#------------------------------------------------------------------------------ #$Date: 2019-11-10 08:44:52 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515833.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4515833 loop_ _publ_author_name 'Schmitt, Daniel C.' 'Niljianskul, Nootaree' 'Sach, Neal W.' 'Trujillo, John I.' _publ_section_title ; A Parallel Approach to 7-(Hetero)arylpyrazolo[1,5- a]pyrimidin-5-ones. ; _journal_issue 5 _journal_name_full 'ACS combinatorial science' _journal_page_first 256 _journal_page_last 260 _journal_paper_doi 10.1021/acscombsci.8b00032 _journal_volume 20 _journal_year 2018 _chemical_formula_sum 'C12 H8 Br N3 O' _chemical_formula_weight 290.12 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 63.424(2) _cell_angle_beta 86.421(2) _cell_angle_gamma 87.903(2) _cell_formula_units_Z 2 _cell_length_a 3.9214(3) _cell_length_b 11.8486(10) _cell_length_c 13.0394(11) _cell_measurement_reflns_used 8449 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 72.17 _cell_measurement_theta_min 3.80 _cell_volume 540.76(8) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 Venture Diffractometer' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_unetI/netI 0.0230 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9237 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.165 _diffrn_reflns_theta_min 3.795 _diffrn_source 'Microfocus TXS Rotating Anode' _exptl_absorpt_coefficient_mu 5.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.782 _exptl_crystal_description PRISM _exptl_crystal_F_000 288 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_transmission_factor_max 1.0000 _exptl_transmission_factor_min 0.7505 _refine_diff_density_max 0.407 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2103 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0205 _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^)+(0.0236P)^2^+0.4994P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.0527 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2078 _reflns_number_total 2103 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file co8b00032_si_003.cif _cod_data_source_block Z917 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Empirical' was changed to 'empirical' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 4515833 _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 0.581 _shelx_estimated_absorpt_t_max 0.905 _shelx_res_file ; Z917.res created by SHELXL-2014/7 TITL Z917.res in P-1 CELL 1.54178 3.9214 11.8486 13.0394 63.424 86.421 87.903 ZERR 2.000 0.0003 0.0010 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H Br N O UNIT 24 16 2 6 2 L.S. 12 ACTA OMIT 3 -9 2 BOND $H FMAP 2 PLAN 0 WPDB -2 SIZE 0.02 0.04 0.12 DFIX 1.0 N1 H1X TEMP -150 WGHT 0.023600 0.499400 FVAR 0.34117 BR1 3 1.096423 0.257226 0.791904 11.00000 0.02090 0.01458 = 0.02215 -0.01123 -0.00315 0.00444 N1 4 0.643652 0.525706 0.619099 11.00000 0.02084 0.01438 = 0.01333 -0.00862 -0.00153 0.00045 H1X 2 0.643947 0.461125 0.597756 11.00000 -1.20000 N2 4 0.741895 0.592510 0.760786 11.00000 0.01783 0.01250 = 0.01198 -0.00654 -0.00197 0.00074 N3 4 0.893847 0.555223 0.863726 11.00000 0.01983 0.01668 = 0.01303 -0.00760 -0.00390 0.00117 O1 5 0.352862 0.654372 0.462651 11.00000 0.03211 0.01838 = 0.01628 -0.00986 -0.00697 0.00413 C1 1 0.699930 0.925312 0.675318 11.00000 0.02584 0.01460 = 0.01751 -0.00629 -0.00258 0.00126 AFIX 43 H1 2 0.781416 0.948352 0.598465 11.00000 -1.20000 AFIX 0 C2 1 0.693605 1.014122 0.718151 11.00000 0.03012 0.01266 = 0.02633 -0.00819 -0.00472 0.00088 AFIX 43 H2 2 0.771358 1.097489 0.670858 11.00000 -1.20000 AFIX 0 C3 1 0.572677 0.979880 0.830619 11.00000 0.02496 0.01884 = 0.02906 -0.01681 -0.00722 0.00567 AFIX 43 H3 2 0.571575 1.039677 0.860615 11.00000 -1.20000 AFIX 0 C4 1 0.453670 0.858786 0.899179 11.00000 0.02112 0.02195 = 0.02035 -0.01310 -0.00158 0.00422 AFIX 43 H4 2 0.366092 0.836686 0.975269 11.00000 -1.20000 AFIX 0 C5 1 0.461926 0.769911 0.857208 11.00000 0.01737 0.01625 = 0.01865 -0.00904 -0.00195 0.00198 AFIX 43 H5 2 0.382661 0.686806 0.904713 11.00000 -1.20000 AFIX 0 C6 1 0.587224 0.802847 0.744751 11.00000 0.01679 0.01399 = 0.01736 -0.00856 -0.00387 0.00279 C7 1 0.595711 0.710218 0.697663 11.00000 0.01661 0.01227 = 0.01583 -0.00644 0.00109 0.00001 C8 1 0.473987 0.732007 0.595361 11.00000 0.02251 0.01292 = 0.01552 -0.00636 -0.00272 0.00287 AFIX 43 H8 2 0.377568 0.812552 0.549502 11.00000 -1.20000 AFIX 0 C9 1 0.484392 0.637429 0.552572 11.00000 0.01954 0.01601 = 0.01412 -0.00719 -0.00075 0.00005 C10 1 0.775545 0.503063 0.721444 11.00000 0.01531 0.01289 = 0.01353 -0.00723 0.00182 -0.00139 C11 1 0.952758 0.403896 0.801513 11.00000 0.01729 0.01320 = 0.01633 -0.00766 -0.00055 0.00077 C12 1 1.018108 0.441463 0.886762 11.00000 0.01807 0.01463 = 0.01463 -0.00657 -0.00214 0.00057 AFIX 43 H12 2 1.138210 0.390696 0.953471 11.00000 -1.20000 AFIX 0 HKLF 4 REM Z917.res in P-1 REM R1 = 0.0205 for 2078 Fo > 4sig(Fo) and 0.0207 for all 2103 data REM 157 parameters refined using 1 restraints END WGHT 0.0234 0.4741 REM Highest difference peak 0.407, deepest hole -0.342, 1-sigma level 0.064 Q1 1 1.5752 0.2626 0.7866 11.00000 0.05 0.41 Q2 1 1.3509 0.2615 0.7848 11.00000 0.05 0.40 Q3 1 0.7990 0.2620 0.7871 11.00000 0.05 0.38 Q4 1 1.0158 0.4184 0.8427 11.00000 0.05 0.33 Q5 1 0.4936 0.6837 0.5793 11.00000 0.05 0.32 Q6 1 0.7770 0.4245 0.7855 11.00000 0.05 0.29 Q7 1 0.7567 0.3967 0.8104 11.00000 0.05 0.28 Q8 1 0.6773 0.6591 0.7216 11.00000 0.05 0.28 Q9 1 1.1033 0.3262 0.8034 11.00000 0.05 0.28 Q10 1 0.9037 0.4651 0.7469 11.00000 0.05 0.27 Q11 1 1.3483 0.2723 0.8369 11.00000 0.05 0.26 Q12 1 0.5987 0.7605 0.7200 11.00000 0.05 0.26 Q13 1 0.4564 1.1213 0.7688 11.00000 0.05 0.26 Q14 1 0.5922 0.7815 0.8071 11.00000 0.05 0.25 Q15 1 0.4541 0.8018 0.7896 11.00000 0.05 0.25 Q16 1 0.7063 0.9630 0.7016 11.00000 0.05 0.25 Q17 1 0.6023 0.7361 0.6217 11.00000 0.05 0.25 Q18 1 0.7370 0.5488 0.7396 11.00000 0.05 0.24 Q19 1 0.6816 0.8508 0.7156 11.00000 0.05 0.24 Q20 1 0.8481 0.2444 0.7454 11.00000 0.05 0.22 ; _shelx_res_checksum 31977 _shelx_hkl_file ; -1 0 0 11.28 0.54 1 0 0 11.18 0.55 2 0 0 94.21 3.86 2 0 0 102.54 4.06 -3 0 0 0.80 0.19 -3 0 0 0.77 0.12 -3 