#------------------------------------------------------------------------------ #$Date: 2020-04-09 06:48:06 +0300 (Thu, 09 Apr 2020) $ #$Revision: 250530 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/74/7157458.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_7157458 loop_ _publ_author_name 'Sarkar, Parantap' 'Inaba, Yuya' 'Shirakura, Hayato' 'Yoneda, Tomoki' 'Inokuma, Yasuhide' _publ_section_title ; Modular synthesis of oligoacetylacetones via site-selective silylation of acetylacetone derivatives ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB00501K _journal_year 2020 _chemical_formula_moiety 'C20 H38 O4 Si2' _chemical_formula_sum 'C10 H19 O2 Si' _chemical_formula_weight 199.34 _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 _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90 _cell_angle_beta 90.224(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1033(14) _cell_length_b 15.700(3) _cell_length_c 10.748(2) _cell_measurement_reflns_used 7967 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 1.89 _cell_volume 1198.6(4) _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _diffrn_ambient_temperature 123(2) _diffrn_detector 'Image Plate' _diffrn_detector_area_resol_mean 10 _diffrn_detector_type 'Rigaku IP' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type RAPID _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_unetI/netI 0.0663 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 10679 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 1.895 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.167 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_correction_T_min 0.1822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR(Rigaku, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 436 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.482 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 2726 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0694 _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^)+(0.0924P)^2^+0.7584P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1738 _refine_ls_wR_factor_ref 0.1941 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2002 _reflns_number_total 2726 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00501k3.cif _cod_data_source_block Compound5a _cod_original_cell_volume 1198.7(4) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7157458 _shelx_shelxl_version_number 2017/1 _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. ; _shelx_estimated_absorpt_t_min 0.948 _shelx_estimated_absorpt_t_max 0.985 _shelx_res_file ; TITL texray_a.res in P2(1)/c texray.res created by SHELXL-2017/1 at 15:31:13 on 19-Jan-2018 REM Yadorkari-X generated CELL 0.71075 7.1033 15.7005 10.7485 90.0000 90.2240 90.0000 ZERR 4.0 0.0014 0.0034 0.0021 0.0000 0.0060 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z REM SPGR P21/c monoclinic SFAC C H O Si UNIT 40 76 8 4 SIZE 0.32 0.26 0.09 TEMP -150.0 L.S. 10 FMAP 2 PLAN -40 ACTA CONF HTAB LIST 4 BOND $H TWIN 1 0 0.005 