#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:31:11 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227280 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035868.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_4035868 loop_ _publ_author_name 'Dumonteil, Geoffrey' 'Bhattacharjee, Nicholus' 'Angelici, Gaetano' 'Roy, Olivier' 'Faure, Sophie' 'Jouffret, Laurent' 'Jolibois, Franck' 'Perrin, Lionel' 'Taillefumier, Claude' _publ_section_title ; Exploring the Conformation of Mixed Cis- Trans \a,\b-Oligopeptoids: A Joint Experimental and Computational Study. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6382 _journal_page_last 6396 _journal_paper_doi 10.1021/acs.joc.8b00606 _journal_volume 83 _journal_year 2018 _chemical_formula_sum 'C19 H28 N2 O4' _chemical_formula_weight 348.43 _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 108.830(17) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.322(12) _cell_length_b 5.730(4) _cell_length_c 19.274(13) _cell_measurement_reflns_used 706 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 39.70 _cell_measurement_theta_min 6.641 _cell_volume 1915(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1359 _diffrn_reflns_av_unetI/netI 0.1864 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 6655 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.210 _diffrn_reflns_theta_max 25.210 _diffrn_reflns_theta_min 3.727 _diffrn_source molybdene _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7270 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.208 _exptl_crystal_description platelet _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.914 _exptl_crystal_size_mid 0.291 _exptl_crystal_size_min 0.076 _refine_diff_density_max 0.304 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.082 _refine_ls_extinction_coef 0.068(10) _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 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 2355 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.1810 _refine_ls_R_factor_gt 0.0978 _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^)+(0.1311P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2205 _refine_ls_wR_factor_ref 0.2674 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1233 _reflns_number_total 2355 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00606_si_002.cif _cod_data_source_block 2018_GD155 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4035868 _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 ; 2018_GD155.res created by SHELXL-2014/7 TITL 2018_GD155_a.res in P2(1)/n CELL 0.71073 18.3216 5.7300 19.2739 90.000 108.830 90.000 ZERR 4.00 0.0123 0.0039 0.0129 0.000 0.017 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 76 112 8 16 LIST 6 TEMP -173.150 ACTA L.S. 10 FMAP 2 PLAN 5 omit -2 0 2 omit 2 0 0 omit 1 0 1 omit -1 0 1 omit 0 0 2 WGHT 0.131100 EXTI 0.068269 FVAR 0.88632 O1 4 0.727241 0.845755 0.930718 11.00000 0.04703 0.04147 = 0.05139 -0.00401 -0.00728 0.01215 O2 4 0.674767 0.570631 0.846991 11.00000 0.05701 0.02815 = 0.05421 -0.00078 -0.00211 0.00615 O3 4 0.465168 0.684100 0.689787 11.00000 0.04097 0.02659 = 0.03670 -0.00773 -0.00315 -0.00616 O4 4 0.504519 0.216373 0.916702 11.00000 0.04574 0.02296 = 0.04027 -0.00041 0.00068 0.00065 N1 3 0.567935 0.893225 0.761713 11.00000 0.03365 0.02218 = 0.02832 0.00363 -0.00708 -0.00670 N2 3 0.399280 0.430133 0.860867 11.00000 0.03419 0.02167 = 0.03720 -0.00108 0.00200 -0.00040 C1 1 0.861499 0.824084 1.000195 11.00000 0.04925 0.11031 = 0.06717 -0.00551 0.00422 0.01775 AFIX 137 H1 2 0.878325 