#------------------------------------------------------------------------------ #$Date: 2021-11-05 00:58:55 +0200 (Fri, 05 Nov 2021) $ #$Revision: 270307 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/92/7129203.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_7129203 loop_ _publ_author_name 'Kim, Youyoung' 'Kim, Dongwook' 'Chang, Sukbok' _publ_section_title ; Ir(iii)-Catalysed electrooxidative intramolecular dehydrogenative C--H/N--H coupling for the synthesis of N--H indoles ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D1CC05882G _journal_year 2021 _chemical_formula_moiety 'C11 H11 N O' _chemical_formula_sum 'C11 H11 N O' _chemical_formula_weight 173.21 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-10-12 deposited with the CCDC. 2021-11-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.083(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.9622(9) _cell_length_b 5.7301(4) _cell_length_c 15.9848(13) _cell_measurement_reflns_used 5247 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.10 _cell_measurement_theta_min 2.65 _cell_volume 876.77(12) _computing_cell_refinement 'Bruker APEXIII' _computing_data_collection 'Bruker APEXIII' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ORTEP _computing_publication_material CIFTAB _computing_structure_refinement SHELXL _computing_structure_solution SHELXS _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'PHOTON II 14' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_unetI/netI 0.0772 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9045 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.497 _diffrn_reflns_theta_min 2.652 _diffrn_source 'I\^I1/4S 3.0 Microfocus' _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.3951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.312 _exptl_crystal_description plate _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.158 _exptl_crystal_size_mid 0.087 _exptl_crystal_size_min 0.024 _refine_diff_density_max 0.613 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef 0.46(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 121 _refine_ls_number_reflns 1590 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.1139 _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^)+(0.1435P)^2^+1.4958P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2674 _refine_ls_wR_factor_ref 0.2778 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1341 _reflns_number_total 1590 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc05882g2.cif _cod_data_source_block A21255_014 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7129203 _shelx_shelxl_version_number 2018/3 _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 0.987 _shelx_estimated_absorpt_t_max 0.998 _shelx_res_file ; TITL A21255_014 in P2(1)/n A21255_014.res created by SHELXL-2018/3 at 20:08:16 on 09-Oct-2021 CELL 0.71073 9.96220 5.73010 15.98480 90.0000 106.0826 90.0000 ZERR 4.00 0.00090 0.00040 0.00130 0.0000 0.0031 