#------------------------------------------------------------------------------ #$Date: 2021-07-14 07:57:56 +0300 (Wed, 14 Jul 2021) $ #$Revision: 267525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243868.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243868 loop_ _publ_author_name 'Martens, Viktor' 'G\"orls, Helmar' 'Imhof, Wolfgang' _publ_section_title ; Crystal structure of 2-oxo-2-phenylethyl diisopropylcarbamate ; _journal_coeditor_code ZL5014 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 785 _journal_page_last 787 _journal_paper_doi 10.1107/S2056989021006927 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C15 H21 N O3' _chemical_formula_moiety 'C15 H21 N O3' _chemical_formula_sum 'C15 H21 N O3' _chemical_formula_weight 263.33 _chemical_name_systematic ; 2-oxo-2-phenylethyl diisopropylcarbamate ; _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 113.4680(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.4574(8) _cell_length_b 5.7020(2) _cell_length_c 14.8058(6) _cell_measurement_reflns_used 13968 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 27.482 _cell_measurement_theta_min 2.751 _cell_volume 1429.33(10) _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) ; _computing_data_collection ; COLLECT (Nonius 1998) ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) ; _computing_molecular_graphics ; ORTEP-3 (Farrugia, 2012) ; _computing_publication_material ; MERCURY (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 133(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi + omega - scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_unetI/netI 0.0478 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 13968 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 2.751 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 568 _exptl_crystal_size_max 0.102 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.084 _refine_diff_density_max 0.267 _refine_diff_density_min -0.206 _refine_ls_extinction_coef 0.0093(16) _refine_ls_extinction_method ; SHELXL2018/3 (Sheldrick 2015) ; _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 177 _refine_ls_number_reflns 3280 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0494 _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^)+(0.0368P)^2^+0.6743P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.1131 _reflns_number_gt 2464 _reflns_number_total 3280 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl5014sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2243868 _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 0.991 _shelx_estimated_absorpt_t_max 0.993 _shelx_hkl_file ; 1 0 0 -0.2586 0.19365 1 1 0 0 0.13959 0.34014 4 -1 0 0 0.51946 0.44770 2 -2 0 0 4231.45 285.659 2 2 0 0 4213.62 260.145 4 2 0 0 3401.65 265.795 2 2 0 0 4062.66 259.186 1 -2 0 0 4277.78 274.272 4 -2 0 0 4229.63 272.782 1 3 0 0 1.77065 1.18732 4 -3 0 0 -0.3149 1.20992 2 3 0 0 0.79952 0.99070 2 -3 0 0 0.83123 1.13705 4 3 0 0 1.02020 0.66511 1 -3 0 0 0.14376 0.51399 1 5 0 0 5.99453 1.63568 1 5 0 0 4.39658 1.60704 2 -5 0 0 7.44037 1.60248 2 5 0 0 3.14920 1.80969 4 -5 0 0 4.99480 1.72855 4 -5 0 0 6.07373 1.42992 1 -6 0 0 46.2038 6.13509 2 6 0 0 62.1080 9.03396 4 -6 0 0 42.2279 6.26042 4 6 0 0 44.7038 4.56035 2 6 0 0 52.9522 8.46299 1 -6 0 0 51.1438 7.35325 1 -7 0 0 16.7450 2.99409 1 -7 0 0 15.7334 3.12710 2 7 0 0 22.2854 4.88293 1 -7 0 0 12.4279 2.50223 4 7 0 0 20.3870 4.36343 4 -8 0 0 128.637 9.99981 2 8 0 0 127.778 9.53817 2 -8 0 0 133.765 9.62032 4 8 0 0 142.416 9.97728 1 -8 0 0 132.291 9.26607 1 8 0 0 148.608 9.88919 4 9 0 0 6.43114 2.95949 4 -9 0 0 2.36815 3.19831 2 -9 0 0 0.42676 1.17249 1 9 0 0 -0.5623 