data_twin _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SSZ-35/C11H24N _chemical_melting_point ? _chemical_formula_moiety 'Si16 O32 F, C11 H24 N' _chemical_formula_sum 'C11 H24 F N O32 Si16' _chemical_formula_weight 1150.75 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' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4025(12) _cell_length_b 11.3530(18) _cell_length_c 11.4856(18) _cell_angle_alpha 105.207(3) _cell_angle_beta 96.995(3) _cell_angle_gamma 94.425(3) _cell_volume 918.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3768 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.3 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.798 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'Twinabs (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ApexII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17537 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5057 _reflns_number_gt 3629 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT and cell_now (Sheldrick, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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. The ammonium ion is disordered with respect to a center of symmetry. The molecule was refined with distance restraints and isotropic thermal parameters as a complete molecule with 0.5 occupancies. The fluorine is also refined at 0.5 occupancy. The structure is twinned with respect to rotation around the reciprocal lattice vector (0 0 1). Two twin components were identified with the use of cell_now and were integrated using SAINT. The final refinement used both single and overlapped reflections (hklf 5). The twin parameter refined to 0.1663(13). The atom F1 is placed at half occupancy in keeping with the overall charge and level of doping. ; _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^)+(0.0323P)^2^+13.3753P] 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_extinction_coef ? _refine_ls_number_reflns 5049 _refine_ls_number_parameters 280 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 0.583 _refine_ls_restrained_S_all 0.584 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.46462(13) -0.07651(9) 0.25275(9) 0.0115(2) Uani 1 1 d . . . Si2 Si 0.28030(13) 0.06829(9) 0.08476(9) 0.0119(2) Uani 1 1 d . . . Si3 Si 0.42808(13) 0.26779(9) -0.02988(9) 0.0121(2) Uani 1 1 d . . . Si4 Si 0.81256(14) 0.38411(10) 0.06695(9) 0.0135(2) Uani 1 1 d . . . Si5 Si 0.89923(13) 0.14715(9) 0.14366(9) 0.0115(2) Uani 1 1 d . . . Si6 Si 0.83777(13) 0.06334(9) 0.37027(9) 0.0113(2) Uani 1 1 d . . . Si7 Si 0.93883(14) 0.65339(10) 0.13293(9) 0.0164(2) Uani 1 1 d . . . Si8 Si 0.89368(13) 