#------------------------------------------------------------------------------ #$Date: 2021-05-25 00:24:25 +0300 (Tue, 25 May 2021) $ #$Revision: 265466 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518738.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4518738 loop_ _publ_author_name 'Mi, Ruijie' 'Zhang, Xuepeng' 'Wang, Jinlei' 'Chen, Haohua' 'Lan, Yu' 'Wang, Fen' 'Li, Xingwei' _publ_section_title ; Rhodium-Catalyzed Regio-, Diastereo-, and Enantioselective Three-Component Carboamination of Dienes via C--H Activation ; _journal_name_full 'ACS Catalysis' _journal_page_first 6692 _journal_page_last 6697 _journal_paper_doi 10.1021/acscatal.1c01615 _journal_year 2021 _chemical_formula_moiety 'C24 H27 I N2 O2, C H2 Cl2' _chemical_formula_sum 'C25 H29 Cl2 I N2 O2' _chemical_formula_weight 587.30 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-02-02 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _cell_angle_alpha 90 _cell_angle_beta 115.579(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.666(3) _cell_length_b 10.1915(18) _cell_length_c 16.848(3) _cell_measurement_reflns_used 9898 _cell_measurement_temperature 226.0 _cell_measurement_theta_max 68.194 _cell_measurement_theta_min 2.939 _cell_volume 2581.2(8) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 226.0 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_unetI/netI 0.0491 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 25932 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.681 _diffrn_reflns_theta_min 2.939 _diffrn_source_current 50.0 _diffrn_source_power 2.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.840 _exptl_absorpt_correction_T_max 0.1665 _exptl_absorpt_correction_T_min 0.0429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1373 before and 0.0893 after correction. The Ratio of minimum to maximum transmission is 0.2577. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.511 _exptl_crystal_description block _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 2.815 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.177 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 4715 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0762 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1485P)^2^+5.7333P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2174 _refine_ls_wR_factor_ref 0.2273 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4042 _reflns_number_total 4715 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c01615_si_001.cif _cod_data_source_block s _cod_database_code 4518738 _shelx_shelxl_version_number 2018/3 _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_max 0.125 _shelx_estimated_absorpt_t_min 0.066 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C1(H1) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C22(H22A,H22B), C15(H15A,H15B), C9(H9A,H9B), C23(H23A,H23B), C3(H3A,H3B) 2.c Aromatic/amide H refined with riding coordinates: N2(H2), C8(H8), C14(H14), C20(H20), C25(H25), C13(H13), C7(H7), C2(H2A), C19(H19), C5(H5) 2.d Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C11(H11A,H11B,H11C) ; _shelx_res_file ; TITL s_a.res in P2(1)/c s.res created by SHELXL-2018/3 at 17:47:57 on 02-Feb-2021 REM Old TITL s in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.199, Rweak 0.012, Alpha 0.045 REM 0.523 for 290 systematic absences, Orientation as input REM Formula found by SHELXT: C25 N O5 I CELL 1.54178 16.6662 10.1915 16.8478 90 115.579 90 ZERR 4 0.0031 0.0018 0.003 0 0.009 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl I N O UNIT 100 116 8 4 8 8 L.S. 4 PLAN 7 SIZE 0.5 0.4 0.3 TEMP -47.15 CONF list 4 fmap 2 53 MORE -1 ACTA BOND $H OMIT 0 8 3 OMIT -2 8 1 OMIT 0 10 0 OMIT 2 0 8 OMIT -1 10 6 OMIT -3 8 7 OMIT -3 6 4 OMIT 2 10 2 OMIT 0 4 3 OMIT -3 10 4 OMIT 2 3 2 OMIT -3 8 1 OMIT 2 8 5 OMIT -7 10 6 OMIT -1 8 3 OMIT -7 8 3 OMIT 0 12 3 OMIT -14 0 6 OMIT -2 4 1 OMIT 6 8 3 OMIT -4 10 2 OMIT -5 8 5 OMIT -5 6 8 REM REM REM WGHT 0.148500 5.733300 FVAR 0.22581 I1 4 0.329955 -0.128119 0.389522 11.00000 0.07283 0.03528 = 0.07087 0.00502 0.03381 -0.00028 CL1 3 0.059217 0.560279 0.270918 11.00000 0.13975 0.10077 = 0.12658 -0.02195 0.01799 -0.00859 CL2 3 0.068587 0.820971 0.339786 11.00000 0.11832 0.08963 = 0.15161 0.01064 0.04264 0.02589 O1 6 0.519427 0.102129 0.266795 11.00000 0.07420 0.03237 = 0.06087 -0.00172 0.02578 0.00156 O3 6 0.311700 0.571019 0.358302 11.00000 0.09415 0.03735 = 0.06116 -0.00204 0.03378 0.00679 N2 5 0.507014 0.318665 0.284966 11.00000 0.06474 0.04273 = 0.04969 -0.00002 0.02665 0.00057 AFIX 43 H2 2 0.488945 0.393719 0.258666 11.00000 -1.20000 AFIX 0 N1 5 0.268561 0.502103 0.218265 11.00000 0.07180 0.03312 = 0.06170 0.00557 0.03177 0.00137 C1 1 0.545499 0.315289 0.380459 11.00000 0.06822 0.03340 = 0.05074 0.00111 0.02756 -0.00003 AFIX 13 H1 2 0.559957 0.222924 0.399466 11.00000 -1.20000 AFIX 0 C4 1 0.320835 0.076503 0.373895 11.00000 0.07605 0.03570 = 0.05803 0.00023 0.03731 0.00040 C6 1 0.497907 0.211291 0.235076 11.00000 0.05856 0.04256 = 0.05481 -0.00411 0.02574 -0.00007 C8 1 0.630034 0.394428 0.422038 11.00000 0.06610 0.03806 = 0.05065 -0.00044 0.02439 0.00079 AFIX 43 H8 2 0.651947 0.412068 0.482551 11.00000 -1.20000 AFIX 0 C10 1 0.758656 0.518360 0.422068 11.00000 0.05985 0.04066 = 0.06124 0.00294 0.02607 0.00094 C12 1 0.392084 0.285375 0.381401 11.00000 0.06396 0.04693 = 0.04903 -0.00553 0.02978 -0.00547 C14 1 0.236963 0.130605 0.328802 11.00000 0.06776 0.04350 = 0.06520 0.00057 0.03511 -0.00256 AFIX 43 H14 2 0.185457 0.079302 0.312950 11.00000 -1.20000 AFIX 