#------------------------------------------------------------------------------ #$Date: 2018-02-24 09:34:23 +0200 (Sat, 24 Feb 2018) $ #$Revision: 206648 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242398.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242398 loop_ _publ_author_name 'Ogbeide, K. Osahon' 'Kumar, Rajesh' Mujeeb-Ur-Rehman 'Owolabi, Bodunde' 'Falodun, Abiodun' 'Choudhary, M. Iqbal' 'Yousuf, Sammer' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of the naturally occurring cassane-type diterpenoid, 6\b-cinnamoyl-7\b-hydroxyvouacapen-5\a-ol ; _journal_coeditor_code IS5486 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 385 _journal_page_last 389 _journal_paper_doi 10.1107/S2056989018002499 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C29 H36 O5' _chemical_formula_moiety 'C29 H36 O5' _chemical_formula_sum 'C29 H36 O5' _chemical_formula_weight 464.58 _chemical_name_systematic '(4aR,5R,6R,6aS,7R,11aS,11bR)-4a,6-Dihydroxy-4,4,7,11b-tetramethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-b]furan-5-yl 3-phenylprop-2-enoate' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 94.9300(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.1129(3) _cell_length_b 7.8973(2) _cell_length_c 12.9253(3) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.26 _cell_measurement_theta_min 3.43 _cell_volume 1231.85(5) _computing_cell_refinement ; SAINT (Bruker, 2000) ; _computing_data_collection ; APEX2 (Bruker, 2000) ; _computing_data_reduction ; SAINT (Bruker, 2000) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21754 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.253 _diffrn_reflns_theta_min 3.432 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.253 _exptl_crystal_description Plate _exptl_crystal_F_000 500 _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.188 _refine_diff_density_min -0.207 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 314 _refine_ls_number_reflns 4526 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0347 _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^)+(0.0501P)^2^+0.2131P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.0845 _reflns_number_gt 4183 _reflns_number_total 4526 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file is5486sup1.cif _cod_data_source_block I _cod_database_code 2242398 _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 0.894 _shelx_estimated_absorpt_t_max 0.961 _shelx_hkl_file ; 1 0 0 1137.59 28.70 1 0 0 1093.39 28.40 -1 0 0 1034.50 28.20 -1 0 0 1098.49 28.40 -1 0 0 1059.19 28.60 2 0 0 316.47 9.90 2 0 0 323.07 9.20 -2 0 0 313.77 8.40 3 0 0 158.58 7.10 3 0 0 146.99 5.60 -3 0 0 149.99 4.30 4 0 0 278.07 9.50 -4 0 0 280.47 8.00 -4 0 0 299.27 7.60 4 0 0 273.77 11.10 -4 0 0 274.87 7.90 -5 0 0 45.00 1.80 5 0 0 41.80 3.80 -5 0 0 44.60 2.70 5 0 0 42.00 6.40 -5 0 0 36.10 3.20 6 0 0 63.09 8.50 6 0 0 63.59 5.30 -6 0 0 61.19 2.50 -6 0 0 53.39 3.50 7 0 0 8.80 6.10 7 0 0 5.30 3.40 8 0 0 229.68 17.10 8 0 0 228.38 10.70 8 0 0 264.77 38.60 -8 0 0 246.18 7.90 8 0 0 261.17 17.60 8 0 0 243.58 11.60 9 0 0 25.90 15.70 9 0 0 28.90 4.20 9 0 0 36.50 6.70 9 0 0 26.00 6.40 9 0 0 18.50 5.30 9 0 0 42.50 11.80 9 0 0 18.00 12.20 9 0 0 27.30 9.90 9 0 0 33.90 6.50 -9 0 0 36.60 4.10 10 0 0 73.19 15.70 10 0 0 87.89 16.50 10 0 0 91.29 16.90 10 0 0 86.99 11.00 10 0 0 87.49 10.40 -10 0 0 95.19 6.20 10 0 0 102.89 12.00 11 0 0 -20.60 10.40 11 0 0 -11.70 6.20 11 0 0 4.20 3.40 11 0 0 2.00 4.80 11 0 0 -1.20 19.90 11 0 0 -1.30 8.70 11 0 0 -3.30 4.60 -11 0 0 -4.00 4.40 12 0 0 5.10 8.40 12 0 0 2.60 4.20 12 0 0 1.30 10.00 12 0 0 -5.70 5.50 13 0 0 11.10 8.10 13 0 0 4.70 4.00 13 0 0 12.90 7.90 13 0 0 7.40 5.00 14 0 0 10.50 3.30 14 0 0 17.00 7.30 14 0 0 22.20 6.70 0 -1 0 0.10 0.40 0 -1 0 -0.10 0.20 0 1 0 0.30 0.50 0 1 0 0.30 0.30 1 -1 0 567.94 15.60 -1 -1 0 593.54 15.50 1 -1 0 595.54 15.90 1 -1 0 593.64 15.70 -1 1 0 602.04 15.90 -1 1 0 596.14 15.50 1 1 0 600.34 16.60 1 1 0 612.14 15.80 -2 -1 0 314.57 8.20 -2 -1 0 291.67 8.20 2 -1 0 313.57 9.00 2 -1 0 319.67 8.50 2 -1 0 315.77 8.50 -2 1 0 314.87 8.60 2 1 0 299.67 10.30 -2 1 0 303.97 8.60 3 -1 0 2269.47 58.09 3 -1 0 2249.18 57.29 -3 1 0 2198.28 57.29 3 1 0 2148.98 57.79 3 1 0 2200.98 59.89 -3 1 0 2134.69 57.29 4 -1 0 476.45 13.50 4 -1 0 464.45 14.50 4 -1 0 481.85 15.60 -4 1 0 476.55 13.10 -4 1 0 500.85 12.70 -4 1 0 478.25 13.20 4 1 0 455.15 14.00 4 1 0 461.95 17.00 5 -1 0 226.78 10.90 5 -1 0 235.88 8.90 -5 1 0 246.98 7.40 5 1 0 229.08 8.50 -5 1 0 251.37 6.80 -5 1 0 233.68 7.20 5 1 0 241.88 12.30 -6 -1 0 249.88 7.40 6 -1 0 265.67 12.70 6 -1 0 270.27 10.70 6 1 0 251.67 9.80 6 1 0 260.67 13.80 -6 1 0 267.47 8.30 -6 1 0 253.77 7.50 -6 1 0 252.07 7.90 7 -1 0 151.88 11.90 7 -1 0 150.28 8.90 -7 -1 0 152.88 5.90 -7 1 0 159.68 5.30 7 1 0 149.19 12.20 -7 1 0 149.39 6.00 7 1 0 158.98 8.00 8 -1 0 16.90 8.00 8 -1 0 13.80 5.30 8 -1 0 21.40 7.10 8 -1 0 2.60 3.90 8 -1 0 24.60 15.30 -8 -1 0 12.50 2.20 8 -1 0 1.90 13.70 8 1 0 20.30 6.70 8 1 0 27.80 11.20 8 1 0 7.20 5.30 8 1 0 3.20 8.60 8 1 0 10.30 14.60 -8 1 0 13.80 3.10 8 1 0 12.90 4.60 -8 1 0 13.50 2.20 8 1 0 11.90 7.70 8 1 0 13.00 6.50 9 -1 0 117.89 12.30 9 -1 0 113.89 7.50 9 -1 0 129.19 10.30 9 -1 0 99.99 13.00 -9 -1 0 116.79 5.70 9 -1 0 112.59 16.10 9 -1 0 126.99 18.20 9 -1 0 135.59 11.00 9 -1 0 128.99 18.00 9 1 0 129.79 10.60 9 1 0 132.29 17.10 9 1 0 114.09 14.00 -9 1 0 122.79 5.90 9 1 0 135.59 8.90 9 1 0 126.09 12.50 9 1 0 96.49 15.00 9 1 0 131.89 11.70 9 1 0 116.49 7.90 9 1 0 128.39 13.60 -10 -1 0 202.98 8.50 10 -1 0 251.07 21.60 10 -1 0 164.58 21.00 10 -1 0 221.58 15.70 10 -1 0 219.08 30.20 10 -1 0 234.48 13.30 10 -1 0 210.48 26.50 10 -1 0 219.18 11.80 10 1 0 220.98 20.20 10 1 0 200.88 11.90 10 1 0 174.08 27.20 10 1 0 168.38 24.00 10 1 0 196.48 14.40 -10 1 0 195.98 8.70 -10 1 0 183.48 10.50 10 1 0 231.28 12.70 10 1 0 221.08 10.60 11 -1 0 38.80 11.40 11 -1 0 27.10 4.50 11 -1 0 20.20 24.40 11 -1 0 27.40 8.80 11 -1 0 33.70 6.20 -11 -1 0 47.50 7.60 11 -1 0 42.50 13.00 11 1 0 31.10 5.00 -11 1 0 26.50 5.20 11 1 0 22.90 22.20 11 1 0 26.80 10.50 