0.14013(9) 0.64258(9) 0.0119(2) Uani 1 1 d . . . O1 O 0.4047(3) 0.0254(2) 0.1869(2) 0.0174(6) Uani 1 1 d . . . O2 O 0.3995(4) 0.1748(3) 0.0524(3) 0.0195(6) Uani 1 1 d . . . O3 O 0.5911(3) 0.3718(2) 0.0423(2) 0.0170(6) Uani 1 1 d . . . O4 O 0.8755(4) 0.2827(2) 0.1340(2) 0.0203(6) Uani 1 1 d . . . O5 O 0.8407(3) 0.1417(2) 0.2729(2) 0.0158(5) Uani 1 1 d . . . O6 O 0.6432(3) -0.0177(2) 0.3517(2) 0.0154(5) Uani 1 1 d . . . O7 O 0.5157(4) -0.1953(2) 0.1581(2) 0.0193(6) Uani 1 1 d . . . O8 O 0.3066(3) -0.1184(2) 0.3223(2) 0.0154(5) Uani 1 1 d . . . O9 O 0.1093(4) 0.1228(3) 0.1433(2) 0.0205(6) Uani 1 1 d . . . O10 O 0.2251(4) -0.0455(3) -0.0344(3) 0.0243(6) Uani 1 1 d . . . O11 O 0.2463(4) 0.3305(3) -0.0541(3) 0.0258(7) Uani 1 1 d . . . O12 O 0.8867(3) 0.3628(3) -0.0612(2) 0.0188(6) Uani 1 1 d . . . O13 O 0.8902(4) 0.5166(2) 0.1548(2) 0.0186(6) Uani 1 1 d . . . O14 O 0.8693(3) 0.1563(2) 0.5052(2) 0.0139(5) Uani 1 1 d . . . O15 O 0.9994(3) 0.0227(2) 0.6433(2) 0.0161(6) Uani 1 1 d . . . O16 O 1.0101(4) 0.2641(3) 0.7275(2) 0.0199(6) Uani 1 1 d . . . F1 F 0.9841(8) 0.8133(5) 0.1125(5) 0.0373(13) Uani 0.50 1 d P . . C49 C 0.6137(15) 0.5399(10) 0.7063(10) 0.047(3) Uiso 0.50 1 d PD A -1 H49A H 0.5257 0.6013 0.7072 0.056 Uiso 0.50 1 calc PR A -1 H49B H 0.6814 0.5568 0.7899 0.056 Uiso 0.50 1 calc PR A -1 C50 C 0.506(2) 0.4093(11) 0.6697(11) 0.036(3) Uiso 0.50 1 d PD A -1 H50A H 0.4146 0.4064 0.7250 0.043 Uiso 0.50 1 calc PR A -1 H50B H 0.5923 0.3485 0.6787 0.043 Uiso 0.50 1 calc PR A -1 C51 C 0.4074(16) 0.3747(11) 0.5347(11) 0.039(4) Uiso 0.50 1 d PD A -1 C52 C 0.5457(15) 0.3941(10) 0.4521(10) 0.045(3) Uiso 0.50 1 d PD A -1 H52A H 0.4797 0.3786 0.3682 0.054 Uiso 0.50 1 calc PR A -1 H52B H 0.6329 0.3319 0.4502 0.054 Uiso 0.50 1 calc PR A -1 N53 N 0.6562(12) 0.5217(8) 0.4877(8) 0.045(2) Uiso 0.50 1 d PD A -1 C54 C 0.7479(15) 0.5536(11) 0.6197(9) 0.047(3) Uiso 0.50 1 d PD A -1 H54A H 0.8448 0.4993 0.6264 0.057 Uiso 0.50 1 calc PR A -1 H54B H 0.8072 0.6393 0.6440 0.057 Uiso 0.50 1 calc PR A -1 C55 C 0.2236(14) 0.4296(10) 0.5263(10) 0.040(2) Uiso 0.50 1 d PD A -1 H55A H 0.2464 0.5195 0.5535 0.061 Uiso 0.50 1 calc PR A -1 H55B H 0.1454 0.4006 0.5784 0.061 Uiso 0.50 1 calc PR A -1 H55C H 0.1622 0.4037 0.4416 0.061 Uiso 0.50 1 calc PR A -1 C56 C 0.360(2) 0.2379(11) 0.5017(15) 0.030(4) Uiso 0.50 1 d PD A -1 H56A H 0.2900 0.2166 0.5620 0.044 Uiso 0.50 1 calc PR A -1 H56B H 0.4726 0.1980 0.5009 0.044 Uiso 0.50 1 calc PR A -1 H56C H 0.2858 0.2098 0.4207 0.044 Uiso 0.50 1 calc PR A -1 C57 C 0.539(2) 0.6220(12) 0.4653(12) 0.044(4) Uiso 0.50 1 d PD A -1 H57 H 0.4376 0.6205 0.5153 0.053 Uiso 0.50 1 calc PR A -1 