#============================================================================== # 1. SUBMISSION DETAILS data_global _publ_contact_author ; Constantin G. Daniliuc Organisch-Chemisches Institut Westf\"alische Wilhelm-Universit\"at M\"unster 48149 M\"unster Germany ; _publ_contact_author_phone '049 251 83-36522' _publ_contact_author_fax '049 251 83-39772' _publ_contact_author_email 'constantin.daniliuc@uni-muenster.de' _publ_requested_journal '.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Deconstructing the Catalytic, Vicinal Difluorination of Alkenes: HF-Free Synthesis and Structural Study of p-TolIF2 ; loop_ _publ_author_name _publ_author_address 'Sarie, Jerome' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Thiehoff, Christian' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Mudd, Richard J.' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Daniliuc, Constantin G.' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Kehr, Gerald' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; 'Gilmour, Ryan' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 40 48149 M\"unster Germany ; #============================================================================= # cif data for "gil8757" (compound p-TolI(III)F2) #============================================================================= data_gil8757 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H7 F2 I' _chemical_formula_iupac ? _chemical_formula_weight 256.03 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.9542(8) _cell_length_b 11.5049(5) _cell_length_c 7.3428(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1516.74(11) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7847 _cell_measurement_theta_min 2.2687 _cell_measurement_theta_max 27.4822 _cell_measurement_temperature 100.(2) _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.249 _exptl_crystal_size_mid 0.073 _exptl_crystal_size_min 0.072 _exptl_crystal_density_diffrn 2.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 4.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin, USA. ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.75 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Mo ImS' _diffrn_source_type 'micro focus tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON 100 CMOS' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 12280 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _refine_special_details ; Refined as a 2-component inversion twin. ; _reflns_number_total 3384 _reflns_number_gt 3134 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0399 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_number_reflns 3384 _refine_ls_number_parameters 184 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.410 _refine_diff_density_min -0.551 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.30(3) 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' F F 0.0171 0.0103 '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' _computing_data_collection ; APEX2 v.2014.1-1 (Bruker AXS Inc., 2014) ; _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014 (Sheldrick, 2014)' 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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1A 0.31392(2) 0.52561(3) 0.70262(4) 0.01200(8) Uani d . . . 