#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:46:16 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225904 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515779.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_4515779 loop_ _publ_author_name 'Lad, Bapurao Sudam' 'Katukojvala, Sreenivas' _publ_section_title ; Piano-Stool Rhodium Enalcarbenoids: Application to Catalyst-Controlled Metal-Templated Annulations of Diazoenals and 1,3-Dicarbonyls ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11807 _journal_paper_doi 10.1021/acscatal.8b03865 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C12 H14 O5' _chemical_formula_sum 'C12 H14 O5' _chemical_formula_weight 238.23 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 82.491(7) _cell_angle_beta 89.314(7) _cell_angle_gamma 82.461(7) _cell_formula_units_Z 2 _cell_length_a 5.8118(8) _cell_length_b 7.6603(10) _cell_length_c 13.506(2) _cell_measurement_reflns_used 7637 _cell_measurement_temperature 140(2) _cell_measurement_theta_max 2.93 _cell_measurement_theta_min 25.05 _cell_volume 590.97(14) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 140(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0224 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16686 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.065 _diffrn_reflns_theta_max 25.065 _diffrn_reflns_theta_min 2.926 _exptl_absorpt_correction_type none _exptl_crystal_colour 'clear whiteish colourless' _exptl_crystal_density_diffrn 1.339 _exptl_crystal_description needle _exptl_crystal_F_000 252 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.215 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.038 _refine_ls_extinction_coef 0.039(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 2086 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0358 _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^)+(0.0402P)^2^+0.2469P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.0908 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1785 _reflns_number_total 2086 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b03865_si_003.cif _cod_data_source_block BL_04-92 _cod_database_code 4515779 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL finalw_a.res in P-1 shelx.res created by SHELXL-2016/6 at 16:31:33 on 22-Apr-2017 CELL 0.71073 5.8118 7.6603 13.5056 82.491 89.314 82.461 ZERR 2.00 0.0008 0.0010 0.0020 0.007 0.007 0.007 LATT 1 SFAC C H O UNIT 24 28 10 MERG 2 OMIT 0 3 0 OMIT 2 2 1 MORE -1 FMAP 2 53 53 PLAN 5 ACTA BOND $H CONF LIST 6 L.S. 11 TEMP -133.15 WGHT 0.040200 0.246900 EXTI 0.038790 FVAR 1.44091 O1 3 0.438431 0.546463 0.306671 11.00000 0.02486 0.02153 = 0.02691 -0.00178 -0.00223 -0.00832 O4 3 0.795673 0.061967 0.582302 11.00000 0.02711 0.02508 = 0.03726 0.00278 -0.00532 -0.01034 O5 3 1.044347 0.265081 0.571858 11.00000 0.02347 0.02449 = 0.03385 -0.00210 -0.00602 -0.00964 O3 3 -0.141086 0.344064 0.156662 11.00000 0.02782 0.02738 = 0.02977 -0.00086 -0.00766 -0.01062 O2 3 -0.132373 0.632525 0.097789 11.00000 0.03356 0.02923 = 0.03882 0.00418 -0.00901 -0.00787 C11 1 0.852650 0.202811 0.544442 11.00000 0.02047 0.02199 = 0.02714 -0.00698 0.00226 -0.00628 C9 1 0.534956 0.279584 0.425594 11.00000 0.02286 0.01984 = 0.02637 -0.00356 0.00261 -0.00487 AFIX 43 H9 2 0.490665 0.168210 0.452788 11.00000 -1.20000 AFIX 0 C4 1 0.391174 0.378670 0.347168 11.00000 0.02428 0.01906 = 0.02497 -0.00209 0.00336 -0.00684 C10 1 0.724730 0.325359 0.465210 11.00000 0.02414 0.01982 = 0.02734 -0.00314 