Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Barbara Gehrhus' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email B.GEHRHUS@SUSSEX.AC.UK _publ_section_title ; Insights into the making of a stable silylene ; _publ_requested_category FM loop_ _publ_author_name 'Barbara Gehrhus' 'P. B. Hitchcock' 'Ruti Pongtavornpinyo' 'Lihong Zhang' data_(6a)-nov1702 _database_code_depnum_ccdc_archive 'CCDC 286727' _audit_creation_date 2002-11-14T09:56:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (K(dme)4)((Si(NEt)2C6H4)4).(dme) _chemical_formula_moiety 'C40 H56 N8 Si4, C16 H40 K O8, C4 H10 O2' _chemical_formula_sum 'C60 H106 K N8 O10 Si4' _chemical_formula_weight 1250.99 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.7940(4) _cell_length_b 18.5198(4) _cell_length_c 20.7545(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7223.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 145333 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.15 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.1275 _diffrn_reflns_av_unetI/netI 0.0774 _diffrn_reflns_number 45950 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 9942 _reflns_number_gt 7976 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0383P)^2^+4.4077P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 9942 _refine_ls_number_parameters 749 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(6) _refine_diff_density_max 0.28 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.22873(5) 0.24432(6) 0.39179(6) 0.0497(3) Uani 1 1 d . . . Si1 Si 0.10156(6) -0.20396(6) 0.38400(6) 0.0299(3) Uani 1 1 d . . . Si2 Si 0.14608(6) -0.19876(6) 0.48996(6) 0.0290(3) Uani 1 1 d . . . Si3 Si 0.14566(6) -0.32532(6) 0.49548(6) 0.0303(3) Uani 1 1 d . . . Si4 Si 0.10785(5) -0.33039(6) 0.38752(6) 0.0302(3) Uani 1 1 d . . . O1 O 0.1994(3) 0.2421(2) 0.52148(19) 0.0928(15) Uani 1 1 d . . . O2 O 0.1655(2) 0.3662(2) 0.4532(2) 0.0772(12) Uani 1 1 d . . . O3 O 0.2785(3) 0.3417(2) 0.2971(2) 0.1005(16) Uani 1 1 d . . . O4 O 0.2479(3) 0.2052(3) 0.2542(2) 0.1048(17) Uani 1 1 d . . . O5 O 0.3470(3) 0.1571(3) 0.4043(3) 0.1228(19) Uani 1 1 d . . . O6 O 0.3613(3) 0.2950(3) 0.4504(4) 0.142(3) Uani 1 1 d . . . O7 O 0.1565(2) 0.1027(2) 0.40560(18) 0.0707(11) Uani 1 1 d . . . O8 O 0.0868(2) 0.2235(2) 0.3535(2) 0.0746(12) Uani 1 1 d . . . O9 O -0.0102(3) -0.2163(3) 0.1200(3) 0.125(2) Uani 1 1 d . . . O10 O 0.0681(3) -0.3463(3) 0.1092(3) 0.1029(15) Uani 1 1 d . . . N1 N 0.01865(17) -0.16440(19) 0.36508(16) 0.0353(9) Uani 1 1 d . . . N2 N 0.14137(16) -0.1470(2) 0.32589(18) 0.0348(9) Uani 1 1 d . . . N3 N 0.10155(18) -0.13901(19) 0.54289(17) 0.0351(9) Uani 1 1 d . . . N4 N 0.22690(17) -0.15536(18) 0.50963(16) 0.0329(8) Uani 1 1 d . . . N5 N 0.21890(18) -0.38078(19) 0.51598(18) 0.0391(9) Uani 1 1 d . . . N6 N 0.09687(19) -0.3664(2) 0.55848(17) 0.0394(10) Uani 1 1 d . . . N7 N 0.15861(18) -0.3762(2) 0.32884(18) 0.0355(9) Uani 1 1 d . . . N8 N 0.03579(17) -0.38794(19) 0.36920(18) 0.0408(10) Uani 1 1 d . . . C1 C 0.0238(2) -0.1081(2) 0.3217(2) 0.0346(10) Uani 1 1 d . . . C2 C 0.0944(2) -0.0972(2) 0.2989(2) 0.0347(11) Uani 1 1 d . . . C3 C 0.1080(3) -0.0442(3) 0.2547(2) 0.0467(12) Uani 1 1 d . . . H3 H 0.1544 -0.0381 0.2388 0.056 Uiso 1 1 calc R . . C4 C 0.0537(3) 0.0005(3) 0.2331(2) 0.0549(14) Uani 1 1 d . . . H4 H 0.0635 0.0366 0.2025 0.066 Uiso 1 1 calc R . . C5 C -0.0144(3) -0.0080(3) 0.2563(3) 0.0552(14) Uani 1 1 d . . . H5 H -0.0507 0.0231 0.2422 0.066 Uiso 1 1 calc R . . C6 C -0.0299(2) -0.0622(3) 0.3005(2) 0.0440(12) Uani 1 1 d . . . H6 H -0.0765 -0.0678 0.316 0.053 Uiso 1 1 calc R . . C7 C -0.0512(2) -0.1912(3) 0.3847(3) 0.0466(12) Uani 1 1 d . . . H7A H -0.081 -0.1501 0.3973 0.056 Uiso 1 1 calc R . . H7B H -0.0455 -0.2222 0.4226 0.056 Uiso 1 1 calc R . . C8 C -0.0886(3) -0.2330(3) 0.3327(3) 0.0619(16) Uani 1 1 d . . . H8A H -0.1345 -0.2492 0.3485 0.093 Uiso 1 1 calc R . . H8B H -0.06 -0.2745 0.3207 0.093 Uiso 1 1 calc R . . H8C H -0.0955 -0.2022 0.2954 0.093 Uiso 1 1 calc R . . C9 C 0.2178(2) -0.1424(3) 0.3107(2) 0.0442(12) Uani 1 1 d . . . H9A H 0.2236 -0.1395 0.2639 0.053 Uiso 1 1 calc R . . H9B H 0.2412 -0.1867 0.3254 0.053 Uiso 1 1 calc R . . C10 C 0.2542(3) -0.0784(3) 0.3413(3) 0.0611(16) Uani 1 1 d . . . H10A H 0.3042 -0.0786 0.3298 0.092 Uiso 1 1 calc R . . H10B H 0.2495 -0.0813 0.3878 0.092 Uiso 1 1 calc R . . H10C H 0.2323 -0.0342 0.3261 0.092 Uiso 1 1 calc R . . C11 C 0.1471(2) -0.0890(2) 0.5714(2) 0.0334(11) Uani 1 1 d . . . C12 C 0.2188(2) -0.0981(2) 0.5524(2) 0.0324(10) Uani 1 1 d . . . C13 C 0.2702(2) -0.0513(2) 0.5754(2) 0.0419(11) Uani 1 1 d . . . H13 H 0.318 -0.0572 0.5631 0.05 Uiso 1 1 calc R . . C14 C 0.2509(3) 0.0046(3) 0.6170(2) 0.0489(13) Uani 1 1 d . . . H14 H 0.2856 0.0371 0.6318 0.059 Uiso 1 1 calc R . . C15 C 0.1818(3) 0.0122(3) 0.6363(2) 0.0505(13) Uani 1 1 d . . . H15 H 0.1696 0.0492 0.6653 0.061 Uiso 1 1 calc R . . C16 C 0.1294(2) -0.0343(2) 0.6135(2) 0.0384(11) Uani 1 1 d . . . H16 H 0.0819 -0.0284 0.6267 0.046 Uiso 1 1 calc R . . C17 C 0.0251(2) -0.1293(3) 0.5488(3) 0.0450(12) Uani 1 1 d . . . H17A H 0.0131 -0.1237 0.5945 0.054 Uiso 1 1 calc R . . H17B H 0.0012 -0.1729 0.5331 0.054 Uiso 1 1 calc R . . C18 C -0.0032(2) -0.0647(3) 0.5121(3) 0.0582(15) Uani 1 1 d . . . H18A H -0.0543 -0.0611 0.5185 0.087 Uiso 1 1 calc R . . H18B H 0.0069 -0.0705 0.4666 0.087 Uiso 1 1 calc R . . H18C H 0.0195 -0.0211 0.5278 0.087 Uiso 1 1 calc R . . C19 C 0.2977(2) -0.1798(2) 0.4912(2) 0.0397(11) Uani 1 1 d . . . H19A H 0.3261 -0.138 0.478 0.048 Uiso 1 1 calc R . . H19B H 0.2936 -0.2121 0.4539 0.048 Uiso 1 1 calc R . . C20 C 0.3365(2) -0.2194(3) 0.5455(3) 0.0545(14) Uani 1 1 d . . . H20A H 0.3829 -0.2349 0.5304 0.082 Uiso 1 1 calc R . . H20B H 0.3089 -0.2612 0.5585 0.082 Uiso 1 1 calc R . . H20C H 0.3423 -0.1872 0.5819 0.082 Uiso 1 1 calc R . . C21 C 0.2039(2) -0.4291(2) 0.5648(2) 0.0382(11) Uani 1 1 d . . . C22 C 0.1340(2) -0.4214(3) 0.5894(2) 0.0413(12) Uani 1 1 d . . . C23 C 0.1102(3) -0.4654(3) 0.6390(2) 0.0579(14) Uani 1 1 d . . . H23 H 0.0642 -0.4596 0.6558 0.07 Uiso 1 1 calc R . . C24 C 0.1554(4) -0.5184(3) 0.6635(3) 0.0711(18) Uani 1 1 d . . . H24 H 0.1394 -0.549 0.6966 0.085 Uiso 1 1 calc R . . C25 C 0.2221(4) -0.5261(3) 0.6399(3) 0.0637(16) Uani 1 1 d . . . H25 H 0.2518 -0.5622 0.6571 0.076 Uiso 1 1 calc R . . C26 C 0.2478(3) -0.4822(3) 0.5912(2) 0.0518(13) Uani 1 1 d . . . H26 H 0.2945 -0.4881 0.5759 0.062 Uiso 1 1 calc R . . C27 C 0.2851(2) -0.3880(2) 0.4797(3) 0.0472(13) Uani 1 1 d . . . H27A H 0.325 -0.3897 0.5101 0.057 Uiso 1 1 calc R . . H27B H 0.2914 -0.3451 0.4527 0.057 Uiso 1 1 calc R . . C28 C 0.2880(3) -0.4540(3) 0.4375(3) 0.0525(14) Uani 1 1 d . . . H28A H 0.3329 -0.455 0.4145 0.079 Uiso 1 1 calc R . . H28B H 0.2491 -0.4526 0.4068 0.079 Uiso 1 1 calc R . . H28C H 0.2838 -0.4969 0.464 0.079 Uiso 1 1 calc R . . C29 C 0.0289(2) -0.3417(3) 0.5838(3) 0.0511(13) Uani 1 1 d . . . H29A H -0.0005 -0.3839 0.594 0.061 Uiso 1 1 calc R . . H29B H 0.0042 -0.3141 0.5502 0.061 Uiso 1 1 calc R . . C30 C 0.0351(3) -0.2956(3) 0.6430(3) 0.0696(17) Uani 1 1 d . . . H30A H -0.012 -0.2811 0.6571 0.104 Uiso 1 1 calc R . . H30B H 0.063 -0.253 0.6332 0.104 Uiso 1 1 calc R . . H30C H 0.0582 -0.3228 0.677 0.104 Uiso 1 1 calc R . . C31 C 0.1235(2) -0.4342(2) 0.3019(2) 0.0362(11) Uani 1 1 d . . . C32 C 0.0529(2) -0.4409(2) 0.3241(2) 0.0405(12) Uani 1 1 d . . . C33 C 0.0096(3) -0.4957(3) 0.3012(3) 0.0542(14) Uani 1 1 d . . . H33 H -0.038 -0.4993 0.3148 0.065 Uiso 1 1 calc R . . C34 C 0.0378(4) -0.5455(3) 0.2577(3) 0.0690(18) Uani 1 1 d . . . H34 H 0.0093 -0.5837 0.2427 0.083 Uiso 1 1 calc R . . C35 C 0.1062(4) -0.5395(3) 0.2366(3) 0.0685(18) Uani 1 1 d . . . H35 H 0.1242 -0.5733 0.207 0.082 Uiso 1 1 calc R . . C36 C 0.1495(3) -0.4842(3) 0.2585(2) 0.0521(14) Uani 1 1 d . . . H36 H 0.1967 -0.4807 0.2439 0.063 Uiso 1 1 calc R . . C37 C 0.2280(2) -0.3540(3) 0.3037(2) 0.0432(12) Uani 1 1 d . . . H37A H 0.2587 -0.3966 0.3004 0.052 Uiso 1 1 calc R . . H37B H 0.2501 -0.3206 0.3344 0.052 Uiso 1 1 calc R . . C38 C 0.2241(3) -0.3179(3) 0.2386(2) 0.0593(15) Uani 1 1 d . . . H38A H 0.2716 -0.3044 0.2248 0.089 Uiso 1 1 calc R . . H38B H 0.1947 -0.275 0.2415 0.089 Uiso 1 1 calc R . . H38C H 0.2036 -0.3511 0.2075 0.089 Uiso 1 1 calc R . . C39 C -0.0299(2) -0.3945(3) 0.4072(3) 0.0518(14) Uani 1 1 d . . . H39A H -0.0701 -0.4009 0.3777 0.062 Uiso 1 1 calc R . . H39B H -0.0376 -0.3494 0.4309 0.062 Uiso 1 1 calc R . . C40 C -0.0292(3) -0.4567(3) 0.4547(3) 0.0582(14) Uani 1 1 d . . . H40A H -0.0741 -0.458 0.4778 0.087 Uiso 1 1 calc R . . H40B H 0.0095 -0.4501 0.485 0.087 Uiso 1 1 calc R . . H40C H -0.0227 -0.5017 0.4316 0.087 Uiso 1 1 calc R . . C41 C 0.1747(6) 0.3021(5) 0.5532(4) 0.127(3) Uani 1 1 d . . . H41A H 0.2151 0.3311 0.5681 0.152 Uiso 1 1 calc R . . H41B H 0.1473 0.2871 0.5911 0.152 Uiso 1 1 calc R . . C42 C 0.1285(4) 0.3471(4) 0.5100(3) 0.099(2) Uani 1 1 d . . . H42A H 0.0856 0.3199 0.4986 0.118 Uiso 1 1 calc R . . H42B H 0.1139 0.391 0.5328 0.118 Uiso 1 1 calc R . . C43 C 0.2426(6) 0.1993(5) 0.5652(4) 0.154(4) Uani 1 1 d . . . H43A H 0.2603 0.157 0.5428 0.232 Uiso 1 1 calc R . . H43B H 0.214 0.1844 0.6017 0.232 Uiso 1 1 calc R . . H43C H 0.2825 0.2281 0.5802 0.232 Uiso 1 1 calc R . . C44 C 0.1313(3) 0.4202(4) 0.4198(4) 0.095(2) Uani 1 1 d . . . H44A H 0.1591 0.4331 0.3821 0.142 Uiso 1 1 calc R . . H44B H 0.1261 0.4622 0.4474 0.142 Uiso 1 1 calc R . . H44C H 0.0847 0.4035 0.4065 0.142 Uiso 1 1 calc R . . C45 C 0.3026(5) 0.3201(5) 0.2409(4) 0.118(3) Uani 1 1 d . . . H45A H 0.3528 0.307 0.246 0.142 Uiso 1 1 calc R . . H45B H 0.3005 0.3611 0.2111 0.142 Uiso 1 1 calc R . . C46 C 0.2662(5) 0.2601(5) 0.2115(4) 0.115(3) Uani 1 1 d . . . H46A H 0.2228 0.2779 0.1908 0.138 Uiso 1 1 calc R . . H46B H 0.2967 0.2398 0.1777 0.138 Uiso 1 1 calc R . . C47 C 0.3130(4) 0.4022(4) 0.3227(4) 0.109(3) Uani 1 1 d . . . H47A H 0.293 0.4135 0.3646 0.164 Uiso 1 1 calc R . . H47B H 0.3066 0.443 0.294 0.164 Uiso 1 1 calc R . . H47C H 0.3634 0.3919 0.3272 0.164 Uiso 1 1 calc R . . C48 C 0.2251(5) 0.1408(5) 0.2234(5) 0.157(4) Uani 1 1 d . . . H48A H 0.2134 0.1049 0.2557 0.236 Uiso 1 1 calc R . . H48B H 0.2629 0.1226 0.196 0.236 Uiso 1 1 calc R . . H48C H 0.1833 0.1509 0.1974 0.236 Uiso 1 1 calc R . . C49 C 0.4088(5) 0.1873(5) 0.4053(9) 0.182(6) Uani 1 1 d . . . H49A H 0.4178 0.2099 0.3634 0.218 Uiso 1 1 calc R . . H49B H 0.4452 0.1502 0.4121 0.218 Uiso 1 1 calc R . . C50 C 0.4153(4) 0.2428(6) 0.4565(7) 0.150(5) Uani 1 1 d . . . H50A H 0.412 0.2197 0.4988 0.18 Uiso 1 1 calc R . . H50B H 0.4619 0.2663 0.4533 0.18 Uiso 1 1 calc R . . C51 C 0.3444(6) 0.1019(6) 0.3578(6) 0.181(5) Uani 1 1 d . . . H51A H 0.298 0.079 0.3587 0.272 Uiso 1 1 calc R . . H51B H 0.3808 0.0663 0.3671 0.272 Uiso 1 1 calc R . . H51C H 0.3527 0.1223 0.3154 0.272 Uiso 1 1 calc R . . C52 C 0.3637(6) 0.3514(5) 0.4950(6) 0.187(5) Uani 1 1 d . . . H52A H 0.3258 0.3854 0.4858 0.28 Uiso 1 1 calc R . . H52B H 0.4092 0.3757 0.492 0.28 Uiso 1 1 calc R . . H52C H 0.3576 0.3321 0.5381 0.28 Uiso 1 1 calc R . . C53 C 0.0817(3) 0.1075(4) 0.3977(4) 0.097(2) Uani 1 1 d . . . H53A H 0.0605 0.1278 0.4369 0.116 Uiso 1 1 calc R . . H53B H 0.062 0.0591 0.3913 0.116 Uiso 1 1 calc R . . C54 C 0.0635(4) 0.1535(4) 0.3421(4) 0.090(2) Uani 1 1 d . . . H54A H 0.0862 0.1345 0.3031 0.107 Uiso 1 1 calc R . . H54B H 0.0119 0.1533 0.3354 0.107 Uiso 1 1 calc R . . C55 C 0.1751(4) 0.0539(4) 0.4550(4) 0.114(3) Uani 1 1 d . . . H55A H 0.2265 0.0512 0.4584 0.17 Uiso 1 1 calc R . . H55B H 0.1563 0.0064 0.4449 0.17 Uiso 1 1 calc R . . H55C H 0.1553 0.0704 0.4956 0.17 Uiso 1 1 calc R . . C56 C 0.0710(4) 0.2683(4) 0.2997(4) 0.111(3) Uani 1 1 d . . . H56A H 0.0863 0.3173 0.3086 0.166 Uiso 1 1 calc R . . H56B H 0.0201 0.2678 0.2919 0.166 Uiso 1 1 calc R . . H56C H 0.0957 0.2503 0.2619 0.166 Uiso 1 1 calc R . . C57 C 0.0306(5) -0.2462(6) 0.1678(4) 0.125(3) Uani 1 1 d . . . H57A H 0.0115 -0.2322 0.21 0.15 Uiso 1 1 calc R . . H57B H 0.0794 -0.2279 0.1646 0.15 Uiso 1 1 calc R . . C58 C 0.0308(5) -0.3250(6) 0.1621(4) 0.125(3) Uani 1 1 d . . . H58A H 0.0522 -0.3461 0.2008 0.15 Uiso 1 1 calc R . . H58B H -0.0183 -0.3425 0.1589 0.15 Uiso 1 1 calc R . . C59 C -0.0195(6) -0.1432(5) 0.1256(5) 0.159(4) Uani 1 1 d . . . H59A H -0.05 -0.1262 0.0911 0.238 Uiso 1 1 calc R . . H59B H 0.0263 -0.1193 0.1228 0.238 Uiso 1 1 calc R . . H59C H -0.0413 -0.1324 0.1668 0.238 Uiso 1 1 calc R . . C60 C 0.0580(4) -0.4192(4) 0.0927(5) 0.134(4) Uani 1 1 d . . . H60A H 0.0866 -0.4308 0.0553 0.201 Uiso 1 1 calc R . . H60B H 0.0081 -0.4274 0.0829 0.201 Uiso 1 1 calc R . . H60C H 0.0721 -0.4496 0.1285 0.201 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 0.0543(6) 0.0475(6) 0.0472(6) 0.0026(6) 0.0009(6) 0.0083(5) Si1 0.0261(5) 0.0334(6) 0.0303(6) 0.0024(6) 0.0002(6) 0.0015(5) Si2 0.0243(6) 0.0324(6) 0.0303(6) -0.0002(6) 0.0009(5) 0.0005(5) Si3 0.0287(6) 0.0326(6) 0.0298(7) 0.0014(6) 0.0020(6) 0.0017(5) Si4 0.0254(6) 0.0327(6) 0.0324(6) -0.0011(6) 0.0009(6) -0.0017(5) O1 0.159(5) 0.072(3) 0.047(2) 0.006(2) -0.011(3) 0.015(3) O2 0.093(3) 0.069(3) 0.070(3) 0.017(2) 0.020(2) 0.035(2) O3 0.150(4) 0.075(3) 0.077(3) 0.003(3) 0.028(3) -0.039(3) O4 0.156(5) 0.085(3) 0.074(3) -0.032(3) 0.014(3) -0.028(3) O5 0.080(3) 0.108(4) 0.180(6) -0.004(4) 0.005(4) 0.036(3) O6 0.139(5) 0.082(3) 0.204(7) 0.014(4) -0.089(5) 0.002(4) O7 0.090(3) 0.060(2) 0.062(3) 0.019(2) 0.004(2) 0.011(2) O8 0.093(3) 0.060(3) 0.071(3) 0.007(2) -0.022(2) 0.003(2) O9 0.155(5) 0.123(5) 0.097(4) -0.020(4) -0.033(4) 0.062(4) O10 0.127(4) 0.085(4) 0.096(4) 0.016(3) 0.012(3) -0.003(3) N1 0.0237(18) 0.046(2) 0.036(2) 0.0062(18) 0.0010(17) 0.0011(17) N2 0.0238(18) 0.037(2) 0.043(2) 0.0086(19) 0.0047(17) 0.0014(16) N3 0.030(2) 0.035(2) 0.040(2) -0.0076(18) 0.0030(18) -0.0014(17) N4 0.0289(18) 0.038(2) 0.032(2) -0.0079(17) 0.0023(16) 0.0041(16) N5 0.033(2) 0.042(2) 0.041(2) 0.003(2) 0.0053(18) 0.0060(17) N6 0.036(2) 0.050(2) 0.032(2) 0.0083(19) 0.0074(18) -0.0008(19) N7 0.0298(19) 0.042(2) 0.035(2) -0.0039(19) -0.0011(17) -0.0045(17) N8 0.0283(19) 0.039(2) 0.055(3) -0.002(2) 0.0023(18) -0.0064(16) C1 0.037(3) 0.039(3) 0.028(2) -0.006(2) -0.002(2) 0.003(2) C2 0.042(3) 0.033(3) 0.029(2) 0.004(2) -0.003(2) 0.002(2) C3 0.057(3) 0.042(3) 0.041(3) 0.006(3) 0.001(3) -0.005(3) C4 0.071(4) 0.050(3) 0.044(3) 0.019(3) -0.006(3) 0.003(3) C5 0.070(4) 0.050(3) 0.046(3) 0.008(3) -0.014(3) 0.020(3) C6 0.043(3) 0.050(3) 0.039(3) 0.001(3) -0.006(2) 0.010(2) C7 0.030(2) 0.056(3) 0.053(3) 0.011(3) 0.005(3) 0.007(2) C8 0.036(3) 0.079(4) 0.072(4) 0.008(3) -0.010(3) -0.006(3) C9 0.039(3) 0.043(3) 0.050(3) 0.012(2) 0.004(2) 0.000(2) C10 0.046(3) 0.059(4) 0.078(4) 0.018(3) -0.008(3) -0.014(3) C11 0.037(2) 0.034(3) 0.029(2) 0.003(2) 0.002(2) 0.005(2) C12 0.035(2) 0.037(3) 0.025(2) 0.002(2) 0.001(2) 0.000(2) C13 0.036(2) 0.044(3) 0.046(3) -0.004(2) -0.006(2) -0.007(2) C14 0.062(3) 0.041(3) 0.044(3) -0.006(2) -0.016(3) -0.005(3) C15 0.069(4) 0.049(3) 0.033(3) -0.012(2) -0.007(3) 0.009(3) C16 0.044(3) 0.041(3) 0.030(2) -0.009(2) 0.003(2) 0.005(2) C17 0.031(2) 0.045(3) 0.059(3) -0.009(2) 0.021(2) 0.002(2) C18 0.034(3) 0.062(4) 0.079(4) -0.017(3) -0.001(3) 0.011(2) C19 0.025(2) 0.048(3) 0.047(3) -0.004(3) 0.005(2) 0.0025(19) C20 0.038(3) 0.067(4) 0.059(3) -0.014(3) -0.005(3) 0.012(3) C21 0.041(3) 0.039(3) 0.035(3) 0.000(2) -0.010(2) -0.003(2) C22 0.052(3) 0.040(3) 0.031(3) 0.008(2) -0.006(2) -0.004(2) C23 0.084(4) 0.052(3) 0.038(3) 0.014(3) 0.001(3) -0.002(3) C24 0.121(6) 0.053(4) 0.040(3) 0.014(3) -0.001(4) -0.011(4) C25 0.104(5) 0.040(3) 0.047(3) 0.013(3) -0.031(4) 0.012(3) C26 0.066(3) 0.042(3) 0.047(3) 0.000(3) -0.021(3) 0.014(3) C27 0.033(2) 0.044(3) 0.065(3) 0.000(3) -0.005(3) 0.007(2) C28 0.045(3) 0.051(3) 0.061(3) -0.002(3) 0.007(2) 0.005(3) C29 0.037(3) 0.060(3) 0.056(3) 0.004(3) 0.018(3) 0.003(2) C30 0.086(4) 0.076(4) 0.047(3) -0.004(3) 0.026(3) 0.012(3) C31 0.045(3) 0.040(3) 0.024(2) 0.001(2) -0.001(2) 0.002(2) C32 0.050(3) 0.034(3) 0.038(3) 0.004(2) -0.016(2) -0.002(2) C33 0.062(3) 0.047(3) 0.053(3) 0.005(3) -0.024(3) -0.013(3) C34 0.119(6) 0.042(3) 0.046(3) 0.000(3) -0.034(4) -0.028(4) C35 0.130(6) 0.038(3) 0.037(3) -0.005(3) -0.002(4) -0.010(4) C36 0.077(4) 0.041(3) 0.039(3) 0.002(3) -0.003(3) -0.001(3) C37 0.043(3) 0.052(3) 0.034(3) -0.002(2) 0.009(2) -0.003(2) C38 0.065(3) 0.070(4) 0.043(3) -0.003(3) 0.009(3) -0.012(3) C39 0.023(2) 0.049(3) 0.082(4) 0.001(3) 0.005(3) -0.004(2) C40 0.043(3) 0.054(3) 0.077(4) 0.009(3) 0.022(3) -0.002(3) C41 0.194(10) 0.120(7) 0.068(5) -0.003(5) 0.038(6) 0.014(7) C42 0.107(5) 0.111(6) 0.078(5) -0.004(4) 0.018(5) 0.038(5) C43 0.250(12) 0.123(7) 0.090(6) 0.046(6) -0.053(7) 0.017(8) C44 0.081(4) 0.077(5) 0.126(7) 0.011(4) -0.020(4) 0.019(4) C45 0.155(8) 0.123(7) 0.077(6) 0.016(5) 0.018(6) -0.033(6) C46 0.138(7) 0.156(8) 0.052(4) -0.006(5) 0.012(5) -0.023(6) C47 0.129(6) 0.067(5) 0.133(7) 0.000(5) 0.008(5) -0.024(5) C48 0.163(8) 0.149(9) 0.158(9) -0.095(8) 0.020(7) -0.018(7) C49 0.074(6) 0.104(7) 0.37(2) 0.019(11) 0.039(10) 0.007(5) C50 0.076(6) 0.124(8) 0.251(14) 0.077(9) -0.053(7) -0.010(6) C51 0.168(9) 0.145(9) 0.232(13) -0.051(10) 0.011(8) 0.091(8) C52 0.243(13) 0.100(7) 0.217(12) -0.013(9) -0.115(11) -0.028(8) C53 0.083(5) 0.079(5) 0.129(7) 0.030(5) 0.008(5) -0.016(4) C54 0.088(5) 0.075(5) 0.106(5) 0.015(4) -0.034(4) -0.010(4) C55 0.149(7) 0.104(6) 0.087(5) 0.041(5) 0.012(5) 0.032(5) C56 0.122(6) 0.106(6) 0.105(6) 0.037(5) -0.037(5) 0.021(5) C57 0.128(7) 0.190(10) 0.057(5) -0.024(6) -0.012(5) 0.060(7) C58 0.098(6) 0.185(10) 0.092(6) 0.063(7) 0.028(5) 0.032(7) C59 0.213(11) 0.119(8) 0.145(8) -0.050(7) -0.010(8) 0.064(7) C60 0.134(7) 0.065(5) 0.203(11) 0.020(6) -0.066(7) 0.000(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K O1 2.748(4) . ? K O5 2.760(5) . ? K O8 2.810(4) . ? K O3 2.827(4) . ? K O2 2.851(4) . ? K O6 2.928(6) . ? K O7 2.967(4) . ? K O4 2.969(5) . ? Si1 N1 1.766(3) . ? Si1 N2 1.768(4) . ? Si1 Si4 2.3455(15) . ? Si1 Si2 2.3549(16) . ? Si2 N4 1.766(3) . ? Si2 N3 1.770(4) . ? Si2 Si3 2.3467(16) . ? Si3 N5 1.769(4) . ? Si3 N6 1.769(4) . ? Si3 Si4 2.3526(16) . ? Si4 N8 1.765(3) . ? Si4 N7 1.765(4) . ? O1 C41 1.373(9) . ? O1 C43 1.453(9) . ? O2 C44 1.376(7) . ? O2 C42 1.413(8) . ? O3 C45 1.314(9) . ? O3 C47 1.399(8) . ? O4 C46 1.392(9) . ? O4 C48 1.419(9) . ? O5 C49 1.291(10) . ? O5 C51 1.407(11) . ? O6 C52 1.396(11) . ? O6 C50 1.407(9) . ? O7 C55 1.411(7) . ? O7 C53 1.417(7) . ? O8 C54 1.389(7) . ? O8 C56 1.422(7) . ? O9 C59 1.370(9) . ? O9 C57 1.370(9) . ? O10 C58 1.361(9) . ? O10 C60 1.406(8) . ? N1 C1 1.380(5) . ? N1 C7 1.461(5) . ? N2 C2 1.395(5) . ? N2 C9 1.472(5) . ? N3 C11 1.393(5) . ? N3 C17 1.453(5) . ? N4 C12 1.392(5) . ? N4 C19 1.457(5) . ? N5 C21 1.381(6) . ? N5 C27 1.461(5) . ? N6 C22 1.392(6) . ? N6 C29 1.456(6) . ? N7 C31 1.378(6) . ? N7 C37 1.464(5) . ? N8 C32 1.393(6) . ? N8 C39 1.470(6) . ? C1 C6 1.391(6) . ? C1 C2 1.422(6) . ? C2 C3 1.368(6) . ? C3 C4 1.388(7) . ? C4 C5 1.376(7) . ? C5 C6 1.391(7) . ? C7 C8 1.503(7) . ? C9 C10 1.509(7) . ? C11 C16 1.380(6) . ? C11 C12 1.414(6) . ? C12 C13 1.382(6) . ? C13 C14 1.396(7) . ? C14 C15 1.366(7) . ? C15 C16 1.392(7) . ? C17 C18 1.515(7) . ? C19 C20 1.530(7) . ? C21 C26 1.395(6) . ? C21 C22 1.416(6) . ? C22 C23 1.387(7) . ? C23 C24 1.394(8) . ? C24 C25 1.354(8) . ? C25 C26 1.385(7) . ? C27 C28 1.505(6) . ? C29 C30 1.501(7) . ? C31 C36 1.381(7) . ? C31 C32 1.410(6) . ? C32 C33 1.386(6) . ? C33 C34 1.396(8) . ? C34 C35 1.363(8) . ? C35 C36 1.385(8) . ? C37 C38 1.510(7) . ? C39 C40 1.515(7) . ? C41 C42 1.502(10) . ? C45 C46 1.440(11) . ? C49 C50 1.482(16) . ? C53 C54 1.476(9) . ? C57 C58 1.464(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K O5 93.46(18) . . ? O1 K O8 94.86(14) . . ? O5 K O8 135.28(17) . . ? O1 K O3 139.20(15) . . ? O5 K O3 99.96(18) . . ? O8 K O3 101.82(14) . . ? O1 K O2 59.38(13) . . ? O5 K O2 139.18(19) . . ? O8 K O2 80.79(13) . . ? O3 K O2 86.74(13) . . ? O1 K O6 76.6(2) . . ? O5 K O6 57.52(19) . . ? O8 K O6 165.86(17) . . ? O3 K O6 78.62(17) . . ? O2 K O6 85.13(17) . . ? O1 K O7 78.47(13) . . ? O5 K O7 80.91(16) . . ? O8 K O7 58.09(11) . . ? O3 K O7 141.50(13) . . ? O2 K O7 117.77(12) . . ? O6 K O7 129.26(14) . . ? O1 K O4 164.39(15) . . ? O5 K O4 81.37(19) . . ? O8 K O4 79.01(14) . . ? O3 K O4 56.41(14) . . ? O2 K O4 132.36(14) . . ? O6 K O4 112.0(2) . . ? O7 K O4 86.14(13) . . ? N1 Si1 N2 88.53(16) . . ? N1 Si1 Si4 117.75(13) . . ? N2 Si1 Si4 126.52(13) . . ? N1 Si1 Si2 120.27(13) . . ? N2 Si1 Si2 117.53(13) . . ? Si4 Si1 Si2 89.65(6) . . ? N4 Si2 N3 88.78(16) . . ? N4 Si2 Si3 116.50(12) . . ? N3 Si2 Si3 126.34(13) . . ? N4 Si2 Si1 122.69(13) . . ? N3 Si2 Si1 115.93(13) . . ? Si3 Si2 Si1 90.20(6) . . ? N5 Si3 N6 88.62(17) . . ? N5 Si3 Si2 126.07(13) . . ? N6 Si3 Si2 117.86(14) . . ? N5 Si3 Si4 116.16(14) . . ? N6 Si3 Si4 122.03(14) . . ? Si2 Si3 Si4 89.68(6) . . ? N8 Si4 N7 88.61(17) . . ? N8 Si4 Si1 123.88(13) . . ? N7 Si4 Si1 119.08(13) . . ? N8 Si4 Si3 117.46(14) . . ? N7 Si4 Si3 120.88(13) . . ? Si1 Si4 Si3 90.29(6) . . ? C41 O1 C43 109.3(6) . . ? C41 O1 K 121.7(4) . . ? C43 O1 K 120.5(5) . . ? C44 O2 C42 111.8(5) . . ? C44 O2 K 123.1(4) . . ? C42 