#------------------------------------------------------------------------------ #$Date: 2024-09-28 01:06:59 +0300 (Sat, 28 Sep 2024) $ #$Revision: 294921 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/26/1572697.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_1572697 loop_ _publ_author_name 'Pan, Xiuhong' 'Lan, Linfeng' 'Zhang, Hongyu' _publ_section_title ; Flexible Organic Crystals with Multi-Stimuli-Responsive CPL for Broadband Multicolor Optical Waveguides ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05005C _journal_year 2024 _chemical_absolute_configuration R _chemical_formula_moiety 'C16 H17 N O' _chemical_formula_sum 'C16 H17 N O' _chemical_formula_weight 239.30 _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 _atom_sites_solution_primary dual _audit_creation_date 2021-11-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488) ; _audit_update_record ; 2024-07-25 deposited with the CCDC. 2024-09-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 128.653(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.291(2) _cell_length_b 5.8861(6) _cell_length_c 14.4945(14) _cell_measurement_reflns_used 5364 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 67.83 _cell_measurement_theta_min 5.58 _cell_volume 1351.9(2) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10141 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.058 _diffrn_reflns_theta_min 5.583 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.176 _exptl_crystal_description needle _exptl_crystal_F_000 512 _refine_diff_density_max 0.123 _refine_diff_density_min -0.118 _refine_diff_density_rms 0.031 _refine_ls_abs_structure_details ; Flack x determined using 780 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_extinction_coef 0.0038(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2449 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0431 _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^)+(0.0541P)^2^+0.1802P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1078 _refine_ls_wR_factor_ref 0.1179 _reflns_Friedel_coverage 0.793 _reflns_Friedel_fraction_full 0.980 _reflns_Friedel_fraction_max 0.977 _reflns_number_gt 2030 _reflns_number_total 2449 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05005c3.cif _cod_data_source_block 1 _cod_database_code 1572697 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C6(H6) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C12(H12A,H12B,H12C) ; _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1_a.res in C2 CELL 1.54178 20.2913 5.8861 14.4945 90 128.653 90 ZERR 4 0.0021 0.0006 0.0014 0 0.004 0 LATT -7 SYMM -X,+Y,-Z SFAC C H N O UNIT 64 68 4 4 L.S. 16 PLAN -18 0 0 TEMP -173.15 HTAB BOND $H CONF fmap 2 acta REM REM REM WGHT 0.054100 0.180200 EXTI 0.003755 FVAR 0.76492 N1 3 0.526508 0.591820 0.377028 11.00000 0.07691 0.06050 = 0.05611 0.00130 0.03827 -0.00114 O2 4 0.597283 0.248873 0.522285 11.00000 0.08175 0.06677 = 0.08123 0.01016 0.04043 -0.00904 C1 1 0.909432 0.714924 0.760059 11.00000 