C58 C 0.648(3) 0.7535(16) 0.518(2) 0.062(7) Uiso 0.50 1 d PD A -1 H58A H 0.6925 0.7671 0.6048 0.093 Uiso 0.50 1 calc PR A -1 H58B H 0.5671 0.8156 0.5075 0.093 Uiso 0.50 1 calc PR A -1 H58C H 0.7523 0.7599 0.4740 0.093 Uiso 0.50 1 calc PR A -1 C59 C 0.445(3) 0.5910(18) 0.3323(15) 0.071(6) Uiso 0.50 1 d PD A -1 H59A H 0.3384 0.5295 0.3199 0.107 Uiso 0.50 1 calc PR A -1 H59B H 0.5312 0.5581 0.2774 0.107 Uiso 0.50 1 calc PR A -1 H59C H 0.4039 0.6656 0.3149 0.107 Uiso 0.50 1 calc PR A -1 C60 C 0.7992(19) 0.5087(14) 0.4063(13) 0.062(4) Uiso 0.50 1 d P A -1 H60A H 0.7448 0.5102 0.3246 0.094 Uiso 0.50 1 calc PR A -1 H60B H 0.8498 0.4306 0.4015 0.094 Uiso 0.50 1 calc PR A -1 H60C H 0.8973 0.5767 0.4391 0.094 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0079(4) 0.0153(5) 0.0110(5) 0.0023(4) 0.0024(4) 0.0021(4) Si2 0.0093(5) 0.0147(5) 0.0120(5) 0.0030(4) 0.0032(4) 0.0029(4) Si3 0.0094(5) 0.0157(5) 0.0127(5) 0.0046(4) 0.0046(4) 0.0039(4) Si4 0.0136(5) 0.0157(5) 0.0113(5) 0.0026(4) 0.0038(4) 0.0028(4) Si5 0.0099(5) 0.0136(5) 0.0113(5) 0.0027(4) 0.0034(4) 0.0030(4) Si6 0.0088(4) 0.0130(5) 0.0116(5) 0.0020(4) 0.0029(4) 0.0015(4) Si7 0.0107(5) 0.0247(6) 0.0099(5) -0.0030(4) 0.0019(4) 0.0050(4) Si8 0.0086(4) 0.0134(5) 0.0118(5) -0.0011(4) 0.0034(4) 0.0018(4) O1 0.0129(13) 0.0222(15) 0.0177(14) 0.0070(11) 0.0007(10) 0.0034(11) O2 0.0156(13) 0.0238(15) 0.0230(15) 0.0127(12) 0.0043(11) 0.0015(11) O3 0.0138(13) 0.0172(13) 0.0193(14) 0.0020(11) 0.0059(11) 0.0026(10) O4 0.0262(15) 0.0167(14) 0.0197(14) 0.0061(12) 0.0052(12) 0.0057(12) O5 0.0149(13) 0.0194(14) 0.0161(13) 0.0071(11) 0.0066(10) 0.0050(11) O6 0.0105(12) 0.0208(14) 0.0136(13) 0.0053(11) -0.0019(10) -0.0012(10) O7 0.0183(14) 0.0200(14) 0.0192(14) 0.0014(11) 0.0097(11) 0.0026(11) O8 0.0129(13) 0.0176(13) 0.0167(13) 0.0045(11) 0.0056(10) 0.0034(10) O9 0.0140(13) 0.0291(16) 0.0199(14) 0.0057(12) 0.0069(11) 0.0079(12) O10 0.0197(15) 0.0251(16) 0.0214(15) -0.0034(12) -0.0007(12) 0.0018(12) O11 0.0213(15) 0.0436(19) 0.0159(14) 0.0091(13) 0.0041(11) 0.0199(14) O12 0.0108(12) 0.0299(16) 0.0154(13) 0.0075(12) 0.0013(10) -0.0037(11) O13 0.0227(14) 0.0141(13) 0.0180(14) 0.0036(11) 0.0000(11) 0.0042(11) O14 0.0134(12) 0.0135(13) 0.0134(12) 0.0005(10) 0.0041(10) 0.0019(10) O15 0.0144(13) 0.0188(14) 0.0138(13) 0.0008(11) 0.0025(10) 0.0060(11) O16 0.0155(13) 0.0226(15) 0.0142(13) -0.0072(11) 0.0051(11) -0.0043(11) F1 0.049(3) 0.030(3) 0.035(3) 0.010(2) 0.013(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O1 1.601(3) . ? Si1 O7 1.598(3) . ? Si1 O8 1.604(3) . ? Si1 O6 1.608(3) . ? Si2 O2 1.591(3) . ? Si2 O9 1.596(3) . ? Si2 O10 1.601(3) . ? Si2 