data_global # start Validation Reply Form _vrf_PLAT331_6a ; PROBLEM: Small Aver Phenyl C-C Dist C11 -C16 . 1.35 Ang. RESPONSE: Small disorder of the phenyl ring does not influence the correctness of the structure. ; _vrf_PLAT029_6c ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.925 Why? RESPONSE: Data collection to high angle and high redundancy, this is not considered to be serious error by us. ; # end Validation Reply Form #Added by publCIF (Cs márc. 21 15:18:30 2019) _publcif_datablock.id '{da566d5c-3912-491c-be16-050ebf2efa3f}' _audit_update_record ; 2018-05-30 # Formatted by publCIF ; # publcif _publ_body_element loop start loop_ _publ_body_element _publ_body_title _publ_body_contents section ; Introduction ; ; ; section ; Experimental ; ; ; subsection ; Synthesis and crystallization ; ; ; subsection ; Refinement ; ; Crystal data, data collection and structure refinement details are summarized in Table 1. ; section ; Results and discussion ; ; ; # publcif _publ_body_element loop end _audit_creation_method 'APEX3 v2017.3-0' _publ_requested_journal 'ACS Omega' _publ_contact_author_name 'Attila B\'enyei' _publ_contact_author_address ; University of Debrecen Department of Pharmaceutical Chemistry Laboratory for X-ray Diffraction. Egyetem ter 1 H4032 Debrecen Hungary ; _publ_contact_author_email 'benyei.attila@science.unideb.hu' _publ_contact_author_fax ? _publ_contact_author_phone '+3652512900' loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'T\'oth, Bal\'azs L.' ; ELTE \#8220;Lend\"ulet\#8221; Catalysis and Organic Synthesis Research Group, Institute of Chemistry, E\"otv\"os Lor\'and University, Faculty of Science, P\'azm\'any P\'eter stny. 1/A, H-1117 Budapest, Hungary ; . ? 'B\'eke, Ferenc' ; ELTE \#8220;Lend\"ulet\#8221; Catalysis and Organic Synthesis Research Group, Institute of Chemistry, E\"otv\"os Lor\'and University, Faculty of Science, P\'azm\'any P\'eter stny. 1/A, H-1117 Budapest, Hungary ; . . 'Egyed, Orsolya' ; Research Centre for Natural Sciences of the Hungarian Academy of Sciences. H-1117 Hungary, Budapest, Magyar Tud\'osok k\"or\'utja 2. ; . . 'B\'enyei, Attila' ; University of Debrecen Department of Pharmaceutical Chemistry Egyetem t\'er 1 H-4032 Debrecen Hungary ; . . 'Stirling, Andr\'as' ; Research Centre for Natural Sciences of the Hungarian Academy of Sciences. H-1117 Hungary, Budapest, Magyar Tud\'osok k\"or\'utja 2. ; . . 'Nov\'ak, Zolt\'an' ; Research Centre for Natural Sciences of the Hungarian Academy of Sciences. H-1117 Hungary, Budapest, Magyar Tud\'osok k\"or\'utja 2. ; . . _publ_section_title ; Synthesis of Multifunctional Aryl(trifloxyalkenyl)iodonium Salts ; _publ_section_abstract ; (type here to add) ; _publ_section_references ; (type here to add) ; data_7a _publcif_datablock.id '{272c6742-734a-498d-aff4-7f6251c31876}' _chemical_name_systematic ? _chemical_name_common 'Novak BF317' _chemical_formula_moiety 'C9 H7 F3 I O3 S, C F3 O3 S' _chemical_formula_sum 'C10 H7 F6 I O6 S2' _chemical_formula_iupac ? _chemical_formula_weight 528.18 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' 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' _cell_length_a 11.402(3) _cell_length_b 6.1909(18) _cell_length_c 25.548(7) _cell_angle_alpha 90 _cell_angle_beta 101.426(10) _cell_angle_gamma 90 _cell_volume 1767.7(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 85 _cell_measurement_theta_min 4.8494 _cell_measurement_theta_max 27.4554 _cell_measurement_temperature 298.(2) _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.754 _exptl_crystal_size_mid 0.147 _exptl_crystal_size_min 0.124 _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2017)' _exptl_absorpt_correction_T_min 0.500 _exptl_absorpt_correction_T_max 0.745 _exptl_special_details ; ; _diffrn_ambient_temperature 298.(2) _diffrn_source 'microsource sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'multilayer mirror ' _diffrn_measurement_device_type 'Bruker D8 Venture with CMOS detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 22513 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_unetI/netI 0.0286 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.36 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _refine_special_details ; ; _reflns_number_total 3243 _reflns_number_gt 3012 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.1030 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_number_reflns 3243 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+1.1695P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.935 _refine_diff_density_min -0.603 _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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 'APEX3 v2017.3-0 (Bruker AXS Inc., 2017)' _computing_cell_refinement 'APEX3 v2017.3-0 (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_molecular_graphics ? _computing_publication_material ? 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 C C10 0.5622(7) 0.3831(16) 0.2330(3) 0.119(3) Uani d . . . 1 . . C C1 0.3635(4) 0.4629(8) 0.36248(16) 0.0623(10) Uani d . . . 1 . . H H1 0.367999 0.612529 0.360449 0.075 Uiso calc U . R 1 . . C C2 0.3665(4) 0.3493(8) 0.32149(18) 0.0693(12) Uani d . . . 1 . . H H2 0.363835 0.199368 0.323084 0.083 Uiso calc U . R 1 . . C C11 0.1835(3) 0.4664(7) 0.43611(14) 0.0527(8) Uani d . . . 1 . . C C12 0.1879(5) 0.6576(8) 0.4629(2) 0.0750(13) Uani d . . . 1 . . H H12 0.260517 0.717823 0.479422 0.09 Uiso calc U . R 1 . . C C13 0.0810(6) 0.7586(11) 0.4646(3) 0.0995(19) Uani d . . . 1 . . H H13 0.080684 0.890254 0.482137 0.119 Uiso calc U . R 1 . . C C14 -0.0237(6) 0.6655(12) 0.4407(3) 0.102(2) Uani d . . . 1 . . H H14 -0.095363 0.734047 0.442532 0.123 Uiso calc U . R 1 . . C C15 -0.0267(4) 0.4756(13) 0.4142(2) 0.101(2) Uani d . . . 1 . . H H15 -0.099636 0.415389 0.39812 0.121 Uiso calc U . R 1 . . C C16 0.0804(4) 0.3700(10) 0.4111(2) 0.0777(13) Uani d . . . 1 . . H H16 0.080914 0.240105 0.392886 0.093 Uiso calc U . R 1 . . C C20 0.3603(6) 0.1476(11) 0.6279(2) 0.0898(18) Uani d . . . 1 . . O O11 0.3740(3) 0.4547(6) 0.27372(13) 0.0830(10) Uani d . . . 1 . . O O12 0.3401(5) 0.4299(11) 0.17861(16) 0.1340(19) Uani d . . . 1 . . O O13 0.3932(4) 0.1000(8) 0.23209(16) 0.0973(12) Uani d . . . 1 . . O O21 0.2950(3) 0.1175(6) 0.52654(12) 0.0706(8) Uani d . . . 1 . . O O22 0.5054(3) 0.1709(6) 0.56307(17) 0.0821(10) Uani d . . . 1 . . O O23 0.4138(3) -0.1720(5) 0.57366(16) 0.0789(10) Uani d . . . 1 . . F F11 0.6160(4) 0.3360(10) 0.2810(2) 0.150(2) Uani d . . . 1 . . F F12 0.5769(6) 0.5912(12) 0.2266(3) 0.192(3) Uani d . . . 1 . . F F13 0.6038(6) 0.2820(14) 0.1983(3) 0.221(4) Uani d . . . 1 . . F F21 0.4519(4) 0.1182(9) 0.66863(13) 0.1299(15) Uani d . . . 1 . . F F22 0.2659(4) 0.0455(9) 0.63723(16) 0.1353(17) Uani d . . . 1 . . F F23 0.3361(4) 0.3570(7) 0.62614(17) 0.1299(16) Uani d . . . 1 . . S S10 0.40187(14) 0.3260(3) 0.22467(5) 0.0837(4) Uani d . . . 1 . . S S20 0.39810(9) 0.05573(17) 0.56627(4) 0.0571(3) Uani d . . . 