#------------------------------------------------------------------------------ #$Date: 2022-03-03 20:26:56 +0000 (Thu, 03 Mar 2022) $ #$Revision: 273249 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/93/4519342.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_4519342 loop_ _publ_author_name 'Wang, Chang-An' 'Rahman, Md. Mahbubur' 'Bisz, Elwira' 'Dziuk, B\/la\.zej' 'Szostak, Roman' 'Szostak, Michal' _publ_section_title ; Palladium-NHC (NHC = N-heterocyclic Carbene)-Catalyzed Suzuki--Miyaura Cross-Coupling of Alkyl Amides ; _journal_issue 4 _journal_name_full 'ACS Catalysis' _journal_page_first 2426 _journal_page_last 2433 _journal_paper_doi 10.1021/acscatal.1c05738 _journal_volume 12 _journal_year 2022 _chemical_formula_sum 'C16 H17 N3 O3' _chemical_formula_weight 299.32 _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 98.806(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.5366(15) _cell_length_b 9.0589(8) _cell_length_c 30.020(3) _cell_measurement_reflns_used 1705 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.4740 _cell_measurement_theta_min 2.0100 _cell_volume 3100.4(6) _computing_cell_refinement 'CrysAlisPro (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2014)' _computing_data_reduction 'CrysAlisPro (Rigaku OD, 2015)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 15.9718 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'KM4 with Eos CCD' _diffrn_measurement_method \w--scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_unetI/netI 0.1731 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 11578 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 1.813 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SCALE3 ABSPACK (Rigaku Oxford Diffraction, 2015). ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.367 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 6087 _refine_ls_number_restraints 384 _refine_ls_restrained_S_all 0.957 _refine_ls_R_factor_all 0.2512 _refine_ls_R_factor_gt 0.1168 _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^)+(0.1347P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2691 _refine_ls_wR_factor_ref 0.3405 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2120 _reflns_number_total 6087 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c05738_si_002.cif _cod_data_source_block B18_MR42_a _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4519342 _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. ; _exptl_absorpt_special_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _shelx_res_file ; B18_MR42_a.res created by SHELXL-2014/7 TITL B18_MR42_a.res in P2(1)/n REM Old TITL B18_MR42 in P2(1)/m REM SHELXT solution in P2(1)/n REM R1 0.295, Rweak 0.428, Alpha 0.084, Orientation as input REM Formula found by SHELXT: C34 N4 O6 CELL 0.71073 11.5366 9.0589 30.0199 90.000 98.806 90.000 ZERR 8.000 0.0015 0.0008 0.0030 0.000 0.010 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 128 136 24 24 OMIT 0 52 OMIT -1 2 1 OMIT -2 2 1 ACTA HTAB CONF L.S. 20 BOND $H LIST 6 FMAP 2 PLAN -20 SIMU 0.01 C1A > C16B DELU 0.01 C1A > C16B ISOR 0.01 C1A > C16B WGHT 0.134700 FVAR 0.27542 N1A 3 0.957387 0.471049 0.359988 11.00000 0.06958 0.02819 = 0.05661 0.00320 -0.00061 -0.00010 N1B 3 0.500828 0.865132 0.386601 11.00000 0.06315 0.02797 = 0.05432 -0.00400 -0.00043 0.00338 N2A 3 0.829938 0.671253 0.351245 11.00000 0.06041 0.04168 = 0.06415 0.00548 0.01348 0.00558 N2B 3 0.470913 1.064248 0.431862 11.00000 0.08736 0.03522 = 0.07247 -0.00660 0.00851 0.00183 N3A 3 0.888619 0.553935 0.287403 11.00000 0.06763 0.04117 = 0.05855 0.00505 0.00981 0.00873 N3B 3 0.654228 0.941555 0.441002 11.00000 0.07627 0.05970 = 0.07460 -0.02038 -0.00482 0.01190 O1A 4 1.087940 0.647344 0.387024 11.00000 0.08203 0.05067 = 0.09564 0.00031 0.00326 -0.02565 O1B 4 0.519491 1.040690 0.335413 11.00000 0.10469 0.04998 = 0.06894 0.00377 -0.00391 -0.02394 O2A 4 1.034969 0.241515 0.366277 11.00000 0.06453 0.02527 = 0.06963 -0.00612 0.00329 0.01036 O2B 4 0.528259 