#------------------------------------------------------------------------------ #$Date: 2017-04-25 03:13:55 +0300 (Tue, 25 Apr 2017) $ #$Revision: 195731 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/57/1545799.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_1545799 loop_ _publ_author_name 'Hu, Feng' 'Nareddy, Pradeep' 'Lalancette, Roger' 'Jordan, Frank' 'Szostak, Michal' _publ_section_title ; \s N--C Bond Difunctionalization in Bridged Twisted Amides: Sew-and-Cut Activation Approach to Functionalized Isoquinolines ; _journal_name_full 'Organic Letters' _journal_paper_doi 10.1021/acs.orglett.7b00913 _journal_year 2017 _chemical_formula_moiety 'C13 H13 N O' _chemical_formula_sum 'C13 H13 N O' _chemical_formula_weight 199.24 _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 93.637(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.2899(6) _cell_length_b 10.1880(5) _cell_length_c 8.5203(5) _cell_measurement_reflns_used 4823 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.48 _cell_measurement_theta_min 3.92 _cell_volume 978.04(9) _computing_cell_refinement 'APEX 2' _computing_data_collection 'APEX 2 (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.951 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measurement_device_type 'Bruker SMART CCD Apex-II area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_Laue_measured_fraction_full 0.951 _diffrn_reflns_Laue_measured_fraction_max 0.929 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 8051 _diffrn_reflns_point_group_measured_fraction_full 0.951 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.956 _diffrn_reflns_theta_min 3.923 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.353 _exptl_crystal_description tablet _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.218 _exptl_crystal_size_mid 0.189 _exptl_crystal_size_min 0.092 _refine_diff_density_max 0.227 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.042 _refine_ls_extinction_coef 0.0027(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 1694 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0366 _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^)+(0.0422P)^2^+0.3128P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.0908 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1467 _reflns_number_total 1694 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol7b00913_si_002.cif _cod_data_source_block FENG7_a _cod_database_code 1545799 _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_estimated_absorpt_t_min 0.867 _shelx_estimated_absorpt_t_max 0.940 _shelx_res_file ; FENG7_a.res created by SHELXL-2014/7 TITL FENG7_a.res in P2(1)/c CELL 1.54178 11.2899 10.1880 8.5203 90.000 93.637 90.000 ZERR 4.000 0.0006 0.0005 0.0005 0.000 0.003 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 52 52 4 4 OMIT -1 5 4 OMIT -4 4 4 OMIT -8 1 4 L.S. 25 ACTA BOND $H FMAP 2 PLAN 2 SIZE 0.092 0.189 0.218 TEMP -173.150 WGHT 0.042200 0.312800 EXTI 0.002690 FVAR 0.95458 O1 4 0.505030 0.666641 0.817421 11.00000 0.02468 0.02027 = 0.02648 -0.00046 -0.00013 0.00453 N1 3 0.650061 0.589951 0.990747 11.00000 0.02294 0.01749 = 0.01775 -0.00171 0.00149 -0.00049 C1 1 0.571151 0.577258 0.862659 11.00000 0.01791 0.01846 = 0.01865 0.00017 0.00491 -0.00183 C2 1 0.572643 0.446738 0.778593 11.00000 0.01747 0.01841 = 0.02046 -0.00060 -0.00058 -0.00151 AFIX 23 H2A 2 0.500074 0.438943 0.707649 11.00000 -1.20000 H2B 2 0.571291 0.375211 0.857109 11.00000 -1.20000 AFIX 0 C3 1 0.694161 0.721765 1.030695 11.00000 0.02823 0.02093 = 0.02342 -0.00495 -0.00127 -0.00119 AFIX 23 H3A 2 0.702617 0.732176 1.146388 11.00000 -1.20000 H3B 2 0.637093 0.788426 0.987790 11.00000 -1.20000 AFIX 0 C4 1 0.812341 0.741279 0.962427 11.00000 0.02619 0.01989 = 0.02274 -0.00075 -0.00564 -0.00454 AFIX 43 H4 2 0.845199 0.827134 0.962969 11.00000 -1.20000 AFIX 0 C5 1 0.873161 0.644117 0.901271 11.00000 0.02078 0.02453 = 0.02061 0.00038 -0.00333 -0.00356 AFIX 43 H5 2 0.943829 0.665255 0.851894 11.00000 -1.20000 AFIX 0 C6 1 0.835511 0.500920 0.906234 11.00000 0.01889 0.02039 = 0.01979 0.00110 -0.00424 0.00184 AFIX 13 H6 2 0.905695 0.448837 0.947948 11.00000 -1.20000 AFIX 0 C7 1 0.740242 0.489348 1.023848 11.00000 0.02570 0.02017 = 0.01592 0.00002 -0.00218 0.00032 AFIX 23 H7A 2 0.703363 0.401233 1.016130 11.00000 -1.20000 H7B 2 0.776247 0.500614 1.132005 11.00000 -1.20000 AFIX 0 C8 1 0.798801 0.448477 0.741703 11.00000 0.02158 0.01112 = 0.01987 0.00302 -0.00047 0.00073 C9 1 0.681042 0.429933 0.682940 11.00000 0.02158 0.01063 = 0.01922 0.00182 0.00065 0.00027 C10 1 0.660402 0.387480 0.527194 11.00000 0.02406 0.01378 = 0.02059 0.00230 -0.00200 -0.00199 AFIX 43 H10 2 0.580889 0.377140 0.485536 11.00000 -1.20000 AFIX 0 C11 1 0.752255 0.360148 0.432178 11.00000 0.03403 0.01558 = 0.01785 0.00059 0.00252 -0.00194 AFIX 43 H11 2 0.735725 0.332307 0.326645 11.00000 -1.20000 AFIX 0 C12 1 0.868384 0.373720 0.492201 11.00000 0.02815 0.01771 = 0.02647 0.00227 0.00984 0.00078 AFIX 43 H12 2 0.932344 0.352686 0.429420 11.00000 -1.20000 AFIX 0 C13 1 0.890394 0.418444 0.645278 11.00000 0.01939 0.01728 = 0.02760 0.00306 0.00118 -0.00014 AFIX 43 H13 2 0.970250 0.428896 0.685522 11.00000 -1.20000 AFIX 0 HKLF 4 REM FENG7_a.res in P2(1)/c REM R1 = 0.0366 for 1467 Fo > 4sig(Fo) and 0.0436 for all 1694 data REM 137 parameters refined using 0 restraints END WGHT 0.0422 0.3127 REM Highest difference peak 0.227, deepest hole -0.185, 1-sigma level 0.042 Q1 1 0.8641 0.6622 0.9905 11.00000 0.05 0.23 Q2 1 0.8078 0.4326 0.4588 11.00000 0.05 0.21 ; _shelx_res_checksum 94569 _shelx_hkl_file ; 0 0 1 2.40 0.50 0 0 1 2.90 0.60 0 0 -1 1.20 0.50 0 0 1 1.70 0.40 0 0 2 4282.57 100.09 0 0 -2 4241.58 100.29 0 0 2 3974.80 100.09 0 0 2 4169.08 100.29 0 0 3 -0.40 0.70 0 0 -3 0.60 0.90 0 0 3 0.40 0.90 0 0 -4 1285.07 33.30 0 0 4 1262.27 33.60 0 0 4 1259.37 32.70 0 0 4 1252.17 33.10 0 0 5 0.10 1.00 0 0 5 -0.30 1.10 0 0 -5 -0.70 1.00 0 0 5 0.00 1.30 0 0 6 646.44 21.50 0 0 6 610.44 19.90 0 0 7 0.70 2.30 0 0 7 -0.80 1.60 0 0 7 -0.70 1.80 0 0 8 65.19 7.20 0 0 8 64.39 6.80 0 0 8 66.89 5.20 0 0 9 0.10 1.60 0 0 9 0.30 1.80 0 0 9 0.00 2.00 0 0 10 14.70 2.20 0 0 10 15.60 2.10 0 1 0 3.00 0.40 0 1 0 1.30 0.20 0 1 0 1.20 0.20 0 -1 0 4.20 0.50 0 -1 0 1.90 0.40 0 -1 0 3.10 0.90 0 -1 0 1.10 0.30 0 -1 0 1.30 0.30 0 1 1 1085.29 26.20 0 1 1 1077.19 26.70 0 1 1 1041.80 26.30 0 -1 1 1073.59 26.50 0 -1 -1 1024.90 27.40 0 -1 -1 1091.39 26.40 0 -1 1 1119.59 26.40 0 -1 -1 1076.79 26.70 0 -1 -1 1101.69 26.60 0 -1 1 1146.09 26.70 0 1 -2 1649.04 43.70 0 1 -2 1748.03 42.80 0 1 2 1675.63 42.50 0 1 2 1777.02 42.90 0 -1 -2 1749.72 42.80 0 -1 -2 1790.82 42.90 0 -1 -2 1781.62 