0.00164 -0.00617 AFIX 43 H10 2 0.776179 0.436227 0.442236 11.00000 -1.20000 AFIX 0 C2 1 0.131869 0.485693 0.225895 11.00000 0.02246 0.02278 = 0.02444 -0.00401 0.00148 -0.00548 C1 1 0.278451 0.609559 0.233403 11.00000 0.02451 0.02292 = 0.02348 -0.00284 0.00109 -0.00442 C3 1 0.206017 0.337842 0.299311 11.00000 0.02271 0.02243 = 0.02772 -0.00345 0.00212 -0.00704 AFIX 43 H3 2 0.138113 0.230935 0.312134 11.00000 -1.20000 AFIX 0 C6 1 -0.058494 0.500442 0.153497 11.00000 0.02324 0.02479 = 0.02562 -0.00202 0.00186 -0.00625 C12 1 1.189932 0.152080 0.646622 11.00000 0.02330 0.02980 = 0.03609 -0.00407 -0.00628 -0.00426 AFIX 137 H12A 2 1.201574 0.028697 0.632965 11.00000 -1.50000 H12B 2 1.121992 0.161431 0.712786 11.00000 -1.50000 H12C 2 1.345046 0.189414 0.644861 11.00000 -1.50000 AFIX 0 C5 1 0.299821 0.788409 0.179639 11.00000 0.03299 0.02438 = 0.03090 -0.00073 -0.00032 -0.01009 AFIX 137 H5A 2 0.290565 0.874707 0.227558 11.00000 -1.50000 H5B 2 0.173631 0.822810 0.130650 11.00000 -1.50000 H5C 2 0.449379 0.785821 0.145204 11.00000 -1.50000 AFIX 0 C7 1 -0.325327 0.338766 0.085931 11.00000 0.02642 0.03686 = 0.02796 -0.00466 -0.00590 -0.00981 AFIX 23 H7A 2 -0.270001 0.365614 0.016689 11.00000 -1.20000 H7B 2 -0.459762 0.427691 0.096859 11.00000 -1.20000 AFIX 0 C8 1 -0.394032 0.155198 0.102544 11.00000 0.04552 0.04394 = 0.03959 -0.00579 -0.00882 -0.02217 AFIX 137 H8A 2 -0.524017 0.148582 0.058221 11.00000 -1.50000 H8B 2 -0.441050 0.128025 0.172192 11.00000 -1.50000 H8C 2 -0.261916 0.069051 0.088072 11.00000 -1.50000 AFIX 0 HKLF 4 REM finalw_a.res in P-1 REM R1 = 0.0358 for 1785 Fo > 4sig(Fo) and 0.0455 for all 2086 data REM 158 parameters refined using 0 restraints END WGHT 0.0402 0.2469 REM Highest difference peak 0.215, deepest hole -0.207, 1-sigma level 0.038 Q1 1 0.1821 0.3917 0.2392 11.00000 0.05 0.21 Q2 1 0.4261 0.3519 0.4049 11.00000 0.05 0.21 Q3 1 0.0380 0.4835 0.1968 11.00000 0.05 0.21 Q4 1 0.5030 0.3084 0.3613 11.00000 0.05 0.21 Q5 1 1.2282 0.2202 0.7006 11.00000 0.05 0.19 ; _shelx_res_checksum 45735 _shelx_hkl_file ; -1 0 0 177.38 6.60 -1 0 0 188.28 6.60 -1 0 0 195.68 6.40 -1 0 0 189.28 6.60 1 0 0 192.88 6.60 1 0 0 179.88 6.80 1 0 0 187.08 6.70 1 0 0 200.68 6.40 1 0 0 190.78 6.50 -2 0 0 797.22 25.20 -2 0 0 821.82 25.00 -2 0 0 814.02 25.50 -2 0 0 842.62 25.40 -2 0 0 804.42 24.80 2 0 0 806.42 25.20 2 0 0 788.22 25.30 2 0 0 826.32 24.80 2 0 0 819.12 25.00 2 0 0 802.42 25.80 -3 0 0 925.11 30.60 -3 0 0 961.90 30.00 -3 0 0 996.60 30.80 -3 0 0 949.90 29.80 -3 0 0 968.70 30.50 3 0 0 943.11 29.60 3 0 0 940.41 30.60 3 0 0 939.71 30.10 3 0 0 946.61 31.30 3 0 0 952.80 30.30 -4 0 0 86.99 8.20 -4 0 0 87.59 8.40 -4 0 0 102.19 10.20 -4 0 0 91.99 6.60 -4 0 0 92.39 4.60 -4 0 0 87.29 7.10 -4 0 0 93.39 8.10 4 0 0 85.09 7.00 4 0 0 85.09 10.10 4 0 0 73.09 8.80 4 0 0 84.89 8.60 4 0 0 91.39 9.80 -5 0 0 1.60 5.30 -5 0 0 -1.60 5.60 -5 0 0 -0.70 7.00 -5 0 0 -2.50 3.90 -5 0 0 4.10 2.30 -5 0 0 0.30 5.80 5 0 0 4.50 7.20 5 0 0 2.40 6.50 5 0 0 6.10 7.60 -6 0 0 8.60 3.00 -6 0 0 1.00 6.00 -6 0 0 9.60 8.30 -6 0 0 3.50 8.50 -6 0 0 5.40 8.10 -6 0 0 10.80 10.80 -6 0 0 6.60 6.70 6 0 0 17.70 12.60 6 0 0 8.50 7.70 6 0 0 0.10 10.10 6 0 0 5.40 6.80 6 0 0 -12.90 8.40 6 -1 0 572.84 22.10 6 -1 0 509.05 25.10 6 -1 0 558.64 27.10 6 -1 0 616.14 24.20 6 -1 0 564.94 30.90 -6 1 0 579.74 23.10 -6 1 0 485.25 29.80 -6 1 0 544.45 22.90 -6 1 0 557.74 19.30 -6 1 0 577.04 26.10 -6 1 0 580.94 25.50 -6 1 0 591.44 25.40 5 -1 0 114.79 14.70 5 -1 0 124.39 9.00 5 -1 0 128.69 11.00 5 -1 0 133.29 13.60 