0.635954 0.360285 11.00000 0.07336 0.02802 = 0.05838 0.00219 0.01429 -0.00089 O3A 4 0.848155 0.271764 0.330601 11.00000 0.06846 0.04199 = 0.08882 -0.01122 -0.00350 0.00153 O3B 4 0.503371 0.665232 0.433143 11.00000 0.10517 0.04512 = 0.04914 0.00644 0.01279 -0.00172 C1A 1 1.044100 0.529006 0.392953 11.00000 0.05582 0.03828 = 0.05488 -0.01056 -0.00347 0.00440 C1B 1 0.473291 0.922625 0.342631 11.00000 0.04761 0.04183 = 0.05753 0.00135 0.01026 0.00117 C2A 1 1.077971 0.445526 0.435901 11.00000 0.06184 0.04983 = 0.05120 -0.00401 0.00104 0.00438 C2B 1 0.389527 0.845665 0.309011 11.00000 0.05280 0.03174 = 0.06096 -0.00481 0.00279 0.00661 C3A 1 0.995634 0.366441 0.454843 11.00000 0.08019 0.05397 = 0.06129 -0.00213 0.01000 0.00972 AFIX 43 H3A 2 0.919737 0.357672 0.439334 11.00000 -1.20000 AFIX 0 C3B 1 0.294200 0.771247 0.320897 11.00000 0.05150 0.04337 = 0.06692 0.00033 0.00681 0.00744 AFIX 43 H3B 2 0.285771 0.762843 0.351110 11.00000 -1.20000 AFIX 0 C4A 1 1.024701 0.299216 0.497068 11.00000 0.10803 0.05017 = 0.06908 -0.00691 0.02161 0.00542 AFIX 43 H4A 2 0.968616 0.249118 0.510427 11.00000 -1.20000 AFIX 0 C4B 1 0.212435 0.710083 0.288507 11.00000 0.06035 0.04353 = 0.08041 -0.00259 -0.00005 0.00341 AFIX 43 H4B 2 0.148405 0.660668 0.296826 11.00000 -1.20000 AFIX 0 C5A 1 1.138871 0.309728 0.518114 11.00000 0.11358 0.07137 = 0.07787 -0.00654 0.00434 0.01700 AFIX 43 H5A 2 1.160019 0.264222 0.545942 11.00000 -1.20000 AFIX 0 C5B 1 0.223841 0.720851 0.243345 11.00000 0.06780 0.04533 = 0.08204 -0.00620 -0.00611 0.00520 AFIX 43 H5B 2 0.168455 0.678738 0.221224 11.00000 -1.20000 AFIX 0 C6A 1 1.221566 0.384121 0.499684 11.00000 0.08364 0.08799 = 0.07433 -0.01327 -0.00256 0.02673 AFIX 43 H6A 2 1.298270 0.387625 0.514688 11.00000 -1.20000 AFIX 0 C6B 1 0.318898 0.795206 0.232036 11.00000 0.08178 0.05347 = 0.06539 -0.00341 0.00218 0.00533 AFIX 43 H6B 2 0.327852 0.802964 0.201859 11.00000 -1.20000 AFIX 0 C7A 1 1.192236 0.456060 0.458035 11.00000 0.07345 0.07447 = 0.06402 -0.01527 -0.00204 0.01127 AFIX 43 H7A 2 1.248217 0.509533 0.445601 11.00000 -1.20000 AFIX 0 C7B 1 0.399518 0.857197 0.263799 11.00000 0.06812 0.04438 = 0.06254 0.00155 0.00905 0.00446 AFIX 43 H7B 2 0.462488 0.908232 0.255228 11.00000 -1.20000 AFIX 0 C8A 1 0.888884 0.570543 0.330264 11.00000 0.04554 0.02507 = 0.04794 0.00530 0.00731 -0.00486 C8B 1 0.545804 0.963004 0.422167 11.00000 0.06101 0.03618 = 0.06059 0.00121 0.00881 0.00218 C9A 1 0.762939 0.762313 0.323065 11.00000 0.05749 0.03763 = 0.08513 0.00397 0.00931 0.00737 AFIX 43 H9A 2 0.720860 0.835707 0.335213 11.00000 -1.20000 AFIX 0 C9B 1 0.515988 1.154673 0.466170 11.00000 0.10312 0.05405 = 0.08189 -0.00434 0.03365 -0.00158 AFIX 43 H9B 2 0.468501 1.228961 0.474863 11.00000 -1.20000 AFIX 0 C10A 1 0.753850 0.752281 0.278002 11.00000 0.07048 0.04316 = 0.07756 0.01865 -0.00212 0.00662 AFIX 43 H10A 2 0.704920 0.815112 0.259156 11.00000 -1.20000 AFIX 0 C10B 1 0.626548 1.141951 0.488303 11.00000 0.10669 0.06000 = 0.07653 -0.00548 0.01710 -0.00902 AFIX 43 H10B 2 0.655278 1.205822 0.511655 11.00000 -1.20000 AFIX 0 C11A 1 0.819084 0.646423 0.260827 11.00000 0.08097 0.05748 = 0.06652 0.00907 0.00229 -0.00259 AFIX 43 H11A 2 0.814930 0.638571 0.229734 11.00000 -1.20000 AFIX 0 C11B 1 0.694560 1.031881 0.475132 11.00000 0.09447 0.06562 = 0.07875 -0.00250 -0.00706 -0.00564 AFIX 43 H11B 2 0.770570 1.019372 0.490198 11.00000 -1.20000 AFIX 0 C12A 1 0.938687 0.316955 0.350853 11.00000 0.05857 0.02705 = 0.04809 -0.00514 0.00632 0.00353 C12B 1 0.508095 0.707935 0.396665 11.00000 0.06587 0.03229 = 0.05188 0.00854 0.01014 -0.00063 C13A 1 1.033613 0.075005 0.368470 11.00000 0.08181 0.03048 = 0.06480 -0.00550 0.00210 0.00452 C13B 1 0.524786 0.468023 0.359724 11.00000 0.06223 0.02627 = 0.06773 0.00037 0.01421 -0.00228 C14A 1 1.013068 0.012476 0.321537 11.00000 0.09675 0.03787 = 0.06927 -0.00516 0.01005 0.00579 AFIX 137 H14A 2 0.939472 0.047809 0.305902 11.00000 -1.50000 H14B 2 1.011390 -0.093341 0.323050 11.00000 -1.50000 H14C 2 1.075220 