1 . . F F1A 0.30873(13) 0.4649(3) 0.9628(4) 0.0228(7) Uani d . . . 1 . . F F2A 0.33189(14) 0.5841(3) 0.4509(4) 0.0182(6) Uani d . . . 1 . . C C1A 0.4206(2) 0.5858(4) 0.7624(6) 0.0116(10) Uani d . . . 1 . . C C2A 0.4816(2) 0.5230(4) 0.7018(7) 0.0118(8) Uani d . . . 1 . . H H2A 0.4752 0.4504 0.6424 0.014 Uiso calc U . R 1 . . C C3A 0.5522(2) 0.5686(4) 0.7296(6) 0.0126(9) Uani d . . . 1 . . H H3A 0.5945 0.5259 0.6901 0.015 Uiso calc U . R 1 . . C C4A 0.5622(2) 0.6754(4) 0.8144(8) 0.0135(9) Uani d . . . 1 . . C C5A 0.4997(3) 0.7350(4) 0.8792(6) 0.0134(10) Uani d . . . 1 . . H H5A 0.5062 0.8063 0.9425 0.016 Uiso calc U . R 1 . . C C6A 0.4278(3) 0.6913(4) 0.8525(6) 0.0142(10) Uani d . . . 1 . . H H6A 0.3854 0.7326 0.8947 0.017 Uiso calc U . R 1 . . C C7A 0.6394(2) 0.7259(4) 0.8341(7) 0.0217(11) Uani d . . . 1 . . H H7A1 0.636 0.8042 0.886 0.033 Uiso calc U . R 1 . . H H7A2 0.6633 0.7299 0.7142 0.033 Uiso calc U . R 1 . . H H7A3 0.6691 0.6764 0.9149 0.033 Uiso calc U . R 1 . . I I1B 0.31704(2) 0.86527(3) 0.31236(3) 0.01011(7) Uani d . . . 1 . . F F1B 0.32703(14) 0.8447(3) 0.5821(4) 0.0193(7) Uani d . . . 1 . . F F2B 0.32499(15) 0.8889(3) 0.0404(4) 0.0179(7) Uani d . . . 1 . . C C1B 0.4336(2) 0.8652(4) 0.3080(8) 0.0100(8) Uani d . . . 1 . . C C2B 0.4715(2) 0.7669(4) 0.3672(6) 0.0124(10) Uani d . . . 1 . . H H2B 0.4452 0.7002 0.4083 0.015 Uiso calc U . R 1 . . C C3B 0.5486(2) 0.7687(4) 0.3647(6) 0.0117(10) Uani d . . . 1 . . H H3B 0.5753 0.7019 0.4037 0.014 Uiso calc U . R 1 . . C C4B 0.5880(2) 0.8662(4) 0.3063(8) 0.0144(8) Uani d . . . 1 . . C C5B 0.5480(2) 0.9639(4) 0.2461(6) 0.0140(11) Uani d . . . 1 . . H H5B 0.5742 1.0306 0.2048 0.017 Uiso calc U . R 1 . . C C6B 0.4713(2) 0.9641(4) 0.2461(6) 0.0121(10) Uani d . . . 1 . . H H6B 0.4445 1.0302 0.2048 0.014 Uiso calc U . R 1 . . C C7B 0.6729(2) 0.8666(4) 0.3076(10) 0.0198(10) Uani d . . . 1 . . H H7B1 0.6907 0.9039 0.4193 0.03 Uiso calc U . R 1 . . H H7B2 0.6913 0.9096 0.2016 0.03 Uiso calc U . R 1 . . H H7B3 0.6912 0.7864 0.3027 0.03 Uiso calc U . R 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 I1A 0.00768(14) 0.01779(15) 0.01054(14) 0.00005(11) -0.00047(17) 0.00320(13) F1A 0.0135(15) 0.042(2) 0.0131(16) 0.0016(14) 0.0011(11) 0.0099(15) F2A 0.0151(14) 0.0264(16) 0.0130(14) -0.0034(12) -0.0008(11) 0.0060(14) C1A 0.007(2) 0.016(2) 0.012(2) 0.0019(18) -0.0019(15) 0.0022(18) C2A 0.015(2) 0.012(2) 0.009(2) 0.0003(17) 0.001(2) 0.001(2) C3A 0.016(2) 0.012(2) 0.010(2) 0.0048(18) 