0.865116 0.958375 11.00000 -1.50000 H3 2 0.901331 0.729500 1.035005 11.00000 -1.50000 H28 2 0.852962 0.966916 1.024468 11.00000 -1.50000 AFIX 0 C2 1 0.788005 0.687734 0.973827 11.00000 0.06533 0.06845 = 0.04826 0.01994 0.00288 0.02205 AFIX 23 H26 2 0.793869 0.555049 0.943153 11.00000 -1.20000 H27 2 0.774594 0.625228 1.016052 11.00000 -1.20000 AFIX 0 C3 1 0.674618 0.764216 0.870185 11.00000 0.04374 0.02818 = 0.03904 -0.00637 0.00477 -0.00636 C4 1 0.615736 0.950674 0.836331 11.00000 0.03190 0.02230 = 0.03489 -0.00219 -0.00422 -0.00058 AFIX 23 H24 2 0.582153 0.972588 0.867052 11.00000 -1.20000 H25 2 0.642722 1.099984 0.835754 11.00000 -1.20000 AFIX 0 C5 1 0.505901 0.749949 0.751359 11.00000 0.03913 0.00799 = 0.03645 -0.00024 0.00352 0.00463 C6 1 0.487726 0.671672 0.818333 11.00000 0.03719 0.02170 = 0.03450 -0.00165 -0.00180 -0.00810 AFIX 23 H13 2 0.469875 0.807018 0.840448 11.00000 -1.20000 H23 2 0.535096 0.609936 0.854891 11.00000 -1.20000 AFIX 0 C7 1 0.425613 0.483324 0.799537 11.00000 0.03519 0.02607 = 0.03571 -0.00366 -0.00348 0.00158 AFIX 23 H21 2 0.381299 0.536443 0.757668 11.00000 -1.20000 H22 2 0.446445 0.339781 0.784342 11.00000 -1.20000 AFIX 0 C8 1 0.328588 0.533977 0.861360 11.00000 0.03363 0.01193 = 0.04114 0.00275 -0.00323 0.00003 C9 1 0.328744 0.728062 0.904280 11.00000 0.03341 0.02432 = 0.06925 -0.00719 0.00136 -0.00168 AFIX 43 H20 2 0.376229 0.793175 0.934000 11.00000 -1.20000 AFIX 0 C10 1 0.260792 0.825449 0.903841 11.00000 0.04684 0.02938 = 0.07438 -0.02824 0.01205 -0.01058 AFIX 43 H17 2 0.261262 0.962380 0.931771 11.00000 -1.20000 AFIX 0 C11 1 0.190925 0.727204 0.863129 11.00000 0.04334 0.02669 = 0.05270 0.00807 0.00856 0.00451 AFIX 43 H2 2 0.143609 0.792035 0.864288 11.00000 -1.20000 AFIX 0 C12 1 0.590452 0.970231 0.697237 11.00000 0.04449 0.01546 = 0.04902 -0.00094 0.00178 -0.00529 C13 1 0.606550 0.759477 0.656583 11.00000 0.05090 0.02040 = 0.04746 -0.00335 0.01134 -0.00368 AFIX 137 H6 2 0.645274 0.660143 0.690810 11.00000 -1.50000 H4 2 0.625916 0.811835 0.617364 11.00000 -1.50000 H5 2 0.558843 0.670515 0.635351 11.00000 -1.50000 AFIX 0 C14 1 0.664155 1.115804 0.721575 11.00000 0.04919 0.02688 = 0.05332 -0.00012 0.00799 -0.00548 AFIX 137 H7 2 0.655962 1.254254 0.747989 11.00000 -1.50000 H9 2 0.677558 1.164324 0.678445 11.00000 -1.50000 H8 2 0.706261 1.022286 0.753916 11.00000 -1.50000 AFIX 0 C15 1 0.526432 1.120980 0.647549 11.00000 0.04700 0.02279 = 0.05475 0.01109 0.00417 0.00276 AFIX 137 H10 2 0.479522 1.027212 0.627965 11.00000 -1.50000 H11 2 0.542317 1.180657 0.606966 11.00000 -1.50000 H12 2 0.516212 1.252190 0.675705 11.00000 -1.50000 AFIX 0 C16 1 0.443806 0.300945 0.918179 11.00000 0.02945 0.01107 = 0.03970 -0.00388 -0.00278 -0.00132 C17 1 0.416765 0.265577 0.981265 11.00000 0.04107 0.02173 = 0.04541 0.00171 0.00546 0.00114 AFIX 137 H14 2 0.447103 0.141609 1.012527 11.00000 -1.50000 H16 2 0.362229 0.220777 0.963927 11.00000 -1.50000 H15 2 0.422906 0.410727 1.009468 11.00000 -1.50000 AFIX 0 C18 1 0.191581 0.536132 0.821521 11.00000 0.03696 0.03657 = 0.04517 -0.00829 -0.00533 -0.00649 AFIX 43 H18 2 0.143961 0.470434 0.792339 11.00000 -1.20000 AFIX 0 C19 1 0.259226 0.435747 0.820585 11.00000 0.04949 0.01633 = 0.05357 -0.00417 0.00830 -0.00463 AFIX 43 H19 2 0.258337 0.299786 0.792115 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 2018_GD155_a.res in P2(1)/n REM R1 = 0.0978 for 1233 Fo > 4sig(Fo) and 0.1810 for all 2355 data REM 232 parameters refined using 0 restraints END WGHT 0.1311 0.0000 REM Highest difference peak 0.304, deepest hole -0.321, 1-sigma level 