#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:25:40 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227260 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035845.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_4035845 loop_ _publ_author_name 'Skalenko, Yevhen A.' 'Druzhenko, Tetiana V.' 'Denisenko, Aleksandr V.' 'Samoilenko, Maryna V.' 'Dacenko, Oleksandr P.' 'Trofymchuk, Serhii A.' 'Grygorenko, Oleksandr O.' 'Tolmachev, Andrey A.' 'Mykhailiuk, Pavel K.' _publ_section_title ; [2+2]-Photocycloaddition of N-Benzylmaleimide to Alkenes As an Approach to Functional 3-Azabicyclo[3.2.0]heptanes. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6275 _journal_page_last 6289 _journal_paper_doi 10.1021/acs.joc.8b00077 _journal_volume 83 _journal_year 2018 _chemical_formula_sum 'C15 H15 N O3' _chemical_formula_weight 257.28 _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-2014/7 _cell_angle_alpha 90 _cell_angle_beta 109.14(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.141(3) _cell_length_b 12.9427(19) _cell_length_c 8.5151(19) _cell_measurement_reflns_used 545 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.1 _cell_measurement_theta_min 3.9 _cell_volume 1264.1(5) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_unetI/netI 0.1105 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 13113 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.000 _diffrn_reflns_theta_min 2.982 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.352 _exptl_crystal_description plate _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.149 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.798 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 3609 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.798 _refine_ls_R_factor_all 0.1991 _refine_ls_R_factor_gt 0.0566 _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^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.1338 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1216 _reflns_number_total 3609 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00077_si_002.cif _cod_data_source_block 24a _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4035845 _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. ; _shelx_estimated_absorpt_t_min 0.981 _shelx_estimated_absorpt_t_max 0.991 _shelx_hkl_file ; 2 0 0 7714.72 56.58 -2 0 0 7194.79 56.02 3 0 0 2.35 2.13 4 0 0 202.30 13.27 5 0 0 54.79 7.74 6 0 0 99.20 11.46 7 0 0 83.16 11.44 8 0 0 1.27 2.55 9 0 0 60.66 10.60 10 0 0 336.69 27.04 11 0 0 14.45 6.36 12 0 0 9.78 