0 C16 1 0.476860 0.364700 0.412548 11.00000 0.06929 0.03679 = 0.05632 -0.00543 0.03158 -0.00106 AFIX 23 H16A 2 0.505049 0.365242 0.477035 11.00000 -1.20000 H16B 2 0.461300 0.455543 0.392827 11.00000 -1.20000 AFIX 0 C18 1 0.297046 0.483562 0.304039 11.00000 0.06547 0.03680 = 0.05800 0.00041 0.02906 -0.00026 C20 1 0.676267 0.441386 0.381190 11.00000 0.06442 0.03722 = 0.05896 0.00039 0.02811 -0.00068 AFIX 43 H20 2 0.654423 0.423910 0.320662 11.00000 -1.20000 AFIX 0 C22 1 0.258580 0.403011 0.150503 11.00000 0.08001 0.04910 = 0.05981 -0.00353 0.03247 0.00055 AFIX 23 H22A 2 0.200763 0.358920 0.129102 11.00000 -1.20000 H22B 2 0.305971 0.337119 0.173320 11.00000 -1.20000 AFIX 0 C24 1 0.308728 0.339222 0.333446 11.00000 0.07324 0.02614 = 0.05665 -0.00116 0.03409 0.00166 C25 1 0.817194 0.521952 0.382766 11.00000 0.07577 0.06407 = 0.07060 -0.00232 0.03745 -0.00270 AFIX 43 H25 2 0.802446 0.476624 0.329692 11.00000 -1.20000 AFIX 0 C13 1 0.779843 0.592624 0.497890 11.00000 0.06627 0.04713 = 0.06551 0.00080 0.02911 -0.00391 AFIX 43 H13 2 0.739717 0.595655 0.523503 11.00000 -1.20000 AFIX 0 C7 1 0.398336 0.151213 0.401791 11.00000 0.06686 0.04337 = 0.05087 0.00097 0.02874 0.00406 AFIX 43 H7 2 0.454189 0.112067 0.433928 11.00000 -1.20000 AFIX 0 C15 1 0.222255 0.612454 0.083174 11.00000 0.08270 0.04914 = 0.06985 0.00813 0.02821 0.00420 AFIX 23 H15A 2 0.242529 0.683260 0.056881 11.00000 -1.20000 H15B 2 0.157325 0.605949 0.052035 11.00000 -1.20000 AFIX 0 C2 1 0.231358 0.263854 0.307629 11.00000 0.06806 0.03445 = 0.06511 0.00371 0.03154 0.00514 AFIX 43 H2A 2 0.175423 0.303012 0.275933 11.00000 -1.20000 AFIX 0 C17 1 0.460480 0.234665 0.137008 11.00000 0.07425 0.05715 = 0.05423 -0.00391 0.03205 0.00023 AFIX 137 H17A 2 0.503703 0.207606 0.115978 11.00000 -1.50000 H17B 2 0.447434 0.327235 0.124836 11.00000 -1.50000 H17C 2 0.406291 0.184149 0.107290 11.00000 -1.50000 AFIX 0 C9 1 0.251507 0.636384 0.180033 11.00000 0.06896 0.04133 = 0.06554 0.00720 0.02738 0.00179 AFIX 23 H9A 2 0.305604 0.689969 0.204833 11.00000 -1.20000 H9B 2 0.204690 0.680265 0.190596 11.00000 -1.20000 AFIX 0 C19 1 0.860159 0.663244 0.536937 11.00000 0.06869 0.05613 = 0.06941 -0.00252 0.02506 -0.00580 AFIX 43 H19 2 0.874833 0.709396 0.589703 11.00000 -1.20000 AFIX 0 C5 1 0.895511 0.589961 0.419782 11.00000 0.06392 0.07114 = 0.08529 -0.00068 0.03479 -0.00618 AFIX 43 H5 2 0.934953 0.586960 0.393372 11.00000 -1.20000 AFIX 0 C21 1 0.917872 0.664132 0.496572 11.00000 0.06534 0.05889 = 0.08931 0.00237 0.03353 -0.00633 C11 1 1.002221 0.745303 0.535342 11.00000 0.06907 0.08128 = 0.12287 -0.01220 0.03610 -0.02193 AFIX 137 H11A 2 0.987233 0.836340 0.539103 11.00000 -1.50000 H11B 2 1.032967 0.738540 0.498021 11.00000 -1.50000 H11C 2 1.040479 0.713011 0.593728 11.00000 -1.50000 AFIX 0 C23 1 0.265640 0.483774 0.079596 11.00000 0.09651 0.06343 = 0.06716 -0.00317 0.03769 -0.00474 AFIX 23 H23A 2 0.234190 0.441803 0.021988 11.00000 -1.20000 H23B 2 0.327989 0.496916 0.091215 11.00000 -1.20000 AFIX 0 C3 1 0.116900 0.666594 0.358760 11.00000 0.08002 0.06613 = 0.11158 0.00598 0.03724 -0.00644 AFIX 23 H3A 2 0.117264 0.630156 0.412744 11.00000 -1.20000 H3B 2 0.178724 0.674112 0.367284 11.00000 -1.20000 AFIX 0 HKLF 4 REM s_a.res in P2(1)/c REM wR2 = 0.2273, GooF = S = 1.062, Restrained GooF = 1.062 for all data REM R1 = 0.0762 for 4042 Fo > 4sig(Fo) and 0.0845 for all 4715 data REM 291 parameters refined using 0 restraints END WGHT 0.1485 5.7335 REM Highest difference peak 2.815, deepest hole -0.665, 1-sigma level 0.177 Q1 1 0.3953 -0.1206 0.4165 11.00000 0.05 2.82 Q2 1 0.2642 -0.1228 0.3637 11.00000 0.05 2.46 Q3 1 0.3376 -0.0574 0.4036 11.00000 0.05 1.93 Q4 1 0.8131 0.3831 0.4577 11.00000 0.05 1.12 Q5 1 0.0388 0.6164 0.2062 11.00000 0.05 0.92 Q6 1 0.3442 -0.2028 0.4141 11.00000 0.05 0.84 Q7 1 0.2910 -0.1378 0.3055 11.00000 0.05 0.81 ; _shelx_res_checksum 8729 _shelx_hkl_file ; 1 0 0 883.31 57.69 -1 0 0 875.11 57.69 2 0 0 981.40 66.39 3 0 0 1908.71 126.89 -4 0 0 504.85 39.60 4 0 0 494.05 40.30 -5 0 0 2686.63 177.68 5 0 0 2663.43 177.68 6 0 0 644.54 53.09 -6 0 0 708.33 53.59 -7 0 0 910.61 69.49 8 0 0 95.09 20.20 -8 0 0 117.89 19.40 9 0 0 280.17 33.00 -9 0 0 260.67 32.40 10 0 0 12.70 1.50 -10 0 0 10.10 1.50 11 0 0 182.98 12.30 -11 0 0 194.18 12.20 12 0 0 181.88 12.30 -12 0 0 196.18 12.30 13 0 0 13.80 1.70 -13 0 0 14.40 1.60 -14 0 0 51.09 3.60 14 0 0 49.90 3.70 -15 0 0 54.59 3.80 15 0 0 55.69 3.90 16 0 0 1.90 0.70 -16 0 0 2.30 0.60 17 0 0 9.50 0.90 17 0 0 8.50 0.80 17 0 0 10.70 0.90 -17 0 0 10.80 0.90 17 0 0 11.50 1.10 18 0 0 14.50 1.10 18 0 0 11.70 0.90 -18 0 0 13.00 0.90 0 -1 0 -0.80 1.90 0 1 0 0.40 1.30 -1 -1 0 415.86 28.80 1 -1 0 400.16 28.10 1 1 0 407.86 28.50 -2 -1 0 319.77 22.80 -2 -1 0 320.87 24.50 2 -1 0 290.47 22.70 -2 1 0 295.67 23.30 -3 -1 0 137.59 13.50 3 -1 0 123.59 13.40 -3 -1 0 142.89 16.80 -3 1 0 141.79 14.80 4 -1 0 1879.51 126.29 -4 -1 0 1930.91 126.79 -4 1 0 1884.91 127.99 -5 -1 0 158.68 19.10 5 -1 0 186.68 20.40 -5 1 0 145.59 19.30 -6 -1 0 13.20 7.50 6 -1 0 3.70 5.90 -6 1 0 8.40 10.60 -6 1 0 -0.70 6.00 -7 -1 0 769.02 61.69 7 -1 0 797.22 63.29 -7 1 0 848.82 58.79 -7 1 0 830.02 65.69 -8 -1 0 144.59 27.90 8 -1 0 199.18 24.20 -9 -1 0 -19.60 11.90 -9 -1 0 14.20 16.10 -9 -1 0 7.60 1.50 -9 1 0 11.30 15.90 10 -1 0 57.39 4.30 -10 -1 0 67.09 4.40 10 1 0 59.99 4.40 -10 1 0 58.79 4.30 -11 -1 0 97.89 6.30 -11 1 0 92.99 6.20 11 1 0 85.09 6.30 -12 -1 0 0.00 0.90 12 -1 0 0.70 0.90 12 1 0 0.50 0.90 -12 1 0 0.30 0.80 -13 -1 0 19.40 1.90 13 -1 0 18.60 2.00 -13 1 0 21.00 1.90 13 1 0 19.80 2.00 14 -1 0 34.50 