Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2001 #========================================================== data_global #========================================================== _journal_coden_Cambridge 1145 #SUBMISSION DETAILS _publ_section_title ; Mesoscopic-scale sheet-like assembly: critical role of inter-tape hydrogen bonds in the organogel formation and gel-liquid crystal transition of an alkylsilylated deoxyguanosine/dodecane system ; _publ_requested_journal 'Journal of Materials Chemistry ' _publ_contact_author_name 'Koji Araki' _publ_contact_author_address ; Institute of Industrial Science, University of Tokyo 4-6-1 Komaba, Meguro-ku, Tokyo 153-8505, Japan ; _publ_contact_author_email 'araki@iis.u-tokyo.ac.jp' _publ_contact_author_fax '+81-3-5452-6364' loop_ _publ_author_name 'Takafumi Sato' 'Masayuki Seko' 'Ryoichi Takasawa' 'Isao Yoshikawa' 'Koji Araki' #======================================================== data_35TIPS-dG #======================================================== _database_code_CSD 153735 #CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2'-deoxy-3',5'-O-bis(triisopropylsilyl)-guanosine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H53 N5 O4 Si2' _chemical_formula_sum 'C28 H53 N5 O4 Si2' _chemical_formula_weight 579.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #CRYSTAL DATA _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'p21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.0140(4) _cell_length_b 11.2140(3) _cell_length_c 18.4050(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.716(2) _cell_angle_gamma 90.00 _cell_volume 3239.19(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 28374 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 73.11 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.7064 _exptl_absorpt_correction_T_max 0.8479 _exptl_special_details ; ? ; #EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MacScience DIPlabo' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28374 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 73.11 _reflns_number_total 8328 _reflns_number_gt 8271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MacScience Xpress' _computing_cell_refinement 'Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus' _computing_publication_material ? #REFINEMENT DATA _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^)+(0.1027P)^2^+3.1674P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.18(3) _refine_ls_number_reflns 8328 _refine_ls_number_parameters 706 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.731 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.073 #ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N1 N 0.04783(18) -0.8200(3) -0.49623(17) 0.0183(6) Uani 1 1 d . . . H1 H 0.0224(14) -0.879(3) -0.4819(8) 0.022 Uiso 1 1 calc R . . C2 C 0.1260(2) -0.8439(4) -0.4980(2) 0.0193(7) Uani 1 1 d . . . N2 N 0.15753(18) -0.9527(3) -0.47524(18) 0.0223(6) Uani 1 1 d . . . H2A H 0.2097(18) -0.9730(8) -0.47515(18) 0.027 Uiso 1 1 calc R . . H2B H 0.1270(11) -1.0071(19) -0.4597(6) 0.027 Uiso 1 1 calc R . . N3 N 0.17021(18) -0.7646(3) -0.52052(17) 0.0193(6) Uani 1 1 d . . . C4 C 0.1290(2) -0.6592(3) -0.54070(19) 0.0170(7) Uani 1 1 d . . . C5 C 0.0522(2) -0.6254(3) -0.53812(19) 0.0171(7) Uani 1 1 d . . . C6 C 0.0043(2) -0.7110(4) -0.51506(19) 0.0189(7) Uani 1 1 d . . . O6 O -0.06516(15) -0.6984(3) -0.51039(16) 0.0241(6) Uani 1 1 d . . . N7 N 0.03242(18) -0.5087(3) -0.56244(18) 0.0204(6) Uani 1 1 d . . . C8 C 0.0962(2) -0.4733(4) -0.5807(2) 0.0203(7) Uani 1 1 d . . . H8 H 0.1001 -0.3959 -0.6000 0.024 Uiso 1 1 calc . . . N9 N 0.15687(16) -0.5610(3) -0.56881(16) 0.0184(6) Uani 1 1 d . . . C10 C 0.2345(2) -0.5543(4) -0.5839(2) 0.0217(7) Uani 1 1 d . . . H10 H 0.2836 -0.5851 -0.5372 0.026 Uiso 1 1 calc . . . C11 C 0.2304(3) -0.6199(4) -0.6578(3) 0.0294(9) Uani 1 1 d . . . H11A H 0.1710 -0.6421 -0.6911 0.035 Uiso 1 1 calc . . . H11B H 0.2657 -0.6930 -0.6441 0.035 Uiso 1 1 calc . . . C12 C 0.2659(2) -0.5289(4) -0.7005(2) 0.0226(8) Uani 1 1 d . . . H12 H 0.2187 -0.4958 -0.7478 0.027 Uiso 1 1 calc . . . O13 O 0.32950(15) -0.5798(3) -0.72241(14) 0.0269(6) Uani 1 1 d . . . C14 C 0.3028(2) -0.4321(4) -0.63841(19) 0.0194(7) Uani 1 1 d . . . H14 H 0.3610 -0.4576 -0.6018 0.023 Uiso 1 1 calc . . . O15 O 0.24773(14) -0.4324(3) -0.59560(14) 0.0199(5) Uani 1 1 d . . . C16 C 0.3090(2) -0.3082(4) -0.6676(2) 0.0234(8) Uani 1 1 d . . . H16A H 0.3156 -0.2499 -0.6252 0.028 Uiso 1 1 calc . . . H16B H 0.3602 -0.3029 -0.6805 0.028 Uiso 1 1 calc . . . O17 O 0.23611(16) -0.2784(3) -0.73494(14) 0.0250(6) Uani 1 1 d . . . Si18 Si 0.33545(6) -0.58998(14) -0.81023(5) 0.0225(2) Uani 1 1 d . . . C19 C 0.3839(2) -0.7403(4) -0.8080(2) 0.0274(8) Uani 1 1 d . . . H19 H 0.3512 -0.7956 -0.7875 0.033 Uiso 1 1 calc . . . C20 C 0.4758(2) -0.7471(4) -0.7484(2) 0.0307(9) Uani 1 1 d . . . H20A H 0.4795 -0.7138 -0.6980 0.046 Uiso 1 1 calc . . . H20B H 0.5127 -0.7014 -0.7680 0.046 Uiso 1 1 calc . . . H20C H 0.4944 -0.8306 -0.7410 0.046 Uiso 1 1 calc . . . C21 C 0.3750(3) -0.7916(5) -0.8874(3) 0.0456(12) Uani 1 1 d . . . H21A H 0.3154 -0.7861 -0.9242 0.068 Uiso 1 1 calc . . . H21B H 0.3927 -0.8754 -0.8809 0.068 Uiso 1 1 calc . . . H21C H 0.4110 -0.7464 -0.9082 0.068 Uiso 1 1 calc . . . C22 C 0.4026(3) -0.4630(4) -0.8200(3) 0.0433(12) Uani 1 1 d . . . H22 H 0.3650 -0.3909 -0.8335 0.052 Uiso 1 1 calc . . . C23 C 0.4788(4) -0.4338(5) -0.7413(4) 0.0572(16) Uani 1 1 d . . . H23A H 0.4576 -0.4206 -0.6995 0.086 Uiso 1 1 calc . . . H23B H 0.5079 -0.3617 -0.7482 0.086 Uiso 1 1 calc . . . H23C H 0.5190 -0.5007 -0.7269 0.086 Uiso 1 1 calc . . . C24 C 0.4350(4) -0.4784(6) -0.8866(4) 0.0600(17) Uani 1 1 d . . . H24A H 0.3871 -0.4989 -0.9355 0.090 Uiso 1 1 calc . . . H24B H 0.4775 -0.5423 -0.8728 0.090 Uiso 1 1 calc . . . H24C H 0.4610 -0.4037 -0.8939 0.090 Uiso 1 1 calc . . . C25 C 0.2228(3) -0.5799(5) -0.8872(3) 0.0427(11) Uani 1 1 d . . . H25 H 0.1973 -0.5093 -0.8713 0.051 Uiso 1 1 calc . . . C26 C 0.1679(3) -0.6843(6) -0.8839(3) 0.0507(14) Uani 1 1 d . . . H26A H 0.1749 -0.6984 -0.8292 0.076 Uiso 1 1 calc . . . H26B H 0.1851 -0.7557 -0.9047 0.076 Uiso 1 1 calc . . . H26C H 0.1080 -0.6663 -0.9157 0.076 Uiso 1 1 calc . . . C27 C 0.2119(4) -0.5550(7) -0.9707(3) 0.0648(18) Uani 1 1 d . . . H27A H 0.2485 -0.4880 -0.9717 0.097 Uiso 1 1 calc . . . H27B H 0.1523 -0.5349 -1.0019 0.097 Uiso 1 1 calc . . . H27C H 0.2279 -0.6259 -0.9930 0.097 Uiso 1 1 calc . . . Si28 Si 0.20642(6) -0.1390 -0.76226(5) 0.0237(2) Uani 1 1 d . . . C29 C 0.1833(2) -0.0631(4) -0.6819(2) 0.0289(8) Uani 1 1 d . . . H29 H 0.2389 -0.0531 -0.6362 0.035 Uiso 1 1 calc . . . C30 C 0.1268(3) -0.1413(5) -0.6541(3) 0.0418(11) Uani 1 1 d . . . H30A H 0.1532 -0.2200 -0.6390 0.063 Uiso 1 1 calc . . . H30B H 0.0707 -0.1501 -0.6968 0.063 Uiso 1 1 calc . . . H30C H 0.1204 -0.1039 -0.6085 0.063 Uiso 1 1 calc . . . C31 C 0.1451(4) 0.0615(5) -0.7055(3) 0.0479(12) Uani 1 1 d . . . H31A H 0.1825 0.1091 -0.7235 0.072 Uiso 1 1 calc . . . H31B H 0.1397 0.1004 -0.6599 0.072 Uiso 1 1 calc . . . H31C H 0.0888 0.0548 -0.7481 0.072 Uiso 1 1 calc . . . C32 C 0.1060(3) -0.1552(5) -0.8543(2) 0.0399(11) Uani 1 1 d . . . H32 H 0.0583 -0.1556 -0.8353 0.048 Uiso 1 1 calc . . . C33 C 0.0988(4) -0.2718(5) -0.8965(3) 0.0528(14) Uani 1 1 d . . . H33A H 0.1101 -0.3375 -0.8587 0.079 Uiso 1 1 calc . . . H33B H 0.1405 -0.2740 -0.9213 0.079 Uiso 1 1 calc . . . H33C H 0.0413 -0.2801 -0.9370 0.079 Uiso 1 1 calc . . . C34 C 0.0891(3) -0.0469(5) -0.9091(3) 0.0457(12) Uani 1 1 d . . . H34A H 0.0943 0.0263 -0.8784 0.069 Uiso 1 1 calc . . . H34B H 0.0315 -0.0523 -0.9498 0.069 Uiso 1 1 calc . . . H34C H 0.1307 -0.0455 -0.9339 0.069 Uiso 1 1 calc . . . C35 C 0.2934(3) -0.0561(4) -0.7793(2) 0.0331(9) Uani 1 1 d . . . H35 H 0.2675 0.0182 -0.8089 0.040 Uiso 1 1 calc . . . C36 C 0.3674(3) -0.0172(5) -0.7028(3) 0.0425(11) Uani 1 1 d . . . H36A H 0.3446 0.0286 -0.6699 0.064 Uiso 1 1 calc . . . H36B H 0.4073 0.0326 -0.7160 0.064 Uiso 1 1 calc . . . H36C H 0.3971 -0.0879 -0.6739 0.064 Uiso 1 1 calc . . . C37 C 0.3296(3) -0.1275(6) -0.8310(3) 0.0490(13) Uani 1 1 d . . . H37A H 0.2829 -0.1526 -0.8795 0.074 Uiso 1 1 calc . . . H37B H 0.3598 -0.1980 -0.8021 0.074 Uiso 1 1 calc . . . H37C H 0.3693 -0.0772 -0.8443 0.074 Uiso 1 1 calc . . . N51 N 0.45516(17) 0.0360(3) -0.49805(16) 0.0170(6) Uani 1 1 d . . . H51 H 0.4785(16) 0.085(3) -0.5054(5) 0.020 Uiso 1 1 calc R . . C52 C 0.3804(2) 0.0624(4) -0.48972(19) 0.0181(7) Uani 1 1 d . . . N52 N 0.35474(19) 0.1765(3) -0.5003(2) 0.0242(7) Uani 1 1 d . . . H52A H 0.3059(17) 0.1974(8) -0.4966(2) 0.029 Uiso 1 1 calc R . . H52B H 0.3866(11) 0.231(2) -0.5110(4) 0.029 Uiso 1 1 calc R . . N53 N 0.33243(17) -0.0191(3) -0.47369(16) 0.0172(6) Uani 1 1 d . . . C54 C 0.3672(2) -0.1288(3) -0.46551(19) 0.0163(7) Uani 1 1 d . . . C55 C 0.4412(2) -0.1634(3) -0.47401(19) 0.0168(7) Uani 1 1 d . . . C56 C 0.4898(2) -0.0766(4) -0.49354(18) 0.0178(7) Uani 1 1 d . . . O56 O 0.55589(14) -0.0919(3) -0.50648(14) 0.0209(5) Uani 1 1 d . . . N57 N 0.45359(18) -0.2855(3) -0.46363(17) 0.0177(6) Uani 1 1 d . . . C58 C 0.3889(2) -0.3230(3) -0.4476(2) 0.0184(7) Uani 1 1 d . . . H58 H 0.3805 -0.4040 -0.4372 0.022 Uiso 1 1 calc . . . N59 N 0.33445(17) -0.2320(3) -0.44743(16) 0.0160(6) Uani 1 1 d . . . C60 C 0.25283(19) -0.2405(3) -0.43694(19) 0.0169(7) Uani 1 1 d . . . H60 H 0.2044 -0.2208 -0.4874 0.020 Uiso 1 1 calc . . . C61 C 0.2388(2) -0.3613(4) -0.4073(2) 0.0191(7) Uani 1 1 d . . . H61A H 0.1775 -0.3824 -0.4281 0.023 Uiso 1 1 calc . . . H61B H 0.2706 -0.4244 -0.4219 0.023 Uiso 1 1 calc . . . C62 C 0.2733(2) -0.3426(4) -0.3191(2) 0.0221(8) Uani 1 1 d . . . H62 H 0.3370 -0.3448 -0.2970 0.027 Uiso 1 1 calc . . . O63 O 0.24146(17) -0.4217(3) -0.27703(15) 0.0266(6) Uani 1 1 d . . . C64 C 0.2425(2) -0.2179(4) -0.3152(2) 0.0209(7) Uani 1 1 d . . . H64 H 0.1798 -0.2206 -0.3279 0.025 Uiso 1 1 calc . . . O65 O 