42.30 0 -1 2 1749.32 42.00 0 -1 2 1711.23 42.00 0 -1 2 1752.62 42.80 0 1 -3 -1.20 0.60 0 1 3 1.30 0.90 0 1 -3 2.10 1.10 0 1 3 1.10 1.00 0 -1 -3 10.60 1.30 0 -1 3 1.20 0.70 0 -1 3 1.20 0.80 0 -1 3 1.80 1.00 0 -1 -3 1.20 0.90 0 1 4 307.67 11.30 0 1 -4 318.87 10.40 0 1 4 327.57 10.30 0 1 4 314.87 10.40 0 -1 -4 304.67 9.40 0 -1 -4 309.97 10.40 0 -1 4 309.37 10.40 0 -1 4 305.47 9.80 0 -1 4 313.97 9.60 0 1 5 45.00 3.70 0 1 5 45.40 4.50 0 1 5 45.50 3.70 0 1 -5 43.80 3.70 0 -1 5 39.50 3.00 0 -1 5 44.80 3.70 0 -1 -5 40.30 3.70 0 -1 5 43.20 3.90 0 1 6 0.60 1.50 0 1 6 0.00 1.90 0 1 6 0.60 2.10 0 -1 6 1.20 1.50 0 -1 6 0.70 1.50 0 1 7 5.40 3.00 0 1 7 5.40 2.10 0 1 7 6.70 3.10 0 -1 7 6.10 3.00 0 -1 7 4.70 2.60 0 -1 7 7.70 2.30 0 1 8 41.20 4.40 0 1 8 37.40 6.30 0 1 8 40.30 6.00 0 1 8 39.30 4.40 0 -1 8 41.90 5.40 0 -1 8 44.10 6.20 0 -1 8 39.60 4.50 0 1 9 173.48 7.90 0 1 9 164.38 9.50 0 1 9 167.38 7.20 0 -1 9 166.78 9.60 0 -1 9 160.98 7.70 0 1 10 1.90 1.40 0 1 10 1.20 1.40 0 1 -10 3.20 1.60 0 -1 -10 1.50 1.60 0 -1 10 3.30 1.40 0 -1 10 3.30 1.40 0 2 0 2904.61 67.79 0 -2 0 2729.43 68.29 0 -2 0 2880.71 68.29 0 -2 0 2915.91 68.59 0 -2 0 2776.62 71.69 0 2 1 1.20 0.90 0 2 1 0.70 0.50 0 -2 1 1.60 0.80 0 -2 -1 2.10 0.80 0 -2 1 1.50 0.70 0 -2 1 1.20 0.60 0 -2 -1 1.40 1.30 0 -2 1 2.40 1.50 0 -2 -1 1.10 0.80 0 -2 -1 1.00 0.70 0 2 2 757.82 19.90 0 2 2 790.92 19.80 0 2 2 811.02 20.90 0 -2 2 807.22 20.80 0 -2 -2 786.32 22.30 0 -2 -2 818.62 20.70 0 -2 2 798.72 20.50 0 -2 -2 796.72 20.20 0 -2 2 749.73 23.40 0 -2 -2 800.92 20.80 0 2 3 1367.26 34.30 0 2 3 1362.36 35.20 0 2 -3 1305.47 36.90 0 2 -3 1390.26 35.00 0 -2 3 1380.76 34.90 0 -2 -3 1356.16 34.10 0 -2 -3 1380.66 35.00 0 2 4 5.60 1.60 0 2 4 5.00 2.00 0 2 4 2.50 1.30 0 2 -4 3.40 1.50 0 -2 4 3.20 1.30 0 -2 -4 2.90 1.00 0 -2 -4 3.00 1.30 0 -2 4 3.40 1.00 0 2 5 21.00 2.90 0 2 -5 26.30 3.50 0 2 5 31.40 3.60 0 2 5 24.10 4.00 0 -2 5 20.90 2.70 0 -2 5 21.50 2.20 0 -2 5 22.60 3.30 0 -2 -5 23.80 2.90 0 2 6 23.80 5.00 0 2 6 20.90 4.10 0 2 6 25.10 3.50 0 -2 6 21.40 3.50 0 -2 6 19.10 3.20 0 2 7 -0.60 2.30 0 2 7 -1.50 1.50 0 2 7 -3.30 2.60 0 2 7 1.40 2.30 0 -2 7 1.90 2.30 0 -2 7 1.20 1.80 0 -2 7 3.60 2.20 0 2 8 169.08 8.10 0 2 8 158.38 10.10 0 2 8 161.08 7.60 0 -2 8 167.38 8.10 0 -2 8 156.68 9.60 0 -2 8 151.08 9.80 0 2 9 65.39 4.60 0 2 9 60.99 4.20 0 -2 9 69.99 6.00 0 -2 -9 58.89 5.40 0 -2 9 60.29 4.50 0 2 10 11.80 1.60 0 2 10 13.80 2.10 0 -2 10 7.20 2.40 0 -2 -10 14.20 2.40 0 3 0 0.30 0.40 0 -3 0 -0.10 1.40 0 -3 0 0.00 0.60 0 -3 0 0.20 0.70 0 -3 0 -0.50 0.70 0 -3 0 0.10 0.70 0 3 1 1047.30 27.40 0 3 1 1111.59 26.60 0 -3 1 1025.40 26.70 0 -3 -1 1045.70 26.30 0 -3 -1 1098.69 27.60 0 -3 -1 1070.19 31.60 0 -3 -1 1094.49 27.30 0 -3 1 1081.19 32.10 0 -3 -1 1102.19 27.60 0 -3 1 1107.09 27.60 0 -3 1 1100.69 27.30 0 3 2 1521.45 37.70 0 3 2 1567.54 39.20 0 -3 -2 1542.15 38.30 0 -3 -2 1556.14 38.90 0 -3 2 1521.75 38.40 0 -3 2 1592.34 39.10 0 -3 -2 1535.35 39.10 0 -3 -2 1483.15 42.00 0 -3 2 1500.75 43.50 0 3 3 1535.25 44.80 0 3 -3 1738.03 43.10 0 3 -3 1652.73 46.80 0 -3 -3 1700.33 42.30 0 -3 3 1726.03 42.80 0 -3 3 1726.43 43.40 0 -3 -3 1709.13 43.10 0 3 -4 176.18 7.30 0 -3 -4 172.98 6.50 0 -3 4 176.58 7.20 0 -3 -4 162.78 7.10 0 3 -5 15.60 2.70 0 -3 5 15.20 1.80 0 -3 -5 15.20 2.80 0 -3 5 15.80 3.00 0 3 6 41.80 5.80 0 3 6 45.10 4.10 0 3 6 36.80 4.10 0 -3 6 