#------------------------------------------------------------------------------ #$Date: 2022-11-08 19:24:16 +0000 (Tue, 08 Nov 2022) $ #$Revision: 279109 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244210.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_2244210 loop_ _publ_author_name 'El Mestehdi, Aly Dawa' 'Abba, Moctar' 'El Housseine, Mohamed Lemine' 'Ould Hadou, Abderrahmane' 'Barry, Aliou Hamady' 'Ould Elemine, Brahim' 'Jelsch, Christian' 'Gaye, Mohamed' _publ_section_title ; Synthesis, crystal structure and Hirshfeld surface analysis of tert-butyl N-acetylcarbamate ; _journal_coeditor_code ZV2015 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1072 _journal_page_last 1076 _journal_paper_doi 10.1107/S2056989022009483 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C7 H13 N O3' _chemical_formula_moiety 'C7 H13 N O3' _chemical_formula_sum 'C7 H13 N O3' _chemical_formula_weight 159.18 _chemical_name_systematic ; tert-Butyl N-acetylcarbamate ; _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXL and MoPro-v21' _cell_angle_alpha 90.00 _cell_angle_beta 98.771(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.0404(6) _cell_length_b 8.6114(7) _cell_length_c 17.6110(17) _cell_measurement_reflns_used 4200 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.6423 _cell_measurement_theta_min 2.4120 _cell_volume 905.35(15) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; MoPro (Jelsch et al., 2005) ; _computing_publication_material ; MoPro (Jelsch et al., 2005) ; _computing_structure_refinement ; MoPro (Jelsch et al., 2005) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker Kappa CCD' _diffrn_measurement_method CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.02642 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2405 _diffrn_reflns_theta_full 27.51 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 2.64 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 344 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.16 _refine_diff_density_min -0.17 _refine_ls_extinction_coef 0.51132 _refine_ls_extinction_method 'Isotropic Gaussian' _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 139 _refine_ls_number_reflns 2059 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 10.437 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0338 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w =1/[4.4*\s^2^(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0716 _reflns_number_gt 1627 _reflns_number_total 2059 _reflns_threshold_expression 'I > 2 \s(I)' _iucr_refine_instructions_details ; ! MoPro v22 28/04/2022 18:20:23 ! molecular file: C:\Users\Christian\Desktop\barry_revision1\new_refi_mopro_trf #_cutoff\exp_191_29.par ! reflections hkl file : C:\Users\Christian\Desktop\barry_revision1\new_refi_mo #pro_trf_cutoff\OBS_NOEXTINCT.hkl refin. vs. F^2 ! atomic table file : D:\MoProSuite\LibMoPro\mopro_v20.tab ! wave functions file : D:\MoProSuite\LibMoPro\WAVEF ! anomalous scattering file : D:\MoProSuite\LibMoPro\asf_Kissel.dat ! Constraints file : C:\Users\Christian\Desktop\barry_revision1\new_refi_mopro_ #trf_cutoff\CONSTRAIN.txt ! Restraints file : C:\Users\Christian\Desktop\barry_revision1\new_refi_mopro_t #rf_cutoff\RESTRAIN.txt ! RF factor = 4.607 % RI factor = 4.361% ! wR2F factor = 3.685 % wR2I factor = 7.158% ! g.o.f.(F**2) = 1.000 Nvar= 139 Nref= 2059 Nfree= 0 0.06CH2 1.092 Z2>CH2 1.091 ! ->CH 1.099 >CHarom 1.083 ! C=CNH2+ ->NH+ 1.033 ! Distance target = 1.015 -NH2 >NH ! reference: Allen FH & Bruno IJ, ! Acta Crystallographic (2010). B66, 380--386 FIXUIJ H1 1 0.098719 0.083440 0.091802 0.027409 0.050873 0.038853 FIXUIJ H7A 1 0.098867 0.104116 0.117966 0.041001 0.040008 0.023948 FIXUIJ H7B 1 0.088218 0.094678 0.160180 -0.000282 0.052289 0.032754 FIXUIJ H7C 1 0.144228 0.136211 0.069529 0.049034 0.031932 0.005902 ! Weighted R-value of the TLS fit to the Uijs is = 0.037; FIXUIJ H4A 1 0.127756 0.133815 0.062631 0.002850 0.007473 0.003544 FIXUIJ H4B 1 0.119327 0.112723 0.101738 0.012871 -0.029730 0.037071 FIXUIJ H4C 1 0.098931 0.116738 0.115377 -0.034896 -0.019844 0.002691 FIXUIJ H3A 1 0.114673 0.095112 0.123959 -0.016590 -0.037796 -0.007239 FIXUIJ H3B 1 0.117018 0.056112 0.179400 -0.003319 -0.010312 0.028186 FIXUIJ H3C 1 0.087551 0.094298 0.143615 -0.015227 0.024328 0.028421 FIXUIJ H2A 1 0.097346 0.113231 0.151598 0.015619 0.053422 0.020032 FIXUIJ H2B 1 0.125612 0.094162 0.151815 0.053404 0.024951 0.019641 FIXUIJ H2C 1 0.153924 0.132175 0.088978 0.049223 0.019500 -0.017999 ! Weighted R-value of the TLS fit to the Uijs is = 0.023; ######################################### ; _cod_data_source_file zv2015sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2244210 _shelx_hkl_file ; 0 0 4 9391.68 325.1631 0 1 1 0.025000 0.0437 0 1 2 3691.59 111.9937 0 1 3 4648.24 115.2258 0 1 4 81.0325 2.1682 0 2 0 4354.60 83.5641 0 2 1 0.276000 0.0874 0 2 2 267.045 3.9304 0 2 3 970.022 18.7278 -1 0 3 3334.17 82.5207 -1 0 1 2688.90 115.4200 1 0 1 2862.84 71.0735 1 0 3 22.0180 0.6296 -1 1 4 15.8660 0.5162 -1 1 3 55.5567 1.1726 -1 1 2 5418.78 116.6350 -1 1 1 1537.44 33.0061 1 1 0 466.192 11.6264 1 1 1 819.005 15.8373 1 1 2 9580.20 165.3091 1 1 3 3821.18 58.0556 -1 2 1 129.078 2.5834 1 2 0 1.8740 0.2076 0 0 6 1206.90 36.7766 0 1 5 10.9633 0.4591 0 1 6 116.018 4.1367 0 2 4 25.0614 0.6773 0 2 5 59.6243 1.7125 0 3 1 621.903 8.2182 0 3 2 575.252 8.8813 -1 0 5 1220.76 52.8350 1 0 5 376.165 