#------------------------------------------------------------------------------ #$Date: 2017-04-06 11:28:47 +0300 (Thu, 06 Apr 2017) $ #$Revision: 195238 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/10/2311084.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_2311084 loop_ _publ_author_name 'van Genderen, E.' 'Clabbers, M. T. B.' 'Das, P. P.' 'Stewart, A.' 'Nederlof, I.' 'Barentsen, K. C.' 'Portillo, Q.' 'Pannu, N. S.' 'Nicolopoulos, S.' 'Gruene, T.' 'Abrahams, J. P.' _publ_section_title ; Ab initio structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section A' _journal_page_first 236 _journal_page_last 242 _journal_paper_doi 10.1107/S2053273315022500 _journal_volume 72 _journal_year 2016 _chemical_formula_sum 'C6 H5 N O2' _chemical_formula_weight 123.12 _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 geom _audit_creation_method SHELXL-2014/8 _cell_angle_alpha 90 _cell_angle_beta 114.45(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.41(3) _cell_length_b 11.692(2) _cell_length_c 7.377(11) _cell_measurement_temperature 293(2) _cell_volume 582(3) _computing_structure_refinement 'SHELXL-2014/8 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.392 _diffrn_measured_fraction_theta_max 0.390 _diffrn_measurement_device_type ; Philips EM30 LaB6 Electron Microscope with Timepix Detector ; _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.2703 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 1337 _diffrn_reflns_theta_full 0.862 _diffrn_reflns_theta_max 0.953 _diffrn_reflns_theta_min 0.123 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type empirical _exptl_crystal_density_diffrn 1.406 _exptl_crystal_description 'data merged from 2 nanocrystals' _exptl_crystal_F_000 256 _refine_diff_density_max 0.550 _refine_diff_density_min -0.816 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.216 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 552 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 2.216 _refine_ls_R_factor_all 0.4019 _refine_ls_R_factor_gt 0.3371 _refine_ls_shift/su_max 1.088 _refine_ls_shift/su_mean 0.028 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.6328 _refine_ls_wR_factor_ref 0.6754 _reflns_number_gt 303 _reflns_number_total 552 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file td5026sup1.cif _cod_data_source_block nicotinic_acid_2x-merged _cod_depositor_comments ; Adding full bibliography for 2311081--2311085.cif. 2017-03-30 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C H0.83 N0.17 O0.33' _cod_original_formula_weight 20.52 _cod_original_formula_units_Z 24 _cod_original_cell_volume 581(2) _cod_database_code 2311084 _cod_database_fobs_code 2311084 _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 ; 1 -6 -8 3.90 7.55 1 -6 -8 -14.38 8.12 1 -7 -8 7.35 8.34 1 -7 -8 -1.82 8.20 2 -8 -8 4.78 9.36 1 -5 -7 5.96 8.50 1 -6 -7 15.98 8.92 1 -6 -7 -5.28 8.86 1 -7 -7 -4.47 8.33 1 -7 -7 -8.71 8.75 2 -7 -7 18.94 9.52 1 -8 -7 -4.13 8.88 1 -8 -7 -4.26 9.09 2 -8 -7 2.19 9.19 2 -8 -7 17.90 9.67 1 -9 -7 28.66 10.77 1 -9 -7 25.35 11.81 2 -9 -7 41.41 11.04 2 -9 -7 25.34 10.39 1 -10 -7 12.71 10.72 1 -10 -7 5.11 11.09 2 -10 -7 14.33 10.04 2 -10 -7 25.93 10.41 3 -10 -7 -0.71 8.79 3 -10 -7 -4.21 8.40 1 -2 -6 -17.04 37.47 1 -5 -6 -5.38 9.98 1 -5 -6 -1.91 10.56 1 -6 -6 1.87 10.02 1 -6 -6 -0.69 10.12 1 -7 -6 -7.63 9.45 1 -7 -6 -5.74 9.77 2 -7 -6 1.17 9.72 1 -8 -6 10.85 10.06 1 -8 -6 31.71 10.90 2 -8 -6 38.80 11.19 2 -8 -6 29.76 10.77 1 -9 -6 20.95 11.13 1 -9 -6 40.51 11.90 2 -9 -6 12.68 9.34 2 -9 -6 1.92 9.28 3 -9 -6 2.05 9.33 1 -10 -6 59.19 13.39 1 -10 -6 38.06 12.46 2 -10 -6 11.32 9.63 2 -10 -6 16.13 10.29 3 -10 -6 -2.09 9.05 3 -10 -6 25.07 9.66 1 -11 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14.94 