0.08323 0.08687 = 0.09357 -0.01177 0.05327 -0.00866 AFIX 137 H1A 2 0.932873 0.691272 0.718730 11.00000 -1.50000 H1B 2 0.948854 0.655831 0.840768 11.00000 -1.50000 H1C 2 0.900587 0.877717 0.762693 11.00000 -1.50000 AFIX 0 C2 1 0.826184 0.591560 0.695309 11.00000 0.07552 0.06967 = 0.06801 -0.00951 0.04712 -0.00364 C3 1 0.752743 0.683960 0.595792 11.00000 0.08047 0.05735 = 0.06720 -0.00035 0.05112 -0.00250 AFIX 43 H3 2 0.755338 0.826692 0.567596 11.00000 -1.20000 AFIX 0 C4 1 0.674966 0.574534 0.535421 11.00000 0.07610 0.05514 = 0.05867 -0.00177 0.04624 -0.00075 C5 1 0.599166 0.682832 0.433681 11.00000 0.08246 0.05566 = 0.06142 0.00234 0.04759 -0.00023 AFIX 43 H5 2 0.603990 0.826566 0.408557 11.00000 -1.20000 AFIX 0 C6 1 0.452981 0.713051 0.275690 11.00000 0.07762 0.06014 = 0.06080 0.00791 0.04141 0.00351 AFIX 13 H6 2 0.473121 0.851925 0.260216 11.00000 -1.20000 AFIX 0 C7 1 0.409646 0.558413 0.168890 11.00000 0.07034 0.06339 = 0.06021 0.00798 0.03935 0.00903 C8 1 0.412074 0.605855 0.077590 11.00000 0.09265 0.08067 = 0.06616 0.00995 0.05083 0.00799 AFIX 43 H8 2 0.439208 0.739929 0.080071 11.00000 -1.20000 AFIX 0 C9 1 0.375134 0.458816 -0.017429 11.00000 0.11773 0.10828 = 0.06410 0.01149 0.05661 0.02241 AFIX 43 H9 2 0.376899 0.493815 -0.079839 11.00000 -1.20000 AFIX 0 C10 1 0.336080 0.263625 -0.022766 11.00000 0.09518 0.08936 = 0.06314 -0.00398 0.03360 0.02001 AFIX 43 H10 2 0.311610 0.162521 -0.087687 11.00000 -1.20000 AFIX 0 C11 1 0.820002 0.381534 0.733470 11.00000 0.07684 0.07415 = 0.06729 0.00438 0.04157 0.00749 AFIX 43 H11 2 0.869509 0.314005 0.801543 11.00000 -1.20000 AFIX 0 C12 1 0.396757 0.786012 0.305799 11.00000 0.09900 0.08075 = 0.07386 0.00244 0.05438 0.01184 AFIX 137 H12A 2 0.381542 0.652891 0.329539 11.00000 -1.50000 H12B 2 0.345425 0.856613 0.236420 11.00000 -1.50000 H12C 2 0.426960 0.895695 0.370902 11.00000 -1.50000 AFIX 0 C13 1 0.369779 0.360951 0.161999 11.00000 0.08991 0.07178 = 0.06805 0.00330 0.04823 -0.00189 AFIX 43 H13 2 0.367853 0.324374 0.224117 11.00000 -1.20000 AFIX 0 C14 1 0.332831 0.216388 0.066836 11.00000 0.08919 0.07582 = 0.07574 -0.00356 0.03938 0.00075 AFIX 43 H14 2 0.304929 0.083125 0.063334 11.00000 -1.20000 AFIX 0 C15 1 0.671103 0.361538 0.576288 11.00000 0.07846 0.05550 = 0.06571 -0.00109 0.04554 -0.00265 C16 1 0.744371 0.268855 0.675578 11.00000 0.08561 0.06060 = 0.07594 0.00719 0.04852 0.00201 AFIX 43 H16 2 0.742510 0.125752 0.704191 11.00000 -1.20000 AFIX 0 H2 2 0.551537 0.350037 0.455790 11.00000 0.10295 HKLF 4 REM 1_a.res in C2 REM R1 = 0.0431 for 2030 Fo > 4sig(Fo) and 0.0528 for all 2449 data REM 170 parameters refined using 1 restraints END WGHT 0.0535 0.1808 REM Instructions for potential hydrogen bonds HTAB O2 N1 REM Highest difference peak 0.123, deepest hole -0.118, 1-sigma level 0.031 Q1 1 0.8389 0.4069 0.6827 11.00000 0.05 0.12 Q2 1 0.6534 0.5922 0.5795 11.00000 0.05 0.12 Q3 1 0.3297 0.7029 0.0957 11.00000 0.05 0.12 Q4 1 0.6905 0.3816 0.5292 11.00000 0.05 0.12 Q5 1 0.6681 0.4894 0.5577 11.00000 0.05 0.12 Q6 