#------------------------------------------------------------------------------ #$Date: 2021-05-29 08:15:26 +0300 (Sat, 29 May 2021) $ #$Revision: 265611 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243842.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_2243842 loop_ _publ_author_name 'Miyamoto, Hisakazu' 'Takahashi, Hiroki' _publ_section_title ; Crystal structure and photoreactive behaviour of N,N-diisopropyl(p-phenylphenyl)glyoxylamide ; _journal_coeditor_code DJ2024 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 653 _journal_page_last 657 _journal_paper_doi 10.1107/S2056989021005387 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C20 H23 N O2' _chemical_formula_moiety 'C20 H23 N O2' _chemical_formula_sum 'C20 H23 N O2' _chemical_formula_weight 309.39 _chemical_name_common ; N,N-Diisopropyl(p-phenylphenyl)glyoxylamide ; _chemical_name_systematic ; 2-([1,1'-Biphenyl]-4-yl)-2-oxo-N,N-bis(propan-2-yl)acetamide ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 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 6.1313(2) _cell_length_b 7.3710(2) _cell_length_c 38.1143(11) _cell_measurement_reflns_used 2939 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.4 _cell_volume 1722.53(9) _computing_cell_refinement ; CrystalClear-SM Expert (Rigaku, 2009) ; _computing_data_collection ; CrystalClear-SM Expert (Rigaku, 2009) ; _computing_data_reduction ; CrystalClear-SM Expert (Rigaku, 2009) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type 'Rigaku Saturn 724+ CCD' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_unetI/netI 0.0180 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_number 16094 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.965 _diffrn_reflns_theta_min 3.365 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.985 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; (CrystalClear-SM Expert; Rigaku, 2009) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.193 _exptl_crystal_description Prism _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.290 _refine_diff_density_max 0.164 _refine_diff_density_min -0.146 _refine_ls_abs_structure_details ; Flack x determined using 1346 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.1(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 3877 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0361 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.3778P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.0803 _reflns_number_gt 3614 _reflns_number_total 3877 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dj2024sup1.cif _cod_data_source_block I _cod_database_code 2243842 _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 0.977 _shelx_estimated_absorpt_t_max 0.978 _shelx_hkl_file ; 0 0 -9 14.17 2.13 0 0 -9 14.64 2.23 0 0 -9 15.63 2.27 0 0 -10 270.43 4.94 0 0 -10 253.40 4.74 0 0 -10 268.73 4.90 0 0 -11 0.14 1.28 0 0 -11 2.09 1.45 0 0 -11 1.09 1.49 0 0 -12 205.27 4.76 0 0 -12 213.04 4.70 0 0 -12 222.14 4.83 0 0 -13 1.22 1.41 0 0 -13 2.04 1.49 0 0 -13 -0.22 1.41 0 0 -14 19.27 2.02 0 0 -14 21.12 2.11 0 0 -14 22.29 2.13 0 0 -15 2.01 1.62 0 0 -15 2.21 1.64 0 0 -15 3.33 1.64 0 0 -16 779.19 10.48 0 0 -16 817.53 10.33 0 0 -16 802.71 10.42 0 0 -17 5.26 1.98 0 0 -17 1.28 1.72 0 0 -17 5.69 2.00 0 0 -18 32.96 2.72 0 0 -18 30.01 2.71 0 0 -18 35.26 2.96 0 0 -19 4.91 2.31 0 0 -19 2.59 2.22 0 0 -20 1303.02 14.64 0 0 -20 1281.77 14.75 0 0 -21 11.67 2.69 0 0 -21 13.26 2.77 0 0 -22 663.83 11.12 0 0 -22 685.03 11.40 0 0 -23 5.12 2.69 0 0 -23 5.17 2.49 0 0 -24 802.56 12.81 0 0 -24 794.12 12.96 0 0 -25 9.58 2.80 0 0 -25 4.86 2.56 0 0 -26 33.97 3.58 0 0 -26 26.48 3.26 0 0 -27 77.04 5.62 0 0 -27 67.36 5.17 0 0 -28 7046.95 41.40 0 0 -28 7104.60 41.16 0 0 -29 139.49 7.33 0 0 -29 123.57 7.05 0 0 -30 4256.84 33.48 0 0 -30 4411.59 33.81 0 0 -31 73.60 5.96 0 0 -31 84.41 6.34 0 0 -32 1981.37 23.79 0 0 -32 1822.72 22.66 0 0 -33 44.44 5.16 0 0 -33 31.82 4.79 0 0 -34 987.45 17.57 0 0 -34 1033.97 17.78 0 0 -35 14.00 4.08 0 -1 -4 2606.45 13.33 0 1 -4 2597.77 13.17 0 -1 -4 2558.49 12.96 0 -1 -5 2063.10 12.45 0 -1 -5 2127.04 12.20 0 -1 -6 599.55 7.21 0 1 -6 616.85 7.12 0 -1 -6 594.96 6.83 0 -1 -7 3125.76 16.89 0 1 -7 3124.25 14.59 0 1 -7 3108.88 16.48 0 -1 -7 3097.56 16.02 0 1 8 1797.10 11.16 0 -1 -8 1822.20 13.43 0 -1 -8 1812.87 12.79 0 1 -8 1835.52 11.65 0 1 -8 1846.59 13.30 0 1 9 30.70 1.94 0 -1 -9 36.43 2.33 0 1 -9 37.20 2.46 0 -1 -9 40.33 2.60 0 -1 -9 35.23 1.87 0 1 -9 36.94 2.14 0 -1 -10 4962.24 18.08 0 1 10 5001.88 20.44 0 1 -10 4937.07 18.37 0 1 -10 4996.58 20.65 0 1 -10 5056.98 23.74 0 -1 -10 4919.17 22.60 0 -1 -10 4981.52 23.70 0 -1 -11 1848.62 11.23 0 1 11 1863.81 13.12 0 1 -11 1855.59 11.85 0 1 -11 1851.29 13.17 0 1 -11 1862.55 15.02 0 -1 -11 1861.17 14.42 0 -1 -11 1834.50 14.95 0 -1 -12 1742.04 11.08 0 1 12 1697.52 13.07 0 1 -12 1712.63 