############################################################################## # # # This CIF contains the data for a data article accepted for # # publication in IUCrData. It conforms to the requirements of # # Notes for Authors for IUCrData, and has been # # peer reviewed under the auspices of IUCrData. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the data # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _journal_date_recd_electronic 2024-04-24 _journal_date_accepted 2024-04-30 _journal_name_full 'IUCrData' _journal_year 2024 _journal_volume 9 _journal_issue 5 _journal_page_first 0 _journal_page_last 0 _journal_paper_category HO _journal_paper_doi 10.1107/S2414314624003948 _journal_coeditor_code HB4468 _publ_contact_author_name 'Jason B Benedict' _publ_contact_author_address ; 771 Natural Sciences Complex Buffalo, NY 14260 ; _publ_contact_author_email jbb6@buffalo.edu _publ_contact_author_fax ? _publ_contact_author_phone '1-716-645-4276' _publ_section_title ; Methyl 2-hydroxy-4-iodobenzoate ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Kimble, Marten J' ; Both authors contributed equally to this work. ; ; 730 Natural Sciences Complex Buffalo, NY 14260-3000 USA ; 'Myers, Shea D' ; Both authors contributed equally to this work. ; ; 730 Natural Sciences Complex Buffalo, NY 14260-3000 USA ; 'Benedict, Jason B' . ; 771 Natural Sciences Complex Buffalo, NY 14260 USA ; _publ_section_synopsis ; The title compound forms a sheet structure of dimers exhibiting intra- and intermolecular hydrogen bonds. ; _chemical_name_systematic ; Methyl 2-hydroxy-4-iodobenzoate ; _chemical_name_common ? _chemical_formula_moiety 'C8 H7 I O3' _chemical_formula_sum 'C8 H7 I O3' _chemical_formula_iupac 'C8 H7 I O3' _chemical_formula_weight 278.04 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.3286(8) _cell_length_b 21.334(4) _cell_length_c 9.2941(16) _cell_angle_alpha 90 _cell_angle_beta 93.744(4) _cell_angle_gamma 90 _cell_volume 856.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6811 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 34.14 _cell_measurement_temperature 90.00 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_absorpt_correction_T_min 0.5639 _exptl_absorpt_correction_T_max 0.7469 _diffrn_ambient_temperature 90.00 _diffrn_source ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23320 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_theta_min 2.395 _diffrn_reflns_theta_max 35.100 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _refine_special_details ; The O-bound H atom was located in a difference map and its position was freely