#------------------------------------------------------------------------------ #$Date: 2018-05-17 21:11:21 +0100 (Thu, 17 May 2018) $ #$Revision: 207832 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500075.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_3500075 loop_ _publ_author_name 'Miguel N. Moreno-Carretero' _journal_name_full 'Personal communication to COD' _journal_year 2018 _chemical_formula_sum 'C7 H9 N3 O3' _chemical_formula_weight 183.17 _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/4 _cell_angle_alpha 90 _cell_angle_beta 107.713(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9021(9) _cell_length_b 9.6475(10) _cell_length_c 9.5670(9) _cell_measurement_temperature 100(2) _cell_volume 782.69(14) _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.0346 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 19530 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.630 _diffrn_reflns_theta_min 2.738 _exptl_absorpt_coefficient_mu 0.124 _exptl_crystal_density_diffrn 1.554 _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.160 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.270 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 132 _refine_ls_number_reflns 1813 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0456 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.3783P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.1170 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1363 _reflns_number_total 1813 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file mo_fh_180514_3136_0m.cif _cod_data_source_block shelx _cod_database_code 3500075 _shelx_shelxl_version_number 2016/4 _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 0.974 _shelx_estimated_absorpt_t_max 0.980 _shelx_res_file ; TITL SIR92 run in space group P 21/n shelx.res created by SHELXL-2016/4 at 13:25:50 on 15-May-2018 CELL 0.71073 8.9021 9.6475 9.5670 90.000 107.713 90.000 ZERR 4.00 0.0009 0.0010 0.0009 0.000 0.004 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 36 12 12 MERG 2 SIZE 0.160 0.190 0.210 ACTA BOND $H CONF L.S. 10 TEMP -173.10 WGHT 0.058600 0.378300 FVAR 0.91248 O2 4 0.653304 0.290989 -0.066700 11.00000 0.01939 0.01697 = 0.01832 0.00203 0.01219 -0.00094 N1 3 0.484586 0.236677 0.062873 11.00000 0.00896 0.00840 = 0.01151 0.00010 0.00362 0.00048 O51 4 0.368180 -0.055224 0.348366 11.00000 0.02029 0.01853 = 0.02246 0.00121 0.01137 -0.00428 N3 3 0.715604 0.106661 0.088555 11.00000 0.00835 0.01449 = 0.01413 -0.00177 0.00568 0.00112 O4 4 0.765289 -0.089708 0.224605 11.00000 0.01538 0.01389 = 0.01918 0.00163 0.00286 0.00529 N6 3 0.320610 0.190639 0.203166 11.00000 0.01404 0.01281 = 0.01879 0.00143 0.00959 0.00150 C5 1 0.536088 0.037257 0.220103 11.00000 0.01111 0.01025 = 0.00997 -0.00217 0.00243 -0.00167 C6 1 0.445493 0.155871 0.163668 11.00000 0.00915 0.01050 = 0.01064 -0.00329 0.00345 -0.00319 C4 1 0.677629 0.009822 0.181498 11.00000 0.01101 0.00935 = 0.01025 -0.00311 0.00030 -0.00088 C51 1 0.489758 -0.059990 0.310975 11.00000 0.01628 0.01413 = 0.01586 0.00025 0.00422 -0.00156 C1 1 0.381928 0.352316 -0.005270 11.00000 0.01613 0.01336 = 0.02028 0.00557 0.00806 0.00451 AFIX 137 H1A 2 0.273353 0.318957 -0.045972 11.00000 -1.50000 H1B 2 0.417664 0.391687 -0.084110 11.00000 -1.50000 H1C 2 0.386032 0.423733 0.068647 11.00000 -1.50000 AFIX 0 C3 1 0.861300 0.082790 0.050701 11.00000 0.01292 0.01904 = 0.02527 -0.00294 0.01161 0.00252 AFIX 137 H3A 2 0.867139 0.148530 -0.025565 11.00000 -1.50000 H3B 2 0.861682 -0.012117 0.014294 11.00000 -1.50000 H3C 2 0.952406 0.096010 0.138088 11.00000 -1.50000 AFIX 0 C2 1 0.621693 0.216777 0.022824 11.00000 0.01109 0.01108 = 0.01125 -0.00402 0.00517 -0.00173 H51 2 0.562498 -0.137016 0.340285 11.00000 0.01822 H62 2 0.263699 0.268871 0.175454 11.00000 0.02417 H61 2 0.294095 0.135911 0.270409 11.00000 0.02981 HKLF 4 REM SIR92 run in space group P 21/n REM R1 = 0.0456 for 1363 Fo > 4sig(Fo) and 0.0701 for all 1813 data REM 132 parameters refined using 0 restraints END WGHT 0.0575 0.3953 REM Highest difference peak 0.270, deepest hole -0.291, 1-sigma level 0.065 Q1 1 0.8260 0.0733 -0.0728 11.00000 0.05 0.27 Q2 1 0.5915 0.0187 0.1945 11.00000 0.05 0.26 Q3 1 0.5163 0.1013 0.2226 11.00000 0.05 0.23 Q4 1 0.5266 0.2105 0.0246 11.00000 0.05 0.22 Q5 1 0.5175 -0.0028 0.2624 11.00000 0.05 0.22 Q6 1 0.9078 0.1649 0.0592 11.00000 0.05 0.21 Q7 1 0.7724 0.0869 0.0574 11.00000 0.05 0.21 Q8 1 0.2770 -0.0275 0.2629 11.00000 0.05 0.19 Q9 1 0.4981 0.2065 0.1361 11.00000 0.05 0.19 Q10 1 0.3203 0.0434 0.3564 11.00000 0.05 0.19 Q11 1 0.4338 0.2871 0.0223 11.00000 0.05 0.18 Q12 1 0.4822 -0.0748 0.5379 11.00000 0.05 0.18 Q13 1 0.6043 0.3578 -0.1348 11.00000 0.05 0.18 Q14 1 0.4175 0.4340 -0.0350 11.00000 0.05 0.18 Q15 1 0.1976 0.0410 0.1923 11.00000 0.05 0.17 Q16 1 1.0530 0.2381 0.0136 11.00000 0.05 0.17 Q17 1 0.7027 0.0669 0.1373 11.00000 0.05 0.17 Q18 1 0.9392 0.0184 0.1143 11.00000 0.05 0.16 Q19 1 0.7180 0.4192 -0.0965 11.00000 0.05 0.16 Q20 1 0.4290 0.0560 0.0021 11.00000 0.05 0.16 ; _shelx_res_checksum 97171 _shelx_hkl_file ; -1 0 0 -0.30 0.80 1 0 0 -1.60 0.80 1 0 0 -0.30 0.90 -1 0 0 0.50 1.10 2 0 0 226.68 9.20 2 0 0 229.08 8.90 -2 0 0 229.88 8.90 -2 0 0 200.78 8.90 3 0 0 -2.20 2.80 -3 0 0 0.80 2.00 3 0 0 -1.10 2.30 -3 0 0 -0.90 2.40 4 0 0 74.39 7.30 -4 0 0 92.39 8.60 -4 0 0 83.39 8.40 4 0 0 84.89 8.20 -4 0 0 88.99 8.50 -5 0 0 6.10 5.10 -5 0 0 0.90 4.00 -5 0 0 1.50 7.00 -5 0 0 2.00 4.80 5 0 0 3.80 5.40 5 0 0 3.90 4.50 5 0 0 -5.70 4.10 -6 0 0 667.53 29.70 6 0 0 614.14 25.40 6 0 0 644.34 29.00 -6 0 0 636.14 26.60 6 0 0 654.33 24.00 -6 0 0 619.64 27.40 7 0 0 -1.00 6.80 7 0 0 8.70 7.30 -7 0 0 4.00 7.40 -7 0 0 -5.50 7.30 -7 0 0 -11.50 9.40 8 0 0 287.77 20.30 8 0 0 297.37 20.70 -8 0 0 263.97 21.90 -8 0 0 282.47 21.60 -8 0 0 288.37 24.80 -9 0 0 -13.80 11.50 9 0 0 -12.30 11.00 -9 0 0 -28.20 16.50 9 0 0 18.40 17.50 -9 0 0 8.00 11.60 -9 0 0 -17.40 19.00 -10 0 0 -1.30 15.00 -10 0 0 0.80 16.20 10 0 0 18.10 16.90 10 0 0 43.50 16.50 -11 0 0 18.40 20.70 -11 0 0 8.00 20.30 11 0 0 26.60 19.80 1 -1 0 2317.37 57.39 -1 -1 0 2437.36 55.59 1 -1 0 2483.55 55.99 1 -1 0 2058.69 57.29 1 -1 0 2446.86 55.59 1 1 0 2375.26 54.39 1 1 0 2478.85 55.99 1 1 0 2251.07 56.89 -1 1 0 2433.96 55.69 -1 1 0 2420.66 55.89 1 1 0 2405.16 55.69 2 -1 0 -0.50 1.80 -2 -1 0 2.20 2.00 2 -1 0 0.00 2.00 2 -1 0 1.30 2.00 2 -1 0 -2.60 2.00 -2 -1 0 -1.10 1.90 -2 -1 0 0.20 1.90 2 1 0 1.40 2.00 -2 1 0 0.00 1.90 -2 1 0 -1.20 1.80 -2 1 0 1.60 2.00 2 1 0 0.40 1.70 -2 1 0 2.60 2.20 2 1 0 -3.50 1.80 -3 -1 0 128.09 8.20 -3 -1 0 125.19 8.00 3 -1 0 133.39 8.60 -3 -1 0 110.29 8.00 3 -1 0 131.99 8.00 3 -1 0 121.59 7.50 -3 1 0 114.89 8.00 3 1 0 118.29 7.70 -3 1 0 121.09 8.00 -3 1 0 129.49 9.10 3 1 0 136.29 8.60 4 -1 0 422.96 16.90 -4 -1 0 393.26 16.90 4 -1 0 418.26 18.00 -4 -1 0 409.66 17.10 4 -1 0 399.06 16.00 -4 -1 0 375.56 17.30 -4 1 0 416.36 18.90 -4 1 0 409.26 17.50 -4 1 0 403.66 17.30 4 1 0 385.06 16.40 4 1 0 398.26 17.50 5 -1 0 596.54 22.00 5 -1 0 