0.25659(15) -0.1561(3) -0.37730(14) 0.0209(5) Uani 1 1 d . . . C66 C 0.2857(2) -0.1540(4) -0.2373(2) 0.0296(9) Uani 1 1 d . . . H66A H 0.3023 -0.2133 -0.1941 0.036 Uiso 1 1 calc . . . H66B H 0.3383 -0.1154 -0.2365 0.036 Uiso 1 1 calc . . . O67 O 0.23272(16) -0.0666(3) -0.22378(15) 0.0278(6) Uani 1 1 d . . . Si68 Si 0.19367(6) -0.07995(14) -0.15438(5) 0.0244(2) Uani 1 1 d . . . C69 C 0.3098(2) -0.6463(4) -0.3114(2) 0.0288(8) Uani 1 1 d . . . H69 H 0.2696 -0.6274 -0.3662 0.035 Uiso 1 1 calc . . . C70 C 0.3984(3) -0.6116(4) -0.3072(2) 0.0320(9) Uani 1 1 d . . . H70A H 0.4008 -0.5251 -0.3137 0.048 Uiso 1 1 calc . . . H70B H 0.4098 -0.6523 -0.3492 0.048 Uiso 1 1 calc . . . H70C H 0.4413 -0.6351 -0.2559 0.048 Uiso 1 1 calc . . . C71 C 0.3042(3) -0.7819(4) -0.3020(3) 0.0355(10) Uani 1 1 d . . . H71A H 0.2469 -0.8028 -0.3054 0.053 Uiso 1 1 calc . . . H71B H 0.3463 -0.8066 -0.2506 0.053 Uiso 1 1 calc . . . H71C H 0.3157 -0.8228 -0.3439 0.053 Uiso 1 1 calc . . . C72 C 0.1685(3) -0.6253(4) -0.2469(2) 0.0305(9) Uani 1 1 d . . . H72 H 0.1802 -0.7102 -0.2293 0.037 Uiso 1 1 calc . . . C73 C 0.1025(3) -0.6256(5) -0.3317(3) 0.0431(12) Uani 1 1 d . . . H73A H 0.1261 -0.6669 -0.3658 0.065 Uiso 1 1 calc . . . H73B H 0.0884 -0.5433 -0.3500 0.065 Uiso 1 1 calc . . . H73C H 0.0510 -0.6669 -0.3338 0.065 Uiso 1 1 calc . . . C74 C 0.1324(3) -0.5629(5) -0.1924(3) 0.0405(11) Uani 1 1 d . . . H74A H 0.1752 -0.5634 -0.1384 0.061 Uiso 1 1 calc . . . H74B H 0.0812 -0.6051 -0.1942 0.061 Uiso 1 1 calc . . . H74C H 0.1176 -0.4804 -0.2099 0.061 Uiso 1 1 calc . . . C75 C 0.3494(3) -0.5441(4) -0.1386(2) 0.0320(9) Uani 1 1 d . . . H75 H 0.3174 -0.5060 -0.1092 0.038 Uiso 1 1 calc . . . C76 C 0.3800(3) -0.6650(5) -0.0986(3) 0.0476(13) Uani 1 1 d . . . H76A H 0.3307 -0.7165 -0.1071 0.071 Uiso 1 1 calc . . . H76B H 0.4114 -0.6529 -0.0419 0.071 Uiso 1 1 calc . . . H76C H 0.4174 -0.7027 -0.1212 0.071 Uiso 1 1 calc . . . C77 C 0.4247(3) -0.4616(5) -0.1274(2) 0.0374(10) Uani 1 1 d . . . H77A H 0.4035 -0.3847 -0.1527 0.056 Uiso 1 1 calc . . . H77B H 0.4613 -0.4979 -0.1515 0.056 Uiso 1 1 calc . . . H77C H 0.4576 -0.4493 -0.0711 0.056 Uiso 1 1 calc . . . Si78 Si 0.27047(6) -0.55886(14) -0.24393(5) 0.0237(2) Uani 1 1 d . . . C79 C 0.1182(3) -0.2105(5) -0.1776(3) 0.0352(10) Uani 1 1 d . . . H79 H 0.1532 -0.2822 -0.1774 0.042 Uiso 1 1 calc . . . C80 C 0.0457(3) -0.2079(5) -0.2595(3) 0.0421(11) Uani 1 1 d . . . H80A H 0.0694 -0.1941 -0.2996 0.063 Uiso 1 1 calc . . . H80B H 0.0059 -0.1436 -0.2616 0.063 Uiso 1 1 calc . . . H80C H 0.0155 -0.2844 -0.2696 0.063 Uiso 1 1 calc . . . C81 C 0.0825(4) -0.2338(7) -0.1142(4) 0.0671(19) Uani 1 1 d . . . H81A H 0.1294 -0.2369 -0.0624 0.101 Uiso 1 1 calc . . . H81B H 0.0519 -0.3100 -0.1247 0.101 Uiso 1 1 calc . . . H81C H 0.0433 -0.1694 -0.1148 0.101 Uiso 1 1 calc . . . C82 C 0.1454(3) 0.0715(4) -0.1564(2) 0.0330(9) Uani 1 1 d . . . H82 H 0.1894 0.1303 -0.1568 0.040 Uiso 1 1 calc . . . C83 C 0.0665(3) 0.0962(5) -0.2312(3) 0.0417(11) Uani 1 1 d . . . H83A H 0.0791 0.0773 -0.2776 0.063 Uiso 1 1 calc . . . H83B H 0.0509 0.1805 -0.2326 0.063 Uiso 1 1 calc . . . H83C H 0.0191 0.0466 -0.2313 0.063 Uiso 1 1 calc . . . C84 C 0.1255(4) 0.1024(6) -0.0834(3) 0.0521(14) Uani 1 1 d . . . H84A H 0.1759 0.0865 -0.0354 0.078 Uiso 1 1 calc . . . H84B H 0.0778 0.0534 -0.0833 0.078 Uiso 1 1 calc . . . H84C H 0.1102 0.1869 -0.0851 0.078 Uiso 1 1 calc . . . C85 C 0.2823(3) -0.1034(5) -0.0549(2) 0.0364(10) Uani 1 1 d . . . H85 H 0.2575 -0.0827 -0.0154 0.044 Uiso 1 1 calc . . . C86 C 0.3540(3) -0.0145(6) -0.0418(3) 0.0555(15) Uani 1 1 d . . . H86A H 0.3302 0.0660 -0.0542 0.083 Uiso 1 1 calc . . . H86B H 0.3841 -0.0346 -0.0760 0.083 Uiso 1 1 calc . . . H86C H 0.3939 -0.0177 0.0134 0.083 Uiso 1 1 calc . . . C87 C 0.3167(4) -0.2311(6) -0.0349(3) 0.0555(15) Uani 1 1 d . . . H87A H 0.2691 -0.2862 -0.0442 0.083 Uiso 1 1 calc . . . H87B H 0.3556 -0.2350 0.0206 0.083 Uiso 1 1 calc . . . H87C H 0.3474 -0.2535 -0.0683 0.083 Uiso 1 1 calc . . . 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 N1 0.0174(13) 0.0152(15) 0.0268(15) 0.0031(12) 0.0135(11) 0.0012(11) C2 0.0210(16) 0.0184(19) 0.0210(16) -0.0006(14) 0.0109(13) -0.0004(14) N2 0.0199(13) 0.0169(16) 0.0367(17) 0.0083(14) 0.0181(12) 0.0034(12) N3 0.0195(13) 0.0173(16) 0.0235(14) 0.0025(12) 0.0108(11) 0.0016(12) C4 0.0180(15) 0.0141(18) 0.0202(16) -0.0002(13) 0.0088(12) -0.0009(13) C5 0.0169(14) 0.0159(18) 0.0192(15) -0.0005(13) 0.0078(12) 0.0000(13) C6 0.0196(15) 0.0203(19) 0.0189(16) -0.0015(14) 0.0098(13) -0.0009(14) O6 0.0178(11) 0.0242(15) 0.0350(14) -0.0001(11) 0.0155(10) -0.0008(10) N7 0.0204(14) 0.0187(16) 0.0232(14) 0.0023(12) 0.0097(11) 0.0014(12) C8 0.0197(16) 0.0182(19) 0.0235(17) 0.0010(14) 0.0089(13) 0.0021(14) N9 0.0160(12) 0.0197(16) 0.0219(13) 0.0023(12) 0.0102(10) -0.0011(12) C10 0.0176(15) 0.0185(19) 0.0323(18) 0.0024(15) 0.0133(13) -0.0024(14) C11 0.041(2) 0.020(2) 0.041(2) -0.0071(17) 0.0307(18) -0.0065(16) C12 