refined. The C-bound H atoms were geometrically placed (C---H = 0.95--0.98 \%A) and refined as riding atoms. ; _reflns_number_total 3651 _reflns_number_gt 3315 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0574 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_number_reflns 3651 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+1.6600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.269 _refine_diff_density_min -1.916 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' _computing_data_collection ; APEX2 (Bruker, 2016) ; _computing_cell_refinement ; SAINT V8.40B (Bruker, 2016) ; _computing_data_reduction ; SAINT V8.40B (Bruker, 2016) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; 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 I I1 0.05964(3) 0.25795(2) 0.54095(2) 0.01430(4) Uani d 1 . . O O3 0.7859(4) 0.39459(9) 0.91310(18) 0.0170(3) Uani d 1 . . O O1 0.4603(4) 0.56516(8) 0.72915(18) 0.0180(3) Uani d 1 . . O O2 0.7790(4) 0.51960(9) 0.89865(19) 0.0212(4) Uani d 1 . . C C6 0.2313(5) 0.34266(10) 0.6295(2) 0.0127(4) Uani d 1 . . C C7 0.4516(5) 0.34172(10) 0.7453(2) 0.0128(4) Uani d 1 . . H H7 0.522507 0.302965 0.785568 0.015 Uiso calc 1 . . C C8 0.5675(5) 0.39821(10) 0.8018(2) 0.0121(3) Uani d 1 . . C C1 0.5827(6) 0.62513(11) 0.7783(3) 0.0203(5) Uani d 1 . . H H1A 0.499780 0.658300 0.713823 0.030 Uiso calc 1 . . H H1B 0.809060 0.624553 0.777897 0.030 Uiso calc 1 . . H H1C 0.522278 0.633151 0.876394 0.030 Uiso calc 1 . . C C5 0.1189(5) 0.39860(11) 0.5688(2) 0.0161(4) Uani d 1 . . H H5 -0.033554 0.398522 0.490504 0.019 Uiso calc 1 . . C C3 0.4577(5) 0.45534(10) 0.7425(2) 0.0123(4) Uani d 1 . . C C2 0.5823(5) 0.51534(11) 0.7990(2) 0.0144(4) Uani d 1 . . C C4 0.2359(5) 0.45406(10) 0.6259(2) 0.0156(4) Uani d 1 . . H H4 0.163744 0.492573 0.584857 0.019 Uiso calc 1 . . H H3 0.836(8) 0.4252(17) 0.929(4) 0.025(9) Uiso d 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 0.01408(6) 0.01099(7) 0.01764(7) -0.00031(5) -0.00056(4) -0.00134(5) O3 0.0173(8) 0.0173(8) 0.0153(7) 0.0008(6) -0.0061(6) -0.0004(6) O1 0.0241(8) 0.0104(7) 0.0188(8) -0.0031(6) -0.0048(6) 0.0007(6) O2 0.0210(8) 0.0204(9) 0.0211(8) -0.0015(6) -0.0083(6) -0.0031(6) C6 0.0114(8) 0.0128(9) 0.0138(9) -0.0012(7) 0.0009(7) -0.0017(7) C7 0.0128(9) 0.0120(9) 0.0136(9) 0.0008(7) 0.0011(7) 0.0006(7) C8 0.0103(8) 0.0155(9) 0.0105(8) 0.0020(7) 0.0003(6) 0.0010(7) C1 0.0282(12) 0.0114(10) 0.0211(11) -0.0062(8) 0.0005(9) -0.0021(8) C5 0.0178(10) 0.0137(10) 0.0158(9) -0.0004(7) -0.0061(7) 0.0005(7) C3 0.0132(9) 0.0108(9) 0.0128(9) 0.0003(7) -0.0010(7) 0.0004(7) C2 0.0140(9) 0.0152(10) 0.0138(9) -0.0006(7) 0.0007(7) -0.0011(7) C4 0.0179(10) 0.0104(9) 0.0177(10) 0.0002(7) -0.0053(8) 0.0012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 I1 C6 . 