#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:27:02 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227264 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035852.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_4035852 loop_ _publ_author_name 'Vila, Carlos' 'Rostoll-Berenguer, Jaume' 'S\'anchez-Garc\'ia, Rub\'en' 'Blay, Gonzalo' 'Fern\'andez, Isabel' 'Mu\~noz, M Carmen' 'Pedro, Jos\'e R' _publ_section_title ; Enantioselective Synthesis of 2-Amino-1,1-diarylalkanes Bearing a Carbocyclic Ring Substituted Indole through Asymmetric Catalytic Reaction of Hydroxyindoles with Nitroalkenes. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6397 _journal_page_last 6407 _journal_paper_doi 10.1021/acs.joc.8b00612 _journal_volume 83 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_sum 'C16 H12 Br N2 O3' _chemical_formula_weight 360.19 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 103.299(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.2991(3) _cell_length_b 5.68602(17) _cell_length_c 15.9291(4) _cell_measurement_reflns_used 3391 _cell_measurement_temperature 200(1) _cell_measurement_theta_max 23.1970 _cell_measurement_theta_min 3.8040 _cell_volume 731.52(4) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 200(1) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measurement_device_type 'SuperNova Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.929 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11372 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.903 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.912 _diffrn_reflns_theta_min 3.817 _exptl_absorpt_coefficient_mu 2.824 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Empirical absorption correction' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.635 _exptl_crystal_description prismatic _exptl_crystal_F_000 362 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.440 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.074 _refine_ls_abs_structure_details ; Flack x determined using 1082 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.006(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 3814 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0414 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.0802 _reflns_Friedel_coverage 0.777 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.872 _reflns_number_gt 3019 _reflns_number_total 3814 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00612_si_003.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 4035852 _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 0.677 _shelx_estimated_absorpt_t_max 0.849 _shelxl_version_number 2014-1 _shelx_res_file ; TITL in P2(1) CELL 0.71073 8.299098 5.686019 15.929101 90.0000 103.2987 90.0000 zerr 2 0.000254 0.000166 0.000444 0.0000 0.0029 0.0000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O BR UNIT 32 24 4 6 2 MERG 2 OMIT -3.00 180.00 FMAP 2 PLAN 25 SIZE 0.060 0.060 0.150 ACTA 50.00 L.S. 8 WGHT 0.030400 FVAR 5.25079 BR 5 0.633464 0.555149 0.045589 11.00000 0.03436 0.04724 = 0.03029 0.00032 0.00366 -0.01086 O1 4 1.068060 1.585964 0.323781 11.00000 0.04219 0.02765 = 0.02749 0.00622 0.00815 0.01094 O2 4 1.594440 1.345022 0.272751 11.00000 0.03487 0.04915 = 0.04558 -0.00847 0.00150 0.00500 O3 4 1.426657 1.625127 0.220790 11.00000 0.04483 