11.91 0 1 -12 1751.59 13.23 0 1 -12 1747.89 15.00 0 -1 -12 1704.49 14.25 0 -1 -12 1732.56 15.01 0 -1 -13 464.26 5.88 0 1 13 440.02 6.99 0 1 -13 451.76 6.51 0 1 -13 460.03 7.16 0 1 -13 458.14 8.04 0 -1 -13 472.00 7.82 0 -1 -13 465.06 8.15 0 -1 -14 196.65 4.00 0 1 14 200.94 5.07 0 1 -14 189.92 4.53 0 1 -14 186.61 4.81 0 1 -14 197.19 5.59 0 -1 -14 193.97 5.33 0 -1 -14 211.09 5.89 0 -1 -15 3085.73 15.25 0 1 -15 3072.47 19.37 0 1 -15 3051.01 18.07 0 -1 -15 3077.39 20.89 0 1 -15 3094.67 21.75 0 -1 -15 3022.46 21.58 0 1 15 3057.47 19.47 0 1 -16 1.20 1.68 0 1 16 2.05 1.84 0 -1 -16 1.32 1.48 0 1 -16 0.55 2.06 0 -1 -16 3.36 2.20 0 -1 -16 8.83 2.70 0 1 -16 2.64 1.68 0 1 17 657.75 9.80 0 1 -17 678.76 10.95 0 -1 -17 672.36 10.47 0 1 -17 674.64 9.76 0 -1 -17 689.87 7.49 0 1 -17 684.49 9.28 0 -1 -17 681.20 10.92 0 1 18 82.30 4.19 0 1 -18 89.85 4.60 0 -1 -18 93.55 4.77 0 1 -18 85.99 3.99 0 -1 -18 86.54 3.04 0 1 -18 83.17 3.76 0 -1 -18 98.95 4.97 0 1 19 4683.47 27.26 0 1 -19 4609.56 29.44 0 -1 -19 4663.42 28.40 0 1 -19 4595.29 26.65 0 -1 -19 4584.15 19.47 0 -1 -19 4623.29 29.49 0 1 20 4.75 2.86 0 1 -20 1.16 2.35 0 -1 -20 9.71 3.21 0 1 -20 -0.62 2.45 0 -1 -20 0.05 1.78 0 1 -20 6.76 2.80 0 1 21 152.79 5.57 0 1 -21 138.89 5.80 0 -1 -21 152.85 5.79 0 1 -21 143.35 5.32 0 -1 -21 144.29 3.79 0 -1 -21 147.28 5.89 0 1 -21 136.62 4.91 0 1 -22 193.29 6.80 0 -1 -22 203.23 6.76 0 1 -22 185.42 6.12 0 1 22 193.71 6.36 0 1 -22 190.71 5.86 0 -1 -22 199.52 6.93 0 1 -23 154.24 6.32 0 -1 -23 156.88 6.23 0 1 -23 154.83 5.83 0 1 23 157.88 5.99 0 1 -23 157.53 5.58 0 -1 -23 159.39 6.39 0 1 -24 422.67 10.23 0 -1 -24 417.02 9.85 0 1 -24 398.93 9.18 0 1 24 415.13 9.54 0 1 -24 428.20 9.05 0 -1 -24 423.73 10.26 0 1 -25 1096.86 16.51 0 -1 -25 1075.14 15.82 0 1 -25 1112.02 15.39 0 1 25 1108.06 15.61 0 -1 -25 1097.55 16.51 0 1 -25 1100.72 14.63 0 1 -26 313.22 9.26 0 -1 -26 316.13 9.12 0 1 -26 324.00 8.81 0 1 26 323.05 9.01 0 -1 -26 317.92 9.39 0 1 -26 300.75 8.17 0 1 -27 1114.51 17.28 0 -1 -27 1096.61 16.60 0 1 -27 1094.57 15.94 0 1 27 1079.58 16.17 0 -1 -27 1079.26 17.03 0 1 -27 1118.59 15.52 0 1 -28 502.52 12.11 0 -1 -28 499.91 11.79 0 1 -28 483.38 11.09 0 1 28 473.89 11.31 0 1 -28 495.92 10.76 0 -1 -28 520.99 12.36 0 1 -29 910.70 16.38 0 -1 -29 933.20 15.98 0 1 -29 939.70 15.49 0 1 29 912.52 15.59 0 1 -29 915.19 14.78 0 -1 -29 948.96 16.66 0 1 -30 70.95 5.56 0 -1 -30 70.53 5.46 0 1 -30 76.37 5.46 0 1 30 65.80 5.20 0 -1 -30 55.44 5.33 0 1 -30 59.63 4.92 0 1 -31 43.16 5.06 0 -1 -31 59.58 5.36 0 1 -31 54.35 4.95 0 1 31 58.53 5.16 0 -1 -31 51.64 5.25 0 1 -32 645.13 14.79 0 1 -32 680.93 13.98 0 -1 -32 702.79 15.29 0 1 32 680.50 14.37 0 -1 -32 698.87 14.68 0 -1 -33 395.81 11.92 0 1 33 367.57 10.98 0 -1 -33 368.15 11.15 0 -1 -34 216.87 9.21 0 -1 -34 200.10 8.59 0 -1 -35 34.67 5.31 0 -1 -35 38.97 5.08 0 -1 -36 371.81 12.11 0 -1 -36 388.76 11.93 0 -1 -37 402.38 12.88 0 -1 -38 969.09 19.70 0 -1 -39 72.70 6.92 0 -1 -40 224.65 10.37 0 -2 -2 1614.66 12.54 0 2 2 1620.29 12.03 0 -2 2 1656.35 13.20 0 -2 -2 1654.36 13.39 0 2 -2 1610.33 12.79 0 2 -2 1629.45 12.75 0 2 -4 1061.30 10.91 0 -2 -4 1081.26 10.94 0 2 4 1087.38 9.82 0 2 -4 1103.67 9.01 0 -2 4 1100.07 10.74 0 -2 -4 1092.55 11.05 0 2 -4 1094.81 10.53 0 2 -5 8225.87 30.85 0 -2 -5 8280.30 30.78 0 2 -5 8332.94 24.33 0 -2 5 8211.86 29.04 0 -2 -5 8246.35 30.30 0 2 -5 8296.04 28.88 0 2 -6 1265.09 12.56 0 2 -6 1304.51 9.63 0 -2 -6 1278.62 12.60 0 2 6 1286.88 10.72 0 2 -6 1309.60 11.79 0 -2 6 1286.82 11.60 0 -2 -6 1274.28 12.11 0 2 -7 150.56 4.73 0 2 -7 161.57 3.56 0 -2 -7 147.41 4.60 0 -2 -7 146.78 4.69 0 2 7 144.95 3.84 0 2 -7 143.46 4.18 0 -2 7 146.80 4.17 0 -2 -7 162.79 4.61 0 2 -8 506.92 8.43 0 2 -8 513.90 6.28 0 -2 -8 496.94 8.22 0 -2 -8 503.48 8.43 0 2 8 509.92 7.02 0 2 -8 487.12 7.46 0 -2 -8 507.33 7.77 0 -2 8 492.76 7.22 0 -2 -9 1499.01 14.37 0 2 9 1489.48 12.09 0 2 -9 1496.63 10.67 0 -2 9 1511.11 12.43 0 -2 -9 1482.00 13.22 0 -2 -9 1493.21 14.74 0 2 -9 1469.53 13.07 0 -2 -10 1688.77 15.57 0 2 10 1706.92 13.26 0 2 -10 1690.58 15.96 0 -2 10 1690.51 13.18 0 -2 -10 1671.42 14.12 0 2 -10 1679.10 14.21 0 2 -10 1663.44 11.57 0 -2 11 50.57 2.83 0 -2 -11 45.87 2.76 0 2 -11 49.35 3.18 0 -2 -11 47.18 3.11 0 2 11 48.08 2.68 0 -2 -11 45.33 3.28 0 2 -11 44.39 2.26 0 2 -11 48.59 2.90 0 -2 12 295.73 5.71 0 -2 -12 304.02 6.27 0 2 -12 301.52 7.27 0 -2 -12 298.21 6.90 0 2 12 308.59 6.10 0 -2 -12 293.39 7.23 0 2 -12 288.03 5.21 0 2 -12 290.43 6.30 0 -2 13 1349.48 11.84 0 -2 -13 1354.27 12.91 0 -2 -13 1390.53 15.65 0 2 -13 1335.04 13.40 0 2 -13 1362.60 15.44 0 -2 -13 1358.59 14.73 0 2 -13 1329.99 11.22 0 -2 -14 207.17 6.49 0 2 -14 219.68 6.69 0 2 14 207.23 5.38 0 2 -14 219.78 5.76 0 -2 14 215.37 4.99 0 -2 -14 224.55 5.51 0 -2 -14 220.31 6.33 0 2 -14 209.65 4.75 0 -2 -15 179.53 6.21 0 2 -15 193.35 6.37 0 -2 15 200.22 4.77 0 -2 -15 192.38 5.17 0 2 15 185.97 