O1 1.602(3) . ? Si3 O11 1.598(3) . ? Si3 O3 1.600(3) . ? Si3 O7 1.608(3) 2_655 ? Si3 O2 1.609(3) . ? Si4 O13 1.594(3) . ? Si4 O12 1.599(3) . ? Si4 O4 1.611(3) . ? Si4 O3 1.618(3) . ? Si5 O4 1.593(3) . ? Si5 O10 1.596(3) 2_655 ? Si5 O9 1.601(3) 1_655 ? Si5 O5 1.611(3) . ? Si6 O5 1.603(3) . ? Si6 O15 1.606(3) 2_756 ? Si6 O6 1.607(3) . ? Si6 O14 1.608(3) . ? Si7 O11 1.599(3) 2_665 ? Si7 O12 1.611(3) 2_765 ? Si7 O16 1.612(3) 2_766 ? Si7 O13 1.656(3) . ? Si7 F1 1.900(6) . ? Si8 O15 1.599(3) . ? Si8 O16 1.601(3) . ? Si8 O8 1.601(3) 2_656 ? Si8 O14 1.626(3) . ? O7 Si3 1.608(3) 2_655 ? O8 Si8 1.601(3) 2_656 ? O9 Si5 1.601(3) 1_455 ? O10 Si5 1.596(3) 2_655 ? O11 Si7 1.599(3) 2_665 ? O12 Si7 1.611(3) 2_765 ? O15 Si6 1.606(3) 2_756 ? O16 Si7 1.612(3) 2_766 ? C49 C54 1.516(12) . ? C49 C50 1.554(14) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.566(13) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C56 1.501(13) . ? C51 C52 1.519(13) . ? C51 C55 1.543(13) . ? C52 N53 1.536(12) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? N53 C60 1.487(16) . ? N53 C54 1.521(12) . ? N53 C57 1.539(16) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.538(15) . ? C57 C58 1.571(15) . ? C57 H57 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 Si1 O7 111.70(15) . . ? O1 Si1 O8 111.66(14) . . ? O7 Si1 O8 108.72(14) . . ? O1 Si1 O6 108.04(15) . . ? O7 Si1 O6 108.24(14) . . ? O8 Si1 O6 108.36(14) . . ? O2 Si2 O9 108.95(16) . . ? O2 Si2 O10 109.52(16) . . ? O9 Si2 O10 113.93(15) . . ? O2 Si2 O1 107.57(15) . . ? O9 Si2 O1 107.50(15) . . ? O10 Si2 O1 109.17(16) . . ? O11 Si3 O3 109.42(16) . . ? O11 Si3 O7 109.50(15) . 2_655 ? O3 Si3 O7 109.12(14) . 2_655 ? O11 Si3 O2 111.24(15) . . ? O3 Si3 O2 107.64(15) . . ? O7 Si3 O2 109.88(15) 2_655 . ? O13 Si4 O12 110.82(15) . . ? O13 Si4 O4 108.16(15) . . ? O12 Si4 O4 110.58(15) . . ? O13 Si4 O3 109.76(14) . . ? O12 Si4 O3 108.50(14) . . ? O4 Si4 O3 108.99(15) . . ? O4 Si5 O10 111.91(16) . 2_655 ? O4 Si5 O9 109.98(16) . 1_655 ? O10 Si5 O9 109.27(15) 2_655 1_655 ? O4 Si5 O5 106.01(14) . . ? O10 Si5 O5 110.62(15) 2_655 . ? O9 Si5 O5 108.98(15) 1_655 . ? O5 Si6 O15 108.95(14) . 2_756 ? O5 Si6 O6 111.06(14) . . ? O15 Si6 O6 110.80(15) 2_756 . ? O5 Si6 O14 108.82(14) . . ? O15 Si6 O14 109.32(14) 2_756 . ? O6 Si6 O14 107.85(13) . . ? O11 Si7 O12 115.14(15) 2_665 2_765 ? O11 Si7 O16 119.02(15) 2_665 2_766 ? O12 Si7 O16 113.27(14) 2_765 2_766 ? O11 Si7 O13 102.14(16) 2_665 . ? O12 Si7 O13 103.76(15) 2_765 . ? O16 Si7 O13 100.08(15) 2_766 . ? O11 Si7 F1 76.4(2) 2_665 . ? O12 Si7 F1 79.3(2) 2_765 . ? O16 Si7 F1 78.4(2) 2_766 . ? O13 Si7 F1 176.9(2) . . ? O15 Si8 O16 111.71(15) . . ? O15 Si8 O8 109.64(14) . 