0.0188(15) 0.025(2) 0.0289(18) 0.0017(16) 0.0147(14) -0.0013(14) O13 0.0220(12) 0.0397(17) 0.0238(12) 0.0008(12) 0.0143(10) 0.0073(12) C14 0.0166(15) 0.025(2) 0.0202(16) 0.0052(15) 0.0107(12) 0.0011(14) O15 0.0204(11) 0.0157(13) 0.0257(12) 0.0017(10) 0.0114(10) -0.0007(10) C16 0.0231(17) 0.027(2) 0.0201(17) 0.0050(15) 0.0078(13) -0.0051(15) O17 0.0304(13) 0.0218(14) 0.0180(11) 0.0029(11) 0.0043(10) -0.0020(11) Si18 0.0276(5) 0.0232(5) 0.0197(4) 0.0018(4) 0.0124(4) 0.0003(4) C19 0.0310(19) 0.025(2) 0.0252(18) 0.0037(16) 0.0096(15) 0.0025(16) C20 0.0275(19) 0.032(2) 0.032(2) 0.0002(17) 0.0108(16) 0.0001(17) C21 0.058(3) 0.038(3) 0.036(2) -0.007(2) 0.012(2) 0.010(2) C22 0.050(3) 0.023(2) 0.074(3) 0.007(2) 0.044(3) 0.004(2) C23 0.049(3) 0.038(3) 0.103(5) -0.020(3) 0.050(3) -0.015(2) C24 0.065(3) 0.056(4) 0.085(4) 0.030(3) 0.058(3) 0.013(3) C25 0.042(2) 0.047(3) 0.032(2) 0.007(2) 0.0061(17) 0.010(2) C26 0.035(2) 0.064(4) 0.039(2) -0.005(2) -0.0004(19) 0.001(2) C27 0.065(3) 0.091(5) 0.033(2) 0.010(3) 0.013(2) 0.025(4) Si28 0.0279(5) 0.0222(5) 0.0179(4) 0.0025(4) 0.0054(4) 0.0004(4) C29 0.0312(18) 0.027(2) 0.0245(18) -0.0018(17) 0.0067(14) 0.0003(17) C30 0.043(2) 0.051(3) 0.037(2) -0.006(2) 0.0219(19) -0.004(2) C31 0.074(3) 0.036(3) 0.037(2) 0.002(2) 0.024(2) 0.016(3) C32 0.046(2) 0.032(3) 0.031(2) 0.0036(19) 0.0019(18) 0.005(2) C33 0.058(3) 0.046(3) 0.037(3) 0.003(2) 0.000(2) -0.006(3) C34 0.052(3) 0.045(3) 0.028(2) 0.011(2) 0.0028(18) 0.004(2) C35 0.039(2) 0.029(2) 0.0308(19) 0.0101(18) 0.0129(16) 0.0047(18) C36 0.036(2) 0.037(3) 0.048(3) 0.013(2) 0.0091(19) -0.010(2) C37 0.059(3) 0.047(3) 0.050(3) 0.011(2) 0.031(2) 0.006(3) N51 0.0156(13) 0.0161(16) 0.0226(14) 0.0003(12) 0.0111(11) 0.0002(11) C52 0.0166(15) 0.0197(19) 0.0197(16) -0.0003(14) 0.0090(12) 0.0007(14) N52 0.0209(14) 0.0160(16) 0.0414(19) 0.0051(14) 0.0183(13) 0.0025(12) N53 0.0187(13) 0.0168(15) 0.0203(14) 0.0017(11) 0.0120(11) -0.0001(11) C54 0.0188(15) 0.0139(17) 0.0170(15) -0.0007(13) 0.0076(12) -0.0014(13) C55 0.0175(15) 0.0157(17) 0.0166(15) -0.0010(13) 0.0059(12) 0.0013(13) C56 0.0172(14) 0.0226(19) 0.0149(14) -0.0014(14) 0.0076(11) -0.0008(14) O56 0.0169(11) 0.0228(14) 0.0271(12) -0.0001(11) 0.0131(9) -0.0005(10) N57 0.0171(13) 0.0169(15) 0.0203(14) 0.0007(12) 0.0087(11) 0.0009(11) C58 0.0177(15) 0.0177(18) 0.0209(16) 0.0032(14) 0.0088(13) 0.0035(13) N59 0.0176(13) 0.0145(15) 0.0181(14) 0.0017(11) 0.0093(11) 0.0008(11) C60 0.0144(15) 0.0189(19) 0.0207(16) 0.0011(13) 0.0104(12) 0.0022(13) C61 0.0172(15) 0.0206(19) 0.0226(17) 0.0009(14) 0.0113(13) -0.0004(14) C62 0.0195(16) 0.025(2) 0.0260(18) 0.0090(15) 0.0132(14) -0.0003(14) O63 0.0349(14) 0.0232(15) 0.0268(13) 0.0079(11) 0.0173(11) 0.0024(11) C64 0.0237(16) 0.023(2) 0.0174(16) 0.0064(14) 0.0095(13) 0.0018(14) O65 0.0275(12) 0.0192(14) 0.0217(11) -0.0015(10) 0.0159(10) -0.0026(10) C66 0.0268(18) 0.037(2) 0.0249(18) -0.0017(18) 0.0097(15) 0.0048(17) O67 0.0352(14) 0.0266(16) 0.0262(12) -0.0027(12) 0.0171(11) 0.0014(12) Si68 0.0289(5) 0.0275(6) 0.0186(4) -0.0021(4) 0.0112(4) -0.0024(4) C69 0.0308(19) 0.026(2) 0.0290(19) 0.0018(17) 0.0108(15) -0.0014(17) C70 0.0318(19) 0.030(2) 0.038(2) 0.0053(18) 0.0182(17) 0.0035(17) C71 0.039(2) 0.028(2) 0.039(2) -0.0011(19) 0.0149(18) 0.0036(19) C72 0.035(2) 0.032(2) 0.0272(18) 0.0080(17) 0.0141(15) -0.0004(17) C73 0.031(2) 0.062(3) 0.033(2) -0.004(2) 0.0083(17) -0.013(2) C74 0.045(2) 0.049(3) 0.036(2) -0.006(2) 0.0261(18) -0.011(2) C75 0.0328(19) 0.036(3) 0.0229(18) 0.0031(18) 0.0060(15) -0.0013(18) C76 0.058(3) 0.043(3) 0.028(2) 0.011(2) 0.000(2) -0.001(2) C77 0.034(2) 0.045(3) 0.028(2) 0.000(2) 0.0060(16) -0.002(2) Si78 0.0267(5) 0.0246(6) 0.0199(4) 0.0052(4) 0.0089(3) -0.0008(4) C79 0.040(2) 0.034(3) 0.036(2) -0.0042(19) 0.0189(19) -0.0076(19) C80 0.037(2) 0.041(3) 0.049(3) -0.008(2) 0.017(2) -0.010(2) C81 0.082(4) 0.076(5) 0.062(4) -0.008(3) 0.048(3) -0.040(4) C82 0.039(2) 0.032(2) 0.0280(19) -0.0036(18) 0.0128(17) -0.0014(18) C83 0.042(2) 0.038(3) 0.041(2) -0.002(2) 0.012(2) 0.005(2) C84 0.074(4) 0.051(3) 0.036(3) -0.001(2) 0.027(2) 0.017(3) C85 0.043(2) 0.042(3) 0.0221(18) -0.0053(18) 0.0104(16) 0.002(2) C86 0.041(3) 0.076(4) 0.036(2) -0.014(3) 0.000(2) -0.011(3) C87 0.074(4) 0.056(4) 0.026(2) 0.008(2) 0.008(2) 0.029(3) #MOLECULAR GEOMETRY 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 N1 C2 1.369(4) . ? N1 C6 1.402(5) . ? C2 N3 1.331(5) . ? C2 N2 1.333(5) . ? N3 C4 1.351(5) . ? C4 N9 1.376(5) . ? C4 C5 1.379(5) . ? C5 N7 1.383(5) . ? C5 C6 1.426(5) . ? C6 O6 1.226(4) . ? N7 C8 1.316(5) . ? C8 N9 1.380(5) . ? N9 C10 1.454(4) . ? C10 O15 1.415(5) . ? C10 C11 1.524(5) . ? C11 C12 1.546(5) . ? C12 O13 1.413(4) . ? C12 C14 1.525(5) . ? O13 Si18 1.662(2) . ? C14 O15 1.439(4) . ? C14 C16 1.508(5) . ? C16 O17 1.414(4) . ? O17 Si28 1.660(3) . ? Si18 C19 1.870(4) . ? Si18 C22 1.877(5) . ? Si18 C25 1.896(4) . ? C19 C21 1.524(6) . ? C19 C20 1.526(5) . ? C22 C24 1.536(7) . ? C22 C23 1.561(8) . ? C25 