#------------------------------------------------------------------------------ #$Date: 2015-07-12 04:08:09 +0300 (Sun, 12 Jul 2015) $ #$Revision: 146545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/09/2240916.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_2240916 loop_ _publ_author_name 'Lou, Benyong' _publ_section_title ; Crystal structure of 1,3-dihydroxy-2-(hydroxymethyl)propan-2-aminium 2-(4-isobutylphenyl)propanoate: a simple organic salt of racemic ibuprofen ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 923 _journal_page_last 925 _journal_paper_doi 10.1107/S2056989015012979 _journal_volume 71 _journal_year 2015 _chemical_formula_iupac 'C4 H12 N O3 +, C13 H17 O2 -' _chemical_formula_moiety 'C4 H12 N O3 +, C13 H17 O2 -' _chemical_formula_sum 'C17 H29 N O5' _chemical_formula_weight 327.41 _chemical_name_systematic ; 1,3-Dihydroxy-2-(hydroxymethyl)propan-2-aminium 2-(4-isobutylphenyl)propanoate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 97.032(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.523(7) _cell_length_b 10.400(4) _cell_length_c 9.976(4) _cell_measurement_reflns_used 4551 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.4778 _cell_measurement_theta_min 2.8393 _cell_volume 1804.3(12) _computing_cell_refinement ; CrystalClear (Rigaku, 2000) ; _computing_data_collection ; CrystalClear (Rigaku, 2000) ; _computing_data_reduction ; CrystalClear (Rigaku, 2000) ; _computing_molecular_graphics ; X-SEED (Barbour, 2001) ; _computing_publication_material ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 13747 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 2.282 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrystalClear; Rigaku, 2000) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.205 _exptl_crystal_description plate _exptl_crystal_F_000 712 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.216 _refine_diff_density_min -0.228 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 260 _refine_ls_number_reflns 4096 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.106 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0580 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.4122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1373 _refine_ls_wR_factor_ref 0.1477 _reflns_number_gt 3391 _reflns_number_total 4096 _reflns_threshold_expression I>2\s(I) _cod_data_source_file su5165sup1.cif _cod_data_source_block I _cod_database_code 2240916 _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_hkl_file ; 2 0 0 30.99 0.87 -2 0 0 28.43 0.74 -2 0 0 29.99 0.62 3 0 0 1.70 0.65 -3 0 0 0.94 0.74 -3 0 0 1.05 0.65 3 0 0 0.38 0.17 4 0 0 328.99 3.47 -4 0 0 331.47 3.28 5 0 0 4401.48 28.60 -5 0 0 4409.51 10.39 6 0 0 872.10 8.23 -6 0 0 884.75 7.18 7 0 0 1637.55 13.33 -7 0 0 1712.22 12.45 8 0 0 2166.43 17.94 -8 0 0 2243.76 15.24 9 0 0 169.36 5.06 -9 0 0 171.24 4.38 10 0 0 182.44 4.35 -10 0 0 171.03 3.30 11 0 0 58.50 3.01 -11 0 0 48.49 3.28 12 0 0 22.45 2.24 -12 0 0 24.10 1.95 13 0 0 23.58 2.33 -13 0 0 27.87 1.96 14 0 0 181.92 6.02 -14 0 0 218.13 5.09 15 0 0 93.81 4.62 -15 0 0 100.35 5.05 16 0 0 0.91 1.78 -16 0 0 2.36 1.55 17 0 0 2.84 1.77 -17 0 0 2.82 1.93 18 0 0 2.09 1.83 -18 0 0 0.84 0.92 19 0 0 18.27 2.70 -19 0 0 15.58 5.73 20 0 0 5.94 2.60 -20 0 0 3.53 1.85 21 0 0 2.28 2.24 -21 0 0 0.86 1.10 22 0 0 1.27 1.76 -22 0 0 1.46 0.95 1 -1 0 484.23 3.41 1 1 0 493.55 3.69 -1 -1 0 489.08 3.71 1 1 0 464.14 3.81 -1 -1 0 480.78 3.27 -1 1 0 492.88 3.36 2 -1 0 14.43 0.58 -2 1 0 15.03 0.72 2 1 0 17.51 0.93 -2 -1 0 15.30 0.69 -2 -1 0 16.41 0.79 2 1 0 15.48 0.71 3 -1 0 3726.81 23.22 3 1 0 3814.09 24.09 3 -1 0 3740.74 23.78 -3 -1 0 3801.81 23.54 4 -1 0 349.13 3.79 4 1 0 341.48 4.11 -4 1 0 350.72 3.39 -4 -1 0 344.33 3.54 5 1 0 23.83 1.59 -5 1 0 21.85 1.43 -5 -1 0 21.10 1.07 6 -1 0 360.58 4.64 6 1 0 356.39 4.83 -6 1 0 361.95 3.84 7 -1 0 852.92 8.35 7 1 0 818.27 8.39 -7 1 0 823.33 7.32 -7 -1 0 836.03 8.07 8 -1 0 23.43 1.54 8 1 0 29.62 1.91 -8 1 0 26.80 1.40 -8 -1 0 27.40 1.55 9 -1 0 59.04 2.59 9 1 0 64.37 3.25 -9 1 0 63.85 5.87 -9 -1 0 58.16 2.18 10 -1 0 0.74 1.24 10 1 0 -0.73 1.35 -10 1 0 0.88 0.84 -10 -1 0 0.60 0.65 11 -1 0 7.85 1.37 11 1 0 10.44 1.70 -11 1 0 9.18 2.61 -11 -1 0 7.48 1.49 12 -1 0 9.67 1.95 12 1 0 5.93 1.23 -12 1 0 8.15 1.88 -12 -1 0 8.14 2.03 13 -1 0 12.05 1.86 13 1 0 9.40 1.86 -13 1 0 8.57 3.18 -13 -1 0 9.06 2.27 14 -1 0 151.78 5.28 14 1 0 148.58 5.18 -14 1 0 143.08 6.49 -14 -1 0 144.77 4.62 15 -1 0 40.40 3.72 15 1 0 37.18 2.93 -15 1 0 40.38 2.62 -15 -1 0 46.74 6.39 16 -1 0 68.37 4.81 16 1 0 66.32 3.87 -16 1 0 61.26 3.75 -16 -1 0 67.18 9.06 17 -1 0 29.76 3.50 17 1 0 30.68 2.80 -17 1 0 29.06 5.33 -17 -1 0 30.57 4.30 18 -1 0 25.34 3.71 18 1 0 23.51 2.68 -18 1 0 16.47 7.45 -18 -1 0 20.98 6.55 19 -1 0 3.42 1.61 19 1 0 6.11 2.33 -19 -1 0 2.27 0.78 20 -1 0 1.16 1.41 20 1 0 3.98 2.43 -20 1 0 0.16 0.51 -20 -1 0 0.46 0.65 21 -1 0 2.13 1.71 21 1 0 1.16 1.53 -21 1 0 0.81 1.08 -21 -1 0 2.18 1.24 22 -1 0 7.44 2.54 22 1 0 7.08 2.51 -22 1 0 1.99 1.23 0 -2 0 559.92 4.27 0 -2 0 561.34 4.83 0 2 0 556.27 3.97 -1 -2 0 20.70 0.91 1 -2 0 21.84 0.78 1 -2 0 21.89 0.94 1 2 0 21.65 0.75 -1 -2 0 21.33 0.61 -1 2 0 21.06 0.55 1 -2 0 21.25 0.56 2 -2 0 433.72 3.74 2 2 0 438.28 4.13 -2 -2 0 440.69 4.29 -2 -2 0 431.98 3.51 -2 2 0 436.51 3.43 3 -2 0 861.64 7.47 3 2 0 874.49 7.21 -3 -2 0 850.34 6.95 -3 2 0 864.81 6.15 4 -2 0 17.23 1.01 4 2 0 18.89 1.29 -4 -2 0 19.76 1.14 5 -2 0 618.66 5.92 5 2 0 605.81 6.46 -5 -2 0 609.65 6.00 6 -2 0 227.19 3.47 6 2 0 230.36 3.96 -6 -2 0 223.67 3.44 7 -2 0 505.20 6.85 7 2 0 488.23 6.05 -7 -2 0 501.25 5.22 8 -2 0 373.06 5.06 8 2 0 369.05 5.66 -8 -2 0 369.98 4.75 9 -2 0 154.19 4.66 9 2 0 156.04 4.79 -9 2 0 162.77 4.15 -9 -2 0 156.77 4.29 10 -2 0 0.99 1.43 10 2 0 0.46 1.25 -10 2 0 0.89 0.80 -10 -2 0 1.40 0.89 11 -2 0 1.41 0.92 11 2 0 1.81 1.27 -11 2 0 0.74 0.70 -11 -2 0 0.61 0.62 12 -2 0 3.09 1.29 12 2 0 6.54 2.18 -12 2 0 3.81 1.01 -12 -2 0 4.93 1.07 13 -2 0 23.20 2.39 13 2 0 24.06 2.38 -13 2 0 22.87 4.71 -13 -2 0 23.69 4.99 14 -2 0 34.36 2.86 14 2 0 35.90 3.12 -14 2 0 33.87 3.55 -14 -2 0 34.50 7.22 15 -2 0 12.89 3.63 15 2 0 13.88 2.21 -15 2 0 9.85 3.63 -15 -2 0 11.51 3.03 16 2 0 14.20 2.23 -16 2 0 14.74 1.56 -16 -2 0 16.49 5.93 17 -2 0 6.80 2.97 17 2 0 4.14 2.00 -17 -2 0 5.95 1.40 18 -2 0 15.62 2.34 18 2 0 16.27 2.85 19 -2 0 20.90 3.16 19 2 0 22.54 2.83 -19 -2 0 16.96 5.21 20 -2 0 10.18 2.62 20 2 