4.41 -13 0 0 -0.35 2.32 13 0 0 5.57 6.79 14 0 0 7.67 6.34 -14 0 0 -2.78 3.24 -14 0 0 -4.63 6.11 -15 0 0 11.93 8.02 -15 0 0 3.12 4.63 15 0 0 -2.51 4.62 16 0 0 0.59 2.52 -16 0 0 1.23 3.74 -16 -1 0 -3.40 4.65 -16 -1 0 -1.30 3.71 -15 -1 0 -4.53 2.65 15 1 0 1.63 3.69 -15 -1 0 -4.69 3.22 14 1 0 -1.88 5.09 -14 -1 0 1.96 2.83 -14 -1 0 -1.95 4.69 -13 -1 0 4.24 5.53 13 1 0 7.56 5.64 12 1 0 22.63 8.28 11 1 0 13.20 5.82 10 1 0 50.56 10.07 9 1 0 31.06 7.97 8 1 0 19.02 6.05 7 1 0 14.61 4.89 6 1 0 6.22 3.59 5 1 0 374.70 18.68 4 1 0 0.50 1.12 3 1 0 96.99 7.16 -2 -1 0 97.77 5.79 2 1 0 105.66 5.90 -2 1 0 86.75 6.78 2 -1 0 97.71 6.87 -2 1 0 110.37 5.92 3 -1 0 97.13 8.36 4 -1 0 -4.66 2.71 5 -1 0 390.53 20.96 6 -1 0 12.78 4.21 7 -1 0 11.11 4.48 8 -1 0 39.84 8.61 9 -1 0 45.72 10.31 10 -1 0 50.37 11.12 -11 1 0 7.92 4.12 11 -1 0 12.32 7.10 -12 1 0 18.12 6.77 12 -1 0 10.60 6.97 13 -1 0 6.39 4.97 -13 1 0 8.18 5.19 14 -1 0 -0.06 3.03 -14 1 0 2.46 4.96 -14 1 0 1.72 4.31 15 -1 0 -1.76 3.21 -15 1 0 0.71 4.39 16 -1 0 -1.93 5.40 -16 -2 0 3.64 7.13 -16 -2 0 -2.96 6.40 -15 -2 0 12.27 7.03 -15 -2 0 3.54 3.24 15 2 0 7.02 5.85 14 2 0 -4.36 5.41 -14 -2 0 3.46 4.43 13 2 0 8.58 4.38 -13 -2 0 1.79 2.69 12 2 0 -0.19 3.61 -12 -2 0 13.73 6.51 11 2 0 0.88 4.66 10 2 0 6.65 4.59 9 2 0 20.47 6.32 8 2 0 72.02 10.82 7 2 0 12.27 4.25 6 2 0 238.61 16.00 5 2 0 -2.42 1.44 4 2 0 271.20 13.62 3 2 0 8.70 2.81 2 2 0 49.82 4.25 -2 -2 0 51.06 4.34 -1 -2 0 -1.06 1.20 -1 -2 0 -0.04 0.56 1 2 0 1.46 0.79 1 2 0 1.16 0.81 0 2 0 223.62 9.15 1 -2 0 0.96 0.69 1 -2 0 1.81 0.52 -1 2 0 2.89 0.99 1 -2 0 5.49 1.50 2 -2 0 45.15 5.29 -2 2 0 46.94 3.78 -2 2 0 48.89 4.02 2 -2 0 48.73 4.18 -3 2 0 9.86 2.36 -3 2 0 7.28 2.02 3 -2 0 14.11 3.62 -4 2 0 285.33 13.71 4 -2 0 279.22 16.88 5 -2 0 1.18 3.61 -5 2 0 0.33 1.16 6 -2 0 260.70 19.46 -6 2 0 256.30 16.62 -7 2 0 15.67 5.02 7 -2 0 6.93 3.39 8 -2 0 72.28 11.67 -8 2 0 76.94 10.65 9 -2 0 25.77 8.70 -9 2 0 25.23 6.78 -10 2 0 -4.01 3.12 10 -2 0 4.27 5.16 11 -2 0 6.02 6.89 -11 2 0 2.78 2.85 12 -2 0 -3.73 6.79 -12 2 0 -0.57 3.68 12 -2 0 5.12 7.16 -13 2 0 4.21 3.40 13 -2 0 -2.76 5.67 14 -2 0 5.19 4.70 -14 2 0 5.27 5.16 15 -2 0 2.81 2.73 16 -2 0 0.59 3.14 17 -2 0 -3.66 2.73 -16 -3 0 1.66 2.59 -16 -3 0 6.05 6.72 -15 -3 0 4.30 2.31 -14 -3 0 3.72 4.15 14 3 0 -0.71 3.77 13 3 0 3.55 3.33 -13 -3 0 13.66 7.22 12 3 0 1.52 2.95 -12 -3 0 -6.25 4.61 -11 -3 0 49.30 11.88 11 3 0 61.40 11.83 10 3 0 -1.12 1.53 9 3 0 178.44 17.41 8 3 0 22.58 5.51 7 3 0 2.97 1.74 6 3 0 56.60 7.68 5 3 0 4.95 2.46 4 3 0 52.23 6.03 3 3 0 965.43 22.94 -2 -3 0 20.81 3.60 2 