Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name C.Krempner _publ_contact_author_email 'clemens.krempner@ttu.edu ' _publ_author_name C.Krempner data_ljhw_krempner_5_0m _database_code_depnum_ccdc_archive 'CCDC 807150' #TrackingRef '- K-4 with checkcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H39 K O6 Si4' _chemical_formula_weight 466.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 8.1549(6) _cell_length_b 19.2942(14) _cell_length_c 16.7811(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.9570(10) _cell_angle_gamma 90.00 _cell_volume 2640.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23434 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.93 _reflns_number_total 4105 _reflns_number_gt 3452 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0276P)^2^+1.5456P] 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 0.0000(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4105 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 2.809 _refine_ls_shift/su_mean 0.012 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 Si3 Si 0.31272(7) 0.21180(3) 0.23795(3) 0.02724(14) Uani 1 1 d . . . Si2 Si 0.30467(7) 0.04434(3) 0.15081(3) 0.02800(15) Uani 1 1 d . . . Si4 Si 0.30705(7) 0.06359(3) 0.36112(3) 0.02797(15) Uani 1 1 d . . . Si1 Si 0.44233(6) 0.10532(3) 0.25052(3) 0.02551(14) Uani 1 1 d . . . O6 O -0.15741(19) 0.17676(8) 0.38994(9) 0.0491(4) Uani 1 1 d . . . O5 O -0.17383(18) 0.19073(8) 0.11889(9) 0.0440(4) Uani 1 1 d . . . O4 O -0.17654(17) -0.02975(7) 0.23481(10) 0.0455(4) Uani 1 1 d . . . O2 O 0.11977(16) 0.20588(7) 0.20175(9) 0.0391(4) Uani 1 1 d . . . O3 O 0.11579(17) 0.09506(7) 0.36917(8) 0.0374(4) Uani 1 1 d . . . O1 O 0.11274(16) 0.02233(7) 0.17543(8) 0.0344(3) Uani 1 1 d . . . C15 C -0.2268(4) 0.24328(16) 0.40039(19) 0.0811(10) Uani 1 1 d . . . H15A H -0.2970 0.2429 0.4472 0.122 Uiso 1 1 calc R . . H15B H -0.2926 0.2556 0.3531 0.122 Uiso 1 1 calc R . . H15C H -0.1390 0.2774 0.4081 0.122 Uiso 1 1 calc R . . C14 C -0.2520(3) 0.16462(16) 0.04917(16) 0.0693(8) Uani 1 1 d . . . H14A H -0.1688 0.1497 0.0113 0.104 Uiso 1 1 calc R . . H14B H -0.3201 0.2010 0.0249 0.104 Uiso 1 1 calc R . . H14C H -0.3211 0.1250 0.0631 0.104 Uiso 1 1 calc R . . C13 C -0.2533(3) -0.06857(14) 0.29467(18) 0.0663(8) Uani 1 1 d . . . H13A H -0.3232 -0.1041 0.2700 0.099 Uiso 1 1 calc R . . H13B H -0.3205 -0.0378 0.3272 0.099 Uiso 1 1 calc R . . H13C H -0.1696 -0.0908 0.3285 0.099 Uiso 1 1 calc R . . C9 C 0.0211(3) 0.26402(11) 0.18032(17) 0.0530(7) Uani 1 1 d . . . H9A H 0.0915 0.3051 0.1723 0.064 Uiso 1 1 calc R . . H9B H -0.0561 0.2745 0.2236 0.064 Uiso 1 1 calc R . . C10 C -0.0724(3) 0.24807(13) 0.10520(15) 0.0518(7) Uani 1 1 d . . . H10A H -0.1397 0.2886 0.0890 0.062 Uiso 1 1 calc R . . H10B H 0.0045 0.2376 0.0618 0.062 Uiso 1 1 calc R . . C2 C 0.4138(3) -0.03955(12) 0.13007(16) 0.0544(7) Uani 1 1 d . . . H2A H 0.4117 -0.0690 0.1776 0.082 Uiso 1 1 calc R . . H2B H 0.5278 -0.0299 0.1162 0.082 Uiso 1 1 calc R . . H2C H 0.3587 -0.0635 0.0856 0.082 Uiso 1 1 calc R . . C1 C 0.2841(3) 0.09068(13) 0.05265(13) 0.0514(6) Uani 1 1 d . . . H1A H 0.2278 0.0606 0.0139 0.077 Uiso 1 1 calc R . . H1B H 0.3934 0.1023 0.0332 0.077 Uiso 1 1 calc R . . H1C H 0.2206 0.1333 0.0597 0.077 Uiso 1 1 calc R . . C5 C 0.4200(3) 0.09042(12) 0.45508(13) 0.0473(6) Uani 1 1 d . . . H5A H 0.4221 0.1411 0.4587 0.071 Uiso 1 1 calc R . . H5B H 0.5326 0.0727 0.4540 0.071 Uiso 1 1 calc R . . H5C H 0.3641 0.0714 0.5014 0.071 Uiso 1 1 calc R . . C4 C 0.2986(3) 0.26303(11) 0.33306(13) 0.0438(6) Uani 1 1 d . . . H4A H 0.2494 0.3084 0.3216 0.066 Uiso 1 1 calc R . . H4B H 0.4087 0.2695 0.3562 0.066 Uiso 1 1 calc R . . H4C H 0.2302 0.2379 0.3709 0.066 Uiso 1 1 calc R . . C11 C 0.0154(3) 0.08733(13) 0.43690(13) 0.0474(6) Uani 1 1 d . . . H11A H 0.0827 0.0713 0.4830 0.057 Uiso 1 1 calc R . . H11B H -0.0704 0.0521 0.4259 0.057 Uiso 1 1 calc R . . C7 C 0.0110(3) -0.02303(12) 0.12990(13) 0.0436(6) Uani 1 1 d . . . H7A H 0.0787 -0.0505 0.0930 0.052 Uiso 1 1 calc R . . H7B H -0.0689 0.0043 0.0978 0.052 Uiso 1 1 calc R . . C12 C -0.0627(3) 0.15490(13) 0.45615(13) 0.0458(6) Uani 1 1 d . . . H12A H -0.1334 0.1497 0.5032 0.055 Uiso 1 1 calc R . . H12B H 0.0227 0.1898 0.4689 0.055 Uiso 1 1 calc R . . C3 C 0.4252(3) 0.26825(11) 0.16576(13) 0.0412(5) Uani 1 1 d . . . H3A H 0.4220 0.2468 0.1128 0.062 Uiso 1 1 calc R . . H3B H 0.5395 0.2735 0.1837 0.062 Uiso 1 1 calc R . . H3C H 0.3728 0.3139 0.1631 0.062 Uiso 1 1 calc R . . C8 C -0.0780(3) -0.07036(11) 0.18449(15) 0.0433(6) Uani 1 1 d . . . H8A H -0.1474 -0.1029 0.1532 0.052 Uiso 1 1 calc R . . H8B H 0.0015 -0.0977 0.2168 0.052 Uiso 1 1 calc R . . C6 C 0.2855(3) -0.03325(10) 0.36610(13) 0.0404(5) Uani 1 1 d . . . H6A H 0.2278 -0.0460 0.4147 0.061 Uiso 1 1 calc R . . H6B H 0.3945 -0.0546 0.3667 0.061 Uiso 1 1 calc R . . H6C H 0.2229 -0.0496 0.3194 0.061 Uiso 1 1 calc R . . K1 K -0.10898(5) 0.10904(2) 0.24799(2) 0.02853(12) Uani 1 1 d . . . 