0 0 0.51 0.19 3 0 0 0.58 0.14 3 0 0 0.50 0.12 3 0 0 0.49 0.35 -4 0 0 21.23 0.85 -4 0 0 21.40 0.95 -4 0 0 20.90 0.93 4 0 0 20.56 0.92 4 0 0 21.18 0.89 4 -1 0 30.04 1.19 4 -1 0 29.03 1.21 -4 1 0 28.50 1.24 -4 1 0 27.20 1.12 -4 1 0 30.62 1.25 3 -1 0 69.62 2.74 3 -1 0 67.63 2.76 3 -1 0 73.71 3.29 -3 1 0 71.78 2.72 -3 1 0 68.66 2.80 -3 1 0 73.67 2.80 2 -1 0 233.02 8.82 2 -1 0 218.85 8.66 1 -1 0 4.88 0.35 1 -1 0 4.91 0.31 1 -1 0 4.83 0.33 -1 1 0 5.11 0.30 0 1 0 229.01 8.67 -1 -1 0 529.18 20.46 1 1 0 550.48 20.36 2 1 0 260.40 10.24 2 1 0 263.74 10.01 -3 -1 0 106.05 4.06 -3 -1 0 107.16 4.01 -3 -1 0 100.41 4.06 3 1 0 108.32 4.64 3 1 0 102.38 4.04 3 1 0 103.99 4.02 -4 -1 0 34.01 1.41 -4 -1 0 33.79 1.35 -4 -1 0 35.07 1.43 4 1 0 33.83 1.38 4 1 0 34.72 1.41 4 -2 0 44.06 1.84 4 -2 0 47.88 1.82 -4 2 0 46.96 1.88 -4 2 0 45.85 1.88 3 -2 0 32.89 1.42 3 -2 0 36.96 1.89 3 -2 0 35.19 1.41 -3 2 0 35.91 1.37 -3 2 0 34.48 1.48 -3 2 0 35.49 1.47 2 -2 0 231.77 9.56 2 -2 0 267.87 9.74 1 -2 0 46.78 1.81 1 -2 0 44.87 1.84 -1 2 0 46.43 1.81 0 -2 0 127.60 4.98 0 -2 0 132.42 4.99 -1 -2 0 5.93 0.46 1 2 0 6.15 0.52 1 2 0 5.83 0.32 -2 -2 0 59.18 2.61 2 2 0 62.10 2.72 2 2 0 61.48 2.45 -3 -2 0 39.09 1.50 -3 -2 0 37.22 1.54 -3 -2 0 36.15 1.54 -3 -2 0 36.14 1.46 3 2 0 38.23 1.50 3 2 0 38.63 2.12 3 2 0 37.43 1.52 -4 -2 0 30.79 1.30 -4 -2 0 31.08 1.26 4 2 0 32.53 1.31 4 2 0 31.87 1.29 4 -3 0 29.40 1.24 -4 3 0 29.71 1.29 -4 3 0 31.92 1.29 3 -3 0 118.85 4.71 3 -3 0 127.27 5.20 -3 3 0 123.02 4.65 -3 3 0 121.22 4.77 -3 3 0 125.22 4.75 -3 3 0 120.93 4.74 2 -3 0 125.05 4.96 2 -3 0 137.44 5.10 -2 3 0 122.75 4.86 -2 3 0 122.55 4.88 1 -3 0 53.89 2.11 1 -3 0 53.50 2.07 1 -3 0 49.83 2.10 -1 3 0 53.60 2.06 0 -3 0 17.95 0.88 0 -3 0 20.11 0.91 0 3 0 20.54 0.76 -1 -3 0 1.57 0.35 1 3 0 1.41 0.18 1 3 0 1.51 0.38 -2 -3 0 142.55 5.84 -2 -3 0 143.02 5.50 -2 -3 0 147.25 5.50 2 3 0 147.61 5.92 2 3 0 138.17 5.49 2 3 0 144.29 5.59 2 3 0 148.41 5.51 -3 -3 0 153.32 5.52 -3 -3 0 142.30 5.54 -3 -3 0 134.07 5.49 3 3 0 144.25 5.52 3 3 0 145.29 6.22 3 3 0 148.40 5.54 3 3 0 143.84 5.54 -4 -3 0 9.90 0.53 -4 -3 0 11.62 0.51 4 3 0 12.46 0.56 4 3 0 10.67 0.53 4 -4 0 40.26 1.65 -4 4 0 43.89 1.70 -4 4 0 39.66 1.67 3 -4 0 2.24 0.57 -3 4 0 2.53 0.34 -3 4 0 2.10 0.33 -3 4 0 2.29 0.32 2 -4 0 45.51 1.90 -2 4 0 41.31 1.66 -2 4 0 39.16 1.67 -2 4 0 40.36 1.69 1 -4 0 40.36 1.59 1 -4 0 37.47 1.67 1 -4 0 40.24 1.69 -1 4 0 41.58 1.59 -1 -4 0 140.23 5.61 1 4 0 141.21 5.36 1 4 0 141.23 5.62 -2 -4 0 5.95 0.32 -2 -4 0 5.31 0.30 -2 -4 0 5.54 0.61 -2 -4 0 6.20 0.32 2 4 0 5.54 0.39 2 4 0 5.49 0.32 2 4 0 5.31 0.31 2 4 0 6.24 0.68 2 4 0 6.41 0.33 -3 -4 0 17.27 0.75 -3 -4 0 16.23 0.72 3 4 0 16.56 1.36 3 4 0 17.03 0.75 3 4 0 16.82 0.77 3 4 0 18.07 0.77 -4 -4 0 34.29 1.42 4 4 0 36.20 1.43 4 4 0 36.90 1.44 4 -5 0 62.35 2.41 -4 5 0 63.61 2.43 -4 5 0 58.68 2.39 -4 5 0 63.04 2.46 3 -5 0 160.41 6.41 -3 5 0 153.75 6.00 -3 5 0 154.69 5.96 -3 5 0 150.81 5.96 2 -5 0 118.74 4.56 -2 5 0 112.46 4.31 -2 5 0 107.20 4.27 -2 5 0 103.94 4.31 -2 5 0 112.68 4.29 1 -5 0 219.79 8.19 1 -5 0 194.38 8.15 1 -5 0 215.72 8.00 0 -5 0 0.16 0.20 -1 -5 0 279.19 