#------------------------------------------------------------------------------ #$Date: 2019-09-04 07:09:03 +0300 (Wed, 04 Sep 2019) $ #$Revision: 217959 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021760.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_2021760 loop_ _publ_author_name 'Ben Ali, Karim' 'Retailleau, Pascal' _publ_section_title ; Crystal structure of (1S,2R)-2-[(3R,4S)-3-methyl-4-phenyl-1,2,3,4-tetrahydroisoquinolin-2-yl]-1,2-diphenylethanol ; _journal_coeditor_code FF2162 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 1399 _journal_paper_doi 10.1107/S2056989019011964 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration rm _chemical_formula_iupac 'C30 H29 N O' _chemical_formula_moiety 'C30 H29 N O' _chemical_formula_sum 'C30 H29 N O' _chemical_formula_weight 419.54 _chemical_name_systematic (1S,2R)-2-[(3R,4S)-3-Methyl-4-phenyl-1,2,3,4-tetrahydroisoquinolin-2-yl]-1,2-diphenylethanol _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.3009(8) _cell_length_b 11.0552(11) _cell_length_c 30.006(3) _cell_measurement_reflns_used 6302 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.1570 _cell_measurement_theta_min 2.0140 _cell_volume 2421.9(4) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2019) ; _computing_data_collection ; DENZO (Otwinowski & Minor, 1997); COLLECT (Hooft, 1998) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2019) ; _computing_publication_material ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'Nonius KappaCCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source '1.5kW sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0238 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 21751 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.346 _diffrn_reflns_theta_min 2.715 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2019) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.151 _exptl_crystal_description prism _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.590 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.350 _refine_diff_density_max 0.105 _refine_diff_density_min -0.110 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_extinction_coef 0.0139(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/3 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 295 _refine_ls_number_reflns 4425 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0379 _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^)+(0.0304P)^2^+0.3321P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.0828 _reflns_number_gt 3948 _reflns_number_total 4427 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ff2162sup1.cif _cod_data_source_block I _cod_original_cell_volume 2421.8(4) _cod_database_code 2021760 _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_hkl_file ; 0 0 3 12.12 1.30 0 0 -3 12.73 1.39 0 0 -3 11.29 1.34 0 0 3 14.70 1.22 0 0 4 4331.68 21.75 0 0 -4 4107.02 21.28 0 0 -4 4201.77 19.47 0 0 4 4287.46 19.69 0 0 -5 43.14 3.08 0 0 -5 39.53 2.75 0 0 5 25.21 2.39 0 0 -6 3422.79 20.92 0 0 6 3380.11 23.92 0 0 -6 3413.22 23.95 0 0 -6 3524.60 21.77 0 0 6 3448.69 21.88 0 0 -7 24.67 2.75 0 0 7 6.21 2.05 0 0 -7 15.10 2.37 0 0 7 10.24 1.85 0 0 -7 5.73 1.85 0 0 -7 16.08 1.32 0 0 8 64.46 3.51 0 0 -8 68.85 3.58 0 0 -8 67.51 3.89 0 0 8 62.77 3.81 0 0 -8 67.97 3.48 0 0 -8 68.65 2.06 0 0 -9 3.96 1.23 0 0 -9 1.31 0.47 0 0 -9 0.48 0.93 0 0 9 0.70 0.72 0 0 -9 2.78 1.27 0 0 9 -0.22 0.49 0 0 -10 278.11 7.96 0 0 10 269.38 8.05 0 0 -10 284.17 4.67 0 0 -10 290.99 9.03 0 0 10 276.47 8.82 0 0 -11 5.45 2.13 0 0 -11 5.10 2.13 0 0 11 1.92 1.53 0 0 -12 866.86 15.50 0 0 -12 844.31 16.89 0 0 -13 12.43 3.65 0 0 -13 7.91 2.82 0 0 -14 1650.98 23.29 0 0 -14 1603.30 25.28 0 0 -15 24.36 4.23 0 0 15 5.28 1.67 0 0 -15 9.73 3.16 0 0 16 530.84 10.65 0 0 -16 530.50 15.61 0 0 -16 528.01 14.15 0 0 -17 5.67 2.44 0 0 17 1.07 0.96 0 0 -18 6.66 2.04 0 0 18 6.04 1.29 0 0 -19 -0.05 1.62 0 0 19 1.98 1.12 0 0 20 143.27 6.26 0 0 -20 142.70 8.47 0 0 -21 2.74 2.18 0 0 -22 17.01 3.18 0 0 -23 1.72 1.88 0 0 -24 16.77 3.41 0 0 -25 -0.92 2.30 0 0 -26 0.82 2.07 0 0 -27 -3.54 2.88 0 0 -28 2.08 1.88 0 0 -29 -3.02 3.04 0 0 -30 28.42 5.16 0 0 -31 -3.56 3.22 0 0 -32 55.25 7.21 0 0 -33 0.94 2.40 0 0 -34 0.76 2.38 0 0 -35 -0.11 2.36 0 0 -36 45.76 7.23 0 0 36 34.83 5.86 0 0 -37 1.71 2.17 0 0 37 -1.19 2.64 0 0 38 -7.30 4.09 0 0 39 -1.52 2.28 0 0 40 1.10 2.53 0 0 41 5.18 3.35 0 1 0 -0.02 0.12 0 -1 0 -0.14 0.15 0 1 -1 8.89 0.86 0 -1 -1 6.36 0.65 0 1 1 15.11 0.95 0 1 1 3.44 0.54 0 -1 -1 8.21 0.80 0 -1 1 8.22 0.70 0 1 -1 11.56 0.82 0 -1 2 2407.83 13.36 0 -1 -2 2460.82 13.77 0 -1 -2 2413.26 14.79 0 -1 2 2517.97 14.09 0 1 -2 2592.73 15.66 0 1 3 1042.54 8.76 0 -1 3 1018.27 10.70 0 1 -3 1013.15 10.70 0 -1 -3 1059.59 8.93 0 1 3 1014.15 10.71 0 -1 3 1080.95 10.27 0 -1 -3 1007.13 10.58 0 1 -3 1120.07 10.43 0 -1 -3 1017.64 8.68 0 -1 -4 48.01 2.09 0 -1 4 41.99 2.38 0 1 -4 43.13 2.43 0 1 -4 45.67 2.38 