2.30566 2 10 0 0 69.9775 5.96651 1 10 0 0 63.0503 6.43503 2 10 0 0 74.6747 6.64865 4 -10 0 0 66.3425 6.61430 2 11 0 0 16.0816 4.24151 2 11 0 0 30.8179 5.73081 1 -11 0 0 21.9651 5.27682 2 12 0 0 401.489 31.9931 1 -12 0 0 395.333 27.7104 2 12 0 0 414.871 33.9291 4 -13 0 0 32.2135 7.34186 2 13 0 0 45.1851 7.37582 1 13 0 0 57.7831 9.17067 4 14 0 0 96.4036 9.26382 4 14 0 0 87.6718 8.13990 1 -14 0 0 73.6818 10.3247 2 15 0 0 9.21226 2.52981 1 15 0 0 19.4066 6.19437 4 -15 0 0 13.6425 7.75517 2 -16 0 0 57.9093 10.8270 2 16 0 0 48.1100 8.17482 4 16 0 0 46.3214 5.51123 1 17 0 0 -0.4237 7.32088 4 -17 0 0 -1.1317 8.91374 2 0 -1 0 1.31413 0.70310 3 0 1 0 -0.5003 0.81353 3 1 -1 0 2550.43 176.226 1 -1 -1 0 2626.79 169.521 3 1 -1 0 2648.12 171.599 4 -1 1 0 2695.18 180.842 1 -1 1 0 2664.25 168.697 4 1 1 0 2685.50 164.146 3 2 -1 0 937.404 62.3863 4 -2 -1 0 919.637 59.5875 1 -2 -1 0 895.115 60.7024 2 -2 -1 0 934.088 61.5234 4 2 -1 0 871.365 62.9008 1 -2 -1 0 921.672 60.5114 3 -2 1 0 915.189 58.1169 1 -2 1 0 929.786 65.9354 4 2 1 0 942.952 58.5958 3 -3 -1 0 8087.29 538.832 1 -3 -1 0 8802.18 535.077 4 3 -1 0 8138.81 548.146 1 3 -1 0 8062.62 549.273 4 3 -1 0 8644.37 553.448 2 -3 -1 0 8074.79 583.429 2 3 1 0 8491.50 528.187 3 3 1 0 8449.85 570.097 1 -3 1 0 8557.24 524.879 1 3 1 0 8573.50 526.732 2 3 1 0 8311.96 569.819 4 -3 1 0 8440.92 527.358 4 -4 -1 0 3971.94 253.651 1 -4 -1 0 4145.31 256.011 4 -4 -1 0 4178.47 261.331 2 4 -1 0 3972.06 256.026 4 4 -1 0 4080.12 260.492 2 4 -1 0 3927.52 263.456 1 4 1 0 3870.40 261.434 4 4 1 0 3997.39 257.189 2 -4 1 0 4018.26 255.927 4 -4 1 0 4010.66 261.055 1 4 1 0 4003.71 257.403 1 4 1 0 4076.41 255.501 3 5 -1 0 113.955 8.57646 2 -5 -1 0 112.420 8.16624 4 5 -1 0 112.777 8.24970 1 -5 -1 0 115.228 7.64083 1 5 -1 0 115.797 8.02240 4 -5 -1 0 128.462 8.41832 2 5 1 0 120.218 7.85963 3 5 1 0 116.836 8.26666 4 5 1 0 120.477 8.32117 1 -5 1 0 124.681 8.46632 1 -5 1 0 119.556 7.94270 4 -5 1 0 118.800 9.16605 2 5 1 0 128.340 8.44104 2 6 -1 0 421.500 28.3880 1 -6 -1 0 447.350 28.2035 4 -6 -1 0 444.280 27.7090 1 6 -1 0 450.593 28.7208 4 6 -1 0 456.857 27.9778 2 -6 -1 0 422.526 28.2255 2 6 1 0 385.118 27.9254 4 6 1 0 438.908 28.0542 3 6 1 0 440.424 31.2302 2 -6 1 0 434.788 28.7240 1 6 1 0 451.329 28.5291 1 -6 1 0 447.231 28.0819 4 -6 1 0 409.264 28.9383 2 -7 -1 0 1155.02 72.6991 1 7 -1 0 1096.75 71.6586 1 -7 -1 0 1169.04 71.3760 2 7 -1 0 1071.91 73.0466 2 7 -1 0 1073.36 71.0196 4 -7 -1 0 1093.08 71.3406 4 -7 1 0 1153.27 74.9220 4 7 1 0 1134.37 72.4101 2 -7 1 0 1155.86 72.2693 1 7 1 0 1177.79 76.6957 1 7 1 0 1111.53 72.8022 3 -7 1 0 1132.59 70.6694 2 7 1 0 1081.76 73.5875 4 8 -1 0 802.951 49.7929 1 8 -1 0 724.395 48.8932 4 -8 -1 0 769.961 49.3828 1 8 -1 0 761.371 49.7857 2 -8 -1 0 798.992 49.3378 4 -8 -1 0 756.651 50.1380 2 8 1 0 752.131 48.6164 4 8 1 0 749.077 51.8535 3 -8 1 0 795.208 49.2558 4 -8 1 0 789.078 49.2975 2 8 1 0 789.672 54.8252 2 -8 1 0 787.710 49.0155 1 8 1 0 770.045 52.5804 1 -9 -1 0 44.5685 5.14826 2 9 -1 0 37.3443 4.42951 4 9 -1 0 43.2233 4.70288 2 -9 -1 0 33.3962 3.20960 1 9 -1 0 48.2921 3.78735 1 9 1 0 34.3103 4.70631 4 -9 1 0 42.7431 3.76741 1 9 1 0 30.6056 4.64781 2 -9 1 0 46.5881 6.21023 2 9 1 0 42.0412 3.76486 1 10 -1 0 342.827 24.4672 4 10 -1 0 361.705 26.7048 1 10 -1 0 366.219 24.2728 2 -10 -1 0 388.241 24.4408 2 -10 1 0 355.982 26.1154 2 10 1 0 362.930 25.4606 2 10 1 0 384.309 24.4180 1 10 1 0 362.932 24.0845 4 -11 -1 0 137.415 11.4654 2 11 -1 0 148.100 11.1260 4 11 -1 0 147.891 9.80565 1 11 1 0 142.942 11.3215 4 -11 1 0 161.363 12.8608 2 11 1 0 138.078 9.81065 1 12 -1 0 171.204 13.6089 2 -12 -1 0 221.350 14.7550 2 12 -1 0 175.791 12.6546 1 12 -1 0 204.431 14.1162 4 