#------------------------------------------------------------------------------ #$Date: 2020-05-13 02:15:35 +0300 (Wed, 13 May 2020) $ #$Revision: 251987 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038342.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_4038342 loop_ _publ_author_name 'Tripathi, Shashank' 'Ambule, Mayur Diliprao' 'Srivastava, Ajay Kumar' _publ_section_title ; Construction of Highly Functionalized Piperazinones via post-Ugi Cyclization and Diastereoselective Nucleophilic Addition. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00108 _journal_year 2020 _chemical_formula_moiety 'C34 H31 N3 O2' _chemical_formula_sum 'C34 H31 N3 O2' _chemical_formula_weight 513.62 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 98.619(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4834(8) _cell_length_b 10.9838(9) _cell_length_c 26.644(2) _cell_measurement_reflns_used 5850 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.428 _cell_measurement_theta_min 2.414 _cell_volume 2744.0(4) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-100' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_unetI/netI 0.0549 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 16418 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.414 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_density_diffrn 1.243 _exptl_crystal_description block _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_min 0.350 _refine_diff_density_max 0.224 _refine_diff_density_min -0.160 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef 0.0088(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 4787 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0519 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1461 _refine_ls_wR_factor_ref 0.1791 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2984 _reflns_number_total 4787 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo0c00108_si_002.cif _cod_data_source_block KA771_0m _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4038342 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.967 _shelx_estimated_absorpt_t_max 0.973 _shelx_res_file ; TITL KA771_0m_a.res in P2(1)/c KA771_0m.res created by SHELXL-2018/3 at 11:11:09 on 29-Jul-2019 CELL 0.71073 9.4834 10.9838 26.6437 90.0000 98.6186 90.0000 ZERR 4.00 0.0008 0.0009 0.0023 0.0000 0.0026 0.0000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O UNIT 136 124 12 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 20.000 ACTA L.S. 40 FMAP 2 OMIT -3 50 PLAN -5 0 0.00 HTAB BOND $H CONF SIZE 0.43 0.38 0.35 WGHT 0.100000 EXTI 0.008817 FVAR 0.37947 C1 1 0.718020 0.563931 0.806921 11.00000 0.04755 0.04541 = 0.04055 0.00634 0.00931 0.00484 C2 1 0.824576 0.526080 0.844715 11.00000 0.06077 0.06500 = 0.05733 0.00088 0.00268 0.02266 AFIX 43 H2 2 0.886555 0.464521 0.838090 11.00000 -1.20000 AFIX 0 C3 1 0.840058 0.578612 0.892192 11.00000 0.07102 0.10186 = 0.05092 -0.00269 -0.00705 0.02234 AFIX 43 H3 2 0.911992 0.551492 0.917302 11.00000 -1.20000 AFIX 0 C4 1 0.751803 0.669507 0.902919 11.00000 0.08229 0.09588 = 0.04487 -0.01304 0.00715 0.01042 AFIX 43 H4 2 0.763921 0.705069 0.934954 11.00000 -1.20000 AFIX 0 C5 1 0.645076 0.707978 0.866060 11.00000 0.07421 0.07082 = 0.05183 -0.00368 0.01742 0.01804 AFIX 43 H5 2 0.583811 0.769745 0.873046 11.00000 -1.20000 AFIX 0 C6 1 0.628164 0.655509 0.818680 11.00000 0.05558 0.05918 = 0.04286 0.00519 0.00902 0.01209 AFIX 43 H6 2 0.554778 0.682121 0.794004 11.00000 -1.20000 AFIX 0 C7 1 0.708187 0.509907 0.754490 11.00000 0.04953 0.04914 = 0.04581 0.00188 0.00871 0.01123 AFIX 23 H7A 2 0.794066 0.530679 0.740667 11.00000 -1.20000 H7AB 2 0.704746 0.421930 0.757233 11.00000 -1.20000 AFIX 0 C8 1 0.459238 0.492893 0.719676 11.00000 0.05485 0.03459 = 0.03736 -0.00178 0.01195 0.00227 C9 1 0.326625 0.540841 0.686592 11.00000 0.04860 0.03170 = 0.04039 0.00170 0.00687 -0.00757 AFIX 13 H9 2 0.274281 0.470768 0.670417 11.00000 -1.20000 AFIX 0 C10 1 0.463361 0.713955 0.666343 11.00000 0.05073 0.03424 = 0.03660 -0.00245 0.00811 -0.00743 AFIX 23 H10A 2 0.426701 0.758449 0.693068 11.00000 -1.20000 H10B 2 0.475993 0.770969 0.639572 11.00000 -1.20000 AFIX 0 C11 1 0.605436 0.656726 0.687205 11.00000 0.05013 0.04196 = 0.03363 -0.00171 0.00732 -0.00631 AFIX 13 H11 2 0.660249 0.717219 0.709073 11.00000 -1.20000 AFIX 0 C12 1 0.322357 0.592996 0.597143 11.00000 0.06345 0.04330 = 0.04091 -0.00536 0.00761 -0.00853 C13 1 0.363743 0.680076 0.558619 11.00000 0.05620 0.04780 = 0.03416 -0.00113 0.00501 -0.00497 C14 1 0.460795 0.644335 0.527911 11.00000 0.07114 0.06854 = 0.04430 -0.00218 0.00703 -0.00003 AFIX 43 H14 2 0.503537 0.568154 0.532599 11.00000 -1.20000 AFIX 0 C15 1 0.495404 0.719904 0.490348 11.00000 0.08160 0.10341 = 0.05549 