Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Alcock, N.' 'Boaretto, Rita' 'Kingsley, Andrew J.' 'Roussel, Paul' 'Scott, Peter' _publ_contact_author_name 'Dr Peter Scott' _publ_contact_author_address ; University of Warwick Coventry UNITED KINGDOM ; _publ_contact_author_email 'PETER.SCOTT@WARWICK.AC.UK' _publ_section_title ; Reactivity of a triamidoamine complex of trivalent uranium ; data_unn3op _database_code_CSD 171263 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H75 N7 O P Si3 U' _chemical_formula_weight 903.24 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' '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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.6213(3) _cell_length_b 19.6503(5) _cell_length_c 19.6564(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4488.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description blocks _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 3.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 27147 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.47 _reflns_number_total 10376 _reflns_number_gt 8129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0206P)^2^+0.5214P] 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 0.00021(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(4) _refine_ls_number_reflns 10376 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.038 _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 U1 U 0.082705(16) 0.512841(10) 0.674816(10) 0.02861(6) Uani 1 1 d . . . P1 P 0.33616(12) 0.39662(7) 0.73941(8) 0.0305(3) Uani 1 1 d . . . O1 O 0.2358(3) 0.44161(17) 0.72385(18) 0.0362(9) Uani 1 1 d . . . Si1A Si -0.05742(13) 0.53626(9) 0.83359(9) 0.0383(6) Uani 0.957(4) 1 d P A 1 Si1B Si -0.0924(19) 0.4867(17) 0.8302(12) 0.007(8) Uiso 0.043(4) 1 d P A 2 Si2 Si -0.02524(14) 0.37739(9) 0.56831(9) 0.0403(4) Uani 1 1 d . A 1 Si3 Si 0.26793(16) 0.66181(9) 0.65072(9) 0.0469(5) Uani 1 1 d . A 1 N11 N -0.0720(3) 0.5184(2) 0.74901(18) 0.0356(10) Uani 1 1 d . A 1 N12 N 0.0107(4) 0.4619(2) 0.5757(2) 0.0352(11) Uani 1 1 d . A 1 N13 N 0.1330(4) 0.6275(2) 0.6592(2) 0.0381(12) Uani 1 1 d . A 1 N14 N -0.0965(4) 0.5855(2) 0.6210(2) 0.0324(10) Uani 1 1 d . A 1 N15 N 0.3852(3) 0.4124(2) 0.8159(2) 0.0388(12) Uani 1 1 d . A 1 N16 N 0.3023(4) 0.3158(2) 0.7391(2) 0.0363(11) Uani 1 1 d . A 1 N17 N 0.4385(3) 0.4090(2) 0.6832(2) 0.0391(11) Uani 1 1 d . A 1 C101 C -0.1880(4) 0.5890(3) 0.6724(3) 0.0385(13) Uani 1 1 d . A 1 H10G H -0.2638 0.5925 0.6497 0.046 Uiso 1 1 calc R A 1 H10H H -0.1772 0.6300 0.7010 0.046 Uiso 1 1 calc R A 1 C102 C -0.1846(4) 0.5252(3) 0.7170(3) 0.0402(15) Uani 1 1 d . A 1 H10I H -0.2448 0.5283 0.7524 0.048 Uiso 1 1 calc R A 1 H10J H -0.2005 0.4846 0.6888 0.048 Uiso 1 1 calc R A 1 C103 C -0.1360(5) 0.5498(3) 0.5590(3) 0.0428(15) Uani 1 1 d . A 1 H10K H -0.1664 0.5834 0.5261 0.051 Uiso 1 1 calc R A 1 H10L H -0.1993 0.5183 0.5710 0.051 Uiso 1 1 calc R A 1 C104 C -0.0400(4) 0.5104(3) 0.5265(3) 0.0430(14) Uani 1 1 d . A 1 H10M H -0.0698 0.4852 0.4866 0.052 Uiso 1 1 calc R A 1 H10N H 0.0202 0.5423 0.5105 0.052 Uiso 1 1 calc R A 1 C105 C -0.0509(5) 0.6540(3) 0.6049(3) 0.0426(16) Uani 1 1 d . A 1 H10O H -0.1151 0.6871 0.6038 0.051 Uiso 1 1 calc R A 1 H10P H -0.0148 0.6533 0.5593 0.051 Uiso 1 1 calc R A 1 C106 C 0.0361(5) 0.6764(3) 0.6565(3) 0.0407(16) Uani 1 1 d . A 1 H10Q H 0.0655 0.7221 0.6443 0.049 Uiso 1 1 calc R A 1 