12 1 0 180.826 14.1351 4 -12 1 0 184.951 15.5766 2 12 1 0 189.129 13.2365 1 13 -1 0 2.37803 1.56596 1 -13 -1 0 4.46844 4.93920 2 13 -1 0 -4.9054 4.13126 4 -13 1 0 -6.0272 5.88972 2 13 1 0 6.99286 4.76937 4 13 1 0 -1.4783 2.11876 1 -14 -1 0 4.84578 5.74084 2 14 -1 0 0.38819 4.69485 4 14 -1 0 0.21612 2.17948 1 -14 1 0 -5.9606 6.54941 2 14 1 0 7.86631 5.59144 4 14 1 0 0.01121 2.39704 1 15 -1 0 6.64904 2.83524 1 -15 -1 0 -3.8783 6.44503 2 15 -1 0 9.80586 5.57737 4 15 1 0 9.68137 3.15894 1 15 1 0 5.13265 6.14550 4 -15 1 0 1.74194 7.52864 2 16 -1 0 35.4629 7.35362 4 16 -1 0 38.2696 4.54509 1 -16 -1 0 30.2803 7.12866 2 -16 1 0 27.0487 7.65913 2 16 1 0 33.4650 8.02283 4 16 1 0 42.3010 5.07201 1 -17 -1 0 19.1049 9.50021 2 17 -1 0 12.0632 7.16700 4 17 1 0 12.4454 8.29637 4 0 -2 0 1.74656 1.17146 3 0 2 0 1.82014 1.32893 3 1 -2 0 562.810 35.6578 3 1 -2 0 547.033 38.8213 1 -1 -2 0 590.205 35.7897 3 1 -2 0 575.154 36.2476 4 1 2 0 581.025 37.5577 3 -2 -2 0 237.570 15.4101 3 2 -2 0 227.910 14.9356 4 2 -2 0 230.549 15.2477 1 -2 -2 0 237.601 15.9547 2 -2 2 0 226.089 14.8196 1 2 2 0 234.544 14.6307 3 -3 -2 0 -2.4164 2.60501 2 -3 -2 0 0.42578 1.17446 3 3 -2 0 2.46685 0.61391 1 3 -2 0 1.22329 0.89365 4 -3 -2 0 1.28729 1.68039 4 -3 -2 0 1.85130 0.62914 1 -3 2 0 2.57553 0.80974 1 3 2 0 -0.5245 1.36429 3 -3 2 0 1.44406 1.13644 4 -4 -2 0 130.141 9.84498 1 -4 -2 0 145.421 10.0998 2 4 -2 0 142.523 9.17141 4 -4 -2 0 144.949 9.20267 3 4 -2 0 133.690 9.60826 1 -4 -2 0 131.520 9.82055 4 -4 2 0 146.661 9.44564 1 4 2 0 142.749 9.28036 3 -4 2 0 140.710 9.03681 4 -5 -2 0 3.88462 2.69174 2 5 -2 0 0.39372 1.25716 4 5 -2 0 0.58139 0.83267 1 5 -2 0 -3.7026 3.09659 2 -5 -2 0 2.34348 0.82493 1 -5 -2 0 1.78695 1.79237 4 5 2 0 2.11257 1.38525 3 -5 2 0 0.25754 1.19948 4 -5 2 0 -0.6996 0.69511 1 6 -2 0 871.928 59.9479 4 -6 -2 0 894.048 55.8378 4 -6 -2 0 878.889 56.6076 2 6 -2 0 886.159 58.1988 1 -6 -2 0 890.650 59.4006 1 6 -2 0 878.026 64.9526 2 -6 2 0 898.389 59.7953 4 6 2 0 929.650 61.9210 3 -6 2 0 901.697 57.0409 1 6 2 0 950.981 72.5651 2 7 -2 0 789.554 54.4739 1 -7 -2 0 818.849 53.6366 2 7 -2 0 846.989 55.6985 4 -7 -2 0 835.945 53.7869 1 7 -2 0 753.616 52.3141 2 -7 -2 0 833.046 51.8131 4 7 2 0 831.795 53.8867 2 7 2 0 827.136 51.5835 3 -7 2 0 841.732 53.4273 4 -7 2 0 802.006 52.4107 1 7 2 0 839.364 55.0753 1 -8 -2 0 4.92355 3.25915 2 8 -2 0 -0.4104 3.70131 2 8 -2 0 3.00617 2.26169 4 -8 -2 0 5.35281 1.28854 1 8 -2 0 4.40462 1.28613 1 -8 2 0 4.27669 1.24637 1 8 2 0 5.28624 1.47136 1 -8 2 0 0.46794 1.99307 4 8 2 0 1.98283 2.31143 4 8 2 0 -1.2957 3.71824 2 8 2 0 2.78928 2.09519 3 -9 -2 0 372.486 22.5789 1 -9 -2 0 357.024 23.5169 2 9 -2 0 354.144 23.3825 4 9 -2 0 336.142 22.5033 1 9 -2 0 322.571 23.3284 2 9 2 0 367.156 24.3087 4 -9 2 0 338.993 26.2139 1 9 2 0 334.307 23.5316 1 10 -2 0 35.5371 4.69237 4 10 -2 0 43.3938 3.89937 1 10 -2 0 52.8247 5.95477 2 10 2 0 47.4811 6.11102 4 10 2 0 46.6823 3.89694 1 11 -2 0 13.2641 3.81942 4 11 -2 0 12.6432 2.19861 1 11 -2 0 2.25604 4.45755 2 -11 -2 0 7.97423 4.36054 2 11 2 0 9.79676 2.32503 1 11 2 0 14.1041 5.13387 4 -12 -2 0 18.4192 5.43659 2 12 -2 0 22.5362 4.58720 4 12 -2 0 26.5102 3.02013 1 12 2 0 24.7060 3.21066 1 12 2 0 25.3668 5.11966 4 -13 -2 0 -0.8628 5.06087 2 13 -2 0 -5.8558 4.21722 4 13 -2 0 -3.4645 1.96706 1 13 2 0 5.79855 2.42767 1 13 2 0 -0.5571 4.20573 4 14 -2 0 43.2993 4.50330 1 -14 -2 0 61.1141 8.14844 2 14 2 0 43.1740 5.66818 1 -15 -2 0 35.7684 8.00508 2 15 -2 0 36.1562 3.92541 1 16 -2 0 14.9950 6.44186 4 -16 -2 0 13.6868 7.67300 2 16 2 0 9.53845 3.89062 1 17 -2 0 12.6752 7.28773 4 -17 -2 0 3.29346 8.35864 2 0 -3 0 1.95740 1.42245 3 -1 -3 0 144.158 9.88549 3 1 -3 0 143.243 9.78616 