#------------------------------------------------------------------------------ #$Date: 2023-12-12 17:51:05 +0200 (Tue, 12 Dec 2023) $ #$Revision: 288256 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515830.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_4515830 loop_ _publ_author_name 'Panda, Subhankar' 'Pradhan, Nirmalya' 'Manna, Debasis' _publ_section_title ; Ring-Opening of Indoles: An Unconventional Route for the Transformation of Indoles to 1 H-Pyrazoles Using Lewis Acid. ; _journal_issue 10 _journal_name_full 'ACS combinatorial science' _journal_page_first 573 _journal_page_last 578 _journal_paper_doi 10.1021/acscombsci.8b00071 _journal_volume 20 _journal_year 2018 _chemical_formula_moiety 'C23 H16 N4 O' _chemical_formula_sum 'C23 H16 N4 O' _chemical_formula_weight 364.40 _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 _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 107.132(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5286(9) _cell_length_b 9.9810(6) _cell_length_c 16.3134(14) _cell_measurement_reflns_used 1079 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 20.02 _cell_measurement_theta_min 3.39 _cell_volume 1949.4(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0853 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7144 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.048 _diffrn_reflns_theta_max 25.048 _diffrn_reflns_theta_min 3.175 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.382 _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details multi-scan _exptl_crystal_colour Pink _exptl_crystal_density_diffrn 1.242 _exptl_crystal_description Needle _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.183 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 3444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.0644 _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^)+(0.0575P)^2^+0.0972P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1289 _refine_ls_wR_factor_ref 0.1759 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1802 _reflns_number_total 3444 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file co8b00071_si_002.cif _cod_data_source_block exp_4814 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4515830 _shelx_shelxl_version_number 2014/7 _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_res_file ; exp_4814.res created by SHELXL-2014/7 TITL exp_4814_a.res in P2(1)/n CELL 0.71073 12.5286 9.981 16.3134 90 107.132 90 ZERR 4 0.0009 0.0006 0.0014 0 0.008 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 92 64 16 4 OMIT -3 50.1 L.S. 10 ACTA BOND $H FMAP 2 PLAN 1 WGHT 0.057500 0.097190 FVAR 0.61774 O22 4 0.217724 0.332852 0.409339 11.00000 0.07603 0.05274 = 0.10470 -0.02299 0.05408 -0.02776 N3 3 0.379710 0.413258 0.396682 11.00000 0.05261 0.04208 = 0.05561 -0.00541 0.02292 -0.01100 AFIX 43 H20 2 0.423989 0.480878 0.403315 11.00000 -1.20000 AFIX 0 N2 3 0.469357 0.565974 0.143413 11.00000 0.05923 0.05607 = 0.06129 0.01154 0.02947 0.01579 N1 3 0.375161 0.599378 0.163652 11.00000 0.06125 0.06044 = 0.06876 0.02028 0.02690 0.02613 AFIX 43 H7 2 0.336686 0.670230 0.144819 11.00000 -1.20000 AFIX 0 C9 1 0.428456 0.411213 0.232519 11.00000 0.04312 0.04607 = 0.04523 0.00173 0.01788 0.00570 C12 1 0.603051 0.385194 0.176548 11.00000 0.05211 0.04248 = 0.05011 0.00585 0.02326 0.00924 C23 1 0.257208 0.556569 0.452840 11.00000 0.04898 0.04440 = 0.04887 -0.00397 0.01785 -0.00636 C6 1 0.410296 0.290615 0.363504 11.00000 0.04687 0.04026 = 0.04981 0.00160 0.01616 0.00025 C10 1 0.501732 0.450869 0.185786 11.00000 0.05177 0.04587 = 0.04768 0.00736 0.01917 0.01311 C1 1 0.432216 0.289805 0.284281 11.00000 0.04480 0.04524 = 0.04803 0.00181 0.01775 