1 . . I I1 0.34882(2) 0.31784(4) 0.43400(2) 0.05560(13) Uani 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 C10 0.108(5) 0.173(7) 0.090(4) -0.052(5) 0.054(4) -0.038(5) C1 0.060(2) 0.073(3) 0.056(2) 0.0103(19) 0.0161(18) 0.010(2) C2 0.074(3) 0.084(3) 0.054(2) 0.007(2) 0.024(2) 0.008(2) C11 0.0467(18) 0.067(2) 0.0461(18) 0.0190(17) 0.0125(15) 0.0042(17) C12 0.073(3) 0.073(3) 0.082(3) 0.018(2) 0.021(2) -0.013(2) C13 0.098(5) 0.095(4) 0.112(5) 0.046(4) 0.037(4) -0.003(4) C14 0.081(4) 0.143(6) 0.088(4) 0.062(4) 0.029(3) 0.018(4) C15 0.048(2) 0.163(6) 0.089(4) 0.018(3) 0.004(2) 0.001(4) C16 0.058(3) 0.100(3) 0.073(3) 0.011(2) 0.007(2) -0.011(3) C20 0.082(4) 0.129(5) 0.061(3) 0.038(3) 0.019(3) 0.000(3) O11 0.099(2) 0.102(3) 0.0571(17) 0.017(2) 0.0366(17) 0.0133(17) O12 0.154(4) 0.188(5) 0.054(2) 0.008(4) 0.007(2) 0.019(3) O13 0.101(3) 0.117(3) 0.075(2) -0.014(3) 0.021(2) -0.021(2) O21 0.0655(18) 0.086(2) 0.0587(17) 0.0232(16) 0.0092(13) 0.0077(15) O22 0.0621(19) 0.092(2) 0.096(3) 0.0017(16) 0.0246(18) -0.0034(18) O23 0.077(2) 0.071(2) 0.092(2) 0.0241(15) 0.0237(18) 0.0141(16) F11 0.081(3) 0.222(6) 0.140(4) -0.013(3) 0.008(3) -0.040(4) F12 0.202(6) 0.204(6) 0.186(6) -0.103(5) 0.076(5) 0.003(5) F13 0.153(5) 0.348(10) 0.201(6) -0.076(6) 0.126(5) -0.139(7) F21 0.127(3) 0.199(4) 0.0558(17) 0.041(3) -0.0008(18) -0.006(2) F22 0.112(3) 0.204(5) 0.111(3) 0.031(3) 0.073(2) 0.027(3) F23 0.145(4) 0.134(3) 0.110(3) 0.055(3) 0.023(3) -0.045(2) S10 0.0791(8) 0.1274(13) 0.0463(6) -0.0043(7) 0.0165(5) -0.0016(6) S20 0.0512(5) 0.0689(6) 0.0529(5) 0.0183(4) 0.0144(4) 0.0027(4) I1 0.04970(18) 0.0710(2) 0.04769(18) 0.01981(10) 0.01363(12) 0.00675(10) _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 C10 F13 . 1.252(9) ? C10 F11 . 1.291(9) ? C10 F12 . 1.314(11) ? C10 S10 . 1.832(7) ? C1 C2 . 1.267(6) ? C1 I1 . 2.072(4) ? C1 H1 . 0.93 ? C2 O11 . 1.401(5) ? C2 H2 . 0.93 ? C11 C16 . 1.360(6) ? C11 C12 . 1.363(6) ? C11 I1 . 2.108(3) ? C12 C13 . 1.378(8) ? C12 H12 . 0.93 ? C13 C14 . 1.358(10) ? C13 H13 . 0.93 ? C14 C15 . 1.353(10) ? C14 H14 . 0.93 ? C15 C16 . 1.401(8) ? C15 H15 . 0.93 ? C16 H16 . 0.93 ? C20 F22 . 1.310(8) ? C20 F23 . 1.325(7) ? C20 F21 . 1.332(6) ? C20 S20 . 1.805(5) ? O11 S10 . 1.570(4) ? O12 S10 . 1.402(5) ? O13 S10 . 1.418(5) ? O21 S20 . 1.444(3) ? O22 S20 . 1.432(4) ? O23 S20 . 1.429(3) ? 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 F13 C10 F11 . . 112.6(10) ? F13 C10 F12 . . 109.0(8) ? F11 C10 F12 . . 107.0(7) ? F13 C10 S10 . . 109.2(5) ? F11 C10 S10 . . 110.0(5) ? F12 C10 S10 . . 108.9(7) ? C2 C1 I1 . . 120.6(4) ? C2 C1 H1 . . 119.7 ? I1 C1 H1 . . 119.7 ? C1 C2 O11 . . 118.5(5) ? C1 C2 H2 . . 120.7 ? O11 C2 H2 . . 120.7 ? C16 C11 C12 . . 124.0(4) ? C16 C11 I1 . . 119.4(3) ? C12 C11 I1 . . 116.6(3) ? C11 C12 C13 . . 117.8(6) ? C11 C12 H12 . . 121.1 ? C13 C12 H12 . . 121.1 ? C14 C13 C12 . . 119.8(6) ? C14 C13 H13 . . 120.1 ? C12 C13 H13 . . 120.1 ? C15 C14 C13 . . 121.8(5) ? C15 C14 H14 . . 119.1 ? C13 C14 H14 . . 119.1 ? C14 C15 C16 . . 119.9(6) ? C14 C15 H15 . . 120.1 ? C16 C15 H15 . . 120.1 ? C11 C16 C15 . . 116.8(5) ? C11 C16 H16 . . 121.6 ? C15 C16 H16 . . 121.6 ? F22 C20 F23 . . 107.7(5) ? F22 C20 F21 . . 109.7(5) ? F23 C20 F21 . . 106.6(6) ? F22 C20 S20 . . 110.7(5) ? F23 C20 S20 . . 111.3(4) ? F21 C20 S20 . . 110.7(4) ? C2 O11 S10 . . 121.1(3) ? O12 S10 O13 . . 121.9(3) ? O12 S10 O11 . . 106.8(3) ? O13 S10 O11 . . 111.3(2) ? O12 S10 C10 . . 109.4(4) ? O13 S10 C10 . . 105.6(4) ? O11 S10 C10 . . 99.4(3) ? O23 S20 O22 . . 114.3(2) ? O23 S20 O21 . . 114.7(2) ? O22 S20 O21 . . 114.4(2) ? O23 S20 C20 . . 103.9(3) ? O22 S20 C20 . . 104.3(3) ? O21 S20 C20 . . 103.2(2) ? C1 I1 C11 . . 93.59(15) ? 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 C1 C2 O11 . . . . 178.7(3) ? C16 C11 C12 C13 . . . . 0.0(8) ? I1 C11 C12 C13 . . . . 179.7(5) ? C11 C12 C13 C14 . . . . 0.8(10) ? C12 C13 C14 C15 . . . . -0.9(11) ? C13 C14 C15 C16 . . . . 0.1(11) ? C12 C11 C16 C15 . . . . -0.7(8) ? I1 C11 C16 C15 . . . . 179.6(4) ? C14 C15 C16 C11 . . . . 0.7(9) ? C1 C2 O11 S10 . . . . 168.6(4) ? C2 O11 S10 O12 . . . . 147.1(4) ? C2 O11 S10 O13 . . . . 11.8(5) ? C2 O11 S10 C10 . . . . -99.2(5) ? F13 C10 S10 O12 . . . . -71.9(9) ? F11 C10 S10 O12 . . . . 164.0(6) ? F12 C10 S10 O12 . . . . 47.1(6) ? F13 C10 S10 O13 . . . . 61.0(9) ? F11 C10 S10 O13 . . . . -63.1(7) ? F12 C10 S10 O13 . . . . 179.9(5) ? F13 C10 S10 O11 . . . . 176.4(8) ? F11 C10 S10 O11 . . . . 52.3(7) ? F12 C10 S10 O11 . . . . -64.6(6) ? F22 C20 S20 O23 . . . . -56.7(5) ? F23 C20 S20 O23 . . . . -176.4(4) ? F21 C20 S20 O23 . . . . 65.2(6) ? F22 C20 S20 O22 . . . . -176.8(4) ? F23 C20 S20 O22 . . . . 63.4(5) ? F21 C20 S20 O22 . . . . -55.0(6) ? F22 C20 S20 O21 . . . . 63.3(5) ? F23 C20 S20 O21 . . . . -56.4(5) ? F21 C20 S20 O21 . . . . -174.8(5) ? 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 C1 H1 O22 3_666 0.93 2.57 3.141(6) 120.5 ? _shelx_res_file ; TITL mo_18097_0m_a.res in P2(1)/n mo_18097_0m.res created by SHELXL-2016/6 at 16:37:31 on 26-May-2018 CELL 0.71073 11.4022 6.1909 25.5482 90.000 101.426 90.000 ZERR 4.00 0.0032 0.0018 0.0066 0.000 0.010 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H O F S I UNIT 40 28 24 24 8 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 25 ACTA EQIV $1 -x+1, -y+1, -z+1 HTAB C1 O22_$1 L.S. 14 FMAP 2 PLAN 5 HTAB BOND $H CONF WGHT 0.062500 1.169500 FVAR 0.34533 C10 1 0.562196 0.383094 0.233040 11.00000 0.10792 0.17272 = 0.08962 -0.03810 0.05354 -0.05206 C1 1 0.363547 0.462859 0.362482 11.00000 0.05963 0.07294 = 0.05620 0.01046 0.01612 0.01030 AFIX 43 H1 2 0.367999 0.612529 0.360449 11.00000 -1.20000 AFIX 0 C2 1 0.366533 0.349319 0.321493 11.00000 0.07438 0.08414 = 0.05402 0.00815 0.02428 0.00680 AFIX 43 H2 2 0.363835 0.199368 0.323084 11.00000 -1.20000 AFIX 0 C11 1 0.183492 0.466407 0.436111 11.00000 0.04671 0.06661 = 0.04608 0.00420 0.01247 0.01896 C12 1 0.187874 0.657603 0.462885 11.00000 0.07313 0.07266 = 0.08170 -0.01306 0.02105 0.01846 AFIX 43 H12 2 0.260517 0.717823 0.479422 11.00000 -1.20000 AFIX 0 C13 1 0.081041 0.758639 0.464622 11.00000 0.09824 0.09515 = 0.11169 -0.00347 0.03677 0.04568 AFIX 43 H13 2 0.080684 0.890254 0.482137 11.00000 -1.20000 AFIX 0 C14 1 -0.023719 0.665498 0.440688 11.00000 0.08142 0.14264 = 0.08839 0.01806 0.02913 0.06171 AFIX 43 H14 2 -0.095363 0.734047 0.442532 11.00000 -1.20000 AFIX 0 C15 1 -0.026672 0.475627 0.414226 11.00000 0.04790 0.16322 = 0.08851 0.00069 0.00355 0.01771 AFIX 43 H15 2 -0.099636 0.415389 0.398120 11.00000 -1.20000 AFIX 0 C16 1 0.080392 0.369963 0.411139 11.00000 0.05761 0.09951 = 0.07334 -0.01074 0.00680 0.01078 AFIX 43 H16 2 0.080914 0.240105 0.392886 11.00000 -1.20000 AFIX 0 C20 1 0.360339 0.147598 0.627894 11.00000 0.08194 0.12865 = 0.06098 0.00026 0.01935 0.03804 O11 3 0.373991 0.454688 0.273721 11.00000 0.09878 0.10193 = 0.05711 0.01334 0.03658 0.01704 O12 3 0.340113 0.429868 0.178609 11.00000 0.15440 0.18755 = 0.05432 0.01852 0.00657 0.00836 O13 3 0.393225 0.100036 0.232090 11.00000 0.10099 0.11671 = 0.07545 -0.02099 0.02057 -0.01395 O21 3 0.295007 0.117515 0.526537 11.00000 0.06555 0.08632 = 0.05870 0.00767 0.00919 0.02317 O22 3 0.505415 0.170866 0.563070 11.00000 0.06212 0.09209 = 0.09577 -0.00342 0.02464 0.00173 O23 3 0.413819 -0.171987 0.573658 11.00000 0.07653 0.07131 = 0.09169 0.01413 0.02371 0.02408 F11 4 0.615982 0.335990 0.281049 11.00000 