1 0.7218 0.6705 0.6207 11.00000 0.05 0.12 Q7 1 0.8094 0.5627 0.7500 11.00000 0.05 0.11 Q8 1 0.4458 0.3181 0.1030 11.00000 0.05 0.11 Q9 1 0.4284 0.1842 0.0797 11.00000 0.05 0.10 Q10 1 0.5354 0.2615 0.5636 11.00000 0.05 0.10 Q11 1 0.5754 0.2650 0.5844 11.00000 0.05 0.10 Q12 1 0.9707 0.3719 0.8786 11.00000 0.05 0.09 Q13 1 0.3814 0.3417 0.0177 11.00000 0.05 0.09 Q14 1 0.9222 0.7609 0.8373 11.00000 0.05 0.09 Q15 1 0.9002 0.2879 0.7865 11.00000 0.05 0.09 Q16 1 0.5631 0.7359 0.4571 11.00000 0.05 0.09 Q17 1 0.6777 0.7872 0.5734 11.00000 0.05 0.09 Q18 1 0.9671 0.5978 0.8109 11.00000 0.05 0.09 ; _shelx_res_checksum 34531 _shelx_hkl_file ; 2 0 0 221.68 14.30 -2 0 0 192.98 14.30 -2 0 0 203.98 14.30 4 0 0 5651.33 358.26 -4 0 0 4828.32 357.96 6 0 0 296.27 20.20 -6 0 0 275.27 20.10 8 0 0 6.00 1.40 8 0 0 7.50 2.00 -8 0 0 6.10 0.80 -10 0 0 24.10 3.00 -10 0 0 22.60 2.20 10 0 0 21.00 2.60 10 0 0 19.10 2.40 10 0 0 16.00 3.70 12 0 0 391.86 29.60 -12 0 0 393.06 29.10 12 0 0 377.66 28.30 -12 0 0 452.25 29.50 -12 0 0 402.86 28.00 12 0 0 354.36 28.10 -14 0 0 272.37 22.10 -14 0 0 289.67 20.80 14 0 0 296.67 22.80 -14 0 0 303.87 22.50 -16 0 0 10.20 2.30 -16 0 0 9.40 3.20 16 0 0 10.40 2.60 -16 0 0 10.30 1.90 -18 0 0 0.40 0.60 -18 0 0 4.40 1.90 18 0 0 -0.60 0.80 1 -1 0 2723.03 169.98 -1 1 0 2563.64 170.38 -1 1 0 2173.28 169.88 3 -1 0 2457.85 182.48 3 -1 0 2612.04 182.48 -3 1 0 2571.44 182.58 -3 1 0 3038.90 182.68 5 -1 0 573.44 40.90 -5 -1 0 608.34 40.90 5 -1 0 593.64 41.20 5 -1 0 585.54 40.90 -5 1 0 609.04 41.10 -7 -1 0 104.29 7.90 7 -1 0 104.49 8.10 7 -1 0 109.99 8.60 7 1 0 116.69 10.10 -7 1 0 116.99 9.00 9 -1 0 58.79 4.90 -9 -1 0 52.69 4.30 -9 -1 0 51.39 4.30 9 -1 0 59.79 5.10 9 -1 0 55.39 5.90 9 1 0 50.09 6.70 -9 1 0 53.79 5.90 -9 1 0 55.09 5.40 11 -1 0 6.40 2.10 -11 -1 0 4.30 0.90 11 -1 0 3.20 1.20 -11 -1 0 4.90 0.90 11 -1 0 4.20 1.40 -11 -1 0 7.10 1.90 11 1 0 5.70 2.70 -11 1 0 5.10 2.00 -11 1 0 1.80 1.70 -11 1 0 6.00 1.70 13 -1 0 40.00 4.20 -13 -1 0 43.70 3.90 -13 -1 0 42.90 4.70 13 -1 0 40.60 4.40 13 -1 0 45.70 5.30 -13 1 0 38.90 4.70 -13 1 0 39.10 6.60 13 1 0 43.80 5.30 -13 1 0 46.80 5.60 15 -1 0 2.20 1.10 -15 -1 0 3.80 1.50 -15 -1 0 1.20 1.30 -15 -1 0 4.10 1.50 -15 -1 0 2.80 1.00 15 -1 0 0.50 1.40 -15 1 0 1.90 1.10 -15 1 0 3.50 2.80 15 1 0 4.10 1.50 -17 -1 0 4.70 1.20 -17 -1 0 3.70 1.40 17 -1 0 4.90 1.70 17 1 0 0.80 1.80 17 1 0 6.70 1.50 -17 1 0 5.10 1.20 0 2 0 4884.11 334.67 2 -2 0 287.97 20.70 2 -2 0 300.97 20.80 -2 2 0 308.57 21.80 -4 -2 0 272.27 19.50 4 -2 0 266.27 19.40 4 -2 0 285.37 19.50 4 -2 0 290.17 19.60 4 2 0 320.87 21.90 -4 2 0 252.37 19.60 -4 2 0 279.37 20.70 -6 -2 0 825.42 58.49 6 -2 0 895.01 59.19 -6 -2 0 859.81 58.69 6 -2 0 835.12 58.89 6 -2 0 795.92 58.49 6 -2 0 809.92 58.49 6 2 0 847.22 61.39 -6 2 0 921.91 59.69 -6 2 0 862.31 60.49 8 -2 0 71.69 6.10 8 -2 0 72.49 5.60 8 -2 0 74.89 6.40 -8 -2 0 76.29 5.60 -8 -2 0 69.79 5.50 -8 2 0 73.49 6.40 8 2 0 54.49 7.80 -8 2 0 80.99 8.20 -8 2 0 70.69 6.10 -8 2 0 71.29 6.20 -8 2 0 61.59 6.30 -8 2 0 77.19 6.50 -10 -2 0 16.90 