#------------------------------------------------------------------------------ #$Date: 2019-12-11 11:29:06 +0200 (Wed, 11 Dec 2019) $ #$Revision: 244983 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556491.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556491 loop_ _publ_author_name 'Seifert, T.' 'Roesky, P.W.' _publ_section_title ; Alkali and Alkaline Earth Metal Complexes Ligated by an Ethynyl Substituted Cyclopentadienyl Ligand ; _journal_name_full Inorganics _journal_page_first 28 _journal_paper_doi 10.3390/inorganics5020028 _journal_volume 5 _journal_year 2017 _chemical_formula_moiety 'C26 H45 Na O3 Si' _chemical_formula_sum 'C26 H45 Na O3 Si' _chemical_formula_weight 456.70 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 99.360(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.1123(4) _cell_length_b 14.1264(5) _cell_length_c 24.7662(14) _cell_measurement_temperature 100(2) _cell_volume 2800.4(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_unetI/netI 0.1005 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 12871 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.088 _diffrn_reflns_theta_min 1.665 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.083 _exptl_crystal_F_000 1000 _refine_diff_density_max 0.702 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.105 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 5468 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.963 _refine_ls_R_factor_all 0.1562 _refine_ls_R_factor_gt 0.0852 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1470P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2044 _refine_ls_wR_factor_ref 0.2505 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2890 _reflns_number_total 5468 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 1.cif _cod_data_source_block tps213 _cod_database_code 1556491 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C25(H25A,H25B), C17(H17A,H17B), C20(H20A,H20B), C23(H23A, H23B), C21(H21A,H21B), C24(H24A,H24B), C26(H26A,H26B), C15(H15A,H15B), C22(H22A,H22B), C27(H27A,H27B), C16(H16A,H16B) 2.b Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B, H14C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C) ; _shelx_res_file ; TITL tps213_a.res in P2(1)/c tps213.res created by SHELXL-2016/6 at 12:59:18 on 10-Feb-2017 REM Old TITL REM SHELXT solution in P2(1)/c REM R1 0.245, Rweak 0.017, Alpha 0.038, Orientation as input REM Formula found by SHELXT: C27 Si2 O2 CELL 0.71073 8.1123 14.1264 24.7662 90 99.36 90 ZERR 4 0.0004 0.0005 0.0014 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Si Na O UNIT 104 180 4 4 12 L.S. 10 PLAN 20 TEMP -173.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.147000 FVAR 0.33970 SI1 3 0.368398 0.288670 0.761410 11.00000 0.03916 0.05079 = 0.01845 0.00010 0.00245 0.00374 NA1 4 0.631013 0.257766 0.557153 11.00000 0.02093 0.05249 = 0.02510 0.00170 -0.00287 0.00148 O3 5 0.810062 0.241766 0.494974 11.00000 0.03042 0.04056 = 0.03993 -0.00630 0.00973 -0.00062 O2 5 0.750755 0.395512 0.596880 11.00000 0.03375 0.08947 = 0.04253 -0.03051 0.01178 -0.02000 O1 5 0.768458 0.155150 0.620530 11.00000 0.03414 0.12643 = 0.04420 0.04385 0.00734 0.02248 C7 1 0.324704 0.333145 0.541387 11.00000 0.01951 0.03588 = 0.02017 -0.00101 0.00071 0.00343 C5 1 0.320927 0.273446 0.637958 11.00000 0.02170 0.03282 = 0.02437 0.00262 0.00402 0.00238 C10 1 0.328343 0.171102 0.554990 11.00000 0.02648 0.03712 = 0.02754 -0.00165 0.00391 -0.00210 C6 1 0.319627 0.260940 0.581522 11.00000 0.01854 0.03424 = 0.02216 0.00117 0.00281 0.00061 C9 1 0.341134 0.188216 0.500698 11.00000 0.02236 0.04344 = 0.02239 -0.00417 0.00027 -0.00282 C8 1 0.339212 0.288208 0.492181 11.00000 0.01794 0.04986 = 0.02103 0.00030 -0.00244 0.00177 C4 1 0.324384 0.281956 0.687290 11.00000 0.03392 0.03861 = 0.02599 0.00294 0.00573 0.00327 C11 1 0.315677 0.437185 0.551143 11.00000 0.04479 0.04232 = 0.02883 0.00477 0.00832 0.00475 AFIX 137 H11A 2 0.317653 0.448941 0.590241 11.00000 -1.50000 H11B 2 0.211935 0.462419 0.530305 11.00000 -1.50000 H11C 2 0.411518 0.468478 0.539286 11.00000 -1.50000 AFIX 0 C12 1 0.350915 0.337005 0.438517 11.00000 0.03775 0.06053 = 0.02373 0.00417 0.00203 0.00526 AFIX 137 H12A 2 0.348121 0.405761 0.443561 11.00000 -1.50000 H12B 2 0.256430 0.317693 