3 1 -3 0 149.090 9.61064 4 1 -3 0 147.573 10.1048 1 1 3 0 140.759 9.97465 3 2 -3 0 103.508 7.48112 3 -2 -3 0 99.1885 7.04505 3 2 -3 0 114.823 6.92449 4 2 -3 0 99.6633 7.09784 1 2 3 0 103.332 7.24557 3 -3 -3 0 8.26896 3.73032 2 3 -3 0 13.8906 2.88729 4 3 -3 0 11.4172 2.59178 3 -3 -3 0 10.9191 2.09397 4 3 -3 0 17.9680 3.64802 1 -3 -3 0 9.21291 1.94639 3 3 3 0 5.27515 1.90323 3 -4 -3 0 275.701 18.1743 2 4 -3 0 260.134 17.1482 4 -4 -3 0 256.845 18.6432 1 -4 -3 0 260.742 17.7583 4 -4 -3 0 254.639 17.0127 3 4 -3 0 277.014 17.1385 1 -4 3 0 289.780 17.8551 1 4 3 0 239.811 17.5356 3 -5 -3 0 161.901 10.6267 1 5 -3 0 156.713 9.60317 1 -5 -3 0 149.634 9.73245 3 -5 -3 0 145.490 10.3154 4 -5 -3 0 139.534 11.2465 2 5 -3 0 143.855 9.77097 4 5 3 0 153.243 9.99850 3 -5 3 0 151.677 9.86154 1 -5 3 0 125.856 9.97012 4 6 -3 0 278.239 18.5415 4 -6 -3 0 284.955 19.0290 2 -6 -3 0 275.079 18.9444 4 6 -3 0 280.039 18.2947 1 -6 -3 0 274.198 19.3889 1 -6 -3 0 278.372 18.0125 3 -6 3 0 275.468 19.8855 1 6 3 0 280.515 19.0009 3 -6 3 0 267.808 17.6277 4 -7 -3 0 1.55449 1.36458 1 7 -3 0 2.90869 1.93270 4 -7 -3 0 3.06998 3.72130 2 7 -3 0 0.36140 1.28154 1 7 -3 0 1.74838 5.18387 2 7 3 0 5.69381 2.68745 3 -7 3 0 3.36170 1.18165 1 -7 3 0 4.50420 1.95785 4 -8 -3 0 33.9710 5.36627 2 -8 -3 0 25.1593 2.50250 1 8 -3 0 22.4402 6.61152 2 8 -3 0 33.3304 3.01251 1 -8 3 0 21.7488 2.43463 1 -8 3 0 29.3404 3.27935 4 8 3 0 24.7551 3.32096 3 -9 -3 0 38.3477 4.96177 1 9 -3 0 48.2191 6.67392 1 9 -3 0 49.0614 6.77471 4 -9 -3 0 44.1559 6.17138 2 9 -3 0 28.7908 7.16727 2 10 -3 0 374.970 22.6262 4 10 -3 0 319.418 23.2659 1 -10 -3 0 309.437 25.9248 2 -11 -3 0 245.463 18.5692 2 11 -3 0 260.303 16.8400 1 11 -3 0 234.962 17.0634 4 -12 -3 0 6.05199 5.51069 2 12 -3 0 8.82663 2.59929 1 12 -3 0 8.25119 4.03971 4 -13 -3 0 13.6581 6.10220 2 13 -3 0 6.92825 4.29381 4 13 -3 0 13.6235 2.72571 1 -14 -3 0 36.0644 7.94536 2 14 -3 0 43.1207 4.58700 1 14 -3 0 41.9019 6.71911 4 -15 -3 0 61.7910 10.1531 2 15 -3 0 65.4942 8.42807 4 15 -3 0 58.5187 5.87635 1 16 -3 0 28.3259 7.21722 4 -16 -3 0 34.2544 7.50538 2 0 -4 0 409.038 25.8341 3 0 -4 0 397.967 30.3897 1 1 -4 0 24.5186 2.03978 1 1 -4 0 21.5516 3.04573 3 -1 -4 0 24.5486 2.77491 3 1 -4 0 29.6798 2.52632 4 2 -4 0 283.968 19.1722 4 -2 -4 0 260.937 17.6825 3 2 -4 0 263.032 18.6151 3 2 -4 0 268.645 18.4130 1 2 4 0 278.272 19.7305 3 -3 -4 0 89.3371 7.43374 4 -3 -4 0 98.3759 7.85224 3 -3 -4 0 89.2109 9.19982 2 3 -4 0 104.303 7.18751 1 3 -4 0 106.838 7.74743 3 3 -4 0 108.301 6.79517 4 3 4 0 85.7349 7.28715 3 -4 -4 0 19.6190 3.13856 4 -4 -4 0 18.7058 5.39551 2 -4 -4 0 14.4089 2.22214 3 4 -4 0 14.5050 2.16076 4 4 -4 0 15.2071 1.75466 1 4 -4 0 14.3328 3.34245 3 -4 -4 0 15.1722 1.79477 1 4 4 0 23.5931 3.14096 3 -5 -4 0 35.1790 5.74582 2 -5 -4 0 23.4893 2.23271 1 5 -4 0 20.4784 2.50094 4 5 -4 0 18.0773 2.03392 1 5 -4 0 17.6755 3.17648 3 -5 -4 0 17.3101 3.98272 4 -5 -4 0 25.0288 2.86122 3 5 4 0 23.0467 3.36758 3 -6 -4 0 136.768 10.3449 3 -6 -4 0 150.016 11.2158 1 6 -4 0 139.602 10.1572 4 6 -4 0 150.712 9.96471 1 -6 -4 0 146.452 12.2809 2 -6 4 0 171.997 10.7190 1 6 4 0 140.954 10.4733 3 -7 -4 0 51.4322 4.54448 1 7 -4 0 45.5609 4.62193 4 -7 -4 0 53.2504 7.16695 2 7 -4 0 49.0662 3.94503 1 -7 4 0 41.6646 3.82912 1 8 -4 0 48.7251 4.42342 1 -8 -4 0 45.9171 3.83353 1 -8 -4 0 36.8827 6.83467 2 8 -4 0 53.1215 5.00992 4 -9 -4 0 45.0726 7.07720 2 9 -4 0 29.5758 3.05629 1 -10 -4 0 83.6021 9.17525 2 10 -4 0 71.0863 5.54320 1 10 -4 0 66.6334 6.55589 4 11 -4 0 22.6938 2.95875 1 11 -4 0 18.1434 4.66771 4 -11 -4 0 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11.5986 2 10 -2 -22 0.98286 5.21035 3 9 -2 -22 47.4801 6.92066 3 -9 -2 22 