#------------------------------------------------------------------------------ #$Date: 2022-08-09 01:27:48 +0300 (Tue, 09 Aug 2022) $ #$Revision: 277156 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/74/1567440.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_1567440 loop_ _publ_author_name 'Mondal, Debashis' 'Dandekar, Bhupendra R.' 'Ahmad, Manzoor' 'Mondal, Abhishek' 'Mondal, Jagannath' 'Talukdar, Pinaki' _publ_section_title ; Selective and rapid water transportation across a self-assembled peptide-diol channel via the formation of a dual water array ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D2SC01737G _journal_year 2022 _chemical_absolute_configuration Chiral _chemical_formula_sum 'C23 H40 N2 O5' _chemical_formula_weight 424.57 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2021-11-16 deposited with the CCDC. 2022-07-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.014(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 37.83(2) _cell_length_b 4.929(3) _cell_length_c 12.845(7) _cell_measurement_reflns_used 1022 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 19.40 _cell_measurement_theta_min 2.53 _cell_volume 2377(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-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.1223 _diffrn_reflns_av_unetI/netI 0.1475 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13714 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 24.998 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 1.085 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.186 _exptl_crystal_description Block _exptl_crystal_F_000 928.0 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Methanol : Water (10 : 1)' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.449 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.119 _refine_ls_abs_structure_details ; Flack x determined using 629 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -1.7(10) _refine_ls_extinction_coef 0.032(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 287 _refine_ls_number_reflns 4026 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.996 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0668 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0749P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1355 _refine_ls_wR_factor_ref 0.1804 _reflns_Friedel_coverage 0.708 _reflns_Friedel_fraction_full 0.917 _reflns_Friedel_fraction_max 0.917 _reflns_number_gt 2420 _reflns_number_total 4026 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2sc01737g2.cif _cod_data_source_block Compound_2R _cod_original_sg_symbol_H-M 'C 2' _cod_database_code 1567440 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL DMM_a.res in C2 DMM_a.res created by SHELXL-2016/6 at 22:36:50 on 04-Nov-2020 CELL 0.71073 37.8327 4.9285 12.8447 90.000 97.014 90.000 ZERR 48.000 0.0210 0.0031 0.0069 0.000 0.013 0.000 LATT -7 SYMM -X, Y, -Z SFAC C H N O UNIT 48 48 48 48 OMIT -2 50 REM Old TITL DMM in C2 REM SHELXT solution in C2 REM R1 0.160, Rweak 0.039, Alpha 0.004, Orientation as input REM Flack x= -2.863 ( 2.148 ) from Parsons' quotients REM Formula found by SHELXT: C23 N2 O5 L.S. 10 ACTA BOND $H FMAP 2 PLAN 30 TEMP 23.000 WGHT 0.074900 EXTI 0.031633 FVAR 0.41303 O5 4 0.523185 0.118791 0.850079 11.00000 0.02898 0.02210 = 0.03414 -0.00251 0.00015 0.00304 O1 4 0.563738 0.667167 0.394456 11.00000 0.03269 0.04136 = 0.02924 0.00843 -0.00066 -0.00655 AFIX 147 H1 2 0.543398 0.725784 0.381321 11.00000 -1.50000 AFIX 0 O4 4 0.585964 0.818478 0.735251 11.00000 0.03867 0.02029 = 0.04284 0.00746 0.01514 0.00258 O2 4 0.533013 0.405160 0.562832 11.00000 0.02276 0.06187 = 0.04289 