H10R H -0.0007 0.6794 0.7018 0.049 Uiso 1 1 calc R A 1 C107 C 0.0975(6) 0.5547(4) 0.8509(3) 0.079(2) Uani 1 1 d . A 1 H10A H 0.1436 0.5141 0.8411 0.118 Uiso 1 1 calc R A 1 H10B H 0.1070 0.5673 0.8988 0.118 Uiso 1 1 calc R A 1 H10C H 0.1231 0.5924 0.8220 0.118 Uiso 1 1 calc R A 1 C108 C -0.1440(6) 0.6126(3) 0.8619(3) 0.065(2) Uani 1 1 d . A 1 H10D H -0.2251 0.6057 0.8500 0.097 Uiso 1 1 calc R A 1 H10E H -0.1151 0.6535 0.8390 0.097 Uiso 1 1 calc R A 1 H10F H -0.1368 0.6181 0.9112 0.097 Uiso 1 1 calc R A 1 C109 C -0.1022(5) 0.4615(3) 0.8889(3) 0.0447(15) Uani 1 1 d . A 1 C110 C -0.2300(5) 0.4436(3) 0.8759(3) 0.0545(17) Uani 1 1 d . A 1 H11A H -0.2531 0.4062 0.9060 0.082 Uiso 1 1 calc R A 1 H11B H -0.2399 0.4297 0.8284 0.082 Uiso 1 1 calc R A 1 H11C H -0.2780 0.4836 0.8851 0.082 Uiso 1 1 calc R A 1 C111 C -0.0829(6) 0.4783(3) 0.9655(3) 0.0641(17) Uani 1 1 d . A 1 H11D H -0.1045 0.4388 0.9932 0.096 Uiso 1 1 calc R A 1 H11E H -0.1304 0.5174 0.9783 0.096 Uiso 1 1 calc R A 1 H11F H -0.0016 0.4891 0.9731 0.096 Uiso 1 1 calc R A 1 C112 C -0.0287(6) 0.3987(3) 0.8696(3) 0.067(2) Uani 1 1 d . A 1 H11G H -0.0460 0.3612 0.9008 0.101 Uiso 1 1 calc R A 1 H11H H 0.0531 0.4103 0.8729 0.101 Uiso 1 1 calc R A 1 H11I H -0.0466 0.3849 0.8229 0.101 Uiso 1 1 calc R A 1 C113 C 0.0153(7) 0.3353(3) 0.6506(3) 0.071(2) Uani 1 1 d . A 1 H11J H -0.0272 0.3566 0.6880 0.107 Uiso 1 1 calc R A 1 H11K H 0.0981 0.3406 0.6583 0.107 Uiso 1 1 calc R A 1 H11L H -0.0039 0.2868 0.6483 0.107 Uiso 1 1 calc R A 1 C114 C -0.1844(5) 0.3634(4) 0.5552(4) 0.066(2) Uani 1 1 d . A 1 H11M H -0.2265 0.3790 0.5955 0.099 Uiso 1 1 calc R A 1 H11N H -0.1992 0.3148 0.5480 0.099 Uiso 1 1 calc R A 1 H11O H -0.2102 0.3891 0.5153 0.099 Uiso 1 1 calc R A 1 C115 C 0.0526(5) 0.3303(3) 0.4963(3) 0.0554(18) Uani 1 1 d . A 1 C116 C 0.0239(7) 0.2539(3) 0.4984(4) 0.080(2) Uani 1 1 d . A 1 H11P H 0.0578 0.2314 0.4586 0.120 Uiso 1 1 calc R A 1 H11Q H -0.0598 0.2479 0.4977 0.120 Uiso 1 1 calc R A 1 H11R H 0.0555 0.2338 0.5400 0.120 Uiso 1 1 calc R A 1 C117 C 0.1806(6) 0.3393(5) 0.5039(5) 0.121(4) Uani 1 1 d . A 1 H11S H 0.2199 0.3168 0.4660 0.182 Uiso 1 1 calc R A 1 H11T H 0.2059 0.3191 0.5469 0.182 Uiso 1 1 calc R A 1 H11U H 0.1992 0.3880 0.5036 0.182 Uiso 1 1 calc R A 1 C118 C 0.0136(8) 0.3575(4) 0.4267(4) 0.090(3) Uani 1 1 d . A 1 H11V H 0.0539 0.3329 0.3905 0.135 Uiso 1 1 calc R A 1 H11W H 0.0317 0.4062 0.4235 0.135 Uiso 1 1 calc R A 1 H11X H -0.0696 0.3510 0.4217 0.135 Uiso 1 1 calc R A 1 C119 C 0.3760(5) 0.6002(4) 0.6860(5) 0.084(3) Uani 1 1 d . A 1 H11Y H 0.3718 0.5573 0.6606 0.126 Uiso 1 1 calc R A 1 H11Z H 0.3592 0.5916 0.7341 0.126 Uiso 1 1 calc R A 1 H12A H 0.4535 0.6194 0.6816 0.126 Uiso 1 1 calc R A 1 C120 C 0.2890(6) 0.7432(3) 0.7000(3) 0.074(2) Uani 1 1 d . A 1 H12B H 0.2651 0.7363 0.7473 0.110 Uiso 1 1 calc R A 1 H12C H 0.2424 0.7794 0.6795 0.110 Uiso 1 1 calc R A 1 H12D H 0.3704 0.7562 0.6987 0.110 Uiso 1 1 calc R A 1 C121 C 0.3073(5) 0.6797(3) 0.5590(3) 0.0501(17) Uani 1 1 d . A 1 C122 C 0.4339(6) 0.7038(4) 0.5506(4) 0.081(2) Uani 1 1 d . A 1 H12E H 0.4530 0.7065 0.5022 0.121 Uiso 1 1 calc R A 1 H12F H 0.4855 0.6713 0.5730 0.121 Uiso 1 1 calc R A 1 H12G H 0.4431 0.7488 0.5715 0.121 Uiso 1 1 calc R A 1 C123 C 0.2273(6) 0.7327(4) 0.5264(4) 0.077(2) Uani 1 1 d . A 1 H12H H 0.2467 0.7379 0.4781 0.116 Uiso 1 1 calc R A 1 H12I H 0.2368 0.7765 0.5495 0.116 Uiso 1 1 calc R A 1 H12J H 0.1472 0.7177 