0.03462 = 0.06187 -0.00930 0.01556 -0.00032 N1 3 1.285075 1.195710 0.581177 11.00000 0.03902 0.04671 = 0.02275 0.00643 0.00174 -0.00589 N2 3 1.464184 1.418612 0.230012 11.00000 0.03277 0.03583 = 0.02732 -0.00975 0.01585 -0.00563 C1 1 1.182378 1.257005 0.219915 11.00000 0.03069 0.02525 = 0.02717 -0.00264 0.01195 -0.00060 C2 1 1.052253 1.081285 0.174117 11.00000 0.02798 0.02842 = 0.01856 0.00197 0.00650 0.00186 C3 1 0.891949 1.100774 0.187482 11.00000 0.03493 0.04084 = 0.03164 -0.00967 0.01188 0.00177 C4 1 0.769538 0.947196 0.149471 11.00000 0.02518 0.04530 = 0.03899 -0.00494 0.00893 0.00046 C5 1 0.803959 0.770529 0.097880 11.00000 0.03032 0.03326 = 0.02289 0.00441 -0.00031 -0.00324 C6 1 0.958167 0.743206 0.082237 11.00000 0.03259 0.03217 = 0.02469 -0.00479 0.00706 0.00017 C7 1 1.083134 0.901652 0.121296 11.00000 0.02523 0.03910 = 0.03036 -0.00215 0.00912 0.00120 C8 1 1.338820 1.238022 0.185754 11.00000 0.03411 0.03300 = 0.03171 -0.00971 0.01334 -0.00362 C9 1 1.216597 1.232356 0.316792 11.00000 0.02704 0.02664 = 0.02314 0.00264 0.00887 -0.00083 C10 1 1.304288 1.035102 0.358965 11.00000 0.03235 0.02387 = 0.03510 -0.00282 0.01267 0.00324 C11 1 1.336840 1.006534 0.447304 11.00000 0.02554 0.02895 = 0.04085 0.00509 0.00534 0.00381 C12 1 1.276920 1.178294 0.494580 11.00000 0.02276 0.02961 = 0.02670 0.00275 0.00524 -0.00518 C13 1 1.209198 1.397945 0.597313 11.00000 0.04320 0.05059 = 0.02629 -0.01218 0.01392 -0.01181 C14 1 1.150395 1.514261 0.523070 11.00000 0.03750 0.03025 = 0.03267 -0.00908 0.01419 -0.00318 C15 1 1.191237 1.379267 0.455629 11.00000 0.02277 0.02432 = 0.02517 -0.00167 0.00927 -0.00450 C16 1 1.159496 1.400534 0.365375 11.00000 0.02586 0.02064 = 0.02375 -0.00171 0.00643 -0.00196 H8A 2 1.393780 1.091795 0.200121 11.00000 0.01789 H6 2 0.983202 0.618593 0.046401 11.00000 0.02408 H3 2 0.877886 1.244444 0.222256 11.00000 0.04932 H1 2 1.138101 1.427911 0.203038 11.00000 0.02478 H10 2 1.342177 0.925586 0.324735 11.00000 0.02410 H13 2 1.214215 1.446643 0.652688 11.00000 0.03500 H8B 2 1.320191 1.275776 0.125101 11.00000 0.04153 H4 2 0.658982 0.968512 0.150424 11.00000 0.05288 H11 2 1.390553 0.855041 0.472345 11.00000 0.04279 H14 2 1.101130 1.642784 0.518240 11.00000 0.02876 H1N 2 1.328421 1.121761 0.617425 11.00000 0.02932 H7 2 1.197677 0.860890 0.113162 11.00000 0.03465 HKLF 4 REM in P2(1) REM R1 = 0.0414 for 3019 Fo > 4sig(Fo) and 0.0622 for all 3814 data REM 247 parameters refined using 1 restraints END WGHT 0.0262 0.0000 REM Highest difference peak 0.440, deepest hole -0.424, 1-sigma level 0.074 Q1 1 1.2564 1.0370 0.4730 11.00000 0.05 0.39 Q2 1 0.8922 1.0443 0.1414 11.00000 0.05 0.39 Q3 1 0.6492 0.4736 0.1019 11.00000 0.05 0.34 Q4 1 0.9824 1.0527 0.1907 11.00000 0.05 0.32 Q5 1 0.6141 0.6410 0.0997 11.00000 0.05 0.31 Q6 1 0.5998 0.5616 -0.0194 11.00000 0.05 0.30 Q7 1 1.3492 1.0563 0.2586 11.00000 0.05 0.29 Q8 1 0.7065 0.2771 -0.0028 11.00000 0.05 0.28 Q9 1 1.0734 0.3417 0.0620 11.00000 0.05 0.28 Q10 1 0.4986 0.4741 0.0543 11.00000 0.05 0.28 Q11 1 1.1338 1.5197 0.3529 11.00000 0.05 0.28 Q12 1 1.0195 1.0707 0.1350 11.00000 0.05 0.27 Q13 1 1.4008 1.7817 0.1338 11.00000 0.05 0.27 Q14 1 1.1630 1.3869 0.4079 11.00000 0.05 0.27 Q15 1 1.0015 0.5684 -0.0296 11.00000 0.05 0.26 Q16 1 1.1716 1.3262 0.3417 11.00000 0.05 0.26 Q17 1 0.6433 0.7688 0.0520 11.00000 0.05 0.26 Q18 1 1.3847 0.9929 