.017(3) -0.0280(18) 0.721(2) 0.075(6) Uani 0.39(3) d PU B 2 H22C H -0.0226 -0.0919 0.7016 0.090 Uiso 0.39(3) calc PR B 2 H22D H -0.0940 -0.0211 0.7472 0.090 Uiso 0.39(3) calc PR B 2 C23A C 0.080(3) -0.004(2) 0.771(2) 0.076(7) Uani 0.39(3) d PU B 2 H23C H 0.1434 -0.0415 0.7596 0.092 Uiso 0.39(3) calc PR B 2 H23D H 0.0525 -0.0103 0.8235 0.092 Uiso 0.39(3) calc PR B 2 C24 C 0.1284(6) 0.0923(4) 0.7608(3) 0.0688(19) Uani 1 d . . . H24A H 0.1334 0.1491 0.7938 0.083 Uiso 1 calc R C 1 H24B H 0.2101 0.0741 0.7600 0.083 Uiso 1 calc R C 1 C25 C 0.3221(4) 0.6963(3) -0.0059(2) 0.0314(10) Uani 1 d . . . H25 H 0.3460 0.6357 -0.0139 0.038 Uiso 1 calc R . . C26 C 0.0770(5) 0.6442(4) -0.0980(3) 0.0631(17) Uani 1 d . . . H26A H 0.0801 0.5805 -0.0961 0.076 Uiso 1 calc R . . H26B H 0.0364 0.6526 -0.1452 0.076 Uiso 1 calc R . . H26C H 0.0311 0.6654 -0.0548 0.076 Uiso 1 calc R . . C27 C 0.2262(5) 0.8289(3) -0.1053(3) 0.0556(15) Uani 1 d . . . H27A H 0.1718 0.8503 -0.0668 0.067 Uiso 1 calc R . . H27B H 0.1930 0.8329 -0.1558 0.067 Uiso 1 calc R . . H27C H 0.3077 0.8659 -0.0992 0.067 Uiso 1 calc R . . C28 C 0.3153(5) 0.6665(4) -0.1800(3) 0.0625(16) Uani 1 d . . . H28A H 0.3990 0.6998 -0.1817 0.075 Uiso 1 calc R . . H28B H 0.2697 0.6742 -0.2255 0.075 Uiso 1 calc R . . H28C H 0.3179 0.6028 -0.1777 0.075 Uiso 1 calc R . . C29 C 0.3401(5) 0.7113(4) 0.1707(3) 0.0532(15) Uani 1 d . . . H29A H 0.3759 0.6570 0.1728 0.064 Uiso 1 calc R . . H29B H 0.2928 0.7210 0.2164 0.064 Uiso 1 calc R . . H29C H 0.4056 0.7628 0.1675 0.064 Uiso 1 calc R . . C30 C 0.1243(5) 0.5918(3) 0.0892(3) 0.0559(15) Uani 1 d . . . H30A H 0.0611 0.5878 0.0498 0.067 Uiso 1 calc R . . H30B H 0.0861 0.5916 0.1390 0.067 Uiso 1 calc R . . H30C H 0.1669 0.5404 0.0808 0.067 Uiso 1 calc R . . C31 C 0.1526(5) 0.7956(3) 0.0957(3) 0.0542(15) Uani 1 d . . . H31A H 0.2114 0.8516 0.0971 0.065 Uiso 1 calc R . . H31B H 0.1065 0.7945 0.1428 0.065 Uiso 1 calc R . . H31C H 0.0959 0.7915 0.0527 0.065 Uiso 1 calc R . . C32 C 0.5790(4) 0.7146(3) 0.0386(2) 0.0304(10) Uani 1 d . . . C33 C 0.5509(4) 0.6235(3) 0.0519(3) 0.0381(12) Uani 1 d . . . H33 H 0.4685 0.5938 0.0456 0.046 Uiso 1 calc R . . C34 C 0.6383(5) 0.5754(3) 0.0739(3) 0.0479(13) Uani 1 d . . . H34 H 0.6151 0.5141 0.0821 0.057 Uiso 1 calc R . . C35 C 0.7590(5) 0.6165(4) 0.0839(3) 0.0580(15) Uani 1 d . . . H35 H 0.8200 0.5835 0.0971 0.070 Uiso 1 calc R . . C36 C 0.7894(4) 0.7068(4) 0.0743(3) 0.0470(13) Uani 1 d . . . H36 H 0.8715 0.7360 0.0837 0.056 Uiso 1 calc R . . C37 C 0.7037(4) 0.7561(3) 0.0514(3) 0.0371(11) Uani 1 d . . . C38 C 0.7445(4) 0.8532(3) 0.0411(3) 0.0424(12) Uani 1 d . . . H38A H 0.6825 0.8875 0.0631 0.051 Uiso 1 calc R . . H38B H 0.8222 0.8748 0.0698 0.051 Uiso 1 calc R . . C39 C 0.7866(5) 0.9697(3) -0.0419(3) 0.0515(14) Uani 1 d . . . H39A H 0.8602 0.9961 -0.0117 0.062 Uiso 1 calc R . . H39B H 0.7164 0.9950 -0.0215 0.062 Uiso 1 calc R . . H39C H 0.7988 0.9829 -0.0945 0.062 Uiso 1 calc R . . C40 C 0.8729(4) 0.8369(3) -0.0671(3) 0.0486(14) Uani 1 d . . . H40A H 0.8877 0.8512 -0.1193 0.058 Uiso 1 calc R . . H40B H 0.8595 0.7718 -0.0656 0.058 Uiso 1 calc R . . H40C H 0.9442 0.8644 -0.0352 0.058 Uiso 1 calc R . . O3 O 0.6520(3) 0.7087(2) -0.16838(18) 0.0479(9) Uani 1 d . . . C41 C 0.645(5) 0.632(3) -0.125(2) 0.077(3) Uani 0.286(18) d PU D 1 H41A H 0.6871 0.6521 -0.0754 0.092 Uiso 0.286(18) calc PR D 1 H41B H 0.5577 0.6098 -0.1147 0.092 Uiso 0.286(18) calc PR D 1 C42 C 0.686(3) 0.5760(17) -0.1537(19) 0.078(2) Uani 0.286(18) d PU D 1 H42A H 0.6191 0.5253 -0.1673 0.093 Uiso 0.286(18) calc PR D 1 H42B H 0.7396 0.5563 -0.1162 0.093 Uiso 0.286(18) calc PR D 1 C43 C 0.751(4) 0.590(2) -0.2150(16) 0.077(2) Uani 0.286(18) d PU D 1 H43A H 0.7221 0.5440 -0.2573 0.092 Uiso 0.286(18) calc PR D 1 H43B H 0.8394 0.5902 -0.2052 0.092 Uiso 0.286(18) calc PR D 1 C41A C 0.6203(19) 0.6226(12) -0.1394(10) 0.076(2) Uani 0.714(18) d PU D 2 H41C H 0.6670 0.6216 -0.0921 0.092 Uiso 0.714(18) calc PR D 2 H41D H 0.5318 0.6106 -0.1283 0.092 Uiso 0.714(18) calc PR D 2 C42A C 0.6489(12) 0.5572(7) -0.1947(8) 0.079(2) Uani 0.714(18) d PU D 2 H42C H 0.5759 0.5309 -0.2266 0.095 Uiso 0.714(18) calc PR D 2 H42D H 0.6787 0.5087 -0.1707 0.095 Uiso 0.714(18) calc PR D 2 C43A C 0.7447(14) 0.6034(7) -0.2403(7) 0.074(2) Uani 0.714(18) d PU D 2 H43C H 0.7371 0.5774 -0.2938 0.089 Uiso 0.714(18) calc PR D 2 H43D H 0.8270 0.5995 -0.2206 0.089 Uiso 0.714(18) calc PR D 2 C44 