#------------------------------------------------------------------------------ #$Date: 2014-08-18 08:23:31 +0300 (Mon, 18 Aug 2014) $ #$Revision: 122172 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/73/1517394.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_1517394 loop_ _publ_author_name 'Wu, Yi-Biao' 'Tang, Yu' 'Luo, Guo-Ying' 'Chen, Yang' 'Hsung, Richard P.' _publ_section_title ; An Approach toward Constructing the Trioxadispiroketal Core in the DEF-Ring of (+)-Spirastrellolide A. ; _journal_name_full 'Organic letters' _journal_page_first 140814153108000 _journal_paper_doi 10.1021/ol502103b _journal_year 2014 _chemical_absolute_configuration rm _chemical_formula_moiety 'C15 H26 O6' _chemical_formula_sum 'C15 H26 O6' _chemical_formula_weight 302.36 _chemical_name_systematic ; ? ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7271(12) _cell_length_b 10.0996(14) _cell_length_c 18.599(3) _cell_measurement_reflns_used 3609 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.92 _cell_measurement_theta_min 2.19 _cell_volume 1639.3(4) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 7.314 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Rigaku Saturn70 CCD' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 16230 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.083 _diffrn_reflns_theta_min 2.190 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.154 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Flack x determined using 795 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.3(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 4313 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.980 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0545 _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^)+(0.0653P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.1290 _reflns_Friedel_coverage 0.741 _reflns_number_gt 2809 _reflns_number_total 4313 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file ol502103b_si_003.cif _[local]_cod_data_source_block shelxl _cod_database_code 1517394 _diffrn_reflns_laue_measured_fraction_full 0.995 _diffrn_reflns_laue_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.984 _reflns_friedel_fraction_full 0.999 _reflns_friedel_fraction_max 0.973 _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 0.978 _shelx_estimated_absorpt_t_max 0.982 _shelxl_version_number 2013-3 _shelx_res_file ; TITL _r131212g CELL 0.71075 8.72710 10.09960 18.59910 90.000 90.000 90.000 ZERR 4 0.00120 0.00140 0.00260 0.000 0.000 0.000 LATT -1 SYMM .50+X, .50-Y, -Z SYMM -X, .50+Y, .50-Z SYMM .50-X, -Y, .50+Z SFAC C H O UNIT 60 104 24 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 LIST 4 HTAB O5 O4_$2 EQIV $2 x-1/2, -y+1/2, -z HTAB C15 O3 HTAB C11 O6_$1 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB C5 O6 SIZE 0.240 0.220 0.200 CONF HTAB WPDB -2 SHEL 99999.000000 0.000000 TEMP 20.1 WGHT 0.065300 FVAR 3.27216 O1 3 0.403594 0.043709 0.185518 11.00000 0.04080 0.04084 = 0.04344 0.00277 -0.00269 -0.00142 O2 3 0.294494 0.191371 0.100382 11.00000 0.03735 0.04490 = 0.04475 0.00707 0.00565 0.00123 O3 3 0.325625 -0.157298 -0.013563 11.00000 0.09342 0.04708 = 0.07227 -0.01224 -0.01348 -0.00917 O4 3 0.547346 0.055183 -0.036631 11.00000 0.04673 0.06948 = 0.04871 -0.01156 0.00721 0.00170 O5 3 0.324247 0.348758 -0.030377 11.00000 0.05655 0.06331 = 0.05190 0.01508 -0.00039 0.00733 O6 3 0.512540 0.251475 0.211676 11.00000 0.05539 0.04008 = 0.06297 0.00235 -0.00200 -0.00582 C1 1 0.270063 0.076420 0.144215 11.00000 0.03641 0.04762 = 0.04474 0.00877 0.00097 -0.00421 C2 1 0.241130 -0.042380 0.095498 11.00000 0.04502 0.05284 = 0.05405 0.00659 -0.00423 -0.01287 AFIX 23 H2A 2 0.144782 -0.029922 0.070391 11.00000 -1.20000 H2B 2 0.232078 -0.121455 0.124792 11.00000 -1.20000 AFIX 0 C3 1 0.369236 -0.062318 0.040347 11.00000 0.05258 0.04094 = 0.05189 -0.00337 -0.00576 -0.00527 AFIX 13 H3 2 0.461628 -0.093556 0.065028 11.00000 -1.20000 AFIX 0 C4 1 0.405136 0.066303 0.001231 11.00000 0.03741 0.04978 = 0.04187 -0.00265 -0.00016 -0.00080 AFIX 13 H4 2 0.322587 0.086808 -0.032710 11.00000 -1.20000 AFIX 0 C5 1 0.425440 0.181054 0.053723 