#------------------------------------------------------------------------------ #$Date: 2019-11-10 08:47:08 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225938 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515838.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_4515838 loop_ _publ_author_name 'Rao, R. Nishanth' 'Mm, Balamurali' 'Maiti, Barnali' 'Thakuria, Ranjit' 'Chanda, Kaushik' _publ_section_title ; Efficient Access to Imidazo[1,2- a]pyridines/pyrazines/pyrimidines via Catalyst-Free Annulation Reaction under Microwave Irradiation in Green Solvent. ; _journal_issue 3 _journal_name_full 'ACS combinatorial science' _journal_page_first 164 _journal_page_last 171 _journal_paper_doi 10.1021/acscombsci.7b00173 _journal_volume 20 _journal_year 2018 _chemical_formula_moiety 'C15 H14 N2 O' _chemical_formula_sum 'C15 H14 N2 O' _chemical_formula_weight 238.28 _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' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc1q5jbr _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2018-01-16 deposited with the CCDC. 2018-01-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.711(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.722(2) _cell_length_b 5.7944(7) _cell_length_c 13.6813(17) _cell_measurement_reflns_used 3406 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.32 _cell_measurement_theta_min 2.64 _cell_volume 1224.6(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11263 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.025 _diffrn_reflns_theta_min 1.318 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.292 _exptl_crystal_description needle _exptl_crystal_F_000 504 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.358 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef 0.0000(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 2930 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0696 _refine_ls_shift/su_max 0.313 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+1.1036P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2214 _refine_ls_wR_factor_ref 0.2379 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1995 _reflns_number_total 2930 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file co7b00173_si_002.cif _cod_data_source_block X _cod_original_cell_volume 1224.7(3) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4515838 _shelx_shelxl_version_number 2016/6 _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 0.984 _shelx_estimated_absorpt_t_max 0.993 _exptl_absorpt_special_details 'Bruker AXS SADABS program' _shelx_res_file ; TITL RT_11_a.res in P2(1)/c rt_11_a.res created by SHELXL-2016/6 at 13:06:59 on 06-Nov-2017 CELL 0.71073 15.7223 5.7944 13.6813 90.000 100.711 90.000 ZERR 4.000 0.0021 0.0007 0.0017 0.000 0.005 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 60 56 8 4 L.S. 10 ACTA BOND $H FMAP 2 PLAN 4 LIST 6 SIZE 0.09 0.12 0.19 TEMP 23.000 WGHT 0.086400 1.103600 EXTI 0.000000 FVAR 0.37569 O1 4 0.432944 0.557212 0.876909 11.00000 0.05727 0.05608 = 0.04934 0.00270 0.00389 -0.00308 N1 3 0.191237 0.584377 0.327052 11.00000 0.04259 0.04042 = 0.04879 -0.00079 0.01337 -0.00025 C1 1 0.164750 0.369268 0.354360 11.00000 0.04104 0.03486 = 0.05104 -0.00502 0.01459 -0.00179 C2 1 0.108232 0.240793 0.281895 11.00000 0.04705 0.04334 = 0.05420 -0.00648 0.01482 -0.00773 AFIX 43 H2 2 0.088238 0.098001 0.298925 11.00000 -1.20000 AFIX 0 N2 3 0.199359 0.322921 0.448753 11.00000 0.04917 0.04139 = 0.05008 -0.00250 0.01288 -0.00542 C5 1 0.166074 0.667757 0.231467 11.00000 0.05531 0.04599 = 0.05009 0.00611 0.01112 -0.00293 AFIX 43 H5 2 0.185591 0.810890 0.214185 