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O UNIT 44 44 4 4 OMIT -9 2 15 OMIT 0 0 18 OMIT -2 5 5 OMIT -4 1 17 OMIT -3 1 18 OMIT -11 1 12 OMIT 6 1 12 OMIT 3 1 16 OMIT 9 1 5 OMIT -5 1 18 OMIT -3 51 ACTA LIST 4 TEMP -100.000 SIZE 0.024 0.087 0.158 CONF MERG 2 L.S. 7 BOND $H FMAP 2 EQIV $1 -x+1, -y, -z+1 HTAB N1 O12_$1 PLAN 5 WGHT 0.143500 1.495800 EXTI 0.462010 FVAR 0.56809 N1 3 0.583155 0.097249 0.308504 11.00000 0.02976 0.02265 = 0.02632 0.00313 0.00913 0.00678 AFIX 43 H1 2 0.618276 -0.033636 0.334242 11.00000 -1.20000 AFIX 0 C2 1 0.609486 0.190516 0.236171 11.00000 0.02350 0.02797 = 0.02392 -0.00574 0.00949 -0.00044 AFIX 43 H2 2 0.670346 0.123304 0.206387 11.00000 -1.20000 AFIX 0 C3 1 0.536837 0.393420 0.212120 11.00000 0.01916 0.02504 = 0.02259 -0.00188 0.00276 -0.00626 C4 1 0.461832 0.431730 0.275033 11.00000 0.01762 0.01983 = 0.02086 0.00420 -0.00080 -0.00464 C5 1 0.492799 0.241943 0.334222 11.00000 0.01852 0.01920 = 0.02203 -0.00288 0.00182 0.00120 C6 1 0.435482 0.224149 0.404119 11.00000 0.02234 0.02292 = 0.01964 0.00539 0.00219 0.00132 AFIX 43 H6 2 0.455570 0.094014 0.442389 11.00000 -1.20000 AFIX 0 C7 1 0.348026 0.402202 0.416319 11.00000 0.01677 0.02413 = 0.01975 -0.00112 -0.00001 -0.00345 C8 1 0.317411 0.593249 0.358355 11.00000 0.02023 0.01822 = 0.02710 0.00140 0.00337 0.00277 AFIX 43 H8 2 0.257836 0.713828 0.367843 11.00000 -1.20000 AFIX 0 C9 1 0.372309 0.608302 0.288190 11.00000 0.02265 0.01792 = 0.02413 0.00305 -0.00197 -0.00204 AFIX 43 H9 2 0.349727 0.736781 0.249247 11.00000 -1.20000 AFIX 0 C10 1 0.533735 0.544538 0.135545 11.00000 0.03238 0.03390 = 0.02981 0.00289 0.01331 -0.00436 AFIX 137 H10A 2 0.569335 0.700004 0.155776 11.00000 -1.50000 H10B 2 0.437472 0.557675 0.098591 11.00000 -1.50000 H10C 2 0.592362 0.475151 0.101992 11.00000 -1.50000 AFIX 0 C11 1 0.290072 0.385025 0.492204 11.00000 0.02127 0.02703 = 0.01807 0.00481 0.00275 -0.00312 O12 4 0.315401 0.217289 0.541208 11.00000 0.03931 0.04136 = 0.03008 0.01329 0.01540 0.00692 C13 1 0.196363 0.576558 0.507383 11.00000 0.03521 0.04373 = 0.02990 0.00307 0.01725 0.00743 AFIX 137 H13A 2 0.248228 0.723979 0.517507 11.00000 -1.50000 H13B 2 0.164134 0.538570 0.558394 11.00000 -1.50000 H13C 2 0.115644 0.591973 0.456142 11.00000 -1.50000 AFIX 0 HKLF 4 REM A21255_014 in P2(1)/n REM wR2 = 0.2778, GooF = S = 1.162, Restrained GooF = 1.162 for all data REM R1 = 0.1139 for 1341 Fo > 4sig(Fo) and 0.1289 for all 1590 data REM 121 parameters refined using 0 restraints END WGHT 0.1430 1.5166 REM Highest difference peak 0.613, deepest hole -0.413, 1-sigma level 0.109 Q1 1 0.4953 0.4344 0.2411 11.00000 0.05 0.61 Q2 1 0.3251 0.4056 0.4525 11.00000 0.05 0.46 Q3 1 0.2823 0.2463 0.5806 11.00000 0.05 0.45 Q4 1 0.5127 0.4091 0.1635 11.00000 0.05 0.44 Q5 1 0.4442 0.2498 0.2833 11.00000 0.05 0.41 ; _shelx_res_checksum 34595 _shelx_hkl_file ; -2 0 0 281.32 26.67 3 0 0 0.41 0.99 -3 0 0 1.37 0.99 -3 0 0 -0.59 1.21 3 0 0 0.12 1.29 4 0 0 5.48 1.49 -4 0 0 5.15 