C27 1.502(7) . ? C25 C26 1.514(8) . ? Si28 C35 1.874(5) . ? Si28 C29 1.875(4) . ? Si28 C32 1.894(4) . ? C29 C30 1.527(6) . ? C29 C31 1.531(6) . ? C32 C33 1.502(8) . ? C32 C34 1.532(7) . ? C35 C37 1.543(7) . ? C35 C36 1.546(6) . ? N51 C52 1.371(4) . ? N51 C56 1.382(5) . ? C52 N53 1.331(5) . ? C52 N52 1.342(5) . ? N53 C54 1.348(5) . ? C54 N59 1.379(5) . ? C54 C55 1.384(5) . ? C55 N57 1.387(5) . ? C55 C56 1.410(5) . ? C56 O56 1.248(4) . ? N57 C58 1.314(5) . ? C58 N59 1.380(5) . ? N59 C60 1.477(4) . ? C60 O65 1.431(4) . ? C60 C61 1.514(5) . ? C61 C62 1.512(5) . ? C62 O63 1.416(4) . ? C62 C64 1.506(6) . ? O63 Si78 1.657(3) . ? C64 O65 1.434(4) . ? C64 C66 1.515(5) . ? C66 O67 1.418(5) . ? O67 Si68 1.658(3) . ? Si68 C82 1.880(5) . ? Si68 C79 1.885(5) . ? Si68 C85 1.887(4) . ? C69 C70 1.528(5) . ? C69 C71 1.538(6) . ? C69 Si78 1.896(4) . ? C72 C74 1.532(6) . ? C72 C73 1.532(6) . ? C72 Si78 1.869(4) . ? C75 C77 1.529(6) . ? C75 C76 1.534(6) . ? C75 Si78 1.892(4) . ? C79 C81 1.533(7) . ? C79 C80 1.535(6) . ? C82 C83 1.531(6) . ? C82 C84 1.547(6) . ? C85 C86 1.520(8) . ? C85 C87 1.537(7) . ? 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 C2 N1 C6 126.2(3) . . ? N3 C2 N2 120.1(3) . . ? N3 C2 N1 123.2(3) . . ? N2 C2 N1 116.7(3) . . ? C2 N3 C4 112.0(3) . . ? N3 C4 N9 125.9(3) . . ? N3 C4 C5 129.0(3) . . ? N9 C4 C5 105.2(3) . . ? C4 C5 N7 111.4(3) . . ? C4 C5 C6 118.9(3) . . ? N7 C5 C6 129.6(3) . . ? O6 C6 N1 121.0(3) . . ? O6 C6 C5 128.4(4) . . ? N1 C6 C5 110.6(3) . . ? C8 N7 C5 104.2(3) . . ? N7 C8 N9 112.6(3) . . ? C4 N9 C8 106.6(3) . . ? C4 N9 C10 125.7(3) . . ? C8 N9 C10 127.7(3) . . ? O15 C10 N9 106.8(3) . . ? O15 C10 C11 106.7(3) . . ? N9 C10 C11 114.4(3) . . ? C10 C11 C12 104.0(3) . . ? O13 C12 C14 111.2(3) . . ? O13 C12 C11 111.8(3) . . ? C14 C12 C11 102.6(3) . . ? C12 O13 Si18 130.2(2) . . ? O15 C14 C16 110.3(3) . . ? O15 C14 C12 104.0(3) . . ? C16 C14 C12 117.0(3) . . ? C10 O15 C14 105.1(3) . . ? O17 C16 C14 111.8(3) . . ? C16 O17 Si28 123.3(2) . . ? O13 Si18 C19 103.41(17) . . ? O13 Si18 C22 108.0(2) . . ? C19 Si18 C22 114.0(2) . . ? O13 Si18 C25 107.40(17) . . ? C19 Si18 C25 112.3(2) . . ? C22 Si18 C25 111.1(2) . . ? C21 C19 C20 111.4(4) . . ? C21 C19 Si18 116.1(3) . . ? C20 C19 Si18 112.5(3) . . ? C24 C22 C23 109.7(4) . . ? C24 C22 Si18 114.2(4) . . ? C23 C22 Si18 112.9(4) . . ? C27 C25 C26 110.5(5) . . ? C27 C25 Si18 117.8(4) . . ? C26 C25 Si18 112.7(3) . . ? O17 Si28 C35 110.49(17) . . ? O17 Si28 C29 108.68(17) . . ? C35 Si28 C29 109.1(2) . . ? O17 Si28 C32 104.16(18) . . ? C35 Si28 C32 113.3(2) . . ? C29 Si28 C32 110.9(2) . . ? C30 C29 C31 111.5(4) . . ? C30 C29 Si28 110.8(3) . . ? C31 C29 Si28 112.7(3) . . ? C33 C32 C34 113.2(4) . . ? C33 C32 Si28 114.3(3) . . ? C34 C32 Si28 112.8(3) . . ? C37 C35 C36 109.3(4) . . ? C37 C35 Si28 112.1(4) . . ? C36 C35 Si28 113.9(3) . . ? C52 N51 C56 125.7(3) . . ? N53 C52 N52 119.6(3) . . ? N53 C52 N51 123.4(3) . . ? N52 C52 N51 117.0(3) . . ? C52 N53 C54 111.8(3) . . ? N53 C54 N59 126.3(3) . . ? N53 C54 C55 128.4(3) . . ? N59 C54 C55 105.2(3) . . ? C54 C55 N57 110.9(3) . . ? C54 C55 C56 119.0(3) . . ? N57 C55 C56 130.1(3) . . ? O56 C56 N51 120.6(3) . . ? O56 C56 C55 127.8(4) . . ? N51 C56 C55 111.6(3) . . ? C58 N57 C55 104.6(3) . . ? N57 C58 N59 112.6(3) . . ? C54 N59 C58 106.7(3) . . ? C54 N59 C60 125.0(3) . . ? C58 N59 C60 128.2(3) . . ? O65 C60 N59 107.0(3) . . ? O65 C60 C61 106.3(3) . . ? N59 C60 C61 113.1(3) . . ? C62 C61 C60 102.3(3) . . ? O63 C62 C64 110.0(3) . . ? O63 C62 C61 115.4(3) . . ? C64 C62 C61 100.5(3) . . ? C62 O63 Si78 131.3(2) . . ? O65 C64 C62 104.0(3) . . ? O65 C64 C66 110.9(3) . . ? C62 C64 C66 115.7(3) . . ? C60 O65 C64 108.7(3) . . ? O67 C66 C64 112.5(3) . . ? C66 O67 Si68 122.9(3) . . ? O67 Si68 C82 101.84(18) . . ? O67 Si68 C79 109.62(17) . . ? C82 Si68 C79 116.3(2) . . ? O67 Si68 C85 110.57(17) . . ? C82 Si68 C85 108.9(2) . . ? C79 Si68 C85 109.4(2) . . ? C70 C69 C71 110.5(4) . . ? C70 C69 Si78 115.2(3) . . ? C71 C69 Si78 112.6(3) . . ? C74 C72 C73 110.3(4) . . ? C74 C72 Si78 113.7(3) . . ? C73 C72 Si78 109.7(3) . . ? C77 C75 C76 111.0(4) . . ? C77 C75 Si78 114.6(3) . . ? C76 C75 Si78 112.9(3) . . ? O63 Si78 C72 102.59(17) . . ? O63 Si78 C75 106.77(18) . . ? C72 Si78 C75 110.36(18) . . ? O63 Si78 C69 111.69(17) . . ? C72 Si78 C69 109.5(2) . . ? C75 Si78 C69 115.21(19) . . ? C81 C79 C80 110.3(4) . . ? C81 C79 Si68 113.3(4) . . ? C80 C79 Si68 115.3(3) . . ? C83 C82 C84 109.3(4) . . ? C83 C82 Si68 113.9(3) . . ? C84 C82 Si68 115.2(3) . . ? C86 C85 C87 111.4(5) . . ? C86 C85 Si68 110.8(3) . . ? C87 C85 Si68 116.8(3) . . ? #======================================================== data_TBDPS-dG _database_code_CSD 153736 #======================================================== #CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2'-deoxy-3',5'-O-bis(tert-butyldiphenylsilyl)-guanosine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H49 N5 O4 Si2' _chemical_formula_sum 'C42 H49 N5 O4 Si2' _chemical_formula_weight 744.