C 0.7244(6) 0.6966(4) -0.2336(3) 0.0710(17) Uani 1 d U . . H44A H 0.8005 0.7415 -0.2329 0.085 Uiso 1 calc R E 1 H44B H 0.6781 0.6953 -0.2815 0.085 Uiso 1 calc R E 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.046(5) 0.037(4) 0.038(5) 0.002(4) 0.009(4) 0.019(4) Li2 0.040(5) 0.046(5) 0.036(4) 0.001(4) 0.014(4) 0.024(4) P1 0.0289(7) 0.0380(7) 0.0350(7) -0.0008(5) 0.0117(5) 0.0146(5) P2 0.0241(6) 0.0342(6) 0.0382(7) 0.0008(5) 0.0128(5) 0.0151(5) Si1 0.0389(8) 0.0487(8) 0.0397(8) -0.0039(6) 0.0181(6) 0.0202(6) Si2 0.0299(8) 0.0426(8) 0.0408(8) 0.0026(6) 0.0076(6) 0.0175(6) Si3 0.0328(8) 0.0449(8) 0.0462(9) 0.0025(7) 0.0030(6) 0.0146(6) Si4 0.0329(8) 0.0391(8) 0.0459(8) -0.0002(6) 0.0199(6) 0.0129(6) N1 0.066(3) 0.046(3) 0.046(3) -0.001(2) 0.008(2) 0.037(2) N2 0.028(2) 0.036(2) 0.048(2) 0.0027(18) 0.0156(18) 0.0144(17) C1 0.024(2) 0.038(3) 0.038(3) -0.002(2) 0.009(2) 0.0132(19) C2 0.096(5) 0.050(4) 0.067(4) 0.008(3) -0.009(4) 0.022(3) C3 0.049(4) 0.061(4) 0.063(4) 0.010(3) -0.012(3) 0.006(3) C4 0.065(4) 0.149(7) 0.041(4) 0.010(4) 0.019(3) 0.050(4) C5 0.069(4) 0.077(4) 0.043(3) -0.007(3) 0.020(3) 0.026(3) C6 0.066(4) 0.073(4) 0.064(4) -0.004(3) 0.028(3) 0.043(3) C7 0.058(4) 0.070(4) 0.052(3) 0.001(3) 0.027(3) 0.015(3) C8 0.022(2) 0.040(3) 0.034(3) 0.000(2) 0.0059(19) 0.0171(19) C9 0.029(3) 0.049(3) 0.052(3) 0.010(2) 0.017(2) 0.018(2) C10 0.041(3) 0.050(3) 0.065(4) 0.011(3) 0.019(3) 0.012(2) C11 0.025(3) 0.073(4) 0.063(4) 0.006(3) 0.020(3) 0.014(3) C12 0.034(3) 0.066(4) 0.045(3) -0.001(3) 0.014(2) 0.027(3) C13 0.028(3) 0.047(3) 0.037(3) -0.002(2) 0.007(2) 0.020(2) C14 0.046(3) 0.053(3) 0.040(3) -0.008(2) 0.013(2) 0.028(2) C15 0.102(6) 0.135(6) 0.052(4) 0.004(4) 0.002(4) 0.097(5) C16 0.210(10) 0.042(4) 0.073(5) 0.001(3) 0.035(5) 0.046(5) O4 0.059(2) 0.0404(19) 0.045(2) 0.0033(16) 0.0101(17) 0.0291(16) C45 0.077(4) 0.074(4) 0.049(4) 0.010(3) 0.005(3) 0.041(3) C46 0.110(6) 0.092(5) 0.067(4) 0.021(4) 0.007(4) 0.062(4) C47 0.066(4) 0.075(4) 0.084(4) 0.015(4) 0.005(3) 0.045(3) C48 0.061(4) 0.043(3) 0.080(4) -0.001(3) 0.015(3) 0.031(3) O1 0.072(3) 0.050(2) 0.053(2) -0.0046(19) -0.001(2) -0.001(2) C17 0.046(6) 0.055(6) 0.049(6) 0.002(5) -0.004(5) 0.019(4) C18 0.062(8) 0.116(10) 0.134(11) 0.068(9) -0.037(7) -0.026(7) C19 0.068(9) 0.106(11) 0.124(11) 0.060(8) -0.022(8) -0.024(8) C20 0.062(7) 0.051(7) 0.130(10) 0.034(7) -0.026(7) 0.004(6) C17A 0.046(8) 0.046(6) 0.047(7) -0.004(5) -0.006(6) 0.013(6) C18A 0.065(9) 0.039(6) 0.090(9) -0.005(6) -0.005(7) 0.012(6) C19A 0.088(14) 0.086(10) 0.112(11) 0.048(9) -0.006(10) 0.021(10) C20A 0.040(8) 0.083(9) 0.074(9) -0.002(7) 0.009(7) -0.004(7) O2 0.050(2) 0.068(3) 0.049(2) 0.018(2) -0.0040(18) 0.0023(19) C21 0.053(8) 0.051(9) 0.098(10) 0.019(8) -0.012(6) 0.011(6) C22 0.067(10) 0.091(11) 0.086(8) 0.020(8) 0.010(7) 0.005(8) C23 0.080(12) 0.062(10) 0.060(8) 0.019(7) 0.011(6) -0.008(7) C21A 0.070(12) 0.045(12) 0.067(11) 0.003(8) -0.007(8) 0.012(9) C22A 0.070(14) 0.049(11) 0.106(12) 0.022(9) -0.005(11) -0.001(10) C23A 0.077(17) 0.081(15) 0.081(17) 0.035(12) -0.008(11) 0.024(11) C24 0.078(5) 0.079(5) 0.047(4) 0.019(3) -0.011(3) 0.000(4) C25 0.024(2) 0.031(2) 0.040(3) -0.001(2) 0.011(2) 0.0106(18) C26 0.044(4) 0.076(4) 0.069(4) 0.009(3) -0.010(3) 0.010(3) C27 0.045(3) 0.056(3) 0.073(4) 0.013(3) 0.000(3) 0.023(3) C28 0.068(4) 0.086(5) 0.037(3) -0.005(3) 0.003(3) 0.028(3) C29 0.064(4) 0.056(3) 0.042(3) -0.001(3) 0.024(3) 0.019(3) C30 0.051(4) 0.052(3) 0.063(4) 0.005(3) 0.023(3) 0.004(3) C31 0.041(3) 0.056(3) 0.068(4) -0.008(3) 0.022(3) 0.023(3) C32 0.028(3) 0.038(3) 0.027(2) -0.0010(19) 0.0091(19) 0.0132(19) C33 0.030(3) 0.044(3) 0.043(3) 0.003(2) 0.012(2) 0.013(2) C34 0.047(3) 0.044(3) 0.058(3) 0.010(3) 0.002(3) 0.022(3) C35 0.044(4) 0.064(4) 0.076(4) 0.018(3) 0.002(3) 0.031(3) C36 0.025(3) 0.056(3) 0.061(4) 0.006(3) 0.002(2) 0.012(2) C37 0.031(3) 0.044(3) 0.038(3) -0.001(2) 0.004(2) 0.015(2) C38 0.030(3) 0.055(3) 0.042(3) -0.003(2) 0.006(2) 0.012(2) C39 0.040(3) 0.044(3) 0.071(4) 0.003(3) 0.007(3) 0.007(2) C40 0.030(3) 0.059(3) 0.063(4) 0.008(3) 0.020(3) 0.022(2) O3 0.058(2) 0.0410(19) 0.050(2) 0.0017(16) 0.0326(18) 0.0264(16) C41 0.126(6) 0.048(4) 0.062(6) 0.001(4) 0.052(5) 0.034(4) C42 0.127(5) 0.049(4) 0.063(5) 0.001(4) 0.049(5) 0.034(4) C43 0.122(5) 0.051(4) 0.063(5) -0.002(4) 0.051(4) 0.038(4) C41A 0.125(6) 0.047(4) 0.062(5) 0.002(4) 0.056(4) 0.033(4) C42A 0.128(5) 0.050(3) 