2.101(2) ? O3 C8 . 1.357(3) ? O3 H3 . 0.70(4) ? O1 C1 . 1.447(3) ? O1 C2 . 1.336(3) ? O2 C2 . 1.220(3) ? C6 C7 . 1.391(3) ? C6 C5 . 1.394(3) ? C7 H7 . 0.9500 ? C7 C8 . 1.395(3) ? C8 C3 . 1.407(3) ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? C1 H1C . 0.9800 ? C5 H5 . 0.9500 ? C5 C4 . 1.379(3) ? C3 C2 . 1.472(3) ? C3 C4 . 1.400(3) ? C4 H4 . 0.9500 ? 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 C8 O3 H3 . . 107(3) ? C2 O1 C1 . . 115.15(18) ? C7 C6 I1 . . 119.85(16) ? C7 C6 C5 . . 121.9(2) ? C5 C6 I1 . . 118.20(15) ? C6 C7 H7 . . 120.3 ? C6 C7 C8 . . 119.4(2) ? C8 C7 H7 . . 120.3 ? O3 C8 C7 . . 116.94(19) ? O3 C8 C3 . . 123.3(2) ? C7 C8 C3 . . 119.80(19) ? O1 C1 H1A . . 109.5 ? O1 C1 H1B . . 109.5 ? O1 C1 H1C . . 109.5 ? H1A C1 H1B . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? C6 C5 H5 . . 121.0 ? C4 C5 C6 . . 118.0(2) ? C4 C5 H5 . . 121.0 ? C8 C3 C2 . . 120.44(19) ? C4 C3 C8 . . 118.89(19) ? C4 C3 C2 . . 120.63(19) ? O1 C2 C3 . . 113.23(18) ? O2 C2 O1 . . 122.9(2) ? O2 C2 C3 . . 123.8(2) ? C5 C4 C3 . . 122.0(2) ? C5 C4 H4 . . 119.0 ? C3 C4 H4 . . 119.0 ? 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 I1 C6 C7 C8 . . . . 178.99(15) ? I1 C6 C5 C4 . . . . -179.01(17) ? O3 C8 C3 C2 . . . . 1.0(3) ? O3 C8 C3 C4 . . . . 178.8(2) ? C6 C7 C8 O3 . . . . -178.90(19) ? C6 C7 C8 C3 . . . . 0.9(3) ? C6 C5 C4 C3 . . . . -0.9(4) ? C7 C6 C5 C4 . . . . 0.8(3) ? C7 C8 C3 C2 . . . . -178.8(2) ? C7 C8 C3 C4 . . . . -0.9(3) ? C8 C3 C2 O1 . . . . 178.4(2) ? C8 C3 C2 O2 . . . . -1.0(3) ? C8 C3 C4 C5 . . . . 0.9(3) ? C1 O1 C2 O2 . . . . 1.2(3) ? C1 O1 C2 C3 . . . . -178.26(19) ? C5 C6 C7 C8 . . . . -0.8(3) ? C2 C3 C4 C5 . . . . 178.8(2) ? C4 C3 C2 O1 . . . . 0.6(3) ? C4 C3 C2 O2 . . . . -178.8(2) ? 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 O3 H3 O2 . 0.70(4) 2.05(4) 2.670(3) 149(4) yes O3 H3 O2 3_767 0.70(4) 2.53(4) 3.087(2) 139(4) yes _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 0.156 _shelx_estimated_absorpt_T_max 0.930 _shelx_hkl_file ; -1 0 0 555.84 26.00 1 0 0 545.25 25.90 1 0 0 559.74 25.80 1 0 0 545.75 26.40 -1 0 0 537.15 26.00 -1 0 0 531.15 25.80 2 0 0 889.61 42.80 -2 0 0 849.22 42.10 -2 0 0 891.81 42.00 2 0 0 877.91 41.60 -2 0 0 863.01 41.50 3 0 0 1.90 0.80 -3 0 0 2.30 1.10 -3 0 0 1.30 0.70 3 0 0 4.90 1.70 -3 0 0 1.00 0.80 -4 0 0 44.80 5.30 4 0 0 46.10 6.50 -4 0 0 49.30 5.80 4 0 0 47.80 3.90 -5 0 0 2.40 1.80 5 0 0 7.70 3.00 5 0 0 6.90 1.80 -5 0 0 3.80 1.70 -6 0 0 164.28 12.80 