1.80 -10 -2 0 17.90 1.80 10 -2 0 15.10 2.40 10 -2 0 18.00 2.70 10 2 0 14.40 4.70 -10 2 0 18.40 2.60 -10 2 0 17.00 2.50 -10 2 0 13.00 3.80 -10 2 0 20.40 3.10 -10 2 0 14.50 2.70 -12 -2 0 66.89 5.30 -12 -2 0 64.59 5.40 -12 -2 0 76.69 8.00 12 -2 0 58.79 6.80 12 -2 0 72.29 6.10 12 -2 0 75.69 6.60 -12 2 0 65.89 6.40 -12 2 0 73.09 7.40 -12 2 0 59.29 6.20 -12 2 0 61.39 6.20 12 2 0 63.59 6.60 -12 2 0 59.29 6.30 -12 2 0 67.59 9.20 -14 -2 0 26.40 3.80 14 -2 0 29.10 4.40 -14 -2 0 25.00 2.90 14 -2 0 27.30 3.60 -14 -2 0 34.30 2.90 14 -2 0 31.10 3.50 -14 2 0 32.90 6.30 14 2 0 29.20 4.00 -14 2 0 28.90 3.50 -14 2 0 38.70 4.90 -16 -2 0 8.10 1.50 16 -2 0 10.40 1.70 16 -2 0 9.50 2.10 -16 -2 0 13.20 2.00 -16 -2 0 7.70 1.30 -16 -2 0 7.50 1.60 16 -2 0 10.00 2.80 16 2 0 7.50 1.90 -16 2 0 11.70 2.20 16 2 0 4.80 2.10 -18 -2 0 0.30 0.60 18 2 0 0.80 0.70 -18 2 0 0.50 0.50 1 -3 0 431.96 31.30 -1 -3 0 441.76 31.50 1 -3 0 441.36 31.50 -1 3 0 490.05 33.20 3 -3 0 38.60 3.40 3 -3 0 43.70 3.50 -3 -3 0 38.90 3.30 3 -3 0 44.50 3.40 -3 3 0 49.30 5.00 -5 -3 0 6.50 1.30 5 -3 0 3.90 0.90 -5 -3 0 5.10 1.00 5 -3 0 4.00 1.10 5 -3 0 5.60 0.90 -5 3 0 7.00 3.10 -5 3 0 5.20 1.30 -5 3 0 4.60 1.30 -5 3 0 5.20 1.50 -5 3 0 3.40 1.80 7 -3 0 44.70 4.60 7 -3 0 43.60 3.70 7 -3 0 47.60 3.70 -7 -3 0 42.20 3.80 7 -3 0 41.60 4.80 -7 -3 0 47.60 3.80 -7 3 0 44.90 4.90 -7 3 0 45.20 4.70 -7 3 0 37.10 4.60 -7 3 0 46.00 4.70 -7 3 0 47.60 4.10 -7 3 0 38.00 5.60 -9 -3 0 4.60 0.90 9 -3 0 3.90 1.10 9 -3 0 4.50 1.70 -9 -3 0 4.50 1.00 9 -3 0 3.40 1.30 -9 3 0 4.70 1.20 -9 3 0 4.60 1.60 -9 3 0 1.60 2.10 -9 3 0 3.40 1.10 -9 3 0 2.70 1.90 -9 3 0 5.80 1.60 11 -3 0 132.79 10.00 -11 -3 0 119.09 9.00 11 -3 0 126.99 10.30 -11 -3 0 129.29 9.00 11 3 0 117.59 10.20 -11 3 0 119.39 9.80 -11 3 0 108.89 13.00 -11 3 0 122.39 10.40 -11 3 0 99.79 10.10 -11 3 0 120.79 10.00 -13 -3 0 10.10 1.30 13 -3 0 13.10 2.40 -13 -3 0 9.20 1.40 -13 3 0 7.60 1.90 -13 3 0 15.20 4.60 -13 3 0 7.10 1.80 -13 3 0 14.60 3.00 13 3 0 13.80 2.30 -13 3 0 10.30 2.10 -15 -3 0 13.00 1.80 -15 -3 0 14.30 2.40 15 -3 0 18.00 2.60 15 -3 0 19.90 2.40 -15 -3 0 18.60 2.00 15 3 0 12.50 3.30 -15 3 0 17.30 2.20 15 3 0 20.90 2.60 -17 -3 0 3.30 0.90 17 3 0 3.40 0.90 -17 3 0 2.50 0.70 0 -4 0 38.10 3.90 0 -4 0 44.20 3.80 0 4 0 45.40 5.80 0 4 0 39.50 4.10 0 4 0 43.80 5.70 0 4 0 36.30 4.20 -2 -4 0 5.00 1.40 -2 -4 0 3.60 1.10 2 -4 0 6.00 1.20 2 -4 0 4.40 0.90 2 -4 0 3.50 1.00 -2 -4 0 5.90 1.00 2 4 0 5.80 1.50 -2 4 0 3.70 2.40 2 4 0 4.50 3.70 2 4 0 3.60 1.30 2 4 0 4.10 4.10 -2 4 0 4.90 2.00 -2 4 0 1.60 1.30 -2 4 0 16.60 6.60 -2 4 0 5.40 1.90 4 -4 0 5.70 1.00 4 -4 0 6.70 2.20 -4 -4 0 8.40 1.20 4 -4 0 7.90 1.20 4 -4 0 10.40 1.60 -4 4 0 6.90 2.90 -4 4 0 7.00 2.00 -4 4 0 7.00 2.00 -4 4 0 8.90 2.20 4 4 0 10.50 1.80 4 4 0 7.10 3.90 -6 -4 0 184.48 13.70 6 -4 0 188.48 13.60 6 -4 0 173.78 14.30 -6 -4 0 195.28 13.60 6 -4 0 187.58 14.10 6 -4 0 211.48 13.80 -6 -4 0 184.08 15.80 6 4 0 174.08 17.80 -6 4 0 172.38 13.30 -6 4 0 194.18 14.80 -6 4 0 191.98 14.90 -6 4 0 183.68 17.30 -6 4 0 187.58 15.60 -8 -4 