0.064(5) -0.001(3) 0.049(4) 0.033(3) C43A 0.119(4) 0.051(3) 0.060(4) 0.002(3) 0.053(4) 0.041(3) C44 0.113(4) 0.053(3) 0.053(3) -0.001(2) 0.050(3) 0.034(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 Li1 O1 1.938(9) . ? Li1 O2 1.973(8) . ? Li1 N1 2.124(9) . ? Li1 P1 2.535(8) . ? Li2 O3 1.965(8) . ? Li2 O4 1.983(8) . ? Li2 N2 2.097(9) . ? Li2 P2 2.535(7) . ? P1 C8 1.816(4) . ? P1 C1 1.895(4) . ? P2 C32 1.823(5) . ? P2 C25 1.900(4) . ? Si1 C7 1.862(5) . ? Si1 C1 1.875(4) . ? Si1 C6 1.875(5) . ? Si1 C5 1.877(6) . ? Si2 C3 1.852(5) . ? Si2 C2 1.868(6) . ? Si2 C4 1.873(5) . ? Si2 C1 1.874(5) . ? Si3 C27 1.866(5) . ? Si3 C25 1.868(5) . ? Si3 C28 1.875(5) . ? Si3 C26 1.885(5) . ? Si4 C29 1.870(5) . ? Si4 C30 1.875(5) . ? Si4 C25 1.878(4) . ? Si4 C31 1.879(5) . ? N1 C16 1.451(7) . ? N1 C14 1.474(6) . ? N1 C15 1.483(8) . ? N2 C39 1.467(6) . ? N2 C38 1.480(6) . ? N2 C40 1.482(5) . ? C8 C9 1.401(6) . ? C8 C13 1.432(6) . ? C9 C10 1.390(6) . ? C10 C11 1.409(7) . ? C11 C12 1.362(7) . ? C12 C13 1.391(6) . ? C13 C14 1.501(6) . ? O4 C45 1.429(6) . ? O4 C48 1.448(5) . ? C45 C46 1.515(7) . ? C46 C47 1.507(7) . ? C47 C48 1.491(7) . ? O1 C17 1.371(8) . ? O1 C17A 1.384(9) . ? O1 C20 1.492(9) . ? O1 C20A 1.501(10) . ? C17 C18 1.491(10) . ? C18 C19 1.472(12) . ? C19 C20 1.481(12) . ? C17A C18A 1.532(11) . ? C18A C19A 1.481(13) . ? C19A C20A 1.512(13) . ? O2 C24 1.393(6) . ? O2 C21 1.422(13) . ? O2 C21A 1.52(2) . ? C21 C22 1.36(2) . ? C22 C23 1.50(2) . ? C23 C24 1.493(16) . ? C21A C22A 1.35(3) . ? C22A C23A 1.37(4) . ? C23A C24 1.50(3) . ? C32 C33 1.411(6) . ? C32 C37 1.427(6) . ? C33 C34 1.387(7) . ? C34 C35 1.380(7) . ? C35 C36 1.385(7) . ? C36 C37 1.390(7) . ? C37 C38 1.499(6) . ? O3 C44 1.425(5) . ? O3 C41A 1.442(19) . ? O3 C41 1.45(5) . ? C41 C42 1.12(5) . ? C42 C43 1.32(3) . ? C43 C44 1.76(3) . ? C41A C42A 1.406(17) . ? C42A C43A 1.461(15) . ? C43A C44 1.468(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O2 105.9(4) . . ? O1 Li1 N1 110.3(4) . . ? O2 Li1 N1 106.2(4) . . ? O1 Li1 P1 120.1(4) . . ? O2 Li1 P1 118.9(4) . . ? N1 Li1 P1 93.8(3) . . ? O3 Li2 O4 109.7(4) . . ? O3 Li2 N2 108.6(4) . . ? O4 Li2 N2 107.1(4) . . ? O3 Li2 P2 115.3(4) . . ? O4 Li2 P2 119.7(3) . . ? N2 Li2 P2 94.5(3) . . ? C8 P1 C1 103.6(2) . . ? C8 P1 Li1 84.9(2) . . ? C1 P1 Li1 123.1(2) . . ? C32 P2 C25 103.1(2) . . ? C32 P2 Li2 89.6(2) . . ? C25 P2 Li2 123.6(2) . . ? C7 Si1 C1 113.5(2) . . ? C7 Si1 C6 107.4(3) . . ? C1 Si1 C6 111.1(2) . . ? C7 Si1 C5 108.2(3) . . ? C1 Si1 C5 110.3(2) . . ? C6 Si1 C5 105.9(3) . . ? C3 Si2 C2 108.3(3) . . ? C3 Si2 C4 106.1(3) . . ? C2 Si2 C4 106.1(3) . . ? C3 Si2 C1 111.4(2) . . ? C2 Si2 C1 111.3(2) . . ? C4 Si2 C1 113.3(2) . . ? C27 Si3 C25 113.3(2) . . ? C27 Si3 C28 107.1(3) . . ? C25 Si3 C28 110.7(2) . . ? C27 Si3 C26 107.4(3) . . ? C25 Si3 C26 112.1(2) . . ? C28 Si3 C26 105.9(3) . . ? C29 Si4 C30 107.6(2) . . ? C29 Si4 C25 113.0(2) . . ? C30 Si4 C25 110.6(2) . . ? C29 Si4 C31 106.0(3) . . ? C30 Si4 C31 109.0(2) . . ? C25 Si4 C31 110.4(2) . . ? C16 N1 C14 108.6(4) . . ? C16 N1 C15 110.6(5) . . ? C14 N1 C15 110.1(4) . . ? C16 N1 Li1 109.1(4) . . ? C14 N1 Li1 109.5(4) . . ? C15 N1 Li1 109.0(4) . . ? C39 N2 C38 108.9(4) . . ? C39 N2 C40 107.9(4) . . ? C38 N2 C40 109.0(4) . . ? C39 N2 Li2 110.0(4) . . ? C38 N2 Li2 111.6(3) . . ? C40 N2 Li2 109.4(4) . . ? Si2 C1 Si1 118.1(2) . . ? Si2 C1 P1 110.5(2) . . ? Si1 C1 P1 110.0(2) . . ? C9 C8 C13 115.1(4) . . ? C9 C8 P1 125.7(3) . . ? C13 C8 P1 119.2(3) . . ? C10 C9 C8 123.7(4) . . ? C9 C10 C11 119.5(5) . . ? C12 C11 C10 118.1(4) . . ? C11 C12 C13 123.0(5) . . ? C12 C13 C8 120.5(4) . . ? C12 C13 C14 120.6(4) . . ? C8 C13 C14 118.9(4) . . ? N1 C14 C13 113.1(4) . . ? C45 O4 C48 109.8(4) . . ? C45 O4 Li2 123.7(4) . . ? C48 O4 Li2 124.5(4) . . ? O4 C45 C46 106.8(4) . . ? C47 C46 C45 102.8(5) . . ? C48 C47 C46 104.0(5) . . ? O4 C48 C47 105.4(4) . . ? C17 O1 C20 106.4(6) . . ? C17A O1 C20A 105.0(7) . . ? C17 O1 Li1 140.1(5) . . ? C17A O1 Li1 133.5(6) . . ? C20 O1 Li1 113.5(5) . . ? C20A O1 Li1 121.5(6) . . ? O1 C17 C18 105.3(7) . . ? C19 C18 C17 106.0(8) . . ? C18 C19 C20 105.5(9) . . ? C19 C20 O1 100.7(8) . . ? O1 C17A C18A 102.3(7) . . ? C19A C18A C17A 104.2(9) . . ? C18A C19A C20A 104.2(10) . . ? O1 C20A C19A 94.7(9) . . ? C24 O2 C21 104.7(7) . . ? C24 O2 Li1 129.2(4) . . ? C21 O2 Li1 125.1(7) . . ? C21A O2 Li1 120.6(9) . . ? C22 C21 O2 113.6(12) . . ? C21 C22 C23 102.2(15) . . ? C24 