0.00344 0.02382 -0.01599 AFIX 43 H15 2 0.560903 0.694788 0.469761 11.00000 -1.20000 AFIX 0 C16 1 0.433138 0.831690 0.483513 11.00000 0.11617 0.09089 = 0.05996 0.02208 0.02215 -0.02237 AFIX 43 H16 2 0.455415 0.882651 0.457952 11.00000 -1.20000 AFIX 0 C17 1 0.337491 0.869315 0.514302 11.00000 0.12549 0.06743 = 0.07361 0.02529 0.01623 0.01271 AFIX 43 H17 2 0.295722 0.945905 0.509758 11.00000 -1.20000 AFIX 0 C18 1 0.303343 0.792927 0.552155 11.00000 0.08810 0.06032 = 0.05890 0.01097 0.01987 0.01455 AFIX 43 H18 2 0.239210 0.818608 0.573166 11.00000 -1.20000 AFIX 0 C19 1 0.227834 0.607407 0.717943 11.00000 0.04275 0.03861 = 0.04277 0.00432 0.01023 -0.00611 C20 1 0.246390 0.606181 0.770456 11.00000 0.06388 0.06566 = 0.04791 0.01323 0.01472 0.01941 AFIX 43 H20 2 0.319257 0.559760 0.788291 11.00000 -1.20000 AFIX 0 C21 1 0.157935 0.673109 0.796697 11.00000 0.07303 0.07692 = 0.04647 0.00634 0.02121 0.01614 AFIX 43 H21 2 0.172949 0.670625 0.831986 11.00000 -1.20000 AFIX 0 C22 1 0.048359 0.743319 0.772350 11.00000 0.04794 0.04903 = 0.06636 0.00134 0.01921 -0.00463 C23 1 0.028647 0.741291 0.720179 11.00000 0.04330 0.06228 = 0.06634 0.00637 0.00700 0.00502 AFIX 43 H23 2 -0.045598 0.786390 0.702433 11.00000 -1.20000 AFIX 0 C24 1 0.115377 0.674546 0.693252 11.00000 0.04900 0.06475 = 0.04753 0.00613 0.00274 -0.00164 AFIX 43 H24 2 0.097755 0.674838 0.657963 11.00000 -1.20000 AFIX 0 C25 1 -0.042735 0.821198 0.800798 11.00000 0.06562 0.07133 = 0.09348 -0.01040 0.02937 0.00474 AFIX 137 H25A 2 0.001977 0.899064 0.807681 11.00000 -1.50000 H25B 2 -0.053814 0.782250 0.832227 11.00000 -1.50000 H25C 2 -0.134683 0.832135 0.780699 11.00000 -1.50000 AFIX 0 C26 1 0.690799 0.624323 0.645849 11.00000 0.04249 0.05678 = 0.03694 -0.00356 0.00732 -0.00552 C27 1 0.724252 0.512797 0.628757 11.00000 0.05280 0.06365 = 0.04776 -0.01063 0.01239 -0.00338 AFIX 43 H27 2 0.697256 0.438952 0.641507 11.00000 -1.20000 AFIX 0 C28 1 0.863541 0.426003 0.563486 11.00000 0.07831 0.12094 = 0.07445 -0.04030 0.02362 0.00970 AFIX 137 H28A 2 0.839489 0.437412 0.527498 11.00000 -1.50000 H28B 2 0.825135 0.349952 0.572955 11.00000 -1.50000 H28C 2 0.965386 0.425293 0.572607 11.00000 -1.50000 AFIX 0 C29 1 0.822464 0.646258 0.581634 11.00000 0.04926 0.09477 = 0.04015 0.00055 0.00881 -0.01019 C30 1 0.896097 0.705734 0.546309 11.00000 0.05941 0.13974 = 0.04735 -0.00060 0.01352 -0.01264 AFIX 43 H30 2 0.942989 0.662565 0.523723 11.00000 -1.20000 AFIX 0 C31 1 0.894652 0.830347 0.547143 11.00000 0.08174 0.12929 = 0.06896 0.02568 0.01284 -0.03731 AFIX 43 H31 2 0.942140 0.872288 0.524375 11.00000 -1.20000 AFIX 0 C32 1 0.826400 0.896005 0.580006 11.00000 0.08159 0.09514 = 0.07502 0.02356 0.00372 -0.02444 AFIX 43 H32 2 0.828554 0.980614 0.579037 11.00000 -1.20000 AFIX 0 C33 1 0.754953 0.838507 0.614309 11.00000 0.06358 0.07229 = 0.05859 0.01048 0.00147 -0.01579 AFIX 43 H33 2 0.708644 0.883661 0.636461 11.00000 -1.20000 AFIX 0 C34 1 0.752401 0.711218 0.615656 11.00000 0.04420 0.06932 = 0.04041 0.00170 0.00111 -0.01076 N1 3 0.584508 0.550579 0.718997 11.00000 0.04752 0.04082 = 0.03829 0.00220 0.00898 0.00245 N2 3 0.362322 0.620095 0.646405 11.00000 0.04942 0.03758 = 0.03469 -0.00009 0.00797 -0.00683 N3 3 0.803847 0.525052 0.589857 11.00000 0.05853 0.09073 = 0.05004 -0.01810 0.01711 0.00554 O1 4 0.448383 0.405502 0.747402 11.00000 0.07312 0.04071 = 0.06108 0.01509 0.01289 0.00162 O2 4 0.253783 0.501486 0.583655 11.00000 0.13549 0.07072 = 0.05172 -0.00491 -0.00048 -0.04783 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA771_0m_a.res in P2(1)/c REM wR2 = 0.1791, GooF = S = 1.089, Restrained GooF = 1.089 for all data REM R1 = 0.0519 for 2984 Fo > 4sig(Fo) and 0.1018 for all 4787 data REM 355 parameters refined using 0 restraints END WGHT 0.0513 0.9930 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y+1/2, -z+3/2 HTAB C10 O1_$1 HTAB C11 O1_$1 REM Highest difference peak 0.224, deepest hole -0.160, 1-sigma level 0.041 Q1 1 0.6889 0.4073 0.6306 11.00000 0.05 0.22 Q2 1 0.3440 0.4993 0.5892 11.00000 0.05 0.20 Q3 1 0.9480 0.6067 0.5224 11.00000 0.05 0.17 Q4 1 0.6388 0.6577 0.6626 11.00000 0.05 0.16 Q5 1 0.1400 0.6196 0.8392 11.00000 0.05 0.16 ; _shelx_res_checksum 9952 _shelx_hkl_file ; 2 0 0 2150.32 82.60 -2 0 0 2211.37 82.74 3 0 0 9.99 1.42 3 0 0 10.72 1.69 -3 0 0 11.06 1.31 -3 0 0 8.30 1.30 4 0 0 25.68 1.99 4 0 0 25.53 2.49 -4 0 0 25.29 1.97 -4 0 0 22.64 2.32 -5 0 0 21.62 2.13 5 0 0 27.85 2.37 -5 0 0 24.42 2.55 6 0 0 7.23 1.68 6 0 0 11.26 1.48 -6 0 0 11.25 2.76 -7 0 0 12.45 1.76 7 0 0 14.74 1.79 8 0 0 2.93 1.27 9 0 0 2.24 1.62 10 0 0 8.80 2.50 -11 0 0 12.54 4.25 11 0 0 0.74 3.28 12 0 0 2.11 4.49 -12 0 0 -1.98 6.34 13 0 0 1.60 4.80 -13 0 0 -0.21 6.95 1 -1 0 159.44 6.45 1 -1 0 166.38 6.42 -1 -1 0 153.50 6.09 -1 1 