0 -1 0 0 0 -1 WGHT 0.092400 0.758400 BASF 0.25484 FVAR 8.90549 SI2 4 0.692274 0.606979 0.842044 11.00000 0.04600 0.02807 = 0.04296 -0.00264 -0.00282 -0.00087 O4 3 0.702191 0.507504 0.787156 11.00000 0.04203 0.03106 = 0.05243 -0.00559 0.00094 -0.00217 O5 3 0.440242 0.366594 0.621648 11.00000 0.04627 0.04316 = 0.06868 0.01520 -0.00827 -0.00841 C10 1 0.843942 0.466042 0.726854 11.00000 0.04228 0.02915 = 0.04345 0.00394 0.00044 0.00152 C11 1 0.585478 0.405648 0.602338 11.00000 0.04614 0.02822 = 0.04156 -0.00261 -0.00221 -0.00090 C12 1 0.770924 0.384274 0.670131 11.00000 0.04157 0.02905 = 0.03953 0.00219 -0.00150 0.00468 C13 1 0.592566 0.475847 0.505595 11.00000 0.04118 0.03344 = 0.04366 0.00491 -0.00296 0.00157 AFIX 23 H1 2 0.623981 0.450654 0.423833 11.00000 -1.20000 H2 2 0.693983 0.516363 0.527969 11.00000 -1.20000 AFIX 0 C14 1 0.443990 0.614858 0.893369 11.00000 0.05312 0.04426 = 0.05393 0.00125 0.00886 0.00632 AFIX 137 H3 2 0.360234 0.608688 0.821263 11.00000 -1.50000 H4 2 0.422980 0.670453 0.932370 11.00000 -1.50000 H5 2 0.417524 0.569597 0.953601 11.00000 -1.50000 AFIX 0 C15 1 0.744401 0.683358 0.715965 11.00000 0.05700 0.03254 = 0.05501 0.00286 -0.00202 -0.00094 AFIX 137 H6 2 0.878322 0.680140 0.694907 11.00000 -1.50000 H7 2 0.713984 0.741193 0.743675 11.00000 -1.50000 H8 2 0.668538 0.669245 0.642458 11.00000 -1.50000 AFIX 0 C16 1 0.853576 0.621261 0.976783 11.00000 0.06902 0.04678 = 0.05407 -0.00710 -0.01618 -0.00474 AFIX 137 H9 2 0.837798 0.573716 1.034889 11.00000 -1.50000 H10 2 0.824062 0.674882 1.019106 11.00000 -1.50000 H11 2 0.984002 0.622722 0.947471 11.00000 -1.50000 AFIX 0 C17 1 0.904944 0.346483 0.574123 11.00000 0.05581 0.03960 = 0.04980 -0.00872 0.00125 0.00943 AFIX 137 H12 2 0.932496 0.389254 0.510334 11.00000 -1.50000 H13 2 0.846119 0.296683 0.535110 11.00000 -1.50000 H14 2 1.022243 0.329253 0.615297 11.00000 -1.50000 AFIX 0 C18 1 1.020555 0.493281 0.722611 11.00000 0.04821 0.03840 = 0.05729 0.00014 0.00094 -0.00161 AFIX 93 H15 2 1.054951 0.544742 0.763256 11.00000 -1.20000 H16 2 1.112656 0.461331 0.678928 11.00000 -1.20000 AFIX 0 C19 1 0.734208 0.320255 0.774724 11.00000 0.05688 0.02833 = 0.05031 0.00615 -0.01115 -0.00205 AFIX 137 H17 2 0.851025 0.310324 0.821317 11.00000 -1.50000 H18 2 0.689902 0.266423 0.738939 11.00000 -1.50000 H19 2 0.638199 0.343044 0.830860 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM texray_a.res in P2(1)/c REM R1 = 0.0694 for 2002 Fo > 4sig(Fo) and 0.0970 for all 2726 data REM 124 parameters refined using 0 restraints END WGHT 0.0924 0.7430 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.482, deepest hole -0.471, 1-sigma level 0.062 Q1 1 0.7889 0.6127 0.9032 11.00000 0.05 0.48 Q2 1 0.8042 0.4279 0.6814 11.00000 0.05 0.33 Q3 1 0.5899 0.6100 0.8984 11.00000 0.05 0.33 Q4 1 0.6795 0.3755 0.6208 11.00000 0.05 0.29 Q5 1 0.5914 0.6079 0.7724 11.00000 0.05 0.25 Q6 1 0.6904 0.3962 0.6385 11.00000 0.05 0.24 Q7 1 0.7874 0.5088 0.7179 11.00000 0.05 0.22 Q8 1 0.6347 0.5628 0.8031 11.00000 0.05 0.21 Q9 1 0.7809 