11 1 0 22.80 9.10 -11 1 0 23.90 5.30 11 1 0 30.50 6.30 11 1 0 33.60 5.70 12 -1 0 26.30 5.20 12 -1 0 23.40 10.40 12 -1 0 29.50 7.20 12 -1 0 29.40 9.40 12 1 0 26.60 5.80 -12 1 0 22.40 5.50 12 1 0 33.10 4.80 12 1 0 28.10 7.70 12 1 0 25.10 4.80 12 1 0 37.60 9.20 13 -1 0 68.69 9.30 13 -1 0 74.69 12.10 13 -1 0 82.09 8.10 13 -1 0 54.99 11.20 13 1 0 88.89 14.50 13 1 0 69.09 6.80 13 1 0 61.29 7.90 13 1 0 94.99 13.40 14 -1 0 31.00 6.80 14 -1 0 33.00 5.00 14 -1 0 36.00 7.90 14 1 0 37.30 6.40 14 1 0 33.90 6.30 -14 1 0 13.80 6.50 0 -2 0 1285.57 33.50 0 -2 0 1221.88 33.40 0 2 0 1307.27 33.60 0 2 0 1289.47 33.80 0 2 0 1294.77 33.30 1 -2 0 347.57 9.80 -1 -2 0 336.97 9.30 1 -2 0 344.27 9.50 1 -2 0 336.27 9.30 -1 2 0 336.57 9.70 1 2 0 330.87 9.10 1 2 0 337.17 9.70 -1 2 0 324.97 9.50 -1 2 0 340.57 9.20 2 -2 0 132.19 4.40 -2 -2 0 131.49 3.90 2 -2 0 125.89 4.10 2 -2 0 129.79 4.80 -2 2 0 125.39 4.40 2 2 0 126.89 4.50 2 2 0 126.59 5.70 -2 2 0 128.39 4.60 -2 2 0 132.99 3.90 3 -2 0 37.60 2.10 3 -2 0 37.20 3.00 -3 -2 0 35.10 1.60 3 -2 0 30.60 2.80 -3 2 0 36.20 2.40 -3 2 0 33.60 2.10 3 2 0 35.20 4.60 -3 2 0 36.70 1.60 -4 -2 0 1400.26 36.60 4 -2 0 1374.26 37.10 4 -2 0 1419.96 38.30 -4 2 0 1464.55 36.70 -4 2 0 1397.06 37.30 4 2 0 1363.66 40.30 -4 2 0 1382.76 37.30 -5 -2 0 778.02 21.30 5 -2 0 781.32 22.30 5 -2 0 797.52 25.00 5 -2 0 811.32 23.90 -5 2 0 802.72 21.30 -5 2 0 801.62 22.00 5 2 0 826.62 26.70 -5 2 0 788.02 22.00 6 -2 0 50.29 7.40 -6 -2 0 50.99 2.80 6 -2 0 62.39 6.40 -6 2 0 53.79 4.00 -6 2 0 54.49 2.70 6 2 0 50.39 8.70 -6 2 0 56.29 3.20 7 -2 0 305.17 15.80 -7 -2 0 320.57 9.50 7 -2 0 325.77 14.00 -7 2 0 330.47 9.60 7 2 0 322.77 17.40 -7 2 0 315.77 10.40 -7 2 0 300.87 10.60 8 -2 0 167.28 23.80 8 -2 0 210.58 23.50 8 -2 0 210.88 12.30 8 -2 0 209.48 23.60 8 -2 0 207.88 15.80 8 -2 0 194.78 14.00 -8 -2 0 203.58 7.00 8 -2 0 213.18 30.10 8 2 0 200.58 13.30 8 2 0 205.28 10.30 8 2 0 205.28 14.50 -8 2 0 194.28 8.10 8 2 0 176.68 16.00 8 2 0 207.48 16.80 8 2 0 200.38 9.90 -8 2 0 210.08 7.20 -8 2 0 189.98 8.20 8 2 0 179.08 13.60 8 2 0 178.58 20.70 8 2 0 181.78 24.10 9 -2 0 262.57 23.40 9 -2 0 291.27 31.10 9 -2 0 249.58 13.90 -9 -2 0 230.98 8.60 9 -2 0 233.88 22.50 9 -2 0 259.77 14.70 9 -2 0 258.97 15.60 9 -2 0 288.67 25.00 9 2 0 257.67 20.10 9 2 0 250.67 13.50 -9 2 0 232.78 9.40 9 2 0 251.37 23.00 9 2 0 257.07 21.50 9 2 0 241.78 14.10 -9 2 0 252.77 10.90 9 2 0 258.87 11.50 9 2 0 250.87 13.10 -9 2 0 247.48 9.00 9 2 0 253.47 14.40 10 -2 0 30.90 13.50 10 -2 0 28.20 10.40 10 -2 0 15.90 10.50 10 -2 0 26.70 5.70 10 -2 0 13.60 6.20 10 -2 0 41.80 17.50 10 -2 0 25.80 12.70 -10 -2 0 15.90 3.70 10 2 0 52.39 16.40 10 2 0 24.10 5.00 10 2 0 -2.40 9.40 -10 2 0 16.60 3.70 10 2 0 16.40 5.80 -10 2 0 13.50 3.80 10 2 0 22.40 8.30 10 2 0 22.40 5.50 11 -2 0 51.09 7.40 11 -2 0 56.69 10.50 -11 -2 0 50.59 5.90 11 -2 0 72.19 9.40 11 -2 0 60.39 11.70 11 -2 0 55.89 14.10 -11 2 0 51.99 7.00 11 2 0 67.79 7.30 11 2 0 59.59 9.80 -11 2 0 59.19 8.30 11 2 0 43.90 9.20 12 -2 0 53.89 10.60 12 -2 0 30.50 11.40 12 -2 0 63.69 10.70 12 -2 0 37.70 5.80 -12 2 0 43.50 6.10 12 2 0 48.20 8.40 12 2 0 46.60 8.50 12 2 0 47.40 5.90 12 2 0 44.50 5.30 13 -2 0 43.10 10.20 13 -2 0 28.20 7.30 13 -2 0 27.50 4.70 13 -2 0 33.40 10.20 -13 2 0 25.70 4.70 13 2 0 25.00 3.90 13 2 0 26.40 6.50 13 2 0 32.30 4.10 13 2 0 16.00 6.60 14 -2 0 25.80 6.30 14 -2 0 16.50 7.60 14 -2 0 12.70 3.30 14 2 0 15.90 5.40 14 2 0 15.70 2.80 14 2 0 19.70 5.80 -14 2 0 2.20 5.20 0 -3 0 0.10 0.80 0 -3 0 2.40 1.10 0 3 0 0.60 1.20 0 3 0 0.50 1.10 0 3 0 1.80 1.40 1 -3 0 363.56 10.90 -1 -3 0 367.46 10.40 1 -3 0 354.26 10.30 1 -3 0 375.16 10.60 -1 -3 0 352.26 10.20 1 3 0 356.76 10.90 -1 3 0 354.26 10.90 -1 3 0 355.16 10.60 1 3 0 363.86 10.50 -1 3 0 364.86 10.00 1 3 0 367.96 10.10 2 -3 0 242.68 7.50 -2 -3 0 261.47 7.50 2 -3 0 240.68 8.20 2 -3 0 239.88 7.70 -2 3 0 247.18 7.70 2 3 0 252.17 8.20 2 3 0 241.48 7.60 -2 3 0 238.48 8.00 -2 3 0 242.98 7.10 3 -3 0 138.79 5.90 3 -3 0 137.39 4.90 -3 -3 0 139.79 4.70 3 -3 0 132.39 5.60 3 3 0 130.29 5.30 -3 3 0 138.39 5.10 -3 3 0 135.39 4.40 -3 3 0 134.69 5.30 4 -3 0 494.95 16.80 4 -3 0 516.75 14.90 -4 -3 0 528.25 14.50 4 3 0 534.55 17.80 -4 3 0 529.05 15.10 -4 3 0 532.35 14.30 -4 3 0 502.45 15.30 5 -3 0 178.08 8.90 5 -3 0 175.18 16.90 5 -3 0 158.68 6.80 -5 3 0 159.08 6.50 -5 3 0 171.08 5.90 -5 3 0 172.08 6.80 5 3 0 173.98 10.10 -5 3 0 161.48 6.20 6 -3 0 178.28 10.50 6 -3 0 130.29 15.70 -6 -3 0 146.59 5.50 6 -3 0 149.39 10.80 -6 3 0 163.48 7.20 6 3 0 156.58 11.80 -6 3 0 161.88 5.40 -6 3 0 152.08 6.30 -6 3 0 143.89 6.20 -7 -3 0 27.40 3.20 7 -3 0 29.50 8.30 7 -3 0 22.40 10.40 7 -3 0 21.40 7.20 7 -3 0 36.70 6.60 -7 3 0 27.30 3.60 7 3 0 14.20 10.30 -7 3 0 30.90 5.90 7 3 0 21.70 6.40 7 3 0 28.20 6.70 -7 3 0 22.20 3.70 7 3 0 27.50 7.00 7 3 0 19.60 10.70 7 3 0 33.50 9.30 7 3 0 21.50 7.70 -7 3 0 26.70 2.70 -8 -3 0 24.60 3.10 8 -3 0 24.30 9.30 8 -3 0 24.60 8.10 8 -3 0 21.90 15.10 8 -3 0 21.10 7.70 8 -3 0 20.60 11.40 8 -3 0 38.40 14.00 8 3 0 26.80 6.70 -8 3 0 28.80 3.20 -8 3 0 29.50 4.90 8 3 0 26.20 10.10 8 3 0 37.10 10.30 -8 3 0 31.30 6.20 8 3 0 25.60 6.40 8 3 0 27.70 8.80 8 3 0 21.20 6.10 8 3 0 22.30 8.90 9 -3 0 63.19 15.30 9 -3 0 70.49 17.80 9 -3 0 64.59 8.20 -9 -3 0 56.99 5.50 9 -3 0 54.19 12.30 9 -3 0 73.29 11.20 9 -3 0 83.99 15.60 -9 3 0 62.09 4.70 -9 3 0 54.69 7.40 -9 3 0 68.29 7.10 9 3 0 60.49 9.90 9 3 0 56.29 10.30 9 3 0 67.09 14.60 9 3 0 65.29 8.80 9 3 0 55.19 8.10 -9 3 0 63.39 4.90 9 3 0 60.09 7.00 10 -3 0 101.39 21.70 10 -3 0 56.29 7.70 -10 -3 0 57.19 7.50 10 -3 0 85.69 13.50 10 -3 0 54.89 15.90 10 -3 0 69.09 13.30 10 -3 0 42.90 12.10 10 3 0 72.49 19.20 -10 3 0 48.40 7.00 10 3 0 60.89 9.40 -10 3 0 60.89 5.30 10 3 0 63.99 8.00 10 3 0 61.49 7.30 -10 3 0 62.89 6.60 -10 3 0 77.89 9.80 10 3 0 68.79 8.90 11 -3 0 176.48 22.90 11 -3 0 223.48 21.70 11 -3 0 170.78 10.90 11 -3 0 164.68 19.40 -11 3 0 147.99 11.00 11 3 0 191.78 13.30 11 3 0 182.98 14.50 11 3 0 180.28 9.10 -11 3 0 158.48 7.60 11 3 0 172.18 9.30 12 -3 0 213.08 26.80 12 -3 0 231.08 17.70 12 -3 0 264.77 22.20 12 -3 0 226.18 12.70 -12 3 0 209.98 