9.83 4 -11 -5 17.24 9.92 1 -12 -5 1.52 10.57 1 -12 -5 25.49 10.32 2 -12 -5 -9.33 9.56 2 -12 -5 40.99 11.12 3 -12 -5 19.60 10.27 3 -12 -5 -1.37 9.82 4 -12 -5 1.76 9.51 4 -12 -5 9.27 9.68 1 -13 -5 1.45 10.44 1 -13 -5 -6.67 7.36 2 -13 -5 0.80 10.14 2 -13 -5 16.01 10.84 3 -13 -5 -1.73 10.33 3 -13 -5 17.03 10.41 1 -3 -4 21.93 35.13 1 -3 -4 7.11 43.25 1 -4 -4 64.57 37.28 1 -4 -4 99.10 49.75 1 -4 -4 46.38 11.86 1 -4 -4 35.18 11.65 1 -5 -4 197.88 50.45 1 -5 -4 260.80 63.82 1 -5 -4 5.17 10.47 1 -5 -4 9.53 10.90 2 -5 -4 18.29 50.62 2 -5 -4 27.31 49.83 1 -6 -4 43.03 40.46 1 -6 -4 234.14 59.44 1 -6 -4 23.43 11.04 1 -6 -4 19.43 11.16 2 -6 -4 55.27 47.31 2 -6 -4 69.36 54.42 2 -6 -4 -36.85 9.09 1 -7 -4 36.66 42.84 1 -7 -4 36.73 49.22 1 -7 -4 -2.07 11.70 1 -7 -4 23.86 12.64 2 -7 -4 0.01 43.09 2 -7 -4 11.15 49.20 2 -7 -4 139.08 20.34 2 -7 -4 226.63 25.28 3 -7 -4 -26.61 67.49 1 -8 -4 73.90 16.05 1 -8 -4 118.81 17.24 2 -8 -4 88.28 17.32 2 -8 -4 74.82 16.14 1 -9 -4 26.70 14.05 1 -9 -4 -48.88 10.26 2 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63.68 2 -5 -3 51.91 70.46 1 -6 -3 83.51 47.97 1 -6 -3 120.10 57.14 1 -6 -3 -2.48 10.17 1 -6 -3 36.67 10.34 2 -6 -3 122.69 56.47 2 -6 -3 137.14 60.99 2 -6 -3 348.67 34.30 2 -6 -3 371.21 36.42 1 -7 -3 147.16 52.85 1 -7 -3 173.57 59.43 1 -7 -3 133.43 18.08 1 -7 -3 114.12 16.88 2 -7 -3 12.24 47.45 2 -7 -3 45.36 53.61 2 -7 -3 50.25 13.05 2 -7 -3 42.85 12.91 3 -7 -3 -14.68 67.82 1 -8 -3 240.36 65.88 1 -8 -3 213.39 66.75 1 -8 -3 -2.01 12.17 1 -8 -3 -9.18 12.27 2 -8 -3 55.96 47.22 2 -8 -3 72.88 53.40 2 -8 -3 175.83 22.78 2 -8 -3 163.07 21.57 3 -8 -3 8.47 56.42 3 -8 -3 10.00 55.12 3 -8 -3 17.85 12.54 1 -9 -3 896.52 80.85 1 -9 -3 716.41 66.39 2 -9 -3 42.72 14.79 2 -9 -3 56.51 15.21 3 -9 -3 -51.00 10.76 3 -9 -3 30.39 13.60 1 -10 -3 1242.20 109.68 1 -10 -3 1321.35 116.39 2 -10 -3 40.51 13.43 2 -10 -3 45.17 13.50 3 -10 -3 65.84 13.15 3 -10 -3 31.99 12.75 4 -10 -3 67.63 14.00 1 -11 -3 99.18 17.88 1 -11 -3 101.44 17.59 2 -11 -3 49.58 11.76 2 -11 -3 22.32 11.36 3 -11 -3 12.33 11.16 3 -11 -3 12.24 9.48 4 -11 -3 75.71 14.51 4 -11 -3 51.25 12.03 1 -12 -3 34.61 12.01 1 -12 -3 26.75 11.31 2 -12 -3 -41.64 8.18 2 -12 -3 9.23 9.93 3 -12 -3 5.39 10.09 3 -12 -3 7.69 9.78 4 -12 -3 28.57 11.06 4 -12 -3 -0.01 9.14 1 -13 -3 20.20 11.53 1 -13 -3 20.29 11.22 2 -13 -3 26.06 9.85 2 -13 -3 27.33 10.77 3 -13 -3 11.92 10.19 3 -13 -3 -3.60 8.78 4 -13 -3 -6.39 9.28 4 -13 -3 4.98 9.05 5 -13 -3 1.61 10.31 5 -13 -3 -0.81 8.62 1 -14 -3 61.89 12.53 1 -14 -3 22.02 10.94 2 -14 -3 43.97 12.42 2 -14 -3 31.18 11.29 3 -14 -3 26.73 11.25 3 -14 -3 15.57 10.39 1 -3 -2 107.34 52.22 1 -3 -2 76.47 51.61 1 -4 -2 143.77 56.23 1 -4 -2 252.07 67.67 1 -4 -2 95.71 15.81 1 -4 -2 114.53 16.42 1 -5 -2 1079.05 155.80 1 -5 -2 1230.09 175.99 1 -5 -2 776.98 68.57 1 -5 -2 703.73 62.63 2 -5 -2 24.75 73.76 2 -5 -2 32.27 75.80 1 -6 -2 236.97 64.86 1 -6 -2 318.30 77.32 1 -6 -2 43.43 12.98 1 -6 -2 54.48 13.52 2 -6 -2 117.52 58.70 2 -6 -2 107.34 61.18 2 -6 -2 493.49 45.75 2 -6 -2 475.07 44.28 1 -7 -2 89.98 51.26 1 -7 -2 124.95 56.38 1 -7 -2 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10.28 10.05 3 -12 -2 9.51 9.43 4 -12 -2 6.30 9.09 4 -12 -2 -4.37 8.08 5 -12 -2 -12.04 7.98 1 -13 -2 34.51 11.88 1 -13 -2 10.96 9.76 2 -13 -2 159.84 21.69 2 -13 -2 141.34 19.89 3 -13 -2 66.60 14.26 3 -13 -2 39.26 12.01 4 -13 -2 10.48 9.45 4 -13 -2 7.45 8.84 5 -13 -2 5.68 9.66 5 -13 -2 10.12 9.02 1 -14 -2 7.77 11.15 1 -14 -2 8.84 10.22 2 -14 -2 158.87 21.90 2 -14 -2 202.89 25.08 3 -14 -2 20.00 10.98 3 -14 -2 17.74 10.25 4 -14 -2 52.31 13.49 4 -14 -2 55.69 13.79 1 -15 -2 110.01 18.96 1 -15 -2 89.25 16.58 2 -15 -2 19.12 13.99 2 -15 -2 33.98 12.73 1 -3 -1 110.17 55.87 1 -3 -1 47.49 50.67 1 -3 -1 500.51 44.99 1 -3 -1 548.73 48.46 1 -4 -1 