0.6176 0.7733 11.00000 0.05 0.21 Q10 1 0.9284 0.4804 0.6692 11.00000 0.05 0.21 Q11 1 0.6079 0.5019 0.7296 11.00000 0.05 0.20 Q12 1 0.8339 0.3699 0.6309 11.00000 0.05 0.20 Q13 1 0.9402 0.6944 0.9860 11.00000 0.05 0.20 Q14 1 0.5356 0.3569 0.8793 11.00000 0.05 0.19 Q15 1 0.7410 0.4680 0.7882 11.00000 0.05 0.19 Q16 1 0.7926 0.6095 1.1033 11.00000 0.05 0.19 Q17 1 0.5063 0.4046 0.6483 11.00000 0.05 0.19 Q18 1 0.9559 0.6030 0.8236 11.00000 0.05 0.19 Q19 1 0.5218 0.6294 0.9658 11.00000 0.05 0.19 Q20 1 0.8022 0.6863 0.9452 11.00000 0.05 0.19 Q21 1 0.7695 0.5012 0.4754 11.00000 0.05 0.19 Q22 1 1.0614 0.6071 0.6985 11.00000 0.05 0.18 Q23 1 0.7423 0.5602 0.8628 11.00000 0.05 0.18 Q24 1 0.6775 0.2767 0.7638 11.00000 0.05 0.18 Q25 1 0.3245 0.4207 0.6516 11.00000 0.05 0.18 Q26 1 0.5952 0.6986 0.6521 11.00000 0.05 0.18 Q27 1 1.0659 0.4431 0.7358 11.00000 0.05 0.18 Q28 1 0.5368 0.6767 0.5767 11.00000 0.05 0.17 Q29 1 0.4055 0.6718 0.7201 11.00000 0.05 0.17 Q30 1 0.1858 0.3478 0.6555 11.00000 0.05 0.17 Q31 1 1.0746 0.6883 0.7249 11.00000 0.05 0.17 Q32 1 0.7772 0.5412 0.8236 11.00000 0.05 0.17 Q33 1 1.1146 0.5349 0.7581 11.00000 0.05 0.17 Q34 1 0.7417 0.7227 0.7206 11.00000 0.05 0.16 Q35 1 0.5615 0.7976 0.6891 11.00000 0.05 0.16 Q36 1 0.6759 0.1775 0.8471 11.00000 0.05 0.16 Q37 1 1.0077 0.3519 0.4983 11.00000 0.05 0.16 Q38 1 0.7404 0.4321 0.8628 11.00000 0.05 0.16 Q39 1 0.7934 0.3396 0.8369 11.00000 0.05 0.16 Q40 1 0.8043 0.5020 0.8486 11.00000 0.05 0.16 ; _shelx_res_checksum 21698 _shelx_hkl_file ; 0 0 1 172.94 120.18 0 0 -1 401.88 207.72 0 0 2317585.617320.41 0 0 -2303574.215826.61 0 0 3 268.52 433.81 0 0 -3 -320.97 474.34 0 0 4 8163.50 577.60 0 0 -4 7677.29 623.34 0 0 5 28.51 529.05 0 0 5 -164.38 442.51 0 0 -5 -434.81 452.11 0 0 6 6896.44 709.17 0 0 6 7459.74 594.23 0 0 -6 6324.06 602.39 0 0 7 1125.29 567.28 0 0 -7 -549.43 485.14 0 0 8 9780.53 886.80 0 0 -8 6674.84 762.93 0 0 9-1517.29 727.89 0 0 -9 28.21 638.61 0 0 10 949.19 778.81 0 0 -10 -406.20 639.44 0 0 11 924.41 821.31 0 0 -11-1085.74 668.96 0 0 12 2265.50 954.27 0 0 -12 1566.55 742.34 0 0 13 -152.00 937.73 0 0 -13 -427.00 720.97 0 -1 130682.62 611.80 0 1 127943.43 574.04 0 1 -130409.87 647.12 0 -1 -129235.12 729.05 0 -1 2587816.151320.97 0 1 2594398.751702.36 0 1 -2594466.552182.32 0 1 -2588826.353074.67 0 -1 -2562338.049387.64 0 -1 318321.85 843.49 0 1 320025.65 808.31 0 1 -317843.53 946.22 0 -1 -318766.73 814.66 0 -1 435808.85 953.84 0 1 438119.89 1233.50 0 1 -438392.43 1403.16 0 -1 -437391.12 1242.67 0 -1 5 6804.22 398.66 0 1 5 7778.74 567.90 0 1 -5 6644.77 632.97 0 -1 -5 7636.81 590.57 0 -1 644550.50 1776.11 0 1 646882.47 1669.33 0 1 -642599.77 1728.15 0 -1 -645714.66 1666.71 0 -1 7 6740.55 701.34 0 1 7 7662.42 781.97 0 1 7 7994.45 680.48 0 1 -7 6686.11 701.47 0 -1 -7 6098.81 634.86 0 -1 817995.95 1097.24 0 1 819222.80 1197.54 0 1 815679.61 972.02 0 1 -814901.58 1037.46 0 -1 -814542.95 1027.74 0 -1 919871.88 1240.88 0 1 921771.42 1354.60 0 1 -914262.25 1177.15 0 -1 -914101.08 1146.50 0 -1 10 3130.15 796.14 0 1 