0 168.77 6.42 1 1 0 147.73 6.09 -2 -1 0 122.69 4.99 2 -1 0 123.21 5.55 2 -1 0 127.33 5.45 -2 -1 0 127.63 5.17 2 1 0 125.31 4.95 2 1 0 124.96 5.22 -2 1 0 128.58 5.46 -2 1 0 124.55 5.61 -3 -1 0 71.68 3.30 -3 -1 0 67.59 3.13 3 -1 0 66.25 3.68 3 -1 0 68.88 3.46 -3 1 0 70.64 3.73 3 1 0 68.92 3.00 3 1 0 68.04 3.38 -3 1 0 68.43 3.49 4 -1 0 23.94 2.64 -4 -1 0 22.13 1.84 -4 -1 0 24.02 1.96 4 -1 0 21.84 2.28 4 1 0 22.25 2.26 -4 1 0 25.10 2.52 4 1 0 23.09 1.69 -4 1 0 21.42 2.02 5 -1 0 3.02 1.63 -5 -1 0 1.34 0.90 5 -1 0 1.84 0.73 -5 -1 0 3.45 1.31 -5 1 0 2.50 1.94 5 1 0 3.28 1.55 5 1 0 2.67 1.15 -6 -1 0 9.63 1.92 6 -1 0 8.63 1.14 6 1 0 7.06 1.05 6 1 0 8.62 1.67 7 -1 0 78.22 4.37 -7 -1 0 82.48 4.26 7 1 0 80.61 4.27 8 -1 0 9.19 1.56 -8 -1 0 8.48 1.63 8 1 0 10.12 1.47 9 -1 0 12.99 1.99 9 1 0 12.79 1.89 10 -1 0 4.87 4.14 10 1 0 1.12 2.21 -11 -1 0 4.97 5.22 11 -1 0 0.73 3.61 11 1 0 2.68 4.18 -11 1 0 4.43 4.58 -12 -1 0 8.16 6.11 12 -1 0 -4.21 4.12 -12 1 0 18.30 6.48 12 1 0 5.64 4.94 13 -1 0 -6.62 4.27 -13 -1 0 -7.81 8.26 -13 1 0 -16.31 7.21 0 -2 0 88.18 3.70 0 2 0 88.58 3.70 1 -2 0 173.43 7.04 -1 -2 0 163.92 6.68 1 2 0 166.87 6.74 -1 2 0 174.66 7.01 2 -2 0 2005.82 77.14 -2 2 0 2040.71 77.05 3 -2 0 77.07 4.09 -3 -2 0 76.84 3.36 -3 -2 0 83.92 3.55 3 2 0 82.63 3.67 3 2 0 77.98 3.30 4 -2 0 33.03 4.86 -4 -2 0 33.67 2.11 -4 -2 0 32.14 2.01 4 -2 0 27.40 2.95 4 2 0 34.55 2.50 4 2 0 34.03 1.83 -4 2 0 31.53 2.52 -5 -2 0 0.91 0.85 5 -2 0 -0.60 0.74 -5 -2 0 2.17 1.16 5 2 0 1.64 0.91 5 2 0 -0.36 1.17 6 -2 0 1.63 0.90 -6 -2 0 3.33 1.46 6 2 0 3.75 1.23 7 -2 0 76.17 4.25 -7 -2 0 80.40 4.52 7 2 0 75.20 4.08 7 2 0 78.21 3.91 8 -2 0 43.85 3.45 8 2 0 49.06 3.16 10 -2 0 5.95 2.65 -10 -2 0 12.02 2.62 10 2 0 10.80 2.60 -11 -2 0 4.04 3.69 11 -2 0 0.63 3.02 -11 2 0 1.63 4.75 11 2 0 -3.95 4.10 -12 -2 0 3.56 4.57 12 -2 0 -2.27 3.77 -12 2 0 -2.73 6.25 12 2 0 6.30 3.91 13 -2 0 7.87 3.90 -13 2 0 4.82 6.84 0 -3 0 0.76 0.68 0 3 0 0.59 0.68 0 3 0 0.56 0.71 -1 -3 0 0.78 0.79 1 -3 0 -0.07 0.87 -1 3 0 -0.07 0.79 2 -3 0 34.33 2.67 -2 -3 0 37.95 1.79 2 -3 0 33.32 2.61 2 3 0 39.42 2.04 -2 3 0 37.68 2.42 3 -3 0 178.11 8.29 3 -3 0 190.61 8.38 -3 -3 0 184.37 7.30 3 3 0 188.97 7.41 4 -3 0 211.95 9.31 -4 -3 0 212.61 8.53 4 3 0 218.64 8.51 5 -3 0 110.85 5.56 -5 -3 0 113.35 5.06 -5 -3 0 115.65 5.16 5 3 0 121.45 5.43 5 3 0 113.98 4.86 -6 -3 0 30.82 2.32 -6 -3 0 33.54 2.39 6 -3 0 29.60 2.31 6 3 0 28.96 2.11 6 3 0 29.36 3.32 -7 -3 0 100.81 5.17 7 -3 0 107.30 5.54 7 3 0 102.00 5.06 7 3 0 97.16 4.66 8 -3 0 91.40 5.54 8 3 0 107.66 5.19 -9 -3 0 6.97 1.54 9 -3 0 12.11 2.29 9 3 0 3.91 1.55 -10 -3 0 11.75 2.36 10 -3 0 9.61 2.81 10 3 0 9.58 2.59 11 -3 0 5.14 3.18 -11 3 0 10.14 5.19 11 3 0 3.91 2.99 12 -3 0 3.42 3.65 -12 3 0 7.44 6.32 0 -4 0 91.22 3.97 0 4 0 87.14 4.11 0 4 0 86.30 3.94 1 -4 0 111.63 5.06 -1 -4 0 107.49 4.86 -1 4 0 106.93 4.93 2 -4 0 47.80 3.20 -2 -4 0 45.19 2.38 2 4 0 48.30 2.79 -2 4 0 44.00 2.81 -3 -4 0 0.55 0.62 3 4 0 -0.32 1.04 -4 -4 0 362.50 14.21 4 -4 0 376.86 15.25 4 4 0 360.64 14.37 -5 -4 0 30.93 2.00 5 -4 0 26.24 2.00 5 4 0 33.11 2.20 6 -4 0 1.37 1.13 -6 -4 0 3.24 1.18 6 4 0 2.48 1.32 7 -4 0 0.70 1.36 -7 -4 0 3.41 1.21 -7 -4 0 3.45 1.47 7 4 0 4.18 1.46 7 4 0 3.44 3.04 8 -4 0 12.34 2.12 -8 -4 0 13.39 2.15 8 4 0 12.54 1.60 9 -4 0 1.43 2.11 -9 -4 0 5.32 2.12 -9 -4 0 4.94 1.66 9 4 0 2.21 1.57 10 -4 0 1.34 2.52 -10 -4 0 -2.48 2.14 -10 4 0 7.32 4.17 10 4 0 -0.77 1.95 11 -4 0 0.63 3.30 -11 4 0 13.10 5.18 12 -4 0 1.77 3.66 -12 4 0 7.43 6.18 0 -5 0 -0.29 1.47 0 -5 0 -0.17 0.84 0 5 0 -0.03 0.95 0 5 0 0.48 1.17 1 -5 0 24.37 2.30 -1 -5 0 22.31 2.17 -1 5 0 16.57 2.55 -1 5 0 22.49 2.08 -2 -5 0 23.14 1.93 2 -5 0 25.55 2.80 -2 5 0 25.01 2.28 -3 -5 0 2.08 0.84 3 -5 0 -0.05 0.74 3 5 0 1.40 1.44 4 -5 0 145.30 6.61 -4 -5 0 141.39 5.80 4 5 0 138.58 6.27 -5 -5 0 7.37 1.09 5 -5 0 4.56 1.05 5 5 0 7.39 1.64 6 -5 0 34.19 2.76 -6 -5 0 36.60 2.37 6 5 0 37.33 2.86 7 -5 0 3.86 1.41 -7 -5 0 4.13 1.47 -8 -5 0 -1.73 1.41 8 -5 0 -0.57 1.79 9 -5 0 3.10 2.33 -10 5 0 14.87 5.07 11 -5 0 -4.73 3.31 -11 5 0 3.82 5.30 12 -5 0 3.49 3.66 -12 5 0 3.96 6.23 0 -6 0 270.86 10.97 0 6 0 269.69 11.19 0 6 0 265.65 10.98 1 -6 0 10.86 1.70 -1 -6 0 10.00 1.84 -1 6 0 11.02 2.04 -1 6 0 13.86 2.14 -2 -6 0 102.48 4.78 2 -6 0 93.38 5.05 -3 -6 0 6.94 1.18 3 -6 0 4.55 0.85 -4 -6 0 12.86 1.45 4 -6 0 17.30 1.74 4 6 0 12.55 2.19 -5 -6 0 -0.28 0.90 5 -6 0 -0.29 1.12 5 6 0 1.87 1.85 -6 -6 0 16.31 1.92 6 -6 0 13.06 1.67 6 6 0 14.30 1.98 7 -6 0 1.55 1.67 -7 -6 0 0.70 1.35 8 -6 0 9.16 2.25 9 -6 0 1.29 2.35 -9 6 0 -5.13 3.94 10 -6 0 -1.18 2.92 -10 6 0 -2.59 4.51 11 -6 0 6.03 3.69 -11 6 0 13.26 5.62 0 -7 0 -0.33 0.90 0 -7 0 -1.12 1.55 0 7 0 0.34 1.37 0 7 0 1.54 1.36 -1 -7 0 153.28 7.25 1 -7 0 170.56 7.37 -1 7 0 144.34 7.14 -1 7 0 165.36 7.99 2 -7 0 1.67 0.82 -2 -7 0 1.73 1.37 -2 7 0 3.08 1.10 3 -7 0 11.50 1.66 -3 -7 0 11.25 1.57 -3 7 0 18.09 2.13 4 -7 0 4.00 1.13 -4 -7 0 6.61 1.27 -5 -7 0 69.77 3.59 5 -7 0 82.91 4.41 6 -7 0 72.64 4.50 -6 -7 0 69.40 3.65 7 -7 0 5.74 1.91 -7 7 0 11.14 3.28 8 -7 0 0.75 2.14 -8 7 0 11.36 3.83 9 -7 0 0.65 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-33 -3.54 2.78 4 -3 -33 4.23 2.59 -4 -3 33 -1.09 4.04 4 3 -33 1.80 2.44 -4 3 33 8.25 5.60 -3 -3 33 -0.32 4.18 3 -3 -33 -0.06 2.36 -3 3 33 6.44 5.61 3 3 -33 2.95 2.44 2 -3 -33 -0.70 2.47 -2 -3 33 2.15 4.19 -2 3 33 -0.26 5.61 1 -3 -33 -2.98 2.36 -1 -3 33 -1.67 4.35 1 3 -33 -1.83 2.41 -1 3 33 -1.73 5.00 0 -3 -33 3.92 2.45 0 -3 33 7.51 4.66 0 3 -33 1.56 2.41 -1 -3 -33 1.22 2.56 1 -3 33 6.93 4.86 -1 3 -33 7.25 2.66 2 -3 33 8.14 5.02 -2 -3 -33 -0.75 2.67 -2 3 -33 -0.59 2.82 -3 -3 -33 11.72 3.11 3 -3 33 9.74 4.74 -3 3 -33 1.17 3.37 -4 -3 -33 -2.31 2.81 6 -4 -33 5.46 3.34 6 4 -33 3.71 2.75 -6 4 33 6.92 5.82 -5 -4 33 3.29 4.01 5 -4 -33 3.17 3.06 5 4 -33 -2.60 2.66 -5 4 33 0.47 6.21 -4 -4 33 0.80 3.75 4 -4 -33 4.83 2.97 4 4 -33 -0.68 2.78 -4 4 33 -5.06 5.69 3 -4 -33 2.28 2.59 -3 -4 33 -3.33 4.03 3 4 -33 -1.63 2.60 -3 4 33 0.49 5.82 2 -4 -33 1.95 2.48 -2 -4 33 6.25 3.88 2 4 -33 -2.20 2.58 -2 4 33 8.42 6.40 1 -4 -33 4.95 2.60 -1 -4 33 2.05 4.24 -1 4 33 12.74 4.76 1 4 -33 -2.73 2.56 0 -4 -33 2.57 2.72 0 -4 33 2.99 4.59 0 4 -33 1.16 2.55 1 -4 33 -1.04 4.48 -1 -4 -33 -0.43 2.65 -1 4 -33 -6.45 2.70 2 -4 33 7.86 5.14 -2 -4 -33 0.90 2.82 -2 4 -33 -2.23 3.04 3 -4 33 2.41 5.19 -3 -4 -33 -2.69 2.77 -6 5 33 2.20 5.42 5 -5 -33 3.46 3.07 5 5 -33 -1.90 2.75 -5 5 33 -0.72 6.53 -4 -5 33 5.71 4.07 4 -5 -33 2.96 3.12 -4 5 33 7.51 6.86 4 5 -33 3.63 2.94 3 -5 -33 4.08 3.16 -3 -5 33 5.77 4.44 -3 5 33 7.18 6.71 3 5 -33 6.72 3.09 -2 -5 33 2.30 4.26 2 -5 -33 5.94 2.86 2 5 -33 2.93 2.95 -2 5 33 10.85 6.12 1 -5 -33 1.49 2.67 -1 -5 33 3.71 4.49 1 5 -33 1.09 2.69 0 -5 -33 6.96 3.08 0 -5 33 13.05 5.00 0 5 -33 -0.17 2.84 -1 -5 -33 9.10 3.07 1 -5 33 3.36 4.83 -1 5 -33 -4.57 3.09 -2 -5 -33 -6.46 2.78 2 -5 33 -2.79 5.06 3 -5 33 2.91 4.63 5 -6 -33 5.08 3.95 -5 6 33 -2.43 6.74 4 -6 -33 5.53 3.22 -4 6 33 10.56 7.18 4 6 -33 1.62 2.86 -3 -6 33 0.52 3.77 3 -6 -33 2.79 3.34 -3 6 33 3.88 6.57 -2 -6 33 2.44 3.76 2 -6 -33 6.04 3.35 2 6 -33 2.33 2.88 -1 -6 33 3.23 3.64 1 -6 -33 -1.37 3.18 1 6 -33 -3.17 2.76 0 -6 33 5.49 3.84 0 -6 -33 7.36 3.04 1 -6 33 5.97 4.51 2 -6 33 3.01 4.67 4 -7 -33 1.84 3.53 -4 7 33 -2.95 7.03 3 -7 -33 6.18 3.48 2 -7 -33 13.19 3.51 1 -7 -33 11.20 3.32 6 0 -34 15.15 3.44 -6 0 34 7.57 4.93 -5 0 34 4.13 4.41 5 0 -34 5.89 2.53 4 0 -34 -4.53 2.71 -4 0 34 0.74 4.91 3 0 -34 -1.87 2.22 -3 0 34 3.46 4.98 -2 0 34 -1.40 4.48 2 0 -34 -3.63 2.29 -1 0 34 22.96 5.52 1 0 -34 9.39 2.45 0 0 -34 7.21 2.57 0 0 34 9.79 4.98 1 0 34 6.29 4.69 -1 0 -34 8.63 2.61 -2 0 -34 1.66 2.58 -3 0 -34 -3.73 2.63 -6 -1 34 2.09 4.20 6 -1 -34 -5.37 3.36 6 1 -34 -1.28 3.11 -6 1 34 -3.51 4.42 -5 -1 34 17.78 5.12 5 1 -34 15.34 2.96 -5 1 34 15.43 5.87 4 -1 -34 2.97 2.54 -4 -1 34 12.19 4.86 4 1 -34 -0.27 2.45 -4 1 34 0.93 5.29 3 -1 -34 -1.06 2.34 -3 -1 34 0.59 4.72 3 1 -34 -4.39 2.44 -3 1 34 -2.42 4.80 2 -1 -34 -0.40 2.30 -2 -1 34 9.78 4.78 2 1 -34 -0.03 2.40 -2 1 34 2.18 5.31 -1 -1 34 5.05 4.76 1 -1 -34 1.49 2.49 1 1 -34 -3.22 2.55 -1 1 34 1.41 5.18 0 -1 34 1.20 4.60 0 -1 -34 0.19 2.49 0 1 34 6.88 5.04 0 1 -34 2.83 2.70 1 -1 34 1.47 5.01 -1 -1 -34 -2.61 2.49 -2 -1 -34 -2.69 2.69 -2 1 -34 -4.25 2.61 -3 -1 -34 -0.19 2.67 -3 1 -34 -1.99 2.74 -4 -1 -34 -3.72 2.92 -6 -2 34 12.47 6.65 -6 2 34 0.38 4.87 -5 -2 34 -0.60 4.57 5 -2 -34 -0.49 2.82 -5 2 34 2.35 5.72 5 2 -34 1.23 2.83 -4 -2 34 3.66 4.74 4 -2 -34 6.50 2.80 4 2 -34 -1.47 2.63 -4 2 34 -3.11 4.98 3 -2 -34 4.01 2.64 -3 -2 34 3.81 4.60 3 2 -34 -3.84 2.42 -3 2 34 2.64 5.49 2 -2 -34 3.07 2.41 -2 -2 34 -2.72 4.58 2 2 -34 -1.11 2.53 -2 2 34 -2.14 5.23 1 -2 -34 2.20 2.37 -1 -2 34 2.65 4.58 -1 2 34 6.06 5.65 1 2 -34 -3.88 2.67 0 -2 -34 3.90 2.49 0 -2 34 4.52 4.88 0 2 34 1.65 4.04 0 2 -34 -3.53 2.39 -1 -2 -34 2.96 2.64 1 -2 34 11.78 5.09 -2 -2 -34 3.23 2.84 2 -2 34 3.60 4.81 -2 2 -34 3.20 2.58 -3 -2 -34 -0.32 2.86 -6 3 34 4.79 5.14 -5 -3 34 12.06 4.38 5 -3 -34 8.20 2.97 -5 3 34 17.54 6.32 5 3 -34 14.29 3.18 -4 -3 34 13.70 5.17 4 -3 -34 6.90 3.25 4 3 -34 7.17 2.80 -4 3 34 13.45 6.15 -3 -3 34 2.16 4.48 3 -3 -34 8.16 2.63 3 3 -34 1.00 2.98 -3 3 34 1.57 6.06 -2 -3 34 2.42 4.20 2 -3 -34 4.71 2.47 2 3 -34 -1.69 2.45 -2 3 34 5.39 6.01 1 -3 -34 0.11 2.42 -1 -3 34 3.48 4.79 -1 3 34 3.43 5.27 1 3 -34 0.83 2.63 0 -3 34 5.50 4.76 0 -3 -34 2.40 2.69 0 3 -34 3.87 2.65 1 -3 34 -1.30 4.88 -1 -3 -34 -4.01 2.71 -1 3 -34 -4.67 2.61 -2 -3 -34 -1.91 2.88 2 -3 34 0.19 4.99 -3 -3 -34 0.09 3.07 5 -4 -34 -4.48 3.10 -5 4 34 13.12 6.31 -4 -4 34 0.57 3.95 4 -4 -34 -0.46 