0.082 Q1 1 0.5398 0.1810 0.8706 11.00000 0.05 0.30 Q2 1 0.5650 0.8237 0.6718 11.00000 0.05 0.29 Q3 1 0.6792 0.8703 0.9677 11.00000 0.05 0.29 Q4 1 0.5205 0.6404 0.6643 11.00000 0.05 0.29 Q5 1 0.6798 0.6982 0.9482 11.00000 0.05 0.29 ; _shelx_res_checksum 69334 _shelx_hkl_file ; -1 0 0 -0.80 1.00 1 0 0 -0.50 1.20 1 0 0 -0.30 0.80 2 0 0 -1.60 5.50 -2 0 0 -2.80 4.60 -3 0 0 22.90 12.20 3 0 0 -3.00 12.30 -4 0 0 240.18 36.80 4 0 0 244.58 37.90 5 0 0 -7.30 20.50 -5 0 0 17.90 17.60 6 0 0 463.85 64.39 -6 0 0 408.36 61.79 -6 0 0 425.46 61.29 -7 0 0 140.69 31.30 -7 0 0 213.28 33.50 7 0 0 100.49 35.00 8 0 0 89.79 35.80 -8 0 0 81.09 29.30 -9 0 0 -17.40 25.50 -9 0 0 48.50 30.00 9 0 0 18.90 35.30 10 0 0 297.17 56.19 -10 0 0 277.67 48.10 -11 0 0 67.69 34.30 -11 0 0 21.80 26.80 11 0 0 45.90 37.90 12 0 0 1100.19 157.28 -12 0 0 1155.98 152.08 13 0 0 87.59 48.20 -13 0 0 16.90 30.60 -13 0 0 91.09 42.50 -14 0 0 117.49 39.30 14 0 0 138.99 59.29 15 0 0 123.49 61.49 -15 0 0 -15.00 34.90 -16 0 0 -73.59 56.79 16 0 0 37.40 62.89 -16 0 0 45.60 38.70 17 0 0 141.89 75.69 0 -1 0 -13.40 15.10 -1 -1 0 -8.60 13.30 -1 -1 0 -12.70 10.50 1 -1 0 -2.10 16.00 -1 1 0 -8.50 16.00 1 1 0 1.80 12.00 -2 -1 0 1747.93 218.08 2 1 0 1653.53 218.08 -3 -1 0 -4.80 16.60 3 1 0 13.40 19.40 -3 1 0 5.50 20.50 -4 -1 0 568.64 74.69 4 -1 0 511.95 76.59 -4 1 0 531.75 76.09 4 1 0 552.04 75.09 -5 -1 0 172.18 29.70 5 -1 0 228.48 34.00 5 -1 0 154.18 33.60 5 1 0 137.29 30.30 5 1 0 121.09 24.70 6 -1 0 30.50 29.40 -6 -1 0 48.90 22.50 6 -1 0 81.09 26.30 6 1 0 51.89 25.30 7 -1 0 326.27 60.39 -7 -1 0 332.47 55.79 7 -1 0 458.35 58.79 -7 1 0 409.16 59.59 -7 1 0 360.76 60.39 7 1 0 330.87 57.99 -8 -1 0 3037.10 398.36 8 -1 0 3219.78 400.36 8 -1 0 3195.58 399.16 -8 1 0 2900.21 399.56 8 1 0 3047.99 399.46 -8 1 0 3231.98 399.36 -9 -1 0 546.65 78.49 9 -1 0 528.15 81.89 9 -1 0 519.45 85.59 -9 1 0 571.84 81.39 9 1 0 569.14 83.29 -9 1 0 503.65 80.99 10 -1 0 1089.29 137.09 -10 -1 0 986.40 134.59 10 -1 0 1065.49 139.59 -10 1 0 1005.30 135.89 10 1 0 887.71 137.69 -11 -1 0 39.60 28.50 11 -1 0 111.49 38.00 11 -1 0 75.39 45.40 11 1 0 91.59 39.20 -11 1 0 77.89 31.70 12 -1 0 30.90 45.10 -12 -1 0 -10.20 27.20 -12 1 0 -3.30 41.20 -12 1 0 45.70 30.90 12 1 0 -11.00 40.20 13 -1 0 -24.60 48.60 -13 -1 0 -17.70 30.00 13 1 0 28.10 44.40 -13 1 0 0.10 31.70 14 -1 0 115.59 61.99 -14 -1 0 85.49 37.30 -14 1 0 73.79 39.30 14 1 0 182.68 57.99 15 -1 0 90.69 60.99 -15 -1 0 20.70 36.10 -15 1 0 60.29 37.60 15 1 0 47.40 58.09 16 -1 0 -40.10 73.79 -16 -1 0 54.19 40.50 16 1 0 10.20 58.99 -16 1 0 12.40 39.20 -16 1 0 -25.70 61.59 17 -1 0 -18.00 72.79 17 1 0 27.70 67.79 0 -2 0 3465.45 443.36 1 -2 0 295.17 48.20 -1 -2 0 307.77 47.10 2 -2 0 1263.97 170.98 -2 -2 0 1330.37 168.88 -3 -2 0 350.96 49.80 3 -2 0 270.27 52.39 3 2 0 351.96 51.69 -4 -2 0 2713.63 346.77 4 2 0 2691.83 347.47 -5 -2 0 74.49 26.50 5 2 0 11.60 30.80 6 -2 0 1700.83 214.68 6 -2 0 1478.25 213.58 -6 -2 0 1794.02 212.58 6 2 0 1667.13 213.18 -6 2 0 1452.75 214.98 -7 -2 0 58.39 27.70 7 -2 0 -14.60 37.70 7 2 0 59.59 31.50 8 -2 0 342.57 57.09 -8 -2 0 341.57 48.80 8 -2 0 290.07 52.59 8 2 0 171.08 43.40 -8 2 0 312.97 57.19 8 2 0 346.07 52.79 9 -2 0 26.50 31.80 -9 -2 0 -1.20 25.80 9 -2 0 35.00 41.30 9 2 0 -49.99 30.60 -9 2 0 3.30 37.50 -10 -2 0 38.10 28.10 10 -2 0 56.69 34.30 -10 -2 0 9.00 35.60 10 -2 0 12.60 40.80 10 2 0 11.70 35.90 -10 2 0 10.60 41.00 -11 -2 0 95.89 40.90 11 -2 0 74.69 39.30 11 -2 0 224.78 53.39 -11 -2 0 68.69 31.60 11 2 0 68.39 40.30 -11 2 0 69.99 49.70 12 -2 0 -2.00 52.69 12 -2 0 1.70 37.10 -12 -2 0 13.60 30.60 12 2 0 33.30 41.10 13 -2 