10.92 1 5 0 279.30 10.90 1 5 0 280.98 10.58 -2 -5 0 50.82 1.95 -2 -5 0 50.60 1.94 -2 -5 0 49.96 2.41 -2 -5 0 49.29 1.93 2 5 0 49.23 1.93 2 5 0 43.97 2.01 2 5 0 50.82 1.94 2 5 0 49.98 1.94 -3 -5 0 98.62 3.71 -3 -5 0 98.71 3.73 3 5 0 96.33 3.74 3 5 0 99.51 3.73 3 5 0 87.77 4.47 3 5 0 98.01 3.73 -4 -5 0 8.10 0.39 4 5 0 7.21 0.40 4 5 0 8.35 0.40 4 5 0 8.17 0.38 -4 6 0 0.31 0.17 -4 6 0 0.21 0.11 -4 6 0 0.06 0.11 3 -6 0 1.06 0.35 -3 6 0 1.65 0.31 -3 6 0 1.36 0.21 -3 6 0 1.29 0.23 2 -6 0 83.31 3.52 -2 6 0 75.82 3.16 -2 6 0 81.41 3.22 -2 6 0 83.92 3.20 -2 6 0 82.23 3.21 1 -6 0 479.42 17.29 -1 6 0 444.31 17.06 -1 6 0 425.71 17.01 0 -6 0 191.89 7.57 -1 -6 0 136.20 5.33 -1 -6 0 137.18 5.35 -1 -6 0 145.93 5.76 1 6 0 144.84 5.35 1 6 0 136.79 5.33 -2 -6 0 5.80 0.36 -2 -6 0 5.98 0.34 -2 -6 0 6.26 0.77 -2 -6 0 6.35 0.37 2 6 0 6.01 0.33 2 6 0 6.09 0.34 2 6 0 6.35 0.35 -3 -6 0 39.17 1.55 -3 -6 0 38.15 1.57 3 6 0 38.36 1.54 3 6 0 38.49 1.58 3 6 0 40.34 1.57 -4 -6 0 24.51 0.98 4 6 0 22.50 0.99 4 6 0 25.95 0.98 -4 7 0 42.69 1.69 -3 7 0 23.59 1.03 -3 7 0 20.96 0.95 -3 7 0 22.56 1.00 2 -7 0 39.65 1.92 -2 7 0 38.31 1.59 -2 7 0 34.17 1.51 -2 7 0 38.06 1.57 -2 7 0 38.14 1.62 1 -7 0 0.07 0.21 -1 7 0 0.15 0.18 -1 7 0 0.07 0.06 -1 7 0 0.07 0.14 -1 7 0 0.16 0.14 0 -7 0 30.93 1.56 0 7 0 29.13 1.26 0 7 0 28.61 1.16 0 7 0 28.39 1.23 -1 -7 0 146.21 6.05 -1 -7 0 147.05 5.56 -1 -7 0 143.72 5.55 1 7 0 150.61 5.55 1 7 0 140.19 5.53 1 7 0 141.79 5.61 1 7 0 149.34 5.64 -2 -7 0 157.46 6.69 -2 -7 0 160.91 6.00 -2 -7 0 158.11 5.99 -2 -7 0 165.12 6.00 2 7 0 161.30 6.00 2 7 0 140.38 6.08 2 7 0 154.83 5.98 -3 -7 0 8.19 0.43 -3 -7 0 7.76 0.41 3 7 0 7.98 0.42 3 7 0 8.13 0.45 -4 -7 0 7.63 0.34 4 7 0 7.81 0.33 4 7 0 7.12 0.34 -3 8 0 3.02 0.33 -3 8 0 3.33 0.35 2 -8 0 31.58 1.64 -2 8 0 31.01 1.34 -2 8 0 30.02 1.35 -2 8 0 32.49 1.40 1 -8 0 60.56 2.73 -1 8 0 62.41 2.46 -1 8 0 60.21 2.39 -1 8 0 55.74 2.38 0 -8 0 162.34 6.31 0 -8 0 150.64 5.80 0 -8 0 149.99 5.82 0 8 0 151.47 5.78 0 8 0 144.69 5.89 0 8 0 154.22 5.87 -1 -8 0 3.28 0.26 -1 -8 0 3.13 0.64 -1 -8 0 3.71 0.31 1 8 0 3.66 0.40 1 8 0 3.36 0.35 1 8 0 3.54 0.26 -2 -8 0 1.34 0.17 -2 -8 0 1.66 0.19 -2 -8 0 0.71 0.41 -2 -8 0 1.64 0.21 2 8 0 1.19 0.16 2 8 0 1.45 0.19 -3 -8 0 28.43 1.23 -3 -8 0 32.84 1.22 3 8 0 31.59 1.21 3 8 0 28.47 1.23 -3 9 0 77.27 2.95 -3 9 0 73.68 2.95 -2 9 0 122.79 4.64 -2 9 0 114.79 4.63 -2 9 0 119.88 4.67 1 -9 0 -0.07 0.21 1 -9 0 0.33 0.15 -1 9 0 -0.01 0.25 -1 9 0 0.15 0.19 0 -9 0 14.09 0.64 0 -9 0 14.66 0.68 0 -9 0 14.28 1.10 0 9 0 15.16 0.75 0 9 0 14.93 0.78 0 9 0 14.69 0.62 -1 -9 0 23.45 1.00 -1 -9 0 22.67 1.53 -1 -9 0 23.97 0.99 1 9 0 24.49 0.98 1 9 0 22.47 1.07 1 9 0 23.45 1.09 -2 -9 0 86.01 3.25 -2 -9 0 82.89 3.25 2 9 0 82.94 3.25 -3 -9 0 17.16 0.68 -3 -9 0 16.22 0.68 3 9 0 16.19 0.69 3 9 0 15.36 0.64 -3 10 0 0.50 0.15 2 -10 0 43.79 1.76 -2 10 0 40.76 1.77 -2 10 0 45.58 1.82 -2 10 0 47.11 1.86 1 -10 0 124.10 4.93 1 -10 0 120.85 5.40 -1 10 0 136.03 5.05 -1 10 0 132.79 5.00 0 -10 0 67.38 3.25 0 -10 0 70.27 2.69 0 -10 0 68.57 2.71 0 10 0 69.15 2.71 0 10 0 68.90 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4 