0.08109 0.22237 = 0.13987 -0.03955 0.00825 -0.01331 F12 4 0.576910 0.591241 0.226593 11.00000 0.20177 0.20381 = 0.18619 0.00320 0.07573 -0.10326 F13 4 0.603768 0.281953 0.198350 11.00000 0.15263 0.34799 = 0.20054 -0.13900 0.12589 -0.07620 F21 4 0.451872 0.118187 0.668634 11.00000 0.12696 0.19930 = 0.05576 -0.00568 -0.00078 0.04104 F22 4 0.265930 0.045541 0.637225 11.00000 0.11188 0.20377 = 0.11112 0.02658 0.07281 0.03055 F23 4 0.336063 0.357018 0.626144 11.00000 0.14451 0.13449 = 0.10975 -0.04461 0.02255 0.05512 S10 5 0.401866 0.325963 0.224665 11.00000 0.07910 0.12739 = 0.04634 -0.00155 0.01647 -0.00433 S20 5 0.398101 0.055735 0.566265 11.00000 0.05117 0.06888 = 0.05294 0.00274 0.01438 0.01829 I1 6 0.348824 0.317842 0.434003 11.00000 0.04970 0.07104 = 0.04769 0.00675 0.01363 0.01981 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_18097_0m_a.res in P2(1)/n REM R1 = 0.0292 for 3012 Fo > 4sig(Fo) and 0.0338 for all 3243 data REM 226 parameters refined using 0 restraints END WGHT 0.0554 0.7266 REM Instructions for potential hydrogen bonds HTAB C1 O22_$1 REM Highest difference peak 0.935, deepest hole -0.603, 1-sigma level 0.160 Q1 1 0.3096 0.2004 0.4238 11.00000 0.05 0.93 Q2 1 0.4018 0.3933 0.6464 11.00000 0.05 0.43 Q3 1 0.3343 -0.0039 0.3385 11.00000 0.05 0.43 Q4 1 0.4085 0.5484 0.6455 11.00000 0.05 0.42 Q5 1 -0.0006 0.5077 0.4384 11.00000 0.05 0.40 ; _shelx_res_checksum 11078 _shelx_hkl_file ; -2 0 0 131.59 5.30 -2 0 0 123.99 5.60 -2 0 0 128.69 5.30 2 0 0 128.79 5.30 2 0 0 132.59 5.30 3 0 0 0.50 0.30 -3 0 0 0.50 0.40 -3 0 0 0.50 0.30 -4 0 0 9999.00 463.75 4 0 0 9975.20 462.55 -5 0 0 1.20 0.90 -5 0 0 0.30 0.50 5 0 0 0.30 0.50 -5 0 0 1.00 0.60 5 0 0 0.50 0.60 6 0 0 237.28 10.40 -6 0 0 266.47 11.50 6 0 0 243.78 10.50 -6 0 0 240.18 10.90 -6 0 0 244.28 10.30 -6 0 0 230.18 10.40 -7 0 0 1.00 0.70 -7 0 0 1.30 0.80 -7 0 0 1.60 1.30 -7 0 0 0.90 0.80 7 0 0 1.00 0.80 -8 0 0 212.08 9.70 -8 0 0 203.28 9.40 8 0 0 218.38 9.70 8 0 0 205.68 9.70 -8 0 0 205.78 10.20 -8 0 0 233.68 10.80 -9 0 0 0.70 0.70 9 0 0 0.50 0.80 -9 0 0 -0.20 0.70 -9 0 0 0.40 1.50 -9 0 0 0.30 0.90 9 0 0 -0.30 0.60 -10 0 0 60.39 4.90 -10 0 0 64.39 3.70 10 0 0 56.09 3.90 -10 0 0 49.50 3.60 10 0 0 60.39 3.90 -11 0 0 1.60 0.90 11 0 0 2.50 1.20 -11 0 0 2.60 2.10 -12 0 0 30.90 3.80 12 0 0 30.30 2.90 -12 0 0 26.60 2.80 -12 0 0 28.90 2.60 -13 0 0 2.60 1.10 -13 0 0 3.70 2.10 -13 0 0 3.10 1.30 13 0 0 2.90 1.30 0 -1 0 0.40 0.20 0 -1 0 0.30 0.40 0 1 0 0.30 0.30 0 1 0 0.00 0.10 0 1 0 0.00 0.10 1 -1 0 9.30 1.00 -1 -1 0 10.00 0.80 -1 1 0 10.00 1.10 -1 1 0 12.20 0.90 1 1 0 12.70 0.90 1 1 0 11.40 0.80 -2 -1 0 6564.24 333.47 2 -1 0 8344.96 357.16 2 1 0 6721.33 346.97 -2 1 0 7253.87 348.57 3 1 0 1292.77 50.39 -4 1 0 1573.04 62.29 4 1 0 1589.84 61.79 -5 -1 0 204.48 9.50 5 -1 0 213.38 9.10 -5 -1 0 210.28 8.80 5 -1 0 237.48 9.80 5 -1 0 212.38 9.40 -5 -1 0 206.28 9.20 -5 1 0 210.78 9.30 5 1 0 209.38 8.80 -5 1 0 213.18 9.20 5 1 0 216.68 9.40 -5 1 0 212.88 10.30 6 -1 0 370.56 15.00 -6 -1 0 327.27 14.20 6 -1 0 350.76 14.30 -6 -1 0 336.77 13.90 -6 -1 0 335.57 14.80 -6 1 0 351.06 14.50 6 1 0 343.97 14.50 -6 1 0 342.17 14.40 6 1 0 343.97 13.90 -6 1 0 307.67 15.50 7 -1 0 528.15 21.50 -7 -1 0 503.35 20.20 7 -1 0 501.45 21.10 -7 -1 0 506.95 21.30 -7 -1 0 490.85 20.70 -7 1 0 508.75 20.80 -7 1 0 440.26 22.00 -7 1 0 509.35 20.80 7 1 0 510.65 20.30 7 1 0 509.75 21.00 -8 -1 0 432.26 17.10 -8 -1 0 410.06 17.60 -8 -1 0 406.16 18.30 8 -1 0 422.26 17.90 8 -1 0 428.16 17.60 -8 -1 0 410.96 18.40 -8 1 0 416.36 17.70 -8 1 0 412.96 19.40 8 1 0 419.26 17.30 8 1 0 427.36 18.00 -8 1 0 404.26 18.30 9 -1 0 84.09 4.50 -9 -1 0 73.89 3.90 -9 -1 0 77.39 5.20 -9 -1 0 75.69 4.90 9 -1 0 75.79 4.70 -9 -1 0 74.99 4.40 9 1 0 76.89 4.70 -9 1 0 69.09 4.30 9 1 0 70.79 4.10 -9 1 0 75.29 4.50 10 -1 0 7.70 1.80 -10 -1 0 4.70 1.50 10 -1 0 6.00 1.50 -10 -1 0 4.20 1.10 -10 -1 0 1.00 1.00 10 1 0 3.70 1.10 -10 1 0 1.90 1.30 -10 1 0 4.30 1.40 -10 1 0 8.80 2.60 -10 1 0 4.20 1.40 11 -1 0 72.49 4.90 -11 -1 0 66.69 3.90 -11 -1 0 78.39 5.60 -11 -1 0 72.09 4.60 -11 1 0 65.19 4.40 11 1 0 67.99 4.20 -11 1 0 64.59 5.90 12 -1 0 60.69 4.60 -12 -1 0 74.19 8.50 -12 -1 0 60.89 4.40 -12 -1 0 60.19 3.70 -12 1 0 62.79 5.90 12 1 0 62.19 4.00 -12 1 0 60.59 4.40 -12 1 0 59.09 4.10 -13 -1 0 21.40 2.90 -13 -1 0 23.80 4.40 -13 -1 0 18.90 2.10 13 -1 0 22.20 3.10 -13 1 0 25.20 3.20 -13 1 0 20.30 3.80 13 1 0 22.40 2.40 -13 1 0 21.80 3.70 0 -2 0 692.93 30.30 0 -2 0 752.72 29.20 0 2 0 795.32 29.30 0 2 0 743.13 29.20 0 2 0 698.73 30.40 -1 -2 0 808.12 36.80 -1 -2 0 868.41 35.70 -1 -2 0 903.81 35.70 1 -2 0 964.10 35.90 1 2 0 926.71 35.60 -1 2 0 900.11 35.60 -1 2 0 849.72 36.80 -1 2 0 946.41 35.90 1 2 0 943.01 35.70 -2 -2 0 1.10 0.50 2 -2 0 0.50 0.50 -2 -2 0 1.10 0.50 2 -2 0 0.60 0.70 2 2 0 0.50 0.40 -2 2 0 0.00 0.40 -2 2 0 1.40 0.90 -3 -2 0 512.65 20.90 -3 -2 0 522.05 20.80 3 -2 0 518.85 20.60 3 -2 0 523.45 21.10 3 -2 0 503.85 21.60 -3 2 0 478.55 21.80 3 2 0 510.15 21.00 -3 2 0 516.55 21.00 3 2 0 527.05 20.90 -4 -2 0 281.17 12.00 4 -2 0 291.87 11.90 4 -2 0 299.27 12.60 -4 -2 0 275.47 12.20 4 -2 0 286.97 12.80 -4 2 0 291.37 12.30 4 2 0 275.57 11.30 -4 2 0 261.47 13.00 4 2 0 290.47 12.20 4 2 0 286.07 12.20 5 -2 0 1203.18 46.50 5 -2 0 1159.98 46.20 -5 -2 0 1123.99 45.70 -5 -2 0 1129.59 46.10 5 -2 0 1171.28 45.60 5 2 0 1149.29 46.00 -5 2 0 1091.79 47.10 -5 2 0 1133.69 46.00 5 2 0 1182.68 45.00 6 -2 0 403.36 16.80 -6 -2 0 396.06 16.80 6 -2 0 409.66 17.40 -6 -2 0 384.46 17.30 6 -2 0 441.96 17.70 6 2 0 403.06 16.10 -6 2 0 401.56 17.20 -6 2 0 390.66 18.50 -6 2 0 393.96 16.90 -7 -2 0 35.30 3.00 -7 -2 0 32.30 2.50 7 -2 0 33.10 3.00 7 -2 0 34.50 2.50 7 -2 0 39.10 3.20 -7 2 0 30.50 2.70 7 2 0 33.80 2.80 7 2 0 32.70 1.90 -7 2 0 33.40 2.70 -7 2 0 31.80 3.60 8 -2 0 3.10 1.30 -8 -2 0 2.70 1.10 8 -2 0 4.90 1.20 -8 -2 0 1.70 1.10 8 -2 0 2.20 1.20 8 2 0 5.10 1.40 8 2 0 1.00 0.60 -8 2 0 2.70 1.30 -8 2 0 0.90 1.50 -8 2 0 2.50 1.10 -9 -2 0 204.68 9.50 9 -2 0 205.28 9.70 9 -2 0 209.68 10.40 -9 -2 0 209.58 10.40 9 -2 0 203.28 10.10 9 2 0 198.98 8.70 -9 2 0 197.78 9.80 -9 2 0 203.38 9.80 9 2 0 201.08 10.10 -9 2 0 181.08 11.50 10 -2 0 90.99 5.30 10 -2 0 99.19 6.10 -10 -2 0 92.69 6.20 -10 -2 0 98.49 6.30 -10 -2 0 87.19 5.30 10 -2 0 98.89 6.20 -10 2 0 99.99 5.70 10 2 0 94.89 4.70 -10 2 0 89.89 5.60 -10 2 0 89.59 7.40 11 -2 0 92.79 5.50 -11 -2 0 84.69 6.10 -11 -2 0 90.19 6.30 11 -2 0 92.49 6.00 -11 2 0 92.59 5.60 -11 2 0 96.09 5.80 -11 2 0 82.89 7.50 -11 2 0 84.59 5.90 11 2 0 85.59 4.50 -12 -2 0 29.90 3.00 12 -2 0 35.40 3.70 -12 -2 0 37.30 4.10 -12 2 0 31.40 3.30 -12 2 0 28.10 3.10 -12 2 0 33.30 4.70 12 2 0 32.50 2.60 0 -3 0 1.70 1.50 0 -3 0 0.00 0.50 0 3 0 0.10 0.50 0 3 0 -0.10 0.60 1 -3 0 355.56 17.50 -1 -3 0 376.96 16.00 -1 -3 0 443.66 19.00 -1 3 0 395.66 16.30 -1 3 0 394.96 16.10 1 3 0 408.46 16.10 -1 3 0 346.27 18.60 1 3 0 396.96 16.00 2 -3 0 185.08 10.00 -2 -3 0 198.68 8.90 -2 -3 0 200.18 8.80 2 -3 0 220.28 9.90 -2 -3 0 178.78 10.30 -2 3 0 201.78 9.00 2 3 0 213.18 8.80 -2 3 0 205.88 8.80 2 3 0 198.38 8.50 -2 3 0 176.48 10.30 3 -3 0 1413.06 58.69 3 -3 0 1456.45 57.79 -3 -3 0 1453.15 57.49 -3 -3 0 1494.85 57.49 3 3 0 1467.05 56.89 -3 3 0 1491.05 57.69 -3 3 0 1294.97 58.99 3 3 0 