0 116.29 59.49 13 -2 0 98.79 46.80 -13 -2 0 76.89 37.50 -13 2 0 85.19 59.19 13 2 0 59.89 47.60 14 -2 0 96.29 65.99 14 -2 0 70.99 47.20 -14 -2 0 27.30 37.60 14 2 0 67.39 29.50 14 2 0 76.09 52.89 15 -2 0 -27.30 53.79 -15 -2 0 12.60 40.00 15 -2 0 -63.09 69.09 15 2 0 15.20 29.80 15 2 0 -37.90 53.49 16 -2 0 70.09 78.19 16 2 0 17.30 31.40 16 2 0 -24.90 60.49 -16 2 0 -90.79 70.59 0 -3 0 -21.40 33.00 -1 -3 0 76.09 25.70 1 -3 0 23.30 34.20 -2 -3 0 258.07 43.10 2 -3 0 217.58 48.70 -3 -3 0 400.06 60.49 -4 -3 0 101.59 26.80 4 -3 0 84.59 35.30 -4 -3 0 86.19 32.40 -5 -3 0 308.27 55.79 -5 -3 0 361.66 54.79 5 -3 0 363.96 58.29 5 3 0 335.27 56.19 6 -3 0 22.00 31.30 -6 -3 0 -28.10 31.70 -6 -3 0 53.59 25.60 6 3 0 8.60 30.60 -7 -3 0 187.38 36.10 7 -3 0 169.18 44.70 7 -3 0 105.39 41.60 -7 -3 0 141.09 41.20 7 3 0 167.78 41.50 8 -3 0 118.39 39.30 8 -3 0 191.68 48.20 8 -3 0 115.09 43.80 8 -3 0 125.89 55.49 -8 -3 0 193.88 36.80 -8 -3 0 145.29 42.40 8 3 0 132.49 40.50 -9 -3 0 64.29 39.80 9 -3 0 25.30 52.09 9 -3 0 102.79 48.20 9 -3 0 75.69 34.10 -9 -3 0 61.59 30.50 9 -3 0 57.09 43.60 9 3 0 53.49 37.50 -10 -3 0 11.90 42.50 -10 -3 0 -27.40 29.20 10 -3 0 5.30 32.60 10 -3 0 39.60 47.50 10 -3 0 -24.10 53.69 10 -3 0 -14.90 39.10 -10 3 0 -28.30 55.49 10 3 0 -15.20 38.10 11 -3 0 -25.90 40.30 11 -3 0 -23.60 54.79 11 -3 0 -8.20 54.39 -11 -3 0 -23.00 32.30 11 -3 0 -4.00 35.80 11 3 0 -81.69 39.30 -11 3 0 -54.49 56.89 12 -3 0 -63.99 39.80 12 -3 0 -20.30 57.59 -12 -3 0 -38.30 33.70 12 -3 0 -49.30 61.79 -12 3 0 -4.40 59.29 12 3 0 56.69 44.40 13 -3 0 421.56 81.19 13 -3 0 304.67 85.49 13 -3 0 210.68 58.59 -13 -3 0 234.38 52.49 13 3 0 168.98 44.50 13 3 0 212.48 59.09 -13 3 0 279.27 79.19 14 -3 0 2.20 66.69 14 -3 0 -17.40 78.69 -14 -3 0 39.30 40.40 14 3 0 77.19 50.79 -14 3 0 22.60 73.29 15 -3 0 42.30 82.79 15 3 0 71.99 57.69 0 -4 0 843.12 106.19 0 -4 0 845.52 110.89 0 -4 0 598.44 102.39 -1 -4 0 147.29 34.00 -1 -4 0 160.68 33.10 1 -4 0 110.19 40.60 -1 -4 0 70.29 37.60 2 -4 0 29.80 36.20 -2 -4 0 42.10 27.10 -2 -4 0 -36.50 31.80 -2 -4 0 8.10 23.70 -3 -4 0 30.50 33.40 -3 -4 0 57.19 27.30 3 -4 0 102.69 39.10 3 -4 0 86.29 55.09 -3 -4 0 50.59 29.80 4 -4 0 224.48 63.19 -4 -4 0 173.28 42.40 -4 -4 0 183.68 39.00 4 -4 0 213.98 48.20 -4 -4 0 168.38 41.30 -5 -4 0 1.50 25.20 -5 -4 0 -38.30 33.20 5 -4 0 105.69 58.29 5 -4 0 -29.80 36.80 6 -4 0 154.78 46.60 6 -4 0 238.58 64.49 -6 -4 0 123.09 34.50 -6 -4 0 112.79 44.00 -7 -4 0 91.79 33.90 7 -4 0 106.49 44.40 -7 -4 0 103.89 31.60 -7 -4 0 93.79 44.60 7 -4 0 141.29 62.79 7 4 0 44.90 28.50 8 -4 0 102.39 43.20 8 -4 0 93.39 63.09 -8 -4 0 77.19 32.00 -8 -4 0 64.79 35.00 8 4 0 58.79 37.30 9 -4 0 78.19 80.39 9 -4 0 126.59 56.19 9 -4 0 204.28 60.09 9 -4 0 53.09 43.50 -9 -4 0 122.39 40.10 9 4 0 115.99 44.40 10 -4 0 823.12 106.29 10 -4 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49.50 11 -3 -14 57.99 52.59 -10 -3 14 57.69 50.39 10 -3 -14 166.38 84.39 10 -3 -14 52.09 50.39 9 -3 -14 -32.30 44.30 -9 -3 14 14.10 46.60 9 -3 -14 37.30 79.49 -9 3 14 -21.30 49.99 8 -3 -14 56.09 79.89 8 -3 -14 33.70 43.30 -8 -3 14 67.79 50.99 7 -3 -14 -0.10 40.40 -7 -3 14 -6.20 51.59 7 -3 -14 -95.99 74.79 -7 3 14 33.60 46.10 6 -3 -14 150.38 48.90 -6 -3 14 97.79 57.19 -6 3 14 177.78 53.49 5 -3 -14 19.40 41.50 -5 -3 14 84.39 55.69 -5 3 14 65.49 48.60 4 -3 -14 61.89 44.30 -4 3 14 45.00 48.80 3 -3 -14 118.59 47.70 -2 -3 14 54.39 67.89 -1 -3 14 231.28 79.89 0 -3 14 676.03 123.59 -2 -3 -14 110.99 41.80 2 3 14 191.18 43.20 9 -4 -14 152.18 46.10 8 -4 -14 51.69 39.40 7 -4 -14 113.29 39.80 6 -4 -14 0.80 35.10 5 -4 -14 65.89 35.90 4 -4 -14 