0 28.80 2.50 8 -4 0 26.70 3.20 -8 -4 0 27.30 2.60 8 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-14 8.80 1.80 -12 4 14 7.70 2.40 10 -4 -14 2.40 1.20 10 -4 -14 -0.20 1.20 -10 4 14 2.00 0.70 -10 4 14 1.50 0.80 -10 4 14 3.20 1.20 22 0 -15 1.70 1.50 20 0 -15 2.90 1.30 -20 0 15 4.30 1.20 -20 0 15 2.50 1.00 -18 0 15 0.80 0.80 18 0 -15 0.50 1.00 16 0 -15 10.40 2.50 16 0 -15 17.00 2.60 -14 0 15 12.60 2.70 14 0 -15 8.70 2.20 14 0 -15 12.80 3.00 12 0 -15 -1.90 2.00 12 0 -15 -1.10 1.40 -12 0 15 0.10 0.90 12 0 -15 -1.20 1.00 -12 0 15 2.70 1.90 -10 0 15 9.70 2.40 10 0 -15 5.30 2.60 -10 0 15 7.60 1.80 10 0 -15 9.10 2.60 10 0 -15 5.20 2.00 8 0 -15 5.00 1.90 -8 0 15 8.50 1.80 -8 0 15 9.00 2.10 8 0 -15 7.40 2.10 6 0 -15 2.60 2.00 -6 0 15 4.40 1.20 -4 0 15 1.10 1.00 21 -1 -15 3.50 1.50 -21 -1 15 3.60 1.00 -21 1 15 7.50 1.50 -21 1 15 4.90 1.00 21 1 -15 4.90 1.50 19 -1 -15 1.80 1.50 19 -1 -15 -1.50 1.70 19 -1 -15 2.10 1.50 -19 -1 15 3.30 1.00 -19 1 15 3.10 1.00 -19 1 15 4.70 1.30 19 1 -15 1.40 1.40 17 -1 -15 6.00 1.90 17 -1 -15 7.50 2.40 -17 -1 15 7.60 1.80 -17 1 15 6.10 1.50 17 1 -15 5.30 2.10 15 -1 -15 11.60 2.80 -15 -1 15 11.30 2.20 15 -1 -15 7.40 2.70 15 -1 -15 10.70 2.30 15 1 -15 8.90 2.60 -15 1 15 11.50 2.00 -15 1 15 12.30 2.30 -13 -1 15 2.50 1.20 13 -1 -15 2.40 1.50 13 -1 -15 3.60 1.20 13 -1 -15 0.90 1.40 13 1 -15 0.20 1.40 -13 1 15 1.80 1.50 -13 1 15 2.30 1.30 -13 1 15 2.80 1.70 11 -1 -15 -0.80 1.00 11 -1 -15 2.20 1.30 -11 -1 15 1.00 0.90 11 -1 -15 0.30 2.00 -11 1 15 0.50 1.10 -11 1 15 2.90 1.60 11 1 -15 1.20 1.90 -9 -1 15 73.19 6.90 9 -1 -15 59.69 6.10 -9 1 15 80.69 7.00 -9 1 15 68.09 6.50 9 1 -15 62.29 7.10 7 -1 -15 0.90 1.30 -7 -1 15 3.20 1.20 7 -1 -15 1.40 2.40 -7 1 15 3.70 1.30 -7 1 15 4.60 1.20 -5 -1 15 0.10 0.90 5 -1 -15 1.50 1.50 -5 1 15 -0.20 0.70 -20 -2 15 2.20 0.90 20 -2 -15 -0.30 1.10 20 -2 -15 3.60 1.40 20 2 -15 2.80 2.00 -20 2 15 3.60 0.90 -20 2 15 1.50 0.70 -18 -2 15 3.10 0.90 18 -2 -15 -0.20 1.50 18 -2 -15 1.80 1.80 18 -2 -15 2.60 1.40 18 2 -15 -0.40 2.10 -18 2 15 3.70 1.00 -18 2 15 3.50 0.90 -18 2 15 2.90 0.80 -16 -2 15 5.90 1.50 16 -2 -15 3.50 1.60 16 -2 -15 4.90 1.80 16 -2 -15 5.00 1.50 -16 2 15 4.50 1.20 -16 2 15 4.90 1.90 -16 2 15 5.20 1.10 -16 2 15 6.00 1.10 -16 2 15 5.30 1.50 16 2 -15 8.50 2.70 14 -2 -15 0.40 1.20 14 -2 -15 5.40 1.70 14 -2 -15 0.30 1.20 -14 2 15 2.10 1.10 14 2 -15 11.30 3.40 -14 2 15 3.00 1.00 -14 2 15 0.10 1.30 12 -2 -15 1.70 1.30 12 -2 -15 4.30 1.40 12 -2 -15 1.60 1.20 -12 2 15 2.00 1.40 -12 2 15 2.60 1.00 -12 2 15 3.10 1.60 10 -2 -15 18.60 2.90 10 -2 -15 25.40 3.00 -10 2 15 19.00 2.80 8 -2 -15 0.20 1.40 8 -2 -15 2.10 1.10 -8 -2 15 2.70 1.40 -8 2 15 2.80 1.40 -8 2 15 2.20 0.90 -8 2 15 3.50 0.90 -6 -2 15 -0.70 0.90 6 -2 -15 1.60 1.00 -6 2 15 -0.40 0.90 17 -3 -15 14.70 2.30 -17 -3 15 13.50 1.90 17 -3 -15 11.00 2.10 -17 3 15 18.40 2.30 15 -3 -15 18.80 2.70 15 -3 -15 16.40 3.10 15 -3 -15 23.00 3.30 -15 3 15 22.50 2.60 -15 3 15 16.10 2.90 13 -3 -15 -1.70 1.10 13 -3 -15 0.70 1.40 13 -3 -15 1.70 1.40 -13 -3 15 1.40 1.20 -13 