0.043029 0.305687 11.00000 -1.50000 AFIX 0 C14B 1 0.626612 0.411430 0.391920 11.00000 0.07196 0.03241 = 0.09328 0.01163 0.01205 0.00781 AFIX 137 H14D 2 0.634924 0.307241 0.387493 11.00000 -1.50000 H14E 2 0.613565 0.429589 0.422267 11.00000 -1.50000 H14F 2 0.696816 0.461074 0.386702 11.00000 -1.50000 AFIX 0 C15A 1 1.156124 0.044131 0.393275 11.00000 0.09837 0.05394 = 0.11115 0.00243 -0.02461 0.02629 AFIX 137 H15A 2 1.165761 -0.060170 0.398157 11.00000 -1.50000 H15B 2 1.166867 0.094261 0.421785 11.00000 -1.50000 H15C 2 1.213159 0.078792 0.375557 11.00000 -1.50000 AFIX 0 C15B 1 0.407820 0.414670 0.370044 11.00000 0.07205 0.04153 = 0.09102 -0.00405 0.01749 -0.00288 AFIX 137 H15D 2 0.345870 0.467256 0.351658 11.00000 -1.50000 H15E 2 0.403215 0.431884 0.401279 11.00000 -1.50000 H15F 2 0.399984 0.310936 0.363760 11.00000 -1.50000 AFIX 0 C16A 1 0.939240 0.027827 0.396169 11.00000 0.13097 0.03865 = 0.08617 0.00432 0.03525 -0.00567 AFIX 137 H16A 2 0.864355 0.064360 0.382155 11.00000 -1.50000 H16B 2 0.957339 0.067452 0.426086 11.00000 -1.50000 H16C 2 0.936758 -0.077961 0.397663 11.00000 -1.50000 AFIX 0 C16B 1 0.537093 0.439548 0.311322 11.00000 0.09565 0.03434 = 0.08026 -0.00447 0.02759 -0.01127 AFIX 137 H16D 2 0.528824 0.335787 0.305145 11.00000 -1.50000 H16E 2 0.612958 0.471977 0.305946 11.00000 -1.50000 H16F 2 0.477355 0.492702 0.291975 11.00000 -1.50000 AFIX 0 HKLF 4 REM B18_MR42_a.res in P2(1)/n REM R1 = 0.1168 for 2120 Fo > 4sig(Fo) and 0.2512 for all 6087 data REM 403 parameters refined using 384 restraints END WGHT 0.1347 0.0000 REM Instructions for potential hydrogen bonds HTAB C14A O3A HTAB C14B O3B HTAB C15B O3B HTAB C16A O3A REM Highest difference peak 0.367, deepest hole -0.398, 1-sigma level 0.090 Q1 1 0.4869 0.6626 0.4599 11.00000 0.05 0.37 Q2 1 1.1572 0.4441 0.4195 11.00000 0.05 0.35 Q3 1 1.1629 0.2926 0.3115 11.00000 0.05 0.33 Q4 1 0.5379 1.1405 0.5086 11.00000 0.05 0.32 Q5 1 1.0420 0.2856 0.3054 11.00000 0.05 0.32 Q6 1 0.4094 0.6731 0.4401 11.00000 0.05 0.31 Q7 1 1.0366 0.3641 0.2171 11.00000 0.05 0.31 Q8 1 0.8426 0.2724 0.3738 11.00000 0.05 0.29 Q9 1 1.0398 0.0608 0.4028 11.00000 0.05 0.28 Q10 1 0.9116 0.2751 0.3087 11.00000 0.05 0.28 Q11 1 1.0992 0.3591 0.2728 11.00000 0.05 0.28 Q12 1 1.0565 0.4508 0.4585 11.00000 0.05 0.28 Q13 1 0.9653 0.6594 0.4312 11.00000 0.05 0.27 Q14 1 0.8763 0.5775 0.1974 11.00000 0.05 0.26 Q15 1 0.7465 0.7683 0.3517 11.00000 0.05 0.26 Q16 1 0.8436 0.6572 0.3936 11.00000 0.05 0.26 Q17 1 0.2046 0.7160 0.2597 11.00000 0.05 0.26 Q18 1 0.6353 0.7017 0.3751 11.00000 0.05 0.26 Q19 1 0.8251 0.6573 0.3075 11.00000 0.05 0.26 Q20 1 1.2822 0.4430 0.4857 11.00000 0.05 0.25 ; _shelx_res_checksum 46701 _shelx_hkl_file ; 0 0 -3 0.46 0.76 0 0 3 1.14 0.89 0 0 -4 1466.53 30.76 0 0 4 1481.19 31.26 0 0 5 0.51 1.30 0 0 -5 1.55 1.87 0 0 6 456.35 21.31 0 0 -6 465.56 21.31 0 0 7 30.57 7.81 0 0 -7 31.47 8.33 0 0 8 363.30 22.64 0 0 -8 347.89 21.97 0 0 -9 2.17 1.51 0 0 -10 136.37 14.92 0 0 -11 2.41 2.83 0 0 -12 4.94 2.89 0 0 13 0.28 1.01 0 0 -13 0.58 2.39 0 0 -14 13.66 7.06 0 0 14 15.27 5.44 0 0 15 -0.05 1.25 0 0 16 101.01 11.95 0 0 17 0.95 1.83 0 0 18 84.79 11.71 0 0 19 0.23 2.44 0 0 20 3.94 3.24 0 0 21 1.09 0.98 0 0 22 0.55 1.83 0 0 23 0.65 1.85 0 0 24 48.70 10.06 0 0 25 -1.54 2.62 0 0 26 -0.13 1.49 0 0 27 1.42 1.02 0 0 28 61.16 12.62 0 0 29 1.97 3.11 0 0 30 12.54 6.26 0 0 31 1.26 1.06 0 0 32 11.93 5.29 0 0 33 -0.93 2.87 0 0 34 1.27 3.39 0 0 35 -3.01 2.77 0 0 36 1.79 3.53 0 0 37 -0.18 1.23 0 1 0 0.38 0.46 0 -1 0 -0.12 0.55 0 1 -1 77.79 5.36 0 -1 1 83.29 5.71 0 -1 1 78.32 6.30 0 1 -2 201.54 10.19 0 -1 2 198.20 10.76 0 1 -3 168.19 11.13 0 -1 3 180.87 11.80 0 -1 -4 223.20 9.83 0 -1 4 230.43 14.79 0 1 -4 193.58 13.46 0 -1 5 6.73 3.13 0 -1 -5 5.48 1.75 0 1 -5 4.17 2.37 0 1 -6 49.71 7.94 0 -1 -6 41.36 5.38 0 -1 6 45.68 8.58 0 1 -7 110.64 12.45 0 -1 -7 102.43 9.86 0 -1 7 101.55 12.61 0 -1 -8 374.24 20.35 0 -1 8 376.54 24.72 0 1 -8 378.12 23.96 0 -1 9 92.94 12.93 0 -1 -9 100.45 11.11 0 1 -9 119.48 