41.50 5.40 0 -3 6 35.80 3.80 0 -3 6 45.40 4.50 0 -3 6 39.80 4.30 0 3 7 0.30 1.90 0 3 7 0.30 1.70 0 3 7 0.20 2.30 0 -3 7 -1.30 1.60 0 -3 7 -2.00 1.90 0 -3 7 -0.30 1.50 0 3 8 177.28 8.30 0 3 8 188.38 7.70 0 -3 -8 192.48 10.10 0 -3 8 172.88 9.70 0 -3 8 170.18 10.20 0 -3 8 169.98 8.20 0 3 9 25.10 2.70 0 3 9 28.50 3.30 0 -3 9 31.40 3.30 0 -3 -9 28.80 4.00 0 -3 9 22.80 3.90 0 4 0 1125.49 27.70 0 -4 0 1135.89 29.20 0 -4 0 1123.59 28.90 0 -4 0 1131.49 28.70 0 -4 0 1117.59 35.10 0 4 1 3893.91 92.39 0 -4 -1 3840.22 93.69 0 -4 1 3906.11 92.49 0 -4 -1 3709.63 94.69 0 -4 1 3831.82 93.69 0 -4 -1 3839.72 93.69 0 -4 -1 3815.72 93.29 0 -4 1 3825.92 93.29 0 -4 -1 3856.11 99.89 0 -4 1 3857.11 100.49 0 4 2 58.49 2.80 0 -4 2 62.29 6.50 0 -4 2 61.09 3.60 0 -4 -2 60.89 5.90 0 -4 2 55.39 3.00 0 -4 -2 60.89 3.30 0 -4 -2 85.19 4.60 0 -4 2 56.39 3.30 0 -4 -2 58.69 3.60 0 -4 -2 60.19 3.80 0 4 -3 550.34 21.00 0 -4 3 547.85 16.70 0 -4 -3 563.04 16.70 0 -4 3 553.34 16.10 0 -4 -3 567.24 15.90 0 4 -4 31.70 3.20 0 -4 4 28.70 2.90 0 -4 -4 29.00 2.70 0 -4 -4 27.20 3.10 0 4 5 -1.80 8.20 0 -4 5 0.40 1.50 0 4 6 143.39 7.00 0 4 6 144.39 6.50 0 -4 -6 139.59 8.40 0 -4 6 142.49 9.10 0 4 7 3.20 1.80 0 4 7 4.00 1.90 0 -4 -7 -2.20 2.00 0 -4 7 3.00 1.80 0 -4 7 2.60 2.60 0 4 8 -1.90 1.30 0 4 8 1.80 1.70 0 -4 8 -0.60 2.00 0 -4 -8 1.60 2.00 0 4 9 86.59 4.80 0 -4 -9 88.19 5.80 0 -4 9 83.79 5.90 0 5 0 1.10 0.60 0 -5 0 0.50 0.90 0 -5 0 0.60 1.00 0 -5 0 -0.40 0.80 0 -5 0 0.10 1.80 0 -5 0 1.00 0.90 0 5 1 1555.74 37.60 0 5 -1 1535.25 36.80 0 -5 1 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4.30 9 -6 3 46.80 4.30 -9 -6 -3 49.10 4.60 9 -6 3 49.99 4.10 9 6 4 0.10 1.30 -9 -6 -4 1.50 1.80 9 -6 4 -1.10 1.40 9 -6 4 -0.50 1.40 9 6 5 24.50 2.60 9 -6 5 23.00 2.50 -9 -7 5 113.49 5.20 -9 -7 4 5.80 3.70 -9 -7 4 2.80 1.60 -9 -7 3 169.08 14.30 -9 -7 3 162.18 7.30 -9 -7 3 143.39 14.50 -9 7 2 21.70 6.50 -9 -7 2 22.30 6.90 9 -7 -2 23.20 3.90 -9 -7 2 24.40 3.30 -9 -7 2 20.10 6.50 -9 7 1 8.90 6.20 -9 -7 1 18.40 2.90 9 -7 -1 17.40 3.70 -9 -7 1 13.30 5.80 -9 7 0 158.68 16.00 9 7 0 161.88 7.40 9 -7 0 155.28 8.80 -9 -7 0 170.38 15.20 9 7 1 256.67 9.70 -9 7 -1 258.07 19.30 -9 -7 -1 247.68 18.00 9 -7 1 246.08 11.20 -9 7 -2 111.69 13.80 9 7 2 112.49 5.80 9 -7 2 113.99 5.60 9 -7 2 102.69 6.90 9 7 3 2.70 1.60 -9 -7 -3 2.50 1.80 9 -7 3 1.50 1.60 9 -7 3 5.50 2.40 9 -7 3 2.80 1.80 9 7 4 73.09 4.10 9 -7 4 64.69 3.70 9 -8 -3 120.69 6.40 -9 -8 3 121.59 12.20 -9 -8 3 124.29 5.60 -9 -8 3 129.59 11.20 9 8 -2 43.70 3.20 -9 8 2 41.70 7.20 -9 -8 2 36.80 7.50 -9 -8 2 37.40 7.70 9 -8 -2 40.10 4.30 9 8 -1 55.39 3.90 -9 8 1 49.99 9.00 -9 -8 1 60.19 9.20 9 -8 -1 50.29 4.90 -9 8 0 51.79 9.70 9 8 0 56.59 3.90 9 -8 0 60.09 5.10 -9 -8 0 62.79 9.10 9 -8 0 62.69 3.50 9 8 1 12.70 2.30 -9 8 -1 4.60 4.70 9 -8 1 11.00 2.10 9 -8 1 9.40 2.60 -9 -8 -1 12.80 4.70 9 8 2 10.70 2.00 -9 8 -2 15.80 5.20 9 -8 2 10.50 2.50 9 -8 2 8.20 1.90 9 -8 3 -0.30 1.10 -9 9 1 2.60 2.60 -9 -9 1 3.40 2.90 -9 9 0 89.39 8.80 -9 -9 0 88.79 8.80 -10 0 7 0.20 1.20 -10 0 7 0.10 2.30 -10 0 6 7.40 4.30 -10 0 6 12.90 2.40 -10 0 5 -1.30 3.50 -10 0 5 0.00 1.80 -10 0 3 1.10 4.20 -10 0 3 1.30 1.90 -10 0 2 594.34 30.60 -10 0 1 0.30 3.90 -10 0 0 2.80 4.30 -10 0 -1 0.00 4.70 -10 0 -2 341.87 22.90 -10 0 -4 5.90 2.30 -10 0 -5 2.20 1.70 -10 0 -6 36.90 3.30 -10 1 7 3.00 1.30 -10 1 7 2.10 3.60 -10 -1 7 4.90 3.60 -10 -1 7 6.30 1.60 -10 1 6 44.30 8.60 -10 1 6 57.39 3.80 -10 -1 6 46.30 3.80 -10 -1 6 44.90 8.50 -10 -1 6 49.50 3.90 -10 1 5 20.20 3.00 -10 1 5 21.40 7.60 -10 -1 5 19.50 2.90 -10 -1 5 14.60 5.80 -10 -1 5 19.60 3.00 -10 1 2 48.00 10.30 -10 -1 2 57.19 10.50 -10 1 1 53.89 10.40 -10 -1 1 58.99 10.80 -10 1 0 67.59 11.50 -10 -1 0 60.19 11.10 -10 1 -1 401.76 25.60 -10 -1 -1 418.76 25.80 -10 1 -2 35.70 9.50 -10 -1 -2 32.10 8.90 -10 1 -4 200.38 8.60 -10 -1 -4 189.98 8.70 -10 1 -5 0.80 1.70 -10 -1 -5 1.00 1.60 -10 1 -6 19.90 3.60 -10 -1 -6 20.20 3.60 -10 -2 7 32.60 2.90 -10 2 6 -0.60 2.70 -10 2 6 -0.30 1.30 -10 -2 6 -0.30 2.60 -10 -2 6 2.10 1.40 -10 -2 6 0.70 1.50 -10 2 5 8.30 2.00 -10 -2 5 7.70 2.10 -10 -2 5 6.00 4.40 -10 -2 5 8.90 2.30 -10 2 3 25.00 7.50 -10 -2 3 32.70 4.10 -10 -2 3 31.90 8.40 -10 -2 3 46.50 4.60 -10 -2 3 28.00 6.40 -10 2 2 226.08 18.30 -10 -2 2 230.08 10.10 -10 -2 2 216.78 18.00 -10 2 1 423.16 25.70 -10 -2 1 429.56 25.60 -10 -2 1 427.56 15.10 -10 2 0 154.88 15.80 -10 -2 0 156.78 8.20 -10 -2 0 158.48 15.80 10 2 1 127.59 6.80 -10 2 -1 141.39 15.90 -10 -2 -1 140.79 15.40 -10 2 -2 191.28 17.10 10 2 2 184.18 8.20 -10 -2 -2 180.78 16.20 10 -2 3 16.40 2.50 -10 2 -4 29.60 3.60 10 -2 4 26.10 2.70 -10 -2 -4 25.30 3.60 -10 2 -5 19.30 2.80 -10 -2 -5 15.70 2.60 -10 -3 6 8.60 2.10 -10 -3 6 4.90 3.40 -10 -3 6 5.90 1.70 -10 -3 5 13.20 5.60 -10 -3 5 19.90 3.00 -10 -3 5 11.80 2.40 -10 -3 4 7.40 5.40 -10 -3 4 11.10 2.80 -10 -3 4 10.30 2.60 -10 3 3 86.09 11.80 -10 -3 3 88.79 6.10 -10 -3 3 92.99 8.10 -10 -3 3 101.89 12.80 -10 -3 3 84.09 11.90 -10 -3 3 85.19 5.70 -10 3 1 218.18 17.90 -10 -3 1 221.98 9.90 -10 -3 1 209.58 17.90 -10 3 0 55.49 10.70 -10 -3 0 60.99 5.30 -10 -3 0 56.79 10.60 -10 3 -1 306.87 21.10 10 3 1 299.37 11.20 -10 -3 -1 295.17 20.90 10 3 2 66.59 4.90 -10 3 -2 84.69 12.80 -10 -3 -2 72.89 11.60 10 -3 2 65.19 4.10 10 3 3 60.39 4.70 10 -3 3 60.89 4.00 -10 3 -4 167.68 7.70 10 3 4 172.08 7.40 10 -3 4 172.18 6.30 -10 -3 -4 171.08 7.80 -10 3 -5 44.50 3.80 10 3 5 44.40 3.40 10 -3 5 45.70 2.70 -10 -3 -5 48.80 4.00 -10 -4 6 16.20 2.30 -10 -4 6 18.80 2.50 -10 -4 6 12.00 4.30 -10 -4 5 10.20 2.40 -10 -4 5 5.30 3.70 -10 -4 4 8.70 4.90 -10 -4 4 12.10 2.50 -10 -4 4 9.90 2.70 -10 4 3 184.38 15.50 -10 -4 3 201.88 9.00 -10 -4 3 202.48 16.90 -10 -4 3 180.48 10.80 -10 -4 3 171.98 17.50 -10 4 2 26.80 7.50 -10 -4 2 26.60 7.60 -10 -4 2 27.10 5.30 -10 -4 2 30.90 4.10 -10 4 1 306.47 21.50 -10 -4 1 329.07 12.60 -10 -4 1 308.47 21.60 -10 4 0 65.89 11.70 -10 -4 0 85.89 12.10 -10 -4 0 73.79 5.70 10 4 1 41.20 4.20 -10 4 -1 49.00 10.60 10 -4 1 45.20 3.60 -10 -4 -1 39.90 9.60 -10 4 -2 352.66 22.20 10 4 2 329.37 12.10 -10 -4 -2 318.77 20.70 10 -4 2 345.97 10.80 10 4 3 -0.60 1.60 10 -4 3 2.70 1.60 -10 4 -4 291.77 10.80 10 4 4 304.97 10.60 10 -4 4 309.27 9.50 -10 -4 -4 306.67 11.10 -10 4 -5 34.80 4.20 10 4 5 44.10 3.20 10 -4 5 34.00 2.40 -10 -4 -5 35.00 3.60 -10 -5 6 71.59 4.50 -10 -5 5 107.59 5.40 -10 -5 5 88.89 10.70 -10 -5 4 12.70 2.40 -10 -5 4 7.90 4.40 -10 5 3 129.19 12.60 -10 -5 3 130.79 14.70 -10 -5 3 138.89 13.80 -10 -5 3 139.29 7.10 -10 5 2 106.29 12.30 -10 -5 2 115.79 6.60 -10 -5 2 103.39 12.70 -10 5 1 89.39 12.20 -10 -5 1 92.99 12.00 -10 -5 1 93.79 6.10 -10 5 0 37.90 8.80 10 5 0 35.80 3.70 -10 -5 0 43.30 9.20 10 5 1 156.98 7.50 -10 5 -1 176.18 15.90 10 -5 1 159.28 6.20 -10 -5 -1 155.68 14.90 -10 5 -2 23.00 7.60 10 5 2 22.50 3.20 10 -5 2 19.80 2.60 10 5 3 0.90 1.70 10 -5 3 -0.50 1.40 -10 5 -4 2.50 1.70 10 5 4 0.70 1.30 10 -5 4 1.20 1.30 -10 -5 -4 -0.70 1.50 10 5 5 3.00 1.50 -10 -6 5 0.70 1.20 -10 -6 4 33.20 3.30 -10 -6 4 22.50 5.90 -10 -6 3 44.10 8.80 -10 -6 3 56.69 9.00 -10 -6 3 49.00 4.10 -10 6 2 9.70 5.20 -10 -6 2 9.50 5.30 -10 -6 2 8.10 2.20 -10 6 1 4.00 4.30 -10 -6 1 5.10 2.00 -10 -6 1 3.80 4.00 -10 6 0 48.40 9.20 10 6 0 46.70 3.90 -10 -6 0 48.70 9.20 -10 6 -1 113.39 12.60 10 6 1 115.79 6.00 10 -6 1 118.69 4.90 -10 -6 -1 119.09 12.40 10 6 2 21.90 2.90 -10 6 -2 30.40 7.80 10 -6 2 26.70 2.70 10 6 3 3.10 1.50 10 -6 3 0.30 1.30 10 6 4 -0.40 1.10 10 -6 4 -0.20 1.10 -10 -7 4 54.99 4.50 -10 -7 3 15.60 2.30 -10 -7 3 14.20 5.00 -10 -7 3 9.70 4.10 -10 7 2 74.99 9.10 -10 -7 2 82.09 10.10 -10 7 1 63.29 9.20 10 7 -1 54.49 3.80 -10 -7 1 45.90 8.50 10 7 0 8.60 2.10 -10 7 0 8.50 4.50 -10 -7 0 9.20 4.50 -10 7 -1 154.08 13.20 10 7 1 160.38 6.70 -10 -7 -1 152.98 12.50 -10 7 -2 150.78 12.00 10 7 2 131.69 6.00 10 -7 2 145.19 5.00 10 7 3 97.79 4.60 10 -7 3 112.99 5.20 -10 -8 2 1.20 2.80 -10 8 1 16.10 4.60 10 8 -1 23.00 2.50 -10 -8 1 19.10 5.00 -10 8 0 199.58 13.20 10 8 0 197.28 7.00 -10 -8 0 193.58 12.70 -10 8 -1 4.80 3.50 -11 0 3 -0.50 3.40 -11 0 2 25.70 7.60 -11 0 1 -0.30 3.60 -11 0 0 105.99 13.10 -11 0 -1 -0.40 4.00 -11 0 -2 383.16 22.30 -11 -1 6 80.49 4.00 -11 -1 5 70.69 4.40 -11 1 3 33.30 8.00 -11 -1 3 35.00 8.10 -11 1 2 82.79 11.50 -11 -1 2 87.19 11.70 -11 1 1 31.00 8.30 -11 -1 1 34.40 8.30 -11 1 0 42.80 9.40 -11 -1 0 46.60 10.10 -11 1 -1 47.70 9.90 -11 -1 -1 51.39 10.00 -11 1 -2 1.80 4.20 -11 -1 -2 0.90 4.00 -11 -2 5 4.40 1.80 -11 -2 5 0.50 1.30 -11 -2 4 42.30 3.90 -11 2 3 29.40 7.40 -11 -2 3 31.90 7.60 -11 2 2 25.30 7.20 -11 -2 2 30.40 3.90 -11 -2 2 29.80 8.20 -11 2 1 1.10 4.10 -11 -2 1 -0.60 3.30 -11 -2 1 0.60 1.80 11 2 0 23.10 3.10 -11 2 0 21.80 7.30 -11 -2 0 21.80 7.00 11 2 1 77.29 5.00 -11 2 -1 91.29 12.40 -11 -2 -1 78.49 11.20 -11 2 -2 145.29 14.00 -11 -2 -2 150.88 13.70 -11 -3 5 6.70 1.80 -11 -3 5 5.30 3.40 -11 -3 4 3.60 1.70 -11 3 3 147.69 13.50 -11 -3 3 155.38 7.50 -11 -3 3 172.78 14.80 -11 3 2 17.40 6.00 -11 -3 2 20.00 6.60 -11 -3 2 21.10 3.30 -11 3 1 0.00 3.60 -11 -3 1 -0.60 3.20 -11 -3 1 0.20 1.70 -11 3 0 110.19 12.90 11 3 0 108.29 5.70 -11 -3 0 97.79 12.20 -11 3 -1 130.89 13.60 11 3 1 130.19 6.50 -11 -3 -1 129.19 13.40 -11 3 -2 48.40 9.30 11 3 2 51.39 4.00 -11 -3 -2 45.80 8.80 11 3 3 2.30 1.60 11 3 4 0.10 1.40 -11 -4 5 4.50 1.50 -11 -4 4 0.70 1.30 -11 4 3 5.60 4.10 -11 -4 3 3.70 1.80 -11 -4 3 4.30 4.10 -11 4 2 15.80 5.80 -11 -4 2 15.40 5.80 -11 -4 2 17.50 2.90 -11 4 1 144.59 14.10 -11 -4 1 156.48 14.60 -11 -4 1 152.68 7.60 -11 4 0 191.48 15.90 11 4 0 183.68 7.80 -11 -4 0 181.88 15.70 11 4 1 6.30 2.10 -11 4 -1 3.10 4.30 -11 -4 -1 8.10 4.90 11 4 2 39.80 3.70 -11 4 -2 51.69 8.90 11 4 3 46.60 3.70 11 4 4 3.20 1.50 -11 -5 4 9.30 4.80 -11 -5 4 11.00 2.00 -11 -5 3 14.60 5.30 -11 -5 3 13.90 2.40 -11 5 2 14.70 5.20 -11 -5 2 19.80 2.80 -11 -5 2 13.50 5.40 11 5 -1 19.90 2.90 -11 5 1 18.60 6.10 -11 -5 1 16.40 6.00 -11 5 0 78.39 10.40 11 5 0 77.69 4.80 -11 -5 0 71.29 10.50 11 5 1 6.00 2.00 -11 5 -1 6.20 4.60 -11 -5 -1 3.80 4.20 -11 5 -2 47.80 8.40 11 5 2 46.40 3.70 11 5 3 2.30 1.40 -11 -6 3 4.10 1.50 -11 -6 3 