572.74 22.60 -5 -1 0 608.84 24.00 -5 -1 0 592.84 24.50 -5 -1 0 558.34 23.30 5 -1 0 585.74 24.40 -5 1 0 608.34 26.10 5 1 0 600.84 24.50 5 1 0 593.34 22.80 -5 1 0 586.54 24.40 -5 1 0 633.04 24.40 -6 -1 0 135.89 12.80 6 -1 0 117.69 11.40 6 -1 0 172.98 15.40 6 -1 0 141.79 12.40 -6 -1 0 130.79 14.20 -6 -1 0 123.79 12.90 -6 1 0 150.78 16.40 -6 1 0 122.99 12.20 6 1 0 146.89 15.00 -6 1 0 128.89 14.20 6 1 0 125.99 12.40 -7 -1 0 -0.50 9.50 7 -1 0 -1.70 7.50 7 -1 0 5.90 7.10 -7 -1 0 -5.80 7.30 -7 -1 0 -1.40 7.40 -7 1 0 8.30 9.70 7 1 0 -1.30 7.00 7 1 0 -1.60 6.60 -7 1 0 -6.60 7.10 -8 -1 0 22.30 11.50 8 -1 0 50.79 12.10 -8 -1 0 35.70 12.20 8 -1 0 5.50 22.20 8 -1 0 19.50 10.10 -8 -1 0 43.40 15.30 8 1 0 50.09 12.30 -8 1 0 49.90 15.30 8 1 0 29.50 9.90 -8 1 0 23.80 10.80 8 1 0 49.80 12.90 -8 1 0 66.49 13.80 -8 1 0 43.60 17.10 9 -1 0 14.30 14.00 -9 -1 0 72.19 20.40 -9 -1 0 10.90 13.60 9 -1 0 33.60 13.40 -9 -1 0 44.10 15.40 9 -1 0 25.70 17.80 -9 -1 0 26.50 20.10 -9 1 0 27.30 13.90 -9 1 0 1.20 18.80 9 1 0 24.10 12.10 9 1 0 62.29 18.30 -9 1 0 8.90 13.70 9 1 0 40.00 13.00 -9 1 0 -29.40 18.20 -10 -1 0 77.09 19.80 10 -1 0 16.10 15.70 -10 -1 0 103.29 21.80 10 1 0 75.49 17.30 10 1 0 64.89 17.50 -10 1 0 35.60 17.90 -10 1 0 67.69 19.00 -11 -1 0 43.20 22.40 -11 -1 0 2.40 21.60 11 -1 0 -4.20 20.10 -11 1 0 5.70 21.10 -11 1 0 23.00 22.60 11 1 0 35.00 20.50 0 -2 0 15.50 2.70 0 -2 0 18.10 2.70 0 -2 0 13.40 3.00 0 -2 0 7.90 2.50 0 2 0 12.80 2.20 0 2 0 12.20 3.00 0 2 0 17.10 2.70 0 2 0 17.10 2.90 0 2 0 13.20 2.70 1 -2 0 251.07 9.80 -1 -2 0 243.98 10.30 -1 -2 0 254.37 8.90 -1 -2 0 250.07 9.50 1 -2 0 233.78 9.30 -1 -2 0 241.48 10.00 -1 -2 0 245.88 8.10 1 -2 0 271.67 10.10 -1 2 0 247.78 9.40 1 2 0 250.77 10.20 1 2 0 246.98 8.80 1 2 0 262.47 9.70 1 2 0 245.48 7.90 -1 2 0 257.17 9.50 -1 2 0 248.28 10.00 -1 2 0 252.87 9.90 2 -2 0 38.90 4.60 2 -2 0 41.80 5.00 2 -2 0 33.60 4.50 2 -2 0 31.50 4.50 -2 -2 0 35.10 4.80 -2 -2 0 30.20 4.70 -2 2 0 40.20 4.40 2 2 0 36.40 4.90 2 2 0 41.40 4.60 -2 2 0 33.40 4.40 2 2 0 39.40 4.90 -2 2 0 40.80 5.10 2 2 0 39.50 3.80 -2 2 0 41.70 5.10 3 -2 0 780.52 24.80 -3 -2 0 771.02 24.70 3 -2 0 756.42 25.80 -3 -2 0 793.42 25.40 -3 -2 0 743.33 25.10 3 -2 0 743.23 24.70 3 -2 0 763.02 24.70 3 2 0 810.82 25.40 3 2 0 803.82 25.20 -3 2 0 742.23 24.50 3 2 0 766.72 24.40 -3 2 0 808.72 26.20 -3 2 0 804.22 25.20 -3 2 0 782.62 25.20 4 -2 0 95.09 8.50 4 -2 0 96.79 9.30 -4 -2 0 79.69 8.50 4 -2 0 78.79 8.00 -4 -2 0 85.19 9.10 -4 -2 0 93.99 9.00 4 2 0 82.79 8.20 -4 2 0 86.89 8.70 -4 2 0 86.79 9.30 4 2 0 84.39 8.50 -4 2 0 76.99 9.80 4 2 0 85.59 9.10 5 -2 0 334.27 16.90 -5 -2 0 351.76 18.30 -5 -2 0 337.97 17.80 -5 -2 0 344.97 18.70 5 -2 0 327.57 18.00 5 -2 0 368.46 17.60 -5 2 0 323.67 17.60 -5 2 0 341.87 20.00 -5 2 0 378.76 18.80 5 2 0 365.46 18.80 5 2 0 354.36 17.30 6 -2 0 22.90 7.40 6 -2 0 46.00 9.00 6 -2 0 32.10 9.90 -6 -2 0 28.30 8.40 -6 -2 0 38.40 9.00 -6 -2 0 21.50 8.70 6 2 0 17.00 9.00 -6 2 0 29.50 9.40 6 2 0 25.60 7.50 -6 2 0 27.80 7.70 -6 2 0 28.20 10.90 7 -2 0 129.79 15.00 -7 -2 0 136.29 15.30 -7 -2 0 157.68 17.00 7 -2 0 136.09 14.10 -7 2 0 130.19 14.90 7 2 0 122.59 14.70 -7 2 0 112.49 17.70 -7 2 0 157.38 18.00 -8 -2 0 -2.50 13.50 8 -2 0 9.70 11.10 -8 -2 0 -0.50 10.70 -8 -2 0 0.70 10.20 -8 -2 0 -0.80 12.70 8 -2 0 4.90 9.50 8 -2 0 13.40 11.30 -8 2 0 -3.70 9.80 -8 2 0 -33.70 13.70 -8 2 0 23.90 13.90 8 2 0 -0.10 8.10 8 2 0 -9.10 12.70 8 2 0 0.50 8.50 9 -2 0 32.10 14.20 -9 -2 0 39.10 21.20 -9 -2 0 48.30 18.50 -9 -2 0 38.70 14.80 9 -2 0 61.59 18.90 9 -2 