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 Si3 0.0296(3) 0.0208(3) 0.0314(3) 0.0000(2) 0.0033(2) -0.0022(2) Si2 0.0273(3) 0.0306(3) 0.0262(3) -0.0066(2) 0.0036(2) -0.0015(2) Si4 0.0337(3) 0.0258(3) 0.0242(3) 0.0022(2) -0.0029(2) 0.0009(2) Si1 0.0250(3) 0.0235(3) 0.0280(3) -0.0020(2) -0.0002(2) -0.0005(2) O6 0.0472(9) 0.0566(11) 0.0435(10) -0.0148(8) 0.0030(8) 0.0157(8) O5 0.0404(9) 0.0557(10) 0.0359(9) 0.0138(7) -0.0046(7) -0.0029(8) O4 0.0349(8) 0.0258(8) 0.0763(11) 0.0046(8) 0.0170(8) 0.0000(7) O2 0.0319(8) 0.0230(8) 0.0621(10) 0.0051(7) -0.0069(7) 0.0023(6) O3 0.0384(8) 0.0467(9) 0.0274(8) 0.0091(7) 0.0091(6) 0.0087(7) O1 0.0305(8) 0.0386(8) 0.0343(8) -0.0135(7) 0.0037(6) -0.0093(6) C15 0.088(2) 0.075(2) 0.080(2) -0.0153(17) 0.0181(18) 0.0433(18) C14 0.0675(19) 0.091(2) 0.0491(16) 0.0014(15) -0.0202(14) 0.0105(16) C13 0.0578(17) 0.0462(16) 0.096(2) 0.0131(15) 0.0305(16) -0.0067(13) C9 0.0417(14) 0.0273(12) 0.090(2) 0.0103(13) -0.0046(13) 0.0068(10) C10 0.0430(14) 0.0531(16) 0.0594(16) 0.0292(13) 0.0054(12) 0.0124(12) C2 0.0449(14) 0.0483(15) 0.0698(17) -0.0300(13) -0.0003(13) 0.0055(12) C1 0.0593(16) 0.0661(17) 0.0287(12) -0.0020(12) -0.0003(11) -0.0147(13) C5 0.0608(16) 0.0472(14) 0.0335(13) -0.0011(11) -0.0103(11) -0.0020(12) C4 0.0577(15) 0.0299(12) 0.0442(14) -0.0051(10) 0.0122(11) -0.0006(11) C11 0.0515(15) 0.0566(16) 0.0345(13) 0.0123(11) 0.0136(11) 0.0008(12) C7 0.0372(13) 0.0495(14) 0.0439(13) -0.0174(11) -0.0035(10) -0.0107(11) C12 0.0500(14) 0.0569(16) 0.0308(12) -0.0076(11) 0.0130(11) -0.0062(12) C3 0.0503(14) 0.0300(12) 0.0436(13) 0.0049(10) 0.0101(11) -0.0030(10) C8 0.0344(12) 0.0279(12) 0.0676(16) -0.0109(11) -0.0015(11) -0.0029(10) C6 0.0513(14) 0.0306(12) 0.0393(13) 0.0074(10) -0.0016(11) -0.0030(10) K1 0.0297(2) 0.0265(2) 0.0295(2) 0.00018(18) 0.00141(18) 0.00051(18) _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 Si3 O2 1.6811(15) . ? Si3 C3 1.880(2) . ? Si3 C4 1.882(2) . ? Si3 Si1 2.3185(8) . ? Si2 O1 1.6800(14) . ? Si2 C1 1.879(2) . ? Si2 C2 1.882(2) . ? Si2 Si1 2.3198(8) . ? Si4 O3 1.6813(15) . ? Si4 C6 1.879(2) . ? Si4 C5 1.885(2) . ? Si4 Si1 2.3191(8) . ? Si1 K1 3.6607(7) 1_655 ? O6 C12 1.407(3) . ? O6 C15 1.415(3) . ? O6 K1 2.7511(15) . ? O5 C10 1.402(3) . ? O5 C14 1.416(3) . ? O5 K1 2.7238(15) . ? O4 C13 1.408(3) . ? O4 C8 1.413(3) . ? O4 K1 2.7420(15) . ? O2 C9 1.423(2) . ? O2 K1 2.7607(14) . ? O3 C11 1.420(2) . ? O3 K1 2.7283(14) . ? O1 C7 1.420(2) . ? O1 K1 2.7611(14) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 C10 1.495(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C11 C12 1.489(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C7 C8 1.490(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? K1 Si1 3.6607(7) 1_455 ? 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 O2 Si3 C3 105.69(9) . . ? O2 Si3 C4 105.78(9) . . ? C3 Si3 C4 106.25(10) . . ? O2 Si3 Si1 113.28(5) . . ? C3 Si3 Si1 110.21(7) . . ? C4 Si3 Si1 114.99(8) . . ? O1 Si2 C1 105.43(9) . . ? O1 Si2 C2 105.87(10) . . ? C1 Si2 C2 106.41(12) . . ? O1 Si2 Si1 113.10(5) . . ? C1 Si2 Si1 115.21(8) . . ? C2 Si2 Si1 110.18(8) . . ? O3 Si4 C6 105.55(9) . . ? O3 Si4 C5 105.94(10) . . ? C6 Si4 C5 106.30(10) . . ? O3 Si4 Si1 113.16(5) . . ? C6 Si4 Si1 115.27(8) . . ? C5 Si4 Si1 109.98(8) . . ? Si3 Si1 Si4 99.10(3) . . ? Si3 Si1 Si2 99.75(3) . . ? Si4 Si1 Si2 99.80(3) . . ? Si3 Si1 K1 115.84(2) . 1_655 ? Si4 Si1 K1 120.33(2) . 1_655 ? Si2 Si1 K1 118.25(2) . 1_655 ? C12 O6 C15 112.92(19) . . ? C12 O6 K1 117.17(12) . . ? C15 O6 K1 126.99(16) . . ? C10 O5 C14 113.81(19) . . ? C10 O5 K1 118.67(12) . . ? C14 O5 K1 122.02(15) . . ? C13 O4 C8 113.29(17) . . ? C13 O4 K1 123.58(15) . . ? C8 O4 K1 118.31(12) . . ? C9 O2 Si3 124.03(13) . . ? C9 O2 K1 102.86(12) . . ? Si3 O2 K1 125.25(7) . . ? C11 O3 Si4 125.08(13) . . ? C11 O3 K1 102.57(12) . . ? Si4 O3 K1 126.04(7) . . ? C7 O1 Si2 124.19(13) . . ? C7 O1 K1 103.26(12) . . ? Si2 O1 K1 125.10(7) . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C9 C10 109.22(19) . . ? O2 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O2 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? O5 C10 C9 108.55(18) . . ? O5 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O5 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C11 C12 109.65(18) . . ? O3 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O3 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O1 C7 C8 109.44(18) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O6 C12 C11 108.80(18) . . ? O6 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? O6 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? Si3 C3 H3A 109.5 . . ? Si3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O4 C8 C7 108.37(17) . . ? O4 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O4 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O5 K1 O3 140.27(5) . . ? O5 K1 O4 117.70(5) . . ? O3 K1 O4 95.46(5) . . ? O5 K1 O6 112.65(5) . . ? O3 K1 O6 60.39(4) . . ? O4 K1 O6 120.14(5) . . ? O5 K1 O2 60.52(4) . . ? O3 K1 O2 80.08(4) . . ? O4 K1 O2 140.72(4) . . ? O6 K1 O2 91.68(5) . . ? O5 K1 O1 96.88(5) . . ? O3 K1 O1 80.33(4) . . ? O4 K1 O1 60.33(4) . . ? O6 K1 O1 140.72(5) . . ? O2 K1 O1 80.54(4) . . ? O5 K1 Si1 80.78(3) . 1_455 ? O3 K1 Si1 130.44(3) . 1_455 ? O4 K1 Si1 77.42(3) . 1_455 ? O6 K1 Si1 80.87(4) . 1_455 ? O2 K1 Si1 134.17(3) . 1_455 ? O1 K1 Si1 130.94(3) . 1_455 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.93 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.257 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.040 # Attachment '- Li-4 with checkcif.txt' data_ljhw_krempner_2_0m _database_code_depnum_ccdc_archive 'CCDC 807151' #TrackingRef '- Li-4 with checkcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H Li O6 Si4' _chemical_formula_weight 396.46 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' Li Li -0.0003 0.0001 '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 ? _symmetry_space_group_name_H-M ? 