0.3913 11.00000 0.05 0.25 Q19 1 0.6549 0.4402 -0.0075 11.00000 0.05 0.25 Q20 1 0.9255 0.5540 0.0213 11.00000 0.05 0.25 Q21 1 0.6751 0.6196 0.0985 11.00000 0.05 0.24 Q22 1 1.0247 1.5612 0.2945 11.00000 0.05 0.24 Q23 1 1.2183 1.2651 0.2770 11.00000 0.05 0.24 Q24 1 1.5822 1.5533 0.1660 11.00000 0.05 0.24 Q25 1 1.2008 1.2580 0.4667 11.00000 0.05 0.24 ; _shelx_res_checksum 15090 _shelx_hkl_file ; 0 -7 0 429.694 420.184 1 0 -7 -1 698.023 523.340 1 0 -7 1 136.599 408.521 1 0 -7 2-91.3244 311.136 1 0 -7 -2 67.7629 342.805 1 0 -7 2 806.375 493.094 2 0 -7 -3 62.5387 388.945 1 0 -7 3 362.413 389.241 2 0 -7 3 923.738 591.031 1 0 -7 4-231.156 415.921 1 0 -7 -4 379.819 467.351 1 0 -7 5 836.323 528.318 2 0 -7 -5 3386.95 933.839 1 0 -7 5 2215.96 830.516 1 0 -7 6 3102.14 914.711 2 0 -7 6 3541.82 1076.75 1 0 -7 -6 2797.96 877.719 1 0 -7 7 2922.13 976.253 2 0 -7 8 300.749 459.864 2 0 -6 0 17519.3 1885.69 1 0 -6 0 16442.6 1519.35 2 0 -6 1 3077.90 807.088 1 0 -6 -1 5267.75 1039.61 1 0 -6 1 3535.52 740.109 2 0 -6 -1 3475.28 707.256 2 0 -6 -2 6604.68 1163.04 1 0 -6 2 7347.85 1140.06 2 0 -6 2 6389.79 1198.18 1 0 -6 3 3077.48 788.636 2 0 -6 3 3356.19 926.845 1 0 -6 -3 2177.10 721.373 1 0 -6 -4 244.107 310.123 1 0 -6 4 1337.85 633.311 1 0 -6 4 978.400 561.529 2 0 -6 5 510.331 436.335 2 0 -6 -5 392.669 355.836 1 0 -6 -6-478.198 401.273 1 0 -6 6 122.903 458.421 2 0 -6 -7 2235.65 799.590 1 0 -6 7 874.185 551.317 2 0 -6 -8 972.404 556.892 1 0 -6 8 2182.65 767.094 2 0 -6 9 1753.38 769.276 2 0 -6 -9 3313.28 872.810 1 0 -6 -10 2687.90 875.676 1 0 -6 10 2211.37 851.753 2 0 -6 11 510.304 667.651 2 0 -6 -11 1058.52 516.940 7 0 -6 -11 2029.85 797.347 1 0 -6 -12 1148.38 643.490 1 0 -5 0 125.487 239.328 2 0 -5 0-113.347 339.015 1 0 -5 1 1130.40 512.985 1 0 -5 1 1140.62 395.729 2 0 -5 -1 990.841 486.204 1 0 -5 -1 416.833 221.797 2 0 -5 -2 5822.32 1000.46 1 0 -5 -2 4770.65 697.812 2 0 -5 2 7000.39 997.165 2 0 -5 2 7133.81 1093.08 1 0 -5 -3 14776.8 1565.59 1 0 -5 -3 11987.4 1038.09 2 0 -5 3 13382.5 1388.67 2 0 -5 4 18610.7 1689.14 2 0 -5 -4 18704.1 1231.83 2 0 -5 -4 17439.2 1694.01 1 0 -5 5 12662.2 1439.54 2 0 -5 -5 12060.3 1433.36 1 0 -5 -6 1937.47 655.460 1 0 -5 6-456.550 450.676 2 0 -5 -7 4685.93 948.507 1 0 -5 7 3737.16 866.779 2 0 -5 -8 12505.2 1501.04 1 0 -5 8 11696.0 1517.30 2 0 -5 9 2673.45 793.825 2 0 -5 -9 3790.76 852.597 1 0 -5 10 112.654 371.932 2 0 -5 -10-417.865 385.936 1 0 -5 11 826.087 588.097 2 0 -5 -11 499.158 396.671 7 0 -5 -11-44.8080 326.904 1 0 -5 -12 990.596 520.150 7 0 -5 -12-172.682 391.910 1 0 -5 12-688.060 712.153 2 0 -5 -13 395.164 282.976 7 0 -5 13 1.31302 342.611 2 0 -5 -13 744.440 438.184 1 0 -5 -14 2836.06 726.700 7 0 -5 -14 3584.60 930.853 1 0 -5 14 1631.14 791.069 2 0 -4 0 16097.9 1199.25 2 0 -4 0 13695.8 1313.87 1 0 -4 1 26494.0 1603.34 2 0 -4 -1 25676.9 1429.09 2 0 -4 -1 27529.0 1837.13 1 0 -4 1 27206.6 1848.46 1 0 -4 2 14565.8 1240.39 2 0 -4 2 12200.0 756.761 6 0 -4 -2 12275.0 952.075 2 0 -4 -2 16208.3 1428.31 1 0 -4 -3 16008.3 1030.51 2 0 -4 3 15298.8 802.110 9 0 -4 3 17644.3 1425.74 2 0 -4 -3 15856.2 1411.82 1 0 -4 -4 3131.87 671.182 1 0 -4 4 3394.68 661.799 2 0 -4 4 3324.14 363.406 9 0 -4 -4 2863.02 433.230 2 0 -4 5 577.724 345.896 2 0 -4 -5 1113.88 431.085 1 0 -4 -6 525.717 298.522 1 0 -4 6-132.866 326.622 2 0 -4 7 3825.48 791.672 2 0 -4 -7 3128.68 690.999 1 0 -4 -8 15235.4 