O2 K 112.3(4) . . ? C45 O3 C47 114.9(6) . . ? C45 O3 K 122.5(5) . . ? C47 O3 K 113.6(4) . . ? C46 O4 C48 113.7(7) . . ? C46 O4 K 117.6(4) . . ? C48 O4 K 127.0(5) . . ? C49 O5 C51 110.9(9) . . ? C49 O5 K 118.2(5) . . ? C51 O5 K 109.5(5) . . ? C52 O6 C50 115.6(8) . . ? C52 O6 K 122.8(6) . . ? C50 O6 K 115.5(5) . . ? C55 O7 C53 111.7(5) . . ? C55 O7 K 121.5(4) . . ? C53 O7 K 112.8(3) . . ? C54 O8 C56 110.2(5) . . ? C54 O8 K 118.4(4) . . ? C56 O8 K 109.9(4) . . ? C59 O9 C57 114.1(8) . . ? C58 O10 C60 114.0(8) . . ? C1 N1 C7 120.1(3) . . ? C1 N1 Si1 113.3(3) . . ? C7 N1 Si1 126.2(3) . . ? C2 N2 C9 119.6(4) . . ? C2 N2 Si1 113.6(3) . . ? C9 N2 Si1 126.4(3) . . ? C11 N3 C17 119.3(4) . . ? C11 N3 Si2 112.8(3) . . ? C17 N3 Si2 126.7(3) . . ? C12 N4 C19 120.3(3) . . ? C12 N4 Si2 113.6(3) . . ? C19 N4 Si2 125.7(3) . . ? C21 N5 C27 119.5(4) . . ? C21 N5 Si3 113.2(3) . . ? C27 N5 Si3 126.3(3) . . ? C22 N6 C29 120.3(4) . . ? C22 N6 Si3 113.3(3) . . ? C29 N6 Si3 126.0(3) . . ? C31 N7 C37 120.0(4) . . ? C31 N7 Si4 113.3(3) . . ? C37 N7 Si4 126.3(3) . . ? C32 N8 C39 119.8(4) . . ? C32 N8 Si4 113.1(3) . . ? C39 N8 Si4 125.4(3) . . ? N1 C1 C6 128.1(4) . . ? N1 C1 C2 113.0(4) . . ? C6 C1 C2 118.9(4) . . ? C3 C2 N2 128.7(4) . . ? C3 C2 C1 120.0(4) . . ? N2 C2 C1 111.3(4) . . ? C2 C3 C4 120.5(5) . . ? C5 C4 C3 120.1(5) . . ? C4 C5 C6 120.5(5) . . ? C5 C6 C1 119.9(5) . . ? N1 C7 C8 113.3(4) . . ? N2 C9 C10 113.5(4) . . ? C16 C11 N3 127.5(4) . . ? C16 C11 C12 119.6(4) . . ? N3 C11 C12 112.9(4) . . ? C13 C12 N4 128.4(4) . . ? C13 C12 C11 119.7(4) . . ? N4 C12 C11 111.8(4) . . ? C12 C13 C14 119.8(4) . . ? C15 C14 C13 120.3(4) . . ? C14 C15 C16 120.6(4) . . ? C11 C16 C15 119.9(4) . . ? N3 C17 C18 113.8(4) . . ? N4 C19 C20 113.0(4) . . ? N5 C21 C26 128.6(4) . . ? N5 C21 C22 112.9(4) . . ? C26 C21 C22 118.5(4) . . ? C23 C22 N6 127.6(5) . . ? C23 C22 C21 120.5(5) . . ? N6 C22 C21 111.9(4) . . ? C22 C23 C24 119.2(6) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 121.6(5) . . ? C25 C26 C21 119.7(5) . . ? N5 C27 C28 113.9(4) . . ? N6 C29 C30 113.9(4) . . ? N7 C31 C36 128.1(4) . . ? N7 C31 C32 112.7(4) . . ? C36 C31 C32 119.2(4) . . ? C33 C32 N8 127.6(5) . . ? C33 C32 C31 120.3(5) . . ? N8 C32 C31 112.1(4) . . ? C32 C33 C34 118.9(5) . . ? C35 C34 C33 120.8(5) . . ? C34 C35 C36 120.6(5) . . ? C35 C36 C31 120.1(5) . . ? N7 C37 C38 113.6(4) . . ? N8 C39 C40 113.9(4) . . ? O1 C41 C42 110.9(7) . . ? O2 C42 C41 110.7(6) . . ? O3 C45 C46 116.6(7) . . ? O4 C46 C45 114.3(6) . . ? O5 C49 C50 112.8(10) . . ? O6 C50 C49 110.7(9) . . ? O7 C53 C54 110.9(5) . . ? O8 C54 C53 109.4(6) . . ? O9 C57 C58 110.2(8) . . ? O10 C58 C57 110.9(7) . . ? #===END data_(9)-jun1003 _database_code_depnum_ccdc_archive 'CCDC 286728' _audit_creation_date 2003-06-19T14:10:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C80 H120 K2 N8 O6 Si4) 4(C4 H8 O1)' _chemical_formula_sum 'C96 H152 K2 N8 O10 Si4' _chemical_formula_weight 1768.82 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 _symmetry_space_group_name_Hall 'P 4nw 2abw' _symmetry_Int_Tables_number 96 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' '-y, -x, -z+1/2' _cell_length_a 22.8047(8) _cell_length_b 22.8049(8) _cell_length_c 40.8980(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 21269.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 257582 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7664 _exptl_special_details ; The crystals diffracted poorly; giving rather diffuse spots which did not extend to high angle and were poorly resolved in some frames. Three different crystals were used to try to get better data. Smaller crystals gave too weak diffraction and for the best data set an uncut block ca. 0.4x0.4x0.4 was used. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.6458E-2 _diffrn_orient_matrix_ub_12 0.388849E-1 _diffrn_orient_matrix_ub_13 -0.107127E-1 _diffrn_orient_matrix_ub_21 -0.360446E-1 _diffrn_orient_matrix_ub_22 0.59919E-2 _diffrn_orient_matrix_ub_23 0.135183E-1 _diffrn_orient_matrix_ub_31 0.241238E-1 _diffrn_orient_matrix_ub_32 0.193624E-1 _diffrn_orient_matrix_ub_33 0.173306E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1142 _diffrn_reflns_av_unetI/netI 0.1115 _diffrn_reflns_number 23757 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 0.915 _diffrn_measured_fraction_theta_max 0.915 _reflns_number_total 12397 _reflns_number_gt 8651 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The structure is disordered; with alternative lower occupancy(29%) K sites in the two obvious sites associated with the C1-C6 and C30-C35 rings. Also there four very diffuse regions of electron density which are probably thf solvate molecules. These were included as regular pentagons with all atoms as carbon with occupancy 1.067 and hydrogens omitted. 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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 12397 _refine_ls_number_parameters 969 _refine_ls_number_restraints 378 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.1224 _refine_ls_wR_factor_ref 0.3508 _refine_ls_wR_factor_gt 0.3237 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.34(14) _refine_diff_density_max 0.502 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.11268(13) 0.62665(13) 0.87971(6) 0.0576(9) Uani 0.712(4) 1 d PU A 1 K2 K -0.10961(17) 0.13289(16) 0.86501(8) 0.0854(11) Uani 0.712(4) 1 d PU A 1 Si1 Si 0.07020(11) 0.39501(12) 0.87410(5) 0.0510(7) Uani 1 1 d U A 1 Si2 Si -0.01581(11) 0.44739(11) 0.87485(5) 0.0487(6) Uani 1 1 d U A 1 Si3 Si -0.06870(10) 0.36123(11) 0.87254(5) 0.0479(6) Uani 1 1 d U A 1 Si4 Si 0.01831(11) 0.30899(11) 0.87024(5) 0.0479(6) Uani 1 1 d U A 1 O1 O 0.1385(4) 0.6992(4) 0.92915(19) 0.101(2) Uani 1 1 d U A 1 O2 O 0.1303(4) 0.7108(4) 0.8323(2) 0.110(3) Uani 1 1 d U A 1 O3 O 0.2312(4) 0.6020(4) 0.8806(2) 0.106(2) Uani 1 1 d U A 1 O4 O -0.1417(5) 0.0578(5) 0.8194(2) 0.128(3) Uani 1 1 d U A 1 O5 O -0.1273(6) 0.0487(5) 0.9116(3) 0.141(3) Uani 1 1 d U A 1 O6 O -0.2281(4) 0.1596(5) 0.8687(3) 0.137(3) Uani 1 1 d U A 1 N1 N 0.1296(3) 0.4080(3) 0.84521(16) 0.0576(19) Uani 1 1 d U A 1 N2 N 0.1254(3) 0.4028(4) 0.90525(16) 0.0569(18) Uani 1 1 d U A 1 N3 N -0.0266(3) 0.5011(3) 0.90644(14) 0.0526(18) Uani 1 1 d U A 1 N4 N -0.0263(3) 0.5080(3) 0.84665(14) 0.0467(17) Uani 1 1 d U A 1 N5 N -0.1265(3) 0.3522(3) 0.84216(14) 0.0470(17) Uani 1 1 d U A 1 N6 N -0.1244(3) 0.3472(3) 0.90214(14) 0.0490(17) Uani 1 1 d U A 1 N7 N 0.0285(3) 0.2546(3) 0.83814(14) 0.0526(18) Uani 1 1 d U A 1 N8 N 0.0298(3) 0.2482(3) 0.89757(15) 0.0504(17) Uani 1 1 d U A 1 C1 C 0.1854(4) 0.4012(4) 0.8586(2) 0.055(2) Uani 1 1 d U A 1 C2 C 0.1841(4) 0.3980(5) 0.8937(2) 0.059(2) Uani 1 1 d U A 1 C3 C 0.2344(5) 0.3930(5) 0.9109(3) 0.072(3) Uani 1 1 d U A 1 H3 H 0.2335 0.3931 0.9341 0.087 Uiso 1 1 calc R A 1 C4 C 0.2879(5) 0.3875(6) 0.8942(3) 0.088(4) Uani 1 1 d U A 1 H4 H 0.3227 0.3823 0.9067 0.105 Uiso 1 1 calc R A 1 C5 C 0.2923(5) 0.3895(5) 0.8618(3) 0.078(3) Uani 1 1 d U A 1 H5 H 0.3293 0.3857 0.8513 0.093 Uiso 1 1 calc R A 1 C6 C 0.2398(5) 0.3975(5) 0.8432(3) 0.072(3) Uani 1 1 d U A 1 H6 H 0.2421 0.4002 0.8201 0.087 Uiso 1 1 calc R A 1 C7 C 0.1227(4) 0.4241(4) 0.81024(19) 0.054(2) Uani 1 1 d U A 1 H7A H 0.0804 0.4241 0.8048 0.065 Uiso 1 1 calc R A 1 H7B H 0.1419 0.3937 0.7966 0.065 Uiso 1 1 calc R A 1 C8 C 0.1480(5) 0.4829(4) 0.8015(2) 0.058(2) Uani 1 1 d U A 1 H8 H 0.1917 0.4801 0.8029 0.07 Uiso 1 1 calc R A 1 C9 C 0.1279(5) 0.5335(5) 0.8237(3) 0.079(3) Uani 1 1 d U A 1 H9A H 0.1459 0.5702 0.8163 0.119 Uiso 1 1 calc R A 1 H9B H 0.1398 0.5255 0.8463 0.119 Uiso 1 1 calc R A 1 H9C H 0.0851 0.537 0.8227 0.119 Uiso 1 1 calc R A 1 C10 C 0.1311(6) 0.4956(5) 0.7647(2) 0.089(4) Uani 1 1 d U A 1 H10A H 0.1469 0.5337 0.7581 0.134 Uiso 1 1 calc R A 1 H10B H 0.0883 0.496 0.7624 0.134 Uiso 1 1 calc R A 1 H10C H 0.1475 0.4648 0.7506 0.134 Uiso 1 1 calc R A 1 C11 C 0.1152(4) 0.4120(5) 0.94031(19) 0.064(2) Uani 1 1 d U A 1 H11A H 0.1319 0.3781 0.9522 0.076 Uiso 1 1 calc R A 1 H11B H 0.0724 0.4118 0.9441 0.076 Uiso 1 1 calc R A 1 C12 C 0.1399(5) 0.4670(5) 0.9551(2) 0.063(2) Uani 1 1 d U A 1 H12 H 0.1835 0.4624 0.9554 0.076 Uiso 1 1 calc R A 1 C13 C 0.1261(5) 0.5208(5) 0.9328(2) 0.074(3) Uani 1 1 d U A 1 H13A H 0.1397 0.5128 0.9105 0.11 Uiso 1 1 calc R A 1 H13B H 0.1461 0.5556 0.9413 0.11 Uiso 1 1 calc R A 1 H13C H 0.0837 0.5277 0.9325 0.11 Uiso 1 1 calc R A 1 C14 C 0.1213(5) 0.4763(6) 0.9887(2) 0.081(3) Uani 1 1 d U A 1 H14A H 0.1386 0.5127 0.997 0.121 Uiso 1 1 calc R A 1 H14B H 0.1343 0.4433 1.0023 0.121 Uiso 1 1 calc R A 1 H14C H 0.0785 0.4791 0.9896 0.121 Uiso 1 1 calc R A 1 C15 C -0.0199(4) 0.5585(4) 0.8963(2) 0.058(2) Uani 1 1 d U A 1 C16 C -0.0222(4) 0.5626(4) 0.86053(18) 0.0469(19) Uani 1 1 d U A 1 C17 C -0.0166(5) 0.6168(4) 0.8461(2) 0.058(2) Uani 1 1 d U A 1 H17 H -0.0159 0.6186 0.8229 0.07 Uiso 1 1 calc R A 1 C18 C -0.0117(5) 0.6697(5) 0.8635(2) 0.069(2) Uani 1 1 d U A 1 H18 H -0.0088 0.7065 0.8527 0.083 Uiso 1 1 calc R A 1 C19 C -0.0114(5) 0.6650(5) 0.8979(2) 0.067(2) Uani 1 1 d U A 1 H19 H -0.0086 0.6997 0.9106 0.081 Uiso 1 1 calc R A 1 C20 C -0.0152(5) 0.6097(5) 0.9140(2) 0.061(2) Uani 1 1 d U A 1 H20 H -0.0145 0.6081 0.9372 0.073 Uiso 1 1 calc R A 1 C21 C -0.0399(4) 0.4890(5) 0.94117(18) 0.060(2) Uani 1 1 d U A 1 H21A H -0.0079 0.5055 0.9547 0.072 Uiso 1 1 calc R A 1 H21B H -0.04 0.446 0.9445 0.072 Uiso 1 1 calc R A 1 C22 C -0.0975(5) 0.5134(4) 0.95333(19) 0.058(2) Uani 1 1 d U A 1 H22 H -0.0944 0.5571 0.9534 0.069 Uiso 1 1 calc R A 1 C23 C -0.1470(5) 0.4966(5) 0.9309(2) 0.069(3) Uani 1 1 d U A 1 H23A H -0.1392 0.5119 0.9089 0.103 Uiso 1 1 calc R A 1 H23B H -0.1837 0.5132 0.9391 0.103 Uiso 1 1 calc R A 1 H23C H -0.1502 0.4538 0.9299 0.103 Uiso 1 1 calc R A 1 C24 C -0.1081(5) 0.4931(5) 0.9886(2) 0.076(3) Uani 1 1 d U A 1 H24A H -0.0753 0.5056 1.0024 0.115 Uiso 1 1 calc R A 1 H24B H -0.1112 0.4502 0.9892 0.115 Uiso 1 1 calc R A 1 H24C H -0.1446 0.5104 0.9968 0.115 Uiso 1 1 calc R A 1 C25 C -0.0394(4) 0.5011(4) 0.81175(18) 0.047(2) Uani 1 1 d U A 1 H25A H -0.0381 0.4589 0.8061 0.057 Uiso 1 1 calc R A 1 H25B H -0.0087 0.5213 0.7988 0.057 Uiso 1 1 calc R A 1 C26 C -0.1005(5) 0.5263(5) 0.80225(19) 0.066(3) Uani 1 1 d U A 1 H26 H -0.0973 0.57 0.8028 0.079 Uiso 1 1 calc R A 1 C27 C -0.1143(6) 0.5080(6) 0.7652(2) 0.089(4) Uani 1 1 d U A 1 H27A H -0.1523 0.5242 0.7587 0.133 Uiso 1 1 calc R A 1 H27B H -0.1154 0.4651 0.7635 0.133 Uiso 1 1 calc R A 1 H27C H -0.0836 0.5234 0.7509 0.133 Uiso 1 1 calc R A 1 C28 C -0.1482(5) 0.5094(6) 0.8252(3) 0.092(4) Uani 1 1 d U A 1 H28A H -0.1852 0.5271 0.818 0.138 Uiso 1 1 calc R A 1 H28B H -0.1387 0.5234 0.8472 0.138 Uiso 1 1 calc R A 1 H28C H -0.1522 0.4666 0.8255 0.138 Uiso 1 1 calc R A 1 C29 C -0.1822(4) 0.3578(4) 0.8553(2) 0.055(2) Uani 1 1 d U A 1 C30 C -0.1813(4) 0.3528(5) 0.8906(2) 0.059(2) Uani 1 1 d U A 1 C31 C -0.2348(5) 0.3581(5) 0.9080(2) 0.070(3) Uani 1 1 d U A 1 H31 H -0.2346 0.358 0.9313 0.084 Uiso 1 1 calc R A 1 C32 C -0.2883(5) 0.3636(5) 0.8908(3) 0.071(3) Uani 1 1 d U A 1 H32 H -0.3244 0.3644 0.9023 0.085 Uiso 1 1 calc R A 1 C33 C -0.2874(5) 0.3675(5) 0.8576(3) 0.076(3) Uani 1 1 d U A 1 H33 H -0.3235 0.3729 0.8464 0.092 Uiso 1 1 calc R A 1 C34 C -0.2357(5) 0.3640(5) 0.8391(2) 0.062(2) Uani 1 1 d U A 1 H34 H -0.237 0.3658 0.8159 0.075 Uiso 1 1 calc R A 1 C35 C -0.1187(4) 0.3451(4) 0.80709(18) 0.057(2) Uani 1 1 d U A 1 H35A H -0.0762 0.3461 0.802 0.068 Uiso 1 1 calc R A 1 H35B H -0.1374 0.3786 0.7957 0.068 Uiso 1 1 calc R A 1 C36 C -0.1457(6) 0.2855(5) 0.7932(2) 0.079(3) Uani 1 1 d U A 1 H36 H -0.1894 0.2883 0.7942 0.095 Uiso 1 1 calc R A 1 C37 C -0.1270(6) 0.2341(5) 0.8122(3) 0.092(3) Uani 1 1 d U A 1 H37A H -0.1461 0.1989 0.8035 0.138 Uiso 1 1 calc R A 1 H37B H -0.1381 0.2393 0.8352 0.138 Uiso 1 1 calc R A 1 H37C H -0.0843 0.2298 0.8106 0.138 Uiso 1 1 calc R A 1 C38 C -0.1266(6) 0.2823(6) 0.7568(2) 0.104(5) Uani 1 1 d U A 1 H38A H -0.1396 0.3178 0.7453 0.156 Uiso 1 1 calc R A 1 H38B H -0.1444 0.2478 0.7465 0.156 Uiso 1 1 calc R A 1 H38C H -0.0838 0.2793 0.7555 0.156 Uiso 1 1 calc R A 1 C39 C -0.1147(4) 0.3304(4) 0.93591(18) 0.057(2) Uani 1 1 d U A 1 H39A H -0.1328 0.3603 0.9502 0.069 Uiso 1 1 calc R A 1 H39B H -0.0719 0.3306 0.9402 0.069 Uiso 1 1 calc R A 1 C40 C -0.1400(5) 0.2676(5) 0.9458(2) 0.072(3) Uani 1 1 d U A 1 H40 H -0.1838 0.2706 0.9457 0.086 Uiso 1 1 calc R A 1 C41 C -0.1214(5) 0.2544(5) 0.9810(2) 0.079(3) Uani 1 1 d U A 1 H41A H -0.1364 0.285 0.9956 0.118 Uiso 1 1 calc R A 1 H41B H -0.0785 0.2533 0.9823 0.118 Uiso 1 1 calc R A 1 H41C H -0.1373 0.2163 0.9877 0.118 Uiso 1 1 calc R A 1 C42 C -0.1238(5) 0.2238(5) 0.9218(2) 0.077(3) Uani 1 1 d U A 1 H42A H -0.1397 0.2349 0.9004 0.116 Uiso 1 1 calc R A 1 H42B H -0.1398 0.1857 0.9283 0.116 Uiso 1 1 calc R A 1 H42C H -0.081 0.2213 0.9205 0.116 Uiso 1 1 calc R A 1 C43 C 0.0234(4) 0.1987(5) 0.8484(2) 0.057(2) Uani 1 1 d U A 1 C44 C 0.0221(4) 0.1933(4) 0.8821(2) 0.060(2) Uani 1 1 d U A 1 C45 C 0.0180(5) 0.1379(5) 0.8976(2) 0.072(2) Uani 1 1 d U A 1 H45 H 0.0175 0.1346 0.9207 0.086 Uiso 1 1 calc R A 1 C46 C 0.0147(5) 0.0865(5) 0.8770(3) 0.080(2) Uani 1 1 d U A 1 H46 H 0.0129 0.0485 0.8864 0.096 Uiso 1 1 calc R A 1 C47 C 0.0140(5) 0.0928(5) 0.8445(3) 0.081(2) Uani 1 1 d U A 1 H47 H 0.0112 0.0588 0.8312 0.098 Uiso 1 1 calc R A 1 C48 C 0.0173(5) 0.1474(5) 0.8295(2) 0.074(2) Uani 1 1 d U A 1 H48 H 0.0155 0.1501 0.8064 0.089 Uiso 1 1 calc R A 1 C49 C 0.0407(4) 0.2695(5) 0.80387(19) 0.062(2) Uani 1 1 d U A 1 H49A H 0.0406 0.3127 0.8013 0.074 Uiso 1 1 calc R A 1 H49B H 0.0093 0.2533 0.7898 0.074 Uiso 1 1 calc R A 1 C50 C 0.1042(5) 0.2436(5) 0.7918(2) 0.067(3) Uani 1 1 d U A 1 H50 H 0.1011 0.1999 0.7903 0.08 Uiso 1 1 calc R A 1 C51 C 0.1546(5) 0.2589(5) 0.8157(3) 0.072(3) Uani 1 1 d U A 1 H51A H 0.1465 0.2415 0.8371 0.107 Uiso 1 1 calc R A 1 H51B H 0.1575 0.3016 0.8179 0.107 Uiso 1 1 calc R A 1 H51C H 0.1916 0.2433 0.8072 0.107 Uiso 1 1 calc R A 1 C52 C 0.1133(5) 0.2679(6) 0.7574(2) 0.089(4) Uani 1 1 d U A 1 H52A H 0.0813 0.2548 0.7432 0.134 Uiso 1 1 calc R A 1 H52B H 0.1508 0.2538 0.7487 0.134 Uiso 1 1 calc R A 1 H52C H 0.1137 0.3109 0.7583 0.134 Uiso 1 1 calc R A 1 C53 C 0.0406(4) 0.2526(5) 0.93260(19) 0.063(3) Uani 1 1 d U A 1 H53A H 0.0096 0.231 0.9445 0.076 Uiso 1 1 calc R A 1 H53B H 0.0386 0.2942 0.9393 0.076 Uiso 1 1 calc R A 1 C54 C 0.1019(6) 0.2271(7) 0.9422(2) 0.105(4) Uani 1 1 d U A 1 H54 H 0.0985 0.1835 0.9404 0.126 Uiso 1 1 calc R A 1 C55 C 0.1494(5) 0.2443(6) 0.9208(3) 0.094(4) Uani 1 1 d U A 1 H55A H 0.1856 0.2247 0.9278 0.141 Uiso 1 1 calc R A 1 H55B H 0.1548 0.2869 0.922 0.141 Uiso 1 1 calc R A 1 H55C H 0.1401 0.2331 0.8983 0.141 Uiso 1 1 calc R A 1 C56 C 0.1098(7) 0.2413(6) 0.9789(3) 0.110(5) Uani 1 1 d U A 1 H56A H 0.0751 0.2284 0.9911 0.164 Uiso 1 1 calc R A 1 H56B H 0.1149 0.2837 0.9817 0.164 Uiso 1 1 calc R A 1 H56C H 0.1445 0.2208 0.9873 0.164 Uiso 1 1 calc R A 1 C57 C 0.1232(9) 0.6935(8) 0.9597(3) 0.157(8) Uani 1 1 d U A 1 H57A H 0.1464 0.6617 0.9699 0.188 Uiso 1 1 calc R A 1 H57B H 0.0813 0.6827 0.9609 0.188 Uiso 1 1 calc R A 1 C58 C 0.1334(11) 0.7506(8) 0.9783(4) 0.169(8) Uani 1 1 d U A 1 H58A H 0.096 0.7668 0.9867 0.203 Uiso 1 1 calc R A 1 H58B H 0.1605 0.7445 0.9969 0.203 Uiso 1 1 calc R A 1 C59 C 0.1593(12) 0.7895(9) 0.9537(4) 0.197(11) Uani 1 1 d U A 1 H59A H 0.135 0.8249 0.9504 0.236 Uiso 1 1 calc R A 1 H59B H 0.1994 0.8016 0.9601 0.236 Uiso 1 1 calc R A 1 C60 C 0.1603(8) 0.7529(7) 0.9243(3) 0.129(6) Uani 1 1 d U A 1 H60A H 0.1374 0.7725 0.9069 0.155 Uiso 1 1 calc R A 1 H60B H 0.2013 0.7493 0.9166 0.155 Uiso 1 1 calc R A 1 C61 C 0.1883(7) 0.7305(8) 0.8273(3) 0.127(6) Uani 1 1 d U A 1 H61A H 0.2165 0.6987 0.8323 0.152 Uiso 1 1 calc R A 1 H61B H 0.1969 0.7642 0.8418 0.152 Uiso 1 1 calc R A 1 C62 C 0.1933(7) 0.7484(11) 0.7921(3) 0.164(8) Uani 1 1 d U A 1 H62A H 0.2259 0.7273 0.7813 0.197 Uiso 1 1 calc R A 1 H62B H 0.2006 0.7911 0.7903 0.197 Uiso 1 1 calc R A 1 C63 C 0.1345(7) 0.7323(9) 0.7763(3) 0.139(6) Uani 1 1 d U A 1 H63A H 0.1192 0.7652 0.763 0.167 Uiso 1 1 calc R A 1 H63B H 0.1386 0.6972 0.7622 0.167 Uiso 1 1 calc R A 1 C64 C 0.0960(7) 0.7203(8) 0.8039(3) 0.128(5) Uani 1 1 d U A 1 H64A H 0.0692 0.7539 0.8074 0.153 Uiso 1 1 calc R A 1 H64B H 0.0719 0.6851 0.7992 0.153 Uiso 1 1 calc R A 1 C65 C 0.2638(7) 0.5477(9) 0.8737(7) 0.200(11) Uani 1 1 d U A 1 H65A H 0.2398 0.513 0.8793 0.24 Uiso 1 1 calc R A 1 H65B H 0.2742 0.5457 0.8502 0.24 Uiso 1 1 calc R A 1 C66 C 0.3147(10) 0.5492(8) 0.8929(7) 0.227(13) Uani 1 1 d U A 1 H66A H 0.309 0.527 0.9134 0.272 Uiso 1 1 calc R A 1 H66B H 0.3484 0.5322 0.8809 0.272 Uiso 1 1 calc R A 1 C67 C 0.3238(8) 0.6076(8) 0.8992(6) 0.175(9) Uani 1 1 d U A 1 H67A H 0.3377 0.6126 0.922 0.21 Uiso 1 1 calc R A 1 H67B H 0.3542 0.6232 0.8843 0.21 Uiso 1 1 calc R A 1 C68 C 0.2726(6) 0.6376(7) 0.8949(4) 0.118(5) Uani 1 1 d U A 1 H68A H 0.2797 0.6722 0.8808 0.142 Uiso 1 1 calc R A 1 H68B H 0.258 0.6517 0.9163 0.142 Uiso 1 1 calc R A 1 C69 C -0.1657(8) 0.0020(7) 0.8248(3) 0.120(5) Uani 1 1 d U A 1 H69A H -0.1491 -0.0158 0.8449 0.144 Uiso 1 1 calc R A 1 H69B H -0.2088 0.0044 0.8272 0.144 Uiso 1 1 calc R A 1 C70 C -0.1508(12) -0.0314(9) 0.7972(4) 0.183(10) Uani 1 1 d U A 1 H70A H -0.1195 -0.0596 0.8031 0.22 Uiso 1 1 calc R A 1 H70B H -0.1854 -0.054 0.7899 0.22 Uiso 1 1 calc R A 1 C71 C -0.1314(9) 0.0041(8) 0.7719(4) 0.144(6) Uani 1 1 d U A 1 H71A H -0.1612 0.0065 0.7543 0.172 Uiso 1 1 calc R A 1 H71B H -0.0944 -0.011 0.7625 0.172 Uiso 1 1 calc R A 1 C72 C -0.1221(8) 0.0632(8) 0.7875(3) 0.135(6) Uani 1 1 d U A 1 H72A H -0.08 0.074 0.7871 0.162 Uiso 1 1 calc R A 1 H72B H -0.1447 0.0938 0.7758 0.162 Uiso 1 1 calc R A 1 C73 C -0.0926(9) 0.0305(12) 0.9403(5) 0.208(12) Uani 1 1 d U A 1 H73A H -0.0592 0.0058 0.9333 0.249 Uiso 1 1 calc R A 1 H73B H -0.0767 0.0655 0.9516 0.249 Uiso 1 1 calc R A 1 C74 C -0.1241(13) 0.003(2) 0.9588(8) 0.42(3) Uani 1 1 d U A 1 H74A H -0.1154 0.0145 0.9816 0.501 Uiso 1 1 calc R A 1 H74B H -0.116 -0.0393 0.9565 0.501 Uiso 1 1 calc R A 1 C75 C -0.1877(11) 0.0147(15) 0.9516(4) 0.246(15) Uani 1 1 d U A 1 H75A H -0.2124 -0.0206 0.9547 0.295 Uiso 1 1 calc R A 1 H75B H -0.2036 0.0477 0.9646 0.295 Uiso 1 1 calc R A 1 C76 C -0.1806(8) 0.0287(8) 0.9194(3) 0.133(6) Uani 1 1 d U A 1 H76A H -0.189 -0.0065 0.9061 0.16 Uiso 1 1 calc R A 1 H76B H -0.21 0.0589 0.9135 0.16 Uiso 1 1 calc R A 1 C77 C -0.2621(8) 0.2072(8) 0.8793(6) 0.173(9) Uani 1 1 d U A 1 H77A H -0.2473 0.2439 0.8693 0.207 Uiso 1 1 calc R A 1 H77B H -0.2593 0.211 0.9033 0.207 Uiso 1 1 calc R A 1 C78 C -0.3209(7) 0.1981(9) 0.8700(5) 0.174(9) Uani 1 1 d U A 1 H78A H -0.3356 0.233 0.8582 0.208 Uiso 1 1 calc R A 1 H78B H -0.3452 0.1926 0.8898 0.208 Uiso 1 1 calc R A 1 C79 C -0.3257(10) 0.1479(12) 0.8496(7) 0.274(18) Uani 1 1 d U A 1 H79A H -0.3623 0.1259 0.8542 0.329 Uiso 1 1 calc R A 1 H79B H -0.3251 0.159 0.8262 0.329 Uiso 1 1 calc R A 1 C80 C -0.2758(7) 0.1146(8) 0.8580(5) 0.158(8) Uani 1 1 d U A 1 H80A H -0.262 0.0915 0.839 0.19 Uiso 1 1 calc R A 1 H80B H -0.2849 0.0874 0.8762 0.19 Uiso 1 1 calc R A 1 K1A K 0.2464(5) 0.2602(6) 0.8719(2) 0.111(4) Uani 0.288(4) 1 d P A 2 K2A K -0.2440(3) 0.4880(3) 0.87759(13) 0.041(2) Uani 0.288(4) 1 d P A 2 C1A C 0.1578(9) 0.0017(12) 0.9698(6) 0.255(13) Uiso 1.07 1 d PGU B 2 C2A C 0.1202(12) 0.0403(9) 0.9492(5) 0.251(12) Uiso 1.07 1 d PGU B 2 C3A C 0.0599(10) 0.0150(11) 0.9488(5) 0.212(9) Uiso 1.07 1 d PGU B 2 C4A C 0.0602(11) -0.0392(10) 0.9691(6) 0.265(13) Uiso 1.07 1 d PGU B 2 C5A C 0.1208(13) -0.0475(10) 0.9822(5) 0.260(13) Uiso 1.07 1 d PGU B 2 C6A C -0.1143(19) -0.1938(12) 0.7598(7) 0.297(15) Uiso 1.07 1 d PGU C 2 C7A C -0.1518(12) -0.2184(17) 0.7806(9) 0.300(16) Uiso 1.07 1 d PGU C 2 C8A C -0.1251(17) -0.2640(16) 0.7944(7) 0.46(3) Uiso 1.07 1 d PGU C 2 C9A C -0.0712(15) -0.2675(13) 0.7822(8) 0.275(14) Uiso 1.07 1 d PGU C 2 C10A C -0.0645(14) -0.2241(17) 0.7608(8) 0.51(3) Uiso 1.07 1 d PGU C 2 C11A C -0.018(2) -0.0745(15) 0.8671(7) 0.40(3) Uiso 1.07 1 d PGU D 2 C12A C -0.0435(13) -0.129(2) 0.8669(6) 0.276(14) Uiso 1.07 1 d PGU D 2 C13A C 0.000(2) -0.1695(13) 0.8739(8) 0.44(3) Uiso 1.07 1 d PGU D 2 C14A C 0.0513(16) -0.140(2) 0.8784(7) 0.37(2) Uiso 1.07 1 d PGU D 2 C15A C 0.0402(19) -0.081(2) 0.8741(7) 0.323(18) Uiso 1.07 1 d PGU D 2 C16A C -0.1794(11) -0.0513(15) 1.0403(6) 0.318(17) Uiso 1.07 1 d PGU E 2 C17A C -0.1782(15) -0.1140(16) 1.0402(7) 0.40(2) Uiso 1.07 1 d PGU E 2 C18A C -0.2330(16) -0.1344(11) 1.0276(7) 0.39(2) Uiso 1.07 1 d PGU E 2 C19A C -0.2680(9) -0.0843(12) 1.0198(5) 0.219(10) Uiso 1.07 1 d PGU E 2 C20A C -0.2349(11) -0.0330(8) 1.0276(4) 0.182(7) Uiso 1.07 1 d PGU E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0629(18) 0.0579(19) 0.0519(15) -0.0029(12) 0.0022(13) -0.0079(14) K2 0.093(2) 0.080(3) 0.083(2) -0.0086(17) 0.0040(18) -0.002(2) Si1 0.0535(15) 0.0567(16) 0.0428(12) -0.0018(12) 0.0016(11) 0.0032(12) Si2 0.0545(15) 0.0550(16) 0.0365(11) -0.0002(11) 0.0017(11) 0.0031(12) Si3 0.0491(15) 0.0556(16) 0.0390(11) -0.0020(11) -0.0011(11) 0.0032(12) Si4 0.0511(15) 0.0541(16) 0.0386(11) 0.0011(11) -0.0022(11) 0.0010(12) O1 0.122(6) 0.098(5) 0.082(4) -0.014(4) -0.006(4) -0.021(5) O2 0.118(6) 0.121(6) 0.090(4) 