0 14.05 2.46 -20 -2 0 7.68 3.05 21 -2 0 12.47 2.30 21 2 0 10.67 2.42 22 -2 0 0.38 1.54 22 2 0 0.14 1.74 -22 -2 0 0.50 0.80 0 -3 0 0.77 0.38 0 -3 0 1.25 1.11 0 3 0 0.72 0.46 -1 -3 0 307.52 3.00 1 -3 0 302.72 2.92 -1 -3 0 311.71 5.80 1 -3 0 311.76 3.78 1 3 0 310.12 2.84 -1 3 0 305.45 2.61 -2 -3 0 42.08 1.85 2 -3 0 40.34 1.24 -2 -3 0 40.19 2.15 2 -3 0 38.37 1.51 2 3 0 41.46 1.44 -2 3 0 36.62 0.94 3 -3 0 1.10 0.59 3 3 0 1.03 0.92 -3 -3 0 0.47 1.13 -3 3 0 -0.07 0.54 4 -3 0 66.12 1.81 4 3 0 68.12 2.10 -4 -3 0 64.06 1.93 -4 3 0 64.83 1.75 5 -3 0 1.85 0.88 5 3 0 2.00 0.84 -5 -3 0 0.19 0.97 -5 3 0 0.44 0.58 6 -3 0 23.61 1.34 6 3 0 21.59 1.52 -6 -3 0 20.05 1.38 7 -3 0 37.73 1.87 7 3 0 37.37 2.10 -7 -3 0 35.79 1.86 8 -3 0 5.86 1.01 8 3 0 3.21 1.18 -8 -3 0 5.66 1.08 9 -3 0 83.46 2.57 9 3 0 77.57 3.15 -9 -3 0 82.48 2.57 10 -3 0 36.47 2.05 10 3 0 41.16 2.51 -10 -3 0 36.99 1.82 11 -3 0 6.64 1.35 11 3 0 8.12 1.66 -11 -3 0 5.03 1.13 12 -3 0 2.50 1.26 12 3 0 3.98 2.14 -12 -3 0 4.02 1.63 13 -3 0 0.30 1.23 13 3 0 2.61 1.50 -13 -3 0 2.36 1.34 14 -3 0 20.35 2.28 14 3 0 16.13 2.18 -14 -3 0 20.43 4.23 15 -3 0 16.54 2.06 15 3 0 12.03 2.06 -15 -3 0 15.19 2.92 16 -3 0 21.89 4.57 16 3 0 20.15 2.39 -16 -3 0 22.96 6.10 17 -3 0 35.07 4.07 17 3 0 35.47 3.14 -17 -3 0 42.14 2.72 18 -3 0 10.69 2.29 18 3 0 11.08 2.86 -18 -3 0 9.86 5.22 19 -3 0 22.16 2.76 19 3 0 19.08 2.66 -19 -3 0 17.19 6.60 20 -3 0 2.90 2.23 20 3 0 5.31 2.55 -20 -3 0 2.16 1.09 21 -3 0 2.83 1.63 21 3 0 3.21 2.01 -21 -3 0 1.65 1.30 22 -3 0 9.72 2.92 22 3 0 12.40 3.03 0 -4 0 356.57 4.69 0 -4 0 353.54 4.69 0 4 0 354.63 3.55 -1 -4 0 7.55 2.00 1 -4 0 7.87 1.64 -1 -4 0 5.55 1.02 1 -4 0 6.22 0.82 1 4 0 7.53 0.74 -1 4 0 8.88 0.62 -2 -4 0 333.81 3.81 2 -4 0 323.90 3.51 -2 -4 0 332.36 4.79 2 -4 0 325.71 4.29 2 4 0 326.57 3.06 -2 4 0 324.33 3.51 3 -4 0 11.77 1.08 3 4 0 12.98 1.57 -3 -4 0 11.29 1.24 3 -4 0 11.17 1.22 -3 4 0 9.31 0.68 4 4 0 1171.27 9.04 -4 -4 0 1146.82 9.59 5 -4 0 51.31 2.14 5 4 0 52.06 2.29 -5 -4 0 43.41 2.07 -5 4 0 49.82 1.81 6 -4 0 44.72 2.02 6 4 0 35.61 1.94 -6 -4 0 42.73 2.10 -6 4 0 41.05 1.82 7 -4 0 1.33 1.08 7 4 0 0.73 1.03 -7 -4 0 1.00 1.02 -7 4 0 1.64 0.59 8 -4 0 15.28 1.56 8 4 0 11.97 1.41 -8 -4 0 11.68 1.36 -8 4 0 12.03 0.90 9 -4 0 28.06 1.89 9 4 0 23.03 2.16 -9 -4 0 24.01 1.69 -9 4 0 25.18 1.34 10 -4 0 2.28 1.10 10 4 0 2.74 1.87 -10 -4 0 1.55 1.02 11 -4 0 5.27 1.25 11 4 0 6.26 1.65 -11 -4 0 5.34 1.21 12 -4 0 255.26 5.20 12 4 0 252.70 6.04 -12 -4 0 267.16 5.89 13 -4 0 145.17 4.75 13 4 0 149.94 5.44 -13 -4 0 149.95 4.56 14 -4 0 0.32 1.29 14 4 0 -0.04 1.31 -14 -4 0 1.87 1.16 15 -4 0 12.46 2.31 15 4 0 10.92 2.38 -15 -4 0 8.54 2.57 16 -4 0 2.18 2.00 16 4 0 1.79 1.62 -16 -4 0 1.73 1.27 17 -4 0 39.12 4.01 17 4 0 32.60 3.26 -17 -4 0 34.40 5.71 18 -4 0 5.14 2.03 18 4 0 5.39 2.01 -18 -4 0 3.77 2.37 19 -4 0 18.25 2.40 19 4 0 24.04 3.02 -19 -4 0 19.62 6.53 20 -4 0 2.44 1.87 20 4 0 2.76 1.98 -20 -4 0 3.10 1.78 -20 4 0 0.80 1.02 21 -4 0 0.73 1.49 21 4 0 -0.51 1.74 -21 -4 0 1.75 1.37 -21 4 0 1.35 1.06 0 -5 0 0.96 0.63 0 -5 0 0.76 1.05 0 5 0 1.06 0.31 -1 -5 0 5.25 2.02 1 -5 0 6.60 1.61 -1 -5 0 5.76 1.28 1 -5 0 7.18 1.47 1 5 0 7.13 1.20 -1 5 0 7.27 1.55 -2 -5 0 271.28 3.74 2 -5 0 266.33 3.55 -2 -5 0 254.11 4.66 2 -5 0 263.17 4.55 2 5 0 273.25 3.03 -2 5 0 266.91 2.99 -3 -5 0 613.51 6.11 3 -5 0 604.05 5.41 -3 -5 0 606.29 6.84 3 -5 0 618.05 6.57 -3 5 0 600.95 5.41 4 -5 0 28.49 1.99 4 5 0 28.95 1.66 -4 -5 0 27.42 1.87 4 -5 0 29.67 2.15 -4 5 0 30.98 1.34 5 -5 0 18.32 2.80 5 5 0 17.45 1.64 -5 -5 0 18.43 1.72 -5 5 0 16.06 0.97 6 -5 0 0.15 0.74 6 5 0 -0.53 0.98 -6 -5 0 1.52 1.55 -6 5 0 0.53 0.56 7 -5 0 104.52 2.76 7 5 0 103.15 3.21 -7 -5 0 110.29 3.80 -7 5 0 105.77 2.30 8 -5 0 23.78 1.69 8 5 0 24.47 1.91 -8 -5 0 22.82 1.72 -8 5 0 24.76 1.29 9 -5 0 1.02 0.98 9 5 0 1.42 1.32 -9 -5 0 0.32 1.04 -9 5 0 0.66 0.46 10 -5 0 67.37 3.19 10 5 0 72.22 3.79 -10 -5 0 66.38 3.22 -10 5 0 72.27 2.77 11 -5 0 56.12 2.85 11 5 0 58.73 3.44 -11 -5 0 59.76 3.34 -11 5 0 59.56 3.95 12 -5 0 112.15 6.92 12 5 0 120.80 5.03 -12 -5 0 111.35 4.28 -12 5 0 113.80 3.30 13 -5 0 30.72 2.32 13 5 0 29.02 2.92 -13 -5 0 30.14 2.32 -13 5 0 26.49 1.70 14 -5 0 95.92 4.24 14 5 0 93.55 4.27 -14 -5 0 89.01 3.87 -14 5 0 93.98 3.59 15 -5 0 78.86 3.64 15 5 0 81.96 4.09 -15 -5 0 74.29 3.44 -15 5 0 81.00 2.96 16 -5 0 21.84 3.03 16 5 0 26.78 3.16 -16 -5 0 23.51 6.89 -16 5 0 25.26 1.98 17 -5 0 10.76 2.32 17 5 0 15.45 3.53 -17 -5 0 10.16 2.33 -17 5 0 10.05 1.62 18 -5 0 2.79 1.36 18 5 0 3.50 1.80 -18 -5 0 1.52 1.30 -18 5 0 2.59 1.07 19 -5 0 2.61 1.87 19 5 0 3.56 1.90 -19 -5 0 3.71 1.50 -19 5 0 4.59 2.57 20 -5 0 5.08 2.82 20 5 0 4.47 1.72 -20 -5 0 4.80 2.96 -20 5 0 3.30 1.61 0 -6 0 100.60 3.52 0 -6 0 108.01 3.74 0 6 0 111.19 2.16 -1 -6 0 59.03 5.53 1 -6 0 56.93 2.66 -1 -6 0 54.30 2.50 1 -6 0 53.30 2.73 1 6 0 53.64 2.36 -1 6 0 56.51 2.83 -2 -6 0 19.40 3.67 2 -6 0 21.68 3.81 -2 -6 0 18.92 2.08 2 -6 0 18.77 1.67 2 6 0 19.85 1.42 -2 6 0 19.14 1.50 -3 -6 0 67.21 3.12 3 -6 0 64.96 2.33 -3 -6 0 68.23 2.98 3 -6 0 68.07 2.79 -3 6 0 65.57 2.97 4 -6 0 453.97 5.94 4 6 0 461.31 6.63 -4 -6 0 452.49 7.43 4 -6 0 472.90 7.13 -4 6 0 461.56 5.47 5 -6 0 330.04 5.02 5 6 0 313.28 5.33 -5 -6 0 321.38 7.06 -5 6 0 315.61 4.25 6 -6 0 311.98 5.03 6 6 0 301.76 5.48 -6 -6 0 314.16 5.85 6 -6 0 324.37 5.77 -6 6 0 316.54 4.49 7 -6 0 3.44 0.96 -7 -6 0 2.06 1.13 -7 6 0 1.49 0.66 8 -6 0 1.79 0.85 8 6 0 0.98 1.23 -8 -6 0 1.36 1.11 -8 6 0 0.76 0.63 9 -6 0 6.74 1.51 9 6 0 7.28 1.64 -9 -6 0 5.74 1.34 -9 6 0 6.42 0.94 10 -6 0 25.60 1.92 10 6 0 21.31 2.09 -10 -6 0 25.36 2.21 -10 6 0 24.14 1.52 11 -6 0 72.79 3.33 11 6 0 81.00 4.25 -11 -6 0 72.81 3.49 -11 6 0 68.89 2.52 12 -6 0 92.96 4.01 12 6 0 96.00 4.96 -12 -6 0 94.51 4.29 -12 6 0 94.94 5.61 13 -6 0 176.01 5.06 13 6 0 189.23 5.93 -13 -6 0 176.85 5.38 -13 6 0 176.67 3.89 14 -6 0 1.69 1.87 14 6 0 1.65 1.41 -14 -6 0 2.23 1.86 -14 6 0 0.27 0.86 15 -6 0 63.21 3.25 15 6 0 68.07 4.19 -15 -6 0 65.84 3.61 -15 6 0 66.23 2.87 16 -6 0 48.56 3.78 16 6 0 37.42 3.63 -16 -6 0 46.01 3.41 -16 6 0 42.09 4.43 17 -6 0 2.90 1.80 17 6 0 6.37 2.69 -17 -6 0 3.01 1.66 -17 6 0 4.44 1.31 18 -6 0 1.95 1.27 18 6 0 3.03 1.91 -18 -6 0 1.71 0.88 -18 6 0 2.21 0.87 19 -6 0 14.21 2.76 19 6 0 8.84 2.42 -19 6 0 13.79 4.32 20 -6 0 3.26 2.05 20 6 0 3.61 1.82 -20 -6 0 1.83 1.19 -20 6 0 1.76 1.05 0 -7 0 0.77 0.50 0 -7 0 1.87 1.22 0 7 0 0.85 0.50 -1 -7 0 2.03 0.56 1 -7 0 2.33 0.55 -1 -7 0 2.91 1.38 1 -7 0 1.00 1.14 