3 0 13.57 2.57 -2 -3 0 17.40 3.14 -2 -3 0 14.13 2.45 -1 -3 0 1558.56 26.08 1 3 0 1639.44 26.59 -1 -3 0 1652.79 29.71 -1 -3 0 1682.12 33.02 0 -3 0 1.35 0.79 0 3 0 -1.31 1.59 0 -3 0 1.52 1.26 1 -3 0 1671.05 31.93 1 -3 0 1613.93 22.07 -1 3 0 1619.50 23.83 -1 3 0 1643.49 22.84 2 -3 0 12.64 3.36 -2 3 0 11.96 1.92 -2 3 0 14.25 2.54 2 -3 0 13.22 2.10 2 -3 0 12.88 2.36 3 -3 0 988.25 30.33 -3 3 0 1031.43 22.60 3 -3 0 908.47 21.61 -3 3 0 946.48 20.58 -4 3 0 56.42 5.94 4 -3 0 44.45 7.10 5 -3 0 3.61 3.63 -5 3 0 3.22 1.88 6 -3 0 50.92 9.43 -6 3 0 49.16 7.13 -7 3 0 4.30 3.16 7 -3 0 -4.07 2.48 -8 3 0 24.55 6.19 8 -3 0 24.80 8.14 -9 3 0 193.92 18.00 9 -3 0 172.99 20.15 -10 3 0 3.20 2.34 10 -3 0 6.77 4.89 -11 3 0 67.55 12.28 11 -3 0 67.62 14.61 -12 3 0 4.98 2.83 12 -3 0 6.73 5.06 13 -3 0 14.50 8.19 13 -3 0 7.69 4.66 -13 3 0 4.10 1.76 14 -3 0 -1.92 7.46 15 -3 0 -7.18 7.52 16 -3 0 1.95 4.99 -16 -4 0 8.21 8.96 -15 -4 0 -2.22 5.76 -14 -4 0 2.60 3.48 -13 -4 0 -0.94 3.01 13 4 0 0.50 2.06 12 4 0 -2.26 2.79 -12 -4 0 5.17 5.08 11 4 0 6.44 4.44 -11 -4 0 5.01 6.76 -10 -4 0 26.94 8.51 10 4 0 28.39 6.89 -9 -4 0 3.04 3.30 9 4 0 -0.95 1.90 -8 -4 0 57.40 10.75 8 4 0 51.65 8.63 7 4 0 0.50 1.79 -6 -4 0 -0.91 2.64 6 4 0 1.37 1.15 -5 -4 0 12.13 3.67 5 4 0 9.22 2.94 -4 -4 0 27.90 5.59 4 4 0 33.36 5.27 -3 -4 0 -2.16 1.42 -3 -4 0 -1.27 1.70 3 4 0 0.24 1.04 2 4 0 642.46 19.61 -2 -4 0 674.59 25.33 -2 -4 0 605.42 22.50 -1 -4 0 5.90 2.03 -1 -4 0 11.71 3.32 0 -4 0 61.34 6.48 0 -4 0 67.03 6.06 1 -4 0 9.09 2.03 -1 4 0 9.25 2.30 1 -4 0 13.59 3.45 -1 4 0 8.45 1.47 2 -4 0 675.46 24.54 -2 4 0 641.91 15.98 2 -4 0 629.95 15.67 2 -4 0 603.56 17.49 -3 4 0 0.24 0.52 3 -4 0 2.07 1.40 3 -4 0 -0.60 1.70 -3 4 0 1.65 1.56 4 -4 0 34.22 6.19 -4 4 0 36.65 4.82 5 -4 0 10.40 4.81 -5 4 0 11.30 3.35 -6 4 0 0.39 1.62 6 -4 0 1.47 3.03 7 -4 0 2.97 3.54 -7 4 0 -0.33 1.91 -8 4 0 54.90 8.42 8 -4 0 65.75 12.50 9 -4 0 8.56 4.55 -9 4 0 2.15 2.57 10 -4 0 21.02 7.50 -10 4 0 14.10 4.97 -11 4 0 10.47 5.00 11 -4 0 1.23 4.66 12 -4 0 3.47 2.22 -12 4 0 2.24 3.49 13 -4 0 13.22 7.69 14 -4 0 2.58 2.85 14 -4 0 -6.52 5.51 15 -4 0 -1.57 3.94 16 -4 0 5.41 6.65 -16 -5 0 -5.87 7.68 -15 -5 0 4.64 4.32 -14 -5 0 -6.72 5.75 -13 -5 0 -0.20 2.02 -12 -5 0 3.77 3.15 12 5 0 -3.75 4.05 11 5 0 -0.22 2.33 -11 -5 0 -3.71 5.77 -10 -5 0 -1.11 2.04 10 5 0 -4.98 3.96 -9 -5 0 2.52 3.71 9 5 0 -2.33 1.31 -8 -5 0 -5.70 6.37 8 5 0 0.21 2.53 -7 -5 0 25.01 6.24 7 5 0 28.89 6.28 -6 -5 0 -3.10 2.29 6 5 0 4.42 3.03 5 5 0 253.09 15.57 -5 -5 0 268.95 19.72 -4 -5 0 2.64 3.29 4 5 0 -1.65 1.43 -3 -5 0 100.75 11.21 3 5 0 