1.60 3.10 -11 6 2 10.10 4.20 11 6 -2 17.10 2.40 -11 -6 2 15.90 5.20 -11 6 1 10.60 4.60 11 6 -1 13.00 2.30 -11 -6 1 13.60 5.00 11 6 0 19.60 2.70 -11 6 0 16.40 5.30 -11 -6 0 19.60 5.70 -11 6 -1 113.89 10.80 11 6 1 129.39 5.60 -11 -6 -1 112.99 10.60 -11 6 -2 49.10 7.50 11 6 2 59.79 3.70 11 7 -1 17.00 2.20 -11 7 1 11.60 4.00 -11 -7 1 13.40 4.40 -11 7 0 3.90 3.10 11 7 0 3.40 1.40 -11 -7 0 0.30 2.90 -12 0 3 3.50 3.60 -12 0 2 12.00 5.00 -12 0 1 -0.10 3.50 -12 0 0 176.68 15.00 -12 0 -1 1.20 3.40 -12 0 -2 2.20 3.60 -12 1 3 6.40 3.90 -12 -1 3 6.90 4.20 -12 1 2 13.50 5.40 -12 -1 2 14.30 5.40 -12 1 1 159.48 14.20 -12 -1 1 154.08 14.00 -12 1 0 -0.40 3.40 -12 -1 0 -1.20 3.00 -12 1 -1 0.70 3.20 -12 -1 -1 0.40 3.20 -12 1 -2 25.10 6.20 -12 -1 -2 22.80 6.10 -12 2 3 9.40 4.40 -12 -2 3 11.60 4.90 -12 2 2 43.10 8.10 -12 -2 2 45.40 8.50 -12 2 1 -0.90 3.30 -12 -2 1 1.00 3.30 -12 2 0 72.89 10.00 -12 -2 0 83.69 10.50 -12 2 -1 55.29 8.90 -12 -2 -1 49.40 8.80 -12 2 -2 61.09 8.60 -12 -3 4 1.70 1.20 -12 3 3 5.20 3.50 -12 -3 3 6.20 1.70 -12 -3 3 5.70 3.80 -12 3 2 25.30 6.30 -12 -3 2 23.00 6.30 12 3 -1 152.98 6.50 -12 3 1 156.58 13.50 -12 -3 1 148.09 13.30 -12 3 0 -0.10 3.50 12 3 0 -1.80 1.40 -12 -3 0 -1.30 3.10 12 3 1 45.70 3.60 -12 3 -1 56.89 8.60 -12 -3 -1 47.40 8.30 12 3 2 0.00 1.10 -12 3 -2 14.90 5.00 -12 -4 3 1.20 2.90 -12 -4 3 1.20 1.20 12 4 -2 33.50 3.00 -12 4 2 40.50 7.00 -12 -4 2 34.00 7.50 -12 4 1 76.29 9.60 12 4 -1 76.29 4.50 -12 -4 1 79.09 9.70 -12 4 0 4.00 3.80 12 4 0 3.20 1.70 -12 -4 0 3.00 3.50 -12 4 -1 28.40 6.30 12 4 1 27.90 2.80 -12 -4 -1 25.20 6.20 12 4 2 1.40 1.30 -12 4 -2 1.60 2.90 -12 5 2 1.70 2.70 12 5 -2 2.50 1.40 -12 -5 2 -0.30 2.70 12 5 -1 -2.40 1.20 -12 5 1 -0.90 2.70 -12 -5 1 -0.70 2.70 12 5 0 -3.00 1.20 -12 5 0 1.10 2.80 -12 -5 0 0.10 2.90 12 5 1 77.59 4.10 -12 5 -1 83.19 8.60 -13 0 2 8.60 4.00 -13 0 1 2.20 2.90 -13 0 0 592.24 25.50 -13 0 -1 1.50 3.20 -13 1 2 57.99 7.70 -13 -1 2 62.79 8.10 -13 1 1 13.40 4.50 -13 -1 1 15.70 5.00 -13 1 0 12.50 4.60 -13 -1 0 11.50 4.60 -13 1 -1 9.70 4.10 -13 -1 -1 11.00 4.40 -13 2 2 8.80 3.70 -13 -2 2 5.10 3.40 -13 2 1 -0.80 2.70 -13 -2 1 -0.60 2.70 -13 2 0 42.70 7.10 -13 -2 0 47.50 7.50 -13 2 -1 8.00 3.60 -13 -2 -1 4.50 4.10 -13 -3 2 0.70 3.00 -13 3 1 -0.40 2.30 -13 -3 1 -0.20 2.30 -13 3 0 56.19 7.20 -13 -3 0 56.99 7.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 43735 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 0.50503(9) 0.66664(10) 0.81742(11) 0.0239(3) Uani 1 1 d . . N1 N 0.65006(10) 0.58995(12) 0.99075(13) 0.0194(3) Uani 1 1 d . . C1 C 0.57115(12) 0.57726(14) 0.86266(15) 0.0182(3) Uani 1 1 d . . C2 C 0.57264(12) 0.44674(14) 0.77859(15) 0.0189(3) Uani 1 1 d . . H2A H 0.5001 0.4389 0.7076 0.023 Uiso 1 1 calc R U H2B H 0.5713 0.3752 0.8571 0.023 Uiso 1 1 calc R U C3 C 0.69416(13) 0.72177(15) 1.03069(16) 0.0243(4) Uani 1 1 d . . H3A H 0.7026 0.7322 1.1464 0.029 Uiso 1 1 calc R U H3B H 0.6371 0.7884 0.9878 0.029 Uiso 1 1 calc R U C4 C 0.81234(13) 0.74128(15) 0.96243(16) 0.0232(4) Uani 1 1 d . . H4 H 0.8452 0.8271 0.9630 0.028 Uiso 1 1 calc R U C5 C 0.87316(13) 0.64412(15) 0.90127(15) 0.0222(3) Uani 1 1 d . . H5 H 0.9438 0.6653 0.8519 0.027 Uiso 1 1 calc R U C6 C 0.83551(13) 0.50092(14) 0.90623(15) 0.0199(3) Uani 1 1 d . . H6 H 0.9057 0.4488 0.9479 0.024 Uiso 1 1 calc R U C7 C 0.74024(13) 0.48935(14) 