6 0 0 171.88 11.00 6 0 0 171.98 13.80 -1 -1 0 573.74 28.10 1 -1 0 590.14 27.90 -1 -1 0 601.54 28.00 1 -1 0 560.44 27.80 1 -1 0 597.54 28.40 1 1 0 587.34 27.90 -1 1 0 589.84 27.80 -1 1 0 594.44 28.10 1 1 0 595.14 28.50 1 1 0 594.84 28.00 -1 1 0 568.24 28.10 1 1 0 622.84 28.20 2 -1 0 745.53 34.60 2 -1 0 735.43 35.60 -2 -1 0 723.83 34.60 -2 -1 0 744.83 34.90 -2 -1 0 711.13 35.00 -2 1 0 687.73 35.00 -2 1 0 705.43 34.40 2 1 0 703.33 35.70 2 1 0 725.63 34.50 -2 1 0 731.73 34.90 -3 -1 0 822.02 40.10 3 -1 0 844.92 41.90 -3 -1 0 784.62 40.90 -3 -1 0 851.01 40.70 3 -1 0 841.72 40.20 -3 1 0 839.02 40.80 3 1 0 843.52 42.00 -3 1 0 786.12 40.90 -3 1 0 851.11 39.90 3 1 0 843.82 40.20 4 -1 0 544.95 26.90 -4 -1 0 511.95 28.10 4 -1 0 547.85 29.30 -4 -1 0 505.55 27.40 -4 1 0 509.45 28.00 -4 1 0 525.25 27.70 4 1 0 549.45 26.90 4 1 0 567.14 29.60 -5 -1 0 315.87 19.50 5 -1 0 318.97 20.50 -5 -1 0 307.67 18.60 5 -1 0 345.57 18.00 -5 1 0 325.97 19.00 5 1 0 320.87 20.70 -5 1 0 348.27 19.80 5 1 0 325.37 17.80 6 -1 0 99.19 7.40 -6 -1 0 99.59 10.80 6 -1 0 113.59 12.40 6 1 0 93.29 11.90 6 1 0 97.79 7.40 -6 1 0 92.29 10.50 -1 -2 0 2647.34 128.79 1 -2 0 2793.82 127.79 1 -2 0 2854.61 128.29 1 -2 0 2694.53 128.49 1 -2 0 2714.13 129.09 -1 -2 0 2877.01 127.99 -1 -2 0 2779.92 128.09 -1 2 0 2620.74 127.99 1 2 0 2693.63 128.09 1 2 0 2591.84 128.19 -1 2 0 2767.02 128.19 1 2 0 2836.12 128.59 1 2 0 2817.72 128.09 -2 -2 0 882.91 42.20 2 -2 0 888.61 42.90 -2 -2 0 883.21 42.50 2 -2 0 883.91 42.00 -2 2 0 842.32 42.30 2 2 0 866.51 41.90 -2 2 0 912.71 41.70 -2 2 0 876.11 42.40 2 2 0 884.71 43.20 3 -2 0 334.37 18.70 3 -2 0 340.27 17.20 -3 -2 0 338.47 17.30 -3 -2 0 333.87 17.60 -3 -2 0 323.87 18.00 -3 2 0 323.27 17.80 3 2 0 332.17 18.90 3 2 0 340.27 17.10 -3 2 0 348.97 18.10 4 -2 0 2.70 1.90 -4 -2 0 1.80 1.20 -4 -2 0 1.60 0.90 4 -2 0 1.80 0.90 -4 -2 0 0.40 0.90 4 2 0 3.30 1.80 -4 2 0 1.50 1.00 -4 2 0 1.20 1.10 4 2 0 3.20 1.20 -5 -2 0 40.00 5.50 -5 -2 0 52.19 7.00 5 -2 0 63.69 5.00 5 -2 0 60.19 7.80 5 2 0 54.69 4.60 -5 2 0 55.69 7.20 -5 2 0 50.29 6.40 5 2 0 57.59 8.40 -6 -2 0 46.70 7.40 6 -2 0 38.10 5.00 6 -2 0 60.99 8.90 -6 2 0 49.30 7.20 6 2 0 32.70 6.90 6 2 0 48.80 5.50 0 -3 0 0.10 0.30 0 -3 0 0.20 0.40 0 -3 0 -0.10 0.10 0 -3 0 1.40 0.60 0 -3 0 0.30 0.10 0 3 0 0.10 0.10 0 3 0 0.30 0.30 0 3 0 0.80 0.60 0 3 0 0.10 0.30 -1 -3 0 179.58 9.10 1 -3 0 179.98 8.80 -1 -3 0 179.18 9.30 -1 -3 0 178.98 8.80 1 -3 0 186.58 9.00 1 -3 0 186.18 9.20 -1 3 0 174.88 9.30 1 3 0 179.98 9.20 1 3 0 178.78 9.60 1 3 0 170.08 8.80 -1 3 0 178.18 9.10 -2 -3 0 567.84 28.30 2 -3 0 559.34 28.60 2 -3 0 600.84 27.90 -2 -3 0 575.54 28.10 2 -3 0 575.14 