0 56.69 17.80 -9 -2 0 62.49 16.60 -9 2 0 42.40 15.50 -9 2 0 53.49 19.00 9 2 0 31.30 12.10 9 2 0 56.59 19.20 -9 2 0 41.70 19.10 9 2 0 37.30 13.30 -9 2 0 31.80 14.00 -10 -2 0 7.10 16.40 10 -2 0 7.80 20.40 10 -2 0 7.70 15.20 -10 -2 0 31.80 19.00 10 2 0 6.60 14.50 -10 2 0 4.20 17.10 10 2 0 24.00 15.20 -10 2 0 12.10 17.00 0 -3 0 3.10 2.50 0 -3 0 0.20 1.80 0 -3 0 0.90 2.30 0 -3 0 3.00 2.90 0 -3 0 1.30 2.20 0 3 0 1.30 2.10 0 3 0 -1.70 2.60 0 3 0 -1.70 2.00 0 3 0 2.50 2.10 0 3 0 0.90 3.10 -1 -3 0 253.97 12.20 1 -3 0 252.17 10.60 -1 -3 0 244.18 11.60 -1 -3 0 260.07 11.10 1 -3 0 245.38 11.30 1 -3 0 248.08 10.40 1 -3 0 259.07 11.40 -1 -3 0 251.07 10.30 1 3 0 263.57 11.70 1 3 0 260.47 11.60 -1 3 0 243.38 11.30 -1 3 0 247.08 10.30 1 3 0 247.18 8.90 1 3 0 246.48 10.80 -1 3 0 261.27 11.50 1 3 0 223.18 9.90 -1 3 0 270.77 12.90 2 -3 0 12.30 3.70 -2 -3 0 14.40 3.80 2 -3 0 18.40 4.00 2 -3 0 19.30 4.70 -2 -3 0 19.60 3.30 -2 -3 0 25.10 4.10 -2 -3 0 18.90 4.50 2 3 0 22.30 4.60 2 3 0 13.40 4.10 -2 3 0 17.40 3.90 2 3 0 23.50 4.20 -2 3 0 17.60 3.90 -2 3 0 21.70 4.20 -2 3 0 23.30 4.80 2 3 0 19.30 3.20 3 -3 0 180.98 11.20 -3 -3 0 190.68 11.20 3 -3 0 182.28 11.20 -3 -3 0 170.08 8.80 3 -3 0 177.28 10.80 -3 -3 0 183.88 11.60 3 -3 0 172.18 10.60 -3 3 0 180.68 11.50 3 3 0 166.88 8.50 3 3 0 177.88 11.40 3 3 0 177.98 11.20 -3 3 0 166.98 10.80 -3 3 0 175.78 11.10 3 3 0 168.38 10.20 -3 3 0 173.68 10.70 4 -3 0 62.09 8.40 4 -3 0 54.79 8.50 -4 -3 0 65.69 8.70 4 -3 0 55.49 8.40 4 -3 0 55.79 9.00 -4 -3 0 44.00 8.20 -4 -3 0 57.59 8.70 -4 3 0 58.39 8.10 -4 3 0 60.19 8.20 4 3 0 66.69 8.90 4 3 0 59.99 7.90 -4 3 0 76.89 10.00 4 3 0 45.20 5.80 -4 3 0 58.99 8.80 4 3 0 45.20 7.40 -5 -3 0 24.00 7.40 5 -3 0 12.40 6.80 -5 -3 0 12.50 6.40 -5 -3 0 19.60 7.10 5 -3 0 18.20 7.60 5 -3 0 29.20 7.60 -5 3 0 27.10 8.70 5 3 0 24.60 8.00 5 3 0 31.70 7.00 -5 3 0 22.00 7.10 5 3 0 12.60 4.90 -5 3 0 18.00 7.70 5 3 0 20.90 7.70 -6 -3 0 945.51 37.00 6 -3 0 943.91 36.50 -6 -3 0 943.91 36.20 -6 -3 0 1030.40 37.30 6 -3 0 951.00 35.00 6 -3 0 969.00 35.30 -6 3 0 962.20 38.70 -6 3 0 941.61 35.90 6 3 0 990.20 37.00 -6 3 0 940.31 36.70 6 3 0 984.00 35.30 7 -3 0 201.18 20.00 7 -3 0 224.08 17.30 7 -3 0 244.88 19.40 -7 -3 0 238.58 20.00 -7 -3 0 218.98 18.60 -7 3 0 288.17 22.40 7 3 0 255.57 18.70 -7 3 0 232.98 17.60 -7 3 0 270.27 23.80 8 -3 0 20.00 11.70 -8 -3 0 30.50 12.80 -8 -3 0 10.20 10.40 -8 -3 0 17.20 14.80 8 -3 0 -0.50 13.90 8 -3 0 4.30 12.10 -8 3 0 58.39 16.00 -8 3 0 4.80 10.10 8 3 0 10.90 14.40 -8 3 0 36.60 17.00 8 3 0 14.00 9.40 -9 -3 0 -23.10 37.40 9 -3 0 12.20 15.40 -9 -3 0 3.40 13.20 9 -3 0 5.50 13.30 -9 -3 0 -12.40 14.20 -9 3 0 9.30 13.40 9 3 0 14.80 11.10 -9 3 0 0.90 24.00 9 3 0 -24.90 20.70 10 -3 0 83.89 23.20 10 -3 0 122.09 22.10 -10 -3 0 98.59 22.90 -10 -3 0 63.99 22.00 10 3 0 95.89 20.10 10 3 0 109.59 17.10 -10 3 0 125.19 22.60 10 3 0 75.39 14.30 0 -4 0 1.40 3.30 0 -4 0 2.30 3.30 0 -4 0 -1.00 3.60 0 -4 0 3.90 2.70 0 -4 0 3.60 3.60 0 4 0 6.20 4.60 0 4 0 6.80 3.80 0 4 0 -1.00 2.80 0 4 0 7.10 3.20 -1 -4 0 1409.16 38.80 1 -4 0 1476.75 39.80 -1 -4 0 1392.06 40.70 1 -4 0 1358.56 38.50 -1 -4 0 1408.26 39.00 1 -4 0 1473.55 40.70 -1 -4 0 1348.67 41.70 1 -4 0 1429.16 40.60 -1 -4 0 1446.76 39.90 -1 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14.70 -7 0 11 34.80 18.40 -7 0 11 80.99 18.80 -7 0 11 85.69 16.40 -6 0 11 0.60 11.40 -6 0 11 10.40 14.10 -6 0 11 -10.60 11.80 -6 0 11 -8.50 25.20 -6 0 11 -2.40 12.60 -5 0 11 -1.40 12.80 -5 0 11 1.60 13.50 -5 0 11 10.90 6.10 -5 0 11 68.59 25.30 -5 0 11 9.10 10.90 -5 0 11 19.60 10.90 -4 0 11 57.89 22.80 -4 0 11 -10.00 10.00 -4 0 11 5.80 12.60 -4 0 11 -14.00 12.80 -4 0 11 3.90 6.50 -4 0 11 0.40 8.50 -3 0 11 41.10 23.20 3 0 -11 35.10 20.00 -3 0 11 57.59 10.10 -3 0 11 48.30 7.40 -3 0 11 55.89 14.90 2 0 -11 4.00 18.90 -2 0 11 -5.70 9.40 -2 0 11 8.10 12.90 -2 0 11 3.00 14.80 1 0 -11 106.09 24.00 -1 0 11 84.39 17.60 -1 0 11 109.59 15.10 -1 0 11 104.69 19.00 0 0 -11 -0.10 38.90 0 0 11 38.90 18.60 0 0 11 1.20 15.00 0 0 11 -4.00 12.60 0 0 -11 64.09 24.40 -1 0 -11 33.20 24.40 1 0 11 40.80 16.40 1 0 11 22.00 18.50 -1 0 -11 15.70 26.90 2 0 11 -19.50 18.40 2 0 11 20.80 23.90 -2 0 -11 -14.30 24.20 -8 -1 11 48.10 20.50 -8 -1 11 49.40 15.00 -8 -1 11 72.59 30.20 -8 -1 11 43.10 9.70 -8 -1 11 63.09 19.80 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18.80 3 -1 -11 119.39 25.10 -3 -1 11 68.59 25.30 -3 1 11 115.59 16.90 -3 1 11 130.69 13.90 3 1 -11 91.59 26.90 -3 1 11 90.99 9.70 -3 1 11 87.59 19.50 -2 -1 11 42.80 15.40 -2 -1 11 24.50 12.70 -2 -1 11 15.00 9.90 2 -1 -11 19.20 20.30 -2 1 11 6.60 11.90 2 1 -11 16.40 17.80 -1 -1 11 -15.90 10.40 -1 -1 11 12.40 17.70 -1 -1 11 10.30 13.70 1 -1 -11 20.60 21.60 -1 1 11 -13.80 17.90 -1 1 11 17.70 13.40 1 1 -11 14.20 19.60 -1 1 11 -20.30 10.10 0 -1 11 23.50 15.90 0 -1 11 17.30 13.60 0 -1 -11 18.00 19.70 0 -1 11 3.80 19.10 0 1 11 17.40 19.50 0 1 -11 9.20 25.20 0 1 11 18.30 13.30 0 1 -11 29.20 22.80 0 1 11 5.70 14.10 1 -1 11 16.70 15.30 1 -1 11 -6.30 17.60 -1 -1 -11 29.00 25.70 1 -1 11 -14.30 17.00 -1 -1 -11 29.80 24.30 1 1 11 -27.30 15.00 -1 1 -11 -7.40 23.10 1 1 11 -1.90 15.00 -1 1 -11 52.39 28.20 1 1 11 -0.80 22.60 2 -1 11 109.79 24.40 2 1 11 125.09 21.00 -7 -2 11 -1.30 8.90 -7 -2 11 12.40 11.40 -7 -2 11 -42.20 25.00 -7 -2 11 8.70 8.40 -7 -2 11 27.80 11.40 -7 -2 11 4.60 17.70 -7 -2 11 17.90 17.20 -7 2 11 4.20 5.10 -7 2 11 15.70 16.40 -7 2 11 -10.70 12.90 -7 2 11 17.40 15.30 -6 -2 11 83.69 24.80 -6 -2 11 63.79 9.70 -6 -2 11 94.89 19.20 -6 -2 11 49.20 10.60 -6 -2 11 56.09 16.50 -6 -2 11 53.19 9.50 -6 -2 11 93.99 15.50 -6 2 11 69.09 14.60 -6 2 11 93.29 18.40 -6 2 11 76.29 17.60 -6 2 11 55.39 15.20 -5 -2 11 3.40 12.20 -5 -2 11 11.20 7.90 -5 -2 11 11.20 8.40 -5 -2 11 29.10 13.40 -5 -2 11 -6.60 22.30 -5 -2 11 20.10 8.30 -5 2 11 25.70 14.70 -5 2 11 18.70 13.30 -5 2 11 31.60 11.90 -5 2 11 -2.80 10.10 -5 2 11 6.50 5.90 -4 -2 11 -6.60 20.90 -4 -2 11 4.50 8.50 -4 -2 11 -1.40 10.90 -4 -2 11 15.90 8.60 -4 -2 11 9.20 7.10 -4 -2 11 -15.00 14.80 -4 2 11 -7.60 13.10 -4 2 11 -4.70 10.00 -4 2 11 10.70 9.20 -4 2 11 1.10 17.00 -4 2 11 3.90 7.10 -3 -2 11 272.67 17.00 -3 -2 11 259.67 16.70 -3 -2 11 234.78 29.50 -3 -2 11 258.17 14.80 -3 -2 11 247.98 19.00 -3 2 11 251.67 21.30 -3 2 11 243.68 17.00 3 2 -11 263.37 32.70 -3 2 11 225.98 13.30 -3 2 11 241.08 15.30 -3 2 11 280.57 28.30 -2 -2 11 131.09 23.10 -2 -2 11 100.59 14.10 -2 -2 11 109.29 13.00 -2 -2 11 77.59 11.30 2 -2 -11 83.39 24.10 -2 2 11 114.09 20.90 -2 2 11 74.09 14.50 -2 2 11 62.09 12.50 2 2 -11 108.19 23.50 -1 -2 11 9.60 10.70 -1 -2 11 7.30 11.60 1 -2 -11 7.60 18.60 -1 -2 11 -12.40 20.40 -1 2 11 8.00 11.70 -1 2 11 -2.10 16.00 1 2 -11 30.30 20.60 -1 2 11 11.20 12.30 -1 2 11 -46.20 20.40 0 -2 11 -26.20 12.40 0 -2 11 6.60 14.10 0 -2 11 -16.30 15.50 0 -2 -11 3.20 22.60 0 2 11 1.90 13.10 0 2 -11 32.10 26.90 0 2 -11 23.20 21.40 0 2 11 -4.80 22.90 0 2 11 -2.50 12.80 1 -2 11 -8.20 15.60 -1 -2 -11 41.60 23.00 1 -2 11 -7.80 18.60 1 -2 11 -8.00 17.50 1 2 11 32.70 15.10 1 2 11 7.20 16.50 1 2 11 4.40 25.80 -1 2 -11 22.80 24.20 -7 -3 11 65.19 20.50 -7 -3 11 60.09 13.00 -7 -3 11 75.69 12.20 -7 -3 11 51.19 19.80 -7 -3 11 88.89 26.80 -7 -3 11 67.59 9.80 -7 3 11 66.69 22.80 -7 3 11 39.80 17.50 -7 3 11 54.49 14.30 -6 -3 11 2.40 6.10 -6 -3 11 10.90 17.70 -6 -3 11 17.20 10.20 -6 -3 11 18.90 10.90 -6 -3 11 8.40 12.40 -6 -3 11 -4.40 14.90 -6 3 11 3.10 11.20 -6 3 11 27.70 21.20 -6 3 11 13.50 16.40 -6 3 11 7.00 13.20 -5 -3 11 1.60 11.00 -5 -3 11 6.30 9.90 -5 -3 11 23.70 13.90 -5 -3 11 10.40 16.60 -5 3 11 7.80 15.00 -5 3 11 -5.30 9.20 -5 3 11 -0.30 6.40 -5 3 11 9.70 11.70 -4 -3 11 352.86 24.80 -4 -3 11 313.17 31.40 -4 -3 11 341.97 21.50 -4 3 11 317.17 21.30 -4 3 11 342.37 17.60 -4 3 11 342.27 20.50 -4 3 11 384.66 31.30 -3 -3 11 339.37 21.90 -3 -3 11 352.26 32.00 -3 -3 11 341.17 22.80 -3 3 11 375.06 16.70 -3 3 11 349.27 20.20 -3 3 11 317.47 19.70 -3 3 11 353.86 31.80 -3 3 11 320.37 20.60 3 3 -11 328.77 32.80 -2 -3 11 10.50 14.70 2 -3 -11 33.10 21.20 -2 -3 11 9.70 11.80 -2 3 11 -18.70 10.00 -2 3 11 -1.30 15.20 -2 3 11 13.50 9.50 -1 -3 11 53.69 14.60 -1 -3 11 23.30 6.50 -1 -3 11 61.79 20.70 1 -3 -11 51.59 24.50 -1 -3 11 14.90 6.30 -1 3 11 21.90 19.00 -1 3 11 28.20 11.30 1 3 -11 42.30 21.50 -1 3 11 6.00 12.80 0 -3 -11 -14.20 21.80 0 -3 11 2.10 18.10 0 -3 11 -15.00 9.50 0 -3 11 6.70 14.70 0 3 11 -7.50 13.50 0 3 11 27.40 17.80 0 3 11 13.70 28.90 0 3 -11 12.20 22.10 1 -3 11 -0.40 18.80 -1 -3 -11 49.90 27.60 1 -3 11 67.99 23.00 -1 3 -11 40.30 26.20 1 3 11 24.50 21.70 -6 -4 11 3.00 13.30 -6 -4 11 54.79 21.00 -6 -4 11 21.90 13.90 -6 -4 11 40.40 13.00 -6 -4 11 19.60 18.00 -6 -4 11 -13.80 18.00 -6 4 11 29.20 8.50 -6 4 11 59.99 18.80 -6 4 11 21.70 15.00 -6 4 11 36.20 18.10 -5 -4 11 15.30 19.50 -5 -4 11 22.90 20.00 -5 -4 11 21.00 14.60 -5 -4 11 20.70 16.60 -5 -4 11 17.70 12.50 -5 4 11 12.70 12.70 -5 4 11 59.09 9.80 -5 4 11 28.80 16.90 -5 4 11 21.00 18.50 -5 4 11 24.20 6.90 -4 -4 11 13.50 11.80 -4 -4 11 54.89 15.20 -4 -4 11 15.90 19.40 -4 -4 11 31.90 14.50 -4 4 11 13.00 9.50 -4 4 11 37.40 17.80 -4 4 11 8.80 20.30 -4 4 11 3.70 11.10 -3 -4 11 -0.50 13.30 -3 -4 11 37.30 13.00 -3 -4 11 -2.40 18.10 -3 4 11 18.40 16.80 3 4 -11 62.09 21.70 -3 4 11 4.60 10.60 -3 4 11 3.20 8.30 -3 4 11 2.80 11.80 -2 -4 11 17.20 17.90 -2 -4 11 -10.60 12.90 2 4 -11 30.80 25.60 -2 4 11 10.30 11.40 -2 4 11 0.60 18.00 1 -4 -11 19.60 23.90 -1 -4 11 14.70 19.50 -1 -4 11 6.10 15.10 -1 4 11 15.00 13.20 -1 4 11 14.50 18.40 1 4 -11 36.40 22.50 0 -4 11 1.10 17.40 0 -4 11 10.40 21.60 0 -4 -11 -23.60 24.30 0 4 -11 -17.70 22.80 0 4 11 -8.20 20.40 0 4 11 11.60 16.60 -5 -5 11 15.40 19.90 -5 -5 11 22.60 14.70 -5 -5 11 23.00 19.80 -5 -5 11 12.40 21.90 -5 5 11 37.60 11.70 -5 5 11 28.60 20.50 -5 5 11 52.09 21.10 -5 5 11 -1.20 24.80 -4 -5 11 12.70 16.70 -4 -5 11 18.10 14.50 -4 -5 11 38.10 20.30 -4 -5 11 23.20 20.10 -4 -5 11 31.30 23.30 -4 5 11 17.00 11.20 -4 5 11 38.20 20.30 -4 5 11 25.80 20.70 -3 -5 11 72.19 16.90 -3 -5 11 74.99 16.70 -3 -5 11 118.49 26.20 -3 -5 11 70.29 23.00 -3 5 11 73.49 14.40 -3 5 11 63.29 19.80 -3 5 11 47.00 20.70 3 5 -11 68.89 22.80 -2 -5 11 64.79 17.50 -2 -5 11 35.50 22.10 -2 5 11 79.59 15.50 2 5 -11 85.89 24.20 -2 5 11 59.39 20.60 -1 -5 11 -0.60 16.70 -1 -5 11 11.30 22.40 1 -5 -11 -23.10 24.10 1 5 -11 58.79 27.30 -1 5 11 8.00 15.40 -1 5 11 -0.60 19.10 -6 0 12 23.90 19.60 -6 0 12 23.10 17.50 -6 0 12 28.20 15.10 -6 0 12 16.90 14.40 -5 0 12 10.00 12.90 -5 0 12 26.20 17.50 -5 0 12 -6.50 19.50 -5 0 12 -2.60 12.40 -5 0 12 1.10 7.60 -4 0 12 39.60 19.10 -4 0 12 36.50 9.50 -4 0 12 