# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof Richard Laine' _publ_contact_author_address ; Department of Materials Science and Eng. University of Michigan 2300 Hayward St. Ann Arbor Michigan 48109-2136 UNITED STATES OF AMERICA ; _publ_contact_author_email TALSDAD@UMICH.EDU _publ_section_title ; The selective dissolution of rice hull ash to form [OSiO1.5]8[R4N]8 (R = Me, CH2CH2OH) octasilicates. Basic nanobuilding blocks and possible models of intermediates formed during biosilification processes. ; loop_ _publ_author_name 'Richard Laine' 'M. Z. Asuncion' 'I. Hasegawa' 'Jeff W. Kampf' data_cholsi _database_code_depnum_ccdc_archive 'CCDC 263910' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H160 N8 O52 Si8' _chemical_formula_weight 1810.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.9649(9) _cell_length_b 16.5185(12) _cell_length_c 20.8305(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.8860(10) _cell_angle_gamma 90.00 _cell_volume 4116.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 5542 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.94 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; 2332 frames x 20 sec. @ 4.939 cm; 0.3 deg. steps in omega & phi ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40536 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.40 _reflns_number_total 8427 _reflns_number_gt 5610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; One of the choline cations is disordered over two inversion related positions. Modest DFIX restraints were applied to maintain chemical sensibility. Hydrogen atoms of the lattice water solvated were not included in the refinement. 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^)+(0.1487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8427 _refine_ls_number_parameters 522 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2294 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.77802(8) 0.46684(6) -0.00181(5) 0.0217(3) Uani 1 1 d . . . Si2 Si 0.91059(8) 0.53757(6) -0.11612(5) 0.0218(3) Uani 1 1 d . . . Si3 Si 0.97017(8) 0.34308(6) 0.02221(5) 0.0229(3) Uani 1 1 d . . . Si4 Si 0.89715(8) 0.58760(6) 0.09196(4) 0.0212(3) Uani 1 1 d . . . O1 O 0.8111(2) 0.51586(16) -0.06635(12) 0.0269(6) Uani 1 1 d . . . O2 O 0.9811(2) 0.61351(16) -0.08644(11) 0.0256(6) Uani 1 1 d . . . O3 O 0.9948(2) 0.46046(15) -0.12097(12) 0.0255(6) Uani 1 1 d . . . O4 O 0.8589(2) 0.55970(16) -0.18446(12) 0.0281(6) Uani 1 1 d . . . O5 O 0.6489(2) 0.44486(16) -0.00184(12) 0.0274(6) Uani 1 1 d . . . O6 O 