0.02383 0.01208 0.01251 N1 3 0.593114 0.373573 0.700671 11.00000 0.01729 0.02296 = 0.02871 0.00257 0.00232 0.00172 AFIX 43 H24 2 0.594836 0.212780 0.726806 11.00000 -1.20000 AFIX 0 N2 3 0.540196 0.555291 0.875961 11.00000 0.02194 0.02242 = 0.02924 -0.00142 0.00793 0.00556 AFIX 43 H2A 2 0.533533 0.718041 0.887836 11.00000 -1.20000 AFIX 0 C21 1 0.515259 0.359294 0.860837 11.00000 0.02174 0.02566 = 0.01111 -0.00095 0.00337 0.00168 C3 1 0.597445 0.409615 0.589895 11.00000 0.01982 0.01708 = 0.02402 0.00377 0.00161 -0.00057 AFIX 13 H3 2 0.599461 0.604227 0.576116 11.00000 -1.20000 AFIX 0 C4 1 0.631429 0.270844 0.564973 11.00000 0.02076 0.02145 = 0.02696 0.00059 0.00248 0.00174 AFIX 23 H4A 2 0.629668 0.078203 0.578927 11.00000 -1.20000 H4B 2 0.633289 0.292323 0.490772 11.00000 -1.20000 AFIX 0 C12 1 0.586628 0.579131 0.762595 11.00000 0.01577 0.02012 = 0.03249 0.00262 0.00528 -0.00101 C9 1 0.799734 0.360951 0.700619 11.00000 0.01924 0.03441 = 0.03569 -0.00093 0.00480 0.00178 AFIX 23 H9A 2 0.798099 0.318925 0.773651 11.00000 -1.20000 H9B 2 0.799477 0.556921 0.693581 11.00000 -1.20000 AFIX 0 C15 1 0.640110 0.620379 0.961326 11.00000 0.02198 0.02111 = 0.03609 -0.00430 0.00031 0.00200 C2 1 0.564230 0.301070 0.522074 11.00000 0.01983 0.02447 = 0.03211 0.00265 0.00159 0.00242 AFIX 13 H2C 2 0.564113 0.102625 0.526851 11.00000 -1.20000 AFIX 0 C8 1 0.767209 0.247079 0.634640 11.00000 0.01828 0.03134 = 0.04138 0.00114 0.00210 0.00153 AFIX 23 H8A 2 0.767075 0.051386 0.642633 11.00000 -1.20000 H8B 2 0.768869 0.286667 0.561423 11.00000 -1.20000 AFIX 0 C22 1 0.476936 0.455537 0.857310 11.00000 0.02377 0.02730 = 0.02218 -0.00349 0.00428 0.00275 AFIX 23 H22A 2 0.475268 0.580843 0.914740 11.00000 -1.20000 H22B 2 0.470283 0.552974 0.792252 11.00000 -1.20000 AFIX 0 C10 1 0.835176 0.254833 0.672397 11.00000 0.02314 0.03465 = 0.04022 0.00206 0.00672 -0.00039 AFIX 23 H10A 2 0.835931 0.059415 0.681372 11.00000 -1.20000 H10B 2 0.836836 0.293518 0.599109 11.00000 -1.20000 AFIX 0 C5 1 0.665183 0.380107 0.627293 11.00000 0.02168 0.02793 = 0.04024 -0.00028 0.00181 -0.00312 AFIX 23 H5A 2 0.666266 0.574470 0.616229 11.00000 -1.20000 H5B 2 0.663823 0.350076 0.701331 11.00000 -1.20000 AFIX 0 C7 1 0.732500 0.359882 0.663391 11.00000 0.02099 0.03249 = 0.03971 -0.00089 0.00147 0.00430 AFIX 23 H7A 2 0.731025 0.319676 0.736660 11.00000 -1.20000 H7B 2 0.732949 0.555713 0.656129 11.00000 -1.20000 AFIX 0 C6 1 0.699208 0.253183 0.599027 11.00000 0.01710 0.03346 = 0.03504 -0.00146 0.00619 -0.00101 AFIX 23 H6A 2 0.697992 0.058369 0.608724 11.00000 -1.20000 H6B 2 0.700918 0.286781 0.525401 11.00000 -1.20000 AFIX 0 C13 1 0.578313 0.502638 0.873016 11.00000 0.01721 0.01884 = 0.03073 0.00178 0.00436 0.00298 AFIX 13 H13 2 0.583364 0.309765 0.886068 11.00000 -1.20000 AFIX 0 C23 1 0.450820 0.223066 0.865039 11.00000 0.02320 0.03456 = 0.02885 0.00063 0.00372 -0.00221 AFIX 137 H23A 2 0.453960 0.089418 0.812577 11.00000 -1.50000 H23B 2 0.426898 0.291512 0.854073 11.00000 -1.50000 H23C 2 0.455153 0.141833 0.933335 11.00000 -1.50000 AFIX 0 C16 1 0.660948 0.764390 0.898539 11.00000 0.02753 0.04156 = 0.04005 0.00382 0.00520 -0.00044 AFIX 43 H16 2 0.650555 0.897585 0.853481 11.00000 -1.20000 AFIX 0 C20 1 0.656060 0.423013 1.026884 11.00000 0.03305 0.03833 = 0.04112 0.00170 0.00441 0.00323 AFIX 43 H20 2 0.642449 0.324105 1.069092 11.00000 -1.20000 AFIX 0 C11 1 0.866820 0.379546 0.738786 11.00000 0.02063 0.05404 = 0.03583 0.00565 0.00495 0.00148 AFIX 137 H11A 2 0.867390 0.571124 0.725589 11.00000 -1.50000 H11B 2 0.888358 0.297810 0.721272 11.00000 -1.50000 H11C 2 0.864793 0.348836 0.811622 11.00000 -1.50000 AFIX 0 C17 1 0.697111 0.711435 0.902400 11.00000 