1511.75 57.49 -4 -3 0 75.89 4.20 -4 -3 0 70.49 4.30 4 -3 0 80.59 4.00 4 -3 0 79.69 4.60 4 -3 0 80.09 5.20 -4 3 0 69.59 5.30 4 3 0 81.29 4.50 -4 3 0 70.99 4.40 4 3 0 80.39 4.30 5 -3 0 89.79 4.40 -5 -3 0 84.99 4.50 -5 -3 0 82.79 4.70 5 -3 0 83.99 5.00 5 3 0 83.09 3.60 5 3 0 83.49 4.70 -5 3 0 73.79 5.70 5 3 0 80.79 4.80 -5 3 0 76.19 4.70 6 -3 0 42.10 3.50 -6 -3 0 39.60 3.40 -6 -3 0 45.50 3.00 6 -3 0 43.10 3.70 6 3 0 40.30 3.20 6 3 0 44.10 2.10 -6 3 0 49.60 3.50 -6 3 0 40.30 4.30 -7 -3 0 342.77 15.40 7 -3 0 383.46 16.70 7 -3 0 359.86 15.40 7 -3 0 369.56 16.30 -7 -3 0 354.86 16.20 7 3 0 359.86 14.30 7 3 0 361.26 16.10 -7 3 0 362.16 16.00 -7 3 0 338.47 17.70 8 -3 0 90.09 5.90 8 -3 0 100.79 5.30 8 -3 0 100.69 6.20 -8 -3 0 96.29 5.40 -8 -3 0 94.79 6.00 8 3 0 93.09 4.10 8 3 0 99.49 5.90 -8 3 0 101.09 5.80 -8 3 0 89.99 7.30 9 -3 0 45.90 4.00 -9 -3 0 40.50 3.10 9 -3 0 37.40 3.70 9 -3 0 38.20 3.00 -9 -3 0 41.10 3.80 -9 3 0 39.00 4.90 9 3 0 44.90 3.80 -9 3 0 35.80 3.30 -10 -3 0 46.20 4.50 -10 -3 0 53.99 3.80 10 -3 0 58.59 5.10 10 -3 0 49.50 5.00 -10 3 0 38.80 5.30 -10 3 0 50.99 4.00 10 3 0 36.40 3.80 -11 -3 0 24.40 3.50 11 -3 0 23.80 5.00 11 -3 0 27.10 3.40 11 -3 0 24.40 2.70 -11 -3 0 26.60 2.90 -11 3 0 30.20 5.20 -11 3 0 28.20 3.20 -12 -3 0 6.70 2.20 12 -3 0 4.90 1.90 -12 -3 0 6.20 1.80 -12 3 0 6.20 2.80 0 -4 0 188.58 11.30 0 -4 0 216.28 9.40 0 4 0 219.48 9.40 0 4 0 213.88 9.50 -1 -4 0 622.24 25.20 -1 -4 0 560.54 27.50 1 -4 0 576.94 27.30 -1 4 0 659.93 25.30 -1 4 0 630.04 25.60 1 4 0 655.73 25.30 1 4 0 638.84 25.30 -1 4 0 590.94 27.70 -2 -4 0 14.00 2.00 -2 -4 0 10.70 3.00 2 -4 0 19.40 3.20 -2 -4 0 12.40 1.70 2 4 0 13.60 1.80 2 4 0 14.90 1.80 -2 4 0 15.70 1.80 -2 4 0 13.60 3.50 -2 4 0 15.20 3.80 -3 -4 0 248.88 11.20 -3 -4 0 255.27 11.20 3 -4 0 239.58 12.70 -3 -4 0 230.48 13.30 3 4 0 264.97 13.10 3 4 0 249.08 10.60 -3 4 0 256.67 11.10 -3 4 0 232.68 13.20 -3 4 0 253.67 11.40 -4 -4 0 32.60 2.70 4 -4 0 36.60 3.10 4 -4 0 32.10 3.60 -4 -4 0 34.50 2.80 -4 4 0 30.80 2.60 4 4 0 32.50 2.10 -4 4 0 27.40 3.80 4 4 0 34.10 2.70 -4 4 0 32.80 2.90 -5 -4 0 233.78 10.60 5 -4 0 236.78 10.40 5 -4 0 235.68 12.10 5 -4 0 232.78 11.20 -5 -4 0 233.28 11.70 5 4 0 244.98 10.80 -5 4 0 198.08 12.40 -5 4 0 229.58 11.00 5 4 0 223.78 9.60 6 -4 0 -0.20 1.10 -6 -4 0 1.50 1.10 -6 -4 0 0.10 1.00 6 -4 0 1.50 0.90 6 -4 0 3.50 1.70 6 4 0 1.50 1.20 -6 4 0 0.50 1.10 6 4 0 0.60 0.50 -6 4 0 0.80 1.40 6 4 0 2.10 0.50 7 -4 0 1.00 1.30 -7 -4 0 1.20 1.20 7 -4 0 -0.30 0.80 7 -4 0 1.40 1.30 -7 -4 0 0.00 1.00 7 4 0 0.60 0.90 -7 4 0 0.10 1.50 8 -4 0 5.10 1.80 -8 -4 0 9.50 2.20 8 -4 0 6.80 1.90 -8 -4 0 7.00 1.60 8 -4 0 5.30 1.30 8 4 0 10.50 2.10 -8 4 0 6.80 2.60 -8 4 0 9.40 3.20 9 -4 0 45.00 4.50 9 -4 0 34.90 4.10 -9 -4 0 42.70 3.90 -9 -4 0 40.00 3.40 -9 4 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8.30 3.50 10 5 -4 6.00 0.90 9 -5 -4 42.10 4.40 -9 -5 4 41.60 3.40 9 -5 -4 35.70 4.10 -9 -5 4 31.70 3.80 9 5 -4 37.80 2.30 9 5 -4 35.50 2.30 -9 5 4 35.10 5.00 8 -5 -4 57.49 4.90 -8 -5 4 48.20 3.80 8 -5 -4 70.19 6.80 8 -5 -4 49.50 3.80 -8 5 4 42.20 5.50 8 5 -4 57.79 4.60 8 5 -4 49.20 2.90 7 -5 -4 14.60 2.60 -7 -5 4 15.70 2.60 -7 -5 4 18.20 2.40 7 -5 -4 21.90 4.10 7 5 -4 17.50 2.60 -7 5 4 20.00 4.80 -6 -5 4 13.20 2.00 6 -5 -4 9.70 1.90 -6 -5 4 14.90 2.50 6 -5 -4 14.10 3.20 6 -5 -4 12.50 2.30 6 5 -4 15.60 1.80 -6 5 4 18.30 4.50 6 5 -4 15.70 2.50 -6 5 4 17.00 2.10 5 -5 -4 182.08 9.70 -5 -5 4 176.38 9.40 -5 -5 4 194.18 9.00 -5 -5 4 176.18 11.90 5 -5 -4 189.48 10.80 -5 5 4 165.18 11.20 -5 5 4 176.68 8.60 5 5 -4 178.68 8.50 5 5 -4 198.28 9.50 -5 5 4 182.98 9.30 -4 -5 4 189.98 8.80 4 -5 -4 175.88 10.60 4 -5 -4 195.28 9.60 -4 -5 4 173.68 11.60 -4 -5 4 186.18 9.30 -4 5 4 168.48 11.20 4 5 -4 173.78 8.50 -4 5 4 181.48 9.20 -4 5 4 181.28 8.40 4 5 -4 180.78 9.20 3 -5 -4 15.30 3.70 3 -5 -4 14.00 2.30 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0 -7 4 28.10 3.20 0 7 4 28.10 2.10 0 7 -4 27.00 3.00 0 7 -4 26.20 3.50 0 7 4 30.30 2.90 1 -7 4 -0.50 1.20 -1 -7 -4 -0.10 1.40 1 7 4 0.70 0.70 -1 7 -4 0.90 1.30 -1 7 -4 0.60 1.00 1 7 4 2.40 1.30 -2 -7 -4 8.30 2.20 -2 7 -4 4.90 1.60 2 7 4 6.60 1.30 2 7 4 7.60 1.70 -3 -7 -4 -2.00 1.10 -3 -7 -4 -0.20 0.80 -3 7 -4 -0.20 1.50 -3 7 -4 2.00 1.30 3 7 4 -1.10 0.90 -13 0 5 48.10 4.00 -13 0 5 43.30 3.50 -13 0 5 53.69 4.90 13 0 -5 51.69 4.10 -12 0 5 2.00 0.90 -12 0 5 2.30 1.50 12 0 -5 4.20 1.50 -12 0 5 5.70 1.50 -12 0 5 5.30 2.00 -11 0 5 222.38 10.90 11 0 -5 227.98 11.10 -11 0 5 245.58 12.00 -11 0 5 226.38 10.60 10 0 -5 -0.40 0.70 -10 0 5 2.70 1.00 -10 0 5 0.60 0.70 10 0 -5 0.70 0.90 -10 0 5 -0.80 0.70 -10 0 5 1.30 1.40 9 0 -5 371.66 16.20 -9 0 5 361.86 15.90 9 0 -5 368.86 16.10 -9 0 5 365.16 16.10 -9 0 5 356.96 16.70 -9 0 5 414.86 17.10 -8 0 5 2.70 1.40 -8 0 5 0.80 0.80 -8 0 5 -0.60 0.80 -8 0 5 2.30 0.90 8 0 -5 0.60 0.90 7 0 -5 5.60 1.20 -7 0 5 7.80 1.70 -7 0 5 4.60 1.10 -7 0 5 6.00 1.10 -7 0 5 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2.10 4 3 -26 6.50 1.80 3 -3 -26 13.00 1.50 3 -3 -26 13.90 2.90 -3 -3 26 14.90 2.40 3 3 -26 14.80 2.90 3 3 -26 9.10 2.00 2 -3 -26 0.30 0.60 2 -3 -26 0.70 1.00 2 -3 -26 -2.20 0.90 2 -3 -26 0.00 1.00 -2 -3 26 0.60 1.40 2 3 -26 0.50 1.80 2 3 -26 -0.50 1.10 1 -3 -26 39.70 3.00 1 -3 -26 36.50 3.80 1 -3 -26 38.10 4.20 1 -3 -26 31.40 2.40 -1 -3 26 42.40 3.80 1 3 -26 35.00 4.60 1 3 -26 36.90 4.10 0 -3 -26 18.30 2.90 0 -3 -26 21.00 2.40 0 -3 26 20.00 2.90 0 3 -26 22.40 4.30 0 3 -26 13.20 2.90 -1 -3 -26 20.40 3.00 -1 -3 -26 19.50 2.60 -1 -3 -26 18.50 2.70 -1 -3 -26 19.50 2.10 -1 3 -26 21.80 3.60 -1 3 -26 22.80 3.70 2 -3 26 4.90 2.30 -2 -3 -26 5.90 1.80 -2 -3 -26 4.60 1.60 -2 -3 -26 6.70 2.20 -2 -3 -26 1.60 1.00 -2 3 -26 6.00 2.60 -2 3 -26 5.30 1.80 8 0 -27 1.50 1.60 8 0 -27 -0.60 0.80 8 0 -27 3.80 1.50 7 0 -27 30.20 2.50 7 0 -27 33.60 3.50 6 0 -27 -0.40 1.20 6 0 -27 -0.20 0.90 6 0 -27 -0.30 0.70 -6 0 27 0.40 0.90 5 0 -27 239.08 11.90 5 0 -27 246.18 12.10 -5 0 27 240.58 12.30 4 0 -27 0.00 1.10 -4 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43.30 4.00 6 1 -27 45.10 4.70 5 -1 -27 0.90 1.30 5 -1 -27 2.70 1.10 -5 -1 27 -0.10 1.80 5 -1 -27 2.10 1.20 -5 1 27 0.80 1.20 5 1 -27 0.50 1.40 5 1 -27 2.90 1.60 5 1 -27 4.00 0.80 4 -1 -27 5.20 1.50 4 -1 -27 3.90 2.10 4 -1 -27 5.80 1.30 4 1 -27 5.30 2.50 4 1 -27 5.90 1.80 -4 1 27 6.40 1.70 4 1 -27 6.50 0.80 3 -1 -27 191.38 9.40 3 -1 -27 186.88 8.40 3 -1 -27 188.38 9.50 3 1 -27 190.18 9.60 3 1 -27 166.28 7.40 3 1 -27 177.48 7.50 3 1 -27 191.08 13.40 2 -1 -27 89.49 5.60 2 -1 -27 89.39 6.20 2 -1 -27 93.89 5.30 2 1 -27 91.19 6.40 2 1 -27 99.59 8.50 1 -1 -27 16.20 2.20 1 -1 -27 21.70 3.00 1 -1 -27 17.30 2.20 1 -1 -27 18.00 2.60 1 1 -27 17.80 2.70 1 1 -27 17.30 3.50 0 -1 -27 1.00 1.00 0 -1 -27 0.60 0.80 0 -1 -27 -0.20 0.90 0 -1 -27 1.30 1.20 0 1 -27 0.30 1.20 0 1 -27 3.00 1.90 -1 -1 -27 23.10 2.70 -1 -1 -27 19.30 2.60 -1 -1 -27 16.30 2.30 -1 -1 -27 18.80 2.10 -1 1 -27 20.30 3.50 -1 1 -27 21.40 3.20 -2 -1 -27 40.00 2.90 -2 -1 -27 44.00 3.80 -2 -1 -27 37.10 3.20 -2 -1 -27 35.80 3.60 -2 1 -27 37.50 5.70 -2 1 -27 36.60 4.20 -2 1 -27 45.10 4.30 -3 -1 -27 28.20 2.40 -3 -1 -27 31.00 3.40 -3 -1 -27 32.80 3.50 -3 -1 -27 27.50 2.80 -3 1 -27 30.80 3.90 -3 1 -27 24.20 3.70 7 -2 -27 2.50 1.20 7 -2 -27 