3 15 0.20 0.60 -13 3 15 -0.60 0.80 -13 3 15 -0.60 0.90 11 -3 -15 0.70 1.00 11 -3 -15 -0.30 1.10 -11 -3 15 4.70 1.30 11 -3 -15 -1.00 1.40 -11 3 15 1.20 1.10 -11 3 15 1.20 0.90 -11 3 15 -0.30 0.70 -9 -3 15 -0.10 1.40 -9 3 15 -1.00 1.00 -9 3 15 0.50 1.00 -9 3 15 1.30 0.60 -20 0 16 -1.00 0.40 20 0 -16 1.00 1.20 18 0 -16 0.90 1.30 -18 0 16 2.00 0.90 16 0 -16 9.90 2.90 16 0 -16 17.60 2.80 -16 0 16 16.70 2.50 14 0 -16 2.80 1.90 -14 0 16 3.90 1.40 14 0 -16 8.20 2.00 -12 0 16 3.80 1.30 12 0 -16 1.50 1.40 12 0 -16 0.90 2.50 -10 0 16 21.10 2.90 10 0 -16 19.20 3.20 -10 0 16 26.60 5.30 -8 0 16 -0.30 0.80 -21 -1 16 1.70 0.80 -21 1 16 1.10 0.70 -21 1 16 0.10 0.50 -19 -1 16 1.20 0.70 19 -1 -16 0.30 1.60 19 -1 -16 3.30 0.90 19 1 -16 -1.10 1.00 -19 1 16 1.00 0.70 -19 1 16 0.10 0.70 17 -1 -16 4.50 1.70 -17 -1 16 3.80 1.20 17 -1 -16 2.00 2.00 17 -1 -16 6.90 1.60 -17 1 16 4.10 1.20 17 1 -16 6.20 1.60 -17 1 16 6.50 1.30 15 -1 -16 3.10 2.50 15 -1 -16 2.50 1.40 15 -1 -16 1.00 1.20 -15 -1 16 1.10 0.80 -15 1 16 2.70 1.00 15 1 -16 0.20 1.70 -13 -1 16 0.60 1.00 13 -1 -16 -0.20 1.20 13 -1 -16 -0.60 2.00 13 -1 -16 0.70 1.10 -13 1 16 2.90 1.20 -13 1 16 0.60 0.90 13 1 -16 -3.60 1.80 -11 -1 16 0.00 0.80 11 -1 -16 0.10 1.20 11 -1 -16 0.60 2.00 11 -1 -16 -0.20 0.90 -11 1 16 -0.10 0.80 -11 1 16 -0.50 1.20 11 1 -16 7.30 4.20 9 -1 -16 15.40 2.70 -9 -1 16 22.80 2.90 -9 1 16 20.30 2.50 -9 1 16 24.00 3.10 -7 -1 16 2.40 1.00 -7 1 16 0.50 0.70 -7 1 16 2.50 1.80 18 -2 -16 4.90 1.60 -18 -2 16 6.10 1.10 18 -2 -16 5.40 1.80 -18 2 16 7.10 1.60 16 -2 -16 2.50 1.40 16 -2 -16 2.70 1.80 -16 -2 16 1.50 0.80 16 -2 -16 1.30 1.10 -16 2 16 1.70 0.90 14 -2 -16 -1.70 1.30 -14 -2 16 -0.30 0.70 14 -2 -16 -0.70 1.50 14 -2 -16 -0.50 0.80 -14 2 16 0.00 0.70 12 -2 -16 8.80 1.70 -12 -2 16 12.30 1.80 12 -2 -16 6.60 2.30 12 -2 -16 6.00 2.00 -12 2 16 13.20 2.00 -12 2 16 11.30 2.20 -10 -2 16 16.30 2.10 10 -2 -16 9.90 2.00 -10 2 16 13.90 1.90 -10 2 16 16.10 2.40 18 0 -17 1.90 1.20 -18 0 17 1.90 0.70 -18 0 17 1.30 0.60 16 0 -17 -0.30 1.10 -16 0 17 0.30 0.60 -14 0 17 5.20 1.10 14 0 -17 3.30 1.90 12 0 -17 4.20 2.00 -12 0 17 7.10 1.40 -17 -1 17 4.80 1.00 17 -1 -17 4.60 1.60 -17 1 17 2.80 0.90 -17 1 17 2.50 0.70 17 1 -17 1.80 2.10 15 -1 -17 1.40 1.00 15 -1 -17 2.90 2.10 -15 -1 17 0.60 0.70 -15 1 17 0.30 0.50 -15 1 17 0.30 0.60 -13 -1 17 6.30 1.30 13 -1 -17 2.50 1.40 -13 1 17 3.70 0.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 76105 _olex2_submission_special_instructions 'No special instructions were received' 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 N1 N 0.52651(15) 0.5918(4) 0.37703(19) 0.0667(6) Uani 1 1 d . . . . . O2 O 0.59728(14) 0.2489(4) 0.5223(2) 0.0837(6) Uani 1 1 d . . . . . C1 C 0.90943(19) 0.7149(7) 0.7601(3) 0.0892(10) Uani 1 1 d . . . . . H1A H 0.9329 0.6913 0.7187 0.134 Uiso 1 1 calc GR . . . . H1B H 0.9489 0.6558 0.8408 0.134 Uiso 1 1 calc GR . . . . H1C H 0.9006 0.8777 0.7627 0.134 Uiso 1 1 calc GR . . . . C2 C 0.82618(17) 0.5916(5) 0.6953(2) 0.0695(7) Uani 1 1 d . . . . . C3 C 0.75274(17) 