1839.07 243.92 1 -4 -1 1481.27 201.03 1 -4 -1 2188.80 184.39 1 -4 -1 2387.48 200.63 1 -5 -1 5288.65 668.35 1 -5 -1 5519.64 698.80 1 -5 -1 4006.06 335.51 1 -5 -1 4181.33 349.88 2 -5 -1 13.50 79.97 2 -5 -1 -41.19 67.27 2 -5 -1 334.13 33.86 2 -5 -1 260.39 27.08 1 -6 -1 510.45 94.34 1 -6 -1 655.75 112.99 1 -6 -1 126.97 17.61 1 -6 -1 169.29 20.27 2 -6 -1 59.45 57.28 2 -6 -1 213.95 59.83 2 -6 -1 627.40 56.49 2 -6 -1 632.25 56.67 1 -7 -1 186.90 59.50 1 -7 -1 203.29 62.53 1 -7 -1 71.31 12.74 1 -7 -1 97.89 15.09 2 -7 -1 25.59 52.46 2 -7 -1 79.83 52.27 2 -7 -1 346.17 34.12 2 -7 -1 376.94 36.08 3 -7 -1 -33.93 54.57 1 -8 -1 1034.63 153.94 1 -8 -1 1083.90 160.00 1 -8 -1 1050.78 92.16 1 -8 -1 893.29 78.90 2 -8 -1 45.78 51.54 2 -8 -1 38.46 48.16 2 -8 -1 61.56 13.53 2 -8 -1 61.19 12.90 3 -8 -1 -90.70 44.19 3 -8 -1 82.71 52.76 3 -8 -1 61.41 13.87 3 -8 -1 56.59 12.79 1 -9 -1 2098.34 281.23 1 -9 -1 1804.34 248.60 1 -9 -1 2151.64 184.07 1 -9 -1 1861.69 159.68 2 -9 -1 -34.11 31.01 2 -9 -1 34.22 49.85 2 -9 -1 41.17 13.54 2 -9 -1 48.69 13.42 3 -9 -1 87.23 16.53 3 -9 -1 90.54 15.47 1 -10 -1 182.37 24.60 1 -10 -1 150.47 21.51 2 -10 -1 7.72 12.53 2 -10 -1 4.87 11.27 3 -10 -1 368.62 37.71 3 -10 -1 336.64 34.19 4 -10 -1 21.40 11.23 4 -10 -1 0.23 9.12 1 -11 -1 436.95 44.11 1 -11 -1 427.18 42.48 2 -11 -1 22.69 12.49 2 -11 -1 23.34 11.03 3 -11 -1 6.71 10.77 3 -11 -1 17.12 10.14 4 -11 -1 72.18 13.87 4 -11 -1 85.21 14.36 1 -12 -1 88.52 16.82 1 -12 -1 95.87 16.76 2 -12 -1 69.30 14.91 2 -12 -1 91.75 15.36 3 -12 -1 4.66 9.88 3 -12 -1 -6.51 8.70 4 -12 -1 14.47 10.03 4 -12 -1 8.38 8.52 5 -12 -1 2.32 7.77 1 -13 -1 82.22 15.48 1 -13 -1 83.76 14.91 2 -13 -1 33.37 12.26 2 -13 -1 13.66 10.12 3 -13 -1 18.04 10.12 3 -13 -1 -6.35 8.58 4 -13 -1 13.55 10.14 4 -13 -1 21.97 9.36 5 -13 -1 14.21 10.09 5 -13 -1 5.61 8.22 1 -14 -1 34.33 11.66 1 -14 -1 17.79 10.22 2 -14 -1 66.80 14.63 2 -14 -1 116.31 17.89 3 -14 -1 20.06 10.42 3 -14 -1 24.80 9.78 4 -14 -1 24.13 10.64 4 -14 -1 6.86 10.28 1 -15 -1 7.40 11.02 1 -15 -1 6.30 9.65 2 -15 -1 35.59 12.40 2 -15 -1 22.26 11.64 0 -1 0 331.79 62.48 0 -1 0 361.03 63.98 0 -2 0 2871.28 364.75 0 -2 0 2610.40 333.08 0 -3 0 -17.56 57.30 0 -3 0 -15.24 55.54 1 -3 0 158.30 59.28 1 -3 0 267.34 62.42 1 -3 0 556.97 48.86 1 -3 0 552.45 48.44 0 -4 0 1471.58 200.46 0 -4 0 1228.47 171.23 1 -4 0 240.93 63.37 1 -4 0 349.80 70.17 1 -4 0 279.70 27.15 1 -4 0 301.91 28.83 0 -5 0 77.93 60.80 0 -5 0 171.55 62.49 1 -5 0 2400.41 313.86 1 -5 0 2451.29 320.16 1 -5 0 2120.95 178.90 1 -5 0 1857.65 157.17 2 -5 0 81.98 77.92 2 -5 0 150.95 73.97 2 -5 0 425.81 39.46 2 -5 0 586.13 52.44 0 -6 0 656.07 111.46 0 -6 0 615.04 105.89 1 -6 0 1100.05 157.90 1 -6 0 1322.16 184.88 1 -6 0 805.65 70.67 1 -6 0 817.37 71.76 2 -6 0 195.21 62.79 2 -6 0 174.22 56.82 2 -6 0 712.13 62.73 2 -6 0 664.72 59.04 0 -7 0 -1.59 56.51 0 -7 0 -159.52 52.38 1 -7 0 142.55 56.37 1 -7 0 271.22 63.82 1 -7 0 34.37 11.33 1 -7 0 14.78 10.60 2 -7 0 -23.18 46.75 2 -7 0 23.70 44.58 2 -7 0 -4.52 9.03 2 -7 0 7.17 9.39 3 -7 0 139.49 17.81 3 -7 0 109.20 15.56 0 -8 0 324.28 79.85 0 -8 0 746.94 119.78 1 -8 0 404.08 83.51 1 -8 0 407.71 78.29 1 -8 0 409.65 39.10 1 -8 0 369.27 35.77 2 -8 0 302.47 61.67 2 -8 0 168.97 55.73 2 -8 0 119.05 16.36 2 -8 0 139.89 17.78 3 -8 0 -0.18 1.04 3 -8 0 23.37 51.13 3 -8 0 13.15 11.39 3 -8 0 28.03 11.23 0 -9 0 178.17 59.02 0 -9 0 -12.40 63.45 1 -9 0 -104.59 64.02 1 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0 61.85 13.79 3 -14 0 4.31 9.45 3 -14 0 10.90 8.99 1 -15 0 139.16 20.26 1 -15 0 109.44 17.55 2 -15 0 9.33 10.85 2 -15 0 24.02 10.85 0 -1 1 12.59 34.67 0 -1 1 12.03 8.96 0 -1 1 -61.00 35.86 0 -1 1 40.12 9.25 0 -1 1 -23.70 38.41 0 -1 1 -28.58 37.29 0 -2 1 235.28 56.81 0 -2 1 237.21 23.64 0 -2 1 207.49 53.42 0 -2 1 236.89 23.06 0 -2 