4.30 1.90 7 -2 -27 2.20 1.00 7 2 -27 1.30 1.50 -7 2 27 4.50 1.60 7 2 -27 2.50 0.80 7 2 -27 0.90 1.80 6 -2 -27 42.10 4.10 6 -2 -27 45.60 3.50 6 -2 -27 44.40 3.90 -6 2 27 42.90 3.60 6 2 -27 39.80 3.90 6 2 -27 40.60 2.30 6 2 -27 43.60 4.50 5 -2 -27 71.29 4.30 5 -2 -27 66.19 5.20 5 -2 -27 64.09 4.30 5 2 -27 65.39 4.90 -5 2 27 64.39 4.50 5 2 -27 65.49 5.40 4 -2 -27 88.89 5.20 -4 -2 27 97.29 5.00 4 -2 -27 92.29 6.20 4 -2 -27 90.59 5.30 4 2 -27 100.19 6.80 4 2 -27 87.19 6.00 3 -2 -27 19.80 2.20 -3 -2 27 16.70 3.80 3 -2 -27 24.00 3.30 -3 -2 27 20.40 2.40 3 2 -27 21.60 3.40 3 2 -27 10.80 2.30 2 -2 -27 9.40 1.70 -2 -2 27 12.40 2.50 2 -2 -27 8.20 2.30 2 2 -27 8.60 2.30 2 2 -27 7.00 2.10 2 2 -27 10.40 2.90 -1 -2 27 42.30 3.60 1 -2 -27 39.70 3.60 1 -2 -27 39.20 3.10 1 -2 -27 34.10 3.30 1 2 -27 33.10 4.10 1 2 -27 37.70 3.80 1 2 -27 40.30 4.20 0 -2 -27 110.29 6.70 0 -2 -27 112.09 6.40 0 -2 27 119.59 6.80 0 -2 -27 112.19 6.30 0 -2 -27 112.49 6.30 0 2 -27 118.39 7.60 0 2 -27 103.39 7.70 -1 -2 -27 24.90 2.80 -1 -2 -27 21.60 2.80 -1 -2 -27 24.50 2.70 -1 -2 -27 26.00 2.70 1 -2 27 20.00 2.80 -1 2 -27 22.60 3.60 -1 2 -27 22.80 3.60 -2 -2 -27 11.00 2.50 -2 -2 -27 6.10 1.50 -2 -2 -27 8.30 1.90 -2 -2 -27 6.00 1.50 -2 2 -27 9.40 2.70 -2 2 -27 5.10 2.00 -5 -3 27 4.30 1.50 5 -3 -27 3.00 1.30 5 -3 -27 2.90 1.60 5 3 -27 2.80 1.50 5 3 -27 -0.60 1.20 4 -3 -27 33.30 3.90 4 -3 -27 31.30 2.50 -4 -3 27 42.90 3.50 4 3 -27 41.00 3.90 4 3 -27 37.50 4.30 3 -3 -27 13.20 1.60 3 -3 -27 10.20 3.80 -3 -3 27 15.50 2.50 3 3 -27 15.30 2.80 3 3 -27 15.30 3.00 2 -3 -27 72.79 4.70 2 -3 -27 67.99 3.90 -2 -3 27 80.09 5.30 2 -3 -27 70.09 5.40 2 3 -27 65.79 5.90 2 3 -27 75.19 6.00 1 -3 -27 17.40 2.10 1 -3 -27 18.10 3.00 1 -3 -27 13.90 1.60 1 -3 -27 11.30 2.50 1 -3 -27 11.80 2.40 -1 -3 27 16.40 3.00 1 3 -27 14.20 2.90 1 3 -27 16.10 4.20 0 -3 -27 -0.50 1.10 0 -3 -27 1.20 1.20 0 -3 -27 1.10 0.70 0 -3 27 -1.40 1.30 0 -3 -27 -0.90 1.20 0 3 -27 -1.50 1.10 0 3 -27 -0.10 1.60 -1 -3 -27 1.00 0.80 -1 -3 -27 -0.50 1.10 -1 -3 -27 1.90 1.50 -1 -3 -27 3.70 1.50 -1 3 -27 4.00 3.10 -1 3 -27 1.10 1.60 8 0 -28 37.30 3.80 8 0 -28 33.70 3.60 -8 0 28 37.90 4.10 8 0 -28 32.40 2.60 7 0 -28 0.00 1.00 7 0 -28 1.70 1.30 7 0 -28 0.10 0.80 -7 0 28 -1.00 1.20 6 0 -28 134.49 7.80 6 0 -28 124.29 9.40 6 0 -28 128.59 6.30 5 0 -28 0.40 1.10 -5 0 28 1.50 0.90 5 0 -28 -0.40 0.80 5 0 -28 -1.30 1.00 4 0 -28 5.90 1.90 4 0 -28 4.30 1.60 4 0 -28 5.00 1.00 -4 0 28 5.20 1.90 3 0 -28 0.60 0.70 3 0 -28 0.10 0.60 3 0 -28 1.90 1.20 3 0 -28 1.10 1.10 2 0 -28 139.79 6.40 2 0 -28 145.49 8.30 2 0 -28 153.18 8.40 1 0 -28 2.70 1.90 1 0 -28 2.70 1.50 1 0 -28 0.30 0.60 1 0 -28 0.20 0.50 1 0 -28 -0.60 1.00 0 0 -28 51.29 4.40 0 0 -28 57.49 4.70 0 0 -28 56.09 4.20 0 0 -28 52.89 2.90 -1 0 -28 -0.20 0.80 -1 0 -28 1.00 1.40 -1 0 -28 0.80 1.30 -1 0 -28 -0.30 0.80 -2 0 -28 15.80 3.20 -2 0 -28 11.70 1.30 -2 0 -28 17.60 3.00 -2 0 -28 14.70 2.20 -3 0 -28 -1.90 0.90 -3 0 -28 -1.10 0.90 -3 0 -28 -0.90 0.50 -3 0 -28 0.70 1.40 7 -1 -28 20.10 2.80 7 -1 -28 18.00 2.10 7 -1 -28 25.70 3.60 7 1 -28 17.50 1.90 7 1 -28 15.80 2.90 7 1 -28 25.80 3.60 -7 1 28 21.30 3.10 6 -1 -28 8.00 2.20 6 -1 -28 6.00 1.30 6 -1 -28 4.70 1.50 -6 -1 28 4.20 1.90 6 1 -28 6.00 1.10 6 1 -28 5.50 2.00 -6 1 28 6.70 1.90 6 1 -28 2.90 1.50 -5 -1 28 17.00 3.20 5 -1 -28 16.40 2.60 5 -1 -28 21.00 2.10 5 -1 -28 16.70 2.50 5 1 -28 18.20 2.70 5 1 -28 14.20 4.60 5 1 -28 18.70 1.50 -5 1 28 21.20 2.90 4 -1 -28 146.09 7.20 4 -1 -28 153.28 8.10 -4 -1 28 155.98 9.10 4 -1 -28 152.68 8.40 4 1 -28 156.38 8.50 4 1 -28 140.99 6.30 4 1 -28 152.98 8.80 -3 -1 28 37.20 4.10 3 -1 -28 39.60 3.70 3 -1 -28 37.10 2.70 3 -1 -28 40.80 3.50 3 1 -28 32.10 3.70 3 1 -28 35.00 3.60 2 -1 -28 13.10 2.50 2 -1 -28 12.50 2.20 2 -1 -28 12.00 1.80 2 -1 -28 13.30 1.70 2 1 -28 6.10 1.90 2 1 -28 19.30 4.20 2 1 -28 13.20 2.40 1 -1 -28 33.00 3.10 1 -1 -28 29.00 2.70 1 -1 -28 33.00 3.20 1 -1 -28 30.80 3.00 1 1 -28 35.50 3.40 1 1 -28 31.00 3.70 1 1 -28 31.00 3.60 0 -1 -28 58.59 3.70 0 -1 -28 55.19 4.30 0 -1 -28 58.39 4.50 0 -1 -28 55.39 4.20 0 1 -28 56.69 4.40 0 1 -28 54.19 4.90 -1 -1 -28 46.50 3.20 -1 -1 -28 51.39 4.20 -1 -1 -28 47.00 4.60 -1 -1 -28 47.80 4.10 -1 1 -28 45.70 4.00 -1 1 -28 43.60 4.60 -1 1 -28 46.20 4.50 -2 -1 -28 47.60 3.70 -2 -1 -28 53.89 4.20 -2 -1 -28 45.30 4.10 -2 -1 -28 45.50 3.20 -2 1 -28 47.20 4.00 -2 1 -28 46.80 4.80 -2 1 -28 46.50 4.50 6 -2 -28 57.59 3.80 6 -2 -28 61.49 4.90 6 -2 -28 47.90 3.70 6 2 -28 46.60 2.50 6 2 -28 53.69 4.40 6 2 -28 53.69 4.80 -6 2 28 47.60 3.90 5 -2 -28 50.09 3.60 5 -2 -28 51.39 3.80 5 -2 -28 56.59 4.60 5 2 -28 49.50 4.80 5 2 -28 54.19 4.40 4 -2 -28 -1.50 0.80 4 -2 -28 2.20 1.60 -4 -2 28 0.60 1.00 4 -2 -28 0.00 1.00 4 2 -28 1.40 1.50 4 2 -28 -0.90 1.30 -3 -2 28 30.80 2.70 3 -2 -28 27.30 2.70 3 -2 -28 32.30 3.50 3 2 -28 25.90 3.80 3 2 -28 27.30 3.30 2 -2 -28 89.99 5.80 -2 -2 28 97.89 5.60 2 -2 -28 98.59 6.30 2 -2 -28 88.29 5.40 2 2 -28 94.79 6.80 2 2 -28 97.89 6.30 2 2 -28 86.99 6.40 1 -2 -28 106.29 6.20 1 -2 -28 95.49 5.70 1 -2 -28 98.69 6.20 -1 -2 28 100.79 6.00 1 2 -28 103.69 6.50 1 2 -28 88.19 6.90 1 2 -28 105.89 7.20 0 -2 -28 8.50 1.80 0 -2 -28 10.50 2.20 0 -2 -28 8.20 2.00 0 -2 -28 9.20 1.80 0 -2 28 13.50 2.70 0 2 -28 11.80 2.30 0 2 -28 10.30 2.50 0 2 -28 11.10 2.90 -1 -2 -28 18.20 2.50 -1 -2 -28 11.60 2.10 -1 -2 -28 13.80 2.20 -1 -2 -28 16.40 2.60 -1 2 -28 15.30 3.50 -1 2 -28 12.20 2.80 3 -3 -28 58.59 5.00 -3 -3 28 61.39 4.40 3 -3 -28 53.09 3.30 3 3 -28 57.69 4.70 3 3 -28 55.49 5.30 -2 -3 28 0.80 1.50 2 -3 -28 1.40 0.70 2 3 -28 0.20 1.40 2 3 -28 1.90 1.30 2 3 -28 1.20 1.80 7 0 -29 15.60 1.80 -7 0 29 13.40 2.50 7 0 -29 12.90 2.50 7 0 -29 19.60 5.00 6 0 -29 -1.20 0.80 6 0 -29 -2.30 0.70 -6 0 29 0.20 1.10 6 0 -29 -1.50 0.60 5 0 -29 -1.30 0.90 5 0 -29 -0.10 0.60 4 0 -29 -0.60 1.00 4 0 -29 -0.80 1.10 4 0 -29 0.30 0.60 3 0 -29 91.19 6.00 3 0 -29 94.89 4.50 3 0 -29 95.09 6.20 3 0 -29 95.29 4.90 2 0 -29 0.10 1.10 2 0 -29 -1.10 1.00 2 0 -29 0.20 0.50 1 0 -29 45.40 3.90 1 0 -29 50.09 4.10 1 0 -29 49.00 2.60 1 0 -29 51.19 4.90 1 0 -29 50.09 2.80 0 0 -29 7.00 2.10 0 0 -29 2.40 0.70 0 0 -29 3.00 0.70 0 0 -29 3.30 1.50 0 0 -29 3.40 1.30 -1 0 -29 107.39 6.60 -1 0 -29 117.79 7.40 -1 0 -29 119.39 5.60 -1 0 -29 116.59 7.50 6 -1 -29 28.00 3.30 6 -1 -29 29.80 3.20 6 -1 -29 33.00 2.50 6 1 -29 33.70 3.50 6 1 -29 31.30 2.20 6 1 -29 35.10 3.70 -6 1 29 37.20 3.50 5 -1 -29 63.09 4.50 5 -1 -29 59.09 4.60 5 -1 -29 55.79 3.50 5 1 -29 56.09 4.80 5 1 -29 60.69 4.70 -5 1 29 61.59 4.70 5 1 -29 52.59 2.90 4 -1 -29 3.30 1.10 -4 -1 29 2.10 1.50 4 -1 -29 4.00 1.50 4 -1 -29 1.90 1.30 4 1 -29 7.50 2.20 4 1 -29 3.50 0.60 4 1 -29 2.90 0.60 4 1 -29 2.30 1.60 3 -1 -29 2.80 1.50 3 -1 -29 3.40 1.50 3 -1 -29 3.70 1.10 3 1 -29 4.10 1.60 3 1 -29 1.30 1.60 2 -1 -29 20.60 2.60 2 -1 -29 21.10 2.00 2 -1 -29 19.30 2.80 2 -1 -29 26.40 3.40 2 1 -29 19.00 3.20 2 1 -29 25.60 3.40 2 1 -29 20.40 2.90 1 -1 -29 85.39 4.90 1 -1 -29 86.69 5.60 1 -1 -29 86.49 6.30 1 1 -29 87.99 6.30 1 1 -29 85.79 5.60 1 1 -29 74.59 5.70 0 -1 -29 4.70 1.70 0 -1 -29 6.90 2.00 0 -1 -29 7.40 2.10 0 -1 -29 4.50 1.20 0 1 -29 6.30 2.30 0 1 -29 4.30 1.90 0 1 -29 2.70 1.40 -1 -1 -29 36.90 2.70 -1 -1 -29 35.70 3.30 -1 -1 -29 36.00 3.50 -1 -1 -29 35.60 