0.6840(5) 0.5958(2) 0.0649(7) Uani 1 1 d . . . . . H3 H 0.7553 0.8267 0.5676 0.078 Uiso 1 1 calc R . . . . C4 C 0.67497(17) 0.5745(5) 0.5354(2) 0.0605(6) Uani 1 1 d . . . . . C5 C 0.59917(18) 0.6828(5) 0.4337(2) 0.0647(7) Uani 1 1 d . . . . . H5 H 0.6040 0.8266 0.4086 0.078 Uiso 1 1 calc R . . . . C6 C 0.45298(17) 0.7131(5) 0.2757(2) 0.0674(7) Uani 1 1 d . . . . . H6 H 0.4731 0.8519 0.2602 0.081 Uiso 1 1 calc R . . . . C7 C 0.40965(16) 0.5584(5) 0.1689(2) 0.0656(7) Uani 1 1 d . . . . . C8 C 0.4121(2) 0.6059(6) 0.0776(3) 0.0790(8) Uani 1 1 d . . . . . H8 H 0.4392 0.7399 0.0801 0.095 Uiso 1 1 calc R . . . . C9 C 0.3751(3) 0.4588(8) -0.0174(3) 0.0968(11) Uani 1 1 d . . . . . H9 H 0.3769 0.4938 -0.0798 0.116 Uiso 1 1 calc R . . . . C10 C 0.3361(2) 0.2636(8) -0.0228(3) 0.0934(11) Uani 1 1 d . . . . . H10 H 0.3116 0.1625 -0.0877 0.112 Uiso 1 1 calc R . . . . C11 C 0.8200(2) 0.3815(6) 0.7335(3) 0.0751(8) Uani 1 1 d . . . . . H11 H 0.8695 0.3140 0.8015 0.090 Uiso 1 1 calc R . . . . C12 C 0.3968(2) 0.7860(6) 0.3058(3) 0.0843(9) Uani 1 1 d . . . . . H12A H 0.3815 0.6529 0.3295 0.126 Uiso 1 1 calc GR . . . . H12B H 0.3454 0.8566 0.2364 0.126 Uiso 1 1 calc GR . . . . H12C H 0.4270 0.8957 0.3709 0.126 Uiso 1 1 calc GR . . . . C13 C 0.3698(2) 0.3610(6) 0.1620(3) 0.0773(8) Uani 1 1 d . . . . . H13 H 0.3679 0.3244 0.2241 0.093 Uiso 1 1 calc R . . . . C14 C 0.3328(2) 0.2164(6) 0.0668(3) 0.0885(9) Uani 1 1 d . . . . . H14 H 0.3049 0.0831 0.0633 0.106 Uiso 1 1 calc R . . . . C15 C 0.67110(19) 0.3615(5) 0.5763(2) 0.0662(7) Uani 1 1 d . . . . . C16 C 0.74437(19) 0.2689(5) 0.6756(3) 0.0754(8) Uani 1 1 d . . . . . H16 H 0.7425 0.1258 0.7042 0.090 Uiso 1 1 calc R . . . . H2 H 0.552(2) 0.350(8) 0.456(3) 0.103(11) 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 N1 0.0769(14) 0.0605(13) 0.0561(12) 0.0013(10) 0.0383(11) -0.0011(11) O2 0.0817(13) 0.0668(12) 0.0812(14) 0.0102(11) 0.0404(11) -0.0090(11) C1 0.0832(19) 0.087(2) 0.094(2) -0.0118(18) 0.0533(17) -0.0087(18) C2 0.0755(17) 0.0697(17) 0.0680(16) -0.0095(14) 0.0471(14) -0.0036(14) C3 0.0805(17) 0.0574(15) 0.0672(16) -0.0004(13) 0.0511(14) -0.0025(13) C4 0.0761(15) 0.0551(14) 0.0587(13) -0.0018(11) 0.0462(13) -0.0008(12) C5 0.0825(17) 0.0557(14) 0.0614(15) 0.0023(12) 0.0476(14) -0.0002(13) C6 0.0776(16) 0.0601(16) 0.0608(15) 0.0079(13) 0.0414(14) 0.0035(13) C7 0.0703(15) 0.0634(16) 0.0602(14) 0.0080(12) 0.0393(13) 0.0090(13) C8 0.0927(19) 0.0807(19) 0.0662(16) 0.0099(15) 0.0508(15) 0.0080(16) C9 0.118(3) 0.108(3) 0.0641(18) 0.0115(19) 0.0566(19) 0.022(2) C10 0.095(2) 0.089(3) 0.0631(18) -0.0040(17) 0.0336(17) 0.020(2) C11 0.0768(18) 0.0742(19) 0.0673(17) 0.0044(15) 0.0416(15) 0.0075(15) C12 0.099(2) 0.081(2) 0.0739(18) 0.0024(15) 0.0544(18) 0.0118(17) C13 0.090(2) 0.0718(18) 0.0681(17) 0.0033(15) 0.0482(16) -0.0019(16) C14 0.0892(19) 0.076(2) 0.076(2) -0.0036(17) 0.0394(16) 0.0007(18) C15 0.0785(17) 0.0555(14) 0.0657(15) -0.0011(14) 0.0455(14) -0.0026(13) C16 0.0856(19) 0.0606(16) 0.0759(18) 0.0072(15) 0.0485(16) 0.0020(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 N1 C6 119.0(2) . . ? C15 O2 H2 107(2) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C3 C2 C1 121.2(3) . . ? C3 C2 C11 117.3(3) . . ? C11 C2 C1 121.6(3) . . ? C2 C3 H3 118.9 . . ? C2 C3 C4 122.2(3) . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 C15 119.0(2) . . ? C15 C4 C5 121.0(2) . . ? N1 C5 C4 122.3(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N1 C6 H6 108.6 . . ? N1 C6 C7 108.0(2) . . ? N1 C6 C12 109.1(2) . . ? C7 C6 H6 108.6 . . ? C7 C6 C12 113.8(2) . . ? C12 C6 H6 108.6 . . ? C8 C7 C6 120.7(3) . . ? C8 C7 C13 118.0(3) . . ? C13 C7 C6 121.2(2) . . ? C7 C8 H8 119.8 . . ? C7 C8 C9 120.3(3) . . ? C9 C8 H8 119.8 . . ? C8 C9 H9 119.5 . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9 119.5 . . ? C9 C10 H10 120.5 . . ? C14 C10 C9 119.0(4) . . ? C14 C10 H10 120.5 . . ? C2 C11 H11 119.0 . . ? C16 C11 C2 122.0(3) . . ? C16 C11 H11 119.0 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13 119.4 . . ? C14 C13 C7 121.3(3) . . ? C14 C13 H13 119.4 . . ? C10 C14 C13 120.4(4) . . ? C10 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? O2 C15 C4 121.7(3) . . ? O2 C15 C16 119.4(3) . . ? C16 C15 C4 118.9(3) . . ? C11 C16 C15 120.7(3) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? 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 N1 C5 1.274(3) . ? N1 C6 1.468(3) . ? O2 C15 1.353(3) . ? O2 H2 1.01(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.510(4) . ? C2 C3 1.383(4) . ? C2 C11 1.392(5) . ? C3 H3 0.9500 . ? C3 C4 1.395(4) . ? C4 C5 1.454(4) . ? C4 C15 1.410(4) . ? C5 H5 0.9500 . ? C6 H6 1.0000 . ? C6 C7 1.516(4) . ? C6 C12 1.516(4) . ? C7 C8 1.383(4) . ? C7 C13 1.384(4) . ? C8 H8 0.9500 . ? C8 C9 1.385(5) . ? C9 H9 0.9500 . ? C9 C10 1.370(6) . ? C10 H10 0.9500 . ? C10 C14 1.369(5) . ? C11 H11 0.9500 . ? C11 C16 1.375(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13 0.9500 . ? C13 C14 1.377(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(4) . ? C16 H16 0.9500 . ? 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 N1 C6 C7 C8 -109.8(3) . . . . ? N1 C6 C7 C13 67.4(3) . . . . ? O2 C15 C16 C11 -178.8(3) . . . . ? C1 C2 C3 C4 -179.2(2) . . . . ? C1 C2 C11 C16 179.5(3) . . . . ? C2 C3 C4 C5 177.8(2) . . . . ? C2 C3 C4 C15 -0.7(4) . . . . ? C2 C11 C16 C15 0.1(5) . . . . ? C3 C2 C11 C16 -0.1(4) . . . . ? C3 C4 C5 N1 -178.6(2) . . . . ? C3 C4 C15 O2 179.1(2) . . . . ? C3 C4 C15 C16 0.6(4) . . . . ? C4 C15 C16 C11 -0.3(4) . . . . ? C5 N1 C6 C7 123.6(3) . . . . ? C5 N1 C6 C12 -112.2(3) . . . . ? C5 C4 C15 O2 0.6(4) . . . . ? C5 C4 C15 C16 -177.9(3) . . . . ? C6 N1 C5 C4 179.6(2) . . . . ? C6 C7 C8 C9 177.5(3) . . . . ? C6 C7 C13 C14 -177.8(3) . . . . ? C7 C8 C9 C10 -0.4(5) . . . . ? C7 C13 C14 C10 1.1(5) . . . . ? C8 C7 C13 C14 -0.6(4) . . . . ? C8 C9 C10 C14 0.9(5) . . . . ? C9 C10 C14 C13 -1.3(5) . . . . ? C11 C2 C3 C4 0.4(4) . . . . ? C12 C6 C7 C8 129.0(3) . . . . ? C12 C6 C7 C13 -53.9(4) . . . . ? C13 C7 C8 C9 0.2(4) . . . . ? C15 C4 C5 N1 -0.1(4) . . . . ?