1 102.82 52.91 0 -2 1 149.18 54.88 1 -2 1 822.21 69.36 1 -2 1 645.65 54.78 0 -3 1 146.35 54.42 0 -3 1 155.15 18.17 0 -3 1 169.53 52.28 0 -3 1 132.86 16.04 0 -3 1 51.58 54.53 0 -3 1 46.38 53.34 1 -3 1 974.86 135.85 1 -3 1 706.23 103.14 1 -3 1 740.31 63.21 1 -3 1 698.88 59.70 0 -4 1 2184.76 284.22 0 -4 1 1465.12 124.46 0 -4 1 2127.41 276.71 0 -4 1 1302.78 110.81 0 -4 1 340.35 74.34 0 -4 1 440.10 85.78 1 -4 1 6748.92 845.63 1 -4 1 6653.61 832.71 1 -4 1 5848.36 487.27 1 -4 1 5978.40 498.17 0 -5 1 639.60 105.56 0 -5 1 415.14 39.09 0 -5 1 549.70 95.55 0 -5 1 364.26 34.62 0 -5 1 129.79 62.31 0 -5 1 242.62 76.31 1 -5 1 2504.60 324.93 1 -5 1 2738.01 352.63 1 -5 1 2090.26 176.07 1 -5 1 2045.84 172.52 2 -5 1 409.57 91.02 2 -5 1 488.97 93.12 2 -5 1 948.21 81.57 2 -5 1 977.29 84.00 0 -6 1 151.84 62.05 0 -6 1 31.85 12.81 0 -6 1 134.24 56.03 0 -6 1 35.79 12.47 0 -6 1 67.27 59.54 0 -6 1 93.45 67.12 1 -6 1 1623.42 218.48 1 -6 1 1886.73 249.17 1 -6 1 1739.73 147.48 1 -6 1 1726.00 146.43 2 -6 1 64.23 46.48 2 -6 1 52.51 40.31 2 -6 1 29.80 9.85 2 -6 1 28.97 9.56 0 -7 1 150.23 61.22 0 -7 1 77.25 14.53 0 -7 1 127.61 56.89 0 -7 1 86.50 14.30 0 -7 1 48.12 55.58 0 -7 1 35.94 59.15 1 -7 1 140.21 51.45 1 -7 1 189.80 52.04 1 -7 1 -6.85 9.35 1 -7 1 -0.12 9.51 2 -7 1 168.24 53.88 2 -7 1 181.56 50.03 2 -7 1 236.81 24.48 2 -7 1 253.04 25.69 3 -7 1 54.33 12.18 3 -7 1 36.06 10.41 0 -8 1 356.91 81.66 0 -8 1 90.94 15.28 0 -8 1 317.17 76.15 0 -8 1 59.87 13.89 0 -8 1 157.34 64.48 0 -8 1 190.05 70.07 1 -8 1 1256.74 174.13 1 -8 1 1058.05 152.25 1 -8 1 865.02 76.02 1 -8 1 831.90 73.20 2 -8 1 -16.86 20.43 2 -8 1 38.56 39.54 2 -8 1 23.35 10.44 2 -8 1 36.31 10.39 3 -8 1 11.04 48.06 3 -8 1 16.55 11.08 3 -8 1 22.85 10.39 0 -9 1 -14.89 25.00 0 -9 1 561.41 53.02 0 -9 1 1003.94 157.09 0 -9 1 786.35 72.20 0 -9 1 442.04 94.26 0 -9 1 354.73 89.73 1 -9 1 -0.12 0.72 1 -9 1 559.07 96.52 1 -9 1 205.47 23.72 1 -9 1 187.30 22.28 2 -9 1 119.86 50.92 2 -9 1 153.22 19.67 2 -9 1 184.07 21.18 3 -9 1 8.91 10.46 3 -9 1 5.63 9.30 4 -9 1 20.62 10.03 4 -9 1 -2.08 7.56 0 -10 1 4838.77 407.23 0 -10 1 9999.00 835.13 1 -10 1 135.53 19.76 1 -10 1 130.44 18.21 2 -10 1 116.55 17.32 2 -10 1 174.54 20.44 3 -10 1 277.68 29.41 3 -10 1 235.68 25.00 4 -10 1 54.57 10.98 4 -10 1 32.49 9.20 0 -11 1 467.72 47.22 0 -11 1 91.51 21.77 1 -11 1 15.54 11.74 1 -11 1 0.29 9.85 2 -11 1 30.93 11.34 2 -11 1 19.72 9.66 3 -11 1 169.29 20.93 3 -11 1 160.00 19.19 4 -11 1 16.64 8.56 4 -11 1 33.13 9.17 5 -11 1 2.89 7.41 0 -12 1 9.56 12.42 0 -12 1 5.49 12.36 1 -12 1 -13.49 10.27 1 -12 1 -1.89 8.59 2 -12 1 89.41 15.13 2 -12 1 80.43 13.20 3 -12 1 16.86 9.79 3 -12 1 7.56 7.97 4 -12 1 0.85 8.00 4 -12 1 4.95 7.59 5 -12 1 2.94 7.75 5 -12 1 6.89 7.94 0 -13 1 27.02 12.23 1 -13 1 53.61 13.72 1 -13 1 86.83 14.48 2 -13 1 10.42 10.48 2 -13 1 2.09 8.68 3 -13 1 0.35 8.81 3 -13 1 11.07 7.94 4 -13 1 26.29 9.71 4 -13 1 24.33 9.17 0 -14 1 63.52 14.31 1 -14 1 11.28 11.16 1 -14 1 39.29 11.49 2 -14 1 74.64 14.63 2 -14 1 114.45 16.68 3 -14 1 5.44 9.30 3 -14 1 25.34 9.09 0 -15 1 8.25 10.30 1 -15 1 31.92 11.40 1 -15 1 25.72 10.64 0 -1 2 3392.23 282.77 0 -1 2 4192.63 349.16 0 -1 2 2845.43 357.07 0 -1 2 2091.88 265.89 0 -2 2 37.86 35.63 0 -2 2 136.74 15.52 0 -2 2 12.68 34.58 0 -2 2 191.18 19.30 0 -2 2 25.61 40.51 0 -2 2 53.07 42.73 1 -2 2 57.84 7.26 1 -2 2 68.75 7.58 0 -3 2 56.61 39.40 0 -3 2 38.11 10.48 0 -3 2 -186.98 40.28 0 -3 2 18.30 8.92 0 -3 2 23.18 46.30 0 -3 2 14.20 50.83 1 -3 2 81.57 48.78 1 -3 2 107.26 38.89 1 -3 2 68.70 9.68 1 -3 2 105.40 11.21 0 -4 2 467.00 80.68 0 -4 2 612.38 54.26 0 -4 2 287.86 58.78 0 -4 2 565.13 50.41 0 -4 2 119.70 56.68 0 -4 2 86.58 64.12 1 -4 2 546.63 87.96 1 -4 2 517.48 80.00 1 -4 2 536.94 46.87 1 -4 2 542.19 47.13 2 -4 2 375.41 33.62 2 -4 2 399.96 35.48 0 -5 2 268.47 