5 -1 0 121.29 13.50 -5 1 0 131.79 11.80 -5 1 0 147.79 9.40 -5 1 0 109.69 12.70 -5 1 0 133.79 6.40 -5 1 0 136.29 12.40 -5 1 0 115.99 9.70 4 -1 0 106.29 10.50 4 -1 0 89.59 9.90 4 -1 0 71.89 6.60 4 -1 0 100.49 8.00 -4 1 0 91.69 7.20 -4 1 0 83.09 4.50 -4 1 0 92.49 6.40 -4 1 0 89.39 8.20 -4 1 0 93.79 9.00 -4 1 0 101.29 8.40 3 -1 0 114.49 8.00 3 -1 0 114.29 6.70 3 -1 0 104.99 7.10 -3 1 0 112.19 7.20 -3 1 0 108.69 6.80 -3 1 0 116.79 5.80 -3 1 0 115.89 6.10 -3 1 0 99.19 5.90 -3 1 0 113.39 6.80 -3 1 0 116.19 4.70 2 -1 0 214.48 8.50 2 -1 0 213.88 9.10 2 -1 0 218.28 8.20 -2 1 0 228.18 8.00 -2 1 0 222.68 7.90 -2 1 0 224.78 8.30 -2 1 0 218.88 7.80 -2 1 0 218.48 8.60 -2 1 0 224.98 7.30 1 -1 0 2000.60 57.49 1 -1 0 1929.21 57.69 -1 1 0 2148.29 56.99 -1 1 0 2022.60 57.49 -1 1 0 1947.41 57.59 -1 -1 0 1619.34 46.00 -1 -1 0 1571.44 45.80 -1 -1 0 1589.84 46.20 -1 -1 0 1594.44 46.10 -1 -1 0 1543.75 46.20 1 1 0 1597.14 45.90 1 1 0 1593.64 45.80 1 1 0 1648.44 46.20 1 1 0 1572.54 46.20 1 1 0 1495.35 46.10 -2 -1 0 3031.10 87.49 -2 -1 0 3130.39 87.29 -2 -1 0 3004.10 87.49 -2 -1 0 3051.89 87.69 -2 -1 0 3044.40 86.99 2 1 0 3029.50 87.09 2 1 0 3047.99 86.99 2 1 0 3009.10 87.69 2 1 0 2892.51 87.29 2 1 0 2875.11 87.39 -3 -1 0 162.58 8.80 -3 -1 0 149.59 8.00 -3 -1 0 155.08 8.90 -3 -1 0 156.38 9.90 -3 -1 0 165.18 9.30 3 1 0 167.08 9.60 3 1 0 153.58 9.10 3 1 0 153.38 8.20 3 1 0 156.68 9.50 3 1 0 151.48 8.80 -4 -1 0 120.19 10.60 -4 -1 0 108.99 7.80 -4 -1 0 109.49 9.00 -4 -1 0 110.49 8.80 -4 -1 0 99.69 9.30 4 1 0 90.69 9.10 4 1 0 96.49 8.70 4 1 0 98.49 7.80 4 1 0 105.29 10.00 4 1 0 93.79 10.10 -5 -1 0 103.59 14.20 -5 -1 0 88.19 13.40 -5 -1 0 86.59 13.80 -5 -1 0 85.89 11.40 -5 -1 0 84.09 9.50 5 1 0 92.09 14.60 5 1 0 73.79 14.60 5 1 0 84.89 11.00 5 1 0 87.19 13.20 5 1 0 96.99 9.50 -6 -1 0 199.98 9.20 -6 -1 0 208.18 14.20 -6 -1 0 242.28 18.20 -6 -1 0 205.28 17.00 -6 -1 0 208.68 15.60 -6 -1 0 203.38 17.00 -6 -1 0 249.58 21.30 6 1 0 271.07 22.40 6 1 0 153.08 16.80 6 1 0 212.88 20.60 6 -2 0 272.57 25.40 6 -2 0 286.27 14.00 6 -2 0 309.57 19.50 -6 2 0 283.77 18.40 -6 2 0 277.27 16.00 -6 2 0 275.17 15.90 -6 2 0 271.97 11.20 -6 2 0 253.97 14.60 5 -2 0 119.89 8.40 5 -2 0 146.09 12.60 -5 2 0 119.59 9.80 -5 2 0 116.09 5.90 -5 2 0 88.49 14.70 -5 2 0 120.89 9.60 -5 2 0 98.19 8.80 4 -2 0 26.50 6.50 4 -2 0 20.00 3.60 4 -2 0 19.70 5.00 -4 2 0 22.40 4.00 -4 2 0 17.20 3.40 -4 2 0 20.90 4.50 -4 2 0 22.80 4.00 -4 2 0 18.10 2.40 3 -2 0 315.77 10.50 3 -2 0 294.87 13.40 -3 2 0 287.87 11.90 -3 2 0 308.37 11.50 -3 2 0 315.47 10.10 2 -2 0 54.99 4.90 2 -2 0 56.99 3.70 -2 2 0 55.99 4.00 -2 2 0 49.80 2.60 -2 2 0 47.30 3.80 1 -2 0 17.60 2.00 1 -2 0 16.50 2.40 -1 2 0 17.30 1.40 -1 2 0 15.30 2.40 0 -2 0 1064.09 32.40 0 -2 0 1074.99 32.20 0 -2 0 1119.99 32.10 0 2 0 1145.69 32.10 0 2 0 1251.77 32.30 0 2 0 1113.39 32.30 0 2 0 1058.59 32.30 -1 -2 0 1.60 1.50 -1 -2 0 4.00 2.10 -1 -2 0 4.10 2.00 -1 -2 0 2.50 1.80 -1 -2 0 2.80 2.10 1 2 0 2.00 1.90 1 2 0 3.40 2.10 1 2 0 4.20 2.00 1 2 0 4.90 1.70 1 2 0 0.40 1.70 -2 -2 0 286.97 11.50 -2 -2 0 290.67 11.40 -2 -2 0 293.27 12.10 -2 -2 0 285.77 10.80 -2 -2 0 295.87 11.40 2 2 0 281.77 11.70 2 2 0 275.77 11.60 2 2 0 286.67 11.20 2 2 0 312.37 12.00 2 2 0 293.07 11.00 -3 -2 0 10.10 3.30 -3 -2 0 5.00 4.10 -3 -2 0 11.10 4.70 -3 -2 0 12.10 3.60 -3 -2 0 5.60 3.20 3 2 0 13.60 4.60 3 2 0 9.30 3.00 3 2 0 8.40 4.20 3 2 0 11.70 4.20 3 2 0 7.10 3.90 -4 -2 0 139.99 11.20 -4 -2 0 143.29 9.50 -4 -2 0 155.18 10.30 -4 -2 0 152.88 10.80 -4 -2 0 167.08 12.50 4 2 0 150.38 9.60 4 2 0 169.68 