93.48 8.52 -3 -5 0 101.03 10.40 2 5 0 1.06 1.49 -2 -5 0 0.22 1.70 -2 -5 0 1.69 2.07 -1 -5 0 447.22 21.49 -1 -5 0 454.76 19.96 -1 -5 0 445.43 19.15 0 -5 0 0.75 2.40 0 -5 0 -0.74 1.63 1 -5 0 443.10 20.64 1 -5 0 446.19 15.57 -2 5 0 1.62 1.42 2 -5 0 -0.18 1.26 -2 5 0 -0.10 0.64 2 -5 0 1.42 2.02 3 -5 0 92.08 10.47 3 -5 0 91.91 6.86 -4 5 0 -0.27 1.23 4 -5 0 -5.39 2.96 5 -5 0 263.69 20.26 -5 5 0 263.81 14.95 6 -5 0 4.02 4.16 -6 5 0 -0.73 1.55 7 -5 0 43.47 9.58 -7 5 0 31.48 5.78 -8 5 0 2.65 2.72 8 -5 0 -4.88 2.82 -9 5 0 4.87 2.97 9 -5 0 3.50 5.19 10 -5 0 -5.99 4.75 -10 5 0 -0.54 2.22 11 -5 0 4.02 5.31 -11 5 0 9.05 4.48 12 -5 0 8.28 6.90 13 -5 0 -1.39 3.40 14 -5 0 4.98 6.50 15 -5 0 4.50 9.80 15 -5 0 5.81 6.23 16 -5 0 -1.78 4.27 -15 -6 0 6.81 6.37 -14 -6 0 6.53 5.33 -13 -6 0 -1.88 2.12 -12 -6 0 -0.47 3.88 -11 -6 0 5.09 3.44 11 6 0 3.97 2.32 -10 -6 0 20.10 7.43 10 6 0 22.33 6.61 -9 -6 0 12.93 5.49 9 6 0 16.53 5.11 8 6 0 3.38 3.06 -8 -6 0 -3.47 3.99 -7 -6 0 30.11 8.25 7 6 0 23.63 5.91 -6 -6 0 5.57 3.54 6 6 0 5.62 2.63 5 6 0 6.35 2.39 -5 -6 0 10.19 4.66 -4 -6 0 20.70 5.92 -4 -6 0 23.69 5.90 4 6 0 21.79 4.93 3 6 0 3.21 1.86 -3 -6 0 -0.07 1.69 -3 -6 0 0.96 2.54 -2 -6 0 39.12 4.12 -2 -6 0 56.91 8.89 -2 -6 0 49.70 7.39 -1 -6 0 2.08 2.50 -1 -6 0 -0.77 2.03 -1 -6 0 3.77 2.67 0 -6 0 59.87 7.03 0 -6 0 73.53 7.64 0 -6 0 77.91 9.51 1 -6 0 1.42 1.18 1 -6 0 1.14 2.26 2 -6 0 56.24 5.88 2 -6 0 58.69 8.58 -2 6 0 45.27 4.38 3 -6 0 -0.59 1.21 3 -6 0 0.93 1.44 4 -6 0 16.79 3.20 4 -6 0 20.46 5.07 5 -6 0 -1.75 2.65 -5 6 0 4.94 2.08 6 -6 0 8.88 2.93 -6 6 0 2.73 1.83 -7 6 0 20.18 4.97 7 -6 0 11.72 5.79 -8 6 0 4.36 2.37 8 -6 0 -4.20 5.59 -9 6 0 19.29 4.94 9 -6 0 17.57 6.78 10 -6 0 20.54 7.19 -10 6 0 29.37 7.65 11 -6 0 4.59 4.67 12 -6 0 -5.47 5.55 13 -6 0 -1.39 3.53 14 -6 0 -2.66 4.21 15 -6 0 8.13 6.16 -15 -7 0 4.05 6.94 -14 -7 0 -6.15 7.69 -13 -7 0 3.78 6.05 -12 -7 0 -0.07 3.04 -11 -7 0 0.95 2.42 -10 -7 0 2.23 3.94 10 7 0 1.30 3.02 9 7 0 -3.17 3.13 -9 -7 0 4.50 4.06 -8 -7 0 -0.32 2.91 8 7 0 1.19 1.18 -7 -7 0 15.01 6.54 7 7 0 10.23 3.64 -6 -7 0 7.73 4.29 6 7 0 -0.21 1.88 -5 -7 0 78.87 12.04 5 7 0 61.29 8.47 4 7 0 7.03 3.01 -4 -7 0 4.73 2.32 -4 -7 0 3.58 2.87 -3 -7 0 176.42 15.89 -3 -7 0 172.28 16.48 3 7 0 156.94 12.93 -2 -7 0 -2.38 1.65 -2 -7 0 -0.05 0.64 -2 -7 0 -1.29 1.23 -1 -7 0 37.15 7.25 -1 -7 0 37.05 6.56 -1 -7 0 37.10 7.28 0 -7 0 3.43 2.49 0 -7 0 -1.56 1.96 0 -7 0 -0.38 1.69 1 -7 0 40.40 7.29 1 -7 0 33.39 5.35 2 -7 0 -0.80 1.45 -2 7 0 0.10 0.45 2 -7 0 1.58 1.71 3 -7 0 192.17 17.35 3 -7 0 157.13 10.17 4 -7 0 3.07 1.68 4 -7 0 