9.0312 -1 1 5 52.0440 1.2773 1 1 4 6253.20 84.7310 -1 2 4 301.769 9.2011 -1 2 3 116.538 2.4059 -1 2 2 381.364 6.2967 1 2 1 4545.10 159.8255 1 2 2 83.5983 1.7520 1 2 3 3400.46 69.0945 -2 0 2 736.284 14.2460 2 0 0 76.8800 1.6830 -2 1 2 36.9736 0.9255 -2 1 1 3.6130 0.1843 2 1 0 188.208 2.6341 2 1 1 1406.21 22.8475 0 1 7 2.1662 0.1654 0 2 6 435.028 9.5491 0 3 3 720.812 10.4577 0 3 4 4.2911 0.2230 -1 0 7 2239.00 96.6900 -1 1 6 1492.42 37.3820 1 1 5 4.0200 0.1770 1 1 6 313.633 5.0490 -1 2 5 47.0843 1.1344 1 2 4 537.114 8.2501 1 2 5 775.058 11.8783 -1 3 3 11.4430 0.3095 -1 3 2 1588.08 22.9057 -1 3 1 1261.32 28.4067 1 3 0 566.828 9.3188 1 3 1 71.5957 1.4273 1 3 2 327.436 5.7939 -2 0 4 1912.12 43.1443 2 0 2 37.3150 2.7102 -2 1 5 81.0770 1.3027 -2 1 4 570.257 8.2682 -2 1 3 1906.73 30.7945 2 1 2 831.869 12.7331 2 1 3 0.764400 0.1253 -2 2 3 830.177 12.0405 -2 2 2 83.0150 1.6672 -2 2 1 1950.82 29.7194 2 2 0 2385.58 36.3785 2 2 1 5.9311 0.3562 0 0 8 32.1400 1.2735 0 2 7 336.725 6.6688 0 3 5 184.399 3.1750 0 4 0 7.1783 0.3811 1 0 7 2633.62 56.6560 -1 1 7 89.0950 2.6721 -1 2 6 527.063 9.4389 -1 3 5 0.328600 0.1690 -1 3 4 146.754 2.2630 1 3 3 63.1475 1.2180 1 3 4 992.586 17.6096 -2 0 6 2765.70 68.7249 2 0 4 1896.23 36.3131 -2 1 6 679.905 11.2422 2 1 4 296.405 4.3953 -2 2 4 344.945 5.0813 2 2 2 675.704 10.5377 2 2 3 21.7857 0.6828 0 1 8 663.701 10.9534 0 3 6 9.5433 0.4414 0 4 1 732.558 9.6163 0 4 2 721.727 9.9553 0 4 3 443.699 6.9572 -1 1 8 208.924 4.7564 1 1 7 89.0900 2.2571 -1 2 7 0.366000 0.2233 1 2 6 1311.52 23.1914 -1 3 6 2.1044 0.2761 1 3 5 2783.00 48.9245 -1 4 2 511.157 6.7860 -1 4 1 594.558 7.8430 1 4 0 1.6758 0.1883 1 4 1 598.011 8.7610 -2 1 7 126.589 2.4464 2 1 5 60.7291 1.0620 -2 2 6 82.1089 1.4453 -2 2 5 1257.23 19.2079 2 2 4 619.237 8.5510 -2 3 3 19.8062 0.5258 -2 3 2 58.2537 2.0694 -2 3 1 74.9163 1.4184 2 3 0 1086.58 16.6496 2 3 1 138.003 2.5484 -3 0 1 282.837 7.6620 0 1 9 491.052 8.4660 0 2 8 85.6717 1.8764 0 3 7 210.196 4.9989 0 4 4 20.2944 0.5423 -1 0 9 55.2775 1.6335 -1 1 9 1211.15 21.4296 1 1 8 1245.57 20.3874 -1 2 8 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17.0400 2.5300 -5 2 20 2.6500 1.3316 5 8 6 1.0800 1.2300 -6 1 18 0.953300 1.0859 6 6 7 0.800000 1.7300 7 4 5 1.6900 1.6600 0 5 21 0.260000 1.4185 0 11 7 0.450000 1.6279 -1 8 17 2.4550 1.7252 1 11 6 1.3533 1.0546 -2 10 11 1.3150 1.5656 2 11 3 10.4550 1.9902 3 7 15 1.5050 1.3574 3 8 13 4.0700 1.7600 -3 10 9 2.1400 1.4314 4 2 18 0.310000 1.5600 -4 6 18 1.6500 1.8600 4 9 7 3.6700 1.4800 -4 10 3 3.3000 1.2400 -4 10 2 1.2800 1.1600 5 1 16 2.1033 0.9769 5 3 15 2.1000 1.7100 5 9 0 2.8300 1.5900 -6 3 17 1.6700 1.2200 -6 4 16 1.0050 1.3252 6 7 4 4.1400 1.8300 -7 2 14 5.4700 1.3133 -7 5 9 1.0550 1.6352 