1460.96 1 0 -4 8 15605.4 1594.96 2 0 -4 9 10404.0 1333.25 2 0 -4 -9 7531.16 1041.51 1 0 -4 10 8022.44 1218.36 2 0 -4 -10 10761.7 1267.45 1 0 -4 -10 9639.64 1093.46 7 0 -4 11 1128.38 526.049 2 0 -4 -11 1466.84 551.084 1 0 -4 -11 1942.43 552.834 7 0 -4 12 6860.46 1198.14 2 0 -4 -12 6018.97 952.066 7 0 -4 -12 8645.48 1215.17 1 0 -4 13 3552.14 889.978 2 0 -4 -13 4169.10 898.036 1 0 -4 -13 4712.56 865.755 7 0 -4 -14 4633.80 898.474 7 0 -4 14 6160.03 1190.20 2 0 -4 -15 581.086 438.063 7 0 -4 15 180.543 332.138 2 0 -4 16 398.879 332.583 2 0 -4 -16 1546.88 648.136 7 0 -4 17-166.751 471.945 2 0 -3 0 230.478 244.227 1 0 -3 0-52.0628 132.956 2 0 -3 1 11330.3 906.569 2 0 -3 1 9910.69 616.119 9 0 -3 -1 10619.7 981.652 1 0 -3 -1 10306.6 768.520 2 0 -3 1 9896.08 554.929 6 0 -3 2 24531.9 905.121 9 0 -3 -2 22441.8 1435.48 1 0 -3 2 23821.7 1371.46 2 0 -3 2 24152.7 1000.49 6 0 -3 -2 23500.8 1088.94 2 0 -3 3 7823.53 491.791 9 0 -3 -3 7610.12 842.995 1 0 -3 3 7067.17 797.746 2 0 -3 -3 7473.44 575.870 2 0 -3 3 6872.16 601.368 6 0 -3 4 58603.3 2350.65 2 0 -3 -4 55464.2 2284.06 1 0 -3 4 52571.6 1264.30 9 0 -3 -4 55212.3 1444.15 2 0 -3 -5 8709.25 570.833 4 0 -3 5 8742.92 979.128 2 0 -3 5 7816.79 515.591 9 0 -3 -5 9341.09 959.640 1 0 -3 6 26770.0 1739.10 2 0 -3 -6 24453.3 1577.43 1 0 -3 -6 25492.9 776.510 4 0 -3 -6 24158.7 1952.71 5 0 -3 -7 29219.2 1754.14 1 0 -3 -7 30908.1 2298.03 5 0 -3 7 26677.3 1785.54 2 0 -3 -8 21847.5 1543.81 1 0 -3 8 17667.6 1521.80 2 0 -3 -8 19832.5 1954.80 5 0 -3 -9 1493.92 431.620 7 0 -3 -9 1976.85 526.926 1 0 -3 -9 955.372 540.081 5 0 -3 9 1818.28 586.266 2 0 -3 -10 19052.9 1414.70 7 0 -3 -10 19958.6 2066.83 5 0 -3 10 17165.8 1580.39 2 0 -3 -10 17884.9 1481.62 1 0 -3 -11 937.693 407.710 7 0 -3 -11 1033.65 461.811 1 0 -3 -11 539.324 569.470 5 0 -3 11 975.232 445.560 2 0 -3 -12 9153.84 1513.54 5 0 -3 12 11053.5 1367.52 2 0 -3 -12 8820.24 1050.35 7 0 -3 -13 1179.19 419.814 7 0 -3 13 1655.63 612.366 2 0 -3 -13 491.625 419.964 5 0 -3 -14 9459.02 1679.95 5 0 -3 14 10592.5 1438.89 2 0 -3 -14 11346.2 1284.85 7 0 -3 -15 12522.6 1949.58 5 0 -3 15 11330.6 1502.28 2 0 -3 -15 10663.7 1323.32 7 0 -3 -16 2896.82 967.008 5 0 -3 16 2252.49 724.767 2 0 -3 -16 3194.01 780.653 7 0 -3 -17 4396.26 931.969 7 0 -3 -17 6061.18 1384.89 5 0 -3 17 3417.24 894.306 2 0 -3 18 2481.28 778.302 2 0 -3 -18 4191.04 957.422 7 0 -3 19-439.236 512.237 2 0 -2 0 73153.1 1471.53 9 0 -2 0 69268.9 1067.72 6 0 -2 0 73816.6 1754.30 2 0 -2 0 75633.7 1861.07 8 0 -2 1 29598.0 832.391 9 0 -2 1 30753.3 1223.09 2 0 -2 -1 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725.464 1 -3 -7 5 1943.78 764.689 2 -3 -7 5 1244.56 727.645 1 3 -7 -4 764.469 580.535 1 -3 -7 4-122.419 562.622 1 -3 -7 3 319.331 573.649 1 3 -7 -3 1654.90 740.080 1 3 -7 -2 1222.90 600.653 1 -3 -7 2 699.563 492.486 1 3 -7 -1 597.306 505.574 2 -3 -7 1 1094.05 604.437 1 3 -7 -1 1142.14 654.823 1 -3 -7 0 284.755 454.700 1 3 -7 0 870.946 557.577 2 3 -7 0 1782.57 713.828 1 3 -7 1 3388.14 1024.21 1 -3 -7 -1 2563.94 906.541 1 3 -7 1 623.860 521.858 2 3 -7 2 1178.01 596.516 1 3 -7 2 896.523 685.045 2 -3 -7 -2 683.228 519.745 1 -3 -7 -3 508.454 440.708 1 3 -7 3 2238.38 820.467 1 3 -7 3 1085.13 621.342 2 3 -7 4 577.118 478.776 2 -3 -7 -4 917.810 678.487 1 3 -7 4 1483.75 698.416 1 -3 -7 -5 335.885 419.920 1 3 -7 5 88.0512 461.825 1 3 -6 -12-116.599 517.165 