7.89 3.35 5 -7 0 83.69 13.01 -6 7 0 3.48 1.80 6 -7 0 8.22 4.69 7 -7 0 19.94 8.32 -7 7 0 10.61 3.59 -8 7 0 -1.90 0.95 8 -7 0 -1.78 3.54 9 -7 0 -3.74 3.41 -9 7 0 -1.49 2.67 10 -7 0 -0.85 3.64 11 -7 0 2.75 4.18 12 -7 0 -5.56 5.44 13 -7 0 10.26 4.96 14 -7 0 -0.54 3.46 15 -7 0 4.75 6.62 -14 -8 0 -4.86 4.81 -13 -8 0 6.08 7.00 -12 -8 0 -4.03 6.60 -11 -8 0 -2.48 2.41 -10 -8 0 -0.95 4.19 9 8 0 0.96 1.05 -9 -8 0 -0.48 4.68 8 8 0 32.19 6.72 -8 -8 0 48.15 11.58 -7 -8 0 6.79 6.11 7 8 0 2.37 3.18 -6 -8 0 6.39 4.27 6 8 0 5.38 2.74 -5 -8 0 8.72 5.62 5 8 0 6.08 3.13 -4 -8 0 61.96 10.66 4 8 0 54.15 8.08 -4 -8 0 70.07 11.55 -3 -8 0 11.79 5.16 -3 -8 0 9.04 4.38 -2 -8 0 92.11 12.78 -2 -8 0 84.32 11.17 -2 -8 0 82.48 10.86 -1 -8 0 1.66 2.15 -1 -8 0 3.27 2.96 -1 -8 0 0.21 1.49 0 -8 0 626.89 25.77 0 -8 0 643.10 30.72 1 -8 0 -2.80 1.95 1 -8 0 -1.43 2.50 2 -8 0 82.24 11.73 -2 8 0 56.66 3.83 2 -8 0 72.64 7.83 3 -8 0 12.27 2.91 3 -8 0 17.42 6.42 4 -8 0 43.48 9.64 4 -8 0 45.48 5.90 5 -8 0 15.37 5.83 6 -8 0 5.93 3.96 7 -8 0 13.49 8.22 -8 8 0 39.41 7.30 8 -8 0 59.05 13.65 9 -8 0 5.83 4.29 10 -8 0 -3.42 7.28 11 -8 0 4.70 5.69 12 -8 0 8.22 8.38 13 -8 0 0.66 6.47 14 -8 0 -5.91 6.47 -14 -9 0 9.18 8.74 -13 -9 0 -7.21 5.78 -12 -9 0 4.86 4.45 -11 -9 0 -2.51 3.50 -10 -9 0 -0.39 4.69 -9 -9 0 -5.67 4.17 -8 -9 0 2.70 4.10 8 9 0 1.52 1.61 7 9 0 5.74 3.42 -7 -9 0 1.32 2.39 6 9 0 15.21 5.01 -6 -9 0 12.76 6.32 -5 -9 0 28.65 7.37 -5 -9 0 32.42 9.64 5 9 0 31.01 6.85 -4 -9 0 4.96 3.96 -4 -9 0 6.83 4.44 -3 -9 0 55.64 9.86 -3 -9 0 70.60 11.95 -3 -9 0 61.52 10.20 -2 -9 0 -1.16 2.22 -2 -9 0 3.46 2.35 -2 -9 0 2.21 2.98 -1 -9 0 44.12 8.48 -1 -9 0 44.51 9.22 -1 -9 0 44.47 7.88 0 -9 0 -0.85 1.87 0 -9 0 1.63 1.71 0 -9 0 -0.70 4.22 1 -9 0 52.58 9.54 1 -9 0 39.74 6.56 2 -9 0 0.18 0.99 2 -9 0 0.81 3.91 3 -9 0 60.02 7.25 3 -9 0 71.63 11.66 4 -9 0 7.40 2.57 4 -9 0 7.43 3.85 5 -9 0 22.03 4.22 5 -9 0 19.17 7.27 6 -9 0 9.64 3.92 7 -9 0 3.03 4.24 8 -9 0 8.43 6.91 9 -9 0 -0.05 4.43 10 -9 0 -2.53 7.09 11 -9 0 0.20 3.65 12 -9 0 -3.67 5.00 13 -9 0 2.09 2.91 14 -9 0 -10.94 7.25 -13 -10 0 2.33 4.57 -12 -10 0 -1.84 3.83 -11 -10 0 3.63 2.57 -10 -10 0 6.43 6.44 -9 -10 0 -4.86 5.27 -8 -10 0 37.84 11.53 7 10 0 7.40 3.83 -7 -10 0 17.34 7.45 6 10 0 3.02 1.79 -6 -10 0 3.43 2.05 -5 -10 0 21.64 6.97 -5 -10 0 16.78 5.49 -4 -10 0 7.68 6.45 -4 -10 0 8.06 2.93 -3 -10 0 4.34 2.87 -3 -10 0 9.84 4.92 -3 -10 0 14.82 5.52 -2 -10 0 4.87 2.86 -2 -10 0 7.35 3.92 -2 -10 0 6.22 3.47 -1 -10 0 1.58 2.32 -1 -10 0 -1.15 3.53 -1 -10 0 5.31 2.46 -1 -10 0 3.44 1.46 0 -10 0 200.70 19.31 0 -10 0 207.84 