27.40 2 3 0 586.84 28.30 2 3 0 579.64 27.70 -2 3 0 584.54 28.40 -2 3 0 555.14 28.20 2 3 0 559.04 29.00 3 -3 0 718.53 36.80 3 -3 0 742.53 35.50 -3 -3 0 729.83 35.80 -3 -3 0 722.83 35.80 -3 -3 0 753.12 36.50 3 3 0 701.73 37.30 3 3 0 761.72 35.40 -3 3 0 708.83 36.20 -3 3 0 706.33 36.20 4 -3 0 488.35 24.80 -4 -3 0 486.95 24.80 4 -3 0 494.35 26.80 -4 -3 0 477.05 25.30 -4 -3 0 488.35 26.20 4 3 0 480.95 27.30 4 3 0 489.25 24.70 -4 3 0 479.55 26.00 -4 3 0 498.05 26.00 5 -3 0 313.87 16.50 -5 -3 0 280.97 18.00 -5 -3 0 277.07 16.80 5 -3 0 296.27 18.60 -5 3 0 278.97 17.40 5 3 0 284.87 19.30 -5 3 0 297.67 17.90 5 3 0 296.87 16.20 6 -3 0 129.29 8.70 -6 -3 0 107.99 11.80 6 -3 0 110.79 12.30 6 3 0 125.49 14.20 -6 3 0 111.79 11.80 0 -4 0 1174.68 54.09 0 -4 0 1119.19 54.99 0 -4 0 1114.19 54.19 0 -4 0 1196.68 54.59 0 4 0 1253.47 54.39 0 4 0 1102.89 54.09 0 4 0 1160.08 55.19 0 4 0 1166.58 54.59 1 -4 0 2071.49 94.59 -1 -4 0 1998.80 94.49 -1 -4 0 2131.79 95.09 1 -4 0 2067.99 94.39 1 -4 0 2022.50 94.29 1 4 0 1938.71 94.19 1 4 0 1985.50 95.09 -1 4 0 1988.90 94.49 -1 4 0 1969.90 94.89 1 4 0 2035.90 94.69 -2 -4 0 617.94 30.40 2 -4 0 624.74 30.00 2 -4 0 633.44 30.60 2 -4 0 616.44 29.50 -2 -4 0 616.64 30.30 -2 4 0 585.44 30.30 2 4 0 643.34 30.40 -2 4 0 639.74 30.70 2 4 0 618.44 29.80 2 4 0 610.34 31.30 3 -4 0 232.18 12.50 3 -4 0 232.28 13.60 -3 -4 0 224.78 13.30 -3 -4 0 234.28 12.90 3 4 0 230.18 14.30 -3 4 0 238.98 13.40 -3 4 0 236.98 13.30 3 4 0 244.68 12.50 4 -4 0 6.30 1.60 -4 -4 0 8.50 2.20 -4 -4 0 8.20 2.30 -4 -4 0 7.30 1.80 4 -4 0 8.40 2.60 -4 4 0 10.90 2.60 4 4 0 9.70 2.00 4 4 0 5.80 2.60 -4 4 0 6.00 2.00 -5 -4 0 46.90 6.60 -5 -4 0 27.70 4.40 5 -4 0 35.30 6.00 5 -4 0 37.00 4.40 5 4 0 31.80 4.00 -5 4 0 30.30 5.20 5 4 0 36.40 6.50 -5 4 0 28.20 4.90 -6 -4 0 54.09 8.00 6 -4 0 61.09 6.60 6 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15.00 4.60 0 -11 -13 49.60 8.80 0 -11 13 36.80 6.40 0 11 -13 37.80 5.50 0 11 13 37.20 7.00 0 11 13 48.60 7.50 -1 -11 -13 30.40 7.20 1 -11 13 15.20 4.20 1 11 13 16.20 4.10 -1 11 -13 14.00 3.60 2 -12 -13 29.30 5.80 -2 -12 13 23.40 4.00 -2 12 13 24.00 5.70 2 12 -13 17.30 5.10 -1 -12 13 4.80 2.60 -1 12 13 3.70 3.10 1 12 -13 2.50 2.60 0 -12 13 1.20 1.90 0 -12 -13 1.60 2.40 0 12 13 3.30 2.20 0 12 -13 3.30 1.90 0 12 13 -0.80 2.30 -1 -12 -13 39.80 8.30 1 -12 13 22.70 5.30 1 12 13 22.90 5.40 -1 12 -13 12.20 3.50 2 -13 -13 28.00 5.80 2 13 -13 12.60 4.60 -2 13 13 15.70 5.40 1 -13 -13 46.40 7.50 -1 -13 13 37.70 6.50 -1 13 13 25.50 6.40 1 13 -13 43.20 7.40 0 -13 -13 25.00 6.10 0 -13 13 28.90 5.90 0 13 13 16.50 4.70 0 13 13 35.20 6.80 0 13 -13 21.00 3.80 1 -13 13 48.20 