0.024(4) -0.004(4) -0.043(5) O3 0.073(4) 0.114(6) 0.131(6) -0.015(5) 0.008(4) -0.017(4) O4 0.149(7) 0.122(6) 0.112(5) -0.030(5) 0.013(5) -0.044(6) O5 0.148(8) 0.145(7) 0.129(6) 0.042(6) 0.009(6) -0.039(6) O6 0.096(4) 0.128(8) 0.186(9) -0.026(6) -0.009(5) 0.003(5) N1 0.062(4) 0.066(5) 0.045(3) 0.003(3) 0.008(3) 0.008(4) N2 0.054(4) 0.065(5) 0.051(3) -0.006(3) -0.002(3) 0.005(4) N3 0.069(5) 0.057(4) 0.032(3) -0.006(3) -0.003(3) -0.002(4) N4 0.053(5) 0.047(4) 0.040(3) -0.003(3) -0.002(3) -0.004(3) N5 0.052(4) 0.054(5) 0.034(3) -0.002(3) -0.001(3) -0.003(4) N6 0.051(4) 0.059(5) 0.038(3) -0.003(3) -0.006(3) -0.004(4) N7 0.060(5) 0.062(4) 0.035(3) -0.006(3) 0.001(3) -0.001(4) N8 0.056(5) 0.054(4) 0.041(3) 0.004(3) -0.006(3) 0.003(4) C1 0.054(5) 0.048(6) 0.064(4) -0.008(4) -0.001(4) -0.009(5) C2 0.058(5) 0.061(6) 0.059(4) 0.002(5) 0.003(4) 0.015(5) C3 0.068(6) 0.068(7) 0.081(6) -0.016(6) -0.013(4) 0.013(6) C4 0.063(6) 0.106(10) 0.095(6) 0.023(7) -0.007(5) 0.001(7) C5 0.065(6) 0.076(8) 0.093(6) -0.011(6) 0.003(5) 0.003(6) C6 0.074(6) 0.067(7) 0.075(5) -0.021(6) 0.004(4) 0.015(6) C7 0.053(6) 0.065(5) 0.044(4) -0.001(4) 0.010(4) -0.003(5) C8 0.051(6) 0.067(6) 0.057(4) 0.006(4) 0.017(4) 0.000(5) C9 0.079(7) 0.083(6) 0.076(5) -0.011(5) 0.016(5) 0.004(6) C10 0.142(12) 0.065(8) 0.061(5) 0.021(5) 0.024(6) 0.004(7) C11 0.060(6) 0.085(6) 0.046(4) -0.009(4) -0.013(4) 0.012(5) C12 0.060(7) 0.077(6) 0.052(4) -0.004(4) -0.014(4) 0.011(6) C13 0.065(6) 0.087(6) 0.069(5) 0.006(5) -0.012(5) -0.001(5) C14 0.102(9) 0.093(9) 0.048(4) -0.010(5) -0.022(5) 0.020(7) C15 0.068(6) 0.062(5) 0.044(4) -0.004(3) 0.001(4) -0.017(5) C16 0.052(5) 0.049(4) 0.040(4) 0.000(3) 0.007(4) 0.010(4) C17 0.073(5) 0.054(5) 0.049(4) 0.006(3) 0.002(4) 0.008(4) C18 0.081(5) 0.047(5) 0.080(5) 0.006(4) 0.004(5) 0.007(5) C19 0.079(5) 0.053(5) 0.070(4) -0.012(4) -0.001(4) 0.007(5) C20 0.074(5) 0.062(5) 0.047(4) -0.009(3) 0.005(4) 0.000(5) C21 0.070(6) 0.070(7) 0.039(4) -0.011(4) 0.012(4) -0.029(5) C22 0.078(6) 0.051(6) 0.044(4) -0.002(4) 0.009(4) -0.010(5) C23 0.079(7) 0.072(7) 0.055(5) 0.004(5) 0.001(5) 0.017(6) C24 0.081(8) 0.102(9) 0.047(4) 0.001(5) 0.010(5) -0.007(7) C25 0.059(5) 0.040(5) 0.043(4) 0.005(3) 0.005(4) -0.004(4) C26 0.081(7) 0.077(7) 0.041(4) 0.003(4) -0.012(4) 0.016(6) C27 0.090(9) 0.125(11) 0.052(5) 0.005(6) -0.020(5) -0.011(8) C28 0.070(7) 0.126(11) 0.080(6) -0.002(7) 0.005(5) 0.017(7) C29 0.060(5) 0.057(6) 0.048(4) 0.000(4) -0.006(3) -0.006(5) C30 0.059(5) 0.067(7) 0.051(4) 0.010(5) 0.010(4) 0.020(5) C31 0.064(6) 0.075(7) 0.071(5) 0.002(6) 0.014(4) -0.005(6) C32 0.056(6) 0.074(8) 0.083(6) -0.006(6) 0.008(5) 0.004(6) C33 0.054(6) 0.077(8) 0.099(6) -0.006(6) -0.009(5) 0.002(6) C34 0.066(5) 0.064(7) 0.057(5) -0.002(5) -0.004(4) 0.006(6) C35 0.054(6) 0.075(6) 0.042(4) 0.002(4) -0.005(4) -0.003(5) C36 0.100(9) 0.094(7) 0.042(4) -0.026(4) -0.014(5) 0.026(6) C37 0.129(9) 0.077(6) 0.070(5) -0.019(4) -0.013(6) 0.023(6) C38 0.143(12) 0.119(11) 0.050(5) -0.022(5) -0.011(6) 0.009(9) C39 0.061(6) 0.076(6) 0.035(4) -0.006(4) 0.004(4) 0.004(5) C40 0.066(7) 0.093(7) 0.057(5) 0.020(4) 0.025(5) -0.001(6) C41 0.084(9) 0.086(8) 0.065(5) 0.012(5) 0.003(5) -0.014(7) C42 0.075(7) 0.091(6) 0.066(5) 0.009(4) 0.022(5) -0.018(5) C43 0.056(6) 0.067(5) 0.049(4) -0.005(4) 0.011(4) 0.018(5) C44 0.071(6) 0.055(4) 0.054(4) 0.004(4) 0.001(5) 0.021(5) C45 0.089(5) 0.071(5) 0.056(4) 0.004(4) 0.014(4) 0.000(5) C46 0.109(5) 0.053(5) 0.077(5) 0.005(4) -0.004(5) -0.002(5) C47 0.105(6) 0.064(5) 0.076(5) -0.008(4) 0.013(5) 0.003(5) C48 0.097(5) 0.061(5) 0.064(4) -0.007(4) 0.001(5) 0.017(5) C49 0.069(6) 0.074(7) 0.042(4) -0.003(4) 0.008(4) 0.019(5) C50 0.068(6) 0.073(7) 0.059(5) -0.006(5) 0.020(4) 0.009(6) C51 0.072(6) 0.056(7) 0.086(6) -0.002(5) 0.018(5) -0.005(6) C52 0.092(9) 0.106(10) 0.069(5) 0.002(6) 0.027(5) 0.021(7) C53 0.074(6) 0.080(7) 0.035(4) 0.013(4) 0.009(4) 0.001(5) C54 0.103(8) 0.156(13) 0.055(5) 0.011(7) -0.019(5) 0.034(8) C55 0.075(7) 0.100(10) 0.108(8) 0.029(7) -0.019(6) 0.029(7) C56 0.170(14) 0.090(9) 0.069(5) -0.013(6) -0.052(7) 0.046(9) C57 0.23(2) 0.160(13) 0.079(7) -0.021(7) 0.010(10) -0.066(14) C58 0.29(3) 0.125(13) 0.094(8) -0.023(7) 0.044(12) -0.002(14) C59 0.33(3) 0.176(15) 0.082(8) -0.048(9) 0.033(13) -0.113(18) C60 0.198(18) 0.099(10) 0.090(7) -0.022(6) -0.001(9) -0.049(10) C61 0.132(10) 0.177(15) 0.072(6) 0.007(8) 0.007(6) -0.091(11) C62 0.100(9) 0.30(3) 0.093(8) 0.069(12) 0.005(7) 0.013(12) C63 0.132(12) 0.195(17) 0.092(7) 0.034(10) 0.004(6) -0.029(12) C64 0.122(9) 0.180(16) 0.081(7) 0.018(8) 0.000(6) 0.001(11) C65 0.060(9) 0.158(15) 0.38(3) -0.100(19) -0.010(13) 0.012(8) C66 0.169(17) 0.085(9) 0.43(4) 0.048(16) -0.12(2) -0.016(10) C67 0.117(12) 0.110(11) 0.30(2) -0.018(15) -0.075(14) 0.019(10) C68 0.082(7) 0.131(10) 0.142(12) -0.026(10) -0.030(8) 0.007(7) C69 0.166(16) 0.098(9) 0.096(8) -0.004(6) 0.025(9) -0.043(9) C70 0.32(3) 0.140(11) 0.091(9) -0.025(8) 0.032(13) -0.081(17) C71 0.195(19) 0.144(13) 0.092(8) -0.008(7) 0.012(10) -0.025(13) C72 0.191(17) 0.149(11) 0.065(6) -0.008(6) 0.020(8) -0.049(12) C73 0.146(12) 0.31(3) 0.164(17) 0.113(16) -0.054(11) -0.111(18) C74 0.22(2) 0.69(7) 0.34(4) 0.39(5) -0.18(2) -0.28(3) C75 0.184(15) 0.47(5) 0.086(9) -0.027(15) 0.049(11) -0.08(2) C76 0.134(10) 0.168(15) 0.097(8) 0.034(9) -0.041(8) -0.075(11) C77 0.112(9) 0.102(11) 0.30(3) -0.042(13) -0.046(14) 0.038(9) C78 0.092(8) 0.160(15) 0.27(2) -0.108(16) 0.007(13) 0.008(9) C79 0.144(14) 0.29(3) 0.39(3) -0.23(3) -0.13(2) 0.138(17) C80 0.103(8) 0.158(13) 0.214(18) -0.104(14) -0.076(11) 0.047(8) K1A 0.088(7) 0.152(11) 0.091(6) 0.013(7) 0.001(6) 0.021(7) K2A 0.036(4) 0.050(4) 0.036(3) 0.001(3) 0.000(3) 0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.678(8) . ? K1 O2 2.755(8) . ? K1 O3 2.760(9) . ? K1 C19 3.053(11) . ? K1 C18 3.074(11) . ? K1 C9 3.143(11) . ? K1 C20 3.260(11) . ? K1 C17 3.260(11) . ? K1 C13 3.261(11) . ? K2 O4 2.637(10) . ? K2 O5 2.734(10) . ? K2 O6 2.773(11) . ? K2 C46 3.064(13) . ? K2 C47 3.080(12) . ? K2 C42 3.130(11) . ? K2 C37 3.186(12) . ? K2 C45 3.203(13) . ? K2 C48 3.255(12) . ? Si1 N2 1.800(7) . ? Si1 N1 1.822(7) . ? Si1 Si4 2.296(4) . ? Si1 Si2 2.297(4) . ? Si2 N3 1.797(7) . ? Si2 N4 1.815(7) . ? Si2 Si3 2.307(4) . ? Si3 N6 1.783(7) . ? Si3 N5 1.824(7) . ? Si3 Si4 2.316(3) . ? Si4 N8 1.800(7) . ? Si4 N7 1.820(7) . ? O1 C57 1.302(15) . ? O1 C60 1.336(15) . ? O2 C61 1.412(15) . ? O2 C64 1.420(15) . ? O3 C68 1.376(15) . ? O3 C65 1.473(19) . ? O4 C72 1.384(15) . ? O4 C69 1.403(15) . ? O5 C76 1.338(17) . ? O5 C73 1.476(19) . ? O6 C77 1.404(17) . ? O6 C80 1.557(19) . ? N1 C1 1.396(12) . ? N1 C7 1.485(10) . ? N2 C2 1.424(12) . ? N2 C11 1.467(10) . ? N3 C15 1.382(12) . ? N3 C21 1.478(10) . ? N4 C16 1.373(11) . ? N4 C25 1.467(9) . ? N5 C29 1.385(11) . ? N5 C35 1.454(10) . ? N6 C30 1.388(11) . ? N6 C39 1.451(10) . ? N7 C43 1.348(12) . ? N7 C49 1.469(10) . ? N8 C44 1.413(12) . ? N8 C53 1.457(10) . ? C1 C6 1.394(13) . ? C1 C2 1.436(12) . ? C2 C3 1.350(14) . ? C3 C4 1.404(15) . ? C4 C5 1.331(15) . ? C5 C6 1.430(14) . ? C7 C8 1.504(13) . ? C8 C9 1.538(14) . ? C8 C10 1.581(14) . ? C11 C12 1.501(14) . ? C12 C14 1.455(13) . ? C12 C13 1.561(14) . ? C15 C20 1.380(13) . ? C15 C16 1.466(11) . ? C16 C17 1.376(12) . ? C17 C18 1.406(13) . ? C18 C19 1.411(13) . ? C19 C20 1.427(14) . ? C21 C22 1.510(14) . ? C22 C23 1.505(14) . ? C22 C24 1.535(12) . ? C25 C26 1.558(13) . ? C26 C28 1.489(15) . ? C26 C27 1.601(13) . ? C29 C34 1.395(13) . ? C29 C30 1.448(12) . ? C30 C31 1.417(13) . ? C31 C32 1.415(14) . ? C32 C33 1.362(14) . ? C33 C34 1.404(14) . ? C35 C36 1.596(15) . ? C36 C37 1.470(14) . ? C36 C38 1.556(14) . ? C39 C40 1.597(14) . ? C40 C42 1.449(14) . ? C40 C41 1.532(14) . ? C43 C44 1.386(12) . ? C43 C48 1.407(14) . ? C44 C45 1.415(14) . ? C45 C46 1.446(14) . ? C46 C47 1.335(14) . ? C47 C48 1.389(15) . ? C49 C50 1.640(13) . ? C50 C52 1.526(13) . ? C50 C51 1.547(14) . ? C53 C54 1.562(16) . ? C54 C55 1.446(17) . ? C54 C56 1.549(14) . ? C57 C58 1.53(2) . ? C58 C59 1.47(2) . ? C59 C60 1.465(18) . ? C61 C62 1.502(17) . ? C62 C63 1.53(2) . ? C63 C64 1.454(19) . ? C65 C66 1.40(2) . ? C66 C67 1.37(2) . ? C67 C68 1.364(19) . ? C69 C70 1.40(2) . ? C70 C71 1.39(2) . ? C71 C72 1.51(2) . ? C73 C74 1.22(2) . ? C74 C75 1.50(3) . ? C75 C76 1.36(2) . ? C77 C78 1.41(2) . ? C78 C79 1.42(2) . ? C79 C80 1.41(2) . ? C1A C5A 1.492(13) . ? C1A C2A 1.492(13) . ? C2A C3A 1.492(13) . ? C3A C4A 1.492(13) . ? C4A C5A 1.492(13) . ? C6A C7A 1.331(16) . ? C6A C10A 1.331(16) . ? C7A C8A 1.331(16) . ? C8A C9A 1.331(16) . ? C9A C10A 1.331(16) . ? C11A C12A 1.374(18) . ? C11A C15A 1.374(18) . ? C12A C13A 1.374(18) . ? C13A C14A 1.374(18) . ? C14A C15A 1.374(18) . ? C16A C20A 1.429(14) . ? C16A C17A 1.429(14) . ? C17A C18A 1.429(14) . ? C18A C19A 1.429(14) . ? C19A C20A 1.429(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O2 93.9(3) . . ? O1 K1 O3 84.3(3) . . ? O2 K1 O3 90.5(3) . . ? O1 K1 C19 81.0(3) . . ? O2 K1 C19 96.1(3) . . ? O3 K1 C19 164.2(3) . . ? O1 K1 C18 99.7(3) . . ? O2 K1 C18 76.1(3) . . ? O3 K1 C18 166.2(3) . . ? C19 K1 C18 26.6(3) . . ? O1 K1 C9 160.6(3) . . ? O2 K1 C9 86.7(3) . . ? O3 K1 C9 76.4(3) . . ? C19 K1 C9 118.2(3) . . ? C18 K1 C9 99.2(3) . . ? O1 K1 C20 86.8(3) . . ? O2 K1 C20 121.0(3) . . ? O3 K1 C20 147.8(3) . . ? C19 K1 C20 25.9(3) . . ? C18 K1 C20 46.0(3) . . ? C9 K1 C20 109.4(3) . . ? O1 K1 C17 124.1(3) . . ? O2 K1 C17 83.3(3) . . ? O3 K1 C17 151.2(3) . . ? C19 K1 C17 44.3(3) . . ? C18 K1 C17 25.4(2) . . ? C9 K1 C17 75.3(3) . . ? C20 K1 C17 50.6(2) . . ? O1 K1 C13 86.2(3) . . ? O2 K1 C13 165.9(3) . . ? O3 K1 C13 75.4(3) . . ? C19 K1 C13 97.9(3) . . ? C18 K1 C13 117.8(3) . . ? C9 K1 C13 88.5(3) . . ? C20 K1 C13 73.1(3) . . ? C17 K1 C13 108.3(3) . . ? O4 K2 O5 89.8(4) . . ? O4 K2 O6 84.9(4) . . ? O5 K2 O6 88.5(4) . . ? O4 K2 C46 98.3(3) . . ? O5 K2 C46 77.5(4) . . ? O6 K2 C46 165.5(4) . . ? O4 K2 C47 82.4(3) . . ? O5 K2 C47 96.7(4) . . ? O6 K2 C47 166.3(3) . . ? C46 K2 C47 25.1(3) . . ? O4 K2 C42 157.9(4) . . ? O5 K2 C42 86.2(3) . . ? O6 K2 C42 73.4(3) . . ? C46 K2 C42 101.9(3) . . ? C47 K2 C42 119.6(3) . . ? O4 K2 C37 87.5(3) . . ? O5 K2 C37 164.3(4) . . ? O6 K2 C37 75.9(4) . . ? C46 K2 C37 118.2(3) . . ? C47 K2 C37 98.3(3) . . ? C42 K2 C37 90.6(3) . . ? O4 K2 C45 124.7(3) . . ? O5 K2 C45 82.5(3) . . ? O6 K2 C45 148.8(3) . . ? C46 K2 C45 26.6(3) . . ? C47 K2 C45 44.9(3) . . ? C42 K2 C45 76.2(3) . . ? C37 K2 C45 111.6(3) . . ? O4 K2 C48 89.8(3) . . ? O5 K2 C48 120.9(4) . . ? O6 K2 C48 150.2(3) . . ? C46 K2 C48 44.2(3) . . ? C47 K2 C48 25.1(3) . . ? C42 K2 C48 110.8(3) . . ? C37 K2 C48 74.6(3) . . ? C45 K2 C48 51.2(3) . . ? N2 Si1 N1 85.6(3) . . ? N2 Si1 Si4 119.6(3) . . ? N1 Si1 Si4 118.5(3) . . ? N2 Si1 Si2 122.4(3) . . ? N1 Si1 Si2 124.0(3) . . ? Si4 Si1 Si2 90.29(13) . . ? N3 Si2 N4 85.4(3) . . ? N3 Si2 Si1 118.7(3) . . ? N4 Si2 Si1 120.0(3) . . ? N3 Si2 Si3 122.6(3) . . ? N4 Si2 Si3 123.6(2) . . ? Si1 Si2 Si3 90.17(13) . . ? N6 Si3 N5 85.8(3) . . ? N6 Si3 Si2 119.8(3) . . ? N5 Si3 Si2 120.1(3) . . ? N6 Si3 Si4 123.1(3) . . ? N5 Si3 Si4 122.3(2) . . ? Si2 Si3 Si4 89.54(13) . . ? N8 Si4 N7 84.5(3) . . ? N8 Si4 Si1 122.7(3) . . ? N7 Si4 Si1 124.4(3) . . ? N8 Si4 Si3 119.7(3) . . ? N7 Si4 Si3 119.3(3) . . ? Si1 Si4 Si3 89.96(13) . . ? C57 O1 C60 109.4(11) . . ? C57 O1 K1 127.1(9) . . ? C60 O1 K1 122.4(7) . . ? C61 O2 C64 110.4(10) . . ? C61 O2 K1 117.4(8) . . ? C64 O2 K1 127.1(9) . . ? C68 O3 C65 103.3(11) . . ? C68 O3 K1 123.9(8) . . ? C65 O3 K1 131.6(8) . . ? C72 O4 C69 110.9(11) . . ? C72 O4 K2 121.3(9) . . ? C69 O4 K2 125.8(8) . . ? C76 O5 C73 101.6(12) . . ? C76 O5 K2 122.7(10) . . ? C73 O5 K2 132.2(10) . . ? C77 O6 C80 102.1(11) . . ? C77 O6 K2 136.5(10) . . ? C80 O6 K2 121.4(8) . . ? C1 N1 C7 120.2(7) . . ? C1 N1 Si1 113.9(6) . . ? C7 N1 Si1 125.9(6) . . ? C2 N2 C11 118.9(7) . . ? C2 N2 Si1 114.5(5) . . ? C11 N2 Si1 126.5(6) . . ? C15 N3 C21 119.2(7) . . ? C15 N3 Si2 114.5(5) . . ? C21 N3 Si2 126.3(6) . . ? C16 N4 C25 120.9(7) . . ? C16 N4 Si2 114.8(5) . . ? C25 N4 Si2 124.3(5) . . ? C29 N5 C35 120.4(7) . . ? C29 N5 Si3 112.8(5) . . ? C35 N5 Si3 126.5(6) . . ? C30 N6 C39 119.4(7) . . ? C30 N6 Si3 114.8(5) . . ? C39 N6 Si3 125.8(6) . . ? C43 N7 C49 122.1(7) . . ? C43 N7 Si4 114.2(5) . . ? C49 N7 Si4 123.7(6) . . ? C44 N8 C53 121.4(7) . . ? C44 N8 Si4 112.7(5) . . ? C53 N8 Si4 125.6(6) . . ? C6 C1 N1 129.9(8) . . ? C6 C1 C2 117.8(9) . . ? N1 C1 C2 112.3(8) . . ? C3 C2 N2 129.2(9) . . ? C3 C2 C1 120.5(10) . . ? N2 C2 C1 110.3(8) . . ? C2 C3 C4 119.5(10) . . ? C5 C4 C3 123.2(11) . . ? C4 C5 C6 118.1(11) . . ? C1 C6 C5 120.8(10) . . ? N1 C7 C8 114.2(7) . . ? C7 C8 C9 114.4(8) . . ? C7 C8 C10 107.2(8) . . ? C9 C8 C10 110.7(8) . . ? C8 C9 K1 165.9(8) . . ? N2 C11 C12 117.0(8) . . ? C14 C12 C11 113.2(9) . . ? C14 C12 C13 112.3(9) . . ? C11 C12 C13 110.2(7) . . ? C12 C13 K1 171.8(7) . . ? C20 C15 N3 130.7(8) . . ? C20 C15 C16 118.3(9) . . ? N3 C15 C16 110.9(8) . . ? N4 C16 C17 130.1(7) . . ? N4 C16 C15 110.9(8) . . ? C17 C16 C15 118.9(8) . . ? C16 C17 C18 124.1(8) . . ? C16 C17 K1 88.0(6) . . ? C18 C17 K1 69.9(6) . . ? C17 C18 C19 116.1(9) . . ? C17 C18 K1 84.7(6) . . ? C19 C18 K1 75.9(7) . . ? C18 C19 C20 122.0(9) . . ? C18 C19 K1 77.5(7) . . ? C20 C19 K1 85.2(6) . . ? C15 C20 C19 120.6(8) . . ? C15 C20 K1 86.7(6) . . ? C19 C20 K1 68.9(6) . . ? N3 C21 C22 115.3(8) . . ? C23 C22 C21 111.0(7) . . ? C23 C22 C24 112.3(8) . . ? C21 C22 C24 109.6(9) . . ? N4 C25 C26 112.6(7) . . ? C28 C26 C25 113.6(8) . . ? C28 C26 C27 112.7(10) . . ? C25 C26 C27 108.4(8) . . ? N5 C29 C34 128.7(8) . . ? N5 C29 C30 111.5(8) . . ? C34 C29 C30 119.6(9) . . ? N6 C30 C31 129.9(8) . . ? N6 C30 C29 111.0(8) . . ? C31 C30 C29 118.9(9) . . ? C32 C31 C30 119.9(9) . . ? C33 C32 C31 119.4(10) . . ? C32 C33 C34 123.1(11) . . ? C29 C34 C33 118.9(9) . . ? N5 C35 C36 113.4(8) . . ? C37 C36 C38 112.7(9) . . ? C37 C36 C35 112.4(8) . . ? C38 C36 C35 105.8(10) . . ? C36 C37 K2 166.5(8) . . ? N6 C39 C40 115.1(7) . . ? C42 C40 C41 115.5(10) . . ? C42 C40 C39 110.7(7) . . ? C41 C40 C39 108.3(9) . . ? C40 C42 K2 170.5(8) . . ? N7 C43 C44 113.2(8) . . ? N7 C43 C48 128.8(8) . . ? C44 C43 C48 118.0(9) . . ? C43 C44 N8 111.4(8) . . ? C43 C44 C45 121.6(9) . . ? N8 C44 C45 126.8(8) . . ? C44 C45 C46 117.9(8) . . ? C44 C45 K2 84.7(7) . . ? C46 C45 K2 71.4(6) . . ? C47 C46 C45 119.5(10) . . ? C47 C46 K2 78.1(7) . . ? C45 C46 K2 82.1(7) . . ? C46 C47 C48 122.3(10) . . ? C46 C47 K2 76.8(7) . . ? C48 C47 K2 84.5(7) . . ? C47 C48 C43 120.6(9) . . ? C47 C48 K2 70.4(7) . . ? C43 C48 K2 85.9(6) . . ? N7 C49 C50 111.7(7) . . ? C52 C50 C51 113.5(9) . . ? C52 C50 C49 105.4(8) . . ? C51 C50 C49 112.6(7) . . ? N8 C53 C54 111.9(8) . . ? C55 C54 C56 116.1(12) . . ? C55 C54 C53 114.7(9) . . ? C56 C54 C53 105.7(10) . . ? O1 C57 C58 110.8(14) . . ? C59 C58 C57 103.5(12) . . ? C60 C59 C58 103.0(14) . . ? O1 C60 C59 113.3(13) . . ? O2 C61 C62 107.3(12) . . ? C61 C62 C63 105.7(13) . . ? C64 C63 C62 104.4(12) . . ? O2 C64 C63 109.4(13) . . ? C66 C65 O3 106.9(17) . . ? C67 C66 C65 104.7(17) . . ? C68 C67 C66 109.5(17) . . ? C67 C68 O3 110.3(15) . . ? C70 C69 O4 105.6(12) . . ? C71 C70 C69 111.2(16) . . ? C70 C71 C72 104.5(13) . . ? O4 C72 C71 105.9(13) . . ? C74 C73 O5 108.8(18) . . ? C73 C74 C75 111(2) . . ? C76 C75 C74 96.6(18) . . ? O5 C76 C75 114.8(15) . . ? O6 C77 C78 109.2(15) . . ? C77 C78 C79 110.6(15) . . ? C80 C79 C78 103.0(16) . . ? C79 C80 O6 106.2(17) . . ? C5A C1A C2A 108 . . ? C3A C2A C1A 108 . . ? C2A C3A C4A 108 . . ? C3A C4A C5A 108 . . ? C1A C5A C4A 108 . . ? C7A C6A C10A 108 . . ? C8A C7A C6A 108 . . ? C7A C8A C9A 108 . . ? C8A C9A C10A 108 . . ? C9A C10A C6A 108 . . ? C12A C11A C15A 108 . . ? C13A C12A C11A 108 . . ? C12A C13A C14A 108 . . ? C13A C14A C15A 108 . . ? C14A C15A C11A 108 . . ? C20A C16A C17A 108 . . ? C18A C17A C16A 108 . . ? C19A C18A C17A 108 . . ? C18A C19A C20A 108 . . ? C19A C20A C16A 108 . . ? #===END data_(11)-feb1803 _database_code_depnum_ccdc_archive 'CCDC 286729' _audit_creation_date 2003-02-17T09:05:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((K(thf)3Si(NCH2tBu)2C6H4)2) _chemical_formula_moiety 'C56 H100 K2 N4 O6 Si2' _chemical_formula_sum 'C56 H100 K2 N4 O6 Si2' _chemical_formula_weight 1059.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.0808(2) _cell_length_b 20.3241(2) _cell_length_c 20.7401(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6356.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51094 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_number 67088 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 11102 _reflns_number_gt 9491 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; One of the thf groups was clearly disordered and alternative C atom positions were refined. 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^)+(0.0683P)^2^+2.7924P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 11102 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.40(5) _refine_diff_density_max 0.389 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.49940(5) 0.64139(3) 0.63783(3) 0.04623(17) Uani 1 1 d . . . K2 K 0.50484(5) 0.36697(3) 0.38333(3) 0.04787(17) Uani 1 1 d . . . Si1 Si 0.43279(6) 0.54152(4) 0.51482(4) 0.03899(19) Uani 1 1 d . A 1 Si2 Si 0.56502(6) 0.46727(4) 0.50700(4) 0.03908(19) Uani 1 1 d . A 1 N1 N 0.41018(16) 0.55206(12) 0.42808(11) 0.0388(6) Uani 1 1 d . A 1 N2 N 0.34381(16) 0.47973(12) 0.50994(11) 0.0389(5) Uani 1 1 d . A 1 N3 N 0.65567(16) 0.52770(12) 0.51012(11) 0.0392(5) Uani 1 1 d . A 1 N4 N 0.58811(16) 0.45764(12) 0.59365(11) 0.0389(5) Uani 1 1 d . A 1 C1 C 0.3734(2) 0.49682(15) 0.40100(15) 0.0418(7) Uani 1 1 d . A 1 C2 C 0.3355(2) 0.45416(15) 0.44873(15) 0.0417(7) Uani 1 1 d . A 1 C3 C 0.2968(2) 0.39467(17) 0.42919(17) 0.0509(8) Uani 1 1 d . A 1 H3 H 0.2713 0.366 0.4602 0.061 Uiso 1 1 calc R A 1 C4 C 0.2958(2) 0.37776(19) 0.36385(18) 0.0587(9) Uani 1 1 d . A 1 H4 H 0.2704 0.3371 0.351 0.07 Uiso 1 1 calc R A 1 C5 C 0.3308(2) 0.41875(19) 0.31821(18) 0.0578(9) Uani 1 1 d . A 1 H5 H 0.3285 0.4067 0.274 0.069 Uiso 1 1 calc R A 1 C6 C 0.3698(2) 0.47840(17) 0.33629(16) 0.0490(8) Uani 1 1 d . A 1 H6 H 0.3941 0.5065 0.3043 0.059 Uiso 1 1 calc R A 1 C7 C 0.4563(2) 0.60074(16) 0.38924(15) 0.0474(8) Uani 1 1 d . A 1 H7A H 0.4779 0.5791 0.3495 0.057 Uiso 1 1 calc R A 1 H7B H 0.5089 0.6161 0.4135 0.057 Uiso 1 1 calc R A 1 C8 C 0.4002(2) 0.66160(18) 0.36976(18) 0.0566(9) Uani 1 1 d . A 1 C9 C 0.3223(3) 0.64126(19) 0.32705(19) 0.0642(10) Uani 1 1 d . A 1 H9A H 0.2844 0.6102 0.3505 0.096 Uiso 1 1 calc R A 1 H9B H 0.3448 0.6202 0.2878 0.096 Uiso 1 1 calc R A 1 H9C H 0.2877 0.6803 0.3154 0.096 Uiso 1 1 calc R A 1 C10 C 0.4603(3) 0.7082(2) 0.3333(3) 0.0950(16) Uani 1 1 d . A 1 H10A H 0.4829 0.6863 0.2946 0.143 Uiso 1 1 calc R A 1 H10B H 0.5102 0.721 0.3609 0.143 Uiso 1 1 calc R A 1 H10C H 0.4268 0.7476 0.3209 0.143 Uiso 1 1 calc R A 1 C11 C 0.3643(3) 0.6952(2) 0.4300(2) 0.0773(12) Uani 1 1 d . A 1 H11A H 0.3254 0.6647 0.4533 0.116 Uiso 1 1 calc R A 1 H11B H 0.3307 0.7344 0.4176 0.116 Uiso 1 1 calc R A 1 H11C H 0.4138 0.7079 0.458 0.116 Uiso 1 1 calc R A 1 C12 C 0.3045(2) 0.44786(15) 0.56532(14) 0.0421(7) Uani 1 1 d . A 1 H12A H 0.3448 0.4537 0.6026 0.05 Uiso 1 1 calc R A 1 H12B H 0.3006 0.4001 0.5564 0.05 Uiso 1 1 calc R A 1 C13 C 0.2114(2) 0.47274(16) 0.58474(15) 0.0462(7) Uani 1 1 d . A 1 C14 C 0.1460(2) 0.4630(2) 0.53002(17) 0.0596(9) Uani 1 1 d . A 1 H14A H 0.1424 0.4161 0.5193 0.089 Uiso 1 1 calc R A 1 H14B H 0.166 0.4877 0.4921 0.089 Uiso 1 1 calc R A 1 H14C H 0.0874 0.4789 0.5433 0.089 Uiso 1 1 calc R A 1 C15 C 0.1817(3) 0.4346(2) 0.64420(19) 0.0688(11) Uani 1 1 d . A 1 H15A H 0.2237 0.4422 0.6795 0.103 Uiso 1 1 calc R A 1 H15B H 0.1796 0.3875 0.6341 0.103 Uiso 1 1 calc R A 1 H15C H 0.1226 0.4496 0.6573 0.103 Uiso 1 1 calc R A 1 C16 C 0.2160(3) 0.54597(17) 0.60023(18) 0.0584(9) Uani 1 1 d . A 1 H16A H 0.257 0.5531 0.6362 0.088 Uiso 1 1 calc R A 1 H16B H 0.1569 0.5619 0.6122 0.088 Uiso 1 1 calc R A 1 H16C H 0.2371 0.5701 0.5623 0.088 Uiso 1 1 calc R A 1 C17 C 0.66649(19) 0.55407(15) 0.57114(14) 0.0382(7) Uani 1 1 d . A 1 C18 C 0.62850(19) 0.51258(14) 0.61983(14) 0.0385(7) Uani 1 1 d . A 1 C19 C 0.6346(2) 0.53172(16) 0.68401(14) 0.0460(7) Uani 1 1 d . A 1 H19 H 0.6104 0.5044 0.7168 0.055 Uiso 1 1 calc R A 1 C20 C 0.6762(2) 0.59102(17) 0.70075(17) 0.0529(9) Uani 1 1 d . A 1 H20 H 0.68 0.6034 0.7448 0.063 Uiso 1 1 calc R A 1 C21 C 0.7112(2) 0.63118(17) 0.65444(17) 0.0544(8) Uani 1 1 d . A 1 H21 H 0.7383 0.6716 0.6664 0.065 Uiso 1 1 calc R A 1 C22 C 0.7071(2) 0.61266(15) 0.58895(16) 0.0469(7) Uani 1 1 d . A 1 H22 H 0.7322 0.6404 0.5569 0.056 Uiso 1 1 calc R A 1 C23 C 0.6945(2) 0.55799(16) 0.45332(15) 0.0452(7) Uani 1 1 d . A 1 H23A H 0.7009 0.6058 0.4612 0.054 Uiso 1 1 calc R A 1 H23B H 0.6533 0.5523 0.4166 0.054 Uiso 1 1 calc R A 1 C24 C 0.7865(2) 0.52968(17) 0.43401(15) 0.0515(8) Uani 1 1 d . A 1 C25 C 0.8153(3) 0.5643(2) 0.37187(19) 0.0755(12) Uani 1 1 d . A 1 H25A H 0.8206 0.6116 0.3798 0.113 Uiso 1 1 calc R A 1 H25B H 0.771 0.5565 0.3382 0.113 Uiso 1 1 calc R A 1 H25C H 0.8727 0.5468 0.3579 0.113 Uiso 1 1 calc R A 1 C26 C 0.7788(3) 0.45633(18) 0.42142(19) 