45.5959 7.23805 4 -9 -2 22 25.9790 11.1353 2 8 -2 -22 36.6461 6.38150 3 -8 -2 22 29.6134 11.2682 2 -8 -2 22 29.3347 6.61402 4 7 -2 -22 65.6035 7.96307 3 -7 -2 22 83.7511 8.55060 4 -6 -2 22 -0.1619 5.14697 4 6 -2 -22 2.56264 4.70534 3 -5 -2 22 3.26364 5.28152 4 5 -2 -22 1.32143 4.75734 3 4 -2 -22 14.4002 5.43795 3 -4 -2 22 22.2271 6.21574 4 3 -2 -22 36.3041 6.16305 3 -3 -2 22 32.2266 7.08935 4 2 -2 -22 57.5337 7.11932 3 -2 -2 22 37.3997 7.58082 4 -1 -2 22 0.16904 6.36282 4 1 -2 -22 1.65217 5.18130 3 10 -3 -22 12.3520 6.76809 3 -10 -3 22 28.1691 12.4096 2 9 -3 -22 30.3277 7.23414 3 -9 -3 22 20.9870 13.8884 2 -8 -3 22 3.66592 6.27970 4 8 -3 -22 5.99674 6.15921 3 7 -3 -22 -2.3911 5.77861 3 -7 -3 22 5.32077 6.25820 4 -6 -3 22 99.4256 10.1560 4 6 -3 -22 85.1879 9.40476 3 5 -3 -22 4.61653 5.87464 3 -5 -3 22 6.78464 4.58214 4 4 -3 -22 7.61385 5.67479 3 -13 0 23 -4.0264 12.0003 2 11 0 -23 -1.1771 6.66954 3 -11 0 23 1.72560 4.51368 4 10 0 -23 13.0034 4.77934 3 -10 0 23 22.5751 5.23727 4 9 0 -23 -0.1661 3.59926 3 -9 0 23 -2.5944 4.12459 4 8 0 -23 39.4622 5.23060 3 -8 0 23 45.6365 6.15148 4 -7 0 23 -3.3731 4.29208 4 7 0 -23 5.39135 3.78760 3 6 0 -23 73.3415 6.77761 3 -6 0 23 51.8574 7.85140 4 -5 0 23 1.92162 4.69045 4 5 0 -23 0.57112 3.60542 3 -4 0 23 10.7943 5.32824 4 4 0 -23 3.26541 4.06647 3 -3 0 23 -1.0690 5.35984 4 3 0 -23 3.21849 4.33004 3 -2 0 23 -0.8952 5.62739 4 2 0 -23 -2.1834 4.70635 3 12 -1 -23 24.1999 6.95500 3 -12 -1 23 17.8779 14.8844 2 -11 -1 23 4.16273 14.0082 2 11 -1 -23 8.11158 5.13704 3 -11 1 23 1.62954 5.93040 4 -10 -1 23 -3.9312 8.77396 2 10 -1 -23 4.56834 4.70246 3 -10 -1 23 2.43294 5.23587 4 -10 1 23 -2.9613 3.70851 4 -9 -1 23 1.93964 11.9148 2 -9 -1 23 -1.7091 5.07715 4 9 -1 -23 -1.4212 4.28961 3 -9 1 23 -0.5447 3.79446 4 -8 -1 23 1.64392 4.82222 4 8 -1 -23 -2.7787 4.30440 3 -8 1 23 4.08252 3.84812 4 7 -1 -23 10.5191 4.62633 3 -7 -1 23 2.01084 4.88735 4 -7 1 23 0.44065 4.04042 4 6 -1 -23 3.28616 4.41352 3 -6 -1 23 1.15037 4.95734 4 -6 1 23 1.24831 3.94477 4 -5 -1 23 1.24548 5.12462 4 5 -1 -23 -1.7842 4.25907 3 -5 1 23 3.20342 4.19548 4 -4 -1 23 34.7186 6.61975 4 4 -1 -23 23.8945 5.48286 3 -4 1 23 38.3333 6.72894 4 -3 -1 23 0.22261 5.86107 4 3 -1 -23 4.76189 4.59060 3 -3 1 23 0.18394 4.98842 4 -2 -1 23 34.3692 7.11515 4 2 -1 -23 16.2159 5.63333 3 -2 1 23 20.6471 5.97033 4 -11 -2 23 0.27836 9.65492 2 11 -2 -23 5.54974 6.16144 3 -10 -2 23 -1.0623 13.0133 2 10 -2 -23 -4.3962 5.47651 3 -10 -2 23 -2.5504 5.87000 4 -9 -2 23 3.29129 5.85954 4 9 -2 -23 12.8010 5.84663 3 -8 -2 23 10.2906 6.06094 4 8 -2 -23 3.90701 5.42254 3 7 -2 -23 20.0587 5.74709 3 -6 -2 23 1.88507 5.60476 4 6 -2 -23 0.17774 5.25277 3 5 -2 -23 3.62969 5.29171 3 -5 -2 23 4.14518 5.80774 4 -4 -2 23 2.25782 6.16187 4 4 -2 -23 0.72540 5.34300 3 -10 0 24 4.38067 4.82644 4 -9 0 24 -5.9380 4.96435 4 -8 0 24 8.75892 5.10412 4 -7 0 24 -1.1775 4.83995 4 7 0 -24 0.64760 5.04369 3 -6 0 24 47.8488 7.15060 4 6 0 -24 48.6609 5.92767 3 5 0 -24 -0.3298 3.92678 3 -5 0 24 -0.7212 5.32305 4 -10 -1 24 15.6368 10.7360 2 9 -1 -24 33.2109 5.75214 3 -9 -1 24 21.3345 6.17106 4 8 -1 -24 3.24133 4.67266 3 -8 -1 24 2.38467 5.44542 4 7 -1 -24 -1.7942 4.63280 3 -7 -1 24 0.18356 5.42588 4 -7 1 24 -2.6950 7.19684 4 6 -1 -24 51.0140 6.86735 3 -6 -1 24 47.8981 7.50564 4 -6 1 24 52.9182 6.75853 4 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6738 _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 0.71058 14.813 5.700 18.458 90.052 113.480 89.910 ) ; _shelx_hkl_checksum 94275 _shelx_res_file ; TITL p21c_a.res in P2(1)/c fo7441.res created by SHELXL-2018/3 at 11:50:24 on 23-Jun-2021 CELL 0.71073 18.4574 5.7020 14.8058 90.000 113.468 90.000 ZERR 