2_656 ? O16 Si8 O8 113.10(14) . 2_656 ? O15 Si8 O14 108.63(13) . . ? O16 Si8 O14 105.74(15) . . ? O8 Si8 O14 107.79(14) 2_656 . ? Si1 O1 Si2 151.88(19) . . ? Si2 O2 Si3 150.90(19) . . ? Si3 O3 Si4 136.91(17) . . ? Si5 O4 Si4 155.3(2) . . ? Si6 O5 Si5 145.27(18) . . ? Si6 O6 Si1 142.39(18) . . ? Si1 O7 Si3 153.7(2) . 2_655 ? Si8 O8 Si1 159.24(19) 2_656 . ? Si2 O9 Si5 155.3(2) . 1_455 ? Si5 O10 Si2 159.9(2) 2_655 . ? Si7 O11 Si3 154.6(2) 2_665 . ? Si4 O12 Si7 146.98(18) . 2_765 ? Si4 O13 Si7 134.20(18) . . ? Si6 O14 Si8 134.74(17) . . ? Si8 O15 Si6 158.50(19) . 2_756 ? Si8 O16 Si7 142.96(19) . 2_766 ? C54 C49 C50 112.3(10) . . ? C54 C49 H49A 109.2 . . ? C50 C49 H49A 109.2 . . ? C54 C49 H49B 109.2 . . ? C50 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C49 C50 C51 111.1(10) . . ? C49 C50 H50A 109.4 . . ? C51 C50 H50A 109.4 . . ? C49 C50 H50B 109.4 . . ? C51 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C56 C51 C52 104.5(10) . . ? C56 C51 C55 106.1(10) . . ? C52 C51 C55 120.1(10) . . ? C56 C51 C50 104.5(11) . . ? C52 C51 C50 109.1(10) . . ? C55 C51 C50 111.2(10) . . ? C51 C52 N53 115.9(9) . . ? C51 C52 H52A 108.3 . . ? N53 C52 H52A 108.3 . . ? C51 C52 H52B 108.3 . . ? N53 C52 H52B 108.3 . . ? H52A C52 H52B 107.4 . . ? C60 N53 C54 109.2(9) . . ? C60 N53 C57 109.0(10) . . ? C54 N53 C57 111.3(8) . . ? C60 N53 C52 104.5(9) . . ? C54 N53 C52 110.1(9) . . ? C57 N53 C52 112.5(9) . . ? C49 C54 N53 112.5(9) . . ? C49 C54 H54A 109.1 . . ? N53 C54 H54A 109.1 . . ? C49 C54 H54B 109.1 . . ? N53 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? N53 C57 C59 112.0(11) . . ? N53 C57 C58 111.4(12) . . ? C59 C57 C58 115.9(14) . . ? N53 C57 H57 105.6 . . ? C59 C57 H57 105.6 . . ? C58 C57 H57 105.6 . . ? 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 O7 Si1 O1 Si2 54.5(4) . . . . ? O8 Si1 O1 Si2 -67.5(4) . . . . ? O6 Si1 O1 Si2 173.4(4) . . . . ? O2 Si2 O1 Si1 -149.6(4) . . . . ? O9 Si2 O1 Si1 93.2(4) . . . . ? O10 Si2 O1 Si1 -30.9(4) . . . . ? O9 Si2 O2 Si3 -71.5(4) . . . . ? O10 Si2 O2 Si3 53.8(4) . . . . ? O1 Si2 O2 Si3 172.3(4) . . . . ? O11 Si3 O2 Si2 44.3(4) . . . . ? O3 Si3 O2 Si2 164.2(4) . . . . ? O7 Si3 O2 Si2 -77.1(4) 2_655 . . . ? O11 Si3 O3 Si4 -160.8(2) . . . . ? O7 Si3 O3 Si4 -41.0(3) 2_655 . . . ? O2 Si3 O3 Si4 78.2(3) . . . . ? O13 Si4 O3 Si3 -177.4(2) . . . . ? O12 Si4 O3 Si3 61.3(3) . . . . ? O4 Si4 O3 Si3 -59.2(3) . . . . ? O10 Si5 O4 Si4 -14.6(5) 2_655 . . . ? O9 Si5 O4 Si4 107.0(5) 1_655 . . . ? O5 Si5 O4 Si4 -135.3(5) . . . . ? O13 Si4 O4 Si5 -172.8(4) . . . . ? O12 Si4 O4 Si5 -51.3(5) . . . . ? O3 Si4 O4 Si5 