0.0630(9) Uani 1 1 d . A 1 H26A H 0.7595 0.434 0.4609 0.095 Uiso 1 1 calc R A 1 H26B H 0.8366 0.439 0.4081 0.095 Uiso 1 1 calc R A 1 H26C H 0.7352 0.4486 0.3872 0.095 Uiso 1 1 calc R A 1 C27 C 0.8546(2) 0.5414(2) 0.48765(19) 0.0700(11) Uani 1 1 d . A 1 H27A H 0.8603 0.5887 0.4956 0.105 Uiso 1 1 calc R A 1 H27B H 0.9122 0.5235 0.4744 0.105 Uiso 1 1 calc R A 1 H27C H 0.835 0.5193 0.5272 0.105 Uiso 1 1 calc R A 1 C28 C 0.5388(2) 0.41218(16) 0.63385(15) 0.0449(7) Uani 1 1 d . A 1 H28A H 0.4843 0.3993 0.6104 0.054 Uiso 1 1 calc R A 1 H28B H 0.5201 0.4358 0.6733 0.054 Uiso 1 1 calc R A 1 C29 C 0.5871(2) 0.34955(16) 0.65426(17) 0.0542(8) Uani 1 1 d . A 1 C30 C 0.6072(4) 0.30865(19) 0.5963(2) 0.0842(14) Uani 1 1 d . A 1 H30A H 0.5518 0.2972 0.5743 0.126 Uiso 1 1 calc R A 1 H30B H 0.6377 0.2683 0.6097 0.126 Uiso 1 1 calc R A 1 H30C H 0.6454 0.3336 0.5668 0.126 Uiso 1 1 calc R A 1 C31 C 0.5257(3) 0.3120(2) 0.7000(3) 0.0933(16) Uani 1 1 d . A 1 H31A H 0.4707 0.3007 0.6774 0.14 Uiso 1 1 calc R A 1 H31B H 0.512 0.3395 0.7374 0.14 Uiso 1 1 calc R A 1 H31C H 0.5551 0.2715 0.7143 0.14 Uiso 1 1 calc R A 1 C32 C 0.6730(3) 0.36639(19) 0.6891(2) 0.0715(12) Uani 1 1 d . A 1 H32A H 0.703 0.3257 0.702 0.107 Uiso 1 1 calc R A 1 H32B H 0.6596 0.3927 0.7275 0.107 Uiso 1 1 calc R A 1 H32C H 0.7116 0.3916 0.6602 0.107 Uiso 1 1 calc R A 1 O1 O 0.5555(3) 0.75838(13) 0.59150(16) 0.0912(10) Uani 1 1 d . A 1 C33 C 0.5908(4) 0.7596(2) 0.5280(2) 0.0919(15) Uani 1 1 d . A 1 H33A H 0.5644 0.7247 0.5008 0.11 Uiso 1 1 calc R A 1 H33B H 0.6561 0.7544 0.5284 0.11 Uiso 1 1 calc R A 1 C34 C 0.5649(5) 0.8258(3) 0.5051(3) 0.1139(19) Uani 1 1 d . A 1 H34A H 0.6028 0.8402 0.4688 0.137 Uiso 1 1 calc R A 1 H34B H 0.5021 0.8266 0.4912 0.137 Uiso 1 1 calc R A 1 C35 C 0.5786(4) 0.8676(2) 0.5622(3) 0.1049(17) Uani 1 1 d . A 1 H35A H 0.5386 0.9063 0.5616 0.126 Uiso 1 1 calc R A 1 H35B H 0.6408 0.8829 0.5651 0.126 Uiso 1 1 calc R A 1 C36 C 0.5561(5) 0.8219(3) 0.6166(3) 0.1061(17) Uani 1 1 d . A 1 H36A H 0.6009 0.8256 0.6514 0.127 Uiso 1 1 calc R A 1 H36B H 0.4972 0.833 0.6347 0.127 Uiso 1 1 calc R A 1 O2 O 0.3505(2) 0.71745(16) 0.65980(15) 0.0821(9) Uani 1 1 d . A 1 C37 C 0.3006(4) 0.7344(2) 0.6033(2) 0.0989(17) Uani 1 1 d . A 1 H37A H 0.2982 0.6967 0.5731 0.119 Uiso 1 1 calc R A 1 H37B H 0.328 0.7723 0.5809 0.119 Uiso 1 1 calc R A 1 C38 C 0.2100(5) 0.7515(4) 0.6263(3) 0.132(3) Uani 1 1 d . A 1 H38A H 0.1987 0.7991 0.6201 0.159 Uiso 1 1 calc R A 1 H38B H 0.1649 0.7266 0.6017 0.159 Uiso 1 1 calc R A 1 C39 C 0.2053(3) 0.7356(3) 0.6909(2) 0.0938(16) Uani 1 1 d . A 1 H39A H 0.1543 0.7061 0.6989 0.113 Uiso 1 1 calc R A 1 H39B H 0.1974 0.7759 0.7171 0.113 Uiso 1 1 calc R A 1 C40 C 0.2893(3) 0.7023(2) 0.70868(19) 0.0721(11) Uani 1 1 d . A 1 H40A H 0.3108 0.7183 0.7509 0.086 Uiso 1 1 calc R A 1 H40B H 0.2803 0.6541 0.7115 0.086 Uiso 1 1 calc R A 1 O3 O 0.4428(2) 0.59668(16) 0.75671(12) 0.0759(8) Uani 1 1 d . A 1 C41 C 0.3923(3) 0.5372(3) 0.7540(2) 0.0870(14) Uani 1 1 d . A 1 H41A H 0.4114 0.5099 0.717 0.104 Uiso 1 1 calc R A 1 H41B H 0.3283 0.5471 0.7492 0.104 Uiso 1 1 calc R A 1 C42 C 0.4090(4) 0.5026(4) 0.8151(4) 0.153(4) Uani 1 1 d . A 1 H42A H 0.3542 0.4813 0.831 0.184 Uiso 1 1 calc R A 1 H42B H 0.4553 0.4685 0.8095 0.184 Uiso 1 1 calc R A 1 C43 C 0.4383(5) 0.5528(4) 0.8592(3) 0.138(3) Uani 1 1 d . A 1 H43A H 0.4833 0.5351 0.8893 0.166 Uiso 1 1 calc R A 1 H43B H 0.3878 0.5701 0.8846 0.166 Uiso 1 1 calc R A 1 C44 C 0.4765(5) 0.6046(3) 0.8191(2) 0.1092(19) Uani 1 1 d . A 1 H44A H 0.4602 0.6484 0.8362 0.131 Uiso 1 1 calc R A 1 H44B H 0.542 0.601 0.8186 0.131 Uiso 1 1 calc R A 1 O4 O 0.4471(4) 0.24311(17) 0.4007(2) 0.1312(16) Uani 1 1 d . A 1 C45 C 0.4101(9) 0.2354(6) 0.4608(6) 0.114(4) Uiso 0.552(8) 1 d P A 1 H45A H 0.3452 0.2426 0.46 0.137 Uiso 0.552(8) 1 calc PR A 1 H45B H 0.4375 0.2652 0.4928 0.137 Uiso 0.552(8) 1 calc PR A 1 C46 C 0.4339(6) 0.1610(4) 0.4747(4) 0.160(3) Uiso 0.552(8) 1 d P A 1 H46A H 0.4949 0.1563 0.4917 0.192 Uiso 0.552(8) 1 calc PR A 1 H46B H 0.3915 0.1408 0.5053 0.192 Uiso 0.552(8) 1 calc PR A 1 C47 C 0.4261(7) 0.1343(5) 0.4142(4) 0.091(3) Uiso 0.552(8) 1 d P A 1 H47A H 0.3657 0.1163 0.4081 0.11 Uiso 0.552(8) 1 calc PR A 1 H47B H 0.4692 0.0979 0.4089 0.11 Uiso 0.552(8) 1 calc PR A 1 C48 C 0.4437(8) 0.1867(5) 0.3657(5) 0.091(3) Uiso 0.552(8) 1 d P A 1 H48A H 0.5007 0.1788 0.3433 0.11 Uiso 0.552(8) 1 calc PR A 1 H48B H 0.3956 0.1886 0.3333 0.11 Uiso 0.552(8) 1 calc PR A 1 O5 O 0.6559(2) 0.29341(19) 0.36777(14) 0.0903(10) Uani 1 1 d . A 1 C49 C 0.7174(3) 0.2748(2) 0.4165(2) 0.0795(12) Uani 1 1 d . A 1 H49A H 0.6995 0.2328 0.4368 0.095 Uiso 1 1 calc R A 1 H49B H 0.7213 0.3091 0.4503 0.095 Uiso 1 1 calc R A 1 C50 C 0.8032(3) 0.2675(3) 0.3827(2) 0.0949(16) Uani 1 1 d . A 1 H50A H 0.8392 0.2323 0.4027 0.114 Uiso 1 1 calc R A 1 H50B H 0.8372 0.3092 0.384 0.114 Uiso 1 1 calc R A 1 C51 C 0.7795(3) 0.2501(2) 0.3150(2) 0.0719(11) Uani 1 1 d . A 1 H51A H 0.8183 0.2733 0.2839 0.086 Uiso 1 1 calc R A 1 H51B H 0.7845 0.2021 0.3077 0.086 Uiso 1 1 calc R A 1 C52 C 0.6868(3) 0.2721(3) 0.3088(2) 0.0784(12) Uani 1 1 d . A 1 H52A H 0.6831 0.3084 0.2771 0.094 Uiso 1 1 calc R A 1 H52B H 0.6496 0.2354 0.2931 0.094 Uiso 1 1 calc R A 1 O6 O 0.5620(2) 0.41093(16) 0.26369(13) 0.0791(8) Uani 1 1 d . A 1 C53 C 0.5281(5) 0.4070(3) 0.1995(2) 0.111(2) Uani 1 1 d . A 1 H53A H 0.463 0.413 0.1989 0.134 Uiso 1 1 calc R A 1 H53B H 0.5428 0.3642 0.1795 0.134 Uiso 1 1 calc R A 1 C54 C 0.5746(5) 0.4633(4) 0.1646(3) 0.153(4) Uani 1 1 d . A 1 H54A H 0.6291 0.4477 0.1429 0.183 Uiso 1 1 calc R A 1 H54B H 0.535 0.4836 0.1321 0.183 Uiso 1 1 calc R A 1 C55 C 0.5954(5) 0.5090(5) 0.2147(4) 0.161(4) Uani 1 1 d . A 1 H55A H 0.545 0.5391 0.2226 0.193 Uiso 1 1 calc R A 1 H55B H 0.6482 0.5354 0.2032 0.193 Uiso 1 1 calc R A 1 C56 C 0.6125(3) 0.4693(3) 0.2704(3) 0.0963(16) Uani 1 1 d . A 1 H56A H 0.6764 0.4586 0.2733 0.116 Uiso 1 1 calc R A 1 H56B H 0.5949 0.493 0.3101 0.116 Uiso 1 1 calc R A 1 C45A C 0.4966(11) 0.2038(7) 0.4507(7) 0.122(5) Uiso 0.448(8) 1 d P A 2 H45C H 0.5466 0.1795 0.431 0.146 Uiso 0.448(8) 1 calc PR A 2 H45D H 0.5198 0.2327 0.4852 0.146 Uiso 0.448(8) 1 calc PR A 2 C46A C 0.4339(6) 0.1610(4) 0.4747(4) 0.160(3) Uiso 0.448(8) 1 d P A 2 H46C H 0.4109 0.1786 0.5159 0.192 Uiso 0.448(8) 1 calc PR A 2 H46D H 0.4625 0.1182 0.4838 0.192 Uiso 0.448(8) 1 calc PR A 2 C47A C 0.3587(9) 0.1503(6) 0.4301(6) 0.097(4) Uiso 0.448(8) 1 d P A 2 H47C H 0.3611 0.1062 0.41 0.116 Uiso 0.448(8) 1 calc PR A 2 H47D H 0.301 0.156 0.4521 0.116 Uiso 0.448(8) 1 calc PR A 2 C48A C 0.3748(15) 0.2021(10) 0.3834(9) 0.155(7) Uiso 0.450(8) 1 d P A 2 H48C H 0.3869 0.182 0.3408 0.186 Uiso 0.450(8) 1 calc PR A 2 H48D H 0.3207 0.2294 0.3793 0.186 Uiso 0.450(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0479(4) 0.0457(3) 0.0450(3) 0.0026(3) 0.0029(3) 0.0033(3) K2 0.0487(4) 0.0460(4) 0.0489(4) -0.0027(3) -0.0010(3) 0.0061(3) Si1 0.0385(4) 0.0434(4) 0.0351(4) 0.0017(3) -0.0045(3) -0.0003(4) Si2 0.0368(4) 0.0442(4) 0.0362(4) 0.0002(3) -0.0038(3) -0.0009(4) N1 0.0402(14) 0.0408(13) 0.0356(13) 0.0056(10) -0.0048(10) 0.0001(11) N2 0.0365(14) 0.0432(13) 0.0369(13) 0.0010(11) -0.0009(10) 0.0007(11) N3 0.0382(14) 0.0453(14) 0.0340(13) 0.0026(11) 0.0003(10) -0.0043(11) N4 0.0390(14) 0.0407(13) 0.0369(13) 0.0045(11) -0.0033(10) -0.0007(11) C1 0.0336(16) 0.0497(17) 0.0421(18) 0.0003(13) -0.0094(13) 0.0083(13) C2 0.0327(16) 0.0465(17) 0.0458(17) -0.0068(14) -0.0047(12) 0.0047(13) C3 0.0400(18) 0.0533(19) 0.059(2) -0.0078(15) 0.0005(15) -0.0043(15) C4 0.0403(19) 0.061(2) 0.075(2) -0.0262(19) -0.0088(17) 0.0019(16) C5 0.050(2) 0.073(2) 0.050(2) -0.0200(18) -0.0088(16) 0.0120(18) C6 0.0439(19) 0.060(2) 0.0430(17) -0.0049(15) -0.0033(14) 0.0134(15) C7 0.0450(19) 0.0557(19) 0.0414(16) 0.0103(14) -0.0036(13) -0.0030(15) C8 0.056(2) 0.056(2) 0.059(2) 0.0224(17) -0.0148(17) -0.0041(16) C9 0.065(2) 0.064(2) 0.064(2) 0.0133(19) -0.0221(18) 0.0038(19) C10 0.094(3) 0.088(3) 0.104(3) 0.049(3) -0.027(3) -0.034(3) C11 0.096(3) 0.059(2) 0.076(3) -0.003(2) -0.021(2) 0.019(2) C12 0.0378(17) 0.0427(16) 0.0457(17) 0.0073(13) -0.0004(12) 0.0018(13) C13 0.0389(17) 0.0559(19) 0.0437(16) 0.0097(14) 0.0045(13) -0.0016(15) C14 0.0350(18) 0.081(3) 0.063(2) -0.0016(19) -0.0008(15) 0.0033(18) C15 0.065(3) 0.081(3) 0.061(2) 0.020(2) 0.0202(18) 0.003(2) C16 0.056(2) 0.056(2) 0.064(2) -0.0010(17) 0.0082(17) 0.0091(17) C17 0.0294(15) 0.0425(16) 0.0425(16) 0.0023(13) -0.0032(12) 0.0032(12) C18 0.0331(16) 0.0422(15) 0.0402(17) -0.0005(12) -0.0058(12) 0.0074(12) C19 0.0487(18) 0.0515(18) 0.0379(16) 0.0027(14) -0.0059(13) 0.0069(15) C20 0.051(2) 0.059(2) 0.0488(19) -0.0141(16) -0.0103(15) 0.0077(16) C21 0.048(2) 0.0513(19) 0.064(2) -0.0135(17) -0.0071(16) -0.0013(16) C22 0.0446(18) 0.0429(17) 0.0530(18) -0.0027(14) -0.0004(14) 0.0026(15) C23 0.0468(19) 0.0463(17) 0.0425(17) 0.0078(14) 0.0054(13) 0.0026(14) C24 0.047(2) 0.060(2) 0.0479(18) 0.0027(15) 0.0109(14) -0.0008(16) C25 0.079(3) 0.084(3) 0.064(2) 0.003(2) 0.032(2) -0.010(2) C26 0.057(2) 0.063(2) 0.070(2) -0.0089(19) 0.0135(18) 0.0082(18) C27 0.042(2) 0.101(3) 0.067(2) -0.015(2) 0.0047(16) 0.007(2) C28 0.0365(16) 0.0508(17) 0.0475(17) 0.0072(14) -0.0058(13) 0.0009(13) C29 0.052(2) 0.0462(18) 0.064(2) 0.0150(16) -0.0066(16) -0.0011(15) C30 0.111(4) 0.049(2) 0.094(3) -0.004(2) -0.008(3) 0.018(2) C31 0.081(3) 0.086(3) 0.113(4) 0.052(3) 0.004(3) -0.009(2) C32 0.059(2) 0.054(2) 0.101(3) 0.024(2) -0.029(2) 0.0037(18) O1 0.124(3) 0.0542(16) 0.095(2) 0.0115(15) 0.037(2) -0.0069(17) C33 0.127(4) 0.071(3) 0.078(3) 0.005(2) 0.018(3) -0.009(3) C34 0.152(5) 0.086(3) 0.104(4) 0.027(3) -0.006(4) 0.015(4) C35 0.121(5) 0.051(2) 0.142(5) -0.001(3) 0.003(4) -0.014(3) C36 0.122(4) 0.093(4) 0.103(4) -0.020(3) 0.017(3) 0.009(3) O2 0.0666(19) 0.098(2) 0.081(2) 0.0174(17) 0.0159(15) 0.0206(17) C37 0.144(5) 0.079(3) 0.074(3) 0.023(2) 0.034(3) 0.027(3) C38 0.099(5) 0.179(7) 0.120(5) 0.069(5) 0.006(4) 0.038(4) C39 0.062(3) 0.150(5) 0.070(3) 0.012(3) -0.005(2) 0.038(3) C40 0.070(3) 0.089(3) 0.057(2) -0.003(2) 0.0005(19) 0.014(2) O3 0.0751(19) 0.100(2) 0.0524(15) 0.0243(14) 0.0043(13) 0.0093(17) C41 0.064(3) 0.101(4) 0.096(3) -0.010(3) 0.002(2) 0.018(3) C42 0.090(4) 0.158(6) 0.211(9) 0.117(6) -0.052(5) -0.042(4) C43 0.098(4) 0.247(9) 0.069(3) 0.071(5) 0.006(3) 0.056(5) C44 0.164(6) 0.104(4) 0.060(3) -0.001(3) -0.017(3) 0.020(4) O4 0.182(5) 0.067(2) 0.145(3) 0.013(2) 0.019(3) -0.036(2) O5 0.076(2) 0.123(3) 0.0721(19) -0.0232(18) -0.0027(15) 0.0474(19) C49 0.094(3) 0.087(3) 0.058(2) -0.005(2) -0.005(2) 0.024(3) C50 0.070(3) 0.109(4) 0.105(4) -0.027(3) -0.019(3) 0.017(3) C51 0.072(3) 0.074(3) 0.071(3) -0.003(2) 0.010(2) 0.010(2) C52 0.073(3) 0.098(3) 0.064(2) -0.014(2) -0.003(2) 0.025(2) O6 0.084(2) 0.097(2) 0.0561(16) 0.0192(14) 0.0029(14) 0.0235(19) C53 0.173(6) 0.100(4) 0.062(3) -0.007(3) -0.027(3) 0.030(4) C54 0.146(6) 0.252(9) 0.061(3) 0.070(5) 0.038(4) 0.112(6) C55 0.108(5) 0.214(9) 0.159(7) 0.107(7) -0.019(5) -0.049(5) C56 0.059(3) 0.125(5) 0.105(4) 0.009(3) 0.004(3) 0.008(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.700(3) . ? K1 O3 2.763(3) . ? K1 O2 2.764(3) . ? K1 C20 3.140(3) . ? K1 C19 3.169(3) . ? K1 C21 3.220(4) . ? K1 C18 3.284(3) . ? K1 C22 3.344(3) . ? K1 C17 3.378(3) . ? K1 Si1 3.4114(10) . ? K2 O4 2.688(3) . ? K2 O5 2.744(3) . ? K2 O6 2.774(3) . ? K2 C5 3.134(3) . ? K2 C4 3.186(4) . ? K2 C6 3.198(3) . ? K2 C1 3.321(3) . ? K2 C3 3.327(3) . ? K2 C2 3.392(3) . ? K2 Si2 3.3997(10) . ? Si1 N2 1.841(3) . ? Si1 N1 1.843(2) . ? Si1 Si2 2.5061(11) . ? Si2 N3 1.839(3) . ? Si2 N4 1.841(2) . ? N1 C1 1.372(4) . ? N1 C7 1.453(4) . ? N2 C2 1.377(4) . ? N2 C12 1.446(4) . ? N3 C17 1.384(4) . ? N3 C23 1.453(4) . ? N4 C18 1.383(4) . ? N4 C28 1.450(4) . ? C1 C6 1.394(4) . ? C1 C2 1.435(4) . ? C2 C3 1.403(4) . ? C3 C4 1.398(5) . ? C4 C5 1.367(5) . ? C5 C6 1.399(5) . ? C7 C8 1.552(5) . ? C8 C10 1.514(5) . ? C8 C11 1.524(6) . ? C8 C9 1.528(5) . ? C12 C13 1.546(4) . ? C13 C14 1.517(5) . ? C13 C16 1.524(5) . ? C13 C15 1.524(4) . ? C17 C22 1.389(4) . ? C17 C18 1.435(4) . ? C18 C19 1.390(4) . ? C19 C20 1.402(5) . ? C20 C21 1.367(5) . ? C21 C22 1.411(5) . ? C23 C24 1.554(5) . ? C24 C26 1.518(5) . ? C24 C25 1.531(5) . ? C24 C27 1.533(5) . ? C28 C29 1.526(4) . ? C29 C30 1.493(6) . ? C29 C32 1.522(5) . ? C29 C31 1.529(5) . ? O1 C36 1.393(6) . ? O1 C33 1.421(5) . ? C33 C34 1.479(7) . ? C34 C35 1.472(7) . ? C35 C36 1.500(7) . ? O2 C40 1.406(5) . ? O2 C37 1.435(6) . ? C37 C38 1.489(8) . ? C38 C39 1.382(7) . ? C39 C40 1.483(6) . ? O3 C44 1.399(5) . ? O3 C41 1.430(6) . ? C41 C42 1.471(8) . ? C42 C43 1.442(10) . ? C43 C44 1.460(9) . ? O4 C48 1.358(10) . ? O4 C45 1.375(12) . ? O4 C48A 1.42(2) . ? O4 C45A 1.508(15) . ? C45 C46 1.581(13) . ? C46 C47 1.371(11) . ? C47 C48 1.488(12) . ? O5 C52 1.379(5) . ? O5 C49 1.423(5) . ? C49 C50 1.479(7) . ? C50 C51 1.492(6) . ? C51 C52 1.474(6) . ? O6 C56 1.416(6) . ? O6 C53 1.429(5) . ? C53 C54 1.524(9) . ? C54 C55 1.428(11) . ? C55 C56 1.433(8) . ? C47A C48A 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O3 134.74(10) . . ? O1 K1 O2 79.67(10) . . ? O3 K1 O2 77.63(9) . . ? O1 K1 C20 99.73(11) . . ? O3 K1 C20 77.55(9) . . ? O2 K1 C20 143.48(9) . . ? O1 K1 C19 121.69(11) . . ? O3 K1 C19 72.41(9) . . ? O2 K1 C19 150.02(9) . . ? C20 K1 C19 25.68(9) . . ? O1 K1 C21 77.53(11) . . ? O3 K1 C21 100.95(9) . . ? O2 K1 C21 145.53(10) . . ? C20 K1 C21 24.78(9) . . ? C19 K1 C21 44.28(9) . . ? O1 K1 C18 118.41(10) . . ? O3 K1 C18 91.29(8) . . ? O2 K1 C18 161.14(9) . . ? C20 K1 C18 44.27(8) . . ? C19 K1 C18 24.79(7) . . ? C21 K1 C18 51.14(8) . . ? O1 K1 C22 75.66(10) . . ? O3 K1 C22 120.18(9) . . ? O2 K1 C22 155.32(9) . . ? C20 K1 C22 43.42(9) . . ? C19 K1 C22 50.67(8) . . ? C21 K1 C22 24.73(8) . . ? C18 K1 C22 43.19(8) . . ? O1 K1 C17 94.77(9) . . ? O3 K1 C17 115.04(8) . . ? O2 K1 C17 165.31(8) . . ? C20 K1 C17 50.62(8) . . ? C19 K1 C17 43.48(7) . . ? C21 K1 C17 43.10(8) . . ? C18 K1 C17 24.83(7) . . ? C22 K1 C17 23.84(7) . . ? O1 K1 Si1 110.48(8) . . ? O3 K1 Si1 112.38(7) . . ? O2 K1 Si1 102.53(8) . . ? C20 K1 Si1 111.52(7) . . ? C19 K1 Si1 89.83(6) . . ? C21 K1 Si1 109.50(6) . . ? C18 K1 Si1 67.37(5) . . ? C22 K1 Si1 86.86(6) . . ? C17 K1 Si1 66.48(5) . . ? O4 K2 O5 76.97(15) . . ? O4 K2 O6 121.46(13) . . ? O5 K2 O6 79.20(10) . . ? O4 K2 C5 95.77(15) . . ? O5 K2 C5 145.86(9) . . ? O6 K2 C5 76.50(10) . . ? O4 K2 C4 76.15(14) . . ? O5 K2 C4 147.58(10) . . ? O6 K2 C4 99.89(10) . . ? C5 K2 C4 24.96(10) . . ? O4 K2 C6 119.85(14) . . ? O5 K2 C6 151.48(10) . . ? O6 K2 C6 72.35(9) . . ? C5 K2 C6 25.51(9) . . ? C4 K2 C6 44.16(10) . . ? O4 K2 C1 122.41(14) . . ? O5 K2 C1 160.31(11) . . ? O6 K2 C1 91.61(8) . . ? C5 K2 C1 44.01(8) . . ? C4 K2 C1 50.85(9) . . ? C6 K2 C1 24.61(8) . . ? O4 K2 C3 79.31(13) . . ? O5 K2 C3 155.35(11) . . ? O6 K2 C3 119.61(9) . . ? C5 K2 C3 43.65(10) . . ? C4 K2 C3 24.67(9) . . ? C6 K2 C3 50.72(9) . . ? C1 K2 C3 43.20(8) . . ? O4 K2 C2 101.05(13) . . ? O5 K2 C2 163.12(8) . . ? O6 K2 C2 115.04(8) . . ? C5 K2 C2 50.67(8) . . ? C4 K2 C2 43.08(8) . . ? C6 K2 C2 43.33(8) . . ? C1 K2 C2 24.66(8) . . ? C3 K2 C2 24.07(8) . . ? O4 K2 Si2 123.17(11) . . ? O5 K2 Si2 101.17(7) . . ? O6 K2 Si2 113.50(8) . . ? C5 K2 Si2 110.33(7) . . ? C4 K2 Si2 108.57(7) . . ? C6 K2 Si2 88.60(6) . . ? C1 K2 Si2 66.39(5) . . ? C3 K2 Si2 86.25(6) . . ? C2 K2 Si2 65.54(5) . . ? N2 Si1 N1 83.73(11) . . ? N2 Si1 Si2 99.54(9) . . ? N1 Si1 Si2 98.86(8) . . ? N2 Si1 K1 131.43(8) . . ? N1 Si1 K1 135.66(8) . . ? Si2 Si1 K1 99.93(3) . . ? N3 Si2 N4 84.04(11) . . ? N3 Si2 Si1 100.78(9) . . ? N4 Si2 Si1 98.70(8) . . ? N3 Si2 K2 128.72(8) . . ? N4 Si2 K2 136.32(8) . . ? Si1 Si2 K2 101.39(3) . . ? C1 N1 C7 121.6(2) . . ? C1 N1 Si1 112.28(19) . . ? C7 N1 Si1 122.1(2) . . ? C2 N2 C12 121.7(3) . . ? C2 N2 Si1 112.0(2) . . ? C12 N2 Si1 124.11(19) . . ? C17 N3 C23 122.0(2) . . ? C17 N3 Si2 112.24(19) . . ? C23 N3 Si2 123.7(2) . . ? C18 N4 C28 121.0(2) . . ? C18 N4 Si2 112.38(19) . . ? C28 N4 Si2 122.2(2) . . ? N1 C1 C6 129.0(3) . . ? N1 C1 C2 111.9(3) . . ? C6 C1 C2 119.1(3) . . ? N1 C1 K2 117.01(18) . . ? C6 C1 K2 72.75(18) . . ? C2 C1 K2 80.45(17) . . ? N2 C2 C3 129.0(3) . . ? N2 C2 C1 111.8(3) . . ? C3 C2 C1 119.2(3) . . ? N2 C2 K2 119.80(18) . . ? C3 C2 K2 75.38(18) . . ? C1 C2 K2 74.90(17) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 K2 72.0(2) . . ? C2 C3 K2 80.55(19) . . ? C5 C4 C3 121.2(3) . . ? C5 C4 K2 75.4(2) . . ? C3 C4 K2 83.3(2) . . ? C4 C5 C6 120.3(3) . . ? C4 C5 K2 79.6(2) . . ? C6 C5 K2 79.78(19) . . ? C1 C6 C5 120.5(3) . . ? C1 C6 K2 82.64(18) . . ? C5 C6 K2 74.71(19) . . ? N1 C7 C8 115.2(3) . . ? C10 C8 C11 110.0(4) . . ? C10 C8 C9 109.9(3) . . ? C11 C8 C9 108.9(3) . . ? C10 C8 C7 107.6(3) . . ? C11 C8 C7 109.7(3) . . ? C9 C8 C7 110.7(3) . . ? N2 C12 C13 115.6(2) . . ? C14 C13 C16 108.3(3) . . ? C14 C13 C15 110.3(3) . . ? C16 C13 C15 109.9(3) . . ? C14 C13 C12 110.7(3) . . ? C16 C13 C12 109.5(3) . . ? C15 C13 C12 108.2(3) . . ? N3 C17 C22 128.8(3) . . ? N3 C17 C18 111.6(3) . . ? C22 C17 C18 119.5(3) . . ? N3 C17 K1 119.33(17) . . ? C22 C17 K1 76.69(18) . . ? C18 C17 K1 73.90(16) . . ? N4 C18 C19 129.1(3) . . ? N4 C18 C17 112.0(2) . . ? C19 C18 C17 118.9(3) . . ? N4 C18 K1 115.29(18) . . ? C19 C18 K1 72.97(17) . . ? C17 C18 K1 81.28(16) . . ? C18 C19 C20 120.5(3) . . ? C18 C19 K1 82.23(17) . . ? C20 C19 K1 76.00(18) . . ? C21 C20 C19 120.8(3) . . ? C21 C20 K1 80.9(2) . . ? C19 C20 K1 78.32(18) . . ? C20 C21 C22 120.0(3) . . ? C20 C21 K1 74.3(2) . . ? C22 C21 K1 82.6(2) . . ? C17 C22 C21 120.3(3) . . ? C17 C22 K1 79.47(18) . . ? C21 C22 K1 72.70(19) . . ? N3 C23 C24 114.3(3) . . ? C26 C24 C25 109.1(3) . . ? C26 C24 C27 109.2(3) . . ? C25 C24 C27 110.5(3) . . ? C26 C24 C23 109.8(3) . . ? C25 C24 C23 107.4(3) . . ? C27 C24 C23 110.7(3) . . ? N4 C28 C29 116.5(3) . . ? C30 C29 C32 109.5(4) . . ? C30 C29 C28 109.8(3) . . ? C32 C29 C28 110.5(3) . . ? C30 C29 C31 110.1(4) . . ? C32 C29 C31 109.5(3) . . ? C28 C29 C31 107.4(3) . . ? C36 O1 C33 109.1(4) . . ? C36 O1 K1 133.3(3) . . ? C33 O1 K1 117.6(2) . . ? O1 C33 C34 102.4(4) . . ? C35 C34 C33 103.3(4) . . ? C34 C35 C36 102.5(4) . . ? O1 C36 C35 107.1(4) . . ? C40 O2 C37 107.3(3) . . ? C40 O2 K1 122.0(2) . . ? C37 O2 K1 115.2(3) . . ? O2 C37 C38 106.1(4) . . ? C39 C38 C37 107.6(5) . . ? C38 C39 C40 107.7(4) . . ? O2 C40 C39 106.4(3) . . ? C44 O3 C41 109.1(4) . . ? C44 O3 K1 132.4(3) . . ? C41 O3 K1 114.0(3) . . ? O3 C41 C42 106.2(4) . . ? C43 C42 C41 105.1(5) . . ? C42 C43 C44 105.6(5) . . ? O3 C44 C43 107.5(5) . . ? C48 O4 C45 111.9(7) . . ? C48 O4 C48A 48.7(9) . . ? C45 O4 C48A 81.4(10) . . ? C48 O4 C45A 86.4(7) . . ? C45 O4 C45A 61.1(7) . . ? C48A O4 C45A 104.1(10) . . ? C48 O4 K2 137.0(5) . . ? C45 O4 K2 111.1(6) . . ? C48A O4 K2 140.0(9) . . ? C45A O4 K2 115.3(6) . . ? O4 C45 C46 100.5(8) . . ? C47 C46 C45 101.1(8) . . ? C46 C47 C48 108.6(8) . . ? O4 C48 C47 104.5(7) . . ? C52 O5 C49 109.0(3) . . ? C52 O5 K2 123.8(2) . . ? C49 O5 K2 127.1(2) . . ? O5 C49 C50 105.1(4) . . ? C49 C50 C51 105.1(4) . . ? C52 C51 C50 103.7(4) . . ? O5 C52 C51 109.8(4) . . ? C56 O6 C53 109.3(4) . . ? C56 O6 K2 110.4(3) . . ? C53 O6 K2 134.8(3) . . ? O6 C53 C54 103.7(5) . . ? C55 C54 C53 104.1(4) . . ? C54 C55 C56 105.1(7) . . ? O6 C56 C55 107.2(5) . . ? O4 C48A C47A 112.8(14) . . ? #===END data_(12)-nov1302 _database_code_depnum_ccdc_archive 'CCDC 286730' _audit_creation_date 2002-11-08T13:29:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (Na(thf)6)(Na(thf)5)((Si(NCH2tBu)2C6H4)3) _chemical_formula_moiety 'C48 H78 N6 Si3, C24 H48 Na O6, C20 H40 Na O5' _chemical_formula_sum 'C92 H166 N6 Na2 O11 Si3' _chemical_formula_weight 1662.56 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m _symmetry_space_group_name_Hall '-P 6c' _symmetry_Int_Tables_number 176 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' 'y, -x+y, z+1/2' '-x+y, -x, z' 'x-y, x, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' '-y, x-y, -z-1/2' 'x-y, x, -z' '-x+y, -x, -z-1/2' _cell_length_a 15.0722(1) _cell_length_b 15.0722(1) _cell_length_c 25.4341(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5003.80(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 52369 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_unetI/netI 0.0184 _diffrn_reflns_number 51637 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 3004 _reflns_number_gt 2638 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The [Na(thf)5] cation shows disorder of the thf group lying on the 3-fold axis, and also for one of the C atoms in the other thf group. H atoms were omitted for the former thf. 