0.410857 11.00000 -1.50000 H12C 2 0.455769 0.319152 0.426391 11.00000 -1.50000 AFIX 0 C13 1 0.350570 0.114269 0.457491 11.00000 0.04633 0.05051 = 0.03528 -0.01221 0.00873 -0.00466 AFIX 137 H13A 2 0.442960 0.129254 0.437895 11.00000 -1.50000 H13B 2 0.245422 0.113435 0.431624 11.00000 -1.50000 H13C 2 0.369469 0.052004 0.474843 11.00000 -1.50000 AFIX 0 C14 1 0.320649 0.076629 0.581711 11.00000 0.05554 0.03807 = 0.04044 0.00053 0.01652 0.00420 AFIX 137 H14A 2 0.415156 0.037756 0.574862 11.00000 -1.50000 H14B 2 0.215762 0.045016 0.566558 11.00000 -1.50000 H14C 2 0.325988 0.085204 0.621225 11.00000 -1.50000 AFIX 0 C18 1 0.919266 0.424074 0.595562 11.00000 0.03085 0.05225 = 0.03706 -0.00736 0.00143 -0.00214 AFIX 23 H18A 2 0.923338 0.469695 0.565464 11.00000 -1.20000 H18B 2 0.989001 0.368558 0.589938 11.00000 -1.20000 AFIX 0 C25 1 0.996084 0.086170 0.678928 11.00000 0.03321 0.06759 = 0.03832 0.01940 0.00249 0.00632 AFIX 23 H25A 2 1.094474 0.122538 0.696676 11.00000 -1.20000 H25B 2 1.026125 0.018276 0.678538 11.00000 -1.20000 AFIX 0 C17 1 0.981389 0.469800 0.650287 11.00000 0.03681 0.05598 = 0.03858 -0.00830 -0.00205 -0.00998 AFIX 23 H17A 2 1.092128 0.444545 0.666649 11.00000 -1.20000 H17B 2 0.989236 0.539389 0.646711 11.00000 -1.20000 AFIX 0 C20 1 0.867345 0.312837 0.462392 11.00000 0.06044 0.04222 = 0.05992 -0.00981 0.02473 -0.01062 AFIX 23 H20A 2 0.980920 0.333798 0.478814 11.00000 -1.20000 H20B 2 0.791683 0.368250 0.459313 11.00000 -1.20000 AFIX 0 C1 1 0.516807 0.387754 0.782136 11.00000 0.05156 0.07987 = 0.03631 -0.01621 0.00240 -0.01304 AFIX 137 H1A 2 0.625146 0.372953 0.771521 11.00000 -1.50000 H1B 2 0.530801 0.396292 0.821889 11.00000 -1.50000 H1C 2 0.472538 0.446137 0.763899 11.00000 -1.50000 AFIX 0 C23 1 0.874043 0.155626 0.477354 11.00000 0.06658 0.05302 = 0.03102 -0.00079 0.00966 0.01100 AFIX 23 H23A 2 0.806695 0.101093 0.486282 11.00000 -1.20000 H23B 2 0.991545 0.146129 0.494856 11.00000 -1.20000 AFIX 0 C2 1 0.462829 0.173239 0.788081 11.00000 0.06750 0.07484 = 0.03179 0.01485 0.00769 0.02447 AFIX 137 H2A 2 0.395124 0.120840 0.770557 11.00000 -1.50000 H2B 2 0.466043 0.170259 0.827772 11.00000 -1.50000 H2C 2 0.576662 0.168303 0.779850 11.00000 -1.50000 AFIX 0 C3 1 0.175566 0.308978 0.791056 11.00000 0.04780 0.07449 = 0.02620 0.00010 0.00637 0.00340 AFIX 137 H3A 2 0.120532 0.366878 0.775524 11.00000 -1.50000 H3B 2 0.204530 0.315699 0.830854 11.00000 -1.50000 H3C 2 0.099776 0.255086 0.782449 11.00000 -1.50000 AFIX 0 C21 1 0.869375 0.269631 0.406824 11.00000 0.07873 0.05756 = 0.04353 0.00534 0.01710 -0.00787 AFIX 23 H21A 2 0.771977 0.291146 0.380272 11.00000 -1.20000 H21B 2 0.973007 0.286796 0.392845 11.00000 -1.20000 AFIX 0 C24 1 0.935723 0.122005 0.621586 11.00000 0.03388 0.07831 = 0.04621 0.02373 -0.00010 0.01131 AFIX 23 H24A 2 1.008135 0.174116 0.612531 11.00000 -1.20000 H24B 2 0.937778 0.070424 0.594643 11.00000 -1.20000 AFIX 0 C26 1 0.847704 0.101465 0.708307 11.00000 0.04468 0.09370 = 0.04486 0.02520 0.00712 0.01476 AFIX 23 H26A 2 0.832832 0.046705 0.731994 11.00000 -1.20000 H26B 2 0.863018 0.159339 0.731117 11.00000 -1.20000 AFIX 0 C15 1 0.704818 0.422507 0.647960 11.00000 0.05317 0.10546 = 0.04388 -0.03057 0.02090 -0.03597 AFIX 23 H15A 2 0.630628 0.478561 0.643164 11.00000 -1.20000 H15B 2 0.645280 0.370088 0.663056 11.00000 -1.20000 AFIX 0 C22 1 0.861586 0.166773 0.416052 11.00000 0.10986 0.05995 = 0.03083 -0.00323 0.00436 0.00034 AFIX 23 H22A 2 0.955350 0.134088 0.402826 11.00000 -1.20000 H22B 2 0.755014 0.140304 0.396824 11.00000 -1.20000 AFIX 0 C27 1 0.706347 0.111214 0.665179 11.00000 0.04730 0.19717 = 0.06396 0.07145 0.02225 0.03808 AFIX 23 H27A 2 0.657905 0.048436 0.654196 11.00000 -1.20000 H27B 2 0.618947 0.150984 0.677417 11.00000 -1.20000 AFIX 0 C16 1 0.853084 0.443671 0.683068 11.00000 0.04627 0.23908 = 0.05085 -0.05765 0.00846 -0.05182 AFIX 23 H16A 2 0.890453 0.387944 0.706074 11.00000 -1.20000 H16B 2 0.834384 0.496747 0.707466 11.00000 -1.20000 AFIX 0 HKLF 4 REM tps213_a.res in P2(1)/c REM R1 = 0.0852 for 2890 Fo > 4sig(Fo) and 0.1562 for all 5468 data REM 287 parameters refined using 0 restraints END WGHT 0.1470 0.0000 REM Highest difference peak 0.702, deepest hole -0.441, 1-sigma level 0.105 Q1 1 0.7554 0.1809 0.6845 11.00000 0.05 0.70 Q2 1 0.7874 0.3427 0.6119 11.00000 