1 7 0 2.89 0.87 -1 7 0 1.92 0.66 -2 -7 0 0.84 0.60 2 -7 0 2.45 0.65 -2 -7 0 1.80 1.29 2 -7 0 1.49 1.24 2 7 0 1.62 0.54 -2 7 0 2.75 1.05 -3 -7 0 27.80 1.55 3 -7 0 27.65 2.99 -3 -7 0 22.12 1.98 3 -7 0 28.14 2.26 3 7 0 30.37 1.38 -3 7 0 31.06 2.04 4 -7 0 5.09 1.41 4 7 0 4.56 0.84 -4 -7 0 6.19 1.54 4 -7 0 5.84 1.53 -4 7 0 7.92 1.87 5 -7 0 8.05 1.02 5 7 0 8.42 1.30 -5 -7 0 6.97 1.42 5 -7 0 8.47 1.62 -5 7 0 8.09 0.88 6 -7 0 10.49 1.07 6 7 0 10.81 1.45 -6 -7 0 14.29 4.03 6 -7 0 11.80 1.81 -6 7 0 13.55 1.06 7 -7 0 9.70 1.14 7 7 0 11.68 1.69 -7 -7 0 12.10 1.70 7 -7 0 10.37 1.53 -7 7 0 11.11 1.14 8 -7 0 45.25 2.33 8 7 0 43.69 2.75 -8 -7 0 46.54 3.12 8 -7 0 44.55 2.81 -8 7 0 45.52 1.87 9 -7 0 110.28 4.29 9 7 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35.47 2.59 2 8 0 39.43 1.72 -2 8 0 36.38 1.64 -3 -8 0 -0.10 0.66 3 -8 0 1.79 0.73 -3 -8 0 1.06 1.57 3 -8 0 1.62 1.82 -3 8 0 1.53 0.75 4 -8 0 38.04 1.79 4 8 0 37.56 2.32 -4 -8 0 38.82 3.36 4 -8 0 32.60 2.20 -4 8 0 39.75 1.87 5 -8 0 1.47 0.62 5 8 0 2.05 1.19 -5 -8 0 0.92 1.01 5 -8 0 1.31 1.20 -5 8 0 0.82 0.44 6 -8 0 5.80 1.02 6 8 0 7.89 1.63 -6 -8 0 5.33 1.68 6 -8 0 4.82 1.27 -6 8 0 5.17 0.92 7 -8 0 7.65 1.10 7 8 0 7.66 1.43 -7 -8 0 7.98 1.80 7 -8 0 10.45 1.99 -7 8 0 8.04 1.24 8 -8 0 1.64 0.92 8 8 0 1.42 1.65 -8 -8 0 1.77 2.20 8 -8 0 1.84 1.25 -8 8 0 2.92 1.51 9 -8 0 18.42 4.69 9 8 0 20.26 2.27 -9 -8 0 24.67 3.11 9 -8 0 17.41 2.50 -9 8 0 19.13 1.48 10 -8 0 84.67 3.55 10 8 0 72.81 4.08 -10 -8 0 72.80 3.69 10 -8 0 82.42 4.10 -10 8 0 80.62 2.70 11 -8 0 1.04 1.09 11 8 0 0.97 1.43 -11 -8 0 1.89 2.14 11 -8 0 2.52 2.29 -11 8 0 1.06 1.42 12 -8 0 0.85 1.09 12 8 0 0.80 1.38 -12 -8 0 2.54 2.19 12 -8 0 3.27 1.80 -12 8 0 -0.08 0.87 13 -8 0 9.00 1.95 13 8 0 8.13 1.95 -13 -8 0 7.98 2.44 -13 8 0 10.48 1.65 14 -8 0 15.08 1.94 14 8 0 12.40 2.65 -14 -8 0 11.75 2.39 -14 8 0 6.30 4.55 15 -8 0 1.19 1.07 15 8 0 2.36 1.60 -15 -8 0 2.89 1.95 -15 8 0 0.12 1.02 16 8 0 10.57 2.99 -16 -8 0 6.29 2.86 -16 8 0 6.85 3.82 17 -8 0 2.94 1.94 17 8 0 0.40 1.49 -17 -8 0 1.79 1.43 -17 8 0 1.29 1.24 18 -8 0 5.20 1.81 -18 -8 0 3.86 1.57 -18 8 0 5.00 2.31 0 -9 0 0.15 0.38 0 -9 0 0.65 2.27 0 9 0 0.59 0.52 -1 -9 0 82.03 4.11 1 -9 0 81.17 4.32 -1 -9 0 79.19 3.75 1 -9 0 80.14 3.78 1 9 0 76.62 2.46 -1 9 0 84.84 2.69 -2 -9 0 82.13 3.03 2 -9 0 66.88 2.87 -2 -9 0 73.17 4.15 2 -9 0 66.26 3.48 2 9 0 74.75 2.47 -2 9 0 65.91 3.29 -3 -9 0 21.77 1.41 3 -9 0 23.17 4.17 -3 -9 0 21.97 2.43 3 -9 0 22.29 2.21 -3 9 0 21.95 3.68 4 -9 0 0.68 0.70 4 9 0 2.02 1.53 -4 -9 0 -0.55 1.67 4 -9 0 3.54 2.10 -4 9 0 1.45 0.99 5 -9 0 -0.60 0.86 5 9 0 1.66 1.45 -5 -9 0 -0.14 1.50 5 -9 0 2.05 2.11 -5 9 0 0.88 0.79 6 9 0 129.34 4.31 -6 -9 0 136.45 4.91 6 -9 0 129.70 4.35 -6 9 0 135.09 3.56 7 -9 0 47.34 2.33 7 9 0 45.53 2.99 -7 -9 0 45.34 3.13 7 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2.29 1.98 -20 -6 3 1.34 1.46 -20 6 3 0.63 1.07 19 -6 -3 3.99 2.32 19 6 -3 2.81 2.08 -19 6 3 6.13 1.50 18 -6 -3 3.36 2.27 18 6 -3 3.34 1.66 -18 -6 3 5.89 1.49 -18 6 3 6.59 1.61 17 -6 -3 22.48 5.85 17 6 -3 26.21 3.34 -17 -6 3 21.94 4.75 -17 6 3 23.97 2.17 16 -6 -3 5.19 3.60 16 6 -3 8.09 1.81 -16 -6 3 5.24 2.86 -16 6 3 7.76 1.39 15 -6 -3 3.07 1.25 15 6 -3 2.76 2.38 -15 -6 3 0.67 1.59 -15 6 3 5.34 1.71 14 -6 -3 9.71 1.27 14 6 -3 10.73 2.49 -14 -6 3 15.08 2.36 -14 6 3 10.35 1.47 13 -6 -3 44.85 2.34 13 6 -3 38.52 3.17 -13 -6 3 46.02 3.14 -13 6 3 46.17 2.59 12 -6 -3 15.20 3.95 12 6 -3 15.60 2.42 -12 -6 3 15.14 2.34 -12 6 3 15.60 1.64 11 -6 -3 50.98 2.61 11 6 -3 48.43 3.25 -11 -6 3 39.50 2.54 -11 6 3 50.22 2.62 10 -6 -3 1.13 1.10 10 6 -3 1.48 1.35 -10 -6 3 0.95 1.54 -10 6 3 0.68 0.91 9 -6 -3 61.83 2.39 9 6 -3 58.21 3.38 -9 -6 3 53.12 2.78 -9 6 3 52.85 2.38 8 -6 -3 26.86 1.53 8 6 -3 25.68 2.20 -8 -6 3 28.75 2.68 -8 6 3 29.05 1.87 7 -6 -3 24.98 1.38 7 6 -3 25.16 2.25 -7 -6 3 22.80 2.19 -7 6 3 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4 -6 3 28.78 1.90 -4 6 -3 27.05 1.68 5 -6 3 42.56 2.22 5 6 3 40.48 1.99 -5 -6 -3 39.17 2.27 5 -6 3 42.45 2.13 -5 6 -3 43.08 2.03 6 -6 3 37.89 2.28 6 6 3 32.68 2.00 -6 -6 -3 40.24 2.31 6 -6 3 40.05 2.03 -6 6 -3 38.52 1.47 7 -6 3 57.38 2.57 7 6 3 53.56 2.31 -7 -6 -3 50.63 3.76 7 -6 3 52.82 2.34 -7 6 -3 54.60 1.83 8 -6 3 3.82 1.31 8 6 3 4.47 1.06 -8 -6 -3 5.64 1.72 8 -6 3 4.08 1.39 9 -6 3 8.28 2.31 9 6 3 6.73 1.52 -9 -6 -3 8.05 2.33 9 -6 3 6.57 1.08 10 -6 3 111.98 5.81 10 6 3 112.60 4.57 -10 -6 -3 120.69 4.69 10 -6 3 121.65 4.65 11 -6 3 50.85 3.09 11 6 3 41.90 2.59 -11 -6 -3 49.33 4.01 11 -6 3 42.56 3.93 12 -6 3 141.20 4.58 12 6 3 130.42 4.37 -12 -6 -3 138.01 4.28 12 -6 3 130.83 3.58 13 -6 3 4.64 2.10 -13 -6 -3 5.42 1.49 13 -6 3 3.02 1.17 14 -6 3 3.10 2.01 14 6 3 1.77 1.14 -14 -6 -3 2.47 1.11 14 -6 3 0.28 0.75 15 -6 3 7.45 2.20 15 6 3 6.09 2.20 -15 -6 -3 3.31 1.61 16 -6 3 2.55 1.34 16 6 3 1.00 1.32 -16 -6 -3 1.05 1.17 17 -6 3 2.23 1.37 17 6 3 2.27 1.79 -17 -6 -3 1.20 1.11 18 -6 3 10.19 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3 4 122.55 2.60 -1 -3 -4 118.59 2.61 1 -3 4 126.46 3.63 -1 -3 -4 119.38 3.44 1 3 4 121.18 4.24 2 -3 4 65.97 2.53 2 3 4 62.25 1.84 -2 -3 -4 59.29 1.68 2 -3 4 63.37 1.92 -2 -3 -4 68.79 2.38 3 -3 4 9.04 1.26 3 3 4 9.95 0.70 3 -3 4 9.40 0.94 -3 -3 -4 10.70 1.04 4 -3 4 1.13 1.07 4 3 4 0.46 0.76 4 -3 4 0.57 0.63 -4 -3 -4 0.57 0.65 5 -3 4 58.28 3.32 5 3 4 60.99 2.03 -5 -3 -4 57.96 2.10 5 -3 4 58.61 1.69 6 -3 4 8.08 1.29 6 3 4 7.78 1.06 -6 -3 -4 7.40 1.96 6 -3 4 5.76 0.60 7 -3 4 27.03 1.87 7 3 4 31.85 3.68 -7 -3 -4 29.20 2.78 7 -3 4 26.35 1.04 8 -3 4 3.96 1.70 8 3 4 3.98 0.94 -8 -3 -4 2.75 0.80 8 -3 4 3.71 0.62 9 -3 4 93.11 4.08 9 3 4 91.79 3.62 -9 -3 -4 94.02 3.24 10 -3 4 375.64 6.72 10 3 4 381.65 6.34 -10 -3 -4 391.75 5.29 11 -3 4 5.60 1.42 11 3 4 5.61 1.87 -11 -3 -4 3.30 0.83 12 -3 4 5.74 1.89 12 3 4 7.05 2.10 -12 -3 -4 4.18 1.18 13 -3 4 3.50 2.23 13 3 4 1.60 1.28 -13 -3 -4 0.38 0.89 14 -3 4 18.93 2.45 14 3 4 15.27 3.61 -14 -3 -4 12.59 3.74 15 -3 4 42.05 2.90 15 3 4 45.30 3.39 -15 -3 -4 39.85 6.09 16 -3 4 2.40 1.32 16 3 4 0.78 1.13 17 -3 4 3.90 1.92 17 3 4 1.57 1.26 18 -3 4 2.49 1.62 18 3 4 1.12 1.34 19 -3 4 8.07 2.34 20 -3 4 5.44 1.55 20 3 4 1.45 1.47 21 -4 -4 1.30 1.32 21 4 -4 5.63 3.02 -21 -4 4 3.74 1.82 -21 4 4 0.50 1.08 20 -4 -4 5.84 1.93 20 4 -4 5.51 2.16 -20 -4 4 6.69 2.54 -20 4 4 6.39 1.66 19 -4 -4 -0.19 1.18 19 4 -4 0.73 1.92 -19 -4 4 1.29 1.38 -19 4 4 0.12 1.03 18 -4 -4 1.79 1.19 18 4 -4 3.90 1.97 -18 -4 4 4.41 1.16 -18 4 4 2.49 