5.20 0 2 -15 182.79 5.47 0 2 -15 204.18 4.85 0 -2 -15 192.83 6.11 0 2 -16 3.46 1.58 0 -2 16 3.83 1.85 0 -2 -16 3.45 1.77 0 -2 -16 5.54 2.23 0 2 -16 1.06 2.10 0 2 -16 2.98 2.03 0 2 16 2.90 1.88 0 -2 -16 1.55 2.15 0 -2 17 159.51 4.34 0 2 17 153.38 5.08 0 2 -17 147.63 5.14 0 2 -17 144.51 4.41 0 -2 -17 152.56 4.73 0 2 -17 151.58 6.02 0 -2 -17 168.46 6.36 0 -2 -17 160.09 5.83 0 -2 18 1047.36 10.50 0 2 18 1034.42 12.70 0 2 -18 1012.11 13.00 0 2 -18 1030.38 11.39 0 -2 -18 1028.13 11.75 0 2 -18 1000.71 14.80 0 -2 -18 1046.88 15.32 0 -2 -18 1039.52 14.45 0 -2 19 2726.49 16.80 0 -2 -19 2824.46 19.38 0 2 -19 2885.26 19.44 0 -2 -19 2859.08 24.24 0 2 -19 2834.58 25.20 0 2 19 2805.99 21.40 0 2 -19 2786.24 21.83 0 -2 -19 2834.89 25.37 0 -2 -20 85.52 3.91 0 2 -20 83.12 3.82 0 -2 -20 83.69 5.10 0 2 -20 83.69 4.96 0 2 20 92.13 4.56 0 2 -20 83.15 4.36 0 -2 -20 101.28 5.99 0 -2 -21 2167.24 17.31 0 2 -21 2152.39 17.83 0 -2 -21 2188.17 22.06 0 2 -21 2153.46 22.98 0 2 21 2133.43 19.68 0 2 -21 2130.46 20.04 0 -2 -21 2180.25 23.19 0 -2 -22 56.16 3.46 0 2 22 53.10 3.86 0 -2 -22 52.02 4.59 0 2 -22 57.54 4.66 0 2 -22 54.33 3.53 0 -2 -22 51.98 4.97 0 2 -22 60.37 4.09 0 -2 -23 1509.55 19.08 0 2 -23 1514.48 17.58 0 2 -23 1463.78 15.50 0 -2 -23 1457.39 19.80 0 2 23 1445.18 17.05 0 2 -23 1465.86 19.66 0 2 -24 31.13 3.25 0 -2 -24 32.20 4.21 0 2 -24 31.11 3.42 0 2 -24 26.63 4.05 0 2 24 27.76 3.39 0 -2 -24 35.93 4.17 0 2 -25 41.41 3.43 0 -2 -25 45.48 4.54 0 2 -25 42.01 3.86 0 2 -25 39.17 4.18 0 2 25 42.94 3.95 0 -2 -25 44.95 4.51 0 2 -26 -2.48 2.67 0 2 -26 1.04 3.37 0 -2 -26 5.01 3.67 0 2 26 1.27 2.66 0 -2 -26 8.11 3.58 0 -2 -27 974.81 17.56 0 2 -27 917.22 15.05 0 2 -27 919.54 16.93 0 2 27 931.19 15.04 0 -2 -27 920.76 16.17 0 -2 -28 1385.36 21.08 0 2 -28 1476.48 19.22 0 2 -28 1410.23 21.12 0 2 28 1451.64 19.09 0 -2 -28 1458.03 20.56 0 -2 -29 1012.37 18.44 0 2 -29 1004.01 16.42 0 2 -29 978.65 18.16 0 2 29 1013.68 16.39 0 -2 -29 1044.26 17.94 0 -2 -30 1013.63 17.98 0 -2 -30 1036.51 19.06 0 2 -30 1032.44 16.90 0 -2 -31 2174.61 27.63 0 2 -31 2104.35 27.07 0 -2 -31 2156.66 26.22 0 -2 -32 664.54 15.97 0 -2 -32 626.43 14.92 0 -2 -33 191.58 9.07 0 2 -33 173.85 8.77 0 -2 -33 182.88 8.65 0 -2 -34 216.68 9.83 0 2 -34 223.27 9.85 0 -2 -34 233.24 9.63 0 -2 -35 8.11 4.28 0 2 -35 7.50 4.36 0 -2 -35 2.30 3.91 0 -2 -36 -2.25 4.37 0 2 -36 4.97 4.39 0 -2 -36 -0.27 3.89 0 -2 -37 39.46 5.70 0 2 -37 23.66 4.98 0 -2 -37 34.15 5.41 0 -2 -38 29.62 5.63 0 2 -38 26.24 5.28 0 -2 -38 32.86 5.36 0 -2 -39 53.38 6.41 0 2 -39 49.63 6.39 0 -2 -40 38.87 5.89 0 -2 -41 2.31 4.58 0 -2 -42 60.06 7.18 0 -2 -43 8.49 5.55 0 -2 -44 13.67 5.55 0 -3 0 0.84 1.61 0 3 0 1.98 1.90 0 -3 0 -1.57 2.10 0 3 0 3.71 1.88 0 -3 -1 2225.93 18.98 0 -3 1 2181.24 18.67 0 3 1 2242.55 18.72 0 3 -1 2202.87 18.44 0 -3 -1 2181.37 17.24 0 3 -1 2190.77 18.01 0 -3 2 481.15 8.98 0 -3 -2 506.93 9.22 0 3 -2 479.59 8.72 0 3 2 509.89 9.10 0 3 2 498.17 8.35 0 -3 -2 493.09 8.52 0 3 -2 481.95 8.69 0 -3 3 660.65 10.33 0 -3 -3 638.01 10.39 0 3 -3 629.47 9.94 0 3 3 654.14 10.40 0 3 3 642.79 9.42 0 -3 -3 643.31 9.90 0 3 -3 625.04 9.95 0 -3 4 390.46 8.13 0 -3 -4 400.80 8.32 0 3 -4 384.92 7.84 0 3 4 389.25 7.39 0 -3 -4 374.87 7.80 0 3 -4 386.98 8.07 0 3 -5 2868.27 21.53 0 -3 -5 2895.95 22.02 0 -3 5 2897.40 21.56 0 3 -5 2888.05 18.02 0 3 5 2960.19 19.73 0 -3 -5 2920.48 21.62 0 3 -5 2847.04 20.82 0 3 -6 229.93 6.43 0 -3 -6 239.42 6.65 0 -3 6 237.75 6.48 0 3 -6 230.02 5.28 0 3 6 233.39 5.82 0 -3 -6 228.01 6.44 0 3 -6 228.63 6.17 0 3 -7 573.02 10.18 0 -3 -7 573.69 10.05 0 -3 7 565.51 9.74 0 3 -7 574.13 8.01 0 3 7 584.52 8.99 0 -3 -7 568.13 10.06 0 3 -7 551.43 9.33 0 3 -8 2970.50 23.28 0 3 -8 3008.94 18.00 0 -3 8 2979.64 21.69 0 -3 -8 2946.73 22.37 0 3 8 3002.95 20.15 0 -3 -8 2965.22 23.10 0 3 -8 2958.87 21.57 0 -3 -9 -1.77 2.26 0 3 -9 0.49 1.91 0 -3 -9 1.24 2.35 0 3 -9 0.88 1.53 0 3 9 2.93 1.78 0 3 -9 4.29 2.59 0 -3 9 2.81 2.37 0 -3 10 1473.59 15.44 0 -3 -10 1483.21 16.05 0 -3 -10 1506.69 17.18 0 3 -10 1489.19 17.02 0 3 -10 1476.83 15.48 0 3 -10 1492.16 12.73 0 3 10 1493.89 14.44 0 -3 11 1020.45 12.89 0 -3 -11 1037.31 13.56 0 3 -11 1029.09 10.69 0 -3 -11 1003.37 14.37 0 3 -11 1044.62 14.65 0 3 11 1054.13 12.25 0 3 -11 1029.36 13.10 0 -3 -12 96.94 4.58 0 -3 12 104.37 4.61 0 -3 -12 101.60 5.10 0 3 -12 98.61 4.99 0 3 -12 104.01 3.72 0 3 -12 113.52 4.70 0 -3 -12 106.43 5.11 0 3 12 104.61 4.25 0 -3 13 4.14 2.14 0 -3 -13 0.53 2.10 0 3 -13 0.12 2.07 0 3 13 0.06 1.73 0 3 -13 1.40 2.09 0 3 -13 0.51 1.59 0 -3 -13 1.05 2.33 0 -3 -13 0.20 2.30 0 -3 -14 56.38 4.44 0 3 -14 52.50 3.59 0 3 -14 41.29 3.88 0 -3 14 51.17 3.56 0 -3 -14 51.56 3.67 0 -3 -14 41.74 3.83 0 3 14 49.35 3.31 0 3 -14 53.84 2.99 0 -3 15 1187.14 13.85 0 -3 -15 1174.63 14.55 0 3 15 1181.43 13.72 0 3 -15 1168.06 14.60 0 3 -15 1218.89 16.94 0 -3 -15 1175.96 16.21 0 3 -15 1178.82 11.93 0 -3 16 1.15 2.23 