2.70 -14 -1 0 32.50 2.50 -14 1 0 32.30 2.50 14 1 0 31.10 2.60 14 1 0 23.80 10.30 15 -1 0 5.10 1.30 -15 -1 0 3.00 0.80 15 1 0 3.60 0.90 -15 1 0 3.70 0.80 -16 -1 0 11.90 1.20 16 -1 0 12.30 1.30 16 1 0 12.60 1.30 -16 1 0 11.10 1.10 17 -1 0 1.10 0.50 17 -1 0 0.60 0.40 -17 -1 0 0.90 0.40 17 1 0 1.10 0.40 -17 1 0 1.00 0.40 17 1 0 0.60 0.60 17 1 0 0.90 0.30 18 -1 0 1.40 0.40 18 -1 0 1.20 0.30 -18 -1 0 1.00 0.20 -18 1 0 1.40 0.30 18 1 0 1.30 0.30 18 1 0 1.30 0.40 0 -2 0 10.90 4.10 0 2 0 11.30 3.70 -1 -2 0 31.00 6.60 1 -2 0 18.10 4.40 1 2 0 24.10 5.10 -1 2 0 33.70 7.30 2 -2 0 1966.00 128.69 -2 2 0 2001.00 129.59 2 2 0 1939.51 129.29 3 -2 0 262.87 22.10 -3 -2 0 273.67 24.90 -3 2 0 256.07 23.50 4 -2 0 7.10 4.90 -4 -2 0 22.70 10.80 -4 2 0 19.30 5.40 -4 2 0 17.90 6.10 -5 -2 0 31.20 8.70 5 -2 0 28.20 8.30 -5 -2 0 22.00 9.90 -5 2 0 23.30 7.20 -5 2 0 38.90 12.30 -6 -2 0 12.00 11.10 6 -2 0 1.80 6.00 -6 -2 0 6.50 6.80 -6 2 0 4.30 6.30 -6 2 0 1.40 7.90 -7 -2 0 -9.10 11.50 -7 -2 0 -7.50 6.80 7 -2 0 15.30 10.00 -7 2 0 -7.20 10.00 -7 2 0 0.20 5.80 -8 -2 0 24.90 11.60 -8 -2 0 5.30 15.60 -8 2 0 12.30 7.40 -8 2 0 3.60 14.40 -9 -2 0 3.90 1.10 -9 -2 0 -10.70 14.10 9 -2 0 4.90 1.10 -9 2 0 7.40 6.90 -9 2 0 2.50 0.90 -10 -2 0 3.90 1.10 10 -2 0 2.80 1.00 -10 2 0 2.70 0.90 10 2 0 4.10 1.20 11 -2 0 1.80 0.90 -11 -2 0 4.70 1.10 11 2 0 2.90 1.00 -11 2 0 6.00 1.10 12 -2 0 0.20 0.80 -12 -2 0 1.10 0.90 -12 2 0 0.90 0.90 12 2 0 0.60 0.90 -13 -2 0 7.00 1.10 13 -2 0 7.80 1.50 -13 2 0 5.70 1.00 13 2 0 5.70 1.10 14 -2 0 1.70 0.80 14 -2 0 -5.40 8.70 -14 -2 0 2.00 0.80 -14 2 0 2.90 0.90 14 2 0 2.90 0.90 14 2 0 7.20 9.30 -15 -2 0 0.50 0.60 15 -2 0 0.10 0.60 -15 2 0 0.00 0.60 15 2 0 0.20 0.70 -16 -2 0 -0.40 0.40 16 -2 0 0.40 0.60 -16 2 0 0.10 0.50 16 2 0 0.40 0.60 16 2 0 0.10 0.40 17 -2 0 0.20 0.50 -17 -2 0 -0.10 0.30 17 -2 0 0.00 0.40 17 2 0 0.30 0.50 -17 2 0 0.40 0.40 17 2 0 -0.10 0.40 0 -3 0 0.40 3.30 0 3 0 -2.30 3.10 1 -3 0 883.21 61.49 1 -3 0 831.22 56.09 -1 -3 0 922.21 62.59 1 3 0 864.81 61.79 -1 3 0 895.81 62.29 -2 -3 0 1124.19 77.59 2 -3 0 1180.78 76.09 2 3 0 1092.49 72.79 -2 3 0 978.70 72.09 -2 3 0 1149.98 77.59 3 -3 0 70.19 10.10 -3 -3 0 77.19 13.00 -3 3 0 73.39 12.20 -3 3 0 63.39 9.00 3 3 0 85.79 11.90 4 -3 0 744.63 51.79 -4 -3 0 714.43 50.99 -4 -3 0 721.93 55.49 -4 3 0 595.64 47.10 -4 3 0 693.33 53.79 -5 -3 0 333.97 29.50 5 -3 0 369.66 31.20 -5 -3 0 372.26 37.00 -5 3 0 325.47 33.90 -5 3 0 334.07 27.20 -6 -3 0 -1.80 9.80 6 -3 0 -6.60 5.40 -6 -3 0 -6.00 6.40 -6 3 0 -3.50 4.50 -6 3 0 18.70 10.60 -7 -3 0 350.76 43.80 7 -3 0 351.26 35.00 -7 -3 0 382.76 35.30 -7 3 0 298.07 40.70 -7 3 0 343.07 29.50 -8 -3 0 69.89 16.90 8 -3 0 67.69 5.50 -8 -3 0 34.40 22.00 -8 3 0 61.89 13.60 9 -3 0 1.20 1.00 -9 -3 0 0.50 1.00 -9 3 0 1.50 1.00 9 3 0 0.80 1.00 -9 3 0 2.70 6.40 10 -3 0 54.89 4.30 -10 -3 0 61.59 4.40 -10 3 0 62.99 4.30 -10 3 0 57.99 13.40 10 3 0 54.39 4.40 11 -3 0 29.70 2.80 -11 -3 0 38.40 2.80 -11 3 0 31.10 2.70 11 3 0 28.00 2.90 -12 -3 0 26.90 2.30 12 -3 0 23.90 2.30 -12 3 0 23.70 2.20 12 3 0 22.10 2.50 -13 -3 0 29.40 2.30 13 -3 0 26.80 2.40 13 3 0 26.30 12.10 -13 3 0 27.70 2.30 13 3 0 26.40 2.50 -14 -3 0 12.60 1.40 14 -3 0 -0.30 9.70 14 -3 0 13.30 1.60 14 3 0 11.40 1.60 14 3 0 5.50 13.80 -14 3 0 12.70 1.50 15 -3 0 2.60 0.80 -15 -3 0 2.30 0.60 -15 3 0 2.10 0.70 15 3 0 2.00 0.80 -16 -3 0 10.10 0.90 16 -3 0 10.90 1.10 16 3 0 11.00 1.20 -16 3 0 10.50 1.00 16 3 0 9.00 1.10 17 -3 0 2.50 0.40 17 -3 0 2.20 0.50 17 3 0 2.50 0.50 17 3 0 2.40 0.50 -17 3 0 2.10 0.40 0 -4 0 3709.93 240.18 0 4 0 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1.10 13 -6 0 2.20 0.60 13 -6 0 1.50 0.70 -13 -6 0 1.10 1.00 -13 6 0 2.00 0.70 13 6 0 1.20 0.80 -14 -6 0 0.10 0.60 14 -6 0 0.00 0.50 14 -6 0 0.30 0.40 -14 -6 0 0.30 0.70 -14 -6 0 -0.10 0.60 -14 6 0 0.20 0.50 14 6 0 0.40 0.70 15 -6 0 1.20 0.30 -15 -6 0 0.90 0.40 -15 -6 0 1.90 0.50 15 -6 0 1.40 0.40 -15 -6 0 0.50 0.50 15 6 0 1.10 0.50 -15 6 0 1.10 0.40 0 -7 0 0.00 0.60 0 7 0 3.20 4.30 0 7 0 0.60 0.60 -1 -7 0 158.98 11.50 1 -7 0 166.28 11.40 1 7 0 210.38 18.00 -1 7 0 190.08 11.50 1 7 0 172.28 11.50 -2 -7 0 196.58 13.60 2 -7 0 213.98 13.60 -2 7 0 221.28 13.60 2 7 0 208.78 13.60 -3 -7 0 26.00 2.20 3 -7 0 26.30 2.20 -3 7 0 19.30 5.60 -3 7 0 24.50 2.20 3 7 0 23.90 2.40 4 -7 0 49.99 3.80 -4 -7 0 48.90 3.90 -4 7 0 55.19 3.80 4 7 0 55.09 4.00 -5 -7 0 198.98 13.20 -5 -7 0 169.58 13.30 5 -7 0 206.98 13.10 -5 7 0 234.28 20.80 -5 7 0 204.88 13.10 5 7 0 211.88 13.30 -6 -7 0 6.20 1.30 6 7 0 5.70 1.40 -6 7 0 11.50 1.60 -6 7 0 4.60 5.10 -7 -7 0 63.39 4.70 -7 -7 0 49.00 4.70 7 -7 0 61.29 4.40 -7 7 0 63.69 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147.49 15.50 2 -8 0 265.77 17.50 -2 -8 0 262.37 17.60 2 8 0 286.07 24.40 -2 8 0 300.57 24.40 2 8 0 267.37 17.60 -2 8 0 268.67 17.50 3 -8 0 189.68 13.10 -3 -8 0 188.38 13.10 -3 8 0 225.78 20.20 3 8 0 199.88 13.20 -3 8 0 194.18 13.00 3 8 0 246.58 20.90 4 -8 0 2.90 0.80 -4 -8 0 3.20 1.00 4 8 0 3.30 1.20 -4 8 0 2.90 4.80 -4 8 0 3.80 1.00 -5 -8 0 11.40 1.90 5 -8 0 14.20 1.70 5 8 0 13.60 2.00 -5 8 0 13.00 1.70 -5 8 0 16.50 7.10 6 -8 0 134.49 8.80 -6 -8 0 133.39 9.00 -6 8 0 130.09 8.80 6 8 0 132.29 9.00 -6 8 0 128.99 16.50 7 -8 0 10.20 1.60 -7 -8 0 6.40 1.40 7 8 0 7.80 1.60 -7 8 0 6.80 6.20 -7 8 0 12.80 1.70 -8 -8 0 2.40 1.10 8 -8 0 1.80 0.90 -8 -8 0 2.00 2.00 8 8 0 2.70 1.20 -8 8 0 2.50 1.10 -8 8 0 2.30 5.90 -9 -8 0 90.39 6.70 9 -8 0 103.79 6.60 9 8 0 103.69 12.00 -9 8 0 84.29 6.60 9 8 0 101.99 6.80 10 -8 0 9.00 1.40 -10 -8 0 6.10 2.00 -10 -8 0 10.70 1.70 10 8 0 10.20 1.50 -10 8 0 9.40 1.30 10 8 0 11.30 6.80 -10 8 0 -2.30 5.80 -11 -8 0 9.40 1.50 11 -8 0 9.00 1.20 11 8 0 7.50 1.20 -11 8 0 9.90 1.30 -11 8 0 7.00 5.70 12 -8 0 33.80 2.60 -12 -8 0 40.20 2.80 -12 8 0 37.00 2.60 12 8 0 37.10 2.80 13 -8 0 2.90 0.50 -13 -8 0 2.60 0.60 -13 8 0 2.80 0.50 13 8 0 1.20 0.60 0 -9 0 0.30 0.70 0 9 0 1.70 4.70 0 9 0 -0.40 0.70 1 -9 0 69.79 4.80 -1 -9 0 66.99 4.80 -1 9 0 70.39 4.80 1 9 0 69.09 4.80 -1 9 0 58.59 10.70 1 9 0 59.89 10.60 2 -9 0 89.99 5.90 -2 -9 0 87.09 5.90 2 9 0 82.79 12.60 2 9 0 88.99 6.00 -2 9 0 84.09 5.90 -2 9 0 77.49 12.20 3 -9 0 8.90 1.40 -3 -9 0 6.80 1.10 -3 9 0 3.70 4.60 -3 9 0 5.40 1.00 3 9 0 7.10 5.40 3 9 0 7.00 1.30 -4 -9 0 126.59 8.30 4 -9 0 123.69 8.10 4 9 0 127.39 8.30 4 9 0 109.29 14.90 -4 9 0 118.19 15.10 -4 9 0 120.09 8.10 5 -9 0 147.59 9.40 -5 -9 0 147.99 9.60 5 9 0 145.79 9.60 -5 9 0 134.89 16.60 -5 9 0 142.89 9.40 5 9 0 126.09 15.80 -6 -9 0 -0.60 0.80 6 -9 0 1.40 0.80 6 9 0 1.00 1.10 -6 9 0 0.70 0.80 6 9 0 -2.30 4.30 -6 9 0 0.10 4.80 -7 -9 0 33.70 2.80 7 -9 0 30.90 2.50 -7 9 0 30.00 2.60 -7 9 0 20.70 7.70 7 9 0 28.90 2.90 7 9 0 23.70 7.30 8 -9 0 27.00 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25.70 2.00 7 -10 0 3.90 0.80 -7 -10 0 2.00 0.90 -7 10 0 -0.30 4.50 -7 10 0 4.40 1.00 7 10 0 2.60 1.00 7 10 0 1.90 4.30 -8 -10 0 7.70 1.30 8 -10 0 9.10 1.20 -8 10 0 6.70 1.10 8 10 0 6.20 1.10 -8 10 0 5.80 4.80 9 -10 0 11.00 1.10 -9 -10 0 9.40 1.20 9 10 0 8.50 1.20 -9 10 0 7.70 1.20 -10 -10 0 -0.60 0.50 10 -10 0 -0.30 0.40 -10 10 0 -0.20 0.50 10 10 0 0.00 0.50 0 -11 0 0.00 0.60 0 11 0 0.20 0.60 0 11 0 2.20 4.20 1 -11 0 29.20 2.30 -1 -11 0 26.80 2.30 -1 11 0 36.60 9.00 -1 11 0 32.90 2.30 1 11 0 28.20 7.40 1 11 0 30.70 2.40 2 -11 0 32.90 2.50 -2 -11 0 31.90 2.60 2 11 0 35.90 2.60 -2 11 0 36.00 2.50 -2 11 0 36.50 7.80 2 11 0 36.30 8.30 3 -11 0 0.50 0.50 -3 -11 0 0.90 0.60 3 11 0 -2.30 3.70 3 11 0 0.90 0.70 -3 11 0 1.60 3.50 -3 11 0 1.40 0.60 -4 -11 0 10.00 1.30 4 -11 0 8.80 1.10 4 11 0 7.10 5.10 4 11 0 10.50 1.40 -4 11 0 11.60 1.20 -4 11 0 17.30 5.80 -5 -11 0 21.00 1.80 5 -11 0 19.10 1.70 5 11 0 18.70 5.10 -5 11 0 11.90 5.30 -5 11 0 23.60 1.80 5 11 0 22.60 1.90 -6 -11 0 0.30 0.60 6 -11 0 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4 -4 13.60 1.30 -17 -4 4 19.10 1.50 17 -4 -4 16.90 1.50 -17 -4 4 18.30 1.60 17 -4 -4 21.30 1.60 -17 4 4 18.80 1.60 17 4 -4 21.50 1.70 16 -4 -4 3.60 0.70 16 -4 -4 3.10 0.60 -16 -4 4 3.60 0.70 16 4 -4 3.90 0.90 16 4 -4 3.60 0.70 -16 4 4 4.00 0.80 15 -4 -4 34.30 2.50 -15 -4 4 31.60 2.50 15 -4 -4 29.90 2.40 15 4 -4 31.40 2.50 15 4 -4 35.80 2.80 -15 4 4 33.10 2.60 -14 -4 4 88.49 6.00 14 -4 -4 90.59 5.90 14 -4 -4 87.89 5.90 14 4 -4 88.19 6.20 14 4 -4 87.59 6.00 -14 4 4 85.49 6.00 13 -4 -4 6.40 1.10 -13 -4 4 7.30 1.20 13 -4 -4 5.50 7.60 13 -4 -4 6.40 1.00 13 4 -4 6.70 1.40 -13 4 4 7.00 1.10 13 4 -4 2.80 6.60 13 4 -4 5.80 1.20 -12 -4 4 87.29 6.00 12 -4 -4 89.79 5.90 12 -4 -4 56.79 15.20 12 4 -4 92.99 6.40 -12 4 4 83.59 5.90 12 4 -4 81.89 5.90 -11 -4 4 146.89 10.60 11 -4 -4 138.29 21.90 11 -4 -4 179.88 10.50 11 4 -4 148.09 10.60 11 4 -4 168.18 10.50 11 4 -4 144.49 23.30 -11 4 4 163.48 10.60 10 -4 -4 7.90 5.70 -10 -4 4 3.20 1.10 10 -4 -4 3.40 1.00 10 -4 -4 3.50 2.00 -10 4 4 2.90 5.60 -10 4 4 1.10 1.10 10 4 -4 5.40 1.10 10 4 -4 2.70 6.80 10 4 -4 2.80 1.20 9 -4 -4 382.56 23.60 9 -4 -4 350.66 34.60 -9 -4 4 359.96 22.90 9 -4 -4 350.46 22.90 -9 4 4 301.77 23.20 -9 4 4 418.36 29.60 9 4 -4 398.06 37.90 9 4 -4 344.17 23.00 9 4 -4 346.67 22.90 8 -4 -4 176.98 20.60 -8 -4 4 163.18 10.50 8 -4 -4 160.08 11.10 8 -4 -4 139.19 10.80 8 4 -4 180.28 21.50 -8 4 4 191.58 16.20 8 4 -4 148.79 10.60 -7 -4 4 25.00 12.70 7 -4 -4 12.30 5.60 -7 -4 4 27.90 12.40 -7 4 4 8.90 4.40 7 4 -4 14.70 6.60 6 -4 -4 271.97 24.30 -6 -4 4 269.57 32.20 -6 4 4 241.98 19.90 6 4 -4 277.57 25.30 6 4 -4 232.78 19.00 -5 -4 4 445.36 40.00 5 -4 -4 417.56 32.60 5 4 -4 459.55 34.90 5 4 -4 472.85 42.90 -5 4 4 381.56 29.60 5 4 -4 362.16 28.90 4 -4 -4 11.10 3.90 4 -4 -4 10.20 4.40 4 4 -4 14.50 3.90 4 4 -4 11.30 6.90 4 4 -4 10.10 5.00 -4 4 4 15.20 5.00 -3 -4 4 1133.89 82.09 3 -4 -4 1134.59 73.99 3 -4 -4 1162.78 76.39 3 4 -4 1127.89 81.09 3 4 -4 1113.89 76.39 -3 4 4 1123.49 76.99 3 4 -4 968.00 72.69 2 -4 -4 1146.39 82.79 -2 -4 4 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5 -4 95.39 22.40 6 5 -4 68.39 11.60 6 5 -4 80.79 5.80 -5 -5 4 49.30 14.10 5 5 -4 13.60 11.10 5 5 -4 20.40 6.30 -5 5 4 16.10 4.90 5 5 -4 18.90 5.20 -4 -5 4 244.48 30.90 4 5 -4 215.68 30.70 4 5 -4 270.67 21.00 4 5 -4 298.37 23.00 -3 -5 4 16.30 9.90 3 5 -4 11.70 4.20 3 5 -4 35.20 14.20 -2 -5 4 10.40 8.40 2 5 -4 -7.00 10.90 2 5 -4 9.90 4.20 -1 -5 4 546.05 47.20 1 5 -4 511.85 38.70 1 5 -4 566.14 49.50 0 -5 4 36.80 9.70 0 5 -4 29.00 11.40 0 5 -4 30.60 7.60 1 -5 4 197.88 29.10 -1 5 -4 159.28 27.40 -1 5 -4 216.68 19.50 2 -5 4 39.10 13.20 -2 5 -4 56.29 11.40 -2 5 -4 40.10 16.80 -3 5 -4 223.18 14.80 -3 5 -4 182.98 46.30 -3 5 -4 258.27 23.80 -4 -5 -4 238.58 14.90 4 -5 4 216.58 14.60 -4 5 -4 234.88 24.30 -4 5 -4 218.98 14.60 -5 -5 -4 91.19 6.40 5 -5 4 81.69 5.90 -5 5 -4 87.79 6.00 -5 5 -4 80.19 16.20 -6 -5 -4 30.60 3.10 6 -5 4 34.00 3.00 -6 5 -4 25.00 2.90 -7 5 -4 32.50 10.90 -7 5 -4 30.70 3.00 -8 -5 -4 88.19 6.60 8 -5 4 85.39 6.30 -8 5 -4 84.29 16.70 -8 5 -4 94.99 6.20 9 -5 4 1.10 1.30 -9 -5 -4 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-5 77.49 6.30 11 -6 -5 81.39 5.20 11 6 -5 78.79 5.30 10 -6 -5 197.48 13.70 10 -6 -5 209.78 12.90 10 -6 -5 201.38 12.80 -10 -6 5 190.08 13.00 10 6 -5 206.28 13.00 -10 6 5 190.08 19.90 -10 6 5 186.18 13.00 9 -6 -5 10.40 1.70 9 -6 -5 9.20 1.10 -9 -6 5 10.20 