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^)+(0.0948P)^2^+4.9246P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 3004 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.076 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.738 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.054 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' 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 Si Si 0.57100(7) 0.26082(7) 0.75 0.0266(3) Uani 1 2 d S . . N N 0.46830(15) 0.18913(15) 0.70181(8) 0.0313(5) Uani 1 1 d . . . C1 C 0.37058(17) 0.14999(17) 0.72173(10) 0.0314(6) Uani 1 1 d . . . C2 C 0.27849(19) 0.1162(2) 0.69518(12) 0.0399(6) Uani 1 1 d . . . H2 H 0.2777 0.116 0.6578 0.048 Uiso 1 1 calc R . . C3 C 0.1869(2) 0.0824(2) 0.72294(13) 0.0463(7) Uani 1 1 d . . . H3 H 0.1245 0.0594 0.7043 0.056 Uiso 1 1 calc R . . C4 C 0.48753(19) 0.19575(19) 0.64559(10) 0.0347(6) Uani 1 1 d . . . C5 C 0.4833(2) 0.1006(2) 0.61940(11) 0.0414(6) Uani 1 1 d . . . C6 C 0.3731(2) 0.0136(2) 0.61137(15) 0.0594(9) Uani 1 1 d . . . H6A H 0.3355 0.0384 0.5902 0.089 Uiso 1 1 calc R . . H6B H 0.3396 -0.0098 0.6456 0.089 Uiso 1 1 calc R . . H6C H 0.3736 -0.0434 0.5931 0.089 Uiso 1 1 calc R . . C7 C 0.5346(3) 0.1352(3) 0.56522(12) 0.0623(9) Uani 1 1 d . . . H7A H 0.4972 0.1603 0.5441 0.093 Uiso 1 1 calc R . . H7B H 0.5335 0.0772 0.5473 0.093 Uiso 1 1 calc R . . H7C H 0.6056 0.1903 0.5698 0.093 Uiso 1 1 calc R . . C8 C 0.5408(2) 0.0617(2) 0.65263(13) 0.0506(7) Uani 1 1 d . . . H8A H 0.6114 0.1172 0.658 0.076 Uiso 1 1 calc R . . H8B H 0.5413 0.0046 0.6345 0.076 Uiso 1 1 calc R . . H8C H 0.5068 0.0384 0.6868 0.076 Uiso 1 1 calc R . . Na1 Na 0 0 0.5 0.0416(6) Uani 1 6 d S . 1 O1 O 0.12922(16) 0.13746(16) 0.55240(8) 0.0542(6) Uani 1 1 d . A 1 C9 C 0.2330(3) 0.2016(3) 0.53767(17) 0.0732(11) Uani 1 1 d . A 1 H9A H 0.2386 0.2105 0.499 0.088 Uiso 1 1 calc R A 1 H9B H 0.2746 0.1709 0.5489 0.088 Uiso 1 1 calc R A 1 C10 C 0.2695(4) 0.3007(4) 0.5635(3) 0.118(2) Uani 1 1 d . A 1 H10A H 0.3343 0.3213 0.5825 0.141 Uiso 1 1 calc R A 1 H10B H 0.282 0.3541 0.5372 0.141 Uiso 1 1 calc R A 1 C11 C 0.1935(4) 0.2894(4) 0.5988(3) 0.130(2) Uani 1 1 d . A 1 H11A H 0.1672 0.3356 0.5889 0.156 Uiso 1 1 calc R A 1 H11B H 0.222 0.3073 0.6348 0.156 Uiso 1 1 calc R A 1 C12 C 0.1092(3) 0.1814(3) 0.59717(14) 0.0685(10) Uani 1 1 d . A 1 H12A H 0.1087 0.1448 0.6296 0.082 Uiso 1 1 calc R A 1 H12B H 0.0421 0.1778 0.5937 0.082 Uiso 1 1 calc R A 1 Na2 Na 0.6667 0.3333 0.25 0.0540(8) Uani 1 6 d S . 2 O2 O 0.4935(3) 0.2363(3) 0.25 0.0818(12) Uani 1 2 d S . 2 O3 O 0.6667 0.3333 0.3439(2) 0.0880(15) Uani 1 3 d S . 2 C13 C 0.4587(5) 0.1326(5) 0.2677(3) 0.0655(19) Uiso 0.5 1 d P . 2 H13A H 0.5014 0.1062 0.2523 0.079 Uiso 0.5 1 calc PR . 2 H13B H 0.4623 0.1302 0.3065 0.079 Uiso 0.5 1 calc PR . 2 C14 C 0.3543(4) 0.0728(5) 0.25 0.0864(19) Uani 1 2 d S . 2 H14A H 0.3136 0.0151 0.2743 0.104 Uiso 0.5 1 calc PR . 2 H14B H 0.3512 0.0453 0.2143 0.104 Uiso 0.5 1 calc PR . 2 C15 C 0.3164(4) 0.1472(5) 0.25 0.0821(17) Uani 1 2 d S . 2 H15A H 0.2745 0.1381 0.2183 0.099 Uiso 0.5 1 calc PR . 2 H15B H 0.2745 0.1381 0.2817 0.099 Uiso 0.5 1 calc PR . 2 C16 C 0.4092(5) 0.2482(5) 0.25 0.095(2) Uani 1 2 d S . 2 H16A H 0.4101 0.2871 0.2185 0.114 Uiso 0.5 1 calc PR . 2 H16B H 0.4101 0.2871 0.2815 0.114 Uiso 0.5 1 calc PR . 2 C18 C 0.7237(10) 0.3766(18) 0.4290(4) 0.176(6) Uani 0.67 1 d P . 2 C17 C 0.656(2) 0.3989(16) 0.3760(4) 0.246(9) Uani 0.67 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0228(5) 0.0236(5) 0.0323(5) 0 0 0.0108(4) N 0.0260(10) 0.0305(11) 0.0345(11) -0.0015(8) -0.0017(8) 0.0118(8) C1 0.0271(12) 0.0220(11) 0.0446(14) -0.0012(10) -0.0017(10) 0.0121(10) C2 0.0325(13) 0.0340(13) 0.0519(16) -0.0011(11) -0.0069(12) 0.0158(11) C3 0.0267(13) 0.0386(14) 0.0713(18) -0.0009(13) -0.0077(12) 0.0145(11) C4 0.0366(13) 0.0314(13) 0.0329(13) -0.0006(10) -0.0026(10) 0.0145(11) C5 0.0399(14) 0.0393(14) 0.0398(14) -0.0063(12) -0.0012(12) 0.0160(12) C6 0.0487(18) 0.0436(17) 0.076(2) -0.0215(16) -0.0091(16) 0.0161(14) C7 0.069(2) 0.068(2) 0.0431(17) -0.0094(16) 0.0039(16) 0.0291(18) C8 0.0552(18) 0.0447(16) 0.0591(19) -0.0059(14) -0.0002(14) 0.0304(14) Na1 0.0395(9) 0.0395(9) 0.0459(15) 0 0 0.0198(4) O1 0.0529(13) 0.0497(12) 0.0538(13) -0.0124(10) -0.0032(10) 0.0209(10) C9 0.054(2) 0.083(3) 0.074(2) -0.019(2) -0.0005(18) 0.0280(19) C10 0.088(3) 0.075(3) 0.135(5) -0.037(3) -0.002(3) 0.000(3) C11 0.096(4) 0.098(4) 0.175(6) -0.086(4) -0.001(4) 0.032(3) C12 0.077(2) 0.086(3) 0.051(2) -0.0108(18) -0.0006(18) 0.047(2) Na2 0.0463(10) 0.0463(10) 0.069(2) 0 0 0.0232(5) O2 0.0440(18) 0.056(2) 0.139(4) 0 0 0.0203(16) O3 0.099(2) 0.099(2) 0.066(3) 0 0 0.0496(12) C14 0.051(3) 0.062(3) 0.137(6) 0 0 0.022(3) C15 0.051(3) 0.098(4) 0.107(5) 0 0 0.044(3) C16 0.067(4) 0.077(4) 0.156(7) 0 0 0.048(3) C18 0.142(11) 0.212(17) 0.076(5) 0.008(8) -0.031(6) 0.014(9) C17 0.55(3) 0.32(2) 0.076(6) 0.021(9) 0.058(12) 0.37(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si N 1.842(2) . ? Si Si 2.2567(15) 5_665 ? N C1 1.380(3) . ? N C4 1.453(3) . ? C1 C2 1.391(4) . ? C1 C1 1.438(5) 8_557 ? C2 C3 1.401(4) . ? C3 C3 1.376(6) 8_557 ? C4 C5 1.553(4) . ? C5 C8 1.523(4) . ? C5 C6 1.530(4) . ? C5 C7 1.538(4) . ? Na1 O1 2.414(2) . ? O1 C9 1.417(4) . ? O1 C12 1.423(4) . ? C9 C10 1.465(6) . ? C10 C11 1.396(7) . ? C11 C12 1.482(6) . ? Na2 O2 2.265(3) . ? Na2 O3 2.387(5) . ? O2 C16 1.369(7) . ? O2 C13 1.449(7) 8_556 ? O2 C13 1.449(7) . ? O3 C17 1.351(10) 5_665 ? O3 C17 1.351(10) 3_655 ? O3 C17 1.351(10) . ? C13 C14 1.439(8) . ? C14 C15 1.491(8) . ? C15 C16 1.465(9) . ? C18 C18 1.345(17) 3_655 ? C18 C18 1.345(17) 5_665 ? C18 C17 1.51(2) 5_665 ? C18 C17 1.82(2) . ? C17 C18 1.51(2) 3_655 ? C17 C17 1.861(18) 5_665 ? C17 C17 1.861(17) 3_655 ? 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 N Si N 83.42(13) . 8_557 ? N Si Si 128.39(7) . 5_665 ? N Si Si 132.01(7) . 3_655 ? Si Si Si 60 5_665 3_655 ? C1 N C4 121.6(2) . . ? C1 N Si 114.24(16) . . ? C4 N Si 122.31(16) . . ? N C1 C2 129.4(2) . . ? N C1 C1 111.54(13) . 8_557 ? C2 C1 C1 119.04(16) . 8_557 ? C1 C2 C3 120.7(3) . . ? C3 C3 C2 120.27(17) 8_557 . ? N C4 C5 116.4(2) . . ? C8 C5 C6 109.1(3) . . ? C8 C5 C7 110.0(3) . . ? C6 C5 C7 108.5(3) . . ? C8 C5 C4 110.4(2) . . ? C6 C5 C4 112.0(2) . . ? C7 C5 C4 106.8(2) . . ? O1 Na1 O1 180 7_556 . ? O1 Na1 O1 92.45(7) . 5 ? O1 Na1 O1 87.55(7) . 9_556 ? O1 Na1 O1 92.45(7) 9_556 11_556 ? C9 O1 C12 108.2(3) . . ? C9 O1 Na1 125.5(2) . . ? C12 O1 Na1 125.0(2) . . ? O1 C9 C10 107.5(3) . . ? C11 C10 C9 107.3(4) . . ? C10 C11 C12 108.5(4) . . ? O1 C12 C11 105.6(3) . . ? O2 Na2 O2 120 3_655 . ? O2 Na2 O3 90 . . ? O3 Na2 O3 180 8_556 . ? C16 O2 C13 106.4(4) . . ? C16 O2 Na2 139.5(4) . . ? C13 O2 Na2 112.1(3) . . ? C17 O3 C17 87.1(7) 3_655 . ? C17 O3 Na2 127.3(5) . . ? C14 C13 O2 105.8(5) . . ? C13 C14 C15 103.8(5) . . ? C16 C15 C14 104.8(4) . . ? O2 C16 C15 109.3(5) . . ? C18 C18 C17 104.9(7) 3_655 5_665 ? O3 C17 C18 106.9(13) . 3_655 ? #===END data_(13)-apr404 _database_code_depnum_ccdc_archive 'CCDC 286731' _audit_creation_date 2004-04-15T11:18:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety ; C64 H104 N8 Si4, C24 H48 Na O6, C20 H40 Na O5, 2(C4 H8 O) ; _chemical_formula_sum 'C116 H208 N8 Na2 O13 Si4' _chemical_formula_weight 2081.24 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3212(2) _cell_length_b 15.2868(2) _cell_length_c 28.9584(4) _cell_angle_alpha 85.999(1) _cell_angle_beta 79.241(1) _cell_angle_gamma 89.254(1) _cell_volume 6213.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 76591 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.346375E-1 _diffrn_orient_matrix_ub_12 0.203919E-1 _diffrn_orient_matrix_ub_13 0.306239E-1 _diffrn_orient_matrix_ub_21 0.597654E-1 _diffrn_orient_matrix_ub_22 0.27484E-1 _diffrn_orient_matrix_ub_23 0.52968E-2 _diffrn_orient_matrix_ub_31 -0.167369E-1 _diffrn_orient_matrix_ub_32 0.559372E-1 _diffrn_orient_matrix_ub_33 -0.165977E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_number 82730 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 21654 _reflns_number_gt 16448 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; All the thf moieties are poorly defined. After lengthy and unsuccessful attempts to refine these groups with anisotopic ADPs and allowing for disorder I finally decided to leave the thf C atoms isotropic, model the obvious disorder in two thfs, constrain the C-O and C-C bond lengths to idealised values, and apply SADi constraints to non-bonded distances. One tBu group is also disodered. 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^)+(0.1843P)^2^+18.8612P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 21654 _refine_ls_number_parameters 1056 _refine_ls_number_restraints 744 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.3128 _refine_ls_wR_factor_gt 0.2858 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 4.701 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.318 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si1 Si 0.7621(4) 0.1319(3) 0.20694(17) 0.0223(12) Uani 1 1 d . . . Si2 Si 0.7586(4) 0.0487(3) 0.27708(17) 0.0226(12) Uani 1 1 d . . . Si3 Si 0.8315(3) 0.1656(3) 0.30291(17) 0.0217(12) Uani 1 1 d . . . Si4 Si 0.8887(4) 0.2070(3) 0.22440(17) 0.0223(12) Uani 1 1 d . . . N1 N 0.7728(12) 0.0756(11) 0.1528(6) 0.029(4) Uani 1 1 d . . . N2 N 0.6522(11) 0.1770(11) 0.1906(6) 0.028(4) Uani 1 1 d . . . N3 N 0.8001(12) -0.0637(10) 0.2868(6) 0.029(4) Uani 1 1 d . . . N4 N 0.6464(11) 0.0089(11) 0.3116(6) 0.028(4) Uani 1 1 d . . . N5 N 0.9146(11) 0.1475(11) 0.3432(6) 0.027(3) Uani 1 1 d . . . N6 N 0.7784(11) 0.2472(11) 0.3433(6) 0.028(4) Uani 1 1 d . . . N7 N 1.0082(11) 0.1973(10) 0.1886(6) 0.028(4) Uani 1 1 d . . . N8 N 0.9011(12) 0.3224(10) 0.2051(6) 0.028(4) Uani 1 1 d . . . C1 C 0.6861(15) 0.0658(14) 0.1391(7) 0.034(5) Uani 1 1 d . . . C2 C 0.6166(15) 0.1261(14) 0.1602(7) 0.033(4) Uani 1 1 d . . . C3 C 0.5251(17) 0.1251(17) 0.1499(9) 0.045(6) Uani 1 1 d . . . H3 H 0.4788 0.1661 0.163 0.054 Uiso 1 1 calc R . . C4 C 0.5019(19) 0.063(2) 0.1205(10) 0.057(7) Uani 1 1 d . . . H4 H 0.4395 0.0626 0.1138 0.069 Uiso 1 1 calc R . . C5 C 0.567(2) 0.005(2) 0.1014(10) 0.060(7) Uani 1 1 d . . . H5 H 0.55 -0.0366 0.0815 0.072 Uiso 1 1 calc R . . C6 C 0.6599(18) 0.0049(16) 0.1108(9) 0.045(6) Uani 1 1 d . . . H6 H 0.7048 -0.0371 0.0977 0.054 Uiso 1 1 calc R . . C7 C 0.8601(15) 0.0435(13) 0.1250(7) 0.033(5) Uani 1 1 d . . . H7A H 0.8508 -0.019 0.12 0.04 Uiso 1 1 calc R . . H7B H 0.911 0.046 0.1438 0.04 Uiso 1 1 calc R . . C8 C 0.8955(16) 0.0927(15) 0.0761(7) 0.038(5) Uani 1 1 d . . . C9 C 0.8804(18) 0.1909(15) 0.0787(8) 0.044(5) Uani 1 1 d . . . H9A H 0.9104 0.2114 0.1037 0.066 Uiso 1 1 calc R . . H9B H 0.8122 0.2035 0.0855 0.066 Uiso 1 1 calc R . . H9C H 0.9091 0.221 0.0485 0.066 Uiso 1 1 calc R . . C10 C 0.848(2) 0.0610(19) 0.0372(8) 0.051(6) Uani 1 1 d . . . H10A H 0.7796 0.0734 0.0444 0.077 Uiso 1 1 calc R . . H10B H 0.8578 -0.0023 0.0352 0.077 Uiso 1 1 calc R . . H10C H 0.8758 0.0915 0.007 0.077 Uiso 1 1 calc R . . C11 C 1.0000(18) 0.0718(19) 0.0634(9) 0.052(6) Uani 1 1 d D . . H11A H 1.0328 0.0916 0.0876 0.079 Uiso 1 1 calc R . . H11B H 1.0267 0.1019 0.0329 0.079 Uiso 1 1 calc R . . H11C H 1.0083 0.0084 0.0615 0.079 Uiso 1 1 calc R . . C12 C 0.5982(15) 0.2470(14) 0.2141(7) 0.033(4) Uani 1 1 d . . . H12A H 0.623 0.2561 0.2431 0.039 Uiso 1 1 calc R . . H12B H 0.5315 0.2272 0.224 0.039 Uiso 1 1 calc R . . C13 C 0.5981(16) 0.3374(15) 0.1856(8) 0.038(5) Uani 1 1 d . . . C14 C 0.581(2) 0.4068(17) 0.2220(10) 0.055(7) Uani 1 1 d . . . H14A H 0.5197 0.3961 0.243 0.083 Uiso 1 1 calc R . . H14B H 0.5812 0.4652 0.2058 0.083 Uiso 1 1 calc R . . H14C H 0.6319 0.4033 0.2406 0.083 Uiso 1 1 calc R . . C15 C 0.6935(19) 0.3527(16) 0.1529(8) 0.048(6) Uani 1 1 d . . . H15A H 0.7443 0.3493 0.1715 0.071 Uiso 1 1 calc R . . H15B H 0.694 0.4109 0.1364 0.071 Uiso 1 1 calc R . . H15C H 0.7038 0.3079 0.1299 0.071 Uiso 1 1 calc R . . C16 C 0.516(2) 0.346(2) 0.1593(12) 0.068(8) Uani 1 1 d D . . H16A H 0.4563 0.3353 0.1815 0.102 Uiso 1 1 calc R . . H16B H 0.5238 0.3029 0.1353 0.102 Uiso 1 1 calc R . . H16C H 0.5159 0.4052 0.144 0.102 Uiso 1 1 calc R . . C17 C 0.7454(15) -0.1090(13) 0.3255(7) 0.031(4) Uani 1 1 d . . . C18 C 0.6578(14) -0.0655(13) 0.3408(7) 0.031(4) Uani 1 1 d . . . C19 C 0.5980(17) -0.0964(16) 0.3822(8) 0.042(5) Uani 1 1 d . . . H19 H 0.5407 -0.0663 0.3934 0.05 Uiso 1 1 calc R . . C20 C 0.6229(19) -0.1720(18) 0.4070(9) 0.051(6) Uani 1 1 d . . . H20 H 0.5817 -0.1937 0.4349 0.062 Uiso 1 1 calc R . . C21 C 0.706(2) -0.2153(17) 0.3917(9) 0.053(7) Uani 1 1 d . . . H21 H 0.7211 -0.267 0.4088 0.063 Uiso 1 1 calc R . . C22 C 0.7680(17) -0.1842(14) 0.3509(8) 0.041(5) Uani 1 1 d . . . H22 H 0.8257 -0.2144 0.3407 0.049 Uiso 1 1 calc R . . C23 C 0.8892(15) -0.0973(13) 0.2631(8) 0.034(5) Uani 1 1 d . . . H23A H 0.9232 -0.1244 0.2873 0.041 Uiso 1 1 calc R . . H23B H 0.928 -0.0471 0.247 0.041 Uiso 1 1 calc R . . C24 C 0.8846(19) -0.1659(14) 0.2261(9) 0.045(6) Uani 1 1 d . . . C25 C 0.799(2) -0.1467(18) 0.2025(10) 0.058(7) Uani 1 1 d . . . H25A H 0.7403 -0.1531 0.2261 0.087 Uiso 1 1 calc R . . H25B H 0.798 -0.1881 0.1782 0.087 Uiso 1 1 calc R . . H25C H 0.8033 -0.0867 0.188 0.087 Uiso 1 1 calc R . . C26 C 0.976(2) -0.156(2) 0.1899(11) 0.068(8) Uani 1 1 d . . . H26A H 0.9816 -0.0961 0.1755 0.102 Uiso 1 1 calc R . . H26B H 0.9761 -0.1974 0.1655 0.102 Uiso 1 1 calc R . . H26C H 1.0307 -0.1689 0.2055 0.102 Uiso 1 1 calc R . . C27 C 0.872(3) -0.2594(17) 0.2489(12) 0.084(11) Uani 1 1 d . . . H27A H 0.8129 -0.2636 0.2719 0.126 Uiso 1 1 calc R . . H27B H 0.9259 -0.2741 0.2648 0.126 Uiso 1 1 calc R . . H27C H 0.8708 -0.3005 0.2245 0.126 Uiso 1 1 calc R . . C28 C 0.5536(14) 0.0480(14) 0.3119(8) 0.035(5) Uani 1 1 d . . . H28A H 0.5629 0.1071 0.2954 0.041 Uiso 1 1 calc R . . H28B H 0.5238 0.0561 0.345 0.041 Uiso 1 1 calc R . . C29 C 0.4828(17) -0.0025(19) 0.2893(9) 0.052(7) Uani 1 1 d . . . C30 C 0.535(2) -0.046(2) 0.2454(10) 0.067(8) Uani 1 1 d . . . H30A H 0.4887 -0.0778 0.2318 0.1 Uiso 1 1 calc R . . H30B H 0.5828 -0.0863 0.2541 0.1 Uiso 1 1 calc R . . H30C H 0.5653 -0.0002 0.2221 0.1 Uiso 1 1 calc R . . C31 C 0.410(2) 0.064(3) 0.2766(14) 0.083(11) Uani 1 1 d . . . H31A H 0.3781 0.0908 0.3051 0.125 Uiso 1 1 calc R . . H31B H 0.3633 0.0348 0.2624 0.125 Uiso 1 1 calc R . . H31C H 0.4427 0.1099 0.2541 0.125 Uiso 1 1 calc R . . C32 C 0.428(2) -0.074(2) 0.3233(11) 0.072(9) Uani 1 1 d . . . H32A H 0.3959 -0.0476 0.3519 0.108 Uiso 1 1 calc R . . H32B H 0.4731 -0.1186 0.3317 0.108 Uiso 1 1 calc R . . H32C H 0.3815 -0.101 0.3081 0.108 Uiso 1 1 calc R . . C33 C 0.9190(14) 0.2187(14) 0.3699(7) 0.031(4) Uani 1 1 d . . . C34 C 0.8394(14) 0.2749(13) 0.3708(7) 0.029(4) Uani 1 1 d . . . C35 C 0.8340(16) 0.3506(14) 0.3958(8) 0.037(5) Uani 1 1 d . . . H35 H 0.7809 0.3888 0.3967 0.045 Uiso 1 1 calc R . . C36 C 0.9068(18) 0.3697(16) 0.4194(8) 0.045(6) Uani 1 1 d . . . H36 H 0.9026 0.4208 0.4365 0.053 Uiso 1 1 calc R . . C37 C 0.9853(18) 0.3155(18) 0.4181(9) 0.049(6) Uani 1 1 d . . . H37 H 1.0345 0.3294 0.4343 0.059 Uiso 1 1 calc R . . C38 C 0.9919(16) 0.2401(16) 0.3930(8) 0.039(5) Uani 1 1 d . . . H38 H 1.0462 0.2033 0.3916 0.047 Uiso 1 1 calc R . . C39 C 0.9715(15) 0.0695(15) 0.3485(8) 0.036(5) Uani 1 1 d . . . H39A H 1.0383 0.088 0.3463 0.043 Uiso 1 1 calc R . . H39B H 0.9696 0.0336 0.3215 0.043 Uiso 1 1 calc R . . C40 C 0.9421(18) 0.0098(15) 0.3950(8) 0.043(5) Uani 1 1 d . . . C41 C 0.8347(18) 0.0043(18) 0.4090(9) 0.051(6) Uani 1 1 d . . . H41A H 0.8081 -0.0163 0.3829 0.077 Uiso 1 1 calc R . . H41B H 0.8091 0.0624 0.4164 0.077 Uiso 1 1 calc R . . H41C H 0.8177 -0.0368 0.4368 0.077 Uiso 1 1 calc R . . C42 C 0.983(2) 0.041(2) 0.4361(10) 0.061(7) Uani 1 1 d . . . H42A H 1.0527 0.0454 0.427 0.091 Uiso 1 1 calc R . . H42B H 0.9668 -0.0009 0.4635 0.091 Uiso 1 1 calc R . . H42C H 0.957 0.0988 0.4441 0.091 Uiso 1 1 calc R . . C43 C 0.983(3) -0.0811(19) 0.3847(12) 0.069(9) Uani 1 1 d . . . H43A H 0.959 -0.1026 0.3581 0.104 Uiso 1 1 calc R . . H43B H 0.9648 -0.1216 0.4126 0.104 Uiso 1 1 calc R . . H43C H 1.0529 -0.0773 0.3767 0.104 Uiso 1 1 calc R . . C44 C 0.6863(15) 0.2874(14) 0.3429(7) 0.033(4) Uani 1 1 d . . . H44A H 0.6657 0.2737 0.3134 0.039 Uiso 1 1 calc R . . H44B H 0.6942 0.3518 0.3418 0.039 Uiso 1 1 calc R . . C45 C 0.6046(15) 0.2602(14) 0.3850(8) 0.036(5) Uani 1 1 d . . . C46 C 0.5117(17) 0.2721(18) 0.3663(10) 0.050(6) Uani 1 1 d . . . H46A H 0.5051 0.3337 0.3555 0.075 Uiso 1 1 calc R . . H46B H 0.4579 0.2554 0.3915 0.075 Uiso 1 1 calc R . . H46C H 0.5127 0.235 0.34 0.075 Uiso 1 1 calc R . . C47 C 0.6007(19) 0.3175(18) 0.4268(9) 0.050(6) Uani 1 1 d . . . H47A H 0.593 0.3791 0.4164 0.076 Uiso 1 1 calc R . . H47B H 0.6598 0.3106 0.4392 0.076 Uiso 1 1 calc R . . H47C H 0.5467 0.2995 0.4517 0.076 Uiso 1 1 calc R . . C48 C 0.6175(16) 0.1646(15) 0.4022(8) 0.041(5) Uani 1 1 d . . . H48A H 0.62 0.127 0.3759 0.061 Uiso 1 1 calc R . . H48B H 0.564 0.1468 0.4273 0.061 Uiso 1 1 calc R . . H48C H 0.6769 0.1587 0.4143 0.061 Uiso 1 1 calc R . . C49 C 1.0271(14) 0.2644(13) 0.1534(7) 0.030(4) Uani 1 1 d . . . C50 C 0.9635(14) 0.3363(13) 0.1622(7) 0.029(4) Uani 1 1 d . . . C51 C 0.9654(17) 0.4051(14) 0.1280(8) 0.040(5) Uani 1 1 d . . . H51 H 0.9214 0.452 0.1331 0.048 Uiso 1 1 calc R . . C52 C 1.0319(19) 0.4050(16) 0.0862(8) 0.048(6) Uani 1 1 d . . . H52 H 1.0334 0.4524 0.063 0.058 Uiso 1 1 calc R . . C53 C 1.0956(18) 0.3371(17) 0.0780(8) 0.046(6) Uani 1 1 d . . . H53 H 1.1406 0.338 0.0494 0.056 Uiso 1 1 calc R . . C54 C 1.0945(16) 0.2667(16) 0.1117(8) 0.040(5) Uani 1 1 d . . . H54 H 1.1394 0.2205 0.1062 0.048 Uiso 1 1 calc R . . C55 C 1.0652(14) 0.1185(14) 0.1874(8) 0.034(5) Uani 1 1 d . E . H55A H 1.0851 0.1048 0.1541 0.04 Uiso 1 1 calc R . . H55B H 1.0244 0.0696 0.2036 0.04 Uiso 1 1 calc R . . C56 C 1.1553(15) 0.1209(15) 0.2098(8) 0.038(5) Uani 1 1 d . . . C60 C 0.8522(15) 0.3950(13) 0.2290(8) 0.033(5) Uani 1 1 d . . . H60A H 0.8001 0.3708 0.2537 0.039 Uiso 1 1 calc R . . H60B H 0.8227 0.4314 0.2059 0.039 Uiso 1 1 calc R . . C61 C 0.9138(16) 0.4560(13) 0.2522(8) 0.037(5) Uani 1 1 d . . . C62 C 0.9834(18) 0.4021(16) 0.2765(9) 0.047(6) Uani 1 1 d . . . H62A H 0.9483 0.3587 0.2995 0.07 Uiso 1 1 calc R . . H62B H 1.0186 0.4411 0.2926 0.07 Uiso 1 1 calc R . . H62C H 1.0281 0.3719 0.2529 0.07 Uiso 1 1 calc R . . C63 C 0.970(2) 0.5229(15) 0.2161(9) 0.050(6) Uani 1 1 d . . . H63A H 0.9261 0.5577 0.2001 0.075 Uiso 1 1 calc R . . H63B H 1.0148 0.4921 0.1928 0.075 Uiso 1 1 calc R . . H63C H 1.0053 0.5617 0.2322 0.075 Uiso 1 1 calc R . . C64 C 0.846(2) 0.5059(16) 0.2880(9) 0.053(7) Uani 1 1 d . . . H64A H 0.8013 0.54 0.272 0.079 Uiso 1 1 calc R . . H64B H 0.8821 0.5457 0.3031 0.079 Uiso 1 1 calc R . . H64C H 0.8104 0.4643 0.312 0.079 Uiso 1 1 calc R . . Na1A Na 0.2707(6) 0.6052(6) 0.3836(3) 0.039(2) Uani 1 1 d . C . O1A O 0.0997(11) 0.5994(12) 0.4035(6) 0.050(4) Uani 1 1 d D . . O2A O 0.2436(15) 0.6990(16) 0.3194(7) 0.075(6) Uani 1 1 d D . . O3A O 0.2704(12) 0.4790(12) 0.3395(7) 0.057(5) Uani 1 1 d D . . O4A O 0.2961(14) 0.5155(11) 0.4503(6) 0.052(4) Uani 1 1 d D . . O5A O 0.2685(13) 0.7279(11) 0.4309(7) 0.059(5) Uani 1 1 d D . . O6A O 0.4402(11) 0.6178(12) 0.3553(6) 0.053(4) Uani 1 1 d D . . C1A C 0.029(2) 0.604(2) 0.3751(11) 0.075(9) Uiso 1 1 d D . . H1A1 H 0.0157 0.5449 0.3658 0.09 Uiso 1 1 calc R . . H1A2 H 0.0497 0.6427 0.3463 0.09 Uiso 1 1 calc R . . C2A C -0.057(2) 0.640(2) 0.4045(11) 0.077(9) Uiso 1 1 d D . . H2A1 H -0.115 0.6087 0.4005 0.093 Uiso 1 1 calc R . . H2A2 H -0.0646 0.7032 0.3957 0.093 Uiso 1 1 calc R . . C3A C -0.042(2) 0.627(2) 0.4544(10) 0.072(8) Uiso 1 1 d D . . H3A1 H -0.0372 0.6835 0.4681 0.086 Uiso 1 1 calc R . . H3A2 H -0.0945 0.5921 0.4742 0.086 Uiso 1 1 calc R . . C4A C 0.0497(18) 0.5775(18) 0.4503(9) 0.055(6) Uiso 1 1 d D . . H4A1 H 0.0866 0.5955 0.4738 0.066 Uiso 1 1 calc R . . H4A2 H 0.038 0.5135 0.4554 0.066 Uiso 1 1 calc R . . C5A C 0.245(4) 0.677(3) 0.2737(16) 0.120(16) Uiso 1 1 d D . . H5A1 H 0.2009 0.6279 0.2732 0.144 Uiso 1 1 calc R . . H5A2 H 0.31 0.6594 0.2586 0.144 Uiso 1 1 calc R . . C6A C 0.214(7) 0.759(5) 0.2488(19) 0.23(4) Uiso 1 1 d D . . H6A1 H 0.2694 0.7885 0.2281 0.279 Uiso 1 1 calc R . . H6A2 H 0.1674 0.745 0.2292 0.279 Uiso 1 1 calc R . . C7A C 0.172(6) 0.815(4) 0.285(2) 0.19(3) Uiso 1 1 d D . . H7A1 H 0.1021 0.8159 0.2872 0.231 Uiso 1 1 calc R . . H7A2 H 0.1958 0.8759 0.2763 0.231 Uiso 1 1 calc R . . C8A C 0.197(3) 0.782(2) 0.3294(13) 0.091(11) Uiso 1 1 d D . . H8A1 H 0.24 0.8236 0.3399 0.109 Uiso 1 1 calc R . . H8A2 H 0.139 0.7741 0.3541 0.109 Uiso 1 1 calc R . . C9A C 0.193(2) 0.419(2) 0.3481(14) 0.088(11) Uiso 1 1 d D . . H9A1 H 0.1359 0.4467 0.3387 0.105 Uiso 1 1 calc R . . H9A2 H 0.1774 0.3992 0.3819 0.105 Uiso 1 1 calc R . . C10A C 0.226(4) 0.343(3) 0.319(2) 0.14(2) Uiso 1 1 d D . . H10D H 0.2159 0.2877 0.3388 0.173 Uiso 1 1 calc R . . H10E H 0.1875 0.3407 0.2937 0.173 Uiso 1 1 calc R . . C11A C 0.318(2) 0.353(2) 0.2994(12) 0.069(8) Uiso 1 1 d D . . H11D H 0.328 0.3456 0.2651 0.082 Uiso 1 1 calc R . . H11E H 0.3565 0.3078 0.3138 0.082 Uiso 1 1 calc R . . C12A C 0.3474(18) 0.4434(17) 0.3084(10) 0.053(6) Uiso 1 1 d D . . H12C H 0.4049 0.4404 0.3229 0.063 Uiso 1 1 calc R . . H12D H 0.3617 0.4804 0.2785 0.063 Uiso 1 1 calc R . . C13A C 0.313(3) 0.4132(19) 0.4534(11) 0.074(9) Uiso 1 1 d D . . H13A H 0.2528 0.3809 0.4546 0.088 Uiso 1 1 calc R . . H13B H 0.3602 0.3953 0.4262 0.088 Uiso 1 1 calc R . . C14A C 0.349(3) 0.398(2) 0.4974(14) 0.088(11) Uiso 1 1 d D . . H14D H 0.3222 0.3425 0.5143 0.105 Uiso 1 1 calc R . . H14E H 0.4187 0.393 0.4907 0.105 Uiso 1 1 calc R . . C15A C 0.320(3) 0.471(2) 0.5264(11) 0.077(9) Uiso 1 1 d D . . H15D H 0.3678 