11.30 4 2 0 153.28 12.00 4 2 0 133.69 11.80 4 2 0 131.09 10.20 -5 -2 0 7.60 7.40 -5 -2 0 6.00 8.30 -5 -2 0 -0.70 5.20 5 2 0 -5.50 4.80 5 2 0 9.50 13.70 5 2 0 -11.40 6.40 5 2 0 -10.00 6.80 -6 -2 0 31.80 8.40 -6 -2 0 25.10 12.30 -6 -2 0 21.50 8.30 -6 -2 0 28.00 9.10 -6 -2 0 13.40 10.40 6 2 0 36.90 11.60 6 2 0 14.70 9.50 6 2 0 15.60 8.00 6 2 0 48.20 13.20 6 -3 0 -2.70 14.40 6 -3 0 29.50 10.50 -6 3 0 35.30 8.90 -6 3 0 21.40 3.40 -6 3 0 31.60 8.60 5 -3 0 194.48 27.80 -5 3 0 163.78 7.80 -5 3 0 183.58 12.20 4 -3 0 13.00 6.90 -4 3 0 6.40 4.00 -4 3 0 7.10 3.90 -4 3 0 5.20 1.80 3 -3 0 49.70 7.60 3 -3 0 37.60 4.90 -3 3 0 29.30 4.80 -3 3 0 36.70 5.00 -3 3 0 32.80 2.70 2 -3 0 429.76 15.40 2 -3 0 432.66 15.00 -2 3 0 451.55 14.50 -2 3 0 440.66 13.90 -2 3 0 456.25 15.30 1 -3 0 0.50 0.90 1 -3 0 0.60 1.30 -1 3 0 -0.10 0.80 0 -3 0 240.48 7.70 0 -3 0 232.68 8.20 0 -3 0 224.08 7.60 0 3 0 230.78 7.90 0 3 0 231.08 7.90 0 3 0 188.68 8.10 0 3 0 247.38 7.50 -1 -3 0 291.07 11.50 -1 -3 0 305.87 10.60 -1 -3 0 296.37 11.10 -1 -3 0 290.17 11.00 1 3 0 298.47 11.30 1 3 0 302.37 11.50 1 3 0 299.87 10.80 1 3 0 297.57 11.00 -2 -3 0 806.02 25.90 -2 -3 0 771.62 25.90 -2 -3 0 761.22 25.20 -2 -3 0 802.22 25.60 -2 -3 0 785.82 26.40 2 3 0 784.52 25.60 2 3 0 841.52 26.00 2 3 0 757.12 25.30 2 3 0 775.52 26.00 2 3 0 766.02 26.20 -3 -3 0 23.70 4.70 -3 -3 0 16.50 4.20 -3 -3 0 21.30 4.50 -3 -3 0 17.50 5.20 -3 -3 0 17.70 5.00 3 3 0 24.20 4.10 3 3 0 17.80 5.00 3 3 0 13.50 4.30 3 3 0 19.00 5.10 3 3 0 20.50 5.10 -4 -3 0 50.89 8.20 -4 -3 0 39.50 6.30 -4 -3 0 38.00 7.20 -4 -3 0 49.80 8.20 -4 -3 0 43.80 7.00 4 3 0 43.20 8.30 4 3 0 35.40 6.40 4 3 0 42.00 7.10 4 3 0 54.29 8.00 4 3 0 33.70 5.80 -5 -3 0 104.89 13.40 -5 -3 0 102.19 11.30 -5 -3 0 128.99 16.20 -5 -3 0 110.69 12.30 -5 -3 0 78.39 11.40 5 3 0 106.79 10.90 5 3 0 107.99 15.20 5 3 0 87.89 10.20 5 3 0 100.99 13.60 5 3 0 97.69 14.50 -6 -3 0 127.99 16.30 -6 -3 0 120.59 16.20 -6 -3 0 144.09 15.20 -6 -3 0 155.38 19.20 6 3 0 142.09 21.70 6 3 0 157.78 21.30 6 3 0 139.39 19.20 6 3 0 122.89 15.20 6 3 0 108.69 12.60 5 -4 0 13.20 11.90 -5 4 0 1.90 6.70 -5 4 0 4.70 2.50 -5 4 0 0.20 5.80 4 -4 0 58.99 9.00 -4 4 0 45.80 4.00 -4 4 0 45.80 5.70 3 -4 0 195.08 9.90 3 -4 0 207.08 11.70 -3 4 0 204.48 10.50 -3 4 0 188.68 7.60 2 -4 0 335.97 12.70 2 -4 0 344.17 11.60 2 -4 0 333.37 12.90 -2 4 0 338.17 11.40 1 -4 0 12.70 2.70 1 -4 0 12.50 2.00 -1 4 0 12.50 1.80 0 -4 0 211.58 8.90 0 -4 0 220.88 7.90 0 4 0 228.18 8.10 0 4 0 239.08 7.70 -1 -4 0 396.96 14.60 -1 -4 0 411.96 15.30 -1 -4 0 394.36 14.40 -1 -4 0 398.26 13.80 1 4 0 390.06 14.20 1 4 0 407.56 12.90 1 4 0 392.56 14.20 1 4 0 408.56 15.10 1 4 0 422.86 14.90 -2 -4 0 2078.49 62.39 -2 -4 0 2147.29 62.89 -2 -4 0 2098.19 63.09 -2 -4 0 2031.00 63.09 -2 -4 0 2079.59 63.79 2 4 0 2122.39 62.99 2 4 0 2060.39 63.59 2 4 0 2154.18 62.79 2 4 0 2113.09 63.59 -3 -4 0 47.00 6.50 -3 -4 0 43.60 6.70 -3 -4 0 36.90 5.20 -3 -4 0 43.10 6.20 -3 -4 0 47.20 7.40 3 4 0 38.10 5.70 3 4 0 44.70 6.90 3 4 0 40.10 6.10 3 4 0 46.00 6.70 3 4 0 42.50 6.70 -4 -4 0 144.59 11.00 -4 -4 0 162.38 14.80 -4 -4 0 156.28 12.30 -4 -4 0 163.38 11.70 -4 -4 0 129.89 13.50 4 4 0 150.38 13.20 4 4 0 169.98 13.70 4 4 0 128.29 11.70 4 4 0 133.79 11.10 4 4 0 150.88 13.60 -5 -4 0 116.39 12.70 -5 -4 0 105.49 12.70 -5 -4 0 144.09 18.30 -5 -4 0 131.59 14.00 -5 -4 0 122.79 15.00 5 4 0 110.39 14.10 5 4 0 135.79 16.70 5 4 0 123.89 12.40 5 4 0 127.69 15.80 5 4 0 141.79 17.10 -6 -4 0 3.80 10.90 -6 -4 0 -9.70 9.70 -6 -4 0 4.70 11.70 -6 -4 0 43.20 15.20 -6 -4 0 -0.30 