0 -1 4 48.57 2.42 0 -1 -4 46.17 2.03 0 1 4 45.27 2.05 0 -1 -4 43.94 2.06 0 1 4 44.36 2.00 0 -1 -5 708.16 8.02 0 1 -5 694.63 10.50 0 -1 5 669.04 10.21 0 -1 5 702.21 9.84 0 1 -5 722.37 9.97 0 1 5 707.49 8.91 0 -1 -5 700.78 8.65 0 -1 -5 717.43 8.98 0 1 5 686.20 8.64 0 -1 -6 289.57 5.36 0 1 -6 281.62 6.79 0 -1 6 282.37 6.72 0 -1 6 264.51 6.98 0 1 -6 276.28 7.12 0 -1 -6 284.55 6.08 0 1 6 282.54 6.22 0 1 6 291.88 6.14 0 -1 -6 283.45 6.22 0 1 7 2.93 0.82 0 -1 7 0.05 0.45 0 1 -7 0.33 0.46 0 -1 7 0.57 0.44 0 -1 -7 0.40 0.44 0 1 -7 2.69 1.20 0 -1 -7 1.70 0.85 0 1 7 2.82 0.92 0 -1 -7 0.16 0.53 0 -1 -8 69.92 2.86 0 1 -8 64.32 3.97 0 -1 -8 70.06 3.57 0 -1 8 66.15 3.92 0 1 -8 69.76 3.84 0 -1 8 67.83 3.73 0 -1 -8 66.32 3.43 0 1 8 68.28 3.56 0 -1 9 242.04 7.88 0 -1 -9 258.21 5.70 0 1 -9 243.61 8.14 0 -1 -9 257.61 7.20 0 1 9 250.38 7.13 0 -1 -9 249.80 7.02 0 1 -9 257.74 7.67 0 1 9 245.80 8.30 0 1 -10 326.45 9.85 0 1 10 342.51 10.17 0 -1 10 334.16 4.96 0 -1 10 337.62 9.75 0 -1 -10 346.03 6.88 0 1 10 337.52 8.79 0 1 -10 356.18 9.50 0 -1 -10 342.04 8.63 0 -1 11 142.95 3.54 0 -1 11 145.46 6.69 0 1 11 145.76 6.89 0 1 -11 136.71 6.73 0 -1 -11 142.42 5.92 0 1 -11 153.21 6.56 0 -1 -11 143.74 4.62 0 -1 -12 124.69 5.87 0 1 -12 136.21 6.52 0 -1 -12 124.66 4.47 0 1 -12 121.12 6.64 0 -1 12 126.95 3.57 0 1 -13 811.88 16.28 0 -1 -13 814.61 15.36 0 1 -13 779.76 17.42 0 -1 -13 813.28 11.61 0 -1 13 813.90 9.55 0 -1 -14 2.94 1.26 0 1 -14 11.41 2.85 0 -1 -14 9.80 2.56 0 -1 14 5.85 1.27 0 1 -14 3.09 2.42 0 -1 -15 216.05 8.65 0 1 -15 219.25 9.22 0 -1 -15 212.75 6.25 0 1 -15 210.64 9.80 0 -1 15 219.39 5.50 0 -1 -16 518.28 13.78 0 1 -16 561.96 14.95 0 -1 -16 523.08 10.12 0 -1 16 526.36 8.96 0 1 -16 512.19 15.90 0 -1 17 188.40 5.60 0 -1 -17 186.11 6.23 0 1 -17 186.12 9.96 0 1 -17 203.38 9.54 0 -1 -17 196.70 8.87 0 -1 18 173.69 5.65 0 -1 -18 178.82 6.14 0 1 -18 170.37 9.87 0 1 -18 181.64 9.24 0 -1 -18 185.63 8.84 0 1 -19 8.86 2.78 0 -1 -19 5.92 2.20 0 1 -19 5.49 2.52 0 -1 19 4.29 1.10 0 -1 -20 14.94 2.83 0 1 -20 19.60 3.19 0 1 -20 14.33 3.31 0 -1 20 13.44 1.64 0 -1 -21 10.61 2.53 0 1 -21 12.80 2.94 0 1 -21 8.73 2.67 0 -1 21 10.15 1.52 0 1 -22 0.06 1.78 0 -1 -22 -1.46 2.35 0 1 -22 -2.54 2.66 0 1 -23 21.77 3.89 0 -1 -23 19.19 3.44 0 1 -23 15.00 3.25 0 1 -24 9.93 3.35 0 -1 -24 12.15 3.15 0 1 -24 5.77 2.21 0 1 -25 102.40 9.00 0 1 -25 109.57 8.75 0 -1 -25 114.61 8.53 0 -1 -26 52.53 6.02 0 1 -26 65.07 7.10 0 -1 -27 5.39 2.84 0 1 -27 9.37 3.79 0 1 -28 -1.65 2.34 0 -1 -28 0.08 2.47 0 -1 -29 10.65 3.75 0 1 -29 9.36 3.80 0 -1 -30 40.23 6.02 0 1 -30 45.62 6.65 0 -1 -31 61.24 7.43 0 1 -31 62.66 7.94 0 -1 -32 41.21 6.24 0 1 -32 37.60 6.27 0 -1 33 14.54 3.82 0 -1 -33 11.12 3.79 0 1 -33 13.08 3.56 0 -1 34 -2.71 3.43 0 -1 -34 0.32 2.14 0 1 -34 1.01 2.80 0 -1 35 9.20 3.39 0 -1 -35 18.29 4.94 0 -1 36 -1.20 3.45 0 -1 -36 0.69 2.10 0 -1 37 -0.34 2.73 0 -1 -37 -1.43 2.21 0 -1 38 5.43 3.72 0 1 38 -6.25 3.98 0 -1 -38 -4.08 3.44 0 1 39 1.24 1.82 0 -1 39 8.45 3.98 0 -1 -39 1.41 2.11 0 -1 40 7.62 4.10 0 1 40 2.69 2.29 0 1 41 0.97 2.24 0 -2 0 298.32 5.50 0 2 0 297.07 5.27 0 -2 0 270.24 6.28 0 -2 0 282.73 5.68 0 2 0 288.47 5.67 0 -2 1 809.58 9.32 0 -2 -1 809.35 8.97 0 2 1 818.25 8.70 0 2 -1 834.33 9.24 0 -2 -1 812.56 9.88 0 2 1 816.30 9.66 0 2 -1 807.57 9.60 0 -2 -1 804.10 10.90 0 2 1 782.52 10.85 0 2 -1 809.67 11.34 0 2 -2 657.70 8.76 0 2 2 654.44 7.93 0 -2 2 676.58 8.88 0 -2 -2 664.52 9.18 0 2 2 675.41 9.06 0 -2 -2 662.84 9.21 0 -2 -2 649.90 8.16 0 2 2 645.79 10.00 0 -2 -2 652.45 10.01 0 2 2 660.68 7.23 0 -2 2 653.26 10.30 0 2 -2 647.24 10.44 0 -2 3 1669.47 14.81 0 2 -3 1645.40 14.83 0 -2 -3 1719.65 14.97 0 -2 -3 1659.40 15.36 0 2 3 1665.44 15.01 0 -2 -3 1688.09 13.47 0 2 3 1638.21 13.19 0 -2 -3 1656.38 16.51 0 2 3 1636.98 16.78 0 -2 3 1642.37 16.87 0 2 -3 1631.76 17.14 0 -2 -3 1621.09 12.99 0 2 3 1675.36 12.26 0 -2 4 835.88 12.50 0 2 -4 812.22 12.64 0 -2 4 915.57 12.09 0 -2 -4 801.87 9.81 0 -2 -4 852.41 11.03 0 -2 -4 791.83 11.25 0 2 4 830.17 9.90 0 -2 -4 837.34 12.39 0 2 4 817.37 11.11 0 2 4 795.95 12.28 0 -2 4 844.64 11.29 0 2 4 851.93 9.43 0 -2 -4 818.63 9.88 0 2 -5 9688.77 45.62 0 -2 5 9975.77 44.90 0 -2 5 9999.00 42.41 0 -2 -5 9919.35 35.27 0 -2 -5 9734.43 41.31 0 2 5 9591.41 35.83 0 -2 -5 9799.13 44.56 0 2 5 9660.02 44.75 0 -2 -5 9633.45 35.76 0 -2 5 9435.45 40.38 0 -2 6 1473.22 18.18 0 2 -6 1428.03 18.43 0 2 6 1502.06 15.05 0 -2 -6 1524.36 14.74 0 -2 -6 1511.01 15.62 0 -2 -6 1468.35 17.03 0 2 6 1458.27 18.24 0 -2 6 1519.85 17.32 0 2 6 1509.13 14.42 0 -2 -6 1471.74 15.04 0 -2 6 1489.75 16.77 0 2 7 4888.83 28.71 0 -2 -7 5025.19 28.34 0 -2 -7 4948.57 28.43 0 2 7 4937.95 27.87 0 -2 -7 4855.63 29.18 0 2 7 4789.88 34.94 0 2 -7 4915.80 35.31 0 -2 7 4921.43 34.50 0 2 -7 4857.64 32.96 0 -2 7 4955.59 32.88 0 -2 -8 19.79 3.20 0 -2 8 8.05 1.17 0 -2 -8 7.73 1.46 0 -2 -8 6.17 1.21 0 2 8 5.75 1.14 0 -2 8 5.29 1.42 0 2 -8 10.07 2.05 0 2 -8 9.14 2.46 0 2 8 5.04 1.44 0 2 8 6.79 1.42 0 