0.4811 0.5463 0.093 Uiso 1 1 calc R . . H15E H 0.2578 0.4592 0.5472 0.093 Uiso 1 1 calc R . . C16A C 0.315(2) 0.5456(18) 0.4930(10) 0.061(7) Uiso 1 1 d D . . H16D H 0.2634 0.5856 0.5064 0.073 Uiso 1 1 calc R . . H16E H 0.3755 0.5784 0.4868 0.073 Uiso 1 1 calc R . . C17A C 0.356(2) 0.770(2) 0.4343(12) 0.070(8) Uiso 1 1 d D C . H17A H 0.3898 0.7904 0.4026 0.084 Uiso 1 1 calc R A 1 H17B H 0.397 0.7277 0.4486 0.084 Uiso 1 1 calc R A 1 C21A C 0.483(2) 0.662(2) 0.3113(12) 0.074(9) Uiso 1 1 d D C . H21A H 0.4585 0.7227 0.3088 0.088 Uiso 1 1 calc R . . H21B H 0.4688 0.6306 0.2846 0.088 Uiso 1 1 calc R . . C22A C 0.586(3) 0.663(3) 0.3105(14) 0.092(11) Uiso 1 1 d D . . H22A H 0.6054 0.7185 0.3212 0.11 Uiso 1 1 calc R C . H22B H 0.6216 0.6547 0.2784 0.11 Uiso 1 1 calc R . . C23A C 0.601(2) 0.587(2) 0.3439(13) 0.082(10) Uiso 1 1 d D C . H23C H 0.611 0.5316 0.3277 0.099 Uiso 1 1 calc R . . H23D H 0.6572 0.597 0.3586 0.099 Uiso 1 1 calc R . . C24A C 0.513(2) 0.584(2) 0.3791(11) 0.069(8) Uiso 1 1 d D C . H24A H 0.4985 0.5232 0.392 0.082 Uiso 1 1 calc R . . H24B H 0.5194 0.6205 0.4053 0.082 Uiso 1 1 calc R . . Na1B Na 0.4009(8) 0.6722(7) 0.0686(4) 0.057(3) Uani 1 1 d . . . O1B O 0.3209(19) 0.8038(17) 0.0727(10) 0.093(8) Uani 1 1 d D . . O2B O 0.4940(17) 0.6924(14) 0.1249(7) 0.072(6) Uani 1 1 d D . . O3B O 0.3326(15) 0.6110(14) 0.0109(7) 0.069(6) Uani 1 1 d D . . O4B O 0.306(2) 0.5752(19) 0.1226(9) 0.110(10) Uani 1 1 d D . . O5B O 0.5337(16) 0.7106(19) 0.0113(7) 0.090(8) Uani 1 1 d D . . C1B C 0.348(3) 0.880(3) 0.0424(16) 0.109(14) Uiso 1 1 d D . . H1B1 H 0.3391 0.8708 0.0099 0.131 Uiso 1 1 calc R . . H1B2 H 0.4147 0.8955 0.0418 0.131 Uiso 1 1 calc R . . C2B C 0.280(3) 0.950(3) 0.0643(17) 0.112(14) Uiso 1 1 d D . . H2B1 H 0.312 0.9873 0.0833 0.135 Uiso 1 1 calc R . . H2B2 H 0.2575 0.9882 0.0394 0.135 Uiso 1 1 calc R . . C3B C 0.202(3) 0.904(4) 0.093(2) 0.138(19) Uiso 1 1 d D . . H3B1 H 0.1773 0.936 0.1216 0.165 Uiso 1 1 calc R . . H3B2 H 0.1501 0.8966 0.0758 0.165 Uiso 1 1 calc R . . C4B C 0.238(4) 0.820(4) 0.107(2) 0.14(2) Uiso 1 1 d D . . H4B1 H 0.1893 0.7743 0.1076 0.171 Uiso 1 1 calc R . . H4B2 H 0.2537 0.8207 0.1387 0.171 Uiso 1 1 calc R . . C5B C 0.491(3) 0.764(3) 0.1534(15) 0.095(12) Uiso 1 1 d D . . H5B1 H 0.4357 0.759 0.1794 0.114 Uiso 1 1 calc R . . H5B2 H 0.4874 0.8197 0.1345 0.114 Uiso 1 1 calc R . . C6B C 0.580(4) 0.759(3) 0.1719(19) 0.131(18) Uiso 1 1 d D . . H6B1 H 0.6257 0.8034 0.1546 0.157 Uiso 1 1 calc R . . H6B2 H 0.5673 0.7709 0.2057 0.157 Uiso 1 1 calc R . . C7B C 0.618(3) 0.673(4) 0.166(2) 0.130(17) Uiso 1 1 d D . . H7B1 H 0.606 0.6377 0.1964 0.156 Uiso 1 1 calc R . . H7B2 H 0.6872 0.676 0.1541 0.156 Uiso 1 1 calc R . . C8B C 0.571(3) 0.634(3) 0.1325(18) 0.115(15) Uiso 1 1 d D . . H8B1 H 0.5464 0.575 0.1451 0.137 Uiso 1 1 calc R . . H8B2 H 0.6165 0.6273 0.1025 0.137 Uiso 1 1 calc R . . C9B C 0.352(3) 0.532(3) -0.014(2) 0.124(16) Uiso 1 1 d D . . H9B1 H 0.4031 0.5422 -0.0417 0.149 Uiso 1 1 calc R . . H9B2 H 0.3722 0.4842 0.0072 0.149 Uiso 1 1 calc R . . C10B C 0.265(3) 0.508(2) -0.0279(14) 0.087(10) Uiso 1 1 d D . . H10F H 0.2368 0.4557 -0.0088 0.105 Uiso 1 1 calc R . . H10G H 0.2776 0.4952 -0.0615 0.105 Uiso 1 1 calc R . . C11B C 0.199(2) 0.582(2) -0.0209(13) 0.077(9) Uiso 1 1 d D . . H11F H 0.1436 0.5664 0.004 0.093 Uiso 1 1 calc R . . H11G H 0.1765 0.6004 -0.0504 0.093 Uiso 1 1 calc R . . C12B C 0.256(3) 0.654(2) -0.0066(14) 0.086(10) Uiso 1 1 d D . . H12E H 0.2801 0.695 -0.0339 0.103 Uiso 1 1 calc R . . H12F H 0.2163 0.6865 0.0182 0.103 Uiso 1 1 calc R . . C13B C 0.236(8) 0.515(8) 0.113(3) 0.28(5) Uiso 1 1 d D . . H13C H 0.2562 0.4895 0.0823 0.338 Uiso 1 1 calc R . . H13D H 0.1733 0.5434 0.1141 0.338 Uiso 1 1 calc R . . C14B C 0.233(4) 0.444(3) 0.1545(17) 0.114(15) Uiso 1 1 d D . . H14F H 0.1703 0.4157 0.1631 0.136 Uiso 1 1 calc R . . H14G H 0.2827 0.3989 0.1465 0.136 Uiso 1 1 calc R . . C15B C 0.252(4) 0.493(4) 0.1908(17) 0.139(19) Uiso 1 1 d D . . H15F H 0.2746 0.4552 0.2156 0.167 Uiso 1 1 calc R . . H15G H 0.1949 0.5255 0.2052 0.167 Uiso 1 1 calc R . . C16B C 0.330(5) 0.556(5) 0.166(3) 0.20(3) Uiso 1 1 d D . . H16F H 0.3299 0.6098 0.1832 0.236 Uiso 1 1 calc R . . H16G H 0.393 0.528 0.1629 0.236 Uiso 1 1 calc R . . C17B C 0.533(3) 0.710(3) -0.0384(13) 0.083(10) Uiso 1 1 d D . . H17C H 0.4808 0.7462 -0.047 0.1 Uiso 1 1 calc R . . H17D H 0.5258 0.6492 -0.0472 0.1 Uiso 1 1 calc R . . C18B C 0.626(3) 0.746(2) -0.0624(11) 0.080(9) Uiso 1 1 d D . . H18A H 0.6721 0.6986 -0.0712 0.097 Uiso 1 1 calc R . . H18B H 0.6192 0.7826 -0.0912 0.097 Uiso 1 1 calc R . . C19B C 0.656(3) 0.799(3) -0.0277(14) 0.094(11) Uiso 1 1 d D . . H19A H 0.7266 0.8012 -0.0323 0.113 Uiso 1 1 calc R . . H19B H 0.6321 0.8601 -0.0305 0.113 Uiso 1 1 calc R . . C20B C 0.616(3) 0.756(3) 0.0182(13) 0.092(11) Uiso 1 1 d D . . H20A H 0.6624 0.7148 0.0291 0.11 Uiso 1 1 calc R . . H20B H 0.5984 0.8001 0.042 0.11 Uiso 1 1 calc R . . O1E O 0.8185(19) 0.6889(19) 0.0644(10) 0.098(8) Uiso 1 1 d D . . C1E C 0.863(3) 0.770(2) 0.0530(15) 0.092(11) Uiso 1 1 d D D . H1E1 H 0.8282 0.8148 0.0728 0.11 Uiso 1 1 calc R . . H1E2 H 0.8627 0.7889 0.0196 0.11 Uiso 1 1 calc R . . C2E C 0.960(3) 0.763(3) 0.0607(19) 0.119(15) Uiso 1 1 d D . . H2E1 H 0.9727 0.808 0.0818 0.143 Uiso 1 1 calc R B 1 H2E2 H 1.0053 0.771 0.0305 0.143 Uiso 1 1 calc R B 1 O1F O 0.213(5) 1.196(4) 0.445(3) 0.26(3) Uiso 1 1 d D . . C1F C 0.259(7) 1.143(6) 0.404(3) 0.21(3) Uiso 1 1 d D . . H1F1 H 0.2105 1.1144 0.3897 0.251 Uiso 1 1 calc R . . H1F2 H 0.2999 1.1807 0.379 0.251 Uiso 1 1 calc R . . C2F C 0.314(6) 1.080(5) 0.425(3) 0.19(3) Uiso 1 1 d D . . H2F1 H 0.377 1.0745 0.4046 0.225 Uiso 1 1 calc R . . H2F2 H 0.2819 1.0225 0.4287 0.225 Uiso 1 1 calc R . . C3F C 0.325(6) 1.106(6) 0.470(3) 0.21(4) Uiso 1 1 d D . . H3F1 H 0.3032 1.0594 0.495 0.257 Uiso 1 1 calc R . . H3F2 H 0.3933 1.1182 0.4703 0.257 Uiso 1 1 calc R . . C4F C 0.271(10) 1.183(8) 0.479(3) 0.30(6) Uiso 1 1 d D . . H4F1 H 0.2311 1.1771 0.511 0.362 Uiso 1 1 calc R . . H4F2 H 0.3135 1.2342 0.4775 0.362 Uiso 1 1 calc R . . C18A C 0.333(3) 0.843(2) 0.4632(14) 0.084(10) Uiso 0.49(10) 1 d PD C 1 H18C H 0.3741 0.8941 0.4503 0.1 Uiso 0.49(10) 1 calc PR C 1 H18D H 0.3413 0.8273 0.496 0.1 Uiso 0.49(10) 1 calc PR C 1 C19A C 0.226(4) 0.862(4) 0.460(3) 0.07(2) Uiso 0.49(10) 1 d PD C 1 H19C H 0.193 0.8911 0.4882 0.087 Uiso 0.49(10) 1 calc PR C 1 H19D H 0.22 0.8977 0.4313 0.087 Uiso 0.49(10) 1 calc PR C 1 C20A C 0.191(2) 0.772(2) 0.4598(14) 0.083(10) Uiso 0.49(10) 1 d PD C 1 H20C H 0.1771 0.7435 0.492 0.099 Uiso 0.49(10) 1 calc PR C 1 H20D H 0.1333 0.7721 0.4459 0.099 Uiso 0.49(10) 1 calc PR C 1 C3E C 0.966(3) 0.671(4) 0.084(2) 0.130(18) Uiso 0.54(11) 1 d PD D 1 H3E1 H 1.0301 0.6459 0.0741 0.156 Uiso 0.54(11) 1 calc PR D 1 H3E2 H 0.951 0.6711 0.1184 0.156 Uiso 0.54(11) 1 calc PR D 1 C4E C 0.900(5) 0.624(3) 0.068(3) 0.09(3) Uiso 0.54(11) 1 d PD D 1 H4E1 H 0.8779 0.5729 0.0901 0.105 Uiso 0.54(11) 1 calc PR D 1 H4E2 H 0.9266 0.6021 0.0366 0.105 Uiso 0.54(11) 1 calc PR D 1 C57 C 1.137(3) 0.181(3) 0.2519(14) 0.050(10) Uani 0.72(5) 1 d P E 1 H57A H 1.0809 0.1598 0.2748 0.075 Uiso 0.72(5) 1 calc PR E 1 H57B H 1.1248 0.2413 0.2402 0.075 Uiso 0.72(5) 1 calc PR E 1 H57C H 1.1922 0.1805 0.2671 0.075 Uiso 0.72(5) 1 calc PR E 1 C58 C 1.239(2) 0.151(3) 0.1760(16) 0.058(12) Uani 0.72(5) 1 d P E 1 H58A H 1.2504 0.1127 0.1498 0.087 Uiso 0.72(5) 1 calc PR E 1 H58B H 1.2942 0.1497 0.1916 0.087 Uiso 0.72(5) 1 calc PR E 1 H58C H 1.2285 0.2112 0.164 0.087 Uiso 0.72(5) 1 calc PR E 1 C59 C 1.168(3) 0.025(2) 0.2303(16) 0.056(12) Uani 0.72(5) 1 d P E 1 H59A H 1.1106 0.0072 0.2531 0.084 Uiso 0.72(5) 1 calc PR E 1 H59B H 1.2229 0.0223 0.246 0.084 Uiso 0.72(5) 1 calc PR E 1 H59C H 1.1779 -0.0147 0.2047 0.084 Uiso 0.72(5) 1 calc PR E 1 C18C C 0.333(3) 0.843(2) 0.4632(14) 0.084(10) Uiso 0.51(10) 1 d P C 2 H18E H 0.3383 0.8987 0.4434 0.1 Uiso 0.51(10) 1 calc PR C 2 H18F H 0.3775 0.845 0.4857 0.1 Uiso 0.51(10) 1 calc PR C 2 C19C C 0.237(4) 0.828(4) 0.488(3) 0.06(2) Uiso 0.51(10) 1 d P C 2 H19E H 0.2027 0.8844 0.4917 0.076 Uiso 0.51(10) 1 calc PR C 2 H19F H 0.2369 0.7988 0.5195 0.076 Uiso 0.51(10) 1 calc PR C 2 C20C C 0.191(2) 0.772(2) 0.4598(14) 0.083(10) Uiso 0.51(10) 1 d P C 2 H20E H 0.1486 0.7292 0.4803 0.099 Uiso 0.51(10) 1 calc PR C 2 H20F H 0.154 0.8078 0.4399 0.099 Uiso 0.51(10) 1 calc PR C 2 C3G C 0.966(3) 0.671(4) 0.084(2) 0.130(18) Uiso 0.46(11) 1 d P D 2 H3G1 H 1.0005 0.6312 0.0607 0.156 Uiso 0.46(11) 1 calc PR D 2 H3G2 H 0.9988 0.6714 0.1108 0.156 Uiso 0.46(11) 1 calc PR D 2 C4G C 0.864(6) 0.641(5) 0.100(3) 0.08(3) Uiso 0.46(11) 1 d P D 2 H4G1 H 0.8574 0.5767 0.0989 0.091 Uiso 0.46(11) 1 calc PR D 2 H4G2 H 0.8375 0.6583 0.132 0.091 Uiso 0.46(11) 1 calc PR D 2 C57X C 1.134(5) 0.119(8) 0.259(3) 0.04(2) Uani 0.28(5) 1 d P E 2 H57D H 1.1935 0.1205 0.2714 0.059 Uiso 0.28(5) 1 calc PR E 2 H57E H 1.1 0.0642 0.2715 0.059 Uiso 0.28(5) 1 calc PR E 2 H57F H 1.0947 0.1691 0.2691 0.059 Uiso 0.28(5) 1 calc PR E 2 C58X C 1.221(6) 0.209(8) 0.193(3) 0.05(3) Uani 0.28(5) 1 d P E 2 H58D H 1.237 0.2143 0.1581 0.072 Uiso 0.28(5) 1 calc PR E 2 H58E H 1.2791 0.2042 0.2057 0.072 Uiso 0.28(5) 1 calc PR E 2 H58F H 1.185 0.261 0.2038 0.072 Uiso 0.28(5) 1 calc PR E 2 C59X C 1.224(6) 0.046(7) 0.190(3) 0.05(3) Uani 0.28(5) 1 d P E 2 H59D H 1.2346 0.0518 0.1552 0.08 Uiso 0.28(5) 1 calc PR E 2 H59E H 1.1948 -0.011 0.201 0.08 Uiso 0.28(5) 1 calc PR E 2 H59F H 1.2844 0.0509 0.2003 0.08 Uiso 0.28(5) 1 calc PR E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.026(3) 0.022(3) 0.019(3) 0.0001(19) -0.005(2) 0.000(2) Si2 0.024(3) 0.022(3) 0.022(3) 0.0017(19) -0.005(2) -0.0023(19) Si3 0.022(3) 0.023(3) 0.019(2) -0.0005(19) -0.0031(19) -0.0002(19) Si4 0.024(3) 0.021(2) 0.021(3) 0.0011(19) -0.002(2) -0.0009(19) N1 0.032(9) 0.031(9) 0.024(8) -0.006(7) -0.007(7) 0.002(7) N2 0.027(8) 0.033(9) 0.025(8) -0.003(7) -0.008(7) 0.005(7) N3 0.033(9) 0.023(8) 0.029(9) 0.003(7) -0.005(7) 0.000(7) N4 0.026(8) 0.029(9) 0.029(9) 0.004(7) -0.005(7) -0.004(7) N5 0.025(8) 0.032(9) 0.025(8) 0.000(7) -0.007(7) 0.001(7) N6 0.028(8) 0.033(9) 0.024(8) -0.006(7) -0.005(7) 0.002(7) N7 0.025(8) 0.028(8) 0.029(9) 0.004(7) -0.001(7) 0.002(7) N8 0.032(9) 0.023(8) 0.027(9) 0.003(6) 0.001(7) -0.002(7) C1 0.039(12) 0.036(11) 0.028(11) -0.002(9) -0.009(9) -0.004(9) C2 0.033(11) 0.037(11) 0.030(11) -0.002(9) -0.010(9) -0.001(9) C3 0.040(13) 0.054(14) 0.044(13) -0.003(11) -0.019(11) 0.002(11) C4 0.046(15) 0.072(18) 0.063(17) -0.008(14) -0.029(13) -0.010(13) C5 0.061(17) 0.066(18) 0.062(17) -0.020(14) -0.029(14) -0.013(14) C6 0.048(14) 0.049(14) 0.042(13) -0.014(11) -0.012(11) -0.005(11) C7 0.041(12) 0.030(11) 0.031(11) -0.008(8) -0.011(9) 0.009(9) C8 0.041(12) 0.046(13) 0.027(11) -0.011(9) -0.004(9) 0.004(10) C9 0.056(15) 0.043(13) 0.029(11) 0.002(9) -0.001(10) 0.001(11) C10 0.061(16) 0.066(17) 0.029(12) -0.011(11) -0.009(11) -0.003(13) C11 0.048(14) 0.066(17) 0.041(14) -0.013(12) 0.002(11) 0.008(12) C12 0.032(11) 0.038(11) 0.028(10) 0.001(8) -0.005(8) 0.007(9) C13 0.039(12) 0.040(12) 0.038(12) 0.000(9) -0.012(10) 0.011(9) C14 0.062(17) 0.042(14) 0.058(16) -0.008(12) -0.002(13) 0.020(12) C15 0.065(16) 0.038(13) 0.038(13) 0.002(10) -0.005(12) 0.006(11) C16 0.08(2) 0.059(17) 0.08(2) 0.014(15) -0.045(17) 0.009(15) C17 0.037(11) 0.028(10) 0.027(10) 0.003(8) -0.006(9) -0.005(8) C18 0.033(11) 0.030(10) 0.031(11) 0.005(8) -0.009(9) -0.009(8) C19 0.040(12) 0.046(13) 0.037(12) 0.011(10) -0.003(10) -0.007(10) C20 0.052(15) 0.060(16) 0.038(13) 0.022(12) -0.005(11) -0.017(12) C21 0.065(17) 0.043(14) 0.048(15) 0.022(11) -0.014(13) -0.007(12) C22 0.045(13) 0.033(11) 0.045(13) 0.009(10) -0.012(11) -0.002(10) C23 0.038(11) 0.025(10) 0.037(12) 0.001(8) -0.004(9) 0.003(8) C24 0.064(16) 0.025(11) 0.044(13) -0.004(9) -0.004(12) 0.008(10) C25 0.08(2) 0.045(15) 0.047(15) -0.010(12) -0.014(14) -0.004(13) C26 0.07(2) 0.067(19) 0.058(18) -0.019(15) 0.000(15) 0.023(16) C27 0.15(4) 0.026(13) 0.07(2) -0.011(13) -0.02(2) 0.006(17) C28 0.025(10) 0.037(11) 0.040(12) 0.004(9) -0.004(9) -0.003(8) C29 0.039(13) 0.069(17) 0.051(15) 0.017(13) -0.019(11) -0.023(12) C30 0.072(19) 0.08(2) 0.053(17) 0.000(15) -0.030(15) -0.032(16) C31 0.042(16) 0.11(3) 0.10(3) 0.03(2) -0.036(17) -0.010(17) C32 0.058(18) 0.09(2) 0.07(2) 0.024(17) -0.024(15) -0.046(17) C33 0.031(10) 0.038(11) 0.022(10) -0.001(8) -0.004(8) -0.007(9) C34 0.032(10) 0.032(10) 0.022(10) -0.002(8) -0.001(8) -0.007(8) C35 0.044(12) 0.035(11) 0.033(11) -0.007(9) -0.003(9) -0.007(9) C36 0.053(15) 0.044(13) 0.036(12) -0.012(10) -0.004(11) -0.020(11) C37 0.045(14) 0.065(16) 0.042(14) -0.010(12) -0.014(11) -0.019(12) C38 0.034(11) 0.053(14) 0.033(12) -0.003(10) -0.010(9) -0.009(10) C39 0.030(11) 0.044(12) 0.034(11) -0.006(9) -0.011(9) 0.009(9) C40 0.052(14) 0.042(13) 0.039(13) 0.003(10) -0.023(11) 0.006(10) C41 0.055(15) 0.055(15) 0.045(14) 0.014(11) -0.016(12) -0.010(12) C42 0.072(19) 0.072(19) 0.045(15) 0.012(13) -0.035(14) -0.007(15) C43 0.09(2) 0.051(16) 0.07(2) 0.004(14) -0.034(18) 0.022(15) C44 0.035(11) 0.033(11) 0.030(11) -0.005(8) -0.006(9) 0.007(9) C45 0.031(11) 0.041(12) 0.034(11) -0.008(9) -0.002(9) 0.007(9) C46 0.033(12) 0.055(15) 0.061(16) -0.009(12) -0.007(11) 0.013(11) C47 0.049(14) 0.057(16) 0.041(14) -0.018(12) 0.008(11) 0.004(12) C48 0.035(12) 0.047(13) 0.038(12) -0.003(10) 0.000(10) -0.001(10) C49 0.026(10) 0.034(11) 0.029(10) 0.001(8) -0.003(8) -0.006(8) C50 0.030(10) 0.030(10) 0.025(10) 0.002(8) -0.003(8) -0.008(8) C51 0.049(13) 0.031(11) 0.037(12) 0.006(9) -0.007(10) -0.005(10) C52 0.065(16) 0.046(14) 0.029(12) 0.013(10) -0.003(11) -0.013(12) C53 0.047(14) 0.058(15) 0.028(12) 0.005(10) 0.009(10) -0.013(12) C54 0.037(12) 0.048(13) 0.031(12) 0.000(10) 0.002(9) -0.007(10) C55 0.030(11) 0.034(11) 0.038(12) -0.007(9) -0.007(9) 0.006(8) C56 0.030(11) 0.041(12) 0.045(13) -0.005(10) -0.011(10) 0.006(9) C60 0.035(11) 0.022(10) 0.038(12) 0.002(8) -0.001(9) 0.005(8) C61 0.041(12) 0.024(10) 0.043(12) -0.004(9) 0.000(10) -0.003(9) C62 0.053(15) 0.040(13) 0.051(15) -0.007(11) -0.016(12) -0.007(11) C63 0.068(17) 0.028(12) 0.049(15) 0.000(10) 0.004(12) -0.014(11) C64 0.074(18) 0.032(12) 0.047(14) -0.005(10) 0.007(13) -0.001(12) Na1A 0.036(5) 0.043(5) 0.037(5) -0.003(4) -0.006(4) 0.002(4) O1A 0.034(9) 0.071(12) 0.043(10) -0.002(8) -0.006(7) -0.007(8) O2A 0.069(13) 0.094(16) 0.055(12) 0.022(11) -0.004(10) 0.024(12) O3A 0.042(10) 0.068(12) 0.060(11) -0.025(9) -0.001(8) 0.001(8) O4A 0.077(12) 0.041(9) 0.041(9) -0.007(7) -0.020(9) 0.007(8) O5A 0.054(11) 0.046(10) 0.077(13) -0.019(9) -0.004(10) -0.002(8) O6A 0.037(9) 0.062(11) 0.056(11) 0.006(9) -0.003(8) -0.001(8) Na1B 0.059(6) 0.067(7) 0.044(6) 0.011(5) -0.012(5) -0.017(5) O1B 0.090(18) 0.087(17) 0.098(19) 0.012(14) -0.012(15) 0.012(14) O2B 0.103(17) 0.061(12) 0.063(13) -0.004(10) -0.040(12) -0.014(11) O3B 0.073(13) 0.075(14) 0.063(13) 0.000(10) -0.026(11) -0.012(11) O4B 0.13(2) 0.12(2) 0.079(17) 0.035(15) -0.029(16) -0.077(19) O5B 0.076(15) 0.15(2) 0.040(11) 0.015(13) -0.011(10) -0.057(15) C57 0.04(2) 0.05(3) 0.06(2) -0.001(19) -0.019(17) -0.003(18) C58 0.028(18) 0.08(3) 0.07(3) 0.00(2) -0.004(17) -0.002(18) C59 0.04(2) 0.05(2) 0.09(3) 0.004(19) -0.03(2) 0.009(15) C57X 0.02(4) 0.07(7) 0.03(4) -0.01(4) -0.01(3) 0.01(4) C58X 0.04(5) 0.06(7) 0.04(5) 0.01(5) -0.01(4) -0.01(4) C59X 0.04(5) 0.08(7) 0.05(6) -0.04(5) -0.03(4) 0.03(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 N1 1.822(16) . ? Si1 N2 1.838(16) . ? Si1 Si4 2.311(7) . ? Si1 Si2 2.313(7) . ? Si2 N4 1.816(16) . ? Si2 N3 1.832(16) . ? Si2 Si3 2.316(7) . ? Si3 N5 1.821(16) . ? Si3 N6 1.830(16) . ? Si3 Si4 2.315(7) . ? Si4 N8 1.813(16) . ? Si4 N7 1.837(16) . ? N1 C1 1.39(3) . ? N1 C7 1.45(3) . ? N2 C2 1.38(3) . ? N2 C12 1.45(3) . ? N3 C17 1.39(3) . ? N3 C23 1.44(3) . ? N4 C18 1.40(3) . ? N4 C28 1.45(3) . ? N5 C33 1.39(3) . ? N5 C39 1.45(3) . ? N6 C34 1.38(3) . ? N6 C44 1.45(3) . ? N7 C49 1.39(3) . ? N7 C55 1.44(3) . ? N8 C50 1.39(3) . ? N8 C60 1.45(3) . ? C1 C6 1.38(3) . ? C1 C2 1.43(3) . ? C2 C3 1.40(3) . ? C3 C4 1.40(4) . ? C4 C5 1.36(4) . ? C5 C6 1.41(4) . ? C7 C8 1.56(3) . ? C8 C11 1.51(3) . ? C8 C9 1.52(3) . ? C8 C10 1.53(3) . ? C12 C13 1.56(3) . ? C13 C16 1.51(3) . ? C13 C15 1.52(3) . ? C13 C14 1.53(3) . ? C17 C22 1.39(3) . ? C17 C18 1.42(3) . ? C18 C19 1.39(3) . ? C19 C20 1.40(3) . ? C20 C21 1.37(4) . ? C21 C22 1.40(3) . ? C23 C24 1.56(3) . ? C24 C26 1.52(4) . ? C24 C25 1.53(4) . ? C24 C27 1.53(4) . ? C28 C29 1.55(3) . ? C29 C31 1.52(4) . ? C29 C32 1.53(4) . ? C29 C30 1.54(4) . ? C33 C38 1.39(3) . ? C33 C34 1.42(3) . ? C34 C35 1.40(3) . ? C35 C36 1.39(3) . ? C36 C37 1.38(4) . ? C37 C38 1.40(3) . ? C39 C40 1.57(3) . ? C40 C41 1.52(4) . ? C40 C43 1.53(4) . ? C40 C42 1.53(3) . ? C44 C45 1.56(3) . ? C45 C48 1.53(3) . ? C45 C46 1.53(3) . ? C45 C47 1.54(3) . ? C49 C54 1.40(3) . ? C49 C50 1.42(3) . ? C50 C51 1.39(3) . ? C51 C52 1.39(3) . ? C52 C53 1.38(4) . ? C53 C54 1.40(3) . ? C55 C56 1.55(3) . ? C56 C57X 1.40(8) . ? C56 C58 1.46(4) . ? C56 C57 1.56(5) . ? C56 C59 1.56(4) . ? C56 C59X 1.57(8) . ? C56 C58X 1.64(10) . ? C60 C61 1.56(3) . ? C61 C64 1.52(3) . ? C61 C62 1.53(3) . ? C61 C63 1.53(3) . ? Na1A O2A 2.36(2) . ? Na1A O4A 2.371(18) . ? Na1A O3A 2.388(19) . ? Na1A O5A 2.395(19) . ? Na1A O1A 2.411(17) . ? Na1A O6A 2.418(18) . ? O1A C1A 1.42(3) . ? O1A C4A 1.43(3) . ? O2A C5A 1.39(4) . ? O2A C8A 1.46(4) . ? O3A C12A 1.42(3) . ? O3A C9A 1.42(4) . ? O4A C16A 1.42(3) . ? O4A C13A 1.58(3) . ? O5A C17A 1.43(4) . ? O5A C20A 1.45(4) . ? O6A C24A 1.43(3) . ? O6A C21A 1.43(4) . ? C1A C2A 1.49(4) . ? C2A C3A 1.50(4) . ? C3A C4A 1.49(4) . ? C5A C6A 1.51(6) . ? C6A C7A 1.43(6) . ? C7A C8A 1.46(6) . ? C9A C10A 1.50(5) . ? C10A C11A 1.35(6) . ? C11A C12A 1.51(4) . ? C13A C14A 1.46(5) . ? C14A C15A 1.45(5) . ? C15A C16A 1.46(4) . ? C17A C18A 1.44(5) . ? C21A C22A 1.47(5) . ? C22A C23A 1.50(5) . ? C23A C24A 1.47(4) . ? Na1B O1B 2.30(3) . ? Na1B O4B 2.33(2) . ? Na1B O5B 2.33(2) . ? Na1B O2B 2.33(2) . ? Na1B O3B 2.34(2) . ? O1B C1B 1.42(5) . ? O1B C4B 1.43(6) . ? O2B C5B 1.41(4) . ? O2B C8B 1.45(5) . ? O3B C12B 1.43(4) . ? O3B C9B 1.45(5) . ? O4B C16B 1.37(7) . ? O4B C13B 1.45(9) . ? O5B C20B 1.43(4) . ? O5B C17B 1.44(4) . ? C1B C2B 1.53(6) . ? C2B C3B 1.43(6) . ? C3B C4B 1.42(7) . ? C5B C6B 1.47(6) . ? C6B C7B 1.43(6) . ? C7B C8B 1.44(6) . ? C9B C10B 1.44(6) . ? C10B C11B 1.46(5) . ? C11B C12B 1.50(5) . ? C13B C14B 1.55(9) . ? C14B C15B 1.40(6) . ? C15B C16B 1.52(8) . ? C17B C18B 1.47(5) . ? C18B C19B 1.47(5) . ? C19B C20B 1.46(5) . ? O1E C1E 1.40(4) . ? O1E C4G 1.46(8) . ? O1E C4E 1.54(7) . ? C1E C2E 1.44(5) . ? C2E C3E 1.53(6) . ? O1F C4F 1.41(10) . ? O1F C1F 1.53(8) . ? C1F C2F 1.41(8) . ? C2F C3F 1.44(8) . ? C3F C4F 1.41(10) . ? C18A C19A 1.57(7) . ? C19A C20A 1.47(7) . ? C3E C4E 1.35(8) . ? 