7 -3 -6 12 719.249 519.514 2 -3 -6 11 505.969 504.161 2 3 -6 -11 132.684 366.869 1 -3 -6 10 3830.33 1086.22 2 3 -6 -10 518.958 416.389 1 -3 -6 9 4034.34 1022.05 2 3 -6 -9 3295.59 888.956 1 3 -6 -8 2333.70 772.899 1 -3 -6 8 2159.15 807.226 2 3 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477.178 1 3 -6 7-91.7666 379.355 1 3 -6 7 621.159 524.647 2 3 -6 8 213.954 573.242 2 3 -6 8 607.412 627.946 1 -3 -6 -8 1485.44 717.485 1 3 -6 9 1052.11 675.921 2 -3 -6 -9 505.773 443.498 1 -3 -6 -10 1029.44 568.170 1 -3 -6 -11 995.920 585.423 1 3 -5 -16 3398.90 939.587 7 3 -5 -15 1011.68 691.115 7 -3 -5 15 664.146 586.739 2 3 -5 -14 2066.60 715.574 7 -3 -5 14 1338.18 726.479 2 3 -5 -14 2199.86 736.246 1 3 -5 -13 2911.06 871.117 7 -3 -5 13 3785.62 970.438 2 3 -5 -13 5599.07 1134.59 1 3 -5 -12 5990.42 1110.84 7 -3 -5 12 6863.00 1283.91 2 3 -5 -12 8566.43 1357.89 1 -3 -5 11-226.475 387.911 2 3 -5 -11 317.047 410.972 1 -3 -5 10-166.806 389.992 2 3 -5 -10-780.564 499.666 1 -3 -5 9 2218.51 753.959 2 3 -5 -9 3031.73 871.334 1 -3 -5 8 436.575 437.858 2 3 -5 -8 5.57256 288.322 1 3 -5 -7 710.300 487.285 1 -3 -5 7 649.599 397.457 2 3 -5 -6 2006.80 643.498 1 -3 -5 6 1550.75 575.392 2 3 -5 -5 11503.4 1383.98 1 -3 -5 5 12813.5 1433.82 2 3 -5 -4 19995.3 1800.10 1 -3 -5 4 17698.2 1622.49 2 -3 -5 3 1671.95 519.542 2 3 -5 -3 2029.05 625.107 1 -3 -5 2 10226.1 1153.55 2 3 -5 -2 8995.27 1146.98 2 3 -5 -2 10096.6 1270.09 1 -3 -5 2 11178.3 1379.64 1 3 -5 -1 6062.57 1007.71 1 -3 -5 1 6199.26 876.455 2 3 -5 -1 5978.06 952.431 2 -3 -5 1 6850.10 1119.46 1 3 -5 0 3947.73 848.406 1 -3 -5 0 4220.25 848.102 1 -3 -5 0 5338.02 779.252 2 3 -5 0 5265.80 925.653 2 -3 -5 -1 786.397 295.968 2 3 -5 1 1150.27 503.364 1 -3 -5 -1 344.567 259.721 1 3 -5 1 973.992 481.689 2 3 -5 2 2780.96 724.551 1 -3 -5 -2 2202.12 674.907 1 3 -5 2 2646.99 664.395 2 3 -5 3 679.098 499.846 2 -3 -5 -3-416.796 543.011 5 3 -5 3 44.8686 289.803 1 -3 -5 -3-19.0870 279.844 1 3 -5 4 1154.36 528.060 2 3 -5 4 386.299 366.113 1 -3 -5 -4 120.257 411.320 5 -3 -5 -4 328.430 345.058 1 3 -5 5 4007.71 910.893 2 -3 -5 -5 3795.62 825.602 1 -3 -5 -5 5497.28 1206.19 5 3 -5 5 4559.23 917.934 1 3 -5 6 7021.09 1207.82 2 -3 -5 -6 9264.34 1255.97 1 -3 -5 -6 9145.45 1569.87 5 -3 -5 -7 6096.75 1052.40 1 -3 -5 -7 5219.64 1262.36 5 3 -5 7 4362.74 1017.97 2 -3 -5 -8 3111.82 787.891 1 3 -5 8 987.372 560.072 2 -3 -5 -8 1885.25 769.454 5 3 -5 9 2567.64 807.917 2 -3 -5 -9 3859.45 1189.05 5 -3 -5 -9 6057.54 1061.16 1 -3 -5 -10 3050.81 1119.03 5 3 -5 10 2537.02 859.579 2 -3 -5 -10 4316.51 918.919 1 -3 -5 -11 43.1996 480.360 5 -3 -5 -11 851.754 437.078 1 3 -5 12-138.206 536.143 2 -3 -5 -12 1244.32 599.485 1 -3 -5 -12 953.131 692.966 5 -3 -5 -13-389.273 466.342 1 3 -4 -18 551.207 425.368 7 3 -4 -17 2851.42 841.922 7 -3 -4 17 2893.65 916.487 2 3 -4 -16 2205.43 739.835 7 -3 -4 16 2203.63 847.679 2 3 -4 -15 210.716 413.444 7 -3 -4 15 186.338 514.570 2 3 -4 -14 317.778 323.796 7 -3 -4 14 417.111 484.496 2 3 -4 -13 647.793 427.399 7 -3 -4 13 2148.46 692.685 2 3 -4 -13 1171.08 602.557 1 3 -4 -12 3662.91 846.815 7 -3 -4 12 4962.46 1062.08 2 3 -4 -12 5039.48 1007.97 1 3 -4 -11 5107.41 953.810 7 3 -4 -11 3691.49 810.160 1 -3 -4 11 3232.69 866.239 2 3 -4 -10 21464.9 1829.94 1 -3 -4 10 24398.6 2080.06 2 3 -4 -9 12570.7 1375.44 1 -3 -4 9 11928.7 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742.233 