9.10 6 4 0 2.50 11.80 6 4 0 -6.60 11.40 6 4 0 -24.10 13.00 6 4 0 -19.40 8.40 6 4 0 0.20 10.90 5 -5 0 12.20 13.90 -5 5 0 3.50 2.50 4 -5 0 159.78 9.20 4 -5 0 170.58 11.80 4 -5 0 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966.10 39.40 -5 -4 4 912.21 37.40 -5 -4 4 958.70 35.60 4 4 -4 4.70 5.70 4 4 -4 9.00 7.80 4 4 -4 2.90 6.40 4 4 -4 -5.30 7.00 4 4 -4 11.30 6.20 -4 -4 4 3.00 5.00 -4 -4 4 0.40 5.50 -4 -4 4 11.50 8.50 -4 -4 4 0.00 4.60 -4 -4 4 7.90 6.90 3 4 -4 10.00 4.70 3 4 -4 1.70 5.80 3 4 -4 -2.30 4.80 3 4 -4 5.30 5.20 3 4 -4 8.00 4.80 -3 -4 4 8.80 5.80 -3 -4 4 13.10 6.30 -3 -4 4 5.40 3.70 -3 -4 4 7.80 4.90 -3 -4 4 4.00 3.50 2 4 -4 54.29 7.50 2 4 -4 78.29 7.80 2 4 -4 56.09 7.10 2 4 -4 59.19 8.90 2 4 -4 58.79 6.90 -2 -4 4 73.39 8.50 -2 -4 4 57.99 7.00 -2 -4 4 69.39 5.80 -2 -4 4 61.59 5.10 -2 -4 4 55.39 8.70 1 4 -4 46.50 5.60 1 4 -4 53.19 6.00 1 4 -4 48.40 6.80 1 4 -4 51.09 6.00 -1 -4 4 52.89 4.70 -1 -4 4 48.30 5.70 -1 -4 4 58.99 7.20 -1 -4 4 49.40 5.30 0 4 -4 351.56 12.50 0 4 -4 361.86 13.90 0 4 -4 346.47 12.70 0 4 -4 375.16 13.40 0 -4 4 354.36 13.70 0 -4 4 373.16 14.40 0 -4 4 360.86 13.20 0 -4 4 374.06 12.20 0 -4 4 371.26 12.70 -1 4 -4 78.99 5.20 -1 4 -4 81.29 4.30 -1 4 -4 78.59 4.80 -1 4 -4 92.89 6.40 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10.70 3 2 14 47.50 9.00 3 2 14 39.70 12.40 3 2 14 73.89 13.20 3 2 14 55.99 11.60 3 2 14 69.39 9.60 2 -3 -14 9.00 8.50 2 -3 -14 -2.20 5.10 2 -3 -14 -2.60 7.70 2 -3 -14 12.30 7.00 2 -3 -14 0.40 9.10 2 -3 -14 23.60 8.00 -2 3 14 6.70 2.70 -2 3 14 9.40 7.70 -2 3 14 17.20 12.30 -2 3 14 29.70 11.00 -2 3 14 7.20 5.20 1 -3 -14 356.66 18.00 1 -3 -14 354.36 17.80 1 -3 -14 315.57 15.60 1 -3 -14 316.47 14.60 -1 3 14 313.67 20.00 -1 3 14 301.87 10.70 -1 3 14 318.87 18.20 -1 3 14 337.27 15.20 -1 3 14 321.97 15.50 0 -3 -14 36.30 7.10 0 -3 -14 22.60 5.70 0 -3 -14 43.20 9.10 0 -3 -14 23.60 6.20 0 3 14 33.90 8.30 0 3 14 20.30 6.70 0 3 14 30.80 8.40 0 3 14 37.70 6.20 0 3 14 32.10 8.40 -1 -3 -14 -2.90 9.10 -1 -3 -14 -5.10 5.70 -1 -3 -14 6.00 5.80 -1 -3 -14 -2.40 4.60 1 3 14 -5.30 6.40 1 3 14 2.40 6.90 1 3 14 0.40 8.30 1 3 14 3.30 5.30 1 3 14 2.20 7.00 -2 -3 -14 155.38 18.20 -2 -3 -14 214.68 14.40 -2 -3 -14 203.78 14.80 -2 -3 -14 173.58 12.70 2 3 14 196.08 14.60 2 3 14 176.28 16.70 2 3 14 133.39 18.40 2 3 14 181.08 13.40 2 3 14 197.18 13.10 -3 -3 -14 73.09 10.60 -3 -3 -14 76.69 14.70 -3 -3 -14 68.99 9.70 -3 -3 -14 68.39 10.90 -3 -3 -14 74.89 14.60 3 3 14 69.49 9.60 3 3 14 71.99 11.30 3 3 14 83.29 10.30 3 3 14 79.99 14.30 3 3 14 110.59 13.40 2 -4 -14 58.79 8.20 2 -4 -14 55.29 9.70 2 -4 -14 40.60 11.00 2 -4 -14 55.29 7.80 -2 4 14 41.30 10.70 -2 4 14 45.10 7.70 -2 4 14 69.09 5.00 1 -4 -14 5.50 8.00 1 -4 -14 27.00 9.20 1 -4 -14 0.00 5.70 1 -4 -14 -9.40 5.70 -1 4 14 -2.50 9.80 -1 4 14 9.30 17.30 -1 4 14 -4.90 6.00 -1 4 14 2.30 8.50 -1 4 14 2.50 5.70 -1 4 14 -2.60 2.70 0 -4 -14 36.10 7.10 0 -4 -14 32.70 6.10 0 -4 -14 23.80 11.00 0 -4 -14 44.50 8.00 0 4 14 28.60 7.90 0 4 14 35.40 9.80 0 4 14 39.90 9.20 0 4 14 48.50 7.10 0 4 14 57.89 9.90 -1 -4 -14 38.80 8.00 -1 -4 -14 35.20 7.40 -1 -4 -14 35.90 6.40 -1 -4 -14 14.60 10.80 1 4 14 44.20 8.30 1 4 14 39.10 8.20 1 4 14 28.20 7.40 1 4 14 31.00 6.30 1 4 14 11.80 9.50 -2 -4 -14 120.99 19.30 -2 -4 -14 94.89 14.20 -2 -4 -14 123.59 12.20 -2 -4 -14 120.49 13.70 2 4 14 81.79 13.50 2 4 14 97.19 12.40 2 4 14 116.19 12.40 2 4 14 110.79 14.00 2 4 14 87.19 11.40 1 -5 -14 31.00 11.80 1 -5 -14 49.90 8.40 1 -5 -14 48.90 7.60 -1 5 14 51.99 10.90 -1 5 14 49.00 5.50 -1 5 14 46.20 