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 Si1 N2 84.4(7) . . ? N1 Si1 Si4 121.4(6) . . ? N2 Si1 Si4 128.3(6) . . ? N1 Si1 Si2 118.5(6) . . ? N2 Si1 Si2 121.0(6) . . ? Si4 Si1 Si2 87.3(2) . . ? N4 Si2 N3 84.8(7) . . ? N4 Si2 Si1 120.3(6) . . ? N3 Si2 Si1 129.2(6) . . ? N4 Si2 Si3 118.4(6) . . ? N3 Si2 Si3 120.7(6) . . ? Si1 Si2 Si3 87.4(2) . . ? N5 Si3 N6 84.7(7) . . ? N5 Si3 Si4 119.5(6) . . ? N6 Si3 Si4 120.2(6) . . ? N5 Si3 Si2 120.9(6) . . ? N6 Si3 Si2 128.6(6) . . ? Si4 Si3 Si2 87.2(2) . . ? N8 Si4 N7 84.4(7) . . ? N8 Si4 Si1 117.7(6) . . ? N7 Si4 Si1 120.5(6) . . ? N8 Si4 Si3 119.9(6) . . ? N7 Si4 Si3 130.6(6) . . ? Si1 Si4 Si3 87.4(2) . . ? C1 N1 C7 121.1(16) . . ? C1 N1 Si1 112.5(13) . . ? C7 N1 Si1 126.5(13) . . ? C2 N2 C12 122.6(17) . . ? C2 N2 Si1 112.7(13) . . ? C12 N2 Si1 123.5(13) . . ? C17 N3 C23 122.0(16) . . ? C17 N3 Si2 112.9(13) . . ? C23 N3 Si2 124.1(13) . . ? C18 N4 C28 121.1(16) . . ? C18 N4 Si2 112.2(13) . . ? C28 N4 Si2 126.6(13) . . ? C33 N5 C39 121.4(16) . . ? C33 N5 Si3 112.2(13) . . ? C39 N5 Si3 126.4(13) . . ? C34 N6 C44 122.3(16) . . ? C34 N6 Si3 113.1(13) . . ? C44 N6 Si3 124.2(13) . . ? C49 N7 C55 121.5(17) . . ? C49 N7 Si4 111.8(13) . . ? C55 N7 Si4 124.5(13) . . ? C50 N8 C60 121.2(16) . . ? C50 N8 Si4 112.2(13) . . ? C60 N8 Si4 126.6(13) . . ? C6 C1 N1 129(2) . . ? C6 C1 C2 119(2) . . ? N1 C1 C2 112.0(17) . . ? N2 C2 C3 129(2) . . ? N2 C2 C1 111.6(17) . . ? C3 C2 C1 119(2) . . ? C4 C3 C2 120(2) . . ? C5 C4 C3 121(2) . . ? C4 C5 C6 120(2) . . ? C1 C6 C5 120(2) . . ? N1 C7 C8 116.6(17) . . ? C11 C8 C9 111(2) . . ? C11 C8 C10 107.3(19) . . ? C9 C8 C10 109(2) . . ? C11 C8 C7 105.7(19) . . ? C9 C8 C7 110.9(17) . . ? C10 C8 C7 113.2(19) . . ? N2 C12 C13 117.1(17) . . ? C16 C13 C15 112(2) . . ? C16 C13 C14 106(2) . . ? C15 C13 C14 110(2) . . ? C16 C13 C12 112(2) . . ? C15 C13 C12 110.0(18) . . ? C14 C13 C12 106.2(19) . . ? N3 C17 C22 129(2) . . ? N3 C17 C18 111.6(17) . . ? C22 C17 C18 119.3(19) . . ? C19 C18 N4 128(2) . . ? C19 C18 C17 119.7(19) . . ? N4 C18 C17 112.1(17) . . ? C18 C19 C20 119(2) . . ? C21 C20 C19 121(2) . . ? C20 C21 C22 121(2) . . ? C17 C22 C21 120(2) . . ? N3 C23 C24 116.9(18) . . ? C26 C24 C25 110(2) . . ? C26 C24 C27 111(2) . . ? C25 C24 C27 107(2) . . ? C26 C24 C23 107(2) . . ? C25 C24 C23 109.7(19) . . ? C27 C24 C23 112(2) . . ? N4 C28 C29 117.1(19) . . ? C31 C29 C32 107(2) . . ? C31 C29 C30 111(3) . . ? C32 C29 C30 108(3) . . ? C31 C29 C28 107(2) . . ? C32 C29 C28 113(2) . . ? C30 C29 C28 111(2) . . ? N5 C33 C38 128(2) . . ? N5 C33 C34 112.5(17) . . ? C38 C33 C34 119.8(19) . . ? N6 C34 C35 129(2) . . ? N6 C34 C33 111.8(17) . . ? C35 C34 C33 119.4(19) . . ? C36 C35 C34 120(2) . . ? C37 C36 C35 121(2) . . ? C36 C37 C38 120(2) . . ? C33 C38 C37 120(2) . . ? N5 C39 C40 116.6(18) . . ? C41 C40 C43 110(2) . . ? C41 C40 C42 109(2) . . ? C43 C40 C42 107(2) . . ? C41 C40 C39 110.7(18) . . ? C43 C40 C39 106(2) . . ? C42 C40 C39 113(2) . . ? N6 C44 C45 116.9(17) . . ? C48 C45 C46 111.0(19) . . ? C48 C45 C47 108.4(19) . . ? C46 C45 C47 108.6(19) . . ? C48 C45 C44 109.9(17) . . ? C46 C45 C44 106.2(18) . . ? C47 C45 C44 112.7(19) . . ? N7 C49 C54 129(2) . . ? N7 C49 C50 112.0(17) . . ? C54 C49 C50 119.4(19) . . ? C51 C50 N8 129(2) . . ? C51 C50 C49 119.6(19) . . ? N8 C50 C49 111.4(17) . . ? C50 C51 C52 120(2) . . ? C53 C52 C51 121(2) . . ? C52 C53 C54 120(2) . . ? C49 C54 C53 120(2) . . ? N7 C55 C56 116.5(17) . . ? C57X C56 C55 113(3) . . ? C58 C56 C55 113(2) . . ? C58 C56 C57 110(3) . . ? C55 C56 C57 109(2) . . ? C58 C56 C59 112(3) . . ? C55 C56 C59 105(2) . . ? C57 C56 C59 108(3) . . ? C57X C56 C59X 114(6) . . ? C55 C56 C59X 108(3) . . ? C57X C56 C58X 106(6) . . ? C55 C56 C58X 113(4) . . ? C59X C56 C58X 102(6) . . ? N8 C60 C61 116.5(17) . . ? C64 C61 C62 110(2) . . ? C64 C61 C63 108.2(18) . . ? C62 C61 C63 109(2) . . ? C64 C61 C60 107.1(19) . . ? C62 C61 C60 110.6(17) . . ? C63 C61 C60 112.0(19) . . ? O2A Na1A O4A 177.6(8) . . ? O2A Na1A O3A 91.7(8) . . ? O4A Na1A O3A 90.7(7) . . ? O2A Na1A O5A 90.5(9) . . ? O4A Na1A O5A 87.2(7) . . ? O3A Na1A O5A 177.5(8) . . ? O2A Na1A O1A 84.1(7) . . ? O4A Na1A O1A 95.3(7) . . ? O3A Na1A O1A 89.8(7) . . ? O5A Na1A O1A 89.2(7) . . ? O2A Na1A O6A 89.8(7) . . ? O4A Na1A O6A 90.8(7) . . ? O3A Na1A O6A 88.9(7) . . ? O5A Na1A O6A 92.4(7) . . ? O1A Na1A O6A 173.8(7) . . ? C1A O1A C4A 105.2(19) . . ? C1A O1A Na1A 131.8(16) . . ? C4A O1A Na1A 122.6(14) . . ? C5A O2A C8A 113(2) . . ? C5A O2A Na1A 127(2) . . ? C8A O2A Na1A 118.0(19) . . ? C12A O3A C9A 109(2) . . ? C12A O3A Na1A 127.8(15) . . ? C9A O3A Na1A 121.9(17) . . ? C16A O4A C13A 106.1(19) . . ? C16A O4A Na1A 126.0(15) . . ? C13A O4A Na1A 127.2(14) . . ? C17A O5A C20A 108(2) . . ? C17A O5A Na1A 120.1(16) . . ? C20A O5A Na1A 131.8(17) . . ? C24A O6A C21A 109(2) . . ? C24A O6A Na1A 126.5(16) . . ? C21A O6A Na1A 124.4(16) . . ? O1A C1A C2A 106(2) . . ? C1A C2A C3A 105(2) . . ? C4A C3A C2A 104(2) . . ? O1A C4A C3A 105(2) . . ? O2A C5A C6A 105(3) . . ? C7A C6A C5A 107(4) . . ? C6A C7A C8A 109(4) . . ? O2A C8A C7A 104(3) . . ? O3A C9A C10A 106(3) . . ? C11A C10A C9A 110(3) . . ? C10A C11A C12A 107(3) . . ? O3A C12A C11A 107(2) . . ? C14A C13A O4A 103(2) . . ? C15A C14A C13A 109(3) . . ? C14A C15A C16A 105(3) . . ? O4A C16A C15A 109(2) . . ? O5A C17A C18A 108(2) . . ? O6A C21A C22A 106(2) . . ? C21A C22A C23A 104(3) . . ? C24A C23A C22A 103(3) . . ? O6A C24A C23A 107(2) . . ? O1B Na1B O4B 105.3(12) . . ? O1B Na1B O5B 100.6(11) . . ? O4B Na1B O5B 154.1(13) . . ? O1B Na1B O2B 98.2(10) . . ? O4B Na1B O2B 88.9(10) . . ? O5B Na1B O2B 87.6(9) . . ? O1B Na1B O3B 99.4(10) . . ? O4B Na1B O3B 86.4(9) . . ? O5B Na1B O3B 89.2(8) . . ? O2B Na1B O3B 162.4(10) . . ? C1B O1B C4B 111(3) . . ? C1B O1B Na1B 125(2) . . ? C4B O1B Na1B 124(3) . . ? C5B O2B C8B 110(3) . . ? C5B O2B Na1B 127(2) . . ? C8B O2B Na1B 123(2) . . ? C12B O3B C9B 106(3) . . ? C12B O3B Na1B 120.8(19) . . ? C9B O3B Na1B 133(2) . . ? C16B O4B C13B 112(4) . . ? C16B O4B Na1B 119(3) . . ? C13B O4B Na1B 127(4) . . ? C20B O5B C17B 110(2) . . ? C20B O5B Na1B 126.4(19) . . ? C17B O5B Na1B 122.5(18) . . ? O1B C1B C2B 103(3) . . ? C3B C2B C1B 106(3) . . ? C4B C3B C2B 107(4) . . ? C3B C4B O1B 107(4) . . ? O2B C5B C6B 106(3) . . ? C7B C6B C5B 107(3) . . ? C6B C7B C8B 108(3) . . ? C7B C8B O2B 106(3) . . ? C10B C9B O3B 107(3) . . ? C9B C10B C11B 108(3) . . ? C10B C11B C12B 105(3) . . ? O3B C12B C11B 106(3) . . ? O4B C13B C14B 101(4) . . ? C15B C14B C13B 103(4) . . ? C14B C15B C16B 103(4) . . ? O4B C16B C15B 104(4) . . ? O5B C17B C18B 106(3) . . ? C19B C18B C17B 105(3) . . ? C20B C19B C18B 105(3) . . ? O5B C20B C19B 106(3) . . ? C1E O1E C4G 109(4) . . ? C1E O1E C4E 105(3) . . ? O1E C1E C2E 109(3) . . ? C1E C2E C3E 104(3) . . ? C4F O1F C1F 106(5) . . ? C2F C1F O1F 103(4) . . ? C1F C2F C3F 110(4) . . ? C4F C3F C2F 107(5) . . ? O1F C4F C3F 109(5) . . ? C17A C18A C19A 103(3) . . ? C20A C19A C18A 100(4) . . ? O5A C20A C19A 104(3) . . ? C4E C3E C2E 105(4) . . ? C3E C4E O1E 104(4) . . ? #===END data_(14)-dec804 _database_code_depnum_ccdc_archive 'CCDC 286732' _audit_creation_date 2004-12-10T15:23:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety ; 'C136 H228 K4 N16 O2 Si8, C72 H124 K2 N8 O2 Si4, 4(C4 H10 O)' ; _chemical_formula_sum 'C224 H392 K6 N24 O8 Si12' _chemical_formula_weight 4121.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 22.8776(7) _cell_length_b 15.9344(6) _cell_length_c 33.8306(11) _cell_angle_alpha 90 _cell_angle_beta 101.086(2) _cell_angle_gamma 90 _cell_volume 12102.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 154669 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4500 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.3562E-3 _diffrn_orient_matrix_ub_12 -0.62755E-1 _diffrn_orient_matrix_ub_13 -0.1395E-3 _diffrn_orient_matrix_ub_21 -0.346739E-1 _diffrn_orient_matrix_ub_22 0.5149E-3 _diffrn_orient_matrix_ub_23 -0.230611E-1 _diffrn_orient_matrix_ub_31 0.279568E-1 _diffrn_orient_matrix_ub_32 -0.1609E-3 _diffrn_orient_matrix_ub_33 -0.193764E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_unetI/netI 0.0994 _diffrn_reflns_number 32607 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 8638 _reflns_number_gt 5263 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Very weak data, non-existent at higher angle. Only K and Si atoms were anisotropic. The Et2O solvate molecules were poorly defined and their H atoms were omitted. 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^)+(0.0511P)^2^+175.3251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8638 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1807 _refine_ls_R_factor_gt 0.1132 _refine_ls_wR_factor_ref 0.2495 _refine_ls_wR_factor_gt 0.2164 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.762 _refine_diff_density_min -0.77 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K -0.04154(10) 0.5 0.41759(7) 0.0406(7) Uani 1 2 d S . . K2 K 0.25160(11) 0.5 0.26550(7) 0.0422(7) Uani 1 2 d S . . Si1 Si 0.03212(12) 0.5 0.32330(8) 0.0276(7) Uani 1 2 d S . . Si2 Si 0.09191(12) 0.5 0.38625(8) 0.0262(7) Uani 1 2 d S . . Si3 Si 0.17758(12) 0.5 0.36001(8) 0.0259(7) Uani 1 2 d S . . Si4 Si 0.11777(12) 0.5 0.29687(8) 0.0250(7) Uani 1 2 d S . . O1 O 0.2788(5) 0.5 0.1934(3) 0.081(3) Uiso 1 2 d S . . N1 N -0.0277(3) 0.5772(4) 0.31532(17) 0.0341(15) Uiso 1 1 d . . . N2 N 0.0796(2) 0.4214(4) 0.42424(16) 0.0271(14) Uiso 1 1 d . . . N3 N 0.2371(2) 0.5779(4) 0.36838(16) 0.0289(14) Uiso 1 1 d . . . N4 N 0.1301(2) 0.5773(4) 0.25896(16) 0.0284(14) Uiso 1 1 d . . . C1 C -0.0786(3) 0.5443(5) 0.3264(2) 0.039(2) Uiso 1 1 d . . . C2 C -0.1251(3) 0.5874(6) 0.3383(2) 0.042(2) Uiso 1 1 d . . . H2 H -0.1254 0.647 0.3384 0.05 Uiso 1 1 calc R . . C3 C -0.1720(4) 0.5420(5) 0.3504(2) 0.051(2) Uiso 1 1 d . . . H3 H -0.2038 0.5715 0.3585 0.061 Uiso 1 1 calc R . . C4 C -0.0236(3) 0.6648(5) 0.3051(2) 0.0354(19) Uiso 1 1 d . . . H4A H 0.0191 0.6791 0.3081 0.042 Uiso 1 1 calc R . . H4B H -0.0397 0.6983 0.3252 0.042 Uiso 1 1 calc R . . C5 C -0.0557(3) 0.6934(5) 0.2625(2) 0.044(2) Uiso 1 1 d . . . C6 C -0.0305(4) 0.7801(6) 0.2547(3) 0.060(3) Uiso 1 1 d . . . H6A H -0.0498 0.8 0.2279 0.09 Uiso 1 1 calc R . . H6B H 0.0125 0.7756 0.2559 0.09 Uiso 1 1 calc R . . H6C H -0.0383 0.8198 0.2752 0.09 Uiso 1 1 calc R . . C7 C -0.0448(4) 0.6298(5) 0.2309(2) 0.048(2) Uiso 1 1 d . . . H7A H -0.0657 0.6479 0.2042 0.072 Uiso 1 1 calc R . . H7B H -0.0596 0.5747 0.2372 0.072 Uiso 1 1 calc R . . H7C H -0.0019 0.6262 0.2311 0.072 Uiso 1 1 calc R . . C8 C -0.1228(4) 0.7029(6) 0.2595(3) 0.061(3) Uiso 1 1 d . . . H8A H -0.1412 0.7197 0.2321 0.091 Uiso 1 1 calc R . . H8B H -0.1306 0.7458 0.2786 0.091 Uiso 1 1 calc R . . H8C H -0.1397 0.6492 0.2659 0.091 Uiso 1 1 calc R . . C10 C 0.0991(3) 0.4551(4) 0.4628(2) 0.0270(17) Uiso 1 1 d . . . C11 C 0.1205(3) 0.4133(5) 0.4983(2) 0.0323(18) Uiso 1 1 d . . . H11 H 0.1209 0.3537 0.4985 0.039 Uiso 1 1 calc R . . C12 C 0.1413(3) 0.4563(5) 0.5340(2) 0.0338(19) Uiso 1 1 d . . . H12 H 0.1555 0.4263 0.5582 0.041 Uiso 1 1 calc R . . C13 C 0.0888(3) 0.6672(4) 0.4166(2) 0.0274(17) Uiso 1 1 d . . . H13A H 0.0924 0.6722 0.388 0.033 Uiso 1 1 calc R . . H13B H 0.128 0.683 0.433 0.033 Uiso 1 1 calc R . . C14 C 0.0431(3) 0.7347(5) 0.4245(2) 0.0349(19) Uiso 1 1 d . . . C15 C 0.0592(4) 0.7732(6) 0.4670(2) 0.052(2) Uiso 1 1 d . . . H15A H 0.0996 0.7965 0.4711 0.077 Uiso 1 1 calc R . . H15B H 0.0574 0.7296 0.4871 0.077 Uiso 1 1 calc R . . H15C H 0.0309 0.818 0.4697 0.077 Uiso 1 1 calc R . . C16 C 0.0464(4) 0.8063(6) 0.3945(3) 0.056(2) Uiso 1 1 d . . . H16A H 0.0872 0.8281 0.3987 0.084 Uiso 1 1 calc R . . H16B H 0.0192 0.8515 0.3988 0.084 Uiso 1 1 calc R . . H16C H 0.035 0.7851 0.3669 0.084 Uiso 1 1 calc R . . C17 C -0.0193(4) 0.6997(6) 0.4185(2) 0.051(2) Uiso 1 1 d . . . H17A H -0.0206 0.6545 0.438 0.077 Uiso 1 1 calc R . . H17B H -0.0308 0.6776 0.3911 0.077 Uiso 1 1 calc R . . H17C H -0.047 0.7443 0.4227 0.077 Uiso 1 1 calc R . . C18 C 0.2881(3) 0.5446(4) 0.3567(2) 0.0276(17) Uiso 1 1 d . . . C19 C 0.3331(3) 0.5882(5) 0.3433(2) 0.0358(19) Uiso 1 1 d . . . H19 H 0.3327 0.6478 0.3425 0.043 Uiso 1 1 calc R . . C20 C 0.3796(4) 0.5427(5) 0.3308(2) 0.045(2) Uiso 1 1 d . . . H20 H 0.4111 0.5722 0.3223 0.053 Uiso 1 1 calc R . . C21 C 0.2331(3) 0.6657(5) 0.3785(2) 0.0363(19) Uiso 1 1 d . . . H21A H 0.1904 0.6801 0.3761 0.044 Uiso 1 1 calc R . . H21B H 0.2486 0.6993 0.3582 0.044 Uiso 1 1 calc R . . C22 C 0.2661(3) 0.6933(5) 0.4208(2) 0.0359(19) Uiso 1 1 d . . . C23 C 0.2423(4) 0.7798(6) 0.4293(3) 0.058(3) Uiso 1 1 d . . . H23A H 0.2623 0.7989 0.456 0.086 Uiso 1 1 calc R . . H23B H 0.1993 0.7761 0.4285 0.086 Uiso 1 1 calc R . . H23C H 0.2499 0.8197 0.4088 0.086 Uiso 1 1 calc R . . C24 C 0.2573(4) 0.6301(6) 0.4529(2) 0.050(2) Uiso 1 1 d . . . H24A H 0.2724 0.5751 0.4466 0.075 Uiso 1 1 calc R . . H24B H 0.2148 0.6255 0.4536 0.075 Uiso 1 1 calc R . . H24C H 0.279 0.6489 0.4793 0.075 Uiso 1 1 calc R . . C25 C 0.3340(4) 0.7037(6) 0.4226(3) 0.057(3) Uiso 1 1 d . . . H25A H 0.3511 0.6498 0.4167 0.086 Uiso 1 1 calc R . . H25B H 0.3531 0.7223 0.4496 0.086 Uiso 1 1 calc R . . H25C H 0.3408 0.7455 0.4027 0.086 Uiso 1 1 calc R . . C26 C 0.1081(3) 0.5445(5) 0.2206(2) 0.0318(18) Uiso 1 1 d . . . C27 C 0.0842(3) 0.5874(6) 0.1857(2) 0.043(2) Uiso 1 1 d . . . H27 H 0.0834 0.647 0.1857 0.052 Uiso 1 1 calc R . . C28 C 0.0610(4) 0.5426(5) 0.1502(3) 0.051(2) Uiso 1 1 d . . . H28 H 0.0454 0.5723 0.1261 0.061 Uiso 1 1 calc R . . C29 C 0.1235(3) 0.6675(5) 0.2664(2) 0.0359(19) Uiso 1 1 d . . . H29A H 0.1207 0.6738 0.2951 0.043 Uiso 1 1 calc R . . H29B H 0.0847 0.6853 0.2503 0.043 Uiso 1 1 calc R . . C30 C 0.1712(3) 0.7311(5) 0.2578(2) 0.038(2) Uiso 1 1 d . . . C31 C 0.1638(4) 0.8089(6) 0.2836(2) 0.053(2) Uiso 1 1 d . . . H31A H 0.1236 0.8319 0.2751 0.08 Uiso 1 1 calc R . . H31B H 0.1932 0.8514 0.28 0.08 Uiso 1 1 calc R . . H31C H 0.1698 0.7927 0.312 0.08 Uiso 1 1 calc R . . C32 C 0.2337(4) 0.6963(6) 0.2709(3) 0.053(2) Uiso 1 1 d . . . H32A H 0.2394 0.6777 0.299 0.08 Uiso 1 1 calc R . . H32B H 0.2629 0.7401 0.2684 0.08 Uiso 1 1 calc R . . H32C H 0.2393 0.6485 0.2537 0.08 Uiso 1 1 calc R . . C33 C 0.1630(4) 0.7594(6) 0.2145(2) 0.058(3) Uiso 1 1 d . . . H33A H 0.1229 0.7825 0.2059 0.087 Uiso 1 1 calc R . . H33B H 0.1683 0.7114 0.1974 0.087 Uiso 1 1 calc R . . H33C H 0.1925 0.8027 0.212 0.087 Uiso 1 1 calc R . . C34 C 0.3360(9) 0.5 0.1831(6) 0.132(8) Uiso 1 2 d S . . H34A H 0.3397 0.5502 0.1665 0.159 Uiso 0.5 1 calc PR . . H34B H 0.3397 0.4498 0.1665 0.159 Uiso 0.5 1 calc PR . . C35 C 0.3846(7) 0.5 0.2180(5) 0.092(5) Uiso 1 2 d S . . H35A H 0.4228 0.5 0.2089 0.138 Uiso 1 2 calc SR . . H35B H 0.3818 0.4498 0.2343 0.138 Uiso 0.5 1 calc PR . . H35C H 0.3818 0.5502 0.2343 0.138 Uiso 0.5 1 calc PR . . C36 C 0.2324(8) 0.5458(12) 0.1600(5) 0.062(5) Uiso 0.5 1 d P . . H36A H 0.1955 0.5568 0.1704 0.075 Uiso 0.5 1 calc PR . . H36B H 0.2489 0.6006 0.1538 0.075 Uiso 0.5 1 calc PR . . C37 C 0.2191(9) 0.5 0.1262(6) 0.121(7) Uiso 1 2 d S . . H37A H 0.1893 0.5297 0.1064 0.182 Uiso 0.5 1 calc PR . . H37B H 0.2031 0.4455 0.1324 0.182 Uiso 0.5 1 calc PR . . H37C H 0.2552 0.4913 0.1151 0.182 Uiso 0.5 1 calc PR . . K1B K 0.36302(11) 0.5 -0.12060(8) 0.0478(7) Uani 1 2 d S . 1 Si1B Si 0.43028(12) 0.5 -0.02018(8) 0.0280(7) Uani 1 2 d S . 1 Si2B Si 0.48261(12) 0.5 0.04519(8) 0.0274(7) Uani 1 2 d S . 1 O1B O 0.2487(5) 0.5 -0.1593(3) 0.083(3) Uiso 1 2 d S . 1 N1B N 0.3717(3) 0.5779(4) -0.03797(17) 0.0326(15) Uiso 1 1 d . . 1 N2B N 0.4796(2) 0.5778(4) 0.08480(17) 0.0305(15) Uiso 1 1 d . A 1 C1B C 0.3167(3) 0.5450(5) -0.0320(2) 0.0369(19) Uiso 1 1 d . . 1 C2B C 0.2676(3) 0.5876(6) -0.0241(2) 0.045(2) Uiso 1 1 d . . 1 H2B H 0.2674 0.6472 -0.0236 0.054 Uiso 1 1 calc R . 1 C3B C 0.2183(4) 0.5430(5) -0.0169(2) 0.051(2) Uiso 1 1 d . . 1 H3B H 0.1843 0.5725 -0.012 0.061 Uiso 1 1 calc R . 1 C4B C 0.3837(3) 0.6677(5) -0.0313(2) 0.037(2) Uiso 1 1 d . . 1 H4B1 H 0.4274 0.6742 -0.0226 0.045 Uiso 1 1 calc R . 1 H4B2 H 0.3656 0.6849 -0.0082 0.045 Uiso 1 1 calc R . 1 C5B C 0.3633(4) 0.7313(5) -0.0655(2) 0.043(2) Uiso 1 1 d . . 1 C6B C 0.3726(4) 0.7003(7) -0.1054(3) 0.073(3) Uiso 1 1 d . . 1 H6B1 H 0.3586 0.7427 -0.126 0.109 Uiso 1 1 calc R . 1 H6B2 H 0.3502 0.6481 -0.1121 0.109 Uiso 1 1 calc R . 1 H6B3 H 0.4151 0.6897 -0.1042 0.109 Uiso 1 1 calc R . 1 C7B C 0.2993(4) 0.7621(7) -0.0690(3) 0.082(3) Uiso 1 1 d . . 1 H7B1 H 0.2933 0.7823 -0.0427 0.122 Uiso 1 1 calc R . 1 H7B2 H 0.2718 0.7158 -0.078 0.122 Uiso 1 1 calc R . 1 H7B3 H 0.2918 0.8079 -0.0886 0.122 Uiso 1 1 calc R . 1 C8B C 0.4030(4) 0.8088(7) -0.0541(3) 0.074(3) Uiso 1 1 d . . 1 H8B1 H 0.3978 0.8299 -0.0278 0.111 Uiso 1 1 calc R . 1 H8B2 H 0.3917 0.8526 -0.0745 0.111 Uiso 1 1 calc R . 1 H8B3 H 0.4448 0.7933 -0.0528 0.111 Uiso 1 1 calc R . 1 C9B C 0.5036(3) 0.5450(5) 0.1223(2) 0.0306(18) Uiso 1 1 d . . 1 C10B C 0.5293(3) 0.5869(5) 0.1572(2) 0.037(2) Uiso 1 1 d . . 1 H10B H 0.5295 0.6465 0.1574 0.044 Uiso 1 1 calc R . 1 C11B C 0.5548(3) 0.5435(5) 0.1919(2) 0.043(2) Uiso 1 1 d . . 1 H11B H 0.5722 0.5734 0.2155 0.051 Uiso 1 1 calc R . 1 C12B C 0.4617(3) 0.6654(5) 0.0794(2) 0.0327(19) Uiso 1 1 d . A 1 H12A H 0.4588 0.6797 0.0506 0.039 Uiso 1 1 calc R A 1 H12B H 0.494 0.7002 0.095 0.039 Uiso 1 1 calc R A 1 C13B C 0.4029(3) 0.6910(5) 0.0917(2) 0.042(2) Uiso 1 1 d . A 1 C14B C 0.3544(4) 0.6277(6) 0.0754(2) 0.051(2) Uiso 1 1 d . A 1 H14A H 0.3172 0.6441 0.0836 0.076 Uiso 1 1 calc R A 1 H14B H 0.3664 0.5719 0.0862 0.076 Uiso 1 1 calc R A 1 H14C H 0.3484 0.6264 0.0459 0.076 Uiso 1 1 calc R A 1 C15B C 0.4092(4) 0.6981(6) 0.1375(3) 0.063(3) Uiso 1 1 d . A 1 H15D H 0.4406 0.7387 0.1479 0.095 Uiso 1 1 calc R A 1 H15E H 0.4198 0.6432 0.1498 0.095 Uiso 1 1 calc R A 1 H15F H 0.3714 0.7169 0.144 0.095 Uiso 1 1 calc R A 1 C16B C 0.3863(4) 0.7786(6) 0.0735(3) 0.067(3) Uiso 1 1 d . A 1 H16D H 0.4179 0.8186 0.0842 0.1 Uiso 1 1 calc R A 1 H16E H 0.3487 0.797 0.0806 0.1 Uiso 1 1 calc R A 1 H16F H 0.3817 0.7757 0.0441 0.1 Uiso 1 1 calc R A 1 C17B C 0.2074(10) 0.5413(14) -0.1328(7) 0.085(7) Uiso 0.5 1 d P . 1 H17D H 0.2272 0.5308 -0.1045 0.101 Uiso 0.5 1 calc PR . 1 H17E H 0.2101 0.6026 -0.137 0.101 Uiso 0.5 1 calc PR . 1 C18B C 0.1597(10) 0.5282(18) -0.1340(7) 0.116(10) Uiso 0.5 1 d P . 1 H18A H 0.145 0.5634 -0.1142 0.174 Uiso 0.5 1 calc PR . 1 H18B H 0.1546 0.469 -0.1277 0.174 Uiso 0.5 1 calc PR . 1 H18C H 0.1373 0.5407 -0.161 0.174 Uiso 0.5 1 calc PR . 1 C19B C 0.2224(10) 0.5 -0.2011(7) 0.143(8) Uiso 1 2 d S . 1 H19A H 0.1966 0.4499 -0.2068 0.171 Uiso 0.5 1 calc PR . 1 H19B H 0.1966 0.5501 -0.2068 0.171 Uiso 0.5 1 calc PR . 1 C20B C 0.2624(7) 0.5 -0.2277(5) 0.084(5) Uiso 1 2 d S . 1 H20A H 0.2402 0.5 -0.2555 0.126 Uiso 1 2 calc SR . 1 H20B H 0.2875 0.4498 -0.223 0.126 Uiso 0.5 1 calc PR . 1 H20C H 0.2875 0.5502 -0.223 0.126 Uiso 0.5 1 calc PR . 1 O1S O 0.5 0 0 0.148(8) Uiso 1 4 d S . 1 O2S O 0.1186(4) 0 0.3816(3) 0.076(3) Uiso 1 2 d S B 1 O3S O 0 0 0.5 0.125(7) Uiso 1 4 d S . 1 C1S C 0.474(2) 0.014(11) 0.0317(15) 0.31(3) Uiso 0.5 1 d P . 1 C2S C 0.4478(12) 0 0.0560(8) 0.142(9) Uiso 1 2 d S . 1 C3S C 0.1742(8) 0 0.4048(5) 0.094(5) Uiso 1 2 d S B 1 H3S1 H 0.1961 0.0502 0.3983 0.113 Uiso 0.5 1 calc PR B 1 H3S2 H 0.1961 -0.0502 0.3983 0.113 Uiso 0.5 1 calc PR B 1 C4S C 0.1728(8) 0 0.4477(5) 0.102(6) Uiso 1 2 d S B 1 H4S1 H 0.2137 0 0.4633 0.152 Uiso 1 2 calc SR B 1 H4S2 H 0.152 -0.0502 0.4544 0.152 Uiso 0.5 1 calc PR B 1 H4S3 H 0.152 0.0502 0.4544 0.152 Uiso 0.5 1 calc PR B 1 C5S C 0.1137(7) 0 0.3402(5) 0.086(5) Uiso 1 2 d S B 1 H5S1 H 0.1344 -0.0501 0.3325 0.103 Uiso 0.5 1 calc PR B 1 H5S2 H 0.1344 0.0501 0.3325 0.103 Uiso 0.5 1 calc PR B 1 C6S C 0.0540(8) 0 0.3181(5) 0.108(6) Uiso 1 2 d S B 1 H6S1 H 0.0544 0 0.2892 0.162 Uiso 1 2 calc SR B 1 H6S2 H 0.0333 0.0502 0.3249 0.162 Uiso 0.5 1 calc PR B 1 H6S3 H 0.0333 -0.0502 0.3249 0.162 Uiso 0.5 1 calc PR B 1 C7S C 0.0389(13) 0 0.5322(9) 0.193(13) Uiso 1 2 d S C 1 H7S1 H 0.061 -0.0487 0.5242 0.231 Uiso 0.5 1 calc PR C 1 H7S2 H 0.061 0.0487 0.5242 0.231 Uiso 0.5 1 calc PR C 1 C8S C 0.0635(15) 0 0.5646(10) 0.227(16) Uiso 1 2 d S C 1 H8S1 H 0.1065 0 0.5653 0.34 Uiso 1 2 calc SR C 1 H8S2 H 0.0526 -0.0502 0.5782 0.34 Uiso 0.5 1 calc PR C 1 H8S3 H 0.0526 0.0502 0.5782 0.34 Uiso 0.5 1 calc PR C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0279(13) 0.0506(18) 0.0443(15) 0 0.0093(12) 0 K2 0.0386(15) 0.0496(18) 0.0401(15) 0 0.0120(12) 0 Si1 0.0231(15) 0.0352(19) 0.0233(15) 0 0.0015(13) 0 Si2 0.0217(15) 0.0307(18) 0.0260(16) 0 0.0040(13) 0 Si3 0.0213(15) 0.0315(18) 0.0248(15) 0 0.0042(12) 0 Si4 0.0234(15) 0.0262(17) 0.0253(15) 0 0.0041(12) 0 K1B 0.0382(15) 0.061(2) 0.0432(15) 0 0.0041(12) 0 Si1B 0.0242(15) 0.0309(19) 0.0294(16) 0 0.0063(13) 0 Si2B 0.0261(16) 0.0288(18) 0.0271(16) 0 0.0048(13) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N2 3.010(6) 6_565 ? K1 N2 3.010(6) . ? K1 C1 3.118(8) . ? K1 C1 3.118(8) 6_565 ? K1 C12 3.133(7) 5_566 ? K1 C12 3.133(7) 2_556 ? K2 O1 2.629(10) . ? K2 N4 3.008(6) 6_565 ? K2 N4 3.008(6) . ? K2 C18 3.120(7) 6_565 ? K2 C18 3.120(7) . ? K2 C32 3.164(9) 6_565 ? Si1 N1 1.821(6) 6_565 ? Si1 N1 1.821(6) . ? Si1 Si2 2.299(4) . ? Si1 Si4 2.305(4) . ? Si2 N2 1.855(6) 6_565 ? Si2 N2 1.855(6) . ? Si2 Si3 2.302(4) . ? Si3 N3 1.824(6) . ? Si3 N3 1.824(6) 6_565 ? Si3 Si4 2.304(4) . ? Si4 N4 1.839(6) . ? Si4 N4 1.839(6) 6_565 ? O1 C34 1.42(2) . ? O1 C36 1.574(18) 6_565 ? O1 C36 1.574(18) . ? N1 C1 1.394(9) . ? N1 C4 1.444(9) . ? N2 C10 1.402(8) . ? N2 C13 1.457(9) 6_565 ? N3 C18 1.406(8) . ? N3 C21 1.447(9) . ? N4 C26 1.401(9) . ? N4 C29 1.472(9) . ? C1 C2 1.388(10) . ? C1 C1 1.412(16) 6_565 ? C2 C3 1.418(11) . ? C3 C3 1.340(17) 6_565 ? C4 C5 1.555(10) . ? C5 C8 1.527(11) . ? C5 C7 1.528(11) . ? C5 C6 1.539(12) . ? C10 C11 1.380(9) . ? C10 C10 1.430(14) 6_565 ? C11 C12 1.390(10) . ? C12 C12 1.392(15) 6_565 ? C12 K1 3.133(7) 5_566 ? C13 N2 1.457(9) 6_565 ? C13 C14 1.559(10) . ? C14 C17 1.510(11) . ? C14 C16 1.538(11) . ? C14 C15 1.542(10) . ? C18 C19 1.387(10) . ? C18 C18 1.423(14) 6_565 ? C19 C20 1.418(10) . ? C20 C20 1.361(16) 6_565 ? C21 C22 1.547(10) . ? C22 C24 1.526(11) . ? C22 C23 1.529(11) . ? C22 C25 1.552(11) . ? C26 C27 1.381(10) . ? C26 C26 1.417(15) 6_565 ? C27 C28 1.411(11) . ? C28 C28 1.359(17) 6_565 ? C29 C30 1.556(10) . ? C30 C33 1.511(11) . ? C30 C32 1.519(11) . ? C30 C31 1.544(11) . ? C34 C35 1.46(2) . ? C36 C37 1.34(2) . ? K1B O1B 2.691(11) . ? K1B N1B 3.030(6) 6_565 ? K1B N1B 3.030(6) . ? K1B C9B 3.147(7) 2_655 ? K1B C9B 3.147(7) 5_665 ? Si1B N1B 1.842(6) 6_565 ? Si1B N1B 1.842(6) . ? Si1B Si2B 2.303(4) . ? Si1B Si2B 2.310(4) 5_665 ? Si2B N2B 1.837(6) 6_565 ? Si2B N2B 1.837(6) . ? Si2B Si1B 2.310(4) 5_665 ? O1B C19B 1.43(2) . ? O1B C17B 1.57(2) 6_565 ? O1B C17B 1.57(2) . ? N1B C1B 1.412(9) . ? N1B C4B 1.467(10) . ? N2B C9B 1.385(9) . ? N2B C12B 1.455(9) . ? C1B C2B 1.383(10) . ? C1B C1B 1.433(15) 6_565 ? C2B C3B 1.393(11) . ? C3B C3B 1.370(17) 6_565 ? C4B C5B 1.541(11) . ? C5B C6B 1.491(12) . ? C5B C7B 1.526(12) . ? C5B C8B 1.537(12) . ? C9B C10B 1.384(10) . ? C9B C9B 1.435(14) 6_565 ? C9B K1B 3.147(7) 5_665 ? C10B C11B 1.391(10) . ? C11B C11B 1.388(16) 6_565 ? C12B C13B 1.539(10) . ? C13B C14B 1.522(11) . ? C13B C15B 1.530(11) . ? C13B C16B 1.544(12) . ? C17B C18B 1.10(2) . ? C19B C20B 1.40(2) . ? O1S C1S 1.34(6) 2_655 ? O1S C1S 1.34(6) 5_655 ? O1S C1S 1.34(6) . ? O1S C1S 1.34(6) 6 ? O2S C3S 1.360(17) . ? O2S C5S 1.384(16) . ? O3S C7S 1.27(3) 5_556 ? O3S C7S 1.27(3) . ? C1S C2S 1.13(6) . ? C2S C2S 0.00(5) 6 ? C3S C4S 1.46(2) . ? C5S C6S 1.43(2) . ? C7S C8S 1.13(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 K1 N2 49.2(2) 6_565 . ? N2 K1 C1 92.94(18) 6_565 . ? N2 K1 C1 103.88(19) . . ? N2 K1 C1 103.88(19) 6_565 6_565 ? N2 K1 C1 92.94(18) . 