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 34.560(2) _cell_length_b 9.6993(7) _cell_length_c 17.1971(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.9710(10) _cell_angle_gamma 90.00 _cell_volume 5091.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21754 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 23.73 _reflns_number_total 3859 _reflns_number_gt 3238 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^+4.8777P] 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 0.00000(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3859 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 3.483 _refine_ls_shift/su_mean 0.014 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 C1 C 0.91974(7) 0.6287(2) 0.97566(15) 0.0416(6) Uani 1 1 d . . . H1A H 0.9449 0.5722 0.9842 0.062 Uiso 1 1 calc R . . H1B H 0.9263 0.6766 1.0307 0.062 Uiso 1 1 calc R . . H1C H 0.9137 0.6967 0.9292 0.062 Uiso 1 1 calc R . . C2 C 0.82335(7) 0.6362(2) 0.91687(16) 0.0423(6) Uani 1 1 d . . . H2A H 0.8167 0.6872 0.8628 0.063 Uiso 1 1 calc R . . H2B H 0.8312 0.7012 0.9656 0.063 Uiso 1 1 calc R . . H2C H 0.7976 0.5829 0.9085 0.063 Uiso 1 1 calc R . . C3 C 0.76691(7) 0.2888(2) 0.88228(17) 0.0477(6) Uani 1 1 d . . . H3A H 0.7681 0.3592 0.8426 0.071 Uiso 1 1 calc R . . H3B H 0.7580 0.3315 0.9231 0.071 Uiso 1 1 calc R . . H3C H 0.7456 0.2176 0.8478 0.071 Uiso 1 1 calc R . . C4 C 0.81370(8) 0.0538(2) 1.00211(16) 0.0449(6) Uani 1 1 d . . . H4A H 0.7894 -0.0013 0.9588 0.067 Uiso 1 1 calc R . . H4B H 0.8067 0.0845 1.0484 0.067 Uiso 1 1 calc R . . H4C H 0.8404 -0.0022 1.0282 0.067 Uiso 1 1 calc R . . C5 C 0.94261(9) 0.0533(3) 1.08539(19) 0.0623(8) Uani 1 1 d . . . H5A H 0.9164 0.0002 1.0472 0.093 Uiso 1 1 calc R . . H5B H 0.9472 0.0501 1.1461 0.093 Uiso 1 1 calc R . . H5C H 0.9681 0.0138 1.0830 0.093 Uiso 1 1 calc R . . C6 C 0.98869(7) 0.3253(3) 1.12024(16) 0.0578(7) Uani 1 1 d . . . H6A H 1.0131 0.2657 1.1277 0.087 Uiso 1 1 calc R . . H6B H 0.9904 0.3435 1.1778 0.087 Uiso 1 1 calc R . . H6C H 0.9903 0.4126 1.0933 0.087 Uiso 1 1 calc R . . C7 C 0.85453(7) 0.5236(2) 0.77129(13) 0.0349(5) Uani 1 1 d . . . H7A H 0.8815 0.5244 0.7646 0.042 Uiso 1 1 calc R . . H7B H 0.8472 0.6199 0.7783 0.042 Uiso 1 1 calc R . . C8 C 0.81768(7) 0.4600(2) 0.69211(14) 0.0351(5) Uani 1 1 d . . . H8A H 0.7899 0.4691 0.6954 0.042 Uiso 1 1 calc R . . H8B H 0.8141 0.5066 0.6379 0.042 Uiso 1 1 calc R . . C9 C 0.80988(7) 0.0407(2) 0.80841(14) 0.0360(5) Uani 1 1 d . . . H9A H 0.7891 0.0827 0.7515 0.043 Uiso 1 1 calc R . . H9B H 0.7929 -0.0113 0.8316 0.043 Uiso 1 1 calc R . . C10 C 0.84042(7) -0.0539(2) 0.79557(15) 0.0386(5) Uani 1 1 d . . . H10B H 0.8598 -0.1013 0.8515 0.046 Uiso 1 1 calc R . . H10A H 0.8236 -0.1247 0.7509 0.046 Uiso 1 1 calc R . . C13 C 0.79588(8) 0.2498(3) 0.61550(14) 0.0478(6) Uani 1 1 d . . . H13A H 0.7675 0.2558 0.6152 0.072 Uiso 1 1 calc R . . H13B H 0.8041 0.1527 0.6170 0.072 Uiso 1 1 calc R . . H13C H 0.7938 0.2934 0.5623 0.072 Uiso 1 1 calc R . . C14 C 0.89520(8) -0.0580(3) 0.75166(17) 0.0519(7) Uani 1 1 d . . . H14A H 0.9147 -0.1073 0.8058 0.078 Uiso 1 1 calc R . . H14B H 0.9127 0.0003 0.7334 0.078 Uiso 1 1 calc R . . H14C H 0.8785 -0.1248 0.7051 0.078 Uiso 1 1 calc R . . C15 C 0.92554(8) 0.3142(3) 0.70908(15) 0.0545(7) Uani 1 1 d . . . H15A H 0.9356 0.4102 0.7204 0.082 Uiso 1 1 calc R . . H15B H 0.8957 0.3109 0.6602 0.082 Uiso 1 1 calc R . . H15C H 0.9451 0.2606 0.6938 0.082 Uiso 1 1 calc R . . C16 C 0.96677(6) 0.1792(2) 0.93146(13) 0.0339(5) Uani 1 1 d . . . H11A H 0.9616 0.0808 0.9145 0.041 Uiso 1 1 calc R . . H11B H 0.9950 0.1872 0.9860 0.041 Uiso 1 1 calc R . . C17 C 0.96821(7) 0.2614(2) 0.85944(14) 0.0383(5) Uani 1 1 d . . . H12A H 0.9767 0.3578 0.8789 0.046 Uiso 1 1 calc R . . H12B H 0.9901 0.2217 0.8439 0.046 Uiso 1 1 calc R . . Li1 Li 0.87488(10) 0.2428(3) 0.8255(2) 0.0280(7) Uani 1 1 d . . . O1 O 0.86147(4) 0.44382(13) 0.84668(8) 0.0308(3) Uani 1 1 d . . . O2 O 0.83514(4) 0.14552(13) 0.86921(9) 0.0307(3) Uani 1 1 d . . . O3 O 0.93209(4) 0.23143(14) 0.94599(8) 0.0299(3) Uani 1 1 d . . . O4 O 0.82819(4) 0.31845(14) 0.69094(8) 0.0317(3) Uani 1 1 d . . . O5 O 0.86572(5) 0.02574(14) 0.76726(9) 0.0354(4) Uani 1 1 d . . . O6 O 0.92604(4) 0.25770(14) 0.78562(9) 0.0328(3) Uani 1 1 d . . . Si1 Si 0.876363(18) 0.35208(6) 1.04649(4) 0.02855(15) Uani 1 1 d . . . Si2 Si 0.870598(18) 0.51540(5) 0.94313(4) 0.02636(15) Uani 1 1 d . . . Si3 Si 0.822482(18) 0.20841(6) 0.94623(4) 0.02762(15) Uani 1 1 d . . . Si4 Si 0.935238(18) 0.23682(6) 1.04696(4) 0.02958(16) Uani 1 1 d . . . 