0.5307 0.116 Uiso 1 1 calc R A 1 C124 C 0.2917(6) 0.6130(4) 0.5181(4) 0.077(2) Uani 1 1 d . A 1 H12K H 0.3065 0.6218 0.4698 0.116 Uiso 1 1 calc R A 1 H12L H 0.2128 0.5963 0.5237 0.116 Uiso 1 1 calc R A 1 H12M H 0.3459 0.5787 0.5348 0.116 Uiso 1 1 calc R A 1 C125 C 0.3980(5) 0.4817(3) 0.8402(3) 0.0635(18) Uani 1 1 d . A 1 H12N H 0.3712 0.4845 0.8874 0.095 Uiso 1 1 calc R A 1 H12O H 0.3522 0.5124 0.8118 0.095 Uiso 1 1 calc R A 1 H12P H 0.4792 0.4950 0.8380 0.095 Uiso 1 1 calc R A 1 C126 C 0.4424(5) 0.3620(3) 0.8585(3) 0.0575(18) Uani 1 1 d . A 1 H12Q H 0.4098 0.3634 0.9044 0.086 Uiso 1 1 calc R A 1 H12R H 0.5249 0.3721 0.8606 0.086 Uiso 1 1 calc R A 1 H12S H 0.4311 0.3166 0.8390 0.086 Uiso 1 1 calc R A 1 C127 C 0.2122(5) 0.2912(3) 0.7841(3) 0.0589(19) Uani 1 1 d . A 1 H12T H 0.1523 0.2686 0.7572 0.088 Uiso 1 1 calc R A 1 H12U H 0.1786 0.3296 0.8089 0.088 Uiso 1 1 calc R A 1 H12V H 0.2450 0.2587 0.8166 0.088 Uiso 1 1 calc R A 1 C128 C 0.3620(6) 0.2627(3) 0.7008(4) 0.077(2) Uani 1 1 d . A 1 H12W H 0.3071 0.2392 0.6712 0.116 Uiso 1 1 calc R A 1 H12X H 0.3961 0.2299 0.7326 0.116 Uiso 1 1 calc R A 1 H12Y H 0.4228 0.2833 0.6731 0.116 Uiso 1 1 calc R A 1 C129 C 0.4138(7) 0.4186(4) 0.6116(3) 0.076(2) Uani 1 1 d . A 1 H12Z H 0.4565 0.4582 0.5946 0.114 Uiso 1 1 calc R A 1 H13A H 0.3311 0.4263 0.6055 0.114 Uiso 1 1 calc R A 1 H13B H 0.4371 0.3780 0.5862 0.114 Uiso 1 1 calc R A 1 C130 C 0.5592(5) 0.4016(5) 0.6983(4) 0.094(3) Uani 1 1 d . A 1 H13C H 0.6019 0.4399 0.6788 0.141 Uiso 1 1 calc R A 1 H13D H 0.5876 0.3589 0.6787 0.141 Uiso 1 1 calc R A 1 H13E H 0.5703 0.4008 0.7478 0.141 Uiso 1 1 calc R A 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 U1 0.02787(9) 0.02656(9) 0.03141(9) 0.00325(10) -0.00239(10) -0.00021(9) P1 0.0274(8) 0.0282(8) 0.0359(8) 0.0014(7) -0.0030(7) 0.0003(6) O1 0.033(2) 0.032(2) 0.044(2) 0.0030(18) -0.0079(18) 0.0023(17) Si1A 0.0355(10) 0.0421(12) 0.0374(10) -0.0024(8) 0.0002(8) -0.0043(7) Si2 0.0430(10) 0.0366(11) 0.0412(10) -0.0040(8) -0.0082(8) -0.0018(8) Si3 0.0501(11) 0.0371(10) 0.0535(11) 0.0039(8) 0.0032(9) -0.0129(8) N11 0.031(2) 0.042(3) 0.033(2) 0.010(2) -0.001(2) 0.001(3) N12 0.045(3) 0.032(3) 0.029(2) -0.002(2) -0.005(2) 0.003(2) N13 0.043(3) 0.030(3) 0.041(3) 0.000(2) 0.005(2) -0.006(2) N14 0.035(3) 0.028(3) 0.035(2) 0.003(2) -0.005(2) 0.004(2) N15 0.046(3) 0.036(3) 0.035(3) -0.001(2) -0.011(2) 0.0081(19) N16 0.036(3) 0.024(3) 0.049(3) 0.002(2) 0.004(2) 0.000(2) N17 0.033(3) 0.045(3) 0.040(3) 0.001(2) 0.001(2) -0.002(2) C101 0.031(3) 0.042(3) 0.043(3) -0.001(4) -0.006(3) 0.005(2) C102 0.035(3) 0.047(4) 0.039(3) -0.008(3) 0.001(2) -0.006(3) C103 0.046(4) 0.045(4) 0.037(3) -0.001(3) -0.013(3) 0.010(3) C104 0.055(3) 0.044(4) 0.031(3) -0.011(3) -0.001(3) 0.006(3) C105 0.055(4) 0.034(4) 0.039(3) 0.009(3) 0.007(3) 0.012(3) C106 0.046(3) 0.030(3) 0.047(4) 0.004(3) 0.013(3) -0.002(3) C107 0.060(5) 0.129(7) 0.047(4) -0.007(4) -0.007(4) -0.033(5) C108 0.094(6) 0.045(4) 0.056(4) -0.006(4) 0.012(4) 0.006(4) C109 0.050(4) 0.049(4) 0.035(3) 0.004(3) 0.005(3) 0.007(3) C110 0.055(4) 0.050(4) 0.058(4) 0.016(3) 0.000(3) -0.010(3) C111 0.072(4) 0.085(5) 0.035(3) 0.001(3) 0.001(3) 0.006(5) C112 0.097(6) 0.052(5) 0.054(4) 0.002(4) -0.006(4) 0.027(4) C113 0.110(6) 0.044(4) 0.060(5) 0.016(4) -0.028(4) -0.016(4) C114 0.048(4) 0.069(5) 0.081(5) -0.013(4) 0.001(4) -0.011(4) C115 0.052(5) 0.041(4) 0.073(5) -0.022(4) -0.006(3) 