#------------------------------------------------------------------------------ #$Date: 2020-02-01 08:20:12 +0200 (Sat, 01 Feb 2020) $ #$Revision: 247446 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557210.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_1557210 loop_ _publ_author_name 'Dean, Raven' 'Miller, Chelsea N.' 'Zingales, Sarah K.' 'Padgett, Clifford W.' _publ_section_title ; 3-(4-Iodophenyl)-2,3-dihydro-1H-benzo[f]chromen-1-one ; _journal_coeditor_code HB4334 _journal_issue 1 _journal_name_full IUCrData _journal_page_first x200110 _journal_paper_doi 10.1107/S2414314620001108 _journal_volume 5 _journal_year 2020 _chemical_formula_iupac 'C19 H13 I O2' _chemical_formula_moiety 'C19 H13 I O2' _chemical_formula_sum 'C19 H13 I O2' _chemical_formula_weight 400.19 _chemical_name_systematic ; 3-(4-Iodophenyl)-2,3-dihydro-1H-benzo[f]chromen-1-one ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 104.947(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.0481(3) _cell_length_b 18.2185(8) _cell_length_c 12.6391(6) _cell_measurement_reflns_used 5447 _cell_measurement_temperature 170 _cell_measurement_theta_max 28.8050 _cell_measurement_theta_min 2.0100 _cell_volume 1568.02(12) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2018) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 170.0 _diffrn_detector_area_resol_mean 13.6612 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB mini' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23424 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.059 _diffrn_reflns_theta_min 2.008 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2018) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.768 _exptl_crystal_size_mid 0.343 _exptl_crystal_size_min 0.335 _refine_diff_density_max 0.724 _refine_diff_density_min -0.813 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 5656 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.123 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0451 _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^)+(0.0197P)^2^+1.6677P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.0962 _reflns_number_gt 3493 _reflns_number_total 5656 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb4334sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557210 _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 0.302 _shelx_estimated_absorpt_t_max 0.547 _shelx_hkl_file ; 0 0 2 479.51 9.60 0 0 -2 484.54 10.92 0 0 2 464.17 9.45 0 0 3 9.32 1.44 0 0 3 7.57 1.68 0 0 -3 8.31 2.11 0 0 -4 4199.49 46.40 0 0 4 4250.31 41.24 0 0 4 4271.59 40.97 0 0 -5 4.34 1.74 0 0 5 7.41 2.13 0 0 6 3990.73 49.22 0 0 6 3945.51 49.84 0 0 -6 3831.16 55.22 0 0 7 4.17 2.59 0 0 7 -0.37 2.69 0 0 -7 4.31 3.07 0 0 8 397.31 18.80 0 0 -8 436.94 21.93 0 0 8 382.23 18.32 0 0 9 21.48 7.30 0 0 9 16.02 5.71 0 0 -9 20.39 7.15 0 0 10 320.79 19.74 0 0 -10 326.72 22.38 0 0 10 356.14 20.89 0 0 11 3.82 2.60 0 0 11 1.26 1.79 0 0 12 169.04 17.08 0 0 -12 189.56 18.75 0 0 12 188.08 16.82 0 0 13 1.24 2.80 0 0 -13 9.31 5.41 0 0 13 9.91 5.74 0 0 -14 1.08 3.73 0 0 14 3.46 4.26 0 0 -15 14.59 9.04 0 0 15 20.47 8.95 0 0 -16 3.68 4.62 0 0 16 11.69 6.33 0 0 -17 -2.39 4.08 0 0 17 -0.57 4.32 0 0 18 11.39 7.60 0 0 -18 16.69 8.03 0 -1 1 162.92 4.50 0 1 2 538.28 11.05 0 1 -2 517.90 7.93 0 -1 2 517.19 7.08 0 1 -2 489.83 10.97 0 -1 -2 486.50 11.25 0 -1 2 503.41 9.75 0 1 2 518.63 10.81 0 1 3 4883.63 39.56 0 -1 -3 4832.52 42.88 0 -1 3 4876.07 37.17 0 1 -3 4811.53 42.27 0 -1 3 4863.16 23.03 0 1 3 4900.68 39.60 0 -1 4 129.51 3.96 0 1 -4 127.50 8.24 0 -1 -4 130.71 8.41 0 1 4 132.20 7.40 0 -1 4 125.37 7.12 0 1 4 128.00 7.43 0 -1 5 667.50 18.50 0 1 -5 682.40 21.13 0 -1 5 694.47 18.76 0 -1 -5 713.41 21.59 0 -1 5 689.77 9.45 0 1 5 699.75 19.15 0 1 5 669.57 19.11 0 1 6 44.23 6.55 0 1 -6 41.53 6.97 0 -1 -6 34.26 6.30 0 -1 6 43.54 6.40 0 1 6 26.44 4.88 0 -1 6 32.79 5.44 0 1 7 192.91 12.19 0 -1 7 230.67 12.96 0 -1 7 206.19 12.51 0 -1 7 204.60 5.00 0 1 7 197.90 12.28 0 -1 -7 214.90 14.18 0 1 -7 186.96 13.22 0 1 -8 114.32 11.47 0 1 8 117.23 10.95 0 -1 8 129.86 10.54 0 1 8 114.55 10.20 0 -1 -8 126.06 12.16 0 -1 8 124.55 10.06 0 1 9 596.59 24.56 0 -1 9 