13 5.30 0.45 0 -4 -13 25.92 1.07 0 -4 -13 26.56 1.06 0 4 13 24.25 1.07 -1 -4 -13 29.16 1.19 -1 -4 -13 30.15 1.19 -1 -4 -13 29.52 1.19 1 4 13 28.10 1.22 -2 -4 -13 21.51 0.88 -2 -4 -13 21.65 0.87 2 4 13 20.88 0.91 2 4 13 21.72 0.87 -3 -4 -13 38.78 1.41 -3 -4 -13 35.73 1.40 3 4 13 34.75 1.42 2 -5 -13 78.23 3.04 2 -5 -13 76.88 3.02 -2 5 13 78.88 3.09 -2 5 13 79.55 3.09 -2 5 13 81.57 3.07 1 -5 -13 10.86 0.50 1 -5 -13 10.64 0.53 -1 5 13 10.42 0.47 -1 5 13 10.31 0.59 -1 5 13 10.82 0.59 -1 5 13 11.49 0.63 0 -5 -13 74.43 2.86 0 -5 -13 73.31 2.88 0 5 13 72.82 2.87 0 5 13 75.55 2.91 0 5 13 73.44 2.93 -1 -5 -13 28.45 1.14 -1 -5 -13 26.43 1.14 -1 -5 -13 28.17 1.15 1 5 13 28.74 1.17 -2 -5 -13 14.25 0.62 -2 -5 -13 15.39 0.62 2 5 13 13.67 0.65 -3 -5 -13 0.43 0.08 3 5 13 0.29 0.09 2 -6 -13 4.52 0.29 -2 6 13 4.34 0.40 -2 6 13 4.38 0.34 -2 6 13 4.79 0.35 1 -6 -13 19.78 0.82 1 -6 -13 19.83 0.85 -1 6 13 19.95 0.91 -1 6 13 19.07 0.89 -1 6 13 19.22 0.92 0 -6 -13 12.34 0.55 0 -6 -13 11.75 0.57 0 6 13 11.36 0.63 0 6 13 11.91 0.56 0 6 13 12.41 0.64 -1 -6 -13 88.70 3.38 -1 -6 -13 88.31 3.38 1 6 13 85.76 3.39 -2 -6 -13 51.55 1.96 -2 -6 -13 54.54 1.98 -2 -6 -13 49.54 1.98 2 6 13 47.99 2.01 -3 -6 -13 7.82 0.33 -3 -6 -13 8.32 0.35 3 6 13 8.89 0.38 2 -7 -13 15.38 0.68 -2 7 13 15.73 0.71 -2 7 13 16.85 0.74 -2 7 13 16.31 0.76 1 -7 -13 65.70 2.44 1 -7 -13 61.83 2.46 -1 7 13 61.46 2.48 -1 7 13 64.33 2.53 -1 7 13 62.30 2.51 0 -7 -13 40.75 1.57 0 -7 -13 39.72 1.59 0 7 13 40.29 1.64 0 7 13 36.53 1.62 0 7 13 40.14 1.56 -1 -7 -13 50.85 2.00 -1 -7 -13 50.77 1.98 1 7 13 50.15 2.00 -2 -7 -13 17.50 0.74 -2 -7 -13 19.19 0.74 -2 -7 -13 17.89 0.73 2 7 13 16.62 0.77 -3 -7 -13 11.97 0.47 3 7 13 11.73 0.50 2 -8 -13 16.77 0.70 -2 8 13 15.66 0.69 -2 8 13 17.45 0.78 -2 8 13 17.62 0.75 1 -8 -13 4.02 0.29 -1 8 13 3.84 0.36 -1 8 13 5.06 0.41 0 -8 -13 86.70 3.33 0 -8 -13 85.10 3.30 0 8 13 85.98 3.28 0 8 13 88.27 3.37 0 8 13 86.22 3.53 0 8 13 83.47 3.36 -1 -8 -13 50.89 1.91 -1 -8 -13 49.50 1.89 1 8 13 44.87 1.90 1 8 13 47.11 1.89 -2 -8 -13 51.90 1.93 -2 -8 -13 50.23 1.92 2 8 13 46.77 1.94 -2 9 13 69.68 2.68 -2 9 13 68.93 2.70 1 -9 -13 72.98 2.78 -1 9 13 74.92 2.82 -1 9 13 67.11 2.88 -1 9 13 72.58 2.84 0 -9 -13 22.24 0.96 0 -9 -13 23.23 0.93 0 9 13 24.01 1.23 0 9 13 22.47 1.01 0 9 13 22.51 1.00 -1 -9 -13 2.58 0.24 -1 -9 -13 2.14 0.20 1 9 13 2.40 0.21 1 9 13 2.57 0.54 1 9 13 2.43 0.28 1 9 13 2.12 0.28 -2 -9 -13 10.08 0.44 -2 -9 -13 9.77 0.44 2 9 13 9.86 0.45 1 -10 -13 3.04 0.23 -1 10 13 3.35 0.45 -1 10 13 3.94 0.35 -1 10 13 3.73 0.29 0 -10 -13 14.04 0.63 0 -10 -13 14.04 0.60 0 10 13 14.27 0.66 0 10 13 14.22 0.70 0 10 13 15.91 0.92 -1 -10 -13 77.67 2.82 -1 -10 -13 73.49 2.80 1 10 13 70.33 2.99 1 10 13 71.44 2.82 1 10 13 71.72 2.83 1 10 13 72.66 2.77 -2 -10 -13 32.32 1.24 -2 -10 -13 31.65 1.24 2 10 13 30.92 1.24 1 -11 -13 69.39 2.77 -1 11 13 78.47 2.83 -1 11 13 73.68 2.78 -1 11 13 68.23 2.85 0 -11 -13 27.17 1.09 0 11 13 27.80 1.15 0 11 13 25.50 1.09 0 11 13 28.42 1.30 -1 -11 -13 0.68 0.12 -1 -11 -13 0.77 0.10 1 11 13 0.96 0.18 1 11 13 0.67 0.35 -2 -11 -13 0.54 0.08 -2 -11 -13 0.41 0.08 -1 12 13 0.29 0.16 0 -12 -13 38.33 1.54 0 12 13 41.23 1.59 0 12 13 39.51 1.69 -1 -12 -13 13.79 0.57 -1 -12 -13 13.56 0.54 1 12 13 13.39 0.59 1 12 13 12.77 0.72 0 0 -14 5.85 0.29 0 0 -14 6.70 0.29 0 0 14 6.70 0.32 -1 0 -14 11.94 0.49 1 0 14 11.83 0.51 1 -1 -14 0.46 0.09 -1 1 14 0.54 0.18 -1 1 14 0.44 0.09 0 -1 -14 21.95 0.93 0 -1 -14 24.11 0.94 0 1 14 24.11 0.95 -1 -1 -14 18.51 0.83 -1 -1 -14 21.70 0.82 1 1 14 22.26 0.84 1 1 14 20.40 0.85 1 -2 -14 47.80 1.85 1 -2 -14 49.28 1.85 -1 2 14 45.96 1.84 -1 2 14 45.83 1.84 -1 2 14 50.14 1.91 0 -2 -14 5.85 0.29 0 -2 -14 5.24 0.30 0 -2 -14 6.47 0.31 0 2 14 6.02 0.35 0 2 14 5.81 0.33 -1 -2 -14 0.13 0.09 -1 -2 -14 0.16 0.09 1 2 14 0.33 0.14 -2 -2 -14 0.94 0.12 2 2 14 0.93 0.12 1 -3 -14 1.00 0.13 1 -3 -14 0.62 0.13 -1 3 14 0.88 0.16 -1 3 14 0.77 0.22 -1 3 14 0.85 0.12 0 -3 -14 1.34 0.20 0 -3 -14 1.73 0.19 0 3 14 1.37 0.21 0 3 14 1.59 0.21 -1 -3 -14 42.59 1.72 -1 -3 -14 47.60 1.72 1 3 14 41.75 1.74 -2 -3 -14 23.24 0.95 -2 -3 -14 24.02 0.94 2 3 14 25.18 0.98 2 -4 -14 1.23 0.15 -2 4 14 1.31 0.20 1 -4 -14 47.33 1.81 1 -4 -14 48.58 1.83 -1 4 14 46.23 1.79 -1 4 14 46.62 1.87 -1 4 14 44.05 1.83 -1 4 14 46.83 1.85 0 -4 -14 77.39 2.98 0 -4 -14 74.39 2.97 0 4 14 78.32 2.98 0 4 14 78.13 3.01 -1 -4 -14 1.31 0.18 -1 -4 -14 1.46 0.18 -1 -4 -14 1.29 0.17 1 4 14 1.59 0.20 -2 -4 -14 1.16 0.13 -2 -4 -14 1.01 0.13 2 4 14 1.05 0.14 2 -5 -14 48.93 1.87 -2 5 14 46.57 1.88 -2 5 14 48.82 1.89 -2 5 14 48.83 1.87 1 -5 -14 16.80 0.71 1 -5 -14 16.56 0.68 -1 5 14 15.79 0.74 -1 5 14 16.90 0.74 -1 5 14 16.16 0.74 -1 5 14 15.40 0.64 0 -5 -14 23.35 0.97 0 -5 -14 23.62 0.95 0 5 14 22.07 0.95 0 5 14 23.43 1.01 -1 -5 -14 42.00 1.64 -1 -5 -14 42.23 1.64 1 5 14 41.16 1.66 -2 -5 -14 60.62 2.46 -2 -5 -14 68.12 2.46 2 5 14 63.65 2.49 2 -6 -14 52.04 2.00 -2 6 14 50.46 2.02 -2 6 14 52.91 2.01 -2 6 14 51.73 2.01 1 -6 -14 62.23 2.35 1 -6 -14 59.04 2.32 -1 6 14 61.46 2.38 -1 6 14 61.05 2.38 -1 6 14 57.56 2.36 0 -6 -14 32.68 1.28 0 -6 -14 33.11 1.30 0 6 14 28.66 1.30 0 6 14 32.61 1.34 0 6 14 32.82 1.28 -1 -6 -14 4.02 0.26 -1 -6 -14 3.63 0.27 1 6 14 3.85 0.28 -2 -6 -14 0.25 0.10 -2 -6 -14 0.28 0.09 2 6 14 0.27 0.13 2 -7 -14 14.02 0.59 -2 7 14 14.56 0.62 -2 7 14 13.92 0.63 1 -7 -14 24.81 0.99 1 -7 -14 23.81 0.95 -1 7 14 23.92 1.04 -1 7 14 25.57 1.03 -1 7 14 21.84 0.98 0 -7 -14 38.58 1.57 0 -7 -14 41.04 1.55 0 7 14 39.59 1.53 0 7 14 37.49 1.59 0 7 14 40.34 1.61 -1 -7 -14 59.67 2.25 -1 -7 -14 58.29 2.26 1 7 14 56.08 2.26 -2 -7 -14 13.45 0.56 2 7 14 13.15 0.58 1 -8 -14 28.07 1.15 -1 8 14 27.72 1.19 -1 8 14 29.91 1.21 0 -8 -14 17.77 0.76 0 -8 -14 18.00 0.74 0 8 14 18.16 0.81 0 8 14 17.16 0.80 -1 -8 -14 0.61 0.12 -1 -8 -14 0.55 0.12 1 8 14 0.57 0.17 1 8 14 0.64 0.13 -2 -8 -14 11.21 0.46 -2 -8 -14 9.70 0.43 2 8 14 11.00 0.47 1 -9 -14 0.10 0.10 -1 9 14 0.31 0.17 -1 9 14 0.37 0.20 0 -9 -14 46.16 1.78 0 -9 -14 46.09 1.81 0 9 14 45.19 1.83 0 9 14 46.40 1.84 -1 -9 -14 44.39 1.73 -1 -9 -14 43.78 1.71 1 9 14 44.51 1.70 1 9 14 43.67 1.75 -2 -9 -14 34.18 1.31 -2 -9 -14 33.69 1.29 2 9 14 34.51 1.31 2 9 14 32.21 1.31 1 -10 -14 37.86 1.51 -1 10 14 40.65 1.56 -1 10 14 38.14 1.53 0 -10 -14 10.71 0.47 0 -10 -14 10.15 0.44 0 10 14 9.57 0.70 0 10 14 10.32 0.52 0 10 14 10.69 0.50 -1 -10 -14 0.71 0.12 -1 -10 -14 0.50 0.09 1 10 14 0.57 0.14 -2 -10 -14 16.22 0.65 -1 11 14 11.53 0.54 0 -11 -14 4.64 0.25 0 11 14 5.05 0.32 0 11 14 3.63 0.48 0 11 14 4.21 0.24 -1 -11 -14 117.61 4.40 -1 -11 -14 113.66 4.38 0 -12 -14 24.06 0.96 0 12 14 24.79 0.99 0 -2 -15 18.28 0.72 0 2 15 17.73 0.73 -1 -2 -15 27.90 1.07 1 2 15 27.42 1.09 1 -3 -15 42.56 1.63 1 -3 -15 41.48 1.62 -1 3 15 43.01 1.66 0 -3 -15 6.89 0.31 0 3 15 6.37 0.32 0 3 15 6.50 0.34 -1 -3 -15 5.29 0.26 1 3 15 5.62 0.30 1 3 15 5.42 0.29 1 -4 -15 7.64 0.35 1 -4 -15 7.72 0.34 -1 4 15 7.65 0.37 -1 4 15 7.57 0.38 0 -4 -15 39.15 1.50 0 -4 -15 38.19 1.51 0 4 15 37.29 1.53 0 4 15 40.12 1.54 0 4 15 38.51 1.51 -1 -4 -15 36.69 1.39 1 4 15 36.64 1.43 1 4 15 34.04 1.41 1 -5 -15 30.21 1.18 1 -5 -15 30.97 1.20 -1 5 15 29.40 1.21 -1 5 15 30.56 1.21 0 -5 -15 7.37 0.36 0 -5 -15 7.44 0.35 0 5 15 7.26 0.41 0 5 15 6.64 0.35 0 5 15 7.32 0.34 -1 -5 -15 0.63 0.09 -1 -5 -15 0.84 0.11 1 5 15 0.97 0.13 1 5 15 0.91 0.17 1 -6 -15 2.43 0.16 1 -6 -15 2.50 0.20 -1 6 15 2.43 0.25 0 -6 -15 31.44 1.24 0 -6 -15 31.38 1.23 0 6 15 30.16 1.21 0 6 15 31.60 1.28 -1 -6 -15 40.59 1.58 -1 -6 -15 40.66 1.59 1 6 15 40.35 1.60 1 6 15 42.08 1.63 -2 -6 -15 24.60 0.91 2 6 15 22.30 0.93 1 -7 -15 10.78 0.48 -1 7 15 11.73 0.52 -1 7 15 10.34 0.50 0 -7 -15 25.49 1.04 0 -7 -15 26.07 1.06 0 7 15 27.19 1.10 -1 -7 -15 0.30 0.10 -1 -7 -15 0.38 0.09 1 7 15 0.35 0.10 1 7 15 0.25 0.14 1 -8 -15 17.41 0.70 -1 8 15 17.70 0.74 -1 8 15 16.37 0.72 0 -8 -15 33.11 1.32 0 -8 -15 33.95 1.34 0 8 15 34.61 1.37 -1 -8 -15 51.65 1.96 -1 -8 -15 51.88 1.95 1 8 15 50.34 1.99 1 8 15 48.74 1.94 1 -9 -15 17.45 0.71 -1 9 15 17.38 0.73 -1 9 15 17.85 0.73 0 -9 -15 11.21 0.48 0 -9 -15 11.58 0.51 0 9 15 11.71 0.53 -1 -9 -15 5.86 0.27 -1 -9 -15 5.54 0.28 1 9 15 5.24 0.31 0 -10 -15 88.24 3.35 0 10 15 87.38 3.36 -1 -10 -15 13.82 0.56 -1 -10 -15 13.97 0.57 0 -6 -16 0.07 0.07 0 -6 -16 0.05 0.06 0 6 16 0.19 0.12 0 -7 -16 53.13 2.03 0 -7 -16 50.99 2.02 0 7 16 54.59 2.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 59019 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Br1 Br 1.09642(4) 0.25723(2) 0.79190(2) 0.01811(8) Uani 1 1 d . . N1 N 0.6437(4) 0.52571(14) 0.61910(12) 0.0153(3) Uani 1 1 d D . H1X H 0.644(6) 0.4611(18) 0.5978(18) 0.018 Uiso 1 1 d D U N2 N 0.7419(4) 0.59251(13) 0.76079(12) 0.0137(3) Uani 1 1 d . . N3 N 0.8938(4) 0.55522(14) 0.86373(12) 0.0160(3) Uani 1 1 d . . O1 O 0.3529(3) 0.65437(12) 0.46265(10) 0.0213(3) Uani 1 1 d . . C1 C 0.6999(5) 0.92531(17) 0.67532(15) 0.0196(4) Uani 1 1 d . . H1 H 0.7814 0.9484 0.5985 0.024 Uiso 1 1 calc R U C2 C 0.6936(5) 1.01412(17) 0.71815(17) 0.0231(4) Uani 1 1 d . . H2 H 0.7714 1.0975 0.6709 0.028 Uiso 1 1 calc R U C3 C 0.5727(5) 0.97988(18) 0.83062(17) 0.0219(4) Uani 1 1 d . . H3 H 0.5716 1.0397 0.8606 0.026 Uiso 1 1 calc R U C4 C 0.4537(5) 0.85879(18) 0.89918(16) 0.0199(4) Uani 1 1 d . . H4 H 0.3661 0.8367 0.9753 0.024 Uiso 1 1 calc R U C5 C 0.4619(4) 0.76991(17) 0.85721(15) 0.0170(3) Uani 