29.90 34.10 3 -4 -14 77.69 37.00 3 4 -14 37.90 68.49 2 -4 -14 4.60 33.50 1 -4 -14 21.90 34.90 0 -4 -14 -4.40 37.50 19 0 -15 59.29 67.69 18 0 -15 -78.39 60.59 -18 0 15 20.10 33.70 -17 0 15 -27.90 32.60 17 0 -15 51.19 56.59 -16 0 15 -41.60 31.30 16 0 -15 23.60 56.59 15 0 -15 55.09 52.49 -15 0 15 30.30 31.70 -14 0 15 14.60 28.80 -13 0 15 35.60 29.30 -12 0 15 -6.70 25.90 -11 0 15 60.09 27.80 -10 0 15 15.00 24.20 2 0 15 -26.20 43.80 3 0 15 279.87 63.49 4 0 15 -9.50 38.60 5 0 15 -20.30 39.40 6 0 15 49.10 44.30 7 0 15 13.80 45.60 8 0 15 12.70 47.80 19 -1 -15 -13.30 63.79 -19 1 15 17.80 34.10 18 -1 -15 87.29 62.79 18 1 -15 29.00 68.69 -18 1 15 -35.50 32.00 17 -1 -15 -18.80 53.59 17 1 -15 5.00 58.99 -16 -1 15 18.30 36.60 16 1 -15 -41.00 34.10 -15 -1 15 29.10 36.90 -14 -1 15 0.60 35.70 -13 -1 15 8.80 33.90 -12 -1 15 73.69 34.70 -11 -1 15 19.10 31.40 -10 -1 15 1.10 27.80 -9 -1 15 34.50 29.00 -8 -1 15 -16.70 28.20 -7 -1 15 58.39 32.40 -6 -1 15 197.68 42.20 -5 -1 15 99.29 34.30 4 -1 15 76.89 54.39 4 1 15 57.99 36.30 5 -1 15 211.48 60.19 5 1 15 95.39 41.80 6 -1 15 12.10 57.99 6 1 15 111.39 42.00 7 -1 15 -14.70 49.80 7 1 15 1.60 40.50 8 -1 15 -40.70 56.89 8 1 15 -27.90 43.70 9 1 15 -7.50 47.50 10 1 15 -15.50 50.39 -18 2 15 -15.90 77.29 -17 2 15 25.20 75.89 -14 -2 15 -61.09 53.89 -13 -2 15 12.00 42.70 -12 -2 15 28.90 42.40 -11 -2 15 148.29 47.30 -10 -2 15 -4.30 39.50 10 -2 -15 11.30 42.90 9 -2 -15 17.00 40.60 -9 -2 15 16.80 35.40 -8 -2 15 -16.00 37.00 8 -2 -15 6.90 38.90 -7 -2 15 -67.59 41.00 7 -2 -15 -34.50 37.50 -6 -2 15 -43.10 40.80 6 -2 -15 -10.10 37.00 -5 -2 15 18.60 42.40 5 -2 -15 -8.20 38.10 4 -2 -15 114.99 42.30 7 2 15 -20.20 37.50 8 2 15 -50.09 37.90 9 2 15 59.39 46.80 10 2 15 -1.50 52.69 -15 3 15 226.38 86.09 12 -3 -15 -50.59 53.79 11 -3 -15 101.19 54.59 10 -3 -15 -62.59 45.10 10 -3 -15 59.99 85.19 9 -3 -15 3.40 81.99 -9 -3 15 -63.59 56.29 9 -3 -15 -49.99 43.40 8 -3 -15 -29.40 43.50 -8 -3 15 -45.30 48.80 8 -3 -15 -51.19 83.59 7 -3 -15 -73.19 41.80 -7 -3 15 -36.80 51.89 6 -3 -15 -21.50 41.40 -6 -3 15 5.40 53.79 -6 3 15 19.40 48.90 -5 -3 15 312.37 79.39 5 -3 -15 361.36 68.19 -5 3 15 395.26 71.59 4 -3 -15 62.09 45.50 -4 3 15 114.99 51.69 3 -3 -15 23.30 44.60 2 -3 -15 13.90 45.00 11 -4 -15 50.29 45.50 9 -4 -15 23.80 38.40 8 -4 -15 113.89 41.50 7 -4 -15 102.09 42.00 6 -4 -15 76.09 37.40 5 -4 -15 30.00 34.60 4 -4 -15 102.59 39.40 3 -4 -15 30.00 34.30 2 -4 -15 29.60 33.90 19 0 -16 -97.59 67.59 -18 0 16 47.60 37.20 18 0 -16 183.88 72.29 17 0 -16 -45.70 56.19 -17 0 16 -7.80 33.70 -16 0 16 -19.30 32.90 16 0 -16 17.00 34.00 -15 0 16 -46.90 29.70 -14 0 16 25.20 28.60 -13 0 16 -36.90 26.80 -12 0 16 -11.20 26.20 2 0 16 100.99 48.00 3 0 16 24.70 46.80 4 0 16 44.50 41.40 5 0 16 1.70 42.00 6 0 16 50.39 44.80 7 0 16 20.60 47.20 8 0 16 58.99 50.79 -19 1 16 -2.10 36.10 -18 1 16 13.80 33.70 18 1 -16 10.50 46.70 -16 -1 16 -17.90 39.20 -15 -1 16 -29.90 35.30 -14 -1 16 -25.40 31.80 -13 -1 16 -31.10 33.20 -12 -1 16 64.99 33.90 -11 -1 16 129.69 37.60 -10 -1 16 61.69 31.60 -9 -1 16 15.70 33.30 -8 -1 16 22.30 33.90 -7 -1 16 39.40 34.30 7 -1 -16 25.40 36.20 -6 -1 16 130.49 41.80 6 -1 -16 97.29 39.70 -5 -1 16 4.70 31.00 5 -1 -16 1.60 35.40 4 -1 16 217.08 62.59 4 1 16 143.29 43.90 5 -1 16 -1.90 52.99 6 -1 16 -38.30 47.70 6 1 16 1.50 38.60 7 -1 16 58.69 58.89 7 1 16 3.90 42.10 8 1 16 -30.30 42.50 9 1 16 12.40 47.90 -18 2 16 92.79 81.39 -13 -2 16 -31.60 40.10 12 -2 -16 70.29 52.29 -12 -2 16 126.29 46.90 11 -2 -16 -21.00 47.90 -11 -2 16 17.70 42.80 -10 -2 16 -19.50 35.90 10 -2 -16 3.10 43.10 -9 -2 16 63.99 46.60 9 -2 -16 50.99 42.40 -8 -2 16 -52.09 38.30 8 -2 -16 27.80 40.00 7 -2 -16 159.58 46.00 -7 -2 16 128.59 48.90 -6 -2 16 198.58 57.09 6 -2 -16 132.49 46.90 5 -2 -16 58.89 41.90 -5 -2 16 89.69 52.39 4 -2 -16 37.30 41.00 11 -3 -16 -46.50 58.89 10 -3 -16 36.90 49.00 9 -3 -16 -74.49 43.00 8 -3 -16 -127.19 86.99 8 -3 -16 -22.80 43.20 7 -3 -16 -78.59 43.20 6 -3 -16 -0.90 45.00 5 -3 -16 20.60 44.70 4 -3 -16 471.55 83.19 3 -3 -16 121.69 50.69 2 -3 -16 70.59 55.39 9 -4 -16 116.89 43.50 8 -4 -16 17.60 39.10 7 -4 -16 65.59 39.10 6 -4 -16 112.59 42.30 5 -4 -16 145.19 44.50 4 -4 -16 103.49 44.20 19 0 -17 79.19 68.19 -18 0 17 -1.50 36.10 18 0 -17 40.80 41.00 -17 0 17 24.10 34.60 -16 0 17 -23.80 32.60 -15 0 17 18.20 30.50 -14 0 17 10.30 28.80 -12 0 17 14.30 28.00 1 0 17 130.89 51.79 2 0 17 -7.00 46.50 3 0 17 63.39 42.90 4 0 17 -51.79 39.20 5 0 17 -13.30 42.20 6 0 17 10.90 45.50 7 0 17 22.90 47.10 -15 -1 17 -27.00 37.30 -14 -1 17 68.29 41.30 -13 -1 17 9.70 34.30 -12 -1 17 14.90 33.70 -11 -1 17 64.39 37.10 -10 -1 17 22.60 35.90 -9 -1 17 -12.60 29.20 -8 -1 17 43.00 37.50 8 -1 -17 1.60 38.60 -7 -1 17 15.20 38.60 7 -1 -17 73.79 39.40 6 -1 -17 94.59 39.90 -6 -1 17 81.49 38.30 -5 -1 17 94.69 49.50 5 -1 -17 72.99 40.10 4 -1 -17 145.49 45.10 4 -1 17 -5.10 54.59 5 -1 17 111.99 62.09 5 1 17 100.69 43.80 6 -1 17 -24.60 53.69 6 1 17 -27.10 38.70 7 1 17 43.50 45.20 8 1 17 51.69 48.90 15 -2 -17 -132.09 58.19 14 -2 -17 -43.80 57.79 12 -2 -17 -35.30 50.19 -12 -2 17 43.20 46.00 11 -2 -17 24.80 49.99 -11 -2 17 114.69 46.80 -10 -2 17 58.49 48.10 10 -2 -17 25.90 44.90 -9 -2 17 -8.80 44.30 9 -2 -17 -24.90 41.40 -8 -2 17 59.29 47.40 8 -2 -17 40.20 43.30 -7 -2 17 106.69 52.29 7 -2 -17 24.30 43.00 6 -2 -17 4.20 40.80 -6 -2 17 -51.09 48.50 -5 -2 17 196.98 61.89 5 -2 -17 112.89 49.50 4 -2 -17 36.30 42.80 3 -2 -17 -8.30 42.60 8 -3 -17 -26.70 47.20 7 -3 -17 124.19 53.19 6 -3 -17 79.29 51.99 -17 0 18 -35.50 34.70 -16 0 18 -24.90 34.80 -15 0 18 -28.70 30.90 -14 0 18 -28.70 30.50 1 0 18 25.80 48.70 2 0 18 89.19 51.99 3 0 18 -32.10 39.00 4 0 18 5.50 42.50 5 0 18 -43.50 41.00 6 0 18 63.79 49.90 -15 -1 18 -28.60 37.50 -14 -1 18 9.00 40.50 -13 -1 18 34.40 35.30 -12 -1 18 -15.70 34.80 -11 -1 18 9.50 39.20 -10 -1 18 193.98 49.50 -9 -1 18 48.10 38.00 8 -1 -18 37.00 41.40 -8 -1 18 -28.90 37.80 7 -1 -18 14.30 39.50 -7 -1 18 9.50 43.60 -6 -1 18 30.40 46.60 6 -1 -18 -17.00 37.20 5 -1 -18 50.19 40.50 -5 -1 18 115.09 51.59 4 -1 -18 85.19 42.60 3 -1 18 -9.80 56.19 4 -1 18 -35.90 58.39 6 1 18 -0.20 44.30 15 -2 -18 -195.78 58.89 14 -2 -18 -160.38 57.09 13 -2 -18 -103.69 51.79 12 -2 -18 -59.29 52.99 11 -2 -18 -34.50 50.79 -11 -2 18 31.00 50.79 10 -2 -18 22.10 46.00 -10 -2 18 36.20 48.60 9 -2 -18 -17.50 44.70 -9 -2 18 40.60 47.10 -8 -2 18 1.20 48.50 8 -2 -18 29.50 44.50 -7 -2 18 248.58 66.59 7 -2 -18 176.08 53.89 -6 -2 18 -14.30 54.49 6 -2 -18 147.59 48.80 -5 -2 18 -78.09 53.49 5 -2 -18 1.10 43.90 4 -2 -18 -61.49 43.90 3 -2 -18 38.30 47.10 14 -3 -18 116.19 43.80 -17 0 19 -48.90 39.40 -15 0 19 -5.90 29.10 0 0 19 51.99 52.49 1 0 19 13.90 48.80 2 0 19 1.10 41.00 3 0 19 35.30 41.30 4 0 19 17.30 42.70 5 0 19 11.40 45.10 -14 -1 19 -32.40 40.00 -13 -1 19 5.80 41.00 -12 -1 19 -17.90 41.30 -11 -1 19 -7.80 40.90 -10 -1 19 7.10 39.70 -9 -1 19 75.09 44.00 9 -1 -19 24.60 42.20 -8 -1 19 0.20 42.40 8 -1 -19 29.40 40.60 7 -1 -19 -57.79 38.70 -7 -1 19 -32.40 43.00 6 -1 -19 3.10 40.60 -6 -1 19 -38.40 46.10 -5 -1 19 72.29 52.39 5 -1 -19 69.29 46.80 4 -1 -19 94.99 49.40 3 -1 19 -0.20 58.99 15 -2 -19 -104.09 63.79 14 -2 -19 -179.78 55.49 13 -2 -19 -84.99 54.49 12 -2 -19 -76.49 52.19 11 -2 -19 -17.70 