0.05 0.54 Q3 1 0.7627 0.3721 0.6675 11.00000 0.05 0.50 Q4 1 0.3558 0.2509 0.4913 11.00000 0.05 0.49 Q5 1 0.3251 0.2210 0.5718 11.00000 0.05 0.46 Q6 1 0.3263 0.2411 0.5546 11.00000 0.05 0.44 Q7 1 0.8469 0.2407 0.4464 11.00000 0.05 0.43 Q8 1 0.3154 0.3713 0.5491 11.00000 0.05 0.41 Q9 1 0.3356 0.3015 0.5120 11.00000 0.05 0.40 Q10 1 0.2762 0.0675 0.4524 11.00000 0.05 0.38 Q11 1 0.3107 0.1752 0.5298 11.00000 0.05 0.37 Q12 1 0.3630 0.2800 0.4529 11.00000 0.05 0.37 Q13 1 0.3156 0.1922 0.6665 11.00000 0.05 0.36 Q14 1 0.6867 0.2589 0.5132 11.00000 0.05 0.35 Q15 1 0.3002 0.1860 0.5994 11.00000 0.05 0.34 Q16 1 0.8259 0.2197 0.5017 11.00000 0.05 0.33 Q17 1 0.3710 0.2183 0.7710 11.00000 0.05 0.33 Q18 1 0.6472 0.3281 0.5475 11.00000 0.05 0.33 Q19 1 0.3719 0.2642 0.4089 11.00000 0.05 0.31 Q20 1 0.3439 0.3611 0.7862 11.00000 0.05 0.31 ; _shelx_res_checksum 76639 _shelx_hkl_file ; -2 0 -4 688.24 8.53 0 1 -14 925.98 14.19 0 1 -13 1.21 4.80 0 1 -12 -6.63 3.15 0 1 -11 6.80 3.43 0 1 -10 834.59 10.91 0 1 -9 330.73 7.29 1 1 -15 302.55 8.00 1 1 -7 122.15 3.96 2 1 -16 17.66 4.08 2 1 -8 645.98 6.73 3 1 -13 30.71 3.47 3 1 -12 42.92 3.38 4 0 -21 0.15 4.31 5 0 -18 206.56 6.29 5 0 -17 -3.73 2.80 -7 -5 -5 16.50 4.84 -7 -5 -4 79.93 5.94 -6 -5 4 2.85 1.65 -5 -3 1 76.04 3.16 -5 -2 -9 5.19 5.45 -5 -2 -8 38.32 5.93 -5 -2 -7 6.61 4.11 -4 -2 1 31.52 2.31 -4 -1 -10 115.62 7.41 -4 -1 -9 -3.86 4.31 -4 -1 -8 4.84 4.20 -4 -1 -7 29.13 4.45 -1 0 -1 -0.37 1.27 0 1 -16 12.54 5.64 0 1 -15 10.96 3.75 0 1 -8 260.52 5.81 0 1 -7 53.27 4.24 1 1 -18 166.76 8.14 1 1 -17 41.02 4.92 2 1 -18 31.79 5.38 2 1 -17 0.69 2.80 3 1 -16 32.18 4.25 3 1 -15 45.75 3.78 3 1 -14 25.35 3.14 3 1 -11 150.48 4.14 4 0 -22 104.14 7.04 5 0 -19 7.71 3.86 -6 -3 -7 57.76 6.02 -5 -2 -5 34.57 4.07 -4 -1 -6 22.20 3.17 -4 -1 -5 9.74 3.59 -3 0 -12 27.33 6.15 -3 0 -11 -7.85 4.86 -3 0 -10 1335.85 17.21 -3 0 -9 -3.86 4.73 -2 0 -3 -2.82 2.94 -1 1 -14 110.55 6.98 -1 1 -12 4.75 5.12 -1 1 -11 54.19 5.78 -1 1 -10 -9.54 4.67 0 1 -17 71.42 5.96 1 1 -6 42.69 3.07 2 1 -19 41.13 5.82 2 1 -7 22.76 1.94 3 1 -17 73.13 5.28 3 1 -10 192.16 4.09 5 0 -20 29.21 4.96 -4 -1 -4 142.08 5.33 -3 -1 0 2.46 1.67 -3 0 -8 82.23 5.00 -3 0 -7 -1.50 4.36 -1 1 -15 11.62 3.94 -1 1 -9 269.99 6.93 -1 1 -8 586.67 9.57 0 1 -6 1004.35 9.35 3 1 -19 11.59 4.95 3 1 -9 52.61 2.56 -6 -4 1 47.73 3.13 -6 -3 -4 84.35 5.39 -5 -2 -3 51.64 3.80 -3 0 -6 148.00 6.19 -1 1 -7 78.96 4.84 3 1 -21 1.92 5.04 3 1 -20 6.29 4.91 -5 -3 2 172.26 3.58 -4 -1 -3 58.73 4.01 -3 0 -5 -0.98 3.77 -2 0 -2 915.86 8.25 -2 1 -14 53.75 6.49 -2 1 -13 255.40 9.46 -2 1 -12 73.13 7.00 -2 1 -11 22.68 5.49 -2 1 -10 122.95 6.85 0 1 -5 244.57 5.62 1 1 -5 0.99 2.62 2 1 -6 133.14 2.78 4 1 -18 52.31 5.22 4 1 -17 105.14 5.02 4 1 -16 264.53 6.48 4 1 -15 95.33 4.15 4 1 -14 178.72 4.92 -7 -4 -6 8.60 5.01 -7 -4 -5 -4.66 4.17 -5 -2 -2 1.72 2.88 -2 1 -9 20.66 5.13 -1 1 -6 56.46 3.56 3 1 -8 133.27 2.76 4 1 -19 4.94 4.38 4 1 -13 60.53 3.12 -7 -4 -4 55.78 5.06 -6 -4 2 12.56 2.25 -6 -3 -2 1.81 3.40 -5 -1 -9 1.80 4.05 -4 -2 2 51.92 2.15 -4 -1 -2 783.91 9.44 -4 0 -11 1.43 4.26 -4 0 -9 0.87 4.36 -3 0 -4 26.22 2.98 -2 1 -8 178.03 6.14 1 2 -16 -3.59 4.01 1 2 -15 23.50 4.54 4 1 -21 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9.54 -7 -5 -5 18.25 12.45 -7 -3 -2 38.35 13.15 -7 -2 0 188.05 14.04 -7 -1 2 154.98 12.94 -7 2 12 51.68 9.01 -6 -9 -10 8.88 7.38 -6 -2 -2 404.25 17.36 -6 -1 0 2.01 7.25 -6 0 2 132.25 11.29 -6 1 5 -4.09 6.55 -6 2 9 53.27 7.27 -6 3 15 -2.75 5.02 -5 -10 -12 -4.27 6.68 -5 -6 -9 16.89 7.51 -5 -3 -5 5.75 7.84 -9 -5 -1 1.02 12.30 -9 -3 2 24.75 14.68 -9 -2 4 5.65 12.59 -9 -1 7 11.60 12.15 -9 0 10 2.85 11.45 -9 1 15 -5.45 9.89 -9 1 16 6.87 9.51 -8 -7 -6 27.47 11.46 -8 -4 -2 1.57 11.66 -8 -1 4 19.23 9.21 -8 2 16 -3.33 8.14 -7 -9 -9 23.11 8.69 -7 -4 -4 46.65 11.64 -7 -2 -1 0.83 10.87 -7 -1 1 11.64 9.76 -7 0 4 6.08 7.77 -7 2 11 4.03 7.50 -6 -10 -11 2.70 6.32 -6 -8 -10 10.03 8.40 -6 -7 -9 16.71 9.93 -6 -6 -8 -1.26 8.71 -6 -5 -7 10.05 9.75 -6 2 8 18.96 7.35 -6 3 13 20.67 5.96 -6 3 14 31.13 6.21 -5 -8 -11 24.82 8.20 -5 -7 -10 20.14 6.03 -5 -5 -8 -4.28 6.92 -5 -4 -7 22.23 7.90 -5 -2 -4 -0.53 6.90 -5 -1 -2 0.31 6.06 -5 1 3 7.89 5.01 -4 -10 -13 12.68 5.96 -4 -7 -11 4.32 5.87 -4 -6 -10 49.33 7.06 -3 -9 -13 1.57 4.53 -9 -5 -2 2.09 11.98 -9 -4 0 -5.10 9.40 -9 0 9 -14.26 