493.483 2 4 -4 -14 6632.09 1203.21 7 -4 -4 14 3228.92 948.763 2 4 -4 -13 5105.92 1030.36 7 -4 -4 13 3695.95 956.520 2 4 -4 -12 8881.86 1267.88 7 -4 -4 12 6572.42 1169.98 2 4 -4 -12 7305.50 1158.06 1 4 -4 -11 8245.59 1214.39 7 -4 -4 11 8352.04 1292.44 2 4 -4 -11 9813.24 1306.47 1 -4 -4 10 4739.50 983.428 2 4 -4 -10 3563.87 814.507 1 4 -4 -9 6355.65 1000.54 1 -4 -4 9 7771.99 1193.77 2 -4 -4 8 2972.42 755.150 2 4 -4 -8 3595.52 768.098 1 4 -4 -8 2868.37 521.053 4 -4 -4 7 1540.64 553.112 2 4 -4 -7 1905.38 562.942 1 4 -4 -7 751.386 305.701 4 -4 -4 6 185.275 338.665 2 4 -4 -6 249.439 245.865 4 4 -4 -6 514.510 377.747 1 4 -4 -5 1847.75 458.955 4 4 -4 -5 2176.54 586.736 1 -4 -4 5 1128.09 471.645 2 4 -4 -4 14994.5 1381.36 1 4 -4 -4 17003.6 1381.26 4 -4 -4 4 15484.6 1431.51 2 4 -4 -3 3025.99 639.142 1 -4 -4 3 4328.84 732.123 2 -4 -4 3 4014.25 681.799 5 4 -4 -2 22767.0 1668.34 1 -4 -4 2 23734.8 1742.73 5 -4 -4 2 22529.7 1589.06 2 -4 -4 1 1861.91 522.203 1 -4 -4 1 2049.55 564.810 5 -4 -4 1 1936.74 476.243 2 4 -4 -1 2137.88 535.790 1 4 -4 0 21458.7 1752.10 2 4 -4 0 19271.7 1521.90 1 -4 -4 0 23820.1 1768.15 1 -4 -4 0 20156.5 1793.85 5 -4 -4 0 21900.2 1446.99 2 4 -4 1 15921.4 1541.87 2 4 -4 1 16631.3 1405.99 1 -4 -4 -1 15861.1 1436.11 1 -4 -4 -1 12297.4 1477.82 5 -4 -4 -1 14732.9 1128.27 2 -4 -4 -2 3294.43 676.229 1 -4 -4 -2 3792.73 554.990 2 -4 -4 -2 3159.20 822.353 5 4 -4 2 3245.95 648.691 1 4 -4 2 3824.71 805.756 2 4 -4 3 1247.21 411.027 1 -4 -4 -3 1940.94 721.002 5 -4 -4 -3 1466.97 490.963 1 4 -4 3 1138.73 528.870 2 4 -4 4 5807.43 873.866 1 -4 -4 -4 6257.63 1173.12 5 -4 -4 -4 4781.87 785.961 1 4 -4 4 6684.74 1084.14 2 4 -4 5-2.77759 348.320 2 -4 -4 -5 836.622 415.298 1 4 -4 5 356.617 253.192 1 -4 -4 -5 303.564 438.654 5 4 -4 6 835.335 522.003 2 -4 -4 -6 979.351 414.436 1 -4 -4 -6 861.428 611.450 5 4 -4 7 1245.79 573.391 2 -4 -4 -7 1933.31 558.957 1 -4 -4 -7 1571.71 748.009 5 4 -4 8 9644.70 1426.59 2 -4 -4 -8 7694.59 1454.70 5 -4 -4 -8 9626.11 1127.12 1 4 -4 9 6871.84 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1740.77 784.049 6 10 0 0-154.221 385.923 4 -10 0 -1 287.990 526.315 6 10 0 1 78.8279 577.312 4 -10 0 -2 380.143 467.232 6 10 0 2 768.781 577.910 4 -10 0 -3 3121.59 945.599 6 10 0 3 1848.93 782.721 4 -10 0 -4 3301.66 994.012 6 10 0 4 2583.24 938.841 4 -10 1 13 5830.73 1298.68 8 10 1 -12 1888.91 768.255 4 -10 1 12 2576.11 941.715 8 -10 1 11 3420.92 1100.26 6 10 1 -11 3471.06 1119.00 4 -10 1 11 3509.70 957.199 8 -10 1 10 688.692 633.417 6 10 1 -10 945.667 630.410 4 -10 1 10 1163.17 646.463 8 -10 1 9 484.251 443.256 6 10 1 -9 1981.87 882.476 4 -10 1 9 2145.41 755.059 8 -10 1 8 7.62373 506.244 6 10 1 -8 85.8341 456.428 4 -10 1 8-3.37979 459.543 8 -10 1 7 303.696 540.783 6 10 1 -7 218.117 644.019 4 -10 1 7 132.579 379.933 8 -10 1 6 4151.42 1141.20 6 10 1 -6 4798.48 1217.02 4 -10 1 6 4724.35 978.846 8 -10 1 5 2795.14 962.849 6 10 1 -5 2591.30 943.988 4 -10 1 5 752.406 505.610 8 -10 1 4 6130.93 1311.11 6 10 1 -4 6872.23 1374.87 4 -10 1 4 5173.54 1012.58 8 -10 1 3 772.439 554.651 6 10 1 -3 989.609 767.120 4 -10 1 2 1201.11 595.372 6 10 1 -2 1659.26 760.653 4 -10 1 1 5480.43 1346.83 6 10 1 -1 6079.93 1314.45 4 -10 1 0 4019.84 1119.79 6 10 1 0 4272.22 1151.90 4 -10 1 -1 3455.16 1116.27 6 10 1 1 1680.66 727.334 4 -10 1 -2 535.309 403.206 6 10 1 2 2266.97 815.659 4 