61.86 0 -5 2 260.72 26.87 0 -5 2 194.41 52.93 0 -5 2 350.85 33.65 0 -5 2 51.35 53.89 0 -5 2 -300.53 66.56 1 -5 2 228.09 57.01 1 -5 2 334.46 61.96 1 -5 2 23.33 9.88 1 -5 2 20.14 9.15 2 -5 2 48.90 43.86 2 -5 2 166.46 17.41 2 -5 2 162.67 16.93 0 -6 2 -80.61 45.01 0 -6 2 203.94 22.74 0 -6 2 180.19 52.63 0 -6 2 207.98 23.24 0 -6 2 42.73 52.58 0 -6 2 24.33 59.99 1 -6 2 1370.62 185.36 1 -6 2 1268.05 171.47 1 -6 2 1332.66 113.56 1 -6 2 1281.78 109.28 2 -6 2 35.62 43.09 2 -6 2 33.11 34.07 2 -6 2 61.75 10.70 2 -6 2 29.50 8.55 3 -6 2 19.05 8.51 0 -7 2 174.62 52.17 0 -7 2 100.64 15.34 0 -7 2 162.18 51.25 0 -7 2 90.54 15.15 0 -7 2 29.15 49.87 0 -7 2 2.30 56.21 1 -7 2 154.59 45.12 1 -7 2 81.09 38.78 1 -7 2 48.11 10.95 1 -7 2 53.64 11.11 2 -7 2 -2.01 30.60 2 -7 2 76.56 36.79 2 -7 2 61.48 11.38 2 -7 2 33.20 9.47 3 -7 2 26.05 10.23 3 -7 2 44.12 10.69 0 -8 2 379.53 69.42 0 -8 2 67.29 14.44 0 -8 2 59.44 46.47 0 -8 2 62.13 14.57 0 -8 2 16.81 51.94 0 -8 2 24.83 58.12 1 -8 2 -44.85 30.13 1 -8 2 232.21 54.88 1 -8 2 89.81 14.45 1 -8 2 117.44 15.78 2 -8 2 -0.11 0.64 2 -8 2 210.88 52.31 2 -8 2 329.61 32.36 2 -8 2 102.82 14.26 3 -8 2 16.37 9.93 3 -8 2 36.49 9.77 0 -9 2 -0.12 0.73 0 -9 2 488.80 47.79 0 -9 2 632.73 106.29 0 -9 2 492.12 47.92 0 -9 2 97.97 62.11 0 -9 2 86.02 67.18 1 -9 2 651.15 106.05 1 -9 2 626.75 57.26 2 -9 2 8.74 10.63 2 -9 2 22.25 9.36 3 -9 2 157.74 18.66 3 -9 2 166.46 18.81 4 -9 2 47.52 10.32 4 -9 2 46.69 9.91 0 -10 2 1232.51 108.87 0 -10 2 1075.82 96.11 1 -10 2 -4.30 10.48 2 -10 2 44.90 11.60 2 -10 2 49.16 10.63 3 -10 2 19.59 8.78 3 -10 2 7.84 8.13 4 -10 2 10.48 8.06 4 -10 2 4.81 7.48 0 -11 2 48.32 16.03 0 -11 2 23.96 14.11 1 -11 2 1.20 9.83 2 -11 2 18.10 9.51 2 -11 2 16.53 8.74 3 -11 2 10.18 8.30 3 -11 2 7.93 7.62 4 -11 2 11.69 8.25 4 -11 2 13.07 7.69 5 -11 2 0.11 7.50 0 -12 2 37.48 12.02 0 -12 2 16.01 11.00 1 -12 2 45.21 11.87 2 -12 2 22.78 9.77 2 -12 2 20.07 8.50 3 -12 2 0.62 7.71 3 -12 2 -2.47 7.49 4 -12 2 11.35 8.33 4 -12 2 -13.46 7.20 0 -13 2 -1.53 8.02 0 -13 2 -0.45 9.32 1 -13 2 50.85 12.36 2 -13 2 80.74 13.83 2 -13 2 65.16 11.68 3 -13 2 25.44 9.35 3 -13 2 42.12 9.88 0 -14 2 -29.01 7.63 0 -14 2 5.83 9.91 1 -14 2 57.54 13.26 2 -14 2 -2.55 9.03 2 -14 2 11.24 8.68 0 -15 2 79.28 14.59 0 -15 2 34.80 13.08 1 0 3 13.61 5.43 1 0 3 -0.19 5.70 0 -1 3 21.40 25.64 1 -1 3 348.35 30.85 1 -1 3 383.73 33.98 1 -1 3 377.99 32.03 0 -2 3 30.71 35.99 0 -2 3 86.42 12.94 0 -2 3 90.78 13.49 0 -2 3 22.43 34.40 0 -2 3 28.05 45.04 1 -2 3 411.02 36.86 1 -2 3 326.78 30.32 0 -3 3 43.98 37.49 0 -3 3 145.46 17.32 0 -3 3 119.46 15.66 0 -3 3 25.10 39.88 0 -3 3 23.85 51.71 1 -3 3 279.86 58.10 1 -3 3 766.00 66.55 1 -3 3 216.05 44.31 1 -3 3 303.04 29.81 0 -4 3 193.84 50.18 0 -4 3 748.15 65.68 0 -4 3 60.43 38.36 0 -4 3 618.76 55.20 0 -4 3 70.03 43.98 0 -4 3 34.72 55.27 1 -4 3 1470.77 193.52 1 -4 3 2893.09 243.11 1 -4 3 2005.45 257.00 2 -4 3 34.12 7.31 2 -4 3 48.23 7.35 0 -5 3 328.32 64.35 0 -5 3 857.75 75.03 0 -5 3 143.12 44.78 0 -5 3 823.83 72.55 0 -5 3 108.31 48.24 0 -5 3 236.81 65.66 1 -5 3 468.61 76.07 1 -5 3 207.33 23.19 1 -5 3 582.49 86.50 2 -5 3 62.85 43.19 2 -5 3 143.69 15.52 2 -5 3 132.78 14.57 0 -6 3 6.32 40.32 0 -6 3 53.86 12.13 0 -6 3 6.97 35.76 0 -6 3 37.70 11.03 0 -6 3 0.98 43.13 0 -6 3 78.96 53.83 1 -6 3 832.71 119.62 1 -6 3 615.53 55.93 1 -6 3 795.56 112.43 2 -6 3 146.84 47.70 2 -6 3 64.61 34.08 2 -6 3 93.29 12.69 2 -6 3 99.18 12.84 3 -6 3 0.79 8.19 3 -6 3 20.08 8.83 0 -7 3 -2.14 42.31 0 -7 3 3.58 11.23 0 -7 3 3.02 36.09 0 -7 3 48.87 10.31 0 -7 3 24.04 46.51 0 -7 3 20.36 53.21 1 -7 3 205.88 47.95 1 -7 3 18.37 11.19 1 -7 3 80.20 35.52 2 -7 3 27.65 9.19 2 -7 3 -2.14 7.86 3 -7 3 6.04 8.55 3 -7 3 10.19 8.04 0 -8 3 -23.05 25.03 0 -8 3 173.65 22.81 0 -8 3 107.02 44.82 0 -8 3 11.77 12.04 0 -8 3 38.36 