8.20 -1 5 14 58.59 8.10 -1 5 14 35.70 9.90 -1 5 14 35.90 11.70 0 -5 -14 7.10 7.00 0 -5 -14 -0.40 7.80 0 -5 -14 1.10 5.30 0 -5 -14 -4.40 11.10 0 5 14 20.80 9.50 0 5 14 22.50 10.60 0 5 14 17.10 6.40 0 5 14 29.10 9.00 -1 -5 -14 32.80 6.60 -1 -5 -14 23.30 8.60 -1 -5 -14 35.20 8.10 -1 -5 -14 28.90 12.30 1 5 14 30.90 8.10 1 5 14 42.80 9.30 1 5 14 9.20 9.20 1 5 14 28.60 11.80 1 5 14 25.60 7.50 2 5 14 30.50 13.30 1 2 -15 79.79 10.80 1 2 -15 117.49 19.70 -1 -2 15 66.89 10.40 -1 -2 15 76.89 15.40 0 2 -15 83.49 12.80 0 2 -15 66.39 10.00 0 2 -15 100.09 13.10 0 2 -15 63.79 11.10 0 -2 15 66.99 10.90 0 -2 15 50.59 13.20 0 -2 15 41.40 13.00 0 -2 15 63.29 9.00 2 1 -15 76.19 12.50 2 1 -15 64.49 12.50 2 1 -15 38.40 13.20 2 1 -15 59.19 9.10 -2 -1 15 62.59 8.40 -2 -1 15 69.69 17.10 -2 -1 15 43.20 15.70 1 1 -15 7.20 10.50 1 1 -15 -5.40 7.60 1 1 -15 0.20 9.30 1 1 -15 21.10 9.10 1 1 -15 -2.00 6.50 -1 -1 15 3.30 8.40 -1 -1 15 -15.30 11.50 -1 -1 15 18.30 11.50 -1 -1 15 5.40 6.30 0 1 -15 269.77 15.40 0 1 -15 224.38 16.40 0 1 -15 258.07 19.50 0 1 -15 249.48 16.40 0 -1 15 221.98 18.00 0 -1 15 238.58 15.40 -1 1 -15 29.10 7.80 -1 1 -15 5.50 9.80 -1 1 -15 33.00 7.50 -1 1 -15 40.80 10.10 -1 1 -15 26.90 8.40 1 -1 15 46.00 10.30 1 -1 15 2.60 10.30 1 -1 15 24.60 5.30 1 -1 15 20.50 10.40 1 -1 15 21.00 8.30 2 0 -15 28.80 11.50 2 0 -15 26.10 10.10 2 0 -15 12.40 10.70 2 0 -15 22.70 8.30 2 0 -15 30.00 6.80 -2 0 15 19.60 13.40 -2 0 15 36.40 8.00 -2 0 15 14.90 6.20 -2 0 15 11.90 15.10 1 0 -15 57.49 9.30 1 0 -15 44.00 10.30 1 0 -15 59.19 8.70 1 0 -15 74.39 10.60 -1 0 15 47.50 7.30 -1 0 15 54.29 12.30 -1 0 15 45.80 8.80 -1 0 15 40.70 12.70 0 0 -15 362.16 17.20 0 0 -15 371.26 19.20 0 0 -15 327.77 17.90 0 0 -15 382.06 20.10 0 0 15 352.86 14.50 0 0 15 286.87 19.40 0 0 15 351.56 17.60 -1 0 -15 24.80 8.90 -1 0 -15 21.70 7.60 -1 0 -15 34.20 9.70 -1 0 -15 29.00 6.90 1 0 15 28.50 10.50 1 0 15 21.30 10.10 1 0 15 22.80 9.60 1 0 15 32.00 8.00 -2 0 -15 8.10 8.50 -2 0 -15 16.10 11.10 -2 0 -15 1.20 8.90 -2 0 -15 3.80 7.80 2 0 15 -2.90 9.10 2 0 15 -4.30 11.40 2 0 15 5.50 8.90 2 0 15 5.00 6.00 2 0 15 11.00 9.80 2 -1 -15 30.80 11.30 2 -1 -15 41.70 8.90 2 -1 -15 29.10 7.00 2 -1 -15 20.90 10.70 2 -1 -15 35.10 11.00 2 -1 -15 13.30 9.70 -2 1 15 35.70 8.30 -2 1 15 29.40 6.60 -2 1 15 15.50 20.90 -2 1 15 34.10 13.60 -2 1 15 31.60 3.90 1 -1 -15 42.40 9.40 1 -1 -15 34.20 6.60 1 -1 -15 23.30 8.10 1 -1 -15 37.30 8.00 -1 1 15 32.30 8.20 -1 1 15 24.40 11.10 -1 1 15 42.90 7.10 -1 1 15 26.00 3.60 -1 1 15 19.50 11.10 0 -1 -15 3.70 5.70 0 -1 -15 -12.40 7.60 0 -1 -15 2.60 6.80 0 -1 -15 11.40 8.50 0 1 15 9.90 6.70 0 1 15 20.60 9.60 0 1 15 7.50 4.80 0 1 15 0.10 9.00 0 1 15 5.40 7.90 -1 -1 -15 45.40 8.90 -1 -1 -15 54.09 10.20 -1 -1 -15 46.30 7.30 -1 -1 -15 29.50 7.10 -1 -1 -15 30.00 7.50 1 1 15 59.29 10.40 1 1 15 33.90 8.40 1 1 15 48.30 6.70 1 1 15 49.30 10.20 1 1 15 22.40 9.50 -2 -1 -15 54.29 8.10 -2 -1 -15 67.29 9.80 -2 -1 -15 64.59 10.00 -2 -1 -15 66.79 9.00 -2 -1 -15 72.19 14.10 2 1 15 49.50 10.00 2 1 15 73.39 10.70 2 1 15 60.69 12.80 2 1 15 75.89 11.00 2 1 15 52.99 20.90 2 -2 -15 23.00 9.40 2 -2 -15 46.70 9.00 2 -2 -15 38.00 7.20 2 -2 -15 37.20 11.60 2 -2 -15 16.70 9.90 2 -2 -15 25.00 8.60 -2 2 15 28.10 8.90 -2 2 15 29.10 13.60 -2 2 15 32.80 6.70 -2 2 15 32.70 3.80 -2 2 15 42.90 14.50 1 -2 -15 48.60 9.20 1 -2 -15 14.50 8.50 1 -2 -15 6.20 7.50 1 -2 -15 27.40 6.70 -1 2 15 23.40 11.30 -1 2 15 27.20 8.00 -1 2 15 21.00 3.20 -1 2 15 -1.30 10.70 -1 2 15 17.20 6.80 0 -2 -15 136.89 19.10 0 -2 -15 128.29 13.50 0 -2 -15 