11.50 -1 -13 -13 43.30 8.90 1 13 13 20.00 5.30 2 14 -13 18.90 7.40 1 -14 -13 1.80 2.50 -1 -14 13 2.40 2.40 1 14 -13 -0.40 2.20 -1 14 13 -0.10 3.10 0 -14 -13 -1.70 2.50 0 -14 13 3.70 2.90 0 14 13 3.30 2.70 0 14 13 1.80 3.00 0 14 -13 0.70 1.80 1 14 13 3.80 2.80 -1 -15 13 75.89 9.80 -1 15 13 46.70 8.70 1 15 -13 62.69 9.60 0 -15 -13 41.00 8.60 0 -15 13 30.60 9.20 0 15 13 35.40 7.30 1 15 13 13.90 4.70 1 16 -13 2.20 2.90 0 -16 -13 2.20 2.90 -1 0 14 91.89 10.50 0 0 -14 63.69 9.30 0 0 14 73.79 10.00 0 0 14 70.99 8.50 -1 0 -14 22.80 4.40 1 0 14 30.30 5.70 -2 0 -14 12.30 3.50 -1 -1 14 9.70 3.10 -1 1 14 6.50 2.60 0 -1 14 38.50 6.20 0 -1 14 30.60 6.50 0 1 14 24.60 5.10 1 -1 14 71.09 10.30 1 -1 14 59.79 8.00 1 1 14 63.89 8.60 -1 1 -14 38.10 5.90 -2 -1 -14 31.90 5.30 -1 -2 14 94.19 10.40 -1 2 14 79.79 9.10 -1 2 14 85.59 9.90 0 -2 14 80.79 9.30 0 -2 14 87.79 10.60 0 2 -14 60.09 7.40 0 2 14 82.39 9.30 1 -2 14 63.19 9.30 1 -2 14 42.00 6.60 -1 -2 -14 52.79 9.40 1 2 14 47.60 7.20 -1 2 -14 35.10 5.50 -2 -3 14 3.80 1.90 -1 -3 14 3.40 2.20 -1 3 14 0.50 1.30 0 -3 -14 11.30 3.90 0 -3 14 16.50 4.60 0 3 14 12.80 3.70 1 -3 14 29.70 6.70 1 -3 14 28.80 5.40 -1 -3 -14 40.90 8.20 1 3 14 34.10 6.10 -1 3 -14 27.60 4.90 -2 -4 14 58.19 6.20 -1 -4 14 96.29 9.20 -1 4 14 104.39 8.90 0 -4 14 112.89 12.30 0 -4 -14 102.89 13.00 0 4 -14 88.29 8.00 0 4 14 102.99 10.90 1 -4 14 46.60 7.00 1 -4 14 50.29 8.60 -1 -4 -14 44.50 8.60 -1 4 -14 28.20 4.90 1 4 14 34.20 6.10 -2 -5 14 7.60 2.20 -2 5 14 7.70 5.10 -1 -5 14 0.60 1.80 -1 5 14 1.30 2.00 0 -5 -14 17.90 5.10 0 -5 14 24.30 5.60 0 5 -14 25.70 4.30 0 5 14 22.30 4.90 1 -5 14 50.89 7.20 -1 -5 -14 35.80 8.10 1 -5 14 44.90 11.80 1 5 14 49.10 7.60 -1 5 -14 32.40 5.60 -2 -6 14 52.69 5.90 -2 6 14 59.99 8.60 -2 6 14 55.09 8.40 -1 -6 14 76.59 9.30 -1 6 14 61.09 8.00 0 -6 -14 49.10 8.80 0 -6 14 52.89 8.10 0 6 -14 38.60 5.70 0 6 14 49.60 7.40 -1 -6 -14 42.70 11.60 -1 6 -14 30.10 5.30 1 6 14 44.70 8.40 -2 -7 14 6.30 2.30 -2 7 14 9.90 4.00 2 7 -14 6.90 4.30 -1 -7 14 7.90 3.20 -1 7 14 5.30 2.40 0 -7 -14 23.40 5.90 0 -7 14 13.10 4.20 0 7 -14 11.40 2.90 0 7 14 12.80 3.70 -1 7 -14 31.50 6.80 -2 8 14 33.30 6.60 2 8 -14 37.60 7.20 -1 -8 14 69.89 8.80 -1 8 14 58.59 7.90 0 -8 14 48.90 8.10 0 -8 -14 54.79 9.40 0 8 14 40.00 6.70 0 8 -14 46.50 6.20 2 9 -14 13.20 3.80 -1 -9 14 1.70 2.20 -1 9 14 5.70 3.60 -1 9 14 1.60 1.90 0 -9 -14 13.50 4.80 0 -9 14 16.30 4.70 0 9 14 12.50 4.70 0 9 -14 21.80 4.30 -1 -10 14 59.99 8.60 -1 10 14 55.39 11.50 -1 10 14 59.19 9.40 0 -10 -14 72.99 11.00 -1 -11 14 4.70 3.30 -1 11 14 -2.30 2.80 0 -11 -14 13.70 5.30 0 1 15 2.40 4.