0.003(3) C116 0.110(7) 0.040(4) 0.090(6) -0.017(4) -0.008(5) 0.014(4) C117 0.058(5) 0.134(8) 0.171(10) -0.100(8) 0.002(6) 0.003(5) C118 0.157(8) 0.058(5) 0.055(5) -0.010(4) 0.025(5) 0.009(5) C119 0.047(4) 0.075(5) 0.130(8) 0.042(6) -0.008(5) -0.014(3) C120 0.090(6) 0.064(5) 0.067(5) -0.018(4) 0.007(4) -0.033(4) C121 0.050(4) 0.036(4) 0.064(5) -0.002(3) 0.019(3) -0.006(3) C122 0.074(6) 0.082(6) 0.086(6) -0.009(4) 0.032(5) -0.034(5) C123 0.090(6) 0.082(6) 0.060(5) 0.029(4) 0.025(5) 0.000(5) C124 0.070(5) 0.089(6) 0.073(5) -0.020(5) 0.028(4) -0.022(4) C125 0.074(4) 0.054(4) 0.063(4) -0.014(4) -0.027(3) 0.008(4) C126 0.059(5) 0.065(5) 0.048(4) 0.007(3) -0.016(3) 0.012(3) C127 0.054(4) 0.047(4) 0.076(5) 0.013(4) 0.014(4) -0.006(3) C128 0.082(5) 0.044(5) 0.106(7) -0.015(4) 0.023(5) -0.002(4) C129 0.078(5) 0.103(6) 0.048(4) 0.000(4) 0.010(5) 0.019(5) C130 0.031(4) 0.177(9) 0.075(5) 0.016(5) 0.011(4) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N11 2.318(4) . y U1 N12 2.345(4) . y U1 N13 2.347(4) . y U1 O1 2.460(3) . y U1 N14 2.738(4) . y P1 O1 1.495(4) . y P1 N16 1.636(4) . ? P1 N15 1.637(5) . ? P1 N17 1.641(4) . ? Si1A N11 1.707(4) . y Si1A C107 1.868(6) . ? Si1A C108 1.890(6) . ? Si1A C109 1.901(6) . ? Si2 N12 1.718(5) . y Si2 C113 1.876(6) . ? Si2 C114 1.888(6) . ? Si2 C115 1.918(6) . ? Si3 N13 1.715(4) . y Si3 C120 1.885(6) . ? Si3 C119 1.878(7) . ? Si3 C121 1.893(6) . ? N11 C102 1.458(6) . ? N12 C104 1.480(6) . ? N13 C106 1.481(6) . ? N14 C101 1.468(7) . ? N14 C105 1.481(6) . ? N14 C103 1.480(6) . ? N15 C125 1.451(7) . ? N15 C126 1.458(6) . ? N16 C127 1.454(6) . ? N16 C128 1.461(7) . ? N17 C130 1.442(7) . ? N17 C129 1.450(7) . ? C101 C102 1.530(7) . ? C103 C104 1.501(7) . ? C105 C106 1.497(7) . ? C109 C110 1.548(8) . ? C109 C112 1.547(8) . ? C109 C111 1.557(7) . ? C115 C117 1.505(9) . ? C115 C116 1.537(9) . ? C115 C118 1.539(9) . ? C121 C123 1.537(9) . ? C121 C124 1.548(8) . ? C121 C122 1.555(9) . ? 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 N11 U1 N12 105.43(14) . . y N11 U1 N13 103.29(15) . . y N12 U1 N13 112.97(15) . . y N11 U1 O1 109.96(13) . . y N12 U1 O1 109.92(13) . . y N13 U1 O1 114.65(13) . . y N11 U1 N14 68.18(13) . . y N12 U1 N14 68.30(13) . . y N13 U1 N14 68.79(14) . . y O1 U1 N14 176.53(12) . . y O1 P1 N16 112.7(2) . . y O1 P1 N15 110.3(2) . . y N16 P1 N15 105.7(2) . . ? O1 P1 N17 109.9(2) . . y N16 P1 N17 108.4(2) . . ? N15 P1 N17 109.7(2) . . ? P1 O1 U1 168.7(2) . . y N11 Si1A C107 108.3(2) . . ? N11 Si1A C108 113.3(3) . . ? C107 Si1A C108 107.8(3) . . ? N11 Si1A C109 111.8(2) . . ? C107 Si1A C109 108.0(3) . . ? C108 Si1A C109 107.4(3) . . ? N12 Si2 C113 107.0(3) . . ? N12 Si2 C114 113.0(3) . . ? C113 Si2 C114 107.4(3) . . ? N12 Si2 C115 114.5(3) . . ? C113 Si2 C115 107.7(3) . . ? C114 Si2 C115 106.9(3) . . ? N13 Si3 C120 113.7(3) . . ? N13 Si3 C119 108.8(3) . . ? C120 Si3 C119 105.7(4) . . ? N13 Si3 C121 112.7(3) . . ? C120 Si3 C121 107.5(3) . . ? C119 Si3 C121 108.0(3) . . ? C102 N11 Si1A 119.4(3) . . ? C102 N11 U1 115.4(3) . . ? Si1A N11 U1 123.0(2) . . ? C104 N12 Si2 118.1(3) . . ? C104 N12 U1 114.2(3) . . ? Si2 N12 U1 124.7(2) . . ? C106 N13 Si3 115.9(3) . . ? C106 N13 U1 116.0(3) . . ? Si3 N13 U1 128.2(2) . . ? C101 N14 C105 111.3(4) . . ? C101 N14 C103 111.3(4) . . ? C105 N14 C103 111.5(4) . . ? C101 N14 U1 108.0(3) . . ? C105 N14 U1 106.5(3) . . ? C103 N14 U1 107.8(3) . . ? C125 N15 C126 