11.00000 0.03270 0.04432 = 0.04042 0.00253 0.00473 0.00054 AFIX 13 H5 2 0.516194 0.163650 0.083280 11.00000 -1.20000 AFIX 0 C6 1 0.444976 0.314384 0.017749 11.00000 0.04264 0.04794 = 0.05065 0.00578 0.00422 -0.00242 AFIX 23 H6A 2 0.452104 0.381961 0.054657 11.00000 -1.20000 H6B 2 0.540879 0.314355 -0.008613 11.00000 -1.20000 AFIX 0 C7 1 0.135499 0.109714 0.192567 11.00000 0.04120 0.06908 = 0.05837 0.01035 0.00876 -0.00135 AFIX 23 H7A 2 0.101046 0.029920 0.216674 11.00000 -1.20000 H7B 2 0.051492 0.142549 0.163441 11.00000 -1.20000 AFIX 0 C8 1 0.177634 0.213320 0.248568 11.00000 0.05286 0.07167 = 0.06190 0.00093 0.01742 0.00774 AFIX 23 H8A 2 0.198729 0.297037 0.225002 11.00000 -1.20000 H8B 2 0.092313 0.226249 0.281247 11.00000 -1.20000 AFIX 0 C9 1 0.317895 0.169030 0.290559 11.00000 0.06269 0.07667 = 0.04738 -0.00432 0.00903 0.00028 AFIX 23 H9A 2 0.348767 0.239493 0.322903 11.00000 -1.20000 H9B 2 0.291211 0.092582 0.319540 11.00000 -1.20000 AFIX 0 C10 1 0.450977 0.133830 0.242509 11.00000 0.05091 0.04214 = 0.04185 -0.00103 0.00034 -0.00574 C11 1 0.585204 0.066393 0.279475 11.00000 0.05469 0.05293 = 0.04970 0.00463 -0.00816 -0.00552 AFIX 23 H11A 2 0.571257 -0.028832 0.281293 11.00000 -1.20000 H11B 2 0.599519 0.099821 0.327904 11.00000 -1.20000 AFIX 0 C12 1 0.719241 0.103929 0.231032 11.00000 0.04784 0.07630 = 0.07073 0.00654 -0.00651 0.00090 AFIX 23 H12A 2 0.815309 0.103019 0.257257 11.00000 -1.20000 H12B 2 0.726923 0.044770 0.190105 11.00000 -1.20000 AFIX 0 C13 1 0.676950 0.242415 0.207866 11.00000 0.05903 0.06048 = 0.05829 0.00094 -0.00201 -0.02002 AFIX 23 H13A 2 0.723867 0.307131 0.239495 11.00000 -1.20000 H13B 2 0.711844 0.258813 0.159157 11.00000 -1.20000 AFIX 0 C14 1 0.356477 -0.289054 0.003501 11.00000 0.15650 0.05021 = 0.10466 -0.01080 -0.00396 -0.00523 AFIX 137 H14A 2 0.461146 -0.297258 0.018740 11.00000 -1.20000 H14B 2 0.339736 -0.343448 -0.038092 11.00000 -1.20000 H14C 2 0.289792 -0.317175 0.041605 11.00000 -1.20000 AFIX 0 C15 1 0.538152 0.027155 -0.110604 11.00000 0.08082 0.10949 = 0.05084 -0.01673 0.01488 -0.01525 AFIX 137 H15A 2 0.496657 -0.060001 -0.117325 11.00000 -1.20000 H15B 2 0.638687 0.031416 -0.131425 11.00000 -1.20000 H15C 2 0.472841 0.090926 -0.133535 11.00000 -1.20000 AFIX 0 H1 2 0.244042 0.365102 -0.001367 11.00000 0.11215 HKLF 4 REM _r131212g REM R1 = 0.0545 for 2809 Fo > 4sig(Fo) and 0.0851 for all 4313 data REM 196 parameters refined using 0 restraints END WGHT 0.0653 0.0000 REM Instructions for potential hydrogen bonds HTAB C5 O6 HTAB C11 O6_$1 HTAB C15 O3 HTAB O5 O4_$2 REM Highest difference peak 0.154, deepest hole -0.198, 1-sigma level 0.046 Q1 1 0.7184 0.2347 0.3207 11.00000 0.05 0.15 Q2 1 0.6184 0.2037 0.3312 11.00000 0.05 0.15 Q3 1 0.5497 0.1802 0.0930 11.00000 0.05 0.14 Q4 1 0.6732 0.1881 0.3083 11.00000 0.05 0.14 Q5 1 0.3143 -0.4527 0.0350 11.00000 0.05 0.14 ; _shelx_res_checksum 62745 _shelx_hkl_file ; 0 -1 0 -13.16 12.69 0 1 0 -6.71 14.53 0 1 0 -10.09 14.14 0 -1 0 12.29 14.11 0 0 -2 1133.02 31.31 0 0 -2 1248.03 26.61 0 0 2 1080.30 23.93 0 0 2 1164.57 38.32 0 1 150368.29 814.95 -1 0 0 5.07 4.71 1 0 0 -10.59 18.56 -1 0 0 -5.16 14.52 1 0 0 2.01 4.32 1 0 0 235.31 20.56 -1 0 0 -29.45 29.08 0 -1 225475.62 422.92 0 1 -225987.95 431.30 0 1 -224133.48 393.56 0 -1 224498.16 399.22 0 1 -224024.23 392.46 0 1 223675.46 388.80 0 -1 -224450.49 401.37 0 1 224539.32 404.81 0 -1 -226770.11 440.58 0 -1 223817.36 394.21 -1 1 047897.62 779.86 -1 -1 049238.26 808.34 1 1 048108.44 786.89 1 1 158589.70 1572.56 -1 -1 -154066.66 882.03 1 1 -152198.01 853.60 -1 -1 155058.32 1478.08 -1 1 -152238.80 850.42 0 0 3 -32.15 106.45 0 0 -3 -89.15 52.54 0 0 3 -19.72 34.76 0 0 -3 -17.06 55.06 -1 1 -2 4045.80 80.65 1 -1 2 3795.05 87.44 1 1 2 4076.55 82.07 1 -1 -2 3923.67 94.00 -1 1 -2 3726.41 80.06 1 -1 2 4062.10 92.48 1 1 -2 4256.03 87.82 -1 -1 2 3860.57 76.57 -1 -1 -2 4083.03 84.21 1 -1 2 4208.01 76.44 -1 1 2 4326.15 86.40 -1 -1 -2 4040.48 74.97 -1 1 2 4002.37 77.77 1 -1 -2 4001.04 78.90 1 1 2 4260.18 88.04 -1 -1 -2 4064.91 108.99 -1 -1 2 3892.92 69.47 1 1 -2 4228.38 154.19 0 -1 317627.02 303.36 0 -1 -317832.95 297.66 0 1 -318059.05 298.40 0 -1 317888.80 294.16 0 -1 -317723.70 299.19 0 -1 317808.46 306.43 0 1 -316929.09 291.49 0 1 317152.12 287.29 0 -1 -318340.34 308.09 0 1 -317703.33 292.82 1 0 -339027.85 636.93 1 0 336407.50 593.43 -1 0 -339147.83 647.41 1 0 339242.08 642.75 -1 0 338140.13 624.51 -1 0 -334877.16 568.67 -1 0 -340650.59 674.37 0 2 0 6005.07 121.09 0 -2 0 5166.86 105.32 0 -2 0 5390.81 112.42 0 2 0 5489.94 121.96 -1 1 -3 4918.23 85.27 1 1 -3 4842.07 213.97 -1 -1 -3 4955.31 99.83 1 -1 3 5708.09 130.62 -1 -1 3 4726.57 105.75 1 1 -3 4706.63 115.56 1 -1 3 4281.74 81.43 -1 -1 3 4783.44 121.32 1 -1 3 4924.92 99.33 1 -1 -3 5376.91 116.86 -1 1 -3 5074.49 120.36 1 -1 -3 5018.47 93.87 -1 1 -3 5020.31 104.96 1 1 3 5061.96 99.19 -1 -1 -3 5232.49 109.86 1 1 3 5000.61 98.54 -1 1 3 4677.88 129.45 0 -2 -2 2580.55 75.29 0 -2 2 2468.46 72.98 0 2 2 2135.96 54.62 0 2 -2 2544.01 86.96 0 2 -2 2500.17 77.36 0 -2 -2 2468.14 83.02 0 -2 2 2612.95 77.92 0 2 2 2336.55 99.14 -1 -2 020138.23 342.07 -1 2 020790.95 377.18 1 2 021219.02 359.40 1 -2 021281.22 356.18 1 -2 023647.69 402.89 -1 -2 021230.54 360.68 -1 -2 021757.02 376.55 -1 2 020230.33 330.03 1 2 021282.38 371.92 1 -2 020772.71 340.88 -2 0 0 4675.67 105.01 2 0 0 4590.80 154.72 -2 0 0 4043.71 75.58 2 0 0 4496.11 83.10 -2 0 0 4253.21 94.84 2 0 0 4630.92 103.12 -1 -2 -112092.31 236.60 -1 2 112224.34 220.92 1 -2 112471.79 215.70 -1 -2 112194.94 216.22 1 -2 -111592.46 213.85 1 2 -112855.69 242.38 1 2 112313.99 220.69 -1 -2 112739.14 243.38 1 -2 112381.84 208.27 1 2 112907.82 239.76 -1 -2 -112587.65 229.20 -1 2 -112416.83 204.75 -1 2 112558.30 210.88 1 -2 -112168.57 204.83 -1 -2 -112994.44 234.64 1 2 -112847.68 229.72 1 -2 113030.75 234.23 -1 2 -112237.74 223.49 0 -1 -4 2841.60 74.49 0 -1 4 3033.73 226.18 0 1 -4 3100.68 127.72 0 1 -4 2755.95 65.27 0 -1 4 2844.39 64.25 0 1 4 2967.75 67.48 0 -1 -4 2972.85 66.16 0 1 4 2843.06 71.78 0 1 -4 2957.79 62.02 0 -1 4 2557.14 58.88 -1 0 -411271.85 223.15 1 0 410499.72 181.41 -1 0 -411070.12 195.67 1 0 410663.20 199.10 -1 0 -411070.59 197.31 1 0 -412415.57 215.46 1 0 -410731.17 176.09 -1 0 411678.04 207.08 2 1 0 3038.16 56.75 2 -1 0 3341.92 102.49 -2 1 0 3434.09 77.20 2 1 0 3160.12 93.44 2 -1 0 3386.37 68.90 2 1 0 2960.72 90.22 2 -1 0 3438.51 79.97 -2 -1 0 3290.98 174.85 2 -1 0 3446.09 94.07 -2 1 0 3162.69 92.26 -2 -1 0 3023.75 82.00 1 2 -228949.63 498.01 1 -2 227534.79 467.62 -1 -2 227718.54 482.97 -1 2 227593.76 454.43 1 2 -227831.26 469.73 -1 2 -227990.76 475.46 1 2 226257.46 552.23 1 -2 -227042.04 444.64 -1 2 -226842.41 439.24 -1 2 -227194.10 441.31 -1 2 227254.00 462.11 -1 -2 225872.09 447.78 1 2 226810.66 447.12 -1 -2 -226626.79 472.37 -1 -2 -228815.95 478.23 1 -2 -227587.89 465.82 1 -2 228280.25 468.61 1 2 227253.90 466.34 -1 -2 -224688.80 419.72 -1 2 -227191.71 459.68 -2 0 -2 1698.99 61.98 2 0 -2 1713.10 54.56 -2 0 -2 1588.61 75.17 2 0 -2 1730.78 43.14 -2 0 -2 1684.04 70.37 2 0 2 1722.83 59.15 -2 0 2 1612.56 93.29 2 0 2 1622.80 66.18 2 0 -2 1658.21 63.57 2 0 2 1761.18 74.07 -2 -1 -1 8471.83 198.00 2 1 -1 8782.52 186.57 2 -1 1 8505.19 157.22 2 -1 -1 8713.49 157.63 -2 -1 1 8498.87 214.56 2 1 1 8269.28 154.59 2 -1 1 8816.20 167.69 -2 1 1 8207.63 153.76 2 -1 -1 8055.76 140.43 2 1 1 9422.20 184.45 -2 1 -1 8555.33 163.40 2 -1 1 8420.25 163.17 -2 -1 -1 9400.56 401.07 2 1 -1 8956.37 159.04 -2 1 -1 8831.26 155.43 -2 1 1 8478.73 166.98 2 -1 -1 8917.50 160.12 -2 -1 1 8272.77 156.93 -2 1 -1 8504.14 157.30 -2 1 1 8008.58 145.43 2 1 -1 8924.80 158.10 0 2 339658.43 655.28 0 2 340114.04 660.07 0 -2 340288.13 674.69 0 2 -339039.14 641.21 0 -2 338800.56 635.46 0 -2 -339292.97 651.61 0 2 -338433.46 645.45 0 2 -337333.71 618.96 0 -2 -339917.91 662.73 -1 -1 4 9716.19 214.09 1 -1 410063.90 178.73 -1 -1 -4 9388.55 171.28 1 -1 -410049.12 182.96 1 -1 4 9869.75 195.86 -1 1 -4 9637.37 209.62 -1 1 4 9494.72 169.07 1 1 410991.50 194.69 1 -1 410075.46 179.33 1 1 -4 9826.44 334.21 1 -1 -4 9893.85 192.76 -1 1 -4 9742.90 165.46 -1 -1 -4 9691.71 178.43 1 1 -410110.57 180.81 -1 1 -410052.80 194.35 1 1 4 9575.39 178.47 -1 -1 410540.39 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10 14 125.66 118.27 -6 1 21 113.59 91.92 -10 4 -10 84.38 62.33 10 4 -10 6.15 43.76 10 4 10 75.70 