647.07 25.74 0 -1 9 575.97 23.80 0 1 9 568.13 24.77 0 1 -9 601.02 27.62 0 -1 -9 566.88 27.49 0 1 10 71.77 9.69 0 1 -10 81.39 10.84 0 -1 10 73.31 9.78 0 -1 -10 91.10 11.90 0 1 10 64.56 9.16 0 -1 10 77.98 10.54 0 -1 -11 26.24 7.35 0 1 11 27.76 6.55 0 1 -11 21.22 5.55 0 1 11 30.21 7.05 0 -1 11 25.88 6.01 0 -1 11 20.91 6.34 0 1 -12 32.24 8.83 0 -1 12 15.30 5.79 0 -1 12 13.79 5.27 0 1 12 17.99 6.95 0 -1 -12 30.57 8.49 0 -1 -13 63.21 12.16 0 1 13 51.92 9.96 0 -1 13 57.60 9.71 0 1 -13 66.33 12.18 0 -1 13 56.16 10.19 0 -1 -14 13.26 5.58 0 1 -14 16.90 5.77 0 1 14 12.16 4.60 0 -1 14 10.96 5.20 0 -1 14 14.05 5.43 0 1 -15 68.98 13.86 0 -1 15 60.88 12.29 0 -1 -15 52.35 12.33 0 1 15 69.30 13.13 0 -1 -16 11.36 6.66 0 1 16 3.45 4.55 0 -1 16 6.57 5.27 0 1 -16 8.66 7.28 0 -1 -17 2.24 4.24 0 1 17 -1.31 3.26 0 -1 17 0.22 2.63 0 1 -17 6.23 5.78 0 1 -18 -3.53 5.25 0 -1 -18 5.12 5.33 0 1 18 -3.69 4.47 0 -1 18 -1.88 3.35 0 -2 -1 748.41 11.23 0 -2 1 715.36 10.00 0 2 1 749.38 11.27 0 2 1 743.42 11.36 0 -2 1 766.34 11.59 0 2 -1 733.13 10.26 0 -2 -1 760.95 10.66 0 2 -1 740.68 9.29 0 -2 2 4422.82 28.08 0 2 -2 4461.34 33.55 0 -2 -2 4347.42 26.74 0 2 -2 4478.78 29.66 0 -2 -2 4469.11 34.93 0 2 2 4502.90 35.09 0 2 2 4362.42 26.41 0 2 -3 17.28 2.54 0 -2 3 15.64 2.24 0 2 3 14.50 2.28 0 -2 3 14.08 1.67 0 -2 -3 14.37 2.40 0 -2 -3 18.51 1.75 0 -2 4 756.62 17.14 0 -2 -4 739.62 10.26 0 -2 -4 733.96 19.71 0 2 4 714.53 18.42 0 -2 4 755.53 11.97 0 2 -4 738.68 19.23 0 -2 -5 1236.02 28.80 0 -2 5 1260.07 15.83 0 2 -5 1241.90 28.13 0 -2 5 1260.51 24.94 0 2 5 1229.25 26.51 0 2 5 1297.74 26.62 0 -2 -6 1358.90 33.21 0 -2 6 1361.17 16.72 0 -2 6 1385.20 29.41 0 2 6 1376.02 30.39 0 2 -6 1470.63 33.96 0 2 6 1421.25 31.14 0 -2 7 179.81 11.55 0 2 -7 199.32 13.53 0 -2 -7 176.51 13.15 0 2 7 173.60 12.41 0 2 7 174.68 11.85 0 -2 7 176.89 11.74 0 -2 7 168.31 5.90 0 -2 8 84.47 8.94 0 2 -8 86.20 11.69 0 2 8 84.37 9.33 0 -2 8 62.01 3.46 0 2 8 94.39 10.46 0 -2 -8 86.91 11.46 0 -2 8 87.06 10.45 0 2 9 12.28 4.17 0 -2 9 10.26 3.73 0 2 -9 9.56 4.68 0 -2 9 11.74 3.10 0 -2 -9 6.85 3.79 0 -2 10 138.71 13.22 0 -2 -10 164.44 16.02 0 2 -10 160.48 14.87 0 2 10 129.55 13.20 0 -2 10 134.70 12.11 0 -2 11 206.58 16.78 0 -2 -11 191.94 17.60 0 -2 11 221.35 17.20 0 2 11 177.68 16.67 0 2 -11 190.74 17.74 0 -2 12 100.13 12.60 0 2 12 65.82 10.94 0 2 -12 82.95 12.21 0 -2 12 75.20 10.52 0 -2 -12 74.78 12.35 0 -2 13 29.02 7.62 0 -2 -13 50.94 11.23 0 2 -13 33.40 9.05 0 -2 13 34.63 8.13 0 2 13 35.25 8.74 0 2 -14 -9.05 5.70 0 -2 -14 7.85 5.96 0 2 14 6.82 4.40 0 -2 14 4.59 3.39 0 -2 14 0.24 2.72 0 2 -15 5.20 4.91 0 -2 15 10.37 6.10 0 -2 -15 14.98 7.36 0 -2 15 5.56 4.78 0 2 15 6.11 5.21 0 2 16 22.96 8.75 0 -2 16 27.73 9.75 0 -2 -16 28.54 9.51 0 2 -16 27.34 9.12 0 2 -17 -4.65 4.64 0 2 17 6.08 6.17 0 -2 -17 2.96 4.03 0 -2 17 12.83 6.90 0 2 -18 -1.45 5.34 0 -2 18 -4.72 4.45 0 -2 -18 0.98 6.27 0 2 18 6.56 6.06 0 -3 0 4.42 1.09 0 -3 0 3.66 0.68 0 -3 -1 586.73 10.02 0 -3 1 602.44 12.57 0 3 -1 584.02 9.99 0 3 -1 617.70 9.83 0 3 1 596.94 11.47 0 -3 -1 607.49 12.48 0 -3 -2 5618.35 37.69 0 -3 2 5731.04 38.75 0 -3 -2 5693.76 40.54 0 3 2 5702.95 42.35 0 3 -2 5613.99 39.03 0 3 -2 5753.23 34.72 0 3 3 1311.59 23.35 0 -3 3 1330.69 18.70 0 3 -3 1314.12 22.60 0 -3 -3 1306.07 23.31 0 3 -3 1340.87 20.05 0 -3 3 1314.73 19.72 0 -3 -3 1325.86 18.05 0 -3 -4 3672.55 29.32 0 3 4 3675.92 43.53 0 -3 -4 3665.57 44.61 0 -3 4 3709.52 31.51 0 -3 4 3757.04 38.19 0 3 -4 3797.54 44.10 0 -3 -5 440.61 17.52 0 3 -5 460.96 17.29 0 -3 -5 431.69 9.56 0 -3 5 451.93 14.99 0 3 5 463.72 16.87 0 -3 5 467.06 11.39 0 -3 -6 10.88 1.29 0 -3 6 12.58 1.94 0 -3 6 14.38 2.85 0 3 6 11.18 2.77 0 -3 -6 12.71 3.79 0 3 -6 16.00 4.32 0 3 -7 461.36 20.69 0 3 7 421.91 19.02 0 -3 7 441.72 18.10 0 -3 -7 453.49 21.35 0 -3 7 421.99 11.04 0 3 -8 1618.78 42.04 0 3 8 1647.05 39.68 0 -3 -8 1611.26 42.12 0 -3 8 1702.89 37.68 0 3 9 0.10 2.98 0 3 -9 7.15 2.66 0 -3 9 7.14 2.57 0 -3 9 0.13 2.08 0 -3 -9 2.38 2.06 0 3 10 236.61 17.39 0 -3 10 252.63 17.38 0 -3 -10 236.55 19.34 0 -3 10 245.97 16.78 0 3 -10 273.59 19.51 0 3 -11 21.07 7.42 0 -3 11 29.51 7.49 0 3 11 28.80 8.00 0 -3 11 23.85 7.93 0 -3 -11 30.49 9.05 0 -3 -12 7.27 4.59 0 -3 12 