14.53 0 -1 -10 31.80 6.77 0 -1 10 26.29 7.33 0 1 -10 34.40 8.59 0 1 -11 447.60 29.44 0 -1 11 437.54 30.33 0 -1 -11 391.67 24.39 0 1 -12 12.88 5.65 0 -1 12 19.86 6.92 0 -1 -12 16.87 5.10 0 -1 12 16.57 4.49 0 -1 -13 0.47 1.20 0 1 13 -0.09 1.62 0 1 -13 0.41 1.33 0 -1 13 0.71 1.86 0 1 14 5.82 2.81 0 -1 -14 3.06 0.53 0 -1 14 3.40 2.62 0 -1 -15 140.61 17.54 0 -1 15 130.37 13.89 0 1 15 129.77 13.42 0 1 16 10.37 4.33 0 -1 16 7.05 4.00 0 -1 -16 15.60 6.81 0 -1 17 24.31 6.67 0 1 17 25.00 5.91 0 -1 18 1.44 1.83 0 1 18 1.78 0.78 0 1 19 21.45 6.03 0 -1 19 19.29 5.76 0 -1 20 34.38 8.98 0 1 20 45.58 8.79 0 1 21 63.88 10.83 0 -1 21 56.04 10.10 0 -1 21 67.51 10.76 0 -1 22 12.18 4.37 0 1 22 14.03 5.11 0 1 23 5.92 3.90 0 -1 23 6.27 3.83 0 1 24 5.18 3.68 0 -1 24 1.71 1.66 0 -1 25 9.06 4.86 0 1 25 6.38 2.62 0 -1 26 21.48 6.67 0 1 26 27.33 8.23 0 1 27 7.28 4.71 0 -1 27 5.55 3.51 0 1 28 0.48 2.79 0 -1 28 -0.11 2.15 0 -1 29 13.99 6.02 0 1 29 16.07 6.81 0 1 30 1.93 4.05 0 -1 30 0.63 0.38 0 1 31 4.17 1.84 0 -1 31 3.83 4.25 0 -1 32 6.75 5.04 0 1 32 10.82 7.00 0 -1 33 2.12 3.46 0 1 33 0.58 1.84 0 -1 34 1.98 3.48 0 1 34 4.12 3.86 0 1 35 -1.95 3.50 0 -1 35 -7.18 4.99 0 1 36 -0.09 1.21 0 1 37 -4.20 3.95 0 -2 0 239.02 16.66 0 2 0 240.03 17.46 0 -2 0 207.51 10.20 0 2 0 195.95 9.56 0 2 -1 5.48 2.06 0 2 1 4.92 1.33 0 -2 -1 4.92 0.98 0 -2 1 6.02 3.01 0 2 1 6.76 3.24 0 2 -1 4.75 2.30 0 -2 1 4.24 1.38 0 -2 2 913.86 31.49 0 -2 2 869.69 27.01 0 2 -2 840.04 25.50 0 2 -3 48.41 6.67 0 -2 3 50.95 7.14 0 2 -4 1348.51 37.23 0 -2 4 1381.37 39.48 0 2 -5 7.95 3.15 0 -2 5 5.53 2.77 0 2 -6 153.07 15.77 0 -2 6 154.56 16.25 0 -2 -6 146.47 8.90 0 -2 7 40.89 9.38 0 -2 -7 29.96 4.66 0 2 -7 50.79 9.21 0 -2 -7 56.38 6.80 0 -2 -8 238.78 14.34 0 -2 -8 373.08 19.01 0 -2 8 273.55 22.94 0 2 -8 356.71 24.60 0 -2 -9 57.71 7.43 0 -2 9 58.20 10.59 0 2 -9 72.48 11.97 0 -2 -10 2.83 1.82 0 -2 10 0.39 0.52 0 -2 -10 4.22 2.66 0 2 -10 2.51 3.67 0 -2 -11 32.36 8.01 0 -2 -11 18.50 4.93 0 -2 11 30.15 8.58 0 2 -11 14.11 7.22 0 2 12 27.21 5.67 0 -2 -12 25.11 5.79 0 2 13 7.14 3.80 0 -2 -13 2.24 2.20 0 -2 -14 -0.13 0.46 0 2 14 2.87 2.31 0 -2 14 1.58 1.84 0 -2 15 131.31 12.11 0 2 15 124.85 13.34 0 2 16 -0.13 0.71 0 -2 16 0.07 1.06 0 2 17 8.19 3.40 0 -2 17 8.93 3.48 0 -2 17 6.73 3.80 0 -2 18 -0.84 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-3 15 -1.41 2.22 -13 -3 14 4.49 5.44 -13 -3 13 7.93 6.30 -13 -3 12 2.84 3.34 -13 -3 11 -0.65 3.66 -13 -3 10 3.01 4.80 -13 -3 9 0.55 2.29 -13 -3 8 4.49 6.44 -13 -3 7 -0.42 0.07 -13 -3 6 -0.67 2.98 -13 -3 5 1.95 3.57 -13 -3 4 11.04 7.12 -13 -3 3 6.86 6.85 -13 -3 2 1.25 2.73 -13 -3 1 1.65 5.49 -13 -3 0 10.03 8.38 -13 -3 -1 4.75 5.92 -13 -3 -2 2.83 4.77 -13 -3 -3 5.15 4.48 -13 -3 -4 1.99 3.07 -13 -3 -5 4.26 4.50 -13 -3 -6 0.41 5.05 -13 -3 -7 3.40 4.56 -13 -4 15 6.90 6.00 -13 -4 14 12.44 8.37 -13 -4 13 10.00 7.16 -13 -4 12 0.62 0.99 -13 -4 11 4.26 5.36 -13 -4 10 7.43 6.16 -13 -4 9 3.09 3.73 -13 -4 8 2.31 2.51 -13 -4 7 2.37 4.28 -13 -4 6 -1.79 3.32 -13 -4 5 -1.09 2.98 -13 -4 4 1.00 1.62 -13 -4 3 4.67 4.79 -13 -4 2 3.77 5.14 -13 -4 1 0.61 3.61 -13 -4 0 -5.47 6.07 -13 -4 -1 2.57 3.24 -13 -4 -2 4.58 6.85 -13 -4 -3 9.48 7.74 -13 -4 -4 3.43 5.38 -13 -5 11 8.23 8.06 -13 -5 10 7.74 7.27 -13 -5 9 2.65 4.98 -13 -5 8 2.63 1.17 -13 -5 7 -0.59 4.54 -13 -5 6 2.83 4.46 -13 -5 5 -0.72 3.82 -13 -5 4 6.49 5.28 -13 -5 3 4.83 7.20 -13 -5 2 8.63 6.44 -13 -5 1 2.39 2.84 -13 -5 0 7.20 5.70 -14 0 15 -1.65 2.95 -14 0 14 0.32 2.30 -14 0 13 2.64 6.10 -14 0 12 3.05 5.90 -14 0 11 1.21 1.07 -14 0 10 4.11 5.14 -14 0 9 5.98 5.66 -14 0 8 3.34 5.64 -14 0 7 2.13 3.93 -14 0 6 3.23 4.57 -14 0 5 3.50 3.91 -14 0 4 -2.39 5.04 -14 0 3 -0.43 3.89 -14 0 2 3.56 2.44 -14 0 1 0.02 3.58 -14 0 0 1.03 3.64 -14 0 -1 -3.21 3.47 -14 0 -2 2.42 2.57 -14 0 -3 7.79 6.64 -14 0 -4 -0.33 4.97 -14 0 -5 -1.77 2.33 -14 1 16 0.36 1.57 -14 1 15 0.41 4.04 -14 -1 14 14.82 8.85 -14 1 14 -5.10 5.38 -14 -1 13 8.70 7.73 -14 1 13 7.17 4.17 -14 -1 12 5.59 5.58 -14 1 12 5.12 7.50 -14 -1 11 4.19 3.73 -14 1 11 10.09 7.95 -14 -1 10 1.12 6.31 -14 1 10 8.92 6.18 -14 -1 9 6.73 6.81 -14 1 9 -0.43 0.96 -14 -1 8 4.94 6.11 -14 1 8 -0.96 4.29 -14 -1 7 7.62 6.72 -14 1 7 0.03 3.07 -14 -1 6 1.31 5.02 -14 1 6 1.43 5.17 -14 -1 5 2.98 2.78 -14 1 5 4.62 4.41 -14 -1 4 -0.37 1.84 -14 1 4 -1.92 2.75 -14 -1 3 2.09 2.04 -14 1 3 0.81 3.56 -14 -1 2 0.79 3.07 -14 1 2 3.31 5.87 -14 -1 1 -1.04 2.10 -14 1 1 3.82 4.07 -14 -1 0 -1.23 3.94 -14 1 0 -2.21 2.75 -14 -1 -1 1.19 1.40 -14 1 -1 2.05 4.59 -14 -1 -2 3.85 6.08 -14 1 -2 -5.52 3.47 -14 -1 -3 5.90 7.26 -14 -2 11 2.02 3.87 -14 -2 10 6.92 8.37 -14 -2 9 13.78 8.19 -14 -2 8 2.49 5.88 -14 -2 7 7.44 6.13 -14 -2 6 4.85 5.49 -14 -2 5 5.01 6.38 -14 -2 4 8.69 7.28 -14 -2 3 10.76 8.46 -14 -2 2 4.68 6.88 -14 -2 1 0.42 4.32 -14 -2 0 0.51 2.25 TITL B18_MR42 in P2(1)/m REM P2(1)/m (#11 in standard setting) CELL 0.71073 11.536620 9.058948 30.019894 90.0000 98.8062 90.0000 ZERR 14.00 0.001487 0.000790 0.003001 0.0000 0.0105 0.0000 LATT 1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 154.00 140.00 14.00 14.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 90051 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1A N 0.9574(5) 0.4710(5) 0.35999(17) 0.0525(14) Uani 1 1 d . . . . . N1B N 0.5008(4) 0.8651(5) 0.38660(16) 0.0495(13) Uani 1 1 d . . . . . N2A N 0.8299(5) 0.6713(6) 0.35124(17) 0.0550(14) Uani 1 1 d . . . . . N2B N 0.4709(5) 1.0642(6) 0.43186(19) 0.0654(16) Uani 1 1 d . . . . . N3A N 0.8886(5) 0.5539(6) 0.28740(18) 0.0558(14) Uani 1 1 d . . . . . N3B N 0.6542(5) 0.9416(7) 0.4410(2) 0.0719(17) Uani 1 1 d . . . . . O1A O 1.0879(4) 0.6473(6) 0.38702(17) 0.0772(15) Uani 1 1 d . . . . . O1B O 0.5195(5) 1.0407(5) 0.33541(15) 0.0763(15) Uani 1 1 d . . . . . O2A O 1.0350(4) 0.2415(4) 0.36628(14) 0.0539(11) Uani 1 1 d . . . . . O2B O 0.5283(4) 0.6360(4) 0.36028(14) 0.0528(11) Uani 1 1 d . . . . . O3A O 0.8482(4) 0.2718(5) 0.33060(16) 0.0680(13) Uani 1 1 d . . . . . O3B O 0.5034(4) 0.6652(5) 0.43314(14) 0.0664(13) Uani 1 1 d . . . . . C1A C 1.0441(6) 0.5290(7) 0.3930(2) 0.0509(15) Uani 1 1 d . U . . . C1B C 0.4733(5) 0.9226(7) 0.3426(2) 0.0488(14) Uani 1 1 d . U . . . C2A C 1.0780(6) 0.4455(7) 0.4359(2) 0.0551(15) Uani 1 1 d . U . . . C2B C 0.3895(5) 0.8457(6) 0.3090(2) 0.0491(14) Uani 1 1 d . U . . . C3A C 0.9956(7) 0.3664(8) 0.4548(2) 0.0652(17) Uani 1 1 d . U . . . H3A H 0.9197 0.3577 0.4393 0.078 Uiso 1 1 calc R U . . . C3B C 0.2942(5) 0.7712(7) 0.3209(2) 0.0542(15) Uani 1 1 d . U . . . H3B H 0.2858 0.7628 0.3511 0.065 Uiso 1 1 calc R U . . . C4A C 1.0247(8) 0.2992(8) 0.4971(2) 0.0749(18) Uani 1 1 d . U . . . H4A H 0.9686 0.2491 0.5104 0.090 Uiso 1 1 calc R U . . . C4B C 0.2124(6) 0.7101(7) 0.2885(2) 0.0626(17) Uani 1 1 d . U . . . H4B H 0.1484 0.6607 0.2968 0.075 Uiso 1 1 calc R U . . . C5A C 1.1389(8) 0.3097(10) 0.5181(3) 0.089(2) Uani 1 1 d . U . . . H5A H 1.1600 0.2642 0.5459 0.106 Uiso 1 1 calc R U . . . C5B C 0.2238(6) 0.7209(7) 0.2433(3) 0.0669(17) Uani 1 1 d . U . . . H5B H 0.1685 0.6787 0.2212 0.080 Uiso 1 1 calc R U . . . C6A C 1.2216(7) 0.3841(9) 0.4997(3) 0.084(2) Uani 1 1 d . U . . . H6A H 1.2983 0.3876 0.5147 0.100 Uiso 1 1 calc R U . . . C6B C 0.3189(7) 0.7952(8) 0.2320(2) 0.0678(17) Uani 1 1 d . U . . . H6B H 0.3279 0.8030 0.2019 0.081 Uiso 1 1 calc R U . . . C7A C 1.1922(6) 0.4561(9) 0.4580(2) 0.0720(18) Uani 1 1 d . U . . . H7A H 1.2482 0.5095 0.4456 0.086 Uiso 1 1 calc R U . . . C7B C 0.3995(6) 0.8572(7) 0.2638(2) 0.0584(16) Uani 1 1 d . U . . . H7B H 0.4625 0.9082 0.2552 0.070 Uiso 1 1 calc R U . . . C8A C 0.8889(5) 0.5705(6) 0.33026(19) 0.0395(14) Uani 1 1 d . U . . . C8B C 0.5458(6) 0.9630(7) 0.4222(2) 0.0526(16) Uani 1 1 d . U . . . C9A C 0.7629(6) 0.7623(7) 0.3231(2) 0.0603(17) Uani 1 1 d . U . . . H9A H 0.7209 0.8357 0.3352 0.072 Uiso 1 1 calc R U . . . C9B C 0.5160(8) 1.1547(9) 0.4662(3) 0.078(2) Uani 1 1 d . U . . . H9B H 0.4685 1.2290 0.4749 0.093 Uiso 1 1 calc R U . . . C10A C 0.7538(6) 0.7523(7) 0.2780(2) 0.0651(18) Uani 1 1 d . U . . . H10A H 0.7049 0.8151 0.2592 0.078 