0 -3 -16 -1.01 2.23 0 3 -16 1.73 1.70 0 3 -16 -1.11 2.13 0 3 16 0.16 1.87 0 3 -16 1.22 2.59 0 -3 -16 4.70 2.56 0 -3 -16 -0.16 2.37 0 -3 -17 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3.03 2 -4 13 693.35 12.97 -2 -4 -13 715.67 14.84 2 4 -13 684.79 14.29 -2 -4 -13 706.04 14.59 -2 4 13 730.07 14.29 -2 -4 -13 716.46 13.71 2 -4 12 262.79 8.37 -2 -4 -12 240.71 8.80 2 4 -12 250.35 8.87 -2 -4 -12 252.26 8.90 -2 4 12 245.82 8.62 -2 -4 -12 261.02 8.55 2 -4 11 511.32 11.36 -2 -4 -11 488.94 12.10 2 4 -11 490.96 12.08 -2 -4 -11 499.15 11.90 -2 4 11 480.87 11.56 2 4 -11 478.00 9.13 -2 -4 -11 500.88 11.53 2 -4 10 137.56 6.58 -2 -4 -10 147.03 7.01 2 4 -10 132.01 6.58 -2 -4 -10 136.36 6.61 -2 4 10 123.86 6.40 2 4 -10 136.68 5.35 -2 -4 -10 130.25 6.39 2 -4 9 2045.13 22.40 -2 -4 -9 2002.79 23.26 2 4 -9 2007.10 23.60 -2 -4 -9 2030.86 22.67 2 4 -9 2030.61 18.76 -2 4 9 2028.85 23.22 -2 -4 -9 2020.35 22.61 2 -4 8 730.07 13.65 2 4 -8 735.55 14.35 -2 -4 -8 717.51 13.96 -2 -4 -8 723.41 13.46 2 4 -8 751.05 11.61 -2 4 8 697.80 13.78 -2 -4 -8 745.65 13.99 2 4 -7 58.80 3.89 -2 4 7 64.60 5.09 2 -4 7 60.74 4.98 -2 -4 -7 60.23 4.83 -2 -4 -7 62.37 4.73 -2 -4 -7 66.37 5.07 2 4 -7 61.74 4.79 -2 -4 -6 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0 162.56 7.02 -2 -4 1 83.49 4.10 -2 4 -1 94.37 5.51 2 -4 -1 100.85 5.91 -2 4 -1 93.48 4.66 -2 4 -1 79.06 5.28 -2 -4 1 89.93 5.60 2 4 1 92.77 5.63 -2 -4 2 652.38 10.04 2 -4 -2 657.82 13.58 -2 4 -2 661.94 13.47 -2 4 -2 684.53 11.51 -2 -4 2 627.02 13.21 2 4 2 655.83 13.30 -2 4 -2 677.39 13.30 2 -4 -3 1501.67 20.16 -2 4 -3 1517.60 20.18 -2 4 -3 1494.96 17.17 2 4 3 1525.58 19.95 -2 4 -3 1517.28 19.67 2 -4 -4 217.41 8.33 -2 4 -4 220.56 8.23 -2 4 -4 232.17 7.43 -2 -4 4 229.18 8.58 2 4 4 227.60 8.20 -2 4 -4 225.07 8.06 2 -4 -5 1953.48 23.23 -2 4 -5 2000.72 23.39 -2 4 -5 2011.30 20.79 -2 -4 5 1996.60 23.05 2 4 5 1990.76 23.02 -2 4 -5 1937.77 22.19 2 -4 -6 1689.57 21.72 -2 4 -6 1635.73 21.37 -2 4 -6 1686.77 19.47 -2 -4 6 1639.84 21.04 2 4 6 1679.63 21.11 -2 4 -6 1657.70 20.53 2 -4 -7 55.58 4.97 -2 4 -7 55.42 4.87 -2 4 -7 63.01 4.72 -2 -4 7 58.85 5.49 2 4 7 58.88 4.98 -2 4 -7 52.77 4.58 2 -4 -8 742.06 14.76 -2 4 -8 725.33 13.73 -2 4 -8 764.39 14.96 -2 4 -8 730.63 13.41 -2 -4 8 740.41 14.49 2 4 8 712.30 14.16 -2 4 -9 1978.22 23.97 2 4 9 2049.11 23.61 -2 4 -9 2015.17 22.37 -2 4 -9 2036.24 22.82 2 -4 -9 2059.77 24.15 -2 4 -10 143.47 7.15 2 4 10 133.55 6.62 -2 4 -10 133.20 6.54 -2 4 -10 134.55 6.49 2 -4 -10 144.05 7.12 -2 -4 10 124.11 6.82 -2 4 -11 493.60 12.39 2 4 11 502.61 12.01 -2 4 -11 505.12 11.90 -2 4 -11 481.34 11.51 2 -4 -11 503.47 12.42 -2 -4 11 461.55 11.73 -2 4 -12 283.70 9.69 2 4 12 266.40 9.06 -2 4 -12 244.18 8.64 -2 4 -12 264.01 8.76 2 -4 -12 243.19 8.89 -2 -4 12 243.96 8.89 -2 4 -13 722.02 15.14 -2 4 -13 737.94 14.11 2 4 13 734.76 14.82 -2 4 -13 720.11 14.53 -2 -4 13 698.41 14.26 2 -4 -13 702.11 14.64 2 -4 -14 6.36 3.16 -2 -4 14 2.64 3.54 -2 4 -14 12.18 3.40 -2 4 -14 3.83 3.20 2 4 14 -0.22 3.00 -2 4 -14 -0.52 3.07 -2 4 -15 288.95 9.24 2 4 15 290.76 9.70 -2 4 -15 285.65 9.74 -2 4 -15 272.57 9.67 2 -4 -15 287.87 9.78 -2 -4 15 273.23 9.26 2 4 16 164.51 7.77 -2 4 -16 183.99 8.37 -2 4 -16 162.97 7.90 2 -4 -16 162.33 7.68 -2 -4 16 165.83 7.51 2 -4 -17 30.07 4.40 -2 4 -17 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6.19 6 6 2 16.09 7.15 6 -6 -2 11.37 6.84 -6 6 -3 13.71 7.28 6 6 3 -2.98 6.77 6 -6 -3 23.00 7.26 -6 6 -4 15.80 6.61 -6 6 -5 34.35 7.85 -6 6 -6 167.74 11.87 -6 6 -7 47.54 8.67 -6 6 -8 4.95 7.29 -6 6 -9 167.43 12.41 -7 0 -6 13.54 5.50 -7 0 -7 3.98 5.25 -7 0 -8 10.27 5.34 -7 0 -9 15.55 5.90 -7 0 -9 18.51 6.02 -7 0 -10 8.21 6.09 -7 0 -10 -2.80 5.16 -7 0 -11 109.94 9.27 -7 0 -12 20.08 6.67 -7 0 -13 -0.70 5.39 -7 0 -14 11.36 5.80 -7 0 -15 14.18 6.70 -7 0 -16 -2.10 5.40 -7 0 -17 10.55 5.93 7 0 18 3.82 5.65 -7 0 -18 -0.59 5.73 -7 0 -19 47.87 8.16 7 0 19 42.72 7.69 7 0 20 14.16 6.18 -7 0 -20 10.68 6.33 -7 0 -20 25.99 7.35 7 0 21 36.24 7.29 -7 0 -21 25.37 7.04 -7 0 -21 15.77 6.75 7 0 22 16.89 6.66 -7 0 -22 21.71 7.16 -7 0 -22 23.42 7.21 7 0 23 25.45 6.97 -7 0 -23 22.18 6.95 7 0 24 -3.18 6.50 -7 0 -24 -5.56 6.34 7 -1 24 2.02 6.08 -7 -1 -24 -1.89 6.66 7 -1 23 3.48 6.08 -7 -1 -23 6.33 6.25 -7 -1 -22 3.30 6.42 -7 -1 -21 14.08 6.79 -7 -1 -20 32.13 7.59 -7 -1 -19 144.60 11.12 -7 -1 -18 55.18 8.40 -7 -1 -17 36.03 7.44 -7 -1 -16 -4.19 5.97 -7 -1 -15 20.21 6.54 -7 -1 -14 38.72 7.20 -7 -1 -13 64.12 7.88 -7 -1 -12 18.68 6.09 -7 -1 -11 11.74 5.80 -7 -1 -10 96.81 8.84 -7 -1 -9 77.44 8.45 -7 -1 -8 24.46 6.95 -7 -1 -7 45.69 7.37 -7 -1 -6 43.14 7.22 -7 -1 -5 26.02 6.68 -7 -1 -4 117.71 9.60 -7 -1 -3 73.81 8.56 -7 -1 -2 121.50 9.80 -7 -1 -1 57.42 7.92 -7 -1 0 145.06 10.48 -7 1 -1 29.05 6.15 -7 -1 1 38.55 7.45 -7 1 -2 103.49 8.79 -7 -1 2 117.85 10.12 -7 1 -3 65.32 7.69 -7 -1 3 56.05 8.22 -7 1 -4 112.34 9.14 -7 -1 4 81.54 8.92 -7 1 -5 18.47 5.99 -7 -1 5 27.59 7.28 -7 1 -6 33.62 6.68 -7 -1 6 50.93 7.64 -7 1 -7 47.30 7.31 -7 -1 7 39.62 7.78 -7 1 -8 11.41 5.70 -7 -1 8 20.78 6.61 -7 1 -9 74.62 8.26 -7 -1 9 78.72 9.03 -7 1 -10 98.92 9.10 -7 -1 10 92.55 9.56 -7 1 -11 6.38 5.72 -7 -1 11 12.05 6.51 -7 1 -12 14.88 6.51 -7 -1 12 17.35 6.67 -7 1 -13 48.12 7.36 7 1 13 63.60 7.73 -7 -1 13 64.98 8.81 7 1 14 49.01 7.26 -7 1 -14 29.73 7.30 -7 -1 14 40.88 8.11 -7 1 -15 39.56 7.30 7 1 15 17.04 6.18 -7 -1 15 26.17 7.21 -7 1 -16 18.21 7.09 7 1 16 8.22 5.87 -7 -1 16 14.04 6.91 -7 1 -17 27.31 7.29 -7 -1 17 38.37 7.64 7 1 17 27.41 6.73 -7 1 -18 64.17 8.50 -7 -1 18 79.15 9.44 7 1 18 72.01 8.63 -7 1 -18 52.14 8.24 -7 1 -19 141.42 11.01 7 1 19 141.38 10.54 -7 -1 19 152.95 11.65 -7 1 -19 177.96 12.23 -7 1 -20 7.98 6.55 -7 -1 20 21.54 7.49 -7 1 -20 30.19 7.39 7 1 20 25.51 7.08 -7 -1 21 15.84 7.28 -7 1 -21 14.76 6.62 7 1 21 14.11 6.47 -7 1 -22 7.59 6.41 7 1 22 -7.84 6.49 -7 1 -23 11.07 7.03 7 1 23 5.42 6.19 -7 -2 -21 173.06 12.45 -7 -2 -20 24.39 7.60 -7 -2 -19 126.16 10.49 -7 -2 -18 37.17 7.78 -7 -2 -17 79.17 8.92 -7 -2 -16 0.93 6.15 -7 -2 -11 39.20 7.65 -7 -2 -10 67.85 8.27 -7 -2 -9 73.07 8.39 -7 -2 -8 26.55 6.75 -7 -2 -7 8.86 6.40 -7 -2 -6 52.65 7.84 -7 -2 -5 12.38 6.07 -7 2 4 7.46 5.45 -7 -2 -4 1.30 6.10 -7 2 3 30.11 6.29 -7 -2 -3 40.21 7.21 -7 2 2 81.77 8.28 -7 -2 -2 44.03 7.73 -7 2 1 27.39 6.33 -7 -2 -1 17.71 6.79 -7 2 0 40.12 6.77 -7 -2 0 37.22 7.27 -7 2 -1 27.43 6.45 7 -2 -1 32.00 6.85 -7 -2 1 36.26 7.46 -7 2 -2 70.89 8.31 7 -2 -2 61.86 8.28 -7 -2 2 69.08 8.30 -7 2 -3 23.77 6.44 7 -2 -3 32.03 7.38 -7 -2 3 25.03 6.81 -7 2 -4 4.68 5.49 7 -2 -4 5.40 5.77 -7 -2 4 18.21 7.07 -7 2 -5 20.00 6.29 7 -2 -5 11.76 6.23 -7 -2 5 23.97 7.02 -7 2 -6 38.24 6.90 7 -2 -6 47.85 7.69 -7 -2 6 38.79 7.46 -7 2 -7 9.91 6.05 7 -2 -7 7.15 5.91 -7 -2 7 10.19 6.42 -7 2 -8 24.62 6.60 7 -2 -8 18.69 6.93 -7 -2 8 14.65 6.78 7 2 9 62.34 7.89 -7 2 -9 56.76 7.95 7 -2 -9 64.29 8.62 -7 -2 9 50.27 8.22 7 2 10 73.39 7.99 -7 2 -10 67.56 8.44 7 -2 -10 82.18 9.01 -7 -2 10 100.51 9.63 -7 2 -11 50.79 8.05 7 -2 -11 55.48 8.49 -7 -2 11 45.26 7.92 7 2 12 15.18 5.99 -7 2 -12 25.50 7.17 7 -2 -12 21.21 6.91 -7 -2 12 32.76 7.46 7 2 13 47.96 7.23 -7 2 -13 43.18 7.77 7 -2 -13 47.87 8.51 7 2 14 25.96 6.93 -7 -2 14 24.51 7.42 -7 2 -14 17.13 6.58 7 -2 -14 13.72 6.78 7 2 15 5.00 5.52 -7 -2 15 4.18 6.43 -7 2 -15 4.69 6.12 7 2 16 9.46 6.29 -7 2 -16 1.82 6.04 -7 2 -17 107.38 9.59 -7 -2 17 100.24 10.47 -7 2 -17 91.97 9.62 7 2 17 75.10 8.81 7 2 18 39.70 7.68 -7 2 -18 34.40 7.91 -7 -2 18 37.49 7.91 -7 2 -18 33.39 7.45 7 2 19 99.84 9.64 -7 2 -19 111.03 10.03 7 2 20 26.08 7.37 -7 2 -20 31.14 7.73 -7 2 -21 167.86 12.01 -7 -3 -11 11.42 6.57 -7 -3 -10 55.61 8.29 -7 -3 -9 15.72 6.99 -7 3 9 10.27 6.12 -7 -3 -8 44.35 8.03 -7 3 8 30.79 6.85 7 -3 7 11.87 6.39 -7 -3 -7 15.21 6.78 -7 3 7 5.32 5.90 -7 -3 -6 46.96 8.23 7 -3 6 44.60 7.77 -7 -3 -5 55.44 8.18 7 -3 5 47.97 7.85 -7 3 5 52.66 7.89 7 -3 4 20.83 6.82 -7 -3 -4 18.51 6.56 -7 3 4 7.01 6.09 7 -3 3 12.50 6.48 -7 -3 -3 8.09 6.75 -7 3 3 2.47 5.62 7 -3 2 26.89 7.04 -7 -3 -2 29.31 7.33 -7 3 2 30.06 7.08 7 -3 1 17.59 6.53 -7 -3 -1 29.94 7.63 -7 3 1 27.73 7.20 -7 -3 0 96.40 9.47 7 -3 0 85.88 9.21 -7 3 0 83.84 8.96 7 -3 -1 23.42 6.77 -7 3 -1 25.20 6.62 -7 -3 1 10.97 6.55 7 -3 -2 21.30 6.86 -7 3 -2 12.56 6.14 -7 -3 2 19.71 7.33 7 -3 -3 12.13 6.66 -7 3 -3 10.70 6.16 -7 -3 3 19.59 7.12 7 -3 -4 23.06 7.17 -7 3 -4 16.38 6.49 -7 -3 4 29.94 7.38 -7 3 -5 63.45 8.32 7 -3 -5 60.82 8.75 7 3 5 60.23 7.72 -7 -3 5 60.75 8.60 -7 3 -6 59.05 8.51 7 -3 -6 48.11 7.89 7 3 6 55.47 7.93 -7 -3 6 78.18 9.30 -7 3 -7 10.20 6.54 7 -3 -7 0.87 6.14 7 3 7 2.75 6.03 -7 -3 7 2.36 6.66 -7 3 -8 36.21 7.37 7 -3 -8 28.72 7.28 7 3 8 31.70 7.05 -7 -3 8 47.55 8.16 -7 3 -9 16.24 6.86 7 -3 -9 20.56 7.53 7 3 9 11.93 6.13 -7 -3 9 16.76 7.21 -7 3 -10 67.62 8.95 7 -3 -10 65.61 9.39 7 3 10 60.88 7.96 -7 -3 10 53.04 8.46 -7 3 -11 4.60 6.43 7 -3 -11 7.15 7.10 7 3 11 8.68 6.27 -7 -3 11 9.62 6.95 -7 3 -12 35.87 7.63 7 -3 -12 32.09 7.56 7 3 12 43.31 7.69 -7 -3 12 46.54 8.50 -7 3 -13 45.97 8.35 7 -3 -13 45.30 8.32 -7 -3 13 47.94 8.68 7 3 13 53.28 8.13 -7 3 -14 4.37 6.63 7 3 14 5.39 6.24 -7 3 -15 32.56 7.64 7 3 15 32.96 7.58 -7 3 -16 36.19 7.72 7 3 16 39.04 7.90 -7 3 -17 33.18 7.67 7 3 17 26.26 7.40 -7 3 -18 22.45 7.27 -7 4 13 2.39 6.59 -7 4 12 15.87 7.18 -7 -4 -11 98.15 10.18 -7 4 11 96.29 10.06 -7 -4 -10 11.46 7.34 -7 4 10 27.77 7.46 -7 4 9 67.10 9.01 -7 -4 -9 72.51 9.33 -7 4 8 42.50 8.01 -7 -4 -8 43.15 8.46 -7 -4 -7 48.47 8.77 7 -4 7 35.64 7.74 -7 4 7 40.86 8.00 7 -4 6 17.61 7.22 -7 4 6 22.32 7.01 -7 -4 -6 30.18 8.07 7 -4 5 11.30 7.29 -7 4 5 7.32 6.36 -7 -4 -5 14.93 7.30 7 -4 4 12.61 6.97 -7 4 4 -2.54 6.31 -7 -4 -4 6.82 6.96 -7 4 3 12.65 6.82 -7 -4 -3 25.94 7.35 7 -4 2 21.14 7.21 -7 4 2 19.94 7.04 -7 -4 -2 9.68 6.98 -7 -4 -1 28.64 7.65 7 -4 1 21.15 7.00 -7 4 1 40.53 8.20 -7 4 0 19.36 6.99 7 -4 0 5.52 6.77 -7 -4 0 16.29 7.49 7 -4 -1 50.82 8.69 -7 -4 1 29.10 7.73 -7 4 -1 25.65 7.23 7 4 1 29.13 7.19 -7 -4 2 33.93 8.60 7 4 2 10.30 6.44 -7 4 -2 19.93 7.08 7 -4 -2 16.51 7.10 -7 -4 3 44.01 8.64 7 -4 -3 44.73 8.29 -7 4 -3 17.14 6.52 7 4 3 41.23 7.64 7 4 4 5.39 6.10 -7 4 -4 -13.99 6.95 7 -4 -4 -8.27 7.18 7 4 5 8.67 6.58 -7 4 -5 14.63 6.92 7 -4 -5 4.35 6.82 7 4 6 25.77 7.02 7 4 7 51.68 8.17 7 4 8 41.59 7.97 7 4 9 33.28 7.79 7 4 10 15.27 7.18 7 4 11 91.10 9.97 -7 4 -13 14.27 6.89 -7 4 -14 18.70 7.47 -8 0 -5 10.59 7.28 -8 0 -6 17.62 7.75 -8 0 -7 6.27 6.76 0 0 0 0.00 0.00 TITL pPh-2 in P2(1)2(1)2 REM P2(1)2(1)2 (#18 in standard setting) CELL 0.71073 6.131272 7.371038 38.114260 90.0000 90.0000 90.0000 ZERR 4.00 0.000181 0.000219 0.001120 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 80.00 96.00 4.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 63284 _shelx_res_file ; TITL pph-2_a.res in P2(1)2(1)2(1) pPh-2.res created by SHELXL-2018/3 at 18:43:43 on 24-Mar-2021 REM Yadorkari-X generated CELL 0.71073 6.1313 7.3710 38.1143 90.0000 90.0000 90.0000 ZERR 4.0 0.0002 0.0002 0.0011 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z REM SPGR P212121 orthorhombic SFAC C H N O UNIT 80 92 4 8 SIZE 0.31 0.29 0.29 TEMP -100.0 L.S. 10 FMAP 2 PLAN -2 ACTA CONF HTAB LIST 4 BOND $H list 4 fmap 2 53 HTAB C9 O1 HTAB C14 O2 WGHT 0.031400 0.377800 FVAR 1.33237 C1 1 0.509290 0.572772 0.664694 11.00000 0.02849 0.02339 = 0.02008 0.00115 -0.00348 0.00242 C2 1 0.616063 0.649088 0.693556 11.00000 0.02488 0.02750 = 0.02674 0.00017 -0.00310 -0.00269 AFIX 43 H1 2 0.757076 0.700514 0.690769 11.00000 -1.20000 AFIX 0 C3 1 0.517117 0.649902 0.726088 11.00000 0.02748 0.02775 = 0.02162 -0.00222 -0.00615 -0.00330 AFIX 43 H2 2 0.591743 0.702783 0.745390 11.00000 -1.20000 AFIX 0 C4 1 0.309739 0.574953 0.731455 11.00000 0.02671 0.02018 = 0.02228 0.00087 -0.00315 0.00283 O1 4 0.812817 0.613273 0.626559 11.00000 0.03588 0.05939 = 0.02856 -0.00201 0.00361 -0.00635 O2 4 0.486930 0.326285 0.596650 11.00000 0.05984 0.02591 = 0.02850 0.00041 -0.00790 0.00302 N1 3 0.418843 0.610841 0.575092 11.00000 0.03761 0.02549 = 0.01975 -0.00014 -0.00165 0.00023 C5 1 0.203960 0.500748 0.702096 11.00000 0.02520 0.03125 = 0.02828 -0.00169 -0.00368 -0.00482 AFIX 43 H3 2 0.062937 0.449217 0.704797 11.00000 -1.20000 AFIX 0 C6 1 0.301194 0.501145 0.669218 11.00000 0.03025 0.03336 = 0.02235 -0.00335 -0.00812 -0.00056 AFIX 43 H4 2 0.225190 0.452194 0.649669 11.00000 -1.20000 AFIX 0 C7 1 0.622739 0.569664 0.630282 11.00000 0.03383 0.02707 = 0.02443 0.00209 -0.00234 -0.00001 C8 1 0.498538 0.492713 0.598625 11.00000 0.03649 0.02844 = 0.01940 -0.00002 0.00067 0.00096 C9 1 0.436361 0.809947 0.580339 11.00000 0.04421 0.02636 = 0.02476 0.00110 -0.00176 -0.00253 AFIX 13 H5 2 0.497384 0.829750 0.604367 11.00000 -1.20000 AFIX 0 C10 1 0.594948 0.894656 0.554486 11.00000 0.04456 0.03823 = 0.05814 0.01043 0.00893 -0.00287 AFIX 137 H6 2 0.736401 0.833410 0.556225 11.00000 -1.50000 H7 2 0.612914 1.023717 0.559944 11.00000 -1.50000 H8 2 0.537864 0.881506 0.530604 11.00000 -1.50000 AFIX 0 C11 1 0.214463 0.901298 0.579288 11.00000 0.05062 0.03155 = 0.04514 -0.00447 0.01347 0.00383 AFIX 137 H9 2 0.156583 0.896594 0.555338 11.00000 -1.50000 H10 2 0.229103 1.028114 0.586642 11.00000 -1.50000 H11 2 0.114502 0.838140 0.595205 11.00000 -1.50000 AFIX 0 C12 1 0.311127 0.544467 0.542502 11.00000 0.04212 0.03108 = 0.01953 -0.00203 -0.00497 0.00740 AFIX 13 H12 2 0.270143 0.654227 0.528562 11.00000 -1.20000 AFIX 0 C13 1 0.467955 0.434545 0.519928 11.00000 0.05932 0.05703 = 0.02341 -0.00811 -0.00233 0.01837 AFIX 137 H13 2 0.601203 0.504937 0.515886 11.00000 -1.50000 H14 2 0.398812 0.406781 0.497376 11.00000 -1.50000 H15 2 0.504725 0.321214 0.532000 11.00000 -1.50000 AFIX 0 C14 1 0.100730 0.444152 0.550627 11.00000 0.04757 0.04331 = 0.03947 -0.00805 -0.00929 -0.00282 AFIX 137 H16 2 0.134408 0.331101 0.563027 11.00000 -1.50000 H17 2 0.024513 0.416204 0.528682 11.00000 -1.50000 H18 2 0.007510 0.520425 0.565414 11.00000 -1.50000 AFIX 0 C15 1 0.206828 0.572909 0.766995 11.00000 0.02934 0.01932 = 0.02403 -0.00016 -0.00040 0.00186 C16 1 0.314950 0.645021 0.796305 11.00000 0.03965 0.03233 = 0.02598 -0.00159 0.00046 -0.00756 AFIX 43 H19 2 0.454724 0.698538 0.793378 11.00000 -1.20000 AFIX 0 C17 1 0.221902 0.639734 0.829444 11.00000 0.05680 0.03506 = 0.02376 -0.00334 0.00094 -0.00800 AFIX 43 H20 2 0.299212 0.687471 0.848972 11.00000 -1.20000 AFIX 0 C18 1 0.017205 0.565321 0.834177 11.00000 0.05546 0.03224 = 0.02854 0.00310 0.01258 0.00053 AFIX 43 H21 2 -0.047408 0.563386 0.856828 11.00000 -1.20000 AFIX 0 C19 1 -0.092955 0.493691 0.805721 11.00000 0.03596 0.03480 = 0.03733 0.00376 0.00896 -0.00092 AFIX 43 H22 2 -0.233437 0.441822 0.808872 11.00000 -1.20000 AFIX 0 C20 1 0.000499 0.497174 