11.00000 -1.20000 AFIX 0 C7 1 0.248386 0.513830 0.482179 11.00000 0.04143 0.04075 = 0.04707 -0.00496 0.01464 -0.00289 C6 1 0.243816 0.675990 0.409167 11.00000 0.04903 0.03859 = 0.05494 -0.00526 0.00951 -0.00876 AFIX 43 H6 2 0.270828 0.819411 0.414039 11.00000 -1.20000 AFIX 0 C9 1 0.349059 0.717175 0.616846 11.00000 0.05896 0.04124 = 0.04871 0.00070 0.01609 -0.00819 AFIX 43 H9 2 0.352374 0.836925 0.572449 11.00000 -1.20000 AFIX 0 C8 1 0.298150 0.526969 0.584365 11.00000 0.04211 0.03809 = 0.04863 -0.00428 0.01682 0.00042 C11 1 0.391109 0.557425 0.780073 11.00000 0.03867 0.04565 = 0.04940 0.00062 0.00963 0.00220 C10 1 0.395432 0.735069 0.713744 11.00000 0.05308 0.04251 = 0.05146 -0.00605 0.01197 -0.01134 AFIX 43 H10 2 0.428915 0.865047 0.733579 11.00000 -1.20000 AFIX 0 C3 1 0.082666 0.321635 0.188211 11.00000 0.04158 0.05223 = 0.05617 -0.00955 0.01151 -0.00366 C4 1 0.113380 0.541289 0.163760 11.00000 0.05146 0.05431 = 0.05290 0.00033 0.00592 0.00164 AFIX 43 H4 2 0.096551 0.598215 0.099516 11.00000 -1.20000 AFIX 0 C14 1 0.025302 0.186944 0.107803 11.00000 0.06716 0.07280 = 0.06027 -0.01439 0.00572 -0.01624 AFIX 137 H14A 2 0.009394 0.043507 0.134580 11.00000 -1.50000 H14B 2 0.055835 0.156590 0.054577 11.00000 -1.50000 H14C 2 -0.025923 0.274796 0.082948 11.00000 -1.50000 AFIX 0 C13 1 0.295558 0.349035 0.652808 11.00000 0.04284 0.03950 = 0.05762 -0.00214 0.01570 -0.00375 AFIX 43 H13 2 0.262662 0.217991 0.633106 11.00000 -1.20000 AFIX 0 C12 1 0.341017 0.364685 0.749127 11.00000 0.05004 0.03813 = 0.05308 0.00412 0.01337 0.00163 AFIX 43 H12 2 0.338024 0.244964 0.793636 11.00000 -1.20000 AFIX 0 C15 1 0.481544 0.757450 0.913452 11.00000 0.06552 0.07087 = 0.05118 -0.00378 0.00336 -0.01592 AFIX 137 H15A 2 0.527581 0.779620 0.877097 11.00000 -1.50000 H15B 2 0.505463 0.737370 0.982763 11.00000 -1.50000 H15C 2 0.444271 0.890013 0.905070 11.00000 -1.50000 AFIX 0 HKLF 4 REM RT_11_a.res in P2(1)/c REM R1 = 0.0696 for 1995 Fo > 4sig(Fo) and 0.0971 for all 2930 data REM 166 parameters refined using 0 restraints END WGHT 0.0864 1.1036 REM Highest difference peak 0.358, deepest hole -0.295, 1-sigma level 0.071 Q1 1 0.0443 0.6319 0.0447 11.00000 0.05 0.36 Q2 1 0.0150 0.4422 0.0572 11.00000 0.05 0.33 Q3 1 0.1155 0.6601 0.1971 11.00000 0.05 0.32 Q4 1 0.3752 0.4348 0.7396 11.00000 0.05 0.31 ; _shelx_res_checksum 91241 _shelx_hkl_file ; 0 0 1 0.00 0.10 0 0 1 0.00 0.10 0 0 -1 0.00 0.10 0 0 -1 0.00 0.10 0 0 3 0.00 0.10 0 0 -3 -0.20 0.10 0 0 -3 0.00 0.10 0 0 3 -0.30 0.10 0 0 -4 291.57 10.00 0 0 4 272.27 10.00 0 0 4 282.97 10.00 0 0 -4 286.37 10.00 0 0 -5 0.10 0.20 0 0 5 -0.10 0.20 0 0 -5 -0.10 0.20 0 0 6 95.89 3.70 0 0 -6 102.99 3.70 0 0 -7 0.00 0.20 0 0 7 0.00 0.20 0 0 -8 14.80 0.90 0 0 8 15.60 0.90 0 0 -9 0.00 0.20 0 0 9 0.10 0.20 0 0 -10 15.90 1.00 0 0 10 13.80 1.00 0 0 -11 -0.10 0.30 0 0 11 -0.10 0.30 0 0 12 0.40 0.40 0 0 -12 1.10 0.40 0 0 13 0.10 0.40 0 0 -13 0.10 0.40 0 0 14 0.00 0.40 0 0 -14 -0.20 0.40 0 0 15 -0.30 0.40 0 0 -15 -0.10 0.40 0 0 15 -2.00 0.50 0 0 -16 3.90 0.80 0 0 16 2.90 0.90 0 1 0 -0.50 0.10 0 1 0 -0.30 0.10 0 1 0 -0.50 0.10 0 -1 0 -0.20 0.10 0 -1 0 -0.40 0.10 0 -1 0 -0.50 0.10 0 -1 0 -0.30 0.10 0 1 1 331.07 10.90 0 -1 -1 326.97 11.10 0 -1 -1 332.67 10.90 0 -1 1 333.57 10.90 0 -1 -1 270.97 10.90 0 -1 1 267.67 10.80 0 1 2 144.59 5.10 0 -1 -2 124.79 5.00 0 -1 -2 140.59 5.00 0 -1 2 148.19 5.00 0 -1 -2 144.29 5.00 0 1 3 86.29 3.40 0 1 3 88.09 3.30 0 1 -3 99.19 3.30 0 -1 -3 91.39 3.20 0 -1 3 90.89 3.30 0 -1 -3 91.59 3.30 0 1 4 47.70 1.70 0 1 -4 45.40 1.80 0 1 4 46.10 1.90 0 1 4 45.70 1.80 0 1 4 45.30 1.80 0 1 -4 47.50 1.80 0 -1 -4 46.20 1.80 0 -1 4 43.10 1.80 0 1 5 35.90 1.50 0 