C23 C22 106.2(13) . . ? C22A C21A O2 105.2(19) . . ? C21A C22A C23A 112(2) . . ? C22A C23A C24 105.0(19) . . ? O2 C24 C23 107.3(9) . . ? O2 C24 C23A 104.9(13) . . ? Si3 C25 Si4 117.8(2) . . ? Si3 C25 P2 109.7(2) . . ? Si4 C25 P2 110.9(2) . . ? C33 C32 C37 115.8(4) . . ? C33 C32 P2 125.2(3) . . ? C37 C32 P2 118.9(3) . . ? C34 C33 C32 123.0(4) . . ? C35 C34 C33 120.1(5) . . ? C34 C35 C36 118.7(5) . . ? C35 C36 C37 122.2(5) . . ? C36 C37 C32 120.2(4) . . ? C36 C37 C38 118.9(4) . . ? C32 C37 C38 120.9(4) . . ? N2 C38 C37 114.3(4) . . ? C44 O3 C41 110(2) . . ? C44 O3 Li2 134.3(4) . . ? C41A O3 Li2 117.9(7) . . ? C41 O3 Li2 111.6(18) . . ? C42 C41 O3 113(4) . . ? C41 C42 C43 119(3) . . ? C42 C43 C44 102(2) . . ? C42A C41A O3 108.0(12) . . ? C41A C42A C43A 106.0(10) . . ? C42A C43A C44 104.4(8) . . ? O3 C44 C43A 107.3(6) . . ? O3 C44 C43 94.9(10) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.765 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.106 #===END data_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H47 N3 Na P Si2' _chemical_formula_weight 463.77 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 9.5849(15) _cell_length_b 11.8767(18) _cell_length_c 14.424(2) _cell_angle_alpha 67.669(4) _cell_angle_beta 87.913(4) _cell_angle_gamma 71.329(3) _cell_volume 1432.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 6725 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10581 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.81 _reflns_number_total 6468 _reflns_number_gt 4790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material '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^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6468 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Na Na 1.11077(7) -0.10487(7) 0.22224(6) 0.02416(18) Uani 1 1 d . . . P P 0.81013(5) 0.04668(4) 0.21121(4) 0.01982(12) Uani 1 1 d . . . Si1 Si 0.85145(6) 0.29673(5) 0.20822(4) 0.02478(14) Uani 1 1 d . . . Si2 Si 0.54640(5) 0.23638(5) 0.25807(4) 0.02343(14) Uani 1 1 d . . . N1 N 0.99476(16) -0.21976(14) 0.15497(12) 0.0214(3) Uani 1 1 d . . . N2 N 1.27074(17) -0.21347(16) 0.38127(12) 0.0259(4) Uani 1 1 d . . . N3 N 1.37009(17) -0.14948(16) 0.17190(12) 0.0270(4) Uani 1 1 d . . . C1 C 0.75427(19) 0.17586(16) 0.26530(14) 0.0196(4) Uani 1 1 d . . . H1 H 0.7906 0.1315 0.3385 0.024 Uiso 1 1 calc R . . C2 C 0.8281(3) 0.4049(2) 0.2786(2) 0.0459(6) Uani 1 1 d . . . H2A H 0.8908 0.4589 0.2532 0.069 Uiso 1 1 calc R . . H2B H 0.8569 0.3522 0.3505 0.069 Uiso 1 1 calc R . . H2C H 0.7243 0.4599 0.2689 0.069 Uiso 1 1 calc R . . C3 C 0.7829(3) 0.4005(2) 0.07386(17) 0.0461(6) Uani 1 1 d . . . H3A H 0.7811 0.3461 0.0373 0.069 Uiso 1 1 calc R . . H3B H 0.8487 0.4502 0.0437 0.069 Uiso 1 1 calc R . . H3C H 0.6827 0.4597 0.0698 0.069 Uiso 1 1 calc R . . C4 C 1.0557(2) 0.2150(2) 0.21668(19) 0.0403(6) Uani 1 1 d . . . H4A H 1.0770 0.1704 0.1703 0.061 Uiso 1 1 calc R . . H4B H 1.0914 0.1522 0.2857 0.061 Uiso 1 1 calc R . . H4C H 1.1059 0.2795 0.1985 0.061 Uiso 1 1 calc R . . C5 C 0.4612(2) 0.2858(2) 0.12812(16) 0.0392(6) Uani 1 1 d . . . H5A H 0.4922 0.2116 0.1085 0.059 Uiso 1 1 calc R . . H5B H 0.4936 0.3551 0.0809 0.059 Uiso 1 1 calc R . . H5C H 0.3532 0.3165 0.1269 0.059 Uiso 1 1 calc R . . C6 C 0.4679(2) 0.3818(2) 0.29132(19) 0.0416(6) Uani 1 1 d . . . H6A H 0.3611 0.4005 0.2950 0.062 Uiso 1 1 calc R . . H6B H 0.4865 0.4563 0.2396 0.062 Uiso 1 1 calc R . . H6C H 0.5153 0.3643 0.3567 0.062 Uiso 1 1 calc R . . C7 C 0.4775(2) 0.1088(2) 0.34723(16) 0.0308(5) Uani 1 1 d . . . H7A H 0.3704 0.1339 0.3321 0.046 Uiso 1 1 calc R . . H7B H 0.4988 0.0987 0.4164 0.046 Uiso 1 1 calc R . . H7C H 0.5270 0.0269 0.3400 0.046 Uiso 1 1 calc R . . C8 C 0.82659(18) -0.10283(16) 0.31765(13) 0.0187(4) Uani 1 1 d . . . C9 C 0.82073(19) -0.11749(17) 0.41962(14) 0.0225(4) Uani 1 1 d . . . H9 H 0.8095 -0.0446 0.4355 0.027 Uiso 1 1 calc R . . C10 C 0.8307(2) -0.23395(18) 0.49722(15) 0.0272(4) Uani 1 1 d . . . H10 H 0.8265 -0.2391 0.5646 0.033 Uiso 1 1 calc R . . C11 C 0.8467(2) -0.34276(18) 0.47789(15) 0.0284(5) Uani 1 1 d . . . H11 H 0.8536 -0.4225 0.5311 0.034 Uiso 1 1 calc R . . C12 C 0.85258(19) -0.33254(18) 0.37894(15) 0.0242(4) Uani 1 1 d . . . H12 H 0.8626 -0.4065 0.3648 0.029 Uiso 1 1 calc R . . C13 C 0.84413(18) -0.21715(17) 0.29975(14) 0.0191(4) Uani 1 1 d . . . C14 C 0.84832(18) -0.21123(18) 0.19367(14) 0.0213(4) Uani 1 1 d . . . H14A