0.02985 0.04536 = 0.05282 -0.00507 0.01035 -0.00823 AFIX 43 H17 2 0.710879 0.808528 0.860082 11.00000 -1.20000 AFIX 0 C14 1 0.600510 0.674459 0.956187 11.00000 0.02493 0.02783 = 0.03339 -0.00043 0.00597 0.00054 AFIX 23 H14A 2 0.596042 0.864943 0.940783 11.00000 -1.20000 H14B 2 0.592950 0.636824 1.024221 11.00000 -1.20000 AFIX 0 C1 1 0.562591 0.380269 0.409505 11.00000 0.02659 0.02987 = 0.03553 -0.00944 0.00154 0.00166 AFIX 23 H1A 2 0.582430 0.297665 0.380103 11.00000 -1.20000 H1B 2 0.540782 0.309690 0.371584 11.00000 -1.20000 AFIX 0 C18 1 0.712546 0.513963 0.969353 11.00000 0.02249 0.04028 = 0.06268 -0.01187 -0.00407 -0.00006 AFIX 43 H18 2 0.736812 0.478848 0.972720 11.00000 -1.20000 AFIX 0 C19 1 0.692152 0.370096 1.030685 11.00000 0.02870 0.03871 = 0.05388 0.00129 -0.00498 0.00529 AFIX 43 H19 2 0.702563 0.235899 1.075230 11.00000 -1.20000 AFIX 0 O3 4 0.493536 0.883779 0.364019 11.00000 0.03970 0.05148 = 0.04855 -0.01614 0.01662 -0.01955 H25 2 0.486602 0.949490 0.305122 11.00000 0.14495 H26 2 0.480555 0.721972 0.383385 11.00000 0.06367 H27 2 0.522263 0.283045 0.565102 11.00000 0.10700 HKLF 4 REM DMM_a.res in C2 REM R1 = 0.0668 for 2420 Fo > 4sig(Fo) and 0.1303 for all 4026 data REM 287 parameters refined using 1 restraints END WGHT 0.0732 0.0000 REM Highest difference peak 0.449, deepest hole -0.486, 1-sigma level 0.119 Q1 1 0.7114 0.2478 0.6410 11.00000 0.05 0.45 Q2 1 0.7306 0.3838 0.6369 11.00000 0.05 0.42 Q3 1 0.7428 0.2227 0.6496 11.00000 0.05 0.41 Q4 1 0.8107 0.2940 0.6884 11.00000 0.05 0.39 Q5 1 0.6844 0.3467 0.6050 11.00000 0.05 0.38 Q6 1 0.7870 0.2711 0.6577 11.00000 0.05 0.38 Q7 1 0.6885 0.2906 0.6144 11.00000 0.05 0.37 Q8 1 0.7594 0.3786 0.6730 11.00000 0.05 0.37 Q9 1 0.6612 0.2797 0.5814 11.00000 0.05 0.36 Q10 1 0.8074 0.4337 0.6829 11.00000 0.05 0.36 Q11 1 0.7392 0.8578 0.9397 11.00000 0.05 0.32 Q12 1 0.7933 0.1146 0.7024 11.00000 0.05 0.31 Q13 1 0.6833 0.7857 0.9126 11.00000 0.05 0.30 Q14 1 0.8098 0.0145 0.6812 11.00000 0.05 0.30 Q15 1 0.7094 0.5307 0.6191 11.00000 0.05 0.29 Q16 1 0.6615 0.1475 0.6332 11.00000 0.05 0.29 Q17 1 0.7419 0.2912 1.0394 11.00000 0.05 0.29 Q18 1 0.7312 0.3424 1.1168 11.00000 0.05 0.29 Q19 1 0.8422 0.3557 0.6803 11.00000 0.05 0.28 Q20 1 0.7262 0.7965 0.8267 11.00000 0.05 0.28 Q21 1 0.6633 0.8550 0.8938 11.00000 0.05 0.28 Q22 1 0.7208 0.9609 0.8805 11.00000 0.05 0.28 Q23 1 0.7002 0.4432 0.6752 11.00000 0.05 0.28 Q24 1 0.6085 0.3634 0.5665 11.00000 0.05 0.28 Q25 1 0.7221 0.3066 1.0943 11.00000 0.05 0.27 Q26 1 0.5985 0.7852 0.8715 11.00000 0.05 0.26 Q27 1 0.6770 0.3079 1.0689 11.00000 0.05 0.26 Q28 1 0.6446 0.1106 0.5794 11.00000 0.05 0.26 Q29 1 0.5300 0.7848 0.8326 11.00000 0.05 0.25 Q30 1 0.8354 0.5363 0.7002 11.00000 0.05 0.25 ; _shelx_res_checksum 18484 _shelx_hkl_file ; 2 0 0 0.00 0.50 2 0 0 -1.10 0.70 2 0 0 -0.50 0.40 2 0 0 0.80 0.80 -2 0 0 2.40 1.20 -2 0 0 -0.80 0.50 -2 0 0 0.00 0.50 -4 0 0 3.60 2.40 -4 0 0 1.40 3.20 4 0 0 7.90 3.60 4 0 0 1.90 2.50 4 0 0 3.80 2.40 4 0 0 2.80 3.10 4 0 0 2.40 3.20 -4 0 0 -3.20 1.40 -4 0 0 2.20 3.20 -4 0 0 2.40 3.00 -6 0 0 2.40 4.50 -6 0 0 0.80 4.60 -6 0 0 -5.30 3.10 6 0 0 2.90 5.50 6 0 0 -2.00 4.70 6 0 0 5.10 3.90 6 0 0 -4.60 4.60 -6 0 0 8.70 3.40 -6 0 0 -0.50 4.00 8 0 0 845.62 89.59 8 0 0 873.01 88.99 -8 0 0 864.51 88.59 8 0 0 880.21 89.89 -8 0 0 876.11 89.99 8 0 0 896.81 89.69 -8 0 0 810.42 89.49 -8 0 0 777.92 88.89 -10 0 0 48.60 9.80 -10 0 0 46.90 8.50 -10 0 0 47.20 12.40 -10 0 0 51.69 10.80 -10 0 0 63.39 11.80 10 0 0 53.49 11.00 10 0 0 57.49 11.20 10 0 0 48.50 11.50 10 0 0 49.60 9.60 -12 0 0 43.80 11.60 -12 0 0 51.69 10.00 12 0 0 49.00 10.60 -12 0 0 27.80 10.10 12 0 0 64.59 12.40 12 0 0 52.69 12.60 12 0 0 