1 -5 39.50 1.60 0 1 5 41.60 1.80 0 1 5 40.40 1.70 0 1 5 43.20 1.70 0 1 -5 40.40 1.60 0 -1 -5 43.70 1.70 0 -1 5 41.90 1.70 0 1 6 158.88 5.90 0 1 6 163.38 5.60 0 1 6 155.38 5.80 0 1 -6 160.08 5.80 0 1 6 161.68 5.80 0 1 -6 157.78 5.80 0 -1 -6 156.38 5.80 0 -1 6 153.88 5.80 0 1 7 6.80 0.60 0 1 7 6.90 0.60 0 1 -7 7.80 0.60 0 1 7 7.10 0.40 0 1 -7 6.30 0.50 0 1 7 6.60 0.70 0 -1 7 7.20 0.60 0 -1 -7 6.40 0.60 0 1 8 1.00 0.30 0 1 8 1.30 0.20 0 1 8 2.00 0.60 0 1 -8 0.50 0.30 0 1 -8 0.90 0.30 0 -1 8 0.80 0.30 0 -1 -8 0.50 0.30 0 1 9 20.40 1.20 0 1 -9 24.70 1.30 0 1 9 22.00 1.00 0 1 9 22.50 1.40 0 1 -9 21.60 1.20 0 -1 -9 21.90 1.20 0 -1 9 22.40 1.20 0 1 10 43.10 1.80 0 1 10 41.40 2.20 0 1 10 44.20 2.00 0 1 -10 44.40 2.00 0 -1 -10 45.30 2.00 0 -1 10 41.50 2.00 0 1 11 12.60 1.20 0 1 -11 12.50 1.00 0 1 11 13.60 0.80 0 1 11 13.50 1.00 0 -1 -11 13.60 1.00 0 -1 11 13.30 1.00 0 1 12 29.50 1.80 0 1 12 25.00 1.50 0 1 -12 25.80 1.50 0 -1 12 26.40 1.50 0 -1 -12 27.40 1.60 0 1 13 1.70 0.70 0 1 -13 1.10 0.50 0 1 13 1.10 0.50 0 -1 13 1.90 0.80 0 -1 -13 1.60 0.60 0 1 -14 2.10 0.60 0 1 14 1.90 0.60 0 1 14 2.00 0.70 0 -1 -14 2.00 0.60 0 1 15 -0.10 0.40 0 1 -15 -0.10 0.50 0 1 15 0.00 0.70 0 1 -16 0.90 0.60 0 1 16 0.90 0.60 0 1 -17 1.60 0.70 0 1 17 0.60 0.60 0 -2 0 320.57 10.90 0 -2 0 303.47 11.10 0 -2 0 315.77 11.20 0 2 -1 70.79 2.70 0 2 1 77.39 2.70 0 2 1 76.49 3.00 0 -2 1 77.69 3.00 0 -2 1 80.19 2.80 0 -2 -1 80.89 3.00 0 -2 -1 80.19 2.80 0 -2 -1 77.09 3.00 0 2 2 47.60 1.90 0 2 -2 41.70 1.70 0 2 2 46.40 1.70 0 2 -2 46.00 1.70 0 2 2 45.30 1.70 0 2 2 47.10 1.90 0 -2 -2 47.30 1.70 0 -2 -2 45.10 1.90 0 -2 2 44.80 1.70 0 -2 -2 45.10 1.80 0 2 -3 54.29 2.00 0 2 3 53.39 2.00 0 2 3 53.29 2.00 0 2 3 53.49 2.20 0 2 3 54.69 2.10 0 2 -3 53.59 2.00 0 -2 3 50.19 2.00 0 -2 -3 53.59 2.00 0 -2 -3 52.49 2.20 0 -2 -3 55.09 2.10 0 2 4 3.40 0.40 0 2 4 3.30 0.50 0 2 -4 3.10 0.30 0 2 4 2.80 0.30 0 2 -4 2.90 0.30 0 -2 -4 2.50 0.50 0 -2 -4 3.20 0.30 0 -2 4 3.40 0.30 0 -2 -4 3.00 0.30 0 2 -5 10.60 0.60 0 2 5 8.50 0.80 0 2 5 9.00 0.60 0 -2 5 9.00 0.60 0 -2 -5 10.10 0.60 0 -2 -5 9.40 0.80 0 2 6 122.19 4.40 0 2 -6 129.69 4.60 0 2 6 124.39 4.60 0 2 6 122.99 4.80 0 -2 -6 119.99 4.60 0 -2 6 118.59 4.50 0 -2 -6 121.69 4.40 0 2 7 5.90 0.70 0 2 7 5.10 0.50 0 2 -7 5.40 0.50 0 2 7 5.30 0.50 0 2 7 5.70 0.50 0 -2 7 5.30 0.50 0 -2 -7 5.60 0.50 0 2 -8 1.50 0.30 0 2 -8 2.30 0.40 0 2 8 2.40 0.40 0 2 8 2.50 0.60 0 2 8 2.50 0.40 0 2 8 2.70 0.40 0 -2 -8 2.80 0.40 0 -2 8 2.80 0.40 0 2 9 -0.30 0.20 0 2 9 0.10 0.20 0 2 9 0.70 0.50 0 2 9 -0.20 0.30 0 2 -9 0.20 0.20 0 2 -9 0.00 0.20 0 -2 9 -0.10 0.20 0 -2 -9 0.20 0.20 0 2 10 20.30 1.50 0 2 10 23.20 1.30 0 2 -10 21.50 1.30 0 -2 10 20.20 1.20 0 -2 -10 22.00 1.30 0 2 11 11.30 1.20 0 2 11 12.20 1.00 0 2 -11 13.40 1.00 0 -2 -11 11.50 1.00 0 2 12 5.30 1.00 0 2 -12 5.70 0.80 0 2 12 7.70 0.90 0 2 13 20.80 1.40 0 2 13 20.80 1.70 0 2 -13 20.30 1.40 0 2 14 -0.50 0.40 0 2 14 -0.60 0.60 0 2 -14 0.00 0.40 0 2 -15 0.50 0.40 0 2 15 -0.10 0.50 0 2 16 0.50 0.50 0 2 -16 0.40 0.50 0 2 -17 0.40 0.50 0 2 17 0.10 0.50 0 -3 0 -0.40 0.30 0 -3 0 0.10 0.30 0 3 1 84.49 3.40 0 -3 -1 81.59 3.40 0 -3 1 87.69 3.40 0 -3 -1 83.99 3.40 0 -3 1 83.79 3.50 0 3 2 29.30 1.10 0 3 2 28.60 1.50 0 3 2 28.60 1.10 0 -3 2 29.00 1.40 0 -3 2 28.90 1.60 0 -3 -2 28.80 1.40 0 -3 -2 28.00 1.50 0 3 -3 90.39 3.20 0 3 3 89.29 3.20 0 3 3 87.99 3.20 0 3 -3 88.39 3.20 0 3 3 87.69 3.60 0 -3 -3 88.89 3.40 0 -3 -3 85.89 3.60 0 3 -4 88.59 3.20 0 3 4 86.59 3.30 0 3 4 90.99 3.60 0 3 4 89.09 3.30 0 3 -4 89.79 3.20 0 -3 -4 87.09 3.40 0 -3 -4 87.29 3.60 0 -3 -4 88.59 3.30 0 3 -5 67.69 2.60 0 3 5 70.29 2.70 0 3 5 69.09 2.60 0 3 5 66.79 3.00 0 3 5 66.79 2.60 0 3 -5 