0.00564 C21 1 0.283893 0.426111 0.417821 11.00000 0.05032 0.04987 = 0.05165 -0.00187 0.02366 -0.00750 C13 1 0.618822 0.377011 0.096261 11.00000 0.05477 0.05270 = 0.05412 0.01429 0.02325 0.01279 AFIX 43 H13 2 0.565903 0.414132 0.049278 11.00000 -1.20000 AFIX 0 C15 1 0.790349 0.259779 0.154621 11.00000 0.05094 0.05922 = 0.06116 0.00582 0.02833 0.01623 C8 1 0.348214 0.510566 0.216039 11.00000 0.05616 0.06092 = 0.05465 0.01034 0.02320 0.01026 AFIX 43 H8 2 0.287058 0.515063 0.237244 11.00000 -1.20000 AFIX 0 N19 3 0.956913 0.140346 0.123042 11.00000 0.07808 0.11386 = 0.07536 0.01568 0.04101 0.04241 C2 1 0.459508 0.166658 0.254241 11.00000 0.06517 0.05298 = 0.06183 0.00308 0.02802 0.00970 AFIX 43 H2 2 0.473103 0.163303 0.201226 11.00000 -1.20000 AFIX 0 C14 1 0.711276 0.315018 0.084643 11.00000 0.06381 0.06606 = 0.05157 0.00657 0.02890 0.01515 AFIX 43 H14 2 0.720710 0.310169 0.030269 11.00000 -1.20000 AFIX 0 C17 1 0.684176 0.331500 0.246648 11.00000 0.06056 0.07952 = 0.04847 0.00934 0.02312 0.02162 AFIX 43 H17 2 0.675907 0.338430 0.301303 11.00000 -1.20000 AFIX 0 C5 1 0.417943 0.173640 0.410278 11.00000 0.06473 0.05716 = 0.05444 0.00669 0.02408 -0.00048 AFIX 43 H5 2 0.403368 0.175609 0.462964 11.00000 -1.20000 AFIX 0 C16 1 0.777034 0.267881 0.235277 11.00000 0.05612 0.07844 = 0.05539 0.01043 0.02128 0.02410 AFIX 43 H16 2 0.830286 0.230708 0.282041 11.00000 -1.20000 AFIX 0 C3 1 0.466725 0.050259 0.301303 11.00000 0.06742 0.03977 = 0.08058 0.00278 0.02295 0.00763 AFIX 43 H3 2 0.484895 -0.030277 0.280032 11.00000 -1.20000 AFIX 0 C4 1 0.446811 0.054132 0.380122 11.00000 0.07072 0.05100 = 0.07301 0.01502 0.02449 0.00673 AFIX 43 H4 2 0.452842 -0.023491 0.412709 11.00000 -1.20000 AFIX 0 C18 1 0.884922 0.192690 0.139698 11.00000 0.06515 0.07064 = 0.06215 0.01256 0.03027 0.01598 C28 1 0.167314 0.557052 0.485077 11.00000 0.07746 0.05866 = 0.09396 -0.00776 0.05102 -0.00514 AFIX 43 H28 2 0.127746 0.478142 0.484831 11.00000 -1.20000 AFIX 0 C26 1 0.191547 0.787169 0.517298 11.00000 0.07509 0.05950 = 0.10130 -0.01688 0.02586 0.01117 AFIX 43 H26 2 0.169591 0.865619 0.538532 11.00000 -1.20000 AFIX 0 C27 1 0.134747 0.672526 0.517792 11.00000 0.08300 0.07641 = 0.10106 -0.00552 0.05172 0.01181 AFIX 43 H27 2 0.074308 0.671238 0.539920 11.00000 -1.20000 AFIX 0 C24 1 0.314366 0.673468 0.453621 11.00000 0.07168 0.05568 = 0.14365 -0.02026 0.05989 -0.01518 AFIX 43 H24 2 0.375697 0.675847 0.432543 11.00000 -1.20000 AFIX 0 C25 1 0.279775 0.788580 0.486250 11.00000 0.08887 0.05041 = 0.17823 -0.02940 0.05842 -0.01255 AFIX 43 H25 2 0.318389 0.868271 0.486645 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_4814_a.res in P2(1)/n REM R1 = 0.0644 for 1802 Fo > 4sig(Fo) and 0.1314 for all 3444 data REM 253 parameters refined using 0 restraints END WGHT 0.0501 0.0096 REM Highest difference peak 0.183, deepest hole -0.184, 1-sigma level 0.043 Q1 1 0.5752 0.3812 -0.0001 11.00000 0.05 0.18 ; _shelx_res_checksum 26069 _shelx_hkl_file ; 0 0 -3 -0.65 1.17 0 0 3 1.06 1.44 0 0 4 97.84 9.26 0 0 -4 87.87 8.43 0 0 5 0.98 1.42 0 0 -5 0.73 1.16 0 0 -6 357.78 21.08 0 0 6 372.72 22.20 0 0 -7 0.18 2.49 0 0 -8 555.22 30.81 0 0 -9 -5.54 3.97 0 0 -10 5.67 4.65 0 0 -11 2.22 1.94 0 0 -12 86.16 14.60 0 0 -12 78.23 14.42 0 0 -13 3.99 2.76 0 0 -13 -3.38 1.80 0 0 -14 -4.66 5.49 0 0 -14 0.62 2.94 0 0 -15 1.38 3.64 0 0 -15 -1.68 1.76 0 0 -16 11.45 6.20 0 0 -16 20.87 8.70 0 0 -17 -4.68 5.30 0 0 -17 0.69 2.05 0 0 -18 11.72 8.51 0 0 -19 6.75 5.77 0 0 -20 2.29 3.39 0 1 2 8.28 2.25 0 -1 3 4914.31 59.62 0 1 3 4721.86 57.87 0 -1 -3 4861.34 58.58 0 -1 4 36.42 6.00 0 -1 -4 33.64 5.49 0 1 4 38.08 5.91 0 1 5 1189.87 36.68 0 -1 -5 1179.96 36.18 0 1 -5 1174.06 35.68 0 -1 5 1190.76 37.38 0 -1 6 20.32 5.27 0 1 -6 16.47 4.68 0 1 6 12.57 3.99 0 -1 -6 16.67 2.62 0 -1 -6 11.34 3.96 0 -1 -7 44.98 8.38 0 1 -7 50.64 8.95 0 -1 -7 38.86 3.89 0 -1 -8 111.13 13.94 0 -1 -8 88.73 5.70 0 1 -8 113.78 13.86 0 -1 -9 1.62 1.65 0 1 -9 0.18 3.25 0 -1 -10 0.23 3.60 0 1 -10 1.87 3.76 0 -1 -11 0.81 2.74 0 1 -11 1.38 3.51 0 1 -12 30.56 8.88 0 -1 -12 37.09 10.02 0 1 -12 24.81 7.92 0 -1 -13 13.37 6.21 0 1 -13 21.92 8.61 0 1 -13 14.12 5.70 0 -1 -13 11.05 5.30 0 -1 -14 8.46 4.97 0 1 -14 -5.58 5.21 0 -1 -14 0.61 3.99 0 1 -15 2.64 2.65 0 -1 -15 3.88 3.14 0 -1 -16 27.64 10.66 0 -1 -16 14.72 5.95 0 1 -16 32.50 9.28 0 1 -17 15.38 7.56 0 -1 -17 10.43 6.74 0 -1 -17 0.30 2.16 0 -1 -18 12.35 9.89 0 -1 -18 3.40 4.65 0 1 -18 10.32 6.49 0 -1 -19 3.98 7.51 0 1 -19 9.96 7.07 0 -1 -19 9.20 6.75 0 -1 -20 0.55 2.27 0 -1 -20 4.09 2.66 0 -2 0 1057.52 19.11 0 -2 -1 200.79 11.32 0 -2 -2 228.03 13.49 0 2 2 241.19 13.30 0 2 3 3.76 1.59 0 -2 -3 3.61 1.63 0 -2 -4 166.09 13.31 0 2 4 162.42 13.13 0 -2 5 542.40 26.82 0 2 5 560.75 26.12 0 -2 -5 532.17 25.91 0 2 6 46.14 8.02 0 -2 -6 51.75 9.09 0 -2 -7 317.69 22.82 0 -2 -8 263.58 22.04 0 -2 -8 271.23 14.49 0 -2 -9 492.39 31.95 0 -2 -9 502.68 19.68 0 -2 -10 84.89 13.92 0 -2 -10 100.13 8.39 0 -2 10 80.25 5.11 0 2 -11 -1.20 2.86 0 -2 -11 0.34 0.47 0 2 -12 54.62 9.91 0 -2 -12 65.85 13.67 0 -2 -12 48.94 11.94 0 2 -13 134.14 16.87 0 -2 -13 117.39 18.80 0 -2 -13 105.03 17.72 0 2 -14 12.34 4.61 0 -2 -14 10.42 6.79 0 -2 -15 -0.84 1.84 0 -2 -15 0.60 3.27 0 2 -15 5.88 4.65 0 2 -16 3.39 2.28 0 -2 -16 -0.77 4.29 0 -2 -16 2.98 3.92 0 -2 -17 -1.24 5.22 0 2 -17 -12.95 6.34 0 -2 -17 8.72 6.73 0 -2 -18 19.35 8.79 0 -2 -18 8.98 5.28 0 -2 -19 -7.77 6.29 0 -2 -19 2.28 3.82 0 -2 -20 -4.78 5.19 0 -2 -20 0.02 3.33 0 -3 0 1.37 1.02 0 -3 1 68.31 4.70 0 -3 -1 73.88 7.41 0 -3 -2 675.75 26.56 0 -3 -3 1433.12 41.09 0 3 3 1425.96 39.07 0 3 4 27.74 5.84 0 -3 -4 21.22 5.51 0 -3 -5 1.86 2.11 0 -3 -6 719.82 33.96 0 -3 -7 8.24 4.32 0 -3 -8 11.40 5.80 0 -3 -9 61.93 8.44 0 3 -9 74.01 9.05 0 -3 -9 90.60 14.48 0 -3 -10 27.99 5.92 0 -3 -10 23.67 7.15 0 3 -10 28.51 6.26 0 -3 -11 151.62 20.52 0 -3 -11 153.80 20.09 0 3 -11 153.02 14.93 0 -3 11 148.25 10.18 0 -3 -11 158.63 13.60 0 -3 -12 26.85 8.81 0 -3 -12 20.40 7.75 0 3 -12 22.39 6.39 0 3 -13 39.23 8.55 0 -3 -13 31.21 10.89 0 -3 -13 22.16 9.20 0 3 -14 20.98 7.26 0 -3 -14 22.92 9.19 0 -3 -14 10.38 7.06 0 -3 -15 70.08 16.38 0 -3 -15 57.87 14.04 0 3 -15 60.35 11.73 0 -3 -16 2.65 2.06 0 -3 -16 4.45 4.73 0 -3 -17 6.35 5.96 0 -3 -17 -4.09 3.24 0 -3 -18 10.80 6.53 0 -3 -18 2.28 6.37 0 -3 -19 12.59 8.80 0 -3 -19 -6.44 5.68 0 -4 0 295.86 14.18 0 -4 -1 235.30 14.45 0 -4 1 190.16 9.75 0 -4 -2 100.21 10.86 0 -4 -2 89.97 11.58 0 -4 2 93.71 5.30 0 -4 -3 8.56 4.00 0 -4 -3 4.97 2.38 0 -4 -4 498.89 27.89 0 -4 -5 4.04 2.03 0 -4 -6 189.47 18.72 0 4 -6 190.52 7.09 0 4 -7 51.18 4.85 0 -4 -7 51.60 10.09 0 -4 -8 0.17 1.87 0 4 -8 0.67 0.86 0 -4 -9 89.35 14.87 0 4 -9 108.01 9.64 0 -4 -9 100.10 15.99 0 4 -10 12.53 3.63 0 -4 -10 6.97 5.82 0 -4 -10 2.31 1.78 0 -4 -11 -1.15 3.03 0 -4 -11 -4.12 5.84 0 4 -11 1.01 1.82 0 -4 -12 110.77 19.72 0 4 -12 102.49 11.96 0 -4 -12 93.25 16.63 0 -4 -13 28.24 10.36 0 -4 -13 39.55 11.30 0 4 -13 30.69 7.02 0 -4 -14 80.12 17.42 0 -4 -14 63.07 15.46 0 -4 -15 9.18 6.25 0 -4 -15 24.61 11.14 0 -4 -16 4.68 5.16 0 -4 -16 15.47 7.62 0 -4 -17 3.79 7.20 0 -4 -17 -0.90 2.26 0 -4 -18 -5.67 5.62 0 -4 -18 2.65 3.96 0 -4 -19 -0.27 2.38 0 -5 0 -0.07 1.10 0 -5 -1 0.23 1.29 0 -5 1 -0.30 0.72 0 -5 -2 214.20 16.47 0 -5 -2 217.06 19.69 0 -5 2 200.45 9.49 0 -5 -3 585.62 29.88 0 -5 -3 672.50 35.20 0 -5 -4 12.01 5.42 0 -5 -4 17.85 5.52 0 -5 -5 30.68 8.17 0 -5 -5 33.28 8.39 0 -5 -6 206.65 21.01 0 -5 -6 208.87 20.77 0 -5 -7 98.80 15.04 0 -5 -7 91.49 14.71 0 -5 -8 37.39 9.96 0 -5 -8 23.33 6.34 0 5 -9 69.43 5.68 0 -5 -9 75.75 14.44 0 -5 -9 68.37 13.76 0 -5 -10 19.26 9.15 0 -5 -10 16.86 7.52 0 5 -10 14.04 3.05 0 -5 -11 37.56 10.46 0 -5 -11 46.18 12.66 0 -5 -12 8.55 5.12 0 -5 -12 0.05 4.80 0 -5 -13 0.03 2.37 0 -5 -13 3.37 6.11 0 -5 -14 30.89 11.97 0 -5 -14 3.10 3.98 0 -5 -15 -0.70 3.30 0 -5 -15 2.26 7.27 0 -5 -16 21.92 10.68 0 -5 -16 1.84 4.52 0 -5 -17 1.55 3.21 0 -5 -17 8.63 5.91 0 -5 -18 3.95 4.09 0 -5 -18 -7.28 6.33 0 -6 0 8.33 3.04 0 -6 -1 3.17 2.49 0 -6 1 3.41 2.26 0 -6 -2 56.48 8.82 0 -6 2 50.21 5.40 0 -6 -2 57.50 10.91 0 -6 -3 63.60 10.25 0 -6 3 63.94 4.84 0 -6 -3 79.91 13.55 0 -6 -4 107.64 14.01 0 -6 -4 95.29 14.57 0 -6 -5 1.86 2.81 0 -6 -5 0.17 3.23 0 -6 -6 191.76 21.89 0 -6 -6 191.02 20.67 0 -6 -7 5.28 4.96 0 -6 -7 0.16 3.22 0 -6 -8 3.51 4.26 0 -6 -8 2.82 4.59 0 -6 -9 9.03 5.08 0 -6 -9 2.49 3.57 0 -6 -10 9.97 6.59 0 -6 -10 2.81 2.69 0 -6 -11 8.73 5.20 0 -6 -11 0.73 4.24 0 -6 -12 4.20 3.35 0 -6 -12 2.19 4.74 0 -6 -13 2.58 3.31 0 -6 -13 2.23 2.97 0 -6 -14 5.14 4.68 0 -6 -14 2.86 4.00 0 -6 -15 9.04 5.42 0 -6 -15 7.78 7.10 0 -6 -16 -0.37 4.53 0 -6 -16 13.06 5.59 0 -6 -17 10.72 7.14 0 -6 -17 0.97 3.03 0 -7 0 0.40 1.59 0 -7 -1 1.83 2.55 0 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5.07 12 -8 -5 -13.84 8.32 12 -8 -4 0.56 2.37 12 -8 -3 15.34 8.61 -12 -8 2 -2.28 4.15 -12 -8 1 15.76 9.76 -12 -8 0 3.80 4.52 12 -9 -6 3.27 7.64 12 -9 -5 14.79 9.32 12 -9 -4 3.93 4.84 12 -9 -3 10.90 7.67 13 0 -17 4.13 5.08 13 0 -16 -5.33 5.52 13 0 -15 -4.36 4.89 13 0 -14 1.47 6.03 13 0 -14 2.11 2.81 13 0 -13 -0.20 2.57 13 0 -13 7.77 6.16 13 0 -12 -0.50 2.46 13 0 -12 -2.40 3.52 13 0 -11 8.40 7.45 13 0 -11 4.29 4.38 13 0 -10 -5.99 3.72 13 0 -10 2.56 3.20 13 0 -9 0.67 4.50 13 0 -9 20.51 8.19 13 0 -8 2.50 4.97 13 0 -8 3.86 4.62 13 0 -7 17.60 9.38 13 0 -6 6.47 5.54 13 0 -5 -6.91 5.44 13 0 -4 -4.96 7.13 13 0 -3 49.31 14.67 13 0 -2 -2.09 5.93 13 0 -1 -11.90 11.03 13 0 0 -3.57 4.69 13 0 1 3.45 6.16 13 0 2 -3.22 4.69 13 0 3 3.11 4.08 13 0 4 -3.42 4.63 13 0 5 -4.90 5.39 -13 0 -5 1.42 5.67 13 0 6 -8.34 6.85 -13 0 -6 -5.42 5.50 13 0 7 4.21 6.52 -13 0 -7 -1.80 3.55 13 1 -17 1.59 2.93 13 1 -16 10.39 7.03 13 -1 -16 -0.19 4.78 13 1 -15 1.72 4.22 13 -1 -15 -7.41 6.33 13 1 -14 -7.79 6.04 13 1 -14 0.21 3.88 13 -1 -14 1.91 3.18 13 -1 -14 1.36 5.29 13 1 -13 -7.09 5.90 13 -1 -13 15.98 7.58 13 -1 -13 17.51 9.09 13 1 -12 4.96 3.76 13 -1 -12 -2.59 5.76 13 -1 -12 5.42 3.76 13 1 -11 13.06 7.22 13 1 -11 1.95 3.36 13 -1 -11 2.61 4.08 13 -1 -11 10.55 5.78 13 1 -10 7.27 5.14 13 1 -10 22.85 9.25 13 -1 -10 6.09 3.43 13 -1 -10 15.98 7.20 13 1 -9 -3.23 3.34 13 1 -9 5.27 2.68 13 -1 -9 3.15 3.63 13 1 -8 1.13 3.14 13 -1 -8 6.37 4.25 13 1 -7 -3.37 3.35 13 1 -6 14.52 9.19 13 1 -5 32.26 11.62 13 1 -4 25.43 11.14 13 1 -3 6.06 6.70 13 1 -2 18.83 9.87 13 1 -1 3.45 4.70 13 1 0 -16.88 9.14 13 -1 0 -17.24 9.89 13 1 1 -5.27 5.46 13 -1 1 -1.44 5.01 13 1 2 14.42 9.21 13 -1 2 6.83 7.24 13 1 3 2.89 5.07 -13 -1 -3 9.22 8.22 13 1 4 13.36 8.79 13 -1 4 19.67 8.22 -13 -1 -4 7.04 7.84 13 -1 5 -5.29 5.76 -13 -1 -5 -5.35 5.63 -13 -1 -6 -3.03 4.44 13 -1 6 0.02 5.19 13 1 6 0.71 2.70 -13 -1 -7 10.24 7.37 13 -1 7 4.27 5.09 13 1 7 9.24 8.33 -13 1 -7 8.98 9.56 -13 1 -8 14.79 9.51 13 2 -17 8.68 8.03 13 2 -16 3.75 4.64 13 -2 -16 -5.34 5.64 13 2 -15 2.03 4.21 13 -2 -15 0.07 4.91 13 2 -14 14.60 7.97 13 -2 -14 10.83 8.33 13 2 -14 7.02 5.90 13 2 -13 -3.22 6.22 13 -2 -13 4.69 5.10 13 2 -13 2.68 3.67 13 2 -12 3.01 3.53 13 2 -12 1.23 2.95 13 -2 -12 8.70 6.81 13 2 -11 -6.89 6.76 13 -2 -11 -6.64 5.81 13 2 -10 0.27 2.67 13 -2 -10 12.20 5.97 13 2 -9 32.43 10.98 13 -2 -9 38.75 12.06 13 2 -8 2.78 2.34 13 -2 -8 0.86 3.21 13 2 -7 27.96 10.68 13 -2 -7 29.40 9.92 13 2 -6 17.04 8.19 