1 1 d . . H5 H 0.3827 0.6868 0.9047 0.020 Uiso 1 1 calc R U C6 C 0.5872(4) 0.80285(16) 0.74475(14) 0.0154(3) Uani 1 1 d . . C7 C 0.5957(4) 0.71022(16) 0.69766(14) 0.0149(3) Uani 1 1 d . . C8 C 0.4740(5) 0.73201(16) 0.59536(14) 0.0170(3) Uani 1 1 d . . H8 H 0.3776 0.8126 0.5495 0.020 Uiso 1 1 calc R U C9 C 0.4844(4) 0.63743(16) 0.55257(14) 0.0164(3) Uani 1 1 d . . C10 C 0.7755(4) 0.50306(15) 0.72144(14) 0.0135(3) Uani 1 1 d . . C11 C 0.9528(4) 0.40390(16) 0.80151(14) 0.0152(3) Uani 1 1 d . . C12 C 1.0181(4) 0.44146(16) 0.88676(14) 0.0157(3) Uani 1 1 d . . H12 H 1.1382 0.3907 0.9535 0.019 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02090(12) 0.01458(11) 0.02215(11) -0.01123(8) -0.00315(7) 0.00444(7) N1 0.0208(7) 0.0144(7) 0.0133(6) -0.0086(6) -0.0015(5) 0.0004(6) N2 0.0178(7) 0.0125(7) 0.0120(6) -0.0065(5) -0.0020(5) 0.0007(5) N3 0.0198(7) 0.0167(7) 0.0130(6) -0.0076(6) -0.0039(5) 0.0012(6) O1 0.0321(7) 0.0184(6) 0.0163(6) -0.0099(5) -0.0070(5) 0.0041(5) C1 0.0258(9) 0.0146(8) 0.0175(8) -0.0063(7) -0.0026(7) 0.0013(7) C2 0.0301(10) 0.0127(8) 0.0263(9) -0.0082(7) -0.0047(8) 0.0009(7) C3 0.0250(9) 0.0188(9) 0.0291(9) -0.0168(8) -0.0072(7) 0.0057(7) C4 0.0211(9) 0.0219(9) 0.0203(8) -0.0131(7) -0.0016(7) 0.0042(7) C5 0.0174(8) 0.0163(8) 0.0187(8) -0.0090(7) -0.0020(6) 0.0020(6) C6 0.0168(8) 0.0140(8) 0.0174(8) -0.0086(7) -0.0039(6) 0.0028(6) C7 0.0166(8) 0.0123(8) 0.0158(8) -0.0064(6) 0.0011(6) 0.0000(6) C8 0.0225(9) 0.0129(8) 0.0155(8) -0.0064(6) -0.0027(6) 0.0029(6) C9 0.0195(8) 0.0160(8) 0.0141(8) -0.0072(7) -0.0008(6) 0.0001(6) C10 0.0153(8) 0.0129(8) 0.0135(7) -0.0072(6) 0.0018(6) -0.0014(6) C11 0.0173(8) 0.0132(8) 0.0163(8) -0.0077(6) -0.0006(6) 0.0008(6) C12 0.0181(8) 0.0146(8) 0.0146(7) -0.0066(6) -0.0021(6) 0.0006(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 C9 N1 C10 121.87(14) C9 N1 H1X 118.9(14) C10 N1 H1X 118.9(14) C10 N2 N3 112.11(13) C10 N2 C7 122.54(14) N3 N2 C7 125.15(14) C12 N3 N2 103.78(13) C2 C1 C6 120.28(17) C2 C1 H1 119.9 C6 C1 H1 119.9 C3 C2 C1 119.56(17) C3 C2 H2 120.2 C1 C2 H2 120.2 C4 C3 C2 120.29(17) C4 C3 H3 119.9 C2 C3 H3 119.9 C5 C4 C3 120.32(17) C5 C4 H4 119.8 C3 C4 H4 119.8 C4 C5 C6 119.85(16) C4 C5 H5 120.1 C6 C5 H5 120.1 C1 C6 C5 119.68(16) C1 C6 C7 119.42(15) C5 C6 C7 120.88(15) C8 C7 N2 116.77(15) C8 C7 C6 124.69(16) N2 C7 C6 118.53(14) C7 C8 C9 122.93(16) C7 C8 H8 118.5 C9 C8 H8 118.5 O1 C9 N1 121.08(15) O1 C9 C8 122.93(16) N1 C9 C8 115.97(15) N2 C10 N1 119.76(15) N2 C10 C11 106.37(14) N1 C10 C11 133.86(16) C10 C11 C12 105.10(15) C10 C11 Br1 126.45(13) C12 C11 Br1 128.33(13) N3 C12 C11 112.63(15) N3 C12 H12 123.7 C11 C12 H12 123.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C11 1.8621(17) N1 C9 1.369(2) N1 C10 1.370(2) N1 H1X 0.924(16) N2 C10 1.368(2) N2 N3 1.3791(19) N2 C7 1.387(2) N3 C12 1.324(2) O1 C9 1.240(2) C1 C2 1.394(3) C1 C6 1.394(2) C1 H1 0.9500 C2 C3 1.391(3) C2 H2 0.9500 C3 C4 1.387(3) C3 H3 0.9500 C4 C5 1.386(3) C4 H4 0.9500 C5 C6 1.399(2) C5 H5 0.9500 C6 C7 1.477(2) C7 C8 1.355(2) C8 C9 1.457(2) C8 H8 0.9500 C10 C11 1.374(2) C11 C12 1.409(2) C12 H12 0.9500