3.60 -1 1 -29 33.60 3.90 -1 1 -29 33.50 3.40 -1 1 -29 36.40 4.20 5 -2 -29 7.00 2.20 5 -2 -29 7.00 1.50 5 -2 -29 6.80 1.80 5 2 -29 9.80 2.30 5 2 -29 11.50 2.80 4 -2 -29 32.50 2.70 4 -2 -29 31.30 3.40 4 -2 -29 29.00 2.80 4 2 -29 33.30 4.00 4 2 -29 31.30 3.50 3 -2 -29 39.50 3.30 3 -2 -29 43.50 3.20 3 -2 -29 49.40 4.20 3 2 -29 49.00 4.80 3 2 -29 40.60 3.80 2 -2 -29 24.00 3.00 2 -2 -29 23.90 3.40 2 -2 -29 23.00 2.50 2 2 -29 26.70 3.80 2 2 -29 21.00 3.10 2 2 -29 26.10 3.10 1 -2 -29 2.20 1.20 1 -2 -29 -0.40 0.90 1 -2 -29 4.90 3.00 1 2 -29 1.50 1.20 1 2 -29 2.50 1.70 1 2 -29 0.80 1.50 0 -2 -29 17.80 2.60 0 -2 -29 29.10 2.80 0 -2 -29 26.80 3.10 0 -2 -29 27.80 2.80 0 2 -29 30.10 3.30 0 2 -29 27.60 3.80 0 2 -29 25.00 4.10 5 0 -30 0.00 0.60 5 0 -30 -0.80 0.90 5 0 -30 -1.90 0.80 -5 0 30 -1.30 1.00 4 0 -30 65.19 3.40 4 0 -30 58.19 4.70 4 0 -30 63.09 4.90 3 0 -30 -0.80 0.40 3 0 -30 -1.60 0.80 3 0 -30 0.10 1.00 3 0 -30 0.80 0.70 2 0 -30 -0.40 1.20 2 0 -30 -0.60 0.50 2 0 -30 1.40 1.10 1 0 -30 0.00 0.50 1 0 -30 -0.60 1.10 1 0 -30 0.50 0.60 1 0 -30 0.70 1.20 1 0 -30 3.70 1.40 0 0 -30 157.18 8.90 0 0 -30 154.68 8.40 0 0 -30 187.48 12.10 0 0 -30 149.09 6.70 0 0 -30 148.89 6.70 5 -1 -30 6.80 1.30 5 -1 -30 7.10 1.90 5 -1 -30 4.70 1.50 -5 1 30 4.50 1.60 5 1 -30 7.30 1.90 5 1 -30 5.10 1.70 5 1 -30 6.60 0.90 4 -1 -30 16.10 2.70 4 -1 -30 12.50 1.60 4 -1 -30 7.90 1.70 4 1 -30 9.70 0.80 4 1 -30 9.00 2.20 4 1 -30 15.50 2.80 4 1 -30 9.70 0.90 3 -1 -30 0.70 1.20 3 -1 -30 2.50 0.90 3 -1 -30 2.40 1.20 3 -1 -30 0.80 1.00 3 1 -30 1.90 1.40 3 1 -30 2.10 1.50 2 -1 -30 61.09 3.60 2 -1 -30 56.69 4.60 2 -1 -30 65.99 4.10 2 -1 -30 61.19 4.60 2 1 -30 69.89 5.00 2 1 -30 65.89 5.30 2 1 -30 63.79 4.70 1 -1 -30 1.90 1.00 1 -1 -30 1.00 1.10 1 -1 -30 0.30 1.30 1 -1 -30 5.50 2.30 1 1 -30 0.70 1.10 1 1 -30 3.90 1.90 1 1 -30 0.20 1.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35910 data_7b _publcif_datablock.id '{4675ca5d-215d-4631-9d16-5485990eef55}' _chemical_name_systematic ? _chemical_name_common 'Novak Z' _chemical_formula_moiety 'C13 H15 F3 I O3 S, C F3 O3 S' _chemical_formula_sum 'C14 H15 F6 I O6 S2' _chemical_formula_iupac ? _chemical_formula_weight 584.28 _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 11.491(3) _cell_length_b 8.9223(19) _cell_length_c 21.300(4) _cell_angle_alpha 90 _cell_angle_beta 95.394(7) _cell_angle_gamma 90 _cell_volume 2174.1(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 647 _cell_measurement_theta_min 2.4630 _cell_measurement_theta_max 25.5767 _cell_measurement_temperature 298.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.673 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.122 _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.82 _exptl_special_details ; ; _diffrn_ambient_temperature 298.(2) _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'INCOATEC I\mS 3.0' _diffrn_radiation_type ' Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 18582 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _refine_special_details ; ; _reflns_number_total 3963 _reflns_number_gt 3332 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_gt 0.1510 _refine_ls_wR_factor_ref 0.1594 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_number_reflns 3963 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+4.5274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.900 _refine_diff_density_min -0.627 _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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 'Bruker Instrument Service vV6.2.6' _computing_cell_refinement 'APEX3 v2017.3-0 (Bruker AXS)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics Mercury _computing_publication_material 'WinGX, PublCIF' 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 C C1 0.3736(6) 0.2991(6) 0.3362(3) 0.0697(14) Uani d . . . 1 . . C C2 0.2828(5) 0.3805(6) 0.3452(3) 0.0707(14) Uani d . . . 1 . . C C3 0.2359(6) 0.4454(7) 0.4013(3) 0.0814(17) Uani d . . . 1 . . H H3A 0.224324 0.55209 0.394621 0.098 Uiso calc U . R 1 . . H H3B 0.293445 0.432843 0.437275 0.098 Uiso calc U . R 1 . . C C4 0.1226(7) 0.3767(11) 0.4166(5) 0.118(3) Uani d . . . 1 . . H H4A 0.084316 0.443155 0.44354 0.177 Uiso calc U . R 1 . . H H4B 0.137909 0.282742 0.437701 0.177 Uiso calc U . R 1 . . H H4C 0.073173 0.360467 0.37831 0.177 Uiso calc U . R 1 . . C C10 0.0738(17) 0.6207(19) 0.2426(10) 0.191(7) Uani d . . . 1 . . C C11 0.5986(5) 0.4309(6) 0.4065(2) 0.0673(13) Uani d . . . 1 . . C C12 0.7132(7) 0.3999(10) 0.3979(4) 0.104(2) Uani d . . . 1 . . H H12 0.740311 0.302209 0.39504 0.124 Uiso calc U . R 1 . . C C13 0.7859(8) 0.5227(15) 0.3937(5) 0.136(4) Uani d . . . 1 . . H H13 0.863911 0.507374 0.387145 0.164 Uiso calc U . R 1 . . C C14 0.7456(10) 0.6660(12) 0.3991(4) 0.119(3) Uani d . . . 1 . . H H14 0.796551 0.746516 0.397086 0.142 Uiso calc U . R 1 . . C C15 0.6330(9) 0.6906(9) 0.4071(4) 0.103(2) Uani d . . . 1 . . H H15 0.605898 0.788562 0.409227 0.124 Uiso calc U . R 1 . . C C16 0.5572(7) 0.5743(7) 0.4122(3) 0.0835(17) Uani d . . . 1 . . H H16 0.47978 0.591573 0.419402 0.1 Uiso calc U . R 1 . . C C20 0.1434(10) 0.8936(13) 0.4613(10) 0.171(6) Uani d . . . 1 . . C C21 0.4132(9) 0.2326(7) 0.2765(3) 0.091(2) Uani d . . . 1 . . H H21A 0.369496 0.278887 0.240397 0.11 Uiso calc U . R 1 . . H H21B 0.4952 0.255923 0.274399 0.11 Uiso calc U . R 1 . . C C22 0.3971(11) 0.0657(9) 0.2725(4) 0.133(4) Uani d . . . 1 . . H H22A 0.418073 0.030605 0.232477 0.2 Uiso calc U . R 1 . . H H22B 0.316786 0.041363 0.276709 0.2 Uiso calc U . R 1 . . H H22C 0.446022 0.018392 0.305766 0.2 Uiso calc U . R 1 . . O O11 0.2060(5) 0.4048(5) 0.2878(2) 0.0946(14) Uani d . . . 1 . . O O12 0.2370(14) 0.5000(11) 0.1835(4) 0.262(7) Uani d . . . 1 . . O O13 0.3003(7) 0.6515(9) 0.2790(4) 0.161(3) Uani d . . . 1 . . O O21 0.3476(5) 0.7759(6) 0.4702(3) 0.1021(16) Uani d . . . 1 . . O O22 0.3076(17) 0.9853(12) 0.5259(5) 0.330(10) Uani d . . . 1 . . O O23 0.3143(7) 1.0201(12) 0.4202(5) 0.204(5) Uani d . . . 1 . . F F11 0.0125(13) 0.515(2) 0.2103(9) 0.371(11) Uani d . . . 1 . . F F12 0.0502(11) 0.6460(15) 0.2967(7) 0.262(7) Uani d . . . 1 . . F F13 0.0798(11) 0.7408(11) 0.2060(6) 0.278(7) Uani d . . . 1 . . F F21 0.1156(9) 0.7997(19) 0.4973(10) 0.392(14) Uani d . . . 1 . . F F22 0.0813(6) 0.9990(10) 0.4501(6) 0.240(5) Uani d . . . 1 . . F F23 0.1177(13) 0.8131(18) 0.4089(11) 0.403(16) Uani d . . . 1 . . S S1 0.2256(3) 0.5473(3) 0.24522(11) 0.1233(9) Uani d . . . 1 . . S S2 0.29646(16) 0.91645(19) 0.46272(10) 0.0900(5) Uani d . . . 