1.04 17 -4 -4 63.46 4.04 17 4 -4 59.30 4.70 -17 4 4 66.07 4.99 16 -4 -4 41.82 3.68 16 4 -4 45.57 4.11 -16 -4 4 40.44 3.10 -16 4 4 40.18 2.32 15 -4 -4 6.50 1.61 15 4 -4 10.37 2.75 -15 -4 4 6.74 2.55 -15 4 4 9.06 1.36 14 -4 -4 0.74 1.15 14 4 -4 0.02 1.81 -14 -4 4 1.81 1.05 -14 4 4 0.21 0.89 13 -4 -4 4.47 1.43 13 4 -4 5.28 2.69 -13 -4 4 2.65 1.58 -13 4 4 2.47 1.02 12 -4 -4 0.95 0.98 12 4 -4 2.02 1.75 -12 -4 4 0.76 1.06 -12 4 4 0.99 0.83 11 -4 -4 1.92 1.26 11 4 -4 3.20 1.81 -11 -4 4 1.18 1.37 -11 4 4 0.93 0.79 10 -4 -4 24.93 2.15 10 4 -4 25.17 2.57 -10 -4 4 22.16 1.88 -10 4 4 22.26 3.50 9 -4 -4 155.43 4.91 9 4 -4 145.05 5.85 -9 -4 4 141.22 5.02 -9 4 4 144.51 4.48 8 4 -4 104.59 3.94 -8 -4 4 93.45 3.11 -8 4 4 101.70 3.52 -8 -4 4 95.61 1.41 7 -4 -4 1.98 0.60 7 4 -4 -0.65 1.29 -7 -4 4 1.39 0.96 -7 4 4 1.99 0.73 -7 -4 4 1.50 0.45 -6 -4 4 31.79 5.83 6 -4 -4 24.84 1.48 -6 -4 4 25.77 1.85 -6 4 4 24.94 1.68 -5 -4 4 11.65 2.68 5 -4 -4 8.39 0.69 -5 -4 4 8.22 1.08 -5 4 4 9.97 2.40 -4 -4 4 22.32 2.37 4 -4 -4 19.19 1.11 -4 4 4 17.21 0.72 -4 -4 4 23.61 1.67 -4 4 4 20.24 1.24 -3 -4 4 80.22 3.33 3 -4 -4 75.73 1.42 3 -4 -4 78.28 1.47 -3 -4 4 79.24 2.79 -3 4 4 81.22 2.07 -2 -4 4 646.81 8.98 -2 -4 4 659.69 6.01 -2 4 4 647.40 8.09 -1 -4 4 231.25 4.33 -1 -4 4 230.23 3.90 1 4 -4 225.53 2.14 -1 4 4 229.62 4.12 1 4 -4 229.07 2.11 0 -4 4 60.14 2.45 0 -4 4 57.91 2.46 0 -4 -4 50.24 2.22 1 -4 4 18.03 1.75 1 -4 4 18.40 1.36 -1 -4 -4 18.05 1.34 1 4 4 18.68 2.48 2 -4 4 70.55 2.68 2 4 4 66.08 1.58 -2 -4 -4 61.51 1.51 2 -4 4 64.93 2.21 -2 -4 -4 66.97 2.50 3 -4 4 157.04 3.56 3 4 4 148.04 2.24 3 -4 4 147.49 3.90 -3 -4 -4 147.30 3.29 4 -4 4 8.82 1.63 4 4 4 8.10 0.74 4 -4 4 9.33 2.10 -4 -4 -4 12.22 2.39 5 -4 4 16.16 1.61 5 4 4 8.26 2.19 -5 -4 -4 7.31 1.13 5 -4 4 8.86 2.23 6 -4 4 169.00 4.05 6 4 4 170.74 3.35 -6 -4 -4 165.81 5.51 6 -4 4 170.72 3.07 7 -4 4 119.00 4.41 7 4 4 122.04 4.13 -7 -4 -4 125.85 4.85 7 -4 4 124.81 3.80 8 -4 4 129.62 4.10 8 4 4 130.39 3.30 -8 -4 -4 127.67 5.53 8 -4 4 125.06 3.80 9 -4 4 17.19 1.94 9 4 4 16.23 1.61 -9 -4 -4 16.23 3.43 9 -4 4 15.13 1.10 10 -4 4 3.17 1.51 -10 -4 -4 3.59 1.10 10 -4 4 1.57 0.78 11 -4 4 14.90 1.93 11 4 4 13.01 1.76 -11 -4 -4 13.28 1.44 11 -4 4 10.60 2.63 12 -4 4 40.69 7.89 12 4 4 41.42 2.98 -12 -4 -4 38.76 2.22 12 -4 4 32.85 1.85 13 -4 4 44.16 3.06 13 4 4 40.06 2.78 -13 -4 -4 37.22 2.00 14 -4 4 20.19 2.25 14 4 4 20.95 2.13 -14 -4 -4 17.40 1.80 15 -4 4 1.07 1.40 15 4 4 1.04 1.30 16 -4 4 2.32 1.24 16 4 4 2.97 1.81 17 -4 4 2.81 1.60 17 4 4 1.64 1.49 18 -4 4 1.03 1.34 18 4 4 3.23 1.89 19 -4 4 0.61 1.38 19 4 4 4.29 2.45 20 -5 -4 3.13 1.70 20 5 -4 2.11 2.05 -20 -5 4 2.24 1.29 -20 5 4 4.43 1.42 19 -5 -4 3.79 1.83 19 5 -4 3.24 1.90 -19 -5 4 1.95 1.62 -19 5 4 2.47 1.49 18 -5 -4 8.19 2.08 18 5 -4 4.92 1.91 -18 -5 4 5.86 2.12 17 -5 -4 0.50 0.98 17 5 -4 -0.95 1.63 -17 -5 4 2.18 1.52 -17 5 4 1.64 1.28 16 5 -4 14.46 2.86 -16 -5 4 17.34 3.14 -16 5 4 14.42 1.69 15 -5 -4 7.75 1.69 15 5 -4 8.28 2.54 -15 -5 4 7.68 3.30 -15 5 4 6.84 1.35 14 -5 -4 52.07 2.95 14 5 -4 54.50 3.82 -14 -5 4 47.16 6.69 -14 5 4 52.23 2.35 13 5 -4 1.83 1.71 -13 -5 4 0.84 1.52 -13 5 4 1.03 0.90 12 -5 -4 35.45 2.28 12 5 -4 30.71 2.77 -12 -5 4 35.40 2.77 -12 5 4 33.21 2.02 11 -5 -4 40.90 2.16 11 5 -4 40.50 3.23 -11 -5 4 38.62 2.56 -11 5 4 38.10 2.07 10 -5 -4 45.07 2.05 10 5 -4 41.89 2.90 -10 -5 4 45.66 2.46 -10 5 4 46.67 2.23 9 -5 -4 4.37 0.99 9 5 -4 3.97 1.83 -9 -5 4 3.05 1.08 -9 5 4 3.28 0.96 8 -5 -4 75.07 2.65 8 5 -4 62.41 3.50 -8 -5 4 73.74 3.85 -8 5 4 68.37 3.56 -8 -5 4 65.81 1.76 7 -5 -4 2.58 0.69 7 5 -4 2.49 1.18 -7 -5 4 4.99 1.39 -7 -5 4 1.96 0.32 -7 5 4 4.20 1.12 -7 -5 4 1.97 0.36 -6 -5 4 190.09 6.66 6 -5 -4 195.25 2.85 -6 -5 4 194.97 4.60 -6 5 4 186.67 4.87 -5 -5 4 73.82 4.16 5 -5 -4 73.41 1.65 -5 -5 4 73.08 2.98 -5 5 4 69.55 2.11 -4 -5 4 58.23 2.64 4 -5 -4 57.97 1.24 -4 5 4 56.18 1.25 -4 -5 4 63.89 2.50 -4 5 4 59.31 2.88 -3 -5 4 42.62 3.72 -3 -5 4 42.33 2.03 -3 5 4 39.11 1.87 -2 -5 4 16.20 3.54 -2 -5 4 20.54 1.73 -2 5 4 20.21 1.33 -1 -5 4 49.90 2.92 -1 -5 4 49.77 2.48 1 -5 -4 51.55 2.46 -1 5 4 51.08 1.98 1 5 -4 47.09 0.98 0 -5 4 120.34 3.16 0 -5 4 111.86 4.72 0 -5 -4 119.95 3.34 0 5 4 114.78 3.66 0 5 -4 120.31 1.55 1 -5 4 8.23 2.10 1 -5 4 9.89 1.03 -1 -5 -4 9.74 2.14 1 5 4 11.14 3.06 -1 5 -4 10.19 0.70 2 5 4 25.13 1.05 2 -5 4 29.23 2.34 2 5 4 26.72 0.72 2 -5 4 27.90 1.87 -2 -5 -4 30.91 1.78 2 5 4 30.44 1.84 3 -5 4 20.60 2.04 3 5 4 19.20 0.90 3 -5 4 21.23 1.38 -3 -5 -4 20.51 1.50 4 -5 4 6.56 1.64 4 5 4 3.71 0.65 4 -5 4 5.70 1.66 -4 -5 -4 9.35 2.11 5 -5 4 53.36 2.65 5 5 4 50.29 2.02 -5 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0.51 0.87 16 -6 -4 4.37 1.28 16 6 -4 4.45 1.83 -16 -6 4 2.24 1.55 -16 6 4 3.72 1.34 15 -6 -4 22.37 2.29 15 6 -4 14.93 2.86 -15 -6 4 21.75 5.78 -15 6 4 23.51 1.91 14 -6 -4 12.39 1.70 14 6 -4 10.61 2.42 -14 -6 4 10.94 2.26 -14 6 4 11.80 2.11 13 -6 -4 1.49 1.19 13 6 -4 1.82 1.54 -13 -6 4 0.96 1.51 -13 6 4 0.18 0.89 12 -6 -4 19.02 5.39 12 6 -4 22.42 2.63 -12 -6 4 19.39 2.00 -12 6 4 18.81 1.63 11 -6 -4 9.72 1.32 11 6 -4 11.84 2.48 -11 -6 4 7.85 1.99 -11 6 4 6.18 1.09 10 -6 -4 0.99 1.02 10 6 -4 0.87 1.33 -10 -6 4 2.26 2.02 -10 6 4 1.57 1.04 9 -6 -4 0.91 1.09 9 6 -4 1.41 1.35 -9 -6 4 1.42 1.34 -9 6 4 1.63 0.97 8 -6 -4 209.73 4.09 8 6 -4 219.04 6.21 -8 -6 4 218.02 5.78 -8 6 4 222.27 5.66 7 -6 -4 313.89 3.88 7 6 -4 329.58 7.26 -7 -6 4 297.66 5.89 -7 6 4 307.29 5.33 -6 -6 4 14.55 3.13 6 -6 -4 11.25 1.17 -6 -6 4 12.02 2.06 -6 6 4 10.96 3.90 -5 -6 4 99.38 3.98 5 -6 -4 96.07 2.69 -5 -6 4 84.93 3.70 -5 6 4 98.40 3.82 -4 -6 4 77.36 7.54 4 -6 -4 71.61 1.94 -4 6 4 63.86 1.84 -4 -6 4 71.38 3.46 -4 6 4 73.46 3.01 -3 -6 4 26.32 2.40 -3 -6 4 22.44 2.15 3 -6 -4 26.71 2.23 -3 6 4 25.21 5.22 -2 -6 4 53.68 3.40 -2 -6 4 58.48 5.13 2 -6 -4 60.41 3.05 -2 6 4 54.67 2.31 -1 -6 4 98.61 3.80 -1 -6 4 102.94 3.87 1 -6 -4 109.80 4.35 -1 6 4 100.61 3.40 1 6 -4 96.68 2.45 0 -6 4 54.66 4.04 0 -6 4 54.89 2.80 0 -6 -4 57.04 3.00 0 6 4 58.55 3.91 0 6 -4 56.51 1.71 1 -6 4 41.81 3.03 1 -6 4 50.33 4.01 -1 -6 -4 50.44 2.74 1 6 4 50.31 3.15 -1 6 -4 48.25 1.53 2 -6 4 9.25 2.68 2 6 4 6.77 0.39 2 -6 4 7.31 1.12 -2 -6 -4 5.90 1.27 2 6 4 8.50 2.87 -2 6 -4 6.50 1.05 3 -6 4 164.54 5.40 3 6 4 158.64 4.25 3 -6 4 157.49 4.97 -3 -6 -4 165.09 5.48 -3 6 -4 150.97 4.10 4 -6 4 2.58 1.07 4 6 4 4.26 0.74 4 -6 4 4.70 1.16 -4 -6 -4 4.08 1.25 -4 6 -4 4.21 0.57 5 -6 4 25.14 1.98 5 6 4 23.96 1.35 -5 -6 -4 23.76 1.89 