68.19 12.90 -12 0 0 77.49 14.40 -12 0 0 63.29 9.60 -14 0 0 192.88 26.10 14 0 0 204.38 28.90 14 0 0 223.58 27.00 14 0 0 259.37 30.20 -14 0 0 265.17 28.70 -14 0 0 232.08 25.70 -14 0 0 195.58 29.20 -16 0 0 933.41 95.39 16 0 0 916.51 96.49 -16 0 0 785.62 97.09 16 0 0 934.61 97.89 -16 0 0 982.50 96.59 -16 0 0 874.31 98.29 -18 0 0 766.22 82.79 -18 0 0 758.32 80.39 -18 0 0 792.22 84.19 18 0 0 780.82 83.79 -18 0 0 733.83 81.49 18 0 0 736.43 81.69 -20 0 0 58.59 10.40 -20 0 0 36.30 15.70 20 0 0 36.00 12.10 -20 0 0 56.19 14.30 20 0 0 52.79 15.10 -22 0 0 -3.80 9.80 -22 0 0 -5.40 8.20 -22 0 0 9.60 7.00 22 0 0 12.00 9.40 -24 0 0 -6.40 12.90 -24 0 0 5.40 6.50 24 0 0 -4.70 10.50 -24 0 0 -6.60 10.30 26 0 0 41.90 17.70 -26 0 0 41.90 10.10 -26 0 0 52.69 15.80 -28 0 0 798.62 84.79 -28 0 0 713.63 78.99 28 0 0 726.83 85.19 -30 0 0 818.42 84.19 -30 0 0 792.02 89.69 30 0 0 702.13 89.09 32 0 0 -1.50 15.30 -32 0 0 2.00 7.00 -32 0 0 -21.10 10.90 -34 0 0 -4.10 14.60 -34 0 0 15.70 8.40 34 0 0 -5.60 16.80 36 0 0 29.30 19.40 -36 0 0 -9.90 15.00 38 0 0 9.10 17.80 -38 0 0 -8.70 15.80 -40 0 0 92.09 27.10 40 0 0 91.89 26.60 42 0 0 14.00 22.20 -42 0 0 20.30 22.00 -44 0 0 -5.40 22.60 44 0 0 51.39 26.10 -1 -1 0 2264.47 258.97 1 -1 0 2759.42 258.97 1 -1 0 2379.06 258.97 -1 1 0 2459.15 259.07 -1 1 0 2653.83 258.87 3 -1 0 713.33 67.39 3 -1 0 629.44 67.39 -3 -1 0 632.34 67.59 3 1 0 659.23 67.19 -3 1 0 549.95 67.39 -3 1 0 634.04 66.89 -3 1 0 565.64 65.99 -5 -1 0 164.98 20.00 -5 -1 0 153.28 21.60 5 -1 0 154.68 20.90 5 -1 0 185.48 20.50 -5 1 0 180.38 21.10 -5 1 0 160.98 22.00 -5 1 0 91.49 18.60 5 1 0 131.99 19.40 5 1 0 169.18 21.90 -7 -1 0 955.40 101.19 7 -1 0 1065.89 101.69 -7 -1 0 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10.30 21.20 10 2 13 24.90 23.20 12 -2 13 -4.40 22.10 12 2 13 31.60 24.40 12 2 13 46.60 24.30 -12 2 -13 -30.20 19.10 12 2 13 27.10 26.60 14 -2 13 24.20 25.20 -14 2 -13 -11.10 22.80 14 2 13 2.70 21.70 14 2 13 18.40 25.40 13 3 -13 11.50 22.60 -13 3 13 24.30 28.50 -13 3 13 1.30 24.00 -11 3 13 32.80 29.10 11 3 -13 56.49 29.30 -11 3 13 100.89 35.10 9 3 -13 -0.70 24.10 -9 3 13 0.30 25.50 -9 3 13 -4.90 23.50 -7 -3 13 94.19 25.70 7 3 -13 61.69 29.00 -7 3 13 90.79 33.40 -7 3 13 78.59 34.40 -5 -3 13 9.00 20.80 -5 3 13 -3.40 23.50 5 3 -13 40.30 26.50 -5 3 13 8.60 23.40 -3 -3 13 -2.20 20.60 -3 3 13 39.90 25.40 -3 3 13 82.79 30.00 3 3 -13 10.60 22.40 -1 -3 13 7.00 22.00 -1 3 13 11.10 26.80 -1 3 13 42.00 26.60 1 3 -13 7.80 22.00 -1 3 13 3.00 21.00 1 -3 13 10.90 23.80 1 3 13 -17.60 18.40 1 3 13 10.30 24.20 1 3 13 6.10 16.30 -1 3 -13 -34.90 17.80 3 -3 13 26.10 25.00 3 3 13 -17.80 17.30 3 3 13 5.40 24.60 -3 3 -13 25.40 25.80 3 3 13 -11.50 19.70 -3 3 -13 -11.60 22.70 5 3 13 5.50 27.60 -5 3 -13 -8.90 22.70 -24 0 14 11.30 20.10 -22 0 14 13.70 17.30 -22 0 14 25.70 23.10 -20 0 14 50.19 21.80 -20 0 14 94.29 29.60 -18 0 14 -3.10 14.40 -18 0 14 -20.70 17.00 -16 0 14 -10.10 16.00 -16 0 14 6.10 18.10 -14 0 14 7.70 15.20 -14 0 14 20.00 22.50 -12 0 14 -13.00 13.80 -12 0 14 2.50 18.80 -10 0 14 -11.50 18.30 -10 0 14 4.60 15.70 -10 0 14 -7.00 17.30 -8 0 14 2.30 15.50 -8 0 14 -8.00 15.10 -8 0 14 0.60 17.90 -6 0 14 27.10 17.10 -6 0 14 33.20 19.30 -6 0 14 2.90 18.80 -4 0 14 93.29 28.30 -4 0 14 100.19 24.90 -4 0 14 48.10 22.20 -2 0 14 57.59 23.50 -2 0 14 105.89 29.30 -2 0 14 70.39 23.80 0 0 14 -13.70 20.10 0 0 14 -2.10 17.00 0 0 14 8.80 17.20 2 0 14 23.90 22.40 2 0 14 29.70 23.50 2 0 14 105.09 24.80 4 0 14 38.70 20.10 4 0 14 91.99 28.70 4 0 14 66.49 26.20 6 0 14 11.50 16.70 6 0 14 -16.20 17.30 -6 0 -14 -7.10 30.40 6 0 14 -15.50 15.80 8 0 14 183.08 39.40 8 0 14 187.88 35.60 10 0 14 41.10 29.00 10 0 14 9.20 19.90 10 0 14 4.50 17.00 -10 0 -14 