H 0.8192 -0.2828 0.1910 0.026 Uiso 1 1 calc R . . H14B H 0.7745 -0.1293 0.1489 0.026 Uiso 1 1 calc R . . C15 C 0.9767(2) -0.1665(2) 0.04485(15) 0.0336(5) Uani 1 1 d . . . H15A H 1.0739 -0.1733 0.0192 0.050 Uiso 1 1 calc R . . H15B H 0.9140 -0.0757 0.0198 0.050 Uiso 1 1 calc R . . H15C H 0.9302 -0.2150 0.0218 0.050 Uiso 1 1 calc R . . C16 C 1.0920(2) -0.35454(18) 0.19237(16) 0.0300(5) Uani 1 1 d . . . H16A H 1.0965 -0.3926 0.2660 0.045 Uiso 1 1 calc R . . H16B H 1.1915 -0.3584 0.1720 0.045 Uiso 1 1 calc R . . H16C H 1.0529 -0.4028 0.1641 0.045 Uiso 1 1 calc R . . C17 C 1.2276(3) -0.1451(2) 0.44957(17) 0.0390(5) Uani 1 1 d . . . H17A H 1.2921 -0.1941 0.5128 0.058 Uiso 1 1 calc R . . H17B H 1.1246 -0.1364 0.4634 0.058 Uiso 1 1 calc R . . H17C H 1.2373 -0.0593 0.4180 0.058 Uiso 1 1 calc R . . C18 C 1.2541(3) -0.3411(2) 0.42907(17) 0.0375(5) Uani 1 1 d . . . H18A H 1.3162 -0.3894 0.4933 0.056 Uiso 1 1 calc R . . H18B H 1.2846 -0.3882 0.3847 0.056 Uiso 1 1 calc R . . H18C H 1.1503 -0.3311 0.4411 0.056 Uiso 1 1 calc R . . C19 C 1.4245(2) -0.2249(2) 0.35834(15) 0.0315(5) Uani 1 1 d . . . H19A H 1.4926 -0.2956 0.4160 0.038 Uiso 1 1 calc R . . H19B H 1.4417 -0.1438 0.3500 0.038 Uiso 1 1 calc R . . C20 C 1.4600(2) -0.2515(2) 0.26391(16) 0.0315(5) Uani 1 1 d . . . H20A H 1.5657 -0.2627 0.2548 0.038 Uiso 1 1 calc R . . H20B H 1.4450 -0.3337 0.2733 0.038 Uiso 1 1 calc R . . C21 C 1.4091(2) -0.1929(2) 0.08870(17) 0.0398(6) Uani 1 1 d . . . H21A H 1.3486 -0.1276 0.0267 0.060 Uiso 1 1 calc R . . H21B H 1.3907 -0.2745 0.1046 0.060 Uiso 1 1 calc R . . H21C H 1.5140 -0.2056 0.0794 0.060 Uiso 1 1 calc R . . C22 C 1.3997(2) -0.0284(2) 0.14793(18) 0.0380(5) Uani 1 1 d . . . H22A H 1.3647 0.0057 0.1997 0.057 Uiso 1 1 calc R . . H22B H 1.3479 0.0343 0.0822 0.057 Uiso 1 1 calc R . . H22C H 1.5064 -0.0443 0.1458 0.057 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 Na 0.0181(3) 0.0267(4) 0.0290(4) -0.0126(3) 0.0013(3) -0.0069(3) P 0.0234(2) 0.0160(2) 0.0184(3) -0.00666(19) 0.00258(18) -0.00438(18) Si1 0.0279(3) 0.0192(3) 0.0270(3) -0.0076(2) 0.0050(2) -0.0095(2) Si2 0.0203(2) 0.0202(3) 0.0260(3) -0.0087(2) 0.0008(2) -0.0019(2) N1 0.0198(7) 0.0216(8) 0.0241(9) -0.0113(7) 0.0044(6) -0.0057(6) N2 0.0250(8) 0.0308(9) 0.0253(9) -0.0128(7) 0.0044(7) -0.0115(7) N3 0.0221(8) 0.0344(9) 0.0267(9) -0.0126(8) 0.0056(7) -0.0119(7) C1 0.0208(8) 0.0162(8) 0.0205(10) -0.0073(7) 0.0015(7) -0.0042(7) C2 0.0595(15) 0.0410(13) 0.0595(17) -0.0296(12) 0.0225(13) -0.0346(12) C3 0.0511(14) 0.0370(13) 0.0345(14) 0.0019(11) 0.0060(11) -0.0139(11) C4 0.0286(11) 0.0411(13) 0.0513(15) -0.0142(11) 0.0054(10) -0.0163(10) C5 0.0292(11) 0.0448(13) 0.0316(13) -0.0065(11) -0.0061(9) -0.0060(10) C6 0.0357(11) 0.0271(12) 0.0575(16) -0.0217(11) 0.0036(11) 0.0019(9) C7 0.0224(9) 0.0339(11) 0.0354(12) -0.0127(10) 0.0054(8) -0.0099(8) C8 0.0148(8) 0.0177(9) 0.0217(10) -0.0069(7) 0.0015(7) -0.0040(7) C9 0.0254(9) 0.0172(9) 0.0239(10) -0.0099(8) 0.0035(8) -0.0037(7) C10 0.0287(10) 0.0269(10) 0.0196(10) -0.0062(8) 0.0058(8) -0.0048(8) C11 0.0299(10) 0.0203(10) 0.0279(11) -0.0027(8) 0.0065(8) -0.0078(8) C12 0.0228(9) 0.0161(9) 0.0347(12) -0.0105(8) 0.0059(8) -0.0071(7) C13 0.0137(7) 0.0190(9) 0.0249(10) -0.0096(8) 0.0023(7) -0.0047(7) C14 0.0173(8) 0.0207(9) 0.0290(11) -0.0127(8) 0.0023(7) -0.0067(7) C15 0.0348(11) 0.0392(12) 0.0284(12) -0.0151(10) 0.0072(9) -0.0125(10) C16 0.0252(9) 0.0272(11) 0.0368(12) -0.0143(9) 0.0069(9) -0.0057(8) C17 0.0452(13) 0.0427(13) 0.0315(13) -0.0197(11) 0.0048(10) -0.0115(11) C18 0.0440(12) 0.0420(13) 0.0334(13) -0.0142(10) 0.0096(10) -0.0243(11) C19 0.0260(10) 0.0390(12) 0.0287(12) -0.0107(10) -0.0026(8) -0.0122(9) C20 0.0202(9) 0.0380(12) 0.0351(12) -0.0146(10) 0.0036(8) -0.0079(9) C21 0.0341(11) 0.0579(15) 0.0371(13) -0.0255(12) 0.0127(10) -0.0200(11) C22 0.0287(10) 0.0394(13) 0.0463(14) -0.0151(11) 0.0057(10) -0.0140(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na N2 2.4533(18) . ? Na N1 2.4689(18) . ? Na N3 2.5108(17) . ? Na P 2.8396(9) . ? Na C8 3.0040(18) . ? P C8 1.8171(18) . ? P C1 1.8980(18) . ? Si1 C3 1.862(2) . ? Si1 C4 1.871(2) . ? Si1 C1 1.8731(18) . ? Si1 C2 1.877(2) . ? Si2 C7 1.867(2) . ? Si2 C5 1.869(2) . ? Si2 C1 1.8811(18) . ? Si2 C6 1.885(2) . ? N1 C15 1.463(2) . ? N1 C16 1.465(2) . ? N1 C14 1.479(2) . ? N2 C18 1.467(3) . ? N2 C17 1.471(3) . ? N2 C19 1.473(2) . ? N3 C22 1.464(3) . ? N3 C21 1.470(3) . ? N3 C20 