6 -6 4 10.79 1.70 6 6 4 11.57 1.19 -6 -6 -4 11.70 1.54 6 -6 4 9.26 1.41 7 -6 4 23.51 2.12 7 6 4 15.90 1.39 -7 -6 -4 20.44 3.28 7 -6 4 19.88 1.45 8 -6 4 338.22 6.03 8 6 4 325.16 6.71 8 -6 4 333.59 4.94 9 -6 4 66.54 3.80 9 6 4 71.50 3.49 -9 -6 -4 72.39 3.66 9 -6 4 69.97 3.02 10 -6 4 2.91 1.23 10 6 4 2.95 1.30 -10 -6 -4 1.52 1.68 10 -6 4 0.28 0.73 11 -6 4 14.28 2.32 11 6 4 16.43 2.08 -11 -6 -4 15.09 3.05 11 -6 4 15.69 1.53 12 -6 4 10.35 2.35 12 6 4 7.58 1.61 -12 -6 -4 5.28 1.27 13 -6 4 0.55 1.01 13 6 4 0.49 0.99 -13 -6 -4 1.87 1.60 14 -6 4 1.59 1.53 14 6 4 3.38 1.87 -14 -6 -4 0.81 0.96 15 -6 4 3.39 1.96 15 6 4 1.19 1.11 -15 -6 -4 2.39 1.64 16 -6 4 16.96 2.31 16 6 4 14.08 2.16 -16 -6 -4 10.52 1.47 17 -6 4 5.70 2.11 18 -6 4 15.42 2.93 18 -7 -4 3.47 2.06 18 7 -4 6.69 2.05 -18 -7 4 9.05 2.43 -18 7 4 5.23 1.72 17 -7 -4 22.90 2.30 17 7 -4 20.94 3.37 -17 -7 4 16.89 6.72 -17 7 4 24.32 2.12 -16 -7 4 16.63 5.02 -16 7 4 23.36 2.06 15 -7 -4 3.39 1.17 15 7 -4 3.91 1.78 -15 -7 4 4.49 1.78 -15 7 4 2.16 1.37 14 -7 -4 2.71 1.08 14 7 -4 1.76 1.57 -14 -7 4 0.89 1.55 -14 7 4 1.01 0.99 13 -7 -4 5.30 1.07 13 7 -4 3.53 1.60 -13 -7 4 6.46 2.11 -13 7 4 4.65 1.73 12 -7 -4 13.48 1.53 12 7 -4 10.85 2.27 -12 -7 4 15.39 2.18 -12 7 4 12.96 1.55 11 -7 -4 0.52 0.61 11 7 -4 0.20 1.49 -11 -7 4 4.79 1.96 -11 7 4 2.69 1.17 10 -7 -4 63.52 2.24 10 7 -4 53.52 4.05 -10 -7 4 59.44 3.19 -10 7 4 54.50 2.41 9 7 -4 152.43 6.26 -9 -7 4 146.72 5.98 -9 7 4 149.49 7.05 8 7 -4 1.53 1.49 -8 -7 4 4.37 1.53 -8 7 4 4.47 1.40 7 -7 -4 0.96 0.66 7 7 -4 0.08 1.42 -7 -7 4 2.94 1.74 -7 7 4 1.12 0.65 -6 -7 4 2.01 1.39 6 -7 -4 0.85 0.51 -6 -7 4 0.82 1.84 -6 7 4 1.14 0.96 -5 -7 4 32.41 4.53 5 -7 -4 27.88 1.29 -5 -7 4 31.69 2.26 5 -7 -4 36.95 2.69 -5 7 4 33.32 3.20 -4 -7 4 2.19 1.37 -4 -7 4 1.17 1.28 4 -7 -4 0.94 1.43 -4 7 4 2.22 0.98 -3 -7 4 212.21 7.58 -3 -7 4 215.54 8.98 3 -7 -4 218.18 7.61 -3 7 4 223.61 4.22 -2 -7 4 74.44 5.17 -2 -7 4 71.80 3.27 2 -7 -4 74.26 3.53 -2 7 4 78.25 2.69 -1 -7 4 1.63 1.40 -1 -7 4 3.59 2.04 1 -7 -4 2.82 1.72 1 7 -4 0.93 0.42 -1 7 4 3.15 1.13 0 -7 4 321.62 10.66 0 -7 4 307.95 5.51 0 -7 -4 291.07 5.68 0 7 4 324.13 5.10 0 7 -4 310.04 3.05 1 -7 4 162.91 4.06 1 -7 4 155.35 3.92 -1 -7 -4 157.48 4.49 1 7 4 161.55 3.88 -1 7 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13 7 4 10.85 1.75 -13 -7 -4 7.84 1.45 14 -7 4 11.05 3.32 -14 -7 -4 13.88 2.00 15 -7 4 25.72 3.30 15 7 4 18.52 2.66 -15 -7 -4 17.33 1.95 16 -7 4 1.79 1.29 16 7 4 0.82 1.15 -16 -7 -4 0.56 0.95 17 -7 4 1.41 1.47 17 7 4 0.86 1.19 -17 7 -4 1.65 0.77 17 8 -4 2.43 1.98 -17 -8 4 1.33 1.55 -17 8 4 1.50 1.11 16 8 -4 1.96 2.02 -16 -8 4 3.14 2.10 -16 8 4 1.08 0.72 15 8 -4 1.99 1.75 -15 -8 4 2.81 2.21 -15 8 4 0.11 0.78 14 8 -4 -0.01 1.62 -14 -8 4 1.21 1.50 -14 8 4 1.59 1.24 13 8 -4 3.88 1.70 -13 -8 4 3.26 2.27 -13 8 4 2.92 1.57 12 8 -4 2.39 1.64 -12 -8 4 6.14 2.00 -12 8 4 5.03 2.01 11 8 -4 16.51 3.27 -11 -8 4 15.81 2.42 -11 8 4 11.53 2.95 10 8 -4 30.26 2.72 -10 -8 4 29.83 2.55 -10 8 4 25.21 7.05 9 8 -4 44.71 3.07 -9 -8 4 50.04 3.43 -9 8 4 44.74 3.01 8 8 -4 19.14 2.36 -8 -8 4 21.26 2.33 -8 8 4 24.13 6.51 7 8 -4 2.82 1.54 -7 -8 4 3.78 2.08 7 -8 -4 4.71 2.03 -7 8 4 2.68 1.03 -6 -8 4 59.76 3.08 -6 -8 4 58.56 3.42 6 -8 -4 69.65 4.20 -6 8 4 66.70 3.22 -5 -8 4 100.39 6.56 -5 -8 4 100.41 4.72 5 -8 -4 98.43 4.88 -5 8 4 98.56 3.82 -4 -8 4 134.64 6.01 -4 -8 4 151.29 4.98 4 -8 -4 138.13 5.28 -4 8 4 142.74 4.02 -3 -8 4 10.14 2.17 -3 -8 4 7.93 1.85 3 -8 -4 10.92 2.09 -3 8 4 11.65 3.24 -2 -8 4 5.93 1.55 -2 -8 4 4.73 1.67 2 -8 -4 4.83 2.29 -2 8 4 5.61 2.12 -1 -8 4 16.89 3.73 -1 -8 4 17.76 5.12 1 -8 -4 17.50 2.10 -1 8 4 20.14 5.51 0 -8 4 287.59 8.14 0 -8 4 275.09 6.70 0 -8 -4 296.55 7.55 0 8 4 287.25 6.57 1 -8 4 187.23 5.55 1 -8 4 167.17 4.77 -1 -8 -4 176.52 5.60 1 8 4 180.78 4.75 2 -8 4 16.18 4.58 2 -8 4 12.67 2.12 -2 -8 -4 16.02 2.10 2 8 4 19.11 2.10 -2 8 -4 13.89 1.20 3 -8 4 24.67 3.70 3 -8 4 21.01 2.02 -3 -8 -4 23.92 6.29 -3 8 -4 22.32 0.98 4 -8 4 63.45 6.08 4 -8 4 61.71 3.27 -4 -8 -4 63.97 5.33 -4 8 -4 63.44 2.32 5 -8 4 3.35 1.65 -5 -8 -4 3.72 1.80 5 -8 4 0.84 0.99 -5 8 -4 2.16 1.00 6 -8 4 1.07 1.22 -6 -8 -4 0.92 1.37 6 -8 4 0.36 0.97 -6 8 -4 0.71 0.71 7 -8 4 3.10 1.36 -7 -8 -4 4.70 1.93 7 -8 4 3.52 1.32 -7 8 -4 2.27 0.63 -8 -8 -4 1.06 1.79 8 -8 4 1.76 1.35 9 -8 4 15.97 2.33 -9 -8 -4 20.73 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5.02 -12 4 5 21.47 1.89 11 -4 -5 1.92 1.35 11 4 -5 0.25 1.66 -11 -4 5 0.99 0.81 -11 4 5 0.67 0.83 -11 -4 5 0.96 0.62 10 -4 -5 280.81 5.81 10 4 -5 275.25 7.33 -10 -4 5 287.31 6.72 -10 4 5 275.82 5.57 -10 -4 5 277.64 4.18 9 -4 -5 40.27 1.95 9 4 -5 35.78 3.04 -9 -4 5 42.06 2.49 -9 4 5 39.43 1.80 -9 -4 5 41.41 0.92 8 -4 -5 0.09 0.64 8 4 -5 0.23 1.21 -8 -4 5 0.32 1.07 -8 4 5 0.42 0.54 -8 -4 5 0.22 0.19 7 -4 -5 1.92 0.59 7 4 -5 2.50 1.33 -7 -4 5 2.16 1.27 -7 -4 5 0.95 0.29 -7 4 5 1.84 0.68 -6 -4 5 9.65 2.38 6 -4 -5 8.79 0.84 -6 -4 5 8.22 1.27 -6 4 5 8.95 2.72 -5 -4 5 176.41 4.06 5 -4 -5 169.30 2.35 -5 -4 5 160.54 6.19 -5 4 5 169.91 4.70 -4 -4 5 82.70 4.02 4 -4 -5 76.63 1.09 4 -4 -5 80.30 1.18 -4 -4 5 85.23 2.66 -4 4 5 87.40 2.41 -3 -4 5 8.76 2.80 -3 -4 5 8.23 1.08 -3 4 5 10.42 2.66 -2 -4 5 2.59 0.93 -2 -4 5 3.75 1.23 -2 4 5 3.49 1.03 -1 -4 5 140.73 6.75 -1 4 5 139.56 3.11 0 -4 5 282.48 5.57 0 -4 5 280.18 5.81 0 -4 -5 284.58 4.91 0 4 5 276.06 4.82 1 -4 5 0.25 0.90 1 -4 5 0.52 0.68 -1 -4 -5 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4.72 2.41 -11 -6 5 1.94 1.34 -11 6 5 1.13 0.63 10 -6 -5 0.85 0.60 10 6 -5 2.79 1.73 -10 -6 5 2.87 1.98 -10 6 5 1.05 0.94 9 -6 -5 29.66 1.56 9 6 -5 28.36 2.63 -9 -6 5 30.17 2.42 -9 6 5 30.53 2.19 8 -6 -5 1.84 0.83 8 6 -5 1.27 1.68 -8 -6 5 2.33 1.30 -8 6 5 0.82 1.21 -7 -6 5 90.00 3.23 7 -6 -5 99.85 2.18 -7 -6 5 102.58 3.83 -7 6 5 100.33 4.11 -6 -6 5 33.34 3.86 6 -6 -5 25.98 1.22 -6 -6 5 36.02 2.27 -6 6 5 29.23 2.12 -5 -6 5 3.38 1.85 5 -6 -5 0.60 0.18 -5 -6 5 1.57 1.26 -5 6 5 0.83 0.44 -4 -6 5 77.85 3.92 -4 -6 5 79.67 3.33 -4 6 5 78.80 3.39 -3 -6 5 94.11 6.86 -3 -6 5 92.35 3.37 3 -6 -5 94.10 4.00 -3 6 5 92.65 2.83 -2 -6 5 76.44 3.03 -2 -6 5 75.92 5.60 2 -6 -5 75.52 3.27 -2 6 5 72.96 2.40 -1 -6 5 237.33 5.95 -1 -6 5 231.75 4.44 1 -6 -5 244.07 5.36 -1 6 5 236.85 7.45 0 -6 5 132.01 3.84 0 -6 5 140.85 3.88 0 -6 -5 141.71 4.11 0 6 5 138.41 3.37 0 6 -5 129.76 1.42 1 -6 5 73.67 4.31 1 -6 5 68.88 2.62 -1 -6 -5 69.02 2.77 1 6 5 66.69 4.54 -1 6 -5 68.17 1.17 2 -6 5 24.82 5.96 2 -6 5 24.14 1.82 -2 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-9 3 11 2.68 1.08 8 3 -11 0.96 1.68 -8 -3 11 0.52 1.15 -8 3 11 1.25 0.78 7 3 -11 1.57 1.72 -7 -3 11 1.20 0.84 -7 3 11 1.41 0.84 -6 -3 11 4.08 1.40 -6 3 11 3.52 1.99 -5 -3 11 10.55 4.17 -4 -3 11 0.14 0.97 -3 -3 11 1.95 2.54 -2 -3 11 1.57 0.89 -1 -3 11 10.45 3.21 0 -3 11 21.36 6.75 1 -3 11 29.27 4.02 2 -3 11 40.46 4.48 3 -3 11 27.45 8.57 4 -3 11 11.76 4.73 5 -3 11 1.79 1.42 6 -3 11 0.65 1.05 7 -3 11 0.86 0.95 8 -3 11 0.37 0.71 12 4 -11 8.37 2.29 -12 -4 11 6.33 2.80 -12 4 11 5.30 3.66 11 4 -11 5.30 2.22 -11 -4 11 0.99 0.60 -11 4 11 0.83 0.93 -10 -4 11 1.60 1.42 -10 4 11 1.14 0.79 9 4 -11 2.54 1.36 -9 -4 11 1.63 0.81 -9 4 11 2.46 1.03 8 4 -11 -0.89 1.25 -8 -4 11 0.57 0.59 -8 4 11 0.53 0.77 -6 -4 11 4.35 3.21 -6 4 11 4.78 2.37 -5 -4 11 7.62 2.88 -5 4 11 8.47 4.12 -4 -4 11 13.53 4.33 -3 -4 11 1.37 1.18 -2 -4 11 6.89 3.08 -1 -4 11 2.11 1.26 0 -4 11 10.19 4.08 1 -4 11 9.25 2.61 2 -4 11 4.72 1.94 3 -4 11 3.00 1.22 4 -4 11 2.45 1.36 5 -4 11 1.23 0.64 6 -4 11 1.81 1.18 7 -4 11 1.86 1.33 10 5 -11 1.86 1.68 -10 -5 11 1.01 0.90 -10 5 11 3.08 0.92 -9 -5 11 0.52 0.75 -9 5 11 0.83 0.85 -8 -5 11 1.36 0.99 -8 5 11 0.73 0.80 -7 -5 11 0.32 0.48 -7 5 11 1.45 1.47 -6 -5 11 0.91 1.32 -6 5 11 0.96 0.61 -5 -5 11 6.84 3.88 -5 5 11 5.24 3.01 -4 -5 11 0.67 0.86 -3 -5 11 2.21 2.09 -2 -5 11 0.65 0.64 -1 -5 11 0.87 0.68 0 -5 11 0.79 0.78 1 -5 11 1.91 0.84 2 -5 11 7.79 2.46 3 -5 11 3.39 2.53 4 -5 11 1.77 1.11 5 -5 11 2.47 1.25 6 -5 11 0.64 0.81 8 6 -11 2.16 2.22 -8 6 11 1.12 1.06 -7 -6 11 2.94 1.73 -7 6 11 1.80 1.25 -6 -6 11 1.78 1.21 -6 6 11 1.16 1.36 -5 -6 11 1.48 0.79 5 -6 -11 -0.62 1.09 -5 6 11 0.79 1.02 -4 -6 11 1.68 0.92 -2 -6 11 3.43 1.70 -1 -6 11 1.95 1.69 0 -6 11 2.08 1.21 1 -6 11 0.98 0.58 2 -6 11 1.94 1.23 3 -6 11 1.83 1.75 4 -6 11 1.20 0.70 -4 -7 11 2.09 1.61 4 -7 -11 1.73 1.45 -4 7 11 0.05 1.03 -3 -7 11 0.90 0.90 -2 -7 11 2.41 2.04 -1 -7 11 2.79 1.91 10 1 -12 0.92 1.06 -10 -1 12 3.03 1.02 8 1 -12 0.31 0.90 5 1 -12 0.74 0.80 -4 -1 12 0.39 0.68 -3 -1 12 0.72 0.69 -2 -1 12 2.22 0.81 -1 -1 12 12.85 5.40 1 -1 12 -0.35 0.78 2 -1 12 0.91 0.61 3 -1 12 2.70 1.96 4 -1 12 2.15 1.35 10 2 -12 1.36 1.65 -10 2 12 2.56 1.77 9 2 -12 2.60 1.77 -9 2 12 0.69 0.73 8 2 -12 0.26 1.08 -8 2 12 0.40 0.53 -5 -2 12 2.14 1.40 -4 -2 12 2.07 1.59 -3 -2 12 0.14 0.92 -2 -2 12 1.35 0.97 -1 -2 12 2.43 1.39 0 -2 12 6.79 3.00 1 -2 12 5.24 3.27 3 -2 12 5.15 2.09 4 -2 12 0.55 0.89 5 -2 12 2.87 2.16 9 3 -12 6.46 2.04 8 3 -12 11.74 2.20 -8 3 12 9.07 6.19 7 3 -12 6.36 1.74 -7 3 12 7.10 4.31 -5 -3 12 0.83 0.84 -4 -3 12 2.05 1.17 -3 -3 12 4.65 2.28 -2 -3 12 1.86 0.99 2 -3 12 1.25 1.04 3 -3 12 1.74 1.33 4 -3 12 0.96 0.69 -7 4 12 4.57 3.58 -6 -4 12 6.72 3.26 -5 -4 12 2.07 1.35 -4 -4 12 0.83 0.72 -3 -4 12 1.17 1.58 -2 -4 12 1.62 1.52 -1 -4 12 0.48 1.03 0 -4 12 1.77 0.88 2 -4 12 3.15 2.04 -4 -5 12 1.47 0.91 -3 -5 12 2.74 1.28 -2 -5 12 1.06 0.96 -1 -5 12 4.42 3.53 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 87687 _shelx_res_file ; TITL I P 21/C R 0.07 CELL 0.71073 17.52300 10.40000 9.97600 90.00000 97.03200 90.00000 ZERR 4 0.00700 0.00400 0.00400 0.00000 0.00700 0.00000 LATT 1 SYMM -X, Y+ 0.50000, -Z+ 0.50000 SFAC C H N O UNIT 68 116 4 20 TEMP -100 PLAN 30 FMAP 2 L.S. 9 BOND $H BUMP DFIX 0.98 .02 C2 H2 C2' H2' CONF ACTA HTAB EQIV $1 -X, Y+1/2, -Z+3/2 HTAB O3 O2_$1 EQIV $2 -X, Y-1/2, -Z+3/2 HTAB O4 O1_$2 HTAB O5 O1 HTAB O5 O2 HTAB N1 O1 HTAB N1 O4 EQIV $3 -X, -Y+1, -Z+2 HTAB N1 O4_$3 EQIV $4 X, -Y+3/2, Z+1/2 HTAB N1 O5_$4 WGHT 0.064600 0.412200 FVAR 0.58230 O1 4 0.117731 0.776399 0.784292 11.00000 0.03568 0.02955 = 0.06467 0.00379 -0.00118 -0.00028 O2 4 0.134301 0.580015 0.710391 11.00000 0.04521 0.03607 = 0.07949 -0.00667 -0.00177 0.00242 C1 1 0.157678 0.677411 0.776664 11.00000 0.03320 0.02955 = 0.06250 0.00992 0.00098 -0.00217 PART 1 C2 1 0.233747 0.678153 0.875442 10.70000 0.03699 0.03679 = 0.04733 0.00535 -0.00003 0.00238 H2 2 0.218161 0.669895 0.966374 10.70000 -1.20000 C3 1 0.284403 0.562997 0.853723 10.70000 0.04815 0.04584 = 0.08419 0.00286 -0.01079 0.01322 AFIX 137 H3A 2 0.299246 0.566019 0.762201 10.70000 -1.50000 H3B 2 0.255931 0.483460 0.865244 10.70000 -1.50000 H3C 2 0.330651 0.565360 0.919739 10.70000 -1.50000 PART 2 AFIX 0 C2' 1 0.246394 0.673514 0.806063 10.30000 0.03788 0.04151 = 0.04610 0.00602 0.00721 0.00147 H2' 2 0.271121 0.616017 0.746434 10.30000 -1.20000 C3' 1 0.258499 0.589381 0.931222 10.30000 0.05427 0.06319 = 0.08748 0.02201 -0.00874 0.00142 AFIX 137 H3'1 2 0.311508 0.598863 0.974444 10.30000 -1.50000 H3'2 2 0.248967 0.499326 0.905505 10.30000 -1.50000 H3'3 2 0.222835 0.615644 0.994512 10.30000 -1.50000 PART 0 AFIX 0 C4 1 0.274355 0.807915 0.857546 11.00000 0.02931 0.04500 = 0.08382 0.00228 -0.01150 -0.00272 C5 1 0.260392 0.901019 0.948524 11.00000 0.03947 0.05783 = 0.06364 0.00587 0.00252 -0.00341 AFIX 43 H5 2 0.228085 0.881713 1.015680 11.00000 -1.20000 AFIX 0 C6 1 0.292080 1.021981 0.944964 11.00000 0.04156 0.05507 = 0.06670 -0.01084 0.00281 -0.00186 AFIX 43 H6 2 0.282534 1.082987 1.011809 11.00000 -1.20000 AFIX 0 C7 1 0.320409 0.840981 0.759858 11.00000 0.04801 0.06558 = 0.08588 -0.02943 0.00580 -0.00387 AFIX 43 H7 2 0.331513 0.778542 0.695488 11.00000 -1.20000 AFIX 0 C8 1 0.350654 0.963834 0.754330 11.00000 0.04933 0.08003 = 0.07766 -0.00670 0.01798 -0.01289 AFIX 43 H8 2 0.381301 0.984260 0.685023 11.00000 -1.20000 AFIX 0 C9 1 0.337320 1.057109 0.847026 11.00000 0.03681 0.04959 = 0.07635 -0.00156 -0.00070 -0.00671 C10 1 0.370788 1.190562 0.843297 11.00000 0.05699 0.05226 = 0.11864 0.00996 0.00074 -0.01100 AFIX 23 H10A 2 0.334447 1.252201 0.876780 11.00000 -1.20000 H10B 2 0.375456 1.213095 0.748227 11.00000 -1.20000 AFIX 0 C11 1 0.448613 1.206698 0.925650 11.00000 0.06392 0.05520 = 0.11190 -0.00709 0.01321 -0.01957 AFIX 13 H11 2 0.443761 1.175377 1.019001 11.00000 -1.20000 AFIX 0 C12 1 0.470611 1.348040 0.936911 11.00000 0.09728 0.06594 = 0.17708 -0.01618 0.01526 -0.03416 AFIX 137 H12A 2 0.471033 1.384200 0.846290 11.00000 -1.50000 H12B 2 0.521863 1.356527 0.987795 11.00000 -1.50000 H12C 2 0.433116 1.394503 0.983908 11.00000 -1.50000 AFIX 0 C13 1 0.511368 1.130305 0.874256 11.00000 0.05876 0.09374 = 0.14320 -0.00574 0.00583 -0.00917 AFIX 137 H13A 2 0.518618 1.159970 0.783435 11.00000 -1.50000 H13B 2 0.497286 1.039065 0.870848 11.00000 -1.50000 H13C 2 0.559279 1.141874 0.934844 11.00000 -1.50000 AFIX 0 O3 4 -0.151568 