2.98 -4 4 34 0.79 6.29 4 4 -34 -1.38 2.44 -3 -4 34 1.80 4.29 -3 4 34 3.45 6.10 3 4 -34 -0.36 2.68 -2 -4 34 2.00 4.41 2 -4 -34 1.17 2.75 2 4 -34 0.51 2.74 -2 4 34 9.53 6.38 -1 -4 34 6.95 4.59 1 -4 -34 1.38 2.73 1 4 -34 -1.28 2.56 0 -4 34 6.08 4.91 0 -4 -34 8.30 3.05 0 4 -34 2.44 2.63 -1 -4 -34 9.96 3.10 1 -4 34 13.01 5.35 -2 -4 -34 -1.12 2.80 2 -4 34 4.62 5.26 3 -4 34 15.69 4.91 -5 5 34 -1.32 6.06 4 -5 -34 0.78 3.15 -4 5 34 -8.52 6.66 -3 -5 34 4.74 3.64 3 -5 -34 -0.28 3.13 -3 5 34 9.06 6.88 3 5 -34 7.37 2.84 2 -5 -34 3.77 3.15 -2 -5 34 -0.76 3.51 2 5 -34 -1.17 2.74 -1 -5 34 4.90 4.21 1 -5 -34 -0.71 3.04 1 5 -34 -6.18 2.99 0 -5 -34 0.97 2.94 0 -5 34 2.74 4.18 1 -5 34 1.94 4.54 -1 -5 -34 -3.80 2.98 2 -5 34 1.95 4.46 -5 6 34 1.34 6.60 4 -6 -34 1.05 3.49 -4 6 34 -3.54 7.21 3 -6 -34 9.15 3.51 -3 6 34 -0.94 7.20 2 -6 -34 6.07 3.44 1 -6 -34 5.08 3.51 0 -6 -34 0.47 3.15 2 -7 -34 12.50 3.70 5 0 -35 -1.32 3.09 -5 0 35 4.64 4.22 -4 0 35 2.29 5.26 4 0 -35 -0.01 2.59 3 0 -35 1.95 2.45 -3 0 35 5.75 5.04 2 0 -35 -5.53 2.47 -2 0 35 -4.08 4.93 -1 0 35 10.97 5.35 0 0 -35 2.16 2.61 0 0 35 2.96 5.27 -1 0 -35 1.98 2.70 -2 0 -35 -3.93 2.61 -5 -1 35 -0.33 4.00 -5 1 35 -2.97 5.22 -4 -1 35 9.31 5.19 4 -1 -35 0.26 2.58 4 1 -35 2.21 2.53 -4 1 35 6.22 5.37 3 -1 -35 -0.33 2.47 -3 -1 35 -6.64 4.72 -3 1 35 7.49 5.67 3 1 -35 -3.69 2.39 2 -1 -35 0.89 2.52 -2 -1 35 4.90 5.05 2 1 -35 1.77 2.47 -2 1 35 7.42 5.79 1 -1 -35 -0.09 2.61 -1 -1 35 1.32 5.00 1 1 -35 -6.25 2.65 -1 1 35 5.91 5.84 0 -1 35 0.72 5.23 0 -1 -35 -5.62 2.47 0 1 -35 -2.48 2.58 0 1 35 1.04 4.79 1 -1 35 5.15 4.83 -1 -1 -35 -4.42 2.75 -1 1 -35 1.14 2.54 -2 -1 -35 -0.43 2.73 -3 -1 -35 -1.46 3.20 -5 -2 35 3.42 4.74 -5 2 35 0.85 5.41 4 -2 -35 3.66 2.69 -4 -2 35 6.22 4.21 4 2 -35 -2.27 2.65 -4 2 35 -0.96 5.50 -3 -2 35 3.75 4.67 3 -2 -35 1.97 2.65 -3 2 35 2.10 5.89 3 2 -35 5.89 2.62 -2 -2 35 0.89 4.97 2 -2 -35 -1.74 2.58 -2 2 35 5.86 6.00 2 2 -35 -1.19 2.50 -1 -2 35 2.04 4.67 1 -2 -35 1.26 2.51 1 2 -35 2.80 2.60 -1 2 35 5.91 5.58 0 -2 35 1.29 4.98 0 2 -35 0.05 2.62 1 -2 35 1.48 5.25 -1 -2 -35 -1.85 2.61 -1 2 -35 4.37 2.76 2 -2 35 16.24 5.39 -3 -2 -35 8.08 3.04 -5 3 35 11.86 5.75 -4 -3 35 2.84 3.64 4 -3 -35 1.92 2.89 -4 3 35 4.83 6.31 -3 -3 35 5.44 4.74 3 -3 -35 -1.64 2.82 -3 3 35 9.27 6.60 3 3 -35 7.60 2.66 2 -3 -35 -1.63 2.64 -2 -3 35 4.43 4.20 -2 3 35 4.25 6.15 2 3 -35 3.18 3.00 1 -3 -35 0.48 2.73 -1 -3 35 2.91 5.05 1 3 -35 0.57 2.70 -1 3 35 7.44 6.87 0 -3 35 4.37 5.16 0 -3 -35 3.47 2.74 -1 -3 -35 -0.95 2.82 1 -3 35 7.26 5.45 -2 -3 -35 -1.14 2.73 2 -3 35 10.85 5.27 -5 4 35 1.60 5.51 4 -4 -35 -3.23 3.23 -4 4 35 -3.02 6.27 3 -4 -35 1.36 3.03 -3 -4 35 -6.33 3.67 -3 4 35 -1.75 6.93 2 -4 -35 -0.49 2.83 -2 -4 35 1.30 4.20 -2 4 35 8.87 5.74 1 -4 -35 2.10 2.94 -1 -4 35 0.83 4.75 0 -4 -35 -0.96 2.87 0 -4 35 2.37 4.72 1 -4 35 -4.80 4.55 -1 -4 -35 -3.11 2.96 -2 -4 -35 8.88 3.33 2 -4 35 5.25 4.94 -4 5 35 14.60 6.56 3 -5 -35 -0.27 3.29 -3 5 35 -3.58 6.08 2 -5 -35 1.72 3.21 1 -5 -35 5.43 3.25 0 -5 35 4.58 6.65 0 -5 -35 1.08 3.16 3 -6 -35 6.56 3.90 2 -6 -35 2.17 3.60 1 -6 -35 8.88 3.59 -4 0 36 1.94 4.87 -3 0 36 6.12 5.87 3 0 -36 5.77 2.94 -2 0 36 1.17 5.68 2 0 -36 -0.01 2.82 1 0 -36 11.44 2.68 -1 0 36 13.39 6.12 0 0 -36 3.90 2.84 0 0 36 10.73 5.44 -4 -1 36 7.84 4.23 -4 1 36 8.59 5.35 -3 -1 36 3.72 5.29 3 -1 -36 -4.64 2.63 -3 1 36 2.44 5.90 -2 -1 36 4.67 5.27 2 -1 -36 -1.99 2.69 2 1 -36 5.98 2.68 -2 1 36 -4.60 5.61 1 -1 -36 -2.28 2.71 -1 -1 36 2.61 5.55 -1 1 36 5.76 6.23 1 1 -36 1.60 2.94 0 -1 -36 -5.59 2.58 0 -1 36 -1.93 5.72 -1 -1 -36 -2.38 2.87 1 -1 36 9.01 5.09 -4 -2 36 1.34 6.31 -4 2 36 4.45 5.69 -3 -2 36 3.05 4.59 3 -2 -36 -1.04 2.80 -3 2 36 4.74 5.95 -2 -2 36 -6.03 4.96 -2 2 36 4.80 6.22 -1 -2 36 3.53 5.31 1 -2 -36 -0.25 2.68 -1 2 36 -2.84 5.11 0 -2 36 4.35 5.39 0 -2 -36 -2.97 2.87 1 -2 36 2.52 5.35 -1 -2 -36 -3.71 2.74 -4 3 36 0.72 5.36 -3 -3 36 -1.57 5.79 3 -3 -36 -0.33 3.33 -3 3 36 3.43 6.56 -2 -3 36 3.08 4.40 2 -3 -36 -2.64 2.74 -2 3 36 3.80 5.97 -1 -3 36 7.32 5.17 1 -3 -36 0.54 2.83 0 -3 36 1.95 5.11 0 -3 -36 -2.63 2.87 -1 -3 -36 -5.03 2.90 1 -3 36 5.16 5.06 -4 4 36 -12.11 5.73 -3 4 36 13.76 6.72 2 -4 -36 3.18 3.04 -1 -4 36 5.02 6.62 1 -4 -36 1.47 3.03 0 -4 36 3.21 5.16 0 -4 -36 -2.77 3.08 2 -5 -36 2.94 3.96 -3 0 37 -0.77 5.12 -2 0 37 1.33 5.68 -1 0 37 1.63 5.92 0 0 37 1.35 5.26 -4 1 37 1.85 7.46 -3 -1 37 6.77 4.51 -3 1 37 7.28 5.71 -2 -1 37 10.71 5.34 -2 1 37 -3.72 5.77 -1 -1 37 3.57 5.73 -1 1 37 -3.83 5.70 0 -1 37 3.17 5.24 -4 2 37 8.20 6.25 -3 2 37 5.44 6.14 -2 -2 37 -0.39 4.50 -2 2 37 0.20 6.03 -1 -2 37 11.13 5.16 0 -2 37 4.69 4.81 -3 3 37 7.84 5.98 -2 3 37 8.87 6.37 -2 0 38 6.29 5.56 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6438 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71074 9.474 10.972 26.623 