1.56 -4 0 0 6.85 1.82 4 0 0 7.80 1.87 5 0 0 0.76 1.14 5 0 0 -1.75 1.49 -5 0 0 -1.05 1.49 -5 0 0 0.98 1.52 6 0 0 94.47 9.81 -6 0 0 99.41 9.83 6 0 0 103.80 10.02 -6 0 0 92.14 9.97 7 0 0 0.42 1.51 -7 0 0 1.08 1.95 7 0 0 2.48 1.93 -8 0 0 59.96 6.70 -8 0 0 53.99 6.80 8 0 0 58.35 6.52 9 0 0 0.54 2.35 -9 0 0 -1.47 1.71 9 0 0 -0.44 1.99 -9 0 0 3.33 2.83 -10 0 0 2.12 2.24 10 0 0 4.27 2.43 -10 0 0 4.04 3.18 10 0 0 6.63 3.00 -11 0 0 2.55 2.55 11 0 0 1.48 2.67 -12 0 0 12.56 3.62 0 -1 0 0.06 0.89 0 1 0 -0.36 0.66 -1 1 0 573.10 54.03 2 -1 0 16.03 2.19 2 -1 0 18.73 2.23 -2 -1 0 20.85 2.22 -2 1 0 19.17 2.11 2 1 0 18.40 2.32 -2 1 0 18.10 2.34 -3 -1 0 39.50 4.48 3 -1 0 44.90 4.37 -3 -1 0 43.45 4.39 3 -1 0 41.44 4.39 -3 1 0 40.26 4.47 -3 1 0 45.42 4.30 3 1 0 36.66 4.45 3 1 0 41.00 4.36 -4 -1 0 127.49 13.02 -4 -1 0 142.23 12.95 4 -1 0 128.11 12.88 4 1 0 137.73 12.93 -4 1 0 122.38 12.98 4 1 0 137.28 13.04 -5 -1 0 136.54 13.75 -5 -1 0 147.24 13.65 5 -1 0 142.17 13.65 5 -1 0 133.29 13.58 5 1 0 140.08 13.62 5 1 0 134.99 13.73 -5 1 0 148.95 13.56 -5 1 0 126.43 13.68 6 -1 0 232.30 24.39 -6 -1 0 249.32 24.61 -6 -1 0 269.67 24.81 6 -1 0 250.99 24.49 -6 1 0 241.01 24.54 6 1 0 245.47 24.43 -6 1 0 285.97 24.43 -7 -1 0 44.53 4.95 7 -1 0 42.44 5.68 7 -1 0 36.04 4.82 7 1 0 48.91 5.31 7 1 0 45.36 5.05 -7 1 0 36.65 5.12 8 -1 0 14.66 2.99 -8 -1 0 17.63 3.22 -8 -1 0 11.93 3.56 8 -1 0 12.41 3.06 -8 1 0 11.22 2.66 8 1 0 13.64 2.99 -8 1 0 13.85 3.54 8 1 0 10.32 3.30 -9 -1 0 16.52 3.46 -9 -1 0 17.86 4.35 9 1 0 16.35 3.87 -9 1 0 14.10 5.99 9 1 0 12.01 3.40 -9 1 0 18.53 3.82 -10 -1 0 3.41 3.67 -10 -1 0 4.95 2.48 10 -1 0 2.78 2.62 10 -1 0 2.09 2.75 -10 1 0 2.87 2.15 10 1 0 7.66 2.63 10 1 0 2.60 2.97 -11 -1 0 42.83 5.77 11 -1 0 40.34 5.90 -11 -1 0 60.27 9.43 11 1 0 42.87 6.14 -11 1 0 45.18 5.65 11 1 0 34.25 5.82 -12 -1 0 2.93 2.93 12 1 0 3.52 3.58 -12 1 0 4.72 3.44 0 -2 0 5.68 1.33 0 -2 0 2.59 1.38 0 2 0 3.37 0.87 0 2 0 2.23 1.16 1 -2 0 10.57 1.93 1 -2 0 16.07 2.47 -1 -2 0 15.93 1.95 -1 -2 0 15.08 1.77 1 2 0 15.41 2.05 1 2 0 13.43 1.77 -1 2 0 15.45 2.22 -2 -2 0 10.23 1.58 2 -2 0 9.60 1.83 -2 -2 0 9.92 1.85 2 -2 0 9.16 1.87 -2 2 0 7.57 1.47 -2 2 0 7.53 1.98 3 -2 0 58.88 5.80 -3 -2 0 57.23 5.94 -3 -2 0 58.48 5.80 3 -2 0 49.06 5.83 3 2 0 59.14 5.82 -3 2 0 56.63 5.67 -3 2 0 51.28 6.02 3 2 0 60.69 5.95 4 -2 0 -0.63 1.15 -4 -2 0 3.44 1.78 -4 -2 0 -0.77 1.16 4 -2 0 0.45 1.30 -4 2 0 -0.61 1.52 -4 2 0 -0.01 0.92 4 2 0 0.20 1.46 4 2 0 0.08 1.05 5 -2 0 15.62 2.68 -5 -2 0 17.85 2.73 -5 -2 0 22.26 3.10 5 -2 0 18.18 2.65 5 2 0 25.31 3.62 -5 2 0 21.48 2.55 5 2 0 18.87 2.73 -5 2 0 18.79 3.25 6 -2 0 0.85 1.49 -6 -2 0 -0.09 1.87 -6 -2 0 -0.33 1.49 6 2 0 -1.09 1.81 -6 2 0 -0.04 1.80 6 2 0 1.30 1.52 7 -2 0 25.12 3.56 7 -2 0 22.60 3.54 -7 -2 0 25.06 4.04 -7 -2 0 25.32 3.64 -7 2 0 26.78 3.31 -7 2 0 29.96 4.57 7 2 0 24.88 3.90 7 2 0 22.62 3.54 8 -2 0 6.28 2.48 -8 -2 0 7.30 2.47 -8 -2 0 10.84 3.47 -8 2 0 5.95 3.41 8 2 0 8.28 3.13 8 2 0 8.87 2.55 -8 2 0 8.13 3.70 9 -2 0 1.76 2.17 