0.825738 0.844403 11.00000 0.06241 0.03232 = 0.05975 0.00120 0.01240 0.01200 H3 2 -0.153753 0.910266 0.825486 11.00000 0.08130 O4 4 -0.085441 0.447267 0.917007 11.00000 0.05415 0.02865 = 0.04115 0.00641 -0.00133 -0.00505 H4 2 -0.090314 0.387097 0.867941 11.00000 0.06551 O5 4 -0.008417 0.645375 0.588484 11.00000 0.04007 0.04173 = 0.03718 0.00802 0.00475 -0.00261 H5A 2 0.038739 0.626801 0.615828 11.00000 0.05867 N1 3 -0.015569 0.682831 0.870455 11.00000 0.03587 0.02431 = 0.03296 -0.00038 0.00145 -0.00028 H1A 2 0.023425 0.719881 0.825836 11.00000 0.04906 H1B 2 0.008005 0.612599 0.919257 11.00000 0.04431 H1C 2 -0.028989 0.745420 0.926951 11.00000 0.04650 C14 1 -0.130800 0.759033 0.730823 11.00000 0.04527 0.03241 = 0.04387 0.00233 -0.00207 0.00462 AFIX 23 H14A 2 -0.099737 0.815689 0.678961 11.00000 -1.20000 H14B 2 -0.177639 0.733494 0.671034 11.00000 -1.20000 AFIX 0 C15 1 -0.130773 0.551211 0.859009 11.00000 0.03865 0.03060 = 0.04065 0.00249 0.00433 -0.00457 AFIX 23 H15A 2 -0.150728 0.601161 0.931701 11.00000 -1.20000 H15B 2 -0.175327 0.516803 0.799142 11.00000 -1.20000 AFIX 0 C16 1 -0.057596 0.568737 0.658239 11.00000 0.04533 0.03098 = 0.03441 -0.00102 0.00413 -0.00646 AFIX 23 H16A 2 -0.030041 0.489512 0.690985 11.00000 -1.20000 H16B 2 -0.103025 0.543043 0.595004 11.00000 -1.20000 AFIX 0 C17 1 -0.084401 0.639733 0.777973 11.00000 0.03307 0.02580 = 0.03311 0.00053 -0.00062 -0.00169 HKLF 4 REM I P 21/C R 0.07 REM R1 = 0.0580 for 3391 Fo > 4sig(Fo) and 0.0738 for all 4096 data REM 260 parameters refined using 6 restraints END WGHT 0.0645 0.4122 REM Instructions for potential hydrogen bonds HTAB O3 O2_$1 HTAB O4 O1_$2 HTAB O5 O1 HTAB O5 O2 HTAB N1 O1 HTAB N1 O4_$3 HTAB N1 O5_$4 REM Highest difference peak 0.216, deepest hole -0.228, 1-sigma level 0.036 Q1 1 -0.1063 0.6882 0.7540 11.00000 0.05 0.22 Q2 1 -0.1034 0.5957 0.8217 11.00000 0.05 0.19 Q3 1 0.4445 1.3804 0.8128 11.00000 0.05 0.19 Q4 1 0.4316 1.2283 0.8153 11.00000 0.05 0.18 Q5 1 0.3463 1.2756 0.7948 11.00000 0.05 0.17 Q6 1 0.2829 0.8230 0.7903 11.00000 0.05 0.17 Q7 1 -0.0569 0.6599 0.8150 11.00000 0.05 0.17 Q8 1 -0.0707 0.6024 0.7253 11.00000 0.05 0.16 Q9 1 0.4183 1.4125 0.8671 11.00000 0.05 0.16 Q10 1 0.3718 1.0037 0.9154 11.00000 0.05 0.15 Q11 1 0.3905 0.9132 0.8380 11.00000 0.05 0.14 Q12 1 0.1981 0.6736 0.8199 11.00000 0.05 0.14 Q13 1 0.2764 0.8503 0.9149 11.00000 0.05 0.12 Q14 1 0.4032 1.1805 0.7087 11.00000 0.05 0.12 Q15 1 0.1174 0.5651 0.6578 11.00000 0.05 0.12 Q16 1 0.4013 1.4142 0.7580 11.00000 0.05 0.11 Q17 1 0.2555 0.7489 0.8723 11.00000 0.05 0.11 Q18 1 0.1576 0.5034 0.7482 11.00000 0.05 0.11 Q19 1 0.3442 0.7760 0.7709 11.00000 0.05 0.11 Q20 1 0.3481 0.6125 0.8654 11.00000 0.05 0.11 Q21 1 0.2635 1.1992 1.1524 11.00000 0.05 0.11 Q22 1 0.5007 1.3117 0.6994 11.00000 0.05 0.10 Q23 1 0.1016 0.7925 0.7250 11.00000 0.05 0.10 Q24 1 0.4877 1.1420 1.0197 11.00000 0.05 0.10 Q25 1 0.2565 0.6172 0.8460 11.00000 0.05 0.10 Q26 1 0.1532 0.6137 0.7079 11.00000 0.05 0.10 Q27 1 0.2672 0.9607 0.9305 11.00000 0.05 0.10 Q28 1 -0.1219 0.4370 1.0544 11.00000 0.05 0.09 Q29 1 0.4480 1.1339 1.0541 11.00000 0.05 0.09 Q30 1 0.3485 1.2201 0.9755 11.00000 0.05 0.09 ; _shelx_res_checksum 23270 _shelxl_version_number 2014/6 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_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 _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.11773(7) 0.77640(11) 0.78429(13) 0.0439(3) Uani d 1 . . O O2 0.13430(7) 0.58002(12) 0.71039(15) 0.0544(4) Uani d 1 . . C C1 0.15768(10) 0.67741(15) 0.7767(2) 0.0422(4) Uani d 1 . . C C2 0.23375(17) 0.6782(3) 0.8754(4) 0.0408(6) Uani d 0.7 A 1 H H2 0.2182(17) 0.670(3) 0.966(2) 0.049 Uiso d 0.7 B 1 C C3 0.28440(19) 0.5630(3) 0.8537(4) 0.0610(9) Uani d 0.7 A 1 H H3A 0.2992 0.5660 0.7622 0.091 Uiso calc 0.7 A 1 H H3B 0.2559 0.4835 0.8652 0.091 Uiso calc 0.7 A 1 H H3C 0.3307 0.5654 0.9197 0.091 Uiso calc 0.7 A 1 C C2' 0.2464(4) 0.6735(7) 0.8061(9) 0.0417(16) Uani d 0.3 A 2 H H2' 0.271(3) 0.616(2) 0.746(6) 0.050 Uiso d 0.3 C 2 C C3' 0.2585(5) 0.5894(9) 0.9312(11) 0.070(2) Uani d 0.3 A 2 H H3'1 0.3115 0.5989 0.9744 0.105 Uiso calc 0.3 A 2 H H3'2 0.2490 0.4993 0.9055 0.105 Uiso calc 0.3 A 2 H H3'3 0.2228 0.6156 0.9945 0.105 Uiso calc 0.3 A 2 C C4 0.27435(10) 0.80792(18) 0.8575(2) 0.0542(5) Uani d 1 . . C C5 0.26039(11) 0.9010(2) 0.9485(2) 0.0540(5) Uani d 1 . . H H5 0.2281 0.8817 1.0157 0.065 Uiso calc 1 . . C C6 0.29208(11) 1.0220(2) 0.9450(2) 0.0548(5) Uani d 1 . . H H6 0.2825 1.0830 1.0118 0.066 Uiso calc 1 . . C C7 0.32041(12) 0.8410(2) 0.7599(3) 0.0667(6) Uani d 1 . . H H7 0.3315 0.7785 0.6955 0.080 Uiso calc 1 . . C C8 0.35065(13) 0.9638(2) 0.7543(3) 0.0682(6) Uani d 1 . . H H8 0.3813 0.9843 0.6850 0.082 Uiso calc 1 . . C C9 0.33732(11) 1.05711(19) 0.8470(2) 0.0549(5) Uani d 1 . . C C10 0.37079(14) 1.1906(2) 0.8433(3) 0.0768(7) Uani d 1 . . H H10A 0.3344 1.2522 0.8768 0.092 Uiso calc 1 . . H H10B 0.3755 1.2131 0.7482 0.092 Uiso calc 1 . . C C11 0.44861(14) 1.2067(2) 0.9256(3) 0.0768(7) Uani d 1 . . H H11 0.4438 1.1754 1.0190 0.092 Uiso calc 1 . . C C12 0.4706(2) 1.3480(3) 0.9369(4) 0.1136(12) Uani d 1 . . H H12A 0.4710 1.3842 0.8463 0.170 Uiso calc 1 . . H H12B 0.5219 1.3565 0.9878 0.170 Uiso calc 1 . . H H12C 0.4331 1.3945 0.9839 0.170 Uiso calc 1 . . C C13 0.51137(16) 1.1303(3) 0.8743(4) 0.0991(10) Uani d 1 . . H H13A 0.5186 1.1600 0.7834 0.149 Uiso calc 1 . . H H13B 0.4973 1.0391 0.8708 0.149 Uiso calc 1 . . H H13C 0.5593 1.1419 0.9348 0.149 Uiso calc 1 . . O O3 -0.15157(8) 0.82574(12) 0.84440(14) 0.0511(4) Uani d 1 . . H H3 -0.1538(14) 0.910(2) 0.825(2) 0.081(8) Uiso d 1 . . O O4 -0.08544(7) 0.44727(12) 0.91701(13) 0.0419(3) Uani d 1 . . H H4 -0.0903(12) 0.387(2) 0.868(2) 0.066(7) Uiso d 1 . . O O5 -0.00842(7) 0.64538(11) 0.58848(12) 0.0397(3) Uani d 1 . . H H5A 0.0387(12) 0.6268(18) 0.616(2) 0.059(6) Uiso d 1 . . N N1 -0.01557(8) 0.68283(13) 0.87045(14) 0.0313(3) Uani d 1 . . H H1A 0.0234(12) 0.7199(19) 0.826(2) 0.049(5) Uiso d 1 . . H H1B 0.0080(11) 0.6126(19) 0.9193(19) 0.044(5) Uiso d 1 . . H H1C -0.0290(11) 0.745(2) 0.927(2) 0.046(5) Uiso d 1 . . C C14 -0.13080(10) 0.75903(15) 0.73082(18) 0.0411(4) Uani d 1 . . H H14A -0.0997 0.8157 0.6790 0.049 Uiso calc 1 . . H H14B -0.1776 0.7335 0.6710 0.049 Uiso calc 1 . . C C15 -0.13077(9) 0.55121(15) 0.85901(17) 0.0367(4) Uani d 1 . . H H15A -0.1507 0.6012 0.9317 0.044 Uiso calc 1 . . H H15B -0.1753 