0.0034(19) -0.001(2) C4A 0.014(2) 0.015(2) 0.011(2) -0.0044(17) -0.004(2) 0.006(2) C5A 0.020(2) 0.009(2) 0.012(2) 0.002(2) -0.0009(17) -0.0021(19) C6A 0.016(3) 0.017(2) 0.010(3) 0.0051(19) 0.0014(17) 0.0011(18) C7A 0.014(2) 0.029(3) 0.022(3) -0.009(2) -0.001(2) 0.001(2) I1B 0.00716(14) 0.01303(14) 0.01015(14) 0.00077(11) 0.00036(18) -0.00017(13) F1B 0.0129(16) 0.0358(18) 0.0092(16) -0.0019(12) -0.0006(11) -0.0014(13) F2B 0.0133(16) 0.0300(18) 0.0106(16) 0.0026(12) -0.0007(11) 0.0028(14) C1B 0.007(2) 0.0137(19) 0.0096(19) -0.0019(17) -0.003(3) -0.0022(19) C2B 0.013(2) 0.012(2) 0.012(2) -0.0022(19) 0.0055(17) 0.0002(17) C3B 0.008(2) 0.016(2) 0.010(2) 0.0053(19) -0.0013(17) 0.0010(17) C4B 0.013(2) 0.017(2) 0.013(2) -0.0008(18) -0.002(2) -0.005(2) C5B 0.015(3) 0.011(2) 0.016(3) -0.0064(19) 0.0017(18) 0.0014(18) C6B 0.013(2) 0.013(2) 0.009(2) 0.0029(19) 0.0022(16) 0.0001(17) C7B 0.009(2) 0.025(2) 0.026(2) -0.0010(19) -0.001(2) -0.008(3) _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 I1A F2A . 1.993(3) ? I1A F1A . 2.036(3) ? I1A C1A . 2.084(4) ? C1A C2A . 1.386(6) ? C1A C6A . 1.388(6) ? C2A C3A . 1.387(6) ? C2A H2A . 0.95 ? C3A C4A . 1.389(7) ? C3A H3A . 0.95 ? C4A C5A . 1.399(7) ? C4A C7A . 1.511(6) ? C5A C6A . 1.398(7) ? C5A H5A . 0.95 ? C6A H6A . 0.95 ? C7A H7A1 . 0.98 ? C7A H7A2 . 0.98 ? C7A H7A3 . 0.98 ? I1B F1B . 2.003(3) ? I1B F2B . 2.021(3) ? I1B C1B . 2.094(4) ? C1B C2B . 1.389(6) ? C1B C6B . 1.400(6) ? C2B C3B . 1.386(6) ? C2B H2B . 0.95 ? C3B C4B . 1.393(7) ? C3B H3B . 0.95 ? C4B C5B . 1.405(6) ? C4B C7B . 1.524(5) ? C5B C6B . 1.376(6) ? C5B H5B . 0.95 ? C6B H6B . 0.95 ? C7B H7B1 . 0.98 ? C7B H7B2 . 0.98 ? C7B H7B3 . 0.98 ? 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 F2A I1A F1A . . 173.30(10) ? F2A I1A C1A . . 86.23(14) ? F1A I1A C1A . . 87.61(14) ? C2A C1A C6A . . 122.3(4) ? C2A C1A I1A . . 119.0(3) ? C6A C1A I1A . . 118.5(4) ? C1A C2A C3A . . 118.6(4) ? C1A C2A H2A . . 120.7 ? C3A C2A H2A . . 120.7 ? C2A C3A C4A . . 121.2(4) ? C2A C3A H3A . . 119.4 ? C4A C3A H3A . . 119.4 ? C3A C4A C5A . . 118.9(4) ? C3A C4A C7A . . 120.1(4) ? C5A C4A C7A . . 121.0(4) ? C6A C5A C4A . . 121.1(4) ? C6A C5A H5A . . 119.5 ? C4A C5A H5A . . 119.5 ? C1A C6A C5A . . 117.9(4) ? C1A C6A H6A . . 121.1 ? C5A C6A H6A . . 121.1 ? C4A C7A H7A1 . . 109.5 ? C4A C7A H7A2 . . 109.5 ? H7A1 C7A H7A2 . . 109.5 ? C4A C7A H7A3 . . 109.5 ? H7A1 C7A H7A3 . . 109.5 ? H7A2 C7A H7A3 . . 109.5 ? F1B I1B F2B . . 170.76(9) ? F1B I1B C1B . . 85.73(17) ? F2B I1B C1B . . 85.08(17) ? C2B C1B C6B . . 121.8(4) ? C2B C1B I1B . . 119.0(3) ? C6B C1B I1B . . 119.2(3) ? C3B C2B C1B . . 118.2(4) ? C3B C2B H2B . . 120.9 ? C1B C2B H2B . . 120.9 ? C2B C3B C4B . . 121.6(4) ? C2B C3B H3B . . 119.2 ? C4B C3B H3B . . 119.2 ? C3B C4B C5B . . 118.7(4) ? C3B C4B C7B . . 120.5(4) ? C5B C4B C7B . . 120.8(4) ? C6B C5B C4B . . 120.9(4) ? C6B C5B H5B . . 119.6 ? C4B C5B H5B . . 