0.8533(2) 0.38471(15) 0.00102(12) 0.0256(6) Uani 1 1 d . . . O7 O 0.9489(2) 0.24949(16) 0.03689(13) 0.0321(6) Uani 1 1 d . . . O8 O 1.0591(2) 0.35278(15) -0.03507(12) 0.0257(6) Uani 1 1 d . . . O9 O 0.8115(2) 0.52178(15) 0.06008(12) 0.0268(6) Uani 1 1 d . . . O10 O 0.8359(2) 0.63745(16) 0.14608(12) 0.0276(6) Uani 1 1 d . . . O11 O 0.4105(3) 0.7013(2) -0.00184(18) 0.0553(9) Uani 1 1 d . . . H11 H 0.3614 0.6775 0.0196 0.083 Uiso 1 1 calc R . . O12 O 1.1974(3) 0.2080(2) -0.13683(17) 0.0565(10) Uani 1 1 d . . . H12 H 1.1793 0.2571 -0.1380 0.085 Uiso 1 1 calc R . . O13 O 0.5885(3) 0.1950(2) -0.26569(16) 0.0633(11) Uani 1 1 d . . . H13 H 0.6224 0.1541 -0.2793 0.095 Uiso 1 1 calc R . . O89 O 0.9276(3) 0.6487(2) 0.26314(15) 0.0514(9) Uani 1 1 d . . . O90 O 1.0172(3) 0.1932(2) 0.14898(16) 0.0561(9) Uani 1 1 d . . . O91 O 0.9227(3) 0.4741(2) -0.28593(16) 0.0631(11) Uani 1 1 d . . . O92 O 0.6040(3) 0.5764(2) 0.29568(16) 0.0635(10) Uani 1 1 d . . . O93 O 0.2542(3) 0.8149(2) -0.0242(2) 0.0664(11) Uani 1 1 d . . . O94 O 1.2984(4) -0.0971(3) -0.1369(2) 0.0857(14) Uani 1 1 d . . . O95 O 0.5246(5) 0.9664(3) 0.1045(2) 0.1008(17) Uani 1 1 d . . . O97 O 0.5000(2) 0.50618(19) -0.08773(13) 0.0361(7) Uani 1 1 d . . . O98 O 0.6201(2) 0.6006(2) 0.16940(14) 0.0436(8) Uani 1 1 d . . . O99 O 0.6340(3) 0.5816(2) -0.18353(17) 0.0532(9) Uani 1 1 d . . . N1 N 0.6404(3) 0.7662(2) -0.04794(19) 0.0426(9) Uani 1 1 d . . . N2 N 1.2451(3) 0.1422(2) -0.28023(16) 0.0366(8) Uani 1 1 d . . . N3 N 0.7809(5) 0.2615(4) -0.1771(2) 0.0921(19) Uani 1 1 d . . . C1 C 0.5088(4) 0.7092(4) 0.0357(2) 0.0597(15) Uani 1 1 d . . . H1A H 0.5077 0.6684 0.0705 0.072 Uiso 1 1 calc R . . H1B H 0.5096 0.7634 0.0560 0.072 Uiso 1 1 calc R . . C2 C 0.6132(4) 0.6988(3) -0.0014(3) 0.0537(14) Uani 1 1 d . . . H2A H 0.6075 0.6476 -0.0258 0.064 Uiso 1 1 calc R . . H2B H 0.6765 0.6932 0.0294 0.064 Uiso 1 1 calc R . . C3 C 0.5598(5) 0.7701(4) -0.1027(3) 0.0707(18) Uani 1 1 d . . . H3A H 0.5723 0.8199 -0.1272 0.106 Uiso 1 1 calc R . . H3B H 0.4834 0.7699 -0.0865 0.106 Uiso 1 1 calc R . . H3C H 0.5706 0.7231 -0.1307 0.106 Uiso 1 1 calc R . . C4 C 0.7554(5) 0.7501(4) -0.0736(3) 0.079(2) Uani 1 1 d . . . H4A H 0.7549 0.6991 -0.0975 0.119 Uiso 1 1 calc R . . H4B H 0.8092 0.7463 -0.0377 0.119 Uiso 1 1 calc R . . H4C H 0.7770 0.7944 -0.1021 0.119 Uiso 1 1 calc R . . C5 C 0.6422(6) 0.8463(3) -0.0130(3) 0.0750(18) Uani 1 1 d . . . H5A H 0.7007 0.8453 0.0204 0.113 Uiso 1 1 calc R . . H5B H 0.5695 0.8556 0.0067 0.113 Uiso 1 1 calc R . . H5C H 0.6575 0.8899 -0.0435 0.113 Uiso 