9 -2 0 0.44 2.05 -9 -2 0 0.43 2.12 -9 -2 0 -0.49 2.90 9 2 0 1.02 2.24 -9 2 0 1.47 2.87 -9 2 0 -1.25 1.65 9 2 0 -0.80 2.55 -10 -2 0 17.30 3.89 -10 -2 0 16.63 5.02 10 -2 0 16.25 3.86 10 2 0 22.20 4.11 -10 2 0 13.47 3.32 10 2 0 19.57 4.58 -11 -2 0 -0.18 2.56 -11 -2 0 0.49 3.95 11 -2 0 12.69 3.59 11 2 0 5.97 2.99 0 -3 0 -0.10 1.15 0 -3 0 -0.08 1.40 0 3 0 0.14 1.19 0 3 0 -0.31 0.78 -1 -3 0 80.97 7.25 1 -3 0 61.76 7.38 -1 3 0 61.80 7.26 1 3 0 78.13 7.10 2 -3 0 67.88 6.98 -2 -3 0 70.55 6.71 -2 3 0 61.12 6.76 -3 -3 0 17.10 2.31 3 -3 0 17.16 2.50 -3 -3 0 18.42 2.64 3 -3 0 17.24 2.84 -3 3 0 16.64 2.86 3 3 0 17.72 2.33 -3 3 0 16.58 2.24 4 -3 0 34.91 4.01 -4 -3 0 39.28 4.36 4 -3 0 29.13 4.22 -4 -3 0 35.34 4.01 4 3 0 36.88 4.07 4 3 0 37.29 4.23 -4 3 0 29.83 4.40 -4 3 0 36.90 3.85 5 -3 0 11.21 2.58 -5 -3 0 10.30 2.71 -5 -3 0 9.72 2.30 5 -3 0 8.48 2.10 5 3 0 11.24 2.29 5 3 0 11.34 2.70 -5 3 0 8.75 2.78 -5 3 0 14.12 2.09 -6 -3 0 1.92 1.73 6 -3 0 0.85 1.90 6 -3 0 1.67 1.55 -6 -3 0 0.04 2.18 -6 3 0 -1.83 2.22 -6 3 0 0.49 1.19 6 3 0 -0.18 1.46 7 -3 0 6.34 2.35 -7 -3 0 7.64 2.45 -7 -3 0 7.46 3.12 7 -3 0 8.92 2.96 7 3 0 5.67 2.14 -7 3 0 7.51 2.02 -7 3 0 4.99 3.37 7 3 0 5.23 2.81 -8 -3 0 2.22 3.17 8 -3 0 -0.07 2.05 8 -3 0 -0.49 1.74 -8 -3 0 2.47 2.15 8 3 0 1.52 2.12 8 3 0 4.25 2.85 -8 3 0 -0.65 1.46 -8 3 0 5.70 3.22 -9 -3 0 0.90 3.10 9 -3 0 0.56 2.23 -9 -3 0 -1.43 2.24 -9 3 0 -0.14 1.68 9 3 0 1.20 2.27 9 3 0 1.58 2.84 -10 -3 0 20.12 4.50 10 -3 0 21.77 4.38 -10 -3 0 31.35 6.13 -10 3 0 21.08 3.84 10 3 0 22.12 4.65 10 3 0 23.80 5.22 -11 -3 0 2.96 3.08 11 -3 0 4.06 2.76 -11 -3 0 2.62 4.35 -11 3 0 1.69 2.16 11 3 0 3.88 3.47 0 -4 0 84.07 8.44 0 4 0 82.54 8.26 1 -4 0 1.00 2.35 -1 -4 0 0.83 1.42 1 -4 0 2.20 1.52 1 4 0 0.92 1.08 -1 4 0 1.85 1.80 -1 4 0 1.07 0.93 -2 -4 0 31.91 5.52 -2 -4 0 39.80 4.47 2 -4 0 37.94 4.84 2 4 0 42.29 4.23 -2 4 0 32.36 4.43 3 -4 0 9.35 2.01 3 -4 0 12.14 2.57 -3 -4 0 11.47 3.20 -3 4 0 12.99 2.25 3 4 0 15.47 2.61 -4 -4 0 38.25 4.64 4 -4 0 30.05 4.27 4 -4 0 35.71 4.30 -4 -4 0 35.74 4.23 4 4 0 39.65 4.32 4 4 0 49.15 7.12 -4 4 0 43.67 4.15 -4 4 0 28.59 4.29 -5 -4 0 53.63 6.02 -5 -4 0 43.81 5.42 5 -4 0 38.49 5.66 5 -4 0 48.48 5.42 -5 4 0 56.19 5.25 5 4 0 48.90 5.71 -5 4 0 42.11 5.78 5 4 0 51.80 5.55 6 -4 0 2.32 2.57 6 -4 0 -2.69 1.53 -6 -4 0 0.00 2.31 -6 -4 0 2.51 1.85 6 4 0 2.41 2.22 6 4 0 -0.76 1.66 -6 4 0 -1.20 1.15 -6 4 0 0.88 5.60 -7 -4 0 27.64 4.41 7 -4 0 33.01 4.52 -7 -4 0 31.65 5.47 7 -4 0 26.44 3.79 7 4 0 27.21 4.00 -7 4 0 24.01 3.44 -7 4 0 22.39 4.94 7 4 0 33.45 5.12 8 -4 0 2.69 1.93 -8 -4 0 -2.20 3.05 8 4 0 0.92 2.66 8 4 0 -0.13 1.97 -8 4 0 1.17 1.58 9 -4 0 5.03 2.48 -9 -4 0 2.32 3.83 -9 -4 0 1.05 2.54 9 4 0 -1.75 2.06 -9 4 0 3.99 1.93 9 4 0 0.79 1.70 -10 -4 0 1.91 2.53 -10 -4 0 4.52 4.22 10 -4 0 1.37 2.34 10 4 0 -0.38 2.42 -10 4 0 2.25 1.95 0 -5 0 2.04 2.18 0 -5 0 -1.16 1.53 0 5 0 0.17 1.07 -1 -5 0 141.86 13.92 -1 5 0 142.07 13.58 1 5 0 133.74 13.67 -2 -5 0 48.30 5.98 -2 5 0 53.60 5.51 2 5 0 55.83 5.79 -3 -5 0 48.60 5.58 3 -5 0 50.68 5.70 -3 5 0 41.03 5.06 3 5 0 42.58 5.11 -4 -5 0 15.83 4.55 4 -5 0 21.03 3.31 -4 5 0 23.29 2.90 4 5 0 21.35 3.14 -5 -5 0 28.19 4.47 5 -5 0 35.07 3.93 5 5 0 24.27 3.77 -5 5 0 25.34 3.38 -6 -5 0 12.72 4.81 6 -5 0 16.09 3.09 -6 -5 0 16.36 3.35 -6 -5 0 28.71 4.96 -6 5 0 16.53 2.53 7 -5 0 10.04 2.60 -7 -5 0 14.13 4.41 -7 -5 0 13.09 5.04 -7 -5 0 10.63 2.97 -7 5 0 9.11 2.15 8 -5 0 23.24 4.56 -8 -5 0 27.34 5.84 -8 -5 0 19.27 6.39 -8 5 0 17.74 4.02 1 -6 0 7.76 2.36 1 -6 0 7.95 3.29 -1 -6 0 1.27 2.44 1 6 0 4.06 2.31 1 6 0 6.24 1.86 -1 6 0 7.82 2.85 -1 6 0 9.24 1.89 -2 -6 0 12.38 3.06 2 -6 0 11.79 3.85 2 -6 0 12.24 2.67 -2 -6 0 8.91 3.34 -2 6 0 17.45 3.18 2 6 0 8.97 2.35 -3 -6 0 11.33 3.77 3 -6 0 12.52 3.46 -3 -6 0 17.92 3.83 3 6 0 19.60 3.31 -3 6 0 16.92 2.30 -3 6 0 17.20 3.02 4 -6 0 8.34 2.53 -4 -6 0 7.82 3.46 -4 -6 0 6.25 3.00 -4 6 0 6.71 1.82 -4 6 0 6.61 1.59 5 -6 0 2.01 1.87 -5 -6 0 0.09 3.58 -5 -6 0 2.77 3.48 5 6 0 -0.39 1.26 -5 6 0 -0.27 1.17 -6 -6 0 29.05 5.89 -6 -6 0 16.40 6.36 -6 6 0 30.65 3.45 -7 -6 0 3.45 4.56 -7 -6 0 0.06 3.34 7 -6 0 -0.46 1.70 7 6 0 1.91 2.13 -7 6 0 -0.21 1.19 7 6 0 0.52 2.90 0 -7 0 13.63 3.47 0 7 0 5.93 2.87 0 7 0 4.27 1.89 1 -7 0 3.15 3.18 1 -7 0 3.44 2.14 -1 -7 0 5.73 3.24 -1 -7 0 2.86 2.40 -1 7 0 7.01 2.86 1 7 0 5.49 1.93 1 7 0 1.78 2.28 -1 7 0 0.99 1.36 -2 -7 0 -2.11 2.22 2 -7 0 4.88 2.17 2 -7 0 3.47 3.11 -2 -7 0 2.62 2.77 2 7 0 0.94 2.03 2 7 0 0.69 1.21 -2 7 0 3.64 2.26 -2 7 0 6.62 2.01 -3 -7 0 2.99 3.03 3 -7 0 3.54 1.87 3 -7 0 8.22 2.93 3 7 0 5.07 2.40 3 7 0 2.40 1.69 -3 7 0 2.94 1.26 -3 7 0 2.90 1.70 12 0 -1 5.95 3.73 -12 0 1 6.46 2.87 11 0 -1 5.30 3.29 -11 0 1 -0.67 2.15 10 0 -1 1.17 2.84 -10 0 1 -0.20 3.23 10 0 -1 1.73 4.05 -9 0 1 3.25 2.10 9 0 -1 2.80 2.26 -9 0 1 6.18 3.20 9 0 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-17 14.83 5.91 -2 3 17 7.83 7.50 2 3 -17 15.34 4.42 1 -3 -17 3.86 5.20 -1 -3 17 1.51 4.53 1 -3 -17 2.44 6.18 1 3 -17 9.48 4.17 -1 3 17 -4.88 6.89 -1 3 17 2.19 3.26 1 3 -17 4.52 2.16 0 -3 -17 8.11 4.82 0 -3 17 8.23 4.94 0 -3 17 12.10 2.97 0 -3 -17 3.36 5.16 0 3 17 14.18 8.36 1 3 17 28.13 10.33 -4 -4 17 6.19 4.04 4 -4 -17 11.26 5.69 4 4 -17 17.05 3.82 3 -4 -17 31.09 6.77 -3 -4 17 14.24 3.66 -3 4 17 4.18 3.96 3 4 -17 22.54 4.98 -2 -4 17 56.93 7.60 2 -4 -17 36.63 8.13 -2 4 17 38.66 7.57 -8 0 18 20.53 6.30 -7 0 18 22.50 5.80 -7 0 18 12.44 6.23 -6 0 18 34.22 6.87 -5 0 18 0.94 3.44 5 0 -18 9.11 3.75 -5 0 18 3.92 5.14 -4 0 18 -2.63 4.50 -4 0 18 3.74 4.11 4 0 -18 8.08 3.54 3 0 -18 13.24 3.76 -3 0 18 -2.62 4.57 -3 0 18 6.57 4.15 3 0 -18 16.08 3.83 -2 0 18 10.56 6.26 -2 0 18 8.20 4.36 -1 0 18 9.77 6.64 -1 0 18 3.06 4.01 0 0 -18 15.85 3.90 0 0 18 19.50 8.71 1 0 18 -8.76 14.03 1 0 18 2.33 3.21 2 0 18 11.12 4.20 2 0 18 22.62 8.70 8 -1 -18 18.60 5.03 -8 -1 18 6.27 5.26 -8 -1 18 16.96 5.42 8 1 -18 8.73 4.00 -8 1 18 20.09 6.07 8 1 -18 15.37 3.90 -7 -1 18 19.63 5.65 -7 -1 18 19.53 5.93 7 -1 -18 10.24 5.18 -7 1 18 19.00 5.99 7 1 -18 11.28 4.06 -7 1 18 19.62 7.33 -6 -1 18 23.48 5.42 -6 1 18 8.65 6.61 -5 -1 18 11.93 5.17 5 -1 -18 15.24 4.67 5 -1 -18 11.37 4.99 -5 -1 18 12.46 5.65 -5 1 18 5.63 6.04 -5 1 18 2.18 4.39 5 1 -18 13.40 3.24 4 -1 -18 13.16 5.32 -4 -1 18 10.06 4.49 -4 1 18 11.15 5.25 -4 1 18 12.33 6.44 -3 -1 18 20.47 5.72 -3 1 18 22.86 7.76 -3 1 18 24.14 5.78 2 -1 -18 27.71 5.64 -2 -1 18 13.29 7.61 -2 -1 18 22.52 5.59 -2 1 18 15.22 5.04 2 1 -18 19.02 4.70 -2 1 18 25.13 8.51 1 -1 -18 39.76 5.80 -1 -1 18 9.57 6.81 -1 1 18 24.81 8.27 0 -1 18 15.16 7.08 0 -1 18 12.92 4.19 0 -1 -18 8.75 3.66 0 1 18 19.07 4.71 0 1 -18 11.73 3.63 1 -1 18 19.86 7.83 1 -1 18 15.68 4.40 1 1 18 8.93 8.49 -2 -1 -18 47.26 7.02 2 1 18 42.50 10.84 -7 -2 18 11.06 4.45 7 -2 -18 5.67 5.57 7 -2 -18 19.75 5.88 -7 -2 18 0.17 3.99 7 2 -18 3.70 3.22 -7 2 18 5.74 4.87 6 -2 -18 14.75 5.17 6 -2 -18 10.37 5.73 -6 -2 18 5.75 4.44 -6 -2 18 3.03 3.95 -6 2 18 18.07 7.20 6 2 -18 6.18 3.59 -6 2 18 8.02 4.45 5 -2 -18 6.35 5.36 -5 -2 18 9.33 4.72 -5 -2 18 13.58 4.71 -5 2 18 12.92 7.19 5 2 -18 7.49 3.37 4 -2 -18 6.99 4.79 -4 -2 18 9.70 4.42 -4 -2 18 6.11 4.80 -4 2 18 8.53 4.23 -4 2 18 14.87 6.99 4 2 -18 6.61 3.20 -3 -2 18 39.57 6.46 3 -2 -18 28.01 6.29 3 -2 -18 18.38 6.36 -3 -2 18 22.96 6.65 3 2 -18 30.57 4.65 -3 2 18 10.78 8.02 -3 2 18 23.09 6.05 -2 -2 18 20.45 5.15 2 2 -18 17.68 4.72 2 2 -18 29.95 4.52 -2 2 18 10.62 4.77 -1 -2 18 37.74 8.88 -1 -2 18 42.13 6.55 -1 2 18 61.41 12.19 0 -2 18 16.91 4.76 0 -2 18 13.84 6.73 0 -2 -18 6.58 3.51 0 2 18 8.67 3.83 0 2 18 30.65 9.12 0 2 -18 8.86 3.01 1 -2 18 12.68 3.98 1 -2 18 15.56 7.35 1 2 18 13.36 8.46 1 2 18 15.17 4.71 -6 -3 18 46.41 7.15 6 -3 -18 42.98 9.42 -6 3 18 59.71 16.70 -6 3 18 55.53 8.43 5 -3 -18 11.79 5.93 -5 -3 18 8.09 4.61 -5 -3 18 17.94 3.97 -5 3 18 18.25 8.82 -5 3 18 5.71 4.51 -4 -3 18 5.25 4.77 4 -3 -18 14.83 5.13 -4 3 18 6.19 8.47 4 3 -18 11.85 3.62 -3 -3 18 21.00 5.87 3 -3 -18 15.20 5.90 3 -3 -18 21.86 7.68 -3 3 18 14.95 5.07 2 -3 -18 17.64 5.76 -2 -3 18 6.33 4.89 -2 -3 18 2.93 2.82 -2 3 18 14.00 8.71 -2 3 18 9.42 4.07 -1 -3 18 13.27 5.20 1 -3 -18 9.67 4.52 -1 -3 18 5.69 2.62 1 3 -18 6.41 3.08 -1 3 18 3.45 3.74 -7 0 19 6.70 6.36 -7 0 19 13.92 7.05 7 0 -19 5.49 3.73 6 0 -19 6.23 3.77 -6 0 19 9.02 5.69 -6 0 19 0.45 4.30 5 0 -19 11.54 4.35 -5 0 19 11.60 5.56 -5 0 19 10.77 4.65 4 0 -19 13.68 4.18 -4 0 19 5.72 5.59 -4 0 19 3.06 4.11 3 0 -19 6.77 3.77 -3 0 19 8.49 5.50 -3 0 19 3.22 3.81 -2 0 19 4.78 3.95 -2 0 19 14.52 6.95 -1 0 19 3.72 3.61 -1 0 19 9.52 7.10 0 0 19 115.40 14.65 0 0 -19 82.87 12.48 1 0 19 10.70 11.01 7 -1 -19 52.71 6.62 7 1 -19 40.72 6.03 -6 -1 19 13.69 5.78 6 -1 -19 5.99 4.49 -6 -1 19 19.79 5.99 -6 1 19 3.46 4.65 -6 1 19 11.85 6.22 -5 -1 19 13.19 5.90 5 -1 -19 6.93 3.86 -5 1 19 17.32 6.47 4 -1 -19 6.70 3.90 -4 -1 19 14.34 5.02 -4 1 19 14.34 7.16 -4 1 19 12.28 8.91 -3 -1 19 0.30 5.35 3 -1 -19 13.31 4.06 -3 -1 19 2.13 3.89 -3 1 19 7.97 7.16 3 1 -19 5.51 3.01 -2 -1 19 3.19 3.73 2 -1 -19 9.27 3.89 -2 1 19 7.19 3.86 2 1 -19 18.00 