21.12 0 -10 0 179.71 15.33 1 -10 0 5.12 5.44 1 -10 0 -0.42 1.56 2 -10 0 4.76 3.84 2 -10 0 5.45 2.41 3 -10 0 4.21 2.22 3 -10 0 -2.05 3.75 4 -10 0 8.03 2.64 4 -10 0 18.55 7.56 5 -10 0 33.92 8.90 6 -10 0 16.83 6.80 7 -10 0 11.43 6.55 8 -10 0 35.56 10.92 9 -10 0 2.54 2.84 10 -10 0 18.39 9.36 11 -10 0 -11.17 8.99 12 -10 0 -5.65 4.78 13 -10 0 -11.99 8.91 -12 -11 0 -6.28 5.87 -11 -11 0 5.63 4.68 -10 -11 0 3.63 6.06 -9 -11 0 -1.65 3.97 -8 -11 0 -0.58 2.47 -7 -11 0 26.66 8.39 -6 -11 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-3.21 4.33 -6 -6 11 -2.73 1.89 6 6 -11 0.24 6.49 -5 -6 11 3.82 4.12 5 6 -11 -1.43 2.96 -4 -6 11 -1.47 2.89 4 6 -11 -1.83 3.87 -3 -6 11 -1.04 2.58 -2 -6 11 -1.35 2.45 10 7 -11 0.46 4.85 9 7 -11 -4.66 4.03 8 7 -11 4.04 7.63 -8 -7 11 0.33 3.78 7 7 -11 13.07 9.34 -7 -7 11 -3.81 5.42 -6 -7 11 -5.17 3.77 6 7 -11 -3.01 3.60 -5 -7 11 2.69 2.91 5 7 -11 -7.95 8.12 -4 -7 11 -2.94 5.28 4 7 -11 0.16 3.79 3 7 -11 -2.96 5.42 9 8 -11 -8.37 7.06 8 8 -11 -0.72 6.62 7 8 -11 12.25 8.06 6 8 -11 6.58 6.66 5 8 -11 3.19 6.31 3 8 -11 -1.51 6.90 -5 5 12 6.45 6.25 -5 4 12 0.94 3.14 -4 4 12 -4.28 5.13 -3 4 12 -1.66 2.73 -5 3 12 3.41 4.39 -4 3 12 2.63 4.36 -3 3 12 -0.97 1.75 -2 3 12 0.05 2.18 -4 2 12 -0.01 4.32 -3 2 12 -2.31 4.85 -2 2 12 4.20 3.89 -6 1 12 -1.30 3.89 -5 1 12 -4.33 4.52 -3 1 12 3.16 4.98 -2 1 12 1.93 5.26 -1 1 12 -2.05 2.63 -8 0 12 -5.33 3.67 -7 0 12 1.95 3.64 -6 0 12 6.07 5.64 6 0 -12 -0.20 5.54 -5 0 12 -4.10 3.25 5 0 -12 -0.92 6.66 -4 0 12 5.60 6.20 -1 0 12 -1.56 1.62 -10 -1 12 0.46 2.80 -9 -1 12 0.65 3.81 -8 -1 12 1.40 4.43 -7 -1 12 -0.16 2.69 -6 -1 12 -1.84 2.46 -5 -1 12 1.45 4.64 -4 -1 12 -1.18 2.97 -3 -1 12 -1.85 2.11 -10 -2 12 1.05 4.62 -10 -2 12 -0.76 4.22 -9 -2 12 -17.89 8.37 -9 -2 12 0.64 2.87 -8 -2 12 3.31 2.71 -7 -2 12 -0.30 3.47 -6 -2 12 0.03 4.49 -5 -2 12 0.72 1.93 -4 -2 12 -3.68 5.52 -10 -3 12 4.45 5.65 -10 -3 12 1.67 4.04 -9 -3 12 -4.50 5.58 -8 -3 12 -4.77 6.80 -7 -3 12 8.68 6.49 -6 -3 12 7.34 6.29 -5 -3 12 -1.30 5.33 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 63066 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 O1 O 0.44581(16) 0.11133(12) 0.5981(2) 0.0746(6) Uani 1 1 d . . O2 O 0.05724(17) 0.10832(13) 0.3127(2) 0.0740(6) Uani 1 1 d . . O3 O 0.23580(17) -0.23617(11) 0.6461(2) 0.0673(5) Uani 1 1 d . . N1 N 0.25491(18) 0.12625(13) 0.4341(2) 0.0467(5) Uani 1 1 d . . C1 C 0.3383(2) -0.21403(17) 0.6058(3) 0.0678(8) Uani 1 1 d . . H1B H 0.3547 -0.2692 0.5396 0.081 Uiso 1 1 calc R U H1A H 0.4049 -0.2055 0.7059 0.081 Uiso 1 1 calc R U C2 C 0.3114(2) -0.11458(16) 