49.85 0 -8 3 46.63 56.07 1 -8 3 -0.11 0.68 1 -8 3 30.03 12.61 2 -8 3 66.93 11.74 2 -8 3 69.65 11.41 3 -8 3 -5.13 7.39 3 -8 3 10.10 7.30 4 -8 3 0.40 6.22 0 -9 3 1037.05 92.64 0 -9 3 1056.44 93.85 1 -9 3 0.90 11.71 2 -9 3 110.33 14.61 2 -9 3 112.91 14.59 3 -9 3 43.95 9.37 3 -9 3 22.32 8.18 4 -9 3 12.37 7.36 4 -9 3 20.88 7.43 0 -10 3 215.25 26.82 0 -10 3 209.59 26.59 1 -10 3 -4.53 10.09 2 -10 3 139.16 17.26 2 -10 3 146.92 17.28 3 -10 3 0.57 7.47 3 -10 3 6.59 7.36 4 -10 3 16.08 7.29 4 -10 3 8.76 7.03 0 -11 3 390.99 39.71 0 -11 3 391.24 40.75 1 -11 3 3.36 9.56 2 -11 3 1.53 7.99 2 -11 3 2.84 7.73 3 -11 3 79.08 12.87 3 -11 3 81.33 12.39 4 -11 3 -2.30 7.25 4 -11 3 -5.60 7.19 0 -12 3 28.87 12.18 0 -12 3 36.12 12.99 1 -12 3 10.94 9.67 2 -12 3 17.18 8.49 2 -12 3 4.44 7.78 3 -12 3 15.09 8.55 3 -12 3 5.83 8.13 0 -13 3 47.06 13.01 0 -13 3 23.20 11.49 1 -13 3 -15.88 9.39 2 -13 3 -3.12 8.08 2 -13 3 -5.64 7.53 0 -14 3 57.65 13.79 0 -14 3 52.56 13.56 1 -14 3 7.60 10.96 1 0 4 20.42 5.58 1 0 4 21.53 6.22 0 -1 4 1100.86 141.99 1 -1 4 68.56 9.39 1 -1 4 94.98 11.65 0 -2 4 566.58 49.72 0 -2 4 645.82 56.80 0 -2 4 458.68 68.10 0 -2 4 188.35 48.19 1 -2 4 68.99 10.27 1 -2 4 64.64 10.90 0 -3 4 4.73 31.30 0 -3 4 155.80 17.77 0 -3 4 205.55 22.02 0 -3 4 12.28 31.87 0 -3 4 -10.67 43.44 1 -3 4 5.00 34.54 1 -3 4 65.44 11.03 1 -3 4 15.36 26.86 1 -3 4 48.08 10.82 2 -3 4 18.06 4.43 0 -4 4 12.00 33.29 0 -4 4 36.15 10.85 0 -4 4 50.29 11.94 0 -4 4 3.02 33.71 0 -4 4 28.51 46.64 1 -4 4 18.29 32.20 1 -4 4 2.95 9.43 1 -4 4 40.60 28.55 1 -4 4 -1.99 10.17 2 -4 4 53.27 8.00 2 -4 4 58.62 7.25 0 -5 4 35.49 36.22 0 -5 4 162.10 19.33 0 -5 4 208.30 23.20 0 -5 4 3.81 36.83 0 -5 4 -9.05 51.81 1 -5 4 111.62 39.80 1 -5 4 189.88 21.52 1 -5 4 124.54 36.10 1 -5 4 199.58 22.64 2 -5 4 29.76 7.77 2 -5 4 59.52 8.65 0 -6 4 67.87 40.38 0 -6 4 165.17 20.65 0 -6 4 17.35 37.43 0 -6 4 274.04 28.67 0 -6 4 18.61 40.97 0 -6 4 -228.98 53.30 1 -6 4 223.24 51.37 1 -6 4 167.35 20.66 1 -6 4 274.85 52.72 1 -6 4 150.95 19.67 2 -6 4 7.58 7.75 2 -6 4 1.19 6.94 3 -6 4 18.14 7.02 3 -6 4 14.74 6.67 0 -7 4 150.63 43.27 0 -7 4 54.73 13.13 0 -7 4 13.32 36.86 0 -7 4 45.50 12.62 0 -7 4 10.76 42.24 0 -7 4 20.39 54.92 1 -7 4 18.74 11.86 1 -7 4 16.56 11.81 2 -7 4 48.91 9.61 2 -7 4 26.65 8.34 3 -7 4 -3.69 6.82 3 -7 4 -2.64 6.34 0 -8 4 10.37 12.24 0 -8 4 24.59 12.32 1 -8 4 1.06 10.80 1 -8 4 16.34 11.30 2 -8 4 14.17 8.04 2 -8 4 18.71 7.79 3 -8 4 8.40 7.50 3 -8 4 5.75 6.60 4 -8 4 1.51 6.52 4 -8 4 9.95 6.25 0 -9 4 283.82 30.79 0 -9 4 262.25 29.61 1 -9 4 108.07 16.36 1 -9 4 99.99 15.69 2 -9 4 31.45 8.58 2 -9 4 13.37 7.53 3 -9 4 28.41 8.78 3 -9 4 35.65 8.31 4 -9 4 -7.63 6.81 4 -9 4 1.74 6.50 0 -10 4 63.68 14.34 0 -10 4 70.01 15.41 1 -10 4 24.00 10.52 1 -10 4 15.52 10.64 2 -10 4 8.97 7.86 2 -10 4 11.27 7.71 3 -10 4 11.38 7.51 3 -10 4 10.46 6.91 4 -10 4 2.11 6.90 4 -10 4 -0.26 6.41 0 -11 4 21.60 11.84 0 -11 4 59.51 12.60 1 -11 4 26.22 10.64 1 -11 4 32.65 11.75 2 -11 4 16.29 8.54 2 -11 4 7.38 7.45 3 -11 4 15.22 7.65 3 -11 4 2.31 7.20 0 -12 4 9.54 10.38 0 -12 4 -25.36 7.73 1 -12 4 39.24 11.96 1 -12 4 16.86 10.64 2 -12 4 23.92 8.65 2 -12 4 7.46 7.31 0 -13 4 1.98 9.73 0 -13 4 17.79 9.13 1 -13 4 60.70 14.23 1 -13 4 30.79 11.67 1 0 5 51.63 7.92 1 0 5 10.17 7.01 0 -1 5 -1.06 19.28 1 -1 5 13.91 7.48 1 -1 5 12.42 8.11 0 -2 5 13.09 8.98 0 -2 5 24.72 24.57 1 -2 5 22.43 8.61 1 -2 5 54.20 10.43 0 -3 5 7.31 27.94 0 -3 5 26.93 10.18 0 -3 5 20.35 10.64 0 -3 5 16.74 29.46 0 -3 5 1.77 38.37 1 -3 5 71.01 12.05 1 -3 5 48.02 29.28 1 -3 5 59.65 11.43 2 -3 5 -53.09 4.90 0 -4 5 17.62 30.94 0 -4 5 226.39 24.21 0 -4 5 248.84 26.15 0 -4 5 33.10 32.94 0 -4 5 29.86 43.33 1 -4 5 45.99 11.58 1 -4 5 32.34 11.23 2 -4 5 2.72 4.53 0 -5 5 21.22 36.04 0 -5 5 89.33 15.07 0 -5 5 85.69 15.14 0 -5 5 7.92 38.04 1 -5 