4.35 -2 1 19 10.40 6.97 1 -1 -19 10.87 3.55 -1 -1 19 33.55 8.13 -1 -1 19 5.26 3.90 -1 1 19 14.62 4.54 1 1 -19 14.54 3.88 -1 1 19 26.99 8.30 0 1 19 35.45 10.38 -1 -1 -19 73.41 9.07 -1 1 -19 53.93 8.46 6 -2 -19 44.18 9.27 -6 -2 19 62.32 8.34 -6 -2 19 43.23 9.03 -6 2 19 43.41 10.46 -6 2 19 51.18 8.17 -5 -2 19 31.72 7.66 -5 -2 19 32.04 6.99 5 2 -19 41.91 5.56 -5 2 19 49.50 9.54 -4 -2 19 19.64 6.32 -4 -2 19 22.16 5.53 -4 2 19 10.74 4.73 -3 -2 19 36.07 6.89 -3 -2 19 30.21 8.00 -3 2 19 41.83 10.63 3 2 -19 41.54 5.63 -3 2 19 25.32 6.73 -2 -2 19 11.05 4.52 2 -2 -19 7.38 3.41 -2 -2 19 13.60 6.04 -2 2 19 3.48 7.64 2 2 -19 20.14 6.26 -2 2 19 5.74 3.82 -1 -2 19 18.96 7.79 -1 -2 19 26.03 6.34 -1 2 19 24.31 9.24 1 2 -19 35.22 8.26 -6 0 20 16.40 6.52 6 0 -20 6.65 3.69 -6 0 20 6.83 5.03 -4 0 20 19.56 6.83 4 0 -20 7.27 3.60 -4 0 20 6.25 4.53 -3 0 20 20.54 7.21 1 0 -20 25.41 7.82 -5 -1 20 13.70 5.42 -5 -1 20 25.63 6.33 4 -1 -20 14.39 4.77 4 1 -20 13.96 4.64 -4 1 20 18.62 8.31 -4 1 20 7.26 4.90 3 -1 -20 7.74 3.92 -3 -1 20 14.10 4.94 -3 1 20 11.42 7.11 -3 1 20 8.15 4.39 3 1 -20 9.43 4.06 -2 -1 20 15.51 4.91 2 -1 -20 10.47 3.94 -2 1 20 27.13 9.44 2 1 -20 11.75 4.07 -2 1 20 21.43 5.49 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 30946 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.5832(3) 0.0972(6) 0.3085(2) 0.0260(10) Uani 1 1 d . . . . . H1 H 0.618276 -0.033636 0.334242 0.031 Uiso 1 1 calc R U . . . C2 C 0.6095(4) 0.1905(7) 0.2362(3) 0.0245(10) Uani 1 1 d . . . . . H2 H 0.670346 0.123304 0.206387 0.029 Uiso 1 1 calc R U . . . C3 C 0.5368(4) 0.3934(7) 0.2121(3) 0.0229(10) Uani 1 1 d . . . . . C4 C 0.4618(4) 0.4317(6) 0.2750(2) 0.0207(10) Uani 1 1 d . . . . . C5 C 0.4928(4) 0.2419(6) 0.3342(2) 0.0207(10) Uani 1 1 d . . . . . C6 C 0.4355(4) 0.2241(7) 0.4041(3) 0.0224(10) Uani 1 1 d . . . . . H6 H 0.455570 0.094014 0.442389 0.027 Uiso 1 1 calc R U . . . C7 C 0.3480(4) 0.4022(7) 0.4163(2) 0.0212(10) Uani 1 1 d . . . . . C8 C 0.3174(4) 0.5932(6) 0.3584(3) 0.0225(10) Uani 1 1 d . . . . . H8 H 0.257836 0.713828 0.367843 0.027 Uiso 1 1 calc R U . . . C9 C 0.3723(4) 0.6083(7) 0.2882(3) 0.0233(10) Uani 1 1 d . . . . . H9 H 0.349727 0.736781 0.249247 0.028 Uiso 1 1 calc R U . . . C10 C 0.5337(5) 0.5445(8) 0.1355(3) 0.0311(11) Uani 1 1 d . . . . . H10A H 0.569335 0.700004 0.155776 0.047 Uiso 1 1 calc R U . . . H10B H 0.437472 0.557675 0.098591 0.047 Uiso 1 1 calc R U . . . H10C H 0.592362 0.475151 0.101992 0.047 Uiso 1 1 calc R U . . . C11 C 0.2901(4) 0.3850(7) 0.4922(2) 0.0227(10) Uani 1 1 d . . . . . O12 O 0.3154(3) 0.2173(6) 0.5412(2) 0.0358(10) Uani 1 1 d . . . . . C13 C 0.1964(5) 0.5766(8) 0.5074(3) 0.0346(12) Uani 1 1 d . . . . . H13A H 0.248228 0.723979 0.517507 0.052 Uiso 1 1 calc R U . . . H13B H 0.164134 0.538570 0.558394 0.052 Uiso 1 1 calc R U . . . H13C H 0.115644 0.591973 0.456142 0.052 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 N1 0.0298(19) 0.0226(18) 0.0263(19) 0.0031(14) 0.0091(14) 0.0068(14) C2 