2 -9 241.31 8.60 0 -2 9 244.90 8.39 0 2 9 252.60 7.32 0 -2 -9 255.67 7.15 0 2 -9 263.37 8.35 0 -2 -9 256.73 6.86 0 2 9 254.15 7.17 0 -2 -9 251.20 7.38 0 2 -10 142.60 6.88 0 2 10 143.83 5.70 0 2 -10 146.42 6.57 0 -2 -10 142.42 5.32 0 2 10 141.67 5.84 0 -2 -10 139.97 5.54 0 -2 -11 34.92 2.95 0 -2 -11 33.42 2.71 0 2 -11 38.01 3.74 0 2 -11 43.49 3.79 0 2 11 35.21 3.07 0 -2 -12 80.11 4.65 0 2 -12 93.19 5.99 0 -2 -12 79.06 4.24 0 2 -12 72.70 5.35 0 2 -13 1081.81 19.82 0 -2 -13 1064.08 17.35 0 -2 -13 1052.57 15.39 0 2 -13 1015.29 20.61 0 2 -14 108.80 6.96 0 -2 -14 78.01 5.13 0 -2 -14 83.96 4.57 0 2 -14 79.23 6.12 0 2 -15 337.48 11.98 0 -2 -15 325.75 10.44 0 -2 -15 328.54 9.01 0 2 -15 322.78 12.45 0 2 -16 245.06 10.58 0 -2 -16 227.50 9.04 0 -2 -16 225.44 7.68 0 2 -16 216.27 10.61 0 -2 -17 26.97 2.88 0 2 -17 28.32 4.01 0 -2 -17 31.39 3.74 0 2 -17 27.67 3.93 0 -2 -18 62.76 5.25 0 -2 -18 55.55 4.00 0 2 -18 58.57 5.87 0 2 -18 63.39 5.93 0 -2 -19 153.40 8.11 0 2 -19 154.00 9.13 0 2 -19 137.52 9.25 0 -2 -19 147.59 6.59 0 -2 -20 32.33 3.34 0 2 -20 29.24 4.54 0 -2 -20 34.55 4.40 0 2 -20 40.59 5.24 0 -2 -21 170.42 7.33 0 2 -21 203.74 11.07 0 -2 -21 178.96 9.44 0 2 -21 176.86 11.12 0 -2 -22 223.98 8.48 0 -2 -22 228.05 10.96 0 2 -22 248.28 12.35 0 2 -22 228.22 13.02 0 2 -23 62.82 7.08 0 2 -23 77.89 7.34 0 -2 -23 69.83 6.29 0 2 -24 1.30 2.01 0 2 -24 0.82 2.40 0 -2 -24 0.88 1.87 0 2 -25 31.62 5.44 0 2 -25 36.65 5.74 0 -2 -25 41.12 5.62 0 2 -26 283.71 14.54 0 -2 -26 271.22 13.20 0 2 -26 269.91 15.26 0 2 -27 0.98 2.14 0 2 -27 4.19 3.88 0 -2 -27 5.01 3.89 0 -2 -28 268.09 13.86 0 2 -28 245.84 14.28 0 2 -28 251.92 15.41 0 -2 29 192.57 12.68 0 -2 -29 201.59 12.42 0 2 -29 216.94 13.82 0 2 -29 191.12 13.89 0 2 -30 134.59 11.70 0 -2 30 131.95 10.54 0 2 -30 140.37 11.43 0 -2 -30 127.99 10.09 0 -2 31 70.85 7.92 0 -2 -31 87.57 8.60 0 -2 32 17.98 4.46 0 -2 -32 27.87 5.40 0 -2 33 22.84 4.88 0 -2 -33 23.33 4.66 0 -2 34 2.33 2.47 0 -2 -34 9.41 3.80 0 -2 35 9.40 3.85 0 -2 -35 9.81 3.78 0 -2 36 -0.23 2.42 0 -2 -36 2.25 2.64 0 -2 37 2.38 3.19 0 -2 -37 4.52 2.67 0 -2 38 2.10 2.55 0 -2 -38 2.77 2.40 0 -2 39 -4.87 3.57 0 2 39 -2.38 2.21 0 -2 -39 0.13 1.94 0 2 40 -3.38 3.17 0 -2 -40 4.80 2.76 0 3 0 -0.28 0.52 0 -3 0 1.43 0.61 0 -3 -1 1118.52 14.16 0 -3 -1 1125.29 14.13 0 3 -1 1094.22 13.56 0 -3 1 1176.46 13.75 0 3 1 1105.35 13.55 0 -3 1 1094.59 15.50 0 -3 -1 1107.65 15.60 0 3 1 1113.11 15.46 0 -3 -1 1108.87 13.00 0 -3 1 1090.91 13.25 0 3 -1 1144.89 13.04 0 3 1 1138.59 12.42 0 3 -2 2898.30 21.53 0 -3 2 2801.91 21.83 0 3 2 2844.65 19.62 0 -3 -2 2810.17 22.96 0 -3 -2 2914.93 22.90 0 -3 2 2850.54 20.84 0 3 2 2905.95 22.41 0 -3 -2 2854.45 20.81 0 3 2 2817.06 25.34 0 -3 -2 2900.97 25.49 0 3 2 2863.77 17.61 0 3 -2 2852.13 26.19 0 3 -3 2418.37 20.56 0 3 3 2343.37 18.41 0 -3 3 2333.43 20.50 0 -3 -3 2367.05 21.64 0 -3 3 2382.48 18.62 0 -3 -3 2339.07 21.13 0 3 3 2378.06 20.84 0 -3 -3 2388.84 19.23 0 3 3 2284.49 23.36 0 -3 -3 2309.51 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522.21 11.23 2 -2 -1 548.42 10.32 -2 -2 2 1665.11 16.57 2 -2 -2 1714.98 22.73 2 -2 -2 1655.65 14.63 -2 -2 2 1619.96 22.89 2 -2 -2 1612.56 21.21 2 -2 -2 1651.08 23.25 -2 -2 2 1686.67 11.56 -2 2 -2 1588.88 17.30 -2 2 -2 1675.36 20.84 2 -2 -2 1710.81 17.34 -2 -2 3 566.15 13.55 2 -2 -3 579.52 12.82 2 -2 -3 548.40 13.70 2 -2 -3 577.30 8.04 2 -2 -3 583.15 13.40 -2 -2 3 588.89 10.06 -2 2 -3 572.74 12.78 -2 2 -3 571.52 10.77 2 -2 -4 723.57 8.38 -2 -2 4 728.48 15.39 2 -2 -4 709.52 15.54 -2 2 -4 724.32 14.97 2 -2 -4 732.60 14.62 2 -2 -4 720.98 15.32 -2 -2 4 743.19 11.49 -2 2 -4 746.20 12.81 2 -2 -5 2049.99 13.37 -2 -2 5 1990.15 25.56 2 -2 -5 1976.19 24.42 2 -2 -5 2026.99 26.62 -2 2 -5 1993.56 25.84 2 -2 -5 2020.88 25.87 -2 2 -5 2027.42 22.07 -2 -2 5 1992.18 19.18 -2 -2 6 263.44 9.30 2 -2 -6 267.59 9.30 2 -2 -6 265.25 9.77 2 -2 -6 270.21 4.90 -2 2 -6 255.21 9.70 2 -2 -6 259.26 9.60 -2 -2 6 264.92 7.32 -2 2 -6 257.92 8.38 -2 -2 7 631.46 14.66 -2 2 -7 620.07 15.59 2 -2 -7 642.07 14.35 2 -2 -7 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27.26 8.22 8 -7 -4 7.75 3.83 -8 -7 4 8.54 5.42 8 -7 -5 7.63 4.37 -8 -7 5 3.91 4.06 8 -7 -6 8.45 5.14 -8 -7 6 14.60 6.12 8 -7 -7 11.17 4.74 -8 -7 7 32.53 9.04 8 -7 -8 4.12 4.15 -8 -7 8 10.95 6.08 8 -7 -9 4.59 2.99 -8 -7 9 3.61 3.76 8 -7 -10 6.22 4.22 -8 -7 10 -1.52 4.11 8 -7 -11 -3.70 2.97 8 -7 -12 3.57 3.13 8 -7 -13 0.66 1.94 8 -7 -14 5.47 3.78 -8 7 -15 -3.97 2.63 -8 7 -16 -4.08 3.06 8 -8 9 17.49 5.54 8 -8 8 9.39 4.98 8 -8 7 20.08 6.58 8 -8 6 20.80 7.35 8 -8 5 16.56 6.28 8 -8 4 11.21 5.57 8 -8 3 37.18 7.81 8 -8 2 41.55 8.90 8 -8 1 22.61 7.16 8 -8 0 25.08 7.08 8 -8 -1 20.74 7.25 8 -8 -2 28.14 7.27 8 -8 -3 36.26 8.39 8 -8 -4 12.96 6.37 8 -8 -5 15.22 5.39 8 -8 -6 7.99 4.27 8 -8 -7 24.42 6.38 8 -8 -8 5.68 4.91 -9 0 0 2.36 3.07 -9 0 -1 1.72 2.49 -9 0 1 -0.13 2.69 -9 0 2 6.65 3.26 -9 0 -2 0.13 3.37 -9 0 3 -1.82 2.51 -9 0 3 1.04 1.91 -9 0 -3 -1.48 2.55 9 0 -3 -0.66 3.12 -9 0 4 -1.96 2.65 -9 0 4 -2.99 2.99 -9 0 -4 2.99 3.09 9 0 -4 4.14 4.59 -9 0 5 15.55 5.90 -9 0 -5 15.19 4.73 9 0 -5 16.24 5.52 -9 0 -6 18.04 5.57 9 0 -6 18.10 6.55 -9 0 7 99.97 11.39 -9 0 -7 86.53 10.73 9 0 -7 91.43 12.00 -9 0 -8 9.03 5.36 9 0 -8 3.15 4.80 -9 0 9 3.36 2.67 -9 0 -9 4.30 4.36 9 0 -9 6.49 4.86 -9 0 10 2.38 2.89 -9 0 -10 3.19 3.24 9 0 -10 8.49 4.51 -9 0 11 15.59 5.14 -9 0 -11 9.25 4.10 -9 0 12 1.83 3.06 -9 0 -12 3.27 3.35 -9 0 13 0.99 2.46 -9 0 -13 1.95 3.44 -9 0 14 -1.28 2.39 -9 0 -14 1.37 3.19 -9 0 -15 5.84 4.36 -9 -1 -14 0.16 3.48 -9 1 13 7.49 4.21 -9 -1 -13 -4.09 3.67 -9 1 12 13.35 5.11 -9 -1 -12 13.69 5.06 -9 1 11 2.78 3.36 -9 -1 -11 -8.15 4.01 -9 1 10 1.61 1.96 -9 -1 -10 7.31 4.48 9 1 -10 14.48 5.50 -9 1 9 18.26 5.39 -9 -1 -9 16.64 5.37 9 1 -9 17.52 5.26 -9 1 8 4.66 3.87 -9 -1 -8 9.49 5.10 9 1 -8 3.03 4.64 -9 1 7 7.12 3.96 -9 -1 -7 8.45 4.84 -9 1 6 7.02 3.84 -9 -1 -6 15.09 5.34 -9 1 5 22.98 6.16 -9 -1 -5 21.13 6.26 -9 1 4 8.63 5.77 -9 -1 -4 12.87 4.98 -9 1 3 20.92 5.65 -9 -1 -3 26.14 6.19 9 -1 3 26.44 6.49 -9 -1 -2 5.70 3.64 9 -1 2 3.74 3.83 -9 -1 -1 7.68 3.73 9 -1 1 7.31 3.97 -9 -1 0 4.68 4.01 9 -1 0 -2.44 3.21 -9 -1 1 14.45 5.13 -9 1 -1 15.59 4.87 9 -1 -1 9.10 4.13 -9 -1 2 3.89 3.61 -9 1 -2 2.26 3.18 -9 -1 2 2.98 4.37 9 -1 -2 4.56 3.51 -9 -1 3 25.19 5.78 -9 1 -3 19.85 5.29 -9 -1 3 19.46 5.60 9 -1 -3 30.37 7.09 -9 -1 4 8.84 4.68 -9 -1 4 8.48 4.96 -9 1 -4 4.59 3.80 9 -1 -4 11.11 4.76 -9 -1 5 16.75 5.31 -9 -1 5 19.00 5.33 -9 1 -5 19.19 5.24 9 -1 -5 18.67 6.09 -9 -1 6 8.46 4.31 -9 1 -6 9.68 4.55 -9 -1 6 4.95 3.51 9 -1 -6 11.13 4.79 -9 -1 7 13.64 4.91 -9 1 -7 11.01 4.11 -9 -1 7 10.45 4.28 9 -1 -7 9.33 5.42 -9 -1 8 -1.20 2.04 -9 1 -8 -1.21 2.63 -9 -1 8 11.57 4.94 9 -1 -8 13.15 5.21 -9 -1 9 16.88 5.34 -9 1 -9 20.97 5.40 9 -1 -9 21.01 6.53 -9 -1 10 16.65 5.20 -9 1 -10 15.24 5.30 9 -1 -10 8.24 4.87 -9 -1 11 7.53 3.91 -9 1 -11 7.23 5.07 -9 -1 12 9.90 4.06 -9 1 -12 11.34 4.81 -9 -1 13 2.67 3.38 -9 1 -13 7.61 4.42 -9 -1 14 5.74 3.42 -9 1 -14 -5.25 3.01 -9 -1 15 0.13 1.75 -9 1 -15 2.96 2.88 -9 -1 16 -2.15 2.46 -9 1 -16 -4.20 4.34 9 -2 14 7.37 3.41 -9 -2 -13 0.49 3.02 9 -2 13 -5.40 3.87 -9 -2 -12 -4.40 4.22 9 -2 12 -4.49 3.74 -9 2 11 1.22 3.57 -9 -2 -11 0.32 3.13 9 -2 11 5.91 3.33 -9 2 10 3.81 3.31 -9 -2 -10 10.82 4.74 9 -2 10 9.99 4.09 -9 2 9 12.94 4.88 -9 -2 -9 21.15 6.95 9 -2 9 14.25 5.09 -9 2 8 11.23 4.42 -9 -2 -8 12.10 5.55 9 -2 8 6.11 3.88 -9 2 7 1.21 2.58 -9 -2 -7 2.49 4.02 9 -2 7 -1.41 2.81 -9 2 6 13.04 6.29 -9 -2 -6 14.45 6.36 9 -2 6 7.57 3.95 -9 2 5 33.99 7.58 -9 -2 -5 32.25 7.61 9 -2 5 23.41 6.65 -9 2 4 19.59 5.80 -9 -2 -4 12.88 4.97 9 -2 4 20.89 6.26 -9 -2 -3 13.16 4.86 9 -2 3 13.81 5.52 -9 -2 -2 7.64 4.17 9 -2 2 11.95 5.08 -9 -2 -1 2.14 3.58 9 -2 1 2.23 3.77 -9 -2 0 -0.46 3.03 9 -2 0 4.95 3.72 -9 -2 1 2.43 3.05 -9 -2 1 -3.52 4.26 9 -2 -1 2.24 4.37 -9 -2 2 9.73 4.65 -9 -2 2 6.60 4.36 9 -2 -2 9.94 4.75 -9 -2 3 21.61 5.52 -9 -2 3 16.82 5.47 9 -2 -3 21.41 5.89 -9 -2 4 24.11 5.97 -9 -2 4 9.30 4.80 9 -2 -4 23.62 6.82 -9 -2 5 27.62 6.34 -9 -2 5 24.83 6.31 9 -2 -5 29.21 7.32 -9 -2 6 6.63 2.82 -9 -2 6 10.35 4.94 9 -2 -6 12.08 5.69 -9 -2 7 -7.15 2.71 -9 2 -7 2.87 3.17 -9 -2 7 5.95 4.36 9 -2 -7 -1.94 2.80 -9 -2 8 12.39 4.41 -9 2 -8 10.64 3.84 -9 -2 8 15.31 5.79 9 -2 -8 -2.26 3.68 -9 -2 9 20.12 5.17 -9 2 -9 25.69 6.24 -9 -2 9 13.63 5.37 -9 -2 10 5.33 3.70 -9 2 -10 11.28 4.90 -9 -2 10 9.08 3.99 -9 -2 11 1.27 2.48 -9 2 -11 4.66 2.95 -9 -2 11 5.41 3.54 -9 -2 12 3.18 2.98 -9 2 -12 -1.76 2.16 -9 -2 12 5.13 4.04 -9 -2 13 7.12 3.94 -9 2 -13 -1.65 3.00 -9 2 -14 9.22 4.49 -9 -2 14 9.02 3.65 -9 2 -15 8.86 4.84 -9 -2 15 -2.79 2.52 -9 2 -16 7.27 3.93 -9 -2 16 4.96 2.83 -9 -2 17 -4.38 3.43 9 -3 13 1.49 2.29 9 -3 12 0.45 2.48 -9 -3 -11 10.58 5.48 9 -3 11 4.36 3.57 -9 -3 -10 6.90 4.75 9 -3 10 7.71 4.20 -9 -3 -9 5.32 4.13 9 -3 9 1.06 2.97 -9 -3 -8 9.38 5.17 9 -3 8 6.40 3.89 -9 3 7 18.84 5.84 -9 -3 -7 17.92 5.87 9 -3 7 6.58 3.04 -9 3 6 10.94 5.32 -9 -3 -6 8.54 4.90 9 -3 6 2.61 2.95 -9 3 5 0.48 3.37 -9 -3 -5 6.56 4.66 9 -3 5 0.31 3.19 -9 3 4 2.70 3.43 -9 -3 -4 -0.65 3.62 9 -3 4 -6.33 4.44 -9 -3 -3 17.83 5.56 9 -3 3 14.28 5.08 -9 -3 -2 2.95 3.83 9 -3 2 0.94 2.88 -9 -3 -1 -2.93 4.33 9 -3 1 -3.92 4.69 -9 -3 0 -3.76 3.48 9 -3 0 2.35 3.42 -9 -3 1 -0.16 2.63 9 -3 -1 1.73 3.05 -9 -3 2 0.16 2.44 9 -3 -2 5.18 3.93 -9 -3 3 22.38 6.63 9 -3 -3 14.67 5.16 -9 -3 4 -1.63 4.24 9 -3 -4 -1.43 3.07 -9 -3 5 8.84 4.95 9 -3 -5 0.63 2.59 -9 -3 6 6.38 4.68 9 -3 -6 6.38 4.08 -9 -3 7 11.49 4.80 -9 -3 8 8.57 4.20 -9 -3 9 -1.66 3.62 -9 -3 10 9.33 5.15 -9 -3 11 7.01 4.10 -9 -3 12 2.34 2.23 -9 -3 13 6.73 4.85 -9 3 -13 -0.79 2.67 -9 -3 14 8.11 5.58 -9 3 -14 -0.41 2.85 -9 -3 15 7.14 4.42 -9 3 -15 5.25 3.04 -9 3 -16 2.54 2.85 9 -4 11 7.78 4.07 9 -4 10 9.15 4.29 9 -4 9 13.45 4.90 -9 -4 -8 12.36 5.61 9 -4 8 19.14 5.51 -9 -4 -7 11.84 5.44 9 -4 7 10.08 4.27 -9 -4 -6 -0.17 3.73 9 -4 6 9.85 4.26 -9 -4 -5 13.38 5.62 9 -4 5 3.31 3.35 -9 -4 -4 -0.17 