113.6(4) . . ? C125 N15 P1 121.1(4) . . ? C126 N15 P1 123.9(4) . . ? C127 N16 C128 114.7(5) . . ? C127 N16 P1 119.6(4) . . ? C128 N16 P1 125.5(4) . . ? C130 N17 C129 113.9(5) . . ? C130 N17 P1 123.5(4) . . ? C129 N17 P1 122.0(4) . . ? N14 C101 C102 109.7(4) . . ? N11 C102 C101 110.2(4) . . ? N14 C103 C104 111.4(4) . . ? N12 C104 C103 110.5(4) . . ? N14 C105 C106 111.4(4) . . ? N13 C106 C105 110.3(5) . . ? C110 C109 C112 108.0(5) . . ? C110 C109 C111 110.3(5) . . ? C112 C109 C111 109.1(5) . . ? C110 C109 Si1A 110.1(4) . . ? C112 C109 Si1A 108.9(4) . . ? C111 C109 Si1A 110.5(4) . . ? C117 C115 C116 109.1(6) . . ? C117 C115 C118 109.7(7) . . ? C116 C115 C118 107.4(6) . . ? C117 C115 Si2 109.7(5) . . ? C116 C115 Si2 110.5(5) . . ? C118 C115 Si2 110.4(4) . . ? C123 C121 C124 106.7(6) . . ? C123 C121 C122 108.8(6) . . ? C124 C121 C122 108.3(5) . . ? C123 C121 Si3 112.2(4) . . ? C124 C121 Si3 108.0(4) . . ? C122 C121 Si3 112.7(5) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.517 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.111 data_unplat _database_code_CSD 171264 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H69 N4 O P Si3 U' _chemical_formula_weight 831.14 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' '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' 'U' 'U' -9.6767 9.6646 '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 11.5920(3) _cell_length_b 12.4323(2) _cell_length_c 13.6752(3) _cell_angle_alpha 89.4280(10) _cell_angle_beta 87.7850(10) _cell_angle_gamma 84.1600(10) _cell_volume 1959.07(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 54 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max .08 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 4.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.496634 _exptl_absorpt_correction_T_max 0.927989 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11548 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8248 _reflns_number_gt 6791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^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 8248 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.14369(3) 0.11671(3) 0.25927(3) 0.01773(12) Uani 1 d . . . O1 O 0.1074(6) 0.1083(5) 0.1071(4) 0.0169(14) Uani 1 d . . . H1A H 0.1399 0.1562 0.0759 0.025 Uiso 1 calc R . . Si11 Si -0.1384(3) 0.2778(2) 0.3067(2) 0.0251(6) Uani 1 d . . . Si12 Si 0.3273(3) 0.3043(2) 0.1361(2) 0.0284(7) Uani 1 d . . . Si13 Si 0.3911(3) -0.0819(2) 0.2445(2) 0.0253(6) Uani 1 d . . . P1 P -0.0615(2) -0.1038(2) 0.18853(19) 0.0242(6) Uani 1 d . . . N1 N -0.0126(8) 0.2068(7) 0.3427(6) 0.026(2) Uani 1 d . . . N2 N 0.2498(8) 0.2629(7) 0.2367(6) 0.028(2) Uani 1 d . . . N3 N 0.2942(8) -0.0008(7) 0.3180(6) 0.027(2) Uani 1 d . . . N4 N 0.2024(8) 0.1763(7) 0.4322(6) 0.028(2) Uani 1 d . . . C1 C 0.1017(10) 0.2277(9) 0.4874(7) 0.030(3) Uani 1 d . . . H1B H 0.0963 0.3072 0.4782 0.036 Uiso 1 calc R . . H1C H 0.1086 0.2114 0.5580 0.036 Uiso 1 calc R . . C2 C -0.0051(10) 0.1839(9) 0.4499(7) 0.033(3) Uani 1 d . . . H2A H -0.0009 0.1049 0.4618 0.039 Uiso 1 calc R . . H2B H -0.0753 0.2183 0.4851 0.039 Uiso 1 calc R . . C3 C 0.2922(11) 0.2522(10) 0.4138(8) 0.037(3) Uani 1 d . . . H3A H 0.3684 0.2106 0.4000 0.045 Uiso 1 calc R . . H3B H 0.2985 0.2963 0.4729 0.045 Uiso 1 calc R . . C4 C 0.2609(11) 0.3262(9) 0.3273(8) 0.033(3) Uani 1 d . . . H4A H 0.1866 0.3704 0.3428 0.040 Uiso 