0.0235(19) 0.028(2) 0.024(2) -0.0057(17) 0.0095(16) -0.0004(16) C3 0.0192(18) 0.025(2) 0.023(2) -0.0019(16) 0.0028(15) -0.0063(15) C4 0.0176(18) 0.020(2) 0.021(2) 0.0042(15) -0.0008(15) -0.0046(14) C5 0.0185(18) 0.0192(19) 0.022(2) -0.0029(15) 0.0018(15) 0.0012(14) C6 0.0223(19) 0.023(2) 0.020(2) 0.0054(16) 0.0022(15) 0.0013(15) C7 0.0168(18) 0.024(2) 0.020(2) -0.0011(15) 0.0000(15) -0.0034(14) C8 0.0202(19) 0.0182(19) 0.027(2) 0.0014(16) 0.0034(16) 0.0028(14) C9 0.0226(19) 0.0179(19) 0.024(2) 0.0031(15) -0.0020(16) -0.0020(15) C10 0.032(2) 0.034(2) 0.030(2) 0.0029(19) 0.0133(18) -0.0044(18) C11 0.0213(19) 0.027(2) 0.018(2) 0.0048(17) 0.0027(15) -0.0031(15) O12 0.0393(18) 0.041(2) 0.0301(18) 0.0133(15) 0.0154(14) 0.0069(14) C13 0.035(2) 0.044(3) 0.030(2) 0.003(2) 0.0172(19) 0.0074(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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C5 108.3(3) . . ? C2 N1 H1 125.8 . . ? C5 N1 H1 125.8 . . ? N1 C2 C3 111.1(3) . . ? N1 C2 H2 124.4 . . ? C3 C2 H2 124.4 . . ? C2 C3 C4 105.8(3) . . ? C2 C3 C10 127.8(4) . . ? C4 C3 C10 126.4(4) . . ? C9 C4 C5 118.9(4) . . ? C9 C4 C3 134.1(4) . . ? C5 C4 C3 107.0(3) . . ? N1 C5 C6 130.3(4) . . ? N1 C5 C4 107.7(3) . . ? C6 C5 C4 122.0(3) . . ? C7 C6 C5 118.1(3) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C6 C7 C8 120.5(4) . . ? C6 C7 C11 117.8(3) . . ? C8 C7 C11 121.7(4) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C4 119.2(4) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O12 C11 C7 121.2(4) . . ? O12 C11 C13 119.9(4) . . ? C7 C11 C13 118.9(3) . . ? 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 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.364(5) . ? N1 C5 1.368(5) . ? N1 H1 0.8800 . ? C2 C3 1.367(6) . ? C2 H2 0.9500 . ? C3 C4 1.426(6) . ? C3 C10 1.493(6) . ? C4 C9 1.403(5) . ? C4 C5 1.418(5) . ? C5 C6 1.392(6) . ? C6 C7 1.390(5) . ? C6 H6 0.9500 . ? C7 C8 1.412(5) . ? C7 C11 1.484(5) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O12 1.221(5) . ? C11 C13 1.503(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 O12 0.88 2.19 2.949(4) 144.8 3_656 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 C3 -0.9(4) . . . . ? N1 C2 C3 C4 1.2(4) . . . . ? N1 C2 C3 C10 -178.1(4) . . . . ? C2 C3 C4 C9 178.3(4) . . . . ? C10 C3 C4 C9 -2.4(7) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C10 C3 C4 C5 178.3(4) . . . . ? C2 N1 C5 C6 -179.6(4) . . . . ? C2 N1 C5 C4 0.2(4) . . . . ? C9 C4 C5 N1 -178.9(3) . . . . ? C3 C4 C5 N1 0.5(4) . . . . ? C9 C4 C5 C6 0.9(5) . . . . ? C3 C4 C5 C6 -179.6(3) . . . . ? N1 C5 C6 C7 178.4(4) . . . . ? C4 C5 C6 C7 -1.5(5) . . . . ? C5 C6 C7 C8 0.9(5) . . . . ? C5 C6 C7 C11 -178.5(3) . . . . ? C6 C7 C8 C9 0.3(6) . . . . ? C11 C7 C8 C9 179.7(3) . . . . ? C7 C8 C9 C4 -0.9(6) . . . . ? C5 C4 C9 C8 0.3(5) . . . . ? C3 C4 C9 C8 -178.9(4) . . . . ? C6 C7 C11 O12 -1.8(6) . . . . ? C8 C7 C11 O12 178.8(4) . . . . ? C6 C7 C11 C13 179.4(3) . . . . ? C8 C7 C11 C13 0.0(5) . . . . ?