24.30 17.70 12 0 14 10.60 19.90 12 0 14 2.00 18.60 -12 0 -14 2.80 19.90 12 0 14 9.60 26.50 14 0 14 58.79 24.60 -14 0 -14 9.20 23.20 14 0 14 -2.80 20.40 -23 1 14 50.09 22.60 -21 -1 14 30.00 24.50 -21 1 14 -21.90 17.40 -21 1 14 24.90 21.60 -19 -1 14 7.10 22.40 -19 1 14 -4.50 20.50 -19 1 14 15.70 19.30 -17 -1 14 -20.10 12.00 -17 -1 14 9.00 23.00 -17 1 14 11.20 20.50 -17 1 14 0.20 17.20 -15 -1 14 -17.80 12.80 -15 -1 14 -6.80 19.00 -15 1 14 -11.50 18.10 -15 1 14 6.30 21.20 -13 -1 14 -10.10 19.50 -13 -1 14 -9.10 15.00 -13 1 14 4.60 17.30 -13 1 14 0.60 18.70 -11 -1 14 -5.80 18.80 -11 -1 14 28.60 17.10 -11 1 14 12.50 17.40 -11 1 14 -13.60 16.80 -9 -1 14 36.20 24.30 -9 -1 14 7.30 17.30 9 1 -14 47.50 30.70 -9 1 14 26.50 22.20 -9 1 14 8.90 19.40 -7 -1 14 21.30 23.90 -7 -1 14 16.10 17.30 -7 1 14 -0.70 17.10 -7 1 14 65.09 25.70 7 1 -14 11.10 17.60 -5 -1 14 28.30 20.80 -5 -1 14 1.10 21.80 5 1 -14 14.20 18.20 -5 1 14 35.90 22.10 -5 1 14 22.50 20.30 -5 1 14 32.20 20.60 -3 -1 14 36.00 19.20 -3 -1 14 25.70 23.30 -3 1 14 32.50 23.90 3 1 -14 23.20 18.50 -3 1 14 9.00 18.80 -3 1 14 61.89 25.90 -1 -1 14 69.89 28.10 -1 -1 14 35.50 21.90 1 1 -14 66.09 22.70 -1 1 14 46.30 23.60 -1 1 14 80.89 27.90 -1 1 14 84.99 27.10 1 -1 14 52.89 29.30 1 -1 14 98.49 28.30 1 1 14 71.69 26.80 -1 1 -14 27.30 19.50 1 1 14 43.20 24.70 1 1 14 28.10 22.20 3 -1 14 -46.50 17.90 3 -1 14 18.50 19.00 3 1 14 -4.80 19.70 3 1 14 -6.60 19.10 3 1 14 5.50 19.30 -3 1 -14 2.40 15.00 5 -1 14 -14.70 20.00 5 -1 14 -5.70 18.40 5 1 14 34.50 22.70 5 1 14 -38.50 17.20 5 1 14 -6.50 18.20 -5 1 -14 -17.40 19.10 7 -1 14 16.90 21.50 7 1 14 28.40 23.20 -7 1 -14 34.60 24.50 7 1 14 3.20 18.90 7 1 14 -12.30 17.80 9 -1 14 22.10 22.60 9 1 14 10.30 19.70 -9 1 -14 20.00 21.10 9 1 14 39.00 24.60 9 1 14 29.90 24.30 11 -1 14 9.30 21.60 -11 1 -14 -12.60 22.80 11 1 14 35.10 21.40 11 1 14 -9.20 18.50 11 1 14 7.20 22.30 13 -1 14 -6.80 19.50 13 1 14 61.19 27.00 13 1 14 -0.90 21.20 -13 1 -14 26.60 24.00 -16 -2 14 -5.50 24.40 -16 2 14 19.50 22.30 -16 2 14 11.40 20.20 16 2 -14 8.50 20.50 -14 -2 14 23.80 25.20 -14 2 14 27.00 22.80 -14 2 14 35.50 23.60 14 2 -14 20.70 21.00 -12 -2 14 -15.00 22.00 -12 -2 14 -6.30 14.20 12 2 -14 -7.10 21.90 -12 2 14 35.30 24.50 -12 2 14 22.20 25.60 -10 -2 14 21.30 25.00 -10 -2 14 37.60 20.50 -10 2 14 2.10 21.20 -10 2 14 28.70 22.00 10 2 -14 14.60 23.60 -8 -2 14 20.40 19.70 -8 -2 14 9.70 25.80 8 2 -14 30.10 23.90 -8 2 14 54.19 25.00 -8 2 14 2.40 19.80 -6 -2 14 25.00 19.80 -6 -2 14 26.20 25.50 6 2 -14 2.50 17.70 -6 2 14 18.80 22.90 -6 2 14 -20.70 18.10 -4 -2 14 29.80 19.60 -4 2 14 -9.90 22.60 -4 2 14 -16.80 20.20 4 2 -14 20.90 21.10 -4 2 14 23.30 24.50 -2 -2 14 27.60 19.40 -2 2 14 58.69 28.50 -2 2 14 16.80 22.00 2 2 -14 17.80 21.60 -2 2 14 12.20 24.70 0 -2 14 11.80 21.80 0 2 14 63.89 28.70 0 2 -14 8.20 20.80 0 2 14 22.10 24.90 0 2 14 14.10 23.30 2 -2 14 7.70 18.50 2 2 14 -10.60 20.80 2 2 14 21.80 22.50 -2 2 -14 37.00 26.10 2 2 14 -12.00 24.20 4 -2 14 -8.10 18.90 -4 2 -14 -2.40 21.10 4 2 14 -11.90 18.30 4 2 14 11.30 21.80 4 2 14 10.20 26.20 6 -2 14 50.89 25.40 6 2 14 -8.70 22.60 6 2 14 9.80 23.50 6 2 14 17.90 22.40 -6 2 -14 -12.50 21.30 -16 0 15 22.70 25.20 -16 0 15 -18.40 16.70 -14 0 15 -28.80 13.40 -14 0 15 30.20 23.40 -12 0 15 -25.50 17.10 -12 0 15 -8.30 18.90 -10 0 15 -9.60 18.10 -10 0 15 18.60 21.50 -8 0 15 46.90 25.40 -8 0 15 12.40 17.80 -8 0 15 5.80 18.60 -6 0 15 13.20 21.60 -6 0 15 25.20 22.60 -6 0 15 0.00 18.40 -4 0 15 14.70 18.70 -4 0 15 32.30 23.70 -4 0 15 5.30 17.90 -2 0 15 73.09 25.70 -2 0 15 46.40 26.90 -2 0 15 101.59 29.00 0 0 15 2.90 19.40 0 0 15 0.10 20.20 0 0 15 -7.50 20.00 2 0 15 35.60 21.60 2 0 15 12.30 19.80 2 0 15 42.80 26.40 4 0 