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 C1 0.0396(13) 0.0415(13) 0.0408(13) -0.0015(11) 0.0165(11) -0.0115(11) C2 0.0451(14) 0.0305(12) 0.0615(15) 0.0046(11) 0.0336(12) 0.0061(10) C3 0.0311(13) 0.0412(14) 0.0649(17) -0.0011(12) 0.0177(12) 0.0022(10) C4 0.0510(15) 0.0417(14) 0.0485(15) 0.0040(11) 0.0288(12) -0.0089(11) C5 0.0703(19) 0.0560(17) 0.088(2) 0.0384(15) 0.0605(17) 0.0335(14) C6 0.0352(14) 0.088(2) 0.0418(14) -0.0127(14) 0.0114(11) 0.0005(14) C7 0.0494(14) 0.0230(11) 0.0326(12) 0.0048(9) 0.0196(11) 0.0029(10) C8 0.0397(13) 0.0338(12) 0.0315(12) 0.0071(9) 0.0165(10) 0.0101(10) C9 0.0333(12) 0.0344(12) 0.0417(13) -0.0106(10) 0.0189(11) -0.0125(10) C10 0.0426(13) 0.0277(12) 0.0458(14) -0.0061(10) 0.0209(11) -0.0076(10) C13 0.0522(15) 0.0528(15) 0.0306(13) -0.0096(11) 0.0128(11) -0.0074(12) C14 0.0579(16) 0.0476(15) 0.0619(17) -0.0138(13) 0.0380(14) 0.0046(12) C15 0.0502(15) 0.0829(19) 0.0432(14) 0.0221(14) 0.0325(13) 0.0152(14) C16 0.0244(11) 0.0469(13) 0.0325(12) 0.0020(10) 0.0151(9) 0.0066(10) C17 0.0263(12) 0.0525(14) 0.0398(13) 0.0030(11) 0.0186(10) 0.0011(10) Li1 0.0278(18) 0.0305(18) 0.0297(18) 0.0008(14) 0.0168(15) 0.0002(14) O1 0.0424(8) 0.0222(7) 0.0259(7) 0.0014(6) 0.0143(7) 0.0030(6) O2 0.0325(8) 0.0277(8) 0.0356(8) -0.0088(6) 0.0190(7) -0.0101(6) O3 0.0218(7) 0.0433(9) 0.0269(8) 0.0011(6) 0.0135(6) 0.0064(6) O4 0.0307(8) 0.0323(8) 0.0285(8) -0.0041(6) 0.0107(6) 0.0019(6) O5 0.0406(9) 0.0290(8) 0.0441(9) -0.0026(7) 0.0263(8) 0.0011(7) O6 0.0282(8) 0.0449(9) 0.0290(8) 0.0077(6) 0.0166(7) 0.0026(7) Si1 0.0323(3) 0.0298(3) 0.0287(3) -0.0024(2) 0.0185(3) 0.0010(2) Si2 0.0274(3) 0.0226(3) 0.0309(3) -0.0033(2) 0.0152(3) -0.0006(2) Si3 0.0267(3) 0.0263(3) 0.0352(3) 0.0019(2) 0.0189(3) 0.0001(2) Si4 0.0281(3) 0.0360(3) 0.0265(3) 0.0052(2) 0.0144(3) 0.0054(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 C1 Si2 1.875(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si2 1.884(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si3 1.877(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 Si3 1.881(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si4 1.874(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si4 1.885(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O1 1.430(2) . ? C7 C8 1.493(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O4 1.423(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O2 1.426(2) . ? C9 C10 1.491(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O5 1.413(2) . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? C13 O4 1.419(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O5 1.424(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O6 1.419(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O3 1.427(2) . ? C16 C17 1.493(3) . ? C16 H11A 0.9900 . ? C16 H11B 0.9900 . ? C17 O6 1.415(2) . ? C17 H12A 0.9900 . ? C17 H12B 0.9900 . ? Li1 O2 2.076(3) . ? Li1 O1 2.076(3) . ? Li1 O3 2.091(3) . ? Li1 O6 2.181(3) . ? Li1 O4 2.235(3) . ? Li1 O5 2.289(3) . ? O1 Si2 1.6858(14) . ? O2 Si3 1.6916(14) . ? O3 Si4 1.6888(14) . ? Si1 Si3 2.3175(8) . ? Si1 Si4 2.3184(8) . ? Si1 Si2 2.3186(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 Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si3 C3 H3A 109.5 . . ? Si3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 108.18(17) . . ? O1 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O4 C8 C7 107.29(16) . . ? O4 C8 H8A 110.3 . . ? C7 C8 H8A 110.3 . . ? O4 C8 H8B 110.3 . . ? C7 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? O2 C9 C10 108.37(17) . . ? O2 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O2 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O5 C10 C9 108.03(17) . . ? O5 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? O5 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? H10B C10 H10A 108.4 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 C17 108.28(17) . . ? O3 C16 H11A 110.0 . . ? C17 C16 H11A 110.0 . . ? O3 C16 H11B 110.0 . . ? C17 C16 H11B 110.0 . . ? H11A C16 H11B 108.4 . . ? O6 C17 C16 108.05(16) . . ? O6 C17 H12A 110.1 . . ? C16 C17 H12A 110.1 . . ? O6 C17 H12B 110.1 . . ? C16 C17 H12B 110.1 . . ? H12A C17 H12B 108.4 . . ? O2 Li1 O1 97.09(14) . . ? O2 Li1 O3 95.52(14) . . ? O1 Li1 O3 93.49(14) . . ? O2 Li1 O6 156.32(18) . . ? O1 Li1 O6 105.87(14) . . ? O3 Li1 O6 77.63(12) . . ? O2 Li1 O4 104.19(14) . . ? O1 Li1 O4 76.17(12) . . ? O3 Li1 O4 158.64(17) . . ? O6 Li1 O4 87.16(12) . . ? O2 Li1 O5 76.19(11) . . ? O1 Li1 O5 160.82(18) . . ? O3 Li1 O5 104.94(14) . . ? O6 Li1 O5 83.65(12) . . ? O4 Li1 O5 87.95(12) . . ? C7 O1 Si2 122.93(12) . . ? C7 O1 Li1 107.80(14) . . ? Si2 O1 Li1 127.25(11) . . ? C9 O2 Si3 122.49(12) . . ? C9 O2 Li1 109.88(14) . . ? Si3 O2 Li1 125.28(12) . . ? C16 O3 Si4 122.45(12) . . ? C16 O3 Li1 109.08(14) . . ? Si4 O3 Li1 126.31(11) . . ? C13 O4 C8 111.67(16) . . ? C13 O4 Li1 131.97(16) . . ? C8 O4 Li1 111.55(14) . . ? C10 O5 C14 111.46(16) . . ? C10 O5 Li1 109.46(14) . . ? C14 O5 Li1 130.02(15) . . ? C17 O6 C15 112.45(16) . . ? C17 O6 Li1 111.44(14) . . ? C15 O6 Li1 131.21(15) . . ? Si3 Si1 Si4 96.33(3) . . ? Si3 Si1 Si2 95.18(3) . . ? Si4 Si1 Si2 95.27(3) . . ? O1 Si2 C1 105.09(9) . . ? O1 Si2 C2 106.20(9) . . ? C1 Si2 C2 105.60(11) . . ? O1 Si2 Si1 112.46(5) . . ? C1 Si2 Si1 115.58(8) . . ? C2 Si2 Si1 111.20(7) . . ? O2 Si3 C3 105.09(10) . . ? O2 Si3 C4 106.00(9) . . ? C3 Si3 C4 105.33(11) . . ? O2 Si3 Si1 112.75(5) . . ? C3 Si3 Si1 115.49(8) . . ? C4 Si3 Si1 111.42(8) . . ? O3 Si4 C5 105.41(10) . . ? O3 Si4 C6 105.78(9) . . ? C5 Si4 C6 105.54(13) . . ? O3 Si4 Si1 112.22(5) . . ? C5 Si4 Si1 115.67(8) . . ? C6 Si4 Si1 111.48(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.291 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.040 # Attachment '- Na-4 with checkcif.txt' data_krempner1a _database_code_depnum_ccdc_archive 'CCDC 807152' #TrackingRef '- Na-4 with checkcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H Na O6 Si4' _chemical_formula_weight 412.51 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' Na Na 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6614(18) _cell_length_b 9.8943(12) _cell_length_c 17.206(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2666.