84.99 9.00 0 -2 -15 84.39 10.80 0 2 15 105.99 12.20 0 2 15 76.29 11.10 0 2 15 97.19 15.30 0 2 15 95.79 9.80 0 2 15 154.68 25.20 -1 -2 -15 129.69 13.30 -1 -2 -15 99.49 11.60 -1 -2 -15 96.49 10.60 -1 -2 -15 122.79 12.50 1 2 15 109.29 13.80 1 2 15 131.69 14.70 1 2 15 97.29 12.20 1 2 15 114.59 10.80 1 2 15 120.39 16.00 -2 -2 -15 10.70 8.30 -2 -2 -15 17.00 8.00 -2 -2 -15 13.60 11.70 -2 -2 -15 17.90 6.60 -2 -2 -15 13.60 8.00 2 2 15 26.30 7.40 2 2 15 31.30 11.90 2 2 15 30.20 9.10 2 2 15 15.80 8.90 2 2 15 16.00 8.30 1 -3 -15 5.00 5.70 1 -3 -15 4.00 6.90 1 -3 -15 20.90 9.00 -1 3 15 -3.50 11.20 -1 3 15 1.00 10.90 -1 3 15 13.20 6.80 -1 3 15 2.60 2.90 -1 3 15 -3.40 8.80 0 -3 -15 0.70 6.20 0 -3 -15 26.10 10.30 0 -3 -15 3.30 6.30 0 -3 -15 2.70 7.10 0 3 15 2.30 9.00 0 3 15 5.50 5.70 0 3 15 2.80 7.20 0 3 15 28.40 10.40 0 3 15 6.60 9.60 -1 -3 -15 68.09 9.00 -1 -3 -15 70.79 13.10 -1 -3 -15 68.99 10.00 -1 -3 -15 68.39 9.50 1 3 15 60.69 11.60 1 3 15 59.59 9.60 1 3 15 79.59 11.00 1 3 15 68.29 10.40 1 3 15 77.39 10.30 -2 -3 -15 10.20 6.90 -2 -3 -15 -10.30 11.60 -2 -3 -15 6.40 8.00 -2 -3 -15 6.30 8.60 2 3 15 3.10 8.10 2 3 15 -19.70 11.00 2 3 15 5.80 8.20 2 3 15 1.80 6.80 2 3 15 -5.10 9.40 0 -4 -15 -0.30 7.40 0 -4 -15 6.60 6.40 0 -4 -15 -5.10 11.90 0 -4 -15 -5.00 8.00 0 4 15 20.00 9.90 0 4 15 13.40 6.50 0 4 15 -7.00 8.20 0 4 15 6.00 10.60 0 4 15 30.50 10.40 -1 -4 -15 17.70 6.40 -1 -4 -15 10.90 8.20 -1 -4 -15 10.80 18.10 -1 -4 -15 31.60 9.20 1 4 15 10.00 6.90 1 4 15 1.70 11.20 1 4 15 28.20 11.10 0 -1 -16 2.70 10.30 0 -1 -16 6.00 8.20 0 -1 -16 15.60 7.20 0 -1 -16 29.40 10.20 0 1 16 13.30 12.30 0 1 16 16.30 6.20 0 1 16 16.60 8.10 0 1 16 24.40 9.80 0 1 16 12.70 11.20 0 -2 -16 -4.00 9.20 0 -2 -16 29.40 11.20 0 -2 -16 2.70 8.00 0 2 16 -0.40 9.10 0 2 16 26.30 11.00 0 2 16 5.90 6.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 17082 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.43843(17) 0.54646(13) 0.30667(7) 0.0241(3) Uani 1 1 d . . O4 O 0.79567(18) 0.06197(14) 0.58230(8) 0.0298(3) Uani 1 1 d . . O5 O 1.04435(18) 0.26508(14) 0.57186(8) 0.0268(3) Uani 1 1 d . . O3 O -0.14109(18) 0.34406(14) 0.15666(8) 0.0279(3) Uani 1 1 d . . O2 O -0.1324(2) 0.63252(15) 0.09779(9) 0.0342(3) Uani 1 1 d . . C11 C 0.8527(2) 0.20281(19) 0.54444(11) 0.0226(3) Uani 1 1 d . . C9 C 0.5350(3) 0.2796(2) 0.42559(11) 0.0228(3) Uani 1 1 d . . H9 H 0.490665 0.168210 0.452788 0.027 Uiso 1 1 calc R U C4 C 0.3912(3) 0.37867(19) 0.34717(11) 0.0225(3) Uani 1 1 d . . C10 C 0.7247(3) 0.3254(2) 0.46521(11) 0.0235(3) Uani 1 1 d . . H10 H 0.776179 0.436227 0.442236 0.028 Uiso 1 1 calc R U C2 C 0.1319(3) 0.4857(2) 0.22590(11) 0.0229(3) Uani 1 1 d . . C1 C 0.2785(3) 0.6096(2) 0.23340(11) 0.0235(3) Uani 1 1 d . . C3 C 0.2060(3) 0.3378(2) 0.29931(11) 0.0239(3) Uani 1 1 d . . H3 H 0.138113 0.230935 0.312134 0.029 Uiso 1 1 calc R U C6 C -0.0585(3) 0.5004(2) 0.15350(11) 0.0244(4) Uani 1 1 d . . C12 C 1.1899(3) 0.1521(2) 0.64662(12) 0.0296(4) Uani 1 1 d . . H12A H 1.201574 0.028697 0.632965 0.044 Uiso 1 1 calc R U H12B H 1.121992 0.161431 0.712786 0.044 Uiso 1 1 calc R U H12C H 1.345046 0.189414 0.644861 0.044 Uiso 1 1 calc R U C5 C 0.2998(3) 0.7884(2) 0.17964(12) 0.0291(4) Uani 1 1 d . . H5A H 0.290565 0.874707 0.227558 0.044 Uiso 1 1 calc R U H5B H 0.173631 0.822810 0.130650 0.044 Uiso 1 1 calc R U H5C H 0.449379 0.785821 0.145204 0.044 Uiso 1 1 calc R U C7 C -0.3253(3) 0.3388(2) 0.08593(12) 0.0298(4) Uani 1 1 d . . H7A H -0.270001 0.365614 0.016689 0.036 Uiso 1 1 calc R U H7B H -0.459762 0.427691 