58.89 14.90 -4 0 12 46.40 18.10 -4 0 12 69.39 10.30 -3 0 12 -10.80 17.60 -3 0 12 17.90 13.40 -3 0 12 2.30 16.90 -3 0 12 -0.80 10.00 3 0 -12 -43.50 22.00 -3 0 12 22.20 18.50 -2 0 12 114.69 16.20 -2 0 12 89.29 20.50 -2 0 12 105.99 21.30 2 0 -12 74.39 28.10 -1 0 12 -15.30 24.30 1 0 -12 -28.80 26.10 -1 0 12 0.60 17.30 -1 0 12 -2.50 13.00 -6 -1 12 -13.30 15.50 -6 -1 12 0.60 12.20 -6 -1 12 7.70 18.30 -6 -1 12 42.20 16.40 -6 1 12 -2.20 16.00 -6 1 12 24.80 15.90 -6 1 12 19.40 14.10 -5 -1 12 -9.40 16.90 -5 -1 12 -14.40 19.80 -5 -1 12 -5.20 11.40 -5 -1 12 1.10 12.20 -5 -1 12 8.20 8.00 -5 1 12 11.20 11.90 -5 1 12 4.20 7.60 -5 1 12 10.80 14.80 -5 1 12 -16.10 14.00 -5 1 12 -10.10 17.40 -4 -1 12 35.90 10.20 -4 -1 12 10.80 19.00 -4 -1 12 29.30 10.60 -4 -1 12 42.00 12.10 -4 1 12 27.00 8.70 -4 1 12 33.10 15.30 -4 1 12 25.70 9.20 -4 1 12 50.29 15.80 -4 1 12 32.10 17.50 -3 -1 12 66.99 13.00 -3 -1 12 35.20 31.50 -3 -1 12 60.39 13.30 -3 -1 12 47.20 15.20 3 -1 -12 23.90 24.20 3 1 -12 26.70 24.10 -3 1 12 30.00 15.80 -3 1 12 43.70 11.10 -3 1 12 34.50 18.90 2 -1 -12 103.79 28.70 -2 -1 12 66.19 35.30 -2 -1 12 112.39 16.30 2 1 -12 104.89 28.30 -2 1 12 63.69 23.60 -2 1 12 103.59 19.00 -2 1 12 78.39 14.40 -2 1 12 93.29 25.80 -1 -1 12 -26.80 18.90 -1 -1 12 -8.70 14.30 1 -1 -12 -9.80 24.30 -1 1 12 52.79 23.60 -1 1 12 5.10 13.60 -1 1 12 24.90 17.30 1 1 -12 6.20 25.60 -5 -2 12 9.20 8.20 -5 -2 12 20.70 18.70 -5 -2 12 16.10 14.10 -5 -2 12 28.80 9.50 -5 -2 12 20.70 16.90 -5 2 12 7.50 7.60 -5 2 12 29.00 18.80 -5 2 12 45.10 20.20 -5 2 12 11.60 12.40 -5 2 12 -3.90 12.90 -4 -2 12 55.19 12.50 -4 -2 12 66.19 13.60 -4 -2 12 73.39 9.20 -4 -2 12 46.10 19.60 -4 2 12 95.89 19.30 -4 2 12 76.09 19.90 -4 2 12 55.29 10.80 -4 2 12 33.50 14.00 -4 2 12 76.09 11.00 -3 -2 12 49.70 13.20 -3 -2 12 32.40 8.50 -3 -2 12 7.40 19.60 -3 2 12 34.80 14.30 -3 2 12 48.70 21.80 3 2 -12 16.70 23.80 -3 2 12 24.20 11.70 -2 -2 12 151.18 25.40 -2 -2 12 194.08 15.30 -2 -2 12 168.18 19.90 2 -2 -12 142.09 29.90 -2 2 12 159.18 26.90 -2 2 12 165.18 21.50 -2 2 12 112.89 18.20 2 2 -12 157.68 31.50 -4 -3 12 492.55 27.80 -4 -3 12 478.05 40.10 -4 -3 12 452.25 29.00 -4 3 12 483.15 38.60 -4 3 12 553.84 25.50 -4 3 12 554.14 23.90 -4 3 12 547.65 24.00 -3 -3 12 180.58 22.50 -3 -3 12 152.38 25.50 3 3 -12 239.98 35.30 -3 3 12 175.78 20.30 -3 3 12 185.98 28.70 -3 3 12 252.37 19.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 45908 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 O2 O 0.65330(15) 0.29099(13) -0.06670(13) 0.0168(3) Uani 1 1 d . . . . . N1 N 0.48459(16) 0.23668(14) 0.06287(15) 0.0095(3) Uani 1 1 d . . . . . O51 O 0.36818(15) -0.05522(13) 0.34837(14) 0.0193(3) Uani 1 1 d . . . . . N3 N 0.71560(16) 0.10666(15) 0.08855(15) 0.0118(3) Uani 1 1 d . . . . . O4 O 0.76529(15) -0.08971(12) 0.22461(13) 0.0167(3) Uani 1 1 d . . . . . N6 N 0.32061(18) 0.19064(16) 0.20317(17) 0.0142(3) Uani 1 1 d . . . . . C5 C 0.5361(2) 0.03726(17) 0.22010(18) 0.0106(4) Uani 1 1 d . . . . . C6 C 0.44549(19) 0.15587(17) 0.16367(18) 0.0100(4) Uani 1 1 d . . . . . C4 C 0.67763(19) 0.00982(17) 0.18150(17) 0.0109(4) Uani 1 1 d . . . . . C51 C 0.4898(2) -0.05999(19) 0.31097(19) 0.0156(4) Uani 1 1 d . . . . . C1 C 0.3819(2) 0.35232(18) -0.0053(2) 0.0160(4) Uani 1 1 d . . . . . H1A H 0.273353 0.318957 -0.045972 0.024 Uiso 1 1 calc R U . . . H1B H 0.417664 0.391687 -0.084110 0.024 Uiso 1 1 calc R U . . . H1C H 0.386032 0.423733 0.068647 0.024 Uiso 1 1 calc R U . . . C3 C 0.8613(2) 0.08279(19) 0.0507(2) 0.0178(4) Uani 1 1 