1.471(3) . ? C8 C9 1.415(3) . ? C9 C10 1.386(2) . ? C10 C11 1.384(3) . ? C11 C12 1.386(3) . ? C12 C13 1.391(2) . ? C13 C14 1.505(3) . ? C19 C20 1.515(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Na N1 122.37(6) . . ? N2 Na N3 74.91(6) . . ? N1 Na N3 106.11(6) . . ? N2 Na P 121.45(5) . . ? N1 Na P 81.40(4) . . ? N3 Na P 155.40(5) . . ? N2 Na C8 95.59(6) . . ? N1 Na C8 73.07(5) . . ? N3 Na C8 168.41(6) . . ? P Na C8 36.09(4) . . ? C8 P C1 104.88(8) . . ? C8 P Na 76.89(5) . . ? C1 P Na 121.53(6) . . ? C3 Si1 C4 108.62(11) . . ? C3 Si1 C1 112.40(10) . . ? C4 Si1 C1 110.99(9) . . ? C3 Si1 C2 107.93(12) . . ? C4 Si1 C2 105.38(12) . . ? C1 Si1 C2 111.22(9) . . ? C7 Si2 C5 108.65(10) . . ? C7 Si2 C1 110.47(8) . . ? C5 Si2 C1 111.44(9) . . ? C7 Si2 C6 106.22(10) . . ? C5 Si2 C6 105.65(11) . . ? C1 Si2 C6 114.07(10) . . ? C15 N1 C16 109.46(16) . . ? C15 N1 C14 109.41(15) . . ? C16 N1 C14 110.16(15) . . ? C15 N1 Na 112.51(12) . . ? C16 N1 Na 106.76(12) . . ? C14 N1 Na 108.50(11) . . ? C18 N2 C17 108.85(17) . . ? C18 N2 C19 110.94(16) . . ? C17 N2 C19 109.95(16) . . ? C18 N2 Na 105.79(13) . . ? C17 N2 Na 112.71(13) . . ? C19 N2 Na 108.54(12) . . ? C22 N3 C21 108.98(17) . . ? C22 N3 C20 111.31(17) . . ? C21 N3 C20 107.77(16) . . ? C22 N3 Na 104.58(12) . . ? C21 N3 Na 120.37(12) . . ? C20 N3 Na 103.69(11) . . ? Si1 C1 Si2 118.20(9) . . ? Si1 C1 P 110.77(9) . . ? Si2 C1 P 107.68(9) . . ? C10 C9 C8 122.61(18) . . ? C11 C10 C9 120.89(18) . . ? C10 C11 C12 118.38(18) . . ? C11 C12 C13 121.91(18) . . ? C12 C13 C8 120.82(17) . . ? C12 C13 C14 119.55(17) . . ? C8 C13 C14 119.60(16) . . ? N1 C14 C13 113.82(15) . . ? N2 C19 C20 112.76(16) . . ? N3 C20 C19 114.07(17) . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 28.81 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 0.452 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.054 #===END data_compound_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H54 K N4 P Si2' _chemical_formula_weight 536.97 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 10.1740(2) _cell_length_b 28.7226(6) _cell_length_c 12.1761(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.877(1) _cell_angle_gamma 90.00 _cell_volume 3366.77(13) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 10470 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.64 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.907 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21064 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.82 _reflns_number_total 7949 _reflns_number_gt 5451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material '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^)+(0.0485P)^2^+0.2726P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7949 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K K 0.11439(4) 0.138678(15) 0.96175(4) 0.02908(11) Uani 1 1 d . . . P P -0.20488(5) 0.112212(17) 0.82186(4) 0.02660(12) Uani 1 1 d . . . N1 N -0.01061(15) 0.12928(5) 1.13449(13) 0.0273(4) Uani 1 1 d . . . N2 N 0.27129(17) 0.05441(6) 0.99292(16) 0.0384(4) Uani 1 1 d . . . N3 N 0.40898(15) 0.14564(5) 1.06614(13) 0.0274(4) Uani 1 1 d . . . N4 N 0.24293(16) 0.22791(6) 0.96456(14) 0.0317(4) Uani 1 1 d . . . Si1 Si -0.17290(6) 0.08401(2) 0.58869(5) 0.03265(14) Uani 1 1 d . . . Si2 Si -0.47478(5) 0.09981(2) 0.62282(4) 0.02925(14) Uani 1 1 d . . . C1 C -0.28728(19) 0.11545(7) 0.65728(15) 0.0270(4) Uani 1 1 d . . . H1A H -0.2851 0.1490 0.6360 0.032 Uiso 1 1 calc R . . C2 C -0.1338(3) 0.02345(8) 0.6454(2) 0.0488(6) Uani 1 1 d . . . H2A H -0.0993 0.0241 0.7304 0.073 Uiso 1 1 calc R . . H2B H -0.0631 0.0098 0.6165 0.073 Uiso 1 1 calc R . . H2C H -0.2187 0.0046 0.6191 0.073 Uiso 1 1 calc R . . C3 C -0.0062(2) 0.11683(9) 0.6156(2) 0.0511(6) Uani 1 1 d . . . H3A H -0.0258 0.1475 0.5784 0.077 Uiso 1 1 calc R . . H3B H 0.0554 0.0994 0.5832 0.077 Uiso 1 1 calc R . . H3C H 0.0390 0.1208 0.6993 0.077 Uiso 1 1 calc R . . C4 C -0.2513(2) 0.07992(10) 0.42649(19) 0.0521(6) Uani 1 1 d . . . H4A H -0.3351 0.0606 0.4067 0.078 Uiso 1 1 calc R . . H4B H -0.1840 0.0658 0.3942 0.078 Uiso 1 1 calc R . . H4C H -0.2756 0.1112 0.3940 0.078 Uiso 1 1 calc R . . C5 C -0.5608(2) 0.13985(8) 0.70024(18) 0.0381(5) Uani 1 1 d . . . H5A H -0.5141 0.1375 0.7842 0.057 Uiso 1 1 calc R . . H5B H -0.6587 0.1311 0.6820 0.057 Uiso 1 1 calc R . . H5C H -0.5547 0.1720 0.6751 0.057 Uiso 1 1 calc R . . C6 C -0.5772(2) 0.10642(10) 