68.09 2.60 0 -3 -5 66.29 2.70 0 -3 -5 71.89 2.70 0 -3 5 69.79 2.60 0 3 6 16.00 0.90 0 3 6 15.30 1.20 0 3 -6 16.30 0.80 0 3 -6 16.40 0.80 0 3 6 15.20 0.80 0 3 6 16.70 0.90 0 -3 6 14.60 0.80 0 -3 -6 15.00 0.90 0 -3 -6 17.00 0.80 0 3 7 10.50 0.70 0 3 7 10.60 0.70 0 3 -7 11.30 0.70 0 3 7 11.40 0.70 0 3 -7 11.70 0.70 0 3 7 11.30 1.10 0 -3 -7 11.30 0.60 0 -3 7 10.10 0.70 0 -3 -7 11.30 0.70 0 3 -8 3.50 0.50 0 3 -8 2.90 0.40 0 3 8 3.20 0.50 0 3 8 4.70 0.80 0 3 8 3.90 0.50 0 -3 -8 2.80 0.50 0 3 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7 79.29 3.10 0 -4 -7 80.69 3.10 0 4 -8 0.00 0.20 0 4 8 0.10 0.30 0 4 8 0.20 0.50 0 4 -8 0.40 0.20 0 -4 -8 0.80 0.30 0 4 9 0.00 0.30 0 4 -9 -0.10 0.20 0 4 9 0.30 0.50 0 4 10 28.10 1.90 0 4 -10 25.70 1.40 0 4 10 30.30 1.50 0 4 11 0.10 0.60 0 4 -11 1.00 0.40 0 4 11 0.70 0.40 0 4 -12 1.90 0.50 0 4 12 2.40 0.60 0 4 13 -0.10 0.40 0 4 -13 -0.40 0.30 0 -4 13 0.80 0.80 0 4 14 0.80 0.50 0 4 -14 0.80 0.50 0 -4 14 1.90 1.00 0 4 -15 1.90 0.60 0 4 15 2.30 0.70 0 -4 15 5.60 1.40 0 -5 0 -0.60 0.50 0 -5 1 20.80 1.60 0 -5 -1 22.30 1.60 0 -5 2 0.70 0.70 0 -5 -2 0.40 0.60 0 -5 -3 12.30 1.20 0 -5 3 11.90 1.40 0 5 4 4.60 0.80 0 -5 -4 4.30 0.80 0 -5 4 3.10 0.90 0 5 5 17.20 0.70 0 5 5 17.40 0.70 0 5 5 18.20 1.40 0 -5 5 17.10 1.60 0 -5 -5 15.70 1.20 0 5 6 0.10 0.20 0 5 6 0.00 0.20 0 5 6 0.50 0.50 0 -5 -6 0.20 0.50 0 -5 6 0.30 0.70 0 5 7 2.10 0.70 0 5 -7 2.30 0.30 0 5 -7 1.60 0.20 0 5 7 1.10 0.30 0 5 -7 1.90 0.20 0 5 7 1.60 0.30 0 -5 7 1.00 0.70 0 5 -8 1.20 0.30 0 5 8 1.50 0.30 0 5 8 0.70 0.60 0 5 -8 1.00 0.30 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2 2 29.50 1.20 1 2 2 27.50 1.40 -1 2 -2 30.00 1.10 1 2 2 27.40 1.30 -1 2 -2 28.70 1.10 1 2 2 28.40 1.10 -1 -2 -2 28.00 1.30 1 -2 2 32.10 1.10 -1 -2 -2 29.00 1.20 -1 -2 -2 29.40 1.40 -1 2 -3 1.30 0.20 -1 2 -3 1.50 0.20 1 2 3 1.60 0.30 1 2 3 1.40 0.40 1 2 3 1.40 0.20 1 2 3 1.00 0.20 1 -2 3 1.50 0.20 -1 -2 -3 1.30 0.20 -1 -2 -3 1.40 0.30 -1 -2 -3 1.10 0.40 1 2 4 155.78 5.30 -1 2 -4 145.99 5.30 1 2 4 144.69 5.50 -1 2 -4 149.49 5.30 1 2 4 145.79 5.30 1 -2 4 149.39 5.30 -1 -2 -4 144.29 5.30 -1 -2 -4 141.49 5.50 -1 -2 -4 144.39 5.30 -1 2 -5 4.50 0.40 1 2 5 4.90 0.50 1 2 5 4.60 0.50 -1 2 -5 5.70 0.40 1 2 5 3.30 0.40 1 2 5 4.90 0.60 -1 -2 -5 5.10 0.60 -1 -2 -5 4.90 0.40 -1 -2 -5 4.70 0.40 1 -2 5 4.90 0.40 -1 2 -6 8.20 0.60 1 2 6 9.30 0.60 1 2 6 8.10 0.80 1 2 6 9.00 0.60 1 2 6 9.00 0.60 -1 -2 -6 8.70 0.60 -1 -2 -6 9.00 0.50 1 -2 6 8.90 0.60 1 2 7 5.50 0.70 1 2 7 6.00 0.60 -1 2 -7 7.40 0.50 1 2 7 3.50 0.50 1 2 7 5.50 0.50 1 -2 7 5.60 0.50 -1 -2 -7 5.40 0.50 1 2 8 0.40 0.30 1 2 8 0.20 0.50 1 2 8 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26.40 1.90 16 2 -6 0.60 0.60 -16 2 6 1.10 0.50 -16 -2 6 0.90 0.90 -16 -2 6 0.70 0.70 16 2 -5 0.70 0.60 -16 2 5 0.20 0.40 -16 -2 5 0.30 0.50 -16 -2 5 1.40 0.70 -16 2 4 2.40 0.50 16 2 -4 1.30 0.50 -16 -2 4 1.30 0.80 -16 -2 4 2.20 0.60 -16 2 3 5.80 0.70 16 2 -3 6.30 0.90 -16 -2 3 4.70 0.80 -16 -2 3 5.40 0.90 16 2 -2 8.90 1.10 -16 2 2 7.50 0.80 -16 -2 2 9.70 1.20 -16 -2 2 7.60 1.00 16 2 -1 0.20 0.50 -16 2 1 0.60 0.40 -16 -2 1 -0.40 0.40 -16 -2 1 0.80 0.60 -16 2 0 14.30 1.10 16 2 0 14.70 1.30 -16 -2 0 13.00 1.20 -16 -2 0 13.30 1.20 -16 2 -1 0.00 0.40 16 2 1 -1.00 0.30 -16 -2 -1 -0.30 0.40 -16 -2 -1 0.50 0.50 -16 2 -2 4.10 0.70 16 2 2 3.60 0.70 -16 -2 -2 4.30 1.00 -16 -2 -2 5.00 0.90 16 2 3 6.90 1.00 -16 2 -3 6.90 0.90 -16 -2 -3 7.80 1.00 -16 2 -4 1.70 0.50 16 2 4 1.50 0.60 -16 2 -5 3.90 0.70 16 2 5 6.50 1.00 -16 2 -6 2.90 0.60 -16 2 -7 0.10 0.50 16 3 -11 0.20 0.60 16 3 -11 -0.50 0.50 -16 3 11 0.00 0.50 -16 -3 11 -0.40 0.90 -16 3 10 1.80 0.60 16 3 -10 1.10 0.70 16 3 -10 0.70 