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8855 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18024 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3658 _reflns_number_gt 2398 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0082P)^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 0.00000(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3658 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0615 _refine_ls_goodness_of_fit_ref 0.815 _refine_ls_restrained_S_all 0.815 _refine_ls_shift/su_max 0.810 _refine_ls_shift/su_mean 0.003 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 Na1 Na 0.75015(6) 0.49825(9) 0.30163(5) 0.0287(2) Uani 1 1 d . . . Si1 Si 0.74558(4) 0.61453(7) 0.07902(4) 0.03410(19) Uani 1 1 d . . . Si2 Si 0.72917(4) 0.77796(7) 0.17466(4) 0.03152(18) Uani 1 1 d . . . Si3 Si 0.86781(5) 0.51364(8) 0.12809(4) 0.03474(19) Uani 1 1 d . . . Si4 Si 0.64364(4) 0.46235(7) 0.12245(4) 0.03070(17) Uani 1 1 d . . . O1 O 0.70840(11) 0.71221(15) 0.26233(9) 0.0362(4) Uani 1 1 d . . . O2 O 0.87293(10) 0.51844(18) 0.22612(9) 0.0405(5) Uani 1 1 d . . . O3 O 0.66931(10) 0.38909(15) 0.20764(9) 0.0329(4) Uani 1 1 d . . . O4 O 0.65439(10) 0.58914(16) 0.39533(9) 0.0358(4) Uani 1 1 d . . . O5 O 0.86950(12) 0.5101(2) 0.38601(9) 0.0493(5) Uani 1 1 d . . . O6 O 0.72454(11) 0.27229(16) 0.34466(10) 0.0406(4) Uani 1 1 d . . . C1 C 0.82586(17) 0.8885(3) 0.18790(16) 0.0474(7) Uani 1 1 d . . . H1A H 0.8148 0.9548 0.2290 0.071 Uiso 1 1 calc R . . H1B H 0.8382 0.9359 0.1392 0.071 Uiso 1 1 calc R . . H1C H 0.8749 0.8325 0.2024 0.071 Uiso 1 1 calc R . . C2 C 0.63787(18) 0.8956(3) 0.15360(17) 0.0504(8) Uani 1 1 d . . . H2A H 0.5882 0.8431 0.1365 0.076 Uiso 1 1 calc R . . H2B H 0.6545 0.9590 0.1126 0.076 Uiso 1 1 calc R . . H2C H 0.6232 0.9460 0.2008 0.076 Uiso 1 1 calc R . . C3 C 0.96704(17) 0.6026(3) 0.09306(16) 0.0540(8) Uani 1 1 d . . . H3A H 0.9698 0.6931 0.1161 0.081 Uiso 1 1 calc R . . H3B H 0.9654 0.6102 0.0363 0.081 Uiso 1 1 calc R . . H3C H 1.0175 0.5507 0.1086 0.081 Uiso 1 1 calc R . . C4 C 0.88045(18) 0.3307(3) 0.10092(17) 0.0533(8) Uani 1 1 d . . . H4A H 0.9325 0.2947 0.1247 0.080 Uiso 1 1 calc R . . H4B H 0.8844 0.3225 0.0443 0.080 Uiso 1 1 calc R . . H4C H 0.8310 0.2795 0.1196 0.080 Uiso 1 1 calc R . . C5 C 0.53539(16) 0.5385(3) 0.13688(18) 0.0498(8) Uani 1 1 d . . . H5A H 0.4947 0.4673 0.1510 0.075 Uiso 1 1 calc R . . H5B H 0.5169 0.5821 0.0886 0.075 Uiso 1 1 calc R . . H5C H 0.5380 0.6058 0.1786 0.075 Uiso 1 1 calc R . . C6 C 0.62788(18) 0.3180(3) 0.05275(16) 0.0508(8) Uani 1 1 d . . . H6A H 0.6814 0.2675 0.0475 0.076 Uiso 1 1 calc R . . H6B H 0.6108 0.3534 0.0019 0.076 Uiso 1 1 calc R . . H6C H 0.5832 0.2578 0.0726 0.076 Uiso 1 1 calc R . . C7 C 0.69613(18) 0.7887(2) 0.33143(14) 0.0416(7) Uani 1 1 d . . . H7A H 0.6791 0.8822 0.3180 0.050 Uiso 1 1 calc R . . H7B H 0.7501 0.7928 0.3612 0.050 Uiso 1 1 calc R . . C8 C 0.62849(16) 0.7240(2) 0.37932(14) 0.0397(6) Uani 1 1 d . . . H8A H 0.6207 0.7745 0.4285 0.048 Uiso 1 1 calc R . . H8B H 0.5736 0.7239 0.3508 0.048 Uiso 1 1 calc R . . C9 C 0.94520(18) 0.4763(4) 0.26922(16) 0.0677(10) Uani 1 1 d . . . H9A H 0.9981 0.4999 0.2407 0.081 Uiso 1 1 calc R . . H9B H 0.9438 0.3771 0.2765 0.081 Uiso 1 1 calc R . . C10 C 0.94440(18) 0.5455(3) 0.34684(17) 0.0604(9) Uani 1 1 d . . . H10A H 0.9948 0.5174 0.3776 0.072 Uiso 1 1 calc R . . H10B H 0.9468 0.6447 0.3397 0.072 Uiso 1 1 calc R . . C11 C 0.61920(16) 0.2897(2) 0.24597(15) 0.0393(7) Uani 1 1 d . . . H11A H 0.5854 0.2383 0.2074 0.047 Uiso 1 1 calc R . . H11B H 0.5791 0.3339 0.2824 0.047 Uiso 1 1 calc R . . C12 C 0.67684(18) 0.1958(2) 0.28957(16) 0.0428(7) Uani 1 1 d . . . H12A H 0.6426 0.1261 0.3166 0.051 Uiso 1 1 calc R . . H12B H 0.7161 0.1498 0.2530 0.051 Uiso 1 1 calc R . . C13 C 0.5902(2) 0.5166(3) 0.43607(16) 0.0598(9) Uani 1 1 d . . . H13A H 0.5779 0.5623 0.4854 0.090 Uiso 1 1 calc R . . H13B H 0.6102 0.4245 0.4464 0.090 Uiso 1 1 calc R . . H13C H 0.5382 0.5131 0.4045 0.090 Uiso 1 1 calc R . . C14 C 0.8645(2) 0.5644(4) 0.46323(17) 0.0903(14) Uani 1 1 d . . . H14A H 0.9103 0.5261 0.4951 0.135 Uiso 1 1 calc R . . H14B H 0.8091 0.5414 0.4861 0.135 Uiso 1 1 calc R . . H14C H 0.8707 0.6629 0.4612 0.135 Uiso 1 1 calc R . . C15 C 0.7865(2) 0.1911(3) 0.38312(17) 0.0603(9) Uani 1 1 d . . . H15A H 0.7579 0.1164 0.4100 0.090 Uiso 1 1 calc R . . H15B H 0.8177 0.2463 0.4210 0.090 Uiso 1 1 calc R . . H15C H 0.8267 0.1545 0.3448 0.090 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 Na1 0.0278(5) 0.0282(5) 0.0301(5) 0.0004(4) -0.0017(4) 0.0020(4) Si1 0.0331(4) 0.0410(4) 0.0282(4) 0.0044(3) -0.0028(3) -0.0024(3) Si2 0.0301(4) 0.0283(4) 0.0362(4) 0.0061(3) -0.0029(3) -0.0020(3) Si3 0.0259(4) 0.0474(4) 0.0309(4) -0.0034(3) 0.0010(3) 0.0022(3) Si4 0.0259(4) 0.0339(4) 0.0323(4) -0.0025(3) -0.0065(3) -0.0013(3) O1 0.0510(12) 0.0250(9) 0.0325(10) -0.0012(7) 0.0096(8) 0.0060(8) O2 0.0240(9) 0.0673(12) 0.0302(9) -0.0004(9) -0.0018(7) 0.0085(9) O3 0.0313(9) 0.0294(9) 0.0380(9) 0.0058(8) -0.0062(8) -0.0082(8) O4 0.0355(10) 0.0363(10) 0.0355(10) 0.0046(8) 0.0062(8) 0.0041(8) O5 0.0424(12) 0.0757(13) 0.0299(10) -0.0118(10) -0.0070(9) 0.0102(11) O6 0.0479(11) 0.0304(9) 0.0434(10) 0.0062(8) -0.0081(9) 0.0039(9) C1 0.0428(17) 0.0462(17) 0.0534(18) -0.0029(14) 0.0017(14) -0.0103(14) C2 0.0502(18) 0.0338(15) 0.0673(19) 0.0059(14) -0.0134(16) 