10 1 3-8.51764 488.478 4 10 1 4 846.676 586.804 4 10 1 5 499.678 535.974 4 -10 2 11-162.050 512.747 8 -10 2 10 1903.45 719.566 8 -10 2 9 2726.07 1044.42 6 10 2 -9 2086.44 875.940 4 -10 2 9 1546.27 661.267 8 -10 2 8 1744.90 765.534 6 10 2 -8 1722.57 858.797 4 -10 2 8 853.045 594.079 8 -10 2 7 58.8057 416.687 6 10 2 -7 578.976 574.505 4 -10 2 7-101.239 534.394 8 -10 2 6 1957.53 798.347 6 10 2 -6 4048.03 1112.42 4 -10 2 6 4027.44 1078.31 8 -10 2 5 4776.43 1336.42 6 10 2 -5 6892.25 1450.81 4 -10 2 5 5151.21 1099.19 8 -10 2 4-194.791 561.346 6 10 2 -4 673.316 625.561 4 -10 2 4 206.497 430.492 8 -10 2 3 498.432 540.616 6 10 2 -3 750.889 612.182 4 -10 2 3 1782.53 675.903 8 -10 2 2 221.163 519.530 6 10 2 -2 1.44636 475.132 4 -10 2 2-74.6049 259.975 8 -10 2 1 264.009 459.454 6 10 2 -1 442.379 509.915 4 -10 2 0 1263.73 630.592 6 10 2 0 2111.26 860.858 4 10 2 1 1257.83 769.963 4 10 2 2 2803.03 924.486 4 10 2 3 147.357 422.488 4 10 2 4 1952.66 817.423 4 10 2 5 1556.23 735.623 4 -10 3 8 639.593 508.705 8 -10 3 7-73.6546 433.717 8 -10 3 6-118.561 402.849 8 -10 3 5 740.200 603.869 8 10 3 -4 2733.50 1018.91 4 -10 3 4 1107.32 621.931 8 10 3 -3 1470.33 770.312 4 -10 3 3 1346.49 615.007 8 10 3 -2 1423.18 721.850 4 10 3 -1 1710.25 723.176 4 10 3 0 1697.60 815.557 4 10 3 1 1623.89 849.520 4 10 3 2-200.958 454.897 4 -11 -2 7-69.7365 421.997 6 -11 -2 6-1187.55 737.258 6 -11 -2 5 719.405 578.191 6 -11 -2 4-1335.89 692.505 6 -11 -2 3 2204.44 863.344 6 -11 -2 2-80.1137 425.779 6 -11 -2 1 1584.04 742.961 6 -11 -1 6 2724.40 1054.26 6 -11 -1 5 701.909 709.084 6 -11 -1 4 359.908 589.653 6 -11 -1 3 3371.51 1072.36 6 -11 -1 2 731.560 645.323 6 -11 0 12 4399.06 1142.55 8 -11 1 10 1530.84 737.460 8 -11 1 9-39.9571 458.776 8 -11 1 8 2946.04 920.880 8 -11 2 7 565.010 578.411 8 -11 2 6 252.569 501.503 8 -11 2 5 1089.66 756.449 8 0 0 0 0.00 0.00 0 TITL carlos18 in P2(1) REM P2(1) (#4 in standard setting) CELL 0.71073 8.299098 5.686019 15.929101 90.0000 103.2987 90.0000 ZERR 3.00 0.000254 0.000166 0.000444 0.0000 0.0029 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END ; _shelx_hkl_checksum 18767 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Br Br 0.63346(6) 0.55515(12) 0.04559(3) 0.03791(16) Uani 1 1 d O1 O 1.0681(4) 1.5860(7) 0.32378(19) 0.0324(8) Uani 1 1 d O2 O 1.5944(5) 1.3450(7) 0.2728(2) 0.0445(10) Uani 1 1 d O3 O 1.4267(6) 1.6251(7) 0.2208(3) 0.0466(12) Uani 1 1 d N1 N 1.2851(6) 1.1957(9) 0.5812(3) 0.0370(11) Uani 1 1 d N2 N 1.4642(6) 1.4186(8) 0.2300(3) 0.0305(11) Uani 1 1 d C1 C 1.1824(6) 1.2570(9) 0.2199(3) 0.0268(10) Uani 1 1 d C2 C 1.0523(5) 1.0813(11) 0.1741(2) 0.0248(10) Uani 1 1 d C3 C 0.8919(6) 1.1008(10) 0.1875(3) 0.0351(14) Uani 1 1 d C4 C 0.7695(7) 0.9472(10) 0.1495(4) 0.0362(13) Uani 1 1 d C5 C 0.8040(6) 0.7705(9) 0.0979(3) 0.0299(11) Uani 1 1 d C6 C 0.9582(6) 0.7432(9) 0.0822(3) 0.0297(11) Uani 1 1 d C7 C 1.0831(6) 0.9017(9) 0.1213(3) 0.0311(11) Uani 1 1 d C8 C 1.3388(7) 1.2380(10) 0.1858(4) 0.0320(12) Uani 1 1 d C9 C 1.2166(6) 1.2324(8) 0.3168(3) 0.0251(10) Uani 1 1 d C10 C 1.3043(5) 1.0351(12) 0.3590(3) 0.0296(10) Uani 1 1 d C11 C 1.3368(6) 1.0065(9) 0.4473(3) 0.0322(14) Uani 1 1 d C12 C 1.2769(6) 1.1783(8) 0.4946(3) 0.0264(11) Uani 1 1 d C13 C 1.2092(7) 1.3979(11) 0.5973(4) 0.0391(14) Uani 1 1 d C14 C 1.1504(7) 1.5143(11) 0.5231(4) 0.0325(13) Uani 1 1 d C15 C 1.1912(5) 