0.46424(18) 0.0522(7) Uani 1 1 d . . . H6A H -0.5619 0.1376 0.4379 0.078 Uiso 1 1 calc R . . H6B H -0.6763 0.1022 0.4530 0.078 Uiso 1 1 calc R . . H6C H -0.5468 0.0829 0.4193 0.078 Uiso 1 1 calc R . . C7 C -0.4967(2) 0.03838(8) 0.6640(2) 0.0467(6) Uani 1 1 d . . . H7A H -0.4617 0.0171 0.6169 0.070 Uiso 1 1 calc R . . H7B H -0.5954 0.0321 0.6505 0.070 Uiso 1 1 calc R . . H7C H -0.4445 0.0336 0.7463 0.070 Uiso 1 1 calc R . . C8 C -0.21259(17) 0.17143(6) 0.87090(15) 0.0236(4) Uani 1 1 d . . . C9 C -0.2452(2) 0.21141(7) 0.79826(17) 0.0316(4) Uani 1 1 d . . . H9A H -0.2633 0.2074 0.7172 0.038 Uiso 1 1 calc R . . C10 C -0.2519(2) 0.25563(7) 0.83985(18) 0.0364(5) Uani 1 1 d . . . H10A H -0.2739 0.2811 0.7873 0.044 Uiso 1 1 calc R . . C11 C -0.2269(2) 0.26348(7) 0.95684(19) 0.0361(5) Uani 1 1 d . . . H11A H -0.2319 0.2939 0.9856 0.043 Uiso 1 1 calc R . . C12 C -0.19441(19) 0.22547(7) 1.03088(18) 0.0307(4) Uani 1 1 d . . . H12A H -0.1775 0.2304 1.1114 0.037 Uiso 1 1 calc R . . C13 C -0.18552(17) 0.18037(6) 0.99225(16) 0.0244(4) Uani 1 1 d . . . C14 C -0.15855(18) 0.14090(7) 1.07796(16) 0.0272(4) Uani 1 1 d . . . H14A H -0.1997 0.1490 1.1389 0.033 Uiso 1 1 calc R . . H14B H -0.2071 0.1128 1.0374 0.033 Uiso 1 1 calc R . . C15 C 0.0571(2) 0.16501(8) 1.21911(19) 0.0429(5) Uani 1 1 d . . . H15A H 0.0080 0.1682 1.2760 0.064 Uiso 1 1 calc R . . H15B H 0.0549 0.1948 1.1792 0.064 Uiso 1 1 calc R . . H15C H 0.1537 0.1560 1.2590 0.064 Uiso 1 1 calc R . . C16 C 0.0007(2) 0.08472(8) 1.1938(2) 0.0451(6) Uani 1 1 d . . . H16A H 0.0989 0.0769 1.2306 0.068 Uiso 1 1 calc R . . H16B H -0.0443 0.0605 1.1375 0.068 Uiso 1 1 calc R . . H16C H -0.0449 0.0868 1.2533 0.068 Uiso 1 1 calc R . . C17 C 0.2045(3) 0.01483(9) 1.0290(3) 0.0638(8) Uani 1 1 d . . . H17A H 0.1071 0.0130 0.9797 0.096 Uiso 1 1 calc R . . H17B H 0.2093 0.0189 1.1101 0.096 Uiso 1 1 calc R . . H17C H 0.2525 -0.0140 1.0212 0.096 Uiso 1 1 calc R . . C18 C 0.2659(3) 0.04807(11) 0.8739(2) 0.0627(7) Uani 1 1 d . . . H18A H 0.3164 0.0197 0.8675 0.094 Uiso 1 1 calc R . . H18B H 0.3087 0.0749 0.8491 0.094 Uiso 1 1 calc R . . H18C H 0.1688 0.0453 0.8242 0.094 Uiso 1 1 calc R . . C19 C 0.4144(2) 0.05872(7) 1.0705(2) 0.0414(5) Uani 1 1 d . . . H19A H 0.4690 0.0321 1.0569 0.050 Uiso 1 1 calc R . . H19B H 0.4148 0.0568 1.1518 0.050 Uiso 1 1 calc R . . C20 C 0.4851(2) 0.10337(7) 1.0554(2) 0.0385(5) Uani 1 1 d . . . H20A H 0.5787 0.1044 1.1143 0.046 Uiso 1 1 calc R . . H20B H 0.4972 0.1032 0.9780 0.046 Uiso 1 1 calc R . . C21 C 0.4081(2) 0.15070(8) 1.18499(18) 0.0437(6) Uani 1 1 d . . . H21A H 0.5036 0.1540 1.2375 0.066 Uiso 1 1 calc R . . H21B H 0.3656 0.1231 1.2068 0.066 Uiso 1 1 calc R . . H21C H 0.3543 0.1784 1.1906 0.066 Uiso 1 1 calc R . . C22 C 0.4712(2) 0.18665(7) 1.03130(18) 0.0334(5) Uani 1 1 d . . . H22A H 0.4767 0.1814 0.9526 0.040 Uiso 1 1 calc R . . H22B H 0.5672 0.1904 1.0851 0.040 Uiso 1 1 calc R . . C23 C 0.3911(2) 0.23142(7) 1.03070(18) 0.0349(5) Uani 1 1 d . . . H23A H 0.4014 0.2401 1.1118 0.042 Uiso 1 1 calc R . . H23B H 0.4325 0.2567 0.9973 0.042 Uiso 1 1 calc R . . C24 C 0.2205(2) 0.22512(8) 0.84034(18) 0.0459(6) Uani 1 1 d . . . H24A H 0.1206 0.2238 0.7982 0.069 Uiso 1 1 calc R . . H24B H 0.2654 0.1970 0.8237 0.069 Uiso 1 1 calc R . . H24C H 0.2604 0.2527 0.8156 0.069 Uiso 1 1 calc R . . C25 C 0.1677(2) 0.26777(8) 0.9901(2) 0.0433(5) Uani 1 1 d . . . H25A H 0.2047 0.2967 0.9689 0.065 Uiso 1 1 calc R . . H25B H 0.1791 0.2682 1.0732 0.065 Uiso 1 1 calc R . . H25C H 0.0688 0.2651 0.9453 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 K 0.0205(2) 0.0332(2) 0.0322(2) 0.00233(18) 0.00673(17) -0.00076(17) P 0.0296(3) 0.0229(3) 0.0217(2) 0.00020(19) 0.0005(2) -0.0003(2) N1 0.0262(8) 0.0295(9) 0.0239(8) -0.0008(7) 0.0051(7) -0.0016(7) N2 0.0341(10) 0.0300(10) 0.0532(12) 0.0060(8) 0.0169(9) 0.0016(7) N3 0.0219(8) 0.0315(9) 0.0284(9) 0.0020(7) 0.0078(7) -0.0001(7) N4 0.0312(9) 0.0307(9) 0.0310(9) 0.0043(7) 0.0069(7) 0.0031(7) Si1 0.0330(3) 0.0345(3) 0.0306(3) 0.0013(2) 0.0106(2) 0.0019(2) Si2 0.0278(3) 0.0355(3) 0.0207(3) -0.0002(2) 0.0026(2) -0.0007(2) C1 0.0313(10) 0.0238(10) 0.0226(10) 0.0013(7) 0.0043(8) 0.0002(8) C2 0.0538(15) 0.0369(13) 0.0580(16) 0.0001(11) 0.0211(13) 0.0084(11) C3 0.0359(12) 0.0610(17) 0.0563(16) 0.0089(12) 0.0150(11) -0.0003(11) C4 0.0540(15) 0.0701(18) 0.0368(13) -0.0063(12) 0.0209(12) 0.0033(13) C5 0.0344(11) 0.0459(13) 0.0343(12) 0.0013(10) 