1 1 calc R . . C6 C 1.2991(4) 0.1971(3) -0.1688(2) 0.0490(12) Uani 1 1 d . . . H6A H 1.3262 0.1416 -0.1597 0.059 Uiso 1 1 calc R . . H6B H 1.3546 0.2351 -0.1499 0.059 Uiso 1 1 calc R . . C7 C 1.2970(4) 0.2090(3) -0.2400(2) 0.0416(11) Uani 1 1 d . . . H7A H 1.3749 0.2168 -0.2542 0.050 Uiso 1 1 calc R . . H7B H 1.2560 0.2598 -0.2495 0.050 Uiso 1 1 calc R . . C8 C 1.2475(5) 0.1691(5) -0.3492(3) 0.080(2) Uani 1 1 d . . . H8A H 1.3252 0.1767 -0.3621 0.121 Uiso 1 1 calc R . . H8B H 1.2069 0.2204 -0.3538 0.121 Uiso 1 1 calc R . . H8C H 1.2120 0.1279 -0.3764 0.121 Uiso 1 1 calc R . . C9 C 1.1261(4) 0.1279(4) -0.2613(3) 0.0614(15) Uani 1 1 d . . . H9A H 1.0922 0.0874 -0.2899 0.092 Uiso 1 1 calc R . . H9B H 1.0842 0.1787 -0.2647 0.092 Uiso 1 1 calc R . . H9C H 1.1244 0.1082 -0.2169 0.092 Uiso 1 1 calc R . . C10 C 1.3147(5) 0.0669(3) -0.2723(3) 0.0606(15) Uani 1 1 d . . . H10A H 1.3119 0.0485 -0.2276 0.091 Uiso 1 1 calc R . . H10B H 1.3923 0.0787 -0.2834 0.091 Uiso 1 1 calc R . . H10C H 1.2852 0.0243 -0.3006 0.091 Uiso 1 1 calc R . . C11 C 0.5926(4) 0.1956(3) -0.1989(2) 0.0529(13) Uani 1 1 d . . . H11A H 0.5454 0.1506 -0.1833 0.063 Uiso 1 1 calc R . . H11B H 0.5584 0.2467 -0.1840 0.063 Uiso 1 1 calc R . . C12 C 0.7058(5) 0.1879(4) -0.1676(3) 0.0656(16) Uani 1 1 d . . . H12A H 0.7435 0.1396 -0.1851 0.079 Uiso 1 1 calc R . . H12B H 0.6962 0.1791 -0.1210 0.079 Uiso 1 1 calc R . . C13 C 0.8119(7) 0.2685(5) -0.2468(3) 0.099(2) Uani 1 1 d . . . H13A H 0.7458 0.2839 -0.2723 0.149 Uiso 1 1 calc R . . H13B H 0.8403 0.2164 -0.2619 0.149 Uiso 1 1 calc R . . H13C H 0.8699 0.3099 -0.2513 0.149 Uiso 1 1 calc R . . C14 C 0.7375(8) 0.3386(6) -0.1568(4) 0.129(3) Uani 1 1 d . . . H14A H 0.7897 0.3816 -0.1688 0.193 Uiso 1 1 calc R . . H14B H 0.7286 0.3384 -0.1101 0.193 Uiso 1 1 calc R . . H14C H 0.6649 0.3482 -0.1778 0.193 Uiso 1 1 calc R . . C15 C 0.8834(8) 0.2462(6) -0.1366(4) 0.139(3) Uani 1 1 d . . . H15A H 0.9360 0.2911 -0.1418 0.209 Uiso 1 1 calc R . . H15B H 0.9186 0.1956 -0.1502 0.209 Uiso 1 1 calc R . . H15C H 0.8624 0.2420 -0.0915 0.209 Uiso 1 1 calc R . . O14 O 0.5804(10) 0.5256(6) -0.3026(5) 0.052(3) Uani 0.50 1 d PD A 1 H14 H 0.5364 0.4895 -0.2901 0.078 Uiso 0.50 1 calc PR A 1 O14A O 0.7482(6) 0.4524(5) -0.3619(4) 0.068(2) Uani 0.50 1 d PD A 2 H14D H 0.7981 0.4828 -0.3764 0.102 Uiso 0.50 1 calc PR A 2 C16 C 0.6368(15) 0.4978(14) -0.3615(8) 0.154(8) Uani 1 1 d D . . H16A H 0.6385 0.4382 -0.3564 0.185 Uiso 0.50 1 calc PR A 1 H16B H 0.7151 0.5156 -0.3546 0.185 Uiso 0.50 1 calc PR A 1 H16A' H 0.6431 0.5502 -0.3387 0.185 Uiso 0.50 1 calc PR A 2 H16B' H 0.5769 0.4649 -0.3421 0.185 Uiso 0.50 1 calc PR A 2 C17 C 0.6176(14) 0.5095(12) -0.4355(8) 0.113(5) Uani 1 1 d D A . H17A H 0.6716 0.5516 -0.4485 0.136 Uiso 1 1 calc R . . H17B H 0.6428 0.4585 -0.4556 0.136 Uiso 1 1 calc R . . N4 N 0.5059(10) 0.5316(7) -0.4703(6) 0.085(3) Uani 1 1 d . A 1 C18 C 0.5400(10) 0.5415(7) -0.5435(5) 0.060(3) Uani 1 1 d . . . H18A H 0.4729 0.5382 -0.5710 0.090 Uiso 1 1 calc R A -1 H18B H 0.5919 0.4982 -0.5551 0.090 Uiso 1 1 calc R A -1 H18C H 0.5762 0.5941 -0.5496 0.090 Uiso 1 1 calc R A -1 C19 C 0.4745(13) 0.6095(10) -0.4438(7) 0.088(4) Uani 1 1 d . A 1 H19A H 0.5122 0.6172 -0.4022 0.132 Uiso 1 1 calc R A -1 H19B H 0.3934 0.6111 -0.4381 0.132 Uiso 1 1 calc R A -1 H19C H 0.4966 0.6527 -0.4732 0.132 Uiso 1 1 calc R A -1 O84 O 0.3825(13) 0.9571(7) -0.0027(6) 0.115(4) Uani 0.50 1 d P B 1 O85 O 0.3229(15) 0.9531(8) 0.0363(7) 0.152(7) Uani 0.50 1 d P C 2 O86 O 0.4008(9) 0.6408(7) -0.4672(5) 0.095(3) Uani 0.50 1 d P D 3 O87 O 0.5966(14) 0.5632(10) -0.3141(9) 0.136(8) Uani 0.50 1 d P E 3 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 0.0171(5) 0.0266(6) 0.0213(5) -0.0005(4) 0.0009(4) -0.0022(4) Si2 0.0194(5) 0.0263(6) 0.0196(5) 0.0027(4) 0.0004(4) 0.0001(4) Si3 0.0226(5) 0.0232(5) 0.0229(5) 0.0014(4) 0.0024(4) -0.0016(4) Si4 0.0213(5) 0.0229(5) 0.0195(5) -0.0021(4) 0.0023(4) 0.0007(4) O1 0.0222(13) 0.0324(15) 0.0260(14) 0.0048(11) 0.0022(10) 0.0001(11) O2 0.0271(13) 0.0283(14) 0.0213(13) 0.0001(11) 0.0000(10) -0.0022(11) O3 0.0231(13) 0.0281(15) 0.0253(13) -0.0005(11) -0.0013(10) 0.0022(10) O4 0.0258(13) 0.0358(15) 0.0225(13) 0.0041(11) -0.0029(10) 0.0013(11) O5 0.0189(12) 0.0351(15) 0.0281(14) -0.0010(12) 0.0010(10) -0.0051(11) O6 0.0240(13) 0.0245(14) 0.0284(13) -0.0014(11) -0.0009(10) -0.0005(10) O7 0.0364(15) 0.0243(15) 0.0357(15) 0.0042(12) 0.0017(12) -0.0049(11) O8 0.0272(13) 0.0248(14) 0.0252(13) 0.0009(11) 0.0045(10) 0.0019(10) O9 0.0243(13) 0.0292(14) 0.0269(14) -0.0027(11) 0.0023(10) -0.0031(11) O10 0.0288(14) 0.0294(15) 0.0248(13) -0.0031(11) 0.0051(11) 0.0031(11) O11 0.0421(19) 0.047(2) 0.076(2) 0.0165(18) -0.0109(17) -0.0180(16) O12 0.073(2) 0.0378(19) 0.060(2) -0.0010(17) 0.0329(19) 0.0090(17) O13 0.080(3) 0.065(2) 0.045(2) -0.0247(17) -0.0192(18) 0.021(2) O89 0.058(2) 0.058(2) 0.0381(18) -0.0098(15) -0.0067(15) 0.0086(17) O90 0.071(2) 0.049(2) 0.048(2) 0.0136(17) 0.0083(17) 0.0047(18) O91 0.079(3) 0.076(3) 0.0354(18) 0.0011(17) 0.0053(17) 0.026(2) O92 0.094(3) 0.054(2) 0.0427(19) -0.0072(17) 0.0112(19) 