1.3793(8) 0.4556(3) 0.0235(10) Uani 1 1 d C16 C 1.1595(6) 1.4005(8) 0.3654(3) 0.0233(10) Uani 1 1 d H8A H 1.394(5) 1.092(9) 0.200(2) 0.018(12) Uiso 1 1 d H6 H 0.983(5) 0.619(8) 0.046(3) 0.024(13) Uiso 1 1 d H3 H 0.878(7) 1.244(10) 0.222(3) 0.049(17) Uiso 1 1 d H1 H 1.138(5) 1.428(8) 0.203(3) 0.025(12) Uiso 1 1 d H10 H 1.342(6) 0.926(8) 0.325(3) 0.024(13) Uiso 1 1 d H13 H 1.214(6) 1.447(8) 0.653(3) 0.035(15) Uiso 1 1 d H8B H 1.320(7) 1.276(9) 0.125(4) 0.042(16) Uiso 1 1 d H4 H 0.659(7) 0.969(9) 0.150(3) 0.053(19) Uiso 1 1 d H11 H 1.391(6) 0.855(10) 0.472(3) 0.043(16) Uiso 1 1 d H14 H 1.101(6) 1.643(9) 0.518(4) 0.029(16) Uiso 1 1 d H1N H 1.328(6) 1.122(9) 0.617(3) 0.029(17) Uiso 1 1 d H7 H 1.198(7) 0.861(9) 0.113(3) 0.035(14) Uiso 1 1 d 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 Br 0.0344(3) 0.0472(3) 0.0303(2) 0.0003(3) 0.00366(17) -0.0109(3) O1 0.0422(19) 0.028(2) 0.0275(15) 0.0062(19) 0.0082(13) 0.0109(18) O2 0.035(2) 0.049(2) 0.046(2) -0.008(2) 0.0015(18) 0.0050(19) O3 0.045(3) 0.035(3) 0.062(3) -0.0093(19) 0.016(2) -0.0003(18) N1 0.039(3) 0.047(3) 0.023(2) 0.006(2) 0.002(2) -0.006(2) N2 0.033(3) 0.036(3) 0.027(2) -0.010(2) 0.016(2) -0.006(2) C1 0.031(3) 0.025(3) 0.027(3) -0.003(2) 0.012(2) -0.001(2) C2 0.028(2) 0.028(3) 0.0186(19) 0.002(2) 0.0065(16) 0.002(2) C3 0.035(3) 0.041(4) 0.032(2) -0.010(3) 0.012(2) 0.002(2) C4 0.025(3) 0.045(3) 0.039(3) -0.005(2) 0.009(2) 0.000(2) C5 0.030(3) 0.033(3) 0.023(2) 0.004(2) 0.000(2) -0.003(2) C6 0.033(3) 0.032(3) 0.025(3) -0.005(2) 0.007(2) 0.000(2) C7 0.025(3) 0.039(3) 0.030(3) -0.002(2) 0.009(2) 0.001(2) C8 0.034(3) 0.033(3) 0.032(3) -0.010(3) 0.013(2) -0.004(2) C9 0.027(3) 0.027(3) 0.023(2) 0.003(2) 0.009(2) -0.001(2) C10 0.032(2) 0.024(3) 0.035(2) -0.003(3) 0.0127(19) 0.003(3) C11 0.026(2) 0.029(4) 0.041(3) 0.005(2) 0.005(2) 0.004(2) C12 0.023(2) 0.030(3) 0.027(3) 0.003(2) 0.005(2) -0.005(2) C13 0.043(3) 0.051(4) 0.026(3) -0.012(3) 0.014(2) -0.012(3) C14 0.038(3) 0.030(4) 0.033(3) -0.009(2) 0.014(2) -0.003(2) C15 0.023(2) 0.024(2) 0.025(2) -0.002(2) 0.0093(19) -0.0045(19) C16 0.026(2) 0.021(2) 0.024(2) -0.0017(19) 0.0064(19) -0.0020(19) 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' Br Br -0.2901 2.4595 '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 C13 N1 C12 109.5(5) O2 N2 O3 124.9(5) O2 N2 C8 117.1(5) O3 N2 C8 118.0(5) C9 C1 C2 111.9(4) C9 C1 C8 112.5(4) C2 C1 C8 110.5(4) C7 C2 C3 117.8(5) C7 C2 C1 124.3(4) C3 C2 C1 117.9(5) C4 C3 C2 121.1(5) C5 C4 C3 119.8(5) C6 C5 C4 121.7(5) C6 C5 Br 118.5(4) C4 C5 Br 119.7(4) C5 C6 C7 118.2(5) C2 C7 C6 121.4(5) N2 C8 C1 109.7(4) C16 C9 C10 119.1(4) C16 C9 C1 120.0(4) C10 C9 C1 120.8(4) C11 C10 C9 122.3(5) C10 C11 C12 117.3(5) N1 C12 C11 130.9(5) N1 C12 C15 106.7(5) C11 C12 C15 122.4(4) C14 C13 N1 109.8(5) C13 C14 C15 107.3(5) C16 C15 C12 118.4(4) C16 C15 C14 134.8(5) C12 C15 C14 106.7(4) O1 C16 C9 118.9(4) O1 C16 C15 120.7(4) C9 C16 C15 120.4(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br C5 1.911(5) O1 C16 1.377(6) O2 N2 1.212(6) O3 N2 1.215(6) N1 C13 1.364(8) N1 C12 1.369(6) N2 C8 1.515(7) C1 C9 1.510(6) C1 C2 1.528(7) C1 C8 1.523(7) C2 C7 1.384(7) C2 C3 1.399(6) C3 C4 1.370(7) C4 C5 1.369(7) C5 C6 1.368(7) C6 C7 1.406(7) C9 C16 1.381(6) C9 C10 1.419(7) C10 C11 1.380(7) C11 C12 1.393(7) C12 C15 1.412(6) C13 C14 1.345(8) C14 C15 1.423(7) C15 C16 1.406(6)