4.22 3.15 0 3 -12 6.97 3.25 0 3 12 11.97 5.27 0 -3 12 14.57 5.00 0 3 -13 28.34 8.69 0 -3 13 22.01 6.78 0 -3 13 32.56 8.93 0 -3 -13 40.33 9.00 0 3 13 29.73 8.38 0 3 14 13.69 5.36 0 3 -14 16.72 6.54 0 -3 14 19.71 6.85 0 -3 -14 5.79 5.60 0 -3 14 19.55 5.93 0 -3 -15 -0.89 3.10 0 3 -15 8.67 6.17 0 -3 15 3.16 2.65 0 -3 15 1.12 4.19 0 3 15 -3.70 5.00 0 3 -16 24.56 8.24 0 -3 16 22.19 7.83 0 3 16 33.64 10.80 0 -3 16 40.93 11.32 0 -3 -16 24.22 9.63 0 -3 17 0.90 3.50 0 3 17 2.77 3.21 0 -3 -17 3.08 3.99 0 3 -17 -0.14 3.91 0 3 18 -1.06 5.51 0 -3 18 4.95 5.43 0 3 -18 2.78 5.04 0 -3 -18 -5.46 5.23 0 4 0 3.42 0.96 0 -4 0 7.05 1.36 0 4 0 5.48 1.12 0 -4 1 2090.86 26.85 0 4 -1 2061.59 20.68 0 -4 -1 2084.04 20.34 0 4 1 2081.37 23.95 0 4 -1 2107.78 20.59 0 -4 -1 2073.74 26.87 0 -4 -2 184.68 8.00 0 4 -2 199.74 7.63 0 4 2 191.82 8.25 0 4 -2 196.79 6.85 0 -4 2 212.02 8.73 0 -4 -2 196.51 7.56 0 4 -3 28.27 2.97 0 4 -3 28.16 3.40 0 -4 3 28.95 3.34 0 -4 -3 29.91 3.20 0 4 3 27.88 3.65 0 -4 -3 28.87 3.57 0 -4 -4 15.38 3.32 0 -4 4 15.36 2.50 0 4 4 17.12 3.31 0 -4 4 17.01 2.99 0 -4 -4 16.72 2.49 0 4 -4 15.16 3.20 0 4 -4 18.74 3.18 0 4 -5 2156.09 37.60 0 -4 5 2094.30 27.31 0 -4 -5 2039.66 37.35 0 -4 -5 2040.25 25.11 0 -4 5 2156.63 32.72 0 4 5 2134.37 37.54 0 -4 -6 11.17 2.78 0 4 6 8.71 2.80 0 -4 -6 7.52 1.46 0 -4 6 8.95 2.56 0 -4 6 7.97 1.75 0 4 -6 6.74 1.79 0 -4 -7 696.24 12.11 0 -4 7 719.93 16.17 0 4 7 741.94 25.31 0 -4 -7 699.22 26.32 0 4 -7 753.72 26.61 0 -4 7 755.78 23.18 0 4 8 26.83 7.79 0 4 -8 36.33 8.45 0 -4 -8 29.68 7.72 0 -4 8 20.10 3.21 0 -4 8 34.20 7.51 0 4 9 54.67 7.88 0 -4 9 54.84 4.53 0 -4 -9 55.88 8.48 0 4 -9 52.19 8.51 0 -4 9 65.32 7.80 0 4 -10 6.86 4.63 0 -4 10 18.22 5.27 0 -4 -10 14.53 4.85 0 -4 10 4.57 3.14 0 4 10 13.50 4.64 0 -4 11 322.20 20.62 0 4 11 325.10 21.63 0 4 -11 303.45 22.92 0 -4 11 323.67 20.23 0 -4 -11 319.11 22.64 0 -4 12 2.48 2.88 0 -4 12 -1.30 2.09 0 4 -12 -4.72 4.93 0 -4 -12 -2.54 3.81 0 4 12 -7.54 5.37 0 4 13 98.32 13.54 0 -4 13 89.45 12.93 0 -4 13 90.13 12.23 0 4 -13 84.03 13.38 0 -4 -13 96.86 14.33 0 -4 14 6.08 5.45 0 4 -14 -3.59 3.65 0 -4 14 12.50 5.97 0 4 14 9.27 5.32 0 -4 -14 13.14 6.45 0 4 15 9.17 5.73 0 4 -15 15.06 6.13 0 -4 15 12.23 6.79 0 -4 -15 14.75 6.27 0 -4 15 12.54 6.37 0 4 16 6.96 5.66 0 -4 -16 5.65 6.24 0 -4 16 11.16 6.35 0 4 -16 5.21 5.67 0 -4 16 3.00 3.19 0 -4 17 23.21 9.84 0 4 17 16.07 8.74 0 -4 -17 21.52 9.31 0 4 -17 9.14 7.86 0 4 -18 1.55 3.82 0 4 18 -0.32 5.18 0 -4 -18 -1.32 3.75 0 5 0 0.25 0.60 0 -5 0 1.29 1.56 0 5 0 1.56 0.74 0 5 1 164.21 7.29 0 -5 1 172.46 8.60 0 -5 -1 162.62 6.19 0 5 -1 169.03 6.44 0 5 -1 160.64 6.35 0 -5 -1 164.21 8.35 0 -5 2 3596.19 39.42 0 5 -2 3639.63 31.51 0 -5 -2 3565.69 39.52 0 -5 -2 3641.11 33.81 0 5 -2 3462.71 33.60 0 5 2 3529.42 37.65 0 -5 -3 910.30 19.86 0 5 3 887.58 21.15 0 -5 3 892.45 19.55 0 5 -3 879.42 19.46 0 5 -3 901.63 17.41 0 -5 -3 896.44 19.63 0 -5 4 1249.37 23.19 0 5 -4 1225.15 25.79 0 -5 -4 1235.83 22.74 0 5 -4 1250.24 22.82 0 5 4 1217.54 27.30 0 -5 -4 1184.73 25.77 0 -5 -5 153.47 10.29 0 -5 5 149.21 8.99 0 -5 -5 175.60 8.40 0 -5 5 166.74 8.60 0 5 -5 154.03 9.24 0 5 5 170.46 10.93 0 5 -5 165.51 10.68 0 5 -6 256.85 14.54 0 -5 -6 265.24 14.96 0 -5 -6 248.25 9.68 0 5 6 249.29 14.82 0 -5 6 251.06 10.53 0 -5 6 250.24 12.72 0 -5 7 429.57 18.19 0 -5 -7 441.81 11.84 0 -5 7 442.66 14.19 0 5 -7 436.04 20.75 0 5 7 463.60 20.64 0 -5 -7 466.61 21.31 0 -5 8 590.67 22.67 0 5 -8 639.03 26.68 0 -5 -8 594.92 25.61 0 5 8 551.65 24.83 0 -5 8 573.78 15.98 0 -5 9 26.23 3.35 0 -5 9 27.35 5.47 0 -5 -9 29.73 6.03 0 5 9 25.69 5.72 0 5 -9 28.82 6.09 0 5 -10 91.66 11.80 0 -5 -10 81.41 10.73 0 -5 10 88.25 10.52 0 5 10 66.07 9.56 0 5 11 52.99 9.63 0 -5 11 64.54 10.26 0 -5 -11 56.88 10.01 0 -5 11 50.63 8.93 0 5 -11 60.46 10.85 0 5 -12 0.81 2.92 0 -5 12 2.86 3.05 0 -5 -12 9.13 5.10 0 -5 12 6.70 2.94 0 5 12 2.93 1.80 0 -5 13 5.95 2.88 0 5 13 6.92 4.65 0 -5 13 11.77 5.05 0 5 -13 5.16 4.84 0 -5 -13 8.79 4.30 0 -5 14 56.75 10.95 0 5 -14 41.16 10.49 0 5 14 51.55 10.66 0 -5 14 38.61 8.69 0 -5 -14 46.60 10.10 0 -5 15 1.66 2.88 0 5 15 0.10 3.27 0 -5 -15 4.54 4.62 0 -5 15 5.55 2.89 0 5 -15 -0.41 3.22 0 -5 -16 6.38 5.48 0 5 16 8.35 5.51 0 -5 