4.000 0.0008 0.0002 0.0006 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 60 84 4 12 ACTA L.S. 10 BOND $H SHEL 9999.0 0.77 FMAP 2 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C2 O1_$1 EQIV $2 x, y+1, z EQIV $3 x, -y+3/2, z+1/2 HTAB C5 O3_$3 HTAB C9 O2_$2 REM MPLA 8 C1 O1 C10 > C15 MPLA 4 N1 C3 O3 O2 PLAN 20 TEMP -140 SIZE 0.102 0.098 0.084 REM COLOR:colourless WGHT 0.026600 0.814800 EXTI 0.009331 FVAR 0.80966 O1 4 0.386054 0.794907 0.388258 11.00000 0.03164 0.03107 = 0.03863 -0.00760 0.01399 0.00497 O2 4 0.279356 0.458098 0.326097 11.00000 0.02043 0.03691 = 0.02602 0.00687 0.00868 0.00106 O3 4 0.242280 0.620212 0.174579 11.00000 0.02609 0.03752 = 0.02287 0.00315 0.01081 0.00093 N1 3 0.170539 0.683649 0.267093 11.00000 0.02005 0.04328 = 0.02189 0.00366 0.00807 0.00182 C1 1 0.410052 0.613684 0.366872 11.00000 0.02477 0.02687 = 0.01821 0.00141 0.00803 0.00411 C2 1 0.354483 0.407913 0.324883 11.00000 0.02270 0.02784 = 0.02635 0.00209 0.00949 0.00225 AFIX 23 H2A 2 0.348514 0.377390 0.256450 11.00000 -1.20000 H2B 2 0.376866 0.265560 0.364461 11.00000 -1.20000 AFIX 0 C3 1 0.231363 0.594545 0.249649 11.00000 0.01994 0.03104 = 0.02112 0.00070 0.00547 -0.00381 C4 1 0.167619 0.674685 0.365339 11.00000 0.02567 0.06268 = 0.02510 0.00437 0.01245 0.00335 AFIX 13 H4 2 0.211633 0.570586 0.407718 11.00000 -1.20000 AFIX 0 C5 1 0.181518 0.915455 0.413315 11.00000 0.06108 0.09090 = 0.03254 -0.02245 0.02171 -0.03774 AFIX 137 H5A 2 0.228794 0.985787 0.409862 11.00000 -1.50000 H5B 2 0.188987 0.899895 0.482386 11.00000 -1.50000 H5C 2 0.135734 1.015930 0.378631 11.00000 -1.50000 AFIX 0 C6 1 0.090723 0.566550 0.360260 11.00000 0.04869 0.05122 = 0.04747 0.00032 0.03143 -0.00612 AFIX 137 H6A 2 0.046572 0.670305 0.322993 11.00000 -1.50000 H6B 2 0.093071 0.545940 0.427083 11.00000 -1.50000 H6C 2 0.083000 0.413759 0.327431 11.00000 -1.50000 AFIX 0 C7 1 0.110690 0.827084 0.190387 11.00000 0.02183 0.03171 = 0.02693 -0.00078 0.00646 0.00257 AFIX 13 H7 2 0.074178 0.887235 0.220031 11.00000 -1.20000 AFIX 0 C8 1 0.060553 0.678021 0.102397 11.00000 0.02513 0.03523 = 0.02894 -0.00186 0.00412 -0.00056 AFIX 137 H8A 2 0.019602 0.775918 0.054376 11.00000 -1.50000 H8B 2 0.035643 0.551161 0.124422 11.00000 -1.50000 H8C 2 0.094128 0.610990 0.071729 11.00000 -1.50000 AFIX 0 C9 1 0.144961 1.041256 0.160959 11.00000 0.04180 0.03267 = 0.04166 0.00022 0.01082 -0.00352 AFIX 137 H9A 2 0.176297 0.991762 0.124230 11.00000 -1.50000 H9B 2 0.178789 1.126741 0.220191 11.00000 -1.50000 H9C 2 0.101940 1.143637 0.119443 11.00000 -1.50000 AFIX 0 C10 1 0.493700 0.586150 0.378100 11.00000 0.02265 0.03353 = 0.01735 0.00347 0.00692 0.00358 C11 1 0.519830 0.386293 0.346075 11.00000 0.02778 0.04041 = 0.02565 0.00013 0.01007 0.00659 AFIX 43 H11 2 0.484354 0.260546 0.317232 11.00000 -1.20000 AFIX 0 C12 1 0.597812 0.370992 0.356344 11.00000 0.03226 0.06724 = 0.02764 0.00471 0.01328 0.02007 AFIX 43 H12 2 0.615586 0.234665 0.334388 11.00000 -1.20000 AFIX 0 C13 1 0.649247 0.551857 0.398044 11.00000 0.02091 0.09229 = 0.03107 0.01593 0.01114 0.00912 AFIX 43 H13 2 0.702529 0.540331 0.404875 11.00000 -1.20000 AFIX 0 C14 1 0.623893 0.751192 0.430240 11.00000 0.02649 0.06659 = 0.03183 0.00675 0.00510 -0.01229 AFIX 43 H14 2 0.659736 0.876252 0.458872 11.00000 -1.20000 AFIX 0 C15 1 0.546368 0.768618 0.420784 11.00000 0.02885 0.04043 = 0.02520 0.00032 0.00684 -0.00381 AFIX 43 H15 2 0.529143 0.904967 0.443406 11.00000 -1.20000 AFIX 0 HKLF 4 1 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.000 REM p21c_a.res in P2(1)/c REM wR2 = 0.1131, GooF = S = 1.041, Restrained GooF = 1.041 for all data REM R1 = 0.0494 for 2464 Fo > 4sig(Fo) and 0.0718 for all 3280 