10.93 -9 1 13 6.70 9.87 -9 1 14 14.07 10.70 -8 -8 -7 13.19 8.75 -8 -6 -5 5.46 8.58 -8 -3 -1 1.00 11.16 -8 -2 1 0.24 8.46 -8 -1 3 -5.17 10.30 -8 0 6 32.52 9.19 -8 2 14 6.50 8.43 -7 -8 -9 1.50 9.85 -7 -7 -8 5.44 9.82 -7 -6 -7 12.01 10.43 -7 -5 -6 50.71 11.98 -7 -3 -3 5.10 10.07 -7 0 3 -3.38 9.03 -7 1 6 25.54 9.23 -7 2 10 17.64 7.77 -7 3 17 4.42 6.06 -7 3 18 33.19 6.79 -6 -9 -11 24.78 9.04 -6 -4 -6 19.16 7.30 -6 -2 -3 8.02 8.69 -6 -1 -1 17.25 7.15 -6 0 1 3.13 7.96 -6 1 4 48.73 7.35 -6 2 7 14.05 6.82 -6 3 12 -3.35 5.06 -5 -9 -12 0.85 7.16 -5 -3 -6 61.25 8.54 -5 0 0 34.65 5.76 -4 -8 -12 5.94 5.40 -4 -4 -8 6.97 5.65 -9 -4 -1 -5.60 12.98 -9 -3 1 -2.50 9.10 -9 -2 3 4.32 9.19 -9 -1 5 2.65 12.73 -9 0 8 -0.28 11.62 -9 1 12 29.81 11.61 -8 -7 -7 7.82 10.27 -8 -6 -6 10.34 10.59 -8 -4 -3 -5.21 8.45 -8 -3 -2 7.27 10.72 -8 -2 0 0.14 11.85 -8 -1 2 3.94 11.68 -8 1 8 4.66 10.08 -8 2 13 -3.43 8.44 -7 -4 -5 -1.22 9.30 -7 -2 -2 45.12 11.76 -7 -1 0 207.44 15.14 -7 1 5 13.22 8.77 -7 2 9 1.84 7.12 -7 3 15 0.64 6.15 -7 3 16 -3.90 5.22 -6 -10 -12 11.18 7.80 -6 -7 -10 -1.08 7.70 -6 -6 -9 8.45 8.59 -6 1 3 -0.36 7.24 -6 3 11 4.59 5.86 -5 -10 -13 0.44 6.43 -5 -6 -10 30.80 7.30 -5 1 2 62.19 7.03 -5 2 5 4.97 5.74 -4 -9 -13 1.85 5.49 -4 -3 -7 27.54 6.34 -9 -2 2 -0.80 11.50 -9 -1 4 37.79 13.64 -9 0 7 11.31 11.97 -9 1 11 3.97 10.99 -9 2 17 -8.81 7.24 -8 -5 -5 9.18 8.48 -8 -4 -4 -0.27 11.66 -8 1 7 -2.46 9.91 -8 2 11 4.25 8.00 -8 2 12 -2.21 5.86 -7 -7 -9 16.43 9.74 -7 -6 -8 11.29 9.91 -7 -5 -7 11.29 10.29 -7 -3 -4 12.34 7.77 -7 0 2 -1.85 7.08 -7 2 8 3.18 7.40 -7 3 14 6.91 6.77 -6 -8 -11 2.46 8.30 -6 -4 -7 6.54 9.06 -6 -2 -4 111.47 11.68 -6 -1 -2 88.58 8.97 -6 0 0 840.15 21.05 -5 -8 -12 5.25 6.87 -5 -7 -11 -1.03 5.23 -5 -5 -9 2.23 5.21 -5 -2 -5 33.42 7.60 -5 -1 -3 -2.07 4.07 -5 0 -1 -1.65 4.28 -4 -6 -11 16.55 5.89 -9 -5 -4 4.98 11.95 -9 -4 -2 6.04 9.37 -9 -1 3 -5.39 11.30 -9 0 6 8.20 11.91 -9 1 10 9.87 9.79 -9 2 15 15.23 8.75 -9 2 16 4.70 8.84 -8 -7 -8 4.90 10.99 -8 -5 -6 -2.49 10.14 -8 -2 -1 -2.44 8.07 -8 -1 1 -3.73 8.14 -8 0 3 -5.30 11.10 -8 1 6 10.01 10.41 -8 2 10 52.04 10.45 -8 3 18 4.92 6.94 -7 -9 -11 7.94 9.19 -7 -8 -10 7.76 7.60 -7 -4 -6 7.72 9.47 -7 -2 -3 15.63 10.89 -7 -1 -1 7.56 7.60 -7 0 1 -3.76 9.06 -7 3 12 21.48 7.21 -7 3 13 0.23 6.31 -6 -9 -12 6.18 7.11 -6 -3 -6 121.72 11.22 -6 2 5 19.53 7.30 -6 3 10 0.19 5.53 -5 -9 -13 -7.65 6.44 -5 -3 -7 3.63 6.05 -4 -8 -13 -3.40 4.69 -4 -7 -12 56.90 6.76 -4 -5 -10 77.53 6.62 -4 -4 -9 21.84 6.53 -4 -2 -6 184.21 9.55 -9 -4 -3 6.64 13.53 -9 0 5 9.60 12.37 -9 1 9 6.24 7.75 -9 2 14 4.99 9.67 -8 -4 -5 5.97 11.81 -8 -2 -2 0.90 11.80 -8 -1 0 61.01 13.36 -8 2 9 7.07 9.49 -8 3 15 19.01 7.49 -8 3 16 6.86 7.54 -8 3 17 -0.32 6.14 -7 -7 -10 -8.10 8.81 -7 -3 -5 5.33 7.66 -7 1 3 -0.17 8.98 -7 3 11 6.30 6.98 -6 -10 -13 13.58 7.53 -6 -7 -11 7.72 8.11 -6 -6 -10 -2.15 8.13 -6 -5 -9 20.58 9.12 -6 -4 -8 40.26 9.17 -6 -2 -5 52.52 9.88 -6 -1 -3 8.08 8.42 -6 0 -1 -0.39 8.14 -6 3 9 14.22 6.17 -5 -10 -14 24.32 6.88 -5 -6 -11 -3.78 6.22 -5 -5 -10 33.58 7.45 -5 -1 -4 14.01 7.18 -5 0 -2 65.90 8.28 -4 -3 -8 4.02 5.69 -3 -9 -14 6.54 4.05 -9 -5 -5 -4.86 13.17 -9 -3 -2 -2.84 12.01 -9 -2 0 -3.20 9.19 -9 -1 2 32.27 10.36 -9 0 4 21.56 12.33 -9 1 8 75.78 10.81 -9 2 12 18.98 10.83 -8 -7 -9 8.34 11.90 -8 -6 -8 56.75 12.95 -8 -3 -4 17.41 11.38 -8 1 5 -2.75 7.44 -8 3 14 18.73 8.38 -7 -8 -11 5.79 9.05 -7 -4 -7 11.43 9.71 -7 -2 -4 28.36 10.54 -7 -1 -2 35.14 8.74 -7 2 6 -6.35 6.13 -7 3 10 48.98 8.15 -6 -9 -13 1.51 6.93 -6 -8 -12 1.64 6.08 -6 -3 -7 47.45 9.73 -6 2 4 -1.35 7.16 -6 3 8 156.44 9.72 -6 4 15 7.71 4.47 -6 4 16 24.44 5.09 -5 -8 -13 16.84 7.13 -5 -7 -12 20.14 5.88 -5 -4 -9 18.45 7.50 -5 2 3 -0.17 6.86 -4 -9 -14 -2.05 5.33 -9 -4 -4 4.19 9.76 -9 -2 -1 2.80 13.69 -9 1 7 1.32 8.38 -9 2 11 -3.52 10.72 -8 -4 -6 46.45 12.33 -8 -2 -3 -18.79 10.68 -8 -1 -1 -4.16 8.33 -8 0 1 -0.85 11.95 -8 1 4 14.01 8.36 -8 2 7 6.89 10.16 -8 3 12 3.70 7.99 -8 3 13 4.96 7.83 -7 -6 -10 0.72 9.00 -7 -3 -6 9.99 8.07 -7 -1 -3 13.32 11.31 -7 0 -1 -5.26 9.53 -6 -5 -10 -2.63 7.87 -6 -2 -6 20.90 9.22 -6 -1 -4 95.65 11.06 -6 0 -2 436.76 16.62 -6 4 14 3.14 4.77 -5 -9 -14 3.14 6.42 -5 -1 -5 19.53 7.57 -5 0 -3 3.11 7.23 -4 -7 -13 20.69 5.96 -4 -6 -12 28.55 6.41 -4 -5 -11 6.35 6.12 -4 -4 -10 23.35 6.99 -4 -2 -7 5.56 6.27 -10 0 6 77.68 12.86 -9 -4 -5 4.34 