49.10 10 -2 -19 -38.80 46.30 9 -2 -19 2.00 50.49 -8 -2 19 42.60 50.79 8 -2 -19 -4.00 46.10 -7 -2 19 57.19 56.09 7 -2 -19 38.40 46.10 6 -2 -19 -23.10 52.19 -6 -2 19 -4.90 54.49 5 -2 -19 10.20 58.99 -5 -2 19 49.50 58.39 4 -2 -19 76.19 51.49 3 -2 -19 17.40 48.20 2 -2 -19 43.00 53.89 5 0 -20 6.40 39.10 1 0 20 -38.70 48.80 2 0 20 15.00 43.00 3 0 20 4.50 42.10 4 0 20 80.69 50.29 -14 -1 20 16.80 46.90 -13 -1 20 -8.30 38.70 -12 -1 20 -18.10 42.60 -11 -1 20 70.09 45.10 -9 -1 20 -21.60 45.00 9 -1 -20 56.09 54.39 -8 -1 20 -20.20 55.29 8 -1 -20 -11.40 44.10 7 -1 -20 4.70 42.60 -7 -1 20 35.60 58.69 -6 -1 20 33.00 52.29 6 -1 -20 62.99 46.20 -5 -1 20 -19.60 52.19 5 -1 -20 -22.10 43.80 4 -1 -20 -6.90 54.59 3 -1 -20 112.79 50.49 2 -1 20 13.20 52.79 13 -2 -20 -87.39 64.29 12 -2 -20 -50.19 55.69 11 -2 -20 -72.69 50.49 10 -2 -20 13.40 66.29 9 -2 -20 -4.30 48.60 8 -2 -20 -13.10 44.70 7 -2 -20 37.90 49.80 5 -2 -20 -7.80 48.40 -13 -1 21 -9.00 46.30 -12 -1 21 -99.29 41.70 -11 -1 21 44.50 48.60 -9 -1 21 103.59 53.89 -8 -1 21 -18.60 54.89 -7 -1 21 54.39 60.29 -6 -1 21 -27.70 51.59 6 -1 -21 -14.20 44.10 5 -1 -21 -28.60 54.19 -5 -1 21 10.20 56.79 4 -1 -21 -12.90 50.29 3 -1 -21 153.88 57.49 10 -2 -21 7.60 49.99 9 -2 -21 -57.89 66.39 8 -2 -21 -37.60 50.49 7 -2 -21 -20.00 51.09 -9 -1 22 -45.90 45.20 -8 -1 22 -32.80 56.79 -7 -1 22 32.70 61.99 -6 -1 22 61.69 53.99 -5 -1 22 44.40 54.69 3 -1 -22 18.20 55.29 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 77110 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 O1 O 0.7272(3) 0.8458(8) 0.9307(3) 0.0522(17) Uani 1 1 d . . O2 O 0.6748(3) 0.5706(8) 0.8470(3) 0.0513(17) Uani 1 1 d . . O3 O 0.4652(2) 0.6841(7) 0.6898(3) 0.0385(14) Uani 1 1 d . . O4 O 0.5045(3) 0.2164(7) 0.9167(3) 0.0395(14) Uani 1 1 d . . N1 N 0.5679(3) 0.8932(8) 0.7617(3) 0.0321(16) Uani 1 1 d . . N2 N 0.3993(3) 0.4301(8) 0.8609(4) 0.0333(16) Uani 1 1 d . . C1 C 0.8615(4) 0.8241(18) 1.0002(6) 0.079(3) Uani 1 1 d . . H1 H 0.8783 0.8651 0.9584 0.119 Uiso 1 1 calc R U H3 H 0.9013 0.7295 1.0350 0.119 Uiso 1 1 calc R U H28 H 0.8530 0.9669 1.0245 0.119 Uiso 1 1 calc R U C2 C 0.7880(4) 0.6877(15) 0.9738(6) 0.064(3) Uani 1 1 d . . H26 H 0.7939 0.5550 0.9432 0.077 Uiso 1 1 calc R U H27 H 0.7746 0.6252 1.0161 0.077 Uiso 1 1 calc R U C3 C 0.6746(4) 0.7642(11) 0.8702(5) 0.039(2) Uani 1 1 d . . C4 C 0.6157(3) 0.9507(10) 0.8363(4) 0.0333(19) Uani 1 1 d . . H24 H 0.5822 0.9726 0.8671 0.040 Uiso 1 1 calc R U H25 H 0.6427 1.1000 0.8358 0.040 Uiso 1 1 calc R U C5 C 0.5059(4) 0.7499(9) 0.7514(5) 0.0299(19) Uani 1 1 d . . C6 C 0.4877(4) 0.6717(10) 0.8183(4) 0.0343(19) Uani 1 1 d . . H13 H 0.4699 0.8070 0.8404 0.041 Uiso 1 1 calc R U H23 H 0.5351 0.6099 0.8549 0.041 Uiso 1 1 calc R U C7 C 0.4256(3) 0.4833(10) 0.7995(4) 0.036(2) Uani 1 1 d . . H21 H 0.3813 0.5364 0.7577 0.043 Uiso 1 1 calc R U H22 H 0.4464 0.3398 0.7843 0.043 Uiso 1 1 calc R U C8 C 0.3286(3) 0.5340(9) 0.8614(4) 0.033(2) Uani 1 1 d . . C9 C 0.3287(4) 0.7281(11) 0.9043(5) 0.046(2) Uani 1 1 d . . H20 H 0.3762 0.7932 0.9340 0.055 Uiso 1 1 calc R U C10 C 0.2608(4) 0.8254(11) 0.9038(5) 0.052(3) Uani 1 1 d . . H17 H 0.2613 0.9624 0.9318 0.062 Uiso 1 1 calc R U C11 C 0.1909(4) 0.7272(11) 0.8631(5) 0.043(2) Uani 1 1 d . . H2 H 0.1436 0.7920 0.8643 0.051 Uiso 1 1 calc R U C12 C 0.5905(4) 0.9702(10) 0.6972(5) 0.040(2) Uani 1 1 d . . C13 C 0.6065(4) 0.7595(10) 0.6566(5) 0.041(2) Uani 1 1 d . . H6 H 0.6453 0.6601 0.6908 0.061 Uiso 1 1 calc R U H4 H 0.6259 0.8118 0.6174 0.061 Uiso 1 1 calc R U H5 H 0.5588 0.6705 0.6354 0.061 Uiso 1 1 calc R U C14 C 0.6642(4) 1.1158(11) 