0.010(2) O93 0.065(2) 0.043(2) 0.091(3) -0.007(2) 0.011(2) -0.0117(18) O94 0.076(3) 0.110(4) 0.072(3) -0.002(3) 0.020(2) -0.012(3) O95 0.117(4) 0.096(4) 0.090(3) 0.022(3) 0.021(3) 0.026(3) O97 0.0259(14) 0.0527(19) 0.0299(15) 0.0008(13) 0.0022(11) 0.0000(13) O98 0.0343(16) 0.060(2) 0.0366(16) -0.0031(15) 0.0071(13) -0.0013(15) O99 0.0322(17) 0.063(2) 0.064(2) 0.0197(18) -0.0017(15) 0.0075(15) N1 0.036(2) 0.042(2) 0.050(2) 0.0013(18) 0.0062(17) 0.0048(17) N2 0.0317(18) 0.045(2) 0.0337(19) -0.0112(16) 0.0067(14) -0.0027(15) N3 0.099(4) 0.118(4) 0.061(3) -0.048(3) 0.032(3) -0.073(3) C1 0.057(3) 0.071(4) 0.051(3) 0.016(3) -0.012(2) -0.034(3) C2 0.050(3) 0.041(3) 0.069(3) 0.004(2) -0.027(3) -0.004(2) C3 0.054(3) 0.112(5) 0.046(3) 0.022(3) 0.007(3) 0.025(3) C4 0.045(3) 0.114(6) 0.078(4) -0.008(4) 0.011(3) 0.024(3) C5 0.088(4) 0.042(3) 0.096(5) -0.005(3) 0.039(4) -0.005(3) C6 0.053(3) 0.052(3) 0.041(3) -0.012(2) -0.003(2) 0.017(2) C7 0.038(2) 0.040(3) 0.046(3) -0.007(2) 0.005(2) -0.0033(19) C8 0.082(4) 0.123(6) 0.036(3) -0.002(3) 0.012(3) 0.017(4) C9 0.036(3) 0.072(4) 0.076(4) -0.023(3) 0.012(2) -0.017(2) C10 0.056(3) 0.052(3) 0.075(4) -0.020(3) 0.002(3) 0.011(3) C11 0.058(3) 0.059(3) 0.042(3) -0.019(2) 0.004(2) -0.022(2) C12 0.065(3) 0.082(4) 0.050(3) -0.005(3) 0.001(3) -0.028(3) C13 0.125(5) 0.107(5) 0.067(4) -0.034(3) 0.049(4) -0.069(4) C14 0.136(6) 0.129(6) 0.124(6) -0.052(5) 0.044(5) -0.052(5) C15 0.119(6) 0.185(7) 0.114(5) -0.041(5) -0.005(5) -0.057(5) O14 0.056(4) 0.055(5) 0.046(4) 0.008(4) 0.014(3) 0.003(4) O14A 0.052(4) 0.099(5) 0.053(4) -0.036(4) -0.010(3) 0.022(4) C16 0.158(10) 0.151(10) 0.153(10) 0.004(7) 0.002(7) -0.014(7) C17 0.108(8) 0.121(8) 0.110(8) 0.032(7) 0.010(6) 0.014(6) N4 0.082(6) 0.075(6) 0.100(6) 0.022(5) 0.031(5) 0.029(5) C18 0.071(6) 0.048(5) 0.060(5) 0.010(4) -0.016(5) -0.025(4) C19 0.089(7) 0.101(7) 0.073(6) 0.000(6) -0.001(6) 0.017(6) O84 0.151(12) 0.089(8) 0.105(9) 0.000(7) 0.013(8) -0.041(8) O85 0.229(18) 0.112(10) 0.115(11) 0.003(8) 0.023(11) -0.104(11) O86 0.087(7) 0.101(8) 0.097(7) -0.062(6) -0.007(5) 0.009(6) O87 0.123(13) 0.140(14) 0.144(14) -0.094(11) -0.079(10) 0.102(11) _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 O5 1.586(2) . ? Si1 O9 1.622(3) . ? Si1 O1 1.624(3) . ? Si1 O6 1.629(3) . ? Si2 O4 1.586(3) . ? Si2 O3 1.628(3) . ? Si2 O2 1.629(3) . ? Si2 O1 1.630(3) . ? Si3 O7 1.597(3) . ? Si3 O6 1.613(3) . ? Si3 O2 1.619(3) 3_765 ? Si3 O8 1.619(3) . ? Si4 O10 1.585(3) . ? Si4 O3 1.626(3) 3_765 ? Si4 O9 1.629(3) . ? Si4 O8 1.633(3) 3_765 ? O2 Si3 1.618(3) 