0.60 -16 -3 10 1.00 1.00 -16 3 9 1.00 0.50 16 3 -9 1.30 0.70 -16 -3 9 1.40 1.00 16 3 -8 2.60 0.70 -16 3 8 1.00 0.50 -16 -3 8 2.20 0.90 -16 3 7 16.70 1.10 16 3 -7 15.10 1.40 -16 -3 7 12.90 1.60 -16 3 6 -0.10 0.30 16 3 -6 0.50 0.50 -16 -3 6 0.30 0.80 16 3 -5 0.40 0.50 -16 3 5 0.50 0.30 -16 -3 5 -0.20 0.70 16 3 -4 2.00 0.70 -16 3 4 2.70 0.50 -16 -3 4 2.20 0.90 -16 3 3 0.20 0.30 16 3 -3 0.40 0.50 -16 -3 3 1.40 0.80 -16 3 2 1.90 0.50 16 3 -2 3.90 0.80 -16 -3 2 2.70 0.90 -16 3 1 0.50 0.30 16 3 -1 1.20 0.60 -16 -3 1 1.40 0.70 -16 3 0 0.50 0.30 16 3 0 0.20 0.50 -16 -3 0 1.00 0.60 -16 3 -1 0.10 0.30 16 3 1 0.20 0.50 -16 -3 -1 0.40 0.50 -16 3 -2 0.90 0.40 16 3 2 1.60 0.60 -16 -3 -2 0.50 0.60 -16 3 -3 0.20 0.30 16 3 3 0.10 0.50 -16 -3 -3 1.70 0.60 -16 3 -4 -0.50 0.30 16 3 4 0.30 0.60 -16 -3 -4 0.70 0.50 -16 3 -5 0.30 0.40 16 3 5 0.40 0.60 -16 -3 -5 1.00 0.60 16 3 6 -0.50 0.50 -16 3 -6 0.00 0.40 16 4 -9 -0.80 0.40 -16 4 9 -0.30 0.30 16 4 -8 1.30 0.70 -16 4 8 0.00 0.30 16 4 -7 1.80 0.70 -16 4 7 1.80 0.40 -16 -4 7 3.30 1.30 -16 4 6 2.60 0.40 16 4 -6 5.00 0.80 -16 -4 6 2.10 1.00 -16 4 5 1.10 0.30 16 4 -5 0.70 0.50 -16 -4 5 1.10 0.90 16 4 -4 -0.20 0.40 -16 4 4 -0.30 0.20 -16 -4 4 0.90 0.90 -16 4 3 -0.10 0.20 16 4 -3 0.30 0.50 -16 -4 3 0.80 0.80 16 4 -2 -0.30 0.40 -16 4 2 0.10 0.20 -16 -4 2 0.80 0.80 16 4 -1 0.10 0.50 -16 4 1 0.60 0.30 -16 -4 1 0.80 0.70 16 4 0 -0.10 0.50 -16 4 0 0.30 0.30 -16 -4 0 1.60 0.70 -16 4 -1 -0.10 0.20 16 4 1 -0.40 0.50 -16 -4 -1 1.10 0.70 16 4 2 0.00 0.50 -16 4 -2 0.00 0.30 -16 -4 -2 0.80 0.70 -16 4 -3 0.40 0.30 16 4 3 1.20 0.60 -17 0 12 0.20 0.60 -17 0 11 0.00 0.50 -17 0 10 0.40 0.50 -17 0 9 -0.50 0.40 -17 0 9 0.50 0.40 -17 0 8 1.00 0.40 -17 0 8 0.40 0.50 -17 0 7 1.00 0.50 -17 0 7 -0.20 0.50 -17 0 6 1.20 0.40 -17 0 6 0.60 0.50 -17 0 5 -0.40 0.50 -17 0 5 -0.20 0.30 -17 0 4 9.50 0.90 -17 0 4 8.80 1.00 -17 0 3 0.60 0.40 -17 0 3 -0.80 0.40 -17 0 2 1.60 0.60 -17 0 1 -0.10 0.50 -17 0 0 2.70 0.70 -17 0 -1 -0.50 0.40 -17 0 -2 2.00 0.60 -17 0 -3 -0.30 0.40 -17 0 -4 0.50 0.50 -17 0 -5 -0.30 0.40 -17 0 -6 0.80 0.50 -17 0 -7 -0.10 0.50 -17 1 12 0.80 0.60 -17 1 11 -0.30 0.50 -17 -1 11 0.10 0.60 -17 1 10 1.80 0.70 -17 -1 10 2.30 0.70 -17 -1 10 1.60 0.60 -17 1 9 1.00 0.60 -17 -1 9 2.10 0.70 -17 -1 9 2.50 0.70 -17 1 8 4.40 0.80 -17 -1 8 5.00 0.80 -17 -1 8 4.10 0.80 -17 1 7 3.60 0.70 -17 -1 7 3.90 0.80 -17 -1 7 1.90 0.70 -17 1 6 -0.20 0.40 -17 -1 6 0.30 0.50 -17 -1 6 -0.60 0.40 -17 1 5 7.70 0.90 -17 -1 5 7.50 1.00 -17 -1 5 7.00 1.00 -17 1 4 0.20 0.40 -17 -1 4 0.80 0.50 -17 -1 4 -0.40 0.40 -17 1 3 0.50 0.40 -17 -1 3 0.10 0.40 -17 -1 3 -0.40 0.40 -17 1 2 0.30 0.40 -17 -1 2 0.50 0.50 -17 -1 2 0.90 0.50 -17 1 1 -0.40 0.40 -17 -1 1 -0.10 0.40 -17 -1 1 0.00 0.50 -17 1 0 0.30 0.50 -17 -1 0 1.30 0.50 -17 -1 0 0.30 0.50 -17 1 -1 3.10 0.70 -17 -1 -1 3.30 0.70 -17 1 -2 0.50 0.50 -17 -1 -2 1.40 0.60 -17 1 -3 3.00 0.70 -17 -1 -3 2.10 0.70 -17 1 -4 4.00 0.70 -17 -1 -4 4.50 0.80 -17 1 -5 0.70 0.50 -17 -1 -5 0.60 0.50 -17 1 -6 -0.70 0.40 -17 -1 -6 1.00 0.60 -17 1 -7 0.30 0.50 -17 -1 -7 0.00 0.50 -17 2 11 -0.20 0.50 -17 -2 11 0.70 0.80 -17 2 10 0.20 0.50 17 2 -10 -0.70 0.50 17 2 -10 0.50 0.70 -17 -2 10 0.20 0.70 17 2 -9 -0.20 0.50 -17 2 9 -0.50 0.40 17 2 -9 -0.60 0.50 -17 -2 9 0.40 0.70 -17 2 8 17.90 1.40 17 2 -8 17.10 1.50 -17 -2 8 17.30 1.50 -17 2 7 1.50 0.50 17 2 -7 1.00 0.60 -17 -2 7 0.50 0.70 17 2 -6 0.60 0.50 -17 2 6 1.10 0.50 -17 -2 6 1.30 0.70 17 2 -5 1.30 0.60 -17 2 5 1.70 0.50 -17 -2 5 2.50 0.80 17 2 -4 1.00 0.60 -17 2 4 0.90 0.50 -17 -2 4 1.40 0.70 -17 2 3 7.00 0.80 17 2 -3 5.50 0.90 -17 -2 3 8.20 1.10 -17 2 2 0.40 0.40 17 2 -2 -0.20 0.50 -17 -2 2 1.40 0.60 -17 2 1 9.20 1.00 17 2 -1 10.00 1.20 -17 -2 1 9.60 1.20 17 2 0 0.20 0.40 -17 2 0 -0.30 0.40 -17 -2 0 0.20 0.50 -17 2 -1 0.30 0.40 17 2 1 0.30 0.50 -17 -2 -1 1.40 0.60 -17 2 -2 0.30 0.40 17 2 2 0.90 0.60 -17 -2 -2 1.50 0.60 17 2 3 1.50 0.80 -17 2 -3 0.90 0.50 -17 -2 -3 2.00 0.60 -17 2 -4 2.60 0.60 -17 2 -5 0.20 0.40 -17 2 -6 0.30 0.40 17 3 -10 -0.30 0.60 -17 3 10 -0.10 0.50 -17 -3 10 -0.80 0.80 17 3 -9 0.30 0.60 -17 3 9 0.60 0.50 -17 -3 9 0.30 0.90 -17 3 8 1.80 0.50 17 3 -8 1.40 0.70 -17 -3 8 1.30 1.00 -17 3 7 3.80 0.60 17 3 -7 4.20 0.80 -17 -3 7 4.50 1.20 -17 3 6 0.60 0.40 17 3 -6 2.10 0.70 -17 -3 6 1.20 0.80 17 3 -5 -0.30 0.50 -17 3 5 -0.20 0.30 -17 -3 5 0.00 0.70 -17 3 4 1.60 0.50 17 3 -4 2.80 0.70 -17 -3 4 2.40 0.80 17 3 -3 7.40 1.00 -17 3 3 6.10 0.70 -17 -3 3 6.00 1.10 17 3 -2 0.60 0.60 -17 3 2 0.40 0.40 -17 -3 2 1.70 0.80 -17 3 1 0.40 0.40 17 3 -1 0.50 0.50 -17 -3 1 1.10 0.70 -17 3 0 2.90 0.50 17 3 0 2.80 0.70 -17 -3 0 2.50 0.80 -17 3 -1 0.20 0.30 17 3 1 -0.20 0.50 -17 -3 -1 0.60 0.60 17 3 2 0.60 0.60 -17 3 -2 0.50 0.40 -17 -3 -2 1.00 0.70 -17 3 -3 0.70 0.40 17 3 3 0.90 0.60 -17 -3 -3 1.60 0.70 -17 3 -4 0.80 0.40 17 3 4 0.50 0.60 17 4 -7 1.50 0.60 -17 4 6 0.50 0.30 17 4 -6 0.00 0.50 -17 4 5 -0.10 0.30 17 4 -5 0.70 0.50 -17 4 4 0.00 0.30 17 4 -4 0.60 0.60 17 4 -3 0.00 0.50 -17 4 3 0.30 0.30 17 4 -2 0.10 0.50 -17 4 2 0.00 0.30 17 4 -1 -0.10 0.50 -17 4 1 0.50 0.30 17 4 0 0.20 0.50 -17 4 0 0.30 0.30 -17 4 -1 0.50 0.30 17 4 1 0.40 0.60 -18 0 11 0.30 0.60 -18 0 10 1.90 0.70 -18 0 9 -0.40 0.50 -18 0 8 3.80 0.80 -18 0 8 4.30 0.70 -18 0 7 0.80 0.40 -18 0 7 0.00 0.50 -18 0 6 4.80 0.70 -18 0 6 3.60 0.80 -18 0 5 0.10 0.50 -18 0 5 0.90 0.50 -18 0 4 3.70 0.70 -18 0 4 5.70 0.80 -18 0 3 -0.70 0.40 -18 0 2 0.50 0.50 -18 0 1 -0.40 0.50 -18 0 0 0.40 0.50 -18 0 -1 -0.60 0.50 -18 0 -2 40.40 2.30 -18 0 -3 0.60 0.50 -18 0 -4 1.90 0.60 -18 0 -5 -0.30 0.50 -18 1 11 1.80 0.70 -18 1 10 0.40 0.60 -18 -1 10 0.60 0.60 -18 -1 10 1.60 0.80 -18 1 9 1.50 0.60 -18 -1 9 -0.50 0.40 -18 -1 9 1.30 0.60 -18 1 8 -0.60 0.40 -18 -1 8 -0.40 0.50 -18 -1 8 0.90 0.50 -18 1 7 0.60 0.50 -18 -1 7 -0.10 0.50 -18 -1 7 0.20 0.50 -18 1 6 0.20 0.50 -18 -1 6 0.40 0.50 -18 -1 6 0.40 0.50 -18 1 5 0.10 0.50 -18 -1 5 0.30 0.60 -18 -1 5 0.90 0.60 -18 1 4 7.80 1.00 -18 -1 4 8.70 1.10 -18 -1 4 8.40 1.10 -18 1 3 -0.10 0.40 -18 -1 3 0.60 0.50 -18 -1 3 0.80 0.50 -18 1 2 4.90 0.80 -18 -1 2 7.20 1.00 -18 -1 2 6.10 0.90 -18 1 1 3.30 0.70 -18 -1 1 2.30 0.70 -18 -1 1 2.90 0.70 -18 1 0 1.00 0.60 -18 -1 0 0.00 0.50 -18 -1 0 1.10 0.50 -18 1 -1 7.60 1.00 -18 -1 -1 8.20 1.10 -18 1 -2 6.30 0.90 -18 -1 -2 5.30 0.90 -18 1 -3 0.20 0.50 -18 -1 -3 0.90 0.60 -18 1 -4 2.50 0.70 -18 -1 -4 1.60 0.60 -18 1 -5 1.40 0.60 -18 -1 -5 1.70 0.70 -18 2 10 2.10 0.60 -18 -2 10 2.30 0.90 -18 2 9 0.30 0.50 -18 -2 9 1.30 0.80 -18 2 8 0.60 0.50 -18 -2 8 0.20 0.60 -18 2 7 0.40 0.50 18 2 -7 0.20 0.60 -18 -2 7 1.80 0.80 -18 2 6 0.70 0.50 18 2 -6 1.40 0.70 -18 -2 6 1.80 0.80 18 2 -5 1.60 0.60 -18 2 5 1.80 0.60 -18 -2 5 2.10 0.70 -18 2 4 1.00 0.50 18 2 -4 0.70 0.60 18 2 -3 2.00 0.70 -18 2 3 1.10 0.50 -18 -2 3 2.40 0.80 18 2 -2 -0.10 0.50 -18 2 2 -0.10 0.40 -18 -2 2 0.70 0.60 -18 2 1 1.00 0.50 18 2 -1 0.40 0.50 -18 -2 1 0.30 0.50 -18 2 0 -0.30 0.40 -18 -2 0 0.30 0.50 -18 2 -1 0.90 0.50 -18 -2 -1 1.00 0.60 -18 2 -2 -0.50 0.40 -18 -2 -2 0.80 0.50 -18 2 -3 0.90 0.50 -18 2 -4 2.30 0.60 -18 3 8 13.70 1.20 18 3 -8 13.00 1.40 -18 -3 8 11.80 1.80 18 3 -7 1.40 0.70 -18 3 7 1.40 0.50 -18 -3 7 2.00 1.00 -18 3 6 2.10 0.50 18 3 -6 2.00 0.70 -18 -3 6 4.40 1.10 -18 3 5 0.80 0.40 18 3 -5 0.20 0.60 -18 -3 5 0.90 0.80 18 3 -4 1.00 0.60 -18 3 4 0.00 0.30 -18 -3 4 0.20 0.80 -18 3 3 0.50 0.40 18 3 -3 0.30 0.60 -18 -3 3 1.40 0.80 -18 3 2 0.00 0.40 18 3 -2 -0.10 0.50 -18 -3 2 0.50 0.70 18 3 -1 1.10 0.60 -18 3 1 1.50 0.50 -18 -3 1 2.30 0.90 -18 3 0 0.80 0.40 18 3 0 0.10 0.60 -18 3 -1 0.30 0.40 18 3 1 1.10 0.60 18 3 2 -0.40 0.50 -18 3 -2 0.00 0.40 -19 0 10 2.50 0.80 -19 0 9 -0.20 0.50 -19 0 8 3.60 0.70 -19 0 8 2.10 0.70 -19 0 7 -0.50 0.50 -19 0 7 0.80 0.40 -19 0 6 5.90 0.80 -19 0 6 5.50 0.90 -19 0 5 0.20 0.50 -19 0 4 0.20 0.50 -19 0 3 -0.90 0.40 -19 0 2 -0.50 0.50 -19 0 1 -0.30 0.40 -19 0 0 4.80 0.90 -19 0 -1 1.30 0.60 -19 0 -2 5.10 0.90 -19 0 -3 0.90 0.60 -19 0 -4 0.30 0.50 -19 1 9 0.90 0.60 -19 -1 9 1.70 0.60 -19 -1 9 1.40 0.70 -19 1 8 0.60 0.50 -19 -1 8 0.60 0.60 -19 -1 8 1.20 0.60 -19 1 7 0.40 0.50 -19 -1 7 1.80 0.70 -19 -1 7 0.80 0.60 -19 1 6 0.00 0.50 -19 -1 6 1.20 0.60 -19 -1 6 -0.50 0.40 -19 1 5 1.80 0.60 -19 -1 5 1.90 0.70 -19 -1 5 2.30 0.60 -19 1 4 4.80 0.80 -19 -1 4 5.40 0.90 -19 -1 4 4.30 0.80 -19 1 3 -0.50 0.40 -19 -1 3 0.10 0.50 -19 -1 3 1.20 0.50 -19 1 2 1.50 0.60 -19 -1 2 3.30 0.80 -19 -1 2 2.00 0.70 -19 1 1 0.70 0.50 -19 -1 1 1.10 0.50 -19 -1 1 -0.40 0.50 -19 1 0 0.80 0.50 -19 -1 0 -0.20 0.40 -19 1 -1 0.60 0.50 -19 -1 -1 1.20 0.70 -19 1 -2 1.40 0.60 -19 -1 -2 1.70 0.60 -19 1 -3 0.00 0.50 -19 -1 -3 0.30 0.60 -19 -2 8 3.70 0.90 -19 2 7 -0.80 0.40 -19 -2 7 0.90 0.70 -19 2 6 0.80 0.50 -19 -2 6 1.90 0.70 -19 2 5 0.90 0.50 -19 -2 5 1.70 0.80 -19 2 4 5.20 0.80 -19 -2 4 5.70 1.00 -19 2 3 0.60 0.50 -19 -2 3 2.40 0.80 -19 2 2 0.00 0.40 -19 -2 2 1.30 0.60 -19 2 1 2.10 0.60 -19 -2 1 3.80 1.00 -19 2 -1 0.10 0.50 -19 2 -2 0.50 0.50 19 3 -4 1.20 0.70 -19 3 4 0.40 0.40 -19 3 3 0.80 0.40 19 3 -3 0.90 0.60 19 3 -2 1.50 0.70 -19 3 2 1.30 0.40 -20 0 7 -0.40 0.50 -20 0 6 0.10 0.50 -20 0 5 1.30 0.60 -20 0 4 1.40 0.70 -20 0 3 -0.10 0.50 -20 0 2 0.90 0.60 -20 0 1 -0.30 0.50 -20 0 0 6.00 1.00 -20 0 -1 1.20 0.60 -20 1 7 1.50 0.70 -20 -1 7 1.10 0.60 -20 -1 7 1.20 0.50 -20 1 6 0.20 0.50 -20 -1 6 -0.40 0.50 -20 -1 6 1.40 0.60 -20 1 5 0.10 0.50 -20 -1 5 0.90 0.50 -20 -1 5 -0.30 0.50 -20 1 4 0.20 0.50 -20 -1 4 0.60 0.60 -20 -1 4 0.90 0.50 -20 1 3 -0.30 0.50 -20 -1 3 0.20 0.60 -20 -1 3 0.90 0.50 -20 1 2 0.20 0.50 -20 -1 2 2.80 0.80 -20 -1 2 0.50 0.60 -20 1 1 -0.40 0.50 -20 -1 1 -0.40 0.50 -20 1 0 0.30 0.50 -20 -1 0 1.10 0.60 -20 2 4 1.10 0.60 -20 2 3 1.10 0.50 -20 2 2 3.30 0.70 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 7041 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_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 O1 O 0.43294(14) 0.5572(4) 0.87691(16) 0.0550(6) Uani 1 1 d . . N1 N 0.19124(15) 0.5844(4) 0.32705(18) 0.0433(6) Uani 1 1 d . . C1 C 0.16475(17) 0.3693(5) 0.3544(2) 0.0415(7) Uani 1 1 d . . C2 C 0.10823(19) 0.2408(5) 0.2819(2) 0.0475(7) Uani 1 1 d . . H2 H 0.088238 0.098001 0.298925 0.057 Uiso 1 1 calc R U N2 N 0.19936(16) 0.3229(4) 0.44875(19) 0.0464(6) Uani 1 1 d . . C5 C 0.1661(2) 0.6678(6) 0.2315(2) 0.0503(8) Uani 1 1 d . . H5 H 0.185591 0.810890 0.214185 0.060 Uiso 1 1 calc R U C7 C 0.24839(17) 0.5138(5) 0.4822(2) 0.0423(7) Uani 1 1 d . . C6 C 0.24382(19) 0.6760(5) 0.4092(2) 0.0475(7) Uani 1 1 d . . H6 H 0.270828 0.819411 0.414039 0.057 Uiso 1 1 calc R U C9 C 0.3491(2) 0.7172(5) 0.6168(2) 0.0489(7) Uani 1 1 d . . H9 H 0.352374 0.836925 0.572449 0.059 Uiso 1 1 calc R U C8 C 0.29815(17) 0.5270(5) 0.5844(2) 0.0419(7) Uani 1 1 d . . C11 C 0.39111(17) 0.5574(5) 0.7801(2) 0.0444(7) Uani 1 1 d . . C10 C 0.3954(2) 0.7351(5) 0.7137(2) 0.0487(7) Uani 1 1 d . . H10 H 0.428915 0.865047 0.733579 0.058 Uiso 1 1 calc R U C3 C 0.08267(19) 0.3216(6) 0.1882(2) 0.0497(8) Uani 1 1 d . . C4 C 0.1134(2) 0.5413(6) 0.1638(3) 0.0534(8) Uani 1 1 d . . H4 H 0.096551 0.598215 