8.90 12 3 0 255.57 15.30 12 3 0 242.18 12.70 12 3 0 235.78 9.80 13 -3 0 33.50 4.90 13 -3 0 45.60 10.00 13 -3 0 42.20 9.80 13 3 0 40.40 6.90 13 3 0 36.80 5.00 13 3 0 36.60 5.10 0 -4 0 728.03 21.80 0 -4 0 757.42 21.20 0 -4 0 793.92 21.10 0 -4 0 759.72 23.00 0 4 0 765.02 21.20 0 4 0 768.92 22.00 0 4 0 756.52 20.70 1 -4 0 1307.77 38.00 -1 -4 0 1408.26 37.70 1 -4 0 1456.35 38.00 -1 -4 0 1443.36 37.60 -1 -4 0 1422.46 39.30 1 -4 0 1310.97 38.10 -1 4 0 1419.86 37.30 1 4 0 1426.06 37.70 -1 4 0 1406.06 38.50 1 4 0 1465.95 38.70 -1 4 0 1390.56 37.80 2 -4 0 1539.95 43.90 -2 -4 0 1650.23 43.20 -2 -4 0 1633.04 45.00 2 -4 0 1694.63 46.30 -2 -4 0 1639.14 43.30 2 -4 0 1566.54 43.40 -2 4 0 1626.24 43.50 2 4 0 1673.63 44.20 2 4 0 1519.35 43.00 -2 4 0 1601.94 43.20 -2 4 0 1676.63 44.20 -2 4 0 1604.24 42.70 3 -4 0 595.04 21.20 3 -4 0 602.24 18.80 -3 -4 0 618.84 17.50 3 -4 0 627.84 17.60 -3 -4 0 634.34 17.60 -3 -4 0 620.84 20.00 3 4 0 635.84 18.30 -3 4 0 606.84 17.00 -3 4 0 617.14 18.50 -3 4 0 577.44 17.50 -3 4 0 604.34 17.80 -4 -4 0 96.29 4.60 -4 -4 0 78.79 9.60 4 -4 0 90.39 7.70 4 -4 0 97.99 5.50 4 -4 0 102.19 12.00 -4 4 0 89.49 3.80 -4 4 0 89.69 4.70 -4 4 0 81.49 5.60 -4 4 0 85.19 4.80 5 -4 0 271.17 15.70 -5 -4 0 272.57 13.20 -5 -4 0 280.77 9.30 5 -4 0 263.77 12.60 -5 4 0 262.97 8.50 -5 4 0 274.57 9.30 -5 4 0 281.97 10.60 -5 4 0 274.67 9.60 6 -4 0 25.20 8.70 6 -4 0 20.70 7.10 6 -4 0 37.00 7.40 -6 -4 0 30.00 3.90 -6 -4 0 18.20 7.00 6 4 0 33.60 5.90 -6 4 0 35.30 5.20 -6 4 0 34.80 2.90 -6 4 0 35.90 4.40 6 4 0 15.30 11.00 -6 4 0 30.60 4.10 6 4 0 35.10 7.10 7 -4 0 153.88 17.10 -7 -4 0 138.39 6.90 7 -4 0 155.58 15.10 7 -4 0 117.49 17.50 -7 -4 0 139.99 13.10 7 -4 0 151.88 13.60 7 4 0 124.79 9.70 7 4 0 148.39 16.80 -7 4 0 155.08 5.90 -7 4 0 162.48 12.60 -7 4 0 142.09 6.20 7 4 0 128.19 17.10 -7 4 0 145.59 7.30 7 4 0 135.49 12.10 -7 4 0 146.29 8.30 8 -4 0 -6.40 11.00 8 -4 0 -6.70 23.00 8 -4 0 17.90 10.80 8 -4 0 -4.60 16.20 8 -4 0 -4.00 13.60 -8 -4 0 5.80 8.10 8 -4 0 -3.10 10.50 -8 -4 0 -3.70 3.40 8 4 0 -1.20 10.10 -8 4 0 1.80 2.10 -8 4 0 2.40 2.30 8 4 0 4.10 4.80 -8 4 0 7.50 3.50 8 4 0 0.90 4.90 9 -4 0 11.30 15.30 9 -4 0 11.20 20.00 -9 -4 0 11.50 10.10 9 -4 0 9.40 10.10 9 -4 0 -15.60 13.40 -9 -4 0 2.20 4.90 9 -4 0 -7.80 13.90 -9 -4 0 -1.00 6.30 9 -4 0 13.60 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389.56 13.20 -5 5 0 381.86 12.70 -5 5 0 388.46 13.30 -5 5 0 365.46 14.80 5 5 0 359.36 18.10 5 5 0 410.96 22.20 -6 -5 0 78.39 11.30 -6 -5 0 61.59 6.00 6 -5 0 60.99 9.50 -6 -5 0 63.59 7.40 6 -5 0 72.89 12.80 6 -5 0 77.79 13.70 6 5 0 49.70 7.20 -6 5 0 78.09 8.50 -6 5 0 66.39 6.00 -6 5 0 63.59 4.40 -6 5 0 54.59 4.40 -6 5 0 51.79 5.60 6 5 0 76.29 11.50 6 5 0 68.39 10.70 7 -5 0 189.28 27.70 -7 -5 0 218.78 14.60 7 -5 0 239.08 23.60 -7 -5 0 208.18 9.90 -7 -5 0 198.58 11.90 7 -5 0 210.48 16.00 -7 5 0 221.18 10.10 7 5 0 235.18 16.40 7 5 0 201.18 12.10 -7 5 0 217.98 8.20 -7 5 0 208.18 10.30 -7 5 0 224.48 8.90 -8 -5 0 104.59 9.10 8 -5 0 85.29 13.00 8 -5 0 105.89 12.70 8 -5 0 132.49 27.20 -8 -5 0 96.49 12.20 8 -5 0 127.89 18.60 -8 -5 0 103.99 14.10 -8 5 0 108.19 8.10 -8 5 0 98.79 7.00 8 5 0 107.79 8.40 -8 5 0 106.09 5.50 8 5 0 128.89 13.80 -8 5 0 108.59 6.40 9 -5 0 112.69 11.00 -9 -5 0 93.19 10.50 9 -5 0 102.89 17.80 -9 -5 0 77.29 10.50 9 -5 0 100.99 13.30 9 5 0 100.49 11.00 -9 5 0 100.49 5.00 -9 5 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140.69 17.30 -6 6 0 114.89 6.10 6 6 0 129.29 14.20 -6 6 0 117.69 8.30 6 6 0 112.99 10.60 6 6 0 141.09 7.10 -6 6 0 110.49 9.10 7 -6 0 169.38 19.80 -7 -6 0 137.69 11.50 7 -6 0 150.28 13.30 -7 6 0 135.59 9.90 -7 6 0 151.88 9.40 -7 6 0 152.48 7.00 7 6 0 163.88 13.60 7 6 0 135.89 10.30 8 -6 0 88.39 12.50 8 -6 0 85.69 11.70 8 -6 0 111.39 18.30 -8 -6 0 127.89 12.80 -8 6 0 125.39 6.30 8 6 0 110.89 8.80 8 6 0 109.29 11.20 -8 6 0 114.99 9.40 -8 6 0 116.19 5.50 9 -6 0 68.19 16.30 -9 -6 0 48.00 8.60 9 -6 0 60.09 8.10 -9 6 0 56.49 7.70 -9 6 0 56.49 4.20 9 6 0 45.40 6.90 9 6 0 53.49 6.50 -9 6 0 53.09 4.90 10 -6 0 -0.30 5.80 10 -6 0 -3.80 13.10 -10 -6 0 16.40 10.50 10 -6 0 13.60 9.80 10 6 0 9.70 5.00 -10 6 0 8.30 2.10 10 6 0 8.20 3.30 -10 6 0 9.20 2.70 11 -6 0 126.49 16.00 11 -6 0 132.09 14.90 11 -6 0 109.19 9.90 -11 6 0 132.09 5.80 -11 6 0 135.29 6.00 11 6 0 131.39 6.30 0 -7 0 -2.10 3.50 0 -7 0 -0.20 5.50 0 -7 0 2.70 8.70 0 -7 0 3.10 5.30 0 7 0 6.90 9.60 0 7 0 -6.30 3.90 0 7 0 -2.80 2.90 1 -7 0 20.00 6.20 1 -7 0 19.60 10.80 -1 -7 0 21.50 8.90 -1 -7 0 11.50 4.20 -1 -7 0 1.00 7.10 -1 -7 0 14.40 5.60 1 -7 0 21.70 6.20 1 -7 0 19.30 4.10 1 7 0 15.40 3.40 -1 7 0 24.30 3.70 -1 7 0 17.30 9.40 -1 7 0 19.10 3.50 2 -7 0 49.80 7.50 -2 -7 0 71.99 11.30 -2 -7 0 69.99 9.30 -2 -7 0 72.39 10.30 2 -7 0 64.19 6.70 -2 -7 0 61.39 7.80 -2 7 0 60.09 7.10 -2 7 0 65.19 6.20 -2 7 0 67.69 5.50 -2 7 0 74.89 11.10 2 7 0 73.09 5.90 -3 -7 0 9.90 7.40 -3 -7 0 12.10 6.30 3 -7 0 5.70 3.70 -3 -7 0 9.00 9.10 -3 -7 0 0.80 4.70 3 -7 0 2.70 7.00 -3 7 0 3.50 3.30 -3 7 0 0.50 10.20 3 7 0 10.80 8.30 3 7 0 2.60 3.00 -3 7 0 -0.30 5.10 -3 7 0 6.50 2.80 -4 -7 0 499.05 18.00 -4 -7 0 485.75 19.40 4 -7 0 468.85 24.20 -4 -7 0 502.95 20.50 -4 7 0 511.75 18.10 4 7 0 504.95 23.30 -4 7 0 495.65 15.70 4 7 0 524.45 15.60 -4 7 0 489.95 16.50 -5 -7 0 -16.00 7.80 -5 -7 0 1.00 6.20 5 -7 0 -14.80 7.30 5 -7 0 -2.80 8.50 -5 -7 0 5.50 5.20 -5 7 0 2.20 4.10 -5 7 0 -3.10 5.10 -5 7 0 1.60 2.40 5 7 0 0.20 7.70 -5 7 0 -1.00 3.50 5 7 0 7.40 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209.28 16.60 -3 -6 9 201.18 10.80 -3 -6 9 212.08 17.50 3 6 -9 189.58 7.40 -3 6 9 201.08 8.10 3 6 -9 201.88 15.30 -3 6 9 190.28 9.10 2 -6 -9 59.99 10.40 -2 -6 9 75.49 14.20 -2 -6 9 62.29 9.50 -2 -6 9 48.50 7.60 2 6 -9 50.29 4.80 -2 6 9 58.59 5.10 -2 6 9 58.39 8.40 2 6 -9 46.00 9.10 -1 -6 9 31.80 12.40 -1 -6 9 6.20 4.60 -1 -6 9 15.50 6.10 -1 6 9 6.40 3.00 1 6 -9 3.60 8.80 1 6 -9 10.70 2.90 0 -6 -9 69.69 11.90 0 -6 -9 32.90 4.30 0 -6 9 41.80 5.90 0 -6 9 40.30 6.70 0 -6 9 45.50 11.70 0 6 -9 31.90 4.60 0 6 -9 53.59 10.20 0 6 9 38.10 5.00 0 6 9 29.40 4.60 -1 -6 -9 2.40 6.20 1 -6 9 -9.60 10.40 -1 -6 -9 1.60 3.60 1 -6 9 1.70 5.80 1 -6 9 8.00 5.30 -1 6 -9 5.70 2.70 1 6 9 1.00 3.70 1 6 9 1.40 3.00 -1 6 -9 9.30 9.10 -2 -6 -9 28.70 6.90 2 -6 9 37.30 11.30 2 -6 9 33.20 6.70 2 -6 9 14.80 7.40 -2 6 -9 32.30 4.60 -2 6 -9 45.10 11.10 2 6 9 45.80 12.70 2 6 9 34.10 5.10 -3 -6 -9 18.40 7.20 3 -6 9 7.20 6.10 -3 -6 -9 15.10 4.20 3 6 9 -1.80 10.30 -3 6 -9 14.30 2.90 3 6 9 16.00 3.50 -3 6 -9 21.90 10.70 4 -6 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-4 -4 -13 108.39 13.50 4 -4 13 85.59 5.20 -4 4 -13 83.59 4.40 4 4 13 92.49 5.40 4 4 13 71.89 9.10 -3 -5 13 31.60 5.00 -3 -5 13 55.59 9.10 3 -5 -13 31.50 6.20 -3 5 13 37.70 3.40 -2 -5 13 40.10 6.00 -2 -5 13 40.20 5.70 2 -5 -13 40.30 6.30 -2 5 13 40.80 3.50 -1 -5 13 32.00 4.00 1 -5 -13 34.40 6.50 -1 -5 13 39.10 6.90 1 5 -13 40.00 3.50 -1 5 13 38.80 3.60 0 -5 -13 9.50 5.20 0 -5 13 13.30 3.20 0 5 13 7.70 4.80 0 5 -13 7.90 1.90 0 5 13 3.30 2.10 -1 -5 -13 0.20 5.10 1 -5 13 0.90 2.60 1 5 13 2.30 7.80 1 5 13 6.90 3.60 1 5 13 -3.00 2.60 -1 5 -13 -0.90 1.70 7 0 -14 37.80 7.40 -7 0 14 20.10 5.60 7 0 -14 11.00 4.60 -6 0 14 49.10 9.80 6 0 -14 33.40 8.60 6 0 -14 41.90 6.00 -5 0 14 38.40 7.40 -5 0 14 31.00 4.90 5 0 -14 29.60 9.00 -4 0 14 6.10 4.70 4 0 -14 0.20 8.60 -4 0 14 5.30 6.10 4 0 -14 7.30 5.90 -4 0 14 -4.30 3.80 3 0 -14 42.00 12.00 -3 0 14 30.10 5.30 3 0 -14 43.90 6.70 3 0 -14 45.10 3.70 -3 0 14 45.70 6.00 -3 0 14 38.20 6.80 -2 0 14 31.10 6.10 -2 0 14 30.20 4.40 2 0 -14 34.60 3.50 2 0 -14 26.30 6.80 -2 0 14 28.20 5.60 -1 0 14 29.00 5.90 -1 0 14 27.10 6.10 1 0 -14 34.10 3.70 1 0 -14 42.60 7.20 -1 0 14 40.60 5.40 0 0 14 171.48 8.10 0 0 14 173.58 11.50 0 0 -14 169.78 6.80 0 0 14 172.38 11.30 0 0 -14 171.38 11.90 -1 0 -14 7.60 6.10 1 0 14 5.30 3.20 1 0 14 3.30 5.80 -2 0 -14 25.10 4.00 2 0 14 17.40 3.30 2 0 14 25.10 7.20 3 0 14 156.68 15.00 -3 0 -14 186.28 7.20 3 0 14 186.38 7.50 4 0 14 45.50 4.40 -4 0 -14 46.80 5.10 5 0 14 -6.90 12.50 -7 -1 14 12.20 5.50 7 -1 -14 8.20 6.20 7 -1 -14 10.40 4.70 -7 1 14 9.50 4.80 7 1 -14 11.50 4.30 6 -1 -14 47.40 6.00 -6 -1 14 59.19 7.90 6 -1 -14 50.39 8.20 -6 -1 14 63.39 9.00 -6 1 14 56.59 7.20 -6 1 14 81.49 13.20 -6 1 14 38.40 6.30 6 1 -14 43.00 6.10 -5 -1 14 32.70 5.20 5 -1 -14 31.50 6.50 -5 -1 14 37.50 7.30 5 -1 -14 24.40 5.60 -5 -1 14 27.40 5.00 -5 1 14 33.10 10.70 -5 1 14 20.60 3.80 -5 1 14 27.10 5.00 5 1 -14 31.30 5.90 4 -1 -14 88.39 12.60 -4 -1 14 79.59 10.10 4 -1 -14 70.79 10.20 -4 -1 14 94.29 7.30 -4 -1 14 67.39 8.10 -4 1 14 104.49 11.20 4 1 -14 80.29 9.80 -4 1 14 76.39 6.10 -4 1 14 69.79 7.70 -3 -1 14 25.60 6.00 -3 -1 14 17.60 5.00 -3 -1 14 19.20 4.10 3 -1 -14 22.50 3.30 3 -1 -14 15.50 6.30 3 -1 -14 31.60 8.20 -3 1 14 22.70 6.50 3 1 -14 19.40 6.00 -3 1 14 13.20 5.00 -3 1 14 13.40 3.50 3 1 -14 15.30 2.20 -2 -1 14 12.60 3.80 -2 -1 14 9.80 5.80 2 -1 -14 13.10 9.00 -2 -1 14 4.10 4.70 2 -1 -14 5.50 2.10 2 -1 -14 14.90 6.60 -2 1 14 7.20 5.80 -2 1 14 6.80 3.40 2 1 -14 9.40 2.10 -2 1 14 10.50 5.20 2 1 -14 6.50 6.20 1 -1 -14 117.59 10.80 -1 -1 14 114.69 9.80 -1 -1 14 85.79 8.70 1 -1 -14 100.29 14.50 -1 -1 14 91.59 6.60 1 -1 -14 105.69 5.00 -1 1 14 106.79 6.50 1 1 -14 131.19 10.90 -1 1 14 98.29 10.30 1 1 -14 104.29 4.90 -1 1 14 90.09 9.80 0 -1 -14 29.70 7.00 0 -1 -14 33.90 3.80 0 -1 -14 55.09 10.20 0 -1 14 46.90 6.60 0 -1 14 27.40 6.00 0 -1 14 40.10 5.50 0 1 -14 24.60 6.90 0 1 14 31.70 7.90 0 1 14 31.30 4.90 0 1 -14 33.70 3.90 1 -1 14 51.19 7.10 -1 -1 -14 59.79 9.80 -1 -1 -14 73.89 11.40 -1 -1 -14 56.69 4.40 1 -1 14 65.99 5.70 -1 1 -14 59.19 4.40 1 1 14 51.49 7.40 -1 1 -14 74.89 10.00 1 1 14 56.69 5.10 -2 -1 -14 11.10 10.40 2 -1 14 18.60 7.30 -2 -1 -14 9.20 6.40 -2 -1 -14 8.80 2.70 2 -1 14 6.80 3.20 2 1 14 12.40 6.80 -2 1 -14 10.60 6.50 -2 1 -14 12.70 2.60 2 1 14 13.00 3.00 3 -1 14 34.90 11.10 3 -1 14 30.60 4.70 -3 -1 -14 33.00 4.70 3 1 14 23.90 3.30 -3 1 -14 26.60 4.00 3 1 14 37.10 8.10 -4 -1 -14 78.79 5.70 4 -1 14 77.29 4.90 4 1 14 83.29 4.90 -4 1 -14 69.19 5.00 4 1 14 65.99 11.30 5 -1 14 19.80 7.20 -5 -1 -14 31.80 4.70 -5 -1 -14 26.90 3.70 5 1 14 52.89 12.70 -5 1 -14 31.10 4.50 -6 -2 14 12.40 5.30 6 -2 -14 16.30 4.50 -6 -2 14 11.00 7.90 6 -2 -14 8.30 5.80 -6 2 14 11.30 3.50 6 2 -14 16.90 5.10 -6 2 14 12.10 4.30 -5 -2 14 39.70 6.80 5 -2 -14 37.90 6.90 5 -2 -14 24.80 5.90 -5 2 14 44.60 11.50 -5 2 14 32.00 4.60 5 2 -14 24.20 5.60 -5 2 14 23.90 7.50 4 -2 -14 18.00 6.10 -4 -2 14 23.70 5.50 4 -2 -14 18.80 6.70 -4 -2 14 21.00 4.60 -4 -2 14 17.80 4.70 -4 2 14 17.80 4.60 -4 2 14 18.10 3.20 4 2 -14 16.00 5.70 3 -2 -14 34.80 7.20 -3 -2 14 44.50 7.20 -3 -2 14 43.40 6.30 3 -2 -14 36.10 7.50 -3 -2 14 43.30 6.00 3 2 -14 36.20 6.90 -3 2 14 57.69 8.20 -3 2 14 49.40 4.60 -3 2 14 46.40 7.70 2 -2 -14 50.99 8.20 2 -2 -14 64.39 4.00 -2 -2 14 51.29 7.40 -2 -2 14 56.49 8.20 2 -2 -14 65.69 8.00 -2 -2 14 62.39 6.30 -2 2 14 55.89 4.70 2 2 -14 51.89 7.00 -2 2 14 64.89 8.60 -2 2 14 67.29 10.50 2 2 -14 54.19 3.70 1 -2 -14 182.38 6.70 1 -2 -14 180.38 14.00 -1 -2 14 170.88 10.30 -1 -2 14 158.98 10.60 -1 -2 14 189.48 8.30 1 -2 -14 169.58 12.70 1 2 -14 175.18 11.80 -1 2 14 190.18 12.50 -1 2 14 192.08 7.60 -1 2 14 190.88 17.50 1 2 -14 184.28 6.60 0 -2 14 16.70 3.70 0 -2 14 19.10 6.00 0 -2 14 11.60 5.80 0 -2 -14 12.10 7.10 0 -2 -14 17.10 2.60 0 -2 -14 18.30 7.40 0 2 14 20.80 6.60 0 2 14 19.80 3.10 0 2 -14 20.70 6.50 0 2 -14 19.70 2.50 -1 -2 -14 68.99 4.50 -1 -2 -14 74.69 11.60 1 -2 14 55.99 5.60 -1 -2 -14 72.69 10.70 1 -2 14 70.39 10.20 1 2 14 51.09 7.30 -1 2 -14 61.29 4.00 1 2 14 61.49 4.60 -1 2 -14 64.39 9.60 -2 -2 -14 19.10 2.90 2 -2 14 27.40 8.50 -2 -2 -14 26.20 7.60 -2 2 -14 19.70 6.50 2 2 14 13.20 6.30 2 2 14 19.80 3.10 -2 2 -14 18.90 2.50 -3 -2 -14 18.80 7.50 -3 -2 -14 0.50 2.70 -3 -2 -14 17.50 7.00 -3 2 -14 4.20 5.50 3 2 14 8.40 6.90 -3 2 -14 2.00 2.00 3 2 14 -2.10 2.60 -4 -2 -14 0.90 3.00 -4 -2 -14 5.30 6.60 -4 -2 -14 13.60 8.60 4 -2 14 0.30 2.80 4 2 14 17.20 9.60 -4 2 -14 -3.30 5.00 4 2 14 -0.60 3.80 -4 2 -14 2.60 2.30 5 -3 -14 8.20 4.50 -5 -3 14 15.70 6.00 -5 -3 14 15.60 5.20 -5 3 14 9.90 2.70 5 3 -14 4.60 8.20 -5 3 14 13.30 4.60 4 -3 -14 32.90 10.50 -4 -3 14 