13.72 -9 -2 -2 44.79 14.03 -9 -1 0 -1.84 12.22 -9 0 3 -2.14 9.12 -9 1 6 7.05 8.60 -9 2 9 -2.56 9.59 -9 2 10 0.82 7.52 -9 3 16 -2.68 7.70 -8 -6 -9 4.35 11.80 -8 -5 -8 -9.81 11.49 -8 -3 -5 3.03 8.83 -8 1 3 -2.03 11.51 -8 3 11 6.84 8.73 -7 -7 -11 -2.69 7.56 -7 -5 -9 13.41 7.89 -7 -4 -8 -6.90 10.56 -7 -2 -5 4.98 8.04 -7 3 8 9.18 7.79 -7 4 15 7.45 5.79 -7 4 16 5.48 6.01 -6 -8 -13 12.21 8.51 -6 -7 -12 1.45 8.08 -6 -4 -9 49.62 9.70 -6 1 0 5.90 6.54 -6 2 3 2.74 5.97 -6 4 12 142.28 8.81 -6 4 13 63.55 6.74 -5 -6 -12 -2.31 7.53 -5 -5 -11 -2.59 6.80 -5 -2 -7 3.78 7.31 -5 1 -1 0.47 6.77 -5 2 2 5.99 7.45 -4 -8 -14 34.54 6.05 -9 -3 -4 15.89 13.09 -9 0 2 0.33 11.96 -9 1 5 15.06 9.22 -9 2 8 -4.29 11.13 -9 3 14 2.28 9.42 -9 3 15 11.19 8.55 -8 -4 -7 9.14 9.06 -8 -3 -6 10.20 12.70 -8 -2 -4 4.55 9.18 -8 0 0 5.84 8.93 -8 1 2 4.64 11.97 -8 3 10 16.99 10.07 -7 -3 -7 12.32 8.14 -7 -1 -4 149.66 14.83 -7 3 7 22.55 8.45 -7 4 14 8.91 6.92 -6 -9 -14 -1.73 7.61 -6 -1 -5 1.20 8.97 -6 0 -3 2.58 9.07 -6 2 2 -1.01 7.88 -6 3 6 -2.65 5.35 -6 4 11 2.35 5.79 -5 -8 -14 10.20 7.16 -5 -7 -13 -1.02 5.26 -5 -3 -9 1.47 7.50 -4 -3 -9 9.63 5.29 -4 -1 -6 18.77 6.94 -9 -4 -6 7.12 12.66 -9 -1 -1 3.55 9.78 -9 0 1 10.57 13.66 -9 1 4 31.30 10.30 -9 2 7 5.02 11.73 -9 3 12 16.05 10.59 -9 3 13 -5.98 8.70 -8 -6 -10 -8.43 11.04 -8 -5 -9 12.83 12.10 -8 -4 -8 1.31 10.90 -8 -2 -5 -0.54 12.58 -8 -1 -3 -4.64 11.31 -8 0 -1 -6.02 12.17 -8 3 9 25.21 9.26 -7 -7 -12 20.82 10.78 -7 -6 -11 5.37 7.21 -7 -5 -10 9.76 7.63 -7 -4 -9 19.71 11.29 -7 -2 -6 -4.99 7.75 -7 2 3 38.82 8.42 -7 4 13 15.02 6.62 -6 -7 -13 2.58 8.65 -6 -6 -12 10.63 8.83 -6 -5 -11 12.99 9.31 -6 -4 -10 -7.88 9.20 -6 -2 -7 22.27 7.84 -6 1 -1 20.58 7.35 -6 3 5 6.58 7.21 -5 -9 -15 2.65 6.64 -5 -1 -6 -0.05 7.41 -5 0 -4 273.31 11.96 -5 1 -2 2.62 7.28 -5 2 1 1.72 5.93 -4 -6 -13 2.56 5.73 -4 -2 -8 6.42 7.02 -9 -4 -7 4.04 12.31 -9 -2 -4 -5.90 12.18 -9 -1 -2 -12.20 13.68 -9 0 0 40.54 14.33 -9 1 3 -17.31 10.92 -9 2 6 10.16 11.73 -9 3 11 4.02 10.48 -8 -3 -7 24.35 12.95 -8 -1 -4 22.95 11.93 -8 2 4 2.39 7.99 -8 3 8 68.07 9.36 -8 4 14 -1.66 7.36 -8 4 15 10.99 7.33 -7 -8 -13 -0.86 7.01 -7 -3 -8 71.44 10.20 -7 0 -3 3.08 10.37 -7 3 6 96.92 9.41 -7 4 11 21.67 8.05 -6 -8 -14 7.02 8.50 -6 -3 -9 23.59 9.40 -6 0 -4 909.01 23.16 -6 1 -2 98.99 10.96 -6 2 1 4.15 8.36 -5 -6 -13 20.89 8.15 -5 -5 -12 81.79 9.60 -5 -4 -11 53.32 8.50 -5 -2 -8 26.12 6.77 -5 3 4 433.11 12.83 -4 -7 -14 61.37 7.03 -4 -4 -11 10.17 6.48 -9 -3 -6 -5.43 12.84 -9 3 9 10.35 10.05 -9 3 10 14.11 8.42 -8 -5 -10 -1.21 11.01 -8 -4 -9 4.87 10.73 -8 -2 -6 87.95 14.68 -8 2 3 5.15 9.97 -8 3 7 6.58 7.29 -8 4 12 16.35 7.79 -8 4 13 -1.85 7.51 -7 -7 -13 32.42 10.61 -7 -6 -12 4.17 10.23 -7 -5 -11 -0.51 10.03 -7 -4 -10 13.63 10.58 -7 3 5 12.51 6.97 -7 4 10 -11.77 7.14 -6 -9 -15 32.90 8.63 -6 -6 -13 10.43 8.08 -6 -5 -12 8.84 8.54 -6 -2 -8 -7.88 8.23 -5 -8 -15 16.69 6.34 -5 -7 -14 6.64 6.55 -5 -3 -10 25.60 8.78 -5 -1 -7 -3.65 7.02 -5 0 -5 -0.52 7.36 -5 1 -3 3.36 6.21 -5 2 0 17.52 5.22 -5 3 3 336.03 12.20 -4 -8 -15 78.55 7.51 -4 -3 -10 126.37 8.36 -4 -1 -7 21.69 7.58 -9 -2 -5 -3.98 11.42 -9 -1 -3 7.29 9.83 -9 0 -1 3.13 9.42 -9 1 1 -0.10 11.95 -9 2 4 11.24 11.46 -9 3 8 43.72 11.65 -9 4 15 -1.33 6.78 -8 -3 -8 -1.03 9.96 -8 0 -3 6.14 11.79 -8 2 2 3.80 10.64 -8 3 6 -2.56 6.82 -8 4 11 8.95 8.56 -7 -3 -9 17.69 7.98 -7 -1 -6 5.62 9.58 -7 0 -4 274.35 14.74 -7 4 9 16.42 7.10 -6 -7 -14 17.20 8.48 -6 -4 -11 10.52 6.54 -6 -1 -7 67.90 10.49 -6 1 -3 -0.15 8.17 -6 2 0 188.66 11.03 -6 3 3 18.31 7.86 -6 4 7 49.33 7.23 -5 -2 -9 7.14 7.48 -9 -3 -7 7.01 9.10 -9 -2 -6 22.75 11.24 -9 -1 -4 24.32 12.54 -9 0 -2 182.83 17.20 -9 1 0 2.35 10.34 -9 2 3 8.40 11.67 -9 3 7 23.06 10.12 -9 4 13 28.60 9.22 -9 4 14 -0.74 7.75 -8 -5 -11 -2.99 9.60 -8 -2 -7 17.60 8.70 -8 2 1 8.80 10.26 -8 3 5 -4.60 6.62 -8 4 9 21.57 8.58 -8 4 10 46.95 9.02 -7 -6 -13 -3.40 8.38 -7 -5 -12 19.19 9.58 -7 -4 -11 2.64 9.45 -7 0 -5 9.06 10.71 -7 2 0 205.70 13.69 -7 3 3 13.81 8.78 -6 -8 -15 1.35 6.11 -6 3 2 180.89 10.64 -5 -6 -14 -1.37 6.25 -5 -5 -13 4.36 7.31 -5 -4 -12 5.41 6.51 -5 3 2 202.92 10.52 -4 -6 -14 -0.49 4.72 -4 -5 -13 21.31 6.02 -4 -4 -12 16.58 5.79 -8 -1 -6 9.93 7.97 -8 0 -4 8.42 7.97 -8 3 4 52.87 8.36 -7 -3 -10 4.45 6.68 -7 -1 -7 0.34 6.86 -7 1 -3 7.20 7.12 -7 4 7 0.62 5.02 -6 4 6 13.74 4.99 -5 1 -4 7.82 5.22 -4 0 -6 