10 4295.26 552.41 0 1 -10 3102.31 719.57 0 -1 -10 2581.57 719.15 0 -1 11 895.15 755.31 0 1 11 542.73 869.12 0 1 -11 1288.70 678.41 0 -1 -11 614.28 687.45 0 -1 12 1068.92 820.23 0 1 12 127.80 925.14 0 1 -12 28.51 722.55 0 -1 -12 327.08 698.16 0 -1 13 674.92 850.93 0 1 13 120.72 1070.50 0 1 -13 409.45 723.17 0 -1 -13 330.97 742.34 0 2 0390513.922931.37 0 -2 0377180.922532.75 0 2 1 4459.36 272.86 0 -2 1 4912.97 641.34 0 -2 -1 4664.40 538.30 0 2 -1 4669.48 587.21 0 -2 220093.87 845.51 0 2 219198.22 895.27 0 2 -219713.38 829.12 0 -2 -218564.11 949.76 0 2 -219680.99 734.50 0 -2 3 7431.72 532.90 0 2 -3 6522.65 528.67 0 -2 -3 6778.14 548.38 0 -2 445842.97 1527.11 0 2 446423.66 1492.35 0 2 -448191.38 1793.32 0 -2 -445996.85 1500.21 0 -2 516159.28 782.22 0 2 515717.60 790.46 0 2 -514707.55 898.30 0 -2 -516843.57 770.47 0 -2 6 5465.26 571.12 0 2 6 6223.45 557.40 0 2 -6 6412.53 632.08 0 -2 -6 6149.39 538.65 0 -2 734111.85 1056.25 0 2 732086.22 1515.63 0 -2 -732791.93 1428.81 0 -2 8 2055.03 583.61 0 2 8 2172.25 432.71 0 2 -8 1836.81 648.84 0 -2 -8 2123.99 575.81 0 -2 9 6384.24 795.73 0 2 9 8827.20 967.22 0 2 -9 7307.04 839.65 0 -2 -9 6769.80 770.79 0 -2 10 85.00 664.75 0 2 10 1602.18 799.77 0 2 -10 803.90 660.45 0 -2 -10 1245.74 640.16 0 -2 11 1600.16 735.20 0 2 11 1824.25 917.24 0 2 -11 1142.12 736.15 0 -2 -11 1901.50 716.28 0 -2 12 499.17 716.37 0 2 12-1033.99 922.36 0 2 -12 416.42 707.89 0 -2 -12 98.45 711.56 0 2 -12 327.10 624.58 0 -2 13 -941.08 757.89 0 2 13 255.03 619.21 0 2 -13 -701.20 767.04 0 -2 -13 96.71 788.08 0 2 -13 -364.07 658.81 0 3 0 147.88 635.38 0 -3 0 1058.48 684.50 0 3 111324.58 914.44 0 -3 111388.30 1052.33 0 -3 -111234.65 972.36 0 3 -111145.71 623.17 0 3 2978060.3132783.3 0 3 -2952602.6125688.9 0 -3 -2971167.8131471.7 0 3 -21012047.136345.8 0 -3 360367.11 1823.91 0 3 358434.30 1946.61 0 3 -360792.92 1805.19 0 -3 -357948.29 1913.76 0 3 -361419.73 2539.12 0 -3 467746.25 2200.74 0 3 467516.82 2294.47 0 3 -465928.25 2125.17 0 -3 -464198.16 2207.47 0 -3 548891.59 1669.64 0 3 550612.67 1797.87 0 3 -548576.34 1503.44 0 -3 -546555.92 1668.43 0 -3 6 1943.10 471.36 0 3 6 2455.25 520.48 0 3 -6 2782.59 598.50 0 -3 -6 3278.29 478.11 0 -3 712240.02 778.97 0 3 713980.80 826.22 0 3 -712613.80 943.96 0 -3 -712714.25 794.77 0 -3 8 4579.23 607.26 0 3 8 4947.82 669.18 0 3 -8 3777.63 722.60 0 -3 -8 3937.86 621.00 0 -3 9 -150.57 552.10 0 3 9 -160.92 441.83 0 3 9 1922.83 661.26 0 3 -9 1013.06 645.76 0 -3 -9 553.33 570.45 0 -3 10 -12.14 350.95 0 3 10 -164.10 797.44 0 3 10 1.39 569.28 0 3 -10 261.17 685.24 0 -3 -10 -12.27 604.18 0 -3 11 21.71 633.06 0 3 11 652.24 856.75 0 3 -11 160.54 699.98 0 -3 -11 1137.52 688.30 0 3 -11 216.83 670.96 0 -3 12 587.59 683.11 0 3 12 446.18 925.44 0 3 -12 -280.52 744.44 0 -3 -12 767.60 754.24 0 3 -12 502.61 690.12 0 -3 13 1231.29 781.62 0 3 13 1754.33 1094.71 0 3 -13 2330.34 823.30 0 -3 -13 2780.46 915.77 0 3 -13 1481.39 761.52 0 4 0524902.746190.43 0 -4 0515566.645215.90 0 4 1 7548.47 818.69 0 -4 1 6537.62 519.97 0 -4 -1 6712.10 845.52 0 4 -1 