34.60 5.20 4 -3 -14 33.20 5.50 -4 -3 14 37.50 5.30 4 3 -14 36.60 6.50 -4 3 14 65.19 11.20 -4 3 14 52.99 7.90 -4 3 14 35.80 4.00 -3 -3 14 18.80 4.30 3 -3 -14 12.10 5.60 3 -3 -14 32.20 14.90 -3 3 14 16.60 2.80 -3 3 14 29.70 8.70 3 3 -14 10.80 5.90 -3 3 14 20.00 5.40 -2 -3 14 31.50 4.40 -2 -3 14 39.20 5.80 -2 -3 14 40.10 6.00 2 -3 -14 18.90 9.00 2 -3 -14 32.00 6.20 2 3 -14 32.80 3.40 2 3 -14 32.30 6.90 -2 3 14 37.50 4.10 -2 3 14 35.10 7.40 -1 -3 14 85.89 13.30 1 -3 -14 75.19 10.00 -1 -3 14 79.99 11.50 -1 -3 14 70.69 6.10 1 -3 -14 54.59 7.40 -1 3 14 75.79 10.70 -1 3 14 76.79 4.90 1 3 -14 74.39 9.80 1 3 -14 76.89 4.00 0 -3 14 226.78 8.80 0 -3 -14 205.98 12.50 0 -3 14 223.18 12.60 0 -3 -14 246.48 14.30 0 -3 14 213.78 13.10 0 -3 -14 224.48 7.80 0 3 14 235.58 8.30 0 3 -14 243.68 12.40 0 3 -14 227.78 7.40 0 3 14 220.78 12.70 -1 -3 -14 155.88 6.10 1 -3 14 132.89 13.10 1 -3 14 146.59 7.00 -1 -3 -14 138.99 19.70 -1 -3 -14 158.28 10.80 -1 3 -14 168.68 11.30 1 3 14 153.28 6.30 1 3 14 139.29 10.00 -1 3 -14 152.58 5.60 1 3 14 155.78 14.80 -2 -3 -14 20.00 10.40 2 -3 14 5.00 2.70 -2 -3 -14 9.30 2.50 -2 -3 -14 -1.40 5.40 -2 3 -14 12.40 6.80 2 3 14 5.00 2.40 -2 3 -14 8.10 1.90 2 3 14 -1.30 5.90 -3 -3 -14 19.80 5.90 -3 -3 -14 13.50 2.90 3 -3 14 18.00 2.70 -3 -3 -14 -2.10 13.20 3 3 14 13.00 4.00 -3 3 -14 34.10 7.40 -3 3 -14 20.80 3.00 3 3 14 14.50 3.10 3 3 14 14.00 7.10 2 -4 -14 42.10 6.00 -2 -4 14 78.39 9.60 -2 -4 14 54.39 5.70 -2 -4 14 63.59 8.90 -2 4 14 54.59 8.70 -2 4 14 53.29 3.80 -1 -4 14 12.20 6.70 -1 -4 14 1.80 3.10 -1 -4 14 4.00 7.00 1 -4 -14 2.90 4.80 -1 4 14 4.00 6.50 -1 4 14 -3.10 2.00 0 -4 14 36.30 4.40 0 -4 -14 13.70 5.20 0 4 14 28.70 3.30 0 4 -14 25.50 3.00 0 4 14 35.60 6.90 -5 0 15 22.50 9.70 -5 0 15 16.30 5.40 5 0 -15 19.40 4.70 -5 0 15 5.80 4.30 4 0 -15 10.30 4.80 -4 0 15 6.90 5.10 -4 0 15 10.10 3.40 -4 0 15 21.90 7.50 -3 0 15 15.10 6.40 -3 0 15 11.80 3.10 -3 0 15 12.40 5.30 3 0 -15 17.90 5.40 -2 0 15 32.90 6.20 2 0 -15 27.50 5.70 2 0 -15 20.00 2.90 -2 0 15 30.30 4.60 -2 0 15 40.00 7.40 -1 0 15 27.90 7.80 -1 0 15 20.70 3.30 1 0 -15 25.60 2.90 -1 0 15 24.00 9.10 1 0 -15 28.40 5.80 0 0 15 50.59 7.30 0 0 -15 49.40 6.60 0 0 15 45.10 4.60 0 0 -15 45.30 3.40 -1 0 -15 117.79 4.90 -1 0 -15 122.39 9.00 1 0 15 118.99 5.80 1 0 15 138.69 11.30 -2 0 -15 1.10 1.80 -2 0 -15 4.30 5.00 2 0 15 -1.90 8.60 2 0 15 1.70 2.30 4 -1 -15 16.60 6.50 -4 -1 15 11.10 6.60 -4 -1 15 4.80 5.10 -4 -1 15 8.80 3.60 4 -1 -15 9.90 4.90 -4 1 15 14.40 8.70 -4 1 15 12.30 2.90 4 1 -15 11.40 4.50 -4 1 15 10.30 5.30 -3 -1 15 11.10 5.90 -3 -1 15 -6.40 4.90 -3 -1 15 -1.90 3.20 3 -1 -15 6.90 5.30 3 -1 -15 6.40 7.90 -3 1 15 0.30 5.50 -3 1 15 5.60 2.60 3 1 -15 15.70 5.30 -3 1 15 -5.80 7.10 -2 -1 15 186.28 10.80 2 -1 -15 163.48 5.60 2 -1 -15 131.49 17.90 2 -1 -15 153.38 10.20 -2 -1 15 157.68 10.80 -2 -1 15 169.18 7.30 2 1 -15 157.58 5.70 -2 1 15 175.38 12.10 2 1 -15 160.88 9.80 -2 1 15 164.28 6.80 -2 1 15 175.08 11.90 1 -1 -15 19.30 10.00 -1 -1 15 12.20 7.00 -1 -1 15 13.60 3.10 1 -1 -15 13.90 5.50 -1 -1 15 17.20 5.80 1 -1 -15 15.40 2.00 -1 1 15 12.40 2.80 1 1 -15 12.50 1.80 -1 1 15 22.10 6.30 1 1 -15 10.40 5.40 0 -1 15 -5.10 5.70 0 -1 15 5.30 2.80 0 -1 -15 -0.20 1.80 0 -1 -15 4.70 5.60 0 1 15 -1.90 2.50 0 1 -15 3.60 5.10 0 1 -15 3.10 1.80 0 1 15 10.00 6.30 1 -1 15 43.70 8.30 1 -1 15 27.60 3.90 -1 -1 -15 32.00 3.20 -1 -1 -15 30.00 6.00 -1 1 -15 28.10 3.10 1 1 15 23.90 6.90 -1 1 -15 21.50 5.30 1 1 15 21.80 2.90 -2 -1 -15 57.29 7.60 -2 -1 -15 57.69 3.80 2 -1 15 61.89 4.10 2 1 15 57.29 8.60 -2 1 -15 61.79 7.40 -2 1 -15 53.99 3.60 2 1 15 58.69 3.90 3 -2 -15 32.50 7.90 -3 -2 15 44.60 6.80 -3 -2 15 37.50 5.10 3 -2 -15 26.50 7.20 -3 -2 15 24.60 5.70 -3 2 15 64.39 10.10 3 2 -15 42.60 5.50 -3 2 15 37.50 3.90 -3 2 15 43.50 9.00 2 -2 -15 18.20 6.20 2 -2 -15 17.60 6.50 -2 -2 15 7.70 5.80 -2 -2 15 10.80 6.00 -2 2 15 22.90 3.60 2 2 -15 16.30 5.20 -2 2 15 21.80 7.70 1 -2 -15 27.20 9.60 -1 -2 15 35.80 6.50 -1 -2 15 29.40 8.00 -1 -2 15 37.70 4.50 1 -2 -15 26.20 3.00 1 -2 -15 25.00 6.40 1 2 -15 33.60 5.60 -1 2 15 30.70 3.70 -1 2 15 33.50 7.30 1 2 -15 31.50 3.60 0 -2 -15 5.70 1.70 0 -2 -15 1.00 7.40 0 -2 15 12.00 7.00 0 -2 -15 3.90 6.60 0 2 15 7.30 2.30 0 2 15 2.20 6.70 0 2 -15 5.90 5.00 1 -2 15 25.00 3.70 -1 -2 -15 23.50 6.70 1 -2 15 12.90 13.00 -1 -2 -15 32.10 8.60 1 2 15 29.00 7.00 -1 2 -15 25.40 2.70 -1 2 -15 20.30 5.30 1 2 15 26.80 3.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 43257 _shelx_res_file ; TITL CP93123rrrr_0m_a.res in P2(1) shelx.res created by SHELXL-2016/6 at 13:17:54 on 19-Jan-2018 REM Old TITL CP93123rrrr_0m in P2(1) REM SHELXT solution in P2(1) REM R1 0.096, Rweak 0.027, Alpha 0.002, Orientation as input REM Flack x = 0.172 ( 0.071 ) from Parsons' quotients REM Formula found by SHELXT: C29 O5 CELL 1.54178 12.1129 7.8973 12.9253 90.000 94.930 90.000 ZERR 2.000 0.0003 0.0002 0.0003 0.000 0.001 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H O UNIT 58 72 10 TEMP -173.150 SIZE 0.06 0.13 0.17 L.S. 20 ACTA CONF BOND $H EQIV $1 x, y+1, z HTAB O5 O2_$1 HTAB LIST 4 FMAP 2 MPLA 5 O2 C12 C13 C15 C16 TWIN PLAN 20 WGHT 0.050100 0.213100 BASF 0.04629 FVAR 0.85987 O1 3 0.517800 0.195961 0.125454 11.00000 0.01556 0.02757 = 0.01518 0.00416 0.00700 0.00229 AFIX 147 H1 2 0.583625 0.166840 0.119366 11.00000 -1.50000 AFIX 0 O2 3 0.228094 -0.468747 -0.012841 11.00000 0.02894 0.01529 = 0.02195 0.00114 -0.00274 0.00127 O3 3 0.319466 0.190745 0.318523 11.00000 0.02015 0.02013 = 0.01376 0.00120 0.00846 0.00305 O4 3 0.286264 0.467799 0.349030 11.00000 0.03324 0.02325 = 0.03606 -0.00849 0.01764 -0.00109 O5 3 0.190743 0.278195 0.145540 11.00000 0.01841 0.01684 = 0.02243 0.00352 0.00553 0.00657 AFIX 147 H5 2 0.187516 0.371232 0.113926 11.00000 -1.50000 AFIX 0 C1 1 0.573823 -0.146272 0.193362 11.00000 0.02100 0.02536 = 0.02008 -0.00191 -0.00124 0.00909 AFIX 23 H1A 2 0.563465 -0.270610 0.191241 11.00000 -1.20000 H1B 2 0.596970 -0.110358 0.125098 11.00000 -1.20000 AFIX 0 C2 1 0.665830 -0.103320 0.277136 11.00000 0.02268 0.03498 = 0.02560 -0.00867 -0.00475 0.01300 AFIX 23 