7.76 4.37 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46092 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.36840(15) 0.28867(9) 0.76141(5) 0.0364(3) Uani 1 1 d . . . . . Na1 Na 0.63101(17) 0.25777(12) 0.55715(6) 0.0336(4) Uani 1 1 d . . . . . O3 O 0.8101(3) 0.2418(2) 0.49497(12) 0.0365(7) Uani 1 1 d . . . . . O2 O 0.7508(4) 0.3955(3) 0.59688(13) 0.0546(10) Uani 1 1 d . . . . . O1 O 0.7685(4) 0.1552(3) 0.62053(14) 0.0681(12) Uani 1 1 d . . . . . C7 C 0.3247(4) 0.3331(3) 0.54139(15) 0.0255(8) Uani 1 1 d . . . . . C5 C 0.3209(4) 0.2734(3) 0.63796(16) 0.0263(8) Uani 1 1 d . . . . . C10 C 0.3283(5) 0.1711(3) 0.55499(16) 0.0304(9) Uani 1 1 d . . . . . C6 C 0.3196(4) 0.2609(3) 0.58152(15) 0.0250(8) Uani 1 1 d . . . . . C9 C 0.3411(4) 0.1882(3) 0.50070(16) 0.0298(9) Uani 1 1 d . . . . . C8 C 0.3392(4) 0.2882(3) 0.49218(15) 0.0302(9) Uani 1 1 d . . . . . C4 C 0.3244(5) 0.2820(3) 0.68729(17) 0.0327(9) Uani 1 1 d . . . . . C11 C 0.3157(5) 0.4372(3) 0.55114(18) 0.0384(10) Uani 1 1 d . . . . . H11A H 0.317653 0.448941 0.590241 0.058 Uiso 1 1 calc GR . . . . H11B H 0.211935 0.462419 0.530305 0.058 Uiso 1 1 calc GR . . . . H11C H 0.411518 0.468478 0.539286 0.058 Uiso 1 1 calc GR . . . . C12 C 0.3509(5) 0.3370(3) 0.43852(17) 0.0410(11) Uani 1 1 d . . . . . H12A H 0.348121 0.405761 0.443561 0.062 Uiso 1 1 calc GR . . . . H12B H 0.256430 0.317693 0.410857 0.062 Uiso 1 1 calc GR . . . . H12C H 0.455769 0.319152 0.426391 0.062 Uiso 1 1 calc GR . . . . C13 C 0.3506(6) 0.1143(3) 0.45749(19) 0.0438(11) Uani 1 1 d . . . . . H13A H 0.442960 0.129254 0.437895 0.066 Uiso 1 1 calc GR . . . . H13B H 0.245422 0.113435 0.431624 0.066 Uiso 1 1 calc GR . . . . H13C H 0.369469 0.052004 0.474843 0.066 Uiso 1 1 calc GR . . . . C14 C 0.3206(6) 0.0766(3) 0.5817(2) 0.0437(11) Uani 1 1 d . . . . . H14A H 0.415156 0.037756 0.574862 0.066 Uiso 1 1 calc GR . . . . H14B H 0.215762 0.045016 0.566558 0.066 Uiso 1 1 calc GR . . . . H14C H 0.325988 0.085204 0.621225 0.066 Uiso 1 1 calc GR . . . . C18 C 0.9193(5) 0.4241(3) 0.59556(19) 0.0405(11) Uani 1 1 d . . . . . H18A H 0.923338 0.469695 0.565464 0.049 Uiso 1 1 calc R . . . . H18B H 0.989001 0.368558 0.589938 0.049 Uiso 1 1 calc R . . . . C25 C 0.9961(5) 0.0862(4) 0.67893(19) 0.0467(12) Uani 1 1 d . . . . . H25A H 1.094474 0.122538 0.696676 0.056 Uiso 1 1 calc R . . . . H25B H 1.026125 0.018276 0.678538 0.056 Uiso 1 1 calc R . . . . C17 C 0.9814(5) 0.4698(4) 0.65029(18) 0.0447(11) Uani 1 1 d . . . . . H17A H 1.092128 0.444545 0.666649 0.054 Uiso 1 1 calc R . . . . H17B H 0.989236 0.539389 0.646711 0.054 Uiso 1 1 calc R . . . . C20 C 0.8673(7) 0.3128(3) 0.4624(2) 0.0525(13) Uani 1 1 d . . . . . H20A H 0.980920 0.333798 0.478814 0.063 Uiso 1 1 calc R . . . . H20B H 0.791683 0.368250 0.459313 0.063 Uiso 1 1 calc R . . . . C1 C 0.5168(6) 0.3878(4) 0.7821(2) 0.0564(14) Uani 1 1 d . . . . . H1A H 0.625146 0.372953 0.771521 0.085 Uiso 1 1 calc GR . . . . H1B H 0.530801 0.396292 0.821889 0.085 Uiso 1 1 calc GR . . . . H1C H 0.472538 0.446137 0.763899 0.085 Uiso 1 1 calc GR . . . . C23 C 0.8740(7) 0.1556(3) 0.47735(19) 0.0500(12) Uani 1 1 d . . . . . H23A H 0.806695 0.101093 0.486282 0.060 Uiso 1 1 calc R . . . . H23B H 0.991545 0.146129 0.494856 0.060 Uiso 1 1 calc R . . . . C2 C 0.4628(7) 0.1732(4) 0.7881(2) 0.0581(14) Uani 1 1 d . . . . . H2A H 0.395124 0.120840 0.770557 0.087 Uiso 1 1 calc GR . . . . H2B H 0.466043 0.170259 0.827772 0.087 Uiso 1 1 calc GR . . . . H2C H 0.576662 0.168303 0.779850 0.087 Uiso 1 1 calc GR . . . . C3 C 0.1756(6) 0.3090(4) 0.79106(19) 0.0495(12) Uani 1 1 d . . . . . H3A H 0.120532 0.366878 0.775524 0.074 Uiso 1 1 calc GR . . . . H3B H 0.204530 0.315699 0.830854 0.074 Uiso 1 1 calc GR . . . . H3C H 0.099776 0.255086 0.782449 0.074 Uiso 1 1 calc GR . . . . C21 C 0.8694(8) 0.2696(4) 0.4068(2) 0.0591(14) Uani 1 1 d . . . . . H21A H 0.771977 0.291146 0.380272 0.071 Uiso 1 1 calc R . . . . H21B H 0.973007 0.286796 0.392845 0.071 Uiso 1 1 calc R . . . . C24 C 0.9357(5) 0.1220(4) 0.6216(2) 0.0535(13) Uani 1 1 d . . . . . H24A H 1.008135 0.174116 0.612531 0.064 Uiso 1 1 calc R . . . . H24B H 0.937778 0.070424 0.594643 0.064 Uiso 1 1 calc R . . . . C26 C 0.8477(6) 0.1015(5) 0.7083(2) 0.0611(15) Uani 1 1 d . . . . . H26A H 0.832832 0.046705 0.731994 0.073 