d . . . . . H3A H 0.867139 0.148530 -0.025565 0.027 Uiso 1 1 calc R U . . . H3B H 0.861682 -0.012117 0.014294 0.027 Uiso 1 1 calc R U . . . H3C H 0.952406 0.096010 0.138088 0.027 Uiso 1 1 calc R U . . . C2 C 0.6217(2) 0.21678(17) 0.02282(18) 0.0107(4) Uani 1 1 d . . . . . H51 H 0.562(2) -0.137(2) 0.340(2) 0.018(5) Uiso 1 1 d . . . . . H62 H 0.264(3) 0.269(2) 0.175(2) 0.024(6) Uiso 1 1 d . . . . . H61 H 0.294(3) 0.136(2) 0.270(3) 0.030(6) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0194(7) 0.0170(6) 0.0183(7) 0.0020(5) 0.0122(6) -0.0009(5) N1 0.0090(7) 0.0084(7) 0.0115(7) 0.0001(5) 0.0036(6) 0.0005(5) O51 0.0203(7) 0.0185(7) 0.0225(7) 0.0012(6) 0.0114(6) -0.0043(5) N3 0.0084(7) 0.0145(7) 0.0141(7) -0.0018(6) 0.0057(6) 0.0011(6) O4 0.0154(6) 0.0139(6) 0.0192(7) 0.0016(5) 0.0029(5) 0.0053(5) N6 0.0140(8) 0.0128(7) 0.0188(8) 0.0014(6) 0.0096(6) 0.0015(6) C5 0.0111(8) 0.0103(8) 0.0100(8) -0.0022(6) 0.0024(6) -0.0017(6) C6 0.0092(8) 0.0105(8) 0.0106(8) -0.0033(6) 0.0035(6) -0.0032(6) C4 0.0110(8) 0.0094(8) 0.0103(8) -0.0031(6) 0.0003(7) -0.0009(6) C51 0.0163(9) 0.0141(9) 0.0159(9) 0.0003(7) 0.0042(7) -0.0016(7) C1 0.0161(9) 0.0134(9) 0.0203(9) 0.0056(7) 0.0081(8) 0.0045(7) C3 0.0129(9) 0.0190(9) 0.0253(10) -0.0029(8) 0.0116(8) 0.0025(7) C2 0.0111(8) 0.0111(8) 0.0112(8) -0.0040(6) 0.0052(7) -0.0017(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 C6 N1 C2 123.11(14) . . C6 N1 C1 119.42(14) . . C2 N1 C1 117.46(13) . . C2 N3 C4 124.99(14) . . C2 N3 C3 117.84(14) . . C4 N3 C3 117.03(14) . . C6 N6 H62 125.0(13) . . C6 N6 H61 118.2(14) . . H62 N6 H61 117(2) . . C6 C5 C51 122.07(15) . . C6 C5 C4 119.60(15) . . C51 C5 C4 118.30(15) . . N6 C6 N1 118.33(15) . . N6 C6 C5 121.98(15) . . N1 C6 C5 119.68(15) . . O4 C4 N3 118.94(15) . . O4 C4 C5 125.02(16) . . N3 C4 C5 116.04(14) . . O51 C51 C5 126.35(17) . . O51 C51 H51 120.7(12) . . C5 C51 H51 113.0(12) . . N1 C1 H1A 109.5 . . N1 C1 H1B 109.5 . . H1A C1 H1B 109.5 . . N1 C1 H1C 109.5 . . H1A C1 H1C 109.5 . . H1B C1 H1C 109.5 . . N3 C3 H3A 109.5 . . N3 C3 H3B 109.5 . . H3A C3 H3B 109.5 . . N3 C3 H3C 109.5 . . H3A C3 H3C 109.5 . . H3B C3 H3C 109.5 . . O2 C2 N3 122.53(15) . . O2 C2 N1 121.42(16) . . N3 C2 N1 116.04(14) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O2 C2 1.213(2) . N1 C6 1.365(2) . N1 C2 1.399(2) . N1 C1 1.464(2) . O51 C51 1.240(2) . N3 C2 1.380(2) . N3 C4 1.400(2) . N3 C3 1.467(2) . O4 C4 1.227(2) . N6 C6 1.322(2) . N6 H62 0.90(2) . N6 H61 0.92(2) . C5 C6 1.409(2) . C5 C51 1.423(2) . C5 C4 1.441(2) . C51 H51 0.97(2) . C1 H1A 0.9800 . C1 H1B 0.9800 . C1 H1C 0.9800 . C3 H3A 0.9800 . C3 H3B 0.9800 . C3 H3C 0.9800 . 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 C2 N1 C6 N6 174.21(15) . . . . C1 N1 C6 N6 -4.2(2) . . . . C2 N1 C6 C5 -7.1(2) . . . . C1 N1 C6 C5 174.46(15) . . . . C51 C5 C6 N6 6.6(3) . . . . C4 C5 C6 N6 -175.49(15) . . . . C51 C5 C6 N1 -171.99(15) . . . . C4 C5 C6 N1 5.9(2) . . . . C2 N3 C4 O4 174.56(15) . . . . C3 N3 C4 O4 -0.9(2) . . . . C2 N3 C4 C5 -6.0(2) . . . . C3 N3 C4 C5 178.51(14) . . . . C6 C5 C4 O4 179.73(16) . . . . C51 C5 C4 O4 -2.3(3) . . . . C6 C5 C4 N3 0.3(2) . . . . C51 C5 C4 N3 178.27(14) . . . . C6 C5 C51 O51 1.5(3) . . . . C4 C5 C51 O51 -176.40(17) . . . . C4 N3 C2 O2 -173.53(16) . . . . C3 N3 C2 O2 2.0(2) . . . . C4 N3 C2 N1 5.1(2) . . . . C3 N3 C2 N1 -179.45(14) . . . . C6 N1 C2 O2 -179.63(15) . . . . C1 N1 C2 O2 -1.2(2) . . . . C6 N1 C2 N3 1.8(2) . . . . C1 N1 C2 N3 -179.77(14) . . . . _cod_database_fobs_code 3500075