1.60 9 -6 -5 12.10 2.30 9 6 -5 9.20 1.40 -9 6 5 6.10 4.70 -9 6 5 12.70 1.50 8 -6 -5 307.17 20.80 8 -6 -5 331.57 21.50 -8 -6 5 305.97 21.00 8 -6 -5 334.37 20.70 -8 6 5 371.06 27.00 8 6 -5 312.17 20.90 -8 6 5 330.27 20.80 7 -6 -5 377.96 23.80 7 -6 -5 369.16 23.90 7 -6 -5 372.86 24.50 7 -6 -5 381.56 24.50 -7 -6 5 353.16 24.10 7 6 -5 370.66 28.10 7 6 -5 369.26 24.00 -7 6 5 430.36 29.90 -7 6 5 371.26 23.90 6 -6 -5 11.70 1.90 6 -6 -5 9.20 1.60 -6 -6 5 7.50 1.20 6 -6 -5 9.90 1.30 6 6 -5 6.10 4.20 -6 6 5 9.60 1.40 -6 6 5 9.80 4.70 6 6 -5 7.20 1.20 5 -6 -5 372.66 23.80 -5 -6 5 339.07 23.50 5 -6 -5 366.66 23.80 5 -6 -5 366.06 23.30 5 6 -5 376.86 28.20 -5 6 5 402.26 28.80 5 6 -5 357.56 23.40 4 -6 -5 321.57 19.20 -4 -6 5 244.08 18.00 4 -6 -5 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2.80 3 -2 -18 1.90 1.50 3 -2 -18 1.70 0.80 3 2 -18 0.50 2.40 3 2 -18 1.40 1.20 3 2 -18 2.50 1.20 2 -2 -18 -0.20 0.60 2 -2 -18 -0.40 1.20 2 -2 -18 0.40 2.10 2 2 -18 0.60 2.20 2 2 -18 -0.40 0.90 2 2 -18 0.60 1.00 1 -2 -18 0.30 1.10 1 -2 -18 0.50 1.80 1 -2 -18 1.20 0.60 1 2 -18 -0.10 2.00 1 2 -18 1.30 0.90 0 -2 -18 0.00 0.90 0 -2 -18 0.40 0.40 0 -2 -18 0.30 1.10 0 2 -18 0.60 0.80 0 2 -18 -0.30 1.50 14 -3 -18 6.10 0.60 14 -3 -18 7.00 0.80 14 3 -18 7.10 0.80 14 3 -18 3.90 1.40 13 -3 -18 15.30 1.40 13 -3 -18 15.80 1.20 13 3 -18 18.10 1.40 13 3 -18 11.60 2.30 12 -3 -18 3.10 0.50 12 -3 -18 0.80 1.50 12 -3 -18 2.10 0.60 12 3 -18 3.30 0.60 12 3 -18 1.10 1.40 11 -3 -18 0.00 2.30 11 -3 -18 0.50 1.80 11 -3 -18 1.30 0.40 11 -3 -18 1.10 0.70 11 3 -18 1.10 0.60 11 3 -18 0.40 1.40 11 3 -18 1.70 2.00 10 -3 -18 7.60 0.80 10 -3 -18 7.50 1.10 10 -3 -18 7.10 1.80 10 -3 -18 2.00 2.80 10 -3 -18 3.60 2.30 10 3 -18 3.10 2.90 10 3 -18 5.90 1.90 10 3 -18 7.80 0.90 9 -3 -18 1.70 1.20 9 -3 -18 1.70 2.90 9 -3 -18 3.00 0.80 9 -3 -18 1.60 2.10 9 -3 -18 2.60 0.50 9 -3 -18 2.80 1.60 9 3 -18 3.10 0.70 9 3 -18 1.00 1.50 9 3 -18 1.00 2.90 8 -3 -18 2.20 0.80 8 -3 -18 0.30 2.80 8 -3 -18 3.40 1.70 8 -3 -18 3.10 1.20 8 -3 -18 3.40 0.60 8 -3 -18 1.60 2.00 8 3 -18 1.40 1.70 8 3 -18 0.40 2.70 8 3 -18 3.00 0.70 7 -3 -18 6.50 4.00 7 -3 -18 15.50 2.90 7 -3 -18 11.50 2.10 7 -3 -18 13.10 1.90 7 -3 -18 14.60 1.50 7 3 -18 8.40 3.70 7 3 -18 13.10 1.30 7 3 -18 12.00 2.30 6 -3 -18 6.00 1.80 6 -3 -18 6.30 2.20 6 -3 -18 7.50 1.30 6 -3 -18 2.40 3.20 6 3 -18 3.40 3.20 6 3 -18 6.00 1.70 5 -3 -18 1.10 3.00 5 -3 -18 2.40 1.60 5 -3 -18 0.40 1.60 5 -3 -18 1.20 0.90 5 3 -18 1.70 0.90 5 3 -18 1.10 2.70 5 3 -18 0.70 1.20 4 -3 -18 7.80 1.90 4 -3 -18 6.70 1.10 4 -3 -18 5.50 1.60 4 -3 -18 1.80 2.90 4 3 -18 5.00 1.50 4 3 -18 3.50 2.60 4 3 -18 5.30 1.10 3 -3 -18 -0.10 0.70 3 -3 -18 -0.40 2.20 3 -3 -18 -0.30 1.20 3 3 -18 -0.60 2.10 3 3 -18 1.40 1.00 3 3 -18 0.90 0.90 2 -3 -18 1.30 1.30 2 -3 -18 1.70 0.70 2 -3 -18 0.30 1.90 2 3 -18 2.00 0.90 2 3 -18 -0.30 1.90 1 -3 -18 0.80 1.60 1 -3 -18 4.70 0.80 1 -3 -18 2.90 1.10 1 3 -18 4.00 0.90 1 3 -18 1.00 1.80 13 -4 -18 0.40 0.50 13 -4 -18 0.50 0.30 13 4 -18 0.70 1.00 13 4 -18 0.90 0.40 12 -4 -18 10.90 1.10 12 -4 -18 11.30 0.90 12 4 -18 11.40 1.00 12 4 -18 13.40 2.00 11 -4 -18 7.00 1.90 11 -4 -18 10.30 0.80 11 -4 -18 8.10 1.10 11 4 -18 8.70 1.90 11 4 -18 10.30 0.90 10 -4 -18 4.00 0.50 10 -4 -18 0.70 2.50 10 -4 -18 3.30 0.70 10 -4 -18 2.20 1.80 10 4 -18 4.00 1.60 10 4 -18 3.60 0.60 10 4 -18 2.10 2.30 9 -4 -18 34.90 2.30 9 -4 -18 35.10 2.60 9 -4 -18 34.80 3.40 9 -4 -18 42.20 3.10 9 -4 -18 26.80 3.90 9 4 -18 31.10 4.80 9 4 -18 32.70 3.30 8 -4 -18 8.00 1.30 8 -4 -18 13.80 1.40 8 -4 -18 10.10 2.60 8 -4 -18 17.10 2.40 8 4 -18 9.40 3.30 8 4 -18 11.90 2.10 7 -4 -18 3.60 1.60 7 -4 -18 2.00 0.80 7 -4 -18 4.10 1.10 7 -4 -18 3.20 2.00 7 -4 -18 0.90 2.80 7 4 -18 1.00 2.80 7 4 -18 2.00 1.50 6 -4 -18 8.30 3.60 6 -4 -18 11.90 1.30 6 -4 -18 19.40 2.40 6 4 -18 6.30 3.10 5 -4 -18 10.90 1.90 5 -4 -18 4.40 3.10 5 -4 -18 6.00 0.90 5 -4 -18 10.70 1.40 5 4 -18 1.30 2.50 5 4 -18 7.70 1.60 4 -4 -18 0.40 2.30 4 -4 -18 0.90 0.50 4 -4 -18 1.80 1.40 4 -4 -18 0.50 0.70 4 4 -18 0.60 0.90 4 4 -18 0.20 2.10 3 -4 -18 7.30 2.90 3 4 -18 4.70 2.40 2 -4 -18 9.90 1.60 11 -5 -18 10.50 0.80 11 5 -18 9.40 1.70 10 -5 -18 12.30 0.90 10 5 -18 9.60 1.70 9 -5 -18 0.10 0.90 9 -5 -18 0.20 0.60 9 5 -18 0.50 1.20 9 5 -18 -0.10 1.70 8 -5 -18 4.40 0.90 8 -5 -18 6.00 1.60 8 5 -18 6.60 1.40 8 5 -18 4.50 2.40 7 -5 -18 9.30 1.70 7 -5 -18 9.60 1.20 7 -5 -18 13.70 1.60 7 5 -18 13.40 1.90 7 5 -18 10.90 2.90 6 -5 -18 -0.40 0.50 6 -5 -18 0.40 0.80 6 -5 -18 1.90 1.30 6 5 -18 0.10 2.00 6 5 -18 2.20 1.00 5 -5 -18 11.70 1.40 5 -5 -18 10.90 1.70 5 -5 -18 8.50 1.00 5 5 -18 6.40 2.30 4 -5 -18 1.00 1.20 4 -5 -18 1.00 0.70 4 -5 -18 0.10 0.50 4 5 -18 0.00 1.70 14 0 -19 0.30 0.30 14 0 -19 -0.30 1.20 14 0 -19 -0.20 0.40 13 0 -19 0.30 0.30 13 0 -19 0.00 0.50 13 0 -19 0.60 1.20 12 0 -19 -0.10 0.50 12 0 -19 0.30 1.40 12 0 -19 1.00 1.70 12 0 -19 0.00 0.30 11 0 -19 0.00 0.50 11 0 -19 0.60 2.00 11 0 -19 -0.40 1.30 11 0 -19 -0.10 0.40 10 0 -19 0.20 1.50 10 0 -19 0.00 0.40 10 0 -19 -1.00 2.20 10 0 -19 0.10 0.50 9 0 -19 0.10 2.50 9 0 -19 0.10 0.60 9 0 -19 0.50 1.10 9 0 -19 0.00 1.50 8 0 -19 -0.40 1.50 8 0 -19 -0.10 1.10 8 0 -19 -0.10 0.60 8 0 -19 0.50 2.80 7 0 -19 0.00 1.10 7 0 -19 0.00 0.60 7 0 -19 0.90 2.80 7 0 -19 -0.10 1.40 6 0 -19 1.70 2.80 6 0 -19 0.70 1.40 6 0 -19 -1.20 1.10 5 0 -19 0.40 2.60 5 0 -19 0.40 1.30 5 0 -19 0.20 1.10 4 0 -19 0.40 1.20 4 0 -19 0.10 2.30 4 0 -19 -0.90 1.00 3 0 -19 0.50 1.00 3 0 -19 -0.20 1.00 3 0 -19 0.60 1.90 2 0 -19 0.80 1.60 2 0 -19 -0.20 0.80 14 -1 -19 1.70 0.50 14 -1 -19 1.90 0.30 14 -1 -19 0.70 1.00 14 1 -19 0.70 1.00 14 1 -19 