45.66 -10 -4 -10 35.67 52.78 7 8 -13 143.99 173.69 7 8 13 163.73 87.17 -8 6 -14 88.37 76.78 -7 8 -13 87.37 85.02 8 6 14 135.08 48.82 -8 6 14 50.09 48.14 -8 -6 -14 93.74 81.62 -5 -4 -21 -13.97 90.81 -5 4 21 69.26 57.97 -5 -4 -21 -24.69 75.49 5 4 -21 63.20 118.41 -5 4 -21 14.36 38.38 5 4 21 -5.58 44.93 -5 4 -21 -10.05 85.65 5 4 -21 75.54 73.48 0 13 6 22.32 31.05 -6 -5 -19 226.48 195.97 -6 5 19 221.13 110.18 0 -12 -11 24.89 82.83 0 12 11 -3.20 50.93 0 12 -11 105.28 111.74 6 5 19 146.82 105.70 -6 5 -19 283.48 138.71 6 5 -19 172.92 112.47 0 12 11 -1.43 39.94 6 5 -19 351.13 174.88 -6 5 -19 199.51 200.18 6 6 -18 325.67 107.38 -6 6 -18 226.51 210.03 3 5 -22 43.77 59.18 -3 -5 -22 -2.17 105.67 6 6 18 163.10 149.81 6 6 -18 110.60 73.92 -3 5 22 50.23 50.70 -6 6 18 281.96 136.37 -3 5 -22 -30.24 72.25 -6 6 -18 155.53 140.20 3 5 22 12.59 54.16 3 5 -22 63.68 37.23 -6 -6 -18 284.25 175.05 -3 -5 -22 8.55 39.86 6 11 6 38.42 64.63 9 8 5 23.53 50.22 -9 8 5 -0.81 48.43 6 11 -6 77.56 85.50 -6 11 6 37.90 30.12 -6 -11 -6 53.60 58.00 -9 -8 -5 -53.28 83.61 9 8 -5 28.51 87.49 -4 12 7 55.36 52.62 4 12 7 51.30 37.96 -4 -12 -7 82.32 106.82 4 12 -7 29.18 38.36 -4 -12 7 29.03 30.86 4 12 -7 44.81 76.22 8 3 17 70.02 50.85 8 3 -17 98.99 109.42 3 12 9 143.35 121.41 -8 -3 -17 103.70 47.45 -8 3 -17 98.69 53.62 3 12 -9 284.23 73.12 3 12 -9 174.18 152.23 -3 12 9 220.25 195.58 3 12 9 238.54 224.00 -1 6 22 97.60 59.74 1 6 -22 54.74 88.36 -7 -10 -7 50.61 88.42 -7 10 7 39.00 48.14 1 6 22 57.19 73.27 -1 6 -22 118.33 92.17 7 10 -7 84.08 71.09 -7 10 -7 59.70 81.52 7 10 7 80.29 56.43 -5 -12 3 108.62 74.33 -5 -12 -3 145.39 88.29 -4 4 -22 41.86 52.43 4 4 -22 42.23 79.86 5 12 3 165.04 85.59 4 4 -22 29.39 57.55 -4 -4 -22 -21.18 90.23 -4 4 22 59.99 69.87 1 11 -14 148.19 73.19 -5 12 3 27.53 74.39 1 -11 -14 93.54 64.06 -1 -11 -14 63.71 84.08 1 11 14 -10.45 65.78 5 12 -3 143.14 143.29 -4 -4 -22 46.37 77.41 -1 11 14 32.16 43.63 4 4 22 164.73 91.77 1 3 24 28.52 15.80 -5 2 22 -15.88 74.40 -9 -6 -11 6.31 55.28 -5 2 -22 7.11 74.34 -9 6 -11 72.20 100.73 5 2 22 45.92 61.66 -1 3 24 34.13 50.53 9 6 11 44.55 76.10 5 2 -22 86.38 105.17 5 2 -22 92.13 93.00 1 -3 -24 103.85 78.35 -5 2 -22 18.40 45.85 -1 3 -24 -16.53 114.69 -5 -2 -22 -12.30 56.50 -5 -2 -22 -35.87 84.19 1 -3 24 53.22 35.18 5 -2 -22 26.59 50.68 -1 -3 -24 40.14 88.08 1 3 -24 19.62 72.61 -1 -3 24 -32.11 68.71 1 7 -21 128.69 73.30 -1 -7 -21 123.92 57.06 1 7 -21 53.49 46.34 -1 7 21 72.77 69.92 -1 7 -21 110.19 75.97 -10 -2 -12 103.26 115.72 -10 2 -12 49.57 66.62 10 2 -12 155.25 86.96 10 -2 -12 124.11 117.01 -11 -2 -7 -3.61 58.06 -11 2 -7 43.14 62.67 11 2 -7 60.27 69.70 -10 -6 -6 -49.08 83.04 10 6 6 37.01 55.73 -10 6 -6 37.16 43.35 10 6 -6 44.95 75.28 -11 4 -3 54.36 57.18 11 4 -3 135.91 106.64 11 4 3 -32.25 65.34 -11 -4 -3 27.51 34.98 5 9 -15 30.08 40.48 2 -10 -16 -8.58 63.04 -2 10 16 136.68 134.94 2 10 16 30.17 62.17 2 10 -16 -29.63 56.90 -5 9 15 52.05 57.04 5 9 15 84.74 43.91 -2 -10 -16 31.05 65.06 5 9 -15 62.40 96.14 -5 9 -15 146.09 119.03 2 10 -16 122.42 79.64 -7 7 -15 161.62 166.08 1 13 6 227.26 171.25 7 7 15 127.13 37.99 1 13 6 280.38 99.69 4 8 -18 66.43 77.89 -4 8 18 92.01 44.42 -1 13 -6 451.81 98.66 4 8 -18 120.98 53.50 7 7 -15 241.91 193.75 -4 8 -18 114.90 99.08 -1 13 6 227.55 131.00 -11 0 -8 39.22 30.80 11 0 -8 -21.96 61.94 -7 7 15 184.72 159.54 -4 -8 -18 185.88 67.14 -1 12 -11 91.06 81.11 -1 -12 -11 109.22 72.65 -1 12 11 65.92 64.27 1 -12 -11 65.20 53.68 0 -5 -23 39.92 127.14 -1 12 11 78.75 94.34 1 12 -11 101.90 82.15 1 12 11 12.33 29.49 -7 3 -19 48.34 42.69 -7 3 19 50.20 83.65 7 3 -19 57.14 46.71 3 13 0 27.25 30.26 -3 -13 0 -21.63 84.48 7 3 19 108.30 80.49 7 3 -19 34.91 133.07 -7 -3 -19 184.75 90.70 8 9 7 122.87 89.60 -8 9 7 11.73 25.82 -8 9 -7 10.93 70.15 -8 -9 -7 69.65 83.61 8 0 -18 83.05 56.82 -8 0 -18 -7.09 74.97 3 13 -1 144.62 57.56 -3 -13 1 34.93 47.32 9 7 9 129.21 64.64 9 7 -9 171.85 94.03 -9 -7 -9 85.06 138.31 3 13 1 14.52 48.26 -3 -13 -1 36.51 75.19 4 2 23 54.24 59.18 -4 -2 -23 35.24 76.34 4 -2 -23 -65.19 135.55 4 2 -23 -78.35 107.31 -4 2 -23 36.15 72.57 -4 -2 -23 113.87 57.55 11 3 -6 257.40 107.05 11 3 6 62.79 50.52 -11 -3 -6 67.72 62.17 -11 3 -6 72.40 96.61 