16 12.96 6.97 0 5 -16 1.03 4.68 0 -5 16 4.58 3.89 0 5 17 2.90 5.95 0 -5 -17 -0.65 3.87 0 5 -17 4.59 5.81 0 -5 17 4.64 4.78 0 5 18 -3.52 5.28 0 -5 -18 -11.43 8.47 0 5 -18 1.42 4.25 0 -6 0 3894.52 44.99 0 6 0 3930.96 35.14 0 6 0 3819.50 32.18 0 6 -1 650.04 13.94 0 -6 -1 622.55 13.10 0 -6 -1 608.29 17.86 0 6 1 623.39 13.61 0 6 -1 625.75 13.58 0 -6 1 620.80 17.98 0 6 1 631.26 15.40 0 6 -2 435.35 11.91 0 6 -2 437.86 12.55 0 -6 2 446.97 15.31 0 -6 -2 453.35 12.53 0 6 2 434.20 14.03 0 -6 -2 434.86 15.13 0 -6 -3 48.34 5.22 0 6 -3 43.81 4.07 0 -6 -3 46.94 4.67 0 6 -3 49.46 4.78 0 -6 3 53.82 5.79 0 6 3 40.33 4.96 0 6 -4 475.30 14.65 0 6 4 505.17 17.98 0 6 -4 521.76 17.24 0 -6 4 487.59 16.02 0 -6 -4 507.59 15.99 0 -6 -4 452.50 16.26 0 -6 5 252.82 11.75 0 6 -5 294.63 14.18 0 -6 -5 281.20 11.78 0 6 -5 265.53 12.14 0 -6 -5 293.99 14.13 0 6 5 279.43 14.60 0 -6 5 277.44 12.03 0 -6 6 979.67 24.45 0 -6 -6 961.06 28.07 0 6 6 995.27 29.05 0 6 -6 1016.85 29.01 0 -6 6 944.34 22.31 0 -6 -6 954.97 21.27 0 -6 -7 187.48 13.81 0 6 -7 180.04 13.52 0 -6 7 187.48 12.03 0 -6 7 184.89 10.07 0 -6 -7 180.93 8.88 0 6 7 178.28 13.28 0 6 8 408.89 20.97 0 -6 8 395.28 14.67 0 -6 -8 371.15 11.47 0 6 -8 433.01 21.96 0 -6 -8 369.27 20.43 0 -6 8 392.19 18.51 0 -6 9 13.46 5.24 0 6 9 11.24 5.81 0 -6 9 8.86 2.77 0 6 -9 12.62 6.75 0 -6 -9 17.12 6.39 0 -6 10 94.32 10.13 0 -6 -10 105.20 12.17 0 6 10 88.24 11.29 0 -6 10 79.07 6.28 0 6 -10 93.29 11.99 0 -6 11 105.04 12.58 0 6 11 116.04 13.90 0 6 -11 129.50 14.87 0 -6 11 132.14 13.40 0 -6 -11 108.61 13.24 0 -6 -12 35.62 8.62 0 -6 12 38.27 7.84 0 6 -12 32.86 7.63 0 -6 12 34.43 7.16 0 6 12 39.48 8.31 0 -6 13 8.17 3.79 0 -6 -13 1.83 2.91 0 -6 13 8.12 3.03 0 6 -13 0.97 2.50 0 6 13 6.14 4.89 0 -6 14 4.21 4.63 0 -6 14 -0.94 2.85 0 6 14 -1.78 3.80 0 -6 -14 1.51 3.71 0 6 -14 1.77 4.09 0 6 -15 4.09 3.06 0 6 15 9.75 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109.65 13.56 -5 12 8 97.67 12.87 5 -12 -8 109.19 15.18 5 12 -7 19.12 7.07 -5 -12 7 3.69 1.70 -5 12 7 10.19 5.79 5 -12 -7 9.61 5.36 5 12 -6 8.44 3.55 -5 -12 6 17.63 5.22 -5 12 6 12.05 5.08 5 -12 -6 14.50 4.96 -5 -12 5 21.43 6.87 5 12 -5 13.41 5.37 -5 12 5 17.21 5.87 5 -12 -5 18.81 6.64 5 -12 -4 289.43 23.39 -5 -12 4 284.24 20.38 5 12 -4 300.58 21.32 -5 12 4 286.97 20.03 -5 -12 3 8.98 4.32 -5 12 3 7.53 2.76 5 -12 -3 7.70 4.73 5 12 -3 1.39 4.32 -5 -12 2 235.37 18.55 5 12 -2 231.29 18.23 -5 12 2 227.06 17.54 5 -12 -2 237.31 21.14 5 12 -1 12.17 1.88 -5 -12 1 27.10 6.43 -5 12 1 24.88 5.47 5 -12 -1 15.00 3.44 -5 -12 0 32.10 6.72 -5 12 0 30.07 5.30 5 12 0 31.43 7.27 5 -12 0 30.85 7.73 -5 -12 -1 4.04 1.98 -5 12 -1 16.11 4.09 5 -12 1 18.31 6.51 5 12 1 13.73 4.56 5 12 2 297.85 21.57 -5 -12 -2 254.40 19.52 -5 12 -2 260.96 18.86 5 -12 2 271.15 22.31 -5 -12 -3 14.59 4.38 -5 12 -3 17.36 4.73 5 12 3 17.70 5.82 5 -12 3 3.38 2.75 5 12 4 53.26 9.69 -5 -12 -4 62.03 9.29 -5 12 -4 49.76 8.43 5 -12 4 63.40 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8.51 6.36 8 -7 -9 7.96 5.12 -8 -7 9 12.77 6.03 -8 7 9 4.80 4.46 8 7 -9 8.52 5.83 8 -7 -8 6.50 4.24 8 7 -8 0.99 4.52 -8 -7 8 3.15 3.68 -8 7 8 0.39 2.34 8 -7 -7 11.53 6.70 8 7 -7 9.71 3.65 -8 -7 7 3.09 3.36 -8 7 7 7.27 3.80 8 -7 -6 17.71 7.20 -8 -7 6 7.84 5.26 8 7 -6 5.10 5.18 -8 7 6 12.65 4.65 8 -7 -5 74.59 13.29 -8 -7 5 81.91 12.64 8 7 -5 64.02 11.44 -8 7 5 78.20 11.08 -8 -7 4 -2.66 2.72 -8 7 4 -4.06 3.29 8 7 -4 -9.10 5.45 8 -7 -4 0.31 3.15 -8 -7 3 123.08 15.63 -8 7 3 115.37 12.92 8 7 -3 142.94 16.61 8 -7 -3 136.98 17.81 8 7 -2 -9.89 6.14 -8 -7 2 -3.59 3.61 -8 7 2 -4.14 3.80 8 -7 -2 5.18 4.40 -8 -7 1 7.00 3.13 8 7 -1 1.67 4.06 -8 7 1 7.68 3.52 8 -7 -1 3.37 3.42 -8 -7 0 5.34 3.13 8 7 0 14.07 5.61 -8 7 0 7.52 2.71 8 -7 0 15.25 5.97 -8 -7 -1 133.17 16.38 -8 7 -1 112.29 13.31 8 7 1 129.47 16.23 8 -7 1 129.13 17.92 -8 -7 -2 1.82 3.90 -8 7 -2 -2.54 2.10 8 7 2 -6.03 5.41 8 -7 2 4.61 3.30 8 7 3 59.12 11.91 -8 7 -3 70.93 11.55 8 -7 3 82.25 14.61 8 -7 4 -9.31 6.05 8 7 4 -2.43 4.05 -8 7 -4 -1.36 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4.49 8 -10 -8 15.26 7.47 8 10 -7 36.12 9.62 -8 -10 7 29.04 7.91 -8 10 7 24.07 7.47 8 -10 -7 27.61 9.32 -8 -10 6 12.82 6.07 8 10 -6 5.04 3.77 -8 10 6 