15 19.50 20.80 4 0 15 -1.30 19.60 4 0 15 -18.40 19.30 6 0 15 51.79 24.10 6 0 15 27.60 26.10 -13 -1 15 -6.80 22.50 -13 -1 15 -1.20 16.50 -13 1 15 2.90 22.10 -13 1 15 8.90 19.00 -11 -1 15 -4.20 16.10 -11 -1 15 33.00 24.60 -11 1 15 -6.00 19.30 -11 1 15 22.20 21.40 -9 -1 15 12.90 20.20 -9 -1 15 10.50 25.00 -9 1 15 -14.20 21.10 -9 1 15 16.20 20.10 -9 1 15 -5.00 21.00 -7 -1 15 -4.40 22.90 -7 -1 15 10.50 17.40 -7 1 15 36.10 25.00 -7 1 15 1.90 21.50 -7 1 15 31.60 21.30 -5 -1 15 5.70 21.20 -5 -1 15 36.40 25.80 -5 1 15 47.70 23.80 -5 1 15 34.50 24.00 -5 1 15 -4.10 20.20 -3 -1 15 72.89 26.30 -3 -1 15 64.69 28.10 -3 1 15 75.39 30.90 -3 1 15 103.49 31.90 -3 1 15 70.39 28.60 -1 -1 15 -1.10 19.50 -1 -1 15 2.00 24.60 -1 1 15 11.70 26.30 -1 1 15 -12.50 18.20 -1 1 15 9.60 22.00 1 -1 15 -38.90 14.60 1 -1 15 40.30 30.50 1 1 15 -29.70 22.10 1 1 15 27.50 22.50 1 1 15 6.90 23.40 3 -1 15 4.20 19.50 -3 1 -15 12.80 21.70 3 1 15 9.10 25.80 3 1 15 -0.50 19.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 7129 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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 O5 O 0.52318(11) 0.1188(9) 0.8501(3) 0.0287(12) Uani 1 1 d . . . . . O1 O 0.56374(11) 0.6672(10) 0.3945(3) 0.0348(13) Uani 1 1 d . . . . . H1 H 0.543398 0.725784 0.381321 0.052 Uiso 1 1 calc R U . . . O4 O 0.58596(12) 0.8185(9) 0.7353(3) 0.0331(12) Uani 1 1 d . . . . . O2 O 0.53301(13) 0.4052(14) 0.5628(4) 0.0418(16) Uani 1 1 d . . . . . N1 N 0.59311(12) 0.3736(12) 0.7007(4) 0.0230(12) Uani 1 1 d . . . . . H24 H 0.594836 0.212780 0.726806 0.028 Uiso 1 1 calc R U . . . N2 N 0.54020(12) 0.5553(12) 0.8760(4) 0.0241(13) Uani 1 1 d . . . . . H2A H 0.533533 0.718041 0.887836 0.029 Uiso 1 1 calc R U . . . C21 C 0.51526(15) 0.3593(15) 0.8608(4) 0.0194(14) Uani 1 1 d . . . . . C3 C 0.59744(14) 0.4096(14) 0.5899(4) 0.0204(14) Uani 1 1 d . . . . . H3 H 0.599461 0.604227 0.576116 0.024 Uiso 1 1 calc R U . . . C4 C 0.63143(14) 0.2708(14) 0.5650(4) 0.0231(15) Uani 1 1 d . . . . . H4A H 0.629668 0.078203 0.578927 0.028 Uiso 1 1 calc R U . . . H4B H 0.633289 0.292323 0.490772 0.028 Uiso 1 1 calc R U . . . C12 C 0.58663(15) 0.5791(14) 0.7626(5) 0.0226(15) Uani 1 1 d . . . . . C9 C 0.79973(14) 0.3610(16) 0.7006(5) 0.0297(17) Uani 1 1 d . . . . . H9A H 0.798099 0.318925 0.773651 0.036 Uiso 1 1 calc R U . . . H9B H 0.799477 0.556921 0.693581 0.036 Uiso 1 1 calc R U . . . C15 C 0.64011(15) 0.6204(14) 0.9613(5) 0.0267(16) Uani 1 1 d . . . . . C2 C 0.56423(14) 0.3011(14) 0.5221(4) 0.0256(17) Uani 1 1 d . . . . . H2C H 0.564113 0.102625 0.526851 0.031 Uiso 1 1 calc R U . . . C8 C 0.76721(14) 0.2471(16) 0.6346(5) 0.0305(17) Uani 1 1 d . . . . . H8A H 0.767075 0.051386 0.642633 0.037 Uiso 1 1 calc R U . . . H8B H 0.768869 0.286667 0.561423 0.037 Uiso 1 1 calc R U . . . C22 C 0.47694(15) 0.4555(14) 0.8573(5) 0.0243(16) Uani 1 1 d . . . . . H22A H 0.475268 0.580843 0.914740 0.029 Uiso 1 1 calc R U . . . H22B H 0.470283 0.552974 0.792252 0.029 Uiso 1 1 calc R U . . . C10 C 0.83518(15) 0.2548(16) 0.6724(5) 0.0324(17) Uani 1 1 d . . . . . H10A H 0.835931 0.059415 0.681372 0.039 Uiso 1 1 calc R U . . . H10B H 0.836836 0.293518 0.599109 0.039 Uiso 1 1 calc R U . . . C5 C 0.66518(15) 0.3801(17) 0.6273(5) 0.0301(16) Uani 1 1 d . . . . . H5A H 0.666266 0.574470 0.616229 0.036 Uiso 1 1 calc R U . . . H5B H 0.663823 0.350076 0.701331 0.036 Uiso 1 1 calc R U . . . C7 C 0.73250(14) 0.3599(17) 0.6634(5) 0.0312(16) Uani 1 1 d . . . . . H7A H 0.731025 0.319676 0.736660 0.037 Uiso 1 1 calc R U . . . H7B H 0.732949 0.555713 0.656129 0.037 Uiso 1 1 calc R U . . . C6 C 0.69921(14) 0.2532(16) 0.5990(5) 0.0283(16) Uani 1 1 d . . . . . H6A H 0.697992 