13 2 -5 5.33 2.38 13 2 -4 4.90 5.78 13 2 -3 -2.70 5.51 13 2 -2 -2.85 4.92 13 2 -1 12.78 8.52 13 2 0 11.28 6.51 13 2 1 4.10 5.22 13 2 2 22.53 11.06 -13 -2 -2 -0.82 2.66 13 2 3 11.40 8.24 -13 -2 -3 -4.89 5.62 13 -2 4 8.70 7.55 -13 -2 -4 -0.33 2.20 -13 -2 -5 4.88 5.48 13 -2 5 29.93 13.28 13 2 5 14.79 8.62 -13 -2 -6 3.43 4.76 13 2 6 1.24 2.20 13 2 7 0.80 6.06 13 -2 7 -0.13 2.35 13 -3 -16 5.40 4.20 13 -3 -15 1.83 5.03 13 3 -14 1.47 2.14 13 -3 -14 0.67 3.38 13 3 -13 -5.26 4.96 13 -3 -13 10.84 7.88 13 3 -12 -3.99 4.42 13 -3 -12 4.27 5.93 13 3 -11 2.34 3.39 13 -3 -11 4.16 3.98 13 3 -10 -2.64 4.07 13 -3 -10 8.22 5.59 13 -3 -9 9.69 5.27 13 3 -9 20.69 10.94 13 -3 -8 51.68 13.62 13 3 -8 67.24 17.15 13 -3 -7 4.66 4.68 13 3 -7 9.02 6.70 13 3 -6 0.26 4.14 13 3 -5 11.94 8.80 13 3 -4 0.08 5.48 13 3 -3 -6.00 9.19 13 3 -2 4.54 4.80 13 3 -1 15.57 8.13 13 3 0 7.93 6.25 13 3 1 3.15 5.61 -13 -3 -1 15.44 9.30 13 3 2 4.16 6.86 -13 -3 -2 -18.14 9.82 13 3 3 25.27 12.76 -13 -3 -3 -1.73 6.32 -13 -3 -4 2.18 2.67 13 3 4 -0.34 2.36 -13 -3 -5 -10.53 7.76 13 3 5 8.04 7.40 13 3 6 -0.02 2.65 13 3 7 13.29 9.99 13 -3 7 6.09 3.40 13 -4 -15 3.32 3.85 13 4 -14 10.55 6.69 13 -4 -14 2.15 3.29 13 4 -13 4.68 7.50 13 -4 -13 1.35 4.88 13 4 -12 30.66 11.31 13 -4 -12 20.06 9.61 13 -4 -11 69.33 17.92 13 4 -11 72.76 17.78 13 -4 -10 30.00 11.41 13 4 -10 24.74 11.15 13 -4 -9 12.95 6.63 13 4 -9 12.63 8.12 13 -4 -8 5.52 3.43 13 4 -8 2.22 6.22 13 -4 -7 1.70 3.25 13 4 -7 0.89 3.84 13 4 -6 11.47 7.56 13 -4 -6 1.94 2.62 13 4 -5 9.93 7.97 13 4 -4 10.93 6.72 13 4 -3 8.00 5.92 13 4 -2 -5.05 4.07 13 4 -1 4.95 5.89 13 4 0 -0.28 4.97 -13 -4 0 14.34 10.13 13 4 1 5.23 8.01 -13 -4 -1 12.40 9.39 13 4 2 12.68 6.57 -13 -4 -2 19.28 9.95 13 4 3 14.56 8.74 -13 -4 -3 6.17 6.33 13 4 4 -0.66 5.06 13 4 5 0.41 4.16 13 4 6 1.18 4.65 13 -5 -14 1.93 3.55 13 -5 -13 10.94 7.79 13 5 -12 16.20 9.62 13 -5 -12 2.01 1.87 13 -5 -11 4.81 6.35 13 5 -11 13.06 8.37 13 5 -10 19.09 10.06 13 -5 -10 5.47 5.04 13 -5 -9 -7.04 5.73 13 5 -9 -2.53 4.12 13 -5 -8 1.33 2.14 13 5 -8 0.27 7.63 13 -5 -7 4.32 3.91 13 5 -7 4.11 5.38 13 -5 -6 4.09 4.46 13 5 -6 7.36 6.72 13 5 -5 14.75 8.20 13 5 -4 11.42 7.84 13 5 -3 -1.24 2.05 13 5 -2 23.77 11.75 13 5 -1 6.24 6.65 13 5 0 6.09 6.09 -13 -5 0 -3.56 4.80 13 5 1 7.45 5.69 -13 -5 -1 -2.91 5.57 -13 -5 -2 -7.72 8.28 13 5 2 9.25 6.42 13 5 3 10.69 9.10 13 5 4 8.35 8.96 13 -6 -12 8.14 7.53 13 -6 -11 6.78 4.50 13 -6 -10 -6.46 5.95 13 -6 -9 3.50 6.22 13 -6 -8 18.03 9.12 13 6 -8 9.55 8.01 13 -6 -7 -9.17 6.55 13 6 -7 -0.06 2.98 13 6 -6 8.43 5.83 13 -6 -6 -5.37 1.96 13 6 -5 -0.15 4.43 13 6 -4 4.09 6.06 13 6 -3 11.41 8.92 13 6 -2 -4.46 5.15 13 6 -1 3.98 5.20 -13 -6 1 3.40 4.99 13 6 0 14.22 11.89 -13 -6 0 1.43 4.82 13 -7 -11 11.28 8.09 13 -7 -10 1.42 4.98 13 -7 -9 -3.11 5.80 13 -7 -8 -2.36 3.85 13 -7 -7 -3.80 4.52 13 -7 -6 1.85 4.56 13 -8 -8 -2.54 4.23 13 -8 -7 9.75 7.44 13 -8 -6 5.47 5.63 14 0 -16 11.91 9.67 14 0 -15 6.84 7.09 14 0 -14 5.10 5.25 14 0 -14 9.44 6.53 14 0 -13 -5.44 2.10 14 0 -13 6.03 6.11 14 0 -12 -4.50 6.58 14 0 -12 -3.23 4.09 14 0 -11 1.94 3.33 14 0 -10 3.98 3.10 14 0 -9 -5.99 5.52 14 0 -8 9.06 5.82 14 0 -7 3.22 5.12 14 0 -6 26.52 12.54 14 0 -5 11.61 8.59 14 0 -4 -3.78 5.73 14 0 -3 0.42 2.51 14 0 -2 -4.32 5.37 14 0 -1 2.13 5.01 14 0 0 7.60 6.45 14 0 1 8.30 7.40 14 0 2 3.88 8.06 14 0 3 5.06 7.75 14 0 4 15.99 12.30 14 0 5 -9.83 7.76 14 0 6 -0.03 2.69 14 1 -16 0.42 2.47 14 -1 -16 6.17 7.53 14 1 -15 4.09 7.04 14 -1 -15 3.41 5.18 14 1 -14 4.16 5.74 14 1 -14 -2.99 3.97 14 -1 -14 1.04 4.84 14 -1 -14 1.89 5.49 14 1 -13 4.93 5.83 14 1 -13 6.62 4.76 14 -1 -13 -5.44 5.45 14 -1 -13 10.07 7.10 14 1 -12 4.85 4.37 14 1 -12 4.15 5.27 14 -1 -12 3.18 3.12 14 -1 -12 2.53 2.67 14 1 -11 -5.62 5.21 14 -1 -11 -5.81 5.44 14 -1 -11 9.96 6.48 14 1 -10 -13.44 7.96 14 -1 -10 -4.46 3.34 14 1 -9 -2.79 4.86 14 -1 -9 2.30 5.19 14 1 -8 6.39 6.06 14 -1 -8 9.17 5.40 14 1 -7 9.14 6.81 14 -1 -7 2.43 4.67 14 1 -6 9.03 8.00 14 -1 -6 2.22 4.09 14 1 -5 -2.13 6.34 14 -1 -5 -7.22 9.12 14 1 -4 9.55 8.52 14 -1 -4 0.54 5.58 14 1 -3 4.20 3.49 14 -1 -3 6.59 5.00 14 1 -2 7.27 8.32 14 -1 -2 13.30 9.86 14 1 -1 -17.34 9.75 14 -1 -1 -2.98 4.12 14 1 0 1.39 2.07 14 -1 0 -5.03 7.46 14 1 1 -7.36 4.09 14 -1 1 4.31 3.13 14 1 2 -21.33 10.89 14 -1 2 2.55 4.68 14 1 3 -13.05 8.62 14 -1 3 4.32 6.03 14 1 4 5.59 6.92 14 -1 4 -13.01 9.24 14 -1 5 -0.03 3.02 14 1 5 -8.63 7.22 14 -1 6 -4.57 5.74 14 1 6 0.03 5.36 14 -2 -15 -5.60 5.75 14 -2 -14 -3.64 4.39 14 -2 -14 -10.68 7.51 14 2 -14 0.08 5.35 14 2 -13 12.03 8.61 14 -2 -13 3.18 1.99 14 2 -12 -6.99 5.52 14 -2 -12 -7.18 5.99 14 2 -11 -3.92 4.47 14 -2 -11 3.57 3.22 14 2 -10 11.79 7.53 14 -2 -10 7.44 4.05 14 2 -9 1.16 4.87 14 2 -8 1.95 3.87 14 2 -7 5.44 3.71 14 2 -6 -5.12 5.21 14 2 -5 10.22 8.66 14 2 -4 -10.13 7.13 14 2 -3 4.51 6.24 14 2 -2 3.30 3.07 14 2 -1 37.72 14.49 14 2 0 2.37 3.13 14 2 1 -9.68 7.44 14 2 2 -6.79 9.28 14 -2 2 -8.68 10.06 14 -2 3 10.49 7.11 14 2 3 3.55 5.36 -14 -2 -3 -2.48 4.44 14 -2 4 -13.29 9.75 14 2 4 -14.67 9.24 14 2 5 1.52 4.90 14 -2 5 -25.90 13.06 14 -2 6 8.44 10.04 14 -3 -15 8.25 8.90 14 3 -14 -2.46 3.74 14 -3 -14 -2.26 4.03 14 3 -13 -1.47 4.34 14 -3 -13 0.99 6.03 14 3 -12 0.42 3.85 14 -3 -12 3.48 4.28 14 3 -11 0.87 2.46 14 -3 -11 4.92 5.08 14 3 -10 11.08 6.80 14 -3 -10 8.17 5.79 14 3 -9 16.01 9.09 14 3 -8 14.45 8.09 14 3 -7 22.86 10.18 14 3 -6 0.11 3.20 14 3 -5 17.47 9.06 14 3 -4 -7.46 5.37 14 3 -3 -11.56 7.87 14 3 -2 2.49 4.72 14 3 -1 -9.62 7.41 14 3 0 -5.86 5.94 14 3 1 8.57 8.94 14 3 2 -2.04 3.99 -14 -3 -2 2.55 6.57 14 3 3 1.54 3.78 14 3 4 20.59 11.70 14 -4 -14 6.47 5.55 14 4 -14 0.13 2.27 14 4 -13 8.15 6.65 14 -4 -13 -4.15 4.95 14 4 -12 18.63 9.13 14 -4 -12 -4.40 5.03 14 -4 -11 3.67 2.81 14 4 -11 15.82 8.36 14 -4 -10 7.97 6.68 14 4 -10 0.17 5.96 14 4 -9 2.03 4.31 14 4 -8 1.28 4.01 14 4 -7 1.50 4.13 14 4 -6 3.79 3.17 14 4 -5 -4.73 5.16 14 4 -4 2.23 2.57 14 4 -3 -2.63 5.52 14 4 -2 1.32 2.92 14 4 -1 -2.56 4.06 14 4 0 6.13 6.86 14 4 1 8.93 8.76 14 4 2 4.67 4.23 14 5 -13 6.06 7.01 14 -5 -13 -1.43 3.39 14 -5 -12 4.72 5.29 14 5 -12 16.77 10.13 14 5 -11 15.24 9.84 14 -5 -11 6.50 5.23 14 -5 -10 -6.59 5.92 14 5 -10 14.54 8.87 14 -5 -9 17.74 9.46 14 5 -9 19.21 10.31 14 5 -8 4.50 7.00 14 5 -7 7.52 5.07 14 5 -6 -1.74 3.13 14 5 -5 7.23 9.69 14 5 -4 13.25 11.08 14 5 -3 1.48 6.31 14 5 -2 25.33 13.49 14 -6 -11 7.77 5.22 14 -6 -10 10.73 7.93 14 -6 -9 7.27 6.19 14 -7 -9 21.99 12.52 15 0 -14 4.91 5.11 15 0 -13 0.02 4.91 15 0 -12 0.87 3.37 15 0 -11 22.07 11.32 15 0 -10 -1.55 3.43 15 0 -9 1.67 4.34 15 0 -8 4.42 6.28 15 0 -7 7.70 6.93 15 0 -6 12.05 10.17 15 0 -5 -4.94 5.89 15 0 -4 7.74 7.92 15 0 -3 -6.13 8.22 15 0 -2 -8.93 7.84 15 0 -1 -10.01 8.23 15 0 0 -13.19 9.38 15 0 1 4.35 5.23 15 1 -14 1.85 5.03 15 -1 -14 -1.74 3.48 15 1 -13 6.37 5.84 15 -1 -13 12.49 8.04 15 1 -12 6.05 5.31 15 -1 -12 0.21 2.07 15 1 -11 0.60 2.65 15 -1 -11 1.50 3.50 15 1 -10 -4.25 3.25 15 -1 -10 -0.75 4.70 15 1 -9 -2.53 3.97 15 -1 -9 6.61 9.50 15 1 -8 -15.96 9.25 15 -1 -8 -0.83 5.74 15 1 -7 0.89 4.17 15 -1 -7 1.87 3.02 15 1 -6 2.88 5.87 15 -1 -6 6.42 4.18 15 1 -5 7.17 4.01 15 -1 -5 2.19 6.86 15 1 -4 -9.04 8.41 15 -1 -4 9.65 6.92 15 1 -3 9.54 9.15 15 -1 -3 -10.14 8.62 15 1 -2 0.43 6.56 15 -1 -2 2.51 6.18 15 1 -1 5.10 5.65 15 -1 -1 -11.42 9.25 15 1 0 1.82 4.07 15 -1 0 5.91 9.90 15 -2 -14 0.84 2.82 15 2 -14 2.96 3.84 15 -2 -13 0.02 3.96 15 2 -13 -9.32 6.94 15 -2 -12 -11.76 8.04 15 2 -12 12.58 7.27 15 2 -11 2.12 3.51 15 2 -10 0.25 4.26 15 2 -9 0.32 2.37 15 2 -8 10.22 6.87 15 2 -7 28.27 12.41 15 2 -6 10.70 7.18 15 2 -5 -5.38 2.53 15 2 -4 11.52 7.71 15 2 -3 13.33 7.14 15 2 -2 -12.56 8.57 15 2 -1 0.05 6.80 15 -2 -1 1.61 4.46 15 3 -14 -5.15 5.34 15 3 -13 2.19 5.80 15 3 -12 6.67 7.11 15 3 -11 2.33 3.88 15 3 -10 -4.87 6.74 15 3 -9 26.24 12.35 15 3 -8 11.25 7.54 15 3 -7 16.96 9.91 15 3 -6 1.37 4.63 15 3 -5 1.41 3.67 15 3 -4 -10.71 8.50 15 3 -3 11.05 7.06 15 4 -10 1.82 6.93 15 4 -9 13.08 8.26 15 4 -8 10.11 6.27 0 0 0 0.00 0.00 TITL exp_4814 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 12.528557 9.981055 16.313378 90.0000 107.1320 90.0000 ZERR 4.00 0.000895 0.000617 0.001381 0.0000 0.0083 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 92.00 64.00 16.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 59909 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 O22 O 0.21772(19) 0.3329(2) 0.40934(16) 0.0719(8) Uani 1 1 d . . N3 N 0.3797(2) 0.4133(3) 0.39668(15) 0.0486(7) Uani 1 1 d . . H20 H 0.4240 0.4809 0.4033 0.058 Uiso 1 1 calc R U N2 N 0.4694(2) 0.5660(3) 0.14341(17) 0.0563(8) Uani 1 1 d . . N1 N 0.3752(2) 0.5994(3) 0.16365(17) 0.0618(8) Uani 1 1 d . . H7 H 0.3367 0.6702 0.1448 0.074 Uiso 1 1 calc R U C9 C 0.4285(2) 0.4112(3) 0.23252(19) 0.0438(8) Uani 1 1 d . . C12 C 0.6031(2) 0.3852(3) 0.17655(19) 0.0465(8) Uani 1 1 d . . C23 C 0.2572(2) 0.5566(3) 0.45284(19) 0.0467(8) Uani 1 1 d . . C6 C 0.4103(2) 0.2906(3) 0.3635(2) 0.0452(8) Uani 1 1 d . . C10 C 0.5017(2) 0.4509(3) 0.18579(19) 0.0475(8) Uani 1 1 d . . C1 C 0.4322(2) 0.2898(3) 0.2843(2) 0.0451(8) Uani 1 1 d . . C21 C 0.2839(3) 0.4261(3) 0.41782(19) 0.0488(8) Uani 1 1 d . . C13 C 0.6188(3) 0.3770(3) 0.0963(2) 0.0523(9) Uani 1 1 d . . H13 H 0.5659 0.4141 0.0493 0.063 Uiso 1 1 calc R U C15 C 0.7903(3) 0.2598(3) 0.1546(2) 0.0546(9) Uani 1 1 d . . C8 C 0.3482(3) 0.5106(3) 0.2160(2) 0.0558(9) Uani 1 1 d . . H8 H 0.2871 0.5151 0.2372 0.067 Uiso 1 1 calc R U N19 N 0.9569(3) 0.1403(4) 0.1230(2) 0.0851(11) Uani 1 1 d . . C2 C 0.4595(3) 0.1667(3) 0.2542(2) 0.0580(9) Uani 1 1 d . . H2 H 0.4731 0.1633 0.2012 0.070 Uiso 1 1 calc R U C14 C 0.7113(3) 0.3150(3) 0.0846(2) 0.0579(9) Uani 1 1 d . . H14 H 0.7207 0.3102 0.0303 0.070 Uiso 1 1 calc R U C17 C 0.6842(3) 0.3315(4) 0.2466(2) 0.0613(10) Uani 1 1 d . . H17 H 0.6759 0.3384 0.3013 0.074 Uiso 1 1 calc R U C5 C 0.4179(3) 0.1736(4) 0.4103(2) 0.0574(9) Uani 1 1 d . . H5 H 0.4034 0.1756 0.4630 0.069 Uiso 1 1 calc R U C16 C 0.7770(3) 0.2679(4) 0.2353(2) 0.0623(10) Uani 1 1 d . . H16 H 0.8303 0.2307 0.2820 0.075 Uiso 1 1 calc R U C3 C 0.4667(3) 0.0503(3) 0.3013(2) 0.0623(10) Uani 1 1 d . . H3 H 0.4849 -0.0303 0.2800 0.075 Uiso 1 1 calc R U C4 C 0.4468(3) 0.0541(4) 0.3801(2) 0.0642(10) Uani 1 1 d . . H4 H 0.4528 -0.0235 0.4127 0.077 Uiso 1 1 calc R U C18 C 0.8849(3) 0.1927(4) 0.1397(2) 0.0635(10) Uani 1 1 d . . C28 C 0.1673(3) 0.5571(4) 0.4851(2) 0.0711(11) Uani 1 1 d . . H28 H 0.1277 0.4781 0.4848 0.085 Uiso 1 1 calc R U C26 C 0.1915(3) 0.7872(4) 0.5173(3) 0.0787(12) Uani 1 1 d . . H26 H 0.1696 0.8656 0.5385 0.094 Uiso 1 1 calc R U C27 C 0.1347(3) 0.6725(4) 0.5178(3) 0.0815(12) Uani 1 1 d . . H27 H 0.0743 0.6712 0.5399 0.098 Uiso 1 1 calc R U C24 C 0.3144(3) 0.6735(4) 0.4536(3) 0.0843(13) Uani 1 1 d . . H24 H 0.3757 0.6758 0.4325 0.101 Uiso 1 1 calc R U C25 C 0.2798(4) 0.7886(4) 0.4862(3) 0.1017(17) Uani 1 1 d . . H25 H 0.3184 0.8683 0.4866 0.122 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 O22 0.0760(16) 0.0527(15) 0.105(2) -0.0230(15) 0.0541(14) -0.0278(13) N3 0.0526(16) 0.0421(16) 0.0556(17) -0.0054(14) 0.0229(13) -0.0110(13) N2 0.0592(17) 0.0561(19) 0.0613(18) 0.0115(15) 0.0295(14) 0.0158(15) N1 0.0613(18) 0.060(2) 0.069(2) 0.0203(17) 0.0269(15) 0.0261(15) C9 0.0431(17) 0.0461(19) 