2.00 0.50 13 -1 -19 5.00 1.50 13 -1 -19 4.80 0.60 13 -1 -19 5.10 0.70 13 1 -19 5.40 0.80 13 1 -19 3.10 1.40 12 -1 -19 5.40 1.70 12 -1 -19 3.00 1.90 12 1 -19 5.70 1.60 12 1 -19 5.00 1.90 11 -1 -19 -0.60 1.80 11 -1 -19 0.10 0.30 11 -1 -19 -0.40 1.50 11 -1 -19 0.20 0.60 11 1 -19 0.60 1.90 11 1 -19 -0.20 1.30 11 1 -19 0.10 0.50 10 -1 -19 10.40 2.20 10 -1 -19 14.20 1.30 10 -1 -19 13.60 1.10 10 1 -19 9.40 2.20 10 1 -19 12.70 1.30 9 -1 -19 3.30 1.70 9 -1 -19 7.90 1.60 9 -1 -19 3.30 3.00 9 1 -19 2.50 3.00 9 1 -19 4.90 1.80 8 -1 -19 1.50 1.70 8 -1 -19 2.30 1.30 8 -1 -19 0.60 2.90 8 -1 -19 2.30 0.80 8 1 -19 -0.20 2.80 8 1 -19 2.50 0.70 8 1 -19 2.00 1.00 8 1 -19 1.90 1.50 7 -1 -19 15.60 1.50 7 -1 -19 11.70 1.90 7 -1 -19 13.40 2.60 7 1 -19 11.20 1.80 7 1 -19 11.50 2.50 7 1 -19 16.70 1.40 6 -1 -19 6.70 1.80 6 -1 -19 7.30 1.60 6 -1 -19 6.00 1.00 6 -1 -19 5.50 2.90 6 1 -19 5.80 1.70 6 1 -19 5.20 3.40 6 1 -19 7.40 1.30 5 -1 -19 0.70 0.70 5 -1 -19 1.00 1.40 5 -1 -19 1.00 1.20 5 -1 -19 -0.70 2.80 5 1 -19 0.20 1.20 5 1 -19 1.80 1.10 5 1 -19 -0.50 2.40 4 -1 -19 4.60 2.90 4 -1 -19 7.70 1.40 4 -1 -19 11.00 1.90 4 1 -19 8.20 1.30 4 1 -19 8.90 1.70 4 1 -19 4.00 2.60 3 -1 -19 4.30 2.50 3 -1 -19 8.20 1.30 3 1 -19 5.10 2.50 3 1 -19 7.80 1.30 3 1 -19 5.30 1.20 2 -1 -19 -0.40 0.90 2 -1 -19 -0.10 1.40 2 1 -19 -0.70 0.80 2 1 -19 -0.50 1.50 13 -2 -19 2.60 0.40 13 -2 -19 1.20 1.10 13 -2 -19 2.80 0.60 13 2 -19 2.30 1.30 13 2 -19 2.60 0.50 12 -2 -19 1.20 0.50 12 -2 -19 1.30 0.40 12 -2 -19 0.20 1.30 12 2 -19 1.10 0.50 12 2 -19 0.80 1.40 11 -2 -19 26.00 1.70 11 -2 -19 24.30 1.90 11 -2 -19 18.40 3.10 11 2 -19 26.00 1.80 11 2 -19 19.90 3.00 10 -2 -19 19.30 1.40 10 -2 -19 15.00 2.30 10 -2 -19 18.50 1.60 10 2 -19 20.80 1.60 10 2 -19 16.50 2.70 9 -2 -19 2.10 0.70 9 -2 -19 1.30 0.40 9 -2 -19 0.50 2.70 9 -2 -19 0.70 1.80 9 -2 -19 2.50 1.40 9 2 -19 1.20 1.60 9 2 -19 2.00 0.60 9 2 -19 0.30 2.80 8 -2 -19 30.00 3.00 8 -2 -19 19.90 4.60 8 -2 -19 28.60 2.60 8 -2 -19 32.20 2.40 8 -2 -19 25.60 3.50 8 2 -19 31.90 3.30 8 2 -19 34.90 2.30 7 -2 -19 8.70 2.10 7 -2 -19 11.30 1.80 7 -2 -19 7.40 3.30 7 -2 -19 10.50 1.50 7 2 -19 8.30 1.90 7 2 -19 5.60 3.10 6 -2 -19 10.10 2.00 6 -2 -19 4.40 2.80 6 -2 -19 10.90 1.80 6 -2 -19 10.20 1.40 6 2 -19 12.30 2.10 6 2 -19 6.30 3.00 5 -2 -19 17.20 4.00 5 -2 -19 24.80 1.90 5 -2 -19 21.20 2.80 5 -2 -19 25.80 2.50 5 2 -19 14.80 3.90 5 2 -19 25.00 2.50 5 2 -19 20.90 2.00 4 -2 -19 -1.10 2.20 4 -2 -19 1.20 1.20 4 -2 -19 3.10 0.70 4 2 -19 0.20 1.00 4 2 -19 0.00 2.30 4 2 -19 2.20 0.90 3 -2 -19 5.20 0.80 3 -2 -19 1.50 1.90 3 -2 -19 5.70 1.20 3 2 -19 5.40 1.00 3 2 -19 1.90 2.20 12 -3 -19 0.50 1.20 12 -3 -19 3.00 0.40 12 -3 -19 2.50 0.60 12 3 -19 2.60 0.50 12 3 -19 1.60 1.30 11 -3 -19 0.40 0.60 11 -3 -19 0.90 1.30 11 -3 -19 1.10 0.30 11 3 -19 0.50 1.30 11 3 -19 0.80 1.50 11 3 -19 2.50 0.50 10 -3 -19 6.50 1.80 10 -3 -19 6.40 0.60 10 -3 -19 2.20 2.20 10 -3 -19 5.70 0.90 10 3 -19 2.30 2.00 10 3 -19 5.40 0.70 10 3 -19 5.90 1.60 9 -3 -19 0.60 2.20 9 -3 -19 0.60 0.60 9 -3 -19 -0.30 1.50 9 -3 -19 1.10 1.20 9 3 -19 0.30 1.20 9 3 -19 0.60 0.40 9 3 -19 -1.20 2.00 8 -3 -19 1.70 0.90 8 -3 -19 1.00 1.50 8 -3 -19 0.20 2.20 8 -3 -19 1.10 1.30 8 3 -19 1.10 1.20 8 3 -19 0.00 2.30 7 -3 -19 4.60 1.50 7 -3 -19 5.20 1.00 7 -3 -19 3.80 1.60 7 -3 -19 0.80 2.40 7 3 -19 3.20 1.30 7 3 -19 3.30 2.60 6 -3 -19 2.20 2.60 6 -3 -19 5.60 1.50 6 -3 -19 9.20 1.30 6 -3 -19 5.60 1.60 6 3 -19 9.40 1.80 6 3 -19 3.20 2.30 5 -3 -19 -0.30 1.10 5 -3 -19 1.20 2.20 5 -3 -19 1.10 0.70 5 3 -19 0.90 0.90 5 3 -19 0.30 1.80 4 -3 -19 4.90 1.30 4 -3 -19 5.60 0.80 4 3 -19 1.00 2.00 10 4 -19 -0.40 1.00 10 4 -19 0.30 1.30 9 4 -19 0.90 1.70 9 4 -19 0.60 1.10 8 -4 -19 0.20 2.10 8 -4 -19 0.30 0.80 8 -4 -19 0.70 1.10 8 4 -19 0.80 1.90 8 4 -19 0.90 1.00 7 -4 -19 0.70 2.30 7 -4 -19 0.70 0.70 7 -4 -19 0.80 1.10 7 4 -19 0.20 0.90 7 4 -19 1.50 1.90 6 -4 -19 -0.80 1.90 6 -4 -19 0.10 0.60 6 -4 -19 0.30 1.20 6 4 -19 0.20 0.70 6 4 -19 0.20 1.60 11 0 -20 1.40 1.20 11 0 -20 2.80 0.50 11 0 -20 1.10 1.50 10 0 -20 5.90 1.60 10 0 -20 7.00 0.80 10 0 -20 4.80 2.20 9 0 -20 1.00 2.00 9 0 -20 0.30 1.20 9 0 -20 1.10 0.50 8 0 -20 0.70 2.10 8 0 -20 0.80 1.00 8 0 -20 3.90 1.40 7 0 -20 2.80 0.90 7 0 -20 1.10 2.20 7 0 -20 4.10 1.30 6 0 -20 -0.90 0.70 6 0 -20 0.40 1.00 6 0 -20 0.30 1.90 11 -1 -20 1.20 1.40 11 -1 -20 1.20 1.20 11 1 -20 0.10 1.30 11 1 -20 3.00 0.60 11 1 -20 1.90 1.30 10 -1 -20 0.70 0.50 10 -1 -20 -0.30 1.30 10 -1 -20 -0.30 1.80 10 1 -20 0.60 0.40 10 1 -20 -0.30 1.60 10 1 -20 -0.20 1.10 9 -1 -20 1.40 2.00 9 -1 -20 1.50 0.90 9 -1 -20 4.00 0.70 9 -1 -20 3.10 1.30 9 1 -20 4.60 1.30 9 1 -20 1.20 2.00 9 1 -20 3.50 0.60 8 -1 -20 0.80 0.90 8 -1 -20 0.50 1.90 8 -1 -20 0.40 1.10 8 1 -20 1.20 1.20 8 1 -20 0.20 2.00 7 -1 -20 0.40 1.90 7 -1 -20 0.10 0.90 7 -1 -20 -0.20 1.00 7 1 -20 0.00 1.90 7 1 -20 0.00 1.10 6 -1 -20 1.10 1.00 6 -1 -20 0.70 1.90 6 -1 -20 1.20 1.20 6 1 -20 1.40 1.10 6 1 -20 0.40 1.90 9 -2 -20 0.20 1.70 9 -2 -20 0.80 0.90 9 -2 -20 -0.10 1.20 9 2 -20 0.60 1.00 9 2 -20 -0.30 1.60 8 -2 -20 -0.90 1.00 8 -2 -20 0.00 1.70 8 -2 -20 0.20 1.10 8 2 -20 0.20 1.00 8 2 -20 -1.50 1.