0.058369 0.608724 0.034 Uiso 1 1 calc R U . . . H6B H 0.700918 0.286781 0.525401 0.034 Uiso 1 1 calc R U . . . C13 C 0.57831(14) 0.5026(14) 0.8730(5) 0.0221(15) Uani 1 1 d . . . . . H13 H 0.583364 0.309765 0.886068 0.027 Uiso 1 1 calc R U . . . C23 C 0.45082(15) 0.2231(15) 0.8650(5) 0.0288(16) Uani 1 1 d . . . . . H23A H 0.453960 0.089418 0.812577 0.043 Uiso 1 1 calc R U . . . H23B H 0.426898 0.291512 0.854073 0.043 Uiso 1 1 calc R U . . . H23C H 0.455153 0.141833 0.933335 0.043 Uiso 1 1 calc R U . . . C16 C 0.66095(16) 0.7644(16) 0.8985(5) 0.0363(19) Uani 1 1 d . . . . . H16 H 0.650555 0.897585 0.853481 0.044 Uiso 1 1 calc R U . . . C20 C 0.65606(17) 0.4230(16) 1.0269(5) 0.0375(19) Uani 1 1 d . . . . . H20 H 0.642449 0.324105 1.069092 0.045 Uiso 1 1 calc R U . . . C11 C 0.86682(16) 0.3795(18) 0.7388(5) 0.0367(19) Uani 1 1 d . . . . . H11A H 0.867390 0.571124 0.725589 0.055 Uiso 1 1 calc R U . . . H11B H 0.888358 0.297810 0.721272 0.055 Uiso 1 1 calc R U . . . H11C H 0.864793 0.348836 0.811622 0.055 Uiso 1 1 calc R U . . . C17 C 0.69711(17) 0.7114(18) 0.9024(6) 0.042(2) Uani 1 1 d . . . . . H17 H 0.710879 0.808528 0.860082 0.051 Uiso 1 1 calc R U . . . C14 C 0.60051(15) 0.6745(15) 0.9562(5) 0.0285(17) Uani 1 1 d . . . . . H14A H 0.596042 0.864943 0.940783 0.034 Uiso 1 1 calc R U . . . H14B H 0.592950 0.636824 1.024221 0.034 Uiso 1 1 calc R U . . . C1 C 0.56259(17) 0.3803(16) 0.4095(5) 0.0308(16) Uani 1 1 d . . . . . H1A H 0.582430 0.297665 0.380103 0.037 Uiso 1 1 calc R U . . . H1B H 0.540782 0.309690 0.371584 0.037 Uiso 1 1 calc R U . . . C18 C 0.71255(18) 0.5140(17) 0.9694(6) 0.043(2) Uani 1 1 d . . . . . H18 H 0.736812 0.478848 0.972720 0.051 Uiso 1 1 calc R U . . . C19 C 0.69215(17) 0.3701(18) 1.0307(6) 0.0413(19) Uani 1 1 d . . . . . H19 H 0.702563 0.235899 1.075230 0.050 Uiso 1 1 calc R U . . . O3 O 0.49354(14) 0.8838(15) 0.3640(5) 0.0457(15) Uani 1 1 d . . . . . H25 H 0.487(3) 0.95(3) 0.305(9) 0.14(6) Uiso 1 1 d . . . . . H26 H 0.481(2) 0.72(2) 0.383(6) 0.06(3) Uiso 1 1 d . . . . . H27 H 0.522(3) 0.28(3) 0.565(9) 0.11(5) 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 O5 0.029(2) 0.022(3) 0.034(3) -0.003(2) 0.0001(19) 0.003(2) O1 0.033(3) 0.041(4) 0.029(2) 0.008(2) -0.001(2) -0.007(2) O4 0.039(3) 0.020(3) 0.043(3) 0.007(2) 0.015(2) 0.003(2) O2 0.023(3) 0.062(5) 0.043(3) 0.024(3) 0.012(2) 0.013(3) N1 0.017(3) 0.023(3) 0.029(3) 0.003(3) 0.002(2) 0.002(3) N2 0.022(3) 0.022(3) 0.029(3) -0.001(3) 0.008(2) 0.006(3) C21 0.022(3) 0.026(4) 0.011(3) -0.001(3) 0.003(2) 0.002(3) C3 0.020(3) 0.017(4) 0.024(3) 0.004(3) 0.002(2) -0.001(3) C4 0.021(3) 0.021(4) 0.027(3) 0.001(3) 0.002(3) 0.002(3) C12 0.016(3) 0.020(4) 0.032(4) 0.003(3) 0.005(3) -0.001(3) C9 0.019(3) 0.034(4) 0.036(4) -0.001(4) 0.005(3) 0.002(3) C15 0.022(3) 0.021(4) 0.036(4) -0.004(3) 0.000(3) 0.002(3) C2 0.020(3) 0.024(4) 0.032(4) 0.003(3) 0.002(3) 0.002(3) C8 0.018(3) 0.031(4) 0.041(4) 0.001(4) 0.002(3) 0.002(3) C22 0.024(3) 0.027(4) 0.022(3) -0.003(3) 0.004(3) 0.003(3) C10 0.023(3) 0.035(5) 0.040(4) 0.002(4) 0.007(3) 0.000(3) C5 0.022(3) 0.028(4) 0.040(4) 0.000(4) 0.002(3) -0.003(3) C7 0.021(3) 0.032(4) 0.040(4) -0.001(4) 0.001(3) 0.004(3) C6 0.017(3) 0.033(4) 0.035(4) -0.001(3) 0.006(3) -0.001(3) C13 0.017(3) 0.019(4) 0.031(3) 0.002(3) 0.004(3) 0.003(3) C23 0.023(3) 0.035(4) 0.029(3) 0.001(3) 0.004(3) -0.002(3) C16 0.028(4) 0.042(5) 0.040(4) 0.004(4) 0.005(3) 0.000(4) C20 0.033(4) 0.038(5) 0.041(4) 0.002(4) 0.004(3) 0.003(4) C11 0.021(3) 0.054(5) 0.036(4) 0.006(4) 0.005(3) 0.001(4) C17 0.030(4) 0.045(5) 0.053(4) -0.005(4) 0.010(3) -0.008(4) C14 0.025(3) 0.028(4) 0.033(4) 0.000(3) 0.006(3) 0.001(3) C1 0.027(4) 0.030(4) 