0 2 23 8.8250 1.9150 0 6 20 0.785000 1.3905 1 9 14 2.7550 1.6494 1 10 11 0.840000 1.8800 -1 11 7 2.6350 1.5785 -2 4 22 4.8200 1.6400 -2 11 5 1.0300 1.4100 -4 1 22 1.7300 1.4200 4 10 0 5.0300 1.6600 -5 6 16 1.2500 1.8800 -5 8 11 0.980000 1.0500 7 2 8 5.9800 1.3700 7 3 7 1.3800 1.3600 7 5 3 0.810000 1.7371 0 4 22 0.355000 1.4554 0 8 17 24.6667 1.7612 1 3 22 2.5300 1.4400 1 7 18 1.6400 1.0800 -1 9 15 12.0000 2.2000 -1 10 12 1.0550 1.6059 2 3 21 0.210000 1.2100 2 11 4 3.7100 1.4800 -3 1 23 2.1300 1.5600 3 5 18 12.4200 2.5400 4 5 16 0.340000 1.5600 4 7 13 0.705000 1.2849 -4 10 5 4.8100 1.4200 4 10 1 0.550000 1.4800 5 9 1 21.0200 2.4200 6 1 13 4.2833 0.9892 6 3 12 0.570000 1.1600 -7 0 15 1.2000 1.5500 -7 4 12 1.1050 1.7254 -8 2 5 0.480000 1.2000 -8 2 3 1.4200 1.2800 0 10 12 4.9500 1.4766 -1 3 23 2.5500 1.5300 -1 7 19 4.1150 1.4433 2 7 17 0.340000 1.0300 -2 11 6 0.910000 1.5000 -5 4 19 8.3500 2.0600 5 8 7 1.7200 1.2800 -6 5 15 1.8500 1.6224 -6 6 13 1.8750 1.7954 -7 1 15 2.9633 1.3149 7 4 6 0.280000 1.5900 -7 6 4 1.7800 1.6600 -7 6 3 0.580000 1.5600 -7 6 2 2.5900 1.6000 0 9 15 13.6233 1.4212 0 11 8 0.840000 1.8100 1 0 23 3.5600 1.7900 1 11 7 0.965000 1.6112 -2 3 23 0.570000 1.5900 2 9 13 0.380000 1.6300 3 6 17 1.0900 1.6700 3 9 11 0.965000 1.4456 -4 2 22 3.4500 1.5700 4 8 11 0.980000 1.2700 4 10 2 2.1500 1.4400 5 2 16 0.290000 1.5700 -5 5 18 1.6100 2.0100 5 6 12 4.1900 1.5500 7 1 9 1.7100 1.1000 -7 5 10 1.3200 1.8100 -7 6 5 0.300000 1.5400 -7 6 1 0.860000 1.5100 0 7 19 10.4433 1.3329 1 1 23 0.715000 1.6877 -1 11 8 0.640000 1.0185 2 10 10 0.675000 1.5847 2 11 5 6.4600 1.8213 -3 2 23 1.7600 1.7000 4 3 18 1.3600 1.6700 4 6 15 2.0200 1.6600 4 9 8 3.4300 1.4900 -5 0 21 1.0400 1.2300 -5 3 20 4.8300 2.0400 6 2 13 0.935000 1.1763 6 5 10 1.6200 1.4000 6 6 8 2.0500 1.7900 -7 3 14 0.950000 1.6400 7 5 4 1.0300 1.6800 -7 6 6 1.5600 1.7300 0 3 23 0.290000 1.4500 -2 10 12 6.1800 2.0200 -2 11 7 4.0500 1.6600 -5 8 12 0.340000 1.0500 -7 2 15 1.5550 1.8093 7 6 0 1.1400 1.5800 1 5 21 3.0800 1.3400 -2 0 24 1.4700 1.8300 -3 11 2 5.8900 1.5700 -3 11 1 5.0700 1.6200 -4 10 7 1.8700 1.2600 5 4 15 1.2900 1.7100 -6 1 19 7.9500 4.3000 -6 4 17 3.6100 1.7200 6 8 0 0.230000 1.2600 7 2 9 0.880000 1.1498 7 3 8 1.9700 1.4800 -8 3 5 0.550000 1.5000 -8 3 4 0.270000 1.4500 -8 3 3 2.1700 1.4800 1 8 17 3.6500 1.5900 1 10 12 4.6500 1.5000 1 11 8 25.4750 2.9458 2 5 20 1.4400 1.0700 3 8 14 2.2700 1.5363 -3 11 3 3.0600 1.5000 3 11 0 1.8200 1.3500 -5 6 17 0.420000 1.9600 -5 7 15 1.2100 1.2600 -6 3 18 1.2400 1.4871 7 6 1 0.290000 1.5500 -8 3 2 0.270000 1.5000 0 0 24 5.8900 2.1200 1 2 23 6.8600 1.8600 1 4 22 0.270000 1.5700 -1 5 22 0.460000 1.3200 -1 6 21 0.620000 1.3600 -1 8 18 2.5400 1.5500 -1 10 13 10.4250 