data REM 177 parameters refined using 0 restraints END WGHT 0.0266 0.8128 REM Highest difference peak 0.267, deepest hole -0.206, 1-sigma level 0.041 Q1 1 0.3810 0.5217 0.3365 11.00000 0.05 0.27 Q2 1 0.4601 0.5736 0.3870 11.00000 0.05 0.23 Q3 1 0.5099 0.6757 0.3902 11.00000 0.05 0.20 Q4 1 0.2406 0.8880 0.4254 11.00000 0.05 0.20 Q5 1 0.6192 0.4647 0.3890 11.00000 0.05 0.18 Q6 1 0.1376 0.6044 0.3858 11.00000 0.05 0.18 Q7 1 0.5632 0.3395 0.3676 11.00000 0.05 0.17 Q8 1 0.6098 0.1292 0.3369 11.00000 0.05 0.16 Q9 1 0.4707 0.1414 0.3499 11.00000 0.05 0.16 Q10 1 0.0830 0.7916 0.1364 11.00000 0.05 0.16 Q11 1 0.1882 0.7854 0.3915 11.00000 0.05 0.16 Q12 1 0.5059 0.4742 0.3908 11.00000 0.05 0.15 Q13 1 0.1436 0.7440 0.2251 11.00000 0.05 0.15 Q14 1 0.1788 1.0383 0.4828 11.00000 0.05 0.15 Q15 1 0.1958 0.7154 0.1336 11.00000 0.05 0.15 Q16 1 0.3011 0.5961 0.3566 11.00000 0.05 0.14 Q17 1 0.5213 1.0120 0.3960 11.00000 0.05 0.14 Q18 1 0.3684 0.2475 0.3123 11.00000 0.05 0.14 Q19 1 0.1653 0.6836 0.3222 11.00000 0.05 0.13 Q20 1 0.6375 0.6839 0.3958 11.00000 0.05 0.13 ; _shelx_res_checksum 41830 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.38605(6) 0.7949(2) 0.38826(9) 0.0338(3) Uani d 1 . . O O2 0.27936(6) 0.4581(2) 0.32610(8) 0.0280(3) Uani d 1 . . O O3 0.24228(6) 0.6202(2) 0.17458(8) 0.0285(3) Uani d 1 . . N N1 0.17054(7) 0.6836(3) 0.26709(9) 0.0285(3) Uani d 1 . . C C1 0.41005(8) 0.6137(3) 0.36687(11) 0.0234(3) Uani d 1 . . C C2 0.35448(8) 0.4079(3) 0.32488(12) 0.0257(3) Uani d 1 . . H H2A 0.348514 0.377390 0.256450 0.031 Uiso calc 1 . . H H2B 0.376866 0.265560 0.364461 0.031 Uiso calc 1 . . C C3 0.23136(8) 0.5945(3) 0.24965(11) 0.0249(3) Uani d 1 . . C C4 0.16762(9) 0.6747(4) 0.36534(12) 0.0371(4) Uani d 1 . . H H4 0.211633 0.570586 0.407718 0.044 Uiso calc 1 . . C C5 0.18152(13) 0.9155(5) 0.41331(15) 0.0605(7) Uani d 1 . . H H5A 0.228794 0.985787 0.409862 0.091 Uiso calc 1 . . H H5B 0.188987 0.899895 0.482386 0.091 Uiso calc 1 . . H H5C 0.135734 1.015930 0.378631 0.091 Uiso calc 1 . . C C6 0.09072(11) 0.5665(4) 0.36026(15) 0.0452(5) Uani d 1 . . H H6A 0.046572 0.670305 0.322993 0.068 Uiso calc 1 . . H H6B 0.093071 0.545940 0.427083 0.068 Uiso calc 1 . . H H6C 0.083000 0.413759 0.327431 0.068 Uiso calc 1 . . C C7 0.11069(9) 0.8271(3) 0.19039(11) 0.0278(4) Uani d 1 . . H H7 0.074178 0.887235 0.220031 0.033 Uiso calc 1 . . C C8 0.06055(9) 0.6780(3) 0.10240(12) 0.0319(4) Uani d 1 . . H H8A 0.019602 0.775918 0.054376 0.048 Uiso calc 1 . . H H8B 0.035643 0.551161 0.124422 0.048 Uiso calc 1 . . H H8C 0.094128 0.610990 0.071729 0.048 Uiso calc 1 . . C C9 0.14496(11) 1.0413(3) 0.16096(14) 0.0405(5) Uani d 1 . . H H9A 0.176297 0.991762 0.124230 0.061 Uiso calc 1 . . H H9B 0.178789 1.126741 0.220191 0.061 Uiso calc 1 . . H H9C 0.101940 1.143637 0.119443 0.061 Uiso calc 1 . . C C10 0.49370(8) 0.5861(3) 0.37810(11) 0.0248(3) Uani d 1 . . C C11 0.51983(9) 0.3863(3) 0.34607(12) 0.0315(4) Uani d 1 . . H H11 0.484354 0.260546 0.317232 0.038 Uiso calc 1 . . C C12 0.59781(10) 0.3710(4) 0.35634(13) 0.0420(5) Uani d 1 . . H H12 0.615586 0.234665 0.334388 0.050 Uiso calc 1 . . C C13 0.64925(10) 0.5519(4) 0.39804(13) 0.0478(6) Uani d 1 . . H H13 0.702529 0.540331 0.404875 0.057 Uiso calc 1 . . C C14 0.62389(10) 0.7512(4) 0.43024(13) 0.0437(5) Uani d 1 . . H H14 0.659736 0.876252 0.458872 0.052 Uiso calc 1 . . C C15 0.54637(9) 0.7686(3) 0.42078(12) 0.0327(4) Uani d 1 . . H H15 0.529143 0.904967 0.443406 0.039 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0316(6) 0.0311(6) 0.0386(7) 0.0050(5) 0.0140(5) -0.0076(5) O2 0.0204(5) 0.0369(6) 0.0260(6) 0.0011(5) 0.0087(4) 0.0069(5) O3 0.0261(5) 0.0375(7) 0.0229(6) 0.0009(5) 