6_565 ? C1 K1 C1 26.2(3) . 6_565 ? N2 K1 C12 128.42(18) 6_565 5_566 ? N2 K1 C12 143.75(19) . 5_566 ? C1 K1 C12 112.3(2) . 5_566 ? C1 K1 C12 118.7(2) 6_565 5_566 ? N2 K1 C12 143.75(19) 6_565 2_556 ? N2 K1 C12 128.42(18) . 2_556 ? C1 K1 C12 118.7(2) . 2_556 ? C1 K1 C12 112.3(2) 6_565 2_556 ? C12 K1 C12 25.7(3) 5_566 2_556 ? O1 K2 N4 108.2(2) . 6_565 ? O1 K2 N4 108.2(2) . . ? N4 K2 N4 48.3(2) 6_565 . ? O1 K2 C18 148.3(3) . 6_565 ? N4 K2 C18 92.70(17) 6_565 6_565 ? N4 K2 C18 103.51(18) . 6_565 ? O1 K2 C18 148.3(3) . . ? N4 K2 C18 103.51(18) 6_565 . ? N4 K2 C18 92.70(17) . . ? C18 K2 C18 26.4(3) 6_565 . ? O1 K2 C32 96.28(16) . 6_565 ? N4 K2 C32 58.12(19) 6_565 6_565 ? N4 K2 C32 106.3(2) . 6_565 ? C18 K2 C32 74.4(2) 6_565 6_565 ? C18 K2 C32 100.5(2) . 6_565 ? N1 Si1 N1 85.0(4) 6_565 . ? N1 Si1 Si2 115.7(2) 6_565 . ? N1 Si1 Si2 115.7(2) . . ? N1 Si1 Si4 127.8(2) 6_565 . ? N1 Si1 Si4 127.8(2) . . ? Si2 Si1 Si4 87.74(14) . . ? N2 Si2 N2 85.0(4) 6_565 . ? N2 Si2 Si1 120.0(2) 6_565 . ? N2 Si2 Si1 120.0(2) . . ? N2 Si2 Si3 121.4(2) 6_565 . ? N2 Si2 Si3 121.4(2) . . ? Si1 Si2 Si3 92.39(14) . . ? N3 Si3 N3 85.8(4) . 6_565 ? N3 Si3 Si2 127.3(2) . . ? N3 Si3 Si2 127.3(2) 6_565 . ? N3 Si3 Si4 115.9(2) . . ? N3 Si3 Si4 115.9(2) 6_565 . ? Si2 Si3 Si4 87.69(13) . . ? N4 Si4 N4 84.1(4) . 6_565 ? N4 Si4 Si3 120.2(2) . . ? N4 Si4 Si3 120.2(2) 6_565 . ? N4 Si4 Si1 121.8(2) . . ? N4 Si4 Si1 121.8(2) 6_565 . ? Si3 Si4 Si1 92.18(14) . . ? C34 O1 C36 110.5(12) . 6_565 ? C34 O1 C36 110.5(12) . . ? C36 O1 C36 55.3(14) 6_565 . ? C34 O1 K2 128.5(11) . . ? C36 O1 K2 114.8(9) 6_565 . ? C36 O1 K2 114.8(9) . . ? C1 N1 C4 121.6(6) . . ? C1 N1 Si1 110.4(5) . . ? C4 N1 Si1 127.3(5) . . ? C10 N2 C13 120.3(6) . 6_565 ? C10 N2 Si2 108.7(4) . . ? C13 N2 Si2 119.0(4) 6_565 . ? C10 N2 K1 92.0(4) . . ? C13 N2 K1 123.6(4) 6_565 . ? Si2 N2 K1 85.8(2) . . ? C18 N3 C21 121.7(6) . . ? C18 N3 Si3 109.5(5) . . ? C21 N3 Si3 128.0(5) . . ? C26 N4 C29 119.5(6) . . ? C26 N4 Si4 108.7(5) . . ? C29 N4 Si4 120.0(5) . . ? C26 N4 K2 94.4(4) . . ? C29 N4 K2 120.8(4) . . ? Si4 N4 K2 86.5(2) . . ? C2 C1 N1 128.2(7) . . ? C2 C1 C1 119.7(5) . 6_565 ? N1 C1 C1 112.1(4) . 6_565 ? C2 C1 K1 84.5(5) . . ? N1 C1 K1 105.6(4) . . ? C1 C1 K1 76.91(14) 6_565 . ? C1 C2 C3 119.7(8) . . ? C3 C3 C2 120.7(5) 6_565 . ? N1 C4 C5 117.7(6) . . ? C8 C5 C7 108.5(7) . . ? C8 C5 C6 107.7(7) . . ? C7 C5 C6 111.0(7) . . ? C8 C5 C4 112.3(7) . . ? C7 C5 C4 110.0(7) . . ? C6 C5 C4 107.3(7) . . ? C11 C10 N2 128.4(7) . . ? C11 C10 C10 118.9(4) . 6_565 ? N2 C10 C10 112.6(4) . 6_565 ? C10 C11 C12 121.6(7) . . ? C11 C12 C12 119.5(4) . 6_565 ? C11 C12 K1 113.6(5) . 5_566 ? C12 C12 K1 77.17(13) 6_565 5_566 ? N2 C13 C14 120.9(6) 6_565 . ? C17 C14 C16 110.6(6) . . ? C17 C14 C15 108.7(6) . . ? C16 C14 C15 106.6(7) . . ? C17 C14 C13 111.8(7) . . ? C16 C14 C13 106.3(6) . . ? C15 C14 C13 112.7(6) . . ? C19 C18 N3 127.6(7) . . ? C19 C18 C18 120.0(4) . 6_565 ? N3 C18 C18 112.2(4) . 6_565 ? C19 C18 K2 82.2(4) . . ? N3 C18 K2 106.6(4) . . ? C18 C18 K2 76.82(13) 6_565 . ? C18 C19 C20 119.2(7) . . ? C20 C20 C19 120.7(5) 6_565 . ? N3 C21 C22 116.9(6) . . ? C24 C22 C23 111.1(7) . . ? C24 C22 C21 111.3(6) . . ? C23 C22 C21 107.6(6) . . ? C24 C22 C25 108.1(6) . . ? C23 C22 C25 106.7(7) . . ? C21 C22 C25 112.0(6) . . ? C27 C26 N4 128.2(7) . . ? C27 C26 C26 119.7(5) . 6_565 ? N4 C26 C26 111.9(4) . 6_565 ? C26 C27 C28 120.0(8) . . ? C28 C28 C27 120.3(5) 6_565 . ? N4 C29 C30 120.3(6) . . ? C33 C30 C32 109.0(7) . . ? C33 C30 C31 107.6(7) . . ? C32 C30 C31 109.2(7) . . ? C33 C30 C29 114.6(7) . . ? C32 C30 C29 111.3(7) . . ? C31 C30 C29 105.1(6) . . ? C30 C32 K2 118.0(5) . . ? O1 C34 C35 113.3(17) . . ? C37 C36 O1 111.8(15) . . ? O1B K1B N1B 109.5(2) . 6_565 ? O1B K1B N1B 109.5(2) . . ? N1B K1B N1B 48.4(2) 6_565 . ? O1B K1B C9B 147.8(3) . 2_655 ? N1B K1B C9B 102.66(18) 6_565 2_655 ? N1B K1B C9B 91.86(18) . 2_655 ? O1B K1B C9B 147.8(3) . 5_665 ? N1B K1B C9B 91.86(18) 6_565 5_665 ? N1B K1B C9B 102.66(18) . 5_665 ? C9B K1B C9B 26.4(3) 2_655 5_665 ? N1B Si1B N1B 84.8(4) 6_565 . ? N1B Si1B Si2B 121.7(2) 6_565 . ? N1B Si1B Si2B 121.7(2) . . ? N1B Si1B Si2B 120.4(2) 6_565 5_665 ? N1B Si1B Si2B 120.4(2) . 5_665 ? Si2B Si1B Si2B 91.48(14) . 5_665 ? N2B Si2B N2B 84.9(4) 6_565 . ? N2B Si2B Si1B 127.9(2) 6_565 . ? N2B Si2B Si1B 127.9(2) . . ? N2B Si2B Si1B 115.1(2) 6_565 5_665 ? N2B Si2B Si1B 115.1(2) . 5_665 ? Si1B Si2B Si1B 88.52(14) . 5_665 ? C19B O1B C17B 112.5(13) . 6_565 ? C19B O1B C17B 112.5(13) . . ? C17B O1B C17B 49.6(17) 6_565 . ? C19B O1B K1B 131.9(11) . . ? C17B O1B K1B 110.9(9) 6_565 . ? C17B O1B K1B 110.9(9) . . ? C1B N1B C4B 119.1(6) . . ? C1B N1B Si1B 108.4(5) . . ? C4B N1B Si1B 120.2(5) . . ? C1B N1B K1B 94.4(4) . . ? C4B N1B K1B 121.3(4) . . ? Si1B N1B K1B 86.5(2) . . ? C9B N2B C12B 121.9(6) . . ? C9B N2B Si2B 110.5(5) . . ? C12B N2B Si2B 127.2(5) . . ? C2B C1B N1B 128.6(7) . . ? C2B C1B C1B 119.4(5) . 6_565 ? N1B C1B C1B 111.8(4) . 6_565 ? C1B C2B C3B 119.9(8) . . ? C3B C3B C2B 120.7(5) 6_565 . ? N1B C4B C5B 120.4(6) . . ? C6B C5B C7B 109.6(7) . . ? C6B C5B C8B 108.2(8) . . ? C7B C5B C8B 105.9(8) . . ? C6B C5B C4B 112.7(7) . . ? C7B C5B C4B 114.7(7) . . ? C8B C5B C4B 105.2(7) . . ? C10B C9B N2B 128.9(7) . . ? C10B C9B C9B 118.8(4) . 6_565 ? N2B C9B C9B 112.2(4) . 6_565 ? C10B C9B K1B 82.6(4) . 5_665 ? N2B C9B K1B 106.5(4) . 5_665 ? C9B C9B K1B 76.82(13) 6_565 5_665 ? C9B C10B C11B 121.4(8) . . ? C11B C11B C10B 119.8(5) 6_565 . ? N2B C12B C13B 117.3(6) . . ? C14B C13B C15B 109.7(7) . . ? C14B C13B C12B 109.9(7) . . ? C15B C13B C12B 112.1(7) . . ? C14B C13B C16B 110.3(7) . . ? C15B C13B C16B 107.8(7) . . ? C12B C13B C16B 107.0(7) . . ? C18B C17B O1B 127(2) . . ? C20B C19B O1B 115.7(18) . . ? C1S O1S C1S 161(10) 2_655 . ? C1S O1S C1S 180(4) 5_655 . ? C1S O1S C1S 180(10) 2_655 6 ? C1S O1S C1S 161(10) 5_655 6 ? C3S O2S C5S 117.9(13) . . ? C7S O3S C7S 180(2) 5_556 . ? C2S C1S O1S 158(10) . . ? O2S C3S C4S 112.1(15) . . ? O2S C5S C6S 114.5(15) . . ? C8S C7S O3S 166(4) . . ? #===END data_(15)-apr603 _database_code_depnum_ccdc_archive 'CCDC 286733' _audit_creation_date 2003-04-04T09:23:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C38 H70 N4 Si4' _chemical_formula_sum 'C38 H70 N4 Si4' _chemical_formula_weight 695.34 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0126(2) _cell_length_b 10.7343(2) _cell_length_c 17.9366(4) _cell_angle_alpha 90 _cell_angle_beta 93.993(1) _cell_angle_gamma 90 _cell_volume 2115.18(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 73077 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.17 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.290956E-1 _diffrn_orient_matrix_ub_12 -0.57648E-2 _diffrn_orient_matrix_ub_13 0.514704E-1 _diffrn_orient_matrix_ub_21 0.852764E-1 _diffrn_orient_matrix_ub_22 0.120106E-1 _diffrn_orient_matrix_ub_23 0.217732E-1 _diffrn_orient_matrix_ub_31 -0.129276E-1 _diffrn_orient_matrix_ub_32 0.922018E-1 _diffrn_orient_matrix_ub_33 0.3818E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_number 25773 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 4801 _reflns_number_gt 4178 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0570P)^2^+1.0611P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 4801 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.387 _refine_diff_density_min -0.36 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 Si1 Si 0.53647(4) 0.39753(4) 0.52428(2) 0.02232(12) Uani 1 1 d . . . Si2 Si 0.75295(4) 0.38646(4) 0.53843(3) 0.03096(14) Uani 1 1 d . . . N1 N 0.46404(12) 0.27438(12) 0.47299(7) 0.0260(3) Uani 1 1 d . . . N2 N 0.46362(12) 0.35363(13) 0.60504(7) 0.0275(3) Uani 1 1 d . . . C1 C 0.35753(14) 0.24236(15) 0.50773(8) 0.0276(3) Uani 1 1 d . . . C2 C 0.35720(14) 0.28746(15) 0.58193(8) 0.0285(3) Uani 1 1 d . . . C3 C 0.25566(16) 0.26915(18) 0.62215(10) 0.0383(4) Uani 1 1 d . . . H3 H 0.2547 0.2998 0.6718 0.046 Uiso 1 1 calc R . . C4 C 0.15512(17) 0.2057(2) 0.58969(11) 0.0455(5) Uani 1 1 d . . . H4 H 0.0858 0.193 0.6175 0.055 Uiso 1 1 calc R . . C5 C 0.15533(17) 0.1613(2) 0.51783(12) 0.0457(5) Uani 1 1 d . . . H5 H 0.0863 0.118 0.4963 0.055 Uiso 1 1 calc R . . C6 C 0.25634(16) 0.17956(18) 0.47627(10) 0.0369(4) Uani 1 1 d . . . H6 H 0.2559 0.1491 0.4265 0.044 Uiso 1 1 calc R . . C7 C 0.47346(16) 0.25529(15) 0.39268(8) 0.0294(3) Uani 1 1 d . . . H7A H 0.5237 0.3237 0.3742 0.035 Uiso 1 1 calc R . . H7B H 0.3909 0.2641 0.3677 0.035 Uiso 1 1 calc R . . C8 C 0.52709(17) 0.13099(16) 0.36670(9) 0.0345(4) Uani 1 1 d . . . C9 C 0.4479(2) 0.01875(19) 0.38224(13) 0.0506(5) Uani 1 1 d . . . H9A H 0.366 0.0312 0.3584 0.076 Uiso 1 1 calc R . . H9B H 0.4431 0.0094 0.4363 0.076 Uiso 1 1 calc R . . H9C H 0.4838 -0.0565 0.362 0.076 Uiso 1 1 calc R . . C10 C 0.5360(2) 0.1438(2) 0.28185(11) 0.0558(6) Uani 1 1 d . . . H10A H 0.4546 0.157 0.2575 0.084 Uiso 1 1 calc R . . H10B H 0.5712 0.0676 0.2623 0.084 Uiso 1 1 calc R . . H10C H 0.5881 0.215 0.2716 0.084 Uiso 1 1 calc R . . C11 C 0.6531(2) 0.1097(2) 0.40449(12) 0.0485(5) Uani 1 1 d . . . H11A H 0.7054 0.181 0.3949 0.073 Uiso 1 1 calc R . . H11B H 0.6882 0.0338 0.3845 0.073 Uiso 1 1 calc R . . H11C H 0.6471 0.1005 0.4585 0.073 Uiso 1 1 calc R . . C12 C 0.47251(17) 0.42341(16) 0.67533(9) 0.0323(4) Uani 1 1 d . . . H12A H 0.3903 0.4555 0.6838 0.039 Uiso 1 1 calc R . . H12B H 0.5252 0.4966 0.6684 0.039 Uiso 1 1 calc R . . C13 C 0.52151(19) 0.35578(18) 0.74765(9) 0.0402(4) Uani 1 1 d . . . C14 C 0.64480(19) 0.2970(2) 0.73708(11) 0.0505(5) Uani 1 1 d . . . H14A H 0.6357 0.2324 0.6984 0.076 Uiso 1 1 calc R . . H14B H 0.6768 0.2595 0.7842 0.076 Uiso 1 1 calc R . . H14C H 0.7013 0.3611 0.7217 0.076 Uiso 1 1 calc R . . C15 C 0.5349(3) 0.4565(3) 0.80760(13) 0.0900(11) Uani 1 1 d . . . H15A H 0.4553 0.4944 0.814 0.135 Uiso 1 1 calc R . . H15B H 0.5915 0.5206 0.7924 0.135 Uiso 1 1 calc R . . H15C H 0.5664 0.4193 0.8549 0.135 Uiso 1 1 calc R . . C16 C 0.4372(2) 0.2528(3) 0.77233(13) 0.0659(7) Uani 1 1 d . . . H16A H 0.3566 0.2877 0.7792 0.099 Uiso 1 1 calc R . . H16B H 0.4709 0.217 0.8196 0.099 Uiso 1 1 calc R . . H16C H 0.4302 0.1876 0.734 0.099 Uiso 1 1 calc R . . C17 C 0.8199(2) 0.4200(2) 0.44724(13) 0.0504(5) Uani 1 1 d . . . H17A H 0.792 0.5017 0.4288 0.076 Uiso 1 1 calc R . . H17B H 0.7938 0.3558 0.4107 0.076 Uiso 1 1 calc R . . H17C H 0.9089 0.4199 0.4546 0.076 Uiso 1 1 calc R . . C18 C 0.80653(17) 0.22942(18) 0.57398(11) 0.0437(4) Uani 1 1 d . . . H18A H 0.7721 0.2123 0.6219 0.066 Uiso 1 1 calc R . . H18B H 0.8956 0.2291 0.5809 0.066 Uiso 1 1 calc R . . H18C H 0.7798 0.1651 0.5377 0.066 Uiso 1 1 calc R . . C19 C 0.81202(19) 0.5108(2) 0.60507(12) 0.0481(5) Uani 1 1 d . . . H19A H 0.7844 0.5926 0.5864 0.072 Uiso 1 1 calc R . . H19B H 0.9012 0.5087 0.6093 0.072 Uiso 1 1 calc R . . H19C H 0.7813 0.4961 0.6543 0.072 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 Si1 0.0200(2) 0.0248(2) 0.0220(2) 0.00017(15) 0.00075(15) 0.00031(15) Si2 0.0211(2) 0.0322(3) 0.0393(3) 0.00240(18) 0.00034(18) 0.00100(17) N1 0.0275(7) 0.0276(7) 0.0231(6) -0.0019(5) 0.0038(5) -0.0036(5) N2 0.0309(7) 0.0304(7) 0.0211(6) 0.0006(5) 0.0020(5) -0.0025(6) C1 0.0266(8) 0.0285(8) 0.0279(7) 0.0031(6) 0.0023(6) -0.0022(6) C2 0.0287(8) 0.0306(8) 0.0265(7) 0.0044(6) 0.0031(6) -0.0007(6) C3 0.0370(9) 0.0464(10) 0.0327(8) 0.0048(7) 0.0111(7) -0.0012(8) C4 0.0313(9) 0.0567(12) 0.0501(11) 0.0108(9) 0.0127(8) -0.0062(9) C5 0.0297(9) 0.0529(12) 0.0541(11) 0.0050(9) 0.0003(8) -0.0128(8) C6 0.0332(9) 0.0404(10) 0.0367(9) -0.0004(7) -0.0007(7) -0.0080(8) C7 0.0362(9) 0.0281(8) 0.0241(7) 0.0009(6) 0.0037(6) -0.0022(7) C8 0.0442(10) 0.0305(8) 0.0296(8) -0.0035(7) 0.0081(7) -0.0009(7) C9 0.0633(14) 0.0322(10) 0.0578(12) -0.0085(9) 0.0149(10) -0.0075(9) C10 0.0802(16) 0.0573(13) 0.0314(10) -0.0079(9) 0.0150(10) 0.0044(12) C11 0.0493(12) 0.0429(11) 0.0536(12) -0.0040(9) 0.0064(9) 0.0092(9) C12 0.0421(10) 0.0310(8) 0.0236(7) -0.0009(6) 0.0006(6) 0.0052(7) C13 0.0537(11) 0.0442(10) 0.0222(8) 0.0001(7) -0.0016(7) 0.0114(9) C14 0.0496(12) 0.0596(13) 0.0411(10) 0.0092(9) -0.0053(8) 0.0084(10) C15 0.147(3) 0.084(2) 0.0346(12) -0.0244(12) -0.0260(14) 0.047(2) C16 0.0610(14) 0.0910(19) 0.0466(12) 0.0380(12) 0.0106(10) 0.0103(13) C17 0.0438(11) 0.0511(12) 0.0585(12) 0.0066(10) 0.0199(9) -0.0002(9) C18 0.0360(10) 0.0424(10) 0.0517(11) 0.0045(8) -0.0036(8) 0.0113(8) C19 0.0412(11) 0.0443(11) 0.0568(12) -0.0021(9) -0.0109(9) -0.0079(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 N2 1.7680(13) . ? Si1 N1 1.7686(13) . ? Si1 Si2 2.3828(6) . ? Si1 Si1 2.4791(8) 3_666 ? Si2 C17 1.875(2) . ? Si2 C19 1.878(2) . ? Si2 C18 1.8825(19) . ? N1 C1 1.4086(19) . ? N1 C7 1.4657(19) . ? N2 C2 1.408(2) . ? N2 C12 1.464(2) . ? C1 C6 1.388(2) . ? C1 C2 1.416(2) . ? C2 C3 1.386(2) . ? C3 C4 1.392(3) . ? C4 C5 1.374(3) . ? C5 C6 1.395(3) . ? C7 C8 1.544(2) . ? C8 C11 1.519(3) . ? C8 C9 1.524(3) . ? C8 C10 1.538(2) . ? C12 C13 1.550(2) . ? C13 C15 1.525(3) . ? C13 C14 1.521(3) . ? C13 C16 1.529(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 Si1 N1 90.74(6) . . ? N2 Si1 Si2 114.03(5) . . ? N1 Si1 Si2 115.45(5) . . ? N2 Si1 Si1 111.71(5) . 3_666 ? N1 Si1 Si1 110.92(5) . 3_666 ? Si2 Si1 Si1 112.27(3) . 3_666 ? C17 Si2 C19 106.21(10) . . ? C17 Si2 C18 109.53(10) . . ? C19 Si2 C18 109.54(9) . . ? C17 Si2 Si1 110.41(7) . . ? C19 Si2 Si1 109.39(7) . . ? C18 Si2 Si1 111.62(7) . . ? C1 N1 C7 121.25(13) . . ? C1 N1 Si1 108.15(10) . . ? C7 N1 Si1 123.75(10) . . ? C2 N2 C12 121.07(13) . . ? C2 N2 Si1 108.01(10) . . ? C12 N2 Si1 124.21(11) . . ? C6 C1 N1 127.46(15) . . ? C6 C1 C2 119.56(15) . . ? N1 C1 C2 112.89(13) . . ? C3 C2 N2 127.11(15) . . ? C3 C2 C1 119.70(15) . . ? N2 C2 C1 113.11(13) . . ? C2 C3 C4 119.90(17) . . ? C5 C4 C3 120.56(17) . . ? C4 C5 C6 120.39(17) . . ? C1 C6 C5 119.88(17) . . ? N1 C7 C8 118.17(13) . . ? C11 C8 C9 108.41(17) . . ? C11 C8 C10 109.61(17) . . ? C9 C8 C10 109.19(16) . . ? C11 C8 C7 110.63(15) . . ? C9 C8 C7 113.08(15) . . ? C10 C8 C7 105.87(15) . . ? N2 C12 C13 118.65(14) . . ? C15 C13 C14 109.8(2) . . ? C15 C13 C16 109.9(2) . . ? C14 C13 C16 107.51(18) . . ? C15 C13 C12 105.60(17) . . ? C14 C13 C12 110.60(15) . . ? C16 C13 C12 113.46(16) . . ? #===END data_(17)-aug1801 _database_code_depnum_ccdc_archive 'CCDC 286734' _audit_creation_date 2001-08-28T15:19:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((C6H4(NCH2tBu)2Si(Cl))2) _chemical_formula_moiety 'C32 H52 Cl2 N4 Si2' _chemical_formula_sum 'C32 H52 Cl2 N4 Si2' _chemical_formula_weight 619.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.1952(14) _cell_length_b 20.166(3) _cell_length_c 12.5955(14) _cell_angle_alpha 90 _cell_angle_beta 97.602(6) _cell_angle_gamma 90 _cell_volume 3574.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6553 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 7749 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_unetI/netI 0.0801 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 23 _diffrn_reflns_theta_full 23 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2478 _reflns_number_gt 1785 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0329P)^2^+4.5528P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2478 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.05 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.204 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Si Si -0.08200(6) 0.31196(5) 0.21634(7) 0.0285(3) Uani 1 1 d . . . Cl Cl -0.09739(6) 0.38832(5) 0.10353(7) 0.0426(3) Uani 1 1 d . . . N1 N -0.15883(17) 0.31678(13) 0.3105(2) 0.0296(7) Uani 1 1 d . . . N2 N -0.13411(17) 0.24256(13) 0.1552(2) 0.0268(7) Uani 1 1 d . . . C1 C -0.2302(2) 0.26770(16) 0.2884(3) 0.0277(8) Uani 1 1 d . . . C2 C -0.2170(2) 0.22659(16) 0.2014(3) 0.0286(8) Uani 1 1 d . . . C3 C -0.2819(2) 0.17700(17) 0.1693(3) 0.0329(8) Uani 1 1 d . . . H3 H -0.2729 0.1491 0.1107 0.039 Uiso 1 1 calc R . . C4 C -0.3604(2) 0.16813(18) 0.2233(3) 0.0392(9) Uani 1 1 d . . . H4 H -0.4057 0.1347 0.2006 0.047 Uiso 1 1 calc R . . C5 C -0.3724(2) 0.20776(19) 0.3094(3) 0.0398(9) Uani 1 1 d . . . H5 H -0.4257 0.201 0.3465 0.048 Uiso 1 1 calc R . . C6 C -0.3078(2) 0.25748(17) 0.3427(3) 0.0352(9) Uani 1 1 d . . . H6 H -0.3166 0.2844 0.4025 0.042 Uiso 1 1 calc R . . C7 C -0.1526(2) 0.35601(17) 0.4101(3) 0.0338(8) Uani 1 1 d . . . H7A H -0.0845 0.3614 0.4379 0.041 Uiso 1 1 calc R . . H7B H -0.1817 0.3296 0.4635 0.041 Uiso 1 1 calc R . . C8 C -0.1985(2) 0.42510(18) 0.4049(3) 0.0416(10) Uani 1 1 d . . . C9 C -0.1384(3) 0.4752(2) 0.3540(4) 0.0791(16) Uani 1 1 d . . . H9A H -0.0736 0.475 0.3922 0.119 Uiso 1 1 calc R . . H9B H -0.1661 0.5195 0.3583 0.119 Uiso 1 1 calc R . . H9C H -0.1369 0.4635 0.2788 0.119 Uiso 1 1 calc R . . C10 C -0.2019(3) 0.4468(2) 0.5209(3) 0.0662(13) Uani 1 1 d . . . H10A H -0.1375 0.4468 0.56 0.099 Uiso 1 1 calc R . . H10B H -0.2418 0.4159 0.5553 0.099 Uiso 1 1 calc R . . H10C H -0.2287 0.4915 0.5217 0.099 Uiso 1 1 calc R . . C11 C -0.2988(3) 0.4246(2) 0.3463(4) 0.0753(15) Uani 1 1 d . . . H11A H -0.325 0.4696 0.3446 0.113 Uiso 1 1 calc R . . H11B H -0.3384 0.395 0.3834 0.113 Uiso 1 1 calc R . . H11C H -0.2979 0.4088 0.2728 0.113 Uiso 1 1 calc R . . C12 C -0.1224(2) 0.21802(17) 0.0468(3) 0.0332(9) Uani 1 1 d . . . H12A H -0.0981 0.2552 0.0068 0.04 Uiso 1 1 calc R . . H12B H -0.1862 0.2066 0.0097 0.04 Uiso 1 1 calc R . . C13 C -0.0572(2) 0.15818(17) 0.0381(3) 0.0318(8) Uani 1 1 d . . . C14 C 0.0447(2) 0.17548(18) 0.0846(3) 0.0406(9) Uani 1 1 d . . . H14A H 0.0857 0.1368 0.0795 0.061 Uiso 1 1 calc R . . H14B H 0.0464 0.1882 0.1599 0.061 Uiso 1 1 calc R . . H14C H 0.0673 0.2125 0.0443 0.061 Uiso 1 1 calc R . . C15 C -0.0621(3) 0.1431(2) -0.0821(3) 0.0576(12) Uani 1 1 d . . . H15A H -0.1275 0.1318 -0.1113 0.086 Uiso 1 1 calc R . . H15B H -0.0202 0.1056 -0.0923 0.086 Uiso 1 1 calc R . . H15C H -0.0416 0.1821 -0.1193 0.086 Uiso 1 1 calc R . . C16 C -0.0893(2) 0.09766(18) 0.0963(3) 0.0489(11) Uani 1 1 d . . . H16A H -0.1547 0.0863 0.0669 0.073 Uiso 1 1 calc R . . H16B H -0.0864 0.1076 0.1728 0.073 Uiso 1 1 calc R . . H16C H -0.0474 0.0601 0.0867 0.073 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 Si 0.0261(5) 0.0270(5) 0.0322(5) 0.0025(5) 0.0031(4) 0.0023(4) Cl 0.0404(5) 0.0371(6) 0.0493(6) 0.0138(5) 0.0024(4) 0.0023(4) N1 0.0284(15) 0.0283(16) 0.0321(16) -0.0026(14) 0.0040(13) 0.0015(13) N2 0.0246(14) 0.0276(16) 0.0278(15) -0.0002(13) 0.0017(12) 0.0020(12) C1 0.0247(18) 0.024(2) 0.0335(19) 0.0015(16) -0.0011(16) 0.0034(15) C2 0.0225(17) 0.029(2) 0.0328(19) 0.0044(17) -0.0018(15) 0.0030(15) C3 0.0258(18) 0.037(2) 0.0345(19) -0.0006(17) -0.0018(16) 0.0016(16) C4 0.031(2) 0.036(2) 0.049(2) -0.0013(19) -0.0010(18) -0.0077(16) C5 0.0266(19) 0.044(2) 0.050(2) 0.003(2) 0.0077(18) 0.0001(18) C6 0.0301(19) 0.037(2) 0.039(2) -0.0006(18) 0.0067(17) 0.0012(17) C7 0.0304(19) 0.036(2) 0.035(2) -0.0063(18) 0.0052(16) -0.0018(17) C8 0.040(2) 0.037(2) 0.048(2) -0.0065(19) 0.0083(19) 0.0049(18) C9 0.097(4) 0.039(3) 0.111(4) 0.008(3) 0.052(3) 0.013(3) C10 0.078(3) 0.054(3) 0.065(3) -0.026(2) 0.005(2) 0.009(2) C11 0.064(3) 0.055(3) 0.097(4) -0.027(3) -0.025(3) 0.031(2) C12 0.0305(19) 0.040(2) 0.0277(19) 0.0009(17) 0.0000(15) -0.0003(17) C13 0.0274(18) 0.036(2) 0.0320(19) -0.0069(17) 0.0021(16) -0.0009(16) C14 0.034(2) 0.045(2) 0.043(2) -0.0117(19) 0.0066(17) 0.0008(18) C15 0.058(3) 0.071(3) 0.044(2) -0.023(2) 0.006(2) 0.004(2) C16 0.041(2) 0.037(2) 0.069(3) -0.003(2) 0.011(2) 0.0044(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si N1 1.716(3) . ? Si N2 1.717(3) . ? Si Cl 2.0870(13) . ? Si Si 2.3700(18) 2 ? N1 C1 1.417(4) . ? N1 C7 1.476(4) . ? N2 C2 1.417(4) . ? N2 C12 1.483(4) . ? C1 C6 1.387(4) . ? C1 C2 1.406(4) . ? C2 C3 1.383(4) . ? C3 C4 1.392(4) . ? C4 C5 1.376(5) . ? C5 C6 1.386(5) . ? C7 C8 1.536(5) . ? C8 C11 1.516(5) . ? C8 C9 1.518(5) . ? C8 C10 1.532(5) . ? C12 C13 1.533(4) . ? C13 C16 1.525(5) . ? C13 C14 1.527(4) . ? C13 C15 1.536(5) . ? 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 Si N2 94.62(13) . . ? N1 Si Cl 114.18(10) . . ? N2 Si Cl 107.22(10) . . ? N1 Si Si 115.89(11) . 2 ? N2 Si Si 120.33(9) . 2 ? Cl Si Si 104.65(5) . 2 ? C1 N1 C7 120.1(2) . . ? C1 N1 Si 109.1(2) . . ? C7 N1 Si 130.2(2) . . ? C2 N2 C12 120.2(3) . . ? C2 N2 Si 109.4(2) . . ? C12 N2 Si 126.2(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 N1 126.9(3) . . ? C2 C1 N1 113.5(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 N2 126.9(3) . . ? C1 C2 N2 112.9(3) . . ? C2 C3 C4 119.7(3) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 120.8(3) . . ? C5 C6 C1 119.7(3) . . ? N1 C7 C8 118.2(3) . . ? C11 C8 C9 110.1(4) . . ? C11 C8 C10 108.7(3) . . ? C9 C8 C10 107.7(4) . . ? C11 C8 C7 112.3(3) . . ? C9 C8 C7 111.3(3) . . ? C10 C8 C7 106.6(3) . . ? N2 C12 C13 118.1(3) . . ? C16 C13 C14 109.0(3) . . ? C16 C13 C12 112.0(3) . . ? C14 C13 C12 110.0(3) . . ? C16 C13 C15 109.7(3) . . ? C14 C13 C15 109.9(3) . . ? C12 C13 C15 106.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl Si Si Cl 80.61(9) . . 2 2 ? #===END