1 . . I I1 0.48644(3) 0.24875(4) 0.41772(2) 0.06873(19) Uani 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 C1 0.093(4) 0.056(3) 0.059(3) 0.007(3) -0.002(3) 0.002(2) C2 0.081(4) 0.054(3) 0.073(3) 0.004(3) -0.014(3) -0.004(2) C3 0.075(4) 0.074(4) 0.093(4) 0.020(3) -0.007(3) -0.014(3) C4 0.099(6) 0.123(7) 0.135(7) -0.003(5) 0.027(5) -0.011(6) C10 0.205(16) 0.141(11) 0.213(16) 0.041(11) -0.062(14) 0.078(12) C11 0.072(3) 0.071(3) 0.058(3) 0.004(3) 0.002(2) 0.008(2) C12 0.083(5) 0.107(6) 0.122(6) 0.015(4) 0.017(4) 0.025(5) C13 0.077(5) 0.174(10) 0.158(9) -0.017(6) 0.008(5) 0.058(8) C14 0.126(8) 0.109(7) 0.119(7) -0.036(6) 0.001(5) 0.019(5) C15 0.141(8) 0.077(4) 0.091(5) -0.013(5) 0.011(5) -0.005(4) C16 0.110(5) 0.067(4) 0.075(4) -0.002(3) 0.017(3) -0.007(3) C20 0.107(7) 0.106(7) 0.308(19) 0.024(6) 0.056(10) 0.091(10) C21 0.140(7) 0.073(4) 0.062(4) 0.016(4) 0.012(4) 0.000(3) C22 0.233(12) 0.077(5) 0.093(5) 0.005(6) 0.034(6) -0.023(4) O11 0.118(4) 0.069(2) 0.088(3) 0.010(2) -0.037(3) 0.005(2) O12 0.50(2) 0.186(8) 0.097(5) 0.173(11) 0.032(8) 0.040(5) O13 0.173(7) 0.123(5) 0.178(7) -0.053(5) -0.032(5) 0.044(5) O21 0.091(3) 0.090(3) 0.123(4) 0.025(3) -0.001(3) -0.006(3) O22 0.63(3) 0.174(9) 0.149(8) 0.129(13) -0.156(12) -0.091(7) O23 0.128(6) 0.223(9) 0.267(11) 0.014(6) 0.049(6) 0.159(8) F11 0.290(15) 0.41(2) 0.368(19) -0.127(15) -0.211(15) 0.150(15) F12 0.245(11) 0.264(13) 0.292(13) 0.164(10) 0.108(11) 0.130(12) F13 0.272(12) 0.242(11) 0.317(13) 0.116(9) 0.005(10) 0.176(10) F21 0.131(7) 0.367(17) 0.70(3) 0.084(9) 0.177(13) 0.35(2) F22 0.127(5) 0.191(7) 0.415(14) 0.094(5) 0.096(7) 0.133(8) F23 0.264(14) 0.210(11) 0.67(4) 0.053(11) -0.28(2) -0.114(19) S1 0.166(2) 0.1050(15) 0.0965(15) 0.0470(16) 0.0006(14) 0.0299(12) S2 0.0840(10) 0.0672(9) 0.1170(14) 0.0023(8) -0.0006(9) 0.0261(9) I1 0.0774(3) 0.0639(3) 0.0640(3) 0.00983(15) 0.00170(19) 0.01087(14) _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 C1 C2 . 1.300(8) ? C1 C21 . 1.512(9) ? C1 I1 . 2.116(6) ? C2 O11 . 1.455(7) ? C2 C3 . 1.475(9) ? C3 C4 . 1.502(11) ? C10 F12 . 1.23(2) ? C10 F13 . 1.331(17) ? C10 F11 . 1.33(2) ? C10 S1 . 1.859(18) ? C11 C12 . 1.374(9) ? C11 C16 . 1.374(8) ? C11 I1 . 2.102(6) ? C12 C13 . 1.386(13) ? C13 C14 . 1.368(15) ? C14 C15 . 1.340(13) ? C15 C16 . 1.366(10) ? C20 F22 . 1.191(11) ? C20 F21 . 1.199(13) ? C20 F23 . 1.34(2) ? C20 S2 . 1.768(11) ? C21 C22 . 1.502(10) ? O11 S1 . 1.589(5) ? O12 S1 . 1.399(8) ? O13 S1 . 1.416(8) ? O21 S2 . 1.387(5) ? O22 S2 . 1.473(8) ? O23 S2 . 1.323(7) ? 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 C2 C1 C21 . . 130.7(6) ? C2 C1 I1 . . 115.9(4) ? C21 C1 I1 . . 113.4(5) ? C1 C2 O11 . . 113.0(5) ? C1 C2 C3 . . 134.2(5) ? O11 C2 C3 . . 112.6(5) ? C2 C3 C4 . . 113.9(6) ? F12 C10 F13 . . 115.5(18) ? F12 C10 F11 . . 118.(2) ? F13 C10 F11 . . 108.7(16) ? F12 C10 S1 . . 109.0(11) ? F13 C10 S1 . . 101.6(14) ? F11 C10 S1 . . 102.5(15) ? C12 C11 C16 . . 122.9(7) ? C12 C11 I1 . . 117.7(5) ? C16 C11 I1 . . 119.3(5) ? C11 C12 C13 . . 116.2(8) ? C14 C13 C12 . . 121.5(9) ? C15 C14 C13 . . 120.2(9) ? C14 C15 C16 . . 121.1(8) ? C15 C16 C11 . . 118.2(7) ? F22 C20 F21 . . 119.3(12) ? F22 C20 F23 . . 100.1(17) ? F21 C20 F23 . . 96.2(17) ? F22 C20 S2 . . 119.3(9) ? F21 C20 S2 . . 113.2(11) ? F23 C20 S2 . . 102.6(12) ? C22 C21 C1 . . 113.0(6) ? C2 O11 S1 . . 119.4(4) ? O12 S1 O13 . . 124.7(8) ? O12 S1 O11 . . 109.0(5) ? O13 S1 O11 . . 110.3(4) ? O12 S1 C10 . . 104.4(9) ? O13 S1 C10 . . 107.8(8) ? O11 S1 C10 . . 96.7(6) ? O23 S2 O21 . . 128.3(6) ? O23 S2 O22 . . 109.1(8) ? O21 S2 O22 . . 105.8(5) ? O23 S2 C20 . . 106.6(6) ? O21 S2 C20 . . 107.9(4) ? O22 S2 C20 . . 93.7(11) ? C11 I1 C1 . . 94.4(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 C3 H3B I1 . 0.97 2.82 3.361(6) 115.9 ? C16 H16 O21 . 0.93 2.55 3.336(9) 142.7 ? C21 H21A S1 . 0.97 2.92 3.564(8) 125.1 ? _shelx_res_file ; TITL mo_18123_0m_a.res in P2(1)/c mo_18123_0m.res created by SHELXL-2016/6 at 20:13:06 on 18-Oct-2018 CELL 0.71073 11.4909 8.9223 21.2996 90.000 95.394 90.000 ZERR 4.00 0.0025 0.0019 0.0042 0.000 0.007 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H O F S I UNIT 56 60 24 24 8 4 ACTA LIST 4 TEMP 25 SIZE 0.122 0.211 0.673 L.S. 14 FMAP 2 PLAN 5 HTAB HTAB C3 I1 HTAB C16 O21 HTAB C21 S1 WGHT 0.086200 4.527400 FVAR 0.30552 C1 1 0.373568 0.299085 0.336194 11.00000 0.09273 0.05585 = 0.05883 0.00221 -0.00175 0.00733 C2 1 0.282780 0.380513 0.345152 11.00000 0.08113 0.05421 = 0.07256 -0.00380 -0.01443 0.00372 C3 1 0.235944 0.445387 0.401305 11.00000 0.07464 0.07382 = 0.09293 -0.01376 -0.00702 0.02010 AFIX 23 H3A 2 0.224324 0.552090 0.394621 11.00000 -1.20000 H3B 2 0.293445 0.432843 0.437275 11.00000 -1.20000 AFIX 0 C4 1 0.122607 0.376743 0.416594 11.00000 0.09938 0.12336 = 0.13452 -0.01078 0.02719 -0.00322 AFIX 137 H4A 2 0.084316 0.443155 0.443540 11.00000 -1.50000 H4B 2 0.137909 0.282742 0.437701 11.00000 -1.50000 H4C 2 0.073173 0.360467 0.378310 11.00000 -1.50000 AFIX 0 C10 1 0.073819 0.620699 0.242564 11.00000 0.20508 0.14099 = 0.21274 0.07762 -0.06184 0.04064 C11 1 0.598594 0.430913 0.406473 11.00000 0.07210 0.07127 = 0.05770 0.00821 0.00164 0.00351 C12 1 0.713158 0.399936 0.397888 11.00000 0.08335 0.10731 = 0.12166 0.02528 0.01694 0.01461 AFIX 43 H12 2 0.740311 0.302209 0.395040 11.00000 -1.20000 AFIX 0 C13 1 0.785930 0.522734 0.393717 11.00000 0.07661 0.17396 = 0.15810 0.05843 0.00801 -0.01685 AFIX 43 H13 2 0.863911 0.507374 0.387145 11.00000 -1.20000 AFIX 0 C14 1 0.745623 0.666000 0.399050 11.00000 0.12557 0.10875 = 0.11941 0.01925 0.00113 -0.03643 AFIX 43 H14 2 0.796551 0.746516 0.397086 11.00000 -1.20000 AFIX 0 C15 1 0.632962 0.690631 0.407097 11.00000 0.14124 0.07691 = 0.09088 -0.00538 0.01083 -0.01267 AFIX 43 H15 2 0.605898 0.788562 0.409227 11.00000 -1.20000 AFIX 0 C16 1 0.557230 0.574261 0.412220 11.00000 0.10980 0.06748 = 0.07469 -0.00749 0.01692 -0.00205 AFIX 43 H16 2 0.479780 0.591573 0.419402 11.00000 -1.20000 AFIX 0 C20 1 0.143396 0.893579 0.461315 11.00000 0.10711 0.10555 = 0.30843 0.09125 0.05635 0.02425 C21 1 0.413201 0.232617 0.276485 11.00000 0.13987 0.07280 = 0.06194 0.00046 0.01161 0.01554 AFIX 23 H21A 2 0.369496 0.278887 0.240397 11.00000 -1.20000 H21B 2 0.495200 0.255923 0.274399 11.00000 -1.20000 AFIX 0 C22 1 0.397064 0.065677 0.272499 11.00000 0.23327 0.07743 = 0.09254 -0.02298 0.03427 0.00494 AFIX 137 H22A 2 0.418073 0.030605 0.232477 11.00000 -1.50000 H22B 2 0.316786 0.041363 0.276709 11.00000 -1.50000 H22C 2 0.446022 0.018392 0.305766 11.00000 -1.50000 AFIX 0 O11 3 0.206020 0.404802 0.287769 11.00000 0.11815 0.06874 = 0.08816 0.00470 -0.03697 0.01017 O12 3 0.236991 0.500048 0.183481 11.00000 0.50464 0.18593 = 0.09736 0.03964 0.03180 0.17291 O13 3 0.300348 0.651542 0.279031 11.00000 0.17322 0.12326 = 0.17771 0.04399 -0.03249 -0.05325 O21 3 0.347578 0.775930 0.470233 11.00000 0.09108 0.08995 = 0.12315 -0.00629 -0.00060 0.02490 O22 3 0.307556 0.985278 0.525878 11.00000 0.62992 0.17360 = 0.14942 -0.09058 -0.15574 0.12855 O23 3 0.314262 1.020071 0.420208 11.00000 0.12813 0.22254 = 0.26655 0.15945 0.04871 0.01412 F11 4 0.012462 0.515278 0.210256 11.00000 0.29001 0.41003 = 0.36761 0.15029 -0.21129 -0.12690 F12 4 0.050192 0.645997 0.296735 11.00000 0.24494 0.26398 = 0.29240 0.13014 0.10805 0.16393 F13 4 0.079818 0.740776 0.205953 11.00000 0.27163 0.24217 = 0.31691 0.17638 0.00522 0.11566 F21 4 0.115598 0.799664 0.497296 11.00000 0.13090 0.36745 = 0.70299 0.35223 0.17671 0.08374 F22 4 0.081283 0.999002 0.450126 11.00000 0.12651 0.19120 = 0.41472 0.13313 0.09583 0.09434 F23 4 0.117662 0.813051 0.408855 11.00000 0.26448 0.20983 = 0.67202 -0.11421 -0.28372 0.05280 S1 5 0.225568 0.547262 0.245217 11.00000 0.16640 0.10497 = 0.09645 0.02985 0.00060 0.04701 S2 5 0.296465 0.916447 0.462719 11.00000 0.08398 0.06717 = 0.11700 0.02614 -0.00063 0.00227 I1 6 0.486439 0.248754 0.417718 11.00000 