3_765 ? O3 Si4 1.626(3) 3_765 ? O8 Si4 1.633(3) 3_765 ? O11 C1 1.409(6) . ? O12 C6 1.408(6) . ? O13 C11 1.392(6) . ? N1 C3 1.484(6) . ? N1 C4 1.508(6) . ? N1 C5 1.509(7) . ? N1 C2 1.515(6) . ? N2 C9 1.502(5) . ? N2 C8 1.504(6) . ? N2 C10 1.505(6) . ? N2 C7 1.513(5) . ? N3 C14 1.442(10) . ? N3 C15 1.498(10) . ? N3 C13 1.508(7) . ? N3 C12 1.526(7) . ? C1 C2 1.489(8) . ? C6 C7 1.497(6) . ? C11 C12 1.499(7) . ? O14 C16 1.482(15) . ? O14A C16 1.529(15) . ? C16 C17 1.568(16) . ? C17 N4 1.554(19) . ? N4 C19 1.451(17) . ? N4 C18 1.594(16) . ? 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 O5 Si1 O9 110.91(14) . . ? O5 Si1 O1 111.32(14) . . ? O9 Si1 O1 108.59(14) . . ? O5 Si1 O6 110.33(14) . . ? O9 Si1 O6 107.92(13) . . ? O1 Si1 O6 107.65(14) . . ? O4 Si2 O3 110.95(14) . . ? O4 Si2 O2 110.84(14) . . ? O3 Si2 O2 107.98(14) . . ? O4 Si2 O1 110.09(14) . . ? O3 Si2 O1 109.01(14) . . ? O2 Si2 O1 107.89(14) . . ? O7 Si3 O6 108.95(14) . . ? O7 Si3 O2 109.09(14) . 3_765 ? O6 Si3 O2 109.67(14) . 3_765 ? O7 Si3 O8 110.22(15) . . ? O6 Si3 O8 109.43(14) . . ? O2 Si3 O8 109.46(14) 3_765 . ? O10 Si4 O3 111.31(14) . 3_765 ? O10 Si4 O9 109.98(14) . . ? O3 Si4 O9 108.51(14) 3_765 . ? O10 Si4 O8 111.09(14) . 3_765 ? O3 Si4 O8 107.59(13) 3_765 3_765 ? O9 Si4 O8 108.26(13) . 3_765 ? Si1 O1 Si2 145.69(17) . . ? Si3 O2 Si2 146.40(17) 3_765 . ? Si4 O3 Si2 148.03(17) 3_765 . ? Si3 O6 Si1 147.28(17) . . ? Si3 O8 Si4 144.70(17) . 3_765 ? Si1 O9 Si4 147.55(18) . . ? C3 N1 C4 108.7(4) . . ? C3 N1 C5 109.7(5) . . ? C4 N1 C5 108.6(4) . . ? C3 N1 C2 112.4(4) . . ? C4 N1 C2 107.6(4) . . ? C5 N1 C2 109.7(4) . . ? C9 N2 C8 109.2(4) . . ? C9 N2 C10 111.5(4) . . ? C8 N2 C10 109.3(4) . . ? C9 N2 C7 110.6(3) . . ? C8 N2 C7 107.4(4) . . ? C10 N2 C7 108.7(3) . . ? C14 N3 C15 106.2(6) . . ? C14 N3 C13 108.0(7) . . ? C15 N3 C13 110.0(6) . . ? C14 N3 C12 116.8(6) . . ? C15 N3 C12 105.7(6) . . ? C13 N3 C12 110.0(4) . . ? O11 C1 C2 113.6(4) . . ? C1 C2 N1 116.0(4) . . ? O12 C6 C7 116.8(4) . . ? C6 C7 N2 117.0(4) . . ? O13 C11 C12 116.9(5) . . ? C11 C12 N3 114.0(5) . . ? O14 C16 O14A 124.4(13) . . ? O14 C16 C17 135.5(14) . . ? O14A C16 C17 99.8(11) . . ? N4 C17 C16 126.9(14) . . ? C19 N4 C17 104.9(13) . . ? C19 N4 C18 110.2(10) . . ? C17 N4 C18 103.9(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 O5 0.84 2.07 2.518(4) 113.2 3_665 O12 H12 O10 0.84 1.76 2.591(4) 170.2 3_765 O13 H13 O4 0.84 1.75 2.548(4) 158.2 2_644 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.802 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.099