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #CRYSTAL DATA _symmetry_cell_setting 'orthorhombic' _symmetry_space_groupe_name_H-M 'p212121' 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 9.5300(1) _cell_length_b 11.0750(1) _cell_length_c 39.4220(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4160.79(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 40833 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 73.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.8179 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; #EXPERIMENTAL DATA _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mac Science DIP-Lab' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7002 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 73.25 _reflns_number_total 7002 _reflns_number_gt 6926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MacScience Xpress' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus' _computing_publication_material ? #REFINEMRNT DATA _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^)+(0.1145P)^2^+4.1631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(4) _refine_ls_number_reflns 7002 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.959 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.078 #ATOMIC COORDINATESAND THERMAL PARAMETERS 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 N1 N 1.4577(4) -0.2696(3) 0.73227(7) 0.0385(7) Uani 1 1 d . . . H1 H 1.4846(18) -0.320(3) 0.7426(7) 0.046 Uiso 1 1 calc R . . C2 C 1.3937(4) -0.2979(3) 0.70257(9) 0.0391(8) Uani 1 1 d . . . N2 N 1.3837(4) -0.4152(3) 0.69486(8) 0.0446(8) Uani 1 1 d . . . H2A H 1.3438(15) -0.4380(9) 0.6753(7) 0.054 Uiso 1 1 calc R . . H2B H 1.4169(13) -0.471(2) 0.7093(5) 0.054 Uiso 1 1 calc R . . N3 N 1.3442(4) -0.2172(3) 0.68105(7) 0.0377(7) Uani 1 1 d . . . C4 C 1.3622(4) -0.1032(3) 0.69267(8) 0.0352(8) Uani 1 1 d . . . C5 C 1.4220(5) -0.0656(3) 0.72262(9) 0.0390(8) Uani 1 1 d . . . C6 C 1.4770(4) -0.1539(3) 0.74493(8) 0.0364(8) Uani 1 1 d . . . O6 O 1.5385(3) -0.1377(2) 0.77240(6) 0.0441(7) Uani 1 1 d . . . N7 N 1.4221(4) 0.0587(3) 0.72452(8) 0.0403(7) Uani 1 1 d . . . C8 C 1.3630(5) 0.0958(3) 0.69617(9) 0.0396(8) Uani 1 1 d . . . H8 H 1.3482 0.1781 0.6904 0.047 Uiso 1 1 calc . . . N9 N 1.3251(4) -0.0015(3) 0.67572(7) 0.0370(7) Uani 1 1 d . . . C10 C 1.2551(4) 0.0012(3) 0.64286(8) 0.0379(8) Uani 1 1 d . . . H10 H 1.3016 -0.0585 0.6275 0.045 Uiso 1 1 calc . . . C11 C 1.1002(4) -0.0265(3) 0.64432(9) 0.0388(8) Uani 1 1 d . . . H11A H 1.0560 0.0079 0.6649 0.047 Uiso 1 1 calc . . . H11B H 1.0822 -0.1145 0.6435 0.047 Uiso 1 1 calc . . . C12 C 1.0499(4) 0.0364(3) 0.61234(8) 0.0373(8) Uani 1 1 d . . . H12 H 0.9469 0.0533 0.6127 0.045 Uiso 1 1 calc . . . O13 O 1.0917(3) -0.0329(3) 0.58360(7) 0.0494(7) Uani 1 1 d . . . C14 C 1.1383(4) 0.1512(4) 0.61309(8) 0.0368(8) Uani 1 1 d . . . H14 H 1.1555 0.1797 0.5894 0.044 Uiso 1 1 calc . . . O15 O 1.2698(3) 0.1181(3) 0.62870(6) 0.0386(6) Uani 1 1 d . . . C16 C 1.0753(5) 0.2519(4) 0.63369(9) 0.0451(9) Uani 1 1 d . . . H16A H 1.0612 0.2247 0.6574 0.054 Uiso 1 1 calc . . . H16B H 1.1401 0.3218 0.6340 0.054 Uiso 1 1 calc . . . O17 O 0.9454(3) 0.2867(3) 0.61947(6) 0.0444(7) Uani 1 1 d . . . Si18 Si 1.00193(12) -0.12476(11) 0.55885(2) 0.0429(3) Uani 1 1 d . . . C19 C 0.8183(6) -0.1419(5) 0.57551(13) 0.0603(12) Uani 1 1 d . . . C20 C 0.8028(6) -0.2130(6) 0.60544(12) 0.0658(14) Uani 1 1 d . . . H20 H 0.8848 -0.2478 0.6151 0.079 Uiso 1 1 calc . . . C21 C 0.6775(7) -0.2341(6) 0.62105(13) 0.0712(14) Uani 1 1 d . . . H21 H 0.6699 -0.2833 0.6407 0.085 Uiso 1 1 calc . . . C22 C 0.5639(6) -0.1799(6) 0.60659(13) 0.0675(14) Uani 1 1 d . . . H22 H 0.4771 -0.1910 0.6180 0.081 Uiso 1 1 calc . . . C23 C 0.5593(7) -0.1131(6) 0.57841(14) 0.0720(15) Uani 1 1 d . . . H23 H 0.4753 -0.0803 0.5693 0.086 Uiso 1 1 calc . . . C24 C 0.6988(7) -0.0961(5) 0.56305(13) 0.0704(15) Uani 1 1 d . . . H24 H 0.7044 -0.0494 0.5429 0.084 Uiso 1 1 calc . . . C25 C 1.0821(5) -0.2788(4) 0.56392(9) 0.0462(9) Uani 1 1 d . . . C26 C 1.2000(5) -0.2960(4) 0.58288(10) 0.0500(10) Uani 1 1 d . . . H26 H 1.2424 -0.2283 0.5935 0.060 Uiso 1 1 calc . . . C27 C 1.2600(6) -0.4088(5) 0.58713(11) 0.0561(11) Uani 1 1 d . . . H27 H 1.3427 -0.4169 0.6004 0.067 Uiso 1 1 calc . . . C28 C 1.2013(6) -0.5094(4) 0.57230(13) 0.0608(12) Uani 1 1 d . . . H28 H 1.2428 -0.5868 0.5747 0.073 Uiso 1 1 calc . . . C29 C 1.0798(7) -0.4934(5) 0.55383(16) 0.0744(16) Uani 1 1 d . . . H29 H 1.0362 -0.5618 0.5438 0.089 Uiso 1 1 calc . . . C30 C 1.0190(7) -0.3801(5) 0.54943(14) 0.0703(15) Uani 1 1 d . . . H30 H 0.9351 -0.3718 0.5366 0.084 Uiso 1 1 calc . . . C31 C 1.0311(6) -0.0632(5) 0.51486(10) 0.0568(12) Uani 1 1 d . . . C32 C 0.9548(8) -0.1438(5) 0.48810(11) 0.0756(18) Uani 1 1 d . . . H32A H 0.8535 -0.1422 0.4924 0.113 Uiso 1 1 calc . . . H32B H 0.9891 -0.2269 0.4899 0.113 Uiso 1 1 calc . . . H32C H 0.9738 -0.1127 0.4653 