0.0068(14) C3 0.0354(16) 0.075(2) 0.0514(18) -0.0084(16) 0.0106(14) -0.0050(16) C4 0.0438(18) 0.0548(18) 0.0614(19) -0.0090(15) -0.0049(15) 0.0110(15) C5 0.0307(15) 0.0435(18) 0.075(2) 0.0047(15) -0.0008(15) 0.0002(13) C6 0.0506(18) 0.0547(18) 0.0470(17) -0.0152(14) -0.0077(14) -0.0105(15) C7 0.0536(18) 0.0287(14) 0.0424(16) -0.0017(12) 0.0055(14) 0.0027(13) C8 0.0418(16) 0.0406(16) 0.0367(15) -0.0057(13) 0.0033(13) 0.0144(14) C9 0.0331(17) 0.132(3) 0.0384(17) 0.0014(19) -0.0062(13) 0.0243(19) C10 0.0370(18) 0.094(3) 0.0501(18) -0.0008(18) -0.0202(15) -0.0019(17) C11 0.0364(15) 0.0350(15) 0.0465(16) 0.0038(13) -0.0025(13) -0.0081(13) C12 0.0476(17) 0.0287(14) 0.0522(17) 0.0060(13) 0.0024(14) -0.0063(13) C13 0.067(2) 0.067(2) 0.0448(17) 0.0122(16) 0.0217(16) -0.0070(18) C14 0.073(3) 0.153(4) 0.045(2) -0.038(2) -0.0222(18) 0.036(3) C15 0.072(2) 0.0497(19) 0.060(2) 0.0168(16) -0.0206(17) 0.0085(17) _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 Na1 O1 2.3166(17) . ? Na1 O3 2.3205(17) . ? Na1 O2 2.3292(19) . ? Na1 O5 2.3698(19) . ? Na1 O4 2.3785(17) . ? Na1 O6 2.3891(18) . ? Si1 Si3 2.3181(10) . ? Si1 Si4 2.3183(10) . ? Si1 Si2 2.3214(10) . ? Si2 O1 1.6747(16) . ? Si2 C2 1.879(3) . ? Si2 C1 1.882(3) . ? Si3 O2 1.6893(17) . ? Si3 C4 1.880(3) . ? Si3 C3 1.885(3) . ? Si4 O3 1.6838(17) . ? Si4 C5 1.872(3) . ? Si4 C6 1.881(3) . ? O1 C7 1.423(3) . ? O2 C9 1.416(3) . ? O3 C11 1.421(3) . ? O4 C13 1.420(3) . ? O4 C8 1.421(3) . ? O5 C10 1.397(3) . ? O5 C14 1.435(3) . ? O6 C15 1.424(3) . ? O6 C12 1.425(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.487(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.497(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 Na1 O3 93.89(6) . . ? O1 Na1 O2 89.53(7) . . ? O3 Na1 O2 95.83(7) . . ? O1 Na1 O5 110.87(7) . . ? O3 Na1 O5 151.69(7) . . ? O2 Na1 O5 71.72(6) . . ? O1 Na1 O4 71.00(6) . . ? O3 Na1 O4 107.72(7) . . ? O2 Na1 O4 150.02(7) . . ? O5 Na1 O4 93.63(7) . . ? O1 Na1 O6 153.93(7) . . ? O3 Na1 O6 71.87(6) . . ? O2 Na1 O6 113.06(7) . . ? O5 Na1 O6 89.37(7) . . ? O4 Na1 O6 92.17(6) . . ? Si3 Si1 Si4 99.88(4) . . ? Si3 Si1 Si2 97.65(4) . . ? Si4 Si1 Si2 98.49(4) . . ? O1 Si2 C2 105.45(11) . . ? O1 Si2 C1 105.85(11) . . ? C2 Si2 C1 106.01(12) . . ? O1 Si2 Si1 112.92(6) . . ? C2 Si2 Si1 112.27(10) . . ? C1 Si2 Si1 113.68(9) . . ? O2 Si3 C4 105.69(12) . . ? O2 Si3 C3 105.49(11) . . ? C4 Si3 C3 106.45(13) . . ? O2 Si3 Si1 113.00(7) . . ? C4 Si3 Si1 114.27(9) . . ? C3 Si3 Si1 111.30(10) . . ? O3 Si4 C5 105.90(11) . . ? O3 Si4 C6 105.04(11) . . ? C5 Si4 C6 105.73(13) . . ? O3 Si4 Si1 113.32(6) . . ? C5 Si4 Si1 113.91(9) . . ? C6 Si4 Si1 112.20(10) . . ? C7 O1 Si2 124.92(13) . . ? C7 O1 Na1 106.29(13) . . ? Si2 O1 Na1 124.27(8) . . ? C9 O2 Si3 123.55(16) . . ? C9 O2 Na1 110.03(15) . . ? Si3 O2 Na1 121.02(9) . . ? C11 O3 Si4 124.77(14) . . ? C11 O3 Na1 107.46(13) . . ? Si4 O3 Na1 122.45(8) . . ? C13 O4 C8 111.57(19) . . ? C13 O4 Na1 126.16(16) . . ? C8 O4 Na1 113.80(13) . . ? C10 O5 C14 113.5(2) . . ? C10 O5 Na1 112.27(14) . . ? C14 O5 Na1 122.86(19) . . ? C15 O6 C12 111.52(19) . . ? C15 O6 Na1 123.91(16) . . ? C12 O6 Na1 112.29(13) . . ? Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si3 C3 H3A 109.5 . . ? Si3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 109.3(2) . . ? O1 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O1 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? O4 C8 C7 107.97(19) . . ? O4 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O4 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? O2 C9 C10 109.0(2) . . ? O2 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O2 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O5 C10 C9 108.8(2) . . ? O5 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O5 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O3 C11 C12 109.2(2) . . ? O3 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O3 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? O6 C12 C11 108.63(19) . . ? O6 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? O6 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.3 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.782 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.782 _refine_diff_density_max 0.173 _refine_diff_density_min -0.137 _refine_diff_density_rms 0.035 # Attachment '- Na-5 with checkcif.txt' data_krempner_3_final _database_code_depnum_ccdc_archive 'CCDC 807153' #TrackingRef '- Na-5 with checkcif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H45 Na O6 Si4' _chemical_formula_weight 492.89 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' Na Na 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M ? 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 11.248(4) _cell_length_b 15.467(5) _cell_length_c 16.551(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2879.