1 calc R . . H4B H 0.3217 0.3759 0.3160 0.040 Uiso 1 calc R . . C5 C 0.2480(11) 0.0755(9) 0.4820(8) 0.037(3) Uani 1 d . . . H5A H 0.1828 0.0329 0.5004 0.045 Uiso 1 calc R . . H5B H 0.2850 0.0940 0.5428 0.045 Uiso 1 calc R . . C6 C 0.3348(10) 0.0080(10) 0.4185(8) 0.034(3) Uani 1 d . . . H6A H 0.4092 0.0408 0.4160 0.041 Uiso 1 calc R . . H6B H 0.3489 -0.0652 0.4475 0.041 Uiso 1 calc R . . C7 C -0.1315(11) 0.2881(10) 0.1681(7) 0.036(3) Uani 1 d . . . H7A H -0.1176 0.2155 0.1401 0.054 Uiso 1 calc R . . H7B H -0.0681 0.3306 0.1471 0.054 Uiso 1 calc R . . H7C H -0.2051 0.3237 0.1455 0.054 Uiso 1 calc R . . C8 C -0.2669(11) 0.2056(10) 0.3483(9) 0.044(3) Uani 1 d . . . H8A H -0.2561 0.1308 0.3251 0.066 Uiso 1 calc R . . H8B H -0.3376 0.2425 0.3215 0.066 Uiso 1 calc R . . H8C H -0.2739 0.2059 0.4200 0.066 Uiso 1 calc R . . C9 C -0.1654(12) 0.4256(9) 0.3539(9) 0.040(3) Uani 1 d . . . C10 C -0.1795(15) 0.4303(10) 0.4651(9) 0.058(4) Uani 1 d . . . H10A H -0.1930 0.5059 0.4858 0.086 Uiso 1 calc R . . H10B H -0.1088 0.3962 0.4941 0.086 Uiso 1 calc R . . H10C H -0.2457 0.3918 0.4868 0.086 Uiso 1 calc R . . C11 C -0.0658(12) 0.4915(10) 0.3203(11) 0.049(3) Uani 1 d . . . H11A H -0.0810 0.5653 0.3454 0.074 Uiso 1 calc R . . H11B H -0.0602 0.4935 0.2487 0.074 Uiso 1 calc R . . H11C H 0.0072 0.4576 0.3455 0.074 Uiso 1 calc R . . C12 C -0.2769(13) 0.4810(11) 0.3102(11) 0.061(5) Uani 1 d . . . H12A H -0.2912 0.5552 0.3345 0.091 Uiso 1 calc R . . H12B H -0.3426 0.4408 0.3297 0.091 Uiso 1 calc R . . H12C H -0.2678 0.4821 0.2387 0.091 Uiso 1 calc R . . C13 C 0.3513(12) 0.1954(9) 0.0430(8) 0.040(3) Uani 1 d . . . H13A H 0.2762 0.1753 0.0228 0.061 Uiso 1 calc R . . H13B H 0.3959 0.1322 0.0711 0.061 Uiso 1 calc R . . H13C H 0.3945 0.2215 -0.0140 0.061 Uiso 1 calc R . . C14 C 0.4770(11) 0.3373(12) 0.1682(11) 0.057(4) Uani 1 d . . . H14A H 0.5177 0.2751 0.2012 0.086 Uiso 1 calc R . . H14B H 0.4700 0.4000 0.2117 0.086 Uiso 1 calc R . . H14C H 0.5209 0.3541 0.1082 0.086 Uiso 1 calc R . . C15 C 0.2520(10) 0.4277(9) 0.0727(8) 0.032(3) Uani 1 d . . . C16 C 0.3318(13) 0.4741(12) -0.0049(11) 0.063(5) Uani 1 d . . . H16A H 0.2904 0.5371 -0.0361 0.094 Uiso 1 calc R . . H16B H 0.3557 0.4190 -0.0544 0.094 Uiso 1 calc R . . H16C H 0.4006 0.4958 0.0261 0.094 Uiso 1 calc R . . C17 C 0.2152(18) 0.5160(12) 0.1454(12) 0.078(6) Uani 1 d . . . H17A H 0.1768 0.5787 0.1113 0.116 Uiso 1 calc R . . H17B H 0.2837 0.5372 0.1773 0.116 Uiso 1 calc R . . H17C H 0.1613 0.4897 0.1948 0.116 Uiso 1 calc R . . C18 C 0.1444(13) 0.3991(12) 0.0246(12) 0.064(5) Uani 1 d . . . H18A H 0.1069 0.4633 -0.0077 0.097 Uiso 1 calc R . . H18B H 0.0907 0.3729 0.0744 0.097 Uiso 1 calc R . . H18C H 0.1658 0.3424 -0.0239 0.097 Uiso 1 calc R . . C19 C 0.5360(9) -0.0248(10) 0.2311(9) 0.039(3) Uani 1 d . . . H19A H 0.5243 0.0501 0.2076 0.059 Uiso 1 calc R . . H19B H 0.5865 -0.0682 0.1842 0.059 Uiso 1 calc R . . H19C H 0.5723 -0.0266 0.2947 0.059 Uiso 1 calc R . . C20 C 0.3320(10) -0.0887(10) 0.1190(7) 0.037(3) Uani 1 d . . . H20A H 0.3156 -0.0154 0.0927 0.055 Uiso 1 calc R . . H20B H 0.2603 -0.1244 0.1229 0.055 Uiso 1 calc R . . H20C H 0.3893 -0.1301 0.0758 0.055 Uiso 1 calc R . . C21 C 0.4205(9) -0.2282(9) 0.2907(8) 0.029(2) Uani 1 d . . . C22 C 0.4803(10) -0.2980(9) 0.2083(8) 0.033(3) Uani 1 d . . . H22A H 0.4957 -0.3727 0.2316 0.050 Uiso 1 calc R . . H22B H 0.5537 -0.2700 0.1883 0.050 Uiso 1 calc R . . H22C