Uiso 1 1 calc R U . . . C10B C 0.6265(8) 1.1420(9) 0.4883(3) 0.081(2) Uani 1 1 d . U . . . H10B H 0.6553 1.2058 0.5117 0.097 Uiso 1 1 calc R U . . . C11A C 0.8191(7) 0.6464(8) 0.2608(2) 0.0693(19) Uani 1 1 d . U . . . H11A H 0.8149 0.6386 0.2297 0.083 Uiso 1 1 calc R U . . . C11B C 0.6946(8) 1.0319(9) 0.4751(3) 0.082(2) Uani 1 1 d . U . . . H11B H 0.7706 1.0194 0.4902 0.098 Uiso 1 1 calc R U . . . C12A C 0.9387(6) 0.3170(6) 0.3509(2) 0.0448(15) Uani 1 1 d . U . . . C12B C 0.5081(6) 0.7079(7) 0.3967(2) 0.0499(16) Uani 1 1 d . U . . . C13A C 1.0336(6) 0.0750(7) 0.3685(2) 0.0600(17) Uani 1 1 d . U . . . C13B C 0.5248(6) 0.4680(6) 0.3597(2) 0.0516(15) Uani 1 1 d . U . . . C14A C 1.0131(7) 0.0125(7) 0.3215(2) 0.0682(19) Uani 1 1 d . U . . . H14A H 0.9395 0.0478 0.3059 0.102 Uiso 1 1 calc R U . . . H14B H 1.0114 -0.0933 0.3231 0.102 Uiso 1 1 calc R U . . . H14C H 1.0752 0.0430 0.3057 0.102 Uiso 1 1 calc R U . . . C14B C 0.6266(6) 0.4114(7) 0.3919(2) 0.0659(18) Uani 1 1 d . U . . . H14D H 0.6349 0.3072 0.3875 0.099 Uiso 1 1 calc R U . . . H14E H 0.6136 0.4296 0.4223 0.099 Uiso 1 1 calc R U . . . H14F H 0.6968 0.4611 0.3867 0.099 Uiso 1 1 calc R U . . . C15A C 1.1561(7) 0.0441(8) 0.3933(3) 0.092(3) Uani 1 1 d . U . . . H15A H 1.1658 -0.0602 0.3982 0.138 Uiso 1 1 calc R U . . . H15B H 1.1669 0.0943 0.4218 0.138 Uiso 1 1 calc R U . . . H15C H 1.2132 0.0788 0.3756 0.138 Uiso 1 1 calc R U . . . C15B C 0.4078(6) 0.4147(7) 0.3700(2) 0.0677(19) Uani 1 1 d . U . . . H15D H 0.3459 0.4673 0.3517 0.102 Uiso 1 1 calc R U . . . H15E H 0.4032 0.4319 0.4013 0.102 Uiso 1 1 calc R U . . . H15F H 0.4000 0.3109 0.3638 0.102 Uiso 1 1 calc R U . . . C16A C 0.9392(8) 0.0278(8) 0.3962(3) 0.083(2) Uani 1 1 d . U . . . H16A H 0.8644 0.0644 0.3822 0.125 Uiso 1 1 calc R U . . . H16B H 0.9573 0.0675 0.4261 0.125 Uiso 1 1 calc R U . . . H16C H 0.9368 -0.0780 0.3977 0.125 Uiso 1 1 calc R U . . . C16B C 0.5371(7) 0.4395(7) 0.3113(2) 0.0686(19) Uani 1 1 d . U . . . H16D H 0.5288 0.3358 0.3051 0.103 Uiso 1 1 calc R U . . . H16E H 0.6130 0.4720 0.3059 0.103 Uiso 1 1 calc R U . . . H16F H 0.4774 0.4927 0.2920 0.103 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 N1A 0.070(4) 0.028(3) 0.057(3) 0.003(2) -0.001(3) 0.000(3) N1B 0.063(3) 0.028(3) 0.054(3) -0.004(2) 0.000(2) 0.003(3) N2A 0.060(3) 0.042(3) 0.064(3) 0.005(3) 0.013(3) 0.006(3) N2B 0.087(4) 0.035(3) 0.072(4) -0.007(3) 0.009(3) 0.002(3) N3A 0.068(4) 0.041(3) 0.059(4) 0.005(3) 0.010(3) 0.009(3) N3B 0.076(4) 0.060(4) 0.075(4) -0.020(3) -0.005(3) 0.012(3) O1A 0.082(4) 0.051(3) 0.096(4) 0.000(3) 0.003(3) -0.026(3) O1B 0.105(4) 0.050(3) 0.069(3) 0.004(2) -0.004(3) -0.024(3) O2A 0.065(3) 0.025(2) 0.070(3) -0.006(2) 0.003(2) 0.010(2) O2B 0.073(3) 0.028(2) 0.058(3) 0.002(2) 0.014(2) -0.001(2) O3A 0.068(3) 0.042(3) 0.089(4) -0.011(2) -0.004(3) 0.002(2) O3B 0.105(4) 0.045(3) 0.049(3) 0.006(2) 0.013(3) -0.002(3) C1A 0.056(4) 0.038(3) 0.055(3) -0.011(3) -0.003(3) 0.004(3) C1B 0.048(3) 0.042(3) 0.058(3) 0.001(3) 0.010(3) 0.001(3) C2A 0.062(3) 0.050(3) 0.051(3) -0.004(3) 0.001(2) 0.004(3) C2B 0.053(3) 0.032(3) 0.061(3) -0.005(3) 0.003(3) 0.007(2) C3A 0.080(4) 0.054(4) 0.061(3) -0.002(3) 0.010(3) 0.010(3) C3B 0.051(3) 0.043(3) 0.067(3) 0.000(3) 0.007(3) 0.007(3) C4A 0.108(4) 0.050(3) 0.069(4) -0.007(3) 0.022(3) 0.005(4) C4B 0.060(3) 0.044(3) 0.080(4) -0.003(3) 0.000(3) 0.003(3) C5A 0.114(5) 0.071(4) 0.078(4) -0.007(4) 0.004(3) 0.017(4) C5B 0.068(4) 0.045(3) 0.082(4) -0.006(3) -0.006(3) 0.005(3) C6A 0.084(4) 0.088(5) 0.074(4) -0.013(4) -0.003(3) 0.027(4) C6B 0.082(4) 0.053(4) 0.065(3) -0.003(3) 0.002(3) 0.005(3) C7A 0.073(4) 0.074(4) 0.064(3) -0.015(3) -0.002(3) 0.011(3) C7B 0.068(4) 0.044(3) 0.063(3) 0.002(3) 0.009(3) 0.004(3) C8A 0.046(3) 0.025(3) 0.048(3) 0.005(3) 0.007(3) -0.005(3) C8B 0.061(4) 0.036(3) 0.061(4) 0.001(3) 0.009(3) 0.002(3) C9A 0.057(4) 0.038(3) 0.085(4) 0.004(3) 0.009(3) 0.007(3) C9B 0.103(5) 0.054(4) 0.082(4) -0.004(4) 0.034(4) -0.002(4) C10A 0.070(4) 0.043(3) 0.078(4) 0.019(3) -0.002(3) 