90.036 98.659 89.987 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 36571 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7180(3) 0.5639(2) 0.80692(8) 0.0442(6) Uani 1 1 d . . . . . C2 C 0.8246(3) 0.5261(3) 0.84472(10) 0.0617(8) Uani 1 1 d . . . . . H2 H 0.886555 0.464521 0.838090 0.074 Uiso 1 1 calc R U . . . C3 C 0.8401(4) 0.5786(3) 0.89219(11) 0.0763(10) Uani 1 1 d . . . . . H3 H 0.911992 0.551492 0.917302 0.092 Uiso 1 1 calc R U . . . C4 C 0.7518(3) 0.6695(3) 0.90292(11) 0.0746(9) Uani 1 1 d . . . . . H4 H 0.763921 0.705069 0.934954 0.090 Uiso 1 1 calc R U . . . C5 C 0.6451(3) 0.7080(3) 0.86606(10) 0.0648(8) Uani 1 1 d . . . . . H5 H 0.583811 0.769745 0.873046 0.078 Uiso 1 1 calc R U . . . C6 C 0.6282(3) 0.6555(2) 0.81868(9) 0.0524(7) Uani 1 1 d . . . . . H6 H 0.554778 0.682121 0.794004 0.063 Uiso 1 1 calc R U . . . C7 C 0.7082(3) 0.5099(2) 0.75449(9) 0.0480(6) Uani 1 1 d . . . . . H7A H 0.794066 0.530679 0.740667 0.058 Uiso 1 1 calc R U . . . H7AB H 0.704746 0.421930 0.757233 0.058 Uiso 1 1 calc R U . . . C8 C 0.4592(3) 0.4929(2) 0.71968(8) 0.0418(6) Uani 1 1 d . . . . . C9 C 0.3266(3) 0.5408(2) 0.68659(8) 0.0402(6) Uani 1 1 d . . . . . H9 H 0.274281 0.470768 0.670417 0.048 Uiso 1 1 calc R U . . . C10 C 0.4634(2) 0.7140(2) 0.66634(8) 0.0404(6) Uani 1 1 d . . . . . H10A H 0.426701 0.758449 0.693068 0.048 Uiso 1 1 calc R U . . . H10B H 0.475993 0.770969 0.639572 0.048 Uiso 1 1 calc R U . . . C11 C 0.6054(3) 0.6567(2) 0.68720(8) 0.0418(6) Uani 1 1 d . . . . . H11 H 0.660249 0.717219 0.709073 0.050 Uiso 1 1 calc R U . . . C12 C 0.3224(3) 0.5930(2) 0.59714(9) 0.0492(7) Uani 1 1 d . . . . . C13 C 0.3637(3) 0.6801(2) 0.55862(8) 0.0462(6) Uani 1 1 d . . . . . C14 C 0.4608(3) 0.6443(3) 0.52791(9) 0.0615(8) Uani 1 1 d . . . . . H14 H 0.503537 0.568154 0.532599 0.074 Uiso 1 1 calc R U . . . C15 C 0.4954(4) 0.7199(4) 0.49035(11) 0.0788(10) Uani 1 1 d . . . . . H15 H 0.560903 0.694788 0.469761 0.095 Uiso 1 1 calc R U . . . C16 C 0.4331(4) 0.8317(4) 0.48351(12) 0.0881(11) Uani 1 1 d . . . . . H16 H 0.455415 0.882651 0.457952 0.106 Uiso 1 1 calc R U . . . C17 C 0.3375(4) 0.8693(3) 0.51430(13) 0.0887(11) Uani 1 1 d . . . . . H17 H 0.295722 0.945905 0.509758 0.106 Uiso 1 1 calc R U . . . C18 C 0.3033(3) 0.7929(3) 0.55216(11) 0.0682(8) Uani 1 1 d . . . . . H18 H 0.239210 0.818608 0.573166 0.082 Uiso 1 1 calc R U . . . C19 C 0.2278(2) 0.6074(2) 0.71794(8) 0.0410(6) Uani 1 1 d . . . . . C20 C 0.2464(3) 0.6062(3) 0.77046(9) 0.0585(8) Uani 1 1 d . . . . . H20 H 0.319257 0.559760 0.788291 0.070 Uiso 1 1 calc R U . . . C21 C 0.1579(3) 0.6731(3) 0.79670(10) 0.0642(8) Uani 1 1 d . . . . . H21 H 0.172949 0.670625 0.831986 0.077 Uiso 1 1 calc R U . . . C22 C 0.0484(3) 0.7433(2) 0.77235(10) 0.0534(7) Uani 1 1 d . . . . . C23 C 0.0286(3) 0.7413(3) 0.72018(10) 0.0574(7) Uani 1 1 d . . . . . H23 H -0.045598 0.786390 0.702433 0.069 Uiso 1 1 calc R U . . . C24 C 0.1154(3) 0.6745(3) 0.69325(10) 0.0542(7) Uani 1 1 d . . . . . H24 H 0.097755 0.674838 0.657963 0.065 Uiso 1 1 calc R U . . . C25 C -0.0427(3) 0.8212(3) 0.80080(12) 0.0750(9) Uani 1 1 d . . . . . H25A H 0.001977 0.899064 0.807681 0.113 Uiso 1 1 calc R U . . . H25B H -0.053814 0.782250 0.832227 0.113 Uiso 1 1 calc R U . . . H25C H -0.134683 0.832135 0.780699 0.113 Uiso 1 1 calc R U . . . C26 C 0.6908(3) 0.6243(2) 0.64585(8) 0.0453(6) Uani 1 1 d . . . . . C27 C 0.7243(3) 0.5128(3) 0.62876(9) 0.0542(7) Uani 1 1 d . . . . . H27 H 0.697256 0.438952 0.641507 0.065 Uiso 1 1 calc R U . . . C28 C 0.8635(4) 0.4260(4) 0.56349(12) 0.0900(11) Uani 1 1 d . . . . . H28A H 0.839489 0.437412 0.527498 0.135 Uiso 1 1 calc R U . . . H28B H 0.825135 0.349952 0.572955 0.135 Uiso 1 1 calc R U . . . H28C H 0.965386 0.425293 0.572607 0.135 Uiso 1 1 calc R U . . . C29 C 0.8225(3) 0.6463(3) 0.58163(9) 0.0612(8) Uani 1 1 d . . . . . C30 C 0.8961(3) 0.7057(4) 0.54631(11) 0.0816(11) Uani 1 1 d . . . . . H30 H 0.942989 0.662565 0.523723 0.098 Uiso 1 1 calc R U . . . C31 C 0.8947(4) 0.8303(4) 0.54714(14) 0.0932(12) Uani 1 1 d . . . . . H31 H 0.942140 0.872288 0.524375 0.112 Uiso 1 1 calc R U . . . C32 C 0.8264(4) 0.8960(4) 0.58001(13) 0.0847(11) Uani 1 1 d . . . . . H32 H 0.828554 0.980614 0.579037 0.102 Uiso 1 1 calc R U . . . C33 C 0.7550(3) 0.8385(3) 0.61431(11) 0.0656(8) Uani 1 1 d . . . . . H33 H 0.708644 0.883661 0.636461 0.079 Uiso 1 1 calc R U . . . C34 C 0.7524(3) 0.7112(3) 0.61566(9) 0.0518(7) Uani 1 1 d . . . . . N1 N 0.5845(2) 0.55058(18) 0.71900(7) 0.0419(5) Uani 1 1 d . . . . . N2 N 0.3623(2) 0.62010(17) 0.64641(6) 0.0404(5) Uani 1 1 d . . . . . N3 N 0.8038(2) 0.5251(3) 0.58986(8) 0.0655(7) Uani 1 1 d . . . . . O1 O 0.4484(2) 0.40550(15) 0.74740(7) 0.0580(5) Uani 1 1 d . . . . . O2 O 0.2538(3) 0.5015(2) 0.58365(7) 