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 31344 _olex2_submission_special_instructions 'No special instructions were received' 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.32996(3) -0.12812(4) 0.38952(3) 0.0587(2) Uani 1 1 d . . . . . Cl1 Cl 0.0592(3) 0.5603(4) 0.2709(3) 0.1363(14) Uani 1 1 d . . . . . Cl2 Cl 0.0686(3) 0.8210(4) 0.3398(3) 0.1254(12) Uani 1 1 d . . . . . O1 O 0.5194(4) 0.1021(5) 0.2668(4) 0.0570(12) Uani 1 1 d . . . . . O3 O 0.3117(4) 0.5710(5) 0.3583(4) 0.0641(13) Uani 1 1 d . . . . . N2 N 0.5070(4) 0.3187(6) 0.2850(4) 0.0517(12) Uani 1 1 d . . . . . H2 H 0.488945 0.393719 0.258666 0.062 Uiso 1 1 calc R U . . . N1 N 0.2686(4) 0.5021(6) 0.2183(4) 0.0545(13) Uani 1 1 d . . . . . C1 C 0.5455(5) 0.3153(7) 0.3805(4) 0.0501(14) Uani 1 1 d . . . . . H1 H 0.559957 0.222924 0.399466 0.060 Uiso 1 1 calc R U . . . C4 C 0.3208(5) 0.0765(8) 0.3739(5) 0.0536(16) Uani 1 1 d . . . . . C6 C 0.4979(5) 0.2113(7) 0.2351(5) 0.0515(14) Uani 1 1 d . . . . . C8 C 0.6300(5) 0.3944(7) 0.4220(5) 0.0519(15) Uani 1 1 d . . . . . H8 H 0.651947 0.412068 0.482551 0.062 Uiso 1 1 calc R U . . . C10 C 0.7587(5) 0.5184(7) 0.4221(5) 0.0539(15) Uani 1 1 d . . . . . C12 C 0.3921(5) 0.2854(7) 0.3814(4) 0.0514(14) Uani 1 1 d . . . . . C14 C 0.2370(6) 0.1306(7) 0.3288(6) 0.0566(17) Uani 1 1 d . . . . . H14 H 0.185457 0.079302 0.312950 0.068 Uiso 1 1 calc R U . . . C16 C 0.4769(5) 0.3647(6) 0.4125(5) 0.0525(15) Uani 1 1 d . . . . . H16A H 0.505049 0.365242 0.477035 0.063 Uiso 1 1 calc R U . . . H16B H 0.461300 0.455543 0.392827 0.063 Uiso 1 1 calc R U . . . C18 C 0.2970(5) 0.4836(7) 0.3040(5) 0.0526(15) Uani 1 1 d . . . . . C20 C 0.6763(5) 0.4414(7) 0.3812(5) 0.0530(15) Uani 1 1 d . . . . . H20 H 0.654423 0.423910 0.320662 0.064 Uiso 1 1 calc R U . . . C22 C 0.2586(6) 0.4030(8) 0.1505(5) 0.0622(17) Uani 1 1 d . . . . . H22A H 0.200763 0.358920 0.129102 0.075 Uiso 1 1 calc R U . . . H22B H 0.305971 0.337119 0.173320 0.075 Uiso 1 1 calc R U . . . C24 C 0.3087(5) 0.3392(6) 0.3334(5) 0.0499(14) Uani 1 1 d . . . . . C25 C 0.8172(6) 0.5220(10) 0.3828(6) 0.068(2) Uani 1 1 d . . . . . H25 H 0.802446 0.476624 0.329692 0.082 Uiso 1 1 calc R U . . . C13 C 0.7798(5) 0.5926(8) 0.4979(5) 0.0594(17) Uani 1 1 d . . . . . H13 H 0.739717 0.595655 0.523503 0.071 Uiso 1 1 calc R U . . . C7 C 0.3983(5) 0.1512(7) 0.4018(5) 0.0525(15) Uani 1 1 d . . . . . H7 H 0.454189 0.112067 0.433928 0.063 Uiso 1 1 calc R U . . . C15 C 0.2223(7) 0.6125(8) 0.0832(6) 0.069(2) Uani 1 1 d . . . . . H15A H 0.242529 0.683260 0.056881 0.083 Uiso 1 1 calc R U . . . H15B H 0.157325 0.605949 0.052035 0.083 Uiso 1 1 calc R U . . . C2 C 0.2314(5) 0.2639(7) 0.3076(5) 0.0549(15) Uani 1 1 d . . . . . H2A H 0.175423 0.303012 0.275933 0.066 Uiso 1 1 calc R U . . . C17 C 0.4605(6) 0.2347(9) 0.1370(5) 0.0603(17) Uani 1 1 d . . . . . H17A H 0.503703 0.207606 0.115978 0.091 Uiso 1 1 calc R U . . . H17B H 0.447434 0.327235 0.124836 0.091 Uiso 1 1 calc R U . . . H17C H 0.406291 0.184149 0.107290 0.091 Uiso 1 1 calc R U . . . C9 C 0.2515(6) 0.6364(7) 0.1800(6) 0.0592(18) Uani 1 1 d . . . . . H9A H 0.305604 0.689969 0.204833 0.071 Uiso 1 1 calc R U . . . H9B H 0.204690 0.680265 0.190596 0.071 Uiso 1 1 calc R U . . . C19 C 0.8602(6) 0.6632(9) 0.5369(6) 0.0664(19) Uani 1 1 d . . . . . H19 H 0.874833 0.709396 0.589703 0.080 Uiso 1 1 calc R U . . . C5 C 0.8955(6) 0.5900(10) 0.4198(7) 0.073(2) Uani 1 1 d . . . . . H5 H 0.934953 0.586960 0.393372 0.087 Uiso 1 1 calc R U . . . C21 C 0.9179(6) 0.6641(10) 0.4966(7) 0.071(2) Uani 1 1 d . . . . . C11 C 1.0022(7) 0.7453(12) 0.5353(9) 0.093(3) Uani 1 1 d . . . . . H11A H 0.987233 0.836340 0.539103 0.139 Uiso 1 1 calc R U . . . H11B H 1.032967 0.738540 0.498021 0.139 Uiso 1 1 calc R U . . . H11C H 1.040479 0.713011 0.593728 0.139 Uiso 1 1 calc R U . . . C23 C 0.2656(7) 0.4838(10) 0.0796(6) 0.075(2) Uani 1 1 d . . . . . H23A H 0.234190 0.441803 0.021988 0.090 Uiso 1 1 calc R U . . . H23B H 0.327989 0.496916 0.091215 0.090 Uiso 1 1 calc R U . . . C3 C 0.1169(8) 0.6666(11) 0.3588(9) 0.087(3) Uani 1 1 d . . . . . H3A H 0.117264 0.630156 0.412744 0.105 Uiso 1 1 calc R U . . . H3B H 0.178724 0.674112 0.367284 0.105 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0728(4) 0.0353(3) 0.0709(4) 0.00502(17) 0.0338(3) -0.00028(16) Cl1 0.140(3) 0.101(3) 0.127(3) -0.022(2) 0.018(2) -0.009(2) Cl2 0.118(2) 0.090(2) 0.152(3) 0.011(2) 0.043(2) 0.0259(18) O1 0.074(3) 0.032(2) 0.061(3) -0.002(2) 0.026(2) 0.002(2) O3 0.094(4) 0.037(3) 0.061(3) -0.002(2) 0.034(3) 0.007(2) N2 0.065(3) 0.043(3) 0.050(3) 0.000(2) 0.027(3) 0.001(2) N1 0.072(4) 0.033(3) 0.062(3) 0.006(2) 0.032(3) 0.001(2) C1 0.068(4) 0.033(3) 0.051(3) 0.001(3) 0.028(3) 0.000(3) C4 0.076(4) 0.036(4) 0.058(4) 0.000(3) 0.037(3) 0.000(3) C6 0.059(3) 0.043(4) 0.055(4) -0.004(3) 0.026(3) 0.000(3) C8 0.066(4) 0.038(3) 0.051(3) 0.000(3) 0.024(3) 0.001(3) C10 0.060(4) 0.041(3) 0.061(4) 0.003(3) 0.026(3) 0.001(3) C12 0.064(4) 0.047(4) 0.049(3) -0.006(3) 0.030(3) -0.005(3) C14 0.068(4) 0.043(4) 0.065(4) 0.001(3) 0.035(4) -0.003(3) C16 0.069(4) 0.037(3) 0.056(4) -0.005(3) 0.032(3) -0.001(3) C18 0.065(4) 0.037(3) 0.058(4) 0.000(3) 0.029(3) 0.000(3) C20 0.064(4) 0.037(3) 0.059(4) 0.000(3) 0.028(3) -0.001(3) C22 0.080(5) 0.049(4) 0.060(4) -0.004(3) 0.032(4) 0.001(4) C24 0.073(4) 0.026(3) 0.057(4) -0.001(3) 0.034(3) 0.002(3) C25 0.076(5) 0.064(5) 0.071(5) -0.002(4) 0.037(4) -0.003(4) C13 0.066(4) 0.047(4) 0.066(4) 0.001(3) 0.029(3) -0.004(3) C7 0.067(4) 0.043(4) 0.051(3) 0.001(3) 0.029(3) 0.004(3) C15 0.083(5) 0.049(4) 0.070(5) 0.008(4) 0.028(4) 0.004(4) C2 0.068(4) 0.034(3) 0.065(4) 0.004(3) 0.032(3) 0.005(3) C17 0.074(4) 0.057(4) 0.054(4) -0.004(3) 0.032(3) 0.000(3) C9 0.069(4) 0.041(4) 0.066(4) 0.007(3) 0.027(4) 0.002(3) C19 0.069(5) 0.056(4) 0.069(5) -0.003(4) 0.025(4) -0.006(4) C5 0.064(4) 0.071(5) 0.085(6) -0.001(5) 0.035(4) -0.006(4) C21 0.065(4) 0.059(5) 0.089(6) 0.002(4) 0.034(4) -0.006(4) C11 0.069(5) 0.081(7) 0.123(9) -0.012(6) 0.036(6) -0.022(5) C23 0.097(6) 0.063(5) 