6948.06 539.88 0 4 2147500.2 6166.54 0 -4 2144466.9 6663.20 0 -4 -2144009.0 6057.65 0 4 -2147535.8 6903.76 0 4 324650.50 1017.58 0 4 -325777.41 863.87 0 -4 -325862.30 1048.91 0 4 -326756.77 913.20 0 -4 4623487.462723.19 0 4 4646908.266756.36 0 4 -4651308.365067.75 0 -4 -4656697.167271.68 0 4 -4660430.567886.42 0 -4 5 4440.07 510.59 0 4 5 4771.50 552.34 0 4 -5 4788.73 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-8 -6 -2 2302.11 1342.66 8 6 3 138.36 850.78 8 6 3 1071.02 1249.19 -8 6 -3 322.36 1164.19 -8 -6 -3 577.64 1406.16 8 6 4 -27.10 761.04 8 6 4-1570.04 1264.56 -8 6 -4 -244.56 1298.24 -8 -6 -4 1598.70 1432.74 8 6 5 1034.66 707.92 8 6 5 1076.37 864.12 -8 6 -5 3384.49 1474.50 -8 -6 -5 1772.53 1618.37 8 7 -5 2970.29 1536.55 8 7 -5 1337.15 1287.04 -8 7 5 415.62 792.00 8 7 -4 353.05 888.06 8 7 -4 1196.79 983.15 -8 7 4 -684.58 1142.41 -8 -7 4 1549.23 1022.15 8 7 -3 2684.51 1352.35 8 7 -3 149.56 870.66 -8 7 3 416.37 588.57 -8 -7 3 -525.27 1099.67 8 7 -2 3265.69 1334.15 8 7 -2 2632.27 1011.87 -8 7 2 1677.02 902.29 -8 7 2 890.97 587.25 -8 -7 2 3312.33 1256.38 -8 7 2 592.56 709.05 8 7 -1 862.52 690.20 8 7 -1 -42.80 981.30 -8 7 1-1199.49 657.96 -8 -7 1 816.95 1217.27 -8 7 1 190.37 756.63 8 7 0 3253.82 1158.11 8 7 0 2634.25 1155.97 -8 7 0 736.09 852.50 -8 -7 0 2745.78 1388.76 8 7 1 1186.86 594.32 8 7 1 760.40 671.89 -8 7 -1 -330.71 915.86 -8 -7 -1 -859.28 1362.15 8 7 2 2567.60 1055.13 8 7 2 8266.72 1363.12 -8 7 -2 4557.29 783.64 -8 -7 -2 5343.01 1044.81 8 7 3 90.96 782.74 8 7 3 1001.05 1297.18 -8 7 -3 725.39 1196.53 -8 -7 -3 697.88 1471.20 8 7 4 1147.99 743.29 8 7 4 1881.88 875.77 -8 7 -4 1366.16 1397.33 -8 -7 -4 1873.18 968.33 8 8 -4 4404.92 1583.55 8 8 -4 426.85 957.70 -8 8 4 1495.39 1147.70 -8 -8 4 1561.90 1111.43 8 8 -3 890.70 805.33 8 8 -3 -633.63 945.08 -8 8 3 -877.96 933.01 -8 -8 3 1541.99 1148.66 8 8 -2 -36.41 1368.47 8 8 -2 2634.15 1121.88 -8 8 2 3134.06 889.38 -8 8 2 1601.37 623.13 -8 -8 2 2678.23 1327.73 -8 8 2 911.03 714.05 8 8 -1 1824.04 1221.99 8 8 -1 1747.37 695.31 -8 8 1 1437.78 697.65 -8 -8 1 1588.27 1368.71 8 8 0 5275.08 1235.54 8 8 0 4988.75 1326.53 -8 8 0 3044.99 587.32 -8 -8 0 5064.45 989.84 -8 8 0 2265.54 1050.44 8 8 1 712.18 965.23 8 8 1 333.68 1180.29 -8 8 -1 -143.16 927.93 -8 -8 -1 455.42 1382.96 8 8 2 73.13 535.21 8 8 2 1694.96 753.85 -8 8 -2 754.74 1115.71 -8 -8 -2 -400.24 1439.37 8 8 3 1058.44 782.37 8 8 3 1807.10 1293.42 -8 8 -3 1671.95 1300.65 -8 -8 -3 104.37 939.97 8 8 4 3596.01 1604.10 -8 8 -4 3011.68 1595.08 -8 -8 -4 4824.18 1785.76 8 9 -3 7977.82 1739.91 8 9 -3 8262.66 1405.73 -8 9 3 5930.38 1200.19 -8 -9 3 5823.25 1590.94 8 9 -2 1560.15 1237.64 8 9 -2 716.47 1088.61 -8 9 2 -700.02 804.24 -8 9 2 -0.05 584.26 -8 -9 2 2029.34 1285.07 -8 9 2 63.73 681.37 8 9 -1 -440.92 1167.48 8 9 -1 330.63 1171.15 -8 9 1 608.22 440.40 -8 9 1 554.12 704.33 -8 -9 1 2922.16 1358.97 -8 9 1 116.13 821.67 8 9 0-1142.93 635.51 8 9 0 358.55 1165.13 -8 9 0 179.59 839.17 -8 -9 0 -936.29 1397.35 -8 9 0 611.13 913.10 8 9 1 1608.35 961.80 8 9 1 417.08 752.04 -8 9 -1 686.41 990.29 -8 -9 -1 344.23 1495.87 -8 9 -1 1058.34 1059.82 8 9 2 -556.01 827.28 8 9 2 1547.97 1263.43 -8 9 -2 -49.11 684.48 -8 -9 -2 771.13 1458.34 -8 9 -2 -17.19 694.12 8 9 3 2169.25 857.06 8 9 3 5628.94 1494.32 -8 9 -3 2461.29 876.63 -8 -9 -3 1625.03 1694.68 8 10 -1 1373.84 1212.85 8 10 -1 2884.99 1243.29 -8 10 1 535.07 715.67 -8 10 1 1811.95 779.51 8 10 0 3671.10 1060.91 8 10 0 268.54 1268.56 -8 10 0 391.60 569.49 -8 10 0 62.92 949.74 8 10 1 826.88 570.53 8 10 1 1277.88 1296.71 -8 10 -1 -475.08 1036.87 9 0 -3 -817.74 1469.81 9 0 -2 1171.33 1448.55 9 0 -2 2128.38 882.74 -9 0 2 126.02 927.02 9 0 -1 520.45 1323.50 9 0 -1 1327.61 987.84 -9 0 1 302.83 967.90 9 0 0 606.99 774.85 9 0 0 1950.21 1050.56 -9 0 0 1559.10 1046.72 9 0 1 282.50 1261.93 9 0 1 2435.80 1168.82 -9 0 -1 2364.01 1194.87 9 0 2 2077.18 1257.12 9 0 2 3813.94 1299.40 -9 0 -2 3066.60 1366.50 9 0 3 1482.61 1090.35 -9 0 -3 760.53 1357.55 9 1 -3 1785.27 1504.27 9 -1 -3 1439.54 885.19 9 1 -2 2279.35 1417.26 9 -1 -2 2398.84 1335.42 9 1 -2 94.60 940.53 -9 1 2 535.78 852.55 -9 -1 2 -8.41 996.55 9 1 -1 3536.88 1461.79 9 -1 -1 3607.22 838.81 9 -1 -1 1675.71 621.25 9 1 -1 1638.21 1069.80 -9 1 1 2303.23 958.40 -9 -1 1 1726.47 1133.83 9 1 0 744.82 1315.69 9 -1 0 -589.89 1168.71 9 -1 0-1568.62 945.77 9 1 0 220.81 637.29 -9 1 0 198.24 958.08 -9 -1 0 -342.61 648.02 9 1 1 3473.20 897.61 9 -1 1 2506.90 1204.06 9 -1 1 4102.79 1221.79 9 1 1 2796.09 748.07 -9 1 -1 2185.87 726.34 -9 -1 -1 3098.57 1318.86 9 1 2 4162.43 1429.30 9 -1 2 2235.76 1114.04 9 -1 2 3752.47 1306.39 9 1 2 3101.87 792.82 -9 1 -2 2917.89 1321.71 -9 -1 -2 5160.18 1447.88 9 2 -2 1678.60 1411.82 9 -2 -2-1096.76 1280.90 9 2 -2 898.10 991.43 -9 2 2 -224.13 754.06 -9 -2 2 728.84 1041.27 9 2 -1 1162.86 1421.01 9 -2 -1 1299.45 1176.96 9 2 -1 -477.79 1024.60 -9 2 1 25.30 831.20 -9 -2 1 692.98 1143.91 9 2 0 718.49 1408.22 9 -2 0 2126.75 1087.60 9 2 0 618.69 1062.20 -9 2 0 725.48 557.26 -9 -2 0 323.44 1201.69 9 2 1 2278.88 1475.00 9 -2 1 1220.16 1027.60 9 2 1 430.39 1129.60 -9 2 -1 2781.15 1078.20 -9 -2 -1 591.50 790.59 9 2 2 670.54 1410.82 9 -2 2 904.28 865.65 9 -2 2 229.60 682.10 9 2 2 194.18 1140.33 -9 2 -2 -248.30 701.18 -9 -2 -2 2423.84 1396.16 9 3 -2 2538.24 1515.88 9 -3 -2 1282.28 774.16 9 3 -2 1321.67 1103.25 -9 -3 2 2285.12 1182.45 9 3 -1 872.43 1456.14 9 -3 -1 1905.04 1120.94 9 3 -1 1102.69 1047.26 -9 3 1 355.22 794.19 -9 -3 1 629.35 1326.88 9 3 0 1660.80 1461.48 9 -3 0 1352.50 1011.61 9 3 0-1991.36 1075.96 -9 3 0 1873.73 917.28 -9 -3 0 2566.68 1429.63 9 3 1 1649.62 1462.79 9 -3 1 1608.07 918.26 9 3 1 1647.41 1121.00 -9 3 -1 788.62 1020.64 -9 -3 -1 1093.05 1521.65 9 3 2 4198.24 1597.22 9 -3 2 3206.66 913.50 9 3 2 5188.03 1277.38 -9 3 -2 2155.03 1294.06 -9 -3 -2 4176.46 1036.88 9 4 -1 1119.64 1420.12 9 4 -1 -576.76 1005.10 -9 4 1 1020.49 737.28 -9 -4 1 264.54 1317.32 9 4 0 3846.28 1530.01 9 4 0 2706.28 1150.77 -9 4 0 1896.62 925.05 -9 -4 0 3789.19 1566.36 9 4 1-1049.70 1314.43 9 4 1 -874.76 654.87 -9 4 -1 841.25 982.50 -9 -4 -1 -200.28 