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9300 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13489 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 22.15 _reflns_number_total 2661 _reflns_number_gt 1839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^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 0.00013(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2661 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _refine_ls_shift/su_max 0.001 _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 C1 C 0.5780(3) 0.8445(2) 1.22409(17) 0.0507(10) Uani 1 1 d . . . H1A H 0.5137 0.8868 1.2178 0.076 Uiso 1 1 calc R . . H1B H 0.6236 0.8579 1.2730 0.076 Uiso 1 1 calc R . . H1C H 0.5441 0.7864 1.2286 0.076 Uiso 1 1 calc R . . C2 C 0.7293(3) 0.96525(18) 1.12583(19) 0.0487(10) Uani 1 1 d . . . H2A H 0.7753 0.9735 1.0761 0.073 Uiso 1 1 calc R . . H2B H 0.7790 0.9794 1.1726 0.073 Uiso 1 1 calc R . . H2C H 0.6596 1.0032 1.1250 0.073 Uiso 1 1 calc R . . C3 C 0.6116(3) 0.5969(2) 1.17557(18) 0.0509(10) Uani 1 1 d . . . H3B H 0.5490 0.6401 1.1678 0.076 Uiso 1 1 calc R . . H3A H 0.6365 0.5967 1.2323 0.076 Uiso 1 1 calc R . . H3C H 0.5811 0.5396 1.1610 0.076 Uiso 1 1 calc R . . C4 C 0.8446(3) 0.52850(18) 1.1201(2) 0.0513(10) Uani 1 1 d . . . H4B H 0.8040 0.4764 1.1007 0.077 Uiso 1 1 calc R . . H4A H 0.8660 0.5211 1.1771 0.077 Uiso 1 1 calc R . . H4C H 0.9167 0.5381 1.0881 0.077 Uiso 1 1 calc R . . C5 C 1.0336(3) 0.87650(19) 1.0280(2) 0.0454(9) Uani 1 1 d . . . H5A H 1.0704 0.8869 0.9752 0.068 Uiso 1 1 calc R . . H5B H 1.0959 0.8671 1.0685 0.068 Uiso 1 1 calc R . . H5C H 0.9857 0.9268 1.0433 0.068 Uiso 1 1 calc R . . C6 C 1.0374(3) 0.6861(2) 0.99240(19) 0.0477(9) Uani 1 1 d . . . H6A H 0.9910 0.6328 0.9870 0.072 Uiso 1 1 calc R . . H6B H 1.0983 0.6783 1.0341 0.072 Uiso 1 1 calc R . . H6C H 1.0757 0.6996 0.9407 0.072 Uiso 1 1 calc R . . C7 C 0.4831(3) 0.8748(2) 1.0377(2) 0.0463(9) Uani 1 1 d . . . H7A H 0.4793 0.8936 0.9806 0.056 Uiso 1 1 calc R . . H7B H 0.4782 0.9269 1.0723 0.056 Uiso 1 1 calc R . . C8 C 0.3777(3) 0.8153(2) 1.0560(2) 0.0578(11) Uani 1 1 d . . . H8A H 0.3673 0.8108 1.1153 0.069 Uiso 1 1 calc R . . H8B H 0.3043 0.8409 1.0332 0.069 Uiso 1 1 calc R . . C9 C 0.3955(3) 0.7257(2) 1.0210(2) 0.0514(10) Uani 1 1 d . . . H9A H 0.4536 0.6941 1.0548 0.062 Uiso 1 1 calc R . . H9B H 0.3191 0.6939 1.0236 0.062 Uiso 1 1 calc R . . C10 C 0.6469(3) 0.54878(17) 0.97361(18) 0.0378(8) Uani 1 1 d . . . H10A H 0.5678 0.5624 0.9507 0.045 Uiso 1 1 calc R . . H10B H 0.6369 0.5015 1.0134 0.045 Uiso 1 1 calc R . . C11 C 0.7293(3) 0.51895(18) 0.90632(18) 0.0412(9) Uani 1 1 d . . . H11A H 0.6865 0.4769 0.8719 0.049 Uiso 1 1 calc R . . H11B H 0.7984 0.4889 0.9304 0.049 Uiso 1 1 calc R . . C12 C 0.7737(3) 0.59316(19) 0.85372(18) 0.0392(8) Uani 1 1 d . . . H12A H 0.8358 0.6253 0.8837 0.047 Uiso 1 1 calc R . . H12B H 0.8110 0.5689 0.8045 0.047 Uiso 1 1 calc R . . C13 C 0.8851(3) 0.81950(18) 0.86376(16) 0.0313(8) Uani 1 1 d . . . H13A H 0.8496 0.7807 0.8227 0.038 Uiso 1 1 calc R . . H13B H 0.9726 0.8138 0.8605 0.038 Uiso 1 1 calc R . . C14 C 0.8499(3) 0.91201(18) 0.84596(18) 0.0346(8) Uani 1 1 d . . . H14A H 0.8585 0.9229 0.7873 0.042 Uiso 1 1 calc R . . H14B H 0.9049 0.9515 0.8747 0.042 Uiso 1 1 calc R . . C15 C 0.7226(3) 0.93248(18) 0.87132(18) 0.0365(8) Uani 1 1 d . . . H15A H 0.7196 0.9375 0.9309 0.044 Uiso 1 1 calc R . . H15B H 0.6997 0.9892 0.8484 0.044 Uiso 1 1 calc R . . C16 C 0.3468(3) 0.7499(3) 0.8832(2) 0.0675(12) Uani 1 1 d . . . H16A H 0.2789 0.7107 0.8887 0.101 Uiso 1 1 calc R . . H16B H 0.3785 0.7462 0.8281 0.101 Uiso 1 1 calc R . . H16C H 0.3210 0.8093 0.8940 0.101 Uiso 1 1 calc R . . C17 C 0.6095(3) 0.6205(2) 0.76819(19) 0.0532(10) Uani 1 1 d . . . H17A H 0.6586 0.6050 0.7214 0.080 Uiso 1 1 calc R . . H17B H 0.5527 0.6655 0.7526 0.080 Uiso 1 1 calc R . . H17C H 0.5663 0.5693 0.7870 0.080 Uiso 1 1 calc R . . C18 C 0.6145(3) 0.8729(2) 0.7618(2) 0.0608(11) Uani 1 1 d . . . H18A H 0.5930 0.9322 0.7467 0.091 Uiso 1 1 calc R . . H18B H 0.5486 0.8339 0.7488 0.091 Uiso 1 1 calc R . . H18C H 0.6855 0.8553 0.7317 0.091 Uiso 1 1 calc R . . Na1 Na 0.64686(9) 0.74939(6) 0.93934(6) 0.0256(3) Uani 1 1 d . . . O1 O 0.59313(16) 0.83208(12) 1.05189(11) 0.0313(5) Uani 1 1 d . . . O2 O 0.69326(17) 0.62344(11) 1.01332(11) 0.0301(5) Uani 1 1 d . . . O3 O 0.84549(15) 0.79400(11) 0.94282(11) 0.0271(5) Uani 1 1 d . . . O4 O 0.43659(17) 0.72615(13) 0.93923(12) 0.0426(6) Uani 1 1 d . . . O5 O 0.68284(18) 0.65152(12) 0.83058(12) 0.0356(5) Uani 1 1 d . . . O6 O 0.63851(18) 0.86929(12) 0.84616(12) 0.0365(5) Uani 1 1 d . . . Si1 Si 0.83602(8) 0.75269(6) 1.14279(5) 0.0324(2) Uani 1 1 d . . . Si2 Si 0.67956(8) 0.84959(5) 1.13293(5) 0.0321(2) Uani 1 1 d . . . Si3 Si 0.74288(8) 0.62424(5) 1.10932(5) 0.0326(2) Uani 1 1 d . . . Si4 Si 0.93559(7) 0.77789(5) 1.02206(5) 0.0293(2) Uani 1 1 d . . . 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 C1 0.056(2) 0.056(2) 0.040(2) -0.0052(18) 0.0078(19) 0.0045(19) C2 0.056(2) 0.037(2) 0.053(2) -0.0067(17) -0.001(2) 0.0002(18) C3 0.058(2) 0.055(2) 0.039(2) 0.0141(18) 0.0018(19) -0.008(2) C4 0.053(2) 0.039(2) 0.063(2) 0.0115(18) -0.007(2) 0.0055(18) C5 0.0316(19) 0.052(2) 0.052(2) -0.0005(17) -0.0065(18) -0.0115(17) C6 0.0301(19) 0.049(2) 0.064(2) 0.0078(19) 0.0068(18) 0.0066(17) C7 0.040(2) 0.055(2) 0.044(2) -0.0100(17) -0.0007(18) 0.0211(19) C8 0.027(2) 0.098(3) 0.049(2) -0.011(2) 0.0015(18) 0.017(2) C9 0.0271(19) 0.080(3) 0.047(2) 0.017(2) -0.0015(17) -0.0112(19) C10 0.044(2) 0.0281(18) 0.041(2) 0.0020(16) -0.0028(17) -0.0103(17) C11 0.053(2) 0.0267(19) 0.044(2) -0.0061(16) 0.0008(19) 0.0006(16) C12 0.042(2) 0.0335(18) 0.042(2) -0.0094(16) 0.0026(17) 0.0039(17) C13 0.0319(19) 0.0343(18) 0.0278(18) 0.0007(15) 0.0050(15) -0.0017(15) C14 0.0387(19) 0.0332(19) 0.0319(19) 0.0020(15) -0.0023(16) -0.0096(16) C15 0.043(2) 0.0291(18) 0.038(2) 0.0055(15) 0.0025(17) -0.0004(17) C16 0.042(2) 0.117(3) 0.044(2) 0.007(2) -0.0115(19) -0.007(2) C17 