2 13 5 69.16 28.85 2 13 5 -31.10 45.90 2 13 -5 -28.29 58.89 -2 -13 5 14.27 40.75 -3 0 24 79.00 71.54 -3 0 -24 25.73 52.84 3 0 -24 112.86 119.13 -2 -9 -18 34.98 45.24 2 9 -18 25.79 64.04 2 9 -18 57.95 99.80 -2 9 18 18.34 50.50 2 -9 -18 59.34 94.41 3 0 24 39.07 39.94 0 -8 -20 93.27 78.50 -11 1 -8 61.33 47.77 -11 -1 -8 -37.53 67.52 11 1 -8 54.10 67.52 -6 4 -20 -82.32 50.50 -6 4 20 41.72 61.25 -5 -12 4 70.39 42.88 -6 4 -20 66.42 46.77 5 12 -4 133.17 108.98 -6 -4 -20 -64.21 76.92 -5 12 4 -7.75 55.08 5 12 4 88.88 77.08 -5 -12 -4 -37.04 89.74 6 4 -20 43.90 34.07 6 4 20 -15.83 31.71 -8 -1 -18 131.42 117.40 -3 -13 -2 145.34 198.42 -6 2 -21 36.76 65.61 6 -2 -21 253.55 148.41 8 -1 -18 105.18 90.57 3 13 2 127.64 76.50 -6 2 21 83.29 97.10 6 2 21 76.89 86.32 -6 -2 -21 100.65 57.21 8 -1 -18 72.94 61.60 -8 1 -18 31.38 57.10 8 1 -18 -17.40 101.48 -6 2 -21 108.96 83.76 6 2 -21 46.36 33.15 -3 -13 2 237.11 174.00 7 9 -11 26.44 103.71 1 5 -23 50.39 57.38 -1 -5 -23 66.18 85.55 7 9 11 99.61 74.32 9 -4 -14 311.74 182.96 -7 9 -11 131.48 87.62 9 4 -14 546.81 160.45 1 5 23 100.95 74.98 -6 7 17 96.48 78.97 -6 7 -17 35.60 51.90 -6 7 -17 91.01 48.14 6 7 -17 125.34 128.16 6 7 -17 29.58 38.51 -6 -7 -17 -21.81 96.28 6 7 17 11.26 39.28 3 8 -19 83.55 86.13 -3 8 19 51.28 70.24 -3 -8 -19 71.87 67.80 3 8 -19 127.06 111.28 -3 8 -19 135.52 145.22 5 8 -17 59.51 34.74 -5 -8 -17 22.23 42.79 -5 8 -17 68.88 81.91 5 8 -17 61.19 100.64 -5 8 17 30.08 72.96 -11 -4 -4 45.40 56.69 11 4 4 96.72 64.36 11 4 -4 187.52 107.40 -11 4 -4 123.40 78.57 -10 5 -9 59.03 48.26 10 5 -9 103.94 78.85 -10 -5 -9 -18.16 75.46 10 5 9 92.81 39.84 3 11 -13 106.53 69.98 -3 11 13 124.78 62.07 3 11 13 51.75 46.72 -3 -1 24 17.88 36.53 -3 -1 -24 46.22 57.01 3 -11 -13 55.22 45.19 3 1 24 45.59 50.68 3 -1 24 103.56 63.44 3 11 -13 48.82 74.62 -3 1 -24 73.15 98.69 -10 -7 0 0.17 34.05 -9 -8 -6 -32.43 84.22 -9 8 6 19.72 28.94 9 8 6 112.20 57.84 -10 -7 -1 98.55 86.86 -5 10 -13 129.66 87.58 -1 -8 -20 2.76 22.01 5 10 -13 305.05 109.92 9 5 13 130.45 47.34 5 10 -13 215.98 176.70 0 13 7 98.13 78.72 0 13 7 71.73 63.35 0 13 -7 267.39 127.99 7 0 -20 31.17 48.43 -7 0 -20 -64.27 61.05 7 0 -20 91.20 63.03 -6 11 7 125.91 127.64 6 11 -7 362.24 134.97 -6 11 -7 246.57 180.90 -6 -11 -7 137.70 120.99 -3 -13 -3 -71.01 70.78 3 13 -3 38.69 40.11 3 13 -3 27.20 44.59 -3 -13 3 55.24 69.10 3 13 3 112.93 75.92 10 0 -13 76.07 80.80 9 -3 -15 58.08 102.19 9 3 15 57.61 45.52 -6 10 -11 -2.66 71.82 6 10 -11 333.98 159.71 9 0 -16 -2.86 81.21 5 11 -10 161.47 86.30 -5 11 -10 81.82 120.60 3 4 23 64.10 50.04 3 4 -23 93.37 68.13 -3 -4 -23 53.19 51.00 -3 4 -23 108.27 76.89 3 4 -23 77.27 100.50 -3 -4 -23 18.35 39.06 -2 -6 -22 49.86 65.68 2 6 -22 76.41 93.58 2 11 -14 107.26 85.27 -2 11 14 51.71 25.26 10 7 -2 140.94 85.45 2 -11 -14 5.50 37.63 2 11 14 19.60 47.25 -2 -11 -14 116.04 95.50 -10 -7 -2 52.74 47.39 2 3 24 79.30 60.61 -2 -3 24 38.23 37.07 -2 3 -24 74.83 92.50 -2 -3 -24 118.36 144.91 4 12 -8 125.20 88.94 4 12 8 79.01 61.02 0 0 25 22.58 43.30 4 12 -8 83.84 91.85 2 7 -21 66.73 71.50 -2 -7 -21 37.77 37.22 10 6 7 61.16 76.07 -10 -6 -7 47.94 70.36 2 7 -21 46.71 55.06 -7 10 8 128.56 72.20 -7 -10 -8 88.23 69.74 -7 10 -8 115.99 73.36 -7 1 -20 53.06 77.23 7 -1 -20 71.43 58.16 7 1 -20 66.05 47.22 -8 7 -13 135.68 98.41 8 7 13 103.30 64.40 -7 -1 -20 79.70 51.57 1 13 7 140.55 124.28 1 13 -7 117.97 90.10 10 1 -13 127.55 89.54 1 13 7 83.87 51.21 10 -1 -13 25.03 71.23 -5 -12 -5 74.58 66.95 -5 12 -5 171.30 96.58 5 12 5 27.23 72.51 -5 -12 5 53.49 82.29 5 12 -5 123.57 80.67 -11 2 -8 245.17 69.71 11 2 -8 411.32 148.52 -11 -2 -8 109.21 126.07 4 11 -12 102.07 61.77 4 11 -12 127.88 63.56 2 13 6 54.40 21.02 9 -1 -16 81.84 119.97 2 13 6 71.54 68.94 -2 -13 6 22.38 39.36 2 13 -6 -5.60 57.97 9 1 -16 347.30 120.47 2 -12 -11 -6.68 84.77 -2 12 11 52.73 38.60 2 12 -11 40.39 37.75 2 12 11 20.19 37.47 0 10 17 175.21 73.78 5 3 -22 -39.00 91.28 0 -10 -17 130.34 67.84 -5 -3 -22 1.95 27.14 5 -3 -22 -104.42 106.34 -5 3 -22 68.00 43.28 -5 3 -22 21.23 74.13 5 3 22 70.30 46.00 -5 -3 -22 49.16 55.00 8 -2 -18 27.79 55.78 8 -2 -18 11.44 58.57 0 1 25 73.59 63.71 0 -1 25 56.02 75.91 8 8 11 34.32 62.55 -8 8 -11 32.04 67.94 10 3 -12 