0.099516 0.064 Uiso 1 1 calc R U C14 C 0.0253(2) 0.1869(7) 0.1078(3) 0.0675(10) Uani 1 1 d . . H14A H 0.009394 0.043507 0.134580 0.101 Uiso 1 1 calc R U H14B H 0.055835 0.156590 0.054577 0.101 Uiso 1 1 calc R U H14C H -0.025923 0.274796 0.082948 0.101 Uiso 1 1 calc R U C13 C 0.29556(18) 0.3490(5) 0.6528(2) 0.0458(7) Uani 1 1 d . . H13 H 0.262662 0.217991 0.633106 0.055 Uiso 1 1 calc R U C12 C 0.34102(18) 0.3647(5) 0.7491(2) 0.0466(7) Uani 1 1 d . . H12 H 0.338024 0.244964 0.793636 0.056 Uiso 1 1 calc R U C15 C 0.4815(2) 0.7575(7) 0.9135(3) 0.0635(9) Uani 1 1 d . . H15A H 0.527581 0.779620 0.877097 0.095 Uiso 1 1 calc R U H15B H 0.505463 0.737370 0.982763 0.095 Uiso 1 1 calc R U H15C H 0.444271 0.890013 0.905070 0.095 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 O1 0.0573(13) 0.0561(14) 0.0493(13) 0.0027(10) 0.0039(10) -0.0031(11) N1 0.0426(12) 0.0404(13) 0.0488(14) -0.0008(10) 0.0134(10) -0.0003(10) C1 0.0410(14) 0.0349(15) 0.0510(17) -0.0050(12) 0.0146(12) -0.0018(11) C2 0.0470(16) 0.0433(16) 0.0542(18) -0.0065(13) 0.0148(14) -0.0077(13) N2 0.0492(14) 0.0414(14) 0.0501(15) -0.0025(11) 0.0129(11) -0.0054(11) C5 0.0553(18) 0.0460(17) 0.0501(18) 0.0061(13) 0.0111(14) -0.0029(14) C7 0.0414(14) 0.0407(15) 0.0471(16) -0.0050(12) 0.0146(12) -0.0029(12) C6 0.0490(16) 0.0386(16) 0.0549(18) -0.0053(13) 0.0095(13) -0.0088(13) C9 0.0590(18) 0.0412(16) 0.0487(17) 0.0007(13) 0.0161(14) -0.0082(13) C8 0.0421(14) 0.0381(15) 0.0486(16) -0.0043(12) 0.0168(12) 0.0004(11) C11 0.0387(14) 0.0457(16) 0.0494(17) 0.0006(13) 0.0096(12) 0.0022(12) C10 0.0531(17) 0.0425(16) 0.0515(17) -0.0061(13) 0.0120(14) -0.0113(13) C3 0.0416(15) 0.0522(19) 0.0562(18) -0.0096(14) 0.0115(13) -0.0037(13) C4 0.0515(17) 0.0543(19) 0.0529(18) 0.0003(15) 0.0059(14) 0.0016(14) C14 0.067(2) 0.073(3) 0.060(2) -0.0144(18) 0.0057(17) -0.0162(19) C13 0.0428(15) 0.0395(16) 0.0576(18) -0.0021(13) 0.0157(13) -0.0038(12) C12 0.0500(16) 0.0381(16) 0.0531(17) 0.0041(13) 0.0134(13) 0.0016(13) C15 0.066(2) 0.071(2) 0.0512(19) -0.0038(17) 0.0034(16) -0.0159(18) 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 C11 O1 C15 118.0(2) C6 N1 C5 131.5(3) C6 N1 C1 107.0(2) C5 N1 C1 121.5(3) N2 C1 N1 110.7(2) N2 C1 C2 131.6(3) N1 C1 C2 117.7(3) C3 C2 C1 121.3(3) C3 C2 H2 119.4 C1 C2 H2 119.4 C1 N2 C7 105.2(2) C4 C5 N1 119.6(3) C4 C5 H5 120.2 N1 C5 H5 120.2 C6 C7 N2 111.1(3) C6 C7 C8 127.3(3) N2 C7 C8 121.5(3) C7 C6 N1 106.0(3) C7 C6 H6 127.0 N1 C6 H6 127.0 C8 C9 C10 122.2(3) C8 C9 H9 118.9 C10 C9 H9 118.9 C9 C8 C13 117.3(3) C9 C8 C7 121.3(3) C13 C8 C7 121.4(3) O1 C11 C10 124.3(3) O1 C11 C12 116.1(3) C10 C11 C12 119.6(3) C11 C10 C9 119.2(3) C11 C10 H10 120.4 C9 C10 H10 120.4 C2 C3 C4 118.6(3) C2 C3 C14 123.0(3) C4 C3 C14 118.4(3) C5 C4 C3 121.3(3) C5 C4 H4 119.3 C3 C4 H4 119.3 C3 C14 H14A 109.5 C3 C14 H14B 109.5 H14A C14 H14B 109.5 C3 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C12 C13 C8 121.1(3) C12 C13 H13 119.5 C8 C13 H13 119.5 C13 C12 C11 120.6(3) C13 C12 H12 119.7 C11 C12 H12 119.7 O1 C15 H15A 109.5 O1 C15 H15B 109.5 H15A C15 H15B 109.5 O1 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C11 1.365(4) O1 C15 1.428(4) N1 C6 1.372(4) N1 C5 1.381(4) N1 C1 1.387(4) C1 N2 1.332(4) C1 C2 1.414(4) C2 C3 1.354(4) C2 H2 0.9300 N2 C7 1.377(4) C5 C4 1.340(4) C5 H5 0.9300 C7 C6 1.364(4) C7 C8 1.472(4) C6 H6 0.9300 C9 C8 1.386(4) C9 C10 1.393(4) C9 H9 0.9300 C8 C13 1.398(4) C11 C10 1.382(4) C11 C12 1.387(4) C10 H10 0.9300 C3 C4 1.423(5) C3 C14 1.505(4) C4 H4 0.9300 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C13 C12 1.380(4) C13 H13 0.9300 C12 H12 0.9300 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600