H2A 2 0.646674 -0.150083 0.344371 11.00000 -1.20000 H2B 2 0.735565 -0.157536 0.259730 11.00000 -1.20000 AFIX 0 C3 1 0.683985 0.086438 0.288172 11.00000 0.01834 0.03687 = 0.02377 -0.00514 -0.00273 0.00427 AFIX 23 H3A 2 0.711327 0.130558 0.223380 11.00000 -1.20000 H3B 2 0.742076 0.107536 0.345374 11.00000 -1.20000 AFIX 0 C4 1 0.577788 0.184991 0.310524 11.00000 0.01833 0.02454 = 0.01792 -0.00161 0.00102 0.00060 C5 1 0.483324 0.132969 0.223784 11.00000 0.01668 0.02102 = 0.01070 0.00200 0.00536 0.00203 C6 1 0.374999 0.233520 0.227382 11.00000 0.01849 0.01595 = 0.01370 0.00264 0.00780 -0.00015 AFIX 13 H6 2 0.392800 0.357187 0.229305 11.00000 -1.20000 AFIX 0 C7 1 0.295302 0.197620 0.132329 11.00000 0.01509 0.01566 = 0.01495 0.00321 0.00597 0.00514 AFIX 13 H7 2 0.326559 0.247100 0.069884 11.00000 -1.20000 AFIX 0 C8 1 0.272048 0.010491 0.112479 11.00000 0.01524 0.01645 = 0.01224 0.00401 0.00458 0.00213 AFIX 13 H8 2 0.232224 -0.032713 0.171772 11.00000 -1.20000 AFIX 0 C9 1 0.381193 -0.092005 0.111387 11.00000 0.01605 0.01562 = 0.01108 0.00145 0.00389 0.00378 AFIX 13 H9 2 0.419571 -0.052008 0.050411 11.00000 -1.20000 AFIX 0 C10 1 0.462111 -0.061511 0.210628 11.00000 0.01886 0.01678 = 0.01314 0.00039 0.00218 0.00420 C11 1 0.357608 -0.284585 0.095462 11.00000 0.02401 0.01907 = 0.01512 0.00167 -0.00036 0.00530 AFIX 23 H11A 2 0.421988 -0.339792 0.067248 11.00000 -1.20000 H11B 2 0.346108 -0.337965 0.163002 11.00000 -1.20000 AFIX 0 C12 1 0.257459 -0.308355 0.022521 11.00000 0.02282 0.01602 = 0.01406 0.00138 0.00492 0.00042 C13 1 0.180785 -0.194773 -0.012871 11.00000 0.01636 0.01873 = 0.01621 0.00286 0.00544 -0.00029 C14 1 0.192425 -0.010517 0.012212 11.00000 0.01381 0.01717 = 0.02014 0.00173 0.00269 0.00340 AFIX 13 H14 2 0.117939 0.033202 0.027082 11.00000 -1.20000 AFIX 0 C15 1 0.097104 -0.286795 -0.074855 11.00000 0.01612 0.02387 = 0.02405 0.00312 0.00075 -0.00176 AFIX 43 H15 2 0.031927 -0.241267 -0.110517 11.00000 -1.20000 AFIX 0 C16 1 0.128795 -0.449796 -0.072679 11.00000 0.02416 0.02179 = 0.02539 0.00144 -0.00206 -0.00469 AFIX 43 H16 2 0.088574 -0.539445 -0.107408 11.00000 -1.20000 AFIX 0 C17 1 0.556459 0.151567 0.425065 11.00000 0.02815 0.03055 = 0.01654 -0.00445 -0.00066 0.00301 AFIX 137 H17A 2 0.612996 0.209595 0.470912 11.00000 -1.50000 H17B 2 0.559908 0.029565 0.438823 11.00000 -1.50000 H17C 2 0.482962 0.194371 0.438008 11.00000 -1.50000 AFIX 0 C18 1 0.601204 0.375986 0.303394 11.00000 0.02452 0.02668 = 0.03065 -0.00338 0.00102 -0.00211 AFIX 137 H18A 2 0.540690 0.439604 0.330854 11.00000 -1.50000 H18B 2 0.606793 0.407338 0.230669 11.00000 -1.50000 H18C 2 0.671040 0.402637 0.344118 11.00000 -1.50000 AFIX 0 C19 1 0.413595 -0.144417 0.305960 11.00000 0.02913 0.01685 = 0.01207 0.00237 0.00145 0.00434 AFIX 137 H19A 2 0.444707 -0.088795 0.369703 11.00000 -1.50000 H19B 2 0.432678 -0.265020 0.308648 11.00000 -1.50000 H19C 2 0.332817 -0.131699 0.299626 11.00000 -1.50000 AFIX 0 C20 1 0.228866 0.085684 -0.082405 11.00000 0.02899 0.01789 = 0.01747 0.00419 -0.00429 -0.00221 AFIX 137 H20A 2 0.225048 0.207822 -0.069787 11.00000 -1.50000 H20B 2 0.179661 0.056395 -0.143969 11.00000 -1.50000 H20C 2 0.305132 0.054200 -0.093813 11.00000 -1.50000 AFIX 0 C21 1 0.273203 0.319956 0.368081 11.00000 0.01810 0.02574 = 0.01783 -0.00493 0.00376 0.00020 C22 1 0.206569 0.251919 0.449279 11.00000 0.01971 0.03139 = 0.01538 -0.00261 0.00296 0.00088 AFIX 43 H22 2 0.205628 0.133757 0.462953 11.00000 -1.20000 AFIX 0 C23 1 0.147853 0.358001 0.503084 11.00000 0.01789 0.03537 = 0.01722 -0.00578 0.00142 -0.00104 AFIX 43 H23 2 0.153196 0.474847 0.486769 11.00000 -1.20000 AFIX 0 C24 1 0.075610 0.313968 0.585039 11.00000 0.01336 0.04340 = 0.01568 -0.00730 0.00007 -0.00033 C25 1 0.060838 0.148712 0.619041 11.00000 0.02143 0.04481 = 0.01857 -0.00447 0.00118 0.00376 AFIX 43 H25 2 0.098725 0.058097 0.589145 11.00000 -1.20000 AFIX 0 C26 1 -0.009157 0.115767 0.696594 11.00000 0.02645 0.04875 = 0.02351 0.00428 0.00296 -0.00323 AFIX 43 H26 2 -0.019633 0.002787 0.719015 11.00000 -1.20000 AFIX 0 C27 1 -0.063781 0.248637 0.741244 11.00000 0.02520 0.06442 = 0.01985 -0.00106 0.00945 0.00106 AFIX 43 H27 2 -0.111276 0.226126 0.794396 11.00000 -1.20000 AFIX 0 C28 1 -0.049227 0.413229 0.708586 11.00000 0.02129 0.05366 = 0.02655 -0.00920 0.00712 0.00294 AFIX 43 H28 2 -0.086528 0.503687 0.739264 11.00000 -1.20000 AFIX 0 C29 1 0.019914 0.445736 0.631003 11.00000 0.01943 0.04321 = 0.02473 -0.00597 0.00451 0.00048 AFIX 43 H29 2 0.029684 0.558944 0.608671 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM CP93123rrrr_0m_a.res in P2(1) REM R1 = 0.0347 for 4183 Fo > 4sig(Fo) and 0.0398 for all 4526 data REM 314 parameters refined using 1 restraints END WGHT 0.0439 0.2229 REM Instructions for potential hydrogen bonds HTAB O5 O2_$1 REM Highest difference peak 0.188, deepest hole -0.207, 1-sigma level 0.041 Q1 1 0.5253 0.1581 0.2744 11.00000 0.05 0.19 Q2 1 0.7904 0.2757 0.5345 11.00000 0.05 0.18 Q3 1 0.5181 -0.0967 0.2014 11.00000 0.05 0.17 Q4 1 -0.0546 -0.2860 -0.1371 11.00000 0.05 0.15 Q5 1 0.0827 0.0066 0.6056 11.00000 0.05 0.14 Q6 1 0.3367 0.2150 0.1786 11.00000 0.05 0.14 Q7 1 0.2831 0.0998 0.1212 11.00000 0.05 0.14 Q8 1 0.4215 -0.0829 0.1649 11.00000 0.05 0.13 Q9 1 0.2272 0.0043 0.0636 11.00000 0.05 0.13 Q10 1 0.4350 0.1758 0.2339 11.00000 0.05 0.12 Q11 1 0.0168 -0.0136 0.7009 11.00000 0.05 0.12 Q12 1 0.4754 0.0340 0.2196 11.00000 0.05 0.12 Q13 1 0.2032 -0.2364 0.3705 11.00000 0.05 0.12 Q14 1 0.3491 0.1989 -0.1123 11.00000 0.05 0.12 Q15 1 0.6154 -0.1185 0.2334 11.00000 0.05 0.11 Q16 1 0.3587 0.5083 0.3400 11.00000 0.05 0.11 Q17 1 0.6439 -0.0529 0.4971 11.00000 0.05 0.11 Q18 1 0.0388 0.0669 0.0370 11.00000 0.05 0.11 Q19 1 0.8841 0.2799 0.2848 11.00000 0.05 0.11 Q20 1 0.4060 0.5005 0.4055 11.00000 0.05 0.11 ; _shelx_res_checksum 8659 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O1 0.51780(13) 0.1960(2) 0.12545(11) 0.0191(4) Uani d 1 H H1 0.583625 0.166840 0.119366 0.029 Uiso calc 1 O O2 0.22809(14) -0.4687(2) -0.01284(13) 0.0223(4) Uani d 1 O O3 0.31947(13) 0.1907(2) 