2.54 9 -4 4 -2.25 2.63 -9 -4 -3 2.78 3.09 9 -4 3 1.36 2.62 -9 -4 -2 -2.62 4.01 9 -4 2 -4.57 4.02 -9 -4 -1 2.80 3.94 9 -4 1 -4.60 4.09 -9 -4 0 -3.49 4.52 9 -4 0 1.68 2.84 -9 -4 1 -0.87 3.65 9 -4 -1 1.39 2.56 -9 -4 2 2.26 3.32 9 -4 -2 2.48 3.44 -9 -4 3 3.83 3.51 9 -4 -3 7.29 4.28 -9 -4 4 -1.40 2.81 -9 -4 5 6.48 4.98 -9 -4 6 5.97 4.87 -9 -4 7 6.33 4.55 -9 -4 8 2.65 2.88 -9 -4 9 6.40 4.20 -9 -4 10 3.74 4.23 -9 -4 11 8.41 5.70 -9 -4 12 21.93 6.85 -9 -4 13 20.43 7.56 -9 -4 14 2.72 3.54 9 -5 9 5.95 3.73 9 -5 8 15.45 5.30 9 -5 7 8.37 3.88 9 -5 6 4.07 3.75 9 -5 5 5.96 3.79 9 -5 4 0.59 3.11 9 -5 3 1.63 3.36 -9 -5 -2 -2.04 3.08 9 -5 2 4.18 5.09 -9 -5 -1 7.78 4.70 9 -5 1 21.37 6.28 -9 -5 0 7.22 5.61 -9 -5 1 19.42 6.85 -9 -5 2 2.59 4.88 -9 -5 3 12.61 5.46 -9 -5 4 0.37 3.45 -9 -5 5 6.54 4.51 -9 -5 6 5.06 5.35 -9 -5 7 8.46 4.81 9 -6 8 13.56 4.84 -10 0 -5 7.12 4.51 -10 0 -6 12.00 4.74 -10 -1 -3 14.03 6.41 -10 -1 -2 15.33 5.33 -10 -1 -1 3.96 4.32 -10 -1 0 4.59 3.47 -10 -2 3 -0.17 3.01 -10 -2 4 0.68 2.24 -10 -2 5 3.93 3.82 0 0 0 0.00 0.00 TITL mm_newset in P2(1)2(1)2 REM P2(1)2(1)2 (#18 in standard setting) CELL 0.71073 7.300913 11.055154 30.005681 90.0000 90.0000 90.0000 ZERR 4.00 0.000793 0.001139 0.003325 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM -x+1/2, y+1/2,-z SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 120.00 116.00 4.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1037 _shelx_res_file ; TITL $orthorhombic $P 21 21 21 $? $colourless $ mm_newset.res created by SHELXL-2018/3 at 19:47:46 on 20-Jul-2019 CELL 0.71073 7.3009 11.0552 30.0057 90 90 90 ZERR 4 0.0008 0.0011 0.0033 0 0 0 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, -Z SYMM -X, 0.5+Y, 0.5-Z SFAC C N O H UNIT 120 4 4 116 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 6 REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.132, Rweak 0.040, Alpha 0.002, Orientation as input REM Flack x = -0.280 ( 0.566 ) from Parsons' quotients REM Formula found by SHELXT: C29 C8 O fmap 2 OMIT 0 1 2 OMIT 0 1 1 MORE -1 BOND $H ACTA CONF REM D:\data\2019\07\pascal_kccd\KARIM032\KARIM032\sfrm\struct\olex2_mm_ne REM wset\mm_newset.hkl SHEL 999 0.83 EQIV $1 -x,1/2+y,1/2-z HTAB O19 N2 HTAB C27 O19 HTAB C6 O19_$1 TWIN WGHT 0.030400 0.332100 EXTI 0.013914 BASF -0.10886 FVAR 0.78382 C1 1 0.328630 -0.001498 0.217656 11.00000 0.05624 0.03881 = 0.04256 0.00381 0.00676 -0.00484 AFIX 23 H1A 4 0.428447 -0.038350 0.234113 11.00000 -1.15000 H1B 4 0.243483 -0.065133 0.209524 11.00000 -1.15000 AFIX 0 N2 2 0.401901 0.053517 0.176891 11.00000 0.03614 0.03360 = 0.03687 0.00008 0.00579 -0.00080 C3 1 0.502710 0.165522 0.187410 11.00000 0.03845 0.03909 = 0.04258 -0.00030 0.00392 -0.00368 AFIX 13 H3 4 0.556815 0.195001 0.159563 11.00000 -1.15000 AFIX 0 C4 1 0.361610 0.260230 0.202711 11.00000 0.04191 0.03216 = 0.03951 -0.00374 0.00056 -0.00589 AFIX 13 H4 4 0.430488 0.329448 0.214349 11.00000 -1.15000 AFIX 0 C5 1 0.154668 0.289074 0.269310 11.00000 0.04408 0.05362 = 0.04367 -0.00782 -0.00426 0.00378 AFIX 43 H5 4 0.162708 0.372208 0.264993 11.00000 -1.15000 AFIX 0 C6 1 0.050734 0.244678 0.304069 11.00000 0.04210 0.08264 = 0.04129 -0.01267 0.00045 0.00742 AFIX 43 H6 4 -0.009196 0.297836 0.323159 11.00000 -1.15000 AFIX 0 C7 1 0.035715 0.122188 0.310496 11.00000 0.04821 0.08503 = 0.03945 0.00147 0.00643 -0.00758 AFIX 43 H7 4 -0.035474 0.092057 0.333677 11.00000 -1.15000 AFIX 0 C8 1 0.126535 0.044336 0.282461 11.00000 0.05515 0.05960 = 0.04063 0.00357 0.00309 -0.01263 AFIX 43 H8 4 0.116921 -0.038604 0.287084 11.00000 -1.15000 AFIX 0 C9 1 0.232797 0.087146 0.247229 11.00000 0.04227 0.04725 = 0.03200 0.00019 0.00104 -0.00296 C10 1 0.247851 0.211405 0.240547 11.00000 0.03638 0.04421 = 0.03423 -0.00304 -0.00185 0.00019 C11 1 0.658851 0.150244 0.221006 11.00000 0.04333 0.05889 = 0.06802 -0.00637 -0.00808 -0.00144 AFIX 137 H11A 4 0.726198 0.224575 0.223262 11.00000 -1.20000 H11B 4 0.739191 0.086877 0.211187 11.00000 -1.20000 H11C 4 0.609065 0.129700 0.249634 11.00000 -1.20000 AFIX 0 C12 1 0.249156 0.305714 0.163720 11.00000 0.04944 0.03190 = 0.03868 -0.00365 0.00682 0.00434 C13 1 0.319491 0.395550 0.136734 11.00000 0.06528 0.04700 = 0.05864 0.00848 0.00742 -0.00244 AFIX 43 H13 4 0.431991 0.430129 0.143737 11.00000 -1.15000 AFIX 0 C14 1 0.225438 0.434975 0.099463 11.00000 0.09272 0.06367 = 0.05577 0.02031 0.01226 0.00996 AFIX 43 H14 4 0.275393 0.495164 0.081543 11.00000 -1.15000 AFIX 0 C15 1 0.059331 0.385783 0.088877 11.00000 0.09053 0.07662 = 0.04255 0.00371 -0.00200 0.03309 AFIX 43 H15 4 -0.003927 0.412441 0.063832 11.00000 -1.15000 AFIX 0 C16 1 -0.013797 0.296714 0.115425 11.00000 0.05892 0.07372 = 0.05436 -0.01078 -0.00777 0.01106 AFIX 43 H16 4 -0.126869 0.262995 0.108399 11.00000 -1.15000 AFIX 0 C17 1 0.080886 0.257326 0.152568 11.00000 0.05260 0.04848 = 0.04517 0.00126 -0.00086 0.00239 AFIX 43 H17 4 0.030362 0.197119 0.170385 11.00000 -1.15000 AFIX 0 C18 1 0.503206 -0.034773 0.149467 11.00000 0.03358 0.03909 = 0.03755 0.00102 -0.00156 0.00337 AFIX 13 H18 4 0.600714 -0.070012 0.167776 11.00000 -1.15000 AFIX 0 C19 1 0.368389 -0.137404 0.136095 11.00000 0.03959 0.03904 = 0.04628 -0.00086 -0.00057 0.00034 AFIX 13 H19 4 0.338016 -0.182861 0.163143 11.00000 -1.15000 AFIX 0 O19 3 0.204621 -0.087653 0.119335 11.00000 0.04137 0.05509 = 0.07153 -0.00693 -0.00921 0.00367 HOH 4 0.197817 -0.016387 0.130727 11.00000 -1.20000 C20 1 0.589615 0.021108 0.108552 11.00000 0.04146 0.04026 = 0.03639 -0.00416 0.00153 -0.00095 C21 1 0.494250 0.099669 0.080940 11.00000 0.06172 0.05946 = 0.04478 0.00490 0.00151 0.00466 AFIX 43 H21 4 0.377223 0.125320 0.088719 11.00000 -1.15000 AFIX 0 C22 1 0.574230 0.139836 0.041649 11.00000 0.09705 0.07517 = 0.04674 0.01287 -0.00257 -0.00387 AFIX 43 H22 4 0.510686 0.192712 0.023154 11.00000 -1.15000 AFIX 0 C23 1 0.746717 0.101824 0.029986 11.00000 0.09498 0.09148 = 0.04688 -0.00424 0.02442 -0.02406 AFIX 43 H23 4 0.798359 0.127746 0.003312 11.00000 -1.15000 AFIX 0 C24 1 0.842838 0.026252 0.057289 11.00000 0.06215 0.08179 = 0.06159 -0.01758 0.02092 -0.01385 AFIX 43 H24 4 0.960600 0.001927 0.049589 11.00000 -1.15000 AFIX 0 C25 1 0.764398 -0.013703 0.096270 11.00000 0.04519 0.05324 = 0.05217 -0.00901 0.00728 -0.00348 AFIX 43 H25 4 0.830335 -0.065258 0.114775 11.00000 -1.15000 AFIX 0 C26 1 0.452303 -0.224701 0.103326 11.00000 0.04564 0.03840 = 0.04611 -0.00461 -0.00118 -0.00546 C27 1 0.414959 -0.219668 0.058428 11.00000 0.08603 0.05769 = 0.05069 -0.00599 -0.01306 0.01025 AFIX 43 H27 4 0.330932 -0.163529 0.047712 11.00000 -1.15000 AFIX 0 C28 1 0.501331 -0.297369 0.029146 11.00000 0.12155 0.07566 = 0.04773 -0.01582 -0.00088 0.00747 AFIX 43 H28 4 0.474735 -0.293390 -0.001130 11.00000 -1.15000 AFIX 0 C29 1 0.625152 -0.379754 0.044308 11.00000 0.09542 0.06223 = 0.07818 -0.02392 0.02159 0.00706 AFIX 43 H29 4 0.684240 -0.431168 0.024431 11.00000 -1.15000 AFIX 0 C30 1 0.662155 -0.386507 0.088868 11.00000 0.06904 0.05683 = 0.08191 -0.01510 0.00106 0.01367 AFIX 43 H30 4 0.746120 -0.442975 0.099374 11.00000 -1.15000 AFIX 0 C31 1 0.575175 -0.309684 0.118347 11.00000 0.05815 0.04531 = 0.05633 -0.00658 -0.00495 0.00579 AFIX 43 H31 4 0.599963 -0.315488 0.148673 11.00000 -1.15000 AFIX 0 HKLF 4 REM $orthorhombic $P 21 21 21 $? $colourless $ REM wR2 = 0.0828, GooF = S = 1.072, Restrained GooF = 1.072 for all data REM R1 = 0.0379 for 3948 Fo > 4sig(Fo) and 0.0443 for all 4425 data REM 295 parameters refined using 0 restraints END WGHT 0.0304 0.3320 REM Highest difference peak 0.105, deepest hole -0.110, 1-sigma level 0.024 Q1 1 0.3190 0.1416 0.2559 11.00000 0.05 0.11 Q2 1 0.0063 0.3205 0.3370 11.00000 0.05 0.10 Q3 1 0.4349 0.2124 0.1960 11.00000 0.05 0.10 Q4 1 0.7402 -0.0250 -0.0160 11.00000 0.05 0.09 Q5 1 0.3178 0.0844 0.1558 11.00000 0.05 0.09 Q6 1 0.2014 0.1425 0.2343 11.00000 0.05 0.09 Q7 1 0.5362 0.0737 0.2584 11.00000 0.05 0.09 Q8 1 0.2494 0.1556 0.2391 11.00000 0.05 0.09 Q9 1 -0.0238 0.2186 0.1996 11.00000 0.05 0.09 Q10 1 0.5153 0.0250 0.0870 11.00000 0.05 0.08 Q11 1 0.2446 -0.0706 0.0885 11.00000 0.05 0.08 Q12 1 0.2613 0.0574 0.2712 11.00000 0.05 0.08 Q13 1 0.5381 -0.2377 -0.0070 11.00000 0.05 0.08 Q14 1 -0.1932 0.1628 0.0950 11.00000 0.05 0.08 Q15 1 0.2326 -0.0114 0.1002 11.00000 0.05 0.08 Q16 1 -0.0672 0.3758 0.3198 11.00000 0.05 0.08 Q17 1 0.5370 0.0027 0.1273 11.00000 0.05 0.08 Q18 1 0.1966 0.2618 0.1470 11.00000 0.05 0.08 Q19 1 0.1495 0.2669 0.2918 11.00000 0.05 0.08 Q20 1 0.5771 -0.2142 0.1044 11.00000 0.05 0.08 ; _shelx_res_checksum 6060 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -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 C C1 0.3286(4) -0.0015(2) 0.21766(7) 0.0459(6) Uani d 1 H H1A 0.428447 -0.038350 0.234113 0.053 Uiso calc 1 H H1B 0.243483 -0.065133 0.209524 0.053 Uiso calc 1 N N2 0.4019(2) 0.05352(14) 0.17689(6) 0.0355(4) Uani d 1 C C3 0.5027(3) 0.16552(19) 0.18741(7) 0.0400(5) Uani d 1 H H3 0.556815 0.195001 0.159563 0.046 Uiso calc 1 C C4 0.3616(3) 0.26023(18) 0.20271(7) 0.0379(5) Uani d 1 H H4 0.430488 0.329448 0.214349 0.044 Uiso calc 1 C C5 0.1547(3) 0.2891(2) 0.26931(7) 0.0471(6) Uani d 1 H H5 0.162708 0.372208 0.264993 0.054 Uiso calc 1 C C6 0.0507(3) 0.2447(3) 0.30407(8) 0.0553(7) Uani d 1 H H6 -0.009196 0.297836 0.323159 0.064 Uiso calc 1 C C7 0.0357(4) 0.1222(3) 0.31050(8) 0.0576(7) Uani d 1 H H7 -0.035474 0.092057 0.333677 0.066 Uiso calc 1 C C8 0.1265(3) 0.0443(2) 0.28246(8) 0.0518(6) Uani d 1 H H8 0.116921 -0.038604 0.287084 0.060 Uiso calc 1 C C9 0.2328(3) 0.0871(2) 0.24723(7) 0.0405(5) Uani d 1 C C10 0.2479(3) 0.2114(2) 0.24055(7) 0.0383(5) Uani d 1 C C11 0.6589(3) 0.1502(2) 0.22101(9) 0.0567(7) Uani d 1 H H11A 0.726198 0.224575 0.223262 0.068 Uiso calc 1 H H11B 0.739191 0.086877 0.211187 0.068 Uiso calc 1 H H11C 0.609065 0.129700 0.249634 0.068 Uiso calc 1 C C12 0.2492(3) 0.30571(18) 0.16372(7) 0.0400(5) Uani d 1 C C13 0.3195(4) 