0.772632 11.00000 0.03046 0.02808 = 0.02998 0.00003 -0.00234 0.00115 AFIX 43 H23 2 -0.077146 0.447082 0.753360 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM pph-2_a.res in P2(1)2(1)2(1) REM wR2 = 0.0803, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0361 for 3614 Fo > 4sig(Fo) and 0.0399 for all 3877 data REM 212 parameters refined using 0 restraints END WGHT 0.0308 0.3780 REM Instructions for potential hydrogen bonds HTAB C9 O1 HTAB C13 O2 HTAB C14 O2 REM Highest difference peak 0.164, deepest hole -0.146, 1-sigma level 0.029 Q1 1 0.2423 0.6380 0.7803 11.00000 0.05 0.16 Q2 1 0.2769 0.4954 0.7200 11.00000 0.05 0.16 ; _shelx_res_checksum 28522 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 _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.5093(3) 0.5728(2) 0.66469(4) 0.0240(3) Uani d 1 . . C C2 0.6161(3) 0.6491(2) 0.69356(4) 0.0264(4) Uani d 1 . . H H1 0.757076 0.700514 0.690769 0.032 Uiso calc 1 . . C C3 0.5171(3) 0.6499(2) 0.72609(4) 0.0256(3) Uani d 1 . . H H2 0.591743 0.702783 0.745390 0.031 Uiso calc 1 . . C C4 0.3097(3) 0.5750(2) 0.73146(4) 0.0231(3) Uani d 1 . . O O1 0.8128(2) 0.6133(2) 0.62656(3) 0.0413(3) Uani d 1 . . O O2 0.4869(2) 0.32629(16) 0.59665(3) 0.0381(3) Uani d 1 . . N N1 0.4188(2) 0.61084(19) 0.57509(4) 0.0276(3) Uani d 1 . . C C5 0.2040(3) 0.5007(2) 0.70210(5) 0.0282(4) Uani d 1 . . H H3 0.062937 0.449217 0.704797 0.034 Uiso calc 1 . . C C6 0.3012(3) 0.5011(2) 0.66922(4) 0.0287(4) Uani d 1 . . H H4 0.225190 0.452194 0.649669 0.034 Uiso calc 1 . . C C7 0.6227(3) 0.5697(2) 0.63028(4) 0.0284(4) Uani d 1 . . C C8 0.4985(3) 0.4927(2) 0.59863(4) 0.0281(4) Uani d 1 . . C C9 0.4364(3) 0.8099(2) 0.58034(5) 0.0318(4) Uani d 1 . . H H5 0.497384 0.829750 0.604367 0.038 Uiso calc 1 . . C C10 0.5949(4) 0.8947(3) 0.55449(6) 0.0470(5) Uani d 1 . . H H6 0.736401 0.833410 0.556225 0.070 Uiso calc 1 . . H H7 0.612914 1.023717 0.559944 0.070 Uiso calc 1 . . H H8 0.537864 0.881506 0.530604 0.070 Uiso calc 1 . . C C11 0.2145(4) 0.9013(3) 0.57929(6) 0.0424(5) Uani d 1 . . H H9 0.156583 0.896594 0.555338 0.064 Uiso calc 1 . . H H10 0.229103 1.028114 0.586642 0.064 Uiso calc 1 . . H H11 0.114502 0.838140 0.595205 0.064 Uiso calc 1 . . C C12 0.3111(3) 0.5445(2) 0.54250(4) 0.0309(4) Uani d 1 . . H H12 0.270143 0.654227 0.528562 0.037 Uiso calc 1 . . C C13 0.4680(4) 0.4345(3) 0.51993(5) 0.0466(5) Uani d 1 . . H H13 0.601203 0.504937 0.515886 0.070 Uiso calc 1 . . H H14 0.398812 0.406781 0.497376 0.070 Uiso calc 1 . . H H15 0.504725 0.321214 0.532000 0.070 Uiso calc 1 . . C C14 0.1007(4) 0.4442(3) 0.55063(6) 0.0434(5) Uani d 1 . . H H16 0.134408 0.331101 0.563027 0.065 Uiso calc 1 . . H H17 0.024513 0.416204 0.528682 0.065 Uiso calc 1 . . H H18 0.007510 0.520425 0.565414 0.065 Uiso calc 1 . . C C15 0.2068(3) 0.5729(2) 0.76699(4) 0.0242(3) Uani d 1 . . C C16 0.3150(3) 0.6450(2) 0.79631(5) 0.0327(4) Uani d 1 . . H H19 0.454724 0.698538 0.793378 0.039 Uiso calc 1 . . C C17 0.2219(4) 0.6397(3) 0.82944(5) 0.0385(5) Uani d 1 . . H H20 0.299212 0.687471 0.848972 0.046 Uiso calc 1 . . C C18 0.0172(4) 0.5653(3) 0.83418(5) 0.0387(5) Uani d 1 . . H H21 -0.047408 0.563386 0.856828 0.046 Uiso calc 1 . . C C19 -0.0930(3) 0.4937(3) 0.80572(5) 0.0360(4) Uani d 1 . . H H22 -0.233437 0.441822 0.808872 0.043 Uiso calc 1 . . C C20 0.0005(3) 0.4972(2) 0.77263(5) 0.0295(4) Uani d 1 . . H H23 -0.077146 0.447082 0.753360 0.035 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 0.0285(8) 0.0234(7) 0.0201(8) 0.0024(7) -0.0035(6) 0.0011(6) C2 0.0249(8) 0.0275(8) 0.0267(9) -0.0027(7) -0.0031(7) 0.0002(7) C3 0.0275(8) 0.0278(8) 0.0216(8) -0.0033(7) -0.0061(7) -0.0022(6) C4 0.0267(8) 0.0202(7) 0.0223(8) 0.0028(7) -0.0031(6) 0.0009(6) O1 0.0359(7) 0.0594(9) 0.0286(7) -0.0063(7) 0.0036(6) -0.0020(6) O2 0.0598(9) 0.0259(6) 0.0285(6) 0.0030(6) -0.0079(6) 0.0004(5) N1 0.0376(8) 0.0255(7) 0.0198(7) 0.0002(6) -0.0016(6) -0.0001(6) C5 0.0252(8) 0.0313(8) 0.0283(9) -0.0048(8) -0.0037(7) -0.0017(7) C6 0.0303(9) 0.0334(9) 0.0224(8) -0.0006(8) -0.0081(7) -0.0034(7) C7 0.0338(10) 0.0271(8) 0.0244(8) 0.0000(7) -0.0023(7) 0.0021(7) C8 0.0365(10) 0.0284(8) 0.0194(8) 0.0010(8) 0.0007(7) 0.0000(7) C9 0.0442(11) 0.0264(8) 0.0248(9) -0.0025(8) -0.0018(8) 0.0011(7) C10 0.0446(11) 0.0382(11) 0.0581(13) -0.0029(10) 0.0089(10) 0.0104(10) C11 0.0506(12) 0.0316(9) 0.0451(11) 0.0038(9) 0.0135(10) -0.0045(9) C12 0.0421(10) 0.0311(9) 0.0195(8) 0.0074(8) -0.0050(7) -0.0020(7) C13 0.0593(14) 0.0570(13) 0.0234(9) 0.0184(12) -0.0023(9) -0.0081(9) C14 0.0476(12) 0.0433(11) 0.0395(11) -0.0028(10) -0.0093(10) -0.0081(9) C15 0.0293(8) 0.0193(7) 0.0240(8) 0.0019(7) -0.0004(7) -0.0002(6) C16 0.0396(10) 0.0323(9) 0.0260(9) -0.0076(8) 0.0005(8) -0.0016(7) C17 0.0568(12) 0.0351(10) 0.0238(9) -0.0080(9) 0.0009(9) -0.0033(8) C18 0.0555(13) 0.0322(9) 0.0285(9) 0.0005(9) 0.0126(9) 0.0031(8) C19 0.0360(10) 0.0348(9) 0.0373(10) -0.0009(8) 0.0090(9) 0.0038(8) C20 0.0305(9) 0.0281(8) 0.0300(9) 0.0011(8) -0.0023(7) 0.0000(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 C6 C1 C2 . . 