119.6 ? C5B C6B C1B . . 118.8(4) ? C5B C6B H6B . . 120.6 ? C1B C6B H6B . . 120.6 ? C4B C7B H7B1 . . 109.5 ? C4B C7B H7B2 . . 109.5 ? H7B1 C7B H7B2 . . 109.5 ? C4B C7B H7B3 . . 109.5 ? H7B1 C7B H7B3 . . 109.5 ? H7B2 C7B H7B3 . . 109.5 ? 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 C6A C1A C2A C3A . . . . -1.1(7) ? I1A C1A C2A C3A . . . . 174.9(3) ? C1A C2A C3A C4A . . . . -0.8(7) ? C2A C3A C4A C5A . . . . 2.8(8) ? C2A C3A C4A C7A . . . . -176.8(5) ? C3A C4A C5A C6A . . . . -3.0(8) ? C7A C4A C5A C6A . . . . 176.6(4) ? C2A C1A C6A C5A . . . . 0.9(6) ? I1A C1A C6A C5A . . . . -175.2(3) ? C4A C5A C6A C1A . . . . 1.2(7) ? C6B C1B C2B C3B . . . . 0.3(7) ? I1B C1B C2B C3B . . . . -179.5(3) ? C1B C2B C3B C4B . . . . 0.6(7) ? C2B C3B C4B C5B . . . . -1.0(8) ? C2B C3B C4B C7B . . . . 179.1(5) ? C3B C4B C5B C6B . . . . 0.6(8) ? C7B C4B C5B C6B . . . . -179.5(5) ? C4B C5B C6B C1B . . . . 0.3(7) ? C2B C1B C6B C5B . . . . -0.7(7) ? I1B C1B C6B C5B . . . . 179.1(3) ? _shelx_res_file ; gil8757.res created by SHELXL-2014/7 TITL gil8757.res in Pca2(1) CELL 0.71073 17.9542 11.5049 7.3428 90.000 90.000 90.000 ZERR 8.000 0.0008 0.0005 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM 1/2+X, -Y, Z SYMM 1/2-X, Y, 1/2+Z SFAC C H F I UNIT 56 56 16 8 SIZE 0.072 0.073 0.249 TEMP -173.200 ACTA CONF L.S. 20 BOND $H FMAP 2 PLAN 10 OMIT 2 2 -2 OMIT 2 0 0 OMIT 4 1 -1 OMIT 4 1 1 TWIN WGHT 0.013200 BASF 0.30209 FVAR 0.23972 I1A 4 0.313917 0.525610 0.702624 11.00000 0.00768 0.01779 = 0.01054 0.00320 -0.00047 0.00005 F1A 3 0.308730 0.464881 0.962758 11.00000 0.01354 0.04183 = 0.01308 0.00990 0.00112 0.00157 F2A 3 0.331889 0.584130 0.450946 11.00000 0.01515 0.02643 = 0.01302 0.00601 -0.00083 -0.00336 C1A 1 0.420584 0.585849 0.762450 11.00000 0.00664 0.01631 = 0.01172 0.00221 -0.00191 0.00193 C2A 1 0.481602 0.523042 0.701802 11.00000 0.01463 0.01197 = 0.00879 0.00094 0.00126 0.00032 AFIX 43 H2A 2 0.475196 0.450363 0.642424 11.00000 -1.20000 AFIX 0 C3A 1 0.552218 0.568559 0.729646 11.00000 0.01555 0.01172 = 0.01041 -0.00052 0.00336 0.00477 AFIX 43 H3A 2 0.594535 0.525906 0.690065 11.00000 -1.20000 AFIX 0 C4A 1 0.562188 0.675377 0.814357 11.00000 0.01431 0.01546 = 0.01077 0.00608 -0.00416 -0.00442 C5A 1 0.499685 0.734983 0.879237 11.00000 0.01957 0.00907 = 0.01159 -0.00205 -0.00092 0.00192 AFIX 43 H5A 2 0.506163 0.806299 0.942497 11.00000 -1.20000 AFIX 0 C6A 1 0.427849 0.691349 0.852531 11.00000 0.01608 0.01659 = 0.00996 0.00109 0.00139 0.00514 AFIX 43 H6A 2 0.385359 0.732559 0.894669 11.00000 -1.20000 AFIX 0 C7A 1 0.639433 0.725919 0.834109 11.00000 0.01378 0.02889 = 0.02243 0.00085 -0.00103 -0.00870 AFIX 137 H7A1 2 0.635998 0.804222 0.885972 11.00000 -1.50000 H7A2 2 0.663305 0.729919 0.714249 11.00000 -1.50000 H7A3 2 0.669102 0.676399 0.914917 11.00000 -1.50000 AFIX 0 I1B 4 0.317036 0.865274 0.312358 11.00000 0.00716 0.01303 = 0.01015 -0.00017 0.00036 