0.3956(2) 0.13673(8) 0.0570(7) Uani d 1 H H13 0.431991 0.430129 0.143737 0.066 Uiso calc 1 C C14 0.2254(5) 0.4350(3) 0.09946(9) 0.0707(9) Uani d 1 H H14 0.275393 0.495164 0.081543 0.081 Uiso calc 1 C C15 0.0593(5) 0.3858(3) 0.08888(9) 0.0699(9) Uani d 1 H H15 -0.003927 0.412441 0.063832 0.080 Uiso calc 1 C C16 -0.0138(4) 0.2967(3) 0.11542(9) 0.0623(7) Uani d 1 H H16 -0.126869 0.262995 0.108399 0.072 Uiso calc 1 C C17 0.0809(3) 0.2573(2) 0.15257(8) 0.0488(6) Uani d 1 H H17 0.030362 0.197119 0.170385 0.056 Uiso calc 1 C C18 0.5032(3) -0.03477(18) 0.14947(7) 0.0367(5) Uani d 1 H H18 0.600714 -0.070012 0.167776 0.042 Uiso calc 1 C C19 0.3684(3) -0.13740(19) 0.13610(8) 0.0416(5) Uani d 1 H H19 0.338016 -0.182861 0.163143 0.048 Uiso calc 1 O O19 0.2046(2) -0.08765(16) 0.11933(6) 0.0560(5) Uani d 1 H HOH 0.198(4) -0.016(3) 0.1307(9) 0.067 Uiso d 1 C C20 0.5896(3) 0.02111(19) 0.10855(7) 0.0394(5) Uani d 1 C C21 0.4942(4) 0.0997(2) 0.08094(8) 0.0553(7) Uani d 1 H H21 0.377223 0.125320 0.088719 0.064 Uiso calc 1 C C22 0.5742(5) 0.1398(3) 0.04165(9) 0.0730(8) Uani d 1 H H22 0.510686 0.192712 0.023154 0.084 Uiso calc 1 C C23 0.7467(5) 0.1018(3) 0.02999(10) 0.0778(10) Uani d 1 H H23 0.798359 0.127746 0.003312 0.089 Uiso calc 1 C C24 0.8428(4) 0.0263(3) 0.05729(10) 0.0685(8) Uani d 1 H H24 0.960600 0.001927 0.049589 0.079 Uiso calc 1 C C25 0.7644(3) -0.0137(2) 0.09627(8) 0.0502(6) Uani d 1 H H25 0.830335 -0.065258 0.114775 0.058 Uiso calc 1 C C26 0.4523(3) -0.22470(19) 0.10333(7) 0.0434(5) Uani d 1 C C27 0.4150(4) -0.2197(2) 0.05843(9) 0.0648(8) Uani d 1 H H27 0.330932 -0.163529 0.047712 0.075 Uiso calc 1 C C28 0.5013(5) -0.2974(3) 0.02915(9) 0.0816(10) Uani d 1 H H28 0.474735 -0.293390 -0.001130 0.094 Uiso calc 1 C C29 0.6252(5) -0.3798(3) 0.04431(11) 0.0786(9) Uani d 1 H H29 0.684240 -0.431168 0.024431 0.090 Uiso calc 1 C C30 0.6622(4) -0.3865(2) 0.08887(11) 0.0693(8) Uani d 1 H H30 0.746120 -0.442975 0.099374 0.080 Uiso calc 1 C C31 0.5752(4) -0.3097(2) 0.11835(9) 0.0533(6) Uani d 1 H H31 0.599963 -0.315488 0.148673 0.061 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 C1 0.0562(15) 0.0388(12) 0.0426(13) -0.0048(11) 0.0068(11) 0.0038(10) N2 0.0361(10) 0.0336(8) 0.0369(9) -0.0008(8) 0.0058(8) 0.0001(7) C3 0.0384(12) 0.0391(11) 0.0426(12) -0.0037(10) 0.0039(10) -0.0003(9) C4 0.0419(13) 0.0322(10) 0.0395(12) -0.0059(10) 0.0006(10) -0.0037(9) C5 0.0441(13) 0.0536(14) 0.0437(13) 0.0038(11) -0.0043(11) -0.0078(11) C6 0.0421(14) 0.0826(19) 0.0413(13) 0.0074(14) 0.0005(11) -0.0127(13) C7 0.0482(15) 0.0850(19) 0.0395(13) -0.0076(14) 0.0064(12) 0.0015(13) C8 0.0552(15) 0.0596(14) 0.0406(13) -0.0126(13) 0.0031(12) 0.0036(11) C9 0.0423(13) 0.0472(12) 0.0320(11) -0.0030(11) 0.0010(10) 0.0002(9) C10 0.0364(12) 0.0442(12) 0.0342(11) 0.0002(10) -0.0019(10) -0.0030(9) C11 0.0433(14) 0.0589(15) 0.0680(17) -0.0014(12) -0.0081(13) -0.0064(13) C12 0.0494(14) 0.0319(10) 0.0387(12) 0.0043(11) 0.0068(10) -0.0036(9) C13 0.0653(17) 0.0470(13) 0.0586(16) -0.0024(13) 0.0074(14) 0.0085(12) C14 0.093(2) 0.0637(17) 0.0558(17) 0.0100(18) 0.0123(17) 0.0203(14) C15 0.091(2) 0.0766(19) 0.0426(15) 0.0331(19) -0.0020(15) 0.0037(14) C16 0.0589(16) 0.0737(17) 0.0544(16) 0.0111(15) -0.0078(14) -0.0108(14) C17 0.0526(15) 0.0485(13) 0.0452(13) 0.0024(12) -0.0009(11) 0.0013(11) C18 0.0336(11) 0.0391(11) 0.0375(11) 0.0034(10) -0.0016(10) 0.0010(9) C19 0.0396(12) 0.0390(11) 0.0463(13) 0.0003(10) -0.0006(10) -0.0009(10) O19 0.0414(9) 0.0551(10) 0.0715(12) 0.0037(8) -0.0092(9) -0.0069(9) C20 0.0415(13) 0.0403(11) 0.0364(12) -0.0010(10) 0.0015(10) -0.0042(9) C21 0.0617(17) 0.0595(14) 0.0448(14) 0.0047(14) 0.0015(12) 0.0049(12) C22 0.097(2) 0.0752(19) 0.0467(15) -0.0039(19) -0.0026(17) 0.0129(14) C23 0.095(3) 0.091(2) 0.0469(16) -0.024(2) 0.0244(17) -0.0042(16) C24 0.0622(18) 0.082(2) 0.0616(18) -0.0138(17) 0.0209(15) -0.0176(16) C25 0.0452(14) 0.0532(14) 0.0522(15) -0.0035(12) 0.0073(11) -0.0090(11) C26 0.0456(14) 0.0384(11) 0.0461(13) -0.0055(11) -0.0012(11) -0.0046(10) C27 0.086(2) 0.0577(15) 0.0507(16) 0.0103(16) -0.0131(15) -0.0060(12) C28 0.122(3) 0.076(2) 0.0477(16) 0.007(2) -0.0009(18) -0.0158(15) C29 0.095(2) 0.0622(18) 0.078(2) 0.0071(19) 0.0216(19) -0.0239(16) C30 0.069(2) 0.0568(16) 0.082(2) 0.0137(15) 0.0011(17) -0.0151(15) C31 0.0581(16) 0.0453(12) 0.0563(15) 0.0058(12) -0.0049(13) -0.0066(11) 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' 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' H H 0.0000 0.0000 '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 N2 C1 C9 113.18(17) N2 C1 H1A 108.9 C9 C1 H1A 108.9 N2 C1 H1B 108.9 C9 C1 H1B 108.9 H1A C1 H1B 107.8 C1 N2 C3 110.59(16) C1 N2 C18 111.93(16) C3 N2 C18 115.13(16) N2 C3 C11 114.83(18) N2 C3 C4 107.52(17) C11 C3 C4 112.15(18) N2 C3 H3 107.3 C11 C3 H3 107.3 C4 C3 H3 107.3 C10 C4 C12 113.71(18) C10 C4 C3 110.49(17) C12 C4 C3 110.99(17) C10 C4 H4 107.1 C12 C4 H4 107.1 C3 C4 H4 