16.35 6.21 8 -10 -6 20.62 8.44 -8 -10 5 8.68 4.82 8 10 -5 9.64 4.54 -8 10 5 12.39 4.63 8 -10 -5 14.44 7.00 -8 -10 4 3.65 4.46 -8 10 4 2.45 3.40 8 10 -4 -5.43 5.47 8 -10 -4 9.91 5.11 -8 -10 3 4.52 3.70 -8 10 3 1.06 2.79 8 10 -3 -4.31 5.30 8 -10 -3 6.94 5.27 8 10 -2 10.90 4.89 -8 -10 2 12.07 5.32 -8 10 2 13.37 5.06 8 -10 -2 8.89 5.53 8 10 -1 96.13 14.92 -8 -10 1 87.37 14.01 -8 10 1 100.22 13.40 8 -10 -1 115.41 18.34 -8 -10 0 33.76 8.74 8 10 0 10.80 4.68 -8 10 0 22.43 6.45 8 -10 0 36.22 10.29 -8 -10 -1 30.45 8.52 8 10 1 38.72 10.22 -8 10 -1 40.38 8.48 8 -10 1 43.59 11.18 -8 10 -2 6.50 3.68 8 10 2 11.57 4.11 8 -10 2 8.68 6.14 -8 10 -3 1.69 3.05 8 10 3 4.80 3.06 8 -10 3 3.11 4.58 8 10 4 1.14 3.44 -8 10 -4 -0.57 3.65 8 -10 5 113.02 15.68 8 10 5 94.58 16.21 -8 10 -5 93.40 14.63 8 10 6 10.70 5.68 8 11 -13 2.11 4.80 -8 -11 12 1.33 3.25 8 11 -12 9.55 5.97 -8 -11 11 -1.24 4.04 8 11 -11 -2.85 3.57 8 -11 -11 -0.58 3.77 -8 -11 10 8.42 5.34 -8 11 10 12.23 6.47 8 11 -10 6.50 4.43 8 -11 -10 8.17 6.94 8 11 -9 -8.46 5.73 -8 -11 9 4.73 5.23 -8 11 9 5.62 4.70 8 -11 -9 -1.67 5.24 8 11 -8 -1.47 2.95 -8 -11 8 1.36 2.90 -8 11 8 9.11 5.36 8 -11 -8 3.04 4.18 8 11 -7 4.04 4.55 -8 -11 7 10.78 5.36 -8 11 7 -0.13 2.40 8 -11 -7 -2.28 4.08 -8 -11 6 6.08 4.63 8 11 -6 -4.62 5.38 -8 11 6 -1.84 3.65 8 -11 -6 2.62 5.45 -8 -11 5 -6.93 4.40 8 11 -5 -3.05 3.68 -8 11 5 -1.02 2.54 -8 -11 4 57.54 11.33 -8 11 4 46.38 9.59 8 11 -4 43.85 10.09 8 -11 -4 66.18 14.13 -8 -11 3 -2.21 3.51 -8 11 3 -12.06 6.65 8 11 -3 -10.87 6.40 8 -11 -3 2.22 5.46 -8 -11 2 16.14 7.18 -8 11 2 12.76 5.51 8 -11 -2 18.73 8.97 8 11 -2 15.47 6.99 8 11 -1 1.01 3.57 -8 -11 1 4.52 3.78 -8 11 1 2.95 2.93 8 -11 -1 0.74 2.72 -8 -11 0 16.77 6.62 8 11 0 15.73 6.30 -8 11 0 23.56 7.29 8 -11 0 11.31 6.65 -8 -11 -1 8.42 5.11 8 11 1 -10.70 6.36 -8 11 -1 -8.56 5.73 8 -11 1 8.02 6.93 -8 11 -2 72.45 12.19 8 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3.61 9 -12 -5 -12.14 7.27 -9 -12 4 5.02 4.28 9 12 -4 4.43 4.55 9 -12 -4 3.03 7.10 -9 -12 3 9.12 5.07 9 12 -3 11.05 6.14 9 -12 -3 3.13 5.91 -9 -12 2 9.01 5.27 9 12 -2 5.80 6.05 9 -12 -2 10.78 7.37 9 12 -1 0.42 4.48 9 -12 -1 -1.68 5.49 9 12 0 5.18 4.97 9 12 1 0.93 4.65 9 13 -9 5.42 5.78 -9 -13 9 -7.91 6.44 9 13 -8 0.50 3.86 -9 -13 8 1.09 3.89 9 -13 -8 -7.65 5.35 -9 -13 7 -5.80 5.60 9 -13 -7 0.65 3.61 -9 -13 6 -2.54 3.32 9 13 -6 13.81 7.13 9 -13 -6 6.71 6.32 -9 -13 5 -0.55 4.02 9 13 -5 5.43 5.22 9 -13 -5 8.74 6.75 -9 -13 4 -1.71 3.51 9 13 -4 4.69 4.62 9 -13 -4 -0.65 4.04 -9 -13 3 -2.28 4.96 9 13 -3 -4.34 5.32 9 -13 -3 -0.44 4.34 9 13 -2 -0.06 4.08 9 -13 -2 2.69 4.95 9 -13 -1 6.54 6.03 9 13 -1 18.48 6.99 9 13 0 11.64 7.53 9 14 -8 4.09 5.34 -9 -14 8 0.12 3.27 9 -14 -8 2.73 6.97 9 14 -7 -0.38 2.94 -9 -14 7 0.75 3.51 9 -14 -7 9.78 6.38 -9 -14 6 -2.06 4.74 9 14 -6 -8.24 5.78 9 -14 -6 5.92 5.48 -9 -14 5 -0.63 4.40 9 14 -5 7.90 7.30 9 -14 -5 13.51 7.92 -9 -14 4 -4.99 5.23 9 14 -4 7.14 5.34 9 -14 -4 4.77 5.16 9 14 -3 5.22 5.54 9 -14 -3 8.03 6.61 9 14 -2 0.82 3.44 9 -14 -2 0.85 5.41 9 14 -1 -1.21 4.63 -9 -15 6 8.05 6.48 9 15 -6 3.66 4.57 9 -15 -6 4.74 6.75 9 15 -5 0.58 3.37 9 -15 -5 -2.66 7.46 9 15 -4 1.80 4.35 9 -15 -4 7.15 7.38 9 15 -3 2.88 4.49 9 -15 -3 0.47 5.43 10 0 -10 -2.61 4.11 -10 0 10 0.31 2.86 10 0 -9 -1.45 3.94 -10 0 9 6.64 5.82 10 0 -8 7.32 5.34 -10 0 8 5.19 6.15 10 0 -7 -2.18 5.55 -10 0 7 -3.25 4.77 10 0 -6 32.55 10.70 -10 0 6 24.37 8.61 10 0 -5 3.18 4.58 -10 0 5 -1.53 3.38 10 0 -4 10.52 6.78 -10 0 4 -0.12 3.32 10 0 -3 -5.31 5.99 -10 0 3 -1.12 2.78 10 0 -2 13.23 6.64 -10 0 2 19.57 7.30 10 0 -1 -5.66 6.39 10 -1 -10 1.81 4.47 10 1 -10 2.61 3.86 -10 1 10 7.70 6.43 -10 -1 10 2.71 4.50 10 -1 -9 8.99 7.10 10 1 -9 -4.86 6.87 -10 1 9 11.91 7.38 -10 -1 9 4.31 3.69 10 -1 -8 0.07 3.65 10 1 -8 -2.39 6.27 -10 1 8 6.35 5.11 -10 -1 8 5.75 3.83 10 -1 -7 2.84 3.93 10 1 -7 -0.26 4.05 -10 1 7 1.41 5.04 -10 -1 7 1.72 3.88 10 -1 -6 8.86 5.49 10 1 -6 2.54 5.63 -10 1 6 0.70 4.12 -10 -1 6 2.24 4.97 10 -1 -5 21.08 9.03 10 1 -5 14.62 6.83 -10 1 5 18.38 8.31 -10 -1 5 5.66 4.31 10 -1 -4 2.64 3.29 10 1 -4 -8.17 7.22 -10 1 4 -2.40 4.76 -10 -1 4 -0.53 4.37 10 -1 -3 18.57 7.80 10 1 -3 16.54 6.91 -10 -1 3 26.04 8.14 10 -1 -2 -0.32 4.12 