0.00077 F1B 3 0.327032 0.844684 0.582118 11.00000 0.01289 0.03583 = 0.00916 -0.00143 -0.00060 -0.00188 F2B 3 0.324994 0.888874 0.040375 11.00000 0.01330 0.02995 = 0.01056 0.00276 -0.00069 0.00256 C1B 1 0.433648 0.865242 0.307979 11.00000 0.00683 0.01369 = 0.00957 -0.00225 -0.00345 -0.00195 C2B 1 0.471480 0.766898 0.367214 11.00000 0.01298 0.01184 = 0.01223 0.00017 0.00545 -0.00218 AFIX 43 H2B 2 0.445170 0.700231 0.408317 11.00000 -1.20000 AFIX 0 C3B 1 0.548643 0.768748 0.364680 11.00000 0.00848 0.01610 = 0.01040 0.00096 -0.00125 0.00527 AFIX 43 H3B 2 0.575343 0.701946 0.403688 11.00000 -1.20000 AFIX 0 C4B 1 0.588008 0.866232 0.306292 11.00000 0.01334 0.01685 = 0.01289 -0.00533 -0.00236 -0.00079 C5B 1 0.547965 0.963877 0.246085 11.00000 0.01535 0.01115 = 0.01554 0.00140 0.00171 -0.00640 AFIX 43 H5B 2 0.574154 1.030624 0.204844 11.00000 -1.20000 AFIX 0 C6B 1 0.471341 0.964116 0.246059 11.00000 0.01339 0.01331 = 0.00946 0.00013 0.00218 0.00290 AFIX 43 H6B 2 0.444496 1.030209 0.204751 11.00000 -1.20000 AFIX 0 C7B 1 0.672887 0.866583 0.307599 11.00000 0.00916 0.02459 = 0.02552 -0.00764 -0.00111 -0.00101 AFIX 137 H7B1 2 0.690731 0.903915 0.419347 11.00000 -1.50000 H7B2 2 0.691282 0.909642 0.201590 11.00000 -1.50000 H7B3 2 0.691231 0.786417 0.302701 11.00000 -1.50000 AFIX 0 HKLF 4 REM gil8757.res in Pca2(1) REM R1 = 0.0197 for 3134 Fo > 4sig(Fo) and 0.0241 for all 3384 data REM 184 parameters refined using 1 restraints END WGHT 0.0132 0.0000 REM Highest difference peak 0.410, deepest hole -0.551, 1-sigma level 0.107 Q1 1 0.5068 0.7845 0.3510 11.00000 0.05 0.41 Q2 1 0.3890 0.8387 0.8166 11.00000 0.05 0.40 Q3 1 0.5001 0.7222 0.3061 11.00000 0.05 0.39 Q4 1 0.4966 0.7645 0.5843 11.00000 0.05 0.39 Q5 1 0.4752 0.8285 0.9630 11.00000 0.05 0.38 Q6 1 0.3208 0.9588 0.3152 11.00000 0.05 0.38 Q7 1 0.5120 0.9378 0.2482 11.00000 0.05 0.37 Q8 1 0.6192 0.8731 0.2872 11.00000 0.05 0.37 Q9 1 0.5215 1.1580 0.1422 11.00000 0.05 0.36 Q10 1 0.3796 0.5869 0.3380 11.00000 0.05 0.36 ; _shelx_res_checksum 39713 _shelx_hkl_file ; 0 0 -1 0.40 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121.99 6.40 -7 9 -4 73.69 10.00 -7 -9 4 57.09 9.30 -7 -9 -4 91.29 10.10 7 9 -4 68.79 9.50 -7 -9 -4 70.79 7.00 7 -9 -5 124.49 10.80 -7 9 -5 100.29 13.00 -7 -9 5 120.39 13.90 7 9 -5 97.69 12.50 -7 -9 -5 113.29 11.00 -7 -9 -5 111.69 8.00 -7 9 -6 268.67 19.90 7 -9 -6 234.68 15.00 -7 -9 6 246.28 18.60 -7 -9 -6 230.08 14.00 7 9 -6 238.38 18.40 -7 -9 7 17.10 9.90 7 -9 7 25.60 9.50 -7 10 0 -0.60 4.50 -7 -10 0 -3.80 4.80 -7 10 0 0.00 4.40 7 10 0 1.60 3.40 -7 -10 0 -4.40 5.60 -7 -10 1 41.10 7.50 -7 10 -1 32.00 6.90 -7 -10 1 26.60 7.20 7 10 1 26.40 3.30 -7 -10 -1 34.60 8.20 -7 10 1 42.20 5.80 -7 -10 -1 30.90 5.90 -7 10 1 24.10 4.90 7 10 -1 25.40 5.60 -7 10 -2 664.03 29.70 -7 -10 2 616.44 29.90 -7 -10 2 677.73 31.80 -7 10 2 649.43 26.30 -7 -10 -2 636.24 27.70 -7 -10 -2 653.13 30.70 -7 10 2 653.23 26.30 -7 10 -3 36.50 8.10 -7 -10 3 32.20 8.30 -7 -10 3 11.20 7.50 -7 -10 -3 36.10 5.50 7 10 -3 36.10 7.50 -7 -10 4 1002.30 43.30 -7 10 -4 1002.00 42.50 -7 -10 -4 937.61 44.10 7 10 -4 984.10 42.10 -7 -10 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782.52 30.90 -7 -12 0 772.92 37.00 -7 -12 0 692.43 33.60 -7 12 -1 -1.30 7.10 -7 12 -1 6.50 7.00 7 12 1 5.20 2.60 -7 -12 1 7.70 8.30 7 12 -1 4.60 10.50 -7 12 1 1.70 4.90 -7 -12 -1 5.60 8.10 -7 -12 -1 5.80 6.10 -7 12 1 8.80 5.20 -7 12 -2 470.05 24.80 -7 -12 2 470.45 29.10 -7 -12 -2 468.05 23.40 -7 12 2 470.95 20.20 7 12 -2 464.05 24.20 -7 12 2 494.15 20.20 -7 -12 -2 515.05 27.80 -7 -12 3 19.90 9.30 -7 12 -3 2.70 7.90 -7 -12 -3 16.00 6.70 -7 -12 -3 22.70 9.00 7 12 -3 -4.10 7.60 -7 -12 4 11.30 10.00 -7 12 -4 23.20 9.60 -7 -12 -4 44.70 10.20 7 12 -4 34.70 10.40 7 13 0 8.50 6.00 -7 13 0 -0.90 6.90 -7 -13 0 15.00 9.80 -7 -13 1 72.99 12.90 -7 13 -1 71.49 9.90 -7 13 -1 83.99 11.80 7 13 -1 55.49 12.40 -7 -13 -1 90.29 13.00 -7 -13 -1 80.59 13.40 -7 13 1 80.69 10.00 -7 13 1 88.29 11.60 -7 13 -2 351.96 21.10 -7 -13 2 362.56 24.40 7 13 -2 363.66 20.90 -7 -13 -2 351.56 24.30 -7 -13 -2 323.37 20.40 -7 13 -3 39.20 10.60 -7 -13 3 17.10 13.10 -7 -13 -3 18.40 8.60 -7 -13 -3 23.50 10.00 7 13 -3 0.80 8.60 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3.00 8 -1 -5 20.80 4.10 -8 -1 5 19.90 3.40 8 -1 -5 17.30 4.10 -8 -1 5 18.80 5.20 8 1 -5 15.20 4.30 -8 1 5 14.10 3.40 8 1 -5 22.70 4.60 8 -1 5 17.30 2.90 -8 -1 6 877.51 33.90 8 -1 -6 836.22 34.40 8 1 6 847.32 32.80 8 -1 -6 878.91 35.30 -8 1 6 864.71 33.40 8 1 -6 853.41 35.80 8 1 -6 896.51 35.30 8 -1 6 866.81 33.10 8 -1 -7 17.90 6.00 8 -1 -7 25.80 5.80 -8 1 -7 22.20 5.50 -8 -1 7 21.60 3.70 -8 -1 7 17.10 5.60 8 1 -7 25.40 5.70 8 1 -7 26.30 6.00 8 -1 7 18.90 2.90 -8 1 -8 222.38 15.40 8 -1 -8 230.68 15.70 -8 -1 -8 234.08 14.30 8 1 -8 239.78 16.20 8 -2 0 1381.36 53.29 -8 -2 0 1458.65 53.29 8 2 0 1366.86 52.99 8 2 0 1467.95 54.09 -8 2 0 1492.75 53.49 -8 -2 0 1376.86 53.49 8 2 1 27.40 3.00 -8 -2 1 19.70 3.10 8 -2 -1 18.90 3.00 8 2 1 20.80 3.40 -8 -2 1 19.40 3.10 8 -2 -1 19.40 3.10 -8 2 -1 16.10 3.00 -8 2 1 26.30 3.60 8 -2 1 18.50 3.00 8 2 -1 15.50 3.30 -8 -2 -1 23.00 3.00 -8 -2 -1 20.90 3.00 8 2 -1 25.20 3.40 -8 -2 2 751.62 29.20 8 -2 -2 736.03 28.60 8 2 2 749.13 28.90 -8 -2 2 722.13 28.90 8 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20.50 7.90 -23 -1 -1 30.00 9.30 -23 -2 0 189.08 15.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 15887 #============================================================================= # end of cif data for "gil8757" (compound p-TolI(III)F2) #============================================================================= #============================================================================= # end of cif file #=============================================================================