0.0115(9) 0.0019(10) C6 0.0383(13) 0.083(2) 0.0286(12) -0.0032(12) 0.0019(10) 0.0033(12) C7 0.0438(13) 0.0393(13) 0.0553(15) -0.0070(11) 0.0139(12) -0.0122(10) C8 0.0176(8) 0.0255(10) 0.0260(10) -0.0002(8) 0.0046(7) -0.0027(7) C9 0.0363(11) 0.0282(11) 0.0277(10) 0.0025(8) 0.0069(9) 0.0012(8) C10 0.0404(12) 0.0249(11) 0.0405(12) 0.0036(9) 0.0084(10) 0.0039(9) C11 0.0397(12) 0.0241(11) 0.0458(13) -0.0071(9) 0.0157(10) 0.0019(9) C12 0.0294(10) 0.0338(11) 0.0306(11) -0.0058(9) 0.0123(9) -0.0019(8) C13 0.0177(9) 0.0276(10) 0.0281(10) -0.0025(8) 0.0077(8) -0.0034(7) C14 0.0252(10) 0.0326(11) 0.0242(10) -0.0013(8) 0.0086(8) -0.0052(8) C15 0.0311(11) 0.0491(14) 0.0393(13) -0.0114(10) -0.0013(10) -0.0016(10) C16 0.0465(13) 0.0432(14) 0.0412(13) 0.0123(10) 0.0083(11) 0.0043(11) C17 0.0727(18) 0.0428(15) 0.084(2) -0.0019(14) 0.0366(16) -0.0188(13) C18 0.0478(15) 0.079(2) 0.0538(17) 0.0109(14) 0.0068(13) 0.0060(14) C19 0.0397(12) 0.0326(12) 0.0512(14) 0.0087(10) 0.0136(11) 0.0104(10) C20 0.0258(10) 0.0402(13) 0.0476(13) 0.0050(10) 0.0093(10) 0.0065(9) C21 0.0484(13) 0.0517(15) 0.0309(12) 0.0026(10) 0.0126(10) -0.0037(11) C22 0.0254(10) 0.0391(12) 0.0360(12) 0.0035(9) 0.0104(9) -0.0034(9) C23 0.0331(11) 0.0299(11) 0.0404(12) 0.0020(9) 0.0103(9) -0.0048(9) C24 0.0564(15) 0.0434(14) 0.0344(13) 0.0024(10) 0.0098(11) 0.0059(11) C25 0.0461(13) 0.0407(13) 0.0427(13) 0.0060(10) 0.0138(11) 0.0108(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K N1 2.8008(16) . ? K N2 2.8565(17) . ? K N3 2.8590(15) . ? K N4 2.8725(17) . ? K P 3.2326(6) . ? K C8 3.2854(17) . ? P C8 1.8127(19) . ? P C1 1.9080(18) . ? N1 C16 1.456(3) . ? N1 C15 1.459(2) . ? N1 C14 1.477(2) . ? N2 C18 1.444(3) . ? N2 C17 1.462(3) . ? N2 C19 1.463(3) . ? N3 C21 1.457(3) . ? N3 C22 1.464(2) . ? N3 C20 1.468(2) . ? N4 C24 1.457(3) . ? N4 C23 1.465(2) . ? N4 C25 1.466(3) . ? Si1 C2 1.866(2) . ? Si1 C1 1.870(2) . ? Si1 C3 1.874(2) . ? Si1 C4 1.879(2) . ? Si2 C7 1.868(2) . ? Si2 C1 1.8705(19) . ? Si2 C5 1.874(2) . ? Si2 C6 1.884(2) . ? C8 C9 1.422(3) . ? C8 C13 1.436(2) . ? C9 C10 1.377(3) . ? C10 C11 1.382(3) . ? C11 C12 1.386(3) . ? C12 C13 1.391(3) . ? C13 C14 1.505(2) . ? C19 C20 1.510(3) . ? C22 C23 1.521(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 K N2 100.87(5) . . ? N1 K N3 109.77(5) . . ? N2 K N3 62.60(5) . . ? N1 K N4 113.12(5) . . ? N2 K N4 121.45(5) . . ? N3 K N4 61.61(4) . . ? N1 K P 75.53(3) . . ? N2 K P 107.09(4) . . ? N3 K P 168.77(4) . . ? N4 K P 126.31(3) . . ? N1 K C8 67.93(4) . . ? N2 K C8 138.49(5) . . ? N3 K C8 158.64(5) . . ? N4 K C8 98.98(5) . . ? P K C8 32.28(3) . . ? C24 K C8 94.43(5) . . ? C8 P C1 104.42(8) . . ? C8 P K 75.46(5) . . ? C1 P K 124.55(6) . . ? C16 N1 C15 108.93(17) . . ? C16 N1 C14 109.57(15) . . ? C15 N1 C14 110.31(15) . . ? C16 N1 K 118.38(13) . . ? C15 N1 K 103.73(12) . . ? C14 N1 K 105.67(10) . . ? C18 N2 C17 109.4(2) . . ? C18 N2 C19 111.45(17) . . ? C17 N2 C19 109.52(18) . . ? C18 N2 K 97.77(14) . . ? C17 N2 K 113.87(14) . . ? C19 N2 K 114.26(12) . . ? C21 N3 C22 110.48(16) . . ? C21 N3 C20 110.11(16) . . ? C22 N3 C20 110.48(15) . . ? C21 N3 K 96.07(11) . . ? C22 N3 K 114.64(11) . . ? C20 N3 K 114.19(11) . . ? C24 N4 C23 111.23(17) . . ? C24 N4 C25 110.26(16) . . ? C23 N4 C25 110.19(16) . . ? C24 N4 K 91.19(12) . . ? C23 N4 K 116.84(11) . . ? C25 N4 K 115.62(13) . . ? C2 Si1 C1 111.94(10) . . ? C2 Si1 C3 109.37(11) . . ? C1 Si1 C3 109.75(10) . . ? C2 Si1 C4 107.32(12) . . ? C1 Si1 C4 112.69(10) . . ? C3 Si1 C4 105.51(11) . . ? C7 Si2 C1 111.62(9) . . ? C7 Si2 C5 109.20(10) . . ? C1 Si2 C5 110.39(9) . . ? C7 Si2 C6 107.22(12) . . ? C1 Si2 C6 113.05(10) . . ? C5 Si2 C6 105.08(10) . . ? Si1 C1 Si2 121.39(10) . . ? Si1 C1 P 108.67(9) . . ? Si2 C1 P 107.07(9) . . ? C9 C8 C13 115.09(17) . . ? C9 C8 P 125.41(14) . . ? C13 C8 P 119.50(14) . . ? C9 C8 K 116.62(12) . . ? C13 C8 K 82.44(10) . . ? P C8 K 72.26(6) . . ? C10 C9 C8 123.07(19) . . ? C9 C10 C11 120.99(19) . . ? C10 C11 C12 117.87(18) . . ? C11 C12 C13 122.79(19) . . ? C12 C13 C8 120.18(17) . . ? C12 C13 C14 118.97(17) . . ? C8 C13 C14 120.67(16) . . ? N1 C14 C13 115.04(15) . . ? N2 C19 C20 114.01(17) . . ? N3 C20 C19 113.96(17) . . ? N3 C22 C23 113.62(16) . . ? N4 C23 C22 113.51(16) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.82 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.303 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.052 #===END