1469.50 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 18156 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 Si2 Si 0.69227(18) 0.60698(6) 0.84204(11) 0.0390(3) Uani 1 1 d . . . . . O4 O 0.7022(4) 0.50750(15) 0.7872(3) 0.0418(6) Uani 1 1 d . . . . . O5 O 0.4402(4) 0.36659(19) 0.6216(3) 0.0527(8) Uani 1 1 d . . . . . C10 C 0.8439(5) 0.4660(2) 0.7269(4) 0.0383(9) Uani 1 1 d . . . . . C11 C 0.5855(6) 0.4056(2) 0.6023(4) 0.0386(9) Uani 1 1 d . . . . . C12 C 0.7709(5) 0.3843(2) 0.6701(4) 0.0367(8) Uani 1 1 d . . . . . C13 C 0.5926(5) 0.4758(2) 0.5056(4) 0.0394(9) Uani 1 1 d . . . . . H1 H 0.623981 0.450654 0.423833 0.047 Uiso 1 1 calc R U . . . H2 H 0.693983 0.516363 0.527969 0.047 Uiso 1 1 calc R U . . . C14 C 0.4440(7) 0.6149(3) 0.8934(4) 0.0504(11) Uani 1 1 d . . . . . H3 H 0.360234 0.608688 0.821263 0.076 Uiso 1 1 calc R U . . . H4 H 0.422980 0.670453 0.932370 0.076 Uiso 1 1 calc R U . . . H5 H 0.417524 0.569597 0.953601 0.076 Uiso 1 1 calc R U . . . C15 C 0.7444(6) 0.6834(2) 0.7160(4) 0.0482(10) Uani 1 1 d . . . . . H6 H 0.878322 0.680140 0.694907 0.072 Uiso 1 1 calc R U . . . H7 H 0.713984 0.741193 0.743675 0.072 Uiso 1 1 calc R U . . . H8 H 0.668538 0.669245 0.642458 0.072 Uiso 1 1 calc R U . . . C16 C 0.8536(7) 0.6213(3) 0.9768(4) 0.0567(12) Uani 1 1 d . . . . . H9 H 0.837798 0.573716 1.034889 0.085 Uiso 1 1 calc R U . . . H10 H 0.824062 0.674882 1.019106 0.085 Uiso 1 1 calc R U . . . H11 H 0.984002 0.622722 0.947471 0.085 Uiso 1 1 calc R U . . . C17 C 0.9049(7) 0.3465(3) 0.5741(4) 0.0484(10) Uani 1 1 d . . . . . H12 H 0.932496 0.389254 0.510334 0.073 Uiso 1 1 calc R U . . . H13 H 0.846119 0.296683 0.535110 0.073 Uiso 1 1 calc R U . . . H14 H 1.022243 0.329253 0.615297 0.073 Uiso 1 1 calc R U . . . C18 C 1.0206(6) 0.4933(3) 0.7226(4) 0.0480(10) Uani 1 1 d . . . . . H15 H 1.054951 0.544742 0.763256 0.058 Uiso 1 1 calc R U . . . H16 H 1.112656 0.461331 0.678928 0.058 Uiso 1 1 calc R U . . . C19 C 0.7342(6) 0.3203(2) 0.7747(4) 0.0452(10) Uani 1 1 d . . . . . H17 H 0.851025 0.310324 0.821317 0.068 Uiso 1 1 calc R U . . . H18 H 0.689902 0.266423 0.738939 0.068 Uiso 1 1 calc R U . . . H19 H 0.638199 0.343044 0.830860 0.068 Uiso 1 1 calc R U . . . 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 Si2 0.0460(6) 0.0281(5) 0.0430(5) -0.0026(4) -0.0028(6) -0.0009(5) O4 0.0420(13) 0.0311(13) 0.0524(16) -0.0056(11) 0.0009(14) -0.0022(12) O5 0.0463(16) 0.0432(17) 0.069(2) 0.0152(14) -0.0083(16) -0.0084(13) C10 0.042(2) 0.0291(17) 0.043(2) 0.0039(15) 0.0004(18) 0.0015(15) C11 0.046(2) 0.0282(18) 0.042(2) -0.0026(15) -0.0022(19) -0.0009(16) C12 0.042(2) 0.0291(17) 0.0395(19) 0.0022(14) -0.0015(18) 0.0047(14) C13 0.041(2) 0.0334(19) 0.044(2) 0.0049(16) -0.0030(18) 0.0016(16) C14 0.053(3) 0.044(2) 0.054(2) 0.0012(19) 0.009(2) 0.006(2) C15 0.057(3) 0.0325(19) 0.055(2) 0.0029(17) -0.002(2) -0.0009(17) C16 0.069(3) 0.047(3) 0.054(3) -0.007(2) -0.016(2) -0.005(2) C17 0.056(3) 0.040(2) 0.050(2) -0.0087(19) 0.001(2) 0.0094(19) C18 0.048(2) 0.038(2) 0.057(3) 0.0001(19) 