0.113 Uiso 1 1 calc . . . C33 C 1.1896(7) -0.0638(6) 0.50859(13) 0.0744(16) Uani 1 1 d . . . H33A H 1.2250 -0.1467 0.5102 0.112 Uiso 1 1 calc . . . H33B H 1.2361 -0.0135 0.5257 0.112 Uiso 1 1 calc . . . H33C H 1.2092 -0.0316 0.4859 0.112 Uiso 1 1 calc . . . C34 C 0.9776(9) 0.0669(6) 0.51223(17) 0.090(2) Uani 1 1 d . . . H34A H 0.8762 0.0684 0.5163 0.136 Uiso 1 1 calc . . . H34B H 0.9974 0.0984 0.4895 0.136 Uiso 1 1 calc . . . H34C H 1.0250 0.1170 0.5292 0.136 Uiso 1 1 calc . . . Si35 Si 0.80942(13) 0.32185(10) 0.64379(2) 0.0409(3) Uani 1 1 d . . . C36 C 0.7899(5) 0.1970(4) 0.67592(9) 0.0422(9) Uani 1 1 d . . . C37 C 0.7411(5) 0.0820(4) 0.66639(9) 0.0449(9) Uani 1 1 d . . . H37 H 0.7070 0.0699 0.6440 0.054 Uiso 1 1 calc . . . C38 C 0.7417(5) -0.0128(4) 0.68868(11) 0.0497(10) Uani 1 1 d . . . H38 H 0.7087 -0.0897 0.6816 0.060 Uiso 1 1 calc . . . C39 C 0.7900(5) 0.0027(4) 0.72147(11) 0.0499(10) Uani 1 1 d . . . H39 H 0.7888 -0.0627 0.7371 0.060 Uiso 1 1 calc . . . C40 C 0.8398(5) 0.1140(4) 0.73124(10) 0.0524(11) Uani 1 1 d . . . H40 H 0.8755 0.1248 0.7535 0.063 Uiso 1 1 calc . . . C41 C 0.8383(5) 0.2102(4) 0.70887(10) 0.0474(10) Uani 1 1 d . . . H41 H 0.8710 0.2869 0.7162 0.057 Uiso 1 1 calc . . . C42 C 0.8536(5) 0.4664(4) 0.66596(9) 0.0416(9) Uani 1 1 d . . . C43 C 0.7756(5) 0.5136(4) 0.69360(10) 0.0430(9) Uani 1 1 d . . . H43 H 0.6965 0.4706 0.7019 0.052 Uiso 1 1 calc . . . C44 C 0.8138(5) 0.6216(4) 0.70854(10) 0.0513(10) Uani 1 1 d . . . H44 H 0.7601 0.6527 0.7269 0.062 Uiso 1 1 calc . . . C45 C 0.9302(6) 0.6850(4) 0.69696(11) 0.0531(11) Uani 1 1 d . . . H45 H 0.9568 0.7585 0.7076 0.064 Uiso 1 1 calc . . . C46 C 1.0067(5) 0.6416(4) 0.67012(11) 0.0493(10) Uani 1 1 d . . . H46 H 1.0860 0.6851 0.6622 0.059 Uiso 1 1 calc . . . C47 C 0.9680(5) 0.5335(4) 0.65450(10) 0.0460(10) Uani 1 1 d . . . H47 H 1.0206 0.5051 0.6357 0.055 Uiso 1 1 calc . . . C48 C 0.6554(5) 0.3418(4) 0.61375(9) 0.0470(10) Uani 1 1 d . . . C49 C 0.5260(6) 0.3671(6) 0.63404(12) 0.0651(14) Uani 1 1 d . . . H49A H 0.5064 0.2985 0.6490 0.098 Uiso 1 1 calc . . . H49B H 0.4464 0.3794 0.6187 0.098 Uiso 1 1 calc . . . H49C H 0.5403 0.4399 0.6477 0.098 Uiso 1 1 calc . . . C50 C 0.6306(8) 0.2301(7) 0.59193(16) 0.099(3) Uani 1 1 d . . . H50A H 0.7151 0.2128 0.5786 0.148 Uiso 1 1 calc . . . H50B H 0.5515 0.2447 0.5766 0.148 Uiso 1 1 calc . . . H50C H 0.6093 0.1610 0.6066 0.148 Uiso 1 1 calc . . . C51 C 0.6889(7) 0.4458(6) 0.59007(14) 0.0801(19) Uani 1 1 d . . . H51A H 0.7735 0.4268 0.5770 0.120 Uiso 1 1 calc . . . H51B H 0.7049 0.5193 0.6034 0.120 Uiso 1 1 calc . . . H51C H 0.6100 0.4587 0.5745 0.120 Uiso 1 1 calc . . . 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 N1 0.050(2) 0.0321(15) 0.0333(14) 0.0017(11) -0.0050(12) 0.0003(14) C2 0.043(2) 0.0369(19) 0.0372(17) 0.0009(14) -0.0026(15) 0.0000(17) N2 0.062(2) 0.0333(16) 0.0387(15) -0.0020(12) -0.0107(15) 0.0022(16) N3 0.046(2) 0.0328(15) 0.0346(14) -0.0016(11) -0.0069(12) -0.0001(14) C4 0.038(2) 0.0342(18) 0.0339(16) -0.0014(13) -0.0014(13) 0.0003(16) C5 0.049(2) 0.0338(18) 0.0344(17) -0.0005(14) -0.0020(15) 0.0015(17) C6 0.042(2) 0.0352(18) 0.0321(16) -0.0007(13) -0.0037(14) 0.0022(16) O6 0.0560(19) 0.0377(14) 0.0388(12) -0.0007(10) -0.0120(11) -0.0005(13) N7 0.051(2) 0.0329(15) 0.0364(15) 0.0011(12) -0.0103(14) -0.0002(15) C8 0.049(2) 0.0356(18) 0.0343(16) -0.0002(14) -0.0042(15) -0.0007(17) N9 0.0413(19) 0.0377(16) 0.0319(13) -0.0009(11) -0.0045(12) -0.0024(14) C10 0.044(2) 0.0384(18) 0.0309(15) -0.0003(14) -0.0034(14) -0.0007(16) C11 0.042(2) 0.0377(18) 0.0369(17) 0.0011(14) -0.0011(15) -0.0031(17) C12 0.041(2) 0.0409(19) 0.0298(15) -0.0031(13) 0.0001(14) -0.0062(16) O13 0.0426(17) 0.0687(19) 0.0370(13) -0.0136(12) 0.0050(12) -0.0064(15) C14 0.0342(19) 0.048(2) 0.0281(15) 0.0077(14) -0.0029(13) -0.0028(16) O15 0.0348(14) 0.0474(15) 0.0336(11) 0.0071(10) -0.0028(10) -0.0028(12) C16 0.048(2) 0.051(2) 0.0358(17) 0.0032(16) -0.0085(15) 0.001(2) O17 0.0429(16) 0.0513(16) 0.0389(13) 0.0076(11) -0.0072(11) 0.0023(13) Si18 0.0368(6) 0.0594(7) 0.0326(5) -0.0057(4) -0.0013(4) -0.0011(5) C19 0.050(3) 0.059(3) 0.072(3) -0.025(2) -0.007(2) 0.002(2) C20 0.054(3) 0.088(4) 0.055(3) -0.002(2) 0.006(2) -0.011(3) C21 0.072(4) 0.081(4) 0.061(3) -0.002(3) 0.007(3) 0.001(3) C22 0.059(3) 0.080(4) 0.063(3) -0.024(3) -0.006(2) 0.018(3) C23 0.069(4) 0.085(4) 0.063(3) -0.010(3) 0.008(2) -0.024(3) C24 0.089(4) 0.057(3) 0.065(3) 0.001(2) 0.000(3) 0.011(3) C25 0.045(2) 0.060(3) 0.0344(17) 0.0028(16) 0.0005(15) -0.009(2) C26 0.042(2) 0.060(3) 0.048(2) -0.0042(18) -0.0013(17) -0.005(2) C27 0.055(3) 0.064(3) 0.050(2) 0.006(2) 0.0005(19) 0.003(2) C28 0.065(3) 0.046(2) 0.071(3) 0.014(2) 0.008(2) -0.004(2) C29 0.078(4) 0.047(3) 0.098(4) 0.002(3) -0.027(3) -0.013(3) C30 0.076(4) 0.059(3) 0.076(3) -0.001(2) -0.027(3) -0.013(3) C31 0.061(3) 0.067(3) 0.043(2) 0.0068(19) -0.0059(19) 0.017(2) C32 0.119(5) 0.075(4) 0.033(2) -0.002(2) -0.014(2) 0.012(4) C33 0.079(4) 