0.31852(11) 0.0176(3) Uani d 1 O O4 0.28626(16) 0.4678(2) 0.34903(15) 0.0300(4) Uani d 1 O O5 0.19074(13) 0.2782(2) 0.14554(12) 0.0190(4) Uani d 1 H H5 0.187516 0.371232 0.113926 0.029 Uiso calc 1 C C1 0.5738(2) -0.1463(3) 0.19336(19) 0.0223(5) Uani d 1 H H1A 0.563465 -0.270610 0.191241 0.027 Uiso calc 1 H H1B 0.596970 -0.110358 0.125098 0.027 Uiso calc 1 C C2 0.6658(2) -0.1033(4) 0.2771(2) 0.0281(6) Uani d 1 H H2A 0.646674 -0.150083 0.344371 0.034 Uiso calc 1 H H2B 0.735565 -0.157536 0.259730 0.034 Uiso calc 1 C C3 0.6840(2) 0.0864(4) 0.2882(2) 0.0266(6) Uani d 1 H H3A 0.711327 0.130558 0.223380 0.032 Uiso calc 1 H H3B 0.742076 0.107536 0.345374 0.032 Uiso calc 1 C C4 0.57779(19) 0.1850(3) 0.31052(18) 0.0203(5) Uani d 1 C C5 0.48332(19) 0.1330(3) 0.22378(17) 0.0159(5) Uani d 1 C C6 0.37500(19) 0.2335(3) 0.22738(17) 0.0157(5) Uani d 1 H H6 0.392800 0.357187 0.229305 0.019 Uiso calc 1 C C7 0.29530(18) 0.1976(3) 0.13233(16) 0.0150(5) Uani d 1 H H7 0.326559 0.247100 0.069884 0.018 Uiso calc 1 C C8 0.27205(19) 0.0105(3) 0.11248(17) 0.0144(5) Uani d 1 H H8 0.232224 -0.032713 0.171772 0.017 Uiso calc 1 C C9 0.38119(18) -0.0920(3) 0.11139(16) 0.0141(5) Uani d 1 H H9 0.419571 -0.052008 0.050411 0.017 Uiso calc 1 C C10 0.46211(19) -0.0615(3) 0.21063(17) 0.0162(5) Uani d 1 C C11 0.35761(19) -0.2846(3) 0.09546(18) 0.0195(5) Uani d 1 H H11A 0.421988 -0.339792 0.067248 0.023 Uiso calc 1 H H11B 0.346108 -0.337965 0.163002 0.023 Uiso calc 1 C C12 0.25746(19) -0.3084(3) 0.02252(17) 0.0174(5) Uani d 1 C C13 0.1808(2) -0.1948(3) -0.01287(18) 0.0169(5) Uani d 1 C C14 0.19243(19) -0.0105(3) 0.01221(18) 0.0170(5) Uani d 1 H H14 0.117939 0.033202 0.027082 0.020 Uiso calc 1 C C15 0.09710(19) -0.2868(3) -0.07485(19) 0.0214(5) Uani d 1 H H15 0.031927 -0.241267 -0.110517 0.026 Uiso calc 1 C C16 0.1288(2) -0.4498(3) -0.0727(2) 0.0240(5) Uani d 1 H H16 0.088574 -0.539445 -0.107408 0.029 Uiso calc 1 C C17 0.5565(2) 0.1516(3) 0.42506(18) 0.0252(6) Uani d 1 H H17A 0.612996 0.209595 0.470912 0.038 Uiso calc 1 H H17B 0.559908 0.029565 0.438823 0.038 Uiso calc 1 H H17C 0.482962 0.194371 0.438008 0.038 Uiso calc 1 C C18 0.6012(2) 0.3760(3) 0.3034(2) 0.0274(6) Uani d 1 H H18A 0.540690 0.439604 0.330854 0.041 Uiso calc 1 H H18B 0.606793 0.407338 0.230669 0.041 Uiso calc 1 H H18C 0.671040 0.402637 0.344118 0.041 Uiso calc 1 C C19 0.4136(2) -0.1444(3) 0.30596(17) 0.0194(5) Uani d 1 H H19A 0.444707 -0.088795 0.369703 0.029 Uiso calc 1 H H19B 0.432678 -0.265020 0.308648 0.029 Uiso calc 1 H H19C 0.332817 -0.131699 0.299626 0.029 Uiso calc 1 C C20 0.2289(2) 0.0857(3) -0.08241(18) 0.0218(5) Uani d 1 H H20A 0.225048 0.207822 -0.069787 0.033 Uiso calc 1 H H20B 0.179661 0.056395 -0.143969 0.033 Uiso calc 1 H H20C 0.305132 0.054200 -0.093813 0.033 Uiso calc 1 C C21 0.2732(2) 0.3200(3) 0.36808(18) 0.0204(5) Uani d 1 C C22 0.2066(2) 0.2519(4) 0.44928(18) 0.0221(6) Uani d 1 H H22 0.205628 0.133757 0.462953 0.026 Uiso calc 1 C C23 0.1479(2) 0.3580(4) 0.50308(18) 0.0235(6) Uani d 1 H H23 0.153196 0.474847 0.486769 0.028 Uiso calc 1 C C24 0.0756(2) 0.3140(4) 0.58504(19) 0.0242(6) Uani d 1 C C25 0.0608(2) 0.1487(4) 0.61904(19) 0.0283(6) Uani d 1 H H25 0.098725 0.058097 0.589145 0.034 Uiso calc 1 C C26 -0.0092(2) 0.1158(4) 0.6966(2) 0.0329(7) Uani d 1 H H26 -0.019633 0.002787 0.719015 0.039 Uiso calc 1 C C27 -0.0638(2) 0.2486(5) 0.7412(2) 0.0361(8) Uani d 1 H H27 -0.111276 0.226126 0.794396 0.043 Uiso calc 1 C C28 -0.0492(2) 0.4132(4) 0.7086(2) 0.0335(7) Uani d 1 H H28 -0.086528 0.503687 0.739264 0.040 Uiso calc 1 C C29 0.0199(2) 0.4457(4) 0.6310(2) 0.0290(6) Uani d 1 H H29 0.029684 0.558944 0.608671 0.035 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0156(8) 0.0276(9) 0.0152(8) 0.0023(7) 0.0070(6) 0.0042(7) O2 0.0289(9) 0.0153(9) 0.0219(9) 0.0013(7) -0.0027(7) 0.0011(7) O3 0.0202(8) 0.0201(8) 0.0138(7) 0.0030(7) 0.0085(6) 0.0012(7) O4 0.0332(11) 0.0233(10) 0.0361(10) -0.0011(8) 0.0176(9) -0.0085(8) O5 0.0184(9) 0.0168(8) 0.0224(8) 0.0066(7) 0.0055(7) 0.0035(7) C1 0.0210(13) 0.0254(13) 0.0201(12) 0.0091(10) -0.0012(10) -0.0019(10) C2 0.0227(13) 0.0350(15) 0.0256(13) 0.0130(12) -0.0047(11) -0.0087(12) C3 0.0183(12) 0.0369(16) 0.0238(13) 0.0043(11) -0.0027(10) -0.0051(11) C4 0.0183(11) 0.0245(13) 0.0179(11) 0.0006(11) 0.0010(9) -0.0016(11) C5 0.0167(11) 0.0210(12) 0.0107(10) 0.0020(9) 0.0054(9) 0.0020(9) C6 0.0185(11) 0.0159(12) 0.0137(10) -0.0002(9) 0.0078(9) 0.0026(9) C7 0.0151(11) 0.0157(11) 0.0149(10) 0.0051(10) 0.0060(9) 0.0032(10) C8 0.0152(11) 0.0164(12) 0.0122(10) 0.0021(9) 0.0046(9) 0.0040(9) C9 0.0161(11) 0.0156(11) 0.0111(10) 0.0038(9) 0.0039(8) 0.0015(9) C10 0.0189(12) 0.0168(12) 0.0131(10) 0.0042(9) 0.0022(9) 0.0004(9) C11 0.0240(12) 0.0191(12) 0.0151(10) 0.0053(11) -0.0004(9) 0.0017(10) C12 0.0228(12) 0.0160(11) 0.0141(10) 0.0004(10) 0.0049(9) 0.0014(10) C13 0.0164(11) 0.0187(12) 0.0162(11) -0.0003(9) 0.0054(9) 0.0029(9) C14 0.0138(11) 0.0172(12) 0.0201(11) 0.0034(9) 0.0027(9) 0.0017(9) C15 0.0161(11) 0.0239(13) 0.0241(12) -0.0018(10) 0.0007(9) 0.0031(11) C16 0.0242(13) 0.0218(13) 0.0254(13) -0.0047(11) -0.0021(10) 0.0014(11) C17 0.0281(14) 0.0306(15) 0.0165(11) 0.0030(11) -0.0007(10) -0.0044(10) C18 0.0245(13) 0.0267(15) 0.0307(14) -0.0021(11) 0.0010(11) -0.0034(11) C19 0.0291(13) 0.0169(12) 0.0121(10) 0.0043(10) 0.0014(10) 0.0024(9) C20 0.0290(13) 0.0179(12) 0.0175(12) -0.0022(11) -0.0043(10) 0.0042(9) C21 0.0181(12) 0.0257(14) 0.0178(12) 0.0002(10) 0.0038(10) -0.0049(10) C22 0.0197(12) 0.0314(15) 0.0154(11) 0.0009(10) 0.0030(10) -0.0026(10) C23 0.0179(12) 0.0354(15) 0.0172(12) -0.0010(11) 0.0014(10) -0.0058(11) C24 0.0134(12) 0.0434(17) 0.0157(11) -0.0003(11) 0.0001(10) -0.0073(11) C25 0.0214(13) 0.0448(18) 0.0186(12) 0.0038(11) 0.0012(10) -0.0045(12) C26 0.0265(14) 0.0487(18) 0.0235(13) -0.0032(13) 0.0030(11) 0.0043(13) C27 0.0252(14) 0.064(2) 0.0198(13) 0.0011(14) 0.0094(11) -0.0011(13) C28 0.0213(13) 0.054(2) 0.0265(14) 0.0029(13) 0.0071(11) -0.0092(14) C29 0.0194(13) 0.0432(18) 0.0247(13) 0.0005(12) 