5 237.94 25.30 1 -5 5 257.81 26.94 2 -5 5 18.30 5.97 3 -5 5 -42.43 4.84 0 -6 5 57.60 13.13 0 -6 5 73.96 14.36 1 -6 5 19.55 10.70 1 -6 5 16.39 10.71 2 -6 5 0.76 5.89 3 -6 5 31.35 6.58 3 -6 5 34.14 6.62 0 -7 5 16.96 11.10 0 -7 5 29.74 11.78 1 -7 5 10.99 9.77 1 -7 5 4.13 10.40 2 -7 5 17.87 6.72 3 -7 5 9.27 6.09 3 -7 5 4.29 5.68 4 -7 5 -0.04 5.14 0 -8 5 48.34 12.74 0 -8 5 51.61 13.20 1 -8 5 15.85 10.22 1 -8 5 -2.27 10.10 2 -8 5 17.84 7.21 3 -8 5 15.42 6.84 3 -8 5 8.59 6.00 4 -8 5 0.77 6.09 4 -8 5 5.26 6.20 0 -9 5 58.37 12.91 0 -9 5 38.53 12.49 1 -9 5 38.79 11.40 1 -9 5 22.01 11.02 2 -9 5 0.54 6.97 3 -9 5 5.62 6.77 3 -9 5 4.12 6.32 0 -10 5 28.23 11.12 0 -10 5 19.15 10.81 1 -10 5 0.45 9.80 1 -10 5 -1.93 9.16 2 -10 5 32.12 9.14 3 -10 5 6.28 7.90 0 -11 5 22.60 10.74 0 -11 5 18.81 10.73 1 -11 5 10.74 10.13 1 -11 5 -3.31 8.88 2 -11 5 6.65 7.04 0 -12 5 13.58 9.88 0 -12 5 -7.46 9.48 1 -12 5 17.66 10.49 1 -12 5 20.16 9.87 1 0 6 1.68 6.39 2 0 6 45.56 6.78 2 0 6 24.77 6.08 1 -1 6 22.41 7.00 1 -1 6 27.83 7.96 2 -1 6 58.28 8.49 2 -1 6 55.83 8.71 2 -1 6 51.24 6.54 2 -1 6 54.22 6.42 1 -2 6 4.42 7.03 1 -2 6 -1.00 7.69 2 -2 6 0.56 6.14 2 -2 6 1.65 6.50 2 -2 6 5.22 2.82 0 -3 6 38.91 10.87 0 -3 6 66.51 12.49 1 -3 6 10.92 7.75 1 -3 6 14.68 8.42 2 -3 6 -8.76 6.62 2 -3 6 -2.66 7.41 0 -4 6 -4.88 9.00 0 -4 6 -4.03 9.48 1 -4 6 12.07 8.20 1 -4 6 21.14 9.05 2 -4 6 -0.03 7.27 2 -4 6 6.04 8.49 0 -5 6 -2.15 8.99 0 -5 6 -9.65 9.44 1 -5 6 5.01 8.51 1 -5 6 18.90 9.41 2 -5 6 -1.74 7.65 3 -5 6 -0.92 3.82 3 -5 6 6.44 4.09 0 -6 6 29.62 10.22 0 -6 6 31.05 11.47 1 -6 6 -3.01 8.20 1 -6 6 5.03 9.00 2 -6 6 32.48 9.61 3 -6 6 14.42 5.31 3 -6 6 -34.69 4.39 0 -7 6 24.72 10.17 0 -7 6 1.63 9.68 1 -7 6 -4.20 8.05 1 -7 6 5.33 8.92 2 -7 6 16.91 8.96 3 -7 6 -3.12 5.32 3 -7 6 6.43 5.21 0 -8 6 2.79 9.68 0 -8 6 7.36 9.65 1 -8 6 2.25 8.99 1 -8 6 10.51 9.44 2 -8 6 23.72 9.44 0 -9 6 28.62 11.16 0 -9 6 12.74 10.86 1 -9 6 2.28 9.36 1 -9 6 -6.93 9.15 2 -9 6 22.56 9.71 0 -10 6 19.53 10.23 0 -10 6 20.96 10.90 1 -10 6 17.31 10.16 1 -10 6 -6.86 9.68 0 -11 6 7.03 9.19 0 -11 6 6.77 9.39 2 0 7 4.38 4.48 2 0 7 2.53 4.89 1 -1 7 2.19 5.29 1 -1 7 1.86 6.23 2 -1 7 -6.61 5.08 2 -1 7 -3.83 5.80 2 -1 7 6.92 4.37 2 -1 7 2.83 3.60 1 -2 7 4.95 6.11 1 -2 7 7.33 7.09 2 -2 7 -3.94 5.71 2 -2 7 -2.80 6.64 2 -2 7 0.13 3.12 0 -3 7 10.60 8.12 1 -3 7 5.01 6.36 1 -3 7 13.06 7.78 2 -3 7 -3.42 6.15 2 -3 7 3.55 7.20 0 -4 7 10.31 7.65 0 -4 7 10.21 8.51 1 -4 7 4.16 6.72 1 -4 7 0.70 7.50 2 -4 7 -7.94 6.67 2 -4 7 -1.48 7.48 0 -5 7 -4.10 7.90 0 -5 7 8.40 8.61 1 -5 7 16.69 7.95 1 -5 7 17.61 8.51 2 -5 7 -6.79 7.33 2 -5 7 12.20 8.13 0 -6 7 12.28 8.63 0 -6 7 28.45 9.72 1 -6 7 4.34 7.76 1 -6 7 1.68 8.16 2 -6 7 -0.13 7.78 2 -6 7 -4.63 7.80 0 -7 7 11.08 8.72 0 -7 7 -1.35 8.57 1 -7 7 11.38 7.89 1 -7 7 3.79 8.38 0 -8 7 1.42 9.07 0 -8 7 -2.57 9.22 1 -8 7 5.74 8.06 1 -8 7 7.94 8.72 0 -9 7 3.23 9.51 0 -9 7 13.33 10.09 1 -1 8 3.56 5.97 1 -2 8 -0.98 5.91 1 -2 8 4.63 6.46 0 -3 8 0.15 6.87 1 -3 8 -6.53 6.06 1 -3 8 14.70 7.10 0 -4 8 -2.92 6.97 0 -4 8 9.20 7.76 1 -4 8 -0.51 6.67 1 -4 8 11.88 7.27 0 -5 8 8.66 7.08 0 -5 8 19.00 8.10 0 -6 8 -11.38 7.58 0 -6 8 -2.15 8.02 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 81314 _shelx_res_file ; nicotinic_acid_2x-merged.res created by SHELXL-2014/8 TITL nicotinic_acid_2x-merged.res in P2(1)/c REM Old TITL na_merge in P2(1)_c REM SHELXT solution in P2(1)/c REM R1 0.460, Rweak 0.390, Alpha 0.184, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: C5 N3 O CELL 0.02508 7.4060 11.6915 7.3770 90.000 114.448 90.000 ZERR 24.000 0.0250 0.0020 0.0110 0.000 0.140 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 0.86500 = 51.65125 0.21560 0.00330 0.00160 11.500 0.68000 12.01000 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 0.04081 = 