107.1 C6 C5 C10 121.1(2) C6 C5 H5 119.4 C10 C5 H5 119.4 C7 C6 C5 120.1(2) C7 C6 H6 120.0 C5 C6 H6 120.0 C6 C7 C8 119.6(2) C6 C7 H7 120.2 C8 C7 H7 120.2 C7 C8 C9 121.3(2) C7 C8 H8 119.3 C9 C8 H8 119.3 C10 C9 C8 119.2(2) C10 C9 C1 121.60(19) C8 C9 C1 119.2(2) C9 C10 C5 118.7(2) C9 C10 C4 120.36(19) C5 C10 C4 121.0(2) C3 C11 H11A 109.5 C3 C11 H11B 109.5 H11A C11 H11B 109.5 C3 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C13 C12 C17 117.9(2) C13 C12 C4 119.3(2) C17 C12 C4 122.7(2) C12 C13 C14 121.1(3) C12 C13 H13 119.5 C14 C13 H13 119.5 C15 C14 C13 120.2(3) C15 C14 H14 119.9 C13 C14 H14 119.9 C14 C15 C16 119.7(3) C14 C15 H15 120.2 C16 C15 H15 120.2 C15 C16 C17 119.9(3) C15 C16 H16 120.0 C17 C16 H16 120.0 C12 C17 C16 121.2(2) C12 C17 H17 119.4 C16 C17 H17 119.4 N2 C18 C20 113.06(16) N2 C18 C19 108.02(16) C20 C18 C19 110.66(17) N2 C18 H18 108.3 C20 C18 H18 108.3 C19 C18 H18 108.3 O19 C19 C26 111.22(19) O19 C19 C18 110.15(17) C26 C19 C18 112.22(18) O19 C19 H19 107.7 C26 C19 H19 107.7 C18 C19 H19 107.7 C19 O19 HOH 105(2) C25 C20 C21 118.6(2) C25 C20 C18 119.2(2) C21 C20 C18 122.1(2) C20 C21 C22 119.7(3) C20 C21 H21 120.1 C22 C21 H21 120.1 C23 C22 C21 120.3(3) C23 C22 H22 119.9 C21 C22 H22 119.9 C24 C23 C22 120.4(3) C24 C23 H23 119.8 C22 C23 H23 119.8 C23 C24 C25 119.5(3) C23 C24 H24 120.2 C25 C24 H24 120.2 C24 C25 C20 121.4(3) C24 C25 H25 119.3 C20 C25 H25 119.3 C31 C26 C27 118.6(2) C31 C26 C19 119.3(2) C27 C26 C19 122.2(2) C26 C27 C28 120.5(3) C26 C27 H27 119.8 C28 C27 H27 119.8 C29 C28 C27 120.4(3) C29 C28 H28 119.8 C27 C28 H28 119.8 C28 C29 C30 119.7(3) C28 C29 H29 120.2 C30 C29 H29 120.2 C29 C30 C31 120.2(3) C29 C30 H30 119.9 C31 C30 H30 119.9 C26 C31 C30 120.7(3) C26 C31 H31 119.7 C30 C31 H31 119.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N2 1.467(3) C1 C9 1.496(3) C1 H1A 0.9700 C1 H1B 0.9700 N2 C3 1.475(3) N2 C18 1.475(3) C3 C11 1.531(3) C3 C4 1.539(3) C3 H3 0.9800 C4 C10 1.507(3) C4 C12 1.515(3) C4 H4 0.9800 C5 C6 1.380(3) C5 C10 1.395(3) C5 H5 0.9300 C6 C7 1.372(4) C6 H6 0.9300 C7 C8 1.374(4) C7 H7 0.9300 C8 C9 1.394(3) C8 H8 0.9300 C9 C10 1.393(3) C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 C12 C13 1.380(3) C12 C17 1.381(3) C13 C14 1.383(4) C13 H13 0.9300 C14 C15 1.367(4) C14 H14 0.9300 C15 C16 1.374(4) C15 H15 0.9300 C16 C17 1.382(3) C16 H16 0.9300 C17 H17 0.9300 C18 C20 1.512(3) C18 C19 1.555(3) C18 H18 0.9800 C19 O19 1.409(3) C19 C26 1.508(3) C19 H19 0.9800 O19 HOH 0.86(3) C20 C25 1.383(3) C20 C21 1.388(3) C21 C22 1.389(4) C21 H21 0.9300 C22 C23 1.373(4) C22 H22 0.9300 C23 C24 1.364(4) C23 H23 0.9300 C24 C25 1.375(4) C24 H24 0.9300 C25 H25 0.9300 C26 C31 1.375(3) C26 C27 1.376(3) C27 C28 1.381(4) C27 H27 0.9300 C28 C29 1.362(4) C28 H28 0.9300 C29 C30 1.366(4) C29 H29 0.9300 C30 C31 1.381(4) C30 H30 0.9300 C31 H31 0.9300 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 O19 HOH N2 . 0.86(3) 2.18(3) 2.737(2) 123(2) yes C27 H27 O19 . 0.93 2.48 2.798(3) 99.9 yes C21 H21 Cg3 . 0.93 3.14 3.930(4) 144 yes C6 H6 O19 4 0.93 2.57 3.492(3) 170.1 yes C14 H14 Cg5 1_565 0.93 2.95 3.770(4) 147 yes C16 H16 Cg4 1_455 0.93 2.92 3.743(3) 148 yes C31 H31 Cg2 4_645 0.93 2.96 3.803(3) 152 yes 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 C9 C1 N2 C3 47.4(2) C9 C1 N2 C18 177.26(19) C1 N2 C3 C11 56.3(2) C18 N2 C3 C11 -71.7(2) C1 N2 C3 C4 -69.2(2) C18 N2 C3 C4 162.68(16) N2 C3 C4 C10 54.4(2) C11 C3 C4 C10 -72.8(2) N2 C3 C4 C12 -72.7(2) C11 C3 C4 C12 160.16(19) C10 C5 C6 C7 -0.8(4) C5 C6 C7 C8 0.8(4) C6 C7 C8 C9 -0.6(4) C7 C8 C9 C10 0.4(4) C7 C8 C9 C1 -179.9(2) N2 C1 C9 C10 -12.7(3) N2 C1 C9 C8 167.7(2) C8 C9 C10 C5 -0.4(3) C1 C9 C10 C5 179.9(2) C8 C9 C10 C4 -179.9(2) C1 C9 C10 C4 0.4(3) C6 C5 C10 C9 0.6(3) C6 C5 C10 C4 -179.8(2) C12 C4 C10 C9 104.1(2) C3 C4 C10 C9 -21.5(3) C12 C4 C10 C5 -75.4(2) C3 C4 C10 C5 159.02(19) C10 C4 C12 C13 152.5(2) C3 C4 C12 C13 -82.2(2) C10 C4 C12 C17 -30.5(3) C3 C4 C12 C17 94.8(2) C17 C12 C13 C14 -0.7(4) C4 C12 C13 C14 176.5(2) C12 C13 C14 C15 0.5(4) C13 C14 C15 C16 -0.1(4) C14 C15 C16 C17 -0.1(4) C13 C12 C17 C16 0.5(3) C4 C12 C17 C16 -176.6(2) C15 C16 C17 C12 -0.1(4) C1 N2 C18 C20 -176.66(18) C3 N2 C18 C20 -49.2(2) C1 N2 C18 C19 60.5(2) C3 N2 C18 C19 -172.04(17) N2 C18 C19 O19 48.5(2) C20 C18 C19 O19 -75.7(2) N2 C18 C19 C26 173.03(17) C20 C18 C19 C26 48.8(2) N2 C18 C20 C25 138.8(2) C19 C18 C20 C25 -99.9(2) N2 C18 C20 C21 -46.1(3) C19 C18 C20 C21 75.2(2) C25 C20 C21 C22 1.0(4) C18 C20 C21 C22 -174.2(2) C20 C21 C22 C23 0.2(4) C21 C22 C23 C24 -1.4(5) C22 C23 C24 C25 1.3(4) C23 C24 C25 C20 -0.1(4) C21 C20 C25 C24 -1.1(3) C18 C20 C25 C24 174.2(2) O19 C19 C26 C31 -159.3(2) C18 C19 C26 C31 76.8(3) O19 C19 C26 C27 23.1(3) C18 C19 C26 C27 -100.8(3) C31 C26 C27 C28 -0.9(4) C19 C26 C27 C28 176.8(3) C26 C27 C28 C29 -0.2(5) C27 C28 C29 C30 0.9(5) C28 C29 C30 C31 -0.4(5) C27 C26 C31 C30 1.4(4) C19 C26 C31 C30 -176.4(2) C29 C30 C31 C26 -0.8(4) _cod_database_fobs_code 2021760