0.0452(18) 0.0017(16) 0.0179(14) 0.0057(16) C12 0.0521(19) 0.0425(19) 0.050(2) 0.0059(16) 0.0233(16) 0.0092(15) C23 0.0490(18) 0.044(2) 0.0489(19) -0.0040(16) 0.0179(15) -0.0064(16) C6 0.0469(19) 0.0403(19) 0.050(2) 0.0016(16) 0.0162(15) 0.0003(15) C10 0.0518(19) 0.046(2) 0.0477(19) 0.0074(17) 0.0192(15) 0.0131(16) C1 0.0448(18) 0.045(2) 0.0480(19) 0.0018(17) 0.0177(15) 0.0056(15) C21 0.0503(19) 0.050(2) 0.052(2) -0.0019(17) 0.0237(15) -0.0075(17) C13 0.055(2) 0.053(2) 0.054(2) 0.0143(18) 0.0233(16) 0.0128(17) C15 0.051(2) 0.059(2) 0.061(2) 0.0058(19) 0.0283(17) 0.0162(17) C8 0.056(2) 0.061(2) 0.055(2) 0.0103(19) 0.0232(16) 0.0103(18) N19 0.078(2) 0.114(3) 0.075(2) 0.016(2) 0.0410(18) 0.042(2) C2 0.065(2) 0.053(2) 0.062(2) 0.0031(19) 0.0280(17) 0.0097(18) C14 0.064(2) 0.066(2) 0.052(2) 0.0066(19) 0.0289(17) 0.0151(19) C17 0.061(2) 0.080(3) 0.048(2) 0.009(2) 0.0231(17) 0.022(2) C5 0.065(2) 0.057(2) 0.054(2) 0.007(2) 0.0241(17) -0.0005(19) C16 0.056(2) 0.078(3) 0.055(2) 0.010(2) 0.0213(17) 0.0241(19) C3 0.067(2) 0.040(2) 0.081(3) 0.003(2) 0.0230(19) 0.0076(18) C4 0.071(2) 0.051(2) 0.073(3) 0.015(2) 0.0245(19) 0.0067(19) C18 0.065(2) 0.071(3) 0.062(2) 0.013(2) 0.0303(18) 0.016(2) C28 0.077(3) 0.059(2) 0.094(3) -0.008(2) 0.051(2) -0.005(2) C26 0.075(3) 0.059(3) 0.101(3) -0.017(2) 0.026(2) 0.011(2) C27 0.083(3) 0.076(3) 0.101(3) -0.006(3) 0.052(2) 0.012(3) C24 0.072(3) 0.056(3) 0.144(4) -0.020(3) 0.060(3) -0.015(2) C25 0.089(3) 0.050(3) 0.178(5) -0.029(3) 0.058(3) -0.013(2) 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 C21 N3 C6 122.3(3) C21 N3 H20 118.9 C6 N3 H20 118.9 C10 N2 N1 103.8(3) C8 N1 N2 113.1(3) C8 N1 H7 123.4 N2 N1 H7 123.4 C8 C9 C10 104.2(3) C8 C9 C1 127.0(3) C10 C9 C1 128.7(3) C13 C12 C17 118.8(3) C13 C12 C10 119.3(3) C17 C12 C10 121.9(3) C24 C23 C28 118.6(3) C24 C23 C21 124.8(3) C28 C23 C21 116.6(3) C5 C6 C1 120.3(3) C5 C6 N3 119.7(3) C1 C6 N3 120.0(3) N2 C10 C9 111.9(3) N2 C10 C12 117.8(3) C9 C10 C12 130.3(3) C6 C1 C2 117.6(3) C6 C1 C9 123.0(3) C2 C1 C9 119.5(3) O22 C21 N3 121.4(3) O22 C21 C23 118.9(3) N3 C21 C23 119.7(3) C14 C13 C12 121.2(3) C14 C13 H13 119.4 C12 C13 H13 119.4 C16 C15 C14 120.3(3) C16 C15 C18 121.7(3) C14 C15 C18 118.0(3) N1 C8 C9 107.0(3) N1 C8 H8 126.5 C9 C8 H8 126.5 C3 C2 C1 121.7(3) C3 C2 H2 119.1 C1 C2 H2 119.1 C13 C14 C15 119.5(3) C13 C14 H14 120.3 C15 C14 H14 120.3 C16 C17 C12 120.3(3) C16 C17 H17 119.8 C12 C17 H17 119.8 C4 C5 C6 121.1(3) C4 C5 H5 119.4 C6 C5 H5 119.4 C15 C16 C17 119.9(3) C15 C16 H16 120.1 C17 C16 H16 120.1 C4 C3 C2 119.6(3) C4 C3 H3 120.2 C2 C3 H3 120.2 C5 C4 C3 119.7(3) C5 C4 H4 120.2 C3 C4 H4 120.2 N19 C18 C15 176.1(4) C23 C28 C27 121.2(4) C23 C28 H28 119.4 C27 C28 H28 119.4 C25 C26 C27 120.3(4) C25 C26 H26 119.8 C27 C26 H26 119.8 C26 C27 C28 119.3(4) C26 C27 H27 120.4 C28 C27 H27 120.4 C23 C24 C25 119.2(4) C23 C24 H24 120.4 C25 C24 H24 120.4 C26 C25 C24 121.3(4) C26 C25 H25 119.3 C24 C25 H25 119.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O22 C21 1.227(3) N3 C21 1.349(4) N3 C6 1.435(4) N3 H20 0.8600 N2 C10 1.341(4) N2 N1 1.357(3) N1 C8 1.342(4) N1 H7 0.8600 C9 C8 1.381(4) C9 C10 1.412(4) C9 C1 1.470(4) C12 C13 1.383(4) C12 C17 1.394(4) C12 C10 1.475(4) C23 C24 1.367(4) C23 C28 1.376(4) C23 C21 1.499(4) C6 C5 1.383(4) C6 C1 1.398(4) C1 C2 1.402(4) C13 C14 1.375(4) C13 H13 0.9300 C15 C16 1.377(4) C15 C14 1.386(4) C15 C18 1.443(4) C8 H8 0.9300 N19 C18 1.142(4) C2 C3 1.381(4) C2 H2 0.9300 C14 H14 0.9300 C17 C16 1.385(4) C17 H17 0.9300 C5 C4 1.379(4) C5 H5 0.9300 C16 H16 0.9300 C3 C4 1.381(4) C3 H3 0.9300 C4 H4 0.9300 C28 C27 1.381(5) C28 H28 0.9300 C26 C25 1.345(5) C26 C27 1.349(5) C26 H26 0.9300 C27 H27 0.9300 C24 C25 1.388(5) C24 H24 0.9300 C25 H25 0.9300