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 23569 _shelx_res_file ; TITL mjk_012401_0m_a.res in P2(1)/c mjk_012401_0m.res created by SHELXL-2018/3 at 12:54:59 on 23-Apr-2024 REM Old TITL MJK_012401_0m in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.049, Rweak 0.004, Alpha 0.029 REM 1.174 for 64 systematic absences, Orientation as input REM Formula found by SHELXT: C8 O3 I CELL 0.71073 4.3286 21.3336 9.2941 90 93.744 90 ZERR 4 0.0008 0.0036 0.0016 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I O UNIT 32 28 4 12 EQIV $1 2-X,1-Y,2-Z L.S. 50 PLAN 1 SIZE 0.2 0.02 0.8 TEMP -183.15 CONF HTAB O3 O2 HTAB O3 O2_$1 list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.000000 1.660000 FVAR 0.26023 I1 3 0.059644 0.257952 0.540949 11.00000 0.01408 0.01099 = 0.01764 -0.00134 -0.00056 -0.00031 O3 4 0.785856 0.394585 0.913096 11.00000 0.01730 0.01728 = 0.01535 -0.00036 -0.00615 0.00082 O1 4 0.460274 0.565163 0.729149 11.00000 0.02406 0.01036 = 0.01880 0.00072 -0.00478 -0.00314 O2 4 0.778976 0.519599 0.898646 11.00000 0.02098 0.02035 = 0.02115 -0.00310 -0.00828 -0.00147 C6 1 0.231263 0.342659 0.629514 11.00000 0.01145 0.01278 = 0.01375 -0.00174 0.00085 -0.00123 C7 1 0.451623 0.341715 0.745319 11.00000 0.01281 0.01201 = 0.01362 0.00055 0.00114 0.00078 AFIX 43 H7 2 0.522507 0.302965 0.785568 11.00000 -1.20000 AFIX 0 C8 1 0.567517 0.398212 0.801782 11.00000 0.01031 0.01547 = 0.01050 0.00104 0.00028 0.00199 C1 1 0.582733 0.625132 0.778282 11.00000 0.02816 0.01143 = 0.02114 -0.00206 0.00053 -0.00616 AFIX 137 H1A 2 0.499780 0.658300 0.713823 11.00000 -1.50000 H1B 2 0.809060 0.624553 0.777897 11.00000 -1.50000 H1C 2 0.522278 0.633151 0.876394 11.00000 -1.50000 AFIX 0 C5 1 0.118915 0.398595 0.568809 11.00000 0.01777 0.01372 = 0.01578 0.00049 -0.00611 -0.00043 AFIX 43 H5 2 -0.033554 0.398522 0.490504 11.00000 -1.20000 AFIX 0 C3 1 0.457661 0.455335 0.742504 11.00000 0.01319 0.01077 = 0.01281 0.00038 -0.00097 0.00028 C2 1 0.582309 0.515337 0.798979 11.00000 0.01402 0.01517 = 0.01384 -0.00111 0.00065 -0.00063 C4 1 0.235872 0.454060 0.625901 11.00000 0.01790 0.01041 = 0.01767 0.00118 -0.00530 0.00021 AFIX 43 H4 2 0.163744 0.492573 0.584857 11.00000 -1.20000 AFIX 0 H3 2 0.836119 0.425250 0.928983 11.00000 0.02548 HKLF 4 REM mjk_012401_0m_a.res in P2(1)/c REM wR2 = 0.0574, GooF = S = 1.111, Restrained GooF = 1.111 for all data REM R1 = 0.0299 for 3315 Fo > 4sig(Fo) and 0.0349 for all 3651 data REM 114 parameters refined using 0 restraints END WGHT 0.0000 1.6600 REM Highest difference peak 1.269, deepest hole -1.916, 1-sigma level 0.143 Q1 1 0.0570 0.2892 0.5413 11.00000 0.05 1.27 ; _shelx_res_checksum 73258