118.98(15) ? C6 C1 C7 . . 122.22(15) ? C2 C1 C7 . . 118.80(15) ? C3 C2 C1 . . 120.18(15) ? C3 C2 H1 . . 119.9 ? C1 C2 H1 . . 119.9 ? C2 C3 C4 . . 121.88(15) ? C2 C3 H2 . . 119.1 ? C4 C3 H2 . . 119.1 ? C3 C4 C5 . . 117.15(15) ? C3 C4 C15 . . 121.29(14) ? C5 C4 C15 . . 121.56(15) ? C8 N1 C9 . . 121.65(14) ? C8 N1 C12 . . 120.38(14) ? C9 N1 C12 . . 117.97(14) ? C6 C5 C4 . . 121.36(16) ? C6 C5 H3 . . 119.3 ? C4 C5 H3 . . 119.3 ? C5 C6 C1 . . 120.44(15) ? C5 C6 H4 . . 119.8 ? C1 C6 H4 . . 119.8 ? O1 C7 C1 . . 123.19(16) ? O1 C7 C8 . . 118.74(16) ? C1 C7 C8 . . 117.87(15) ? O2 C8 N1 . . 125.77(17) ? O2 C8 C7 . . 116.41(16) ? N1 C8 C7 . . 117.78(15) ? N1 C9 C10 . . 111.42(16) ? N1 C9 C11 . . 111.71(16) ? C10 C9 C11 . . 111.97(16) ? N1 C9 H5 . . 107.1 ? C10 C9 H5 . . 107.1 ? C11 C9 H5 . . 107.1 ? C9 C10 H6 . . 109.5 ? C9 C10 H7 . . 109.5 ? H6 C10 H7 . . 109.5 ? C9 C10 H8 . . 109.5 ? H6 C10 H8 . . 109.5 ? H7 C10 H8 . . 109.5 ? C9 C11 H9 . . 109.5 ? C9 C11 H10 . . 109.5 ? H9 C11 H10 . . 109.5 ? C9 C11 H11 . . 109.5 ? H9 C11 H11 . . 109.5 ? H10 C11 H11 . . 109.5 ? N1 C12 C14 . . 111.50(15) ? N1 C12 C13 . . 111.46(16) ? C14 C12 C13 . . 113.10(17) ? N1 C12 H12 . . 106.8 ? C14 C12 H12 . . 106.8 ? C13 C12 H12 . . 106.8 ? C12 C13 H13 . . 109.5 ? C12 C13 H14 . . 109.5 ? H13 C13 H14 . . 109.5 ? C12 C13 H15 . . 109.5 ? H13 C13 H15 . . 109.5 ? H14 C13 H15 . . 109.5 ? C12 C14 H16 . . 109.5 ? C12 C14 H17 . . 109.5 ? H16 C14 H17 . . 109.5 ? C12 C14 H18 . . 109.5 ? H16 C14 H18 . . 109.5 ? H17 C14 H18 . . 109.5 ? C20 C15 C16 . . 117.12(16) ? C20 C15 C4 . . 121.66(15) ? C16 C15 C4 . . 121.21(16) ? C17 C16 C15 . . 121.34(18) ? C17 C16 H19 . . 119.3 ? C15 C16 H19 . . 119.3 ? C18 C17 C16 . . 120.26(18) ? C18 C17 H20 . . 119.9 ? C16 C17 H20 . . 119.9 ? C17 C18 C19 . . 119.54(17) ? C17 C18 H21 . . 120.2 ? C19 C18 H21 . . 120.2 ? C18 C19 C20 . . 120.33(19) ? C18 C19 H22 . . 119.8 ? C20 C19 H22 . . 119.8 ? C19 C20 C15 . . 121.40(17) ? C19 C20 H23 . . 119.3 ? C15 C20 H23 . . 119.3 ? 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 C1 C6 . 1.392(3) ? C1 C2 . 1.398(2) ? C1 C7 . 1.485(2) ? C2 C3 . 1.380(2) ? C2 H1 . 0.9500 ? C3 C4 . 1.401(2) ? C3 H2 . 0.9500 ? C4 C5 . 1.404(2) ? C4 C15 . 1.494(2) ? O1 C7 . 1.217(2) ? O2 C8 . 1.231(2) ? N1 C8 . 1.342(2) ? N1 C9 . 1.485(2) ? N1 C12 . 1.489(2) ? C5 C6 . 1.388(2) ? C5 H3 . 0.9500 ? C6 H4 . 0.9500 ? C7 C8 . 1.535(2) ? C9 C10 . 1.519(3) ? C9 C11 . 1.519(3) ? C9 H5 . 1.0000 ? C10 H6 . 0.9800 ? C10 H7 . 0.9800 ? C10 H8 . 0.9800 ? C11 H9 . 0.9800 ? C11 H10 . 0.9800 ? C11 H11 . 0.9800 ? C12 C14 . 1.519(3) ? C12 C13 . 1.524(3) ? C12 H12 . 1.0000 ? C13 H13 . 0.9800 ? C13 H14 . 0.9800 ? C13 H15 . 0.9800 ? C14 H16 . 0.9800 ? C14 H17 . 0.9800 ? C14 H18 . 0.9800 ? C15 C20 . 1.399(3) ? C15 C16 . 1.404(2) ? C16 C17 . 1.386(3) ? C16 H19 . 0.9500 ? C17 C18 . 1.382(3) ? C17 H20 . 0.9500 ? C18 C19 . 1.382(3) ? C18 H21 . 0.9500 ? C19 C20 . 1.385(3) ? C19 H22 . 0.9500 ? C20 H23 . 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 C9 H5 O1 . 1.00 2.65 3.245(2) 119 yes C13 H15 O2 . 0.98 2.47 3.033(3) 117 yes C14 H16 O2 . 0.98 2.51 3.072(3) 116 yes C14 H18 O1 1_455 0.98 2.71 3.612(3) 154 yes C17 H20 O2 4_656 0.95 2.66 3.608(2) 179 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 1.2(2) ? C7 C1 C2 C3 . . . . -178.37(15) ? C1 C2 C3 C4 . . . . 0.3(2) ? C2 C3 C4 C5 . . . . -1.0(2) ? C2 C3 C4 C15 . . . . 178.55(15) ? C3 C4 C5 C6 . . . . 0.2(3) ? C15 C4 C5 C6 . . . . -179.27(16) ? C4 C5 C6 C1 . . . . 1.2(3) ? C2 C1 C6 C5 . . . . -1.9(2) ? C7 C1 C6 C5 . . . . 177.64(16) ? C6 C1 C7 O1 . . . . -171.73(18) ? C2 C1 C7 O1 . . . . 7.8(3) ? C6 C1 C7 C8 . . . . 3.1(2) ? C2 C1 C7 C8 . . . . -177.40(15) ? C9 N1 C8 O2 . . . . 178.42(19) ? C12 N1 C8 O2 . . . . -2.2(3) ? C9 N1 C8 C7 . . . . -3.9(2) ? C12 N1 C8 C7 . . . . 175.50(16) ? O1 C7 C8 O2 . . . . 97.1(2) ? C1 C7 C8 O2 . . . . -77.9(2) ? O1 C7 C8 N1 . . . . -80.7(2) ? C1 C7 C8 N1 . . . . 104.20(19) ? C8 N1 C9 C10 . . . . 110.4(2) ? C12 N1 C9 C10 . . . . -69.1(2) ? C8 N1 C9 C11 . . . . -123.57(18) ? C12 N1 C9 C11 . . . . 57.0(2) ? C8 N1 C12 C14 . . . . 65.9(2) ? C9 N1 C12 C14 . . . . -114.69(18) ? C8 N1 C12 C13 . . . . -61.6(2) ? C9 N1 C12 C13 . . . . 117.88(18) ? C3 C4 C15 C20 . . . . -179.53(16) ? C5 C4 C15 C20 . . . . -0.1(2) ? C3 C4 C15 C16 . . . . -0.4(2) ? C5 C4 C15 C16 . . . . 179.07(17) ? C20 C15 C16 C17 . . . . 0.6(3) ? C4 C15 C16 C17 . . . . -178.57(17) ? C15 C16 C17 C18 . . . . -1.1(3) ? C16 C17 C18 C19 . . . . 1.0(3) ? C17 C18 C19 C20 . . . . -0.3(3) ? C18 C19 C20 C15 . . . . -0.2(3) ? C16 C15 C20 C19 . . . . 0.0(2) ? C4 C15 C20 C19 . . . . 179.20(16) ? _cod_database_fobs_code 2243842