0.0875(8) Uani 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 C1 0.0476(15) 0.0454(15) 0.0405(13) 0.0063(11) 0.0093(11) 0.0048(12) C2 0.0608(18) 0.065(2) 0.0573(16) 0.0009(14) 0.0027(14) 0.0227(15) C3 0.071(2) 0.102(3) 0.0509(16) -0.0027(17) -0.0070(15) 0.022(2) C4 0.082(2) 0.096(3) 0.0449(16) -0.0130(16) 0.0072(16) 0.010(2) C5 0.074(2) 0.071(2) 0.0518(16) -0.0037(14) 0.0174(15) 0.0180(17) C6 0.0556(16) 0.0592(17) 0.0429(14) 0.0052(12) 0.0090(12) 0.0121(14) C7 0.0495(15) 0.0491(16) 0.0458(13) 0.0019(11) 0.0087(12) 0.0112(13) C8 0.0549(16) 0.0346(14) 0.0374(12) -0.0018(11) 0.0119(11) 0.0023(12) C9 0.0486(14) 0.0317(13) 0.0404(12) 0.0017(10) 0.0069(11) -0.0076(11) C10 0.0507(15) 0.0342(13) 0.0366(12) -0.0025(10) 0.0081(11) -0.0074(11) C11 0.0501(15) 0.0420(14) 0.0336(12) -0.0017(10) 0.0073(11) -0.0063(12) C12 0.0635(17) 0.0433(16) 0.0409(14) -0.0054(12) 0.0076(12) -0.0085(14) C13 0.0562(15) 0.0478(16) 0.0342(12) -0.0011(11) 0.0050(11) -0.0050(13) C14 0.0711(19) 0.069(2) 0.0443(14) -0.0022(14) 0.0070(14) 0.0000(16) C15 0.082(2) 0.103(3) 0.0555(18) 0.0034(18) 0.0238(16) -0.016(2) C16 0.116(3) 0.091(3) 0.060(2) 0.0221(19) 0.022(2) -0.022(2) C17 0.125(3) 0.067(2) 0.074(2) 0.0253(18) 0.016(2) 0.013(2) C18 0.088(2) 0.060(2) 0.0589(17) 0.0110(15) 0.0199(16) 0.0146(17) C19 0.0428(14) 0.0386(14) 0.0428(13) 0.0043(11) 0.0102(11) -0.0061(12) C20 0.0639(18) 0.0657(19) 0.0479(15) 0.0132(13) 0.0147(13) 0.0194(15) C21 0.0730(19) 0.077(2) 0.0465(15) 0.0063(14) 0.0212(15) 0.0161(18) C22 0.0479(15) 0.0490(16) 0.0664(18) 0.0013(13) 0.0192(14) -0.0046(14) C23 0.0433(15) 0.0623(19) 0.0663(18) 0.0064(14) 0.0070(14) 0.0050(14) C24 0.0490(16) 0.0647(19) 0.0475(14) 0.0061(13) 0.0027(12) -0.0016(14) C25 0.0656(19) 0.071(2) 0.093(2) -0.0104(18) 0.0294(18) 0.0047(17) C26 0.0425(14) 0.0568(17) 0.0369(12) -0.0036(12) 0.0073(11) -0.0055(13) C27 0.0528(16) 0.0637(19) 0.0478(14) -0.0106(13) 0.0124(12) -0.0034(14) C28 0.078(2) 0.121(3) 0.074(2) -0.040(2) 0.0236(18) 0.010(2) C29 0.0493(16) 0.095(3) 0.0402(14) 0.0005(15) 0.0088(12) -0.0102(16) C30 0.0594(19) 0.140(4) 0.0473(17) -0.001(2) 0.0135(14) -0.013(2) C31 0.082(3) 0.129(4) 0.069(2) 0.026(2) 0.0128(19) -0.037(3) C32 0.082(2) 0.095(3) 0.075(2) 0.024(2) 0.0037(19) -0.024(2) C33 0.0636(19) 0.072(2) 0.0586(17) 0.0105(15) 0.0015(14) -0.0158(16) C34 0.0442(15) 0.069(2) 0.0404(13) 0.0017(13) 0.0011(11) -0.0108(14) N1 0.0475(12) 0.0408(12) 0.0383(10) 0.0022(9) 0.0090(9) 0.0025(10) N2 0.0494(12) 0.0376(11) 0.0347(10) -0.0001(8) 0.0080(9) -0.0068(10) N3 0.0585(15) 0.091(2) 0.0500(13) -0.0181(13) 0.0171(11) 0.0055(14) O1 0.0731(13) 0.0407(11) 0.0611(11) 0.0151(9) 0.0129(9) 0.0016(9) O2 0.135(2) 0.0707(15) 0.0517(11) -0.0049(10) -0.0005(12) -0.0478(15) 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 C2 C1 C6 117.5(2) . . ? C2 C1 C7 119.6(2) . . ? C6 C1 C7 122.8(2) . . ? C3 C2 C1 120.6(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 121.4(2) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N1 C7 C1 114.29(19) . . ? N1 C7 H7A 108.7 . . ? C1 C7 H7A 108.7 . . ? N1 C7 H7AB 108.7 . . ? C1 C7 H7AB 108.7 . . ? H7A C7 H7AB 107.6 . . ? O1 C8 N1 122.0(2) . . ? O1 C8 C9 119.0(2) . . ? N1 C8 C9 118.9(2) . . ? N2 C9 C8 111.73(19) . . ? N2 C9 C19 110.11(18) . . ? C8 C9 C19 111.74(18) . . ? N2 C9 H9 107.7 . . ? C8 C9 H9 107.7 . . ? C19 C9 H9 107.7 . . ? N2 C10 C11 109.96(19) . . ? N2 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N1 C11 C26 111.6(2) . . ? N1 C11 C10 110.52(18) . . ? C26 C11 C10 112.09(18) . . ? N1 C11 H11 107.5 . . ? C26 C11 H11 107.5 . . ? C10 C11 H11 107.5 . . ? O2 C12 N2 122.0(2) . . ? O2 C12 C13 120.4(2) . . ? N2 C12 C13 117.6(2) . . ? C18 C13 C14 119.3(2) . . ? C18 C13 C12 121.2(2) . . ? C14 C13 C12 119.5(2) . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 120.1(3) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C24 C19 C20 117.3(2) . . ? C24 C19 C9 119.2(2) . . ? C20 C19 C9 123.5(2) . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 122.2(2) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C23 C22 C21 116.5(2) . . ? C23 C22 C25 121.3(3) . . ? C21 C22 C25 122.2(3) . . ? C22 C23 C24 122.2(3) . . ? C22 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C19 C24 C23 120.9(2) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C34 106.1(2) . . ? C27 C26 C11 129.5(2) . . ? C34 C26 C11 124.4(2) . . ? C26 C27 N3 110.2(3) . . ? C26 C27 H27 124.9 . . ? N3 C27 H27 124.9 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C34 108.0(2) . . ? N3 C29 C30 130.3(3) . . ? C34 C29 C30 121.8(3) . . ? C31 C30 C29 116.4(3) . . ? C31 C30 H30 121.8 . . ? C29 C30 H30 121.8 . . ? C30 C31 C32 122.9(3) . . ? C30 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C34 119.3(3) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C29 C34 C33 118.8(3) . . ? C29 C34 C26 107.4(3) . . ? C33 C34 C26 133.8(2) . . ? C8 N1 C7 118.1(2) . . ? C8 N1 C11 125.1(2) . . ? C7 N1 C11 116.74(19) . . ? C12 N2 C10 126.04(19) . . ? C12 N2 C9 121.49(19) . . ? C10 N2 C9 111.59(17) . . ? C29 N3 C27 108.3(2) . . ? C29 N3 C28 125.6(3) . . ? C27 N3 C28 126.0(3) . . ? 