10 1 -2 -3.06 5.20 -10 -1 2 0.54 4.21 10 -1 -1 1.89 3.56 10 -2 -10 2.44 4.84 -10 -2 10 0.74 3.02 10 -2 -9 5.21 3.07 -10 -2 9 3.94 6.25 10 -2 -8 9.82 6.74 -10 2 8 -0.83 4.03 -10 -2 8 1.80 3.55 10 -2 -7 3.66 3.54 -10 2 7 -1.59 2.89 -10 -2 7 -2.79 4.93 10 -2 -6 12.34 7.06 -10 -2 6 7.02 4.85 10 -2 -5 -1.10 4.91 -10 -2 5 4.15 5.52 10 -2 -4 -2.92 5.56 -10 -2 4 -1.25 4.05 10 -2 -3 4.50 5.12 10 2 -3 -0.51 5.28 -10 -2 3 -0.18 3.85 10 -2 -2 12.67 5.67 10 2 -2 6.97 4.20 -10 -2 2 10.54 6.31 10 -2 -1 11.91 5.34 10 -3 -10 12.77 7.91 -10 -3 10 0.99 3.20 10 -3 -9 -2.69 5.90 -10 -3 9 -0.18 3.56 10 -3 -8 -2.85 4.18 -10 -3 8 5.30 5.85 10 -3 -7 1.97 5.16 -10 -3 7 2.30 3.76 10 -3 -6 -12.05 7.48 -10 -3 6 1.71 3.64 10 -3 -5 -4.20 4.91 -10 -3 5 -2.54 3.97 10 -3 -4 25.47 9.03 -10 -3 4 41.96 11.19 10 -3 -3 -1.92 5.41 -10 -3 3 -4.55 6.28 10 -3 -2 -0.73 3.73 -10 -3 2 1.99 5.17 10 -4 -10 2.69 5.47 -10 -4 10 -9.32 5.47 10 -4 -9 2.38 5.67 -10 -4 9 0.73 3.97 10 -4 -8 -1.07 4.81 -10 -4 8 -8.12 6.26 10 -4 -7 10.51 6.18 -10 -4 7 10.42 6.07 10 -4 -6 -1.20 3.70 -10 -4 6 -4.13 4.00 10 -4 -5 -1.00 4.66 -10 -4 5 0.65 3.32 10 -4 -4 -1.53 4.14 -10 -4 4 -2.08 3.62 10 -4 -3 9.14 6.15 -10 -4 3 -3.83 5.59 10 -4 -2 -0.47 4.14 -10 -4 2 6.15 4.56 10 -5 -10 16.20 8.55 -10 -5 10 8.99 5.67 10 -5 -9 -0.14 4.67 -10 -5 9 -7.50 6.46 10 -5 -8 12.75 6.67 -10 -5 8 4.81 4.37 10 -5 -7 3.45 6.11 -10 -5 7 -0.95 4.43 10 -5 -6 3.85 6.08 -10 -5 6 2.38 3.40 10 -5 -5 -2.98 6.13 -10 -5 5 0.59 2.37 10 -5 -4 23.38 9.42 -10 -5 4 6.69 4.43 -10 -5 3 30.58 10.11 10 -5 -3 16.86 8.96 -10 -5 2 6.68 5.81 10 -5 -2 6.79 5.12 -10 -6 10 6.95 6.37 10 -6 -9 7.43 7.07 -10 -6 9 -5.30 5.54 10 -6 -8 -0.83 5.20 -10 -6 8 5.58 6.41 10 -6 -7 -3.03 5.64 -10 -6 7 9.87 6.28 -10 -6 6 2.40 4.93 10 -6 -6 1.79 4.76 -10 -6 5 1.51 3.28 10 -6 -5 -2.96 4.82 -10 -6 4 5.81 5.15 10 -6 -4 1.25 5.01 -10 -6 3 9.13 4.59 10 -6 -3 3.85 6.86 10 -6 -2 13.98 7.69 -10 -7 9 -1.00 3.36 10 -7 -9 2.29 5.06 -10 -7 8 -0.86 3.54 10 -7 -8 1.91 5.11 -10 -7 7 2.87 3.56 10 -7 -7 0.42 4.32 -10 -7 6 1.40 3.07 10 -7 -6 0.56 4.98 -10 -7 5 16.16 6.13 10 -7 -5 18.87 8.22 -10 -7 4 -0.25 3.32 10 -7 -4 2.90 6.30 -10 -7 3 -3.89 4.75 10 -7 -3 14.47 8.26 10 -7 -2 -2.73 6.82 -10 -8 9 3.16 4.21 -10 -8 8 3.93 4.90 10 -8 -8 7.49 6.67 -10 -8 7 -3.10 4.18 10 -8 -7 2.08 4.27 -10 -8 6 12.44 8.60 10 -8 -6 4.65 6.48 -10 -8 5 -0.56 3.96 10 -8 -5 -5.75 5.86 -10 -8 4 0.56 3.30 10 -8 -4 2.17 4.89 10 -8 -3 4.38 6.30 -10 -9 8 10.24 6.46 10 -9 -8 -8.54 6.37 -10 -9 7 8.54 6.00 10 -9 -7 2.27 5.52 -10 -9 6 1.08 4.73 10 -9 -6 4.41 5.45 -10 -9 5 -3.87 4.00 10 -9 -5 13.77 7.80 10 -9 -4 -0.82 3.29 10 -9 -3 10.45 7.74 10 -10 -7 -3.55 6.12 10 -10 -6 3.47 4.51 10 -10 -5 0.30 4.92 10 -10 -4 6.10 5.91 0 0 0 0.00 0.00 TITL x1030b in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 7.048063 18.218545 12.639143 90.0000 104.9472 90.0000 ZERR 22.00 0.000258 0.000832 0.000613 0.0000 0.0043 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C N O I UNIT 22.00 22.00 22.00 22.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6508 _shelx_res_file ; TITL x1030b_a.res in P2(1)/n i.res created by SHELXL-2018/1 at 12:22:06 on 22-Dec-2019 REM Old TITL x1030b in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.169, Rweak 0.214, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C19 O2 I CELL 0.71073 7.0481 18.2185 12.6391 90 104.947 90 ZERR 4 0.0003 0.0008 0.0006 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H I O UNIT 76 52 4 8 L.S. 10 PLAN 5 SIZE 0.335 0.343 0.768 TEMP -103.15 list 4 fmap 2 53 acta bond $H REM REM REM WGHT 0.019700 1.667700 FVAR 0.46299 I1 3 -0.509484 0.433923 0.163355 11.00000 0.04458 0.06445 = 0.06874 -0.01116 -0.00216 -0.00698 O1 4 0.355095 0.600409 0.449183 11.00000 0.04143 0.04011 = 0.06262 0.00698 -0.00870 -0.00477 C1 1 0.383789 0.756214 0.430187 11.00000 0.04239 0.04583 = 0.05628 0.00396 0.00297 0.00269 O2 4 0.385510 0.822692 0.424564 11.00000 0.05884 0.04144 = 0.10257 0.00911 -0.00936 0.00455 C2 1 0.200587 0.713587 0.376446 11.00000 0.04174 0.04845 = 0.07173 0.00767 -0.00649 0.00187 AFIX 23 H2A 2 0.111796 0.713332 0.425697 11.00000 -1.20000 H2B 2 0.131632 0.738742 0.307874 11.00000 -1.20000 AFIX 0 C3 