0.0045(11) -0.0060(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 C5 O1 H1 109.5 C16 O2 C12 105.83(18) C21 O3 C6 116.78(18) C7 O5 H5 109.5 C2 C1 C10 113.4(2) C2 C1 H1A 108.9 C10 C1 H1A 108.9 C2 C1 H1B 108.9 C10 C1 H1B 108.9 H1A C1 H1B 107.7 C3 C2 C1 112.2(2) C3 C2 H2A 109.2 C1 C2 H2A 109.2 C3 C2 H2B 109.2 C1 C2 H2B 109.2 H2A C2 H2B 107.9 C2 C3 C4 113.4(2) C2 C3 H3A 108.9 C4 C3 H3A 108.9 C2 C3 H3B 108.9 C4 C3 H3B 108.9 H3A C3 H3B 107.7 C18 C4 C17 105.7(2) C18 C4 C3 108.7(2) C17 C4 C3 107.6(2) C18 C4 C5 109.7(2) C17 C4 C5 117.6(2) C3 C4 C5 107.32(19) O1 C5 C6 99.16(17) O1 C5 C10 107.26(18) C6 C5 C10 112.19(19) O1 C5 C4 106.52(18) C6 C5 C4 114.24(19) C10 C5 C4 115.66(18) O3 C6 C7 107.87(17) O3 C6 C5 111.22(17) C7 C6 C5 111.28(18) O3 C6 H6 108.8 C7 C6 H6 108.8 C5 C6 H6 108.8 O5 C7 C8 107.28(18) O5 C7 C6 108.97(18) C8 C7 C6 114.34(19) O5 C7 H7 108.7 C8 C7 H7 108.7 C6 C7 H7 108.7 C7 C8 C9 111.26(18) C7 C8 C14 109.65(18) C9 C8 C14 113.85(17) C7 C8 H8 107.3 C9 C8 H8 107.3 C14 C8 H8 107.3 C8 C9 C11 111.34(18) C8 C9 C10 112.74(17) C11 C9 C10 110.70(18) C8 C9 H9 107.3 C11 C9 H9 107.3 C10 C9 H9 107.3 C1 C10 C19 109.14(19) C1 C10 C5 107.69(19) C19 C10 C5 113.40(18) C1 C10 C9 108.06(17) C19 C10 C9 109.40(18) C5 C10 C9 109.01(18) C12 C11 C9 109.77(19) C12 C11 H11A 109.7 C9 C11 H11A 109.7 C12 C11 H11B 109.7 C9 C11 H11B 109.7 H11A C11 H11B 108.2 C13 C12 O2 110.4(2) C13 C12 C11 129.5(2) O2 C12 C11 120.0(2) C12 C13 C15 106.7(2) C12 C13 C14 121.8(2) C15 C13 C14 131.5(2) C13 C14 C20 109.7(2) C13 C14 C8 108.94(19) C20 C14 C8 114.22(19) C13 C14 H14 107.9 C20 C14 H14 107.9 C8 C14 H14 107.9 C16 C15 C13 106.7(2) C16 C15 H15 126.7 C13 C15 H15 126.7 C15 C16 O2 110.4(2) C15 C16 H16 124.8 O2 C16 H16 124.8 C4 C17 H17A 109.5 C4 C17 H17B 109.5 H17A C17 H17B 109.5 C4 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C4 C18 H18A 109.5 C4 C18 H18B 109.5 H18A C18 H18B 109.5 C4 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C10 C19 H19A 109.5 C10 C19 H19B 109.5 H19A C19 H19B 109.5 C10 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C14 C20 H20A 109.5 C14 C20 H20B 109.5 H20A C20 H20B 109.5 C14 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O4 C21 O3 124.5(2) O4 C21 C22 125.8(2) O3 C21 C22 109.6(2) C23 C22 C21 119.4(2) C23 C22 H22 120.3 C21 C22 H22 120.3 C22 C23 C24 127.1(3) C22 C23 H23 116.4 C24 C23 H23 116.4 C25 C24 C29 118.9(2) C25 C24 C23 123.3(2) C29 C24 C23 117.9(3) C26 C25 C24 120.3(3) C26 C25 H25 119.8 C24 C25 H25 119.8 C27 C26 C25 119.9(3) C27 C26 H26 120.1 C25 C26 H26 120.1 C28 C27 C26 120.3(3) C28 C27 H27 119.9 C26 C27 H27 119.9 C27 C28 C29 119.8(3) C27 C28 H28 120.1 C29 C28 H28 120.1 C28 C29 C24 120.9(3) C28 C29 H29 119.6 C24 C29 H29 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C5 1.459(3) O1 H1 0.8400 O2 C16 1.381(3) O2 C12 1.383(3) O3 C21 1.352(3) O3 C6 1.446(3) O4 C21 1.206(3) O5 C7 1.441(3) O5 H5 0.8400 C1 C2 1.524(3) C1 C10 1.543(3) C1 H1A 0.9900 C1 H1B 0.9900 C2 C3 1.520(4) C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.552(3) C3 H3A 0.9900 C3 H3B 0.9900 C4 C18 1.539(4) C4 C17 1.547(3) C4 C5 1.586(3) C5 C6 1.538(3) C5 C10 1.564(3) C6 C7 1.522(3) C6 H6 1.0000 C7 C8 1.522(3) C7 H7 1.0000 C8 C9 1.551(3) C8 C14 1.556(3) C8 H8 1.0000 C9 C11 1.558(3) C9 C10 1.565(3) C9 H9 1.0000 C10 C19 1.555(3) C11 C12 1.483(3) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.343(3) C13 C15 1.435(3) C13 C14 1.495(3) C14 C20 1.536(3) C14 H14 1.0000 C15 C16 1.343(4) C15 H15 0.9500 C16 H16 0.9500 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 C22 1.479(3) C22 C23 1.333(3) C22 H22 0.9500 C23 C24 1.472(3) C23 H23 0.9500 C24 C25 1.394(4) C24 C29 1.400(4) C25 C26 1.392(4) C25 H25 0.9500 C26 C27 1.392(4) C26 H26 0.9500 C27 C28 1.383(5) C27 H27 0.9500 C28 C29 1.385(4) C28 H28 0.9500 C29 H29 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O5 H5 O2 1_565 0.84 2.16 2.924(2) 151 C3 H3A Cg1 2_655 0.98 2.94 3.896(3) 163 C17 H17C O3 . 0.98 2.40 3.091(3) 127 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 C1 C2 C3 -56.4(3) C1 C2 C3 C4 56.2(3) C2 C3 C4 C18 -171.4(2) C2 C3 C4 C17 74.6(3) C2 C3 C4 C5 -52.8(3) C18 C4 C5 O1 52.4(2) C17 C4 C5 O1 173.2(2) C3 C4 C5 O1 -65.5(2) C18 C4 C5 C6 -56.0(2) C17 C4 C5 C6 64.8(3) C3 C4 C5 C6 -173.9(2) C18 C4 C5 C10 171.51(19) C17 C4 C5 C10 -67.7(3) C3 C4 C5 C10 53.6(3) C21 O3 C6 C7 -98.4(2) C21 O3 C6 C5 139.3(2) O1 C5 C6 O3 178.25(17) C10 C5 C6 O3 65.3(2) C4 C5 C6 O3 -68.9(2) O1 C5 C6 C7 58.0(2) C10 C5 C6 C7 -55.0(2) C4 C5 C6 C7 170.81(19) O3 C6 C7 O5 50.8(2) C5 C6 C7 O5 173.09(18) O3 C6 C7 C8 -69.2(2) C5 C6 C7 C8 53.1(2) O5 C7 C8 C9 -172.61(16) C6 C7 C8 C9 -51.7(2) O5 C7 C8 C14 60.5(2) C6 C7 C8 C14 -178.51(17) C7 C8 C9 C11 177.74(18) C14 C8 C9 C11 -57.7(2) C7 C8 C9 C10 52.6(2) C14 C8 C9 C10 177.15(19) C2 C1 C10 C19 -70.0(3) C2 C1 C10 C5 53.5(3) C2 C1 C10 C9 171.1(2) O1 C5 C10 C1 64.7(2) C6 C5 C10 C1 172.59(17) C4 C5 C10 C1 -53.9(2) O1 C5 C10 C19 -174.41(18) C6 C5 C10 C19 -66.6(2) C4 C5 C10 C19 66.9(3) O1 C5 C10 C9 -52.3(2) C6 C5 C10 C9 55.6(2) C4 C5 C10 C9 -170.95(17) C8 C9 C10 C1 -171.20(19) C11 C9 C10 C1 63.3(2) C8 C9 C10 C19 70.1(2) C11 C9 C10 C19 -55.4(2) C8 C9 C10 C5 -54.4(2) C11 C9 C10 C5 -179.89(18) C8 C9 C11 C12 36.7(2) C10 C9 C11 C12 162.98(17) C16 O2 C12 C13 0.1(2) C16 O2 C12 C11 176.0(2) C9 C11 C12 C13 -12.6(3) C9 C11 C12 O2 172.36(19) O2 C12 C13 C15 -0.1(3) C11 C12 C13 C15 -175.5(2) O2 C12 C13 C14 -179.1(2) C11 C12 C13 C14 5.5(4) C12 C13 C14 C20 103.5(2) C15 C13 C14 C20 -75.2(3) C12 C13 C14 C8 -22.2(3) C15 C13 C14 C8 159.1(2) C7 C8 C14 C13 173.58(18) C9 C8 C14 C13 48.2(2) C7 C8 C14 C20 50.6(2) C9 C8 C14 C20 -74.8(3) C12 C13 C15 C16 0.0(3) C14 C13 C15 C16 178.9(2) C13 C15 C16 O2 0.0(3) C12 O2 C16 C15 -0.1(3) C6 O3 C21 O4 -9.1(3) C6 O3 C21 C22 171.78(18) O4 C21 C22 C23 5.2(4) O3 C21 C22 C23 -175.7(2) C21 C22 C23 C24 178.9(2) C22 C23 C24 C25 1.2(4) C22 C23 C24 C29 -179.2(2) C29 C24 C25 C26 0.7(4) C23 C24 C25 C26 -179.7(2) C24 C25 C26 C27 -0.7(4) C25 C26 C27 C28 0.3(4) C26 C27 C28 C29 0.1(4) C27 C28 C29 C24 -0.1(4) C25 C24 C29 C28 -0.3(4) C23 C24 C29 C28 -179.9(2) _cod_database_fobs_code 2242398