0.090(4) 0.055(3) 0.025(3) 0.022(3) 0.016(3) C34 0.110(6) 0.060(3) 0.101(4) 0.017(3) -0.042(4) 0.016(4) Si35 0.0444(6) 0.0420(5) 0.0364(5) 0.0069(4) -0.0041(4) -0.0024(5) C36 0.041(2) 0.043(2) 0.0421(19) 0.0026(15) -0.0018(15) -0.0041(18) C37 0.046(2) 0.050(2) 0.0391(18) 0.0011(16) 0.0055(16) -0.0052(19) C38 0.054(3) 0.046(2) 0.050(2) -0.0028(17) 0.0119(18) -0.012(2) C39 0.055(3) 0.043(2) 0.051(2) 0.0123(17) 0.0073(19) 0.001(2) C40 0.060(3) 0.057(3) 0.0402(19) 0.0125(18) -0.0062(18) -0.003(2) C41 0.054(3) 0.044(2) 0.045(2) 0.0050(16) -0.0027(17) -0.007(2) C42 0.045(2) 0.042(2) 0.0380(17) 0.0084(14) -0.0062(15) -0.0001(18) C43 0.041(2) 0.043(2) 0.0453(19) 0.0073(16) 0.0010(16) 0.0003(18) C44 0.055(3) 0.053(2) 0.045(2) 0.0012(17) -0.0043(18) 0.000(2) C45 0.064(3) 0.050(2) 0.046(2) 0.0019(18) -0.0178(19) -0.007(2) C46 0.048(3) 0.047(2) 0.053(2) 0.0105(17) -0.0083(18) -0.008(2) C47 0.047(3) 0.047(2) 0.0435(19) 0.0098(16) -0.0005(16) -0.0035(19) C48 0.047(2) 0.057(2) 0.0370(18) 0.0076(17) -0.0053(16) 0.002(2) C49 0.050(3) 0.096(4) 0.050(2) 0.010(2) -0.0045(19) -0.001(3) C50 0.107(5) 0.103(5) 0.087(4) -0.042(4) -0.056(4) 0.035(4) C51 0.068(4) 0.096(4) 0.077(3) 0.048(3) -0.029(3) -0.024(3) #MOLECULAR GEOMETRY 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 N1 C2 1.357(5) . ? N1 C6 1.387(5) . ? C2 N3 1.320(5) . ? C2 N2 1.337(5) . ? N3 C4 1.354(5) . ? C4 N9 1.357(5) . ? C4 C5 1.376(5) . ? C5 N7 1.379(5) . ? C5 C6 1.416(5) . ? C6 O6 1.244(4) . ? N7 C8 1.317(5) . ? C8 N9 1.393(5) . ? N9 C10 1.458(4) . ? C10 O15 1.417(5) . ? C10 C11 1.509(6) . ? C11 C12 1.518(5) . ? C12 O13 1.425(4) . ? C12 C14 1.525(5) . ? O13 Si18 1.649(3) . ? C14 O15 1.444(4) . ? C14 C16 1.505(6) . ? C16 O17 1.413(5) . ? O17 Si35 1.658(3) . ? Si18 C19 1.879(6) . ? Si18 C25 1.880(5) . ? Si18 C31 1.884(4) . ? C19 C24 1.340(8) . ? C19 C20 1.426(8) . ? C20 C21 1.364(8) . ? C21 C22 1.363(8) . ? C22 C23 1.335(8) . ? C23 C24 1.473(9) . ? C25 C26 1.362(6) . ? C25 C30 1.395(7) . ? C26 C27 1.384(7) . ? C27 C28 1.377(7) . ? C28 C29 1.379(8) . ? C29 C30 1.393(8) . ? C31 C33 1.530(8) . ? C31 C34 1.531(8) . ? C31 C32 1.561(7) . ? Si35 C42 1.872(4) . ? Si35 C36 1.885(4) . ? Si35 C48 1.899(4) . ? C36 C41 1.386(5) . ? C36 C37 1.407(6) . ? C37 C38 1.369(6) . ? C38 C39 1.383(6) . ? C39 C40 1.375(7) . ? C40 C41 1.383(6) . ? C42 C47 1.394(6) . ? C42 C43 1.419(6) . ? C43 C44 1.382(6) . ? C44 C45 1.391(7) . ? C45 C46 1.372(7) . ? C46 C47 1.396(6) . ? C48 C49 1.497(7) . ? C48 C51 1.517(6) . ? C48 C50 1.525(7) . ? 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 C2 N1 C6 125.7(3) . . ? N3 C2 N2 119.1(3) . . ? N3 C2 N1 123.9(4) . . ? N2 C2 N1 116.9(3) . . ? C2 N3 C4 111.7(3) . . ? N3 C4 N9 125.1(3) . . ? N3 C4 C5 128.6(3) . . ? N9 C4 C5 106.2(3) . . ? C4 C5 N7 110.4(3) . . ? C4 C5 C6 118.6(3) . . ? N7 C5 C6 131.0(3) . . ? O6 C6 N1 120.6(3) . . ? O6 C6 C5 128.0(3) . . ? N1 C6 C5 111.4(3) . . ? C8 N7 C5 105.4(3) . . ? N7 C8 N9 111.1(3) . . ? C4 N9 C8 106.8(3) . . ? C4 N9 C10 125.0(3) . . ? C8 N9 C10 128.1(3) . . ? O15 C10 N9 108.9(3) . . ? O15 C10 C11 107.3(3) . . ? N9 C10 C11 114.2(3) . . ? C10 C11 C12 100.6(3) . . ? O13 C12 C11 109.0(3) . . ? O13 C12 C14 108.1(3) . . ? C11 C12 C14 101.1(3) . . ? C12 O13 Si18 131.1(3) . . ? O15 C14 C16 107.7(3) . . ? O15 C14 C12 106.0(3) . . ? C16 C14 C12 114.1(3) . . ? C10 O15 C14 108.3(3) . . ? O17 C16 C14 109.7(3) . . ? C16 O17 Si35 121.3(2) . . ? O13 Si18 C19 109.81(18) . . ? O13 Si18 C25 106.62(18) . . ? C19 Si18 C25 104.5(2) . . ? O13 Si18 C31 104.2(2) . . ? C19 Si18 C31 119.7(2) . . ? C25 Si18 C31 111.5(2) . . ? C24 C19 C20 115.1(5) . . ? C24 C19 Si18 128.7(5) . . ? C20 C19 Si18 116.2(4) . . ? C21 C20 C19 123.9(5) . . ? C22 C21 C20 115.6(5) . . ? C23 C22 C21 128.2(6) . . ? C22 C23 C24 112.5(6) . . ? C19 C24 C23 124.6(5) . . ? C26 C25 C30 117.9(5) . . ? C26 C25 Si18 121.4(3) . . ? C30 C25 Si18 120.7(4) . . ? C25 C26 C27 122.3(4) . . ? C28 C27 C26 120.7(5) . . ? C27 C28 C29 117.5(5) . . ? C28 C29 C30 122.0(5) . . ? C29 C30 C25 119.6(5) . . ? C33 C31 C34 108.8(5) . . ? C33 C31 C32 110.4(5) . . ? C34 C31 C32 109.7(4) . . ? C33 C31 Si18 107.0(3) . . ? C34 C31 Si18 110.7(4) . . ? C32 C31 Si18 110.3(4) . . ? O17 Si35 C42 107.14(18) . . ? O17 Si35 C36 107.07(17) . . ? C42 Si35 C36 109.63(17) . . ? O17 Si35 C48 105.72(16) . . ? C42 Si35 C48 111.45(19) . . ? C36 Si35 C48 115.4(2) . . ? C41 C36 C37 117.1(4) . . ? C41 C36 Si35 121.3(3) . . ? C37 C36 Si35 121.2(3) . . ? C38 C37 C36 121.4(4) . . ? C37 C38 C39 120.4(4) . . ? C40 C39 C38 119.2(4) . . ? C39 C40 C41 120.6(4) . . ? C40 C41 C36 121.3(4) . . ? C47 C42 C43 117.5(4) . . ? C47 C42 Si35 118.7(3) . . ? C43 C42 Si35 123.8(3) . . ? C44 C43 C42 120.5(4) . . ? C43 C44 C45 120.5(4) . . ? C46 C45 C44 120.0(4) . . ? C45 C46 C47 120.0(4) . . ? C42 C47 C46 121.4(4) . . ? C49 C48 C51 111.1(5) . . ? C49 C48 C50 109.0(5) . . ? C51 C48 C50 107.6(5) . . ? C49 C48 Si35 109.0(3) . . ? C51 C48 Si35 108.0(3) . . ? C50 C48 Si35 112.1(3) . . ?