55.59 93.45 -11 4 -5 60.30 36.03 -11 -4 -5 51.77 71.18 11 4 -5 202.89 106.86 11 4 5 122.59 51.80 -11 -3 -7 2.72 77.42 -11 3 -7 43.09 48.06 11 3 -7 -61.90 78.09 3 12 -10 46.37 29.79 3 12 -10 12.62 45.90 3 12 10 22.80 57.90 10 7 3 33.04 64.20 -8 -9 -8 53.12 49.07 -1 0 25 148.04 85.12 1 0 25 119.87 81.45 10 4 -11 56.13 77.68 -8 9 -8 87.32 91.88 -10 -7 -3 26.94 42.11 10 4 11 31.44 34.22 -8 -10 0 45.68 60.70 -3 -13 4 45.13 37.60 3 13 -4 80.23 67.55 3 13 4 50.07 65.96 3 13 4 49.89 29.56 0 -4 24 55.80 38.06 -3 -2 24 -25.80 66.76 3 2 24 64.51 67.11 11 0 -9 956.01 145.13 -3 2 -24 -13.46 100.64 -3 -2 -24 -85.76 109.92 -8 -10 1 7.31 36.10 -8 -10 -1 54.25 24.20 -8 10 1 65.85 55.92 -7 5 -18 77.58 62.53 -7 5 -18 58.86 35.02 7 5 18 15.36 51.96 -7 5 18 -33.93 72.39 8 5 16 33.30 31.07 -8 5 16 12.83 40.79 -2 -5 -23 116.94 134.40 2 5 -23 47.39 77.98 4 3 23 62.60 40.78 -4 -3 -23 -11.56 58.72 -4 3 -23 53.63 44.73 0 12 12 139.78 95.81 -4 -3 -23 -16.68 89.02 4 3 -23 12.12 101.22 -1 -10 -17 0.32 36.03 1 -10 -17 -16.46 45.05 -1 10 17 -9.24 68.25 1 1 25 97.27 42.57 1 -1 25 79.48 63.55 -7 -11 0 66.03 45.05 -7 11 0 54.41 75.23 -1 -1 25 73.13 40.30 -7 6 17 48.34 96.16 7 6 17 34.59 33.30 -7 6 -17 106.98 95.04 -7 6 -17 138.52 75.03 -8 -10 2 41.31 26.31 8 4 17 24.49 45.25 11 1 -9 91.11 82.67 -9 -8 -7 54.83 99.94 -7 -11 -1 50.48 52.96 -8 -10 -2 46.54 43.34 -7 -11 1 42.31 34.53 -11 -1 -9 62.49 49.67 9 7 10 4.93 52.62 6 9 -14 206.64 131.28 11 5 0 87.13 76.01 -6 9 -14 153.70 115.61 -6 3 -21 85.67 83.05 6 -3 -21 150.06 97.26 6 3 -21 70.08 50.52 -6 3 -21 85.19 66.82 6 3 21 34.19 38.56 -6 -3 -21 58.89 72.76 -11 -5 -1 80.18 42.40 0 11 15 51.69 61.41 2 8 -20 71.51 73.12 11 5 -1 174.65 74.58 -2 -8 -20 109.89 64.48 0 -11 -15 88.67 75.66 11 5 1 106.40 68.09 -7 8 -14 113.10 68.21 0 -9 -19 51.34 23.99 5 6 -20 19.73 36.31 -5 6 -20 34.65 69.97 -5 6 20 41.22 73.78 -5 6 -20 -17.89 47.22 4 6 -21 216.50 112.55 5 6 -20 302.09 130.93 -4 6 -21 -49.71 86.48 -4 -6 -21 52.83 56.31 -5 -6 -20 47.08 59.67 4 6 -21 31.97 49.35 -4 -6 -21 -40.46 67.48 3 10 -16 27.59 83.67 3 -10 -16 20.20 36.84 3 10 -16 89.30 101.26 -3 10 16 -34.57 49.69 -7 -2 -20 147.59 99.11 7 2 -20 194.17 127.71 7 2 20 156.42 79.61 -7 2 -20 96.65 84.10 7 -2 -20 179.96 70.93 -4 9 17 40.25 44.19 4 9 -17 130.44 83.00 -10 -7 -4 11.08 40.13 10 7 4 60.60 40.05 4 9 -17 46.60 42.20 -6 8 16 27.46 42.25 -6 8 -16 76.54 78.11 4 10 -15 52.27 59.49 10 2 -13 174.54 121.32 4 -10 -15 37.31 30.93 4 10 -15 117.41 80.21 10 -2 -13 110.51 91.27 -4 10 15 50.74 42.64 -7 -11 -2 43.09 85.91 1 12 -12 240.38 149.26 1 12 12 112.87 52.96 -7 -11 2 17.85 76.38 -1 12 12 207.96 116.35 0 13 8 110.68 83.07 0 13 8 136.05 73.59 9 -2 -16 83.84 63.20 -7 4 19 35.96 61.66 7 4 19 36.38 31.34 -7 4 -19 44.13 49.95 -8 6 15 7.90 72.23 8 6 15 57.68 57.58 -7 4 -19 29.37 29.60 6 11 -8 -4.38 99.55 5 12 -6 -39.05 69.72 -6 11 -8 132.86 90.30 11 5 2 29.05 46.13 11 5 -2 49.61 48.76 -11 -5 -2 38.18 39.31 -11 5 -2 25.83 24.01 0 -2 25 78.53 69.75 -8 -10 -3 44.12 77.44 -8 10 -3 70.76 61.62 10 5 10 -0.90 47.99 3 13 5 30.25 46.43 3 13 5 168.01 124.67 -4 -7 -20 37.00 36.32 -4 7 20 40.68 44.09 3 13 -5 41.10 55.94 -3 -13 5 36.47 38.97 -4 7 -20 34.36 54.86 4 7 -20 211.07 163.86 4 7 -20 76.12 68.86 -5 -5 -21 -16.71 71.71 5 5 -21 -32.12 71.61 5 5 21 44.23 29.46 -5 5 -21 55.24 58.30 -5 5 -21 29.32 45.53 -3 9 18 70.61 47.88 -3 -9 -18 91.47 49.68 3 9 -18 2.04 48.84 3 9 -18 175.47 89.67 -11 -4 -6 13.92 45.29 11 4 6 117.27 75.53 11 4 -6 96.81 73.49 1 -11 -15 53.75 57.76 -1 11 15 102.19 47.60 1 11 15 85.37 53.53 -1 -9 -19 108.30 66.87 1 -9 -19 103.75 87.77 -10 -6 -8 -4.71 89.22 2 13 7 27.35 33.41 -2 -13 7 1.16 26.39 10 6 8 12.62 40.57 2 13 -7 31.45 27.35 2 13 7 -56.07 49.27 -5 7 -19 24.21 48.28 -5 7 19 85.46 45.99 5 7 -19 32.39 68.29 5 7 -19 59.45 102.60 -7 9 -12 0.11 78.27 -4 5 -22 102.27 67.11 4 5 -22 52.58 49.31 4 5 -22 36.93 94.65 -4 -5 -22 48.15 37.99 -4 -5 -22 102.49 57.64 1 13 8 50.66 48.50 1 13 8 91.82 57.44 1 13 -8 68.52 49.71 -7 11 3 96.64 92.38 -7 -11 3 62.43 50.71 4 12 -9 48.76 35.27 -7 11 -3 41.47 57.75 -7 -11 -3 100.66 65.65 4 12 -9 97.98 88.61 -5 0 -23 94.87 72.51 -5 0 -23 85.16 43.35 -9 -9 0 58.71 55.33 -7 10 -9 30.37 60.02 -7 10 9 3.45 82.83 -11 5 -3 6.08 70.33 11 5 3 72.22 45.68 -11 -5 -3 -11.91 51.35 -9 -9 -1 67.79 28.27 -11 -3 -8 95.83 108.33 5 9 -16 59.89 70.78 -5 9 -16 61.80 82.88 -7 7 -16 -7.52 61.09 -10 -7 -5 23.90 47.62 -8 10 4 58.84 52.33 -8 -10 -4 56.66 57.05 5 1 -23 90.26 51.74 -9 -9 -2 16.14 65.49 -6 6 -19 55.46 61.80 -9 9 2 54.41 37.02 9 -4 -15 66.38 63.89 ; _shelx_hkl_checksum 83223 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 O1 O 0.40359(19) 0.04371(18) 0.18552(9) 0.0417(4) Uani 1 1 d . . O2 O 0.2945(2) 0.19137(18) 0.10038(9) 0.0423(4) Uani 1 1 d . . O3 O 0.3256(3) -0.1573(2) -0.01356(12) 0.0709(7) Uani 1 1 d . . O4 O 0.5473(2) 0.0552(2) -0.03663(10) 0.0550(5) Uani 1 1 d . . O5 O 0.3242(3) 0.3488(2) -0.03038(11) 0.0573(6) Uani 1 1 d . . O6 O 0.5125(2) 0.25148(19) 0.21168(11) 0.0528(5) Uani 1 1 d . . C1 C 0.2701(3) 0.0764(3) 0.14422(14) 0.0429(6) Uani 1 1 d . . C2 C 0.2411(3) -0.0424(3) 0.09550(16) 0.0506(7) Uani 1 1 d . . H2A H 0.1448 -0.0299 0.0704 0.061 Uiso 1 1 calc R U H2B H 0.2321 -0.1215 0.1248 0.061 Uiso 1 1 calc R U C3 C 0.3692(3) -0.0623(3) 0.04035(15) 0.0485(7) Uani 1 1 d . . H3 H 0.4616 -0.0936 0.0650 0.058 Uiso 1 1 calc R U C4 C 0.4051(3) 0.0663(3) 0.00123(13) 0.0430(6) Uani 1 1 d . . H4 H 0.3226 0.0868 -0.0327 0.052 Uiso 1 1 calc R U C5 C 0.4254(3) 0.1811(3) 0.05372(14) 0.0391(6) Uani 1 1 d . . H5 H 0.5162 0.1636 0.0833 0.047 Uiso 1 1 calc R U C6 C 0.4450(3) 0.3144(3) 0.01775(16) 0.0471(7) Uani 1 1 d . . H6A H 0.4521 0.3820 0.0547 0.056 Uiso 1 1 calc R U H6B H 0.5409 0.3144 -0.0086 0.056 Uiso 1 1 calc R U C7 C 0.1355(3) 0.1097(3) 0.19257(16) 0.0562(8) Uani 1 1 d . . H7A H 0.1010 0.0299 0.2167 0.067 Uiso 1 1 calc R U H7B H 0.0515 0.1425 0.1634 0.067 Uiso 1 1 calc R U C8 C 0.1776(4) 0.2133(4) 0.24857(18) 0.0621(9) Uani 1 1 d . . H8A H 0.1987 0.2970 0.2250 0.075 Uiso 1 1 calc R U H8B H 0.0923 0.2262 0.2812 0.075 Uiso 1 1 calc R U C9 C 0.3179(4) 0.1690(4) 0.29056(16) 0.0622(9) Uani 1 1 d . . H9A H 0.3488 0.2395 0.3229 0.075 Uiso 1 1 calc R U H9B H 0.2912 0.0926 0.3195 0.075 Uiso 1 1 calc R U C10 C 0.4510(3) 0.1338(3) 0.24251(14) 0.0450(7) Uani 1 1 d . . C11 C 0.5852(3) 0.0664(3) 0.27948(15) 0.0524(7) Uani 1 1 d . . H11A H 0.5713 -0.0288 0.2813 0.063 Uiso 1 1 calc R U H11B H 0.5995 0.0998 0.3279 0.063 Uiso 1 1 calc R U C12 C 0.7192(4) 0.1039(4) 0.23103(19) 0.0650(9) Uani 1 1 d . . H12A H 0.8153 0.1030 0.2573 0.078 Uiso 1 1 calc R U H12B H 0.7269 0.0448 0.1901 0.078 Uiso 1 1 calc R U C13 C 0.6769(4) 0.2424(3) 0.20787(17) 0.0593(8) Uani 1 1 d . . H13A H 0.7239 0.3071 0.2395 0.071 Uiso 1 1 calc R U H13B H 0.7118 0.2588 0.1592 0.071 Uiso 1 1 calc R U C14 C 0.3565(6) -0.2891(4) 0.0035(3) 0.1038(15) Uani 1 1 d . . H14A H 0.4611 -0.2973 0.0187 0.125 Uiso 1 1 calc R U H14B H 0.3397 -0.3434 -0.0381 0.125 Uiso 1 1 calc R U H14C H 0.2898 -0.3172 0.0416 0.125 Uiso 1 1 calc R U C15 C 0.5382(5) 0.0272(4) -0.11060(16) 0.0804(12) Uani 1 1 d . . H15A H 0.4967 -0.0600 -0.1173 0.096 Uiso 1 1 calc R U H15B H 0.6387 0.0314 -0.1314 0.096 Uiso 1 1 calc R U H15C H 0.4728 0.0909 -0.1335 0.096 Uiso 1 1 calc R U H1 H 0.244(6) 0.365(5) -0.001(2) 0.112(16) Uiso 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 O1 0.0408(9) 0.0408(11) 0.0434(9) 0.0028(8) -0.0027(8) -0.0014(8) O2 0.0373(10) 0.0449(10) 0.0447(9) 0.0071(8) 0.0057(8) 0.0012(8) O3 0.0934(16) 0.0471(13) 0.0723(14) -0.0122(11) -0.0135(13) -0.0092(12) O4 0.0467(11) 0.0695(14) 0.0487(10) -0.0116(11) 0.0072(9) 0.0017(10) O5 0.0566(12) 0.0633(14) 0.0519(11) 0.0151(11) -0.0004(11) 0.0073(11) O6 0.0554(12) 0.0401(11) 0.0630(13) 0.0024(9) -0.0020(10) -0.0058(9) C1 0.0364(14) 0.0476(16) 0.0447(13) 0.0088(12) 0.0010(11) -0.0042(12) C2 0.0450(16) 0.0528(17) 0.0541(15) 0.0066(14) -0.0042(13) -0.0129(14) C3 0.0526(17) 0.0409(16) 0.0519(15) -0.0034(13) -0.0058(13) -0.0053(13) C4 0.0374(13) 0.0498(16) 0.0419(13) -0.0026(12) -0.0002(11) -0.0008(13) C5 0.0327(13) 0.0443(15) 0.0404(13) 0.0025(11) 0.0047(10) 0.0005(12) C6 0.0426(15) 0.0479(16) 0.0506(15) 0.0058(13) 0.0042(12) -0.0024(13) C7 0.0412(16) 0.069(2) 0.0584(16) 0.0103(16) 0.0088(13) -0.0014(14) C8 0.0529(17) 0.072(2) 0.0619(19) 0.0009(17) 0.0174(16) 0.0077(17) C9 0.063(2) 