1 0.242639 0.635793 0.350465 11.00000 0.03841 0.05247 = 0.04806 0.00269 0.00095 -0.00040 AFIX 13 H3 2 0.323461 0.636549 0.296041 11.00000 -1.20000 AFIX 0 C4 1 0.519612 0.636854 0.504814 11.00000 0.03641 0.03969 = 0.04687 0.00269 0.00648 -0.00304 C5 1 0.657456 0.591711 0.575869 11.00000 0.04663 0.03861 = 0.06205 0.00925 -0.00305 -0.00286 AFIX 43 H5 2 0.631204 0.540920 0.581550 11.00000 -1.20000 AFIX 0 C6 1 0.827673 0.620913 0.636130 11.00000 0.04198 0.05370 = 0.06131 0.01136 -0.00446 0.00071 AFIX 43 H6 2 0.916930 0.590867 0.687195 11.00000 -1.20000 AFIX 0 C7 1 0.874939 0.695353 0.624397 11.00000 0.03662 0.05099 = 0.04866 -0.00024 0.00200 -0.00448 C8 1 1.057544 0.724163 0.683651 11.00000 0.04634 0.06774 = 0.05936 0.00301 -0.00364 -0.00948 AFIX 43 H8 2 1.146842 0.693508 0.733673 11.00000 -1.20000 AFIX 0 C9 1 1.107808 0.794992 0.670376 11.00000 0.05511 0.07342 = 0.07270 -0.00181 -0.00364 -0.02304 AFIX 43 H9 2 1.231105 0.813773 0.710556 11.00000 -1.20000 AFIX 0 C10 1 0.975893 0.839594 0.597016 11.00000 0.06837 0.06346 = 0.07318 0.00061 0.00040 -0.02777 AFIX 43 H10 2 1.012377 0.888683 0.586249 11.00000 -1.20000 AFIX 0 C11 1 0.794385 0.814611 0.539738 11.00000 0.05646 0.04621 = 0.05965 0.00285 0.00545 -0.00872 AFIX 43 H11 2 0.706231 0.846849 0.491926 11.00000 -1.20000 AFIX 0 C12 1 0.738166 0.741110 0.551629 11.00000 0.04081 0.04266 = 0.04207 -0.00038 0.00829 -0.00560 C13 1 0.549506 0.710917 0.495293 11.00000 0.03752 0.03998 = 0.03577 -0.00364 0.00423 0.00130 C14 1 0.064773 0.588380 0.305854 11.00000 0.03695 0.04726 = 0.05291 0.00295 0.00234 -0.00027 C15 1 0.019744 0.564132 0.199328 11.00000 0.04471 0.06009 = 0.05447 -0.00117 0.00960 -0.00263 AFIX 43 H15 2 0.101446 0.577554 0.153307 11.00000 -1.20000 AFIX 0 C16 1 -0.144401 0.520067 0.157954 11.00000 0.04721 0.06379 = 0.04643 -0.00470 0.00027 0.00161 AFIX 43 H16 2 -0.174482 0.503502 0.084224 11.00000 -1.20000 AFIX 0 C17 1 -0.261736 0.500902 0.224472 11.00000 0.03775 0.04928 = 0.05139 -0.00350 -0.00270 0.00051 C18 1 -0.218795 0.524036 0.331651 11.00000 0.05057 0.07508 = 0.04919 -0.00546 0.00825 -0.01386 AFIX 43 H18 2 -0.299918 0.509947 0.377662 11.00000 -1.20000 AFIX 0 C19 1 -0.055094 0.568330 0.371919 11.00000 0.05094 0.07537 = 0.04528 -0.00915 0.00125 -0.01402 AFIX 43 H19 2 -0.025515 0.584942 0.445616 11.00000 -1.20000 AFIX 0 HKLF 4 REM x1030b_a.res in P2(1)/n REM R1 = 0.0451 for 3493 Fo > 4sig(Fo) and 0.0863 for all 5656 data REM 199 parameters refined using 0 restraints END WGHT 0.0197 1.6677 REM Highest difference peak 0.724, deepest hole -0.813, 1-sigma level 0.075 Q1 1 0.9884 0.8033 0.6574 11.00000 0.05 0.72 Q2 1 0.4626 0.5628 0.4935 11.00000 0.05 0.58 Q3 1 -0.4762 0.4184 0.1085 11.00000 0.05 0.41 Q4 1 -0.4770 0.4340 0.2241 11.00000 0.05 0.38 Q5 1 1.0084 0.8631 0.6839 11.00000 0.05 0.31 ; _shelx_res_checksum 68643 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy I I1 -0.50948(3) 0.43392(2) 0.16336(2) 0.06235(10) Uani d 1 O O1 0.3551(3) 0.60041(12) 0.4492(2) 0.0521(6) Uani d 1 C C1 0.3838(5) 0.75621(18) 0.4302(3) 0.0500(8) Uani d 1 O O2 0.3855(4) 0.82269(13) 0.4246(3) 0.0732(8) Uani d 1 C C2 0.2006(5) 0.71359(18) 0.3764(3) 0.0579(9) Uani d 1 H H2A 0.111796 0.713332 0.425697 0.069 Uiso calc 1 H H2B 0.131632 0.738742 0.307874 0.069 Uiso calc 1 C C3 0.2426(4) 0.63579(18) 0.3505(3) 0.0482(8) Uani d 1 H H3 0.323461 0.636549 0.296041 0.058 Uiso calc 1 C C4 0.5196(4) 0.63685(16) 0.5048(3) 0.0418(7) Uani d 1 C C5 0.6575(5) 0.59171(18) 0.5759(3) 0.0522(8) Uani d 1 H H5 0.631204 0.540920 0.581550 0.063 Uiso calc 1 C C6 0.8277(5) 0.6209(2) 0.6361(3) 0.0556(9) Uani d 1 H H6 0.916930 0.590867 0.687195 0.067 Uiso calc 1 C C7 0.8749(4) 0.69535(18) 0.6244(3) 0.0471(7) Uani d 1 C C8 1.0575(5) 0.7242(2) 0.6837(3) 0.0610(10) Uani d 1 H H8 1.146842 0.693508 0.733673 0.073 Uiso calc 1 C C9 1.1078(6) 0.7950(2) 0.6704(4) 0.0708(11) Uani d 1 H H9 1.231105 0.813773 0.710556 0.085 Uiso calc 1 C C10 0.9759(6) 0.8396(2) 0.5970(4) 0.0716(12) Uani d 1 H H10 1.012377 0.888683 0.586249 0.086 Uiso calc 1 C C11 0.7944(5) 0.81461(19) 0.5397(3) 0.0559(9) Uani d 1 H H11 0.706231 0.846849 0.491926 0.067 Uiso calc 1 C C12 0.7382(4) 0.74111(17) 0.5516(3) 