0.007(3) C10B 0.107(5) 0.060(4) 0.077(4) -0.005(4) 0.017(4) -0.009(4) C11A 0.081(4) 0.057(4) 0.067(4) 0.009(3) 0.002(3) -0.003(4) C11B 0.094(5) 0.066(4) 0.079(4) -0.002(4) -0.007(4) -0.006(4) C12A 0.059(4) 0.027(3) 0.048(3) -0.005(3) 0.006(3) 0.004(3) C12B 0.066(4) 0.032(3) 0.052(4) 0.009(3) 0.010(3) -0.001(3) C13A 0.082(4) 0.030(3) 0.065(4) -0.006(3) 0.002(3) 0.005(3) C13B 0.062(4) 0.026(3) 0.068(4) 0.000(3) 0.014(3) -0.002(3) C14A 0.097(5) 0.038(4) 0.069(4) -0.005(3) 0.010(3) 0.006(4) C14B 0.072(4) 0.032(3) 0.093(5) 0.012(3) 0.012(3) 0.008(3) C15A 0.098(5) 0.054(5) 0.111(6) 0.002(4) -0.025(4) 0.026(4) C15B 0.072(4) 0.042(4) 0.091(5) -0.004(4) 0.017(4) -0.003(4) C16A 0.131(6) 0.039(4) 0.086(5) 0.004(4) 0.035(4) -0.006(4) C16B 0.096(5) 0.034(4) 0.080(4) -0.004(3) 0.028(4) -0.011(4) 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 C1A N1A C8A 118.4(5) . . ? C1A N1A C12A 124.9(5) . . ? C8A N1A C12A 116.4(5) . . ? C1B N1B C8B 118.5(5) . . ? C1B N1B C12B 123.6(5) . . ? C8B N1B C12B 116.8(5) . . ? C9A N2A C8A 113.9(5) . . ? C8B N2B C9B 113.5(6) . . ? C8A N3A C11A 115.5(6) . . ? C8B N3B C11B 116.0(7) . . ? C12A O2A C13A 121.1(5) . . ? C12B O2B C13B 119.6(5) . . ? O1A C1A N1A 119.9(6) . . ? O1A C1A C2A 121.0(6) . . ? N1A C1A C2A 119.0(6) . . ? O1B C1B N1B 116.4(6) . . ? O1B C1B C2B 123.5(6) . . ? N1B C1B C2B 120.0(6) . . ? C3A C2A C7A 120.2(7) . . ? C3A C2A C1A 120.8(6) . . ? C7A C2A C1A 118.9(6) . . ? C3B C2B C7B 118.6(6) . . ? C3B C2B C1B 121.5(6) . . ? C7B C2B C1B 119.7(6) . . ? C2A C3A C4A 121.0(7) . . ? C2A C3A H3A 119.5 . . ? C4A C3A H3A 119.5 . . ? C4B C3B C2B 120.3(6) . . ? C4B C3B H3B 119.8 . . ? C2B C3B H3B 119.8 . . ? C5A C4A C3A 117.8(8) . . ? C5A C4A H4A 121.1 . . ? C3A C4A H4A 121.1 . . ? C3B C4B C5B 120.7(7) . . ? C3B C4B H4B 119.7 . . ? C5B C4B H4B 119.7 . . ? C6A C5A C4A 122.2(8) . . ? C6A C5A H5A 118.9 . . ? C4A C5A H5A 118.9 . . ? C6B C5B C4B 118.4(7) . . ? C6B C5B H5B 120.8 . . ? C4B C5B H5B 120.8 . . ? C5A C6A C7A 120.4(8) . . ? C5A C6A H6A 119.8 . . ? C7A C6A H6A 119.8 . . ? C7B C6B C5B 121.3(7) . . ? C7B C6B H6B 119.3 . . ? C5B C6B H6B 119.3 . . ? C2A C7A C6A 118.5(8) . . ? C2A C7A H7A 120.8 . . ? C6A C7A H7A 120.8 . . ? C6B C7B C2B 120.7(7) . . ? C6B C7B H7B 119.7 . . ? C2B C7B H7B 119.7 . . ? N3A C8A N2A 128.1(5) . . ? N3A C8A N1A 117.8(5) . . ? N2A C8A N1A 114.0(5) . . ? N3B C8B N2B 128.5(6) . . ? N3B C8B N1B 116.6(6) . . ? N2B C8B N1B 114.9(6) . . ? N2A C9A C10A 122.9(6) . . ? N2A C9A H9A 118.6 . . ? C10A C9A H9A 118.6 . . ? C10B C9B N2B 123.1(8) . . ? C10B C9B H9B 118.5 . . ? N2B C9B H9B 118.5 . . ? C9A C10A C11A 117.7(6) . . ? C9A C10A H10A 121.2 . . ? C11A C10A H10A 121.2 . . ? C9B C10B C11B 117.5(8) . . ? C9B C10B H10B 121.2 . . ? C11B C10B H10B 121.2 . . ? N3A C11A C10A 121.9(7) . . ? N3A C11A H11A 119.0 . . ? C10A C11A H11A 119.0 . . ? N3B C11B C10B 121.4(8) . . ? N3B C11B H11B 119.3 . . ? C10B C11B H11B 119.3 . . ? O3A C12A O2A 128.3(5) . . ? O3A C12A N1A 121.6(6) . . ? O2A C12A N1A 110.0(5) . . ? O3B C12B O2B 130.4(6) . . ? O3B C12B N1B 120.5(6) . . ? O2B C12B N1B 108.8(5) . . ? C14A C13A O2A 109.7(5) . . ? C14A C13A C15A 113.0(6) . . ? O2A C13A C15A 101.0(5) . . ? C14A C13A C16A 112.4(6) . . ? O2A C13A C16A 108.4(5) . . ? C15A C13A C16A 111.6(6) . . ? C14B C13B C16B 112.7(6) . . ? C14B C13B C15B 113.4(6) . . ? C16B C13B C15B 111.3(5) . . ? C14B C13B O2B 108.6(5) . . ? C16B C13B O2B 100.1(5) . . ? C15B C13B O2B 109.9(5) . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13A C15A H15A 109.5 . . ? C13A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C13A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C13A C16A H16A 109.5 . . ? C13A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C13A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C13B C16B H16D 109.5 . . ? C13B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C13B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? 