0.5079(3) 0.0493(6) Uani 1 1 d . . H2 H 0.3544 -0.1044 0.4298 0.059 Uiso 1 1 calc R U C3 C 0.3015(2) -0.01685(16) 0.6096(3) 0.0490(6) Uani 1 1 d . . H3 H 0.3253 -0.0267 0.7302 0.059 Uiso 1 1 calc R U C4 C 0.3471(2) 0.07889(17) 0.5541(3) 0.0499(6) Uani 1 1 d . . C5 C 0.1485(2) 0.07839(17) 0.4111(3) 0.0507(6) Uani 1 1 d . . C6 C 0.1698(2) -0.01457(15) 0.5201(3) 0.0455(6) Uani 1 1 d . . H6 H 0.1222 -0.0185 0.5933 0.055 Uiso 1 1 calc R U C7 C 0.1764(2) -0.11596(15) 0.4277(3) 0.0484(6) Uani 1 1 d . . H7 H 0.1478 -0.1108 0.3061 0.058 Uiso 1 1 calc R U C8 C 0.1413(2) -0.21359(17) 0.4969(3) 0.0620(7) Uani 1 1 d . . H8B H 0.0696 -0.2029 0.5214 0.074 Uiso 1 1 calc R U H8A H 0.1298 -0.2699 0.4179 0.074 Uiso 1 1 calc R U C9 C 0.2698(2) 0.21291(15) 0.3322(3) 0.0587(7) Uani 1 1 d . . H9B H 0.2090 0.2095 0.2247 0.070 Uiso 1 1 calc R U H9A H 0.3441 0.2053 0.3136 0.070 Uiso 1 1 calc R U C10 C 0.2659(2) 0.31696(16) 0.4068(3) 0.0439(6) Uani 1 1 d . . C11 C 0.1611(2) 0.36572(18) 0.3858(3) 0.0569(7) Uani 1 1 d . . H11 H 0.0921 0.3338 0.3229 0.068 Uiso 1 1 calc R U C12 C 0.1567(3) 0.4605(2) 0.4561(3) 0.0693(8) Uani 1 1 d . . H12 H 0.0853 0.4925 0.4401 0.083 Uiso 1 1 calc R U C13 C 0.2579(3) 0.50783(18) 0.5498(3) 0.0713(9) Uani 1 1 d . . H13 H 0.2552 0.5717 0.5984 0.086 Uiso 1 1 calc R U C14 C 0.3628(3) 0.46110(19) 0.5716(3) 0.0679(8) Uani 1 1 d . . H14 H 0.4315 0.4933 0.6348 0.082 Uiso 1 1 calc R U C15 C 0.3669(2) 0.36673(17) 0.5006(3) 0.0539(6) Uani 1 1 d . . H15 H 0.4387 0.3357 0.5158 0.065 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0462(13) 0.0631(12) 0.1075(16) 0.0016(10) 0.0157(12) -0.0120(10) O2 0.0573(14) 0.0638(12) 0.0870(15) 0.0057(10) 0.0047(12) 0.0060(10) O3 0.0842(16) 0.0533(10) 0.0682(13) 0.0097(9) 0.0302(13) -0.0029(10) N1 0.0525(14) 0.0388(10) 0.0501(12) -0.0016(9) 0.0186(11) -0.0022(10) C1 0.0617(19) 0.0484(15) 0.088(2) 0.0039(13) 0.0182(17) 0.0016(14) C2 0.0459(16) 0.0467(13) 0.0584(15) -0.0040(11) 0.0215(14) -0.0006(12) C3 0.0551(17) 0.0444(13) 0.0468(14) -0.0024(10) 0.0159(14) -0.0037(12) C4 0.0489(17) 0.0459(14) 0.0544(16) -0.0020(11) 0.0162(15) 0.0019(13) C5 0.0493(17) 0.0448(14) 0.0575(17) -0.0062(11) 0.0168(15) 0.0048(13) C6 0.0445(15) 0.0440(13) 0.0538(15) -0.0028(11) 0.0241(13) -0.0032(11) C7 0.0542(17) 0.0415(13) 0.0500(14) -0.0044(10) 0.0177(14) -0.0050(12) C8 0.0580(19) 0.0485(15) 0.081(2) -0.0019(13) 0.0246(17) -0.0056(13) C9 0.079(2) 0.0461(13) 0.0564(16) -0.0021(11) 0.0296(16) -0.0043(13) C10 0.0549(17) 0.0401(12) 0.0375(13) 0.0036(9) 0.0160(13) 0.0000(12) C11 0.0545(18) 0.0589(16) 