Uiso 1 1 calc R . . . . H26B H 0.863018 0.159339 0.731117 0.073 Uiso 1 1 calc R . . . . C15 C 0.7048(7) 0.4225(5) 0.6480(2) 0.0661(17) Uani 1 1 d . . . . . H15A H 0.630628 0.478561 0.643164 0.079 Uiso 1 1 calc R . . . . H15B H 0.645280 0.370088 0.663056 0.079 Uiso 1 1 calc R . . . . C22 C 0.8616(9) 0.1668(4) 0.4161(2) 0.0677(16) Uani 1 1 d . . . . . H22A H 0.955350 0.134088 0.402826 0.081 Uiso 1 1 calc R . . . . H22B H 0.755014 0.140304 0.396824 0.081 Uiso 1 1 calc R . . . . C27 C 0.7063(7) 0.1112(7) 0.6652(3) 0.101(3) Uani 1 1 d . . . . . H27A H 0.657905 0.048436 0.654196 0.122 Uiso 1 1 calc R . . . . H27B H 0.618947 0.150984 0.677417 0.122 Uiso 1 1 calc R . . . . C16 C 0.8531(7) 0.4437(7) 0.6831(3) 0.112(3) Uani 1 1 d . . . . . H16A H 0.890453 0.387944 0.706074 0.134 Uiso 1 1 calc R . . . . H16B H 0.834384 0.496747 0.707466 0.134 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0392(6) 0.0508(7) 0.0184(6) 0.0001(5) 0.0024(5) 0.0037(6) Na1 0.0209(7) 0.0525(10) 0.0251(9) 0.0017(7) -0.0029(6) 0.0015(7) O3 0.0304(14) 0.0406(16) 0.0399(17) -0.0063(13) 0.0097(12) -0.0006(13) O2 0.0338(16) 0.089(3) 0.043(2) -0.0305(18) 0.0118(14) -0.0200(17) O1 0.0341(17) 0.126(3) 0.044(2) 0.044(2) 0.0073(15) 0.022(2) C7 0.0195(16) 0.036(2) 0.020(2) -0.0010(15) 0.0007(14) 0.0034(16) C5 0.0217(18) 0.033(2) 0.024(2) 0.0026(16) 0.0040(15) 0.0024(16) C10 0.0265(19) 0.037(2) 0.028(2) -0.0016(17) 0.0039(16) -0.0021(18) C6 0.0185(16) 0.034(2) 0.022(2) 0.0012(16) 0.0028(14) 0.0006(16) C9 0.0224(17) 0.043(2) 0.022(2) -0.0042(17) 0.0003(15) -0.0028(18) C8 0.0179(17) 0.050(2) 0.021(2) 0.0003(18) -0.0024(14) 0.0018(18) C4 0.034(2) 0.039(2) 0.026(2) 0.0029(17) 0.0057(17) 0.0033(18) C11 0.045(2) 0.042(2) 0.029(2) 0.0048(18) 0.0083(19) 0.005(2) C12 0.038(2) 0.061(3) 0.024(2) 0.004(2) 0.0020(17) 0.005(2) C13 0.046(2) 0.051(3) 0.035(3) -0.012(2) 0.009(2) -0.005(2) C14 0.056(3) 0.038(2) 0.040(3) 0.001(2) 0.017(2) 0.004(2) C18 0.031(2) 0.052(3) 0.037(3) -0.007(2) 0.0014(18) -0.002(2) C25 0.033(2) 0.068(3) 0.038(3) 0.019(2) 0.0025(19) 0.006(2) C17 0.037(2) 0.056(3) 0.039(3) -0.008(2) -0.0020(19) -0.010(2) C20 0.060(3) 0.042(3) 0.060(3) -0.010(2) 0.025(3) -0.011(2) C1 0.052(3) 0.080(4) 0.036(3) -0.016(3) 0.002(2) -0.013(3) C23 0.067(3) 0.053(3) 0.031(3) -0.001(2) 0.010(2) 0.011(3) C2 0.067(3) 0.075(4) 0.032(3) 0.015(2) 0.008(2) 0.024(3) C3 0.048(3) 0.074(3) 0.026(2) 0.000(2) 0.006(2) 0.003(2) C21 0.079(4) 0.058(3) 0.044(3) 0.005(2) 0.017(3) -0.008(3) C24 0.034(2) 0.078(4) 0.046(3) 0.024(3) 0.000(2) 0.011(2) C26 0.045(3) 0.094(4) 0.045(3) 0.025(3) 0.007(2) 0.015(3) C15 0.053(3) 0.105(5) 0.044(3) -0.031(3) 0.021(2) -0.036(3) C22 0.110(5) 0.060(3) 0.031(3) -0.003(2) 0.004(3) 0.000(3) C27 0.047(3) 0.197(8) 0.064(4) 0.071(5) 0.022(3) 0.038(4) C16 0.046(3) 0.239(10) 0.051(4) -0.058(5) 0.008(3) -0.052(5) 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C4 Si1 C1 109.3(2) . . C4 Si1 C2 108.2(2) . . C4 Si1 C3 111.6(2) . . C1 Si1 C2 110.3(3) . . C3 Si1 C1 108.9(2) . . C3 Si1 C2 108.5(2) . . O3 Na1 O2 95.75(12) . . O3 Na1 C7 128.05(13) . . O3 Na1 C10 127.37(13) . . O3 Na1 C6 150.72(12) . . O3 Na1 C9 102.04(12) . . O3 Na1 C8 101.96(12) . . O2 Na1 C7 92.46(13) . . O2 Na1 C10 134.09(13) . . O2 Na1 C6 103.55(12) . . O2 Na1 C9 142.08(14) . . O2 Na1 C8 112.90(14) . . O1 Na1 O3 96.14(12) . . O1 Na1 O2 96.70(16) . . O1 Na1 C7 133.63(13) . . O1 Na1 C10 93.76(13) . . O1 Na1 C6 103.13(12) . . O1 Na1 C9 114.09(15) . . O1 Na1 C8 143.13(15) . . C7 Na1 C10 50.62(12) . . C7 Na1 C6 30.91(11) . . C7 Na1 C9 50.40(12) . . C6 Na1 C10 30.67(11) . . C6 Na1 C9 49.91(12) . . C9 Na1 C10 29.46(12) . . C8 Na1 C7 30.28(12) . . C8 Na1 C10 49.90(12) . . C8 Na1 C6 50.24(12) . . C8 Na1 C9 30.72(12) . . C20 O3 Na1 128.1(3) . . C20 O3 C23 105.2(3) . . C23 O3 Na1 126.5(3) . . C18 O2 Na1 124.2(3) . . C15 O2 Na1 116.6(3) . . C15 O2 C18 109.4(3) . . C24 O1 Na1 125.0(3) . . C27 O1 Na1 127.7(3) . . C27 O1 C24 107.2(4) . . C6 C7 Na1 75.3(2) . . C6 C7 C11 125.6(3) . . C8 C7 Na1 74.8(2) . . C8 C7 C6 107.4(3) . . C8 C7 C11 127.0(4) . . C11 C7 Na1 115.9(2) . . C4 C5 C6 178.2(4) . . C6 C10 Na1 72.9(2) . . C6 C10 C14 125.3(4) . . C9 C10 Na1 74.5(2) . . C9 C10 C6 107.9(3) . . C9 C10 C14 126.9(4) . . C14 C10 Na1 119.5(3) . . C7 C6 Na1 73.8(2) . . C7 C6 C10 107.7(3) . . C5 C6 Na1 