0.7216(5) 0.045(2) Uani 1 1 d . . H7 H 0.6560 1.2543 0.7480 0.068 Uiso 1 1 calc R U H9 H 0.6776 1.1643 0.6784 0.068 Uiso 1 1 calc R U H8 H 0.7063 1.0223 0.7539 0.068 Uiso 1 1 calc R U C15 C 0.5264(4) 1.1210(10) 0.6475(5) 0.044(2) Uani 1 1 d . . H10 H 0.4795 1.0272 0.6280 0.067 Uiso 1 1 calc R U H11 H 0.5423 1.1807 0.6070 0.067 Uiso 1 1 calc R U H12 H 0.5162 1.2522 0.6757 0.067 Uiso 1 1 calc R U C16 C 0.4438(4) 0.3009(10) 0.9182(4) 0.0301(19) Uani 1 1 d . . C17 C 0.4168(4) 0.2656(11) 0.9813(5) 0.038(2) Uani 1 1 d . . H14 H 0.4471 0.1416 1.0125 0.057 Uiso 1 1 calc R U H16 H 0.3622 0.2208 0.9639 0.057 Uiso 1 1 calc R U H15 H 0.4229 0.4107 1.0095 0.057 Uiso 1 1 calc R U C18 C 0.1916(4) 0.5361(12) 0.8215(5) 0.044(2) Uani 1 1 d . . H18 H 0.1440 0.4704 0.7923 0.053 Uiso 1 1 calc R U C19 C 0.2592(4) 0.4357(11) 0.8206(5) 0.042(2) Uani 1 1 d . . H19 H 0.2583 0.2998 0.7921 0.050 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 0.047(3) 0.041(3) 0.051(5) -0.004(3) -0.007(3) 0.012(2) O2 0.057(3) 0.028(3) 0.054(4) -0.001(3) -0.002(3) 0.006(2) O3 0.041(3) 0.027(2) 0.037(4) -0.008(2) -0.003(2) -0.006(2) O4 0.046(3) 0.023(2) 0.040(4) 0.000(2) 0.001(2) 0.001(2) N1 0.034(3) 0.022(3) 0.028(4) 0.004(3) -0.007(3) -0.007(2) N2 0.034(3) 0.022(3) 0.037(5) -0.001(3) 0.002(3) 0.000(3) C1 0.049(5) 0.110(8) 0.067(9) -0.006(6) 0.004(5) 0.018(5) C2 0.065(5) 0.068(5) 0.048(7) 0.020(5) 0.003(4) 0.022(5) C3 0.044(4) 0.028(4) 0.039(6) -0.006(4) 0.005(4) -0.006(3) C4 0.032(4) 0.022(3) 0.035(6) -0.002(3) -0.004(3) -0.001(3) C5 0.039(4) 0.008(3) 0.036(6) 0.000(3) 0.004(4) 0.005(3) C6 0.037(4) 0.022(3) 0.034(6) -0.002(3) -0.002(3) -0.008(3) C7 0.035(4) 0.026(3) 0.036(6) -0.004(3) -0.003(3) 0.002(3) C8 0.034(4) 0.012(3) 0.041(6) 0.003(3) -0.003(3) 0.000(3) C9 0.033(4) 0.024(4) 0.069(8) -0.007(4) 0.001(4) -0.002(3) C10 0.047(5) 0.029(4) 0.074(8) -0.028(4) 0.012(4) -0.011(4) C11 0.043(4) 0.027(4) 0.053(7) 0.008(4) 0.009(4) 0.005(3) C12 0.044(4) 0.015(3) 0.049(6) -0.001(3) 0.002(4) -0.005(3) C13 0.051(4) 0.020(3) 0.047(6) -0.003(3) 0.011(4) -0.004(3) C14 0.049(4) 0.027(3) 0.053(7) 0.000(4) 0.008(4) -0.005(3) C15 0.047(4) 0.023(3) 0.055(7) 0.011(4) 0.004(4) 0.003(3) C16 0.029(4) 0.011(3) 0.040(6) -0.004(3) -0.003(4) -0.001(3) C17 0.041(4) 0.022(3) 0.045(6) 0.002(3) 0.005(4) 0.001(3) C18 0.037(4) 0.037(4) 0.045(6) -0.008(4) -0.005(4) -0.006(3) C19 0.049(5) 0.016(3) 0.054(7) -0.004(3) 0.008(4) -0.005(3) 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 C3 O1 C2 118.7(6) C5 N1 C4 119.1(6) C5 N1 C12 119.7(6) C4 N1 C12 120.9(5) C16 N2 C8 121.9(7) C16 N2 C7 120.5(6) C8 N2 C7 117.4(6) O1 C2 C1 107.8(7) O2 C3 O1 124.3(6) O2 C3 C4 125.6(7) O1 C3 C4 110.1(5) N1 C4 C3 112.6(5) O3 C5 N1 122.6(7) O3 C5 C6 120.0(6) N1 C5 C6 117.4(6) C5 C6 C7 111.3(6) N2 C7 C6 112.0(6) C19 C8 C9 119.4(6) C19 C8 N2 119.8(6) C9 C8 N2 120.8(5) C10 C9 C8 120.0(6) C9 C10 C11 120.8(7) C18 C11 C10 118.6(6) N1 C12 C13 110.2(5) N1 C12 C15 109.1(6) C13 C12 C15 111.4(7) N1 C12 C14 111.1(6) C13 C12 C14 107.0(6) C15 C12 C14 108.0(5) O4 C16 N2 120.6(7) O4 C16 C17 121.2(6) N2 C16 C17 118.3(6) C11 C18 C19 121.7(6) C18 C19 C8 119.4(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C3 1.335(9) O1 C2 1.467(9) O2 C3 1.196(8) O3 C5 1.239(8) O4 C16 1.222(7) N1 C5 1.364(8) N1 C4 1.460(9) N1 C12 1.497(11) N2 C16 1.361(9) N2 C8 1.428(8) N2 C7 1.446(10) C1 C2 1.497(11) C3 C4 1.509(9) C5 C6 1.502(11) C6 C7 1.525(8) C8 C19 1.380(9) C8 C9 1.385(10) C9 C10 1.362(9) C10 C11 1.387(10) C11 C18 1.359(10) C12 C13 1.519(10) C12 C15 1.521(10) C12 C14 1.527(9) C16 C17 1.468(11) C18 C19 1.372(9)