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 N1A C1A 1.397(7) . ? N1A C8A 1.420(7) . ? N1A C12A 1.433(7) . ? N1B C1B 1.409(7) . ? N1B C8B 1.423(8) . ? N1B C12B 1.455(7) . ? N2A C9A 1.339(8) . ? N2A C8A 1.350(7) . ? N2B C8B 1.323(8) . ? N2B C9B 1.356(9) . ? N3A C8A 1.295(7) . ? N3A C11A 1.336(8) . ? N3B C8B 1.306(8) . ? N3B C11B 1.338(9) . ? O1A C1A 1.210(7) . ? O1B C1B 1.229(7) . ? O2A C12A 1.326(7) . ? O2A C13A 1.510(7) . ? O2B C12B 1.323(7) . ? O2B C13B 1.522(7) . ? O3A C12A 1.197(7) . ? O3B C12B 1.170(7) . ? C1A C2A 1.494(8) . ? C1B C2B 1.463(8) . ? C2A C3A 1.380(9) . ? C2A C7A 1.386(9) . ? C2B C3B 1.383(8) . ? C2B C7B 1.384(8) . ? C3A C4A 1.400(9) . ? C3A H3A 0.9300 . ? C3B C4B 1.364(8) . ? C3B H3B 0.9300 . ? C4A C5A 1.374(11) . ? C4A H4A 0.9300 . ? C4B C5B 1.385(9) . ? C4B H4B 0.9300 . ? C5A C6A 1.354(11) . ? C5A H5A 0.9300 . ? C5B C6B 1.373(10) . ? C5B H5B 0.9300 . ? C6A C7A 1.405(10) . ? C6A H6A 0.9300 . ? C6B C7B 1.348(9) . ? C6B H6B 0.9300 . ? C7A H7A 0.9300 . ? C7B H7B 0.9300 . ? C9A C10A 1.344(9) . ? C9A H9A 0.9300 . ? C9B C10B 1.350(11) . ? C9B H9B 0.9300 . ? C10A C11A 1.368(9) . ? C10A H10A 0.9300 . ? C10B C11B 1.364(10) . ? C10B H10B 0.9300 . ? C11A H11A 0.9300 . ? C11B H11B 0.9300 . ? C13A C14A 1.503(9) . ? C13A C15A 1.519(10) . ? C13A C16A 1.529(10) . ? C13B C14B 1.493(9) . ? C13B C16B 1.504(9) . ? C13B C15B 1.509(9) . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8A N1A C1A O1A -25.7(9) . . . . ? C12A N1A C1A O1A 148.2(6) . . . . ? C8A N1A C1A C2A 152.0(5) . . . . ? C12A N1A C1A C2A -34.1(9) . . . . ? C8B N1B C1B O1B 19.9(8) . . . . ? C12B N1B C1B O1B -147.5(6) . . . . ? C8B N1B C1B C2B -157.4(6) . . . . ? C12B N1B C1B C2B 35.2(8) . . . . ? O1A C1A C2A C3A 142.8(7) . . . . ? N1A C1A C2A C3A -34.9(9) . . . . ? O1A C1A C2A C7A -33.2(9) . . . . ? N1A C1A C2A C7A 149.0(6) . . . . ? O1B C1B C2B C3B -142.6(7) . . . . ? N1B C1B C2B C3B 34.5(8) . . . . ? O1B C1B C2B C7B 31.8(9) . . . . ? N1B C1B C2B C7B -151.1(6) . . . . ? C7A C2A C3A C4A 1.8(10) . . . . ? C1A C2A C3A C4A -174.2(6) . . . . ? C7B C2B C3B C4B 0.4(9) . . . . ? C1B C2B C3B C4B 174.9(6) . . . . ? C2A C3A C4A C5A -2.5(10) . . . . ? C2B C3B C4B C5B 0.3(9) . . . . ? C3A C4A C5A C6A 1.1(12) . . . . ? C3B C4B C5B C6B -0.4(10) . . . . ? C4A C5A C6A C7A 1.0(13) . . . . ? C4B C5B C6B C7B -0.3(10) . . . . ? C3A C2A C7A C6A 0.3(10) . . . . ? C1A C2A C7A C6A 176.4(6) . . . . ? C5A C6A C7A C2A -1.7(11) . . . . ? C5B C6B C7B C2B 1.0(10) . . . . ? C3B C2B C7B C6B -1.0(9) . . . . ? C1B C2B C7B C6B -175.6(6) . . . . ? C11A N3A C8A N2A -1.6(9) . . . . ? C11A N3A C8A N1A 177.4(5) . . . . ? C9A N2A C8A N3A 0.7(9) . . . . ? C9A N2A C8A N1A -178.3(5) . . . . ? C1A N1A C8A N3A 122.5(6) . . . . ? C12A N1A C8A N3A -51.9(7) . . . . ? C1A N1A C8A N2A -58.4(7) . . . . ? C12A N1A C8A N2A 127.2(6) . . . . ? C11B N3B C8B N2B 1.3(11) . . . . ? C11B N3B C8B N1B -178.4(6) . . . . ? C9B N2B C8B N3B -0.4(10) . . . . ? C9B N2B C8B N1B 179.3(6) . . . . ? C1B N1B C8B N3B -113.3(7) . . . . ? C12B N1B C8B N3B 55.0(8) . . . . ? C1B N1B C8B N2B 66.9(7) . . . . ? C12B N1B C8B N2B -124.8(6) . . . . ? C8A N2A C9A C10A 1.1(9) . . . . ? C8B N2B C9B C10B -0.2(10) . . . . ? N2A C9A C10A C11A -1.9(10) . . . . ? N2B C9B C10B C11B -0.3(12) . . . . ? C8A N3A C11A C10A 0.7(10) . . . . ? C9A C10A C11A N3A 0.9(10) . . . . ? C8B N3B C11B C10B -1.7(11) . . . . ? C9B C10B C11B N3B 1.3(12) . . . . ? C13A O2A C12A O3A -13.3(10) . . . . ? C13A O2A C12A N1A 169.3(5) . . . . ? C1A N1A C12A O3A 161.5(6) . . . . ? C8A N1A C12A O3A -24.5(9) . . . . ? C1A N1A C12A O2A -20.9(8) . . . . ? C8A N1A C12A O2A 153.1(5) . . . . ? C13B O2B C12B O3B 12.6(10) . . . . ? C13B O2B C12B N1B -172.4(5) . . . . ? C1B N1B C12B O3B -161.7(6) . . . . ? C8B N1B C12B O3B 30.7(9) . . . . ? C1B N1B C12B O2B 22.8(8) . . . . ? C8B N1B C12B O2B -144.9(5) . . . . ? C12A O2A C13A C14A 67.4(7) . . . . ? C12A O2A C13A C15A -173.1(6) . . . . ? C12A O2A C13A C16A -55.7(7) . . . . ? C12B O2B C13B C14B -68.4(7) . . . . ? C12B O2B C13B C16B 173.3(5) . . . . ? C12B O2B C13B C15B 56.1(7) . . . . ?