H 0.4298 -0.2960 0.1524 0.050 Uiso 1 calc R . . C23 C 0.5007(11) -0.2390(10) 0.3780(9) 0.042(3) Uani 1 d . . . H23A H 0.5128 -0.3150 0.3983 0.063 Uiso 1 calc R . . H23B H 0.4650 -0.1955 0.4325 0.063 Uiso 1 calc R . . H23C H 0.5756 -0.2135 0.3587 0.063 Uiso 1 calc R . . C24 C 0.3050(11) -0.2704(10) 0.3206(9) 0.041(3) Uani 1 d . . . H24A H 0.3192 -0.3451 0.3443 0.062 Uiso 1 calc R . . H24B H 0.2556 -0.2683 0.2639 0.062 Uiso 1 calc R . . H24C H 0.2662 -0.2250 0.3727 0.062 Uiso 1 calc R . . C25 C 0.0128(10) -0.0509(9) 0.2804(8) 0.033(3) Uani 1 d . . . H25A H 0.0645 -0.1119 0.3064 0.040 Uiso 1 calc R . . H25B H -0.0457 -0.0301 0.3333 0.040 Uiso 1 calc R . . C26 C 0.0367(11) -0.1679(11) 0.0970(8) 0.041(3) Uani 1 d . . . H26A H 0.0923 -0.1177 0.0749 0.062 Uiso 1 calc R . . H26B H -0.0072 -0.1881 0.0414 0.062 Uiso 1 calc R . . H26C H 0.0785 -0.2328 0.1249 0.062 Uiso 1 calc R . . C27 C -0.1502(11) -0.0010(9) 0.1280(9) 0.039(3) Uani 1 d . . . H27A H -0.1031 0.0566 0.1063 0.059 Uiso 1 calc R . . H27B H -0.2128 0.0289 0.1731 0.059 Uiso 1 calc R . . H27C H -0.1836 -0.0317 0.0711 0.059 Uiso 1 calc R . . C28 C -0.1595(11) -0.2034(10) 0.2242(9) 0.041(3) Uani 1 d . . . H28A H -0.1165 -0.2638 0.2580 0.062 Uiso 1 calc R . . H28B H -0.1933 -0.2302 0.1657 0.062 Uiso 1 calc R . . H28C H -0.2215 -0.1700 0.2680 0.062 Uiso 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 U1 0.0195(2) 0.01832(19) 0.01469(18) -0.00090(12) -0.00316(12) 0.00264(13) O1 0.023(4) 0.024(4) 0.005(3) -0.001(2) -0.001(2) -0.004(3) Si11 0.0267(16) 0.0234(15) 0.0234(14) 0.0001(12) 0.0004(12) 0.0061(12) Si12 0.0257(16) 0.0290(16) 0.0301(15) 0.0063(13) -0.0027(13) -0.0014(12) Si13 0.0227(15) 0.0244(15) 0.0276(15) 0.0010(12) -0.0026(12) 0.0033(12) P1 0.0244(15) 0.0276(14) 0.0210(12) -0.0010(11) -0.0049(11) -0.0035(11) N1 0.028(5) 0.028(5) 0.020(4) 0.002(4) -0.003(4) 0.011(4) N2 0.034(5) 0.024(5) 0.027(5) -0.004(4) -0.011(4) -0.003(4) N3 0.033(5) 0.028(5) 0.020(4) -0.003(4) -0.010(4) 0.006(4) N4 0.039(6) 0.024(5) 0.020(4) -0.004(4) -0.007(4) 0.006(4) C1 0.037(7) 0.031(6) 0.020(5) -0.004(4) -0.009(5) 0.009(5) C2 0.037(7) 0.035(6) 0.022(5) 0.004(5) 0.011(5) 0.007(5) C3 0.046(8) 0.036(7) 0.031(6) -0.008(5) -0.018(5) -0.005(5) C4 0.047(8) 0.025(6) 0.029(6) -0.003(5) -0.002(5) -0.012(5) C5 0.049(8) 0.037(7) 0.023(5) -0.005(5) -0.013(5) 0.015(6) C6 0.038(7) 0.036(7) 0.026(6) -0.005(5) -0.006(5) 0.013(5) C7 0.038(7) 0.045(7) 0.023(5) 0.006(5) -0.005(5) 0.008(5) C8 0.034(7) 0.047(8) 0.048(7) 0.006(6) 0.003(6) 0.010(6) C9 0.054(8) 0.026(6) 0.036(6) -0.002(5) -0.006(6) 0.015(6) C10 0.096(12) 0.029(7) 0.042(7) -0.017(6) 0.004(8) 0.020(7) C11 0.048(9) 0.027(7) 0.072(9) 0.000(6) -0.016(7) 0.001(6) C12 0.050(9) 0.048(9) 0.079(11) -0.025(8) -0.029(8) 0.030(7) C13 0.055(9) 0.030(6) 0.033(6) -0.001(5) 0.007(6) 0.005(6) C14 0.032(8) 0.062(10) 0.080(11) 0.024(8) -0.017(7) -0.015(6) C15 0.034(7) 0.030(6) 0.031(6) 0.005(5) -0.004(5) 0.002(5) C16 0.049(9) 0.063(10) 0.073(10) 0.049(8) 0.012(7) 0.004(7) C17 0.122(17) 0.042(9) 0.063(10) 0.001(8) 0.000(10) 0.020(10) C18 0.048(9) 0.053(9) 0.093(12) 0.015(8) -0.035(9) 0.003(7) C19 0.017(6) 0.045(7) 0.054(8) 0.002(6) -0.002(5) 0.001(5) C20 0.029(7) 0.054(8) 0.025(5) 0.014(5) -0.002(5) 0.003(5) C21 0.024(6) 0.031(6) 0.029(5) -0.006(5) -0.006(4) 0.013(5) C22 0.037(7) 0.026(6) 0.035(6) 0.000(5) 0.000(5) 0.007(5) C23 0.044(8) 0.037(7) 0.041(7) 0.011(6) -0.010(6) 