0.072(3) 0.043(2) 0.045(2) -0.0101(17) -0.012(2) -0.006(2) C18 0.062(3) 0.068(3) 0.052(3) 0.020(2) -0.018(2) -0.022(2) Na1 0.0229(6) 0.0280(6) 0.0259(6) -0.0005(5) 0.0017(5) -0.0014(5) O1 0.0232(11) 0.0393(12) 0.0314(12) -0.0046(10) -0.0008(10) 0.0114(10) O2 0.0386(12) 0.0231(11) 0.0285(12) 0.0012(9) -0.0044(10) -0.0074(10) O3 0.0226(11) 0.0324(11) 0.0264(12) 0.0040(9) 0.0033(9) 0.0000(9) O4 0.0242(12) 0.0652(15) 0.0382(14) 0.0015(11) -0.0015(11) -0.0068(11) O5 0.0439(13) 0.0283(11) 0.0347(13) -0.0075(10) -0.0015(11) -0.0005(11) O6 0.0344(13) 0.0389(13) 0.0362(14) 0.0107(10) -0.0058(11) -0.0042(10) Si1 0.0335(5) 0.0373(5) 0.0264(5) 0.0022(4) -0.0068(4) -0.0002(4) Si2 0.0365(5) 0.0345(5) 0.0253(5) -0.0047(4) 0.0011(4) 0.0009(4) Si3 0.0345(5) 0.0316(5) 0.0317(5) 0.0084(4) -0.0011(4) 0.0001(4) Si4 0.0203(5) 0.0317(5) 0.0359(5) 0.0021(4) -0.0029(4) -0.0009(4) _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 C1 Si2 1.894(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 Si2 1.878(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 Si3 1.887(3) . ? C3 H3B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3C 0.9800 . ? C4 Si3 1.880(3) . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4C 0.9800 . ? C5 Si4 1.885(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si4 1.889(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O1 1.422(3) . ? C7 C8 1.531(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.516(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O4 1.431(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O2 1.427(3) . ? C10 C11 1.520(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.525(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O5 1.417(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O3 1.437(3) . ? C13 C14 1.514(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O6 1.423(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.420(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O5 1.406(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O6 1.424(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Na1 O3 2.339(2) . ? Na1 O1 2.339(2) . ? Na1 O2 2.359(2) . ? Na1 O5 2.387(2) . ? Na1 O4 2.392(2) . ? Na1 O6 2.414(2) . ? O1 Si2 1.678(2) . ? O2 Si3 1.684(2) . ? O3 Si4 1.676(2) . ? Si1 Si3 2.3134(13) . ? Si1 Si2 2.3174(13) . ? Si1 Si4 2.3237(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 Si2 C1 H1A 109.5 . . ? Si2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si3 C3 H3B 109.5 . . ? Si3 C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? Si3 C4 H4B 109.5 . . ? Si3 C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 C8 111.2(2) . . ? O1 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? O1 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C7 111.8(3) . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? O4 C9 C8 113.6(3) . . ? O4 C9 H9A 108.9 . . ? C8 C9 H9A 108.9 . . ? O4 C9 H9B 108.9 . . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? O2 C10 C11 111.1(2) . . ? O2 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? O2 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 112.9(2) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? O5 C12 C11 113.4(3) . . ? O5 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? O5 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 C14 110.8(2) . . ? O3 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 112.8(2) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O6 C15 C14 113.7(2) . . ? O6 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? O6 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? O4 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 H17A 109.5 . . ? O5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 Na1 O1 93.78(7) . . ? O3 Na1 O2 91.12(7) . . ? O1 Na1 O2 95.47(7) . . ? O3 Na1 O5 92.51(7) . . ? O1 Na1 O5 172.45(8) . . ? O2 Na1 O5 80.22(7) . . ? O3 Na1 O4 171.37(8) . . ? O1 Na1 O4 80.06(7) . . ? O2 Na1 O4 95.45(8) . . ? O5 Na1 O4 94.11(8) . . ? O3 Na1 O6 79.99(7) . . ? O1 Na1 O6 94.51(8) . . ? O2 Na1 O6 167.04(8) . . ? O5 Na1 O6 90.69(8) . . ? O4 Na1 O6 94.39(8) . . ? C7 O1 Si2 124.12(19) . . ? C7 O1 Na1 110.33(18) . . ? Si2 O1 Na1 125.09(10) . . ? C10 O2 Si3 124.16(17) . . ? C10 O2 Na1 110.38(16) . . ? Si3 O2 Na1 123.84(9) . . ? C13 O3 Si4 124.45(18) . . ? C13 O3 Na1 110.76(16) . . ? Si4 O3 Na1 123.57(10) . . ? C16 O4 C9 112.9(2) . . ? C16 O4 Na1 131.68(19) . . ? C9 O4 Na1 108.65(17) . . ? C17 O5 C12 113.9(2) . . ? C17 O5 Na1 132.15(19) . . ? C12 O5 Na1 108.82(17) . . ? C15 O6 C18 112.7(2) . . ? C15 O6 Na1 108.36(17) . . ? C18 O6 Na1 131.65(18) . . ? Si3 Si1 Si2 101.23(5) . . ? Si3 Si1 Si4 99.00(4) . . ? Si2 Si1 Si4 101.36(4) . . ? O1 Si2 C2 106.04(13) . . ? O1 Si2 C1 106.29(13) . . ? C2 Si2 C1 105.59(15) . . ? O1 Si2 Si1 113.07(7) . . ? C2 Si2 Si1 113.21(11) . . ? C1 Si2 Si1 112.04(11) . . ? O2 Si3 C4 106.59(13) . . ? O2 Si3 C3 106.69(13) . . ? C4 Si3 C3 104.16(15) . . ? O2 Si3 Si1 112.48(7) . . ? C4 Si3 Si1 112.22(12) . . ? C3 Si3 Si1 114.05(11) . . ? O3 Si4 C5 105.91(12) . . ? O3 Si4 C6 105.96(13) . . ? C5 Si4 C6 105.49(14) . . ? O3 Si4 Si1 113.98(8) . . ? C5 Si4 Si1 111.92(11) . . ? C6 Si4 Si1 112.92(11) . . ? _diffrn_measured_fraction_theta_max 0.740 _diffrn_reflns_theta_full 22.15 _diffrn_measured_fraction_theta_full 0.740 _refine_diff_density_max 0.145 _refine_diff_density_min -0.143 _refine_diff_density_rms 0.030