0.001(2) -0.0016(17) C19 0.057(2) 0.0283(18) 0.050(2) 0.0062(16) -0.011(2) -0.0020(17) 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' 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 O4 Si2 C15 109.80(17) . . ? O4 Si2 C14 102.06(18) . . ? C15 Si2 C14 111.6(2) . . ? O4 Si2 C16 111.19(18) . . ? C15 Si2 C16 111.6(2) . . ? C14 Si2 C16 110.2(2) . . ? C10 O4 Si2 130.2(2) . . ? C18 C10 O4 124.2(4) . . ? C18 C10 C12 125.7(4) . . ? O4 C10 C12 110.1(3) . . ? O5 C11 C13 120.9(4) . . ? O5 C11 C12 122.2(3) . . ? C13 C11 C12 116.9(3) . . ? C10 C12 C17 112.9(3) . . ? C10 C12 C19 108.7(3) . . ? C17 C12 C19 110.5(3) . . ? C10 C12 C11 107.3(3) . . ? C17 C12 C11 107.4(3) . . ? C19 C12 C11 110.0(3) . . ? C11 C13 C13 112.7(4) . 3_666 ? C11 C13 H1 109.1 . . ? C13 C13 H1 109.1 3_666 . ? C11 C13 H2 109.1 . . ? C13 C13 H2 109.1 3_666 . ? H1 C13 H2 107.8 . . ? Si2 C14 H3 109.5 . . ? Si2 C14 H4 109.5 . . ? H3 C14 H4 109.5 . . ? Si2 C14 H5 109.5 . . ? H3 C14 H5 109.5 . . ? H4 C14 H5 109.5 . . ? Si2 C15 H6 109.5 . . ? Si2 C15 H7 109.5 . . ? H6 C15 H7 109.5 . . ? Si2 C15 H8 109.5 . . ? H6 C15 H8 109.5 . . ? H7 C15 H8 109.5 . . ? Si2 C16 H9 109.5 . . ? Si2 C16 H10 109.5 . . ? H9 C16 H10 109.5 . . ? Si2 C16 H11 109.5 . . ? H9 C16 H11 109.5 . . ? H10 C16 H11 109.5 . . ? C12 C17 H12 109.5 . . ? C12 C17 H13 109.5 . . ? H12 C17 H13 109.5 . . ? C12 C17 H14 109.5 . . ? H12 C17 H14 109.5 . . ? H13 C17 H14 109.5 . . ? C10 C18 H15 120.0 . . ? C10 C18 H16 120.0 . . ? H15 C18 H16 120.0 . . ? C12 C19 H17 109.5 . . ? C12 C19 H18 109.5 . . ? H17 C19 H18 109.5 . . ? C12 C19 H19 109.5 . . ? H17 C19 H19 109.5 . . ? H18 C19 H19 109.5 . . ? 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 Si2 O4 1.671(3) . ? Si2 C15 1.848(4) . ? Si2 C14 1.854(5) . ? Si2 C16 1.857(5) . ? O4 C10 1.365(5) . ? O5 C11 1.219(5) . ? C10 C18 1.326(6) . ? C10 C12 1.512(5) . ? C11 C13 1.516(5) . ? C11 C12 1.540(5) . ? C12 C17 1.527(5) . ? C12 C19 1.531(5) . ? C13 C13 1.522(7) 3_666 ? C13 H1 0.9900 . ? C13 H2 0.9900 . ? C14 H3 0.9800 . ? C14 H4 0.9800 . ? C14 H5 0.9800 . ? C15 H6 0.9800 . ? C15 H7 0.9800 . ? C15 H8 0.9800 . ? C16 H9 0.9800 . ? C16 H10 0.9800 . ? C16 H11 0.9800 . ? C17 H12 0.9800 . ? C17 H13 0.9800 . ? C17 H14 0.9800 . ? C18 H15 0.9500 . ? C18 H16 0.9500 . ? C19 H17 0.9800 . ? C19 H18 0.9800 . ? C19 H19 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Si2 O4 C10 55.4(4) . . . . ? C14 Si2 O4 C10 173.9(3) . . . . ? C16 Si2 O4 C10 -68.6(4) . . . . ? Si2 O4 C10 C18 14.7(6) . . . . ? Si2 O4 C10 C12 -167.1(3) . . . . ? C18 C10 C12 C17 -16.8(6) . . . . ? O4 C10 C12 C17 165.0(3) . . . . ? C18 C10 C12 C19 106.1(5) . . . . ? O4 C10 C12 C19 -72.1(4) . . . . ? C18 C10 C12 C11 -134.9(4) . . . . ? O4 C10 C12 C11 46.9(4) . . . . ? O5 C11 C12 C10 -127.3(4) . . . . ? C13 C11 C12 C10 55.1(4) . . . . ? O5 C11 C12 C17 111.1(4) . . . . ? C13 C11 C12 C17 -66.5(4) . . . . ? O5 C11 C12 C19 -9.2(5) . . . . ? C13 C11 C12 C19 173.2(3) . . . . ? O5 C11 C13 C13 32.9(6) . . . 3_666 ? C12 C11 C13 C13 -149.4(4) . . . 3_666 ?