67.9(5) . . . . ? O15 Si6 O5 Si5 25.4(4) 2_756 . . . ? O6 Si6 O5 Si5 -96.9(3) . . . . ? O14 Si6 O5 Si5 144.5(3) . . . . ? O4 Si5 O5 Si6 -169.4(3) . . . . ? O10 Si5 O5 Si6 69.1(3) 2_655 . . . ? O9 Si5 O5 Si6 -51.1(4) 1_655 . . . ? O5 Si6 O6 Si1 21.4(3) . . . . ? O15 Si6 O6 Si1 -99.8(3) 2_756 . . . ? O14 Si6 O6 Si1 140.5(3) . . . . ? O1 Si1 O6 Si6 -44.8(3) . . . . ? O7 Si1 O6 Si6 76.3(3) . . . . ? O8 Si1 O6 Si6 -165.9(3) . . . . ? O1 Si1 O7 Si3 18.1(5) . . . 2_655 ? O8 Si1 O7 Si3 141.7(4) . . . 2_655 ? O6 Si1 O7 Si3 -100.8(4) . . . 2_655 ? O1 Si1 O8 Si8 21.0(6) . . . 2_656 ? O7 Si1 O8 Si8 -102.7(5) . . . 2_656 ? O6 Si1 O8 Si8 139.9(5) . . . 2_656 ? O2 Si2 O9 Si5 101.9(5) . . . 1_455 ? O10 Si2 O9 Si5 -20.8(6) . . . 1_455 ? O1 Si2 O9 Si5 -141.8(5) . . . 1_455 ? O2 Si2 O10 Si5 -119.3(6) . . . 2_655 ? O9 Si2 O10 Si5 3.0(7) . . . 2_655 ? O1 Si2 O10 Si5 123.2(6) . . . 2_655 ? O3 Si3 O11 Si7 140.6(5) . . . 2_665 ? O7 Si3 O11 Si7 21.1(6) 2_655 . . 2_665 ? O2 Si3 O11 Si7 -100.6(5) . . . 2_665 ? O13 Si4 O12 Si7 66.1(4) . . . 2_765 ? O4 Si4 O12 Si7 -53.9(4) . . . 2_765 ? O3 Si4 O12 Si7 -173.4(3) . . . 2_765 ? O12 Si4 O13 Si7 35.0(3) . . . . ? O4 Si4 O13 Si7 156.4(2) . . . . ? O3 Si4 O13 Si7 -84.8(3) . . . . ? O11 Si7 O13 Si4 51.7(3) 2_665 . . . ? O12 Si7 O13 Si4 -68.3(3) 2_765 . . . ? O16 Si7 O13 Si4 174.5(2) 2_766 . . . ? F1 Si7 O13 Si4 113(4) . . . . ? O5 Si6 O14 Si8 -175.7(2) . . . . ? O15 Si6 O14 Si8 -56.8(3) 2_756 . . . ? O6 Si6 O14 Si8 63.8(3) . . . . ? O15 Si8 O14 Si6 33.7(3) . . . . ? O16 Si8 O14 Si6 153.8(2) . . . . ? O8 Si8 O14 Si6 -85.0(2) 2_656 . . . ? O16 Si8 O15 Si6 -54.2(5) . . . 2_756 ? O8 Si8 O15 Si6 179.6(5) 2_656 . . 2_756 ? O14 Si8 O15 Si6 62.0(5) . . . 2_756 ? O15 Si8 O16 Si7 -81.7(3) . . . 2_766 ? O8 Si8 O16 Si7 42.6(4) 2_656 . . 2_766 ? O14 Si8 O16 Si7 160.3(3) . . . 2_766 ? C54 C49 C50 C51 -55.0(14) . . . . ? C49 C50 C51 C56 163.7(11) . . . . ? C49 C50 C51 C52 52.4(13) . . . . ? C49 C50 C51 C55 -82.3(13) . . . . ? C56 C51 C52 N53 -164.7(10) . . . . ? C55 C51 C52 N53 76.5(13) . . . . ? C50 C51 C52 N53 -53.5(13) . . . . ? C51 C52 N53 C60 170.8(10) . . . . ? C51 C52 N53 C54 53.6(12) . . . . ? C51 C52 N53 C57 -71.1(11) . . . . ? C50 C49 C54 N53 55.5(13) . . . . ? C60 N53 C54 C49 -166.8(10) . . . . ? C57 N53 C54 C49 72.7(12) . . . . ? C52 N53 C54 C49 -52.7(12) . . . . ? C60 N53 C57 C59 59.6(15) . . . . ? C54 N53 C57 C59 -179.8(12) . . . . ? C52 N53 C57 C59 -55.8(14) . . . . ? C60 N53 C57 C58 -71.9(15) . . . . ? C54 N53 C57 C58 48.7(15) . . . . ? C52 N53 C57 C58 172.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.545 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.098