1.02385(15) 0.0207(3) Uani 1 1 d . . H7A H 0.7034 0.4012 1.0161 0.025 Uiso 1 1 calc R U H7B H 0.7762 0.5006 1.1320 0.025 Uiso 1 1 calc R U C8 C 0.79880(12) 0.44848(13) 0.74170(15) 0.0176(3) Uani 1 1 d . . C9 C 0.68104(12) 0.42993(13) 0.68294(15) 0.0172(3) Uani 1 1 d . . C10 C 0.66040(13) 0.38748(14) 0.52719(15) 0.0196(3) Uani 1 1 d . . H10 H 0.5809 0.3771 0.4855 0.024 Uiso 1 1 calc R U C11 C 0.75225(14) 0.36015(14) 0.43218(16) 0.0225(3) Uani 1 1 d . . H11 H 0.7357 0.3323 0.3266 0.027 Uiso 1 1 calc R U C12 C 0.86838(14) 0.37372(14) 0.49220(17) 0.0238(4) Uani 1 1 d . . H12 H 0.9323 0.3527 0.4294 0.029 Uiso 1 1 calc R U C13 C 0.89039(13) 0.41844(14) 0.64528(17) 0.0214(3) Uani 1 1 d . . H13 H 0.9702 0.4289 0.6855 0.026 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 0.0247(6) 0.0203(6) 0.0265(5) -0.0005(4) -0.0001(4) 0.0045(4) N1 0.0229(7) 0.0175(7) 0.0177(5) -0.0017(5) 0.0015(4) -0.0005(5) C1 0.0179(8) 0.0185(8) 0.0187(6) 0.0002(6) 0.0049(5) -0.0018(6) C2 0.0175(8) 0.0184(8) 0.0205(7) -0.0006(6) -0.0006(5) -0.0015(6) C3 0.0282(9) 0.0209(8) 0.0234(7) -0.0050(6) -0.0013(6) -0.0012(6) C4 0.0262(9) 0.0199(8) 0.0227(7) -0.0007(6) -0.0056(6) -0.0045(6) C5 0.0208(8) 0.0245(8) 0.0206(7) 0.0004(6) -0.0033(5) -0.0036(6) C6 0.0189(8) 0.0204(8) 0.0198(6) 0.0011(6) -0.0042(5) 0.0018(6) C7 0.0257(8) 0.0202(8) 0.0159(6) 0.0000(6) -0.0022(5) 0.0003(6) C8 0.0216(8) 0.0111(7) 0.0199(7) 0.0030(5) -0.0005(5) 0.0007(5) C9 0.0216(8) 0.0106(7) 0.0192(7) 0.0018(5) 0.0006(5) 0.0003(5) C10 0.0241(8) 0.0138(8) 0.0206(7) 0.0023(6) -0.0020(5) -0.0020(6) C11 0.0340(9) 0.0156(8) 0.0179(6) 0.0006(6) 0.0025(6) -0.0019(6) C12 0.0282(9) 0.0177(8) 0.0265(7) 0.0023(6) 0.0098(6) 0.0008(6) C13 0.0194(8) 0.0173(8) 0.0276(7) 0.0031(6) 0.0012(6) -0.0001(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C1 N1 C7 119.86(12) C1 N1 C3 117.76(12) C7 N1 C3 112.10(11) O1 C1 N1 122.22(13) O1 C1 C2 122.03(12) N1 C1 C2 115.74(12) C1 C2 C9 112.72(11) C1 C2 H2A 109.0 C9 C2 H2A 109.0 C1 C2 H2B 109.0 C9 C2 H2B 109.0 H2A C2 H2B 107.8 N1 C3 C4 109.18(12) N1 C3 H3A 109.8 C4 C3 H3A 109.8 N1 C3 H3B 109.8 C4 C3 H3B 109.8 H3A C3 H3B 108.3 C5 C4 C3 123.14(14) C5 C4 H4 118.4 C3 C4 H4 118.4 C4 C5 C6 123.43(14) C4 C5 H5 118.3 C6 C5 H5 118.3 C7 C6 C5 107.66(12) C7 C6 C8 114.47(12) C5 C6 C8 111.64(11) C7 C6 H6 107.6 C5 C6 H6 107.6 C8 C6 H6 107.6 N1 C7 C6 109.40(11) N1 C7 H7A 109.8 C6 C7 H7A 109.8 N1 C7 H7B 109.8 C6 C7 H7B 109.8 H7A C7 H7B 108.2 C13 C8 C9 118.77(12) C13 C8 C6 116.59(12) C9 C8 C6 124.64(12) C10 C9 C8 118.45(13) C10 C9 C2 116.79(12) C8 C9 C2 124.71(12) C11 C10 C9 122.03(14) C11 C10 H10 119.0 C9 C10 H10 119.0 C12 C11 C10 119.43(13) C12 C11 H11 120.3 C10 C11 H11 120.3 C11 C12 C13 119.26(14) C11 C12 H12 120.4 C13 C12 H12 120.4 C12 C13 C8 122.00(14) C12 C13 H13 119.0 C8 C13 H13 119.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.2242(17) N1 C1 1.3704(17) N1 C7 1.4595(18) N1 C3 1.4648(18) C1 C2 1.5110(19) C2 C9 1.5224(19) C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.502(2) C3 H3A 0.9900 C3 H3B 0.9900 C4 C5 1.330(2) C4 H4 0.9500 C5 C6 1.521(2) C5 H5 0.9500 C6 C7 1.5204(19) C6 C8 1.5326(18) C6 H6 1.0000 C7 H7A 0.9900 C7 H7B 0.9900 C8 C13 1.3949(19) C8 C9 1.4034(19) C9 C10 1.4011(18) C10 C11 1.384(2) C10 H10 0.9500 C11 C12 1.384(2) C11 H11 0.9500 C12 C13 1.389(2) C12 H12 0.9500 C13 H13 0.9500