0.036(4) -0.009(4) 0.002(3) 0.002(3) C18 0.022(4) 0.040(5) 0.063(5) -0.012(4) -0.004(4) 0.000(4) C19 0.029(4) 0.039(5) 0.054(5) 0.001(4) -0.005(3) 0.005(4) O3 0.040(3) 0.051(4) 0.049(3) -0.016(3) 0.017(3) -0.020(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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 H1 109.5 . . ? C2 O2 H27 102(10) . . ? C12 N1 C3 122.7(6) . . ? C12 N1 H24 118.6 . . ? C3 N1 H24 118.6 . . ? C21 N2 C13 122.8(6) . . ? C21 N2 H2A 118.6 . . ? C13 N2 H2A 118.6 . . ? O5 C21 N2 121.9(5) . . ? O5 C21 C22 122.7(6) . . ? N2 C21 C22 115.4(6) . . ? N1 C3 C4 110.3(5) . . ? N1 C3 C2 109.2(5) . . ? C4 C3 C2 112.2(5) . . ? N1 C3 H3 108.4 . . ? C4 C3 H3 108.4 . . ? C2 C3 H3 108.4 . . ? C5 C4 C3 114.0(5) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? O4 C12 N1 124.0(6) . . ? O4 C12 C13 120.0(6) . . ? N1 C12 C13 116.0(6) . . ? C8 C9 C10 114.7(6) . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C20 C15 C16 118.6(6) . . ? C20 C15 C14 120.5(6) . . ? C16 C15 C14 120.9(6) . . ? O2 C2 C1 108.6(5) . . ? O2 C2 C3 108.6(5) . . ? C1 C2 C3 113.1(5) . . ? O2 C2 H2C 108.8 . . ? C1 C2 H2C 108.8 . . ? C3 C2 H2C 108.8 . . ? C9 C8 C7 113.4(6) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C23 C22 C21 112.8(6) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C11 C10 C9 112.7(6) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C6 C5 C4 114.3(6) . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C6 C7 C8 115.3(6) . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C7 C6 C5 113.6(6) . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N2 C13 C14 109.9(5) . . ? N2 C13 C12 107.0(4) . . ? C14 C13 C12 110.6(5) . . ? N2 C13 H13 109.8 . . ? C14 C13 H13 109.8 . . ? C12 C13 H13 109.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C16 C15 120.7(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C15 C20 C19 120.7(7) . . ? C15 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C18 C17 C16 119.7(7) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C15 C14 C13 112.8(5) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O1 C1 C2 113.1(6) . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C19 C18 C17 120.0(7) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.4(8) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? H25 O3 H26 116(10) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O5 C21 1.235(8) . ? O1 C1 1.429(9) . ? O1 H1 0.8200 . ? O4 C12 1.230(8) . ? O2 C2 1.443(8) . ? O2 H27 0.73(12) . ? N1 C12 1.329(8) . ? N1 C3 1.463(7) . ? N1 H24 0.8600 . ? N2 C21 1.348(8) . ? N2 C13 1.470(7) . ? N2 H2A 0.8600 . ? C21 C22 1.521(8) . ? C3 C4 1.524(8) . ? C3 C2 1.535(8) . ? C3 H3 0.9800 . ? C4 C5 1.520(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C12 C13 1.537(8) . ? C9 C8 1.514(8) . ? C9 C10 1.524(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C15 C20 1.377(10) . ? C15 C16 1.390(9) . ? C15 C14 1.515(8) . ? C2 C1 1.492(8) . ? C2 H2C 0.9800 . ? C8 C7 1.513(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C22 C23 1.524(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C10 C11 1.513(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C5 C6 1.515(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C6 1.514(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C13 C14 1.531(9) . ? C13 H13 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C16 C17 1.388(9) . ? C16 H16 0.9300 . ? C20 C19 1.385(9) . ? C20 H20 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C17 C18 1.380(11) . ? C17 H17 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C18 C19 1.366(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? O3 H25 0.84(12) . ? O3 H26 0.98(10) . ?