57.79977 0.00304 0.00000 0.00000 0.624 0.35000 1.00800 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 1.16630 = 0.58260 -11.52901 0.00610 0.00330 19.600 0.68000 14.01000 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 0.86700 = 32.90894 0.25080 0.01060 0.00600 32.500 0.68000 16.00000 UNIT 24 20 4 8 L.S. 100 BOND $H LIST 6 FMAP 2 EQIV $1 -x+1, y-1/2, -z+1/2 ACTA PLAN 20 WGHT 0.200000 FVAR 1.70177 C6 1 0.637740 0.575767 0.291936 11.00000 0.03800 C1 1 0.655367 0.793135 0.279139 11.00000 0.04533 AFIX 43 H1 2 0.522981 0.797748 0.258787 11.00000 -1.20000 AFIX 0 O1 4 0.446915 0.586754 0.249470 11.00000 0.06464 AFIX 147 HO 2 0.392298 0.524371 0.217330 11.00000 -0.00100 AFIX 0 N1 3 0.769786 0.891233 0.289479 11.00000 0.04585 O2 4 0.701526 0.486549 0.299157 11.00000 0.08723 C2 1 0.758171 0.683439 0.302479 11.00000 0.04942 C5 1 0.951630 0.879516 0.333692 11.00000 0.04818 AFIX 43 H5 2 1.026164 0.945344 0.345458 11.00000 -1.20000 REM ##### REM ##### AFIX 0 C4 1 1.047408 0.776961 0.365654 11.00000 0.06289 AFIX 43 H2 2 1.183980 0.778038 0.404756 11.00000 -1.20000 REM ##### AFIX 0 C3 1 0.960179 0.675694 0.345098 11.00000 0.04409 AFIX 43 H3 2 1.026604 0.606620 0.357743 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM nicotinic_acid_2x-merged.res in P2(1)/c REM R1 = 0.3371 for 303 Fo > 4sig(Fo) and 0.4019 for all 552 data REM 39 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.550, deepest hole -0.816, 1-sigma level 0.173 Q1 1 1.1205 0.7195 0.1597 11.00000 0.05 0.55 Q2 1 0.5835 0.7950 0.2012 11.00000 0.05 0.53 Q3 1 0.4290 0.8148 0.1789 11.00000 0.05 0.53 Q4 1 0.7190 0.6810 0.3564 11.00000 0.05 0.50 Q5 1 0.8321 0.6787 0.2406 11.00000 0.05 0.47 Q6 1 0.8954 0.6388 0.1729 11.00000 0.05 0.44 Q7 1 0.6298 0.5812 0.2053 11.00000 0.05 0.43 Q8 1 0.4379 0.5934 0.1430 11.00000 0.05 0.42 Q9 1 0.8243 0.8350 0.1497 11.00000 0.05 0.40 Q10 1 0.7098 0.8940 0.1937 11.00000 0.05 0.37 Q11 1 0.5756 0.7426 0.1411 11.00000 0.05 0.35 Q12 1 0.6754 0.4852 0.3752 11.00000 0.05 0.31 Q13 1 0.4856 0.4369 0.3978 11.00000 0.05 0.29 Q14 1 0.9270 0.8816 0.2413 11.00000 0.05 0.29 Q15 1 0.8730 1.0574 0.3297 11.00000 0.05 0.28 Q16 1 0.2987 0.6419 0.1256 11.00000 0.05 0.28 Q17 1 0.9935 1.0436 0.3156 11.00000 0.05 0.28 Q18 1 0.6888 0.6394 0.4930 11.00000 0.05 0.26 Q19 1 0.9108 0.6682 0.4224 11.00000 0.05 0.26 Q20 1 0.7170 0.3828 0.3103 11.00000 0.05 0.26 ; _shelx_res_checksum 29007 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 C C6 0.638(5) 0.5758(11) 0.292(2) 0.038(3) Uiso d 1 C C1 0.655(5) 0.7931(12) 0.279(2) 0.045(4) Uiso d 1 H H1 0.5230 0.7977 0.2588 0.054 Uiso calc 1 O O1 0.447(5) 0.5868(12) 0.249(2) 0.065(4) Uiso d 1 H HO 0.3923 0.5244 0.2173 0.00(2) Uiso calc 1 N N1 0.770(5) 0.8912(11) 0.289(2) 0.046(4) Uiso d 1 O O2 0.702(6) 0.4865(16) 0.299(3) 0.087(6) Uiso d 1 C C2 0.758(6) 0.6834(13) 0.302(3) 0.049(4) Uiso d 1 C C5 0.952(6) 0.8795(13) 0.334(2) 0.048(4) Uiso d 1 H H5 1.0262 0.9453 0.3455 0.058 Uiso calc 1 C C4 1.047(7) 0.7770(16) 0.366(3) 0.063(5) Uiso d 1 H H2 1.1840 0.7780 0.4048 0.075 Uiso calc 1 C C3 0.960(5) 0.6757(12) 0.345(2) 0.044(4) Uiso d 1 H H3 1.0266 0.6066 0.3577 0.053 Uiso calc 1 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 C6 O1 119(3) O2 C6 C2 122(3) O1 C6 C2 118.5(18) N1 C1 C2 116(3) N1 C1 H1 122.1 C2 C1 H1 122.1 C6 O1 HO 109.5 C5 N1 C1 118.8(17) C3 C2 C1 123(2) C3 C2 C6 120.4(17) C1 C2 C6 117(3) N1 C5 C4 125(3) N1 C5 H5 117.7 C4 C5 H5 117.7 C3 C4 C5 125(4) C3 C4 H2 117.6 C5 C4 H2 117.6 C4 C3 C2 113(3) C4 C3 H3 123.4 C2 C3 H3 123.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C6 O2 1.14(3) C6 O1 1.32(5) C6 C2 1.53(3) C1 N1 1.41(3) C1 C2 1.46(3) C1 H1 0.9300 O1 HO 0.8200 N1 C5 1.26(5) C2 C3 1.40(5) C5 C4 1.36(4) C5 H5 0.9300 C4 C3 1.33(3) C4 H2 0.9300 C3 H3 0.9300