0.096859 0.036 Uiso 1 1 calc R U C8 C -0.3940(3) 0.1552(2) 0.10254(14) 0.0414(5) Uani 1 1 d . . H8A H -0.524017 0.148582 0.058221 0.062 Uiso 1 1 calc R U H8B H -0.441050 0.128025 0.172192 0.062 Uiso 1 1 calc R U H8C H -0.261916 0.069051 0.088072 0.062 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 O1 0.0249(6) 0.0215(6) 0.0269(6) -0.0018(4) -0.0022(4) -0.0083(4) O4 0.0271(6) 0.0251(6) 0.0373(6) 0.0028(5) -0.0053(5) -0.0103(5) O5 0.0235(6) 0.0245(6) 0.0339(6) -0.0021(4) -0.0060(4) -0.0096(5) O3 0.0278(6) 0.0274(6) 0.0298(6) -0.0009(4) -0.0077(4) -0.0106(5) O2 0.0336(7) 0.0292(7) 0.0388(7) 0.0042(5) -0.0090(5) -0.0079(5) C11 0.0205(8) 0.0220(8) 0.0271(8) -0.0070(6) 0.0023(6) -0.0063(6) C9 0.0229(8) 0.0198(8) 0.0264(8) -0.0036(6) 0.0026(6) -0.0049(6) C4 0.0243(8) 0.0191(8) 0.0250(8) -0.0021(6) 0.0034(6) -0.0068(6) C10 0.0241(8) 0.0198(8) 0.0273(8) -0.0031(6) 0.0016(6) -0.0062(6) C2 0.0225(8) 0.0228(8) 0.0244(7) -0.0040(6) 0.0015(6) -0.0055(6) C1 0.0245(8) 0.0229(8) 0.0235(7) -0.0028(6) 0.0011(6) -0.0044(6) C3 0.0227(8) 0.0224(8) 0.0277(8) -0.0035(6) 0.0021(6) -0.0070(6) C6 0.0232(8) 0.0248(8) 0.0256(8) -0.0020(6) 0.0019(6) -0.0063(6) C12 0.0233(8) 0.0298(9) 0.0361(9) -0.0041(7) -0.0063(7) -0.0043(7) C5 0.0330(9) 0.0244(8) 0.0309(8) -0.0007(6) -0.0003(7) -0.0101(7) C7 0.0264(8) 0.0369(9) 0.0280(8) -0.0047(7) -0.0059(6) -0.0098(7) C8 0.0455(11) 0.0439(11) 0.0396(10) -0.0058(8) -0.0088(8) -0.0222(9) 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 C4 107.51(11) C11 O5 C12 116.62(12) C6 O3 C7 115.75(12) O4 C11 O5 122.92(14) O4 C11 C10 125.48(13) O5 C11 C10 111.60(12) C10 C9 C4 127.57(14) C10 C9 H9 116.2 C4 C9 H9 116.2 C3 C4 O1 109.18(13) C3 C4 C9 131.18(14) O1 C4 C9 119.63(13) C9 C10 C11 119.41(14) C9 C10 H10 120.3 C11 C10 H10 120.3 C1 C2 C3 106.68(13) C1 C2 C6 126.29(14) C3 C2 C6 126.99(14) O1 C1 C2 109.51(13) O1 C1 C5 116.10(13) C2 C1 C5 134.38(14) C4 C3 C2 107.12(13) C4 C3 H3 126.4 C2 C3 H3 126.4 O2 C6 O3 123.85(14) O2 C6 C2 126.00(14) O3 C6 C2 110.15(12) O5 C12 H12A 109.5 O5 C12 H12B 109.5 H12A C12 H12B 109.5 O5 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C1 C5 H5A 109.5 C1 C5 H5B 109.5 H5A C5 H5B 109.5 C1 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 O3 C7 C8 107.26(13) O3 C7 H7A 110.3 C8 C7 H7A 110.3 O3 C7 H7B 110.3 C8 C7 H7B 110.3 H7A C7 H7B 108.5 C7 C8 H8A 109.5 C7 C8 H8B 109.5 H8A C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.3625(18) O1 C4 1.3900(17) O4 C11 1.2168(18) O5 C11 1.3421(18) O5 C12 1.4438(19) O3 C6 1.3432(18) O3 C7 1.4515(18) O2 C6 1.2120(18) C11 C10 1.467(2) C9 C10 1.338(2) C9 C4 1.429(2) C9 H9 0.9500 C4 C3 1.353(2) C10 H10 0.9500 C2 C1 1.370(2) C2 C3 1.428(2) C2 C6 1.469(2) C1 C5 1.484(2) C3 H3 0.9500 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C7 C8 1.500(2) C7 H7A 0.9900 C7 H7B 0.9900 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 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 C12 O5 C11 O4 2.8(2) C12 O5 C11 C10 -177.48(12) C1 O1 C4 C3 0.44(16) C1 O1 C4 C9 179.30(13) C10 C9 C4 C3 175.64(16) C10 C9 C4 O1 -2.9(2) C4 C9 C10 C11 -178.67(14) O4 C11 C10 C9 -3.6(2) O5 C11 C10 C9 176.71(13) C4 O1 C1 C2 -0.40(15) C4 O1 C1 C5 -179.53(12) C3 C2 C1 O1 0.22(16) C6 C2 C1 O1 -177.63(13) C3 C2 C1 C5 179.12(16) C6 C2 C1 C5 1.3(3) O1 C4 C3 C2 -0.30(16) C9 C4 C3 C2 -178.99(15) C1 C2 C3 C4 0.06(17) C6 C2 C3 C4 177.88(14) C7 O3 C6 O2 1.7(2) C7 O3 C6 C2 -177.91(12) C1 C2 C6 O2 -9.6(3) C3 C2 C6 O2 172.96(15) C1 C2 C6 O3 169.93(14) C3 C2 C6 O3 -7.5(2) C6 O3 C7 C8 -179.29(13)