0.0528(15) 0.0051(12) 0.0113(14) 0.0039(14) C12 0.081(2) 0.0556(18) 0.081(2) 0.0152(14) 0.039(2) 0.0238(16) C13 0.122(3) 0.0378(14) 0.069(2) 0.0033(13) 0.051(2) 0.0033(18) C14 0.085(2) 0.0556(17) 0.0583(18) -0.0069(13) 0.0168(18) -0.0211(16) C15 0.0539(18) 0.0537(15) 0.0540(15) 0.0060(12) 0.0174(14) 0.0006(13) 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 C1 O3 C8 104.71(17) C4 N1 C5 113.3(2) C4 N1 C9 123.2(2) C5 N1 C9 123.2(2) O3 C1 C2 104.9(2) C1 C2 C7 103.81(18) C1 C2 C3 115.26(19) C7 C2 C3 89.50(16) C4 C3 C6 105.17(19) C4 C3 C2 113.13(17) C6 C3 C2 89.84(17) O1 C4 N1 123.6(2) O1 C4 C3 128.5(3) N1 C4 C3 107.8(2) O2 C5 N1 123.5(2) O2 C5 C6 128.4(2) N1 C5 C6 108.0(2) C5 C6 C3 105.40(18) C5 C6 C7 113.32(18) C3 C6 C7 90.98(16) C8 C7 C6 116.27(17) C8 C7 C2 103.24(19) C6 C7 C2 89.41(17) O3 C8 C7 105.64(19) N1 C9 C10 114.23(16) C11 C10 C15 117.8(2) C11 C10 C9 120.9(2) C15 C10 C9 121.3(2) C12 C11 C10 121.2(3) C13 C12 C11 119.8(3) C14 C13 C12 119.9(2) C13 C14 C15 120.1(3) C14 C15 C10 121.1(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C4 1.207(3) O2 C5 1.213(3) O3 C1 1.424(3) O3 C8 1.435(3) N1 C4 1.387(3) N1 C5 1.387(3) N1 C9 1.465(2) C1 C2 1.510(3) C2 C7 1.555(3) C2 C3 1.560(3) C3 C4 1.496(3) C3 C6 1.529(3) C5 C6 1.489(3) C6 C7 1.546(3) C7 C8 1.513(3) C9 C10 1.496(3) C10 C11 1.379(3) C10 C15 1.383(3) C11 C12 1.374(3) C12 C13 1.370(4) C13 C14 1.366(4) C14 C15 1.371(3) 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 C8 O3 C1 C2 42.2(2) O3 C1 C2 C7 -27.0(2) O3 C1 C2 C3 69.1(3) C1 C2 C3 C4 144.5(2) C7 C2 C3 C4 -110.4(2) C1 C2 C3 C6 -109.0(2) C7 C2 C3 C6 -3.93(16) C5 N1 C4 O1 -176.5(2) C9 N1 C4 O1 8.3(3) C5 N1 C4 C3 5.3(2) C9 N1 C4 C3 -169.94(16) C6 C3 C4 O1 176.7(2) C2 C3 C4 O1 -86.8(3) C6 C3 C4 N1 -5.2(2) C2 C3 C4 N1 91.3(2) C4 N1 C5 O2 179.5(2) C9 N1 C5 O2 -5.3(3) C4 N1 C5 C6 -3.0(2) C9 N1 C5 C6 172.19(16) O2 C5 C6 C3 176.9(2) N1 C5 C6 C3 -0.4(2) O2 C5 C6 C7 78.9(3) N1 C5 C6 C7 -98.4(2) C4 C3 C6 C5 3.4(2) C2 C3 C6 C5 -110.59(16) C4 C3 C6 C7 117.93(17) C2 C3 C6 C7 3.96(16) C5 C6 C7 C8 -152.2(2) C3 C6 C7 C8 100.5(2) C5 C6 C7 C2 103.3(2) C3 C6 C7 C2 -3.97(16) C1 C2 C7 C8 2.9(2) C3 C2 C7 C8 -112.99(17) C1 C2 C7 C6 119.82(17) C3 C2 C7 C6 3.89(16) C1 O3 C8 C7 -40.3(2) C6 C7 C8 O3 -74.1(2) C2 C7 C8 O3 21.9(2) C4 N1 C9 C10 -89.3(3) C5 N1 C9 C10 96.0(3) N1 C9 C10 C11 -84.7(3) N1 C9 C10 C15 94.4(2) C15 C10 C11 C12 -0.2(3) C9 C10 C11 C12 178.96(19) C10 C11 C12 C13 -0.4(3) C11 C12 C13 C14 0.6(4) C12 C13 C14 C15 -0.3(4) C13 C14 C15 C10 -0.3(3) C11 C10 C15 C14 0.5(3) C9 C10 C15 C14 -178.62(19)