0.0108(4) 0.0031(5) N1 0.0201(6) 0.0433(8) 0.0219(7) 0.0018(6) 0.0081(5) 0.0037(6) C1 0.0248(7) 0.0269(8) 0.0182(7) 0.0041(6) 0.0080(6) 0.0014(6) C2 0.0227(7) 0.0278(8) 0.0264(8) 0.0023(6) 0.0095(6) 0.0021(6) C3 0.0199(7) 0.0310(8) 0.0211(7) -0.0038(6) 0.0055(6) 0.0007(6) C4 0.0257(8) 0.0627(13) 0.0251(8) 0.0034(8) 0.0125(7) 0.0044(8) C5 0.0611(13) 0.0909(18) 0.0325(10) -0.0377(13) 0.0217(10) -0.0224(11) C6 0.0487(11) 0.0512(12) 0.0475(11) -0.0061(9) 0.0314(9) 0.0003(9) C7 0.0218(7) 0.0317(9) 0.0269(8) 0.0026(6) 0.0065(6) -0.0008(7) C8 0.0251(7) 0.0352(9) 0.0289(8) -0.0006(7) 0.0041(7) -0.0019(7) C9 0.0418(10) 0.0327(10) 0.0417(10) -0.0035(8) 0.0108(8) 0.0002(8) C10 0.0227(7) 0.0335(9) 0.0174(7) 0.0036(6) 0.0069(6) 0.0035(6) C11 0.0278(8) 0.0404(10) 0.0257(8) 0.0066(7) 0.0101(7) 0.0001(7) C12 0.0323(9) 0.0672(13) 0.0276(9) 0.0201(9) 0.0133(7) 0.0047(9) C13 0.0209(8) 0.0923(17) 0.0311(10) 0.0091(10) 0.0111(7) 0.0159(10) C14 0.0265(8) 0.0666(14) 0.0318(10) -0.0123(9) 0.0051(7) 0.0068(9) C15 0.0288(8) 0.0404(10) 0.0252(8) -0.0038(7) 0.0068(7) 0.0003(7) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 O2 C2 . . 114.64(12) ? C3 N1 C7 . . 119.12(13) ? C3 N1 C4 . . 122.37(13) ? C7 N1 C4 . . 117.83(13) ? O1 C1 C10 . . 121.89(14) ? O1 C1 C2 . . 120.45(14) ? C10 C1 C2 . . 117.64(13) ? O2 C2 C1 . . 110.00(13) ? O2 C2 H2A . . 109.7 ? C1 C2 H2A . . 109.7 ? O2 C2 H2B . . 109.7 ? C1 C2 H2B . . 109.7 ? H2A C2 H2B . . 108.2 ? O3 C3 N1 . . 125.75(14) ? O3 C3 O2 . . 122.46(14) ? N1 C3 O2 . . 111.72(13) ? N1 C4 C5 . . 111.30(16) ? N1 C4 C6 . . 111.37(14) ? C5 C4 C6 . . 111.69(16) ? N1 C4 H4 . . 107.4 ? C5 C4 H4 . . 107.4 ? C6 C4 H4 . . 107.4 ? C4 C5 H5A . . 109.5 ? C4 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? C4 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? C4 C6 H6A . . 109.5 ? C4 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C4 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? N1 C7 C9 . . 113.40(13) ? N1 C7 C8 . . 111.27(13) ? C9 C7 C8 . . 112.63(14) ? N1 C7 H7 . . 106.3 ? C9 C7 H7 . . 106.3 ? C8 C7 H7 . . 106.3 ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C7 C9 H9A . . 109.5 ? C7 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C7 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C15 C10 C11 . . 119.50(15) ? C15 C10 C1 . . 118.42(15) ? C11 C10 C1 . . 122.07(14) ? C12 C11 C10 . . 119.92(17) ? C12 C11 H11 . . 120.0 ? C10 C11 H11 . . 120.0 ? C13 C12 C11 . . 120.25(18) ? C13 C12 H12 . . 119.9 ? C11 C12 H12 . . 119.9 ? C12 C13 C14 . . 120.29(16) ? C12 C13 H13 . . 119.9 ? C14 C13 H13 . . 119.9 ? C13 C14 C15 . . 120.11(18) ? C13 C14 H14 . . 119.9 ? C15 C14 H14 . . 119.9 ? C14 C15 C10 . . 119.93(18) ? C14 C15 H15 . . 120.0 ? C10 C15 H15 . . 120.0 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 . 1.2149(19) ? O2 C3 . 1.3684(18) ? O2 C2 . 1.4230(17) ? O3 C3 . 1.2148(18) ? N1 C3 . 1.348(2) ? N1 C7 . 1.4764(19) ? N1 C4 . 1.478(2) ? C1 C10 . 1.494(2) ? C1 C2 . 1.519(2) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C4 C5 . 1.520(3) ? C4 C6 . 1.522(2) ? C4 H4 . 1.0000 ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C7 C9 . 1.517(2) ? C7 C8 . 1.522(2) ? C7 H7 . 1.0000 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? C10 C15 . 1.392(2) ? C10 C11 . 1.392(2) ? C11 C12 . 1.389(2) ? C11 H11 . 0.9500 ? C12 C13 . 1.371(3) ? C12 H12 . 0.9500 ? C13 C14 . 1.384(3) ? C13 H13 . 0.9500 ? C14 C15 . 1.385(2) ? C14 H14 . 0.9500 ? C15 H15 . 0.9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C2 H2B O1 1_545 0.99 2.70 3.605(2) 151.7 yes C5 H5B O3 4_576 0.98 2.62 3.578(2) 167.3 yes C9 H9B O2 1_565 0.98 2.68 3.599(2) 157.3 yes _cod_database_fobs_code 2243868