0.077(2) 0.0474(16) -0.0043(16) 0.0090(15) 0.0003(18) C10 0.0509(16) 0.0421(16) 0.0418(14) -0.0010(12) 0.0003(12) -0.0057(13) C11 0.0547(17) 0.0529(18) 0.0497(15) 0.0046(14) -0.0082(14) -0.0055(15) C12 0.0478(17) 0.076(2) 0.0707(19) 0.0065(18) -0.0065(16) 0.0009(17) C13 0.0590(19) 0.060(2) 0.0583(18) 0.0009(15) -0.0020(15) -0.0200(17) C14 0.156(4) 0.050(2) 0.105(3) -0.011(2) -0.004(3) -0.005(3) C15 0.081(3) 0.109(3) 0.0508(18) -0.017(2) 0.0149(18) -0.015(2) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 O1 C10 118.4(2) C1 O2 C5 113.72(19) C14 O3 C3 115.3(3) C15 O4 C4 116.6(2) C6 O5 H1 104(3) C10 O6 C13 110.0(2) O1 C1 O2 111.72(19) O1 C1 C7 111.3(2) O2 C1 C7 105.8(2) O1 C1 C2 105.8(2) O2 C1 C2 108.9(2) C7 C1 C2 113.5(2) C1 C2 C3 112.4(2) C1 C2 H2A 109.1 C3 C2 H2A 109.1 C1 C2 H2B 109.1 C3 C2 H2B 109.1 H2A C2 H2B 107.9 O3 C3 C4 106.9(2) O3 C3 C2 111.2(2) C4 C3 C2 111.0(2) O3 C3 H3 109.2 C4 C3 H3 109.2 C2 C3 H3 109.2 O4 C4 C3 110.3(2) O4 C4 C5 105.9(2) C3 C4 C5 111.5(2) O4 C4 H4 109.7 C3 C4 H4 109.7 C5 C4 H4 109.7 O2 C5 C6 107.0(2) O2 C5 C4 110.4(2) C6 C5 C4 114.0(2) O2 C5 H5 108.5 C6 C5 H5 108.5 C4 C5 H5 108.5 O5 C6 C5 114.3(2) O5 C6 H6A 108.7 C5 C6 H6A 108.7 O5 C6 H6B 108.7 C5 C6 H6B 108.7 H6A C6 H6B 107.6 C1 C7 C8 111.8(2) C1 C7 H7A 109.3 C8 C7 H7A 109.3 C1 C7 H7B 109.3 C8 C7 H7B 109.3 H7A C7 H7B 107.9 C9 C8 C7 110.1(3) C9 C8 H8A 109.6 C7 C8 H8A 109.6 C9 C8 H8B 109.6 C7 C8 H8B 109.6 H8A C8 H8B 108.1 C10 C9 C8 112.7(2) C10 C9 H9A 109.1 C8 C9 H9A 109.1 C10 C9 H9B 109.1 C8 C9 H9B 109.1 H9A C9 H9B 107.8 O6 C10 O1 109.6(2) O6 C10 C9 109.4(2) O1 C10 C9 111.1(2) O6 C10 C11 105.4(2) O1 C10 C11 105.5(2) C9 C10 C11 115.5(2) C10 C11 C12 102.3(2) C10 C11 H11A 111.3 C12 C11 H11A 111.3 C10 C11 H11B 111.3 C12 C11 H11B 111.3 H11A C11 H11B 109.2 C13 C12 C11 102.2(3) C13 C12 H12A 111.3 C11 C12 H12A 111.3 C13 C12 H12B 111.3 C11 C12 H12B 111.3 H12A C12 H12B 109.2 O6 C13 C12 106.8(2) O6 C13 H13A 110.4 C12 C13 H13A 110.4 O6 C13 H13B 110.4 C12 C13 H13B 110.4 H13A C13 H13B 108.6 O3 C14 H14A 109.5 O3 C14 H14B 109.5 H14A C14 H14B 109.5 O3 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 O4 C15 H15A 109.5 O4 C15 H15B 109.5 H15A C15 H15B 109.5 O4 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.434(3) O1 C10 1.457(3) O2 C1 1.435(3) O2 C5 1.439(3) O3 C14 1.394(4) O3 C3 1.439(3) O4 C15 1.407(4) O4 C4 1.431(3) O5 C6 1.425(3) O5 H1 0.90(5) O6 C10 1.425(3) O6 C13 1.439(4) C1 C7 1.517(4) C1 C2 1.525(4) C2 C3 1.531(4) C2 H2A 0.9700 C2 H2B 0.9700 C3 C4 1.521(4) C3 H3 0.9800 C4 C5 1.526(3) C4 H4 0.9800 C5 C6 1.513(4) C5 H5 0.9800 C6 H6A 0.9700 C6 H6B 0.9700 C7 C8 1.522(5) C7 H7A 0.9700 C7 H7B 0.9700 C8 C9 1.519(4) C8 H8A 0.9700 C8 H8B 0.9700 C9 C10 1.508(4) C9 H9A 0.9700 C9 H9B 0.9700 C10 C11 1.519(4) C11 C12 1.524(4) C11 H11A 0.9700 C11 H11B 0.9700 C12 C13 1.509(5) C12 H12A 0.9700 C12 H12B 0.9700 C13 H13A 0.9700 C13 H13B 0.9700 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H1 O4 0.90(5) 2.02(5) 2.887(3) 161(4) 2_455 C15 H15A O3 0.96 2.63 3.189(4) 117.5 . C11 H11A O6 0.97 2.34 3.297(4) 168.9 3_645 C5 H5 O6 0.98 2.55 3.117(3) 117.0 . 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 C10 O1 C1 O2 67.7(3) C10 O1 C1 C7 -50.4(3) C10 O1 C1 C2 -174.0(2) C5 O2 C1 O1 55.0(3) C5 O2 C1 C7 176.2(2) C5 O2 C1 C2 -61.4(3) O1 C1 C2 C3 -65.6(3) O2 C1 C2 C3 54.6(3) C7 C1 C2 C3 172.2(2) C14 O3 C3 C4 151.4(3) C14 O3 C3 C2 -87.3(4) C1 C2 C3 O3 -168.5(2) C1 C2 C3 C4 -49.7(3) C15 O4 C4 C3 98.8(3) C15 O4 C4 C5 -140.4(3) O3 C3 C4 O4 -72.7(3) C2 C3 C4 O4 165.9(2) O3 C3 C4 C5 169.9(2) C2 C3 C4 C5 48.5(3) C1 O2 C5 C6 -173.9(2) C1 O2 C5 C4 61.6(3) O4 C4 C5 O2 -173.5(2) C3 C4 C5 O2 -53.6(3) O4 C4 C5 C6 66.1(3) C3 C4 C5 C6 -174.0(2) O2 C5 C6 O5 -66.6(3) C4 C5 C6 O5 55.7(3) O1 C1 C7 C8 51.5(3) O2 C1 C7 C8 -70.1(3) C2 C1 C7 C8 170.6(2) C1 C7 C8 C9 -54.0(3) C7 C8 C9 C10 53.6(4) C13 O6 C10 O1 -96.0(3) C13 O6 C10 C9 142.0(2) C13 O6 C10 C11 17.1(3) C1 O1 C10 O6 -71.6(3) C1 O1 C10 C9 49.4(3) C1 O1 C10 C11 175.33(19) C8 C9 C10 O6 71.5(3) C8 C9 C10 O1 -49.7(4) C8 C9 C10 C11 -169.8(3) O6 C10 C11 C12 -32.9(3) O1 C10 C11 C12 83.1(3) C9 C10 C11 C12 -153.8(3) C10 C11 C12 C13 35.4(3) C10 O6 C13 C12 6.0(3) C11 C12 C13 O6 -26.3(3)