0.067(5) -0.003(4) 0.038(4) -0.005(4) C3 0.080(6) 0.066(6) 0.112(8) 0.006(6) 0.037(6) -0.006(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N2 H2 118.4 . . ? C6 N2 H2 118.4 . . ? C6 N2 C1 123.3(6) . . ? C18 N1 C22 127.8(6) . . ? C18 N1 C9 121.0(6) . . ? C22 N1 C9 110.9(6) . . ? N2 C1 H1 108.1 . . ? N2 C1 C8 112.3(6) . . ? N2 C1 C16 109.9(6) . . ? C8 C1 H1 108.1 . . ? C8 C1 C16 110.3(6) . . ? C16 C1 H1 108.1 . . ? C14 C4 I1 117.7(6) . . ? C14 C4 C7 122.4(7) . . ? C7 C4 I1 119.6(6) . . ? O1 C6 N2 122.3(7) . . ? O1 C6 C17 121.8(6) . . ? N2 C6 C17 115.8(6) . . ? C1 C8 H8 117.0 . . ? C20 C8 C1 126.0(7) . . ? C20 C8 H8 117.0 . . ? C25 C10 C20 119.6(7) . . ? C13 C10 C20 122.4(7) . . ? C13 C10 C25 117.9(7) . . ? C24 C12 C16 122.9(7) . . ? C24 C12 C7 118.6(7) . . ? C7 C12 C16 118.5(7) . . ? C4 C14 H14 121.1 . . ? C4 C14 C2 117.9(7) . . ? C2 C14 H14 121.1 . . ? C1 C16 H16A 108.5 . . ? C1 C16 H16B 108.5 . . ? C12 C16 C1 115.2(6) . . ? C12 C16 H16A 108.5 . . ? C12 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? O3 C18 N1 124.9(7) . . ? O3 C18 C24 120.0(6) . . ? N1 C18 C24 115.1(6) . . ? C8 C20 C10 125.8(7) . . ? C8 C20 H20 117.1 . . ? C10 C20 H20 117.1 . . ? N1 C22 H22A 111.2 . . ? N1 C22 H22B 111.2 . . ? N1 C22 C23 102.7(7) . . ? H22A C22 H22B 109.1 . . ? C23 C22 H22A 111.2 . . ? C23 C22 H22B 111.2 . . ? C12 C24 C18 121.5(6) . . ? C12 C24 C2 121.5(6) . . ? C2 C24 C18 117.0(6) . . ? C10 C25 H25 119.3 . . ? C5 C25 C10 121.5(8) . . ? C5 C25 H25 119.3 . . ? C10 C13 H13 119.3 . . ? C10 C13 C19 121.3(8) . . ? C19 C13 H13 119.3 . . ? C4 C7 C12 119.3(7) . . ? C4 C7 H7 120.3 . . ? C12 C7 H7 120.3 . . ? H15A C15 H15B 108.9 . . ? C9 C15 H15A 110.9 . . ? C9 C15 H15B 110.9 . . ? C9 C15 C23 104.3(7) . . ? C23 C15 H15A 110.9 . . ? C23 C15 H15B 110.9 . . ? C14 C2 C24 120.2(7) . . ? C14 C2 H2A 119.9 . . ? C24 C2 H2A 119.9 . . ? C6 C17 H17A 109.5 . . ? C6 C17 H17B 109.5 . . ? C6 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C9 C15 103.4(6) . . ? N1 C9 H9A 111.1 . . ? N1 C9 H9B 111.1 . . ? C15 C9 H9A 111.1 . . ? C15 C9 H9B 111.1 . . ? H9A C9 H9B 109.0 . . ? C13 C19 H19 120.3 . . ? C21 C19 C13 119.4(8) . . ? C21 C19 H19 120.3 . . ? C25 C5 H5 119.5 . . ? C25 C5 C21 121.0(8) . . ? C21 C5 H5 119.5 . . ? C19 C21 C5 118.7(8) . . ? C19 C21 C11 120.0(10) . . ? C5 C21 C11 121.3(9) . . ? C21 C11 H11A 109.5 . . ? C21 C11 H11B 109.5 . . ? C21 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C22 C23 C15 104.0(8) . . ? C22 C23 H23A 111.0 . . ? C22 C23 H23B 111.0 . . ? C15 C23 H23A 111.0 . . ? C15 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? Cl1 C3 H3A 109.4 . . ? Cl1 C3 H3B 109.4 . . ? Cl2 C3 Cl1 111.4(7) . . ? Cl2 C3 H3A 109.4 . . ? Cl2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 C4 2.099(8) . ? Cl1 C3 1.749(13) . ? Cl2 C3 1.733(12) . ? O1 C6 1.219(9) . ? O3 C18 1.224(9) . ? N2 H2 0.8700 . ? N2 C1 1.453(9) . ? N2 C6 1.348(9) . ? N1 C18 1.326(10) . ? N1 C22 1.479(10) . ? N1 C9 1.487(9) . ? C1 H1 0.9900 . ? C1 C8 1.508(10) . ? C1 C16 1.545(10) . ? C4 C14 1.385(12) . ? C4 C7 1.395(11) . ? C6 C17 1.512(10) . ? C8 H8 0.9400 . ? C8 C20 1.324(11) . ? C10 C20 1.469(10) . ? C10 C25 1.396(11) . ? C10 C13 1.393(11) . ? C12 C16 1.512(10) . ? C12 C24 1.384(11) . ? C12 C7 1.403(11) . ? C14 H14 0.9400 . ? C14 C2 1.397(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C18 C24 1.538(9) . ? C20 H20 0.9400 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 C23 1.497(13) . ? C24 C2 1.399(11) . ? C25 H25 0.9400 . ? C25 C5 1.368(13) . ? C13 H13 0.9400 . ? C13 C19 1.408(12) . ? C7 H7 0.9400 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 C9 1.508(13) . ? C15 C23 1.511(13) . ? C2 H2A 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C19 H19 0.9400 . ? C19 C21 1.397(13) . ? C5 H5 0.9400 . ? C5 C21 1.403(15) . ? C21 C11 1.515(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 C4 C14 C2 -171.3(6) . . . . ? I1 C4 C7 C12 172.1(5) . . . . ? O3 C18 C24 C12 -71.4(9) . . . . ? O3 C18 C24 C2 110.1(8) . . . . ? N2 C1 C8 C20 -12.9(10) . . . . ? N2 C1 C16 C12 60.7(8) . . . . ? N1 C18 C24 C12 110.3(8) . . . . ? N1 C18 C24 C2 -68.1(9) . . . . ? N1 C22 C23 C15 -34.5(9) . . . . ? C1 N2 C6 O1 2.0(11) . . . . ? C1 N2 C6 C17 -177.2(6) . . . . ? C1 C8 C20 C10 -179.9(7) . . . . ? C4 C14 C2 C24 -1.4(11) . . . . ? C6 N2 C1 C8 116.7(7) . . . . ? C6 N2 C1 C16 -120.2(7) . . . . ? C8 C1 C16 C12 -175.0(6) . . . . ? C10 C25 C5 C21 -3.2(16) . . . . ? C10 C13 C19 C21 3.1(13) . . . . ? C12 C24 C2 C14 -1.1(11) . . . . ? C14 C4 C7 C12 -2.1(11) . . . . ? C16 C1 C8 C20 -135.9(7) . . . . ? C16 C12 C24 C18 3.4(10) . . . . ? C16 C12 C24 C2 -178.2(6) . . . . ? C16 C12 C7 C4 179.8(6) . . . . ? C18 N1 C22 C23 -155.1(8) . . . . ? C18 N1 C9 C15 179.1(7) . . . . ? C18 C24 C2 C14 177.4(7) . . . . ? C20 C10 C25 C5 -178.5(9) . . . . ? C20 C10 C13 C19 178.6(8) . . . . ? C22 N1 C18 O3 173.0(8) . . . . ? C22 N1 C18 C24 -8.9(11) . . . . ? C22 N1 C9 C15 5.0(9) . . . . ? C24 C12 C16 C1 -121.9(7) . . . . ? C24 C12 C7 C4 -0.5(10) . . . . ? C25 C10 C20 C8 157.0(8) . . . . ? C25 C10 C13 C19 -3.6(12) . . . . ? C25 C5 C21 C19 2.6(15) . . . . ? C25 C5 C21 C11 -176.8(11) . . . . ? C13 C10 C20 C8 -25.2(12) . . . . ? C13 C10 C25 C5 3.7(13) . . . . ? C13 C19 C21 C5 -2.5(14) . . . . ? C13 C19 C21 C11 176.9(10) . . . . ? C7 C4 C14 C2 3.0(11) . . . . ? C7 C12 C16 C1 57.8(9) . . . . ? C7 C12 C24 C18 -176.4(6) . . . . ? C7 C12 C24 C2 2.0(10) . . . . ? C9 N1 C18 O3 -0.1(12) . . . . ? C9 N1 C18 C24 178.1(6) . . . . ? C9 N1 C22 C23 18.5(9) . . . . ? C9 C15 C23 C22 38.6(10) . . . . ? C23 C15 C9 N1 -26.4(9) . . . . ?