0.07740 0.06389 = 0.06398 0.01087 0.00170 0.00983 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_18123_0m_a.res in P2(1)/c REM R1 = 0.0525 for 3332 Fo > 4sig(Fo) and 0.0607 for all 3963 data REM 264 parameters refined using 0 restraints END WGHT 0.0774 4.4449 REM Instructions for potential hydrogen bonds HTAB C3 I1 HTAB C16 O21 HTAB C21 S1 REM Highest difference peak 0.900, deepest hole -0.627, 1-sigma level 0.089 Q1 1 0.1578 0.5848 0.2816 11.00000 0.05 0.90 Q2 1 0.2752 0.8487 0.3793 11.00000 0.05 0.86 Q3 1 0.4204 0.2835 0.4265 11.00000 0.05 0.80 Q4 1 0.1586 0.9138 0.5336 11.00000 0.05 0.75 Q5 1 0.2834 0.8817 0.4240 11.00000 0.05 0.72 ; _shelx_res_checksum 19052 _shelx_hkl_file ; -2 0 0 19.3162 3.94593 1 -2 0 0 21.0879 0.80589 2 3 0 0 738.354 20.6266 2 3 0 0 738.264 42.8567 1 -3 0 0 625.108 20.6420 2 -3 0 0 735.514 43.4674 1 -4 0 0 1356.76 70.2115 1 4 0 0 1115.12 64.0834 1 -5 0 0 2261.46 107.013 1 5 0 0 1986.58 100.308 1 -6 0 0 234.836 7.66762 2 6 0 0 246.932 7.51586 2 -6 0 0 262.393 34.1790 1 6 0 0 247.850 30.5332 1 -7 0 0 413.995 42.6977 1 -7 0 0 330.136 11.3689 2 7 0 0 418.291 43.9689 1 7 0 0 352.470 10.6921 4 8 0 0 212.759 6.51035 4 -8 0 0 214.414 6.99989 2 9 0 0 103.328 3.46008 4 -9 0 0 107.889 3.96788 2 10 0 0 135.531 4.43162 4 -10 0 0 137.594 4.94954 2 -11 0 0 36.1350 2.08284 2 11 0 0 36.0583 1.66139 4 -12 0 0 2.98512 0.82896 2 12 0 0 2.13257 0.67986 4 -13 0 0 1.83137 0.86668 2 13 0 0 2.92588 0.79318 4 0 -1 0 0.04041 0.04404 4 0 -1 0 1.80096 1.38316 1 0 -1 0 0.02397 0.03522 2 0 1 0 -1.7609 2.16797 1 0 1 0 0.03416 0.03378 3 -1 -1 0 172.334 5.18159 3 1 -1 0 183.413 15.0769 1 -1 -1 0 189.324 19.7943 1 1 -1 0 175.388 5.13445 3 -1 1 0 179.764 5.16357 4 -1 1 0 138.371 13.8442 1 1 1 0 177.711 5.18036 2 1 1 0 162.780 21.3800 1 1 1 0 180.711 5.18697 4 -2 -1 0 1500.85 61.9700 1 2 -1 0 1473.97 62.7522 1 -2 1 0 1482.66 64.7225 1 2 1 0 1449.17 62.6370 1 -3 -1 0 36.1627 8.58981 1 -3 -1 0 35.8324 1.32667 3 3 -1 0 36.8716 1.32494 2 3 -1 0 40.3948 1.27253 4 3 1 0 37.5989 1.30076 2 3 1 0 36.3131 8.16511 1 -3 1 0 35.4298 1.20861 4 -3 1 0 44.7584 12.1999 1 4 -1 0 1948.53 101.604 1 -4 -1 0 1936.07 87.4467 1 4 1 0 1945.99 93.1682 1 -4 1 0 1973.55 120.921 1 5 -1 0 235.500 7.60155 2 5 -1 0 284.458 29.1089 1 -5 -1 0 230.946 26.7186 1 -5 -1 0 238.185 7.51656 3 5 -1 0 245.590 7.39312 4 -5 -1 0 254.329 7.55599 2 -5 1 0 225.601 7.60551 2 -5 1 0 236.368 31.9570 1 5 1 0 262.050 7.80874 2 5 1 0 295.962 30.6528 1 -6 -1 0 35.0230 11.0827 1 6 -1 0 25.6440 1.28231 2 6 -1 0 29.9038 11.7453 1 -6 -1 0 27.3669 1.24473 3 -6 -1 0 26.3231 1.30436 2 6 -1 0 28.6974 1.13538 4 -6 1 0 26.6094 1.34901 2 6 1 0 30.7257 1.27927 2 -6 1 0 49.3553 17.1133 1 6 1 0 40.7745 14.1095 1 7 -1 0 131.799 3.92864 4 7 -1 0 90.7263 22.6886 1 -7 -1 0 122.724 4.41571 3 -7 -1 0 103.653 4.36590 2 -7 -1 0 131.748 23.2580 1 -7 1 0 126.422 4.27176 2 -7 1 0 169.806 29.1384 1 7 1 0 135.557 25.2699 1 8 -1 0 149.347 4.63011 4 -8 -1 0 135.012 5.18197 2 -8 1 0 149.645 5.05647 2 -9 -1 0 139.763 5.22180 2 9 -1 0 147.188 4.82181 4 -9 1 0 162.983 5.33328 2 -10 -1 0 73.0014 3.16355 2 10 -1 0 71.4028 2.75399 4 -10 1 0 80.7943 3.21855 2 11 -1 0 39.9108 1.87434 4 -11 -1 0 41.2995 2.26217 2 -11 1 0 44.1104 2.30556 2 11 1 0 42.6381 1.77995 4 12 -1 0 25.5390 1.50445 4 -12 -1 0 27.4873 1.86669 2 -12 1 0 26.8224 1.83981 2 12 1 0 27.4022 1.42452 4 -13 -1 0 17.4638 1.73400 2 13 -1 0 17.0596 1.36245 4 13 1 0 18.9664 1.33889 4 -13 1 0 21.0907 1.74637 2 0 -2 0 311.561 27.9484 1 0 -2 0 320.799 9.75589 4 0 -2 0 327.990 9.76134 2 0 -2 0 347.048 9.78487 2 0 -2 0 328.470 9.71734 3 0 2 0 328.891 9.76164 2 0 2 0 310.272 27.0371 1 0 2 0 340.409 9.72876 3 -1 -2 0 3236.67 127.783 1 1 -2 0 3184.41 126.341 1 -1 2 0 3207.03 127.467 1 1 2 0 3508.18 129.599 1 2 -2 0 5874.20 206.777 1 -2 -2 0 6274.44 214.241 1 -2 2 0 5588.83 207.679 1 3 -2 0 1915.25 86.6647 1 -3 -2 0 1806.61 83.3412 1 -3 2 0 1744.96 88.3873 1 -4 -2 0 114.265 17.7151 1 -4 -2 0 112.104 3.69117 2 4 -2 0 114.831 3.72549 4 4 -2 0 149.997 18.2100 1 4 -2 0 118.917 3.75856 2 -4 -2 0 117.324 3.82234 3 4 2 0 115.019 3.77158 2 -4 2 0 161.592 22.3091 1 -4 2 0 116.571 3.63087 4 4 2 0 101.787 17.8979 1 -4 2 0 122.830 3.84734 2 -4 2 0 115.027 3.77870 3 5 -2 0 1371.09 39.3804 4 -5 -2 0 1327.05 39.5206 3 5 -2 0 1335.53 76.2605 1 -5 -2 0 1153.86 70.8660 1 -5 2 0 1397.12 39.2627 4 -5 2 0 1423.51 86.0072 1 -5 2 0 1380.16 39.3377 3 5 2 0 1308.23 79.8886 1 5 2 0 1421.53 39.4855 2 -6 -2 0 710.677 51.6544 1 6 -2 0 585.622 17.8220 4 -6 -2 0 586.483 18.1641 3 -6 -2 0 608.605 17.8724 2 6 -2 0 644.241 51.7123 1 6 -2 0 569.848 17.9575 2 -6 2 0 628.560 58.2889 1 -6 2 0 577.377 18.4087 2 6 2 0 604.193 55.4172 1 7 -2 0 375.021 42.2136 1 7 -2 0 409.028 12.1161 4 -7 -2 0 497.660 44.4522 1 -7 -2 0 409.386 12.2970 2 7 2 0 356.017 48.4252 1 -7 2 0 434.529 51.7060 1 -7 2 0 372.187 12.3881 2 8 -2 0 328.900 9.72692 4 -8 -2 0 324.936 9.93814 2 -8 2 0 299.130 10.1045 2 9 -2 0 97.5036 3.63992 4 -9 -2 0 96.0121 3.69244 2 -9 2 0 95.9190 3.78347 2 -10 -2 0 24.8478 1.72654 2 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619.329 18.6284 3 2 3 0 640.338 18.6743 2 2 3 0 689.863 52.6969 1 -2 3 0 631.783 54.2311 1 -2 3 0 626.844 18.6002 4 2 3 0 643.975 18.6737 4 -3 -3 0 0.87588 9.25854 1 3 -3 0 1.00611 0.23974 3 3 -3 0 -5.6803 6.47192 1 3 -3 0 0.94560 0.35736 4 3 -3 0 1.03296 0.27281 2 -3 -3 0 0.54374 0.28369 3 -3 -3 0 10.2057 6.45523 1 -3 -3 0 1.25941 0.34317 2 -3 3 0 4.09656 7.48311 1 -3 3 0 1.01479 0.27764 3 3 3 0 1.38053 0.35136 2 -3 3 0 1.13302 0.31278 2 3 3 0 0.72354 0.35376 4 -3 3 0 0.83151 0.30196 4 3 3 0 0.68677 0.30476 3 4 -3 0 38.6013 14.2968 1 -4 -3 0 51.7814 20.7596 1 -4 -3 0 45.0118 1.79192 3 -4 -3 0 45.1216 1.69312 2 4 -3 0 43.1377 1.73239 4 -4 3 0 63.3755 13.0460 1 -4 3 0 43.4072 1.61439 3 -4 3 0 45.8851 1.63864 4 -4 3 0 43.9149 1.77901 2 4 3 0 42.6557 1.75450 2 4 3 0 48.0410 1.79180 4 4 3 0 45.4104 1.76406 3 -5 -3 0 261.408 38.6331 1 -5 -3 0 255.677 29.4404 1 5 -3 0 240.984 7.58947 4 -5 -3 0 247.269 7.52644 2 5 -3 0 257.142 7.60933 2 5 -3 0 228.939 30.7019 1 5 3 0 251.015 7.66168 4 -5 3 0 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9.09300 1.60188 2 0 -6 0 1231.82 36.7677 2 0 -6 0 1310.81 100.910 1 0 -6 0 1221.04 36.8924 4 0 6 0 1226.19 95.7529 1 0 6 0 1257.18 36.6504 3 -1 -6 0 706.688 72.9850 1 -1 -6 0 773.394 23.1388 2 1 -6 0 733.879 73.6957 1 1 -6 0 768.982 23.2447 2 -1 -6 0 802.574 23.2102 4 1 -6 0 782.286 23.2136 4 1 6 0 786.271 23.0703 3 -1 6 0 681.088 70.7821 1 1 6 0 858.075 74.2991 1 -1 6 0 784.060 23.0117 3 2 -6 0 324.282 10.2466 4 -2 -6 0 306.797 52.2625 1 -2 -6 0 318.887 10.1912 4 2 -6 0 336.009 10.4673 2 -2 6 0 322.963 10.0451 3 2 6 0 364.089 47.5673 1 2 6 0 320.696 10.1300 3 -3 -6 0 379.516 11.7476 2 -3 -6 0 381.992 11.8040 4 3 -6 0 379.473 11.8509 4 3 6 0 376.056 11.7630 3 -3 6 0 385.883 11.6408 3 4 -6 0 419.423 12.5620 4 4 6 0 375.625 11.9784 3 -4 6 0 380.332 11.8175 3 -4 6 0 375.424 12.1063 2 5 -6 0 262.280 8.37081 4 -5 -6 0 262.167 8.20055 2 -5 6 0 261.388 8.11259 3 -5 6 0 244.350 8.38620 2 5 6 0 258.330 8.31249 3 6 -6 0 133.329 4.84756 4 -6 -6 0 132.545 4.64510 2 -6 6 0 138.380 4.59503 3 -6 6 0 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