4.0250 -1 11 9 0.295000 1.5347 2 6 19 2.3600 1.1600 2 11 6 0.250000 1.5100 3 7 16 1.0500 1.3717 3 11 1 0.900000 1.3600 5 3 16 0.320000 1.7300 5 9 4 2.9500 1.4900 6 0 14 1.1500 0.9800 -6 6 14 8.4450 2.1988 -7 1 16 2.5167 1.3368 -8 3 1 4.9600 1.6200 0 1 24 0.350000 1.9000 -1 9 16 6.7900 2.0200 -2 11 8 1.9100 1.5500 3 11 2 10.4800 1.8400 4 9 9 7.5500 1.8600 6 1 14 0.585000 1.2947 -6 5 16 1.6350 1.7349 -8 3 7 1.1500 1.5300 -1 4 23 2.6700 1.5500 2 10 11 9.4100 2.4800 3 9 12 0.360000 1.5800 4 7 14 3.3300 1.7500 4 8 12 1.6800 1.2000 -5 8 13 0.550000 1.1400 -5 9 9 4.5400 1.3300 -6 2 19 3.8800 1.3600 6 6 9 1.2300 1.6700 7 1 10 1.0800 1.2200 0 5 22 1.5700 1.8900 0 6 21 1.8500 1.6400 0 8 18 8.9000 1.9000 0 9 16 8.5050 1.8650 -2 4 23 0.820000 1.5100 6 5 11 3.7500 1.5400 8 3 1 6.5800 1.9100 0 12 1 2.0750 1.6508 0 12 2 1.6900 1.5600 -1 7 20 3.5700 1.3600 1 11 9 3.5800 1.4600 2 11 7 4.3400 1.6400 -3 1 24 8.0700 2.0100 5 9 5 2.6800 1.6600 -7 2 16 1.3500 2.1900 7 6 3 1.4400 1.6900 1 3 23 0.250000 1.5000 4 6 16 1.7800 1.6500 7 2 10 5.5950 2.0250 0 12 3 4.7200 1.9200 -4 2 23 3.9500 1.8800 -5 9 10 6.2400 1.4300 -6 0 20 0.340000 1.7200 -7 0 17 13.0700 2.3100 0 7 20 0.610000 1.6200 4 9 10 0.480000 1.4000 -6 3 19 0.200000 1.1200 -7 1 17 0.690000 1.9600 1 1 24 4.2000 1.8300 1 12 3 0.800000 1.8700 2 5 21 3.8100 1.4200 3 7 17 0.490000 1.0400 3 9 13 4.4700 1.9100 ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_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 0.38211(11) 0.355396(15) 0.40123(4) 0.05484(14) Uani d 1 . . O O2 0.63464(12) 0.29985(8) 0.32233(4) 0.06801(17) Uani d 1 . . O O3 0.73388(12) -0.08048(8) 0.46784(4) 0.06574(16) Uani d 1 . . N N1 0.57479(13) 0.14069(8) 0.42246(5) 0.05046(16) Uani d 1 . . H H1 0.474(2) 0.1271(16) 0.4629(7) 0.08754 Uani calc 1 . . C C5 0.54053(15) 0.27070(10) 0.37571(5) 0.04754(17) Uani d 1 . . C C6 0.73373(15) 0.02549(11) 0.42216(6) 0.05121(18) Uani d 1 . . C C1 0.30097(15) 0.50254(10) 0.36327(6) 0.05446(18) Uani d 1 . . C C7 0.89889(19) 0.03248(14) 0.36770(7) 0.0716(3) Uani d 1 . . H H7A 1.0210(16) -0.0607(14) 0.3829(8) 0.10454 Uani calc 1 . . H H7B 0.9899(18) 0.1427(14) 0.3755(9) 0.11089 Uani calc 1 . . H H7C 0.818(2) 0.0353(17) 0.3076(6) 0.11503 Uani calc 1 . . C C4 0.18467(19) 0.46831(14) 0.28329(7) 0.0740(3) Uani d 1 . . H H4A 0.3039(17) 0.4270(16) 0.2468(6) 0.10880 Uani calc 1 . . H H4B 0.106(2) 0.5761(14) 0.2597(8) 0.11611 Uani calc 1 . . H H4C 0.0505(16) 0.3836(15) 0.2852(8) 0.11411 Uani calc 1 . . C C3 0.4904(2) 0.61607(13) 0.36559(8) 0.0758(2) Uani d 1 . . H H3A 0.578(2) 0.6274(16) 0.4245(8) 0.11708 Uani calc 1 . . H H3B 0.419(2) 0.7310(12) 0.3505(9) 0.12094 Uani calc 1 . . H H3C 0.6142(17) 0.5881(15) 0.3283(7) 0.10779 Uani calc 