111.7(2) . . C5 C6 C7 127.2(3) . . C5 C6 C10 124.9(3) . . C10 C6 Na1 76.4(2) . . C10 C9 Na1 76.1(2) . . C10 C9 C8 108.4(3) . . C10 C9 C13 126.0(4) . . C8 C9 Na1 72.9(2) . . C8 C9 C13 125.6(4) . . C13 C9 Na1 118.5(3) . . C7 C8 Na1 74.9(2) . . C7 C8 C9 108.7(3) . . C7 C8 C12 125.8(4) . . C9 C8 Na1 76.4(2) . . C9 C8 C12 125.4(4) . . C12 C8 Na1 115.2(2) . . C5 C4 Si1 169.8(4) . . C7 C11 H11A 109.5 . . C7 C11 H11B 109.5 . . C7 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . C8 C12 H12A 109.5 . . C8 C12 H12B 109.5 . . C8 C12 H12C 109.5 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C9 C13 H13A 109.5 . . C9 C13 H13B 109.5 . . C9 C13 H13C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . C10 C14 H14A 109.5 . . C10 C14 H14B 109.5 . . C10 C14 H14C 109.5 . . H14A C14 H14B 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . O2 C18 H18A 110.5 . . O2 C18 H18B 110.5 . . O2 C18 C17 106.3(4) . . H18A C18 H18B 108.7 . . C17 C18 H18A 110.5 . . C17 C18 H18B 110.5 . . H25A C25 H25B 109.0 . . C24 C25 H25A 111.0 . . C24 C25 H25B 111.0 . . C24 C25 C26 104.0(4) . . C26 C25 H25A 111.0 . . C26 C25 H25B 111.0 . . C18 C17 H17A 111.2 . . C18 C17 H17B 111.2 . . H17A C17 H17B 109.1 . . C16 C17 C18 103.0(4) . . C16 C17 H17A 111.2 . . C16 C17 H17B 111.2 . . O3 C20 H20A 110.4 . . O3 C20 H20B 110.4 . . O3 C20 C21 106.7(4) . . H20A C20 H20B 108.6 . . C21 C20 H20A 110.4 . . C21 C20 H20B 110.4 . . Si1 C1 H1A 109.5 . . Si1 C1 H1B 109.5 . . Si1 C1 H1C 109.5 . . H1A C1 H1B 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . O3 C23 H23A 110.8 . . O3 C23 H23B 110.8 . . O3 C23 C22 104.5(4) . . H23A C23 H23B 108.9 . . C22 C23 H23A 110.8 . . C22 C23 H23B 110.8 . . Si1 C2 H2A 109.5 . . Si1 C2 H2B 109.5 . . Si1 C2 H2C 109.5 . . H2A C2 H2B 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . Si1 C3 H3A 109.5 . . Si1 C3 H3B 109.5 . . Si1 C3 H3C 109.5 . . H3A C3 H3B 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . C20 C21 H21A 110.9 . . C20 C21 H21B 110.9 . . H21A C21 H21B 108.9 . . C22 C21 C20 104.5(4) . . C22 C21 H21A 110.9 . . C22 C21 H21B 110.9 . . O1 C24 C25 106.7(4) . . O1 C24 H24A 110.4 . . O1 C24 H24B 110.4 . . C25 C24 H24A 110.4 . . C25 C24 H24B 110.4 . . H24A C24 H24B 108.6 . . C25 C26 H26A 110.8 . . C25 C26 H26B 110.8 . . H26A C26 H26B 108.9 . . C27 C26 C25 104.8(5) . . C27 C26 H26A 110.8 . . C27 C26 H26B 110.8 . . O2 C15 H15A 110.4 . . O2 C15 H15B 110.4 . . H15A C15 H15B 108.6 . . C16 C15 O2 106.6(4) . . C16 C15 H15A 110.4 . . C16 C15 H15B 110.4 . . C23 C22 H22A 110.7 . . C23 C22 H22B 110.7 . . C21 C22 C23 105.1(4) . . C21 C22 H22A 110.7 . . C21 C22 H22B 110.7 . . H22A C22 H22B 108.8 . . O1 C27 C26 106.1(5) . . O1 C27 H27A 110.5 . . O1 C27 H27B 110.5 . . C26 C27 H27A 110.5 . . C26 C27 H27B 110.5 . . H27A C27 H27B 108.7 . . C17 C16 H16A 109.9 . . C17 C16 H16B 109.9 . . C15 C16 C17 109.0(5) . . C15 C16 H16A 109.9 . . C15 C16 H16B 109.9 . . H16A C16 H16B 108.3 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 C4 1.815(4) . Si1 C1 1.863(5) . Si1 C2 1.875(5) . Si1 C3 1.855(5) . Na1 O3 2.293(3) . Na1 O2 2.321(3) . Na1 O1 2.289(3) . Na1 C7 2.673(4) . Na1 C10 2.736(4) . Na1 C6 2.691(4) . Na1 C9 2.717(4) . Na1 C8 2.672(4) . O3 C20 1.413(6) . O3 C23 1.419(5) . O2 C18 1.431(5) . O2 C15 1.428(6) . O1 C24 1.432(5) . O1 C27 1.429(7) . C7 C6 1.429(5) . C7 C8 1.396(5) . C7 C11 1.493(6) . C5 C6 1.407(5) . C5 C4 1.223(6) . C10 C6 1.436(5) . C10 C9 1.387(6) . C10 C14 1.495(6) . C9 C8 1.428(6) . C9 C13 1.506(6) . C8 C12 1.514(6) . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C18 H18A 0.9900 . C18 H18B 0.9900 . C18 C17 1.512(6) . C25 H25A 0.9900 . C25 H25B 0.9900 . C25 C24 1.512(6) . C25 C26 1.520(7) . C17 H17A 0.9900 . C17 H17B 0.9900 . C17 C16 1.468(8) . C20 H20A 0.9900 . C20 H20B 0.9900 . C20 C21 1.508(7) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C23 H23A 0.9900 . C23 H23B 0.9900 . C23 C22 1.513(7) . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 . C3 H3A 0.9800 . C3 H3B 0.9800 . C3 H3C 0.9800 . C21 H21A 0.9900 . C21 H21B 0.9900 . C21 C22 1.474(7) . C24 H24A 0.9900 . C24 H24B 0.9900 . C26 H26A 0.9900 . C26 H26B 0.9900 . C26 C27 1.441(8) . C15 H15A 0.9900 . C15 H15B 0.9900 . C15 C16 1.397(7) . C22 H22A 0.9900 . C22 H22B 0.9900 . C27 H27A 0.9900 . C27 H27B 0.9900 . C16 H16A 0.9900 . C16 H16B 0.9900 .