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 C1 C2 1.379(3) . ? C1 C6 1.384(3) . ? C1 C7 1.508(3) . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.360(4) . ? C3 H3 0.9300 . ? C4 C5 1.367(4) . ? C4 H4 0.9300 . ? C5 C6 1.375(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.462(3) . ? C7 H7A 0.9700 . ? C7 H7AB 0.9700 . ? C8 O1 1.225(3) . ? C8 N1 1.349(3) . ? C8 C9 1.518(3) . ? C9 N2 1.459(3) . ? C9 C19 1.531(3) . ? C9 H9 0.9800 . ? C10 N2 1.453(3) . ? C10 C11 1.515(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.472(3) . ? C11 C26 1.504(3) . ? C11 H11 0.9800 . ? C12 O2 1.222(3) . ? C12 N2 1.344(3) . ? C12 C13 1.498(3) . ? C13 C18 1.366(4) . ? C13 C14 1.377(4) . ? C14 C15 1.377(4) . ? C14 H14 0.9300 . ? C15 C16 1.363(5) . ? C15 H15 0.9300 . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.387(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.380(3) . ? C19 C20 1.384(3) . ? C20 C21 1.382(4) . ? C20 H20 0.9300 . ? C21 C22 1.376(4) . ? C21 H21 0.9300 . ? C22 C23 1.375(4) . ? C22 C25 1.500(4) . ? C23 C24 1.380(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.361(3) . ? C26 C34 1.428(3) . ? C27 N3 1.377(3) . ? C27 H27 0.9300 . ? C28 N3 1.455(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N3 1.365(4) . ? C29 C34 1.397(4) . ? C29 C30 1.413(4) . ? C30 C31 1.369(5) . ? C30 H30 0.9300 . ? C31 C32 1.370(5) . ? C31 H31 0.9300 . ? C32 C33 1.371(4) . ? C32 H32 0.9300 . ? C33 C34 1.399(4) . ? C33 H33 0.9300 . ? 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 C6 C1 C2 C3 -0.2(4) . . . . ? C7 C1 C2 C3 176.7(3) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C2 C1 C6 C5 0.7(4) . . . . ? C7 C1 C6 C5 -176.1(3) . . . . ? C2 C1 C7 N1 175.5(2) . . . . ? C6 C1 C7 N1 -7.7(4) . . . . ? O1 C8 C9 N2 -163.91(19) . . . . ? N1 C8 C9 N2 18.5(3) . . . . ? O1 C8 C9 C19 72.2(3) . . . . ? N1 C8 C9 C19 -105.4(2) . . . . ? N2 C10 C11 N1 -46.2(2) . . . . ? N2 C10 C11 C26 79.0(2) . . . . ? O2 C12 C13 C18 110.0(3) . . . . ? N2 C12 C13 C18 -69.4(3) . . . . ? O2 C12 C13 C14 -67.7(4) . . . . ? N2 C12 C13 C14 112.9(3) . . . . ? C18 C13 C14 C15 -1.2(4) . . . . ? C12 C13 C14 C15 176.6(3) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 0.7(5) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C14 C13 C18 C17 1.4(4) . . . . ? C12 C13 C18 C17 -176.4(3) . . . . ? C16 C17 C18 C13 -0.5(5) . . . . ? N2 C9 C19 C24 44.1(3) . . . . ? C8 C9 C19 C24 168.9(2) . . . . ? N2 C9 C19 C20 -134.6(2) . . . . ? C8 C9 C19 C20 -9.8(3) . . . . ? C24 C19 C20 C21 -2.1(4) . . . . ? C9 C19 C20 C21 176.7(2) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? C20 C21 C22 C23 1.6(4) . . . . ? C20 C21 C22 C25 -176.7(3) . . . . ? C21 C22 C23 C24 -1.2(4) . . . . ? C25 C22 C23 C24 177.0(3) . . . . ? C20 C19 C24 C23 2.4(4) . . . . ? C9 C19 C24 C23 -176.4(2) . . . . ? C22 C23 C24 C19 -0.8(4) . . . . ? N1 C11 C26 C27 14.0(3) . . . . ? C10 C11 C26 C27 -110.5(3) . . . . ? N1 C11 C26 C34 -166.9(2) . . . . ? C10 C11 C26 C34 68.5(3) . . . . ? C34 C26 C27 N3 0.4(3) . . . . ? C11 C26 C27 N3 179.5(2) . . . . ? N3 C29 C30 C31 179.5(3) . . . . ? C34 C29 C30 C31 -0.2(4) . . . . ? C29 C30 C31 C32 0.0(5) . . . . ? C30 C31 C32 C33 0.0(5) . . . . ? C31 C32 C33 C34 0.2(5) . . . . ? N3 C29 C34 C33 -179.4(2) . . . . ? C30 C29 C34 C33 0.4(4) . . . . ? N3 C29 C34 C26 0.7(3) . . . . ? C30 C29 C34 C26 -179.5(2) . . . . ? C32 C33 C34 C29 -0.3(4) . . . . ? C32 C33 C34 C26 179.5(3) . . . . ? C27 C26 C34 C29 -0.6(3) . . . . ? C11 C26 C34 C29 -179.9(2) . . . . ? C27 C26 C34 C33 179.5(3) . . . . ? C11 C26 C34 C33 0.2(4) . . . . ? O1 C8 N1 C7 -3.0(3) . . . . ? C9 C8 N1 C7 174.52(18) . . . . ? O1 C8 N1 C11 -179.3(2) . . . . ? C9 C8 N1 C11 -1.7(3) . . . . ? C1 C7 N1 C8 -83.7(3) . . . . ? C1 C7 N1 C11 92.9(2) . . . . ? C26 C11 N1 C8 -109.9(2) . . . . ? C10 C11 N1 C8 15.5(3) . . . . ? C26 C11 N1 C7 73.8(2) . . . . ? C10 C11 N1 C7 -160.76(18) . . . . ? O2 C12 N2 C10 168.8(3) . . . . ? C13 C12 N2 C10 -11.8(4) . . . . ? O2 C12 N2 C9 0.4(4) . . . . ? C13 C12 N2 C9 179.9(2) . . . . ? C11 C10 N2 C12 -103.0(3) . . . . ? C11 C10 N2 C9 66.3(2) . . . . ? C8 C9 N2 C12 119.1(2) . . . . ? C19 C9 N2 C12 -116.2(2) . . . . ? C8 C9 N2 C10 -50.8(2) . . . . ? C19 C9 N2 C10 74.0(2) . . . . ? C34 C29 N3 C27 -0.5(3) . . . . ? C30 C29 N3 C27 179.8(3) . . . . ? C34 C29 N3 C28 -178.0(3) . . . . ? C30 C29 N3 C28 2.3(5) . . . . ? C26 C27 N3 C29 0.1(3) . . . . ? C26 C27 N3 C28 177.5(3) . . . . ?