1 . . C C2 0.1345(2) 0.55587(15) 0.41419(8) 0.0822(3) Uani d 1 . . H H2A 0.0073(16) 0.4648(14) 0.4127(9) 0.11714 Uani calc 1 . . H H2B 0.054(2) 0.6620(14) 0.3891(8) 0.12347 Uani calc 1 . . H H2C 0.232(2) 0.5828(17) 0.4703(7) 0.12492 Uani 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 0.0660(4) 0.0489(4) 0.0515(4) 0.0085(3) 0.0150(3) 0.0127(3) O2 0.0786(5) 0.0669(5) 0.0644(5) 0.0061(4) 0.0300(4) 0.0184(3) O3 0.0745(5) 0.0484(4) 0.0771(5) 0.0077(3) 0.0204(4) 0.0162(3) N1 0.0599(5) 0.0439(4) 0.0495(5) 0.0021(3) 0.0144(3) 0.0091(3) H1 0.09872 0.08344 0.09180 0.02741 0.05087 0.03885 C5 0.0539(5) 0.0441(5) 0.0456(5) -0.0003(4) 0.0107(4) 0.0056(4) C6 0.0573(5) 0.0430(5) 0.0533(5) -0.0001(4) 0.0083(4) 0.0024(4) C1 0.0592(5) 0.0460(5) 0.0551(5) 0.0050(4) -0.0011(4) 0.0103(4) C7 0.0720(7) 0.0747(7) 0.0731(7) 0.0168(6) 0.0274(6) 0.0133(6) H7A 0.09887 0.10412 0.11797 0.04100 0.04001 0.02395 H7B 0.08822 0.09468 0.16018 -0.00028 0.05229 0.03275 H7C 0.14423 0.13621 0.06953 0.04903 0.03193 0.00590 C4 0.0757(7) 0.0794(8) 0.0597(7) -0.0079(6) -0.0129(5) 0.0126(6) H4A 0.12776 0.13382 0.06263 0.00285 0.00747 0.00354 H4B 0.11933 0.11272 0.10174 0.01287 -0.02973 0.03707 H4C 0.09893 0.11674 0.11538 -0.03490 -0.01984 0.00269 C3 0.0723(7) 0.0514(6) 0.0968(9) -0.0083(5) -0.0096(6) 0.0110(6) H3A 0.11467 0.09511 0.12396 -0.01659 -0.03780 -0.00724 H3B 0.11702 0.05611 0.17940 -0.00332 -0.01031 0.02819 H3C 0.08755 0.09430 0.14362 -0.01523 0.02433 0.02842 C2 0.0844(8) 0.0751(8) 0.0889(9) 0.0249(6) 0.0193(6) 0.0046(7) H2A 0.09735 0.11323 0.15160 0.01562 0.05342 0.02003 H2B 0.12561 0.09416 0.15181 0.05340 0.02495 0.01964 H2C 0.15392 0.13217 0.08898 0.04922 0.01950 -0.01800 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 'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177' H H 0.0000 0.0000 'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177' N N 0.0061 0.0033 'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177' O O 0.0106 0.0060 'Clementi & Roetti 1974. Atomic Data & Nuclear Data Tables. 14, 177' 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 O1 C1 . . . 121.38(6) ? C5 N1 C6 . . . 128.22(7) ? C5 N1 H1 . . . 117.3(7) ? C6 N1 H1 . . . 114.4(7) ? O1 C5 O2 . . . 126.91(8) ? O1 C5 N1 . . . 106.93(7) ? O2 C5 N1 . . . 126.15(7) ? O3 C6 N1 . . . 117.82(7) ? O3 C6 C7 . . . 121.61(8) ? N1 C6 C7 . . . 120.57(8) ? O1 C1 C3 . . . 110.28(7) ? O1 C1 C4 . . . 109.28(7) ? O1 C1 C2 . . . 101.29(7) ? C3 C1 C4 . . . 113.48(8) ? C3 C1 C2 . . . 110.99(9) ? C4 C1 C2 . . . 110.85(9) ? C6 C7 H7C . . . 112.4(7) ? C6 C7 H7A . . . 107.8(6) ? C6 C7 H7B . . . 109.1(7) ? H7C C7 H7A . . . 115.8(9) ? H7C C7 H7B . . . 104.0(10) ? H7A C7 H7B . . . 107.3(8) ? C1 C4 H4C . . . 