0.5168 0.7991 0.044 Uiso calc 1 . . C C16 -0.05760(10) 0.56874(15) 0.65824(17) 0.0370(4) Uani d 1 . . H H16A -0.0300 0.4895 0.6910 0.044 Uiso calc 1 . . H H16B -0.1030 0.5430 0.5950 0.044 Uiso calc 1 . . C C17 -0.08440(9) 0.63973(14) 0.77797(16) 0.0310(3) Uani d 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 0.0357(6) 0.0295(6) 0.0647(8) -0.0003(5) -0.0012(6) 0.0038(6) O2 0.0452(7) 0.0361(7) 0.0795(10) 0.0024(5) -0.0018(7) -0.0067(6) C1 0.0332(8) 0.0296(8) 0.0625(12) -0.0022(6) 0.0010(8) 0.0099(8) C2 0.0370(15) 0.0368(14) 0.047(2) 0.0024(11) 0.0000(14) 0.0053(15) C3 0.0481(18) 0.0458(16) 0.084(3) 0.0132(13) -0.0108(17) 0.0029(18) C2' 0.038(3) 0.042(3) 0.046(4) 0.001(2) 0.007(3) 0.006(3) C3' 0.054(5) 0.063(5) 0.087(7) 0.001(4) -0.009(4) 0.022(5) C4 0.0293(8) 0.0450(10) 0.0838(15) -0.0027(7) -0.0115(9) 0.0023(10) C5 0.0395(10) 0.0578(12) 0.0636(13) -0.0034(8) 0.0025(9) 0.0059(10) C6 0.0416(10) 0.0551(11) 0.0667(14) -0.0019(9) 0.0028(9) -0.0108(10) C7 0.0480(12) 0.0656(13) 0.0859(17) -0.0039(10) 0.0058(11) -0.0294(12) C8 0.0493(12) 0.0800(16) 0.0777(16) -0.0129(11) 0.0180(11) -0.0067(13) C9 0.0368(9) 0.0496(11) 0.0763(15) -0.0067(8) -0.0007(9) -0.0016(10) C10 0.0570(13) 0.0523(13) 0.119(2) -0.0110(10) 0.0007(13) 0.0100(13) C11 0.0639(15) 0.0552(13) 0.112(2) -0.0196(11) 0.0132(14) -0.0071(13) C12 0.097(2) 0.0659(17) 0.177(4) -0.0342(16) 0.015(2) -0.016(2) C13 0.0588(16) 0.094(2) 0.143(3) -0.0092(14) 0.0058(17) -0.006(2) O3 0.0624(9) 0.0323(6) 0.0598(9) 0.0120(6) 0.0124(7) 0.0012(6) O4 0.0542(8) 0.0286(6) 0.0411(7) -0.0050(5) -0.0013(6) 0.0064(5) O5 0.0401(7) 0.0417(6) 0.0372(7) -0.0026(5) 0.0048(5) 0.0080(5) N1 0.0359(7) 0.0243(6) 0.0330(8) -0.0003(5) 0.0014(6) -0.0004(6) C14 0.0453(10) 0.0324(8) 0.0439(10) 0.0046(7) -0.0021(8) 0.0023(7) C15 0.0387(8) 0.0306(8) 0.0406(10) -0.0046(6) 0.0043(7) 0.0025(7) C16 0.0453(9) 0.0310(8) 0.0344(9) -0.0065(7) 0.0041(7) -0.0010(7) C17 0.0331(8) 0.0258(7) 0.0331(8) -0.0017(6) -0.0006(6) 0.0005(6) 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' N N 0.0061 0.0033 '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 O2 C1 O1 123.26(16) O2 C1 C2' 109.6(3) O1 C1 C2' 124.5(3) O2 C1 C2 122.54(17) O1 C1 C2 113.51(18) C3 C2 C4 112.7(3) C3 C2 C1 112.0(3) C4 C2 C1 107.6(2) C3 C2 H2 107.2(18) C4 C2 H2 111.5(17) C1 C2 H2 105.7(18) C2 C3 H3A 109.5 C2 C3 H3B 109.5 H3A C3 H3B 109.5 C2 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C3' C2' C1 101.9(6) C3' C2' C4 103.9(7) C1 C2' C4 108.0(4) C3' C2' H2' 97(3) C1 C2' H2' 114(4) C4 C2' H2' 127.3(18) C2' C3' H3'1 109.5 C2' C3' H3'2 109.5 H3'1 C3' H3'2 109.5 C2' C3' H3'3 109.5 H3'1 C3' H3'3 109.5 H3'2 C3' H3'3 109.5 C5 C4 C7 117.28(18) C5 C4 C2 114.7(2) C7 C4 C2 128.0(2) C5 C4 C2' 141.6(3) C7 C4 C2' 100.3(3) C4 C5 C6 121.6(2) C4 C5 H5 119.2 C6 C5 H5 119.2 C5 C6 C9 121.9(2) C5 C6 H6 119.1 C9 C6 H6 119.1 C4 C7 C8 121.1(2) C4 C7 H7 119.5 C8 C7 H7 119.5 C9 C8 C7 121.6(2) C9 C8 H8 119.2 C7 C8 H8 119.2 C8 C9 C6 116.57(19) C8 C9 C10 122.1(2) C6 C9 C10 121.3(2) C9 C10 C11 114.6(2) C9 C10 H10A 108.6 C11 C10 H10A 108.6 C9 C10 H10B 108.6 C11 C10 H10B 108.6 H10A C10 H10B 107.6 C13 C11 C10 114.0(2) C13 C11 C12 110.4(2) C10 C11 C12 110.5(2) C13 C11 H11 107.2 C10 C11 H11 107.2 C12 C11 H11 107.2 C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C11 C13 H13A 109.5 C11 C13 H13B 109.5 H13A C13 H13B 109.5 C11 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C14 O3 H3 108.7(12) C15 O4 H4 109.7(13) C16 O5 H5A 109.7(11) C17 N1 H1A 114.1(12) C17 N1 H1B 110.8(12) H1A N1 H1B 105.3(16) C17 N1 H1C 110.3(13) H1A N1 H1C 104.9(17) H1B N1 H1C 111.3(17) O3 C14 C17 109.37(14) O3 C14 H14A 109.8 C17 C14 H14A 109.8 O3 C14 H14B 109.8 C17 C14 H14B 109.8 H14A C14 H14B 108.2 O4 C15 C17 111.56(13) O4 C15 H15A 109.3 C17 C15 H15A 109.3 O4 C15 H15B 109.3 C17 C15 H15B 109.3 H15A C15 H15B 108.0 O5 C16 C17 112.09(12) O5 C16 H16A 109.2 C17 C16 H16A 109.2 O5 C16 H16B 109.2 C17 C16 H16B 109.2 H16A C16 H16B 107.9 N1 C17 C15 107.22(13) N1 C17 C14 107.80(12) C15 C17 C14 110.87(13) N1 C17 C16 109.01(13) C15 C17 C16 110.98(12) C14 C17 C16 110.83(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.252(2) O2 C1 1.251(2) C1 C2' 1.547(7) C1 C2 1.558(4) C2 C3 1.522(4) C2 C4 1.546(4) C2 H2 0.983(17) C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C2' C3' 1.518(11) C2' C4 1.548(8) C2' H2' 0.98(2) C3' H3'1 0.9800 C3' H3'2 0.9800 C3' H3'3 0.9800 C4 C5 1.369(3) C4 C7 1.383(3) C5 C6 1.377(3) C5 H5 0.9500 C6 C9 1.381(3) C6 H6 0.9500 C7 C8 1.387(3) C7 H7 0.9500 C8 C9 1.380(3) C8 H8 0.9500 C9 C10 1.509(3) C10 C11 1.513(4) C10 H10A 0.9900 C10 H10B 0.9900 C11 C13 1.497(4) C11 C12 1.520(3) C11 H11 1.0000 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 O3 C14 1.414(2) O3 H3 0.90(3) O4 C15 1.422(2) O4 H4 0.79(2) O5 C16 1.4174(19) O5 H5A 0.86(2) N1 C17 1.495(2) N1 H1A 0.94(2) N1 H1B 0.94(2) N1 H1C 0.91(2) C14 C17 1.526(2) C14 H14A 0.9900 C14 H14B 0.9900 C15 C17 1.524(2) C15 H15A 0.9900 C15 H15B 0.9900 C16 C17 1.526(2) C16 H16A 0.9900 C16 H16B 0.9900 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 O3 H3 O2 2_556 0.90(3) 1.84(3) 2.725(2) 167(2) O4 H4 O1 2_546 0.79(2) 1.92(3) 2.689(2) 163.7(18) O5 H5A O1 . 0.86(2) 2.57(2) 3.0825(19) 119.5(17) O5 H5A O2 . 0.86(2) 1.88(2) 2.730(2) 168.1(18) N1 H1A O1 . 0.94(2) 1.85(2) 2.763(2) 162.9(18) N1 H1B O4 3_567 0.94(2) 2.09(2) 2.9224(19) 146.7(16) N1 H1C O5 4_576 0.91(2) 1.97(2) 2.806(2) 152.1(18) 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 O2 C1 C2 C3 14.9(4) O1 C1 C2 C3 -174.3(3) O2 C1 C2 C4 139.3(2) O1 C1 C2 C4 -50.0(3) O2 C1 C2' C3' -83.9(6) O1 C1 C2' C3' 114.1(6) O2 C1 C2' C4 167.0(4) O1 C1 C2' C4 5.0(7) C3 C2 C4 C5 -140.2(3) C1 C2 C4 C5 95.8(3) C3 C2 C4 C7 41.7(4) C1 C2 C4 C7 -82.2(3) C3' C2' C4 C5 -59.3(7) C1 C2' C4 C5 48.5(8) C3' C2' C4 C7 132.5(5) C1 C2' C4 C7 -119.7(4) C7 C4 C5 C6 -1.3(3) C2 C4 C5 C6 -179.6(2) C2' C4 C5 C6 -168.2(5) C4 C5 C6 C9 2.3(3) C5 C4 C7 C8 -0.4(3) C2 C4 C7 C8 177.6(2) C2' C4 C7 C8 171.4(3) C4 C7 C8 C9 1.2(4) C7 C8 C9 C6 -0.3(3) C7 C8 C9 C10 179.1(2) C5 C6 C9 C8 -1.4(3) C5 C6 C9 C10 179.2(2) C8 C9 C10 C11 -90.4(3) C6 C9 C10 C11 89.0(3) C9 C10 C11 C13 65.5(3) C9 C10 C11 C12 -169.5(3) O4 C15 C17 N1 -55.72(17) O4 C15 C17 C14 -173.15(14) O4 C15 C17 C16 63.24(18) O3 C14 C17 N1 -58.01(17) O3 C14 C17 C15 59.06(18) O3 C14 C17 C16 -177.23(13) O5 C16 C17 N1 -56.68(17) O5 C16 C17 C15 -174.56(13) O5 C16 C17 C14 61.80(18) _cod_database_fobs_code 2240916