0.017(6) C24 0.055(9) 0.033(7) 0.035(6) 0.000(5) 0.008(6) -0.006(6) C25 0.040(7) 0.033(6) 0.025(5) -0.007(5) -0.015(5) 0.004(5) C26 0.040(7) 0.051(8) 0.032(6) -0.013(6) -0.004(5) 0.002(6) C27 0.046(8) 0.034(7) 0.039(7) 0.002(5) -0.016(6) 0.000(5) C28 0.037(7) 0.051(8) 0.039(7) 0.007(6) -0.008(6) -0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.145(6) . ? U1 N1 2.301(8) . ? U1 N2 2.308(9) . ? U1 N3 2.322(8) . ? U1 N4 2.620(8) . ? U1 C25 2.706(12) . ? Si11 N1 1.712(9) . ? Si11 C8 1.882(14) . ? Si11 C7 1.898(11) . ? Si11 C9 1.945(12) . ? Si12 N2 1.717(10) . ? Si12 C13 1.861(11) . ? Si12 C14 1.892(13) . ? Si12 C15 1.905(11) . ? Si13 N3 1.730(9) . ? Si13 C20 1.879(11) . ? Si13 C19 1.891(12) . ? Si13 C21 1.921(11) . ? P1 C25 1.723(11) . ? P1 C27 1.776(11) . ? P1 C26 1.794(11) . ? P1 C28 1.814(12) . ? N1 C2 1.494(12) . ? N2 C4 1.492(13) . ? N3 C6 1.478(13) . ? N4 C1 1.460(13) . ? N4 C5 1.481(13) . ? N4 C3 1.487(15) . ? C1 C2 1.512(16) . ? C3 C4 1.523(15) . ? C5 C6 1.498(14) . ? C9 C10 1.524(16) . ? C9 C11 1.535(19) . ? C9 C12 1.540(17) . ? C15 C17 1.507(18) . ? C15 C18 1.507(18) . ? C15 C16 1.527(16) . ? C21 C24 1.526(17) . ? C21 C22 1.529(14) . ? C21 C23 1.538(15) . ? 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 U1 N1 109.6(3) . . ? O1 U1 N2 93.3(3) . . ? N1 U1 N2 97.0(3) . . ? O1 U1 N3 118.0(3) . . ? N1 U1 N3 129.5(3) . . ? N2 U1 N3 96.2(3) . . ? O1 U1 N4 165.3(3) . . ? N1 U1 N4 69.2(3) . . ? N2 U1 N4 72.5(3) . . ? N3 U1 N4 68.9(3) . . ? O1 U1 C25 84.9(3) . . ? N1 U1 C25 82.1(3) . . ? N2 U1 C25 177.6(3) . . ? N3 U1 C25 86.0(3) . . ? N4 U1 C25 109.2(3) . . ? N1 Si11 C8 110.0(5) . . ? N1 Si11 C7 108.0(5) . . ? C8 Si11 C7 109.8(6) . . ? N1 Si11 C9 115.4(5) . . ? C8 Si11 C9 107.6(6) . . ? C7 Si11 C9 105.9(5) . . ? N2 Si12 C13 111.1(5) . . ? N2 Si12 C14 112.0(6) . . ? C13 Si12 C14 105.7(7) . . ? N2 Si12 C15 113.1(5) . . ? C13 Si12 C15 106.8(5) . . ? C14 Si12 C15 107.8(6) . . ? N3 Si13 C20 109.3(5) . . ? N3 Si13 C19 111.3(5) . . ? C20 Si13 C19 107.7(6) . . ? N3 Si13 C21 114.3(5) . . ? C20 Si13 C21 106.8(5) . . ? C19 Si13 C21 107.2(5) . . ? C25 P1 C27 111.2(6) . . ? C25 P1 C26 111.1(6) . . ? C27 P1 C26 106.7(6) . . ? C25 P1 C28 116.9(6) . . ? C27 P1 C28 104.4(6) . . ? C26 P1 C28 105.7(6) . . ? C2 N1 Si11 116.0(7) . . ? C2 N1 U1 109.9(6) . . ? Si11 N1 U1 133.5(4) . . ? C4 N2 Si12 114.8(7) . . ? C4 N2 U1 114.1(7) . . ? Si12 N2 U1 130.9(4) . . ? C6 N3 Si13 112.3(7) . . ? C6 N3 U1 121.7(6) . . ? Si13 N3 U1 124.1(4) . . ? C1 N4 C5 110.1(9) . . ? C1 N4 C3 111.6(9) . . ? C5 N4 C3 112.8(9) . . ? C1 N4 U1 110.7(6) . . ? C5 N4 U1 105.5(6) . . ? C3 N4 U1 105.9(6) . . ? N4 C1 C2 107.8(8) . . ? N1 C2 C1 109.4(9) . . ? N4 C3 C4 110.5(9) . . ? N2 C4 C3 111.4(9) . . ? N4 C5 C6 112.0(9) . . ? N3 C6 C5 111.6(9) . . ? C10 C9 C11 109.0(12) . . ? C10 C9 C12 108.3(11) . . ? C11 C9 C12 107.0(11) . . ? C10 C9 Si11 112.0(8) . . ? C11 C9 Si11 111.0(8) . . ? C12 C9 Si11 109.3(9) . . ? C17 C15 C18 107.5(13) . . ? C17 C15 C16 107.5(12) . . ? C18 C15 C16 108.8(11) . . ? C17 C15 Si12 110.7(9) . . ? C18 C15 Si12 110.5(9) . . ? C16 C15 Si12 111.6(8) . . ? C24 C21 C22 109.5(10) . . ? C24 C21 C23 109.2(10) . . ? C22 C21 C23 107.1(9) . . ? C24 C21 Si13 108.9(7) . . ? C22 C21 Si13 109.1(8) . . ? C23 C21 Si13 113.0(8) . . ? P1 C25 U1 125.2(6) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 3.624 _refine_diff_density_min -3.087 _refine_diff_density_rms 0.225