110.1(7) ? C1 C4 H4A . . . 111.0(6) ? C1 C4 H4B . . . 107.6(6) ? H4C C4 H4A . . . 111.0(10) ? H4C C4 H4B . . . 107.3(10) ? H4A C4 H4B . . . 110.0(10) ? C1 C3 H3C . . . 115.4(7) ? C1 C3 H3B . . . 108.2(6) ? C1 C3 H3A . . . 109.8(7) ? H3C C3 H3B . . . 109.0(10) ? H3C C3 H3A . . . 108.3(10) ? H3B C3 H3A . . . 105.0(10) ? C1 C2 H2C . . . 106.5(7) ? C1 C2 H2B . . . 107.8(8) ? C1 C2 H2A . . . 107.1(7) ? H2C C2 H2B . . . 109.3(10) ? H2C C2 H2A . . . 117.0(10) ? H2B C2 H2A . . . 108.8(10) ? 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 C5 . 1.3344(11) ? O1 C1 . 1.4808(9) ? O2 C5 . 1.1970(11) ? O3 C6 . 1.2164(11) ? N1 C5 . 1.3864(12) ? N1 C6 . 1.3811(12) ? N1 H1 . 1.013(8) ? C6 C7 . 1.4868(15) ? C1 C3 . 1.5009(14) ? C1 C4 . 1.5042(15) ? C1 C2 . 1.5170(16) ? C7 H7C . 1.09500 ? C7 H7A . 1.09500 ? C7 H7B . 1.09500 ? C4 H4C . 1.09500 ? C4 H4A . 1.09500 ? C4 H4B . 1.09500 ? C3 H3C . 1.09500 ? C3 H3B . 1.09500 ? C3 H3A . 1.09500 ? C2 H2C . 1.09500 ? C2 H2B . 1.09500 ? C2 H2A . 1.09500 ? 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 C4 H4A O2 1 1.095 2.479 3.0651(14) 112.16 C3 H3C O2 1 1.095 2.489 2.9928(15) 106.68 N1 H1 O3 3_656 1.013(8) 1.920(9) 2.9285(11) 173.1(2) 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C5 N1 C6 . . . . -174.66(12) ? O1 C5 N1 H1 . . . . 4.0(10) ? O1 C1 C3 H3C . . . . 71.1(8) ? O1 C1 C3 H3B . . . . -166.1(9) ? O1 C1 C3 H3A . . . . -51.6(9) ? O1 C1 C4 H4C . . . . 55.5(7) ? O1 C1 C4 H4A . . . . -67.8(7) ? O1 C1 C4 H4B . . . . 172.1(9) ? O1 C1 C2 H2C . . . . 66.4(7) ? O1 C1 C2 H2B . . . . -176.4(7) ? O1 C1 C2 H2A . . . . -59.4(7) ? O2 C5 O1 C1 . . . . 0.45(12) ? O2 C5 N1 C6 . . . . 5.90(14) ? O2 C5 N1 H1 . . . . -175.0(10) ? O3 C6 N1 C5 . . . . -179.23(13) ? O3 C6 N1 H1 . . . . 2.0(10) ? O3 C6 C7 H7C . . . . 121.4(9) ? O3 C6 C7 H7A . . . . -7.4(8) ? O3 C6 C7 H7B . . . . -123.6(8) ? N1 C5 O1 C1 . . . . -178.99(12) ? N1 C6 C7 H7C . . . . -58.8(8) ? N1 C6 C7 H7A . . . . 172.4(8) ? N1 C6 C7 H7B . . . . 56.1(8) ? H1 N1 C6 C7 . . . . -178.0(10) ? C5 O1 C1 C3 . . . . -60.18(11) ? C5 O1 C1 C4 . . . . 65.21(11) ? C5 O1 C1 C2 . . . . -177.77(12) ? C5 N1 C6 C7 . . . . 1.01(14) ? C4 C1 C3 H3C . . . . -51.9(7) ? C4 C1 C3 H3B . . . . 70.9(7) ? C4 C1 C3 H3A . . . . -174.6(9) ? C4 C1 C2 H2C . . . . -177.8(9) ? C4 C1 C2 H2B . . . . -60.5(7) ? C4 C1 C2 H2A . . . . 56.4(8) ? H4A C4 C1 C3 . . . . 56.0(10) ? H4A C4 C1 C2 . . . . -179.0(10) ? H4B C4 C1 C3 . . . . -64.0(10) ? H4B C4 C1 C2 . . . . 61.0(10) ? H4C C4 C1 C3 . . . . 179.0(10) ? H4C C4 C1 C2 . . . . -55.0(10) ? C3 C1 C2 H2C . . . . -50.7(7) ? C3 C1 C2 H2B . . . . 66.5(8) ? C3 C1 C2 H2A . . . . -176.5(8) ? H3A C3 C1 C2 . . . . 60.0(10) ? H3B C3 C1 C2 . . . . -55.0(10) ? H3C C3 C1 C2 . . . . -177.0(10) ?