0.0423(7) Uani d 1 C C13 0.5495(4) 0.71092(16) 0.4953(2) 0.0387(6) Uani d 1 C C14 0.0648(4) 0.58838(18) 0.3059(3) 0.0474(7) Uani d 1 C C15 0.0197(5) 0.56413(19) 0.1993(3) 0.0537(8) Uani d 1 H H15 0.101446 0.577554 0.153307 0.064 Uiso calc 1 C C16 -0.1444(5) 0.5201(2) 0.1580(3) 0.0546(8) Uani d 1 H H16 -0.174482 0.503502 0.084224 0.066 Uiso calc 1 C C17 -0.2617(4) 0.50090(18) 0.2245(3) 0.0488(8) Uani d 1 C C18 -0.2188(5) 0.5240(2) 0.3317(3) 0.0591(9) Uani d 1 H H18 -0.299918 0.509947 0.377662 0.071 Uiso calc 1 C C19 -0.0551(5) 0.5683(2) 0.3719(3) 0.0592(9) Uani d 1 H H19 -0.025515 0.584942 0.445616 0.071 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 I1 0.04458(13) 0.06445(16) 0.06874(17) -0.00698(11) -0.00216(10) -0.01116(13) O1 0.0414(11) 0.0401(11) 0.0626(15) -0.0048(9) -0.0087(10) 0.0070(10) C1 0.0424(16) 0.0458(18) 0.056(2) 0.0027(14) 0.0030(14) 0.0040(15) O2 0.0588(15) 0.0414(13) 0.103(2) 0.0045(11) -0.0094(14) 0.0091(14) C2 0.0417(16) 0.0484(19) 0.072(2) 0.0019(14) -0.0065(16) 0.0077(17) C3 0.0384(15) 0.0525(19) 0.0481(19) -0.0004(14) 0.0010(13) 0.0027(14) C4 0.0364(14) 0.0397(15) 0.0469(17) -0.0030(12) 0.0065(12) 0.0027(13) C5 0.0466(17) 0.0386(16) 0.062(2) -0.0029(13) -0.0030(15) 0.0093(15) C6 0.0420(16) 0.054(2) 0.061(2) 0.0007(15) -0.0045(15) 0.0114(17) C7 0.0366(14) 0.0510(18) 0.0487(18) -0.0045(13) 0.0020(13) -0.0002(14) C8 0.0463(18) 0.068(2) 0.059(2) -0.0095(17) -0.0036(16) 0.0030(18) C9 0.055(2) 0.073(3) 0.073(3) -0.023(2) -0.0036(19) -0.002(2) C10 0.068(2) 0.063(2) 0.073(3) -0.028(2) 0.000(2) 0.001(2) C11 0.0565(19) 0.0462(18) 0.060(2) -0.0087(15) 0.0055(16) 0.0028(16) C12 0.0408(15) 0.0427(16) 0.0421(16) -0.0056(13) 0.0083(12) -0.0004(13) C13 0.0375(14) 0.0400(15) 0.0358(15) 0.0013(12) 0.0042(11) -0.0036(12) C14 0.0369(15) 0.0473(17) 0.0529(19) -0.0003(13) 0.0023(13) 0.0029(14) C15 0.0447(17) 0.060(2) 0.054(2) -0.0026(16) 0.0096(14) -0.0012(17) C16 0.0472(17) 0.064(2) 0.0464(19) 0.0016(16) 0.0003(14) -0.0047(16) C17 0.0377(15) 0.0493(18) 0.0514(19) 0.0005(13) -0.0027(13) -0.0035(15) C18 0.0506(19) 0.075(2) 0.049(2) -0.0139(18) 0.0083(15) -0.0055(18) C19 0.0509(19) 0.075(2) 0.0453(19) -0.0140(18) 0.0012(15) -0.0091(18) 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' I I -0.4742 1.8119 '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 C4 O1 C3 115.6(2) O2 C1 C2 120.5(3) O2 C1 C13 124.5(3) C13 C1 C2 114.9(3) C1 C2 H2A 109.0 C1 C2 H2B 109.0 H2A C2 H2B 107.8 C3 C2 C1 112.9(3) C3 C2 H2A 109.0 C3 C2 H2B 109.0 O1 C3 C2 109.1(3) O1 C3 H3 108.5 O1 C3 C14 106.6(3) C2 C3 H3 108.5 C2 C3 C14 115.5(3) C14 C3 H3 108.5 O1 C4 C5 113.6(3) O1 C4 C13 124.2(3) C13 C4 C5 122.2(3) C4 C5 H5 120.1 C6 C5 C4 119.7(3) C6 C5 H5 120.1 C5 C6 H6 119.4 C5 C6 C7 121.1(3) C7 C6 H6 119.4 C6 C7 C12 119.5(3) C8 C7 C6 120.5(3) C8 C7 C12 119.9(3) C7 C8 H8 119.4 C9 C8 C7 121.2(3) C9 C8 H8 119.4 C8 C9 H9 120.5 C8 C9 C10 119.0(3) C10 C9 H9 120.5 C9 C10 H10 119.1 C11 C10 C9 121.9(4) C11 C10 H10 119.1 C10 C11 H11 119.8 C10 C11 C12 120.3(3) C12 C11 H11 119.8 C7 C12 C13 118.7(3) C11 C12 C7 117.6(3) C11 C12 C13 123.7(3) C4 C13 C1 118.4(3) C4 C13 C12 118.2(3) C12 C13 C1 123.4(3) C15 C14 C3 120.7(3) C15 C14 C19 119.0(3) C19 C14 C3 120.3(3) C14 C15 H15 119.6 C14 C15 C16 120.8(3) C16 C15 H15 119.6 C15 C16 H16 120.3 C17 C16 C15 119.4(3) C17 C16 H16 120.3 C16 C17 I1 119.9(2) C16 C17 C18 120.8(3) C18 C17 I1 119.3(3) C17 C18 H18 120.4 C17 C18 C19 119.2(3) C19 C18 H18 120.4 C14 C19 C18 120.7(3) C14 C19 H19 119.6 C18 C19 H19 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C17 2.107(3) O1 C3 1.446(4) O1 C4 1.364(3) C1 O2 1.213(4) C1 C2 1.510(4) C1 C13 1.492(4) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.502(5) C3 H3 1.0000 C3 C14 1.507(4) C4 C5 1.406(4) C4 C13 1.376(4) C5 H5 0.9500 C5 C6 1.353(4) C6 H6 0.9500 C6 C7 1.413(5) C7 C8 1.413(4) C7 C12 1.419(4) C8 H8 0.9500 C8 C9 1.360(5) C9 H9 0.9500 C9 C10 1.393(6) C10 H10 0.9500 C10 C11 1.375(5) C11 H11 0.9500 C11 C12 1.415(4) C12 C13 1.445(4) C14 C15 1.374(5) C14 C19 1.381(5) C15 H15 0.9500 C15 C16 1.394(5) C16 H16 0.9500 C16 C17 1.368(5) C17 C18 1.376(5) C18 H18 0.9500 C18 C19 1.392(5) C19 H19 0.9500 _cod_database_fobs_code 1557210